# 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_mx54_11 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H33 O4 Sb' _chemical_formula_sum 'C36 H33 O4 Sb' _chemical_formula_weight 651.37 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' Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.4324(7) _cell_length_b 11.6012(7) _cell_length_c 13.6076(8) _cell_angle_alpha 68.481(2) _cell_angle_beta 72.324(3) _cell_angle_gamma 82.668(3) _cell_volume 1459.53(16) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 9902 _cell_measurement_theta_min 2.54 _cell_measurement_theta_max 29.87 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.482 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 664 _exptl_absorpt_coefficient_mu 0.985 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.857 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker X8 APEXII CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26389 _diffrn_reflns_av_R_equivalents 0.0240 _diffrn_reflns_av_sigmaI/netI 0.0266 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.22 _diffrn_reflns_theta_max 29.90 _reflns_number_total 8253 _reflns_number_gt 7682 _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 ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0167P)^2^+0.7779P] 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 8252 _refine_ls_number_parameters 372 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0236 _refine_ls_R_factor_gt 0.0208 _refine_ls_wR_factor_ref 0.0486 _refine_ls_wR_factor_gt 0.0473 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.054 _refine_ls_shift/su_max 0.003 _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 Sb1 Sb 0.816555(8) 0.805395(8) 0.726818(7) 0.01202(3) Uani 1 1 d . . . O1 O 0.82291(10) 0.88475(9) 0.56070(8) 0.01534(19) Uani 1 1 d . . . O2 O 0.60185(10) 0.91971(10) 0.61214(8) 0.0199(2) Uani 1 1 d . . . O3 O 0.82913(10) 0.71863(9) 0.88982(8) 0.0174(2) Uani 1 1 d . . . O4 O 0.62639(11) 0.76312(10) 0.98761(9) 0.0237(2) Uani 1 1 d . . . C1 C 0.76380(14) 0.97008(13) 0.76066(11) 0.0158(3) Uani 1 1 d . . . C2 C 0.63044(15) 1.00790(15) 0.79243(12) 0.0217(3) Uani 1 1 d . . . H2 H 0.5602 0.9646 0.7907 0.026 Uiso 1 1 calc R . . C3 C 0.60089(18) 1.10946(16) 0.82662(14) 0.0284(3) Uani 1 1 d . . . H3 H 0.5100 1.1355 0.8493 0.034 Uiso 1 1 calc R . . C4 C 0.70376(19) 1.17281(15) 0.82764(14) 0.0297(4) Uani 1 1 d . . . H4 H 0.6831 1.2425 0.8509 0.036 Uiso 1 1 calc R . . C5 C 0.83597(19) 1.13587(15) 0.79526(14) 0.0286(3) Uani 1 1 d . . . H5 H 0.9060 1.1804 0.7957 0.034 Uiso 1 1 calc R . . C6 C 0.86667(16) 1.03344(14) 0.76189(12) 0.0218(3) Uani 1 1 d . . . H6 H 0.9576 1.0071 0.7401 0.026 Uiso 1 1 calc R . . C7 C 1.02565(13) 0.77257(12) 0.67450(11) 0.0135(2) Uani 1 1 d . . . C8 C 1.09964(14) 0.72498(13) 0.75156(11) 0.0173(3) Uani 1 1 d . . . H8 H 1.0562 0.7085 0.8275 0.021 Uiso 1 1 calc R . . C9 C 1.23664(15) 0.70193(14) 0.71660(12) 0.0206(3) Uani 1 1 d . . . H9 H 1.2869 0.6701 0.7690 0.025 Uiso 1 1 calc R . . C10 C 1.30119(14) 0.72480(14) 0.60607(12) 0.0208(3) Uani 1 1 d . . . H10 H 1.3949 0.7078 0.5829 0.025 Uiso 1 1 calc R . . C11 C 1.22829(15) 0.77256(14) 0.52972(12) 0.0210(3) Uani 1 1 d . . . H11 H 1.2724 0.7889 0.4539 0.025 Uiso 1 1 calc R . . C12 C 1.09107(14) 0.79674(13) 0.56319(11) 0.0176(3) Uani 1 1 d . . . H12 H 1.0417 0.8298 0.5103 0.021 Uiso 1 1 calc R . . C13 C 0.69518(13) 0.66277(12) 0.74740(11) 0.0146(2) Uani 1 1 d . . . C14 C 0.58441(14) 0.62298(14) 0.83828(12) 0.0184(3) Uani 1 1 d . . . H14 H 0.5604 0.6613 0.8924 0.022 Uiso 1 1 calc R . . C15 C 0.50923(15) 0.52654(14) 0.84892(12) 0.0208(3) Uani 1 1 d . . . H15 H 0.4333 0.4985 0.9108 0.025 Uiso 1 1 calc R . . C16 C 0.54391(16) 0.47094(14) 0.77023(13) 0.0218(3) Uani 1 1 d . . . H16 H 0.4921 0.4047 0.7783 0.026 Uiso 1 1 calc R . . C17 C 0.65442(17) 0.51165(15) 