# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2014 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_cu-251 _audit_creation_method ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) ; _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C54 H76 Al2 N6' _chemical_formula_weight 863.17 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Al Al 0.2130 0.2455 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 16.54064(8) _cell_length_b 14.23921(7) _cell_length_c 22.09585(11) _cell_angle_alpha 90.00 _cell_angle_beta 90.9867(4) _cell_angle_gamma 90.00 _cell_volume 5203.37(4) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 29164 _cell_measurement_theta_min 3.2970 _cell_measurement_theta_max 73.8320 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.56 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.31 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.102 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1872 _exptl_absorpt_coefficient_mu 0.798 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6635 _exptl_absorpt_correction_T_max 0.7900 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'SuperNova (Cu) X-ray Source' _diffrn_radiation_monochromator mirror _diffrn_measurement_device_type 'SuperNova, Single source at offset, Atlas' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 36966 _diffrn_reflns_av_R_equivalents 0.0230 _diffrn_reflns_av_sigmaI/netI 0.0162 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 3.69 _diffrn_reflns_theta_max 67.50 _reflns_number_total 9324 _reflns_number_gt 8815 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) ; _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^)+(0.0619P)^2^+3.4833P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9324 _refine_ls_number_parameters 646 _refine_ls_number_restraints 119 _refine_ls_R_factor_all 0.0516 _refine_ls_R_factor_gt 0.0493 _refine_ls_wR_factor_ref 0.1272 _refine_ls_wR_factor_gt 0.1252 _refine_ls_goodness_of_fit_ref 1.009 _refine_ls_restrained_S_all 1.048 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Al1 Al 0.45254(3) 0.92486(4) 0.47957(2) 0.03415(15) Uani 1 1 d . . . H1A H 0.3668(12) 0.9377(15) 0.4619(9) 0.041 Uiso 1 1 d . . . H1B H 0.4893(13) 0.8252(15) 0.4735(9) 0.041 Uiso 1 1 d . . . Al2 Al 0.0360(3) 0.4784(2) 0.55612(8) 0.0254(10) Uani 0.296(6) 1 d PD . 1 H2B H 0.004(4) 0.420(4) 0.607(2) 0.030 Uiso 0.296(6) 1 d PD . 1 H2C H 0.119(2) 0.514(5) 0.573(3) 0.039(18) Uiso 0.296(6) 1 d PD . 1 Al2A Al -0.00616(15) 0.45371(9) 0.55552(3) 0.0249(4) Uani 0.704(6) 1 d PD . 2 H2D H -0.0849(13) 0.4046(18) 0.5671(12) 0.030 Uiso 0.704(6) 1 d PD . 2 H2E H 0.0592(14) 0.4466(19) 0.6039(11) 0.030 Uiso 0.704(6) 1 d PD . 2 N1 N 0.48075(8) 0.98102(10) 0.55579(6) 0.0271(3) Uani 1 1 d . . . N2 N 0.41522(8) 0.88545(10) 0.63027(6) 0.0278(3) Uani 1 1 d . . . N3 N 0.49952(8) 0.99286(10) 0.66380(6) 0.0301(3) Uani 1 1 d . . . N4 N 0.02773(8) 0.42369(9) 0.47619(6) 0.0218(3) Uani 1 1 d . . . N5 N 0.05091(8) 0.32082(9) 0.39219(6) 0.0255(3) Uani 1 1 d . . . N6 N 0.06972(8) 0.26288(9) 0.48280(6) 0.0264(3) Uani 1 1 d . . . C1 C 0.46665(9) 0.95581(12) 0.61064(7) 0.0256(3) Uani 1 1 d . . . C2 C 0.41913(11) 0.87838(13) 0.69319(7) 0.0332(4) Uani 1 1 d . . . H2A H 0.3901 0.8350 0.7172 0.040 Uiso 1 1 calc R . . C3 C 0.47079(11) 0.94317(13) 0.71355(7) 0.0348(4) Uani 1 1 d . . . H3A H 0.4856 0.9538 0.7547 0.042 Uiso 1 1 calc R . . C4 C 0.35943(9) 0.83282(11) 0.59261(7) 0.0244(3) Uani 1 1 d . . . C5 C 0.37821(10) 0.73971(12) 0.57786(8) 0.0312(4) Uani 1 1 d . . . C6 C 0.32222(11) 0.69079(13) 0.54237(9) 0.0387(4) Uani 1 1 d . . . H6A H 0.3336 0.6279 0.5309 0.046 Uiso 1 1 calc R . . C7 C 0.25066(12) 0.73163(14) 0.52351(9) 0.0408(4) Uani 1 1 d . . . H7A H 0.2132 0.6967 0.4994 0.049 Uiso 1 1 calc R . . C8 C 0.23314(11) 0.82294(13) 0.53940(8) 0.0346(4) Uani 1 1 d . . . H8A H 0.1832 0.8499 0.5266 0.041 Uiso 1 1 calc R . . C9 C 0.28725(10) 0.87629(11) 0.57389(7) 0.0268(3) Uani 1 1 d . . . C10 C 0.45400(12) 0.69078(14) 0.60126(11) 0.0446(5) Uani 1 1 d . . . H10A H 0.4924 0.7398 0.6167 0.054 Uiso 1 1 calc R . . C11 C 0.43342(15) 0.62544(17) 0.65393(11) 0.0545(6) Uani 1 1 d . . . H11A H 0.4071 0.6616 0.6858 0.082 Uiso 1 1 calc R . . H11B H 0.4832 0.5971 0.6702 0.082 Uiso 1 1 calc R . . H11C H 0.3968 0.5759 0.6395 0.082 Uiso 1 1 calc R . . C12 C 0.49657(16) 0.6342(2) 0.55234(13) 0.0694(8) Uani 1 1 d . . . H12A H 0.5091 0.6754 0.5182 0.104 Uiso 1 1 calc R . . H12B H 0.4611 0.5832 0.5383 0.104 Uiso 1 1 calc R . . H12C H 0.5468 0.6076 0.5691 0.104 Uiso 1 1 calc R . . C13 C 0.26870(11) 0.97788(12) 0.59004(9) 0.0351(4) Uani 1 1 d . . . H13A H 0.3207 1.0137 0.5892 0.042 Uiso 1 1 calc R . . C14 C 0.21020(18) 1.02443(17) 0.54526(12) 0.0649(7) Uani 1 1 d . . . H14A H 0.2087 1.0922 0.5529 0.097 Uiso 1 1 calc R . . H14B H 0.1560 0.9980 0.5501 0.097 Uiso 1 1 calc R . . H14C H 0.2283 1.0130 0.5039 0.097 Uiso 1 1 calc R . . C15 C 0.23485(18) 0.98765(17) 0.65280(11) 0.0616(7) Uani 1 1 d . . . H15A H 0.2717 0.9578 0.6822 0.092 Uiso 1 1 calc R . . H15B H 0.1818 0.9571 0.6542 0.092 Uiso 1 1 calc R . . H15C H 0.2291 1.0544 0.6627 0.092 Uiso 1 1 calc R . . C16 C 0.56150(9) 1.06337(11) 0.66762(7) 0.0248(3) Uani 1 1 d . . . C17 C 0.64177(10) 1.03430(12) 0.67528(7) 0.0285(3) Uani 1 1 d . B . C18 C 0.70087(10) 1.10341(13) 0.67892(8) 0.0343(4) Uani 1 1 d . . . H18A H 0.7559 1.0857 0.6843 0.041 Uiso 1 1 calc R . . C19 C 0.68126(11) 1.19680(13) 0.67494(9) 0.0371(4) Uani 1 1 d . . . H19A H 0.7228 1.2429 0.6771 0.045 Uiso 1 1 calc R . . C20 C 0.60188(11) 1.22421(12) 0.66787(8) 0.0343(4) Uani 1 1 d . . . H20A H 0.5893 1.2892 0.6652 0.041 Uiso 1 1 calc R . . C21 C 0.53961(10) 1.15855(12) 0.66451(7) 0.0283(3) Uani 1 1 d . . . C22 C 0.66524(13) 0.93155(14) 0.67882(9) 0.0435(5) Uani 1 1 d U . . H22 H 0.6181 0.8904 0.6681 0.052 Uiso 1 1 calc R A 3 C23 C 0.6972(6) 0.9092(10) 0.7406(4) 0.0418(14) Uani 0.50 1 d PU B 3 H23A H 0.7123 0.8427 0.7425 0.063 Uiso 0.50 1 calc PR B 3 H23B H 0.6555 0.9222 0.7704 0.063 Uiso 0.50 1 calc PR B 3 H23C H 0.7449 0.9480 0.7494 0.063 Uiso 0.50 1 calc PR B 3 C24 C 0.7391(4) 0.9154(4) 0.6319(2) 0.0601(12) Uani 0.50 1 d PU B 3 H24A H 0.7204 0.9301 0.5907 0.090 Uiso 0.50 1 calc PR B 3 H24B H 0.7568 0.8498 0.6338 0.090 Uiso 0.50 1 calc PR B 3 H24C H 0.7844 0.9566 0.6430 0.090 Uiso 0.50 1 calc PR B 3 C23A C 0.7175(6) 0.9045(10) 0.7327(5) 0.0518(18) Uani 0.50 1 d PU B 4 H23D H 0.6966 0.9341 0.7692 0.078 Uiso 0.50 1 calc PR B 4 H23E H 0.7731 0.9256 0.7262 0.078 Uiso 0.50 1 calc PR B 4 H23F H 0.7169 0.8361 0.7375 0.078 Uiso 0.50 1 calc PR B 4 C24A C 0.6881(5) 0.8906(4) 0.6221(3) 0.0720(14) Uani 0.50 1 d PU B 4 H24D H 0.6499 0.9105 0.5902 0.108 Uiso 0.50 1 calc PR B 4 H24E H 0.6872 0.8220 0.6255 0.108 Uiso 0.50 1 calc PR B 4 H24F H 0.7427 0.9114 0.6120 0.108 Uiso 0.50 1 calc PR B 4 C25 C 0.45200(11) 1.18978(15) 0.65821(9) 0.0395(4) Uani 1 1 d . . . H25A H 0.4246 1.1482 0.6277 0.047 Uiso 1 1 calc R . . C26 C 0.40785(12) 1.17944(18) 0.71821(10) 0.0520(5) Uani 1 1 d . . . H26A H 0.4115 1.1142 0.7321 0.078 Uiso 1 1 calc R . . H26B H 0.3509 1.1967 0.7124 0.078 Uiso 1 1 calc R . . H26C H 0.4329 1.2208 0.7486 0.078 Uiso 1 1 calc R . . C27 C 0.44366(13) 1.29167(17) 0.63631(10) 0.0523(5) Uani 1 1 d . . . H27A H 0.4726 1.2994 0.5983 0.078 Uiso 1 1 calc R . . H27B H 0.4667 1.3341 0.6670 0.078 Uiso 1 1 calc R . . H27C H 0.3863 1.3066 0.6297 0.078 Uiso 1 1 calc R . . C28 C 0.04741(8) 0.34407(10) 0.45277(7) 0.0196(3) Uani 1 1 d . . . C29 C 0.07474(11) 0.22745(11) 0.38603(8) 0.0309(4) Uani 1 1 d . . . H29A H 0.0811 0.1946 0.3490 0.037 Uiso 1 1 calc R . . C30 C 0.08702(11) 0.19250(11) 0.44111(8) 0.0318(4) Uani 1 1 d . . . H30A H 0.1045 0.1305 0.4505 0.038 Uiso 1 1 calc R . . C31 C 0.03718(10) 0.38514(11) 0.34268(7) 0.0256(3) Uani 1 1 d . . . C32 C 0.10106(10) 0.44307(13) 0.32453(8) 0.0325(4) Uani 1 1 d . . . C33 C 0.08592(12) 0.50374(14) 0.27642(8) 0.0403(4) Uani 1 1 d . . . H33A H 0.1277 0.5441 0.2631 0.048 Uiso 1 1 calc R . . C34 C 0.01137(12) 0.50645(13) 0.24768(8) 0.0386(4) Uani 1 1 d . . . H34A H 0.0025 0.5480 0.2146 0.046 Uiso 1 1 calc R . . C35 C -0.05044(11) 0.44925(12) 0.26658(8) 0.0318(4) Uani 1 1 d . . . H35A H -0.1014 0.4518 0.2462 0.038 Uiso 1 1 calc R . . C36 C -0.03939(10) 0.38792(11) 0.31497(7) 0.0268(3) Uani 1 1 d . . . C37 C 0.18419(11) 0.43935(15) 0.35488(9) 0.0411(4) Uani 1 1 d U . . H37 H 0.1772 0.4258 0.3989 0.049 Uiso 1 1 calc R C 7 C38 C 0.2330(4) 0.3639(4) 0.3287(3) 0.0443(12) Uani 0.60 1 d PU . 7 H38A H 0.2862 0.3622 0.3489 0.066 Uiso 0.60 1 calc PR . 7 H38B H 0.2396 0.3755 0.2853 0.066 Uiso 0.60 1 calc PR . 7 H38C H 0.2056 0.3035 0.3344 0.066 Uiso 0.60 1 calc PR . 7 C39 C 0.23151(18) 0.5375(2) 0.34862(15) 0.0352(6) Uani 0.60 1 d PU . 7 H39A H 0.1992 0.5879 0.3662 0.053 Uiso 0.60 1 calc PR . 7 H39B H 0.2404 0.5509 0.3057 0.053 Uiso 0.60 1 calc PR . 7 H39C H 0.2837 0.5334 0.3701 0.053 Uiso 0.60 1 calc PR . 7 C38A C 0.2472(7) 0.3829(7) 0.3162(5) 0.0484(17) Uani 0.40 1 d PU . 8 H38D H 0.2206 0.3281 0.2978 0.073 Uiso 0.40 1 calc PR . 8 H38E H 0.2920 0.3619 0.3424 0.073 Uiso 0.40 1 calc PR . 8 H38F H 0.2681 0.4235 0.2842 0.073 Uiso 0.40 1 calc PR . 8 C39A C 0.2111(4) 0.5194(5) 0.3831(4) 0.0682(14) Uani 0.40 1 d PU . 8 H39D H 0.2649 0.5082 0.4009 0.102 Uiso 0.40 1 calc PR . 8 H39E H 0.1736 0.5366 0.4152 0.102 Uiso 0.40 1 calc PR . 8 H39F H 0.2139 0.5705 0.3536 0.102 Uiso 0.40 1 calc PR . 8 C40 C -0.10874(11) 0.32673(14) 0.33581(8) 0.0379(4) Uani 1 1 d . . . H40A H -0.0962 0.3055 0.3781 0.045 Uiso 1 1 calc R . . C41 C -0.11723(18) 0.24034(19) 0.29613(16) 0.0782(9) Uani 1 1 d . . . H41A H -0.1600 0.1999 0.3118 0.117 Uiso 1 1 calc R . . H41B H -0.0660 0.2058 0.2963 0.117 Uiso 1 1 calc R . . H41C H -0.1312 0.2595 0.2547 0.117 Uiso 1 1 calc R . . C42 C -0.18872(14) 0.3791(2) 0.33610(14) 0.0684(7) Uani 1 1 d . . . H42A H -0.2301 0.3393 0.3543 0.103 Uiso 1 1 calc R . . H42B H -0.2051 0.3946 0.2945 0.103 Uiso 1 1 calc R . . H42C H -0.1826 0.4370 0.3597 0.103 Uiso 1 1 calc R . . C43 C 0.09379(10) 0.26019(11) 0.54590(7) 0.0253(3) Uani 1 1 d . . . C44 C 0.16951(10) 0.29659(13) 0.56224(8) 0.0344(4) Uani 1 1 d . . . C45 C 0.19172(11) 0.29368(15) 0.62311(9) 0.0412(4) Uani 1 1 d . . . H45A H 0.2425 0.3189 0.6356 0.049 Uiso 1 1 calc R . . C46 C 0.14184(11) 0.25505(14) 0.66570(8) 0.0377(4) Uani 1 1 d . . . H46A H 0.1584 0.2537 0.7071 0.045 Uiso 1 1 calc R . . C47 C 0.06773(11) 0.21827(13) 0.64831(8) 0.0329(4) Uani 1 1 d . . . H47A H 0.0341 0.1909 0.6779 0.040 Uiso 1 1 calc R . . C48 C 0.04161(10) 0.22076(11) 0.58803(7) 0.0270(3) Uani 1 1 d . . . C49 C 0.22677(11) 0.33608(17) 0.51536(10) 0.0490(5) Uani 1 1 d U . . H49 H 0.1965 0.3557 0.4779 0.059 Uiso 1 1 calc R D 5 C50 C 0.29266(14) 0.26688(19) 0.50073(12) 0.0633(7) Uani 1 1 d U . . H50A H 0.2683 0.2074 0.4875 0.095 Uiso 1 1 calc R . . H50B H 0.3266 0.2561 0.5369 0.095 Uiso 1 1 calc R . . H50C H 0.3259 0.2922 0.4683 0.095 Uiso 1 1 calc R . . C51 C 0.2779(4) 0.4282(4) 0.5465(3) 0.0533(11) Uani 0.50 1 d PU . 5 H51A H 0.2396 0.4774 0.5575 0.080 Uiso 0.50 1 calc PR . 5 H51B H 0.3161 0.4531 0.5171 0.080 Uiso 0.50 1 calc PR . 5 H51C H 0.3077 0.4070 0.5827 0.080 Uiso 0.50 1 calc PR . 5 C51A C 0.2509(3) 0.4285(4) 0.5224(2) 0.0454(10) Uani 0.50 1 d PU . 6 H51D H 0.2037 0.4676 0.5313 0.068 Uiso 0.50 1 calc PR . 6 H51E H 0.2756 0.4505 0.4850 0.068 Uiso 0.50 1 calc PR . 6 H51F H 0.2903 0.4330 0.5558 0.068 Uiso 0.50 1 calc PR . 6 C52 C -0.03984(11) 0.17941(13) 0.56988(8) 0.0337(4) Uani 1 1 d . . . H52A H -0.0553 0.2038 0.5289 0.040 Uiso 1 1 calc R . . C53 C -0.03491(15) 0.07346(16) 0.56662(15) 0.0645(7) Uani 1 1 d . . . H53A H 0.0055 0.0553 0.5369 0.097 Uiso 1 1 calc R . . H53B H -0.0878 0.0480 0.5544 0.097 Uiso 1 1 calc R . . H53C H -0.0193 0.0484 0.6064 0.097 Uiso 1 1 calc R . . C54 C -0.10724(13) 0.20445(18) 0.61385(11) 0.0548(6) Uani 1 1 d . . . H54A H -0.1081 0.2726 0.6202 0.082 Uiso 1 1 calc R . . H54B H -0.0973 0.1727 0.6526 0.082 Uiso 1 1 calc R . . H54C H -0.1595 0.1841 0.5968 0.082 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Al1 0.0402(3) 0.0423(3) 0.0199(2) 0.0016(2) -0.0008(2) -0.0220(2) Al2 0.035(2) 0.0211(11) 0.0199(8) -0.0029(6) -0.0027(8) 0.0096(13) Al2A 0.0370(10) 0.0178(4) 0.0199(4) 0.0006(3) 0.0050(3) 0.0070(5) N1 0.0270(7) 0.0349(7) 0.0193(6) 0.0013(5) -0.0014(5) -0.0107(6) N2 0.0293(7) 0.0329(7) 0.0213(6) 0.0046(5) -0.0010(5) -0.0107(6) N3 0.0332(7) 0.0380(8) 0.0189(6) 0.0019(6) -0.0018(5) -0.0134(6) N4 0.0262(6) 0.0186(6) 0.0207(6) -0.0010(5) 0.0020(5) 0.0039(5) N5 0.0328(7) 0.0218(6) 0.0217(6) -0.0044(5) -0.0007(5) 0.0076(5) N6 0.0384(8) 0.0179(6) 0.0230(7) 0.0009(5) 0.0066(5) 0.0066(5) C1 0.0240(7) 0.0308(8) 0.0220(8) 0.0021(6) -0.0013(6) -0.0073(6) C2 0.0399(9) 0.0384(10) 0.0211(8) 0.0075(7) 0.0016(7) -0.0093(8) C3 0.0423(10) 0.0436(10) 0.0184(8) 0.0049(7) -0.0011(7) -0.0109(8) C4 0.0243(7) 0.0264(8) 0.0226(7) 0.0033(6) 0.0019(6) -0.0077(6) C5 0.0271(8) 0.0277(8) 0.0388(9) 0.0057(7) 0.0057(7) -0.0039(7) C6 0.0406(10) 0.0258(9) 0.0500(11) -0.0057(8) 0.0067(8) -0.0065(7) C7 0.0391(10) 0.0379(10) 0.0451(11) -0.0053(8) -0.0055(8) -0.0150(8) C8 0.0284(8) 0.0361(9) 0.0391(10) 0.0036(8) -0.0051(7) -0.0053(7) C9 0.0264(8) 0.0271(8) 0.0271(8) 0.0038(6) 0.0037(6) -0.0044(6) C10 0.0313(9) 0.0349(10) 0.0676(14) 0.0090(9) 0.0014(9) 0.0032(8) C11 0.0560(13) 0.0505(13) 0.0569(13) 0.0140(10) -0.0037(10) 0.0116(10) C12 0.0566(14) 0.0674(16) 0.0850(19) 0.0230(14) 0.0293(13) 0.0277(12) C13 0.0326(9) 0.0266(9) 0.0462(10) 0.0001(7) 0.0045(8) -0.0022(7) C14 0.0900(19) 0.0462(13) 0.0586(15) 0.0065(11) 0.0000(13) 0.0267(13) C15 0.0905(18) 0.0483(13) 0.0464(13) -0.0029(10) 0.0135(12) 0.0224(12) C16 0.0256(8) 0.0310(8) 0.0176(7) -0.0018(6) -0.0013(6) -0.0053(6) C17 0.0299(8) 0.0322(9) 0.0234(8) -0.0032(6) -0.0035(6) 0.0020(7) C18 0.0232(8) 0.0440(10) 0.0357(9) -0.0024(8) -0.0009(7) -0.0007(7) C19 0.0326(9) 0.0379(10) 0.0406(10) 0.0000(8) -0.0023(7) -0.0110(8) C20 0.0411(10) 0.0266(8) 0.0350(9) -0.0023(7) -0.0042(7) -0.0002(7) C21 0.0273(8) 0.0368(9) 0.0208(7) -0.0042(6) -0.0018(6) 0.0031(7) C22 0.0541(12) 0.0333(9) 0.0427(10) -0.0057(8) -0.0130(9) 0.0118(8) C23 0.049(4) 0.033(2) 0.044(2) 0.009(2) 0.003(2) 0.008(3) C24 0.088(3) 0.049(3) 0.044(2) 0.0003(19) 0.012(2) 0.037(2) C23A 0.063(4) 0.039(2) 0.053(3) 0.002(3) -0.017(3) 0.010(4) C24A 0.112(4) 0.055(3) 0.049(2) -0.006(2) -0.002(3) 0.038(3) C25 0.0285(9) 0.0533(12) 0.0364(10) -0.0081(8) -0.0042(7) 0.0084(8) C26 0.0344(10) 0.0679(15) 0.0542(13) 0.0010(11) 0.0130(9) 0.0093(10) C27 0.0448(11) 0.0636(14) 0.0484(12) 0.0040(10) -0.0034(9) 0.0210(10) C28 0.0181(7) 0.0190(7) 0.0217(7) -0.0005(6) 0.0026(5) -0.0001(5) C29 0.0409(9) 0.0215(8) 0.0302(9) -0.0080(6) 0.0018(7) 0.0063(7) C30 0.0455(10) 0.0167(7) 0.0336(9) -0.0023(6) 0.0081(7) 0.0059(7) C31 0.0341(8) 0.0242(8) 0.0184(7) -0.0041(6) 0.0037(6) 0.0070(6) C32 0.0330(9) 0.0384(9) 0.0262(8) -0.0065(7) 0.0075(7) 0.0021(7) C33 0.0449(11) 0.0444(11) 0.0320(9) 0.0033(8) 0.0097(8) -0.0090(9) C34 0.0533(11) 0.0352(9) 0.0273(9) 0.0074(7) 0.0032(8) -0.0013(8) C35 0.0393(9) 0.0312(9) 0.0249(8) 0.0008(7) -0.0015(7) 0.0040(7) C36 0.0342(9) 0.0248(8) 0.0214(7) -0.0029(6) 0.0016(6) 0.0034(7) C37 0.0316(9) 0.0545(11) 0.0373(10) -0.0038(8) 0.0056(7) -0.0019(8) C38 0.030(2) 0.045(2) 0.058(3) 0.007(2) 0.0101(19) 0.0033(17) C39 0.0278(14) 0.0436(15) 0.0345(16) 0.0018(13) 0.0120(12) -0.0075(12) C38A 0.036(4) 0.062(4) 0.047(4) 0.006(3) 0.013(2) 0.006(3) C39A 0.059(3) 0.064(3) 0.080(3) -0.017(3) -0.014(3) 0.000(2) C40 0.0368(10) 0.0448(11) 0.0319(9) 0.0125(8) -0.0023(7) -0.0045(8) C41 0.0661(17) 0.0490(14) 0.120(3) -0.0159(15) 0.0120(16) -0.0255(13) C42 0.0391(12) 0.0851(19) 0.0815(18) 0.0164(15) 0.0188(12) 0.0031(12) C43 0.0319(8) 0.0192(7) 0.0250(8) 0.0026(6) 0.0040(6) 0.0091(6) C44 0.0269(8) 0.0355(9) 0.0409(10) 0.0112(8) 0.0039(7) 0.0093(7) C45 0.0268(9) 0.0481(11) 0.0484(11) 0.0105(9) -0.0064(8) 0.0024(8) C46 0.0387(10) 0.0434(10) 0.0307(9) 0.0034(8) -0.0072(7) 0.0035(8) C47 0.0377(9) 0.0357(9) 0.0255(8) 0.0037(7) 0.0027(7) -0.0001(7) C48 0.0341(9) 0.0215(8) 0.0254(8) 0.0012(6) 0.0020(6) 0.0022(6) C49 0.0279(9) 0.0666(12) 0.0527(12) 0.0241(10) 0.0034(8) -0.0007(9) C50 0.0495(12) 0.0724(14) 0.0688(15) -0.0279(13) 0.0288(11) -0.0181(11) C51 0.054(3) 0.0382(18) 0.069(3) 0.011(2) 0.019(2) 0.0015(19) C51A 0.035(2) 0.0570(18) 0.044(3) 0.008(2) -0.0018(18) -0.0070(18) C52 0.0393(10) 0.0352(9) 0.0266(8) 0.0049(7) -0.0018(7) -0.0064(7) C53 0.0470(13) 0.0391(12) 0.108(2) -0.0175(13) 0.0049(13) -0.0098(10) C54 0.0371(11) 0.0619(14) 0.0655(15) -0.0051(12) 0.0016(10) 0.0044(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Al1 N1 1.9115(14) 3_676 ? Al1 N1 1.9148(14) . ? Al1 Al1 2.7946(10) 3_676 ? Al1 H1A 1.48(2) . ? Al1 H1B 1.55(2) . ? Al2 N4 1.881(2) 3_566 ? Al2 N4 1.933(2) . ? Al2 Al2 2.801(4) 3_566 ? Al2 H2B 1.50(2) . ? Al2 H2C 1.50(2) . ? Al2 H2E 1.20(2) . ? Al2A N4 1.8982(14) . ? Al2A N4 1.9123(15) 3_566 ? Al2A Al2A 2.7958(17) 3_566 ? Al2A H2B 1.24(4) . ? Al2A H2D 1.50(2) . ? Al2A H2E 1.510(19) . ? N1 C1 1.289(2) . ? N1 Al1 1.9115(14) 3_676 ? N2 C1 1.389(2) . ? N2 C2 1.394(2) . ? N2 C4 1.442(2) . ? N3 C1 1.390(2) . ? N3 C3 1.398(2) . ? N3 C16 1.436(2) . ? N4 C28 1.2904(19) . ? N4 Al2 1.881(2) 3_566 ? N4 Al2A 1.9123(15) 3_566 ? N5 C28 1.3811(19) . ? N5 C29 1.394(2) . ? N5 C31 1.442(2) . ? N6 C28 1.3800(19) . ? N6 C30 1.394(2) . ? N6 C43 1.444(2) . ? C2 C3 1.331(3) . ? C2 H2A 0.9500 . ? C3 H3A 0.9500 . ? C4 C9 1.401(2) . ? C4 C5 1.401(2) . ? C5 C6 1.390(3) . ? C5 C10 1.517(3) . ? C6 C7 1.377(3) . ? C6 H6A 0.9500 . ? C7 C8 1.379(3) . ? C7 H7A 0.9500 . ? C8 C9 1.391(2) . ? C8 H8A 0.9500 . ? C9 C13 1.523(2) . ? C10 C12 1.530(3) . ? C10 C11 1.533(3) . ? C10 H10A 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C15 1.511(3) . ? C13 C14 1.524(3) . ? C13 H13A 1.0000 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.398(2) . ? C16 C21 1.404(2) . ? C17 C18 1.388(3) . ? C17 C22 1.515(2) . ? C18 C19 1.371(3) . ? C18 H18A 0.9500 . ? C19 C20 1.376(3) . ? C19 H19A 0.9500 . ? C20 C21 1.392(2) . ? C20 H20A 0.9500 . ? C21 C25 1.520(2) . ? C22 C24A 1.438(6) . ? C22 C23 1.489(11) . ? C22 C23A 1.509(11) . ? C22 C24 1.631(6) . ? C22 H22 1.0000 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C23A H23D 0.9800 . ? C23A H23E 0.9800 . ? C23A H23F 0.9800 . ? C24A H24D 0.9800 . ? C24A H24E 0.9800 . ? C24A H24F 0.9800 . ? C25 C26 1.532(3) . ? C25 C27 1.535(3) . ? C25 H25A 1.0000 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C29 C30 1.327(2) . ? C29 H29A 0.9500 . ? C30 H30A 0.9500 . ? C31 C36 1.398(2) . ? C31 C32 1.404(2) . ? C32 C33 1.389(3) . ? C32 C37 1.520(3) . ? C33 C34 1.378(3) . ? C33 H33A 0.9500 . ? C34 C35 1.378(3) . ? C34 H34A 0.9500 . ? C35 C36 1.390(2) . ? C35 H35A 0.9500 . ? C36 C40 1.518(2) . ? C37 C39A 1.370(7) . ? C37 C38 1.469(7) . ? C37 C38A 1.579(11) . ? C37 C39 1.609(4) . ? C37 H37 1.0000 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C38A H38D 0.9800 . ? C38A H38E 0.9800 . ? C38A H38F 0.9800 . ? C39A H39D 0.9800 . ? C39A H39E 0.9800 . ? C39A H39F 0.9800 . ? C40 C41 1.516(3) . ? C40 C42 1.518(3) . ? C40 H40A 1.0000 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 C44 1.397(2) . ? C43 C48 1.398(2) . ? C44 C45 1.389(3) . ? C44 C49 1.523(3) . ? C45 C46 1.377(3) . ? C45 H45A 0.9500 . ? C46 C47 1.381(3) . ? C46 H46A 0.9500 . ? C47 C48 1.394(2) . ? C47 H47A 0.9500 . ? C48 C52 1.518(2) . ? C49 C51A 1.384(6) . ? C49 C50 1.508(3) . ? C49 C51 1.699(6) . ? C49 H49 1.0000 . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C51A H51D 0.9800 . ? C51A H51E 0.9800 . ? C51A H51F 0.9800 . ? C52 C53 1.513(3) . ? C52 C54 1.533(3) . ? C52 H52A 1.0000 . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 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 N1 Al1 N1 86.17(6) 3_676 . ? N1 Al1 Al1 43.13(4) 3_676 3_676 ? N1 Al1 Al1 43.04(4) . 3_676 ? N1 Al1 H1A 111.3(8) 3_676 . ? N1 Al1 H1A 113.6(8) . . ? Al1 Al1 H1A 121.5(8) 3_676 . ? N1 Al1 H1B 112.1(8) 3_676 . ? N1 Al1 H1B 111.6(8) . . ? Al1 Al1 H1B 120.6(8) 3_676 . ? H1A Al1 H1B 117.9(11) . . ? N4 Al2 N4 85.49(10) 3_566 . ? N4 Al2 Al2 43.47(6) 3_566 3_566 ? N4 Al2 Al2 42.02(7) . 3_566 ? N4 Al2 H2B 119(3) 3_566 . ? N4 Al2 H2B 116(2) . . ? Al2 Al2 H2B 129(3) 3_566 . ? N4 Al2 H2C 111(3) 3_566 . ? N4 Al2 H2C 115(3) . . ? Al2 Al2 H2C 122(3) 3_566 . ? H2B Al2 H2C 109(4) . . ? N4 Al2 H2E 141.2(13) 3_566 . ? N4 Al2 H2E 131.6(13) . . ? Al2 Al2 H2E 169.0(13) 3_566 . ? H2B Al2 H2E 41(2) . . ? H2C Al2 H2E 68(3) . . ? N4 Al2A N4 85.61(6) . 3_566 ? N4 Al2A Al2A 43.00(4) . 3_566 ? N4 Al2A Al2A 42.61(4) 3_566 3_566 ? N4 Al2A H2B 136(3) . . ? N4 Al2A H2B 135(3) 3_566 . ? Al2A Al2A H2B 167(3) 3_566 . ? N4 Al2A H2D 108.8(10) . . ? N4 Al2A H2D 109.3(10) 3_566 . ? Al2A Al2A H2D 116.4(10) 3_566 . ? H2B Al2A H2D 77(3) . . ? N4 Al2A H2E 114.8(10) . . ? N4 Al2A H2E 116.6(11) 3_566 . ? Al2A Al2A H2E 126.2(11) 3_566 . ? H2B Al2A H2E 41(3) . . ? H2D Al2A H2E 117.4(15) . . ? C1 N1 Al1 134.00(11) . 3_676 ? C1 N1 Al1 131.71(12) . . ? Al1 N1 Al1 93.83(6) 3_676 . ? C1 N2 C2 110.21(13) . . ? C1 N2 C4 125.74(13) . . ? C2 N2 C4 123.79(13) . . ? C1 N3 C3 109.84(13) . . ? C1 N3 C16 125.69(13) . . ? C3 N3 C16 124.03(13) . . ? C28 N4 Al2 129.97(13) . 3_566 ? C28 N4 Al2A 130.45(11) . . ? Al2 N4 Al2A 90.64(8) 3_566 . ? C28 N4 Al2A 134.58(11) . 3_566 ? Al2 N4 Al2A 23.77(12) 3_566 3_566 ? Al2A N4 Al2A 94.39(6) . 3_566 ? C28 N4 Al2 134.93(12) . . ? Al2 N4 Al2 94.51(10) 3_566 . ? Al2A N4 Al2 23.53(12) . . ? Al2A N4 Al2 88.65(8) 3_566 . ? C28 N5 C29 109.86(13) . . ? C28 N5 C31 125.06(12) . . ? C29 N5 C31 124.96(13) . . ? C28 N6 C30 109.92(13) . . ? C28 N6 C43 123.61(13) . . ? C30 N6 C43 124.23(13) . . ? N1 C1 N2 128.04(14) . . ? N1 C1 N3 127.91(14) . . ? N2 C1 N3 104.05(13) . . ? C3 C2 N2 107.80(14) . . ? C3 C2 H2A 126.1 . . ? N2 C2 H2A 126.1 . . ? C2 C3 N3 108.06(14) . . ? C2 C3 H3A 126.0 . . ? N3 C3 H3A 126.0 . . ? C9 C4 C5 122.71(15) . . ? C9 C4 N2 118.33(14) . . ? C5 C4 N2 118.93(15) . . ? C6 C5 C4 117.20(16) . . ? C6 C5 C10 120.04(17) . . ? C4 C5 C10 122.71(16) . . ? C7 C6 C5 121.33(17) . . ? C7 C6 H6A 119.3 . . ? C5 C6 H6A 119.3 . . ? C6 C7 C8 120.30(17) . . ? C6 C7 H7A 119.9 . . ? C8 C7 H7A 119.9 . . ? C7 C8 C9 121.22(17) . . ? C7 C8 H8A 119.4 . . ? C9 C8 H8A 119.4 . . ? C8 C9 C4 117.23(15) . . ? C8 C9 C13 121.13(15) . . ? C4 C9 C13 121.64(15) . . ? C5 C10 C12 112.89(19) . . ? C5 C10 C11 110.15(16) . . ? C12 C10 C11 109.11(18) . . ? C5 C10 H10A 108.2 . . ? C12 C10 H10A 108.2 . . ? C11 C10 H10A 108.2 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C15 C13 C9 112.46(16) . . ? C15 C13 C14 108.34(18) . . ? C9 C13 C14 112.91(17) . . ? C15 C13 H13A 107.6 . . ? C9 C13 H13A 107.6 . . ? C14 C13 H13A 107.6 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C17 C16 C21 122.35(15) . . ? C17 C16 N3 118.39(15) . . ? C21 C16 N3 119.25(14) . . ? C18 C17 C16 117.60(16) . . ? C18 C17 C22 120.12(16) . . ? C16 C17 C22 122.27(16) . . ? C19 C18 C17 121.21(16) . . ? C19 C18 H18A 119.4 . . ? C17 C18 H18A 119.4 . . ? C18 C19 C20 120.43(17) . . ? C18 C19 H19A 119.8 . . ? C20 C19 H19A 119.8 . . ? C19 C20 C21 121.28(17) . . ? C19 C20 H20A 119.4 . . ? C21 C20 H20A 119.4 . . ? C20 C21 C16 117.11(15) . . ? C20 C21 C25 120.78(16) . . ? C16 C21 C25 122.11(16) . . ? C24A C22 C23 128.1(5) . . ? C24A C22 C23A 115.3(5) . . ? C23 C22 C23A 14.8(6) . . ? C24A C22 C17 114.7(3) . . ? C23 C22 C17 109.9(5) . . ? C23A C22 C17 115.5(6) . . ? C24A C22 C24 34.8(3) . . ? C23 C22 C24 107.1(4) . . ? C23A C22 C24 92.3(4) . . ? C17 C22 C24 107.3(2) . . ? C24A C22 H22 76.8 . . ? C23 C22 H22 110.8 . . ? C23A C22 H22 118.1 . . ? C17 C22 H22 110.8 . . ? C24 C22 H22 110.8 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C22 C23A H23D 109.5 . . ? C22 C23A H23E 109.5 . . ? H23D C23A H23E 109.5 . . ? C22 C23A H23F 109.5 . . ? H23D C23A H23F 109.5 . . ? H23E C23A H23F 109.5 . . ? C22 C24A H24D 109.5 . . ? C22 C24A H24E 109.5 . . ? H24D C24A H24E 109.5 . . ? C22 C24A H24F 109.5 . . ? H24D C24A H24F 109.5 . . ? H24E C24A H24F 109.5 . . ? C21 C25 C26 111.14(16) . . ? C21 C25 C27 112.69(17) . . ? C26 C25 C27 108.80(17) . . ? C21 C25 H25A 108.0 . . ? C26 C25 H25A 108.0 . . ? C27 C25 H25A 108.0 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? N4 C28 N6 127.62(14) . . ? N4 C28 N5 127.91(14) . . ? N6 C28 N5 104.47(12) . . ? C30 C29 N5 107.89(14) . . ? C30 C29 H29A 126.1 . . ? N5 C29 H29A 126.1 . . ? C29 C30 N6 107.85(14) . . ? C29 C30 H30A 126.1 . . ? N6 C30 H30A 126.1 . . ? C36 C31 C32 122.60(15) . . ? C36 C31 N5 118.68(14) . . ? C32 C31 N5 118.71(15) . . ? C33 C32 C31 117.20(16) . . ? C33 C32 C37 120.59(17) . . ? C31 C32 C37 122.19(16) . . ? C34 C33 C32 121.21(17) . . ? C34 C33 H33A 119.4 . . ? C32 C33 H33A 119.4 . . ? C35 C34 C33 120.45(17) . . ? C35 C34 H34A 119.8 . . ? C33 C34 H34A 119.8 . . ? C34 C35 C36 121.07(17) . . ? C34 C35 H35A 119.5 . . ? C36 C35 H35A 119.5 . . ? C35 C36 C31 117.43(16) . . ? C35 C36 C40 120.25(15) . . ? C31 C36 C40 122.31(15) . . ? C39A C37 C38 127.7(4) . . ? C39A C37 C32 117.1(3) . . ? C38 C37 C32 110.5(3) . . ? C39A C37 C38A 117.3(5) . . ? C38 C37 C38A 16.7(4) . . ? C32 C37 C38A 112.3(5) . . ? C39A C37 C39 33.1(4) . . ? C38 C37 C39 109.3(3) . . ? C32 C37 C39 111.68(19) . . ? C38A C37 C39 94.0(4) . . ? C39A C37 H37 76.1 . . ? C38 C37 H37 108.4 . . ? C32 C37 H37 108.4 . . ? C38A C37 H37 121.2 . . ? C39 C37 H37 108.4 . