data_feng_react.prod _audit_creation_date 07-10-29 _audit_creation_method CRYSTALS_ver_12.39 _oxford_structure_analysis_title 'Feng Reaktionsprodukt 120K 04-07' _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 10.7070(5) _cell_length_b 13.5317(5) _cell_length_c 16.9215(6) _cell_angle_alpha 68.1644(13) _cell_angle_beta 85.9627(12) _cell_angle_gamma 84.4285(12) _cell_volume 2263.45(16) _symmetry_cell_setting 'Triclinic' _symmetry_space_group_name_H-M 'P -1 ' _symmetry_space_group_name_Hall '?' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' '-x,-y,-z' loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 2 # Given Formula = C57 H60 O3 # Dc = 1.16 Fooo = 857.00 Mu = 0.70 M = 793.10 # Found Formula = C57.50 H55.50 O3.50 # Dc = 1.18 FOOO = 857.00 Mu = 0.72 M = 802.57 _chemical_formula_sum 'C57.50 H55.50 O3.50' _chemical_formula_moiety 'C57.50 H55.50 O3.50' _chemical_compound_source ? _chemical_formula_weight 802.57 _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0 _cell_measurement_theta_max 0 _cell_measurement_temperature 120 _exptl_crystal_description 'prism' _exptl_crystal_colour 'orange' _exptl_crystal_size_min 0.17 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_max 0.50 _exptl_crystal_density_diffrn 1.178 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 857 _exptl_absorpt_coefficient_mu 0.072 # Sheldrick geometric approximatio 0.97 0.99 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SORTAV (Blessing)' _exptl_absorpt_correction_T_min 0.90 _exptl_absorpt_correction_T_max 0.99 _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_radiation_monochromator 'graphite' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method '\f & \w scans' _computing_data_collection 'COLLECT (Nonius BV, 1997)' _computing_data_reduction 'Denzo/Scalepack (Otwinowski & Minor, 1996)' _computing_cell_refinement 'Denzo/Scalepack (Otwinowski & Minor, 1996)' _computing_structure_solution 'SHELXS 86 (Sheldrick, 1986)' _computing_structure_refinement 'CRYSTALS (Betteridge et al 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al 1996)' _diffrn_standards_interval_time ? _diffrn_standards_interval_count ? _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 120 _diffrn_reflns_number 49773 _reflns_number_total 12938 _diffrn_reflns_av_R_equivalents 0.073 # Number of reflections with Friedels Law is 12938 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 13201 _diffrn_reflns_theta_min 4.006 _diffrn_reflns_theta_max 29.999 _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 25.199 _diffrn_measured_fraction_theta_full 0.995 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _reflns_limit_h_min -14 _reflns_limit_h_max 15 _reflns_limit_k_min -17 _reflns_limit_k_max 19 _reflns_limit_l_min 0 _reflns_limit_l_max 23 _oxford_diffrn_Wilson_B_factor 0.00 _oxford_diffrn_Wilson_scale 0.00 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.31 _refine_diff_density_max 0.46 _refine_ls_number_reflns 5323 _refine_ls_number_restraints 0 _refine_ls_number_parameters 568 #_refine_ls_R_factor_ref 0.0557 _refine_ls_wR_factor_ref 0.0161 _refine_ls_goodness_of_fit_ref 1.1562 #_reflns_number_all 12932 _refine_ls_R_factor_all 0.1547 _refine_ls_wR_factor_all 0.0314 # The I/u(I) cutoff below was used for refinement as # well as the _gt R-factors: _reflns_threshold_expression I>3.00u(I) _reflns_number_gt 5323 _refine_ls_R_factor_gt 0.0557 _refine_ls_wR_factor_gt 0.0161 _refine_ls_shift/su_max 0.013586 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration '.' _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment constr # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 6.19 -10.1 2.62 ; # Check this file using the IUCr facility at: # http://journals.iucr.org/services/cif/checking/checkfull.html # The content below is held in the file 'script/refcif.dat'. This is a text # file which you may edit to reflect local conditions. # Items which need looking at are represented by a '?'