# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_[CaL2(thf)4].CIF _database_code_depnum_ccdc_archive 'CCDC 914477' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point 76-80C _chemical_formula_moiety 'C44 H74 Ca O6' _chemical_formula_sum 'C44 H74 Ca O6' _chemical_formula_weight 739.11 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 _symmetry_space_group_name_Hall '-P 2ybc' 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 9.778(2) _cell_length_b 9.6717(19) _cell_length_c 22.946(5) _cell_angle_alpha 90.00 _cell_angle_beta 94.60(3) _cell_angle_gamma 90.00 _cell_volume 2163.1(8) _cell_formula_units_Z 2 _cell_measurement_temperature 123(1) _cell_measurement_reflns_used 19375 _cell_measurement_theta_min 2.09 _cell_measurement_theta_max 27.50 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.135 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 812 _exptl_absorpt_coefficient_mu 0.188 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.9851 _exptl_absorpt_correction_T_max 0.9906 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(1) _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 19375 _diffrn_reflns_av_R_equivalents 0.0750 _diffrn_reflns_av_sigmaI/netI 0.0493 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 2.09 _diffrn_reflns_theta_max 27.50 _reflns_number_total 4978 _reflns_number_gt 3917 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker Apex2 v2.0 (Bruker AXS, 2005)' _computing_cell_refinement 'Bruker Apex2 v2.0 (Bruker AXS, 2005)' _computing_data_reduction 'Bruker Apex2 v2.0 (Bruker AXS, 2005)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 2001)' _computing_publication_material 'CIFTAB (Sheldrick, 1997)' _refine_special_details ; Turt-butyl groups exhibit large ratios of ADP max/min for carbon atoms due to freely rotating primary carbons. 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^)+(0.2000P)^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 SHELXL _refine_ls_extinction_coef ? _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4963 _refine_ls_number_parameters 238 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0646 _refine_ls_R_factor_gt 0.0477 _refine_ls_wR_factor_ref 0.1345 _refine_ls_wR_factor_gt 0.1230 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.050 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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 0.5000 0.0000 0.0000 0.01645(13) Uani 1 2 d S . . O1 O 0.38312(11) -0.11834(11) 0.06150(5) 0.0224(3) Uani 1 1 d . . . O2 O 0.40347(12) 0.21024(11) 0.03507(5) 0.0260(3) Uani 1 1 d . . . O3 O 0.70327(12) 0.01449(12) 0.06842(5) 0.0260(3) Uani 1 1 d . . . C2 C 0.27733(15) -0.22455(15) 0.14202(6) 0.0179(3) Uani 1 1 d . . . C4 C 0.06742(16) -0.36354(16) 0.11925(7) 0.0221(3) Uani 1 1 d . . . C3 C 0.16894(16) -0.30491(15) 0.15825(7) 0.0205(3) Uani 1 1 d . . . H3 H 0.1632 -0.3214 0.1988 0.025 Uiso 1 1 calc R . . C1 C 0.28679(15) -0.19684(15) 0.08098(6) 0.0180(3) Uani 1 1 d . . . C6 C 0.18650(17) -0.25874(16) 0.04203(7) 0.0226(3) Uani 1 1 d . . . H6 H 0.1918 -0.2448 0.0013 0.027 Uiso 1 1 calc R . . C7 C 0.38409(16) -0.16545(17) 0.18810(7) 0.0224(3) Uani 1 1 d . . . C5 C 0.08025(17) -0.33919(17) 0.06012(7) 0.0250(4) Uani 1 1 d . . . H5 H 0.0153 -0.3782 0.0318 0.030 Uiso 1 1 calc R . . C11 C -0.04861(18) -0.44798(18) 0.14292(8) 0.0288(4) Uani 1 1 d . . . C18 C 0.4689(2) 0.34277(17) 0.02933(8) 0.0291(4) Uani 1 1 d . . . H18A H 0.4223 0.3964 -0.0032 0.035 Uiso 1 1 calc R . . H18B H 0.5665 0.3309 0.0218 0.035 Uiso 1 1 calc R . . C10 C 0.35735(18) -0.2094(2) 0.25039(7) 0.0310(4) Uani 1 1 d . . . H10A H 0.2678 -0.1742 0.2599 0.047 Uiso 1 1 calc R . . H10B H 0.4293 -0.1716 0.2781 0.047 Uiso 1 1 calc R . . H10C H 0.3578 -0.3105 0.2530 0.047 Uiso 1 1 calc R . . C19 C 0.83397(18) -0.04231(19) 0.05473(8) 0.0298(4) Uani 1 1 d . . . H19A H 0.8534 -0.0175 0.0144 0.036 Uiso 1 1 calc R . . H19B H 0.8335 -0.1443 0.0583 0.036 Uiso 1 1 calc R . . C8 C 0.52805(17) -0.2173(2) 0.17653(8) 0.0293(4) Uani 1 1 d . . . H8A H 0.5310 -0.3183 0.1798 0.044 Uiso 1 1 calc R . . H8B H 0.5959 -0.1767 0.2053 0.044 Uiso 1 1 calc R . . H8C H 0.5490 -0.1899 0.1371 0.044 Uiso 1 1 calc R . . C22 C 0.72236(19) 0.09455(19) 0.12130(7) 0.0296(4) Uani 1 1 d . . . H22A H 0.6477 0.0760 0.1470 0.036 Uiso 1 1 calc R . . H22B H 0.7234 0.1946 0.1123 0.036 Uiso 1 1 calc R . . C16 C 0.3372(2) 0.3444(2) 0.11321(8) 0.0355(4) Uani 1 1 d . . . H16A H 0.2639 0.4116 0.1202 0.043 Uiso 1 1 calc R . . H16B H 0.3677 0.2989 0.1507 0.043 Uiso 1 1 calc R . . C17 C 0.4562(2) 0.4154(2) 0.08736(9) 0.0387(5) Uani 1 1 d . . . H17A H 0.5415 0.4050 0.1133 0.046 Uiso 1 1 calc R . . H17B H 0.4372 0.5152 0.0813 0.046 Uiso 1 1 calc R . . C15 C 0.28652(18) 0.23788(18) 0.06757(8) 0.0277(4) Uani 1 1 d . . . H15A H 0.2557 0.1527 0.0865 0.033 Uiso 1 1 calc R . . H15B H 0.2094 0.2753 0.0417 0.033 Uiso 1 1 calc R . . C9 C 0.37945(19) -0.00669(17) 0.18605(8) 0.0283(4) Uani 1 1 d . . . H9A H 0.4017 0.0251 0.1474 0.042 Uiso 1 1 calc R . . H9B H 0.4464 0.0309 0.2160 0.042 Uiso 1 1 calc R . . H9C H 0.2873 0.0251 0.1935 0.042 Uiso 1 1 calc R . . C21 C 0.8587(2) 0.04958(19) 0.15046(8) 0.0350(4) Uani 1 1 d . . . H21A H 0.8491 -0.0343 0.1746 0.042 Uiso 1 1 calc R . . H21B H 0.9015 0.1240 0.1753 0.042 Uiso 1 1 calc R . . C13 C -0.1253(2) -0.3606(2) 0.18505(9) 0.0370(4) Uani 1 1 d . . . H13A H -0.1665 -0.2805 0.1642 0.055 Uiso 1 1 calc R . . H13B H -0.0610 -0.3289 0.2172 0.055 Uiso 1 1 calc R . . H13C H -0.1975 -0.4164 0.2007 0.055 Uiso 1 1 calc R . . C20 C 0.9407(2) 0.0199(2) 0.09841(9) 0.0378(5) Uani 1 1 d . . . H20A H 0.9796 0.1058 0.0831 0.045 Uiso 1 1 calc R . . H20B H 1.0160 -0.0463 0.1088 0.045 Uiso 1 1 calc R . . C14 C -0.1518(3) -0.4979(3) 0.09447(11) 0.0659(8) Uani 1 1 d . . . H14A H -0.1953 -0.4181 0.0743 0.099 Uiso 1 1 calc R . . H14B H -0.2220 -0.5543 0.1113 0.099 Uiso 1 1 calc R . . H14C H -0.1046 -0.5536 0.0666 0.099 Uiso 1 1 calc R . . C12 C 0.0111(2) -0.5747(2) 0.17729(13) 0.0571(7) Uani 1 1 d . . . H12A H -0.0621 -0.6209 0.1966 0.086 Uiso 1 1 calc R . . H12B H 0.0828 -0.5442 0.2068 0.086 Uiso 1 1 calc R . . H12C H 0.0503 -0.6393 0.1503 0.086 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 0.0181(2) 0.0168(2) 0.0149(2) 0.00014(16) 0.00412(15) -0.00277(16) O1 0.0235(6) 0.0239(6) 0.0206(5) 0.0029(4) 0.0073(4) -0.0062(5) O2 0.0298(6) 0.0200(6) 0.0296(6) -0.0019(5) 0.0116(5) -0.0019(5) O3 0.0223(6) 0.0362(7) 0.0193(5) -0.0044(5) 0.0011(4) -0.0017(5) C2 0.0184(7) 0.0173(7) 0.0186(7) 0.0005(6) 0.0042(6) 0.0014(6) C4 0.0214(8) 0.0192(7) 0.0270(8) -0.0018(6) 0.0096(6) -0.0044(6) C3 0.0236(8) 0.0191(7) 0.0198(7) 0.0027(6) 0.0075(6) 0.0002(6) C1 0.0193(7) 0.0154(7) 0.0201(7) 0.0021(6) 0.0061(6) -0.0005(6) C6 0.0249(8) 0.0255(8) 0.0179(7) 0.0003(6) 0.0039(6) -0.0025(6) C7 0.0196(8) 0.0288(8) 0.0189(7) 0.0000(6) 0.0029(6) -0.0023(6) C5 0.0245(8) 0.0251(8) 0.0255(8) -0.0044(7) 0.0021(6) -0.0050(6) C11 0.0259(9) 0.0246(8) 0.0375(10) -0.0018(7) 0.0130(7) -0.0081(7) C18 0.0364(10) 0.0196(8) 0.0327(9) -0.0006(7) 0.0119(7) -0.0048(7) C10 0.0277(9) 0.0469(11) 0.0184(8) 0.0019(7) 0.0010(7) -0.0026(8) C19 0.0259(9) 0.0327(9) 0.0305(9) -0.0053(7) 0.0005(7) 0.0035(7) C8 0.0204(8) 0.0408(10) 0.0267(8) 0.0019(7) 0.0017(7) 0.0007(7) C22 0.0313(9) 0.0332(9) 0.0249(8) -0.0066(7) 0.0045(7) -0.0062(7) C16 0.0356(10) 0.0384(10) 0.0339(9) -0.0105(8) 0.0114(8) -0.0026(8) C17 0.0454(12) 0.0329(10) 0.0394(10) -0.0090(8) 0.0131(9) -0.0095(8) C15 0.0237(8) 0.0312(9) 0.0291(9) -0.0036(7) 0.0070(7) 0.0013(7) C9 0.0310(9) 0.0265(8) 0.0277(9) -0.0074(7) 0.0046(7) -0.0064(7) C21 0.0450(11) 0.0290(9) 0.0287(9) -0.0011(8) -0.0100(8) -0.0046(8) C13 0.0294(10) 0.0323(9) 0.0519(12) 0.0016(9) 0.0203(9) -0.0036(8) C20 0.0241(9) 0.0405(11) 0.0473(12) -0.0100(9) -0.0064(8) 0.0034(8) C14 0.0549(15) 0.095(2) 0.0500(14) -0.0181(13) 0.0164(12) -0.0549(15) C12 0.0427(12) 0.0270(10) 0.107(2) 0.0196(12) 0.0422(13) 0.0010(9) _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 2.2061(11) . ? Ca1 O1 2.2061(11) 3_655 ? Ca1 O2 2.4073(12) 3_655 ? Ca1 O2 2.4073(12) . ? Ca1 O3 2.4361(14) 3_655 ? Ca1 O3 2.4361(14) . ? O1 C1 1.3156(18) . ? O2 C15 1.439(2) . ? O2 C18 1.4434(19) . ? O3 C22 1.439(2) . ? O3 C19 1.449(2) . ? C2 C3 1.389(2) . ? C2 C1 1.436(2) . ? C2 C7 1.535(2) . ? C4 C5 1.393(2) . ? C4 C3 1.402(2) . ? C4 C11 1.532(2) . ? C3 H3 0.9500 . ? C1 C6 1.406(2) . ? C6 C5 1.388(2) . ? C6 H6 0.9500 . ? C7 C10 1.534(2) . ? C7 C9 1.537(2) . ? C7 C8 1.537(2) . ? C5 H5 0.9500 . ? C11 C14 1.519(3) . ? C11 C13 1.525(2) . ? C11 C12 1.546(3) . ? C18 C17 1.520(2) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C19 C20 1.512(3) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C22 C21 1.507(3) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C16 C17 1.513(3) . ? C16 C15 1.523(2) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C21 C20 1.518(3) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 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 O1 180.00(7) . 3_655 ? O1 Ca1 O2 90.73(4) . 3_655 ? O1 Ca1 O2 89.27(4) 3_655 3_655 ? O1 Ca1 O2 89.27(4) . . ? O1 Ca1 O2 90.73(4) 3_655 . ? O2 Ca1 O2 180.00(7) 3_655 . ? O1 Ca1 O3 86.83(4) . 3_655 ? O1 Ca1 O3 93.17(4) 3_655 3_655 ? O2 Ca1 O3 93.30(4) 3_655 3_655 ? O2 Ca1 O3 86.70(4) . 