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C37 C39 H39A 109.5 . . ? C37 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C37 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C37 C38A H38D 109.5 . . ? C37 C38A H38E 109.5 . . ? H38D C38A H38E 109.5 . . ? C37 C38A H38F 109.5 . . ? H38D C38A H38F 109.5 . . ? H38E C38A H38F 109.5 . . ? C37 C39A H39D 109.5 . . ? C37 C39A H39E 109.5 . . ? H39D C39A H39E 109.5 . . ? C37 C39A H39F 109.5 . . ? H39D C39A H39F 109.5 . . ? H39E C39A H39F 109.5 . . ? C41 C40 C36 110.69(17) . . ? C41 C40 C42 109.2(2) . . ? C36 C40 C42 112.49(17) . . ? C41 C40 H40A 108.1 . . ? C36 C40 H40A 108.1 . . ? C42 C40 H40A 108.1 . . ? C40 C41 H41A 109.5 . . ? C40 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C40 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C40 C42 H42A 109.5 . . ? C40 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C40 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C44 C43 C48 122.54(15) . . ? C44 C43 N6 118.08(14) . . ? C48 C43 N6 119.38(15) . . ? C45 C44 C43 117.40(16) . . ? C45 C44 C49 120.82(17) . . ? C43 C44 C49 121.76(17) . . ? C46 C45 C44 121.48(17) . . ? C46 C45 H45A 119.3 . . ? C44 C45 H45A 119.3 . . ? C45 C46 C47 120.05(17) . . ? C45 C46 H46A 120.0 . . ? C47 C46 H46A 120.0 . . ? C46 C47 C48 121.01(16) . . ? C46 C47 H47A 119.5 . . ? C48 C47 H47A 119.5 . . ? C47 C48 C43 117.51(16) . . ? C47 C48 C52 120.12(15) . . ? C43 C48 C52 122.36(15) . . ? C51A C49 C50 116.0(3) . . ? C51A C49 C44 117.2(3) . . ? C50 C49 C44 111.39(18) . . ? C51A C49 C51 23.1(2) . . ? C50 C49 C51 103.5(2) . . ? C44 C49 C51 108.7(3) . . ? C51A C49 H49 88.0 . . ? C50 C49 H49 111.0 . . ? C44 C49 H49 111.0 . . ? C51 C49 H49 111.0 . . ? C49 C50 H50A 109.5 . . ? C49 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C49 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C49 C51 H51A 109.5 . . ? C49 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C49 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C49 C51A H51D 109.5 . . ? C49 C51A H51E 109.5 . . ? H51D C51A H51E 109.5 . . ? C49 C51A H51F 109.5 . . ? H51D C51A H51F 109.5 . . ? H51E C51A H51F 109.5 . . ? C53 C52 C48 110.56(16) . . ? C53 C52 C54 107.61(18) . . ? C48 C52 C54 113.21(16) . . ? C53 C52 H52A 108.4 . . ? C48 C52 H52A 108.4 . . ? C54 C52 H52A 108.4 . . ? C52 C53 H53A 109.5 . . ? C52 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C52 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C52 C54 H54A 109.5 . . ? C52 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C52 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 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 N1 Al1 N1 C1 -172.9(2) 3_676 . . . ? Al1 Al1 N1 C1 -172.9(2) 3_676 . . . ? N1 Al1 N1 Al1 0.0 3_676 . . 3_676 ? N4 Al2A N4 C28 -172.11(17) 3_566 . . . ? Al2A Al2A N4 C28 -172.11(17) 3_566 . . . ? N4 Al2A N4 Al2 -23.50(12) 3_566 . . 3_566 ? Al2A Al2A N4 Al2 -23.50(13) 3_566 . . 3_566 ? N4 Al2A N4 Al2A 0.0 3_566 . . 3_566 ? N4 Al2A N4 Al2 76.38(15) 3_566 . . . ? Al2A Al2A N4 Al2 76.38(15) 3_566 . . . ? N4 Al2 N4 C28 -171.43(18) 3_566 . . . ? Al2 Al2 N4 C28 -171.43(18) 3_566 . . . ? N4 Al2 N4 Al2 0.0 3_566 . . 3_566 ? N4 Al2 N4 Al2A -81.2(2) 3_566 . . . ? Al2 Al2 N4 Al2A -81.2(2) 3_566 . . . ? N4 Al2 N4 Al2A 23.06(11) 3_566 . . 3_566 ? Al2 Al2 N4 Al2A 23.06(11) 3_566 . . 3_566 ? Al1 N1 C1 N2 179.34(13) 3_676 . . . ? Al1 N1 C1 N2 -10.6(3) . . . . ? Al1 N1 C1 N3 -0.7(3) 3_676 . . . ? Al1 N1 C1 N3 169.39(13) . . . . ? C2 N2 C1 N1 178.06(17) . . . . ? C4 N2 C1 N1 -7.7(3) . . . . ? C2 N2 C1 N3 -1.92(19) . . . . ? C4 N2 C1 N3 172.35(15) . . . . ? C3 N3 C1 N1 -177.64(17) . . . . ? C16 N3 C1 N1 -5.0(3) . . . . ? C3 N3 C1 N2 2.34(19) . . . . ? C16 N3 C1 N2 174.94(15) . . . . ? C1 N2 C2 C3 0.8(2) . . . . ? C4 N2 C2 C3 -173.61(16) . . . . ? N2 C2 C3 N3 0.7(2) . . . . ? C1 N3 C3 C2 -2.0(2) . . . . ? C16 N3 C3 C2 -174.71(16) . . . . ? C1 N2 C4 C9 -76.7(2) . . . . ? C2 N2 C4 C9 96.8(2) . . . . ? C1 N2 C4 C5 105.34(19) . . . . ? C2 N2 C4 C5 -81.1(2) . . . . ? C9 C4 C5 C6 1.0(2) . . . . ? N2 C4 C5 C6 178.87(15) . . . . ? C9 C4 C5 C10 -176.22(16) . . . . ? N2 C4 C5 C10 1.7(2) . . . . ? C4 C5 C6 C7 -1.2(3) . . . . ? C10 C5 C6 C7 176.08(18) . . . . ? C5 C6 C7 C8 0.3(3) . . . . ? C6 C7 C8 C9 0.9(3) . . . . ? C7 C8 C9 C4 -1.1(3) . . . . ? C7 C8 C9 C13 178.45(17) . . . . ? C5 C4 C9 C8 0.1(2) . . . . ? N2 C4 C9 C8 -177.76(14) . . . . ? C5 C4 C9 C13 -179.41(15) . . . . ? N2 C4 C9 C13 2.7(2) . . . . ? C6 C5 C10 C12 46.7(3) . . . . ? C4 C5 C10 C12 -136.18(19) . . . . ? C6 C5 C10 C11 -75.6(2) . . . . ? C4 C5 C10 C11 101.6(2) . . . . ? C8 C9 C13 C15 98.0(2) . . . . ? C4 C9 C13 C15 -82.5(2) . . . . ? C8 C9 C13 C14 -25.0(2) . . . . ? C4 C9 C13 C14 154.56(18) . . . . ? C1 N3 C16 C17 -95.6(2) . . . . ? C3 N3 C16 C17 76.0(2) . . . . ? C1 N3 C16 C21 85.4(2) . . . . ? C3 N3 C16 C21 -103.0(2) . . . . ? C21 C16 C17 C18 -1.0(2) . . . . ? N3 C16 C17 C18 -179.96(14) . . . . ? C21 C16 C17 C22 179.81(16) . . . . ? N3 C16 C17 C22 0.8(2) . . . . ? C16 C17 C18 C19 -0.2(3) . . . . ? C22 C17 C18 C19 179.03(17) . . . . ? C17 C18 C19 C20 0.7(3) . . . . ? C18 C19 C20 C21 -0.1(3) . . . . ? C19 C20 C21 C16 -1.0(3) . . . . ? C19 C20 C21 C25 178.52(17) . . . . ? C17 C16 C21 C20 1.6(2) . . . . ? N3 C16 C21 C20 -179.44(14) . . . . ? C17 C16 C21 C25 -177.99(15) . . . . ? N3 C16 C21 C25 1.0(2) . . . . ? C18 C17 C22 C24A -85.1(4) . . . . ? C16 C17 C22 C24A 94.1(4) . . . . ? C18 C17 C22 C23 67.5(4) . . . . ? C16 C17 C22 C23 -113.3(4) . . . . ? C18 C17 C22 C23A 52.6(5) . . . . ? C16 C17 C22 C23A -128.2(5) . . . . ? C18 C17 C22 C24 -48.6(3) . . . . ? C16 C17 C22 C24 130.6(3) . . . . ? C20 C21 C25 C26 -104.2(2) . . . . ? C16 C21 C25 C26 75.3(2) . . . . ? C20 C21 C25 C27 18.2(2) . . . . ? C16 C21 C25 C27 -162.28(16) . . . . ? Al2 N4 C28 N6 -156.0(3) 3_566 . . . ? Al2A N4 C28 N6 -18.8(3) . . . . ? Al2A N4 C28 N6 172.27(16) 3_566 . . . ? Al2 N4 C28 N6 12.8(4) . . . . ? Al2 N4 C28 N5 24.0(3) 3_566 . . . ? Al2A N4 C28 N5 161.19(16) . . . . ? Al2A N4 C28 N5 -7.7(3) 3_566 . . . ? Al2 N4 C28 N5 -167.2(3) . . . . ? C30 N6 C28 N4 -179.47(15) . . . . ? C43 N6 C28 N4 -15.9(2) . . . . ? C30 N6 C28 N5 0.54(17) . . . . ? C43 N6 C28 N5 164.15(14) . . . . ? C29 N5 C28 N4 -179.91(15) . . . . ? C31 N5 C28 N4 3.9(3) . . . . ? C29 N5 C28 N6 0.09(17) . . . . ? C31 N5 C28 N6 -176.13(14) . . . . ? C28 N5 C29 C30 -0.7(2) . . . . ? C31 N5 C29 C30 175.52(16) . . . . ? N5 C29 C30 N6 1.0(2) . . . . ? C28 N6 C30 C29 -1.0(2) . . . . ? C43 N6 C30 C29 -164.49(16) . . . . ? C28 N5 C31 C36 -97.14(18) . . . . ? C29 N5 C31 C36 87.2(2) . . . . ? C28 N5 C31 C32 82.34(19) . . . . ? C29 N5 C31 C32 -93.3(2) . . . . ? C36 C31 C32 C33 -1.0(2) . . . . ? N5 C31 C32 C33 179.57(15) . . . . ? C36 C31 C32 C37 -179.86(15) . . . . ? N5 C31 C32 C37 0.7(2) . . . . ? C31 C32 C33 C34 -0.3(3) . . . . ? C37 C32 C33 C34 178.63(17) . . . . ? C32 C33 C34 C35 0.6(3) . . . . ? C33 C34 C35 C36 0.2(3) . . . . ? C34 C35 C36 C31 -1.4(2) . . . . ? C34 C35 C36 C40 178.90(17) . . . . ? C32 C31 C36 C35 1.8(2) . . . . ? N5 C31 C36 C35 -178.75(14) . . . . ? C32 C31 C36 C40 -178.51(16) . . . . ? N5 C31 C36 C40 1.0(2) . . . . ? C33 C32 C37 C39A 63.0(5) . . . . ? C31 C32 C37 C39A -118.2(5) . . . . ? C33 C32 C37 C38 -94.8(3) . . . . ? C31 C32 C37 C38 84.0(3) . . . . ? C33 C32 C37 C38A -77.0(4) . . . . ? C31 C32 C37 C38A 101.8(4) . . . . ? C33 C32 C37 C39 27.0(3) . . . . ? C31 C32 C37 C39 -154.11(19) . . . . ? C35 C36 C40 C41 81.3(2) . . . . ? C31 C36 C40 C41 -98.4(2) . . . . ? C35 C36 C40 C42 -41.2(2) . . . . ? C31 C36 C40 C42 139.12(19) . . . . ? C28 N6 C43 C44 -72.9(2) . . . . ? C30 N6 C43 C44 88.4(2) . . . . ? C28 N6 C43 C48 107.80(18) . . . . ? C30 N6 C43 C48 -90.9(2) . . . . ? C48 C43 C44 C45 -0.9(3) . . . . ? N6 C43 C44 C45 179.86(15) . . . . ? C48 C43 C44 C49 177.77(17) . . . . ? N6 C43 C44 C49 -1.5(2) . . . . ? C43 C44 C45 C46 1.1(3) . . . . ? C49 C44 C45 C46 -177.58(19) . . . . ? C44 C45 C46 C47 -0.2(3) . . . . ? C45 C46 C47 C48 -1.0(3) . . . . ? C46 C47 C48 C43 1.2(3) . . . . ? C46 C47 C48 C52 179.64(17) . . . . ? C44 C43 C48 C47 -0.2(2) . . . . ? N6 C43 C48 C47 179.03(14) . . . . ? C44 C43 C48 C52 -178.66(16) . . . . ? N6 C43 C48 C52 0.6(2) . . . . ? C45 C44 C49 C51A -59.8(3) . . . . ? C43 C44 C49 C51A 121.6(3) . . . . ? C45 C44 C49 C50 77.1(3) . . . . ? C43 C44 C49 C50 -101.5(2) . . . . ? C45 C44 C49 C51 -36.4(3) . . . . ? C43 C44 C49 C51 145.0(3) . . . . ? C47 C48 C52 C53 -77.7(2) . . . . ? C43 C48 C52 C53 100.7(2) . . . . ? C47 C48 C52 C54 43.1(2) . . . . ? C43 C48 C52 C54 -138.51(18) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 67.50 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.755 _refine_diff_density_min -0.659 _refine_diff_density_rms 0.043 _database_code_depnum_ccdc_archive 'CCDC 962234' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_cu-216 _audit_creation_method ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) ; _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C56 H74 Al2 F6 N6 O6 S2, 3(C4 H8 O)' _chemical_formula_sum 'C68 H98 Al2 F6 N6 O9 S2' _chemical_formula_weight 1375.60 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Al Al 0.2130 0.2455 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 26.3370(8) _cell_length_b 12.1672(3) _cell_length_c 25.4631(8) _cell_angle_alpha 90.00 _cell_angle_beta 118.280(4) _cell_angle_gamma 90.00 _cell_volume 7185.7(4) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 11372 _cell_measurement_theta_min 4.1250 _cell_measurement_theta_max 73.7750 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.52 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.272 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2928 _exptl_absorpt_coefficient_mu 1.521 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5052 _exptl_absorpt_correction_T_max 0.7212 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'SuperNova (Cu) X-ray Source' _diffrn_radiation_monochromator mirror _diffrn_measurement_device_type 'SuperNova, Single source at offset, Atlas' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27594 _diffrn_reflns_av_R_equivalents 0.0355 _diffrn_reflns_av_sigmaI/netI 0.0440 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 3.47 _diffrn_reflns_theta_max 67.50 _reflns_number_total 12943 _reflns_number_gt 9958 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) ; _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^)+(0.0700P)^2^+10.0000P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12943 _refine_ls_number_parameters 1022 _refine_ls_number_restraints 618 _refine_ls_R_factor_all 0.1129 _refine_ls_R_factor_gt 0.0928 _refine_ls_wR_factor_ref 0.2386 _refine_ls_wR_factor_gt 0.2238 _refine_ls_goodness_of_fit_ref 1.372 _refine_ls_restrained_S_all 1.459 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Al1 Al 0.24757(5) 0.29848(13) 0.33282(6) 0.0431(3) Uani 1 1 d . . . H1 H 0.253(2) 0.253(4) 0.365(2) 0.052 Uiso 1 1 d . . . Al2 Al 0.22820(5) 0.21466(14) 0.22820(5) 0.0432(4) Uani 1 1 d . A . H2 H 0.214(2) 0.105(4) 0.194(2) 0.052 Uiso 1 1 d . . . C55 C 0.2545(2) 0.6123(4) 0.3933(3) 0.0546(8) Uani 1 1 d U . . S1 S 0.21680(12) 0.54881(17) 0.31985(11) 0.0462(5) Uani 0.80 1 d PU A 1 O1 O 0.25494(18) 0.4530(3) 0.3266(2) 0.0525(9) Uani 0.80 1 d PU A 1 O2 O 0.2191(2) 0.6303(4) 0.2816(2) 0.0582(10) Uani 0.80 1 d PU A 1 O3 O 0.1623(3) 0.5145(8) 0.3139(3) 0.0521(14) Uani 0.80 1 d PU A 1 F1 F 0.2243(3) 0.6944(4) 0.3977(2) 0.0691(12) Uani 0.80 1 d PU A 1 F2 F 0.3043(3) 0.6549(5) 0.4003(3) 0.0612(13) Uani 0.80 1 d PU A 1 F3 F 0.2653(2) 0.5403(4) 0.4368(2) 0.0690(13) Uani 0.80 1 d PU A 1 S1A S 0.2197(6) 0.5238(9) 0.3329(6) 0.0520(12) Uani 0.20 1 d PU A 2 O1A O 0.2514(7) 0.4186(14) 0.3616(9) 0.0502(17) Uani 0.20 1 d PU A 2 O2A O 0.2372(8) 0.5778(17) 0.2896(9) 0.0548(18) Uani 0.20 1 d PU A 2 O3A O 0.1622(15) 0.522(3) 0.3275(15) 0.052(2) Uani 0.20 1 d PU A 2 F1A F 0.2218(11) 0.7116(18) 0.3739(10) 0.066(3) Uani 0.20 1 d PU A 2 F2A F 0.3104(14) 0.632(3) 0.4128(15) 0.061(2) Uani 0.20 1 d PU A 2 F3A F 0.2485(9) 0.5717(17) 0.4403(10) 0.061(2) Uani 0.20 1 d PU A 2 S2 S 0.26319(7) 0.35838(15) 0.15035(7) 0.0355(4) Uani 0.60 1 d PDU A 3 C56 C 0.2352(3) 0.4975(8) 0.1407(4) 0.0593(10) Uani 0.60 1 d PDU A 3 O4 O 0.2273(2) 0.2969(5) 0.1708(2) 0.0477(10) Uani 0.60 1 d PDU A 3 O5 O 0.2555(3) 0.3254(6) 0.0938(3) 0.0601(12) Uani 0.60 1 d PDU A 3 O6 O 0.3211(3) 0.3615(9) 0.1945(4) 0.0511(15) Uani 0.60 1 d PDU A 3 F4 F 0.1838(3) 0.5082(6) 0.0972(3) 0.0787(15) Uani 0.60 1 d PDU A 3 F5 F 0.2701(3) 0.5658(5) 0.1347(3) 0.0785(13) Uani 0.60 1 d PDU A 3 F6 F 0.2304(3) 0.5263(6) 0.1895(3) 0.0773(12) Uani 0.60 1 d PDU A 3 S2A S 0.27025(16) 0.4309(3) 0.18199(16) 0.0633(7) Uani 0.40 1 d PDU A 4 C56A C 0.2377(5) 0.4098(10) 0.1022(5) 0.0614(11) Uani 0.40 1 d PDU A 4 O4A O 0.2289(4) 0.3660(9) 0.1928(4) 0.0610(12) Uani 0.40 1 d PDU A 4 O5A O 0.2644(5) 0.5531(8) 0.1803(5) 0.0746(17) Uani 0.40 1 d PDU A 4 O6A O 0.3251(6) 0.3770(14) 0.2094(5) 0.0523(18) Uani 0.40 1 d PDU A 4 F4A F 0.1925(4) 0.4763(9) 0.0741(4) 0.082(2) Uani 0.40 1 d PDU A 4 F5A F 0.2772(4) 0.4164(9) 0.0845(4) 0.0828(16) Uani 0.40 1 d PDU A 4 F6A F 0.2182(4) 0.3095(7) 0.0876(3) 0.0660(15) Uani 0.40 1 d PDU A 4 N1 N 0.18282(13) 0.2578(3) 0.26242(14) 0.0293(7) Uani 1 1 d . A . N2 N 0.10414(13) 0.2103(3) 0.28182(13) 0.0278(7) Uani 1 1 d . A . N3 N 0.08119(13) 0.2666(3) 0.19226(13) 0.0295(7) Uani 1 1 d . A . N4 N 0.29274(13) 0.2380(3) 0.30255(14) 0.0293(7) Uani 1 1 d . A . N5 N 0.39476(14) 0.2670(3) 0.36621(15) 0.0338(7) Uani 1 1 d . A . N6 N 0.36969(13) 0.1302(3) 0.30290(14) 0.0315(7) Uani 1 1 d . A . C1 C 0.12730(15) 0.2465(3) 0.24653(16) 0.0260(7) Uani 1 1 d . . . C2 C 0.04409(16) 0.2095(4) 0.24830(17) 0.0329(9) Uani 1 1 d . . . H2B H 0.0179 0.1879 0.2622 0.039 Uiso 1 1 calc R A . C3 C 0.02980(16) 0.2443(4) 0.19347(17) 0.0336(9) Uani 1 1 d . A . H3B H -0.0081 0.2523 0.1613 0.040 Uiso 1 1 calc R . . C4 C 0.13298(16) 0.1448(3) 0.33531(16) 0.0294(8) Uani 1 1 d . . . C5 C 0.14895(17) 0.1941(4) 0.39100(17) 0.0335(9) Uani 1 1 d . A . C6 C 0.1740(2) 0.1253(4) 0.44072(19) 0.0421(10) Uani 1 1 d . . . H6A H 0.1858 0.1553 0.4792 0.050 Uiso 1 1 calc R A . C7 C 0.1819(2) 0.0149(4) 0.4351(2) 0.0461(11) Uani 1 1 d . A . H7A H 0.1996 -0.0298 0.4698 0.055 Uiso 1 1 calc R . . C8 C 0.1644(2) -0.0313(4) 0.3800(2) 0.0415(10) Uani 1 1 d . . . H8A H 0.1697 -0.1078 0.3769 0.050 Uiso 1 1 calc R A . C9 C 0.13910(17) 0.0328(3) 0.32866(18) 0.0335(9) Uani 1 1 d . A . C10 C 0.13776(19) 0.3139(4) 0.39666(18) 0.0386(10) Uani 1 1 d . . . H10A H 0.1402 0.3547 0.3638 0.046 Uiso 1 1 calc R A . C11 C 0.0769(2) 0.3297(5) 0.3888(2) 0.0565(13) Uani 1 1 d . A . H11A H 0.0486 0.3034 0.3493 0.085 Uiso 1 1 calc R . . H11B H 0.0703 0.4078 0.3926 0.085 Uiso 1 1 calc R . . H11C H 0.0729 0.2879 0.4195 0.085 Uiso 1 1 calc R . . C12 C 0.1813(2) 0.3648(4) 0.4557(2) 0.0515(12) Uani 1 1 d . A . H12A H 0.2203 0.3538 0.4613 0.077 Uiso 1 1 calc R . . H12B H 0.1778 0.3296 0.4885 0.077 Uiso 1 1 calc R . . H12C H 0.1736 0.4437 0.4554 0.077 Uiso 1 1 calc R . . C13 C 0.11720(18) -0.0218(4) 0.26790(19) 0.0377(9) Uani 1 1 d . . . H13A H 0.1009 0.0369 0.2368 0.045 Uiso 1 1 calc R A . C14 C 0.0688(3) -0.1036(6) 0.2562(3) 0.0681(17) Uani 1 1 d . A . H14A H 0.0370 -0.0653 0.2579 0.102 Uiso 1 1 calc R . . H14B H 0.0835 -0.1616 0.2865 0.102 Uiso 1 1 calc R . . H14C H 0.0551 -0.1364 0.2166 0.102 Uiso 1 1 calc R . . C15 C 0.1651(2) -0.0796(5) 0.2610(2) 0.0529(12) Uani 1 1 d . A . H15A H 0.1956 -0.0267 0.2675 0.079 Uiso 1 1 calc R . . H15B H 0.1494 -0.1102 0.2207 0.079 Uiso 1 1 calc R . . H15C H 0.1812 -0.1390 0.2903 0.079 Uiso 1 1 calc R . . C16 C 0.08059(16) 0.3048(4) 0.13789(16) 0.0333(9) Uani 1 1 d . . . C17 C 0.0723(2) 0.4154(4) 0.12450(19) 0.0447(11) Uani 1 1 d . A . C18 C 0.0662(3) 0.4488(5) 0.0689(2) 0.0606(14) Uani 1 1 d . . . H18A H 0.0605 0.5243 0.0581 0.073 Uiso 1 1 calc R A . C19 C 0.0684(3) 0.3726(5) 0.0302(2) 0.0604(14) Uani 1 1 d . A . H19A H 0.0644 0.3963 -0.0070 0.072 Uiso 1 1 calc R . . C20 C 0.0760(2) 0.2639(5) 0.0442(2) 0.0530(13) Uani 1 1 d . . . H20A H 0.0774 0.2135 0.0164 0.064 Uiso 1 1 calc R A . C21 C 0.08201(18) 0.2244(4) 0.09877(18) 0.0394(10) Uani 1 1 d . A . C22 C 0.0653(3) 0.4996(5) 0.1651(2) 0.0662(17) Uani 1 1 d . . . H22A H 0.0849 0.4696 0.2066 0.079 Uiso 1 1 calc R A . C23 C 0.0002(3) 0.5152(6) 0.1469(3) 0.082(2) Uani 1 1 d . A . H23A H -0.0171 0.4436 0.1464 0.123 Uiso 1 1 calc R . . H23B H -0.0198 0.5483 0.1071 0.123 Uiso 1 1 calc R . . H23C H -0.0034 0.5636 0.1757 0.123 Uiso 1 1 calc R . . C24 C 0.0925(4) 0.6096(5) 0.1659(3) 0.091(2) Uani 1 1 d . A . H24A H 0.1331 0.5988 0.1765 0.137 Uiso 1 1 calc R . . H24B H 0.0899 0.6576 0.1954 0.137 Uiso 1 1 calc R . . H24C H 0.0721 0.6435 0.1264 0.137 Uiso 1 1 calc R . . C25 C 0.08649(19) 0.1039(4) 0.1119(2) 0.0452(11) Uani 1 1 d . . . H25A H 0.1087 0.0949 0.1561 0.054 Uiso 1 1 calc R A . C26 C 0.1182(2) 0.0393(5) 0.0846(2) 0.0604(15) Uani 1 1 d . A . H26A H 0.1538 0.0778 0.0927 0.091 Uiso 1 1 calc R . . H26B H 0.0934 0.0330 0.0414 0.091 Uiso 1 1 calc R . . H26C H 0.1275 -0.0343 0.1023 0.091 Uiso 1 1 calc R . . C27 C 0.0267(2) 0.0529(5) 0.0912(3) 0.0630(15) Uani 1 1 d . A . H27A H 0.0088 0.0859 0.1135 0.095 Uiso 1 1 calc R . . H27B H 0.0307 -0.0266 0.0984 0.095 Uiso 1 1 calc R . . H27C H 0.0025 0.0667 0.0485 0.095 Uiso 1 1 calc R . . C28 C 0.34794(16) 0.2146(3) 0.32270(17) 0.0285(8) Uani 1 1 d . . . C29 C 0.44525(17) 0.2170(4) 0.3724(2) 0.0392(10) Uani 1 1 d . . . H29A H 0.4836 0.2393 0.3989 0.047 Uiso 1 1 calc R A . C30 C 0.42991(17) 0.1328(4) 0.33469(19) 0.0367(9) Uani 1 1 d . A . H30A H 0.4554 0.0831 0.3301 0.044 Uiso 1 1 calc R . . C31 C 0.39804(17) 0.3605(4) 0.4026(2) 0.0410(10) Uani 1 1 d . . . C32 C 0.39476(18) 0.3424(4) 0.4559(2) 0.0457(11) Uani 1 1 d . A . C33 C 0.4057(2) 0.4335(5) 0.4931(3) 0.0594(14) Uani 1 1 d . . . H33A H 0.4028 0.4258 0.5287 0.071 Uiso 1 1 calc R A . C34 C 0.4207(2) 0.5343(5) 0.4797(3) 0.074(2) Uani 1 1 d . A . H34A H 0.4290 0.5940 0.5066 0.089 Uiso 1 1 calc R . . C35 C 0.4236(2) 0.5489(5) 0.4282(3) 0.0678(17) Uani 1 1 d . . . H35A H 0.4338 0.6188 0.4195 0.081 Uiso 1 1 calc R A . C36 C 0.41164(19) 0.4627(4) 0.3879(3) 0.0523(13) Uani 1 1 d . A . C37 C 0.38515(19) 0.2304(4) 0.4744(2) 0.0458(11) Uani 1 1 d . . . H37A H 0.3597 0.1882 0.4374 0.055 Uiso 1 1 calc R A . C38 C 0.3556(2) 0.2333(6) 0.5139(2) 0.0620(15) Uani 1 1 d . A . H38A H 0.3220 0.2821 0.4959 0.093 Uiso 1 1 calc R . . H38B H 0.3828 0.2607 0.5536 0.093 Uiso 1 1 calc R . . H38C H 0.3431 0.1590 0.5173 0.093 Uiso 1 1 calc R . . C39 C 0.4424(2) 0.1688(5) 0.5069(2) 0.0605(14) Uani 1 1 d . A . H39A H 0.4594 0.1605 0.4802 0.091 Uiso 1 1 calc R . . H39B H 0.4357 0.0960 0.5189 0.091 Uiso 1 1 calc R . . H39C H 0.4689 0.2104 0.5423 0.091 Uiso 1 1 calc R . . C40 C 0.4162(2) 0.4829(4) 0.3312(3) 0.0566(13) Uani 1 1 d . . . H40A H 0.4026 0.4154 0.3059 0.068 Uiso 1 1 calc R A . C41 C 0.4797(2) 0.5030(6) 0.3471(3) 0.079(2) Uani 1 1 d . A . H41A H 0.5023 0.4364 0.3649 0.119 Uiso 1 1 calc R . . H41B H 0.4953 0.5638 0.3756 0.119 Uiso 1 1 calc R . . H41C H 0.4820 0.5216 0.3108 0.119 Uiso 1 1 calc R . . C42 C 0.3784(3) 0.5789(5) 0.2955(4) 0.080(2) Uani 1 1 d . A . H42A H 0.3386 0.5658 0.2873 0.120 Uiso 1 1 calc R . . H42B H 0.3796 0.5857 0.2578 0.120 Uiso 1 1 calc R . . H42C H 0.3926 0.6469 0.3185 0.120 Uiso 1 1 calc R . . C43 C 0.34018(16) 0.0296(3) 0.27648(18) 0.0327(8) Uani 1 1 d . . . C44 C 0.33175(17) -0.0463(3) 0.31347(18) 0.0338(9) Uani 1 1 d . A . C45 C 0.30433(19) -0.1451(4) 0.2887(2) 0.0424(10) Uani 1 1 d . . . H45A H 0.2979 -0.1966 0.3129 0.051 Uiso 1 1 calc R A . C46 C 0.2863(2) -0.1698(4) 0.2297(2) 0.0516(12) Uani 1 1 d . A . H46A H 0.2667 -0.2368 0.2132 0.062 Uiso 1 1 calc R . . C47 C 0.2970(2) -0.0969(4) 0.1950(2) 0.0495(12) Uani 1 1 d . . . H47A H 0.2857 -0.1161 0.1548 0.059 Uiso 1 1 calc R A . C48 C 0.32368(18) 0.0042(4) 0.21634(18) 0.0400(10) Uani 1 1 d . A . C49 C 0.35513(18) -0.0268(4) 0.38015(19) 0.0372(9) Uani 1 1 d . . . H49A H 0.3732 0.0478 0.3898 0.045 Uiso 1 1 calc R A . C50 C 0.3071(2) -0.0291(5) 0.3977(2) 0.0501(12) Uani 1 1 d . A . H50A H 0.2777 0.0255 0.3741 0.075 Uiso 1 1 calc R . . H50B H 0.3232 -0.0117 0.4402 0.075 Uiso 1 1 calc R . . H50C H 0.2897 -0.1024 0.3900 0.075 Uiso 1 1 calc R . . C51 C 0.4017(2) -0.1108(5) 0.4154(2) 0.0584(13) Uani 1 1 d . A . H51A H 0.4330 -0.1043 0.4051 0.088 Uiso 1 1 calc R . . H51B H 0.3853 -0.1850 0.4057 0.088 Uiso 1 1 calc R . . H51C H 0.4168 -0.0974 0.4582 0.088 Uiso 1 1 calc R . . C52 C 0.3379(2) 0.0792(5) 0.1776(2) 0.0510(12) Uani 1 1 d . . . H52A H 0.3429 0.1555 0.1939 0.061 Uiso 1 1 calc R A . C53 C 0.3952(3) 0.0425(7) 0.1805(3) 0.078(2) Uani 1 1 d . A . H53A H 0.4264 0.0500 0.2214 0.117 Uiso 1 1 calc R . . H53B H 0.4034 0.0887 0.1539 0.117 Uiso 1 1 calc R . . H53C H 0.3921 -0.0344 0.1679 0.117 Uiso 1 1 calc R . . C54 C 0.2910(2) 0.0813(6) 0.1126(2) 0.0632(15) Uani 1 1 d . A . H54A H 0.2537 0.0963 0.1108 0.095 Uiso 1 1 calc R . . H54B H 0.2896 0.0100 0.0941 0.095 Uiso 1 1 calc R . . H54C H 0.2998 0.1390 0.0913 0.095 Uiso 1 1 calc R . . O7 O 0.08705(17) 0.7349(4) -0.07039(17) 0.0672(10) Uani 1 1 d U . . C57 C 0.0871(3) 0.6806(5) -0.0208(2) 0.0650(12) Uani 1 1 d U C . H57A H 0.0470 0.6611 -0.0306 0.078 Uiso 1 1 calc R B 1 H57B H 0.1097 0.6118 -0.0122 0.078 Uiso 1 1 calc R B 1 C58 C 0.1106(6) 0.7475(12) 0.0289(6) 0.0638(17) Uani 0.50 1 d PU C 1 H58A H 0.1221 0.7052 0.0660 0.077 Uiso 0.50 1 calc PR C 1 H58B H 0.0838 0.8071 0.0261 0.077 Uiso 0.50 1 calc PR C 1 C59 C 0.1621(6) 0.7910(13) 0.0247(6) 0.0668(18) Uani 0.50 1 d PU C 1 H59A H 0.1954 0.7404 0.0437 0.080 Uiso 0.50 1 calc PR C 1 H59B H 0.1735 0.8647 0.0430 0.080 Uiso 0.50 1 calc PR C 1 C60 C 0.1369(6) 0.7957(12) -0.0465(7) 0.0685(17) Uani 0.50 1 d PU C 1 H60A H 0.1287 0.8726 -0.0608 0.082 Uiso 0.50 1 calc PR C 1 H60B H 0.1649 0.7643 -0.0579 0.082 Uiso 0.50 1 calc PR C 1 C58A C 0.1394(7) 0.7453(13) 0.0340(6) 0.0717(19) Uani 0.50 1 d PU C 2 H58C H 0.1253 0.7834 0.0590 0.086 Uiso 0.50 1 calc PR C 2 H58D H 0.1704 0.6937 0.0594 0.086 Uiso 0.50 1 calc PR C 2 C59A C 0.1610(6) 0.8278(12) 0.0042(6) 0.071(2) Uani 0.50 1 d PU C 2 H59C H 0.1671 0.9003 0.0239 0.085 Uiso 0.50 1 calc PR C 2 H59D H 0.1980 0.8027 0.0072 0.085 Uiso 0.50 1 calc PR C 2 C60A C 0.1210(6) 0.8352(12) -0.0529(7) 0.071(2) Uani 0.50 1 d PU C 2 H60C H 0.1397 0.8463 -0.0782 0.085 Uiso 0.50 1 calc PR C 2 H60D H 0.0956 0.8989 -0.0584 0.085 Uiso 0.50 1 calc PR C 2 O8 O 0.50331(18) 0.5731(3) 0.8200(2) 0.0702(10) Uani 1 1 d U . . C61 C 0.4691(3) 0.6687(5) 0.8050(3) 0.0720(12) Uani 1 1 d U . . H61A H 0.4806 0.7157 0.8406 0.086 Uiso 1 1 calc R . . H61B H 0.4279 0.6491 0.7889 0.086 Uiso 1 1 calc R . . C62 C 0.4784(3) 0.7277(6) 0.7588(3) 0.0819(14) Uani 1 1 d U . . H62A H 0.4757 0.8084 0.7618 0.098 Uiso 1 1 calc R . . H62B H 0.4509 0.7033 0.7179 0.098 Uiso 1 1 calc R . . C63 C 0.5392(4) 0.6915(7) 0.7766(4) 0.0983(16) Uani 1 1 d U . . H63A H 0.5428 0.6738 0.7405 0.118 Uiso 1 1 calc R . . H63B H 0.5665 0.7518 0.7981 0.118 Uiso 1 1 calc R . . C64 C 0.5531(3) 0.5972(6) 0.8140(4) 0.0824(14) Uani 1 1 d U . . H64A H 0.5628 0.5343 0.7957 0.099 Uiso 1 1 calc R . . H64B H 0.5864 0.6125 0.8535 0.099 Uiso 1 1 calc R . . O9 O 0.5854(2) 0.3585(5) 0.9070(4) 0.1318(18) Uani 1 1 d DU . . C67 C 0.6382(3) 0.2063(8) 0.9425(5) 0.119(2) Uani 1 1 d DU . . H67A H 0.6359 0.1436 0.9166 0.143 Uiso 1 1 calc R . . H67B H 0.6529 0.1784 0.9837 0.143 Uiso 1 1 calc R . . C68 C 0.5859(3) 0.2502(6) 0.9234(4) 0.0979(18) Uani 1 1 d DU . . H68A H 0.5749 0.2460 0.9556 0.118 Uiso 1 1 calc R . . H68B H 0.5572 0.2078 0.8889 0.118 Uiso 1 1 calc R . . C65 C 0.6442(3) 0.3833(8) 0.9177(6) 0.131(2) Uani 1 1 d DU . . H65A H 0.6439 0.4041 0.8800 0.158 Uiso 1 1 calc R . . H65B H 0.6608 0.4448 0.9463 0.158 Uiso 1 1 calc R . . C66 C 0.6767(4) 0.2871(8) 0.9412(6) 0.130(2) Uani 1 1 d DU . . H66A H 0.7085 0.3007 0.9819 0.155 Uiso 1 1 calc R . . H66B H 0.6936 0.2622 0.9157 0.155 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Al1 0.0243(6) 0.0557(8) 0.0452(7) -0.0207(6) 0.0132(5) 0.0009(6) Al2 0.0247(6) 0.0818(10) 0.0260(6) 0.0091(6) 0.0143(5) 0.0061(6) C55 0.0558(18) 0.0436(19) 0.0696(18) -0.0035(14) 0.0339(17) -0.0023(15) S1 0.0407(8) 0.0358(11) 0.0613(12) 0.0034(7) 0.0233(9) 0.0030(8) O1 0.0414(15) 0.0402(16) 0.069(2) -0.0044(14) 0.0210(15) 0.0044(13) O2 0.062(3) 0.047(2) 0.068(2) 0.0114(19) 0.033(2) 0.0031(19) O3 0.0377(16) 0.049(2) 0.067(3) 0.005(2) 0.022(2) 0.0028(15) F1 0.073(2) 0.060(2) 0.082(3) -0.012(2) 0.043(3) 0.0106(19) F2 0.050(2) 0.051(3) 0.077(3) -0.002(2) 0.026(2) -0.009(2) F3 0.076(3) 0.062(3) 0.0628(18) 0.0062(19) 0.028(2) -0.007(2) S1A 0.0425(16) 0.043(2) 0.068(2) -0.0005(17) 0.0241(18) 0.0049(18) O1A 0.041(2) 0.042(2) 0.066(3) -0.003(2) 0.023(3) 0.005(2) O2A 0.050(3) 0.050(4) 0.067(3) 0.002(3) 0.030(3) 0.007(3) O3A 0.042(2) 0.045(4) 0.066(4) 0.001(4) 0.025(3) 0.007(2) F1A 0.071(4) 0.047(3) 0.077(5) -0.004(3) 0.034(5) 0.007(3) F2A 0.054(3) 0.050(5) 0.075(5) -0.001(4) 0.028(3) -0.008(3) F3A 0.064(5) 0.057(5) 0.070(3) 0.000(3) 0.037(3) 0.002(4) S2 0.0415(8) 0.0499(9) 0.0290(7) 0.0037(7) 0.0283(6) -0.0037(7) C56 0.0544(18) 0.0646(17) 0.0616(19) 0.0080(17) 0.0297(15) 0.0066(15) O4 0.0429(17) 0.068(2) 0.0386(18) 0.0122(18) 0.0246(15) -0.0080(18) O5 0.073(3) 0.078(3) 0.0419(19) 0.002(2) 0.0374(19) 0.000(2) O6 0.0383(18) 0.064(3) 0.055(3) 0.002(3) 0.026(2) 0.001(2) F4 0.059(2) 0.086(3) 0.077(3) 0.016(3) 0.021(2) 0.019(2) F5 0.071(2) 0.061(2) 0.104(3) 0.027(3) 0.042(2) 0.005(2) F6 0.072(3) 0.088(3) 0.080(2) -0.011(2) 0.042(2) 0.019(2) S2A 0.0570(13) 0.0699(15) 0.0592(13) 0.0036(12) 0.0244(11) -0.0009(12) C56A 0.059(2) 0.068(2) 0.0540(17) 0.0080(18) 0.0246(16) 0.0025(19) O4A 0.052(2) 0.076(2) 0.052(2) 0.011(2) 0.0222(19) -0.002(2) O5A 0.073(3) 0.066(2) 0.080(3) 0.001(2) 0.032(3) 0.002(2) O6A 0.052(2) 0.065(3) 0.044(3) 0.001(3) 0.026(2) -0.002(2) F4A 0.070(3) 0.080(3) 0.070(3) 0.007(3) 0.012(3) 0.015(3) F5A 0.080(3) 0.104(4) 0.071(3) 0.001(3) 0.041(3) -0.005(3) F6A 0.072(3) 0.071(2) 0.050(3) 0.003(2) 0.024(3) 0.001(2) N1 0.0238(15) 0.0319(17) 0.0328(16) -0.0013(13) 0.0138(13) 0.0023(13) N2 0.0240(15) 0.0353(17) 0.0255(15) 0.0012(13) 0.0129(13) 0.0019(13) N3 0.0243(15) 0.0412(18) 0.0248(15) -0.0001(14) 0.0131(13) 0.0038(14) N4 