# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 #TrackingRef '- 1_2C7H8_3C7H8.cif' #=============================================================================== # 1. SUBMISSION DETAILS _publ_contact_author # Name and address of author for correspondence ; Marta E. G. Mosquera Departamento de Qu\'imica Inorg\'anica Facultad de Farmacia Universidad de Alcal\'a Campus Universitario 28871 Alcal\'a de Henares Spain ; _publ_contact_author_phone '0034 91 8854779' _publ_contact_author_fax '0034 91 8854683' _publ_contact_author_email martaeg.mosquera@uah.es _publ_contact_letter ; Alcal\'a 07/07/2011 Please receive the CIF for compounds 1, 2.C7H8 and 3.C7H8 submitted to be published in Chem. Commun. Thank you very much. Dr. Marta E. G. Mosquera. ; #============================================================================== # 2. PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ? _journal_techeditor_code ? _journal_techeditor_notes ? _journal_coden_ASTM ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #============================================================================== # 3. TITLE AND AUTHOR LIST _publ_section_title ; Crystal structures of compounds 1, 2 and 3 ; # The loop structure below should contain the names and addresses of all #authors, in the required order of publication. Repeat as necessary. loop_ _publ_author_address ; Departamento de Qu\'imica Inorg\'anica Facultad de Farmacia Universidad de Alcal\'a Campus Universitario 28871 Alcal\'a de Henares Spain ; _publ_contact_author_name 'Marta E. G. Mosquera' loop_ _publ_author_name 'Mayte Munoz' 'Carmen Urbaneja' 'Manuel Temprado' 'Marta E. G. Mosquera' 'Tomas Cuenca' #========================================================================== data_1 _database_code_depnum_ccdc_archive 'CCDC 835936' #TrackingRef '- 1_2C7H8_3C7H8.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H54 Li6 O18' _chemical_formula_weight 960.55 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/a loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x-1/2, -y-1/2, z' _cell_length_a 12.0342(9) _cell_length_b 16.482(3) _cell_length_c 12.6028(16) _cell_angle_alpha 90.00 _cell_angle_beta 111.669(13) _cell_angle_gamma 90.00 _cell_volume 2323.1(5) _cell_formula_units_Z 2 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 31 _cell_measurement_theta_max 20.09 _cell_measurement_theta_min 3.78 _exptl_crystal_description prism _exptl_crystal_colour white _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.33 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.373 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1008 _exptl_absorpt_coefficient_mu 0.102 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; R.H. Blessing, Acta Cryst. (1995), A51, 33-38 ; _exptl_absorpt_correction_T_min 0.864 _exptl_absorpt_correction_T_max 1.408 _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 52973 _diffrn_reflns_av_R_equivalents 0.0758 _diffrn_reflns_av_sigmaI/netI 0.0578 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.07 _diffrn_reflns_theta_max 27.53 _reflns_number_total 5337 _reflns_number_gt 3475 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)' _computing_data_reduction 'EvalCCD (Duisenberg & Schreurs 1990-2000)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.0565P)^2^+1.4455P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5337 _refine_ls_number_parameters 325 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1007 _refine_ls_R_factor_gt 0.0555 _refine_ls_wR_factor_ref 0.1457 _refine_ls_wR_factor_gt 0.1258 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.026 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Li1 Li 0.5698(3) 0.1103(2) 0.5672(3) 0.0320(8) Uani 1 1 d . . . Li2 Li 0.4042(3) 0.0357(2) 0.3310(3) 0.0320(8) Uani 1 1 d . . . Li3 Li 0.3473(3) -0.0313(2) 0.5693(3) 0.0324(8) Uani 1 1 d . . . O1 O 0.46789(12) 0.05392(9) 0.63030(12) 0.0277(3) Uani 1 1 d . . . O2 O 0.52435(13) 0.11750(9) 0.40553(12) 0.0285(3) Uani 1 1 d . . . O3 O 0.31095(12) -0.02206(9) 0.40486(12) 0.0274(3) Uani 1 1 d . . . O4 O 0.59116(14) 0.18907(10) 0.69922(13) 0.0364(4) Uani 1 1 d . . . O6 O 0.70141(16) 0.22594(11) 0.48444(16) 0.0492(5) Uani 1 1 d . . . O7 O 0.33532(14) 0.14282(10) 0.21783(13) 0.0369(4) Uani 1 1 d . . . O5 O 0.34123(15) -0.01414(11) 0.73846(13) 0.0390(4) Uani 1 1 d . . . O8 O 0.26501(13) -0.02949(10) 0.18387(12) 0.0332(4) Uani 1 1 d . . . O9 O 0.14977(14) -0.05476(12) 0.49503(13) 0.0416(4) Uani 1 1 d . . . C1 C 0.46496(17) 0.08995(13) 0.72319(16) 0.0250(4) Uani 1 1 d . . . C2 C 0.52816(19) 0.16152(13) 0.76493(18) 0.0285(5) Uani 1 1 d . . . C3 C 0.5251(2) 0.19935(15) 0.8615(2) 0.0374(5) Uani 1 1 d . . . H3 H 0.5667 0.2475 0.8869 0.045 Uiso 1 1 calc R . . C4 C 0.4599(2) 0.16526(16) 0.9205(2) 0.0401(6) Uani 1 1 d . . . H4 H 0.4579 0.1905 0.9858 0.048 Uiso 1 1 calc R . . C5 C 0.3974(2) 0.09351(16) 0.88244(19) 0.0364(5) Uani 1 1 d . . . H5 H 0.3540 0.0703 0.9222 0.044 Uiso 1 1 calc R . . C6 C 0.40033(18) 0.05698(14) 0.78523(18) 0.0296(5) Uani 1 1 d . . . C7 C 0.6914(2) 0.24025(16) 0.7536(2) 0.0449(6) Uani 1 1 d . . . H7A H 0.7279 0.2545 0.7000 0.067 Uiso 1 1 calc R . . H7B H 0.7485 0.2121 0.8171 0.067 Uiso 1 1 calc R . . H7C H 0.6656 0.2886 0.7802 0.067 Uiso 1 1 calc R . . C8 C 0.3237(3) -0.07152(19) 0.8132(2) 0.0612(8) Uani 1 1 d . . . H8A H 0.2815 -0.1175 0.7703 0.092 Uiso 1 1 calc R . . H8B H 0.2779 -0.0475 0.8533 0.092 Uiso 1 1 calc R . . H8C H 0.3998 -0.0888 0.8671 0.092 Uiso 1 1 calc R . . C11 C 0.20079(17) -0.04080(12) 0.33571(17) 0.0233(4) Uani 1 1 d . . . C12 C 0.16994(18) -0.04497(12) 0.21714(17) 0.0248(4) Uani 1 1 d . . . C13 C 0.0548(2) -0.06313(14) 0.14351(18) 0.0316(5) Uani 1 1 d . . . H13 H 0.0362 -0.0658 0.0651 0.038 Uiso 1 1 calc R . . C14 C -0.0320(2) -0.07721(15) 0.1889(2) 0.0367(5) Uani 1 1 d . . . H14 H -0.1100 -0.0882 0.1401 0.044 Uiso 1 1 calc R . . C15 C -0.0050(2) -0.07527(15) 0.3050(2) 0.0366(6) Uani 1 1 d . . . H15 H -0.0640 -0.0853 