# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Richard Douthwaite' _publ_contact_author_email RED4@YORK.AC.UK _publ_section_title ; Synthesis of Rhodium(I) and Iridium(I) Complexes of Chiral N-Heterocyclic Carbenes and Their Application to Asymmetric Transfer Hydrogenation ; loop_ _publ_author_name 'Richard Douthwaite' 'Gavin Dyson' "Jean-C\'edric Frison" 'Adrian C. Whitwood' # Attachment 'B909290Krevised.cif' data_compound1b _database_code_depnum_ccdc_archive 'CCDC 731703' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C18 H26 N3), 2(C24 H20 B), 3(C6 H12)' _chemical_formula_sum 'C102 H128 B2 N6' _chemical_formula_weight 1459.72 _chemical_absolute_configuration syn 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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 19.5255(14) _cell_length_b 10.9535(8) _cell_length_c 21.0834(15) _cell_angle_alpha 90.00 _cell_angle_beta 114.9760(10) _cell_angle_gamma 90.00 _cell_volume 4087.5(5) _cell_formula_units_Z 2 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 6097 _cell_measurement_theta_min 2.19 _cell_measurement_theta_max 27.98 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.186 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1584 _exptl_absorpt_coefficient_mu 0.068 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.926 _exptl_absorpt_correction_T_max 0.986 _exptl_absorpt_process_details 'SADABS v2.03; (Sheldrick)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 42956 _diffrn_reflns_av_R_equivalents 0.0244 _diffrn_reflns_av_sigmaI/netI 0.0373 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.07 _diffrn_reflns_theta_max 28.31 _reflns_number_total 20011 _reflns_number_gt 16752 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Poor quality data. Nearly higher symmetry - broken by chiral cyclohexyl ring. ; _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^)+(0.1788P)^2^+3.2500P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 1(3) _refine_ls_number_reflns 20011 _refine_ls_number_parameters 1047 _refine_ls_number_restraints 16 _refine_ls_R_factor_all 0.1016 _refine_ls_R_factor_gt 0.0882 _refine_ls_wR_factor_ref 0.2741 _refine_ls_wR_factor_gt 0.2570 _refine_ls_goodness_of_fit_ref 1.015 _refine_ls_restrained_S_all 1.015 _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 C1 C 0.76126(17) 0.1761(3) 0.52802(17) 0.0299(7) Uani 1 1 d . . . H1 H 0.7655 0.2079 0.5714 0.036 Uiso 1 1 calc R . . C2 C 0.7290(2) 0.1507(4) 0.41531(18) 0.0342(7) Uani 1 1 d . . . H2 H 0.7057 0.1633 0.3661 0.041 Uiso 1 1 calc R . . C3 C 0.77688(18) 0.0608(3) 0.44923(17) 0.0274(6) Uani 1 1 d . . . C4 C 0.85354(18) 0.0033(3) 0.57760(16) 0.0292(6) Uani 1 1 d . . . H4 H 0.8723 -0.0626 0.5562 0.035 Uiso 1 1 calc R . . C5 C 0.8149(2) -0.0575(4) 0.6196(2) 0.0404(9) Uani 1 1 d . . . H5A H 0.7927 0.0059 0.6387 0.048 Uiso 1 1 calc R . . H5B H 0.7736 -0.1111 0.5885 0.048 Uiso 1 1 calc R . . C6 C 0.8722(2) -0.1331(5) 0.6798(2) 0.0509(11) Uani 1 1 d . . . H6A H 0.8473 -0.1679 0.7080 0.061 Uiso 1 1 calc R . . H6B H 0.8906 -0.2015 0.6605 0.061 Uiso 1 1 calc R . . C7 C 0.9378(2) -0.0557(6) 0.7255(2) 0.0617(15) Uani 1 1 d . . . H7A H 0.9751 -0.1071 0.7626 0.074 Uiso 1 1 calc R . . H7B H 0.9199 0.0078 0.7484 0.074 Uiso 1 1 calc R . . C8 C 0.9760(2) 0.0059(5) 0.6833(2) 0.0488(10) Uani 1 1 d . . . H8A H 0.9983 -0.0579 0.6645 0.059 Uiso 1 1 calc R . . H8B H 1.0176 0.0586 0.7149 0.059 Uiso 1 1 calc R . . C9 C 0.92065(19) 0.0836(4) 0.62216(17) 0.0354(8) Uani 1 1 d . . . H9 H 0.9016 0.1513 0.6422 0.042 Uiso 1 1 calc R . . C10 C 0.6703(2) 0.3317(3) 0.45345(19) 0.0329(7) Uani 1 1 d . . . H10 H 0.6811 0.3700 0.4997 0.039 Uiso 1 1 calc R . . C11 C 0.5878(2) 0.2945(4) 0.4201(3) 0.0463(10) Uani 1 1 d . . . H11A H 0.5731 0.2731 0.3710 0.069 Uiso 1 1 calc R . . H11B H 0.5566 0.3626 0.4229 0.069 Uiso 1 1 calc R . . H11C H 0.5803 0.2238 0.4450 0.069 Uiso 1 1 calc R . . C12 C 0.6885(2) 0.4241(4) 0.4095(2) 0.0392(8) Uani 1 1 d . . . H12A H 0.7431 0.4388 0.4300 0.059 Uiso 1 1 calc R . . H12B H 0.6620 0.5007 0.4081 0.059 Uiso 1 1 calc R . . H12C H 0.6722 0.3924 0.3618 0.059 Uiso 1 1 calc R . . C13 C 0.80787(19) -0.0413(3) 0.42214(17) 0.0288(7) Uani 1 1 d . . . C14 C 0.8642(2) -0.0165(4) 0.40116(19) 0.0350(8) Uani 1 1 d . . . H14 H 0.8819 0.0646 0.4023 0.042 Uiso 1 1 calc R . . C15 C 0.8953(2) -0.1129(4) 0.3780(2) 0.0423(9) Uani 1 1 d . . . H15 H 0.9352 -0.0977 0.3644 0.051 Uiso 1 1 calc R . . C16 C 0.8677(2) -0.2301(4) 0.3749(2) 0.0429(9) Uani 1 1 d . . . H16 H 0.8890 -0.2955 0.3597 0.052 Uiso 1 1 calc R . . C17 C 0.8098(3) -0.2522(4) 0.3937(2) 0.0446(9) Uani 1 1 d . . . H17 H 0.7907 -0.3328 0.3906 0.054 Uiso 1 1 calc R . . C18 C 0.7785(2) -0.1584(4) 0.41744(19) 0.0347(7) Uani 1 1 d . . . H18 H 0.7381 -0.1740 0.4301 0.042 Uiso 1 1 calc R . . N1 N 0.71962(16) 0.2228(3) 0.46602(15) 0.0313(6) Uani 1 1 d . . . N2 N 0.79674(15) 0.0766(3) 0.51996(14) 0.0286(6) Uani 1 1 d . . . N3 N 0.96019(19) 0.1378(4) 0.58353(19) 0.0433(8) Uani 1 1 d . . . H3B H 0.986(4) 0.084(7) 0.571(4) 0.10(2) Uiso 1 1 d . . . H3A H 0.928(2) 0.187(4) 0.549(2) 0.025(9) Uiso 1 1 d . . . C19 C 0.2306(3) 0.0654(4) 0.9744(2) 0.0458(10) Uani 1 1 d . . . H19 H 0.2215 0.0236 0.9321 0.055 Uiso 1 1 calc R . . C20 C 0.2768(2) 0.1140(3) 1.08517(19) 0.0325(7) Uani 1 1 d . . . H20 H 0.3056 0.1116 1.1344 0.039 Uiso 1 1 calc R . . C21 C 0.2230(2) 0.1973(4) 1.04969(18) 0.0344(8) Uani 1 1 d . . . C22 C 0.1347(3) 0.2311(4) 0.9197(2) 0.0622(15) Uani 1 1 d . . . H22 H 0.1237 0.3010 0.9445 0.075 Uiso 1 1 calc R . . C23 C 0.0566(3) 0.1538(6) 0.8932(5) 0.157(6) Uani 1 1 d . . . H23A H 0.0351 0.1514 0.9282 0.188 Uiso 1 1 calc R . . H23B H 0.0615 0.0701 0.8779 0.188 Uiso 1 1 calc R . . C24 C 0.0084(3) 0.2500(7) 0.8248(3) 0.082(2) Uani 1 1 d . . . H24A H -0.0392 0.2074 0.7952 0.098 Uiso 1 1 calc R . . H24B H -0.0062 0.3213 0.8452 0.098 Uiso 1 1 calc R . . C25 C 0.0373(3) 0.2990(7) 0.7772(3) 0.0759(17) Uani 1 1 d . . . H25A H -0.0006 0.3542 0.7432 0.091 Uiso 1 1 calc R . . H25B H 0.0472 0.2316 0.7509 0.091 Uiso 1 1 calc R . . C26 C 0.1104(5) 0.3692(5) 0.8183(2) 0.100(3) Uani 1 1 d . . . H26A H 0.0983 0.4439 0.8380 0.120 Uiso 1 1 calc R . . H26B H 0.1321 0.3952 0.7857 0.120 Uiso 1 1 calc R . . C27 C 0.1705(3) 0.2951(5) 0.8786(3) 0.0564(13) Uani 1 1 d . . . H27 H 0.1858 0.2283 0.8549 0.068 Uiso 1 1 calc R . . C28 C 0.3353(2) -0.0704(4) 1.0522(2) 0.0411(9) Uani 1 1 d . . . H28 H 0.3271 -0.1099 1.0067 0.049 Uiso 1 1 calc R . . C29 C 0.3208(2) -0.1646(4) 1.0980(2) 0.0421(9) Uani 1 1 d . . . H29A H 0.3320 -0.1287 1.1439 0.063 Uiso 1 1 calc R . . H29B H 0.3534 -0.2356 1.1038 0.063 Uiso 1 1 calc R . . H29C H 0.2678 -0.1900 1.0758 0.063 Uiso 1 1 calc R . . C30 C 0.4166(3) -0.0210(5) 1.0863(3) 0.0552(12) Uani 1 1 d . . . H30A H 0.4236 0.0396 1.0554 0.083 Uiso 1 1 calc R . . H30B H 0.4523 -0.0884 1.0942 0.083 Uiso 1 1 calc R . . H30C H 0.4257 0.0173 1.1312 0.083 Uiso 1 1 calc R . . C31 C 0.1945(2) 0.3035(4) 1.07450(18) 0.0341(7) Uani 1 1 d . . . C32 C 0.2275(2) 0.4167(4) 1.0804(2) 0.0424(9) Uani 1 1 d . . . H32 H 0.2693 0.4266 1.0689 0.051 Uiso 1 1 calc R . . C33 C 0.1996(3) 0.5166(4) 1.1031(2) 0.0472(10) Uani 1 1 d . . . H33 H 0.2221 0.5948 1.1069 0.057 Uiso 1 1 calc R . . C34 C 0.1389(3) 0.5015(5) 1.1200(2) 0.0499(11) Uani 1 1 d . . . H34 H 0.1195 0.5695 1.1351 0.060 Uiso 1 1 calc R . . C35 C 0.1067(3) 0.3881(6) 1.1150(2) 0.0568(13) Uani 1 1 d . . . H35 H 0.0655 0.3779 1.1272 0.068 Uiso 1 1 calc R . . C36 C 0.1341(2) 0.2887(5) 1.0922(2) 0.0471(10) Uani 1 1 d . . . H36 H 0.1116 0.2106 1.0886 0.057 Uiso 1 1 calc R . . N4 N 0.28247(18) 0.0337(3) 1.03757(16) 0.0352(7) Uani 1 1 d . . . N5 N 0.1939(2) 0.1635(3) 0.97930(16) 0.0420(8) Uani 1 1 d . . . N6 N 0.2357(3) 0.3545(5) 0.9181(3) 0.0736(13) Uani 1 1 d D . . H6C H 0.206(4) 0.407(6) 0.933(4) 0.110 Uiso 1 1 d D . . H6D H 0.250(4) 0.387(7) 0.884(3) 0.110 Uiso 1 1 d D . . B1 B 0.23269(19) 0.9609(3) 0.27931(18) 0.0248(7) Uani 1 1 d . . . C37 C 0.26877(17) 0.8235(3) 0.30114(17) 0.0250(6) Uani 1 1 d . . . C38 C 0.23827(19) 0.7157(3) 0.26340(19) 0.0299(7) Uani 1 1 d . . . H38 H 0.1939 0.7210 0.2208 0.036 Uiso 1 1 calc R . . C39 C 0.2711(2) 0.6008(3) 0.2864(2) 0.0342(7) Uani 1 1 d . . . H39 H 0.2496 0.5300 0.2593 0.041 Uiso 1 1 calc R . . C40 C 0.3356(2) 0.5910(4) 0.3494(2) 0.0358(8) Uani 1 1 d . . . H40 H 0.3584 0.5136 0.3652 0.043 Uiso 1 1 calc R . . C41 C 0.36565(19) 0.6930(4) 0.38810(19) 0.0330(7) Uani 1 1 d . . . H41 H 0.4090 0.6862 0.4314 0.040 Uiso 1 1 calc R . . C42 C 0.33365(17) 0.8069(3) 0.36495(17) 0.0279(7) Uani 1 1 d . . . H42 H 0.3561 0.8764 0.3930 0.033 Uiso 1 1 calc R . . C43 C 0.15875(18) 0.9706(3) 0.20350(17) 0.0290(7) Uani 1 1 d . . . C44 C 0.09418(19) 1.0377(4) 0.1941(2) 0.0364(8) Uani 1 1 d . . . H44 H 0.0928 1.0761 0.2339 0.044 Uiso 1 1 calc R . . C45 C 0.0322(2) 1.0518(4) 0.1306(2) 0.0507(11) Uani 1 1 d . . . H45 H -0.0102 1.0983 0.1274 0.061 Uiso 1 1 calc R . . C46 C 0.0331(3) 0.9969(5) 0.0714(2) 0.0537(12) Uani 1 1 d . . . H46 H -0.0093 1.0042 0.0274 0.064 Uiso 1 1 calc R . . C47 C 0.0957(3) 0.9320(5) 0.0771(2) 0.0525(12) Uani 1 1 d . . . H47 H 0.0969 0.8955 0.0367 0.063 Uiso 1 1 calc R . . C48 C 0.1577(2) 0.9194(4) 0.14198(19) 0.0385(8) Uani 1 1 d . . . H48 H 0.2005 0.8748 0.1445 0.046 Uiso 1 1 calc R . . C49 C 0.29647(17) 1.0570(3) 0.27547(16) 0.0247(6) Uani 1 1 d . . . C50 C 0.36752(18) 1.0206(3) 0.28086(18) 0.0289(7) Uani 1 1 d . . . H50 H 0.3809 0.9367 0.2881 0.035 Uiso 1 1 calc R . . C51 C 0.41969(19) 1.1044(3) 0.27585(19) 0.0299(7) Uani 1 1 d . . . H51 H 0.4681 1.0768 0.2817 0.036 Uiso 1 1 calc R . . C52 C 0.40129(19) 1.2256(3) 0.26255(18) 0.0314(7) Uani 1 1 d . . . H52 H 0.4363 1.2820 0.2587 0.038 Uiso 1 1 calc R . . C53 C 0.3302(2) 1.2641(3) 0.25482(17) 0.0306(7) Uani 1 1 d . . . H53 H 0.3161 1.3474 0.2451 0.037 Uiso 1 1 calc R . . C54 C 0.27951(18) 1.1796(3) 0.26141(17) 0.0274(6) Uani 1 1 d . . . H54 H 0.2313 1.2079 0.2560 0.033 Uiso 1 1 calc R . . C55 C 0.20577(16) 0.9954(3) 0.34114(17) 0.0260(6) Uani 1 1 d . . . C56 C 0.2331(2) 1.0941(4) 0.38824(19) 0.0370(8) Uani 1 1 d . . . H56 H 0.2697 1.1474 0.3847 0.044 Uiso 1 1 calc R . . C57 C 0.2076(3) 1.1151(4) 0.4398(2) 0.0466(10) Uani 1 1 d . . . H57 H 0.2281 1.1810 0.4715 0.056 Uiso 1 1 calc R . . C58 C 0.1532(2) 1.0422(4) 0.4457(2) 0.0401(9) Uani 1 1 d . . . H58 H 0.1352 1.0588 0.4802 0.048 Uiso 1 1 calc R . . C59 C 0.1251(2) 0.9443(4) 0.4007(2) 0.0378(8) Uani 1 1 d . . . H59 H 0.0878 0.8925 0.4042 0.045 Uiso 1 1 calc R . . C60 C 0.15173(19) 0.9223(4) 0.3503(2) 0.0351(8) Uani 1 1 d . . . H60 H 0.1323 0.8538 0.3204 0.042 Uiso 1 1 calc R . . B2 B 0.22528(19) 0.8074(3) 0.77861(19) 0.0245(7) Uani 1 1 d . . . C61 C 0.19901(16) 0.7697(3) 0.84103(16) 0.0239(6) Uani 1 1 d . . . C62 C 0.2339(2) 0.6828(3) 0.89210(19) 0.0318(7) Uani 1 1 d . . . H62 H 0.2744 0.6371 0.8904 0.038 Uiso 1 1 calc R . . C63 C 0.2121(2) 0.6591(4) 0.9463(2) 0.0388(8) Uani 1 1 d . . . H63 H 0.2382 0.5997 0.9810 0.047 Uiso 1 1 calc R . . C64 C 0.1519(2) 0.7233(4) 0.94896(19) 0.0355(8) Uani 1 1 d . . . H64 H 0.1356 0.7068 0.9846 0.043 Uiso 1 1 calc R . . C65 C 0.11614(18) 0.8118(4) 0.89878(18) 0.0334(7) Uani 1 1 d . . . H65 H 0.0751 0.8565 0.9002 0.040 Uiso 1 1 calc R . . C66 C 0.13980(18) 0.8354(3) 0.84651(17) 0.0290(7) Uani 1 1 d . . . H66 H 0.1153 0.8979 0.8134 0.035 Uiso 1 1 calc R . . C67 C 0.26168(17) 0.9439(3) 0.80175(17) 0.0255(6) Uani 1 1 d . . . C68 C 0.32717(19) 0.9559(3) 0.86469(18) 0.0299(7) Uani 1 1 d . . . H68 H 0.3487 0.8845 0.8912 0.036 Uiso 1 1 calc R . . C69 C 0.3620(2) 1.0682(4) 0.8900(2) 0.0349(8) Uani 1 1 d . . . H69 H 0.4060 1.0724 0.9329 0.042 Uiso 1 1 calc R . . C70 C 0.3313(2) 1.1747(3) 0.8513(2) 0.0363(8) Uani 1 1 d . . . H70 H 0.3550 1.2515 0.8672 0.044 Uiso 1 1 calc R . . C71 C 0.2676(2) 1.1665(3) 0.7911(2) 0.0358(8) Uani 1 1 d . . . H71 H 0.2464 1.2385 0.7651 0.043 Uiso 1 1 calc R . . C72 C 0.23196(19) 1.0531(3) 0.76633(18) 0.0286(6) Uani 1 1 d . . . H72 H 0.1866 1.0508 0.7245 0.034 Uiso 1 1 calc R . . C73 C 0.28858(16) 0.7134(3) 0.77380(16) 0.0236(6) Uani 1 1 d . . . C74 C 0.35907(18) 0.7486(3) 0.77695(17) 0.0266(6) Uani 1 1 d . . . H74 H 0.3724 0.8326 0.7837 0.032 Uiso 1 1 calc R . . C75 C 0.41043(19) 0.6671(3) 0.77075(19) 0.0313(7) Uani 1 1 d . . . H75 H 0.4573 0.6959 0.7729 0.038 Uiso 1 1 calc R . . C76 C 0.39319(18) 0.5430(3) 0.76138(18) 0.0299(7) Uani 1 1 d . . . H76 H 0.4284 0.4861 0.7583 0.036 Uiso 1 1 calc R . . C77 C 0.32337(19) 0.5044(3) 0.75663(18) 0.0319(7) Uani 1 1 d . . . H77 H 0.3104 0.4203 0.7494 0.038 Uiso 1 1 calc R . . C78 C 0.27253(18) 0.5867(3) 0.76228(18) 0.0274(6) Uani 1 1 d . . . H78 H 0.2251 0.5574 0.7583 0.033 Uiso 1 1 calc R . . C79 C 0.15172(17) 0.8005(3) 0.70260(17) 0.0263(6) Uani 1 1 d . . . C80 C 0.1495(2) 0.8552(4) 0.64189(18) 0.0355(8) Uani 1 1 d . . . H80 H 0.1921 0.9015 0.6452 0.043 Uiso 1 1 calc R . . C81 C 0.0884(2) 0.8454(5) 0.5768(2) 0.0453(10) Uani 1 1 d . . . H81 H 0.0894 0.8872 0.5377 0.054 Uiso 1 1 calc R . . C82 C 0.0258(2) 0.7751(5) 0.5684(2) 0.0487(11) Uani 1 1 d . . . H82 H -0.0159 0.7673 0.5240 0.058 Uiso 1 1 calc R . . C83 C 0.0262(2) 0.7165(5) 0.6271(2) 0.0420(9) Uani 1 1 d . . . H83 H -0.0157 0.6674 0.6228 0.050 Uiso 1 1 calc R . . C84 C 0.08715(18) 0.7291(4) 0.69188(19) 0.0320(7) Uani 1 1 d . . . H84 H 0.0855 0.6880 0.7309 0.038 Uiso 1 1 calc R . . C85 C 0.38499(18) 0.2696(4) 0.55827(18) 0.0331(7) Uani 1 1 d . . . H85A H 0.3332 0.3005 0.5304 0.040 Uiso 1 1 calc R . . H85B H 0.3835 0.2156 0.5953 0.040 Uiso 1 1 calc R . . C86 C 0.4101(2) 0.2019(5) 0.5142(2) 0.0458(10) Uani 1 1 d . . . H86A H 0.3746 0.1341 0.4916 0.055 Uiso 1 1 calc R . . H86B H 0.4606 0.1667 0.5425 0.055 Uiso 1 1 calc R . . C87 C 0.4140(2) 0.2865(4) 0.4587(2) 0.0446(9) Uani 1 1 d . . . H87A H 0.4311 0.2398 0.4279 0.053 Uiso 1 1 calc R . . H87B H 0.3629 0.3190 0.4296 0.053 Uiso 1 1 calc R . . C88 C 0.46350(18) 0.3837(3) 0.48880(18) 0.0291(7) Uani 1 1 d . . . H88A H 0.4640 0.4384 0.4516 0.035 Uiso 1 1 calc R . . H88B H 0.5153 0.3521 0.5155 0.035 Uiso 1 1 calc R . . C89 C 0.4399(3) 0.4502(5) 0.5344(3) 0.0527(11) Uani 1 1 d . . . H89A H 0.3899 0.4878 0.5067 0.063 Uiso 1 1 calc R . . H89B H 0.4764 0.5167 0.5572 0.063 Uiso 1 1 calc R . . C90 C 0.4345(3) 0.3694(6) 0.5894(3) 0.0620(14) Uani 1 1 d . . . H90A H 0.4854 0.3381 0.6202 0.074 Uiso 1 1 calc R . . H90B H 0.4156 0.4173 0.6186 0.074 Uiso 1 1 calc R . . C91A C 0.52922(17) 0.5100(3) 0.26780(16) 0.0205(5) Uani 0.783(8) 1 d P A 1 H91A H 0.4997 0.4746 0.2209 0.025 Uiso 0.783(8) 1 calc PR A 1 H91B H 0.5586 0.4439 0.2997 0.025 Uiso 0.783(8) 1 calc PR A 1 C92A C 0.4801(3) 0.5654(5) 0.2933(3) 0.0373(12) Uani 0.783(8) 1 d P A 1 H92A H 0.5103 0.6014 0.3399 0.045 Uiso 0.783(8) 1 calc PR A 1 H92B H 0.4465 0.5025 0.2987 0.045 Uiso 0.783(8) 1 calc PR A 1 C93A C 0.4324(3) 0.6646(5) 0.2437(3) 0.0338(11) Uani 0.783(8) 1 d P A 1 H93A H 0.4022 0.6299 0.1968 0.041 Uiso 0.783(8) 1 calc PR A 1 H93B H 0.3975 0.7011 0.2615 0.041 Uiso 0.783(8) 1 calc PR A 1 C94A C 0.48463(18) 0.7572(3) 0.24003(17) 0.0235(6) Uani 0.783(8) 1 d P A 1 H94A H 0.4558 0.8251 0.2095 0.028 Uiso 0.783(8) 1 calc PR A 1 H94B H 0.5151 0.7905 0.2873 0.028 Uiso 0.783(8) 1 calc PR A 1 C95A C 0.5326(3) 0.7045(4) 0.2131(3) 0.0322(11) Uani 0.783(8) 1 d P A 1 H95A H 0.5662 0.7677 0.2080 0.039 Uiso 0.783(8) 1 calc PR A 1 H95B H 0.5023 0.6687 0.1664 0.039 Uiso 0.783(8) 1 calc PR A 1 C96A C 0.5800(4) 0.6047(6) 0.2640(4) 0.0389(13) Uani 0.783(8) 1 d P A 1 H96A H 0.6161 0.5691 0.2475 0.047 Uiso 0.783(8) 1 calc PR A 1 H96B H 0.6090 0.6403 0.3110 0.047 Uiso 0.783(8) 1 calc PR A 1 C91B C 0.52922(17) 0.5100(3) 0.26780(16) 0.0205(5) Uani 0.217(8) 1 d PD A 2 H91C H 0.5547 0.5100 0.3196 0.025 Uiso 0.217(8) 1 calc PR A 2 H91D H 0.5286 0.4257 0.2507 0.025 Uiso 0.217(8) 1 calc PR A 2 C92B C 0.4460(9) 0.5625(15) 0.2410(10) 0.035(4) Uani 0.217(8) 1 d P A 2 H92C H 0.4226 0.5705 0.1894 0.042 Uiso 0.217(8) 1 calc PR A 2 H92D H 0.4142 0.5078 0.2548 0.042 Uiso 0.217(8) 1 calc PR A 2 C93B C 0.4533(12) 0.6821(19) 0.2740(12) 0.038(5) Uani 0.217(8) 1 d PU A 2 H93C H 0.4033 0.7133 0.2679 0.045 Uiso 0.217(8) 1 calc PR A 2 H93D