# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 ####################################################################### # # 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_shelxl _database_code_depnum_ccdc_archive 'CCDC 890807' #TrackingRef 'cd.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H17 Cd O9' _chemical_formula_weight 609.82 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' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M c2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 33.321(7) _cell_length_b 9.807(2) _cell_length_c 7.8951(16) _cell_angle_alpha 90.00 _cell_angle_beta 96.68(3) _cell_angle_gamma 90.00 _cell_volume 2562.4(9) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _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 1.581 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1220 _exptl_absorpt_coefficient_mu 0.906 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.8395 _exptl_absorpt_correction_T_max 0.9148 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12124 _diffrn_reflns_av_R_equivalents 0.0413 _diffrn_reflns_av_sigmaI/netI 0.0359 _diffrn_reflns_limit_h_min -41 _diffrn_reflns_limit_h_max 43 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 3.33 _diffrn_reflns_theta_max 27.46 _reflns_number_total 2930 _reflns_number_gt 2149 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _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^)+(0.0500P)^2^+6.8070P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2930 _refine_ls_number_parameters 174 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0637 _refine_ls_R_factor_gt 0.0410 _refine_ls_wR_factor_ref 0.1234 _refine_ls_wR_factor_gt 0.0924 _refine_ls_goodness_of_fit_ref 1.128 _refine_ls_restrained_S_all 1.128 _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 Cd1 Cd 0.0000 0.47079(5) 0.2500 0.04869(18) Uani 1 2 d S . . O1 O 0.04767(9) 0.3316(4) 0.3880(4) 0.0652(9) Uani 1 1 d . . . O1W O 0.0000 0.7005(5) 0.2500 0.0801(15) Uani 1 2 d S . . H1W H -0.0168 0.7284 0.1736 0.120 Uiso 0.50 1 calc PR . . O2 O 0.04396(9) 0.5249(3) 0.5263(5) 0.0611(9) Uani 1 1 d . . . C1 C 0.06120(11) 0.4135(5) 0.5041(6) 0.0533(11) Uani 1 1 d . . . C2 C 0.09935(11) 0.3781(5) 0.6146(5) 0.0472(10) Uani 1 1 d . . . C3 C 0.12107(12) 0.4798(5) 0.7046(6) 0.0508(10) Uani 1 1 d . . . H3 H 0.1110 0.5683 0.7018 0.061 Uiso 1 1 calc R . . C4 C 0.15782(12) 0.4508(4) 0.7993(6) 0.0503(11) Uani 1 1 d . . . H4 H 0.1724 0.5203 0.8585 0.060 Uiso 1 1 calc R . . C5 C 0.17288(11) 0.3196(4) 0.8060(5) 0.0466(10) Uani 1 1 d . . . C6 C 0.15060(13) 0.2178(5) 0.7187(6) 0.0599(13) Uani 1 1 d . . . H6 H 0.1602 0.1287 0.7242 0.072 Uiso 1 1 calc R . . C7 C 0.11409(12) 0.2469(5) 0.6228(6) 0.0572(12) Uani 1 1 d . . . H7 H 0.0995 0.1774 0.5637 0.069 