Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_global # *** Added by check_cif _journal_coden_Cambridge 186 loop_ _publ_author_name _publ_author_address 'Isaac Abrahams' ; Department of Chemistry Queen Mary, University of London Mile End Road London E1 4NS UK ; 'Donald C. Bradley' ; Department of Chemistry Queen Mary, University of London Mile End Road London E1 4NS UK ; 'Halina Chudzynska' ; Department of Chemistry Queen Mary, University of London Mile End Road London E1 4NS UK ; 'Majid Motevalli' ; Department of Chemistry Queen Mary, University of London Mile End Road London E1 4NS UK ; 'Robin A. Sinclair' ; Ceramic technolgy Center 3M St. Paul Minnesota 5514-1000 USA ; _publ_contact_author_name 'Dr. Isaac Abrahams' _publ_contact_author_address ; Department of Chemistry Queen Mary, University of London Mile End Road London E1 4NS UK ; _publ_contact_author_email i.abrahams@qmul.ac.uk _publ_contact_author_fax '44(0)207 882 7794' _publ_contact_author_phone '44(0)207 882 3235' _publ_requested_journal 'J. Chem. Soc Dalton Trans' _publ_section_title ; New Polynuclear aluminium oxoalkoxides. Crystal Structures of [Al5(mu5-O)(mu-OBui)8(OBui)5], [Al8(mu4-O)2(mu-OH)2(mu-OBui)10(OBui)8] ; _publ_section_exptl_refinement ; Single crystals of both compounds were grown from toluene solutions. Summaries of data collection and structure refinement are given in Table 5. The intensity data for 2 were collected using a FAST area detector at 150(2) K. Data collection, reduction and cell refinement procedures are described elsewhere.^15 No absorption correction was carried out. Intensity data for 3 were collected on an Enraf Nonius CAD-4 diffractometer using MoK\a radiation (lambda = 0.71069 angstroms) with omega-2theta scans at 293(2) K. All data were corrected for absorption by empirical methods (psi-scan).^16 Both structures were solved by direct methods using the SHELXS-97 programme^17 and refined on F^2 using the SHELXL-97 programme.^17 Anisotropic parameters were refined for all non-hydrogen atoms. The H atoms were calculated geometrically and refined with a riding model. The structure of 2 crystallises in a tetragonal cell with no systematic absences in the data. A space group of P4 was chosen for the initial solution. However it was apparent that while the Al5O14 cores do indeed show tetragonal symmetry (P4cc), the apical isobutoxy ligand necessitates a lowering of the symmetry to triclinic P1. Isotropic refinement of the core atoms in the triclinic space group was possible but further refinement was hindered by the large number of variable parameters in this space group. The model presented here represents the averaged situation in the tetragonal space group P4. Restraints were required on thermal parameters and bond lengths in several of the isobutoxy ligands. In the case of 3 disorder in some of the isobutoxy ligands was modelled by splitting sites and refining using equal fixed occupancies. Molecular graphics were obtained using ORTEP3 for Windows.^18 ; #----------------------------- COMPOUND(S) DETAILS -------------------------# #--Structure 2 data_altnew _database_code_CSD 173335 _audit_creation_date 2001-10-10T14:29:01-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.1beta5 _audit_conform_dict_location ftp://ftp.iucr.org/cifdics/cif_core_2.1beta5.dic _publ_requested_category FM #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C52 H117 Al5 O14' _chemical_formula_structural 'C52 H117 AL5 O14' _chemical_formula_sum 'C52 H117 Al5 O14' _chemical_formula_weight 1101.36 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'P 4 c c' _symmetry_space_group_name_Hall 'P 4 -2c' _symmetry_Int_Tables_number 103 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, z+1/2' '-x, -y, z' 'x, -y, z+1/2' '-y, -x, z+1/2' 'y, -x, z' '-y, x, z' 'y, x, z+1/2' _cell_length_a 13.4930(10) _cell_length_b 13.4930(10) _cell_length_c 36.699(4) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 6681.5(10) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 250 _cell_measurement_theta_min 2.13 _cell_measurement_theta_max 27.27 _cell_measurement_wavelength 0.71069 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.5 _exptl_crystal_size_min 0.45 _exptl_crystal_density_diffrn 1.095 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2424 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.136 _exptl_absorpt_factor_muR 0.063 _exptl_absorpt_correction_type refdelf _exptl_absorpt_process_details ; Walker, N. & Stuart, D (1983) Acta. Cryst. A39, 158-166 ; _exptl_absorpt_correction_T_min 0.44 _exptl_absorpt_correction_T_max 1 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_reflns_number 28548 _diffrn_reflns_av_R_equivalents 0.0713 _diffrn_reflns_av_sigmaI/netI 0.0643 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -46 _diffrn_reflns_limit_l_max 46 _diffrn_reflns_theta_min 1.87 _diffrn_reflns_theta_max 27.17 _diffrn_reflns_theta_full 27.17 _diffrn_measured_fraction_theta_full 0.954 _diffrn_measured_fraction_theta_max 0.954 _reflns_number_total 6834 _reflns_number_gt 4449 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'MADNES MADONL (Pulgrath & Messerschmidt, 1989)' _computing_cell_refinement 'MADNES REFINE (Pulgrath & Messerschmidt, 1989)' _computing_data_reduction 'MADNES ABSURD (Pulgrath & Messerschmidt, 1989)' _computing_structure_solution 'SHELXS-97(Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0716P)^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_number_reflns 6834 _refine_ls_number_parameters 350 _refine_ls_number_restraints 26 _refine_ls_R_factor_all 0.0734 _refine_ls_R_factor_gt 0.0565 _refine_ls_wR_factor_ref 0.1335 _refine_ls_wR_factor_gt 0.1265 _refine_ls_goodness_of_fit_ref 0.903 _refine_ls_restrained_S_all 0.907 _refine_ls_shift/su_max 0.558 _refine_ls_shift/su_mean 0.035 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.21(18) _refine_diff_density_max 0.324 _refine_diff_density_min -0.288 _refine_diff_density_rms 0.068 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 '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' 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 Al11 Al 0 0 0.4631(2) 0.0481(5) Uani 1 4 d SD . . Al12 