0.3345 0.044 Uiso 1 1 calc R . . C16 C 0.11125(19) -0.05822(14) 0.37744(18) 0.0292(5) Uani 1 1 d . . . C17 C 0.0746(3) -0.0947(2) 0.5456(2) 0.0560(8) Uani 1 1 d . . . H17A H 0.1088 -0.0886 0.6271 0.084 Uiso 1 1 calc R . . H17B H 0.0686 -0.1513 0.5264 0.084 Uiso 1 1 calc R . . H17C H -0.0036 -0.0707 0.5169 0.084 Uiso 1 1 calc R . . C18 C 0.2496(2) -0.04572(18) 0.0686(2) 0.0449(6) Uani 1 1 d . . . H18A H 0.3220 -0.0329 0.0568 0.067 Uiso 1 1 calc R . . H18B H 0.1854 -0.0131 0.0187 0.067 Uiso 1 1 calc R . . H18C H 0.2310 -0.1021 0.0522 0.067 Uiso 1 1 calc R . . C21 C 0.51714(19) 0.18730(13) 0.34969(18) 0.0268(5) Uani 1 1 d . . . C22 C 0.6065(2) 0.24633(15) 0.3869(2) 0.0341(5) Uani 1 1 d . . . C23 C 0.5974(2) 0.31912(15) 0.3284(2) 0.0450(7) Uani 1 1 d . . . H23 H 0.6577 0.3578 0.3544 0.054 Uiso 1 1 calc R . . C24 C 0.4978(3) 0.33336(16) 0.2311(3) 0.0474(7) Uani 1 1 d . . . H24 H 0.4912 0.3821 0.1921 0.057 Uiso 1 1 calc R . . C25 C 0.4084(2) 0.27660(15) 0.1912(2) 0.0405(6) Uani 1 1 d . . . H25 H 0.3419 0.2865 0.1254 0.049 Uiso 1 1 calc R . . C26 C 0.4189(2) 0.20410(13) 0.25063(19) 0.0299(5) Uani 1 1 d . . . C27 C 0.2288(2) 0.15854(18) 0.1224(2) 0.0466(7) Uani 1 1 d . . . H27A H 0.1774 0.1120 0.1077 0.070 Uiso 1 1 calc R . . H27B H 0.2484 0.1697 0.0566 0.070 Uiso 1 1 calc R . . H27C H 0.1886 0.2046 0.1384 0.070 Uiso 1 1 calc R . . C28 C 0.7996(3) 0.2808(2) 0.5205(3) 0.0703(10) Uani 1 1 d . . . H28A H 0.8599 0.2609 0.5893 0.105 Uiso 1 1 calc R . . H28B H 0.7727 0.3331 0.5347 0.105 Uiso 1 1 calc R . . H28C H 0.8323 0.2855 0.4619 0.105 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Li1 0.0319(19) 0.042(2) 0.0232(18) 0.0008(16) 0.0111(15) -0.0018(16) Li2 0.0296(18) 0.036(2) 0.0299(19) -0.0026(16) 0.0110(16) -0.0069(16) Li3 0.0282(18) 0.043(2) 0.0231(18) -0.0020(16) 0.0061(15) -0.0045(16) O1 0.0274(7) 0.0350(8) 0.0215(7) -0.0038(6) 0.0099(6) -0.0030(6) O2 0.0305(8) 0.0298(8) 0.0227(7) 0.0028(6) 0.0067(6) -0.0047(6) O3 0.0215(7) 0.0375(9) 0.0206(7) -0.0018(6) 0.0047(6) -0.0053(6) O4 0.0426(9) 0.0349(9) 0.0347(9) -0.0046(7) 0.0176(8) -0.0116(7) O6 0.0426(10) 0.0520(12) 0.0458(11) -0.0073(9) 0.0078(9) -0.0201(8) O7 0.0334(8) 0.0380(9) 0.0318(9) 0.0035(7) 0.0033(7) -0.0014(7) O5 0.0419(9) 0.0487(10) 0.0283(8) -0.0011(7) 0.0152(7) -0.0173(8) O8 0.0315(8) 0.0469(10) 0.0218(8) 0.0031(7) 0.0104(6) 0.0000(7) O9 0.0321(9) 0.0711(12) 0.0239(8) 0.0024(8) 0.0128(7) -0.0060(8) C1 0.0233(10) 0.0344(12) 0.0163(10) 0.0017(8) 0.0061(8) 0.0053(9) C2 0.0310(11) 0.0287(12) 0.0255(11) 0.0023(9) 0.0101(9) 0.0033(9) C3 0.0439(13) 0.0334(13) 0.0330(13) -0.0062(10) 0.0122(11) 0.0020(11) C4 0.0477(14) 0.0467(15) 0.0279(12) -0.0044(11) 0.0161(11) 0.0103(12) C5 0.0342(12) 0.0518(15) 0.0275(12) 0.0018(11) 0.0165(10) 0.0042(11) C6 0.0241(10) 0.0368(13) 0.0253(11) 0.0000(9) 0.0062(9) 0.0000(9) C7 0.0448(14) 0.0390(14) 0.0516(16) -0.0065(12) 0.0185(13) -0.0117(12) C8 0.090(2) 0.0520(18) 0.0395(16) 0.0060(13) 0.0215(16) -0.0158(17) C11 0.0215(10) 0.0228(10) 0.0228(10) 0.0014(8) 0.0049(8) -0.0001(8) C12 0.0265(10) 0.0225(10) 0.0234(10) 0.0020(8) 0.0070(8) 0.0015(8) C13 0.0341(12) 0.0317(12) 0.0219(11) 0.0010(9) 0.0019(9) 0.0021(10) C14 0.0267(11) 0.0378(13) 0.0359(13) 0.0007(11) 0.0003(10) -0.0067(10) C15 0.0272(11) 0.0440(14) 0.0375(13) 0.0039(11) 0.0108(10) -0.0060(10) C16 0.0275(11) 0.0363(12) 0.0224(11) 0.0018(9) 0.0075(9) -0.0029(9) C17 0.0512(16) 0.083(2) 0.0417(15) 0.0158(15) 0.0267(13) -0.0028(15) C18 0.0465(14) 0.0666(18) 0.0242(12) 0.0066(12) 0.0161(11) 0.0121(13) C21 0.0338(11) 0.0264(11) 0.0257(11) -0.0023(9) 0.0174(9) -0.0019(9) C22 0.0368(12) 0.0359(13) 0.0348(13) -0.0072(10) 0.0193(11) -0.0061(10) C23 0.0561(16) 0.0291(13) 0.0636(18) -0.0052(12) 0.0381(15) -0.0107(12) C24 0.0625(17) 0.0304(14) 0.0642(19) 0.0122(12) 0.0409(16) 0.0057(12) C25 0.0498(15) 0.0379(14) 0.0394(14) 0.0105(11) 0.0230(12) 0.0120(12) C26 0.0358(12) 0.0278(11) 0.0315(12) -0.0010(9) 0.0188(10) 0.0007(9) C27 0.0349(13) 0.0562(17) 0.0386(14) 0.0038(12) 0.0018(11) 0.0070(12) C28 0.0533(18) 0.083(2) 0.069(2) -0.0222(18) 0.0157(16) -0.0388(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Li1 O2 1.908(4) . ? Li1 O1 1.929(4) . ? Li1 O3 1.982(4) 3_656 ? Li1 O4 2.050(4) . ? Li1 Li3 2.630(5) 3_656 ? Li1 Li2 2.691(5) 3_656 ? Li1 C1 2.720(4) . ? Li1 Li2 3.157(5) . ? Li2 O2 1.946(4) . ? Li2 O3 1.951(4) . ? Li2 O1 2.058(4) 3_656 ? Li2 O7 2.228(4) . ? Li2 O8 2.260(4) . ? Li2 Li1 2.691(5) 3_656 ? Li2 C11 2.774(4) . ? Li2 Li3 2.783(5) 3_656 ? Li2 Li3 3.496(5) . ? Li3 O3 1.959(4) . ? Li3 O1 1.961(4) . ? Li3 O2 2.035(4) 3_656 ? Li3 O5 2.179(4) . ? Li3 O9 2.244(4) . ? Li3 Li1 2.630(5) 3_656 ? Li3 C1 2.780(4) . ? Li3 Li2 2.783(5) 3_656 ? O1 C1 1.325(2) . ? O1 Li2 2.058(4) 3_656 ? O2 C21 1.335(3) . ? O2 Li3 2.035(4) 3_656 ? O3 C11 1.326(2) . ? O3 Li1 1.982(4) 3_656 ? O4 C2 1.389(3) . ? O4 C7 1.424(3) . ? O6 C22 1.376(3) . ? O6 C28 1.423(3) . ? O7 C26 1.377(3) . ? O7 C27 1.421(3) . ? O5 C6 1.385(3) . ? O5 C8 1.405(3) . ? O8 C12 1.380(3) . ? O8 C18 1.421(3) . ? O9 C16 1.381(3) . ? O9 C17 1.443(3) . ? C1 C2 1.397(3) . ? C1 C6 1.400(3) . ? C2 C3 1.380(3) . ? C3 C4 1.383(3) . ? C4 C5 1.389(4) . ? C5 C6 1.377(3) . ? C11 C16 1.392(3) . ? C11 C12 1.402(3) . ? C12 C13 1.386(3) . ? C13 C14 1.383(3) . ? C14 C15 1.377(3) . ? C15 C16 1.388(3) . ? C21 C26 1.394(3) . ? C21 C22 1.397(3) . ? C22 C23 1.391(4) . ? C23 C24 1.382(4) . ? C24 C25 1.373(4) . ? C25 C26 1.391(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 O2 Li1 O1 119.7(2) . . ? O2 Li1 O3 97.96(18) . 3_656 ? O1 Li1 O3 95.84(18) . 3_656 ? O2 Li1 O4 136.7(2) . . ? O1 Li1 O4 83.05(15) . . ? O3 Li1 O4 117.07(19) 3_656 . ? O2 Li1 Li3 50.27(13) . 3_656 ? O1 Li1 Li3 118.9(2) . 3_656 ? O3 Li1 Li3 47.77(12) 3_656 3_656 ? O4 Li1 Li3 151.7(2) . 3_656 ? O2 Li1 Li2 120.1(2) . 3_656 ? O1 Li1 Li2 49.60(13) . 3_656 ? O3 Li1 Li2 46.33(12) 3_656 3_656 ? O4 Li1 Li2 102.81(17) . 