3_655 ? O1 Ca1 O3 93.17(4) . . ? O1 Ca1 O3 86.83(4) 3_655 . ? O2 Ca1 O3 86.70(4) 3_655 . ? O2 Ca1 O3 93.30(4) . . ? O3 Ca1 O3 180.00(7) 3_655 . ? C1 O1 Ca1 159.80(10) . . ? C15 O2 C18 105.00(12) . . ? C15 O2 Ca1 132.78(9) . . ? C18 O2 Ca1 122.07(10) . . ? C22 O3 C19 109.26(13) . . ? C22 O3 Ca1 128.20(10) . . ? C19 O3 Ca1 121.80(9) . . ? C3 C2 C1 118.42(14) . . ? C3 C2 C7 121.00(13) . . ? C1 C2 C7 120.57(13) . . ? C5 C4 C3 116.04(14) . . ? C5 C4 C11 124.23(15) . . ? C3 C4 C11 119.73(14) . . ? C2 C3 C4 124.88(14) . . ? C2 C3 H3 117.6 . . ? C4 C3 H3 117.6 . . ? O1 C1 C6 120.76(13) . . ? O1 C1 C2 122.87(14) . . ? C6 C1 C2 116.36(13) . . ? C5 C6 C1 123.31(14) . . ? C5 C6 H6 118.3 . . ? C1 C6 H6 118.3 . . ? C10 C7 C2 112.41(13) . . ? C10 C7 C9 107.37(14) . . ? C2 C7 C9 109.52(13) . . ? C10 C7 C8 107.31(14) . . ? C2 C7 C8 109.95(13) . . ? C9 C7 C8 110.22(14) . . ? C6 C5 C4 120.94(15) . . ? C6 C5 H5 119.5 . . ? C4 C5 H5 119.5 . . ? C14 C11 C13 107.98(18) . . ? C14 C11 C4 112.17(15) . . ? C13 C11 C4 110.17(14) . . ? C14 C11 C12 108.83(19) . . ? C13 C11 C12 107.48(16) . . ? C4 C11 C12 110.08(14) . . ? O2 C18 C17 105.24(13) . . ? O2 C18 H18A 110.7 . . ? C17 C18 H18A 110.7 . . ? O2 C18 H18B 110.7 . . ? C17 C18 H18B 110.7 . . ? H18A C18 H18B 108.8 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? O3 C19 C20 106.23(14) . . ? O3 C19 H19A 110.5 . . ? C20 C19 H19A 110.5 . . ? O3 C19 H19B 110.5 . . ? C20 C19 H19B 110.5 . . ? H19A C19 H19B 108.7 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? O3 C22 C21 105.63(14) . . ? O3 C22 H22A 110.6 . . ? C21 C22 H22A 110.6 . . ? O3 C22 H22B 110.6 . . ? C21 C22 H22B 110.6 . . ? H22A C22 H22B 108.7 . . ? C17 C16 C15 104.82(14) . . ? C17 C16 H16A 110.8 . . ? C15 C16 H16A 110.8 . . ? C17 C16 H16B 110.8 . . ? C15 C16 H16B 110.8 . . ? H16A C16 H16B 108.9 . . ? C16 C17 C18 104.65(15) . . ? C16 C17 H17A 110.8 . . ? C18 C17 H17A 110.8 . . ? C16 C17 H17B 110.8 . . ? C18 C17 H17B 110.8 . . ? H17A C17 H17B 108.9 . . ? O2 C15 C16 104.69(14) . . ? O2 C15 H15A 110.8 . . ? C16 C15 H15A 110.8 . . ? O2 C15 H15B 110.8 . . ? C16 C15 H15B 110.8 . . ? H15A C15 H15B 108.9 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C22 C21 C20 102.10(15) . . ? C22 C21 H21A 111.3 . . ? C20 C21 H21A 111.3 . . ? C22 C21 H21B 111.3 . . ? C20 C21 H21B 111.3 . . ? H21A C21 H21B 109.2 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C19 C20 C21 102.51(15) . . ? C19 C20 H20A 111.3 . . ? C21 C20 H20A 111.3 . . ? C19 C20 H20B 111.3 . . ? C21 C20 H20B 111.3 . . ? H20A C20 H20B 109.2 . . ? C11 C14 H14A 109.5 . . ? C11 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C11 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.459 _refine_diff_density_min -0.412 _refine_diff_density_rms 0.058 data_[Ca2L4(dme)4(dme)].CIF _database_code_depnum_ccdc_archive 'CCDC 914478' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point '160C (dec. 220C)' _chemical_formula_moiety 'C76 H134 Ca2 O14' _chemical_formula_sum 'C76 H134 Ca2 O14' _chemical_formula_weight 1351.99 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 C2/c _symmetry_space_group_name_Hall '-C 2yc' 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 24.136(3) _cell_length_b 13.9781(14) _cell_length_c 25.508(4) _cell_angle_alpha 90.00 _cell_angle_beta 112.206(4) _cell_angle_gamma 90.00 _cell_volume 7967.5(17) _cell_formula_units_Z 4 _cell_measurement_temperature 123(1) _cell_measurement_reflns_used 7013 _cell_measurement_theta_min 1.98 _cell_measurement_theta_max 25 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.127 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2968 _exptl_absorpt_coefficient_mu 0.200 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.9610 _exptl_absorpt_correction_T_max 0.9802 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(1) _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 24237 _diffrn_reflns_av_R_equivalents 0.0720 _diffrn_reflns_av_sigmaI/netI 0.0795 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.98 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7013 _reflns_number_gt 4580 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker Apex2 v2.0 (Bruker AXS, 2005)' _computing_cell_refinement 'Bruker Apex2 v2.0 (Bruker AXS, 2005)' _computing_data_reduction 'Bruker Apex2 v2.0 (Bruker AXS, 2005)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 2001)' _computing_publication_material 'CIFTAB (Sheldrick, 1997)' _refine_special_details ; Turt-butyl groups exhibit large ratios of ADP max/min for carbon atoms due to freely rotating primary carbons.C12 and C14 was refined with occupancies of 80%/20% on two sites. Two chelating dme ligands displayed disorders. C32 was refined with occupancies of 50%/50% on two sites. 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^)+(0.2000P)^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 SHELXL _refine_ls_extinction_coef ? _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 7013 _refine_ls_number_parameters 462 _refine_ls_number_restraints 127 _refine_ls_R_factor_all 0.1104 _refine_ls_R_factor_gt 0.0719 _refine_ls_wR_factor_ref 0.1994 _refine_ls_wR_factor_gt 0.1760 _refine_ls_goodness_of_fit_ref 1.069 _refine_ls_restrained_S_all 1.191 _refine_ls_shift/su_max 0.001 _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 0.29260(3) 0.80478(6) 0.15953(3) 0.0226(2) Uani 1 1 d . B . O1 O 0.36201(12) 0.8178(2) 0.12403(12) 0.0333(7) Uani 1 1 d . . . C1 C 0.40738(17) 0.7948(3) 0.11036(16) 0.0247(9) Uani 1 1 d . . . O2 O 0.21880(12) 0.7897(2) 0.19175(11) 0.0303(7) Uani 1 1 d . . . C2 C 0.44259(16) 0.8627(3) 0.09568(16) 0.0221(9) Uani 1 1 d . . . O3 O 0.2928(2) 0.6250(2) 0.16627(17) 0.0647(12) Uani 1 1 d U B . C3 C 0.48779(17) 0.8298(3) 0.07922(16) 0.0274(9) Uani 1 1 d . . . H3 H 0.5107 0.8762 0.0690 0.033 Uiso 1 1 calc R . . O4 O 0.37787(17) 0.7370(4) 0.24112(18) 0.0833(15) Uani 1 1 d DU . . C4 C 0.5019(2) 0.7343(3) 0.07656(17) 0.0332(10) Uani 1 1 d . A . O5 O 0.33399(14) 0.9385(2) 0.23025(14) 0.0460(9) Uani 1 1 d U . . C5 C 0.4685(2) 0.6683(3) 0.09262(18) 0.0359(11) Uani 1 1 d . . . H5 H 0.4772 0.6021 0.0926 0.043 Uiso 1 1 calc R . . O6 O 0.25104(17) 0.9655(2) 0.12531(14) 0.0549(10) Uani 1 1 d U . . C6 C 0.4224(2) 0.6979(3) 0.10874(17) 0.0327(10) Uani 1 1 d . . . H6 H 0.4001 0.6508 0.1191 0.039 Uiso 1 1 calc R . . O7 O 0.22823(13) 0.7630(2) 0.06163(12) 0.0406(8) Uani 1 1 d . . . C7 C 0.43021(17) 0.9701(3) 0.09630(17) 0.0269(9) Uani 1 1 d . . . C8 C 0.4342(2) 1.0007(3) 0.15498(18) 0.0353(11) Uani 1 1 d . . . H8A H 0.4263 1.0695 0.1549 0.053 Uiso 1 1 calc R . . H8B H 0.4743 0.9869 0.1828 0.053 Uiso 1 1 calc R . . H8C H 0.4045 0.9655 0.1650 0.053 Uiso 1 1 calc R . . C9 C 0.3678(2) 0.9912(3) 0.0526(2) 0.0431(12) Uani 1 1 d . . . H9A H 0.3584 1.0590 0.0546 0.065 Uiso 1 1 calc R . . H9B H 0.3384 0.9517 0.0606 0.065 Uiso 1 1 calc R . . H9C H 0.3667 0.9764 0.0147 0.065 Uiso 1 1 calc R . . C10 C 0.4750(2) 1.0310(3) 0.0817(2) 0.0476(13) Uani 1 1 d . . . H10A H 0.4721 1.0157 0.0432 0.071 Uiso 1 1 calc R . . H10B H 0.5156 1.0174 0.1086 0.071 Uiso 1 1 calc R . . H10C H 0.4660 1.0989 0.0838 0.071 Uiso 1 1 calc R . . C11 C 0.5522(2) 0.7032(4) 0.05769(19) 0.0449(13) Uani 1 1 d D . . C12 C 0.5853(4) 0.7963(6) 0.0438(4) 0.072(2) Uani 0.80 1 d PU A 1 H12A H 0.6183 0.7749 0.0331 0.108 Uiso 0.80 1 calc PR A 1 H12B H 0.6012 0.8370 0.0775 0.108 Uiso 0.80 1 calc PR A 1 H12C H 0.5565 0.8327 0.0126 0.108 Uiso 0.80 1 calc PR A 1 C13 C 0.6041(2) 0.6673(5) 0.1073(3) 0.0706(18) Uani 1 1 d D A . H13A H 0.5934 0.6068 0.1204 0.106 Uiso 1 1 calc R . . H13B H 0.6148 0.7146 0.1379 0.106 Uiso 1 1 calc R . . H13C H 0.6383 0.6571 0.0962 0.106 Uiso 1 1 calc R . . C14 C 0.5322(4) 0.6489(9) 0.0074(4) 0.104(3) Uani 0.80 1 d PU A 1 H14A H 0.5006 0.6840 -0.0224 0.156 Uiso 0.80 1 calc PR A 1 H14B H 0.5164 0.5875 0.0141 0.156 Uiso 0.80 1 calc PR A 1 H14C H 0.5657 0.6375 -0.0046 0.156 Uiso 0.80 1 calc PR A 1 C15 C 0.20757(17) 0.8002(3) 0.23794(16) 0.0227(9) Uani 1 1 d . . . C16 C 0.14915(17) 0.8137(3) 0.23806(16) 0.0225(8) Uani 1 1 d . . . C17 C 0.14339(17) 0.8270(3) 0.28972(17) 0.0240(9) Uani 1 1 d . . . H17 H 0.1042 0.8357 0.2893 0.029 Uiso 1 1 calc R . . C18 C 0.19078(18) 0.8284(3) 0.34211(16) 0.0230(9) Uani 1 1 d . . . C19 C 0.24675(18) 0.8123(3) 0.34148(17) 0.0274(9) Uani 1 1 d . . . H19 H 0.2805 0.8106 0.3762 0.033 Uiso 1 1 calc R . . C20 C 0.25470(18) 0.7987(3) 0.29094(17) 0.0275(9) Uani 1 1 d . . . H20 H 0.2941 0.7877 0.2923 0.033 Uiso 1 1 calc R . . C21 C 0.09471(18) 0.8141(3) 0.18266(17) 0.0303(10) Uani 1 1 d . . . C22 C 0.0910(2) 0.7182(3) 0.15232(19) 0.0389(11) Uani 1 1 d . . . H22A H 0.1281 0.7076 0.1459 0.058 Uiso 1 1 calc R . . H22B H 0.0570 0.7193 0.1159 0.058 Uiso 1 1 calc R . . H22C H 0.0856 0.6664 0.1758 0.058 Uiso 1 1 calc R . . C23 C 0.0360(2) 0.8283(5) 0.1910(2) 0.0593(16) Uani 1 1 d . . . H23A H 0.0311 0.7772 0.2152 0.089 Uiso 1 1 calc R . . H23B H 0.0026 0.8265 0.1542 0.089 Uiso 1 1 calc R . . H23C H 0.0365 0.8904 0.2090 0.089 Uiso 1 1 calc R . . C24 C 0.1004(2) 0.8963(3) 0.14563(19) 0.0423(12) Uani 1 1 d . . . H24A H 0.0990 0.9574 0.1639 0.063 Uiso 1 1 calc R . . H24B H 0.0674 0.8934 0.1086 0.063 Uiso 1 1 calc R . . H24C H 0.1386 0.8909 0.1405 0.063 Uiso 1 1 calc R . . C25 C 0.1790(2) 0.8446(3) 0.39631(17) 0.0311(10) Uani 1 1 d . . . C26 C 0.1425(2) 0.9353(3) 0.3921(2) 0.0389(11) Uani 1 1 d . . . H26A H 0.1649 0.9907 0.3871 0.058 Uiso 1 1 calc R . . H26B H 0.1347 0.9432 0.4269 0.058 Uiso 1 1 calc R . . H26C H 0.1044 0.9303 0.3596 0.058 Uiso 1 1 calc R . . C27 C 0.1447(2) 0.7587(3) 0.4057(2) 0.0442(12) Uani 1 1 d U . . H27A H 0.1060 0.7535 0.3740 0.066 Uiso 1 1 calc R . . H27B H 0.1381 0.7673 0.4410 0.066 Uiso 1 1 calc R . . H27C H 0.1679 0.7003 0.4080 0.066 Uiso 1 1 calc