Al 0.87095(6) 0.08202(6) 0.4044(2) 0.0458(2) Uani 1 1 d . . . O13 O 0.83586(15) -0.03674(16) 0.3839(2) 0.0526(6) Uani 1 1 d . . . O14 O 0.76205(16) 0.14488(16) 0.3964(2) 0.0631(7) Uani 1 1 d . . . O15 O 0.88378(16) 0.08094(16) 0.4531(2) 0.0540(6) Uani 1 1 d . . . O16 O 0 0 0.4115(2) 0.0396(9) Uani 1 4 d S . . O17 O 0 0 0.5103(3) 0.0891(18) Uani 1 4 d SD . . Al21 Al 0.5 0.5 0.1150(2) 0.0511(5) Uani 1 4 d S . . Al22 Al 0.43604(8) 0.36079(8) 0.1740(2) 0.0557(3) Uani 1 1 d . . . O23 O 0.5565(2) 0.34476(17) 0.1949(2) 0.0639(7) Uani 1 1 d . . . O24 O 0.38274(19) 0.24710(19) 0.1815(2) 0.0693(7) Uani 1 1 d . . . O25 O 0.44818(16) 0.36641(16) 0.1252(2) 0.0527(6) Uani 1 1 d . . . O26 O 0.5 0.5 0.1662(2) 0.0512(12) Uani 1 4 d S . . O27 O 0.5 0.5 0.0682(2) 0.0584(12) Uani 1 4 d SD . . C131 C 0.7419(2) -0.0599(2) 0.3671(2) 0.0549(8) Uani 1 1 d . . . H13A H 0.7134 -0.1169 0.3793 0.066 Uiso 1 1 calc R . . H13B H 0.6972 -0.0044 0.3706 0.066 Uiso 1 1 calc R . . C132 C 0.7485(4) -0.0810(5) 0.3286(2) 0.114(2) Uani 1 1 d D . . H132 H 0.7766 -0.148 0.3294 0.137 Uiso 1 1 calc R . . C133 C 0.8102(5) -0.0380(8) 0.3044(3) 0.191(4) Uani 1 1 d D . . H13C H 0.8013 -0.068 0.2809 0.287 Uiso 1 1 calc R . . H13D H 0.8775 -0.047 0.3122 0.287 Uiso 1 1 calc R . . H13E H 0.7957 0.0315 0.3029 0.287 Uiso 1 1 calc R . . C134 C 0.6446(4) -0.1041(5) 0.3136(2) 0.123(2) Uani 1 1 d . . . H13F H 0.6076 -0.1407 0.3315 0.184 Uiso 1 1 calc R . . H13G H 0.6505 -0.1428 0.2918 0.184 Uiso 1 1 calc R . . H13H H 0.6108 -0.0432 0.3082 0.184 Uiso 1 1 calc R . . C141 C 0.6933(3) 0.2134(3) 0.3888(3) 0.1007(17) Uani 1 1 d . . . H14A H 0.695 0.2218 0.3625 0.121 Uiso 1 1 calc R . . H14B H 0.718 0.2748 0.3991 0.121 Uiso 1 1 calc R . . C142 C 0.5954(3) 0.2095(5) 0.3979(3) 0.150(3) Uani 1 1 d . . . H142 H 0.5802 0.1694 0.3763 0.18 Uiso 1 1 calc R . . C143 C 0.5270(3) 0.2894(3) 0.3855(2) 0.0882(13) Uani 1 1 d . . . H14C H 0.4612 0.2757 0.3941 0.132 Uiso 1 1 calc R . . H14D H 0.5269 0.2921 0.3594 0.132 Uiso 1 1 calc R . . H14E H 0.5489 0.3519 0.3951 0.132 Uiso 1 1 calc R . . C144 C 0.5532(4) 0.1351(4) 0.4219(3) 0.120(2) Uani 1 1 d . . . H14F H 0.4834 0.1466 0.4245 0.18 Uiso 1 1 calc R . . H14G H 0.5845 0.1391 0.4453 0.18 Uiso 1 1 calc R . . H14H H 0.5639 0.0705 0.4117 0.18 Uiso 1 1 calc R . . C151 C 0.8165(3) 0.1275(3) 0.4786(2) 0.0684(10) Uani 1 1 d . . . H15A H 0.7977 0.0792 0.497 0.082 Uiso 1 1 calc R . . H15B H 0.7568 0.1468 0.4657 0.082 Uiso 1 1 calc R . . C152 C 0.8592(3) 0.2181(3) 0.4975(2) 0.0735(10) Uani 1 1 d . . . H152 H 0.9187 0.1979 0.5109 0.088 Uiso 1 1 calc R . . C153 C 0.7836(4) 0.2558(4) 0.5247(2) 0.1110(17) Uani 1 1 d . . . H15C H 0.8095 0.3131 0.537 0.167 Uiso 1 1 calc R . . H15D H 0.7696 0.2049 0.5422 0.167 Uiso 1 1 calc R . . H15E H 0.7237 0.2733 0.5121 0.167 Uiso 1 1 calc R . . C154 C 0.8877(3) 0.2994(3) 0.4708(2) 0.0851(13) Uani 1 1 d . . . H15F H 0.916 0.3542 0.4838 0.128 Uiso 1 1 calc R . . H15G H 0.8298 0.3212 0.4579 0.128 Uiso 1 1 calc R . . H15H H 0.9354 0.274 0.4537 0.128 Uiso 1 1 calc R . . C171 C 0.006(2) -0.0394(10) 0.5434(3) 0.075(4) Uani 0.25 1 d PD . . H17A H 0.0685 -0.0743 0.5434 0.09 Uiso 0.25 1 calc PR . . H17B H -0.0447 -0.0906 0.5434 0.09 Uiso 0.25 1 calc PR . . C172 C 0 0 0.5772(3) 0.238(7) Uani 1 4 d SD . . H172 H -0.0354 -0.0407 0.5951 0.285 Uiso 0.25 1 calc PR . . C173 C 0.1081(12) 0.007(4) 0.5831(8) 0.48(3) Uani 0.5 1 d PD . . H17C H 0.1207 0.0291 0.6076 0.721 Uiso 0.5 1 calc PR . . H17D H 0.1357 0.0544 0.5663 0.721 Uiso 0.5 1 calc PR . . H17E H 0.1381 -0.0563 0.5793 0.721 Uiso 0.5 1 calc PR . . C231 C 0.5917(3) 0.2540(3) 0.2124(3) 0.0826(13) Uani 1 1 d . . . H23A H 0.6632 0.2501 0.21 0.099 Uiso 1 1 calc R . . H23B H 0.5634 0.1971 0.2 0.099 Uiso 1 1 calc R . . C232 C 0.5642(6) 0.2497(5) 0.2525(3) 0.146(3) Uani 1 1 d . . . H232 H 0.4918 0.2505 0.2546 0.175 Uiso 1 1 calc R . . C233 C 0.6041(6) 0.3327(6) 0.2730(3) 0.156(3) Uani 1 1 d . . . H23C H 0.5829 0.3282 0.2979 0.234 Uiso 1 1 calc R . . H23D H 0.5805 0.3936 0.2626 0.234 Uiso 1 1 calc R . . H23E H 0.6752 0.3312 0.2719 0.234 Uiso 1 1 calc R . . C234 C 0.6031(7) 0.1505(8) 0.2678(3) 0.222(5) Uani 1 1 d . . . H23F H 0.5871 0.1458 0.2932 0.332 Uiso 1 1 calc R . . H23G H 0.6737 0.1474 0.2647 0.332 Uiso 1 1 calc R . . H23H H 0.5727 0.0966 0.2549 0.332 Uiso 1 1 calc R . . C241 C 0.1587(3) 0.3638(3) 0.6962(2) 0.147(5) Uani 0.475(6) 1 d PD A 1 H24A H 0.1235 0.4256 0.6999 0.176 Uiso 0.475(6) 1 calc PR A 1 H24B H 0.1677 0.3326 0.7198 0.176 Uiso 0.475(6) 1 calc PR A 1 C242 C 0.0996(3) 0.2990(3) 0.67293(18) 0.178(8) Uani 0.475(6) 1 d PD A 1 H242 H 0.1047 0.3203 0.6475 0.214 Uiso 0.475(6) 1 calc PR A 1 C243 C 0.1366(4) 0.2028(3) 0.6767(4) 0.338(10) Uani 0.475(6) 1 d PD A 1 H24C H 0.1021 0.1593 0.6604 0.507 Uiso 0.475(6) 1 calc PR A 1 H24D H 0.1271 0.1808 0.7013 0.507 Uiso 0.475(6) 1 calc PR A 1 H24E H 0.206 0.2023 0.671 0.507 Uiso 0.475(6) 1 calc PR A 1 C244 C 0.0013(2) 0.3050(6) 0.6847(4) 0.338(10) Uani 0.475(6) 1 d PD A 1 H24F H -0.0236 0.3705 0.6803 0.507 Uiso 0.475(6) 1 calc PR A 1 H24G H -0.0019 0.2908 0.7103 0.507 Uiso 0.475(6) 1 calc PR A 1 H24H H -0.0381 0.2577 0.6716 0.507 Uiso 0.475(6) 1 calc PR A 1 C245 C 0.1925(3) 0.2955(4) 0.6750(3) 0.147(5) Uani 0.525(6) 1 d PD A 2 H24I H 0.235 0.2393 0.6803 0.176 Uiso 0.525(6) 1 calc PR A 2 H24J H 0.1769 0.2929 0.6492 0.176 Uiso 0.525(6) 1 calc PR A 2 C246 C 0.1005(6) 0.2831(7) 0.6953(2) 0.178(8) Uani 0.525(6) 1 d PD A 2 H246 H 0.1136 0.2866 0.7215 0.214 Uiso 0.525(6) 1 calc PR A 2 C247 C 0.0615(8) 0.1903(7) 0.6864(6) 0.338(10) Uani 0.525(6) 1 d PD A 2 H24K H 0.1068 0.1394 0.6939 0.507 Uiso 0.525(6) 1 calc PR A 2 H24L H 0.0516 0.1865 0.6605 0.507 Uiso 0.525(6) 1 calc PR A 2 H24M H -0.0008 0.1813 0.6986 0.507 Uiso 0.525(6) 1 calc PR A 2 C248 C 0.0364(6) 0.3593(8) 0.6849(6) 0.338(10) Uani 0.525(6) 1 d PD A 2 H24N H -0.0217 0.3578 0.7 0.507 Uiso 0.525(6) 1 calc PR A 2 H24O H 0.0175 0.3505 0.6599 0.507 Uiso 0.525(6) 1 calc PR A 2 H24P H 0.0692 0.4219 0.6877 0.507 Uiso 0.525(6) 1 calc PR A 2 C251 C 0.4207(3) 0.2915(2) 0.0999(2) 0.0571(8) Uani 1 1 d . . . H25A H 0.3862 0.3225 0.0797 0.069 Uiso 1 1 calc R . . H25B H 0.3744 0.2468 0.1117 0.069 Uiso 1 1 calc R . . C252 C 0.5063(3) 0.2307(3) 0.0847(2) 