# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Peter Junk' _publ_contact_author_email PETER.JUNK@SCI.MONASH.EDU.AU _publ_section_title ; Metal Based Synthetic Routes to Heavy Alkaline Earth Aryloxo Complexes Involving Ligands of Moderate Steric Bulk ; loop_ _publ_author_name 'Peter Junk' 'Glen Deacon' 'Marites A. Guino-o' 'Graeme J. Moxey' 'Karin Ruhlandt-Senge' data_c:\monop _database_code_depnum_ccdc_archive 'CCDC 716846' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C52 H84 Ca2 O12' _chemical_formula_sum 'C52 H84 Ca2 O12' _chemical_formula_weight 981.35 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ca Ca 0.2262 0.3064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 15.8650(3) _cell_length_b 15.5945(3) _cell_length_c 22.0409(4) _cell_angle_alpha 90.00 _cell_angle_beta 102.1970(10) _cell_angle_gamma 90.00 _cell_volume 5329.97(17) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.223 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2128 _exptl_absorpt_coefficient_mu 0.272 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.9604 _exptl_absorpt_correction_T_max 0.9733 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker X8 Apex II CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 95064 _diffrn_reflns_av_R_equivalents 0.0512 _diffrn_reflns_av_sigmaI/netI 0.0263 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.31 _diffrn_reflns_theta_max 25.00 _reflns_number_total 9377 _reflns_number_gt 9066 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART (Bruker)' _computing_cell_refinement 'Bruker SMART (Bruker)' _computing_data_reduction 'Bruker SAINT (Bruker)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 1999)' _computing_publication_material 'CIFTAB (Sheldrick, 1997)' _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^)+(0.0000P)^2^+21.4036P] 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 ? _refine_ls_extinction_coef ? _refine_ls_number_reflns 9377 _refine_ls_number_parameters 615 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0957 _refine_ls_R_factor_gt 0.0934 _refine_ls_wR_factor_ref 0.1612 _refine_ls_wR_factor_gt 0.1603 _refine_ls_goodness_of_fit_ref 1.365 _refine_ls_restrained_S_all 1.365 _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 Ca1 Ca 0.13339(5) 0.75618(5) 0.23631(4) 0.01086(18) Uani 1 1 d . . . O1 O 0.06739(18) 0.8284(2) 0.29808(13) 0.0188(7) Uani 1 1 d . . . C1 C 0.0154(3) 0.8458(3) 0.33592(19) 0.0156(9) Uani 1 1 d . . . Ca2 Ca 0.36866(5) 0.78532(5) 0.25777(4) 0.01026(18) Uani 1 1 d . . . O2 O 0.23498(17) 0.84315(18) 0.20613(12) 0.0139(6) Uani 1 1 d . . . C2 C 0.0465(3) 0.8815(3) 0.3957(2) 0.0198(10) Uani 1 1 d . . . O3 O 0.26676(18) 0.69734(17) 0.28717(13) 0.0140(6) Uani 1 1 d . . . C3 C -0.0100(3) 0.8936(3) 0.4353(2) 0.0218(10) Uani 1 1 d . . . H1 H 0.0120 0.9163 0.4756 0.026 Uiso 1 1 calc R . . O4 O 0.43542(18) 0.71096(18) 0.19780(13) 0.0165(6) Uani 1 1 d . . . C4 C -0.0974(3) 0.8740(3) 0.4187(2) 0.0245(11) Uani 1 1 d . . . O5 O 0.0218(2) 0.8013(2) 0.14676(14) 0.0245(7) Uani 1 1 d . . . C5 C -0.1278(3) 0.8442(3) 0.3591(2) 0.0236(10) Uani 1 1 d . . . H2 H -0.1877 0.8328 0.3460 0.028 Uiso 1 1 calc R . . O6 O -0.0277(2) 0.8768(3) 0.01525(16) 0.0400(10) Uani 1 1 d . . . C6 C -0.0744(3) 0.8301(3) 0.3175(2) 0.0179(9) Uani 1 1 d . . . O7 O 0.04386(19) 0.63024(19) 0.25649(14) 0.0196(7) Uani 1 1 d . . . C7 C 0.1391(3) 0.9094(3) 0.4151(2) 0.0292(11) Uani 1 1 d . . . H3 H 0.1420 0.9722 0.4160 0.044 Uiso 1 1 calc R . . H4 H 0.1719 0.8874 0.3854 0.044 Uiso 1 1 calc R . . H5 H 0.1637 0.8867 0.4566 0.044 Uiso 1 1 calc R . . O8 O 0.1238(2) 0.63477(19) 0.16308(14) 0.0201(7) Uani 1 1 d . . . C8 C -0.1574(4) 0.8873(4) 0.4627(3) 0.0403(14) Uani 1 1 d . . . H6 H -0.2098 0.9165 0.4409 0.061 Uiso 1 1 calc R . . H7 H -0.1286 0.9224 0.4979 0.061 Uiso 1 1 calc R . . H8 H -0.1727 0.8315 0.4779 0.061 Uiso 1 1 calc R . . O9 O 0.47637(19) 0.73825(19) 0.35062(14) 0.0184(6) Uani 1 1 d . . . C9 C -0.1105(3) 0.8006(3) 0.2524(2) 0.0247(10) Uani 1 1 d . . . H9 H -0.1732 0.7939 0.2463 0.037 Uiso 1 1 calc R . . H10 H -0.0846 0.7455 0.2453 0.037 Uiso 1 1 calc R . . H11 H -0.0974 0.8432 0.2229 0.037 Uiso 1 1 calc R . . O10 O 0.5302(2) 0.6312(2) 0.47303(14) 0.0281(8) Uani 1 1 d . . . C10 C 0.2360(3) 0.9189(3) 0.17693(19) 0.0132(8) Uani 1 1 d . . . O11 O 0.38220(18) 0.90885(19) 0.32982(13) 0.0171(6) Uani 1 1 d . . . C11 C 0.2633(3) 0.9244(3) 0.11980(19) 0.0152(9) Uani 1 1 d . . . O12 O 0.45583(19) 0.90999(18) 0.23287(13) 0.0163(6) Uani 1 1 d . . . C12 C 0.2655(3) 1.0031(3) 0.0914(2) 0.0169(9) Uani 1 1 d . . . H12 H 0.2847 1.0055 0.0534 0.020 Uiso 1 1 calc R . . C13 C 0.2411(3) 1.0787(3) 0.1157(2) 0.0182(9) Uani 1 1 d . . . C14 C 0.2145(3) 1.0729(3) 0.1717(2) 0.0167(9) Uani 1 1 d . . . H13 H 0.1970 1.1237 0.1893 0.020 Uiso 1 1 calc R . . C15 C 0.2124(2) 0.9957(3) 0.20297(19) 0.0142(9) Uani 1 1 d . . . C16 C 0.2879(3) 0.8442(3) 0.0899(2) 0.0182(9) Uani 1 1 d . . . H14 H 0.2363 0.8095 0.0746 0.027 Uiso 1 1 calc R . . H15 H 0.3291 0.8111 0.1205 0.027 Uiso 1 1 calc R . . H16 H 0.3145 0.8596 0.0551 0.027 Uiso 1 1 calc R . . C17 C 0.2421(3) 1.1627(3) 0.0821(2) 0.0250(10) Uani 1 1 d . . . H17 H 0.2918 1.1641 0.0621 0.037 Uiso 1 1 calc R . . H18 H 0.2465 1.2100 0.1118 0.037 Uiso 1 1 calc R . . H19 H 0.1888 1.1685 0.0505 0.037 Uiso 1 1 calc R . . C18 C 0.1862(3) 0.9941(3) 0.26454(19) 0.0188(9) Uani 1 1 d . . . H20 H 0.2339 0.9719 0.2964 0.028 Uiso 1 1 calc R . . H21 H 0.1357 0.9569 0.2618 0.028 Uiso 1 1 calc R . . H22 H 0.1718 1.0523 0.2756 0.028 Uiso 1 1 calc R . . C19 C 0.2650(2) 0.6238(3) 0.31832(19) 0.0142(9) Uani 1 1 d . . . C20 C 0.2870(2) 0.5449(3) 0.2939(2) 0.0173(9) Uani 1 1 d . . . C21 C 0.2831(3) 0.4695(3) 0.3270(2) 0.0199(9) Uani 1 1 d . . . H23 H 0.2985 0.4170 0.3103 0.024 Uiso 1 1 calc R . . C22 C 0.2575(3) 0.4681(3) 0.3835(2) 0.0205(10) Uani 1 1 d . . . C23 C 0.2357(3) 0.5462(3) 0.40656(19) 0.0189(9) Uani 1 1 d . . . H24 H 0.2178 0.5471 0.4450 0.023 Uiso 1 1 calc R . . C24 C 0.2393(3) 0.6225(3) 0.3755(2) 0.0164(9) Uani 1 1 d . . . C25 C 0.3120(3) 0.5416(3) 0.2314(2) 0.0212(10) Uani 1 1 d . . . H25 H 0.3334 0.4842 0.2247 0.032 Uiso 1 1 calc R . . H26 H 0.3572 0.5840 0.2303 0.032 Uiso 1 1 calc R . . H27 H 0.2614 0.5545 0.1986 0.032 Uiso 1 1 calc R . . C26 C 0.2549(3) 0.3862(3) 0.4196(2) 0.0307(12) Uani 1 1 d . . . H28 H 0.2514 0.3370 0.3915 0.046 Uiso 1 1 calc R . . H29 H 0.2043 0.3867 0.4385 0.046 Uiso 1 1 calc R . . H30 H 0.3073 0.3817 0.4522 0.046 Uiso 1 1 calc R . . C27 C 0.2163(3) 0.7042(3) 0.4040(2) 0.0242(10) Uani 1 1 d . . . H31 H 0.1920 0.6908 0.4403 0.036 Uiso 1 1 calc R . . H33 H 0.1736 0.7358 0.3735 0.036 Uiso 1 1 calc R . . H32 H 0.2682 0.7394 0.4169 0.036 Uiso 1 1 calc R . . C28 C 0.4918(3) 0.6934(3) 0.16300(19) 0.0155(9) Uani 1 1 d . . . C29 C 0.4658(3) 0.6556(3) 0.1033(2) 0.0174(9) Uani 1 1 d . . . C30 C 0.5270(3) 0.6414(3) 0.0675(2) 0.0212(10) Uani 1 1 d . . . H34 H 0.5083 0.6174 0.0272 0.025 Uiso 1 1 calc R . . C31 C 0.6138(3) 0.6606(3) 0.0874(2) 0.0219(10) Uani 1 1 d . . . C32 C 0.6385(3) 0.6946(3) 0.1465(2) 0.0210(10) Uani 1 1 d . . . H35 H 0.6977 0.7075 0.1617 0.025 Uiso 1 1 calc R . . C33 C 0.5809(3) 0.7107(3) 0.1846(2) 0.0165(9) Uani 1 1 d . . . C34 C 0.3734(3) 0.6295(3) 0.0797(2) 0.0272(11) Uani 1 1 d . . . H36 H 0.3408 0.6780 0.0583 0.041 Uiso 1 1 calc R . . H37 H 0.3482 0.6119 0.1147 0.041 Uiso 1 1 calc R . . H38 H 0.3710 0.5814 0.0507 0.041 Uiso 1 1 calc R . . C35 C 0.6778(3) 0.6455(3) 0.0469(2) 0.0316(12) Uani 1 1 d . . . H40 H 0.6871 0.6990 0.0259 0.047 Uiso 1 1 calc R . . H39 H 0.6553 0.6016 0.0158 0.047 Uiso 1 1 calc R . . H41 H 0.7325 0.6259 0.0725 0.047 Uiso 1 1 calc R . . C36 C 0.6122(3) 0.7440(3) 0.2495(2) 0.0226(10) Uani 1 1 d . . . H42 H 0.6743 0.7548 0.2567 0.034 Uiso 1 1 calc R . . H43 H 0.6006 0.7013 0.2793 0.034 Uiso 1 1 calc R . . H44 H 0.5820 0.7974 0.2547 0.034 Uiso 1 1 calc R . . C37 C -0.0480(3) 0.7495(4) 0.1146(2) 0.0341(12) Uani 1 1 d . . . H45 H -0.1021 0.7818 0.1094 0.051 Uiso 1 1 calc R . . H46 H -0.0522 0.6973 0.1385 0.051 Uiso 1 1 calc R . . H47 H -0.0377 0.7339 0.0737 0.051 Uiso 1 1 calc R . . C38 C 0.0191(3) 0.8880(3) 0.1252(2) 0.0255(11) Uani 1 1 d . . . H48 H 0.0587 0.9233 0.1561 0.031 Uiso 1 1 calc R . . H49 H -0.0400 0.9109 0.1218 0.031 Uiso 1 1 calc R . . C39 C 0.0438(3) 0.8956(3) 0.0637(2) 0.0321(12) Uani 1 1 d . . . H50 H 0.0644 0.9545 0.0585 0.039 Uiso 1 1 calc R . . H51 H 0.0915 0.8553 0.0619 0.039 Uiso 1 1 calc R . . C40 C -0.0019(4) 0.8649(5) -0.0419(2) 0.0512(18) Uani 1 1 d . . . H52 H 0.0318 0.9146 -0.0502 0.077 Uiso 1 1 calc R . . H53 H -0.0531 0.8589 -0.0754 0.077 Uiso 1 1 calc R . . H54 H 0.0334 0.8130 -0.0397 0.077 Uiso 1 1 calc R . . C41 C 0.0195(3) 0.6195(3) 0.3150(2) 0.0220(10) Uani 1 1 d . . . H55 H -0.0347 0.5872 0.3089 0.033 Uiso 1 1 calc R . . H56 H 0.0117 0.6759 0.3326 0.033 Uiso 1 1 calc R . . H57 H 0.0648 0.5880 0.3434 0.033 Uiso 1 1 calc R . . C42 C 0.0631(3) 0.5490(3) 0.2324(2) 0.0212(10) Uani 1 1 d . . . H58 H 0.0168 0.5073 0.2345 0.025 Uiso 1 1 calc R . . H59 H 0.1181 0.5264 0.2570 0.025 Uiso 1 1 calc R . . C43 C 0.0701(3) 0.5623(3) 0.1664(2) 0.0221(10) Uani 1 1 d . . . H60 H 0.0951 0.5106 0.1509 0.027 Uiso 1 1 calc R . . H61 H 0.0121 0.5720 0.1401 0.027 Uiso 1 1 calc R . . C44 C 0.1449(4) 0.6427(3) 0.1041(2) 0.0331(12) Uani 1 1 d . . . H62 H 0.1712 0.5892 0.0938 0.050 Uiso 1 1 calc R . . H63 H 0.1858 0.6900 0.1049 0.050 Uiso 1 1 calc R . . H64 H 0.0925 0.6544 0.0727 0.050 Uiso 1 1 calc R . . C45 C 0.5438(3) 0.7868(3) 0.3889(2) 0.0278(11) Uani 1 1 d . . . H65 H 0.5353 0.7873 0.4316 0.042 Uiso 1 1 calc R . . H66 H 0.5427 0.8457 0.3733 0.042 Uiso 1 1 calc R . . H67 H 0.5997 0.7605 0.3880 0.042 Uiso 1 1 calc R . . C46 C 0.4831(3) 0.6480(3) 0.36315(19) 0.0198(10) Uani 1 1 d . . . H68 H 0.5432 0.6294 0.3650 0.024 Uiso 1 1 calc R . . H69 H 0.4456 0.6168 0.3286 0.024 Uiso 1 1 calc R . . C47 C 0.4576(3) 0.6245(3) 0.4232(2) 0.0211(10) Uani 1 1 d . . . H70 H 0.4114 0.6633 0.4304 0.025 Uiso 1 1 calc R . . H71 H 0.4352 0.5650 0.4206 0.025 Uiso 1 1 calc R . . C48 C 0.5051(3) 0.6224(4) 0.5308(2) 0.0341(12) Uani 1 1 d . . . H72 H 0.4667 0.6698 0.5361 0.051 Uiso 1 1 calc R . . H73 H 0.5564 0.6234 0.5646 0.051 Uiso 1 1 calc R . . H74 H 0.4747 0.5678 0.5316 0.051 Uiso 1 1 calc R . . C49 C 0.3655(3) 0.9058(3) 0.3908(2) 0.0284(11) Uani 1 1 d . . . H75 H 0.4202 0.9075 0.4213 0.043 Uiso 1 1 calc R . . H76 H 0.3347 0.8527 0.3959 0.043 Uiso 1 1 calc R . . H77 H 0.3301 0.9552 0.3970 0.043 Uiso 1 1 calc R . . C50 C 0.4328(3) 0.9833(3) 0.3223(2) 0.0185(9) Uani 1 1 d . . . H78 H 0.4920 0.9770 0.3475 0.022 Uiso 1 1 calc R . . H79 H 0.4066 1.0351 0.3365 0.022 Uiso 1 1 calc R . . C51 C 0.4357(3) 0.9920(3) 0.2551(2) 0.0181(9) Uani 1 1 d . . . H80 H 0.3792 1.0121 0.2312 0.022 Uiso 1 1 calc R . . H81 H 0.4801 1.0344 0.2501 0.022 Uiso 1 1 calc R . . C52 C 0.4835(3) 0.9185(3) 0.17502(19) 0.0183(9) Uani 1 1 d . . . H82 H 0.4394 0.9492 0.1451 0.027 Uiso 1 1 calc R . . H83 H 0.4921 0.8614 0.1587 0.027 Uiso 1 1 calc R . . H84 H 0.5378 0.9505 0.1819 0.027 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 Ca1 0.0098(4) 0.0120(4) 0.0110(4) -0.0016(3) 0.0026(3) -0.0007(3) O1 0.0151(15) 0.0245(17) 0.0178(15) -0.0040(13) 0.0058(12) -0.0001(13) C1 0.019(2) 0.013(2) 0.017(2) 0.0034(17) 0.0089(17) 0.0050(17) Ca2 0.0094(4) 0.0120(4) 0.0099(4) 0.0004(3) 0.0031(3) 0.0007(3) O2 0.0119(14) 0.0146(15) 0.0142(14) 0.0013(12) 0.0006(11) 0.0003(12) C2 0.025(2) 0.015(2) 0.019(2) 0.0019(18) 0.0040(18) 0.0116(19) O3 0.0156(15) 0.0101(14) 0.0170(14) 0.0034(12) 0.0047(12) -0.0002(12) C3 0.036(3) 0.013(2) 0.018(2) 0.0020(18) 0.008(2) 0.008(2) O4 0.0168(15) 0.0148(15) 0.0187(15) -0.0027(12) 0.0058(12) 0.0025(12) C4 0.036(3) 0.015(2) 0.030(3) 0.0067(19) 0.025(2) 0.009(2) O5 0.0219(17) 0.0265(18) 0.0206(16) -0.0003(14) -0.0053(13) 0.0029(14) C5 0.019(2) 0.014(2) 0.042(3) 0.008(2) 0.016(2) 0.0001(18) O6 0.0209(18) 0.077(3) 0.0213(18) 0.0048(18) 0.0016(14) -0.0009(19) C6 0.019(2) 0.011(2) 0.025(2) 0.0030(18) 0.0075(18) 0.0023(17) O7 0.0186(16) 0.0154(16) 0.0258(17) -0.0042(13) 0.0070(13) -0.0012(13) C7 0.026(3) 0.030(3) 0.029(3) -0.013(2) 0.001(2) 0.004(2) O8 0.0224(16) 0.0172(16) 0.0214(16) -0.0048(13) 0.0059(13) -0.0036(13) C8 0.053(4) 0.033(3) 0.045(3) 0.002(3) 0.033(3) 0.005(3) O9 0.0167(15) 0.0130(15) 0.0228(16) -0.0018(12) -0.0020(12) -0.0007(12) C9 0.016(2) 0.027(3) 0.031(3) -0.003(2) 0.0035(19) -0.0001(19) O10 0.0178(16) 0.048(2) 0.0182(16) 0.0096(15) 0.0020(13) 0.0025(15) C10 0.0090(19) 0.012(2) 0.018(2) 0.0048(17) -0.0004(16) -0.0056(16) O11 0.0158(15) 0.0192(16) 0.0165(15) -0.0010(12) 0.0040(12) 0.0000(12) C11 0.010(2) 0.019(2) 0.016(2) -0.0021(17) -0.0002(16) 0.0001(17) O12 0.0196(16) 0.0123(15) 0.0189(15) -0.0022(12) 0.0080(12) 0.0018(12) C12 0.013(2) 0.019(2) 0.018(2) 0.0066(17) -0.0002(17) -0.0048(17) C13 0.015(2) 0.016(2) 0.023(2) -0.0011(18) 0.0014(18) -0.0009(17) C14 0.014(2) 0.009(2) 0.026(2) -0.0041(17) 0.0001(18) -0.0004(17) C15 0.0068(19) 0.017(2) 0.018(2) -0.0002(17) 0.0003(16) 0.0027(16) C16 0.016(2) 0.020(2) 0.019(2) 0.0027(18) 0.0039(17) -0.0021(18) C17 0.028(3) 0.018(2) 0.029(3) 0.006(2) 0.007(2) -0.003(2) C18 0.017(2) 0.022(2) 0.016(2) -0.0002(18) 0.0029(17) 0.0036(19) C19 0.0057(19) 0.020(2) 0.016(2) -0.0020(17) -0.0010(16) -0.0013(16) C20 0.0035(19) 0.025(2) 0.020(2) 0.0030(18) -0.0054(16) -0.0029(17) C21 0.015(2) 0.019(2) 0.023(2) 0.0014(19) 0.0000(18) -0.0001(18) C22 0.011(2) 0.025(3) 0.024(2) 0.0093(19) 0.0009(18) -0.0078(18) C23 0.016(2) 0.027(3) 0.013(2) 0.0012(18) 0.0011(17) -0.0011(19) C24 0.0080(19) 0.019(2) 0.021(2) 0.0047(18) 0.0004(17) 0.0011(17) C25 0.020(2) 0.020(2) 0.023(2) -0.0032(19) 0.0032(18) 0.0013(19) C26 0.024(3) 0.031(3) 0.036(3) 0.009(2) 0.005(2) 0.001(2) C27 0.025(2) 0.025(3) 0.022(2) 0.002(2) 0.0052(19) 0.003(2) C28 0.017(2) 0.012(2) 0.020(2) 0.0042(17) 0.0068(17) 0.0024(17) C29 0.017(2) 0.016(2) 0.020(2) 0.0022(17) 0.0055(17) 0.0037(18) C30 0.031(3) 0.019(2) 0.014(2) 0.0050(18) 0.0047(19) 0.008(2) C31 0.021(2) 0.022(2) 0.026(2) 0.0100(19) 0.0138(19) 0.0110(19) C32 0.016(2) 0.021(2) 0.026(2) 0.0065(19) 0.0043(18) 0.0027(18) C33 0.016(2) 0.011(2) 0.022(2) 0.0057(17) 0.0053(17) 0.0005(17) C34 0.025(3) 0.034(3) 0.022(2) -0.009(2) 0.004(2) 0.001(2) C35 0.036(3) 0.030(3) 0.035(3) 0.006(2) 0.023(2) 0.013(2) C36 0.019(2) 0.025(3) 0.023(2) 0.002(2) 0.0027(19) -0.0001(19) C37 0.027(3) 0.035(3) 0.035(3) -0.003(2) -0.005(2) -0.001(2) C38 0.020(2) 0.024(3) 0.028(3) -0.006(2) -0.004(2) -0.001(2) C39 0.019(2) 0.033(3) 0.040(3) 0.004(2) -0.001(2) -0.003(2) C40 0.037(3) 0.093(5) 0.026(3) 0.013(3) 0.013(3) 0.006(3) C41 0.023(2) 0.022(2) 0.022(2) 0.0003(19) 0.0094(19) -0.0045(19) C42 0.019(2) 0.015(2) 0.030(3) -0.0076(19) 0.0062(19) -0.0042(18) C43 0.014(2) 0.018(2) 0.033(3) -0.009(2) 0.0009(19) 0.0002(18) C44 0.040(3) 0.035(3) 0.028(3) -0.007(2) 0.013(2) 0.000(2) C45 0.023(2) 0.021(3) 0.034(3) -0.003(2) -0.007(2) -0.002(2) C46 0.023(2) 0.019(2) 0.016(2) 0.0016(18) -0.0007(18) 0.0040(19) C47 0.013(2) 0.022(2) 0.027(2) 0.0020(19) -0.0018(18) 0.0000(18) C48 0.029(3) 0.048(3) 0.026(3) 0.007(2) 0.008(2) -0.003(2) C49 0.029(3) 0.037(3) 0.022(2) 0.004(2) 0.011(2) 0.004(2) C50 0.020(2) 0.012(2) 0.023(2) -0.0025(18) 0.0043(18) -0.0001(18) C51 0.018(2) 0.014(2) 0.023(2) 0.0009(18) 0.0040(18) -0.0010(17) C52 0.017(2) 0.022(2) 0.017(2) -0.0004(18) 0.0069(17) -0.0025(18) _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 Ca1 O1 2.196(3) . ? Ca1 O2 2.309(3) . ? Ca1 O3 2.361(3) . ? Ca1 O5 2.460(3) . ? Ca1 O8 2.472(3) . ? Ca1 O7 2.518(3) . ? Ca1 C19 3.209(4) . ? Ca1 Ca2 3.6900(11) . ? O1 C1 1.319(5) . ? C1 C6 1.418(6) . ? C1 C2 1.420(6) . ? Ca2 O4 2.192(3) . ? Ca2 O3 2.315(3) . ? Ca2 O2 2.364(3) . ? Ca2 O11 2.477(3) . ? Ca2 O9 2.484(3) . ? Ca2 O12 2.513(3) . ? Ca2 C10 3.218(4) . ? O2 C10 1.346(5) . ? C2 C3 1.391(6) . ? C2 C7 1.505(7) . ? O3 C19 1.340(5) . ? C3 C4 1.390(7) . ? C3 H1 0.9500 . ? O4 C28 1.324(5) . ? C4 C5 1.380(7) . ? C4 C8 1.512(6) . ? O5 C38 1.432(6) . ? O5 C37 1.432(6) . ? C5 C6 1.391(6) . ? C5 H2 0.9500 . ? O6 C39 1.415(6) . ? O6 C40 1.417(6) . ? C6 C9 1.502(6) . ? O7 C41 1.431(5) . ? O7 C42 1.432(5) . ? C7 H3 0.9800 . ? C7 H4 0.9800 . ? C7 H5 0.9800 . ? O8 C44 1.416(6) . ? O8 C43 1.427(5) . ? C8 H6 0.9800 . ? C8 H7 0.9800 . ? C8 H8 0.9800 . ? O9 C45 1.431(5) . ? O9 C46 1.434(5) . ? C9 H9 0.9800 . ? C9 H10 0.9800 . ? C9 H11 0.9800 . ? O10 C47 1.419(5) . ? O10 C48 1.420(5) . ? C10 C15 1.413(6) . ? C10 C11 1.418(6) . ? O11 C49 1.424(5) . ? O11 C50 1.440(5) . ? C11 C12 1.382(6) . ? C11 C16 1.504(6) . ? O12 C51 1.430(5) . ? O12 C52 1.439(5) . ? C12 C13 1.383(6) . ? C12 H12 0.9500 . ? C13 C14 1.390(6) . ? C13 C17 1.505(6) . ? C14 C15 1.391(6) . ? C14 H13 0.9500 . ? C15 C18 1.501(6) . ? C16 H14 0.9800 . ? C16 H15 0.9800 . ? C16 H16 0.9800 . ? C17 H17 0.9800 . ? C17 H18 0.9800 . ? C17 H19 0.9800 . ? C18 H20 0.9800 . ? C18 H21 0.9800 . ? C18 H22 0.9800 . ? C19 C24 1.405(6) . ? C19 C20 1.415(6) . ? C20 C21 1.391(6) . ? C20 C25 1.513(6) . ? C21 C22 1.389(6) . ? C21 H23 0.9500 . ? C22 C23 1.393(7) . ? C22 C26 1.510(6) . ? C23 C24 1.379(6) . ? C23 H24 0.9500 . ? C24 C27 1.499(6) . ? C25 H25 0.9800 . ? C25 H26 0.9800 . ? C25 H27 0.9800 . ? C26 H28 0.9800 . ? C26 H29 0.9800 . ? C26 H30 0.9800 . ? C27 H31 0.9800 . ? C27 H33 0.9800 . ? C27 H32 0.9800 . ? C28 C33 1.419(6) . ? C28 C29 1.422(6) . ? C29 C30 1.393(6) . ? C29 C34 1.504(6) . ? C30 C31 1.386(7) . ? C30 H34 0.9500 . ? C31 C32 1.385(7) . ? C31 C35 1.506(6) . ? C32 C33 1.389(6) . ? C32 H35 0.9500 . ? C33 C36 1.502(6) . ? C34 H36 0.9800 . ? C34 H37 0.9800 . ? C34 H38 0.9800 . ? C35 H40 0.9800 . ? C35 H39 0.9800 . ? C35 H41 0.9800 . ? C36 H42 0.9800 . ? C36 H43 0.9800 . ? C36 H44 0.9800 . ? C37 H45 0.9800 . ? C37 H46 0.9800 . ? C37 H47 0.9800 . ? C38 C39 1.495(7) . ? C38 H48 0.9900 . ? C38 H49 0.9900 . ? C39 H50 0.9900 . ? C39 H51 0.9900 . ? C40 H52 0.9800 . ? C40 H53 0.9800 . ? C40 H54 0.9800 . ? C41 H55 0.9800 . ? C41 H56 0.9800 . ? C41 H57 0.9800 . ? C42 C43 1.495(6) . ? C42 H58 0.9900 . ? C42 H59 0.9900 . ? C43 H60 0.9900 . ? C43 H61 0.9900 . ? C44 H62 0.9800 . ? C44 H63 0.9800 . ? C44 H64 0.9800 . ? C45 H65 0.9800 . ? C45 H66 0.9800 . ? C45 H67 0.9800 . ? C46 C47 1.507(6) . ? C46 H68 0.9900 . ? C46 H69 0.9900 . ? C47 H70 0.9900 . ? C47 H71 0.9900 . ? C48 H72 0.9800 . ? C48 H73 0.9800 . ? C48 H74 0.9800 . ? C49 H75 0.9800 . ? C49 H76 0.9800 . ? C49 H77 0.9800 . ? C50 C51 1.498(6) . ? C50 H78 0.9900 . ? C50 H79 0.9900 . ? C51 H80 0.9900 . ? C51 H81 0.9900 . ? C52 H82 0.9800 . ? C52 H83 0.9800 . ? C52 H84 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Ca1 O2 109.31(11) . . ? O1 Ca1 O3 113.70(11) . . ? O2 Ca1 O3 75.82(10) . . ? O1 Ca1 O5 89.66(11) . . ? O2 Ca1 O5 91.67(11) . . ? O3 Ca1 O5 155.97(11) . . ? O1 Ca1 O8 145.70(11) . . ? O2 Ca1 O8 102.26(10) . . ? O3 Ca1 O8 86.43(10) . . ? O5 Ca1 O8 76.13(11) . . ? O1 Ca1 O7 85.97(11) . . ? O2 Ca1 O7 164.39(10) . . ? O3 Ca1 O7 95.48(10) . . ? O5 Ca1 O7 91.56(11) . . ? O8 Ca1 O7 63.81(10) . . ? O1 Ca1 C19 108.63(11) . . ? O2 Ca1 C19 97.45(10) . . ? O3 Ca1 C19 21.74(10) . . ? O5 Ca1 C19 155.30(11) . . ? O8 Ca1 C19 79.51(10) . . ? O7 Ca1 C19 73.90(10) . . ? O1 Ca1 Ca2 117.35(8) . . ? O2 Ca1 Ca2 38.37(7) . . ? O3 Ca1 Ca2 37.45(7) . . ? O5 Ca1 Ca2 127.23(8) . . ? O8 Ca1 Ca2 95.69(7) . . ? O7 Ca1 Ca2 131.80(7) . . ? C19 Ca1 Ca2 59.13(7) . . ? C1 O1 Ca1 160.3(3) . . ? O1 C1 C6 120.6(4) . . ? O1 C1 C2 121.8(4) . . ? C6 C1 C2 117.7(4) . . ? O4 Ca2 O3 108.07(11) . . ? O4 Ca2 O2 114.22(11) . . ? O3 Ca2 O2 75.66(10) . . ? O4 Ca2 O11 144.15(11) . . ? O3 Ca2 O11 104.63(10) . . ? O2 Ca2 O11 87.68(10) . . ? O4 Ca2 O9 90.26(10) . . ? O3 Ca2 O9 89.64(10) . . ? O2 Ca2 O9 154.24(10) . . ? O11 Ca2 O9 75.53(10) . . ? O4 Ca2 O12 85.37(10) . . ? O3 Ca2 O12 165.66(10) . . ? O2 Ca2 O12 94.52(10) . . ? O11 Ca2 O12 63.97(9) . . ? O9 Ca2 O12 95.40(10) . . ? O4 Ca2 C10 110.57(11) . . ? O3 Ca2 C10 97.16(10) . . ? O2 Ca2 C10 21.74(10) . . ? O11 Ca2 C10 79.03(10) . . ? O9 Ca2 C10 154.56(10) . . ? O12 Ca2 C10 72.80(10) . . ? O4 Ca2 Ca1 117.52(8) . . ? O3 Ca2 Ca1 38.33(7) . . ? O2 Ca2 Ca1 37.33(7) . . ? O11 Ca2 Ca1 97.26(7) . . ? O9 Ca2 Ca1 124.78(7) . . ? O12 Ca2 Ca1 130.98(7) . . ? C10 Ca2 Ca1 58.87(7) . . ? C10 O2 Ca1 137.1(2) . . ? C10 O2 Ca2 117.7(2) . . ? Ca1 O2 Ca2 104.30(11) . . ? C3 C2 C1 119.5(4) . . ? C3 C2 C7 120.2(4) . . ? C1 C2 C7 120.3(4) . . ? C19 O3 Ca2 137.9(2) . . ? C19 O3 Ca1 117.5(2) . . ? Ca2 O3 Ca1 104.22(11) . . ? C4 C3 C2 122.9(4) . . ? C4 C3 H1 118.6 . . ? C2 C3 H1 118.6 . . ? C28 O4 Ca2 158.5(3) . . ? C5 C4 C3 117.0(4) . . ? C5 C4 C8 121.0(5) . . ? C3 C4 C8 121.9(5) . . ? C38 O5 C37 113.8(4) . . ? C38 O5 Ca1 120.1(3) . . ? C37 O5 Ca1 125.9(3) . . ? C4 C5 C6 122.7(4) . . ? C4 C5 H2 118.6 . . ? C6 C5 H2 118.6 . . ? C39 O6 C40 111.2(4) . . ? C5 C6 C1 120.0(4) . . ? C5 C6 C9 121.1(4) . . ? C1 C6 C9 119.0(4) . . ? C41 O7 C42 110.5(3) . . ? C41 O7 Ca1 121.3(2) . . ? C42 O7 Ca1 116.9(2) . . ? C2 C7 H3 109.5 . . ? C2 C7 H4 109.5 . . ? H3 C7 H4 109.5 . . ? C2 C7 H5 109.5 . . ? H3 C7 H5 109.5 . . ? H4 C7 H5 109.5 . . ? C44 O8 C43 112.1(4) . . ? C44 O8 Ca1 122.6(3) . . ? C43 O8 Ca1 121.9(2) . . ? C4 C8 H6 109.5 . . ? C4 C8 H7 109.5 . . ? H6 C8 H7 109.5 . . ? C4 C8 H8 109.5 . . ? H6 C8 H8 109.5 . . ? H7 C8 H8 109.5 . . ? C45 O9 C46 112.9(3) . . ? C45 O9 Ca2 128.9(3) . . ? C46 O9 Ca2 117.3(2) . . ? C6 C9 H9 109.5 . . ? C6 C9 H10 109.5 . . ? H9 C9 H10 109.5 . . ? C6 C9 H11 109.5 . . ? H9 