R . . C28 C 0.2375(2) 0.8538(4) 0.44820(19) 0.0467(13) Uani 1 1 d U . . H28A H 0.2607 0.7947 0.4529 0.070 Uiso 1 1 calc R . . H28B H 0.2283 0.8649 0.4820 0.070 Uiso 1 1 calc R . . H28C H 0.2608 0.9077 0.4428 0.070 Uiso 1 1 calc R . . C29 C 0.2359(3) 0.5792(5) 0.1434(3) 0.086(2) Uani 1 1 d U . . H29A H 0.2410 0.5102 0.1504 0.129 Uiso 1 1 calc R . . H29B H 0.2178 0.5910 0.1026 0.129 Uiso 1 1 calc R . . H29C H 0.2099 0.6049 0.1616 0.129 Uiso 1 1 calc R . . C30 C 0.3255(4) 0.5958(4) 0.2227(3) 0.085(2) Uani 1 1 d U . . H30A H 0.3047 0.6176 0.2474 0.102 Uiso 1 1 calc R B . H30B H 0.3279 0.5251 0.2245 0.102 Uiso 1 1 calc R . . C31 C 0.3814(4) 0.6331(6) 0.2412(3) 0.097(2) Uani 1 1 d DU B . H31A H 0.4020 0.6121 0.2162 0.117 Uiso 1 1 calc R . . H31B H 0.4047 0.6100 0.2800 0.117 Uiso 1 1 calc R . . C32 C 0.4387(3) 0.7586(8) 0.2489(4) 0.043(2) Uani 0.50 1 d PDU B 1 H32A H 0.4645 0.7501 0.2888 0.064 Uiso 0.50 1 calc PR B 1 H32B H 0.4412 0.8250 0.2377 0.064 Uiso 0.50 1 calc PR B 1 H32C H 0.4517 0.7155 0.2255 0.064 Uiso 0.50 1 calc PR B 1 C33 C 0.3795(3) 0.9358(5) 0.2853(3) 0.091(2) Uani 1 1 d . B . H33A H 0.4157 0.9665 0.2846 0.136 Uiso 1 1 calc R . . H33B H 0.3883 0.8692 0.2975 0.136 Uiso 1 1 calc R . . H33C H 0.3659 0.9701 0.3117 0.136 Uiso 1 1 calc R . . C34 C 0.3096(3) 1.0296(4) 0.2159(2) 0.0610(16) Uani 1 1 d U B . H34A H 0.3040 1.0584 0.2489 0.073 Uiso 1 1 calc R . . H34B H 0.3381 1.0703 0.2064 0.073 Uiso 1 1 calc R . . C35 C 0.2553(3) 1.0283(4) 0.1703(3) 0.082(2) Uani 1 1 d U B . H35A H 0.2465 1.0940 0.1549 0.098 Uiso 1 1 calc R . . H35B H 0.2237 1.0107 0.1845 0.098 Uiso 1 1 calc R . . C36 C 0.2206(3) 0.9980(5) 0.0719(3) 0.0743(19) Uani 1 1 d U B . H36A H 0.1786 1.0088 0.0664 0.111 Uiso 1 1 calc R . . H36B H 0.2227 0.9505 0.0445 0.111 Uiso 1 1 calc R . . H36C H 0.2383 1.0582 0.0662 0.111 Uiso 1 1 calc R . . C37 C 0.1642(2) 0.7661(5) 0.0408(2) 0.0664(17) Uani 1 1 d U B . H37A H 0.1492 0.8075 0.0073 0.100 Uiso 1 1 calc R . . H37B H 0.1514 0.7914 0.0702 0.100 Uiso 1 1 calc R . . H37C H 0.1481 0.7014 0.0304 0.100 Uiso 1 1 calc R . . C38 C 0.2512(2) 0.7169(4) 0.02374(19) 0.0435(12) Uani 1 1 d U . . H38A H 0.2274 0.6588 0.0078 0.052 Uiso 1 1 calc R . . H38B H 0.2931 0.6970 0.0450 0.052 Uiso 1 1 calc R . . C12A C 0.5420(13) 0.7531(14) 0.0034(9) 0.054(7) Uani 0.20 1 d PDU A 2 H12D H 0.5740 0.7363 -0.0098 0.081 Uiso 0.20 1 calc PR A 2 H12E H 0.5420 0.8224 0.0092 0.081 Uiso 0.20 1 calc PR A 2 H12F H 0.5033 0.7335 -0.0250 0.081 Uiso 0.20 1 calc PR A 2 C14A C 0.5284(7) 0.5877(10) 0.0293(6) 0.021(4) Uani 0.20 1 d PDU A 2 H14D H 0.4875 0.5914 0.0010 0.032 Uiso 0.20 1 calc PR A 2 H14E H 0.5295 0.5442 0.0597 0.032 Uiso 0.20 1 calc PR A 2 H14F H 0.5551 0.5638 0.0113 0.032 Uiso 0.20 1 calc PR A 2 C32A C 0.4218(6) 0.8246(10) 0.2663(6) 0.084(4) Uani 0.50 1 d PDU B 2 H32D H 0.4513 0.8075 0.3037 0.127 Uiso 0.50 1 calc PR B 2 H32E H 0.3988 0.8803 0.2698 0.127 Uiso 0.50 1 calc PR B 2 H32F H 0.4426 0.8401 0.2410 0.127 Uiso 0.50 1 calc PR B 2 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 0.0249(4) 0.0249(4) 0.0214(4) -0.0018(3) 0.0126(3) 0.0004(3) O1 0.0288(16) 0.0405(18) 0.0381(17) -0.0111(14) 0.0212(14) -0.0093(13) C1 0.024(2) 0.031(2) 0.021(2) -0.0036(17) 0.0107(17) -0.0029(18) O2 0.0296(16) 0.0402(17) 0.0282(16) -0.0102(13) 0.0191(13) -0.0054(13) C2 0.018(2) 0.025(2) 0.021(2) -0.0007(16) 0.0051(17) 0.0010(16) O3 0.114(3) 0.0344(19) 0.081(3) 0.0115(18) 0.076(3) 0.017(2) C3 0.023(2) 0.036(2) 0.024(2) 0.0068(18) 0.0082(18) 0.0036(18) O4 0.051(2) 0.120(4) 0.072(3) 0.059(3) 0.014(2) 0.006(2) C4 0.039(3) 0.042(3) 0.019(2) 0.0068(19) 0.011(2) 0.019(2) O5 0.047(2) 0.0331(18) 0.044(2) -0.0098(15) 0.0010(16) -0.0082(15) C5 0.052(3) 0.029(2) 0.026(2) -0.0010(18) 0.013(2) 0.012(2) O6 0.089(3) 0.0405(19) 0.0369(19) 0.0108(15) 0.0262(19) 0.0286(18) C6 0.047(3) 0.025(2) 0.027(2) 0.0017(18) 0.015(2) -0.005(2) O7 0.0303(17) 0.069(2) 0.0278(17) -0.0206(15) 0.0167(14) -0.0112(15) C7 0.024(2) 0.021(2) 0.033(2) -0.0046(17) 0.0069(18) -0.0029(17) C8 0.037(3) 0.029(2) 0.036(3) -0.011(2) 0.010(2) -0.005(2) C9 0.042(3) 0.028(2) 0.043(3) -0.006(2) -0.002(2) 0.011(2) C10 0.059(3) 0.034(3) 0.053(3) 0.001(2) 0.025(3) -0.013(2) C11 0.044(3) 0.065(3) 0.030(3) 0.011(2) 0.017(2) 0.033(3) C12 0.069(5) 0.090(5) 0.084(5) 0.025(4) 0.058(4) 0.022(4) C13 0.042(3) 0.102(5) 0.073(4) 0.007(4) 0.027(3) 0.022(3) C14 0.084(6) 0.152(8) 0.097(6) -0.071(6) 0.059(5) -0.022(6) C15 0.028(2) 0.018(2) 0.026(2) -0.0054(16) 0.0149(18) -0.0037(17) C16 0.025(2) 0.022(2) 0.023(2) -0.0015(16) 0.0108(17) -0.0003(17) C17 0.021(2) 0.026(2) 0.030(2) -0.0033(17) 0.0153(18) -0.0026(16) C18 0.035(2) 0.0148(19) 0.023(2) 0.0001(15) 0.0160(19) -0.0011(16) C19 0.028(2) 0.024(2) 0.027(2) -0.0009(17) 0.0074(18) 0.0021(18) C20 0.021(2) 0.032(2) 0.033(2) -0.0063(19) 0.0140(18) 0.0015(18) C21 0.023(2) 0.041(3) 0.027(2) -0.0039(19) 0.0098(18) 0.0001(19) C22 0.037(3) 0.041(3) 0.034(3) -0.009(2) 0.008(2) -0.013(2) C23 0.022(2) 0.108(5) 0.041(3) -0.008(3) 0.004(2) 0.008(3) C24 0.053(3) 0.033(3) 0.029(2) -0.002(2) 0.003(2) 0.005(2) C25 0.043(3) 0.029(2) 0.026(2) 0.0027(18) 0.019(2) 0.001(2) C26 0.056(3) 0.034(3) 0.039(3) -0.002(2) 0.031(2) 0.002(2) C27 0.063(3) 0.043(3) 0.040(3) 0.005(2) 0.034(3) -0.005(2) C28 0.061(3) 0.053(3) 0.028(3) -0.004(2) 0.019(2) -0.001(3) C29 0.108(4) 0.055(3) 0.126(5) -0.006(3) 0.080(4) -0.008(3) C30 0.163(5) 0.044(3) 0.067(4) 0.013(3) 0.064(4) 0.025(3) C31 0.125(5) 0.122(5) 0.057(3) 0.027(3) 0.047(3) 0.078(4) C32 0.025(5) 0.080(6) 0.023(4) -0.002(4) 0.009(4) 0.029(4) C33 0.080(5) 0.081(5) 0.069(5) -0.002(4) -0.020(4) -0.025(4) C34 0.088(4) 0.043(3) 0.060(4) -0.016(3) 0.037(3) 0.009(3) C35 0.096(5) 0.049(3) 0.076(4) -0.020(3) 0.003(4) 0.028(3) C36 0.091(4) 0.076(4) 0.067(4) 0.032(3) 0.042(3) 0.044(3) C37 0.034(3) 0.128(5) 0.042(3) -0.028(3) 0.020(2) -0.015(3) C38 0.041(3) 0.063(3) 0.035(3) -0.024(2) 0.024(2) -0.016(2) C12A 0.070(11) 0.060(11) 0.049(10) 0.005(8) 0.043(9) 0.013(9) C14A 0.022(6) 0.023(6) 0.024(6) -0.009(5) 0.014(5) 0.004(5) C32A 0.067(7) 0.094(8) 0.077(8) 0.012(7) 0.010(6) -0.012(7) _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 2.192(3) . ? Ca1 O2 2.236(3) . ? Ca1 O7 2.462(3) . ? Ca1 O6 2.481(3) . ? Ca1 O4 2.495(4) . ? Ca1 O3 2.518(3) . ? Ca1 O5 2.526(3) . ? O1 C1 1.309(5) . ? C1 C6 1.407(6) . ? C1 C2 1.416(5) . ? O2 C15 1.313(4) . ? C2 C3 1.387(5) . ? C2 C7 1.532(5) . ? O3 C30 1.415(7) . ? O3 C29 1.424(7) . ? C3 C4 1.387(6) . ? C3 H3 0.9500 . ? O4 C32 1.436(9) . ? O4 C31 1.455(9) . ? O4 C32A 1.588(12) . ? C4 C5 1.386(6) . ? C4 C11 1.527(6) . ? O5 C34 1.393(6) . ? O5 C33 1.418(6) . ? C5 C6 1.386(6) . ? C5 H5 0.9500 . ? O6 C36 1.359(6) . ? O6 C35 1.418(6) . ? C6 H6 0.9500 . ? O7 C37 1.433(6) . ? O7 C38 1.436(5) . ? C7 C8 1.525(6) . ? C7 C9 1.525(6) . ? C7 C10 1.528(6) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C14 1.410(9) . ? C11 C12A 1.485(16) . ? C11 C13 1.492(7) . ? C11 C12 1.635(9) . ? C11 C14A 1.773(12) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C20 1.400(6) . ? C15 C16 1.424(5) . ? C16 C17 1.389(5) . ? C16 C21 1.523(5) . ? C17 C18 1.392(5) . ? C17 H17 0.9500 . ? C18 C19 1.376(6) . ? C18 C25 1.530(5) . ? C19 C20 1.386(6) . ? C19 H19 0.9500 . ? C20 H20 0.9500 . ? C21 C23 1.524(6) . ? C21 C24 1.527(6) . ? C21 C22 1.533(6) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C26 1.524(6) . ? C25 C27 1.528(6) . ? C25 C28 1.532(6) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 C31 1.354(10) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 C35 1.386(8) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 C38 1.508(10) 7_565 ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C12A H12D 0.9800 . ? C12A H12E 0.9800 . ? C12A H12F 0.9800 . ? C14A H14D 0.9800 . ? C14A H14E 0.9800 . ? C14A H14F 0.9800 . ? C32A H32D 0.9800 . ? C32A H32E 0.9800 . ? C32A H32F 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 177.34(11) . . ? O1 Ca1 O7 83.59(10) . . ? O2 Ca1 O7 93.75(10) . . ? O1 Ca1 O6 92.87(12) . . ? O2 Ca1 O6 86.70(12) . . ? O7 Ca1 O6 80.90(12) . . ? O1 Ca1 O4 81.83(13) . . ? O2 Ca1 O4 100.26(12) . . ? O7 Ca1 O4 139.59(15) . . ? O6 Ca1 O4 137.18(15) . . ? O1 Ca1 O3 97.41(11) . . ? O2 Ca1 O3 82.05(11) . . ? O7 Ca1 O3 79.42(13) . . ? O6 Ca1 O3 156.59(14) . . ? O4 Ca1 O3 65.47(16) . . ? O1 Ca1 O5 94.37(11) . . ? O2 Ca1 O5 87.84(11) . . ? O7 Ca1 O5 145.86(11) . . ? O6 Ca1 O5 65.13(11) . . ? O4 Ca1 O5 72.92(15) . . ? O3 Ca1 O5 134.37(13) . . ? C1 O1 Ca1 159.5(3) . . ? O1 C1 C6 119.7(4) . . ? O1 C1 C2 123.5(4) . . ? C6 C1 C2 116.8(4) . . ? C15 O2 Ca1 141.5(2) . . ? C3 C2 C1 118.5(4) . . ? C3 C2 C7 120.4(3) . . ? C1 C2 C7 121.1(3) . . ? C30 O3 C29 111.5(5) . . ? C30 O3 Ca1 110.1(3) . . ? C29 O3 Ca1 116.4(4) . . ? C4 C3 C2 124.8(4) . . ? C4 C3 H3 117.6 . . ? C2 C3 H3 117.6 . . ? C32 O4 C31 98.9(6) . . ? C32 O4 C32A 44.8(6) . . ? C31 O4 C32A 137.7(7) . . ? C32 O4 Ca1 120.9(4) . . ? C31 O4 Ca1 114.1(4) . . ? C32A O4 Ca1 105.0(6) . . ? C5 C4 C3 116.4(4) . . ? C5 C4 C11 121.6(4) . . ? C3 C4 C11 122.0(4) . . ? C34 O5 C33 112.1(4) . . ? C34 O5 Ca1 118.4(3) . . ? C33 O5 Ca1 129.5(3) . . ? C4 C5 C6 120.8(4) . . ? C4 C5 H5 119.6 . . ? C6 C5 H5 119.6 . . ? C36 O6 C35 116.8(4) . . ? C36 O6 Ca1 130.5(3) . . ? C35 O6 Ca1 112.3(3) . . ? C5 C6 C1 122.7(4) . . ? C5 C6 H6 118.6 . . ? C1 C6 H6 118.6 . . ? C37 O7 C38 113.6(3) . . ? C37 O7 Ca1 123.3(3) . . ? C38 O7 Ca1 122.2(3) . . ? C8 C7 C9 110.0(4) . . ? C8 C7 C10 107.2(3) . . ? C9 C7 C10 107.9(4) . . ? C8 C7 C2 110.2(3) . . ? C9 C7 C2 108.9(3) . . ? C10 C7 