H 0.4867 0.6774 0.3246 0.045 Uiso 0.217(8) 1 calc PR A 2 C94B C 0.48463(18) 0.7572(3) 0.24003(17) 0.0235(6) Uani 0.217(8) 1 d P A 2 H94C H 0.4839 0.8438 0.2531 0.028 Uiso 0.217(8) 1 calc PR A 2 H94D H 0.4574 0.7490 0.1886 0.028 Uiso 0.217(8) 1 calc PR A 2 C95B C 0.5718(10) 0.7056(19) 0.2685(13) 0.049(6) Uani 0.217(8) 1 d PD A 2 H95C H 0.6024 0.7590 0.2526 0.059 Uiso 0.217(8) 1 calc PR A 2 H95D H 0.5960 0.7020 0.3202 0.059 Uiso 0.217(8) 1 calc PR A 2 C96B C 0.5653(17) 0.5891(15) 0.2399(15) 0.047(8) Uani 0.217(8) 1 d PDU A 2 H96C H 0.5362 0.5935 0.1885 0.056 Uiso 0.217(8) 1 calc PR A 2 H96D H 0.6163 0.5571 0.2499 0.056 Uiso 0.217(8) 1 calc PR A 2 C97 C 0.4448(3) 0.3288(5) 0.0356(3) 0.0569(12) Uani 1 1 d . . . H97A H 0.4804 0.2605 0.0568 0.068 Uiso 1 1 calc R . . H97B H 0.3941 0.2935 0.0083 0.068 Uiso 1 1 calc R . . C98 C 0.4424(3) 0.4078(6) 0.0924(2) 0.0566(12) Uani 1 1 d . . . H98A H 0.4238 0.3594 0.1216 0.068 Uiso 1 1 calc R . . H98B H 0.4940 0.4365 0.1227 0.068 Uiso 1 1 calc R . . C99 C 0.39380(18) 0.5111(4) 0.06384(18) 0.0323(7) Uani 1 1 d . . . H99A H 0.3412 0.4831 0.0370 0.039 Uiso 1 1 calc R . . H99B H 0.3951 0.5644 0.1023 0.039 Uiso 1 1 calc R . . C100 C 0.4178(2) 0.5770(5) 0.0200(2) 0.0469(10) Uani 1 1 d . . . H10A H 0.4692 0.6094 0.0478 0.056 Uiso 1 1 calc R . . H10B H 0.3835 0.6472 -0.0003 0.056 Uiso 1 1 calc R . . C101 C 0.4185(2) 0.4979(4) -0.0382(2) 0.0459(9) Uani 1 1 d . . . H10C H 0.3667 0.4693 -0.0679 0.055 Uiso 1 1 calc R . . H10D H 0.4367 0.5459 -0.0678 0.055 Uiso 1 1 calc R . . C102 C 0.46737(19) 0.3946(3) -0.00895(19) 0.0318(7) Uani 1 1 d . . . H10E H 0.4660 0.3408 -0.0472 0.038 Uiso 1 1 calc R . . H10F H 0.5200 0.4233 0.0174 0.038 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0242(13) 0.0395(18) 0.0254(15) -0.0017(13) 0.0100(12) 0.0050(13) C2 0.0390(17) 0.0360(19) 0.0265(16) 0.0021(14) 0.0128(14) 0.0059(15) C3 0.0286(14) 0.0312(16) 0.0244(14) 0.0018(13) 0.0132(12) -0.0006(13) C4 0.0298(14) 0.0347(16) 0.0247(14) 0.0040(13) 0.0130(12) 0.0111(13) C5 0.0307(16) 0.059(2) 0.0353(18) 0.0141(17) 0.0176(14) 0.0100(16) C6 0.044(2) 0.069(3) 0.044(2) 0.030(2) 0.0221(18) 0.021(2) C7 0.042(2) 0.111(4) 0.0318(19) 0.022(2) 0.0152(16) 0.022(3) C8 0.0340(18) 0.077(3) 0.0321(17) 0.013(2) 0.0112(15) 0.021(2) C9 0.0312(16) 0.050(2) 0.0245(14) -0.0008(14) 0.0110(13) 0.0116(15) C10 0.0362(17) 0.0305(17) 0.0344(17) 0.0058(14) 0.0172(14) 0.0075(14) C11 0.0361(19) 0.044(2) 0.063(3) 0.013(2) 0.0256(19) 0.0112(17) C12 0.0412(18) 0.0346(19) 0.043(2) 0.0068(16) 0.0197(16) 0.0054(15) C13 0.0323(15) 0.0323(17) 0.0234(14) 0.0044(13) 0.0135(12) 0.0061(13) C14 0.0315(16) 0.045(2) 0.0326(17) 0.0003(15) 0.0177(14) 0.0026(15) C15 0.0337(17) 0.058(3) 0.0348(18) -0.0079(17) 0.0139(15) 0.0071(17) C16 0.0413(19) 0.049(2) 0.0335(18) -0.0156(17) 0.0108(15) 0.0119(17) C17 0.064(3) 0.0309(19) 0.037(2) 0.0012(15) 0.0196(19) 0.0051(18) C18 0.0462(19) 0.0321(17) 0.0308(16) 0.0043(14) 0.0210(15) 0.0023(15) N1 0.0309(13) 0.0315(15) 0.0309(14) 0.0004(12) 0.0126(12) 0.0039(12) N2 0.0243(12) 0.0361(15) 0.0258(13) 0.0000(11) 0.0110(10) 0.0038(11) N3 0.0332(15) 0.057(2) 0.0433(17) 0.0103(16) 0.0198(14) -0.0061(15) C19 0.059(2) 0.042(2) 0.0321(18) -0.0069(16) 0.0142(17) -0.0112(19) C20 0.0348(17) 0.0322(18) 0.0295(16) 0.0000(14) 0.0127(14) 0.0020(14) C21 0.0413(18) 0.0323(18) 0.0272(16) 0.0058(14) 0.0120(14) -0.0043(14) C22 0.073(3) 0.043(2) 0.038(2) 0.0104(18) -0.008(2) -0.016(2) C23 0.057(3) 0.051(3) 0.229(10) -0.062(5) -0.070(5) 0.026(3) C24 0.067(3) 0.129(6) 0.051(3) 0.031(3) 0.028(2) 0.065(4) C25 0.074(3) 0.088(4) 0.055(3) 0.012(3) 0.017(3) 0.024(3) C26 0.200(8) 0.050(3) 0.026(2) 0.0049(19) 0.025(3) -0.034(4) C27 0.066(3) 0.067(3) 0.052(2) 0.013(2) 0.041(2) 0.034(3) C28 0.047(2) 0.042(2) 0.041(2) -0.0074(17) 0.0245(17) 0.0041(17) C29 0.045(2) 0.036(2) 0.047(2) -0.0010(17) 0.0217(17) 0.0040(16) C30 0.044(2) 0.062(3) 0.067(3) 0.002(2) 0.031(2) -0.004(2) C31 0.0356(17) 0.0340(18) 0.0262(16) 0.0060(14) 0.0068(13) 0.0038(14) C32 0.050(2) 0.038(2) 0.045(2) 0.0071(17) 0.0253(18) -0.0005(17) C33 0.069(3) 0.0312(19) 0.046(2) 0.0060(17) 0.028(2) 0.0047(18) C34 0.049(2) 0.062(3) 0.0322(19) 0.0010(19) 0.0098(17) 0.019(2) C35 0.039(2) 0.090(4) 0.043(2) -0.020(2) 0.0190(18) -0.012(2) C36 0.043(2) 0.057(3) 0.040(2) -0.0155(19) 0.0169(17) -0.0169(19) N4 0.0411(15) 0.0346(16) 0.0314(14) -0.0021(12) 0.0167(13) -0.0060(13) N5 0.0505(18) 0.0329(16) 0.0294(15) 0.0001(12) 0.0040(13) -0.0069(14) N6 0.077(3) 0.074(3) 0.075(3) 0.003(3) 0.038(3) 0.002(3) B1 0.0233(14) 0.0277(17) 0.0229(15) -0.0033(13) 0.0094(13) 0.0015(13) C37 0.0247(13) 0.0280(16) 0.0264(15) 0.0042(12) 0.0149(12) 0.0027(11) C38 0.0290(15) 0.0294(16) 0.0344(17) 0.0004(14) 0.0164(13) 0.0030(13) C39 0.0415(19) 0.0274(17) 0.0399(19) 0.0004(14) 0.0232(16) -0.0014(14) C40 0.0371(17) 0.0331(19) 0.045(2) 0.0162(16) 0.0254(16) 0.0122(15) C41 0.0266(15) 0.044(2) 0.0318(16) 0.0103(15) 0.0154(13) 0.0041(14) C42 0.0247(14) 0.0359(18) 0.0243(14) 0.0026(13) 0.0114(12) 0.0015(13) C43 0.0304(15) 0.0272(16) 0.0255(15) -0.0015(12) 0.0081(12) -0.0042(12) C44 0.0288(15) 0.0314(18) 0.0386(18) 0.0011(15) 0.0041(14) 0.0020(13) C45 0.0369(19) 0.040(2) 0.055(2) 0.001(2) -0.0011(18) 0.0034(17) C46 0.051(2) 0.046(2) 0.038(2) 0.0085(19) -0.0080(18) -0.009(2) C47 0.077(3) 0.047(2) 0.0235(17) 0.0010(17) 0.0114(18) -0.015(2) C48 0.046(2) 0.039(2) 0.0310(18) 0.0013(15) 0.0172(16) -0.0011(16) C49 0.0257(13) 0.0250(15) 0.0239(14) -0.0002(12) 0.0111(11) 0.0005(12) C50 0.0266(14) 0.0289(16) 0.0324(16) 0.0027(13) 0.0136(12) 0.0023(12) C51 0.0262(15) 0.0322(17) 0.0340(16) 0.0040(14) 0.0155(13) 0.0005(12) C52 0.0333(16) 0.0315(17) 0.0318(16) 0.0022(14) 0.0161(14) -0.0037(13) C53 0.0403(17) 0.0258(16) 0.0295(16) 0.0000(13) 0.0185(14) 0.0005(14) C54 0.0286(15) 0.0281(16) 0.0266(15) -0.0009(12) 0.0126(12) 0.0038(12) C55 0.0215(13) 0.0274(16) 0.0293(15) -0.0001(13) 0.0110(12) 0.0012(11) C56 0.048(2) 0.0366(19) 0.0304(17) -0.0070(15) 0.0206(16) -0.0125(16) C57 0.066(3) 0.048(2) 0.0339(19) -0.0111(18) 0.029(2) -0.010(2) C58 0.047(2) 0.046(2) 0.0314(18) 0.0015(16) 0.0205(16) 0.0072(17) C59 0.0287(15) 0.045(2) 0.046(2) 0.0013(17) 0.0216(15) 0.0022(15) C60 0.0287(15) 0.0376(19) 0.043(2) -0.0101(16) 0.0189(15) -0.0051(14) B2 0.0229(14) 0.0234(16) 0.0277(16) -0.0005(13) 0.0110(13) 0.0030(12) C61 0.0235(13) 0.0255(15) 0.0216(13) -0.0002(11) 0.0084(11) -0.0016(11) C62 0.0340(16) 0.0302(17) 0.0354(17) 0.0043(14) 0.0188(14) 0.0051(13) C63 0.049(2) 0.0337(18) 0.0376(19) 0.0115(15) 0.0218(17) 0.0053(16) C64 0.0390(18) 0.043(2) 0.0349(18) 0.0012(16) 0.0253(15) -0.0062(16) C65 0.0254(14) 0.044(2) 0.0339(17) -0.0007(15) 0.0153(13) 0.0015(14) C66 0.0264(14) 0.0322(17) 0.0273(15) 0.0034(13) 0.0104(12) 0.0047(12) C67 0.0268(14) 0.0265(15) 0.0297(15) 0.0006(12) 0.0181(12) 0.0018(12) C68 0.0329(16) 0.0298(16) 0.0332(17) -0.0042(14) 0.0202(14) -0.0036(13) C69 0.0353(17) 0.0368(19) 0.0397(18) -0.0130(16) 0.0228(15) -0.0079(15) C70 0.0438(19) 0.0283(17) 0.050(2) -0.0105(16) 0.0326(17) -0.0090(15) C71 0.0426(19) 0.0220(15) 0.054(2) 0.0003(15) 0.0315(18) -0.0019(14) C72 0.0316(15) 0.0241(15) 0.0340(16) 0.0009(13) 0.0175(13) 0.0010(12) C73 0.0213(13) 0.0265(15) 0.0213(13) 0.0019(12) 0.0075(11) 0.0006(11) C74 0.0288(14) 0.0246(15) 0.0270(15) -0.0028(12) 0.0123(12) -0.0024(12) C75 0.0258(14) 0.0345(18) 0.0353(17) 0.0000(14) 0.0146(13) 0.0007(13) C76 0.0292(15) 0.0295(17) 0.0340(17) -0.0012(13) 0.0161(13) 0.0064(13) C77 0.0369(17) 0.0227(15) 0.0358(17) -0.0001(14) 0.0148(14) 0.0005(13) C78 0.0252(14) 0.0254(16) 0.0342(16) -0.0010(12) 0.0152(13) -0.0033(12) C79 0.0272(14) 0.0269(15) 0.0280(15) -0.0012(12) 0.0147(12) 0.0034(12) C80 0.0421(19) 0.0379(19) 0.0271(16) 0.0034(14) 0.0153(15) 0.0014(15) C81 0.053(2) 0.051(2) 0.0305(18) 0.0046(17) 0.0168(17) 0.0126(19) C82 0.0368(19) 0.069(3) 0.0285(17) -0.0095(19) 0.0025(15) 0.016(2) C83 0.0246(15) 0.057(2) 0.0394(19) -0.0133(19) 0.0085(14) 0.0016(16) C84 0.0255(14) 0.0386(19) 0.0333(17) -0.0002(15) 0.0137(13) 0.0036(13) C85 0.0244(14) 0.050(2) 0.0281(16) 0.0013(15) 0.0143(13) -0.0045(14) C86 0.0386(19) 0.052(2) 0.044(2) 0.0156(19) 0.0148(17) 0.0062(18) C87 0.048(2) 0.048(2) 0.040(2) 0.0051(18) 0.0215(17) 0.0021(18) C88 0.0251(14) 0.0328(17) 0.0343(16) 0.0069(14) 0.0173(13) -0.0020(12) C89 0.050(2) 0.051(3) 0.058(3) -0.010(2) 0.024(2) -0.002(2) C90 0.060(3) 0.080(4) 0.045(2) -0.009(2) 0.021(2) -0.013(3) C91A 0.0288(13) 0.0112(11) 0.0294(14) 0.0035(10) 0.0198(11) 0.0041(10) C92A 0.046(3) 0.031(2) 0.044(3) 0.007(2) 0.028(2) 0.005(2) C93A 0.035(2) 0.033(3) 0.039(3) 0.003(2) 0.021(2) -0.0008(19) C94A 0.0351(15) 0.0119(12) 0.0344(15) 0.0035(11) 0.0253(13) 0.0049(11) C95A 0.038(2) 0.031(2) 0.037(3) 0.0034(19) 0.025(2) 0.0017(18) C96A 0.041(3) 0.030(3) 0.051(4) 0.009(3) 0.024(3) 0.003(2) C91B 0.0288(13) 0.0112(11) 0.0294(14) 0.0035(10) 0.0198(11) 0.0041(10) C92B 0.034(8) 0.027(8) 0.049(11) 0.015(7) 0.023(8) 0.003(6) C93B 0.038(5) 0.038(5) 0.038(5) 0.001(2) 0.017(3) -0.002(2) C94B 0.0351(15) 0.0119(12) 0.0344(15) 0.0035(11) 0.0253(13) 0.0049(11) C95B 0.030(8) 0.049(12) 0.078(16) -0.019(10) 0.030(10) -0.024(8) C96B 0.047(8) 0.047(8) 0.047(8) 0.001(2) 0.020(4) 0.000(2) C97 0.058(3) 0.052(3) 0.048(2) 0.003(2) 0.010(2) 0.003(2) C98 0.055(3) 0.073(3) 0.040(2) 0.011(2) 0.018(2) 0.010(2) C99 0.0256(14) 0.046(2) 0.0265(15) -0.0015(14) 0.0119(12) 0.0061(14) C100 0.0327(18) 0.058(3) 0.046(2) -0.003(2) 0.0125(16) 0.0089(18) C101 0.046(2) 0.049(2) 0.042(2) 0.0042(18) 0.0172(17) 0.0132(19) C102 0.0303(15) 0.0351(17) 0.0314(16) 0.0024(14) 0.0143(13) 0.0105(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.316(4) . ? C1 N2 1.340(4) . ? C1 H1 0.9500 . ? C2 C3 1.338(5) . ? C2 N1 1.402(5) . ? C2 H2 0.9500 . ? C3 N2 1.384(4) . ? C3 C13 1.495(5) . ? C4 N2 1.488(4) . ? C4 C9 1.527(5) . ? C4 C5 1.537(5) . ? C4 H4 1.0000 . ? C5 C6 1.531(5) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C7 1.498(8) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.538(6) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.541(5) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 N3 1.464(5) . ? C9 H9 1.0000 . ? C10 N1 1.485(5) . ? C10 C12 1.513(5) . ? C10 C11 1.517(5) . ? C10 H10 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.375(5) . ? C13 C18 1.392(5) . ? C14 C15 1.405(5) . ? C14 H14 0.9500 . ? C15 C16 1.383(7) . ? C15 H15 0.9500 . ? C16 C17 1.369(6) . ? C16 H16 0.9500 . ? C17 C18 1.391(6) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? N3 H3B 0.89(8) . ? N3 H3A 0.91(4) . ? C19 N5 1.321(6) . ? C19 N4 1.335(5) . ? C19 H19 0.9500 . ? C20 C21 1.353(5) . ? C20 N4 1.374(5) . ? C20 H20 0.9500 . ? C21 N5 1.396(5) . ? C21 C31 1.477(6) . ? C22 N5 1.495(5) . ? C22 C27 1.498(7) . ? C22 C23 1.624(9) . ? C22 H22 1.0000 . ? C23 C24 1.712(10) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 C25 1.446(8) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C26 1.528(10) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 C27 1.546(8) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 N6 1.357(8) . ? C27 H27 1.0000 . ? C28 N4 1.480(5) . ? C28 C29 1.519(6) . ? C28 C30 1.538(6) . ? C28 H28 1.0000 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 C32 1.379(6) . ? C31 C36 1.388(6) . ? C32 C33 1.395(6) . ? C32 H32 0.9500 . ? C33 C34 1.383(7) . ? C33 H33 0.9500 . ? C34 C35 1.376(8) . ? C34 H34 0.9500 . ? C35 C36 1.386(7) . ? C35 H35 0.9500 . ? C36 H36 0.9500 . ? N6 H6C 0.96(2) . ? N6 H6D 0.95(2) . ? B1 C55 1.642(5) . ? B1 C37 1.643(5) . ? B1 C43 1.644(5) . ? B1 C49 1.658(5) . ? C37 C38 1.407(5) . ? C37 C42 1.417(4) . ? C38 C39 1.403(5) . ? C38 H38 0.9500 . ? C39 C40 1.396(6) . ? C39 H39 0.9500 . ? C40 C41 1.362(6) . ? C40 H40 0.9500 . ? C41 C42 1.388(5) . ? C41 H41 0.9500 . ? C42 H42 0.9500 . ? C43 C44 1.399(5) . ? C43 C48 1.406(5) . ? C44 C45 1.383(5) . ? C44 H44 0.9500 . ? C45 C46 1.392(7) . ? C45 H45 0.9500 . ? C46 C47 1.375(8) . ? C46 H46 0.9500 . ? C47 C48 1.400(6) . ? C47 H47 0.9500 . ? C48 H48 0.9500 . ? C49 C54 1.385(5) . ? C49 C50 1.401(4) . ? C50 C51 1.408(5) . ? C50 H50 0.9500 . ? C51 C52 1.373(5) . ? C51 H51 0.9500 . ? C52 C53 1.392(5) . ? C52 H52 0.9500 . ? C53 C54 1.405(5) . ? C53 H53 0.9500 . ? C54 H54 0.9500 . ? C55 C60 1.402(5) . ? C55 C56 1.411(5) . ? C56 C57 1.393(5) . ? C56 H56 0.9500 . ? C57 C58 1.375(6) . ? C57 H57 0.9500 . ? C58 C59 1.383(6) . ? C58 H58 0.9500 . ? C59 C60 1.386(5) . ? C59 H59 0.9500 . ? C60 H60 0.9500 . ? B2 C67 1.639(5) . ? B2 C79 1.641(5) . ? B2 C73 1.645(5) . ? B2 C61 1.654(5) . ? C61 C62 1.382(5) . ? C61 C66 1.407(4) . ? C62 C63 1.402(5) . ? C62 H62 0.9500 . ? C63 C64 1.390(6) . ? C63 H63 0.9500 . ? C64 C65 1.386(6) . ? C64 H64 0.9500 . ? C65 C66 1.388(5) . ? C65 H65 0.9500 . ? C66 H66 0.9500 . ? C67 C72 1.400(5) . ? C67 C68 1.407(5) . ? C68 C69 1.397(5) . ? C68 H68 0.9500 . ? C69 C70 1.405(6) . ? C69 H69 0.9500 . ? C70 C71 1.355(6) . ? C70 H70 0.9500 . ? C71 C72 1.412(5) . ? C71 H71 0.9500 . ? C72 H72 0.9500 . ? C73 C74 1.404(4) . ? C73 C78 1.421(5) . ? C74 C75 1.390(5) . ? C74 H74 0.9500 . ? C75 C76 1.394(5) . ? C75 H75 0.9500 . ? C76 C77 1.390(5) . ? C76 H76 0.9500 . ? C77 C78 1.383(5) . ? C77 H77 0.9500 . ? C78 H78 0.9500 . ? C79 C80 1.397(5) . ? C79 C84 1.418(5) . ? C80 C81 1.391(5) . ? C80 H80 0.9500 . ? C81 C82 1.391(7) . ? C81 H81 0.9500 . ? C82 C83 1.391(7) . ? C82 H82 0.9500 . ? C83 C84 1.389(5) . ? C83 H83 0.9500 . ? C84 H84 0.9500 . ? C85 C90 1.424(7) . ? C85 C86 1.426(6) . ? C85 H85A 0.9900 . ? C85 H85B 0.9900 . ? C86 C87 1.520(6) . ? C86 H86A 0.9900 . ? C86 H86B 0.9900 . ? C87 C88 1.397(6) . ? C87 H87A 0.9900 . ? C87 H87B 0.9900 . ? C88 C89 1.430(6) . ? C88 H88A 0.9900 . ? C88 H88B 0.9900 . ? C89 C90 1.497(8) . ? C89 H89A 0.9900 . ? C89 H89B 0.9900 . ? C90 H90A 0.9900 . ? C90 H90B 0.9900 . ? C91A C92A 1.419(5) . ? C91A C96A 1.460(6) . ? C91A H91A 0.9900 . ? C91A H91B 0.9900 . ? C92A C93A 1.522(8) . ? C92A H92A 0.9900 . ? C92A H92B 0.9900 . ? C93A C94A 1.463(6) . ? C93A H93A 0.9900 . ? C93A H93B 0.9900 . ? C94A C95A 1.409(5) . ? C94A H94A 0.9900 . ? C94A H94B 0.9900 . ? C95A C96A 1.538(7) . ? C95A H95A 0.9900 . ? C95A H95B 0.9900 . ? C96A H96A 0.9900 . ? C96A H96B 0.9900 . ? C92B C93B 1.46(3) . ? C92B H92C 0.9900 . ? C92B H92D 0.9900 . ? C93B H93C 0.9900 . ? C93B H93D 0.9900 . ? C95B C96B 1.39(2) . ? C95B H95C 0.9900 . ? C95B H95D 0.9900 . ? C96B H96C 0.9900 . ? C96B H96D 0.9900 . ? C97 C102 1.396(6) . ? C97 C98 1.493(7) . ? C97 H97A 0.9900 . ? C97 H97B 0.9900 . ? C98 C99 1.436(6) . ? C98 H98A 0.9900 . ? C98 H98B 0.9900 . ? C99 C100 1.399(6) . ? C99 H99A 0.9900 . ? C99 H99B 0.9900 . ? C100 C101 1.507(6) . ? C100 H10A 0.9900 . ? C100 H10B 0.9900 . ? C101 C102 1.440(5) . ? C101 H10C 0.9900 . ? C101 H10D 0.9900 . ? C102 H10E 0.9900 . ? C102 H10F 0.9900 . ? 