# Electronic Supplementary Material (ESI) for Medicinal Chemistry 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_asch85 _database_code_depnum_ccdc_archive 'CCDC 871295' #TrackingRef 'asch85.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C29 H32 Cr O5' _chemical_formula_sum 'C29 H32 Cr O5' _chemical_formula_weight 512.55 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cr Cr 0.3209 0.6236 '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 P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.8549(10) _cell_length_b 15.641(2) _cell_length_c 16.5024(10) _cell_angle_alpha 90.00 _cell_angle_beta 100.507(6) _cell_angle_gamma 90.00 _cell_volume 2501.0(4) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 11711 _cell_measurement_theta_min 1.81 _cell_measurement_theta_max 27.00 _exptl_crystal_description platelet _exptl_crystal_colour yellow _exptl_crystal_size_max .25 _exptl_crystal_size_mid .25 _exptl_crystal_size_min .07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.361 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1080 _exptl_absorpt_coefficient_mu 0.495 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'Nonius KappaCCD' _diffrn_measurement_method Phi/Omega-Scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11711 _diffrn_reflns_av_R_equivalents 0.0609 _diffrn_reflns_av_sigmaI/netI 0.0928 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.81 _diffrn_reflns_theta_max 27.00 _reflns_number_total 5420 _reflns_number_gt 3388 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius COLLECT' _computing_cell_refinement 'Nonius DENZO (Otwinowski, Minor 1997)' _computing_data_reduction 'Nonius DENZO (Otwinowski, Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SCHAKAL99 (E. Keller 1999)' _computing_publication_material 'PLATON (A. L. Spek 1980-2004)' _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^)+(0.0489P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5420 _refine_ls_number_parameters 319 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0970 _refine_ls_R_factor_gt 0.0497 _refine_ls_wR_factor_ref 0.1167 _refine_ls_wR_factor_gt 0.1018 _refine_ls_goodness_of_fit_ref 0.984 _refine_ls_restrained_S_all 0.984 _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 Cr1 Cr 0.06065(4) 0.18162(3) -0.00321(2) 0.01948(13) Uani 1 1 d . . . O1 O 0.2041(2) 0.01864(14) 0.05740(11) 0.0341(5) Uani 1 1 d . . . O2 O -0.0266(2) 0.10711(13) -0.17196(11) 0.0322(5) Uani 1 1 d . . . O3 O 0.33016(19) 0.22256(13) -0.05482(11) 0.0294(5) Uani 1 1 d . . . O4 O -0.23555(18) 0.26610(13) -0.09803(10) 0.0255(4) Uani 1 1 d . . . O5 O 0.20733(18) 0.39971(12) 0.00875(10) 0.0238(4) Uani 1 1 d . . . C1 C 0.1457(3) 0.0810(2) 0.03344(16) 0.0250(6) Uani 1 1 d . . . C2 C 0.0076(3) 0.13517(19) -0.10593(17) 0.0248(6) Uani 1 1 d . . . C3 C 0.2248(3) 0.20970(18) -0.03431(15) 0.0230(6) Uani 1 1 d . . . C4 C -0.1438(3) 0.25290(18) -0.02635(15) 0.0209(6) Uani 1 1 d . . . C5 C -0.3451(3) 0.2051(2) -0.11853(17) 0.0324(7) Uani 1 1 d . . . H5A H -0.3060 0.1481 -0.1232 0.049 Uiso 1 1 calc R . . H5B H -0.4030 0.2209 -0.1712 0.049 Uiso 1 1 calc R . . H5C H -0.4013 0.2047 -0.0752 0.049 Uiso 1 1 calc R . . C6 C -0.0355(3) 0.31146(18) -0.00971(15) 0.0211(6) Uani 1 1 d . . . H6 H -0.0274 0.3557 -0.0480 0.025 Uiso 1 1 calc R . . C7 C 0.0629(3) 0.30493(16) 0.06475(15) 0.0186(6) Uani 1 1 d . . . C8 C 0.0550(3) 0.23720(17) 0.12074(14) 0.0192(6) Uani 1 1 d . . . C9 C -0.0545(3) 0.17737(18) 0.10197(15) 0.0205(6) Uani 1 1 d . . . C10 C -0.1511(3) 0.18343(18) 0.02711(14) 0.0201(6) Uani 1 1 d . . . H10 H -0.2204 0.1410 0.0131 0.024 Uiso 1 1 calc R . . C11 C -0.0782(3) 0.10729(18) 0.16231(15) 0.0217(6) Uani 1 1 d . . . H11 H -0.0959 0.0523 0.1312 0.026 Uiso 1 1 calc R . . C12 C 0.0468(3) 0.09485(19) 0.23157(15) 0.0268(7) Uani 1 1 d . . . H12A H 0.0187 0.0616 0.2768 0.032 Uiso 1 1 calc R . . H12B H 0.1187 0.0619 0.2104 0.032 Uiso 1 1 calc R . . C13 C 0.1063(3) 0.18042(19) 0.26487(15) 0.0259(6) Uani 1 1 d . . . H13A H 0.0328 0.2160 0.2815 0.031 Uiso 1 1 calc R . . H13B H 0.1792 0.1712 0.3139 0.031 Uiso 1 1 calc R . . C14 C 0.1661(3) 0.22555(18) 0.19813(15) 0.0227(6) Uani 1 1 d . . . H14 H 0.2370 0.1862 0.1825 0.027 Uiso 1 1 calc R . . C15 C 0.2399(3) 0.30898(19) 0.22505(15) 0.0271(7) Uani 1 1 d . . . H15A H 0.3203 0.2975 0.2691 0.032 Uiso 1 1 calc R . . H15B H 0.1765 0.3478 0.2475 0.032 Uiso 1 1 calc R . . C16 C 0.2884(3) 0.35180(19) 0.15186(16) 0.0269(6) Uani 1 1 d . . . H16A H 0.3481 0.3118 0.1279 0.032 Uiso 1 1 calc R . . H16B H 0.3437 0.4031 0.1712 0.032 Uiso 1 1 calc R . . C17 C 0.1654(3) 0.37779(18) 0.08552(15) 0.0207(6) Uani 1 1 d . . . C18 C 0.3125(3) 0.4637(2) 0.01457(16) 0.0400(9) Uani 1 1 d . . . H18A H 0.3979 0.4436 0.0507 0.048 Uiso 1 1 calc R . . H18B H 0.2818 0.5169 0.0384 0.048 Uiso 1 1 calc R . . C19 C 0.3392(3) 0.4805(2) -0.07042(16) 0.0306(7) Uani 1 1 d . . . C20 C 0.2929(3) 0.5550(2) -0.11196(17) 0.0361(8) Uani 1 1 d . . . H20 H 0.2442 0.5961 -0.0861 0.043 Uiso 1 1 calc R . . C21 C 0.3171(3) 0.5701(2) -0.19080(18) 0.0418(9) Uani 1 1 d . . . H21 H 0.2837 0.6211 -0.2189 0.050 Uiso 1 1 calc R . . C22 C 0.3891(3) 0.5118(2) -0.22853(18) 0.0404(9) Uani 1 1 d . . . H22 H 0.4062 0.5225 -0.2824 0.049 Uiso 1 1 calc R . . C23 C 0.4363(3) 0.4376(2) -0.18792(18) 0.0410(9) Uani 1 1 d . . . H23 H 0.4856 0.3971 -0.2141 0.049 Uiso 1 1 calc R . . C24 C 0.4124(3) 0.4217(2) -0.10888(17) 0.0347(8) Uani 1 1 d . . . H24 H 0.4461 0.3706 -0.0811 0.042 Uiso 1 1 calc R . . C25 C 0.0867(3) 0.45275(18) 0.11472(16) 0.0265(6) Uani 1 1 d . . . H25A H 0.1501 0.5007 0.1303 0.040 Uiso 1 1 calc R . . H25B H 0.0474 0.4350 0.1625 0.040 Uiso 1 1 calc R . . H25C H 0.0123 0.4705 0.0701 0.040 Uiso 1 1 calc R . . C26 C -0.2089(3) 0.1302(2) 0.19822(16) 0.0289(7) Uani 1 1 d . . . H26A H -0.2043 0.0990 0.2508 0.035 Uiso 1 1 calc R . . H26B H -0.2056 0.1921 0.2112 0.035 Uiso 1 1 calc R . . C27 C -0.3457(3) 0.1113(2) 0.14477(16) 0.0349(8) Uani 1 1 d . . . C28 C -0.4385(3) 0.1728(3) 0.12256(19) 0.0530(10) Uani 1 1 d . . . H28A H -0.5259 0.1593 0.0903 0.064 Uiso 1 1 calc R . . H28B H -0.4172 0.2302 0.1390 0.064 Uiso 1 1 calc R . . C29 C -0.3740(3) 0.0199(3) 0.1206(2) 0.0532(10) Uani 1 1 d . . . H29A H -0.4700 0.0140 0.0924 0.080 Uiso 1 1 calc R . . H29B H -0.3582 -0.0161 0.1700 0.080 Uiso 1 1 calc R . . H29C H -0.3121 0.0020 0.0835 0.080 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 Cr1 0.0218(2) 0.0162(2) 0.0211(2) -0.00137(19) 0.00566(16) -0.0008(2) O1 0.0418(13) 0.0239(13) 0.0373(12) 0.0022(10) 0.0094(9) 0.0075(10) O2 0.0406(13) 0.0295(13) 0.0266(11) -0.0073(9) 0.0067(9) -0.0044(10) O3 0.0239(11) 0.0320(13) 0.0343(11) -0.0001(9) 0.0107(9) -0.0008(9) O4 0.0214(10) 0.0275(12) 0.0255(10) 0.0033(9) -0.0017(8) -0.0026(9) O5 0.0279(11) 0.0223(12) 0.0223(9) -0.0022(8) 0.0078(8) -0.0082(9) C1 0.0292(16) 0.0234(18) 0.0243(14) -0.0034(13) 0.0097(12) -0.0026(13) C2 0.0223(15) 0.0221(17) 0.0315(16) 0.0003(13) 0.0085(12) 0.0016(12) C3 0.0311(17) 0.0190(16) 0.0176(13) -0.0009(11) 0.0006(12) 0.0020(12) C4 0.0232(14) 0.0199(16) 0.0200(13) -0.0021(11) 0.0049(11) 0.0046(12) C5 0.0237(16) 0.041(2) 0.0299(16) -0.0012(14) -0.0016(12) -0.0062(14) C6 0.0246(15) 0.0192(16) 0.0200(13) 0.0038(11) 0.0053(11) 0.0023(12) C7 0.0217(14) 0.0141(16) 0.0214(13) -0.0044(11) 0.0074(10) 0.0006(11) C8 0.0208(14) 0.0173(15) 0.0198(13) -0.0014(11) 0.0045(10) 0.0031(11) C9 0.0231(14) 0.0170(15) 0.0227(13) 0.0006(12) 0.0078(11) 0.0021(12) C10 0.0207(14) 0.0184(15) 0.0228(13) -0.0017(12) 0.0084(11) 0.0001(12) C11 0.0247(15) 0.0167(16) 0.0240(14) 0.0021(11) 0.0054(11) 0.0009(12) C12 0.0282(16) 0.0284(18) 0.0237(14) 0.0077(13) 0.0040(12) 0.0048(13) C13 0.0287(15) 0.0265(17) 0.0217(13) 0.0054(13) 0.0026(11) 0.0044(13) C14 0.0225(15) 0.0229(17) 0.0225(14) -0.0004(12) 0.0031(11) 0.0022(12) C15 0.0265(15) 0.0311(18) 0.0215(14) -0.0016(13) -0.0012(11) -0.0017(13) C16 0.0257(15) 0.0263(17) 0.0282(14) -0.0036(13) 0.0035(12) -0.0031(13) C17 0.0242(15) 0.0161(15) 0.0226(13) -0.0009(11) 0.0066(11) -0.0034(12) C18 0.046(2) 0.044(2) 0.0310(16) -0.0073(15) 0.0111(14) -0.0291(17) C19 0.0287(16) 0.035(2) 0.0279(15) -0.0038(14) 0.0045(12) -0.0155(14) C20 0.0243(17) 0.045(2) 0.0411(18) -0.0060(16) 0.0114(13) -0.0099(15) C21 0.0316(18) 0.050(2) 0.0422(19) 0.0092(17) 0.0022(15) -0.0062(17) C22 0.0374(19) 0.055(3) 0.0301(17) 0.0002(16) 0.0103(14) -0.0173(18) C23 0.0375(19) 0.049(2) 0.0391(18) -0.0180(17) 0.0132(15) -0.0167(17) C24 0.0390(19) 0.0292(19) 0.0354(17) -0.0020(14) 0.0058(14) -0.0126(15) C25 0.0350(17) 0.0171(16) 0.0292(15) -0.0035(12) 0.0103(12) -0.0028(13) C26 0.0297(17) 0.0321(19) 0.0268(15) 0.0065(13) 0.0102(12) 0.0044(14) C27 0.0287(17) 0.052(2) 0.0260(15) 0.0060(15) 0.0111(13) 0.0004(16) C28 0.034(2) 0.081(3) 0.045(2) 0.016(2) 0.0092(15) 0.011(2) C29 0.036(2) 0.072(3) 0.056(2) -0.017(2) 0.0188(16) -0.0202(19) _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 Cr1 C2 1.831(3) . ? Cr1 C1 1.833(3) . ? Cr1 C3 1.838(3) . ? Cr1 C7 2.229(3) . ? Cr1 C8 2.232(2) . ? Cr1 C10 2.233(2) . ? Cr1 C6 2.235(3) . ? Cr1 C9 2.241(2) . ? Cr1 C4 2.273(3) . ? O1 C1 1.164(3) . ? O2 C2 1.166(3) . ? O3 C3 1.166(3) . ? O4 C4 1.367(3) . ? O4 C5 1.434(3) . ? O5 C18 1.431(3) . ? O5 C17 1.444(3) . ? C4 C6 1.395(4) . ? C4 C10 1.410(4) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 C7 1.423(3) . ? C6 H6 0.9500 . ? C7 C8 1.417(4) . ? C7 C17 1.520(4) . ? C8 C9 1.419(4) . ? C8 C14 1.534(3) . ? C9 C10 1.419(3) . ? C9 C11 1.527(4) . ? C10 H10 0.9500 . ? C11 C12 1.532(3) . ? C11 C26 1.555(4) . ? C11 H11 1.0000 . ? C12 C13 1.523(4) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.515(4) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.520(4) . ? C14 H14 1.0000 . ? C15 C16 1.532(4) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.533(4) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C25 1.531(4) . ? C18 C19 1.497(4) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.387(4) . ? C19 C24 1.392(4) . ? C20 C21 1.385(4) . ? C20 H20 0.9500 . ? C21 C22 1.373(4) . ? C21 H21 0.9500 . ? C22 C23 1.377(5) . ? C22 H22 0.9500 . ? C23 C24 1.390(4) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 C27 1.500(4) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 C28 1.332(5) . ? C27 C29 1.496(5) . ? C28 H28A 0.9500 . ? C28 H28B 0.9500 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 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 C2 Cr1 C1 90.05(12) . . ? C2 Cr1 C3 87.34(11) . . ? C1 Cr1 C3 85.67(12) . . ? C2 Cr1 C7 141.65(11) . . ? C1 Cr1 C7 127.95(11) . . ? C3 Cr1 C7 90.31(11) . . ? C2 Cr1 C8 162.24(11) . . ? C1 Cr1 C8 96.79(11) . . ? C3 Cr1 C8 109.45(11) . . ? C7 Cr1 C8 37.03(9) . . ? C2 Cr1 C10 95.27(11) . . ? C1 Cr1 C10 109.06(11) . . ? C3 Cr1 C10 164.99(12) . . ? C7 Cr1 C10 78.47(10) . . ? C8 Cr1 C10 67.01(9) . . ? C2 Cr1 C6 105.62(11) . . ? C1 Cr1 C6 163.77(10) . . ? C3 Cr1 C6 99.01(11) . . ? C7 Cr1 C6 37.18(9) . . ? C8 Cr1 C6 66.99(9) . . ? C10 Cr1 C6 66.04(10) . . ? C2 Cr1 C9 127.30(11) . . ? C1 Cr1 C9 89.11(10) . . ? C3 Cr1 C9 145.01(11) . . ? C7 Cr1 C9 66.16(9) . . ? C8 Cr1 C9 36.99(9) . . ? C10 Cr1 C9 36.97(9) . . ? C6 Cr1 C9 78.11(9) . . ? C2 Cr1 C4 86.82(11) . . ? C1 Cr1 C4 144.52(11) . . ? C3 Cr1 C4 129.38(11) . . ? C7 Cr1 C4 65.62(10) . . ? C8 Cr1 C4 78.09(9) . . ? C10 Cr1 C4 36.45(9) . . ? C6 Cr1 C4 36.04(9) . . ? C9 Cr1 C4 65.56(9) . . ? C4 O4 C5 117.0(2) . . ? C18 O5 C17 115.26(19) . . ? O1 C1 Cr1 177.6(3) . . ? O2 C2 Cr1 178.7(3) . . ? O3 C3 Cr1 176.1(3) . . ? O4 