Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2001 X-Sun-Data-Type: ciffile X-Sun-Data-Name: 157446.cif X-Sun-Charset: iso-8859-1 X-Sun-Content-Lines: 822 data_global _database_code_CSD 157446 #=============================================================================== _audit_creation_date 20-10-98 # 1. SUBMISSION DETAILS _publ_contact_author_name 'Dominique MATT' _publ_contact_author_address ;Laboratoire de Chimie Inorganique Moleculaire, UMR 7513 CNRSUniversitÄ Louis Pasteur, 1, rue Blaise PascalF 67008 Strasbourg Cedex ; _publ_contact_author_phone '++ 33 (0) 3 90 24 17 19' _publ_contact_author_fax 'xxxxxxxxxx' _publ_contact_author_email dmatt@chimie.u-strasbg.fr _publ_requested_journal 'J. Chem. Soc., Dalton Trans.' _journal_coden_Cambridge 186 _publ_contact_letter ? _publ_requested_category FM #=========================================================== # 2. PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ? _journal_techeditor_code ? _journal_techeditor_notes ? _journal_coden_ASTM ? _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #=========================================================== # 3. TITLE AND AUTHOR LIST _publ_section_title ; Diphosphines based on an inherently chiral calix[4]arene scaffold:synthesis and use in enantioselective catalysis ; loop_ _publ_author_name _publ_author_address 'Dieleman, Cedric' ; Universite Louis Pasteur, Laboratoire de Chimie Inorganique Moleculaire, UMR 7513 CNRS, 1, rue Blaise Pascal, F-67008 Strasbourg Cedex, France ; 'Steyer, Stphane' ;Universite Louis Pasteur, Laboratoire de Chimie Inorganique Moleculaire, UMR 7513 CNRS, 1, rue Blaise Pascal, F-67008 Strasbourg Cedex, France ; 'Jeunesse, Catherine' ;Universite Louis Pasteur, Laboratoire de Chimie Inorganique Moleculaire, UMR 7513 CNRS, 1, rue Blaise Pascal, F-67008 Strasbourg Cedex, France ; 'Matt, Dominique' ;Universite Louis Pasteur, Laboratoire de Chimie Inorganique Moleculaire, UMR 7513 CNRS, 1, rue Blaise Pascal, F-67008 Strasbourg Cedex, France ; # 4. TEXT _publ_section_abstract ? _publ_section_comment ? _publ_section_exptl_prep ? _publ_section_exptl_refinement ? ; Burla, M.C., Camalli, M., Cascarano, G.,Giacovazzo, C., Polidori, G., Spagna, R. &Viterbo, D. (1989). SIR. J. Appl. Cryst. 22, 389-393. OpenMoleN, Interactive Intelligent Structure solution (1997) Nonius B.V., Delft, The Netherlands. KappaCCD Operation Manual (1997), Nonius B.V., Delft, The Nederlands. Otwinowski, Z. & Minor, W. (1997), Methods in Enzymology, 276, 307-326. ; _publ_section_figure_captions ? _publ_section_acknowledgements ? #=========================================================== # If more than one structure is reported, sections 5-10 should be filled in # per structure. For each data set, replace the ? in the data_? line below # by a unique identifier.data_st245A #=============================================================================== # 5. CHEMICAL DATA _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety 'C81 H93 N O8 P2' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C81 H93 N O8 P2' _chemical_formula_weight 1270.59 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? 0.002 0.002 International_Tables_Vol_IV_Table_2.3.1 H ? 0.000 0.000 International_Tables_Vol_IV_Table_2.3.1 N ? 0.004 0.003 International_Tables_Vol_IV_Table_2.3.1 O ? 0.008 0.006 International_Tables_Vol_IV_Table_2.3.1 P ? 