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 N1 C1 N2 109.0(3) . . ? N1 C1 H1 125.5 . . ? N2 C1 H1 125.5 . . ? C3 C2 N1 107.1(3) . . ? C3 C2 H2 126.5 . . ? N1 C2 H2 126.5 . . ? C2 C3 N2 107.4(3) . . ? C2 C3 C13 130.6(3) . . ? N2 C3 C13 122.0(3) . . ? N2 C4 C9 110.0(3) . . ? N2 C4 C5 109.1(3) . . ? C9 C4 C5 113.4(3) . . ? N2 C4 H4 108.1 . . ? C9 C4 H4 108.1 . . ? C5 C4 H4 108.1 . . ? C6 C5 C4 110.3(3) . . ? C6 C5 H5A 109.6 . . ? C4 C5 H5A 109.6 . . ? C6 C5 H5B 109.6 . . ? C4 C5 H5B 109.6 . . ? H5A C5 H5B 108.1 . . ? C7 C6 C5 110.7(4) . . ? C7 C6 H6A 109.5 . . ? C5 C6 H6A 109.5 . . ? C7 C6 H6B 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 108.1 . . ? C6 C7 C8 111.5(4) . . ? C6 C7 H7A 109.3 . . ? C8 C7 H7A 109.3 . . ? C6 C7 H7B 109.3 . . ? C8 C7 H7B 109.3 . . ? H7A C7 H7B 108.0 . . ? C7 C8 C9 112.7(3) . . ? C7 C8 H8A 109.1 . . ? C9 C8 H8A 109.1 . . ? C7 C8 H8B 109.1 . . ? C9 C8 H8B 109.1 . . ? H8A C8 H8B 107.8 . . ? N3 C9 C4 114.1(3) . . ? N3 C9 C8 109.9(3) . . ? C4 C9 C8 108.2(4) . . ? N3 C9 H9 108.1 . . ? C4 C9 H9 108.1 . . ? C8 C9 H9 108.1 . . ? N1 C10 C12 110.1(3) . . ? N1 C10 C11 110.4(3) . . ? C12 C10 C11 112.0(3) . . ? N1 C10 H10 108.1 . . ? C12 C10 H10 108.1 . . ? C11 C10 H10 108.1 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C14 C13 C18 121.4(3) . . ? C14 C13 C3 118.9(3) . . ? C18 C13 C3 119.7(3) . . ? C13 C14 C15 119.1(4) . . ? C13 C14 H14 120.5 . . ? C15 C14 H14 120.5 . . ? C16 C15 C14 119.7(4) . . ? C16 C15 H15 120.1 . . ? C14 C15 H15 120.1 . . ? C17 C16 C15 120.3(4) . . ? C17 C16 H16 119.8 . . ? C15 C16 H16 119.8 . . ? C16 C17 C18 121.0(4) . . ? C16 C17 H17 119.5 . . ? C18 C17 H17 119.5 . . ? C17 C18 C13 118.4(3) . . ? C17 C18 H18 120.8 . . ? C13 C18 H18 120.8 . . ? C1 N1 C2 108.3(3) . . ? C1 N1 C10 124.8(3) . . ? C2 N1 C10 126.9(3) . . ? C1 N2 C3 108.3(3) . . ? C1 N2 C4 125.6(3) . . ? C3 N2 C4 125.9(3) . . ? C9 N3 H3B 113(5) . . ? C9 N3 H3A 109(2) . . ? H3B N3 H3A 117(5) . . ? N5 C19 N4 110.0(4) . . ? N5 C19 H19 125.0 . . ? N4 C19 H19 125.0 . . ? C21 C20 N4 108.1(3) . . ? C21 C20 H20 125.9 . . ? N4 C20 H20 125.9 . . ? C20 C21 N5 106.4(4) . . ? C20 C21 C31 130.9(3) . . ? N5 C21 C31 122.7(3) . . ? N5 C22 C27 109.6(4) . . ? N5 C22 C23 108.1(4) . . ? C27 C22 C23 130.2(6) . . ? N5 C22 H22 101.6 . . ? C27 C22 H22 101.6 . . ? C23 C22 H22 101.6 . . ? C22 C23 C24 94.1(6) . . ? C22 C23 H23A 112.9 . . ? C24 C23 H23A 112.9 . . ? C22 C23 H23B 112.9 . . ? C24 C23 H23B 112.9 . . ? H23A C23 H23B 110.3 . . ? C25 C24 C23 125.1(5) . . ? C25 C24 H24A 106.0 . . ? C23 C24 H24A 106.0 . . ? C25 C24 H24B 106.0 . . ? C23 C24 H24B 106.0 . . ? H24A C24 H24B 106.3 . . ? C24 C25 C26 109.8(5) . . ? C24 C25 H25A 109.7 . . ? C26 C25 H25A 109.7 . . ? C24 C25 H25B 109.7 . . ? C26 C25 H25B 109.7 . . ? H25A C25 H25B 108.2 . . ? C25 C26 C27 113.9(5) . . ? C25 C26 H26A 108.8 . . ? C27 C26 H26A 108.8 . . ? C25 C26 H26B 108.8 . . ? C27 C26 H26B 108.8 . . ? H26A C26 H26B 107.7 . . ? N6 C27 C22 114.5(4) . . ? N6 C27 C26 116.3(5) . . ? C22 C27 C26 110.1(5) . . ? N6 C27 H27 104.9 . . ? C22 C27 H27 104.9 . . ? C26 C27 H27 104.9 . . ? N4 C28 C29 110.8(3) . . ? N4 C28 C30 108.5(4) . . ? C29 C28 C30 111.9(4) . . ? N4 C28 H28 108.5 . . ? C29 C28 H28 108.5 . . ? C30 C28 H28 108.5 . . ? 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 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 . . ? C32 C31 C36 119.9(4) . . ? C32 C31 C21 120.6(4) . . ? C36 C31 C21 119.5(4) . . ? C31 C32 C33 120.0(4) . . ? C31 C32 H32 120.0 . . ? C33 C32 H32 120.0 . . ? C34 C33 C32 119.7(4) . . ? C34 C33 H33 120.1 . . ? C32 C33 H33 120.1 . . ? C35 C34 C33 120.1(4) . . ? C35 C34 H34 119.9 . . ? C33 C34 H34 119.9 . . ? C34 C35 C36 120.3(4) . . ? C34 C35 H35 119.9 . . ? C36 C35 H35 119.9 . . ? C35 C36 C31 119.9(4) . . ? C35 C36 H36 120.1 . . ? C31 C36 H36 120.1 . . ? C19 N4 C20 107.5(3) . . ? C19 N4 C28 125.2(3) . . ? C20 N4 C28 127.3(3) . . ? C19 N5 C21 107.9(3) . . ? C19 N5 C22 126.1(4) . . ? C21 N5 C22 125.8(4) . . ? C27 N6 H6C 87(5) . . ? C27 N6 H6D 103(5) . . ? H6C N6 H6D 116(7) . . ? C55 B1 C37 103.4(3) . . ? C55 B1 C43 108.2(2) . . ? C37 B1 C43 115.4(3) . . ? C55 B1 C49 113.0(3) . . ? C37 B1 C49 110.7(2) . . ? C43 B1 C49 106.3(3) . . ? C38 C37 C42 115.1(3) . . ? C38 C37 B1 125.5(3) . . ? C42 C37 B1 119.3(3) . . ? C39 C38 C37 122.3(3) . . ? C39 C38 H38 118.9 . . ? C37 C38 H38 118.9 . . ? C40 C39 C38 119.7(4) . . ? C40 C39 H39 120.2 . . ? C38 C39 H39 120.2 . . ? C41 C40 C39 119.6(3) . . ? C41 C40 H40 120.2 . . ? C39 C40 H40 120.2 . . ? C40 C41 C42 120.7(3) . . ? C40 C41 H41 119.7 . . ? C42 C41 H41 119.7 . . ? C41 C42 C37 122.6(3) . . ? C41 C42 H42 118.7 . . ? C37 C42 H42 118.7 . . ? C44 C43 C48 114.7(3) . . ? C44 C43 B1 122.7(3) . . ? C48 C43 B1 122.4(3) . . ? C45 C44 C43 124.3(4) . . ? C45 C44 H44 117.9 . . ? C43 C44 H44 117.9 . . ? C44 C45 C46 118.9(4) . . ? C44 C45 H45 120.5 . . ? C46 C45 H45 120.5 . . ? C47 C46 C45 119.4(4) . . ? C47 C46 H46 120.3 . . ? C45 C46 H46 120.3 . . ? C46 C47 C48 120.5(4) . . ? C46 C47 H47 119.8 . . ? C48 C47 H47 119.8 . . ? C47 C48 C43 122.1(4) . . ? C47 C48 H48 118.9 . . ? C43 C48 H48 118.9 . . ? C54 C49 C50 115.6(3) . . ? C54 C49 B1 120.6(3) . . ? C50 C49 B1 123.6(3) . . ? C49 C50 C51 122.1(3) . . ? C49 C50 H50 118.9 . . ? C51 C50 H50 118.9 . . ? C52 C51 C50 120.7(3) . . ? C52 C51 H51 119.7 . . ? C50 C51 H51 119.7 . . ? C51 C52 C53 118.6(3) . . ? C51 C52 H52 120.7 . . ? C53 C52 H52 120.7 . . ? C52 C53 C54 119.9(3) . . ? C52 C53 H53 120.1 . . ? C54 C53 H53 120.1 . . ? C49 C54 C53 123.0(3) . . ? C49 C54 H54 118.5 . . ? C53 C54 H54 118.5 . . ? C60 C55 C56 115.1(3) . . ? C60 C55 B1 119.3(3) . . ? C56 C55 B1 125.6(3) . . ? C57 C56 C55 121.5(4) . . ? C57 C56 H56 119.3 . . ? C55 C56 H56 119.3 . . ? C58 C57 C56 121.2(4) . . ? C58 C57 H57 119.4 . . ? C56 C57 H57 119.4 . . ? C57 C58 C59 119.1(4) . . ? C57 C58 H58 120.5 . . ? C59 C58 H58 120.5 . . ? C58 C59 C60 119.5(4) . . ? C58 C59 H59 120.3 . . ? C60 C59 H59 120.2 . . ? C59 C60 C55 123.6(4) . . ? C59 C60 H60 118.2 . . ? C55 C60 H60 118.2 . . ? C67 B2 C79 115.1(3) . . ? C67 B2 C73 110.3(2) . . ? C79 B2 C73 106.3(2) . . ? C67 B2 C61 103.4(3) . . ? C79 B2 C61 109.1(2) . . ? C73 B2 C61 112.7(3) . . ? C62 C61 C66 116.1(3) . . ? C62 C61 B2 125.2(3) . . ? C66 C61 B2 118.6(3) . . ? C61 C62 C63 123.0(3) . . ? C61 C62 H62 118.5 . . ? C63 C62 H62 118.5 . . ? C64 C63 C62 119.4(3) . . ? C64 C63 H63 120.3 . . ? C62 C63 H63 120.3 . . ? C65 C64 C63 119.0(3) . . ? C65 C64 H64 120.5 . . ? C63 C64 H64 120.5 . . ? C64 C65 C66 120.5(3) . . ? C64 C65 H65 119.8 . . ? C66 C65 H65 119.8 . . ? C65 C66 C61 122.0(3) . . ? C65 C66 H66 119.0 . . ? C61 C66 H66 119.0 . . ? C72 C67 C68 115.5(3) . . ? C72 C67 B2 126.2(3) . . ? C68 C67 B2 118.2(3) . . ? C69 C68 C67 123.0(3) . . ? C69 C68 H68 118.5 . . ? C67 C68 H68 118.5 . . ? C68 C69 C70 119.3(3) . . ? C68 C69 H69 120.3 . . ? C70 C69 H69 120.3 . . ? C71 C70 C69 119.1(3) . . ? C71 C70 H70 120.4 . . ? C69 C70 H70 120.4 . . ? C70 C71 C72 121.3(4) . . ? C70 C71 H71 119.4 . . ? C72 C71 H71 119.4 . . ? C67 C72 C71 121.7(3) . . ? C67 C72 H72 119.1 . . ? C71 C72 H72 119.1 . . ? C74 C73 C78 114.7(3) . . ? C74 C73 B2 124.9(3) . . ? C78 C73 B2 120.3(3) . . ? C75 C74 C73 123.4(3) . . ? C75 C74 H74 118.3 . . ? C73 C74 H74 118.3 . . ? C74 C75 C76 119.9(3) . . ? C74 C75 H75 120.0 . . ? C76 C75 H75 120.0 . . ? C77 C76 C75 118.5(3) . . ? C77 C76 H76 120.7 . . ? C75 C76 H76 120.7 . . ? C78 C77 C76 120.9(3) . . ? C78 C77 H77 119.6 . . ? C76 C77 H77 119.6 . . ? C77 C78 C73 122.5(3) . . ? C77 C78 H78 118.8 . . ? C73 C78 H78 118.8 . . ? C80 C79 C84 114.1(3) . . ? C80 C79 B2 123.4(3) . . ? C84 C79 B2 122.3(3) . . ? C81 C80 C79 123.5(4) . . ? C81 C80 H80 118.2 . . ? C79 C80 H80 118.2 . . ? C82 C81 C80 120.7(4) . . ? C82 C81 H81 119.7 . . ? C80 C81 H81 119.7 . . ? C83 C82 C81 117.8(4) . . ? C83 C82 H82 121.1 . . ? C81 C82 H82 121.1 . . ? C84 C83 C82 120.7(4) . . ? C84 C83 H83 119.7 . . ? C82 C83 H83 119.7 . . ? C83 C84 C79 123.1(4) . . ? C83 C84 H84 118.4 . . ? C79 C84 H84 118.4 . . ? C90 C85 C86 110.3(4) . . ? C90 C85 H85A 109.6 . . ? C86 C85 H85A 109.6 . . ? C90 C85 H85B 109.6 . . ? C86 C85 H85B 109.6 . . ? H85A C85 H85B 108.1 . . ? C85 C86 C87 109.1(4) . . ? C85 C86 H86A 109.9 . . ? C87 C86 H86A 109.9 . . ? C85 C86 H86B 109.9 . . ? C87 C86 H86B 109.9 . . ? H86A C86 H86B 108.3 . . ? C88 C87 C86 111.4(4) . . ? C88 C87 H87A 109.3 . . ? C86 C87 H87A 109.3 . . ? C88 C87 H87B 109.3 . . ? C86 C87 H87B 109.3 . . ? H87A C87 H87B 108.0 . . ? C87 C88 C89 109.6(3) . . ? C87 C88 H88A 109.7 . . ? C89 C88 H88A 109.7 . . ? C87 C88 H88B 109.7 . . ? C89 C88 H88B 109.7 . . ? H88A C88 H88B 108.2 . . ? C88 C89 C90 111.6(4) . . ? C88 C89 H89A 109.3 . . ? C90 C89 H89A 109.3 . . ? C88 C89 H89B 109.3 . . ? C90 C89 H89B 109.3 . . ? H89A C89 H89B 108.0 . . ? C85 C90 C89 110.6(4) . . ? C85 C90 H90A 109.5 . . ? C89 C90 H90A 109.5 . . ? C85 C90 H90B 109.5 . . ? C89 C90 H90B 109.5 . . ? H90A C90 H90B 108.1 . . ? C92A C91A C96A 107.5(4) . . ? C92A C91A H91A 110.2 . . ? C96A C91A H91A 110.2 . . ? C92A C91A H91B 110.2 . . ? C96A C91A H91B 110.2 . . ? H91A C91A H91B 108.5 . . ? C91A C92A C93A 111.1(4) . . ? C91A C92A H92A 109.4 . . ? C93A C92A H92A 109.4 . . ? C91A C92A H92B 109.4 . . ? C93A C92A H92B 109.4 . . ? H92A C92A H92B 108.0 . . ? C94A C93A C92A 107.1(4) . . ? C94A C93A H93A 110.3 . . ? C92A C93A H93A 110.3 . . ? C94A C93A H93B 110.3 . . ? C92A C93A H93B 110.3 . . ? H93A C93A H93B 108.6 . . ? C95A C94A C93A 109.6(3) . . ? C95A C94A H94A 109.8 . . ? C93A C94A H94A 109.8 . . ? C95A C94A H94B 109.8 . . ? C93A C94A H94B 109.8 . . ? H94A C94A H94B 108.2 . . ? C94A C95A C96A 108.3(4) . . ? C94A C95A H95A 110.0 . . ? C96A C95A H95A 110.0 . . ? C94A C95A H95B 110.0 . . ? C96A C95A H95B 110.0 . . ? H95A C95A H95B 108.4 . . ? C91A C96A C95A 108.8(5) . . ? C91A C96A H96A 109.9 . . ? C95A C96A H96A 109.9 . . ? C91A C96A H96B 109.9 . . ? C95A C96A H96B 109.9 . . ? H96A C96A H96B 108.3 . . ? C93B C92B H92C 110.5 . . ? C93B C92B H92D 110.5 . . ? H92C C92B H92D 108.7 . . ? C92B C93B H93C 110.7 . . ? C92B C93B H93D 110.7 . . ? H93C C93B H93D 108.8 . . ? C96B C95B H95C 110.7 . . ? C96B C95B H95D 110.7 . . ? H95C C95B H95D 108.8 . . ? C95B C96B H96C 109.5 . . ? C95B C96B H96D 109.5 . . ? H96C C96B H96D 108.0 . . ? C102 C97 C98 111.5(4) . . ? C102 C97 H97A 109.3 . . ? C98 C97 H97A 109.3 . . ? C102 C97 H97B 109.3 . . ? C98 C97 H97B 109.3 . . ? H97A C97 H97B 108.0 . . ? C99 C98 C97 111.1(4) . . ? C99 C98 H98A 109.4 . . ? C97 C98 H98A 109.4 . . ? C99 C98 H98B 109.4 . . ? C97 C98 H98B 109.4 . . ? H98A C98 H98B 108.0 . . ? C100 C99 C98 109.7(3) . . ? C100 C99 H99A 109.7 . . ? C98 C99 H99A 109.7 . . ? C100 C99 H99B 109.7 . . ? C98 C99 H99B 109.7 . . ? H99A C99 H99B 108.2 . . ? C99 C100 C101 111.2(4) . . ? C99 C100 H10A 109.4 . . ? C101 C100 H10A 109.4 . . ? C99 C100 H10B 109.4 . . ? C101 C100 H10B 109.4 . . ? H10A C100 H10B 108.0 . . ? C102 C101 C100 109.6(3) . . ? C102 C101 H10C 109.7 . . ? C100 C101 H10C 109.7 . . ? C102 C101 H10D 109.7 . . ? C100 C101 H10D 109.7 . . ? H10C C101 H10D 108.2 . . ? C97 C102 C101 110.7(4) . . ? C97 C102 H10E 109.5 . . ? C101 C102 H10E 109.5 . . ? C97 C102 H10F 109.5 . . ? C101 C102 H10F 109.5 . . ? H10E C102 H10F 108.1 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C2 C3 N2 0.2(4) . . . . ? N1 C2 C3 C13 -179.2(3) . . . . ? N2 C4 C5 C6 -179.6(3) . . . . ? C9 C4 C5 C6 -56.6(5) . . . . ? C4 C5 C6 C7 56.0(5) . . . . ? C5 C6 C7 C8 -56.3(5) . . . . ? C6 C7 C8 C9 56.5(6) . . . . ? N2 C4 C9 N3 -60.2(4) . . . . ? C5 C4 C9 N3 177.4(3) . . . . ? N2 C4 C9 C8 177.1(3) . . . . ? C5 C4 C9 C8 54.6(4) . . . . ? C7 C8 C9 N3 -179.1(4) . . . . ? C7 C8 C9 C4 -53.9(5) . . . . ? C2 C3 C13 C14 76.3(5) . . . . ? N2 C3 C13 C14 -103.0(4) . . . . ? C2 C3 C13 C18 -102.6(5) . . . . ? N2 C3 C13 C18 78.1(4) . . . . ? C18 C13 C14 C15 -3.4(5) . . . . ? C3 C13 C14 C15 177.8(3) . . . . ? C13 C14 C15 C16 1.6(6) . . . . ? C14 C15 C16 C17 0.6(6) . . . . ? C15 C16 C17 C18 -1.2(6) . . . . ? C16 C17 C18 C13 -0.5(6) . . . . ? C14 C13 C18 C17 2.8(6) . . . . ? C3 C13 C18 C17 -178.4(3) . . . . ? N2 C1 N1 C2 -0.5(4) . . . . ? N2 C1 N1 C10 178.2(3) . . . . ? C3 C2 N1 C1 0.2(4) . . . . ? C3 C2 N1 C10 -178.5(3) . . . . ? C12 C10 N1 C1 127.1(4) . . . . ? C11 C10 N1 C1 -108.7(4) . . . . ? C12 C10 N1 C2 -54.4(5) . . . . ? C11 C10 N1 C2 69.8(5) . . . . ? N1 C1 N2 C3 0.7(4) . . . . ? N1 C1 N2 C4 175.1(3) . . . . ? C2 C3 N2 C1 -0.5(4) . . . . ? C13 C3 N2 C1 178.9(3) . . . . ? C2 C3 N2 C4 -174.9(3) . . . . ? C13 C3 N2 C4 4.5(5) . . . . ? C9 C4 N2 C1 -59.3(4) . . . . ? C5 C4 N2 C1 65.7(4) . . . . ? C9 C4 N2 C3 114.1(4) . . . . ? C5 C4 N2 C3 -120.9(4) . . . . ? N4 C20 C21 N5 2.0(4) . . . . ? N4 C20 C21 C31 -179.5(4) . . . . ? N5 C22 C23 C24 -175.9(5) . . . . ? C27 C22 C23 C24 -38.4(8) . . . . ? C22 C23 C24 C25 44.5(9) . . . . ? C23 C24 C25 C26 -57.5(9) . . . . ? C24 C25 C26 C27 53.0(8) . . . . ? N5 C22 C27 N6 -44.8(6) . . . . ? C23 C22 C27 N6 178.2(5) . . . . ? N5 C22 C27 C26 -178.0(4) . . . . ? C23 C22 C27 C26 45.0(8) . . . . ? C25 C26 C27 N6 -178.1(5) . . . . ? C25 C26 C27 C22 -45.8(7) . . . . ? C20 C21 C31 C32 89.9(5) . . . . ? N5 C21 C31 C32 -91.9(5) . . . . ? C20 C21 C31 C36 -90.0(5) . . . . ? N5 C21 C31 C36 88.3(5) . . . . ? C36 C31 C32 C33 -0.9(6) . . . . ? C21 C31 C32 C33 179.2(4) . . . . ? C31 C32 C33 C34 0.3(7) . . . . ? C32 C33 C34 C35 0.5(7) . . . . ? C33 C34 C35 C36 -0.8(7) . . . . ? C34 C35 C36 C31 0.2(7) . . . . ? C32 C31 C36 C35 0.7(6) . . . . ? C21 C31 C36 C35 -179.5(4) . . . . ? N5 C19 N4 C20 1.7(5) . . . . ? N5 C19 N4 C28 -178.8(4) . . . . ? C21 C20 N4 C19 -2.3(4) . . . . ? C21 C20 N4 C28 178.2(4) . . . . ? C29 C28 N4 C19 -116.5(4) . . . . ? C30 C28 N4 C19 120.3(4) . . . . ? C29 C28 N4 C20 62.9(5) . . . . ? C30 C28 N4 C20 -60.3(5) . . . . ? N4 C19 N5 C21 -0.4(5) . . . . ? N4 C19 N5 C22 176.3(4) . . . . ? C20 C21 N5 C19 -1.0(4) . . . . ? C31 C21 N5 C19 -179.7(4) . . . . ? C20 C21 N5 C22 -177.7(4) . . . . ? C31 C21 N5 C22 3.6(6) . . . . ? C27 C22 N5 C19 -69.7(6) . . . . ? C23 C22 N5 C19 77.1(7) . . . . ? C27 C22 N5 C21 106.4(5) . . . . ? C23 C22 N5 C21 -106.8(6) . . . . ? C55 B1 C37 C38 112.8(3) . . . . ? C43 B1 C37 C38 -5.2(5) . . . . ? C49 B1 C37 C38 -125.9(3) . . . . ? C55 B1 C37 C42 -63.4(3) . . . . ? C43 B1 C37 C42 178.6(3) . . . . ? C49 B1 C37 C42 57.9(4) . . . . ? C42 C37 C38 C39 -1.8(5) . . . . ? B1 C37 C38 C39 -178.1(3) . . . . ? C37 C38 C39 C40 1.1(5) . . . . ? C38 C39 C40 C41 0.5(5) . . . . ? C39 C40 C41 C42 -1.2(5) . . . . ? C40 C41 C42 C37 0.4(5) . . . . ? C38 C37 C42 C41 1.0(5) . . . . ? B1 C37 C42 C41 177.6(3) . . . . ? C55 B1 C43 C44 20.4(4) . . . . ? C37 B1 C43 C44 135.6(3) . . . . ? C49 B1 C43 C44 -101.3(4) . . . . ? C55 B1 C43 C48 -164.3(3) . . . . ? C37 B1 C43 C48 -49.1(5) . . . . ? C49 B1 C43 C48 74.0(4) . . . . ? C48 C43 C44 C45 1.7(6) . . . . ? B1 C43 C44 C45 177.3(4) . . . . ? C43 C44 C45 C46 -0.3(7) . . . . ? C44 C45 C46 C47 -1.2(7) . . . . ? C45 C46 C47 C48 1.0(7) . . . . ? C46 C47 C48 C43 0.6(7) . . . . ? C44 C43 C48 C47 -1.9(6) . . . . ? B1 C43 C48 C47 -177.5(4) . . . . ? C55 B1 C49 C54 -61.3(4) . . . . ? C37 B1 C49 C54 -176.7(3) . . . . ? C43 B1 C49 C54 57.3(4) . . . . ? C55 B1 C49 C50 123.4(3) . . . . ? C37 B1 C49 C50 8.0(4) . . . . ? C43 B1 C49 C50 -118.0(3) . . . . ? C54 C49 C50 C51 3.1(5) . . . . ? B1 C49 C50 C51 178.6(3) . . . . ? C49 C50 C51 C52 -2.6(5) . . . . ? C50 C51 C52 C53 0.6(5) . . . . ? C51 C52 C53 C54 0.7(5) . . . . ? C50 C49 C54 C53 -1.8(5) . . . . ? B1 C49 C54 C53 -177.4(3) . . . . ? C52 C53 C54 C49 -0.1(5) . . . . ? C37 B1 C55 C60 -60.5(4) . . . . ? C43 B1 C55 C60 62.3(4) . . . . ? C49 B1 C55 C60 179.8(3) . . . . ? C37 B1 C55 C56 118.7(4) . . . . ? C43 B1 C55 C56 -118.5(4) . . . . ? C49 B1 C55 C56 -1.0(5) . . . . ? C60 C55 C56 C57 0.2(6) . . . . ? B1 C55 C56 C57 -179.0(4) . . . . ? C55 C56 C57 C58 -1.7(7) . . . . ? C56 C57 C58 C59 1.8(7) . . . . ? C57 C58 C59 C60 -0.5(6) . . . . ? C58 C59 C60 C55 -1.0(6) . . . . ? C56 C55 C60 C59 1.1(5) . . . . ? B1 C55 C60 C59 -179.6(3) . . . . ? C67 B2 C61 C62 -108.6(4) . . . . ? C79 B2 C61 C62 128.4(3) . . . . ? C73 B2 C61 C62 10.5(4) . . . . ? C67 B2 C61 C66 67.0(3) . . . . ? C79 B2 C61 C66 -56.0(4) . . . . ? C73 B2 C61 C66 -173.9(3) . . . . ? C66 C61 C62 C63 0.5(5) . . . . ? B2 C61 C62 C63 176.2(4) . . . . ? C61 C62 C63 C64 1.3(6) . . . . ? C62 C63 C64 C65 -1.7(6) . . . . ? C63 C64 C65 C66 0.3(6) . . . . ? C64 C65 C66 C61 1.6(6) . . . . ? C62 C61 C66 C65 -2.0(5) . . . . ? B2 C61 C66 C65 -177.9(3) . . . . ? C79 B2 C67 C72 6.2(4) . . . . ? C73 B2 C67 C72 126.5(3) . . . . ? C61 B2 C67 C72 -112.7(3) . . . . ? C79 B2 C67 C68 -176.9(3) . . . . ? C73 B2 C67 C68 -56.6(4) . . . . ? C61 B2 C67 C68 64.2(3) . . . . ? C72 C67 C68 C69 -1.6(5) . . . . ? B2 C67 C68 C69 -178.8(3) . . . . ? C67 C68 C69 C70 -0.4(5) . . . . ? C68 C69 C70 C71 1.5(5) . . . . ? C69 C70 C71 C72 -0.6(5) . . . . ? C68 C67 C72 C71 2.5(5) . . . . ? B2 C67 C72 C71 179.5(3) . . . . ? C70 C71 C72 C67 -1.5(5) . . . . ? C67 B2 C73 C74 -10.2(4) . . . . ? C79 B2 C73 C74 115.1(3) . . . . ? C61 B2 C73 C74 -125.3(3) . . . . ? C67 B2 C73 C78 172.9(3) . . . . ? C79 B2 C73 C78 -61.7(4) . . . . ? C61 B2 C73 C78 57.9(4) . . . . ? C78 C73 C74 C75 -1.2(5) . . . . ? B2 C73 C74 C75 -178.1(3) . . . . ? C73 C74 C75 C76 -0.5(5) . . . . ? C74 C75 C76 C77 1.7(5) . . . . ? C75 C76 C77 C78 -1.1(5) . . . . ? C76 C77 C78 C73 -0.6(6) . . . . ? C74 C73 C78 C77 1.7(5) . . . . ? B2 