Supplementary Material (ESI) for Journal of Materials Chemistry This journal is © The Royal Society of Chemistry 2004 data_global _journal_name_full 'Journal of Materials Chemistry' _journal_coden_Cambridge 1145 _publ_contact_author_name 'Dr Stephane Parola' _publ_contact_author_address ; LMI UMR CNRS 5615 Université Claude Bernard Lyon 1 43 bd 11 novembre 1918 Villeurbanne 69622 FRANCE ; _publ_contact_author_email STEPHANE.PAROLA@UNIV-LYON1.FR _publ_section_title ; Purpose Construction Versus Self-Assembly in Approach to Single Source Precursors of Spinel Materials. Synthesis, Structure and Stability Studies of MIIAl2(acac)3(OiPr)4(OAc), MII = Mn, Co, Zn A New Class of Heterometallic Heteroleptic Alkoxide Complexes. ; loop_ _publ_author_name 'Parola Stephane' 'Michel Andrieux' 'Fernand Chassagneux' 'Vadim Kessler' 'Mikael Kritikos' ; L.Rapenne ; 'Gulaim A. Seisenbaeva' 'Evgeniya V. Suslova' data_znalac2i _database_code_depnum_ccdc_archive 'CCDC 200109' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32.50 H56 Al2 O12 Zn' _chemical_formula_weight 758.10 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 '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 11.5823(14) _cell_length_b 16.170(2) _cell_length_c 23.010(3) _cell_angle_alpha 103.741(2) _cell_angle_beta 103.341(2) _cell_angle_gamma 90.417(2) _cell_volume 4064.3(9) _cell_formula_units_Z 4 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 994(I>2sigma(I)) _cell_measurement_theta_min 0.94 _cell_measurement_theta_max 20.00 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.239 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1612 _exptl_absorpt_coefficient_mu 0.700 _exptl_absorpt_correction_type Empyrical _exptl_absorpt_correction_T_min 0.7434 _exptl_absorpt_correction_T_max 0.9022 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(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 'Bruker SMART CCD 1k' _diffrn_measurement_method 'Bruker SMART' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12724 _diffrn_reflns_av_R_equivalents 0.0743 _diffrn_reflns_av_sigmaI/netI 0.1323 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 0.94 _diffrn_reflns_theta_max 20.00 _reflns_number_total 7520 _reflns_number_gt 3787 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINTPLUS' _computing_data_reduction 'Bruker SAINTPLUS' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL-NT' _computing_publication_material 'Bruker SHELXTL-NT' _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^)+(0.1014P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7520 _refine_ls_number_parameters 821 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1506 _refine_ls_R_factor_gt 0.0711 _refine_ls_wR_factor_ref 0.1898 _refine_ls_wR_factor_gt 0.1654 _refine_ls_goodness_of_fit_ref 0.908 _refine_ls_restrained_S_all 0.908 _refine_ls_shift/su_max 0.009 _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 Zn1 Zn 0.59496(11) 0.73967(8) 0.39867(6) 0.0587(4) Uani 1 1 d . . . Al1 Al 0.3414(3) 0.73447(19) 0.42296(14) 0.0502(9) Uani 1 1 d . . . Al2 Al 0.3598(3) 0.7547(2) 0.30537(14) 0.0533(9) Uani 1 1 d . . . O1 O 0.3853(5) 0.8185(4) 0.3871(3) 0.0514(18) Uani 1 1 d . . . O2 O 0.3569(6) 0.6686(4) 0.3475(3) 0.0520(18) Uani 1 1 d . . . O5 O 0.3196(6) 0.8138(4) 0.4941(3) 0.0562(19) Uani 1 1 d . . . O3 O 0.5001(5) 0.7259(4) 0.4564(3) 0.0540(18) Uani 1 1 d . . . O6 O 0.2935(6) 0.6456(4) 0.4536(3) 0.0584(19) Uani 1 1 d . . . O9 O 0.7180(7) 0.8362(4) 0.4380(3) 0.070(2) Uani 1 1 d . . . O7 O 0.3198(6) 0.6802(4) 0.2252(3) 0.064(2) Uani 1 1 d . . . O11 O 0.1749(6) 0.7444(4) 0.3868(4) 0.0561(19) Uani 1 1 d . . . O8 O 0.3540(6) 0.8482(4) 0.2706(4) 0.064(2) Uani 1 1 d . . . O10 O 0.7141(7) 0.6534(4) 0.3987(3) 0.066(2) Uani 1 1 d . . . O4 O 0.5227(5) 0.7476(4) 0.3156(3) 0.060(2) Uani 1 1 d . . . O12 O 0.1889(6) 0.7619(4) 0.2953(3) 0.0591(19) Uani 1 1 d . . . C94 C 0.8302(12) 0.8267(8) 0.4513(5) 0.061(3) Uani 1 1 d . . . C4 C 0.5822(11) 0.7462(8) 0.2686(6) 0.080(4) Uani 1 1 d . . . H27A H 0.5220 0.7546 0.2332 0.096 Uiso 1 1 calc R . . C61 C 0.1305(10) 0.7567(7) 0.3353(6) 0.060(3) Uani 1 1 d . . . C54 C 0.2496(9) 0.6486(8) 0.5001(6) 0.064(3) Uani 1 1 d . . . C52 C 0.2672(10) 0.8018(8) 0.5347(5) 0.061(3) Uani 1 1 d . . . C92 C 0.8241(12) 0.6688(8) 0.4180(5) 0.052(3) Uani 1 1 d . . . C3 C 0.5489(9) 0.7183(7) 0.5172(5) 0.057(3) Uani 1 1 d . . . H36A H 0.4831 0.7226 0.5378 0.068 Uiso 1 1 calc R . . C31 C 0.6401(11) 0.7873(8) 0.5548(5) 0.095(4) Uani 1 1 d . . . H38A H 0.6064 0.8416 0.5565 0.142 Uiso 1 1 calc R . . H38B H 0.7068 0.7852 0.5365 0.142 Uiso 1 1 calc R . . H38C H 0.6658 0.7795 0.5958 0.142 Uiso 1 1 calc R . . C74 C 0.3093(11) 0.8519(9) 0.2150(7) 0.072(4) Uani 1 1 d . . . C53 C 0.2300(9) 0.7218(8) 0.5387(5) 0.063(3) Uani 1 1 d . . . H41A H 0.1902 0.7184 0.5689 0.075 Uiso 1 1 calc R . . C72 C 0.2792(10) 0.6996(9) 0.1750(6) 0.067(3) Uani 1 1 d . . . C73 C 0.2701(10) 0.7821(11) 0.1677(6) 0.080(4) Uani 1 1 d . . . H44A H 0.2357 0.7900 0.1288 0.096 Uiso 1 1 calc R . . C51 C 0.2486(11) 0.8828(7) 0.5787(5) 0.088(4) Uani 1 1 d . . . H46A H 0.2803 0.9308 0.5683 0.132 Uiso 1 1 calc R . . H46B H 0.2885 0.8816 0.6200 0.132 Uiso 1 1 calc R . . H46C H 0.1650 0.8876 0.5760 0.132 Uiso 1 1 calc R . . C1 C 0.3968(10) 0.9101(7) 0.4149(5) 0.067(3) Uani 1 1 d . . . H47A H 0.4212 0.9165 0.4595 0.080 Uiso 1 1 calc R . . C91 C 0.9013(10) 0.5960(7) 0.4115(6) 0.085(4) Uani 1 1 d . . . H52A H 0.8528 0.5439 0.3924 0.128 Uiso 1 1 calc R . . H52B H 0.9468 0.5932 0.4514 0.128 Uiso 1 1 calc R . . H52C H 0.9541 0.6038 0.3863 0.128 Uiso 1 1 calc R . . C32 C 0.5952(12) 0.6315(8) 0.5170(6) 0.102(4) Uani 1 1 d . . . H54A H 0.5331 0.5884 0.4945 0.153 Uiso 1 1 calc R . . H54B H 0.6211 0.6261 0.5586 0.153 Uiso 1 1 calc R . . H54C H 0.6609 0.6247 0.4977 0.153 Uiso 1 1 calc R . . C41 C 0.6728(11) 0.8198(9) 0.2857(6) 0.117(5) Uani 1 1 d . . . H57A H 0.6356 0.8721 0.2969 0.176 Uiso 1 1 calc R . . H57B H 0.7059 0.8203 0.2512 0.176 Uiso 1 1 calc R . . H57C H 0.7350 0.8141 0.3199 0.176 Uiso 1 1 calc R . . C55 C 0.2211(10) 0.5641(7) 0.5109(6) 0.093(4) Uani 1 1 d . . . H59A H 0.2405 0.5193 0.4797 0.140 Uiso 1 1 calc R . . H59B H 0.1379 0.5581 0.5094 0.140 Uiso 1 1 calc R . . H59C H 0.2667 0.5605 0.5507 0.140 Uiso 1 1 calc R . . C2 C 0.3455(11) 0.5793(8) 0.3212(6) 0.079(4) Uani 1 1 d . . . H61A H 0.3696 0.5737 0.2824 0.095 Uiso 1 1 calc R . . C21 C 0.2152(12) 0.5467(8) 0.3006(6) 0.112(5) Uani 1 1 d . . . H62A H 0.1704 0.5830 0.2776 0.168 Uiso 1 1 calc R . . H62B H 0.1850 0.5469 0.3362 0.168 Uiso 1 1 calc R . . H62C H 0.2081 0.4896 0.2752 0.168 Uiso 1 1 calc R . . C11 C 0.4919(9) 0.9559(6) 0.3989(5) 0.075(3) Uani 1 1 d . . . H64A H 0.5649 0.9285 0.4076 0.113 Uiso 1 1 calc R . . H64B H 0.5025 1.0140 0.4228 0.113 Uiso 1 1 calc R . . H64C H 0.4698 0.9548 0.3558 0.113 Uiso 1 1 calc R . . C71 C 0.2407(12) 0.6247(8) 0.1205(5) 0.106(5) Uani 1 1 d . . . H65A H 0.2524 0.5728 0.1338 0.159 Uiso 1 1 calc R . . H65B H 0.2870 0.6264 0.0911 0.159 Uiso 1 1 calc R . . H65C H 0.1581 0.6270 0.1017 0.159 Uiso 1 1 calc R . . C95 C 0.9039(10) 0.9088(7) 0.4782(6) 0.097(4) Uani 1 1 d . . . H68A H 0.8530 0.9554 0.4797 0.146 Uiso 1 1 calc R . . H68B H 0.9577 0.9141 0.4530 0.146 Uiso 1 1 calc R . . H68C H 0.9484 0.9096 0.5191 0.146 Uiso 1 1 calc R . . C93 C 0.8814(10) 0.7523(9) 0.4457(5) 0.061(3) Uani 1 1 d . . . H69A H 0.9632 0.7551 0.4616 0.073 Uiso 1 1 calc R . . C12 C 0.2779(11) 0.9486(7) 0.4030(6) 0.091(4) Uani 1 1 d . . . H71A H 0.2211 0.9172 0.4153 0.137 Uiso 1 1 calc R . . H71B H 0.2513 0.9462 0.3598 0.137 Uiso 1 1 calc R . . H71C H 0.2858 1.0070 0.4262 0.137 Uiso 1 1 calc R . . C75 C 0.3051(11) 0.9391(8) 0.2040(5) 0.097(4) Uani 1 1 d . . . H79A H 0.3367 0.9805 0.2422 0.146 Uiso 1 1 calc R . . H79B H 0.2242 0.9500 0.1876 0.146 Uiso 1 1 calc R . . H79C H 0.3517 0.9431 0.1751 0.146 Uiso 1 1 calc R . . C62 C -0.0015(9) 0.7661(9) 0.3176(5) 0.103(5) Uani 1 1 d . . . H81A H -0.0226 0.7775 0.2775 0.155 Uiso 1 1 calc R . . H81B H -0.0225 0.8124 0.3472 0.155 Uiso 1 1 calc R . . H81C H -0.0435 0.7142 0.3168 0.155 Uiso 1 1 calc R . . C42 C 0.6284(13) 0.6629(10) 0.2480(6) 0.125(5) Uani 1 1 d . . . H98A H 0.5649 0.6192 0.2360 0.187 Uiso 1 1 calc R . . H98B H 0.6890 0.6518 0.2810 0.187 Uiso 1 1 calc R . . H98C H 0.6615 0.6630 0.2134 0.187 Uiso 1 1 calc R . . Zn1A Zn 0.84876(11) 0.22832(8) 0.10888(6) 0.0655(5) Uani 1 1 d . . . Al1A Al 0.6102(3) 0.2292(2) 0.14933(15) 0.0595(10) Uani 1 1 d . . . Al2A Al 0.8221(3) 0.2117(2) 0.23775(15) 0.0581(10) Uani 1 1 d . . . O2A O 0.7418(6) 0.2968(4) 0.2044(3) 0.0591(19) Uani 1 1 d . . . O1A O 0.7122(5) 0.1460(4) 0.1690(3) 0.0515(18) Uani 1 1 d . . . O9A O 0.8962(7) 0.1442(5) 0.0410(3) 0.075(2) Uani 1 1 d . . . O8A O 0.8862(7) 0.1195(4) 0.2675(4) 0.066(2) Uani 1 1 d . . . O3A O 0.6779(6) 0.2305(4) 0.0849(3) 0.063(2) Uani 1 1 d . . . O10A O 0.9247(7) 0.3261(4) 0.0910(4) 0.075(2) Uani 1 1 d . . . O11A O 0.5428(6) 0.2267(5) 0.2189(4) 0.070(2) Uani 1 1 d . . . O5A O 0.4831(7) 0.1531(4) 0.1021(3) 0.065(2) Uani 1 1 d . . . O4A O 0.9285(6) 0.2121(4) 0.1893(3) 0.0568(19) Uani 1 1 d . . . O7A O 0.9195(7) 0.2872(5) 0.3071(4) 0.071(2) Uani 1 1 d . . . C61A C 0.5971(13) 0.2187(7) 0.2714(6) 0.066(3) Uani 1 1 d . . . O12A O 0.7062(7) 0.2123(5) 0.2879(3) 0.068(2) Uani 1 1 d . . . O6A O 0.5176(8) 0.3208(4) 0.1400(3) 0.071(2) Uani 1 1 d . . . C3A C 0.6079(11) 0.2340(8) 0.0242(6) 0.086(4) Uani 1 1 d . . . H29A H 0.5265 0.2449 0.0279 0.103 Uiso 1 1 calc R . . C4A C 1.0543(11) 0.2060(8) 0.2077(6) 0.083(4) Uani 1 1 d . . . H30A H 1.0709 0.1996 0.2501 0.099 Uiso 1 1 calc R . . C92A C 0.9764(10) 0.3198(9) 0.0468(7) 0.078(4) Uani 1 1 d . . . C93A C 0.9844(10) 0.2435(10) 0.0047(6) 0.076(4) Uani 1 1 d . . . H37A H 1.0200 0.2482 -0.0268 0.091 Uiso 1 1 calc R . . C72A C 0.9885(10) 0.2697(10) 0.3539(6) 0.070(4) Uani 1 1 d . . . C74A C 0.9567(11) 0.1148(10) 0.3175(7) 0.069(4) Uani 1 1 d . . . C94A C 0.9469(10) 0.1628(9) 0.0036(6) 0.073(4) Uani 1 1 d . . . C52A C 0.3743(14) 0.1684(10) 0.0867(5) 0.076(4) Uani 1 1 d . . . C95A C 0.9647(11) 0.0912(8) -0.0472(5) 0.095(4) Uani 1 1 d . . . H49A H 0.9318 0.0388 -0.0432 0.142 Uiso 1 1 calc R . . H49B H 1.0482 0.0872 -0.0450 0.142 Uiso 1 1 calc R . . H49C H 0.9255 0.1016 -0.0861 0.142 Uiso 1 1 calc R . . C53A C 0.3341(12) 0.2471(12) 0.0949(6) 0.089(4) Uani 1 1 d . . . H50A H 0.2528 0.2520 0.0821 0.107 Uiso 1 1 calc R . . C73A C 1.0061(11) 0.1872(11) 0.3616(6) 0.081(4) Uani 1 1 d . . . H53A H 1.0539 0.1810 0.3986 0.097 Uiso 1 1 calc R . . C1A C 0.6917(10) 0.0573(8) 0.1454(6) 0.078(4) Uani 1 1 d . . . H55A H 0.6292 0.0543 0.1080 0.094 Uiso 1 1 calc R . . C54A C 0.4072(14) 0.3216(11) 0.1214(6) 0.082(4) Uani 1 1 d . . . C2A C 0.7518(11) 0.3880(8) 0.2262(6) 0.089(4) Uani 1 1 d . . . H58A H 0.6955 0.4040 0.1923 0.106 Uiso 1 1 calc R . . C21A C 0.6921(12) 0.4167(7) 0.2768(6) 0.106(5) Uani 1 1 d . . . H60A H 0.6133 0.3896 