C4 C6 115.6(2) . . ? O4 C4 C10 123.8(2) . . ? C6 C4 C10 120.5(2) . . ? O4 C4 Cr1 130.21(16) . . ? C6 C4 Cr1 70.51(15) . . ? C10 C4 Cr1 70.25(15) . . ? O4 C5 H5A 109.5 . . ? O4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? O4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C4 C6 C7 119.9(2) . . ? C4 C6 Cr1 73.45(16) . . ? C7 C6 Cr1 71.18(15) . . ? C4 C6 H6 120.0 . . ? C7 C6 H6 120.0 . . ? Cr1 C6 H6 127.4 . . ? C8 C7 C6 120.5(2) . . ? C8 C7 C17 121.8(2) . . ? C6 C7 C17 117.4(2) . . ? C8 C7 Cr1 71.61(15) . . ? C6 C7 Cr1 71.65(15) . . ? C17 C7 Cr1 135.01(17) . . ? C7 C8 C9 118.7(2) . . ? C7 C8 C14 121.1(2) . . ? C9 C8 C14 120.1(2) . . ? C7 C8 Cr1 71.35(14) . . ? C9 C8 Cr1 71.84(14) . . ? C14 C8 Cr1 125.70(17) . . ? C10 C9 C8 120.6(2) . . ? C10 C9 C11 117.2(2) . . ? C8 C9 C11 122.1(2) . . ? C10 C9 Cr1 71.21(13) . . ? C8 C9 Cr1 71.17(13) . . ? C11 C9 Cr1 133.27(18) . . ? C4 C10 C9 119.6(2) . . ? C4 C10 Cr1 73.30(14) . . ? C9 C10 Cr1 71.82(14) . . ? C4 C10 H10 120.2 . . ? C9 C10 H10 120.2 . . ? Cr1 C10 H10 126.5 . . ? C9 C11 C12 112.3(2) . . ? C9 C11 C26 108.6(2) . . ? C12 C11 C26 110.7(2) . . ? C9 C11 H11 108.4 . . ? C12 C11 H11 108.4 . . ? C26 C11 H11 108.4 . . ? C13 C12 C11 111.2(2) . . ? C13 C12 H12A 109.4 . . ? C11 C12 H12A 109.4 . . ? C13 C12 H12B 109.4 . . ? C11 C12 H12B 109.4 . . ? H12A C12 H12B 108.0 . . ? C14 C13 C12 108.8(2) . . ? C14 C13 H13A 109.9 . . ? C12 C13 H13A 109.9 . . ? C14 C13 H13B 109.9 . . ? C12 C13 H13B 109.9 . . ? H13A C13 H13B 108.3 . . ? C13 C14 C15 114.6(2) . . ? C13 C14 C8 110.3(2) . . ? C15 C14 C8 111.8(2) . . ? C13 C14 H14 106.5 . . ? C15 C14 H14 106.5 . . ? C8 C14 H14 106.5 . . ? C14 C15 C16 110.3(2) . . ? C14 C15 H15A 109.6 . . ? C16 C15 H15A 109.6 . . ? C14 C15 H15B 109.6 . . ? C16 C15 H15B 109.6 . . ? H15A C15 H15B 108.1 . . ? C15 C16 C17 111.0(2) . . ? C15 C16 H16A 109.4 . . ? C17 C16 H16A 109.4 . . ? C15 C16 H16B 109.4 . . ? C17 C16 H16B 109.4 . . ? H16A C16 H16B 108.0 . . ? O5 C17 C7 105.37(19) . . ? O5 C17 C25 109.7(2) . . ? C7 C17 C25 106.9(2) . . ? O5 C17 C16 112.0(2) . . ? C7 C17 C16 111.6(2) . . ? C25 C17 C16 111.0(2) . . ? O5 C18 C19 108.0(2) . . ? O5 C18 H18A 110.1 . . ? C19 C18 H18A 110.1 . . ? O5 C18 H18B 110.1 . . ? C19 C18 H18B 110.1 . . ? H18A C18 H18B 108.4 . . ? C20 C19 C24 118.8(3) . . ? C20 C19 C18 120.8(3) . . ? C24 C19 C18 120.4(3) . . ? C21 C20 C19 120.7(3) . . ? C21 C20 H20 119.6 . . ? C19 C20 H20 119.6 . . ? C22 C21 C20 120.3(3) . . ? C22 C21 H21 119.9 . . ? C20 C21 H21 119.9 . . ? C21 C22 C23 119.7(3) . . ? C21 C22 H22 120.1 . . ? C23 C22 H22 120.1 . . ? C22 C23 C24 120.5(3) . . ? C22 C23 H23 119.7 . . ? C24 C23 H23 119.7 . . ? C23 C24 C19 120.0(3) . . ? C23 C24 H24 120.0 . . ? C19 C24 H24 120.0 . . ? C17 C25 H25A 109.5 . . ? C17 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C17 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C27 C26 C11 116.6(2) . . ? C27 C26 H26A 108.1 . . ? C11 C26 H26A 108.1 . . ? C27 C26 H26B 108.1 . . ? C11 C26 H26B 108.1 . . ? H26A C26 H26B 107.3 . . ? C28 C27 C29 122.1(3) . . ? C28 C27 C26 121.1(3) . . ? C29 C27 C26 116.7(3) . . ? C27 C28 H28A 120.0 . . ? C27 C28 H28B 120.0 . . ? H28A C28 H28B 120.0 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? 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 C2 Cr1 C1 O1 120(5) . . . . ? C3 Cr1 C1 O1 33(5) . . . . ? C7 Cr1 C1 O1 -55(5) . . . . ? C8 Cr1 C1 O1 -77(5) . . . . ? C10 Cr1 C1 O1 -145(5) . . . . ? C6 Cr1 C1 O1 -75(5) . . . . ? C9 Cr1 C1 O1 -113(5) . . . . ? C4 Cr1 C1 O1 -156(5) . . . . ? C1 Cr1 C2 O2 -163(11) . . . . ? C3 Cr1 C2 O2 -77(11) . . . . ? C7 Cr1 C2 O2 10(11) . . . . ? C8 Cr1 C2 O2 84(11) . . . . ? C10 Cr1 C2 O2 88(11) . . . . ? C6 Cr1 C2 O2 22(11) . . . . ? C9 Cr1 C2 O2 108(11) . . . . ? C4 Cr1 C2 O2 53(11) . . . . ? C2 Cr1 C3 O3 -59(3) . . . . ? C1 Cr1 C3 O3 31(3) . . . . ? C7 Cr1 C3 O3 159(3) . . . . ? C8 Cr1 C3 O3 127(3) . . . . ? C10 Cr1 C3 O3 -160(3) . . . . ? C6 Cr1 C3 O3 -164(3) . . . . ? C9 Cr1 C3 O3 113(3) . . . . ? C4 Cr1 C3 O3 -143(3) . . . . ? C5 O4 C4 C6 177.7(2) . . . . ? C5 O4 C4 C10 0.3(3) . . . . ? C5 O4 C4 Cr1 92.2(3) . . . . ? C2 Cr1 C4 O4 -14.8(2) . . . . ? C1 Cr1 C4 O4 -100.4(3) . . . . ? C3 Cr1 C4 O4 69.2(3) . . . . ? C7 Cr1 C4 O4 137.8(3) . . . . ? C8 Cr1 C4 O4 174.7(3) . . . . ? C10 Cr1 C4 O4 -118.1(3) . . . . ? C6 Cr1 C4 O4 107.6(3) . . . . ? C9 Cr1 C4 O4 -148.5(3) . . . . ? C2 Cr1 C4 C6 -122.33(16) . . . . ? C1 Cr1 C4 C6 152.06(18) . . . . ? C3 Cr1 C4 C6 -38.40(19) . . . . ? C7 Cr1 C4 C6 30.24(13) . . . . ? C8 Cr1 C4 C6 67.10(15) . . . . ? C10 Cr1 C4 C6 134.4(2) . . . . ? C9 Cr1 C4 C6 103.90(16) . . . . ? C2 Cr1 C4 C10 103.30(17) . . . . ? C1 Cr1 C4 C10 17.7(3) . . . . ? C3 Cr1 C4 C10 -172.77(16) . . . . ? C7 Cr1 C4 C10 -104.14(17) . . . . ? C8 Cr1 C4 C10 -67.28(16) . . . . ? C6 Cr1 C4 C10 -134.4(2) . . . . ? C9 Cr1 C4 C10 -30.48(15) . . . . ? O4 C4 C6 C7 177.9(2) . . . . ? C10 C4 C6 C7 -4.6(4) . . . . ? Cr1 C4 C6 C7 -56.0(2) . . . . ? O4 C4 C6 Cr1 -126.1(2) . . . . ? C10 C4 C6 Cr1 51.3(2) . . . . ? C2 Cr1 C6 C4 61.17(16) . . . . ? C1 Cr1 C6 C4 -103.3(4) . . . . ? C3 Cr1 C6 C4 150.92(15) . . . . ? C7 Cr1 C6 C4 -130.6(2) . . . . ? C8 Cr1 C6 C4 -101.69(15) . . . . ? C10 Cr1 C6 C4 -27.69(14) . . . . ? C9 Cr1 C6 C4 -64.57(15) . . . . ? C2 Cr1 C6 C7 -168.21(15) . . . . ? C1 Cr1 C6 C7 27.3(5) . . . . ? C3 Cr1 C6 C7 -78.46(15) . . . . ? C8 Cr1 C6 C7 28.93(14) . . . . ? C10 Cr1 C6 C7 102.93(15) . . . . ? C9 Cr1 C6 C7 66.05(14) . . . . ? C4 Cr1 C6 C7 130.6(2) . . . . ? C4 C6 C7 C8 2.6(4) . . . . ? Cr1 C6 C7 C8 -54.5(2) . . . . ? C4 C6 C7 C17 -171.1(2) . . . . ? Cr1 C6 C7 C17 131.9(2) . . . . ? C4 C6 C7 Cr1 57.1(2) . . . . ? C2 Cr1 C7 C8 150.83(18) . . . . ? C1 Cr1 C7 C8 -38.3(2) . . . . ? C3 Cr1 C7 C8 -123.07(16) . . . . ? C10 Cr1 C7 C8 66.96(15) . . . . ? C6 Cr1 C7 C8 132.3(2) . . . . ? C9 Cr1 C7 C8 30.21(14) . . . . ? C4 Cr1 C7 C8 102.97(16) . . . . ? C2 Cr1 C7 C6 18.5(2) . . . . ? C1 Cr1 C7 C6 -170.65(15) . . . . ? C3 Cr1 C7 C6 104.59(15) . . . . ? C8 Cr1 C7 C6 -132.3(2) . . . . ? C10 Cr1 C7 C6 -65.37(14) . . . . ? C9 Cr1 C7 C6 -102.12(16) . . . . ? C4 Cr1 C7 C6 -29.36(14) . . . . ? C2 Cr1 C7 C17 -92.3(3) . . . . ? C1 Cr1 C7 C17 78.6(3) . . . . ? C3 Cr1 C7 C17 -6.2(3) . . . . ? C8 Cr1 C7 C17 116.9(3) . . . . ? C10 Cr1 C7 C17 -176.2(3) . . . . ? C6 Cr1 C7 C17 -110.8(3) . . . . ? C9 Cr1 C7 C17 147.1(3) . . . . ? C4 Cr1 C7 C17 -140.2(3) . . . . ? C6 C7 C8 C9 -1.5(3) . . . . ? C17 C7 C8 C9 171.9(2) . . . . ? Cr1 C7 C8 C9 -56.0(2) . . . . ? C6 C7 C8 C14 175.5(2) . . . . ? C17 C7 C8 C14 -11.1(4) . . . . ? Cr1 C7 C8 C14 121.0(2) . . . . ? C6 C7 C8 Cr1 54.5(2) . . . . ? C17 C7 C8 Cr1 -132.1(2) . . . . ? C2 Cr1 C8 C7 -97.5(4) . . . . ? C1 Cr1 C8 C7 150.50(16) . . . . ? C3 Cr1 C8 C7 62.71(17) . . . . ? C10 Cr1 C8 C7 -101.64(16) . . . . ? C6 Cr1 C8 C7 -29.03(14) . . . . ? C9 Cr1 C8 C7 -130.1(2) . . . . ? C4 Cr1 C8 C7 -65.11(15) . . . . ? C2 Cr1 C8 C9 32.6(4) . . . . ? C1 Cr1 C8 C9 -79.40(17) . . . . ? C3 Cr1 C8 C9 -167.19(16) . . . . ? C7 Cr1 C8 C9 130.1(2) . . . . ? C10 Cr1 C8 C9 28.46(15) . . . . ? C6 Cr1 C8 C9 101.06(17) . . . . ? C4 Cr1 C8 C9 64.99(16) . . . . ? C2 Cr1 C8 C14 147.1(3) . . . . ? C1 Cr1 C8 C14 35.1(2) . . . . ? C3 Cr1 C8 C14 -52.7(2) . . . . ? C7 Cr1 C8 C14 -115.4(3) . . . . ? C10 Cr1 C8 C14 143.0(2) . . . . ? C6 Cr1 C8 C14 -144.4(2) . . . . ? C9 Cr1 C8 C14 114.5(3) . . . . ? C4 Cr1 C8 C14 179.5(2) . . . . ? C7 C8 C9 C10 2.4(4) . . . . ? C14 C8 C9 C10 -174.7(2) . . . . ? Cr1 C8 C9 C10 -53.3(2) . . . . ? C7 C8 C9 C11 -174.4(2) . . . . ? C14 C8 C9 C11 8.6(4) . . . . ? Cr1 C8 C9 C11 129.9(2) . . . . ? C7 C8 C9 Cr1 55.7(2) . . . . ? C14 C8 C9 Cr1 -121.3(2) . . . . ? C2 Cr1 C9 C10 -34.9(2) . . . . ? C1 Cr1 C9 C10 -124.31(18) . . . . ? C3 Cr1 C9 C10 154.5(2) . . . . ? C7 Cr1 C9 C10 102.91(17) . . . . ? C8 Cr1 C9 C10 133.2(2) . . . . ? C6 Cr1 C9 C10 65.77(16) . . . . ? C4 Cr1 C9 C10 30.07(16) . . . . ? C2 Cr1 C9 C8 -168.08(16) . . . . ? C1 Cr1 C9 C8 102.54(17) . . . . ? C3 Cr1 C9 C8 21.4(3) . . . . ? C7 Cr1 C9 C8 -30.24(15) . . . . ? C10 Cr1 C9 C8 -133.2(2) . . . . ? C6 Cr1 C9 C8 -67.38(16) . . . . ? C4 Cr1 C9 C8 -103.09(17) . . . . ? C2 Cr1 C9 C11 75.2(3) . . . . ? C1 Cr1 C9 C11 -14.2(3) . . . . ? C3 Cr1 C9 C11 -95.4(3) . . . . ? C7 Cr1 C9 C11 -147.0(3) . . . . ? C8 Cr1 C9 C11 -116.8(3) . . . . ? C10 Cr1 C9 C11 110.1(3) . . . . ? C6 Cr1 C9 C11 175.9(3) . . . . ? C4 Cr1 C9 C11 140.2(3) . . . . ? O4 C4 C10 C9 -177.2(2) . . . . ? C6 C4 C10 C9 5.5(4) . . . . ? Cr1 C4 C10 C9 57.0(2) . . . . ? O4 C4 C10 Cr1 125.8(2) . . . . ? C6 C4 C10 Cr1 -51.5(2) . . . . ? C8 C9 C10 C4 -4.4(4) . . . . ? C11 C9 C10 C4 172.5(2) . . . . ? Cr1 C9 C10 C4 -57.7(2) . . . . ? C8 C9 C10 Cr1 53.3(2) . . . . ? C11 C9 C10 Cr1 -129.7(2) . . . . ? C2 Cr1 C10 C4 -77.37(17) . . . . ? C1 Cr1 C10 C4 -169.25(16) . . . . ? C3 Cr1 C10 C4 22.1(5) . . . . ? C7 Cr1 C10 C4 64.35(16) . . . . ? C8 Cr1 C10 C4 101.36(17) . . . . ? C6 Cr1 C10 C4 27.40(15) . . . . ? C9 Cr1 C10 C4 129.8(2) . . . . ? C2 Cr1 C10 C9 152.79(17) . . . . ? C1 Cr1 C10 C9 60.91(18) . . . . ? C3 Cr1 C10 C9 -107.8(4) . . . . ? C7 Cr1 C10 C9 -65.50(16) . . . . ? C8 Cr1 C10 C9 -28.48(16) . . . . ? C6 Cr1 C10 C9 -102.44(17) . . . . ? C4 Cr1 C10 C9 -129.8(2) . . . . ? C10 C9 C11 C12 168.1(2) . . . . ? C8 C9 C11 C12 -15.0(3) . . . . ? Cr1 C9 C11 C12 78.8(3) . . . . ? C10 C9 C11 C26 -69.1(3) . . . . ? C8 C9 C11 C26 107.8(3) . . . . ? Cr1 C9 C11 C26 -158.4(2) . . . . ? C9 C11 C12 C13 43.3(3) . . . . ? C26 C11 C12 C13 -78.3(3) . . . . ? C11 C12 C13 C14 -66.5(3) . . . . ? C12 C13 C14 C15 -175.2(2) . . . . ? C12 C13 C14 C8 57.5(3) . . . . ? C7 C8 C14 C13 153.3(2) . . . . ? C9 C8 C14 C13 -29.7(3) . . . . ? Cr1 C8 C14 C13 -118.2(2) . . . . ? C7 C8 C14 C15 24.5(3) . . . . ? C9 C8 C14 C15 -158.5(2) . . . . ? Cr1 C8 C14 C15 113.0(2) . . . . ? C13 C14 C15 C16 -176.6(2) . . . . ? C8 C14 C15 C16 -50.0(3) . . . . ? C14 C15 C16 C17 64.3(3) . . . . ? C18 O5 C17 C7 -175.8(2) . . . . ? C18 O5 C17 C25 69.5(3) . . . . ? C18 O5 C17 C16 -54.2(3) . . . . ? C8 C7 C17 O5 144.6(2) . . . . ? C6 C7 C17 O5 -41.8(3) . . . . ? Cr1 C7 C17 O5 49.2(3) . . . . ? C8 C7 C17 C25 -98.7(3) . . . . ? C6 C7 C17 C25 74.9(3) . . . . ? Cr1 C7 C17 C25 165.9(2) . . . . ? C8 C7 C17 C16 22.9(3) . . . . ? C6 C7 C17 C16 -163.6(2) . . . . ? Cr1 C7 C17 C16 -72.5(3) . . . . ? C15 C16 C17 O5 -166.6(2) . . . . ? C15 C16 C17 C7 -48.7(3) . . . . ? C15 C16 C17 C25 70.5(3) . . . . ? C17 O5 C18 C19 -178.0(2) . . . . ? O5 C18 C19 C20 106.2(3) . . . . ? O5 C18 C19 C24 -74.5(4) . . . . ? C24 C19 C20 C21 1.1(4) . . . . ? C18 C19 C20 C21 -179.6(3) . . . . ? C19 C20 C21 C22 -0.9(5) . . . . ? C20 C21 C22 C23 0.5(5) . . . . ? C21 C22 C23 C24 -0.4(5) . . . . ? C22 C23 C24 C19 0.6(5) . . . . ? C20 C19 C24 C23 -0.9(4) . . . . ? C18 C19 C24 C23 179.8(3) . . . . ? C9 C11 C26 C27 79.4(3) . . . . ? C12 C11 C26 C27 -156.9(3) . . . . ? C11 C26 C27 C28 -121.9(3) . . . . ? C11 C26 C27 C29 60.2(3) . . . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.279 _refine_diff_density_min -0.582 _refine_diff_density_rms 0.069 data_asch117 _database_code_depnum_ccdc_archive 'CCDC 871296' #TrackingRef 'asch117.