0.0643(9) Uani 1 1 d . . . H252 H 0.5507 0.2755 0.0715 0.077 Uiso 1 1 calc R . . C253 C 0.5638(3) 0.1826(3) 0.1144(2) 0.0909(14) Uani 1 1 d . . . H25C H 0.5876 0.2323 0.1309 0.136 Uiso 1 1 calc R . . H25D H 0.619 0.1474 0.1042 0.136 Uiso 1 1 calc R . . H25E H 0.5218 0.137 0.1273 0.136 Uiso 1 1 calc R . . C254 C 0.4677(4) 0.1545(3) 0.0583(3) 0.0986(16) Uani 1 1 d . . . H25F H 0.5222 0.1171 0.0486 0.148 Uiso 1 1 calc R . . H25G H 0.4333 0.1871 0.0388 0.148 Uiso 1 1 calc R . . H25H H 0.4231 0.1105 0.0708 0.148 Uiso 1 1 calc R . . C271 C 0.4718(19) 0.5402(17) 0.0352(4) 0.075(4) Uani 0.25 1 d PD . . H27A H 0.3999 0.5421 0.0352 0.09 Uiso 0.25 1 calc PR . . H27B H 0.4943 0.6084 0.0352 0.09 Uiso 0.25 1 calc PR . . C272 C 0.5 0.5 0.0032(5) 0.238(7) Uani 1 4 d SD . . H272 H 0.4566 0.4422 0.0058 0.285 Uiso 0.25 1 calc PR . . C273 C 0.437(4) 0.547(6) -0.0212(8) 0.48(3) Uani 0.5 1 d PD . . H27C H 0.4308 0.5074 -0.0428 0.721 Uiso 0.5 1 calc PR . . H27D H 0.4644 0.6106 -0.0275 0.721 Uiso 0.5 1 calc PR . . H27E H 0.3734 0.5559 -0.0102 0.721 Uiso 0.5 1 calc PR . . 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 Al11 0.0609(7) 0.0609(7) 0.0226(9) 0 0 0 Al12 0.0438(4) 0.0441(4) 0.0493(6) 0.0021(5) -0.0001(5) -0.0012(4) O13 0.0449(11) 0.0567(12) 0.0563(15) 0.0037(11) 0.0012(10) -0.0037(10) O14 0.0499(11) 0.0539(12) 0.085(2) -0.0004(12) 0.0063(12) -0.0022(11) O15 0.0570(12) 0.0528(12) 0.0523(16) -0.0034(10) 0.0091(11) 0.0041(10) O16 0.0463(12) 0.0463(12) 0.026(2) 0 0 0 O17 0.099(3) 0.099(3) 0.069(5) 0 0 0 Al21 0.0437(6) 0.0437(6) 0.0658(15) 0 0 0 Al22 0.0585(6) 0.0563(5) 0.0523(7) 0.0027(5) 0.0050(5) -0.0013(5) O23 0.0814(16) 0.0526(13) 0.0576(17) 0.0124(11) 0.0038(13) 0.0104(12) O24 0.0740(15) 0.0682(15) 0.0658(18) 0.0126(13) 0.0137(13) -0.0029(13) O25 0.0528(11) 0.0498(11) 0.0556(17) -0.0019(10) 0.0037(11) -0.0063(10) O26 0.0459(13) 0.0459(13) 0.062(4) 0 0 0 O27 0.0694(18) 0.0694(18) 0.037(3) 0 0 0 C131 0.0476(16) 0.0402(15) 0.077(3) 0.0038(16) -0.0134(17) 0.0017(13) C132 0.129(4) 0.176(5) 0.038(2) 0.017(3) -0.028(3) -0.094(4) C133 0.132(5) 0.364(14) 0.077(4) 0.009(7) -0.027(4) -0.037(7) C134 0.110(4) 0.187(6) 0.072(3) 0.017(3) -0.039(3) -0.081(4) C141 0.073(3) 0.083(3) 0.146(5) 0.049(3) 0.038(3) 0.020(2) C142 0.066(3) 0.117(4) 0.268(9) 0.065(5) 0.031(4) 0.020(3) C143 0.064(2) 0.100(3) 0.101(3) -0.009(3) -0.015(2) 0.036(2) C144 0.073(3) 0.137(4) 0.150(5) 0.041(4) 0.031(3) -0.001(3) C151 0.0605(19) 0.077(2) 0.068(3) -0.005(2) 0.0183(19) 0.0035(19) C152 0.092(3) 0.068(2) 0.060(2) -0.0172(19) 0.009(2) 0.013(2) C153 0.118(4) 0.114(4) 0.101(4) -0.031(3) 0.047(3) 0.009(3) C154 0.095(3) 0.068(2) 0.092(4) -0.025(2) 0.006(3) 0.010(2) C171 0.063(7) 0.096(10) 0.067(5) 0.005(5) -0.008(8) 0.006(6) C172 0.305(12) 0.305(12) 0.103(8) 0 0 0 C173 0.44(4) 0.53(5) 0.47(4) -0.23(5) -0.26(4) 0.22(4) C231 0.067(2) 0.084(3) 0.096(3) 0.043(3) 0.008(2) 0.013(2) C232 0.165(6) 0.129(5) 0.144(7) 0.068(5) 0.050(5) 0.054(5) C233 0.176(6) 0.191(7) 0.102(5) 0.086(5) -0.061(5) -0.087(6) C234 0.170(7) 0.253(10) 0.242(11) 0.192(9) 0.035(7) 0.056(7) C241 0.076(5) 0.148(10) 0.216(15) 0.059(9) -0.018(6) -0.048(6) C242 0.070(3) 0.115(6) 0.35(2) 0.043(9) -0.013(8) -0.040(4) C243 0.167(9) 0.118(6) 0.73(3) 0.034(13) -0.079(16) -0.018(7) C244 0.167(9) 0.118(6) 0.73(3) 0.034(13) -0.079(16) -0.018(7) C245 0.076(5) 0.148(10) 0.216(15) 0.059(9) -0.018(6) -0.048(6) C246 0.070(3) 0.115(6) 0.35(2) 0.043(9) -0.013(8) -0.040(4) C247 0.167(9) 0.118(6) 0.73(3) 0.034(13) -0.079(16) -0.018(7) C248 0.167(9) 0.118(6) 0.73(3) 0.034(13) -0.079(16) -0.018(7) C251 0.066(2) 0.0519(18) 0.053(2) -0.0071(16) 0.0020(17) -0.0054(16) C252 0.0652(19) 0.0588(18) 0.069(2) -0.0123(18) 0.0060(19) -0.0014(17) C253 0.096(3) 0.080(3) 0.097(3) -0.003(3) 0.030(3) 0.024(2) C254 0.095(3) 0.088(3) 0.113(4) -0.050(3) 0.020(3) -0.009(3) C271 0.063(7) 0.096(10) 0.067(5) 0.005(5) -0.008(8) 0.006(6) C272 0.305(12) 0.305(12) 0.103(8) 0 0 0 C273 0.44(4) 0.53(5) 0.47(4) -0.23(5) -0.26(4) 0.22(4) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 Al11 O17 1.734(6) . y Al11 O16 1.890(4) . y Al11 O15 1.945(2) 1_455 y Al11 O15 1.945(2) 6_565 ? Al11 O15 1.945(2) 3_655 ? Al11 O15 1.945(2) 7_545 ? Al11 Al12 2.9821(17) 1_455 ? Al11 Al12 2.9821(17) 7_545 ? Al11 Al12 2.9821(17) 6_565 ? Al11 Al12 2.9821(17) 3_655 ? Al12 O14 1.722(2) . y Al12 O15 1.797(3) . y Al12 O13 1.828(2) 6_665 ? Al12 O13 1.832(2) . y Al12 O16 2.0798(10) 1_655 y Al12 Al12 2.9177(12) 6_665 ? Al12 Al12 2.9177(12) 7_645 ? Al12 Al11 2.9821(17) 1_655 ? O13 C131 1.445(4) . y O13 Al12 1.828(2) 7_645 ? O14 C141 1.339(4) . y O15 C151 1.447(4) . y O15 Al11 1.945(2) 1_655 ? O16 Al12 2.0798(10) 6_565 ? O16 Al12 2.0798(10) 1_455 ? O16 Al12 2.0798(10) 7_545 ? O16 Al12 2.0798(10) 3_655 ? O17 C171 1.330(9) 7 ? O17 C171 1.330(9) 3 ? O17 C171 1.330(9) . y O17 C171 1.330(9) 6 ? Al21 O27 1.718(5) . y Al21 O26 1.880(5) . y Al21 O25 1.969(2) 3_665 ? Al21 O25 1.969(2) . y Al21 O25 1.969(2) 6_565 ? Al21 O25 1.969(2) 7_655 ? Al21 Al22 2.994(2) 3_665 ? Al21 Al22 2.994(2) 7_655 ? Al21 Al22 2.994(2) 6_565 ? Al21 Al22 2.994(2) . ? Al22 O24 1.716(3) . y Al22 O25 1.801(3) . y Al22 O23 1.808(3) . y Al22 O23 1.830(3) 6_565 ? Al22 O26 2.0869(12) . y Al22 Al22 2.9234(15) 7_655 ? Al22 Al22 2.9234(15) 6_565 ? O23 C231 1.463(4) . y O23 Al22 1.830(3) 7_655 ? O24 C241 1.333(7) 8_554 y O24 C245 1.410(6) 8_554 y O25 C251 1.423(4) . y O26 Al22 2.0869(12) 3_665 ? O26 Al22 2.0869(12) 7_655 ? O26 Al22 2.0869(12) 6_565 ? O27 C271 1.379(10) 7_655 ? O27 C271 1.379(10) 3_665 ? O27 C271 1.379(10) . y O27 C271 1.379(10) 6_565 ? C131 C132 1.442(6) . ? C132 C133 1.3491(10) . ? C132 C134 1.539(6) . ? C141 C142 1.364(6) . ? C142 C144 1.451(8) . ? C142 C143 1.489(6) . ? C151 C152 1.520(5) . ? C152 C153 1.514(5) . ? C152 C154 1.523(6) . ? C171 C172 1.3494(10) . ? C172 C173 1.478(17) . ? C172 C173 1.478(17) 7 ? C231 C232 1.519(8) . ? C232 C233 1.452(10) . ? C232 C234 1.543(8) . ? C241 O24 1.333(7) 8 ? C241 C242 1.459(3) . ? C242 C243 1.3969(19) . ? C242 C244 1.3969(19) . ? C245 O24 1.410(6) 8 ? C245 C246 1.459(3) . ? C246 C248 1.3969(19) . ? C246 C247 1.3969(19) . ? C251 C252 1.522(5) . ? C252 C253 1.486(6) . ? C252 C254 1.506(5) . ? C271 C272 1.3498(10) . ? C272 C273 1.39(2) . ? C272 C273 1.39(2) 3_665 ? 