3_656 ? Li3 Li1 Li2 82.14(16) 3_656 3_656 ? O2 Li1 C1 138.82(18) . . ? O1 Li1 C1 26.81(8) . . ? O3 Li1 C1 106.23(16) 3_656 . ? O4 Li1 C1 56.25(11) . . ? Li3 Li1 C1 143.16(19) 3_656 . ? Li2 Li1 C1 63.14(12) 3_656 . ? O2 Li1 Li2 35.41(11) . . ? O1 Li1 Li2 85.69(15) . . ? O3 Li1 Li2 92.58(16) 3_656 . ? O4 Li1 Li2 149.13(18) . . ? Li3 Li1 Li2 56.63(13) 3_656 . ? Li2 Li1 Li2 91.31(15) 3_656 . ? C1 Li1 Li2 109.49(14) . . ? O2 Li2 O3 124.3(2) . . ? O2 Li2 O1 91.47(16) . 3_656 ? O3 Li2 O1 92.77(17) . 3_656 ? O2 Li2 O7 78.15(15) . . ? O3 Li2 O7 123.26(19) . . ? O1 Li2 O7 142.1(2) 3_656 . ? O2 Li2 O8 156.8(2) . . ? O3 Li2 O8 77.09(13) . . ? O1 Li2 O8 96.67(16) 3_656 . ? O7 Li2 O8 82.16(14) . . ? O2 Li2 Li1 117.05(19) . 3_656 ? O3 Li2 Li1 47.30(12) . 3_656 ? O1 Li2 Li1 45.56(12) 3_656 3_656 ? O7 Li2 Li1 164.60(19) . 3_656 ? O8 Li2 Li1 83.47(15) . 3_656 ? O2 Li2 C11 143.98(19) . . ? O3 Li2 C11 25.83(8) . . ? O1 Li2 C11 104.92(16) 3_656 . ? O7 Li2 C11 104.54(15) . . ? O8 Li2 C11 53.74(9) . . ? Li1 Li2 C11 62.05(12) 3_656 . ? O2 Li2 Li3 46.97(12) . 3_656 ? O3 Li2 Li3 118.89(19) . 3_656 ? O1 Li2 Li3 44.73(12) 3_656 3_656 ? O7 Li2 Li3 113.18(17) . 3_656 ? O8 Li2 Li3 134.86(19) . 3_656 ? Li1 Li2 Li3 81.08(15) 3_656 3_656 ? C11 Li2 Li3 141.97(18) . 3_656 ? O2 Li2 Li1 34.62(10) . . ? O3 Li2 Li1 90.82(15) . . ? O1 Li2 Li1 84.25(14) 3_656 . ? O7 Li2 Li1 104.54(16) . . ? O8 Li2 Li1 167.89(18) . . ? Li1 Li2 Li1 88.69(15) 3_656 . ? C11 Li2 Li1 114.31(14) . . ? Li3 Li2 Li1 52.10(12) 3_656 . ? O2 Li2 Li3 98.65(15) . . ? O3 Li2 Li3 26.65(9) . . ? O1 Li2 Li3 86.34(14) 3_656 . ? O7 Li2 Li3 130.94(17) . . ? O8 Li2 Li3 103.51(14) . . ? Li1 Li2 Li3 48.18(12) 3_656 . ? C11 Li2 Li3 51.96(10) . . ? Li3 Li2 Li3 97.02(14) 3_656 . ? Li1 Li2 Li3 64.45(11) . . ? O3 Li3 O1 101.74(18) . . ? O3 Li3 O2 94.57(17) . 3_656 ? O1 Li3 O2 91.73(16) . 3_656 ? O3 Li3 O5 161.8(2) . . ? O1 Li3 O5 79.09(14) . . ? O2 Li3 O5 103.63(17) 3_656 . ? O3 Li3 O9 77.51(13) . . ? O1 Li3 O9 143.5(2) . . ? O2 Li3 O9 124.8(2) 3_656 . ? O5 Li3 O9 90.97(15) . . ? O3 Li3 Li1 48.50(12) . 3_656 ? O1 Li3 Li1 101.96(17) . 3_656 ? O2 Li3 Li1 46.14(12) 3_656 3_656 ? O5 Li3 Li1 149.6(2) . 3_656 ? O9 Li3 Li1 103.95(16) . 3_656 ? O3 Li3 C1 122.65(18) . . ? O1 Li3 C1 25.75(8) . . ? O2 Li3 C1 103.38(15) 3_656 . ? O5 Li3 C1 54.31(10) . . ? O9 Li3 C1 127.07(17) . . ? Li1 Li3 C1 126.44(16) 3_656 . ? O3 Li3 Li2 105.25(17) . 3_656 ? O1 Li3 Li2 47.61(12) . 3_656 ? O2 Li3 Li2 44.34(11) 3_656 3_656 ? O5 Li3 Li2 88.87(15) . 3_656 ? O9 Li3 Li2 168.5(2) . 3_656 ? Li1 Li3 Li2 71.28(15) 3_656 3_656 ? C1 Li3 Li2 61.22(12) . 3_656 ? O3 Li3 Li2 26.53(9) . . ? O1 Li3 Li2 76.09(13) . . ? O2 Li3 Li2 88.66(14) 3_656 . ? O5 Li3 Li2 152.58(18) . . ? O9 Li3 Li2 102.11(14) . . ? Li1 Li3 Li2 49.68(12) 3_656 . ? C1 Li3 Li2 99.30(13) . . ? Li2 Li3 Li2 82.98(14) 3_656 . ? C1 O1 Li1 112.12(17) . . ? C1 O1 Li3 114.24(17) . . ? Li1 O1 Li3 132.41(17) . . ? C1 O1 Li2 111.96(16) . 3_656 ? Li1 O1 Li2 84.84(16) . 3_656 ? Li3 O1 Li2 87.66(16) . 3_656 ? C21 O2 Li1 123.61(18) . . ? C21 O2 Li2 116.78(17) . . ? Li1 O2 Li2 109.97(17) . . ? C21 O2 Li3 125.59(17) . 3_656 ? Li1 O2 Li3 83.59(16) . 3_656 ? Li2 O2 Li3 88.69(17) . 3_656 ? C11 O3 Li2 114.32(16) . . ? C11 O3 Li3 117.12(16) . . ? Li2 O3 Li3 126.82(17) . . ? C11 O3 Li1 115.36(17) . 3_656 ? Li2 O3 Li1 86.36(16) . 3_656 ? Li3 O3 Li1 83.73(16) . 3_656 ? C2 O4 C7 117.32(18) . . ? C2 O4 Li1 110.14(16) . . ? C7 O4 Li1 126.56(18) . . ? C22 O6 C28 116.6(2) . . ? C26 O7 C27 116.81(19) . . ? C26 O7 Li2 109.35(16) . . ? C27 O7 Li2 133.84(18) . . ? C6 O5 C8 117.71(19) . . ? C6 O5 Li3 109.19(16) . . ? C8 O5 Li3 129.5(2) . . ? C12 O8 C18 117.80(18) . . ? C12 O8 Li2 106.58(15) . . ? C18 O8 Li2 134.91(18) . . ? C16 O9 C17 115.99(19) . . ? C16 O9 Li3 109.79(15) . . ? C17 O9 Li3 129.41(18) . . ? O1 C1 C2 121.53(19) . . ? O1 C1 C6 121.4(2) . . ? C2 C1 C6 117.05(19) . . ? O1 C1 Li1 41.06(12) . . ? C2 C1 Li1 80.48(15) . . ? C6 C1 Li1 162.34(18) . . ? O1 C1 Li3 40.01(12) . . ? C2 C1 Li3 159.35(17) . . ? C6 C1 Li3 82.30(15) . . ? Li1 C1 Li3 80.62(12) . . ? C3 C2 O4 125.2(2) . . ? C3 C2 C1 121.7(2) . . ? O4 C2 C1 113.11(18) . . ? C2 C3 C4 119.7(2) . . ? C3 C4 C5 120.2(2) . . ? C6 C5 C4 119.4(2) . . ? C5 C6 O5 124.8(2) . . ? C5 C6 C1 121.9(2) . . ? O5 C6 C1 113.24(18) . . ? O3 C11 C16 121.67(18) . . ? O3 C11 C12 121.25(18) . . ? C16 C11 C12 117.07(18) . . ? O3 C11 Li2 39.85(12) . . ? C16 C11 Li2 156.07(17) . . ? C12 C11 Li2 83.57(14) . . ? O8 C12 C13 124.94(19) . . ? O8 C12 C11 113.07(17) . . ? C13 C12 C11 122.0(2) . . ? C14 C13 C12 118.7(2) . . ? C15 C14 C13 121.2(2) . . ? C14 C15 C16 119.3(2) . . ? O9 C16 C15 124.9(2) . . ? O9 C16 C11 113.39(18) . . ? C15 C16 C11 121.7(2) . . ? O2 C21 C26 120.79(19) . . ? O2 C21 C22 122.1(2) . . ? C26 C21 C22 117.1(2) . . ? O6 C22 C23 124.1(2) . . ? O6 C22 C21 114.3(2) . . ? C23 C22 C21 121.5(2) . . ? C24 C23 C22 119.3(2) . . ? C25 C24 C23 121.0(2) . . ? C24 C25 C26 119.0(2) . . ? O7 C26 C25 123.9(2) . . ? O7 C26 C21 114.02(19) . . ? C25 C26 C21 122.1(2) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.53 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.302 _refine_diff_density_min -0.238 _refine_diff_density_rms 0.050 #====== END data_2.C7H8 _database_code_depnum_ccdc_archive 'CCDC 835937' #TrackingRef '- 1_2C7H8_3C7H8.