Uiso 1 1 calc R . . C8 C 0.21275(11) 0.2861(4) 0.9069(5) 0.0429(9) Uani 1 1 d . . . C9 C 0.21324(11) 0.2251(4) 1.0673(5) 0.0431(9) Uani 1 1 d . . . C10 C 0.24867(11) 0.3117(4) 0.8375(5) 0.0439(9) Uani 1 1 d . . . C11 C 0.24964(13) 0.3726(5) 0.6742(6) 0.0543(11) Uani 1 1 d . . . H11 H 0.2254 0.3974 0.6109 0.065 Uiso 1 1 calc R . . C12 C 0.28472(14) 0.3955(5) 0.6086(6) 0.0579(11) Uani 1 1 d . . . H12 H 0.2843 0.4353 0.5016 0.069 Uiso 1 1 calc R . . C13 C 0.32189(13) 0.3593(5) 0.7013(6) 0.0577(12) Uani 1 1 d . . . H13 H 0.3459 0.3752 0.6551 0.069 Uiso 1 1 calc R . . C14 C 0.17722(12) 0.1985(4) 1.1426(6) 0.0513(11) Uani 1 1 d . . . H14 H 0.1524 0.2214 1.0829 0.062 Uiso 1 1 calc R . . O3WB O 0.9466(5) 0.8514(15) 0.030(2) 0.367(9) Uani 1 1 d . . . O2WA O 0.0551(5) 0.0740(14) 0.2551(18) 0.355(10) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.0318(2) 0.0590(3) 0.0499(3) 0.000 -0.01802(17) 0.000 O1 0.0425(16) 0.091(2) 0.0555(19) 0.0008(17) -0.0230(14) 0.0047(16) O1W 0.094(4) 0.061(3) 0.080(4) 0.000 -0.010(3) 0.000 O2 0.0317(14) 0.072(2) 0.076(2) 0.0129(17) -0.0108(14) 0.0139(15) C1 0.0278(18) 0.077(3) 0.051(3) 0.012(2) -0.0089(17) 0.001(2) C2 0.0288(18) 0.066(3) 0.043(2) 0.0047(19) -0.0111(16) 0.0057(17) C3 0.0326(19) 0.052(2) 0.063(3) 0.008(2) -0.0125(18) 0.0066(17) C4 0.036(2) 0.053(3) 0.057(3) 0.0003(19) -0.0179(18) 0.0042(17) C5 0.0328(18) 0.056(3) 0.046(2) 0.0026(19) -0.0151(16) 0.0063(17) C6 0.046(2) 0.053(3) 0.073(3) -0.004(2) -0.025(2) 0.0102(19) C7 0.043(2) 0.061(3) 0.061(3) -0.010(2) -0.022(2) 0.005(2) C8 0.0328(18) 0.045(2) 0.046(2) -0.0001(17) -0.0149(16) 0.0044(16) C9 0.0355(19) 0.043(2) 0.047(2) -0.0037(17) -0.0129(16) 0.0054(16) C10 0.040(2) 0.044(2) 0.044(2) -0.0007(17) -0.0156(16) 0.0049(16) C11 0.046(2) 0.055(3) 0.056(3) 0.004(2) -0.0206(19) 0.0034(19) C12 0.058(3) 0.059(3) 0.054(3) 0.008(2) -0.006(2) -0.002(2) C13 0.046(2) 0.060(3) 0.065(3) 0.000(2) -0.001(2) -0.001(2) C14 0.038(2) 0.054(3) 0.058(3) -0.001(2) -0.0114(18) 0.0059(18) O3WB 0.382(18) 0.301(17) 0.41(2) 0.144(15) -0.007(16) 0.166(14) O2WA 0.48(2) 0.237(12) 0.306(16) -0.120(11) -0.137(16) 0.131(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 O1W 2.253(5) . ? Cd1 O1 2.274(3) 2 ? Cd1 O1 2.274(3) . ? Cd1 O2 2.423(4) 5_566 ? Cd1 O2 2.423(4) 6_565 ? Cd1 O2 2.538(3) 2 ? Cd1 O2 2.538(3) . ? Cd1 C1 2.747(4) 2 ? Cd1 C1 2.747(4) . ? O1 C1 1.262(6) . ? O1W H1W 0.8200 . ? O2 C1 1.256(6) . ? O2 Cd1 2.423(4) 5_566 ? C1 C2 1.497(5) . ? C2 C7 1.377(6) . ? C2 C3 1.379(6) . ? C3 C4 1.388(5) . ? C3 H3 0.9300 . ? C4 C5 1.380(6) . ? C4 H4 0.9300 . ? C5 C6 1.380(6) . ? C5 C8 1.503(4) . ? C6 C7 1.386(5) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 C10 1.395(6) . ? C8 C9 1.399(6) . ? C9 C14 1.424(6) . ? C9 C10 1.443(5) 7_557 ? C10 C11 1.426(6) . ? C10 C9 1.443(5) 7_557 ? C11 C12 1.351(7) . ? C11 H11 0.9300 . ? C12 C13 1.409(6) . ? C12 H12 0.9300 . ? C13 C14 1.354(6) 7_557 ? C13 H13 0.9300 . ? C14 C13 1.354(6) 7_557 ? C14 H14 0.9300 . ? 