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C29 H31 Cr F O5' _chemical_formula_sum 'C29 H31 Cr F O5' _chemical_formula_weight 530.54 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' Cr Cr 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.9722(4) _cell_length_b 12.8619(7) _cell_length_c 13.5661(5) _cell_angle_alpha 68.848(3) _cell_angle_beta 81.683(3) _cell_angle_gamma 81.459(2) _cell_volume 1276.66(11) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 7740 _cell_measurement_theta_min 1.62 _cell_measurement_theta_max 27.00 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max .3 _exptl_crystal_size_mid .2 _exptl_crystal_size_min .1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.380 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 556 _exptl_absorpt_coefficient_mu 0.493 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'Nonius KappaCCD' _diffrn_measurement_method Phi/Omega-Scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7740 _diffrn_reflns_av_R_equivalents 0.0176 _diffrn_reflns_av_sigmaI/netI 0.0523 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.62 _diffrn_reflns_theta_max 27.00 _reflns_number_total 5554 _reflns_number_gt 4396 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius COLLECT' _computing_cell_refinement 'Nonius DENZO (Otwinowski, Minor 1997)' _computing_data_reduction 'Nonius DENZO (Otwinowski, Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SCHAKAL99 (E. Keller 1999)' _computing_publication_material 'PLATON (A. L. Spek 1980-2004)' _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^)+(0.0358P)^2^+0.2863P] 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 5554 _refine_ls_number_parameters 328 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0510 _refine_ls_R_factor_gt 0.0354 _refine_ls_wR_factor_ref 0.0903 _refine_ls_wR_factor_gt 0.0853 _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_restrained_S_all 1.059 _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 Cr1 Cr 0.52063(4) 0.40152(2) 0.30564(2) 0.01478(9) Uani 1 1 d . . . F1 F 0.91032(15) 1.01417(11) 0.10619(9) 0.0368(3) Uani 1 1 d . . . O1 O 0.70278(18) 0.57802(12) 0.13189(11) 0.0309(3) Uani 1 1 d . . . O2 O 0.80375(18) 0.36498(13) 0.44280(11) 0.0334(4) Uani 1 1 d . . . O3 O 0.72594(18) 0.23482(13) 0.21718(11) 0.0322(3) Uani 1 1 d . . . O4 O 0.35578(17) 0.39821(11) 0.54677(9) 0.0219(3) Uani 1 1 d . . . O5 O 0.34424(16) 0.70026(10) 0.19923(9) 0.0178(3) Uani 1 1 d . . . C1 C 0.6310(2) 0.51096(16) 0.19945(14) 0.0193(4) Uani 1 1 d . . . C2 C 0.6938(3) 0.38145(16) 0.39012(14) 0.0224(4) Uani 1 1 d . . . C3 C 0.6464(2) 0.29967(17) 0.25211(14) 0.0206(4) Uani 1 1 d . . . C4 C 0.3316(2) 0.39693(16) 0.45037(13) 0.0175(4) Uani 1 1 d . . . C5 C 0.3912(3) 0.29258(16) 0.62939(13) 0.0223(4) Uani 1 1 d . . . H5A H 0.2958 0.2476 0.6431 0.033 Uiso 1 1 calc R . . H5B H 0.4064 0.3055 0.6943 0.033 Uiso 1 1 calc R . . H5C H 0.4955 0.2525 0.6071 0.033 Uiso 1 1 calc R . . C6 C 0.3104(2) 0.50268(15) 0.37079(13) 0.0170(4) Uani 1 1 d . . . H6 H 0.3190 0.5682 0.3859 0.020 Uiso 1 1 calc R . . C7 C 0.2762(2) 0.51236(15) 0.26826(12) 0.0152(4) Uani 1 1 d . . . C8 C 0.2713(2) 0.41502(15) 0.24305(12) 0.0146(4) Uani 1 1 d . . . C9 C 0.2989(2) 0.30837(15) 0.32289(13) 0.0156(4) Uani 1 1 d . . . C10 C 0.3313(2) 0.29991(16) 0.42588(13) 0.0176(4) Uani 1 1 d . . . H10 H 0.3530 0.2282 0.4784 0.021 Uiso 1 1 calc R . . C11 C 0.2879(2) 0.19914(15) 0.30536(13) 0.0164(4) Uani 1 1 d . . . H11 H 0.3927 0.1479 0.3296 0.020 Uiso 1 1 calc R . . C12 C 0.2810(2) 0.21580(16) 0.18785(13) 0.0188(4) Uani 1 1 d . . . H12A H 0.3976 0.2209 0.1509 0.023 Uiso 1 1 calc R . . H12B H 0.2367 0.1501 0.1829 0.023 Uiso 1 1 calc R . . C13 C 0.1669(2) 0.32217(16) 0.13306(13) 0.0186(4) Uani 1 1 d . . . H13A H 0.1554 0.3271 0.0598 0.022 Uiso 1 1 calc R . . H13B H 0.0519 0.3198 0.1723 0.022 Uiso 1 1 calc R . . C14 C 0.2459(2) 0.42428(15) 0.13035(13) 0.0165(4) Uani 1 1 d . . . H14 H 0.3616 0.4230 0.0906 0.020 Uiso 1 1 calc R . . C15 C 0.1470(2) 0.53568(16) 0.07276(14) 0.0195(4) Uani 1 1 d . . . H15A H 0.0281 0.5374 0.1060 0.023 Uiso 1 1 calc R . . H15B H 0.1444 0.5436 -0.0024 0.023 Uiso 1 1 calc R . . C16 C 0.2300(2) 0.63287(15) 0.07784(13) 0.0189(4) Uani 1 1 d . . . H16A H 0.1704 0.7046 0.0346 0.023 Uiso 1 1 calc R . . H16B H 0.3502 0.6291 0.0470 0.023 Uiso 1 1 calc R . . C17 C 0.2241(2) 0.63038(15) 0.19193(13) 0.0171(4) Uani 1 1 d . . . C18 C 0.3093(3) 0.81827(16) 0.14349(15) 0.0239(4) Uani 1 1 d . . . H18A H 0.2153 0.8507 0.1833 0.029 Uiso 1 1 calc R . . H18B H 0.2749 0.8315 0.0723 0.029 Uiso 1 1 calc R . . C19 C 0.4689(2) 0.87192(15) 0.13304(13) 0.0193(4) Uani 1 1 d . . . C20 C 0.4780(3) 0.94280(16) 0.18821(14) 0.0215(4) Uani 1 1 d . . . H20 H 0.3815 0.9581 0.2328 0.026 Uiso 1 1 calc R . . C21 C 0.6263(3) 0.99173(16) 0.17926(14) 0.0241(4) Uani 1 1 d . . . H21 H 0.6322 1.0407 0.2166 0.029 Uiso 1 1 calc R . . C22 C 0.7641(3) 0.96719(17) 0.11489(14) 0.0242(4) Uani 1 1 d . . . C23 C 0.7600(3) 0.89776(17) 0.05823(14) 0.0245(4) Uani 1 1 d . . . H23 H 0.8569 0.8829 0.0137 0.029 Uiso 1 1 calc R . . C24 C 0.6111(3) 0.85047(16) 0.06800(13) 0.0227(4) Uani 1 1 d . . . H24 H 0.6057 0.8024 0.0296 0.027 Uiso 1 1 calc R . . C25 C 0.0439(2) 0.66526(17) 0.23496(14) 0.0219(4) Uani 1 1 d . . . H25A H 0.0477 0.6708 0.3048 0.033 Uiso 1 1 calc R . . H25B H -0.0318 0.6091 0.2416 0.033 Uiso 1 1 calc R . . H25C H 0.0008 0.7382 0.1859 0.033 Uiso 1 1 calc R . . C26 C 0.1312(2) 0.14182(15) 0.37446(13) 0.0192(4) Uani 1 1 d . . . H26A H 0.1202 0.1512 0.4445 0.023 Uiso 1 1 calc R . . H26B H 0.0268 0.1796 0.3397 0.023 Uiso 1 1 calc R . . C27 C 0.1451(3) 0.01823(17) 0.39090(14) 0.0262(5) Uani 1 1 d . . . C28 C 0.0471(3) -0.0220(2) 0.34487(17) 0.0391(6) Uani 1 1 d . . . H28A H 0.0581 -0.1001 0.3567 0.047 Uiso 1 1 calc R . . H28B H -0.0341 0.0272 0.3001 0.047 Uiso 1 1 calc R . . C29 C 0.2760(3) -0.05617(19) 0.46270(17) 0.0382(6) Uani 1 1 d . . . H29A H 0.2628 -0.1349 0.4766 0.057 Uiso 1 1 calc R . . H29B H 0.2596 -0.0420 0.5300 0.057 Uiso 1 1 calc R . . H29C H 0.3906 -0.0398 0.4282 0.057 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 Cr1 0.01581(16) 0.01361(16) 0.01451(15) -0.00366(11) -0.00420(10) -0.00073(12) F1 0.0290(7) 0.0432(8) 0.0391(7) -0.0100(6) -0.0046(5) -0.0162(6) O1 0.0230(8) 0.0241(8) 0.0350(8) -0.0006(6) 0.0063(6) -0.0036(7) O2 0.0295(8) 0.0376(9) 0.0400(8) -0.0193(7) -0.0200(7) 0.0066(7) O3 0.0233(8) 0.0326(9) 0.0498(9) -0.0270(7) 0.0002(6) -0.0020(7) O4 0.0359(8) 0.0171(7) 0.0123(6) -0.0040(5) -0.0064(5) -0.0007(6) O5 0.0209(7) 0.0113(7) 0.0199(6) -0.0017(5) -0.0072(5) -0.0021(5) C1 0.0145(9) 0.0194(10) 0.0232(9) -0.0069(8) -0.0047(7) 0.0022(8) C2 0.0252(11) 0.0188(11) 0.0238(10) -0.0087(8) -0.0037(8) 0.0003(9) C3 0.0159(10) 0.0223(11) 0.0241(9) -0.0065(8) -0.0026(7) -0.0068(8) C4 0.0182(10) 0.0196(10) 0.0141(8) -0.0053(7) -0.0022(7) -0.0009(8) C5 0.0329(11) 0.0191(10) 0.0122(8) -0.0016(7) -0.0062(7) -0.0002(9) C6 0.0204(10) 0.0144(10) 0.0172(9) -0.0063(7) -0.0037(7) -0.0011(8) C7 0.0118(9) 0.0169(10) 0.0151(8) -0.0032(7) -0.0006(6) -0.0023(7) C8 0.0120(9) 0.0153(10) 0.0157(8) -0.0039(7) -0.0023(6) -0.0016(7) C9 0.0138(9) 0.0161(10) 0.0160(8) -0.0048(7) -0.0003(6) -0.0019(7) C10 0.0210(10) 0.0146(10) 0.0146(8) -0.0017(7) -0.0021(7) -0.0021(8) C11 0.0180(10) 0.0131(9) 0.0170(8) -0.0038(7) -0.0024(7) -0.0014(8) C12 0.0232(10) 0.0174(10) 0.0170(9) -0.0066(7) -0.0007(7) -0.0057(8) C13 0.0223(10) 0.0188(10) 0.0154(8) -0.0047(7) -0.0049(7) -0.0050(8) C14 0.0151(9) 0.0184(10) 0.0153(8) -0.0046(7) -0.0024(7) -0.0017(8) C15 0.0223(10) 0.0187(10) 0.0176(9) -0.0041(7) -0.0078(7) -0.0023(8) C16 0.0227(10) 0.0147(10) 0.0173(9) -0.0018(7) -0.0070(7) -0.0007(8) C17 0.0183(10) 0.0142(10) 0.0180(9) -0.0029(7) -0.0055(7) -0.0024(8) C18 0.0261(11) 0.0124(10) 0.0300(10) -0.0012(8) -0.0095(8) -0.0015(8) C19 0.0242(10) 0.0108(9) 0.0187(9) 0.0017(7) -0.0088(7) -0.0006(8) C20 0.0247(11) 0.0157(10) 0.0212(9) -0.0036(7) -0.0026(7) 0.0001(8) C21 0.0321(12) 0.0171(10) 0.0248(10) -0.0068(8) -0.0083(8) -0.0034(9) C22 0.0243(11) 0.0224(11) 0.0220(9) 0.0012(8) -0.0076(8) -0.0077(9) C23 0.0263(11) 0.0229(11) 0.0195(9) -0.0022(8) -0.0021(8) -0.0011(9) C24 0.0340(12) 0.0162(10) 0.0168(9) -0.0031(7) -0.0072(8) -0.0017(9) C25 0.0189(10) 0.0188(10) 0.0261(10) -0.0054(8) -0.0046(8) 0.0002(8) C26 0.0210(10) 0.0162(10) 0.0192(9) -0.0042(7) -0.0003(7) -0.0045(8) C27 0.0288(11) 0.0250(12) 0.0239(10) -0.0089(8) 0.0095(8) -0.0106(9) C28 0.0472(15) 0.0394(14) 0.0369(12) -0.0206(11) 0.0128(10) -0.0213(12) C29 0.0413(14) 0.0213(12) 0.0395(12) -0.0004(9) 0.0058(10) -0.0006(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cr1 C3 1.826(2) . ? Cr1 C1 1.835(2) . ? Cr1 C2 1.8505(19) . ? Cr1 C9 2.2188(19) . ? Cr1 C10 2.2320(19) . ? Cr1 C8 2.2317(17) . ? Cr1 C7 2.2416(17) . ? Cr1 C6 2.2443(17) . ? Cr1 C4 2.2840(17) . ? F1 C22 1.362(2) . ? O1 C1 1.156(2) . ? O2 C2 1.158(2) . ? O3 C3 1.168(2) . ? O4 C4 1.3555(19) . ? O4 C5 1.435(2) . ? O5 C18 1.435(2) . ? O5 C17 1.443(2) . ? C4 C10 1.403(3) . ? C4 C6 1.403(2) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 C7 1.414(2) . ? C6 H6 0.9500 . ? C7 C8 1.419(2) . ? C7 C17 1.534(2) . ? C8 C9 1.418(2) . ? C8 C14 1.531(2) . ? C9 C10 1.420(2) . ? C9 C11 1.524(2) . ? C10 H10 0.9500 . ? C11 C12 1.538(2) . ? C11 C26 1.555(3) . ? C11 H11 1.0000 . ? C12 C13 1.531(2) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.525(3) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.523(2) . ? C14 H14 1.0000 . ? C15 C16 1.525(3) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.531(2) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C25 1.537(3) . ? C18 C19 1.501(3) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.387(3) . ? C19 C24 1.390(3) . ? C20 C21 1.390(3) . ? C20 H20 0.9500 . ? C21 C22 1.374(3) . ? C21 H21 0.9500 . ? C22 C23 1.379(3) . ? C23 C24 1.381(3) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 C27 1.513(3) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 C28 1.328(3) . ? C27 C29 1.510(3) . ? C28 H28A 0.9500 . ? C28 H28B 0.9500 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 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 C3 Cr1 C1 87.71(8) . . ? C3 Cr1 C2 87.79(8) . . ? C1 Cr1 C2 89.50(8) . . ? C3 Cr1 C9 86.96(8) . . ? C1 Cr1 C9 136.73(7) . . ? C2 Cr1 C9 133.09(8) . . ? C3 Cr1 C10 103.05(8) . . ? C1 Cr1 C10 165.93(7) . . ? C2 Cr1 C10 99.81(8) . . ? C9 Cr1 C10 37.22(6) . . ? C3 Cr1 C8 100.61(7) . . ? C1 Cr1 C8 102.54(7) . . ? C2 Cr1 C8 165.49(7) . . ? C9 Cr1 C8 37.15(6) . . ? C10 Cr1 C8 66.91(6) . . ? C3 Cr1 C7 134.41(7) . . ? C1 Cr1 C7 87.98(7) . . ? C2 Cr1 C7 137.52(7) . . ? C9 Cr1 C7 66.37(6) . . ? C10 Cr1 C7 78.02(6) . . ? C8 Cr1 C7 36.99(6) . . ? C3 Cr1 C6 165.16(8) . . ? C1 Cr1 C6 102.09(7) . . ? C2 Cr1 C6 103.25(7) . . ? C9 Cr1 C6 78.26(7) . . ? C10 Cr1 C6 65.65(7) . . ? C8 Cr1 C6 66.61(6) . . ? C7 Cr1 C6 36.74(6) . . ? C3 Cr1 C4 136.89(8) . . ? C1 Cr1 C4 135.08(7) . . ? C2 Cr1 C4 87.76(7) . . ? C9 Cr1 C4 65.87(6) . . ? C10 Cr1 C4 36.17(6) . . ? C8 Cr1 C4 78.02(6) . . ? C7 Cr1 C4 65.38(6) . . ? C6 Cr1 C4 36.09(6) . . ? C4 O4 C5 117.88(14) . . ? C18 O5 C17 115.79(13) . . ? O1 C1 Cr1 178.45(17) . . ? O2 C2 Cr1 177.48(17) . . ? O3 C3 Cr1 179.40(16) . . ? O4 C4 C10 125.04(16) . . ? O4 C4 C6 115.22(16) . . ? C10 C4 C6 119.72(15) . . ? O4 C4 Cr1 130.83(13) . . ? C10 C4 Cr1 69.89(10) . . ? C6 C4 Cr1 70.41(10) . . ? O4 C5 H5A 109.5 . . ? O4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? O4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C4 C6 C7 120.41(16) . . ? C4 C6 Cr1 73.50(10) . . ? C7 C6 Cr1 71.52(10) . . ? C4 C6 H6 119.8 . . ? C7 C6 H6 119.8 . . ? Cr1 C6 H6 127.2 . . ? C6 C7 C8 120.39(16) . . ? C6 C7 C17 117.15(15) . . ? C8 C7 C17 122.05(14) . . ? C6 C7 Cr1 71.74(10) . . ? C8 C7 Cr1 71.13(10) . . ? C17 C7 Cr1 136.25(12) . . ? C9 C8 C7 