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C33 H54 Al3 Li3 O9.C7 H8' _chemical_formula_sum 'C40 H62 Al3 Li3 O9' _chemical_formula_weight 788.66 _chemical_compound_source 'synthesis as described' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.8598(13) _cell_length_b 22.364(3) _cell_length_c 21.162(5) _cell_angle_alpha 90.00 _cell_angle_beta 99.163(14) _cell_angle_gamma 90.00 _cell_volume 4606.6(14) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 51 _cell_measurement_theta_min 3.987 _cell_measurement_theta_max 19.023 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.47 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.3 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.137 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1688 _exptl_absorpt_coefficient_mu 0.129 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; R.H. Blessing, Acta Cryst. (1995), A51, 33-38 ; _exptl_absorpt_correction_T_min 0.755 _exptl_absorpt_correction_T_max 1.163 _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 81139 _diffrn_reflns_av_R_equivalents 0.0662 _diffrn_reflns_av_sigmaI/netI 0.0556 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 3.05 _diffrn_reflns_theta_max 25.91 _reflns_number_total 8911 _reflns_number_gt 6058 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)' _computing_data_reduction 'EvalCCD (Duisenberg & Schreurs 1990-2000)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.0862P)^2^+2.6033P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8911 _refine_ls_number_parameters 433 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1024 _refine_ls_R_factor_gt 0.0670 _refine_ls_wR_factor_ref 0.1832 _refine_ls_wR_factor_gt 0.1644 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.050 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.003 0.000 0.000 288 33 ' ' 2 0.000 0.500 0.000 203 29 ' ' 3 0.085 0.500 0.500 288 33 ' ' 4 0.500 0.000 0.500 203 29 ' ' _platon_squeeze_details ; ; 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 -0.07594(10) 0.31551(4) 0.45296(4) 0.0416(2) Uani 1 1 d . . . Al2 Al 0.19341(9) 0.26481(4) 0.23027(4) 0.0410(2) Uani 1 1 d . . . Al3 Al 0.00034(8) 0.08164(4) 0.32541(4) 0.0356(2) Uani 1 1 d . . . Li1 Li 0.1543(6) 0.2998(2) 0.3607(3) 0.0499(13) Uani 1 1 d . . . Li2 Li -0.0789(5) 0.2099(2) 0.2431(2) 0.0405(11) Uani 1 1 d . . . Li3 Li -0.0946(5) 0.1901(2) 0.4003(2) 0.0425(11) Uani 1 1 d . . . O1 O 0.04505(19) 0.25847(8) 0.42553(8) 0.0360(4) Uani 1 1 d . . . O2 O 0.04075(19) 0.28107(8) 0.27125(9) 0.0349(4) Uani 1 1 d . . . O3 O -0.11316(17) 0.15183(8) 0.31368(8) 0.0295(4) Uani 1 1 d . . . O4 O 0.2917(2) 0.30986(11) 0.44375(11) 0.0535(6) Uani 1 1 d . . . O5 O -0.0056(2) 0.16016(9) 0.48731(9) 0.0466(5) Uani 1 1 d . . . O6 O 0.1651(2) 0.38100(10) 0.31214(12) 0.0570(6) Uani 1 1 d . . . O7 O -0.2209(2) 0.27760(8) 0.21651(9) 0.0396(5) Uani 1 1 d . . . O8 O -0.2056(2) 0.14330(9) 0.18973(9) 0.0429(5) Uani 1 1 d . . . O9 O -0.2834(2) 0.14919(9) 0.39969(9) 0.0435(5) Uani 1 1 d . . . C1 C 0.2258(4) 0.32793(18) 0.16939(18) 0.0642(10) Uani 1 1 d . . . H1A H 0.2574 0.3643 0.1930 0.096 Uiso 1 1 calc R . . H1B H 0.1401 0.3363 0.1403 0.096 Uiso 1 1 calc R . . H1C H 0.2959 0.3145 0.1445 0.096 Uiso 1 1 calc R . . C2 C 0.3477(3) 0.25693(15) 0.30267(16) 0.0507(8) Uani 1 1 d . . . H2A H 0.3168 0.2344 0.3375 0.076 Uiso 1 1 calc R . . H2B H 0.3783 0.2968 0.3181 0.076 Uiso 1 1 calc R . . H2C H 0.4241 0.2357 0.2881 0.076 Uiso 1 1 calc R . . C3 C 0.1315(4) 0.19000(16) 0.18481(16) 0.0529(8) Uani 1 1 d . . . H3A H 0.1275 0.1579 0.2160 0.079 Uiso 1 1 calc R . . H3B H 0.1962 0.1790 0.1561 0.079 Uiso 1 1 calc R . . H3C H 0.0400 0.1960 0.1598 0.079 Uiso 1 1 calc R . . C4 C 0.0136(4) 0.39479(16) 0.4528(2) 0.0674(10) Uani 1 1 d . . . H4A H 0.0283 0.4045 0.4092 0.101 Uiso 1 1 calc R . . H4B H 0.1023 0.3938 0.4813 0.101 Uiso 1 1 calc R . . H4C H -0.0454 0.4252 0.4677 0.101 Uiso 1 1 calc R . . C5 C -0.1103(4) 0.29202(17) 0.53912(16) 0.0585(9) Uani 1 1 d . . . H5A H -0.1550 0.2528 0.5368 0.088 Uiso 1 1 calc R . . H5B H -0.1702 0.3217 0.5548 0.088 Uiso 1 1 calc R . . H5C H -0.0229 0.2900 0.5685 0.088 Uiso 1 1 calc R . . C6 C -0.2388(3) 0.30320(17) 0.38591(16) 0.0546(9) Uani 1 1 d . . . H6A H -0.2171 0.3159 0.3444 0.082 Uiso 1 1 calc R . . H6B H -0.3160 0.3268 0.3963 0.082 Uiso 1 1 calc R . . H6C H -0.2637 0.2607 0.3840 0.082 Uiso 1 1 calc R . . C7 C -0.0014(4) 0.03798(15) 0.24380(17) 0.0569(9) Uani 1 1 d . . . H7A H -0.0928 0.0209 0.2299 0.085 Uiso 1 1 calc R . . H7B H 0.0669 0.0058 0.2501 0.085 Uiso 1 1 calc R . . H7C H 0.0209 0.0657 0.2111 0.085 Uiso 1 1 calc R . . C8 C 0.1794(3) 0.11855(18) 0.35833(18) 0.0582(9) Uani 1 1 d . . . H8A H 0.2088 0.1434 0.3248 0.087 Uiso 1 1 calc R . . H8B H 0.2477 0.0871 0.3709 0.087 Uiso 1 1 calc R . . H8C H 0.1707 0.1435 0.3956 0.087 Uiso 1 1 calc R . . C9 C -0.0749(3) 0.02860(14) 0.38599(15) 0.0471(8) Uani 1 1 d . . . H9A H -0.1635 0.0125 0.3655 0.071 Uiso 1 1 calc R . . H9B H -0.0877 0.0514 0.4241 0.071 Uiso 1 1 calc R . . H9C H -0.0108 -0.0044 0.3984 0.071 Uiso 1 1 calc R . . C11 C -0.3807(4) 0.15691(18) 0.44385(18) 0.0640(10) Uani 1 1 d . . . H11A H -0.3313 0.1685 0.4860 0.096 Uiso 1 1 calc R . . H11B H -0.4295 0.1192 0.4476 0.096 Uiso 1 1 calc R . . H11C H -0.4469 0.1882 0.4278 0.096 Uiso 1 1 calc R . . C20 C -0.3389(3) 0.13276(12) 0.33792(14) 0.0350(6) Uani 1 1 d . . . C21 C -0.4733(3) 0.11418(14) 0.31866(17) 0.0481(8) Uani 1 1 d . . . H21 H -0.5338 0.1096 0.3490 0.058 Uiso 1 1 calc R . . C22 C -0.5177(3) 0.10255(14) 0.25487(18) 0.0503(8) Uani 1 1 d . . . H22 H -0.6089 0.0887 0.2417 0.060 Uiso 1 1 calc R . . C24 C -0.4327(3) 0.11049(13) 0.20967(16) 0.0459(8) Uani 1 1 d . . . H24 H -0.4659 0.1036 0.1656 0.055 Uiso 1 1 calc R . . C25 C -0.2988(3) 0.12855(12) 0.22947(14) 0.0364(6) Uani 1 1 d . . . C27 C -0.2490(3) 0.13732(11) 0.29416(13) 0.0301(6) Uani 1 1 d . . . C30 C 0.2501(5) 0.4333(2) 0.3169(3) 0.1056(18) Uani 1 1 d . . . H30A H 0.3414 0.4235 0.3402 0.158 Uiso 1 1 calc R . . H30B H 0.2085 0.4647 0.3398 0.158 Uiso 1 1 calc R . . H30C H 0.2586 0.4474 0.2738 0.158 Uiso 1 1 calc R . . C31 C -0.0492(5) 0.11502(16) 0.52800(17) 0.0666(11) Uani 1 1 d . . . H31A H -0.1421 0.1017 0.5102 0.100 Uiso 1 1 calc R . . H31B H -0.0492 0.1316 0.5709 0.100 Uiso 1 1 calc R . . H31C H 0.0140 0.0810 0.5307 0.100 Uiso 1 1 calc R . . C32 C 0.4168(4) 0.3438(2) 0.4575(2) 0.0816(13) Uani 1 1 d . . . H32A H 0.4145 0.3767 0.4268 0.122 Uiso 1 1 calc R . . H32B H 0.4953 0.3178 0.4542 0.122 Uiso 1 1 calc R . . H32C H 0.4259 0.3601 0.5010 0.122 Uiso 1 1 calc R . . C33 C -0.2396(4) 0.12762(19) 0.12378(16) 0.0673(11) Uani 1 1 d . . . H33A H -0.1656 0.1405 0.1009 0.101 Uiso 1 1 calc R . . H33B H -0.3254 0.1474 0.1053 0.101 Uiso 1 1 calc R . . H33C H -0.2511 