C73 C78 C77 178.9(3) . . . . ? C67 B2 C79 C80 47.6(4) . . . . ? C73 B2 C79 C80 -74.8(4) . . . . ? C61 B2 C79 C80 163.3(3) . . . . ? C67 B2 C79 C84 -137.9(3) . . . . ? C73 B2 C79 C84 99.6(3) . . . . ? C61 B2 C79 C84 -22.2(4) . . . . ? C84 C79 C80 C81 2.5(5) . . . . ? B2 C79 C80 C81 177.4(4) . . . . ? C79 C80 C81 C82 -2.4(7) . . . . ? C80 C81 C82 C83 0.7(6) . . . . ? C81 C82 C83 C84 0.5(6) . . . . ? C82 C83 C84 C79 -0.1(6) . . . . ? C80 C79 C84 C83 -1.3(5) . . . . ? B2 C79 C84 C83 -176.2(3) . . . . ? C90 C85 C86 C87 -57.9(5) . . . . ? C85 C86 C87 C88 59.3(4) . . . . ? C86 C87 C88 C89 -58.0(5) . . . . ? C87 C88 C89 C90 56.5(5) . . . . ? C86 C85 C90 C89 57.3(6) . . . . ? C88 C89 C90 C85 -56.4(6) . . . . ? C96A C91A C92A C93A 61.8(6) . . . . ? C91A C92A C93A C94A -61.4(6) . . . . ? C92A C93A C94A C95A 61.4(5) . . . . ? C93A C94A C95A C96A -62.8(6) . . . . ? C92A C91A C96A C95A -60.9(6) . . . . ? C94A C95A C96A C91A 62.5(6) . . . . ? C102 C97 C98 C99 56.4(6) . . . . ? C97 C98 C99 C100 -56.5(5) . . . . ? C98 C99 C100 C101 57.9(5) . . . . ? C99 C100 C101 C102 -58.1(5) . . . . ? C98 C97 C102 C101 -56.4(5) . . . . ? C100 C101 C102 C97 56.7(5) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 28.31 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.480 _refine_diff_density_min -0.714 _refine_diff_density_rms 0.087 #============= Material Relevant to Complex(6b)===================== data_comple6b _database_code_depnum_ccdc_archive 'CCDC 731704' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C41 H57 Cl Ir N3 O' _chemical_formula_sum 'C41 H57 Cl Ir N3 O' _chemical_formula_weight 835.55 _chemical_absolute_configuration ad 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' N N 0.0061 0.0033 '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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ir Ir -1.4442 7.9887 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 12.7958(7) _cell_length_b 16.4449(9) _cell_length_c 18.4264(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3877.4(4) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 8481 _cell_measurement_theta_min 2.30 _cell_measurement_theta_max 29.92 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.431 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1704 _exptl_absorpt_coefficient_mu 3.546 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.555 _exptl_absorpt_correction_T_max 0.730 _exptl_absorpt_process_details 'SADABS v2.03; (Sheldrick)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 58607 _diffrn_reflns_av_R_equivalents 0.0317 _diffrn_reflns_av_sigmaI/netI 0.0344 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.66 _diffrn_reflns_theta_max 30.05 _reflns_number_total 11251 _reflns_number_gt 10675 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0124P)^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 mixed _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 -0.009(3) _refine_ls_number_reflns 11251 _refine_ls_number_parameters 452 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0206 _refine_ls_R_factor_gt 0.0186 _refine_ls_wR_factor_ref 0.0377 _refine_ls_wR_factor_gt 0.0374 _refine_ls_goodness_of_fit_ref 0.973 _refine_ls_restrained_S_all 0.973 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.22374(15) 0.65679(12) 0.10185(12) 0.0154(4) Uani 1 1 d . . . C2 C 0.34295(16) 0.73709(13) 0.04772(11) 0.0188(4) Uani 1 1 d . . . H2 H 0.3822 0.7630 0.0106 0.023 Uiso 1 1 calc R . . C3 C 0.35359(15) 0.74899(12) 0.11913(12) 0.0173(4) Uani 1 1 d . . . C4 C 0.25441(16) 0.70485(13) 0.23141(11) 0.0170(4) Uani 1 1 d . . . H4 H 0.3115 0.7375 0.2543 0.020 Uiso 1 1 calc R . . C5 C 0.25248(18) 0.62318(13) 0.26954(12) 0.0217(5) Uani 1 1 d . . . H5A H 0.3211 0.5962 0.2636 0.026 Uiso 1 1 calc R . . H5B H 0.1987 0.5881 0.2470 0.026 Uiso 1 1 calc R . . C6 C 0.2286(2) 0.63312(15) 0.35019(12) 0.0282(5) Uani 1 1 d . . . H6A H 0.2250 0.5790 0.3735 0.034 Uiso 1 1 calc R . . H6B H 0.2854 0.6644 0.3737 0.034 Uiso 1 1 calc R . . C7 C 0.1253(2) 0.67726(16) 0.36045(13) 0.0351(6) Uani 1 1 d . . . H7A H 0.1119 0.6850 0.4129 0.042 Uiso 1 1 calc R . . H7B H 0.0679 0.6440 0.3401 0.042 Uiso 1 1 calc R . . C8 C 0.1277(2) 0.75964(15) 0.32272(12) 0.0326(6) Uani 1 1 d . . . H8A H 0.1809 0.7944 0.3463 0.039 Uiso 1 1 calc R . . H8B H 0.0589 0.7864 0.3286 0.039 Uiso 1 1 calc R . . C9 C 0.15278(17) 0.75263(13) 0.24195(12) 0.0196(4) Uani 1 1 d . . . H9 H 0.0943 0.7243 0.2164 0.024 Uiso 1 1 calc R . . C10 C 0.13038(16) 0.84806(13) 0.14778(11) 0.0206(5) Uani 1 1 d . . . H10 H 0.0943 0.8056 0.1234 0.025 Uiso 1 1 calc R . . C11 C 0.14170(15) 0.92608(13) 0.11107(12) 0.0197(4) Uani 1 1 d . . . C12 C 0.19118(17) 0.99247(13) 0.14507(11) 0.0211(4) Uani 1 1 d . . . C13 C 0.19991(15) 1.06738(13) 0.10826(12) 0.0215(4) Uani 1 1 d . . . C14 C 0.15839(16) 1.07080(15) 0.03870(11) 0.0227(4) Uani 1 1 d . . . H14 H 0.1644 1.1208 0.0131 0.027 Uiso 1 1 calc R . . C15 C 0.10838(19) 1.00627(12) 0.00335(11) 0.0217(4) Uani 1 1 d . . . C16 C 0.10085(17) 0.93455(12) 0.04098(10) 0.0207(4) Uani 1 1 d . . . H16 H 0.0670 0.8895 0.0189 0.025 Uiso 1 1 calc R . . C17 C 0.22395(17) 0.65875(13) -0.03468(11) 0.0198(4) Uani 1 1 d . . . H17 H 0.1686 0.6164 -0.0284 0.024 Uiso 1 1 calc R . . C18 C 0.30978(19) 0.62388(15) -0.08223(12) 0.0261(5) Uani 1 1 d . . . H18A H 0.3613 0.6663 -0.0929 0.039 Uiso 1 1 calc R . . H18B H 0.2794 0.6040 -0.1277 0.039 Uiso 1 1 calc R . . H18C H 0.3440 0.5788 -0.0568 0.039 Uiso 1 1 calc R . . C19 C 0.17400(19) 0.73413(14) -0.06830(12) 0.0266(5) Uani 1 1 d . . . H19A H 0.1175 0.7536 -0.0368 0.040 Uiso 1 1 calc R . . H19B H 0.1455 0.7204 -0.1161 0.040 Uiso 1 1 calc R . . H19C H 0.2268 0.7769 -0.0735 0.040 Uiso 1 1 calc R . . C20 C 0.42718(15) 0.80438(13) 0.15562(12) 0.0176(4) Uani 1 1 d . . . C21 C 0.48873(16) 0.78067(14) 0.21432(11) 0.0198(4) Uani 1 1 d . . . H21 H 0.4816 0.7276 0.2340 0.024 Uiso 1 1 calc R . . C22 C 0.56052(17) 0.83454(15) 0.24405(12) 0.0242(5) Uani 1 1 d . . . H22 H 0.6008 0.8186 0.2850 0.029 Uiso 1 1 calc R . . C23 C 0.57383(17) 0.91045(14) 0.21497(13) 0.0264(5) Uani 1 1 d . . . H23 H 0.6232 0.9469 0.2355 0.032 Uiso 1 1 calc R . . C24 C 0.51524(16) 0.93379(15) 0.15568(13) 0.0265(5) Uani 1 1 d . . . H24 H 0.5256 0.9860 0.1349 0.032 Uiso 1 1 calc R . . C25 C 0.44134(17) 0.88178(13) 0.12611(12) 0.0227(5) Uani 1 1 d . . . H25 H 0.4004 0.8988 0.0858 0.027 Uiso 1 1 calc R . . C26 C 0.25357(19) 1.14117(14) 0.14296(13) 0.0250(5) Uani 1 1 d . . . C27 C 0.36767(19) 1.12067(15) 0.16024(15) 0.0327(6) Uani 1 1 d . . . H27A H 0.3701 1.0764 0.1958 0.049 Uiso 1 1 calc R . . H27B H 0.4025 1.1688 0.1802 0.049 Uiso 1 1 calc R . . H27C H 0.4034 1.1037 0.1157 0.049 Uiso 1 1 calc R . . C28 C 0.1964(2) 1.16595(16) 0.21313(14) 0.0328(6) Uani 1 1 d . . . H28A H 0.1237 1.1798 0.2018 0.049 Uiso 1 1 calc R . . H28B H 0.2312 1.2133 0.2346 0.049 Uiso 1 1 calc R . . H28C H 0.1979 1.1206 0.2476 0.049 Uiso 1 1 calc R . . C29 C 0.2540(2) 1.21509(15) 0.09202(13) 0.0326(6) Uani 1 1 d . . . H29A H 0.2920 1.2015 0.0475 0.049 Uiso 1 1 calc R . . H29B H 0.2884 1.2610 0.1162 0.049 Uiso 1 1 calc R . . H29C H 0.1819 1.2300 0.0799 0.049 Uiso 1 1 calc R . . C30 C 0.0636(2) 1.02005(15) -0.07257(13) 0.0249(5) Uani 1 1 d . . . C31 C 0.0123(2) 0.94305(14) -0.10314(14) 0.0345(6) Uani 1 1 d . . . H31A H 0.0641 0.8993 -0.1056 0.052 Uiso 1 1 calc R . . H31B H -0.0147 0.9542 -0.1519 0.052 Uiso 1 1 calc R . . H31C H -0.0454 0.9265 -0.0714 0.052 Uiso 1 1 calc R . . C32 C 0.1499(2) 1.04709(18) -0.12466(13) 0.0407(7) Uani 1 1 d . . . H32A H 0.1805 1.0982 -0.1074 0.061 Uiso 1 1 calc R . . H32B H 0.1203 1.0553 -0.1732 0.061 Uiso 1 1 calc R . . H32C H 0.2043 1.0052 -0.1268 0.061 Uiso 1 1 calc R . . C33 C -0.0205(2) 1.08656(16) -0.06824(14) 0.0338(6) Uani 1 1 d . . . H33A H -0.0714 1.0724 -0.0306 0.051 Uiso 1 1 calc R . . H33B H -0.0561 1.0910 -0.1152 0.051 Uiso 1 1 calc R . . H33C H 0.0124 1.1387 -0.0562 0.051 Uiso 1 1 calc R . . C34 C 0.19804(19) 0.48256(14) 0.06608(13) 0.0225(5) Uani 1 1 d . . . H34 H 0.255(2) 0.5064(15) 0.0387(14) 0.027(7) Uiso 1 1 d . . . C35 C 0.20949(19) 0.47946(14) 0.14231(13) 0.0205(5) Uani 1 1 d . . . H35 H 0.2708(19) 0.5013(15) 0.1583(14) 0.022(6) Uiso 1 1 d . . . C36 C 0.16022(18) 0.41549(15) 0.19114(12) 0.0261(5) Uani 1 1 d . . . H36A H 0.2076 0.4043 0.2324 0.031 Uiso 1 1 calc R . . H36B H 0.1516 0.3644 0.1634 0.031 Uiso 1 1 calc R . . C37 C 0.05404(19) 0.44235(14) 0.22032(12) 0.0268(5) Uani 1 1 d . . . H37A H 0.0119 0.3936 0.2318 0.032 Uiso 1 1 calc R . . H37B H 0.0645 0.4731 0.2659 0.032 Uiso 1 1 calc R . . C38 C -0.00558(18) 0.49481(15) 0.16728(14) 0.0248(5) Uani 1 1 d . . . H38 H -0.0537(19) 0.5301(14) 0.1867(13) 0.018(6) Uiso 1 1 d . . . C39 C -0.01615(19) 0.48015(16) 0.09330(13) 0.0253(6) Uani 1 1 d . . . H39 H -0.0694(18) 0.5098(14) 0.0703(13) 0.017(6) Uiso 1 1 d . . . C40 C 0.0262(2) 0.40681(15) 0.05396(13) 0.0322(6) Uani 1 1 d . . . H40A H -0.0229 0.3911 0.0148 0.039 Uiso 1 1 calc R . . H40B H 0.0314 0.3607 0.0883 0.039 Uiso 1 1 calc R . . C41 C 0.13446(18) 0.42370(17) 0.02095(12) 0.0283(5) Uani 1 1 d . . . H41A H 0.1732 0.3718 0.0166 0.034 Uiso 1 1 calc R . . H41B H 0.1255 0.4463 -0.0285 0.034 Uiso 1 1 calc R . . Cl5 Cl -0.02594(4) 0.67444(3) 0.10409(4) 0.02696(12) Uani 1 1 d . . . H1 H 0.216(2) 0.937(2) 0.2253(15) 0.048(9) Uiso 1 1 d . . . Ir1 Ir 0.104766(6) 0.573244(5) 0.111696(4) 0.01652(2) Uani 1 1 d . . . N1 N 0.26500(13) 0.68069(11) 0.03771(9) 0.0170(4) Uani 1 1 d . . . N2 N 0.27963(13) 0.69809(10) 0.15338(9) 0.0162(4) Uani 1 1 d . . . N3 N 0.16678(15) 0.83415(11) 0.21129(10) 0.0207(4) Uani 1 1 d . . . O1 O 0.22972(14) 0.98479(11) 0.21296(9) 0.0263(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0161(9) 0.0166(10) 0.0134(11) 0.0008(8) 0.0002(8) 0.0042(7) C2 0.0172(10) 0.0208(11) 0.0184(10) 0.0017(8) -0.0002(8) -0.0027(8) C3 0.0143(8) 0.0172(9) 0.0205(11) 0.0020(9) 0.0010(8) 0.0005(7) C4 0.0191(10) 0.0196(11) 0.0124(9) 0.0025(8) -0.0009(8) 0.0014(8) C5 0.0234(11) 0.0223(11) 0.0194(11) 0.0046(9) -0.0018(9) 0.0034(9) C6 0.0390(14) 0.0273(12) 0.0182(11) 0.0088(9) -0.0032(10) 0.0011(11) C7 0.0475(17) 0.0375(14) 0.0202(11) 0.0106(10) 0.0125(11) 0.0074(12) C8 0.0476(17) 0.0310(13) 0.0193(11) 0.0057(10) 0.0141(11) 0.0141(11) C9 0.0221(11) 0.0207(11) 0.0161(10) 0.0032(8) 0.0039(8) 0.0060(8) C10 0.0239(12) 0.0200(11) 0.0179(10) 0.0027(8) 0.0032(8) 0.0052(8) C11 0.0218(8) 0.0195(9) 0.0178(9) 0.0043(12) 0.0016(8) 0.0038(8) C12 0.0206(11) 0.0227(11) 0.0200(11) 0.0008(9) -0.0005(9) 0.0051(9) C13 0.0235(9) 0.0186(9) 0.0222(9) 0.0011(11) -0.0009(9) 0.0021(8) C14 0.0265(11) 0.0190(10) 0.0225(10) 0.0055(10) -0.0017(8) 0.0010(10) C15 0.0237(10) 0.0219(10) 0.0194(10) 0.0031(8) -0.0035(10) 0.0006(10) C16 0.0234(9) 0.0186(10) 0.0203(9) 0.0004(8) -0.0023(9) -0.0003(11) C17 0.0208(11) 0.0245(12) 0.0140(10) 0.0002(9) -0.0009(8) -0.0047(9) C18 0.0280(12) 0.0307(13) 0.0196(11) -0.0043(9) 0.0036(9) -0.0037(10) C19 0.0285(12) 0.0288(13) 0.0226(11) 0.0003(10) -0.0081(10) -0.0020(10) C20 0.0145(9) 0.0194(10) 0.0188(10) -0.0021(8) 0.0019(8) -0.0002(7) C21 0.0193(10) 0.0225(11) 0.0177(10) -0.0017(9) 0.0006(8) 0.0025(9) C22 0.0202(10) 0.0325(13) 0.0200(11) -0.0085(10) -0.0022(9) 0.0033(9) C23 0.0213(10) 0.0266(13) 0.0314(12) -0.0148(10) 0.0014(9) -0.0024(9) C24 0.0236(10) 0.0196(11) 0.0363(13) -0.0017(11) 0.0055(9) -0.0012(10) C25 0.0196(10) 0.0231(11) 0.0253(13) 0.0010(9) -0.0002(9) 0.0018(9) C26 0.0297(13) 0.0197(12) 0.0255(12) -0.0020(9) -0.0051(10) -0.0004(10) C27 0.0338(14) 0.0274(13) 0.0368(14) -0.0030(11) -0.0096(11) -0.0023(10) C28 0.0374(15) 0.0288(13) 0.0322(14) -0.0082(11) -0.0010(12) 0.0005(11) C29 0.0404(14) 0.0218(12) 0.0355(15) -0.0003(10) -0.0089(11) -0.0034(11) C30 0.0316(12) 0.0252(12) 0.0179(11) 0.0050(9) -0.0053(9) -0.0037(10) C31 0.0452(14) 0.0312(14) 0.0272(13) 0.0024(11) -0.0115(12) -0.0043(11) C32 0.0396(14) 0.0587(18) 0.0237(14) 0.0072(12) -0.0004(11) -0.0080(12) C33 0.0381(14) 0.0334(15) 0.0297(13) 0.0057(11) -0.0123(11) 0.0018(11) C34 0.0268(13) 0.0187(11) 0.0220(12) 0.0028(9) 0.0070(10) 0.0004(10) C35 0.0192(11) 0.0173(11) 0.0249(12) 0.0016(9) 0.0016(9) -0.0012(9) C36 0.0342(13) 0.0204(13) 0.0238(11) 0.0035(10) 0.0004(9) -0.0014(10) C37 0.0329(12) 0.0268(14) 0.0205(11) 0.0023(9) 0.0048(9) -0.0093(10) C38 0.0207(11) 0.0280(13) 0.0257(12) -0.0011(10) 0.0061(10) -0.0070(10) C39 0.0211(11) 0.0311(13) 0.0237(14) 0.0022(10) -0.0019(9) -0.0104(10) C40 0.0430(15) 0.0310(14) 0.0227(12) -0.0025(10) -0.0007(11) -0.0139(11) C41 0.0427(14) 0.0230(11) 0.0192(10) -0.0007(11) 0.0055(9) -0.0023(12) Cl5 0.0191(2) 0.0308(3) 0.0310(3) 0.0044(3) -0.0032(3) 0.0059(2) Ir1 0.01443(3) 0.01891(3) 0.01622(3) 0.00150(3) 0.00145(3) -0.00134(3) N1 0.0160(9) 0.0208(9) 0.0141(9) 0.0013(7) -0.0009(7) -0.0019(7) N2 0.0161(8) 0.0175(9) 0.0151(9) 0.0019(7) 0.0004(7) 0.0007(7) N3 0.0256(10) 0.0184(9) 0.0182(9) 0.0026(7) 0.0044(7) 0.0075(8) O1 0.0372(10) 0.0218(9) 0.0198(8) 0.0023(7) -0.0078(7) 0.0036(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.353(3) . ? C1 N2 1.369(3) . ? C1 Ir1 2.059(2) . ? C2 C3 1.337(3) . ? C2 N1 1.374(3) . ? C2 H2 0.9500 . ? C3 N2 1.412(3) . ? C3 C20 1.473(3) . ? C4 N2 1.478(3) . ? C4 C5 1.516(3) . ? C4 C9 1.532(3) . ? C4 H4 1.0000 . ? C5 C6 1.526(3) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C7 1.519(3) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.523(3) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.527(3) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 N3 1.466(3) . ? C9 H9 1.0000 . ? C10 N3 1.280(3) . ? C10 C11 1.458(3) . ? C10 H10 0.9500 . ? C11 C16 1.400(3) . ? C11 C12 1.409(3) . ? C12 O1 1.351(3) . ? C12 C13 1.411(3) . ? C13 C14 1.389(3) . ? C13 C26 1.534(3) . ? C14 C15 1.400(3) . ? C14 H14 0.9500 . ? C15 C16 1.372(3) . ? C15 C30 1.528(3) . ? C16 H16 0.9500 . ? C17 N1 1.478(3) . ? C17 C18 1.518(3) . ? C17 C19 1.526(3) . ? C17 H17 1.0000 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 C21 1.394(3) . ? C20 C25 1.396(3) . ? C21 C22 1.389(3) . ? C21 H21 0.9500 . ? C22 C23 1.369(3) . ? C22 H22 0.9500 . ? C23 C24 1.379(3) . ? C23 H23 0.9500 . ? C24 C25 1.387(3) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? C26 C27 1.532(3) . ? C26 C29 1.536(3) . ? C26 C28 1.541(3) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 C32 1.529(3) . ? C30 C31 1.534(3) . ? C30 C33 1.536(4) . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 C35 1.413(3) . ? C34 C41 1.513(3) . ? C34 Ir1 2.087(2) . ? C34 H34 0.97(3) . ? C35 C36 1.521(3) . ? C35 Ir1 2.120(2) . ? C35 H35 0.91(2) . ? C36 C37 1.526(3) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 C38 1.510(3) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 C39 1.391(4) . ? C38 Ir1 2.169(2) . ? C38 H38 0.92(2) . ? C39 C40 1.508(4) . ? C39 Ir1 2.203(2) . ? C39 H39 0.94(2) . ? C40 C41 1.538(3) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? Cl5 Ir1 2.3635(5) . ? O1 H1 0.84(3) . ? 