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 O17 Al11 O16 180.000(2) . . y O17 Al11 O15 100.79(9) . 1_455 y O16 Al11 O15 79.21(9) . 1_455 y O17 Al11 O15 100.79(9) . 6_565 ? O16 Al11 O15 79.21(9) . 6_565 ? O15 Al11 O15 87.99(3) 1_455 6_565 y O17 Al11 O15 100.79(9) . 3_655 ? O16 Al11 O15 79.21(9) . 3_655 ? O15 Al11 O15 158.42(17) 1_455 3_655 y O15 Al11 O15 87.99(3) 6_565 3_655 ? O17 Al11 O15 100.79(9) . 7_545 ? O16 Al11 O15 79.21(9) . 7_545 ? O15 Al11 O15 87.99(3) 1_455 7_545 ? O15 Al11 O15 158.42(17) 6_565 7_545 ? O15 Al11 O15 87.99(3) 3_655 7_545 ? O17 Al11 Al12 136.22(3) . 1_455 ? O16 Al11 Al12 43.78(3) . 1_455 ? O15 Al11 Al12 35.49(8) 1_455 1_455 ? O15 Al11 Al12 83.88(8) 6_565 1_455 ? O15 Al11 Al12 122.94(11) 3_655 1_455 ? O15 Al11 Al12 80.57(8) 7_545 1_455 ? O17 Al11 Al12 136.22(3) . 7_545 ? O16 Al11 Al12 43.78(3) . 7_545 ? O15 Al11 Al12 83.88(8) 1_455 7_545 ? O15 Al11 Al12 122.94(11) 6_565 7_545 ? O15 Al11 Al12 80.57(8) 3_655 7_545 ? O15 Al11 Al12 35.49(8) 7_545 7_545 ? Al12 Al11 Al12 58.58(4) 1_455 7_545 ? O17 Al11 Al12 136.22(3) . 6_565 ? O16 Al11 Al12 43.78(3) . 6_565 ? O15 Al11 Al12 80.57(8) 1_455 6_565 ? O15 Al11 Al12 35.49(8) 6_565 6_565 ? O15 Al11 Al12 83.88(8) 3_655 6_565 ? O15 Al11 Al12 122.94(11) 7_545 6_565 ? Al12 Al11 Al12 58.58(4) 1_455 6_565 ? Al12 Al11 Al12 87.55(6) 7_545 6_565 ? O17 Al11 Al12 136.22(3) . 3_655 ? O16 Al11 Al12 43.78(3) . 3_655 ? O15 Al11 Al12 122.94(11) 1_455 3_655 ? O15 Al11 Al12 80.57(8) 6_565 3_655 ? O15 Al11 Al12 35.49(8) 3_655 3_655 ? O15 Al11 Al12 83.88(8) 7_545 3_655 ? Al12 Al11 Al12 87.55(6) 1_455 3_655 ? Al12 Al11 Al12 58.58(4) 7_545 3_655 ? Al12 Al11 Al12 58.58(4) 6_565 3_655 ? O14 Al12 O15 104.83(12) . . y O14 Al12 O13 102.28(11) . 6_665 y O15 Al12 O13 110.37(11) . 6_665 y O14 Al12 O13 98.07(11) . . y O15 Al12 O13 115.20(12) . . y O13 Al12 O13 122.55(16) 6_665 . y O14 Al12 O16 176.48(13) . 1_655 y O15 Al12 O16 77.84(13) . 1_655 y O13 Al12 O16 78.70(9) 6_665 1_655 y O13 Al12 O16 78.62(9) . 1_655 y O14 Al12 Al12 136.54(8) . 6_665 ? O15 Al12 Al12 84.71(8) . 6_665 ? O13 Al12 Al12 37.18(8) 6_665 6_665 ? O13 Al12 Al12 116.27(7) . 6_665 ? O16 Al12 Al12 45.457(13) 1_655 6_665 ? O14 Al12 Al12 131.79(8) . 7_645 ? O15 Al12 Al12 88.35(7) . 7_645 ? O13 Al12 Al12 116.32(7) 6_665 7_645 ? O13 Al12 Al12 37.10(8) . 7_645 ? O16 Al12 Al12 45.457(14) 1_655 7_645 ? Al12 Al12 Al12 90.0000(10) 6_665 7_645 ? O14 Al12 Al11 143.54(10) . 1_655 ? O15 Al12 Al11 38.93(8) . 1_655 ? O13 Al12 Al11 97.10(8) 6_665 1_655 ? O13 Al12 Al11 97.02(8) . 1_655 ? O16 Al12 Al11 38.97(11) 1_655 1_655 ? Al12 Al12 Al11 60.712(19) 6_665 1_655 ? Al12 Al12 Al11 60.712(19) 7_645 1_655 ? C131 O13 Al12 124.07(18) . 7_645 y C131 O13 Al12 126.26(18) . . y Al12 O13 Al12 105.72(13) 7_645 . y C141 O14 Al12 165.2(2) . . y C151 O15 Al12 125.4(2) . . y C151 O15 Al11 128.9(2) . 1_655 y Al12 O15 Al11 105.58(12) . 1_655 y Al11 O16 Al12 97.26(11) . 6_565 y Al11 O16 Al12 97.26(11) . 1_455 ? Al12 O16 Al12 89.09(3) 6_565 1_455 y Al11 O16 Al12 97.26(11) . 7_545 ? Al12 O16 Al12 165.5(2) 6_565 7_545 y Al12 O16 Al12 89.09(3) 1_455 7_545 ? Al11 O16 Al12 97.26(11) . 3_655 ? Al12 O16 Al12 89.09(3) 6_565 3_655 ? Al12 O16 Al12 165.5(2) 1_455 3_655 y Al12 O16 Al12 89.09(3) 7_545 3_655 ? C171 O17 C171 33.2(6) 7 3 ? C171 O17 C171 33.2(6) 7 . ? C171 O17 C171 47.6(9) 3 . ? C171 O17 C171 47.6(9) 7 6 ? C171 O17 C171 33.2(6) 3 6 ? C171 O17 C171 33.2(6) . 6 ? C171 O17 Al11 156.2(5) 7 . ? C171 O17 Al11 156.2(5) 3 . ? C171 O17 Al11 156.2(5) . . y C171 O17 Al11 156.2(5) 6 . ? O27 Al21 O26 180 . . y O27 Al21 O25 100.95(10) . 3_665 ? O26 Al21 O25 79.05(10) . 3_665 ? O27 Al21 O25 100.95(10) . . y O26 Al21 O25 79.05(10) . . y O25 Al21 O25 158.1(2) 3_665 . y O27 Al21 O25 100.95(10) . 6_565 ? O26 Al21 O25 79.05(10) . 6_565 ? O25 Al21 O25 87.93(4) 3_665 6_565 ? O25 Al21 O25 87.93(4) . 6_565 y O27 Al21 O25 100.95(10) . 7_655 ? O26 Al21 O25 79.05(10) . 7_655 ? O25 Al21 O25 87.93(4) 3_665 7_655 ? O25 Al21 O25 87.93(4) . 7_655 ? O25 Al21 O25 158.1(2) 6_565 7_655 ? O27 Al21 Al22 136.34(4) . 3_665 ? O26 Al21 Al22 43.66(4) . 3_665 ? O25 Al21 Al22 35.50(8) 3_665 3_665 ? O25 Al21 Al22 122.62(13) . 3_665 ? O25 Al21 Al22 84.47(9) 6_565 3_665 ? O25 Al21 Al22 79.72(9) 7_655 3_665 ? O27 Al21 Al22 136.34(4) . 7_655 ? O26 Al21 Al22 43.66(4) . 7_655 ? O25 Al21 Al22 84.47(9) 3_665 7_655 ? O25 Al21 Al22 79.72(9) . 7_655 ? O25 Al21 Al22 122.62(13) 6_565 7_655 ? O25 Al21 Al22 35.50(8) 7_655 7_655 ? Al22 Al21 Al22 58.45(5) 3_665 7_655 ? O27 Al21 Al22 136.34(4) . 6_565 ? O26 Al21 Al22 43.66(4) . 6_565 ? O25 Al21 Al22 79.72(9) 3_665 6_565 ? O25 Al21 Al22 84.47(9) . 6_565 ? O25 Al21 Al22 35.50(8) 6_565 6_565 ? O25 Al21 Al22 122.62(13) 7_655 6_565 ? Al22 Al21 Al22 58.45(5) 3_665 6_565 ? Al22 Al21 Al22 87.33(8) 7_655 6_565 ? O27 Al21 Al22 136.34(4) . . ? O26 Al21 Al22 43.66(4) . . ? O25 Al21 Al22 122.62(13) 3_665 . ? O25 Al21 Al22 35.50(8) . . ? O25 Al21 Al22 79.72(9) 6_565 . ? O25 Al21 Al22 84.47(9) 7_655 . ? Al22 Al21 Al22 87.33(8) 3_665 . ? Al22 Al21 Al22 58.45(5) 7_655 . ? Al22 Al21 Al22 58.45(5) 6_565 . ? O24 Al22 O25 103.61(13) . . y O24 Al22 O23 101.64(14) . . y O25 Al22 O23 110.11(12) . . y O24 Al22 O23 101.32(13) . 6_565 y O25 Al22 O23 116.81(12) . 6_565 y O23 Al22 O23 120.07(18) . 6_565 y O24 Al22 O26 178.59(17) . . y O25 Al22 O26 77.76(15) . . y O23 Al22 O26 78.12(11) . . y O23 Al22 O26 77.66(10) 6_565 . y O24 Al22 Al22 134.70(11) . 7_655 ? O25 Al22 Al22 84.27(8) . 7_655 ? O23 Al22 Al22 36.78(9) . 7_655 ? O23 Al22 Al22 114.79(8) 6_565 7_655 ? O26 Al22 Al22 45.539(18) . 7_655 ? O24 Al22 Al22 133.83(11) . 6_565 ? O25 Al22 Al22 89.55(7) . 6_565 ? O23 Al22 Al22 115.10(9) . 6_565 ? O23 Al22 Al22 36.29(9) 6_565 6_565 ? O26 Al22 Al22 45.539(18) . 6_565 ? Al22 Al22 Al22 90.0000(10) 7_655 6_565 ? O24 Al22 Al21 142.89(12) . . ? O25 Al22 Al21 39.43(8) . . ? O23 Al22 Al21 97.00(9) . . ? O23 Al22 Al21 96.51(9) 6_565 . ? O26 Al22 Al21 38.45(13) . . ? Al22 Al22 Al21 60.78(2) 7_655 . ? Al22 Al22 Al21 60.78(2) 6_565 . ? C231 O23 Al22 125.3(3) . . y C231 O23 Al22 123.3(2) . 7_655 y Al22 O23 Al22 106.93(14) . 