C2 112.6(3) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C14 C11 C12A 61.6(9) . . ? C14 C11 C13 118.8(6) . . ? C12A C11 C13 137.6(12) . . ? C14 C11 C4 113.6(5) . . ? C12A C11 C4 106.8(10) . . ? C13 C11 C4 109.9(4) . . ? C14 C11 C12 105.0(6) . . ? C12A C11 C12 49.2(10) . . ? C13 C11 C12 97.3(5) . . ? C4 C11 C12 110.7(4) . . ? C14 C11 C14A 36.1(7) . . ? C12A C11 C14A 97.6(8) . . ? C13 C11 C14A 94.6(6) . . ? C4 C11 C14A 102.4(7) . . ? C12 C11 C14A 138.2(7) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C11 C14 H14A 109.5 . . ? C11 C14 H14B 109.5 . . ? C11 C14 H14C 109.5 . . ? O2 C15 C20 119.8(3) . . ? O2 C15 C16 123.9(4) . . ? C20 C15 C16 116.3(3) . . ? C17 C16 C15 118.3(4) . . ? C17 C16 C21 121.3(3) . . ? C15 C16 C21 120.4(3) . . ? C16 C17 C18 124.9(4) . . ? C16 C17 H17 117.6 . . ? C18 C17 H17 117.6 . . ? C19 C18 C17 116.1(4) . . ? C19 C18 C25 123.6(4) . . ? C17 C18 C25 120.2(4) . . ? C18 C19 C20 121.0(4) . . ? C18 C19 H19 119.5 . . ? C20 C19 H19 119.5 . . ? C19 C20 C15 123.3(4) . . ? C19 C20 H20 118.4 . . ? C15 C20 H20 118.4 . . ? C16 C21 C23 113.1(3) . . ? C16 C21 C24 109.2(3) . . ? C23 C21 C24 107.1(4) . . ? C16 C21 C22 109.3(3) . . ? C23 C21 C22 107.7(4) . . ? C24 C21 C22 110.3(4) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C21 C24 H24A 109.5 . . ? C21 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C21 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C26 C25 C27 109.3(4) . . ? C26 C25 C18 111.1(3) . . ? C27 C25 C18 108.8(3) . . ? C26 C25 C28 108.1(4) . . ? C27 C25 C28 107.9(4) . . ? C18 C25 C28 111.6(4) . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C25 C28 H28A 109.5 . . ? C25 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C25 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? O3 C29 H29A 109.5 . . ? O3 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? O3 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C31 C30 O3 110.0(6) . . ? C31 C30 H30A 109.7 . . ? O3 C30 H30A 109.7 . . ? C31 C30 H30B 109.7 . . ? O3 C30 H30B 109.7 . . ? H30A C30 H30B 108.2 . . ? C30 C31 O4 109.6(5) . . ? C30 C31 H31A 109.8 . . ? O4 C31 H31A 109.8 . . ? C30 C31 H31B 109.8 . . ? O4 C31 H31B 109.8 . . ? H31A C31 H31B 108.2 . . ? O4 C32 H32A 109.5 . . ? O4 C32 H32B 109.5 . . ? O4 C32 H32C 109.5 . . ? O5 C33 H33A 109.5 . . ? O5 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? O5 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C35 C34 O5 112.4(5) . . ? C35 C34 H34A 109.1 . . ? O5 C34 H34A 109.1 . . ? C35 C34 H34B 109.1 . . ? O5 C34 H34B 109.1 . . ? H34A C34 H34B 107.9 . . ? C34 C35 O6 116.3(5) . . ? C34 C35 H35A 108.2 . . ? O6 C35 H35A 108.2 . . ? C34 C35 H35B 108.2 . . ? O6 C35 H35B 108.2 . . ? H35A C35 H35B 107.4 . . ? O6 C36 H36A 109.5 . . ? O6 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? O6 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? O7 C37 H37A 109.5 . . ? O7 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? O7 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? O7 C38 C38 111.0(5) . 7_565 ? O7 C38 H38A 109.4 . . ? C38 C38 H38A 109.4 7_565 . ? O7 C38 H38B 109.4 . . ? C38 C38 H38B 109.4 7_565 . ? H38A C38 H38B 108.0 . . ? C11 C12A H12D 109.5 . . ? C11 C12A H12E 109.5 . . ? H12D C12A H12E 109.5 . . ? C11 C12A H12F 109.5 . . ? H12D C12A H12F 109.5 . . ? H12E C12A H12F 109.5 . . ? C11 C14A H14D 109.5 . . ? C11 C14A H14E 109.5 . . ? H14D C14A H14E 109.5 . . ? C11 C14A H14F 109.5 . . ? H14D C14A H14F 109.5 . . ? H14E C14A H14F 109.5 . . ? O4 C32A H32D 109.5 . . ? O4 C32A H32E 109.5 . . ? H32D C32A H32E 109.5 . . ? O4 C32A H32F 109.5 . . ? H32D C32A H32F 109.5 . . ? H32E C32A H32F 109.5 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.711 _refine_diff_density_min -0.483 _refine_diff_density_rms 0.068 data_[Sr3L6(thf)6].CIF _database_code_depnum_ccdc_archive 'CCDC 914479' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point 'Dec. (150C)' _chemical_formula_moiety 'C108 H174 O12 Sr3, C6 H6' _chemical_formula_sum 'C114 H180 O12 Sr3' _chemical_formula_weight 2005.44 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 trigonal _symmetry_space_group_name_H-M R-3C _symmetry_space_group_name_Hall '-R 3 2"c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x-y, -y, -z+1/2' '-x, -x+y, -z+1/2' 'y, x, -z+1/2' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x-y+2/3, -y+1/3, -z+5/6' '-x+2/3, -x+y+1/3, -z+5/6' 'y+2/3, x+1/3, -z+5/6' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' 'x-y+1/3, -y+2/3, -z+7/6' '-x+1/3, -x+y+2/3, -z+7/6' 'y+1/3, x+2/3, -z+7/6' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+y, y, z-1/2' 'x, x-y, z-1/2' '-y, -x, z-1/2' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+y+2/3, y+1/3, z-1/6' 'x+2/3, x-y+1/3, z-1/6' '-y+2/3, -x+1/3, z-1/6' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' '-x+y+1/3, y+2/3, z+1/6' 'x+1/3, x-y+2/3, z+1/6' '-y+1/3, -x+2/3, z+1/6' _cell_length_a 21.738(3) _cell_length_b 21.738(3) _cell_length_c 40.897(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 16737(5) _cell_formula_units_Z 6 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 3272 _cell_measurement_theta_min 2.27 _cell_measurement_theta_max 25.00 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.04 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.194 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6444 _exptl_absorpt_coefficient_mu 1.485 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9430 _exptl_absorpt_correction_T_max 0.9853 _exptl_absorpt_process_details XDS _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Synchrotron _diffrn_radiation_source 'Australian Synchrotron' _diffrn_radiation_monochromator 'Silicon Double Crystal' _diffrn_measurement_device_type 'ADSC Quantum 210r' _diffrn_measurement_method 'Phi Scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 68739 _diffrn_reflns_av_R_equivalents 0.0561 _diffrn_reflns_av_sigmaI/netI 0.0160 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -48 _diffrn_reflns_limit_l_max 48 _diffrn_reflns_theta_min 2.27 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3272 _reflns_number_gt 3103 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'BluIce (McPhillips, 2002)' _computing_cell_refinement 'XDS (Kabsch, 1993)' _computing_data_reduction 'XDS (Kabsch, 1993)' _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 ; Turt-butyl groups exhibit large ratios of ADP max/min for carbon atoms due to freely rotating primary carbons. 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^)+(0.0460P)^2^+140.8476P] 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 3272 _refine_ls_number_parameters 201 _refine_ls_number_restraints 24 _refine_ls_R_factor_all 0.0539 _refine_ls_R_factor_gt 0.0521 _refine_ls_wR_factor_ref 0.1250 _refine_ls_wR_factor_gt 0.1238 _refine_ls_goodness_of_fit_ref 1.101 _refine_ls_restrained_S_all 1.120 _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 0.6667 0.3333 -0.003638(11) 0.01695(17) Uani 1 3 d S . . O1 O 0.66721(10) 0.41522(11) 0.03747(5) 0.0169(4) Uani 1 1 d . . . C1 C 0.71791(15) 0.48340(15) 0.03721(7) 0.0147(6) Uani 1 1 d . . . Sr2 Sr 0.6667 0.3333 0.0833 0.01471(18) Uani 1 6 d S . . O2 O 0.73885(14) 0.43850(14) -0.04544(6) 0.0333(6) Uani 1 1 d . . . C2 C 0.70595(16) 0.54022(16) 0.02841(7) 0.0191(6) Uani 1 1 d . . . C3 C 0.76402(17) 0.60901(17) 0.02906(8) 0.0226(7) Uani 1 1 d . . . H3 H 0.7564 0.6467 0.0227 0.027 Uiso 1 1 calc R . . C4 C 0.83304(17) 0.62664(17) 0.03849(8) 0.0232(7) Uani 1 1 d . . . C5 C 0.84329(16) 0.57073(17) 0.04673(7) 0.0198(6) Uani 1 1 d . . . H5 H 0.8892 0.5800 0.0530 0.024 Uiso 1 1 calc R . . C6 C 0.78746(16) 0.50150(16) 0.04597(7) 0.0173(6) Uani 1 1 d . . . H6 H 0.7966 0.4644 0.0516 0.021 Uiso 1 1 calc R . . C7 C 0.63174(17) 0.52672(18) 0.01904(8) 0.0254(7) Uani 1 1 d . . . C8 C 0.58103(18) 0.49423(19) 0.04779(9) 0.0284(8) Uani 1 1 d . . . H8A H 0.5971 0.5282 0.0659 0.043 Uiso 1 1 calc R . . H8B H 0.5802 0.4507 0.0548 0.043 Uiso 1 1 calc R . . H8C H 0.5332 0.4829 0.0411 0.043 Uiso 1 1 calc R . . C9 C 0.6011(2) 0.4731(3) -0.00969(10) 0.0522(12) Uani 1 1 d . . . H9A H 0.5547 0.4664 -0.0160 0.078 Uiso 1 1 calc R . . H9B H 0.5957 0.4274 -0.0028 0.078 Uiso 1 1 calc R . . H9C H 0.6336 0.4915 -0.0284 0.078 Uiso 1 1 calc R . . C10 C 0.6317(2) 0.5939(3) 0.00872(15) 0.0667(17) Uani 1 1 d . . . H10A H 0.5836 0.5819 0.0022 0.100 Uiso 1 1 calc R . . H10B H 0.6642 0.6158 -0.0097 0.100 Uiso 1 1 calc R . . H10C H 0.6472 0.6273 0.0271 0.100 Uiso 1 1 calc R . . C11 C 0.89285(19) 0.70473(18) 0.03861(10) 0.0344(9) Uani 1 1 d . . . C12 C 0.9574(2) 0.7130(2) 0.05755(16) 0.0667(16) Uani 1 1 d . . . H12A H 0.9940 0.7633 0.0584 0.100 Uiso 1 1 calc R . . H12B H 0.9765 0.6861 0.0465 0.100 Uiso 1 1 calc R . . H12C H 0.9430 0.6949 0.0798 0.100 Uiso 1 1 calc R . . C13 C 0.8679(2) 0.7516(2) 0.05499(12) 0.0448(10) Uani 1 1 d . . . H13A H 0.8511 0.7341 0.0772 0.067 Uiso 1 1 calc R . . H13B H 0.8290 0.7502 0.0422 0.067 Uiso 1 1 calc R . . H13C H 0.9075 0.8006 0.0561 0.067 Uiso 1 1 calc R . . C14 C 0.9144(3) 0.7291(2) 0.00338(12) 0.0597(14) Uani 1 1 d . . . H14A H 0.8745 0.7281 -0.0082 0.090 Uiso 1 1 calc R . . H14B H 0.9276 0.6972 -0.0076 0.090 Uiso 1 1 calc R . . H14C H 0.9551 0.7776 0.0033 0.090 Uiso 1 1 calc R . . C15 C 0.8049(3) 0.5039(3) -0.03979(10) 0.0608(14) Uani 1 1 d U . . H15A H 0.8464 0.4988 -0.0454 0.073 Uiso 1 1 calc R . . H15B H 0.8089 0.5197 -0.0168 0.073 Uiso 1 1 calc R . . C16 C 0.7975(4) 0.5555(3) -0.06344(14) 0.0787(19) Uani 1 1 d U . . H16A H 0.7671 