. # Items for which there are choices are prefixed with 'choose from'. _publ_contact_letter ; ; _publ_contact_author_name 'Volker Enkelmann' _publ_contact_author_address ; Max-Planck-Institut for Polymer Research Postfach 3148 D-55021 Mainz Germany ; _publ_contact_author_phone 'Int+6131 379133' _publ_contact_author_fax 'Int+6131 379100' _publ_contact_author_email 've@mpip-mainz.mpg.de' # Insert your own references if required - in alphabetical order _publ_section_references ; Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K., Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Blessing, SORTAV ( ) Nonius BV, COLLECT Software, (1997-2001) Otwinowski, Z. & Minor, W. (1996), Processing of X-ray Diffraction Data Collected in Oscillation Mode. Methods Enzymol. 276, 1997, 307-326. Ed Carter, C.W. & Sweet, R.M., Academic Press. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. Sheldrick, G.M. (1986). SHELXS86. Program for the solution of crystal structures. Univ. of Gottingen, Federal Republic of Germany. Watkin D.J. (1994), Acta Cryst, A50, 411-437 Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996) CAMERON, Chemical Crystallography Laboratory, OXFORD, UK. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atoms attached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens O1 O 1.01143(14) 0.35725(13) 0.52566(9) 0.0457 1.0000 Uani . . . . . . O2 O 0.79867(17) 0.09095(14) 0.10872(10) 0.0616 1.0000 Uani . . . . . . O3 O 0.00646(14) 0.84163(12) 0.15788(9) 0.0412 1.0000 Uani . . . . . . C1 C 0.42139(15) 0.53452(14) 0.23892(10) 0.0153 1.0000 Uani . . . . . . C2 C 0.51559(16) 0.53706(14) 0.29191(10) 0.0163 1.0000 Uani . . . . . . C3 C 0.62009(16) 0.46191(14) 0.31045(10) 0.0162 1.0000 Uani . . . . . . C4 C 0.64125(16) 0.38580(14) 0.27284(10) 0.0160 1.0000 Uani . . . . . . C5 C 0.54926(15) 0.38538(13) 0.21789(10) 0.0143 1.0000 Uani . . . . . . C6 C 0.44000(15) 0.45522(14) 0.20381(10) 0.0157 1.0000 Uani . . . . . . C7 C 0.52877(16) 0.61597(14) 0.33155(10) 0.0175 1.0000 Uani . . . . . . C8 C 0.45902(17) 0.70843(14) 0.32879(11) 0.0211 1.0000 Uani . . . . . . C9 C 0.49989(18) 0.76741(14) 0.37338(11) 0.0240 1.0000 Uani . . . . . . C10 C 0.60875(18) 0.73798(15) 0.41929(11) 0.0233 1.0000 Uani . . . . . . C11 C 0.68059(17) 0.64556(15) 0.41995(11) 0.0218 1.0000 Uani . . . . . . C12 C 0.64018(17) 0.58639(14) 0.37660(10) 0.0183 1.0000 Uani . . . . . . C13 C 0.70652(17) 0.48194(14) 0.37188(10) 0.0176 1.0000 Uani . . . . . . C14 C 0.69565(17) 0.39827(14) 0.46070(10) 0.0207 1.0000 Uani . . . . . . C15 C 0.79446(18) 0.35636(15) 0.50919(11) 0.0267 1.0000 Uani . . . . . . C16 C 0.92186(19) 0.38651(16) 0.47804(13) 0.0315 1.0000 Uani . . . . . . C17 C 0.93710(19) 0.45404(16) 0.38831(12) 0.0280 1.0000 Uani . . . . . . C18 C 0.83921(17) 0.49651(14) 0.33899(11) 0.0210 1.0000 Uani . . . . . . C19 C 0.6526(2) 0.80231(16) 0.46910(12) 0.0308 1.0000 Uani . . . . . . C20 C 0.5552(2) 0.8928(2) 0.47012(16) 0.0537 1.0000 Uani . . . . . . C21 C 0.6769(3) 0.72770(19) 0.56053(13) 0.0537 1.0000 Uani . . . . . . C22 C 0.7736(2) 0.85207(17) 0.42544(14) 0.0406 1.0000 Uani . . . . . . C23 C 0.75765(16) 