0.0842 0.1198 0.101 Uiso 1 1 calc R . . C34 C 0.1468(3) 0.23556(13) 0.47145(13) 0.0381(7) Uani 1 1 d . . . C35 C 0.2252(4) 0.16073(18) 0.55098(16) 0.0602(10) Uani 1 1 d . . . H35 H 0.2075 0.1262 0.5746 0.072 Uiso 1 1 calc R . . C36 C 0.3515(4) 0.1879(2) 0.56172(17) 0.0665(11) Uani 1 1 d . . . H36 H 0.4214 0.1718 0.5933 0.080 Uiso 1 1 calc R . . C37 C 0.3800(4) 0.23785(19) 0.52803(16) 0.0601(10) Uani 1 1 d . . . H37 H 0.4684 0.2558 0.5358 0.072 Uiso 1 1 calc R . . C38 C 0.2764(3) 0.26151(15) 0.48241(14) 0.0457(8) Uani 1 1 d . . . C39 C 0.1235(3) 0.18481(14) 0.50470(14) 0.0444(7) Uani 1 1 d . . . C41 C -0.3673(3) 0.27492(16) 0.19639(17) 0.0549(9) Uani 1 1 d . . . H41A H -0.3950 0.2333 0.1873 0.082 Uiso 1 1 calc R . . H41B H -0.3925 0.2991 0.1577 0.082 Uiso 1 1 calc R . . H41C H -0.4139 0.2905 0.2305 0.082 Uiso 1 1 calc R . . C42 C -0.0371(4) 0.44086(15) 0.26805(18) 0.0626(10) Uani 1 1 d . . . H42 H 0.0070 0.4777 0.2806 0.075 Uiso 1 1 calc R . . C44 C -0.2380(4) 0.38733(15) 0.22026(16) 0.0521(8) Uani 1 1 d . . . H44 H -0.3315 0.3876 0.2005 0.063 Uiso 1 1 calc R . . C45 C -0.1711(4) 0.43974(15) 0.23835(18) 0.0650(10) Uani 1 1 d . . . H45 H -0.2191 0.4765 0.2301 0.078 Uiso 1 1 calc R . . C46 C -0.1668(3) 0.33388(13) 0.23123(13) 0.0385(7) Uani 1 1 d . . . C47 C 0.0325(3) 0.38761(14) 0.27936(15) 0.0468(8) Uani 1 1 d . . . C48 C -0.0300(3) 0.33346(12) 0.26012(13) 0.0368(6) Uani 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 0.0442(5) 0.0399(5) 0.0413(5) 0.0023(4) 0.0087(4) 0.0040(4) Al2 0.0377(5) 0.0442(5) 0.0430(5) 0.0053(4) 0.0125(4) -0.0013(4) Al3 0.0304(4) 0.0352(5) 0.0422(5) 0.0044(4) 0.0092(4) 0.0059(3) Li1 0.048(3) 0.051(3) 0.049(3) 0.008(2) 0.005(2) -0.004(2) Li2 0.040(3) 0.037(3) 0.043(3) 0.005(2) 0.003(2) 0.001(2) Li3 0.050(3) 0.047(3) 0.032(2) 0.000(2) 0.009(2) 0.000(2) O1 0.0354(10) 0.0381(11) 0.0330(10) 0.0017(8) 0.0007(8) 0.0016(8) O2 0.0336(10) 0.0312(10) 0.0409(10) 0.0073(8) 0.0087(8) 0.0009(8) O3 0.0231(9) 0.0309(9) 0.0345(10) 0.0019(8) 0.0046(7) -0.0010(7) O4 0.0408(12) 0.0619(15) 0.0576(14) -0.0083(12) 0.0069(10) -0.0128(10) O5 0.0591(14) 0.0436(12) 0.0362(11) 0.0097(9) 0.0046(10) -0.0009(10) O6 0.0533(14) 0.0408(12) 0.0746(16) 0.0060(11) 0.0026(12) -0.0159(10) O7 0.0375(11) 0.0377(11) 0.0416(11) 0.0037(9) 0.0004(9) 0.0044(9) O8 0.0470(12) 0.0489(12) 0.0316(10) -0.0006(9) 0.0024(9) -0.0033(10) O9 0.0414(12) 0.0499(12) 0.0432(12) -0.0010(10) 0.0186(9) 0.0020(9) C1 0.064(2) 0.073(2) 0.060(2) 0.0169(19) 0.0219(18) -0.0106(19) C2 0.0379(17) 0.0509(19) 0.064(2) 0.0014(16) 0.0111(15) 0.0007(14) C3 0.054(2) 0.060(2) 0.0476(18) -0.0047(16) 0.0162(16) 0.0022(16) C4 0.075(3) 0.048(2) 0.084(3) -0.0021(19) 0.027(2) -0.0007(18) C5 0.071(2) 0.059(2) 0.0473(19) -0.0021(16) 0.0167(17) 0.0063(18) C6 0.0406(18) 0.069(2) 0.054(2) 0.0088(17) 0.0092(15) 0.0098(16) C7 0.074(2) 0.0441(18) 0.058(2) -0.0011(16) 0.0256(18) 0.0104(17) C8 0.0314(17) 0.081(3) 0.062(2) 0.0121(19) 0.0061(15) 0.0030(16) C9 0.0527(19) 0.0405(17) 0.0477(18) 0.0099(14) 0.0070(15) 0.0020(14) C11 0.066(2) 0.076(3) 0.060(2) -0.0047(19) 0.0410(19) 0.0024(19) C20 0.0325(15) 0.0290(14) 0.0447(16) 0.0012(12) 0.0098(13) 0.0021(11) C21 0.0314(16) 0.0417(17) 0.074(2) 0.0017(16) 0.0155(15) 0.0007(13) C22 0.0272(15) 0.0392(17) 0.081(2) -0.0029(16) -0.0030(16) -0.0033(13) C24 0.0411(17) 0.0347(16) 0.0560(19) -0.0044(14) -0.0103(15) -0.0014(13) C25 0.0364(16) 0.0271(14) 0.0443(16) -0.0007(12) 0.0021(13) 0.0021(11) C27 0.0260(13) 0.0228(12) 0.0410(15) 0.0027(11) 0.0042(11) 0.0050(10) C30 0.085(3) 0.068(3) 0.152(5) 0.019(3) -0.015(3) -0.042(3) C31 0.106(3) 0.051(2) 0.0436(19) 0.0096(16) 0.014(2) -0.014(2) C32 0.060(2) 0.111(4) 0.074(3) -0.027(2) 0.014(2) -0.042(2) C33 0.082(3) 0.082(3) 0.0361(18) -0.0080(17) 0.0033(18) 0.002(2) C34 0.0378(16) 0.0428(16) 0.0317(14) -0.0047(13) -0.0007(12) 0.0077(13) C35 0.073(3) 0.068(2) 0.0373(17) 0.0060(16) -0.0003(17) 0.025(2) C36 0.055(2) 0.092(3) 0.045(2) -0.004(2) -0.0116(17) 0.028(2) C37 0.0408(19) 0.093(3) 0.0442(19) -0.021(2) -0.0017(15) 0.0115(18) C38 0.0394(17) 0.057(2) 0.0399(16) -0.0135(15) 0.0043(13) 0.0040(14) C39 0.0485(19) 0.0502(18) 0.0322(15) -0.0033(14) -0.0007(13) 0.0109(15) C41 0.0383(18) 0.058(2) 0.064(2) 0.0171(17) -0.0044(15) 0.0052(15) C42 0.084(3) 0.0311(17) 0.071(2) 0.0062(16) 0.005(2) -0.0013(17) C44 0.057(2) 0.0464(19) 0.0510(19) 0.0071(15) 0.0025(16) 0.0171(16) C45 0.090(3) 0.0343(18) 0.069(2) 0.0078(17) 0.008(2) 0.0229(18) C46 0.0475(18) 0.0336(15) 0.0352(15) 0.0047(12) 0.0088(13) 0.0063(13) C47 0.057(2) 0.0368(17) 0.0474(18) 0.0040(14) 0.0117(15) -0.0028(14) C48 0.0457(17) 0.0304(14) 0.0361(15) 0.0077(12) 0.0115(13) 0.0040(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Al1 O1 1.899(2) . ? Al1 C4 1.981(4) . ? Al1 C5 1.978(3) . ? Al1 C6 1.985(3) . ? Al1 Li3 3.013(5) . ? Al1 Li1 3.241(6) . ? Al2 O2 1.888(2) . ? Al2 C1 1.971(3) . ? Al2 C3 1.977(3) . ? Al2 C2 1.988(3) . ? Al2 Li1 2.952(6) . ? Al2 Li2 3.004(5) . ? Al3 O3 1.9208(19) . ? Al3 C8 1.973(3) . ? Al3 C9 1.976(3) . ? Al3 C7 1.982(3) . ? Al3 Li3 3.121(5) . ? Li1 O4 2.053(6) . ? Li1 O1 2.090(6) . ? Li1 O2 2.082(6) . ? Li1 O6 2.098(6) . ? Li1 C48 2.677(6) . ? Li1 C34 2.760(6) . ? Li1 C47 2.758(6) . ? Li2 O2 2.014(5) . ? Li2 O3 2.047(5) . ? Li2 O7 2.078(5) . ? Li2 O8 2.146(5) . ? Li2 C27 2.682(6) . ? Li2 Li3 3.384(7) . ? Li3 O3 2.005(5) . ? Li3 O5 2.023(5) . ? Li3 O1 2.070(5) . ? Li3 O9 2.073(6) . ? Li3 C27 2.769(6) . ? O1 C34 1.380(3) . ? O2 C48 1.365(3) . ? O3 C27 1.376(3) . ? O4 C38 1.378(4) . ? O4 C32 1.438(4) . ? O5 C39 1.381(4) . ? O5 C31 1.437(4) . ? O6 C47 1.387(4) . ? O6 C30 1.433(4) . ? O7 C46 1.383(3) . ? O7 C41 1.439(4) . ? O8 C25 1.380(4) . ? O8 C33 1.426(4) . ? O9 C20 1.384(3) . ? O9 C11 1.452(4) . ? C20 C27 1.383(4) . ? C20 C21 1.387(4) . ? C21 C22 1.376(5) . ? C22 C24 1.380(5) . ? C24 C25 1.381(4) . ? C25 C27 1.392(4) . ? C34 C39 1.374(4) . ? C34 C38 1.389(4) . ? C35 C36 1.372(6) . ? C35 C39 1.394(4) . ? C36 C37 1.377(6) . ? C37 C38 1.393(5) . ? C42 