0.0235(15) 0.0316(17) 0.0326(16) 0.0034(14) 0.0131(13) 0.0021(13) N5 0.0235(16) 0.0364(18) 0.0406(18) -0.0003(15) 0.0143(14) 0.0021(14) N6 0.0255(16) 0.0348(18) 0.0356(17) 0.0020(14) 0.0157(14) 0.0028(13) C1 0.0250(17) 0.0285(18) 0.0258(17) -0.0019(14) 0.0132(15) 0.0029(14) C2 0.0232(18) 0.048(2) 0.0294(19) 0.0023(17) 0.0142(16) 0.0032(17) C3 0.0228(18) 0.049(2) 0.0287(19) 0.0001(17) 0.0120(15) 0.0036(17) C4 0.0242(18) 0.037(2) 0.0284(18) 0.0039(16) 0.0136(15) 0.0017(16) C5 0.0312(19) 0.041(2) 0.0293(19) 0.0027(17) 0.0152(16) 0.0020(17) C6 0.046(2) 0.050(3) 0.030(2) 0.0063(19) 0.0181(19) 0.006(2) C7 0.051(3) 0.051(3) 0.039(2) 0.017(2) 0.023(2) 0.010(2) C8 0.046(2) 0.034(2) 0.047(2) 0.0096(19) 0.025(2) 0.0077(19) C9 0.0290(19) 0.039(2) 0.036(2) 0.0031(17) 0.0180(17) 0.0017(17) C10 0.046(2) 0.043(2) 0.0291(19) 0.0026(18) 0.0201(18) 0.007(2) C11 0.050(3) 0.069(3) 0.046(3) -0.009(2) 0.019(2) 0.015(3) C12 0.054(3) 0.056(3) 0.045(3) -0.009(2) 0.024(2) 0.005(2) C13 0.034(2) 0.037(2) 0.042(2) -0.0040(18) 0.0175(18) -0.0005(18) C14 0.060(3) 0.082(4) 0.071(4) -0.030(3) 0.038(3) -0.032(3) C15 0.051(3) 0.065(3) 0.051(3) -0.006(2) 0.030(2) 0.009(2) C16 0.0273(19) 0.051(3) 0.0231(18) 0.0010(17) 0.0137(15) 0.0025(17) C17 0.057(3) 0.051(3) 0.031(2) 0.006(2) 0.025(2) 0.002(2) C18 0.083(4) 0.066(3) 0.037(2) 0.008(2) 0.032(3) -0.004(3) C19 0.077(4) 0.081(4) 0.035(2) 0.005(3) 0.036(3) -0.005(3) C20 0.051(3) 0.084(4) 0.031(2) -0.012(2) 0.025(2) -0.004(3) C21 0.030(2) 0.060(3) 0.030(2) -0.0075(19) 0.0156(17) -0.0016(19) C22 0.116(5) 0.044(3) 0.041(3) 0.005(2) 0.039(3) 0.007(3) C23 0.121(6) 0.076(4) 0.083(4) 0.015(4) 0.076(4) 0.035(4) C24 0.151(7) 0.051(4) 0.063(4) 0.003(3) 0.042(4) 0.002(4) C25 0.039(2) 0.059(3) 0.036(2) -0.016(2) 0.0170(19) 0.001(2) C26 0.049(3) 0.078(4) 0.053(3) -0.029(3) 0.023(2) 0.003(3) C27 0.051(3) 0.070(4) 0.074(4) -0.026(3) 0.034(3) -0.013(3) C28 0.0266(18) 0.0285(19) 0.0321(19) 0.0040(15) 0.0152(16) 0.0003(15) C29 0.0222(18) 0.041(2) 0.052(2) 0.000(2) 0.0161(18) 0.0032(17) C30 0.0246(19) 0.039(2) 0.047(2) 0.0023(19) 0.0177(18) 0.0041(17) C31 0.0214(18) 0.040(2) 0.053(3) -0.008(2) 0.0100(18) 0.0025(17) C32 0.026(2) 0.053(3) 0.049(3) -0.014(2) 0.0099(19) 0.0040(19) C33 0.040(3) 0.066(4) 0.063(3) -0.025(3) 0.017(2) 0.004(2) C34 0.046(3) 0.058(4) 0.102(5) -0.038(4) 0.020(3) 0.000(3) C35 0.047(3) 0.040(3) 0.105(5) -0.017(3) 0.027(3) 0.000(2) C36 0.029(2) 0.037(2) 0.080(4) -0.002(2) 0.017(2) 0.0022(19) C37 0.034(2) 0.063(3) 0.037(2) -0.007(2) 0.0136(19) 0.003(2) C38 0.053(3) 0.096(4) 0.037(2) -0.004(3) 0.021(2) 0.007(3) C39 0.049(3) 0.072(4) 0.053(3) 0.003(3) 0.017(2) 0.015(3) C40 0.039(3) 0.045(3) 0.082(4) 0.013(3) 0.026(3) 0.000(2) C41 0.043(3) 0.079(4) 0.113(5) 0.023(4) 0.036(3) -0.003(3) C42 0.059(4) 0.056(4) 0.119(6) 0.025(4) 0.038(4) 0.008(3) C43 0.0264(18) 0.036(2) 0.037(2) -0.0020(17) 0.0160(16) 0.0034(16) C44 0.0293(19) 0.035(2) 0.039(2) -0.0027(17) 0.0182(17) 0.0036(16) C45 0.040(2) 0.037(2) 0.054(3) -0.006(2) 0.025(2) 0.0000(19) C46 0.047(3) 0.048(3) 0.061(3) -0.018(2) 0.026(2) -0.009(2) C47 0.043(2) 0.063(3) 0.041(2) -0.017(2) 0.019(2) 0.000(2) C48 0.033(2) 0.056(3) 0.034(2) -0.005(2) 0.0169(18) 0.0045(19) C49 0.037(2) 0.038(2) 0.040(2) 0.0026(18) 0.0213(18) 0.0018(18) C50 0.051(3) 0.061(3) 0.049(3) -0.004(2) 0.033(2) -0.004(2) C51 0.058(3) 0.062(3) 0.048(3) 0.012(3) 0.019(2) 0.017(3) C52 0.042(2) 0.076(3) 0.040(2) 0.008(2) 0.023(2) 0.006(2) C53 0.054(3) 0.131(6) 0.065(3) 0.028(4) 0.040(3) 0.020(4) C54 0.056(3) 0.100(5) 0.038(2) 0.006(3) 0.025(2) 0.012(3) O7 0.0554(19) 0.075(2) 0.0557(17) 0.0148(16) 0.0140(15) -0.0093(16) C57 0.059(2) 0.072(3) 0.057(2) 0.012(2) 0.022(2) -0.002(2) C58 0.053(3) 0.071(4) 0.060(3) 0.006(3) 0.021(3) 0.002(3) C59 0.057(3) 0.074(4) 0.061(3) 0.003(3) 0.020(3) -0.004(3) C60 0.057(3) 0.074(4) 0.062(3) 0.010(3) 0.018(3) -0.009(3) C58A 0.068(3) 0.072(3) 0.059(2) 0.007(3) 0.017(3) -0.003(3) C59A 0.063(3) 0.074(4) 0.062(3) 0.005(3) 0.017(3) -0.007(3) C60A 0.056(4) 0.075(4) 0.065(3) 0.012(3) 0.016(3) -0.010(3) O8 0.069(2) 0.060(2) 0.096(3) 0.0080(18) 0.051(2) -0.0042(17) C61 0.078(3) 0.061(3) 0.096(3) 0.010(2) 0.056(3) -0.001(2) C62 0.096(3) 0.069(3) 0.098(3) 0.012(2) 0.061(3) -0.007(2) C63 0.102(3) 0.087(3) 0.138(4) 0.015(3) 0.084(3) -0.006(3) C64 0.077(3) 0.077(3) 0.115(3) -0.001(3) 0.063(3) -0.006(2) O9 0.075(2) 0.111(3) 0.199(4) 0.042(3) 0.057(3) 0.006(2) C67 0.067(3) 0.112(4) 0.177(5) 0.040(4) 0.059(3) 0.014(3) C68 0.052(2) 0.094(3) 0.156(5) 0.042(4) 0.055(3) 0.009(2) C65 0.076(3) 0.119(4) 0.201(5) 0.044(4) 0.066(4) -0.004(3) C66 0.067(3) 0.129(4) 0.197(5) 0.042(4) 0.066(4) 0.005(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Al1 O1A 1.617(17) . ? Al1 N4 1.849(3) . ? Al1 N1 1.863(3) . ? Al1 O1 1.904(5) . ? Al1 Al2 2.6663(19) . ? Al1 H1 0.95(6) . ? Al2 O4 1.761(5) . ? Al2 N1 1.858(3) . ? Al2 N4 1.872(3) . ? Al2 O4A 2.054(10) . ? Al2 H2 1.53(5) . ? C55 F1 1.316(7) . ? C55 F2A 1.33(3) . ? C55 F3 1.333(7) . ? C55 F2 1.341(9) . ? C55 F3A 1.37(2) . ? C55 F1A 1.43(2) . ? C55 S1A 1.740(14) . ? C55 S1 1.822(6) . ? S1 O2 1.410(5) . ? S1 O3 1.433(8) . ? S1 O1 1.494(5) . ? S1A O3A 1.45(4) . ? S1A O1A 1.51(2) . ? S1A O2A 1.53(2) . ? S2 O6 1.402(7) . ? S2 O5 1.414(6) . ? S2 O4 1.481(5) . ? S2 C56 1.816(9) . ? C56 F4 1.286(9) . ? C56 F5 1.301(9) . ? C56 F6 1.354(9) . ? S2A O6A 1.431(12) . ? S2A O4A 1.473(9) . ? S2A O5A 1.494(10) . ? S2A C56A 1.811(12) . ? C56A F6A 1.308(12) . ? C56A F5A 1.318(12) . ? C56A F4A 1.333(12) . ? N1 C1 1.327(5) . ? N2 C1 1.376(5) . ? N2 C2 1.397(5) . ? N2 C4 1.445(5) . ? N3 C1 1.362(5) . ? N3 C3 1.395(5) . ? N3 C16 1.453(5) . ? N4 C28 1.324(5) . ? N5 C28 1.364(5) . ? N5 C29 1.401(5) . ? N5 C31 1.444(6) . ? N6 C28 1.382(5) . ? N6 C30 1.398(5) . ? N6 C43 1.435(5) . ? C2 C3 1.331(6) . ? C2 H2B 0.9500 . ? C3 H3B 0.9500 . ? C4 C9 1.392(6) . ? C4 C5 1.408(6) . ? C5 C6 1.395(6) . ? C5 C10 1.508(6) . ? C6 C7 1.377(7) . ? C6 H6A 0.9500 . ? C7 C8 1.374(7) . ? C7 H7A 0.9500 . ? C8 C9 1.391(6) . ? C8 H8A 0.9500 . ? C9 C13 1.524(6) . ? C10 C12 1.525(6) . ? C10 C11 1.531(7) . ? C10 H10A 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C15 1.527(6) . ? C13 C14 1.530(7) . ? C13 H13A 1.0000 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.380(7) . ? C16 C21 1.409(6) . ? C17 C18 1.406(6) . ? C17 C22 1.527(7) . ? C18 C19 1.374(8) . ? C18 H18A 0.9500 . ? C19 C20 1.359(8) . ? C19 H19A 0.9500 . ? C20 C21 1.407(6) . ? C20 H20A 0.9500 . ? C21 C25 1.496(7) . ? C22 C24 1.514(9) . ? C22 C23 1.562(10) . ? C22 H22A 1.0000 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C26 1.531(6) . ? C25 C27 1.535(7) . ? C25 H25A 1.0000 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C29 C30 1.330(6) . ? C29 H29A 0.9500 . ? C30 H30A 0.9500 . ? C31 C36 1.393(7) . ? C31 C32 1.417(7) . ? C32 C33 1.395(7) . ? C32 C37 1.503(7) . ? C33 C34 1.380(10) . ? C33 H33A 0.9500 . ? C34 C35 1.361(10) . ? C34 H34A 0.9500 . ? C35 C36 1.395(8) . ? C35 H35A 0.9500 . ? C36 C40 1.525(8) . ? C37 C39 1.529(7) . ? C37 C38 1.536(7) . ? C37 H37A 1.0000 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 C42 1.524(8) . ? C40 C41 1.543(7) . ? C40 H40A 1.0000 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 C44 1.409(6) . ? C43 C48 1.414(6) . ? C44 C45 1.391(6) . ? C44 C49 1.526(6) . ? C45 C46 1.376(7) . ? C45 H45A 0.9500 . ? C46 C47 1.372(8) . ? C46 H46A 0.9500 . ? C47 C48 1.394(7) . ? C47 H47A 0.9500 . ? C48 C52 1.514(7) . ? C49 C51 1.521(6) . ? C49 C50 1.528(6) . ? C49 H49A 1.0000 . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C52 C54 1.525(7) . ? C52 C53 1.542(7) . ? C52 H52A 1.0000 . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? O7 C60 1.372(14) . ? O7 C57 1.425(7) . ? O7 C60A 1.452(15) . ? C57 C58 1.379(14) . ? C57 C58A 1.626(15) . ? C57 H57A 0.9900 . ? C57 H57B 0.9900 . ? C58 C59 1.505(19) . ? C58 H58A 0.9900 . ? C58 H58B 0.9900 . ? C59 C60 1.61(2) . ? C59 H59A 0.9900 . ? C59 H59B 0.9900 . ? C60 H60A 0.9900 . ? C60 H60B 0.9900 . ? C58A C59A 1.52(2) . ? C58A H58C 0.9900 . ? C58A H58D 0.9900 . ? C59A C60A 1.334(19) . ? C59A H59C 0.9900 . ? C59A H59D 0.9900 . ? C60A H60C 0.9900 . ? C60A H60D 0.9900 . ? O8 C61 1.409(7) . ? O8 C64 1.420(7) . ? C61 C62 1.494(9) . ? C61 H61A 0.9900 . ? C61 H61B 0.9900 . ? C62 C63 1.509(10) . ? C62 H62A 0.9900 . ? C62 H62B 0.9900 . ? C63 C64 1.424(10) . ? C63 H63A 0.9900 . ? C63 H63B 0.9900 . ? C64 H64A 0.9900 . ? C64 H64B 0.9900 . ? O9 C68 1.380(8) . ? O9 C65 1.472(8) . ? C67 C68 1.338(8) . ? C67 C66 1.424(10) . ? C67 H67A 0.9900 . ? C67 H67B 0.9900 . ? C68 H68A 0.9900 . ? C68 H68B 0.9900 . ? C65 C66 1.406(10) . ? C65 H65A 0.9900 . ? C65 H65B 0.9900 . ? C66 H66A 0.9900 . ? C66 H66B 0.9900 . ? 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 O1A Al1 N4 129.4(7) . . ? O1A Al1 N1 120.5(6) . . ? N4 Al1 N1 88.27(15) . . ? O1A Al1 O1 32.6(7) . . ? N4 Al1 O1 104.32(19) . . ? N1 Al1 O1 105.40(19) . . ? O1A Al1 Al2 137.7(7) . . ? N4 Al1 Al2 44.58(10) . . ? N1 Al1 Al2 44.14(10) . . ? O1 Al1 Al2 105.89(17) . . ? O1A Al1 H1 101(3) . . ? N4 Al1 H1 106(3) . . ? N1 Al1 H1 112(3) . . ? O1 Al1 H1 132(3) . . ? Al2 Al1 H1 122(3) . . ? O4 Al2 N1 118.0(2) . . ? O4 Al2 N4 113.7(2) . . ? N1 Al2 N4 87.72(15) . . ? O4 Al2 O4A 29.1(3) . . ? N1 Al2 O4A 95.4(3) . . ? N4 Al2 O4A 96.6(3) . . ? O4 Al2 Al1 122.2(2) . . ? N1 Al2 Al1 44.29(10) . . ? N4 Al2 Al1 43.88(10) . . ? O4A Al2 Al1 93.4(3) . . ? O4 Al2 H2 97.4(19) . . ? N1 Al2 H2 117.5(19) . . ? N4 Al2 H2 124.5(19) . . ? O4A Al2 H2 125.8(19) . . ? Al1 Al2 H2 140.4(19) . . ? F1 C55 F2A 116.1(16) . . ? F1 C55 F3 109.0(5) . . ? F2A C55 F3 92.6(12) . . ? F1 C55 F2 106.8(5) . . ? F2A C55 F2 17.2(12) . . ? F3 C55 F2 109.6(5) . . ? F1 C55 F3A 82.7(9) . . ? F2A C55 F3A 107.6(16) . . ? F3 C55 F3A 26.5(8) . . ? F2 C55 F3A 122.3(11) . . ? F1 C55 F1A 25.5(9) . . ? F2A C55 F1A 111.0(17) . . ? F3 C55 F1A 134.2(10) . . ? F2 C55 F1A 96.3(11) . . ? F3A C55 F1A 107.7(13) . . ? F1 C55 S1A 117.3(6) . . ? F2A C55 S1A 117.8(18) . . ? F3 C55 S1A 98.3(5) . . ? F2 C55 S1A 115.5(7) . . ? F3A C55 S1A 108.5(11) . . ? F1A C55 S1A 103.8(10) . . ? F1 C55 S1 110.6(4) . . ? F2A C55 S1 115.3(17) . . ? F3 C55 S1 111.9(4) . . ? F2 C55 S1 108.9(5) . . ? F3A C55 S1 120.7(10) . . ? F1A C55 S1 93.3(9) . . ? S1A C55 S1 13.6(4) . . ? O2 S1 O3 120.0(4) . . ? O2 S1 O1 112.5(4) . . ? O3 S1 O1 111.7(4) . . ? O2 S1 C55 103.3(3) . . ? O3 S1 C55 105.4(3) . . ? O1 S1 C55 101.6(3) . . ? S1 O1 Al1 133.7(3) . . ? O3A S1A O1A 110.0(19) . . ? O3A S1A O2A 126.6(18) . . ? O1A S1A O2A 115.1(14) . . ? O3A S1A C55 100.7(16) . . ? O1A S1A C55 99.0(9) . . ? O2A S1A C55 99.1(10) . . ? S1A O1A Al1 130.1(13) . . ? O6 S2 O5 113.7(5) . . ? O6 S2 O4 111.4(5) . . ? O5 S2 O4 114.1(4) . . ? O6 S2 C56 107.5(5) . . ? O5 S2 C56 105.9(4) . . ? O4 S2 C56 103.4(4) . . ? F4 C56 F5 110.4(8) . . ? F4 C56 F6 104.3(7) . . ? F5 C56 F6 108.7(8) . . ? F4 C56 S2 113.9(7) . . ? F5 C56 S2 110.3(6) . . ? F6 C56 S2 109.0(6) . . ? S2 O4 Al2 144.9(4) . . ? O6A S2A O4A 109.2(9) . . ? O6A S2A O5A 122.5(9) . . ? O4A S2A O5A 117.6(7) . . ? O6A S2A C56A 108.3(7) . . ? O4A S2A C56A 97.7(6) . . ? O5A S2A C56A 97.0(6) . . ? F6A C56A F5A 103.1(10) . . ? F6A C56A F4A 106.5(10) . . ? F5A C56A F4A 115.4(11) . . ? F6A C56A S2A 111.4(8) . . ? F5A C56A S2A 110.1(8) . . ? F4A C56A S2A 110.1(9) . . ? S2A O4A Al2 136.3(6) . . ? C1 N1 Al2 133.5(3) . . ? C1 N1 Al1 134.1(3) . . ? Al2 N1 Al1 91.57(15) . . ? C1 N2 C2 109.1(3) . . ? C1 N2 C4 126.5(3) . . ? C2 N2 C4 120.7(3) . . ? C1 N3 C3 110.5(3) . . ? C1 N3 C16 128.8(3) . . ? C3 N3 C16 120.7(3) . . ? C28 N4 Al1 136.9(3) . . ? C28 N4 Al2 131.6(3) . . ? Al1 N4 Al2 91.53(15) . . ? C28 N5 C29 109.5(3) . . ? C28 N5 C31 130.2(3) . . ? C29 N5 C31 120.3(3) . . ? C28 N6 C30 108.9(3) . . ? C28 N6 C43 125.3(3) . . ? C30 N6 C43 120.3(3) . . ? N1 C1 N3 128.0(3) . . ? N1 C1 N2 126.8(3) . . ? N3 C1 N2 105.2(3) . . ? C3 C2 N2 108.3(3) . . ? C3 C2 H2B 125.8 . . ? N2 C2 H2B 125.8 . . ? C2 C3 N3 106.9(3) . . ? C2 C3 H3B 126.6 . . ? N3 C3 H3B 126.6 . . ? C9 C4 C5 122.9(4) . . ? C9 C4 N2 117.7(3) . . ? C5 C4 N2 119.1(4) . . ? C6 C5 C4 116.5(4) . . ? C6 C5 C10 121.5(4) . . ? C4 C5 C10 122.0(4) . . ? C7 C6 C5 121.4(4) . . ? C7 C6 H6A 119.3 . . ? C5 C6 H6A 119.3 . . ? C8 C7 C6 120.7(4) . . ? C8 C7 H7A 119.6 . . ? C6 C7 H7A 119.6 . . ? C7 C8 C9 120.7(4) . . ? C7 C8 H8A 119.7 . . ? C9 C8 H8A 119.7 . . ? C8 C9 C4 117.8(4) . . ? C8 C9 C13 119.5(4) . . ? C4 C9 C13 122.7(4) . . ? C5 C10 C12 113.4(4) . . ? C5 C10 C11 110.4(4) . . ? C12 C10 C11 109.2(4) . . ? C5 C10 H10A 107.9 . . ? C12 C10 H10A 107.9 . . ? C11 C10 H10A 107.9 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C9 C13 C15 112.4(4) . . ? C9 C13 C14 111.2(4) . . ? C15 C13 C14 109.6(4) . . ? C9 C13 H13A 107.8 . . ? C15 C13 H13A 107.8 . . ? C14 C13 H13A 107.8 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C17 C16 C21 123.8(4) . . ? C17 C16 N3 118.4(4) . . ? C21 C16 N3 117.3(4) . . ? C16 C17 C18 117.3(5) . . ? C16 C17 C22 122.9(4) . . ? C18 C17 C22 119.6(5) . . ? C19 C18 C17 120.2(5) . . ? C19 C18 H18A 119.9 . . ? C17 C18 H18A 119.9 . . ? C20 C19 C18 121.4(5) . . ? C20 C19 H19A 119.3 . . ? C18 C19 H19A 119.3 . . ? C19 C20 C21 121.6(5) . . ? C19 C20 H20A 119.2 . . ? C21 C20 H20A 119.2 . . ? C20 C21 C16 115.7(5) . . ? C20 C21 C25 121.0(4) . . ? C16 C21 C25 123.3(4) . . ? C24 C22 C17 113.2(5) . . ? C24 C22 C23 110.0(6) . . ? C17 C22 C23 110.4(5) . . ? C24 C22 H22A 107.7 . . ? C17 C22 H22A 107.7 . . ? C23 C22 H22A 107.7 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C21 C25 C26 113.8(4) . . ? C21 C25 C27 111.1(4) . . ? C26 C25 C27 109.1(4) . . ? C21 C25 H25A 107.5 . . ? C26 C25 H25A 107.5 . . ? C27 C25 H25A 107.5 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? N4 C28 N5 128.2(4) . . ? N4 C28 N6 126.0(4) . . ? N5 C28 N6 105.8(3) . . ? C30 C29 N5 107.8(4) . . ? C30 C29 H29A 126.1 . . ? N5 C29 H29A 126.1 . . ? C29 C30 N6 108.0(4) . . ? C29 C30 H30A 126.0 . . ? N6 C30 H30A 126.0 . . ? C36 C31 C32 122.4(4) . . ? C36 C31 N5 118.4(4) . . ? C32 C31 N5 118.7(4) . . ? C33 C32 C31 116.1(5) . . ? C33 C32 C37 121.3(5) . . ? C31 C32 C37 122.4(4) . . ? C34 C33 C32 122.0(6) . . ? C34 C33 H33A 119.0 . . ? C32 C33 H33A 119.0 . . ? C35 C34 C33 120.5(5) . . ? C35 C34 H34A 119.8 . . ? C33 C34 H34A 119.8 . . ? C34 C35 C36 121.0(6) . . ? C34 C35 H35A 119.5 . . ? C36 C35 H35A 119.5 . . ? C31 C36 C35 118.0(6) . . ? C31 C36 C40 123.0(5) . . ? C35 C36 C40 118.9(5) . . ? C32 C37 C39 110.2(4) . . ? C32 C37 C38 113.4(4) . . ? C39 C37 C38 109.5(4) . . ? C32 C37 H37A 107.9 . . ? C39 C37 H37A 107.9 . . ? C38 C37 H37A 107.9 . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C37 C39 H39A 109.5 . . ? C37 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C37 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C42 C40 C36 111.5(5) . . ? C42 C40 C41 110.9(5) . . ? C36 C40 C41 109.9(5) . . ? C42 C40 H40A 108.2 . . ? C36 C40 H40A 108.2 . . ? C41 C40 H40A 108.2 . . ? C40 C41 H41A 109.5 . . ? C40 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C40 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C40 C42 H42A 109.5 . . ? C40 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C40 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C44 C43 C48 121.0(4) . . ? C44 C43 N6 117.8(3) . . ? C48 C43 N6 121.0(4) . . ? C45 C44 C43 118.4(4) . . ? C45 C44 C49 119.2(4) . . ? C43 C44 C49 122.3(4) . . ? C46 C45 C44 121.4(5) . . ? C46 C45 H45A 119.3 . . ? C44 C45 H45A 119.3 . . ? C47 C46 C45 119.5(5) . . ? C47 C46 H46A 120.3 . . ? C45 C46 H46A 120.3 . . ? C46 C47 C48 122.6(4) . . ? C46 C47 H47A 118.7 . . ? C48 C47 H47A 118.7 . . ? C47 C48 C43 117.1(4) . . ? C47 C48 C52 120.8(4) . . ? C43 C48 C52 122.0(4) . . ? C51 C49 C44 109.9(4) . . ? C51 C49 C50 111.3(4) . . ? C44 C49 C50 111.7(4) . . ? C51 C49 H49A 107.9 . . ? C44 C49 H49A 107.9 . . ? C50 C49 H49A 107.9 . . ? C49 C50 H50A 109.5 . . ? C49 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C49 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C49 C51 H51A 109.5 . . ? C49 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C49 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C48 C52 C54 113.3(4) . . ? C48 C52 C53 109.4(4) . . ? C54 C52 C53 109.0(4) . . ? C48 C52 H52A 108.3 . . ? C54 C52 H52A 108.3 . . ? C53 C52 H52A 108.3 . . ? C52 C53 H53A 109.5 . . ? C52 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C52 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C52 C54 H54A 109.5 . . ? C52 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C52 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C60 O7 C57 105.0(7) . . ? C60 O7 C60A 24.6(8) . . ? C57 O7 C60A 112.1(7) . . ? C58 C57 O7 110.5(7) . . ? C58 C57 C58A 25.5(7) . . ? O7 C57 C58A 100.4(7) . . ? C58 C57 H57A 109.6 . . ? O7 C57 H57A 109.6 . . ? C58A C57 H57A 134.5 . . ? C58 C57 H57B 109.6 . . ? O7 C57 H57B 109.6 . . ? C58A C57 H57B 92.5 . . ? H57A C57 H57B 108.1 . . ? C57 C58 C59 99.9(10) . . ? C57 C58 H58A 111.8 . . ? C59 C58 H58A 111.8 . . ? C57 C58 H58B 111.8 . . ? C59 C58 H58B 111.8 . . ? H58A C58 H58B 109.5 . . ? C58 C59 C60 100.8(10) . . ? C58 C59 H59A 111.6 . . ? C60 C59 H59A 111.6 . . ? C58 C59 H59B 111.6 . . ? C60 C59 H59B 111.6 . . ? H59A C59 H59B 109.4 . . ? O7 C60 C59 106.1(11) . . ? O7 C60 H60A 110.5 . . ? C59 C60 H60A 110.5 . . ? O7 C60 H60B 110.5 . . ? C59 C60 H60B 110.5 . . ? H60A C60 H60B 108.7 . . ? C59A C58A C57 104.9(10) . . ? C59A C58A H58C 110.8 . . ? C57 C58A H58C 110.8 . . ? C59A C58A H58D 110.8 . . ? C57 C58A H58D 110.8 . . ? H58C C58A H58D 108.8 . . ? C60A C59A C58A 107.4(12) . . ? C60A C59A H59C 110.2 . . ? C58A C59A H59C 110.2 . . ? C60A C59A H59D 110.2 . . ? C58A C59A H59D 110.2 . . ? H59C C59A H59D 108.5 . . ? C59A C60A O7 109.3(12) . . ? C59A C60A H60C 109.8 . . ? O7 C60A H60C 109.8 . . ? C59A C60A H60D 109.8 . . ? O7 C60A H60D 109.8 . . ? H60C C60A H60D 108.3 . . ? C61 O8 C64 107.8(5) . . ? O8 C61 C62 106.7(5) . . ? O8 C61 H61A 110.4 . . ? C62 C61 H61A 110.4 . . ? O8 C61 H61B 110.4 . . ? C62 C61 H61B 110.4 . . ? H61A C61 H61B 108.6 . . ? C61 C62 C63 99.8(6) . . ? C61 C62 H62A 111.8 . . ? C63 C62 H62A 111.8 . . ? C61 C62 H62B 111.8 . . ? C63 C62 H62B 111.8 . . ? H62A C62 H62B 109.5 . . ? C64 C63 C62 109.6(6) . . ? C64 C63 H63A 109.7 . . ? C62 C63 H63A 109.7 . . ? C64 C63 H63B 109.7 . . ? C62 C63 H63B 109.7 . . ? H63A C63 H63B 108.2 . . ? O8 C64 C63 106.3(6) . . ? O8 C64 H64A 110.5 . . ? C63 C64 H64A 110.5 . . ? O8 C64 H64B 110.5 . . ? C63 C64 H64B 110.5 . . ? H64A C64 H64B 108.7 . . ? C68 O9 C65 106.3(6) . . ? C68 C67 C66 109.8(8) . . ? C68 C67 H67A 109.7 . . ? C66 C67 H67A 109.7 . . ? C68 C67 H67B 109.7 . . ? C66 C67 H67B 109.7 . . ? H67A C67 H67B 108.2 . . ? C67 C68 O9 110.6(6) . . ? C67 C68 H68A 109.5 . . ? O9 C68 H68A 109.5 . . ? C67 C68 H68B 109.5 . . ? O9 C68 H68B 109.5 . . ? H68A C68 H68B 108.1 . . ? C66 C65 O9 106.5(7) . . ? C66 C65 H65A 110.4 . . ? O9 C65 H65A 110.4 . . ? C66 C65 H65B 110.4 . . ? O9 C65 H65B 110.4 . . ? H65A C65 H65B 108.6 . . ? C65 C66 C67 106.7(7) . . ? C65 C66 H66A 110.4 . . ? C67 C66 H66A 110.4 . . ? C65 C66 H66B 110.4 . . ? C67 C66 H66B 110.4 . . ? H66A C66 H66B 108.6 . . ? 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 O1A Al1 Al2 O4 11.4(9) . . . . ? N4 Al1 Al2 O4 -91.8(3) . . . . ? N1 Al1 Al2 O4 98.6(3) . . . . ? O1 Al1 Al2 O4 2.7(3) . . . . ? O1A Al1 Al2 N1 -87.2(9) . . . . ? N4 Al1 Al2 N1 169.6(2) . . . . ? O1 Al1 Al2 N1 -95.9(2) . . . . ? O1A Al1 Al2 N4 103.1(9) . . . . ? N1 Al1 Al2 N4 -169.6(2) . . . . ? O1 Al1 Al2 N4 94.4(2) . . . . ? O1A Al1 Al2 O4A 7.1(9) . . . . ? N4 Al1 Al2 O4A -96.1(3) . . . . ? N1 Al1 Al2 O4A 94.3(3) . . . . ? O1 Al1 Al2 O4A -1.6(3) . . . . ? F1 C55 S1 O2 68.8(5) . . . . ? F2A C55 S1 O2 -65.5(14) . . . . ? F3 C55 S1 O2 -169.5(4) . . . . ? F2 C55 S1 O2 -48.3(5) . . . . ? F3A C55 S1 O2 162.5(10) . . . . ? F1A C55 S1 O2 49.6(11) . . . . ? S1A C55 S1 O2 -169(2) . . . . ? F1 C55 S1 O3 -57.9(6) . . . . ? F2A C55 S1 O3 167.9(14) . . . . ? F3 C55 S1 O3 63.8(6) . . . . ? F2 C55 S1 O3 -174.9(5) . . . . ? F3A C55 S1 O3 35.8(11) . . . . ? F1A C55 S1 O3 -77.1(11) . . . . ? S1A C55 S1 O3 64(2) . . . . ? F1 C55 S1 O1 -174.5(4) . . . . ? F2A C55 S1 O1 51.3(14) . . . . ? F3 C55 S1 O1 -52.8(5) . . . . ? F2 C55 S1 O1 68.4(5) . . . . ? F3A C55 S1 O1 -80.8(10) . . . . ? F1A C55 S1 O1 166.3(11) . . . . ? S1A C55 S1 O1 -53(2) . . . . ? O2 S1 O1 Al1 -142.0(4) . . . . ? O3 S1 O1 Al1 -3.7(6) . . . . ? C55 S1 O1 Al1 108.2(4) . . . . ? O1A Al1 O1 S1 -62.9(12) . . . . ? N4 Al1 O1 S1 152.4(4) . . . . ? N1 Al1 O1 S1 60.2(5) . . . . ? Al2 Al1 O1 S1 106.2(4) . . . . ? F1 C55 S1A O3A -35.8(18) . . . . ? F2A C55 S1A O3A 178(2) . . . . ? F3 C55 S1A O3A 80.6(17) . . . . ? F2 C55 S1A O3A -163.1(17) . . . . ? F3A C55 S1A O3A 55(2) . . . . ? F1A C55 S1A O3A -59(2) . . . . ? S1 C55 S1A O3A -99(3) . . . . ? F1 C55 S1A O1A -148.3(9) . . . . ? F2A C55 S1A O1A 65.5(17) . . . . ? F3 C55 S1A O1A -31.9(10) . . . . ? F2 C55 S1A O1A 84.5(10) . . . . ? F3A C55 S1A O1A -57.1(14) . . . . ? F1A C55 S1A O1A -171.5(14) . . . . ? S1 C55 S1A O1A 148(3) . . . . ? F1 C55 S1A O2A 94.3(11) . . . . ? F2A C55 S1A O2A -52.0(17) . . . . ? F3 C55 S1A O2A -149.3(10) . . . . ? F2 C55 S1A O2A -32.9(11) . . . . ? F3A C55 S1A O2A -174.5(12) . . . . ? F1A C55 S1A O2A 71.1(14) . . . . ? S1 C55 S1A O2A 30.8(19) . . . . ? O3A S1A O1A Al1 81(2) . . . . ? O2A S1A O1A Al1 -70(2) . . . . ? C55 S1A O1A Al1 -174.5(13) . . . . ? N4 Al1 O1A S1A 94.2(16) . . . . ? N1 Al1 O1A S1A -22(2) . . . . ? O1 Al1 O1A S1A 47.7(14) . . . . ? Al2 Al1 O1A S1A 32(2) . . . . ? O6 S2 C56 F4 173.7(7) . . . . ? O5 S2 C56 F4 51.9(7) . . . . ? O4 S2 C56 F4 -68.4(7) . . . . ? O6 S2 C56 F5 48.9(8) . . . . ? O5 S2 C56 F5 -72.9(7) . . . . ? O4 S2 C56 F5 166.8(6) . . . . ? O6 S2 C56 F6 -70.3(8) . . . . ? O5 S2 C56 F6 167.8(6) . . . . ? O4 S2 C56 F6 47.6(6) . . . . ? O6 S2 O4 Al2 -7.0(10) . . . . ? O5 S2 O4 Al2 123.4(8) . . . . ? C56 S2 O4 Al2 -122.1(8) . . . . ? N1 Al2 O4 S2 126.1(7) . . . . ? N4 Al2 O4 S2 25.5(9) . . . . ? O4A Al2 O4 S2 83.5(10) . . . . ? Al1 Al2 O4 S2 74.6(8) . . . . ? O6A S2A C56A F6A 74.6(12) . . . . ? O4A S2A C56A F6A -38.6(10) . . . . ? O5A S2A C56A F6A -157.8(9) . . . . ? O6A S2A C56A F5A -39.1(13) . . . . ? O4A S2A C56A F5A -152.3(9) . . . . ? O5A S2A C56A F5A 88.5(10) . . . . ? O6A S2A C56A F4A -167.5(12) . . . . ? O4A S2A C56A F4A 79.3(10) . . . . ? O5A S2A C56A F4A -39.9(11) . . . . ? O6A S2A O4A Al2 -8.1(12) . . . . ? O5A S2A O4A Al2 -153.5(9) . . . . ? C56A S2A O4A Al2 104.5(9) . . . . ? O4 Al2 O4A S2A -71.6(10) . . . . ? N1 Al2 O4A S2A 145.3(9) . . . . ? N4 Al2 O4A S2A 56.9(10) . . . . ? Al1 Al2 O4A S2A 100.9(9) . . . . ? O4 Al2 N1 C1 81.2(4) . . . . ? N4 Al2 N1 C1 -163.0(4) . . . . ? O4A Al2 N1 C1 100.5(5) . . . . ? Al1 Al2 N1 C1 -170.2(5) . . . . ? O4 Al2 N1 Al1 -108.6(3) . . . . ? N4 Al2 N1 Al1 7.17(16) . . . . ? O4A Al2 N1 Al1 -89.3(3) . . . . ? O1A Al1 N1 C1 -61.2(9) . . . . ? N4 Al1 N1 C1 162.9(4) . . . . ? O1 Al1 N1 C1 -92.8(4) . . . . ? Al2 Al1 N1 C1 170.1(5) . . . . ? O1A Al1 N1 Al2 128.7(8) . . . . ? N4 Al1 N1 Al2 -7.26(16) . . . . ? O1 Al1 N1 Al2 97.13(19) . . . . ? O1A Al1 N4 C28 60.0(10) . . . . ? N1 Al1 N4 C28 -170.8(4) . . . . ? O1 Al1 N4 C28 83.8(4) . . . . ? Al2 Al1 N4 C28 -178.0(5) . . . . ? O1A Al1 N4 Al2 -122.1(9) . . . . ? N1 Al1 N4 Al2 7.20(16) . . . . ? O1 Al1 N4 Al2 -98.25(19) . . . . ? O4 Al2 N4 C28 -69.4(4) . . . . ? N1 Al2 N4 C28 170.9(4) . . . . ? O4A Al2 N4 C28 -93.9(5) . . . . ? Al1 Al2 N4 C28 178.1(4) . . . . ? O4 Al2 N4 Al1 112.5(3) . . . . ? N1 Al2 N4 Al1 -7.22(16) . . . . ? O4A Al2 N4 Al1 88.0(3) . . . . ? Al2 N1 C1 N3 -47.5(6) . . . . ? Al1 N1 C1 N3 146.2(3) . . . . ? Al2 N1 C1 N2 131.7(4) . . . . ? Al1 N1 C1 N2 -34.6(6) . . . . ? C3 N3 C1 N1 179.8(4) . . . . ? C16 N3 C1 N1 0.4(7) . . . . ? C3 N3 C1 N2 0.5(4) . . . . ? C16 N3 C1 N2 -179.0(4) . . . . ? C2 N2 C1 N1 -179.6(4) . . . . ? C4 N2 C1 N1 -21.6(6) . . . . ? C2 N2 C1 N3 -0.3(4) . . . . ? C4 N2 C1 N3 157.7(3) . . . . ? C1 N2 C2 C3 0.0(5) . . . . ? C4 N2 C2 C3 -159.5(4) . . . . ? N2 C2 C3 N3 0.3(5) . . . . ? C1 N3 C3 C2 -0.5(5) . . . . ? C16 N3 C3 C2 179.0(4) . . . . ? C1 N2 C4 C9 -77.4(5) . . . . ? C2 N2 C4 C9 78.3(5) . . . . ? C1 N2 C4 C5 108.1(4) . . . . ? C2 N2 C4 C5 -96.2(4) . . . . ? C9 C4 C5 C6 2.7(6) . . . . ? N2 C4 C5 C6 176.8(4) . . . . ? C9 C4 C5 C10 -175.2(4) . . . . ? N2 C4 C5 C10 -1.0(6) . . . . ? C4 C5 C6 C7 -0.7(7) . . . . ? C10 C5 C6 C7 177.2(4) . . . . ? C5 C6 C7 C8 -1.0(7) . . . . ? C6 C7 C8 C9 0.9(7) . . . . ? C7 C8 C9 C4 1.0(6) . . . . ? C7 C8 C9 C13 -176.7(4) . . . . ? C5 C4 C9 C8 -2.8(6) . . . . ? N2 C4 C9 C8 -177.1(3) . . . . ? C5 C4 C9 C13 174.8(4) . . . . ? N2 C4 C9 C13 0.5(6) . . . . ? C6 C5 C10 C12 31.0(6) . . . . ? C4 C5 C10 C12 -151.2(4) . . . . ? C6 C5 C10 C11 -91.9(5) . . . . ? C4 C5 C10 C11 85.8(5) . . . . ? C8 C9 C13 C15 -60.8(5) . . . . ? C4 C9 C13 C15 121.7(5) . . . . ? C8 C9 C13 C14 62.5(6) . . . . ? C4 C9 C13 C14 -115.0(5) . . . . ? C1 N3 C16 C17 -97.4(5) . . . . ? C3 N3 C16 C17 83.2(5) . . . . ? C1 N3 C16 C21 89.6(5) . . . . ? C3 N3 C16 C21 -89.7(5) . . . . ? C21 C16 C17 C18 -1.4(7) . . . . ? N3 C16 C17 C18 -173.9(4) . . . . ? C21 C16 C17 C22 174.1(5) . . . . ? N3 C16 C17 C22 1.7(7) . . . . ? C16 C17 C18 C19 0.2(8) . . . . ? C22 C17 C18 C19 -175.5(6) . . . . ? C17 C18 C19 C20 0.4(9) . . . . ? C18 C19 C20 C21 0.1(9) . . . . ? C19 C20 C21 C16 -1.2(7) . . . . ? C19 C20 C21 C25 175.9(5) . . . . ? C17 C16 C21 C20 1.9(7) . . . . ? N3 C16 C21 C20 174.4(4) . . . . ? C17 C16 C21 C25 -175.1(4) . . . . ? N3 C16 C21 C25 -2.6(6) . . . . ? C16 C17 C22 C24 144.2(6) . . . . ? C18 C17 C22 C24 -40.3(8) . . . . ? C16 C17 C22 C23 -91.9(6) . . . . ? C18 C17 C22 C23 83.5(6) . . . . ? C20 C21 C25 C26 33.9(6) . . . . ? C16 C21 C25 C26 -149.3(4) . . . . ? C20 C21 C25 C27 -89.8(5) . . . . ? C16 C21 C25 C27 87.0(5) . . . . ? Al1 N4 C28 N5 -30.4(7) . . . . ? Al2 N4 C28 N5 152.3(3) . . . . ? Al1 N4 C28 N6 149.8(3) . . . . ? Al2 N4 C28 N6 -27.4(6) . . . . ? C29 N5 C28 N4 -178.4(4) . . . . ? C31 N5 C28 N4 0.5(7) . . . . ? C29 N5 C28 N6 1.3(4) . . . . ? C31 N5 C28 N6 -179.7(4) . . . . ? C30 N6 C28 N4 179.5(4) . . . . ? C43 N6 C28 N4 -26.7(6) . . . . ? C30 N6 C28 N5 -0.3(4) . . . . ? C43 N6 C28 N5 153.5(4) . . . . ? C28 N5 C29 C30 -1.9(5) . . . . ? C31 N5 C29 C30 179.0(4) . . . . ? N5 C29 C30 N6 1.7(5) . . . . ? C28 N6 C30 C29 -0.9(5) . . . . ? C43 N6 C30 C29 -156.3(4) . . . . ? C28 N5 C31 C36 -102.0(5) . . . . ? C29 N5 C31 C36 76.8(5) . . . . ? C28 N5 C31 C32 86.0(5) . . . . ? C29 N5 C31 C32 -95.1(5) . . . . ? C36 C31 C32 C33 0.3(6) . . . . ? N5 C31 C32 C33 171.9(4) . . . . ? C36 C31 C32 C37 -174.6(4) . . . . ? N5 C31 C32 C37 -3.0(6) . . . . ? C31 C32 C33 C34 -2.0(7) . . . . ? C37 C32 C33 C34 173.0(5) . . . . ? C32 C33 C34 C35 1.9(8) . . . . ? C33 C34 C35 C36 -0.1(9) . . . . ? C32 C31 C36 C35 1.4(7) . . . . ? N5 C31 C36 C35 -170.2(4) . . . . ? C32 C31 C36 C40 179.0(4) . . . . ? N5 C31 C36 C40 7.4(6) . . . . ? C34 C35 C36 C31 -1.5(8) . . . . ? C34 C35 C36 C40 -179.3(5) . . . . ? C33 C32 C37 C39 -90.6(5) . . . . ? C31 C32 C37 C39 84.0(5) . . . . ? C33 C32 C37 C38 32.4(6) . . . . ? C31 C32 C37 C38 -153.0(4) . . . . ? C31 C36 C40 C42 126.6(5) . . . . ? C35 C36 C40 C42 -55.7(6) . . . . ? C31 C36 C40 C41 -110.1(5) . . . . ? C35 C36 C40 C41 67.6(6) . . . . ? C28 N6 C43 C44 -69.6(5) . . . . ? C30 N6 C43 C44 81.5(5) . . . . ? C28 N6 C43 C48 114.7(4) . . . . ? C30 N6 C43 C48 -94.2(5) . . . . ? C48 C43 C44 C45 -2.9(6) . . . . ? N6 C43 C44 C45 -178.6(3) . . . . ? C48 C43 C44 C49 172.9(4) . . . . ? N6 C43 C44 C49 -2.8(6) . . . . ? C43 C44 C45 C46 0.8(6) . . . . ? C49 C44 C45 C46 -175.1(4) . . . . ? C44 C45 C46 C47 1.8(7) . . . . ? C45 C46 C47 C48 -2.4(8) . . . . ? C46 C47 C48 C43 0.4(7) . . . . ? C46 C47 C48 C52 176.3(5) . . . . ? C44 C43 C48 C47 2.3(6) . . . . ? N6 C43 C48 C47 177.9(4) . . . . ? C44 C43 C48 C52 -173.5(4) . . . . ? N6 C43 C48 C52 2.0(6) . . . . ? C45 C44 C49 C51 62.5(5) . . . . ? C43 C44 C49 C51 -113.3(5) . . . . ? C45 C44 C49 C50 -61.5(5) . . . . ? C43 C44 C49 C50 122.7(4) . . . . ? C47 C48 C52 C54 39.4(6) . . . . ? C43 C48 C52 C54 -144.9(5) . . . . ? C47 C48 C52 C53 -82.5(6) . . . . ? C43 C48 C52 C53 93.2(6) . . . . ? C60 O7 C57 C58 35.7(11) . . . . ? C60A O7 C57 C58 10.8(11) . . . . ? C60 O7 C57 C58A 11.3(11) . . . . ? C60A O7 C57 C58A -13.5(10) . . . . ? O7 C57 C58 C59 -44.1(11) . . . . ? C58A C57 C58 C59 26.3(17) . . . . ? C57 C58 C59 C60 33.2(13) . . . . ? C57 O7 C60 C59 -10.2(12) . . . . ? C60A O7 C60 C59 100(3) . . . . ? C58 C59 C60 O7 -14.4(15) . . . . ? C58 C57 C58A C59A -117(3) . . . . ? O7 C57 C58A C59A -0.6(12) . . . . ? C57 C58A C59A C60A 15.3(17) . . . . ? C58A C59A C60A O7 -24.2(18) . . . . ? C60 O7 C60A C59A -52(2) . . . . ? C57 O7 C60A C59A 25.4(16) . . . . ? C64 O8 C61 C62 31.7(7) . . . . ? O8 C61 C62 C63 -29.2(8) . . . . ? C61 C62 C63 C64 17.5(9) . . . . ? C61 O8 C64 C63 -19.6(8) . . . . ? C62 C63 C64 O8 0.2(10) . . . . ? C66 C67 C68 O9 1.7(15) . . . . ? C65 O9 C68 C67 -0.4(13) . . . . ? C68 O9 C65 C66 -1.0(13) . . . . ? O9 C65 C66 C67 2.0(14) . . . . ? C68 C67 C66 C65 -2.3(15) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 67.