C9 H11 109.5 . . ? H10 C9 H11 109.5 . . ? C47 O10 C48 110.6(4) . . ? O2 C10 C15 121.3(4) . . ? O2 C10 C11 121.0(4) . . ? C15 C10 C11 117.7(4) . . ? O2 C10 Ca2 40.55(17) . . ? C15 C10 Ca2 121.5(3) . . ? C11 C10 Ca2 104.1(3) . . ? C49 O11 C50 110.7(3) . . ? C49 O11 Ca2 124.8(3) . . ? C50 O11 Ca2 121.9(2) . . ? C12 C11 C10 119.9(4) . . ? C12 C11 C16 120.4(4) . . ? C10 C11 C16 119.7(4) . . ? C51 O12 C52 110.7(3) . . ? C51 O12 Ca2 116.4(2) . . ? C52 O12 Ca2 123.3(2) . . ? C11 C12 C13 123.1(4) . . ? C11 C12 H12 118.5 . . ? C13 C12 H12 118.5 . . ? C12 C13 C14 116.8(4) . . ? C12 C13 C17 121.2(4) . . ? C14 C13 C17 122.0(4) . . ? C13 C14 C15 122.7(4) . . ? C13 C14 H13 118.6 . . ? C15 C14 H13 118.6 . . ? C14 C15 C10 119.7(4) . . ? C14 C15 C18 120.2(4) . . ? C10 C15 C18 120.0(4) . . ? C11 C16 H14 109.5 . . ? C11 C16 H15 109.5 . . ? H14 C16 H15 109.5 . . ? C11 C16 H16 109.5 . . ? H14 C16 H16 109.5 . . ? H15 C16 H16 109.5 . . ? C13 C17 H17 109.5 . . ? C13 C17 H18 109.5 . . ? H17 C17 H18 109.5 . . ? C13 C17 H19 109.5 . . ? H17 C17 H19 109.5 . . ? H18 C17 H19 109.5 . . ? C15 C18 H20 109.5 . . ? C15 C18 H21 109.5 . . ? H20 C18 H21 109.5 . . ? C15 C18 H22 109.5 . . ? H20 C18 H22 109.5 . . ? H21 C18 H22 109.5 . . ? O3 C19 C24 120.9(4) . . ? O3 C19 C20 121.0(4) . . ? C24 C19 C20 118.1(4) . . ? O3 C19 Ca1 40.73(17) . . ? C24 C19 Ca1 103.7(3) . . ? C20 C19 Ca1 121.9(3) . . ? C21 C20 C19 119.6(4) . . ? C21 C20 C25 119.8(4) . . ? C19 C20 C25 120.6(4) . . ? C22 C21 C20 122.5(4) . . ? C22 C21 H23 118.8 . . ? C20 C21 H23 118.8 . . ? C21 C22 C23 117.1(4) . . ? C21 C22 C26 122.2(4) . . ? C23 C22 C26 120.8(4) . . ? C24 C23 C22 122.3(4) . . ? C24 C23 H24 118.8 . . ? C22 C23 H24 118.8 . . ? C23 C24 C19 120.5(4) . . ? C23 C24 C27 119.1(4) . . ? C19 C24 C27 120.5(4) . . ? C20 C25 H25 109.5 . . ? C20 C25 H26 109.5 . . ? H25 C25 H26 109.5 . . ? C20 C25 H27 109.5 . . ? H25 C25 H27 109.5 . . ? H26 C25 H27 109.5 . . ? C22 C26 H28 109.5 . . ? C22 C26 H29 109.5 . . ? H28 C26 H29 109.5 . . ? C22 C26 H30 109.5 . . ? H28 C26 H30 109.5 . . ? H29 C26 H30 109.5 . . ? C24 C27 H31 109.5 . . ? C24 C27 H33 109.5 . . ? H31 C27 H33 109.5 . . ? C24 C27 H32 109.5 . . ? H31 C27 H32 109.5 . . ? H33 C27 H32 109.5 . . ? O4 C28 C33 120.8(4) . . ? O4 C28 C29 121.5(4) . . ? C33 C28 C29 117.6(4) . . ? C30 C29 C28 119.3(4) . . ? C30 C29 C34 120.4(4) . . ? C28 C29 C34 120.3(4) . . ? C31 C30 C29 123.4(4) . . ? C31 C30 H34 118.3 . . ? C29 C30 H34 118.3 . . ? C32 C31 C30 116.5(4) . . ? C32 C31 C35 121.7(4) . . ? C30 C31 C35 121.8(4) . . ? C31 C32 C33 123.2(4) . . ? C31 C32 H35 118.4 . . ? C33 C32 H35 118.4 . . ? C32 C33 C28 119.9(4) . . ? C32 C33 C36 120.7(4) . . ? C28 C33 C36 119.4(4) . . ? C29 C34 H36 109.5 . . ? C29 C34 H37 109.5 . . ? H36 C34 H37 109.5 . . ? C29 C34 H38 109.5 . . ? H36 C34 H38 109.5 . . ? H37 C34 H38 109.5 . . ? C31 C35 H40 109.5 . . ? C31 C35 H39 109.5 . . ? H40 C35 H39 109.5 . . ? C31 C35 H41 109.5 . . ? H40 C35 H41 109.5 . . ? H39 C35 H41 109.5 . . ? C33 C36 H42 109.5 . . ? C33 C36 H43 109.5 . . ? H42 C36 H43 109.5 . . ? C33 C36 H44 109.5 . . ? H42 C36 H44 109.5 . . ? H43 C36 H44 109.5 . . ? O5 C37 H45 109.5 . . ? O5 C37 H46 109.5 . . ? H45 C37 H46 109.5 . . ? O5 C37 H47 109.5 . . ? H45 C37 H47 109.5 . . ? H46 C37 H47 109.5 . . ? O5 C38 C39 112.3(4) . . ? O5 C38 H48 109.1 . . ? C39 C38 H48 109.1 . . ? O5 C38 H49 109.1 . . ? C39 C38 H49 109.1 . . ? H48 C38 H49 107.9 . . ? O6 C39 C38 110.2(4) . . ? O6 C39 H50 109.6 . . ? C38 C39 H50 109.6 . . ? O6 C39 H51 109.6 . . ? C38 C39 H51 109.6 . . ? H50 C39 H51 108.1 . . ? O6 C40 H52 109.5 . . ? O6 C40 H53 109.5 . . ? H52 C40 H53 109.5 . . ? O6 C40 H54 109.5 . . ? H52 C40 H54 109.5 . . ? H53 C40 H54 109.5 . . ? O7 C41 H55 109.5 . . ? O7 C41 H56 109.5 . . ? H55 C41 H56 109.5 . . ? O7 C41 H57 109.5 . . ? H55 C41 H57 109.5 . . ? H56 C41 H57 109.5 . . ? O7 C42 C43 107.7(4) . . ? O7 C42 H58 110.2 . . ? C43 C42 H58 110.2 . . ? O7 C42 H59 110.2 . . ? C43 C42 H59 110.2 . . ? H58 C42 H59 108.5 . . ? O8 C43 C42 109.1(3) . . ? O8 C43 H60 109.9 . . ? C42 C43 H60 109.9 . . ? O8 C43 H61 109.9 . . ? C42 C43 H61 109.9 . . ? H60 C43 H61 108.3 . . ? O8 C44 H62 109.5 . . ? O8 C44 H63 109.5 . . ? H62 C44 H63 109.5 . . ? O8 C44 H64 109.5 . . ? H62 C44 H64 109.5 . . ? H63 C44 H64 109.5 . . ? O9 C45 H65 109.5 . . ? O9 C45 H66 109.5 . . ? H65 C45 H66 109.5 . . ? O9 C45 H67 109.5 . . ? H65 C45 H67 109.5 . . ? H66 C45 H67 109.5 . . ? O9 C46 C47 112.7(4) . . ? O9 C46 H68 109.1 . . ? C47 C46 H68 109.1 . . ? O9 C46 H69 109.1 . . ? C47 C46 H69 109.1 . . ? H68 C46 H69 107.8 . . ? O10 C47 C46 109.7(4) . . ? O10 C47 H70 109.7 . . ? C46 C47 H70 109.7 . . ? O10 C47 H71 109.7 . . ? C46 C47 H71 109.7 . . ? H70 C47 H71 108.2 . . ? O10 C48 H72 109.5 . . ? O10 C48 H73 109.5 . . ? H72 C48 H73 109.5 . . ? O10 C48 H74 109.5 . . ? H72 C48 H74 109.5 . . ? H73 C48 H74 109.5 . . ? O11 C49 H75 109.5 . . ? O11 C49 H76 109.5 . . ? H75 C49 H76 109.5 . . ? O11 C49 H77 109.5 . . ? H75 C49 H77 109.5 . . ? H76 C49 H77 109.5 . . ? O11 C50 C51 108.7(3) . . ? O11 C50 H78 109.9 . . ? C51 C50 H78 109.9 . . ? O11 C50 H79 109.9 . . ? C51 C50 H79 109.9 . . ? H78 C50 H79 108.3 . . ? O12 C51 C50 108.3(3) . . ? O12 C51 H80 110.0 . . ? C50 C51 H80 110.0 . . ? O12 C51 H81 110.0 . . ? C50 C51 H81 110.0 . . ? H80 C51 H81 108.4 . . ? O12 C52 H82 109.5 . . ? O12 C52 H83 109.5 . . ? H82 C52 H83 109.5 . . ? O12 C52 H84 109.5 . . ? H82 C52 H84 109.5 . . ? H83 C52 H84 109.5 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.681 _refine_diff_density_min -1.079 _refine_diff_density_rms 0.076 data_c:\monop2 _database_code_depnum_ccdc_archive 'CCDC 716847' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C52 H84 O12 Sr2' _chemical_formula_sum 'C52 H84 O12 Sr2' _chemical_formula_weight 1076.43 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sr Sr -1.5307 3.2498 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 16.1057(4) _cell_length_b 15.7854(4) _cell_length_c 22.3065(6) _cell_angle_alpha 90.00 _cell_angle_beta 103.024(2) _cell_angle_gamma 90.00 _cell_volume 5525.2(2) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.294 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2272 _exptl_absorpt_coefficient_mu 1.987 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7163 _exptl_absorpt_correction_T_max 0.7549 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker X8 Apex II CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 60509 _diffrn_reflns_av_R_equivalents 0.0568 _diffrn_reflns_av_sigmaI/netI 0.0473 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.30 _diffrn_reflns_theta_max 27.50 _reflns_number_total 12644 _reflns_number_gt 8823 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART (Bruker)' _computing_cell_refinement 'Bruker SMART (Bruker)' _computing_data_reduction 'Bruker SAINT (Bruker)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 1999)' _computing_publication_material 'CIFTAB (Sheldrick, 1997)' _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^)+(0.0333P)^2^+0.8057P] 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 ? _refine_ls_extinction_coef ? _refine_ls_number_reflns 12644 _refine_ls_number_parameters 615 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0646 _refine_ls_R_factor_gt 0.0313 _refine_ls_wR_factor_ref 0.0741 _refine_ls_wR_factor_gt 0.0637 _refine_ls_goodness_of_fit_ref 1.014 _refine_ls_restrained_S_all 1.014 _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 Sr1 Sr 0.127890(12) 0.256920(11) 0.237830(8) 0.01449(5) Uani 1 1 d . . . O1 O 0.06110(9) 0.33069(9) 0.30380(6) 0.0239(3) Uani 1 1 d . . . C1 C 0.00796(14) 0.34600(13) 0.33962(9) 0.0200(5) Uani 1 1 d . . . Sr2 Sr 0.372430(12) 0.286040(11) 0.257780(8) 0.01373(5) Uani 1 1 d . . . O2 O 0.23224(9) 0.34577(9) 0.20411(6) 0.0205(3) Uani 1 1 d . . . C2 C 0.03704(15) 0.37911(14) 0.39972(10) 0.0253(5) Uani 1 1 d . . . O3 O 0.26806(9) 0.19515(9) 0.28951(6) 0.0201(3) Uani 1 1 d . . . C3 C -0.02103(17) 0.39127(14) 0.43650(10) 0.0316(6) Uani 1 1 d . . . H1 H -0.0006 0.4127 0.4769 0.038 Uiso 1 1 calc R . . O4 O 0.44116(9) 0.21054(9) 0.19408(6) 0.0235(3) Uani 1 1 d . . . C4 C -0.10711(17) 0.37374(15) 0.41725(11) 0.0337(6) Uani 1 1 d . . . O5 O 0.01497(10) 0.30378(10) 0.14144(7) 0.0296(4) Uani 1 1 d . . . C5 C -0.13488(15) 0.34459(14) 0.35747(11) 0.0299(6) Uani 1 1 d . . . H2 H -0.1939 0.3335 0.3425 0.036 Uiso 1 1 calc R . . O6 O -0.02693(11) 0.37264(14) 0.01059(7) 0.0521(6) Uani 1 1 d . . . C6 C -0.08014(14) 0.33100(13) 0.31863(10) 0.0224(5) Uani 1 1 d . . . O7 O 0.03552(9) 0.12378(9) 0.25363(6) 0.0230(3) Uani 1 1 d . . . C7 C 0.12822(15) 0.40453(17) 0.42147(11) 0.0399(7) Uani 1 1 d . . . H3 H 0.1333 0.4456 0.4550 0.060 Uiso 1 1 calc R . . H4 H 0.1484 0.4302 0.3874 0.060 Uiso 1 1 calc R . . H5 H 0.1627 0.3544 0.4363 0.060 Uiso 1 1 calc R . . O8 O 0.11838(9) 0.12958(9) 0.16211(6) 0.0243(3) Uani 1 1 d . . . C8 C -0.16786(19) 0.38681(17) 0.45874(13) 0.0543(9) Uani 1 1 d . . . H6 H -0.1838 0.3317 0.4731 0.081 Uiso 1 1 calc R . . H7 H -0.2191 0.4159 0.4360 0.081 Uiso 1 1 calc R . . H8 H -0.1403 0.4212 0.4942 0.081 Uiso 1 1 calc R . . O9 O 0.48201(9) 0.23872(9) 0.35609(6) 0.0242(3) Uani 1 1 d . . . C9 C -0.11282(14) 0.30200(15) 0.25346(10) 0.0305(6) Uani 1 1 d . . . H9 H -0.0956 0.3426 0.2253 0.046 Uiso 1 1 calc R . . H10 H -0.1751 0.2984 0.2446 0.046 Uiso 1 1 calc R . . H11 H -0.0891 0.2461 0.2480 0.046 Uiso 1 1 calc R . . O10 O 0.52947(10) 0.13336(12) 0.47766(7) 0.0369(4) Uani 1 1 d . . . C10 C 0.23439(12) 0.42051(13) 0.17585(9) 0.0173(4) Uani 1 1 d . . . O11 O 0.38549(9) 0.41608(9) 0.33126(6) 0.0223(3) Uani 1 1 d . . . C11 C 0.26121(13) 0.42545(13) 0.12015(9) 0.0188(5) Uani 1 1 d . . . O12 O 0.46328(9) 0.41778(9) 0.23625(6) 0.0211(3) Uani 1 1 d . . . C12 C 0.26356(13) 0.50345(13) 0.09174(9) 0.0206(5) Uani 1 1 d . . . H12 H 0.2823 0.5059 0.0543 0.025 Uiso 1 1 calc R . . C13 C 0.23959(13) 0.57773(14) 0.11610(9) 0.0215(5) Uani 1 1 d . . . C14 C 0.21379(13) 0.57243(13) 0.17123(9) 0.0207(5) Uani 1 1 d . . . H13 H 0.1974 0.6228 0.1888 0.025 Uiso 1 1 calc R . . C15 C 0.21101(13) 0.49611(13) 0.20184(9) 0.0181(4) Uani 1 1 d . . . C16 C 0.28596(14) 0.34631(14) 0.09085(10) 0.0245(5) Uani 1 1 d . . . H14 H 0.3033 0.3611 0.0528 0.037 Uiso 1 1 calc R . . H15 H 0.2372 0.3076 0.0814 0.037 Uiso 1 1 calc R . . H16 H 0.3335 0.3187 0.1193 0.037 Uiso 1 1 calc R . . C17 C 0.23955(15) 0.66075(14) 0.08255(10) 0.0297(5) Uani 1 1 d . . . H17 H 0.2862 0.6610 0.0609 0.045 Uiso 1 1 calc R . . H18 H 0.2474 0.7075 0.1122 0.045 Uiso 1 1 calc R . . H19 H 0.1851 0.6677 0.0527 0.045 Uiso 1 1 calc R . . C18 C 0.18537(14) 0.49351(14) 0.26249(9) 0.0257(5) Uani 1 1 d . . . H20 H 0.1712 0.5508 0.2738 0.039 Uiso 1 1 calc R . . H21 H 0.2326 0.4713 0.2942 0.039 Uiso 1 1 calc R . . H22 H 0.1355 0.4567 0.2591 0.039 Uiso 1 1 calc R . . C19 C 0.26561(12) 0.12202(13) 0.31973(9) 0.0175(4) Uani 1 1 d . . . C20 C 0.28738(13) 0.04428(13) 0.29558(9) 0.0198(5) Uani 1 1 d . . . C21 C 0.28418(13) -0.02974(14) 0.32872(10) 0.0221(5) Uani 1 1 d . . . H23 H 0.2993 -0.0816 0.3124 0.027 Uiso 1 1 calc R . . C22 C 0.25995(13) -0.03149(14) 0.38448(10) 0.0239(5) Uani 1 1 d . . . C23 C 0.23822(13) 0.04496(14) 0.40700(10) 0.0231(5) Uani 1 1 d . . . H24 H 0.2209 0.0454 0.4450 0.028 Uiso 1 1 calc R . . C24 C 0.24068(13) 0.12118(13) 0.37640(9) 0.0197(5) Uani 1 1 d . . . C25 C 0.31147(14) 0.04277(14) 0.23423(9) 0.0262(5) Uani 1 1 d . . . H25 H 0.3270 -0.0151 0.2251 0.039 Uiso 1 1 calc R . . H26 H 0.3601 0.0806 0.2354 0.039 Uiso 1 1 calc R . . H27 H 0.2630 0.0618 0.2021 0.039 Uiso 1 1 calc R . . C26 C 0.25906(15) -0.11231(15) 0.42048(11) 0.0342(6) Uani 1 1 d . . . H31 H 0.3120 -0.1168 0.4522 0.051 Uiso 1 1 calc R . . H32 H 0.2542 -0.1609 0.3926 0.051 Uiso 1 1 calc R . . H33 H 0.2104 -0.1117 0.4400 0.051 Uiso 1 1 calc R . . C27 C 0.21877(15) 0.20239(14) 0.40390(10) 0.0270(5) Uani 1 1 d . . . H28 H 0.2048 0.1907 0.4436 0.041 Uiso 1 1 calc R . . H29 H 0.1696 0.2286 0.3761 0.041 Uiso 1 1 calc R . . H30 H 0.2676 0.2410 0.4099 0.041 Uiso 1 1 calc R . . C28 C 0.49732(14) 0.19504(12) 0.16042(9) 0.0184(5) Uani 1 1 d . . . C29 C 0.47223(14) 0.16005(13) 0.10053(9) 0.0212(5) Uani 1 1 d . . . C30 C 0.53308(15) 0.14630(13) 0.06647(9) 0.0242(5) Uani 1 1 d . . . H34 H 0.5152 0.1236 0.0262 0.029 Uiso 1 1 calc R . . C31 C 0.61859(15) 0.16407(14) 0.08838(10) 0.0252(5) Uani 1 1 d . . . C32 C 0.64288(14) 0.19604(13) 0.14774(10) 0.0242(5) Uani 1 1 d . . . H35 H 0.7014 0.2078 0.1642 0.029 Uiso 1 1 calc R . . C33 C 0.58478(14) 0.21153(13) 0.18392(9) 0.0206(5) Uani 1 1 d . . . C34 C 0.38078(14) 0.13555(16) 0.07608(10) 0.0324(6) Uani 1 1 d . . . H36 H 0.3765 0.0986 0.0402 0.049 Uiso 1 1 calc R . . H37 H 0.3465 0.1866 0.0640 0.049 Uiso 1 1 calc R . . H38 H 0.3597 0.1054 0.1081 0.049 Uiso 1 1 calc R . . C35 C 0.68335(16) 0.14948(16) 0.04997(11) 0.0375(6) Uani 1 1 d . . . H39 H 0.6619 0.1064 0.0187 0.056 Uiso 1 1 calc R . . H40 H 0.7370 0.1300 0.0765 0.056 Uiso 1 1 calc R . . H41 H 0.6932 0.2025 0.0298 0.056 Uiso 1 1 calc R . . C36 C 0.61378(15) 0.24327(15) 0.24884(10) 0.0282(5) Uani 1 1 d . . . H42 H 0.5852 0.2970 0.2532 0.042 Uiso 1 1 calc R . . H43 H 0.6756 0.2521 0.2582 0.042 Uiso 1 1 calc R . . H44 H 0.5994 0.2014 0.2774 0.042 Uiso 1 1 calc R . . C37 C -0.05458(16) 0.25290(16) 0.10999(12) 0.0413(7) Uani 1 1 d . . . H45 H -0.1080 0.2841 0.1066 0.062 Uiso 1 1 calc R . . H46 H -0.0566 0.2004 0.1331 0.062 Uiso 1 1 calc R . . H47 H -0.0468 0.2392 0.0687 0.062 Uiso 1 1 calc R . . C38 C 0.01477(16) 0.38856(15) 0.11892(10) 0.0322(6) Uani 1 1 d . . . H48 H 0.0535 0.4235 0.1500 0.039 Uiso 1 1 calc R . . H49 H -0.0434 0.4123 0.1134 0.039 Uiso 1 1 calc R . . C39 C 0.04203(15) 0.39448(17) 0.05904(11) 0.0371(6) Uani 1 1 d . . . H50 H 0.0610 0.4529 0.0531 0.045 Uiso 1 1 calc R . . H51 H 0.0904 0.3556 0.0595 0.045 Uiso 1 1 calc R . . C40 C -0.00138(18) 0.3605(2) -0.04571(12) 0.0613(10) Uani 1 1 d . . . H52 H 0.0281 0.4114 -0.0553 0.092 Uiso 1 1 calc R . . H53 H -0.0517 0.3501 -0.0788 0.092 Uiso 1 1 calc R . . H54 H 0.0372 0.3118 -0.0419 0.092 Uiso 1 1 calc R . . C41 C 0.01691(14) 0.11316(14) 0.31298(10) 0.0262(5) Uani 1 1 d . . . H55 H -0.0341 0.0779 0.3092 0.039 Uiso 1 1 calc R . . H56 H 0.0068 0.1687 0.3297 0.039 Uiso 1 1 calc R . . H57 H 0.0652 0.0856 0.3407 0.039 Uiso 1 1 calc R . . C42 C 0.05902(14) 0.04507(13) 0.22990(10) 0.0256(5) Uani 1 1 d . . . H58 H 0.0161 0.0011 0.2323 0.031 Uiso 1 1 calc R . . H59 H 0.1149 0.0259 0.2545 0.031 Uiso 1 1 calc R . . C43 C 0.06391(15) 0.05836(14) 0.16472(10) 0.0270(5) Uani 1 1 d . . . H60 H 0.0871 0.0071 0.1488 0.032 Uiso 1 1 calc R . . H61 H 0.0063 0.0693 0.1390 0.032 Uiso 1 1 calc R . . C44 C 0.13949(16) 0.13708(17) 0.10368(10) 0.0376(6) Uani 1 1 d . . . H62 H 0.1654 0.0841 0.0939 0.056 Uiso 1 1 calc R . . H63 H 0.1799 0.1838 0.1048 0.056 Uiso 1 1 calc R . . H64 H 0.0877 0.1485 0.0721 0.056 Uiso 1 1 calc R . . C45 C 0.54977(15) 0.28581(15) 0.39407(11) 0.0322(6) Uani 1 1 d . . . H65 H 0.5463 0.2806 0.4372 0.048 Uiso 1 1 calc R . . H66 H 0.5449 0.3456 0.3819 0.048 Uiso 1 1 calc R . . H67 H 0.6046 0.2635 0.3891 0.048 Uiso 1 1 calc R . . C46 C 0.48628(15) 0.14984(14) 0.36873(10) 0.0261(5) Uani 1 1 d . . . H68 H 0.5455 0.1303 0.3717 0.031 Uiso 1 1 calc R . . H69 H 0.4492 0.1198 0.3338 0.031 Uiso 1 1 calc R . . C47 C 0.45984(14) 0.12605(15) 0.42662(10) 0.0291(5) Uani 1 1 d . . . H70 H 0.4131 0.1636 0.4324 0.035 Uiso 1 1 calc R . . H71 H 0.4385 0.0670 0.4234 0.035 Uiso 1 1 calc R . . C48 C 0.50350(17) 0.12283(18) 0.53368(11) 0.0420(7) Uani 1 1 d . . . H72 H 0.4640 0.1683 0.5382 0.063 Uiso 1 1 calc R . . H73 H 0.5535 0.1249 0.5681 0.063 Uiso 1 1 calc R . . H74 H 0.4750 0.0680 0.5336 0.063 Uiso 1 1 calc R . . C49 C 0.36794(16) 0.41339(16) 0.39105(10) 0.0338(6) Uani 1 1 d . . . H75 H 0.4217 0.4121 0.4222 0.051 Uiso 1 1 calc R . . H76 H 0.3347 0.3625 0.3949 0.051 Uiso 1 1 calc R . . H77 H 0.3353 0.4638 0.3972 0.051 Uiso 1 1 calc R . . C50 C 0.43684(14) 0.48795(13) 0.32419(10) 0.0235(5) Uani 1 1 d . . . H78 H 0.4954 0.4801 0.3492 0.028 Uiso 1 1 calc R . . H79 H 0.4127 0.5397 0.3387 0.028 Uiso 1 1 calc R . . C51 C 0.43886(14) 0.49726(13) 0.25789(9) 0.0220(5) Uani 1 1 d . . . H80 H 0.3819 0.5140 0.2337 0.026 Uiso 1 1 calc R . . H81 H 0.4802 0.5417 0.2531 0.026 Uiso 1 1 calc R . . C52 C 0.48569(14) 0.42608(14) 0.17804(9) 0.0234(5) Uani 1 1 d . . . H82 H 0.4390 0.4537 0.1488 0.035 Uiso 1 1 calc R . . H83 H 0.4960 0.3698 0.1626 0.035 Uiso 1 1 calc R . . H84 H 0.5375 0.4604 0.1829 0.035 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 Sr1 0.01337(11) 0.01429(11) 0.01606(9) -0.00056(7) 0.00386(7) -0.00038(8) O1 0.0211(9) 0.0244(8) 0.0281(8) -0.0043(7) 0.0095(7) 0.0018(7) C1 0.0229(13) 0.0141(11) 0.0240(11) 0.0007(8) 0.0074(9) 0.0029(9) Sr2 0.01286(11) 0.01295(10) 0.01579(9) 0.00006(7) 0.00407(7) 0.00006(8) O2 0.0197(8) 0.0170(8) 0.0249(8) 0.0069(6) 0.0049(6) 0.0014(6) C2 0.0322(14) 0.0183(12) 0.0242(11) 0.0012(9) 0.0039(10) 0.0055(10) O3 0.0195(8) 0.0165(8) 0.0239(7) 0.0044(6) 0.0037(6) 0.0005(6) C3 0.0555(18) 0.0193(12) 0.0223(11) 0.0022(9) 0.0140(12) 0.0087(11) O4 0.0231(9) 0.0230(8) 0.0270(8) -0.0031(6) 0.0112(7) 0.0013(7) C4 0.0498(18) 0.0195(12) 0.0414(14) 0.0051(11) 0.0305(13) 0.0027(11) O5 0.0265(10) 0.0319(10) 0.0261(8) 0.0009(7) -0.0030(7) 0.0034(7) C5 0.0295(14) 0.0197(12) 0.0461(14) 0.0021(10) 0.0204(12) -0.0013(10) O6 0.0227(10) 0.1056(18) 0.0265(9) 0.0058(10) 0.0021(8) -0.0005(10) C6 0.0248(13) 0.0160(11) 0.0285(11) 0.0015(9) 0.0105(10) 0.0019(9) O7 0.0264(9) 0.0173(8) 0.0273(8) -0.0011(6) 0.0101(7) -0.0006(7) C7 0.0356(16) 0.0391(16) 0.0388(14) -0.0150(12) -0.0046(12) 0.0065(12) O8 0.0264(9) 0.0241(8) 0.0239(8) -0.0067(6) 0.0092(7) -0.0049(7) C8 0.083(2) 0.0360(17) 0.0625(19) -0.0037(14) 0.0548(18) -0.0015(15) O9 0.0240(9) 0.0201(8) 0.0248(8) -0.0010(6) -0.0020(7) 0.0019(7) C9 0.0212(14) 0.0307(14) 0.0379(13) -0.0018(11) 0.0033(11) -0.0012(10) O10 0.0209(10) 0.0662(13) 0.0220(8) 0.0056(8) 0.0015(7) 0.0016(8) C10 0.0113(11) 0.0177(11) 0.0216(10) 0.0036(8) 0.0010(8) -0.0003(8) O11 0.0285(9) 0.0178(8) 0.0231(7) -0.0027(6) 0.0110(7) -0.0034(7) C11 0.0123(11) 0.0197(11) 0.0228(11) 0.0004(9) 0.0009(9) 0.0012(9) O12 0.0258(9) 0.0159(8) 0.0241(7) -0.0005(6) 0.0110(7) 0.0002(6) C12 0.0195(12) 0.0226(12) 0.0199(10) 0.0041(9) 0.0049(9) -0.0016(9) C13 0.0167(12) 0.0202(12) 0.0260(11) 0.0045(9) 0.0016(9) 0.0000(9) C14 0.0172(12) 0.0180(11) 0.0260(11) -0.0012(9) 0.0032(9) 0.0015(9) C15 0.0114(11) 0.0206(11) 0.0210(11) 0.0009(8) 0.0011(9) 0.0003(9) C16 0.0250(13) 0.0228(12) 0.0257(11) 0.0001(9) 0.0055(10) 0.0002(10) C17 0.0329(15) 0.0217(13) 0.0349(13) 0.0067(10) 0.0083(11) -0.0008(10) C18 0.0272(14) 0.0259(13) 0.0243(11) 0.0024(9) 0.0062(10) 0.0030(10) C19 0.0107(11) 0.0169(11) 0.0232(10) 0.0051(9) 0.0005(8) -0.0020(8) C20 0.0132(12) 0.0207(12) 0.0239(11) 0.0014(9) 0.0006(9) -0.0005(9) C21 0.0146(12) 0.0179(11) 0.0320(12) 0.0003(9) 0.0015(9) -0.0004(9) C22 0.0159(12) 0.0212(12) 0.0328(12) 0.0079(10) 0.0018(10) -0.0018(9) C23 0.0173(12) 0.0279(13) 0.0240(11) 0.0058(9) 0.0046(9) -0.0010(10) C24 0.0130(12) 0.0212(12) 0.0231(11) 0.0038(9) 0.0005(9) -0.0001(9) C25 0.0257(14) 0.0263(13) 0.0271(12) -0.0015(10) 0.0072(10) 0.0028(10) C26 0.0329(15) 0.0263(14) 0.0437(14) 0.0151(11) 0.0091(12) -0.0005(11) C27 0.0287(14) 0.0264(13) 0.0264(11) 0.0008(10) 0.0069(10) 0.0028(10) C28 0.0238(13) 0.0118(10) 0.0213(10) 0.0033(8) 0.0087(9) 0.0036(9) C29 0.0243(13) 0.0177(11) 0.0211(10) 0.0025(8) 0.0044(9) 0.0045(9) C30 0.0345(15) 0.0216(12) 0.0177(10) 0.0029(9) 0.0087(10) 0.0045(10) C31 0.0295(14) 0.0227(12) 0.0284(12) 0.0068(9) 0.0169(10) 0.0051(10) C32 0.0204(13) 0.0203(12) 0.0343(12) 0.0040(9) 0.0108(10) 0.0017(9) C33 0.0222(13) 0.0153(11) 0.0251(11) 0.0027(9) 0.0072(9) 0.0009(9) C34 0.0281(15) 0.0361(15) 0.0311(13) -0.0081(11) 0.0025(11) 0.0018(11) C35 0.0415(17) 0.0403(16) 0.0385(14) -0.0003(12) 0.0254(13) 0.0029(12) C36 0.0239(14) 0.0296(14) 0.0305(12) -0.0021(10) 0.0046(10) 0.0012(10) C37 0.0316(17) 0.0345(17) 0.0506(16) 0.0020(12) -0.0059(13) -0.0011(12) C38 0.0293(15) 0.0272(14) 0.0348(13) -0.0047(10) -0.0041(11) 0.0032(11) C39 0.0214(14) 0.0444(16) 0.0423(15) 0.0097(12) 0.0006(11) -0.0009(12) C40 0.0441(19) 0.108(3) 0.0358(16) 0.0048(17) 0.0175(14) -0.0009(18) C41 0.0251(13) 0.0262(13) 0.0289(12) 0.0022(10) 0.0091(10) -0.0027(10) C42 0.0239(13) 0.0149(11) 0.0392(13) -0.0031(9) 0.0097(11) -0.0021(9) C43 0.0241(13) 0.0209(12) 0.0360(13) -0.0108(10) 0.0067(10) -0.0036(10) C44 0.0479(18) 0.0409(16) 0.0265(12) -0.0054(11) 0.0138(12) -0.0019(13) C45 0.0287(15) 0.0252(14) 0.0383(13) -0.0053(10) -0.0020(11) -0.0001(11) C46 0.0300(14) 0.0202(12) 0.0244(11) -0.0037(9) -0.0016(10) 0.0023(10) C47 0.0223(13) 0.0302(13) 0.0310(12) 0.0034(10) -0.0021(10) 0.0006(10) C48 0.0376(17) 0.061(2) 0.0299(13) 0.0050(13) 0.0138(12) 0.0026(14) C49 0.0451(17) 0.0344(14) 0.0259(12) -0.0014(10) 0.0161(12) -0.0022(12) C50 0.0238(13) 0.0174(11) 0.0293(12) -0.0051(9) 0.0063(10) -0.0025(9) C51 0.0221(13) 0.0165(11) 0.0284(12) -0.0020(9) 0.0079(10) -0.0005(9) C52 0.0248(13) 0.0227(12) 0.0246(11) 0.0009(9) 0.0094(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 Sr1 O1 2.3221(14) . ? Sr1 O2 2.4346(14) . ? Sr1 O3 2.4906(14) . ? Sr1 O5 2.5914(15) . ? Sr1 O8 2.6077(14) . ? Sr1 O7 2.6440(14) . ? Sr1 C19 3.311(2) . ? Sr1 Sr2 3.8899(3) . ? O1 C1 1.318(2) . ? C1 C6 1.410(3) . ? C1 C2 1.417(3) . ? Sr2 O4 2.3181(14) . ? Sr2 O3 2.4334(14) . ? Sr2 O2 2.4904(14) . ? Sr2 