0.5728 -0.0539 0.094 Uiso 1 1 calc R . . H16B H 0.8445 0.5967 -0.0689 0.094 Uiso 1 1 calc R . . C17 C 0.7635(3) 0.5103(3) -0.09294(13) 0.0667(15) Uani 1 1 d U . . H17A H 0.7407 0.5301 -0.1071 0.080 Uiso 1 1 calc R . . H17B H 0.7977 0.5029 -0.1060 0.080 Uiso 1 1 calc R . . C18 C 0.7119(3) 0.4461(3) -0.07651(11) 0.0601(14) Uani 1 1 d U . . H18A H 0.6676 0.4475 -0.0730 0.072 Uiso 1 1 calc R . . H18B H 0.7006 0.4045 -0.0904 0.072 Uiso 1 1 calc R . . C19 C 0.07077(19) 0.0181(2) 0.00002(9) 0.0308(8) Uani 1 1 d . . . H19 H 0.1193 0.0305 0.0001 0.037 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 0.0197(2) 0.0197(2) 0.0114(3) 0.000 0.000 0.00986(10) O1 0.0170(10) 0.0129(10) 0.0192(10) 0.0000(8) 0.0002(8) 0.0064(9) C1 0.0177(14) 0.0147(14) 0.0110(13) -0.0009(11) 0.0010(11) 0.0076(12) Sr2 0.0159(2) 0.0159(2) 0.0123(3) 0.000 0.000 0.00796(12) O2 0.0404(15) 0.0350(14) 0.0196(12) 0.0092(10) 0.0042(10) 0.0153(12) C2 0.0181(15) 0.0202(15) 0.0197(15) 0.0061(12) 0.0017(12) 0.0102(13) C3 0.0216(16) 0.0171(15) 0.0311(17) 0.0092(13) 0.0037(13) 0.0112(13) C4 0.0201(16) 0.0157(16) 0.0293(17) 0.0011(13) 0.0059(13) 0.0056(13) C5 0.0157(15) 0.0235(16) 0.0201(15) -0.0018(12) -0.0009(12) 0.0097(13) C6 0.0198(15) 0.0178(15) 0.0172(14) -0.0004(11) -0.0007(12) 0.0116(13) C7 0.0209(16) 0.0309(18) 0.0286(17) 0.0136(14) 0.0021(13) 0.0160(15) C8 0.0242(17) 0.036(2) 0.0342(19) 0.0071(15) 0.0054(14) 0.0222(16) C9 0.043(2) 0.097(4) 0.034(2) -0.017(2) -0.0158(18) 0.047(3) C10 0.031(2) 0.051(3) 0.126(5) 0.050(3) 0.006(3) 0.026(2) C11 0.0246(18) 0.0153(16) 0.055(2) 0.0021(16) 0.0078(17) 0.0036(15) C12 0.030(2) 0.024(2) 0.129(5) -0.013(3) -0.022(3) 0.0003(18) C13 0.041(2) 0.0216(19) 0.065(3) -0.0055(19) 0.008(2) 0.0097(17) C14 0.065(3) 0.024(2) 0.069(3) 0.012(2) 0.039(3) 0.006(2) C15 0.058(3) 0.056(3) 0.026(2) 0.0050(19) 0.0091(19) -0.003(2) C16 0.117(5) 0.039(3) 0.083(4) 0.025(3) 0.057(3) 0.041(3) C17 0.068(3) 0.092(4) 0.059(3) 0.033(3) 0.017(3) 0.054(3) C18 0.067(3) 0.083(4) 0.034(2) 0.029(2) 0.006(2) 0.040(3) C19 0.0236(18) 0.0302(18) 0.0387(19) 0.0009(16) 0.0007(15) 0.0135(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 Sr1 O1 2.444(2) 3_665 ? Sr1 O1 2.444(2) 2_655 ? Sr1 O1 2.444(2) . ? Sr1 O2 2.650(2) 3_665 ? Sr1 O2 2.650(2) . ? Sr1 O2 2.650(2) 2_655 ? Sr1 C1 3.323(3) 3_665 ? Sr1 C1 3.323(3) 2_655 ? O1 C1 1.333(4) . ? O1 Sr2 2.582(2) . ? C1 C6 1.405(4) . ? C1 C2 1.429(4) . ? Sr2 O1 2.582(2) 3_665 ? Sr2 O1 2.582(2) 2_655 ? Sr2 O1 2.582(2) 18_544 ? Sr2 O1 2.582(2) 16_554 ? Sr2 O1 2.582(2) 17_654 ? Sr2 Sr1 3.5567(8) 16_554 ? O2 C18 1.442(5) . ? O2 C15 1.447(5) . ? C2 C3 1.394(4) . ? C2 C7 1.537(4) . ? C3 C4 1.404(5) . ? C3 H3 0.9500 . ? C4 C5 1.383(5) . ? C4 C11 1.538(4) . ? C5 C6 1.383(4) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C10 1.521(5) . ? C7 C8 1.523(4) . ? C7 C9 1.552(5) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C14 1.526(6) . ? C11 C13 1.529(5) . ? C11 C12 1.533(6) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C16 1.548(7) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.497(9) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.447(7) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C19 1.384(4) 20 ? C19 C19 1.384(4) 21 ? C19 H19 0.9500 . ? 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 O1 77.90(7) 3_665 2_655 ? O1 Sr1 O1 77.90(7) 3_665 . ? O1 Sr1 O1 77.90(7) 2_655 . ? O1 Sr1 O2 91.74(7) 3_665 3_665 ? O1 Sr1 O2 109.28(7) 2_655 3_665 ? O1 Sr1 O2 166.09(7) . 3_665 ? O1 Sr1 O2 109.28(7) 3_665 . ? O1 Sr1 O2 166.09(7) 2_655 . ? O1 Sr1 O2 91.74(7) . . ? O2 Sr1 O2 82.86(8) 3_665 . ? O1 Sr1 O2 166.09(7) 3_665 2_655 ? O1 Sr1 O2 91.74(7) 2_655 2_655 ? O1 Sr1 O2 109.28(7) . 2_655 ? O2 Sr1 O2 82.86(8) 3_665 2_655 ? O2 Sr1 O2 82.86(8) . 2_655 ? O1 Sr1 C1 20.28(7) 3_665 3_665 ? O1 Sr1 C1 76.75(7) 2_655 3_665 ? O1 Sr1 C1 97.46(7) . 3_665 ? O2 Sr1 C1 73.39(7) 3_665 3_665 ? O2 Sr1 C1 114.22(8) . 3_665 ? O2 Sr1 C1 148.05(8) 2_655 3_665 ? O1 Sr1 C1 97.46(7) 3_665 2_655 ? O1 Sr1 C1 20.28(7) 2_655 2_655 ? O1 Sr1 C1 76.75(7) . 2_655 ? O2 Sr1 C1 114.22(8) 3_665 2_655 ? O2 Sr1 C1 148.05(8) . 2_655 ? O2 Sr1 C1 73.39(7) 2_655 2_655 ? C1 Sr1 C1 96.94(6) 3_665 2_655 ? C1 O1 Sr1 120.27(17) . . ? C1 O1 Sr2 119.25(17) . . ? Sr1 O1 Sr2 90.05(7) . . ? O1 C1 C6 119.0(3) . . ? O1 C1 C2 123.8(3) . . ? C6 C1 C2 117.2(3) . . ? O1 Sr2 O1 73.05(7) 3_665 2_655 ? O1 Sr2 O1 73.05(7) 3_665 . ? O1 Sr2 O1 73.05(7) 2_655 . ? O1 Sr2 O1 93.18(9) 3_665 18_544 ? O1 Sr2 O1 140.22(9) 2_655 18_544 ? O1 Sr2 O1 139.39(9) . 18_544 ? O1 Sr2 O1 139.38(9) 3_665 16_554 ? O1 Sr2 O1 93.18(9) 2_655 16_554 ? O1 Sr2 O1 140.23(9) . 16_554 ? O1 Sr2 O1 73.05(7) 18_544 16_554 ? O1 Sr2 O1 140.22(9) 3_665 17_654 ? O1 Sr2 O1 139.39(9) 2_655 17_654 ? O1 Sr2 O1 93.18(9) . 17_654 ? O1 Sr2 O1 73.05(7) 18_544 17_654 ? O1 Sr2 O1 73.05(7) 16_554 17_654 ? O1 Sr2 Sr1 136.59(5) 3_665 16_554 ? O1 Sr2 Sr1 136.59(5) 2_655 16_554 ? O1 Sr2 Sr1 136.59(5) . 16_554 ? O1 Sr2 Sr1 43.41(5) 18_544 16_554 ? O1 Sr2 Sr1 43.41(5) 16_554 16_554 ? O1 Sr2 Sr1 43.41(5) 17_654 16_554 ? C18 O2 C15 106.8(3) . . ? C18 O2 Sr1 124.6(3) . . ? C15 O2 Sr1 127.8(2) . . ? C3 C2 C1 117.6(3) . . ? C3 C2 C7 120.7(3) . . ? C1 C2 C7 121.7(3) . . ? C2 C3 C4 124.7(3) . . ? C2 C3 H3 117.7 . . ? C4 C3 H3 117.7 . . ? C5 C4 C3 116.6(3) . . ? C5 C4 C11 123.4(3) . . ? C3 C4 C11 120.0(3) . . ? C4 C5 C6 120.8(3) . . ? C4 C5 H5 119.6 . . ? C6 C5 H5 119.6 . . ? C5 C6 C1 123.1(3) . . ? C5 C6 H6 118.4 . . ? C1 C6 H6 118.4 . . ? C10 C7 C8 108.1(3) . . ? C10 C7 C2 113.0(3) . . ? C8 C7 C2 110.1(3) . . ? C10 C7 C9 107.8(4) . . ? C8 C7 C9 107.3(3) . . ? C2 C7 C9 110.3(3) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C14 C11 C13 109.4(3) . . ? C14 C11 C12 109.4(4) . . ? C13 C11 C12 108.1(4) . . ? C14 C11 C4 108.9(3) . . ? C13 C11 C4 110.6(3) . . ? C12 C11 C4 110.5(3) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C11 C14 H14A 109.5 . . ? C11 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C11 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? O2 C15 C16 101.6(4) . . ? O2 C15 H15A 111.5 . . ? C16 C15 H15A 111.5 . . ? O2 C15 H15B 111.5 . . ? C16 C15 H15B 111.5 . . ? H15A C15 H15B 109.3 . . ? C17 C16 C15 103.0(4) . . ? C17 C16 H16A 111.2 . . ? C15 C16 H16A 111.2 . . ? C17 C16 H16B 111.2 . . ? C15 C16 H16B 111.2 . . ? H16A C16 H16B 109.1 . . ? C18 C17 C16 98.6(4) . . ? C18 C17 H17A 112.1 . . ? C16 C17 H17A 112.1 . . ? C18 C17 H17B 112.1 . . ? C16 C17 H17B 112.1 . . ? H17A C17 H17B 109.7 . . ? O2 C18 C17 110.9(4) . . ? O2 C18 H18A 109.5 . . ? C17 C18 H18A 109.5 . . ? O2 C18 H18B 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 108.1 . . ? C19 C19 C19 120.000(4) 20 21 ? C19 C19 H19 120.0 20 . ? C19 C19 H19 120.0 21 . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.712 _refine_diff_density_min -1.382 _refine_diff_density_rms 0.079 data_[Sr2L4(dme)3].CIF _database_code_depnum_ccdc_archive 'CCDC 914480' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point dec.(260C) _chemical_formula_moiety 'C68 H114 O10 Sr2' _chemical_formula_sum 'C68 H114 O10 Sr2' _chemical_formula_weight 1266.83 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/n _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 16.312(3) _cell_length_b 25.924(5) _cell_length_c 16.982(3) _cell_angle_alpha 90.00 _cell_angle_beta 96.27(3) _cell_angle_gamma 90.00 _cell_volume 7138(2) _cell_formula_units_Z 4 _cell_measurement_temperature 123(1) _cell_measurement_reflns_used 16384 _cell_measurement_theta_min 1.44 _cell_measurement_theta_max 27.5 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.179 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2712 _exptl_absorpt_coefficient_mu 1.545 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7475 _exptl_absorpt_correction_T_max 0.8863 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(1) _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 50398 _diffrn_reflns_av_R_equivalents 0.0935 _diffrn_reflns_av_sigmaI/netI 0.1117 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.44 _diffrn_reflns_theta_max 27.50 _reflns_number_total 16384 _reflns_number_gt 10598 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker Apex2 v2.0 (Bruker AXS, 2005)' _computing_cell_refinement 'Bruker Apex2 v2.0 (Bruker AXS, 2005)' _computing_data_reduction 'Bruker Apex2 v2.0 (Bruker AXS, 2005)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 2001)' _computing_publication_material 'CIFTAB (Sheldrick, 1997)' _refine_special_details ; Turt-butyl groups exhibit large ratios of ADP max/min for carbon atoms due to freely rotating primary carbons. 