0.31162(14) 0.28614(10) 0.0168 1.0000 Uani . . . . . . C24 C 0.77087(18) 0.21728(15) 0.35667(11) 0.0230 1.0000 Uani . . . . . . C25 C 0.87687(18) 0.14658(15) 0.36461(11) 0.0235 1.0000 Uani . . . . . . C26 C 0.97415(17) 0.16670(14) 0.30376(11) 0.0186 1.0000 Uani . . . . . . C27 C 0.96242(18) 0.26267(15) 0.23404(11) 0.0257 1.0000 Uani . . . . . . C28 C 0.85644(17) 0.33371(15) 0.22598(11) 0.0241 1.0000 Uani . . . . . . C29 C 1.08614(19) 0.08487(15) 0.30820(11) 0.0228 1.0000 Uani . . . . . . C30 C 1.0536(2) 0.01542(17) 0.25933(14) 0.0374 1.0000 Uani . . . . . . C31 C 1.20635(18) 0.13965(16) 0.26753(12) 0.0329 1.0000 Uani . . . . . . C32 C 1.1122(2) 0.01231(17) 0.40039(12) 0.0408 1.0000 Uani . . . . . . C33 C 0.35884(16) 0.42941(14) 0.14751(10) 0.0169 1.0000 Uani . . . . . . C34 C 0.24001(17) 0.46811(15) 0.11646(10) 0.0207 1.0000 Uani . . . . . . C35 C 0.19010(17) 0.42761(14) 0.06163(10) 0.0214 1.0000 Uani . . . . . . C36 C 0.25536(17) 0.34956(14) 0.03620(10) 0.0195 1.0000 Uani . . . . . . C37 C 0.37357(17) 0.30905(14) 0.06940(10) 0.0182 1.0000 Uani . . . . . . C38 C 0.42273(16) 0.34847(14) 0.12419(10) 0.0175 1.0000 Uani . . . . . . C39 C 0.55206(16) 0.31388(14) 0.16518(10) 0.0167 1.0000 Uani . . . . . . C40 C 0.56078(18) 0.19677(15) 0.21940(11) 0.0241 1.0000 Uani . . . . . . C41 C 0.6407(2) 0.12614(16) 0.20048(12) 0.0325 1.0000 Uani . . . . . . C42 C 0.7270(2) 0.15687(19) 0.12745(13) 0.0355 1.0000 Uani . . . . . . C43 C 0.72736(19) 0.27147(17) 0.07528(12) 0.0317 1.0000 Uani . . . . . . C44 C 0.64912(16) 0.34368(15) 0.09347(11) 0.0223 1.0000 Uani . . . . . . C45 C 0.20415(18) 0.30790(15) -0.02785(11) 0.0231 1.0000 Uani . . . . . . C46 C 0.07204(18) 0.35901(18) -0.05599(13) 0.0360 1.0000 Uani . . . . . . C47 C 0.29378(18) 0.33455(15) -0.10592(11) 0.0271 1.0000 Uani . . . . . . C48 C 0.1965(2) 0.18658(16) 0.01290(12) 0.0382 1.0000 Uani . . . . . . C49 C 0.31115(16) 0.61506(14) 0.21862(10) 0.0180 1.0000 Uani . . . . . . C50 C 0.21272(17) 0.60969(16) 0.27702(12) 0.0235 1.0000 Uani . . . . . . C51 C 0.10973(18) 0.68497(17) 0.25832(13) 0.0321 1.0000 Uani . . . . . . C52 C 0.1075(2) 0.76785(18) 0.17845(15) 0.0378 1.0000 Uani . . . . . . C53 C 0.2051(2) 0.77478(16) 0.12016(13) 0.0354 1.0000 Uani . . . . . . C54 C 0.30776(19) 0.69883(15) 0.13968(11) 0.0253 1.0000 Uani . . . . . . C551 C 0.0270(4) 0.9398(3) 0.0718(3) 0.0364 0.5000 Uani . . . . . . C552 C -0.1076(4) 0.8222(3) 0.2249(3) 0.0325 0.5000 Uani . . . . . . O59 O 0.4661(3) 0.8876(2) -0.00412(18) 0.0438 0.5000 Uani . . . . . . C60 C 0.4933(2) 0.94971(16) 0.02787(14) 0.0402 1.0000 Uani . . . . . . C61 C 0.5202(3) 0.9332(2) 0.11722(16) 0.0627 1.0000 Uani . . . . . . C62 C 0.4113(5) 0.9641(3) 0.1664(3) 0.0463 0.5000 Uani . . . . . . H81 H 0.3844 0.7308 0.2975 0.0299 1.0000 Uiso R . . . . . H91 H 0.4507 0.8301 0.3725 0.0340 1.0000 Uiso R . . . . . H111 H 0.7559 0.6234 0.4504 0.0336 1.0000 Uiso R . . . . . H141 H 0.6152 0.3744 0.4823 0.0294 1.0000 Uiso R . . . . . H151 H 0.7822 0.3062 0.5654 0.0368 1.0000 Uiso R . . . . . H171 H 1.0196 0.4672 0.3645 0.0420 1.0000 Uiso R . . . . . H181 H 0.8539 0.5383 0.2805 0.0320 1.0000 Uiso R . . . . . H201 H 0.5852 0.9306 0.5014 0.0916 1.0000 Uiso R . . . . . H202 H 0.5415 0.9401 0.4132 0.0916 1.0000 Uiso R . . . . . H203 H 0.4786 0.8638 0.4959 0.0916 1.0000 Uiso R . . . . . H211 H 0.7044 0.7666 0.5918 0.0769 1.0000 Uiso R . . . . . H212 H 0.7398 0.6733 0.5601 0.0769 1.0000 Uiso R . . . . . H213 H 0.6016 0.6962 0.5865 0.0769 1.0000 Uiso R . . . . . H221 H 0.8029 0.8919 0.4553 0.0591 1.0000 Uiso R . . . . . H222 H 0.7572 0.8980 0.3685 0.0591 1.0000 Uiso R . . . . . H223 H 0.8356 0.7970 0.4251 0.0591 1.0000 Uiso R . . . . . H241 H 0.7059 0.2011 0.3997 0.0305 1.0000 Uiso R . . . . . H251 H 0.8829 0.0822 0.4132 0.0298 1.0000 Uiso R . . . . . H271 H 1.0281 0.2797 0.1915 0.0325 1.0000 Uiso R . . . . . H281 H 0.8510 0.3987 0.1780 0.0308 1.0000 Uiso R . . . . . H301 H 1.1215 -0.0360 0.2610 0.0583 1.0000 Uiso R . . . . . H302 H 1.0381 0.0593 0.2018 0.0583 1.0000 Uiso R . . . . . H303 H 0.9806 -0.0200 0.2853 0.0583 1.0000 Uiso R . . . . . H311 H 1.2735 0.0869 0.2714 0.0432 1.0000 Uiso R . . . . . H312 H 1.2263 0.1835 0.2968 0.0432 1.0000 Uiso R . . . . . H313 H 1.1936 0.1824 0.2093 0.0432 1.0000 Uiso R . . . . . H321 H 1.1818 -0.0372 0.4013 0.0509 1.0000 Uiso R . . . . . H322 H 1.1302 0.0540 0.4320 0.0509 1.0000 Uiso R . . . . . H323 H 1.0401 -0.0253 0.4250 0.0509 1.0000 Uiso R . . . . . H341 H 0.1936 0.5214 0.1327 0.0277 1.0000 Uiso R . . . . . H351 H 0.1087 0.4542 0.0406 0.0302 1.0000 Uiso R . . . . . H371 H 0.4201 0.2549 0.0543 0.0258 1.0000 Uiso R . . . . . H401 H 0.5073 0.1728 0.2690 0.0361 1.0000 Uiso R . . . . . H411 H 0.6406 0.0530 0.2364 0.0449 1.0000 Uiso R . . . . . H431 H 0.7852 0.2944 0.0280 0.0477 1.0000 Uiso R . . . . . H441 H 0.6544 0.4172 0.0596 0.0344 1.0000 Uiso R . . . . . H461 H 0.0435 0.3317 -0.0952 0.0532 1.0000 Uiso R . . . . . H462 H 0.0748 0.4342 -0.0824 0.0532 1.0000 Uiso R . . . . . H463 H 0.0162 0.3428 -0.0075 0.0532 1.0000 Uiso R . . . . . H471 H 0.2639 0.3100 -0.1464 0.0378 1.0000 Uiso R . . . . . H472 H 0.2988 0.4097 -0.1308 0.0378 1.0000 Uiso R . . . . . H473 H 0.3747 0.3007 -0.0890 0.0378 1.0000 Uiso R . . . . . H481 H 0.1646 0.1611 -0.0264 0.0539 1.0000 Uiso R . . . . . H482 H 0.2780 0.1532 0.0285 0.0539 1.0000 Uiso R . . . . . H483 H 0.1423 0.1703 0.0623 0.0539 1.0000 Uiso R . . . . . H501 H 0.2154 0.5534 0.3313 0.0363 1.0000 Uiso R . . . . . H511 H 0.0422 0.6808 0.2987 0.0504 1.0000 Uiso R . . . . . H531 H 0.2028 0.8319 0.0664 0.0514 1.0000 Uiso R . . . . . H541 H 0.3754 0.7041 0.0992 0.0377 1.0000 Uiso R . . . . . H5511 H -0.0461 0.9879 0.0611 0.0450 0.5000 Uiso R . . . . . H5512 H 0.0966 0.9753 0.0769 0.0450 0.5000 Uiso R . . . . . H5513 H 0.0433 0.9154 0.0259 0.0450 0.5000 Uiso R . . . . . H5521 H -0.1725 0.8775 0.2046 0.0454 0.5000 Uiso R . . . . . H5522 H -0.0790 0.8218 0.2769 0.0454 0.5000 Uiso R . . . . . H5523 H -0.1390 0.7553 0.2341 0.0454 0.5000 Uiso R . . . . . H611 H 0.5884 0.9739 0.1158 0.0805 1.0000 Uiso R . . . . . H612 H 0.5436 0.8595 0.1461 0.0805 1.0000 Uiso R . . . . . H621 H 0.4351 0.9514 0.2226 0.0630 0.5000 Uiso R . . . . . H622 H 0.3874 1.0379 0.1385 0.0630 0.5000 Uiso R . . . . . H623 H 0.3426 0.9235 0.1688 0.0630 0.5000 Uiso 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 O1 0.0335(9) 0.0576(11) 0.0453(9) -0.0163(8) -0.0233(7) 0.0046(8) O2 0.0661(12) 0.0661(13) 0.0594(11) -0.0387(10) -0.0131(9) 0.0351(10) O3 0.0398(10) 0.0401(9) 0.0499(10) -0.0259(8) -0.0229(8) 0.0213(8) C1 0.0137(9) 0.0178(9) 0.0144(8) -0.0062(7) -0.0008(7) -0.0006(7) C2 0.0158(10) 0.0194(10) 0.0150(8) -0.0069(7) -0.0007(7) -0.0053(8) C3 0.0146(9) 0.0180(10) 0.0147(8) -0.0039(7) -0.0032(7) -0.0029(7) C4 0.0159(9) 0.0155(9) 0.0162(8) -0.0053(7) -0.0030(7) 0.0001(7) C5 0.0147(9) 0.0157(9) 0.0142(8) -0.0069(7) -0.0002(6) -0.0031(7) C6 0.0132(9) 0.0191(9) 0.0175(8) -0.0087(7) -0.0027(7) -0.0040(7) C7 0.0193(10) 0.0192(10) 0.0162(8) -0.0082(8) 0.0016(7) -0.0056(8) C8 0.0212(10) 0.0221(10) 0.0226(9) -0.0110(8) -0.0028(7) -0.0015(8) C9 0.0266(11) 