0.67930(13) 0.0254(3) Uani 1 1 d . . . H17 H 0.6779 0.4735 0.6251 0.031 Uiso 1 1 calc R . . C18 C 0.73042(16) 0.60786(14) 0.66758(12) 0.0208(3) Uani 1 1 d . . . H18 H 0.8061 0.6360 0.6054 0.025 Uiso 1 1 calc R . . C19 C 0.70584(14) 0.92056(12) 0.54019(11) 0.0145(2) Uani 1 1 d . . . C20 C 0.71226(14) 0.95679(13) 0.41993(11) 0.0165(3) Uani 1 1 d . . . H20A H 0.6345 1.0114 0.4041 0.020 Uiso 1 1 calc R . . H20B H 0.7958 1.0026 0.3732 0.020 Uiso 1 1 calc R . . C21 C 0.70985(14) 0.84023(13) 0.39499(11) 0.0159(3) Uani 1 1 d . . . C22 C 0.59137(15) 0.80754(14) 0.38653(12) 0.0206(3) Uani 1 1 d . . . H22 H 0.5146 0.8611 0.3907 0.025 Uiso 1 1 calc R . . C23 C 0.58548(18) 0.69655(16) 0.37194(13) 0.0267(3) Uani 1 1 d . . . H23 H 0.5041 0.6740 0.3665 0.032 Uiso 1 1 calc R . . C24 C 0.69659(19) 0.61828(15) 0.36519(12) 0.0274(3) Uani 1 1 d . . . H24 H 0.6905 0.5418 0.3564 0.033 Uiso 1 1 calc R . . C25 C 0.81744(17) 0.65007(14) 0.37114(12) 0.0237(3) Uani 1 1 d . . . C26 C 0.82194(15) 0.76177(14) 0.38600(11) 0.0194(3) Uani 1 1 d . . . H26 H 0.9037 0.7850 0.3901 0.023 Uiso 1 1 calc R . . C27 C 0.9390(2) 0.56579(17) 0.36358(15) 0.0359(4) Uani 1 1 d . . . H27A H 0.9821 0.5749 0.2864 0.054 Uiso 1 1 calc R . . H27B H 0.9115 0.4797 0.4056 0.054 Uiso 1 1 calc R . . H27C H 1.0026 0.5877 0.3938 0.054 Uiso 1 1 calc R . . C28 C 0.74423(15) 0.73338(13) 0.97798(11) 0.0181(3) Uani 1 1 d . . . C29 C 0.80417(17) 0.70504(18) 1.07367(12) 0.0284(4) Uani 1 1 d . . . H29A H 0.7649 0.7644 1.1123 0.034 Uiso 1 1 calc R . . H29B H 0.7766 0.6210 1.1262 0.034 Uiso 1 1 calc R . . C30 C 0.95491(16) 0.71094(15) 1.04321(11) 0.0218(3) Uani 1 1 d . . . C31 C 1.03296(19) 0.60412(16) 1.06804(13) 0.0291(4) Uani 1 1 d . . . H31 H 0.9909 0.5259 1.1061 0.035 Uiso 1 1 calc R . . C32 C 1.1715(2) 0.61038(17) 1.03792(14) 0.0326(4) Uani 1 1 d . . . H32 H 1.2241 0.5367 1.0565 0.039 Uiso 1 1 calc R . . C33 C 1.23355(17) 0.72281(17) 0.98117(13) 0.0282(3) Uani 1 1 d . . . H33 H 1.3289 0.7261 0.9604 0.034 Uiso 1 1 calc R . . C34 C 1.15838(15) 0.83169(15) 0.95384(12) 0.0216(3) Uani 1 1 d . . . C35 C 1.01923(15) 0.82419(14) 0.98633(11) 0.0200(3) Uani 1 1 d . . . H35 H 0.9665 0.8981 0.9694 0.024 Uiso 1 1 calc R . . C36 C 1.22722(19) 0.95395(18) 0.89063(15) 0.0345(4) Uani 1 1 d . . . H36A H 1.1613 1.0182 0.8670 0.052 Uiso 1 1 calc R . . H36B H 1.2977 0.9478 0.8259 0.052 Uiso 1 1 calc R . . H36C H 1.2676 0.9756 0.9377 0.052 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 Sb1 0.01087(4) 0.01230(5) 0.01332(4) -0.00529(3) -0.00288(3) -0.00033(3) O1 0.0143(4) 0.0160(5) 0.0159(4) -0.0046(4) -0.0061(4) 0.0007(4) O2 0.0168(5) 0.0229(5) 0.0209(5) -0.0098(4) -0.0050(4) 0.0025(4) O3 0.0185(5) 0.0194(5) 0.0137(4) -0.0059(4) -0.0033(4) -0.0010(4) O4 0.0204(5) 0.0281(6) 0.0227(5) -0.0118(4) -0.0015(4) -0.0027(4) C1 0.0188(6) 0.0140(6) 0.0158(6) -0.0066(5) -0.0054(5) 0.0014(5) C2 0.0188(7) 0.0249(8) 0.0255(7) -0.0138(6) -0.0077(6) 0.0043(6) C3 0.0308(8) 0.0312(9) 0.0300(8) -0.0188(7) -0.0139(7) 0.0142(7) C4 0.0478(11) 0.0204(8) 0.0305(8) -0.0158(7) -0.0203(8) 0.0113(7) C5 0.0382(9) 0.0207(8) 0.0347(9) -0.0130(7) -0.0158(7) -0.0027(7) C6 0.0226(7) 0.0200(7) 0.0253(7) -0.0100(6) -0.0070(6) -0.0016(6) C7 0.0120(6) 0.0117(6) 0.0168(6) -0.0052(5) -0.0036(5) -0.0004(5) C8 0.0160(6) 0.0192(7) 0.0167(6) -0.0063(5) -0.0052(5) 0.0010(5) C9 0.0170(7) 0.0225(7) 0.0225(7) -0.0067(6) -0.0083(5) 0.0026(6) C10 0.0133(6) 0.0210(7) 0.0254(7) -0.0074(6) -0.0029(5) 0.0010(5) C11 0.0158(6) 0.0250(8) 0.0187(6) -0.0072(6) -0.0007(5) 0.0001(6) C12 0.0154(6) 0.0204(7) 0.0162(6) -0.0051(5) -0.0047(5) -0.0001(5) C13 0.0145(6) 0.0133(6) 0.0163(6) -0.0042(5) -0.0062(5) 0.0006(5) C14 0.0153(6) 0.0217(7) 0.0194(6) -0.0094(5) -0.0037(5) -0.0012(5) C15 0.0163(6) 0.0224(7) 0.0228(7) -0.0068(6) -0.0036(5) -0.0052(6) C16 0.0222(7) 0.0175(7) 