O9 2.5956(14) . ? Sr2 O11 2.6056(14) . ? Sr2 O12 2.6482(14) . ? Sr2 C10 3.310(2) . ? O2 C10 1.342(2) . ? C2 C3 1.389(3) . ? C2 C7 1.494(3) . ? O3 C19 1.342(2) . ? C3 C4 1.384(3) . ? C3 H1 0.9500 . ? O4 C28 1.322(2) . ? C4 C5 1.386(3) . ? C4 C8 1.505(3) . ? O5 C37 1.428(3) . ? O5 C38 1.429(3) . ? C5 C6 1.385(3) . ? C5 H2 0.9500 . ? O6 C39 1.407(3) . ? O6 C40 1.420(3) . ? C6 C9 1.502(3) . ? O7 C41 1.432(2) . ? O7 C42 1.434(2) . ? C7 H3 0.9800 . ? C7 H4 0.9800 . ? C7 H5 0.9800 . ? O8 C44 1.424(2) . ? O8 C43 1.435(2) . ? C8 H6 0.9800 . ? C8 H7 0.9800 . ? C8 H8 0.9800 . ? O9 C46 1.430(2) . ? O9 C45 1.430(3) . ? C9 H9 0.9800 . ? C9 H10 0.9800 . ? C9 H11 0.9800 . ? O10 C47 1.411(3) . ? O10 C48 1.414(3) . ? C10 C11 1.407(3) . ? C10 C15 1.414(3) . ? O11 C49 1.425(2) . ? O11 C50 1.433(2) . ? C11 C12 1.389(3) . ? C11 C16 1.505(3) . ? O12 C52 1.430(2) . ? O12 C51 1.431(2) . ? C12 C13 1.383(3) . ? C12 H12 0.9500 . ? C13 C14 1.386(3) . ? C13 C17 1.509(3) . ? C14 C15 1.390(3) . ? C14 H13 0.9500 . ? C15 C18 1.501(3) . ? C16 H14 0.9800 . ? C16 H15 0.9800 . ? C16 H16 0.9800 . ? C17 H17 0.9800 . ? C17 H18 0.9800 . ? C17 H19 0.9800 . ? C18 H20 0.9800 . ? C18 H21 0.9800 . ? C18 H22 0.9800 . ? C19 C24 1.410(3) . ? C19 C20 1.416(3) . ? C20 C21 1.390(3) . ? C20 C25 1.504(3) . ? C21 C22 1.385(3) . ? C21 H23 0.9500 . ? C22 C23 1.382(3) . ? C22 C26 1.509(3) . ? C23 C24 1.388(3) . ? C23 H24 0.9500 . ? C24 C27 1.497(3) . ? C25 H25 0.9800 . ? C25 H26 0.9800 . ? C25 H27 0.9800 . ? C26 H31 0.9800 . ? C26 H32 0.9800 . ? C26 H33 0.9800 . ? C27 H28 0.9800 . ? C27 H29 0.9800 . ? C27 H30 0.9800 . ? C28 C33 1.412(3) . ? C28 C29 1.418(3) . ? C29 C30 1.386(3) . ? C29 C34 1.501(3) . ? C30 C31 1.382(3) . ? C30 H34 0.9500 . ? C31 C32 1.388(3) . ? C31 C35 1.509(3) . ? C32 C33 1.388(3) . ? C32 H35 0.9500 . ? C33 C36 1.504(3) . ? C34 H36 0.9800 . ? C34 H37 0.9800 . ? C34 H38 0.9800 . ? C35 H39 0.9800 . ? C35 H40 0.9800 . ? C35 H41 0.9800 . ? C36 H42 0.9800 . ? C36 H43 0.9800 . ? C36 H44 0.9800 . ? C37 H45 0.9800 . ? C37 H46 0.9800 . ? C37 H47 0.9800 . ? C38 C39 1.500(3) . ? C38 H48 0.9900 . ? C38 H49 0.9900 . ? C39 H50 0.9900 . ? C39 H51 0.9900 . ? C40 H52 0.9800 . ? C40 H53 0.9800 . ? C40 H54 0.9800 . ? C41 H55 0.9800 . ? C41 H56 0.9800 . ? C41 H57 0.9800 . ? C42 C43 1.489(3) . ? C42 H58 0.9900 . ? C42 H59 0.9900 . ? C43 H60 0.9900 . ? C43 H61 0.9900 . ? C44 H62 0.9800 . ? C44 H63 0.9800 . ? C44 H64 0.9800 . ? C45 H65 0.9800 . ? C45 H66 0.9800 . ? C45 H67 0.9800 . ? C46 C47 1.496(3) . ? C46 H68 0.9900 . ? C46 H69 0.9900 . ? C47 H70 0.9900 . ? C47 H71 0.9900 . ? C48 H72 0.9800 . ? C48 H73 0.9800 . ? C48 H74 0.9800 . ? C49 H75 0.9800 . ? C49 H76 0.9800 . ? C49 H77 0.9800 . ? C50 C51 1.494(3) . ? C50 H78 0.9900 . ? C50 H79 0.9900 . ? C51 H80 0.9900 . ? C51 H81 0.9900 . ? C52 H82 0.9800 . ? C52 H83 0.9800 . ? C52 H84 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Sr1 O2 110.95(5) . . ? O1 Sr1 O3 113.83(5) . . ? O2 Sr1 O3 75.62(4) . . ? O1 Sr1 O5 92.52(5) . . ? O2 Sr1 O5 89.05(5) . . ? O3 Sr1 O5 152.78(5) . . ? O1 Sr1 O8 146.00(5) . . ? O2 Sr1 O8 100.83(5) . . ? O3 Sr1 O8 85.00(5) . . ? O5 Sr1 O8 75.81(5) . . ? O1 Sr1 O7 87.66(5) . . ? O2 Sr1 O7 161.34(5) . . ? O3 Sr1 O7 96.06(4) . . ? O5 Sr1 O7 91.53(5) . . ? O8 Sr1 O7 61.38(4) . . ? O1 Sr1 C19 108.74(5) . . ? O2 Sr1 C19 96.76(5) . . ? O3 Sr1 C19 21.30(5) . . ? O5 Sr1 C19 154.01(5) . . ? O8 Sr1 C19 78.22(5) . . ? O7 Sr1 C19 75.07(5) . . ? O1 Sr1 Sr2 118.03(4) . . ? O2 Sr1 Sr2 38.34(3) . . ? O3 Sr1 Sr2 37.30(3) . . ? O5 Sr1 Sr2 124.36(4) . . ? O8 Sr1 Sr2 94.32(3) . . ? O7 Sr1 Sr2 131.63(3) . . ? C19 Sr1 Sr2 58.52(3) . . ? C1 O1 Sr1 158.89(14) . . ? O1 C1 C6 120.67(18) . . ? O1 C1 C2 121.3(2) . . ? C6 C1 C2 118.00(19) . . ? O4 Sr2 O3 109.38(5) . . ? O4 Sr2 O2 113.98(5) . . ? O3 Sr2 O2 75.65(4) . . ? O4 Sr2 O9 92.42(5) . . ? O3 Sr2 O9 88.13(5) . . ? O2 Sr2 O9 152.29(5) . . ? O4 Sr2 O11 143.96(5) . . ? O3 Sr2 O11 104.16(4) . . ? O2 Sr2 O11 86.56(5) . . ? O9 Sr2 O11 75.65(5) . . ? O4 Sr2 O12 86.15(5) . . ? O3 Sr2 O12 164.13(4) . . ? O2 Sr2 O12 95.37(4) . . ? O9 Sr2 O12 94.64(5) . . ? O11 Sr2 O12 61.70(4) . . ? O4 Sr2 C10 110.20(5) . . ? O3 Sr2 C10 96.70(5) . . ? O2 Sr2 C10 21.32(5) . . ? O9 Sr2 C10 153.53(5) . . ? O11 Sr2 C10 77.94(5) . . ? O12 Sr2 C10 74.10(5) . . ? O4 Sr2 Sr1 118.70(4) . . ? O3 Sr2 Sr1 38.34(3) . . ? O2 Sr2 Sr1 37.33(3) . . ? O9 Sr2 Sr1 122.74(3) . . ? O11 Sr2 Sr1 95.81(3) . . ? O12 Sr2 Sr1 131.19(3) . . ? C10 Sr2 Sr1 58.39(3) . . ? C10 O2 Sr1 138.11(12) . . ? C10 O2 Sr2 116.24(12) . . ? Sr1 O2 Sr2 104.33(5) . . ? C3 C2 C1 119.1(2) . . ? C3 C2 C7 121.0(2) . . ? C1 C2 C7 119.8(2) . . ? C19 O3 Sr2 138.92(12) . . ? C19 O3 Sr1 116.30(12) . . ? Sr2 O3 Sr1 104.36(5) . . ? C4 C3 C2 123.4(2) . . ? C4 C3 H1 118.3 . . ? C2 C3 H1 118.3 . . ? C28 O4 Sr2 157.76(13) . . ? C3 C4 C5 116.6(2) . . ? C3 C4 C8 121.8(2) . . ? C5 C4 C8 121.6(3) . . ? C37 O5 C38 114.50(17) . . ? C37 O5 Sr1 124.99(14) . . ? C38 O5 Sr1 120.30(13) . . ? C6 C5 C4 122.7(2) . . ? C6 C5 H2 118.6 . . ? C4 C5 H2 118.6 . . ? C39 O6 C40 112.11(19) . . ? C5 C6 C1 120.1(2) . . ? C5 C6 C9 121.3(2) . . ? C1 C6 C9 118.65(19) . . ? C41 O7 C42 111.56(16) . . ? C41 O7 Sr1 117.24(12) . . ? C42 O7 Sr1 115.86(11) . . ? C2 C7 H3 109.5 . . ? C2 C7 H4 109.5 . . ? H3 C7 H4 109.5 . . ? C2 C7 H5 109.5 . . ? H3 C7 H5 109.5 . . ? H4 C7 H5 109.5 . . ? C44 O8 C43 112.11(16) . . ? C44 O8 Sr1 122.51(13) . . ? C43 O8 Sr1 121.65(11) . . ? C4 C8 H6 109.5 . . ? C4 C8 H7 109.5 . . ? H6 C8 H7 109.5 . . ? C4 C8 H8 109.5 . . ? H6 C8 H8 109.5 . . ? H7 C8 H8 109.5 . . ? C46 O9 C45 113.39(16) . . ? C46 O9 Sr2 116.25(12) . . ? C45 O9 Sr2 129.33(13) . . ? C6 C9 H9 109.5 . . ? C6 C9 H10 109.5 . . ? H9 C9 H10 109.5 . . ? C6 C9 H11 109.5 . . ? H9 C9 H11 109.5 . . ? H10 C9 H11 109.5 . . ? C47 O10 C48 111.33(17) . . ? O2 C10 C11 120.62(18) . . ? O2 C10 C15 120.79(18) . . ? C11 C10 C15 118.58(19) . . ? O2 C10 Sr2 42.44(9) . . ? C11 C10 Sr2 102.80(13) . . ? C15 C10 Sr2 121.50(13) . . ? C49 O11 C50 111.57(16) . . ? C49 O11 Sr2 124.08(13) . . ? C50 O11 Sr2 121.41(11) . . ? C12 C11 C10 119.83(19) . . ? C12 C11 C16 120.04(19) . . ? C10 C11 C16 120.12(19) . . ? C52 O12 C51 111.77(15) . . ? C52 O12 Sr2 119.97(12) . . ? C51 O12 Sr2 114.98(11) . . ? C13 C12 C11 122.2(2) . . ? C13 C12 H12 118.9 . . ? C11 C12 H12 118.9 . . ? C12 C13 C14 117.59(19) . . ? C12 C13 C17 120.68(19) . . ? C14 C13 C17 121.7(2) . . ? C13 C14 C15 122.5(2) . . ? C13 C14 H13 118.8 . . ? C15 C14 H13 118.8 . . ? C14 C15 C10 119.26(19) . . ? C14 C15 C18 120.80(19) . . ? C10 C15 C18 119.93(18) . . ? C11 C16 H14 109.5 . . ? C11 C16 H15 109.5 . . ? H14 C16 H15 109.5 . . ? C11 C16 H16 109.5 . . ? H14 C16 H16 109.5 . . ? H15 C16 H16 109.5 . . ? C13 C17 H17 109.5 . . ? C13 C17 H18 109.5 . . ? H17 C17 H18 109.5 . . ? C13 C17 H19 109.5 . . ? H17 C17 H19 109.5 . . ? H18 C17 H19 109.5 . . ? C15 C18 H20 109.5 . . ? C15 C18 H21 109.5 . . ? H20 C18 H21 109.5 . . ? C15 C18 H22 109.5 . . ? H20 C18 H22 109.5 . . ? H21 C18 H22 109.5 . . ? O3 C19 C24 120.33(19) . . ? O3 C19 C20 121.11(18) . . ? C24 C19 C20 118.55(19) . . ? O3 C19 Sr1 42.40(9) . . ? C24 C19 Sr1 102.12(13) . . ? C20 C19 Sr1 122.69(13) . . ? C21 C20 C19 118.97(19) . . ? C21 C20 C25 121.2(2) . . ? C19 C20 C25 119.78(19) . . ? C22 C21 C20 123.1(2) . . ? C22 C21 H23 118.5 . . ? C20 C21 H23 118.5 . . ? C23 C22 C21 117.0(2) . . ? C23 C22 C26 120.7(2) . . ? C21 C22 C26 122.2(2) . . ? C22 C23 C24 122.7(2) . . ? C22 C23 H24 118.6 . . ? C24 C23 H24 118.6 . . ? C23 C24 C19 119.6(2) . . ? C23 C24 C27 120.34(19) . . ? C19 C24 C27 120.02(19) . . ? C20 C25 H25 109.5 . . ? C20 C25 H26 109.5 . . ? H25 C25 H26 109.5 . . ? C20 C25 H27 109.5 . . ? H25 C25 H27 109.5 . . ? H26 C25 H27 109.5 . . ? C22 C26 H31 109.5 . . ? C22 C26 H32 109.5 . . ? H31 C26 H32 109.5 . . ? C22 C26 H33 109.5 . . ? H31 C26 H33 109.5 . . ? H32 C26 H33 109.5 . . ? C24 C27 H28 109.5 . . ? C24 C27 H29 109.5 . . ? H28 C27 H29 109.5 . . ? C24 C27 H30 109.5 . . ? H28 C27 H30 109.5 . . ? H29 C27 H30 109.5 . . ? O4 C28 C33 120.53(18) . . ? O4 C28 C29 121.4(2) . . ? C33 C28 C29 118.05(18) . . ? C30 C29 C28 119.4(2) . . ? C30 C29 C34 121.17(19) . . ? C28 C29 C34 119.38(19) . . ? C31 C30 C29 123.1(2) . . ? C31 C30 H34 118.5 . . ? C29 C30 H34 118.5 . . ? C30 C31 C32 117.07(19) . . ? C30 C31 C35 122.0(2) . . ? C32 C31 C35 121.0(2) . . ? C33 C32 C31 122.4(2) . . ? C33 C32 H35 118.8 . . ? C31 C32 H35 118.8 . . ? C32 C33 C28 119.9(2) . . ? C32 C33 C36 121.0(2) . . ? C28 C33 C36 119.10(19) . . ? C29 C34 H36 109.5 . . ? C29 C34 H37 109.5 . . ? H36 C34 H37 109.5 . . ? C29 C34 H38 109.5 . . ? H36 C34 H38 109.5 . . ? H37 C34 H38 109.5 . . ? C31 C35 H39 109.5 . . ? C31 C35 H40 109.5 . . ? H39 C35 H40 109.5 . . ? C31 C35 H41 109.5 . . ? H39 C35 H41 109.5 . . ? H40 C35 H41 109.5 . . ? C33 C36 H42 109.5 . . ? C33 C36 H43 109.5 . . ? H42 C36 H43 109.5 . . ? C33 C36 H44 109.5 . . ? H42 C36 H44 109.5 . . ? H43 C36 H44 109.5 . . ? O5 C37 H45 109.5 . . ? O5 C37 H46 109.5 . . ? H45 C37 H46 109.5 . . ? O5 C37 H47 109.5 . . ? H45 C37 H47 109.5 . . ? H46 C37 H47 109.5 . . ? O5 C38 C39 113.2(2) . . ? O5 C38 H48 108.9 . . ? C39 C38 H48 108.9 . . ? O5 C38 H49 108.9 . . ? C39 C38 H49 108.9 . . ? H48 C38 H49 107.8 . . ? O6 C39 C38 109.27(19) . . ? O6 C39 H50 109.8 . . ? C38 C39 H50 109.8 . . ? O6 C39 H51 109.8 . . ? C38 C39 H51 109.8 . . ? H50 C39 H51 108.3 . . ? O6 C40 H52 109.5 . . ? O6 C40 H53 109.5 . . ? H52 C40 H53 109.5 . . ? O6 C40 H54 109.5 . . ? H52 C40 H54 109.5 . . ? H53 C40 H54 109.5 . . ? O7 C41 H55 109.5 . . ? O7 C41 H56 109.5 . . ? H55 C41 H56 109.5 . . ? O7 C41 H57 109.5 . . ? H55 C41 H57 109.5 . . ? H56 C41 H57 109.5 . . ? O7 C42 C43 108.35(17) . . ? O7 C42 H58 110.0 . . ? C43 C42 H58 110.0 . . ? O7 C42 H59 110.0 . . ? C43 C42 H59 110.0 . . ? H58 C42 H59 108.4 . . ? O8 C43 C42 108.50(17) . . ? O8 C43 H60 110.0 . . ? C42 C43 H60 110.0 . . ? O8 C43 H61 110.0 . . ? C42 C43 H61 110.0 . . ? H60 C43 H61 108.4 . . ? O8 C44 H62 109.5 . . ? O8 C44 H63 109.5 . . ? H62 C44 H63 109.5 . . ? O8 C44 H64 109.5 . . ? H62 C44 H64 109.5 . . ? H63 C44 H64 109.5 . . ? O9 C45 H65 109.5 . . ? O9 C45 H66 109.5 . . ? H65 C45 H66 109.5 . . ? O9 C45 H67 109.5 . . ? H65 C45 H67 109.5 . . ? H66 C45 H67 109.5 . . ? O9 C46 C47 113.97(18) . . ? O9 C46 H68 108.8 . . ? C47 C46 H68 108.8 . . ? O9 C46 H69 108.8 . . ? C47 C46 H69 108.8 . . ? H68 C46 H69 107.7 . . ? O10 C47 C46 110.29(18) . . ? O10 C47 H70 109.6 . . ? C46 C47 H70 109.6 . . ? O10 C47 H71 109.6 . . ? C46 C47 H71 109.6 . . ? H70 C47 H71 108.1 . . ? O10 C48 H72 109.5 . . ? O10 C48 H73 109.5 . . ? H72 C48 H73 109.5 . . ? O10 C48 H74 109.5 . . ? H72 C48 H74 109.5 . . ? H73 C48 H74 109.5 . . ? O11 C49 H75 109.5 . . ? O11 C49 H76 109.5 . . ? H75 C49 H76 109.5 . . ? O11 C49 H77 109.5 . . ? H75 C49 H77 109.5 . . ? H76 C49 H77 109.5 . . ? O11 C50 C51 109.18(17) . . ? O11 C50 H78 109.8 . . ? C51 C50 H78 109.8 . . ? O11 C50 H79 109.8 . . ? C51 C50 H79 109.8 . . ? H78 C50 H79 108.3 . . ? O12 C51 C50 108.46(17) . . ? O12 C51 H80 110.0 . . ? C50 C51 H80 110.0 . . ? O12 C51 H81 110.0 . . ? C50 C51 H81 110.0 . . ? H80 C51 H81 108.4 . . ? O12 C52 H82 109.5 . . ? O12 C52 H83 109.5 . . ? H82 C52 H83 109.5 . . ? O12 C52 H84 109.5 . . ? H82 C52 H84 109.5 . . ? H83 C52 H84 109.5 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.524 _refine_diff_density_min -0.492 _refine_diff_density_rms 0.067 data_c:\monoc _database_code_depnum_ccdc_archive 'CCDC 716848' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C66 H110 O18 Sr5, 2(C4 H10 O2)' _chemical_formula_sum 'C74 H130 O22 Sr5' _chemical_formula_weight 1809.88 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sr Sr -1.5307 3.2498 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 18.279(4) _cell_length_b 17.256(4) _cell_length_c 28.189(6) _cell_angle_alpha 90.00 _cell_angle_beta 104.46(3) _cell_angle_gamma 90.00 _cell_volume 8610(3) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.396 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3760 _exptl_absorpt_coefficient_mu 3.143 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.6500 _exptl_absorpt_correction_T_max 0.7440 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker X8 Apex II CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 40931 _diffrn_reflns_av_R_equivalents 0.0992 _diffrn_reflns_av_sigmaI/netI 0.1132 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 1.65 _diffrn_reflns_theta_max 27.50 _reflns_number_total 9870 _reflns_number_gt 5839 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART (Bruker)' _computing_cell_refinement 'Bruker SMART (Bruker)' _computing_data_reduction 'Bruker SAINT (Bruker)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 1999)' _computing_publication_material 'CIFTAB (Sheldrick, 1997)' _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^)+(0.0429P)^2^+58.8058P] 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 ? _refine_ls_extinction_coef ? _refine_ls_number_reflns 9870 _refine_ls_number_parameters 476 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1404 _refine_ls_R_factor_gt 0.0679 _refine_ls_wR_factor_ref 0.1446 _refine_ls_wR_factor_gt 0.1238 _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 Sr1 Sr 0.14327(3) 0.34234(3) 0.259740(18) 0.02392(14) Uani 1 1 d . . . O1 O 0.0000 0.3591(4) 0.2500 0.0365(14) Uani 1 2 d S . . C1 C 0.0000 0.4524(9) 0.2500 0.115(5) Uani 1 2 d S . . H1 H -0.0267 0.4713 0.2175 0.173 Uiso 0.50 1 calc PR . . H2 H 0.0522 0.4713 0.2580 0.173 Uiso 0.50 1 calc PR . . H3 H -0.0255 0.4713 0.2745 0.173 Uiso 0.50 1 calc PR . . Sr2 Sr 0.0000 0.18238(4) 0.2500 0.0289(2) Uani 1 2 d S . . O2 O 0.0750(2) 0.2428(2) 0.19881(13) 0.0294(9) Uani 1 1 d . . . C2 C 0.1051(4) 0.1824(4) 0.1759(2) 0.0471(17) Uani 1 1 d . . . H4 H 0.0923 0.1324 0.1882 0.071 Uiso 1 1 calc R . . H5 H 0.1601 0.1878 0.1831 0.071 Uiso 1 1 calc R . . H6 H 0.0838 0.1850 0.1404 0.071 Uiso 1 1 calc R . . Sr3 Sr 0.02211(3) 0.34119(3) 0.343820(18) 0.02790(15) Uani 1 1 d . . . O3 O 0.10029(19) 0.2432(2) 0.31308(13) 0.0279(9) Uani 1 1 d . . . C3 C 0.1339(5) 0.1905(4) 0.3495(3) 0.063(2) Uani 1 1 d . . . H7 H 0.1155 0.1999 0.3788 0.095 Uiso 1 1 calc R . . H8 H 0.1889 0.1971 0.3575 0.095 Uiso 1 1 calc R . . H9 H 0.1209 0.1376 0.3377 0.095 Uiso 1 1 calc R . . O4 O 0.1369(2) 0.4149(2) 0.33698(14) 0.0373(10) Uani 1 1 d . . . C4 C 0.1906(3) 0.4576(4) 0.3640(2) 0.0358(15) Uani 1 1 d . . . O5 O -0.1029(2) 0.4143(2) 0.31980(14) 0.0342(10) Uani 1 1 d . . . C5 C 0.1986(5) 0.5368(4) 0.3538(3) 0.059(2) Uani 1 1 d . . . O6 O 0.0000 0.0484(3) 0.2500 0.0491(17) Uani 1 2 d S . . C6 C 0.2580(7) 0.5801(5) 0.3835(5) 0.100(4) Uani 1 1 d . . . H10 H 0.2637 0.6333 0.3765 0.120 Uiso 1 1 calc R . . O7 O 0.2654(2) 0.2611(2) 0.28961(15) 0.0390(10) Uani 1 1 d . . . C7 C 0.3081(8) 0.5457(9) 0.4227(5) 0.130(6) Uani 1 1 d . . . O8 O 0.2751(2) 0.4114(2) 0.26443(16) 0.0389(10) Uani 1 1 d . . . C8 C 0.2991(5) 0.4716(7) 0.4332(3) 0.093(3) Uani 1 1 d . . . H11 H 0.3333 0.4489 0.4607 0.112 Uiso 1 1 calc R . . O9 O 0.0400(3) 0.4148(3) 0.42905(16) 0.0585(14) Uani 1 1 d . . . C9 C 0.2416(4) 0.4264(4) 0.4053(2) 0.0477(18) Uani 1 1 d . . . O10 O 0.0162(3) 0.2588(3) 0.42374(16) 0.0554(13) Uani 1 1 d . . . C10 C 0.1460(5) 0.5734(5) 0.3119(4) 0.104(4) Uani 1 1 d . . . H12 H 0.0943 0.5685 0.3156 0.156 Uiso 1 1 calc R . . H13 H 0.1498 0.5478 0.2816 0.156 Uiso 1 1 calc R . . H14 H 0.1588 0.6284 0.3106 0.156 Uiso 1 1 calc R . . O11 O 0.4616(5) 0.6702(6) 0.5622(3) 0.134(3) Uani 1 1 d . . . C11 C 0.3736(9) 0.5962(10) 0.4544(5) 0.233(10) Uani 1 1 d . . . H15 H 0.4219 0.5796 0.4485 0.350 Uiso 1 1 calc R . . H16 H 0.3752 0.5897 0.4891 0.350 Uiso 1 1 calc R . . H17 H 0.3648 0.6508 0.4453 0.350 Uiso 1 1 calc R . . O12 O 0.3794(7) 0.8084(5) 0.5275(3) 0.140(4) Uani 1 1 d . . . C12 C 0.2352(4) 0.3434(5) 0.4179(3) 0.071(2) Uani 1 1 d . . . H18 H 0.1875 0.3351 0.4271 0.106 Uiso 1 1 calc R . . H19 H 0.2775 0.3293 0.4454 0.106 Uiso 1 1 calc R . . H20 H 0.2362 0.3111 0.3895 0.106 Uiso 1 1 calc R . . C13 C -0.1335(3) 0.4552(3) 0.3503(2) 0.0332(14) Uani 1 1 d . . . C14 C -0.1927(4) 0.4246(4) 0.3693(2) 0.0435(16) Uani 1 1 d . . . C15 C -0.2220(4) 0.4695(5) 0.4010(2) 0.057(2) Uani 1 1 d . . . H21 H -0.2616 0.4484 0.4134 0.068 Uiso 1 1 calc R . . C16 C -0.1967(4) 0.5428(5) 0.4155(2) 0.054(2) Uani 1 1 d . . . C17 C -0.1408(4) 0.5722(4) 0.3964(2) 0.0521(19) Uani 1 1 d . . . H22 H -0.1228 0.6230 0.4057 0.062 Uiso 1 1 calc R . . C18 C -0.1092(4) 0.5311(3) 0.3641(2) 0.0383(15) Uani 1 1 d . . . C19 C -0.2239(4) 0.3446(4) 0.3531(3) 0.067(2) Uani 1 1 d . . . H23 H -0.2512 0.3247 0.3764 0.101 Uiso 1 1 calc R . . H24 H -0.1822 0.3095 0.3521 0.101 Uiso 1 1 calc R . . H25 H -0.2585 0.3480 0.3205 0.101 Uiso 1 1 calc R . . C20 C -0.2312(5) 0.5900(5) 0.4501(3) 0.086(3) Uani 1 1 d . . . H26 H -0.2122 0.6433 0.4517 0.129 Uiso 1 1 calc R . . H27 H -0.2171 0.5669 0.4829 0.129 Uiso 1 1 calc R . . H28 H -0.2863 0.5902 0.4381 0.129 Uiso 1 1 calc R . . C21 C -0.0501(4) 0.5665(4) 0.3428(2) 0.0531(19) Uani 1 1 d . . . H29 H -0.0387 0.6190 0.3560 0.080 Uiso 1 1 calc R . . H30 H -0.0685 0.5691 0.3071 0.080 Uiso 1 1 calc R . . H31 H -0.0042 0.5348 0.3515 0.080 Uiso 1 1 calc R . . C22 C 0.0000 -0.0277(5) 0.2500 0.039(2) Uani 1 2 d S . . C23 C 0.0386(3) -0.0699(4) 0.2920(2) 0.0405(16) Uani 1 1 d . . . C24 C 0.0378(3) -0.1505(4) 0.2900(3) 0.0478(18) Uani 1 1 d . . . H32 H 0.0648 -0.1783 0.3180 0.057 Uiso 1 1 calc R . . C25 C 0.0000 -0.1920(5) 0.2500 0.044(2) Uani 1 2 d S . . C26 C 0.0780(4) -0.0268(5) 0.3372(3) 0.066(2) Uani 1 1 d . . . H33 H 0.1213 0.0014 0.3311 0.099 Uiso 1 1 calc R . . H34 H 0.0956 -0.0636 0.3641 0.099 Uiso 1 1 calc R . . H35 H 0.0428 0.0101 0.3461 0.099 Uiso 1 1 calc R . . C27 C 0.0000 -0.2801(5) 0.2500 0.081(4) Uani 1 2 d S . . H36 H 0.0418 -0.2991 0.2371 0.121 Uiso 0.50 1 calc PR . . H37 H -0.0480 -0.2991 0.2293 0.121 Uiso 0.50 1 calc PR . . H38 H 0.0062 -0.2991 0.2835 0.121 Uiso 0.50 1 calc PR . . C28 C 0.2635(4) 0.1796(4) 0.2817(3) 0.058(2) Uani 1 1 d . . . H39 H 0.2779 0.1683 0.2512 0.087 Uiso 1 1 calc R . . H40 H 0.2123 0.1603 0.2793 0.087 Uiso 1 1 calc R . . H41 H 0.2989 0.1541 0.3091 0.087 Uiso 1 1 calc R . . C29 C 0.3375(3) 0.2934(4) 0.2905(3) 0.0470(18) Uani 1 1 d . . . H42 H 0.3497 0.2846 0.2587 0.056 Uiso 1 1 calc R . . H43 H 0.3769 0.2682 0.3165 0.056 Uiso 1 1 calc R . . C30 C 0.3356(3) 0.3779(4) 0.3003(3) 0.0505(18) Uani 1 1 d . . . H44 H 0.3281 0.3868 0.3335 0.061 Uiso 1 1 calc R . . H45 H 0.3841 0.4021 0.2987 0.061 Uiso 1 1 calc R . . C31 C 0.2869(4) 0.4917(3) 0.2559(3) 0.0475(17) Uani 1 1 d . . . H46 H 0.2904 0.5210 0.2862 0.071 Uiso 1 1 calc R . . H47 H 0.2444 0.5113 0.2302 0.071 Uiso 1 1 calc R . . H48 H 0.3339 0.4978 0.2455 0.071 Uiso 1 1 calc R . . C32 C 0.0707(4) 0.4866(4) 0.4461(2) 0.0560(19) Uani 1 1 d . . . H49 H 0.0298 0.5243 0.4438 0.084 Uiso 1 1 calc R . . H50 H 0.1044 0.5042 0.4262 0.084 Uiso 1 1 calc R . . H51 H 0.0993 0.4817 0.4803 0.084 Uiso 1 1 calc R . . C33 C -0.0034(5) 0.3848(5) 0.4603(3) 0.073(2) Uani 1 1 d . . . H52 H -0.0422 0.4229 0.4638 0.088 Uiso 1 1 calc R . . H53 H 0.0296 0.3739 0.4932 0.088 Uiso 1 1 calc R . . C34 C -0.0392(5) 0.3139(5) 0.4383(3) 0.084(3) Uani 1 1 d . . . H54 H -0.0798 0.3270 0.4089 0.101 Uiso 1 1 calc R . . H55 H -0.0629 0.2875 0.4619 0.101 Uiso 1 1 calc R . . C35 C 0.0593(6) 0.2316(7) 0.4660(3) 0.110(4) Uani 1 1 d . . . H56 H 0.0982 0.2698 0.4803 0.166 Uiso 1 1 calc R . . H57 H 0.0834 0.1832 0.4599 0.166 Uiso 1 1 calc R . . H58 H 0.0277 0.2217 0.4888 0.166 Uiso 1 1 calc R . . C36 C 0.5253(7) 0.6228(10) 0.5758(5) 0.186(8) Uani 1 1 d . . . H59 H 0.5691 0.6499 0.5696 0.279 Uiso 1 1 calc R . . H60 H 0.5166 0.5748 0.5566 0.279 Uiso 1 1 calc R . . H61 H 0.5351 0.6103 0.6108 0.279 Uiso 1 1 calc R . . C37 C 0.4649(9) 0.7428(9) 0.5864(4) 0.148(7) Uani 1 1 d . . . H62 H 0.5033 0.7759 0.5770 0.177 Uiso 1 1 calc R . . H63 H 0.4810 0.7345 0.6223 0.177 Uiso 1 1 calc R . . C38 C 0.3915(8) 0.7830(9) 0.5741(4) 0.137(6) Uani 1 1 d . . . H64 H 0.3507 0.7471 0.5772 0.164 Uiso 1 1 calc R . . H65 H 0.3922 0.8273 0.5965 0.164 Uiso 1 1 calc R . . C39 C 0.3091(10) 0.8467(9) 0.5106(6) 0.173(7) Uani 1 1 d . . . H66 H 0.2680 0.8088 0.5066 0.259 Uiso 1 1 calc R . . H67 H 0.3071 0.8716 0.4791 0.259 Uiso 1 1 calc R . . H68 H 0.3035 0.8860 0.5346 0.259 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 Sr1 0.0204(3) 0.0285(3) 0.0243(3) 0.0019(2) 0.0083(2) 0.0014(2) O1 0.016(3) 0.074(4) 0.020(3) 0.000 0.006(2) 0.000 C1 0.097(11) 0.158(16) 0.099(12) 0.000 0.037(10) 0.000 Sr2 0.0295(4) 0.0269(4) 0.0310(4) 0.000 0.0089(3) 0.000 O2 0.027(2) 0.034(2) 0.027(2) -0.0037(17) 0.0068(17) 0.0020(17) C2 0.056(4) 0.049(4) 0.035(4) -0.001(3) 0.010(3) 0.014(3) Sr3 0.0241(3) 0.0397(3) 0.0217(3) -0.0047(2) 0.0090(2) -0.0038(3) O3 0.025(2) 0.033(2) 0.026(2) 0.0047(17) 0.0066(17) 0.0032(17) C3 0.112(7) 0.041(4) 0.037(4) 0.004(3) 0.019(4) 0.006(4) O4 0.034(2) 0.048(3) 0.030(2) -0.005(2) 0.0086(19) -0.007(2) C4 0.038(4) 0.040(4) 0.037(4) -0.012(3) 0.024(3) -0.009(3) O5 0.037(2) 0.038(2) 0.032(2) -0.0036(18) 0.0158(19) -0.0031(19) C5 0.074(5) 0.050(5) 0.073(6) -0.001(4) 0.056(5) -0.002(4) O6 0.052(4) 0.031(4) 0.073(5) 0.000 0.031(4) 0.000 C6 0.143(11) 0.056(6) 0.140(11) -0.030(7) 0.110(9) -0.051(7) O7 0.029(2) 0.042(3) 0.048(3) 0.005(2) 0.012(2) 0.0106(19) C7 0.157(13) 0.167(13) 0.085(9) -0.072(9) 0.068(9) -0.113(11) O8 0.026(2) 0.043(3) 0.050(3) 0.004(2) 0.013(2) -0.0068(19) C8 0.079(6) 0.160(10) 0.041(5) -0.019(6) 