# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _journal_volume ? _journal_year ? _journal_page_first ? _publ_contact_author_name 'Malcolm Chisholm' _publ_contact_author_address ; Department of Chemistry The Ohio State University 100 West 18th Avenue Columbus Ohio 43210 UNITED STATES OF AMERICA ; _publ_contact_author_email CHISHOLM@CHEMISTRY.OHIO-STATE.EDU _publ_section_title ; Concerning the relative importance of enantiomorphic site versus chain end control in the stereoselective polymerization of lactides: reactions of (R,R-salen)- and (S,S-salen)-aluminum alkoxides LAlOCH2R complexes (R == CH3 and S-CHMeCl) ; loop_ _publ_author_name 'Malcolm Chisholm' 'Nathan J. Patmore' data_chis1261 _database_code_depnum_ccdc_archive 'CCDC 243022' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C39 H58 Al Cl N2 O3' _chemical_formula_weight 665.30 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 14.9232(10) _cell_length_b 11.0214(10) _cell_length_c 23.440(3) _cell_angle_alpha 90.00 _cell_angle_beta 93.397(1) _cell_angle_gamma 90.00 _cell_volume 3848.6(7) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description chunk _exptl_crystal_colour yellow _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.148 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1440 _exptl_absorpt_coefficient_mu 0.159 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 60183 _diffrn_reflns_av_R_equivalents 0.073 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.58 _diffrn_reflns_theta_max 22.99 _reflns_number_total 10692 _reflns_number_gt 8295 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 1999)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _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. The large refine_ls_shift/su_max value is for the BASF parameter. This is due to SHELXL-97 trying to refine to a physically impossible negative value for the BASF parameter, that it automatically resets to 0.00001 at the start of every refinement cycle. The negative value of BASF is small (shift x error == -0.094) and within the error indicating the correct absolute structure has been found. However, despite numerous refinement cycles, this parameter will not change as SHELXL-97 is constantly reseting the BASF value to zero at the start of each refinement cycle. ; _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^)+(0.0819P)^2^+0.6290P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00(9) _refine_ls_number_reflns 10692 _refine_ls_number_parameters 886 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0749 _refine_ls_R_factor_gt 0.0508 _refine_ls_wR_factor_ref 0.1364 _refine_ls_wR_factor_gt 0.1237 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.021 _refine_ls_shift/su_max 1.073 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Al1 Al 0.09334(8) 0.17712(11) 0.37416(5) 0.0273(3) Uani 1 1 d . . . Al2 Al 0.91017(7) 0.42262(11) 0.12708(5) 0.0239(3) Uani 1 1 d . . . Cl1 Cl 0.24762(10) 0.04570(13) 0.20807(6) 0.0675(4) Uani 1 1 d . . . Cl2 Cl 0.74550(12) 0.54632(15) 0.29269(6) 0.0837(5) Uani 1 1 d . . . N1 N 0.1843(2) 0.3126(3) 0.38323(13) 0.0298(8) Uani 1 1 d . . . N2 N 0.0193(2) 0.3198(3) 0.34768(13) 0.0277(8) Uani 1 1 d . . . N3 N 0.8393(2) 0.2759(3) 0.10282(13) 0.0254(8) Uani 1 1 d . . . N4 N 0.9804(2) 0.2918(3) 0.16891(12) 0.0235(8) Uani 1 1 d . . . O1 O 0.14787(18) 0.1035(3) 0.43522(11) 0.0324(7) Uani 1 1 d . . . O2 O -0.00956(17) 0.0990(2) 0.38751(11) 0.0303(7) Uani 1 1 d . . . O3 O 0.13268(19) 0.1164(2) 0.31154(11) 0.0317(7) Uani 1 1 d . . . O4 O 0.85892(17) 0.4997(2) 0.06484(11) 0.0290(7) Uani 1 1 d . . . O5 O 1.01357(18) 0.5017(2) 0.11826(11) 0.0322(7) Uani 1 1 d . . . O6 O 0.85623(19) 0.4759(3) 0.18621(11) 0.0342(7) Uani 1 1 d . . . C1 C 0.2286(3) 0.1126(4) 0.46210(17) 0.0318(11) Uani 1 1 d . . . C2 C 0.2593(3) 0.0224(4) 0.50216(17) 0.0332(11) Uani 1 1 d . . . C3 C 0.3422(3) 0.0408(5) 0.53090(18) 0.0405(12) Uani 1 1 d . . . H3 H 0.3616 -0.0171 0.5577 0.049 Uiso 1 1 calc R . . C4 C 0.3990(3) 0.1397(5) 0.52275(19) 0.0442(12) Uani 1 1 d . A . C5 C 0.3684(3) 0.2231(5) 0.48274(19) 0.0439(13) Uani 1 1 d . . . H5 H 0.4045 0.2895 0.4754 0.053 Uiso 1 1 calc R . . C6 C 0.2857(3) 0.2123(4) 0.45272(17) 0.0321(11) Uani 1 1 d . . . C7 C 0.2009(3) -0.0889(5) 0.51527(17) 0.0390(12) Uani 1 1 d . . . C8 C 0.1148(3) -0.0450(5) 0.5414(2) 0.0505(14) Uani 1 1 d . . . H8A H 0.1302 0.0007 0.5755 0.076 Uiso 1 1 calc R . . H8B H 0.0790 -0.1137 0.5507 0.076 Uiso 1 1 calc R . . H8C H 0.0815 0.0055 0.5144 0.076 Uiso 1 1 calc R . . C9 C 0.1791(4) -0.1612(4) 0.4610(2) 0.0563(15) Uani 1 1 d . . . H9A H 0.2337 -0.1889 0.4457 0.084 Uiso 1 1 calc R . . H9B H 0.1470 -0.1106 0.4334 0.084 Uiso 1 1 calc R . . H9C H 0.1426 -0.2298 0.4696 0.084 Uiso 1 1 calc R . . C10 C 0.2491(3) -0.1761(5) 0.5581(2) 0.0511(14) Uani 1 1 d . . . H10A H 0.2642 -0.1338 0.5932 0.077 Uiso 1 1 calc R . . H10B H 0.3029 -0.2059 0.5425 0.077 Uiso 1 1 calc R . . H10C H 0.2102 -0.2430 0.5655 0.077 Uiso 1 1 calc R . . C11 C 0.4881(4) 0.1542(6) 0.5581(2) 0.0637(17) Uani 1 1 d . . . C12 C 0.5354(13) 0.281(2) 0.5477(10) 0.080(7) Uani 0.450(19) 1 d P A 1 H12A H 0.5428 0.2914 0.5076 0.121 Uiso 0.450(19) 1 calc PR A 1 H12B H 0.5931 0.2826 0.5681 0.121 Uiso 0.450(19) 1 calc PR A 1 H12C H 0.4988 0.3454 0.5611 0.121 Uiso 0.450(19) 1 calc PR A 1 C13 C 0.4704(13) 0.160(3) 0.6204(7) 0.116(13) Uani 0.450(19) 1 d P A 1 H13A H 0.4463 0.0839 0.6322 0.174 Uiso 0.450(19) 1 calc PR A 1 H13B H 0.4280 0.2236 0.6265 0.174 Uiso 0.450(19) 1 calc PR A 1 H13C H 0.5255 0.1764 0.6423 0.174 Uiso 0.450(19) 1 calc PR A 1 C14 C 0.5482(15) 0.068(3) 0.5454(14) 0.146(18) Uani 0.450(19) 1 d P A 1 H14A H 0.5630 0.0762 0.5063 0.218 Uiso 0.450(19) 1 calc PR A 1 H14B H 0.5227 -0.0111 0.5509 0.218 Uiso 0.450(19) 1 calc PR A 1 H14C H 0.6016 0.0766 0.5700 0.218 Uiso 0.450(19) 1 calc PR A 1 C12A C 0.5644(12) 0.124(2) 0.5154(7) 0.120(10) Uani 0.550(19) 1 d P A 2 H12D H 0.5524 0.0459 0.4980 0.180 Uiso 0.550(19) 1 calc PR A 2 H12E H 0.6217 0.1217 0.5362 0.180 Uiso 0.550(19) 1 calc PR A 2 H12F H 0.5648 0.1847 0.4862 0.180 Uiso 0.550(19) 1 calc PR A 2 C13A C 0.5019(8) 0.0419(15) 0.6021(5) 0.069(5) Uani 0.550(19) 1 d P A 2 H13D H 0.5040 -0.0326 0.5811 0.103 Uiso 0.550(19) 1 calc PR A 2 H13E H 0.4527 0.0393 0.6267 0.103 Uiso 0.550(19) 1 calc PR A 2 H13F H 0.5571 0.0524 0.6248 0.103 Uiso 0.550(19) 1 calc PR A 2 C14A C 0.4961(16) 0.266(2) 0.5841(14) 0.19(2) Uani 0.550(19) 1 d P A 2 H14D H 0.4481 0.2772 0.6091 0.280 Uiso 0.550(19) 1 calc PR A 2 H14E H 0.4931 0.3287 0.5555 0.280 Uiso 0.550(19) 1 calc PR A 2 H14F H 0.5526 0.2712 0.6058 0.280 Uiso 0.550(19) 1 calc PR A 2 C15 C 0.2587(3) 0.3072(4) 0.41405(17) 0.0351(11) Uani 1 1 d . . . H15 H 0.2985 0.3714 0.4108 0.042 Uiso 1 1 calc R . . C16 C 0.1633(2) 0.4167(3) 0.34506(16) 0.0288(9) Uani 1 1 d . . . H16 H 0.1713 0.3898 0.3058 0.035 Uiso 1 1 calc R . . C17 C 0.2180(3) 0.5306(4) 0.35493(19) 0.0376(11) Uani 1 1 d . . . H17A H 0.2808 0.5134 0.3499 0.045 Uiso 1 1 calc R . . H17B H 0.2125 0.5589 0.3937 0.045 Uiso 1 1 calc R . . C18 C 0.1849(3) 0.6297(4) 0.3124(2) 0.0435(11) Uani 1 1 d . . . H18A H 0.2179 0.7041 0.3204 0.052 Uiso 1 1 calc R . . H18B H 0.1958 0.6044 0.2738 0.052 Uiso 1 1 calc R . . C19 C 0.0850(3) 0.6525(4) 0.3171(2) 0.0429(11) Uani 1 1 d . . . H19A H 0.0648 0.7117 0.2886 0.051 Uiso 1 1 calc R . . H19B H 0.0754 0.6865 0.3544 0.051 Uiso 1 1 calc R . . C20 C 0.0290(3) 0.5374(4) 0.30887(19) 0.0374(11) Uani 1 1 d . . . H20A H -0.0333 0.5548 0.3154 0.045 Uiso 1 1 calc R . . H20B H 0.0320 0.5084 0.2700 0.045 Uiso 1 1 calc R . . C21 C 0.0641(2) 0.4411(3) 0.35017(16) 0.0293(9) Uani 1 1 d . . . H21 H 0.0576 0.4730 0.3887 0.035 Uiso 1 1 calc R . . C22 C -0.0625(3) 0.3119(4) 0.32621(16) 0.0273(10) Uani 1 1 d . . . H22 H -0.0863 0.3794 0.3069 0.033 Uiso 1 1 calc R . . C23 C -0.1187(3) 0.2086(4) 0.32976(16) 0.0263(10) Uani 1 1 d . . . C24 C -0.2066(3) 0.2156(4) 0.30373(17) 0.0301(11) Uani 1 1 d . . . H24 H -0.2220 0.2822 0.2808 0.036 Uiso 1 1 calc R . . C25 C -0.2698(3) 0.1280(4) 0.31108(17) 0.0292(10) Uani 1 1 d . . . C26 C -0.2425(3) 0.0315(4) 0.34606(16) 0.0290(10) Uani 1 1 d . . . H26 H -0.2849 -0.0282 0.3521 0.035 Uiso 1 1 calc R . . C27 C -0.1577(3) 0.0157(4) 0.37285(17) 0.0290(10) Uani 1 1 d . . . C28 C -0.0921(3) 0.1077(4) 0.36324(16) 0.0273(10) Uani 1 1 d . . . C29 C -0.1366(3) -0.0938(4) 0.41180(19) 0.0390(12) Uani 1 1 d . . . C30 C -0.2157(3) -0.1824(5) 0.4130(2) 0.0504(14) Uani 1 1 d . . . H30A H -0.2665 -0.1416 0.4275 0.076 Uiso 1 1 calc R . . H30B H -0.1992 -0.2499 0.4373 0.076 Uiso 1 1 calc R . . H30C H -0.2310 -0.2110 0.3750 0.076 Uiso 1 1 calc R . . C31 C -0.0586(3) -0.1664(4) 0.3894(2) 0.0551(14) Uani 1 1 d . . . H31A H -0.0744 -0.1933 0.3512 0.083 Uiso 1 1 calc R . . H31B H -0.0464 -0.2354 0.4136 0.083 Uiso 1 1 calc R . . H31C H -0.0062 -0.1159 0.3894 0.083 Uiso 1 1 calc R . . C32 C -0.1158(3) -0.0486(5) 0.47299(18) 0.0559(14) Uani 1 1 d . . . H32A H -0.1661 -0.0034 0.4854 0.084 Uiso 1 1 calc R . . H32B H -0.0638 0.0027 0.4740 0.084 Uiso 1 1 calc R . . H32C H -0.1046 -0.1167 0.4979 0.084 Uiso 1 1 calc R . . C33 C -0.3652(3) 0.1340(4) 0.28513(18) 0.0361(11) Uani 1 1 d . . . C34 C -0.3927(3) 0.0143(5) 0.2563(2) 0.0560(14) Uani 1 1 d . . . H34A H -0.4535 0.0201 0.2408 0.084 Uiso 1 1 calc R . . H34B H -0.3881 -0.0500 0.2840 0.084 Uiso 1 1 calc R . . H34C H -0.3538 -0.0024 0.2261 0.084 Uiso 1 1 calc R . . C35 C -0.4278(3) 0.1625(5) 0.3337(2) 0.0540(14) Uani 1 1 d . . . H35A H -0.4106 0.2384 0.3511 0.081 Uiso 1 1 calc R . . H35B H -0.4230 0.0992 0.3618 0.081 Uiso 1 1 calc R . . H35C H -0.4887 0.1677 0.3182 0.081 Uiso 1 1 calc R . . C36 C -0.3774(3) 0.2332(5) 0.2397(2) 0.0508(13) Uani 1 1 d . . . H36A H -0.3619 0.3104 0.2564 0.076 Uiso 1 1 calc R . . H36B H -0.4388 0.2346 0.2250 0.076 Uiso 1 1 calc R . . H36C H -0.3391 0.2166 0.2091 0.076 Uiso 1 1 calc R . . C38 C 0.1527(4) -0.0031(5) 0.3009(2) 0.0574(15) Uani 1 1 d . . . H38A H 0.1077 -0.0354 0.2734 0.069 Uiso 1 1 calc R . . H38B H 0.1493 -0.0490 0.3360 0.069 Uiso 1 1 calc R . . C39 C 0.2438(3) -0.0210(4) 0.2784(2) 0.0502(13) Uani 1 1 d . . . H39 H 0.2531 -0.1086 0.2743 0.060 Uiso 1 1 calc R . . C40 C 0.3177(4) 0.0261(7) 0.3184(3) 0.097(2) Uani 1 1 d . . . H40A H 0.3743 0.0148 0.3017 0.146 Uiso 1 1 calc R . . H40B H 0.3177 -0.0171 0.3539 0.146 Uiso 1 1 calc R . . H40C H 0.3084 0.1110 0.3251 0.146 Uiso 1 1 calc R . . C41 C 0.7784(3) 0.4901(4) 0.03797(16) 0.0262(10) Uani 1 1 d . . . C42 C 0.7460(3) 0.5799(4) -0.00175(16) 0.0273(10) Uani 1 1 d . . . C43 C 0.6618(3) 0.5615(4) -0.02794(17) 0.0328(11) Uani 1 1 d . . . H43 H 0.6398 0.6215 -0.0529 0.039 Uiso 1 1 calc R . . C44 C 0.6070(3) 0.4613(4) -0.02038(17) 0.0361(11) Uani 1 1 d . B . C45 C 0.6404(3) 0.3742(4) 0.01658(17) 0.0365(11) Uani 1 1 d . . . H45 H 0.6064 0.3051 0.0226 0.044 Uiso 1 1 calc R . . C46 C 0.7259(3) 0.3865(4) 0.04609(16) 0.0303(10) Uani 1 1 d . . . C47 C 0.8031(3) 0.6887(4) -0.01719(17) 0.0331(11) Uani 1 1 d . . . C48 C 0.8328(3) 0.7619(4) 0.03657(18) 0.0429(12) Uani 1 1 d . . . H48A H 0.8687 0.8296 0.0259 0.064 Uiso 1 1 calc R . . H48B H 0.8675 0.7109 0.0627 0.064 Uiso 1 1 calc R . . H48C H 0.7808 0.7909 0.0546 0.064 Uiso 1 1 calc R . . C49 C 0.8857(3) 0.6428(5) -0.04723(19) 0.0437(12) Uani 1 1 d . . . H49A H 0.9222 0.7106 -0.0569 0.066 Uiso 1 1 calc R . . H49B H 0.8663 0.5998 -0.0814 0.066 Uiso 1 1 calc R . . H49C H 0.9200 0.5894 -0.0221 0.066 Uiso 1 1 calc R . . C50 C 0.7532(3) 0.7760(5) -0.05811(18) 0.0452(13) Uani 1 1 d . . . H50A H 0.7918 0.8426 -0.0664 0.068 Uiso 1 1 calc R . . H50B H 0.7009 0.8062 -0.0409 0.068 Uiso 1 1 calc R . . H50C H 0.7355 0.7343 -0.0929 0.068 Uiso 1 1 calc R . . C51 C 0.5163(3) 0.4471(5) -0.0540(2) 0.0488(13) Uani 1 1 d . . . C52 C 0.4666(7) 0.3220(14) -0.0362(5) 0.080(5) Uani 0.573(17) 1 d P B 1 H52A H 0.5071 0.2549 -0.0393 0.121 Uiso 0.573(17) 1 calc PR B 1 H52B H 0.4143 0.3092 -0.0613 0.121 Uiso 0.573(17) 1 calc PR B 1 H52C H 0.4493 0.3282 0.0025 0.121 Uiso 0.573(17) 1 calc PR B 1 C53 C 0.4536(8) 0.5465(12) -0.0464(10) 0.141(12) Uani 0.573(17) 1 d P B 1 H53A H 0.3994 0.5323 -0.0695 0.211 Uiso 0.573(17) 1 calc PR B 1 H53B H 0.4803 0.6214 -0.0577 0.211 Uiso 0.573(17) 1 calc PR B 1 H53C H 0.4400 0.5514 -0.0069 0.211 Uiso 0.573(17) 1 calc PR B 1 C54 C 0.5369(8) 0.422(2) -0.1170(5) 0.116(9) Uani 0.573(17) 1 d P B 1 H54A H 0.5804 0.3585 -0.1184 0.173 Uiso 0.573(17) 1 calc PR B 1 H54B H 0.5602 0.4948 -0.1334 0.173 Uiso 0.573(17) 1 calc PR B 1 H54C H 0.4827 0.3986 -0.1382 0.173 Uiso 0.573(17) 1 calc PR B 1 C52A C 0.5188(14) 0.3380(17) -0.0895(11) 0.111(12) Uani 0.427(17) 1 d P B 2 H52D H 0.4629 0.3300 -0.1116 0.166 Uiso 0.427(17) 1 calc PR B 2 H52E H 0.5280 0.2681 -0.0654 0.166 Uiso 0.427(17) 1 calc PR B 2 H52F H 0.5670 0.3445 -0.1146 0.166 Uiso 0.427(17) 1 calc PR B 2 C53A C 0.4424(9) 0.455(3) -0.0111(8) 0.116(12) Uani 0.427(17) 1 d P B 2 H53D H 0.3846 0.4489 -0.0313 0.174 Uiso 0.427(17) 1 calc PR B 2 H53E H 0.4469 0.5307 0.0088 0.174 Uiso 0.427(17) 1 calc PR B 2 H53F H 0.4494 0.3892 0.0158 0.174 Uiso 0.427(17) 1 calc PR B 2 C54A C 0.4941(9) 0.5637(16) -0.0939(6) 0.063(5) Uani 0.427(17) 1 d P B 2 H54D H 0.4373 0.5522 -0.1146 0.095 Uiso 0.427(17) 1 calc PR B 2 H54E H 0.5403 0.5733 -0.1204 0.095 Uiso 0.427(17) 1 calc PR B 2 H54F H 0.4917 0.6349 -0.0704 0.095 Uiso 0.427(17) 1 calc PR B 2 C55 C 0.7619(3) 0.2824(4) 0.07492(16) 0.0309(10) Uani 1 1 d . . . H55 H 0.7267 0.2127 0.0737 0.037 Uiso 1 1 calc R . . C56 C 0.8729(2) 0.1566(3) 0.12434(15) 0.0264(9) Uani 1 1 d . . . H56 H 0.9170 0.1278 0.0981 0.032 Uiso 1 1 calc R . . C57 C 0.8060(3) 0.0551(4) 0.13105(17) 0.0322(10) Uani 1 1 d . . . H57A H 0.7782 0.0340 0.0939 0.039 Uiso 1 1 calc R . . H57B H 0.7592 0.0824 0.1550 0.039 Uiso 1 1 calc R . . C58 C 0.8518(3) -0.0561(3) 0.15772(17) 0.0357(10) Uani 1 1 d . . . H58A H 0.8068 -0.1173 0.1643 0.043 Uiso 1 1 calc R . . H58B H 0.8928 -0.0894 0.1312 0.043 Uiso 1 1 calc R . . C59 C 0.9032(3) -0.0272(3) 0.21383(17) 0.0348(10) Uani 1 1 d . . . H59A H 0.9341 -0.0994 0.2281 0.042 Uiso 1 1 calc R . . H59B H 0.8615 -0.0023 0.2418 0.042 Uiso 1 1 calc R . . C60 C 0.9711(3) 0.0734(4) 0.20617(17) 0.0305(10) Uani 1 1 d . . . H60A H 1.0160 0.0461 0.1808 0.037 Uiso 1 1 calc R . . H60B H 1.0012 0.0932 0.2428 0.037 Uiso 1 1 calc R . . C61 C 0.9239(2) 0.1859(3) 0.18117(15) 0.0265(9) Uani 1 1 d . . . H61 H 0.8799 0.2121 0.2080 0.032 Uiso 1 1 calc R . . C62 C 1.0636(3) 0.2957(4) 0.18563(15) 0.0243(10) Uani 1 1 d . . . H62 H 1.0868 0.2300 0.2066 0.029 Uiso 1 1 calc R . . C63 C 1.1240(3) 0.3932(4) 0.17473(15) 0.0236(9) Uani 1 1 d . . . C64 C 1.2138(3) 0.3820(4) 0.19630(16) 0.0269(10) Uani 1 1 d . . . H64 H 1.2305 0.3138 0.2177 0.032 Uiso 1 1 calc R . . C65 C 1.2775(3) 0.4688(4) 0.18669(17) 0.0310(10) Uani 1 1 d . . . C66 C 1.2466(3) 0.5700(4) 0.15408(16) 0.0309(11) Uani 1 1 d . . . H66 H 1.2880 0.6307 0.1475 0.037 Uiso 1 1 calc R . . C67 C 1.1601(3) 0.5861(4) 0.13117(16) 0.0261(10) Uani 1 1 d . . . C68 C 1.0973(3) 0.4946(4) 0.14114(17) 0.0251(10) Uani 1 1 d . . . C69 C 1.1338(3) 0.7003(4) 0.09714(18) 0.0343(11) Uani 1 1 d . . . C70 C 1.0606(3) 0.7683(4) 0.1277(2) 0.0537(14) Uani 1 1 d . . . H70A H 1.0101 0.7155 0.1317 0.081 Uiso 1 1 calc R . . H70B H 1.0419 0.8383 0.1057 0.081 Uiso 1 1 calc R . . H70C H 1.0840 0.7934 0.1649 0.081 Uiso 1 1 calc R . . C71 C 1.1013(3) 0.6661(5) 0.03666(19) 0.0501(13) Uani 1 1 d . . . H71A H 1.0520 0.6103 0.0379 0.075 Uiso 1 1 calc R . . H71B H 1.1494 0.6285 0.0177 0.075 Uiso 1 1 calc R . . H71C H 1.0820 0.7377 0.0161 0.075 Uiso 1 1 calc R . . C72 C 1.2135(3) 0.7879(4) 0.0930(2) 0.0485(13) Uani 1 1 d . . . H72A H 1.2366 0.8094 0.1308 0.073 Uiso 1 1 calc R . . H72B H 1.1938 0.8598 0.0729 0.073 Uiso 1 1 calc R . . H72C H 1.2599 0.7492 0.0729 0.073 Uiso 1 1 calc R . . C73 C 1.3757(3) 0.4611(4) 0.20787(18) 0.0371(11) Uani 1 1 d . . . C74 C 1.3898(3) 0.3597(5) 0.2532(2) 0.0502(14) Uani 1 1 d . . . H74A H 1.4520 0.3564 0.2661 0.075 Uiso 1 1 calc R . . H74B H 1.3720 0.2831 0.2365 0.075 Uiso 1 1 calc R . . H74C H 1.3540 0.3765 0.2849 0.075 Uiso 1 1 calc R . . C75 C 1.4073(3) 0.5822(4) 0.2365(2) 0.0512(13) Uani 1 1 d . . . H75A H 1.4693 0.5754 0.2496 0.077 Uiso 1 1 calc R . . H75B H 1.3717 0.5989 0.2684 0.077 Uiso 1 1 calc R . . H75C H 1.4005 0.6470 0.2093 0.077 Uiso 1 1 calc R . . C76 C 1.4328(3) 0.4351(6) 0.1577(2) 0.0616(16) Uani 1 1 d . . . H76A H 1.4948 0.4302 0.1710 0.092 Uiso 1 1 calc R . . H76B H 1.4252 0.4991 0.1301 0.092 Uiso 1 1 calc R . . H76C H 1.4145 0.3595 0.1404 0.092 Uiso 1 1 calc R . . C78 C 0.8139(3) 0.5883(4) 0.1901(2) 0.0500(13) Uani 1 1 d . . . H78A H 0.8040 0.6220 0.1520 0.060 Uiso 1 1 calc R . . H78B H 0.8533 0.6431 0.2121 0.060 Uiso 1 1 calc R . . C79 C 0.7264(3) 0.5811(5) 0.2173(2) 0.0566(14) Uani 1 1 d . . . H79 H 0.6924 0.5135 0.1995 0.068 Uiso 1 1 calc R . . C80 C 0.6681(4) 0.6953(5) 0.2103(3) 0.112(3) Uani 1 1 d . . . H80A H 0.6124 0.6825 0.2278 0.168 Uiso 1 1 calc R . . H80B H 0.6565 0.7121 0.1703 0.168 Uiso 1 1 calc R . . H80C H 0.6991 0.7627 0.2282 0.168 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 0.0255(7) 0.0288(8) 0.0271(7) 0.0018(6) -0.0021(6) 0.0007(6) Al2 0.0229(7) 0.0245(7) 0.0239(6) 0.0013(5) -0.0024(5) -0.0004(5) Cl1 0.0956(11) 0.0561(8) 0.0540(8) 0.0031(7) 0.0307(8) 0.0077(8) Cl2 0.1192(14) 0.0662(10) 0.0700(10) 0.0032(8) 0.0410(10) 0.0208(10) N1 0.028(2) 0.033(2) 0.0281(18) -0.0007(16) -0.0033(16) -0.0009(16) N2 0.029(2) 0.0258(19) 0.0284(18) -0.0007(15) -0.0001(16) -0.0026(15) N3 0.028(2) 0.0244(18) 0.0239(17) 0.0016(14) -0.0018(15) 0.0018(15) N4 0.029(2) 0.0213(18) 0.0202(17) 0.0015(14) -0.0028(15) 0.0002(14) O1 0.0266(17) 0.0388(19) 0.0310(15) 0.0076(14) -0.0051(14) -0.0040(14) O2 0.0210(16) 0.0336(17) 0.0358(16) 0.0110(14) -0.0029(13) 0.0033(13) O3 0.0402(18) 0.0240(17) 0.0310(15) -0.0011(13) 0.0018(13) 0.0053(13) O4 0.0260(16) 0.0307(17) 0.0296(15) 0.0051(13) -0.0044(13) -0.0027(13) O5 0.0292(17) 0.0308(17) 0.0356(16) 0.0085(13) -0.0072(13) -0.0063(14) O6 0.0404(18) 0.0305(18) 0.0322(16) 0.0022(13) 0.0065(14) 0.0094(14) C1 0.029(3) 0.045(3) 0.021(2) 0.000(2) -0.003(2) 0.009(2) C2 0.030(3) 0.043(3) 0.026(2) 0.004(2) 0.003(2) 0.008(2) C3 0.035(3) 0.057(3) 0.029(2) 0.006(2) -0.002(2) 0.016(3) C4 0.026(3) 0.064(3) 0.041(3) 0.005(3) -0.004(2) -0.002(3) C5 0.030(3) 0.055(3) 0.045(3) 0.002(3) -0.005(2) -0.001(2) C6 0.027(3) 0.040(3) 0.029(2) 0.002(2) -0.004(2) -0.004(2) C7 0.033(3) 0.052(3) 0.032(2) 0.014(2) 0.002(2) 0.008(2) C8 0.040(3) 0.060(3) 0.052(3) 0.023(3) 0.010(2) 0.003(3) C9 0.081(4) 0.040(3) 0.046(3) 0.011(2) -0.015(3) -0.008(3) C10 0.043(3) 0.060(3) 0.050(3) 0.025(3) 0.002(2) 0.014(3) C11 0.035(3) 0.088(5) 0.065(4) 0.020(3) -0.025(3) -0.003(3) C12 0.039(10) 0.079(13) 0.121(15) 0.003(12) -0.016(9) -0.013(10) C13 0.100(15) 0.18(3) 0.062(11) 0.045(15) -0.046(10) -0.076(19) C14 0.053(17) 0.14(2) 0.23(4) -0.07(3) -0.09(2) 0.040(16) C12A 0.029(7) 0.24(3) 0.090(10) 0.071(13) -0.010(7) -0.002(11) C13A 0.055(8) 0.096(11) 0.051(7) 0.016(7) -0.029(6) -0.003(7) C14A 0.12(2) 0.11(2) 0.31(5) -0.13(3) -0.17(3) 0.063(17) C15 0.026(3) 0.041(3) 0.038(2) -0.003(2) 0.001(2) -0.011(2) C16 0.035(2) 0.026(2) 0.025(2) 0.0020(17) 0.0002(18) -0.0039(18) C17 0.034(2) 0.029(2) 0.049(3) 0.003(2) -0.001(2) -0.007(2) C18 0.045(3) 0.029(2) 0.057(3) 0.006(2) 0.008(2) -0.005(2) C19 0.049(3) 0.032(2) 0.048(3) 0.005(2) 0.005(2) 0.000(2) C20 0.039(3) 0.029(2) 0.044(3) 0.006(2) -0.002(2) -0.004(2) C21 0.031(2) 0.027(2) 0.030(2) 0.0000(18) 0.0021(19) 0.0004(18) C22 0.024(3) 0.029(2) 0.028(2) 0.0014(18) -0.0009(18) 0.004(2) C23 0.027(2) 0.030(2) 0.022(2) -0.0025(19) -0.0015(18) 0.004(2) C24 0.033(3) 0.030(2) 0.026(2) 0.0026(19) -0.002(2) 0.009(2) C25 0.023(2) 0.035(3) 0.029(2) -0.001(2) -0.0024(19) 0.005(2) C26 0.023(2) 0.036(3) 0.029(2) 0.001(2) -0.0002(19) -0.008(2) C27 0.031(3) 0.030(3) 0.026(2) -0.0016(19) 0.005(2) -0.004(2) C28 0.024(2) 0.033(3) 0.024(2) -0.001(2) -0.0038(19) 0.001(2) C29 0.035(3) 0.037(3) 0.046(3) 0.014(2) 0.001(2) -0.003(2) C30 0.039(3) 0.053(3) 0.058(3) 0.019(3) 0.000(2) -0.010(3) C31 0.045(3) 0.042(3) 0.080(4) 0.025(3) 0.009(3) 0.010(2) C32 0.058(3) 0.072(4) 0.036(3) 0.014(3) -0.006(2) -0.018(3) C33 0.024(2) 0.042(3) 0.041(3) -0.004(2) -0.004(2) -0.002(2) C34 0.044(3) 0.061(4) 0.061(3) 0.003(3) -0.017(3) -0.006(3) C35 0.031(3) 0.078(4) 0.053(3) 0.005(3) -0.001(2) 0.006(3) C36 0.038(3) 0.057(3) 0.056(3) 0.003(3) -0.007(2) 0.012(2) C38 0.073(4) 0.051(3) 0.048(3) 0.006(2) 0.005(3) 0.010(3) C39 0.051(3) 0.044(3) 0.057(3) 0.003(2) 0.008(3) 0.007(2) C40 0.063(4) 0.118(5) 0.108(5) 0.006(4) -0.006(4) -0.014(4) C41 0.019(2) 0.034(3) 0.025(2) -0.004(2) -0.0041(18) -0.0038(19) C42 0.025(2) 0.034(3) 0.022(2) -0.001(2) -0.0007(19) 0.007(2) C43 0.032(3) 0.037(3) 0.029(2) 0.006(2) -0.001(2) 0.004(2) C44 0.026(2) 0.051(3) 0.030(2) -0.001(2) -0.006(2) 0.008(2) C45 0.027(3) 0.044(3) 0.038(3) -0.001(2) 0.002(2) -0.007(2) C46 0.025(2) 0.039(3) 0.026(2) 0.001(2) -0.0053(19) 0.002(2) C47 0.038(3) 0.032(3) 0.029(2) 0.005(2) -0.003(2) 0.003(2) C48 0.057(3) 0.033(3) 0.038(3) 0.002(2) -0.003(2) -0.002(2) C49 0.030(3) 0.062(3) 0.039(3) 0.003(2) 0.000(2) -0.001(2) C50 0.044(3) 0.050(3) 0.041(3) 0.013(2) -0.001(2) 0.001(3) C51 0.031(3) 0.057(3) 0.056(3) 0.005(3) -0.018(2) 0.000(3) C52 0.033(6) 0.117(12) 0.087(9) 0.045(8) -0.039(6) -0.039(7) C53 0.044(9) 0.060(8) 0.31(4) -0.009(14) -0.041(15) 0.015(7) C54 0.069(8) 0.22(3) 0.055(8) 0.017(11) -0.040(6) -0.059(14) C52A 0.090(17) 0.084(13) 0.15(3) -0.013(14) -0.09(2) -0.007(12) C53A 0.027(8) 0.19(3) 0.123(15) 0.084(17) -0.032(9) -0.039(12) C54A 0.013(7) 0.121(14) 0.054(9) 0.028(9) -0.017(6) 0.007(8) C55 0.029(3) 0.032(2) 0.032(2) -0.0003(19) 0.001(2) -0.004(2) C56 0.025(2) 0.027(2) 0.027(2) 0.0005(17) -0.0006(17) 0.0029(18) C57 0.030(2) 0.031(2) 0.035(2) -0.0032(19) -0.0010(19) -0.0048(19) C58 0.035(2) 0.026(2) 0.046(3) 0.000(2) -0.001(2) -0.0057(19) C59 0.045(3) 0.027(2) 0.033(2) 0.0076(19) 0.002(2) -0.0005(19) C60 0.034(2) 0.026(2) 0.031(2) 0.0022(18) -0.0014(19) 0.0024(19) C61 0.028(2) 0.029(2) 0.023(2) 0.0026(18) 0.0030(17) -0.0057(18) C62 0.030(3) 0.024(2) 0.018(2) 0.0002(17) -0.0032(18) 0.0047(19) C63 0.024(2) 0.025(2) 0.022(2) -0.0009(19) -0.0011(18) -0.0016(19) C64 0.029(3) 0.027(2) 0.024(2) 0.0000(18) -0.0027(19) 0.004(2) C65 0.030(2) 0.031(2) 0.032(2) -0.003(2) -0.001(2) -0.004(2) C66 0.030(3) 0.031(3) 0.032(2) 0.000(2) 0.005(2) -0.005(2) C67 0.028(2) 0.026(2) 0.025(2) -0.0026(19) -0.0010(19) 0.001(2) C68 0.018(2) 0.029(2) 0.028(2) -0.0047(19) -0.0003(19) 0.0027(19) C69 0.029(3) 0.031(3) 0.042(3) 0.010(2) -0.003(2) -0.005(2) C70 0.042(3) 0.036(3) 0.083(4) 0.013(3) 0.006(3) 0.005(2) C71 0.052(3) 0.057(3) 0.040(3) 0.023(2) -0.009(2) -0.010(3) C72 0.052(3) 0.038(3) 