C45 1.370(5) . ? C42 C47 1.376(5) . ? C44 C45 1.369(5) . ? C44 C46 1.387(4) . ? C46 C48 1.390(4) . ? C47 C48 1.390(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 O1 Al1 C4 107.37(14) . . ? O1 Al1 C5 108.15(13) . . ? C4 Al1 C5 112.42(17) . . ? O1 Al1 C6 99.46(12) . . ? C4 Al1 C6 115.65(17) . . ? C5 Al1 C6 112.59(16) . . ? O1 Al1 Li3 42.78(12) . . ? C4 Al1 Li3 146.46(15) . . ? C5 Al1 Li3 94.83(14) . . ? C6 Al1 Li3 67.16(15) . . ? O1 Al1 Li1 37.68(11) . . ? C4 Al1 Li1 74.98(15) . . ? C5 Al1 Li1 139.98(15) . . ? C6 Al1 Li1 96.83(14) . . ? Li3 Al1 Li1 71.54(14) . . ? O2 Al2 C1 112.72(14) . . ? O2 Al2 C3 100.34(12) . . ? C1 Al2 C3 110.95(16) . . ? O2 Al2 C2 103.38(12) . . ? C1 Al2 C2 112.55(16) . . ? C3 Al2 C2 116.05(15) . . ? O2 Al2 Li1 44.55(12) . . ? C1 Al2 Li1 118.71(16) . . ? C3 Al2 Li1 127.06(15) . . ? C2 Al2 Li1 60.05(15) . . ? O2 Al2 Li2 41.22(11) . . ? C1 Al2 Li2 126.30(15) . . ? C3 Al2 Li2 59.13(14) . . ? C2 Al2 Li2 118.66(14) . . ? Li1 Al2 Li2 76.83(14) . . ? O3 Al3 C8 100.02(13) . . ? O3 Al3 C9 107.65(11) . . ? C8 Al3 C9 115.44(15) . . ? O3 Al3 C7 111.47(12) . . ? C8 Al3 C7 113.38(16) . . ? C9 Al3 C7 108.53(15) . . ? O3 Al3 Li3 38.28(10) . . ? C8 Al3 Li3 79.60(15) . . ? C9 Al3 Li3 87.88(14) . . ? C7 Al3 Li3 149.73(14) . . ? O4 Li1 O1 79.9(2) . . ? O4 Li1 O2 170.4(3) . . ? O1 Li1 O2 104.4(2) . . ? O4 Li1 O6 104.2(3) . . ? O1 Li1 O6 140.9(3) . . ? O2 Li1 O6 77.9(2) . . ? O4 Li1 C48 157.1(3) . . ? O1 Li1 C48 106.9(2) . . ? O2 Li1 C48 30.15(11) . . ? O6 Li1 C48 56.48(15) . . ? O4 Li1 C34 55.49(15) . . ? O1 Li1 C34 29.09(11) . . ? O2 Li1 C34 125.8(2) . . ? O6 Li1 C34 151.2(3) . . ? C48 Li1 C34 135.7(2) . . ? O4 Li1 C47 128.2(3) . . ? O1 Li1 C47 120.4(2) . . ? O2 Li1 C47 57.18(15) . . ? O6 Li1 C47 29.37(11) . . ? C48 Li1 C47 29.58(11) . . ? C34 Li1 C47 146.4(2) . . ? O4 Li1 Al2 131.5(3) . . ? O1 Li1 Al2 130.9(2) . . ? O2 Li1 Al2 39.51(11) . . ? O6 Li1 Al2 75.35(17) . . ? C48 Li1 Al2 60.29(13) . . ? C34 Li1 Al2 133.0(2) . . ? C47 Li1 Al2 73.37(15) . . ? O4 Li1 Al1 84.39(19) . . ? O1 Li1 Al1 33.75(11) . . ? O2 Li1 Al1 104.0(2) . . ? O6 Li1 Al1 107.2(2) . . ? C48 Li1 Al1 89.80(17) . . ? C34 Li1 Al1 55.16(12) . . ? C47 Li1 Al1 91.22(17) . . ? Al2 Li1 Al1 143.16(19) . . ? O2 Li2 O3 116.3(2) . . ? O2 Li2 O7 80.91(19) . . ? O3 Li2 O7 118.5(3) . . ? O2 Li2 O8 165.6(3) . . ? O3 Li2 O8 78.12(18) . . ? O7 Li2 O8 93.0(2) . . ? O2 Li2 C27 137.2(2) . . ? O3 Li2 C27 30.22(10) . . ? O7 Li2 C27 96.5(2) . . ? O8 Li2 C27 56.16(14) . . ? O2 Li2 Al2 38.15(10) . . ? O3 Li2 Al2 125.4(2) . . ? O7 Li2 Al2 104.54(19) . . ? O8 Li2 Al2 133.6(2) . . ? C27 Li2 Al2 155.40(19) . . ? O2 Li2 Li3 85.93(18) . . ? O3 Li2 Li3 32.98(13) . . ? O7 Li2 Li3 103.1(2) . . ? O8 Li2 Li3 108.2(2) . . ? C27 Li2 Li3 52.80(14) . . ? Al2 Li2 Li3 108.89(17) . . ? O3 Li3 O5 130.8(3) . . ? O3 Li3 O1 120.7(3) . . ? O5 Li3 O1 80.53(19) . . ? O3 Li3 O9 81.6(2) . . ? O5 Li3 O9 96.8(2) . . ? O1 Li3 O9 152.6(3) . . ? O3 Li3 C27 28.12(10) . . ? O5 Li3 C27 134.4(2) . . ? O1 Li3 C27 141.4(2) . . ? O9 Li3 C27 55.20(14) . . ? O3 Li3 Al1 136.6(2) . . ? O5 Li3 Al1 88.82(17) . . ? O1 Li3 Al1 38.56(10) . . ? O9 Li3 Al1 114.5(2) . . ? C27 Li3 Al1 133.63(19) . . ? O3 Li3 Al3 36.41(10) . . ? O5 Li3 Al3 94.78(19) . . ? O1 Li3 Al3 117.6(2) . . ? O9 Li3 Al3 89.75(17) . . ? C27 Li3 Al3 55.08(10) . . ? Al1 Li3 Al3 154.90(19) . . ? O3 Li3 Li2 33.77(12) . . ? O5 Li3 Li2 149.0(2) . . ? O1 Li3 Li2 91.39(19) . . ? O9 Li3 Li2 103.5(2) . . ? C27 Li3 Li2 50.47(12) . . ? Al1 Li3 Li2 103.42(16) . . ? Al3 Li3 Li2 62.49(12) . . ? C34 O1 Al1 117.12(16) . . ? C34 O1 Li3 106.7(2) . . ? Al1 O1 Li3 98.66(17) . . ? C34 O1 Li1 103.5(2) . . ? Al1 O1 Li1 108.57(18) . . ? Li3 O1 Li1 123.3(2) . . ? C48 O2 Al2 120.58(16) . . ? C48 O2 Li2 111.6(2) . . ? Al2 O2 Li2 100.62(17) . . ? C48 O2 Li1 99.8(2) . . ? Al2 O2 Li1 95.94(18) . . ? Li2 O2 Li1 129.2(2) . . ? C27 O3 Al3 111.43(14) . . ? C27 O3 Li3 108.5(2) . . ? Al3 O3 Li3 105.32(17) . . ? C27 O3 Li2 101.31(19) . . ? Al3 O3 Li2 116.89(16) . . ? Li3 O3 Li2 113.2(2) . . ? C38 O4 C32 117.7(3) . . ? C38 O4 Li1 107.6(2) . . ? C32 O4 Li1 131.2(3) . . ? C39 O5 C31 118.1(3) . . ? C39 O5 Li3 111.0(2) . . ? C31 O5 Li3 130.5(3) . . ? C47 O6 C30 116.2(3) . . ? C47 O6 Li1 102.7(2) . . ? C30 O6 Li1 138.3(3) . . ? C46 O7 C41 115.9(2) . . ? C46 O7 Li2 112.5(2) . . ? C41 O7 Li2 130.6(2) . . ? C25 O8 C33 117.5(3) . . ? C25 O8 Li2 103.5(2) . . ? C33 O8 Li2 135.4(3) . . ? C20 O9 C11 116.0(2) . . ? C20 O9 Li3 110.0(2) . . ? C11 O9 Li3 128.9(2) . . ? O9 C20 C27 114.5(2) . . ? O9 C20 C21 124.9(3) . . ? C27 C20 C21 120.6(3) . . ? C22 C21 C20 119.0(3) . . ? C24 C22 C21 121.5(3) . . ? C22 C24 C25 119.0(3) . . ? O8 C25 C24 125.6(3) . . ? O8 C25 C27 113.6(2) . . ? C24 C25 C27 120.6(3) . . ? O3 C27 C20 120.8(2) . . ? O3 C27 C25 120.1(2) . . ? C20 C27 C25 119.0(2) . . ? O3 C27 Li2 48.47(15) . . ? C20 C27 Li2 145.3(2) . . ? C25 C27 Li2 80.4(2) . . ? O3 C27 Li3 43.35(15) . . ? C20 C27 Li3 79.42(19) . . ? C25 C27 Li3 156.9(2) . . ? Li2 C27 Li3 76.73(16) . . ? C39 C34 O1 120.3(3) . . ? C39 C34 C38 119.0(3) . . ? O1 C34 C38 120.6(3) . . ? C39 C34 Li1 153.4(2) . . ? O1 C34 Li1 47.42(17) . . ? C38 C34 Li1 77.1(2) . . ? C36 C35 C39 118.6(4) . . ? C35 C36 C37 121.9(3) . . ? C36 C37 C38 118.7(3) . . ? C34 C38 C37 120.7(3) . . ? C34 C38 O4 114.4(3) . . ? C37 C38 O4 124.9(3) . . ? O5 C39 C34 114.6(2) . . ? O5 C39 C35 124.2(3) . . ? C34 C39 C35 121.2(3) . . ? C45 C42 C47 118.8(3) . . ? C45 C44 C46 118.9(3) . . ? C42 C45 C44 122.0(3) . . ? O7 C46 C44 125.4(3) . . ? O7 C46 C48 113.9(2) . . ? C44 C46 C48 120.6(3) . . ? C42 C47 C48 121.2(3) . . ? C42 C47 O6 125.7(3) . . ? C48 C47 O6 113.1(3) . . ? C42 C47 Li1 151.7(3) . . ? C48 C47 Li1 72.0(2) . . ? O6 C47 Li1 47.91(17) . . ? O2 C48 C47 120.5(3) . . ? O2 C48 C46 121.0(2) . . ? C47 C48 C46 118.5(3) . . ? O2 C48 Li1 50.03(17) . . ? C47 C48 Li1 78.4(2) . . ? C46 C48 Li1 147.1(2) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.91 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.322 _refine_diff_density_min -0.308 _refine_diff_density_rms 0.057 #====== END data_3.C7H8 _database_code_depnum_ccdc_archive 'CCDC 835938' #TrackingRef '- 1_2C7H8_3C7H8.