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 O1W Cd1 O1 126.89(9) . 2 ? O1W Cd1 O1 126.89(9) . . ? O1 Cd1 O1 106.22(17) 2 . ? O1W Cd1 O2 89.00(8) . 5_566 ? O1 Cd1 O2 84.95(12) 2 5_566 ? O1 Cd1 O2 96.26(12) . 5_566 ? O1W Cd1 O2 89.00(8) . 6_565 ? O1 Cd1 O2 96.26(12) 2 6_565 ? O1 Cd1 O2 84.95(12) . 6_565 ? O2 Cd1 O2 178.01(16) 5_566 6_565 ? O1W Cd1 O2 77.93(8) . 2 ? O1 Cd1 O2 54.03(11) 2 2 ? O1 Cd1 O2 146.98(12) . 2 ? O2 Cd1 O2 106.59(11) 5_566 2 ? O2 Cd1 O2 72.97(11) 6_565 2 ? O1W Cd1 O2 77.93(8) . . ? O1 Cd1 O2 146.98(12) 2 . ? O1 Cd1 O2 54.03(11) . . ? O2 Cd1 O2 72.97(11) 5_566 . ? O2 Cd1 O2 106.59(11) 6_565 . ? O2 Cd1 O2 155.86(15) 2 . ? O1W Cd1 C1 101.80(11) . 2 ? O1 Cd1 C1 27.07(14) 2 2 ? O1 Cd1 C1 130.17(14) . 2 ? O2 Cd1 C1 94.33(12) 5_566 2 ? O2 Cd1 C1 86.08(12) 6_565 2 ? O2 Cd1 C1 27.13(13) 2 2 ? O2 Cd1 C1 167.30(12) . 2 ? O1W Cd1 C1 101.80(11) . . ? O1 Cd1 C1 130.17(14) 2 . ? O1 Cd1 C1 27.07(14) . . ? O2 Cd1 C1 86.08(12) 5_566 . ? O2 Cd1 C1 94.33(12) 6_565 . ? O2 Cd1 C1 167.30(12) 2 . ? O2 Cd1 C1 27.13(13) . . ? C1 Cd1 C1 156.4(2) 2 . ? C1 O1 Cd1 97.8(3) . . ? Cd1 O1W H1W 109.5 . . ? C1 O2 Cd1 116.2(3) . 5_566 ? C1 O2 Cd1 85.7(3) . . ? Cd1 O2 Cd1 107.03(11) 5_566 . ? O2 C1 O1 121.6(4) . . ? O2 C1 C2 119.4(4) . . ? O1 C1 C2 118.9(4) . . ? O2 C1 Cd1 67.1(2) . . ? O1 C1 Cd1 55.1(2) . . ? C2 C1 Cd1 168.9(3) . . ? C7 C2 C3 119.3(3) . . ? C7 C2 C1 121.2(4) . . ? C3 C2 C1 119.5(4) . . ? C2 C3 C4 120.5(4) . . ? C2 C3 H3 119.8 . . ? C4 C3 H3 119.8 . . ? C5 C4 C3 120.4(4) . . ? C5 C4 H4 119.8 . . ? C3 C4 H4 119.8 . . ? C6 C5 C4 118.9(3) . . ? C6 C5 C8 119.9(4) . . ? C4 C5 C8 121.2(4) . . ? C5 C6 C7 120.8(4) . . ? C5 C6 H6 119.6 . . ? C7 C6 H6 119.6 . . ? C2 C7 C6 120.2(4) . . ? C2 C7 H7 119.9 . . ? C6 C7 H7 119.9 . . ? C10 C8 C9 120.8(3) . . ? C10 C8 C5 119.9(4) . . ? C9 C8 C5 119.3(4) . . ? C8 C9 C14 122.3(3) . . ? C8 C9 C10 119.7(4) . 7_557 ? C14 C9 C10 118.0(4) . 7_557 ? C8 C10 C11 122.7(3) . . ? C8 C10 C9 119.6(4) . 7_557 ? C11 C10 C9 117.7(4) . 7_557 ? C12 C11 C10 121.9(4) . . ? C12 C11 H11 119.1 . . ? C10 C11 H11 119.1 . . ? C11 C12 C13 120.5(4) . . ? C11 C12 H12 119.8 . . ? C13 C12 H12 119.8 . . ? C14 C13 C12 120.2(4) 7_557 . ? C14 C13 H13 119.9 7_557 . ? C12 C13 H13 119.9 . . ? C13 C14 C9 121.8(4) 7_557 . ? C13 C14 H14 119.1 7_557 . ? C9 C14 H14 119.1 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1W Cd1 O1 C1 24.9(3) . . . . ? O1 Cd1 O1 C1 -155.1(3) 2 . . . ? O2 Cd1 O1 C1 -68.5(3) 5_566 . . . ? O2 Cd1 O1 C1 109.9(3) 6_565 . . . ? O2 Cd1 O1 C1 157.4(3) 2 . . . ? O2 Cd1 O1 C1 -4.9(3) . . . . ? C1 Cd1 O1 C1 -169.61(17) 2 . . . ? O1W Cd1 O2 C1 -151.2(3) . . . . ? O1 Cd1 O2 C1 66.0(3) 2 . . . ? O1 Cd1 O2 C1 4.9(3) . . . . ? O2 Cd1 O2 C1 116.1(3) 5_566 . . . ? O2 Cd1 O2 C1 -65.9(2) 6_565 . . . ? O2 Cd1 O2 C1 -151.2(3) 2 . . . ? C1 Cd1 O2 C1 118.7(7) 2 . . . ? O1W Cd1 O2 Cd1 92.69(10) . . . 