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^)+(0.2000P)^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 SHELXL _refine_ls_extinction_coef ? _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 16384 _refine_ls_number_parameters 734 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1090 _refine_ls_R_factor_gt 0.0560 _refine_ls_wR_factor_ref 0.1373 _refine_ls_wR_factor_gt 0.1197 _refine_ls_goodness_of_fit_ref 1.020 _refine_ls_restrained_S_all 1.020 _refine_ls_shift/su_max 0.001 _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 0.48051(2) 0.163170(13) 0.673024(17) 0.01498(9) Uani 1 1 d . . . Sr2 Sr 0.671536(19) 0.203068(13) 0.770272(17) 0.01412(9) Uani 1 1 d . . . C19 C 0.4386(2) 0.07119(14) 0.87806(18) 0.0183(8) Uani 1 1 d . . . H19 H 0.4399 0.0354 0.8662 0.022 Uiso 1 1 calc R . . C16 C 0.4389(2) 0.17759(14) 0.91292(18) 0.0149(7) Uani 1 1 d . . . C20 C 0.4860(2) 0.10508(14) 0.83936(18) 0.0173(8) Uani 1 1 d . . . H20 H 0.5188 0.0915 0.8012 0.021 Uiso 1 1 calc R . . C29 C 0.6760(2) 0.10486(14) 0.65256(18) 0.0147(7) Uani 1 1 d . . . C1 C 0.2963(2) 0.23806(15) 0.66059(18) 0.0188(8) Uani 1 1 d . . . C3 C 0.1615(2) 0.26694(16) 0.68837(19) 0.0225(9) Uani 1 1 d . . . H3 H 0.1066 0.2588 0.6977 0.027 Uiso 1 1 calc R . . C15 C 0.4883(2) 0.15863(14) 0.85352(18) 0.0153(7) Uani 1 1 d . . . C30 C 0.7008(2) 0.05271(14) 0.64903(18) 0.0152(7) Uani 1 1 d . . . C43 C 0.5585(2) 0.28499(14) 0.65512(19) 0.0183(8) Uani 1 1 d . . . C5 C 0.2632(2) 0.32958(15) 0.67173(19) 0.0235(9) Uani 1 1 d . . . H5 H 0.2811 0.3644 0.6703 0.028 Uiso 1 1 calc R . . C2 C 0.2140(2) 0.22590(15) 0.67724(18) 0.0193(8) Uani 1 1 d . . . C6 C 0.3177(2) 0.29022(15) 0.65861(19) 0.0227(9) Uani 1 1 d . . . H6 H 0.3719 0.2991 0.6478 0.027 Uiso 1 1 calc R . . C34 C 0.7094(2) 0.14024(14) 0.60240(19) 0.0180(8) Uani 1 1 d . . . H34 H 0.6923 0.1752 0.6034 0.022 Uiso 1 1 calc R . . C4 C 0.1829(2) 0.31913(15) 0.68691(19) 0.0223(8) Uani 1 1 d . . . C45 C 0.5365(2) 0.36954(15) 0.5958(2) 0.0260(9) Uani 1 1 d . . . H45 H 0.5321 0.3908 0.5500 0.031 Uiso 1 1 calc R . . C18 C 0.3890(2) 0.08885(13) 0.93430(18) 0.0150(7) Uani 1 1 d . . . C17 C 0.3919(2) 0.14152(14) 0.94927(18) 0.0164(8) Uani 1 1 d . . . H17 H 0.3589 0.1542 0.9878 0.020 Uiso 1 1 calc R . . C31 C 0.7588(2) 0.04018(14) 0.59704(19) 0.0187(8) Uani 1 1 d . . . H31 H 0.7764 0.0053 0.5955 0.022 Uiso 1 1 calc R . . C46 C 0.5273(2) 0.39332(15) 0.6687(2) 0.0287(9) Uani 1 1 d . . . C48 C 0.5468(2) 0.30905(14) 0.7268(2) 0.0216(8) Uani 1 1 d . . . H48 H 0.5495 0.2884 0.7732 0.026 Uiso 1 1 calc R . . C47 C 0.5317(2) 0.36103(16) 0.7336(2) 0.0281(9) Uani 1 1 d . . . H47 H 0.5241 0.3749 0.7840 0.034 Uiso 1 1 calc R . . C33 C 0.7662(2) 0.12627(15) 0.55158(19) 0.0200(8) Uani 1 1 d . . . H33 H 0.7876 0.1517 0.5192 0.024 Uiso 1 1 calc R . . C32 C 0.7924(2) 0.07542(15) 0.5473(2) 0.0210(8) Uani 1 1 d . . . C44 C 0.5516(2) 0.31712(15) 0.5857(2) 0.0198(8) Uani 1 1 d . . . O4 O 0.57691(14) 0.23491(9) 0.65421(12) 0.0175(5) Uani 1 1 d . . . O2 O 0.53385(14) 0.18874(9) 0.81212(12) 0.0156(5) Uani 1 1 d . . . O3 O 0.62201(14) 0.12215(9) 0.70097(12) 0.0164(5) Uani 1 1 d . . . O7 O 0.77807(16) 0.26788(10) 0.70862(14) 0.0262(6) Uani 1 1 d . . . O1 O 0.35118(15) 0.20237(10) 0.64707(14) 0.0227(6) Uani 1 1 d . . . O8 O 0.82813(15) 0.17290(10) 0.77143(14) 0.0249(6) Uani 1 1 d . . . C23 C 0.5231(2) 0.25601(15) 0.9565(2) 0.0233(9) Uani 1 1 d . . . H23A H 0.5476 0.2384 1.0045 0.035 Uiso 1 1 calc R . . H23B H 0.5200 0.2931 0.9668 0.035 Uiso 1 1 calc R . . H23C H 0.5574 0.2500 0.9135 0.035 Uiso 1 1 calc R . . C49 C 0.5621(2) 0.29496(15) 0.50349(19) 0.0226(8) Uani 1 1 d . . . C35 C 0.6648(2) 0.01102(14) 0.69952(19) 0.0192(8) Uani 1 1 d . . . C7 C 0.1864(2) 0.16993(14) 0.6844(2) 0.0210(8) Uani 1 1 d . . . C10 C 0.0957(2) 0.16531(16) 0.7013(2) 0.0328(10) Uani 1 1 d . . . H10A H 0.0886 0.1826 0.7514 0.049 Uiso 1 1 calc R . . H10B H 0.0810 0.1288 0.7050 0.049 Uiso 1 1 calc R . . H10C H 0.0599 0.1816 0.6582 0.049 Uiso 1 1 calc R . . C21 C 0.4359(2) 0.23479(14) 0.93278(19) 0.0174(8) Uani 1 1 d . . . C25 C 0.3340(2) 0.05142(14) 0.97450(19) 0.0203(8) Uani 1 1 d . . . C26 C 0.2947(2) 0.07678(15) 1.0431(2) 0.0296(10) Uani 1 1 d . . . H26A H 0.2599 0.1057 1.0227 0.044 Uiso 1 1 calc R . . H26B H 0.3382 0.0895 1.0827 0.044 Uiso 1 1 calc R . . H26C H 0.2609 0.0514 1.0675 0.044 Uiso 1 1 calc R . . C39 C 0.8561(2) 0.06053(16) 0.4909(2) 0.0272(9) Uani 1 1 d . . . C24 C 0.3863(2) 0.24584(15) 1.0026(2) 0.0250(9) Uani 1 1 d . . . H24A H 0.3283 0.2368 0.9878 0.038 Uiso 1 1 calc R . . H24B H 0.3905 0.2826 1.0161 0.038 Uiso 1 1 calc R . . H24C H 0.4084 0.2252 1.0485 0.038 Uiso 1 1 calc R . . C9 C 0.1932(2) 0.14034(15) 0.6072(2) 0.0270(9) Uani 1 1 d . . . H9A H 0.1547 0.1550 0.5648 0.040 Uiso 1 1 calc R . . H9B H 0.1797 0.1040 0.6146 0.040 Uiso 1 1 calc R . . H9C H 0.2497 0.1431 0.5929 0.040 Uiso 1 1 calc R . . C22 C 0.3939(2) 0.26429(14) 0.8599(2) 0.0232(8) Uani 1 1 d . . . H22A H 0.4251 0.2588 0.8145 0.035 Uiso 1 1 calc R . . H22B H 0.3925 0.3012 0.8720 0.035 Uiso 1 1 calc R . . H22C H 0.3374 0.2515 0.8472 0.035 Uiso 1 1 calc R . . C62 C 0.8620(2) 0.25794(18) 0.7352(2) 0.0336(11) Uani 1 1 d . . . H62A H 0.8736 0.2678 0.7917 0.040 Uiso 1 1 calc R . . H62B H 0.8979 0.2788 0.7042 0.040 Uiso 1 1 calc R . . C11 C 0.1200(3) 0.36095(17) 0.7025(2) 0.0321(10) Uani 1 1 d . . . C63 C 0.8800(2) 0.20202(17) 0.7256(2) 0.0334(10) Uani 1 1 d . . . H63A H 0.8695 0.1922 0.6691 0.040 Uiso 1 1 calc R . . H63B H 0.9387 0.1949 0.7439 0.040 Uiso 1 1 calc R . . C8 C 0.2395(3) 0.14362(16) 0.7538(2) 0.0316(10) Uani 1 1 d . . . H8A H 0.2977 0.1450 0.7445 0.047 Uiso 1 1 calc R . . H8B H 0.2223 0.1076 0.7578 0.047 Uiso 1 1 calc R . . H8C H 0.2321 0.1616 0.8033 0.047 Uiso 1 1 calc R . . C50 C 0.5051(3) 0.24794(17) 0.4855(2) 0.0346(10) Uani 1 1 d . . . H50A H 0.5006 0.2403 0.4287 0.052 Uiso 1 1 calc R . . H50B H 0.4503 0.2556 0.5011 0.052 Uiso 1 1 calc R . . H50C H 0.5283 0.2180 0.5154 0.052 Uiso 1 1 calc R . . C37 C 0.5717(2) 0.00655(15) 0.6757(2) 0.0265(9) Uani 1 1 d . . . H37A H 0.5453 0.0397 0.6842 0.040 Uiso 1 1 calc R . . H37B H 0.5488 -0.0200 0.7080 0.040 Uiso 1 1 calc R . . H37C H 0.5616 -0.0029 0.6196 0.040 Uiso 1 1 calc R . . C52 C 0.5396(3) 0.33499(18) 0.4373(2) 0.0419(12) Uani 1 1 d . . . H52A H 0.5781 0.3641 0.4441 0.063 Uiso 1 1 calc R . . H52B H 0.4833 0.3474 0.4402 0.063 Uiso 1 1 calc R . . H52C H 0.5432 0.3189 0.3856 0.063 Uiso 1 1 calc R . . C64 C 0.8522(2) 0.11988(16) 0.7777(2) 0.0350(10) Uani 1 1 d . . . H64A H 0.8457 0.1040 0.7251 0.053 Uiso 1 1 calc R . . H64B H 0.8175 0.1018 0.8124 0.053 Uiso 1 1 calc R . . H64C H 0.9101 0.1176 0.8001 0.053 Uiso 1 1 calc R . . C36 C 0.6807(2) 0.02463(16) 0.78809(19) 0.0276(9) Uani 1 1 d . . . H36A H 0.6595 0.0593 0.7968 0.041 Uiso 1 1 calc R . . H36B H 0.7402 0.0237 0.8048 0.041 Uiso 1 1 calc R . . H36C H 0.6527 -0.0004 0.8190 0.041 Uiso 1 1 calc R . . C27 C 0.3849(2) 0.00501(15) 1.0089(2) 0.0285(9) Uani 1 1 d . . . H27A H 0.3488 -0.0189 1.0336 0.043 Uiso 1 1 calc R . . H27B H 0.4286 0.0171 1.0487 0.043 Uiso 1 1 calc R . . H27C H 0.4095 -0.0127 0.9663 0.043 Uiso 1 1 calc R . . C40 C 0.8759(3) 0.00277(16) 0.4930(2) 0.0343(11) Uani 1 1 d . . . H40A H 0.8252 -0.0169 0.4784 0.051 Uiso 1 1 calc R . . H40B H 0.8994 -0.0070 0.5465 0.051 Uiso 1 1 calc R . . H40C H 0.9157 -0.0048 0.4553 0.051 Uiso 1 1 calc R . . C51 C 0.6515(2) 0.27838(16) 0.4999(2) 0.0301(10) Uani 1 1 d . . . H51A H 0.6685 0.2551 0.5442 0.045 Uiso 1 1 calc R . . H51B H 0.6872 0.3089 0.5034 0.045 Uiso 1 1 calc R . . H51C H 0.6562 0.2605 0.4497 0.045 Uiso 1 1 calc R . . C61 C 0.7653(3) 0.32110(17) 0.6899(3) 0.0389(11) Uani 1 1 d . . . H61A H 0.7888 0.3423 0.7346 0.058 Uiso 1 1 calc R . . H61B H 0.7061 0.3280 0.6794 0.058 Uiso 1 1 calc R . . H61C H 0.7923 0.3296 0.6428 0.058 Uiso 1 1 calc R . . C42 C 0.8220(3) 0.07531(19) 0.4058(2) 0.0465(13) Uani 1 1 d . . . H42A H 0.8615 0.0652 0.3692 0.070 Uiso 1 1 calc R . . H42B H 0.8131 0.1127 0.4027 0.070 Uiso 1 1 calc R . . H42C H 0.7695 0.0575 0.3915 0.070 Uiso 1 1 calc R . . C38 C 0.7025(3) -0.04256(15) 0.6893(2) 0.0297(10) Uani 1 1 d . . . H38A H 0.6769 -0.0676 0.7222 0.044 Uiso 1 1 calc R . . H38B H 0.7620 -0.0413 0.7055 0.044 Uiso 1 1 calc R . . H38C H 0.6927 -0.0530 0.6336 0.044 Uiso 1 1 calc R . . C28 C 0.2646(3) 0.03255(17) 0.9136(2) 0.0370(11) Uani 1 1 d . . . H28A H 0.2319 0.0065 0.9379 0.055 Uiso 1 1 calc R . . H28B H 0.2882 0.0174 0.8683 0.055 Uiso 1 1 calc R . . H28C H 0.2291 0.0617 0.8956 0.055 Uiso 1 1 calc R . . C41 C 0.9369(3) 0.09024(17) 0.5146(3) 0.0450(12) Uani 1 1 d . . . H41A H 0.9585 0.0810 0.5689 0.067 Uiso 1 1 calc R . . H41B H 0.9260 0.1274 0.5116 0.067 Uiso 1 1 calc R . . H41C H 0.9775 0.0812 0.4784 0.067 Uiso 1 1 calc R . . C53 C 0.5097(3) 0.45121(17) 0.6734(3) 0.0411(11) Uani 1 1 d . . . O10 O 0.72585(15) 0.16211(10) 0.90794(13) 0.0237(6) Uani 1 1 d . . . O9 O 0.72624(16) 0.26919(10) 0.88519(13) 0.0250(6) Uani 1 1 d . . . O6 O 0.48779(15) 0.12349(10) 0.52885(13) 0.0242(6) Uani 1 1 d . . . O5 O 0.38866(15) 0.07588(10) 0.62976(13) 0.0246(6) Uani 1 1 d . . . C60 C 0.5403(2) 0.09326(18) 0.4849(2) 0.0354(11) Uani 1 1 d . . . H60A H 0.5373 0.0570 0.5006 0.053 Uiso 1 1 calc R . . H60B H 0.5972 0.1055 0.4957 0.053 Uiso 1 1 calc R . . H60C H 0.5222 0.0965 0.4281 0.053 Uiso 1 1 calc R . . C59 C 0.4025(2) 0.11444(16) 0.5062(2) 0.0275(9) Uani 1 1 d . . . H59A H 0.3931 0.1097 0.4481 0.033 Uiso 1 1 calc R . . H59B H 0.3704 0.1449 0.5201 0.033 Uiso 1 1 calc R . . C57 C 0.3561(2) 0.03546(16) 0.6737(2) 0.0326(10) Uani 1 1 d . . . H57A H 0.2963 0.0331 0.6593 0.049 Uiso 1 1 calc R . . H57B H 0.3675 0.0427 0.7305 0.049 Uiso 1 1 calc R . . H57C H 0.3819 0.0027 0.6615 0.049 Uiso 1 1 calc R . . C58 C 0.3725(2) 0.06759(15) 0.5464(2) 0.0272(9) Uani 1 1 d . . . H58A H 0.3127 0.0627 0.5313 0.033 Uiso 1 1 calc R . . H58B H 0.4019 0.0364 0.5308 0.033 Uiso 1 1 calc R . . C13 C 0.0419(3) 0.3563(2) 0.6423(3) 0.0562(10) Uani 1 1 d . . . H13A H 0.0017 0.3826 0.6540 0.084 Uiso 1 1 calc R . . H13B H 0.0177 0.3220 0.6463 0.084 Uiso 1 1 calc R . . H13C H 0.0569 0.3616 0.5885 0.084 Uiso 1 1 calc R . . C12 C 0.1544(3) 0.41520(19) 0.6958(3) 0.0593(11) Uani 1 1 d . . . H12A H 0.2003 0.4204 0.7373 0.089 Uiso 1 1 calc R . . H12B H 0.1110 0.4405 0.7021 0.089 Uiso 1 1 calc R . . H12C H 0.1741 0.4196 0.6437 0.089 Uiso 1 1 calc R . . C14 C 0.0946(4) 0.3532(2) 0.7867(4) 0.0831(14) Uani 1 1 d . . . H14A H 0.1432 