0.0175(10) 0.0315(10) -0.0135(8) 0.0007(8) -0.0013(8) C10 0.0253(11) 0.0259(11) 0.0251(10) -0.0153(9) 0.0038(8) -0.0105(8) C11 0.0204(10) 0.0255(11) 0.0240(9) -0.0133(8) -0.0057(8) -0.0019(8) C12 0.0200(10) 0.0180(10) 0.0185(8) -0.0084(8) -0.0008(7) -0.0017(7) C13 0.0204(10) 0.0168(9) 0.0160(8) -0.0053(7) -0.0062(7) -0.0018(7) C14 0.0235(10) 0.0215(10) 0.0192(9) -0.0091(8) -0.0022(7) -0.0037(8) C15 0.0328(12) 0.0266(11) 0.0203(9) -0.0072(8) -0.0067(8) -0.0018(9) C16 0.0313(13) 0.0326(12) 0.0350(11) -0.0173(10) -0.0117(9) 0.0042(9) C17 0.0196(11) 0.0344(13) 0.0360(11) -0.0192(10) -0.0039(8) -0.0025(9) C18 0.0199(10) 0.0222(10) 0.0233(9) -0.0098(8) -0.0006(7) -0.0076(8) C19 0.0360(13) 0.0307(12) 0.0355(11) -0.0216(10) -0.0006(9) -0.0115(10) C20 0.0427(15) 0.0633(18) 0.0849(19) -0.0624(16) -0.0022(13) -0.0013(13) C21 0.084(2) 0.0566(17) 0.0334(12) -0.0283(12) -0.0052(12) -0.0188(14) C22 0.0419(14) 0.0354(13) 0.0537(14) -0.0244(11) -0.0050(11) -0.0111(10) C23 0.0163(9) 0.0173(10) 0.0183(8) -0.0076(7) -0.0045(7) -0.0019(7) C24 0.0218(10) 0.0265(11) 0.0169(9) -0.0039(8) 0.0032(7) -0.0029(8) C25 0.0231(11) 0.0208(10) 0.0201(9) -0.0005(8) -0.0034(8) 0.0017(8) C26 0.0194(10) 0.0181(10) 0.0196(9) -0.0084(8) -0.0042(7) 0.0009(8) C27 0.0221(11) 0.0262(11) 0.0245(10) -0.0056(9) 0.0058(8) -0.0009(8) C28 0.0207(10) 0.0214(10) 0.0233(9) -0.0010(8) -0.0022(8) 0.0016(8) C29 0.0236(10) 0.0208(10) 0.0231(9) -0.0084(8) -0.0042(8) 0.0058(8) C30 0.0358(13) 0.0341(13) 0.0516(14) -0.0277(11) -0.0018(10) 0.0017(10) C31 0.0223(11) 0.0364(13) 0.0383(11) -0.0125(10) -0.0045(9) 0.0032(9) C32 0.0395(14) 0.0409(14) 0.0291(11) -0.0037(10) -0.0040(10) 0.0220(11) C33 0.0154(9) 0.0193(10) 0.0159(8) -0.0053(7) -0.0019(7) -0.0041(7) C34 0.0216(10) 0.0187(10) 0.0217(9) -0.0076(8) -0.0037(7) 0.0017(8) C35 0.0164(10) 0.0266(11) 0.0215(9) -0.0076(8) -0.0053(7) -0.0048(8) C36 0.0226(10) 0.0209(10) 0.0169(8) -0.0070(8) -0.0018(7) -0.0094(8) C37 0.0205(10) 0.0173(10) 0.0187(9) -0.0084(7) -0.0010(7) -0.0030(7) C38 0.0152(10) 0.0193(10) 0.0183(8) -0.0064(8) -0.0014(7) -0.0035(8) C39 0.0154(9) 0.0185(10) 0.0201(8) -0.0115(8) -0.0053(7) 0.0021(7) C40 0.0302(12) 0.0238(11) 0.0208(9) -0.0090(8) -0.0076(8) -0.0050(8) C41 0.0430(14) 0.0254(11) 0.0325(11) -0.0141(9) -0.0168(10) 0.0063(10) C42 0.0345(13) 0.0442(14) 0.0376(12) -0.0284(11) -0.0178(10) 0.0172(11) C43 0.0254(12) 0.0497(14) 0.0286(10) -0.0244(10) 0.0011(8) -0.0045(10) C44 0.0184(10) 0.0296(11) 0.0227(9) -0.0127(8) -0.0028(7) -0.0052(8) C45 0.0244(11) 0.0273(11) 0.0202(9) -0.0092(8) -0.0049(7) -0.0103(8) C46 0.0252(12) 0.0541(16) 0.0388(12) -0.0258(11) -0.0120(9) -0.0065(11) C47 0.0303(11) 0.0316(11) 0.0207(9) -0.0096(8) -0.0043(8) -0.0064(9) C48 0.0567(16) 0.0296(12) 0.0325(11) -0.0115(10) -0.0072(10) -0.0186(10) C49 0.0184(10) 0.0190(10) 0.0205(9) -0.0111(8) -0.0074(7) 0.0014(8) C50 0.0200(10) 0.0278(11) 0.0258(10) -0.0128(8) -0.0046(8) -0.0014(8) C51 0.0197(11) 0.0426(14) 0.0470(13) -0.0322(12) -0.0074(9) 0.0055(10) C52 0.0365(14) 0.0349(13) 0.0579(15) -0.0356(12) -0.0311(12) 0.0186(11) C53 0.0526(15) 0.0258(12) 0.0317(11) -0.0140(9) -0.0255(11) 0.0099(10) C54 0.0316(12) 0.0235(11) 0.0223(9) -0.0093(8) -0.0089(8) -0.0003(9) C551 0.040(3) 0.022(2) 0.046(2) -0.011(2) -0.011(2) 0.0078(19) C552 0.027(2) 0.031(2) 0.046(2) -0.023(2) -0.0119(19) 0.0096(18) O59 0.052(2) 0.044(2) 0.0365(17) -0.0152(15) -0.0006(14) -0.0086(16) C60 0.0387(13) 0.0304(13) 0.0557(15) -0.0214(11) 0.0029(11) -0.0037(11) C61 0.082(2) 0.0620(19) 0.0526(15) -0.0310(14) -0.0099(14) -0.0014(16) C62 0.068(3) 0.032(3) 0.036(2) -0.007(2) -0.010(2) -0.002(2) _refine_ls_extinction_method 'None' _oxford_refine_ls_scale 2.887(2) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag O1 . C16 . 