# Electronic Supplementary Material (ESI) for Chemical Communications # 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_mo_dm12037_0m _database_code_depnum_ccdc_archive 'CCDC 892574' #TrackingRef 'mo_dm12037_0m.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H19 Cl' _chemical_formula_weight 414.90 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n 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 13.7094(11) _cell_length_b 9.4888(8) _cell_length_c 19.2635(16) _cell_angle_alpha 90.00 _cell_angle_beta 92.874(2) _cell_angle_gamma 90.00 _cell_volume 2502.8(4) _cell_formula_units_Z 4 _cell_measurement_temperature 133(2) _cell_measurement_reflns_used 31 _cell_measurement_theta_min 2.79 _cell_measurement_theta_max 23.51 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.39 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.28 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.101 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 864 _exptl_absorpt_coefficient_mu 0.165 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9383 _exptl_absorpt_correction_T_max 0.9552 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 133(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 APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 15488 _diffrn_reflns_av_R_equivalents 0.0302 _diffrn_reflns_av_sigmaI/netI 0.0412 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.61 _diffrn_reflns_theta_max 25.09 _reflns_number_total 4409 _reflns_number_gt 3544 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.1144P)^2^+8.0500P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0044(12) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4409 _refine_ls_number_parameters 290 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1051 _refine_ls_R_factor_gt 0.0920 _refine_ls_wR_factor_ref 0.2524 _refine_ls_wR_factor_gt 0.2434 _refine_ls_goodness_of_fit_ref 0.926 _refine_ls_restrained_S_all 0.926 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.020 -0.141 0.283 131 63 ' ' 2 0.020 0.138 0.717 130 63 ' ' 3 0.520 0.359 0.217 131 64 ' ' 4 0.480 0.638 0.783 130 63 ' ' _platon_squeeze_details ; ; loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cl1 Cl 0.02594(10) 0.8950(2) 0.06166(9) 0.0458(5) Uani 0.60 1 d PU . . Cl2 Cl 0.91808(19) 0.9049(3) 0.51355(14) 0.0475(6) Uani 0.40 1 d P . . C1 C 0.3982(3) 0.8836(3) 0.23298(18) 0.0258(7) Uani 1 1 d . . . C2 C 0.4893(2) 0.8811(3) 0.20119(17) 0.0238(7) Uani 1 1 d . . . C3 C 0.4943(2) 0.8791(3) 0.12807(17) 0.0252(7) Uani 1 1 d . . . H3 H 0.4354 0.8778 0.0999 0.030 Uiso 1 1 calc R . . C4 C 0.5831(2) 0.8791(3) 0.09635(17) 0.0234(7) Uani 1 1 d . . . C5 C 0.5879(2) 0.8772(3) 0.02183(17) 0.0263(7) Uani 1 1 d . . . H5 H 0.5293 0.8727 -0.0065 0.032 Uiso 1 1 calc R . . C6 C 0.6756(3) 0.8816(3) -0.00847(18) 0.0290(8) Uani 1 1 d . . . H6 H 0.6777 0.8806 -0.0577 0.035 Uiso 1 1 calc R . . C7 C 0.7641(2) 0.8877(3) 0.03328(18) 0.0275(7) Uani 1 1 d . . . H7 H 0.8247 0.8931 0.0116 