0.3564 0.8256 0.125 Uiso 1 1 calc R . . H14B H 0.0705 0.3188 0.7907 0.125 Uiso 1 1 calc R . . H14C H 0.0538 0.3794 0.7972 0.125 Uiso 1 1 calc R . . C66 C 0.7539(2) 0.24787(15) 0.96229(19) 0.0236(9) Uani 1 1 d . . . H66A H 0.7074 0.2458 0.9951 0.028 Uiso 1 1 calc R . . H66B H 0.7975 0.2699 0.9900 0.028 Uiso 1 1 calc R . . C68 C 0.6767(3) 0.13581(16) 0.9609(2) 0.0311(10) Uani 1 1 d . . . H68A H 0.7124 0.1140 0.9973 0.047 Uiso 1 1 calc R . . H68B H 0.6355 0.1143 0.9301 0.047 Uiso 1 1 calc R . . H68C H 0.6488 0.1612 0.9913 0.047 Uiso 1 1 calc R . . C67 C 0.7871(2) 0.19519(15) 0.9490(2) 0.0237(9) Uani 1 1 d . . . H67A H 0.8347 0.1981 0.9177 0.028 Uiso 1 1 calc R . . H67B H 0.8070 0.1795 1.0008 0.028 Uiso 1 1 calc R . . C65 C 0.7044(3) 0.32234(16) 0.8901(2) 0.0335(10) Uani 1 1 d . . . H65A H 0.6609 0.3261 0.9251 0.050 Uiso 1 1 calc R . . H65B H 0.6845 0.3351 0.8371 0.050 Uiso 1 1 calc R . . H65C H 0.7529 0.3423 0.9113 0.050 Uiso 1 1 calc R . . C54 C 0.5233(3) 0.47230(19) 0.7578(3) 0.0593(11) Uani 1 1 d . . . H54A H 0.5174 0.5099 0.7566 0.089 Uiso 1 1 calc R . . H54B H 0.5789 0.4632 0.7815 0.089 Uiso 1 1 calc R . . H54C H 0.4825 0.4573 0.7893 0.089 Uiso 1 1 calc R . . C55 C 0.5729(3) 0.48149(19) 0.6286(3) 0.0562(10) Uani 1 1 d . . . H55A H 0.5646 0.4728 0.5721 0.084 Uiso 1 1 calc R . . H55B H 0.6291 0.4720 0.6501 0.084 Uiso 1 1 calc R . . H55C H 0.5649 0.5186 0.6353 0.084 Uiso 1 1 calc R . . C56 C 0.4258(4) 0.4627(2) 0.6379(4) 0.0831(14) Uani 1 1 d . . . H56A H 0.4168 0.4473 0.5850 0.125 Uiso 1 1 calc R . . H56B H 0.4184 0.5002 0.6337 0.125 Uiso 1 1 calc R . . H56C H 0.3860 0.4484 0.6713 0.125 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 0.01177(16) 0.01627(19) 0.01648(15) -0.00140(13) -0.00039(12) 0.00022(14) Sr2 0.01218(16) 0.01588(19) 0.01414(15) -0.00031(13) 0.00078(12) -0.00199(15) C19 0.023(2) 0.0120(19) 0.0196(17) -0.0005(14) 0.0003(15) -0.0029(16) C16 0.0124(17) 0.019(2) 0.0133(15) 0.0005(14) 0.0004(14) -0.0007(15) C20 0.0184(19) 0.020(2) 0.0143(16) -0.0027(14) 0.0037(14) -0.0003(16) C29 0.0117(17) 0.016(2) 0.0155(16) -0.0034(14) -0.0023(14) -0.0006(15) C1 0.0137(18) 0.026(2) 0.0154(16) 0.0008(15) -0.0027(14) 0.0049(17) C3 0.0134(18) 0.036(3) 0.0185(17) 0.0007(16) 0.0015(15) 0.0003(18) C15 0.0087(17) 0.019(2) 0.0174(16) 0.0017(14) -0.0036(14) -0.0016(15) C30 0.0139(17) 0.015(2) 0.0153(16) -0.0015(14) -0.0039(14) 0.0002(15) C43 0.0133(18) 0.022(2) 0.0198(17) 0.0041(15) 0.0004(15) -0.0002(16) C5 0.028(2) 0.023(2) 0.0186(17) 0.0005(15) -0.0022(16) -0.0021(18) C2 0.0196(19) 0.027(2) 0.0112(15) -0.0019(15) -0.0005(14) 0.0036(17) C6 0.0164(19) 0.030(2) 0.0213(18) 0.0006(16) -0.0010(15) 0.0003(18) C34 0.0190(19) 0.0115(19) 0.0235(17) -0.0028(15) 0.0023(15) 0.0016(16) C4 0.023(2) 0.026(2) 0.0180(17) -0.0015(16) 0.0001(16) 0.0055(18) C45 0.019(2) 0.024(2) 0.034(2) 0.0133(17) 0.0016(17) -0.0023(18) C18 0.0125(17) 0.014(2) 0.0174(16) 0.0044(14) -0.0016(14) 0.0001(15) C17 0.0149(18) 0.018(2) 0.0158(16) -0.0014(14) 0.0017(14) 0.0017(16) C31 0.0159(18) 0.016(2) 0.0237(17) -0.0033(15) -0.0003(15) -0.0008(16) C46 0.023(2) 0.021(2) 0.043(2) 0.0040(19) 0.0071(19) -0.0001(18) C48 0.022(2) 0.020(2) 0.0227(18) 0.0030(15) 0.0057(16) 0.0012(17) C47 0.026(2) 0.028(2) 0.032(2) -0.0010(18) 0.0076(18) -0.0013(19) C33 0.0180(19) 0.021(2) 0.0208(17) -0.0007(15) 0.0023(15) -0.0044(17) C32 0.0147(18) 0.022(2) 0.0257(18) -0.0040(16) 0.0010(15) -0.0004(17) C44 0.0139(18) 0.021(2) 0.0239(18) 0.0054(15) 0.0002(15) -0.0034(17) O4 0.0165(13) 0.0145(14) 0.0213(12) 0.0057(10) 0.0011(10) 0.0030(11) O2 0.0135(12) 0.0170(14) 0.0169(11) 0.0004(10) 0.0044(10) -0.0028(11) O3 0.0147(12) 0.0145(14) 0.0203(11) -0.0029(10) 0.0034(10) 0.0013(11) O7 0.0220(14) 0.0283(17) 0.0281(13) 0.0038(12) 0.0017(12) -0.0100(13) O1 0.0159(13) 0.0232(15) 0.0290(13) 0.0016(11) 0.0030(11) 0.0056(12) O8 0.0181(14) 0.0294(17) 0.0272(13) -0.0042(12) 0.0025(11) 0.0021(12) C23 0.027(2) 0.018(2) 0.0256(18) -0.0062(16) 0.0047(17) -0.0050(18) C49 0.025(2) 0.024(2) 0.0191(17) 0.0073(16) 0.0002(16) 0.0011(18) C35 0.022(2) 0.016(2) 0.0199(17) 0.0006(15) 0.0015(15) 0.0018(16) C7 0.0173(19) 0.022(2) 0.0240(18) 0.0012(16) 0.0023(15) -0.0008(17) C10 0.024(2) 0.034(3) 0.042(2) 0.000(2) 0.0150(19) -0.002(2) C21 0.0150(18) 0.018(2) 0.0197(17) 0.0012(15) 0.0048(15) 0.0040(16) C25 0.0200(19) 0.018(2) 0.0222(17) 0.0045(15) 0.0006(16) -0.0006(17) C26 0.033(2) 0.019(2) 0.040(2) 0.0080(18) 0.0198(19) -0.0010(19) C39 0.022(2) 0.026(2) 0.037(2) -0.0078(18) 0.0171(18) -0.0041(18) C24 0.027(2) 0.018(2) 0.032(2) -0.0069(17) 0.0104(18) 0.0011(18) C9 0.027(2) 0.023(2) 0.032(2) -0.0033(17) 0.0070(18) -0.0032(19) C22 0.023(2) 0.019(2) 0.0269(19) 0.0023(16) -0.0005(16) 0.0039(17) C62 0.019(2) 0.050(3) 0.031(2) 0.004(2) 0.0007(18) -0.019(2) C11 0.037(3) 0.038(3) 0.0206(19) -0.0073(18) 0.0024(18) 0.013(2) C63 0.015(2) 0.053(3) 0.032(2) -0.001(2) 0.0076(17) -0.002(2) C8 0.034(2) 0.027(2) 0.033(2) 0.0114(18) 0.0028(19) -0.001(2) C50 0.035(2) 0.040(3) 0.025(2) 0.0011(19) -0.0089(18) -0.008(2) C37 0.027(2) 0.020(2) 0.033(2) 0.0009(17) 0.0009(18) -0.0036(18) C52 0.056(3) 0.047(3) 0.022(2) 0.0125(19) 0.000(2) 0.006(3) C64 0.023(2) 0.035(3) 0.046(2) -0.012(2) -0.0066(19) 0.009(2) C36 0.033(2) 0.029(2) 0.0214(18) 0.0037(16) 0.0032(17) 0.002(2) C27 0.034(2) 0.022(2) 0.031(2) 0.0087(17) 0.0110(19) 0.0030(19) C40 0.031(2) 0.027(3) 0.048(2) -0.015(2) 0.021(2) -0.002(2) C51 0.030(2) 0.032(3) 0.029(2) 0.0018(18) 0.0070(18) -0.004(2) C61 0.034(3) 0.035(3) 0.047(3) 0.008(2) 0.002(2) -0.012(2) C42 0.055(3) 0.053(3) 0.035(2) -0.003(2) 0.020(2) 0.007(3) C38 0.038(2) 0.018(2) 0.034(2) 0.0042(17) 0.0072(19) 0.0042(19) C28 0.035(2) 0.040(3) 0.036(2) 0.008(2) 0.000(2) -0.018(2) C41 0.029(2) 0.030(3) 0.080(3) -0.012(2) 0.025(3) -0.005(2) C53 0.034(3) 0.028(3) 0.061(3) 0.004(2) 0.003(2) 0.008(2) O10 0.0226(14) 0.0280(16) 0.0193(12) 0.0022(11) -0.0028(11) -0.0062(13) O9 0.0284(15) 0.0273(17) 0.0183(12) -0.0029(11) -0.0021(11) -0.0026(13) O6 0.0235(14) 0.0277(16) 0.0208(12) -0.0060(11) -0.0004(11) -0.0075(13) O5 0.0245(15) 0.0227(16) 0.0255(13) -0.0003(11) -0.0020(11) -0.0058(12) C60 0.028(2) 0.054(3) 0.024(2) -0.0125(19) 0.0023(18) -0.004(2) C59 0.024(2) 0.032(3) 0.0252(19) -0.0038(17) -0.0048(17) 0.0023(19) C57 0.025(2) 0.026(3) 0.046(2) 0.0016(19) 0.0010(19) -0.007(2) C58 0.020(2) 0.029(2) 0.031(2) -0.0151(18) -0.0037(17) -0.0022(19) C13 0.060(3) 0.040(2) 0.069(2) -0.0029(18) 0.013(2) 0.006(2) C12 0.075(3) 0.033(2) 0.070(2) -0.0131(18) 0.008(2) 0.011(2) C14 0.073(3) 0.052(3) 0.119(4) -0.011(3) -0.013(3) 0.033(2) C66 0.020(2) 0.034(3) 0.0147(17) -0.0027(16) -0.0040(15) -0.0061(19) C68 0.033(2) 0.030(3) 0.030(2) 0.0041(18) 0.0035(19) -0.009(2) C67 0.0181(19) 0.034(3) 0.0175(17) 0.0008(16) -0.0037(15) -0.0012(18) C65 0.040(3) 0.027(3) 0.031(2) -0.0016(18) -0.0057(19) -0.009(2) C54 0.075(3) 0.033(2) 0.070(2) -0.0131(18) 0.008(2) 0.011(2) C55 0.060(3) 0.040(2) 0.069(2) -0.0029(18) 0.013(2) 0.006(2) C56 0.073(3) 0.052(3) 0.119(4) -0.011(3) -0.013(3) 0.033(2) _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 2.340(2) . ? Sr1 O4 2.478(2) . ? Sr1 O2 2.515(2) . ? Sr1 O3 2.539(2) . ? Sr1 O6 2.670(2) . ? Sr1 O5 2.769(3) . ? Sr2 O2 2.457(2) . ? Sr2 O3 2.496(2) . ? Sr2 O4 2.507(2) . ? Sr2 O10 2.632(2) . ? Sr2 O8 2.669(3) . ? Sr2 O9 2.676(2) . ? Sr2 O7 2.709(2) . ? C19 C20 1.383(5) . ? C19 C18 1.396(4) . ? C19 H19 0.9500 . ? C16 C17 1.395(5) . ? C16 C15 1.444(4) . ? C16 C21 1.523(5) . ? C20 C15 1.409(5) . ? C20 H20 0.9500 . ? C29 O3 1.345(4) . ? C29 C34 1.402(5) . ? C29 C30 1.415(5) . ? C1 O1 1.325(4) . ? C1 C6 1.398(5) . ? C1 C2 1.436(5) . ? C3 C2 1.392(5) . ? C3 C4 1.398(5) . ? C3 H3 0.9500 . ? C15 O2 1.331(4) . ? C30 C31 1.400(4) . ? C30 C35 1.536(5) . ? C43 O4 1.333(4) . ? C43 C48 1.398(5) . ? C43 C44 1.438(5) . ? C5 C6 1.388(5) . ? C5 C4 1.389(5) . ? C5 H5 0.9500 . ? C2 C7 1.528(5) . ? C6 H6 0.9500 . ? C34 C33 1.382(5) . ? C34 H34 0.9500 . ? C4 C11 1.535(5) . ? C45 C44 1.395(5) . ? C45 C46 1.406(5) . ? C45 H45 0.9500 . ? C18 C17 1.389(5) . ? C18 C25 1.531(5) . ? C17 H17 0.9500 . ? C31 C32 1.397(5) . ? C31 H31 0.9500 . ? C46 C47 1.379(5) . ? C46 C53 1.532(6) . ? C48 C47 1.377(5) . ? C48 H48 0.9500 . ? C47 H47 0.9500 . ? C33 C32 1.390(5) . ? C33 H33 0.9500 . ? C32 C39 1.538(5) . ? C44 C49 1.536(5) . ? O7 C62 1.418(5) . ? O7 C61 1.426(5) . ? O8 C63 1.427(4) . ? O8 C64 1.430(5) . ? C23 C21 1.537(5) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C49 C51 1.528(5) . ? C49 C50 1.543(5) . ? C49 C52 1.544(5) . ? C35 C37 1.532(5) . ? C35 C38 1.537(5) . ? C35 C36 1.539(5) . ? C7 C9 1.533(5) . ? C7 C10 1.541(5) . ? C7 C8 1.544(5) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C21 C24 1.534(4) . ? C21 C22 1.550(5) . ? C25 C28 1.529(5) . ? C25 C26 1.537(5) . ? C25 C27 1.540(5) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C39 C40 1.531(5) . ? C39 C42 1.539(6) . ? C39 C41 1.541(6) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C62 C63 1.492(6) . ? C62 H62A 0.9900 . ? C62 H62B 0.9900 . ? C11 C12 1.523(6) . ? C11 C14 1.546(7) . ? C11 C13 1.548(6) . ? C63 H63A 0.9900 . ? C63 H63B 0.9900 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C64 H64A 0.9800 . ? C64 H64B 0.9800 . ? C64 H64C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C61 H61A 0.9800 . ? C61 H61B 0.9800 . ? C61 H61C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C53 C56 1.465(7) . ? C53 C54 1.527(6) . ? C53 C55 1.559(6) . ? O10 C67 1.438(4) . ? O10 C68 1.440(4) . ? O9 C65 1.428(5) . ? O9 C66 1.447(4) . ? O6 