7_655 y C241 O24 C245 56.0(4) 8_554 8_554 ? C241 O24 Al22 160.9(4) 8_554 . y C245 O24 Al22 142.1(3) 8_554 . y C251 O25 Al22 126.6(2) . . y C251 O25 Al21 128.2(2) . . y Al22 O25 Al21 105.06(14) . . y Al21 O26 Al22 97.88(13) . 3_665 y Al21 O26 Al22 97.88(13) . 7_655 ? Al22 O26 Al22 88.92(4) 3_665 7_655 y Al21 O26 Al22 97.88(13) . . ? Al22 O26 Al22 164.2(3) 3_665 . y Al22 O26 Al22 88.92(4) 7_655 . ? Al21 O26 Al22 97.88(13) . 6_565 ? Al22 O26 Al22 88.92(4) 3_665 6_565 ? Al22 O26 Al22 164.2(3) 7_655 6_565 ? Al22 O26 Al22 88.92(4) . 6_565 ? C271 O27 C271 39.7(7) 7_655 3_665 ? C271 O27 C271 39.7(7) 7_655 . ? C271 O27 C271 57.4(11) 3_665 . ? C271 O27 C271 57.4(11) 7_655 6_565 ? C271 O27 C271 39.7(7) 3_665 6_565 ? C271 O27 C271 39.7(7) . 6_565 ? C271 O27 Al21 151.3(6) 7_655 . ? C271 O27 Al21 151.3(6) 3_665 . ? C271 O27 Al21 151.3(6) . . y C271 O27 Al21 151.3(6) 6_565 . ? C132 C131 O13 114.0(3) . . ? C133 C132 C131 126.7(5) . . ? C133 C132 C134 114.4(5) . . ? C131 C132 C134 109.5(4) . . ? O14 C141 C142 126.5(4) . . ? C141 C142 C144 123.7(5) . . ? C141 C142 C143 119.9(5) . . ? C144 C142 C143 116.3(4) . . ? O15 C151 C152 114.0(3) . . ? C153 C152 C151 108.4(4) . . ? C153 C152 C154 110.7(4) . . ? C151 C152 C154 112.4(3) . . ? O17 C171 C172 132.8(10) . . ? C171 C172 C173 96.1(9) . . ? C171 C172 C173 121.8(12) . 7 ? C173 C172 C173 88.8(3) . 7 ? O23 C231 C232 112.2(4) . . ? C233 C232 C231 112.4(6) . . ? C233 C232 C234 110.8(8) . . ? C231 C232 C234 107.6(6) . . ? O24 C241 C242 111.6(5) 8 . ? C243 C242 C244 111.2(3) . . ? C243 C242 C241 107.7(2) . . ? C244 C242 C241 107.7(2) . . ? O24 C245 C246 116.9(7) 8 . ? C248 C246 C247 111.2(3) . . ? C248 C246 C245 107.7(2) . . ? C247 C246 C245 107.7(2) . . ? O25 C251 C252 115.1(3) . . ? C253 C252 C254 110.7(4) . . ? C253 C252 C251 111.3(3) . . ? C254 C252 C251 109.9(3) . . ? C272 C271 O27 121.9(11) . . ? C271 C272 C273 102.0(7) . . ? C271 C272 C273 157(2) . 3_665 ? C273 C272 C273 99.5(12) . 3_665 ? #===END # Structure 3 data_alumh _database_code_CSD 173336 _audit_creation_date 2001-06-12T17:21:27-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.1beta5 _audit_conform_dict_location ftp://ftp.iucr.org/cifdics/cif_core_2.1beta5.dic _publ_requested_category FM #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C72 H164 Al8 O22' _chemical_formula_structural 'C72 H164 AL8 O22' _chemical_formula_sum 'C72 H164 Al8 O22' _chemical_formula_weight 1597.87 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 29.282(5) _cell_length_b 19.276(8) _cell_length_c 18.192(4) _cell_angle_alpha 90 _cell_angle_beta 99.81(3) _cell_angle_gamma 90 _cell_volume 10118(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 18 _cell_measurement_theta_min 10.1385 _cell_measurement_theta_max 14.4425 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.25 _exptl_crystal_density_diffrn 1.049 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3504 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.137 _exptl_absorpt_factor_muR 0 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details ; North A.C.T., Phillips D.C. & Mathews F.S. (1968) Acta. Cryst. A24, 351 Number of psi-scan sets used was 3 Theta correction was applied. Averaged transmission function was used. No Fourier smoothing was applied. ; _exptl_absorpt_correction_T_min 0.9569 _exptl_absorpt_correction_T_max 0.9995 _exptl_absorpt_correction_T_ave 0.9744 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'scintillation LiI' _diffrn_detector_dtime 1.195 _diffrn_orient_matrix_type ; x-axis points to radiation source the matrix is specified in reciprocal space ; _diffrn_orient_matrix_ub_11 -0.2244E-2 _diffrn_orient_matrix_ub_12 0.15304E-1 _diffrn_orient_matrix_ub_13 0.51774E-1 _diffrn_orient_matrix_ub_21 0.25811E-1 _diffrn_orient_matrix_ub_22 0.33671E-1 _diffrn_orient_matrix_ub_23 -0.1048E-2 _diffrn_orient_matrix_ub_31 -0.23006E-1 _diffrn_orient_matrix_ub_32 0.36433E-1 _diffrn_orient_matrix_ub_33 -0.02068 _diffrn_measurement_device '\k-geometry diffractometer' _diffrn_measurement_device_type 'Enraf Nonius CAD4' _diffrn_measurement_method 'non-profiled omega/2theta scans' _diffrn_standards_number 2 _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 5 _diffrn_standards_decay_corr_max 1.088 _diffrn_standards_decay_corr_min 0.97 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 16 -2 -2 1 -1 -9 _diffrn_reflns_number 9062 _diffrn_reflns_av_R_equivalents 0.0329 _diffrn_reflns_av_sigmaI/netI 0.1315 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 34 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.62 _diffrn_reflns_theta_max 25 _diffrn_reflns_theta_full 25 _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.996 _reflns_number_total 8876 _reflns_number_gt 3822 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'CAD4 Express (Enraf Nonius, 1994)' _computing_cell_refinement 'CAD4 Express (Enraf Nonius, 1994)' _computing_data_reduction 'XCAD4 (Harms & Wocadlo, 1995)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.1000P)^2^+2.5000P] 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 SHELXL _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_coef 0.00005(6) _refine_ls_number_reflns 8876 _refine_ls_number_parameters 519 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1997 _refine_ls_R_factor_gt 0.0624 _refine_ls_wR_factor_ref 0.2009 _refine_ls_wR_factor_gt 0.1517 _refine_ls_goodness_of_fit_ref 0.948 _refine_ls_restrained_S_all 0.948 _refine_ls_shift/su_max 0.321 _refine_ls_shift/su_mean 0.014 _refine_diff_density_max 0.323 _refine_diff_density_min -0.333 _refine_diff_density_rms 0.049 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 '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' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Al1 Al 0.22478(4) 0.21574(7) 0.04680(7) 0.0442(3) Uani 1 1 d . . . Al2 Al 0.17256(4) 0.23699(7) 0.16453(7) 0.0498(4) Uani 1 1 d . C . Al3 Al 0.14882(4) 0.12633(7) 0.05953(7) 0.0494(4) Uani 1 1 d . C . Al4 Al 0.10651(4) 0.26310(7) 0.02680(7) 0.0515(4) Uani 1 1 d . C . O1 O 0.04914(11) 0.28717(19) 0.0107(2) 0.0789(11) Uani 1 1 d . . . O2 O 0.13064(10) 0.31172(16) -0.03942(17) 0.0634(9) Uani 1 1 d . . . O3 O 0.20627(9) 0.12607(14) 0.02791(15) 0.0481(7) Uani 1 1 d . . . O4 O 0.23439(9) 0.23354(14) 0.14679(14) 0.0469(7) Uani 