0.015(4) -0.075(7) O9 0.063(3) 0.086(4) 0.035(3) -0.027(3) 0.030(2) -0.025(3) C9 0.036(4) 0.075(5) 0.035(4) -0.011(4) 0.015(3) -0.016(4) O10 0.054(3) 0.084(4) 0.030(3) 0.012(2) 0.013(2) -0.001(3) C10 0.089(7) 0.078(6) 0.178(11) 0.058(7) 0.096(8) 0.025(6) O11 0.123(7) 0.167(8) 0.085(6) 0.043(6) -0.025(5) -0.047(6) C11 0.252(18) 0.32(2) 0.145(13) -0.117(14) 0.082(12) -0.246(18) O12 0.277(13) 0.108(7) 0.063(6) -0.009(4) 0.093(7) -0.044(7) C12 0.059(5) 0.092(6) 0.059(5) 0.026(5) 0.011(4) 0.006(5) C13 0.034(3) 0.039(4) 0.023(3) -0.002(3) 0.001(3) 0.006(3) C14 0.044(4) 0.055(4) 0.035(4) 0.002(3) 0.017(3) 0.004(3) C15 0.047(4) 0.095(6) 0.033(4) 0.004(4) 0.017(3) 0.015(4) C16 0.061(5) 0.072(5) 0.024(4) 0.005(4) 0.001(3) 0.042(4) C17 0.076(5) 0.044(4) 0.030(4) -0.001(3) 0.001(4) 0.018(4) C18 0.046(4) 0.039(4) 0.026(3) 0.002(3) 0.001(3) 0.010(3) C19 0.071(5) 0.076(6) 0.068(6) 0.000(4) 0.042(5) -0.025(5) C20 0.099(7) 0.114(7) 0.045(5) -0.003(5) 0.018(5) 0.069(6) C21 0.067(5) 0.048(4) 0.038(4) -0.005(3) 0.002(4) -0.011(4) C22 0.030(5) 0.031(5) 0.063(7) 0.000 0.024(5) 0.000 C23 0.026(3) 0.047(4) 0.052(4) 0.003(3) 0.016(3) -0.007(3) C24 0.032(4) 0.049(4) 0.070(5) 0.026(4) 0.027(3) 0.006(3) C25 0.041(5) 0.028(5) 0.071(7) 0.000 0.031(5) 0.000 C26 0.059(5) 0.076(6) 0.059(5) 0.001(4) 0.008(4) -0.020(4) C27 0.080(8) 0.034(6) 0.157(13) 0.000 0.086(9) 0.000 C28 0.060(5) 0.042(4) 0.071(6) 0.006(4) 0.012(4) 0.020(4) C29 0.027(3) 0.063(5) 0.054(5) 0.017(4) 0.014(3) 0.015(3) C30 0.025(3) 0.073(5) 0.054(5) 0.005(4) 0.010(3) -0.002(3) C31 0.043(4) 0.036(4) 0.069(5) -0.006(3) 0.024(4) -0.003(3) C32 0.057(5) 0.074(5) 0.031(4) -0.014(4) 0.002(3) 0.009(4) C33 0.086(6) 0.102(7) 0.041(5) -0.025(5) 0.035(4) -0.025(5) C34 0.096(7) 0.105(7) 0.064(6) 0.013(5) 0.044(5) 0.006(6) C35 0.096(7) 0.165(10) 0.059(6) 0.054(7) 0.000(5) -0.041(7) C36 0.097(9) 0.278(19) 0.146(13) 0.132(14) -0.039(9) -0.031(11) C37 0.221(17) 0.180(15) 0.042(6) -0.035(8) 0.032(9) -0.129(14) C38 0.150(12) 0.205(15) 0.062(8) -0.017(9) 0.039(9) -0.073(12) C39 0.28(2) 0.133(14) 0.116(13) 0.002(10) 0.074(15) -0.016(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sr1 O5 2.508(4) 2 ? Sr1 O2 2.527(4) . ? Sr1 O3 2.529(4) . ? Sr1 O4 2.539(4) . ? Sr1 O1 2.5804(10) . ? Sr1 O7 2.592(4) . ? Sr1 O8 2.662(4) . ? O1 C1 1.610(16) . ? O1 Sr1 2.5804(10) 2 ? O1 Sr3 2.5921(11) 2 ? O1 Sr3 2.5921(11) . ? O1 Sr2 3.049(6) . ? C1 H1 0.9800 . ? C1 H2 0.9800 . ? C1 H3 0.9800 . ? Sr2 O6 2.312(6) . ? Sr2 O3 2.448(4) . ? Sr2 O3 2.448(4) 2 ? Sr2 O2 2.457(4) 2 ? Sr2 O2 2.457(4) . ? Sr2 Sr3 3.7595(9) 2 ? Sr2 Sr1 3.7675(9) 2 ? O2 C2 1.408(7) . ? O2 Sr3 2.532(4) 2 ? C2 H4 0.9800 . ? C2 H5 0.9800 . ? C2 H6 0.9800 . ? Sr3 O4 2.502(4) . ? Sr3 O3 2.505(4) . ? Sr3 O2 2.532(4) 2 ? Sr3 O5 2.550(4) . ? Sr3 O9 2.665(4) . ? Sr3 O10 2.689(4) . ? Sr3 Sr1 3.6407(15) 2 ? O3 C3 1.392(7) . ? C3 H7 0.9800 . ? C3 H8 0.9800 . ? C3 H9 0.9800 . ? O4 C4 1.309(7) . ? C4 C9 1.404(9) . ? C4 C5 1.413(9) . ? O5 C13 1.337(6) . ? O5 Sr1 2.508(4) 2 ? C5 C6 1.408(13) . ? C5 C10 1.466(12) . ? O6 C22 1.314(10) . ? C6 C7 1.380(17) . ? C6 H10 0.9500 . ? O7 C28 1.423(7) . ? O7 C29 1.424(7) . ? C7 C8 1.332(16) . ? C7 C11 1.567(14) . ? O8 C30 1.422(7) . ? O8 C31 1.431(7) . ? C8 C9 1.385(10) . ? C8 H11 0.9500 . ? O9 C32 1.394(8) . ? O9 C33 1.422(8) . ? C9 C12 1.488(10) . ? O10 C35 1.339(9) . ? O10 C34 1.520(9) . ? C10 H12 0.9800 . ? C10 H13 0.9800 . ? C10 H14 0.9800 . ? O11 C36 1.397(15) . ? O11 C37 1.421(14) . ? C11 H15 0.9800 . ? C11 H16 0.9800 . ? C11 H17 0.9800 . ? O12 C38 1.349(13) . ? O12 C39 1.417(16) . ? C12 H18 0.9800 . ? C12 H19 0.9800 . ? C12 H20 0.9800 . ? C13 C18 1.407(8) . ? C13 C14 1.423(8) . ? C14 C15 1.389(9) . ? C14 C19 1.520(9) . ? C15 C16 1.372(10) . ? C15 H21 0.9500 . ? C16 C17 1.366(10) . ? C16 C20 1.523(9) . ? C17 C18 1.391(9) . ? C17 H22 0.9500 . ? C18 C21 1.490(9) . ? C19 H23 0.9800 . ? C19 H24 0.9800 . ? C19 H25 0.9800 . ? C20 H26 0.9800 . ? C20 H27 0.9800 . ? C20 H28 0.9800 . ? C21 H29 0.9800 . ? C21 H30 0.9800 . ? C21 H31 0.9800 . ? C22 C23 1.418(7) 2 ? C22 C23 1.418(7) . ? C23 C24 1.392(9) . ? C23 C26 1.497(9) . ? C24 C25 1.368(8) . ? C24 H32 0.9500 . ? C25 C24 1.368(8) 2 ? C25 C27 1.522(13) . ? C26 H33 0.9800 . ? C26 H34 0.9800 . ? C26 H35 0.9800 . ? C27 H36 0.9800 . ? C27 H37 0.9800 . ? C27 H38 0.9800 . ? C28 H39 0.9800 . ? C28 H40 0.9800 . ? C28 H41 0.9800 . ? C29 C30 1.486(9) . ? C29 H42 0.9900 . ? C29 H43 0.9900 . ? C30 H44 0.9900 . ? C30 H45 0.9900 . ? C31 H46 0.9800 . ? C31 H47 0.9800 . ? C31 H48 0.9800 . ? C32 H49 0.9800 . ? C32 H50 0.9800 . ? C32 H51 0.9800 . ? C33 C34 1.451(11) . ? C33 H52 0.9900 . ? C33 H53 0.9900 . ? C34 H54 0.9900 . ? C34 H55 0.9900 . ? C35 H56 0.9800 . ? C35 H57 0.9800 . ? C35 H58 0.9800 . ? C36 H59 0.9800 . ? C36 H60 0.9800 . ? C36 H61 0.9800 . ? C37 C38 1.474(18) . ? C37 H62 0.9900 . ? C37 H63 0.9900 . ? C38 H64 0.9900 . ? C38 H65 0.9900 . ? C39 H66 0.9800 . ? C39 H67 0.9800 . ? C39 H68 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O5 Sr1 O2 75.16(12) 2 . ? O5 Sr1 O3 143.24(12) 2 . ? O2 Sr1 O3 76.71(12) . . ? O5 Sr1 O4 117.15(13) 2 . ? O2 Sr1 O4 142.86(12) . . ? O3 Sr1 O4 74.71(12) . . ? O5 Sr1 O1 77.61(11) 2 . ? O2 Sr1 O1 71.81(13) . . ? O3 Sr1 O1 71.42(13) . . ? O4 Sr1 O1 76.90(11) . . ? O5 Sr1 O7 126.54(13) 2 . ? O2 Sr1 O7 95.30(13) . . ? O3 Sr1 O7 79.11(12) . . ? O4 Sr1 O7 102.02(13) . . ? O1 Sr1 O7 149.77(15) . . ? O5 Sr1 O8 83.28(13) 2 . ? O2 Sr1 O8 128.72(12) . . ? O3 Sr1 O8 133.25(12) . . ? O4 Sr1 O8 88.36(13) . . ? O1 Sr1 O8 146.85(16) . . ? O7 Sr1 O8 62.00(13) . . ? C1 O1 Sr1 96.43(14) . 2 ? C1 O1 Sr1 96.43(14) . . ? Sr1 O1 Sr1 167.1(3) 2 . ? C1 O1 Sr3 96.84(14) . 2 ? Sr1 O1 Sr3 89.00(5) 2 2 ? Sr1 O1 Sr3 89.47(5) . 2 ? C1 O1 Sr3 96.84(14) . . ? Sr1 O1 Sr3 89.47(5) 2 . ? Sr1 O1 Sr3 89.00(5) . . ? Sr3 O1 Sr3 166.3(3) 2 . ? C1 O1 Sr2 180.000(2) . . ? Sr1 O1 Sr2 83.57(14) 2 . ? Sr1 O1 Sr2 83.57(14) . . ? Sr3 O1 Sr2 83.16(14) 2 . ? Sr3 O1 Sr2 83.16(14) . . ? O1 C1 H1 109.5 . . ? O1 C1 H2 109.5 . . ? H1 C1 H2 109.5 . . ? O1 C1 H3 109.5 . . ? H1 C1 H3 109.5 . . ? H2 C1 H3 109.5 . . ? O6 Sr2 O3 115.36(8) . . ? O6 Sr2 O3 115.36(8) . 2 ? O3 Sr2 O3 129.28(17) . 2 ? O6 Sr2 O2 115.11(8) . 2 ? O3 Sr2 O2 79.52(12) . 2 ? O3 Sr2 O2 79.54(12) 2 2 ? O6 Sr2 O2 115.11(8) . . ? O3 Sr2 O2 79.54(12) . . ? O3 Sr2 O2 79.52(12) 2 . ? O2 Sr2 O2 129.78(17) 2 . ? O6 Sr2 O1 180.000(1) . . ? O3 Sr2 O1 64.64(8) . . ? O3 Sr2 O1 64.64(8) 2 . ? O2 Sr2 O1 64.89(8) 2 . ? O2 Sr2 O1 64.89(8) . . ? O6 Sr2 Sr3 136.796(14) . 2 ? O3 Sr2 Sr3 97.37(9) . 2 ? O3 Sr2 Sr3 41.18(8) 2 2 ? O2 Sr2 Sr3 97.24(9) 2 2 ? O2 Sr2 Sr3 41.86(8) . 2 ? O1 Sr2 Sr3 43.204(14) . 2 ? O6 Sr2 Sr1 137.109(13) . 2 ? O3 Sr2 Sr1 96.89(9) . 2 ? O3 Sr2 Sr1 41.62(8) 2 2 ? O2 Sr2 Sr1 41.61(8) 2 2 ? O2 Sr2 Sr1 97.23(9) . 2 ? O1 Sr2 Sr1 42.891(13) . 2 ? Sr3 Sr2 Sr1 57.59(2) 2 2 ? C2 O2 Sr2 107.1(3) . . ? C2 O2 Sr1 129.2(4) . . ? Sr2 O2 Sr1 98.20(12) . . ? C2 O2 Sr3 125.9(3) . 2 ? Sr2 O2 Sr3 97.79(12) . 2 ? Sr1 O2 Sr3 92.04(12) . 2 ? O2 C2 H4 109.5 . . ? O2 C2 H5 109.5 . . ? H4 C2 H5 109.5 . . ? O2 C2 H6 109.5 . . ? H4 C2 H6 109.5 . . ? H5 C2 H6 109.5 . . ? O4 Sr3 O3 75.80(12) . . ? O4 Sr3 O2 143.73(12) . 2 ? O3 Sr3 O2 77.05(12) . 2 ? O4 Sr3 O5 116.20(13) . . ? O3 Sr3 O5 142.50(12) . . ? O2 Sr3 O5 74.34(12) 2 . ? O4 Sr3 O1 77.35(12) . . ? O3 Sr3 O1 71.61(13) . . ? O2 Sr3 O1 71.54(13) 2 . ? O5 Sr3 O1 76.65(11) . . ? O4 Sr3 O9 84.86(13) . . ? O3 Sr3 O9 132.97(14) . . ? O2 Sr3 O9 131.41(13) 2 . ? O5 Sr3 O9 84.48(14) . . ? O1 Sr3 O9 144.67(18) . . ? O4 Sr3 O10 122.89(14) . . ? O3 Sr3 O10 94.49(13) . . ? O2 Sr3 O10 82.72(13) 2 . ? O5 Sr3 O10 105.28(13) . . ? O1 Sr3 O10 152.77(17) . . ? O9 Sr3 O10 61.20(15) . . ? O4 Sr3 Sr1 118.68(9) . 2 ? O3 Sr3 Sr1 99.06(8) . 2 ? O2 Sr3 Sr1 43.93(8) 2 2 ? O5 Sr3 Sr1 43.50(9) . 2 ? O1 Sr3 Sr1 45.13(3) . 2 ? O9 Sr3 Sr1 127.66(11) . 2 ? O10 Sr3 Sr1 118.42(10) . 2 ? C3 O3 Sr2 111.6(4) . . ? C3 O3 Sr3 111.7(4) . . ? Sr2 O3 Sr3 98.75(12) . . ? C3 O3 Sr1 137.2(4) . . ? Sr2 O3 Sr1 98.36(13) . . ? Sr3 O3 Sr1 92.14(12) . . ? O3 C3 H7 109.5 . . ? O3 C3 H8 109.5 . . ? H7 C3 H8 109.5 . . ? O3 C3 H9 109.5 . . ? H7 C3 H9 109.5 . . ? H8 C3 H9 109.5 . . ? C4 O4 Sr3 139.7(3) . . ? C4 O4 Sr1 126.0(3) . . ? Sr3 O4 Sr1 91.97(13) . . ? O4 C4 C9 120.9(6) . . ? O4 C4 C5 121.8(7) . . ? C9 C4 C5 117.3(7) . . ? C13 O5 Sr1 139.4(3) . 2 ? C13 O5 Sr3 125.6(3) . . ? Sr1 O5 Sr3 92.07(12) 2 . ? C6 C5 C4 119.8(9) . . ? C6 C5 C10 120.3(9) . . ? C4 C5 C10 120.0(8) . . ? C22 O6 Sr2 180.000(1) . . ? C7 C6 C5 120.5(9) . . ? C7 C6 H10 119.8 . . ? C5 C6 H10 119.8 . . ? C28 O7 C29 112.1(5) . . ? C28 O7 Sr1 119.8(4) . . ? C29 O7 Sr1 120.8(3) . . ? C8 C7 C6 119.7(10) . . ? C8 C7 C11 121.8(15) . . ? C6 C7 C11 118.5(15) . . ? C30 O8 C31 113.0(5) . . ? C30 O8 Sr1 112.8(3) . . ? C31 O8 Sr1 126.7(3) . . ? C7 C8 C9 122.2(10) . . ? C7 C8 H11 118.9 . . ? C9 C8 H11 118.9 . . ? C32 O9 C33 110.4(5) . . ? C32 O9 Sr3 133.1(4) . . ? C33 O9 Sr3 115.0(4) . . ? C8 C9 C4 120.5(8) . . ? C8 C9 C12 120.0(8) . . ? C4 C9 C12 119.4(6) . . ? C35 O10 C34 105.2(7) . . ? C35 O10 Sr3 142.6(5) . . ? C34 O10 Sr3 93.7(4) . . ? C5 C10 H12 109.5 . . ? C5 C10 H13 109.5 . . ? H12 C10 H13 109.5 . . ? C5 C10 H14 109.5 . . ? H12 C10 H14 109.5 . . ? H13 C10 H14 109.5 . . ? C36 O11 C37 116.9(11) . . ? C7 C11 H15 109.5 . . ? C7 C11 H16 109.5 . . ? H15 C11 H16 109.5 . . ? C7 C11 H17 109.5 . . ? H15 C11 H17 109.5 . . ? H16 C11 H17 109.5 . . ? C38 O12 C39 113.0(12) . . ? C9 C12 H18 109.5 . . ? C9 C12 H19 109.5 . . ? H18 C12 H19 109.5 . . ? C9 C12 H20 109.5 . . ? H18 C12 H20 109.5 . . ? H19 C12 H20 109.5 . . ? O5 C13 C18 121.0(5) . . ? O5 C13 C14 121.7(5) . . ? C18 C13 C14 117.4(5) . . ? C15 C14 C13 119.1(6) . . ? C15 C14 C19 121.6(6) . . ? C13 C14 C19 119.3(6) . . ? C16 C15 C14 123.4(7) . . ? C16 C15 H21 118.3 . . ? C14 C15 H21 118.3 . . ? C17 C16 C15 117.1(6) . . ? C17 C16 C20 121.5(8) . . ? C15 C16 C20 121.4(8) . . ? C16 C17 C18 122.9(7) . . ? C16 C17 H22 118.6 . . ? C18 C17 H22 118.6 . . ? C17 C18 C13 120.1(6) . . ? C17 C18 C21 121.1(6) . . ? C13 C18 C21 118.8(6) . . ? C14 C19 H23 109.5 . . ? C14 C19 H24 109.5 . . ? H23 C19 H24 109.5 . . ? C14 C19 H25 109.5 . . ? H23 C19 H25 109.5 . . ? H24 C19 H25 109.5 . . ? C16 C20 H26 109.5 . . ? C16 C20 H27 109.5 . . ? H26 C20 H27 109.5 . . ? C16 C20 H28 109.5 . . ? H26 C20 H28 109.5 . . ? H27 C20 H28 109.5 . . ? C18 C21 H29 109.5 . . ? C18 C21 H30 109.5 . . ? H29 C21 H30 109.5 . . ? C18 C21 H31 109.5 . . ? H29 C21 H31 109.5 . . ? H30 C21 H31 109.5 . . ? O6 C22 C23 120.9(4) . 2 ? O6 C22 C23 120.9(4) . . ? C23 C22 C23 118.2(8) 2 . ? C24 C23 C22 118.8(7) . . ? C24 C23 C26 121.9(6) . . ? C22 C23 C26 119.3(6) . . ? C25 C24 C23 123.6(7) . . ? C25 C24 H32 118.2 . . ? C23 C24 H32 118.2 . . ? C24 C25 C24 117.0(8) . 2 ? C24 C25 C27 121.5(4) . . ? C24 C25 C27 121.5(4) 2 . ? C23 C26 H33 109.5 . . ? C23 C26 H34 109.5 . . ? H33 C26 H34 109.5 . . ? C23 C26 H35 109.5 . . ? H33 C26 H35 109.5 . . ? H34 C26 H35 109.5 . . ? C25 C27 H36 109.5 . . ? C25 C27 H37 109.5 . . ? H36 C27 H37 109.5 . . ? C25 C27 H38 109.5 . . ? H36 C27 H38 109.5 . . ? H37 C27 H38 109.5 . . ? O7 C28 H39 109.5 . . ? O7 C28 H40 109.5 . . ? H39 C28 H40 109.5 . . ? O7 C28 H41 109.5 . . ? H39 C28 H41 109.5 . . ? H40 C28 H41 109.5 . . ? O7 C29 C30 108.9(5) . . ? O7 C29 H42 109.9 . . ? C30 C29 H42 109.9 . . ? O7 C29 H43 109.9 . . ? C30 C29 H43 109.9 . . ? H42 C29 H43 108.3 . . ? O8 C30 C29 108.4(5) . . ? O8 C30 H44 110.0 . . ? C29 C30 H44 110.0 . . ? O8 C30 H45 110.0 . . ? C29 C30 H45 110.0 . . ? H44 C30 H45 108.4 . . ? O8 C31 H46 109.5 . . ? O8 C31 H47 109.5 . . ? H46 C31 H47 109.5 . . ? O8 C31 H48 109.5 . . ? H46 C31 H48 109.5 . . ? H47 C31 H48 109.5 . . ? O9 C32 H49 109.5 . . ? O9 C32 H50 109.5 . . ? H49 C32 H50 109.5 . . ? O9 C32 H51 109.5 . . ? H49 C32 H51 109.5 . . ? H50 C32 H51 109.5 . . ? O9 C33 C34 107.8(6) . . ? O9 C33 H52 110.1 . . ? C34 C33 H52 110.1 . . ? O9 C33 H53 110.1 . . ? C34 C33 H53 110.1 . . ? H52 C33 H53 108.5 . . ? C33 C34 O10 112.5(7) . . ? C33 C34 H54 109.1 . . ? O10 C34 H54 109.1 . . ? C33 C34 H55 109.1 . . ? O10 C34 H55 109.1 . . ? H54 C34 H55 107.8 . . ? O10 C35 H56 109.5 . . ? O10 C35 H57 109.5 . . ? H56 C35 H57 109.5 . . ? O10 C35 H58 109.5 . . ? H56 C35 H58 109.5 . . ? H57 C35 H58 109.5 . . ? O11 C36 H59 109.5 . . ? O11 C36 H60 109.5 . . ? H59 C36 H60 109.5 . . ? O11 C36 H61 109.5 . . ? H59 C36 H61 109.5 . . ? H60 C36 H61 109.5 . . ? O11 C37 C38 111.9(11) . . ? O11 C37 H62 109.2 . . ? C38 C37 H62 109.2 . . ? O11 C37 H63 109.2 . . ? C38 C37 H63 109.2 . . ? H62 C37 H63 107.9 . . ? O12 C38 C37 107.5(12) . . ? O12 C38 H64 110.2 . . ? C37 C38 H64 110.2 . . ? O12 C38 H65 110.2 . . ? C37 C38 H65 110.2 . . ? H64 C38 H65 108.5 . . ? O12 C39 H66 109.5 . . ? O12 C39 H67 109.5 . . ? H66 C39 H67 109.5 . . ? O12 C39 H68 109.5 . . ? H66 C39 H68 109.5 . . ? H67 C39 H68 109.5 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.029 _refine_diff_density_min -0.794 _refine_diff_density_rms 0.111 data_c:\srsad _database_code_depnum_ccdc_archive 'CCDC 716849' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C78 H114 O12 Sr3' _chemical_formula_sum 'C78 H114 O12 Sr3' _chemical_formula_weight 1506.55 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sr Sr -1.5307 3.2498 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.768(2) _cell_length_b 12.175(2) _cell_length_c 14.278(3) _cell_angle_alpha 110.011(4) _cell_angle_beta 98.708(5) _cell_angle_gamma 96.887(6) _cell_volume 1867.3(6) _cell_formula_units_Z 1 _cell_measurement_temperature 95(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.46 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.340 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 792 _exptl_absorpt_coefficient_mu 2.193 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.4319 _exptl_absorpt_correction_T_max 0.9174 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 95(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker X8 Apex II CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16146 _diffrn_reflns_av_R_equivalents 0.1160 _diffrn_reflns_av_sigmaI/netI 0.3245 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.78 _diffrn_reflns_theta_max 27.50 _reflns_number_total 7706 _reflns_number_gt 3457 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART (Bruker)' _computing_cell_refinement 'Bruker SMART (Bruker)' _computing_data_reduction 'Bruker SAINT (Bruker)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 1999)' _computing_publication_material 'CIFTAB (Sheldrick, 1997)' _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^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7706 _refine_ls_number_parameters 421 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1417 _refine_ls_R_factor_gt 0.0582 _refine_ls_wR_factor_ref 0.1299 _refine_ls_wR_factor_gt 0.1038 _refine_ls_goodness_of_fit_ref 0.648 _refine_ls_restrained_S_all 0.648 _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 Sr1 Sr 0.5000 1.0000 0.5000 0.0122(2) Uani 1 2 d S . . O1 O 0.6243(4) 0.8324(4) 0.4831(3) 0.0183(10) Uani 1 1 d . . . C1 C 0.6660(6) 0.7552(5) 0.4091(5) 0.0179(14) Uani 1 1 d . . . Sr2 Sr 0.67730(5) 0.90002(5) 0.66597(4) 0.01232(15) Uani 1 1 d . . . O2 O 0.6824(4) 1.0881(4) 0.6389(3) 0.0188(10) Uani 1 1 d . . . C2 C 0.7859(6) 0.7735(5) 0.4051(5) 0.0183(14) Uani 1 1 d . . . O3 O 0.4690(4) 0.9121(4) 0.6321(3) 0.0180(10) Uani 1 1 d . . . C3 C 0.8252(5) 0.6999(5) 0.3262(5) 0.0192(14) Uani 1 1 d . . . H1 H 0.9060 0.7153 0.3250 0.023 Uiso 1 1 calc R . . O4 O 0.7806(4) 0.7177(4) 0.6365(3) 0.0195(10) Uani 1 1 d . . . C4 C 0.7534(6) 0.6034(6) 0.2471(5) 0.0230(15) Uani 1 1 d . . . O5 O 0.8888(4) 1.0014(4) 0.7706(3) 0.0197(10) Uani 1 1 d . . . C5 C 0.6359(6) 0.5837(5) 0.2541(5) 0.0221(15) Uani 1 1 d . . . H2 H 0.5841 0.5174 0.2028 0.026 Uiso 1 1 calc R . . O6 O 0.6582(4) 0.8561(4) 0.8353(3) 0.0216(11) Uani 1 1 d . . . C6 C 0.5916(5) 0.6573(5) 0.3332(5) 0.0161(14) Uani 1 1 d . . . C7 C 0.8681(5) 0.8794(6) 0.4882(5) 0.0227(15) Uani 1 1 d . . . H3 H 0.9480 0.8797 0.4763 0.034 Uiso 1 1 calc R . . H4 H 0.8658 0.8736 0.5547 0.034 Uiso 1 1 calc R . . H5 H 0.8436 0.9531 0.4871 0.034 Uiso 1 1 calc R . . C8 C 0.7964(7) 0.5284(6) 0.1573(6) 0.049(2) Uani 1 1 d . . . H6 H 0.7318 0.4663 0.1104 0.073 Uiso 1 1 calc R . . H7 H 0.8589 0.4915 0.1806 0.073 Uiso 1 1 calc R . . H8 H 0.8268 0.5784 0.1222 0.073 Uiso 1 1 calc R . . C9 C 0.4645(5) 0.6320(6) 0.3369(5) 0.0220(16) Uani 1 1 d . . . H9 H 0.4250 0.5601 0.2787 0.033 Uiso 1 1 calc R . . H10 H 0.4281 0.6994 0.3339 0.033 Uiso 1 1 calc R . . H11 H 0.4574 0.6201 0.4004 0.033 Uiso 1 1 calc R . . C10 C 0.7401(5) 1.1969(5) 0.7035(5) 0.0136(13) Uani 1 1 d . . . C11 C 0.7339(5) 1.2388(5) 0.8052(5) 0.0147(14) Uani 1 1 d . . . C12 C 0.7878(5) 1.3546(5) 0.8677(5) 0.0184(14) Uani 1 1 d . . . H12 H 0.7803 1.3830 0.9369 0.022 Uiso 1 1 calc R . . C13 C 0.8523(5) 1.4305(5) 0.8328(5) 0.0187(14) Uani 1 1 d . . . C14 C 0.8581(5) 1.3870(5) 0.7310(4) 0.0148(13) Uani 1 1 d . . . H13 H 0.9010 1.4372 0.7051 0.018 Uiso 1 1 calc R . . C15 C 0.8039(5) 1.2729(5) 0.6646(4) 0.0139(13) Uani 1 1 d . . . C16 C 0.6677(5) 1.1607(5) 0.8479(5) 0.0198(14) Uani 1 1 d . . . H14 H 0.6728 1.2039 0.9208 0.030 Uiso 1 1 calc R . . H15 H 0.7014 1.0889 0.8385 0.030 Uiso 1 1 calc R . . H16 H 0.5855 1.1384 0.8125 0.030 Uiso 1 1 calc R . . C17 C 0.9113(6) 1.5561(6) 0.9032(5) 0.0255(16) Uani 1 1 d . . . H17 H 0.9525 1.5954 0.8652 0.038 Uiso 1 1 calc R . . H18 H 0.9674 1.5528 0.9599 0.038 Uiso 1 1 calc R . . H19 H 0.8521 1.6012 0.9298 0.038 Uiso 1 1 calc R . . C18 C 0.8093(5) 1.2296(6) 0.5535(4) 0.0195(15) Uani 1 1 d . . . H20 H 0.8569 1.2918 0.5396 0.029 Uiso 1 1 calc R . . H21 H 0.7301 1.2106 0.5121 0.029 Uiso 1 1 calc R . . H22 H 0.8446 1.1581 0.5363 0.029 Uiso 1 1 calc R . . C19 C 0.3943(5) 0.8799(5) 0.6855(5) 0.0138(13) Uani 1 1 d . . . C20 C 0.3773(5) 0.7636(5) 0.6862(5) 0.0160(14) Uani 1 1 d . . . C21 C 0.3033(6) 0.7325(6) 0.7443(5) 0.0220(15) Uani 1 1 d . . . H23 H 0.2932 0.6539 0.7444 0.026 Uiso 1 1 calc R . . C22 C 0.2437(5) 0.8147(6) 0.8025(5) 0.0210(15) Uani 1 1 d . . . C23 C 0.2589(5) 0.9281(6) 0.7980(5) 0.0223(15) Uani 1 1 d . . . H24 H 0.2189 0.9850 0.8367 0.027 Uiso 1 1 calc R . . C24 C 0.3293(5) 0.9607(6) 0.7402(5) 0.0191(14) Uani 1 1 d . . . C25 C 0.4443(6) 0.6745(5) 0.6273(5) 0.0236(16) Uani 1 1 d . . . H25 H 0.4231 0.5985 0.6357 0.035 Uiso 1 1 calc R . . H26 H 0.5284 0.7043 0.6532 0.035 Uiso 1 1 calc R . . H27 H 0.4247 0.6628 0.5550 0.035 Uiso 1 1 calc R . . C26 C 0.1665(6) 0.7816(7) 0.8690(6) 0.037(2) Uani 1 1 d . . . H28 H 0.1678 0.6991 0.8628 0.056 Uiso 1 1 calc R . . H29 H 0.0861 0.7899 0.8468 0.056 Uiso 1 1 calc R . . H30 H 0.1960 0.8345 0.9402 0.056 Uiso 1 1 calc R . . C27 C 0.3369(6) 1.0817(6) 0.7321(6) 0.0291(17) Uani 1 1 d . . . H31 H 0.2876 1.1273 0.7742 0.044 Uiso 1 1 calc R . . H32 H 0.3099 1.0724 0.6610 0.044 Uiso 1 1 calc R . . H33 H 0.4182 1.1241 0.7560 0.044 Uiso 1 1 calc R . . C28 C 0.7255(6) 0.5976(5) 0.5669(5) 0.0225(15) Uani 1 1 d . . . H34 H 0.6575 0.5996 0.5177 0.027 Uiso 1 1 calc R . . H35 H 0.6986 0.5486 0.6050 0.027 Uiso 1 1 calc R . . C29 C 0.8205(6) 0.5471(6) 0.5116(5) 0.0275(17) Uani 1 1 d . . . H36 H 0.8191 0.4632 0.5047 0.033 Uiso 1 1 calc R . . H37 H 0.8099 0.5516 0.4430 0.033 Uiso 1 1 calc R . . C30 C 0.9341(6) 0.6254(6) 0.5791(5) 0.0309(18) Uani 1 1 d . . . H38 H 0.9877 0.5769 0.5992 0.037 Uiso 1 1 calc R . . H39 H 0.9734 0.6705 0.5433 0.037 Uiso 1 1 calc R . . C31 C 0.8989(5) 0.7086(6) 0.6711(5) 0.0245(15) Uani 1 1 d . . . H40 H 0.9036 0.6762 0.7261 0.029 Uiso 1 1 calc R . . H41 H 0.9507 0.7876 0.6971 0.029 Uiso 1 1 calc R . . C32 C 0.9749(5) 1.0699(5) 0.7401(5) 0.0181(14) Uani 1 1 d . . . H42 H 0.9376 1.0939 0.6850 0.022 Uiso 1 1 calc R . . H43 H 1.0354 1.0237 0.7162 0.022 Uiso 1 1 calc R . . C33 C 1.0293(5) 1.1817(5) 0.8394(5) 0.0186(15) Uani 1 1 d . . . H44 H 1.1155 1.1992 0.8490 0.022 Uiso 1 1 calc R . . H45 H 0.9977 1.2525 0.8363 0.022 Uiso 1 1 calc R . . C34 C 0.9935(6) 1.1472(6) 0.9247(5) 0.0244(16) Uani 1 1 d . . . H46 H 1.0628 1.1573 0.9778 0.029 Uiso 1 1 calc R . . H47 H 0.9385 1.1966 0.9563 0.029 Uiso 1 1 calc R . . C35 C 0.9351(5) 1.0181(5) 0.8742(5) 0.0199(15) Uani 1 1 d . . . H48 H 0.9925 0.9656 0.8776 0.024 Uiso 1 1 calc R . . H49 H 0.8716 1.0000 0.9080 0.024 Uiso 1 1 calc R . . C36 C 0.6972(7) 0.7570(7) 0.8535(5) 0.0335(18) Uani 1 1 d . . . H50 H 0.7829 0.7646 0.8594 0.040 Uiso 1 1 calc R . . H51 H 0.6587 0.6817 0.7970 0.040 Uiso 1 1 calc R . . C37 C 0.6641(7) 0.7581(7) 0.9534(6) 0.038(2) Uani 1 1 d . . . H52 H 0.6450 0.6764 0.9527 0.045 Uiso 1 1 calc R . . H53 H 0.7282 0.8049 1.0124 0.045 Uiso 1 1 calc R . . C38 C 0.5578(6) 0.8166(6) 0.9564(6) 0.0303(18) Uani 1 1 d . . . H54 H 0.5465 0.8536 1.0269 0.036 Uiso 1 1 calc R . . H55 H 0.4861 0.7593 0.9142 0.036 Uiso 1 1 calc R . . C39 C 0.5909(6) 0.9091(6) 0.9119(5) 0.0224(15) Uani 1 1 d . . . H56 H 0.5200 0.9298 0.8801 0.027 Uiso 1 1 calc R . . H57 H 0.6388 0.9822 0.9656 0.027 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 Sr1 0.0132(5) 0.0129(5) 0.0102(5) 0.0043(4) 0.0046(4) -0.0015(3) O1 0.012(2) 0.017(2) 0.021(3) 0.003(2) 0.004(2) -0.0001(18) C1 0.029(4) 0.017(3) 0.011(3) 0.008(3) 0.007(3) 0.006(3) Sr2 0.0134(3) 0.0110(3) 0.0124(3) 0.0041(3) 0.0046(3) -0.0003(2) O2 0.019(2) 0.014(2) 0.019(2) 0.0038(19) 0.003(2) -0.0083(18) C2 0.023(4) 0.013(3) 0.019(3) 0.008(3) 0.005(3) -0.002(3) O3 0.020(2) 0.022(2) 0.011(2) 0.0047(19) 0.0046(19) 0.0006(19) C3 