1.234(2) yes O2 . C42 . 1.236(2) yes O3 . C52 . 1.369(2) yes O3 . C551 . 1.584(4) yes O3 . C552 . 1.578(4) yes C1 . C2 . 1.407(2) yes C1 . C6 . 1.400(2) yes C1 . C49 . 1.493(2) yes C2 . C3 . 1.406(2) yes C2 . C7 . 1.478(2) yes C3 . C4 . 1.392(2) yes C3 . C13 . 1.551(2) yes C4 . C5 . 1.403(2) yes C4 . C23 . 1.497(2) yes C5 . C6 . 1.406(2) yes C5 . C39 . 1.538(2) yes C6 . C33 . 1.486(2) yes C7 . C8 . 1.380(2) yes C7 . C12 . 1.404(2) yes C8 . C9 . 1.400(2) yes C8 . H81 . 0.950 no C9 . C10 . 1.388(3) yes C9 . H91 . 0.950 no C10 . C11 . 1.400(3) yes C10 . C19 . 1.539(3) yes C11 . C12 . 1.384(2) yes C11 . H111 . 0.950 no C12 . C13 . 1.546(2) yes C13 . C14 . 1.513(2) yes C13 . C18 . 1.493(2) yes C14 . C15 . 1.332(2) yes C14 . H141 . 0.950 no C15 . C16 . 1.467(3) yes C15 . H151 . 0.950 no C16 . C17 . 1.459(3) yes C17 . C18 . 1.332(2) yes C17 . H171 . 0.950 no C18 . H181 . 0.950 no C19 . C20 . 1.533(3) yes C19 . C21 . 1.525(3) yes C19 . C22 . 1.530(3) yes C20 . H201 . 0.950 no C20 . H202 . 0.950 no C20 . H203 . 0.950 no C21 . H211 . 0.950 no C21 . H212 . 0.950 no C21 . H213 . 0.950 no C22 . H221 . 0.950 no C22 . H222 . 0.950 no C22 . H223 . 0.950 no C23 . C24 . 1.389(2) yes C23 . C28 . 1.389(3) yes C24 . C25 . 1.391(2) yes C24 . H241 . 0.950 no C25 . C26 . 1.384(3) yes C25 . H251 . 0.950 no C26 . C27 . 1.394(2) yes C26 . C29 . 1.537(3) yes C27 . C28 . 1.394(3) yes C27 . H271 . 0.950 no C28 . H281 . 0.950 no C29 . C30 . 1.540(3) yes C29 . C31 . 1.536(3) yes C29 . C32 . 1.531(2) yes C30 . H301 . 0.950 no C30 . H302 . 0.950 no C30 . H303 . 0.950 no C31 . H311 . 0.950 no C31 . H312 . 0.950 no C31 . H313 . 0.950 no C32 . H321 . 0.950 no C32 . H322 . 0.950 no C32 . H323 . 0.950 no C33 . C34 . 1.389(2) yes C33 . C38 . 1.400(2) yes C34 . C35 . 1.397(2) yes C34 . H341 . 0.950 no C35 . C36 . 1.393(2) yes C35 . H351 . 0.950 no C36 . C37 . 1.398(2) yes C36 . C45 . 1.546(2) yes C37 . C38 . 1.383(2) yes C37 . H371 . 0.950 no C38 . C39 . 1.545(2) yes C39 . C40 . 1.504(3) yes C39 . C44 . 1.502(2) yes C40 . C41 . 1.334(3) yes C40 . H401 . 0.950 no C41 . C42 . 1.444(3) yes C41 . H411 . 0.950 no C42 . C43 . 1.472(3) yes C43 . C44 . 1.334(2) yes C43 . H431 . 0.950 no C44 . H441 . 0.950 no C45 . C46 . 1.538(3) yes C45 . C47 . 1.527(3) yes C45 . C48 . 1.534(3) yes C46 . H461 . 0.950 no C46 . H462 . 0.950 no C46 . H463 . 0.950 no C47 . H471 . 0.950 no C47 . H472 . 0.950 no C47 . H473 . 0.950 no C48 . H481 . 0.950 no C48 . H482 . 0.950 no C48 . H483 . 0.950 no C49 . C50 . 1.381(3) yes C49 . C54 . 1.394(2) yes C50 . C51 . 1.395(3) yes C50 . H501 . 0.950 no C51 . C52 . 1.399(3) yes C51 . H511 . 0.950 no C52 . C53 . 1.370(3) yes C53 . C54 . 1.397(3) yes C53 . H531 . 0.950 no C54 . H541 . 0.950 no C551 . H5511 . 0.950 no C551 . H5512 . 0.950 no C551 . H5513 . 0.950 no C552 . H5521 . 0.950 no C552 . H5522 . 0.950 no C552 . H5523 . 0.950 no O59 . C60 . 1.222(3) yes C60 . C60 2_675 1.351(4) yes C60 . C61 . 1.489(3) yes C61 . C62 . 1.501(5) yes C61 . H611 . 0.950 no C61 . H612 . 0.950 no C62 . H621 . 0.950 no C62 . H622 . 0.950 no C62 . H623 . 0.950 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C52 . O3 . C551 . 113.6(2) yes C52 . O3 . C552 . 116.7(2) yes C551 . O3 . C552 . 129.4(2) yes C2 . C1 . C6 . 116.16(15) yes C2 . C1 . C49 . 121.52(14) yes C6 . C1 . C49 . 122.27(14) yes C1 . C2 . C3 . 121.61(14) yes C1 . C2 . C7 . 