0.090 0.095 International_Tables_Vol_IV_Table_2.3.1 #=============================================================================== # 6. CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P 1' _symmetry_space_group_name_Hall ' P 1' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' _cell_length_a 10.3099(3) _cell_length_b 13.1130(6) _cell_length_c 15.0380(6) _cell_angle_alpha 109.403(2) _cell_angle_beta 96.716(3) _cell_angle_gamma 97.714(3) _cell_volume 1871.6(1) _cell_formula_units_Z 1 _cell_measurement_temperature 173 _cell_measurement_reflns_used 13115 _cell_measurement_theta_min 1.4 _cell_measurement_theta_max 28.0 _cell_special_details ;Cell parameters refined using Scalepack part of DENZO Z. Otwinowski, W. Minor, 1997 ; _exptl_crystal_description prism _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.13 _exptl_crystal_density_method 'none' _exptl_crystal_F_000 680 _exptl_absorpt_coefficient_mu 0.112 _exptl_absorpt_correction_type none_exptl_absorpt_correction_T_min _exptl_absorpt_correction_T_max ? #=============================================================================== # 7. EXPERIMENTAL DATA _diffrn_special_details; ?; _diffrn_ambient_temperature 173 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mo-K\a _diffrn_source xray _tube_diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method '\p scans' _diffrn_measurement_details ; 13115 reflections were collected using program Collect ("Collect" Data collection software, Nonius B.V., 1998) The conditions were as follow : crystal to detector distance = 35. mm. Scan angle = 2.0 deg 1 scans of 60 sec per frame. Data collection was divided into 1 set(s) with the following starting angles and number of frames : Set 1 Theta = 5.60 Omega = 0.00 Kappa = 0.00 102 frames Friedel pairs were not averaged. Internal R = 0.05 ; _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 13115 _diffrn_reflns_av_R_equivalents 0.050 _diffrn_reflns_av_sigmaI/netI 0.333 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.5 _diffrn_reflns_theta_max 28.05 _reflns_number_total 6711 _reflns_number_gt 5068 _reflns_threshold_expression >3.0\s(I) _computing_structure_solution Direct_methods_(SIR,_Burla_et_al.,_1989) _computing_structure_refinement LSFM_OpenMoleN_(_1997)_computing_molecular_graphics _computing_publication_material CIFGEN_IN_OpenMoleN_(_1997) #=============================================================================== # 8. REFINEMENT DATA _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_expression ? _refine_ls_extinction_coef ? _refine_ls_abs_structure_Flack 0.02(7) _refine_ls_number_reflns 5068 _refine_ls_number_parameters 819 _refine_ls_number_restraints 3 _refine_ls_number_constraints 0 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_R_factor_all 0.067 _refine_ls_R_factor_gt 0.049 _refine_ls_wR_factor_all 0.070 _refine_ls_wR_factor_ref 0.069 _refine_ls_goodness_of_fit_all 1.302 _refine_ls_goodness_of_fit_ref 1.274 _refine_ls_shift/su_max 0.020 _refine_ls_shift/esd_mean 0.00 refine_diff_density_max 0.420 _refine_diff_density_min -0.062 #=============================================================================== # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_type_symbol C1 1.0434 0.4010 0.1415 0.033(2) 1.000 Uani ? ? C C2 1.0354(4) 0.3561(4) 0.0434(3) 0.039(2) 1.000 Uani ? ? C C3 0.9754(4) 0.4005(4) -0.0189(3) 0.042(2) 1.000 Uani ? ? C C4 0.9223(4) 0.4931(4) 0.0213(3) 0.042(2) 1.000 Uani ? ? C C5 0.9275(4) 0.5413(3) 0.1191(3) 0.033(2) 1.000 Uani ? ? C C6 0.9919(4) 0.4954(3) 0.1781(3) 0.031(2) 1.000 Uani ? ? C C7 0.9570(5) 0.3430(5) -0.1273(3) 0.053(3) 1.000 Uani ? ? C C8 0.896(2) 0.405(1) -0.185(1) 0.091(4) 0.500 Uiso ? ? C C9 1.090(1) 0.311(1) -0.1584(8) 0.068(3) 0.500 Uiso ? ? C C10 0.859(1) 0.233(1) -0.1532(9) 0.078(4) 0.500 Uiso ? ? C O1 1.0011(3) 0.5435(2) 0.2784(2) 0.032(1) 1.000 Uani ? ? O C11 1.1113(4) 0.6327(3) 0.3176(3) 