0.014(3) 0.019(3) 0.027(4) 0.011(3) 0.008(3) -0.001(3) O4 0.024(3) 0.014(2) 0.019(2) 0.0033(19) 0.006(2) 0.0009(19) C4 0.031(4) 0.019(4) 0.021(4) 0.005(3) 0.016(3) 0.005(3) O5 0.018(2) 0.015(2) 0.021(3) 0.005(2) -0.001(2) -0.0073(18) C5 0.030(4) 0.013(3) 0.015(3) -0.002(3) 0.005(3) -0.005(3) O6 0.029(3) 0.025(3) 0.014(2) 0.009(2) 0.009(2) 0.003(2) C6 0.018(4) 0.016(3) 0.017(3) 0.009(3) 0.005(3) 0.002(3) C7 0.014(3) 0.029(4) 0.023(4) 0.008(3) 0.007(3) -0.002(3) C8 0.069(6) 0.030(5) 0.048(5) 0.001(4) 0.045(5) 0.005(4) C9 0.019(4) 0.020(4) 0.022(4) 0.002(3) 0.004(3) 0.001(3) C10 0.015(3) 0.009(3) 0.016(3) 0.003(3) 0.005(3) 0.003(2) C11 0.018(3) 0.014(3) 0.014(3) 0.006(3) 0.003(3) 0.007(3) C12 0.017(3) 0.022(4) 0.014(3) 0.005(3) 0.002(3) 0.003(3) C13 0.015(3) 0.018(3) 0.021(4) 0.005(3) 0.001(3) 0.004(3) C14 0.017(3) 0.011(3) 0.015(3) 0.004(3) 0.006(3) -0.003(2) C15 0.013(3) 0.014(3) 0.011(3) 0.003(3) 0.000(3) -0.002(2) C16 0.018(3) 0.020(3) 0.015(3) 0.002(3) 0.000(3) -0.003(3) C17 0.038(4) 0.015(3) 0.021(4) 0.004(3) 0.013(3) -0.002(3) C18 0.022(4) 0.022(4) 0.008(3) 0.001(3) 0.000(3) -0.006(3) C19 0.007(3) 0.025(4) 0.017(3) 0.016(3) 0.005(3) 0.000(2) C20 0.011(3) 0.019(3) 0.015(3) 0.006(3) 0.000(3) -0.003(3) C21 0.027(4) 0.018(3) 0.022(4) 0.011(3) 0.004(3) -0.004(3) C22 0.016(3) 0.035(4) 0.020(4) 0.016(3) 0.011(3) 0.005(3) C23 0.025(4) 0.032(4) 0.014(3) 0.010(3) 0.009(3) 0.009(3) C24 0.018(3) 0.024(4) 0.020(3) 0.016(3) -0.002(3) 0.002(3) C25 0.025(4) 0.016(3) 0.024(4) 0.003(3) 0.007(3) -0.006(3) C26 0.038(5) 0.056(5) 0.034(5) 0.032(4) 0.020(4) 0.011(4) C27 0.025(4) 0.036(4) 0.038(5) 0.023(4) 0.015(4) 0.013(3) C28 0.023(4) 0.019(4) 0.026(4) 0.010(3) 0.007(3) -0.002(3) C29 0.034(4) 0.023(4) 0.027(4) 0.005(3) 0.016(4) 0.007(3) C30 0.031(4) 0.027(4) 0.040(5) 0.011(4) 0.022(4) 0.009(3) C31 0.024(4) 0.020(4) 0.025(4) 0.005(3) 0.001(3) 0.005(3) C32 0.013(3) 0.023(4) 0.016(3) 0.005(3) 0.005(3) 0.001(3) C33 0.015(3) 0.017(3) 0.018(3) 0.003(3) -0.001(3) -0.006(3) C34 0.029(4) 0.020(4) 0.016(4) 0.003(3) 0.003(3) -0.011(3) C35 0.016(3) 0.021(4) 0.022(4) 0.010(3) 0.002(3) 0.000(3) C36 0.042(5) 0.042(5) 0.031(4) 0.023(4) 0.016(4) 0.017(4) C37 0.040(5) 0.047(5) 0.031(5) 0.020(4) 0.008(4) 0.007(4) C38 0.024(4) 0.043(5) 0.036(4) 0.026(4) 0.011(3) 0.008(3) C39 0.021(4) 0.029(4) 0.016(3) 0.006(3) 0.008(3) 0.004(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sr1 O3 2.516(4) 2_676 ? Sr1 O3 2.516(4) . ? Sr1 O2 2.529(4) 2_676 ? Sr1 O2 2.529(4) . ? Sr1 O1 2.616(4) 2_676 ? Sr1 O1 2.616(4) . ? Sr1 Sr2 3.5408(7) 2_676 ? Sr1 Sr2 3.5408(8) . ? O1 C1 1.352(7) . ? O1 Sr2 2.408(4) . ? C1 C6 1.393(8) . ? C1 C2 1.415(8) . ? Sr2 O2 2.445(4) . ? Sr2 O3 2.458(4) . ? Sr2 O4 2.597(4) . ? Sr2 O5 2.613(4) . ? Sr2 O6 2.684(4) . ? Sr2 C19 3.371(6) . ? Sr2 C16 3.372(6) . ? O2 C10 1.351(7) . ? C2 C3 1.362(8) . ? C2 C7 1.520(8) . ? O3 C19 1.354(6) . ? C3 C4 1.391(8) . ? C3 H1 0.9500 . ? O4 C31 1.436(7) . ? O4 C28 1.459(7) . ? C4 C5 1.399(8) . ? C4 C8 1.497(8) . ? O5 C35 1.432(7) . ? O5 C32 1.446(6) . ? C5 C6 1.396(8) . ? C5 H2 0.9500 . ? O6 C36 1.431(8) . ? O6 C39 1.462(7) . ? C6 C9 1.504(8) . ? C7 H3 0.9800 . ? C7 H4 0.9800 . ? C7 H5 0.9800 . ? C8 H6 0.9800 . ? C8 H7 0.9800 . ? C8 H8 0.9800 . ? C9 H9 0.9800 . ? C9 H10 0.9800 . ? C9 H11 0.9800 . ? C10 C11 1.382(8) . ? C10 C15 1.427(8) . ? C11 C12 1.392(8) . ? C11 C16 1.499(8) . ? C12 C13 1.393(8) . ? C12 H12 0.9500 . ? C13 C14 1.382(8) . ? C13 C17 1.521(8) . ? C14 C15 1.392(8) . ? C14 H13 0.9500 . ? C15 C18 1.506(8) . ? C16 H14 0.9800 . ? C16 H15 0.9800 . ? C16 H16 0.9800 . ? C17 H17 0.9800 . ? C17 H18 0.9800 . ? C17 H19 0.9800 . ? C18 H20 0.9800 . ? C18 H21 0.9800 . ? C18 H22 0.9800 . ? C19 C20 1.410(8) . ? C19 C24 1.413(8) . ? C20 C21 1.394(8) . ? C20 C25 1.513(8) . ? C21 C22 1.401(9) . ? C21 H23 0.9500 . ? C22 C23 1.395(9) . ? C22 C26 1.525(8) . ? C23 C24 1.370(8) . ? C23 H24 0.9500 . ? C24 C27 1.510(9) . ? C25 H25 0.9800 . ? C25 H26 0.9800 . ? C25 H27 0.9800 . ? C26 H28 0.9800 . ? C26 H29 0.9800 . ? C26 H30 0.9800 . ? C27 H31 0.9800 . ? C27 H32 0.9800 . ? C27 H33 0.9800 . ? C28 C29 1.533(9) . ? C28 H34 0.9900 . ? C28 H35 0.9900 . ? C29 C30 1.516(9) . ? C29 H36 0.9900 . ? C29 H37 0.9900 . ? C30 C31 1.509(9) . ? C30 H38 0.9900 . ? C30 H39 0.9900 . ? C31 H40 0.9900 . ? C31 H41 0.9900 . ? C32 C33 1.571(8) . ? C32 H42 0.9900 . ? C32 H43 0.9900 . ? C33 C34 1.516(8) . ? C33 H44 0.9900 . ? C33 H45 0.9900 . ? C34 C35 1.510(8) . ? C34 H46 0.9900 . ? C34 H47 0.9900 . ? C35 H48 0.9900 . ? C35 H49 0.9900 . ? C36 C37 1.529(9) . ? C36 H50 0.9900 . ? C36 H51 0.9900 . ? C37 C38 1.511(10) . ? C37 H52 0.9900 . ? C37 H53 0.9900 . ? C38 C39 1.511(9) . ? C38 H54 0.9900 . ? C38 H55 0.9900 . ? C39 H56 0.9900 . ? C39 H57 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Sr1 O3 180.00(15) 2_676 . ? O3 Sr1 O2 74.85(13) 2_676 2_676 ? O3 Sr1 O2 105.15(13) . 2_676 ? O3 Sr1 O2 105.15(13) 2_676 . ? O3 Sr1 O2 74.85(13) . . ? O2 Sr1 O2 180.000(1) 2_676 . ? O3 Sr1 O1 71.50(13) 2_676 2_676 ? O3 Sr1 O1 108.50(13) . 2_676 ? O2 Sr1 O1 73.12(13) 2_676 2_676 ? O2 Sr1 O1 106.88(13) . 2_676 ? O3 Sr1 O1 108.50(13) 2_676 . ? O3 Sr1 O1 71.50(13) . . ? O2 Sr1 O1 106.88(13) 2_676 . ? O2 Sr1 O1 73.12(13) . . ? O1 Sr1 O1 180.000(1) 2_676 . ? O3 Sr1 Sr2 43.95(10) 2_676 2_676 ? O3 Sr1 Sr2 136.05(10) . 2_676 ? O2 Sr1 Sr2 43.66(9) 2_676 2_676 ? O2 Sr1 Sr2 136.34(9) . 2_676 ? O1 Sr1 Sr2 42.85(9) 2_676 2_676 ? O1 Sr1 Sr2 137.15(9) . 2_676 ? O3 Sr1 Sr2 136.05(10) 2_676 . ? O3 Sr1 Sr2 43.95(10) . . ? O2 Sr1 Sr2 136.34(9) 2_676 . ? O2 Sr1 Sr2 43.66(9) . . ? O1 Sr1 Sr2 137.15(9) 2_676 . ? O1 Sr1 Sr2 42.85(9) . . ? Sr2 Sr1 Sr2 180.0 2_676 . ? C1 O1 Sr2 131.6(4) . . ? C1 O1 Sr1 137.6(4) . . ? Sr2 O1 Sr1 89.51(13) . . ? O1 C1 C6 121.0(6) . . ? O1 C1 C2 120.8(5) . . ? C6 C1 C2 118.2(6) . . ? O1 Sr2 O2 78.35(14) . . ? O1 Sr2 O3 76.11(14) . . ? O2 Sr2 O3 77.42(14) . . ? O1 Sr2 O4 85.78(14) . . ? O2 Sr2 O4 142.75(14) . . ? O3 Sr2 O4 131.03(14) . . ? O1 Sr2 O5 123.60(13) . . ? O2 Sr2 O5 82.52(13) . . ? O3 Sr2 O5 148.21(14) . . ? O4 Sr2 O5 78.64(13) . . ? O1 Sr2 O6 147.54(14) . . ? O2 Sr2 O6 128.75(14) . . ? O3 Sr2 O6 91.56(14) . . ? O4 Sr2 O6 79.97(14) . . ? O5 Sr2 O6 82.00(13) . . ? O1 Sr2 C19 91.60(14) . . ? O2 Sr2 C19 92.77(14) . . ? O3 Sr2 C19 19.99(13) . . ? O4 Sr2 C19 121.41(14) . . ? O5 Sr2 C19 142.16(14) . . ? O6 Sr2 C19 71.87(14) . . ? O1 Sr2 C16 131.04(15) . . ? O2 Sr2 C16 55.91(15) . . ? O3 Sr2 C16 77.65(14) . . ? O4 Sr2 C16 141.20(15) . . ? O5 Sr2 C16 70.69(14) . . ? O6 Sr2 C16 72.86(14) . . ? C19 Sr2 C16 75.64(15) . . ? O1 Sr2 Sr1 47.64(10) . . ? O2 Sr2 Sr1 45.57(10) . . ? O3 Sr2 Sr1 45.28(9) . . ? O4 Sr2 Sr1 133.20(10) . . ? O5 Sr2 Sr1 126.80(9) . . ? O6 Sr2 Sr1 135.43(10) . . ? C19 Sr2 Sr1 65.25(10) . . ? C16 Sr2 Sr1 85.07(11) . . ? C10 O2 Sr2 127.4(4) . . ? C10 O2 Sr1 138.0(4) . . ? Sr2 O2 Sr1 90.76(13) . . ? C3 C2 C1 120.2(6) . . ? C3 C2 C7 121.1(6) . . ? C1 C2 C7 118.7(6) . . ? C19 O3 Sr2 121.6(3) . . ? C19 O3 Sr1 147.5(4) . . ? Sr2 O3 Sr1 90.77(13) . . ? C2 C3 C4 123.5(6) . . ? C2 C3 H1 118.3 . . ? C4 C3 H1 118.3 . . ? C31 O4 C28 104.6(5) . . ? C31 O4 Sr2 131.6(4) . . ? C28 O4 Sr2 123.5(4) . . ? C3 C4 C5 115.6(6) . . ? C3 C4 C8 122.7(6) . . ? C5 C4 C8 121.6(6) . . ? C35 O5 C32 106.4(4) . . ? C35 O5 Sr2 127.3(3) . . ? C32 O5 Sr2 125.5(3) . . ? C6 C5 C4 122.9(6) . . ? C6 C5 H2 118.6 . . ? C4 C5 H2 118.6 . . ? C36 O6 C39 108.3(5) . . ? C36 O6 Sr2 122.4(4) . . ? C39 O6 Sr2 128.4(4) . . ? C1 C6 C5 119.5(6) . . ? C1 C6 C9 119.9(6) . . ? C5 C6 C9 120.6(6) . . ? C2 C7 H3 109.5 . . ? C2 C7 H4 109.5 . . ? H3 C7 H4 109.5 . . ? C2 C7 H5 109.5 . . ? H3 C7 H5 109.5 . . ? H4 C7 H5 109.5 . . ? C4 C8 H6 109.5 . . ? C4 C8 H7 109.5 . . ? H6 C8 H7 109.5 . . ? C4 C8 H8 109.5 . . ? H6 C8 H8 109.5 . . ? H7 C8 H8 109.5 . . ? C6 C9 H9 109.5 . . ? C6 C9 H10 109.5 . . ? H9 C9 H10 109.5 . . ? C6 C9 H11 109.5 . . ? H9 C9 H11 109.5 . . ? H10 C9 H11 109.5 . . ? O2 C10 C11 121.5(5) . . ? O2 C10 C15 119.2(5) . . ? C11 C10 C15 119.2(5) . . ? C10 C11 C12 119.8(5) . . ? C10 C11 C16 120.2(5) . . ? C12 C11 C16 120.0(5) . . ? C11 C12 C13 122.6(6) . . ? C11 C12 H12 118.7 . . ? C13 C12 H12 118.7 . . ? C14 C13 C12 116.8(6) . . ? C14 C13 C17 121.8(5) . . ? C12 C13 C17 121.4(6) . . ? C13 C14 C15 122.9(5) . . ? C13 C14 H13 118.5 . . ? C15 C14 H13 118.5 . . ? C14 C15 C10 118.7(5) . . ? C14 C15 C18 121.5(5) . . ? C10 C15 C18 119.8(5) . . ? C11 C16 Sr2 96.4(3) . . ? C11 C16 H14 109.5 . . ? Sr2 C16 H14 146.1 . . ? C11 C16 H15 109.5 . . ? Sr2 C16 H15 39.0 . . ? H14 C16 H15 109.5 . . ? C11 C16 H16 109.5 . . ? Sr2 C16 H16 80.6 . . ? H14 C16 H16 109.5 . . ? H15 C16 H16 109.5 . . ? C13 C17 H17 109.5 . . ? C13 C17 H18 109.5 . . ? H17 C17 H18 109.5 . . ? C13 C17 H19 109.5 . . ? H17 C17 H19 109.5 . . ? H18 C17 H19 109.5 . . ? C15 C18 H20 109.5 . . ? C15 C18 H21 109.5 . . ? H20 C18 H21 109.5 . . ? C15 C18 H22 109.5 . . ? H20 C18 H22 109.5 . . ? H21 C18 H22 109.5 . . ? O3 C19 C20 120.7(5) . . ? O3 C19 C24 121.2(5) . . ? C20 C19 C24 118.0(5) . . ? O3 C19 Sr2 38.4(3) . . ? C20 C19 Sr2 97.2(4) . . ? C24 C19 Sr2 133.7(4) . . ? C21 C20 C19 120.3(6) . . ? C21 C20 C25 120.2(5) . . ? C19 C20 C25 119.4(5) . . ? C20 C21 C22 121.3(6) . . ? C20 C21 H23 119.4 . . ? C22 C21 H23 119.4 . . ? C23 C22 C21 117.3(6) . . ? C23 C22 C26 121.6(6) . . ? C21 C22 C26 121.1(6) . . ? C24 C23 C22 122.7(6) . . ? C24 C23 H24 118.6 . . ? C22 C23 H24 118.6 . . ? C23 C24 C19 120.1(6) . . ? C23 C24 C27 120.9(6) . . ? C19 C24 C27 119.0(6) . . ? C20 C25 H25 109.5 . . ? C20 C25 H26 109.5 . . ? H25 C25 H26 109.5 . . ? C20 C25 H27 109.5 . . ? H25 C25 H27 109.5 . . ? H26 C25 H27 109.5 . . ? C22 C26 H28 109.5 . . ? C22 C26 H29 109.5 . . ? H28 C26 H29 109.5 . . ? C22 C26 H30 109.5 . . ? H28 C26 H30 109.5 . . ? H29 C26 H30 109.5 . . ? C24 C27 H31 109.5 . . ? C24 C27 H32 109.5 . . ? H31 C27 H32 109.5 . . ? C24 C27 H33 109.5 . . ? H31 C27 H33 109.5 . . ? H32 C27 H33 109.5 . . ? O4 C28 C29 105.4(5) . . ? O4 C28 H34 110.7 . . ? C29 C28 H34 110.7 . . ? O4 C28 H35 110.7 . . ? C29 C28 H35 110.7 . . ? H34 C28 H35 108.8 . . ? C30 C29 C28 104.4(5) . . ? C30 C29 H36 110.9 . . ? C28 C29 H36 110.9 . . ? C30 C29 H37 110.9 . . ? C28 C29 H37 110.9 . . ? H36 C29 H37 108.9 . . ? C31 C30 C29 105.1(5) . . ? C31 C30 H38 110.7 . . ? C29 C30 H38 110.7 . . ? C31 C30 H39 110.7 . . ? C29 C30 H39 110.7 . . ? H38 C30 H39 108.8 . . ? O4 C31 C30 105.6(5) . . ? O4 C31 H40 110.6 . . ? C30 C31 H40 110.6 . . ? O4 C31 H41 110.6 . . ? C30 C31 H41 110.6 . . ? H40 C31 H41 108.8 . . ? O5 C32 C33 104.3(4) . . ? O5 C32 H42 110.9 . . ? C33 C32 H42 110.9 . . ? O5 C32 H43 110.9 . . ? C33 C32 H43 110.9 . . ? H42 C32 H43 108.9 . . ? C34 C33 C32 104.5(5) . . ? C34 C33 H44 110.9 . . ? C32 C33 H44 110.9 . . ? C34 C33 H45 110.9 . . ? C32 C33 H45 110.9 . . ? H44 C33 H45 108.9 . . ? C35 C34 C33 105.0(5) . . ? C35 C34 H46 110.7 . . ? C33 C34 H46 110.7 . . ? C35 C34 H47 110.7 . . ? C33 C34 H47 110.7 . . ? H46 C34 H47 108.8 . . ? O5 C35 C34 105.5(5) . . ? O5 C35 H48 110.6 . . ? C34 C35 H48 110.6 . . ? O5 C35 H49 110.6 . . ? C34 C35 H49 110.6 . . ? H48 C35 H49 108.8 . . ? O6 C36 C37 106.5(6) . . ? O6 C36 H50 110.4 . . ? C37 C36 H50 110.4 . . ? O6 C36 H51 110.4 . . ? C37 C36 H51 110.4 . . ? H50 C36 H51 108.6 . . ? C38 C37 C36 103.0(6) . . ? C38 C37 H52 111.2 . . ? C36 C37 H52 111.2 . . ? C38 C37 H53 111.2 . . ? C36 C37 H53 111.2 . . ? H52 C37 H53 109.1 . . ? C37 C38 C39 101.0(5) . . ? C37 C38 H54 111.6 . . ? C39 C38 H54 111.6 . . ? C37 C38 H55 111.6 . . ? C39 C38 H55 111.6 . . ? H54 C38 H55 109.4 . . ? O6 C39 C38 106.3(5) . . ? O6 C39 H56 110.5 . . ? C38 C39 H56 110.5 . . ? O6 C39 H57 110.5 . . ? C38 C39 H57 110.5 . . ? H56 C39 H57 108.7 . . ? _diffrn_measured_fraction_theta_max 0.897 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.897 _refine_diff_density_max 0.980 _refine_diff_density_min -0.623 _refine_diff_density_rms 0.100 data_c:\trica _database_code_depnum_ccdc_archive 'CCDC 716850' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C66 H110 Ba5 O18, C4 H10 O2' _chemical_formula_sum 'C70 H120 Ba5 O20' _chemical_formula_weight 1968.36 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ba Ba -0.3244 2.2819 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.3157(3) _cell_length_b 14.4496(4) _cell_length_c 22.7060(5) _cell_angle_alpha 95.0150(10) _cell_angle_beta 106.0160(10) _cell_angle_gamma 97.7450(10) _cell_volume 4125.14(17) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.585 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1960 _exptl_absorpt_coefficient_mu 2.413 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7135 _exptl_absorpt_correction_T_max 0.7943 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker X8 Apex II CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 53098 _diffrn_reflns_av_R_equivalents 0.0634 _diffrn_reflns_av_sigmaI/netI 0.0935 _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 -29 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 0.94 _diffrn_reflns_theta_max 27.50 _reflns_number_total 18923 _reflns_number_gt 11872 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART (Bruker)' _computing_cell_refinement 'Bruker SMART (Bruker)' _computing_data_reduction 'Bruker SAINT (Bruker)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 1999)' _computing_publication_material 'CIFTAB (Sheldrick, 1997)' _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^)+(0.0505P)^2^+12.2001P] 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 ? _refine_ls_extinction_coef ? _refine_ls_number_reflns 18923 _refine_ls_number_parameters 886 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1072 _refine_ls_R_factor_gt 0.0545 _refine_ls_wR_factor_ref 0.1367 _refine_ls_wR_factor_gt 0.1150 _refine_ls_goodness_of_fit_ref 1.012 _refine_ls_restrained_S_all 1.012 _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 Ba1 Ba 0.49924(4) -0.03689(3) 0.277440(18) 0.02787(11) Uani 1 1 d . . . O1 O 0.4747(4) 0.1309(3) 0.2286(2) 0.0355(13) Uani 1 1 d . . . C1 C 0.5119(9) 0.1018(8) 0.1710(5) 0.077(3) Uani 1 1 d . . . H1 H 0.5028 0.1503 0.1433 0.116 Uiso 1 1 calc R . . H2 H 0.4695 0.0416 0.1490 0.116 Uiso 1 1 calc R . . H3 H 0.5868 0.0951 0.1846 0.116 Uiso 1 1 calc R . . Ba2 Ba 0.39497(4) 0.18995(4) 0.34419(2) 0.03866(13) Uani 1 1 d . . . O2 O 0.3210(4) 0.0212(3) 0.2873(2) 0.0311(12) Uani 1 1 d . . . C2 C 0.2851(7) -0.0334(5) 0.3268(3) 0.0368(19) Uani 1 1 d . . . H5 H 0.2900 0.0063 0.3650 0.055 Uiso 1 1 calc R . . H4 H 0.3287 -0.0827 0.3364 0.055 Uiso 1 1 calc R . . H6 H 0.2112 -0.0625 0.3069 0.055 Uiso 1 1 calc R . . Ba3 Ba 0.67632(4) 0.21427(3) 0.311950(18) 0.02879(11) Uani 1 1 d . . . O3 O 0.5611(4) 0.1097(3) 0.3681(2) 0.0325(12) Uani 1 1 d . . . C3 C 0.6167(7) 0.1237(7) 0.4318(4) 0.050(2) Uani 1 1 d . . . H7 H 0.5787 0.1595 0.4546 0.075 Uiso 1 1 calc R . . H8 H 0.6880 0.1588 0.4381 0.075 Uiso 1 1 calc R . . H9 H 0.6221 0.0625 0.4469 0.075 Uiso 1 1 calc R . . Ba4 Ba 0.26109(3) 0.05949(3) 0.172310(17) 0.02560(11) Uani 1 1 d . . . O4 O 0.5266(4) 0.3182(3) 0.3172(2) 0.0325(12) Uani 1 1 d . . . C4 C 0.5109(7) 0.4080(5) 0.3361(4) 0.039(2) Uani 1 1 d . . . H10 H 0.4587 0.4031 0.3592 0.059 Uiso 1 1 calc R . . H11 H 0.4849 0.4395 0.2997 0.059 Uiso 1 1 calc R . . H12 H 0.5781 0.4445 0.3625 0.059 Uiso 1 1 calc R . . Ba5 Ba 0.44554(3) 0.30109(3) 0.193440(18) 0.02556(11) Uani 1 1 d . . . O5 O 0.2860(4) 0.2288(3) 0.2385(2) 0.0293(11) Uani 1 1 d . . . C5 C 0.2158(7) 0.2806(7) 0.2542(4) 0.049(2) Uani 1 1 d . . . H13 H 0.2145 0.2725 0.2964 0.073 Uiso 1 1 calc R . . H14 H 0.1448 0.2587 0.2255 0.073 Uiso 1 1 calc R . . H15 H 0.2379 0.3473 0.2519 0.073 Uiso 1 1 calc R . . O6 O 0.6482(4) 0.2977(4) 0.2112(2) 0.0337(12) Uani 1 1 d . . . C6 C 0.7409(6) 0.3418(6) 0.2076(3) 0.0330(18) Uani 1 1 d . . . O7 O 0.6945(4) 0.0398(4) 0.2783(2) 0.0349(12) Uani 1 1 d . . . C7 C 0.7762(6) 0.4361(6) 0.2313(3) 0.0342(18) Uani 1 1 d . . . O8 O 0.3587(4) -0.0905(3) 0.1671(2) 0.0336(12) Uani 1 1 d . . . C8 C 0.8733(7) 0.4804(6) 0.2260(4) 0.044(2) Uani 1 1 d . . . H16 H 0.8970 0.5453 0.2414 0.052 Uiso 1 1 calc R . . O9 O 0.3039(4) 0.1808(4) 0.1002(2) 0.0335(12) Uani 1 1 d . . . C9 C 0.9356(7) 0.4316(7) 0.1987(4) 0.045(2) Uani 1 1 d . . . O10 O 0.3164(5) 0.2185(4) 0.4275(3) 0.0568(17) Uani 1 1 d . . . C10 C 0.9000(7) 0.3385(7) 0.1768(4) 0.044(2) Uani 1 1 d . . . H17 H 0.9414 0.3044 0.1577 0.053 Uiso 1 1 calc R . . O11 O 0.5504(5) -0.1430(4) 0.3771(3) 0.0539(16) Uani 1 1 d . . . C11 C 0.8049(7) 0.2924(6) 0.1817(3) 0.0354(18) Uani 1 1 d . . . O12 O 0.5306(5) -0.2301(4) 0.2612(3) 0.0510(16) Uani 1 1 d . . . C12 C 0.7068(7) 0.4905(6) 0.2577(4) 0.047(2) Uani 1 1 d . . . H18 H 0.6392 0.4887 0.2261 0.071 Uiso 1 1 calc R . . H19 H 0.7421 0.5560 0.2711 0.071 Uiso 1 1 calc R . . H20 H 0.6939 0.4623 0.2932 0.071 Uiso 1 1 calc R . . O13 O 0.7720(6) 0.3527(4) 0.4177(3) 0.067(2) Uani 1 1 d . . . C13 C 1.0383(7) 0.4807(8) 0.1913(5) 0.066(3) Uani 1 1 d . . . H21 H 1.0975 0.4536 0.2156 0.098 Uiso 1 1 calc R . . H22 H 1.0480 0.5481 0.2059 0.098 Uiso 1 1 calc R . . H23 H 1.0359 0.4723 0.1476 0.098 Uiso 1 1 calc R . . O14 O 0.8981(5) 0.2582(5) 0.3660(3) 0.0585(18) Uani 1 1 d . . . C14 C 0.7683(8) 0.1892(6) 0.1559(4) 0.053(2) Uani 1 1 d . . . H25 H 0.7737 0.1514 0.1901 0.079 Uiso 1 1 calc R . . H26 H 0.8131 0.1697 0.1310 0.079 Uiso 1 1 calc R . . H24 H 0.6945 0.1799 0.1301 0.079 Uiso 1 1 calc R . . O15 O 0.0625(5) 0.0056(5) 0.1929(3) 0.0559(17) Uani 1 1 d . . . C15 C 0.7583(6) -0.0236(5) 0.2784(3) 0.0310(17) Uani 1 1 d . . . O16 O 0.0818(5) -0.0303(4) 0.0756(2) 0.0487(16) Uani 1 1 d . . . C16 C 0.8300(6) -0.0377(6) 0.3331(3) 0.0336(18) Uani 1 1 d . . . O17 O 0.3886(5) 0.4833(4) 0.1698(3) 0.0490(15) Uani 1 1 d . . . C17 C 0.8960(6) -0.1046(6) 0.3322(3) 0.0376(19) Uani 1 1 d . . . H27 H 0.9455 -0.1124 0.3698 0.045 Uiso 1 1 calc R . . O18 O 0.5033(5) 0.4058(4) 0.1018(2) 0.0491(15) Uani 1 1 d . . . C18 C 0.8920(6) -0.1598(6) 0.2786(4) 0.0380(19) Uani 1 1 d . . . O19 O 1.1601(7) -0.2515(5) 0.4163(3) 0.082(2) Uani 1 1 d . . . C19 C 0.8197(6) -0.1477(5) 0.2256(3) 0.0374(19) Uani 1 1 d . . . H28 H 0.8145 -0.1867 0.1886 0.045 Uiso 1 1 calc R . . O20 O 1.2152(9) -0.4342(7) 0.3926(4) 0.119(4) Uani 1 1 d . . . C20 C 0.7522(6) -0.0801(5) 0.2231(3) 0.0318(17) Uani 1 1 d . . . C21 C 0.8336(7) 0.0163(6) 0.3929(3) 0.045(2) Uani 1 1 d . . . H29 H 0.8550 0.0837 0.3920 0.067 Uiso 1 1 calc R . . H30 H 0.8848 -0.0049 0.4268 0.067 Uiso 1 1 calc R . . H31 H 0.7632 0.0057 0.3992 0.067 Uiso 1 1 calc R . . C22 C 0.9690(7) -0.2264(6) 0.2767(4) 0.054(2) Uani 1 1 d . . . H32 H 0.9302 -0.2878 0.2547 0.081 Uiso 1 1 calc R . . H33 H 1.0080 -0.2338 0.3190 0.081 Uiso 1 1 calc R . . H34 H 1.0190 -0.2010 0.2552 0.081 Uiso 1 1 calc R . . C23 C 0.6764(8) -0.0691(6) 0.1619(3) 0.052(3) Uani 1 1 d . . . H35 H 0.6937 -0.0055 0.1518 0.078 Uiso 1 1 calc R . . H36 H 0.6037 -0.0791 0.1648 0.078 Uiso 1 1 calc R . . H37 H 0.6826 -0.1156 0.1296 0.078 Uiso 1 1 calc R . . C24 C 0.3095(6) -0.1644(5) 0.1255(3) 0.0276(16) Uani 1 1 d . . . C25 C 0.2418(6) -0.2362(5) 0.1389(3) 0.0330(18) Uani 1 1 d . . . C26 C 0.1889(7) -0.3125(5) 0.0942(3) 0.0374(19) Uani 1 1 d . . . H38 H 0.1420 -0.3598 0.1044 0.045 Uiso 1 1 calc R . . C27 C 0.2018(7) -0.3222(6) 0.0361(3) 0.040(2) Uani 1 1 d . . . C28 C 0.2693(7) -0.2500(6) 0.0230(3) 0.043(2) Uani 1 1 d . . . H39 H 0.2793 -0.2547 -0.0169 0.052 Uiso 1 1 calc R . . C29 C 0.3230(6) -0.1713(6) 0.0651(3) 0.0345(18) Uani 1 1 d . . . C30 C 0.2249(7) -0.2295(6) 0.2019(4) 0.047(2) Uani 1 1 d . . . H40 H 0.2930 -0.2257 0.2335 0.070 Uiso 1 1 calc R . . H41 H 0.1765 -0.2854 0.2044 0.070 Uiso 1 1 calc R . . H42 H 0.1943 -0.1729 0.2087 0.070 Uiso 1 1 calc R . . C31 C 0.1481(8) -0.4066(6) -0.0106(4) 0.059(3) Uani 1 1 d . . . H43 H 0.1551 -0.3944 -0.0512 0.088 Uiso 1 1 calc R . . H44 H 0.0729 -0.4195 -0.0129 0.088 Uiso 1 1 calc R . . H45 H 0.1812 -0.4613 0.0017 0.088 Uiso 1 1 calc R . . C32 C 0.3875(7) -0.0923(7) 0.0477(4) 0.051(2) Uani 1 1 d . . . H46 H 0.3877 -0.1074 0.0048 0.076 Uiso 1 1 calc R . . H47 H 0.4603 -0.0826 0.0750 0.076 Uiso 1 1 calc R . . H48 H 0.3572 -0.0348 0.0517 0.076 Uiso 1 1 calc R . . C33 C 0.2666(6) 0.2218(5) 0.0507(3) 0.0300(17) Uani 1 1 d . . . C34 C 0.1715(6) 0.2609(5) 0.0431(3) 0.0340(18) Uani 1 1 d . . . C35 C 0.1349(7) 0.3064(6) -0.0084(3) 0.042(2) Uani 1 1 d . . . H49 H 0.0711 0.3315 -0.0135 0.051 Uiso 1 1 calc R . . C36 C 0.1892(8) 0.3163(5) -0.0526(3) 0.045(2) Uani 1 1 d . . . C37 C 0.2787(7) 0.2783(5) -0.0446(3) 0.042(2) Uani 1 1 d . . . H50 H 0.3159 0.2841 -0.0746 0.050 Uiso 1 1 calc R . . C38 C 0.3192(7) 0.2309(5) 0.0058(3) 0.039(2) Uani 1 1 d . . . C39 C 0.1138(7) 0.2540(7) 0.0906(4) 0.052(2) Uani 1 1 d . . . H51 H 0.1597 0.2872 0.1304 0.078 Uiso 1 1 calc R . . H52 H 0.0939 0.1876 0.0947 0.078 Uiso 1 1 calc R . . H53 H 0.0498 0.2826 0.0780 0.078 Uiso 1 1 calc R . . C40 C 0.1470(10) 0.3652(6) -0.1087(4) 0.072(4) Uani 1 1 d . . . H54 H 0.1505 0.4322 -0.0954 0.109 Uiso 1 1 calc R . . H55 H 0.0733 0.3366 -0.1298 0.109 Uiso 1 1 calc R . . H56 H 0.1900 0.3583 -0.1370 0.109 Uiso 1 1 calc R . . C41 C 0.4169(7) 0.1879(7) 0.0118(4) 0.052(2) Uani 1 1 d . . . H57 H 0.4693 0.2136 0.0514 0.078 Uiso 1 1 calc R . . H58 H 0.4464 0.2026 -0.0220 0.078 Uiso 1 1 calc R . . H59 H 0.3991 0.1195 0.0098 0.078 Uiso 1 1 calc R . . C42 C 0.2681(7) 0.2490(6) 0.4661(3) 0.038(2) Uani 1 1 d . . . C43 C 0.3022(7) 0.3393(6) 0.5008(4) 0.048(2) Uani 1 1 d . . . C44 C 0.2483(7) 0.3692(6) 0.5416(4) 0.046(2) Uani 1 1 