118.78(15) . . ? C9 C8 C14 120.32(15) . . ? C7 C8 C14 120.84(15) . . ? C9 C8 Cr1 70.93(10) . . ? C7 C8 Cr1 71.88(10) . . ? C14 C8 Cr1 126.11(12) . . ? C8 C9 C10 120.23(16) . . ? C8 C9 C11 122.78(14) . . ? C10 C9 C11 116.93(15) . . ? C8 C9 Cr1 71.92(10) . . ? C10 C9 Cr1 71.90(11) . . ? C11 C9 Cr1 130.81(12) . . ? C4 C10 C9 120.32(16) . . ? C4 C10 Cr1 73.94(11) . . ? C9 C10 Cr1 70.89(10) . . ? C4 C10 H10 119.8 . . ? C9 C10 H10 119.8 . . ? Cr1 C10 H10 127.4 . . ? C9 C11 C12 112.67(15) . . ? C9 C11 C26 110.04(14) . . ? C12 C11 C26 110.57(14) . . ? C9 C11 H11 107.8 . . ? C12 C11 H11 107.8 . . ? C26 C11 H11 107.8 . . ? C13 C12 C11 111.40(14) . . ? C13 C12 H12A 109.3 . . ? C11 C12 H12A 109.3 . . ? C13 C12 H12B 109.3 . . ? C11 C12 H12B 109.3 . . ? H12A C12 H12B 108.0 . . ? C14 C13 C12 109.22(14) . . ? C14 C13 H13A 109.8 . . ? C12 C13 H13A 109.8 . . ? C14 C13 H13B 109.8 . . ? C12 C13 H13B 109.8 . . ? H13A C13 H13B 108.3 . . ? C15 C14 C13 113.81(15) . . ? C15 C14 C8 111.14(14) . . ? C13 C14 C8 110.24(14) . . ? C15 C14 H14 107.1 . . ? C13 C14 H14 107.1 . . ? C8 C14 H14 107.1 . . ? C14 C15 C16 110.42(14) . . ? C14 C15 H15A 109.6 . . ? C16 C15 H15A 109.6 . . ? C14 C15 H15B 109.6 . . ? C16 C15 H15B 109.6 . . ? H15A C15 H15B 108.1 . . ? C15 C16 C17 111.84(15) . . ? C15 C16 H16A 109.2 . . ? C17 C16 H16A 109.2 . . ? C15 C16 H16B 109.2 . . ? C17 C16 H16B 109.2 . . ? H16A C16 H16B 107.9 . . ? O5 C17 C16 110.76(15) . . ? O5 C17 C7 105.55(13) . . ? C16 C17 C7 111.67(14) . . ? O5 C17 C25 110.52(14) . . ? C16 C17 C25 111.94(14) . . ? C7 C17 C25 106.12(14) . . ? O5 C18 C19 107.79(14) . . ? O5 C18 H18A 110.1 . . ? C19 C18 H18A 110.1 . . ? O5 C18 H18B 110.1 . . ? C19 C18 H18B 110.1 . . ? H18A C18 H18B 108.5 . . ? C20 C19 C24 118.84(18) . . ? C20 C19 C18 120.95(17) . . ? C24 C19 C18 120.21(17) . . ? C19 C20 C21 120.96(18) . . ? C19 C20 H20 119.5 . . ? C21 C20 H20 119.5 . . ? C22 C21 C20 118.13(18) . . ? C22 C21 H21 120.9 . . ? C20 C21 H21 120.9 . . ? F1 C22 C21 118.53(18) . . ? F1 C22 C23 118.73(18) . . ? C21 C22 C23 122.74(19) . . ? C22 C23 C24 118.12(18) . . ? C22 C23 H23 120.9 . . ? C24 C23 H23 120.9 . . ? C23 C24 C19 121.21(18) . . ? C23 C24 H24 119.4 . . ? C19 C24 H24 119.4 . . ? C17 C25 H25A 109.5 . . ? C17 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C17 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C27 C26 C11 112.60(15) . . ? C27 C26 H26A 109.1 . . ? C11 C26 H26A 109.1 . . ? C27 C26 H26B 109.1 . . ? C11 C26 H26B 109.1 . . ? H26A C26 H26B 107.8 . . ? C28 C27 C29 122.2(2) . . ? C28 C27 C26 121.7(2) . . ? C29 C27 C26 116.11(18) . . ? C27 C28 H28A 120.0 . . ? C27 C28 H28B 120.0 . . ? H28A C28 H28B 120.0 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? 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 C3 Cr1 C1 O1 -5(6) . . . . ? C2 Cr1 C1 O1 83(6) . . . . ? C9 Cr1 C1 O1 -88(6) . . . . ? C10 Cr1 C1 O1 -146(6) . . . . ? C8 Cr1 C1 O1 -106(6) . . . . ? C7 Cr1 C1 O1 -140(6) . . . . ? C6 Cr1 C1 O1 -174(100) . . . . ? C4 Cr1 C1 O1 169(6) . . . . ? C3 Cr1 C2 O2 -26(4) . . . . ? C1 Cr1 C2 O2 -114(4) . . . . ? C9 Cr1 C2 O2 57(4) . . . . ? C10 Cr1 C2 O2 77(4) . . . . ? C8 Cr1 C2 O2 100(4) . . . . ? C7 Cr1 C2 O2 160(4) . . . . ? C6 Cr1 C2 O2 144(4) . . . . ? C4 Cr1 C2 O2 111(4) . . . . ? C1 Cr1 C3 O3 -78(19) . . . . ? C2 Cr1 C3 O3 -167(100) . . . . ? C9 Cr1 C3 O3 59(19) . . . . ? C10 Cr1 C3 O3 93(19) . . . . ? C8 Cr1 C3 O3 25(19) . . . . ? C7 Cr1 C3 O3 7(19) . . . . ? C6 Cr1 C3 O3 54(19) . . . . ? C4 Cr1 C3 O3 108(19) . . . . ? C5 O4 C4 C10 2.8(3) . . . . ? C5 O4 C4 C6 -175.36(16) . . . . ? C5 O4 C4 Cr1 -90.1(2) . . . . ? C3 Cr1 C4 O4 93.78(19) . . . . ? C1 Cr1 C4 O4 -77.62(18) . . . . ? C2 Cr1 C4 O4 9.43(17) . . . . ? C9 Cr1 C4 O4 149.48(18) . . . . ? C10 Cr1 C4 O4 119.5(2) . . . . ? C8 Cr1 C4 O4 -173.44(17) . . . . ? C7 Cr1 C4 O4 -136.66(18) . . . . ? C6 Cr1 C4 O4 -106.9(2) . . . . ? C3 Cr1 C4 C10 -25.67(15) . . . . ? C1 Cr1 C4 C10 162.93(11) . . . . ? C2 Cr1 C4 C10 -110.02(11) . . . . ? C9 Cr1 C4 C10 30.02(10) . . . . ? C8 Cr1 C4 C10 67.11(11) . . . . ? C7 Cr1 C4 C10 103.89(11) . . . . ? C6 Cr1 C4 C10 133.68(15) . . . . ? C3 Cr1 C4 C6 -159.35(11) . . . . ? C1 Cr1 C4 C6 29.25(15) . . . . ? C2 Cr1 C4 C6 116.30(12) . . . . ? C9 Cr1 C4 C6 -103.66(11) . . . . ? C10 Cr1 C4 C6 -133.68(15) . . . . ? C8 Cr1 C4 C6 -66.57(11) . . . . ? C7 Cr1 C4 C6 -29.79(10) . . . . ? O4 C4 C6 C7 -177.03(16) . . . . ? C10 C4 C6 C7 4.7(3) . . . . ? Cr1 C4 C6 C7 56.14(15) . . . . ? O4 C4 C6 Cr1 126.83(15) . . . . ? C10 C4 C6 Cr1 -51.45(16) . . . . ? C3 Cr1 C6 C4 70.2(3) . . . . ? C1 Cr1 C6 C4 -159.34(11) . . . . ? C2 Cr1 C6 C4 -66.97(12) . . . . ? C9 Cr1 C6 C4 64.93(11) . . . . ? C10 Cr1 C6 C4 27.94(10) . . . . ? C8 Cr1 C6 C4 102.08(12) . . . . ? C7 Cr1 C6 C4 130.97(16) . . . . ? C3 Cr1 C6 C7 -60.8(3) . . . . ? C1 Cr1 C6 C7 69.69(12) . . . . ? C2 Cr1 C6 C7 162.06(12) . . . . ? C9 Cr1 C6 C7 -66.04(11) . . . . ? C10 Cr1 C6 C7 -103.03(12) . . . . ? C8 Cr1 C6 C7 -28.89(10) . . . . ? C4 Cr1 C6 C7 -130.97(16) . . . . ? C4 C6 C7 C8 -3.1(3) . . . . ? Cr1 C6 C7 C8 53.96(15) . . . . ? C4 C6 C7 C17 169.63(16) . . . . ? Cr1 C6 C7 C17 -133.29(15) . . . . ? C4 C6 C7 Cr1 -57.08(16) . . . . ? C3 Cr1 C7 C6 161.76(12) . . . . ? C1 Cr1 C7 C6 -113.42(12) . . . . ? C2 Cr1 C7 C6 -26.36(17) . . . . ? C9 Cr1 C7 C6 102.41(11) . . . . ? C10 Cr1 C7 C6 65.14(11) . . . . ? C8 Cr1 C7 C6 132.51(16) . . . . ? C4 Cr1 C7 C6 29.29(11) . . . . ? C3 Cr1 C7 C8 29.25(15) . . . . ? C1 Cr1 C7 C8 114.07(11) . . . . ? C2 Cr1 C7 C8 -158.88(12) . . . . ? C9 Cr1 C7 C8 -30.10(10) . . . . ? C10 Cr1 C7 C8 -67.37(10) . . . . ? C6 Cr1 C7 C8 -132.51(16) . . . . ? C4 Cr1 C7 C8 -103.22(11) . . . . ? C3 Cr1 C7 C17 -87.7(2) . . . . ? C1 Cr1 C7 C17 -2.93(17) . . . . ? C2 Cr1 C7 C17 84.13(19) . . . . ? C9 Cr1 C7 C17 -147.09(18) . . . . ? C10 Cr1 C7 C17 175.63(18) . . . . ? C8 Cr1 C7 C17 -117.0(2) . . . . ? C6 Cr1 C7 C17 110.5(2) . . . . ? C4 Cr1 C7 C17 139.78(18) . . . . ? C6 C7 C8 C9 0.9(3) . . . . ? C17 C7 C8 C9 -171.51(16) . . . . ? Cr1 C7 C8 C9 55.11(14) . . . . ? C6 C7 C8 C14 -176.03(16) . . . . ? C17 C7 C8 C14 11.6(3) . . . . ? Cr1 C7 C8 C14 -121.79(16) . . . . ? C6 C7 C8 Cr1 -54.24(15) . . . . ? C17 C7 C8 Cr1 133.37(16) . . . . ? C3 Cr1 C8 C9 70.33(11) . . . . ? C1 Cr1 C8 C9 160.34(10) . . . . ? C2 Cr1 C8 C9 -54.2(3) . . . . ? C10 Cr1 C8 C9 -29.45(10) . . . . ? C7 Cr1 C8 C9 -130.47(14) . . . . ? C6 Cr1 C8 C9 -101.76(11) . . . . ? C4 Cr1 C8 C9 -65.68(10) . . . . ? C3 Cr1 C8 C7 -159.20(11) . . . . ? C1 Cr1 C8 C7 -69.19(11) . . . . ? C2 Cr1 C8 C7 76.3(3) . . . . ? C9 Cr1 C8 C7 130.47(14) . . . . ? C10 Cr1 C8 C7 101.02(11) . . . . ? C6 Cr1 C8 C7 28.71(10) . . . . ? C4 Cr1 C8 C7 64.78(10) . . . . ? C3 Cr1 C8 C14 -43.80(16) . . . . ? C1 Cr1 C8 C14 46.20(16) . . . . ? C2 Cr1 C8 C14 -168.3(3) . . . . ? C9 Cr1 C8 C14 -114.13(19) . . . . ? C10 Cr1 C8 C14 -143.59(17) . . . . ? C7 Cr1 C8 C14 115.40(19) . . . . ? C6 Cr1 C8 C14 144.11(17) . . . . ? C4 Cr1 C8 C14 -179.82(16) . . . . ? C7 C8 C9 C10 -0.2(3) . . . . ? C14 C8 C9 C10 176.69(16) . . . . ? Cr1 C8 C9 C10 55.35(15) . . . . ? C7 C8 C9 C11 177.01(16) . . . . ? C14 C8 C9 C11 -6.1(3) . . . . ? Cr1 C8 C9 C11 -127.41(17) . . . . ? C7 C8 C9 Cr1 -55.58(15) . . . . ? C14 C8 C9 Cr1 121.34(15) . . . . ? C3 Cr1 C9 C8 -112.05(11) . . . . ? C1 Cr1 C9 C8 -28.64(15) . . . . ? C2 Cr1 C9 C8 163.85(11) . . . . ? C10 Cr1 C9 C8 131.60(15) . . . . ? C7 Cr1 C9 C8 29.97(9) . . . . ? C6 Cr1 C9 C8 66.60(10) . . . . ? C4 Cr1 C9 C8 102.38(11) . . . . ? C3 Cr1 C9 C10 116.35(11) . . . . ? C1 Cr1 C9 C10 -160.24(11) . . . . ? C2 Cr1 C9 C10 32.25(15) . . . . ? C8 Cr1 C9 C10 -131.60(15) . . . . ? C7 Cr1 C9 C10 -101.63(11) . . . . ? C6 Cr1 C9 C10 -65.00(10) . . . . ? C4 Cr1 C9 C10 -29.22(10) . . . . ? C3 Cr1 C9 C11 6.03(15) . . . . ? C1 Cr1 C9 C11 89.44(17) . . . . ? C2 Cr1 C9 C11 -78.07(17) . . . . ? C10 Cr1 C9 C11 -110.32(19) . . . . ? C8 Cr1 C9 C11 118.08(19) . . . . ? C7 Cr1 C9 C11 148.05(16) . . . . ? C6 Cr1 C9 C11 -175.32(16) . . . . ? C4 Cr1 C9 C11 -139.54(16) . . . . ? O4 C4 C10 C9 177.86(16) . . . . ? C6 C4 C10 C9 -4.0(3) . . . . ? Cr1 C4 C10 C9 -55.73(15) . . . . ? O4 C4 C10 Cr1 -126.41(18) . . . . ? C6 C4 C10 Cr1 51.68(16) . . . . ? C8 C9 C10 C4 1.8(3) . . . . ? C11 C9 C10 C4 -175.58(16) . . . . ? Cr1 C9 C10 C4 57.19(16) . . . . ? C8 C9 C10 Cr1 -55.36(15) . . . . ? C11 C9 C10 Cr1 127.24(15) . . . . ? C3 Cr1 C10 C4 162.31(11) . . . . ? C1 Cr1 C10 C4 -58.5(3) . . . . ? C2 Cr1 C10 C4 72.32(11) . . . . ? C9 Cr1 C10 C4 -130.98(15) . . . . ? C8 Cr1 C10 C4 -101.58(11) . . . . ? C7 Cr1 C10 C4 -64.44(10) . . . . ? C6 Cr1 C10 C4 -27.88(10) . . . . ? C3 Cr1 C10 C9 -66.71(11) . . . . ? C1 Cr1 C10 C9 72.5(3) . . . . ? C2 Cr1 C10 C9 -156.70(11) . . . . ? C8 Cr1 C10 C9 29.40(10) . . . . ? C7 Cr1 C10 C9 66.54(10) . . . . ? C6 Cr1 C10 C9 103.10(11) . . . . ? C4 Cr1 C10 C9 130.98(15) . . . . ? C8 C9 C11 C12 11.8(2) . . . . ? C10 C9 C11 C12 -170.89(15) . . . . ? Cr1 C9 C11 C12 -82.14(18) . . . . ? C8 C9 C11 C26 -112.12(18) . . . . ? C10 C9 C11 C26 65.2(2) . . . . ? Cr1 C9 C11 C26 153.95(12) . . . . ? C9 C11 C12 C13 -40.6(2) . . . . ? C26 C11 C12 C13 83.01(19) . . . . ? C11 C12 C13 C14 65.04(19) . . . . ? C12 C13 C14 C15 177.30(14) . . . . ? C12 C13 C14 C8 -57.05(18) . . . . ? C9 C8 C14 C15 155.80(16) . . . . ? C7 C8 C14 C15 -27.3(2) . . . . ? Cr1 C8 C14 C15 -116.61(15) . . . . ? C9 C8 C14 C13 28.7(2) . . . . ? C7 C8 C14 C13 -154.48(16) . . . . ? Cr1 C8 C14 C13 116.25(15) . . . . ? C13 C14 C15 C16 177.57(14) . . . . ? C8 C14 C15 C16 52.4(2) . . . . ? C14 C15 C16 C17 -64.0(2) . . . . ? C18 O5 C17 C16 65.91(18) . . . . ? C18 O5 C17 C7 -173.06(14) . . . . ? C18 O5 C17 C25 -58.74(18) . . . . ? C15 C16 C17 O5 162.93(14) . . . . ? C15 C16 C17 C7 45.6(2) . . . . ? C15 C16 C17 C25 -73.23(19) . . . . ? C6 C7 C17 O5 46.8(2) . . . . ? C8 C7 C17 O5 -140.61(16) . . . . ? Cr1 C7 C17 O5 -44.7(2) . . . . ? C6 C7 C17 C16 167.20(16) . . . . ? C8 C7 C17 C16 -20.2(2) . . . . ? Cr1 C7 C17 C16 75.7(2) . . . . ? C6 C7 C17 C25 -70.57(19) . . . . ? C8 C7 C17 C25 102.05(18) . . . . ? Cr1 C7 C17 C25 -162.09(14) . . . . ? C17 O5 C18 C19 -163.66(14) . . . . ? O5 C18 C19 C20 -111.13(18) . . . . ? O5 C18 C19 C24 68.4(2) . . . . ? C24 C19 C20 C21 -0.1(3) . . . . ? C18 C19 C20 C21 179.44(16) . . . . ? C19 C20 C21 C22 -0.5(3) . . . . ? C20 C21 C22 F1 -179.57(16) . . . . ? C20 C21 C22 C23 0.9(3) . . . . ? F1 C22 C23 C24 179.84(15) . . . . ? C21 C22 C23 C24 -0.7(3) . . . . ? C22 C23 C24 C19 0.0(3) . . . . ? C20 C19 C24 C23 0.4(3) . . . . ? C18 C19 C24 C23 -179.16(16) . . . . ? C9 C11 C26 C27 -160.25(14) . . . . ? C12 C11 C26 C27 74.64(19) . . . . ? C11 C26 C27 C28 -109.3(2) . . . . ? C11 C26 C27 C29 70.9(2) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.457 _refine_diff_density_min -0.335 _refine_diff_density_rms 0.055 data_asch126 _database_code_depnum_ccdc_archive 'CCDC 871297' #TrackingRef 'asch126.