0.2652 0.160 Uiso 1 1 calc R . . H60B H 0.6875 0.4775 0.2851 0.160 Uiso 1 1 calc R . . H60C H 0.7366 0.4017 0.3131 0.160 Uiso 1 1 calc R . . C71A C 1.0515(10) 0.3473(8) 0.4025(5) 0.093(4) Uani 1 1 d . . . H63A H 1.0296 0.3980 0.3889 0.140 Uiso 1 1 calc R . . H63B H 1.1360 0.3434 0.4089 0.140 Uiso 1 1 calc R . . H63C H 1.0288 0.3497 0.4404 0.140 Uiso 1 1 calc R . . C51A C 0.2890(11) 0.0908(9) 0.0555(6) 0.116(5) Uani 1 1 d . . . H66A H 0.3322 0.0401 0.0536 0.174 Uiso 1 1 calc R . . H66B H 0.2506 0.0941 0.0145 0.174 Uiso 1 1 calc R . . H66C H 0.2302 0.0888 0.0786 0.174 Uiso 1 1 calc R . . C91A C 1.0240(11) 0.4046(7) 0.0411(6) 0.102(5) Uani 1 1 d . . . H67A H 1.0096 0.4497 0.0737 0.153 Uiso 1 1 calc R . . H67B H 0.9845 0.4144 0.0020 0.153 Uiso 1 1 calc R . . H67C H 1.1079 0.4032 0.0439 0.153 Uiso 1 1 calc R . . C42A C 1.1249(13) 0.2835(10) 0.2098(8) 0.160(8) Uani 1 1 d . . . H76A H 1.1007 0.3319 0.2365 0.240 Uiso 1 1 calc R . . H76B H 1.1122 0.2925 0.1691 0.240 Uiso 1 1 calc R . . H76C H 1.2078 0.2767 0.2252 0.240 Uiso 1 1 calc R . . C75A C 0.9848(11) 0.0297(8) 0.3264(5) 0.097(4) Uani 1 1 d . . . H78A H 0.9419 -0.0129 0.2912 0.146 Uiso 1 1 calc R . . H78B H 0.9623 0.0226 0.3627 0.146 Uiso 1 1 calc R . . H78C H 1.0687 0.0237 0.3312 0.146 Uiso 1 1 calc R . . C41A C 1.0948(13) 0.1287(10) 0.1709(7) 0.150(6) Uani 1 1 d . . . H82A H 1.1788 0.1259 0.1860 0.225 Uiso 1 1 calc R . . H82B H 1.0783 0.1311 0.1285 0.225 Uiso 1 1 calc R . . H82C H 1.0536 0.0789 0.1742 0.225 Uiso 1 1 calc R . . C62A C 0.5212(11) 0.2164(10) 0.3155(5) 0.120(5) Uani 1 1 d . . . H83A H 0.5701 0.2102 0.3538 0.180 Uiso 1 1 calc R . . H83B H 0.4630 0.1691 0.2985 0.180 Uiso 1 1 calc R . . H83C H 0.4817 0.2686 0.3225 0.180 Uiso 1 1 calc R . . C12A C 0.6252(11) 0.0169(7) 0.1825(6) 0.100(4) Uani 1 1 d . . . H85A H 0.5604 0.0507 0.1909 0.150 Uiso 1 1 calc R . . H85B H 0.6784 0.0142 0.2207 0.150 Uiso 1 1 calc R . . H85C H 0.5947 -0.0397 0.1594 0.150 Uiso 1 1 calc R . . C32A C 0.6536(13) 0.3067(11) 0.0059(7) 0.160(8) Uani 1 1 d . . . H88A H 0.6507 0.3585 0.0362 0.239 Uiso 1 1 calc R . . H88B H 0.6055 0.3103 -0.0333 0.239 Uiso 1 1 calc R . . H88C H 0.7343 0.2989 0.0030 0.239 Uiso 1 1 calc R . . C11A C 0.770(2) 0.0133(10) 0.1231(9) 0.233(13) Uani 1 1 d . . . H90A H 0.8026 0.0433 0.0984 0.349 Uiso 1 1 calc R . . H90B H 0.7343 -0.0410 0.0979 0.349 Uiso 1 1 calc R . . H90C H 0.8331 0.0047 0.1561 0.349 Uiso 1 1 calc R . . C22A C 0.854(2) 0.4304(10) 0.2257(10) 0.253(14) Uani 1 1 d . . . H94A H 0.8752 0.4077 0.1874 0.379 Uiso 1 1 calc R . . H94B H 0.9166 0.4233 0.2592 0.379 Uiso 1 1 calc R . . H94C H 0.8412 0.4900 0.2302 0.379 Uiso 1 1 calc R . . C55A C 0.3560(13) 0.4065(9) 0.1304(8) 0.151(7) Uani 1 1 d . . . H95A H 0.4184 0.4501 0.1512 0.226 Uiso 1 1 calc R . . H95B H 0.2986 0.4080 0.1547 0.226 Uiso 1 1 calc R . . H95C H 0.3180 0.4161 0.0910 0.226 Uiso 1 1 calc R . . C22 C 0.4237(13) 0.5281(8) 0.3522(7) 0.128(5) Uani 1 1 d . . . H10A H 0.5039 0.5518 0.3612 0.192 Uiso 1 1 calc R . . H10B H 0.4174 0.4712 0.3266 0.192 Uiso 1 1 calc R . . H10C H 0.4028 0.5266 0.3900 0.192 Uiso 1 1 calc R . . C31A C 0.6029(14) 0.1465(11) -0.0217(6) 0.160(7) Uani 1 1 d . . . H10D H 0.5734 0.1030 -0.0058 0.239 Uiso 1 1 calc R . . H10E H 0.6813 0.1345 -0.0272 0.239 Uiso 1 1 calc R . . H10F H 0.5511 0.1475 -0.0606 0.239 Uiso 1 1 calc R . . C201 C 0.0753(19) 0.3282(15) -0.1472(9) 0.187(8) Uiso 1 1 d . . . H20A H -0.0012 0.3321 -0.1699 0.224 Uiso 1 1 calc R . . C205 C 0.204(3) 0.2401(18) -0.1112(13) 0.241(11) Uiso 1 1 d . . . H205 H 0.2259 0.1850 -0.1108 0.289 Uiso 1 1 calc R . . C203 C 0.1398(19) 0.4059(16) -0.1226(10) 0.210(9) Uiso 1 1 d D . . H20D H 0.1195 0.4592 -0.1289 0.251 Uiso 1 1 calc R . . C204 C 0.252(2) 0.3827(18) -0.0829(12) 0.220(10) Uiso 1 1 d . . . C207 C 0.328(3) 0.446(2) -0.0590(18) 0.46(3) Uiso 1 1 d D . . H20E H 0.2954 0.4959 -0.0699 0.684 Uiso 1 1 calc R . . H20F H 0.3983 0.4340 -0.0740 0.684 Uiso 1 1 calc R . . H20G H 0.3476 0.4549 -0.0149 0.684 Uiso 1 1 calc R . . C206 C 0.101(2) 0.2500(15) -0.1447(10) 0.189(8) Uiso 1 1 d . . . H20H H 0.0473 0.2037 -0.1661 0.227 Uiso 1 1 calc R . . C202 C 0.276(2) 0.3026(15) -0.0786(10) 0.198(9) Uiso 1 1 d D . . H20I H 0.3460 0.2931 -0.0522 0.238 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 Zn1 0.0508(9) 0.0663(10) 0.0596(9) 0.0114(7) 0.0187(7) 0.0003(7) Al1 0.051(2) 0.054(2) 0.048(2) 0.0094(17) 0.0207(17) 0.0020(16) Al2 0.054(2) 0.061(2) 0.046(2) 0.0094(17) 0.0174(17) 0.0008(17) O1 0.059(5) 0.046(5) 0.050(5) 0.004(4) 0.021(4) -0.002(4) O2 0.075(5) 0.040(5) 0.043(4) 0.006(4) 0.025(4) -0.003(4) O5 0.068(5) 0.063(5) 0.039(4) 0.004(4) 0.025(4) -0.002(4) O3 0.048(5) 0.073(5) 0.040(5) 0.010(4) 0.013(4) -0.005(4) O6 0.056(5) 0.059(5) 0.064(5) 0.021(4) 0.016(4) 0.002(4) O9 0.072(6) 0.064(5) 0.071(6) 0.004(4) 0.027(5) -0.010(5) O7 0.076(6) 0.081(6) 0.033(5) 0.001(4) 0.020(4) 0.006(4) O11 0.047(5) 0.072(5) 0.054(5) 0.014(4) 0.024(4) 0.003(4) O8 0.065(5) 0.073(5) 0.066(6) 0.025(5) 0.031(5) 0.009(4) O10 0.049(5) 0.071(5) 0.071(6) 0.010(4) 0.008(4) -0.011(4) O4 0.048(5) 0.093(6) 0.051(5) 0.021(4) 0.033(4) 0.004(4) O12 0.042(5) 0.085(6) 0.051(5) 0.021(4) 0.006(4) 0.001(4) C94 0.053(9) 0.078(11) 0.058(8) 0.015(7) 0.025(7) 0.005(9) C4 0.083(10) 0.093(11) 0.067(9) 0.020(8) 0.023(8) 0.013(9) C61 0.050(9) 0.095(9) 0.038(8) 0.021(7) 0.010(7) -0.009(6) C54 0.049(8) 0.074(10) 0.067(9) 0.014(8) 0.016(7) -0.006(7) C52 0.060(8) 0.084(11) 0.037(8) 0.006(7) 0.016(6) 0.002(7) C92 0.066(9) 0.054(9) 0.045(7) 0.013(6) 0.031(7) 0.013(8) C3 0.046(7) 0.072(9) 0.052(8) 0.011(7) 0.016(6) 0.012(7) C31 0.113(11) 0.104(10) 0.049(8) -0.009(7) 0.011(8) -0.043(9) C74 0.068(9) 0.085(12) 0.076(11) 0.021(10) 0.038(9) 0.006(8) C53 0.071(9) 0.061(9) 0.055(8) 0.006(7) 0.020(7) -0.006(7) C72 0.070(9) 0.100(12) 0.035(9) 0.017(9) 0.019(7) -0.002(7) C73 0.083(10) 0.104(12) 0.060(10) 0.037(10) 0.013(8) 0.010(9) C51 0.109(11) 0.090(10) 0.068(9) 0.000(8) 0.046(8) 0.014(8) C1 0.065(9) 0.065(9) 0.069(8) 0.000(7) 0.030(7) -0.013(7) C91 0.064(9) 0.084(10) 0.106(11) 0.020(8) 0.022(8) 0.016(7) C32 0.123(12) 0.101(11) 0.098(11) 0.036(9) 0.043(9) 0.043(9) C41 0.091(11) 0.154(14) 0.121(13) 0.036(11) 0.053(9) -0.036(10) C55 0.102(10) 0.076(10) 0.124(12) 0.045(9) 0.051(9) 0.002(8) C2 0.078(10) 0.060(10) 0.095(10) 0.024(8) 0.005(8) -0.003(8) C21 0.122(13) 0.079(10) 0.119(12) 0.002(8) 0.020(10) -0.034(9) C11 0.077(9) 0.056(8) 0.096(10) 0.015(7) 0.031(8) 0.006(7) C71 0.159(14) 0.101(11) 0.052(9) 0.005(9) 0.025(9) -0.017(10) C95 0.067(9) 0.082(10) 0.122(12) 0.011(9) -0.003(8) -0.037(8) C93 0.052(8) 0.081(10) 0.056(8) 0.025(8) 0.016(6) 0.008(8) C12 0.097(11) 0.056(8) 0.130(12) 0.020(8) 0.048(9) 0.031(7) C75 0.122(12) 0.081(11) 0.080(10) 0.022(8) 0.005(8) -0.003(8) C62 0.040(9) 0.204(15) 0.089(10) 0.067(10) 0.026(7) 0.034(8) C42 0.134(14) 0.151(15) 0.104(12) 0.023(10) 0.065(11) 0.040(11) Zn1A 0.0663(10) 0.0738(10) 0.0581(9) 0.0098(8) 0.0252(8) 0.0027(7) Al1A 0.058(2) 0.068(2) 0.049(2) 0.0058(18) 0.0158(18) 0.0061(19) Al2A 0.056(2) 0.066(2) 0.051(2) 0.0051(19) 0.0176(19) 0.0053(18) O2A 0.059(5) 0.050(5) 0.055(5) -0.002(4) 0.004(4) -0.004(4) O1A 0.057(5) 0.050(5) 0.041(4) -0.001(4) 0.012(4) -0.006(4) O9A 0.089(6) 0.078(6) 0.063(6) 0.004(4) 0.040(5) 0.016(5) O8A 0.067(6) 0.065(5) 0.056(5) 0.000(4) 0.010(5) 0.004(4) O3A 0.057(5) 0.079(5) 0.050(5) 0.009(4) 0.016(4) 0.003(4) O10A 0.086(6) 0.065(6) 0.077(6) 0.005(4) 0.038(5) -0.006(4) O11A 0.046(5) 0.098(6) 0.058(6) 0.001(5) 0.013(4) 0.007(4) O5A 0.059(6) 0.084(6) 0.053(5) 0.005(4) 0.024(4) 0.001(5) O4A 0.049(5) 0.072(5) 0.055(5) 0.016(4) 0.024(4) 0.011(4) O7A 0.066(6) 0.083(6) 0.052(5) -0.005(5) 0.010(5) 0.005(4) C61A 0.065(10) 0.082(9) 0.046(9) 0.002(7) 0.015(9) 0.017(7) O12A 0.052(5) 0.105(6) 0.046(5) 0.013(4) 0.015(4) 0.016(5) O6A 0.069(6) 0.079(6) 0.058(5) 0.012(4) 0.007(5) 0.014(5) C3A 0.078(10) 0.106(12) 0.073(10) 0.016(9) 0.022(9) 0.001(8) C4A 0.073(10) 0.098(11) 0.095(10) 0.030(8) 0.049(9) 0.030(8) C92A 0.057(9) 0.078(11) 0.095(11) 0.022(9) 0.008(8) -0.004(8) C93A 0.076(10) 0.090(11) 0.078(10) 0.029(9) 0.044(8) 0.013(8) C72A 0.040(8) 0.119(13) 0.038(9) 0.001(9) 0.005(7) -0.004(8) C74A 0.057(9) 0.098(12) 0.055(10) 0.017(9) 0.022(8) 0.012(8) C94A 0.067(9) 0.076(11) 0.074(10) 0.000(8) 0.032(8) 0.009(7) C52A 0.069(11) 0.103(13) 0.060(9) 0.012(8) 0.034(9) 0.003(10) C95A 0.098(11) 0.118(12) 0.065(9) 0.011(8) 0.027(8) 0.009(8) C53A 0.061(10) 0.118(14) 0.084(11) 0.011(10) 0.023(8) 0.022(11) C73A 0.065(9) 0.114(13) 0.070(11) 0.035(11) 0.012(8) 0.028(9) C1A 0.070(9) 0.077(11) 0.078(9) -0.016(8) 0.035(7) 0.012(8) C54A 0.052(10) 0.117(14) 0.069(10) 0.021(9) -0.001(8) 0.020(10) C2A 0.088(10) 0.070(11) 0.097(11) -0.002(9) 0.027(9) -0.026(8) C21A 0.126(12) 0.073(10) 0.116(12) -0.015(8) 0.060(10) 0.014(8) C71A 0.074(9) 0.118(12) 0.065(9) -0.004(9) 0.000(7) -0.010(8) C51A 0.066(9) 0.135(13) 0.115(12) -0.019(10) 0.009(8) -0.030(10) C91A 0.122(12) 0.081(10) 0.127(12) 0.039(9) 0.063(10) -0.005(8) C42A 0.091(12) 0.160(16) 0.24(2) 0.099(15) 0.011(12) -0.040(11) C75A 0.133(12) 0.077(10) 0.089(10) 0.028(8) 0.035(9) 0.036(9) C41A 0.098(13) 0.186(17) 0.151(15) 0.001(13) 0.038(11) 0.063(12) C62A 0.078(10) 0.239(18) 0.057(9) 0.043(10) 0.037(8) 0.021(10) C12A 0.127(12) 0.067(9) 0.115(11) 0.011(8) 0.061(10) -0.017(8) C32A 0.121(14) 0.23(2) 0.155(16) 0.144(16) -0.009(11) -0.013(13) C11A 0.42(4) 0.079(13) 0.26(2) -0.009(13) 0.27(3) -0.024(17) C22A 0.44(4) 0.087(14) 0.30(3) -0.020(15) 0.28(3) -0.039(18) C55A 0.121(14) 0.113(14) 0.196(18) 0.033(12) -0.005(12) 0.052(11) C22 0.130(14) 0.083(11) 0.155(15) 0.009(11) 0.022(12) 0.010(10) C31A 0.150(16) 0.22(2) 0.062(10) -0.037(12) 0.002(10) 0.046(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O4 1.936(7) . ? Zn1 O3 1.958(6) . ? Zn1 O10 1.969(8) . ? Zn1 O9 1.996(7) . ? Al1 O3 1.842(7) . ? Al1 O2 1.857(7) . ? Al1 O1 1.871(6) . ? Al1 O6 1.876(7) . ? Al1 O5 1.893(7) . ? Al1 O11 1.941(8) . ? Al1 Al2 2.857(4) . ? Al2 O4 1.854(7) . ? Al2 O8 1.866(8) . ? Al2 O1 1.872(7) . ? Al2 O2 1.881(7) . ? Al2 O7 1.900(7) . ? Al2 O12 1.948(7) . ? O1 C1 1.459(11) . ? O2 C2 1.419(12) . ? O5 C52 1.276(11) . ? O3 C3 1.418(11) . ? O6 C54 1.278(12) . ? O9 C94 1.284(12) . ? O7 C72 1.255(12) . ? O11 C61 1.240(11) . ? O8 C74 1.282(13) . ? O10 C92 1.251(12) . ? O4 C4 1.406(12) . ? O12 C61 1.280(11) . ? C94 C93 1.336(14) . ? C94 C95 1.491(14) . ? C4 C42 1.466(15) . ? C4 C41 1.497(15) . ? C61 C62 1.507(14) . ? C54 C53 1.356(14) . ? C54 C55 1.494(14) . ? C52 C53 1.390(14) . ? C52 C51 1.504(14) . ? C92 C93 1.433(14) . ? C92 C91 1.484(13) . ? C3 C31 1.486(13) . ? C3 C32 1.505(13) . ? C74 C73 1.359(15) . ? C74 C75 1.490(15) . ? C72 C73 1.386(15) . ? C72 C71 1.499(15) . ? C1 C11 1.485(12) . ? C1 C12 1.509(14) . ? C2 C22 1.417(15) . ? C2 C21 1.523(15) . ? Zn1A O3A 1.931(7) . ? Zn1A O4A 1.947(6) . ? Zn1A O10A 1.975(7) . ? Zn1A O9A 1.997(7) . ? Al1A O3A 1.835(7) . ? Al1A O5A 