d . . . H60 H 0.2744 0.4292 0.5656 0.055 Uiso 1 1 calc R . . C45 C 0.1611(7) 0.3179(6) 0.5489(4) 0.045(2) Uani 1 1 d . . . C46 C 0.1288(7) 0.2283(6) 0.5153(4) 0.045(2) Uani 1 1 d . . . H61 H 0.0696 0.1891 0.5208 0.054 Uiso 1 1 calc R . . C47 C 0.1790(7) 0.1937(6) 0.4742(3) 0.039(2) Uani 1 1 d . . . C48 C 0.4023(9) 0.3965(7) 0.4956(5) 0.074(3) Uani 1 1 d . . . H68 H 0.4251 0.4511 0.5277 0.112 Uiso 1 1 calc R . . H69 H 0.3886 0.4181 0.4548 0.112 Uiso 1 1 calc R . . H70 H 0.4580 0.3575 0.5008 0.112 Uiso 1 1 calc R . . C49 C 0.1057(8) 0.3522(7) 0.5939(4) 0.060(3) Uani 1 1 d . . . H65 H 0.1389 0.3350 0.6348 0.090 Uiso 1 1 calc R . . H66 H 0.0308 0.3231 0.5798 0.090 Uiso 1 1 calc R . . H67 H 0.1112 0.4208 0.5966 0.090 Uiso 1 1 calc R . . C50 C 0.1438(8) 0.0946(6) 0.4405(4) 0.061(3) Uani 1 1 d . . . H62 H 0.0897 0.0611 0.4562 0.092 Uiso 1 1 calc R . . H63 H 0.2047 0.0614 0.4472 0.092 Uiso 1 1 calc R . . H64 H 0.1142 0.0970 0.3961 0.092 Uiso 1 1 calc R . . C51 C 0.5299(9) -0.1272(9) 0.4348(4) 0.077(3) Uani 1 1 d . . . H71 H 0.4736 -0.1767 0.4371 0.116 Uiso 1 1 calc R . . H72 H 0.5075 -0.0657 0.4389 0.116 Uiso 1 1 calc R . . H73 H 0.5945 -0.1282 0.4682 0.116 Uiso 1 1 calc R . . C52 C 0.5863(13) -0.2270(10) 0.3682(6) 0.109(5) Uani 1 1 d . . . H74 H 0.5328 -0.2784 0.3726 0.131 Uiso 1 1 calc R . . H75 H 0.6518 -0.2261 0.4022 0.131 Uiso 1 1 calc R . . C53 C 0.6084(8) -0.2507(7) 0.3124(5) 0.062(3) Uani 1 1 d . . . H76 H 0.6121 -0.3187 0.3072 0.075 Uiso 1 1 calc R . . H77 H 0.6783 -0.2153 0.3139 0.075 Uiso 1 1 calc R . . C54 C 0.5354(8) -0.2755(7) 0.2036(5) 0.063(3) Uani 1 1 d . . . H78 H 0.6071 -0.2593 0.1999 0.095 Uiso 1 1 calc R . . H79 H 0.4846 -0.2544 0.1694 0.095 Uiso 1 1 calc R . . H80 H 0.5179 -0.3440 0.2021 0.095 Uiso 1 1 calc R . . C55 C 0.7140(11) 0.3673(7) 0.4623(4) 0.086(4) Uani 1 1 d . . . H83 H 0.7308 0.3245 0.4935 0.129 Uiso 1 1 calc R . . H82 H 0.6378 0.3547 0.4412 0.129 Uiso 1 1 calc R . . H81 H 0.7344 0.4327 0.4825 0.129 Uiso 1 1 calc R . . C56 C 0.8790(10) 0.3650(8) 0.4468(5) 0.085(4) Uani 1 1 d . . . H84 H 0.8938 0.3187 0.4765 0.102 Uiso 1 1 calc R . . H85 H 0.9031 0.4290 0.4702 0.102 Uiso 1 1 calc R . . C57 C 0.9366(8) 0.3523(7) 0.4007(6) 0.076(4) Uani 1 1 d . . . H86 H 0.9247 0.4005 0.3722 0.091 Uiso 1 1 calc R . . H87 H 1.0135 0.3596 0.4216 0.091 Uiso 1 1 calc R . . C58 C 0.9592(8) 0.2309(9) 0.3284(5) 0.080(4) Uani 1 1 d . . . H89 H 0.9620 0.2762 0.2989 0.120 Uiso 1 1 calc R . . H88 H 0.9272 0.1682 0.3057 0.120 Uiso 1 1 calc R . . H90 H 1.0312 0.2291 0.3541 0.120 Uiso 1 1 calc R . . C59 C 0.0394(8) 0.0553(8) 0.2416(4) 0.065(3) Uani 1 1 d . . . H92 H 0.0009 0.1057 0.2263 0.098 Uiso 1 1 calc R . . H91 H 0.1055 0.0827 0.2735 0.098 Uiso 1 1 calc R . . H93 H -0.0045 0.0124 0.2592 0.098 Uiso 1 1 calc R . . C60 C -0.0276(7) -0.0205(9) 0.1404(4) 0.073(4) Uani 1 1 d . . . H94 H -0.0492 0.0366 0.1228 0.087 Uiso 1 1 calc R . . H95 H -0.0873 -0.0534 0.1527 0.087 Uiso 1 1 calc R . . C61 C -0.0026(8) -0.0818(7) 0.0945(5) 0.071(3) Uani 1 1 d . . . H96 H -0.0660 -0.1022 0.0584 0.085 Uiso 1 1 calc R . . H97 H 0.0202 -0.1385 0.1121 0.085 Uiso 1 1 calc R . . C62 C 0.0972(9) -0.0771(9) 0.0228(4) 0.087(4) Uani 1 1 d . . . H98 H 0.1104 -0.1408 0.0303 0.130 Uiso 1 1 calc R . . H99 H 0.1582 -0.0422 0.0136 0.130 Uiso 1 1 calc R . . H100 H 0.0337 -0.0810 -0.0123 0.130 Uiso 1 1 calc R . . C63 C 0.3161(9) 0.5181(11) 0.1973(7) 0.117(6) Uani 1 1 d . . . H101 H 0.3287 0.5871 0.2018 0.176 Uiso 1 1 calc R . . H102 H 0.3253 0.4971 0.2380 0.176 Uiso 1 1 calc R . . H103 H 0.2437 0.4942 0.1711 0.176 Uiso 1 1 calc R . . C64 C 0.3678(9) 0.4905(6) 0.1049(4) 0.061(3) Uani 1 1 d . . . H104 H 0.3416 0.5503 0.0959 0.074 Uiso 1 1 calc R . . H105 H 0.3124 0.4377 0.0807 0.074 Uiso 1 1 calc R . . C65 C 0.4640(10) 0.4879(7) 0.0872(4) 0.064(3) Uani 1 1 d . . . H106 H 0.4490 0.4905 0.0423 0.077 Uiso 1 1 calc R . . H107 H 0.5176 0.5434 0.1092 0.077 Uiso 1 1 calc R . . C66 C 0.5928(9) 0.3970(8) 0.0788(4) 0.073(3) Uani 1 1 d . . . H108 H 0.5703 0.3927 0.0336 0.109 Uiso 1 1 calc R . . H109 H 0.6208 0.3400 0.0911 0.109 Uiso 1 1 calc R . . H110 H 0.6480 0.4522 0.0961 0.109 Uiso 1 1 calc R . . C67 C 1.1727(9) -0.1552(7) 0.4332(5) 0.075(3) Uani 1 1 d . . . H111 H 1.2483 -0.1284 0.4457 0.113 Uiso 1 1 calc R . . H112 H 1.1438 -0.1432 0.4679 0.113 Uiso 1 1 calc R . . H113 H 1.1351 -0.1261 0.3981 0.113 Uiso 1 1 calc R . . C68 C 1.2199(9) -0.2778(8) 0.3746(5) 0.077(3) Uani 1 1 d . . . H114 H 1.2096 -0.2374 0.3411 0.093 Uiso 1 1 calc R . . H115 H 1.2963 -0.2666 0.3975 0.093 Uiso 1 1 calc R . . C69 C 1.1880(13) -0.3748(9) 0.3481(5) 0.102(5) Uani 1 1 d . . . H117 H 1.1104 -0.3876 0.3287 0.123 Uiso 1 1 calc R . . H116 H 1.2226 -0.3874 0.3155 0.123 Uiso 1 1 calc R . . C70 C 1.1930(14) -0.5281(9) 0.3687(6) 0.122(6) Uani 1 1 d . . . H118 H 1.1161 -0.5480 0.3528 0.183 Uiso 1 1 calc R . . H119 H 1.2222 -0.5656 0.4012 0.183 Uiso 1 1 calc R . . H120 H 1.2249 -0.5375 0.3350 0.183 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 Ba1 0.0314(3) 0.0224(2) 0.0294(2) 0.00597(16) 0.00619(18) 0.00688(19) O1 0.030(3) 0.022(3) 0.048(3) 0.014(2) -0.004(2) 0.005(2) C1 0.070(8) 0.081(9) 0.076(7) 0.017(6) 0.013(6) 0.010(7) Ba2 0.0445(3) 0.0392(3) 0.0346(2) 0.0051(2) 0.0144(2) 0.0091(2) O2 0.040(3) 0.026(3) 0.031(2) 0.011(2) 0.015(2) 0.004(2) C2 0.054(6) 0.025(4) 0.038(4) 0.011(3) 0.022(4) 0.004(4) Ba3 0.0297(3) 0.0265(3) 0.0270(2) 0.00379(17) 0.00312(18) 0.0043(2) O3 0.038(3) 0.033(3) 0.025(2) 0.006(2) 0.007(2) 0.004(2) C3 0.056(6) 0.056(6) 0.043(5) 0.004(4) 0.017(4) 0.020(5) Ba4 0.0284(3) 0.0235(2) 0.02440(19) 0.00313(16) 0.00656(17) 0.00523(19) O4 0.043(3) 0.022(3) 0.032(2) 0.000(2) 0.012(2) 0.004(2) C4 0.047(5) 0.026(4) 0.043(4) -0.005(3) 0.015(4) 0.002(4) Ba5 0.0291(3) 0.0222(2) 0.02539(19) 0.00577(16) 0.00634(17) 0.00614(19) O5 0.034(3) 0.027(3) 0.032(2) 0.006(2) 0.013(2) 0.014(2) C5 0.055(6) 0.063(6) 0.043(5) 0.013(4) 0.025(4) 0.031(5) O6 0.028(3) 0.038(3) 0.036(3) 0.008(2) 0.010(2) 0.003(2) C6 0.035(5) 0.039(5) 0.028(3) 0.010(3) 0.011(3) 0.011(4) O7 0.028(3) 0.036(3) 0.039(3) 0.004(2) 0.005(2) 0.009(2) C7 0.034(5) 0.035(5) 0.031(4) 0.009(3) 0.004(3) 0.006(4) O8 0.041(3) 0.030(3) 0.029(2) -0.001(2) 0.008(2) 0.007(2) C8 0.037(5) 0.040(5) 0.046(5) 0.013(4) 0.001(4) -0.001(4) O9 0.032(3) 0.041(3) 0.028(2) 0.005(2) 0.006(2) 0.007(2) C9 0.031(5) 0.055(6) 0.050(5) 0.024(4) 0.010(4) 0.009(4) O10 0.066(5) 0.058(4) 0.051(4) 0.013(3) 0.021(3) 0.014(4) C10 0.040(5) 0.059(6) 0.048(5) 0.025(4) 0.020(4) 0.027(5) O11 0.061(4) 0.053(4) 0.053(4) 0.026(3) 0.016(3) 0.019(3) C11 0.039(5) 0.032(5) 0.039(4) 0.017(3) 0.013(4) 0.008(4) O12 0.051(4) 0.041(4) 0.063(4) 0.014(3) 0.012(3) 0.018(3) C12 0.039(5) 0.041(5) 0.057(5) -0.006(4) 0.013(4) -0.002(4) O13 0.093(6) 0.043(4) 0.041(3) -0.006(3) -0.017(4) 0.014(4) C13 0.034(6) 0.082(8) 0.085(7) 0.040(6) 0.017(5) 0.009(5) O14 0.042(4) 0.060(5) 0.059(4) 0.019(3) -0.006(3) -0.005(3) C14 0.064(7) 0.060(6) 0.048(5) 0.022(4) 0.027(5) 0.028(5) O15 0.036(4) 0.074(5) 0.047(3) 0.010(3) 0.007(3) -0.018(3) C15 0.026(4) 0.026(4) 0.040(4) 0.007(3) 0.008(3) 0.002(3) O16 0.046(4) 0.061(4) 0.031(3) -0.010(3) -0.003(3) 0.023(3) C16 0.034(5) 0.038(5) 0.032(4) 0.009(3) 0.012(3) 0.009(4) O17 0.050(4) 0.037(4) 0.067(4) 0.019(3) 0.018(3) 0.020(3) C17 0.035(5) 0.040(5) 0.033(4) 0.007(3) -0.002(3) 0.012(4) O18 0.059(4) 0.045(4) 0.042(3) 0.013(3) 0.009(3) 0.010(3) C18 0.032(5) 0.038(5) 0.043(4) 0.002(3) 0.010(4) 0.008(4) O19 0.117(7) 0.057(5) 0.074(5) 0.012(4) 0.029(5) 0.018(5) C19 0.045(5) 0.030(5) 0.036(4) -0.003(3) 0.014(4) 0.001(4) O20 0.197(11) 0.084(7) 0.070(6) 0.012(5) 0.016(6) 0.046(7) C20 0.035(5) 0.019(4) 0.036(4) 0.004(3) 0.006(3) -0.003(3) C21 0.048(6) 0.045(5) 0.039(4) 0.009(4) 0.004(4) 0.016(4) C22 0.051(6) 0.052(6) 0.057(5) -0.003(4) 0.014(5) 0.014(5) C23 0.069(7) 0.038(5) 0.035(4) 0.000(4) -0.007(4) 0.010(5) C24 0.022(4) 0.024(4) 0.038(4) 0.002(3) 0.010(3) 0.010(3) C25 0.042(5) 0.030(4) 0.031(4) 0.004(3) 0.011(3) 0.018(4) C26 0.043(5) 0.023(4) 0.044(4) 0.008(3) 0.006(4) 0.011(4) C27 0.047(6) 0.032(5) 0.033(4) -0.001(3) -0.005(4) 0.016(4) C28 0.044(5) 0.059(6) 0.027(4) 0.001(4) 0.000(3) 0.034(5) C29 0.029(4) 0.039(5) 0.039(4) 0.007(3) 0.010(3) 0.017(4) C30 0.061(6) 0.029(5) 0.046(5) 0.005(4) 0.012(4) -0.001(4) C31 0.075(7) 0.047(6) 0.039(5) -0.007(4) -0.010(4) 0.018(5) C32 0.040(5) 0.080(7) 0.040(4) 0.010(4) 0.019(4) 0.023(5) C33 0.036(5) 0.027(4) 0.021(3) 0.001(3) 0.003(3) -0.005(3) C34 0.035(5) 0.033(5) 0.030(4) 0.003(3) 0.006(3) 0.003(4) C35 0.046(5) 0.032(5) 0.037(4) -0.002(3) -0.005(4) 0.007(4) C36 0.080(7) 0.023(4) 0.021(3) -0.006(3) -0.001(4) 0.014(4) C37 0.068(6) 0.030(5) 0.029(4) 0.002(3) 0.017(4) 0.010(4) C38 0.053(6) 0.030(5) 0.037(4) 0.006(3) 0.016(4) 0.012(4) C39 0.040(6) 0.066(7) 0.051(5) 0.010(4) 0.012(4) 0.011(5) C40 0.141(11) 0.042(6) 0.030(4) 0.008(4) 0.006(5) 0.037(6) C41 0.068(7) 0.056(6) 0.047(5) 0.013(4) 0.035(5) 0.020(5) C42 0.049(6) 0.041(5) 0.027(4) 0.012(3) 0.009(4) 0.018(4) C43 0.055(6) 0.033(5) 0.055(5) 0.023(4) 0.011(4) 0.003(4) C44 0.062(7) 0.031(5) 0.043(4) 0.001(4) 0.013(4) 0.006(4) C45 0.042(5) 0.046(6) 0.037(4) 0.002(4) 0.000(4) -0.001(4) C46 0.042(5) 0.049(6) 0.041(4) 0.001(4) 0.009(4) 0.007(4) C47 0.033(5) 0.036(5) 0.039(4) 0.004(3) -0.005(4) 0.002(4) C48 0.093(9) 0.048(7) 0.089(8) 0.011(6) 0.046(7) -0.006(6) C49 0.068(7) 0.061(7) 0.049(5) -0.005(4) 0.019(5) 0.010(5) C50 0.055(7) 0.051(6) 0.062(6) -0.016(5) 0.002(5) 0.004(5) C51 0.085(9) 0.103(10) 0.043(5) 0.016(5) 0.013(5) 0.017(7) C52 0.134(13) 0.115(12) 0.096(10) 0.035(9) 0.030(9) 0.076(11) C53 0.053(7) 0.047(6) 0.088(8) 0.024(5) 0.011(6) 0.022(5) C54 0.054(7) 0.045(6) 0.080(7) -0.014(5) 0.006(5) 0.015(5) C55 0.169(13) 0.057(7) 0.033(5) 0.003(4) 0.018(6) 0.047(8) C56 0.102(10) 0.046(7) 0.067(7) -0.007(5) -0.026(7) -0.011(7) C57 0.047(7) 0.056(7) 0.094(8) 0.023(6) -0.019(6) -0.025(5) C58 0.034(6) 0.133(11) 0.074(7) 0.054(7) 0.008(5) 0.009(7) C59 0.054(7) 0.091(8) 0.054(6) 0.012(5) 0.028(5) -0.004(6) C60 0.037(6) 0.118(10) 0.044(5) 0.015(6) 0.003(4) -0.033(6) C61 0.058(7) 0.056(7) 0.070(7) 0.010(5) -0.016(6) -0.014(6) C62 0.071(8) 0.131(11) 0.050(6) -0.020(6) -0.013(5) 0.070(8) C63 0.072(9) 0.179(15) 0.179(14) 0.121(12) 0.103(10) 0.084(10) C64 0.083(8) 0.026(5) 0.057(6) 0.008(4) -0.017(5) 0.023(5) C65 0.105(10) 0.052(7) 0.046(5) 0.020(4) 0.029(6) 0.025(6) C66 0.075(8) 0.096(9) 0.053(6) 0.027(6) 0.030(6) 0.000(7) C67 0.084(9) 0.057(8) 0.074(7) 0.005(6) 0.010(6) 0.005(6) C68 0.076(9) 0.072(8) 0.077(8) -0.003(6) 0.017(6) 0.007(7) C69 0.175(15) 0.080(10) 0.056(7) 0.016(6) 0.034(8) 0.029(10) C70 0.194(18) 0.061(9) 0.104(11) -0.008(8) 0.038(11) 0.017(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 Ba1 O8 2.657(5) . ? Ba1 O7 2.680(5) . ? Ba1 O2 2.681(5) . ? Ba1 O3 2.690(5) . ? Ba1 O1 2.774(5) . ? Ba1 O11 2.823(6) . ? Ba1 O12 2.885(6) . ? O1 C1 1.565(12) . ? O1 Ba5 2.696(5) . ? O1 Ba4 2.786(5) . ? O1 Ba3 2.858(5) . ? O1 Ba2 3.184(6) . ? C1 H1 0.9800 . ? C1 H2 0.9800 . ? C1 H3 0.9800 . ? Ba2 O10 2.432(6) . ? Ba2 O3 2.582(5) . ? Ba2 O2 2.586(5) . ? Ba2 O5 2.591(5) . ? Ba2 O4 2.607(5) . ? O2 C2 1.381(8) . ? O2 Ba4 2.644(4) . ? C2 H5 0.9800 . ? C2 H4 0.9800 . ? C2 H6 0.9800 . ? Ba3 O7 2.632(5) . ? Ba3 O6 2.637(5) . ? Ba3 O3 2.657(5) . ? Ba3 O4 2.674(5) . ? Ba3 O14 2.827(6) . ? Ba3 O13 2.860(6) . ? O3 C3 1.414(9) . ? C3 H7 0.9800 . ? C3 H8 0.9800 . ? C3 H9 0.9800 . ? Ba4 O9 2.612(5) . ? Ba4 O8 2.683(5) . ? Ba4 O5 2.686(5) . ? Ba4 O16 2.824(5) . ? Ba4 O15 2.829(6) . ? O4 C4 1.391(8) . ? O4 Ba5 2.695(5) . ? C4 H10 0.9800 . ? C4 H11 0.9800 . ? C4 H12 0.9800 . ? Ba5 O6 2.624(5) . ? Ba5 O9 2.707(5) . ? Ba5 O5 2.727(5) . ? Ba5 O18 2.886(6) . ? Ba5 O17 2.891(5) . ? O5 C5 1.374(9) . ? C5 H13 0.9800 . ? C5 H14 0.9800 . ? C5 H15 0.9800 . ? O6 C6 1.338(9) . ? C6 C7 1.387(11) . ? C6 C11 1.396(10) . ? O7 C15 1.330(9) . ? C7 C8 1.405(11) . ? C7 C12 1.500(11) . ? O8 C24 1.326(8) . ? C8 C9 1.391(12) . ? C8 H16 0.9500 . ? O9 C33 1.324(8) . ? C9 C10 1.365(12) . ? C9 C13 1.512(12) . ? O10 C42 1.302(9) . ? C10 C11 1.387(11) . ? C10 H17 0.9500 . ? O11 C52 1.381(13) . ? O11 C51 1.416(11) . ? C11 C14 1.515(11) . ? O12 C53 1.411(11) . ? O12 C54 1.434(10) . ? C12 H18 0.9800 . ? C12 H19 0.9800 . ? C12 H20 0.9800 . ? O13 C56 1.375(13) . ? O13 C55 1.450(12) . ? C13 H21 0.9800 . ? C13 H22 0.9800 . ? C13 H23 0.9800 . ? O14 C58 1.400(12) . ? O14 C57 1.461(12) . ? C14 H25 0.9800 . ? C14 H26 0.9800 . ? C14 H24 0.9800 . ? O15 C59 1.393(10) . ? O15 C60 1.419(10) . ? C15 C16 1.391(10) . ? C15 C20 1.414(10) . ? O16 C62 1.403(10) . ? O16 C61 1.447(12) . ? C16 C17 1.395(10) . ? C16 C21 1.492(10) . ? O17 C63 1.408(11) . ? O17 C64 1.437(10) . ? C17 C18 1.378(10) . ? C17 H27 0.9500 . ? O18 C65 1.390(11) . ? O18 C66 1.443(11) . ? C18 C19 1.359(11) . ? C18 C22 1.505(11) . ? O19 C67 1.385(11) . ? O19 C68 1.452(13) . ? C19 C20 1.409(11) . ? C19 H28 0.9500 . ? O20 C70 1.377(13) . ? O20 C69 1.386(13) . ? C20 C23 1.510(10) . ? C21 H29 0.9800 . ? C21 H30 0.9800 . ? C21 H31 0.9800 . ? C22 H32 0.9800 . ? C22 H33 0.9800 . ? C22 H34 0.9800 . ? C23 H35 0.9800 . ? C23 H36 0.9800 . ? C23 H37 0.9800 . ? C24 C25 1.391(10) . ? C24 C29 1.427(10) . ? C25 C26 1.394(10) . ? C25 C30 1.504(10) . ? C26 C27 1.376(11) . ? C26 H38 0.9500 . ? C27 C28 1.391(12) . ? C27 C31 1.498(10) . ? C28 C29 1.390(11) . ? C28 H39 0.9500 . ? C29 C32 1.483(12) . ? C30 H40 0.9800 . ? C30 H41 0.9800 . ? C30 H42 0.9800 . ? C31 H43 0.9800 . ? C31 H44 0.9800 . ? C31 H45 0.9800 . ? C32 H46 0.9800 . ? C32 H47 0.9800 . ? C32 H48 0.9800 . ? C33 C38 1.392(10) . ? C33 C34 1.429(11) . ? C34 C35 1.394(10) . ? C34 C39 1.489(11) . ? C35 C36 1.395(12) . ? C35 H49 0.9500 . ? C36 C37 1.352(12) . ? C36 C40 1.518(11) . ? C37 C38 1.402(10) . ? C37 H50 0.9500 . ? C38 C41 1.494(11) . ? C39 H51 0.9800 . ? C39 H52 0.9800 . ? C39 H53 0.9800 . ? C40 H54 0.9800 . ? C40 H55 0.9800 . ? C40 H56 0.9800 . ? C41 H57 0.9800 . ? C41 H58 0.9800 . ? C41 H59 0.9800 . ? C42 C47 1.403(12) . ? C42 C43 1.411(11) . ? C43 C44 1.393(12) . ? C43 C48 1.511(13) . ? C44 C45 1.348(12) . ? C44 H60 0.9500 . ? C45 C46 1.393(11) . ? C45 C49 1.505(12) . ? C46 C47 1.386(11) . ? C46 H61 0.9500 . ? C47 C50 1.513(11) . ? C48 H68 0.9800 . ? C48 H69 0.9800 . ? C48 H70 0.9800 . ? C49 H65 0.9800 . ? C49 H66 0.9800 . ? C49 H67 0.9800 . ? C50 H62 0.9800 . ? C50 H63 0.9800 . ? C50 H64 0.9800 . ? C51 H71 0.9800 . ? C51 H72 0.9800 . ? C51 H73 0.9800 . ? C52 C53 1.402(15) . ? C52 H74 0.9900 . ? C52 H75 0.9900 . ? C53 H76 0.9900 . ? C53 H77 0.9900 . ? C54 H78 0.9800 . ? C54 H79 0.9800 . ? C54 H80 0.9800 . ? C55 H83 0.9800 . ? C55 H82 0.9800 . ? C55 H81 0.9800 . ? C56 C57 1.473(16) . ? C56 H84 0.9900 . ? C56 H85 0.9900 . ? C57 H86 0.9900 . ? C57 H87 0.9900 . ? C58 H89 0.9800 . ? C58 H88 0.9800 . ? C58 H90 0.9800 . ? C59 H92 0.9800 . ? C59 H91 0.9800 . ? C59 H93 0.9800 . ? C60 C61 1.446(14) . ? C60 H94 0.9900 . ? C60 H95 0.9900 . ? C61 H96 0.9900 . ? C61 H97 0.9900 . ? C62 H98 0.9800 . ? C62 H99 0.9800 . ? C62 H100 0.9800 . ? C63 H101 0.9800 . ? C63 H102 0.9800 . ? C63 H103 0.9800 . ? C64 C65 1.448(14) . ? C64 H104 0.9900 . ? C64 H105 0.9900 . ? C65 H106 0.9900 . ? C65 H107 0.9900 . ? C66 H108 0.9800 . ? C66 H109 0.9800 . ? C66 H110 0.9800 . ? C67 H111 0.9800 . ? C67 H112 0.9800 . ? C67 H113 0.9800 . ? C68 C69 1.434(15) . ? C68 H114 0.9900 . ? C68 H115 0.9900 . ? C69 H117 0.9900 . ? C69 H116 0.9900 . ? C70 H118 0.9800 . ? C70 H119 0.9800 . ? C70 H120 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O8 Ba1 O7 116.43(15) . . ? O8 Ba1 O2 74.80(14) . . ? O7 Ba1 O2 138.13(15) . . ? O8 Ba1 O3 140.10(15) . . ? O7 Ba1 O3 74.09(15) . . ? O2 Ba1 O3 74.10(15) . . ? O8 Ba1 O1 76.29(15) . . ? O7 Ba1 O1 75.06(15) . . ? O2 Ba1 O1 68.72(15) . . ? O3 Ba1 O1 69.51(14) . . ? O8 Ba1 O11 127.95(17) . . ? O7 Ba1 O11 99.84(17) . . ? O2 Ba1 O11 102.67(16) . . ? O3 Ba1 O11 83.18(17) . . ? O1 Ba1 O11 152.62(17) . . ? O8 Ba1 O12 81.71(16) . . ? O7 Ba1 O12 95.93(17) . . ? O2 Ba1 O12 125.95(16) . . ? O3 Ba1 O12 137.48(16) . . ? O1 Ba1 O12 148.90(17) . . ? O11 Ba1 O12 57.41(18) . . ? C1 O1 Ba5 92.0(5) . . ? C1 O1 Ba1 94.7(5) . . ? Ba5 O1 Ba1 173.2(2) . . ? C1 O1 Ba4 95.4(5) . . ? Ba5 O1 Ba4 90.64(14) . . ? Ba1 O1 Ba4 89.38(14) . . ? C1 O1 Ba3 98.5(5) . . ? Ba5 O1 Ba3 89.58(14) . . ? Ba1 O1 Ba3 88.76(13) . . ? Ba4 O1 Ba3 166.0(2) . . ? C1 O1 Ba2 179.0(5) . . ? Ba5 O1 Ba2 87.62(14) . . ? Ba1 O1 Ba2 85.64(14) . . ? Ba4 O1 Ba2 83.64(14) . . ? Ba3 O1 Ba2 82.40(13) . . ? O1 C1 H1 109.5 . . ? O1 C1 H2 109.5 . . ? H1 C1 H2 109.5 . . ? O1 C1 H3 109.5 . . ? H1 C1 H3 109.5 . . ? H2 C1 H3 109.5 . . ? O10 Ba2 O3 117.24(18) . . ? O10 Ba2 O2 109.66(19) . . ? O3 Ba2 O2 77.54(16) . . ? O10 Ba2 O5 114.11(18) . . ? O3 Ba2 O5 128.28(14) . . ? O2 Ba2 O5 80.21(15) . . ? O10 Ba2 O4 122.84(18) . . ? O3 Ba2 O4 80.78(16) . . ? O2 Ba2 O4 127.44(14) . . ? O5 Ba2 O4 76.91(15) . . ? O10 Ba2 O1 172.90(18) . . ? O3 Ba2 O1 64.44(13) . . ? O2 Ba2 O1 63.53(13) . . ? O5 Ba2 O1 63.84(13) . . ? O4 Ba2 O1 63.91(13) . . ? C2 O2 Ba2 108.8(4) . . ? C2 O2 Ba4 140.4(5) . . ? Ba2 O2 Ba4 99.51(16) . . ? C2 O2 Ba1 106.3(4) . . ? Ba2 O2 Ba1 100.88(17) . . ? Ba4 O2 Ba1 94.51(14) . . ? O2 C2 H5 109.5 . . ? O2 C2 H4 109.5 . . ? H5 C2 H4 109.5 . . ? O2 C2 H6 109.5 . . ? H5 C2 H6 109.5 . . ? H4 C2 H6 109.5 . . ? O7 Ba3 O6 105.85(15) . . ? O7 Ba3 O3 75.43(16) . . ? O6 Ba3 O3 138.70(15) . . ? O7 Ba3 O4 139.96(15) . . ? O6 Ba3 O4 75.85(15) . . ? O3 Ba3 O4 78.23(15) . . ? O7 Ba3 O14 89.90(18) . . ? O6 Ba3 O14 102.47(17) . . ? O3 Ba3 O14 118.83(17) . . ? O4 Ba3 O14 129.46(18) . . ? O7 Ba3 O1 74.39(15) . . ? O6 Ba3 O1 72.02(15) . . ? O3 Ba3 O1 68.70(14) . . ? O4 Ba3 O1 68.16(14) . . ? O14 Ba3 O1 160.66(18) . . ? O7 Ba3 O13 136.21(17) . . ? O6 Ba3 O13 109.08(17) . . ? O3 Ba3 O13 94.36(18) . . ? O4 Ba3 O13 75.02(18) . . ? O14 Ba3 O13 57.5(2) . . ? O1 Ba3 O13 141.74(19) . . ? C3 O3 Ba2 112.4(4) . . ? C3 O3 Ba3 107.3(5) . . ? Ba2 O3 Ba3 99.11(16) . . ? C3 O3 Ba1 135.8(5) . . ? Ba2 O3 Ba1 100.70(16) . . ? Ba3 O3 Ba1 94.92(14) . . ? O3 C3 H7 109.5 . . ? O3 C3 H8 109.5 . . ? H7 C3 H8 109.5 . . ? O3 C3 H9 109.5 . . ? H7 C3 H9 109.5 . . ? H8 C3 H9 109.5 . . ? O9 Ba4 O2 142.36(15) . . ? O9 Ba4 O8 112.58(15) . . ? O2 Ba4 O8 74.98(14) . . ? O9 Ba4 O5 75.27(14) . . ? O2 Ba4 O5 77.47(14) . . ? O8 Ba4 O5 140.94(14) . . ? O9 Ba4 O1 77.12(15) . . ? O2 Ba4 O1 69.06(15) . . ? O8 Ba4 O1 75.68(15) . . ? O5 Ba4 O1 68.86(15) . . ? O9 Ba4 O16 89.70(17) . . ? O2 Ba4 O16 127.68(17) . . ? O8 Ba4 O16 91.68(15) . . ? O5 Ba4 O16 127.23(15) . . ? O1 Ba4 O16 156.18(17) . . ? O9 Ba4 O15 126.57(17) . . ? O2 Ba4 O15 78.96(16) . . ? O8 Ba4 O15 110.13(18) . . ? O5 Ba4 O15 90.90(17) . . ? O1 Ba4 O15 144.92(16) . . ? O16 Ba4 O15 58.34(17) . . ? C4 O4 Ba2 110.7(4) . . ? C4 O4 Ba3 143.2(5) . . ? Ba2 O4 Ba3 98.05(16) . . ? C4 O4 Ba5 102.7(4) . . ? Ba2 O4 Ba5 100.80(16) . . ? Ba3 O4 Ba5 93.64(14) . . ? O4 C4 H10 109.5 . . ? O4 C4 H11 109.5 . . ? H10 C4 H11 109.5 . . ? O4 C4 H12 109.5 . . ? H10 C4 H12 109.5 . . ? H11 C4 H12 109.5 . . ? O6 Ba5 O4 75.71(15) . . ? O6 Ba5 O1 74.91(16) . . ? O4 Ba5 O1 70.30(15) . . ? O6 Ba5 O9 118.60(15) . . ? O4 Ba5 O9 139.34(15) . . ? O1 Ba5 O9 77.10(15) . . ? O6 Ba5 O5 138.80(15) . . ? O4 Ba5 O5 73.21(15) . . ? O1 Ba5 O5 69.59(15) . . ? O9 Ba5 O5 73.08(14) . . ? O6 Ba5 O18 74.57(16) . . ? O4 Ba5 O18 131.90(16) . . ? O1 Ba5 O18 134.03(17) . . ? O9 Ba5 O18 88.40(15) . . ? O5 Ba5 O18 146.49(16) . . ? O6 Ba5 O17 113.02(17) . . ? O4 Ba5 O17 104.30(16) . . ? O1 Ba5 O17 169.53(17) . . ? O9 Ba5 O17 103.57(16) . . ? O5 Ba5 O17 100.45(15) . . ? O18 Ba5 O17 56.30(17) . . ? C5 O5 Ba2 103.0(4) . . ? C5 O5 Ba4 132.9(5) . . ? Ba2 O5 Ba4 98.27(15) . . ? C5 O5 Ba5 123.9(5) . . ? Ba2 O5 Ba5 100.36(16) . . ? Ba4 O5 Ba5 92.14(14) . . ? O5 C5 H13 109.5 . . ? O5 C5 H14 109.5 . . ? H13 C5 H14 109.5 . . ? O5 C5 H15 109.5 . . ? H13 C5 H15 109.5 . . ? H14 C5 H15 109.5 . . ? C6 O6 Ba5 147.0(5) . . ? C6 O6 Ba3 110.4(4) . . ? Ba5 O6 Ba3 96.18(16) . . ? O6 C6 C7 120.6(7) . . ? O6 C6 C11 120.1(7) . . ? C7 C6 C11 119.3(8) . . ? C15 O7 Ba3 147.4(4) . . ? C15 O7 Ba1 112.8(4) . . ? Ba3 O7 Ba1 95.73(16) . . ? C6 C7 C8 119.0(7) . . ? C6 C7 C12 119.7(7) . . ? C8 C7 C12 121.2(7) . . ? C24 O8 Ba1 143.9(4) . . ? C24 O8 Ba4 118.5(4) . . ? Ba1 O8 Ba4 94.14(14) . . ? C9 C8 C7 121.6(8) . . ? C9 C8 H16 119.2 . . ? C7 C8 H16 119.2 . . ? C33 O9 Ba4 146.4(5) . . ? C33 O9 Ba5 112.7(4) . . ? Ba4 O9 Ba5 94.23(14) . . ? C10 C9 C8 118.2(8) . . ? C10 C9 C13 120.6(9) . . ? C8 C9 C13 121.2(9) . . ? C42 O10 Ba2 167.7(5) . . ? C9 C10 C11 121.7(8) . . ? C9 C10 H17 119.1 . . ? C11 C10 H17 119.1 . . ? C52 O11 C51 113.4(8) . . ? C52 O11 Ba1 119.0(7) . . ? C51 O11 Ba1 127.0(6) . . ? C10 C11 C6 120.2(8) . . ? C10 C11 C14 119.6(8) . . ? C6 C11 C14 120.2(7) . . ? C53 O12 C54 112.6(7) . . ? C53 O12 Ba1 111.4(5) . . ? C54 O12 Ba1 122.5(5) . . ? C7 C12 H18 109.5 . . ? C7 C12 H19 109.5 . . ? H18 C12 H19 109.5 . . ? C7 C12 H20 109.5 . . ? H18 C12 H20 109.5 . . ? H19 C12 H20 109.5 . . ? C56 O13 C55 110.5(8) . . ? C56 O13 Ba3 120.8(6) . . ? C55 O13 Ba3 118.5(6) . . ? C9 C13 H21 109.5 . . ? C9 C13 H22 109.5 . . ? H21 C13 H22 109.5 . . ? C9 C13 H23 109.5 . . ? H21 C13 H23 109.5 . . ? H22 C13 H23 109.5 . . ? C58 O14 C57 114.3(9) . . ? C58 O14 Ba3 115.4(5) . . ? C57 O14 Ba3 115.1(6) . . ? C11 C14 H25 109.5 . . ? C11 C14 H26 109.5 . . ? H25 C14 H26 109.5 . . ? C11 C14 H24 109.5 . . ? H25 C14 H24 109.5 . . ? H26 C14 H24 109.5 . . ? C59 O15 C60 112.1(8) . . ? C59 O15 Ba4 