128.93(16) yes C3 . C2 . C7 . 109.36(13) yes C2 . C3 . C4 . 122.18(14) yes C2 . C3 . C13 . 110.54(14) yes C4 . C3 . C13 . 127.18(15) yes C3 . C4 . C5 . 116.10(15) yes C3 . C4 . C23 . 122.68(14) yes C5 . C4 . C23 . 121.15(14) yes C4 . C5 . C6 . 122.01(14) yes C4 . C5 . C39 . 126.86(14) yes C6 . C5 . C39 . 111.13(13) yes C5 . C6 . C1 . 121.69(14) yes C5 . C6 . C33 . 108.49(14) yes C1 . C6 . C33 . 129.81(15) yes C2 . C7 . C8 . 133.19(15) yes C2 . C7 . C12 . 107.87(15) yes C8 . C7 . C12 . 118.87(15) yes C7 . C8 . C9 . 118.69(16) yes C7 . C8 . H81 . 120.262 no C9 . C8 . H81 . 121.046 no C8 . C9 . C10 . 122.92(18) yes C8 . C9 . H91 . 118.599 no C10 . C9 . H91 . 118.476 no C9 . C10 . C11 . 117.98(16) yes C9 . C10 . C19 . 122.78(18) yes C11 . C10 . C19 . 119.23(17) yes C10 . C11 . C12 . 119.39(16) yes C10 . C11 . H111 . 120.217 no C12 . C11 . H111 . 120.389 no C7 . C12 . C11 . 122.11(17) yes C7 . C12 . C13 . 111.72(14) yes C11 . C12 . C13 . 126.16(16) yes C12 . C13 . C3 . 100.21(13) yes C12 . C13 . C14 . 106.26(14) yes C3 . C13 . C14 . 111.14(14) yes C12 . C13 . C18 . 111.47(14) yes C3 . C13 . C18 . 113.76(14) yes C14 . C13 . C18 . 113.04(14) yes C13 . C14 . C15 . 122.57(17) yes C13 . C14 . H141 . 118.454 no C15 . C14 . H141 . 118.969 no C14 . C15 . C16 . 121.52(17) yes C14 . C15 . H151 . 119.360 no C16 . C15 . H151 . 119.122 no C15 . C16 . O1 . 121.61(19) yes C15 . C16 . C17 . 116.70(17) yes O1 . C16 . C17 . 121.7(2) yes C16 . C17 . C18 . 122.05(19) yes C16 . C17 . H171 . 118.631 no C18 . C17 . H171 . 119.312 no C13 . C18 . C17 . 122.71(17) yes C13 . C18 . H181 . 118.289 no C17 . C18 . H181 . 118.999 no C10 . C19 . C20 . 112.06(17) yes C10 . C19 . C21 . 109.27(17) yes C20 . C19 . C21 . 109.05(18) yes C10 . C19 . C22 . 108.21(15) yes C20 . C19 . C22 . 108.12(17) yes C21 . C19 . C22 . 110.12(19) yes C19 . C20 . H201 . 109.793 no C19 . C20 . H202 . 109.038 no H201 . C20 . H202 . 109.478 no C19 . C20 . H203 . 109.566 no H201 . C20 . H203 . 109.474 no H202 . C20 . H203 . 109.476 no C19 . C21 . H211 . 109.967 no C19 . C21 . H212 . 109.172 no H211 . C21 . H212 . 109.475 no C19 . C21 . H213 . 109.262 no H211 . C21 . H213 . 109.474 no H212 . C21 . H213 . 109.477 no C19 . C22 . H221 . 109.818 no C19 . C22 . H222 . 109.250 no H221 . C22 . H222 . 109.478 no C19 . C22 . H223 . 109.330 no H221 . C22 . H223 . 109.475 no H222 . C22 . H223 . 109.475 no C4 . C23 . C24 . 122.36(16) yes C4 . C23 . C28 . 120.50(16) yes C24 . C23 . C28 . 117.11(17) yes C23 . C24 . C25 . 121.05(17) yes C23 . C24 . H241 . 119.004 no C25 . C24 . H241 . 119.950 no C24 . C25 . C26 . 122.13(18) yes C24 . C25 . H251 . 119.242 no C26 . C25 . H251 . 118.626 no C25 . C26 . C27 . 116.85(17) yes C25 . C26 . C29 . 122.41(17) yes C27 . C26 . C29 . 120.60(17) yes C26 . C27 . C28 . 121.14(18) yes C26 . C27 . H271 . 119.163 no C28 . C27 . H271 . 119.699 no C27 . C28 . C23 . 121.67(18) yes C27 . C28 . H281 . 119.443 no C23 . C28 . H281 . 118.883 no C26 . C29 . C30 . 108.01(15) yes C26 . C29 . C31 . 111.66(16) yes C30 . C29 . C31 . 108.83(16) yes C26 . C29 . C32 . 111.39(16) yes C30 . C29 . C32 . 108.67(17) yes C31 . C29 . C32 . 108.21(17) yes C29 . C30 . H301 . 109.816 no C29 . C30 . H302 . 109.631 no H301 . C30 . H302 . 109.475 no C29 . C30 . H303 . 108.952 no H301 . C30 . H303 . 109.477 no H302 . C30 . H303 . 109.476 no C29 . C31 . H311 . 109.459 no C29 . C31 . H312 . 109.317 no H311 . C31 . H312 . 109.474 no C29 . C31 . H313 . 109.623 no H311 . C31 . H313 . 109.476 no H312 . C31 . H313 . 109.478 no C29 . C32 . H321 . 109.626 no C29 . C32 . H322 . 