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H48 Al2 Li2 O12. C7 H8' _chemical_formula_sum 'C43 H56 Al2 Li2 O12' _chemical_formula_weight 832.72 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P n c a' _symmetry_space_group_name_Hall '-P 2a 2n' _symmetry_Int_Tables_number 60 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z' 'x+1/2, -y+1/2, -z+1/2' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z' '-x-1/2, y-1/2, z-1/2' 'x, -y-1/2, z-1/2' _cell_length_a 13.6968(12) _cell_length_b 13.9464(18) _cell_length_c 24.2111(19) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4624.8(8) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 139 _cell_measurement_theta_min 3.67 _cell_measurement_theta_max 19.456 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.41 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.34 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.196 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1768 _exptl_absorpt_coefficient_mu 0.120 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; R.H. Blessing, Acta Cryst. (1995), A51, 33-38 ; _exptl_absorpt_correction_T_min 0.947 _exptl_absorpt_correction_T_max 1.105 _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 68740 _diffrn_reflns_av_R_equivalents 0.0860 _diffrn_reflns_av_sigmaI/netI 0.0471 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 3.27 _diffrn_reflns_theta_max 27.50 _reflns_number_total 5314 _reflns_number_gt 3559 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)' _computing_data_reduction 'EvalCCD (Duisenberg & Schreurs 1990-2000)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.0571P)^2^+3.4765P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0005(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 5314 _refine_ls_number_parameters 281 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0957 _refine_ls_R_factor_gt 0.0559 _refine_ls_wR_factor_ref 0.1462 _refine_ls_wR_factor_gt 0.1262 _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_restrained_S_all 1.018 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C2D C 0.9723(6) 0.4543(4) 0.0397(2) 0.1093(17) Uani 1 1 d . . . C4D C 1.1304(8) 0.4129(8) -0.0073(6) 0.193(4) Uani 1 1 d . . . C3D C 1.0479(9) 0.4679(7) 0.0000(6) 0.100(3) Uani 0.50 1 d P . . C1D C 0.8953(11) 0.5111(14) 0.0458(6) 0.148(5) Uani 0.50 1 d P . . C5D C 1.0518(17) 0.4011(8) 0.0316(8) 0.176(9) Uani 0.50 1 d P . . Al1 Al 0.77928(5) 0.17292(4) 0.15238(3) 0.02797(18) Uani 1 1 d . . . Li1 Li 0.8562(3) -0.0024(3) 0.20719(15) 0.0353(9) Uani 1 1 d . . . O1 O 0.87291(11) 0.08318(11) 0.14596(6) 0.0357(4) Uani 1 1 d . . . O2 O 0.73983(10) 0.10935(10) 0.21571(5) 0.0268(3) Uani 1 1 d . . . O3 O 0.89390(14) 0.19168(14) 0.05540(7) 0.0537(5) Uani 1 1 d . . . O4 O 0.62067(13) 0.25175(13) 0.24150(7) 0.0458(4) Uani 1 1 d . . . O5 O 1.00189(11) -0.03957(11) 0.17844(6) 0.0362(4) Uani 1 1 d . . . O6 O 0.87049(11) 0.04043(11) 0.28702(6) 0.0351(4) Uani 1 1 d . . . C1 C 0.67299(18) 0.1635(2) 0.09906(10) 0.0477(6) Uani 1 1 d . . . H1A H 0.6267 0.2139 0.1056 0.072 Uiso 1 1 calc R . . H1B H 0.6412 0.1025 0.1030 0.072 Uiso 1 1 calc R . . H1C H 0.6987 0.1694 0.0623 0.072 Uiso 1 1 calc R . . C2 C 0.8339(2) 0.29917(19) 0.17009(12) 0.0536(7) Uani 1 1 d . . . H2A H 0.7819 0.3451 0.1731 0.080 Uiso 1 1 calc R . . H2B H 0.8779 0.3185 0.1413 0.080 Uiso 1 1 calc R . . H2C H 0.8685 0.2957 0.2045 0.080 Uiso 1 1 calc R . . C3 C 0.8818(3) 0.2226(2) 0.00073(11) 0.0643(9) Uani 1 1 d . . . H3A H 0.8280 0.2666 -0.0012 0.096 Uiso 1 1 calc R . . H3B H 0.8687 0.1683 -0.0225 0.096 Uiso 1 1 calc R . . H3C H 0.9403 0.2540 -0.0115 0.096 Uiso 1 1 calc R . . C4 C 0.5641(3) 0.3353(2) 0.25109(14) 0.0728(10) Uani 1 1 d . . . H4A H 0.5241 0.3480 0.2194 0.109 Uiso 1 1 calc R . . H4B H 0.6066 0.3888 0.2576 0.109 Uiso 1 1 calc R . . H4C H 0.5231 0.3255 0.2828 0.109 Uiso 1 1 calc R . . C5 C 1.0646(2) -0.1174(2) 0.19283(13) 0.0650(9) Uani 1 1 d . . . H5A H 1.0423 -0.1461 0.2266 0.097 Uiso 1 1 calc R . . H5B H 1.1300 -0.0940 0.1977 0.097 Uiso 1 1 calc R . . H5C H 1.0637 -0.1644 0.1639 0.097 Uiso 1 1 calc R . . C6 C 0.9274(2) -0.0103(2) 0.32727(11) 0.0506(7) Uani 1 1 d . . . H6A H 0.9661 -0.0583 0.3091 0.076 Uiso 1 1 calc R . . H6B H 0.8847 -0.0405 0.3535 0.076 Uiso 1 1 calc R . . H6C H 0.9696 0.0338 0.3461 0.076 Uiso 1 1 calc R . . C11 C 0.95360(15) 0.07493(16) 0.11459(9) 0.0306(5) Uani 1 1 d . . . C12 C 1.02464(15) 0.00935(16) 0.13037(9) 0.0316(5) Uani 1 1 d . . . C13 C 1.10880(17) -0.00277(18) 0.09942(10) 0.0416(6) Uani 1 1 d . . . H13 H 1.1566 -0.0461 0.1103 0.050 Uiso 1 1 calc R . . C14 C 1.12007(19) 0.0512(2) 0.05183(11) 0.0493(7) Uani 1 1 d . . . H14 H 1.1763 0.0436 0.0307 0.059 Uiso 1 1 calc R . . C15 C 1.05042(19) 0.1156(2) 0.03503(10) 0.0464(6) Uani 1 1 d . . . H15 H 1.0590 0.1506 0.0027 0.056 Uiso 1 1 calc R . . C16 C 0.96753(17) 0.12785(17) 0.06658(9) 0.0365(5) Uani 1 1 d . . . C21 C 0.74453(15) 0.14803(15) 0.26716(8) 0.0281(5) Uani 1 1 d . . . C22 C 0.80959(15) 0.11234(16) 0.30630(9) 0.0321(5) Uani 1 1 d . . . C23 C 0.81100(19) 0.14835(19) 0.35996(10) 0.0432(6) Uani 1 1 d . . . H23 H 0.8538 0.1234 0.3861 0.052 Uiso 1 1 calc R . . C24 C 0.7481(2) 0.2213(2) 0.37356(10) 0.0502(7) Uani 1 1 d . . . H24 H 0.7489 0.2456 0.4093 0.060 Uiso 1 1 calc R . . C25 C 0.68387(19) 0.25961(19) 0.33587(10) 0.0445(6) Uani 1 1 d . . . H25 H 0.6423 0.3094 0.3459 0.053 Uiso 1 1 calc R . . C26 C 0.68231(17) 0.22261(16) 0.28257(9) 0.0348(5) Uani 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 C2D 0.151(5) 0.098(4) 0.079(3) 0.001(3) -0.039(4) -0.038(4) C4D 0.165(8) 0.156(8) 0.259(12) -0.059(8) -0.036(8) 0.018(7) C3D 0.121(9) 0.063(6) 0.117(8) -0.021(6) -0.044(8) -0.014(5) C1D 0.118(10) 0.184(15) 0.141(12) -0.040(11) -0.059(9) -0.002(11) C5D 0.241(19) 0.059(7) 0.229(17) -0.016(9) -0.184(16) 