118.6(5) . . ? C60 O15 Ba4 117.8(5) . . ? O7 C15 C16 120.9(6) . . ? O7 C15 C20 120.4(7) . . ? C16 C15 C20 118.7(7) . . ? C62 O16 C61 112.4(8) . . ? C62 O16 Ba4 118.8(6) . . ? C61 O16 Ba4 115.8(5) . . ? C15 C16 C17 119.9(7) . . ? C15 C16 C21 120.1(7) . . ? C17 C16 C21 120.0(7) . . ? C63 O17 C64 114.9(8) . . ? C63 O17 Ba5 119.1(6) . . ? C64 O17 Ba5 109.4(4) . . ? C18 C17 C16 122.3(7) . . ? C18 C17 H27 118.9 . . ? C16 C17 H27 118.9 . . ? C65 O18 C66 111.0(8) . . ? C65 O18 Ba5 121.5(5) . . ? C66 O18 Ba5 125.5(5) . . ? C19 C18 C17 117.6(7) . . ? C19 C18 C22 120.0(7) . . ? C17 C18 C22 122.2(7) . . ? C67 O19 C68 113.8(9) . . ? C18 C19 C20 122.9(7) . . ? C18 C19 H28 118.5 . . ? C20 C19 H28 118.5 . . ? C70 O20 C69 113.4(10) . . ? C19 C20 C15 118.5(7) . . ? C19 C20 C23 119.7(7) . . ? C15 C20 C23 121.8(7) . . ? C16 C21 H29 109.5 . . ? C16 C21 H30 109.5 . . ? H29 C21 H30 109.5 . . ? C16 C21 H31 109.5 . . ? H29 C21 H31 109.5 . . ? H30 C21 H31 109.5 . . ? C18 C22 H32 109.5 . . ? C18 C22 H33 109.5 . . ? H32 C22 H33 109.5 . . ? C18 C22 H34 109.5 . . ? H32 C22 H34 109.5 . . ? H33 C22 H34 109.5 . . ? C20 C23 H35 109.5 . . ? C20 C23 H36 109.5 . . ? H35 C23 H36 109.5 . . ? C20 C23 H37 109.5 . . ? H35 C23 H37 109.5 . . ? H36 C23 H37 109.5 . . ? O8 C24 C25 121.1(6) . . ? O8 C24 C29 120.6(7) . . ? C25 C24 C29 118.3(7) . . ? C24 C25 C26 120.5(7) . . ? C24 C25 C30 119.1(7) . . ? C26 C25 C30 120.4(7) . . ? C27 C26 C25 122.7(8) . . ? C27 C26 H38 118.7 . . ? C25 C26 H38 118.7 . . ? C26 C27 C28 116.5(7) . . ? C26 C27 C31 122.2(9) . . ? C28 C27 C31 121.3(8) . . ? C29 C28 C27 123.6(7) . . ? C29 C28 H39 118.2 . . ? C27 C28 H39 118.2 . . ? C28 C29 C24 118.5(8) . . ? C28 C29 C32 121.8(7) . . ? C24 C29 C32 119.6(7) . . ? C25 C30 H40 109.5 . . ? C25 C30 H41 109.5 . . ? H40 C30 H41 109.5 . . ? C25 C30 H42 109.5 . . ? H40 C30 H42 109.5 . . ? H41 C30 H42 109.5 . . ? C27 C31 H43 109.5 . . ? C27 C31 H44 109.5 . . ? H43 C31 H44 109.5 . . ? C27 C31 H45 109.5 . . ? H43 C31 H45 109.5 . . ? H44 C31 H45 109.5 . . ? C29 C32 H46 109.5 . . ? C29 C32 H47 109.5 . . ? H46 C32 H47 109.5 . . ? C29 C32 H48 109.5 . . ? H46 C32 H48 109.5 . . ? H47 C32 H48 109.5 . . ? O9 C33 C38 121.8(7) . . ? O9 C33 C34 119.9(6) . . ? C38 C33 C34 118.2(7) . . ? C35 C34 C33 119.2(7) . . ? C35 C34 C39 120.9(8) . . ? C33 C34 C39 119.8(7) . . ? C34 C35 C36 122.0(8) . . ? C34 C35 H49 119.0 . . ? C36 C35 H49 119.0 . . ? C37 C36 C35 117.6(7) . . ? C37 C36 C40 121.4(8) . . ? C35 C36 C40 121.0(9) . . ? C36 C37 C38 123.3(8) . . ? C36 C37 H50 118.4 . . ? C38 C37 H50 118.4 . . ? C33 C38 C37 119.6(8) . . ? C33 C38 C41 119.1(7) . . ? C37 C38 C41 121.3(7) . . ? C34 C39 H51 109.5 . . ? C34 C39 H52 109.5 . . ? H51 C39 H52 109.5 . . ? C34 C39 H53 109.5 . . ? H51 C39 H53 109.5 . . ? H52 C39 H53 109.5 . . ? C36 C40 H54 109.5 . . ? C36 C40 H55 109.5 . . ? H54 C40 H55 109.5 . . ? C36 C40 H56 109.5 . . ? H54 C40 H56 109.5 . . ? H55 C40 H56 109.5 . . ? C38 C41 H57 109.5 . . ? C38 C41 H58 109.5 . . ? H57 C41 H58 109.5 . . ? C38 C41 H59 109.5 . . ? H57 C41 H59 109.5 . . ? H58 C41 H59 109.5 . . ? O10 C42 C47 121.2(8) . . ? O10 C42 C43 121.4(8) . . ? C47 C42 C43 117.3(7) . . ? C44 C43 C42 119.7(8) . . ? C44 C43 C48 122.6(8) . . ? C42 C43 C48 117.6(9) . . ? C45 C44 C43 123.8(8) . . ? C45 C44 H60 118.1 . . ? C43 C44 H60 118.1 . . ? C44 C45 C46 116.3(8) . . ? C44 C45 C49 122.3(8) . . ? C46 C45 C49 121.3(9) . . ? C47 C46 C45 122.9(9) . . ? C47 C46 H61 118.6 . . ? C45 C46 H61 118.6 . . ? C46 C47 C42 119.9(8) . . ? C46 C47 C50 121.1(8) . . ? C42 C47 C50 118.8(8) . . ? C43 C48 H68 109.5 . . ? C43 C48 H69 109.5 . . ? H68 C48 H69 109.5 . . ? C43 C48 H70 109.5 . . ? H68 C48 H70 109.5 . . ? H69 C48 H70 109.5 . . ? C45 C49 H65 109.5 . . ? C45 C49 H66 109.5 . . ? H65 C49 H66 109.5 . . ? C45 C49 H67 109.5 . . ? H65 C49 H67 109.5 . . ? H66 C49 H67 109.5 . . ? C47 C50 H62 109.5 . . ? C47 C50 H63 109.5 . . ? H62 C50 H63 109.5 . . ? C47 C50 H64 109.5 . . ? H62 C50 H64 109.5 . . ? H63 C50 H64 109.5 . . ? O11 C51 H71 109.5 . . ? O11 C51 H72 109.5 . . ? H71 C51 H72 109.5 . . ? O11 C51 H73 109.5 . . ? H71 C51 H73 109.5 . . ? H72 C51 H73 109.5 . . ? O11 C52 C53 118.5(11) . . ? O11 C52 H74 107.7 . . ? C53 C52 H74 107.7 . . ? O11 C52 H75 107.7 . . ? C53 C52 H75 107.7 . . ? H74 C52 H75 107.1 . . ? C52 C53 O12 111.8(9) . . ? C52 C53 H76 109.3 . . ? O12 C53 H76 109.3 . . ? C52 C53 H77 109.3 . . ? O12 C53 H77 109.3 . . ? H76 C53 H77 107.9 . . ? O12 C54 H78 109.5 . . ? O12 C54 H79 109.5 . . ? H78 C54 H79 109.5 . . ? O12 C54 H80 109.5 . . ? H78 C54 H80 109.5 . . ? H79 C54 H80 109.5 . . ? O13 C55 H83 109.5 . . ? O13 C55 H82 109.5 . . ? H83 C55 H82 109.5 . . ? O13 C55 H81 109.5 . . ? H83 C55 H81 109.5 . . ? H82 C55 H81 109.5 . . ? O13 C56 C57 109.7(9) . . ? O13 C56 H84 109.7 . . ? C57 C56 H84 109.7 . . ? O13 C56 H85 109.7 . . ? C57 C56 H85 109.7 . . ? H84 C56 H85 108.2 . . ? O14 C57 C56 108.7(8) . . ? O14 C57 H86 109.9 . . ? C56 C57 H86 109.9 . . ? O14 C57 H87 109.9 . . ? C56 C57 H87 109.9 . . ? H86 C57 H87 108.3 . . ? O14 C58 H89 109.5 . . ? O14 C58 H88 109.5 . . ? H89 C58 H88 109.5 . . ? O14 C58 H90 109.5 . . ? H89 C58 H90 109.5 . . ? H88 C58 H90 109.5 . . ? O15 C59 H92 109.5 . . ? O15 C59 H91 109.5 . . ? H92 C59 H91 109.5 . . ? O15 C59 H93 109.5 . . ? H92 C59 H93 109.5 . . ? H91 C59 H93 109.5 . . ? O15 C60 C61 109.6(9) . . ? O15 C60 H94 109.7 . . ? C61 C60 H94 109.7 . . ? O15 C60 H95 109.7 . . ? C61 C60 H95 109.7 . . ? H94 C60 H95 108.2 . . ? C60 C61 O16 108.4(8) . . ? C60 C61 H96 110.0 . . ? O16 C61 H96 110.0 . . ? C60 C61 H97 110.0 . . ? O16 C61 H97 110.0 . . ? H96 C61 H97 108.4 . . ? O16 C62 H98 109.5 . . ? O16 C62 H99 109.5 . . ? H98 C62 H99 109.5 . . ? O16 C62 H100 109.5 . . ? H98 C62 H100 109.5 . . ? H99 C62 H100 109.5 . . ? O17 C63 H101 109.5 . . ? O17 C63 H102 109.5 . . ? H101 C63 H102 109.5 . . ? O17 C63 H103 109.5 . . ? H101 C63 H103 109.5 . . ? H102 C63 H103 109.5 . . ? O17 C64 C65 109.7(8) . . ? O17 C64 H104 109.7 . . ? C65 C64 H104 109.7 . . ? O17 C64 H105 109.7 . . ? C65 C64 H105 109.7 . . ? H104 C64 H105 108.2 . . ? O18 C65 C64 110.1(8) . . ? O18 C65 H106 109.6 . . ? C64 C65 H106 109.6 . . ? O18 C65 H107 109.6 . . ? C64 C65 H107 109.6 . . ? H106 C65 H107 108.2 . . ? O18 C66 H108 109.5 . . ? O18 C66 H109 109.5 . . ? H108 C66 H109 109.5 . . ? O18 C66 H110 109.5 . . ? H108 C66 H110 109.5 . . ? H109 C66 H110 109.5 . . ? O19 C67 H111 109.5 . . ? O19 C67 H112 109.5 . . ? H111 C67 H112 109.5 . . ? O19 C67 H113 109.5 . . ? H111 C67 H113 109.5 . . ? H112 C67 H113 109.5 . . ? C69 C68 O19 111.9(11) . . ? C69 C68 H114 109.2 . . ? O19 C68 H114 109.2 . . ? C69 C68 H115 109.2 . . ? O19 C68 H115 109.2 . . ? H114 C68 H115 107.9 . . ? O20 C69 C68 111.2(11) . . ? O20 C69 H117 109.4 . . ? C68 C69 H117 109.4 . . ? O20 C69 H116 109.4 . . ? C68 C69 H116 109.4 . . ? H117 C69 H116 108.0 . . ? O20 C70 H118 109.5 . . ? O20 C70 H119 109.5 . . ? H118 C70 H119 109.5 . . ? O20 C70 H120 109.5 . . ? H118 C70 H120 109.5 . . ? H119 C70 H120 109.5 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.192 _refine_diff_density_min -2.047 _refine_diff_density_rms 0.164 data_c:\basad _database_code_depnum_ccdc_archive 'CCDC 716851' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C78 H114 Ba3 O12' _chemical_formula_sum 'C78 H114 Ba3 O12' _chemical_formula_weight 1655.71 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' Ba Ba -0.3244 2.2819 '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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.8770(6) _cell_length_b 12.2084(6) _cell_length_c 14.5630(7) _cell_angle_alpha 109.9770(10) _cell_angle_beta 97.9640(10) _cell_angle_gamma 97.9570(10) _cell_volume 1925.88(16) _cell_formula_units_Z 1 _cell_measurement_temperature 89(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.428 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 846 _exptl_absorpt_coefficient_mu 1.574 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8336 _exptl_absorpt_correction_T_max 0.8844 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 89(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker X8 Apex II CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19277 _diffrn_reflns_av_R_equivalents 0.0293 _diffrn_reflns_av_sigmaI/netI 0.0442 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.77 _diffrn_reflns_theta_max 27.50 _reflns_number_total 8799 _reflns_number_gt 7328 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART (Bruker)' _computing_cell_refinement 'Bruker SMART (Bruker)' _computing_data_reduction 'Bruker SAINT (Bruker)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 1999)' _computing_publication_material 'CIFTAB (Sheldrick, 1997)' _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^)+(0.0333P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8799 _refine_ls_number_parameters 430 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0425 _refine_ls_R_factor_gt 0.0322 _refine_ls_wR_factor_ref 0.0706 _refine_ls_wR_factor_gt 0.0672 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.028 _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 Ba1 Ba 0.5000 1.0000 0.5000 0.01336(6) Uani 1 2 d S . . O1 O 0.63179(17) 0.82721(18) 0.48271(14) 0.0200(4) Uani 1 1 d . . . C1 C 0.6700(2) 0.7540(2) 0.4081(2) 0.0162(6) Uani 1 1 d . . . Ba2 Ba 0.677340(14) 0.888700(14) 0.671060(12) 0.01528(5) Uani 1 1 d . . . O2 O 0.45876(17) 0.89558(17) 0.62727(15) 0.0195(4) Uani 1 1 d . . . C2 C 0.7889(3) 0.7697(2) 0.4040(2) 0.0175(6) Uani 1 1 d . . . O3 O 0.68772(17) 1.08958(17) 0.64861(14) 0.0196(4) Uani 1 1 d . . . C3 C 0.8252(3) 0.6959(3) 0.3225(2) 0.0230(7) Uani 1 1 d . . . H1 H 0.9054 0.7077 0.3204 0.028 Uiso 1 1 calc R . . O4 O 0.78784(18) 0.70035(18) 0.64348(16) 0.0252(5) Uani 1 1 d . . . C4 C 0.7489(3) 0.6058(3) 0.2442(2) 0.0255(7) Uani 1 1 d . . . O5 O 0.90140(17) 0.99646(18) 0.77283(15) 0.0224(5) Uani 1 1 d . . . C5 C 0.6329(3) 0.5886(3) 0.2508(2) 0.0228(6) Uani 1 1 d . . . H2 H 0.5793 0.5260 0.1985 0.027 Uiso 1 1 calc R . . O6 O 0.65670(19) 0.8486(2) 0.84931(16) 0.0269(5) Uani 1 1 d . . . C6 C 0.5918(3) 0.6596(2) 0.3309(2) 0.0195(6) Uani 1 1 d . . . C7 C 0.8730(3) 0.8684(3) 0.4873(2) 0.0252(7) Uani 1 1 d . . . H3 H 0.8814 0.8488 0.5475 0.038 Uiso 1 1 calc R . . H4 H 0.8440 0.9426 0.5007 0.038 Uiso 1 1 calc R . . H5 H 0.9486 0.8783 0.4682 0.038 Uiso 1 1 calc R . . C8 C 0.7881(4) 0.5309(3) 0.1527(3) 0.0457(10) Uani 1 1 d . . . H6 H 0.7319 0.4557 0.1190 0.069 Uiso 1 1 calc R . . H7 H 0.8643 0.5144 0.1726 0.069 Uiso 1 1 calc R . . H8 H 0.7936 0.5740 0.1072 0.069 Uiso 1 1 calc R . . C9 C 0.4660(3) 0.6392(3) 0.3345(2) 0.0271(7) Uani 1 1 d . . . H9 H 0.4241 0.5698 0.2762 0.041 Uiso 1 1 calc R . . H10 H 0.4350 0.7095 0.3342 0.041 Uiso 1 1 calc R . . H11 H 0.4562 0.6250 0.3955 0.041 Uiso 1 1 calc R . . C10 C 0.3889(2) 0.8685(3) 0.6837(2) 0.0164(6) Uani 1 1 d . . . C11 C 0.3739(2) 0.7556(3) 0.6923(2) 0.0183(6) Uani 1 1 d . . . C12 C 0.3029(2) 0.7317(3) 0.7544(2) 0.0224(6) Uani 1 1 d . . . H12 H 0.2926 0.6552 0.7589 0.027 Uiso 1 1 calc R . . C13 C 0.2467(3) 0.8159(3) 0.8101(2) 0.0241(7) Uani 1 1 d . . . C14 C 0.2601(3) 0.9251(3) 0.7986(2) 0.0236(7) Uani 1 1 d . . . H13 H 0.2213 0.9834 0.8352 0.028 Uiso 1 1 calc R . . C15 C 0.3277(2) 0.9526(3) 0.7364(2) 0.0201(6) Uani 1 1 d . . . C16 C 0.4355(3) 0.6630(3) 0.6351(2) 0.0231(6) Uani 1 1 d . . . H14 H 0.5156 0.6783 0.6711 0.035 Uiso 1 1 calc R . . H15 H 0.4357 0.6664 0.5689 0.035 Uiso 1 1 calc R . . H16 H 0.3954 0.5840 0.6282 0.035 Uiso 1 1 calc R . . C17 C 0.1733(3) 0.7895(3) 0.8794(3) 0.0354(9) Uani 1 1 d . . . H17 H 0.1626 0.8644 0.9275 0.053 Uiso 1 1 calc R . . H18 H 0.2121 0.7458 0.9152 0.053 Uiso 1 1 calc R . . H19 H 0.0975 0.7414 0.8407 0.053 Uiso 1 1 calc R . . C18 C 0.3347(3) 1.0682(3) 0.7208(3) 0.0267(7) Uani 1 1 d . . . H20 H 0.2934 1.1196 0.7662 0.040 Uiso 1 1 calc R . . H21 H 0.2989 1.0533 0.6517 0.040 Uiso 1 1 calc R . . H22 H 0.4162 1.1076 0.7343 0.040 Uiso 1 1 calc R . . C19 C 0.7436(2) 1.1983(2) 0.7097(2) 0.0152(6) Uani 1 1 d . . . C20 C 0.7380(2) 1.2411(3) 0.8116(2) 0.0172(6) Uani 1 1 d . . . C21 C 0.7932(2) 1.3557(3) 0.8734(2) 0.0185(6) Uani 1 1 d . . . H23 H 0.7871 1.3832 0.9415 0.022 Uiso 1 1 calc R . . C22 C 0.8575(2) 1.4318(2) 0.8383(2) 0.0187(6) Uani 1 1 d . . . C23 C 0.8644(2) 1.3883(2) 0.7382(2) 0.0178(6) Uani 1 1 d . . . H24 H 0.9090 1.4384 0.7132 0.021 Uiso 1 1 calc R . . C24 C 0.8090(2) 1.2749(2) 0.6730(2) 0.0164(6) Uani 1 1 d . . . C25 C 0.6700(3) 1.1609(3) 0.8529(2) 0.0226(6) Uani 1 1 d . . . H25 H 0.7166 1.1051 0.8649 0.034 Uiso 1 1 calc R . . H26 H 0.5981 1.1164 0.8048 0.034 Uiso 1 1 calc R . . H27 H 0.6511 1.2092 0.9158 0.034 Uiso 1 1 calc R . . C26 C 0.9159(3) 1.5562(2) 0.9069(2) 0.0250(7) Uani 1 1 d . . . H28 H 0.8678 1.5879 0.9553 0.038 Uiso 1 1 calc R . . H29 H 0.9259 1.6068 0.8677 0.038 Uiso 1 1 calc R . . H30 H 0.9919 1.5550 0.9421 0.038 Uiso 1 1 calc R . . C27 C 0.8131(3) 1.2324(3) 0.5640(2) 0.0234(7) Uani 1 1 d . . . H31 H 0.7369 1.2271 0.5252 0.035 Uiso 1 1 calc R . . H32 H 0.8338 1.1538 0.5435 0.035 Uiso 1 1 calc R . . H33 H 0.8714 1.2885 0.5522 0.035 Uiso 1 1 calc R . . C28 C 0.7346(3) 0.5833(3) 0.5721(3) 0.0316(8) Uani 1 1 d . . . H34 H 0.6650 0.5865 0.5278 0.038 Uiso 1 1 calc R . . H35 H 0.7114 0.5291 0.6065 0.038 Uiso 1 1 calc R . . C29 C 0.8260(3) 0.5410(3) 0.5126(3) 0.0297(7) Uani 1 1 d . . . H36 H 0.8168 0.5585 0.4507 0.036 Uiso 1 1 calc R . . H37 H 0.8214 0.4544 0.4949 0.036 Uiso 1 1 calc R . . C30 C 0.9411(3) 0.6122(3) 0.5837(3) 0.0342(8) Uani 1 1 d . . . H38 H 0.9875 0.5585 0.6017 0.041 Uiso 1 1 calc R . . H39 H 0.9872 0.6583 0.5526 0.041 Uiso 1 1 calc R . . C31 C 0.9067(3) 0.6949(3) 0.6752(3) 0.0312(8) Uani 1 1 d . . . H40 H 0.9136 0.6632 0.7295 0.037 Uiso 1 1 calc R . . H41 H 0.9569 0.7749 0.6995 0.037 Uiso 1 1 calc R . . C32 C 0.9473(3) 1.0148(3) 0.8743(2) 0.0248(7) Uani 1 1 d . . . H42 H 1.0075 0.9671 0.8780 0.030 Uiso 1 1 calc R . . H43 H 0.8851 0.9925 0.9071 0.030 Uiso 1 1 calc R . . C33 C 0.9992(3) 1.1464(3) 0.9230(2) 0.0307(8) Uani 1 1 d . . . H44 H 1.0675 1.1615 0.9763 0.037 Uiso 1 1 calc R . . H45 H 0.9414 1.1916 0.9521 0.037 Uiso 1 1 calc R . . C34 C 1.0345(3) 1.1810(3) 0.8381(2) 0.0223(6) Uani 1 1 d . . . H46 H 1.0018 1.2501 0.8343 0.027 Uiso 1 1 calc R . . H47 H 1.1200 1.2014 0.8476 0.027 Uiso 1 1 calc R . . C35 C 0.9843(3) 1.0713(3) 0.7443(2) 0.0224(6) Uani 1 1 d . . . H48 H 0.9455 1.0937 0.6906 0.027 Uiso 1 1 calc R . . H49 H 1.0463 1.0293 0.7203 0.027 Uiso 1 1 calc R . . C36 C 0.6870(4) 0.7447(3) 0.8642(3) 0.0403(9) Uani 1 1 d . . . H50 H 0.7708 0.7460 0.8661 0.048 Uiso 1 1 calc R . . H51 H 0.6425 0.6715 0.8093 0.048 Uiso 1 1 calc R . . C37 C 0.6573(3) 0.7483(4) 0.9619(3) 0.0430(10) Uani 1 1 d . . . H52 H 0.7228 0.7945 1.0182 0.052 Uiso 1 1 calc R . . H53 H 0.6358 0.6671 0.9623 0.052 Uiso 1 1 calc R . . C38 C 0.5534(3) 0.8104(4) 0.9670(3) 0.0407(9) Uani 1 1 d . . . H54 H 0.4803 0.7535 0.9287 0.049 Uiso 1 1 calc R . . H55 H 0.5453 0.8500 1.0368 0.049 Uiso 1 1 calc R . . C39 C 0.5851(3) 0.9007(3) 0.9196(2) 0.0286(7) Uani 1 1 d . . . H56 H 0.5145 0.9152 0.8846 0.034 Uiso 1 1 calc R . . H57 H 0.6288 0.9771 0.9709 0.034 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 Ba1 0.01349(12) 0.01500(12) 0.01201(11) 0.00544(9) 0.00299(9) 0.00254(9) O1 0.0232(11) 0.0229(11) 0.0140(10) 0.0039(8) 0.0077(8) 0.0087(9) C1 0.0201(14) 0.0182(14) 0.0162(14) 0.0098(12) 0.0079(12) 0.0089(11) Ba2 0.01531(9) 0.01666(9) 0.01387(9) 0.00615(7) 0.00192(6) 0.00276(6) O2 0.0184(10) 0.0254(11) 0.0212(11) 0.0143(9) 0.0090(9) 0.0052(8) C2 0.0236(15) 0.0161(14) 0.0189(15) 0.0113(12) 0.0069(12) 0.0075(12) O3 0.0226(11) 0.0157(10) 0.0154(10) 0.0039(8) -0.0022(8) -0.0019(8) C3 0.0243(16) 0.0240(16) 0.0296(17) 0.0154(14) 0.0150(13) 0.0094(13) O4 0.0274(12) 0.0216(11) 0.0263(12) 0.0064(9) 0.0064(9) 0.0086(9) C4 0.0384(19) 0.0138(14) 0.0270(17) 0.0052(13) 0.0192(15) 0.0073(13) O5 0.0187(11) 0.0208(11) 0.0230(11) 0.0059(9) -0.0012(9) -0.0002(8) C5 0.0297(17) 0.0157(14) 0.0206(16) 0.0042(12) 0.0073(13) 0.0011(12) O6 0.0280(12) 0.0350(13) 0.0234(12) 0.0159(10) 0.0080(10) 0.0078(10) C6 0.0231(15) 0.0168(14) 0.0212(15) 0.0100(12) 0.0054(12) 0.0037(12) C7 0.0201(16) 0.0297(17) 0.0271(17) 0.0112(14) 0.0064(13) 0.0052(13) C8 0.057(3) 0.029(2) 0.049(2) 0.0034(17) 0.037(2) 0.0049(18) C9 0.0197(16) 0.0302(18) 0.0275(17) 0.0077(14) 0.0023(13) 0.0024(13) C10 0.0122(13) 0.0249(15) 0.0133(13) 0.0099(12) 0.0007(11) 0.0019(11) C11 0.0166(14) 0.0233(15) 0.0143(14) 0.0078(12) 0.0004(11) 0.0017(11) C12 0.0178(15) 0.0269(17) 0.0258(16) 0.0158(14) 0.0030(12) 0.0013(12) C13 0.0192(15) 0.0390(19) 0.0236(16) 0.0209(15) 0.0076(13) 0.0079(13) C14 0.0233(16) 0.0323(18) 0.0221(16) 0.0146(14) 0.0080(13) 0.0124(13) C15 0.0166(14) 0.0269(16) 0.0193(15) 0.0128(13) 0.0010(12) 0.0041(12) C16 0.0249(16) 0.0187(15) 0.0251(16) 0.0078(13) 0.0074(13) 0.0009(12) C17 0.0317(19) 0.056(2) 0.041(2) 0.0362(19) 0.0218(16) 0.0194(17) C18 0.0244(17) 0.0273(17) 0.0361(19) 0.0174(15) 0.0096(14) 0.0111(13) C19 0.0122(13) 0.0163(14) 0.0168(14) 0.0066(11) 0.0001(11) 0.0035(11) C20 0.0144(14) 0.0204(15) 0.0192(15) 0.0095(12) 0.0046(11) 0.0049(11) C21 0.0191(14) 0.0214(15) 0.0138(14) 0.0033(12) 0.0053(11) 0.0063(12) C22 0.0186(14) 0.0156(14) 0.0204(15) 0.0062(12) 0.0015(12) 0.0022(11) C23 0.0154(14) 0.0176(14) 0.0232(15) 0.0114(12) 0.0029(12) 0.0029(11) C24 0.0132(13) 0.0211(15) 0.0166(14) 0.0083(12) 0.0037(11) 0.0049(11) C25 0.0223(16) 0.0249(16) 0.0200(15) 0.0078(13) 0.0063(12) 0.0016(12) C26 0.0295(17) 0.0183(15) 0.0211(16) 0.0018(12) 0.0017(13) 0.0022(12) C27 0.0289(17) 0.0227(16) 0.0174(15) 0.0070(13) 0.0050(13) 0.0022(13) C28 0.0320(19) 0.0250(17) 0.0346(19) 0.0055(15) 0.0125(15) 0.0033(14) C29 0.0367(19) 0.0235(17) 0.0296(18) 0.0074(14) 0.0097(15) 0.0119(14) C30 0.034(2) 0.0301(19) 0.043(2) 0.0135(16) 0.0185(17) 0.0120(15) C31 0.0293(18) 0.0293(18) 0.0337(19) 0.0102(15) 0.0012(15) 0.0100(14) C32 0.0186(15) 0.0323(18) 0.0261(17) 0.0158(14) 0.0014(13) 0.0028(13) C33 0.0304(18) 0.0350(19) 0.0185(16) 0.0059(14) 0.0043(14) -0.0088(14) C34 0.0186(15) 0.0265(16) 0.0203(15) 0.0077(13) 0.0036(12) 0.0025(12) C35 0.0207(15) 0.0250(16) 0.0198(15) 0.0070(13) 0.0038(12) 0.0031(12) C36 0.054(2) 0.043(2) 0.035(2) 0.0230(18) 0.0120(18) 0.0202(19) C37 0.044(2) 0.061(3) 0.040(2) 0.036(2) 0.0108(18) 0.0152(19) C38 0.0276(19) 0.069(3) 0.040(2) 0.036(2) 0.0110(16) 0.0084(18) C39 0.0251(17) 0.041(2) 0.0230(17) 0.0133(15) 0.0070(13) 0.0101(15) _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 Ba1 O2 2.6445(18) 2_676 ? Ba1 O2 2.6445(18) . ? Ba1 O3 2.6873(19) . ? Ba1 O3 2.6873(19) 2_676 ? Ba1 O1 2.7611(19) 2_676 ? Ba1 O1 2.7611(19) . ? O1 C1 1.331(3) . ? O1 Ba2 2.5396(19) . ? C1 C6 1.409(4) . ? C1 C2 1.410(4) . ? Ba2 O3 2.5713(19) . ? Ba2 O2 2.6061(19) . ? Ba2 O4 2.743(2) . ? Ba2 O5 2.759(2) . ? Ba2 O6 2.837(2) . ? O2 C10 1.331(3) . ? C2 C3 1.388(4) . ? C2 C7 1.502(4) . ? O3 C19 1.334(3) . ? C3 C4 1.383(4) . ? C3 H1 0.9500 . ? O4 C28 1.440(4) . ? O4 C31 1.441(4) . ? C4 C5 1.386(4) . ? C4 C8 1.512(4) . ? O5 C32 1.430(3) . ? O5 C35 1.449(3) . ? C5 C6 1.390(4) . ? C5 H2 0.9500 . ? O6 C36 1.441(4) . ? O6 C39 1.456(4) . ? C6 C9 1.492(4) . ? C7 H3 0.9800 . ? C7 H4 0.9800 . ? C7 H5 0.9800 . ? C8 H6 0.9800 . ? C8 H7 0.9800 . ? C8 H8 0.9800 . ? C9 H9 0.9800 . ? C9 H10 0.9800 . ? C9 H11 0.9800 . ? C10 C15 1.412(4) . ? C10 C11 1.415(4) . ? C11 C12 1.392(4) . ? C11 C16 1.504(4) . ? C12 C13 1.389(4) . ? C12 H12 0.9500 . ? C13 C14 1.389(4) . ? C13 C17 1.508(4) . ? C14 C15 1.384(4) . ? C14 H13 0.9500 . ? C15 C18 1.497(4) . ? C16 H14 0.9800 . ? C16 H15 0.9800 . ? C16 H16 0.9800 . ? C17 H17 0.9800 . ? C17 H18 0.9800 . ? C17 H19 0.9800 . ? C18 H20 0.9800 . ? C18 H21 0.9800 . ? C18 H22 0.9800 . ? C19 C20 1.410(4) . ? C19 C24 1.421(4) . ? C20 C21 1.386(4) . ? C20 C25 1.513(4) . ? C21 C22 1.393(4) . ? C21 H23 0.9500 . ? C22 C23 1.390(4) . ? C22 C26 1.505(4) . ? C23 C24 1.388(4) . ? C23 H24 0.9500 . ? C24 C27 1.503(4) . ? C25 H25 0.9800 . ? C25 H26 0.9800 . ? C25 H27 0.9800 . ? C26 H28 0.9800 . ? C26 H29 0.9800 . ? C26 H30 0.9800 . ? C27 H31 0.9800 . ? C27 H32 0.9800 . ? C27 H33 0.9800 . ? C28 C29 1.518(4) . ? C28 H34 0.9900 . ? C28 H35 0.9900 . ? C29 C30 1.537(5) . ? C29 H36 0.9900 . ? C29 H37 0.9900 . ? C30 C31 1.519(5) . ? C30 H38 0.9900 . ? C30 H39 0.9900 . ? C31 H40 0.9900 . ? C31 H41 0.9900 . ? C32 C33 1.513(4) . ? C32 H42 0.9900 . ? C32 H43 0.9900 . ? C33 C34 1.528(4) . ? C33 H44 0.9900 . ? C33 H45 0.9900 . ? C34 C35 1.523(4) . ? C34 H46 0.9900 . ? C34 H47 0.9900 . ? C35 H48 0.9900 . ? C35 H49 0.9900 . ? C36 C37 1.502(5) . ? C36 H50 0.9900 . ? C36 H51 0.9900 . ? C37 C38 1.533(5) . ? C37 H52 0.9900 . ? C37 H53 0.9900 . ? C38 C39 1.521(5) . ? C38 H54 0.9900 . ? C38 H55 0.9900 . ? C39 H56 0.9900 . ? C39 H57 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Ba1 O2 180.00(7) 2_676 . ? O2 Ba1 O3 104.81(6) 2_676 . ? O2 Ba1 O3 75.19(6) . . ? O2 Ba1 O3 75.19(6) 2_676 2_676 ? O2 Ba1 O3 104.81(6) . 2_676 ? O3 Ba1 O3 180.0 . 2_676 ? O2 Ba1 O1 70.84(6) 2_676 2_676 ? O2 Ba1 O1 109.16(6) . 2_676 ? O3 Ba1 O1 108.17(6) . 