1.860(8) . ? Al1A O6A 1.860(8) . ? Al1A O1A 1.864(7) . ? Al1A O2A 1.885(7) . ? Al1A O11A 1.945(8) . ? Al1A Al2A 2.867(5) . ? Al2A O4A 1.844(7) . ? Al2A O1A 1.872(7) . ? Al2A O8A 1.873(8) . ? Al2A O7A 1.879(8) . ? Al2A O2A 1.881(7) . ? Al2A O12A 1.960(8) . ? O2A C2A 1.434(12) . ? O1A C1A 1.405(12) . ? O9A C94A 1.236(13) . ? O8A C74A 1.268(13) . ? O3A C3A 1.458(13) . ? O10A C92A 1.278(14) . ? O11A C61A 1.263(12) . ? O5A C52A 1.272(14) . ? O4A C4A 1.432(12) . ? O7A C72A 1.277(13) . ? C61A O12A 1.246(13) . ? C61A C62A 1.494(14) . ? O6A C54A 1.253(13) . ? C3A C32A 1.472(16) . ? C3A C31A 1.543(16) . ? C4A C42A 1.478(15) . ? C4A C41A 1.480(16) . ? C92A C93A 1.394(16) . ? C92A C91A 1.519(14) . ? C93A C94A 1.365(15) . ? C72A C73A 1.397(16) . ? C72A C71A 1.518(15) . ? C74A C73A 1.373(16) . ? C74A C75A 1.466(15) . ? C94A C95A 1.489(15) . ? C52A C53A 1.342(16) . ? C52A C51A 1.515(16) . ? C53A C54A 1.393(17) . ? C1A C11A 1.287(18) . ? C1A C12A 1.520(14) . ? C54A C55A 1.486(17) . ? C2A C22A 1.364(19) . ? C2A C21A 1.473(15) . ? C201 C206 1.31(2) . ? C201 C203 1.38(2) . ? C205 C202 1.27(3) . ? C205 C206 1.30(3) . ? C203 C204 1.51(3) . ? C204 C207 1.27(4) . ? C204 C202 1.35(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 O4 Zn1 O3 122.2(3) . . ? O4 Zn1 O10 111.1(3) . . ? O3 Zn1 O10 108.1(3) . . ? O4 Zn1 O9 108.6(3) . . ? O3 Zn1 O9 110.1(3) . . ? O10 Zn1 O9 92.9(3) . . ? O3 Al1 O2 90.0(3) . . ? O3 Al1 O1 88.7(3) . . ? O2 Al1 O1 78.9(3) . . ? O3 Al1 O6 92.9(3) . . ? O2 Al1 O6 97.6(3) . . ? O1 Al1 O6 176.2(3) . . ? O3 Al1 O5 93.8(3) . . ? O2 Al1 O5 172.0(3) . . ? O1 Al1 O5 94.1(3) . . ? O6 Al1 O5 89.3(3) . . ? O3 Al1 O11 179.1(3) . . ? O2 Al1 O11 89.5(3) . . ? O1 Al1 O11 90.4(3) . . ? O6 Al1 O11 88.0(3) . . ? O5 Al1 O11 86.6(3) . . ? O3 Al1 Al2 98.5(2) . . ? O2 Al1 Al2 40.5(2) . . ? O1 Al1 Al2 40.3(2) . . ? O6 Al1 Al2 135.9(3) . . ? O5 Al1 Al2 131.8(2) . . ? O11 Al1 Al2 80.6(2) . . ? O4 Al2 O8 94.4(3) . . ? O4 Al2 O1 89.6(3) . . ? O8 Al2 O1 95.9(3) . . ? O4 Al2 O2 89.6(3) . . ? O8 Al2 O2 173.0(3) . . ? O1 Al2 O2 78.3(3) . . ? O4 Al2 O7 95.1(3) . . ? O8 Al2 O7 89.8(4) . . ? O1 Al2 O7 172.3(3) . . ? O2 Al2 O7 95.5(3) . . ? O4 Al2 O12 179.5(3) . . ? O8 Al2 O12 86.0(3) . . ? O1 Al2 O12 90.1(3) . . ? O2 Al2 O12 90.0(3) . . ? O7 Al2 O12 85.3(3) . . ? O4 Al2 Al1 98.7(2) . . ? O8 Al2 Al1 133.5(3) . . ? O1 Al2 Al1 40.2(2) . . ? O2 Al2 Al1 39.9(2) . . ? O7 Al2 Al1 132.6(3) . . ? O12 Al2 Al1 80.9(2) . . ? C1 O1 Al1 125.4(6) . . ? C1 O1 Al2 132.5(6) . . ? Al1 O1 Al2 99.5(3) . . ? C2 O2 Al1 132.8(6) . . ? C2 O2 Al2 126.4(6) . . ? Al1 O2 Al2 99.7(3) . . ? C52 O5 Al1 128.8(7) . . ? C3 O3 Al1 125.4(6) . . ? C3 O3 Zn1 124.2(6) . . ? Al1 O3 Zn1 110.2(3) . . ? C54 O6 Al1 129.9(7) . . ? C94 O9 Zn1 123.7(7) . . ? C72 O7 Al2 127.5(8) . . ? C61 O11 Al1 127.7(7) . . ? C74 O8 Al2 129.2(8) . . ? C92 O10 Zn1 125.4(7) . . ? C4 O4 Al2 123.9(7) . . ? C4 O4 Zn1 126.1(7) . . ? Al2 O4 Zn1 110.0(3) . . ? C61 O12 Al2 126.1(7) . . ? O9 C94 C93 125.9(12) . . ? O9 C94 C95 113.5(11) . . ? C93 C94 C95 120.5(12) . . ? O4 C4 C42 112.3(10) . . ? O4 C4 C41 111.5(10) . . ? C42 C4 C41 114.1(12) . . ? O11 C61 O12 124.6(10) . . ? O11 C61 C62 118.7(10) . . ? O12 C61 C62 116.7(10) . . ? O6 C54 C53 124.3(11) . . ? O6 C54 C55 115.3(11) . . ? C53 C54 C55 120.3(12) . . ? O5 C52 C53 123.9(10) . . ? O5 C52 C51 113.7(10) . . ? C53 C52 C51 122.3(11) . . ? O10 C92 C93 124.6(10) . . ? O10 C92 C91 118.1(11) . . ? C93 C92 C91 117.4(11) . . ? O3 C3 C31 114.3(9) . . ? O3 C3 C32 111.1(9) . . ? C31 C3 C32 111.3(10) . . ? O8 C74 C73 123.6(12) . . ? O8 C74 C75 115.6(13) . . ? C73 C74 C75 120.7(14) . . ? C54 C53 C52 122.4(11) . . ? O7 C72 C73 125.0(12) . . ? O7 C72 C71 114.5(12) . . ? C73 C72 C71 120.5(12) . . ? C74 C73 C72 122.7(12) . . ? O1 C1 C11 113.4(8) . . ? O1 C1 C12 111.1(9) . . ? C11 C1 C12 113.5(9) . . ? C22 C2 O2 117.4(11) . . ? C22 C2 C21 115.5(11) . . ? O2 C2 C21 110.8(10) . . ? C94 C93 C92 127.1(11) . . ? O3A Zn1A O4A 121.3(3) . . ? O3A Zn1A O10A 109.9(3) . . ? O4A Zn1A O10A 111.1(3) . . ? O3A Zn1A O9A 106.6(3) . . ? O4A Zn1A O9A 111.4(3) . . ? O10A Zn1A O9A 92.9(3) . . ? O3A Al1A O5A 95.0(3) . . ? O3A Al1A O6A 95.1(3) . . ? O5A Al1A O6A 90.4(4) . . ? O3A Al1A O1A 88.7(3) . . ? O5A Al1A O1A 95.7(3) . . ? O6A Al1A O1A 172.4(4) . . ? O3A Al1A O2A 89.9(3) . . ? O5A Al1A O2A 172.5(4) . . ? O6A Al1A O2A 94.8(4) . . ? O1A Al1A O2A 78.6(3) . . ? O3A Al1A O11A 178.3(4) . . ? O5A Al1A O11A 86.0(3) . . ? O6A Al1A O11A 86.3(3) . . ? O1A Al1A O11A 89.8(3) . . ? O2A Al1A O11A 89.0(3) . . ? O3A Al1A Al2A 98.0(3) . . ? O5A Al1A Al2A 132.9(3) . . ? O6A Al1A Al2A 132.7(3) . . ? O1A Al1A Al2A 40.0(2) . . ? O2A Al1A Al2A 40.4(2) . . ? O11A Al1A Al2A 80.3(3) . . ? O4A Al2A O1A 89.3(3) . . ? O4A Al2A O8A 94.0(3) . . ? O1A Al2A O8A 96.0(3) . . ? O4A Al2A O7A 93.9(3) . . ? O1A Al2A O7A 173.4(4) . . ? O8A Al2A O7A 89.5(4) . . ? O4A Al2A O2A 89.2(3) . . ? O1A Al2A O2A 78.6(3) . . ? O8A Al2A O2A 173.7(4) . . ? O7A Al2A O2A 95.7(3) . . ? O4A Al2A O12A 178.7(4) . . ? O1A Al2A O12A 89.9(3) . . ? O8A Al2A O12A 87.1(3) . . ? O7A Al2A O12A 86.8(3) . . ? O2A Al2A O12A 89.7(3) . . ? O4A Al2A Al1A 98.0(3) . . ? O1A Al2A Al1A 39.8(2) . . ? O8A Al2A Al1A 133.5(3) . . ? O7A Al2A Al1A 133.9(3) . . ? O2A Al2A Al1A 40.5(2) . . ? O12A Al2A Al1A 80.8(3) . . ? C2A O2A Al2A 131.2(7) . . ? C2A O2A Al1A 126.9(7) . . ? Al2A O2A Al1A 99.2(3) . . ? C1A O1A Al1A 126.7(6) . . ? C1A O1A Al2A 131.7(7) . . ? Al1A O1A Al2A 100.3(3) . . ? C94A O9A Zn1A 125.0(8) . . ? C74A O8A Al2A 132.7(8) . . ? C3A O3A Al1A 122.5(7) . . ? C3A O3A Zn1A 126.1(6) . . ? Al1A O3A Zn1A 111.4(4) . . ? C92A O10A Zn1A 124.0(8) . . ? C61A O11A Al1A 127.4(7) . . ? C52A O5A Al1A 127.8(8) . . ? C4A O4A Al2A 126.0(6) . . ? C4A O4A Zn1A 123.0(6) . . ? Al2A O4A Zn1A 111.0(4) . . ? C72A O7A Al2A 128.3(8) . . ? O12A C61A O11A 125.0(11) . . ? O12A C61A C62A 119.4(11) . . ? O11A C61A C62A 115.6(12) . . ? C61A O12A Al2A 126.5(7) . . ? C54A O6A Al1A 129.4(9) . . ? O3A C3A C32A 109.6(11) . . ? O3A C3A C31A 109.7(10) . . ? C32A C3A C31A 115.3(13) . . ? O4A C4A C42A 113.8(10) . . ? O4A C4A C41A 112.4(11) . . ? C42A C4A C41A 111.4(12) . . ? O10A C92A C93A 124.3(11) . . ? O10A C92A C91A 114.1(12) . . ? C93A C92A C91A 121.5(13) . . ? C94A C93A C92A 128.6(11) . . ? O7A C72A C73A 124.6(12) . . ? O7A C72A C71A 114.1(13) . . ? C73A C72A C71A 121.3(13) . . ? O8A C74A C73A 120.9(12) . . ? O8A C74A C75A 117.9(13) . . ? C73A C74A C75A 121.2(13) . . ? O9A C94A C93A 124.9(11) . . ? O9A C94A C95A 116.8(12) . . ? C93A C94A C95A 118.3(13) . . ? O5A C52A C53A 124.2(13) . . ? O5A C52A C51A 115.4(13) . . ? C53A C52A C51A 120.4(15) . . ? C52A C53A C54A 123.9(14) . . ? C74A C73A C72A 123.5(12) . . ? C11A C1A O1A 120.3(12) . . ? C11A C1A C12A 116.8(13) . . ? O1A C1A C12A 112.1(9) . . ? O6A C54A C53A 122.2(13) . . ? O6A C54A C55A 116.9(15) . . ? C53A C54A C55A 120.9(14) . . ? C22A C2A O2A 117.8(12) . . ? C22A C2A C21A 120.4(13) . . ? O2A C2A C21A 111.7(10) . . ? C206 C201 C203 133(2) . . ? C202 C205 C206 123(3) . . ? C201 C203 C204 103(2) . . ? C207 C204 C202 122(2) . . ? C207 C204 C203 112(2) . . ? C202 C204 C203 125(3) . . ? C205 C206 C201 117(3) . . ? C205 C202 C204 120(3) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 20.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.470 _refine_diff_density_min -0.534 _refine_diff_density_rms 0.073 data_coalnw10 _database_code_depnum_ccdc_archive 'CCDC 200110' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32.50 H56 Al2 Co O12' _chemical_formula_weight 751.66 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 '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 11.871(4) _cell_length_b 16.611(6) _cell_length_c 23.617(9) _cell_angle_alpha 103.292(13) _cell_angle_beta 103.795(12) _cell_angle_gamma 90.052(10) _cell_volume 4394(3) _cell_formula_units_Z 4 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 996(I>2sigma(I)) _cell_measurement_theta_min 1.26 _cell_measurement_theta_max 20.00 _exptl_crystal_description plate _exptl_crystal_colour 'bluish violet' _exptl_crystal_size_max 0.65 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.136 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1600 _exptl_absorpt_coefficient_mu 0.479 _exptl_absorpt_correction_type 'not applied' _exptl_absorpt_correction_T_min 0.7458 _exptl_absorpt_correction_T_max 0.9102 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(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 'Bruker SMART CCD 1k' _diffrn_measurement_method 'Bruker SMART' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6458 _diffrn_reflns_av_R_equivalents 0.0712 _diffrn_reflns_av_sigmaI/netI 0.0512 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.26 _diffrn_reflns_theta_max 20.00 _reflns_number_total 6454 _reflns_number_gt 4287 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINTPLUS' _computing_data_reduction 'Bruker SAINTPLUS' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL-NT' _computing_publication_material 'Bruker SHELXTL-NT' _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^)+(0.0870P)^2^+26.8129P] 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 6454 _refine_ls_number_parameters 821 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1344 _refine_ls_R_factor_gt 0.0857 _refine_ls_wR_factor_ref 0.2226 _refine_ls_wR_factor_gt 0.2008 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.053 _refine_ls_shift/su_max 0.006 _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 Co1 Co 0.59364(13) 0.74142(11) 0.39886(7) 0.0571(6) Uani 1 1 d . . . Al1 Al 0.3427(3) 0.7349(2) 0.42371(15) 0.0493(11) Uani 1 1 d . . . Al2 Al 0.3588(3) 0.7542(2) 0.30469(16) 0.0524(11) Uani 1 1 d . . . O1 O 0.3885(6) 0.8185(4) 0.3870(3) 0.051(2) Uani 1 1 d . . . O2 O 0.3554(6) 0.6695(5) 0.3476(3) 0.051(2) Uani 1 1 d . . . O5 O 0.3195(6) 0.8139(5) 0.4934(3) 0.051(2) Uani 1 1 d . . . O3 O 0.5014(6) 0.7249(5) 0.4579(3) 0.055(2) Uani 1 1 d . . . O6 O 0.2918(6) 0.6448(5) 0.4531(4) 0.057(2) Uani 1 1 d . . . O9 O 0.7155(8) 0.8357(5) 0.4374(4) 0.068(3) Uani 1 1 d . . . O7 O 0.3165(7) 0.6804(6) 0.2246(4) 0.072(3) Uani 1 1 d . . . O11 O 0.1755(7) 0.7447(5) 0.3876(4) 0.057(2) Uani 1 1 d . . . O8 O 0.3539(6) 0.8488(5) 0.2704(4) 0.059(2) Uani 1 1 d . . . O10 O 0.7145(7) 0.6542(5) 0.3976(4) 0.065(3) Uani 1 1 d . . . O4 O 0.5207(6) 0.7450(5) 0.3129(3) 0.052(2) Uani 1 1 d . . . O12 O 0.1889(6) 0.7648(5) 0.2960(4) 0.060(2) Uani 1 1 d . . . C94 C 0.8268(13) 0.8266(10) 0.4517(6) 0.058(4) Uani 1 1 d . . . C4 C 0.5808(11) 0.7446(10) 0.2668(6) 0.077(5) Uani 1 1 d . . . H27A H 0.5230 0.7535 0.2319 0.092 Uiso 1 1 calc R . . C61 C 0.1329(10) 0.7593(8) 0.3361(7) 0.051(4) Uani 1 1 d . . . C54 C 0.2472(10) 0.6497(9) 0.4988(6) 0.062(4) Uani 1 1 d . . . C52 C 0.2695(9) 0.8033(8) 0.5338(5) 0.050(3) Uani 1 1 d . . . C92 C 0.8244(12) 0.6716(9) 0.4183(6) 0.058(4) Uani 1 1 d . . . C3 C 0.5493(12) 0.7174(10) 0.5189(7) 0.068(4) Uani 