1 1 d . . . O5 O 0.09703(9) 0.16645(15) 0.00769(16) 0.0541(8) Uani 1 1 d . . . O6 O 0.12157(10) 0.29067(15) 0.12781(16) 0.0574(8) Uani 1 1 d . . . O7 O 0.15373(10) 0.14614(14) 0.15996(15) 0.0536(8) Uani 1 1 d . . . O8 O 0.18236(11) 0.2582(2) 0.25600(18) 0.0765(10) Uani 1 1 d . . . O9 O 0.13675(12) 0.04029(17) 0.0552(2) 0.0741(10) Uani 1 1 d . . . O10 O 0.21798(12) 0.28235(16) -0.02457(18) 0.0496(9) Uani 1 1 d . . . O11 O 0.16515(8) 0.22255(13) 0.06160(14) 0.0417(7) Uani 1 1 d . . . C11 C 0.0075(3) 0.2969(6) 0.0064(8) 0.255(8) Uani 1 1 d . B . H11A H -0.0019 0.2603 -0.0296 0.306 Uiso 1 1 calc R . . H11B H 0.0051 0.2753 0.0537 0.306 Uiso 1 1 calc R . . C12 C -0.0302(4) 0.3253(10) -0.0016(16) 0.272(8) Uani 1 1 d . . . H12 H -0.0179 0.3681 0.0234 0.327 Uiso 1 1 calc R A 1 C13A C -0.0651(17) 0.356(3) -0.041(4) 0.30(3) Uani 0.5 1 d P B 1 H13A H -0.085 0.3747 -0.0095 0.455 Uiso 0.5 1 calc PR B 1 H13B H -0.0821 0.3235 -0.0755 0.455 Uiso 0.5 1 calc PR B 1 H13C H -0.0541 0.3932 -0.0692 0.455 Uiso 0.5 1 calc PR B 1 C14A C -0.0426(11) 0.2902(17) 0.0753(18) 0.266(15) Uani 0.5 1 d P B 1 H14A H -0.0728 0.3052 0.0826 0.398 Uiso 0.5 1 calc PR B 1 H14B H -0.02 0.3043 0.1172 0.398 Uiso 0.5 1 calc PR B 1 H14C H -0.0423 0.2405 0.071 0.398 Uiso 0.5 1 calc PR B 1 C13B C -0.0326(10) 0.324(3) -0.092(3) 0.39(4) Uani 0.5 1 d P B 2 H13D H -0.061 0.3452 -0.1159 0.589 Uiso 0.5 1 calc PR B 2 H13E H -0.0313 0.277 -0.1087 0.589 Uiso 0.5 1 calc PR B 2 H13F H -0.0067 0.3495 -0.1046 0.589 Uiso 0.5 1 calc PR B 2 C14B C -0.0740(9) 0.330(3) 0.001(4) 0.31(4) Uani 0.5 1 d P B 2 H14D H -0.0857 0.3729 -0.0226 0.469 Uiso 0.5 1 calc PR B 2 H14E H -0.0786 0.3297 0.0515 0.469 Uiso 0.5 1 calc PR B 2 H14F H -0.09 0.2919 -0.0258 0.469 Uiso 0.5 1 calc PR B 2 C21 C 0.1053(2) 0.3499(4) -0.1001(3) 0.102(2) Uani 1 1 d . . . H21A H 0.077 0.3249 -0.119 0.122 Uiso 1 1 calc R . . H21B H 0.1235 0.3519 -0.1399 0.122 Uiso 1 1 calc R . . C22 C 0.0930(3) 0.4215(5) -0.0819(5) 0.154(4) Uani 1 1 d . . . H22 H 0.0742 0.4191 -0.0422 0.185 Uiso 1 1 calc R . . C23 C 0.0634(4) 0.4531(6) -0.1503(7) 0.311(9) Uani 1 1 d . . . H23A H 0.0539 0.4988 -0.1386 0.466 Uiso 1 1 calc R . . H23B H 0.0365 0.4247 -0.1656 0.466 Uiso 1 1 calc R . . H23C H 0.0811 0.4557 -0.1901 0.466 Uiso 1 1 calc R . . C24 C 0.1347(4) 0.4619(5) -0.0541(8) 0.239(7) Uani 1 1 d . . . H24A H 0.126 0.5076 -0.0407 0.359 Uiso 1 1 calc R . . H24B H 0.1535 0.4652 -0.0924 0.359 Uiso 1 1 calc R . . H24C H 0.152 0.4393 -0.0111 0.359 Uiso 1 1 calc R . . C31 C 0.23106(16) 0.0679(2) 0.0046(3) 0.0588(13) Uani 1 1 d . . . H31A H 0.2303 0.0299 0.0393 0.071 Uiso 1 1 calc R . . H31B H 0.2632 0.0809 0.006 0.071 Uiso 1 1 calc R . . C32 C 0.2109(2) 0.0437(3) -0.0732(3) 0.0836(17) Uani 1 1 d . . . H32 H 0.1785 0.0309 -0.0734 0.1 Uiso 1 1 calc R . . C33 C 0.2370(2) -0.0221(3) -0.0901(4) 0.118(2) Uani 1 1 d . . . H33A H 0.2349 -0.0565 -0.0526 0.177 Uiso 1 1 calc R . . H33B H 0.2689 -0.011 -0.0901 0.177 Uiso 1 1 calc R . . H33C H 0.2233 -0.0399 -0.1381 0.177 Uiso 1 1 calc R . . C34 C 0.2116(3) 0.0978(4) -0.1304(4) 0.137(3) Uani 1 1 d . . . H34A H 0.1973 0.0803 -0.1781 0.206 Uiso 1 1 calc R . . H34B H 0.2431 0.1105 -0.1322 0.206 Uiso 1 1 calc R . . H34C H 0.195 0.1378 -0.118 0.206 Uiso 1 1 calc R . . C41 C 0.27652(15) 0.2306(3) 0.2015(3) 0.0637(13) Uani 1 1 d . . . H41A H 0.2785 0.2719 0.2323 0.076 Uiso 1 1 calc R . . H41B H 0.3029 0.2306 0.1758 0.076 Uiso 1 1 calc R . . C42 C 0.27914(18) 0.1666(3) 0.2515(3) 0.0747(15) Uani 1 1 d . . . H42 H 0.2526 0.168 0.2777 0.09 Uiso 1 1 calc R . . C43 C 0.3230(2) 0.1727(4) 0.3097(4) 0.132(3) Uani 1 1 d . . . H43A H 0.3225 0.2156 0.3365 0.198 Uiso 1 1 calc R . . H43B H 0.3497 0.1719 0.2854 0.198 Uiso 1 1 calc R . . H43C H 0.3246 0.1346 0.344 0.198 Uiso 1 1 calc R . . C44 C 0.2769(2) 0.0994(3) 0.2091(3) 0.0973(19) Uani 1 1 d . . . H44A H 0.2773 0.0613 0.2431 0.146 Uiso 1 1 calc R . . H44B H 0.3032 0.096 0.1841 0.146 Uiso 1 1 calc R . . H44C H 0.249 0.098 0.1729 0.146 Uiso 1 1 calc R . . C51 C 0.05568(17) 0.1321(3) -0.0274(3) 0.0785(16) Uani 1 1 d . . . H51A H 0.03 0.1646 -0.0327 0.094 Uiso 1 1 calc R . . H51B H 0.0488 0.0943 0.0041 0.094 Uiso 1 1 calc R . . C52 C 0.0601(2) 0.1041(5) -0.1025(4) 0.120(2) Uani 1 1 d . . . H52 H 0.0853 0.0701 -0.0949 0.144 Uiso 1 1 calc R . . C53 C 0.0141(3) 0.0635(5) -0.1330(5) 0.187(5) Uani 1 1 d . . . H53A H 0.0087 0.0292 -0.0972 0.28 Uiso 1 1 calc R . . H53B H 0.017 0.0412 -0.1791 0.28 Uiso 1 1 calc R . . H53C H -0.0115 0.0954 -0.1412 0.28 Uiso 1 1 calc R . . C54 C 0.0720(4) 0.1566(5) -0.1551(4) 0.181(4) Uani 1 1 d . . . H54A H 0.0753 0.1345 -0.2011 0.272 Uiso 1 1 calc R . . H54B H 0.1006 0.1788 -0.134 0.272 Uiso 1 1 calc R . . H54C H 0.0477 0.1907 -0.1643 0.272 Uiso 1 1 calc R . . C61 C 0.0939(2) 0.3312(3) 0.1693(3) 0.093(2) Uani 1 1 d . . . H61A H 0.107 0.3284 0.2219 0.112 Uiso 1 1 calc R . . H61B H 0.0629 0.3119 0.1626 0.112 Uiso 1 1 calc R . . C62 C 0.0909(3) 0.4066(4) 0.1459(5) 0.133(3) Uani 1 1 d . . . H62 H 0.08 0.4094 0.092 0.16 Uiso 1 1 calc R . . C63 C 0.0534(4) 0.4395(6) 0.1878(6) 0.259(7) Uani 1 1 d . . . H63A H 0.0241 0.4173 0.1715 0.388 Uiso 1 1 calc R . . H63B H 0.0507 0.4882 0.1768 0.388 Uiso 1 1 calc R . . H63C H 0.0626 0.433 0.2405 0.388 Uiso 1 1 calc R . . C64 C 0.1376(4) 0.4398(4) 0.1641(7) 0.217(6) Uani 1 1 d . . . H64A H 0.1357 0.487 0.147 0.326 Uiso 1 1 calc R . . H64B H 0.1592 0.4148 0.1398 0.326 Uiso 1 1 calc R . . H64C H 0.1479 0.4389 0.2171 0.326 Uiso 1 1 calc R . . C71 C 0.14347(18) 0.1044(3) 0.2207(3) 0.0681(14) Uani 1 1 d . . . H71A H 0.168 0.1104 0.2633 0.082 Uiso 1 1 calc R . . H71B H 0.1431 0.056 0.2062 0.082 Uiso 1 1 calc R . . C72 C 0.0987(3) 0.1216(5) 0.2435(4) 0.134(3) Uani 1 1 d . . . H72 H 0.1026 0.1685 0.2646 0.161 Uiso 1 1 calc R . . C73 C 0.0925(3) 0.0745(6) 0.3084(5) 0.223(6) Uani 1 1 d . . . H73A H 0.1198 0.0767 0.3461 0.335 Uiso 1 1 calc R . . H73B H 0.0878 0.0277 0.2909 0.335 Uiso 1 1 calc R . . H73C H 0.0662 0.0896 0.3291 0.335 Uiso 1 1 calc R . . C74 C 0.0594(3) 0.1242(6) 0.1910(5) 0.180(4) Uani 1 1 d . . . H74A H 0.0338 0.1384 0.2141 0.27 Uiso 1 1 calc R . . H74B H 0.0532 0.0792 0.1691 0.27 Uiso 1 1 calc R . . H74C H 0.0635 0.157 0.1529 0.27 Uiso 1 1 calc R . . C81 C 0.1971(4) 