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H34 Cr O5' _chemical_formula_sum 'C30 H34 Cr O5' _chemical_formula_weight 526.57 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' Cr Cr 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.9498(5) _cell_length_b 11.2208(9) _cell_length_c 13.8926(11) _cell_angle_alpha 90.023(3) _cell_angle_beta 106.008(4) _cell_angle_gamma 104.171(5) _cell_volume 1296.78(16) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 7661 _cell_measurement_theta_min 1.53 _cell_measurement_theta_max 27.00 _exptl_crystal_description platelet _exptl_crystal_colour yellow _exptl_crystal_size_max .25 _exptl_crystal_size_mid .2 _exptl_crystal_size_min .03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.349 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 556 _exptl_absorpt_coefficient_mu 0.479 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'Nonius KappaCCD' _diffrn_measurement_method Phi/Omega-Scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7661 _diffrn_reflns_av_R_equivalents 0.0367 _diffrn_reflns_av_sigmaI/netI 0.0847 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.53 _diffrn_reflns_theta_max 27.00 _reflns_number_total 5462 _reflns_number_gt 3772 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius COLLECT' _computing_cell_refinement 'Nonius DENZO (Otwinowski, Minor 1997)' _computing_data_reduction 'Nonius DENZO (Otwinowski, Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SCHAKAL99 (E. Keller 1999)' _computing_publication_material 'PLATON (A. L. Spek 1980-2004)' _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^)+(0.0556P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5462 _refine_ls_number_parameters 329 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0735 _refine_ls_R_factor_gt 0.0415 _refine_ls_wR_factor_ref 0.1162 _refine_ls_wR_factor_gt 0.0976 _refine_ls_goodness_of_fit_ref 0.979 _refine_ls_restrained_S_all 0.979 _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 Cr1 Cr 0.49788(4) -0.07513(3) 0.25167(3) 0.01757(13) Uani 1 1 d . . . O1 O 0.2038(2) -0.10225(16) 0.32182(14) 0.0312(5) Uani 1 1 d . . . O2 O 0.4338(2) 0.16993(16) 0.19777(13) 0.0305(4) Uani 1 1 d . . . O3 O 0.2727(2) -0.19169(18) 0.05381(14) 0.0393(5) Uani 1 1 d . . . O4 O 0.77641(18) 0.21785(14) 0.38876(12) 0.0189(4) Uani 1 1 d . . . O5 O 0.56477(18) -0.22933(14) 0.45704(12) 0.0204(4) Uani 1 1 d . . . C1 C 0.3199(3) -0.0956(2) 0.29695(18) 0.0222(6) Uani 1 1 d . . . C2 C 0.4618(3) 0.0756(2) 0.21748(18) 0.0221(6) Uani 1 1 d . . . C3 C 0.3608(3) -0.1452(2) 0.1293(2) 0.0260(6) Uani 1 1 d . . . C4 C 0.7566(3) 0.0189(2) 0.31904(17) 0.0166(5) Uani 1 1 d . . . C5 C 0.7423(3) -0.0514(2) 0.23051(17) 0.0179(5) Uani 1 1 d . . . C6 C 0.6682(3) -0.1797(2) 0.22191(17) 0.0186(5) Uani 1 1 d . . . C7 C 0.6050(3) -0.2334(2) 0.29913(17) 0.0177(5) Uani 1 1 d . . . H7 H 0.5496 -0.3182 0.2910 0.021 Uiso 1 1 calc R . . C8 C 0.6224(3) -0.1646(2) 0.38674(18) 0.0174(5) Uani 1 1 d . . . C9 C 0.6958(3) -0.0371(2) 0.39637(17) 0.0169(5) Uani 1 1 d . . . H9 H 0.7046 0.0112 0.4548 0.020 Uiso 1 1 calc R . . C10 C 0.5509(3) -0.1623(2) 0.54050(18) 0.0232(6) Uani 1 1 d . . . H10A H 0.6579 -0.1155 0.5802 0.035 Uiso 1 1 calc R . . H10B H 0.5014 -0.2201 0.5825 0.035 Uiso 1 1 calc R . . H10C H 0.4838 -0.1054 0.5158 0.035 Uiso 1 1 calc R . . C11 C 0.6620(3) -0.2654(2) 0.13578(18) 0.0216(6) Uani 1 1 d . . . H11 H 0.5522 -0.3230 0.1134 0.026 Uiso 1 1 calc R . . C12 C 0.6948(3) -0.1956(2) 0.04599(18) 0.0255(6) Uani 1 1 d . . . H12A H 0.7176 -0.2513 -0.0003 0.031 Uiso 1 1 calc R . . H12B H 0.5976 -0.1698 0.0091 0.031 Uiso 1 1 calc R . . C13 C 0.8364(3) -0.0823(2) 0.07880(19) 0.0267(6) Uani 1 1 d . . . H13A H 0.9331 -0.1072 0.1177 0.032 Uiso 1 1 calc R . . H13B H 0.8596 -0.0431 0.0189 0.032 Uiso 1 1 calc R . . C14 C 0.7983(3) 0.0097(2) 0.14306(18) 0.0226(6) Uani 1 1 d . . . H14 H 0.7056 0.0371 0.0992 0.027 Uiso 1 1 calc R . . C15 C 0.9348(3) 0.1254(2) 0.18112(19) 0.0260(6) Uani 1 1 d . . . H15A H 0.9608 0.1689 0.1235 0.031 Uiso 1 1 calc R . . H15B H 1.0320 0.1024 0.2216 0.031 Uiso 1 1 calc R . . C16 C 0.8845(3) 0.2101(2) 0.24521(18) 0.0233(6) Uani 1 1 d . . . H16A H 0.7837 0.2285 0.2054 0.028 Uiso 1 1 calc R . . H16B H 0.9686 0.2888 0.2635 0.028 Uiso 1 1 calc R . . C17 C 0.8589(3) 0.1525(2) 0.34094(18) 0.0185(5) Uani 1 1 d . . . C18 C 0.8447(3) 0.3492(2) 0.40502(19) 0.0237(6) Uani 1 1 d . . . H18A H 0.7990 0.3899 0.3447 0.028 Uiso 1 1 calc R . . H18B H 0.9624 0.3676 0.4165 0.028 Uiso 1 1 calc R . . C19 C 0.8087(3) 0.3983(2) 0.49440(19) 0.0220(6) Uani 1 1 d . . . C20 C 0.8673(3) 0.3601(2) 0.58899(19) 0.0247(6) Uani 1 1 d . . . H20 H 0.9274 0.3000 0.5966 0.030 Uiso 1 1 calc R . . C21 C 0.8400(3) 0.4080(2) 0.6729(2) 0.0270(6) Uani 1 1 d . . . H21 H 0.8805 0.3792 0.7368 0.032 Uiso 1 1 calc R . . C22 C 0.7543(3) 0.4973(2) 0.6651(2) 0.0260(6) Uani 1 1 d . . . C23 C 0.6961(3) 0.5356(2) 0.5698(2) 0.0272(6) Uani 1 1 d . . . H23 H 0.6369 0.5963 0.5621 0.033 Uiso 1 1 calc R . . C24 C 0.7225(3) 0.4871(2) 0.4858(2) 0.0256(6) Uani 1 1 d . . . H24 H 0.6812 0.5151 0.4217 0.031 Uiso 1 1 calc R . . C25 C 0.7262(3) 0.5499(3) 0.7568(2) 0.0378(7) Uani 1 1 d . . . H25A H 0.6710 0.4829 0.7897 0.057 Uiso 1 1 calc R . . H25B H 0.6598 0.6082 0.7366 0.057 Uiso 1 1 calc R . . H25C H 0.8297 0.5925 0.8037 0.057 Uiso 1 1 calc R . . C26 C 1.0191(3) 0.1466(2) 0.41589(19) 0.0247(6) Uani 1 1 d . . . H26A H 1.0960 0.2275 0.4250 0.037 Uiso 1 1 calc R . . H26B H 1.0622 0.0852 0.3899 0.037 Uiso 1 1 calc R . . H26C H 1.0011 0.1233 0.4805 0.037 Uiso 1 1 calc R . . C27 C 0.7856(3) -0.3421(2) 0.17660(19) 0.0239(6) Uani 1 1 d . . . H27A H 0.8951 -0.2891 0.1848 0.029 Uiso 1 1 calc R . . H27B H 0.7785 -0.3675 0.2438 0.029 Uiso 1 1 calc R . . C28 C 0.7614(3) -0.4554(2) 0.11013(19) 0.0265(6) Uani 1 1 d . . . C29 C 0.6231(3) -0.5608(2) 0.1120(2) 0.0317(7) Uani 1 1 d . . . H29A H 0.6230 -0.6316 0.0706 0.048 Uiso 1 1 calc R . . H29B H 0.5223 -0.5366 0.0854 0.048 Uiso 1 1 calc R . . H29C H 0.6334 -0.5833 0.1813 0.048 Uiso 1 1 calc R . . C30 C 0.8576(3) -0.4605(3) 0.0533(2) 0.0429(8) Uani 1 1 d . . . H30A H 0.8395 -0.5330 0.0119 0.052 Uiso 1 1 calc R . . H30B H 0.9444 -0.3916 0.0541 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 Cr1 0.0169(2) 0.0163(2) 0.0181(2) -0.00136(16) 0.00415(15) 0.00260(16) O1 0.0233(10) 0.0305(11) 0.0432(12) 0.0024(9) 0.0153(9) 0.0062(8) O2 0.0371(11) 0.0223(10) 0.0328(11) 0.0069(9) 0.0083(8) 0.0107(9) O3 0.0389(11) 0.0395(12) 0.0284(12) -0.0104(10) -0.0075(9) 0.0087(9) O4 0.0196(8) 0.0130(9) 0.0237(10) -0.0036(7) 0.0088(7) 0.0005(7) O5 0.0274(9) 0.0161(9) 0.0184(9) 0.0023(7) 0.0090(7) 0.0037(7) C1 0.0242(14) 0.0173(13) 0.0216(14) 0.0019(11) 0.0025(11) 0.0037(11) C2 0.0209(13) 0.0260(15) 0.0177(13) -0.0011(12) 0.0058(10) 0.0024(11) C3 0.0278(14) 0.0238(15) 0.0286(16) 0.0003(12) 0.0088(12) 0.0096(12) C4 0.0129(11) 0.0145(13) 0.0205(13) -0.0005(10) 0.0023(9) 0.0031(9) C5 0.0161(12) 0.0193(13) 0.0177(13) 0.0003(10) 0.0041(10) 0.0041(10) C6 0.0169(12) 0.0200(13) 0.0186(13) -0.0001(10) 0.0029(10) 0.0065(10) C7 0.0185(12) 0.0138(12) 0.0199(13) 0.0000(10) 0.0053(10) 0.0025(10) C8 0.0143(12) 0.0198(13) 0.0191(13) 0.0024(10) 0.0056(9) 0.0055(10) C9 0.0167(12) 0.0179(13) 0.0157(13) -0.0032(10) 0.0042(9) 0.0043(10) C10 0.0258(13) 0.0217(14) 0.0255(15) 0.0003(11) 0.0127(11) 0.0059(11) C11 0.0231(13) 0.0199(13) 0.0201(14) -0.0041(11) 0.0044(10) 0.0044(11) C12 0.0322(14) 0.0253(15) 0.0199(14) -0.0039(11) 0.0094(11) 0.0066(12) C13 0.0293(14) 0.0311(16) 0.0223(15) 0.0007(12) 0.0132(11) 0.0058(12) C14 0.0248(13) 0.0228(14) 0.0200(14) -0.0002(11) 0.0092(11) 0.0027(11) C15 0.0234(13) 0.0269(15) 0.0278(15) 0.0000(12) 0.0115(11) 0.0019(11) C16 0.0219(13) 0.0185(14) 0.0279(15) 0.0005(11) 0.0093(11) -0.0002(11) C17 0.0171(12) 0.0163(13) 0.0216(14) -0.0006(10) 0.0056(10) 0.0032(10) C18 0.0274(14) 0.0162(13) 0.0257(15) 0.0002(11) 0.0077(11) 0.0019(11) C19 0.0211(13) 0.0138(13) 0.0275(15) -0.0033(11) 0.0056(11) -0.0008(10) C20 0.0225(13) 0.0209(14) 0.0302(16) -0.0008(12) 0.0059(11) 0.0061(11) C21 0.0247(14) 0.0282(15) 0.0252(15) -0.0013(12) 0.0056(11) 0.0032(12) C22 0.0197(13) 0.0180(13) 0.0387(17) -0.0067(12) 0.0126(12) -0.0032(11) C23 0.0213(13) 0.0164(13) 0.0437(18) -0.0040(12) 0.0113(12) 0.0019(11) C24 0.0226(13) 0.0179(14) 0.0321(16) 0.0002(12) 0.0052(11) 0.0005(11) C25 0.0375(16) 0.0305(16) 0.0466(19) -0.0123(14) 0.0224(14) -0.0010(13) C26 0.0193(13) 0.0190(14) 0.0308(15) -0.0013(11) 0.0030(11) 0.0000(11) C27 0.0227(13) 0.0250(15) 0.0227(14) -0.0048(12) 0.0042(11) 0.0065(11) C28 0.0267(14) 0.0276(15) 0.0241(15) -0.0046(12) 0.0010(11) 0.0119(12) C29 0.0385(16) 0.0248(15) 0.0279(16) -0.0048(12) 0.0027(12) 0.0087(13) C30 0.0384(17) 0.051(2) 0.044(2) -0.0130(16) 0.0143(14) 0.0165(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 Cr1 C1 1.833(3) . ? Cr1 C2 1.837(3) . ? Cr1 C3 1.841(3) . ? Cr1 C4 2.227(2) . ? Cr1 C7 2.235(2) . ? Cr1 C5 2.239(2) . ? Cr1 C9 2.242(2) . ? Cr1 C6 2.256(2) . ? Cr1 C8 2.273(2) . ? O1 C1 1.168(3) . ? O2 C2 1.161(3) . ? O3 C3 1.156(3) . ? O4 C17 1.435(3) . ? O4 C18 1.442(3) . ? O5 C8 1.357(3) . ? O5 C10 1.432(3) . ? C4 C9 1.414(3) . ? C4 C5 1.419(3) . ? C4 C17 1.534(3) . ? C5 C6 1.420(3) . ? C5 C14 1.538(3) . ? C6 C7 1.415(3) . ? C6 C11 1.516(3) . ? C7 C8 1.392(3) . ? C7 H7 0.9500 . ? C8 C9 1.409(3) . ? C9 H9 0.9500 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.531(3) . ? C11 C27 1.551(3) . ? C11 H11 1.0000 . ? C12 C13 1.525(3) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.523(3) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.524(3) . ? C14 H14 1.0000 . ? C15 C16 1.525(3) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.528(3) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C26 1.539(3) . ? C18 C19 1.502(3) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.384(4) . ? C19 C24 1.388(3) . ? C20 C21 1.389(3) . ? C20 H20 0.9500 . ? C21 C22 1.391(3) . ? C21 H21 0.9500 . ? C22 C23 1.391(4) . ? C22 C25 1.512(3) . ? C23 C24 1.389(3) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C28 1.507(3) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 C30 1.329(4) . ? C28 C29 1.494(4) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9500 . ? C30 H30B 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 C1 Cr1 C2 84.62(11) . . ? C1 Cr1 C3 87.33(11) . . ? C2 Cr1 C3 89.87(11) . . ? C1 Cr1 C4 133.16(10) . . ? C2 Cr1 C4 88.57(9) . . ? C3 Cr1 C4 139.05(10) . . ? C1 Cr1 C7 107.32(10) . . ? C2 Cr1 C7 165.87(9) . . ? C3 Cr1 C7 98.07(10) . . ? C4 Cr1 C7 77.76(8) . . ? C1 Cr1 C5 167.92(10) . . ? C2 Cr1 C5 100.37(10) . . ? C3 Cr1 C5 103.58(9) . . ? C4 Cr1 C5 37.04(8) . . ? C7 Cr1 C5 66.47(9) . . ? C1 Cr1 C9 101.42(9) . . ? C2 Cr1 C9 105.43(10) . . ? C3 Cr1 C9 162.91(10) . . ? C4 Cr1 C9 36.90(8) . . ? C7 Cr1 C9 65.42(8) . . ? C5 Cr1 C9 66.70(8) . . ? C1 Cr1 C6 141.48(10) . . ? C2 Cr1 C6 133.27(10) . . ? C3 Cr1 C6 86.28(9) . . ? C4 Cr1 C6 65.95(8) . . ? C7 Cr1 C6 36.73(8) . . ? C5 Cr1 C6 36.82(8) . . ? C9 Cr1 C6 77.71(8) . . ? C1 Cr1 C8 90.84(9) . . ? C2 Cr1 C8 139.56(10) . . ? C3 Cr1 C8 130.13(10) . . ? C4 Cr1 C8 65.82(8) . . ? C7 Cr1 C8 35.97(8) . . ? C5 Cr1 C8 78.20(8) . . ? C9 Cr1 C8 36.37(8) . . ? C6 Cr1 C8 65.43(8) . . ? C17 O4 C18 114.88(16) . . ? C8 O5 C10 118.27(18) . . ? O1 C1 Cr1 175.4(2) . . ? O2 C2 Cr1 177.2(2) . . ? O3 C3 Cr1 178.2(2) . . ? C9 C4 C5 120.8(2) . . ? C9 C4 C17 117.4(2) . . ? C5 C4 C17 121.2(2) . . ? C9 C4 Cr1 72.14(13) . . ? C5 C4 Cr1 71.94(12) . . ? C17 C4 Cr1 136.26(16) . . ? C4 C5 C6 118.6(2) . . ? C4 C5 C14 121.4(2) . . ? C6 C5 C14 120.0(2) . . ? C4 C5 Cr1 71.02(12) . . ? C6 C5 Cr1 72.27(13) . . ? C14 C5 Cr1 125.72(16) . . ? C7 C6 C5 119.7(2) . . ? C7 C6 C11 117.3(2) . . ? C5 C6 C11 122.9(2) . . ? C7 C6 Cr1 70.80(13) . . ? C5 C6 Cr1 70.91(13) . . ? C11 C6 Cr1 134.06(16) . . ? C8 C7 C6 121.4(2) . . ? C8 C7 Cr1 73.50(14) . . ? C6 C7 Cr1 72.47(14) . . ? C8 C7 H7 119.3 . . ? C6 C7 H7 119.3 . . ? Cr1 C7 H7 126.7 . . ? O5 C8 C7 115.2(2) . . ? O5 C8 C9 125.4(2) . . ? C7 C8 C9 119.4(2) . . ? O5 C8 Cr1 131.08(15) . . ? C7 C8 Cr1 70.53(14) . . ? C9 C8 Cr1 