1 1 d . . . H36A H 0.4853 0.7222 0.5389 0.082 Uiso 1 1 calc R . . C31 C 0.6412(12) 0.7849(10) 0.5551(6) 0.105(6) Uani 1 1 d . . . H38A H 0.6086 0.8380 0.5567 0.157 Uiso 1 1 calc R . . H38B H 0.7052 0.7823 0.5365 0.157 Uiso 1 1 calc R . . H38C H 0.6682 0.7772 0.5951 0.157 Uiso 1 1 calc R . . C74 C 0.3070(11) 0.8517(10) 0.2134(7) 0.065(4) Uani 1 1 d . . . C53 C 0.2286(10) 0.7249(10) 0.5379(6) 0.063(4) Uani 1 1 d . . . H41A H 0.1887 0.7226 0.5670 0.076 Uiso 1 1 calc R . . C72 C 0.2759(13) 0.6982(11) 0.1744(7) 0.068(4) Uani 1 1 d . . . C73 C 0.2668(12) 0.7810(12) 0.1670(7) 0.082(5) Uani 1 1 d . . . H44A H 0.2321 0.7886 0.1291 0.099 Uiso 1 1 calc R . . C51 C 0.2494(11) 0.8816(8) 0.5790(6) 0.083(5) Uani 1 1 d . . . H46A H 0.2794 0.9297 0.5701 0.125 Uiso 1 1 calc R . . H46B H 0.2886 0.8784 0.6189 0.125 Uiso 1 1 calc R . . H46C H 0.1677 0.8855 0.5762 0.125 Uiso 1 1 calc R . . C1 C 0.3999(10) 0.9085(8) 0.4146(6) 0.065(4) Uani 1 1 d . . . H47A H 0.4258 0.9143 0.4580 0.078 Uiso 1 1 calc R . . C91 C 0.8983(13) 0.5973(9) 0.4092(8) 0.106(6) Uani 1 1 d . . . H52A H 0.8487 0.5479 0.3906 0.159 Uiso 1 1 calc R . . H52B H 0.9449 0.5923 0.4474 0.159 Uiso 1 1 calc R . . H52C H 0.9480 0.6046 0.3839 0.159 Uiso 1 1 calc R . . C32 C 0.5932(14) 0.6294(12) 0.5167(7) 0.114(6) Uani 1 1 d . . . H54A H 0.5310 0.5890 0.4946 0.172 Uiso 1 1 calc R . . H54B H 0.6198 0.6221 0.5568 0.172 Uiso 1 1 calc R . . H54C H 0.6561 0.6224 0.4972 0.172 Uiso 1 1 calc R . . C41 C 0.6761(12) 0.8170(11) 0.2846(7) 0.115(6) Uani 1 1 d . . . H57A H 0.6419 0.8688 0.2958 0.172 Uiso 1 1 calc R . . H57B H 0.7086 0.8172 0.2511 0.172 Uiso 1 1 calc R . . H57C H 0.7363 0.8095 0.3180 0.172 Uiso 1 1 calc R . . C55 C 0.2158(12) 0.5644(8) 0.5089(6) 0.090(5) Uani 1 1 d . . . H59A H 0.2347 0.5210 0.4786 0.135 Uiso 1 1 calc R . . H59B H 0.1342 0.5597 0.5067 0.135 Uiso 1 1 calc R . . H59C H 0.2592 0.5597 0.5478 0.135 Uiso 1 1 calc R . . C2 C 0.3417(13) 0.5794(11) 0.3197(7) 0.087(5) Uani 1 1 d . . . H61A H 0.3654 0.5740 0.2821 0.104 Uiso 1 1 calc R . . C21 C 0.2126(12) 0.5479(9) 0.2999(7) 0.118(6) Uani 1 1 d . . . H62A H 0.1682 0.5833 0.2772 0.178 Uiso 1 1 calc R . . H62B H 0.1840 0.5483 0.3347 0.178 Uiso 1 1 calc R . . H62C H 0.2053 0.4924 0.2754 0.178 Uiso 1 1 calc R . . C11 C 0.4936(11) 0.9551(7) 0.3971(6) 0.072(4) Uani 1 1 d . . . H64A H 0.5658 0.9289 0.4054 0.109 Uiso 1 1 calc R . . H64B H 0.5034 1.0116 0.4199 0.109 Uiso 1 1 calc R . . H64C H 0.4701 0.9538 0.3551 0.109 Uiso 1 1 calc R . . C71 C 0.2371(14) 0.6252(9) 0.1203(6) 0.110(6) Uani 1 1 d . . . H65A H 0.2483 0.5743 0.1330 0.164 Uiso 1 1 calc R . . H65B H 0.2821 0.6270 0.0917 0.164 Uiso 1 1 calc R . . H65C H 0.1563 0.6282 0.1019 0.164 Uiso 1 1 calc R . . C95 C 0.9014(11) 0.9091(8) 0.4784(7) 0.097(5) Uani 1 1 d . . . H68A H 0.8515 0.9546 0.4799 0.146 Uiso 1 1 calc R . . H68B H 0.9531 0.9142 0.4536 0.146 Uiso 1 1 calc R . . H68C H 0.9458 0.9097 0.5182 0.146 Uiso 1 1 calc R . . C93 C 0.8821(12) 0.7513(10) 0.4461(6) 0.068(4) Uani 1 1 d . . . H69A H 0.9621 0.7537 0.4617 0.081 Uiso 1 1 calc R . . C12 C 0.2822(12) 0.9476(8) 0.4036(7) 0.097(5) Uani 1 1 d . . . H71A H 0.2271 0.9170 0.4157 0.145 Uiso 1 1 calc R . . H71B H 0.2551 0.9465 0.3618 0.145 Uiso 1 1 calc R . . H71C H 0.2906 1.0040 0.4267 0.145 Uiso 1 1 calc R . . C75 C 0.3058(14) 0.9409(10) 0.2034(7) 0.104(5) Uani 1 1 d . . . H79A H 0.3367 0.9798 0.2410 0.155 Uiso 1 1 calc R . . H79B H 0.2274 0.9532 0.1870 0.155 Uiso 1 1 calc R . . H79C H 0.3524 0.9449 0.1759 0.155 Uiso 1 1 calc R . . C62 C 0.0009(11) 0.7678(11) 0.3198(6) 0.112(6) Uani 1 1 d . . . H81A H -0.0223 0.7791 0.2807 0.167 Uiso 1 1 calc R . . H81B H -0.0191 0.8125 0.3488 0.167 Uiso 1 1 calc R . . H81C H -0.0383 0.7172 0.3197 0.167 Uiso 1 1 calc R . . C42 C 0.6292(15) 0.6594(11) 0.2468(8) 0.141(8) Uani 1 1 d . . . H98A H 0.5675 0.6171 0.2352 0.211 Uiso 1 1 calc R . . H98B H 0.6883 0.6489 0.2794 0.211 Uiso 1 1 calc R . . H98C H 0.6619 0.6594 0.2133 0.211 Uiso 1 1 calc R . . Co1A Co 0.84808(14) 0.22987(11) 0.10862(8) 0.0620(6) Uani 1 1 d . . . Al1A Al 0.6106(3) 0.2299(2) 0.14887(16) 0.0557(14) Uani 1 1 d . . . Al2A Al 0.8235(3) 0.2124(3) 0.23722(17) 0.0596(15) Uani 1 1 d . . . O2A O 0.7464(7) 0.2971(5) 0.2023(3) 0.062(3) Uani 1 1 d . . . O1A O 0.7127(6) 0.1460(5) 0.1687(3) 0.057(2) Uani 1 1 d . . . O9A O 0.8972(7) 0.1472(5) 0.0428(4) 0.073(3) Uani 1 1 d . . . O8A O 0.8850(8) 0.1200(5) 0.2681(5) 0.067(3) Uani 1 1 d . . . O3A O 0.6751(6) 0.2301(5) 0.0828(4) 0.063(2) Uani 1 1 d . . . O10A O 0.9227(7) 0.3260(5) 0.0903(4) 0.068(3) Uani 1 1 d . . . O11A O 0.5429(7) 0.2281(6) 0.2171(4) 0.073(3) Uani 1 1 d . . . O5A O 0.4809(8) 0.1545(5) 0.1013(3) 0.062(3) Uani 1 1 d . . . O4A O 0.9312(6) 0.2105(5) 0.1888(3) 0.059(2) Uani 1 1 d . . . O7A O 0.9210(8) 0.2871(6) 0.3061(4) 0.068(3) Uani 1 1 d . . . C61A C 0.5957(13) 0.2214(9) 0.2700(7) 0.068(4) Uani 1 1 d . . . O12A O 0.7071(8) 0.2149(6) 0.2874(3) 0.073(3) Uani 1 1 d . . . O6A O 0.5204(9) 0.3232(6) 0.1392(4) 0.078(3) Uani 1 1 d . . . C3A C 0.6062(12) 0.2311(10) 0.0232(7) 0.084(5) Uani 1 1 d . . . H29A H 0.5268 0.2424 0.0266 0.101 Uiso 1 1 calc R . . C4A C 1.0587(12) 0.2030(10) 0.2074(7) 0.087(5) Uani 1 1 d . . . H30A H 1.0765 0.1973 0.2490 0.105 Uiso 1 1 calc R . . C92A C 0.9741(11) 0.3214(9) 0.0462(7) 0.066(4) Uani 1 1 d . . . C93A C 0.9850(11) 0.2467(11) 0.0059(7) 0.075(4) Uani 1 1 d . . . H37A H 1.0226 0.2510 -0.0237 0.089 Uiso 1 1 calc R . . C72A C 0.9876(12) 0.2702(13) 0.3533(7) 0.066(5) Uani 1 1 d . . . C74A C 0.9566(13) 0.1160(13) 0.3201(8) 0.079(5) Uani 1 1 d . . . C94A C 0.9459(11) 0.1659(10) 0.0050(6) 0.070(4) Uani 1 1 d . . . C52A C 0.3736(14) 0.1700(14) 0.0854(6) 0.080(5) Uani 1 1 d . . . C95A C 0.9671(12) 0.0916(9) -0.0457(6) 0.099(5) Uani 1 1 d . . . H49A H 0.9350 0.0410 -0.0415 0.149 Uiso 1 1 calc R . . H49B H 1.0490 0.0878 -0.0423 0.149 Uiso 1 1 calc R . . H49C H 0.9302 0.1009 -0.0843 0.149 Uiso 1 1 calc R . . C53A C 0.3367(13) 0.2506(14) 0.0947(8) 0.097(6) Uani 1 1 d . . . H50A H 0.2574 0.2566 0.0821 0.116 Uiso 1 1 calc R . . C73A C 1.0067(12) 0.1874(13) 0.3621(7) 0.073(5) Uani 1 1 d . . . H53A H 1.0553 0.1818 0.3981 0.088 Uiso 1 1 calc R . . C1A C 0.6926(12) 0.0562(9) 0.1464(7) 0.086(5) Uani 1 1 d . . . H55A H 0.6328 0.0525 0.1092 0.103 Uiso 1 1 calc R . . C54A C 0.4078(17) 0.3236(13) 0.1215(8) 0.094(5) Uani 1 1 d . . . C2A C 0.7532(11) 0.3916(9) 0.2205(7) 0.090(5) Uani 1 1 d . . . H58A H 0.7045 0.4104 0.1868 0.108 Uiso 1 1 calc R . . C21A C 0.6947(12) 0.4170(8) 0.2740(7) 0.106(6) Uani 1 1 d . . . H60A H 0.6180 0.3908 0.2629 0.159 Uiso 1 1 calc R . . H60B H 0.6900 0.4761 0.2840 0.159 Uiso 1 1 calc R . . H60C H 0.7402 0.3999 0.3082 0.159 Uiso 1 1 calc R . . C71A C 1.0502(12) 0.3490(10) 0.4014(6) 0.106(6) Uani 1 1 d . . . H63A H 1.0276 0.3977 0.3872 0.159 Uiso 1 1 calc R . . H63B H 1.1329 0.3455 0.4079 0.159 Uiso 1 1 calc R . . H63C H 1.0285 0.3519 0.4384 0.159 Uiso 1 1 calc R . . C51A C 0.2898(12) 0.0929(11) 0.0574(8) 0.132(7) Uani 1 1 d . . . H66A H 0.3331 0.0440 0.0559 0.198 Uiso 1 1 calc R . . H66B H 0.2487 0.0948 0.0175 0.198 Uiso 1 1 calc R . . H66C H 0.2352 0.0917 0.0814 0.198 Uiso 1 1 calc R . . C91A C 1.0206(13) 0.4075(9) 0.0415(7) 0.101(5) Uani 1 1 d . . . H67A H 1.0059 0.4503 0.0735 0.151 Uiso 1 1 calc R . . H67B H 0.9818 0.4181 0.0036 0.151 Uiso 1 1 calc R . . H67C H 1.1027 0.4067 0.0446 0.151 Uiso 1 1 calc R . . C42A C 1.1260(14) 0.2807(12) 0.2073(10) 0.158(9) Uani 1 1 d . . . H76A H 1.1026 0.3277 0.2331 0.238 Uiso 1 1 calc R . . H76B H 1.1103 0.2887 0.1672 0.238 Uiso 1 1 calc R . . H76C H 1.2077 0.2749 0.2214 0.238 Uiso 1 1 calc R . . C75A C 0.9850(15) 0.0303(11) 0.3288(8) 0.108(6) Uani 1 1 d . . . H78A H 0.9429 -0.0104 0.2943 0.161 Uiso 1 1 calc R . . H78B H 0.9633 0.0228 0.3639 0.161 Uiso 1 1 calc R . . H78C H 1.0669 0.0241 0.3335 0.161 Uiso 1 1 calc R . . C41A C 1.0921(14) 0.1255(12) 0.1706(9) 0.161(9) Uani 1 1 d . . . H82A H 1.1741 0.1201 0.1838 0.242 Uiso 1 1 calc R . . H82B H 1.0731 0.1277 0.1292 0.242 Uiso 1 1 calc R . . H82C H 1.0506 0.0786 0.1751 0.242 Uiso 1 1 calc R . . C62A C 0.5235(12) 0.2192(13) 0.3154(6) 0.145(8) Uani 1 1 d . . . H83A H 0.5735 0.2131 0.3524 0.217 Uiso 1 1 calc R . . H83B H 0.4667 0.1734 0.2997 0.217 Uiso 1 1 calc R . . H83C H 0.4848 0.2700 0.3225 0.217 Uiso 1 1 calc R . . C12A C 0.6256(13) 0.0182(9) 0.1825(7) 0.101(5) Uani 1 1 d . . . H85A H 0.5630 0.0522 0.1901 0.152 Uiso 1 1 calc R . . H85B H 0.6768 0.0149 0.2200 0.152 Uiso 1 1 calc R . . H85C H 0.5948 -0.0364 0.1602 0.152 Uiso 1 1 calc R . . C32A C 0.6496(15) 0.3009(14) 0.0023(9) 0.177(11) Uani 1 1 d . . . H88A H 0.6481 0.3522 0.0308 0.266 Uiso 1 1 calc R . . H88B H 0.6009 0.3031 -0.0360 0.266 Uiso 1 1 calc R . . H88C H 0.7279 0.2923 -0.0012 0.266 Uiso 1 1 calc R . . C11A C 0.780(2) 0.0141(11) 0.1246(10) 0.193(12) Uani 1 1 d . . . H90A H 0.8093 0.0450 0.1010 0.290 Uiso 1 1 calc R . . H90B H 0.7490 -0.0395 0.1001 0.290 Uiso 1 1 calc R . . H90C H 0.8414 0.0075 0.1576 0.290 Uiso 1 1 calc R . . C22A C 0.8737(17) 0.4296(11) 0.2312(9) 0.163(8) Uani 1 1 d . . . H94A H 0.9021 0.4110 0.1958 0.245 Uiso 1 1 calc R . . H94B H 0.9243 0.4131 0.2643 0.245 Uiso 1 1 calc R . . H94C H 0.8718 0.4889 0.2402 0.245 Uiso 1 1 calc R . . C55A C 0.3596(15) 0.4114(12) 0.1302(10) 0.159(9) Uani 1 1 d . . . H95A H 0.4222 0.4522 0.1505 0.238 Uiso 1 1 calc R . . H95B H 0.3033 0.4148 0.1538 0.238 Uiso 1 1 calc R . . H95C H 0.3235 0.4215 0.0917 0.238 Uiso 1 1 calc R . . C22 C 0.4201(17) 0.5318(11) 0.3522(9) 0.132(7) Uani 1 1 d . . . H10A H 0.4978 0.5555 0.3606 0.198 Uiso 1 1 calc R . . H10B H 0.4155 0.4759 0.3287 0.198 Uiso 1 1 calc R . . H10C H 0.3998 0.5319 0.3892 0.198 Uiso 1 1 calc R . . C31A C 0.6001(15) 0.1447(12) -0.0217(7) 0.149(8) Uani 1 1 d . . . H10D H 0.5712 0.1028 -0.0059 0.223 Uiso 1 1 calc R . . H10E H 0.6763 0.1322 -0.0271 0.223 Uiso 1 1 calc R . . H10F H 0.5489 0.1460 -0.0596 0.223 Uiso 1 1 calc R . . C201 C 0.078(2) 0.322(2) -0.1477(12) 0.204(11) Uiso 1 1 d . . . H20A H 0.0022 0.3240 -0.1700 0.244 Uiso 1 1 calc R . . C205 C 0.214(3) 0.238(2) -0.1048(14) 0.246(14) Uiso 1 1 d . . . H205 H 0.2411 0.1882 -0.0979 0.296 Uiso 1 1 calc R . . C203 C 0.135(2) 0.4001(18) -0.1258(11) 0.207(11) Uiso 1 1 d D . . H20D H 0.1076 0.4497 -0.1341 0.249 Uiso 1 1 calc R . . C204 C 0.250(3) 0.387(3) -0.0855(16) 0.245(14) Uiso 1 1 d . . . C207 C 0.317(4) 0.454(3) -0.061(2) 0.44(3) Uiso 1 1 d D . . H20E H 0.2797 0.5001 -0.0737 0.663 Uiso 1 1 calc R . . H20F H 0.3892 0.4472 -0.0718 0.663 Uiso 1 1 calc R . . H20G H 0.3303 0.4640 -0.0177 0.663 Uiso 1 1 calc R . . C206 C 0.105(3) 0.246(2) -0.1447(13) 0.215(12) Uiso 1 1 d . . . H20H H 0.0557 0.2005 -0.1669 0.258 Uiso 1 1 calc R . . C202 C 0.272(2) 0.3103(17) -0.0794(12) 0.196(10) Uiso 1 1 d D . . H20I H 0.3422 0.3070 -0.0521 0.235 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 Co1 0.0356(10) 0.0681(13) 0.0663(12) 0.0170(10) 0.0088(9) 0.0029(10) Al1 0.034(2) 