0.007(9) Al1 0.0275(3) 0.0283(3) 0.0281(3) 0.0016(3) -0.0042(3) 0.0027(3) Li1 0.0278(18) 0.040(2) 0.039(2) 0.0034(17) -0.0005(15) -0.0004(16) O1 0.0303(8) 0.0412(9) 0.0356(8) 0.0095(7) 0.0087(6) 0.0096(7) O2 0.0267(7) 0.0297(8) 0.0241(7) -0.0037(6) -0.0004(6) 0.0022(6) O3 0.0545(12) 0.0688(13) 0.0377(10) 0.0187(9) 0.0064(8) 0.0195(10) O4 0.0452(10) 0.0465(10) 0.0457(10) -0.0101(8) -0.0045(8) 0.0203(8) O5 0.0299(8) 0.0384(9) 0.0403(9) 0.0078(7) 0.0007(7) 0.0062(7) O6 0.0290(8) 0.0392(9) 0.0372(9) 0.0075(7) -0.0082(6) 0.0010(7) C1 0.0420(14) 0.0618(17) 0.0394(14) 0.0127(12) -0.0120(11) -0.0038(13) C2 0.0696(19) 0.0416(14) 0.0497(16) -0.0010(12) -0.0039(14) -0.0118(14) C3 0.089(2) 0.0645(19) 0.0393(15) 0.0110(14) -0.0112(15) 0.0166(17) C4 0.079(2) 0.060(2) 0.079(2) -0.0136(17) -0.0015(18) 0.0408(18) C5 0.0501(17) 0.0654(19) 0.079(2) 0.0292(17) 0.0058(15) 0.0242(15) C6 0.0442(15) 0.0526(16) 0.0549(16) 0.0179(13) -0.0199(12) -0.0014(12) C11 0.0265(11) 0.0362(12) 0.0293(11) -0.0019(9) 0.0039(9) -0.0008(9) C12 0.0265(11) 0.0355(12) 0.0329(11) -0.0019(10) 0.0000(9) -0.0018(9) C13 0.0286(12) 0.0447(14) 0.0515(15) -0.0060(12) 0.0033(10) 0.0049(11) C14 0.0372(14) 0.0646(18) 0.0461(15) -0.0020(13) 0.0187(11) 0.0008(13) C15 0.0474(15) 0.0550(16) 0.0369(13) 0.0037(12) 0.0128(11) -0.0033(13) C16 0.0378(13) 0.0398(13) 0.0318(12) 0.0026(10) 0.0029(10) 0.0024(11) C21 0.0281(11) 0.0293(11) 0.0271(11) -0.0038(9) 0.0011(8) -0.0051(9) C22 0.0284(11) 0.0349(12) 0.0329(11) 0.0000(10) -0.0033(9) -0.0066(9) C23 0.0448(14) 0.0536(16) 0.0311(12) -0.0010(11) -0.0108(10) -0.0115(12) C24 0.0603(17) 0.0573(17) 0.0330(13) -0.0134(12) -0.0006(12) -0.0135(14) C25 0.0503(15) 0.0426(14) 0.0406(14) -0.0149(11) 0.0073(12) -0.0027(12) C26 0.0342(12) 0.0351(12) 0.0351(12) -0.0064(10) 0.0015(10) -0.0006(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C2D C5D 1.33(2) . ? C2D C1D 1.328(16) . ? C2D C3D 1.425(15) . ? C2D C3D 1.476(14) 5_765 ? C4D C3D 1.378(15) . ? C4D C5D 1.44(3) . ? C4D C1D 1.455(19) 5_765 ? C3D C5D 1.206(19) . ? C3D C1D 1.387(19) 5_765 ? C3D C2D 1.476(14) 5_765 ? C3D C3D 1.59(2) 5_765 ? C1D C3D 1.387(19) 5_765 ? C1D C4D 1.455(19) 5_765 ? Al1 O1 1.7987(16) . ? Al1 O2 1.8519(15) . ? Al1 C1 1.950(2) . ? Al1 C2 1.960(3) . ? Al1 Li1 2.974(4) . ? Li1 O1 1.917(4) . ? Li1 O2 1.999(4) 2_655 ? Li1 O6 2.032(4) . ? Li1 O5 2.177(4) . ? Li1 O2 2.238(4) . ? Li1 Li1 2.909(7) 2_655 ? O1 C11 1.346(2) . ? O2 C21 1.359(2) . ? O2 Li1 1.999(4) 2_655 ? O3 C16 1.372(3) . ? O3 C3 1.402(3) . ? O4 C26 1.366(3) . ? O4 C4 1.418(3) . ? O5 C12 1.385(3) . ? O5 C5 1.427(3) . ? O6 C22 1.385(3) . ? O6 C6 1.435(3) . ? C11 C12 1.389(3) . ? C11 C16 1.390(3) . ? C12 C13 1.385(3) . ? C13 C14 1.385(3) . ? C14 C15 1.372(4) . ? C15 C16 1.379(3) . ? C21 C22 1.393(3) . ? C21 C26 1.395(3) . ? C22 C23 1.393(3) . ? C23 C24 1.374(4) . ? C24 C25 1.375(4) . ? C25 C26 1.390(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 C5D C2D C1D 176.7(14) . . ? C5D C2D C3D 51.8(10) . . ? C1D C2D C3D 125.0(10) . . ? C5D C2D C3D 117.8(13) . 5_765 ? C1D C2D C3D 59.0(8) . 5_765 ? C3D C2D C3D 66.4(9) . 5_765 ? C3D C4D C5D 50.6(8) . . ? C3D C4D C1D 58.6(9) . 5_765 ? C5D C4D C1D 108.7(11) . 5_765 ? C5D C3D C1D 130.2(18) . 5_765 ? C5D C3D C4D 67.4(13) . . ? C1D C3D C4D 63.5(11) 5_765 . ? C5D C3D C2D 60.2(15) . . ? C1D C3D C2D 167.3(12) 5_765 . ? C4D C3D C2D 127.5(13) . . ? C5D C3D C2D 171.5(15) . 5_765 ? C1D C3D C2D 55.2(10) 5_765 5_765 ? C4D C3D C2D 118.6(15) . 5_765 ? C2D C3D C2D 113.6(9) . 5_765 ? C5D C3D C3D 118(2) . 5_765 ? C1D C3D C3D 110.1(16) 5_765 5_765 ? C4D C3D C3D 172.6(18) . 5_765 ? C2D C3D C3D 58.4(10) . 5_765 ? C2D C3D C3D 55.3(8) 5_765 5_765 ? C2D C1D C3D 65.8(11) . 5_765 ? C2D C1D C4D 123.7(15) . 5_765 ? C3D C1D C4D 57.9(9) 5_765 5_765 ? C2D C5D C3D 68.1(10) . . ? C2D C5D C4D 130.1(14) . . ? C3D C5D C4D 62.0(15) . . ? O1 Al1 O2 86.93(7) . . ? O1 Al1 C1 115.35(10) . . ? O2 Al1 C1 107.33(9) . . ? O1 Al1 C2 111.84(11) . . ? O2 Al1 C2 111.11(10) . . ? C1 Al1 C2 119.35(12) . . ? O1 Al1 Li1 38.20(8) . . ? O2 Al1 Li1 48.73(8) . . ? C1 Al1 Li1 120.27(11) . . ? C2 Al1 Li1 120.38(12) . . ? O1 Li1 O2 128.5(2) . 2_655 ? O1 Li1 O6 122.8(2) . . ? O2 Li1 O6 100.64(17) 2_655 . ? O1 Li1 O5 77.95(14) . . ? O2 Li1 O5 117.3(2) 2_655 . ? O6 Li1 O5 106.59(17) . . ? O1 Li1 O2 73.93(14) . . ? O2 Li1 O2 92.40(15) 2_655 . ? O6 Li1 O2 77.09(14) . . ? O5 Li1 O2 148.0(2) . . ? O1 Li1 Li1 96.05(16) . 2_655 ? O2 Li1 Li1 50.18(12) 2_655 2_655 ? O6 Li1 Li1 95.15(12) . 2_655 ? O5 Li1 Li1 157.26(17) . 2_655 ? O2 Li1 Li1 43.31(11) . 2_655 ? O1 Li1 Al1 35.47(8) . . ? O2 Li1 Al1 115.25(15) 2_655 . ? O6 Li1 Al1 102.53(16) . . ? O5 Li1 Al1 112.20(15) . . ? O2 Li1 Al1 38.45(7) . . ? Li1 Li1 Al1 68.12(13) 2_655 . ? C11 O1 Al1 133.91(14) . . ? C11 O1 Li1 118.79(17) . . ? Al1 O1 Li1 106.32(13) . . ? C21 O2 Al1 123.71(13) . . ? C21 O2 Li1 114.96(16) . 2_655 ? Al1 O2 Li1 117.63(12) . 2_655 ? C21 O2 Li1 109.09(15) . . ? Al1 O2 Li1 92.82(11) . . ? Li1 O2 Li1 86.51(15) 2_655 . ? C16 O3 C3 118.2(2) . . ? C26 O4 C4 117.6(2) . . ? C12 O5 C5 116.39(19) . . ? C12 O5 Li1 110.96(16) . . ? C5 O5 Li1 130.92(18) . . ? C22 O6 C6 117.10(18) . . ? C22 O6 Li1 118.36(16) . . ? C6 O6 Li1 123.60(19) . . ? O1 C11 C12 118.44(19) . . ? O1 C11 C16 122.6(2) . . ? C12 C11 C16 118.9(2) . . ? O5 C12 C13 125.6(2) . . ? O5 C12 C11 113.45(18) . . ? C13 C12 C11 121.0(2) . . ? C14 C13 C12 118.5(2) . . ? C15 C14 C13 121.7(2) . . ? C14 C15 C16 119.3(2) . . ? O3 C16 C15 125.2(2) . . ? O3 C16 C11 114.11(19) . . ? C15 C16 C11 120.7(2) . . ? O2 C21 C22 120.81(19) . . ? O2 C21 C26 120.80(19) . . ? C22 C21 C26 118.37(19) . . ? C21 C22 O6 114.49(18) . . ? C21 C22 C23 121.0(2) . . ? O6 C22 C23 124.5(2) . . ? C24 C23 C22 118.8(2) . . ? C23 C24 C25 122.0(2) . . ? C24 C25 C26 118.8(2) . . ? O4 C26 C21 113.86(19) . . ? O4 C26 C25 125.1(2) . . ? C21 C26 C25 121.0(2) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.324 _refine_diff_density_min -0.266 _refine_diff_density_rms 0.050