5_566 ? O1 Cd1 O2 Cd1 -50.2(3) 2 . . 5_566 ? O1 Cd1 O2 Cd1 -111.29(18) . . . 5_566 ? O2 Cd1 O2 Cd1 0.0 5_566 . . 5_566 ? O2 Cd1 O2 Cd1 177.97(17) 6_565 . . 5_566 ? O2 Cd1 O2 Cd1 92.69(10) 2 . . 5_566 ? C1 Cd1 O2 Cd1 2.6(7) 2 . . 5_566 ? C1 Cd1 O2 Cd1 -116.1(3) . . . 5_566 ? Cd1 O2 C1 O1 98.5(5) 5_566 . . . ? Cd1 O2 C1 O1 -8.3(4) . . . . ? Cd1 O2 C1 C2 -83.1(4) 5_566 . . . ? Cd1 O2 C1 C2 170.0(4) . . . . ? Cd1 O2 C1 Cd1 106.9(2) 5_566 . . . ? Cd1 O1 C1 O2 9.4(5) . . . . ? Cd1 O1 C1 C2 -169.0(3) . . . . ? O1W Cd1 C1 O2 28.8(3) . . . . ? O1 Cd1 C1 O2 -139.4(3) 2 . . . ? O1 Cd1 C1 O2 -171.3(5) . . . . ? O2 Cd1 C1 O2 -59.4(3) 5_566 . . . ? O2 Cd1 C1 O2 118.7(2) 6_565 . . . ? O2 Cd1 C1 O2 116.2(7) 2 . . . ? C1 Cd1 C1 O2 -151.2(3) 2 . . . ? O1W Cd1 C1 O1 -159.9(3) . . . . ? O1 Cd1 C1 O1 32.0(4) 2 . . . ? O2 Cd1 C1 O1 112.0(3) 5_566 . . . ? O2 Cd1 C1 O1 -70.0(3) 6_565 . . . ? O2 Cd1 C1 O1 -72.4(7) 2 . . . ? O2 Cd1 C1 O1 171.3(5) . . . . ? C1 Cd1 C1 O1 20.1(3) 2 . . . ? O1W Cd1 C1 C2 -99.6(18) . . . . ? O1 Cd1 C1 C2 92.3(18) 2 . . . ? O1 Cd1 C1 C2 60.3(18) . . . . ? O2 Cd1 C1 C2 172.3(19) 5_566 . . . ? O2 Cd1 C1 C2 -9.7(19) 6_565 . . . ? O2 Cd1 C1 C2 -12(2) 2 . . . ? O2 Cd1 C1 C2 -128(2) . . . . ? C1 Cd1 C1 C2 80.4(18) 2 . . . ? O2 C1 C2 C7 164.7(4) . . . . ? O1 C1 C2 C7 -16.9(7) . . . . ? Cd1 C1 C2 C7 -71(2) . . . . ? O2 C1 C2 C3 -18.0(7) . . . . ? O1 C1 C2 C3 160.4(4) . . . . ? Cd1 C1 C2 C3 105.9(18) . . . . ? C7 C2 C3 C4 1.4(7) . . . . ? C1 C2 C3 C4 -175.9(4) . . . . ? C2 C3 C4 C5 -0.7(7) . . . . ? C3 C4 C5 C6 -0.6(7) . . . . ? C3 C4 C5 C8 179.6(4) . . . . ? C4 C5 C6 C7 1.3(8) . . . . ? C8 C5 C6 C7 -179.0(4) . . . . ? C3 C2 C7 C6 -0.8(7) . . . . ? C1 C2 C7 C6 176.5(4) . . . . ? C5 C6 C7 C2 -0.6(8) . . . . ? C6 C5 C8 C10 99.3(5) . . . . ? C4 C5 C8 C10 -81.0(6) . . . . ? C6 C5 C8 C9 -78.5(6) . . . . ? C4 C5 C8 C9 101.3(5) . . . . ? C10 C8 C9 C14 179.5(4) . . . . ? C5 C8 C9 C14 -2.7(6) . . . . ? C10 C8 C9 C10 0.1(7) . . . 7_557 ? C5 C8 C9 C10 177.8(4) . . . 7_557 ? C9 C8 C10 C11 179.5(4) . . . . ? C5 C8 C10 C11 1.8(6) . . . . ? C9 C8 C10 C9 -0.1(7) . . . 7_557 ? C5 C8 C10 C9 -177.8(4) . . . 7_557 ? C8 C10 C11 C12 -179.4(5) . . . . ? C9 C10 C11 C12 0.2(6) 7_557 . . . ? C10 C11 C12 C13 -0.1(7) . . . . ? C11 C12 C13 C14 -0.1(8) . . . 7_557 ? C8 C9 C14 C13 -179.3(4) . . . 7_557 ? C10 C9 C14 C13 0.1(6) 7_557 . . 7_557 ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.722 _refine_diff_density_min -1.018 _refine_diff_density_rms 0.109