C59 1.422(4) . ? O6 C60 1.430(4) . ? O5 C57 1.423(4) . ? O5 C58 1.427(4) . ? C60 H60A 0.9800 . ? C60 H60B 0.9800 . ? C60 H60C 0.9800 . ? C59 C58 1.501(5) . ? C59 H59A 0.9900 . ? C59 H59B 0.9900 . ? C57 H57A 0.9800 . ? C57 H57B 0.9800 . ? C57 H57C 0.9800 . ? C58 H58A 0.9900 . ? C58 H58B 0.9900 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C66 C67 1.495(5) . ? C66 H66A 0.9900 . ? C66 H66B 0.9900 . ? C68 H68A 0.9800 . ? C68 H68B 0.9800 . ? C68 H68C 0.9800 . ? C67 H67A 0.9900 . ? C67 H67B 0.9900 . ? C65 H65A 0.9800 . ? C65 H65B 0.9800 . ? C65 H65C 0.9800 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 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 O4 102.80(8) . . ? O1 Sr1 O2 105.95(8) . . ? O4 Sr1 O2 76.35(7) . . ? O1 Sr1 O3 179.01(8) . . ? O4 Sr1 O3 76.21(8) . . ? O2 Sr1 O3 73.77(7) . . ? O1 Sr1 O6 97.12(8) . . ? O4 Sr1 O6 94.50(8) . . ? O2 Sr1 O6 156.51(8) . . ? O3 Sr1 O6 83.08(8) . . ? O1 Sr1 O5 81.62(8) . . ? O4 Sr1 O5 155.74(7) . . ? O2 Sr1 O5 125.90(7) . . ? O3 Sr1 O5 99.32(8) . . ? O6 Sr1 O5 61.23(7) . . ? O2 Sr2 O3 75.54(7) . . ? O2 Sr2 O4 76.90(7) . . ? O3 Sr2 O4 76.48(8) . . ? O2 Sr2 O10 84.94(8) . . ? O3 Sr2 O10 98.05(8) . . ? O4 Sr2 O10 161.80(7) . . ? O2 Sr2 O8 149.08(8) . . ? O3 Sr2 O8 91.00(8) . . ? O4 Sr2 O8 127.50(7) . . ? O10 Sr2 O8 69.28(8) . . ? O2 Sr2 O9 97.38(8) . . ? O3 Sr2 O9 161.27(7) . . ? O4 Sr2 O9 119.35(8) . . ? O10 Sr2 O9 63.74(8) . . ? O8 Sr2 O9 86.54(8) . . ? O2 Sr2 O7 148.31(8) . . ? O3 Sr2 O7 121.83(7) . . ? O4 Sr2 O7 81.83(8) . . ? O10 Sr2 O7 115.19(8) . . ? O8 Sr2 O7 62.02(8) . . ? O9 Sr2 O7 73.00(8) . . ? C20 C19 C18 120.9(3) . . ? C20 C19 H19 119.6 . . ? C18 C19 H19 119.6 . . ? C17 C16 C15 117.1(3) . . ? C17 C16 C21 121.5(3) . . ? C15 C16 C21 121.3(3) . . ? C19 C20 C15 123.4(3) . . ? C19 C20 H20 118.3 . . ? C15 C20 H20 118.3 . . ? O3 C29 C34 118.5(3) . . ? O3 C29 C30 123.7(3) . . ? C34 C29 C30 117.8(3) . . ? O1 C1 C6 119.7(3) . . ? O1 C1 C2 123.0(3) . . ? C6 C1 C2 117.3(3) . . ? C2 C3 C4 125.4(3) . . ? C2 C3 H3 117.3 . . ? C4 C3 H3 117.3 . . ? O2 C15 C20 119.6(3) . . ? O2 C15 C16 123.8(3) . . ? C20 C15 C16 116.6(3) . . ? C31 C30 C29 117.7(3) . . ? C31 C30 C35 121.0(3) . . ? C29 C30 C35 121.3(3) . . ? O4 C43 C48 119.8(3) . . ? O4 C43 C44 123.5(3) . . ? C48 C43 C44 116.7(3) . . ? C6 C5 C4 121.4(4) . . ? C6 C5 H5 119.3 . . ? C4 C5 H5 119.3 . . ? C3 C2 C1 117.5(3) . . ? C3 C2 C7 121.6(3) . . ? C1 C2 C7 121.0(3) . . ? C5 C6 C1 122.8(3) . . ? C5 C6 H6 118.6 . . ? C1 C6 H6 118.6 . . ? C33 C34 C29 122.7(3) . . ? C33 C34 H34 118.7 . . ? C29 C34 H34 118.7 . . ? C5 C4 C3 115.8(3) . . ? C5 C4 C11 123.7(4) . . ? C3 C4 C11 120.5(3) . . ? C44 C45 C46 125.0(3) . . ? C44 C45 H45 117.5 . . ? C46 C45 H45 117.5 . . ? C17 C18 C19 115.9(3) . . ? C17 C18 C25 123.5(3) . . ? C19 C18 C25 120.6(3) . . ? C18 C17 C16 126.0(3) . . ? C18 C17 H17 117.0 . . ? C16 C17 H17 117.0 . . ? C32 C31 C30 124.5(3) . . ? C32 C31 H31 117.8 . . ? C30 C31 H31 117.8 . . ? C47 C46 C45 115.8(4) . . ? C47 C46 C53 123.2(4) . . ? C45 C46 C53 120.9(4) . . ? C47 C48 C43 123.5(3) . . ? C47 C48 H48 118.2 . . ? C43 C48 H48 118.2 . . ? C48 C47 C46 121.4(4) . . ? C48 C47 H47 119.3 . . ? C46 C47 H47 119.3 . . ? C34 C33 C32 120.8(3) . . ? C34 C33 H33 119.6 . . ? C32 C33 H33 119.6 . . ? C33 C32 C31 116.4(3) . . ? C33 C32 C39 120.2(3) . . ? C31 C32 C39 123.3(3) . . ? C45 C44 C43 117.5(3) . . ? C45 C44 C49 121.0(3) . . ? C43 C44 C49 121.5(3) . . ? C43 O4 Sr1 125.6(2) . . ? C43 O4 Sr2 115.6(2) . . ? Sr1 O4 Sr2 89.80(7) . . ? C15 O2 Sr2 145.4(2) . . ? C15 O2 Sr1 100.70(18) . . ? Sr2 O2 Sr1 90.09(7) . . ? C29 O3 Sr2 111.63(19) . . ? C29 O3 Sr1 131.87(19) . . ? Sr2 O3 Sr1 88.69(7) . . ? C62 O7 C61 111.1(3) . . ? C62 O7 Sr2 113.7(2) . . ? C61 O7 Sr2 127.0(2) . . ? C1 O1 Sr1 152.0(2) . . ? C63 O8 C64 112.0(3) . . ? C63 O8 Sr2 117.7(2) . . ? C64 O8 Sr2 122.5(2) . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C51 C49 C44 110.1(3) . . ? C51 C49 C50 109.1(3) . . ? C44 C49 C50 110.5(3) . . ? C51 C49 C52 108.2(3) . . ? C44 C49 C52 111.6(3) . . ? C50 C49 C52 107.3(3) . . ? C37 C35 C30 109.5(3) . . ? C37 C35 C38 107.4(3) . . ? C30 C35 C38 113.0(3) . . ? C37 C35 C36 109.4(3) . . ? C30 C35 C36 110.5(3) . . ? C38 C35 C36 106.9(3) . . ? C2 C7 C9 110.9(3) . . ? C2 C7 C10 112.7(3) . . ? C9 C7 C10 106.4(3) . . ? C2 C7 C8 109.5(3) . . ? C9 C7 C8 110.2(3) . . ? C10 C7 C8 107.0(3) . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C16 C21 C24 112.6(3) . . ? C16 C21 C23 110.9(3) . . ? C24 C21 C23 106.3(3) . . ? C16 C21 C22 109.0(3) . . ? C24 C21 C22 107.5(3) . . ? C23 C21 C22 110.5(3) . . ? C28 C25 C18 109.1(3) . . ? C28 C25 C26 108.0(3) . . ? C18 C25 C26 112.3(3) . . ? C28 C25 C27 109.6(3) . . ? C18 C25 C27 110.3(3) . . ? C26 C25 C27 107.4(3) . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C40 C39 C32 112.7(3) . . ? C40 C39 C42 108.6(3) . . ? C32 C39 C42 108.8(3) . . ? C40 C39 C41 108.1(3) . . ? C32 C39 C41 109.2(3) . . ? C42 C39 C41 109.4(3) . . ? C21 C24 H24A 109.5 . . ? C21 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C21 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? O7 C62 C63 109.7(3) . . ? O7 C62 H62A 109.7 . . ? C63 C62 H62A 109.7 . . ? O7 C62 H62B 109.7 . . ? C63 C62 H62B 109.7 . . ? H62A C62 H62B 108.2 . . ? C12 C11 C4 112.4(4) . . ? C12 C11 C14 109.1(4) . . ? C4 C11 C14 108.6(4) . . ? C12 C11 C13 107.8(4) . . ? C4 C11 C13 110.4(3) . . ? C14 C11 C13 108.4(4) . . ? O8 C63 C62 108.6(3) . . ? O8 C63 H63A 110.0 . . ? C62 C63 H63A 110.0 . . ? O8 C63 H63B 110.0 . . ? C62 C63 H63B 110.0 . . ? H63A C63 H63B 108.4 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C49 C50 H50A 109.5 . . ? C49 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C49 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C35 C37 H37A 109.5 . . ? C35 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C35 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C49 C52 H52A 109.5 . . ? C49 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C49 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? O8 C64 H64A 109.5 . . ? O8 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? O8 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C39 C40 H40A 109.5 . . ? C39 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C39 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C49 C51 H51A 109.5 . . ? C49 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C49 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? O7 C61 H61A 109.5 . . ? O7 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? O7 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? C39 C42 H42A 109.5 . . ? C39 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C39 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C35 C38 H38A 109.5 . . ? C35 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C35 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C25 C28 H28A 109.5 . . ? C25 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C25 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C39 C41 H41A 109.5 . . ? C39 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C39 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C56 C53 C54 110.3(4) . . ? C56 C53 C46 110.5(4) . . ? C54 C53 C46 113.0(4) . . ? C56 C53 C55 109.6(4) . . ? C54 C53 C55 104.0(4) . . ? C46 C53 C55 109.3(4) . . ? C67 O10 C68 112.6(3) . . ? C67 O10 Sr2 109.8(2) . . ? C68 O10 Sr2 126.1(2) . . ? C65 O9 C66 111.8(3) . . ? C65 O9 Sr2 126.5(2) . . ? C66 O9 Sr2 117.5(2) . . ? C59 O6 C60 113.1(3) . . ? C59 O6 Sr1 99.87(19) . . ? C60 O6 Sr1 141.2(2) . . ? C57 O5 C58 111.7(3) . . ? C57 O5 Sr1 133.3(2) . . ? C58 O5 Sr1 115.0(2) . . ? O6 C60 H60A 109.5 . . ? O6 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? O6 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? O6 C59 C58 111.6(3) . . ? O6 C59 H59A 109.3 . . ? C58 C59 H59A 109.3 . . ? O6 C59 H59B 109.3 . . ? C58 C59 H59B 109.3 . . ? H59A C59 H59B 108.0 . . ? O5 C57 H57A 109.5 . . ? O5 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? O5 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? O5 C58 C59 107.2(3) . . ? O5 C58 H58A 110.3 . . ? C59 C58 H58A 110.3 . . ? O5 C58 H58B 110.3 . . ? C59 C58 H58B 110.3 . . ? H58A C58 H58B 108.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C14 H14A 109.5 . . ? C11 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C11 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? O9 C66 C67 107.1(3) . . ? O9 C66 H66A 110.3 . . ? C67 C66 H66A 110.3 . . ? O9 C66 H66B 110.3 . . ? C67 C66 H66B 110.3 . . ? H66A C66 H66B 108.5 . . ? O10 C68 H68A 109.5 . . ? O10 C68 H68B 109.5 . . ? H68A C68 H68B 109.5 . . ? O10 C68 H68C 109.5 . . ? H68A C68 H68C 109.5 . . ? H68B C68 H68C 109.5 . . ? O10 C67 C66 112.0(3) . . ? O10 C67 H67A 109.2 . . ? C66 C67 H67A 109.2 . . ? O10 C67 H67B 109.2 . . ? C66 C67 H67B 109.2 . . ? H67A C67 H67B 107.9 . . ? O9 C65 H65A 109.5 . . ? O9 C65 H65B 109.5 . . ? H65A C65 H65B 109.5 . . ? O9 C65 H65C 109.5 . . ? H65A C65 H65C 109.5 . . ? H65B C65 H65C 109.5 . . ? C53 C54 H54A 109.5 . . ? C53 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C53 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C53 C55 H55A 109.5 . . ? C53 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? C53 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? C53 C56 H56A 109.5 . . ? C53 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C53 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.251 _refine_diff_density_min -0.931 _refine_diff_density_rms 0.096