70.64(14) . . ? C8 C9 C4 120.0(2) . . ? C8 C9 Cr1 72.99(13) . . ? C4 C9 Cr1 70.96(13) . . ? C8 C9 H9 120.0 . . ? C4 C9 H9 120.0 . . ? Cr1 C9 H9 128.2 . . ? O5 C10 H10A 109.5 . . ? O5 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? O5 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C6 C11 C12 112.3(2) . . ? C6 C11 C27 107.60(19) . . ? C12 C11 C27 111.6(2) . . ? C6 C11 H11 108.4 . . ? C12 C11 H11 108.4 . . ? C27 C11 H11 108.4 . . ? C13 C12 C11 111.7(2) . . ? C13 C12 H12A 109.3 . . ? C11 C12 H12A 109.3 . . ? C13 C12 H12B 109.3 . . ? C11 C12 H12B 109.3 . . ? H12A C12 H12B 107.9 . . ? C14 C13 C12 110.2(2) . . ? C14 C13 H13A 109.6 . . ? C12 C13 H13A 109.6 . . ? C14 C13 H13B 109.6 . . ? C12 C13 H13B 109.6 . . ? H13A C13 H13B 108.1 . . ? C13 C14 C15 114.0(2) . . ? C13 C14 C5 111.4(2) . . ? C15 C14 C5 110.8(2) . . ? C13 C14 H14 106.7 . . ? C15 C14 H14 106.7 . . ? C5 C14 H14 106.7 . . ? C14 C15 C16 109.57(19) . . ? C14 C15 H15A 109.8 . . ? C16 C15 H15A 109.8 . . ? C14 C15 H15B 109.8 . . ? C16 C15 H15B 109.8 . . ? H15A C15 H15B 108.2 . . ? C15 C16 C17 112.1(2) . . ? C15 C16 H16A 109.2 . . ? C17 C16 H16A 109.2 . . ? C15 C16 H16B 109.2 . . ? C17 C16 H16B 109.2 . . ? H16A C16 H16B 107.9 . . ? O4 C17 C16 111.86(19) . . ? O4 C17 C4 106.54(17) . . ? C16 C17 C4 111.59(19) . . ? O4 C17 C26 109.46(19) . . ? C16 C17 C26 111.50(19) . . ? C4 C17 C26 105.6(2) . . ? O4 C18 C19 109.99(19) . . ? O4 C18 H18A 109.7 . . ? C19 C18 H18A 109.7 . . ? O4 C18 H18B 109.7 . . ? C19 C18 H18B 109.7 . . ? H18A C18 H18B 108.2 . . ? C20 C19 C24 118.0(2) . . ? C20 C19 C18 120.6(2) . . ? C24 C19 C18 121.3(2) . . ? C19 C20 C21 121.3(2) . . ? C19 C20 H20 119.4 . . ? C21 C20 H20 119.4 . . ? C20 C21 C22 121.1(3) . . ? C20 C21 H21 119.4 . . ? C22 C21 H21 119.4 . . ? C21 C22 C23 117.3(2) . . ? C21 C22 C25 120.9(3) . . ? C23 C22 C25 121.8(2) . . ? C24 C23 C22 121.6(2) . . ? C24 C23 H23 119.2 . . ? C22 C23 H23 119.2 . . ? C19 C24 C23 120.7(3) . . ? C19 C24 H24 119.7 . . ? C23 C24 H24 119.7 . . ? C22 C25 H25A 109.5 . . ? C22 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C22 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C17 C26 H26A 109.5 . . ? C17 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C17 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C28 C27 C11 113.9(2) . . ? C28 C27 H27A 108.8 . . ? C11 C27 H27A 108.8 . . ? C28 C27 H27B 108.8 . . ? C11 C27 H27B 108.8 . . ? H27A C27 H27B 107.7 . . ? C30 C28 C29 122.4(2) . . ? C30 C28 C27 121.7(3) . . ? C29 C28 C27 115.9(2) . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C28 C30 H30A 120.0 . . ? C28 C30 H30B 120.0 . . ? H30A C30 H30B 120.0 . . ? 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 C2 Cr1 C1 O1 18(3) . . . . ? C3 Cr1 C1 O1 -72(3) . . . . ? C4 Cr1 C1 O1 101(3) . . . . ? C7 Cr1 C1 O1 -169(3) . . . . ? C5 Cr1 C1 O1 133(2) . . . . ? C9 Cr1 C1 O1 123(3) . . . . ? C6 Cr1 C1 O1 -152(3) . . . . ? C8 Cr1 C1 O1 158(3) . . . . ? C1 Cr1 C2 O2 5(5) . . . . ? C3 Cr1 C2 O2 92(5) . . . . ? C4 Cr1 C2 O2 -128(5) . . . . ? C7 Cr1 C2 O2 -143(4) . . . . ? C5 Cr1 C2 O2 -164(5) . . . . ? C9 Cr1 C2 O2 -95(5) . . . . ? C6 Cr1 C2 O2 177(100) . . . . ? C8 Cr1 C2 O2 -80(5) . . . . ? C1 Cr1 C3 O3 -47(7) . . . . ? C2 Cr1 C3 O3 -132(7) . . . . ? C4 Cr1 C3 O3 140(7) . . . . ? C7 Cr1 C3 O3 60(7) . . . . ? C5 Cr1 C3 O3 127(7) . . . . ? C9 Cr1 C3 O3 74(8) . . . . ? C6 Cr1 C3 O3 95(7) . . . . ? C8 Cr1 C3 O3 42(8) . . . . ? C1 Cr1 C4 C9 37.20(19) . . . . ? C2 Cr1 C4 C9 118.45(15) . . . . ? C3 Cr1 C4 C9 -153.39(16) . . . . ? C7 Cr1 C4 C9 -65.17(14) . . . . ? C5 Cr1 C4 C9 -132.2(2) . . . . ? C6 Cr1 C4 C9 -101.91(15) . . . . ? C8 Cr1 C4 C9 -29.29(13) . . . . ? C1 Cr1 C4 C5 169.36(15) . . . . ? C2 Cr1 C4 C5 -109.38(15) . . . . ? C3 Cr1 C4 C5 -21.2(2) . . . . ? C7 Cr1 C4 C5 67.00(14) . . . . ? C9 Cr1 C4 C5 132.2(2) . . . . ? C6 Cr1 C4 C5 30.25(13) . . . . ? C8 Cr1 C4 C5 102.87(15) . . . . ? C1 Cr1 C4 C17 -74.1(3) . . . . ? C2 Cr1 C4 C17 7.2(2) . . . . ? C3 Cr1 C4 C17 95.3(3) . . . . ? C7 Cr1 C4 C17 -176.4(2) . . . . ? C5 Cr1 C4 C17 116.6(3) . . . . ? C9 Cr1 C4 C17 -111.3(3) . . . . ? C6 Cr1 C4 C17 146.8(3) . . . . ? C8 Cr1 C4 C17 -140.6(2) . . . . ? C9 C4 C5 C6 -1.1(3) . . . . ? C17 C4 C5 C6 169.9(2) . . . . ? Cr1 C4 C5 C6 -56.36(19) . . . . ? C9 C4 C5 C14 176.1(2) . . . . ? C17 C4 C5 C14 -12.8(3) . . . . ? Cr1 C4 C5 C14 120.9(2) . . . . ? C9 C4 C5 Cr1 55.24(19) . . . . ? C17 C4 C5 Cr1 -133.7(2) . . . . ? C1 Cr1 C5 C4 -40.1(5) . . . . ? C2 Cr1 C5 C4 73.47(15) . . . . ? C3 Cr1 C5 C4 165.87(15) . . . . ? C7 Cr1 C5 C4 -101.14(15) . . . . ? C9 Cr1 C5 C4 -28.98(13) . . . . ? C6 Cr1 C5 C4 -129.9(2) . . . . ? C8 Cr1 C5 C4 -65.31(14) . . . . ? C1 Cr1 C5 C6 89.8(5) . . . . ? C2 Cr1 C5 C6 -156.67(15) . . . . ? C3 Cr1 C5 C6 -64.28(16) . . . . ? C4 Cr1 C5 C6 129.9(2) . . . . ? C7 Cr1 C5 C6 28.72(13) . . . . ? C9 Cr1 C5 C6 100.87(15) . . . . ? C8 Cr1 C5 C6 64.55(14) . . . . ? C1 Cr1 C5 C14 -155.6(4) . . . . ? C2 Cr1 C5 C14 -42.0(2) . . . . ? C3 Cr1 C5 C14 50.4(2) . . . . ? C4 Cr1 C5 C14 -115.5(2) . . . . ? C7 Cr1 C5 C14 143.4(2) . . . . ? C9 Cr1 C5 C14 -144.5(2) . . . . ? C6 Cr1 C5 C14 114.6(2) . . . . ? C8 Cr1 C5 C14 179.2(2) . . . . ? C4 C5 C6 C7 2.5(3) . . . . ? C14 C5 C6 C7 -174.8(2) . . . . ? Cr1 C5 C6 C7 -53.2(2) . . . . ? C4 C5 C6 C11 -173.5(2) . . . . ? C14 C5 C6 C11 9.2(3) . . . . ? Cr1 C5 C6 C11 130.7(2) . . . . ? C4 C5 C6 Cr1 55.74(19) . . . . ? C14 C5 C6 Cr1 -121.5(2) . . . . ? C1 Cr1 C6 C7 -27.8(2) . . . . ? C2 Cr1 C6 C7 164.89(14) . . . . ? C3 Cr1 C6 C7 -108.80(15) . . . . ? C4 Cr1 C6 C7 102.12(15) . . . . ? C5 Cr1 C6 C7 132.6(2) . . . . ? C9 Cr1 C6 C7 65.16(14) . . . . ? C8 Cr1 C6 C7 28.93(13) . . . . ? C1 Cr1 C6 C5 -160.36(16) . . . . ? C2 Cr1 C6 C5 32.3(2) . . . . ? C3 Cr1 C6 C5 118.65(15) . . . . ? C4 Cr1 C6 C5 -30.43(13) . . . . ? C7 Cr1 C6 C5 -132.6(2) . . . . ? C9 Cr1 C6 C5 -67.39(14) . . . . ? C8 Cr1 C6 C5 -103.63(15) . . . . ? C1 Cr1 C6 C11 82.0(3) . . . . ? C2 Cr1 C6 C11 -85.3(3) . . . . ? C3 Cr1 C6 C11 1.0(2) . . . . ? C4 Cr1 C6 C11 -148.1(3) . . . . ? C7 Cr1 C6 C11 109.8(3) . . . . ? C5 Cr1 C6 C11 -117.7(3) . . . . ? C9 Cr1 C6 C11 175.0(2) . . . . ? C8 Cr1 C6 C11 138.7(2) . . . . ? C5 C6 C7 C8 -3.9(3) . . . . ? C11 C6 C7 C8 172.3(2) . . . . ? Cr1 C6 C7 C8 -57.2(2) . . . . ? C5 C6 C7 Cr1 53.3(2) . . . . ? C11 C6 C7 Cr1 -130.5(2) . . . . ? C1 Cr1 C7 C8 -66.21(15) . . . . ? C2 Cr1 C7 C8 80.5(4) . . . . ? C3 Cr1 C7 C8 -155.92(14) . . . . ? C4 Cr1 C7 C8 65.51(13) . . . . ? C5 Cr1 C7 C8 102.73(14) . . . . ? C9 Cr1 C7 C8 28.70(13) . . . . ? C6 Cr1 C7 C8 131.5(2) . . . . ? C1 Cr1 C7 C6 162.28(14) . . . . ? C2 Cr1 C7 C6 -51.0(4) . . . . ? C3 Cr1 C7 C6 72.57(15) . . . . ? C4 Cr1 C7 C6 -66.00(14) . . . . ? C5 Cr1 C7 C6 -28.78(13) . . . . ? C9 Cr1 C7 C6 -102.81(15) . . . . ? C8 Cr1 C7 C6 -131.5(2) . . . . ? C10 O5 C8 C7 -168.59(19) . . . . ? C10 O5 C8 C9 11.5(3) . . . . ? C10 O5 C8 Cr1 -83.1(2) . . . . ? C6 C7 C8 O5 -176.1(2) . . . . ? Cr1 C7 C8 O5 127.15(19) . . . . ? C6 C7 C8 C9 3.8(3) . . . . ? Cr1 C7 C8 C9 -52.91(19) . . . . ? C6 C7 C8 Cr1 56.7(2) . . . . ? C1 Cr1 C8 O5 12.3(2) . . . . ? C2 Cr1 C8 O5 94.9(2) . . . . ? C3 Cr1 C8 O5 -75.0(2) . . . . ? C4 Cr1 C8 O5 150.3(2) . . . . ? C7 Cr1 C8 O5 -106.9(3) . . . . ? C5 Cr1 C8 O5 -172.9(2) . . . . ? C9 Cr1 C8 O5 120.6(3) . . . . ? C6 Cr1 C8 O5 -136.3(2) . . . . ? C1 Cr1 C8 C7 119.12(14) . . . . ? C2 Cr1 C8 C7 -158.21(15) . . . . ? C3 Cr1 C8 C7 31.90(18) . . . . ? C4 Cr1 C8 C7 -102.88(14) . . . . ? C5 Cr1 C8 C7 -66.01(13) . . . . ? C9 Cr1 C8 C7 -132.57(19) . . . . ? C6 Cr1 C8 C7 -29.50(13) . . . . ? C1 Cr1 C8 C9 -108.31(14) . . . . ? C2 Cr1 C8 C9 -25.6(2) . . . . ? C3 Cr1 C8 C9 164.47(14) . . . . ? C4 Cr1 C8 C9 29.70(13) . . . . ? C7 Cr1 C8 C9 132.57(19) . . . . ? C5 Cr1 C8 C9 66.57(13) . . . . ? C6 Cr1 C8 C9 103.08(14) . . . . ? O5 C8 C9 C4 177.6(2) . . . . ? C7 C8 C9 C4 -2.4(3) . . . . ? Cr1 C8 C9 C4 -55.23(19) . . . . ? O5 C8 C9 Cr1 -127.2(2) . . . . ? C7 C8 C9 Cr1 52.86(19) . . . . ? C5 C4 C9 C8 1.1(3) . . . . ? C17 C4 C9 C8 -170.3(2) . . . . ? Cr1 C4 C9 C8 56.20(19) . . . . ? C5 C4 C9 Cr1 -55.14(19) . . . . ? C17 C4 C9 Cr1 133.5(2) . . . . ? C1 Cr1 C9 C8 75.57(14) . . . . ? C2 Cr1 C9 C8 163.07(13) . . . . ? C3 Cr1 C9 C8 -44.1(4) . . . . ? C4 Cr1 C9 C8 -131.2(2) . . . . ? C7 Cr1 C9 C8 -28.41(12) . . . . ? C5 Cr1 C9 C8 -102.08(14) . . . . ? C6 Cr1 C9 C8 -65.05(13) . . . . ? C1 Cr1 C9 C4 -153.26(14) . . . . ? C2 Cr1 C9 C4 -65.75(15) . . . . ? C3 Cr1 C9 C4 87.0(4) . . . . ? C7 Cr1 C9 C4 102.77(14) . . . . ? C5 Cr1 C9 C4 29.09(13) . . . . ? C6 Cr1 C9 C4 66.13(14) . . . . ? C8 Cr1 C9 C4 131.2(2) . . . . ? C7 C6 C11 C12 166.1(2) . . . . ? C5 C6 C11 C12 -17.8(3) . . . . ? Cr1 C6 C11 C12 77.0(3) . . . . ? C7 C6 C11 C27 -70.8(3) . . . . ? C5 C6 C11 C27 105.3(3) . . . . ? Cr1 C6 C11 C27 -159.87(18) . . . . ? C6 C11 C12 C13 44.3(3) . . . . ? C27 C11 C12 C13 -76.6(3) . . . . ? C11 C12 C13 C14 -63.7(3) . . . . ? C12 C13 C14 C15 178.9(2) . . . . ? C12 C13 C14 C5 52.6(3) . . . . ? C4 C5 C14 C13 156.4(2) . . . . ? C6 C5 C14 C13 -26.4(3) . . . . ? Cr1 C5 C14 C13 -115.4(2) . . . . ? C4 C5 C14 C15 28.4(3) . . . . ? C6 C5 C14 C15 -154.4(2) . . . . ? Cr1 C5 C14 C15 116.6(2) . . . . ? C13 C14 C15 C16 -179.4(2) . . . . ? C5 C14 C15 C16 -52.8(3) . . . . ? C14 C15 C16 C17 65.0(3) . . . . ? C18 O4 C17 C16 -51.0(2) . . . . ? C18 O4 C17 C4 -173.17(19) . . . . ? C18 O4 C17 C26 73.1(2) . . . . ? C15 C16 C17 O4 -166.34(18) . . . . ? C15 C16 C17 C4 -47.1(3) . . . . ? C15 C16 C17 C26 70.7(3) . . . . ? C9 C4 C17 O4 -44.9(3) . . . . ? C5 C4 C17 O4 143.7(2) . . . . ? Cr1 C4 C17 O4 47.5(3) . . . . ? C9 C4 C17 C16 -167.3(2) . . . . ? C5 C4 C17 C16 21.4(3) . . . . ? Cr1 C4 C17 C16 -74.9(3) . . . . ? C9 C4 C17 C26 71.4(2) . . . . ? C5 C4 C17 C26 -99.9(2) . . . . ? Cr1 C4 C17 C26 163.83(18) . . . . ? C17 O4 C18 C19 -152.2(2) . . . . ? O4 C18 C19 C20 62.6(3) . . . . ? O4 C18 C19 C24 -120.4(2) . . . . ? C24 C19 C20 C21 0.5(3) . . . . ? C18 C19 C20 C21 177.7(2) . . . . ? C19 C20 C21 C22 -0.8(4) . . . . ? C20 C21 C22 C23 0.6(4) . . . . ? C20 C21 C22 C25 -179.5(2) . . . . ? C21 C22 C23 C24 -0.2(4) . . . . ? C25 C22 C23 C24 179.9(2) . . . . ? C20 C19 C24 C23 -0.1(3) . . . . ? C18 C19 C24 C23 -177.2(2) . . . . ? C22 C23 C24 C19 -0.1(4) . . . . ? C6 C11 C27 C28 163.3(2) . . . . ? C12 C11 C27 C28 -73.2(3) . . . . ? C11 C27 C28 C30 105.1(3) . . . . ? C11 C27 C28 C29 -74.7(3) . . . . ? _diffrn_measured_fraction_theta_max 0.964 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.964 _refine_diff_density_max 0.379 _refine_diff_density_min -0.487 _refine_diff_density_rms 0.079 data_asch166 _database_code_depnum_ccdc_archive 'CCDC 871298' #TrackingRef 'asch166.