0.055(3) 0.017(2) -0.004(2) -0.009(2) C73 0.025(2) 0.044(3) 0.041(3) 0.005(2) -0.008(2) 0.004(2) C74 0.027(3) 0.059(3) 0.064(3) 0.005(3) -0.012(2) 0.002(2) C75 0.034(3) 0.055(3) 0.063(3) -0.005(3) -0.012(2) -0.011(2) C76 0.031(3) 0.096(5) 0.058(3) 0.006(3) 0.000(2) 0.007(3) C78 0.070(4) 0.037(3) 0.045(3) 0.008(2) 0.013(3) 0.013(3) C79 0.052(3) 0.048(3) 0.072(3) 0.008(3) 0.019(3) 0.010(3) C80 0.092(5) 0.055(3) 0.201(7) 0.054(4) 0.098(5) 0.058(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 O3 1.746(3) . ? Al1 O1 1.797(3) . ? Al1 O2 1.804(3) . ? Al1 N2 1.999(3) . ? Al1 N1 2.021(3) . ? Al2 O6 1.746(3) . ? Al2 O5 1.795(3) . ? Al2 O4 1.817(3) . ? Al2 N3 1.997(3) . ? Al2 N4 2.004(3) . ? Cl1 C39 1.809(5) . ? Cl2 C79 1.813(5) . ? N1 C15 1.289(5) . ? N1 C16 1.477(5) . ? N2 C22 1.295(5) . ? N2 C21 1.495(5) . ? N3 C55 1.295(5) . ? N3 C56 1.485(5) . ? N4 C62 1.280(5) . ? N4 C61 1.479(5) . ? O1 C1 1.330(5) . ? O2 C28 1.329(4) . ? O3 C38 1.377(6) . ? O4 C41 1.327(4) . ? O5 C68 1.332(4) . ? O6 C78 1.395(5) . ? C1 C6 1.415(6) . ? C1 C2 1.425(6) . ? C2 C3 1.389(6) . ? C2 C7 1.545(7) . ? C3 C4 1.400(7) . ? C4 C5 1.372(7) . ? C4 C11 1.533(6) . ? C5 C6 1.390(6) . ? C6 C15 1.426(6) . ? C7 C9 1.521(6) . ? C7 C8 1.534(6) . ? C7 C10 1.537(6) . ? C11 C14 1.35(2) . ? C11 C14A 1.380(18) . ? C11 C13 1.50(2) . ? C11 C12 1.59(2) . ? C11 C12A 1.60(2) . ? C11 C13A 1.617(14) . ? C16 C17 1.508(5) . ? C16 C21 1.516(5) . ? C17 C18 1.540(6) . ? C18 C19 1.522(6) . ? C19 C20 1.526(6) . ? C20 C21 1.510(5) . ? C22 C23 1.420(6) . ? C23 C28 1.405(6) . ? C23 C24 1.416(5) . ? C24 C25 1.367(6) . ? C25 C26 1.390(6) . ? C25 C33 1.516(5) . ? C26 C27 1.389(5) . ? C27 C28 1.436(6) . ? C27 C29 1.535(6) . ? C29 C31 1.531(6) . ? C29 C32 1.533(6) . ? C29 C30 1.533(6) . ? C33 C34 1.527(7) . ? C33 C36 1.530(6) . ? C33 C35 1.546(6) . ? C38 C39 1.501(7) . ? C39 C40 1.497(7) . ? C41 C46 1.404(6) . ? C41 C42 1.424(6) . ? C42 C43 1.380(5) . ? C42 C47 1.527(6) . ? C43 C44 1.392(6) . ? C44 C45 1.368(6) . ? C44 C51 1.533(6) . ? C45 C46 1.422(5) . ? C46 C55 1.421(6) . ? C47 C50 1.521(6) . ? C47 C48 1.539(6) . ? C47 C49 1.541(6) . ? C51 C53 1.459(14) . ? C51 C52A 1.463(19) . ? C51 C53A 1.54(2) . ? C51 C54 1.550(14) . ? C51 C54A 1.612(15) . ? C51 C52 1.631(13) . ? C56 C57 1.513(5) . ? C56 C61 1.529(5) . ? C57 C58 1.519(6) . ? C58 C59 1.517(5) . ? C59 C60 1.519(6) . ? C60 C61 1.526(5) . ? C62 C63 1.435(6) . ? C63 C64 1.409(5) . ? C63 C68 1.410(6) . ? C64 C65 1.378(6) . ? C65 C66 1.413(6) . ? C65 C73 1.521(5) . ? C66 C67 1.379(5) . ? C67 C68 1.407(5) . ? C67 C69 1.529(6) . ? C69 C71 1.519(6) . ? C69 C70 1.537(6) . ? C69 C72 1.539(6) . ? C73 C76 1.519(6) . ? C73 C74 1.548(6) . ? C73 C75 1.554(6) . ? C78 C79 1.490(7) . ? C79 C80 1.533(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 O3 Al1 O1 109.73(14) . . ? O3 Al1 O2 107.17(14) . . ? O1 Al1 O2 89.80(13) . . ? O3 Al1 N2 104.33(14) . . ? O1 Al1 N2 144.87(15) . . ? O2 Al1 N2 88.20(14) . . ? O3 Al1 N1 96.55(14) . . ? O1 Al1 N1 88.85(13) . . ? O2 Al1 N1 155.22(14) . . ? N2 Al1 N1 78.88(14) . . ? O6 Al2 O5 111.60(15) . . ? O6 Al2 O4 106.75(14) . . ? O5 Al2 O4 90.25(13) . . ? O6 Al2 N3 103.73(14) . . ? O5 Al2 N3 143.62(15) . . ? O4 Al2 N3 87.68(13) . . ? O6 Al2 N4 96.09(13) . . ? O5 Al2 N4 88.68(13) . . ? O4 Al2 N4 155.79(13) . . ? N3 Al2 N4 79.03(13) . . ? C15 N1 C16 121.3(3) . . ? C15 N1 Al1 125.1(3) . . ? C16 N1 Al1 113.1(2) . . ? C22 N2 C21 119.0(3) . . ? C22 N2 Al1 124.0(3) . . ? C21 N2 Al1 116.9(2) . . ? C55 N3 C56 119.6(3) . . ? C55 N3 Al2 122.7(3) . . ? C56 N3 Al2 117.3(2) . . ? C62 N4 C61 121.4(3) . . ? C62 N4 Al2 126.5(3) . . ? C61 N4 Al2 112.0(2) . . ? C1 O1 Al1 134.3(3) . . ? C28 O2 Al1 131.9(2) . . ? C38 O3 Al1 127.3(3) . . ? C41 O4 Al2 132.0(2) . . ? C68 O5 Al2 135.8(2) . . ? C78 O6 Al2 125.6(3) . . ? O1 C1 C6 121.4(4) . . ? O1 C1 C2 120.4(4) . . ? C6 C1 C2 118.2(4) . . ? C3 C2 C1 117.3(4) . . ? C3 C2 C7 121.1(4) . . ? C1 C2 C7 121.5(4) . . ? C2 C3 C4 125.2(4) . . ? C5 C4 C3 115.8(4) . . ? C5 C4 C11 122.8(5) . . ? C3 C4 C11 121.4(4) . . ? C4 C5 C6 122.5(5) . . ? C5 C6 C1 120.8(4) . . ? C5 C6 C15 117.9(4) . . ? C1 C6 C15 121.2(4) . . ? C9 C7 C8 110.9(4) . . ? C9 C7 C10 106.8(4) . . ? C8 C7 C10 107.8(4) . . ? C9 C7 C2 110.2(3) . . ? C8 C7 C2 108.9(4) . . ? C10 C7 C2 112.3(4) . . ? C14 C11 C14A 133.4(13) . . ? C14 C11 C13 113.6(15) . . ? C14A C11 C13 63.1(14) . . ? C14 C11 C4 111.9(10) . . ? C14A C11 C4 112.4(8) . . ? C13 C11 C4 109.4(8) . . ? C14 C11 C12 106.2(15) . . ? C14A C11 C12 41.7(15) . . ? C13 C11 C12 102.5(12) . . ? C4 C11 C12 112.8(9) . . ? C14 C11 C12A 37.5(16) . . ? C14A C11 C12A 114.9(16) . . ? C13 C11 C12A 142.5(11) . . ? C4 C11 C12A 105.5(8) . . ? C12 C11 C12A 75.6(11) . . ? C14 C11 C13A 62.7(15) . . ? C14A C11 C13A 113.5(13) . . ? C13 C11 C13A 55.6(11) . . ? C4 C11 C13A 109.8(6) . . ? C12 C11 C13A 136.8(10) . . ? C12A C11 C13A 99.8(10) . . ? N1 C15 C6 126.2(4) . . ? N1 C16 C17 117.4(3) . . ? N1 C16 C21 105.2(3) . . ? C17 C16 C21 111.2(3) . . ? C16 C17 C18 109.9(3) . . ? C19 C18 C17 110.4(4) . . ? C18 C19 C20 112.6(3) . . ? C21 C20 C19 109.7(3) . . ? N2 C21 C20 117.8(3) . . ? N2 C21 C16 106.0(3) . . ? C20 C21 C16 112.2(3) . . ? N2 C22 C23 125.3(4) . . ? C28 C23 C24 120.5(4) . . ? C28 C23 C22 121.3(3) . . ? C24 C23 C22 117.8(4) . . ? C25 C24 C23 122.4(4) . . ? C24 C25 C26 115.7(4) . . ? C24 C25 C33 123.9(4) . . ? C26 C25 C33 120.4(4) . . ? C27 C26 C25 126.2(4) . . ? C26 C27 C28 116.8(4) . . ? C26 C27 C29 121.1(4) . . ? C28 C27 C29 122.0(3) . . ? O2 C28 C23 121.3(4) . . ? O2 C28 C27 120.4(4) . . ? C23 C28 C27 118.3(4) . . ? C31 C29 C32 112.0(4) . . ? C31 C29 C30 106.0(4) . . ? C32 C29 C30 107.7(4) . . ? C31 C29 C27 109.9(4) . . ? C32 C29 C27 108.9(4) . . ? C30 C29 C27 112.4(4) . . ? C25 C33 C34 111.2(4) . . ? C25 C33 C36 112.4(4) . . ? C34 C33 C36 106.9(3) . . ? C25 C33 C35 107.9(3) . . ? C34 C33 C35 110.1(4) . . ? C36 C33 C35 108.4(4) . . ? O3 C38 C39 113.6(4) . . ? C40 C39 C38 112.6(5) . . ? C40 C39 Cl1 111.5(4) . . ? C38 C39 Cl1 110.2(3) . . ? O4 C41 C46 119.8(4) . . ? O4 C41 C42 121.2(4) . . ? C46 C41 C42 118.9(3) . . ? C43 C42 C41 117.0(4) . . ? C43 C42 C47 121.1(4) . . ? C41 C42 C47 121.9(3) . . ? C42 C43 C44 125.9(4) . . ? C45 C44 C43 116.3(4) . . ? C45 C44 C51 122.1(4) . . ? C43 C44 C51 121.6(4) . . ? C44 C45 C46 121.6(4) . . ? C41 C46 C55 121.6(4) . . ? C41 C46 C45 120.3(4) . . ? C55 C46 C45 117.2(4) . . ? C50 C47 C42 112.8(4) . . ? C50 C47 C48 106.9(4) . . ? C42 C47 C48 110.8(3) . . ? C50 C47 C49 107.1(4) . . ? C42 C47 C49 108.9(4) . . ? C48 C47 C49 110.3(4) . . ? C53 C51 C52A 136.4(9) . . ? C53 C51 C44 114.4(7) . . ? C52A C51 C44 109.0(7) . . ? C53 C51 C53A 52.4(11) . . ? C52A C51 C53A 117.3(14) . . ? C44 C51 C53A 107.7(7) . . ? C53 C51 C54 114.4(11) . . ? C52A C51 C54 45.7(10) . . ? C44 C51 C54 106.8(6) . . ? C53A C51 C54 145.3(8) . . ? C53 C51 C54A 50.3(9) . . ? C52A C51 C54A 109.6(10) . . ? C44 C51 C54A 111.1(6) . . ? C53A C51 C54A 101.8(11) . . ? C54 C51 C54A 68.4(9) . . ? C53 C51 C52 107.4(8) . . ? C52A C51 C52 58.5(11) . . ? C44 C51 C52 110.9(5) . . ? C53A C51 C52 61.6(10) . . ? C54 C51 C52 102.3(10) . . ? C54A C51 C52 137.9(6) . . ? N3 C55 C46 125.8(4) . . ? N3 C56 C57 118.6(3) . . ? N3 C56 C61 104.4(3) . . ? C57 C56 C61 111.3(3) . . ? C56 C57 C58 110.8(3) . . ? C59 C58 C57 112.3(3) . . ? C58 C59 C60 110.9(3) . . ? C59 C60 C61 110.1(3) . . ? N4 C61 C60 117.4(3) . . ? N4 C61 C56 104.9(3) . . ? C60 C61 C56 110.9(3) . . ? N4 C62 C63 125.3(4) . . ? C64 C63 C68 120.1(4) . . ? C64 C63 C62 117.6(3) . . ? C68 C63 C62 122.2(3) . . ? C65 C64 C63 