0.033 Uiso 1 1 calc R . . C8 C 0.7630(2) 0.8860(3) 0.10385(17) 0.0237(7) Uani 1 1 d . . . H8 H 0.8230 0.8879 0.1307 0.028 Uiso 1 1 calc R . . C9 C 0.6725(2) 0.8814(3) 0.13840(17) 0.0240(7) Uani 1 1 d . . . C10 C 0.6685(2) 0.8820(3) 0.21029(17) 0.0242(7) Uani 1 1 d . . . H10 H 0.7278 0.8835 0.2380 0.029 Uiso 1 1 calc R . . C11 C 0.5793(2) 0.8804(3) 0.24325(17) 0.0238(7) Uani 1 1 d . . . C12 C 0.5767(2) 0.8807(3) 0.31703(17) 0.0256(7) Uani 1 1 d . . . C13 C 0.4863(3) 0.8827(3) 0.34800(17) 0.0261(7) Uani 1 1 d . . . C14 C 0.4794(3) 0.8840(3) 0.42193(18) 0.0314(8) Uani 1 1 d . . . H14 H 0.5378 0.8837 0.4507 0.038 Uiso 1 1 calc R . . C15 C 0.3922(3) 0.8857(4) 0.45232(19) 0.0359(9) Uani 1 1 d . . . H15 H 0.3903 0.8849 0.5016 0.043 Uiso 1 1 calc R . . C16 C 0.3044(3) 0.8888(4) 0.41093(18) 0.0307(8) Uani 1 1 d . . . H16 H 0.2438 0.8913 0.4327 0.037 Uiso 1 1 calc R . . C17 C 0.3050(3) 0.8884(3) 0.33983(18) 0.0276(7) Uani 1 1 d . . . H17 H 0.2451 0.8894 0.3128 0.033 Uiso 1 1 calc R . . C18 C 0.3964(2) 0.8865(3) 0.30581(17) 0.0251(7) Uani 1 1 d . . . C19 C 0.3053(2) 0.8864(3) 0.18989(17) 0.0249(7) Uani 1 1 d . . . C20 C 0.2715(3) 0.7662(4) 0.15462(19) 0.0321(8) Uani 1 1 d . . . H20 H 0.3088 0.6819 0.1580 0.038 Uiso 1 1 calc R . . C21 C 0.1852(3) 0.7679(4) 0.1150(2) 0.0364(9) Uani 1 1 d . . . H21 H 0.1629 0.6852 0.0914 0.044 Uiso 1 1 calc R . . C22 C 0.1307(3) 0.8913(4) 0.10986(19) 0.0334(8) Uani 1 1 d U . . C23 C 0.1621(3) 1.0117(4) 0.1445(2) 0.0334(8) Uani 1 1 d . . . H23 H 0.1243 1.0955 0.1413 0.040 Uiso 1 1 calc R . . C24 C 0.2495(2) 1.0089(3) 0.18404(17) 0.0262(7) Uani 1 1 d . . . H24 H 0.2717 1.0919 0.2075 0.031 Uiso 1 1 calc R . . C25 C 0.6689(3) 0.8819(4) 0.36238(16) 0.0272(7) Uani 1 1 d . . . C26 C 0.7207(3) 1.0054(4) 0.37414(19) 0.0307(8) Uani 1 1 d . . . H26 H 0.7006 1.0889 0.3502 0.037 Uiso 1 1 calc R . . C27 C 0.8017(3) 1.0093(4) 0.4205(2) 0.0354(9) Uani 1 1 d . . . H27 H 0.8361 1.0951 0.4286 0.042 Uiso 1 1 calc R . . C28 C 0.8321(3) 0.8875(4) 0.45490(19) 0.0355(9) Uani 1 1 d . . . C29 C 0.7828(3) 0.7616(4) 0.4409(2) 0.0404(9) Uani 1 1 d . . . H29 H 0.8047 0.6769 0.4628 0.048 Uiso 1 1 calc R . . C30 C 0.7017(3) 0.7597(4) 0.3950(2) 0.0386(9) Uani 1 1 d . . . H30 H 0.6683 0.6735 0.3859 0.046 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 Cl1 0.0203(7) 0.0644(11) 0.0513(10) -0.0130(8) -0.0119(6) -0.0037(7) Cl2 0.0456(14) 0.0499(15) 0.0466(14) 0.0050(11) -0.0034(11) 0.0064(11) C1 0.0339(17) 0.0149(15) 0.0290(17) -0.0004(12) 0.0069(14) 0.0000(13) C2 0.0328(17) 0.0144(15) 0.0244(16) -0.0021(12) 0.0035(13) 0.0015(12) C3 0.0276(16) 0.0230(16) 0.0250(17) 0.0037(13) 0.0012(13) 0.0024(13) C4 0.0277(16) 0.0172(15) 0.0254(17) 0.0002(12) 0.0035(13) 0.0053(12) C5 0.0331(18) 0.0235(17) 0.0223(16) -0.0004(13) 0.0028(13) 0.0094(13) C6 0.0382(19) 0.0262(17) 0.0233(17) 0.0007(13) 0.0070(14) 0.0060(14) C7 0.0288(17) 0.0234(16) 0.0311(18) 0.0007(13) 0.0107(14) 0.0045(13) C8 0.0287(16) 0.0184(15) 0.0239(16) 0.0011(12) 0.0007(13) 