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H31 Cr F3 O5' _chemical_formula_sum 'C30 H31 Cr F3 O5' _chemical_formula_weight 580.55 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cr Cr 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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 orthorhombic _symmetry_space_group_name_H-M Fdd2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x+1/4, y+1/4, z+1/4' 'x+3/4, -y+3/4, z+1/4' 'x, y+1/2, z+1/2' '-x, -y+1/2, z+1/2' '-x+1/4, y+3/4, z+3/4' 'x+3/4, -y+5/4, z+3/4' 'x+1/2, y, z+1/2' '-x+1/2, -y, z+1/2' '-x+3/4, y+1/4, z+3/4' 'x+5/4, -y+3/4, z+3/4' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z' '-x+3/4, y+3/4, z+1/4' 'x+5/4, -y+5/4, z+1/4' _cell_length_a 32.4358(19) _cell_length_b 34.600(2) _cell_length_c 9.8268(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 11028.4(11) _cell_formula_units_Z 16 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 10633 _cell_measurement_theta_min 1.72 _cell_measurement_theta_max 27.00 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max .2 _exptl_crystal_size_mid .1 _exptl_crystal_size_min .03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.399 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4832 _exptl_absorpt_coefficient_mu 0.473 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'Nonius KappaCCD' _diffrn_measurement_method Phi/Omega-Scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10633 _diffrn_reflns_av_R_equivalents 0.0370 _diffrn_reflns_av_sigmaI/netI 0.0539 _diffrn_reflns_limit_h_min -40 _diffrn_reflns_limit_h_max 33 _diffrn_reflns_limit_k_min -44 _diffrn_reflns_limit_k_max 43 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 1.72 _diffrn_reflns_theta_max 27.00 _reflns_number_total 4737 _reflns_number_gt 3933 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius COLLECT' _computing_cell_refinement 'Nonius DENZO (Otwinowski, Minor 1997)' _computing_data_reduction 'Nonius DENZO (Otwinowski, Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SCHAKAL99 (E. Keller 1999)' _computing_publication_material 'PLATON (A. L. Spek 1980-2004)' _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^)+(0.0348P)^2^+12.3533P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.001(19) _refine_ls_number_reflns 4737 _refine_ls_number_parameters 355 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0545 _refine_ls_R_factor_gt 0.0385 _refine_ls_wR_factor_ref 0.0836 _refine_ls_wR_factor_gt 0.0781 _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 Cr1 Cr 0.055939(15) 0.175964(12) 0.49883(5) 0.01956(12) Uani 1 1 d . . . F1 F 0.23498(11) 0.16731(7) 0.0823(3) 0.0887(10) Uani 1 1 d . . . F2 F 0.23883(10) 0.18956(7) 0.2766(3) 0.0853(10) Uani 1 1 d . . . F3 F 0.18119(7) 0.18515(7) 0.1803(5) 0.1224(16) Uani 1 1 d . . . O1 O 0.13773(7) 0.21571(6) 0.5337(3) 0.0338(6) Uani 1 1 d . . . O2 O 0.01355(7) 0.24291(6) 0.3665(2) 0.0305(6) Uani 1 1 d . . . O3 O 0.08163(7) 0.15913(6) 0.2124(2) 0.0295(5) Uani 1 1 d . . . O4 O 0.08832(7) 0.17231(6) 0.8187(2) 0.0255(5) Uani 1 1 d . . . O5 O 0.10257(6) 0.08627(5) 0.4329(2) 0.0240(5) Uani 1 1 d . . . C1 C 0.10533(10) 0.20099(8) 0.5198(3) 0.0240(7) Uani 1 1 d . . . C2 C 0.03068(10) 0.21769(9) 0.4210(3) 0.0240(7) Uani 1 1 d . . . C3 C 0.07205(10) 0.16423(8) 0.3251(4) 0.0228(7) Uani 1 1 d . . . C4 C 0.06057(9) 0.16081(8) 0.7231(3) 0.0210(7) Uani 1 1 d . . . C5 C 0.08516(10) 0.21044(9) 0.8722(4) 0.0299(8) Uani 1 1 d . . . H5A H 0.0854 0.2291 0.7973 0.045 Uiso 1 1 calc R . . H5B H 0.1085 0.2155 0.9328 0.045 Uiso 1 1 calc R . . H5C H 0.0594 0.2130 0.9234 0.045 Uiso 1 1 calc R . . C6 C 0.07230(10) 0.12868(8) 0.6452(3) 0.0210(7) Uani 1 1 d . . . H6 H 0.0984 0.1170 0.6611 0.025 Uiso 1 1 calc R . . C7 C 0.04643(9) 0.11347(8) 0.5443(3) 0.0202(7) Uani 1 1 d . . . C8 C 0.00709(9) 0.13085(8) 0.5184(3) 0.0198(7) Uani 1 1 d . . . C9 C -0.00451(9) 0.16339(8) 0.5964(3) 0.0193(7) Uani 1 1 d . . . C10 C 0.02261(9) 0.17868(8) 0.6984(3) 0.0205(7) Uani 1 1 d . . . H10 H 0.0148 0.2009 0.7490 0.025 Uiso 1 1 calc R . . C11 C -0.04680(10) 0.18207(8) 0.5832(3) 0.0220(7) Uani 1 1 d . . . H11 H -0.0429 0.2107 0.5802 0.026 Uiso 1 1 calc R . . C12 C -0.06858(10) 0.16975(8) 0.4527(3) 0.0244(7) Uani 1 1 d . . . H12A H -0.0564 0.1838 0.3747 0.029 Uiso 1 1 calc R . . H12B H -0.0981 0.1770 0.4585 0.029 Uiso 1 1 calc R . . C13 C -0.06508(10) 0.12624(9) 0.4279(3) 0.0263(8) Uani 1 1 d . . . H13A H -0.0757 0.1120 0.5079 0.032 Uiso 1 1 calc R . . H13B H -0.0818 0.1189 0.3477 0.032 Uiso 1 1 calc R . . C14 C -0.02032(9) 0.11578(8) 0.4038(3) 0.0229(7) Uani 1 1 d . . . H14 H -0.0117 0.1297 0.3193 0.027 Uiso 1 1 calc R . . C15 C -0.01180(10) 0.07300(8) 0.3790(4) 0.0272(8) Uani 1 1 d . . . H15A H -0.0287 0.0637 0.3017 0.033 Uiso 1 1 calc R . . H15B H -0.0194 0.0579 0.4607 0.033 Uiso 1 1 calc R . . C16 C 0.03405(10) 0.06714(9) 0.3473(3) 0.0259(8) Uani 1 1 d . . . H16A H 0.0421 0.0840 0.2702 0.031 Uiso 1 1 calc R . . H16B H 0.0388 0.0400 0.3200 0.031 Uiso 1 1 calc R . . C17 C 0.06080(9) 0.07674(8) 0.4714(3) 0.0224(7) Uani 1 1 d . . . C18 C 0.12514(10) 0.05810(8) 0.3586(4) 0.0257(7) Uani 1 1 d . . . H18A H 0.1110 0.0522 0.2718 0.031 Uiso 1 1 calc R . . H18B H 0.1275 0.0339 0.4120 0.031 Uiso 1 1 calc R . . C19 C 0.16737(10) 0.07474(9) 0.3314(3) 0.0244(7) Uani 1 1 d . . . C20 C 0.17172(10) 0.11257(9) 0.2831(3) 0.0253(8) Uani 1 1 d . . . H20 H 0.1480 0.1281 0.2684 0.030 Uiso 1 1 calc R . . C21 C 0.21061(10) 0.12747(8) 0.2566(4) 0.0259(7) Uani 1 1 d . . . C22 C 0.21503(11) 0.16705(10) 0.2005(4) 0.0366(9) Uani 1 1 d . . . C23 C 0.24575(10) 0.10541(9) 0.2803(3) 0.0285(8) Uani 1 1 d . . . H23 H 0.2724 0.1158 0.2630 0.034 Uiso 1 1 calc R . . C24 C 0.24138(11) 0.06832(9) 0.3293(3) 0.0295(8) Uani 1 1 d . . . H24 H 0.2652 0.0532 0.3468 0.035 Uiso 1 1 calc R . . C25 C 0.20258(10) 0.05278(9) 0.3534(3) 0.0266(7) Uani 1 1 d . . . H25 H 0.2001 0.0269 0.3852 0.032 Uiso 1 1 calc R . . C26 C 0.06019(10) 0.04320(8) 0.5747(4) 0.0293(8) Uani 1 1 d . . . H26A H 0.0679 0.0191 0.5288 0.044 Uiso 1 1 calc R . . H26B H 0.0324 0.0406 0.6130 0.044 Uiso 1 1 calc R . . H26C H 0.0799 0.0486 0.6480 0.044 Uiso 1 1 calc R . . C27 C -0.07229(10) 0.17219(8) 0.7116(3) 0.0242(7) Uani 1 1 d . . . H27A H -0.0755 0.1438 0.7170 0.029 Uiso 1 1 calc R . . H27B H -0.0566 0.1806 0.7928 0.029 Uiso 1 1 calc R . . C28 C -0.11427(10) 0.19032(9) 0.7160(3) 0.0250(7) Uani 1 1 d . . . C29 C -0.14812(10) 0.16913(10) 0.7209(4) 0.0362(9) Uani 1 1 d . . . H29A H -0.1462 0.1417 0.7216 0.043 Uiso 1 1 calc R . . H29B H -0.1744 0.1813 0.7237 0.043 Uiso 1 1 calc R . . C30 C -0.11573(11) 0.23384(9) 0.7179(4) 0.0367(9) Uani 1 1 d . . . H30A H -0.1444 0.2424 0.7249 0.055 Uiso 1 1 calc R . . H30B H -0.1036 0.2439 0.6337 0.055 Uiso 1 1 calc R . . H30C H -0.1001 0.2435 0.7962 0.055 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 Cr1 0.0187(2) 0.0198(2) 0.0202(3) 0.0000(2) 0.0005(2) 0.0005(2) F1 0.153(3) 0.0522(15) 0.0611(18) 0.0130(13) 0.043(2) -0.0070(17) F2 0.136(3) 0.0492(14) 0.0704(19) 0.0051(13) -0.0259(19) -0.0447(16) F3 0.0396(15) 0.0563(16) 0.271(5) 0.090(2) 0.013(2) 0.0085(12) O1 0.0243(13) 0.0326(12) 0.0446(17) 0.0010(10) -0.0013(12) -0.0038(10) O2 0.0319(14) 0.0234(12) 0.0361(15) 0.0041(10) -0.0047(12) 0.0043(10) O3 0.0302(14) 0.0357(13) 0.0225(15) -0.0010(10) 0.0026(12) 0.0053(10) O4 0.0266(13) 0.0282(11) 0.0217(13) -0.0046(9) -0.0062(11) 0.0035(9) O5 0.0190(12) 0.0207(10) 0.0323(14) -0.0043(9) 0.0048(10) 0.0014(9) C1 0.0294(19) 0.0215(14) 0.0210(19) 0.0021(13) -0.0024(16) 0.0039(13) C2 0.0230(18) 0.0260(16) 0.023(2) -0.0054(13) 0.0077(15) -0.0045(14) C3 0.0176(17) 0.0212(15) 0.030(2) 0.0031(14) -0.0025(16) 0.0014(12) C4 0.0219(17) 0.0223(14) 0.0188(18) 0.0037(13) -0.0025(15) -0.0021(12) C5 0.031(2) 0.0309(17) 0.028(2) -0.0087(14) -0.0046(17) -0.0004(15) C6 0.0209(17) 0.0213(15) 0.0208(18) 0.0030(13) 0.0011(15) 0.0021(13) C7 0.0191(17) 0.0227(15) 0.0187(18) 0.0023(12) 0.0036(14) -0.0023(12) C8 0.0187(16) 0.0229(14) 0.0179(18) 0.0020(13) 0.0040(15) 0.0001(12) C9 0.0171(16) 0.0227(15) 0.0181(17) 0.0013(12) 0.0030(14) -0.0006(12) C10 0.0198(17) 0.0242(15) 0.0175(17) 0.0004(12) 0.0041(14) 0.0001(12) C11 0.0215(18) 0.0236(15) 0.0208(19) 0.0026(13) -0.0001(15) 0.0034(13) C12 0.0209(17) 0.0327(18) 0.0198(19) 0.0013(14) -0.0012(14) 0.0051(14) C13 0.0210(18) 0.0355(18) 0.0223(19) -0.0036(14) -0.0032(15) -0.0018(14) C14 0.0182(17) 0.0274(16) 0.0230(18) -0.0013(13) -0.0013(15) -0.0041(13) C15 0.0267(19) 0.0278(17) 0.027(2) -0.0057(14) 0.0000(16) -0.0049(14) C16 0.0248(19) 0.0272(17) 0.026(2) -0.0046(13) 0.0013(16) -0.0003(13) C17 0.0197(17) 0.0215(14) 0.026(2) -0.0015(13) 0.0032(16) 0.0003(12) C18 0.0274(18) 0.0218(16) 0.028(2) -0.0060(13) 0.0091(16) 0.0011(13) C19 0.0255(18) 0.0264(16) 0.0213(19) -0.0062(13) 0.0004(15) 0.0017(14) C20 0.0238(19) 0.0290(16) 0.023(2) -0.0051(13) -0.0006(15) 0.0063(13) C21 0.0262(18) 0.0290(15) 0.0224(18) -0.0072(14) 0.0007(17) 0.0010(13) C22 0.030(2) 0.0375(19) 0.042(3) -0.0009(16) 0.0086(19) -0.0052(16) C23 0.0215(18) 0.0395(18) 0.025(2) -0.0098(14) 0.0040(15) -0.0027(15) C24 0.025(2) 0.0381(19) 0.025(2) -0.0072(15) -0.0015(16) 0.0071(15) C25 0.030(2) 0.0294(17) 0.0207(19) -0.0049(13) 0.0013(16) 0.0031(15) C26 0.0310(19) 0.0193(15) 0.038(2) 0.0018(14) 0.0048(18) 0.0012(13) C27 0.0233(17) 0.0287(16) 0.0206(18) -0.0007(13) 0.0013(15) 0.0005(13) C28 0.0254(18) 0.0323(17) 0.0172(18) -0.0002(13) 0.0008(15) 0.0041(14) C29 0.0250(19) 0.0410(19) 0.043(3) -0.0069(17) 0.0074(18) -0.0025(15) C30 0.0285(19) 0.0342(18) 0.047(3) -0.0007(16) 0.0091(18) 0.0070(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 Cr1 C2 1.828(3) . ? Cr1 C3 1.831(4) . ? Cr1 C1 1.833(3) . ? Cr1 C9 2.225(3) . ? Cr1 C7 2.229(3) . ? Cr1 C8 2.232(3) . ? Cr1 C10 2.241(3) . ? Cr1 C6 2.242(3) . ? Cr1 C4 2.271(3) . ? F1 C22 1.330(4) . ? F2 C22 1.327(4) . ? F3 C22 1.279(4) . ? O1 C1 1.176(4) . ? O2 C2 1.165(4) . ? O3 C3 1.164(4) . ? O4 C4 1.360(4) . ? O4 C5 1.424(3) . ? O5 C18 1.421(4) . ? O5 C17 1.445(3) . ? C4 C10 1.399(4) . ? C4 C6 1.403(4) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 C7 1.402(4) . ? C6 H6 0.9500 . ? C7 C8 1.433(4) . ? C7 C17 1.532(4) . ? C8 C9 1.413(4) . ? C8 C14 1.526(4) . ? C9 C10 1.435(4) . ? C9 C11 1.522(4) . ? C10 H10 0.9500 . ? C11 C12 1.525(4) . ? C11 C27 1.546(4) . ? C11 H11 1.0000 . ? C12 C13 1.530(4) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.515(4) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.525(4) . ? C14 H14 1.0000 . ? C15 C16 1.533(4) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.533(4) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C26 1.542(4) . ? C18 C19 1.510(4) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C25 1.389(4) . ? C19 C20 1.399(4) . ? C20 C21 1.387(4) . ? C20 H20 0.9500 . ? C21 C23 1.391(4) . ? C21 C22 1.483(5) . ? C23 C24 1.378(4) . ? C23 H23 0.9500 . ? C24 C25 1.389(4) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C28 1.500(4) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 C29 1.321(4) . ? C28 C30 1.507(4) . ? C29 H29A 0.9500 . ? C29 H29B 0.9500 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 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 C2 Cr1 C3 85.00(13) . . ? C2 Cr1 C1 93.77(13) . . ? C3 Cr1 C1 87.73(14) . . ? C2 Cr1 C9 86.54(12) . . ? C3 Cr1 C9 127.57(13) . . ? C1 Cr1 C9 144.49(13) . . ? C2 Cr1 C7 141.99(13) . . ? C3 Cr1 C7 90.65(12) . . ? C1 Cr1 C7 123.82(12) . . ? C9 Cr1 C7 66.56(10) . . ? C2 Cr1 C8 105.67(12) . . ? C3 Cr1 C8 97.34(12) . . ? C1 Cr1 C8 160.23(12) . . ? C9 Cr1 C8 36.96(10) . . ? C7 Cr1 C8 37.48(10) . . ? C2 Cr1 C10 96.71(12) . . ? C3 Cr1 C10 164.32(12) . . ? C1 Cr1 C10 107.65(13) . . ? C9 Cr1 C10 37.47(11) . . ? C7 Cr1 C10 78.38(11) . . ? C8 Cr1 C10 67.15(11) . . ? C2 Cr1 C6 161.98(13) . . ? C3 Cr1 C6 111.64(12) . . ? C1 Cr1 C6 93.76(12) . . ? C9 Cr1 C6 77.86(11) . . ? C7 Cr1 C6 36.53(11) . . ? C8 Cr1 C6 66.59(11) . . ? C10 Cr1 C6 65.39(11) . . ? C2 Cr1 C4 128.19(12) . . ? C3 Cr1 C4 146.62(12) . . ? C1 Cr1 C4 86.67(13) . . ? C9 Cr1 C4 66.11(11) . . ? C7 Cr1 C4 65.83(11) . . ? C8 Cr1 C4 78.58(10) . . ? C10 Cr1 C4 36.12(10) . . ? C6 Cr1 C4 36.21(11) . . ? C4 O4 C5 118.6(2) . . ? C18 O5 C17 117.5(2) . . ? O1 C1 Cr1 177.5(3) . . ? O2 C2 Cr1 176.3(3) . . ? O3 C3 Cr1 175.7(3) . . ? O4 C4 C10 125.0(3) . . ? O4 C4 C6 