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 N1 C1 N2 104.95(17) . . ? N1 C1 Ir1 124.02(15) . . ? N2 C1 Ir1 131.02(16) . . ? C3 C2 N1 107.74(18) . . ? C3 C2 H2 126.1 . . ? N1 C2 H2 126.1 . . ? C2 C3 N2 106.54(18) . . ? C2 C3 C20 127.23(19) . . ? N2 C3 C20 126.2(2) . . ? N2 C4 C5 112.82(17) . . ? N2 C4 C9 110.33(16) . . ? C5 C4 C9 112.45(17) . . ? N2 C4 H4 107.0 . . ? C5 C4 H4 107.0 . . ? C9 C4 H4 107.0 . . ? C4 C5 C6 111.08(18) . . ? C4 C5 H5A 109.4 . . ? C6 C5 H5A 109.4 . . ? C4 C5 H5B 109.4 . . ? C6 C5 H5B 109.4 . . ? H5A C5 H5B 108.0 . . ? C7 C6 C5 110.27(19) . . ? C7 C6 H6A 109.6 . . ? C5 C6 H6A 109.6 . . ? C7 C6 H6B 109.6 . . ? C5 C6 H6B 109.6 . . ? H6A C6 H6B 108.1 . . ? C6 C7 C8 110.5(2) . . ? C6 C7 H7A 109.5 . . ? C8 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? C8 C7 H7B 109.5 . . ? H7A C7 H7B 108.1 . . ? C7 C8 C9 112.45(19) . . ? C7 C8 H8A 109.1 . . ? C9 C8 H8A 109.1 . . ? C7 C8 H8B 109.1 . . ? C9 C8 H8B 109.1 . . ? H8A C8 H8B 107.8 . . ? N3 C9 C8 109.41(18) . . ? N3 C9 C4 108.45(17) . . ? C8 C9 C4 109.92(18) . . ? N3 C9 H9 109.7 . . ? C8 C9 H9 109.7 . . ? C4 C9 H9 109.7 . . ? N3 C10 C11 123.0(2) . . ? N3 C10 H10 118.5 . . ? C11 C10 H10 118.5 . . ? C16 C11 C12 120.1(2) . . ? C16 C11 C10 118.6(2) . . ? C12 C11 C10 121.36(19) . . ? O1 C12 C11 120.2(2) . . ? O1 C12 C13 119.9(2) . . ? C11 C12 C13 119.9(2) . . ? C14 C13 C12 116.7(2) . . ? C14 C13 C26 121.6(2) . . ? C12 C13 C26 121.73(19) . . ? C13 C14 C15 125.0(2) . . ? C13 C14 H14 117.5 . . ? C15 C14 H14 117.5 . . ? C16 C15 C14 116.66(19) . . ? C16 C15 C30 124.3(2) . . ? C14 C15 C30 119.00(19) . . ? C15 C16 C11 121.7(2) . . ? C15 C16 H16 119.1 . . ? C11 C16 H16 119.1 . . ? N1 C17 C18 110.86(17) . . ? N1 C17 C19 108.48(17) . . ? C18 C17 C19 112.07(19) . . ? N1 C17 H17 108.5 . . ? C18 C17 H17 108.5 . . ? C19 C17 H17 108.5 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C21 C20 C25 119.0(2) . . ? C21 C20 C3 122.86(19) . . ? C25 C20 C3 117.98(19) . . ? C22 C21 C20 120.1(2) . . ? C22 C21 H21 119.9 . . ? C20 C21 H21 119.9 . . ? C23 C22 C21 120.6(2) . . ? C23 C22 H22 119.7 . . ? C21 C22 H22 119.7 . . ? C22 C23 C24 119.7(2) . . ? C22 C23 H23 120.1 . . ? C24 C23 H23 120.1 . . ? C23 C24 C25 120.7(2) . . ? C23 C24 H24 119.7 . . ? C25 C24 H24 119.7 . . ? C24 C25 C20 119.9(2) . . ? C24 C25 H25 120.1 . . ? C20 C25 H25 120.1 . . ? C27 C26 C13 109.82(19) . . ? C27 C26 C29 107.3(2) . . ? C13 C26 C29 111.90(19) . . ? C27 C26 C28 109.7(2) . . ? C13 C26 C28 110.3(2) . . ? C29 C26 C28 107.8(2) . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C26 C28 H28A 109.5 . . ? C26 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C26 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C26 C29 H29A 109.5 . . ? C26 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C26 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C15 C30 C32 110.3(2) . . ? C15 C30 C31 111.98(19) . . ? C32 C30 C31 108.6(2) . . ? C15 C30 C33 108.7(2) . . ? C32 C30 C33 109.3(2) . . ? C31 C30 C33 107.9(2) . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C30 C32 H32A 109.5 . . ? C30 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C30 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C30 C33 H33A 109.5 . . ? C30 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C30 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C35 C34 C41 125.4(2) . . ? C35 C34 Ir1 71.62(15) . . ? C41 C34 Ir1 111.77(17) . . ? C35 C34 H34 117.0(15) . . ? C41 C34 H34 112.2(15) . . ? Ir1 C34 H34 110.5(15) . . ? C34 C35 C36 124.7(2) . . ? C34 C35 Ir1 69.12(15) . . ? C36 C35 Ir1 113.49(15) . . ? C34 C35 H35 113.3(16) . . ? C36 C35 H35 116.0(16) . . ? Ir1 C35 H35 110.1(15) . . ? C35 C36 C37 112.2(2) . . ? C35 C36 H36A 109.2 . . ? C37 C36 H36A 109.2 . . ? C35 C36 H36B 109.2 . . ? C37 C36 H36B 109.2 . . ? H36A C36 H36B 107.9 . . ? C38 C37 C36 112.76(19) . . ? C38 C37 H37A 109.0 . . ? C36 C37 H37A 109.0 . . ? C38 C37 H37B 109.0 . . ? C36 C37 H37B 109.0 . . ? H37A C37 H37B 107.8 . . ? C39 C38 C37 125.8(2) . . ? C39 C38 Ir1 72.76(14) . . ? C37 C38 Ir1 108.44(15) . . ? C39 C38 H38 115.2(15) . . ? C37 C38 H38 116.6(15) . . ? Ir1 C38 H38 104.1(15) . . ? C38 C39 C40 125.1(2) . . ? C38 C39 Ir1 70.15(13) . . ? C40 C39 Ir1 112.17(16) . . ? C38 C39 H39 115.0(14) . . ? C40 C39 H39 117.4(14) . . ? Ir1 C39 H39 102.6(14) . . ? C39 C40 C41 111.7(2) . . ? C39 C40 H40A 109.3 . . ? C41 C40 H40A 109.3 . . ? C39 C40 H40B 109.3 . . ? C41 C40 H40B 109.3 . . ? H40A C40 H40B 107.9 . . ? C34 C41 C40 112.48(19) . . ? C34 C41 H41A 109.1 . . ? C40 C41 H41A 109.1 . . ? C34 C41 H41B 109.1 . . ? C40 C41 H41B 109.1 . . ? H41A C41 H41B 107.8 . . ? C1 Ir1 C34 91.06(8) . . ? C1 Ir1 C35 92.38(9) . . ? C34 Ir1 C35 39.25(9) . . ? C1 Ir1 C38 156.88(9) . . ? C34 Ir1 C38 97.90(10) . . ? C35 Ir1 C38 81.56(9) . . ? C1 Ir1 C39 165.85(9) . . ? C34 Ir1 C39 80.97(10) . . ? C35 Ir1 C39 88.82(10) . . ? C38 Ir1 C39 37.09(9) . . ? C1 Ir1 Cl5 92.76(5) . . ? C34 Ir1 Cl5 152.13(7) . . ? C35 Ir1 Cl5 167.28(6) . . ? C38 Ir1 Cl5 89.20(7) . . ? C39 Ir1 Cl5 89.04(7) . . ? C1 N1 C2 111.22(17) . . ? C1 N1 C17 125.37(17) . . ? C2 N1 C17 122.93(17) . . ? C1 N2 C3 109.53(18) . . ? C1 N2 C4 126.73(18) . . ? C3 N2 C4 122.45(18) . . ? C10 N3 C9 118.1(2) . . ? C12 O1 H1 105(2) . . ? 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 N1 C2 C3 N2 0.0(2) . . . . ? N1 C2 C3 C20 -179.69(19) . . . . ? N2 C4 C5 C6 178.73(18) . . . . ? C9 C4 C5 C6 -55.7(2) . . . . ? C4 C5 C6 C7 57.1(3) . . . . ? C5 C6 C7 C8 -57.3(3) . . . . ? C6 C7 C8 C9 56.8(3) . . . . ? C7 C8 C9 N3 -172.9(2) . . . . ? C7 C8 C9 C4 -53.9(3) . . . . ? N2 C4 C9 N3 -60.1(2) . . . . ? C5 C4 C9 N3 172.95(18) . . . . ? N2 C4 C9 C8 -179.71(19) . . . . ? C5 C4 C9 C8 53.4(2) . . . . ? N3 C10 C11 C16 178.7(2) . . . . ? N3 C10 C11 C12 -2.2(3) . . . . ? C16 C11 C12 O1 179.31(19) . . . . ? C10 C11 C12 O1 0.2(3) . . . . ? C16 C11 C12 C13 -0.3(3) . . . . ? C10 C11 C12 C13 -179.38(19) . . . . ? O1 C12 C13 C14 -179.91(19) . . . . ? C11 C12 C13 C14 -0.3(3) . . . . ? O1 C12 C13 C26 0.7(3) . . . . ? C11 C12 C13 C26 -179.70(19) . . . . ? C12 C13 C14 C15 0.6(3) . . . . ? C26 C13 C14 C15 180.0(2) . . . . ? C13 C14 C15 C16 -0.3(3) . . . . ? C13 C14 C15 C30 178.2(2) . . . . ? C14 C15 C16 C11 -0.4(3) . . . . ? C30 C15 C16 C11 -178.7(2) . . . . ? C12 C11 C16 C15 0.7(3) . . . . ? C10 C11 C16 C15 179.8(2) . . . . ? C2 C3 C20 C21 -132.5(2) . . . . ? N2 C3 C20 C21 47.8(3) . . . . ? C2 C3 C20 C25 42.3(3) . . . . ? N2 C3 C20 C25 -137.4(2) . . . . ? C25 C20 C21 C22 2.0(3) . . . . ? C3 C20 C21 C22 176.7(2) . . . . ? C20 C21 C22 C23 -1.8(3) . . . . ? C21 C22 C23 C24 0.2(3) . . . . ? C22 C23 C24 C25 1.4(3) . . . . ? C23 C24 C25 C20 -1.2(3) . . . . ? C21 C20 C25 C24 -0.5(3) . . . . ? C3 C20 C25 C24 -175.47(19) . . . . ? C14 C13 C26 C27 -118.9(2) . . . . ? C12 C13 C26 C27 60.4(3) . . . . ? C14 C13 C26 C29 0.1(3) . . . . ? C12 C13 C26 C29 179.5(2) . . . . ? C14 C13 C26 C28 120.1(2) . . . . ? C12 C13 C26 C28 -60.5(3) . . . . ? C16 C15 C30 C32 -123.0(3) . . . . ? C14 C15 C30 C32 58.7(3) . . . . ? C16 C15 C30 C31 -2.0(3) . . . . ? C14 C15 C30 C31 179.7(2) . . . . ? C16 C15 C30 C33 117.1(3) . . . . ? C14 C15 C30 C33 -61.2(3) . . . . ? C41 C34 C35 C36 0.7(4) . . . . ? Ir1 C34 C35 C36 104.8(2) . . . . ? C41 C34 C35 Ir1 -104.1(2) . . . . ? C34 C35 C36 C37 -92.4(3) . . . . ? Ir1 C35 C36 C37 -12.3(2) . . . . ? C35 C36 C37 C38 33.2(3) . . . . ? C36 C37 C38 C39 44.4(3) . . . . ? C36 C37 C38 Ir1 -37.3(2) . . . . ? C37 C38 C39 C40 3.0(4) . . . . ? Ir1 C38 C39 C40 103.7(2) . . . . ? C37 C38 C39 Ir1 -100.6(2) . . . . ? C38 C39 C40 C41 -94.3(3) . . . . ? Ir1 C39 C40 C41 -13.6(3) . . . . ? C35 C34 C41 C40 45.6(3) . . . . ? Ir1 C34 C41 C40 -36.8(3) . . . . ? C39 C40 C41 C34 32.6(3) . . . . ? N1 C1 Ir1 C34 62.88(18) . . . . ? N2 C1 Ir1 C34 -115.35(19) . . . . ? N1 C1 Ir1 C35 102.13(18) . . . . ? N2 C1 Ir1 C35 -76.10(19) . . . . ? N1 C1 Ir1 C38 176.05(19) . . . . ? N2 C1 Ir1 C38 -2.2(3) . . . . ? N1 C1 Ir1 C39 7.5(4) . . . . ? N2 C1 Ir1 C39 -170.7(3) . . . . ? N1 C1 Ir1 Cl5 -89.51(16) . . . . ? N2 C1 Ir1 Cl5 92.27(18) . . . . ? C35 C34 Ir1 C1 92.47(15) . . . . ? C41 C34 Ir1 C1 -145.93(16) . . . . ? C41 C34 Ir1 C35 121.6(2) . . . . ? C35 C34 Ir1 C38 -66.16(16) . . . . ? C41 C34 Ir1 C38 55.44(17) . . . . ? C35 C34 Ir1 C39 -99.28(16) . . . . ? C41 C34 Ir1 C39 22.32(16) . . . . ? C35 C34 Ir1 Cl5 -169.60(11) . . . . ? C41 C34 Ir1 Cl5 -48.0(2) . . . . ? C34 C35 Ir1 C1 -88.76(15) . . . . ? C36 C35 Ir1 C1 151.29(17) . . . . ? C36 C35 Ir1 C34 -120.0(3) . . . . ? C34 C35 Ir1 C38 113.66(16) . . . . ? C36 C35 Ir1 C38 -6.29(18) . . . . ? C34 C35 Ir1 C39 77.13(16) . . . . ? C36 C35 Ir1 C39 -42.82(18) . . . . ? C34 C35 Ir1 Cl5 157.5(2) . . . . ? C36 C35 Ir1 Cl5 37.5(4) . . . . ? C39 C38 Ir1 C1 -175.37(19) . . . . ? C37 C38 Ir1 C1 -52.6(3) . . . . ? C39 C38 Ir1 C34 -63.49(17) . . . . ? C37 C38 Ir1 C34 59.29(17) . . . . ? C39 C38 Ir1 C35 -99.31(17) . . . . ? C37 C38 Ir1 C35 23.48(17) . . . . ? C37 C38 Ir1 C39 122.8(2) . . . . ? C39 C38 Ir1 Cl5 89.46(15) . . . . ? C37 C38 Ir1 Cl5 -147.76(16) . . . . ? C38 C39 Ir1 C1 172.6(3) . . . . ? C40 C39 Ir1 C1 51.7(4) . . . . ? C38 C39 Ir1 C34 116.17(17) . . . . ? C40 C39 Ir1 C34 -4.68(17) . . . . ? C38 C39 Ir1 C35 77.52(16) . . . . ? C40 C39 Ir1 C35 -43.33(18) . . . . ? C40 C39 Ir1 C38 -120.9(3) . . . . ? C38 C39 Ir1 Cl5 -89.95(15) . . . . ? C40 C39 Ir1 Cl5 149.20(17) . . . . ? N2 C1 N1 C2 -1.5(2) . . . . ? Ir1 C1 N1 C2 179.84(14) . . . . ? N2 C1 N1 C17 -173.73(18) . . . . ? Ir1 C1 N1 C17 7.7(3) . . . . ? C3 C2 N1 C1 1.0(2) . . . . ? C3 C2 N1 C17 173.40(18) . . . . ? C18 C17 N1 C1 -128.2(2) . . . . ? C19 C17 N1 C1 108.4(2) . . . . ? C18 C17 N1 C2 60.5(3) . . . . ? C19 C17 N1 C2 -63.0(3) . . . . ? N1 C1 N2 C3 1.5(2) . . . . ? Ir1 C1 N2 C3 180.00(14) . . . . ? N1 C1 N2 C4 168.63(18) . . . . ? Ir1 C1 N2 C4 -12.9(3) . . . . ? C2 C3 N2 C1 -1.0(2) . . . . ? C20 C3 N2 C1 178.73(18) . . . . ? C2 C3 N2 C4 -168.74(18) . . . . ? C20 C3 N2 C4 11.0(3) . . . . ? C5 C4 N2 C1 61.0(3) . . . . ? C9 C4 N2 C1 -65.7(3) . . . . ? C5 C4 N2 C3 -133.46(19) . . . . ? C9 C4 N2 C3 99.8(2) . . . . ? C11 C10 N3 C9 -178.53(18) . . . . ? C8 C9 N3 C10 -140.8(2) . . . . ? C4 C9 N3 C10 99.3(2) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1 H1 N3 0.84(3) 1.82(3) 2.605(3) 155(3) . _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 30.05 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.163 _refine_diff_density_min -0.299 _refine_diff_density_rms 0.072 #============= Material Relevant to Compound(9)===================== data_compound9 _database_code_depnum_ccdc_archive 'CCDC 731705' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C31 H34 N3, I' _chemical_formula_sum 'C31 H34 I N3' _chemical_formula_weight 575.51 _chemical_absolute_configuration ad 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 9.3749(6) _cell_length_b 11.8875(8) _cell_length_c 51.257(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5712.3(7) _cell_formula_units_Z 8 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 6306 _cell_measurement_theta_min 2.31 _cell_measurement_theta_max 24.94 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.338 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2352 _exptl_absorpt_coefficient_mu 1.144 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.722 _exptl_absorpt_correction_T_max 0.930 _exptl_absorpt_process_details 'SADABS v2.03; (Sheldrick)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 44449 _diffrn_reflns_av_R_equivalents 0.0440 _diffrn_reflns_av_sigmaI/netI 0.0377 _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 -60 _diffrn_reflns_limit_l_max 60 _diffrn_reflns_theta_min 0.79 _diffrn_reflns_theta_max 25.04 _reflns_number_total 10051 _reflns_number_gt 9414 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. There are 2 small voids in the unit cell each with a volume of 31 A^3. Use of SQUEEZE estimates the 1 electron per void. As thee volume is small and the electron density low, the model was deemed acceptable. ; _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^)+(0.0246P)^2^+10.7369P] 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(18) _refine_ls_number_reflns 10051 _refine_ls_number_parameters 635 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0491 _refine_ls_R_factor_gt 0.0444 _refine_ls_wR_factor_ref 0.0896 _refine_ls_wR_factor_gt 0.0884 _refine_ls_goodness_of_fit_ref 1.244 _refine_ls_restrained_S_all 1.244 _refine_ls_shift/su_max 0.002 _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 C1A C 0.5376(5) 0.9334(4) 0.77787(10) 0.0170(10) Uani 1 1 d . . . H1A H 0.5037 0.9125 0.7611 0.020 Uiso 1 1 calc R . . C2A C 0.5458(5) 0.9755(4) 0.81977(9) 0.0163(10) Uani 1 1 d . . . C3A C 0.6807(5) 0.9862(4) 0.81013(9) 0.0147(11) Uani 1 1 d . . . C4A C 0.7908(5) 0.9497(4) 0.76464(10) 0.0187(12) Uani 1 1 d . . . H4A H 0.8777 0.9837 0.7728 0.022 Uiso 1 1 calc R . . C5A C 0.7579(6) 1.0163(5) 0.74037(11) 0.0225(12) Uani 1 1 d . . . H5A H 0.7406 1.0959 0.7451 0.027 Uiso 1 1 calc R . . H5B H 0.6702 0.9864 0.7321 0.027 Uiso 1 1 calc R . . C6A C 0.8808(6) 1.0095(5) 0.72110(11) 0.0282(12) Uani 1 1 d . . . H6A H 0.9658 1.0466 0.7286 0.034 Uiso 1 1 calc R . . H6B H 0.8547 1.0498 0.7049 0.034 Uiso 1 1 calc R . . C7A C 0.9163(5) 0.8873(5) 0.71468(10) 0.0252(13) Uani 1 1 d . . . H7A H 1.0000 0.8852 0.7029 0.030 Uiso 1 1 calc R . . H7B H 0.8348 0.8530 0.7053 0.030 Uiso 1 1 calc R . . C8A C 0.9490(6) 0.8169(4) 0.73949(9) 0.0232(11) Uani 1 1 d . . . H8A H 0.9637 0.7372 0.7346 0.028 Uiso 1 1 calc R . . H8B H 1.0377 0.8448 0.7478 0.028 Uiso 1 1 calc R . . C9A C 0.8248(5) 0.8261(4) 0.75883(9) 0.0158(11) Uani 1 1 d . . . H9A H 0.7386 0.7895 0.7511 0.019 Uiso 1 1 calc R . . C10A C 0.7904(5) 0.6809(5) 0.78869(10) 0.0203(12) Uani 1 1 d . . . H10A H 0.7151 0.6583 0.7774 0.024 Uiso 1 1 calc R . . C11A C 0.8195(6) 0.6139(5) 0.81219(11) 0.0249(13) Uani 1 1 d . . . C12A C 0.7404(6) 0.5185(5) 0.81708(12) 0.0333(14) Uani 1 1 d . . . H12A H 0.6679 0.4964 0.8052 0.040 Uiso 1 1 calc R . . C13A C 0.7660(8) 0.4543(6) 0.83933(15) 0.048(2) Uani 1 1 d . . . H13A H 0.7096 0.3898 0.8429 0.058 Uiso 1 1 calc R . . C14A C 0.8742(7) 0.4854(6) 0.85614(14) 0.050(2) Uani 1 1 d . . . H14A H 0.8924 0.4416 0.8713 0.060 Uiso 1 1 calc R . . C15A C 0.9559(8) 0.5792(6) 0.85111(12) 0.0416(16) Uani 1 1 d . . . H15A H 1.0295 0.6004 0.8629 0.050 Uiso 1 1 calc R . . C16A C 0.9311(6) 0.6419(5) 0.82919(11) 0.0282(13) Uani 1 1 d . . . H16A H 0.9900 0.7049 0.8255 0.034 Uiso 1 1 calc R . . C17A C 0.3002(5) 0.9328(5) 0.79944(11) 0.0213(12) Uani 1 1 d . . . H17A H 0.2653 0.9545 0.8172 0.026 Uiso 1 1 calc R . . C18A C 0.2361(6) 1.0126(5) 0.78010(14) 0.0351(15) Uani 1 1 d . . . H18A H 0.2747 1.0882 0.7830 0.053 Uiso 1 1 calc R . . H18B H 0.1323 1.0140 0.7823 0.053 Uiso 1 1 calc R . . H18C H 0.2593 0.9877 0.7624 0.053 Uiso 1 1 calc R . . C19A C 0.2572(6) 0.8116(5) 0.79460(12) 0.0284(14) Uani 1 1 d . . . H19A H 0.1534 0.8044 0.7962 0.043 Uiso 1 1 calc R . . H19B H 0.3036 0.7629 0.8075 0.043 Uiso 1 1 calc R . . H19C H 0.2868 0.7892 0.7770 0.043 Uiso 1 1 calc R . . C20A C 0.5082(6) 1.0925(5) 0.85988(11) 0.0272(13) Uani 1 1 d . . . H20A H 0.5527 1.1546 0.8515 0.033 Uiso 1 1 calc R . . C21A C 0.4587(8) 1.1026(5) 0.88521(11) 0.0373(15) Uani 1 1 d . . . H21A H 0.4694 1.1721 0.8942 0.045 Uiso 1 1 calc R . . C22A C 0.3947(6) 1.0139(5) 0.89750(11) 0.0287(13) Uani 1 1 d . . . H22A H 0.3623 1.0222 0.9150 0.034 Uiso 1 1 calc R . . C23A C 0.3769(6) 0.9125(5) 0.88479(11) 0.0247(13) Uani 1 1 d . . . H23A H 0.3316 0.8511 0.8933 0.030 Uiso 1 1 calc R . . C24A C 0.4258(5) 0.9016(4) 0.85947(10) 0.0196(12) Uani 1 1 d . . . H24A H 0.4140 0.8321 0.8506 0.023 Uiso 1 1 calc R . . C25A C 0.4925(4) 0.9913(4) 0.84683(9) 0.0161(11) Uani 1 1 d . . . C26A C 0.8158(5) 1.0183(5) 0.82364(10) 0.0155(11) Uani 1 1 d . . . C27A C 0.8663(6) 1.1282(5) 0.82260(13) 0.0332(16) Uani 1 1 d . . . H27A H 0.8173 1.1836 0.8127 0.040 Uiso 1 1 calc R . . C28A C 0.9874(7) 1.1554(5) 0.83602(15) 0.0451(19) Uani 1 1 d . . . H28A H 1.0221 1.2304 0.8354 0.054 Uiso 1 1 calc R . . C29A C 1.0599(6) 1.0766(5) 0.85045(11) 0.0293(13) Uani 1 1 d . . . H29A H 1.1437 1.0973 0.8597 0.035 Uiso 1 1 calc R . . C30A C 1.0106(5) 0.9674(5) 0.85146(11) 0.0267(13) Uani 1 1 d . . . H30A H 1.0606 0.9123 0.8613 0.032 Uiso 1 1 calc R . . C31A C 0.8885(6) 0.9386(5) 0.83812(11) 0.0224(12) Uani 1 1 d . . . H31A H 0.8540 0.8636 0.8389 0.027 Uiso 1 1 calc R . . N1A N 0.4595(5) 0.9431(3) 0.79940(8) 0.0181(9) Uani 1 1 d . . . N2A N 0.6728(4) 0.9584(3) 0.78405(8) 0.0159(9) Uani 1 1 d . . . N3A N 0.8625(4) 0.7683(4) 0.78288(8) 0.0198(9) Uani 1 1 d . . . C1B C 0.3656(6) 0.5374(4) 0.97131(11) 0.0234(12) Uani 1 1 d . . . H1B H 0.2883 0.5292 0.9831 0.028 Uiso 1 1 calc R . . C2B C 0.5548(5) 0.5002(4) 0.94707(10) 0.0217(11) Uani 1 1 d . . . C3B C 0.5222(5) 0.6110(4) 0.94360(10) 0.0180(11) Uani 1 1 d . . . C4B C 0.3019(5) 0.7301(5) 0.95700(10) 0.0171(11) Uani 1 1 d . . . H4B H 0.3522 0.7924 0.9476 0.021 Uiso 1 1 calc R . . C5B C 0.2601(6) 0.7735(5) 0.98398(10) 0.0223(12) Uani 1 1 d . . . H5C H 0.3463 0.7985 0.9935 0.027 Uiso 1 1 calc R . . H5D H 0.2148 0.7123 0.9941 0.027 Uiso 1 1 calc R . . C6B C 0.1558(6) 0.8720(5) 0.98116(11) 0.0270(13) Uani 1 1 d . . . H6C H 0.1227 0.8953 0.9987 0.032 Uiso 1 