0.058(3) 0.058(2) 0.018(2) 0.0105(19) 0.007(2) Al2 0.036(2) 0.067(3) 0.055(2) 0.017(2) 0.0100(19) 0.004(2) O1 0.047(5) 0.041(5) 0.063(5) 0.007(4) 0.015(4) 0.001(4) O2 0.042(5) 0.039(5) 0.067(5) 0.008(4) 0.007(4) 0.007(4) O5 0.039(5) 0.065(6) 0.056(5) 0.029(4) 0.013(4) 0.016(4) O3 0.035(5) 0.080(6) 0.052(5) 0.032(5) -0.003(4) 0.012(5) O6 0.041(5) 0.066(6) 0.071(6) 0.039(5) 0.003(5) 0.017(5) O9 0.046(6) 0.080(7) 0.071(6) 0.010(5) 0.008(5) 0.006(6) O7 0.064(6) 0.098(8) 0.051(6) 0.010(6) 0.014(5) 0.004(6) O11 0.028(5) 0.076(6) 0.068(6) 0.033(5) -0.003(5) 0.006(5) O8 0.038(5) 0.069(6) 0.071(6) 0.033(5) 0.003(5) 0.011(5) O10 0.029(5) 0.069(6) 0.100(7) 0.021(5) 0.019(5) 0.017(5) O4 0.024(4) 0.072(6) 0.063(5) 0.027(5) 0.008(4) 0.031(5) O12 0.023(5) 0.094(7) 0.064(5) 0.031(5) 0.000(4) 0.007(5) C94 0.037(10) 0.069(12) 0.068(9) 0.045(9) -0.015(8) -0.002(10) C4 0.040(8) 0.143(14) 0.054(8) 0.031(9) 0.017(7) 0.002(10) C61 0.014(8) 0.082(11) 0.061(10) 0.041(9) -0.007(8) 0.021(7) C54 0.034(8) 0.084(12) 0.077(10) 0.038(9) 0.011(8) -0.002(8) C52 0.020(7) 0.074(11) 0.051(8) 0.022(8) -0.005(6) 0.011(7) C92 0.044(10) 0.070(11) 0.072(9) 0.036(9) 0.018(8) 0.026(10) C3 0.061(10) 0.084(12) 0.080(12) 0.049(10) 0.030(9) 0.040(10) C31 0.072(10) 0.137(14) 0.083(11) 0.015(10) -0.010(9) -0.030(11) C74 0.041(9) 0.095(13) 0.067(11) 0.046(11) 0.003(8) 0.016(9) C53 0.034(8) 0.090(12) 0.069(10) 0.027(9) 0.010(7) 0.017(9) C72 0.068(11) 0.089(13) 0.050(10) 0.010(11) 0.023(9) 0.012(11) C73 0.064(10) 0.114(14) 0.061(10) 0.014(12) 0.005(8) 0.011(12) C51 0.074(10) 0.094(11) 0.084(10) 0.002(9) 0.040(8) 0.007(9) C1 0.046(9) 0.062(10) 0.084(10) 0.014(8) 0.011(8) 0.015(8) C91 0.072(11) 0.094(13) 0.160(16) 0.050(13) 0.024(11) 0.039(11) C32 0.094(13) 0.154(19) 0.110(14) 0.066(14) 0.020(11) 0.037(14) C41 0.081(11) 0.177(17) 0.097(12) 0.049(12) 0.028(10) -0.012(12) C55 0.088(11) 0.087(11) 0.124(13) 0.061(10) 0.047(10) 0.012(10) C2 0.056(11) 0.087(14) 0.109(12) 0.044(12) -0.017(9) 0.029(11) C21 0.090(12) 0.090(12) 0.142(15) -0.011(11) 0.003(11) -0.044(10) C11 0.069(9) 0.052(9) 0.101(11) 0.019(8) 0.030(8) 0.011(8) C71 0.146(15) 0.111(13) 0.058(10) 0.006(10) 0.011(10) -0.008(12) C95 0.062(10) 0.084(11) 0.125(13) 0.013(10) -0.004(9) -0.023(9) C93 0.040(9) 0.073(11) 0.098(11) 0.050(11) 0.003(8) 0.007(10) C12 0.082(12) 0.055(10) 0.156(15) 0.006(10) 0.051(11) 0.014(9) C75 0.116(14) 0.100(14) 0.103(13) 0.065(11) 0.004(11) 0.020(12) C62 0.057(11) 0.204(19) 0.077(11) 0.047(12) 0.009(9) 0.031(12) C42 0.140(16) 0.174(19) 0.131(15) 0.022(14) 0.091(14) 0.082(15) Co1A 0.0485(11) 0.0715(13) 0.0640(12) 0.0143(10) 0.0114(9) 0.0066(11) Al1A 0.038(2) 0.066(3) 0.052(2) 0.001(2) 0.002(2) 0.004(3) Al2A 0.047(3) 0.070(3) 0.053(2) 0.004(3) 0.008(2) 0.005(3) O2A 0.050(5) 0.056(6) 0.064(5) 0.010(5) -0.011(4) 0.017(5) O1A 0.049(5) 0.057(6) 0.057(5) 0.011(5) 0.002(4) 0.009(5) O9A 0.057(6) 0.091(7) 0.075(6) 0.020(5) 0.024(5) 0.012(5) O8A 0.057(6) 0.054(7) 0.084(7) 0.023(6) 0.003(6) 0.014(6) O3A 0.034(5) 0.093(7) 0.055(6) 0.016(5) 0.000(4) 0.004(5) O10A 0.064(6) 0.066(6) 0.071(6) 0.013(5) 0.015(5) 0.011(5) O11A 0.053(6) 0.103(8) 0.057(6) 0.014(6) 0.007(5) 0.010(6) O5A 0.036(6) 0.089(7) 0.046(5) 0.012(5) -0.013(4) 0.007(6) O4A 0.028(5) 0.082(6) 0.060(5) 0.014(5) 0.003(4) 0.020(5) O7A 0.046(6) 0.087(8) 0.055(6) 0.006(6) -0.007(5) 0.008(6) C61A 0.042(10) 0.095(12) 0.066(11) 0.011(9) 0.017(9) 0.022(9) O12A 0.062(7) 0.103(7) 0.056(6) 0.017(5) 0.020(5) 0.015(6) O6A 0.053(6) 0.084(8) 0.085(7) 0.009(6) 0.007(6) 0.020(7) C3A 0.050(9) 0.127(14) 0.077(11) 0.036(11) 0.005(9) 0.003(10) C4A 0.057(11) 0.113(14) 0.090(11) 0.034(11) 0.003(9) 0.039(11) C92A 0.043(9) 0.080(12) 0.067(10) 0.021(9) -0.008(8) 0.007(8) C93A 0.044(9) 0.110(14) 0.085(11) 0.053(11) 0.015(8) 0.011(10) C72A 0.025(9) 0.115(15) 0.053(10) 0.017(12) 0.003(8) 0.025(12) C74A 0.045(10) 0.129(18) 0.058(11) 0.027(14) -0.003(9) 0.021(13) C94A 0.041(9) 0.100(13) 0.066(10) 0.019(10) 0.007(8) 0.026(9) C52A 0.036(11) 0.147(18) 0.043(9) 0.018(11) -0.011(8) -0.005(13) C95A 0.087(11) 0.144(15) 0.065(10) 0.018(10) 0.021(9) 0.017(11) C53A 0.037(11) 0.120(16) 0.127(15) 0.022(14) 0.017(10) 0.035(13) C73A 0.049(10) 0.111(15) 0.065(11) 0.058(13) -0.011(8) 0.037(12) C1A 0.062(10) 0.081(12) 0.114(12) 0.009(10) 0.033(9) -0.003(9) C54A 0.068(14) 0.120(18) 0.099(13) 0.048(13) 0.005(11) 0.034(15) C2A 0.040(8) 0.081(12) 0.114(13) -0.034(10) 0.005(8) 0.009(9) C21A 0.085(11) 0.062(10) 0.137(14) -0.019(10) 0.005(11) 0.025(9) C71A 0.074(10) 0.136(15) 0.084(11) 0.006(11) -0.009(9) -0.001(11) C51A 0.055(10) 0.158(17) 0.147(16) -0.017(13) 0.007(10) -0.024(11) C91A 0.102(12) 0.086(12) 0.136(14) 0.049(11) 0.049(11) 0.007(10) C42A 0.079(13) 0.156(18) 0.26(3) 0.086(18) 0.038(15) -0.013(13) C75A 0.101(15) 0.100(14) 0.138(16) 0.081(13) 0.007(12) 0.038(13) C41A 0.089(13) 0.20(2) 0.161(18) -0.018(17) 0.031(13) 0.092(15) C62A 0.058(10) 0.32(3) 0.068(10) 0.051(14) 0.031(9) 0.025(13) C12A 0.096(12) 0.089(12) 0.122(13) 0.046(11) 0.014(11) -0.001(10) C32A 0.082(14) 0.29(3) 0.22(2) 0.21(2) -0.002(14) 0.009(17) C11A 0.31(3) 0.096(15) 0.22(2) 0.005(15) 0.18(2) 0.020(18) C22A 0.16(2) 0.114(15) 0.20(2) -0.012(15) 0.057(17) -0.014(14) C55A 0.073(13) 0.122(18) 0.25(3) 0.063(18) -0.034(15) 0.075(14) C22 0.121(16) 0.083(14) 0.163(18) -0.008(13) 0.014(15) 0.003(14) C31A 0.117(15) 0.20(2) 0.078(12) -0.037(14) -0.015(11) 0.012(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O9 2.022(8) . ? Co1 O4 2.024(8) . ? Co1 O3 2.031(7) . ? Co1 O10 2.039(8) . ? Al1 O3 1.889(8) . ? Al1 O2 1.914(8) . ? Al1 O5 1.931(8) . ? Al1 O1 1.937(8) . ? Al1 O6 1.939(8) . ? Al1 O11 1.987(9) . ? Al1 Al2 2.951(5) . ? Al2 O4 1.895(7) . ? Al2 O2 1.919(8) . ? Al2 O8 1.922(9) . ? Al2 O1 1.940(8) . ? Al2 O7 1.953(9) . ? Al2 O12 1.991(8) . ? O1 C1 1.480(13) . ? O2 C2 1.482(16) . ? O5 C52 1.281(12) . ? O3 C3 1.450(15) . ? O6 C54 1.299(13) . ? O9 C94 1.302(15) . ? O7 C72 1.271(16) . ? O11 C61 1.280(13) . ? O8 C74 1.339(14) . ? O10 C92 1.287(14) . ? O4 C4 1.435(12) . ? O12 C61 1.299(13) . ? C94 C93 1.407(17) . ? C94 C95 1.547(17) . ? C4 C42 1.541(19) . ? C4 C41 1.562(17) . ? C61 C62 1.536(16) . ? C54 C53 1.424(17) . ? C54 C55 1.549(16) . ? C52 C53 1.421(16) . ? C52 C51 1.541(16) . ? C92 C93 1.428(17) . ? C92 C91 1.520(17) . ? C3 C31 1.514(17) . ? C3 C32 1.547(18) . ? C74 C73 1.402(19) . ? C74 C75 1.553(18) . ? C72 C73 1.428(19) . ? C72 C71 1.524(18) . ? C1 C12 1.532(17) . ? C1 C11 1.540(15) . ? C2 C22 1.421(19) . ? C2 C21 1.545(18) . ? Co1A O3A 1.998(7) . ? Co1A O10A 2.005(9) . ? Co1A O4A 2.014(8) . ? Co1A O9A 2.023(9) . ? Al1A O3A 1.896(8) . ? Al1A O1A 1.913(10) . ? Al1A O6A 1.910(11) . ? Al1A O5A 1.930(8) . ? Al1A O2A 1.954(8) . ? Al1A O11A 1.971(9) . ? Al1A Al2A 2.931(6) . ? Al2A O4A 1.904(8) . ? Al2A O2A 1.917(10) . ? Al2A O8A 1.919(12) . ? Al2A O7A 1.923(9) . ? Al2A O1A 1.930(8) . ? Al2A O12A 2.018(9) . ? O2A C2A 1.525(15) . ? O1A C1A 1.463(15) . ? O9A C94A 1.267(15) . ? O8A C74A 1.332(16) . ? O3A C3A 1.454(15) . ? O10A C92A 1.316(15) . ? O11A C61A 1.288(15) . ? O5A C52A 1.283(17) . ? O4A C4A 1.485(14) . ? O7A C72A 1.294(17) . ? C61A O12A 1.300(15) . ? C61A C62A 1.529(17) . ? O6A C54A 1.303(18) . ? C3A C32A 1.495(19) . ? C3A C31A 1.57(2) . ? C4A C41A 1.491(19) . ? C4A C42A 1.520(19) . ? C92A C93A 1.407(18) . ? C92A C91A 1.568(17) . ? C93A C94A 1.413(18) . ? C72A C73A 1.446(19) . ? C72A C71A 1.57(2) . ? C74A C73A 1.39(2) . ? C74A C75A 1.51(2) . ? C94A C95A 1.576(17) . ? C52A C53A 1.39(2) . ? C52A C51A 1.54(2) . ? C53A C54A 1.40(2) . ? C1A C11A 1.38(2) . ? C1A C12A 1.525(17) . ? C54A C55A 1.55(2) . ? C2A C22A 1.504(19) . ? C2A C21A 1.560(18) . ? C201 C206 1.31(3) . ? C201 C203 1.39(3) . ? C205 C202 1.32(3) . ? C205 C206 1.44(4) . ? C203 C204 1.51(4) . ? C204 C207 1.30(5) . ? C204 C202 1.34(4) . ? 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 O9 Co1 O4 110.0(3) . . ? O9 Co1 O3 110.4(3) . . ? O4 Co1 O3 123.9(3) . . ? O9 Co1 O10 92.9(3) . . ? O4 Co1 O10 107.7(3) . . ? O3 Co1 O10 107.4(3) . . ? O3 Al1 O2 91.1(3) . . ? O3 Al1 O5 94.4(3) . . ? O2 Al1 O5 170.8(4) . . ? O3 Al1 O1 88.7(3) . . ? O2 Al1 O1 78.3(3) . . ? O5 Al1 O1 94.4(3) . . ? O3 Al1 O6 93.4(4) . . ? O2 Al1 O6 96.8(4) . . ? O5 Al1 O6 90.3(4) . . ? O1 Al1 O6 174.7(4) . . ? O3 Al1 O11 179.6(4) . . ? O2 Al1 O11 88.7(4) . . ? O5 Al1 O11 85.8(3) . . ? O1 Al1 O11 91.6(4) . . ? O6 Al1 O11 86.3(3) . . ? O3 Al1 Al2 99.3(3) . . ? O2 Al1 Al2 39.7(2) . . ? O5 Al1 Al2 131.7(3) . . ? O1 Al1 Al2 40.5(2) . . ? O6 Al1 Al2 134.3(3) . . ? O11 Al1 Al2 80.7(3) . . ? O4 Al2 O2 90.5(4) . . ? O4 Al2 O8 93.7(3) . . ? O2 Al2 O8 172.0(4) . . ? O4 Al2 O1 90.0(3) . . ? O2 Al2 O1 78.1(3) . . ? O8 Al2 O1 95.0(4) . . ? O4 Al2 O7 94.1(4) . . ? O2 Al2 O7 96.1(4) . . ? O8 Al2 O7 90.5(4) . . ? O1 Al2 O7 172.9(4) . . ? O4 Al2 O12 179.5(4) . . ? O2 Al2 O12 90.0(3) . . ? O8 Al2 O12 85.8(4) . . ? O1 Al2 O12 89.9(3) . . ? O7 Al2 O12 86.0(4) . . ? O4 Al2 Al1 99.7(3) . . ? O2 Al2 Al1 39.6(2) . . ? O8 Al2 Al1 132.6(3) . . ? O1 Al2 Al1 40.4(2) . . ? O7 Al2 Al1 132.9(3) . . ? O12 Al2 Al1 80.5(3) . . ? C1 O1 Al1 124.3(7) . . ? C1 O1 Al2 133.2(7) . . ? Al1 O1 Al2 99.2(3) . . ? C2 O2 Al1 133.7(8) . . ? C2 O2 Al2 124.5(8) . . ? Al1 O2 Al2 100.7(4) . . ? C52 O5 Al1 129.6(8) . . ? C3 O3 Al1 125.2(7) . . ? C3 O3 Co1 126.2(7) . . ? Al1 O3 Co1 108.2(4) . . ? C54 O6 Al1 127.9(8) . . ? C94 O9 Co1 124.4(9) . . ? C72 O7 Al2 128.9(10) . . ? C61 O11 Al1 126.0(7) . . ? C74 O8 Al2 127.6(9) . . ? C92 O10 Co1 123.5(8) . . ? C4 O4 Al2 125.8(7) . . ? C4 O4 Co1 126.4(7) . . ? Al2 O4 Co1 107.8(3) . . ? C61 O12 Al2 125.7(7) . . ? O9 C94 C93 126.7(12) . . ? O9 C94 C95 114.0(14) . . ? C93 C94 C95 119.3(13) . . ? O4 C4 C42 111.5(12) . . ? O4 C4 C41 112.7(11) . . ? C42 C4 C41 112.3(12) . . ? O11 C61 O12 126.8(11) . . ? O11 C61 C62 115.8(12) . . ? O12 C61 C62 117.3(12) . . ? O6 C54 C53 125.0(12) . . ? O6 C54 C55 113.9(12) . . ? C53 C54 C55 121.1(12) . . ? O5 C52 C53 124.3(11) . . ? O5 C52 C51 116.9(11) . . ? C53 C52 C51 118.8(11) . . ? O10 C92 C93 127.5(13) . . ? O10 C92 C91 114.2(12) . . ? C93 C92 C91 118.2(13) . . ? O3 C3 C31 113.5(11) . . ? O3 C3 C32 108.6(12) . . ? C31 C3 C32 112.7(13) . . ? O8 C74 C73 123.3(14) . . ? O8 C74 C75 113.4(13) . . ? C73 C74 C75 123.2(14) . . ? C52 C53 C54 121.8(11) . . ? O7 C72 C73 123.5(14) . . ? O7 C72 C71 116.3(16) . . ? C73 C72 C71 120.2(15) . . ? C74 C73 C72 124.1(14) . . ? O1 C1 C12 111.6(10) . . ? O1 C1 C11 113.3(9) . . ? C12 C1 C11 112.6(11) . . ? C22 C2 O2 113.7(12) . . ? C22 C2 C21 116.5(15) . . ? O2 C2 C21 111.5(13) . . ? C94 C93 C92 124.8(12) . . ? O3A Co1A O10A 110.5(4) . . ? O3A Co1A O4A 122.5(3) . . ? O10A Co1A O4A 111.6(3) . . ? O3A Co1A O9A 106.2(3) . . ? O10A Co1A O9A 92.6(4) . . ? O4A Co1A O9A 109.2(3) . . ? O3A Al1A O1A 89.1(4) . . ? O3A Al1A O6A 94.1(4) . . ? O1A Al1A O6A 172.1(4) . . ? O3A Al1A O5A 93.8(3) . . ? O1A Al1A O5A 95.9(4) . . ? O6A Al1A O5A 91.1(4) . . ? O3A Al1A O2A 