0.0276(7) -0.0071(6) -0.0094(6) -0.0037(6) C17 0.0321(8) 0.0218(8) 0.0253(7) -0.0129(6) -0.0041(6) -0.0052(6) C18 0.0241(7) 0.0185(7) 0.0181(6) -0.0076(5) 0.0000(5) -0.0049(6) C19 0.0162(6) 0.0106(6) 0.0192(6) -0.0061(5) -0.0077(5) 0.0009(5) C20 0.0186(6) 0.0143(6) 0.0176(6) -0.0049(5) -0.0075(5) 0.0003(5) C21 0.0194(6) 0.0154(6) 0.0122(6) -0.0039(5) -0.0047(5) -0.0006(5) C22 0.0203(7) 0.0251(8) 0.0185(6) -0.0094(6) -0.0051(5) -0.0019(6) C23 0.0295(8) 0.0307(9) 0.0255(7) -0.0143(7) -0.0067(6) -0.0079(7) C24 0.0443(10) 0.0209(8) 0.0204(7) -0.0108(6) -0.0077(7) -0.0047(7) C25 0.0346(9) 0.0211(7) 0.0151(6) -0.0073(6) -0.0075(6) 0.0057(6) C26 0.0218(7) 0.0199(7) 0.0171(6) -0.0064(5) -0.0069(5) 0.0016(6) C27 0.0499(11) 0.0301(9) 0.0316(9) -0.0170(7) -0.0165(8) 0.0180(8) C28 0.0213(7) 0.0170(7) 0.0150(6) -0.0052(5) -0.0011(5) -0.0082(5) C29 0.0255(8) 0.0443(10) 0.0151(6) -0.0091(7) -0.0023(6) -0.0119(7) C30 0.0254(7) 0.0299(8) 0.0125(6) -0.0077(6) -0.0063(5) -0.0048(6) C31 0.0447(10) 0.0236(8) 0.0204(7) -0.0053(6) -0.0122(7) -0.0046(7) C32 0.0432(10) 0.0298(9) 0.0298(8) -0.0131(7) -0.0196(8) 0.0135(8) C33 0.0230(8) 0.0414(10) 0.0269(8) -0.0180(7) -0.0117(6) 0.0068(7) C34 0.0212(7) 0.0281(8) 0.0180(6) -0.0101(6) -0.0060(5) -0.0012(6) C35 0.0212(7) 0.0230(7) 0.0166(6) -0.0070(5) -0.0072(5) 0.0016(6) C36 0.0298(9) 0.0380(10) 0.0323(9) -0.0080(8) -0.0046(7) -0.0114(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sb1 O1 2.0880(9) . ? Sb1 C1 2.0949(14) . ? Sb1 C13 2.0974(14) . ? Sb1 C7 2.1105(13) . ? Sb1 O3 2.1108(10) . ? O1 C19 1.3170(16) . ? O2 C19 1.2191(17) . ? O3 C28 1.3113(16) . ? O4 C28 1.2143(18) . ? C1 C6 1.383(2) . ? C1 C2 1.390(2) . ? C2 C3 1.386(2) . ? C3 C4 1.382(3) . ? C4 C5 1.378(3) . ? C5 C6 1.390(2) . ? C7 C12 1.3958(18) . ? C7 C8 1.3993(19) . ? C8 C9 1.387(2) . ? C9 C10 1.387(2) . ? C10 C11 1.384(2) . ? C11 C12 1.3895(19) . ? C13 C18 1.3878(19) . ? C13 C14 1.3882(19) . ? C14 C15 1.387(2) . ? C15 C16 1.380(2) . ? C16 C17 1.388(2) . ? C17 C18 1.385(2) . ? C19 C20 1.5150(19) . ? C20 C21 1.5148(19) . ? C21 C22 1.387(2) . ? C21 C26 1.391(2) . ? C22 C23 1.384(2) . ? C23 C24 1.380(2) . ? C24 C25 1.391(2) . ? C25 C26 1.391(2) . ? C25 C27 1.501(2) . ? C28 C29 1.524(2) . ? C29 C30 1.503(2) . ? C30 C31 1.384(2) . ? C30 C35 1.392(2) . ? C31 C32 1.381(3) . ? C32 C33 1.375(3) . ? C33 C34 1.389(2) . ? C34 C35 1.387(2) . ? C34 C36 1.502(2) . ? 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 Sb1 C1 95.36(5) . . ? O1 Sb1 C13 90.81(4) . . ? C1 Sb1 C13 130.18(5) . . ? O1 Sb1 C7 87.14(4) . . ? C1 Sb1 C7 114.55(5) . . ? C13 Sb1 C7 115.11(5) . . ? O1 Sb1 O3 174.48(4) . . ? C1 Sb1 O3 87.92(5) . . ? C13 Sb1 O3 90.46(5) . . ? C7 Sb1 O3 87.46(5) . . ? C19 O1 Sb1 115.56(8) . . ? C28 O3 Sb1 126.25(9) . . ? C6 C1 C2 120.66(13) . . ? C6 C1 Sb1 116.98(11) . . ? C2 C1 Sb1 122.00(11) . . ? C3 C2 C1 119.37(15) . . ? C4 C3 C2 119.92(15) . . ? C5 C4 C3 120.67(15) . . ? C4 C5 C6 119.90(16) . . ? C1 C6 C5 119.48(15) . . ? C12 C7 C8 119.44(12) . . ? C12 C7 Sb1 120.45(10) . . ? C8 C7 Sb1 120.11(10) . . ? C9 C8 C7 119.72(13) . . ? C8 C9 C10 120.75(13) . . ? C11 C10 C9 119.58(13) . . ? C10 C11 C12 120.46(13) . . ? C11 C12 C7 120.05(13) . . ? C18 C13 C14 120.84(13) . . ? C18 C13 Sb1 117.68(10) . . ? C14 C13 Sb1 121.48(10) . . ? C15 C14 C13 119.07(13) . . ? C16 C15 C14 120.50(13) . . ? C15 C16 C17 120.09(14) . . ? C18 C17 C16 120.04(14) . . ? C17 C18 C13 119.45(13) . . ? O2 C19 O1 122.84(12) . . ? O2 C19 C20 123.58(13) . . ? O1 C19 C20 113.52(12) . . ? C21 C20 C19 108.74(11) . . ? C22 C21 C26 119.12(14) . . ? C22 C21 C20 119.36(13) . . ? C26 C21 C20 121.43(13) . . ? C23 C22 C21 119.73(15) . . ? C24 C23 C22 120.66(15) . . ? C23 C24 C25 120.75(15) . . ? C24 C25 C26 118.00(15) . . ? C24 C25 C27 121.18(15) . . ? C26 C25 C27 120.81(16) . . ? C21 C26 C25 121.71(15) . . ? O4 C28 O3 