0.0016(12) C9 0.0333(17) 0.0154(15) 0.0234(16) -0.0047(12) 0.0026(13) 0.0002(12) C10 0.0273(16) 0.0166(15) 0.0288(17) 0.0011(12) 0.0018(13) -0.0008(12) C11 0.0324(17) 0.0154(15) 0.0238(16) 0.0011(12) 0.0034(13) -0.0001(12) C12 0.0325(17) 0.0175(15) 0.0269(17) 0.0027(12) 0.0036(13) -0.0020(13) C13 0.0381(18) 0.0167(15) 0.0241(17) -0.0017(12) 0.0057(14) -0.0051(13) C14 0.044(2) 0.0251(17) 0.0244(17) -0.0005(13) 0.0007(15) -0.0145(15) C15 0.052(2) 0.034(2) 0.0223(17) -0.0025(14) 0.0120(16) -0.0129(17) C16 0.0393(19) 0.0251(17) 0.0288(18) 0.0015(14) 0.0137(15) -0.0027(14) C17 0.0345(18) 0.0200(16) 0.0294(18) 0.0004(13) 0.0114(14) -0.0034(13) C18 0.0348(18) 0.0143(15) 0.0264(17) 0.0008(12) 0.0037(14) -0.0048(13) C19 0.0280(16) 0.0221(16) 0.0257(16) -0.0020(13) 0.0127(13) -0.0047(13) C20 0.0340(18) 0.0237(17) 0.039(2) -0.0020(14) 0.0071(15) 0.0003(14) C21 0.041(2) 0.0300(19) 0.038(2) -0.0085(15) 0.0035(16) -0.0050(16) C22 0.0257(17) 0.041(2) 0.0342(19) -0.0016(16) 0.0051(14) -0.0002(15) C23 0.0306(18) 0.0294(18) 0.041(2) 0.0039(15) 0.0086(15) 0.0050(14) C24 0.0299(17) 0.0239(16) 0.0255(16) -0.0041(13) 0.0081(13) -0.0031(13) C25 0.0374(18) 0.0270(17) 0.0178(15) -0.0040(13) 0.0058(13) -0.0063(14) C26 0.0361(19) 0.0211(16) 0.0353(19) -0.0034(14) 0.0063(15) -0.0020(14) C27 0.039(2) 0.0283(18) 0.039(2) -0.0039(15) 0.0089(16) -0.0095(15) C28 0.041(2) 0.039(2) 0.0262(18) -0.0011(15) 0.0045(15) -0.0112(16) C29 0.056(2) 0.031(2) 0.033(2) 0.0033(15) -0.0110(17) -0.0065(17) C30 0.056(2) 0.0206(17) 0.038(2) 0.0062(15) -0.0094(18) -0.0089(16) _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 Cl1 C22 1.671(4) . ? Cl2 C28 1.600(5) . ? C1 C18 1.405(5) . ? C1 C2 1.418(5) . ? C1 C19 1.486(5) . ? C2 C3 1.414(5) . ? C2 C11 1.441(5) . ? C3 C4 1.389(5) . ? C3 H3 0.9500 . ? C4 C9 1.435(5) . ? C4 C5 1.440(5) . ? C5 C6 1.364(5) . ? C5 H5 0.9500 . ? C6 C7 1.422(5) . ? C6 H6 0.9500 . ? C7 C8 1.360(5) . ? C7 H7 0.9500 . ? C8 C9 1.438(5) . ? C8 H8 0.9500 . ? C9 C10 1.389(5) . ? C10 C11 1.407(5) . ? C10 H10 0.9500 . ? C11 C12 1.424(5) . ? C12 C13 1.402(5) . ? C12 C25 1.501(5) . ? C13 C14 1.432(5) . ? C13 C18 1.442(5) . ? C14 C15 1.357(5) . ? C14 H14 0.9500 . ? C15 C16 1.410(6) . ? C15 H15 0.9500 . ? C16 C17 1.370(5) . ? C16 H16 0.9500 . ? C17 C18 1.443(5) . ? C17 H17 0.9500 . ? C19 C24 1.393(5) . ? C19 C20 1.395(5) . ? C20 C21 1.376(5) . ? C20 H20 0.9500 . ? C21 C22 1.390(5) . ? C21 H21 0.9500 . ? C22 C23 1.381(5) . ? C23 C24 1.387(5) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C25 C26 1.383(5) . ? C25 C30 1.384(5) . ? C26 C27 1.391(5) . ? C26 H26 0.9500 . ? C27 C28 1.385(5) . ? C27 H27 0.9500 . ? C28 C29 1.393(5) . ? C29 C30 1.384(6) . ? C29 H29 0.9500 . ? C30 H30 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 C18 C1 C2 119.5(3) . . ? C18 C1 C19 120.0(3) . . ? C2 C1 C19 120.5(3) . . ? C3 C2 C1 121.2(3) . . ? C3 C2 C11 118.5(3) . . ? C1 C2 C11 120.3(3) . . ? C4 C3 C2 121.7(3) . . ? C4 C3 H3 119.1 . . ? C2 C3 H3 119.1 . . ? C3 C4 C9 