89.4(3) . . ? O1A Al1A O2A 78.7(4) . . ? O6A Al1A O2A 94.1(4) . . ? O5A Al1A O2A 173.7(5) . . ? O3A Al1A O11A 179.3(4) . . ? O1A Al1A O11A 90.6(4) . . ? O6A Al1A O11A 86.4(4) . . ? O5A Al1A O11A 85.6(4) . . ? O2A Al1A O11A 91.2(4) . . ? O3A Al1A Al2A 99.0(3) . . ? O1A Al1A Al2A 40.5(2) . . ? O6A Al1A Al2A 131.7(3) . . ? O5A Al1A Al2A 133.6(4) . . ? O2A Al1A Al2A 40.3(3) . . ? O11A Al1A Al2A 81.1(3) . . ? O4A Al2A O2A 88.6(4) . . ? O4A Al2A O8A 94.2(4) . . ? O2A Al2A O8A 173.6(4) . . ? O4A Al2A O7A 94.1(4) . . ? O2A Al2A O7A 95.7(4) . . ? O8A Al2A O7A 89.9(5) . . ? O4A Al2A O1A 89.4(3) . . ? O2A Al2A O1A 79.2(4) . . ? O8A Al2A O1A 95.0(4) . . ? O7A Al2A O1A 173.8(5) . . ? O4A Al2A O12A 179.0(4) . . ? O2A Al2A O12A 90.6(4) . . ? O8A Al2A O12A 86.5(4) . . ? O7A Al2A O12A 86.5(4) . . ? O1A Al2A O12A 89.9(4) . . ? O4A Al2A Al1A 98.8(3) . . ? O2A Al2A Al1A 41.2(2) . . ? O8A Al2A Al1A 132.5(3) . . ? O7A Al2A Al1A 134.0(4) . . ? O1A Al2A Al1A 40.1(3) . . ? O12A Al2A Al1A 80.3(3) . . ? C2A O2A Al2A 134.4(8) . . ? C2A O2A Al1A 124.1(7) . . ? Al2A O2A Al1A 98.4(4) . . ? C1A O1A Al1A 127.8(8) . . ? C1A O1A Al2A 131.3(8) . . ? Al1A O1A Al2A 99.4(4) . . ? C94A O9A Co1A 125.0(9) . . ? C74A O8A Al2A 131.7(12) . . ? C3A O3A Al1A 123.8(7) . . ? C3A O3A Co1A 126.6(7) . . ? Al1A O3A Co1A 109.6(4) . . ? C92A O10A Co1A 125.3(8) . . ? C61A O11A Al1A 128.0(8) . . ? C52A O5A Al1A 128.4(10) . . ? C4A O4A Al2A 126.6(8) . . ? C4A O4A Co1A 123.9(7) . . ? Al2A O4A Co1A 109.4(4) . . ? C72A O7A Al2A 128.6(11) . . ? O11A C61A O12A 124.1(12) . . ? O11A C61A C62A 118.4(13) . . ? O12A C61A C62A 117.4(14) . . ? C61A O12A Al2A 126.5(8) . . ? C54A O6A Al1A 127.3(12) . . ? O3A C3A C32A 110.1(12) . . ? O3A C3A C31A 111.5(13) . . ? C32A C3A C31A 113.6(15) . . ? O4A C4A C41A 110.0(12) . . ? O4A C4A C42A 111.6(13) . . ? C41A C4A C42A 113.9(15) . . ? O10A C92A C93A 123.5(12) . . ? O10A C92A C91A 113.9(13) . . ? C93A C92A C91A 122.5(13) . . ? C92A C93A C94A 128.0(13) . . ? O7A C72A C73A 124.7(15) . . ? O7A C72A C71A 113.5(17) . . ? C73A C72A C71A 121.8(17) . . ? O8A C74A C73A 121.0(18) . . ? O8A C74A C75A 116.5(16) . . ? C73A C74A C75A 122.4(16) . . ? O9A C94A C93A 125.3(13) . . ? O9A C94A C95A 116.3(14) . . ? C93A C94A C95A 118.4(14) . . ? O5A C52A C53A 122.1(15) . . ? O5A C52A C51A 114.7(18) . . ? C53A C52A C51A 123.2(17) . . ? C52A C53A C54A 126.2(15) . . ? C74A C73A C72A 123.8(15) . . ? C11A C1A O1A 116.7(12) . . ? C11A C1A C12A 120.4(15) . . ? O1A C1A C12A 112.3(12) . . ? O6A C54A C53A 122.4(17) . . ? O6A C54A C55A 114.5(17) . . ? C53A C54A C55A 123.1(17) . . ? C22A C2A O2A 113.3(11) . . ? C22A C2A C21A 115.4(12) . . ? O2A C2A C21A 107.2(12) . . ? C206 C201 C203 136(3) . . ? C202 C205 C206 113(3) . . ? C201 C203 C204 105(3) . . ? C207 C204 C202 127(3) . . ? C207 C204 C203 115(3) . . ? C202 C204 C203 118(4) . . ? C201 C206 C205 116(3) . . ? C205 C202 C204 132(4) . . ? _diffrn_measured_fraction_theta_max 0.786 _diffrn_reflns_theta_full 20.00 _diffrn_measured_fraction_theta_full 0.786 _refine_diff_density_max 0.524 _refine_diff_density_min -0.387 _refine_diff_density_rms 0.069 data_mnal2m _database_code_depnum_ccdc_archive 'CCDC 200111' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32.50 H56 Al2 Mn O12' _chemical_formula_weight 747.67 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 '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 11.6387(15) _cell_length_b 16.187(2) _cell_length_c 23.160(3) _cell_angle_alpha 103.880(2) _cell_angle_beta 103.726(3) _cell_angle_gamma 90.034(3) _cell_volume 4107.4(9) _cell_formula_units_Z 4 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 994(I>2sigma(I)) _cell_measurement_theta_min 0.93 _cell_measurement_theta_max 20.00 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.209 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1592 _exptl_absorpt_coefficient_mu 0.416 _exptl_absorpt_correction_type 'not applied' _exptl_absorpt_correction_T_min 0.8347 _exptl_absorpt_correction_T_max 0.9402 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(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 'Bruker SMART CCD 1k' _diffrn_measurement_method 'Bruker SMART' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10526 _diffrn_reflns_av_R_equivalents 0.0535 _diffrn_reflns_av_sigmaI/netI 0.1287 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 0.93 _diffrn_reflns_theta_max 20.00 _reflns_number_total 7489 _reflns_number_gt 3522 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINTPLUS' _computing_data_reduction 'Bruker SAINTPLUS' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL-NT' _computing_publication_material 'Bruker SHELXTL-NT' _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^)+(0.1014P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7489 _refine_ls_number_parameters 821 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1524 _refine_ls_R_factor_gt 0.0668 _refine_ls_wR_factor_ref 0.1805 _refine_ls_wR_factor_gt 0.1567 _refine_ls_goodness_of_fit_ref 0.868 _refine_ls_restrained_S_all 0.868 _refine_ls_shift/su_max 0.019 _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 Mn1 Mn 0.59332(12) 0.73859(9) 0.39794(6) 0.0637(5) Uani 1 1 d . . . Al1 Al 0.3455(2) 0.73395(17) 0.42430(12) 0.0511(8) Uani 1 1 d . . . Al2 Al 0.3623(2) 0.75445(18) 0.30468(12) 0.0547(8) Uani 1 1 d . . . O1 O 0.3899(4) 0.8174(4) 0.3870(2) 0.0516(16) Uani 1 1 d . . . O2 O 0.3649(5) 0.6682(4) 0.3481(2) 0.0554(16) Uani 1 1 d . . . O5 O 0.3190(5) 0.8145(3) 0.4921(3) 0.0553(17) Uani 1 1 d . . . O3 O 0.5022(5) 0.7259(3) 0.4607(3) 0.0568(17) Uani 1 1 d . . . O6 O 0.2958(5) 0.6436(3) 0.4525(3) 0.0562(17) Uani 1 1 d . . . O9 O 0.7273(6) 0.8321(4) 0.4388(3) 0.073(2) Uani 1 1 d . . . O7 O 0.3186(5) 0.6795(4) 0.2248(3) 0.0651(18) Uani 1 1 d . . . O11 O 0.1799(5) 0.7439(4) 0.3873(3) 0.0640(18) Uani 1 1 d . . . O8 O 0.3523(5) 0.8489(4) 0.2703(3) 0.0638(18) Uani 1 1 d . . . O10 O 0.7253(6) 0.6515(4) 0.3987(3) 0.0657(19) Uani 1 1 d . . . O4 O 0.5207(5) 0.7460(4) 0.3101(3) 0.0589(17) Uani 1 1 d . . . O12 O 0.1921(5) 0.7606(4) 0.2962(3) 0.0663(19) Uani 1 1 d . . . C94 C 0.8360(11) 0.8244(7) 0.4516(4) 0.064(3) Uani 1 1 d . . . C4 C 0.5792(10) 0.7490(7) 0.2638(5) 0.079(3) Uani 1 1 d . . . H27A H 0.5194 0.7579 0.2285 0.094 Uiso 1 1 calc R . . C61 C 0.1366(9) 0.7539(6) 0.3343(5) 0.061(3) Uani 1 1 d . . . C54 C 0.2510(8) 0.6484(7) 0.4980(5) 0.058(3) Uani 1 1 d . . . C52 C 0.2678(8) 0.8027(6) 0.5323(4) 0.055(3) Uani 1 1 d . . . C92 C 0.8346(10) 0.6683(7) 0.4172(4) 0.057(3) Uani 1 1 d . . . C3 C 0.5474(8) 0.7182(6) 0.5224(4) 0.058(3) Uani 1 1 d . . . H36A H 0.4816 0.7223 0.5425 0.069 Uiso 1 1 calc R . . C31 C 0.6368(10) 0.7896(7) 0.5568(4) 0.116(5) Uani 1 1 d . . . H38A H 0.6005 0.8429 0.5576 0.174 Uiso 1 1 calc R . . H38B H 0.7008 0.7875 0.5370 0.174 Uiso 1 1 calc R . . H38C H 0.6669 0.7843 0.5981 0.174 Uiso 1 1 calc R . . C74 C 0.3070(9) 0.8521(8) 0.2156(6) 0.073(3) Uani 1 1 d . . . C53 C 0.2338(8) 0.7234(8) 0.5381(4) 0.066(3) Uani 1 1 d . . . H41A H 0.1986 0.7205 0.5697 0.079 Uiso 1 1 calc R . . C72 C 0.2774(9) 0.6993(8) 0.1753(5) 0.072(3) Uani 1 1 d . . . C73 C 0.2658(9) 0.7810(9) 0.1678(5) 0.079(3) Uani 1 1 d . . . H44A H 0.2291 0.7887 0.1293 0.095 Uiso 1 1 calc R . . C51 C 0.2504(8) 0.8812(6) 0.5785(4) 0.081(3) Uani 1 1 d . . . H46A H 0.2810 0.9305 0.5695 0.121 Uiso 1 1 calc R . . H46B H 0.2917 0.8775 0.6188 0.121 Uiso 1 1 calc R . . H46C H 0.1674 0.8857 0.5766 0.121 Uiso 1 1 calc R . . C1 C 0.4034(8) 0.9081(6) 0.4157(4) 0.064(3) Uani 1 1 d . . . H47A H 0.4279 0.9140 0.4601 0.077 Uiso 1 1 calc R . . C91 C 0.9099(8) 0.5920(6) 0.4090(5) 0.092(4) Uani 1 1 d . . . H52A H 0.8594 0.5410 0.3899 0.138 Uiso 1 1 calc R . . H52B H 0.9563 0.5878 0.4483 0.138 Uiso 1 1 calc R . . H52C H 0.9616 0.5987 0.3835 0.138 Uiso 1 1 calc R . . C32 C 0.5982(10) 0.6336(7) 0.5218(5) 0.103(4) Uani 1 1 d . . . H54A H 0.5381 0.5892 0.4997 0.154 Uiso 1 1 calc R . . H54B H 0.6264 0.6284 0.5632 0.154 Uiso 1 1 calc R . . H54C H 0.6628 0.6287 0.5022 0.154 Uiso 1 1 calc R . . C41 C 0.6710(10) 0.8216(8) 0.2825(5) 0.129(5) Uani 1 1 d . . . H57A H 0.6347 0.8743 0.2938 0.193 Uiso 1 1 calc R . . H57B H 0.7055 0.8223 0.2489 0.193 Uiso 1 1 calc R . . H57C H 0.7316 0.8146 0.3169 0.193 Uiso 1 1 calc R . . C55 C 0.2242(8) 0.5643(6) 0.5108(5) 0.087(3) Uani 1 1 d . . . H59A H 0.2429 0.5186 0.4801 0.131 Uiso 1 1 calc R . . H59B H 0.1417 0.5587 0.5099 0.131 Uiso 1 1 calc R . . H59C H 0.2711 0.5622 0.5505 0.131 Uiso 1 1 calc R . . C2 C 0.3552(10) 0.5785(6) 0.3198(5) 0.082(3) Uani 1 1 d . . . H61A H 0.3799 0.5727 0.2814 0.099 Uiso 1 1 calc R . . C21 C 0.2243(10) 0.5456(6) 0.3008(5) 0.107(4) Uani 1 1 d . . . H62A H 0.1779 0.5812 0.2777 0.161 Uiso 1 1 calc R . . H62B H 0.1965 0.5470 0.3369 0.161 Uiso 1 1 calc R . . H62C H 0.2167 0.4881 0.2761 0.161 Uiso 1 1 calc R . . C11 C 0.4991(8) 0.9539(6) 0.3994(4) 0.084(3) Uani 1 1 d . . . H64A H 0.5719 0.9263 0.4081 0.126 Uiso 1 1 calc R . . H64B H 0.5097 1.0120 0.4230 0.126 Uiso 1 1 calc R . . H64C H 0.4766 0.9526 0.3565 0.126 Uiso 1 1 calc R . . C71 C 0.2375(10) 0.6245(7) 0.1200(5) 0.110(4) Uani 1 1 d . . . H65A H 0.2487 0.5722 0.1327 0.165 Uiso 1 1 calc R . . H65B H 0.2833 0.6263 0.0908 0.165 Uiso 1 1 calc R . . H65C H 0.1551 0.6277 0.1014 0.165 Uiso 1 1 calc R . . C95 C 0.9154(9) 0.9051(6) 0.4777(5) 0.096(4) Uani 1 1 d . . . H68A H 0.8677 0.9536 0.4801 0.144 Uiso 1 1 calc R . . H68B H 0.9674 0.9080 0.4516 0.144 Uiso 1 1 calc R . . H68C H 0.9614 0.9050 0.5180 0.144 Uiso 1 1 calc R . . C93 C 0.8907(9) 0.7494(9) 0.4447(4) 0.070(3) Uani 1 1 d . . . H69A H 0.9726 0.7525 0.4597 0.084 Uiso 1 1 calc R . . C12 C 0.2852(9) 0.9486(6) 0.4033(5) 0.096(4) Uani 1 1 d . . . H71A H 0.2277 0.9182 0.4153 0.143 Uiso 1 1 calc R . . H71B H 0.2591 0.9463 0.3604 0.143 Uiso 1 1 calc R . . H71C H 0.2942 1.0070 0.4265 0.143 Uiso 1 1 calc R . . C75 C 0.3038(10) 0.9405(7) 0.2041(5) 0.111(4) Uani 1 1 d . . . H79A H 0.3352 0.9820 0.2421 0.166 Uiso 1 1 calc R . . H79B H 0.2234 0.9519 0.1873 0.166 Uiso 1 1 calc R . . H79C H 0.3507 0.9437 0.1757 0.166 Uiso 1 1 calc R . . C62 C 0.0039(8) 0.7647(8) 0.3177(4) 0.114(5) Uani 1 1 d . . . H81A H -0.0187 0.7761 0.2779 0.171 Uiso 1 1 calc R . . H81B H -0.0154 0.8114 0.3475 0.171 Uiso 1 1 calc R . . H81C H -0.0380 0.7133 0.3172 0.171 Uiso 1 1 calc R . . C42 C 0.6280(12) 0.6638(8) 0.2438(5) 0.141(5) Uani 1 1 d . . . H98A H 0.5654 0.6199 0.2318 0.211 Uiso 1 1 calc R . . H98B H 0.6883 0.6536 0.2772 0.211 Uiso 1 1 calc R . . H98C H 0.6616 0.6636 0.2097 0.211 Uiso 1 1 calc R . . Mn1A Mn 0.84858(13) 0.22961(10) 0.11138(6) 0.0678(5) Uani 1 1 d . . . Al1A Al 0.6112(2) 0.22966(18) 0.14879(12) 0.0569(9) Uani 1 1 d . . . Al2A Al 0.8257(2) 0.21196(18) 0.23881(12) 0.0560(8) Uani 1 1 d . . . O2A O 0.7463(5) 0.2950(4) 0.2026(2) 0.0590(17) Uani 1 1 d . . . O1A O 0.7177(5) 0.1456(4) 0.1681(2) 0.0574(16) Uani 1 1 d . . . O9A O 0.9006(6) 0.1456(4) 0.0404(3) 0.074(2) Uani 