125.13(13) . . ? O4 C28 C29 120.69(13) . . ? O3 C28 C29 114.15(13) . . ? C30 C29 C28 115.50(12) . . ? C31 C30 C35 118.54(15) . . ? C31 C30 C29 120.94(15) . . ? C35 C30 C29 120.49(15) . . ? C32 C31 C30 120.48(16) . . ? C33 C32 C31 120.28(16) . . ? C32 C33 C34 120.75(16) . . ? C35 C34 C33 118.32(15) . . ? C35 C34 C36 121.34(15) . . ? C33 C34 C36 120.34(15) . . ? C34 C35 C30 121.61(15) . . ? _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.471 _refine_diff_density_min -0.375 _refine_diff_density_rms 0.067 _database_code_depnum_ccdc_archive 'CCDC 857411' ####################################################################### # # 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_mx103_11 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C41 H43 O10 Sb, 0.5(C7 H8)' _chemical_formula_sum 'C44.50 H47 O10 Sb' _chemical_formula_weight 863.57 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' Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.1207(3) _cell_length_b 12.3148(4) _cell_length_c 18.1230(6) _cell_angle_alpha 73.546(3) _cell_angle_beta 76.307(3) _cell_angle_gamma 78.578(2) _cell_volume 2083.78(11) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 9799 _cell_measurement_theta_min 2.0877 _cell_measurement_theta_max 32.3588 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.376 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 890 _exptl_absorpt_coefficient_mu 0.719 _exptl_absorpt_correction_T_min 0.92482 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET) (compiled Aug 3 2011,13:03:54) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Ruby, Gemini ultra' _diffrn_detector_area_resol_mean 10.3389 _diffrn_measurement_method '\w scans' _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24078 _diffrn_reflns_av_R_equivalents 0.0226 _diffrn_reflns_av_sigmaI/netI 0.0457 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.09 _diffrn_reflns_theta_max 32.43 _reflns_number_total 13317 _reflns_number_gt 11375 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET) (compiled Aug 3 2011,13:03:54) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET) (compiled Aug 3 2011,13:03:54) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET) (compiled Aug 3 2011,13:03:54) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics X-SEED _computing_publication_material CIFTAB _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The lattice solvent was modelled as a four-fold disordered PhMe molecule with two overlapping unique components, the remaining two components generated by a crystallographic inversion centre. The PhMe molecules were refined with restrained geomtery and isotropic thermal parameter forms. ; _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^)+(0.0249P)^2^+0.8502P] 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 13317 _refine_ls_number_parameters 535 _refine_ls_number_restraints 36 _refine_ls_R_factor_all 0.0445 _refine_ls_R_factor_gt 0.0315 _refine_ls_wR_factor_ref 0.0723 _refine_ls_wR_factor_gt 0.0651 _refine_ls_goodness_of_fit_ref 1.068 _refine_ls_restrained_S_all 1.074 _refine_ls_shift/su_max 0.002 _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 Sb1 Sb 0.643050(11) 0.697206(9) 0.642262(7) 0.01372(3) Uani 1 1 d . . . O1 O 0.53020(12) 0.61175(10) 0.75218(7) 0.0161(2) Uani 1 1 d . . . O2 O 0.63900(13) 0.45431(11) 0.71544(7) 0.0189(3) Uani 1 1 d . . . O3 O 0.75372(12) 0.79822(11) 0.54032(7) 0.0182(3) Uani 1 1 d . . . O4 O 0.81285(14) 0.65301(11) 0.48221(8) 0.0230(3) Uani 1 1 d . . . O5 O 0.28675(15) 0.45525(12) 1.03522(8) 0.0287(3) Uani 1 1 d . . . O6 O 0.35537(15) 0.22991(12) 1.06238(8) 0.0293(3) Uani 1 1 d . . . O7 O 0.52276(14) 0.12964(11) 0.95588(8) 0.0254(3) Uani 1 1 d . . . O8 O 0.99611(14) 1.11898(11) 0.34887(9) 0.0253(3) Uani 1 1 d . . . O9 O 1.12922(13) 1.03502(11) 0.22713(8) 