122.1(4) . . ? C64 C65 C66 115.5(4) . . ? C64 C65 C73 124.7(4) . . ? C66 C65 C73 119.9(4) . . ? C67 C66 C65 125.5(4) . . ? C66 C67 C68 117.4(4) . . ? C66 C67 C69 121.0(4) . . ? C68 C67 C69 121.6(3) . . ? O5 C68 C67 120.6(3) . . ? O5 C68 C63 119.9(3) . . ? C67 C68 C63 119.5(3) . . ? C71 C69 C67 109.9(4) . . ? C71 C69 C70 111.1(4) . . ? C67 C69 C70 109.0(4) . . ? C71 C69 C72 107.6(4) . . ? C67 C69 C72 111.9(3) . . ? C70 C69 C72 107.3(4) . . ? C76 C73 C65 109.3(3) . . ? C76 C73 C74 109.5(4) . . ? C65 C73 C74 110.7(4) . . ? C76 C73 C75 109.1(4) . . ? C65 C73 C75 110.8(4) . . ? C74 C73 C75 107.4(3) . . ? O6 C78 C79 113.1(4) . . ? C78 C79 C80 114.6(4) . . ? C78 C79 Cl2 109.7(4) . . ? C80 C79 Cl2 109.5(4) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 22.99 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.412 _refine_diff_density_min -0.506 _refine_diff_density_rms 0.047 # END OF CIF # END OF CIF data_chis1278 _database_code_depnum_ccdc_archive 'CCDC 246786' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C39 H58 Al Cl N2 O3' _chemical_formula_sum 'C39 H58 Al Cl N2 O3' _chemical_formula_weight 665.30 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 14.927(1) _cell_length_b 10.941(1) _cell_length_c 23.393(3) _cell_angle_alpha 90.00 _cell_angle_beta 93.69(1) _cell_angle_gamma 90.00 _cell_volume 3812.5(7) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Chunk _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.31 _exptl_crystal_size_min 0.27 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.159 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1440 _exptl_absorpt_coefficient_mu 0.160 _exptl_absorpt_correction_type None _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 60079 _diffrn_reflns_av_R_equivalents 0.058 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.57 _diffrn_reflns_theta_max 25.03 _reflns_number_total 13387 _reflns_number_gt 10157 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _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^)+(0.0769P)^2^+1.9066P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00(8) _refine_ls_number_reflns 13387 _refine_ls_number_parameters 826 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0852 _refine_ls_R_factor_gt 0.0555 _refine_ls_wR_factor_ref 0.1467 _refine_ls_wR_factor_gt 0.1321 _refine_ls_goodness_of_fit_ref 1.020 _refine_ls_restrained_S_all 1.020 _refine_ls_shift/su_max 0.196 _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 0.09114(7) 0.00437(10) 0.87428(4) 0.0215(3) Uani 1 1 d . . . Al2 Al 0.91065(7) 0.75827(10) 0.62715(4) 0.0190(2) Uani 1 1 d . . . Cl1 Cl 0.25225(9) 0.12374(11) 0.70612(5) 0.0560(3) Uani 1 1 d . . . Cl2 Cl 0.74529(9) 0.62427(11) 0.79001(5) 0.0535(3) Uani 1 1 d . . . N1 N 0.18301(19) -0.1307(3) 0.88335(11) 0.0232(7) Uani 1 1 d . . . N2 N 0.01788(19) -0.1397(3) 0.84732(12) 0.0221(7) Uani 1 1 d . . . N3 N 0.98163(18) 0.8899(3) 0.66881(11) 0.0195(7) Uani 1 1 d . . . N4 N 0.83850(19) 0.9070(3) 0.60335(11) 0.0210(7) Uani 1 1 d . . . O1 O 0.12919(16) 0.0655(2) 0.81089(10) 0.0265(6) Uani 1 1 d . . . O2 O 0.14720(16) 0.0793(2) 0.93493(10) 0.0262(6) Uani 1 1 d . . . O3 O -0.01161(16) 0.0826(2) 0.88847(10) 0.0258(6) Uani 1 1 d . . . O4 O 0.85617(17) 0.7035(2) 0.68594(10) 0.0270(6) Uani 1 1 d . . . O5 O 1.01365(15) 0.6768(2) 0.61902(10) 0.0247(6) Uani 1 1 d . . . O6 O 0.86006(16) 0.6804(2) 0.56435(10) 0.0236(6) Uani 1 1 d . . . C1 C 0.1797(3) 0.1722(4) 0.80760(18) 0.0391(11) Uani 1 1 d . . . H1A H 0.1899 0.2064 0.8457 0.047 Uiso 1 1 calc R . . H1B H 0.1457 0.2314 0.7842 0.047 Uiso 1 1 calc R . . C2 C 0.2697(3) 0.1512(4) 0.78235(19) 0.0440(11) Uani 1 1 d . . . H2 H 0.2970 0.0779 0.8002 0.053 Uiso 1 1 calc R . . C3 C 0.3353(3) 0.2563(5) 0.7915(2) 0.0653(15) Uani 1 1 d . . . H3A H 0.3908 0.2359 0.7754 0.098 Uiso 1 1 calc R . . H3B H 0.3460 0.2712 0.8318 0.098 Uiso 1 1 calc R . . H3C H 0.3105 0.3284 0.7733 0.098 Uiso 1 1 calc R . . C4 C 0.2580(2) -0.1251(4) 0.91286(15) 0.0304(9) Uani 1 1 d . . . H4 H 0.2977 -0.1899 0.9096 0.036 Uiso 1 1 calc R . . C5 C 0.2862(2) -0.0262(4) 0.95091(15) 0.0281(9) Uani 1 1 d . . . C6 C 0.2290(2) 0.0733(4) 0.96078(15) 0.0246(9) Uani 1 1 d . . . C7 C 0.2598(2) 0.1624(4) 1.00141(16) 0.0293(10) Uani 1 1 d . . . C8 C 0.3431(3) 0.1458(4) 1.02936(17) 0.0380(11) Uani 1 1 d . . . H8 H 0.3626 0.2045 1.0561 0.046 Uiso 1 1 calc R . . C9 C 0.4008(3) 0.0474(5) 1.02055(17) 0.0396(11) Uani 1 1 d . A . C10 C 0.3714(3) -0.0378(5) 0.98061(17) 0.0362(11) Uani 1 1 d . . . H10 H 0.4078 -0.1040 0.9730 0.043 Uiso 1 1 calc R . . C11 C 0.2008(3) 0.2743(4) 1.01467(15) 0.0309(10) Uani 1 1 d . . . C12 C 0.1767(3) 0.3474(4) 0.96062(17) 0.0445(12) Uani 1 1 d . . . H12A H 0.1394 0.4153 0.9697 0.067 Uiso 1 1 calc R . . H12B H 0.1449 0.2960 0.9329 0.067 Uiso 1 1 calc R . . H12C H 0.2306 0.3771 0.9451 0.067 Uiso 1 1 calc R . . C13 C 0.1159(3) 0.2287(5) 1.04134(18) 0.0458(12) Uani 1 1 d . . . H13A H 0.1324 0.1828 1.0754 0.069 Uiso 1 1 calc R . . H13B H 0.0823 0.1775 1.0144 0.069 Uiso 1 1 calc R . . H13C H 0.0797 0.2973 1.0510 0.069 Uiso 1 1 calc R . . C14 C 0.2490(3) 0.3609(5) 1.05831(18) 0.0443(12) Uani 1 1 d . . . H14A H 0.2646 0.3172 1.0931 0.066 Uiso 1 1 calc R . . H14B H 0.2099 0.4277 1.0662 0.066 Uiso 1 1 calc R . . H14C H 0.3025 0.3920 1.0429 0.066 Uiso 1 1 calc R . . C15 C 0.4909(3) 0.0333(5) 1.0550(2) 0.0576(14) Uani 1 1 d . . . C16 C 0.5014(9) -0.0759(12) 1.0808(6) 0.094(4) Uiso 0.557(8) 1 d P A 1 H16A H 0.5590 -0.0791 1.1014 0.140 Uiso 0.557(8) 1 calc PR A 1 H16B H 0.4974 -0.1394 1.0524 0.140 Uiso 0.557(8) 1 calc PR A 1 H16C H 0.4551 -0.0871 1.1070 0.140 Uiso 0.557(8) 1 calc PR A 1 C17 C 0.5042(5) 0.1423(8) 1.1013(3) 0.042(2) Uiso 0.557(8) 1 d P A 1 H17A H 0.5031 0.2196 1.0818 0.063 Uiso 0.557(8) 1 calc PR A 1 H17B H 0.5609 0.1325 1.1227 0.063 Uiso 0.557(8) 1 calc PR A 1 H17C H 0.4566 0.1397 1.1270 0.063 Uiso 0.557(8) 1 calc PR A 1 C18 C 0.5669(5) 0.0777(8) 1.0097(4) 0.048(2) Uiso 0.557(8) 1 d P A 1 H18A H 0.5523 0.1581 0.9957 0.072 Uiso 0.557(8) 1 calc PR A 1 H18B H 0.5667 0.0216 0.9781 0.072 Uiso 0.557(8) 1 calc PR A 1 H18C H 0.6254 0.0786 1.0293 0.072 Uiso 0.557(8) 1 calc PR A 1 C16A C 0.4747(10) 0.0178(16) 1.1172(6) 0.097(5) Uiso 0.443(8) 1 d P A 2 H16D H 0.4303 -0.0446 1.1214 0.145 Uiso 0.443(8) 1 calc PR A 2 H16E H 0.4537 0.0935 1.1322 0.145 Uiso 0.443(8) 1 calc PR A 2 H16F H 0.5297 -0.0055 1.1379 0.145 Uiso 0.443(8) 1 calc PR A 2 C17A C 0.5548(13) 0.114(2) 1.0408(9) 0.118(7) Uiso 0.443(8) 1 d P A 2 H17D H 0.5561 0.1181 0.9999 0.177 Uiso 0.443(8) 1 calc PR A 2 H17E H 0.6122 0.0880 1.0571 0.177 Uiso 0.443(8) 1 calc PR A 2 H17F H 0.5411 0.1935 1.0554 0.177 Uiso 0.443(8) 1 calc PR A 2 C18A C 0.5339(7) -0.1023(9) 1.0477(4) 0.040(3) Uiso 0.443(8) 1 d P A 2 H18D H 0.4895 -0.1631 1.0544 0.061 Uiso 0.443(8) 1 calc PR A 2 H18E H 0.5844 -0.1124 1.0748 0.061 Uiso 0.443(8) 1 calc PR A 2 H18F H 0.5531 -0.1112 1.0095 0.061 Uiso 0.443(8) 1 calc PR A 2 C19 C 0.1613(2) -0.2365(3) 0.84531(14) 0.0238(8) Uani 1 1 d . . . H19 H 0.1683 -0.2098 0.8059 0.029 Uiso 1 1 calc R . . C20 C 0.2163(3) -0.3520(4) 0.85500(17) 0.0323(10) Uani 1 1 d . . . H20A H 0.2789 -0.3351 0.8494 0.039 Uiso 1 1 calc R . . H20B H 0.2119 -0.3801 0.8941 0.039 Uiso 1 1 calc R . . C21 C 0.1821(2) -0.4504(3) 0.81362(17) 0.0338(9) Uani 1 1 d . . . H21A H 0.2153 -0.5254 0.8217 0.041 Uiso 1 1 calc R . . H21B H 0.1928 -0.4255 0.7748 0.041 Uiso 1 1 calc R . . C22 C 0.0828(3) -0.4744(3) 0.81788(17) 0.0342(9) Uani 1 1 d . . . H22A H 0.0733 -0.5092 0.8551 0.041 Uiso 1 1 calc R . . H22B H 0.0630 -0.5339 0.7890 0.041 Uiso 1 1 calc R . . C23 C 0.0264(3) -0.3588(4) 0.80967(16) 0.0292(9) Uani 1 1 d . . . H23A H 0.0285 -0.3299 0.7706 0.035 Uiso 1 1 calc R . . H23B H -0.0356 -0.3764 0.8167 0.035 Uiso 1 1 calc R . . C24 C 0.0628(2) -0.2608(3) 0.85102(15) 0.0234(8) Uani 1 1 d . . . H24 H 0.0566 -0.2919 0.8899 0.028 Uiso 1 1 calc R . . C25 C -0.0638(2) -0.1301(3) 0.82591(14) 0.0224(8) Uani 1 1 d . . . H25 H -0.0880 -0.1978 0.8065 0.027 Uiso 1 1 calc R . . C26 C -0.1203(2) -0.0259(3) 0.82923(14) 0.0212(8) Uani 1 1 d . . . C27 C -0.0946(2) 0.0756(4) 0.86373(14) 0.0217(8) Uani 1 1 d . . . C28 C -0.1599(2) 0.1669(4) 0.87317(15) 0.0235(9) Uani 1 1 d . . . C29 C -0.2437(2) 0.1535(4) 0.84558(15) 0.0248(9) Uani 1 1 d . . . H29 H -0.2859 0.2141 0.8513 0.030 Uiso 1 1 calc R . . C30 C -0.2709(2) 0.0547(4) 0.80923(15) 0.0262(9) Uani 1 1 d . . . C31 C -0.2089(2) -0.0340(4) 0.80253(14) 0.0236(9) Uani 1 1 d . . . H31 H -0.2244 -0.1018 0.7800 0.028 Uiso 1 1 calc R . . C32 C -0.1385(2) 0.2760(4) 0.91301(16) 0.0284(9) Uani 1 1 d . . . C33 C -0.2190(3) 0.3641(4) 0.91499(17) 0.0368(10) Uani 1 1 d . . . H33A H -0.2031 0.4312 0.9401 0.055 Uiso 1 1 calc R . . H33B H -0.2693 0.3213 0.9290 0.055 Uiso 1 1 calc R . . H33C H -0.2347 0.3946 0.8772 0.055 Uiso 1 1 calc R . . C34 C -0.1166(3) 0.2296(5) 0.97456(16) 0.0442(12) Uani 1 1 d . . . H34A H -0.1034 0.2979 0.9995 0.066 Uiso 1 1 calc R . . H34B H -0.0656 0.1762 0.9751 0.066 Uiso 1 1 calc R . . H34C H -0.1673 0.1859 0.9874 0.066 Uiso 1 1 calc R . . C35 C -0.0610(3) 0.3494(4) 0.8915(2) 0.0463(12) Uani 1 1 d . . . H35A H -0.0484 0.4177 0.9165 0.069 Uiso 1 1 calc R . . H35B H -0.0768 0.3784 0.8535 0.069 Uiso 1 1 calc R . . H35C H -0.0087 0.2984 0.8911 0.069 Uiso 1 1 calc R . . C36 C -0.3662(2) 0.0526(4) 0.78204(16) 0.0318(10) Uani 1 1 d . . . C37 C -0.3892(3) 0.1753(4) 0.75219(18) 0.0391(11) Uani 1 1 d . . . H37A H -0.4494 0.1724 0.7352 0.059 Uiso 1 1 calc R . . H37B H -0.3481 0.1897 0.7229 0.059 Uiso 1 1 calc R . . H37C H -0.3842 0.2401 0.7798 0.059 Uiso 1 1 calc R . . C38 C -0.3791(3) -0.0507(4) 0.73792(17) 0.0390(11) Uani 1 1 d . . . H38A H -0.4397 -0.0497 0.7216 0.059 Uiso 1 1 calc R . . H38B H -0.3670 -0.1279 0.7564 0.059 Uiso 1 1 calc R . . H38C H -0.3384 -0.0392 0.7082 0.059 Uiso 1 1 calc R . . C39 C -0.4311(3) 0.0310(5) 0.83021(18) 0.0467(12) Uani 1 1 d . . . H39A H -0.4918 0.0290 0.8140 0.070 Uiso 1 1 calc R . . H39B H -0.4246 0.0961 0.8577 0.070 Uiso 1 1 calc R . . H39C H -0.4170 -0.0454 0.8488 0.070 Uiso 1 1 calc R . . C40 C 1.0651(2) 0.8859(3) 0.68640(14) 0.0205(8) Uani 1 1 d . . . H40 H 1.0883 0.9521 0.7075 0.025 Uiso 1 1 calc R . . C41 C 1.1256(2) 0.7861(3) 0.67584(14) 0.0195(8) Uani 1 1 d . . . C42 C 1.0967(2) 0.6844(3) 0.64203(14) 0.0197(8) Uani 1 1 d . . . C43 C 1.1609(2) 0.5920(3) 0.63196(14) 0.0212(8) Uani 1 1 d . . . C44 C 1.2472(2) 0.6085(4) 0.65476(14) 0.0234(9) Uani 1 1 d . . . H44 H 1.2890 0.5485 0.6473 0.028 Uiso 1 1 calc R . . C45 C 1.2773(2) 0.7082(3) 0.68827(15) 0.0216(8) Uani 1 1 d . . . C46 C 1.2142(2) 0.7964(4) 0.69796(14) 0.0226(9) Uani 1 1 d . . . H46 H 1.2311 0.8646 0.7198 0.027 Uiso 1 1 calc R . . C47 C 1.1341(2) 0.4771(4) 0.59729(16) 0.0278(9) Uani 1 1 d . . . C48 C 1.1021(3) 0.5134(4) 0.53661(16) 0.0405(11) Uani 1 1 d . . . H48A H 1.0855 0.4414 0.5150 0.061 Uiso 1 1 calc R . . H48B H 1.1495 0.5551 0.5188 0.061 Uiso 1 1 calc R . . H48C H 1.0511 0.5665 0.5378 0.061 Uiso 1 1 calc R . . C49 C 1.0601(3) 0.4067(4) 0.62714(19) 0.0387(10) Uani 1 1 d . . . H49A H 1.0818 0.3852 0.6653 0.058 Uiso 1 1 calc R . . H49B H 1.0447 0.3338 0.6059 0.058 Uiso 1 1 calc R . . H49C H 1.0079 0.4576 0.6287 0.058 Uiso 1 1 calc R . . C50 C 1.2136(3) 0.3885(4) 0.59335(17) 0.0354(10) Uani 1 1 d . . . H50A H 1.2357 0.3650 0.6312 0.053 Uiso 1 1 calc R . . H50B H 1.2607 0.4281 0.5742 0.053 Uiso 1 1 calc R . . H50C H 1.1941 0.3171 0.5722 0.053 Uiso 1 1 calc R . . C51 C 1.3770(2) 0.7170(4) 0.70977(15) 0.0275(9) Uani 1 1 d . . . C52 C 1.4325(3) 0.7446(5) 0.65886(17) 0.0426(11) Uani 1 1 d . . . H52A H 1.4124 0.8198 0.6413 0.064 Uiso 1 1 calc R . . H52B H 1.4256 0.6794 0.6315 0.064 Uiso 1 1 calc R . . H52C H 1.4946 0.7519 0.6718 0.064 Uiso 1 1 calc R . . C53 C 1.3911(3) 0.8177(4) 0.75468(17) 0.0360(11) Uani 1 1 d . . . H53A H 1.3723 0.8946 0.7383 0.054 Uiso 1 1 calc R . . H53B H 1.4536 0.8220 0.7672 0.054 Uiso 1 1 calc R . . H53C H 1.3565 0.7998 0.7868 0.054 Uiso 1 1 calc R . . C54 C 1.4094(3) 0.5982(4) 0.73749(17) 0.0365(10) Uani 1 1 d . . . H54A H 1.3746 0.5806 0.7696 0.055 Uiso 1 1 calc R . . H54B H 1.4715 0.6059 0.7503 0.055 Uiso 1 1 calc R . . H54C H 1.4025 0.5330 0.7101 0.055 Uiso 1 1 calc R . . C55 C 0.9265(2) 0.9974(3) 0.68136(13) 0.0203(7) Uani 1 1 d . . . H55 H 0.8835 0.9717 0.7089 0.024 Uiso 1 1 calc R . . C56 C 0.9741(2) 1.1111(3) 0.70564(15) 0.0238(8) Uani 1 1 d . . . H56A H 1.0174 1.1391 0.6794 0.029 Uiso 1 1 calc R . . H56B H 1.0061 1.0914 0.7419 0.029 Uiso 1 1 calc R . . C57 C 0.9059(2) 1.2120(3) 0.71461(15) 0.0289(8) Uani 1 1 d . . . H57A H 0.9371 1.2853 0.7281 0.035 Uiso 1 1 calc R . . H57B H 0.8662 1.1867 0.7437 0.035 Uiso 1 1 calc R . . C58 C 0.8501(2) 1.2403(3) 0.65873(16) 0.0282(8) Uani 1 1 d . . . H58A H 0.8890 1.2752 0.6313 0.034 Uiso 1 1 calc R . . H58B H 0.8048 1.3007 0.6663 0.034 Uiso 1 1 calc R . . C59 C 0.8037(2) 1.1257(4) 0.63230(16) 0.0262(8) Uani 1 1 d . . . H59A H 0.7586 1.0967 0.6571 0.031 Uiso 1 1 calc R . . H59B H 0.7740 1.1461 0.5955 0.031 Uiso 1 1 calc R . . C60 C 0.8728(2) 1.0260(3) 0.62469(14) 0.0219(8) Uani 1 1 d . . . H60 H 0.9151 1.0562 0.5976 0.026 Uiso 1 1 calc R . . C61 C 0.7605(2) 0.8994(4) 0.57550(14) 0.0252(9) Uani 1 1 d . . . H61 H 0.7242 0.9685 0.5752 0.030 Uiso 1 1 calc R . . C62 C 0.7256(2) 0.7954(4) 0.54567(15) 0.0239(9) Uani 1 1 d . . . C63 C 0.7797(2) 0.6911(4) 0.53758(15) 0.0239(9) Uani 1 1 d . . . C64 C 0.7466(2) 0.5994(4) 0.49756(14) 0.0226(8) Uani 1 1 d . . . C65 C 0.6621(2) 0.6169(4) 0.47088(15) 0.0276(9) Uani 1 1 d . . . H65 H 0.6406 0.5571 0.4453 0.033 Uiso 1 1 calc R . . C66 C 0.6061(2) 0.7186(4) 0.47943(16) 0.0312(10) Uani 1 1 d . B . C67 C 0.6408(2) 0.8048(4) 0.51661(15) 0.0296(10) Uani 1 1 d . . . H67 H 0.6063 0.8736 0.5231 0.035 Uiso 1 1 calc R . . C68 C 0.8043(2) 0.4911(4) 0.48159(14) 0.0266(9) Uani 1 1 d . . . C69 C 0.8857(2) 0.5378(4) 0.45175(16) 0.0291(9) Uani 1 1 d . . . H69A H 0.9223 0.4698 0.4419 0.044 Uiso 1 1 calc R . . H69B H 0.9202 0.5916 0.4770 0.044 Uiso 1 1 calc R . . H69C H 0.8659 0.5812 0.4176 0.044 Uiso 1 1 calc R . . C70 C 0.7538(3) 0.4018(4) 0.44094(16) 0.0323(10) Uani 1 1 d . . . H70A H 0.7022 0.3709 0.4587 0.048 Uiso 1 1 calc R . . H70B H 0.7926 0.3351 0.4325 0.048 Uiso 1 1 calc R . . H70C H 0.7349 0.4432 0.4061 0.048 Uiso 1 1 calc R . . C71 C 0.8347(3) 0.4167(4) 0.53555(16) 0.0356(10) Uani 1 1 d . . . H71A H 0.7829 0.3875 0.5537 0.053 Uiso 1 1 calc R . . H71B H 0.8696 0.4679 0.5618 0.053 Uiso 1 1 calc R . . H71C H 0.8703 0.3485 0.5248 0.053 Uiso 1 1 calc R . . C72 C 0.5156(3) 0.7328(5) 0.44569(18) 0.0400(11) Uani 1 1 d . . . C73 C 0.5383(8) 0.7806(13) 0.3813(5) 0.061(4) Uiso 0.421(8) 1 d P B 3 H73A H 0.5796 0.8479 0.3848 0.091 Uiso 0.421(8) 1 calc PR B 3 H73B H 0.4839 0.8067 0.3608 0.091 Uiso 0.421(8) 1 calc PR B 3 H73C H 0.5647 0.7151 0.3608 0.091 Uiso 0.421(8) 1 calc PR B 3 C74 C 0.4622(8) 0.8518(11) 0.4639(5) 0.052(3) Uiso 0.421(8) 1 d P B 3 H74A H 0.4996 0.9226 0.4608 0.078 Uiso 0.421(8) 1 calc PR B 3 H74B H 0.4461 0.8434 0.5028 0.078 Uiso 0.421(8) 1 calc PR B 3 H74C H 0.4088 0.8611 0.4392 0.078 Uiso 0.421(8) 1 calc PR B 3 C75 C 0.4592(10) 0.6307(14) 0.4472(7) 0.078(5) Uiso 0.421(8) 1 d P B 3 H75A H 