1 calc R . . H6D H 0.2061 0.9367 0.9732 0.032 Uiso 1 1 calc R . . C7B C 0.0264(6) 0.8417(5) 0.96437(11) 0.0288(13) Uani 1 1 d . . . H7C H -0.0311 0.7838 0.9734 0.035 Uiso 1 1 calc R . . H7D H -0.0341 0.9091 0.9620 0.035 Uiso 1 1 calc R . . C8B C 0.0722(6) 0.7973(5) 0.93785(11) 0.0266(13) Uani 1 1 d . . . H8C H 0.1215 0.8578 0.9281 0.032 Uiso 1 1 calc R . . H8D H -0.0131 0.7748 0.9278 0.032 Uiso 1 1 calc R . . C9B C 0.1720(6) 0.6966(5) 0.94072(11) 0.0224(12) Uani 1 1 d . . . H9B H 0.1204 0.6333 0.9495 0.027 Uiso 1 1 calc R . . C10B C 0.2135(6) 0.5566(5) 0.90992(11) 0.0219(13) Uani 1 1 d . . . H10B H 0.1700 0.5075 0.9222 0.026 Uiso 1 1 calc R . . C11B C 0.2679(5) 0.5095(5) 0.88536(10) 0.0208(12) Uani 1 1 d . . . C12B C 0.2497(6) 0.3967(5) 0.87940(13) 0.0306(14) Uani 1 1 d . . . H12B H 0.2033 0.3483 0.8915 0.037 Uiso 1 1 calc R . . C13B C 0.2993(7) 0.3539(6) 0.85570(13) 0.0369(16) Uani 1 1 d . . . H13B H 0.2855 0.2768 0.8516 0.044 Uiso 1 1 calc R . . C14B C 0.3676(7) 0.4228(6) 0.83841(14) 0.0395(17) Uani 1 1 d . . . H14B H 0.4006 0.3933 0.8223 0.047 Uiso 1 1 calc R . . C15B C 0.3888(7) 0.5342(6) 0.84418(12) 0.0369(15) Uani 1 1 d . . . H15B H 0.4374 0.5815 0.8322 0.044 Uiso 1 1 calc R . . C16B C 0.3389(6) 0.5776(5) 0.86765(11) 0.0268(13) Uani 1 1 d . . . H16B H 0.3536 0.6548 0.8716 0.032 Uiso 1 1 calc R . . C17B C 0.4470(7) 0.3389(4) 0.97452(11) 0.0254(12) Uani 1 1 d . . . H17B H 0.5334 0.2974 0.9684 0.031 Uiso 1 1 calc R . . C18B C 0.4486(8) 0.3407(5) 1.00405(11) 0.0338(14) Uani 1 1 d . . . H18D H 0.5301 0.3851 1.0101 0.051 Uiso 1 1 calc R . . H18E H 0.4567 0.2636 1.0107 0.051 Uiso 1 1 calc R . . H18F H 0.3600 0.3745 1.0105 0.051 Uiso 1 1 calc R . . C19B C 0.3178(6) 0.2819(5) 0.96350(13) 0.0332(15) Uani 1 1 d . . . H19D H 0.3175 0.2899 0.9445 0.050 Uiso 1 1 calc R . . H19E H 0.2316 0.3167 0.9707 0.050 Uiso 1 1 calc R . . H19F H 0.3197 0.2019 0.9681 0.050 Uiso 1 1 calc R . . C20B C 0.6714(6) 0.4300(5) 0.93642(11) 0.0240(13) Uani 1 1 d . . . C21B C 0.8042(6) 0.4274(5) 0.94814(12) 0.0289(14) Uani 1 1 d . . . H21B H 0.8236 0.4746 0.9627 0.035 Uiso 1 1 calc R . . C22B C 0.9087(6) 0.3563(6) 0.93873(13) 0.0373(16) Uani 1 1 d . . . H22B H 0.9990 0.3539 0.9471 0.045 Uiso 1 1 calc R . . C23B C 0.8843(6) 0.2894(5) 0.91757(14) 0.0364(16) Uani 1 1 d . . . H23B H 0.9577 0.2421 0.9110 0.044 Uiso 1 1 calc R . . C24B C 0.7515(7) 0.2912(6) 0.90571(14) 0.0394(17) Uani 1 1 d . . . H24B H 0.7330 0.2431 0.8913 0.047 Uiso 1 1 calc R . . C25B C 0.6462(6) 0.3619(5) 0.91462(13) 0.0314(14) Uani 1 1 d . . . H25B H 0.5565 0.3645 0.9060 0.038 Uiso 1 1 calc R . . C26B C 0.5974(5) 0.6973(4) 0.92828(10) 0.0188(12) Uani 1 1 d . . . C27B C 0.6272(5) 0.8020(4) 0.93930(11) 0.0200(12) Uani 1 1 d . . . H27B H 0.5994 0.8174 0.9568 0.024 Uiso 1 1 calc R . . C28B C 0.6971(5) 0.8835(5) 0.92492(11) 0.0239(13) Uani 1 1 d . . . H28B H 0.7165 0.9549 0.9324 0.029 Uiso 1 1 calc R . . C29B C 0.7388(6) 0.8604(5) 0.89943(12) 0.0282(14) Uani 1 1 d . . . H29B H 0.7852 0.9165 0.8893 0.034 Uiso 1 1 calc R . . C30B C 0.7126(6) 0.7567(6) 0.88907(11) 0.0294(14) Uani 1 1 d . . . H30B H 0.7444 0.7403 0.8719 0.035 Uiso 1 1 calc R . . C31B C 0.6412(6) 0.6754(5) 0.90297(11) 0.0247(13) Uani 1 1 d . . . H31B H 0.6218 0.6044 0.8952 0.030 Uiso 1 1 calc R . . N1B N 0.4555(5) 0.4572(3) 0.96460(8) 0.0244(10) Uani 1 1 d . . . N2B N 0.4012(4) 0.6332(4) 0.95867(8) 0.0168(9) Uani 1 1 d . . . N3B N 0.2227(5) 0.6604(4) 0.91526(9) 0.0189(10) Uani 1 1 d . . . I1A I 0.55438(4) 0.26207(3) 0.780647(7) 0.02584(9) Uani 1 1 d . . . I1B I 0.53763(4) 0.02004(3) 0.990220(7) 0.02909(10) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1A 0.015(2) 0.013(2) 0.023(3) -0.002(2) 0.004(3) -0.004(2) C2A 0.013(2) 0.016(2) 0.021(2) 0.001(2) -0.003(2) -0.001(2) C3A 0.014(2) 0.015(3) 0.016(3) 0.002(2) 0.0018(19) -0.005(2) C4A 0.016(3) 0.024(3) 0.016(3) 0.001(2) -0.001(2) -0.004(2) C5A 0.025(3) 0.020(3) 0.023(3) 0.006(2) 0.007(2) 0.007(2) C6A 0.027(3) 0.031(3) 0.027(3) 0.004(3) 0.005(3) -0.006(2) C7A 0.017(3) 0.041(3) 0.017(3) -0.002(2) 0.010(2) -0.006(2) C8A 0.015(2) 0.034(3) 0.021(3) -0.003(2) 0.000(2) 0.000(3) C9A 0.013(2) 0.023(3) 0.012(3) -0.001(2) 0.000(2) -0.005(2) C10A 0.015(3) 0.022(3) 0.024(3) -0.001(2) 0.005(2) 0.002(2) C11A 0.020(3) 0.031(3) 0.024(3) -0.001(3) 0.010(2) 0.002(2) C12A 0.030(3) 0.031(3) 0.039(4) 0.010(3) 0.009(3) 0.001(3) C13A 0.042(4) 0.043(5) 0.059(5) 0.030(4) 0.007(4) 0.006(3) C14A 0.039(4) 0.056(5) 0.056(5) 0.034(4) 0.013(3) 0.019(4) C15A 0.023(3) 0.064(4) 0.037(4) 0.012(3) 0.000(3) 0.012(4) C16A 0.018(3) 0.034(3) 0.032(3) 0.011(3) 0.010(3) 0.007(3) C17A 0.008(2) 0.035(3) 0.022(3) 0.001(3) 0.002(2) -0.007(2) C18A 0.018(3) 0.036(4) 0.051(4) 0.014(4) -0.005(3) -0.003(3) C19A 0.021(3) 0.035(3) 0.029(3) 0.004(3) -0.002(3) -0.013(3) C20A 0.024(3) 0.022(3) 0.036(3) 0.000(3) 0.004(2) -0.008(2) C21A 0.034(3) 0.045(4) 0.033(3) -0.017(3) 0.009(3) -0.007(3) C22A 0.024(3) 0.042(4) 0.021(3) -0.003(3) 0.003(2) 0.000(3) C23A 0.018(3) 0.033(3) 0.023(3) 0.003(3) 0.002(2) 0.004(2) C24A 0.019(3) 0.022(3) 0.018(3) -0.003(2) 0.000(2) 0.000(2) C25A 0.010(2) 0.018(3) 0.020(3) 0.001(2) -0.0027(18) 0.0024(19) C26A 0.012(2) 0.019(3) 0.015(3) 0.003(2) 0.002(2) -0.003(2) C27A 0.029(3) 0.017(3) 0.053(4) 0.009(3) -0.021(3) -0.007(3) C28A 0.031(4) 0.025(3) 0.079(5) 0.000(3) -0.025(3) -0.011(3) C29A 0.019(3) 0.041(3) 0.027(3) -0.002(3) -0.009(3) -0.003(3) C30A 0.020(3) 0.036(3) 0.025(3) 0.005(3) -0.005(2) -0.001(2) C31A 0.020(3) 0.026(3) 0.022(3) 0.006(2) -0.001(2) -0.003(2) N1A 0.013(2) 0.022(2) 0.019(2) 0.0030(17) 0.002(2) 0.001(2) N2A 0.012(2) 0.019(2) 0.018(2) 0.0001(19) 0.0044(18) -0.0036(17) N3A 0.0123(19) 0.023(2) 0.024(2) -0.006(2) -0.0009(18) 0.0045(19) C1B 0.024(3) 0.021(3) 0.025(3) 0.001(2) 0.001(2) -0.001(2) C2B 0.015(2) 0.024(3) 0.026(3) -0.004(2) -0.003(2) -0.001(2) C3B 0.016(3) 0.021(3) 0.017(3) -0.002(2) -0.004(2) 0.002(2) C4B 0.015(2) 0.019(3) 0.017(3) 0.002(2) 0.003(2) 0.005(2) C5B 0.030(3) 0.023(3) 0.014(3) 0.004(2) -0.001(2) 0.001(2) C6B 0.031(3) 0.026(3) 0.025(3) 0.000(3) 0.005(3) 0.006(3) C7B 0.020(3) 0.031(3) 0.035(3) -0.001(3) 0.002(3) 0.008(3) C8B 0.022(3) 0.034(3) 0.025(3) 0.002(2) -0.002(2) 0.010(2) C9B 0.016(3) 0.030(3) 0.021(3) 0.005(2) 0.001(2) 0.000(2) C10B 0.018(3) 0.028(3) 0.019(3) 0.010(2) -0.004(2) -0.001(2) C11B 0.017(3) 0.021(3) 0.024(3) -0.002(2) -0.006(2) 0.003(2) C12B 0.024(3) 0.031(3) 0.037(4) -0.004(3) -0.006(3) -0.006(3) C13B 0.027(3) 0.037(4) 0.047(4) -0.023(3) -0.010(3) 0.003(3) C14B 0.031(4) 0.047(4) 0.040(4) -0.026(3) 0.004(3) 0.007(3) C15B 0.034(3) 0.043(4) 0.033(4) -0.002(3) 0.009(3) 0.003(3) C16B 0.027(3) 0.029(3) 0.024(3) -0.007(3) 0.000(3) 0.001(3) C17B 0.021(3) 0.019(3) 0.037(3) 0.002(2) -0.005(3) 0.005(3) C18B 0.042(3) 0.025(3) 0.034(3) 0.007(2) -0.002(3) 0.006(3) C19B 0.032(3) 0.014(3) 0.053(4) 0.007(3) -0.018(3) -0.004(3) C20B 0.019(3) 0.021(3) 0.031(3) 0.000(3) 0.005(2) 0.004(2) C21B 0.017(3) 0.041(4) 0.028(3) 0.003(3) 0.000(2) -0.002(3) C22B 0.022(3) 0.055(4) 0.035(4) 0.012(3) 0.005(3) 0.010(3) C23B 0.028(3) 0.027(3) 0.054(4) 0.010(3) 0.021(3) 0.013(3) C24B 0.033(4) 0.038(4) 0.048(4) -0.014(3) 0.010(3) 0.004(3) C25B 0.021(3) 0.029(3) 0.044(4) -0.008(3) -0.001(3) 0.002(3) C26B 0.015(3) 0.023(3) 0.019(3) 0.001(2) -0.002(2) 0.003(2) C27B 0.014(3) 0.020(3) 0.025(3) 0.001(2) 0.000(2) 0.003(2) C28B 0.013(3) 0.024(3) 0.034(4) 0.002(3) -0.004(2) -0.002(2) C29B 0.019(3) 0.030(3) 0.036(4) 0.009(3) 0.003(3) 0.002(2) C30B 0.025(3) 0.043(4) 0.020(3) 0.008(3) 0.007(2) 0.007(3) C31B 0.021(3) 0.026(3) 0.027(3) 0.000(3) -0.002(2) 0.009(2) N1B 0.021(2) 0.025(2) 0.028(2) 0.0049(19) -0.002(2) 0.002(2) N2B 0.013(2) 0.019(2) 0.019(2) 0.0008(19) -0.0015(17) 0.0046(17) N3B 0.017(2) 0.023(3) 0.017(2) 0.004(2) 0.0021(19) 0.0050(19) I1A 0.02852(18) 0.02549(18) 0.02351(17) 0.00096(15) -0.00175(17) 0.00920(16) I1B 0.02615(18) 0.02310(18) 0.0380(2) -0.00623(16) -0.00557(18) 0.00542(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1A N1A 1.329(6) . ? C1A N2A 1.340(6) . ? C1A H1A 0.9500 . ? C2A C3A 1.364(7) . ? C2A N1A 1.376(6) . ? C2A C25A 1.486(7) . ? C3A N2A 1.379(6) . ? C3A C26A 1.493(7) . ? C4A N2A 1.491(6) . ? C4A C5A 1.506(7) . ? C4A C9A 1.532(7) . ? C4A H4A 1.0000 . ? C5A C6A 1.520(7) . ? C5A H5A 0.9900 . ? C5A H5B 0.9900 . ? C6A C7A 1.526(8) . ? C6A H6A 0.9900 . ? C6A H6B 0.9900 . ? C7A C8A 1.553(7) . ? C7A H7A 0.9900 . ? C7A H7B 0.9900 . ? C8A C9A 1.533(7) . ? C8A H8A 0.9900 . ? C8A H8B 0.9900 . ? C9A N3A 1.455(6) . ? C9A H9A 1.0000 . ? C10A N3A 1.275(7) . ? C10A C11A 1.470(8) . ? C10A H10A 0.9500 . ? C11A C12A 1.378(8) . ? C11A C16A 1.401(8) . ? C12A C13A 1.393(9) . ? C12A H12A 0.9500 . ? C13A C14A 1.381(11) . ? C13A H13A 0.9500 . ? C14A C15A 1.378(10) . ? C14A H14A 0.9500 . ? C15A C16A 1.368(8) . ? C15A H15A 0.9500 . ? C16A H16A 0.9500 . ? C17A C18A 1.498(8) . ? C17A N1A 1.498(6) . ? C17A C19A 1.516(8) . ? C17A H17A 1.0000 . ? C18A H18A 0.9800 . ? C18A H18B 0.9800 . ? C18A H18C 0.9800 . ? C19A H19A 0.9800 . ? C19A H19B 0.9800 . ? C19A H19C 0.9800 . ? C20A C21A 1.384(8) . ? C20A C25A 1.384(7) . ? C20A H20A 0.9500 . ? C21A C22A 1.367(8) . ? C21A H21A 0.9500 . ? C22A C23A 1.381(8) . ? C22A H22A 0.9500 . ? C23A C24A 1.383(7) . ? C23A H23A 0.9500 . ? C24A C25A 1.396(7) . ? C24A H24A 0.9500 . ? C26A C31A 1.383(7) . ? C26A C27A 1.391(8) . ? C27A C28A 1.366(8) . ? C27A H27A 0.9500 . ? C28A C29A 1.373(8) . ? C28A H28A 0.9500 . ? C29A C30A 1.380(8) . ? C29A H29A 0.9500 . ? C30A C31A 1.376(7) . ? C30A H30A 0.9500 . ? C31A H31A 0.9500 . ? C1B N1B 1.318(7) . ? C1B N2B 1.352(7) . ? C1B H1B 0.9500 . ? C2B C3B 1.364(7) . ? C2B N1B 1.391(7) . ? C2B C20B 1.480(7) . ? C3B N2B 1.397(6) . ? C3B C26B 1.471(7) . ? C4B N2B 1.484(6) . ? C4B C5B 1.527(7) . ? C4B C9B 1.529(7) . ? C4B H4B 1.0000 . ? C5B C6B 1.533(7) . ? C5B H5C 0.9900 . ? C5B H5D 0.9900 . ? C6B C7B 1.530(8) . ? C6B H6C 0.9900 . ? C6B H6D 0.9900 . ? C7B C8B 1.520(8) . ? C7B H7C 0.9900 . ? C7B H7D 0.9900 . ? C8B C9B 1.527(7) . ? C8B H8C 0.9900 . ? C8B H8D 0.9900 . ? C9B N3B 1.454(7) . ? C9B H9B 1.0000 . ? C10B N3B 1.267(7) . ? C10B C11B 1.469(8) . ? C10B H10B 0.9500 . ? C11B C12B 1.386(8) . ? C11B C16B 1.387(8) . ? C12B C13B 1.396(9) . ? C12B H12B 0.9500 . ? C13B C14B 1.366(10) . ? C13B H13B 0.9500 . ? C14B C15B 1.371(9) . ? C14B H14B 0.9500 . ? C15B C16B 1.390(8) . ? C15B H15B 0.9500 . ? C16B H16B 0.9500 . ? C17B N1B 1.497(6) . ? C17B C19B 1.498(8) . ? C17B C18B 1.514(7) . ? C17B H17B 1.0000 . ? C18B H18D 0.9800 . ? C18B H18E 0.9800 . ? C18B H18F 0.9800 . ? C19B H19D 0.9800 . ? C19B H19E 0.9800 . ? C19B H19F 0.9800 . ? C20B C21B 1.383(8) . ? C20B C25B 1.400(8) . ? C21B C22B 1.381(8) . ? C21B H21B 0.9500 . ? C22B C23B 1.364(9) . ? C22B H22B 0.9500 . ? C23B C24B 1.385(9) . ? C23B H23B 0.9500 . ? C24B C25B 1.375(8) . ? C24B H24B 0.9500 . ? C25B H25B 0.9500 . ? C26B C31B 1.385(8) . ? C26B C27B 1.396(7) . ? C27B C28B 1.382(8) . ? C27B H27B 0.9500 . ? C28B C29B 1.391(8) . ? C28B H28B 0.9500 . ? C29B C30B 1.365(9) . ? C29B H29B 0.9500 . ? C30B C31B 1.374(8) . ? C30B H30B 0.9500 . ? C31B H31B 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 N1A C1A N2A 107.8(5) . . ? N1A C1A H1A 126.1 . . ? N2A C1A H1A 126.1 . . ? C3A C2A N1A 107.2(4) . . ? C3A C2A C25A 129.7(4) . . ? N1A C2A C25A 123.1(4) . . ? C2A C3A N2A 106.2(4) . . ? C2A C3A C26A 130.0(5) . . ? N2A C3A C26A 123.8(4) . . ? N2A C4A C5A 111.2(4) . . ? N2A C4A C9A 110.5(4) . . ? C5A C4A C9A 112.7(4) . . ? N2A C4A H4A 107.4 . . ? C5A C4A H4A 107.4 . . ? C9A C4A H4A 107.4 . . ? C4A C5A C6A 110.7(5) . . ? C4A C5A H5A 109.5 . . ? C6A C5A H5A 109.5 . . ? C4A C5A H5B 109.5 . . ? C6A C5A H5B 109.5 . . ? H5A C5A H5B 108.1 . . ? C5A C6A C7A 110.9(4) . . ? C5A C6A H6A 109.5 . . ? C7A C6A H6A 109.5 . . ? C5A C6A H6B 109.5 . . ? C7A C6A H6B 109.5 . . ? H6A C6A H6B 108.1 . . ? C6A C7A C8A 112.3(4) . . ? C6A C7A H7A 109.1 . . ? C8A C7A H7A 109.1 . . ? C6A C7A H7B 109.1 . . ? C8A C7A H7B 109.1 . . ? H7A C7A H7B 107.9 . . ? C9A C8A C7A 109.9(4) . . ? C9A C8A H8A 109.7 . . ? C7A C8A H8A 109.7 . . ? C9A C8A H8B 109.7 . . ? C7A C8A H8B 109.7 . . ? H8A C8A H8B 108.2 . . ? N3A C9A C4A 109.8(4) . . ? N3A C9A C8A 109.3(4) . . ? C4A C9A C8A 110.6(4) . . ? N3A C9A H9A 109.0 . . ? C4A C9A H9A 109.0 . . ? C8A C9A H9A 109.0 . . ? N3A C10A C11A 122.3(5) . . ? N3A C10A H10A 118.9 . . ? C11A C10A H10A 118.9 . . ? C12A C11A C16A 118.9(6) . . ? C12A C11A C10A 119.7(5) . . ? C16A C11A C10A 121.3(5) . . ? C11A C12A C13A 120.5(6) . . ? C11A C12A H12A 119.8 . . ? C13A C12A H12A 119.8 . . ? C14A C13A C12A 119.4(7) . . ? C14A C13A H13A 120.3 . . ? C12A C13A H13A 120.3 . . ? C15A C14A C13A 120.5(6) . . ? C15A C14A H14A 119.7 . . ? C13A C14A H14A 119.7 . . ? C16A C15A C14A 120.0(7) . . ? C16A C15A H15A 120.0 . . ? C14A C15A H15A 120.0 . . ? C15A C16A C11A 120.5(6) . . ? C15A C16A H16A 119.7 . . ? C11A C16A H16A 119.7 . . ? C18A C17A N1A 110.3(4) . . ? C18A C17A C19A 112.7(5) . . ? N1A C17A C19A 110.0(4) . . ? C18A C17A H17A 107.9 . . ? N1A C17A H17A 107.9 . . ? C19A C17A H17A 107.9 . . ? C17A C18A H18A 109.5 . . ? C17A C18A H18B 109.5 . . ? H18A C18A H18B 109.5 . . ? C17A C18A H18C 109.5 . . ? H18A C18A H18C 109.5 . . ? H18B C18A H18C 109.5 . . ? C17A C19A H19A 109.5 . . ? C17A C19A H19B 109.5 . . ? H19A C19A H19B 109.5 . . ? C17A C19A H19C 109.5 . . ? H19A C19A H19C 109.5 . . ? H19B C19A H19C 109.5 . . ? C21A C20A C25A 119.6(5) . . ? C21A C20A H20A 120.2 . . ? C25A C20A H20A 120.2 . . ? C22A C21A C20A 120.8(5) . . ? C22A C21A H21A 119.6 . . ? C20A C21A H21A 119.6 . . ? C21A C22A C23A 120.6(5) . . ? C21A C22A H22A 119.7 . . ? C23A C22A H22A 119.7 . . ? C22A C23A C24A 119.0(5) . . ? C22A C23A H23A 120.5 . . ? C24A C23A H23A 120.5 . . ? C23A C24A C25A 120.8(5) . . ? C23A C24A H24A 119.6 . . ? C25A C24A H24A 119.6 . . ? C20A C25A C24A 119.2(5) . . ? C20A C25A C2A 121.7(5) . . ? C24A C25A C2A 119.1(4) . . ? C31A C26A C27A 119.7(5) . . ? C31A C26A C3A 119.5(5) . . ? C27A C26A C3A 120.7(5) . . ? C28A C27A C26A 119.1(6) . . ? C28A C27A H27A 120.5 . . ? C26A C27A H27A 120.5 . . ? C27A C28A C29A 121.4(6) . . ? C27A C28A H28A 119.3 . . ? C29A C28A H28A 119.3 . . ? C28A C29A C30A 119.8(5) . . ? C28A C29A H29A 120.1 . . ? C30A C29A H29A 120.1 . . ? C31A C30A C29A 119.6(5) . . ? C31A C30A H30A 120.2 . . ? C29A C30A H30A 120.2 . . ? C30A C31A C26A 120.5(5) . . ? C30A C31A H31A 119.8 . . ? C26A C31A H31A 119.8 . . ? C1A N1A C2A 109.3(4) . . ? C1A N1A C17A 122.9(4) . . ? C2A N1A C17A 127.4(4) . . ? C1A N2A C3A 109.4(4) . . ? C1A N2A C4A 121.9(4) . . ? C3A N2A C4A 128.6(4) . . ? C10A N3A C9A 117.0(4) . . ? N1B C1B N2B 109.1(5) . . ? N1B C1B H1B 125.5 . . ? N2B C1B H1B 125.5 . . ? C3B C2B N1B 106.8(5) . . ? C3B C2B C20B 131.4(5) . . ? N1B C2B C20B 121.7(4) . . ? C2B C3B N2B 107.0(5) . . ? C2B C3B C26B 129.4(5) . . ? N2B C3B C26B 123.5(5) . . ? N2B C4B C5B 111.8(4) . . ? N2B C4B C9B 109.2(4) . . ? C5B C4B C9B 112.2(4) . . ? N2B C4B H4B 107.9 . . ? C5B C4B H4B 107.9 . . ? C9B C4B H4B 107.9 . . ? C4B C5B C6B 109.7(4) . . ? C4B C5B H5C 109.7 . . ? C6B C5B H5C 109.7 . . ? C4B C5B H5D 109.7 . . ? C6B C5B H5D 109.7 . . ? H5C C5B H5D 108.2 . . ? C7B C6B C5B 112.2(5) . . ? C7B C6B H6C 109.2 . . ? C5B C6B H6C 109.2 . . ? C7B C6B H6D 109.2 . . ? C5B C6B H6D 109.2 . . ? H6C C6B H6D 107.9 . . ? C8B C7B C6B 111.2(5) . . ? C8B C7B H7C 109.4 . . ? C6B C7B H7C 109.4 . . ? C8B C7B H7D 109.4 . . ? C6B C7B H7D 109.4 . . ? H7C C7B H7D 108.0 . . ? C7B C8B C9B 111.0(4) . . ? C7B C8B H8C 109.4 . . ? C9B C8B H8C 109.4 . . ? C7B C8B H8D 109.4 . . ? C9B C8B H8D 109.4 . . ? H8C C8B H8D 108.0 . . ? N3B C9B C8B 110.2(4) . . ? N3B C9B C4B 107.8(4) . . ? C8B C9B C4B 109.6(5) . . ? N3B C9B H9B 109.7 . . ? C8B C9B H9B 109.7 . . ? C4B C9B H9B 109.7 . . ? N3B C10B C11B 122.2(5) . . ? N3B C10B H10B 118.9 . . ? C11B C10B H10B 118.9 . . ? C12B C11B C16B 118.7(5) . . ? C12B C11B C10B 121.0(5) . . ? C16B C11B C10B 120.3(5) . . ? C11B C12B C13B 120.2(6) . . ? C11B C12B H12B 119.9 . . ? C13B C12B H12B 119.9 . . ? C14B C13B C12B 120.2(6) . . ? C14B C13B H13B 119.9 . . ? C12B C13B H13B 119.9 . . ? C13B C14B C15B 120.4(6) . . ? C13B C14B H14B 