0.0231(3) Uani 1 1 d . . . O10 O 1.10278(14) 0.82888(11) 0.21757(8) 0.0250(3) Uani 1 1 d . . . C1 C 0.82776(17) 0.62280(15) 0.68195(11) 0.0168(3) Uani 1 1 d . . . C2 C 0.93480(17) 0.56040(15) 0.64061(11) 0.0188(3) Uani 1 1 d . . . H2 H 0.9272 0.5497 0.5919 0.023 Uiso 1 1 calc R . . C3 C 1.05295(18) 0.51387(16) 0.67136(12) 0.0226(4) Uani 1 1 d . . . H3 H 1.1258 0.4709 0.6433 0.027 Uiso 1 1 calc R . . C4 C 1.06679(19) 0.52892(17) 0.74237(13) 0.0256(4) Uani 1 1 d . . . C5 C 0.9580(2) 0.59037(18) 0.78303(12) 0.0274(4) Uani 1 1 d . . . H5 H 0.9651 0.6004 0.8320 0.033 Uiso 1 1 calc R . . C6 C 0.83859(19) 0.63758(17) 0.75329(12) 0.0231(4) Uani 1 1 d . . . H6 H 0.7651 0.6796 0.7817 0.028 Uiso 1 1 calc R . . C7 C 1.1967(2) 0.4796(2) 0.77444(16) 0.0399(6) Uani 1 1 d . . . H7A H 1.2554 0.5393 0.7619 0.060 Uiso 1 1 calc R . . H7B H 1.2457 0.4169 0.7508 0.060 Uiso 1 1 calc R . . H7C H 1.1732 0.4505 0.8315 0.060 Uiso 1 1 calc R . . C8 C 0.56046(17) 0.85090(14) 0.67488(10) 0.0162(3) Uani 1 1 d . . . C9 C 0.64608(18) 0.92567(15) 0.67660(11) 0.0183(3) Uani 1 1 d . . . H9 H 0.7430 0.9060 0.6649 0.022 Uiso 1 1 calc R . . C10 C 0.5890(2) 1.02898(15) 0.69543(11) 0.0216(4) Uani 1 1 d . . . H10 H 0.6478 1.0784 0.6983 0.026 Uiso 1 1 calc R . . C11 C 0.4471(2) 1.06164(17) 0.71027(12) 0.0257(4) Uani 1 1 d . . . C12 C 0.3630(2) 0.98522(18) 0.70929(13) 0.0283(4) Uani 1 1 d . . . H12 H 0.2660 1.0051 0.7203 0.034 Uiso 1 1 calc R . . C13 C 0.41871(19) 0.88050(16) 0.69251(12) 0.0231(4) Uani 1 1 d . . . H13 H 0.3599 0.8289 0.6931 0.028 Uiso 1 1 calc R . . C14 C 0.3863(3) 1.17776(19) 0.72503(16) 0.0397(6) Uani 1 1 d . . . H14A H 0.4597 1.2167 0.7281 0.060 Uiso 1 1 calc R . . H14B H 0.3195 1.1684 0.7745 0.060 Uiso 1 1 calc R . . H14C H 0.3404 1.2235 0.6820 0.060 Uiso 1 1 calc R . . C15 C 0.51201(17) 0.66799(15) 0.57763(10) 0.0160(3) Uani 1 1 d . . . C16 C 0.47173(19) 0.76127(16) 0.51904(11) 0.0213(4) Uani 1 1 d . . . H16 H 0.5081 0.8309 0.5079 0.026 Uiso 1 1 calc R . . C17 C 0.37835(19) 0.75183(18) 0.47718(12) 0.0253(4) Uani 1 1 d . . . H17 H 0.3507 0.8159 0.4376 0.030 Uiso 1 1 calc R . . C18 C 0.32386(18) 0.65067(17) 0.49172(11) 0.0222(4) Uani 1 1 d . . . C19 C 0.36764(18) 0.55797(16) 0.54914(12) 0.0211(4) Uani 1 1 d . . . H19 H 0.3340 0.4875 0.5588 0.025 Uiso 1 1 calc R . . C20 C 0.45970(18) 0.56603(15) 0.59276(11) 0.0187(3) Uani 1 1 d . . . H20 H 0.4867 0.5022 0.6327 0.022 Uiso 1 1 calc R . . C21 C 0.2207(2) 0.6421(2) 0.44630(13) 0.0320(5) Uani 1 1 d . . . H21A H 0.2293 0.5630 0.4428 0.048 Uiso 1 1 calc R . . H21B H 0.2382 0.6925 0.3934 0.048 Uiso 1 1 calc R . . H21C H 0.1277 0.6653 0.4732 0.048 Uiso 1 1 calc R . . C22 C 0.81479(17) 0.75266(15) 0.48186(10) 0.0172(3) Uani 1 1 d . . . C23 C 0.89093(17) 0.83150(14) 0.41263(10) 0.0151(3) Uani 1 1 d . . . C24 C 0.89971(17) 0.94185(15) 0.41598(10) 0.0166(3) Uani 1 1 d . . . H24 H 0.8531 0.9696 0.4605 0.020 Uiso 1 1 calc R . . C25 C 0.97808(18) 1.01029(15) 0.35273(11) 0.0179(3) Uani 1 1 d . . . C26 C 1.04639(18) 0.96940(15) 0.28747(11) 0.0180(3) Uani 1 1 d . . . C27 C 1.03417(17) 0.85967(15) 0.28436(10) 0.0170(3) Uani 1 1 d . . . C28 C 0.95646(17) 0.79020(15) 0.34750(10) 0.0165(3) Uani 1 1 d . . . H28 H 0.9485 0.7153 0.3459 0.020 Uiso 1 1 calc R . . C29 C 0.9098(2) 1.17208(17) 0.40705(13) 0.0278(4) Uani 1 1 d . . . H29A H 0.8134 1.1701 0.4072 0.042 Uiso 1 1 calc R . . H29B H 0.9257 1.2517 0.3953 0.042 Uiso 1 1 calc R . . H29C H 0.9309 1.1310 0.4587 0.042 Uiso 1 1 calc R . . C30 C 1.0578(3) 1.1092(2) 0.16869(14) 0.0409(6) Uani 1 1 d . . . H30A H 1.0171 1.0636 0.1458 0.061 Uiso 1 1 calc R . . H30B H 1.1221 1.1536 0.1275 0.061 Uiso 1 1 calc R . . H30C H 0.9849 1.1612 0.1925 0.061 Uiso 1 1 calc R . . C31 C 1.0869(2) 0.71999(16) 0.20984(12) 0.0256(4) Uani 1 1 d . . . H31A H 1.1247 0.6593 0.2507 0.038 Uiso 1 1 calc R . . H31B H 1.1360 