119.6(3) . . ? C3 C4 C5 121.6(3) . . ? C9 C4 C5 118.8(3) . . ? C6 C5 C4 120.8(3) . . ? C6 C5 H5 119.6 . . ? C4 C5 H5 119.6 . . ? C5 C6 C7 120.3(3) . . ? C5 C6 H6 119.8 . . ? C7 C6 H6 119.8 . . ? C8 C7 C6 120.8(3) . . ? C8 C7 H7 119.6 . . ? C6 C7 H7 119.6 . . ? C7 C8 C9 121.1(3) . . ? C7 C8 H8 119.5 . . ? C9 C8 H8 119.5 . . ? C10 C9 C4 119.2(3) . . ? C10 C9 C8 122.6(3) . . ? C4 C9 C8 118.1(3) . . ? C9 C10 C11 121.9(3) . . ? C9 C10 H10 119.1 . . ? C11 C10 H10 119.1 . . ? C10 C11 C12 121.1(3) . . ? C10 C11 C2 119.1(3) . . ? C12 C11 C2 119.8(3) . . ? C13 C12 C11 119.5(3) . . ? C13 C12 C25 119.3(3) . . ? C11 C12 C25 121.2(3) . . ? C12 C13 C14 121.8(3) . . ? C12 C13 C18 120.6(3) . . ? C14 C13 C18 117.6(3) . . ? C15 C14 C13 122.2(3) . . ? C15 C14 H14 118.9 . . ? C13 C14 H14 118.9 . . ? C14 C15 C16 120.1(3) . . ? C14 C15 H15 120.0 . . ? C16 C15 H15 120.0 . . ? C17 C16 C15 121.2(3) . . ? C17 C16 H16 119.4 . . ? C15 C16 H16 119.4 . . ? C16 C17 C18 120.2(3) . . ? C16 C17 H17 119.9 . . ? C18 C17 H17 119.9 . . ? C1 C18 C13 120.3(3) . . ? C1 C18 C17 120.9(3) . . ? C13 C18 C17 118.8(3) . . ? C24 C19 C20 118.4(3) . . ? C24 C19 C1 120.8(3) . . ? C20 C19 C1 120.8(3) . . ? C21 C20 C19 121.1(3) . . ? C21 C20 H20 119.5 . . ? C19 C20 H20 119.5 . . ? C20 C21 C22 119.6(3) . . ? C20 C21 H21 120.2 . . ? C22 C21 H21 120.2 . . ? C23 C22 C21 120.6(3) . . ? C23 C22 Cl1 119.3(3) . . ? C21 C22 Cl1 120.1(3) . . ? C22 C23 C24 119.3(3) . . ? C22 C23 H23 120.3 . . ? C24 C23 H23 120.3 . . ? C23 C24 C19 121.0(3) . . ? C23 C24 H24 119.5 . . ? C19 C24 H24 119.5 . . ? C26 C25 C30 118.9(3) . . ? C26 C25 C12 120.8(3) . . ? C30 C25 C12 120.2(3) . . ? C25 C26 C27 120.9(3) . . ? C25 C26 H26 119.5 . . ? C27 C26 H26 119.5 . . ? C28 C27 C26 119.8(3) . . ? C28 C27 H27 120.1 . . ? C26 C27 H27 120.1 . . ? C27 C28 C29 119.4(4) . . ? C27 C28 Cl2 116.4(3) . . ? C29 C28 Cl2 124.0(3) . . ? C30 C29 C28 120.1(4) . . ? C30 C29 H29 120.0 . . ? C28 C29 H29 120.0 . . ? C29 C30 C25 120.8(3) . . ? C29 C30 H30 119.6 . . ? C25 C30 H30 119.6 . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.09 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.334 _refine_diff_density_min -0.295 _refine_diff_density_rms 0.071 data_mo_dm12096_0ma _database_code_depnum_ccdc_archive 'CCDC 892575' #TrackingRef 'mo_dm12096_0ma.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H24' _chemical_formula_weight 360.47 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 19.0506(16) _cell_length_b 9.9398(8) _cell_length_c 10.6781(9) _cell_angle_alpha 90.00 _cell_angle_beta 102.3300(10) _cell_angle_gamma 90.00 _cell_volume 1975.4(3) _cell_formula_units_Z 4 _cell_measurement_temperature 133(2) _cell_measurement_reflns_used 5314 _cell_measurement_theta_min 2.32 _cell_measurement_theta_max 30.41 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.212 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 768 _exptl_absorpt_coefficient_mu 0.068 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9765 _exptl_absorpt_correction_T_max 0.9878 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 133(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 APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 18988 _diffrn_reflns_av_R_equivalents 0.0275 _diffrn_reflns_av_sigmaI/netI 0.0299 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.19 _diffrn_reflns_theta_max 30.43 _reflns_number_total 5975 _reflns_number_gt 4413 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0681P)^2^+0.3100P] 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 5975 _refine_ls_number_parameters 255 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0656 _refine_ls_R_factor_gt 0.0437 _refine_ls_wR_factor_ref 0.1308 _refine_ls_wR_factor_gt 0.1177 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.039 _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 C1 C 0.21121(5) 0.65694(10) 0.73034(10) 0.02043(19) Uani 1 1 d . . . C2 C 0.19778(5) 0.54876(9) 0.64047(9) 0.01936(19) Uani 1 1 d . . . C3 C 0.13369(5) 0.53968(10) 0.54550(10) 0.0221(2) Uani 1 1 d . . . H3 H 0.0984 0.6079 0.5417 0.027 Uiso 1 1 calc R . . C4 C 0.12032(5) 0.43482(11) 0.45731(10) 0.0221(2) Uani 1 1 d . . . C5 C 0.05397(6) 0.42344(12) 0.36467(11) 0.0287(2) Uani 1 1 d . . . H5 H 0.0172 0.4884 0.3633 0.034 Uiso 1 1 calc R . . C6 C 0.04308(6) 0.32052(13) 0.27866(11) 0.0318(3) Uani 1 1 d . . . H6 H -0.0015 0.3140 0.2186 0.038 Uiso 1 1 calc R . . C7 C 0.09730(6) 0.22265(12) 0.27725(11) 0.0301(2) Uani 1 1 d . . . H7 H 0.0892 0.1528 0.2151 0.036 Uiso 1 1 calc R . . C8 C 0.16089(6) 0.22845(11) 0.36458(10) 0.0257(2) Uani 1 1 d . . . H8 H 0.1967 0.1623 0.3630 0.031 Uiso 1 1 calc R . . C9 C 0.17426(5) 0.33336(10) 0.45872(9) 0.0210(2) Uani 1 1 d . . . C10 C 0.23763(5) 0.34004(10) 0.55176(9) 0.02021(19) Uani 1 1 d . . . H10 H 0.2732 0.2728 0.5531 0.024 Uiso 1 1 calc R . . C11 C 0.25073(5) 0.44368(9) 0.64424(9) 0.01831(19) Uani 1 1 d . . . C12 C 0.31429(5) 0.44469(9) 0.74202(9) 0.01864(19) Uani 1 1 d . . . C13 C 0.32510(5) 0.54618(9) 0.83494(9) 0.01908(19) Uani 1 1 d . . . C14 C 0.38686(6) 0.54490(11) 0.93943(10) 0.0233(2) Uani 1 1 d . . . H14 H 0.4199 0.4723 0.9467 0.028 Uiso 1 1 calc R . . C15 C 0.39897(6) 0.64529(11) 1.02799(11) 0.0270(2) Uani 1 1 d . . . H15 H 0.4398 0.6416 1.0968 0.032 Uiso 1 1 calc R . . C16 C 0.35054(6) 0.75596(11) 1.01780(11) 0.0279(2) Uani 1 1 d . . . H16 H 0.3599 0.8267 1.0789 0.033 Uiso 1 1 calc R . . C17 C 0.29104(6) 0.76127(10) 0.92125(10) 0.0245(2) Uani 1 1 d . . . H17 H 0.2598 0.8365 0.9159 0.029 Uiso 1 1 calc R . . C18 C 0.27409(5) 0.65593(10) 0.82681(9) 0.0201(2) Uani 1 1 d . . . C19 C 0.15725(6) 0.77063(11) 0.71417(10) 0.0250(2) Uani 1 1 d . . . H19A H 0.1650 0.8238 0.7944 0.030 Uiso 1 1 calc R . . H19B H 0.1082 0.7324 0.6992 0.030 Uiso 1 1 calc R . . C20 C 0.16288(6) 0.86493(11) 0.60148(11) 0.0275(2) Uani 1 1 d . . . H20 H 0.1736 0.8080 0.5306 0.033 Uiso 1 1 calc R . . C21 C 0.09149(8) 0.93637(14) 0.55077(14) 0.0425(3) Uani 1 1 d . . . H21A H 0.0798 0.9936 