1 1 d . . . O8A O 0.8842(5) 0.1183(4) 0.2672(3) 0.0655(19) Uani 1 1 d . . . O3A O 0.6699(5) 0.2322(4) 0.0822(3) 0.0668(18) Uani 1 1 d . . . O10A O 0.9313(6) 0.3254(4) 0.0891(3) 0.080(2) Uani 1 1 d . . . O11A O 0.5453(5) 0.2252(4) 0.2169(3) 0.072(2) Uani 1 1 d . . . O5A O 0.4836(6) 0.1520(4) 0.1018(3) 0.0671(19) Uani 1 1 d . . . O4A O 0.9382(5) 0.2129(3) 0.1953(2) 0.0606(17) Uani 1 1 d . . . O7A O 0.9182(5) 0.2873(4) 0.3094(3) 0.0638(18) Uani 1 1 d . . . C61A C 0.5967(10) 0.2180(6) 0.2683(5) 0.067(3) Uani 1 1 d . . . O12A O 0.7081(6) 0.2121(4) 0.2868(3) 0.0672(19) Uani 1 1 d . . . O6A O 0.5169(7) 0.3209(4) 0.1412(3) 0.072(2) Uani 1 1 d . . . C3A C 0.6006(10) 0.2366(8) 0.0225(5) 0.092(4) Uani 1 1 d . . . H29A H 0.5188 0.2463 0.0254 0.110 Uiso 1 1 calc R . . C4A C 1.0646(9) 0.2070(7) 0.2162(4) 0.072(3) Uani 1 1 d . . . H30A H 1.0818 0.1996 0.2581 0.087 Uiso 1 1 calc R . . C92A C 0.9768(10) 0.3206(8) 0.0440(6) 0.075(3) Uani 1 1 d . . . C93A C 0.9860(8) 0.2451(9) 0.0030(5) 0.075(3) Uani 1 1 d . . . H37A H 1.0225 0.2498 -0.0278 0.090 Uiso 1 1 calc R . . C72A C 0.9854(8) 0.2699(8) 0.3566(4) 0.062(3) Uani 1 1 d . . . C74A C 0.9545(10) 0.1166(8) 0.3183(6) 0.070(3) Uani 1 1 d . . . C94A C 0.9485(8) 0.1636(8) 0.0014(4) 0.061(3) Uani 1 1 d . . . C52A C 0.3752(12) 0.1654(9) 0.0873(4) 0.074(3) Uani 1 1 d . . . C95A C 0.9654(9) 0.0888(7) -0.0489(4) 0.096(4) Uani 1 1 d . . . H49A H 0.9320 0.0374 -0.0438 0.143 Uiso 1 1 calc R . . H49B H 1.0484 0.0836 -0.0465 0.143 Uiso 1 1 calc R . . H49C H 0.9264 0.0978 -0.0881 0.143 Uiso 1 1 calc R . . C53A C 0.3344(11) 0.2436(11) 0.0967(6) 0.095(4) Uani 1 1 d . . . H50A H 0.2529 0.2477 0.0847 0.114 Uiso 1 1 calc R . . C73A C 1.0036(9) 0.1880(9) 0.3630(5) 0.074(3) Uani 1 1 d . . . H53A H 1.0518 0.1809 0.3995 0.089 Uiso 1 1 calc R . . C1A C 0.7006(10) 0.0543(7) 0.1443(5) 0.084(3) Uani 1 1 d . . . H55A H 0.6374 0.0524 0.1075 0.101 Uiso 1 1 calc R . . C54A C 0.4026(13) 0.3177(9) 0.1226(5) 0.085(4) Uani 1 1 d . . . C2A C 0.7548(10) 0.3892(7) 0.2238(6) 0.093(4) Uani 1 1 d . . . H58A H 0.6965 0.4040 0.1903 0.111 Uiso 1 1 calc R . . C21A C 0.6948(10) 0.4172(7) 0.2764(5) 0.107(4) Uani 1 1 d . . . H60A H 0.6165 0.3903 0.2649 0.160 Uiso 1 1 calc R . . H60B H 0.6901 0.4780 0.2857 0.160 Uiso 1 1 calc R . . H60C H 0.7402 0.4011 0.3120 0.160 Uiso 1 1 calc R . . C71A C 1.0458(9) 0.3467(7) 0.4050(4) 0.096(4) Uani 1 1 d . . . H63A H 1.0238 0.3973 0.3915 0.144 Uiso 1 1 calc R . . H63B H 1.1301 0.3430 0.4123 0.144 Uiso 1 1 calc R . . H63C H 1.0219 0.3488 0.4423 0.144 Uiso 1 1 calc R . . C51A C 0.2911(9) 0.0896(8) 0.0579(5) 0.123(5) Uani 1 1 d . . . H66A H 0.3339 0.0387 0.0560 0.185 Uiso 1 1 calc R . . H66B H 0.2510 0.0925 0.0172 0.185 Uiso 1 1 calc R . . H66C H 0.2340 0.0886 0.0817 0.185 Uiso 1 1 calc R . . C91A C 1.0243(9) 0.4012(7) 0.0361(5) 0.105(4) Uani 1 1 d . . . H67A H 1.0117 0.4481 0.0678 0.157 Uiso 1 1 calc R . . H67B H 0.9842 0.4095 -0.0032 0.157 Uiso 1 1 calc R . . H67C H 1.1076 0.3981 0.0386 0.157 Uiso 1 1 calc R . . C42A C 1.1301(10) 0.2850(9) 0.2168(7) 0.165(7) Uani 1 1 d . . . H76A H 1.1055 0.3331 0.2434 0.248 Uiso 1 1 calc R . . H76B H 1.1140 0.2932 0.1760 0.248 Uiso 1 1 calc R . . H76C H 1.2135 0.2797 0.2312 0.248 Uiso 1 1 calc R . . C75A C 0.9855(9) 0.0291(7) 0.3288(5) 0.105(4) Uani 1 1 d . . . H78A H 0.9434 -0.0143 0.2941 0.158 Uiso 1 1 calc R . . H78B H 0.9633 0.0228 0.3650 0.158 Uiso 1 1 calc R . . H78C H 1.0692 0.0235 0.3340 0.158 Uiso 1 1 calc R . . C41A C 1.1025(10) 0.1316(8) 0.1763(6) 0.157(6) Uani 1 1 d . . . H82A H 1.1862 0.1272 0.1905 0.235 Uiso 1 1 calc R . . H82B H 1.0849 0.1375 0.1349 0.235 Uiso 1 1 calc R . . H82C H 1.0610 0.0811 0.1777 0.235 Uiso 1 1 calc R . . C62A C 0.5260(9) 0.2181(8) 0.3149(4) 0.121(5) Uani 1 1 d . . . H83A H 0.5778 0.2118 0.3524 0.182 Uiso 1 1 calc R . . H83B H 0.4668 0.1717 0.2995 0.182 Uiso 1 1 calc R . . H83C H 0.4882 0.2710 0.3226 0.182 Uiso 1 1 calc R . . C12A C 0.6307(9) 0.0152(6) 0.1799(5) 0.099(4) Uani 1 1 d . . . H85A H 0.5667 0.0502 0.1875 0.149 Uiso 1 1 calc R . . H85B H 0.6819 0.0115 0.2182 0.149 Uiso 1 1 calc R . . H85C H 0.5992 -0.0409 0.1564 0.149 Uiso 1 1 calc R . . C32A C 0.6452(11) 0.3085(10) 0.0047(6) 0.182(8) Uani 1 1 d . . . H88A H 0.6424 0.3602 0.0349 0.272 Uiso 1 1 calc R . . H88B H 0.5971 0.3121 -0.0344 0.272 Uiso 1 1 calc R . . H88C H 0.7256 0.3004 0.0018 0.272 Uiso 1 1 calc R . . C11A C 0.7760(19) 0.0148(8) 0.1194(8) 0.275(14) Uani 1 1 d . . . H90A H 0.8037 0.0483 0.0958 0.413 Uiso 1 1 calc R . . H90B H 0.7404 -0.0386 0.0929 0.413 Uiso 1 1 calc R . . H90C H 0.8415 0.0047 0.1505 0.413 Uiso 1 1 calc R . . C22A C 0.8532(19) 0.4287(8) 0.2207(8) 0.275(13) Uani 1 1 d . . . H94A H 0.8712 0.4042 0.1821 0.412 Uiso 1 1 calc R . . H94B H 0.9178 0.4220 0.2535 0.412 Uiso 1 1 calc R . . H94C H 0.8412 0.4882 0.2245 0.412 Uiso 1 1 calc R . . C55A C 0.3533(11) 0.4059(8) 0.1333(6) 0.141(5) Uani 1 1 d . . . H95A H 0.4169 0.4482 0.1540 0.211 Uiso 1 1 calc R . . H95B H 0.2971 0.4082 0.1579 0.211 Uiso 1 1 calc R . . H95C H 0.3148 0.4167 0.0945 0.211 Uiso 1 1 calc R . . C22 C 0.4337(10) 0.5293(7) 0.3542(6) 0.126(5) Uani 1 1 d . . . H10A H 0.5136 0.5527 0.3632 0.189 Uiso 1 1 calc R . . H10B H 0.4282 0.4713 0.3306 0.189 Uiso 1 1 calc R . . H10C H 0.4116 0.5310 0.3918 0.189 Uiso 1 1 calc R . . C31A C 0.6002(11) 0.1518(9) -0.0229(5) 0.154(6) Uani 1 1 d . . . H10D H 0.5711 0.1071 -0.0084 0.232 Uiso 1 1 calc R . . H10E H 0.6794 0.1414 -0.0271 0.232 Uiso 1 1 calc R . . H10F H 0.5499 0.1531 -0.0620 0.232 Uiso 1 1 calc R . . C201 C 0.0790(15) 0.3324(12) -0.1467(7) 0.178(6) Uiso 1 1 d . . . H20A H 0.0038 0.3380 -0.1700 0.213 Uiso 1 1 calc R . . C205 C 0.207(2) 0.2371(16) -0.1085(11) 0.260(11) Uiso 1 1 d . . . H205 H 0.2335 0.1839 -0.1047 0.312 Uiso 1 1 calc R . . C203 C 0.1420(16) 0.4102(13) -0.1206(8) 0.198(7) Uiso 1 1 d D . . H20D H 0.1205 0.4631 -0.1274 0.237 Uiso 1 1 calc R . . C204 C 0.250(2) 0.3908(19) -0.0802(12) 0.252(11) Uiso 1 1 d . . . C207 C 0.314(3) 0.440(2) -0.0530(15) 0.48(3) Uiso 1 1 d D . . H20E H 0.2892 0.4937 -0.0614 0.725 Uiso 1 1 calc R . . H20F H 0.3891 0.4288 -0.0628 0.725 Uiso 1 1 calc R . . H20G H 0.3217 0.4432 -0.0104 0.725 Uiso 1 1 calc R . . C206 C 0.1002(17) 0.2479(13) -0.1467(8) 0.203(8) Uiso 1 1 d . . . H20H H 0.0471 0.2026 -0.1702 0.244 Uiso 1 1 calc R . . C202 C 0.2643(16) 0.3035(12) -0.0805(8) 0.181(7) Uiso 1 1 d D . . H20I H 0.3330 0.2954 -0.0528 0.217 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 Mn1 0.0464(10) 0.0739(12) 0.0738(11) 0.0230(9) 0.0162(8) 0.0041(9) Al1 0.047(2) 0.0508(19) 0.0567(18) 0.0145(15) 0.0141(15) 0.0004(15) Al2 0.051(2) 0.060(2) 0.0574(19) 0.0200(16) 0.0157(15) 0.0042(16) O1 0.050(4) 0.042(4) 0.062(4) 0.012(3) 0.013(3) -0.001(3) O2 0.061(4) 0.038(4) 0.064(4) 0.007(3) 0.016(3) 0.000(3) O5 0.057(4) 0.058(4) 0.060(4) 0.016(3) 0.028(4) 0.005(3) O3 0.050(4) 0.055(4) 0.072(4) 0.027(3) 0.015(3) 0.005(3) O6 0.056(4) 0.052(4) 0.066(4) 0.019(3) 0.019(4) 0.001(3) O9 0.049(5) 0.078(5) 0.088(5) 0.015(4) 0.015(4) 0.000(4) O7 0.067(5) 0.070(5) 0.063(5) 0.021(4) 0.020(4) 0.007(4) O11 0.052(4) 0.078(5) 0.069(5) 0.027(4) 0.018(4) 0.008(4) O8 0.058(5) 0.063(5) 0.074(5) 0.027(4) 0.015(4) 0.010(3) O10 0.039(4) 0.068(5) 0.085(5) 0.020(4) 0.003(4) 0.009(4) O4 0.057(4) 0.072(5) 0.056(4) 0.020(3) 0.026(3) 0.006(3) O12 0.052(5) 0.092(5) 0.063(5) 0.027(4) 0.022(4) 0.008(4) C94 0.052(9) 0.068(9) 0.077(8) 0.024(7) 0.020(7) -0.005(8) C4 0.077(9) 0.094(9) 0.072(8) 0.031(7) 0.019(7) 0.021(8) C61 0.045(8) 0.074(8) 0.058(8) 0.011(6) 0.009(7) 0.007(6) C54 0.048(7) 0.070(9) 0.058(7) 0.018(7) 0.013(6) 0.000(6) C52 0.043(7) 0.050(8) 0.063(7) 0.005(6) 0.005(6) -0.001(5) C92 0.041(8) 0.077(9) 0.059(7) 0.028(6) 0.011(6) 0.026(7) C3 0.045(7) 0.081(8) 0.060(7) 0.044(6) 0.011(5) 0.023(6) C31 0.129(11) 0.143(12) 0.057(7) 0.021(7) -0.012(7) -0.051(10) C74 0.066(8) 0.092(10) 0.067(9) 0.034(8) 0.016(7) 0.002(7) C53 0.060(7) 0.078(9) 0.060(7) 0.014(7) 0.019(6) -0.009(7) C72 0.078(8) 0.086(10) 0.058(8) 0.035(8) 0.008(7) 0.014(7) C73 0.070(8) 0.117(11) 0.054(8) 0.047(9) -0.002(6) 0.014(8) C51 0.096(9) 0.072(8) 0.077(7) 0.011(7) 0.034(6) 0.013(6) C1 0.051(7) 0.058(8) 0.082(7) 0.016(6) 0.017(6) -0.008(6) C91 0.056(7) 0.101(9) 0.121(9) 0.042(8) 0.012(7) 0.021(7) C32 0.109(10) 0.106(10) 0.100(9) 0.048(8) 0.017(7) 0.022(8) C41 0.103(10) 0.163(13) 0.133(11) 0.048(10) 0.044(9) -0.053(10) C55 0.090(8) 0.067(8) 0.132(10) 0.053(7) 0.049(7) 0.008(6) C2 0.101(10) 0.051(8) 0.089(8) 0.028(7) 0.003(7) -0.004(7) C21 0.109(11) 0.074(9) 0.117(9) -0.004(7) 0.012(8) -0.026(8) C11 0.083(8) 0.066(8) 0.109(9) 0.015(7) 0.041(7) 0.010(7) C71 0.133(11) 0.098(10) 0.079(8) -0.002(8) 0.010(8) -0.006(8) C95 0.083(9) 0.083(9) 0.109(9) 0.027(7) -0.006(7) -0.031(7) C93 0.042(8) 0.089(10) 0.071(7) 0.019(7) -0.002(6) -0.009(8) C12 0.076(8) 0.080(8) 0.147(10) 0.039(8) 0.049(8) 0.038(7) C75 0.136(11) 0.083(9) 0.120(10) 0.061(8) 0.007(8) 0.004(8) C62 0.054(9) 0.219(15) 0.074(8) 0.057(9) 0.006(6) 0.036(8) C42 0.187(15) 0.148(13) 0.132(11) 0.047(10) 0.113(11) 0.057(11) Mn1A 0.0654(12) 0.0796(12) 0.0644(10) 0.0221(9) 0.0229(9) 0.0062(9) Al1A 0.057(2) 0.064(2) 0.0469(17) 0.0145(16) 0.0074(16) 0.0083(17) Al2A 0.061(2) 0.057(2) 0.0513(18) 0.0158(16) 0.0145(16) 0.0096(16) O2A 0.052(4) 0.053(4) 0.059(4) 0.005(3) -0.001(3) 0.006(3) O1A 0.061(4) 0.052(5) 0.059(4) 0.009(3) 0.018(3) 0.004(3) O9A 0.090(5) 0.078(5) 0.067(5) 0.023(4) 0.040(4) 0.010(4) O8A 0.059(5) 0.068(5) 0.067(5) 0.022(4) 0.007(4) 0.007(4) O3A 0.065(5) 0.077(5) 0.057(4) 0.020(4) 0.010(4) 0.001(4) O10A 0.085(6) 0.085(6) 0.076(5) 0.022(4) 0.032(4) -0.002(4) O11A 0.049(5) 0.108(6) 0.050(4) 0.016(4) -0.001(4) 0.014(4) O5A 0.046(5) 0.086(5) 0.062(4) 0.011(4) 0.006(4) 0.002(4) O4A 0.050(5) 0.063(4) 0.065(4) 0.015(3) 0.009(4) 0.002(3) O7A 0.056(5) 0.069(5) 0.055(4) 0.001(4) 0.009(4) 0.011(4) C61A 0.042(8) 0.101(9) 0.059(8) 0.007(7) 0.027(7) 0.008(7) O12A 0.051(5) 0.098(5) 0.054(4) 0.015(4) 0.020(4) 0.010(4) O6A 0.067(5) 0.075(5) 0.068(4) 0.024(4) -0.003(4) 0.024(4) C3A 0.078(9) 0.133(12) 0.059(8) 0.034(8) -0.001(7) 0.007(8) C4A 0.036(8) 0.103(10) 0.072(7) 0.029(7) -0.007(6) 0.016(7) C92A 0.068(9) 0.073(10) 0.078(9) 0.024(8) 0.000(7) -0.008(7) C93A 0.051(7) 0.096(10) 0.092(9) 0.039(9) 0.029(6) 0.003(7) C72A 0.044(7) 0.098(10) 0.042(7) 0.021(7) 0.006(6) 0.006(7) C74A 0.054(8) 0.088(10) 0.078(9) 0.036(8) 0.022(7) 0.020(7) C94A 0.045(7) 0.090(10) 0.049(7) 0.028(7) 0.004(6) 0.015(7) C52A 0.064(11) 0.105(11) 0.046(7) 0.007(7) 0.014(7) 0.007(10) C95A 0.110(10) 0.107(10) 0.066(7) -0.002(7) 0.039(7) 0.019(7) C53A 0.046(9) 0.123(13) 0.102(10) 0.011(10) 0.004(7) 0.004(10) C73A 0.055(8) 0.110(11) 0.067(8) 0.049(9) 0.004(6) 0.016(8) C1A 0.108(10) 0.049(8) 0.093(8) 0.000(7) 0.041(7) -0.003(7) C54A 0.062(10) 0.114(12) 0.068(8) 0.022(8) -0.004(7) 0.052(9) C2A 0.074(9) 0.070(10) 0.121(10) -0.001(8) 0.023(8) -0.010(7) C21A 0.129(11) 0.084(9) 0.098(9) -0.003(7) 