0.7101 0.1581 0.038 Uiso 1 1 calc R . . H31C H 0.9892 0.7160 0.2154 0.038 Uiso 1 1 calc R . . C32 C 0.56464(17) 0.50055(14) 0.76566(10) 0.0156(3) Uani 1 1 d . . . C33 C 0.50896(17) 0.43166(14) 0.84530(10) 0.0150(3) Uani 1 1 d . . . C34 C 0.42334(18) 0.48381(15) 0.90169(10) 0.0174(3) Uani 1 1 d . . . H34 H 0.4001 0.5646 0.8904 0.021 Uiso 1 1 calc R . . C35 C 0.37205(19) 0.41598(15) 0.97495(11) 0.0196(4) Uani 1 1 d . . . C36 C 0.40832(19) 0.29684(15) 0.99080(11) 0.0206(4) Uani 1 1 d . . . C37 C 0.49439(19) 0.24594(15) 0.93370(11) 0.0187(3) Uani 1 1 d . . . C38 C 0.54465(18) 0.31378(14) 0.86047(10) 0.0167(3) Uani 1 1 d . . . H38 H 0.6029 0.2797 0.8212 0.020 Uiso 1 1 calc R . . C39 C 0.2483(2) 0.57563(17) 1.02274(14) 0.0318(5) Uani 1 1 d . . . H39A H 0.3306 0.6125 1.0116 0.048 Uiso 1 1 calc R . . H39B H 0.1867 0.5929 1.0698 0.048 Uiso 1 1 calc R . . H39C H 0.2010 0.6044 0.9782 0.048 Uiso 1 1 calc R . . C40 C 0.4470(3) 0.2007(2) 1.11657(13) 0.0402(6) Uani 1 1 d . . . H40A H 0.5358 0.1638 1.0933 0.060 Uiso 1 1 calc R . . H40B H 0.4079 0.1480 1.1649 0.060 Uiso 1 1 calc R . . H40C H 0.4598 0.2702 1.1286 0.060 Uiso 1 1 calc R . . C41 C 0.6101(2) 0.07300(16) 0.89898(12) 0.0280(4) Uani 1 1 d . . . H41A H 0.5659 0.0869 0.8539 0.042 Uiso 1 1 calc R . . H41B H 0.6258 -0.0094 0.9226 0.042 Uiso 1 1 calc R . . H41C H 0.6982 0.1028 0.8816 0.042 Uiso 1 1 calc R . . C42 C 0.9413(10) 0.9849(9) 0.0190(6) 0.090(6) Uiso 0.266(5) 1 d PD A -1 C43 C 0.9118(10) 1.1044(9) 0.0047(8) 0.079(5) Uiso 0.266(5) 1 d PDU A -1 H43 H 0.8202 1.1401 0.0178 0.095 Uiso 0.266(5) 1 calc PR A -1 C44 C 1.0175(12) 1.1697(8) -0.0285(7) 0.095(5) Uiso 0.266(5) 1 d PD A -1 H44 H 0.9961 1.2505 -0.0379 0.114 Uiso 0.266(5) 1 calc PR A -1 C45 C 1.1510(10) 1.1233(8) -0.0485(5) 0.049(3) Uiso 0.266(5) 1 d PD A -1 H45 H 1.2214 1.1704 -0.0712 0.059 Uiso 0.266(5) 1 calc PR A -1 C46 C 1.1809(10) 1.0031(9) -0.0342(7) 0.099(5) Uiso 0.266(5) 1 d PDU A -1 H46 H 1.2727 0.9677 -0.0473 0.119 Uiso 0.266(5) 1 calc PR A -1 C47 C 1.0786(10) 0.9385(8) -0.0017(6) 0.047(3) Uiso 0.266(5) 1 d PD A -1 H47 H 1.1008 0.8578 0.0074 0.057 Uiso 0.266(5) 1 calc PR A -1 C48 C 0.8140(14) 0.9322(16) 0.0546(8) 0.087(5) Uiso 0.266(5) 1 d PD A -1 H48A H 0.8363 0.8488 0.0648 0.130 Uiso 0.266(5) 1 calc PR A -1 H48B H 0.7493 0.9594 0.0185 0.130 Uiso 0.266(5) 1 calc PR A -1 H48C H 0.7723 0.9536 0.1040 0.130 Uiso 0.266(5) 1 calc PR A -1 C49 C 1.1387(10) 0.9079(9) -0.0127(8) 0.059(4) Uiso 0.234(5) 1 d PD A -2 H49 H 1.2053 0.8420 -0.0146 0.071 Uiso 0.234(5) 1 calc PR A -2 C50 C 1.1756(10) 1.0158(12) -0.0401(7) 0.103(6) Uiso 0.234(5) 1 d PDU A -2 H50 H 1.2687 1.0262 -0.0616 0.124 Uiso 0.234(5) 1 calc PR A -2 C51 C 1.0761(11) 1.1077(8) -0.0360(5) 0.046(3) Uiso 0.234(5) 1 d PD A -2 C52 C 0.9389(11) 1.1021(10) -0.0061(7) 0.044(3) Uiso 0.234(5) 1 d PDU A -2 H52 H 0.8739 1.1690 -0.0047 0.053 Uiso 0.234(5) 1 calc PR A -2 C53 C 0.8996(10) 0.9923(11) 0.0222(8) 0.074(6) Uiso 0.234(5) 1 d PD A -2 H53 H 0.8061 0.9831 0.0435 0.089 Uiso 0.234(5) 1 calc PR A -2 C54 C 0.9983(12) 0.8977(10) 0.0187(7) 0.069(5) Uiso 0.234(5) 1 d PD A -2 H54 H 0.9712 0.8236 0.0379 0.083 Uiso 0.234(5) 1 calc PR A -2 C55 C 1.122(2) 1.2136(13) -0.0649(8) 0.121(8) Uiso 0.234(5) 1 d PD A -2 H55A H 1.2215 1.2029 -0.0837 0.182 Uiso 0.234(5) 1 calc PR A -2 H55B H 1.0999 1.2540 -0.0231 0.182 Uiso 0.234(5) 1 calc PR A -2 H55C H 1.0766 1.2586 -0.1083 0.182 Uiso 0.234(5) 1 calc PR A -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 Sb1 0.01501(5) 0.01363(6) 0.01067(5) -0.00116(4) -0.00055(4) -0.00278(4) O1 0.0180(6) 0.0125(6) 0.0143(6) 0.0001(5) -0.0008(5) -0.0019(4) O2 0.0236(6) 0.0192(6) 0.0109(6) -0.0021(5) 0.0005(5) -0.0031(5) O3 0.0200(6) 0.0202(6) 0.0123(6) -0.0021(5) 0.0020(5) -0.0068(5) O4 0.0289(7) 0.0158(6) 0.0204(7) -0.0018(5) 0.0022(6) -0.0064(5) O5 0.0401(8) 0.0196(7) 