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.614 _refine_diff_density_min -1.155 _refine_diff_density_rms 0.091 _database_code_depnum_ccdc_archive 'CCDC 962235' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_cu-140a _audit_creation_method ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) ; _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C54 H88 Al2 B4 N6), 3(C7 H8)' _chemical_formula_sum 'C129 H200 Al4 B8 N12' _chemical_formula_weight 2113.41 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 '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 48.7528(13) _cell_length_b 12.0476(3) _cell_length_c 22.9213(5) _cell_angle_alpha 90.00 _cell_angle_beta 105.547(3) _cell_angle_gamma 90.00 _cell_volume 12970.3(6) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 16644 _cell_measurement_theta_min 3.7560 _cell_measurement_theta_max 73.8170 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.082 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4600 _exptl_absorpt_coefficient_mu 0.087 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9711 _exptl_absorpt_correction_T_max 0.9931 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'SuperNova (Cu) X-ray Source' _diffrn_radiation_monochromator mirror _diffrn_measurement_device_type 'SuperNova, Single source at offset, Atlas' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 48749 _diffrn_reflns_av_R_equivalents 0.0730 _diffrn_reflns_av_sigmaI/netI 0.0509 _diffrn_reflns_limit_h_min -60 _diffrn_reflns_limit_h_max 58 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.73 _diffrn_reflns_theta_max 26.31 _reflns_number_total 12943 _reflns_number_gt 10223 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) ; _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^)+(0.0726P)^2^+9.0162P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12943 _refine_ls_number_parameters 865 _refine_ls_number_restraints 585 _refine_ls_R_factor_all 0.0688 _refine_ls_R_factor_gt 0.0529 _refine_ls_wR_factor_ref 0.1514 _refine_ls_wR_factor_gt 0.1366 _refine_ls_goodness_of_fit_ref 1.016 _refine_ls_restrained_S_all 1.068 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group B1 B 0.16850(6) 0.5454(2) 0.39215(11) 0.0425(6) Uani 1 1 d . . . H1A H 0.1733(5) 0.635(2) 0.4106(11) 0.045(6) Uiso 1 1 d . . . H1B H 0.1543(5) 0.557(2) 0.3425(11) 0.047(6) Uiso 1 1 d . . . H1C H 0.1554(6) 0.502(2) 0.4173(12) 0.055(7) Uiso 1 1 d . . . H1D H 0.1877(6) 0.506(2) 0.3897(13) 0.066(8) Uiso 1 1 d . . . B2 B 0.20019(5) 0.7818(2) 0.34753(11) 0.0425(6) Uani 1 1 d . . . H2A H 0.1802(5) 0.814(2) 0.3562(11) 0.050(7) Uiso 1 1 d . . . H2B H 0.1934(5) 0.694(2) 0.3276(11) 0.051(7) Uiso 1 1 d . . . H2C H 0.2168(6) 0.771(2) 0.3901(12) 0.057(7) Uiso 1 1 d . . . H2D H 0.2061(5) 0.8332(19) 0.3101(11) 0.044(6) Uiso 1 1 d . . . B3 B 0.08774(6) 0.9466(2) 0.26997(12) 0.0448(6) Uani 1 1 d . . . H3A H 0.1074(6) 0.915(2) 0.2587(11) 0.054(7) Uiso 1 1 d . . . H3B H 0.0806(5) 0.872(2) 0.2917(11) 0.047(6) Uiso 1 1 d . . . H3C H 0.0713(6) 0.967(2) 0.2269(12) 0.059(7) Uiso 1 1 d . . . H3D H 0.0943(6) 1.016(2) 0.3040(13) 0.068(8) Uiso 1 1 d . . . B4 B 0.06958(5) 0.6684(2) 0.22886(11) 0.0414(5) Uani 1 1 d . . . H4A H 0.0805(5) 0.7432(18) 0.2097(10) 0.035(5) Uiso 1 1 d . . . H4B H 0.0841(5) 0.662(2) 0.2782(11) 0.050(7) Uiso 1 1 d . . . H4C H 0.0720(5) 0.596(2) 0.2027(12) 0.057(7) Uiso 1 1 d . . . H4D H 0.0480(6) 0.698(2) 0.2302(12) 0.065(8) Uiso 1 1 d . . . Al1 Al 0.158204(11) 0.70300(5) 0.33989(2) 0.02643(13) Uani 1 1 d . . . Al2 Al 0.105270(11) 0.77532(5) 0.27884(2) 0.02689(13) Uani 1 1 d . . . N1 N 0.12614(3) 0.76151(12) 0.35997(6) 0.0262(3) Uani 1 1 d . . . N2 N 0.13857(3) 0.82557(13) 0.46386(7) 0.0285(3) Uani 1 1 d . . . N3 N 0.09437(3) 0.77657(14) 0.42506(7) 0.0315(3) Uani 1 1 d . . . N4 N 0.13758(3) 0.71884(12) 0.25820(6) 0.0253(3) Uani 1 1 d . . . N5 N 0.13271(3) 0.75322(12) 0.15189(6) 0.0258(3) Uani 1 1 d . . . N6 N 0.15863(3) 0.61060(12) 0.19200(6) 0.0267(3) Uani 1 1 d . . . C1 C 0.12027(4) 0.78535(15) 0.41149(8) 0.0271(4) Uani 1 1 d . . . C2 C 0.12402(4) 0.84173(18) 0.50801(8) 0.0354(4) Uani 1 1 d . . . H2E H 0.1319 0.8693 0.5478 0.043 Uiso 1 1 calc R . . C3 C 0.09719(4) 0.81161(19) 0.48435(8) 0.0377(5) Uani 1 1 d . . . H3E H 0.0824 0.8136 0.5043 0.045 Uiso 1 1 calc R . . C4 C 0.16741(4) 0.86536(16) 0.47358(8) 0.0308(4) Uani 1 1 d . . . C5 C 0.17150(5) 0.96997(17) 0.45105(10) 0.0398(5) Uani 1 1 d . . . C6 C 0.19948(6) 1.0091(2) 0.46404(13) 0.0548(7) Uani 1 1 d . . . H6A H 0.2032 1.0788 0.4484 0.066 Uiso 1 1 calc R . . C7 C 0.22173(5) 0.9483(2) 0.49911(14) 0.0618(7) Uani 1 1 d . . . H7A H 0.2406 0.9766 0.5073 0.074 Uiso 1 1 calc R . . C8 C 0.21712(5) 0.8473(2) 0.52248(12) 0.0505(6) Uani 1 1 d . . . H8A H 0.2328 0.8071 0.5471 0.061 Uiso 1 1 calc R . . C9 C 0.18966(4) 0.80283(17) 0.51050(9) 0.0354(4) Uani 1 1 d . . . C10 C 0.14649(6) 1.04074(19) 0.41707(10) 0.0502(6) Uani 1 1 d . . . H10A H 0.1309 0.9899 0.3952 0.060 Uiso 1 1 calc R . . C11 C 0.15353(10) 1.1182(3) 0.37072(15) 0.0899(12) Uani 1 1 d . . . H11A H 0.1629 1.0761 0.3449 0.135 Uiso 1 1 calc R . . H11B H 0.1663 1.1770 0.3917 0.135 Uiso 1 1 calc R . . H11C H 0.1359 1.1514 0.3457 0.135 Uiso 1 1 calc R . . C12 C 0.13521(8) 1.1111(3) 0.46081(14) 0.0789(10) Uani 1 1 d . . . H12A H 0.1182 1.1512 0.4383 0.118 Uiso 1 1 calc R . . H12B H 0.1498 1.1645 0.4812 0.118 Uiso 1 1 calc R . . H12C H 0.1304 1.0630 0.4911 0.118 Uiso 1 1 calc R . . C13 C 0.18522(4) 0.69441(18) 0.54002(9) 0.0385(4) Uani 1 1 d . . . H13A H 0.1663 0.6635 0.5174 0.046 Uiso 1 1 calc R . . C14 C 0.20819(5) 0.6079(2) 0.53862(11) 0.0525(6) Uani 1 1 d . . . H14A H 0.2109 0.6045 0.4978 0.079 Uiso 1 1 calc R . . H14B H 0.2022 0.5350 0.5496 0.079 Uiso 1 1 calc R . . H14C H 0.2261 0.6290 0.5676 0.079 Uiso 1 1 calc R . . C15 C 0.18471(5) 0.7138(2) 0.60599(10) 0.0479(5) Uani 1 1 d . . . H15A H 0.1691 0.7643 0.6069 0.072 Uiso 1 1 calc R . . H15B H 0.2028 0.7466 0.6287 0.072 Uiso 1 1 calc R . . H15C H 0.1819 0.6428 0.6244 0.072 Uiso 1 1 calc R . . C16 C 0.06788(4) 0.72795(18) 0.39032(8) 0.0333(4) Uani 1 1 d . . . C17 C 0.04433(4) 0.79847(19) 0.36900(9) 0.0371(4) Uani 1 1 d . . . C18 C 0.01843(4) 0.7487(2) 0.34035(10) 0.0453(5) Uani 1 1 d . . . H18A H 0.0022 0.7940 0.3243 0.054 Uiso 1 1 calc R . . C19 C 0.01590(5) 0.6355(2) 0.33481(10) 0.0500(6) Uani 1 1 d . . . H19A H -0.0020 0.6035 0.3153 0.060 Uiso 1 1 calc R . . C20 C 0.03913(5) 0.5678(2) 0.35732(10) 0.0466(5) Uani 1 1 d . . . H20A H 0.0369 0.4895 0.3533 0.056 Uiso 1 1 calc R . . C21 C 0.06583(4) 0.61208(18) 0.38588(9) 0.0380(4) Uani 1 1 d . . . C22 C 0.04545(4) 0.9239(2) 0.37748(10) 0.0426(5) Uani 1 1 d . . . H22A H 0.0659 0.9476 0.3879 0.051 Uiso 1 1 calc R . . C23 C 0.03308(5) 0.9576(2) 0.42972(11) 0.0540(6) Uani 1 1 d . . . H23A H 0.0443 0.9234 0.4674 0.081 Uiso 1 1 calc R . . H23B H 0.0133 0.9324 0.4211 0.081 Uiso 1 1 calc R . . H23C H 0.0338 1.0385 0.4341 0.081 Uiso 1 1 calc R . . C24 C 0.02933(5) 0.9867(2) 0.32049(12) 0.0572(6) Uani 1 1 d . . . H24A H 0.0353 0.9594 0.2856 0.086 Uiso 1 1 calc R . . H24B H 0.0335 1.0662 0.3259 0.086 Uiso 1 1 calc R . . H24C H 0.0088 0.9747 0.3136 0.086 Uiso 1 1 calc R . . C25 C 0.09136(5) 0.53767(19) 0.41155(10) 0.0452(5) Uani 1 1 d . . . H25A H 0.1080 0.5722 0.4009 0.054 Uiso 1 1 calc R . . C26 C 0.08779(6) 0.4210(2) 0.38460(12) 0.0588(6) Uani 1 1 d . . . H26A H 0.0822 0.4260 0.3403 0.088 Uiso 1 1 calc R . . H26B H 0.0730 0.3815 0.3982 0.088 Uiso 1 1 calc R . . H26C H 0.1058 0.3808 0.3980 0.088 Uiso 1 1 calc R . . C27 C 0.09882(7) 0.5295(2) 0.48028(12) 0.0658(8) Uani 1 1 d . . . H27A H 0.1152 0.4800 0.4946 0.099 Uiso 1 1 calc R . . H27B H 0.0825 0.4999 0.4926 0.099 Uiso 1 1 calc R . . H27C H 0.1036 0.6034 0.4979 0.099 Uiso 1 1 calc R . . C28 C 0.14263(3) 0.69596(14) 0.20589(8) 0.0243(3) Uani 1 1 d . . . C29 C 0.14252(4) 0.70237(15) 0.10667(8) 0.0301(4) Uani 1 1 d . . . H29A H 0.1387 0.7257 0.0657 0.036 Uiso 1 1 calc R . . C30 C 0.15820(4) 0.61573(16) 0.13099(8) 0.0316(4) Uani 1 1 d . . . H30A H 0.1675 0.5659 0.1105 0.038 Uiso 1 1 calc R . . C31 C 0.12008(4) 0.86247(15) 0.14336(8) 0.0274(4) Uani 1 1 d . . . C32 C 0.13795(4) 0.95408(16) 0.16461(8) 0.0304(4) Uani 1 1 d . . . C33 C 0.12542(5) 1.05883(16) 0.15631(9) 0.0366(4) Uani 1 1 d . . . H33A H 0.1366 1.1222 0.1716 0.044 Uiso 1 1 calc R . . C34 C 0.09703(5) 1.07247(17) 0.12632(10) 0.0409(5) Uani 1 1 d . . . H34A H 0.0888 1.1446 0.1218 0.049 Uiso 1 1 calc R . . C35 C 0.08054(4) 0.98157(18) 0.10292(9) 0.0380(5) Uani 1 1 d . . . H35A H 0.0612 0.9924 0.0809 0.046 Uiso 1 1 calc R . . C36 C 0.09156(4) 0.87388(16) 0.11082(8) 0.0309(4) Uani 1 1 d . . . C37 C 0.16965(4) 0.94025(17) 0.19194(9) 0.0371(4) Uani 1 1 d . . . H37A H 0.1729 0.8687 0.2149 0.045 Uiso 1 1 calc R . . C38 C 0.18282(5) 1.0333(2) 0.23543(11) 0.0526(6) Uani 1 1 d . . . H38A H 0.1715 1.0452 0.2643 0.079 Uiso 1 1 calc R . . H38B H 0.1832 1.1017 0.2125 0.079 Uiso 1 1 calc R . . H38C H 0.2023 1.0129 0.2575 0.079 Uiso 1 1 calc R . . C39 C 0.18509(5) 0.9338(2) 0.14161(12) 0.0559(6) Uani 1 1 d . . . H39A H 0.1763 0.8761 0.1125 0.084 Uiso 1 1 calc R . . H39B H 0.2052 0.9158 0.1595 0.084 Uiso 1 1 calc R . . H39C H 0.1836 1.0056 0.1208 0.084 Uiso 1 1 calc R . . C40 C 0.07285(4) 0.77648(18) 0.08260(9) 0.0373(4) Uani 1 1 d . . . H40A H 0.0811 0.7074 0.1046 0.045 Uiso 1 1 calc R . . C41 C 0.07243(5) 0.7633(2) 0.01565(10) 0.0502(6) Uani 1 1 d . . . H41A H 0.0916 0.7451 0.0127 0.075 Uiso 1 1 calc R . . H41B H 0.0661 0.8330 -0.0059 0.075 Uiso 1 1 calc R . . H41C H 0.0593 0.7036 -0.0026 0.075 Uiso 1 1 calc R . . C42 C 0.04215(5) 0.7886(2) 0.08694(11) 0.0507(6) Uani 1 1 d . . . H42A H 0.0423 0.8091 0.1284 0.076 Uiso 1 1 calc R . . H42B H 0.0321 0.7180 0.0763 0.076 Uiso 1 1 calc R . . H42C H 0.0325 0.8466 0.0589 0.076 Uiso 1 1 calc R . . C43 C 0.17203(4) 0.51726(15) 0.22841(8) 0.0284(4) Uani 1 1 d . . . C44 C 0.20182(4) 0.51413(16) 0.24849(8) 0.0340(4) Uani 1 1 d . . . C45 C 0.21410(5) 0.41735(18) 0.27773(10) 0.0426(5) Uani 1 1 d . . . H45A H 0.2342 0.4124 0.2920 0.051 Uiso 1 1 calc R . . C46 C 0.19774(5) 0.32909(18) 0.28634(10) 0.0454(5) Uani 1 1 d . . . H46A H 0.2066 0.2644 0.3065 0.055 Uiso 1 1 calc R . . C47 C 0.16846(5) 0.33415(17) 0.26574(9) 0.0396(5) Uani 1 1 d . . . H47A H 0.1574 0.2726 0.2721 0.048 Uiso 1 1 calc R . . C48 C 0.15469(4) 0.42752(16) 0.23583(8) 0.0321(4) Uani 1 1 d . . . C49 C 0.22091(4) 0.60582(19) 0.23673(10) 0.0407(5) Uani 1 1 d . . . H49A H 0.2092 0.6745 0.2255 0.049 Uiso 1 1 calc R . . C50 C 0.23287(5) 0.5747(3) 0.18348(11) 0.0601(7) Uani 1 1 d . . . H50A H 0.2432 0.5044 0.1922 0.090 Uiso 1 1 calc R . . H50B H 0.2458 0.6332 0.1775 0.090 Uiso 1 1 calc R . . H50C H 0.2172 0.5669 0.1467 0.090 Uiso 1 1 calc R . . C51 C 0.24580(5) 0.6323(2) 0.29197(11) 0.0503(6) Uani 1 1 d . . . H51A H 0.2386 0.6421 0.3277 0.075 Uiso 1 1 calc R . . H51B H 0.2552 0.7006 0.2845 0.075 Uiso 1 1 calc R . . H51C H 0.2595 0.5709 0.2991 0.075 Uiso 1 1 calc R . . C52 C 0.12258(4) 0.43045(17) 0.21057(9) 0.0374(4) Uani 1 1 d . . . H52 H 0.1160 0.5079 0.2150 0.045 Uiso 1 1 calc R . . C53 C 0.11375(5) 0.4012(2) 0.14324(10) 0.0499(6) Uani 1 1 d . . . H53A H 0.1216 0.4561 0.1207 0.075 Uiso 1 1 calc R . . H53B H 0.0929 0.4013 0.1285 0.075 Uiso 1 1 calc R . . H53C H 0.1210 0.3273 0.1374 0.075 Uiso 1 1 calc R . . C54 C 0.10735(5) 0.3527(2) 0.24431(12) 0.0539(6) Uani 1 1 d . . . H54A H 0.1100 0.2757 0.2331 0.081 Uiso 1 1 calc R . . H54B H 0.0870 0.3705 0.2334 0.081 Uiso 1 1 calc R . . H54C H 0.1153 0.3621 0.2881 0.081 Uiso 1 1 calc R . . C55 C 0.02846(16) 0.7307(7) 0.6240(3) 0.0834(11) Uani 0.523(5) 1 d PDU A 1 C56 C 0.02784(19) 0.7675(7) 0.5676(4) 0.0860(12) Uani 0.523(5) 1 d PDU A 1 H56A H 0.0280 0.8450 0.5599 0.103 Uiso 0.523(5) 1 calc PR A 1 C57 C 0.0271(6) 0.6931(8) 0.5215(5) 0.0841(12) Uani 0.523(5) 1 d PDU A 1 H57A H 0.0259 0.7193 0.4819 0.101 Uiso 0.523(5) 1 calc PR A 1 C58 C 0.02792(19) 0.5830(7) 0.5328(3) 0.0859(12) Uani 0.523(5) 1 d PDU A 1 H58A H 0.0282 0.5313 0.5016 0.103 Uiso 0.523(5) 1 calc PR A 1 C59 C 0.02839(16) 0.5461(6) 0.5906(3) 0.0851(13) Uani 0.523(5) 1 d PDU A 1 H59A H 0.0280 0.4686 0.5979 0.102 Uiso 0.523(5) 1 calc PR A 1 C60 C 0.0294(2) 0.6194(7) 0.6378(3) 0.0829(13) Uani 0.523(5) 1 d PDU A 1 H60A H 0.0306 0.5939 0.6777 0.099 Uiso 0.523(5) 1 calc PR A 1 C61 C 0.03023(18) 0.8038(8) 0.6764(4) 0.110(2) Uani 0.523(5) 1 d PU A 1 H61A H 0.0309 0.7586 0.7123 0.165 Uiso 0.523(5) 1 calc PR A 1 H61B H 0.0135 0.8523 0.6681 0.165 Uiso 0.523(5) 1 calc PR A 1 H61C H 0.0475 0.8493 0.6837 0.165 Uiso 0.523(5) 1 calc PR A 1 C55A C 0.02458(19) 0.6868(8) 0.6472(4) 0.0889(13) Uani 0.477(5) 1 d PDU A 2 C56A C 0.02195(18) 0.7871(7) 0.6156(4) 0.0883(13) Uani 0.477(5) 1 d PDU A 2 H56B H 0.0207 0.8553 0.6355 0.106 Uiso 0.477(5) 1 calc PR A 2 C57A C 0.0212(2) 0.7856(8) 0.5569(4) 0.0854(12) Uani 0.477(5) 1 d PDU A 2 H57B H 0.0173 0.8527 0.5344 0.102 Uiso 0.477(5) 1 calc PR A 2 C58A C 0.0259(7) 0.6899(10) 0.5276(5) 0.0864(13) Uani 0.477(5) 1 d PDU A 2 H58B H 0.0262 0.6915 0.4863 0.104 Uiso 0.477(5) 1 calc PR A 2 C59A C 0.0300(2) 0.5950(8) 0.5591(4) 0.0900(13) Uani 0.477(5) 1 d PDU A 2 H59B H 0.0335 0.5284 0.5401 0.108 Uiso 0.477(5) 1 calc PR A 2 C60A C 0.0292(2) 0.5925(7) 0.6182(4) 0.0870(13) Uani 0.477(5) 1 d PDU A 2 H60B H 0.0320 0.5241 0.6396 0.104 Uiso 0.477(5) 1 calc PR A 2 C61A C 0.0244(2) 0.6659(10) 0.7129(4) 0.119(3) Uani 0.477(5) 1 d PU A 2 H61D H 0.0270 0.5865 0.7219 0.178 Uiso 0.477(5) 1 calc PR A 2 H61E H 0.0062 0.6903 0.7188 0.178 Uiso 0.477(5) 1 calc PR A 2 H61F H 0.0399 0.7076 0.7400 0.178 Uiso 0.477(5) 1 calc PR A 2 C62 C 0.2067(2) 0.2887(9) 0.5227(4) 0.100(2) Uani 0.50 1 d PU B -3 H62A H 0.1937 0.3244 0.4877 0.150 Uiso 0.50 1 calc PR B -3 H62B H 0.2101 0.3384 0.5578 0.150 Uiso 0.50 1 calc PR B -3 H62C H 0.1983 0.2192 0.5319 0.150 Uiso 0.50 1 calc PR B -3 C63 C 0.23443(15) 0.2644(5) 0.5086(3) 0.0733(13) Uani 0.50 1 d PDU B -3 C64 C 0.2584(2) 0.2065(12) 0.5417(5) 0.0837(18) Uani 0.50 1 d PDU B -3 H64A H 0.2588 0.1797 0.5809 0.100 Uiso 0.50 1 calc PR B -3 C65 C 0.28111(16) 0.1874(5) 0.5193(3) 0.0911(16) Uani 0.50 1 d PDU B -3 H65A H 0.2969 0.1460 0.5423 0.109 Uiso 0.50 1 calc PR B -3 C66 C 0.28115(16) 0.2300(8) 0.4607(4) 0.0817(16) Uani 0.50 1 d PDU B -3 H66A H 0.2967 0.2180 0.4437 0.098 Uiso 0.50 1 calc PR B -3 C67 C 0.25887(14) 0.2856(5) 0.4324(3) 0.0696(12) Uani 0.50 1 d PDU B -3 H67A H 0.2589 0.3161 0.3942 0.084 Uiso 0.50 1 calc PR B -3 C68 C 0.23467(19) 0.3048(11) 0.4530(4) 0.0644(13) Uani 0.50 1 d PDU B -3 H68A H 0.2189 0.3449 0.4290 0.077 Uiso 0.50 1 calc PR B -3 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 B1 0.0499(14) 0.0418(14) 0.0342(12) 0.0070(10) 0.0082(11) 0.0138(11) B2 0.0318(12) 0.0566(16) 0.0378(12) -0.0064(11) 0.0075(10) 0.0017(11) B3 0.0546(15) 0.0463(14) 0.0383(13) 0.0102(11) 0.0206(12) 0.0170(12) B4 0.0318(12) 0.0563(15) 0.0339(12) -0.0016(10) 0.0053(9) -0.0027(11) Al1 0.0260(3) 0.0303(3) 0.0220(3) 0.0004(2) 0.0046(2) 0.0042(2) Al2 0.0253(3) 0.0332(3) 0.0223(3) 0.0027(2) 0.0065(2) 0.0040(2) N1 0.0268(7) 0.0295(8) 0.0227(7) 0.0012(6) 0.0070(6) 0.0013(6) N2 0.0263(7) 0.0359(8) 0.0236(7) -0.0005(6) 0.0071(6) -0.0001(6) N3 0.0243(8) 0.0456(9) 0.0242(7) -0.0001(6) 0.0058(6) -0.0007(7) N4 0.0256(7) 0.0266(7) 0.0231(7) 0.0002(6) 0.0056(6) 0.0021(6) N5 0.0267(7) 0.0275(8) 0.0231(7) 0.0017(6) 0.0066(6) 0.0028(6) N6 0.0284(7) 0.0264(7) 0.0249(7) 0.0003(6) 0.0065(6) 0.0032(6) C1 0.0245(8) 0.0312(9) 0.0247(8) 0.0024(7) 0.0051(7) 0.0028(7) C2 0.0328(10) 0.0506(12) 0.0244(9) -0.0029(8) 0.0103(7) 0.0009(9) C3 0.0309(10) 0.0584(13) 0.0255(9) -0.0022(8) 0.0107(8) 0.0020(9) C4 0.0306(9) 0.0340(10) 0.0296(9) -0.0072(7) 0.0113(7) -0.0048(8) C5 0.0536(13) 0.0328(10) 0.0405(11) -0.0077(8) 0.0257(10) -0.0042(9) C6 0.0661(16) 0.0389(12) 0.0736(17) -0.0159(11) 0.0431(14) -0.0182(12) C7 0.0410(13) 0.0570(16) 0.096(2) -0.0299(15) 0.0332(14) -0.0178(12) C8 0.0296(11) 0.0548(14) 0.0658(15) -0.0210(12) 0.0107(10) -0.0061(10) C9 0.0296(10) 0.0392(11) 0.0374(10) -0.0119(8) 0.0093(8) -0.0026(8) C10 0.0746(17) 0.0353(11) 0.0420(12) 0.0039(9) 0.0177(11) 0.0010(11) C11 0.163(4) 0.0586(18) 0.0621(18) 0.0157(14) 0.054(2) 0.006(2) C12 0.105(3) 0.0713(19) 0.0724(19) 0.0208(15) 0.0454(18) 0.0444(18) C13 0.0332(10) 0.0413(11) 0.0357(10) -0.0043(8) 0.0002(8) 0.0038(8) C14 0.0522(14) 0.0550(14) 0.0421(12) -0.0045(10) -0.0016(10) 0.0180(11) C15 0.0521(13) 0.0519(13) 0.0364(11) -0.0021(9) 0.0062(10) 0.0037(11) C16 0.0284(9) 0.0488(12) 0.0236(8) -0.0001(8) 0.0082(7) -0.0040(8) C17 0.0279(9) 0.0553(13) 0.0282(9) 0.0000(8) 0.0076(7) -0.0014(9) C18 0.0279(10) 0.0663(15) 0.0405(11) -0.0028(10) 0.0069(9) -0.0007(10) C19 0.0314(11) 0.0720(17) 0.0451(12) -0.0086(11) 0.0081(9) -0.0139(11) C20 0.0456(13) 0.0540(14) 0.0429(12) -0.0052(10) 0.0164(10) -0.0142(10) C21 0.0383(11) 0.0497(12) 0.0284(9) 0.0006(8) 0.0133(8) -0.0063(9) C22 0.0282(10) 0.0534(13) 0.0446(12) 0.0011(10) 0.0068(9) 0.0023(9) C23 0.0480(13) 0.0615(16) 0.0517(14) -0.0115(11) 0.0121(11) 0.0050(11) C24 0.0430(13) 0.0674(17) 0.0598(15) 0.0131(12) 0.0112(11) 0.0160(12) C25 0.0485(13) 0.0448(12) 0.0444(12) 0.0108(9) 0.0162(10) -0.0001(10) C26 0.0741(18) 0.0534(15) 0.0543(14) 0.0018(11) 0.0268(13) 0.0052(13) C27 0.089(2) 0.0571(16) 0.0453(14) 0.0123(12) 0.0070(13) 0.0080(15) C28 0.0207(8) 0.0250(8) 0.0258(8) 0.0006(6) 0.0037(6) -0.0007(6) C29 0.0364(10) 0.0312(9) 0.0237(8) 0.0004(7) 0.0099(7) 0.0026(8) C30 0.0375(10) 0.0320(10) 0.0274(9) -0.0027(7) 0.0123(8) 0.0023(8) C31 0.0319(9) 0.0284(9) 0.0240(8) 0.0038(7) 0.0114(7) 0.0044(7) C32 0.0356(10) 0.0315(10) 0.0275(9) 0.0009(7) 0.0142(7) 0.0000(8) C33 0.0469(12) 0.0279(10) 0.0402(10) 0.0024(8) 0.0205(9) 0.0004(8) C34 0.0511(13) 0.0337(11) 0.0436(11) 0.0086(9) 0.0224(10) 0.0123(9) C35 0.0366(10) 0.0444(12) 0.0343(10) 0.0078(8) 0.0119(8) 0.0122(9) C36 0.0307(9) 0.0383(10) 0.0250(8) 0.0049(7) 0.0095(7) 0.0058(8) C37 0.0356(10) 0.0315(10) 0.0438(11) 0.0004(8) 0.0097(9) -0.0033(8) C38 0.0494(14) 0.0585(15) 0.0502(13) -0.0144(11) 0.0141(11) -0.0128(11) C39 0.0392(12) 0.0645(16) 0.0695(16) -0.0251(13) 0.0241(12) -0.0090(11) C40 0.0313(10) 0.0443(11) 0.0329(10) 0.0028(8) 0.0026(8) 0.0023(8) C41 0.0488(13) 0.0601(15) 0.0379(11) -0.0080(10) 0.0049(10) 0.0037(11) C42 0.0304(11) 0.0705(16) 0.0467(13) 0.0035(11) 0.0025(9) -0.0011(10) C43 0.0320(9) 0.0265(9) 0.0252(8) -0.0007(7) 0.0052(7) 0.0064(7) C44 0.0344(10) 0.0360(10) 0.0284(9) -0.0042(8) 0.0030(8) 0.0060(8) C45 0.0379(11) 0.0439(12) 0.0399(11) -0.0005(9) -0.0003(9) 0.0140(9) C46 0.0575(14) 0.0358(11) 0.0381(11) 0.0052(9) 0.0044(10) 0.0152(10) C47 0.0525(13) 0.0305(10) 0.0356(10) 0.0024(8) 0.0112(9) 0.0042(9) C48 0.0405(10) 0.0297(9) 0.0267(9) -0.0019(7) 0.0101(8) 0.0025(8) C49 0.0309(10) 0.0450(12) 0.0426(11) -0.0029(9) 0.0035(8) 0.0002(9) C50 0.0459(14) 0.088(2) 0.0484(13) -0.0096(13) 0.0159(11) -0.0161(13) C51 0.0311(11) 0.0636(15) 0.0510(13) -0.0145(11) 0.0022(9) 0.0027(10) C52 0.0362(10) 0.0333(10) 0.0433(11) -0.0003(8) 0.0117(9) -0.0008(8) C53 0.0415(12) 0.0621(15) 0.0417(12) 0.0039(10) 0.0032(9) -0.0107(11) C54 0.0527(14) 0.0617(16) 0.0528(14) 0.0019(11) 0.0237(11) -0.0094(12) C55 0.065(2) 0.097(3) 0.087(2) 0.014(2) 0.017(2) -0.006(2) C56 0.067(3) 0.095(2) 0.088(2) 0.0201(18) 0.008(2) -0.012(2) C57 0.061(2) 0.105(2) 0.082(2) 0.0172(18) 0.012(2) -0.015(2) C58 0.068(2) 0.105(2) 0.080(3) 0.014(2) 0.011(3) -0.009(2) C59 0.074(2) 0.097(3) 0.082(3) 0.016(2) 0.017(2) -0.013(2) C60 0.068(2) 0.094(3) 0.084(2) 0.016(2) 0.017(3) -0.013(3) C61 0.093(4) 0.120(4) 0.118(3) -0.015(3) 0.031(4) 0.006(4) C55A 0.069(2) 0.106(3) 0.091(2) 0.019(2) 0.020(2) 0.004(3) C56A 0.070(3) 0.099(3) 0.088(2) 0.013(2) 0.007(2) 0.001(3) C57A 0.064(3) 0.101(2) 0.085(2) 0.015(2) 0.009(2) -0.012(2) C58A 0.064(2) 0.104(2) 0.084(2) 0.0133(19) 0.007(2) -0.013(2) C59A 0.072(2) 0.104(2) 0.088(3) 0.013(2) 0.011(3) -0.009(2) C60A 0.069(2) 0.097(3) 0.092(3) 0.021(2) 0.016(3) -0.007(2) C61A 0.095(5) 0.172(7) 0.098(4) 0.031(4) 0.040(4) 0.013(5) C62 0.140(6) 0.080(5) 0.087(5) -0.036(4) 0.041(4) -0.023(5) C63 0.114(4) 0.046(3) 0.053(2) -0.007(2) 0.010(2) -0.025(3) C64 0.125(4) 0.047(3) 0.059(3) 0.004(2) -0.010(3) -0.031(3) C65 0.110(4) 0.048(3) 0.088(3) -0.006(2) -0.019(3) -0.015(3) C66 0.087(4) 0.056(3) 0.088(3) -0.019(3) 0.000(3) -0.012(3) C67 0.085(3) 0.050(3) 0.064(3) -0.008(2) 0.003(2) -0.016(2) C68 0.093(4) 0.040(3) 0.050(3) -0.001(2) 0.003(3) -0.011(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag B1 Al1 2.229(3) . ? B1 H1A 1.16(2) . ? B1 H1B 1.17(2) . ? B1 H1C 1.10(3) . ? B1 H1D 1.07(3) . ? B2 Al1 2.220(3) . ? B2 H2A 1.12(3) . ? B2 H2B 1.16(3) . ? B2 H2C 1.10(3) . ? B2 H2D 1.16(2) . ? B3 Al2 2.222(3) . ? B3 H3A 1.12(3) . ? B3 H3B 1.13(2) . ? B3 H3C 1.12(3) . ? B3 H3D 1.13(3) . ? B4 Al2 2.220(3) . ? B4 H4A 1.19(2) . ? B4 H4B 1.17(2) . ? B4 H4C 1.08(3) . ? B4 H4D 1.12(3) . ? Al1 N1 1.8810(15) . ? Al1 N4 1.8828(15) . ? Al1 Al2 2.7278(7) . ? Al1 H1A 1.79(2) . ? Al1 H1B 1.77(2) . ? Al1 H2A 1.69(2) . ? Al1 H2B 1.82(2) . ? Al2 N1 1.8727(15) . ? Al2 N4 1.8887(15) . ? Al2 H3A 1.75(3) . ? Al2 H3B 1.76(2) . ? Al2 H4A 1.76(2) . ? Al2 H4B 1.71(2) . ? N1 C1 1.319(2) . ? N2 C1 1.377(2) . ? N2 C2 1.396(2) . ? N2 C4 1.446(2) . ? N3 C1 1.383(2) . ? N3 C3 1.394(2) . ? N3 C16 1.447(2) . ? N4 C28 1.316(2) . ? N5 C28 1.386(2) . ? N5 C29 1.394(2) . ? N5 C31 1.444(2) . ? N6 C28 1.379(2) . ? N6 C30 1.394(2) . ? N6 C43 1.448(2) . ? C2 C3 1.326(3) . ? C2 H2E 0.9500 . ? C3 H3E 0.9500 . ? C4 C5 1.396(3) . ? C4 C9 1.403(3) . ? C5 C6 1.398(3) . ? C5 C10 1.520(3) . ? C6 C7 1.375(4) . ? C6 H6A 0.9500 . ? C7 C8 1.371(4) . ? C7 H7A 0.9500 . ? C8 C9 1.399(3) . ? C8 H8A 0.9500 . ? C9 C13 1.513(3) . ? C10 C11 1.521(3) . ? C10 C12 1.524(4) . ? C10 H10A 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.536(3) . ? C13 C15 1.537(3) . ? C13 H13A 1.0000 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C21 1.401(3) . ? C16 C17 1.406(3) . ? C17 C18 1.393(3) . ? C17 C22 1.523(3) . ? C18 C19 1.372(4) . ? C18 H18A 0.9500 . ? C19 C20 1.379(4) . ? C19 H19A 0.9500 . ? C20 C21 1.397(3) . ? C20 H20A 0.9500 . ? C21 C25 1.519(3) . ? C22 C24 1.532(3) . ? C22 C23 1.533(3) . ? C22 H22A 1.0000 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C27 1.522(3) . ? C25 C26 1.526(3) . ? C25 H25A 1.0000 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C29 C30 1.325(3) . ? C29 H29A 0.9500 . ? C30 H30A 0.9500 . ? C31 C36 1.397(3) . ? C31 C32 1.410(3) . ? C32 C33 1.393(3) . ? C32 C37 1.513(3) . ? C33 C34 1.380(3) . ? C33 H33A 0.9500 . ? C34 C35 1.379(3) . ? C34 H34A 0.9500 . ? C35 C36 1.397(3) . ? C35 H35A 0.9500 . ? C36 C40 1.520(3) . ? C37 C38 1.523(3) . ? C37 C39 1.539(3) . ? C37 H37A 1.0000 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 C42 1.533(3) . ? C40 C41 1.537(3) . ? C40 H40A 1.0000 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 C44 1.402(3) . ? C43 C48 1.411(3) . ? C44 C45 1.397(3) . ? C44 C49 1.514(3) . ? C45 C46 1.375(3) . ? C45 H45A 0.9500 . ? C46 C47 1.380(3) . ? C46 H46A 0.9500 . ? C47 C48 1.393(3) . ? C47 H47A 0.9500 . ? C48 C52 1.517(3) . ? C49 C50 1.533(3) . ? C49 C51 1.534(3) . ? C49 H49A 1.0000 . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C52 C54 1.528(3) . ? C52 C53 1.528(3) . ? C52 H52 1.0000 . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C55 C56 1.361(9) . ? C55 C60 1.376(9) . ? C55 C61 1.473(11) . ? C56 C57 1.377(10) . ? C56 H56A 0.9500 . ? C57 C58 1.350(9) . ? C57 H57A 0.9500 . ? C58 C59 1.391(8) . ? C58 H58A 0.9500 . ? C59 C60 1.388(8) . ? C59 H59A 0.9500 . ? C60 H60A 0.9500 . ? C61 H61A 0.9800 . ? C61 H61B 0.9800 . ? C61 H61C 0.9800 . ? C55A C60A 1.364(9) . ? C55A C56A 1.397(9) . ? C55A C61A 1.529(11) . ? C56A C57A 1.336(9) . ? C56A H56B 0.9500 . ? C57A C58A 1.383(10) . ? C57A H57B 0.9500 . ? C58A C59A 1.338(10) . ? C58A H58B 0.9500 . ? C59A C60A 1.366(9) . ? C59A H59B 0.9500 . ? C60A H60B 0.9500 . ? C61A H61D 0.9800 . ? C61A H61E 0.9800 . ? C61A H61F 0.9800 . ? C62 C63 1.500(12) . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C62 H62C 0.9800 . ? C63 C68 1.367(9) . ? C63 C64 1.397(9) . ? C64 C65 1.360(10) . ? C64 H64A 0.9500 . ? C65 C66 1.438(10) . ? C65 H65A 0.9500 . ? C66 C67 1.292(8) . ? C66 H66A 0.9500 . ? C67 C68 1.403(9) . ? C67 H67A 0.9500 . ? C68 H68A 0.9500 . ? 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 B1 H1A 52.9(12) . . ? Al1 B1 H1B 52.3(12) . . ? H1A B1 H1B 104.7(16) . . ? Al1 B1 H1C 127.4(14) . . ? H1A B1 H1C 110.0(18) . . ? H1B B1 H1C 106.8(18) . . ? Al1 B1 H1D 115.4(15) . . ? H1A B1 H1D 110.1(19) . . ? H1B B1 H1D 107.5(19) . . ? H1C B1 H1D 117(2) . . ? Al1 B2 H2A 47.8(13) . . ? Al1 B2 H2B 54.7(12) . . ? H2A B2 H2B 102.3(17) . . ? Al1 B2 H2C 117.7(14) . . ? H2A B2 H2C 111.0(19) . . ? H2B B2 H2C 107.8(18) . . ? Al1 B2 H2D 125.4(12) . . ? H2A B2 H2D 110.7(17) . . ? H2B B2 H2D 107.1(17) . . ? H2C B2 H2D 116.9(18) . . ? Al2 B3 H3A 51.1(13) . . ? Al2 B3 H3B 51.4(12) . . ? H3A B3 H3B 102.2(17) . . ? Al2 B3 H3C 116.8(14) . . ? H3A B3 H3C 109.0(19) . . ? H3B B3 H3C 109.3(18) . . ? Al2 B3 H3D 126.3(15) . . ? H3A B3 H3D 108(2) . . ? H3B B3 H3D 110.2(19) . . ? H3C B3 H3D 117(2) . . ? Al2 B4 H4A 52.0(10) . . ? Al2 B4 H4B 49.5(12) . . ? H4A B4 H4B 101.2(16) . . ? Al2 B4 H4C 124.6(14) . . ? H4A B4 H4C 106.4(17) . . ? H4B B4 H4C 110.6(18) . . ? Al2 B4 H4D 114.2(14) . . ? H4A B4 H4D 106.5(18) . . ? H4B B4 H4D 109.1(19) . . ? H4C B4 H4D 121(2) . . ? N1 Al1 N4 87.02(7) . . ? N1 Al1 B2 129.01(9) . . ? N4 Al1 B2 105.69(8) . . ? N1 Al1 B1 105.66(9) . . ? N4 Al1 B1 127.17(9) . . ? B2 Al1 B1 104.59(11) . . ? N1 Al1 Al2 43.27(5) . . ? N4 Al1 Al2 43.76(5) . . ? B2 Al1 Al2 128.99(8) . . ? B1 Al1 Al2 126.41(8) . . ? N1 Al1 H1A 96.7(8) . . ? N4 Al1 H1A 158.2(8) . . ? B2 Al1 H1A 88.6(8) . . ? B1 Al1 H1A 31.3(8) . . ? Al2 Al1 H1A 135.6(7) . . ? N1 Al1 H1B 105.0(8) . . ? N4 Al1 H1B 95.8(8) . . ? B2 Al1 H1B 121.8(8) . . ? B1 Al1 H1B 31.5(8) . . ? Al2 Al1 H1B 103.8(8) . . ? H1A Al1 H1B 62.5(11) . . ? N1 Al1 H2A 99.7(9) . . ? N4 Al1 H2A 106.1(8) . . ? B2 Al1 H2A 29.3(9) . . ? B1 Al1 H2A 121.1(8) . . ? Al2 Al1 H2A 108.5(8) . . ? H1A Al1 H2A 94.4(11) . . ? H1B Al1 H2A 147.6(11) . . ? N1 Al1 H2B 160.4(8) . . ? N4 Al1 H2B 97.3(8) . . ? B2 Al1 H2B 31.4(8) . . ? B1 Al1 H2B 87.1(8) . . ? Al2 Al1 H2B 137.9(8) . . ? H1A Al1 H2B 86.4(11) . . ? H1B Al1 H2B 93.6(11) . . ? H2A Al1 H2B 60.6(11) . . ? N1 Al2 N4 87.09(7) . . ? N1 Al2 B4 127.08(8) . . ? N4 Al2 B4 104.63(8) . . ? N1 Al2 B3 105.46(9) . . ? N4 Al2 B3 129.62(9) . . ? B4 Al2 B3 105.22(11) . . ? N1 Al2 Al1 43.51(5) . . ? N4 Al2 Al1 43.59(4) . . ? B4 Al2 Al1 125.61(8) . . ? B3 Al2 Al1 129.14(8) . . ? N1 Al2 H3A 107.0(8) . . ? N4 Al2 H3A 99.7(9) . . ? B4 Al2 H3A 120.9(8) . . ? B3 Al2 H3A 30.0(9) . . ? Al1 Al2 H3A 109.1(9) . . ? N1 Al2 H3B 96.1(8) . . ? N4 Al2 H3B 159.5(8) . . ? B4 Al2 H3B 89.6(8) . . ? B3 Al2 H3B 30.2(8) . . ? Al1 Al2 H3B 136.3(8) . . ? H3A Al2 H3B 60.0(11) . . ? N1 Al2 H4A 159.1(7) . . ? N4 Al2 H4A 96.4(7) . . ? B4 Al2 H4A 32.2(7) . . ? B3 Al2 H4A 88.1(7) . . ? Al1 Al2 H4A 135.9(7) . . ? H3A Al2 H4A 92.7(11) . . ? H3B Al2 H4A 87.8(10) . . ? N1 Al2 H4B 95.9(8) . . ? N4 Al2 H4B 104.5(8) . . ? B4 Al2 H4B 31.2(8) . . ? B3 Al2 H4B 121.8(8) . . ? Al1 Al2 H4B 103.5(8) . . ? H3A Al2 H4B 147.4(12) . . ? H3B Al2 H4B 95.4(12) . . ? H4A Al2 H4B 63.3(11) . . ? C1 N1 Al2 132.77(12) . . ? C1 N1 Al1 134.00(12) . . ? Al2 N1 Al1 93.22(7) . . ? C1 N2 C2 110.15(15) . . ? C1 N2 C4 128.84(15) . . ? C2 N2 C4 120.27(15) . . ? C1 N3 C3 109.80(15) . . ? C1 N3 C16 129.88(15) . . ? C3 N3 C16 119.95(15) . . ? C28 N4 Al1 134.77(12) . . ? C28 N4 Al2 132.52(12) . . ? Al1 N4 Al2 92.65(6) . . ? C28 N5 C29 109.77(14) . . ? C28 N5 C31 127.48(14) . . ? C29 N5 C31 121.24(14) . . ? C28 N6 C30 109.95(14) . . ? C28 N6 C43 129.95(14) . . ? C30 N6 C43 119.72(14) . . ? N1 C1 N2 127.69(16) . . ? N1 C1 N3 127.95(16) . . ? N2 C1 N3 104.36(14) . . ? C3 C2 N2 107.61(16) . . ? C3 C2 H2E 126.2 . . ? N2 C2 H2E 126.2 . . ? C2 C3 N3 108.08(16) . . ? C2 C3 H3E 126.0 . . ? N3 C3 H3E 126.0 . . ? C5 C4 C9 122.95(19) . . ? C5 C4 N2 118.13(18) . . ? C9 C4 N2 118.55(17) . . ? C4 C5 C6 116.9(2) . . ? C4 C5 C10 121.4(2) . . ? C6 C5 C10 121.5(2) . . ? C7 C6 C5 121.1(2) . . ? C7 C6 H6A 119.4 . . ? C5 C6 H6A 119.4 . . ? C8 C7 C6 121.0(2) . . ? C8 C7 H7A 119.5 . . ? C6 C7 H7A 119.5 . . ? C7 C8 C9 120.7(2) . . ? C7 C8 H8A 119.6 . . ? C9 C8 H8A 119.6 . . ? C8 C9 C4 117.2(2) . . ? C8 C9 C13 119.1(2) . . ? C4 C9 C13 123.58(17) . . ? C5 C10 C11 113.7(3) . . ? C5 C10 C12 110.9(2) . . ? C11 C10 C12 107.9(2) . . ? C5 C10 H10A 108.1 . . ? C11 C10 H10A 108.1 . . ? C12 C10 H10A 108.1 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C9 C13 C14 112.58(19) . . ? C9 C13 C15 110.54(18) . . ? C14 C13 C15 109.12(18) . . ? C9 C13 H13A 108.2 . . ? C14 C13 H13A 108.2 . . ? C15 C13 H13A 108.2 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C21 C16 C17 122.75(18) . . ? C21 C16 N3 118.61(18) . . ? C17 C16 N3 118.15(18) . . ? C18 C17 C16 117.1(2) . . ? C18 C17 C22 118.96(19) . . ? C16 C17 C22 123.85(18) . . ? C19 C18 C17 121.3(2) . . ? C19 C18 H18A 119.4 . . ? C17 C18 H18A 119.4 . . ? C18 C19 C20 120.6(2) . . ? C18 C19 H19A 119.7 . . ? C20 C19 H19A 119.7 . . ? C19 C20 C21 121.2(2) . . ? C19 C20 H20A 119.4 . . ? C21 C20 H20A 119.4 . . ? C20 C21 C16 117.0(2) . . ? C20 C21 C25 121.3(2) . . ? C16 C21 C25 121.66(19) . . ? C17 C22 C24 112.9(2) . . ? C17 C22 C23 110.75(19) . . ? C24 C22 C23 108.4(2) . . ? C17 C22 H22A 108.2 . . ? C24 C22 H22A 108.2 . . ? C23 C22 H22A 108.2 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C21 C25 C27 112.5(2) . . ? C21 C25 C26 113.2(2) . . ? C27 C25 C26 109.2(2) . . ? C21 C25 H25A 107.2 . . ? C27 C25 H25A 107.2 . . ? C26 C25 H25A 107.2 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? N4 C28 N6 128.48(15) . . ? N4 C28 N5 127.13(16) . . ? N6 C28 N5 104.38(14) . . ? C30 C29 N5 107.91(16) . . ? C30 C29 H29A 126.0 . . ? N5 C29 H29A 126.0 . . ? C29 C30 N6 107.99(16) . . ? C29 C30 H30A 126.0 . . ? N6 C30 H30A 126.0 . . ? C36 C31 C32 122.81(17) . . ? C36 C31 N5 119.28(16) . . ? C32 C31 N5 117.73(16) . . ? C33 C32 C31 117.03(18) . . ? C33 C32 C37 121.21(18) . . ? C31 C32 C37 121.66(17) . . ? C34 C33 C32 121.36(19) . . ? C34 C33 H33A 119.3 . . ? C32 C33 H33A 119.3 . . ? C35 C34 C33 120.10(19) . . ? C35 C34 H34A 120.0 . . ? C33 C34 H34A 120.0 . . ? C34 C35 C36 121.52(19) . . ? C34 C35 H35A 119.2 . . ? C36 C35 H35A 119.2 . . ? C31 C36 C35 116.98(18) . . ? C31 C36 C40 123.29(17) . . ? C35 C36 C40 119.69(17) . . ? C32 C37 C38 113.24(18) . . ? C32 C37 C39 110.22(18) . . ? C38 C37 C39 108.80(18) . . ? C32 C37 H37A 108.1 . . ? C38 C37 H37A 108.1 . . ? C39 C37 H37A 108.1 . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C37 C39 H39A 109.5 . . ? C37 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C37 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C36 C40 C42 112.55(18) . . ? C36 C40 C41 110.50(17) . . ? C42 C40 C41 108.81(18) . . ? C36 C40 H40A 108.3 . . ? C42 C40 H40A 108.3 . . ? C41 C40 H40A 108.3 . . ? C40 C41 H41A 109.5 . . ? C40 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C40 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C40 C42 H42A 109.5 . . ? C40 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C40 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C44 C43 C48 122.79(17) . . ? C44 C43 N6 118.56(17) . . ? C48 C43 N6 118.20(16) . . ? C45 C44 C43 116.94(19) . . ? C45 C44 C49 119.30(19) . . ? C43 C44 C49 123.64(18) . . ? C46 C45 C44 121.6(2) . . ? C46 C45 H45A 119.2 . . ? C44 C45 H45A 119.2 . . ? C45 C46 C47 120.24(19) . . ? C45 C46 H46A 119.9 . . ? C47 C46 H46A 119.9 . . ? C46 C47 C48 121.5(2) . . ? C46 C47 H47A 119.3 . . ? C48 C47 H47A 119.3 . . ? C47 C48 C43 116.93(18) . . ? C47 C48 C52 121.25(18) . . ? C43 C48 C52 121.78(17) . . ? C44 C49 C50 110.28(18) . . ? C44 C49 C51 113.10(19) . . ? C50 C49 C51 108.80(18) . . ? C44 C49 H49A 108.2 . . ? C50 C49 H49A 108.2 . . ? C51 C49 H49A 108.2 . . ? C49 C50 H50A 109.5 . . ? C49 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C49 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C49 C51 H51A 109.5 . . ? C49 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C49 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C48 C52 C54 112.60(18) . . ? C48 C52 C53 111.26(17) . . ? C54 C52 C53 109.03(19) . . ? C48 C52 H52 107.9 . . ? C54 C52 H52 107.9 . . ? C53 C52 H52 107.9 . . ? C52 C53 H53A 109.5 . . ? C52 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C52 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C52 C54 H54A 109.5 . . ? C52 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C52 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C56 C55 C60 121.8(7) . . ? C56 C55 C61 124.2(8) . . ? C60 C55 C61 113.9(8) . . ? C55 C56 C57 120.4(7) . . ? C55 C56 H56A 119.8 . . ? C57 C56 H56A 119.8 . . ? C58 C57 C56 120.0(7) . . ? C58 C57 H57A 120.0 . . ? C56 C57 H57A 120.0 . . ? C57 C58 C59 119.2(7) . . ? C57 C58 H58A 120.4 . . ? C59 C58 H58A 120.4 . . ? C60 C59 C58 121.9(7) . . ? C60 C59 H59A 119.0 . . ? C58 C59 H59A 119.0 . . ? C55 C60 C59 116.6(6) . . ? C55 C60 H60A 121.7 . . ? C59 C60 H60A 121.7 . . ? C55 C61 H61A 109.5 . . ? C55 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? C55 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? C60A C55A C56A 118.2(7) . . ? C60A C55A C61A 112.8(8) . . ? C56A C55A C61A 128.9(8) . . ? C57A C56A C55A 118.9(7) . . ? C57A C56A H56B 120.5 . . ? C55A C56A H56B 120.5 . . ? C56A C57A C58A 122.5(8) . . ? C56A C57A H57B 118.8 . . ? C58A C57A H57B 118.8 . . ? C59A C58A C57A 118.0(8) . . ? C59A C58A H58B 121.0 . . ? C57A C58A H58B 121.0 . . ? C58A C59A C60A 121.0(8) . . ? C58A C59A H59B 119.5 . . ? C60A C59A H59B 119.5 . . ? C55A C60A C59A 121.1(7) . . ? C55A C60A H60B 119.5 . . ? C59A C60A H60B 119.5 . . ? C55A C61A H61D 109.5 . . ? C55A C61A H61E 109.5 . . ? H61D C61A H61E 109.5 . . ? C55A C61A H61F 109.5 . . ? H61D C61A H61F 109.5 . . ? H61E C61A H61F 109.5 . . ? C63 C62 H62A 109.5 . . ? C63 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C63 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? C68 C63 C64 118.0(7) . . ? C68 C63 C62 111.4(7) . . ? C64 C63 C62 130.6(7) . . ? C65 C64 C63 121.7(8) . . ? C65 C64 H64A 119.1 . . ? C63 C64 H64A 119.1 . . ? C64 C65 C66 119.9(7) . . ? C64 C65 H65A 120.1 . . ? C66 C65 H65A 120.1 . . ? C67 C66 C65 116.2(7) . . ? C67 C66 H66A 121.9 . . ? C65 C66 H66A 121.9 . . ? C66 C67 C68 125.9(7) . . ? C66 C67 H67A 117.0 . . ? C68 C67 H67A 117.0 . . ? C63 C68 C67 118.2(6) . . ? C63 C68 H68A 120.9 . . ? C67 C68 H68A 120.9 . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 26.31 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 0.521 _refine_diff_density_min -0.329 _refine_diff_density_rms 0.046 _database_code_depnum_ccdc_archive 'CCDC 962236' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_mo-82a _audit_creation_method ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) ; _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C54 H72 Al2 Br4 N6), 3(C7 H8)' _chemical_formula_sum 'C129 H168 Al4 Br8 N12' _chemical_formula_weight 2633.95 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 '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 48.620(2) _cell_length_b 12.0902(8) _cell_length_c 22.8590(9) _cell_angle_alpha 90.00 _cell_angle_beta 106.432(7) _cell_angle_gamma 90.00 _cell_volume 12888.4(12) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 8113 _cell_measurement_theta_min 3.3830 _cell_measurement_theta_max 31.5880 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.37 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.357 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5432 _exptl_absorpt_coefficient_mu 2.568 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4265 _exptl_absorpt_correction_T_max 0.6277 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Sapphire3' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 46122 _diffrn_reflns_av_R_equivalents 0.0810 _diffrn_reflns_av_sigmaI/netI 0.0831 _diffrn_reflns_limit_h_min -57 _diffrn_reflns_limit_h_max 57 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 3.37 _diffrn_reflns_theta_max 25.00 _reflns_number_total 11336 _reflns_number_gt 8660 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) ; _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^)+(0.0185P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11336 _refine_ls_number_parameters 801 _refine_ls_number_restraints 861 _refine_ls_R_factor_all 0.0843 _refine_ls_R_factor_gt 0.0499 _refine_ls_wR_factor_ref 0.0815 _refine_ls_wR_factor_gt 0.0739 _refine_ls_goodness_of_fit_ref 1.072 _refine_ls_restrained_S_all 1.092 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Br1 Br 0.167173(9) 0.52212(4) 0.383136(17) 0.03464(12) Uani 1 1 d . . . Br2 Br 0.199597(8) 0.79225(4) 0.355343(17) 0.03378(12) Uani 1 1 d . . . Br3 Br 0.090093(9) 0.94147(4) 0.260449(17) 0.03280(12) Uani 1 1 d . . . Br4 Br 0.068235(8) 0.64265(4) 0.235135(16) 0.03078(12) Uani 1 1 d . . . Al1 Al 0.15804(2) 0.69397(10) 0.33895(4) 0.0194(3) Uani 1 1 d . . . Al2 Al 0.10517(2) 0.76245(10) 0.27767(4) 0.0182(3) Uani 1 1 d . . . N1 N 0.12615(5) 0.7506(3) 0.35909(11) 0.0161(7) Uani 1 1 d . . . N2 N 0.13883(6) 0.8168(3) 0.46333(12) 0.0184(7) Uani 1 1 d . . . N3 N 0.09492(6) 0.7612(3) 0.42479(12) 0.0211(8) Uani 1 1 d . . . N4 N 0.13722(5) 0.7088(3) 0.25693(11) 0.0156(7) Uani 1 1 d . . . N5 N 0.13169(5) 0.7452(2) 0.14993(11) 0.0148(7) Uani 1 1 d . . . N6 N 0.15687(5) 0.5997(3) 0.18890(11) 0.0148(7) Uani 1 1 d . . . C1 C 0.12065(7) 0.7739(3) 0.41098(14) 0.0172(9) Uani 1 1 d . . . C2 C 0.12448(7) 0.8294(4) 0.50746(15) 0.0276(9) Uani 1 1 d U . . H2A H 0.1325 0.8577 0.5474 0.033 Uiso 1 1 calc R . . C3 C 0.09796(7) 0.7957(4) 0.48456(15) 0.0269(9) Uani 1 1 d U . . H3A H 0.0834 0.7949 0.5050 0.032 Uiso 1 1 calc R . . C4 C 0.16693(7) 0.8659(3) 0.47172(15) 0.0218(7) Uani 1 1 d U . . C5 C 0.16851(8) 0.9712(4) 0.44926(16) 0.0290(7) Uani 1 1 d U . . C6 C 0.19554(8) 1.0187(4) 0.46190(17) 0.0366(8) Uani 1 1 d U . . H6A H 0.1976 1.0901 0.4463 0.044 Uiso 1 1 calc R . . C7 C 0.21916(9) 0.9642(4) 0.49646(18) 0.0386(9) Uani 1 1 d U . . H7A H 0.2374 0.9986 0.5044 0.046 Uiso 1 1 calc R . . C8 C 0.21727(8) 0.8610(4) 0.51999(17) 0.0327(8) Uani 1 1 d U . . H8A H 0.2340 0.8254 0.5444 0.039 Uiso 1 1 calc R . . C9 C 0.19057(7) 0.8080(4) 0.50797(16) 0.0254(7) Uani 1 1 d U . . C10 C 0.14195(9) 1.0360(4) 0.41562(17) 0.0360(8) Uani 1 1 d U . . H10A H 0.1269 0.9813 0.3948 0.043 Uiso 1 1 calc R . . C11 C 0.14639(10) 1.1141(4) 0.36708(19) 0.0548(12) Uani 1 1 d U . . H11A H 0.1559 1.0746 0.3408 0.082 Uiso 1 1 calc R . . H11B H 0.1584 1.1765 0.3867 0.082 Uiso 1 1 calc R . . H11C H 0.1278 1.1418 0.3424 0.082 Uiso 1 1 calc R . . C12 C 0.13010(10) 1.1021(4) 0.4602(2) 0.0568(12) Uani 1 1 d U . . H12A H 0.1132 1.1441 0.4375 0.085 Uiso 1 1 calc R . . H12B H 0.1448 1.1534 0.4833 0.085 Uiso 1 1 calc R . . H12C H 0.1247 1.0513 0.4885 0.085 Uiso 1 1 calc R . . C13 C 0.18859(8) 0.6959(4) 0.53630(16) 0.0285(8) Uani 1 1 d U . . H13A H 0.1701 0.6609 0.5132 0.034 Uiso 1 1 calc R . . C14 C 0.21292(8) 0.6183(4) 0.53309(17) 0.0404(11) Uani 1 1 d U . . H14A H 0.2141 0.6151 0.4910 0.061 Uiso 1 1 calc R . . H14B H 0.2092 0.5441 0.5463 0.061 Uiso 1 1 calc R . . H14C H 0.2311 0.6461 0.5599 0.061 Uiso 1 1 calc R . . C15 C 0.18818(8) 0.7100(4) 0.60291(16) 0.0385(10) Uani 1 1 d U . . H15A H 0.1713 0.7534 0.6042 0.058 Uiso 1 1 calc R . . H15B H 0.2056 0.7485 0.6260 0.058 Uiso 1 1 calc R . . H15C H 0.1873 0.6371 0.6211 0.058 Uiso 1 1 calc R . . C16 C 0.06798(7) 0.7135(4) 0.38881(15) 0.0241(7) Uani 1 1 d U . . C17 C 0.04509(7) 0.7870(4) 0.36629(16) 0.0293(7) Uani 1 1 d U . . C18 C 0.01862(8) 0.7384(4) 0.33766(16) 0.0348(8) Uani 1 1 d U . . H18A H 0.0026 0.7846 0.3204 0.042 Uiso 1 1 calc R . . C19 C 0.01519(8) 0.6265(4) 0.33385(17) 0.0375(8) Uani 1 1 d U . . H19A H -0.0032 0.5963 0.3151 0.045 Uiso 1 1 calc R . . C20 C 0.03809(8) 0.5567(4) 0.35683(16) 0.0354(8) Uani 1 1 d U . . H20A H 0.0353 0.4789 0.3538 0.043 Uiso 1 1 calc R . . C21 C 0.06539(8) 0.5994(4) 0.38460(16) 0.0297(7) Uani 1 1 d U . . C22 C 0.04747(8) 0.9106(4) 0.37277(16) 0.0345(8) Uani 1 1 d U . . H22A H 0.0681 0.9310 0.3803 0.041 Uiso 1 1 calc R . . C23 C 0.03752(9) 0.9524(4) 0.42720(18) 0.0453(11) Uani 1 1 d U . . H23A H 0.0503 0.9231 0.4652 0.068 Uiso 1 1 calc R . . H23B H 0.0179 0.9274 0.4227 0.068 Uiso 1 1 calc R . . H23C H 0.0381 1.0335 0.4282 0.068 Uiso 1 1 calc R . . C24 C 0.03019(8) 0.9727(4) 0.31565(18) 0.0485(12) Uani 1 1 d U . . H24A H 0.0341 0.9404 0.2795 0.073 Uiso 1 1 calc R . . H24B H 0.0357 1.0508 0.3189 0.073 Uiso 1 1 calc R . . H24C H 0.0097 0.9664 0.3120 0.073 Uiso 1 1 calc R . . C25 C 0.09108(9) 0.5233(4) 0.40788(17) 0.0357(8) Uani 1 1 d U . . H25A H 0.1072 0.5560 0.3945 0.043 Uiso 1 1 calc R . . C26 C 0.08635(9) 0.4070(4) 0.38174(18) 0.0474(11) Uani 1 1 d U . . H26A H 0.0790 0.4110 0.3372 0.071 Uiso 1 1 calc R . . H26B H 0.0724 0.3685 0.3982 0.071 Uiso 1 1 calc R . . H26C H 0.1046 0.3666 0.3930 0.071 Uiso 1 1 calc R . . C27 C 0.10131(10) 0.5161(4) 0.47759(17) 0.0542(13) Uani 1 1 d U . . H27A H 0.1178 0.4663 0.4899 0.081 Uiso 1 1 calc R . . H27B H 0.0858 0.4875 0.4928 0.081 Uiso 1 1 calc R . . H27C H 0.1069 0.5899 0.4946 0.081 Uiso 1 1 calc R . . C28 C 0.14159(7) 0.6857(3) 0.20357(14) 0.0142(8) Uani 1 1 d . . . C29 C 0.14037(7) 0.6936(3) 0.10412(15) 0.0185(8) Uani 1 1 d U . . H29A H 0.1361 0.7174 0.0629 0.022 Uiso 1 1 calc R . . C30 C 0.15570(7) 0.6049(3) 0.12756(14) 0.0192(8) Uani 1 1 d U . . H30A H 0.1643 0.5543 0.1062 0.023 Uiso 1 1 calc R . . C31 C 0.12006(7) 0.8555(3) 0.14240(14) 0.0177(7) Uani 1 1 d U . . C32 C 0.13889(7) 0.9447(3) 0.16271(15) 0.0199(7) Uani 1 1 d U . . C33 C 0.12733(8) 1.0499(3) 0.15271(15) 0.0229(7) Uani 1 1 d U . . H33A H 0.1393 1.1118 0.1672 0.028 Uiso 1 1 calc R . . C34 C 0.09879(8) 1.0673(3) 0.12229(15) 0.0247(7) Uani 1 1 d U . . H34A H 0.0913 1.1403 0.1161 0.030 Uiso 1 1 calc R . . C35 C 0.08136(8) 0.9777(3) 0.10111(15) 0.0230(7) Uani 1 1 d U . . H35A H 0.0619 0.9904 0.0791 0.028 Uiso 1 1 calc R . . C36 C 0.09105(7) 0.8704(3) 0.11066(15) 0.0204(7) Uani 1 1 d U . . C37 C 0.17077(7) 0.9263(3) 0.19081(16) 0.0261(8) Uani 1 1 d U . . H37A H 0.1733 0.8537 0.2126 0.031 Uiso 1 1 calc R . . C38 C 0.18482(8) 1.0154(4) 0.23673(17) 0.0350(10) Uani 1 1 d U . . H38A H 0.1738 1.0249 0.2663 0.052 Uiso 1 1 calc R . . H38B H 0.1852 1.0853 0.2153 0.052 Uiso 1 1 calc R . . H38C H 0.2045 0.9931 0.2581 0.052 Uiso 1 1 calc R . . C39 C 0.18624(8) 0.9199(4) 0.14112(18) 0.0415(11) Uani 1 1 d U . . H39A H 0.1775 0.8619 0.1118 0.062 Uiso 1 1 calc R . . H39B H 0.2065 0.9026 0.1598 0.062 Uiso 1 1 calc R . . H39C H 0.1846 0.9912 0.1200 0.062 Uiso 1 1 calc R . . C40 C 0.07077(7) 0.7752(3) 0.08680(15) 0.0261(8) Uani 1 1 d U . . H40A H 0.0790 0.7073 0.1102 0.031 Uiso 1 1 calc R . . C41 C 0.06776(8) 0.7536(4) 0.01918(16) 0.0372(10) Uani 1 1 d U . . H41A H 0.0866 0.7372 0.0139 0.056 Uiso 1 1 calc R . . H41B H 0.0598 0.8194 -0.0047 0.056 Uiso 1 1 calc R . . H41C H 0.0549 0.6905 0.0051 0.056 Uiso 1 1 calc R . . C42 C 0.04096(7) 0.7954(4) 0.09566(17) 0.0351(10) Uani 1 1 d U . . H42A H 0.0431 0.8198 0.1376 0.053 Uiso 1 1 calc R . . H42B H 0.0298 0.7266 0.0879 0.053 Uiso 1 1 calc R . . H42C H 0.0310 0.8526 0.0671 0.053 Uiso 1 1 calc R . . C43 C 0.17047(7) 0.5066(3) 0.22542(14) 0.0194(7) Uani 1 1 d U . . C44 C 0.20051(8) 0.5061(3) 0.24749(15) 0.0244(7) Uani 1 1 d U . . C45 C 0.21305(8) 0.4093(4) 0.27620(16) 0.0298(8) Uani 1 1 d U . . H45A H 0.2333 0.4057 0.2921 0.036 Uiso 1 1 calc R . . C46 C 0.19686(8) 0.3190(4) 0.28202(16) 0.0319(8) Uani 1 1 d U . . H46A H 0.2060 0.2539 0.3015 0.038 Uiso 1 1 calc R . . C47 C 0.16749(8) 0.3223(3) 0.25982(15) 0.0274(8) Uani 1 1 d U . . H47A H 0.1566 0.2593 0.2642 0.033 Uiso 1 1 calc R . . C48 C 0.15354(8) 0.4162(3) 0.23100(15) 0.0213(7) Uani 1 1 d U . . C49 C 0.21904(8) 0.6023(4) 0.23945(16) 0.0320(8) Uani 1 1 d U . . H49A H 0.2069 0.6704 0.2320 0.038 Uiso 1 1 calc R . . C50 C 0.23012(9) 0.5834(4) 0.18374(17) 0.0499(12) Uani 1 1 d U . . H50A H 0.2409 0.5140 0.1887 0.075 Uiso 1 1 calc R . . H50B H 0.2427 0.6449 0.1800 0.075 Uiso 1 1 calc R . . H50C H 0.2138 0.5795 0.1469 0.075 Uiso 1 1 calc R . . C51 C 0.24451(8) 0.6227(4) 0.29559(17) 0.0410(11) Uani 1 1 d U . . H51A H 0.2380 0.6200 0.3324 0.062 Uiso 1 1 calc R . . H51B H 0.2528 0.6955 0.2923 0.062 Uiso 1 1 calc R . . H51C H 0.2591 0.5654 0.2980 0.062 Uiso 1 1 calc R . . C52 C 0.12116(7) 0.4172(3) 0.20487(15) 0.0249(8) Uani 1 1 d U . . H52 H 0.1144 0.4946 0.2077 0.030 Uiso 1 1 calc R . . C53 C 0.11241(8) 0.3841(4) 0.13741(15) 0.0340(10) Uani 1 1 d U . . H53A H 0.1198 0.4385 0.1140 0.051 Uiso 1 1 calc R . . H53B H 0.0914 0.3814 0.1221 0.051 Uiso 1 1 calc R . . H53C H 0.1203 0.3110 0.1330 0.051 Uiso 1 1 calc R . . C54 C 0.10609(8) 0.3423(4) 0.23970(17) 0.0380(11) Uani 1 1 d U . . H54A H 0.1096 0.2648 0.2315 0.057 Uiso 1 1 calc R . . H54B H 0.0854 0.3570 0.2265 0.057 Uiso 1 1 calc R . . H54C H 0.1136 0.3568 0.2835 0.057 Uiso 1 1 calc R . . C55 C 0.02823(17) 0.7351(7) 0.6208(3) 0.0567(13) Uani 0.680(5) 1 d PDU A 1 C56 C 0.0271(2) 0.7671(7) 0.5624(3) 0.0584(14) Uani 0.680(5) 1 d PDU A 1 H56A H 0.0258 0.8436 0.5525 0.070 Uiso 0.680(5) 1 calc PR A 1 C57 C 0.0277(5) 0.6912(8) 0.5181(4) 0.0562(14) Uani 0.680(5) 1 d PDU A 1 H57A H 0.0269 0.7154 0.4781 0.067 Uiso 0.680(5) 1 calc PR A 1 C58 C 0.02940(17) 0.5812(7) 0.5316(3) 0.0545(14) Uani 0.680(5) 1 d PDU A 1 H58A H 0.0303 0.5281 0.5015 0.065 Uiso 0.680(5) 1 calc PR A 1 C59 C 0.02989(16) 0.5474(6) 0.5908(3) 0.0565(14) Uani 0.680(5) 1 d PDU A 1 H59A H 0.0304 0.4708 0.6003 0.068 Uiso 0.680(5) 1 calc PR A 1 C60 C 0.0296(2) 0.6238(7) 0.6347(3) 0.0560(14) Uani 0.680(5) 1 d PDU A 1 H60A H 0.0304 0.6002 0.6748 0.067 Uiso 0.680(5) 1 calc PR A 1 C61 C 0.02863(16) 0.8168(8) 0.6696(4) 0.078(2) Uani 0.680(5) 1 d PU A 1 H61A H 0.0293 0.7777 0.7076 0.117 Uiso 0.680(5) 1 calc PR A 1 H61B H 0.0113 0.8624 0.6574 0.117 Uiso 0.680(5) 1 calc PR A 1 H61C H 0.0456 0.8642 0.6761 0.117 Uiso 0.680(5) 1 calc PR A 1 C55A C 0.0237(4) 0.6933(14) 0.6443(6) 0.0590(16) Uani 0.320(5) 1 d PDU A 2 C56A C 0.0209(3) 0.7906(12) 0.6107(7) 0.0600(16) Uani 0.320(5) 1 d PDU A 2 H56B H 0.0189 0.8597 0.6288 0.072 Uiso 0.320(5) 1 calc PR A 2 C57A C 0.0212(4) 0.7846(13) 0.5509(7) 0.0590(15) Uani 0.320(5) 1 d PDU A 2 H57B H 0.0180 0.8498 0.5267 0.071 Uiso 0.320(5) 1 calc PR A 2 C58A C 0.0260(10) 0.6865(16) 0.5252(9) 0.0572(15) Uani 0.320(5) 1 d PDU A 2 H58B H 0.0270 0.6850 0.4843 0.069 Uiso 0.320(5) 1 calc PR A 2 C59A C 0.0294(4) 0.5906(13) 0.5587(7) 0.0573(15) Uani 0.320(5) 1 d PDU A 2 H59B H 0.0320 0.5218 0.5409 0.069 Uiso 0.320(5) 1 calc PR A 2 C60A C 0.0289(5) 0.5960(13) 0.6190(7) 0.0567(15) Uani 0.320(5) 1 d PDU A 2 H60B H 0.0322 0.5308 0.6432 0.068 Uiso 0.320(5) 1 calc PR A 2 C61A C 0.0228(3) 0.6862(16) 0.7091(6) 0.071(3) Uani 0.320(5) 1 d PU A 2 H61D H 0.0251 0.6090 0.7226 0.107 Uiso 0.320(5) 1 calc PR A 2 H61E H 0.0043 0.7140 0.7120 0.107 Uiso 0.320(5) 1 calc PR A 2 H61F H 0.0383 0.7310 0.7350 0.107 Uiso 0.320(5) 1 calc PR A 2 C62 C 0.1989(2) 0.3065(9) 0.5160(4) 0.057(3) Uani 0.50 1 d PU B -3 H62A H 0.1865 0.3424 0.4796 0.086 Uiso 0.50 1 calc PR B -3 H62B H 0.2023 0.3572 0.5508 0.086 Uiso 0.50 1 calc PR B -3 H62C H 0.1896 0.2392 0.5249 0.086 Uiso 0.50 1 calc PR B -3 C63 C 0.2269(4) 0.277(2) 0.5049(9) 0.051(2) Uani 0.50 1 d PDU B -3 C64 C 0.2486(3) 0.228(2) 0.5519(9) 0.056(3) Uani 0.50 1 d PDU B -3 H64A H 0.2458 0.2178 0.5910 0.067 Uiso 0.50 1 calc PR B -3 C65 C 0.2737(4) 0.194(2) 0.5418(10) 0.059(3) Uani 0.50 1 d PDU B -3 H65A H 0.2878 0.1571 0.5732 0.071 Uiso 0.50 1 calc PR B -3 C66 C 0.2788(4) 0.212(2) 0.4866(10) 0.058(3) Uani 0.50 1 d PDU B -3 H66A H 0.2957 0.1850 0.4790 0.069 Uiso 0.50 1 calc PR B -3 C67 C 0.2590(4) 0.272(2) 0.4419(10) 0.055(3) Uani 0.50 1 d PDU B -3 H67A H 0.2633 0.2914 0.4052 0.065 Uiso 0.50 1 calc PR B -3 C68 C 0.2333(4) 0.301(2) 0.4510(9) 0.052(2) Uani 0.50 1 d PDU B -3 H68A H 0.2196 0.3393 0.4196 0.062 Uiso 0.50 1 calc PR B -3 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 Br1 0.0495(3) 0.0297(3) 0.0217(2) 0.00486(19) 0.00507(19) 0.0165(2) Br2 0.0188(2) 0.0533(3) 0.0295(2) -0.0120(2) 0.00726(17) -0.0050(2) Br3 0.0439(3) 0.0334(3) 0.0252(2) 0.00915(19) 0.01639(19) 0.0196(2) Br4 0.0215(2) 0.0486(3) 0.0209(2) -0.0039(2) 0.00390(16) -0.0085(2) Al1 0.0187(6) 0.0253(8) 0.0131(5) -0.0011(5) 