0.033(2) 1.000 Uani ? ? C P1 1.0873(1) 0.7276(1) 0.43035(8) 0.0359(5) 1.000 Uani ? ? P O2 0.9565(3) 0.7621(3) 0.4240(2) 0.046(2) 1.000 Uani ? ? O C12 1.1178(5) 0.6654(4) 0.5191(3) 0.045(2) 1.000 Uani ? ? C C13 1.1950(6) 0.5851(5) 0.5101(4) 0.070(3) 1.000 Uani ? ? C C14 1.2146(6) 0.5398(5) 0.5823(4) 0.087(3) 1.000 Uani ? ? C C15 1.1590(7) 0.5742(6) 0.6606(4) 0.088(3) 1.000 Uani ? ? C C16 1.0811(7) 0.6546(7) 0.6714(4) 0.076(4) 1.000 Uani ? ? C C17 1.0598(6) 0.7008(5) 0.6001(4) 0.062(3) 1.000 Uani ? ? C C18 1.2247(4) 0.8376(4) 0.4510(3) 0.037(2) 1.000 Uani ? ? C C19 1.1992(5) 0.9214(4) 0.4173(4) 0.051(3) 1.000 Uani ? ? C C20 1.3005(6) 1.0061(4) 0.4249(4) 0.060(3) 1.000 Uani ? ? C C21 1.4295(5) 1.0063(4) 0.4640(4) 0.050(3) 1.000 Uani ? ? C C22 1.4555(5) 0.9220(5) 0.4967(3) 0.048(3) 1.000 Uani ? ? C C23 1.3551(4) 0.8385(4) 0.4911(3) 0.041(2) 1.000 Uani ? ? C C24 0.8519(4) 0.6356(3) 0.1598(3) 0.037(2) 1.000 Uani ? ? C C25 0.7071(4) 0.5955(3) 0.1155(3) 0.033(2) 1.000 Uani ? ? C C26 0.6496(4) 0.6374(3) 0.0493(3) 0.035(2) 1.000 Uani ? ? C C27 0.5217(4) 0.5959(3) -0.0016(3) 0.037(2) 1.000 Uani ? ? C C28 0.4493(4) 0.5076(4) 0.0157(3) 0.035(2) 1.000 Uani ? ? C C29 0.5012(4) 0.4644(3) 0.0823(3) 0.034(2) 1.000 Uani ? ? C C30 0.6286(4) 0.5126(3) 0.1334(3) 0.031(2) 1.000 Uani ? ? C C31 0.4604(5) 0.6389(4) -0.0760(3) 0.047(2) 1.000 Uani ? ? C C32 0.5489(9) 0.7438(6) -0.0744(5) 0.140(4) 1.000 Uani ? ? C C33 0.4494(7) 0.5527(6) -0.1740(4) 0.078(3) 1.000 Uani ? ? C C34 0.3235(6) 0.6620(5) -0.0611(4) 0.081(3) 1.000 Uani ? ? C O3 0.6804(3) 0.4676(2) 0.1996(2) 0.033(1) 1.000 Uani ? ? O C35 0.6923(4) 0.5320(3) 0.2990(3) 0.037(2) 1.000 Uani ? ? C P2 0.5497(1) 0.5911(1) 0.33990(7) 0.0360(4) 1.000 Uani ? ? P O4 0.4204(3) 0.5140(3) 0.3116(2) 0.044(1) 1.000 Uani ? ? O C36 0.6014(4) 0.6394(4) 0.4681(3) 0.044(2) 1.000 Uani ? ? C C37 0.6904(5) 0.7357(5) 0.5222(3) 0.050(2) 1.000 Uani ? ? C C38 0.7243(6) 0.7628(6) 0.6215(4) 0.063(3) 1.000 Uani ? ? C C39 0.6709(6) 0.6955(7) 0.6644(4) 0.071(3) 1.000 Uani ? ? C C40 0.5803(6) 0.5995(6) 0.6113(3) 0.082(3) 1.000 Uani ? ? C C41 0.5459(5) 0.5726(5) 0.5145(3) 0.062(3) 1.000 Uani ? ? C C42 0.5440(4) 0.7068(4) 0.3009(3) 0.037(2) 1.000 Uani ? ? C C43 0.6492(4) 0.7923(4) 0.3169(3) 0.044(2) 1.000 Uani ? ? C C44 0.6313(5) 0.8787(4) 0.2861(4) 0.053(2) 1.000 Uani ? ? C C45 0.5081(5) 0.8809(4) 0.2393(3) 0.063(2) 1.000 Uani ? ? C C46 0.4044(5) 0.7948(4) 0.2210(3) 0.058(2) 1.000 Uani ? ? C C47 0.4218(4) 0.7081(4) 0.2507(3) 0.046(2) 1.000 Uani ? ? C C48 0.4189(4) 0.3698(3) 0.0981(3) 0.033(2) 1.000 Uani ? ? C C49 0.4657(4) 0.2613(3) 0.0573(3) 0.033(2) 1.000 Uani ? ? C C50 0.4475(4) 0.2053(4) -0.0411(3) 0.038(2) 1.000 Uani ? ? C C51 0.4929(4) 0.1079(4) -0.0811(3) 0.041(2) 1.000 Uani ? ? C C52 0.5638(4) 0.0688(4) -0.0189(3) 0.041(2) 1.000 Uani ? ? C C53 0.5856(4) 0.1220(3) 0.0799(3) 0.034(2) 1.000 Uani ? ? C C54 0.5328(4) 0.2158(3) 0.1170(3) 0.032(2) 1.000 Uani ? ? C C55 0.4632(6) 0.0443(5) -0.1904(4) 0.053(3) 1.000 Uani ? ? C C56 0.363(1) -0.068(1) -0.2083(9) 0.073(3) 0.500 Uiso ? ? C C57 0.454(1) 0.1203(7) -0.2452(5) 0.112(5) 1.000 Uani ? ? C C58 0.5773(9) -0.0156(7) -0.2231(5) 0.101(5) 1.000 Uani ? ? C O5 0.5529(3) 0.2703(2) 0.2159(2) 0.035(1) 1.000 Uani ? ? O C59 0.4583(4) 0.2359(4) 0.2665(3) 0.037(2) 1.000 Uani ? ? C C60 0.5216(4) 0.2620(4) 0.3684(3) 0.037(2) 1.000 Uani ? ? C O6 0.4507(3) 0.2503(3) 0.4270(2) 0.055(2) 1.000 Uani ? ? O N 0.6540(3) 0.2942(3) 0.3881(2) 0.041(2) 1.000 Uani ? ? N C61 0.7325(5) 0.3192(4) 0.4828(3) 0.045(2) 1.000 Uani ? ? C C62 0.7903(5) 0.2209(4) 0.4897(3) 0.046(2) 1.000 Uani ? ? C C63 0.8752(6) 0.1766(5) 0.4282(4) 0.071(3) 1.000 Uani ? ? C