119.8 . . ? C15B C14B H14B 119.8 . . ? C14B C15B C16B 119.8(7) . . ? C14B C15B H15B 120.1 . . ? C16B C15B H15B 120.1 . . ? C11B C16B C15B 120.7(6) . . ? C11B C16B H16B 119.6 . . ? C15B C16B H16B 119.6 . . ? N1B C17B C19B 109.9(5) . . ? N1B C17B C18B 109.0(4) . . ? C19B C17B C18B 113.0(6) . . ? N1B C17B H17B 108.3 . . ? C19B C17B H17B 108.3 . . ? C18B C17B H17B 108.3 . . ? C17B C18B H18D 109.5 . . ? C17B C18B H18E 109.5 . . ? H18D C18B H18E 109.5 . . ? C17B C18B H18F 109.5 . . ? H18D C18B H18F 109.5 . . ? H18E C18B H18F 109.5 . . ? C17B C19B H19D 109.5 . . ? C17B C19B H19E 109.5 . . ? H19D C19B H19E 109.5 . . ? C17B C19B H19F 109.5 . . ? H19D C19B H19F 109.5 . . ? H19E C19B H19F 109.5 . . ? C21B C20B C25B 119.1(5) . . ? C21B C20B C2B 121.2(5) . . ? C25B C20B C2B 119.7(5) . . ? C22B C21B C20B 120.0(6) . . ? C22B C21B H21B 120.0 . . ? C20B C21B H21B 120.0 . . ? C23B C22B C21B 121.1(6) . . ? C23B C22B H22B 119.5 . . ? C21B C22B H22B 119.5 . . ? C22B C23B C24B 119.4(6) . . ? C22B C23B H23B 120.3 . . ? C24B C23B H23B 120.3 . . ? C25B C24B C23B 120.6(6) . . ? C25B C24B H24B 119.7 . . ? C23B C24B H24B 119.7 . . ? C24B C25B C20B 119.8(6) . . ? C24B C25B H25B 120.1 . . ? C20B C25B H25B 120.1 . . ? C31B C26B C27B 119.1(5) . . ? C31B C26B C3B 120.7(5) . . ? C27B C26B C3B 120.1(5) . . ? C28B C27B C26B 120.3(5) . . ? C28B C27B H27B 119.8 . . ? C26B C27B H27B 119.8 . . ? C27B C28B C29B 119.7(6) . . ? C27B C28B H28B 120.1 . . ? C29B C28B H28B 120.1 . . ? C30B C29B C28B 119.5(5) . . ? C30B C29B H29B 120.3 . . ? C28B C29B H29B 120.3 . . ? C29B C30B C31B 121.4(5) . . ? C29B C30B H30B 119.3 . . ? C31B C30B H30B 119.3 . . ? C30B C31B C26B 119.9(6) . . ? C30B C31B H31B 120.1 . . ? C26B C31B H31B 120.1 . . ? C1B N1B C2B 109.3(4) . . ? C1B N1B C17B 123.8(5) . . ? C2B N1B C17B 126.9(5) . . ? C1B N2B C3B 107.8(4) . . ? C1B N2B C4B 121.8(4) . . ? C3B N2B C4B 128.6(4) . . ? C10B N3B C9B 117.4(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 N1A C2A C3A N2A -0.8(6) . . . . ? C25A C2A C3A N2A 178.0(5) . . . . ? N1A C2A C3A C26A -179.5(5) . . . . ? C25A C2A C3A C26A -0.8(9) . . . . ? N2A C4A C5A C6A 178.4(4) . . . . ? C9A C4A C5A C6A -56.9(6) . . . . ? C4A C5A C6A C7A 55.7(6) . . . . ? C5A C6A C7A C8A -55.6(6) . . . . ? C6A C7A C8A C9A 54.7(6) . . . . ? N2A C4A C9A N3A -57.7(5) . . . . ? C5A C4A C9A N3A 177.1(4) . . . . ? N2A C4A C9A C8A -178.4(4) . . . . ? C5A C4A C9A C8A 56.5(6) . . . . ? C7A C8A C9A N3A -174.9(4) . . . . ? C7A C8A C9A C4A -53.9(6) . . . . ? N3A C10A C11A C12A -178.3(5) . . . . ? N3A C10A C11A C16A -1.3(8) . . . . ? C16A C11A C12A C13A 3.4(9) . . . . ? C10A C11A C12A C13A -179.6(6) . . . . ? C11A C12A C13A C14A -1.7(10) . . . . ? C12A C13A C14A C15A 0.3(11) . . . . ? C13A C14A C15A C16A -0.6(10) . . . . ? C14A C15A C16A C11A 2.3(9) . . . . ? C12A C11A C16A C15A -3.7(9) . . . . ? C10A C11A C16A C15A 179.4(5) . . . . ? C25A C20A C21A C22A 0.1(10) . . . . ? C20A C21A C22A C23A -0.6(10) . . . . ? C21A C22A C23A C24A 0.5(9) . . . . ? C22A C23A C24A C25A 0.0(8) . . . . ? C21A C20A C25A C24A 0.5(8) . . . . ? C21A C20A C25A C2A -179.0(5) . . . . ? C23A C24A C25A C20A -0.5(7) . . . . ? C23A C24A C25A C2A 178.9(5) . . . . ? C3A C2A C25A C20A 58.7(8) . . . . ? N1A C2A C25A C20A -122.8(5) . . . . ? C3A C2A C25A C24A -120.8(6) . . . . ? N1A C2A C25A C24A 57.8(6) . . . . ? C2A C3A C26A C31A 79.9(8) . . . . ? N2A C3A C26A C31A -98.6(6) . . . . ? C2A C3A C26A C27A -97.8(7) . . . . ? N2A C3A C26A C27A 83.7(7) . . . . ? C31A C26A C27A C28A -0.1(10) . . . . ? C3A C26A C27A C28A 177.5(6) . . . . ? C26A C27A C28A C29A 0.1(11) . . . . ? C27A C28A C29A C30A 0.2(11) . . . . ? C28A C29A C30A C31A -0.4(9) . . . . ? C29A C30A C31A C26A 0.3(8) . . . . ? C27A C26A C31A C30A -0.1(8) . . . . ? C3A C26A C31A C30A -177.8(5) . . . . ? N2A C1A N1A C2A 0.3(5) . . . . ? N2A C1A N1A C17A 173.7(4) . . . . ? C3A C2A N1A C1A 0.3(5) . . . . ? C25A C2A N1A C1A -178.5(4) . . . . ? C3A C2A N1A C17A -172.7(5) . . . . ? C25A C2A N1A C17A 8.5(7) . . . . ? C18A C17A N1A C1A -54.1(7) . . . . ? C19A C17A N1A C1A 70.9(6) . . . . ? C18A C17A N1A C2A 118.0(6) . . . . ? C19A C17A N1A C2A -116.9(5) . . . . ? N1A C1A N2A C3A -0.8(5) . . . . ? N1A C1A N2A C4A 176.6(4) . . . . ? C2A C3A N2A C1A 1.0(6) . . . . ? C26A C3A N2A C1A 179.8(5) . . . . ? C2A C3A N2A C4A -176.2(5) . . . . ? C26A C3A N2A C4A 2.7(8) . . . . ? C5A C4A N2A C1A 54.1(6) . . . . ? C9A C4A N2A C1A -71.9(6) . . . . ? C5A C4A N2A C3A -129.1(5) . . . . ? C9A C4A N2A C3A 104.9(6) . . . . ? C11A C10A N3A C9A 178.9(5) . . . . ? C4A C9A N3A C10A 124.2(5) . . . . ? C8A C9A N3A C10A -114.3(5) . . . . ? N1B C2B C3B N2B -1.3(5) . . . . ? C20B C2B C3B N2B -179.2(5) . . . . ? N1B C2B C3B C26B 176.2(5) . . . . ? C20B C2B C3B C26B -1.7(10) . . . . ? N2B C4B C5B C6B -179.1(4) . . . . ? C9B C4B C5B C6B -56.1(6) . . . . ? C4B C5B C6B C7B 54.0(6) . . . . ? C5B C6B C7B C8B -54.8(6) . . . . ? C6B C7B C8B C9B 56.2(6) . . . . ? C7B C8B C9B N3B -176.0(5) . . . . ? C7B C8B C9B C4B -57.4(6) . . . . ? N2B C4B C9B N3B -57.5(5) . . . . ? C5B C4B C9B N3B 178.1(4) . . . . ? N2B C4B C9B C8B -177.5(4) . . . . ? C5B C4B C9B C8B 58.1(6) . . . . ? N3B C10B C11B C12B -176.5(5) . . . . ? N3B C10B C11B C16B 3.5(8) . . . . ? C16B C11B C12B C13B -1.5(8) . . . . ? C10B C11B C12B C13B 178.5(5) . . . . ? C11B C12B C13B C14B 0.8(9) . . . . ? C12B C13B C14B C15B 0.4(10) . . . . ? C13B C14B C15B C16B -0.8(10) . . . . ? C12B C11B C16B C15B 1.0(8) . . . . ? C10B C11B C16B C15B -179.0(5) . . . . ? C14B C15B C16B C11B 0.1(9) . . . . ? C3B C2B C20B C21B 84.4(8) . . . . ? N1B C2B C20B C21B -93.2(7) . . . . ? C3B C2B C20B C25B -97.9(7) . . . . ? N1B C2B C20B C25B 84.5(7) . . . . ? C25B C20B C21B C22B -1.5(9) . . . . ? C2B C20B C21B C22B 176.2(5) . . . . ? C20B C21B C22B C23B 1.3(9) . . . . ? C21B C22B C23B C24B -1.4(10) . . . . ? C22B C23B C24B C25B 1.9(10) . . . . ? C23B C24B C25B C20B -2.2(10) . . . . ? C21B C20B C25B C24B 2.0(9) . . . . ? C2B C20B C25B C24B -175.8(6) . . . . ? C2B C3B C26B C31B 47.3(8) . . . . ? N2B C3B C26B C31B -135.5(5) . . . . ? C2B C3B C26B C27B -131.8(6) . . . . ? N2B C3B C26B C27B 45.3(7) . . . . ? C31B C26B C27B C28B 1.3(7) . . . . ? C3B C26B C27B C28B -179.6(5) . . . . ? C26B C27B C28B C29B -0.6(8) . . . . ? C27B C28B C29B C30B -1.2(8) . . . . ? C28B C29B C30B C31B 2.3(9) . . . . ? C29B C30B C31B C26B -1.6(8) . . . . ? C27B C26B C31B C30B -0.2(8) . . . . ? C3B C26B C31B C30B -179.3(5) . . . . ? N2B C1B N1B C2B 0.3(6) . . . . ? N2B C1B N1B C17B -179.0(5) . . . . ? C3B C2B N1B C1B 0.6(6) . . . . ? C20B C2B N1B C1B 178.8(5) . . . . ? C3B C2B N1B C17B 179.9(5) . . . . ? C20B C2B N1B C17B -1.9(8) . . . . ? C19B C17B N1B C1B 69.0(7) . . . . ? C18B C17B N1B C1B -55.4(8) . . . . ? C19B C17B N1B C2B -110.2(6) . . . . ? C18B C17B N1B C2B 125.4(6) . . . . ? N1B C1B N2B C3B -1.1(6) . . . . ? N1B C1B N2B C4B 164.9(4) . . . . ? C2B C3B N2B C1B 1.5(6) . . . . ? C26B C3B N2B C1B -176.2(5) . . . . ? C2B C3B N2B C4B -163.3(5) . . . . ? C26B C3B N2B C4B 19.0(8) . . . . ? C5B C4B N2B C1B 58.8(6) . . . . ? C9B C4B N2B C1B -65.9(6) . . . . ? C5B C4B N2B C3B -138.3(5) . . . . ? C9B C4B N2B C3B 97.1(6) . . . . ? C11B C10B N3B C9B -176.8(4) . . . . ? C8B C9B N3B C10B -130.6(5) . . . . ? C4B C9B N3B C10B 109.7(5) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.04 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.866 _refine_diff_density_min -1.397 _refine_diff_density_rms 0.094 #============= Material Relevant to Complex(13)=====================# data_complex13 _database_code_depnum_ccdc_archive 'CCDC 731706' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C39 H47 N3 Rh), 2(C32 H12 B F24), 1.5(C7 H8)' _chemical_formula_sum 'C152.50 H130 B2 F48 N6 Rh2' _chemical_formula_weight 3186.07 _chemical_absolute_configuration syn 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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 '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' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P 21 21 2' _symmetry_space_group_name_Hall 'P 2ac 2ab ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 13.297(3) _cell_length_b 13.558(3) _cell_length_c 80.440(16) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 14501(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 9610 _cell_measurement_theta_min 2.16 _cell_measurement_theta_max 22.42 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.459 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6476 _exptl_absorpt_coefficient_mu 0.343 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.857 _exptl_absorpt_correction_T_max 0.996 _exptl_absorpt_process_details 'SADABS v2.03; (Sheldrick)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 104979 _diffrn_reflns_av_R_equivalents 0.0495 _diffrn_reflns_av_sigmaI/netI 0.0374 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -86 _diffrn_reflns_limit_l_max 86 _diffrn_reflns_theta_min 1.81 _diffrn_reflns_theta_max 22.55 _reflns_number_total 19029 _reflns_number_gt 18392 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. A number of atoms were restrained to be approximately iostropic, namely: C79-C85, F4,F5 F6, F4a, F5a, F6a, F10 and F11. ; _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^)+(0.0398P)^2^+72.3843P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.06(3) _refine_ls_number_reflns 19029 _refine_ls_number_parameters 1980 _refine_ls_number_restraints 114 _refine_ls_R_factor_all 0.0716 _refine_ls_R_factor_gt 0.0696 _refine_ls_wR_factor_ref 0.1622 _refine_ls_wR_factor_gt 0.1611 _refine_ls_goodness_of_fit_ref 1.205 _refine_ls_restrained_S_all 1.205 _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 C1 C 0.6247(7) 0.7449(9) 0.21766(13) 0.056(3) Uani 1 1 d . . . H1 H 0.5734 0.7183 0.2101 0.067 Uiso 1 1 calc R . . C2 C 0.6717(9) 0.8307(9) 0.21194(16) 0.068(3) Uani 1 1 d . . . H2 H 0.6459 0.8516 0.2011 0.081 Uiso 1 1 calc R . . C3 C 0.7141(10) 0.9153(9) 0.22171(18) 0.084(5) Uani 1 1 d . . . H3A H 0.6599 0.9586 0.2252 0.101 Uiso 1 1 calc R . . H3B H 0.7595 0.9529 0.2147 0.101 Uiso 1 1 calc R . . C4 C 0.7734(11) 0.8761(9) 0.23780(15) 0.081(4) Uani 1 1 d . . . H4A H 0.8210 0.9259 0.2414 0.097 Uiso 1 1 calc R . . H4B H 0.7261 0.8648 0.2468 0.097 Uiso 1 1 calc R . . C5 C 0.8279(8) 0.7835(10) 0.23410(13) 0.061(3) Uani 1 1 d . . . H5 H 0.9011 0.7896 0.2350 0.073 Uiso 1 1 calc R . . C6 C 0.7941(8) 0.6908(9) 0.23632(11) 0.050(3) Uani 1 1 d . . . H6 H 0.8468 0.6430 0.2390 0.060 Uiso 1 1 calc R . . C7 C 0.6933(7) 0.6660(9) 0.24340(11) 0.053(3) Uani 1 1 d . . . H7A H 0.6817 0.5959 0.2419 0.064 Uiso 1 1 calc R . . H7B H 0.6947 0.6791 0.2553 0.064 Uiso 1 1 calc R . . C8 C 0.6078(8) 0.7206(11) 0.23600(15) 0.076(4) Uani 1 1 d . . . H8A H 0.5977 0.7814 0.2421 0.091 Uiso 1 1 calc R . . H8B H 0.5472 0.6812 0.2371 0.091 Uiso 1 1 calc R . . C9 C 0.7037(5) 0.6355(6) 0.17542(8) 0.0168(17) Uani 1 1 d . . . C10 C 0.8101(6) 0.7113(6) 0.15843(10) 0.0263(18) Uani 1 1 d . . . C11 C 0.7546(6) 0.6995(6) 0.18520(10) 0.037(2) Uani 1 1 d . . . C12 C 0.8937(7) 0.8161(7) 0.18206(12) 0.041(2) Uani 1 1 d . . . H12 H 0.8571 0.8535 0.1906 0.049 Uiso 1 1 calc R . . C13 C 0.9377(8) 0.8917(8) 0.17011(13) 0.050(3) Uani 1 1 d . . . H13A H 0.9810 0.8593 0.1621 0.060 Uiso 1 1 calc R . . H13B H 0.8842 0.9248 0.1641 0.060 Uiso 1 1 calc R . . C14 C 0.9975(9) 0.9658(9) 0.18004(16) 0.067(3) Uani 1 1 d . . . H14A H 0.9535 0.9995 0.1878 0.080 Uiso 1 1 calc R . . H14B H 1.0262 1.0148 0.1726 0.080 Uiso 1 1 calc R . . C15 C 1.0805(9) 0.9141(9) 0.18943(15) 0.071(4) Uani 1 1 d . . . H15A H 1.1166 0.9622 0.1961 0.085 Uiso 1 1 calc R . . H15B H 1.1275 0.8862 0.1815 0.085 Uiso 1 1 calc R . . C16 C 1.0421(8) 0.8306(9) 0.20104(13) 0.058(3) Uani 1 1 d . . . H16A H 1.0989 0.7955 0.2057 0.070 Uiso 1 1 calc R . . H16B H 1.0037 0.8590 0.2101 0.070 Uiso 1 1 calc R . . C17 C 0.9755(7) 0.7582(7) 0.19120(14) 0.055(3) Uani 1 1 d . . . H17 H 1.0174 0.7245 0.1829 0.066 Uiso 1 1 calc R . . C18 C 0.9454(6) 0.5783(6) 0.19664(12) 0.038(2) Uani 1 1 d . . . H18A H 0.8996 0.5667 0.1875 0.045 Uiso 1 1 calc R . . H18B H 1.0135 0.5695 0.1926 0.045 Uiso 1 1 calc R . . C19 C 0.9253(6) 0.5060(6) 0.20999(9) 0.0295(19) Uani 1 1 d . . . C20 C 1.0032(8) 0.4683(8) 0.21939(12) 0.048(3) Uani 1 1 d . . . H20 H 1.0691 0.4847 0.2167 0.057 Uiso 1 1 calc R . . C21 C 0.9856(11) 0.4078(9) 0.23251(16) 0.071(4) Uani 1 1 d . . . H21 H 1.0395 0.3822 0.2385 0.085 Uiso 1 1 calc R . . C22 C 0.8894(14) 0.3840(9) 0.23705(15) 0.082(5) Uani 1 1 d . . . H22 H 0.8770 0.3447 0.2463 0.099 Uiso 1 1 calc R . . C23 C 0.8107(10) 0.4202(9) 0.22747(15) 0.063(3) Uani 1 1 d . . . H23 H 0.7449 0.4032 0.2301 0.076 Uiso 1 1 calc R . . C24 C 0.8289(8) 0.4810(8) 0.21406(16) 0.063(3) Uani 1 1 d . . . H24 H 0.7755 0.5050 0.2078 0.075 Uiso 1 1 calc R . . C25 C 0.6175(7) 0.5806(9) 0.18191(11) 0.049(3) Uani 1 1 d . . . H25 H 0.6187 0.5888 0.1940 0.059 Uiso 1 1 calc R . . C26 C 0.5195(7) 0.6257(13) 0.17593(14) 0.096(6) Uani 1 1 d . . . H26A H 0.5210 0.6957 0.1777 0.144 Uiso 1 1 calc R . . H26B H 0.4644 0.5975 0.1820 0.144 Uiso 1 1 calc R . . H26C H 0.5111 0.6125 0.1643 0.144 Uiso 1 1 calc R . . C27 C 0.6239(11) 0.4712(10) 0.17866(17) 0.090(5) Uani 1 1 d . . . H27A H 0.5776 0.4537 0.1700 0.135 Uiso 1 1 calc R . . H27B H 0.6071 0.4359 0.1886 0.135 Uiso 1 1 calc R . . H27C H 0.6911 0.4546 0.1753 0.135 Uiso 1 1 calc R . . C28 C 0.7045(6) 0.5812(7) 0.14404(10) 0.032(2) Uani 1 1 d . . . C29 C 0.7355(7) 0.4857(8) 0.14241(12) 0.046(2) Uani 1 1 d . . . H29 H 0.7718 0.4557 0.1509 0.055 Uiso 1 1 calc R . . C30 C 0.7129(8) 0.4339(9) 0.12812(14) 0.060(3) Uani 1 1 d . . . H30 H 0.7316 0.3680 0.1272 0.072 Uiso 1 1 calc R . . C31 C 0.6640(9) 0.4776(11) 0.11546(13) 0.065(3) Uani 1 1 d . . . H31 H 0.6511 0.4428 0.1057 0.078 Uiso 1 1 calc R . . C32 C 0.6342(9) 0.5713(10) 0.11695(12) 0.059(3) Uani 1 1 d . . . H32 H 0.5993 0.6007 0.1082 0.070 Uiso 1 1 calc R . . C33 C 0.6538(7) 0.6257(10) 0.13115(14) 0.061(3) Uani 1 1 d . . . H33 H 0.6330 0.6910 0.1320 0.073 Uiso 1 1 calc R . . C34 C 0.8740(6) 0.7398(7) 0.14389(11) 0.036(2) Uani 1 1 d . . . C35 C 0.9633(7) 0.6918(8) 0.14164(11) 0.041(2) Uani 1 1 d . . . H35 H 0.9852 0.6455 0.1494 0.049 Uiso 1 1 calc R . . C36 C 1.0219(8) 0.7134(8) 0.12749(13) 0.054(3) Uani 1 1 d . . . H36 H 1.0804 0.6781 0.1253 0.065 Uiso 1 1 calc R . . C37 C 0.9916(8) 0.7873(8) 0.11694(12) 0.056(3) Uani 1 1 d . . . H37 H 1.0331 0.8052 0.1081 0.067 Uiso 1 1 calc R . . C38 C 0.9024(10) 0.8350(11) 0.11903(15) 0.082(5) Uani 1 1 d . . . H38 H 0.8815 0.8829 0.1115 0.098 Uiso 1 1 calc R . . C39 C 0.8428(7) 0.8102(8) 0.13279(13) 0.054(3) Uani 1 1 d . . . H39 H 0.7815 0.8418 0.1344 0.065 Uiso 1 1 calc R . . N1 N 0.7370(6) 0.6414(6) 0.15871(9) 0.051(2) Uani 1 1 d . . . N2 N 0.8205(5) 0.7472(5) 0.17461(9) 0.0330(18) Uani 1 1 d . . . N3 N 0.9325(5) 0.6824(6) 0.20283(9) 0.0397(19) Uani 1 1 d . . . H3 H 0.9694 0.6866 0.2123 0.048 Uiso 1 1 calc R . . Rh1 Rh 0.77643(5) 0.71810(6) 0.209916(9) 0.03754(19) Uani 1 1 d . . . B1 B 0.2538(7) 0.2518(6) 0.19270(10) 0.025(2) Uani 1 1 d . . . C40 C 0.2665(6) 0.3709(6) 0.19446(10) 0.0272(18) Uani 1 1 d . . . C41 C 0.2856(6) 0.4194(6) 0.20934(11) 0.030(2) Uani 1 1 d . . . H41 H 0.2976 0.3819 0.2188 0.035 Uiso 1 1 calc R . . C42 C 0.2877(6) 0.5212(6) 0.21064(10) 0.0312(19) Uani 1 1 d . . . C43 C 0.2686(6) 0.5811(6) 0.19713(10) 0.032(2) Uani 1 1 d . . . H43 H 0.2709 0.6495 0.1980 0.039 Uiso 1 1 calc R . . C44 C 0.2459(6) 0.5348(6) 0.18227(11) 0.039(2) Uani 1 1 d . A . C45 C 0.2471(6) 0.4329(6) 0.18106(10) 0.0320(19) Uani 1 1 d . . . H45 H 0.2343 0.4044 0.1708 0.038 Uiso 1 1 calc R . . C46 C 0.3117(8) 0.5704(7) 0.22685(13) 0.046(3) Uani 1 1 d . . . C47 C 0.2217(8) 0.5968(7) 0.16738(13) 0.045(3) Uani 1 1 d . . . C48 C 0.3328(6) 0.1906(6) 0.20475(8) 0.0197(17) Uani 1 1 d . . . C49 C 0.4255(5) 0.2286(7) 0.21014(10) 0.030(2) Uani 1 1 d . . . H49 H 0.4425 0.2929 0.2072 0.037 Uiso 1 1 calc R . . C50 C 0.4915(6) 0.1757(8) 0.21944(12) 0.042(3) Uani 1 1 d . . . C51 C 0.4694(7) 0.0773(8) 0.22429(11) 0.045(3) Uani 1 1 d . . . H51 H 0.5130 0.0415 0.2310 0.054 Uiso 1 1 calc R . . C52 