0.0029(4) 0.0043(5) Al2 0.0173(6) 0.0241(8) 0.0129(5) 0.0011(5) 0.0040(4) 0.0033(5) N1 0.0154(16) 0.023(2) 0.0106(15) 0.0007(13) 0.0043(12) -0.0004(14) N2 0.0144(16) 0.027(2) 0.0142(15) -0.0016(14) 0.0054(12) -0.0004(14) N3 0.0139(16) 0.038(2) 0.0111(15) -0.0031(15) 0.0033(12) -0.0015(15) N4 0.0167(16) 0.020(2) 0.0102(15) 0.0006(13) 0.0044(12) 0.0000(14) N5 0.0154(16) 0.0152(19) 0.0127(15) -0.0003(13) 0.0025(12) -0.0017(14) N6 0.0156(16) 0.0149(19) 0.0139(15) 0.0007(13) 0.0041(12) 0.0016(14) C1 0.0151(19) 0.022(3) 0.0116(18) 0.0019(16) -0.0007(15) 0.0026(17) C2 0.0188(16) 0.051(3) 0.0147(17) -0.0046(17) 0.0069(14) -0.0022(18) C3 0.0185(16) 0.051(3) 0.0133(17) -0.0032(17) 0.0076(14) -0.0006(18) C4 0.0204(14) 0.0284(17) 0.0197(15) -0.0099(13) 0.0106(12) -0.0036(13) C5 0.0342(14) 0.0292(16) 0.0284(15) -0.0082(13) 0.0165(13) -0.0038(13) C6 0.0406(16) 0.0326(19) 0.0425(18) -0.0093(15) 0.0212(15) -0.0109(14) C7 0.0320(16) 0.039(2) 0.0484(19) -0.0161(16) 0.0169(15) -0.0130(16) C8 0.0223(14) 0.0376(19) 0.0377(18) -0.0145(15) 0.0076(14) -0.0070(14) C9 0.0193(14) 0.0319(15) 0.0248(14) -0.0110(12) 0.0058(12) -0.0039(12) C10 0.0469(17) 0.031(2) 0.0335(18) 0.0000(14) 0.0159(15) 0.0027(16) C11 0.082(3) 0.043(3) 0.043(2) 0.0066(19) 0.024(2) 0.003(2) C12 0.065(2) 0.057(2) 0.054(2) 0.0017(19) 0.0265(18) 0.0215(19) C13 0.0183(16) 0.0347(18) 0.0274(16) -0.0061(15) -0.0019(14) -0.0021(14) C14 0.033(2) 0.042(3) 0.038(2) -0.006(2) -0.0024(18) 0.0110(19) C15 0.035(2) 0.047(3) 0.0312(19) 0.0013(19) 0.0056(17) -0.001(2) C16 0.0172(14) 0.0451(16) 0.0117(14) -0.0027(15) 0.0067(12) -0.0059(13) C17 0.0184(14) 0.0510(15) 0.0190(14) -0.0003(14) 0.0060(12) -0.0021(13) C18 0.0188(14) 0.0585(18) 0.0269(16) -0.0023(17) 0.0064(13) -0.0029(15) C19 0.0246(15) 0.060(2) 0.0289(16) -0.0069(17) 0.0089(14) -0.0113(16) C20 0.0302(15) 0.0505(19) 0.0278(16) -0.0050(16) 0.0118(14) -0.0138(14) C21 0.0272(14) 0.0458(16) 0.0190(14) -0.0010(14) 0.0112(12) -0.0076(13) C22 0.0208(17) 0.0516(18) 0.0296(16) 0.0049(16) 0.0045(14) 0.0012(15) C23 0.041(2) 0.052(3) 0.041(2) -0.008(2) 0.0098(19) 0.003(2) C24 0.033(2) 0.065(3) 0.045(2) 0.016(2) 0.0087(19) 0.016(2) C25 0.0373(17) 0.0425(19) 0.0281(16) 0.0064(16) 0.0104(15) -0.0044(16) C26 0.062(3) 0.045(2) 0.040(2) 0.002(2) 0.024(2) 0.000(2) C27 0.073(3) 0.048(3) 0.0340(19) 0.0099(19) 0.002(2) 0.000(3) C28 0.0104(18) 0.015(2) 0.0150(18) 0.0006(16) -0.0009(14) -0.0027(16) C29 0.0245(18) 0.023(2) 0.0110(16) -0.0015(15) 0.0090(14) 0.0015(15) C30 0.0227(18) 0.023(2) 0.0137(17) -0.0025(15) 0.0083(14) 0.0040(15) C31 0.0215(13) 0.0206(16) 0.0137(14) 0.0006(13) 0.0096(12) 0.0037(12) C32 0.0241(13) 0.0221(16) 0.0169(14) 0.0034(13) 0.0110(11) -0.0004(12) C33 0.0301(15) 0.0199(16) 0.0223(15) 0.0022(14) 0.0131(13) -0.0016(13) C34 0.0317(16) 0.0213(16) 0.0237(16) 0.0065(14) 0.0122(13) 0.0057(14) C35 0.0241(15) 0.0250(16) 0.0207(15) 0.0061(14) 0.0074(13) 0.0069(13) C36 0.0221(13) 0.0242(15) 0.0161(13) 0.0026(13) 0.0076(11) 0.0023(12) C37 0.0235(15) 0.0259(19) 0.0289(17) -0.0017(15) 0.0073(13) -0.0033(14) C38 0.028(2) 0.040(3) 0.037(2) -0.0104(18) 0.0093(17) -0.0077(19) C39 0.027(2) 0.052(3) 0.051(2) -0.021(2) 0.0198(18) -0.005(2) C40 0.0236(15) 0.0287(18) 0.0228(15) 0.0039(15) 0.0014(14) 0.0003(14) C41 0.039(2) 0.037(3) 0.0311(19) -0.0092(19) 0.0030(17) -0.002(2) C42 0.0200(18) 0.045(3) 0.036(2) 0.003(2) 0.0009(16) -0.0030(19) C43 0.0235(13) 0.0200(17) 0.0139(14) -0.0046(13) 0.0042(13) 0.0051(12) C44 0.0239(13) 0.0269(16) 0.0196(14) -0.0054(13) 0.0019(12) 0.0039(12) C45 0.0273(16) 0.0310(18) 0.0258(16) -0.0037(15) -0.0012(14) 0.0095(13) C46 0.0365(16) 0.0274(18) 0.0272(16) 0.0007(15) 0.0016(15) 0.0120(15) C47 0.0352(15) 0.0226(17) 0.0233(16) -0.0001(14) 0.0064(14) 0.0050(14) C48 0.0272(13) 0.0199(16) 0.0170(14) -0.0031(13) 0.0067(11) 0.0038(12) C49 0.0231(16) 0.036(2) 0.0324(17) -0.0042(16) 0.0006(13) -0.0015(15) C50 0.037(2) 0.073(4) 0.039(2) -0.002(2) 0.0098(18) -0.018(2) C51 0.023(2) 0.047(3) 0.045(2) -0.016(2) -0.0021(17) 0.0021(19) C52 0.0272(15) 0.021(2) 0.0264(16) 0.0003(15) 0.0079(13) -0.0016(14) C53 0.028(2) 0.043(3) 0.0268(17) 0.0034(19) 0.0018(15) -0.008(2) C54 0.037(2) 0.045(3) 0.036(2) 0.003(2) 0.0165(18) -0.008(2) C55 0.040(2) 0.071(3) 0.057(2) 0.009(2) 0.010(2) -0.009(3) C56 0.040(3) 0.071(3) 0.059(3) 0.016(2) 0.004(2) -0.011(3) C57 0.036(3) 0.075(3) 0.054(2) 0.016(2) 0.006(2) -0.014(3) C58 0.038(2) 0.073(3) 0.050(3) 0.012(3) 0.010(3) -0.016(3) C59 0.046(2) 0.069(3) 0.051(3) 0.014(2) 0.009(3) -0.013(3) C60 0.043(3) 0.070(3) 0.052(3) 0.013(2) 0.010(3) -0.011(3) C61 0.062(4) 0.088(4) 0.085(4) -0.011(3) 0.024(4) 0.006(4) C55A 0.043(3) 0.074(4) 0.057(3) 0.011(3) 0.010(3) -0.007(3) C56A 0.043(3) 0.073(3) 0.059(3) 0.011(3) 0.006(3) -0.008(3) C57A 0.040(3) 0.074(3) 0.058(3) 0.014(3) 0.005(3) -0.012(3) C58A 0.038(3) 0.074(3) 0.054(3) 0.015(2) 0.005(3) -0.013(3) C59A 0.042(3) 0.073(3) 0.053(3) 0.013(3) 0.008(3) -0.013(3) C60A 0.042(3) 0.071(3) 0.054(3) 0.013(3) 0.009(3) -0.011(3) C61A 0.059(7) 0.096(9) 0.060(5) 0.013(4) 0.019(6) 0.002(7) C62 0.064(6) 0.050(7) 0.062(6) -0.021(5) 0.024(5) -0.017(5) C63 0.059(6) 0.042(5) 0.053(4) -0.013(4) 0.020(4) -0.022(5) C64 0.063(7) 0.044(4) 0.057(4) -0.008(4) 0.012(5) -0.025(6) C65 0.062(6) 0.044(5) 0.065(5) -0.007(4) 0.009(5) -0.021(6) C66 0.058(7) 0.043(5) 0.070(5) -0.017(5) 0.017(5) -0.025(6) C67 0.062(7) 0.047(4) 0.058(5) -0.015(4) 0.022(4) -0.025(6) C68 0.062(7) 0.044(4) 0.052(4) -0.013(4) 0.020(4) -0.022(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Br1 Al1 2.2979(13) . ? Br2 Al1 2.2817(12) . ? Br3 Al2 2.2834(13) . ? Br4 Al2 2.2980(12) . ? Al1 N1 1.868(3) . ? Al1 N4 1.871(3) . ? Al1 Al2 2.6866(14) . ? Al2 N1 1.858(3) . ? Al2 N4 1.868(3) . ? N1 C1 1.318(4) . ? N2 C1 1.372(4) . ? N2 C2 1.388(4) . ? N2 C4 1.451(4) . ? N3 C1 1.383(4) . ? N3 C3 1.396(4) . ? N3 C16 1.454(4) . ? N4 C28 1.326(4) . ? N5 C29 1.383(4) . ? N5 C28 1.385(4) . ? N5 C31 1.440(4) . ? N6 C28 1.374(4) . ? N6 C30 1.389(4) . ? N6 C43 1.445(4) . ? C2 C3 1.312(5) . ? C4 C5 1.384(5) . ? C4 C9 1.400(5) . ? C5 C6 1.388(5) . ? C5 C10 1.520(5) . ? C6 C7 1.366(6) . ? C7 C8 1.372(6) . ? C8 C9 1.403(5) . ? C9 C13 1.517(5) . ? C10 C11 1.518(5) . ? C10 C12 1.531(5) . ? C13 C14 1.527(5) . ? C13 C15 1.538(5) . ? C16 C21 1.386(6) . ? C16 C17 1.403(5) . ? C17 C18 1.397(5) . ? C17 C22 1.504(6) . ? C18 C19 1.362(6) . ? C19 C20 1.377(6) . ? C20 C21 1.398(5) . ? C21 C25 1.521(6) . ? C22 C24 1.534(5) . ? C22 C23 1.542(5) . ? C25 C26 1.519(6) . ? C25 C27 1.532(5) . ? C29 C30 1.329(5) . ? C31 C36 1.404(4) . ? C31 C32 1.405(5) . ? C32 C33 1.383(5) . ? C32 C37 1.517(5) . ? C33 C34 1.381(5) . ? C34 C35 1.376(5) . ? C35 C36 1.376(5) . ? C36 C40 1.514(5) . ? C37 C38 1.524(5) . ? C37 C39 1.531(5) . ? C40 C41 1.533(5) . ? C40 C42 1.538(5) . ? C43 C48 1.396(5) . ? C43 C44 1.404(5) . ? C44 C45 1.395(5) . ? C44 C49 1.513(5) . ? C45 C46 1.375(6) . ? C46 C47 1.374(5) . ? C47 C48 1.389(5) . ? C48 C52 1.518(5) . ? C49 C51 1.530(5) . ? C49 C50 1.534(5) . ? C52 C54 1.523(5) . ? C52 C53 1.533(5) . ? C55 C56 1.376(8) . ? C55 C60 1.380(9) . ? C55 C61 1.487(10) . ? C56 C57 1.374(9) . ? C57 C58 1.363(9) . ? C58 C59 1.407(7) . ? C59 C60 1.366(8) . ? C55A C60A 1.365(12) . ? C55A C56A 1.390(12) . ? C55A C61A 1.497(17) . ? C56A C57A 1.374(11) . ? C57A C58A 1.372(12) . ? C58A C59A 1.374(12) . ? C59A C60A 1.389(11) . ? C62 C63 1.500(17) . ? C63 C68 1.385(10) . ? C63 C64 1.407(10) . ? C64 C65 1.367(10) . ? C65 C66 1.370(10) . ? C66 C67 1.386(10) . ? C67 C68 1.371(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Al1 N4 87.72(12) . . ? N1 Al1 Br2 121.80(11) . . ? N4 Al1 Br2 108.53(10) . . ? N1 Al1 Br1 107.07(10) . . ? N4 Al1 Br1 120.64(11) . . ? Br2 Al1 Br1 110.29(4) . . ? N1 Al1 Al2 43.70(8) . . ? N4 Al1 Al2 44.03(9) . . ? Br2 Al1 Al2 126.67(6) . . ? Br1 Al1 Al2 123.04(5) . . ? N1 Al2 N4 88.08(12) . . ? N1 Al2 Br3 107.73(11) . . ? N4 Al2 Br3 122.38(11) . . ? N1 Al2 Br4 121.14(11) . . ? N4 Al2 Br4 106.36(10) . . ? Br3 Al2 Br4 110.49(4) . . ? N1 Al2 Al1 43.99(9) . . ? N4 Al2 Al1 44.10(8) . . ? Br3 Al2 Al1 126.53(5) . . ? Br4 Al2 Al1 122.98(6) . . ? C1 N1 Al2 133.7(2) . . ? C1 N1 Al1 134.0(2) . . ? Al2 N1 Al1 92.31(12) . . ? C1 N2 C2 110.1(3) . . ? C1 N2 C4 128.3(3) . . ? C2 N2 C4 120.5(3) . . ? C1 N3 C3 109.8(3) . . ? C1 N3 C16 130.0(3) . . ? C3 N3 C16 120.1(3) . . ? C28 N4 Al2 132.0(2) . . ? C28 N4 Al1 136.0(2) . . ? Al2 N4 Al1 91.87(12) . . ? C29 N5 C28 109.4(3) . . ? C29 N5 C31 121.4(3) . . ? C28 N5 C31 127.8(3) . . ? C28 N6 C30 110.0(3) . . ? C28 N6 C43 129.7(3) . . ? C30 N6 C43 120.0(3) . . ? N1 C1 N2 128.4(3) . . ? N1 C1 N3 127.5(3) . . ? N2 C1 N3 104.1(3) . . ? C3 C2 N2 108.4(3) . . ? C2 C3 N3 107.7(3) . . ? C5 C4 C9 123.9(4) . . ? C5 C4 N2 118.4(3) . . ? C9 C4 N2 117.3(4) . . ? C4 C5 C6 116.9(4) . . ? C4 C5 C10 122.3(4) . . ? C6 C5 C10 120.7(4) . . ? C7 C6 C5 120.8(4) . . ? C6 C7 C8 121.8(4) . . ? C7 C8 C9 120.0(4) . . ? C4 C9 C8 116.6(4) . . ? C4 C9 C13 124.0(3) . . ? C8 C9 C13 119.4(4) . . ? C11 C10 C5 114.5(4) . . ? C11 C10 C12 108.7(4) . . ? C5 C10 C12 111.0(3) . . ? C9 C13 C14 112.6(3) . . ? C9 C13 C15 110.1(3) . . ? C14 C13 C15 110.1(3) . . ? C21 C16 C17 123.9(4) . . ? C21 C16 N3 118.9(3) . . ? C17 C16 N3 116.8(4) . . ? C18 C17 C16 115.8(4) . . ? C18 C17 C22 119.9(4) . . ? C16 C17 C22 124.2(3) . . ? C19 C18 C17 121.8(4) . . ? C18 C19 C20 120.9(4) . . ? C19 C20 C21 120.5(5) . . ? C16 C21 C20 117.1(4) . . ? C16 C21 C25 121.9(4) . . ? C20 C21 C25 121.0(4) . . ? C17 C22 C24 113.2(3) . . ? C17 C22 C23 111.9(4) . . ? C24 C22 C23 107.8(4) . . ? C26 C25 C21 113.9(3) . . ? C26 C25 C27 109.0(4) . . ? C21 C25 C27 113.0(3) . . ? N4 C28 N6 128.5(3) . . ? N4 C28 N5 126.8(3) . . ? N6 C28 N5 104.7(3) . . ? C30 C29 N5 108.4(3) . . ? C29 C30 N6 107.6(3) . . ? C36 C31 C32 122.5(4) . . ? C36 C31 N5 119.0(3) . . ? C32 C31 N5 118.3(3) . . ? C33 C32 C31 117.0(3) . . ? C33 C32 C37 121.6(3) . . ? C31 C32 C37 121.3(3) . . ? C34 C33 C32 121.8(4) . . ? C35 C34 C33 119.2(4) . . ? C36 C35 C34 122.5(3) . . ? C35 C36 C31 116.9(4) . . ? C35 C36 C40 120.1(3) . . ? C31 C36 C40 123.0(3) . . ? C32 C37 C38 113.2(3) . . ? C32 C37 C39 110.5(3) . . ? C38 C37 C39 109.2(3) . . ? C36 C40 C41 111.1(3) . . ? C36 C40 C42 111.9(3) . . ? C41 C40 C42 109.6(3) . . ? C48 C43 C44 123.0(3) . . ? C48 C43 N6 118.5(3) . . ? C44 C43 N6 118.0(3) . . ? C45 C44 C43 116.4(4) . . ? C45 C44 C49 120.4(3) . . ? C43 C44 C49 123.2(3) . . ? C46 C45 C44 121.7(4) . . ? C47 C46 C45 120.3(4) . . ? C46 C47 C48 121.1(4) . . ? C47 C48 C43 117.5(3) . . ? C47 C48 C52 120.4(4) . . ? C43 C48 C52 122.0(3) . . ? C44 C49 C51 113.0(3) . . ? C44 C49 C50 110.3(3) . . ? C51 C49 C50 109.2(3) . . ? C48 C52 C54 112.8(3) . . ? C48 C52 C53 110.8(3) . . ? C54 C52 C53 109.4(3) . . ? C56 C55 C60 118.9(7) . . ? C56 C55 C61 122.0(8) . . ? C60 C55 C61 119.1(7) . . ? C57 C56 C55 121.6(7) . . ? C58 C57 C56 119.8(7) . . ? C57 C58 C59 118.9(6) . . ? C60 C59 C58 120.6(7) . . ? C59 C60 C55 120.1(7) . . ? C60A C55A C56A 119.8(9) . . ? C60A C55A C61A 115.5(14) . . ? C56A C55A C61A 124.7(14) . . ? C57A C56A C55A 118.6(9) . . ? C58A C57A C56A 121.5(10) . . ? C57A C58A C59A 119.9(10) . . ? C58A C59A C60A 118.8(10) . . ? C55A C60A C59A 121.2(10) . . ? C68 C63 C64 117.5(7) . . ? C68 C63 C62 122.9(11) . . ? C64 C63 C62 119.5(11) . . ? C65 C64 C63 120.6(7) . . ? C64 C65 C66 120.5(8) . . ? C65 C66 C67 119.7(8) . . ? C68 C67 C66 119.7(7) . . ? C67 C68 C63 121.5(7) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.477 _refine_diff_density_min -0.498 _refine_diff_density_rms 0.082 _database_code_depnum_ccdc_archive 'CCDC 962237' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_mo-36a _audit_creation_method ; CrysAlisPro, Agilent Technologies, Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET) (compiled Dec 3 2012,18:21:49) ; _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C54 H72 Al2 Cl4 N6), 3(C7 H8)' _chemical_formula_sum 'C129 H168 Al4 Cl8 N12' _chemical_formula_weight 2278.27 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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 48.612(2) _cell_length_b 12.0883(4) _cell_length_c 22.5786(9) _cell_angle_alpha 90.00 _cell_angle_beta 105.956(6) _cell_angle_gamma 90.00 _cell_volume 12756.8(8) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 8533 _cell_measurement_theta_min 3.4610 _cell_measurement_theta_max 27.9340 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.73 _exptl_crystal_size_mid 0.44 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.186 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4856 _exptl_absorpt_coefficient_mu 0.256 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8352 _exptl_absorpt_correction_T_max 0.9482 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET) (compiled Dec 3 2012,18:21:49) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Sapphire3' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 52472 _diffrn_reflns_av_R_equivalents 0.0816 _diffrn_reflns_av_sigmaI/netI 0.0754 _diffrn_reflns_limit_h_min -57 _diffrn_reflns_limit_h_max 57 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 3.37 _diffrn_reflns_theta_max 25.00 _reflns_number_total 11220 _reflns_number_gt 8005 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET) (compiled Dec 3 2012,18:21:49) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET) (compiled Dec 3 2012,18:21:49) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET) (compiled Dec 3 2012,18:21:49) ; _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^)+(0.0390P)^2^+5.8781P] 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 11220 _refine_ls_number_parameters 731 _refine_ls_number_restraints 243 _refine_ls_R_factor_all 0.0915 _refine_ls_R_factor_gt 0.0592 _refine_ls_wR_factor_ref 0.1270 _refine_ls_wR_factor_gt 0.1134 _refine_ls_goodness_of_fit_ref 1.067 _refine_ls_restrained_S_all 1.095 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Al1 Al 0.604129(18) 0.25646(7) 0.77669(4) 0.0248(2) Uani 1 1 d . . . Al2 Al 0.657048(18) 0.18907(7) 0.83823(4) 0.0258(2) Uani 1 1 d . . . Cl1 Cl 0.570083(16) 0.14310(7) 0.73792(4) 0.0394(2) Uani 1 1 d . . . Cl2 Cl 0.589424(18) 0.42200(6) 0.75978(4) 0.0409(2) Uani 1 1 d . . . Cl3 Cl 0.66526(2) 0.02859(7) 0.87948(4) 0.0445(2) Uani 1 1 d . . . Cl4 Cl 0.695868(17) 0.27894(7) 0.85359(4) 0.0453(2) Uani 1 1 d . . . N1 N 0.63655(5) 0.20478(17) 0.75568(10) 0.0219(5) Uani 1 1 d . . . N2 N 0.63177(5) 0.24413(17) 0.64837(10) 0.0215(5) Uani 1 1 d . . . N3 N 0.65729(5) 0.09978(17) 0.68671(10) 0.0216(5) Uani 1 1 d . . . N4 N 0.62511(5) 0.24595(17) 0.85891(10) 0.0227(5) Uani 1 1 d . . . N5 N 0.59382(5) 0.25995(19) 0.92558(10) 0.0267(6) Uani 1 1 d . . . N6 N 0.63779(5) 0.31550(18) 0.96328(10) 0.0236(5) Uani 1 1 d . . . C1 C 0.64154(6) 0.1845(2) 0.70243(13) 0.0204(6) Uani 1 1 d . . . C2 C 0.64128(6) 0.1956(2) 0.60179(13) 0.0257(7) Uani 1 1 d . . . H2A H 0.6374 0.2210 0.5605 0.031 Uiso 1 1 calc R . . C3 C 0.65661(6) 0.1078(2) 0.62516(13) 0.0254(7) Uani 1 1 d . . . H3A H 0.6656 0.0587 0.6035 0.030 Uiso 1 1 calc R . . C4 C 0.62004(6) 0.3555(2) 0.64266(13) 0.0231(6) Uani 1 1 d . . . C5 C 0.59104(6) 0.3706(2) 0.61285(13) 0.0254(7) Uani 1 1 d . . . C6 C 0.58128(6) 0.4791(2) 0.60571(13) 0.0307(7) Uani 1 1 d . . . H6A H 0.5618 0.4930 0.5848 0.037 Uiso 1 1 calc R . . C7 C 0.59902(7) 0.5667(2) 0.62810(14) 0.0340(8) Uani 1 1 d . . . H7A H 0.5916 0.6399 0.6239 0.041 Uiso 1 1 calc R . . C8 C 0.62753(7) 0.5492(2) 0.65660(14) 0.0308(7) Uani 1 1 d . . . H8A H 0.6396 0.6107 0.6717 0.037 Uiso 1 1 calc R . . C9 C 0.63915(6) 0.4428(2) 0.66382(13) 0.0252(7) Uani 1 1 d . . . C10 C 0.57080(6) 0.2754(2) 0.58880(14) 0.0308(7) Uani 1 1 d . . . H10A H 0.5794 0.2073 0.6116 0.037 Uiso 1 1 calc R . . C11 C 0.54148(7) 0.2930(3) 0.59985(16) 0.0456(9) Uani 1 1 d . . . H11A H 0.5440 0.3158 0.6427 0.068 Uiso 1 1 calc R . . H11B H 0.5306 0.2238 0.5919 0.068 Uiso 1 1 calc R . . H11C H 0.5311 0.3507 0.5721 0.068 Uiso 1 1 calc R . . C12 C 0.56738(7) 0.2554(3) 0.52046(15) 0.0455(9) Uani 1 1 d . . . H12A H 0.5860 0.2363 0.5143 0.068 Uiso 1 1 calc R . . H12B H 0.5600 0.3225 0.4972 0.068 Uiso 1 1 calc R . . H12C H 0.5539 0.1943 0.5060 0.068 Uiso 1 1 calc R . . C13 C 0.67098(6) 0.4252(2) 0.68975(14) 0.0315(7) Uani 1 1 d . . . H13A H 0.6739 0.3491 0.7077 0.038 Uiso 1 1 calc R . . C14 C 0.68536(7) 0.5061(3) 0.74029(16) 0.0513(10) Uani 1 1 d . . . H14A H 0.6755 0.5050 0.7727 0.077 Uiso 1 1 calc R . . H14B H 0.6845 0.5808 0.7230 0.077 Uiso 1 1 calc R . . H14C H 0.7054 0.4846 0.7578 0.077 Uiso 1 1 calc R . . C15 C 0.68592(7) 0.4305(3) 0.63814(17) 0.0538(10) Uani 1 1 d . . . H15A H 0.6768 0.3783 0.6055 0.081 Uiso 1 1 calc R . . H15B H 0.7061 0.4108 0.6548 0.081 Uiso 1 1 calc R . . H15C H 0.6844 0.5056 0.6212 0.081 Uiso 1 1 calc R . . C16 C 0.67115(6) 0.0076(2) 0.72477(13) 0.0241(7) Uani 1 1 d . . . C17 C 0.65425(6) -0.0826(2) 0.73119(13) 0.0262(7) Uani 1 1 d . . . C18 C 0.66859(7) -0.1750(2) 0.76158(14) 0.0360(8) Uani 1 1 d . . . H18A H 0.6579 -0.2379 0.7673 0.043 Uiso 1 1 calc R . . C19 C 0.69803(8) -0.1768(3) 0.78349(15) 0.0429(9) Uani 1 1 d . . . H19A H 0.7074 -0.2412 0.8034 0.052 Uiso 1 1 calc R . . C20 C 0.71392(7) -0.0860(3) 0.77672(15) 0.0415(9) Uani 1 1 d . . . H20A H 0.7341 -0.0883 0.7928 0.050 Uiso 1 1 calc R . . C21 C 0.70098(6) 0.0097(2) 0.74670(13) 0.0299(7) Uani 1 1 d . . . C22 C 0.62196(6) -0.0822(2) 0.70531(14) 0.0299(7) Uani 1 1 d . . . H22A H 0.6151 -0.0048 0.7080 0.036 Uiso 1 1 calc R . . C23 C 0.61350(7) -0.1155(3) 0.63751(15) 0.0425(9) Uani 1 1 d . . . H23A H 0.6209 -0.0607 0.6137 0.064 Uiso 1 1 calc R . . H23B H 0.5926 -0.1189 0.6221 0.064 Uiso 1 1 calc R . . H23C H 0.6216 -0.1882 0.6331 0.064 Uiso 1 1 calc R . . C24 C 0.60710(8) -0.1565(3) 0.74159(16) 0.0474(9) Uani 1 1 d . . . H24A H 0.6141 -0.1390 0.7856 0.071 Uiso 1 1 calc R . . H24B H 0.6113 -0.2341 0.7350 0.071 Uiso 1 1 calc R . . H24C H 0.5864 -0.1442 0.7276 0.071 Uiso 1 1 calc R . . C25 C 0.71918(7) 0.1060(3) 0.73739(16) 0.0423(9) Uani 1 1 d . . . H25A H 0.7066 0.1729 0.7280 0.051 Uiso 1 1 calc R . . C26 C 0.73123(8) 0.0856(4) 0.68230(17) 0.0660(12) Uani 1 1 d . . . H26A H 0.7154 0.0777 0.6448 0.099 Uiso 1 1 calc R . . H26B H 0.7427 0.0178 0.6892 0.099 Uiso 1 1 calc R . . H26C H 0.7433 0.1483 0.6777 0.099 Uiso 1 1 calc R . . C27 C 0.74392(7) 0.1317(3) 0.79455(17) 0.0529(10) Uani 1 1 d . . . H27A H 0.7365 0.1378 0.8307 0.079 Uiso 1 1 calc R . . H27B H 0.7530 0.2016 0.7884 0.079 Uiso 1 1 calc R . . H27C H 0.7581 0.0719 0.8011 0.079 Uiso 1 1 calc R . . C28 C 0.61924(6) 0.2717(2) 0.91098(13) 0.0216(6) Uani 1 1 d . . . C29 C 0.59675(6) 0.2952(3) 0.98540(13) 0.0329(8) Uani 1 1 d . . . H29A H 0.5822 0.2943 1.0063 0.039 Uiso 1 1 calc R . . C30 C 0.62350(6) 0.3304(2) 1.00844(13) 0.0296(7) Uani 1 1 d . . . H30A H 0.6314 0.3603 1.0484 0.036 Uiso 1 1 calc R . . C31 C 0.56689(6) 0.2155(3) 0.88878(13) 0.0287(7) Uani 1 1 d . . . C32 C 0.56364(7) 0.1003(3) 0.88333(14) 0.0341(8) Uani 1 1 d . . . C33 C 0.53633(7) 0.0614(3) 0.85421(15) 0.0422(9) Uani 1 1 d . . . H33A H 0.5331 -0.0161 0.8500 0.051 Uiso 1 1 calc R . . C34 C 0.51391(7) 0.1331(3) 0.83136(15) 0.0477(10) Uani 1 1 d . . . H34A H 0.4954 0.1043 0.8120 0.057 Uiso 1 1 calc R . . C35 C 0.51783(7) 0.2457(3) 0.83607(15) 0.0437(9) Uani 1 1 d . . . H35A H 0.5022 0.2936 0.8190 0.052 Uiso 1 1 calc R . . C36 C 0.54448(6) 0.2902(3) 0.86551(13) 0.0320(7) Uani 1 1 d . . . C37 C 0.58875(7) 0.0228(3) 0.90657(15) 0.0411(8) Uani 1 1 d . . . H37A H 0.6051 0.0538 0.8929 0.049 Uiso 1 1 calc R . . C38 C 0.59862(9) 0.0154(3) 0.97667(17) 0.0658(12) Uani 1 1 d . . . H38A H 0.6153 -0.0335 0.9892 0.099 Uiso 1 1 calc R . . H38B H 0.5831 -0.0145 0.9919 0.099 Uiso 1 1 calc R . . H38C H 0.6038 0.0893 0.9940 0.099 Uiso 1 1 calc R . . C39 C 0.58314(9) -0.0937(3) 0.87969(18) 0.0573(11) Uani 1 1 d . . . H39A H 0.5766 -0.0893 0.8347 0.086 Uiso 1 1 calc R . . H39B H 0.5684 -0.1295 0.8952 0.086 Uiso 1 1 calc R . . H39C H 0.6008 -0.1371 0.8920 0.086 Uiso 1 1 calc R . . C40 C 0.54774(7) 0.4147(3) 0.87317(15) 0.0396(8) Uani 1 1 d . . . H40A H 0.5685 0.4331 0.8824 0.048 Uiso 1 1 calc R . . C41 C 0.53686(8) 0.4565(3) 0.92668(17) 0.0549(10) Uani 1 1 d . . . H41A H 0.5486 0.4250 0.9654 0.082 Uiso 1 1 calc R . . H41B H 0.5169 0.4337 0.9203 0.082 Uiso 1 1 calc R . . H41C H 0.5381 0.5373 0.9286 0.082 Uiso 1 1 calc R . . C42 C 0.53182(8) 0.4780(3) 0.81510(17) 0.0582(11) Uani 1 1 d . . . H42A H 0.5369 0.4473 0.7794 0.087 Uiso 1 1 calc R . . H42B H 0.5372 0.5563 0.8198 0.087 Uiso 1 1 calc R . . H42C H 0.5111 0.4710 0.8090 0.087 Uiso 1 1 calc R . . C43 C 0.66537(6) 0.3644(2) 0.96901(13) 0.0255(7) Uani 1 1 d . . . C44 C 0.66613(7) 0.4703(2) 0.94411(14) 0.0325(7) Uani 1 1 d . . . C45 C 0.69292(8) 0.5180(3) 0.95375(17) 0.0472(10) Uani 1 1 d . . . H45A H 0.6944 0.5889 0.9368 0.057 Uiso 1 1 calc R . . C46 C 0.71748(8) 0.4654(3) 0.98733(18) 0.0503(10) Uani 1 1 d . . . H46A H 0.7356 0.5000 0.9928 0.060 Uiso 1 1 calc R . . C47 C 0.71589(7) 0.3629(3) 1.01284(16) 0.0407(9) Uani 1 1 d . . . H47A H 0.7329 0.3285 1.0368 0.049 Uiso 1 1 calc R . . C48 C 0.68980(6) 0.3090(2) 1.00406(13) 0.0284(7) Uani 1 1 d . . . C49 C 0.63911(7) 0.5326(2) 0.91234(15) 0.0390(8) Uani 1 1 d . . . H49A H 0.6239 0.4767 0.8950 0.047 Uiso 1 1 calc R . . C50 C 0.62910(9) 0.6029(3) 0.95859(18) 0.0693(13) Uani 1 1 d . . . H50A H 0.6259 0.5553 0.9913 0.104 Uiso 1 1 calc R . . H50B H 0.6112 0.6403 0.9376 0.104 Uiso 1 1 calc R . . H50C H 0.6437 0.6582 0.9766 0.104 Uiso 1 1 calc R . . C51 C 0.64197(10) 0.6057(3) 0.85945(18) 0.0658(12) Uani 1 1 d . . . H51A H 0.6490 0.5614 0.8303 0.099 Uiso 1 1 calc R . . H51B H 0.6555 0.6656 0.8757 0.099 Uiso 1 1 calc R . . H51C H 0.6233 0.6372 0.8384 0.099 Uiso 1 1 calc R . . C52 C 0.68832(6) 0.1974(2) 1.03391(14) 0.0333(8) Uani 1 1 d . . . H52A H 0.6698 0.1616 1.0118 0.040 Uiso 1 1 calc R . . C53 C 0.68870(7) 0.2122(3) 1.10185(15) 0.0447(9) Uani 1 1 d . . . H53A H 0.6724 0.2579 1.1043 0.067 Uiso 1 1 calc R . . H53B H 0.7065 0.2484 1.1243 0.067 Uiso 1 1 calc R . . H53C H 0.6874 0.1396 1.1202 0.067 Uiso 1 1 calc R . . C54 C 0.71260(7) 0.1205(3) 1.02926(16) 0.0485(9) Uani 1 1 d . . . H54A H 0.7135 0.1177 0.9865 0.073 Uiso 1 1 calc R . . H54B H 0.7091 0.0460 1.0427 0.073 Uiso 1 1 calc R . . H54C H 0.7308 0.1484 1.0556 0.073 Uiso 1 1 calc R . . C55 C 0.52859(15) 0.7665(6) 0.6264(3) 0.0571(19) Uiso 0.611(6) 1 d PD A 1 C56 C 0.52565(19) 0.7295(6) 0.5668(4) 0.068(3) Uiso 0.611(6) 1 d PD A 1 H56A H 0.5235 0.6528 0.5576 0.081 Uiso 0.611(6) 1 calc PR A 1 C57 C 0.5259(2) 0.8025(6) 0.5220(3) 0.053(3) Uiso 0.611(6) 1 d PD A 1 H57A H 0.5239 0.7765 0.4813 0.063 Uiso 0.611(6) 1 calc PR A 1 C58 C 0.52889(17) 0.9154(5) 0.5339(3) 0.066(2) Uiso 0.611(6) 1 d PD A 1 H58A H 0.5293 0.9657 0.5019 0.079 Uiso 0.611(6) 1 calc PR A 1 C59 C 0.53139(16) 0.9545(5) 0.5937(4) 0.066(2) Uiso 0.611(6) 1 d PD A 1 H59A H 0.5334 1.0313 0.6028 0.079 Uiso 0.611(6) 1 calc PR A 1 C60 C 0.53088(15) 0.8775(6) 0.6392(3) 0.053(2) Uiso 0.611(6) 1 d PD A 1 H60A H 0.5321 0.9022 0.6798 0.064 Uiso 0.611(6) 1 calc PR A 1 C61 C 0.52927(17) 0.6857(6) 0.6753(4) 0.093(3) Uiso 0.611(6) 1 d PDU A 1 H61A H 0.5316 0.7245 0.7144 0.140 Uiso 0.611(6) 1 calc PR A 1 H61B H 0.5454 0.6349 0.6790 0.140 Uiso 0.611(6) 1 calc PR A 1 H61C H 0.5113 0.6437 0.6651 0.140 Uiso 0.611(6) 1 calc PR A 1 C55A C 0.5245(2) 0.8167(10) 0.6461(4) 0.065(3) Uiso 0.389(6) 1 d PDU A 2 C56A C 0.5292(2) 0.9119(9) 0.6184(6) 0.065(3) Uiso 0.389(6) 1 d PDU A 2 H56B H 0.5320 0.9778 0.6422 0.078 Uiso 0.389(6) 1 calc PR A 2 C57A C 0.5303(3) 0.9191(9) 0.5579(7) 0.077(3) Uiso 0.389(6) 1 d PDU A 2 H57B H 0.5335 0.9884 0.5410 0.092 Uiso 0.389(6) 1 calc PR A 2 C58A C 0.5268(4) 0.8266(11) 0.5232(6) 0.070(4) Uiso 0.389(6) 1 d PDU A 2 H58B H 0.5276 0.8285 0.4817 0.084 Uiso 0.389(6) 1 calc PR A 2 C59A C 0.5220(3) 0.7280(9) 0.5507(6) 0.073(4) Uiso 0.389(6) 1 d PDU A 2 H59B H 0.5194 0.6628 0.5263 0.087 Uiso 0.389(6) 1 calc PR A 2 C60A C 0.5205(3) 0.7178(9) 0.6108(5) 0.074(3) Uiso 0.389(6) 1 d PDU A 2 H60B H 0.5171 0.6487 0.6275 0.089 Uiso 0.389(6) 1 calc PR A 2 C61A C 0.5230(3) 0.8248(11) 0.7126(6) 0.105(5) Uiso 0.389(6) 1 d PDU A 2 H61D H 0.5268 0.9012 0.7271 0.157 Uiso 0.389(6) 1 calc PR A 2 H61E H 0.5375 0.7758 0.7387 0.157 Uiso 0.389(6) 1 calc PR A 2 H61F H 0.5040 0.8025 0.7149 0.157 Uiso 0.389(6) 1 calc PR A 2 C62 C 0.7181(3) 0.7930(10) 0.0068(7) 0.088(3) Uani 0.50 1 d PDU B -3 C63 C 0.7236(2) 0.8233(9) -0.0484(7) 0.082(2) Uani 0.50 1 d PDU B -3 H63A H 0.7103 0.8634 -0.0797 0.099 Uiso 0.50 1 calc PR B -3 C64 C 0.7508(2) 0.7892(10) -0.0539(7) 0.074(2) Uani 0.50 1 d PDU B -3 H64A H 0.7552 0.8082 -0.0911 0.089 Uiso 0.50 1 calc PR B -3 C65 C 0.7706(2) 0.7329(9) -0.0120(7) 0.076(2) Uani 0.50 1 d PDU B -3 H65A H 0.7883 0.7133 -0.0194 0.092 Uiso 0.50 1 calc PR B -3 C66 C 0.7646(2) 0.7035(10) 0.0439(7) 0.083(3) Uani 0.50 1 d PDU B -3 H66A H 0.7781 0.6649 0.0755 0.099 Uiso 0.50 1 calc PR B -3 C67 C 0.7388(3) 0.7328(11) 0.0500(8) 0.086(3) Uani 0.50 1 d PDU B -3 H67A H 0.7343 0.7107 0.0867 0.103 Uiso 0.50 1 calc PR B -3 C68 C 0.6992(2) 0.8081(8) 0.0068(5) 0.092(3) Uani 0.50 1 d PDU B -3 H68A H 0.6899 0.8525 -0.0295 0.138 Uiso 0.50 1 calc PR B -3 H68B H 0.6991 0.8492 0.0442 0.138 Uiso 0.50 1 calc PR B -3 H68C H 0.6887 0.7384 0.0057 0.138 Uiso 0.50 1 calc PR B -3 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Al1 0.0261(5) 0.0314(5) 0.0174(5) 0.0007(4) 0.0072(4) 0.0033(4) Al2 0.0268(5) 0.0322(5) 0.0179(5) -0.0012(4) 0.0055(4) 0.0045(4) Cl1 0.0311(4) 0.0606(5) 0.0258(5) -0.0049(4) 0.0066(3) -0.0112(4) Cl2 0.0544(6) 0.0411(5) 0.0316(5) 0.0088(4) 0.0191(4) 0.0217(4) Cl3 0.0650(6) 0.0391(4) 0.0272(5) 0.0058(4) 0.0087(4) 0.0204(4) Cl4 0.0289(5) 0.0696(6) 0.0388(5) -0.0164(4) 0.0115(4) -0.0067(4) N1 0.0259(13) 0.0223(12) 0.0184(14) -0.0006(10) 0.0073(10) 0.0010(10) N2 0.0251(13) 0.0207(12) 0.0186(14) 0.0012(10) 