C64 0.9285(6) 0.0881(5) 0.4331(5) 0.089(3) 1.000 Uani ? ? C C65 0.9011(7) 0.0418(5) 0.4986(5) 0.079(3) 1.000 Uani ? ? C C66 0.8181(6) 0.0826(5) 0.5593(4) 0.067(3) 1.000 Uani ? ? C C67 0.7621(5) 0.1730(4) 0.5552(3) 0.053(2) 1.000 Uani ? ? C C68 0.8363(7) 0.4207(5) 0.5073(5) 0.068(3) 1.000 Uani ? ? C C69 0.6711(4) 0.0781(4) 0.1437(3) 0.039(2) 1.000 Uani ? ? C C70 0.8163(4) 0.0988(3) 0.1386(3) 0.037(2) 1.000 Uani ? ? C C71 0.8785(4) 0.0138(4) 0.0912(3) 0.041(2) 1.000 Uani ? ? C C72 1.0130(4) 0.0299(4) 0.0815(3) 0.043(2) 1.000 Uani ? ? C C73 1.0831(4) 0.1373(4) 0.1222(3) 0.041(2) 1.000 Uani ? ? C C74 1.0257(4) 0.2250(3) 0.1713(3) 0.035(2) 1.000 Uani ? ? C C75 0.8924(4) 0.2035(3) 0.1794(3) 0.035(2) 1.000 Uani ? ? C C76 1.0763(5) -0.0647(4) 0.0289(4) 0.054(3) 1.000 Uani ? ? C C77 1.031(2) -0.080(1) -0.094(1) 0.100(5) 0.500 Uiso ? ? C C78 1.236(1) -0.034(1) 0.0613(8) 0.066(3) 0.500 Uiso ? ? C C79 1.033(1) -0.169(1) 0.0453(8) 0.064(3) 0.500 Uiso ? ? C O7 0.8345(3) 0.2901(2) 0.2321(2) 0.038(1) 1.000 Uani ? ? O C80 1.1012(4) 0.3422(4) 0.2059(3) 0.037(2) 1.000 Uani ? ? C C81 0.274(1) 0.2747(7) 0.6105(6) 0.132(5) 1.000 Uani ? ? C O8 0.3926(7) 0.3405(5) 0.6076(4) 0.104(4) 1.000 Uani ? ? O C8A 0.976(2) 0.434(1) -0.176(1) 0.101(5) 0.500 Uiso ? ? C C9A 0.806(2) 0.294(2) -0.161(1) 0.110(5) 0.500 Uiso ? ? C C10A 1.010(3) 0.244(2) -0.165(2) 0.159(9) 0.500 Uiso ? ? C C56A 0.326(2) -0.025(1) -0.216(1) 0.093(4) 0.500 Uiso ? ? C C78A 1.222(1) -0.0337(8) 0.0223(7) 0.051(2) 0.500 Uiso ? ? C C77a 1.011(2) -0.117(2) -0.071(1) 0.110(5) 0.500 Uiso ? ? C C79a 1.072(2) -0.146(1) 0.097(1) 0.094(4) 0.500 Uiso ? ? C H1 1.0726 0.2923 0.0176 0.0537 1.000 Uiso calc C2 H H2 0.8804 0.5251 -0.0198 0.0552 1.000 Uiso calc C4 H H3 1.1201 0.6704 0.2739 0.0448 1.000 Uiso calc C11 H H4 1.1898 0.6046 0.3276 0.0448 1.000 Uiso calc C11 H H5 1.2350 0.5604 0.4548 0.0853 1.000 Uiso calc C13 H H6 1.2676 0.4846 0.5755 0.1066 1.000 Uiso calc C14 H H7 1.1728 0.5433 0.7090 0.1169 1.000 Uiso calc C15 H H8 1.0420 0.6785 0.7272 0.1211 1.000 Uiso calc C16 H H9 1.0063 0.7557 0.6072 0.0876 1.000 Uiso calc C17 H H10 1.1114 0.9202 0.3889 0.0698 1.000 Uiso calc C19 H H11 1.2819 1.0639 0.4035 0.0799 1.000 Uiso calc C20 H H12 1.4997 1.0636 0.4684 0.0730 1.000 Uiso calc C21 H H13 1.5439 0.9222 0.5232 0.0702 1.000 Uiso calc C22 H H14 1.3738 0.7819 0.5141 0.0572 1.000 Uiso calc C23 H H15 0.8861 0.6975 0.1445 0.0471 1.000 Uiso calc C24 H H16 0.8616 0.6557 0.2274 0.0471 1.000 Uiso calc C24 H H17 0.7006 0.6969 0.0388 0.0454 1.000 Uiso calc C26 H H18 0.3620 0.4762 -0.0193 0.0471 1.000 Uiso calc C28 H H19 0.5084 0.7688 -0.1214 0.1848 1.000 Uiso calc C32 H H20 0.5597 0.7993 -0.0130 0.1848 1.000 Uiso calc C32 H H21 0.6333 0.7283 -0.0879 0.1848 1.000 Uiso calc C32 H H22 0.4112 0.5783 -0.2212 0.1086 1.000 Uiso calc C33 H H23 0.5354 0.5389 -0.1849 0.1086 1.000 Uiso calc C33 H H24 0.3947 0.4867 -0.1774 0.1086 1.000 Uiso calc C33 H H25 0.2882 0.6886 -0.1086 0.1015 1.000 Uiso calc C34 H H26 0.2670 0.5962 -0.0659 0.1015 1.000 Uiso calc C34 H H27 0.3290 0.7158 0.0005 0.1015 1.000 Uiso calc C34 H H28 0.7649 0.5912 0.3140 0.0470 1.000 Uiso calc C35 H H29 0.7119 0.4861 0.3343 0.0470 1.000 Uiso calc C35 H H30 0.7281 0.7829 0.4922 0.0701 1.000 Uiso calc C37 H H31 0.7850 0.8287 0.6587 0.0956 1.000 Uiso calc C38 H H32 0.6955 0.7139 0.7315 0.1062 1.000 Uiso calc C39 H H33 0.5426 0.5530 0.6420 0.1012 1.000 Uiso calc C40 H H34 0.4833 0.5075 0.4784 0.0775 1.000 Uiso calc C41 H H35 0.3499 0.6486 0.2370 0.0555 1.000 Uiso calc C47 H H36 0.3204 0.7951 0.1876 0.0691 1.000 Uiso calc C46 H H37 0.4953 0.9414 0.2201 0.0736 1.000 Uiso calc C45 H H38 0.7038 0.9369 0.2972 