115.4(3) . . ? C10 C4 C6 119.6(3) . . ? O4 C4 Cr1 130.26(19) . . ? C10 C4 Cr1 70.79(18) . . ? C6 C4 Cr1 70.78(18) . . ? O4 C5 H5A 109.5 . . ? O4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? O4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C7 C6 C4 121.4(3) . . ? C7 C6 Cr1 71.24(17) . . ? C4 C6 Cr1 73.01(17) . . ? C7 C6 H6 119.3 . . ? C4 C6 H6 119.3 . . ? Cr1 C6 H6 128.9 . . ? C6 C7 C8 120.1(3) . . ? C6 C7 C17 117.4(3) . . ? C8 C7 C17 122.4(3) . . ? C6 C7 Cr1 72.23(17) . . ? C8 C7 Cr1 71.38(16) . . ? C17 C7 Cr1 132.0(2) . . ? C9 C8 C7 118.4(3) . . ? C9 C8 C14 121.2(3) . . ? C7 C8 C14 120.4(3) . . ? C9 C8 Cr1 71.25(16) . . ? C7 C8 Cr1 71.14(16) . . ? C14 C8 Cr1 126.1(2) . . ? C8 C9 C10 120.6(3) . . ? C8 C9 C11 122.2(3) . . ? C10 C9 C11 117.1(3) . . ? C8 C9 Cr1 71.79(17) . . ? C10 C9 Cr1 71.86(17) . . ? C11 C9 Cr1 132.4(2) . . ? C4 C10 C9 119.9(3) . . ? C4 C10 Cr1 73.09(18) . . ? C9 C10 Cr1 70.67(17) . . ? C4 C10 H10 120.1 . . ? C9 C10 H10 120.1 . . ? Cr1 C10 H10 128.4 . . ? C9 C11 C12 111.7(3) . . ? C9 C11 C27 108.6(2) . . ? C12 C11 C27 112.1(2) . . ? C9 C11 H11 108.1 . . ? C12 C11 H11 108.1 . . ? C27 C11 H11 108.1 . . ? C11 C12 C13 112.0(2) . . ? C11 C12 H12A 109.2 . . ? C13 C12 H12A 109.2 . . ? C11 C12 H12B 109.2 . . ? C13 C12 H12B 109.2 . . ? H12A C12 H12B 107.9 . . ? C14 C13 C12 109.3(3) . . ? C14 C13 H13A 109.8 . . ? C12 C13 H13A 109.8 . . ? C14 C13 H13B 109.8 . . ? C12 C13 H13B 109.8 . . ? H13A C13 H13B 108.3 . . ? C13 C14 C15 115.5(3) . . ? C13 C14 C8 111.2(3) . . ? C15 C14 C8 110.1(3) . . ? C13 C14 H14 106.5 . . ? C15 C14 H14 106.5 . . ? C8 C14 H14 106.5 . . ? C14 C15 C16 109.7(2) . . ? C14 C15 H15A 109.7 . . ? C16 C15 H15A 109.7 . . ? C14 C15 H15B 109.7 . . ? C16 C15 H15B 109.7 . . ? H15A C15 H15B 108.2 . . ? C15 C16 C17 111.0(3) . . ? C15 C16 H16A 109.4 . . ? C17 C16 H16A 109.4 . . ? C15 C16 H16B 109.4 . . ? C17 C16 H16B 109.4 . . ? H16A C16 H16B 108.0 . . ? O5 C17 C7 102.6(2) . . ? O5 C17 C16 111.8(2) . . ? C7 C17 C16 112.3(2) . . ? O5 C17 C26 110.9(2) . . ? C7 C17 C26 108.2(3) . . ? C16 C17 C26 110.7(2) . . ? O5 C18 C19 107.3(2) . . ? O5 C18 H18A 110.3 . . ? C19 C18 H18A 110.3 . . ? O5 C18 H18B 110.3 . . ? C19 C18 H18B 110.3 . . ? H18A C18 H18B 108.5 . . ? C25 C19 C20 118.8(3) . . ? C25 C19 C18 120.7(3) . . ? C20 C19 C18 120.5(3) . . ? C21 C20 C19 120.2(3) . . ? C21 C20 H20 119.9 . . ? C19 C20 H20 119.9 . . ? C20 C21 C23 120.6(3) . . ? C20 C21 C22 120.0(3) . . ? C23 C21 C22 119.3(3) . . ? F3 C22 F2 107.4(3) . . ? F3 C22 F1 106.1(4) . . ? F2 C22 F1 101.8(3) . . ? F3 C22 C21 115.3(3) . . ? F2 C22 C21 112.9(3) . . ? F1 C22 C21 112.2(3) . . ? C24 C23 C21 119.0(3) . . ? C24 C23 H23 120.5 . . ? C21 C23 H23 120.5 . . ? C23 C24 C25 120.9(3) . . ? C23 C24 H24 119.6 . . ? C25 C24 H24 119.6 . . ? C19 C25 C24 120.4(3) . . ? C19 C25 H25 119.8 . . ? C24 C25 H25 119.8 . . ? C17 C26 H26A 109.5 . . ? C17 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C17 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C28 C27 C11 114.6(3) . . ? C28 C27 H27A 108.6 . . ? C11 C27 H27A 108.6 . . ? C28 C27 H27B 108.6 . . ? C11 C27 H27B 108.6 . . ? H27A C27 H27B 107.6 . . ? C29 C28 C27 121.6(3) . . ? C29 C28 C30 121.9(3) . . ? C27 C28 C30 116.5(3) . . ? C28 C29 H29A 120.0 . . ? C28 C29 H29B 120.0 . . ? H29A C29 H29B 120.0 . . ? C28 C30 H30A 109.5 . . ? C28 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C28 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? 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 C2 Cr1 C1 O1 -159(7) . . . . ? C3 Cr1 C1 O1 -75(7) . . . . ? C9 Cr1 C1 O1 111(7) . . . . ? C7 Cr1 C1 O1 15(7) . . . . ? C8 Cr1 C1 O1 31(7) . . . . ? C10 Cr1 C1 O1 102(7) . . . . ? C6 Cr1 C1 O1 37(7) . . . . ? C4 Cr1 C1 O1 73(7) . . . . ? C3 Cr1 C2 O2 52(5) . . . . ? C1 Cr1 C2 O2 140(5) . . . . ? C9 Cr1 C2 O2 -76(5) . . . . ? C7 Cr1 C2 O2 -32(5) . . . . ? C8 Cr1 C2 O2 -44(5) . . . . ? C10 Cr1 C2 O2 -112(5) . . . . ? C6 Cr1 C2 O2 -106(4) . . . . ? C4 Cr1 C2 O2 -131(4) . . . . ? C2 Cr1 C3 O3 16(4) . . . . ? C1 Cr1 C3 O3 -78(4) . . . . ? C9 Cr1 C3 O3 97(4) . . . . ? C7 Cr1 C3 O3 158(4) . . . . ? C8 Cr1 C3 O3 121(4) . . . . ? C10 Cr1 C3 O3 113(4) . . . . ? C6 Cr1 C3 O3 -172(4) . . . . ? C4 Cr1 C3 O3 -159(4) . . . . ? C5 O4 C4 C10 -18.4(4) . . . . ? C5 O4 C4 C6 161.1(3) . . . . ? C5 O4 C4 Cr1 75.4(3) . . . . ? C2 Cr1 C4 O4 -85.7(3) . . . . ? C3 Cr1 C4 O4 87.3(3) . . . . ? C1 Cr1 C4 O4 6.5(3) . . . . ? C9 Cr1 C4 O4 -150.1(3) . . . . ? C7 Cr1 C4 O4 136.1(3) . . . . ? C8 Cr1 C4 O4 173.3(3) . . . . ? C10 Cr1 C4 O4 -120.0(3) . . . . ? C6 Cr1 C4 O4 107.5(3) . . . . ? C2 Cr1 C4 C10 34.3(2) . . . . ? C3 Cr1 C4 C10 -152.7(2) . . . . ? C1 Cr1 C4 C10 126.51(18) . . . . ? C9 Cr1 C4 C10 -30.06(16) . . . . ? C7 Cr1 C4 C10 -103.90(18) . . . . ? C8 Cr1 C4 C10 -66.72(17) . . . . ? C6 Cr1 C4 C10 -132.5(3) . . . . ? C2 Cr1 C4 C6 166.83(19) . . . . ? C3 Cr1 C4 C6 -20.2(3) . . . . ? C1 Cr1 C4 C6 -100.98(19) . . . . ? C9 Cr1 C4 C6 102.45(19) . . . . ? C7 Cr1 C4 C6 28.60(18) . . . . ? C8 Cr1 C4 C6 65.78(18) . . . . ? C10 Cr1 C4 C6 132.5(3) . . . . ? O4 C4 C6 C7 179.2(3) . . . . ? C10 C4 C6 C7 -1.3(5) . . . . ? Cr1 C4 C6 C7 -54.5(3) . . . . ? O4 C4 C6 Cr1 -126.3(2) . . . . ? C10 C4 C6 Cr1 53.2(3) . . . . ? C2 Cr1 C6 C7 97.4(4) . . . . ? C3 Cr1 C6 C7 -59.0(2) . . . . ? C1 Cr1 C6 C7 -148.04(19) . . . . ? C9 Cr1 C6 C7 66.84(18) . . . . ? C8 Cr1 C6 C7 29.74(17) . . . . ? C10 Cr1 C6 C7 104.2(2) . . . . ? C4 Cr1 C6 C7 132.8(3) . . . . ? C2 Cr1 C6 C4 -35.4(5) . . . . ? C3 Cr1 C6 C4 168.20(18) . . . . ? C1 Cr1 C6 C4 79.2(2) . . . . ? C9 Cr1 C6 C4 -65.96(18) . . . . ? C7 Cr1 C6 C4 -132.8(3) . . . . ? C8 Cr1 C6 C4 -103.06(19) . . . . ? C10 Cr1 C6 C4 -28.56(17) . . . . ? C4 C6 C7 C8 0.3(5) . . . . ? Cr1 C6 C7 C8 -55.0(2) . . . . ? C4 C6 C7 C17 -176.0(3) . . . . ? Cr1 C6 C7 C17 128.7(3) . . . . ? C4 C6 C7 Cr1 55.3(3) . . . . ? C2 Cr1 C7 C6 -150.1(2) . . . . ? C3 Cr1 C7 C6 127.2(2) . . . . ? C1 Cr1 C7 C6 39.5(2) . . . . ? C9 Cr1 C7 C6 -101.6(2) . . . . ? C8 Cr1 C7 C6 -131.6(3) . . . . ? C10 Cr1 C7 C6 -64.11(19) . . . . ? C4 Cr1 C7 C6 -28.36(18) . . . . ? C2 Cr1 C7 C8 -18.6(3) . . . . ? C3 Cr1 C7 C8 -101.26(19) . . . . ? C1 Cr1 C7 C8 171.04(19) . . . . ? C9 Cr1 C7 C8 30.02(17) . . . . ? C10 Cr1 C7 C8 67.46(18) . . . . ? C6 Cr1 C7 C8 131.6(3) . . . . ? C4 Cr1 C7 C8 103.21(19) . . . . ? C2 Cr1 C7 C17 98.7(3) . . . . ? C3 Cr1 C7 C17 16.0(3) . . . . ? C1 Cr1 C7 C17 -71.7(3) . . . . ? C9 Cr1 C7 C17 147.3(3) . . . . ? C8 Cr1 C7 C17 117.2(4) . . . . ? C10 Cr1 C7 C17 -175.3(3) . . . . ? C6 Cr1 C7 C17 -111.2(4) . . . . ? C4 Cr1 C7 C17 -139.6(3) . . . . ? C6 C7 C8 C9 0.2(4) . . . . ? C17 C7 C8 C9 176.3(3) . . . . ? Cr1 C7 C8 C9 -55.2(2) . . . . ? C6 C7 C8 C14 176.8(3) . . . . ? C17 C7 C8 C14 -7.1(4) . . . . ? Cr1 C7 C8 C14 121.4(3) . . . . ? C6 C7 C8 Cr1 55.4(3) . . . . ? C17 C7 C8 Cr1 -128.5(3) . . . . ? C2 Cr1 C8 C9 -61.5(2) . . . . ? C3 Cr1 C8 C9 -148.35(19) . . . . ? C1 Cr1 C8 C9 107.8(4) . . . . ? C7 Cr1 C8 C9 130.2(3) . . . . ? C10 Cr1 C8 C9 29.26(17) . . . . ? C6 Cr1 C8 C9 101.2(2) . . . . ? C4 Cr1 C8 C9 65.25(18) . . . . ? C2 Cr1 C8 C7 168.25(18) . . . . ? C3 Cr1 C8 C7 81.41(19) . . . . ? C1 Cr1 C8 C7 -22.5(5) . . . . ? C9 Cr1 C8 C7 -130.2(3) . . . . ? C10 Cr1 C8 C7 -100.97(19) . . . . ? C6 Cr1 C8 C7 -29.04(17) . . . . ? C4 Cr1 C8 C7 -64.98(18) . . . . ? C2 Cr1 C8 C14 53.9(3) . . . . ? C3 Cr1 C8 C14 -33.0(3) . . . . ? C1 Cr1 C8 C14 -136.9(4) . . . . ? C9 Cr1 C8 C14 115.4(3) . . . . ? C7 Cr1 C8 C14 -114.4(3) . . . . ? C10 Cr1 C8 C14 144.6(3) . . . . ? C6 Cr1 C8 C14 -143.4(3) . . . . ? C4 Cr1 C8 C14 -179.4(2) . . . . ? C7 C8 C9 C10 0.3(4) . . . . ? C14 C8 C9 C10 -176.3(3) . . . . ? Cr1 C8 C9 C10 -54.8(2) . . . . ? C7 C8 C9 C11 -175.6(3) . . . . ? C14 C8 C9 C11 7.8(4) . . . . ? Cr1 C8 C9 C11 129.2(3) . . . . ? C7 C8 C9 Cr1 55.2(2) . . . . ? C14 C8 C9 Cr1 -121.4(3) . . . . ? C2 Cr1 C9 C8 122.03(19) . . . . ? C3 Cr1 C9 C8 41.0(2) . . . . ? C1 Cr1 C9 C8 -146.3(2) . . . . ? C7 Cr1 C9 C8 -30.42(17) . . . . ? C10 Cr1 C9 C8 -132.2(3) . . . . ? C6 Cr1 C9 C8 -67.04(18) . . . . ? C4 Cr1 C9 C8 -103.20(19) . . . . ? C2 Cr1 C9 C10 -105.74(18) . . . . ? C3 Cr1 C9 C10 173.27(18) . . . . ? C1 Cr1 C9 C10 -14.1(3) . . . . ? C7 Cr1 C9 C10 101.82(19) . . . . ? C8 Cr1 C9 C10 132.2(3) . . . . ? C6 Cr1 C9 C10 65.19(17) . . . . ? C4 Cr1 C9 C10 29.03(16) . . . . ? C2 Cr1 C9 C11 4.7(3) . . . . ? C3 Cr1 C9 C11 -76.3(3) . . . . ? C1 Cr1 C9 C11 96.4(3) . . . . ? C7 Cr1 C9 C11 -147.7(3) . . . . ? C8 Cr1 C9 C11 -117.3(4) . . . . ? C10 Cr1 C9 C11 110.5(3) . . . . ? C6 Cr1 C9 C11 175.7(3) . . . . ? C4 Cr1 C9 C11 139.5(3) . . . . ? O4 C4 C10 C9 -178.7(3) . . . . ? C6 C4 C10 C9 1.8(4) . . . . ? Cr1 C4 C10 C9 55.0(2) . . . . ? O4 C4 C10 Cr1 126.3(3) . . . . ? C6 C4 C10 Cr1 -53.2(3) . . . . ? C8 C9 C10 C4 -1.3(4) . . . . ? C11 C9 C10 C4 174.8(3) . . . . ? Cr1 C9 C10 C4 -56.2(3) . . . . ? C8 C9 C10 Cr1 54.8(2) . . . . ? C11 C9 C10 Cr1 -129.0(3) . . . . ? C2 Cr1 C10 C4 -153.50(18) . . . . ? C3 Cr1 C10 C4 111.1(5) . . . . ? C1 Cr1 C10 C4 -57.36(19) . . . . ? C9 Cr1 C10 C4 131.2(2) . . . . ? C7 Cr1 C10 C4 64.71(17) . . . . ? C8 Cr1 C10 C4 102.29(18) . . . . ? C6 Cr1 C10 C4 28.62(16) . . . . ? C2 Cr1 C10 C9 75.33(18) . . . . ? C3 Cr1 C10 C9 -20.1(5) . . . . ? C1 Cr1 C10 C9 171.47(17) . . . . ? C7 Cr1 C10 C9 -66.46(17) . . . . ? C8 Cr1 C10 C9 -28.89(16) . . . . ? C6 Cr1 C10 C9 -102.55(18) . . . . ? C4 Cr1 C10 C9 -131.2(2) . . . . ? C8 C9 C11 C12 -16.8(4) . . . . ? C10 C9 C11 C12 167.1(3) . . . . ? Cr1 C9 C11 C12 77.4(3) . . . . ? C8 C9 C11 C27 107.3(3) . . . . ? C10 C9 C11 C27 -68.8(3) . . . . ? Cr1 C9 C11 C27 -158.4(2) . . . . ? C9 C11 C12 C13 44.9(3) . . . . ? C27 C11 C12 C13 -77.3(3) . . . . ? C11 C12 C13 C14 -65.0(3) . . . . ? C12 C13 C14 C15 179.3(3) . . . . ? C12 C13 C14 C8 52.9(3) . . . . ? C9 C8 C14 C13 -26.0(4) . . . . ? C7 C8 C14 C13 157.4(3) . . . . ? Cr1 C8 C14 C13 -114.6(3) . . . . ? C9 C8 C14 C15 -155.3(3) . . . . ? C7 C8 C14 C15 28.1(4) . . . . ? Cr1 C8 C14 C15 116.1(3) . . . . ? C13 C14 C15 C16 176.4(3) . . . . ? C8 C14 C15 C16 -56.7(4) . . . . ? C14 C15 C16 C17 66.1(3) . . . . ? C18 O5 C17 C7 -178.5(3) . . . . ? C18 O5 C17 C16 -57.9(3) . . . . ? C18 O5 C17 C26 66.1(3) . . . . ? C6 C7 C17 O5 -49.5(3) . . . . ? C8 C7 C17 O5 134.3(3) . . . . ? Cr1 C7 C17 O5 40.7(4) . . . . ? C6 C7 C17 C16 -169.7(3) . . . . ? C8 C7 C17 C16 14.1(4) . . . . ? Cr1 C7 C17 C16 -79.5(3) . . . . ? C6 C7 C17 C26 67.7(3) . . . . ? C8 C7 C17 C26 -108.5(3) . . . . ? Cr1 C7 C17 C26 158.0(2) . . . . ? C15 C16 C17 O5 -157.3(2) . . . . ? C15 C16 C17 C7 -42.5(3) . . . . ? C15 C16 C17 C26 78.5(3) . . . . ? C17 O5 C18 C19 -179.8(3) . . . . ? O5 C18 C19 C25 133.7(3) . . . . ? O5 C18 C19 C20 -46.5(4) . . . . ? C25 C19 C20 C21 0.6(5) . . . . ? C18 C19 C20 C21 -179.1(3) . . . . ? C19 C20 C21 C23 -1.4(5) . . . . ? C19 C20 C21 C22 177.7(3) . . . . ? C20 C21 C22 F3 0.1(5) . . . . ? C23 C21 C22 F3 179.2(4) . . . . ? C20 C21 C22 F2 124.0(4) . . . . ? C23 C21 C22 F2 -56.9(5) . . . . ? C20 C21 C22 F1 -121.6(4) . . . . ? C23 C21 C22 F1 57.5(5) . . . . ? C20 C21 C23 C24 0.7(5) . . . . ? C22 C21 C23 C24 -178.4(3) . . . . ? C21 C23 C24 C25 0.8(5) . . . . ? C20 C19 C25 C24 0.8(5) . . . . ? C18 C19 C25 C24 -179.5(3) . . . . ? C23 C24 C25 C19 -1.5(5) . . . . ? C9 C11 C27 C28 177.2(3) . . . . ? C12 C11 C27 C28 -58.8(3) . . . . ? C11 C27 C28 C29 119.2(3) . . . . ? C11 C27 C28 C30 -62.1(4) . . . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.468 _refine_diff_density_min -0.387 _refine_diff_density_rms 0.059