0.0056(10) 0.0021(10) N3 0.0262(13) 0.0212(12) 0.0177(13) 0.0009(10) 0.0068(10) 0.0024(10) N4 0.0266(14) 0.0249(12) 0.0179(14) 0.0010(10) 0.0084(10) 0.0009(10) N5 0.0229(14) 0.0396(14) 0.0177(14) -0.0020(11) 0.0056(10) -0.0014(11) N6 0.0241(13) 0.0316(13) 0.0152(13) -0.0016(11) 0.0057(10) -0.0004(11) C1 0.0192(15) 0.0215(14) 0.0200(17) -0.0017(12) 0.0045(12) -0.0048(12) C2 0.0356(18) 0.0271(15) 0.0163(16) -0.0007(13) 0.0105(13) 0.0012(13) C3 0.0314(17) 0.0256(15) 0.0210(17) -0.0042(13) 0.0101(13) 0.0033(13) C4 0.0311(17) 0.0224(14) 0.0188(16) 0.0020(12) 0.0118(13) 0.0029(13) C5 0.0304(17) 0.0281(15) 0.0203(17) 0.0039(13) 0.0113(13) 0.0046(13) C6 0.0310(18) 0.0381(18) 0.0247(18) 0.0068(14) 0.0107(14) 0.0101(14) C7 0.052(2) 0.0251(16) 0.0304(19) 0.0071(14) 0.0198(16) 0.0080(15) C8 0.043(2) 0.0227(15) 0.0301(19) -0.0001(14) 0.0159(15) -0.0036(14) C9 0.0359(18) 0.0236(15) 0.0203(17) 0.0013(13) 0.0147(13) -0.0005(13) C10 0.0288(17) 0.0334(17) 0.0282(19) 0.0047(14) 0.0044(14) 0.0021(14) C11 0.0284(19) 0.060(2) 0.045(2) 0.0045(18) 0.0053(16) -0.0036(17) C12 0.044(2) 0.048(2) 0.041(2) -0.0077(17) 0.0055(16) -0.0055(17) C13 0.0278(18) 0.0250(15) 0.039(2) -0.0026(14) 0.0054(14) -0.0044(13) C14 0.039(2) 0.069(2) 0.046(2) -0.020(2) 0.0116(17) -0.0121(18) C15 0.033(2) 0.068(2) 0.065(3) -0.023(2) 0.0221(19) -0.0075(18) C16 0.0304(17) 0.0259(15) 0.0159(16) 0.0000(13) 0.0064(12) 0.0083(13) C17 0.0342(18) 0.0242(15) 0.0212(17) -0.0034(13) 0.0092(13) 0.0036(13) C18 0.052(2) 0.0258(16) 0.030(2) 0.0019(14) 0.0127(16) 0.0054(15) C19 0.055(2) 0.0361(19) 0.033(2) 0.0072(16) 0.0041(17) 0.0204(17) C20 0.033(2) 0.048(2) 0.038(2) -0.0027(17) 0.0002(15) 0.0132(16) C21 0.0294(18) 0.0342(17) 0.0242(18) -0.0028(14) 0.0043(13) 0.0068(14) C22 0.0338(18) 0.0225(15) 0.035(2) -0.0024(14) 0.0115(14) -0.0007(13) C23 0.039(2) 0.053(2) 0.034(2) 0.0024(17) 0.0072(15) -0.0109(16) C24 0.051(2) 0.053(2) 0.043(2) 0.0023(18) 0.0207(18) -0.0067(18) C25 0.0226(18) 0.048(2) 0.050(2) -0.0025(17) 0.0003(15) -0.0018(15) C26 0.047(2) 0.102(3) 0.047(3) -0.002(2) 0.0110(19) -0.028(2) C27 0.033(2) 0.061(2) 0.058(3) -0.019(2) 0.0017(17) -0.0007(17) C28 0.0256(16) 0.0237(15) 0.0154(16) 0.0003(12) 0.0053(12) 0.0003(12) C29 0.0270(18) 0.057(2) 0.0178(18) -0.0031(15) 0.0112(13) -0.0024(15) C30 0.0299(18) 0.0467(19) 0.0135(16) -0.0060(14) 0.0079(13) -0.0026(14) C31 0.0251(17) 0.0483(19) 0.0136(16) -0.0012(14) 0.0067(12) -0.0088(14) C32 0.0377(19) 0.0468(19) 0.0207(18) -0.0006(15) 0.0127(14) -0.0099(15) C33 0.046(2) 0.053(2) 0.032(2) -0.0103(17) 0.0184(17) -0.0218(18) C34 0.028(2) 0.082(3) 0.033(2) -0.013(2) 0.0093(16) -0.0167(19) C35 0.0268(19) 0.075(3) 0.028(2) -0.0019(18) 0.0049(15) 0.0012(18) C36 0.0247(17) 0.053(2) 0.0199(18) -0.0014(15) 0.0081(13) 0.0008(15) C37 0.046(2) 0.0431(19) 0.036(2) 0.0074(17) 0.0149(16) -0.0049(16) C38 0.094(3) 0.051(2) 0.042(3) 0.009(2) 0.000(2) 0.003(2) C39 0.075(3) 0.050(2) 0.052(3) 0.000(2) 0.026(2) 0.004(2) C40 0.0286(19) 0.049(2) 0.041(2) 0.0052(17) 0.0086(15) 0.0020(15) C41 0.059(3) 0.052(2) 0.053(3) -0.010(2) 0.013(2) 0.0013(19) C42 0.044(2) 0.078(3) 0.053(3) 0.019(2) 0.0144(19) 0.019(2) C43 0.0257(17) 0.0298(16) 0.0228(17) -0.0099(13) 0.0098(13) -0.0075(13) C44 0.044(2) 0.0288(16) 0.0302(19) -0.0070(14) 0.0198(15) -0.0027(15) C45 0.058(3) 0.0271(17) 0.066(3) -0.0119(17) 0.034(2) -0.0097(17) C46 0.039(2) 0.045(2) 0.073(3) -0.024(2) 0.027(2) -0.0190(18) C47 0.0267(18) 0.045(2) 0.050(2) -0.0167(17) 0.0094(16) -0.0081(15) C48 0.0263(17) 0.0333(16) 0.0251(18) -0.0125(14) 0.0064(13) -0.0040(13) C49 0.057(2) 0.0275(16) 0.036(2) 0.0009(15) 0.0191(17) 0.0052(16) C50 0.095(4) 0.067(3) 0.053(3) 0.006(2) 0.033(2) 0.042(2) C51 0.106(4) 0.051(2) 0.049(3) 0.011(2) 0.035(2) 0.008(2) C52 0.0280(18) 0.0363(17) 0.0292(19) -0.0026(15) -0.0027(14) -0.0037(14) C53 0.044(2) 0.052(2) 0.036(2) 0.0037(17) 0.0077(16) 0.0000(17) C54 0.046(2) 0.048(2) 0.045(2) 0.0006(18) 0.0026(17) 0.0112(17) C62 0.082(7) 0.054(4) 0.099(4) -0.016(4) -0.021(5) -0.009(4) C63 0.079(7) 0.043(4) 0.092(4) -0.007(4) -0.033(5) 0.000(4) C64 0.074(7) 0.035(4) 0.081(4) 0.000(4) -0.034(5) 0.001(4) C65 0.078(7) 0.036(4) 0.082(4) 0.005(4) -0.033(5) -0.002(4) C66 0.088(7) 0.047(5) 0.083(4) 0.002(4) -0.028(6) -0.011(5) C67 0.089(7) 0.052(5) 0.089(4) -0.003(4) -0.023(5) -0.015(5) C68 0.086(7) 0.059(4) 0.105(5) -0.032(4) -0.019(5) 0.002(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Al1 N4 1.861(2) . ? Al1 N1 1.874(2) . ? Al1 Cl2 2.1239(11) . ? Al1 Cl1 2.1416(11) . ? Al1 Al2 2.6920(12) . ? Al2 N1 1.866(2) . ? Al2 N4 1.871(2) . ? Al2 Cl4 2.1217(12) . ? Al2 Cl3 2.1414(11) . ? N1 C1 1.313(3) . ? N2 C1 1.384(3) . ? N2 C2 1.390(3) . ? N2 C4 1.454(3) . ? N3 C1 1.382(3) . ? N3 C3 1.384(3) . ? N3 C16 1.454(3) . ? N4 C28 1.321(3) . ? N5 C28 1.371(3) . ? N5 C29 1.386(4) . ? N5 C31 1.447(3) . ? N6 C28 1.379(3) . ? N6 C30 1.394(4) . ? N6 C43 1.438(3) . ? C2 C3 1.320(4) . ? C4 C5 1.397(4) . ? C4 C9 1.400(4) . ? C5 C6 1.390(4) . ? C5 C10 1.514(4) . ? C6 C7 1.372(4) . ? C7 C8 1.375(4) . ? C8 C9 1.397(4) . ? C9 C13 1.511(4) . ? C10 C12 1.525(4) . ? C10 C11 1.528(4) . ? C13 C14 1.519(4) . ? C13 C15 1.535(4) . ? C16 C17 1.397(4) . ? C16 C21 1.398(4) . ? C17 C18 1.393(4) . ? C17 C22 1.517(4) . ? C18 C19 1.380(4) . ? C19 C20 1.374(5) . ? C20 C21 1.400(4) . ? C21 C25 1.512(4) . ? C22 C24 1.525(4) . ? C22 C23 1.526(4) . ? C25 C26 1.533(5) . ? C25 C27 1.534(4) . ? C29 C30 1.331(4) . ? C31 C36 1.401(4) . ? C31 C32 1.404(4) . ? C32 C33 1.391(4) . ? C32 C37 1.514(4) . ? C33 C34 1.377(5) . ? C34 C35 1.374(5) . ? C35 C36 1.392(4) . ? C36 C40 1.519(4) . ? C37 C38 1.525(5) . ? C37 C39 1.528(4) . ? C40 C41 1.531(5) . ? C40 C42 1.532(4) . ? C43 C44 1.402(4) . ? C43 C48 1.403(4) . ? C44 C45 1.386(4) . ? C44 C49 1.513(4) . ? C45 C46 1.381(5) . ? C46 C47 1.377(5) . ? C47 C48 1.391(4) . ? C48 C52 1.519(4) . ? C49 C51 1.523(4) . ? C49 C50 1.526(4) . ? C52 C54 1.528(4) . ? C52 C53 1.539(4) . ? C55 C60 1.371(8) . ? C55 C56 1.388(8) . ? C55 C61 1.467(9) . ? C56 C57 1.345(8) . ? C57 C58 1.391(8) . ? C58 C59 1.403(8) . ? C59 C60 1.392(8) . ? C55A C56A 1.359(10) . ? C55A C60A 1.421(10) . ? C55A C61A 1.526(15) . ? C56A C57A 1.384(11) . ? C57A C58A 1.349(11) . ? C58A C59A 1.393(11) . ? C59A C60A 1.383(11) . ? C62 C68 0.938(13) . ? C62 C63 1.393(10) . ? C62 C67 1.398(10) . ? C63 C64 1.422(9) . ? C63 C68 1.95(2) . ? C64 C65 1.338(9) . ? C65 C66 1.416(10) . ? C66 C67 1.349(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N4 Al1 N1 87.78(10) . . ? N4 Al1 Cl2 107.99(8) . . ? N1 Al1 Cl2 122.25(8) . . ? N4 Al1 Cl1 120.95(8) . . ? N1 Al1 Cl1 107.01(8) . . ? Cl2 Al1 Cl1 110.20(5) . . ? N4 Al1 Al2 43.97(7) . . ? N1 Al1 Al2 43.84(7) . . ? Cl2 Al1 Al2 127.19(5) . . ? Cl1 Al1 Al2 122.60(5) . . ? N1 Al2 N4 87.72(10) . . ? N1 Al2 Cl4 108.53(8) . . ? N4 Al2 Cl4 122.20(8) . . ? N1 Al2 Cl3 120.74(8) . . ? N4 Al2 Cl3 107.02(8) . . ? Cl4 Al2 Cl3 109.98(5) . . ? N1 Al2 Al1 44.08(7) . . ? N4 Al2 Al1 43.68(7) . . ? Cl4 Al2 Al1 127.61(5) . . ? Cl3 Al2 Al1 122.42(5) . . ? C1 N1 Al2 135.51(19) . . ? C1 N1 Al1 132.36(19) . . ? Al2 N1 Al1 92.08(11) . . ? C1 N2 C2 110.0(2) . . ? C1 N2 C4 126.3(2) . . ? C2 N2 C4 121.8(2) . . ? C1 N3 C3 110.1(2) . . ? C1 N3 C16 128.0(2) . . ? C3 N3 C16 121.8(2) . . ? C28 N4 Al1 132.7(2) . . ? C28 N4 Al2 134.9(2) . . ? Al1 N4 Al2 92.35(11) . . ? C28 N5 C29 110.2(2) . . ? C28 N5 C31 129.3(2) . . ? C29 N5 C31 120.5(2) . . ? C28 N6 C30 109.6(2) . . ? C28 N6 C43 127.5(2) . . ? C30 N6 C43 121.4(2) . . ? N1 C1 N3 128.9(2) . . ? N1 C1 N2 127.3(2) . . ? N3 C1 N2 103.9(2) . . ? C3 C2 N2 107.8(3) . . ? C2 C3 N3 108.2(2) . . ? C5 C4 C9 123.6(2) . . ? C5 C4 N2 118.8(2) . . ? C9 C4 N2 117.4(2) . . ? C6 C5 C4 116.5(3) . . ? C6 C5 C10 120.5(3) . . ? C4 C5 C10 123.0(2) . . ? C7 C6 C5 121.7(3) . . ? C6 C7 C8 120.3(3) . . ? C7 C8 C9 121.3(3) . . ? C8 C9 C4 116.4(3) . . ? C8 C9 C13 120.8(3) . . ? C4 C9 C13 122.7(2) . . ? C5 C10 C12 111.3(2) . . ? C5 C10 C11 112.3(3) . . ? C12 C10 C11 109.9(3) . . ? C9 C13 C14 114.3(3) . . ? C9 C13 C15 110.4(3) . . ? C14 C13 C15 109.1(3) . . ? C17 C16 C21 124.0(3) . . ? C17 C16 N3 118.0(2) . . ? C21 C16 N3 117.6(2) . . ? C18 C17 C16 116.6(3) . . ? C18 C17 C22 121.1(3) . . ? C16 C17 C22 122.3(2) . . ? C19 C18 C17 121.2(3) . . ? C20 C19 C18 120.5(3) . . ? C19 C20 C21 121.5(3) . . ? C16 C21 C20 116.2(3) . . ? C16 C21 C25 123.6(3) . . ? C20 C21 C25 120.1(3) . . ? C17 C22 C24 112.6(3) . . ? C17 C22 C23 110.5(2) . . ? C24 C22 C23 110.3(3) . . ? C21 C25 C26 110.9(3) . . ? C21 C25 C27 113.1(3) . . ? C26 C25 C27 109.2(3) . . ? N4 C28 N5 128.3(2) . . ? N4 C28 N6 127.0(3) . . ? N5 C28 N6 104.7(2) . . ? C30 C29 N5 107.9(3) . . ? C29 C30 N6 107.6(3) . . ? C36 C31 C32 123.3(3) . . ? C36 C31 N5 117.6(3) . . ? C32 C31 N5 118.8(3) . . ? C33 C32 C31 116.5(3) . . ? C33 C32 C37 121.9(3) . . ? C31 C32 C37 121.5(3) . . ? C34 C33 C32 121.2(3) . . ? C35 C34 C33 121.1(3) . . ? C34 C35 C36 120.7(3) . . ? C35 C36 C31 117.1(3) . . ? C35 C36 C40 119.5(3) . . ? C31 C36 C40 123.4(3) . . ? C32 C37 C38 112.9(3) . . ? C32 C37 C39 113.2(3) . . ? C38 C37 C39 109.2(3) . . ? C36 C40 C41 111.6(3) . . ? C36 C40 C42 112.7(3) . . ? C41 C40 C42 108.0(3) . . ? C44 C43 C48 123.4(3) . . ? C44 C43 N6 117.8(3) . . ? C48 C43 N6 118.6(3) . . ? C45 C44 C43 116.4(3) . . ? C45 C44 C49 121.6(3) . . ? C43 C44 C49 122.0(3) . . ? C46 C45 C44 121.9(3) . . ? C47 C46 C45 120.3(3) . . ? C46 C47 C48 121.0(3) . . ? C47 C48 C43 117.0(3) . . ? C47 C48 C52 120.4(3) . . ? C43 C48 C52 122.6(3) . . ? C44 C49 C51 114.0(3) . . ? C44 C49 C50 110.6(3) . . ? C51 C49 C50 109.2(3) . . ? C48 C52 C54 112.2(3) . . ? C48 C52 C53 110.5(2) . . ? C54 C52 C53 109.9(3) . . ? C60 C55 C56 120.0(6) . . ? C60 C55 C61 120.6(7) . . ? C56 C55 C61 119.4(7) . . ? C57 C56 C55 119.9(7) . . ? C56 C57 C58 121.3(6) . . ? C57 C58 C59 119.6(6) . . ? C60 C59 C58 118.0(6) . . ? C55 C60 C59 121.0(6) . . ? C56A C55A C60A 117.9(8) . . ? C56A C55A C61A 117.3(11) . . ? C60A C55A C61A 124.8(11) . . ? C55A C56A C57A 124.4(8) . . ? C58A C57A C56A 119.2(9) . . ? C57A C58A C59A 117.4(9) . . ? C60A C59A C58A 125.0(9) . . ? C59A C60A C55A 116.1(8) . . ? C68 C62 C63 112.2(15) . . ? C68 C62 C67 128.2(16) . . ? C63 C62 C67 118.9(8) . . ? C62 C63 C64 114.5(7) . . ? C62 C63 C68 26.4(5) . . ? C64 C63 C68 140.6(7) . . ? C65 C64 C63 126.3(8) . . ? C64 C65 C66 118.2(8) . . ? C67 C66 C65 116.9(8) . . ? C66 C67 C62 125.1(9) . . ? C62 C68 C63 41.4(11) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.455 _refine_diff_density_min -0.390 _refine_diff_density_rms 0.052 _database_code_depnum_ccdc_archive 'CCDC 962238' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_cu-182 _audit_creation_method ; CrysAlisPro, Agilent Technologies, Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET) (compiled Dec 3 2012,18:21:49) ; _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C54 H72 Al2 I4 N6, 6(C4 H8 O)' _chemical_formula_sum 'C78 H120 Al2 I4 N6 O6' _chemical_formula_weight 1799.36 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Al Al 0.2130 0.2455 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.3257 6.8362 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 22.3083(5) _cell_length_b 16.8446(3) _cell_length_c 24.0034(5) _cell_angle_alpha 90.00 _cell_angle_beta 114.736(3) _cell_angle_gamma 90.00 _cell_volume 8192.3(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 12227 _cell_measurement_theta_min 4.0600 _cell_measurement_theta_max 73.7010 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.459 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3664 _exptl_absorpt_coefficient_mu 12.558 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.0618 _exptl_absorpt_correction_T_max 0.1167 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET) (compiled Dec 3 2012,18:21:49) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'SuperNova (Cu) X-ray Source' _diffrn_radiation_monochromator mirror _diffrn_measurement_device_type 'SuperNova, Single source at offset), Atlas' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16135 _diffrn_reflns_av_R_equivalents 0.0479 _diffrn_reflns_av_sigmaI/netI 0.0479 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.41 _diffrn_reflns_theta_max 67.50 _reflns_number_total 7374 _reflns_number_gt 6995 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET) (compiled Dec 3 2012,18:21:49) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET) (compiled Dec 3 2012,18:21:49) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET) (compiled Dec 3 2012,18:21:49) ; _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^)+(0.0842P)^2^+193.7993P] 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 7374 _refine_ls_number_parameters 443 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0695 _refine_ls_R_factor_gt 0.0643 _refine_ls_wR_factor_ref 0.1822 _refine_ls_wR_factor_gt 0.1799 _refine_ls_goodness_of_fit_ref 1.062 _refine_ls_restrained_S_all 1.062 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group I1 I 0.35939(2) 0.40090(3) 0.11088(2) 0.02852(17) Uani 1 1 d . . . I2 I 0.54882(2) 0.36527(3) 0.12945(2) 0.02802(16) Uani 1 1 d . . . Al1 Al 0.47820(10) 0.38336(12) 0.18865(10) 0.0200(4) Uani 1 1 d . . . N1 N 0.5000 0.4606(5) 0.2500 0.0201(17) Uani 1 2 d S . . N2 N 0.5000 0.3059(5) 0.2500 0.0194(16) Uani 1 2 d S . . N3 N 0.5177(3) 0.5895(3) 0.2142(3) 0.0207(12) Uani 1 1 d . . . N4 N 0.4542(3) 0.1773(3) 0.2083(3) 0.0210(12) Uani 1 1 d . . . C1 C 0.5000 0.5398(6) 0.2500 0.0195(19) Uani 1 2 d S . . C2 C 0.5111(4) 0.6687(4) 0.2283(4) 0.0257(15) Uani 1 1 d . . . H2 H 0.5208 0.7142 0.2102 0.031 Uiso 1 1 calc R . . C3 C 0.5498(4) 0.5747(4) 0.1738(4) 0.0224(14) Uani 1 1 d . . . C4 C 0.6183(4) 0.5602(4) 0.2001(4) 0.0255(15) Uani 1 1 d . . . C5 C 0.6500(4) 0.5622(5) 0.1617(4) 0.0318(17) Uani 1 1 d . . . H5 H 0.6963 0.5533 0.1785 0.038 Uiso 1 1 calc R . . C6 C 0.6167(4) 0.5767(5) 0.0993(4) 0.0352(18) Uani 1 1 d . . . H6 H 0.6400 0.5782 0.0741 0.042 Uiso 1 1 calc R . . C7 C 0.5489(4) 0.5891(5) 0.0741(4) 0.0303(17) Uani 1 1 d . . . H7 H 0.5258 0.5978 0.0312 0.036 Uiso 1 1 calc R . . C8 C 0.5142(4) 0.5888(4) 0.1108(4) 0.0245(15) Uani 1 1 d . . . C9 C 0.6550(4) 0.5437(5) 0.2680(4) 0.0318(17) Uani 1 1 d . . . H9 H 0.6242 0.5139 0.2810 0.038 Uiso 1 1 calc R . . C10 C 0.7160(4) 0.4929(6) 0.2842(5) 0.042(2) Uani 1 1 d . . . H10A H 0.7064 0.4496 0.2544 0.064 Uiso 1 1 calc R . . H10B H 0.7292 0.4706 0.3254 0.064 Uiso 1 1 calc R . . H10C H 0.7520 0.5255 0.2834 0.064 Uiso 1 1 calc R . . C11 C 0.6744(5) 0.6206(6) 0.3061(5) 0.047(2) Uani 1 1 d . . . H11A H 0.6986 0.6073 0.3496 0.071 Uiso 1 1 calc R . . H11B H 0.6345 0.6504 0.3002 0.071 Uiso 1 1 calc R . . H11C H 0.7024 0.6530 0.2927 0.071 Uiso 1 1 calc R . . C12 C 0.4406(4) 0.6048(5) 0.0820(4) 0.0295(17) Uani 1 1 d . . . H12 H 0.4223 0.5882 0.1118 0.035 Uiso 1 1 calc R . . C13 C 0.4261(5) 0.6939(6) 0.0684(5) 0.051(3) Uani 1 1 d . . . H13A H 0.4438 0.7115 0.0393 0.076 Uiso 1 1 calc R . . H13B H 0.4471 0.7242 0.1066 0.076 Uiso 1 1 calc R . . H13C H 0.3784 0.7028 0.0507 0.076 Uiso 1 1 calc R . . C14 C 0.4053(4) 0.5570(6) 0.0230(4) 0.039(2) Uani 1 1 d . . . H14A H 0.4176 0.5777 -0.0089 0.059 Uiso 1 1 calc R . . H14B H 0.3575 0.5616 0.0094 0.059 Uiso 1 1 calc R . . H14C H 0.4183 0.5011 0.0308 0.059 Uiso 1 1 calc R . . C15 C 0.5000 0.2271(6) 0.2500 0.0172(18) Uani 1 2 d S . . C16 C 0.4722(4) 0.0981(4) 0.2243(4) 0.0255(15) Uani 1 1 d . . . H16 H 0.4490 0.0526 0.2025 0.031 Uiso 1 1 calc R . . C17 C 0.3895(3) 0.1909(4) 0.1595(4) 0.0229(15) Uani 1 1 d . . . C18 C 0.3807(4) 0.1789(4) 0.0989(4) 0.0284(16) Uani 1 1 d . . . C19 C 0.3159(4) 0.1758(5) 0.0541(4) 0.0351(19) Uani 1 1 d . . . H19 H 0.3080 0.1663 0.0126 0.042 Uiso 1 1 calc R . . C20 C 0.2629(4) 0.1864(5) 0.0691(4) 0.038(2) Uani 1 1 d . . . H20 H 0.2192 0.1836 0.0378 0.045 Uiso 1 1 calc R . . C21 C 0.2729(4) 0.2008(5) 0.1285(4) 0.0342(19) Uani 1 1 d . . . H21 H 0.2360 0.2089 0.1379 0.041 Uiso 1 1 calc R . . C22 C 0.3368(4) 0.2038(4) 0.1758(4) 0.0274(16) Uani 1 1 d . . . C23 C 0.4372(4) 0.1685(5) 0.0808(4) 0.0342(18) Uani 1 1 d . . . H23 H 0.4786 0.1858 0.1161 0.041 Uiso 1 1 calc R . . C24 C 0.4281(5) 0.2201(6) 0.0249(4) 0.044(2) Uani 1 1 d . . . H24A H 0.3928 0.1978 -0.0120 0.066 Uiso 1 1 calc R . . H24B H 0.4694 0.2210 0.0197 0.066 Uiso 1 1 calc R . . H24C H 0.4163 0.2743 0.0314 0.066 Uiso 1 1 calc R . . C25 C 0.4455(6) 0.0804(6) 0.0670(6) 0.054(3) Uani 1 1 d . . . H25A H 0.4547 0.0484 0.1038 0.082 Uiso 1 1 calc R . . H25B H 0.4822 0.0755 0.0549 0.082 Uiso 1 1 calc R . . H25C H 0.4048 0.0615 0.0336 0.082 Uiso 1 1 calc R . . C26 C 0.3482(4) 0.2188(5) 0.2419(4) 0.0319(17) Uani 1 1 d . . . H26 H 0.3886 0.2527 0.2607 0.038 Uiso 1 1 calc R . . C27 C 0.2920(5) 0.2643(6) 0.2472(5) 0.046(2) Uani 1 1 d . . . H27A H 0.2542 0.2287 0.2378 0.069 Uiso 1 1 calc R . . H27B H 0.2790 0.3087 0.2182 0.069 Uiso 1 1 calc R . . H27C H 0.3065 0.2847 0.2891 0.069 Uiso 1 1 calc R . . C28 C 0.3616(6) 0.1433(7) 0.2800(5) 0.052(3) Uani 1 1 d . . . H28A H 0.3697 0.1569 0.3223 0.078 Uiso 1 1 calc R . . H28B H 0.4005 0.1165 0.2798 0.078 Uiso 1 1 calc R . . H28C H 0.3233 0.1080 0.2625 0.078 Uiso 1 1 calc R . . C29 C 0.7678(6) 0.4063(8) 0.1368(9) 0.083(5) Uani 1 1 d . . . H29A H 0.7419 0.3966 0.0925 0.100 Uiso 1 1 calc R . . H29B H 0.7371 0.4139 0.1565 0.100 Uiso 1 1 calc R . . C30 C 0.8101(6) 0.4741(7) 0.1467(10) 0.088(5) Uani 1 1 d . . . H30A H 0.7920 0.5098 0.1107 0.105 Uiso 1 1 calc R . . H30B H 0.8126 0.5040 0.1831 0.105 Uiso 1 1 calc R . . O31 O 0.8740(4) 0.4479(4) 0.1559(4) 0.060(2) Uani 1 1 d . . . C32 C 0.8773(6) 0.3647(7) 0.1648(6) 0.056(3) Uani 1 1 d . . . H32A H 0.9150 0.3511 0.2039 0.067 Uiso 1 1 calc R . . H32B H 0.8837 0.3380 0.1309 0.067 Uiso 1 1 calc R . . C33 C 0.8147(6) 0.3382(7) 0.1663(6) 0.057(3) Uani 1 1 d . . . H33A H 0.8202 0.3294 0.2089 0.068 Uiso 1 1 calc R . . H33B H 0.7987 0.2886 0.1426 0.068 Uiso 1 1 calc R . . C39 C 0.0995(5) 0.2959(6) 0.1491(5) 0.049(2) Uani 1 1 d . . . H39A H 0.0767 0.2703 0.1085 0.059 Uiso 1 1 calc R . . H39B H 0.1307 0.2574 0.1778 0.059 Uiso 1 1 calc R . . O40 O 0.0525(4) 0.3221(4) 0.1718(4) 0.0473(16) Uani 1 1 d . . . C41 C 0.0392(6) 0.4030(7) 0.1573(8) 0.072(4) Uani 1 1 d . . . H41A H 0.0481 0.4340 0.1950 0.086 Uiso 1 1 calc R . . H41B H -0.0077 0.4104 0.1287 0.086 Uiso 1 1 calc R . . C42 C 0.0832(6) 0.4306(7) 0.1279(7) 0.065(3) Uani 1 1 d . . . H42A H 0.0584 0.4345 0.0829 0.078 Uiso 1 1 calc R . . H42B H 0.1026 0.4831 0.1442 0.078 Uiso 1 1 calc R . . C43 C 0.1352(6) 0.3694(7) 0.1443(6) 0.053(3) Uani 1 1 d . . . H43A H 0.1728 0.3817 0.1838 0.064 Uiso 1 1 calc R . . H43B H 0.1515 0.3638 0.1119 0.064 Uiso 1 1 calc R . . O34 O 0.2103(6) 0.7088(9) 0.0516(6) 0.101(4) Uani 1 1 d . . . C35 C 0.2216(8) 0.6520(10) 0.0188(7) 0.079(4) Uani 1 1 d . . . H35A H 0.2693 0.6392 0.0370 0.094 Uiso 1 1 calc R . . H35B H 0.2095 0.6715 -0.0235 0.094 Uiso 1 1 calc R . . C36 C 0.1832(9) 0.5784(11) 0.0163(8) 0.091(5) Uani 1 1 d . . . H36A H 0.2097 0.5395 0.0480 0.109 Uiso 1 1 calc R . . H36B H 0.1663 0.5530 -0.0246 0.109 Uiso 1 1 calc R . . C37 C 0.1268(10) 0.6134(14) 0.0298(12) 0.123(8) Uani 1 1 d . . . H37A H 0.0888 0.6296 -0.0083 0.147 Uiso 1 1 calc R . . H37B H 0.1118 0.5758 0.0529 0.147 Uiso 1 1 calc R . . C38 C 0.1616(8) 0.6841(13) 0.0683(7) 0.093(6) Uani 1 1 d . . . H38A H 0.1297 0.7277 0.0621 0.111 Uiso 1 1 calc R . . H38B H 0.1812 0.6694 0.1123 0.111 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 0.0238(3) 0.0180(3) 0.0363(3) 0.00133(18) 0.0053(2) 0.00128(17) I2 0.0332(3) 0.0178(3) 0.0385(3) -0.00247(18) 0.0203(2) -0.00098(17) Al1 0.0208(10) 0.0085(9) 0.0292(11) 0.0000(8) 0.0088(8) -0.0005(7) N1 0.021(4) 0.008(4) 0.032(4) 0.000 0.011(3) 0.000 N2 0.017(4) 0.008(4) 0.030(4) 0.000 0.007(3) 0.000 N3 0.025(3) 0.007(3) 0.032(3) 0.001(2) 0.013(3) 0.000(2) N4 0.016(3) 0.011(3) 0.033(3) -0.001(2) 0.007(2) -0.001(2) C1 0.019(4) 0.013(5) 0.026(5) 0.000 0.009(4) 0.000 C2 0.031(4) 0.007(3) 0.041(4) 0.002(3) 0.017(3) 0.001(3) C3 0.024(3) 0.010(3) 0.036(4) 0.001(3) 0.015(3) -0.003(3) C4 0.025(4) 0.012(3) 0.039(4) 0.000(3) 0.014(3) -0.001(3) C5 0.026(4) 0.020(4) 0.053(5) -0.005(3) 0.021(4) -0.003(3) C6 0.042(5) 0.029(4) 0.043(5) -0.009(4) 0.026(4) -0.007(4) C7 0.036(4) 0.023(4) 0.037(4) -0.003(3) 0.019(4) -0.003(3) C8 0.029(4) 0.012(3) 0.031(4) 0.000(3) 0.012(3) -0.003(3) C9 0.023(4) 0.023(4) 0.045(5) 0.007(3) 0.011(3) -0.001(3) C10 0.026(4) 0.035(5) 0.063(6) 0.014(4) 0.015(4) 0.007(4) C11 0.037(5) 0.043(5) 0.048(5) -0.011(4) 0.004(4) -0.004(4) C12 0.027(4) 0.023(4) 0.035(4) 0.003(3) 0.009(3) 0.005(3) C13 0.043(5) 0.024(5) 0.067(7) 0.003(4) 0.006(5) 0.009(4) C14 0.036(4) 0.045(5) 0.037(5) -0.003(4) 0.015(4) -0.005(4) C15 0.016(4) 0.009(4) 0.027(5) 0.000 0.009(4) 0.000 C16 0.025(3) 0.008(3) 0.040(4) -0.005(3) 0.011(3) -0.002(3) C17 0.019(3) 0.008(3) 0.038(4) 0.000(3) 0.008(3) -0.002(3) C18 0.028(4) 0.015(3) 0.035(4) 0.002(3) 0.005(3) -0.002(3) C19 0.033(4) 0.024(4) 0.036(4) 0.002(3) 0.003(3) -0.006(3) C20 0.022(4) 0.025(4) 0.051(5) 0.005(4) -0.001(4) -0.004(3) C21 0.019(4) 0.018(4) 0.060(6) 0.005(4) 0.010(4) -0.001(3) C22 0.019(3) 0.009(3) 0.051(5) 0.004(3) 0.013(3) -0.002(3) C23 0.038(4) 0.026(4) 0.040(4) -0.005(3) 0.017(4) -0.008(3) C24 0.053(6) 0.039(5) 0.039(5) -0.002(4) 0.018(4) -0.010(4) C25 0.076(7) 0.026(5) 0.079(8) -0.001(5) 0.050(6) 0.004(5) C26 0.024(4) 0.025(4) 0.050(5) -0.005(4) 0.019(4) -0.005(3) C27 0.039(5) 0.044(6) 0.067(6) -0.010(5) 0.034(5) -0.002(4) C28 0.057(6) 0.053(6) 0.061(6) 0.014(5) 0.038(5) 0.017(5) C29 0.050(7) 0.050(7) 0.161(16) 0.008(8) 0.055(9) 0.008(6) C30 0.060(7) 0.021(5) 0.188(18) 0.001(7) 0.056(9) 0.003(5) O31 0.043(4) 0.027(3) 0.109(7) -0.009(4) 0.031(4) -0.009(3) C32 0.054(6) 0.043(6) 0.070(7) 0.010(5) 0.027(6) 0.008(5) C33 0.068(7) 0.032(5) 0.072(7) 0.010(5) 0.032(6) 0.000(5) C39 0.053(6) 0.037(5) 0.068(7) -0.004(5) 0.035(5) -0.007(4) O40 0.054(4) 0.028(3) 0.069(4) 0.008(3) 0.035(4) -0.001(3) C41 0.059(7) 0.036(6) 0.133(13) 0.034(7) 0.052(8) 0.016(5) C42 0.068(7) 0.035(6) 0.101(10) 0.018(6) 0.043(7) -0.004(5) C43 0.056(6) 0.044(6) 0.069(7) -0.012(5) 0.036(6) -0.020(5) O34 0.100(8) 0.113(10) 0.090(8) -0.001(7) 0.040(7) -0.012(7) C35 0.087(10) 0.081(10) 0.075(9) -0.015(8) 0.041(8) -0.019(8) C36 0.100(12) 0.077(10) 0.088(11) -0.005(9) 0.032(9) -0.027(9) C37 0.091(13) 0.123(18) 0.15(2) -0.007(15) 0.052(14) -0.026(13) C38 0.085(10) 0.130(16) 0.063(8) 0.028(9) 0.031(8) 0.039(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag I1 Al1 2.541(2) . ? I2 Al1 2.543(2) . ? Al1 N1 1.871(6) . ? Al1 N2 1.874(6) . ? Al1 Al1 2.688(4) 2_655 ? N1 C1 1.335(13) . ? N1 Al1 1.871(6) 2_655 ? N2 C15 1.326(13) . ? N2 Al1 1.874(6) 2_655 ? N3 C1 1.370(9) . ? N3 C2 1.399(9) . ? N3 C3 1.448(10) . ? N4 C15 1.376(8) . ? N4 C16 1.401(9) . ? N4 C17 1.447(9) . ? C1 N3 1.370(9) 2_655 ? C2 C2 1.326(16) 2_655 ? C3 C8 1.402(11) . ? C3 C4 1.409(10) . ? C4 C5 1.379(12) . ? C4 C9 1.512(12) . ? C5 C6 1.386(13) . ? C6 C7 1.391(12) . ? C7 C8 1.395(11) . ? C8 C12 1.516(11) . ? C9 C10 1.515(11) . ? C9 C11 1.540(13) . ? C12 C14 1.529(12) . ? C12 C13 1.542(11) . ? C15 N4 1.376(8) 2_655 ? C16 C16 1.334(16) 2_655 ? C17 C18 1.401(12) . ? C17 C22 1.402(11) . ? C18 C19 1.396(11) . ? C18 C23 1.503(12) . ? C19 C20 1.382(14) . ? C20 C21 1.371(14) . ? C21 C22 1.403(11) . ? C22 C26 1.518(12) . ? C23 C24 1.540(13) . ? C23 C25 1.548(13) . ? C26 C27 1.521(11) . ? C26 C28 1.522(13) . ? C29 C30 1.437(18) . ? C29 C33 1.513(17) . ? C30 O31 1.419(14) . ? O31 C32 1.415(13) . ? C32 C33 1.481(16) . ? C39 O40 1.437(12) . ? C39 C43 1.502(14) . ? O40 C41 1.408(13) . ? C41 C42 1.503(17) . ? C42 C43 1.476(17) . ? O34 C35 1.329(19) . ? O34 C38 1.37(2) . ? C35 C36 1.49(2) . ? C36 C37 1.54(3) . ? C37 C38 1.51(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Al1 N2 88.2(3) . . ? N1 Al1 I1 110.19(13) . . ? N2 Al1 I1 120.42(11) . . ? N1 Al1 I2 120.36(11) . . ? N2 Al1 I2 109.76(13) . . ? I1 Al1 I2 107.64(8) . . ? N1 Al1 Al1 44.08(19) . 2_655 ? N2 Al1 Al1 44.17(19) . 2_655 ? I1 Al1 Al1 126.37(12) . 2_655 ? I2 Al1 Al1 125.99(12) . 2_655 ? C1 N1 Al1 134.08(19) . . ? C1 N1 Al1 134.08(19) . 2_655 ? Al1 N1 Al1 91.8(4) . 2_655 ? C15 N2 Al1 134.17(19) . 2_655 ? C15 N2 Al1 134.17(19) . . ? Al1 N2 Al1 91.7(4) 2_655 . ? C1 N3 C2 110.0(6) . . ? C1 N3 C3 132.0(6) . . ? C2 N3 C3 117.2(6) . . ? C15 N4 C16 110.0(6) . . ? C15 N4 C17 132.7(6) . . ? C16 N4 C17 116.5(6) . . ? N1 C1 N3 127.6(4) . . ? N1 C1 N3 127.6(4) . 2_655 ? N3 C1 N3 104.8(8) . 2_655 ? C2 C2 N3 107.6(4) 2_655 . ? C8 C3 C4 122.1(7) . . ? C8 C3 N3 118.6(6) . . ? C4 C3 N3 118.4(7) . . ? C5 C4 C3 117.4(7) . . ? C5 C4 C9 121.8(7) . . ? C3 C4 C9 120.8(7) . . ? C4 C5 C6 122.2(8) . . ? C5 C6 C7 119.4(8) . . ? C6 C7 C8 120.9(8) . . ? C7 C8 C3 117.9(7) . . ? C7 C8 C12 119.5(7) . . ? C3 C8 C12 122.6(7) . . ? C4 C9 C10 113.8(8) . . ? C4 C9 C11 112.1(7) . . ? C10 C9 C11 108.9(7) . . ? C8 C12 C14 111.6(7) . . ? C8 C12 C13 111.0(7) . . ? C14 C12 C13 109.7(7) . . ? N2 C15 N4 127.6(4) . . ? N2 C15 N4 127.6(4) . 2_655 ? N4 C15 N4 104.8(8) . 2_655 ? C16 C16 N4 107.6(4) 2_655 . ? C18 C17 C22 122.9(7) . . ? C18 C17 N4 118.4(7) . . ? C22 C17 N4 118.0(7) . . ? C19 C18 C17 117.0(8) . . ? C19 C18 C23 119.9(8) . . ? C17 C18 C23 123.2(7) . . ? C20 C19 C18 121.3(9) . . ? C21 C20 C19 120.6(8) . . ? C20 C21 C22 121.1(8) . . ? C17 C22 C21 117.1(8) . . ? C17 C22 C26 121.5(7) . . ? C21 C22 C26 121.4(7) . . ? C18 C23 C24 111.4(8) . . ? C18 C23 C25 111.3(7) . . ? C24 C23 C25 109.7(8) . . ? C22 C26 C27 112.8(7) . . ? C22 C26 C28 113.3(7) . . ? C27 C26 C28 109.3(8) . . ? C30 C29 C33 104.4(11) . . ? O31 C30 C29 109.0(9) . . ? C32 O31 C30 108.5(8) . . ? O31 C32 C33 108.2(9) . . ? C32 C33 C29 103.6(9) . . ? O40 C39 C43 105.7(8) . . ? C41 O40 C39 108.4(8) . . ? O40 C41 C42 107.7(10) . . ? C43 C42 C41 104.7(9) . . ? C42 C43 C39 102.4(9) . . ? C35 O34 C38 109.1(15) . . ? O34 C35 C36 111.9(14) . . ? C35 C36 C37 100.3(15) . . ? C38 C37 C36 100.1(15) . . ? O34 C38 C37 109.1(15) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 67.