0.0704 1.000 Uiso calc C44 H H39 0.7339 0.7916 0.3490 0.0559 1.000 Uiso calc C43 H H40 0.3296 0.3614 0.0685 0.0439 1.000 Uiso calc C48 H H41 0.4229 0.3869 0.1650 0.0439 1.000 Uiso calc C48 H H42 0.4020 0.2349 -0.0826 0.0505 1.000 Uiso calc C50 H H43 0.5984 0.0036 -0.0447 0.0539 1.000 Uiso calc C52 H H44 0.4271 0.1589 0.2372 0.0470 1.000 Uiso calc C59 H H45 0.3858 0.2734 0.2651 0.0470 1.000 Uiso calc C59 H H46 0.6758 0.3342 0.5292 0.0614 1.000 Uiso calc C61 H H47 0.8966 0.2081 0.3821 0.0880 1.000 Uiso calc C63 H H48 0.9857 0.0587 0.3899 0.1082 1.000 Uiso calc C64 H H49 0.9398 -0.0189 0.5019 0.1019 1.000 Uiso calc C65 H H50 0.7978 0.0498 0.6049 0.0910 1.000 Uiso calc C66 H H51 0.7041 0.2013 0.5981 0.0703 1.000 Uiso calc C67 H H52 0.8868 0.4363 0.5689 0.0996 1.000 Uiso calc C68 H H53 0.8935 0.4091 0.4611 0.0996 1.000 Uiso calc C68 H H54 0.7944 0.4810 0.5075 0.0996 1.000 Uiso calc C68 H H55 0.6411 0.0010 0.1245 0.0507 1.000 Uiso calc C69 H H56 0.6602 0.1127 0.2081 0.0507 1.000 Uiso calc C69 H H57 0.8276 -0.0587 0.0640 0.0529 1.000 Uiso calc C71 H H58 1.1739 0.1515 0.1162 0.0527 1.000 Uiso calc C73 H H59 1.0920 0.3792 0.2703 0.0491 1.000 Uiso calc C80 H H60 1.1926 0.3421 0.2024 0.0491 1.000 Uiso calc C80 H loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 _atom_site_aniso_type_symbol C1 0.028(2) 0.033(2) 0.038(2) 0.001(2) 0.004(1) 0.010(1) C C2 0.029(2) 0.044(2) 0.044(2) 0.003(2) 0.006(1) 0.009(2) C C3 0.036(2) 0.056(3) 0.036(2) 0.003(2) 0.008(1) 0.011(2) C C4 0.040(2) 0.051(2) 0.036(2) 0.003(2) 0.007(1) 0.017(2) C C5 0.030(2) 0.037(2) 0.034(2) 0.002(2) 0.007(1) 0.011(1) C C6 0.030(2) 0.034(2) 0.029(2) 0.002(2) 0.006(1) 0.008(1) C C7 0.064(3) 0.067(3) 0.035(2) 0.007(3) 0.010(2) 0.001(2) C O1 0.031(1) 0.034(1) 0.032(1) 0.002(1) 0.0044(9) 0.008(1) O C11 0.034(2) 0.033(2) 0.031(2) 0.003(2) 0.001(1) 0.007(1) C P1 0.0338(5) 0.0369(5) 0.0372(5) 0.0061(4) 0.0052(4) 0.0080(4) P O2 0.036(1) 0.048(2) 0.057(2) 0.010(1) 0.006(1) 0.012(1) O C12 0.041(2) 0.052(3) 0.042(2) -0.005(2) -0.001(2) 0.018(2) C C13 0.066(3) 0.078(3) 0.068(2) 0.018(2) 0.010(2) 0.044(2) C C14 0.062(3) 0.110(3) 0.097(3) 0.009(3) -0.003(2) 0.075(2) C C15 0.067(3) 0.124(4) 0.082(3) -0.025(3) -0.022(2) 0.067(2) C C16 0.092(4) 0.123(5) 0.040(2) -0.035(4) 0.004(2) 0.019(3) C C17 0.080(3) 0.074(4) 0.040(2) 0.009(3) 0.015(2) 0.011(2) C C18 0.038(2) 0.035(2) 0.039(2) 0.005(2) 0.009(2) 0.000(2) C C19 0.043(2) 0.044(3) 0.069(3) 0.005(2) 0.009(2) 0.015(2) C C20 0.070(3) 0.040(3) 0.077(3) 0.007(2) 0.021(2) 0.022(2) C C21 0.055(2) 0.042(3) 0.056(2) -0.008(2) 0.017(2) 0.000(2) C C22 0.040(2) 0.061(3) 0.044(2) -0.006(2) 0.002(2) 0.005(2) C C23 0.043(2) 0.042(2) 0.037(2) 0.004(2) 0.005(2) 0.004(2) C C24 0.037(2) 0.033(2) 0.041(2) 0.005(2) 0.009(1) 0.016(1) C C25 0.037(2) 0.033(2) 0.029(2) 0.007(2) 0.003(1) 0.011(1) C C26 0.039(2) 0.034(2) 0.032(2) 0.005(2) 0.004(1) 0.012(1) C C27 0.046(2) 0.035(2) 0.031(2) 0.010(2) 0.001(1) 0.011(1) C C28 0.039(2) 0.035(2) 0.031(2) 0.011(2) 0.000(1) 0.007(1) C C29 0.032(2) 0.035(2) 0.036(2) 0.011(1) 0.007(1) 0.012(1) C C30 0.032(2) 0.029(2) 0.031(1) 0.011(1) 0.009(1) 0.012(1) C C31 0.058(3) 0.043(2) 0.042(2) 0.005(2) -0.008(2) 0.022(1) C C32 0.149(6) 0.109(3) 0.171(3) -0.046(4) -0.083(3) 0.115(2) C C33 0.100(4) 0.124(4) 0.038(2) 0.056(3) 0.008(2) 0.032(2) C C34 0.104(3) 0.093(3) 0.055(2) 0.062(2) 0.010(2) 0.032(2) C O3 0.030(1) 0.035(1) 0.032(1) 0.009(1) 0.0037(9) 0.0151(9) O C35 0.036(2) 0.039(2) 0.035(2) 0.005(2) 0.005(1) 0.016(1) C P2 0.0346(4) 0.0389(5) 0.0347(4) 0.0087(4) 0.0101(3) 0.0147(3) P O4 0.040(1) 0.048(2) 0.045(1) 0.003(1) 0.010(1) 0.021(1) O C36 0.047(2) 0.048(2) 0.039(2) 0.017(2) 