0.6183 0.064 Uiso 1 1 calc R . . H21B H 0.0534 0.8694 0.5247 0.064 Uiso 1 1 calc R . . H21C H 0.0954 0.9920 0.4768 0.064 Uiso 1 1 calc R . . C22 C 0.22441(8) 0.96506(12) 0.64028(13) 0.0380(3) Uani 1 1 d . . . H22A H 0.2311 1.0150 0.5645 0.057 Uiso 1 1 calc R . . H22B H 0.2687 0.9164 0.6776 0.057 Uiso 1 1 calc R . . H22C H 0.2130 1.0281 0.7037 0.057 Uiso 1 1 calc R . . C23 C 0.36981(5) 0.33867(10) 0.74026(9) 0.02004(19) Uani 1 1 d . . . C24 C 0.37359(7) 0.22206(12) 0.81301(11) 0.0320(3) Uani 1 1 d . . . H24 H 0.3408 0.2088 0.8676 0.038 Uiso 1 1 calc R . . C25 C 0.42515(7) 0.12436(13) 0.80642(12) 0.0376(3) Uani 1 1 d . . . H25 H 0.4272 0.0447 0.8563 0.045 Uiso 1 1 calc R . . C26 C 0.47334(6) 0.14281(12) 0.72760(11) 0.0320(3) Uani 1 1 d . . . H26 H 0.5087 0.0763 0.7239 0.038 Uiso 1 1 calc R . . C27 C 0.46998(6) 0.25809(12) 0.65432(11) 0.0297(2) Uani 1 1 d . . . H27 H 0.5030 0.2711 0.6001 0.036 Uiso 1 1 calc R . . C28 C 0.41826(6) 0.35493(11) 0.66022(11) 0.0246(2) Uani 1 1 d . . . H28 H 0.4158 0.4336 0.6089 0.029 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 C1 0.0232(5) 0.0187(4) 0.0211(5) 0.0008(3) 0.0087(4) 0.0018(4) C2 0.0209(5) 0.0186(4) 0.0193(4) 0.0019(3) 0.0060(3) 0.0010(3) C3 0.0212(5) 0.0228(5) 0.0226(5) 0.0034(4) 0.0051(4) 0.0036(4) C4 0.0216(5) 0.0254(5) 0.0192(4) 0.0036(4) 0.0040(4) 0.0001(4) C5 0.0229(5) 0.0369(6) 0.0250(5) 0.0035(4) 0.0017(4) 0.0008(4) C6 0.0261(5) 0.0437(7) 0.0230(5) 0.0008(5) -0.0009(4) -0.0066(5) C7 0.0323(6) 0.0344(6) 0.0228(5) -0.0043(4) 0.0037(4) -0.0081(5) C8 0.0289(5) 0.0253(5) 0.0225(5) -0.0026(4) 0.0047(4) -0.0028(4) C9 0.0232(5) 0.0212(4) 0.0188(4) 0.0008(4) 0.0047(4) -0.0020(4) C10 0.0214(5) 0.0193(4) 0.0200(4) -0.0002(3) 0.0047(4) 0.0015(3) C11 0.0203(4) 0.0172(4) 0.0180(4) 0.0011(3) 0.0052(3) -0.0003(3) C12 0.0202(4) 0.0173(4) 0.0187(4) 0.0011(3) 0.0046(3) 0.0008(3) C13 0.0208(5) 0.0188(4) 0.0184(4) 0.0000(3) 0.0058(3) -0.0012(3) C14 0.0239(5) 0.0242(5) 0.0213(5) -0.0007(4) 0.0038(4) -0.0001(4) C15 0.0272(5) 0.0288(5) 0.0236(5) -0.0035(4) 0.0025(4) -0.0046(4) C16 0.0351(6) 0.0245(5) 0.0248(5) -0.0069(4) 0.0077(4) -0.0051(4) C17 0.0296(5) 0.0202(5) 0.0256(5) -0.0027(4) 0.0100(4) 0.0002(4) C18 0.0238(5) 0.0183(4) 0.0201(4) 0.0000(3) 0.0087(4) 0.0001(4) C19 0.0278(5) 0.0235(5) 0.0251(5) -0.0007(4) 0.0086(4) 0.0058(4) C20 0.0354(6) 0.0217(5) 0.0260(5) 0.0008(4) 0.0080(4) 0.0082(4) C21 0.0475(8) 0.0397(7) 0.0385(7) 0.0059(6) 0.0051(6) 0.0206(6) C22 0.0505(8) 0.0246(6) 0.0384(7) 0.0031(5) 0.0082(6) -0.0010(5) C23 0.0201(4) 0.0197(4) 0.0186(4) -0.0029(3) 0.0003(3) 0.0014(3) C24 0.0408(7) 0.0282(6) 0.0294(6) 0.0062(4) 0.0129(5) 0.0095(5) C25 0.0509(8) 0.0285(6) 0.0324(6) 0.0068(5) 0.0069(5) 0.0163(5) C26 0.0314(6) 0.0302(6) 0.0304(6) -0.0072(4) -0.0020(4) 0.0127(4) C27 0.0243(5) 0.0315(6) 0.0332(6) -0.0074(5) 0.0060(4) 0.0022(4) C28 0.0237(5) 0.0224(5) 0.0273(5) -0.0019(4) 0.0047(4) -0.0002(4) _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 C1 C18 1.4033(14) . ? C1 C2 