109.915 no H321 . C32 . H322 . 109.475 no C29 . C32 . H323 . 108.859 no H321 . C32 . H323 . 109.476 no H322 . C32 . H323 . 109.474 no C6 . C33 . C34 . 133.57(17) yes C6 . C33 . C38 . 108.23(14) yes C34 . C33 . C38 . 118.20(15) yes C33 . C34 . C35 . 119.32(17) yes C33 . C34 . H341 . 119.894 no C35 . C34 . H341 . 120.783 no C34 . C35 . C36 . 122.47(16) yes C34 . C35 . H351 . 119.076 no C36 . C35 . H351 . 118.456 no C35 . C36 . C37 . 117.88(14) yes C35 . C36 . C45 . 123.07(16) yes C37 . C36 . C45 . 119.03(16) yes C36 . C37 . C38 . 119.71(16) yes C36 . C37 . H371 . 120.204 no C38 . C37 . H371 . 120.083 no C33 . C38 . C37 . 122.35(16) yes C33 . C38 . C39 . 111.39(14) yes C37 . C38 . C39 . 126.23(16) yes C5 . C39 . C38 . 100.57(13) yes C5 . C39 . C40 . 112.78(13) yes C38 . C39 . C40 . 110.55(15) yes C5 . C39 . C44 . 111.92(14) yes C38 . C39 . C44 . 106.62(14) yes C40 . C39 . C44 . 113.46(15) yes C39 . C40 . C41 . 122.44(18) yes C39 . C40 . H401 . 118.349 no C41 . C40 . H401 . 119.211 no C40 . C41 . C42 . 122.4(2) yes C40 . C41 . H411 . 118.653 no C42 . C41 . H411 . 118.937 no C41 . C42 . O2 . 122.3(2) yes C41 . C42 . C43 . 117.20(18) yes O2 . C42 . C43 . 120.5(2) yes C42 . C43 . C44 . 121.41(18) yes C42 . C43 . H431 . 119.120 no C44 . C43 . H431 . 119.471 no C39 . C44 . C43 . 122.80(17) yes C39 . C44 . H441 . 118.276 no C43 . C44 . H441 . 118.927 no C36 . C45 . C46 . 111.97(16) yes C36 . C45 . C47 . 108.27(14) yes C46 . C45 . C47 . 109.10(15) yes C36 . C45 . C48 . 110.01(15) yes C46 . C45 . C48 . 107.91(16) yes C47 . C45 . C48 . 109.56(16) yes C45 . C46 . H461 . 109.751 no C45 . C46 . H462 . 109.395 no H461 . C46 . H462 . 109.473 no C45 . C46 . H463 . 109.253 no H461 . C46 . H463 . 109.478 no H462 . C46 . H463 . 109.477 no C45 . C47 . H471 . 109.792 no C45 . C47 . H472 . 109.369 no H471 . C47 . H472 . 109.473 no C45 . C47 . H473 . 109.239 no H471 . C47 . H473 . 109.477 no H472 . C47 . H473 . 109.476 no C45 . C48 . H481 . 109.937 no C45 . C48 . H482 . 109.263 no H481 . C48 . H482 . 109.477 no C45 . C48 . H483 . 109.197 no H481 . C48 . H483 . 109.478 no H482 . C48 . H483 . 109.475 no C1 . C49 . C50 . 121.45(16) yes C1 . C49 . C54 . 119.64(17) yes C50 . C49 . C54 . 118.90(17) yes C49 . C50 . C51 . 121.58(19) yes C49 . C50 . H501 . 119.143 no C51 . C50 . H501 . 119.277 no C50 . C51 . C52 . 118.6(2) yes C50 . C51 . H511 . 121.237 no C52 . C51 . H511 . 120.127 no C51 . C52 . O3 . 119.8(2) yes C51 . C52 . C53 . 120.43(19) yes O3 . C52 . C53 . 119.8(2) yes C52 . C53 . C54 . 120.4(2) yes C52 . C53 . H531 . 119.534 no C54 . C53 . H531 . 120.094 no C53 . C54 . C49 . 120.1(2) yes C53 . C54 . H541 . 120.144 no C49 . C54 . H541 . 119.786 no O3 . C551 . H5511 . 109.543 no O3 . C551 . H5512 . 108.965 no H5511 . C551 . H5512 . 109.477 no O3 . C551 . H5513 . 109.892 no H5511 . C551 . H5513 . 109.474 no H5512 . C551 . H5513 . 109.476 no O3 . C552 . H5521 . 110.055 no O3 . C552 . H5522 . 108.655 no H5521 . C552 . H5522 . 109.477 no O3 . C552 . H5523 . 109.687 no H5521 . C552 . H5523 . 109.475 no H5522 . C552 . H5523 . 109.475 no C60 2_675 C60 . O59 . 114.7(3) yes C60 2_675 C60 . C61 . 113.9(3) yes O59 . C60 . C61 . 131.3(3) yes C60 . C61 . C62 . 114.5(3) yes C60 . C61 . H611 . 108.042 no C62 . C61 . H611 . 108.934 no C60 . C61 . H612 . 107.961 no C62 . C61 . H612 . 107.886 no H611 . C61 . H612 . 109.465 no C61 . C62 . H621 . 109.833 no C61 . C62 . H622 . 108.755 no H621 . C62 . H622 . 109.477 no C61 . C62 . H623 . 109.809 no H621 . C62 . H623 . 109.476 no H622 . C62 . H623 . 109.474 no