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.682 _refine_diff_density_min -1.598 _refine_diff_density_rms 0.182 _database_code_depnum_ccdc_archive 'CCDC 962239' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_franz9 _audit_creation_method ; CrysAlisPro, Agilent Technologies, Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET) (compiled Dec 3 2012,18:21:49) ; _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C61 H80 Li2 N6' _chemical_formula_weight 911.19 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 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' Li Li -0.0003 0.0001 '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' _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 11.1147(7) _cell_length_b 14.8792(11) _cell_length_c 17.4898(10) _cell_angle_alpha 81.656(5) _cell_angle_beta 80.281(5) _cell_angle_gamma 82.250(6) _cell_volume 2802.6(3) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 2791 _cell_measurement_theta_min 3.5670 _cell_measurement_theta_max 26.8490 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.080 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 988 _exptl_absorpt_coefficient_mu 0.062 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9828 _exptl_absorpt_correction_T_max 0.9938 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET) (compiled Dec 3 2012,18:21:49) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Sapphire3' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20755 _diffrn_reflns_av_R_equivalents 0.0834 _diffrn_reflns_av_sigmaI/netI 0.1306 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.43 _diffrn_reflns_theta_max 25.00 _reflns_number_total 9860 _reflns_number_gt 5769 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET) (compiled Dec 3 2012,18:21:49) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET) (compiled Dec 3 2012,18:21:49) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET) (compiled Dec 3 2012,18:21:49) ; _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^)+(0.0383P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9860 _refine_ls_number_parameters 702 _refine_ls_number_restraints 168 _refine_ls_R_factor_all 0.1524 _refine_ls_R_factor_gt 0.0840 _refine_ls_wR_factor_ref 0.1672 _refine_ls_wR_factor_gt 0.1389 _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_restrained_S_all 1.064 _refine_ls_shift/su_max 0.000 _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 Li1 Li 0.0191(5) 0.5624(4) 0.4501(3) 0.0340(14) Uani 1 1 d . . . Li2 Li 0.4900(5) 1.0693(4) 0.0274(3) 0.0356(14) Uani 1 1 d . . . N1 N 0.0605(2) 0.42891(18) 0.44886(14) 0.0285(7) Uani 1 1 d . . . N2 N 0.1831(2) 0.45155(17) 0.32222(14) 0.0233(6) Uani 1 1 d . . . N3 N 0.1908(2) 0.30948(17) 0.38207(13) 0.0231(6) Uani 1 1 d . . . N4 N 0.5327(2) 0.95492(19) 0.07804(14) 0.0309(7) Uani 1 1 d . . . N5 N 0.5810(2) 0.88186(18) 0.20525(13) 0.0233(6) Uani 1 1 d . . . N6 N 0.5881(2) 0.79407(18) 0.11254(14) 0.0267(6) Uani 1 1 d . . . C1 C 0.1332(3) 0.4002(2) 0.39331(17) 0.0223(7) Uani 1 1 d . . . C2 C 0.2676(3) 0.3968(2) 0.27559(18) 0.0290(8) Uani 1 1 d . . . H2A H 0.3143 0.4168 0.2269 0.035 Uiso 1 1 calc R . . C3 C 0.2714(3) 0.3108(2) 0.31174(17) 0.0273(8) Uani 1 1 d . . . H3A H 0.3209 0.2592 0.2926 0.033 Uiso 1 1 calc R . . C4 C 0.1600(3) 0.5489(2) 0.31590(17) 0.0246(8) Uani 1 1 d . . . C5 C 0.0561(3) 0.5922(2) 0.28319(18) 0.0282(8) Uani 1 1 d . B . C6 C 0.0272(3) 0.6863(3) 0.2862(2) 0.0402(9) Uani 1 1 d . . . H6A H -0.0423 0.7172 0.2647 0.048 Uiso 1 1 calc R . . C7 C 0.0970(3) 0.7354(3) 0.3196(2) 0.0437(10) Uani 1 1 d . . . H7A H 0.0759 0.7993 0.3207 0.052 Uiso 1 1 calc R . . C8 C 0.1982(3) 0.6907(2) 0.3516(2) 0.0393(9) Uani 1 1 d . . . H8A H 0.2463 0.7249 0.3742 0.047 Uiso 1 1 calc R . . C9 C 0.2313(3) 0.5973(2) 0.35156(18) 0.0293(8) Uani 1 1 d . . . C10 C -0.0226(3) 0.5401(3) 0.2470(2) 0.0414(9) Uani 1 1 d U . . H10 H 0.0244 0.4797 0.2370 0.050 Uiso 1 1 calc R A 1 C11 C -0.1383(13) 0.5235(10) 0.2967(9) 0.052(3) Uani 0.50 1 d PU B 1 H11A H -0.1218 0.4856 0.3453 0.079 Uiso 0.50 1 calc PR B 1 H11B H -0.1865 0.4917 0.2694 0.079 Uiso 0.50 1 calc PR B 1 H11C H -0.1844 0.5819 0.3087 0.079 Uiso 0.50 1 calc PR B 1 C12 C -0.0491(9) 0.5962(8) 0.1642(7) 0.048(2) Uani 0.50 1 d PU B 1 H12A H 0.0290 0.6052 0.1302 0.072 Uiso 0.50 1 calc PR B 1 H12B H -0.0950 0.6558 0.1729 0.072 Uiso 0.50 1 calc PR B 1 H12C H -0.0975 0.5617 0.1393 0.072 Uiso 0.50 1 calc PR B 1 C11A C -0.1615(13) 0.5527(10) 0.2841(9) 0.054(3) Uani 0.50 1 d PU B 2 H11D H -0.1705 0.5264 0.3392 0.080 Uiso 0.50 1 calc PR B 2 H11E H -0.2095 0.5217 0.2560 0.080 Uiso 0.50 1 calc PR B 2 H11F H -0.1914 0.6180 0.2804 0.080 Uiso 0.50 1 calc PR B 2 C12A C -0.0069(11) 0.5640(9) 0.1609(7) 0.067(3) Uani 0.50 1 d PU B 2 H12D H 0.0788 0.5470 0.1387 0.101 Uiso 0.50 1 calc PR B 2 H12E H -0.0282 0.6299 0.1481 0.101 Uiso 0.50 1 calc PR B 2 H12F H -0.0608 0.5308 0.1391 0.101 Uiso 0.50 1 calc PR B 2 C13 C 0.3396(3) 0.5500(2) 0.38977(18) 0.0334(8) Uani 1 1 d . . . H13A H 0.3375 0.4826 0.3930 0.040 Uiso 1 1 calc R . . C14 C 0.4608(3) 0.5731(3) 0.3405(2) 0.0523(11) Uani 1 1 d . . . H14A H 0.4665 0.5542 0.2885 0.078 Uiso 1 1 calc R . . H14B H 0.5293 0.5408 0.3658 0.078 Uiso 1 1 calc R . . H14C H 0.4646 0.6392 0.3354 0.078 Uiso 1 1 calc R . . C15 C 0.3311(3) 0.5732(3) 0.47295(19) 0.0456(10) Uani 1 1 d . . . H15A H 0.2513 0.5601 0.5029 0.068 Uiso 1 1 calc R . . H15B H 0.3398 0.6382 0.4712 0.068 Uiso 1 1 calc R . . H15C H 0.3969 0.5362 0.4981 0.068 Uiso 1 1 calc R . . C16 C 0.1663(3) 0.2313(2) 0.43742(16) 0.0228(7) Uani 1 1 d . . . C17 C 0.0557(3) 0.1933(2) 0.44140(18) 0.0267(8) Uani 1 1 d . . . C18 C 0.0323(3) 0.1188(2) 0.49637(19) 0.0340(9) Uani 1 1 d . . . H18A H -0.0421 0.0927 0.5000 0.041 Uiso 1 1 calc R . . C19 C 0.1156(3) 0.0812(2) 0.54669(19) 0.0362(9) Uani 1 1 d . . . H19A H 0.0987 0.0294 0.5838 0.043 Uiso 1 1 calc R . . C20 C 0.2231(3) 0.1200(2) 0.54219(18) 0.0357(9) Uani 1 1 d . . . H20A H 0.2795 0.0943 0.5769 0.043 Uiso 1 1 calc R . . C21 C 0.2510(3) 0.1951(2) 0.48864(17) 0.0269(8) Uani 1 1 d . . . C22 C -0.0340(3) 0.2336(2) 0.38513(18) 0.0322(8) Uani 1 1 d . . . H22A H -0.0311 0.3012 0.3759 0.039 Uiso 1 1 calc R . . C23 C -0.1671(3) 0.2166(3) 0.4176(2) 0.0487(11) Uani 1 1 d . . . H23A H -0.1885 0.2344 0.4704 0.073 Uiso 1 1 calc R . . H23B H -0.1756 0.1516 0.4194 0.073 Uiso 1 1 calc R . . H23C H -0.2222 0.2531 0.3837 0.073 Uiso 1 1 calc R . . C24 C 0.0044(3) 0.1970(3) 0.30588(19) 0.0558(12) Uani 1 1 d . . . H24A H 0.0864 0.2134 0.2829 0.084 Uiso 1 1 calc R . . H24B H -0.0546 0.2239 0.2708 0.084 Uiso 1 1 calc R . . H24C H 0.0058 0.1303 0.3134 0.084 Uiso 1 1 calc R . . C25 C 0.3642(3) 0.2421(2) 0.48889(19) 0.0351(9) Uani 1 1 d . . . H25A H 0.3940 0.2671 0.4337 0.042 Uiso 1 1 calc R . . C26 C 0.4710(3) 0.1790(3) 0.5205(2) 0.0480(10) Uani 1 1 d . . . H26A H 0.4883 0.1241 0.4937 0.072 Uiso 1 1 calc R . . H26B H 0.4485 0.1613 0.5768 0.072 Uiso 1 1 calc R . . H26C H 0.5443 0.2113 0.5111 0.072 Uiso 1 1 calc R . . C27 C 0.3285(3) 0.3227(3) 0.5368(2) 0.0491(10) Uani 1 1 d . . . H27A H 0.2666 0.3663 0.5134 0.074 Uiso 1 1 calc R . . H27B H 0.4014 0.3530 0.5370 0.074 Uiso 1 1 calc R . . H27C H 0.2948 0.3002 0.5906 0.074 Uiso 1 1 calc R . . C28 C 0.5626(3) 0.8885(2) 0.12551(17) 0.0252(8) Uani 1 1 d . . . C29 C 0.6179(3) 0.7918(2) 0.23384(18) 0.0306(8) Uani 1 1 d . . . H29A H 0.6369 0.7714 0.2849 0.037 Uiso 1 1 calc R . . C30 C 0.6221(3) 0.7388(2) 0.17797(18) 0.0311(8) Uani 1 1 d . . . H30A H 0.6444 0.6745 0.1823 0.037 Uiso 1 1 calc R . . C31 C 0.5799(3) 0.9594(2) 0.24522(16) 0.0244(7) Uani 1 1 d . . . C32 C 0.6861(3) 1.0031(2) 0.23529(17) 0.0298(8) Uani 1 1 d . D . C33 C 0.6832(3) 1.0775(2) 0.27546(19) 0.0397(9) Uani 1 1 d . . . H33A H 0.7544 1.1081 0.2701 0.048 Uiso 1 1 calc R . . C34 C 0.5776(3) 1.1073(3) 0.3233(2) 0.0430(10) Uani 1 1 d . . . H34A H 0.5770 1.1584 0.3503 0.052 Uiso 1 1 calc R . . C35 C 0.4736(3) 1.0642(2) 0.33221(19) 0.0372(9) Uani 1 1 d . . . H35A H 0.4021 1.0858 0.3654 0.045 Uiso 1 1 calc R . . C36 C 0.4714(3) 0.9895(2) 0.29338(17) 0.0280(8) Uani 1 1 d . . . C37 C 0.8018(3) 0.9715(3) 0.1821(2) 0.0425(9) Uani 1 1 d U . . H37 H 0.7841 0.9226 0.1534 0.051 Uiso 1 1 calc R C 3 C38 C 0.8984(14) 0.9354(13) 0.2277(12) 0.057(3) Uani 0.50 1 d PU D 3 H38A H 0.8723 0.8832 0.2650 0.085 Uiso 0.50 1 calc PR D 3 H38B H 0.9156 0.9830 0.2563 0.085 Uiso 0.50 1 calc PR D 3 H38C H 0.9728 0.9155 0.1929 0.085 Uiso 0.50 1 calc PR D 3 C39 C 0.8380(15) 1.0569(9) 0.1213(8) 0.061(3) Uani 0.50 1 d PU D 3 H39A H 0.7686 1.0816 0.0937 0.092 Uiso 0.50 1 calc PR D 3 H39B H 0.9091 1.0378 0.0834 0.092 Uiso 0.50 1 calc PR D 3 H39C H 0.8587 1.1040 0.1490 0.092 Uiso 0.50 1 calc PR D 3 C38A C 0.9248(14) 0.9566(13) 0.2197(11) 0.049(3) Uani 0.50 1 d PU D 4 H38D H 0.9097 0.9238 0.2726 0.073 Uiso 0.50 1 calc PR D 4 H38E H 0.9516 1.0161 0.2222 0.073 Uiso 0.50 1 calc PR D 4 H38F H 0.9890 0.9208 0.1874 0.073 Uiso 0.50 1 calc PR D 4 C39A C 0.8215(14) 1.0288(9) 0.1058(8) 0.051(3) Uani 0.50 1 d PU D 4 H39D H 0.7490 1.0325 0.0799 0.076 Uiso 0.50 1 calc PR D 4 H39E H 0.8937 1.0016 0.0730 0.076 Uiso 0.50 1 calc PR D 4 H39F H 0.8348 1.0904 0.1138 0.076 Uiso 0.50 1 calc PR D 4 C40 C 0.3553(3) 0.9428(3) 0.30084(19) 0.0357(9) Uani 1 1 d . . . H40A H 0.3811 0.8767 0.2954 0.043 Uiso 1 1 calc R . . C41 C 0.2703(3) 0.9481(3) 0.37872(19) 0.0477(11) Uani 1 1 d . . . H41A H 0.2026 0.9114 0.3811 0.072 Uiso 1 1 calc R . . H41B H 0.2372 1.0119 0.3833 0.072 Uiso 1 1 calc R . . H41C H 0.3167 0.9245 0.4217 0.072 Uiso 1 1 calc R . . C42 C 0.2838(3) 0.9833(3) 0.2337(2) 0.0586(13) Uani 1 1 d . . . H42A H 0.3368 0.9766 0.1836 0.088 Uiso 1 1 calc R . . H42B H 0.2575 1.0483 0.2375 0.088 Uiso 1 1 calc R . . H42C H 0.2115 0.9510 0.2372 0.088 Uiso 1 1 calc R . . C43 C 0.5727(3) 0.7712(2) 0.03890(17) 0.0252(8) Uani 1 1 d . . . C44 C 0.6722(3) 0.7731(2) -0.02200(18) 0.0320(8) Uani 1 1 d . . . C45 C 0.6513(3) 0.7593(3) -0.09588(19) 0.0428(10) Uani 1 1 d . . . H45A H 0.7174 0.7596 -0.1381 0.051 Uiso 1 1 calc R . . C46 C 0.5365(3) 0.7455(3) -0.1084(2) 0.0466(10) Uani 1 1 d . . . H46A H 0.5242 0.7365 -0.1591 0.056 Uiso 1 1 calc R . . C47 C 0.4393(3) 0.7446(2) -0.04801(19) 0.0387(9) Uani 1 1 d . . . H47A H 0.3609 0.7346 -0.0576 0.046 Uiso 1 1 calc R . . C48 C 0.4538(3) 0.7583(2) 0.02730(17) 0.0293(8) Uani 1 1 d . . . C49 C 0.7973(3) 0.7942(3) -0.0092(2) 0.0462(9) Uani 1 1 d U . . H49 H 0.8003 0.7798 0.0481 0.055 Uiso 1 1 calc R E 5 C50 C 0.9087(11) 0.7291(9) -0.0529(6) 0.061(3) Uani 0.50 1 d PU F 5 H50A H 0.8976 0.6649 -0.0345 0.092 Uiso 0.50 1 calc PR F 5 H50B H 0.9871 0.7423 -0.0410 0.092 Uiso 0.50 1 calc PR F 5 H50C H 0.9086 0.7408 -0.1095 0.092 Uiso 0.50 1 calc PR F 5 C51 C 0.8200(11) 0.8887(9) -0.0309(5) 0.056(2) Uani 0.50 1 d PU F 5 H51A H 0.7625 0.9272 0.0030 0.084 Uiso 0.50 1 calc PR F 5 H51B H 0.8084 0.9078 -0.0855 0.084 Uiso 0.50 1 calc PR F 5 H51C H 0.9045 0.8950 -0.0251 0.084 Uiso 0.50 1 calc PR F 5 C50A C 0.8886(11) 0.7167(9) -0.0162(6) 0.060(3) Uani 0.50 1 d PU F 6 H50D H 0.8643 0.6662 0.0235 0.091 Uiso 0.50 1 calc PR F 6 H50E H 0.9678 0.7332 -0.0085 0.091 Uiso 0.50 1 calc PR F 6 H50F H 0.8961 0.6978 -0.0683 0.091 Uiso 0.50 1 calc PR F 6 C51A C 0.8379(12) 0.8815(9) -0.0683(6) 0.064(3) Uani 0.50 1 d PU F 6 H51D H 0.7767 0.9343 -0.0595 0.096 Uiso 0.50 1 calc PR F 6 H51E H 0.8440 0.8685 -0.1223 0.096 Uiso 0.50 1 calc PR F 6 H51F H 0.9180 0.8949 -0.0594 0.096 Uiso 0.50 1 calc PR F 6 C52 C 0.3464(3) 0.7581(3) 0.09420(19) 0.0368(8) Uani 1 1 d U . . H52 H 0.3759 0.7801 0.1384 0.044 Uiso 1 1 calc R G 7 C53 C 0.3177(17) 0.6606(14) 0.1230(11) 0.050(3) Uani 0.50 1 d PU H 7 H53A H 0.3924 0.6229 0.1364 0.075 Uiso 0.50 1 calc PR H 7 H53B H 0.2880 0.6356 0.0817 0.075 Uiso 0.50 1 calc PR H 7 H53C H 0.2544 0.6605 0.1693 0.075 Uiso 0.50 1 calc PR H 7 C54 C 0.2382(13) 0.8219(8) 0.0771(9) 0.053(3) Uani 0.50 1 d PU H 7 H54A H 0.2610 0.8843 0.0652 0.080 Uiso 0.50 1 calc PR H 7 H54B H 0.1734 0.8184 0.1226 0.080 Uiso 0.50 1 calc PR H 7 H54C H 0.2082 0.8053 0.0320 0.080 Uiso 0.50 1 calc PR H 7 C53A C 0.3418(17) 0.6625(13) 0.1389(10) 0.040(3) Uani 0.50 1 d PU H 8 H53D H 0.4181 0.6435 0.1610 0.060 Uiso 0.50 1 calc PR H 8 H53E H 0.3328 0.6196 0.1033 0.060 Uiso 0.50 1 calc PR H 8 H53F H 0.2718 0.6630 0.1813 0.060 Uiso 0.50 1 calc PR H 8 C54A C 0.2182(13) 0.7910(8) 0.0660(9) 0.046(3) Uani 0.50 1 d PU H 8 H54D H 0.2208 0.8517 0.0356 0.069 Uiso 0.50 1 calc PR H 8 H54E H 0.1537 0.7943 0.1116 0.069 Uiso 0.50 1 calc PR H 8 H54F H 0.2005 0.7477 0.0333 0.069 Uiso 0.50 1 calc PR H 8 C55 C 0.6811(4) 0.4060(3) 0.1604(3) 0.0584(12) Uani 1 1 d . . . C56 C 0.5973(4) 0.4690(3) 0.1286(3) 0.0583(12) Uani 1 1 d . . . H56A H 0.5176 0.4805 0.1574 0.070 Uiso 1 1 calc R . . C57 C 0.6260(4) 0.5179(3) 0.0536(3) 0.0700(14) Uani 1 1 d . . . H57A H 0.5658 0.5621 0.0332 0.084 Uiso 1 1 calc R . . C58 C 0.7370(5) 0.5027(3) 0.0107(3) 0.0696(13) Uani 1 1 d . . . H58A H 0.7567 0.5355 -0.0396 0.084 Uiso 1 1 calc R . . C59 C 0.8247(4) 0.4352(4) 0.0437(3) 0.0792(16) Uani 1 1 d . . . H59A H 0.9039 0.4227 0.0145 0.095 Uiso 1 1 calc R . . C60 C 0.7965(4) 0.3885(4) 0.1159(3) 0.0686(14) Uani 1 1 d . . . H60A H 0.8559 0.3435 0.1364 0.082 Uiso 1 1 calc R . . C61 C 0.6513(4) 0.3543(3) 0.2379(3) 0.0836(15) Uani 1 1 d . . . H61A H 0.5620 0.3602 0.2537 0.125 Uiso 1 1 calc R . . H61B H 0.6898 0.3785 0.2759 0.125 Uiso 1 1 calc R . . H61C H 0.6823 0.2897 0.2358 0.125 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 Li1 0.042(4) 0.030(3) 0.030(3) -0.002(3) -0.005(3) -0.002(3) Li2 0.054(4) 0.025(3) 0.030(3) 0.003(3) -0.020(3) 0.000(3) N1 0.0304(16) 0.0278(17) 0.0260(15) -0.0056(14) 0.0006(12) -0.0027(12) N2 0.0242(14) 0.0224(16) 0.0215(14) 0.0006(12) -0.0011(11) -0.0031(12) N3 0.0246(15) 0.0238(16) 0.0199(14) -0.0020(13) -0.0022(11) -0.0011(12) N4 0.0385(17) 0.0281(18) 0.0262(15) 0.0036(14) -0.0143(12) 0.0004(13) N5 0.0243(15) 0.0236(16) 0.0218(14) 0.0015(13) -0.0110(11) 0.0026(12) N6 0.0398(17) 0.0175(15) 0.0228(14) -0.0006(13) -0.0098(12) 0.0010(12) C1 0.0229(17) 0.0206(18) 0.0252(18) -0.0016(15) -0.0080(14) -0.0047(14) C2 0.0254(18) 0.036(2) 0.0224(17) -0.0022(17) 0.0013(14) -0.0020(15) C3 0.0282(19) 0.025(2) 0.0270(18) -0.0035(16) -0.0014(14) 0.0006(15) C4 0.0261(18) 0.026(2) 0.0204(17) 0.0029(15) -0.0019(13) -0.0067(15) C5 0.0274(19) 0.029(2) 0.0274(18) -0.0010(16) -0.0034(14) -0.0041(15) C6 0.038(2) 0.036(2) 0.049(2) -0.005(2) -0.0221(17) 0.0054(18) C7 0.054(3) 0.026(2) 0.052(2) -0.0015(19) -0.0200(19) 0.0060(19) C8 0.048(2) 0.027(2) 0.049(2) -0.0045(19) -0.0195(18) -0.0084(17) C9 0.0266(19) 0.029(2) 0.0318(19) 0.0011(17) -0.0066(14) -0.0052(15) C10 0.0343(19) 0.049(2) 0.0455(19) -0.0139(19) -0.0169(15) -0.0005(17) C11 0.038(5) 0.062(7) 0.061(4) -0.004(4) -0.018(4) -0.009(5) C12 0.044(6) 0.059(6) 0.046(3) -0.013(4) -0.023(4) 0.002(4) C11A 0.034(4) 0.059(7) 0.071(6) -0.009(5) -0.016(4) -0.006(5) C12A 0.071(6) 0.088(7) 0.050(3) -0.009(5) -0.016(4) -0.027(5) C13 0.032(2) 0.032(2) 0.039(2) -0.0019(18) -0.0162(15) -0.0033(16) C14 0.035(2) 0.075(3) 0.045(2) -0.006(2) -0.0092(17) -0.001(2) C15 0.039(2) 0.054(3) 0.046(2) -0.004(2) -0.0172(17) -0.0010(19) C16 0.0326(19) 0.0176(18) 0.0166(16) -0.0023(15) -0.0005(13) -0.0009(14) C17 0.0281(19) 0.024(2) 0.0270(18) -0.0041(16) 0.0001(14) -0.0024(15) C18 0.037(2) 0.029(2) 0.037(2) -0.0065(18) -0.0014(16) -0.0111(17) C19 0.056(2) 0.021(2) 0.0270(19) 0.0083(16) -0.0009(17) -0.0050(18) C20 0.048(2) 0.034(2) 0.0260(19) 0.0001(18) -0.0140(16) 0.0017(18) C21 0.034(2) 0.024(2) 0.0212(17) -0.0001(16) -0.0040(14) -0.0025(15) C22 0.033(2) 0.027(2) 0.040(2) -0.0006(17) -0.0131(15) -0.0079(16) C23 0.030(2) 0.052(3) 0.064(3) -0.005(2) -0.0116(18) -0.0022(18) C24 0.045(2) 0.088(4) 0.041(2) -0.014(2) -0.0149(18) -0.010(2) C25 0.037(2) 0.040(2) 0.0297(19) -0.0014(18) -0.0152(15) -0.0011(17) C26 0.043(2) 0.055(3) 0.049(2) -0.006(2) -0.0207(18) 0.000(2) C27 0.053(2) 0.043(3) 0.061(3) -0.006(2) -0.0372(19) -0.005(2) C28 0.0225(18) 0.033(2) 0.0216(17) -0.0024(17) -0.0072(14) -0.0058(15) C29 0.039(2) 0.032(2) 0.0216(17) 0.0044(17) -0.0151(14) 0.0007(16) C30 0.041(2) 0.0194(19) 0.0301(19) 0.0039(17) -0.0082(15) 0.0021(16) C31 0.0305(19) 0.0237(19) 0.0195(16) 0.0003(15) -0.0115(14) 0.0013(15) C32 0.031(2) 0.039(2) 0.0218(17) -0.0007(17) -0.0085(14) -0.0079(16) C33 0.042(2) 0.042(2) 0.038(2) -0.0023(19) -0.0056(17) -0.0182(18) C34 0.055(3) 0.037(2) 0.042(2) -0.0146(19) -0.0104(19) -0.0114(19) C35 0.037(2) 0.034(2) 0.039(2) -0.0088(18) -0.0047(16) 0.0015(17) C36 0.0305(19) 0.028(2) 0.0250(18) -0.0005(16) -0.0085(14) -0.0014(15) C37 0.032(2) 0.063(3) 0.0369(19) -0.0132(17) -0.0025(15) -0.0168(17) C38 0.032(6) 0.070(7) 0.060(5) -0.003(4) 0.001(4) 0.013(5) C39 0.047(5) 0.077(6) 0.051(6) 0.006(4) 0.006(4) -0.005(5) C38A 0.028(5) 0.062(7) 0.053(5) -0.005(5) -0.007(4) 0.003(4) C39A 0.040(5) 0.077(7) 0.041(4) -0.007(4) -0.009(3) -0.021(4) C40 0.026(2) 0.040(2) 0.041(2) -0.0078(19) -0.0031(16) 0.0001(16) C41 0.036(2) 0.058(3) 0.048(2) 0.002(2) -0.0019(17) -0.0116(19) C42 0.035(2) 0.099(4) 0.046(2) -0.014(3) -0.0088(18) -0.014(2) C43 0.036(2) 0.0159(18) 0.0233(17) 0.0007(15) -0.0067(14) -0.0017(14) C44 0.031(2) 0.032(2) 0.034(2) -0.0042(17) -0.0073(15) -0.0029(16) C45 0.036(2) 0.061(3) 0.031(2) -0.013(2) 0.0058(16) -0.0077(19) C46 0.043(2) 0.069(3) 0.033(2) -0.017(2) -0.0095(17) -0.008(2) C47 0.029(2) 0.050(3) 0.040(2) -0.012(2) -0.0086(16) -0.0069(17) C48 0.032(2) 0.029(2) 0.0283(19) -0.0043(17) -0.0070(15) -0.0027(16) C49 0.0284(19) 0.068(2) 0.043(2) -0.006(2) -0.0075(16) -0.0080(17) C50 0.028(4) 0.081(5) 0.073(6) -0.014(5) -0.004(5) -0.003(4) C51 0.037(5) 0.072(3) 0.060(6) -0.008(5) 0.001(5) -0.018(3) C50A 0.033(5) 0.079(4) 0.069(7) -0.006(5) -0.014(5) -0.002(3) C51A 0.045(5) 0.081(5) 0.066(6) 0.006(5) -0.010(5) -0.018(4) C52 0.0287(18) 0.048(2) 0.0340(19) -0.0046(16) -0.0026(15) -0.0080(15) C53 0.041(7) 0.054(3) 0.049(7) 0.007(5) 0.001(5) -0.009(4) C54 0.035(5) 0.059(6) 0.055(5) 0.001(5) 0.006(4) 0.004(4) C53A 0.035(6) 0.053(4) 0.033(6) -0.001(4) -0.010(4) -0.007(4) C54A 0.030(4) 0.052(6) 0.051(5) -0.004(5) -0.003(3) 0.006(5) C55 0.068(3) 0.045(3) 0.072(3) -0.015(3) -0.028(3) -0.014(2) C56 0.058(3) 0.043(3) 0.075(3) -0.011(3) -0.015(2) -0.001(2) C57 0.070(3) 0.054(3) 0.090(4) -0.018(3) -0.027(3) 0.007(3) C58 0.083(4) 0.060(3) 0.072(3) -0.019(3) -0.019(3) -0.010(3) C59 0.064(3) 0.102(5) 0.082(4) -0.046(4) -0.021(3) 0.004(3) C60 0.046(3) 0.089(4) 0.079(3) -0.034(3) -0.018(2) 0.000(2) C61 0.094(4) 0.065(4) 0.103(4) 0.000(3) -0.034(3) -0.037(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Li1 N1 1.852(5) 2_566 ? Li1 N1 1.981(6) . ? Li1 Li1 2.387(11) 2_566 ? Li1 C4 2.610(6) . ? Li1 C9 2.738(6) . ? Li2 N4 1.841(6) . ? Li2 N4 1.992(6) 2_675 ? Li2 Li2 2.366(11) 2_675 ? Li2 C43 2.548(6) 2_675 ? Li2 C48 2.721(7) 2_675 ? Li2 C44 2.759(6) 2_675 ? N1 C1 1.241(3) . ? N1 Li1 1.852(5) 2_566 ? N2 C2 1.393(3) . ? N2 C4 1.428(4) . ? N2 C1 1.430(4) . ? N3 C3 1.393(3) . ? N3 C16 1.426(4) . ? N3 C1 1.439(4) . ? N4 C28 1.242(4) . ? N4 Li2 1.992(6) 2_675 ? N5 C29 1.393(4) . ? N5 C31 1.430(4) . ? N5 C28 1.431(4) . ? N6 C30 1.385(4) . ? N6 C43 1.421(4) . ? N6 C28 1.439(4) . ? C2 C3 1.341(4) . ? C4 C9 1.408(5) . ? C4 C5 1.411(4) . ? C5 C6 1.400(5) . ? C5 C10 1.510(5) . ? C6 C7 1.381(5) . ? C7 C8 1.387(5) . ? C8 C9 1.389(4) . ? C9 C13 1.516(4) . ? C10 C11 1.454(15) . ? C10 C12A 1.482(13) . ? C10 C11A 1.568(14) . ? C10 C12 1.615(12) . ? C13 C14 1.525(4) . ? C13 C15 1.528(4) . ? C16 C17 1.409(4) . ? C16 C21 1.410(4) . ? C17 C18 1.379(4) . ? C17 C22 1.523(4) . ? C18 C19 1.392(5) . ? C19 C20 1.381(5) . ? C20 C21 1.383(4) . ? C21 C25 1.520(5) . ? C22 C23 1.533(4) . ? C22 C24 1.535(4) . ? C25 C27 1.532(4) . ? C25 C26 1.539(4) . ? C29 C30 1.333(4) . ? C31 C32 1.397(4) . ? C31 C36 1.410(4) . ? C32 C33 1.388(5) . ? C32 C37 1.516(4) . ? C33 C34 1.382(4) . ? C34 C35 1.372(5) . ? C35 C36 1.390(4) . ? C36 C40 1.524(4) . ? C37 C38 1.445(17) . ? C37 C39A 1.476(13) . ? C37 C39 1.584(14) . ? C37 C38A 1.591(16) . ? C40 C41 1.526(4) . ? C40 C42 1.534(5) . ? C43 C44 1.400(4) . ? C43 C48 1.412(4) . ? C43 Li2 2.548(6) 2_675 ? C44 C45 1.399(4) . ? C44 C49 1.524(5) . ? C44 Li2 2.759(6) 2_675 ? C45 C46 1.378(5) . ? C46 C47 1.378(4) . ? C47 C48 1.401(4) . ? C48 C52 1.525(4) . ? C48 Li2 2.721(7) 2_675 ? C49 C50A 1.435(12) . ? C49 C51 1.446(12) . ? C49 C51A 1.603(12) . ? C49 C50 1.620(11) . ? C52 C54 1.472(14) . ? C52 C53 1.52(2) . ? C52 C53A 1.523(19) . ? C52 C54A 1.578(14) . ? C55 C56 1.358(6) . ? C55 C60 1.396(5) . ? C55 C61 1.468(6) . ? C56 C57 1.413(6) . ? C57 C58 1.340(5) . ? C58 C59 1.431(6) . ? C59 C60 1.359(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Li1 N1 103.0(3) 2_566 . ? N1 Li1 Li1 53.9(2) 2_566 2_566 ? N1 Li1 Li1 49.1(2) . 2_566 ? N1 Li1 C4 171.9(3) 2_566 . ? N1 Li1 C4 76.25(18) . . ? Li1 Li1 C4 124.8(3) 2_566 . ? N1 Li1 C9 142.5(3) 2_566 . ? N1 Li1 C9 91.6(2) . . ? Li1 Li1 C9 129.7(3) 2_566 . ? C4 Li1 C9 30.41(11) . . ? N4 Li2 N4 103.9(3) . 2_675 ? N4 Li2 Li2 54.8(2) . 2_675 ? N4 Li2 Li2 49.1(2) 2_675 2_675 ? N4 Li2 C43 178.3(3) . 2_675 ? N4 Li2 C43 77.4(2) 2_675 2_675 ? Li2 Li2 C43 126.5(4) 2_675 2_675 ? N4 Li2 C48 149.4(3) . 2_675 ? N4 Li2 C48 92.4(2) 2_675 2_675 ? Li2 Li2 C48 134.8(4) 2_675 2_675 ? C43 Li2 C48 30.88(12) 2_675 2_675 ? N4 Li2 C44 148.2(3) . 2_675 ? N4 Li2 C44 92.8(2) 2_675 2_675 ? Li2 Li2 C44 134.6(4) 2_675 2_675 ? C43 Li2 C44 30.25(11) 2_675 2_675 ? C48 Li2 C44 53.41(14) 2_675 2_675 ? C1 N1 Li1 160.2(3) . 2_566 ? C1 N1 Li1 119.3(3) . . ? Li1 N1 Li1 77.0(3) 2_566 . ? C2 N2 C4 129.3(2) . . ? C2 N2 C1 111.5(2) . . ? C4 N2 C1 117.9(2) . . ? C3 N3 C16 126.6(2) . . ? C3 N3 C1 110.6(2) . . ? C16 N3 C1 122.8(2) . . ? C28 N4 Li2 166.0(3) . . ? C28 N4 Li2 117.9(3) . 2_675 ? Li2 N4 Li2 76.1(3) . 2_675 ? C29 N5 C31 124.9(3) . . ? C29 N5 C28 110.8(3) . . ? C31 N5 C28 123.7(3) . . ? C30 N6 C43 130.4(3) . . ? C30 N6 C28 111.7(2) . . ? C43 N6 C28 118.0(2) . . ? N1 C1 N2 127.9(3) . . ? N1 C1 N3 131.0(3) . . ? N2 C1 N3 101.1(2) . . ? C3 C2 N2 107.8(3) . . ? C2 C3 N3 108.8(3) . . ? C9 C4 C5 121.9(3) . . ? C9 C4 N2 119.1(3) . . ? C5 C4 N2 118.4(3) . . ? C9 C4 Li1 79.8(2) . . ? C5 C4 Li1 84.9(2) . . ? N2 C4 Li1 98.3(2) . . ? C6 C5 C4 117.3(3) . . ? C6 C5 C10 120.6(3) . . ? C4 C5 C10 122.1(3) . . ? C7 C6 C5 121.8(3) . . ? C6 C7 C8 119.5(4) . . ? C7 C8 C9 121.8(4) . . ? C8 C9 C4 117.7(3) . . ? C8 C9 C13 120.4(3) . . ? C4 C9 C13 121.9(3) . . ? C8 C9 Li1 90.4(2) . . ? C4 C9 Li1 69.8(2) . . ? C13 C9 Li1 108.6(2) . . ? C11 C10 C12A 125.0(9) . . ? C11 C10 C5 113.2(8) . . ? C12A C10 C5 111.1(6) . . ? C11 C10 C11A 19.1(8) . . ? C12A C10 C11A 111.3(8) . . ? C5 C10 C11A 112.7(8) . . ? C11 C10 C12 109.7(7) . . ? C12A C10 C12 22.8(6) . . ? C5 C10 C12 108.9(6) . . ? C11A C10 C12 92.8(7) . . ? C9 C13 C14 111.1(3) . . ? C9 C13 C15 111.6(3) . . ? C14 C13 C15 110.9(3) . . ? C17 C16 C21 121.1(3) . . ? C17 C16 N3 119.1(3) . . ? C21 C16 N3 119.7(3) . . ? C18 C17 C16 118.4(3) . . ? C18 C17 C22 121.6(3) . . ? C16 C17 C22 120.0(3) . . ? C17 C18 C19 121.4(3) . . ? C20 C19 C18 119.3(3) . . ? C19 C20 C21 121.9(3) . . ? C20 C21 C16 117.9(3) . . ? C20 C21 C25 121.3(3) . . ? C16 C21 C25 120.5(3) . . ? C17 C22 C23 113.0(3) . . ? C17 C22 C24 111.0(3) . . ? C23 C22 C24 109.7(3) . . ? C21 C25 C27 109.4(3) . . ? C21 C25 C26 114.4(3) . . ? C27 C25 C26 109.3(3) . . ? N4 C28 N5 131.9(3) . . ? N4 C28 N6 127.4(3) . . ? N5 C28 N6 100.7(3) . . ? C30 C29 N5 109.0(3) . . ? C29 C30 N6 107.8(3) . . ? C32 C31 C36 121.9(3) . . ? C32 C31 N5 119.2(3) . . ? C36 C31 N5 118.9(3) . . ? C33 C32 C31 118.1(3) . . ? C33 C32 C37 120.3(3) . . ? C31 C32 C37 121.7(3) . . ? C34 C33 C32 120.6(3) . . ? C35 C34 C33 120.9(3) . . ? C34 C35 C36 121.0(3) . . ? C35 C36 C31 117.6(3) . . ? C35 C36 C40 121.5(3) . . ? C31 C36 C40 120.9(3) . . ? C38 C37 C39A 123.9(9) . . ? C38 C37 C32 110.1(9) . . ? C39A C37 C32 113.9(7) . . ? C38 C37 C39 111.9(8) . . ? C39A C37 C39 22.0(7) . . ? C32 C37 C39 107.3(6) . . ? C38 C37 C38A 16.2(11) . . ? C39A C37 C38A 109.3(8) . . ? C32 C37 C38A 115.5(8) . . ? C39 C37 C38A 95.8(8) . . ? C36 C40 C41 114.4(3) . . ? C36 C40 C42 109.7(3) . . ? C41 C40 C42 109.4(3) . . ? C44 C43 C48 122.3(3) . . ? C44 C43 N6 118.9(3) . . ? C48 C43 N6 118.4(3) . . ? C44 C43 Li2 83.3(2) . 2_675 ? C48 C43 Li2 81.3(2) . 2_675 ? N6 C43 Li2 99.3(2) . 2_675 ? C45 C44 C43 117.7(3) . . ? C45 C44 C49 121.1(3) . . ? C43 C44 C49 121.1(3) . . ? C45 C44 Li2 90.0(2) . 2_675 ? C43 C44 Li2 66.5(2) . 2_675 ? C49 C44 Li2 110.1(3) . 2_675 ? C46 C45 C44 121.1(3) . . ? C47 C46 C45 120.5(3) . . ? C46 C47 C48 121.3(3) . . ? C47 C48 C43 117.2(3) . . ? C47 C48 C52 121.5(3) . . ? C43 C48 C52 121.4(3) . . ? C47 C48 Li2 90.2(2) . 2_675 ? C43 C48 Li2 67.8(2) . 2_675 ? C52 C48 Li2 111.7(2) . 2_675 ? C50A C49 C51 125.2(7) . . ? C50A C49 C44 111.9(7) . . ? C51 C49 C44 115.0(6) . . ? C50A C49 C51A 111.5(7) . . ? C51 C49 C51A 24.7(5) . . ? C44 C49 C51A 110.0(6) . . ? C50A C49 C50 23.6(6) . . ? C51 C49 C50 109.2(6) . . ? C44 C49 C50 111.8(6) . . ? C51A C49 C50 90.5(6) . . ? C54 C52 C53 113.8(8) . . ? C54 C52 C53A 125.0(9) . . ? C53 C52 C53A 16.0(11) . . ? C54 C52 C48 114.0(7) . . ? C53 C52 C48 110.1(8) . . ? C53A C52 C48 110.2(8) . . ? C54 C52 C54A 22.5(7) . . ? C53 C52 C54A 94.9(8) . . ? C53A C52 C54A 108.6(8) . . ? C48 C52 C54A 113.1(6) . . ? C56 C55 C60 118.2(5) . . ? C56 C55 C61 121.7(4) . . ? C60 C55 C61 120.1(4) . . ? C55 C56 C57 121.5(4) . . ? C58 C57 C56 121.0(4) . . ? C57 C58 C59 117.6(5) . . ? C60 C59 C58 121.2(4) . . ? C59 C60 C55 120.6(5) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.306 _refine_diff_density_min -0.240 _refine_diff_density_rms 0.042 _database_code_depnum_ccdc_archive 'CCDC 962240'