0.015(1) 0.018(2) C C37 0.057(2) 0.061(3) 0.036(2) 0.008(2) 0.006(2) 0.010(2) C C38 0.071(3) 0.097(5) 0.037(2) 0.009(3) 0.008(2) 0.006(3) C C39 0.067(3) 0.139(5) 0.039(2) 0.025(3) 0.014(2) 0.027(3) C C40 0.087(3) 0.116(4) 0.053(2) 0.030(3) 0.027(2) 0.051(2) C C41 0.069(3) 0.071(3) 0.048(2) 0.015(2) 0.017(2) 0.029(2) C C42 0.040(2) 0.042(2) 0.031(2) 0.015(2) 0.013(1) 0.013(1) C C43 0.042(2) 0.040(2) 0.049(2) 0.009(2) 0.015(2) 0.016(2) C C44 0.070(3) 0.036(2) 0.059(2) 0.009(2) 0.024(2) 0.016(2) C C45 0.070(3) 0.055(2) 0.064(2) 0.031(2) 0.031(2) 0.032(2) C C46 0.054(2) 0.073(3) 0.050(2) 0.031(2) 0.020(2) 0.033(2) C C47 0.044(2) 0.050(2) 0.043(2) 0.020(2) 0.014(1) 0.022(2) C C48 0.029(2) 0.036(2) 0.035(2) 0.004(2) 0.001(1) 0.013(1) C C49 0.025(2) 0.036(2) 0.038(2) 0.003(1) 0.007(1) 0.014(1) C C50 0.037(2) 0.040(2) 0.038(2) 0.004(2) 0.001(1) 0.014(1) C C51 0.050(2) 0.038(2) 0.037(2) 0.007(2) 0.009(2) 0.012(2) C C52 0.039(2) 0.036(2) 0.048(2) 0.004(2) 0.009(2) 0.014(2) C C53 0.030(2) 0.033(2) 0.041(2) 0.001(2) 0.008(1) 0.013(1) C C54 0.030(2) 0.034(2) 0.031(2) 0.003(2) 0.005(1) 0.010(1) C C55 0.075(3) 0.052(3) 0.038(2) 0.006(3) 0.005(2) 0.005(2) C C57 0.248(8) 0.119(5) 0.047(3) 0.095(4) 0.012(4) 0.027(3) C C58 0.145(5) 0.129(5) 0.056(3) 0.073(4) 0.035(3) 0.015(4) C O5 0.033(1) 0.037(1) 0.035(1) 0.004(1) 0.0082(9) 0.0137(9) O C59 0.028(2) 0.045(2) 0.039(2) 0.005(2) 0.008(1) 0.019(1) C C60 0.042(2) 0.034(2) 0.036(2) 0.006(2) 0.010(1) 0.012(1) C O6 0.057(2) 0.068(2) 0.043(1) -0.002(2) 0.014(1) 0.023(1) O N 0.036(2) 0.045(2) 0.041(2) 0.008(1) 0.004(1) 0.018(1) N C61 0.051(2) 0.048(2) 0.038(2) 0.008(2) -0.001(2) 0.012(2) C C62 0.047(2) 0.051(3) 0.040(2) 0.005(2) -0.005(2) 0.011(2) C C63 0.063(3) 0.083(3) 0.068(3) 0.030(2) 0.013(2) 0.034(2) C C64 0.084(3) 0.090(3) 0.093(3) 0.052(2) 0.016(3) 0.041(3) C C65 0.090(4) 0.072(3) 0.076(3) 0.039(3) 0.003(3) 0.024(3) C C66 0.080(4) 0.066(3) 0.058(2) 0.000(3) -0.017(2) 0.028(2) C C67 0.059(3) 0.055(3) 0.045(2) 0.007(2) -0.005(2) 0.019(2) C C68 0.081(4) 0.052(3) 0.073(3) -0.003(3) -0.027(3) 0.011(3) C C69 0.037(2) 0.033(2) 0.048(2) 0.004(2) 0.009(1) 0.016(1) C C70 0.033(2) 0.035(2) 0.043(2) 0.007(2) 0.010(1) 0.018(1) C C71 0.040(2) 0.036(2) 0.047(2) 0.006(2) 0.008(2) 0.016(2) C C72 0.041(2) 0.036(2) 0.053(2) 0.011(2) 0.011(2) 0.015(2) C C73 0.034(2) 0.038(2) 0.053(2) 0.009(2) 0.010(2) 0.018(2) C C74 0.032(2) 0.034(2) 0.040(2) 0.008(2) 0.003(1) 0.011(1) C C75 0.036(2) 0.033(2) 0.036(2) 0.009(2) 0.008(1) 0.013(1) C C76 0.045(2) 0.036(2) 0.097(3) 0.012(2) 0.025(2) 0.018(2) C O7 0.035(1) 0.038(1) 0.043(1) 0.007(1) 0.014(1) 0.009(1) O C80 0.029(2) 0.036(2) 0.048(2) 0.008(2) 0.004(1) 0.014(2) C C81 0.198(6) 0.086(5) 0.136(5) 0.025(5) 0.105(4) 0.036(4) C O8 0.157(4) 0.105(4) 0.069(3) 0.006(4) 0.042(3) -0.007(3) O # 10. MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.382(7) . . ? C1 C6 1.382(7) . . ? C1 C80 1.541(6) . . ? C2 C3 1.386(8) . . ? C3 C4 1.382(8) . . ? C3 C7 1.528(8) . . ? C4 C5 1.386(7) . . ? C5 C6 1.385(7) . . ? C5 C24 1.543(7) . . ? C6 O1 1.414(5) . . ? C7 C8 1.51(2) . . ? C7 C9 1.57(2) . . ? C7 C10 1.55(2) . . ? C7 C8A 1.60(2) . . ? C7 C9A 1.56(2) . . ? C7 C10A 1.44(3) . . ? C8 C9A 1.79(3) . . ? C9 C10A 1.10(3) . . ? C10 C9A 1.06(2) . . ? C10 C10A 1.57(4) . . ? O1 C11 1.426(6) . . ? C11 P1 1.807(5) . . ? P1 O2 1.480(4) . . ? P1 C12 1.801(5) . . ? P1 C18 1.799(5) . . ? C12 C13 1.384(9) . . ? C12 C17 1.387(9) . . ? C13 C14 1.408(9) . . ? C14 C15 1.34(1) . . ? C15 C16 1.39(1) . . ? C16 C17 1.41(1) . . ? C18 C19 1.396(8) . . ? C18 C23 1.404(7) . . ? C19 C20 1.384(9) . . ? C20 C21 1.39(1) . . ? C21 C22 1.40(1) . . ? C22 C23 