1.4275(14) . ? C1 C19 1.5125(14) . ? C2 C3 1.4137(14) . ? C2 C11 1.4466(13) . ? C3 C4 1.3913(14) . ? C3 H3 0.9500 . ? C4 C5 1.4336(14) . ? C4 C9 1.4374(14) . ? C5 C6 1.3607(17) . ? C5 H5 0.9500 . ? C6 C7 1.4214(18) . ? C6 H6 0.9500 . ? C7 C8 1.3631(15) . ? C7 H7 0.9500 . ? C8 C9 1.4330(14) . ? C8 H8 0.9500 . ? C9 C10 1.3917(13) . ? C10 C11 1.4119(13) . ? C10 H10 0.9500 . ? C11 C12 1.4201(13) . ? C12 C13 1.3990(13) . ? C12 C23 1.4960(13) . ? C13 C14 1.4382(14) . ? C13 C18 1.4513(13) . ? C14 C15 1.3601(15) . ? C14 H14 0.9500 . ? C15 C16 1.4249(16) . ? C15 H15 0.9500 . ? C16 C17 1.3607(15) . ? C16 H16 0.9500 . ? C17 C18 1.4417(14) . ? C17 H17 0.9500 . ? C19 C20 1.5470(15) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 C22 1.5261(17) . ? C20 C21 1.5273(16) . ? C20 H20 1.0000 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 C24 1.3886(15) . ? C23 C28 1.3948(15) . ? C24 C25 1.3937(16) . ? C24 H24 0.9500 . ? C25 C26 1.3836(19) . ? C25 H25 0.9500 . ? C26 C27 1.3812(17) . ? C26 H26 0.9500 . ? C27 C28 1.3885(15) . ? C27 H27 0.9500 . ? C28 H28 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 C18 C1 C2 119.37(9) . . ? C18 C1 C19 122.82(9) . . ? C2 C1 C19 117.79(9) . . ? C3 C2 C1 122.25(9) . . ? C3 C2 C11 117.66(9) . . ? C1 C2 C11 120.09(9) . . ? C4 C3 C2 122.59(9) . . ? C4 C3 H3 118.7 . . ? C2 C3 H3 118.7 . . ? C3 C4 C5 122.22(10) . . ? C3 C4 C9 119.43(9) . . ? C5 C4 C9 118.35(9) . . ? C6 C5 C4 120.65(10) . . ? C6 C5 H5 119.7 . . ? C4 C5 H5 119.7 . . ? C5 C6 C7 121.02(10) . . ? C5 C6 H6 119.5 . . ? C7 C6 H6 119.5 . . ? C8 C7 C6 120.36(10) . . ? C8 C7 H7 119.8 . . ? C6 C7 H7 119.8 . . ? C7 C8 C9 120.64(10) . . ? C7 C8 H8 119.7 . . ? C9 C8 H8 119.7 . . ? C10 C9 C8 122.18(9) . . ? C10 C9 C4 118.90(9) . . ? C8 C9 C4 118.92(9) . . ? C9 C10 C11 122.06(9) . . ? C9 C10 H10 119.0 . . ? C11 C10 H10 119.0 . . ? C10 C11 C12 121.00(9) . . ? C10 C11 C2 119.30(9) . . ? C12 C11 C2 119.69(9) . . ? C13 C12 C11 119.99(9) . . ? C13 C12 C23 121.29(8) . . ? C11 C12 C23 118.68(8) . . ? C12 C13 C14 121.07(9) . . ? C12 C13 C18 120.28(9) . . ? C14 C13 C18 118.65(9) . . ? C15 C14 C13 121.47(10) . . ? C15 C14 H14 119.3 . . ? C13 C14 H14 119.3 . . ? C14 C15 C16 120.15(10) . . ? C14 C15 H15 119.9 . . ? C16 C15 H15 119.9 . . ? C17 C16 C15 120.59(10) . . ? C17 C16 H16 119.7 . . ? C15 C16 H16 119.7 . . ? C16 C17 C18 121.85(10) . . ? C16 C17 H17 119.1 . . ? C18 C17 H17 119.1 . . ? C1 C18 C17 122.47(9) . . ? C1 C18 C13 120.34(9) . . ? C17 C18 C13 117.19(9) . . ? C1 C19 C20 112.53(9) . . ? C1 C19 H19A 109.1 . . ? C20 C19 H19A 109.1 . . ? C1 C19 H19B 109.1 . . ? C20 C19 H19B 109.1 . . ? H19A C19 H19B 107.8 . . ? C22 C20 C21 111.55(10) . . ? C22 C20 C19 111.15(10) . . ? C21 C20 C19 110.68(10) . . ? C22 C20 H20 107.8 . . ? C21 C20 H20 107.8 . . ? C19 C20 H20 107.8 . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C20 C22 H22A 109.5 . . ? C20 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C20 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C24 C23 C28 118.52(9) . . ? C24 C23 C12 122.23(9) . . ? C28 C23 C12 119.22(9) . . ? C23 C24 C25 120.42(11) . . ? C23 C24 H24 119.8 . . ? C25 C24 H24 119.8 . . ? C26 C25 C24 120.31(11) . . ? C26 C25 H25 119.8 . . ? C24 C25 H25 119.8 . . ? C27 C26 C25 119.87(10) . . ? C27 C26 H26 120.1 . . ? C25 C26 H26 120.1 . . ? C26 C27 C28 119.79(11) . . ? C26 C27 H27 120.1 . . ? C28 C27 H27 120.1 . . ? C27 C28 C23 121.09(10) . . ? C27 C28 H28 119.5 . . ? C23 C28 H28 119.5 . . ? 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 C18 C1 C2 C3 176.37(9) . . . . ? C19 C1 C2 C3 -5.44(14) . . . . ? C18 C1 C2 C11 -3.83(14) . . . . ? C19 C1 C2 C11 174.35(9) . . . . ? C1 C2 C3 C4 179.77(9) . . . . ? C11 C2 C3 C4 -0.02(14) . . . . ? C2 C3 C4 C5 177.40(10) . . . . ? C2 C3 C4 C9 -2.18(15) . . . . ? C3 C4 C5 C6 179.10(11) . . . . ? C9 C4 C5 C6 -1.32(16) . . . . ? C4 C5 C6 C7 -0.75(18) . . . . ? C5 C6 C7 C8 1.59(18) . . . . ? C6 C7 C8 C9 -0.27(17) . . . . ? C7 C8 C9 C10 177.99(10) . . . . ? C7 C8 C9 C4 -1.79(15) . . . . ? C3 C4 C9 C10 2.36(14) . . . . ? C5 C4 C9 C10 -177.23(9) . . . . ? C3 C4 C9 C8 -177.85(9) . . . . ? C5 C4 C9 C8 2.55(14) . . . . ? C8 C9 C10 C11 179.87(9) . . . . ? C4 C9 C10 C11 -0.35(15) . . . . ? C9 C10 C11 C12 176.91(9) . . . . ? C9 C10 C11 C2 -1.86(15) . . . . ? C3 C2 C11 C10 2.03(14) . . . . ? C1 C2 C11 C10 -177.77(9) . . . . ? C3 C2 C11 C12 -176.75(9) . . . . ? C1 C2 C11 C12 3.45(14) . . . . ? C10 C11 C12 C13 -178.06(9) . . . . ? C2 C11 C12 C13 0.70(14) . . . . ? C10 C11 C12 C23 4.09(14) . . . . ? C2 C11 C12 C23 -177.15(9) . . . . ? C11 C12 C13 C14 176.15(9) . . . . ? C23 C12 C13 C14 -6.05(14) . . . . ? C11 C12 C13 C18 -4.37(14) . . . . ? C23 C12 C13 C18 173.42(9) . . . . ? C12 C13 C14 C15 177.95(10) . . . . ? C18 C13 C14 C15 -1.54(15) . . . . ? C13 C14 C15 C16 -0.84(16) . . . . ? C14 C15 C16 C17 1.34(17) . . . . ? C15 C16 C17 C18 0.61(17) . . . . ? C2 C1 C18 C17 -179.65(9) . . . . ? C19 C1 C18 C17 2.26(15) . . . . ? C2 C1 C18 C13 0.18(14) . . . . ? C19 C1 C18 C13 -177.91(9) . . . . ? C16 C17 C18 C1 176.92(10) . . . . ? C16 C17 C18 C13 -2.92(15) . . . . ? C12 C13 C18 C1 3.98(14) . . . . ? C14 C13 C18 C1 -176.53(9) . . . . ? C12 C13 C18 C17 -176.18(9) . . . . ? C14 C13 C18 C17 3.31(14) . . . . ? C18 C1 C19 C20 103.22(11) . . . . ? C2 C1 C19 C20 -74.90(12) . . . . ? C1 C19 C20 C22 -80.24(11) . . . . ? C1 C19 C20 C21 155.22(10) . . . . ? C13 C12 C23 C24 85.70(13) . . . . ? C11 C12 C23 C24 -96.47(12) . . . . ? C13 C12 C23 C28 -96.23(12) . . . . ? C11 C12 C23 C28 81.59(12) . . . . ? C28 C23 C24 C25 0.48(17) . . . . ? C12 C23 C24 C25 178.56(11) . . . . ? C23 C24 C25 C26 0.24(19) . . . . ? C24 C25 C26 C27 -0.51(19) . . . . ? C25 C26 C27 C28 0.03(17) . . . . ? C26 C27 C28 C23 0.71(16) . . . . ? C24 C23 C28 C27 -0.96(15) . . . . ? C12 C23 C28 C27 -179.10(9) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 30.43 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.372 _refine_diff_density_min -0.172 _refine_diff_density_rms 0.043