0.0188(7) -0.0063(6) 0.0101(6) -0.0035(6) O6 0.0425(8) 0.0220(7) 0.0144(7) 0.0011(5) 0.0097(6) -0.0101(6) O7 0.0384(8) 0.0125(6) 0.0175(7) -0.0013(5) 0.0075(6) -0.0046(5) O8 0.0291(7) 0.0197(7) 0.0267(8) -0.0100(6) 0.0080(6) -0.0124(5) O9 0.0239(6) 0.0235(7) 0.0176(7) -0.0010(5) 0.0055(5) -0.0109(5) O10 0.0320(7) 0.0229(7) 0.0179(7) -0.0088(5) 0.0092(6) -0.0100(6) C1 0.0164(8) 0.0162(8) 0.0168(8) -0.0018(6) -0.0019(6) -0.0046(6) C2 0.0182(8) 0.0169(8) 0.0198(9) -0.0031(7) -0.0003(7) -0.0053(6) C3 0.0160(8) 0.0182(9) 0.0308(11) -0.0027(8) -0.0023(7) -0.0038(7) C4 0.0203(9) 0.0229(9) 0.0322(11) 0.0010(8) -0.0096(8) -0.0055(7) C5 0.0286(10) 0.0337(11) 0.0223(10) -0.0047(8) -0.0109(8) -0.0057(8) C6 0.0223(9) 0.0260(10) 0.0208(10) -0.0079(8) -0.0041(7) -0.0002(7) C7 0.0254(10) 0.0449(14) 0.0480(15) -0.0024(11) -0.0186(10) -0.0015(9) C8 0.0194(8) 0.0159(8) 0.0115(8) -0.0020(6) -0.0026(6) -0.0010(6) C9 0.0209(8) 0.0177(8) 0.0145(8) -0.0011(7) -0.0027(7) -0.0035(6) C10 0.0306(10) 0.0167(8) 0.0180(9) -0.0026(7) -0.0064(8) -0.0050(7) C11 0.0328(10) 0.0205(9) 0.0241(10) -0.0075(8) -0.0111(8) 0.0053(8) C12 0.0212(9) 0.0302(11) 0.0355(12) -0.0155(9) -0.0090(8) 0.0069(8) C13 0.0203(8) 0.0233(9) 0.0271(10) -0.0094(8) -0.0052(8) -0.0008(7) C14 0.0458(13) 0.0280(12) 0.0490(16) -0.0208(11) -0.0170(12) 0.0122(10) C15 0.0159(7) 0.0198(8) 0.0119(8) -0.0042(6) -0.0009(6) -0.0029(6) C16 0.0230(9) 0.0222(9) 0.0161(9) 0.0001(7) -0.0030(7) -0.0047(7) C17 0.0241(9) 0.0317(11) 0.0160(9) -0.0005(8) -0.0056(7) -0.0007(8) C18 0.0159(8) 0.0346(11) 0.0173(9) -0.0124(8) -0.0032(7) 0.0022(7) C19 0.0164(8) 0.0252(9) 0.0231(10) -0.0102(8) -0.0018(7) -0.0026(7) C20 0.0191(8) 0.0191(8) 0.0170(9) -0.0040(7) -0.0020(7) -0.0030(6) C21 0.0253(10) 0.0470(13) 0.0287(11) -0.0171(10) -0.0111(9) 0.0017(9) C22 0.0161(8) 0.0194(8) 0.0138(8) -0.0006(6) -0.0013(6) -0.0039(6) C23 0.0141(7) 0.0169(8) 0.0127(8) -0.0019(6) -0.0011(6) -0.0031(6) C24 0.0168(8) 0.0193(8) 0.0132(8) -0.0043(6) 0.0003(6) -0.0048(6) C25 0.0184(8) 0.0168(8) 0.0186(9) -0.0047(7) -0.0011(7) -0.0052(6) C26 0.0173(8) 0.0188(8) 0.0159(8) -0.0023(7) 0.0016(6) -0.0067(6) C27 0.0181(8) 0.0190(8) 0.0127(8) -0.0046(6) 0.0013(6) -0.0036(6) C28 0.0179(8) 0.0152(8) 0.0150(8) -0.0023(6) -0.0008(6) -0.0038(6) C29 0.0335(10) 0.0232(10) 0.0281(11) -0.0133(8) 0.0037(9) -0.0088(8) C30 0.0438(13) 0.0443(14) 0.0242(12) 0.0113(10) -0.0034(10) -0.0150(11) C31 0.0316(10) 0.0224(10) 0.0221(10) -0.0102(8) 0.0031(8) -0.0055(8) C32 0.0150(7) 0.0173(8) 0.0140(8) -0.0013(6) -0.0028(6) -0.0047(6) C33 0.0167(7) 0.0160(8) 0.0119(8) -0.0019(6) -0.0011(6) -0.0053(6) C34 0.0204(8) 0.0157(8) 0.0141(8) -0.0016(6) -0.0007(7) -0.0039(6) C35 0.0228(8) 0.0200(9) 0.0141(8) -0.0050(7) 0.0029(7) -0.0053(7) C36 0.0281(9) 0.0170(8) 0.0130(8) -0.0003(7) 0.0027(7) -0.0077(7) C37 0.0248(9) 0.0140(8) 0.0152(8) -0.0019(6) 0.0007(7) -0.0060(7) C38 0.0202(8) 0.0159(8) 0.0124(8) -0.0033(6) 0.0008(6) -0.0036(6) C39 0.0392(12) 0.0235(10) 0.0274(11) -0.0112(9) 0.0062(9) -0.0003(8) C40 0.0728(17) 0.0293(12) 0.0133(10) 0.0000(8) -0.0031(10) -0.0091(11) C41 0.0404(11) 0.0160(9) 0.0205(10) -0.0042(7) 0.0074(8) -0.0043(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sb1 C8 2.0986(18) . ? Sb1 C15 2.1031(17) . ? Sb1 C1 2.1063(17) . ? Sb1 O3 2.1179(12) . ? Sb1 O1 2.1428(12) . ? O1 C32 1.311(2) . ? O2 C32 1.232(2) . ? O3 C22 1.307(2) . ? O4 C22 1.229(2) . ? O5 C35 1.364(2) . ? O5 C39 1.423(2) . ? O6 C36 1.375(2) . ? O6 C40 1.432(3) . ? O7 C37 1.364(2) . ? O7 C41 1.436(2) . ? O8 C25 1.367(2) . ? O8 C29 1.425(2) . ? O9 C26 1.373(2) . ? O9 C30 1.425(3) . ? O10 C27 1.360(2) . ? O10 C31 1.430(2) . ? C1 C6 1.387(3) . ? C1 C2 1.392(3) . ? C2 C3 1.390(3) . ? C3 C4 1.393(3) . ? C4 C5 1.389(3) . ? C4 C7 1.510(3) . ? C5 C6 1.394(3) . ? C8 C13 1.391(2) . ? C8 C9 1.394(2) . ? C9 C10 