1.375(8) . . ? C24 C25 1.507(7) . . ? C25 C26 1.398(6) . . ? C25 C30 1.386(6) . . ? C26 C27 1.383(7) . . ? C27 C28 1.407(7) . . ? C27 C31 1.523(7) . . ? C28 C29 1.393(7) . . ? C29 C30 1.390(6) . . ? C29 C48 1.509(7) . . ? C30 O3 1.405(5) . . ? C31 C32 1.54(1) . . ? C31 C33 1.51(1) . . ? C31 C34 1.51(1) . . ? O3 C35 1.433(6) . . ? C35 P2 1.828(5) . . ? P2 O4 1.483(4) . . ? P2 C36 1.806(5) . . ? P2 C42 1.804(5) . . ? C36 C37 1.390(9) . . ? C36 C41 1.395(8) . . ? C37 C38 1.403(9) . . ? C38 C39 1.35(1) . . ? C39 C40 1.39(1) . . ? C40 C41 1.368(9) . . ? C42 C43 1.388(7) . . ? C42 C47 1.396(7) . . ? C43 C44 1.384(8) . . ? C44 C45 1.387(9) . . ? C45 C46 1.38(1) . . ? C46 C47 1.378(8) . . ? C48 C49 1.519(7) . . ? C49 C50 1.393(7) . . ? C49 C54 1.400(6) . . ? C50 C51 1.388(8) . . ? C51 C52 1.390(7) . . ? C51 C55 1.547(8) . . ? C52 C53 1.391(7) . . ? C53 C54 1.384(7) . . ? C53 C69 1.528(7) . . ? C54 O5 1.396(5) . . ? C55 C56 1.61(2) . . ? C55 C57 1.49(1) . . ? C55 C58 1.54(1) . . ? C55 C56A 1.51(2) . . ? O5 C59 1.420(5) . . ? C59 C60 1.499(7) . . ? C60 O6 1.242(6) . . ? C60 N 1.340(6) . . ? N C61 1.462(6) . . ? C61 C62 1.519(8) . . ? C61 C68 1.501(9) . . ? C62 C63 1.389(9) . . ? C62 C67 1.370(8) . . ? C63 C64 1.37(1) . . ? C64 C65 1.35(1) . . ? C65 C66 1.35(1) . . ? C66 C67 1.40(1) . . ? C69 C70 1.501(7) . . ? C70 C71 1.390(7) . . ? C70 C75 1.383(7) . . ? C71 C72 1.406(7) . . ? C72 C73 1.390(8) . . ? C72 C76 1.509(8) . . ? C73 C74 1.393(7) . . ? C74 C75 1.393(7) . . ? C74 C80 1.513(7) . . ? C75 O7 1.403(6) . . ? C76 C77 1.79(2) . . ? C76 C78 1.62(2) . . ? C76 C79 1.49(2) . . ? C76 C78A 1.52(1) . . ? C76 C77a 1.46(2) . . ? C76 C79a 1.70(2) . . ? C81 O8 1.41(1) . . ? loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag ? ? ? ? ? ? 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_2_geom_angle _site_symmetry_3_geom_angle _publ_flagC2 C1 C6 118.0(4) . . . ? C2 C1 C80 120.0(4) . . . ? C6 C1 C80 121.9(4) . . . ? C1 C2 C3 122.7(5) . . . ? C2 C3 C4 116.9(5) . . . ? C2 C3 C7 121.3(5) . . . ? C4 C3 C7 121.5(5) . . . ? C3 C4 C5 122.7(5) . . . ? C4 C5 C6 117.9(4) . . . ? C4 C5 C24 120.8(4) . . . ? C6 C5 C24 121.0(4) . . . ? C1 C6 C5 121.7(4) . . . ? C1 C6 O1 118.8(4) . . . ? C5 C6 O1 119.4(4) . . . ? 3 C7 C8 114.9(9) . . . ? C3 C7 C9 110.9(7) . . . ? C3 C7 C10 107.0(7) . . . ? C3 C7 C8A 109.0(9) . . . ? C3 C7 C9A 105.6(9) . . . ? C3 C7 C10A 118(1) . . . ? C8 C7 C9 111(1) . . . ? C8 C7 C10 106(1) . . . ? C8 C7 C8A 30.9(9) . . . ? C8 C7 C9A 71(1) . . . ? C8 C7 C10A 125(1) . . . ? C9 C7 C10 105.7(9) . . . ? C9 C7 C8A 87(1) . . . ? C9 C7 C9A 136(1) . . . ? C9 C7 C10A 42(1) . . . ? C10 C7 C8A 133(1) . . . ? C10 C7 C9A 39.9(9) . . . ? C10 C7 C10A 63(1) . . . ? C8A C7 C9A 102(1) . . . ? 8A C7 C10A 119(1) . . . ? C9A C7 C10A 99(1) . . . ? C7 C8 C9A 55(1) . . . ? C7 C9 C10A 62(1) . . . ? C7 C10 C9A 70(1) . . . ? C7 C10 C10A 55(1) . . . ? C9A C10 C10A 119(2) . . . ? C6 O1 C11 110.5(3) . . . ? O1 C11 P1 110.8(3) . . . ? C11 P1 O2 112.5(2) . . . ? C11 P1 C12 107.4(3) . . . ? C11 P1 C18 100.1(2) . . . ? O2 P1 C12 114.3(2) . . . ? O2 P1 C18 113.2(2) . . . ? C12 P1 C18 108.2(2) . . . ? P1 C12 C13 123.4(5) . . . ? P1 C12 C17 117.3(5) . . . ? C13 C12 C17 119.4(6) . . . ? C12 C13 C14 120.4(7) . . . ? C13 C14 C15 120.3(8) . . . ? C14 C15 C16 120.5(7) . . . ? C15 C16 C17 120.3(7) . . . ? C12 C17 C16 119.2(8) . . . ? P1 C18 C19 116.4(4) . . . ? P1 C18 C23 123.9(4) . . . ? C19 C18 C23 119.4(5) . . . ? C18 C19 C20 120.6(6) . . . ? C19 C20 C21 119.8(6) . . . ? C20 C21 C22 119.7(5) . . . ? C21 C22 C23 120.9(5) . . . ? C18 C23 C22 119.5(5) . . . ? C5 C24 C25 108.1(4) . . . ? C24 C25 C26 120.1(4) . . . ? C24 C25 