0.4045 0.6465 0.4246 0.116 Uiso 0.421(8) 1 calc PR B 3 H75B H 0.4459 0.6145 0.4861 0.116 Uiso 0.421(8) 1 calc PR B 3 H75C H 0.4887 0.5610 0.4320 0.116 Uiso 0.421(8) 1 calc PR B 3 C73A C 0.5172(7) 0.8436(10) 0.4065(4) 0.067(3) Uiso 0.579(8) 1 d P B 4 H73D H 0.5664 0.8365 0.3823 0.101 Uiso 0.579(8) 1 calc PR B 4 H73E H 0.5242 0.9164 0.4293 0.101 Uiso 0.579(8) 1 calc PR B 4 H73F H 0.4618 0.8478 0.3833 0.101 Uiso 0.579(8) 1 calc PR B 4 C74A C 0.4411(6) 0.7397(9) 0.4857(4) 0.070(3) Uiso 0.579(8) 1 d P B 4 H74D H 0.4435 0.6694 0.5104 0.105 Uiso 0.579(8) 1 calc PR B 4 H74E H 0.3843 0.7414 0.4640 0.105 Uiso 0.579(8) 1 calc PR B 4 H74F H 0.4477 0.8125 0.5085 0.105 Uiso 0.579(8) 1 calc PR B 4 C75A C 0.4902(5) 0.6214(7) 0.4064(3) 0.041(2) Uiso 0.579(8) 1 d P B 4 H75D H 0.4941 0.5477 0.4287 0.061 Uiso 0.579(8) 1 calc PR B 4 H75E H 0.5310 0.6166 0.3763 0.061 Uiso 0.579(8) 1 calc PR B 4 H75F H 0.4301 0.6313 0.3900 0.061 Uiso 0.579(8) 1 calc PR B 4 C76 C 0.8413(3) 0.5795(4) 0.6970(2) 0.0489(12) Uani 1 1 d . . . H76A H 0.8879 0.5502 0.7244 0.059 Uiso 1 1 calc R . . H76B H 0.8455 0.5335 0.6618 0.059 Uiso 1 1 calc R . . C77 C 0.7522(3) 0.5559(4) 0.71991(17) 0.0405(10) Uani 1 1 d . . . H77 H 0.7464 0.4673 0.7245 0.049 Uiso 1 1 calc R . . C78 C 0.6762(3) 0.5973(7) 0.6792(3) 0.0857(19) Uani 1 1 d . . . H78A H 0.6201 0.5810 0.6955 0.129 Uiso 1 1 calc R . . H78B H 0.6784 0.5539 0.6436 0.129 Uiso 1 1 calc R . . H78C H 0.6816 0.6834 0.6723 0.129 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 0.0209(6) 0.0233(7) 0.0200(5) -0.0013(5) -0.0027(4) -0.0010(5) Al2 0.0182(5) 0.0198(6) 0.0188(5) -0.0008(5) -0.0013(4) -0.0005(5) Cl1 0.0818(9) 0.0445(7) 0.0448(7) -0.0018(6) 0.0267(6) -0.0104(7) Cl2 0.0742(8) 0.0460(7) 0.0436(6) 0.0002(6) 0.0300(6) -0.0064(6) N1 0.0258(17) 0.0238(17) 0.0196(15) 0.0006(13) -0.0014(13) -0.0031(14) N2 0.0236(16) 0.0211(17) 0.0214(15) 0.0007(13) 0.0012(13) 0.0001(13) N3 0.0198(16) 0.0207(17) 0.0178(14) 0.0000(13) -0.0017(12) 0.0013(12) N4 0.0226(16) 0.0195(16) 0.0204(15) 0.0000(13) -0.0020(12) -0.0003(13) O1 0.0299(14) 0.0262(15) 0.0232(13) 0.0021(11) -0.0012(11) -0.0069(12) O2 0.0230(13) 0.0311(17) 0.0236(13) -0.0055(12) -0.0046(11) 0.0006(12) O3 0.0227(13) 0.0287(16) 0.0257(13) -0.0063(12) -0.0004(11) -0.0022(12) O4 0.0306(14) 0.0238(15) 0.0275(13) -0.0016(11) 0.0084(11) -0.0051(11) O5 0.0202(13) 0.0236(15) 0.0292(14) -0.0067(11) -0.0066(11) 0.0032(11) O6 0.0218(13) 0.0256(15) 0.0228(13) -0.0028(11) -0.0043(11) 0.0002(12) C1 0.054(3) 0.032(3) 0.032(2) -0.0060(19) 0.009(2) -0.007(2) C2 0.037(2) 0.049(3) 0.047(3) -0.004(2) 0.005(2) -0.001(2) C3 0.046(3) 0.051(3) 0.102(4) -0.026(3) 0.029(3) -0.027(2) C4 0.023(2) 0.040(2) 0.028(2) 0.0000(18) 0.0008(16) 0.0090(18) C5 0.023(2) 0.035(2) 0.0259(19) -0.0001(18) -0.0030(16) -0.0032(18) C6 0.022(2) 0.034(2) 0.0170(18) 0.0004(17) -0.0023(15) -0.0052(18) C7 0.025(2) 0.040(3) 0.023(2) -0.0011(19) 0.0022(16) -0.006(2) C8 0.035(2) 0.051(3) 0.027(2) -0.002(2) -0.0083(19) -0.006(2) C9 0.027(2) 0.057(3) 0.033(2) -0.005(2) -0.0093(18) -0.002(2) C10 0.021(2) 0.050(3) 0.037(2) 0.001(2) -0.0045(17) 0.006(2) C11 0.031(2) 0.034(2) 0.027(2) -0.0079(19) -0.0016(17) -0.003(2) C12 0.061(3) 0.035(3) 0.037(2) -0.010(2) -0.004(2) 0.007(2) C13 0.038(3) 0.061(3) 0.039(2) -0.022(2) 0.006(2) -0.003(2) C14 0.039(2) 0.056(3) 0.038(2) -0.017(2) 0.007(2) -0.008(2) C15 0.045(3) 0.057(4) 0.067(3) -0.010(3) -0.023(3) -0.002(3) C19 0.0279(19) 0.0235(19) 0.0199(17) -0.0008(15) 0.0015(14) 0.0030(16) C20 0.031(2) 0.032(2) 0.035(2) 0.0005(18) 0.0046(17) 0.0059(18) C21 0.031(2) 0.025(2) 0.046(2) -0.0020(18) 0.0074(18) 0.0048(17) C22 0.041(2) 0.025(2) 0.037(2) -0.0035(18) 0.0030(18) -0.0010(18) C23 0.032(2) 0.024(2) 0.031(2) -0.0005(17) 0.0026(17) 0.0021(18) C24 0.0280(19) 0.020(2) 0.0218(18) 0.0038(15) 0.0005(15) 0.0009(15) C25 0.025(2) 0.020(2) 0.0219(18) -0.0021(16) 0.0001(15) -0.0065(17) C26 0.0223(19) 0.023(2) 0.0177(17) 0.0010(16) 0.0007(15) -0.0012(17) C27 0.0188(19) 0.029(2) 0.0173(17) 0.0043(16) -0.0017(15) -0.0038(17) C28 0.024(2) 0.024(2) 0.0228(19) 0.0027(16) 0.0039(15) 0.0011(18) C29 0.024(2) 0.024(2) 0.027(2) -0.0027(17) 0.0040(16) -0.0015(18) C30 0.022(2) 0.034(2) 0.0226(19) 0.0040(18) 0.0032(16) 0.0018(19) C31 0.026(2) 0.024(2) 0.0207(19) -0.0017(16) 0.0007(16) -0.0064(18) C32 0.030(2) 0.023(2) 0.032(2) -0.0084(18) 0.0012(17) 0.0006(18) C33 0.034(2) 0.037(3) 0.039(2) -0.009(2) -0.0013(19) 0.008(2) C34 0.047(3) 0.056(3) 0.028(2) -0.016(2) -0.0082(19) 0.016(2) C35 0.040(3) 0.037(3) 0.063(3) -0.014(2) 0.008(2) 0.000(2) C36 0.021(2) 0.038(2) 0.036(2) -0.0037(19) -0.0042(17) -0.0014(18) C37 0.028(2) 0.046(3) 0.042(2) 0.002(2) -0.0085(18) 0.006(2) C38 0.032(2) 0.047(3) 0.038(2) 0.000(2) -0.0049(18) -0.008(2) C39 0.023(2) 0.073(4) 0.044(2) -0.007(2) -0.0008(18) -0.008(2) C40 0.025(2) 0.022(2) 0.0140(16) -0.0028(15) -0.0032(14) -0.0014(16) C41 0.0210(18) 0.020(2) 0.0174(17) 0.0021(16) 0.0012(15) -0.0048(17) C42 0.0189(19) 0.023(2) 0.0174(18) 0.0011(16) 0.0010(15) -0.0022(17) C43 0.0219(19) 0.022(2) 0.0197(17) -0.0014(16) 0.0002(15) -0.0007(17) C44 0.0201(19) 0.027(2) 0.0236(19) 0.0035(18) 0.0030(15) 0.0059(18) C45 0.0216(19) 0.022(2) 0.0210(18) 0.0026(16) -0.0006(15) -0.0003(17) C46 0.024(2) 0.022(2) 0.0208(19) 0.0009(16) 0.0005(16) -0.0032(17) C47 0.021(2) 0.031(2) 0.030(2) -0.0072(18) -0.0042(16) 0.0034(18) C48 0.038(2) 0.046(3) 0.036(2) -0.019(2) -0.0054(19) 0.011(2) C49 0.036(2) 0.026(2) 0.055(3) -0.011(2) 0.0073(19) -0.0080(19) C50 0.034(2) 0.031(2) 0.041(2) -0.014(2) -0.0012(18) 0.0048(19) C51 0.0222(19) 0.035(2) 0.0242(19) -0.0009(18) -0.0036(16) 0.0008(18) C52 0.025(2) 0.059(3) 0.044(2) -0.001(2) 0.0017(18) 0.000(2) C53 0.018(2) 0.047(3) 0.041(2) -0.004(2) -0.0090(17) -0.0011(19) C54 0.021(2) 0.045(3) 0.042(2) 0.002(2) -0.0067(17) 0.0066(19) C55 0.0217(17) 0.0218(19) 0.0172(17) 0.0000(15) 0.0006(14) 0.0037(15) C56 0.028(2) 0.021(2) 0.0216(18) -0.0036(16) -0.0017(15) 0.0004(17) C57 0.038(2) 0.0213(19) 0.0271(19) -0.0050(16) -0.0040(16) -0.0019(16) C58 0.029(2) 0.0179(19) 0.038(2) 0.0009(16) 0.0014(16) 0.0032(16) C59 0.0245(19) 0.024(2) 0.0293(19) 0.0006(17) -0.0030(16) 0.0026(16) C60 0.0197(18) 0.0233(19) 0.0226(18) -0.0002(15) -0.0005(14) -0.0015(15) C61 0.0222(19) 0.028(2) 0.0254(19) -0.0014(17) 0.0010(16) 0.0044(16) C62 0.0199(19) 0.029(2) 0.0225(18) 0.0018(17) -0.0002(15) 0.0019(17) C63 0.0185(19) 0.029(2) 0.0235(19) 0.0024(17) -0.0009(15) -0.0037(17) C64 0.0247(19) 0.028(2) 0.0148(17) 0.0012(17) 0.0008(15) -0.0042(18) C65 0.026(2) 0.034(2) 0.0229(19) -0.0045(19) 0.0002(16) -0.011(2) C66 0.021(2) 0.044(3) 0.028(2) 0.001(2) 0.0014(16) -0.003(2) C67 0.022(2) 0.037(2) 0.030(2) -0.0046(19) -0.0021(17) 0.0026(18) C68 0.032(2) 0.027(2) 0.0204(19) -0.0024(17) 0.0006(16) -0.0007(19) C69 0.026(2) 0.031(2) 0.031(2) -0.0060(18) 0.0025(17) 0.0002(18) C70 0.035(2) 0.032(2) 0.030(2) -0.0083(19) -0.0010(17) -0.008(2) C71 0.048(3) 0.027(2) 0.031(2) -0.0034(18) -0.0058(19) -0.001(2) C72 0.024(2) 0.055(3) 0.040(2) -0.009(2) -0.0107(18) 0.001(2) C76 0.062(3) 0.040(3) 0.046(3) -0.003(2) 0.008(2) -0.006(2) C77 0.042(2) 0.035(2) 0.046(2) -0.008(2) 0.012(2) -0.009(2) C78 0.042(3) 0.123(5) 0.093(4) -0.012(4) 0.003(3) -0.002(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Al1 O1 1.754(3) . ? Al1 O2 1.798(3) . ? Al1 O3 1.806(3) . ? Al1 N2 1.998(3) . ? Al1 N1 2.018(3) . ? Al2 O4 1.748(3) . ? Al2 O5 1.798(3) . ? Al2 O6 1.820(3) . ? Al2 N3 2.004(3) . ? Al2 N4 2.010(3) . ? Cl1 C2 1.810(4) . ? Cl2 C77 1.811(4) . ? N1 C4 1.278(4) . ? N1 C19 1.483(4) . ? N2 C25 1.292(4) . ? N2 C24 