1.389(3) . ? C10 C11 1.396(3) . ? C11 C12 1.394(3) . ? C11 C14 1.512(3) . ? C12 C13 1.388(3) . ? C15 C20 1.390(2) . ? C15 C16 1.393(2) . ? C16 C17 1.384(3) . ? C17 C18 1.394(3) . ? C18 C19 1.388(3) . ? C18 C21 1.510(3) . ? C19 C20 1.390(3) . ? C22 C23 1.503(2) . ? C23 C28 1.389(2) . ? C23 C24 1.398(2) . ? C24 C25 1.393(2) . ? C25 C26 1.394(3) . ? C26 C27 1.399(2) . ? C27 C28 1.395(2) . ? C32 C33 1.494(2) . ? C33 C38 1.388(2) . ? C33 C34 1.393(2) . ? C34 C35 1.395(2) . ? C35 C36 1.403(3) . ? C36 C37 1.395(3) . ? C37 C38 1.392(2) . ? C42 C47 1.399(8) . ? C42 C43 1.402(8) . ? C42 C48 1.483(9) . ? C43 C44 1.384(8) . ? C44 C45 1.364(8) . ? C45 C46 1.412(8) . ? C46 C47 1.350(8) . ? C49 C50 1.374(8) . ? C49 C54 1.415(8) . ? C50 C51 1.364(8) . ? C51 C52 1.373(8) . ? C51 C55 1.389(9) . ? C52 C53 1.405(8) . ? C53 C54 1.382(8) . ? 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 C8 Sb1 C15 107.73(7) . . ? C8 Sb1 C1 112.17(7) . . ? C15 Sb1 C1 140.09(7) . . ? C8 Sb1 O3 86.39(6) . . ? C15 Sb1 O3 91.68(6) . . ? C1 Sb1 O3 90.15(6) . . ? C8 Sb1 O1 87.14(6) . . ? C15 Sb1 O1 93.11(6) . . ? C1 Sb1 O1 89.55(6) . . ? O3 Sb1 O1 172.88(5) . . ? C32 O1 Sb1 111.29(11) . . ? C22 O3 Sb1 119.15(11) . . ? C35 O5 C39 117.26(15) . . ? C36 O6 C40 112.69(16) . . ? C37 O7 C41 117.37(14) . . ? C25 O8 C29 116.90(14) . . ? C26 O9 C30 113.40(15) . . ? C27 O10 C31 117.29(14) . . ? C6 C1 C2 120.33(17) . . ? C6 C1 Sb1 116.59(13) . . ? C2 C1 Sb1 123.08(14) . . ? C3 C2 C1 119.22(18) . . ? C2 C3 C4 121.43(19) . . ? C5 C4 C3 118.33(18) . . ? C5 C4 C7 120.8(2) . . ? C3 C4 C7 120.9(2) . . ? C4 C5 C6 121.1(2) . . ? C1 C6 C5 119.54(19) . . ? C13 C8 C9 119.50(17) . . ? C13 C8 Sb1 119.74(13) . . ? C9 C8 Sb1 120.73(13) . . ? C10 C9 C8 119.73(17) . . ? C9 C10 C11 121.33(17) . . ? C12 C11 C10 118.13(18) . . ? C12 C11 C14 120.95(19) . . ? C10 C11 C14 120.91(19) . . ? C13 C12 C11 121.04(18) . . ? C12 C13 C8 120.20(17) . . ? C20 C15 C16 119.82(16) . . ? C20 C15 Sb1 124.36(13) . . ? C16 C15 Sb1 115.73(13) . . ? C17 C16 C15 119.54(17) . . ? C16 C17 C18 121.61(18) . . ? C19 C18 C17 117.95(17) . . ? C19 C18 C21 121.03(18) . . ? C17 C18 C21 121.02(18) . . ? C18 C19 C20 121.42(17) . . ? C15 C20 C19 119.63(17) . . ? O4 C22 O3 123.84(16) . . ? O4 C22 C23 121.33(17) . . ? O3 C22 C23 114.83(15) . . ? C28 C23 C24 121.43(15) . . ? C28 C23 C22 118.38(15) . . ? C24 C23 C22 120.12(16) . . ? C25 C24 C23 118.69(16) . . ? O8 C25 C24 124.56(17) . . ? O8 C25 C26 114.87(15) . . ? C24 C25 C26 120.57(16) . . ? O9 C26 C25 120.27(16) . . ? O9 C26 C27 119.69(16) . . ? C25 C26 C27 120.01(15) . . ? O10 C27 C28 124.77(16) . . ? O10 C27 C26 115.33(15) . . ? C28 C27 C26 119.90(16) . . ? C23 C28 C27 119.37(16) . . ? O2 C32 O1 122.10(15) . . ? O2 C32 C33 121.18(15) . . ? O1 C32 C33 116.72(15) . . ? C38 C33 C34 121.44(16) . . ? C38 C33 C32 117.38(16) . . ? C34 C33 C32 121.18(15) . . ? C33 C34 C35 119.24(16) . . ? O5 C35 C34 125.52(17) . . ? O5 C35 C36 114.89(16) . . ? C34 C35 C36 119.60(17) . . ? O6 C36 C37 119.97(16) . . ? O6 C36 C35 119.55(17) . . ? C37 C36 C35 120.45(16) . . ? O7 C37 C38 124.98(17) . . ? O7 C37 C36 115.19(15) . . ? C38 C37 C36 119.83(16) . . ? C33 C38 C37 119.44(17) . . ? C47 C42 C43 117.1(6) . . ? C47 C42 C48 132.6(11) . . ? C43 C42 C48 110.4(10) . . ? C44 C43 C42 119.3(7) . . ? C45 C44 C43 123.0(7) . . ? C44 C45 C46 117.7(6) . . ? C47 C46 C45 119.7(7) . . ? C46 C47 C42 123.1(7) . . ? C50 C49 C54 118.0(7) . . ? C51 C50 C49 118.8(7) . . ? C50 C51 C52 125.3(7) . . ? C50 C51 C55 115.2(13) . . ? C52 C51 C55 119.5(13) . . ? C51 C52 C53 116.6(7) . . ? C54 C53 C52 119.3(7) . . ? C53 C54 C49 122.0(7) . . ? _diffrn_measured_fraction_theta_max 0.887 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.176 _refine_diff_density_min -0.555 _refine_diff_density_rms 0.088 _database_code_depnum_ccdc_archive 'CCDC 857412'