C30 122.3(4) . . . ? C26 C25 C30 117.5(4) . . . ? C25 C26 C27 122.9(4) . . . ? C26 C27 C28 117.0(4) . . . ? C26 C27 C31 123.1(5) . . . ? C28 C27 C31 120.0(4) . . . ? C27 C28 C29 122.3(4) . . . ? C28 C29 C30 117.8(4) . . . ? C28 C29 C48 120.0(4) . . . ? C30 C29 C48 122.2(4) . . . ? C25 C30 C29 122.3(4) . . . ? C25 C30 O3 120.2(4) . . . ? C29 C30 O3 117.2(4) . . . ? C27 C31 C32 111.2(5) . . . ? C27 C31 C33 108.5(5) . . . ? C27 C31 C34 111.7(5) . . . ? C32 C31 C33 107.4(7) . . . ? C32 C31 C34 109.3(7) . . . ? C33 C31 C34 108.7(5) . . . ? C30 O3 C35 117.0(3) . . . ? O3 C35 P2 118.2(3) . . . ? C35 P2 O4 116.1(2) . . . ? C35 P2 C36 101.0(2) . . . ? C35 P2 C42 106.8(2) . . . ? O4 P2 C36 110.1(2) . . . ? O4 P2 C42 112.4(2) . . . ? C36 P2 C42 109.8(2) . . . ? P2 C36 C37 125.4(4) . . . ? P2 C36 C41 115.8(5) . . . ? C37 C36 C41 118.8(5) . . . ? C36 C37 C38 119.7(6) . . . ? C37 C38 C39 120.2(7) . . . ? C38 C39 C40 120.7(6) . . . ? C39 C40 C41 119.6(6) . . . ? C36 C41 C40 121.0(7) . . . ? P2 C42 C43 125.6(4) . . . ? P2 C42 C47 115.7(4) . . . ? C43 C42 C47 118.7(5) . . . ? C42 C43 C44 120.3(5) . . . ? C43 C44 C45 120.4(6) . . . ? C44 C45 C46 119.5(5) . . . ? C45 C46 C47 120.3(6) . . . ? C42 C47 C46 120.7(5) . . . ? C29 C48 C49 113.5(4) . . . ? C48 C49 C50 121.2(4) . . . ? C48 C49 C54 121.2(4) . . . ? C50 C49 C54 117.6(4) . . . ? C49 C50 C51 122.8(4) . . . ? C50 C51 C52 117.3(5) . . . ? C50 C51 C55 121.3(5) . . . ? C52 C51 C55 121.4(5) . . . ? C51 C52 C53 122.1(5) . . . ? C52 C53 C54 118.7(4) . . . ? C52 C53 C69 119.3(4) . . . ? C54 C53 C69 122.0(4) . . . ? C49 C54 C53 121.4(4) . . . ? C49 C54 O5 118.9(4) . . . ? C53 C54 O5 119.6(4) . . . ? C51 C55 C56 107.0(7) . . . ? C51 C55 C57 111.6(6) . . . ? C51 C55 C58 110.8(5) . . . ? C51 C55 C56A 108.3(9) . . . ? C56 C55 C57 127.1(9) . . . ? C56 C55 C58 93.1(9) . . . ? C56 C55 C56A 27.9(8) . . . ? C57 C55 C58 105.2(7) . . . ? C57 C55 C56A 103(1) . . . ? C58 C55 C56A 116(1) . . . ? C54 O5 C59 117.2(3) . . . ? O5 C59 C60 109.8(4) . . . ? C59 C60 O6 119.2(4) . . . ? C59 C60 N 115.7(4) . . . ? O6 C60 N 125.0(5) . . . ? C60 N C61 123.2(4) . . . ? N C61 C62 111.4(5) . . . ? N C61 C68 110.1(5) . . . ? C62 C61 C68 112.9(5) . . . ? C61 C62 C63 119.8(5) . . . ? C61 C62 C67 122.4(5) . . . ? C63 C62 C67 117.7(6) . . . ? C62 C63 C64 120.9(7) . . . ? C63 C64 C65 121.1(7) . . . ? C64 C65 C66 119.6(7) . . . ? C65 C66 C67 120.2(7) . . . ? C62 C67 C66 120.5(6) . . . ? C53 C69 C70 113.4(4) . . . ? C69 C70 C71 121.1(5) . . . ? C69 C70 C75 121.2(4) . . . ? C71 C70 C75 117.7(4) . . . ? C70 C71 C72 123.1(5) . . . ? C71 C72 C73 116.4(5) . . . ? C71 C72 C76 121.4(5) . . . ?C 73 C72 C76 122.2(5) . . . ? C72 C73 C74 122.6(5) . . . ? C73 C74 C75 118.3(5) . . . ? C73 C74 C80 121.0(4) . . . ? C75 C74 C80 120.4(4) . . . ? C70 C75 C74 121.9(4) . . . ? C70 C75 O7 119.2(4) . . . ? C74 C75 O7 119.0(4) . . . ? C72 C76 C77 103.7(8) . . . ? C72 C76 C78 110.5(7) . . . ? C72 C76 C79 114.7(7) . . . ? C72 C76 C78A 115.2(7) . . . ? C72 C76 C77a 111(1) . . . ? C72 C76 C79a 104.3(8) . . . ? C77 C76 C78 110(1) . . . ? C77 C76 C79 111(1) . . . ? C77 C76 C78A 89.4(9) . . . ? C77 C76 C77a 22(1) . . . ? C77 C76 C79a 137(1) . . . ? C78 C76 C79 106.1(9) . . . ? C78 C76 C78A 21.4(6) . . . ? C78 C76 C77a 123(1) . . . ? C78 C76 C79a 88(1) . . . ? C79 C76 C78A 118.4(8) . . . ? C79 C76 C77a 89(1) . . . ? C79 C76 C79a 26.7(8) . . . ? C78A C76 C77a 103(1) . . . ? C78A C76 C79a 106.6(9) . . . ? C77a C76 C79a 116(1) . . . ? C1 C80 C74 108.6(4) . . . ? C7 C9A C8 53(1) . . . ? C7 C9A C10 69(1) . . . ? C8 C9A C10 116(2) . . . ? C7 C10A C9 74(2) . . . ? C7 C10A C10 61(1) . . . ? C9 C10A C10 136(3) . . . ?