1.485(4) . ? N3 C40 1.288(4) . ? N3 C55 1.476(4) . ? N4 C61 1.300(4) . ? N4 C60 1.474(4) . ? O1 C1 1.395(5) . ? O2 C6 1.330(4) . ? O3 C27 1.335(4) . ? O4 C76 1.401(5) . ? O5 C42 1.322(4) . ? O6 C63 1.322(4) . ? C1 C2 1.519(6) . ? C2 C3 1.517(6) . ? C4 C5 1.447(6) . ? C5 C6 1.410(6) . ? C5 C10 1.415(5) . ? C6 C7 1.418(5) . ? C7 C8 1.379(5) . ? C7 C11 1.552(6) . ? C8 C9 1.402(6) . ? C9 C10 1.372(6) . ? C9 C15 1.530(6) . ? C11 C12 1.519(6) . ? C11 C13 1.532(6) . ? C11 C14 1.537(6) . ? C15 C16 1.343(13) . ? C15 C17A 1.36(2) . ? C15 C16A 1.501(15) . ? C15 C17 1.616(9) . ? C15 C18A 1.630(11) . ? C15 C18 1.673(10) . ? C19 C24 1.508(5) . ? C19 C20 1.516(5) . ? C20 C21 1.514(5) . ? C21 C22 1.515(5) . ? C22 C23 1.525(5) . ? C23 C24 1.520(5) . ? C25 C26 1.423(5) . ? C26 C27 1.411(5) . ? C26 C31 1.429(5) . ? C27 C28 1.423(5) . ? C28 C29 1.379(5) . ? C28 C32 1.535(5) . ? C29 C30 1.418(5) . ? C30 C31 1.357(5) . ? C30 C36 1.522(5) . ? C32 C35 1.520(6) . ? C32 C34 1.542(6) . ? C32 C33 1.544(5) . ? C36 C38 1.534(6) . ? C36 C37 1.542(6) . ? C36 C39 1.550(6) . ? C40 C41 1.448(5) . ? C41 C46 1.394(5) . ? C41 C42 1.416(5) . ? C42 C43 1.424(5) . ? C43 C44 1.374(5) . ? C43 C47 1.535(5) . ? C44 C45 1.401(5) . ? C45 C46 1.377(5) . ? C45 C51 1.543(5) . ? C47 C48 1.521(5) . ? C47 C50 1.540(5) . ? C47 C49 1.550(6) . ? C51 C54 1.517(6) . ? C51 C52 1.525(5) . ? C51 C53 1.528(6) . ? C55 C56 1.523(5) . ? C55 C60 1.537(4) . ? C56 C57 1.526(5) . ? C57 C58 1.536(5) . ? C58 C59 1.543(5) . ? C59 C60 1.520(5) . ? C61 C62 1.416(5) . ? C62 C67 1.403(5) . ? C62 C63 1.418(6) . ? C63 C64 1.438(5) . ? C64 C65 1.384(5) . ? C64 C68 1.525(5) . ? C65 C66 1.414(6) . ? C66 C67 1.363(6) . ? C66 C72 1.528(5) . ? C68 C70 1.528(5) . ? C68 C69 1.529(5) . ? C68 C71 1.545(5) . ? C72 C75 1.400(15) . ? C72 C74A 1.501(10) . ? C72 C73A 1.521(10) . ? C72 C75A 1.558(9) . ? C72 C74 1.600(12) . ? C72 C73 1.651(13) . ? C76 C77 1.488(6) . ? C77 C78 1.504(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Al1 O2 109.51(13) . . ? O1 Al1 O3 107.44(13) . . ? O2 Al1 O3 89.79(12) . . ? O1 Al1 N2 103.54(13) . . ? O2 Al1 N2 145.75(13) . . ? O3 Al1 N2 88.75(12) . . ? O1 Al1 N1 96.50(13) . . ? O2 Al1 N1 88.42(12) . . ? O3 Al1 N1 155.15(13) . . ? N2 Al1 N1 79.03(12) . . ? O4 Al2 O5 110.95(13) . . ? O4 Al2 O6 106.53(13) . . ? O5 Al2 O6 89.75(12) . . ? O4 Al2 N3 97.02(12) . . ? O5 Al2 N3 88.78(12) . . ? O6 Al2 N3 155.27(13) . . ? O4 Al2 N4 103.16(13) . . ? O5 Al2 N4 144.93(13) . . ? O6 Al2 N4 88.19(12) . . ? N3 Al2 N4 79.04(12) . . ? C4 N1 C19 120.8(3) . . ? C4 N1 Al1 126.0(3) . . ? C19 N1 Al1 112.8(2) . . ? C25 N2 C24 120.4(3) . . ? C25 N2 Al1 122.8(3) . . ? C24 N2 Al1 116.7(2) . . ? C40 N3 C55 120.3(3) . . ? C40 N3 Al2 127.0(2) . . ? C55 N3 Al2 112.7(2) . . ? C61 N4 C60 120.5(3) . . ? C61 N4 Al2 122.2(3) . . ? C60 N4 Al2 116.9(2) . . ? C1 O1 Al1 124.8(2) . . ? C6 O2 Al1 134.7(2) . . ? C27 O3 Al1 131.9(2) . . ? C76 O4 Al2 124.4(3) . . ? C42 O5 Al2 135.4(2) . . ? C63 O6 Al2 131.1(2) . . ? O1 C1 C2 112.9(4) . . ? C3 C2 C1 114.1(4) . . ? C3 C2 Cl1 108.4(3) . . ? C1 C2 Cl1 109.5(3) . . ? N1 C4 C5 125.3(4) . . ? C6 C5 C10 121.5(4) . . ? C6 C5 C4 121.5(3) . . ? C10 C5 C4 116.8(4) . . ? O2 C6 C5 120.8(3) . . ? O2 C6 C7 121.3(4) . . ? C5 C6 C7 117.8(3) . . ? C8 C7 C6 118.1(4) . . ? C8 C7 C11 121.0(4) . . ? C6 C7 C11 120.9(3) . . ? C7 C8 C9 125.1(4) . . ? C10 C9 C8 116.7(4) . . ? C10 C9 C15 121.5(4) . . ? C8 C9 C15 121.8(4) . . ? C9 C10 C5 120.7(4) . . ? C12 C11 C13 110.7(4) . . ? C12 C11 C14 107.7(4) . . ? C13 C11 C14 107.1(3) . . ? C12 C11 C7 110.8(3) . . ? C13 C11 C7 108.7(4) . . ? C14 C11 C7 111.8(3) . . ? C16 C15 C17A 128.7(11) . . ? C16 C15 C16A 59.0(8) . . ? C17A C15 C16A 118.0(12) . . ? C16 C15 C9 113.5(7) . . ? C17A C15 C9 114.4(9) . . ? C16A C15 C9 109.3(7) . . ? C16 C15 C17 110.4(7) . . ? C17A C15 C17 68.0(10) . . ? C16A C15 C17 56.8(7) . . ? C9 C15 C17 110.2(5) . . ? C16 C15 C18A 37.1(6) . . ? C17A C15 C18A 106.2(10) . . ? C16A C15 C18A 95.0(8) . . ? C9 C15 C18A 112.0(5) . . ? C17 C15 C18A 135.2(6) . . ? C16 C15 C18 118.6(8) . . ? C17A C15 C18 30.8(9) . . ? C16A C15 C18 143.6(8) . . ? C9 C15 C18 104.3(4) . . ? C17 C15 C18 98.7(5) . . ? C18A C15 C18 84.8(5) . . ? N1 C19 C24 105.2(3) . . ? N1 C19 C20 117.8(3) . . ? C24 C19 C20 111.1(3) . . ? C21 C20 C19 109.9(3) . . ? C20 C21 C22 111.8(3) . . ? C21 C22 C23 112.5(3) . . ? C24 C23 C22 109.5(3) . . ? N2 C24 C19 106.0(3) . . ? N2 C24 C23 116.8(3) . . ? C19 C24 C23 112.2(3) . . ? N2 C25 C26 126.2(3) . . ? C27 C26 C25 121.4(3) . . ? C27 C26 C31 120.6(3) . . ? C25 C26 C31 117.4(3) . . ? O3 C27 C26 120.2(3) . . ? O3 C27 C28 121.2(3) . . ? C26 C27 C28 118.5(3) . . ? C29 C28 C27 117.6(3) . . ? C29 C28 C32 120.9(3) . . ? C27 C28 C32 121.5(3) . . ? C28 C29 C30 125.3(4) . . ? C31 C30 C29 116.3(3) . . ? C31 C30 C36 124.6(4) . . ? C29 C30 C36 119.1(3) . . ? C30 C31 C26 121.6(4) . . ? C35 C32 C28 110.1(3) . . ? C35 C32 C34 111.2(3) . . ? C28 C32 C34 109.5(3) . . ? C35 C32 C33 106.9(3) . . ? C28 C32 C33 111.8(3) . . ? C34 C32 C33 107.2(3) . . ? C30 C36 C38 111.4(3) . . ? C30 C36 C37 110.5(3) . . ? C38 C36 C37 108.8(3) . . ? C30 C36 C39 108.0(3) . . ? C38 C36 C39 108.7(4) . . ? C37 C36 C39 109.3(4) . . ? N3 C40 C41 124.9(3) . . ? C46 C41 C42 121.2(3) . . ? C46 C41 C40 117.6(3) . . ? C42 C41 C40 121.2(3) . . ? O5 C42 C41 121.4(3) . . ? O5 C42 C43 120.8(3) . . ? C41 C42 C43 117.8(3) . . ? C44 C43 C42 117.8(3) . . ? C44 C43 C47 121.3(3) . . ? C42 C43 C47 120.9(3) . . ? C43 C44 C45 125.4(3) . . ? C46 C45 C44 116.1(3) . . ? C46 C45 C51 123.9(3) . . ? C44 C45 C51 119.9(3) . . ? C45 C46 C41 121.7(3) . . ? C48 C47 C43 109.6(3) . . ? C48 C47 C50 107.8(3) . . ? C43 C47 C50 111.8(3) . . ? C48 C47 C49 111.1(3) . . ? C43 C47 C49 109.8(3) . . ? C50 C47 C49 106.8(3) . . ? C54 C51 C52 109.2(3) . . ? C54 C51 C53 107.3(3) . . ? C52 C51 C53 109.6(4) . . ? C54 C51 C45 111.1(3) . . ? C52 C51 C45 108.6(3) . . ? C53 C51 C45 110.9(3) . . ? N3 C55 C56 118.2(3) . . ? N3 C55 C60 104.9(2) . . ? C56 C55 C60 111.1(3) . . ? C55 C56 C57 110.1(3) . . ? C56 C57 C58 111.0(3) . . ? C57 C58 C59 112.4(3) . . ? C60 C59 C58 109.9(3) . . ? N4 C60 C59 116.8(3) . . ? N4 C60 C55 105.3(3) . . ? C59 C60 C55 111.4(3) . . ? N4 C61 C62 126.0(4) . . ? C67 C62 C61 118.1(4) . . ? C67 C62 C63 119.9(4) . . ? C61 C62 C63 121.2(3) . . ? O6 C63 C62 121.0(3) . . ? O6 C63 C64 120.6(3) . . ? C62 C63 C64 118.3(3) . . ? C65 C64 C63 117.5(4) . . ? C65 C64 C68 120.6(3) . . ? C63 C64 C68 121.7(3) . . ? C64 C65 C66 125.1(4) . . ? C67 C66 C65 115.5(3) . . ? C67 C66 C72 123.1(4) . . ? C65 C66 C72 121.2(4) . . ? C66 C67 C62 123.6(4) . . ? C64 C68 C70 112.7(3) . . ? C64 C68 C69 109.3(3) . . ? C70 C68 C69 107.7(3) . . ? C64 C68 C71 110.5(3) . . ? C70 C68 C71 106.2(3) . . ? C69 C68 C71 110.4(3) . . ? C75 C72 C74A 63.5(8) . . ? C75 C72 C73A 133.2(7) . . ? C74A C72 C73A 112.1(6) . . ? C75 C72 C66 114.7(7) . . ? C74A C72 C66 110.4(5) . . ? C73A C72 C66 110.2(5) . . ? C75 C72 C75A 42.9(6) . . ? C74A C72 C75A 104.2(5) . . ? C73A C72 C75A 106.3(5) . . ? C66 C72 C75A 113.5(4) . . ? C75 C72 C74 109.4(8) . . ? C74A C72 C74 52.5(6) . . ? C73A C72 C74 62.5(6) . . ? C66 C72 C74 112.6(5) . . ? C75A C72 C74 133.5(6) . . ? C75 C72 C73 115.8(8) . . ? C74A C72 C73 139.3(6) . . ? C73A C72 C73 35.4(5) . . ? C66 C72 C73 106.1(5) . . ? C75A C72 C73 76.5(6) . . ? C74 C72 C73 96.9(7) . . ? O4 C76 C77 113.0(4) . . ? C76 C77 C78 112.0(4) . . ? C76 C77 Cl2 111.0(3) . . ? C78 C77 Cl2 111.4(3) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.565 _refine_diff_density_min -0.371 _refine_diff_density_rms 0.054 # END