2_676 ? O3 Ba1 O1 71.83(6) 2_676 2_676 ? O2 Ba1 O1 109.16(6) 2_676 . ? O2 Ba1 O1 70.84(6) . . ? O3 Ba1 O1 71.83(6) . . ? O3 Ba1 O1 108.17(6) 2_676 . ? O1 Ba1 O1 180.0 2_676 . ? C1 O1 Ba2 134.29(17) . . ? C1 O1 Ba1 134.78(17) . . ? Ba2 O1 Ba1 90.27(6) . . ? O1 C1 C6 120.4(3) . . ? O1 C1 C2 121.0(3) . . ? C6 C1 C2 118.6(3) . . ? O1 Ba2 O3 77.42(6) . . ? O1 Ba2 O2 75.05(6) . . ? O3 Ba2 O2 77.84(6) . . ? O1 Ba2 O4 87.59(6) . . ? O3 Ba2 O4 142.66(7) . . ? O2 Ba2 O4 131.16(6) . . ? O1 Ba2 O5 118.86(6) . . ? O3 Ba2 O5 80.72(6) . . ? O2 Ba2 O5 150.99(6) . . ? O4 Ba2 O5 76.99(6) . . ? O1 Ba2 O6 152.21(7) . . ? O3 Ba2 O6 125.85(6) . . ? O2 Ba2 O6 93.89(6) . . ? O4 Ba2 O6 80.69(6) . . ? O5 Ba2 O6 83.03(6) . . ? C10 O2 Ba2 117.83(16) . . ? C10 O2 Ba1 149.03(17) . . ? Ba2 O2 Ba1 91.48(6) . . ? C3 C2 C1 119.6(3) . . ? C3 C2 C7 121.5(3) . . ? C1 C2 C7 118.9(3) . . ? C19 O3 Ba2 130.24(16) . . ? C19 O3 Ba1 135.55(16) . . ? Ba2 O3 Ba1 91.27(6) . . ? C4 C3 C2 122.4(3) . . ? C4 C3 H1 118.8 . . ? C2 C3 H1 118.8 . . ? C28 O4 C31 105.6(2) . . ? C28 O4 Ba2 121.66(18) . . ? C31 O4 Ba2 131.71(18) . . ? C3 C4 C5 117.4(3) . . ? C3 C4 C8 122.0(3) . . ? C5 C4 C8 120.5(3) . . ? C32 O5 C35 106.0(2) . . ? C32 O5 Ba2 126.00(17) . . ? C35 O5 Ba2 126.26(16) . . ? C4 C5 C6 122.6(3) . . ? C4 C5 H2 118.7 . . ? C6 C5 H2 118.7 . . ? C36 O6 C39 109.5(2) . . ? C36 O6 Ba2 121.13(19) . . ? C39 O6 Ba2 126.65(17) . . ? C5 C6 C1 119.3(3) . . ? C5 C6 C9 120.9(3) . . ? C1 C6 C9 119.8(3) . . ? C2 C7 H3 109.5 . . ? C2 C7 H4 109.5 . . ? H3 C7 H4 109.5 . . ? C2 C7 H5 109.5 . . ? H3 C7 H5 109.5 . . ? H4 C7 H5 109.5 . . ? C4 C8 H6 109.5 . . ? C4 C8 H7 109.5 . . ? H6 C8 H7 109.5 . . ? C4 C8 H8 109.5 . . ? H6 C8 H8 109.5 . . ? H7 C8 H8 109.5 . . ? C6 C9 H9 109.5 . . ? C6 C9 H10 109.5 . . ? H9 C9 H10 109.5 . . ? C6 C9 H11 109.5 . . ? H9 C9 H11 109.5 . . ? H10 C9 H11 109.5 . . ? O2 C10 C15 120.3(3) . . ? O2 C10 C11 121.2(3) . . ? C15 C10 C11 118.5(3) . . ? C12 C11 C10 119.6(3) . . ? C12 C11 C16 120.5(3) . . ? C10 C11 C16 119.8(3) . . ? C13 C12 C11 122.1(3) . . ? C13 C12 H12 118.9 . . ? C11 C12 H12 118.9 . . ? C12 C13 C14 117.4(3) . . ? C12 C13 C17 121.3(3) . . ? C14 C13 C17 121.3(3) . . ? C15 C14 C13 122.8(3) . . ? C15 C14 H13 118.6 . . ? C13 C14 H13 118.6 . . ? C14 C15 C10 119.5(3) . . ? C14 C15 C18 121.6(3) . . ? C10 C15 C18 118.9(3) . . ? C11 C16 H14 109.5 . . ? C11 C16 H15 109.5 . . ? H14 C16 H15 109.5 . . ? C11 C16 H16 109.5 . . ? H14 C16 H16 109.5 . . ? H15 C16 H16 109.5 . . ? C13 C17 H17 109.5 . . ? C13 C17 H18 109.5 . . ? H17 C17 H18 109.5 . . ? C13 C17 H19 109.5 . . ? H17 C17 H19 109.5 . . ? H18 C17 H19 109.5 . . ? C15 C18 H20 109.5 . . ? C15 C18 H21 109.5 . . ? H20 C18 H21 109.5 . . ? C15 C18 H22 109.5 . . ? H20 C18 H22 109.5 . . ? H21 C18 H22 109.5 . . ? O3 C19 C20 121.2(2) . . ? O3 C19 C24 120.6(2) . . ? C20 C19 C24 118.2(3) . . ? C21 C20 C19 120.4(3) . . ? C21 C20 C25 120.2(3) . . ? C19 C20 C25 119.3(3) . . ? C20 C21 C22 121.9(3) . . ? C20 C21 H23 119.1 . . ? C22 C21 H23 119.1 . . ? C23 C22 C21 117.3(3) . . ? C23 C22 C26 121.9(3) . . ? C21 C22 C26 120.8(3) . . ? C24 C23 C22 122.9(3) . . ? C24 C23 H24 118.6 . . ? C22 C23 H24 118.6 . . ? C23 C24 C19 119.2(3) . . ? C23 C24 C27 121.7(3) . . ? C19 C24 C27 119.1(3) . . ? C20 C25 H25 109.5 . . ? C20 C25 H26 109.5 . . ? H25 C25 H26 109.5 . . ? C20 C25 H27 109.5 . . ? H25 C25 H27 109.5 . . ? H26 C25 H27 109.5 . . ? C22 C26 H28 109.5 . . ? C22 C26 H29 109.5 . . ? H28 C26 H29 109.5 . . ? C22 C26 H30 109.5 . . ? H28 C26 H30 109.5 . . ? H29 C26 H30 109.5 . . ? C24 C27 H31 109.5 . . ? C24 C27 H32 109.5 . . ? H31 C27 H32 109.5 . . ? C24 C27 H33 109.5 . . ? H31 C27 H33 109.5 . . ? H32 C27 H33 109.5 . . ? O4 C28 C29 105.9(3) . . ? O4 C28 H34 110.6 . . ? C29 C28 H34 110.6 . . ? O4 C28 H35 110.6 . . ? C29 C28 H35 110.6 . . ? H34 C28 H35 108.7 . . ? C28 C29 C30 103.7(3) . . ? C28 C29 H36 111.0 . . ? C30 C29 H36 111.0 . . ? C28 C29 H37 111.0 . . ? C30 C29 H37 111.0 . . ? H36 C29 H37 109.0 . . ? C31 C30 C29 105.2(3) . . ? C31 C30 H38 110.7 . . ? C29 C30 H38 110.7 . . ? C31 C30 H39 110.7 . . ? C29 C30 H39 110.7 . . ? H38 C30 H39 108.8 . . ? O4 C31 C30 105.7(3) . . ? O4 C31 H40 110.6 . . ? C30 C31 H40 110.6 . . ? O4 C31 H41 110.6 . . ? C30 C31 H41 110.6 . . ? H40 C31 H41 108.7 . . ? O5 C32 C33 105.0(2) . . ? O5 C32 H42 110.7 . . ? C33 C32 H42 110.7 . . ? O5 C32 H43 110.7 . . ? C33 C32 H43 110.7 . . ? H42 C32 H43 108.8 . . ? C32 C33 C34 104.3(2) . . ? C32 C33 H44 110.9 . . ? C34 C33 H44 110.9 . . ? C32 C33 H45 110.9 . . ? C34 C33 H45 110.9 . . ? H44 C33 H45 108.9 . . ? C35 C34 C33 104.8(2) . . ? C35 C34 H46 110.8 . . ? C33 C34 H46 110.8 . . ? C35 C34 H47 110.8 . . ? C33 C34 H47 110.8 . . ? H46 C34 H47 108.9 . . ? O5 C35 C34 105.7(2) . . ? O5 C35 H48 110.6 . . ? C34 C35 H48 110.6 . . ? O5 C35 H49 110.6 . . ? C34 C35 H49 110.6 . . ? H48 C35 H49 108.7 . . ? O6 C36 C37 106.5(3) . . ? O6 C36 H50 110.4 . . ? C37 C36 H50 110.4 . . ? O6 C36 H51 110.4 . . ? C37 C36 H51 110.4 . . ? H50 C36 H51 108.6 . . ? C36 C37 C38 102.4(3) . . ? C36 C37 H52 111.3 . . ? C38 C37 H52 111.3 . . ? C36 C37 H53 111.3 . . ? C38 C37 H53 111.3 . . ? H52 C37 H53 109.2 . . ? C39 C38 C37 102.3(3) . . ? C39 C38 H54 111.3 . . ? C37 C38 H54 111.3 . . ? C39 C38 H55 111.3 . . ? C37 C38 H55 111.3 . . ? H54 C38 H55 109.2 . . ? O6 C39 C38 105.7(3) . . ? O6 C39 H56 110.6 . . ? C38 C39 H56 110.6 . . ? O6 C39 H57 110.6 . . ? C38 C39 H57 110.6 . . ? H56 C39 H57 108.7 . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.908 _refine_diff_density_min -0.888 _refine_diff_density_rms 0.098 data_c:\tric _database_code_depnum_ccdc_archive 'CCDC 720258' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C78 Ba3 D114 O12' _chemical_formula_sum 'C78 Ba3 D114 O12' _chemical_formula_weight 1770.40 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' D D 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ba Ba -0.3244 2.2819 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.9104(2) _cell_length_b 12.2311(2) _cell_length_c 14.5434(3) _cell_angle_alpha 109.9290(10) _cell_angle_beta 97.9730(10) _cell_angle_gamma 97.9770(10) _cell_volume 1932.73(6) _cell_formula_units_Z 1 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.521 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 846 _exptl_absorpt_coefficient_mu 1.568 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8341 _exptl_absorpt_correction_T_max 0.8589 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker X8 Apex II CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15097 _diffrn_reflns_av_R_equivalents 0.0144 _diffrn_reflns_av_sigmaI/netI 0.0235 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.26 _diffrn_reflns_theta_max 27.50 _reflns_number_total 8785 _reflns_number_gt 7812 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART (Bruker)' _computing_cell_refinement 'Bruker SMART (Bruker)' _computing_data_reduction 'Bruker SAINT (Bruker)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 1999)' _computing_publication_material 'CIFTAB (Sheldrick, 1997)' _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^)+(0.0177P)^2^+1.2630P] 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 ? _refine_ls_extinction_coef ? _refine_ls_number_reflns 8785 _refine_ls_number_parameters 430 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0245 _refine_ls_R_factor_gt 0.0196 _refine_ls_wR_factor_ref 0.0478 _refine_ls_wR_factor_gt 0.0454 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.031 _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 Ba1 Ba 0.5000 0.0000 0.5000 0.01389(4) Uani 1 2 d S . . O1 O 0.36838(11) 0.17224(11) 0.51702(9) 0.0219(3) Uani 1 1 d . . . C1 C 0.33040(16) 0.24530(15) 0.59182(12) 0.0171(3) Uani 1 1 d . . . Ba2 Ba 0.322110(9) 0.110670(9) 0.328540(7) 0.01641(3) Uani 1 1 d . . . O2 O 0.54046(11) 0.10455(12) 0.37212(10) 0.0222(3) Uani 1 1 d . . . C2 C 0.21219(16) 0.22978(16) 0.59655(13) 0.0201(4) Uani 1 1 d . . . O3 O 0.31232(11) -0.08989(11) 0.35137(9) 0.0210(3) Uani 1 1 d . . . C3 C 0.17558(18) 0.30304(17) 0.67818(15) 0.0257(4) Uani 1 1 d . . . D1 D 0.0956 0.2912 0.6804 0.031 Uiso 1 1 calc R . . O4 O 0.21296(13) 0.29980(12) 0.35708(11) 0.0290(3) Uani 1 1 d . . . C4 C 0.2525(2) 0.39298(17) 0.75665(15) 0.0292(5) Uani 1 1 d . . . O5 O 0.34255(13) 0.15024(13) 0.14973(10) 0.0310(3) Uani 1 1 d . . . C5 C 0.36788(19) 0.41030(17) 0.74995(14) 0.0268(4) Uani 1 1 d . . . D2 D 0.4214 0.4728 0.8022 0.032 Uiso 1 1 calc R . . O6 O 0.09855(11) 0.00342(12) 0.22640(10) 0.0253(3) Uani 1 1 d . . . C6 C 0.40836(17) 0.33950(16) 0.66948(13) 0.0211(4) Uani 1 1 d . . . C7 C 0.12757(17) 0.13122(18) 0.51325(15) 0.0283(4) Uani 1 1 d . . . D3 D 0.1171 0.1519 0.4536 0.043 Uiso 1 1 calc R . . D4 D 0.0531 0.1199 0.5336 0.043 Uiso 1 1 calc R . . D5 D 0.1574 0.0576 0.4983 0.043 Uiso 1 1 calc R . . C8 C 0.2131(3) 0.4674(2) 0.8484(2) 0.0501(7) Uani 1 1 d . . . D6 D 0.2670 0.5440 0.8805 0.075 Uiso 1 1 calc R . . D7 D 0.2113 0.4258 0.8953 0.075 Uiso 1 1 calc R . . D8 D 0.1355 0.4804 0.8289 0.075 Uiso 1 1 calc R . . C9 C 0.53422(18) 0.3604(2) 0.66478(16) 0.0320(5) Uani 1 1 d . . . D9 D 0.5765 0.4286 0.7237 0.048 Uiso 1 1 calc R . . D10 D 0.5432 0.3766 0.6044 0.048 Uiso 1 1 calc R . . D11 D 0.5652 0.2898 0.6631 0.048 Uiso 1 1 calc R . . C10 C 0.61037(14) 0.13184(16) 0.31640(12) 0.0170(3) Uani 1 1 d . . . C11 C 0.62502(15) 0.24459(16) 0.30800(13) 0.0194(4) Uani 1 1 d . . . C12 C 0.69672(16) 0.26938(18) 0.24674(14) 0.0240(4) Uani 1 1 d . . . D12 D 0.7069 0.3459 0.2426 0.029 Uiso 1 1 calc R . . C13 C 0.75383(17) 0.18626(19) 0.19152(15) 0.0268(4) Uani 1 1 d . . . C14 C 0.74083(17) 0.07691(19) 0.20237(14) 0.0261(4) Uani 1 1 d . . . D13 D 0.7805 0.0194 0.1663 0.031 Uiso 1 1 calc R . . C15 C 0.67224(16) 0.04855(17) 0.26386(14) 0.0216(4) Uani 1 1 d . . . C16 C 0.56312(18) 0.33677(17) 0.36513(15) 0.0275(4) Uani 1 1 d . . . D14 D 0.4829 0.3206 0.3295 0.041 Uiso 1 1 calc R . . D15 D 0.6022 0.4156 0.3713 0.041 Uiso 1 1 calc R . . D16 D 0.5639 0.3341 0.4318 0.041 Uiso 1 1 calc R . . C17 C 0.8280(2) 0.2132(2) 0.12269(18) 0.0396(6) Uani 1 1 d . . . D17 D 0.8472 0.1397 0.0803 0.059 Uiso 1 1 calc R . . D18 D 0.8993 0.2695 0.1624 0.059 Uiso 1 1 calc R . . D19 D 0.7854 0.2480 0.0807 0.059 Uiso 1 1 calc R . . C18 C 0.66553(19) -0.06750(19) 0.27887(17) 0.0322(5) Uani 1 1 d . . . D20 D 0.7026 -0.0531 0.3476 0.048 Uiso 1 1 calc R . . D21 D 0.7053 -0.1189 0.2323 0.048 Uiso 1 1 calc R . . D22 D 0.5842 -0.1062 0.2665 0.048 Uiso 1 1 calc R . . C19 C 0.25661(15) -0.19822(15) 0.29083(13) 0.0172(3) Uani 1 1 d . . . C20 C 0.26224(15) -0.24135(16) 0.18841(13) 0.0191(4) Uani 1 1 d . . . C21 C 0.20669(16) -0.35595(16) 0.12730(13) 0.0214(4) Uani 1 1 d . . . D23 D 0.2127 -0.3838 0.0590 0.026 Uiso 1 1 calc R . . C22 C 0.14257(16) -0.43138(16) 0.16242(14) 0.0209(4) Uani 1 1 d . . . C23 C 0.13554(16) -0.38739(16) 0.26289(13) 0.0199(4) Uani 1 1 d . . . D24 D 0.0909 -0.4368 0.2883 0.024 Uiso 1 1 calc R . . C24 C 0.19141(15) -0.27374(15) 0.32737(13) 0.0180(3) Uani 1 1 d . . . C25 C 0.33042(18) -0.16219(18) 0.14720(14) 0.0268(4) Uani 1 1 d . . . D25 D 0.2843 -0.1064 0.1349 0.040 Uiso 1 1 calc R . . D26 D 0.3493 -0.2108 0.0845 0.040 Uiso 1 1 calc R . . D27 D 0.4021 -0.1179 0.1955 0.040 Uiso 1 1 calc R . . C26 C 0.08406(18) -0.55592(16) 0.09405(14) 0.0286(4) Uani 1 1 d . . . D28 D 0.1319 -0.5877 0.0455 0.043 Uiso 1 1 calc R . . D29 D 0.0082 -0.5547 0.0587 0.043 Uiso 1 1 calc R . . D30 D 0.0741 -0.6062 0.1335 0.043 Uiso 1 1 calc R . . C27 C 0.18684(18) -0.23082(17) 0.43666(14) 0.0255(4) Uani 1 1 d . . . D31 D 0.2617 -0.2289 0.4756 0.038 Uiso 1 1 calc R . . D32 D 0.1262 -0.2848 0.4480 0.038 Uiso 1 1 calc R . . D33 D 0.1697 -0.1509 0.4575 0.038 Uiso 1 1 calc R . . C28 C 0.0949(2) 0.3051(2) 0.32508(17) 0.0366(5) Uani 1 1 d . . . D34 D 0.0450 0.2251 0.3004 0.044 Uiso 1 1 calc R . . D35 D 0.0884 0.3369 0.2709 0.044 Uiso 1 1 calc R . . C29 C 0.0598(2) 0.3870(2) 0.41623(19) 0.0409(6) Uani 1 1 d . . . D36 D 0.0139 0.3407 0.4473 0.049 Uiso 1 1 calc R . . D37 D 0.0133 0.4403 0.3981 0.049 Uiso 1 1 calc R . . C30 C 0.1730(2) 0.4576(2) 0.48676(17) 0.0361(5) Uani 1 1 d . . . D38 D 0.1774 0.5438 0.5037 0.043 Uiso 1 1 calc R . . D39 D 0.1813 0.4410 0.5492 0.043 Uiso 1 1 calc R . . C31 C 0.2654(2) 0.41589(19) 0.42950(18) 0.0362(5) Uani 1 1 d . . . D40 D 0.2905 0.4706 0.3960 0.043 Uiso 1 1 calc R . . D41 D 0.3336 0.4120 0.4749 0.043 Uiso 1 1 calc R . . C32 C 0.3122(3) 0.2534(3) 0.1343(2) 0.0490(6) Uani 1 1 d . . . D42 D 0.3540 0.3264 0.1905 0.059 Uiso 1 1 calc R . . D43 D 0.2280 0.2503 0.1297 0.059 Uiso 1 1 calc R . . C33 C 0.3458(3) 0.2530(3) 0.0389(2) 0.0559(7) Uani 1 1 d . . . D44 D 0.3701 0.3349 0.0413 0.067 Uiso 1 1 calc R . . D45 D 0.2812 0.2100 -0.0187 0.067 Uiso 1 1 calc R . . C34 C 0.4466(2) 0.1885(3) 0.0332(2) 0.0473(6) Uani 1 1 d . . . D46 D 0.4538 0.1489 -0.0368 0.057 Uiso 1 1 calc R . . D47 D 0.5203 0.2439 0.0712 0.057 Uiso 1 1 calc R . . C35 C 0.41438(19) 0.0987(2) 0.08000(15) 0.0333(5) Uani 1 1 d . . . D48 D 0.3711 0.0226 0.0284 0.040 Uiso 1 1 calc R . . D49 D 0.4846 0.0841 0.1154 0.040 Uiso 1 1 calc R . . C36 C 0.05370(18) -0.01518(18) 0.12439(15) 0.0293(4) Uani 1 1 d . . . D50 D 0.1165 0.0054 0.0916 0.035 Uiso 1 1 calc R . . D51 D -0.0050 0.0337 0.1200 0.035 Uiso 1 1 calc R . . C37 C -0.0001(2) -0.1456(2) 0.07637(16) 0.0385(6) Uani 1 1 d . . . D52 D 0.0563 -0.1918 0.0464 0.046 Uiso 1 1 calc R . . D53 D -0.0686 -0.1596 0.0237 0.046 Uiso 1 1 calc R . . C38 C -0.03484(17) -0.18033(17) 0.16112(14) 0.0257(4) Uani 1 1 d . . . D54 D -0.0024 -0.2494 0.1648 0.031 Uiso 1 1 calc R . . D55 D -0.1201 -0.2003 0.1520 0.031 Uiso 1 1 calc R . . C39 C 0.01616(17) -0.07040(17) 0.25491(14) 0.0255(4) Uani 1 1 d . . . D56 D -0.0453 -0.0281 0.2790 0.031 Uiso 1 1 calc R . . D57 D 0.0548 -0.0929 0.3087 0.031 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 Ba1 0.01394(7) 0.01548(7) 0.01306(6) 0.00596(5) 0.00361(5) 0.00277(5) O1 0.0254(7) 0.0249(7) 0.0163(6) 0.0047(5) 0.0080(5) 0.0115(5) C1 0.0244(9) 0.0164(8) 0.0156(8) 0.0086(7) 0.0077(7) 0.0093(7) Ba2 0.01670(6) 0.01753(6) 0.01539(5) 0.00678(4) 0.00269(4) 0.00329(4) O2 0.0187(6) 0.0291(7) 0.0264(7) 0.0170(6) 0.0104(5) 0.0052(5) C2 0.0245(9) 0.0186(9) 0.0223(9) 0.0112(7) 0.0086(7) 0.0073(7) O3 0.0228(7) 0.0171(6) 0.0187(6) 0.0059(5) -0.0014(5) -0.0032(5) C3 0.0295(11) 0.0239(10) 0.0343(10) 0.0163(8) 0.0197(9) 0.0117(8) O4 0.0334(8) 0.0228(7) 0.0310(7) 0.0073(6) 0.0081(6) 0.0108(6) C4 0.0441(13) 0.0187(9) 0.0308(10) 0.0086(8) 0.0233(9) 0.0106(9) O5 0.0326(8) 0.0418(9) 0.0267(7) 0.0198(7) 0.0106(6) 0.0101(7) C5 0.0399(12) 0.0171(9) 0.0218(9) 0.0038(7) 0.0115(8) 0.0034(8) O6 0.0213(7) 0.0235(7) 0.0254(7) 0.0066(6) -0.0019(5) -0.0011(5) C6 0.0260(10) 0.0199(9) 0.0209(9) 0.0099(7) 0.0078(7) 0.0069(7) C7 0.0234(10) 0.0307(11) 0.0306(10) 0.0118(9) 0.0054(8) 0.0030(8) C8 0.0693(18) 0.0294(12) 0.0516(15) 0.0029(11) 0.0435(14) 0.0096(12) C9 0.0239(11) 0.0357(12) 0.0309(11) 0.0065(9) 0.0042(8) 0.0042(9) C10 0.0116(8) 0.0244(9) 0.0167(8) 0.0109(7) 0.0016(6) 0.0016(7) C11 0.0168(9) 0.0230(9) 0.0183(8) 0.0089(7) 0.0018(7) 0.0021(7) C12 0.0215(9) 0.0290(10) 0.0278(10) 0.0187(8) 0.0059(8) 0.0033(8) C13 0.0206(10) 0.0432(12) 0.0286(10) 0.0245(9) 0.0110(8) 0.0099(9) C14 0.0235(10) 0.0388(11) 0.0272(10) 0.0193(9) 0.0120(8) 0.0165(9) C15 0.0182(9) 0.0285(10) 0.0233(9) 0.0150(8) 0.0041(7) 0.0075(7) C16 0.0299(11) 0.0232(10) 0.0293(10) 0.0079(8) 0.0114(8) 0.0036(8) C17 0.0337(12) 0.0650(16) 0.0453(13) 0.0412(13) 0.0239(11) 0.0205(11) C18 0.0310(11) 0.0338(11) 0.0453(12) 0.0248(10) 0.0150(10) 0.0157(9) C19 0.0167(8) 0.0162(8) 0.0183(8) 0.0067(7) 0.0010(7) 0.0040(7) C20 0.0166(9) 0.0215(9) 0.0196(8) 0.0083(7) 0.0036(7) 0.0037(7) C21 0.0225(9) 0.0227(9) 0.0175(8) 0.0048(7) 0.0048(7) 0.0057(7) C22 0.0221(9) 0.0160(9) 0.0223(9) 0.0050(7) 0.0024(7) 0.0036(7) C23 0.0192(9) 0.0182(9) 0.0234(9) 0.0094(7) 0.0042(7) 0.0028(7) C24 0.0184(9) 0.0184(9) 0.0173(8) 0.0067(7) 0.0025(7) 0.0047(7) C25 0.0261(10) 0.0301(11) 0.0225(9) 0.0093(8) 0.0069(8) -0.0010(8) C26 0.0339(11) 0.0186(9) 0.0274(10) 0.0036(8) 0.0034(9) 0.0019(8) C27 0.0326(11) 0.0247(10) 0.0192(9) 0.0084(8) 0.0071(8) 0.0030(8) C28 0.0385(13) 0.0319(12) 0.0389(12) 0.0116(10) 0.0020(10) 0.0148(10) C29 0.0357(13) 0.0358(13) 0.0558(15) 0.0159(11) 0.0210(11) 0.0123(10) C30 0.0485(14) 0.0279(11) 0.0362(12) 0.0098(9) 0.0167(10) 0.0181(10) C31 0.0360(12) 0.0242(11) 0.0440(13) 0.0051(9) 0.0138(10) 0.0052(9) C32 0.0612(17) 0.0580(17) 0.0448(14) 0.0330(13) 0.0144(13) 0.0265(14) C33 0.0614(18) 0.075(2) 0.0556(17) 0.0471(16) 0.0206(14) 0.0215(15) C34 0.0317(13) 0.0794(19) 0.0466(14) 0.0422(14) 0.0121(11) 0.0085(12) C35 0.0303(11) 0.0470(13) 0.0245(10) 0.0147(9) 0.0079(9) 0.0076(10) C36 0.0265(10) 0.0310(11) 0.0293(10) 0.0136(9) -0.0013(8) 0.0026(8) C37 0.0416(13) 0.0391(13) 0.0223(10) 0.0055(9) 0.0040(9) -0.0151(10) C38 0.0225(10) 0.0256(10) 0.0260(9) 0.0071(8) 0.0047(8) 0.0013(8) C39 0.0243(10) 0.0275(10) 0.0226(9) 0.0070(8) 0.0043(8) 0.0042(8) _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 Ba1 O2 2.6505(12) . ? Ba1 O2 2.6505(12) 2_656 ? Ba1 O3 2.6899(12) . ? Ba1 O3 2.6899(12) 2_656 ? Ba1 O1 2.7615(13) 2_656 ? Ba1 O1 2.7615(13) . ? Ba1 Ba2 3.76442(11) . ? Ba1 Ba2 3.76442(11) 2_656 ? O1 C1 1.331(2) . ? O1 Ba2 2.5383(12) . ? C1 C2 1.409(3) . ? C1 C6 1.411(3) . ? Ba2 O3 2.5745(13) . ? Ba2 O2 2.6076(13) . ? Ba2 O4 2.7465(14) . ? Ba2 O6 2.7608(13) . ? Ba2 O5 2.8385(14) . ? O2 C10 1.325(2) . ? C2 C3 1.389(3) . ? C2 C7 1.505(3) . ? O3 C19 1.330(2) . ? C3 C4 1.388(3) . ? O4 C28 1.436(3) . ? O4 C31 1.438(2) . ? C4 C5 1.383(3) . ? C4 C8 1.514(3) . ? O5 C32 1.439(3) . ? O5 C35 1.453(2) . ? C5 C6 1.391(2) . ? O6 C36 1.433(2) . ? O6 C39 1.440(2) . ? C6 C9 1.500(3) . ? C10 C15 1.414(3) . ? C10 C11 1.415(2) . ? C11 C12 1.392(2) . ? C11 C16 1.506(3) . ? C12 C13 1.389(3) . ? C13 C14 1.390(3) . ? C13 C17 1.510(3) . ? C14 C15 1.387(3) . ? C15 C18 1.501(3) . ? C19 C24 1.410(2) . ? C19 C20 1.415(2) . ? C20 C21 1.387(3) . ? C20 C25 1.506(3) . ? C21 C22 1.389(3) . ? C22 C23 1.394(2) . ? C22 C26 1.508(2) . ? C23 C24 1.391(2) . ? C24 C27 1.506(2) . ? C28 C29 1.517(3) . ? C29 C30 1.519(3) . ? C30 C31 1.512(3) . ? C32 C33 1.495(3) . ? C33 C34 1.522(4) . ? C34 C35 1.510(3) . ? C36 C37 1.509(3) . ? C37 C38 1.523(3) . ? C38 C39 1.527(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 Ba1 O2 180.0 . 2_656 ? O2 Ba1 O3 75.21(4) . . ? O2 Ba1 O3 104.79(4) 2_656 . ? O2 Ba1 O3 104.79(4) . 2_656 ? O2 Ba1 O3 75.21(4) 2_656 2_656 ? O3 Ba1 O3 180.00(5) . 2_656 ? O2 Ba1 O1 109.32(4) . 2_656 ? O2 Ba1 O1 70.68(4) 2_656 2_656 ? O3 Ba1 O1 108.19(4) . 2_656 ? O3 Ba1 O1 71.81(4) 2_656 2_656 ? O2 Ba1 O1 70.68(4) . . ? O2 Ba1 O1 109.32(4) 2_656 . ? O3 Ba1 O1 71.81(4) . . ? O3 Ba1 O1 108.19(4) 2_656 . ? O1 Ba1 O1 180.0 2_656 . ? O2 Ba1 Ba2 43.83(3) . . ? O2 Ba1 Ba2 136.17(3) 2_656 . ? O3 Ba1 Ba2 43.14(3) . . ? O3 Ba1 Ba2 136.86(3) 2_656 . ? O1 Ba1 Ba2 137.60(3) 2_656 . ? O1 Ba1 Ba2 42.40(3) . . ? O2 Ba1 Ba2 136.17(3) . 2_656 ? O2 Ba1 Ba2 43.83(3) 2_656 2_656 ? O3 Ba1 Ba2 136.86(3) . 2_656 ? O3 Ba1 Ba2 43.14(3) 2_656 2_656 ? O1 Ba1 Ba2 42.40(3) 2_656 2_656 ? O1 Ba1 Ba2 137.60(3) . 2_656 ? Ba2 Ba1 Ba2 180.0 . 2_656 ? C1 O1 Ba2 134.27(11) . . ? C1 O1 Ba1 134.64(11) . . ? Ba2 O1 Ba1 90.42(4) . . ? O1 C1 C2 121.18(16) . . ? O1 C1 C6 120.56(16) . . ? C2 C1 C6 118.26(16) . . ? O1 Ba2 O3 77.41(4) . . ? O1 Ba2 O2 74.96(4) . . ? O3 Ba2 O2 77.93(4) . . ? O1 Ba2 O4 87.39(4) . . ? O3 Ba2 O4 142.88(4) . . ? O2 Ba2 O4 130.63(4) . . ? O1 Ba2 O6 119.17(4) . . ? O3 Ba2 O6 81.00(4) . . ? O2 Ba2 O6 151.17(4) . . ? O4 Ba2 O6 77.27(4) . . ? O1 Ba2 O5 152.15(4) . . ? O3 Ba2 O5 125.76(4) . . ? O2 Ba2 O5 93.70(4) . . ? O4 Ba2 O5 80.91(4) . . ? O6 Ba2 O5 82.85(4) . . ? O1 Ba2 Ba1 47.18(3) . . ? O3 Ba2 Ba1 45.59(3) . . ? O2 Ba2 Ba1 44.74(3) . . ? O4 Ba2 Ba1 134.31(3) . . ? O6 Ba2 Ba1 124.57(3) . . ? O5 Ba2 Ba1 135.73(3) . . ? C10 O2 Ba2 118.36(10) . . ? C10 O2 Ba1 148.63(11) . . ? Ba2 O2 Ba1 91.43(4) . . ? C3 C2 C1 120.08(17) . . ? C3 C2 C7 120.98(18) . . ? C1 C2 C7 118.92(16) . . ? C19 O3 Ba2 130.36(10) . . ? C19 O3 Ba1 135.51(11) . . ? Ba2 O3 Ba1 91.27(4) . . ? C4 C3 C2 121.89(18) . . ? C28 O4 C31 105.67(16) . . ? C28 O4 Ba2 131.29(12) . . ? C31 O4 Ba2 121.91(13) . . ? C5 C4 C3 117.72(17) . . ? C5 C4 C8 120.7(2) . . ? C3 C4 C8 121.6(2) . . ? C32 O5 C35 109.41(17) . . ? C32 O5 Ba2 121.27(13) . . ? C35 O5 Ba2 126.54(12) . . ? C4 C5 C6 122.36(19) . . ? C36 O6 C39 106.30(14) . . ? C36 O6 Ba2 125.66(11) . . ? C39 O6 Ba2 126.22(11) . . ? C5 C6 C1 119.61(18) . . ? C5 C6 C9 120.98(18) . . ? C1 C6 C9 119.40(16) . . ? O2 C10 C15 120.58(16) . . ? O2 C10 C11 121.01(16) . . ? C15 C10 C11 118.41(16) . . ? C12 C11 C10 119.60(17) . . ? C12 C11 C16 120.49(17) . . ? C10 C11 C16 119.92(16) . . ? C13 C12 C11 122.31(18) . . ? C12 C13 C14 117.42(17) . . ? C12 C13 C17 121.61(19) . . ? C14 C13 C17 120.97(19) . . ? C15 C14 C13 122.52(18) . . ? C14 C15 C10 119.65(17) . . ? C14 C15 C18 121.29(18) . . ? C10 C15 C18 119.02(16) . . ? O3 C19 C24 120.79(15) . . ? O3 C19 C20 121.00(16) . . ? C24 C19 C20 118.21(16) . . ? C21 C20 C19 120.08(16) . . ? C21 C20 C25 120.59(16) . . ? C19 C20 C25 119.32(16) . . ? C20 C21 C22 122.28(17) . . ? C21 C22 C23 117.26(16) . . ? C21 C22 C26 120.89(17) . . ? C23 C22 C26 121.84(17) . . ? C24 C23 C22 122.46(17) . . ? C23 C24 C19 119.69(16) . . ? C23 C24 C27 121.20(16) . . ? C19 C24 C27 119.08(16) . . ? O4 C28 C29 105.89(18) . . ? C28 C29 C30 104.96(18) . . ? C31 C30 C29 104.52(18) . . ? O4 C31 C30 105.71(18) . . ? O5 C32 C33 107.0(2) . . ? C32 C33 C34 102.8(2) . . ? C35 C34 C33 103.21(19) . . ? O5 C35 C34 105.78(19) . . ? O6 C36 C37 104.96(16) . . ? C36 C37 C38 104.90(17) . . ? C37 C38 C39 104.41(16) . . ? O6 C39 C38 105.97(15) . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.515 _refine_diff_density_min -0.324 _refine_diff_density_rms 0.063