0.2972(6) 0.3113(5) 0.210(6) Uani 1 1 d . . . H81A H 0.2301 0.2877 0.3203 0.252 Uiso 1 1 calc R . . H81B H 0.1942 0.3431 0.2891 0.252 Uiso 1 1 calc R . . C82 C 0.1888(5) 0.3081(8) 0.3758(5) 0.213(6) Uani 1 1 d . . . H82 H 0.1558 0.3198 0.3653 0.255 Uiso 1 1 calc R . . C83 C 0.2062(5) 0.3610(8) 0.4257(9) 0.353(12) Uani 1 1 d . . . H83A H 0.1931 0.3566 0.4705 0.529 Uiso 1 1 calc R . . H83B H 0.198 0.4053 0.4032 0.529 Uiso 1 1 calc R . . H83C H 0.2393 0.3572 0.4378 0.529 Uiso 1 1 calc R . . C84 C 0.1882(6) 0.2436(12) 0.4183(9) 0.394(15) Uani 1 1 d . . . H84A H 0.1806 0.2538 0.4665 0.591 Uiso 1 1 calc R . . H84B H 0.2181 0.222 0.4243 0.591 Uiso 1 1 calc R . . H84C H 0.1653 0.2127 0.3919 0.591 Uiso 1 1 calc R . . C91A C 0.1510(6) -0.0225(7) 0.0785(9) 0.095(4) Uani 0.5 1 d P C 1 H91A H 0.1738 -0.0163 0.1234 0.114 Uiso 0.5 1 calc PR C 1 H91B H 0.1673 -0.0418 0.041 0.114 Uiso 0.5 1 calc PR C 1 C92A C 0.1175(7) -0.0768(10) 0.0953(11) 0.092(6) Uani 0.5 1 d P C 1 H92A H 0.0995 -0.058 0.1316 0.11 Uiso 0.5 1 calc PR C 1 C93A C 0.0846(9) -0.0884(12) 0.0201(13) 0.172(9) Uani 0.5 1 d P C 1 H93A H 0.0712 -0.0449 0.002 0.259 Uiso 0.5 1 calc PR C 1 H93B H 0.0604 -0.12 0.0273 0.259 Uiso 0.5 1 calc PR C 1 H93C H 0.1018 -0.1075 -0.0156 0.259 Uiso 0.5 1 calc PR C 1 C94A C 0.1370(10) -0.1400(11) 0.1221(18) 0.211(12) Uani 0.5 1 d P C 1 H94A H 0.113 -0.1704 0.1328 0.317 Uiso 0.5 1 calc PR C 1 H94B H 0.159 -0.1321 0.1668 0.317 Uiso 0.5 1 calc PR C 1 H94C H 0.1523 -0.1609 0.085 0.317 Uiso 0.5 1 calc PR C 1 C91B C 0.1151(6) -0.0191(8) 0.0459(10) 0.112(5) Uani 0.5 1 d P C 2 H91C H 0.1014 -0.0218 -0.0065 0.134 Uiso 0.5 1 calc PR C 2 H91D H 0.0895 -0.0163 0.0735 0.134 Uiso 0.5 1 calc PR C 2 C92B C 0.1366(12) -0.0823(11) 0.0642(18) 0.151(10) Uani 0.5 1 d P C 2 H92B H 0.1593 -0.0873 0.0307 0.181 Uiso 0.5 1 calc PR C 2 C93B C 0.1641(11) -0.0878(11) 0.1418(14) 0.259(16) Uani 0.5 1 d P C 2 H93D H 0.1789 -0.1324 0.1482 0.388 Uiso 0.5 1 calc PR C 2 H93E H 0.1438 -0.0825 0.1776 0.388 Uiso 0.5 1 calc PR C 2 H93F H 0.1873 -0.052 0.1493 0.388 Uiso 0.5 1 calc PR C 2 C94B C 0.1026(13) -0.1453(13) 0.046(2) 0.251(17) Uani 0.5 1 d P C 2 H94D H 0.1192 -0.1878 0.0584 0.376 Uiso 0.5 1 calc PR C 2 H94E H 0.0898 -0.1451 -0.0062 0.376 Uiso 0.5 1 calc PR C 2 H94F H 0.078 -0.1415 0.0746 0.376 Uiso 0.5 1 calc PR C 2 H10 H 0.1957(14) 0.293(2) -0.036(2) 0.041(16) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Al1 0.0393(7) 0.0442(8) 0.0494(8) 0.0056(6) 0.0086(6) -0.0021(6) Al2 0.0490(8) 0.0553(9) 0.0461(8) -0.0029(7) 0.0113(6) -0.0051(7) Al3 0.0477(8) 0.0468(8) 0.0550(9) 0.0002(7) 0.0123(6) -0.0068(6) Al4 0.0406(8) 0.0569(9) 0.0572(9) 0.0006(7) 0.0089(6) 0.0030(6) O1 0.041(2) 0.093(3) 0.101(3) -0.011(2) 0.0074(18) 0.0102(18) O2 0.054(2) 0.069(2) 0.066(2) 0.0258(17) 0.0083(16) 0.0119(16) O3 0.0469(17) 0.0413(17) 0.0579(18) -0.0014(14) 0.0143(14) 0.0009(14) O4 0.0383(16) 0.0586(19) 0.0428(17) 0.0019(14) 0.0039(13) -0.0053(14) O5 0.0369(17) 0.059(2) 0.064(2) -0.0079(15) 0.0021(14) -0.0059(14) O6 0.0549(19) 0.063(2) 0.0570(19) -0.0080(16) 0.0166(15) 0.0101(16) O7 0.0577(19) 0.0532(19) 0.0513(18) 0.0064(15) 0.0137(15) -0.0096(15) O8 0.078(2) 0.107(3) 0.045(2) -0.021(2) 0.0100(17) -0.005(2) O9 0.079(2) 0.043(2) 0.104(3) -0.001(2) 0.025(2) -0.0133(19) O10 0.038(2) 0.052(2) 0.060(2) 0.0152(15) 0.0081(16) 0.0047(16) O11 0.0379(15) 0.0443(17) 0.0438(16) 0.0015(13) 0.0094(12) -0.0006(12) C11 0.054(6) 0.261(13) 0.43(2) -0.149(13) 0.002(8) 0.034(7) C12 0.087(9) 0.36(2) 0.38(3) 0.05(2) 0.058(14) 0.087(11) C13A 0.23(6) 0.30(5) 0.34(6) 0.03(4) -0.05(5) 0.17(5) C14A 0.12(2) 0.41(5) 0.27(4) 0.06(3) 0.01(2) -0.04(3) C13B 0.11(2) 0.57(8) 0.50(7) 0.33(7) 0.05(3) 0.11(3) C14B 0.029(11) 0.34(6) 0.57(12) -0.18(6) 0.04(3) 0.02(2) C21 0.080(4) 0.124(6) 0.103(5) 0.059(4) 0.019(4) 0.029(4) C22 0.136(7) 0.132(7) 0.206(9) 0.091(7) 0.062(7) 0.074(6) C23 0.327(16) 0.328(17) 0.289(15) 0.223(14) 0.086(12) 0.221(14) C24 0.132(8) 0.111(8) 0.49(2) 0.079(10) 0.092(11) 0.017(6) C31 0.061(3) 0.047(3) 0.071(3) -0.005(2) 0.016(3) 0.008(2) C32 0.098(4) 0.069(4) 0.086(4) -0.022(3) 0.021(3) 0.002(3) C33 0.139(6) 0.091(5) 0.126(6) -0.044(4) 0.025(5) 0.018(4) C34 0.240(10) 0.100(6) 0.078(5) 0.000(4) 0.044(5) 0.007(6) C41 0.047(3) 0.081(4) 0.059(3) 0.004(3) -0.004(2) -0.011(2) C42 0.071(4) 0.096(4) 0.052(3) 0.012(3) -0.002(3) 0.007(3) C43 0.125(6) 0.135(6) 0.106(5) 0.014(4) -0.063(5) 0.007(5) C44 0.103(5) 0.091(5) 0.093(5) 0.015(4) 0.005(4) 0.015(4) C51 0.052(3) 0.080(4) 0.097(4) -0.026(3) -0.003(3) -0.010(3) C52 0.105(6) 0.148(7) 0.098(6) -0.040(5) -0.009(4) -0.012(5) C53 0.107(6) 0.231(10) 0.203(10) -0.124(8) -0.029(6) -0.037(6) C54 0.241(11) 0.200(10) 0.087(6) 0.006(6) -0.020(6) -0.047(8) C61 0.077(4) 0.124(6) 0.078(4) -0.033(4) 0.014(3) 0.032(4) C62 0.148(7) 0.091(6) 0.149(7) -0.037(5) -0.004(6) 0.055(5) C63 0.263(13) 0.268(13) 0.226(11) -0.136(10) -0.017(9) 0.182(11) C64 0.201(11) 0.083(6) 0.328(16) -0.028(7) -0.066(10) -0.018(6) C71 0.076(4) 0.067(3) 0.066(3) 0.017(3) 0.025(3) -0.010(3) C72 0.082(5) 0.200(8) 0.127(6) 0.082(6) 0.036(5) -0.011(5) C73 0.166(8) 0.331(14) 0.201(10) 0.160(10) 0.110(7) 0.004(9) C74 0.096(6) 0.278(12) 0.178(9) 0.059(9) 0.056(6) -0.034(7) C81 0.230(11) 0.271(13) 0.104(7) -0.080(8) -0.046(7) 0.108(10) C82 0.305(15) 0.265(14) 0.065(6) -0.081(8) 0.021(8) 0.003(12) C83 0.294(17) 0.35(2) 0.37(2) -0.274(19) -0.083(15) 0.088(15) C84 0.37(2) 0.59(4) 0.209(18) 0.17(2) 0.034(15) -0.01(2) C91A 0.114(12) 0.048(9) 0.122(12) -0.003(8) 0.018(10) -0.005(8) C92A 0.126(15) 0.071(11) 0.087(13) 0.013(9) 0.044(11) -0.032(10) C93A 0.22(3) 0.112(17) 0.18(2) 0.016(15) 0.018(18) -0.069(17) C94A 0.31(3) 0.053(12) 0.27(3) 0.028(17) 0.05(3) -0.035(16) C91B 0.128(14) 0.070(11) 0.128(14) 0.004(9) -0.003(11) -0.024(11) C92B 0.22(3) 0.065(13) 0.18(3) 0.027(15) 0.07(2) -0.059(16) C93B 0.44(5) 0.084(15) 0.20(2) 0.037(15) -0.11(3) 0.02(2) C94B 0.33(4) 0.093(17) 0.34(4) -0.07(3) 0.10(3) -0.10(2) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Al1 O10 1.790(4) 7 y Al1 O10 1.813(3) . y Al1 O11 1.816(3) . y Al1 O4 1.825(3) . y Al1 O3 1.827(3) . y Al1 Al1 2.772(2) 7 ? Al1 Al3 2.8541(18) . ? Al1 Al2 2.8651(19) . ? Al2 O8 1.690(3) . y Al2 O7 1.833(3) . y Al2 O6 