0.037(8) 0.033(8) C71A 0.082(8) 0.103(10) 0.077(8) -0.011(7) 0.005(7) -0.018(7) C51A 0.071(9) 0.133(12) 0.135(11) 0.005(9) -0.004(8) -0.045(9) C91A 0.107(10) 0.104(10) 0.116(10) 0.044(8) 0.036(8) -0.015(8) C42A 0.060(9) 0.141(13) 0.29(2) 0.100(14) -0.010(11) -0.034(9) C75A 0.113(10) 0.100(10) 0.111(9) 0.050(8) 0.019(8) 0.048(8) C41A 0.092(10) 0.160(14) 0.193(14) -0.023(11) 0.052(10) 0.062(10) C62A 0.067(8) 0.233(16) 0.070(8) 0.033(9) 0.036(7) 0.025(9) C12A 0.122(10) 0.070(8) 0.111(9) 0.013(7) 0.051(8) -0.022(7) C32A 0.123(12) 0.27(2) 0.195(15) 0.184(16) -0.014(10) -0.047(12) C11A 0.51(4) 0.061(11) 0.36(3) -0.021(13) 0.36(3) 0.016(15) C22A 0.44(3) 0.076(11) 0.39(3) -0.016(14) 0.35(3) -0.054(16) C55A 0.117(11) 0.116(12) 0.176(13) 0.025(10) 0.021(10) 0.052(9) C22 0.108(10) 0.065(8) 0.191(13) 0.022(9) 0.019(10) 0.040(8) C31A 0.141(13) 0.208(17) 0.064(9) -0.026(10) -0.012(8) 0.025(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn1 O3 2.038(6) . ? Mn1 O4 2.042(6) . ? Mn1 O9 2.056(7) . ? Mn1 O10 2.086(6) . ? Mn1 Al2 3.078(3) . ? Mn1 Al1 3.091(3) . ? Al1 O3 1.838(6) . ? Al1 O5 1.874(6) . ? Al1 O6 1.881(6) . ? Al1 O2 1.894(6) . ? Al1 O1 1.899(6) . ? Al1 O11 1.939(7) . ? Al1 Al2 2.919(4) . ? Al2 O4 1.826(6) . ? Al2 O8 1.878(7) . ? Al2 O1 1.885(6) . ? Al2 O2 1.904(6) . ? Al2 O7 1.905(7) . ? Al2 O12 1.949(7) . ? O1 C1 1.452(9) . ? O2 C2 1.434(10) . ? O5 C52 1.269(10) . ? O3 C3 1.437(9) . ? O6 C54 1.267(10) . ? O9 C94 1.242(11) . ? O7 C72 1.249(10) . ? O11 C61 1.260(10) . ? O8 C74 1.266(10) . ? O10 C92 1.249(10) . ? O4 C4 1.409(10) . ? O12 C61 1.235(10) . ? C94 C93 1.365(13) . ? C94 C95 1.510(12) . ? C4 C41 1.497(12) . ? C4 C42 1.502(13) . ? C61 C62 1.521(12) . ? C54 C53 1.388(12) . ? C54 C55 1.508(11) . ? C52 C53 1.388(11) . ? C52 C51 1.499(11) . ? C92 C93 1.399(13) . ? C92 C91 1.516(12) . ? C3 C31 1.488(12) . ? C3 C32 1.491(11) . ? C74 C73 1.383(13) . ? C74 C75 1.517(12) . ? C72 C73 1.378(13) . ? C72 C71 1.515(13) . ? C1 C11 1.505(11) . ? C1 C12 1.519(11) . ? C2 C22 1.437(12) . ? C2 C21 1.539(12) . ? Mn1A O3A 2.032(6) . ? Mn1A O10A 2.053(7) . ? Mn1A O4A 2.057(6) . ? Mn1A O9A 2.078(6) . ? Mn1A Al1A 3.085(3) . ? Mn1A Al2A 3.105(3) . ? Al1A O3A 1.837(6) . ? Al1A O6A 1.858(7) . ? Al1A O5A 1.883(7) . ? Al1A O2A 1.892(6) . ? Al1A O1A 1.903(6) . ? Al1A O11A 1.927(7) . ? Al1A Al2A 2.912(4) . ? Al2A O4A 1.833(6) . ? Al2A O8A 1.861(7) . ? Al2A O7A 1.877(7) . ? Al2A O2A 1.881(6) . ? Al2A O1A 1.895(6) . ? Al2A O12A 1.957(7) . ? O2A C2A 1.481(11) . ? O1A C1A 1.443(10) . ? O9A C94A 1.257(10) . ? O8A C74A 1.276(11) . ? O3A C3A 1.444(10) . ? O10A C92A 1.264(12) . ? O11A C61A 1.232(10) . ? O5A C52A 1.259(12) . ? O4A C4A 1.447(10) . ? O7A C72A 1.276(10) . ? C61A O12A 1.277(11) . ? C61A C62A 1.503(12) . ? O6A C54A 1.294(12) . ? C3A C32A 1.459(14) . ? C3A C31A 1.515(14) . ? C4A C42A 1.470(13) . ? C4A C41A 1.481(13) . ? C92A C93A 1.378(13) . ? C92A C91A 1.485(12) . ? C93A C94A 1.378(13) . ? C72A C73A 1.380(13) . ? C72A C71A 1.501(12) . ? C74A C73A 1.370(13) . ? C74A C75A 1.524(13) . ? C94A C95A 1.515(12) . ? C52A C53A 1.340(14) . ? C52A C51A 1.486(13) . ? C53A C54A 1.361(15) . ? C1A C11A 1.256(15) . ? C1A C12A 1.519(12) . ? C54A C55A 1.525(14) . ? C2A C22A 1.336(15) . ? C2A C21A 1.523(13) . ? C201 C203 1.38(2) . ? C201 C206 1.39(2) . ? C205 C202 1.22(2) . ? C205 C206 1.39(2) . ? C203 C204 1.46(3) . ? C204 C207 1.06(4) . ? C204 C202 1.42(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 O3 Mn1 O4 126.1(2) . . ? O3 Mn1 O9 109.0(2) . . ? O4 Mn1 O9 109.6(2) . . ? O3 Mn1 O10 108.5(2) . . ? O4 Mn1 O10 109.9(2) . . ? O9 Mn1 O10 86.8(3) . . ? O3 Mn1 Al2 91.40(17) . . ? O4 Mn1 Al2 34.91(17) . . ? O9 Mn1 Al2 126.0(2) . . ? O10 Mn1 Al2 134.11(19) . . ? O3 Mn1 Al1 34.92(16) . . ? O4 Mn1 Al1 91.27(17) . . ? O9 Mn1 Al1 126.9(2) . . ? O10 Mn1 Al1 132.06(19) . . ? Al2 Mn1 Al1 56.49(7) . . ? O3 Al1 O5 94.0(3) . . ? O3 Al1 O6 92.7(2) . . ? O5 Al1 O6 91.5(3) . . ? O3 Al1 O2 91.0(3) . . ? O5 Al1 O2 169.6(3) . . ? O6 Al1 O2 97.4(3) . . ? O3 Al1 O1 89.9(3) . . ? O5 Al1 O1 94.0(3) . . ? O6 Al1 O1 173.7(3) . . ? O2 Al1 O1 76.9(3) . . ? O3 Al1 O11 178.9(3) . . ? O5 Al1 O11 84.9(3) . . ? O6 Al1 O11 87.3(3) . . ? O2 Al1 O11 90.1(3) . . ? O1 Al1 O11 90.2(2) . . ? O3 Al1 Al2 100.9(2) . . ? O5 Al1 Al2 130.0(2) . . ? O6 Al1 Al2 134.4(2) . . ? O2 Al1 Al2 39.89(18) . . ? O1 Al1 Al2 39.33(18) . . ? O11 Al1 Al2 79.8(2) . . ? O3 Al1 Mn1 39.41(18) . . ? O5 Al1 Mn1 117.9(2) . . ? O6 Al1 Mn1 120.3(2) . . ? O2 Al1 Mn1 61.81(18) . . ? O1 Al1 Mn1 59.33(17) . . ? O11 Al1 Mn1 141.3(2) . . ? Al2 Al1 Mn1 61.53(8) . . ? O4 Al2 O8 94.1(3) . . ? O4 Al2 O1 92.0(3) . . ? O8 Al2 O1 96.3(3) . . ? O4 Al2 O2 89.9(3) . . ? O8 Al2 O2 172.3(3) . . ? O1 Al2 O2 77.0(2) . . ? O4 Al2 O7 93.3(3) . . ? O8 Al2 O7 90.4(3) . . ? O1 Al2 O7 171.1(3) . . ? O2 Al2 O7 96.0(3) . . ? O4 Al2 O12 178.0(3) . . ? O8 Al2 O12 86.1(3) . . ? O1 Al2 O12 89.9(3) . . ? O2 Al2 O12 90.2(3) . . ? O7 Al2 O12 84.7(3) . . ? O4 Al2 Al1 101.6(2) . . ? O8 Al2 Al1 132.9(2) . . ? O1 Al2 Al1 39.69(17) . . ? O2 Al2 Al1 39.63(18) . . ? O7 Al2 Al1 132.0(2) . . ? O12 Al2 Al1 79.7(2) . . ? O4 Al2 Mn1 39.80(18) . . ? O8 Al2 Mn1 117.9(2) . . ? O1 Al2 Mn1 59.70(18) . . ? O2 Al2 Mn1 62.08(18) . . ? O7 Al2 Mn1 121.9(2) . . ? O12 Al2 Mn1 141.6(2) . . ? Al1 Al2 Mn1 61.98(8) . . ? C1 O1 Al2 132.8(5) . . ? C1 O1 Al1 123.7(5) . . ? Al2 O1 Al1 101.0(3) . . ? C2 O2 Al1 134.0(5) . . ? C2 O2 Al2 123.9(5) . . ? Al1 O2 Al2 100.5(3) . . ? C52 O5 Al1 128.2(6) . . ? C3 O3 Al1 125.3(5) . . ? C3 O3 Mn1 128.9(5) . . ? Al1 O3 Mn1 105.7(3) . . ? C54 O6 Al1 127.7(6) . . ? C94 O9 Mn1 128.5(7) . . ? C72 O7 Al2 127.1(7) . . ? C61 O11 Al1 126.9(6) . . ? C74 O8 Al2 128.8(7) . . ? C92 O10 Mn1 126.8(6) . . ? C4 O4 Al2 126.4(6) . . ? C4 O4 Mn1 128.2(5) . . ? Al2 O4 Mn1 105.3(3) . . ? C61 O12 Al2 127.2(6) . . ? O9 C94 C93 125.9(10) . . ? O9 C94 C95 117.4(10) . . ? C93 C94 C95 116.6(11) . . ? O4 C4 C41 112.8(9) . . ? O4 C4 C42 108.9(9) . . ? C41 C4 C42 113.0(10) . . ? O12 C61 O11 126.5(9) . . ? O12 C61 C62 117.1(9) . . ? O11 C61 C62 116.3(9) . . ? O6 C54 C53 125.3(9) . . ? O6 C54 C55 115.4(9) . . ? C53 C54 C55 119.0(9) . . ? O5 C52 C53 124.7(9) . . ? O5 C52 C51 116.0(9) . . ? C53 C52 C51 119.2(10) . . ? O10 C92 C93 125.9(9) . . ? O10 C92 C91 115.2(10) . . ? C93 C92 C91 118.9(10) . . ? O3 C3 C31 109.6(7) . . ? O3 C3 C32 110.0(8) . . ? C31 C3 C32 111.7(9) . . ? O8 C74 C73 124.0(10) . . ? O8 C74 C75 115.4(11) . . ? C73 C74 C75 120.6(11) . . ? C54 C53 C52 121.8(9) . . ? O7 C72 C73 125.9(10) . . ? O7 C72 C71 114.9(10) . . ? C73 C72 C71 119.2(10) . . ? C72 C73 C74 122.2(9) . . ? O1 C1 C11 113.3(8) . . ? O1 C1 C12 110.7(7) . . ? C11 C1 C12 112.5(8) . . ? O2 C2 C22 114.2(9) . . ? O2 C2 C21 109.7(9) . . ? C22 C2 C21 114.4(9) . . ? C94 C93 C92 125.8(10) . . ? O3A Mn1A O10A 110.1(2) . . ? O3A Mn1A O4A 125.5(2) . . ? O10A Mn1A O4A 110.7(2) . . ? O3A Mn1A O9A 105.5(2) . . ? O10A Mn1A O9A 87.1(3) . . ? O4A Mn1A O9A 111.1(2) . . ? O3A Mn1A Al1A 34.99(17) . . ? O10A Mn1A Al1A 128.7(2) . . ? O4A Mn1A Al1A 90.72(18) . . ? O9A Mn1A Al1A 128.8(2) . . ? O3A Mn1A Al2A 91.02(17) . . ? O10A Mn1A Al2A 129.6(2) . . ? O4A Mn1A Al2A 34.63(17) . . ? O9A Mn1A Al2A 131.81(19) . . ? Al1A Mn1A Al2A 56.11(7) . . ? O3A Al1A O6A 94.1(3) . . ? O3A Al1A O5A 93.5(3) . . ? O6A Al1A O5A 90.8(3) . . ? O3A Al1A O2A 90.9(3) . . ? O6A Al1A O2A 96.4(3) . . ? O5A Al1A O2A 171.3(3) . . ? O3A Al1A O1A 90.4(3) . . ? O6A Al1A O1A 171.8(3) . . ? O5A Al1A O1A 95.8(3) . . ? O2A Al1A O1A 76.7(3) . . ? O3A Al1A O11A 178.3(3) . . ? O6A Al1A O11A 85.6(3) . . ? O5A Al1A O11A 84.8(3) . . ? O2A Al1A O11A 90.9(3) . . ? O1A Al1A O11A 90.1(3) . . ? O3A Al1A Al2A 101.6(2) . . ? O6A Al1A Al2A 132.2(2) . . ? O5A Al1A Al2A 132.2(2) . . ? O2A Al1A Al2A 39.35(18) . . ? O1A Al1A Al2A 39.85(18) . . ? O11A Al1A Al2A 79.9(2) . . ? O3A Al1A Mn1A 39.36(19) . . ? O6A Al1A Mn1A 117.9(2) . . ? O5A Al1A Mn1A 121.3(2) . . ? O2A Al1A Mn1A 59.21(19) . . ? O1A Al1A Mn1A 62.41(18) . . ? O11A Al1A Mn1A 142.1(2) . . ? Al2A Al1A Mn1A 62.29(8) . . ? O4A Al2A O8A 93.4(3) . . ? O4A Al2A O7A 93.0(3) . . ? O8A Al2A O7A 91.1(3) . . ? O4A Al2A O2A 89.6(3) . . ? O8A Al2A O2A 171.1(3) . . ? O7A Al2A O2A 97.1(3) . . ? O4A Al2A O1A 90.9(3) . . ? O8A Al2A O1A 94.4(3) . . ? O7A Al2A O1A 173.0(3) . . ? O2A Al2A O1A 77.2(3) . . ? O4A Al2A O12A 178.8(3) . . ? O8A Al2A O12A 86.3(3) . . ? O7A Al2A O12A 85.8(3) . . ? O2A Al2A O12A 90.8(3) . . ? O1A Al2A O12A 90.3(3) . . ? O4A Al2A Al1A 101.2(2) . . ? O8A Al2A Al1A 131.4(2) . . ? O7A Al2A Al1A 133.3(2) . . ? O2A Al2A Al1A 39.62(18) . . ? O1A Al2A Al1A 40.06(18) . . ? O12A Al2A Al1A 79.9(2) . . ? O4A Al2A Mn1A 39.62(19) . . ? O8A Al2A Mn1A 119.8(2) . . ? O7A Al2A Mn1A 118.5(2) . . ? O2A Al2A Mn1A 58.77(18) . . ? O1A Al2A Mn1A 61.97(18) . . ? O12A Al2A Mn1A 141.4(2) . . ? Al1A Al2A Mn1A 61.60(8) . . ? C2A O2A Al2A 130.9(6) . . ? C2A O2A Al1A 124.5(5) . . ? Al2A O2A Al1A 101.0(3) . . ? C1A O1A Al2A 130.5(6) . . ? C1A O1A Al1A 127.7(6) . . ? Al2A O1A Al1A 100.1(3) . . ? C94A O9A Mn1A 127.6(7) . . ? C74A O8A Al2A 129.0(7) . . ? C3A O3A Al1A 125.8(6) . . ? C3A O3A Mn1A 128.5(6) . . ? Al1A O3A Mn1A 105.7(3) . . ? C92A O10A Mn1A 128.4(7) . . ? C61A O11A Al1A 128.7(6) . . ? C52A O5A Al1A 128.6(7) . . ? C4A O4A Al2A 127.5(5) . . ? C4A O4A Mn1A 126.7(5) . . ? Al2A O4A Mn1A 105.7(3) . . ? C72A O7A Al2A 128.6(7) . . ? O11A C61A O12A 125.3(9) . . ? O11A C61A C62A 119.1(10) . . ? O12A C61A C62A 115.6(10) . . ? C61A O12A Al2A 126.2(6) . . ? C54A O6A Al1A 126.9(7) . . ? O3A C3A C32A 110.0(9) . . ? O3A C3A C31A 109.2(9) . . ? C32A C3A C31A 113.4(11) . . ? O4A C4A C42A 111.2(8) . . ? O4A C4A C41A 109.4(9) . . ? C42A C4A C41A 110.6(11) . . ? O10A C92A C93A 123.7(11) . . ? O10A C92A C91A 117.5(11) . . ? C93A C92A C91A 118.8(12) . . ? C94A C93A C92A 128.8(10) . . ? O7A C72A C73A 123.7(10) . . ? O7A C72A C71A 114.2(10) . . ? C73A C72A C71A 122.1(11) . . ? O8A C74A C73A 124.0(10) . . ? O8A C74A C75A 116.8(11) . . ? C73A C74A C75A 119.2(11) . . ? O9A C94A C93A 123.9(10) . . ? O9A C94A C95A 115.6(10) . . ? C93A C94A C95A 120.5(10) . . ? O5A C52A C53A 123.0(12) . . ? O5A C52A C51A 117.1(12) . . ? C53A C52A C51A 119.9(13) . . ? C52A C53A C54A 125.3(12) . . ? C74A C73A C72A 123.4(10) . . ? C11A C1A O1A 119.3(11) . . ? C11A C1A C12A 122.6(11) . . ? O1A C1A C12A 111.0(9) . . ? O6A C54A C53A 123.5(11) . . ? O6A C54A C55A 112.4(13) . . ? C53A C54A C55A 124.0(13) . . ? C22A C2A O2A 116.2(11) . . ? C22A C2A C21A 123.3(11) . . ? O2A C2A C21A 110.1(9) . . ? C203 C201 C206 135.8(19) . . ? C202 C205 C206 114(2) . . ? C201 C203 C204 105(2) . . ? C207 C204 C202 123(2) . . ? C207 C204 C203 120(3) . . ? C202 C204 C203 117(3) . . ? C205 C206 C201 114(2) . . ? C205 C202 C204 135(3) . . ? _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 20.00 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 0.406 _refine_diff_density_min -0.448 _refine_diff_density_rms 0.060