1.845(3) . y Al2 O11 1.869(3) . y Al2 O4 1.894(3) . y Al2 Al3 2.869(2) . y Al2 Al4 2.936(2) . y Al3 O9 1.695(4) . y Al3 O5 1.817(3) . y Al3 O7 1.848(3) . y Al3 O3 1.868(3) . y Al3 O11 1.914(3) . y Al3 Al4 2.931(2) . ? Al4 O1 1.719(3) . y Al4 O2 1.766(3) . y Al4 O6 1.891(3) . y Al4 O11 1.895(3) . y Al4 O5 1.907(3) . y O1 C11 1.223(8) . y O2 C21 1.426(6) . y O3 C31 1.438(5) . y O4 C41 1.448(5) . y O5 C51 1.431(5) . y O6 C61 1.430(5) . y O7 C71 1.440(5) . y O8 C81 1.271(9) . y O9 C91B 1.306(15) . y O9 C91A 1.325(14) . y O10 Al1 1.790(4) 7 ? C11 C12 1.219(13) . ? C12 C13A 1.29(4) . ? C12 C14B 1.29(3) . ? C12 C13B 1.63(4) . ? C12 C14A 1.65(3) . ? C21 C22 1.478(10) . ? C22 C24 1.465(12) . ? C22 C23 1.518(11) . ? C31 C32 1.511(7) . ? C32 C34 1.475(8) . ? C32 C33 1.538(7) . ? C41 C42 1.527(7) . ? C42 C44 1.504(7) . ? C42 C43 1.524(7) . ? C51 C52 1.493(8) . ? C52 C54 1.474(10) . ? C52 C53 1.574(9) . ? C61 C62 1.513(9) . ? C62 C64 1.496(11) . ? C62 C63 1.572(11) . ? C71 C72 1.477(8) . ? C72 C74 1.366(9) . ? C72 C73 1.524(9) . ? C81 C82 1.257(11) . ? C82 C83 1.401(13) . ? C82 C84 1.466(19) . ? C91A C92A 1.50(2) . ? C92A C94A 1.40(3) . ? C92A C93A 1.55(3) . ? C91B C92B 1.39(3) . ? C92B C93B 1.51(4) . ? C92B C94B 1.57(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 O10 Al1 O10 79.42(18) 7 . y O10 Al1 O11 173.06(15) 7 . y O10 Al1 O11 93.66(15) . . y O10 Al1 O4 103.29(15) 7 . y O10 Al1 O4 124.06(15) . . y O11 Al1 O4 80.07(12) . . y O10 Al1 O3 103.66(15) 7 . y O10 Al1 O3 122.86(15) . . y O11 Al1 O3 80.47(12) . . y O4 Al1 O3 110.85(13) . . y O10 Al1 Al1 40.00(11) 7 7 ? O10 Al1 Al1 39.41(11) . 7 ? O11 Al1 Al1 133.08(12) . 7 ? O4 Al1 Al1 120.99(11) . 7 ? O3 Al1 Al1 120.49(11) . 7 ? O10 Al1 Al3 143.44(13) 7 . ? O10 Al1 Al3 119.59(13) . . ? O11 Al1 Al3 41.37(9) . . ? O4 Al1 Al3 91.30(10) . . ? O3 Al1 Al3 39.96(9) . . ? Al1 Al1 Al3 147.32(8) 7 . ? O10 Al1 Al2 143.65(13) 7 . ? O10 Al1 Al2 115.26(12) . . ? O11 Al1 Al2 39.63(9) . . ? O4 Al1 Al2 40.49(9) . . ? O3 Al1 Al2 95.56(10) . . ? Al1 Al1 Al2 143.06(8) 7 . ? Al3 Al1 Al2 60.21(5) . . ? O8 Al2 O7 105.94(17) . . y O8 Al2 O6 102.24(16) . . y O7 Al2 O6 107.50(15) . . y O8 Al2 O11 173.70(17) . . y O7 Al2 O11 80.20(13) . . y O6 Al2 O11 76.83(13) . . y O8 Al2 O4 99.75(15) . . y O7 Al2 O4 104.34(13) . . y O6 Al2 O4 134.11(14) . . y O11 Al2 O4 77.01(12) . . y O8 Al2 Al1 138.41(13) . . ? O7 Al2 Al1 91.39(10) . . ? O6 Al2 Al1 108.15(11) . . ? O11 Al2 Al1 38.31(8) . . ? O4 Al2 Al1 38.74(8) . . ? O8 Al2 Al3 144.75(14) . . ? O7 Al2 Al3 39.00(9) . . ? O6 Al2 Al3 94.97(11) . . ? O11 Al2 Al3 41.28(9) . . ? O4 Al2 Al3 89.47(10) . . ? Al1 Al2 Al3 59.71(4) . . ? O8 Al2 Al4 140.86(13) . . ? O7 Al2 Al4 88.62(10) . . ? O6 Al2 Al4 38.77(10) . . ? O11 Al2 Al4 39.04(8) . . ? O4 Al2 Al4 111.75(10) . . ? Al1 Al2 Al4 75.19(5) . . ? Al3 Al2 Al4 60.63(5) . . ? O9 Al3 O5 104.08(17) . . y O9 Al3 O7 103.23(16) . . y O5 Al3 O7 110.04(14) . . y O9 Al3 O3 100.06(15) . . y O5 Al3 O3 123.86(14) . . y O7 Al3 O3 112.49(14) . . y O9 Al3 O11 176.93(16) . . y O5 Al3 O11 77.37(13) . . y O7 Al3 O11 78.65(12) . . y O3 Al3 O11 76.93(12) . . y O9 Al3 Al1 138.28(13) . . ? O5 Al3 Al1 107.10(11) . . ? O7 Al3 Al1 91.43(10) . . ? O3 Al3 Al1 38.89(9) . . ? O11 Al3 Al1 38.84(8) . . ? O9 Al3 Al2 141.60(14) . . ? O5 Al3 Al2 96.62(11) . . ? O7 Al3 Al2 38.63(9) . . ? O3 Al3 Al2 94.49(10) . . ? O11 Al3 Al2 40.09(8) . . ? Al1 Al3 Al2 60.08(5) . . ? O9 Al3 Al4 142.49(14) . . ? O5 Al3 Al4 39.19(9) . . ? O7 Al3 Al4 88.50(10) . . ? O3 Al3 Al4 108.15(10) . . ? O11 Al3 Al4 39.45(8) . . ? Al1 Al3 Al4 75.44(5) . . ? Al2 Al3 Al4 60.82(5) . . ? O1 Al4 O2 103.51(17) . . y O1 Al4 O6 98.55(16) . . y O2 Al4 O6 117.36(16) . . y O1 Al4 O11 166.37(17) . . y O2 Al4 O11 90.11(13) . . y O6 Al4 O11 75.12(13) . . y O1 Al4 O5 97.18(16) . . y O2 Al4 O5 117.18(15) . . y O6 Al4 O5 117.02(15) . . y O11 Al4 O5 75.72(12) . . y O1 Al4 Al3 130.12(14) . . ? O2 Al4 Al3 114.31(12) . . ? O6 Al4 Al3 92.00(11) . . ? O11 Al4 Al3 39.94(8) . . ? O5 Al4 Al3 37.02(9) . . ? O1 Al4 Al2 132.36(14) . . ? O2 Al4 Al2 113.03(12) . . ? O6 Al4 Al2 37.67(9) . . ? O11 Al4 Al2 38.41(8) . . ? O5 Al4 Al2 92.43(10) . . ? Al3 Al4 Al2 58.55(4) . . ? C11 O1 Al4 170.8(8) . . y C21 O2 Al4 125.9(3) . . y C31 O3 Al1 130.1(3) . . y C31 O3 Al3 128.3(3) . . y Al1 O3 Al3 101.15(14) . . y C41 O4 Al1 130.2(3) . . y C41 O4 Al2 127.7(3) . . y Al1 O4 Al2 100.77(13) . . y C51 O5 Al3 127.1(3) . . y C51 O5 Al4 128.2(3) . . y Al3 O5 Al4 103.80(14) . . y C61 O6 Al2 127.7(3) . . y C61 O6 Al4 127.4(3) . . y Al2 O6 Al4 103.56(15) . . y C71 O7 Al2 126.8(3) . . y C71 O7 Al3 130.7(3) . . y Al2 O7 Al3 102.37(14) . . y C81 O8 Al2 154.1(7) . . y C91B O9 C91A 50.3(7) . . ? C91B O9 Al3 163.1(9) . . y C91A O9 Al3 145.7(8) . . y Al1 O10 Al1 100.58(18) 7 . y Al1 O11 Al2 102.05(13) . . y Al1 O11 Al4 145.05(16) . . y Al2 O11 Al4 102.55(13) . . y Al1 O11 Al3 99.80(13) . . y Al2 O11 Al3 98.63(13) . . y Al4 O11 Al3 100.61(13) . . y C12 C11 O1 161.8(16) . . ? C11 C12 C13A 152(5) . . ? C11 C12 C14B 156(4) . . ? C13A C12 C14B 45(4) . . ? C11 C12 C13B 90(2) . . ? C13A C12 C13B 63(3) . . ? C14B C12 C13B 99(4) . . ? C11 C12 C14A 92(2) . . ? C13A C12 C14A 113(3) . . ? C14B C12 C14A 69(3) . . ? C13B C12 C14A 150(3) . . ? O2 C21 C22 115.0(6) . . ? C24 C22 C21 110.6(7) . . ? C24 C22 C23 113.3(9) . . ? C21 C22 C23 108.5(9) . . ? O3 C31 C32 112.4(4) . . ? C34 C32 C31 113.1(5) . . ? C34 C32 C33 112.0(5) . . ? C31 C32 C33 108.3(5) . . ? O4 C41 C42 113.1(4) . . ? C44 C42 C43 112.4(5) . . ? C44 C42 C41 113.3(4) . . ? C43 C42 C41 107.6(5) . . ? O5 C51 C52 112.2(5) . . ? C54 C52 C51 114.3(7) . . ? C54 C52 C53 113.2(7) . . ? C51 C52 C53 107.5(6) . . ? O6 C61 C62 112.8(5) . . ? C64 C62 C61 110.0(6) . . ? C64 C62 C63 114.1(8) . . ? C61 C62 C63 105.3(8) . . ? O7 C71 C72 113.6(4) . . ? C74 C72 C71 119.7(7) . . ? C74 C72 C73 111.5(7) . . ? C71 C72 C73 108.2(6) . . ? C82 C81 O8 138.1(13) . . ? C81 C82 C83 128.4(17) . . ? C81 C82 C84 111.9(14) . . ? C83 C82 C84 108.2(12) . . ? O9 C91A C92A 121.4(15) . . ? C94A C92A C91A 116(2) . . ? C94A C92A C93A 109.7(19) . . ? C91A C92A C93A 104.4(15) . . ? O9 C91B C92B 123(2) . . ? C91B C92B C93B 116(2) . . ? C91B C92B C94B 112(3) . . ? C93B C92B C94B 111(2) . . ? #===END