C 0.3815(7) 0.0378(7) 0.21866(12) 0.044(3) Uani 1 1 d . B . C53 C 0.3155(6) 0.0914(6) 0.20878(11) 0.033(2) Uani 1 1 d . . . H53 H 0.2581 0.0605 0.2047 0.040 Uiso 1 1 calc R . . C54 C 0.5892(7) 0.2237(9) 0.22448(14) 0.056(3) Uani 1 1 d . . . C55 C 0.3580(10) -0.0704(10) 0.2223(2) 0.075(4) Uani 1 1 d . . . C56 C 0.2849(6) 0.2136(6) 0.17406(10) 0.032(2) Uani 1 1 d . . . C57 C 0.2352(7) 0.1395(6) 0.16519(10) 0.034(2) Uani 1 1 d . . . H57 H 0.1771 0.1129 0.1698 0.041 Uiso 1 1 calc R . . C58 C 0.2665(8) 0.1034(6) 0.15001(10) 0.041(2) Uani 1 1 d . . . C59 C 0.3527(8) 0.1425(8) 0.14292(12) 0.051(3) Uani 1 1 d . . . H59 H 0.3751 0.1192 0.1327 0.061 Uiso 1 1 calc R . . C60 C 0.4045(7) 0.2148(8) 0.15088(11) 0.043(2) Uani 1 1 d . . . C61 C 0.3708(7) 0.2473(7) 0.16599(10) 0.035(2) Uani 1 1 d . . . H61 H 0.4083 0.2958 0.1713 0.042 Uiso 1 1 calc R . . C62 C 0.2092(10) 0.0263(8) 0.14158(12) 0.061(3) Uani 1 1 d . . . C63 C 0.4940(10) 0.2594(11) 0.14251(18) 0.076(4) Uani 1 1 d . . . C64 C 0.1365(6) 0.2279(5) 0.19681(8) 0.0185(16) Uani 1 1 d . . . C65 C 0.0985(6) 0.1863(5) 0.21171(9) 0.0200(17) Uani 1 1 d . . . H65 H 0.1439 0.1665 0.2198 0.024 Uiso 1 1 calc R . . C66 C -0.0037(6) 0.1737(6) 0.21468(9) 0.0222(18) Uani 1 1 d . . . C67 C -0.0741(6) 0.2069(6) 0.20337(9) 0.0228(17) Uani 1 1 d . . . H67 H -0.1426 0.1993 0.2054 0.027 Uiso 1 1 calc R . . C68 C -0.0396(6) 0.2523(6) 0.18879(10) 0.0258(19) Uani 1 1 d . . . C69 C 0.0623(6) 0.2613(6) 0.18574(9) 0.0264(19) Uani 1 1 d . . . H69 H 0.0827 0.2909 0.1759 0.032 Uiso 1 1 calc R . . C70 C -0.0363(7) 0.1214(7) 0.22970(11) 0.036(2) Uani 1 1 d . . . C71 C -0.1120(6) 0.2887(8) 0.17598(11) 0.038(2) Uani 1 1 d . . . F1 F 0.3503(6) 0.6587(4) 0.22533(7) 0.075(2) Uani 1 1 d . . . F2 F 0.3770(6) 0.5183(5) 0.23627(7) 0.0719(19) Uani 1 1 d . . . F3 F 0.2314(6) 0.5775(5) 0.23666(8) 0.084(2) Uani 1 1 d . . . F4 F 0.144(2) 0.648(3) 0.1681(3) 0.145(12) Uani 0.50 1 d PU A 1 F5 F 0.222(3) 0.5474(10) 0.1528(2) 0.080(8) Uani 0.50 1 d PU A 1 F6 F 0.3014(17) 0.6594(19) 0.1637(2) 0.077(6) Uani 0.50 1 d PU A 1 F4A F 0.1319(18) 0.5704(14) 0.1622(3) 0.079(6) Uani 0.50 1 d PU A 2 F5A F 0.283(2) 0.582(2) 0.1558(3) 0.105(8) Uani 0.50 1 d PU A 2 F6A F 0.216(3) 0.6884(10) 0.1702(3) 0.092(7) Uani 0.50 1 d PU A 2 F7 F 0.6482(4) 0.2399(6) 0.21214(8) 0.083(2) Uani 1 1 d . . . F8 F 0.5726(5) 0.3103(7) 0.23165(11) 0.110(3) Uani 1 1 d . . . F9 F 0.6395(6) 0.1731(8) 0.23571(11) 0.117(4) Uani 1 1 d . . . F10 F 0.368(3) -0.0866(17) 0.2398(3) 0.106(9) Uani 0.50 1 d PU B 1 F11 F 0.2741(12) -0.1007(15) 0.2194(4) 0.086(7) Uani 0.50 1 d PU B 1 F12 F 0.4243(12) -0.1264(9) 0.2176(3) 0.064(4) Uani 0.50 1 d P B 1 F10A F 0.269(2) -0.0702(14) 0.2303(5) 0.143(16) Uani 0.50 1 d P B 2 F11A F 0.351(4) -0.1280(16) 0.2089(2) 0.198(19) Uani 0.50 1 d P B 2 F12A F 0.419(2) -0.102(2) 0.2328(4) 0.129(12) Uani 0.50 1 d P B 2 F13 F 0.2443(8) -0.0032(5) 0.12721(8) 0.118(3) Uani 1 1 d . . . F14 F 0.1149(8) 0.0495(7) 0.13941(17) 0.159(5) Uani 1 1 d . . . F15 F 0.1984(8) -0.0555(6) 0.15068(9) 0.119(4) Uani 1 1 d . . . F16 F 0.4773(7) 0.3373(10) 0.13521(18) 0.202(8) Uani 1 1 d . . . F17 F 0.5427(6) 0.1983(9) 0.13316(10) 0.128(4) Uani 1 1 d . . . F18 F 0.5655(6) 0.2823(7) 0.15354(10) 0.104(3) Uani 1 1 d . . . F19 F 0.0005(5) 0.1616(5) 0.24355(7) 0.0675(18) Uani 1 1 d . . . F20 F -0.0080(5) 0.0283(5) 0.22985(8) 0.0717(19) Uani 1 1 d . . . F21 F -0.1355(4) 0.1215(6) 0.23148(7) 0.068(2) Uani 1 1 d . . . F22 F -0.0926(4) 0.3827(4) 0.17150(6) 0.0490(14) Uani 1 1 d . . . F23 F -0.1076(4) 0.2393(5) 0.16181(6) 0.0589(17) Uani 1 1 d . . . F24 F -0.2068(4) 0.2871(6) 0.18097(7) 0.0678(19) Uani 1 1 d . . . C1' C 0.2663(8) 0.3717(6) 0.02733(10) 0.039(2) Uani 1 1 d . . . H1' H 0.2368 0.3224 0.0348 0.047 Uiso 1 1 calc R . . C2' C 0.3594(8) 0.4037(7) 0.03223(11) 0.043(3) Uani 1 1 d . . . H2' H 0.3833 0.3730 0.0425 0.051 Uiso 1 1 calc R . . C3' C 0.4442(8) 0.4419(8) 0.02107(12) 0.051(3) Uani 1 1 d . . . H3'1 H 0.4926 0.4772 0.0279 0.061 Uiso 1 1 calc R . . H3'2 H 0.4784 0.3862 0.0161 0.061 Uiso 1 1 calc R . . C4' C 0.4073(7) 0.5091(7) 0.00759(12) 0.048(3) Uani 1 1 d . . . H4'1 H 0.3888 0.4695 -0.0020 0.058 Uiso 1 1 calc R . . H4'2 H 0.4620 0.5521 0.0042 0.058 Uiso 1 1 calc R . . C5' C 0.3183(7) 0.5719(6) 0.01253(10) 0.031(2) Uani 1 1 d . . . H5' H 0.3306 0.6431 0.0122 0.037 Uiso 1 1 calc R . . C6' C 0.2197(7) 0.5449(5) 0.00985(9) 0.0257(19) Uani 1 1 d . . . H6' H 0.1739 0.6002 0.0078 0.031 Uiso 1 1 calc R . . C7' C 0.1874(8) 0.4481(6) 0.00202(10) 0.040(2) Uani 1 1 d . . . H7'1 H 0.1152 0.4413 0.0033 0.048 Uiso 1 1 calc R . . H7'2 H 0.2017 0.4509 -0.0098 0.048 Uiso 1 1 calc R . . C8' C 0.2370(9) 0.3579(6) 0.00910(10) 0.048(3) Uani 1 1 d . . . H8'1 H 0.2968 0.3428 0.0027 0.058 Uiso 1 1 calc R . . H8'2 H 0.1914 0.3023 0.0082 0.058 Uiso 1 1 calc R . . C9' C 0.2412(6) 0.4928(5) 0.06137(9) 0.0250(17) Uani 1 1 d . . . C10' C 0.1969(6) 0.4659(5) 0.08775(9) 0.0209(17) Uani 1 1 d . . . C11' C 0.2630(6) 0.5411(5) 0.08769(9) 0.0253(18) Uani 1 1 d . . . C12' C 0.3608(6) 0.6289(6) 0.06402(11) 0.032(2) Uani 1 1 d . . . H12' H 0.3955 0.5937 0.0551 0.038 Uiso 1 1 calc R . . C13' C 0.4447(6) 0.6654(7) 0.07533(10) 0.035(2) Uani 1 1 d . . . H13C H 0.4786 0.6101 0.0805 0.042 Uiso 1 1 calc R . . H13D H 0.4174 0.7073 0.0840 0.042 Uiso 1 1 calc R . . C14' C 0.5187(6) 0.7239(7) 0.06448(11) 0.040(2) Uani 1 1 d . . . H14C H 0.5738 0.7476 0.0713 0.048 Uiso 1 1 calc R . . H14D H 0.5464 0.6809 0.0560 0.048 Uiso 1 1 calc R . . C15' C 0.4670(7) 0.8102(6) 0.05634(12) 0.038(2) Uani 1 1 d . . . H15C H 0.4437 0.8556 0.0648 0.046 Uiso 1 1 calc R . . H15D H 0.5147 0.8451 0.0494 0.046 Uiso 1 1 calc R . . C16' C 0.3793(6) 0.7772(6) 0.04598(10) 0.0314(19) Uani 1 1 d . . . H16C H 0.4043 0.7415 0.0364 0.038 Uiso 1 1 calc R . . H16D H 0.3435 0.8348 0.0420 0.038 Uiso 1 1 calc R . . C17' C 0.3060(6) 0.7112(6) 0.05546(10) 0.0285(19) Uani 1 1 d . . . H17' H 0.2736 0.7516 0.0640 0.034 Uiso 1 1 calc R . . C18' C 0.1212(6) 0.6870(6) 0.05098(11) 0.031(2) Uani 1 1 d . . . H18C H 0.1105 0.6441 0.0605 0.037 Uiso 1 1 calc R . . H18D H 0.1130 0.7548 0.0546 0.037 Uiso 1 1 calc R . . C19' C 0.0469(6) 0.6639(6) 0.03775(10) 0.0243(18) Uani 1 1 d . . . C20' C 0.0179(6) 0.7388(6) 0.02641(12) 0.039(2) Uani 1 1 d . . . H20' H 0.0385 0.8036 0.0280 0.046 Uiso 1 1 calc R . . C21' C -0.0417(7) 0.7141(8) 0.01290(11) 0.043(2) Uani 1 1 d . . . H21' H -0.0613 0.7633 0.0055 0.052 Uiso 1 1 calc R . . C22' C -0.0724(7) 0.6197(8) 0.01013(11) 0.041(2) Uani 1 1 d . . . H22' H -0.1116 0.6051 0.0009 0.050 Uiso 1 1 calc R . . C23' C -0.0460(7) 0.5472(7) 0.02080(12) 0.039(2) Uani 1 1 d . . . H23' H -0.0671 0.4827 0.0189 0.047 Uiso 1 1 calc R . . C24' C 0.0128(6) 0.5691(6) 0.03462(9) 0.0274(19) Uani 1 1 d . . . H24' H 0.0298 0.5188 0.0420 0.033 Uiso 1 1 calc R . . C25' C 0.1193(7) 0.3541(6) 0.06514(11) 0.034(2) Uani 1 1 d . . . H25' H 0.1155 0.3629 0.0531 0.041 Uiso 1 1 calc R . . C26' C 0.1725(8) 0.2565(6) 0.06799(13) 0.050(3) Uani 1 1 d . . . H26D H 0.2420 0.2627 0.0649 0.075 Uiso 1 1 calc R . . H26E H 0.1415 0.2063 0.0613 0.075 Uiso 1 1 calc R . . H26F H 0.1677 0.2387 0.0795 0.075 Uiso 1 1 calc R . . C27' C 0.0145(7) 0.3553(7) 0.07123(11) 0.042(2) Uani 1 1 d . . . H27D H 0.0140 0.3456 0.0831 0.063 Uiso 1 1 calc R . . H27E H -0.0229 0.3034 0.0660 0.063 Uiso 1 1 calc R . . H27F H -0.0158 0.4177 0.0686 0.063 Uiso 1 1 calc R . . C28' C 0.2956(6) 0.6026(6) 0.10181(9) 0.0256(19) Uani 1 1 d . . . C29' C 0.2603(7) 0.6976(6) 0.10395(10) 0.037(2) Uani 1 1 d . . . H29' H 0.2110 0.7214 0.0968 0.044 Uiso 1 1 calc R . . C30' C 0.2947(8) 0.7564(8) 0.11596(13) 0.055(3) Uani 1 1 d . . . H30' H 0.2742 0.8219 0.1163 0.065 Uiso 1 1 calc R . . C31' C 0.3601(8) 0.7218(9) 0.12788(12) 0.056(3) Uani 1 1 d . . . H31' H 0.3818 0.7630 0.1364 0.068 Uiso 1 1 calc R . . C32' C 0.3934(8) 0.6247(10) 0.12710(12) 0.059(3) Uani 1 1 d . . . H32' H 0.4353 0.5995 0.1353 0.071 Uiso 1 1 calc R . . C33' C 0.3625(7) 0.5641(8) 0.11355(10) 0.042(2) Uani 1 1 d . . . H33' H 0.3865 0.5000 0.1125 0.050 Uiso 1 1 calc R . . C34' C 0.1437(6) 0.4260(6) 0.10297(10) 0.028(2) Uani 1 1 d . . . C35' C 0.0588(6) 0.4695(7) 0.10833(10) 0.035(2) Uani 1 1 d U . . H35' H 0.0303 0.5205 0.1022 0.042 Uiso 1 1 calc R . . C36' C 0.0130(8) 0.4381(8) 0.12322(13) 0.052(3) Uani 1 1 d . . . H36' H -0.0450 0.4687 0.1271 0.063 Uiso 1 1 calc R . . C37' C 0.0551(9) 0.3620(9) 0.13191(12) 0.059(3) Uani 1 1 d . . . H37' H 0.0251 0.3397 0.1417 0.070 Uiso 1 1 calc R . . C38' C 0.1415(11) 0.3187(9) 0.12621(15) 0.072(4) Uani 1 1 d . . . H38' H 0.1707 0.2677 0.1322 0.087 Uiso 1 1 calc R . . C39' C 0.1850(9) 0.3497(8) 0.11179(12) 0.055(3) Uani 1 1 d . . . H39' H 0.2431 0.3190 0.1079 0.066 Uiso 1 1 calc R . . F1' F 0.4415(5) 1.0741(9) 0.05088(11) 0.121(4) Uani 1 1 d . . . F2' F 0.4668(5) 1.0288(6) 0.02810(11) 0.098(3) Uani 1 1 d . . . F3' F 0.4344(5) 1.1745(5) 0.03173(17) 0.156(6) Uani 1 1 d . . . F4' F 0.8615(5) 1.3034(4) 0.01853(8) 0.074(2) Uani 1 1 d . . . F5' F 0.8239(5) 1.3723(4) 0.04109(6) 0.0594(17) Uani 1 1 d . . . F6' F 0.7235(6) 1.3786(5) 0.02093(10) 0.095(3) Uani 1 1 d . . . F7' F 1.2783(4) 0.9456(6) 0.07848(8) 0.084(2) Uani 1 1 d . . . F8' F 1.1974(6) 1.0525(5) 0.09123(8) 0.080(2) Uani 1 1 d . . . F9' F 1.1534(5) 0.9066(6) 0.09278(11) 0.108(3) Uani 1 1 d . . . F10' F 1.2278(4) 1.0853(6) 0.02323(7) 0.075(2) Uani 1 1 d . . . F11' F 1.1449(6) 0.9660(6) 0.01287(8) 0.095(3) Uani 1 1 d . . . F12' F 1.0806(5) 1.1093(6) 0.01360(7) 0.070(2) Uani 1 1 d . . . F13' F 0.9473(4) 0.6287(4) 0.07748(6) 0.0445(13) Uani 1 1 d . . . F14' F 0.8023(5) 0.6309(5) 0.08807(8) 0.088(3) Uani 1 1 d . . . F15' F 0.8364(5) 0.5301(4) 0.06879(9) 0.077(2) Uani 1 1 d . . . F16' F 0.5878(4) 0.7590(7) 0.02063(8) 0.101(3) Uani 1 1 d . . . F17' F 0.6555(7) 0.6169(5) 0.02040(7) 0.102(3) Uani 1 1 d . . . F18' F 0.7188(4) 0.7362(4) 0.00694(6) 0.0426(13) Uani 1 1 d . . . F19' F 0.8575(7) 1.2539(7) 0.10782(10) 0.103(3) Uani 1 1 d . . . F20' F 0.9432(7) 1.1427(9) 0.11801(16) 0.185(7) Uani 1 1 d . . . F21' F 0.8068(7) 1.1876(6) 0.12938(8) 0.102(3) Uani 1 1 d . . . F22' F 0.5954(6) 0.8221(8) 0.10793(17) 0.154(5) Uani 1 1 d . . . F23' F 0.5039(5) 0.9156(7) 0.09709(10) 0.101(3) Uani 1 1 d . . . F24' F 0.5489(9) 0.9430(11) 0.12126(12) 0.207(8) Uani 1 1 d . . . N1' N 0.1829(5) 0.4360(4) 0.07151(7) 0.0226(15) Uani 1 1 d . . . N2' N 0.2914(5) 0.5559(5) 0.07110(8) 0.0257(16) Uani 1 1 d . . . N3' N 0.2249(5) 0.6721(5) 0.04422(9) 0.0294(16) Uani 1 1 d . . . H3' H 0.224(6) 0.713(6) 0.0353(10) 0.035 Uiso 1 1 d . . . Rh1' Rh 0.25283(5) 0.51808(4) 0.036125(7) 0.02676(16) Uani 1 1 d . . . B1' B 0.8246(6) 0.9870(7) 0.05915(11) 0.023(2) Uani 1 1 d . . . C40' C 0.7589(6) 1.0667(5) 0.04878(8) 0.0220(16) Uani 1 1 d . . . C41' C 0.6557(6) 1.0537(6) 0.04687(10) 0.0243(18) Uani 1 1 d . . . H41' H 0.6259 0.9967 0.0510 0.029 Uiso 1 1 calc R . . C42' C 0.5950(6) 1.1243(6) 0.03883(11) 0.033(2) Uani 1 1 d . . . C43' C 0.6365(6) 1.2105(6) 0.03305(10) 0.032(2) Uani 1 1 d . . . H43' H 0.5962 1.2576 0.0279 0.038 Uiso 1 1 calc R . . C44' C 0.7376(7) 1.2266(6) 0.03487(10) 0.0338(19) Uani 1 1 d . . . C45' C 0.7969(6) 1.1564(6) 0.04254(9) 0.0246(19) Uani 1 1 d . . . H45' H 0.8653 1.1690 0.0436 0.029 Uiso 1 1 calc R . . C46' C 0.4847(6) 1.1052(7) 0.03676(14) 0.043(2) Uani 1 1 d . . . C47' C 0.7850(6) 1.3193(6) 0.02879(11) 0.034(2) Uani 1 1 d . . . C48' C 0.9478(6) 0.9975(5) 0.05695(9) 0.0228(18) Uani 1 1 d . . . C49' C 1.0158(5) 0.9820(5) 0.07002(9) 0.0209(17) Uani 1 1 d . . . H49' H 0.9910 0.9683 0.0806 0.025 Uiso 1 1 calc R . . C50' C 1.1194(6) 0.9867(6) 0.06766(9) 0.0214(17) Uani 1 1 d . . . C51' C 1.1604(6) 1.0067(6) 0.05254(10) 0.030(2) Uani 1 1 d . . . H51' H 1.2297 1.0091 0.0510 0.036 Uiso 1 1 calc R . . C52' C 1.0953(6) 1.0232(6) 0.03977(10) 0.0299(19) Uani 1 1 d . . . C53' C 0.9919(6) 1.0156(6) 0.04173(9) 0.0243(18) Uani 1 1 d . . . H53' H 0.9508 1.0230 0.0325 0.029 Uiso 1 1 calc R . . C54' C 1.1864(6) 0.9736(7) 0.08293(13) 0.037(2) Uani 1 1 d . . . C55' C 1.1377(7) 1.0448(8) 0.02210(11) 0.044(3) Uani 1 1 d . . . C56' C 0.8004(5) 0.8723(5) 0.05405(8) 0.0163(16) Uani 1 1 d . . . C57' C 0.8325(6) 0.7961(6) 0.06459(10) 0.0256(18) Uani 1 1 d . . . H57' H 0.8670 0.8132 0.0742 0.031 Uiso 1 1 calc R . . C58' C 0.8159(5) 0.6966(6) 0.06149(9) 0.0216(18) Uani 1 1 d . . . C59' C 0.7665(6) 0.6671(6) 0.04733(10) 0.0301(19) Uani 1 1 d . . . H59' H 0.7553 0.6006 0.0451 0.036 Uiso 1 1 calc R . . C60' C 0.7331(6) 0.7413(6) 0.03609(11) 0.033(2) Uani 1 1 d U . . C61' C 0.7535(6) 0.8397(5) 0.03959(7) 0.0181(16) Uani 1 1 d . . . H61' H 0.7346 0.8868 0.0318 0.022 Uiso 1 1 calc R . . C62' C 0.8498(7) 0.6225(7) 0.07361(13) 0.041(2) Uani 1 1 d . . . C63' C 0.6754(6) 0.7114(7) 0.02092(11) 0.038(2) Uani 1 1 d . . . C64' C 0.7892(6) 1.0023(5) 0.07847(9) 0.0250(18) Uani 1 1 d . . . C65' C 0.8317(7) 1.0761(7) 0.08872(11) 0.034(2) Uani 1 1 d . . . H65' H 0.8841 1.1144 0.0846 0.041 Uiso 1 1 calc R . . C66' C 0.7971(7) 1.0931(7) 0.10495(11) 0.039(2) Uani 1 1 d . . . C67' C 0.7171(8) 1.0408(8) 0.11086(10) 0.052(3) Uani 1 1 d U . . H67' H 0.6942 1.0524 0.1216 0.062 Uiso 1 1 calc R . . C68' C 0.6702(6) 0.9720(7) 0.10128(10) 0.036(2) Uani 1 1 d . . . C69' C 0.7062(6) 0.9552(7) 0.08531(11) 0.036(2) Uani 1 1 d . . . H69' H 0.6725 0.9093 0.0788 0.043 Uiso 1 1 calc R . . C70' C 0.8501(10) 1.1673(11) 0.11569(17) 0.073(4) Uani 1 1 d . . . C71' C 0.5805(8) 0.9157(9) 0.10668(11) 0.050(3) Uani 1 1 d . . . C72 C 0.5029(11) 0.2564(12) 0.08408(17) 0.084(4) Uani 1 1 d . . . C73 C 0.5998(15) 0.2394(14) 0.08268(17) 0.106(5) Uani 1 1 d . . . H73 H 0.6258 0.1800 0.0866 0.127 Uiso 1 1 calc R . . C74 C 0.6623(14) 0.3059(13) 0.0758(2) 0.100(5) Uani 1 1 d . . . H74 H 0.7313 0.2943 0.0760 0.120 Uiso 1 1 calc R . . C75 C 0.6242(11) 0.3958(13) 0.0680(2) 0.094(5) Uani 1 1 d . . . H75 H 0.6654 0.4392 0.0622 0.113 Uiso 1 1 calc R . . C76 C 0.5331(17) 0.4097(12) 0.0697(3) 0.129(8) Uani 1 1 d . . . H76 H 0.5042 0.4668 0.0654 0.155 Uiso 1 1 calc R . . C77 C 0.4708(14) 0.3390(13) 0.07818(19) 0.094(5) Uani 1 1 d . . . H77 H 0.4030 0.3539 0.0795 0.113 Uiso 1 1 calc R . . C78 C 0.4336(10) 0.1766(11) 0.09225(18) 0.089(4) Uani 1 1 d . . . H78A H 0.3838 0.2085 0.0990 0.133 Uiso 1 1 calc R . . H78B H 0.4736 0.1336 0.0990 0.133 Uiso 1 1 calc R . . H78C H 0.4010 0.1389 0.0837 0.133 Uiso 1 1 calc R . . C79 C 0.6220(11) 1.0171(14) 0.1723(2) 0.131(14) Uani 0.50 1 d PGU . . C80 C 0.5279(13) 1.0319(11) 0.17947(18) 0.060(6) Uani 0.50 1 d PGU . . H80 H 0.5172 1.0856 0.1864 0.072 Uiso 0.50 1 calc PR . . C81 C 0.4500(11) 0.9664(14) 0.1762(2) 0.165(16) Uani 0.50 1 d PGU . . H81 H 0.3871 0.9763 0.1810 0.198 Uiso 0.50 1 calc PR . . C82 C 0.4661(15) 0.8862(13) 0.1658(2) 0.088(9) Uani 0.50 1 d PGU . . H82 H 0.4139 0.8423 0.1636 0.105 Uiso 0.50 1 calc PR . . C83 C 0.5601(18) 0.8713(13) 0.1586(2) 0.135(15) Uani 0.50 1 d PGU . . H83 H 0.5708 0.8176 0.1517 0.162 Uiso 0.50 1 calc PR . . C84 C 0.6380(13) 0.9368(16) 0.1619(2) 0.108(12) Uani 0.50 1 d PGU . . H84 H 0.7009 0.9269 0.1572 0.129 Uiso 0.50 1 calc PR . . C85 C 0.6953(18) 1.057(2) 0.1750(4) 0.087(9) Uani 0.50 1 d PU . . H85A H 0.6816 1.1183 0.1804 0.131 Uiso 0.50 1 calc PR . . H85B H 0.7298 1.0692 0.1647 0.131 Uiso 0.50 1 calc PR . . H85C H 0.7368 1.0166 0.1820 0.131 Uiso 0.50 1 calc PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.036(5) 0.081(9) 0.051(6) -0.009(6) 0.022(5) 0.017(6) C2 0.067(7) 0.066(8) 0.071(8) 0.015(7) 0.020(7) 0.015(6) C3 0.094(10) 0.051(7) 0.107(11) -0.038(7) 0.055(9) 0.010(7) C4 0.104(11) 0.074(8) 0.064(8) -0.039(7) 0.049(8) -0.020(8) C5 0.046(6) 0.083(9) 0.053(7) -0.040(7) 0.001(5) -0.016(7) C6 0.061(7) 0.069(8) 0.019(5) -0.010(5) -0.005(5) 0.004(6) C7 0.046(6) 0.094(9) 0.020(5) -0.010(5) 0.007(4) -0.004(6) C8 0.050(7) 0.105(10) 0.073(8) -0.034(8) 0.046(6) -0.032(8) C9 0.003(3) 0.034(5) 0.013(4) 0.008(3) 0.004(3) -0.001(3) C10 0.024(4) 0.026(4) 0.029(4) 0.000(4) -0.001(3) -0.002(4) C11 0.021(4) 0.048(5) 0.041(5) 0.006(4) 0.001(4) 0.002(5) C12 0.032(5) 0.032(5) 0.059(6) -0.011(5) 0.006(5) 0.000(4) C13 0.049(6) 0.044(6) 0.058(7) -0.010(5) 0.010(5) -0.017(5) C14 0.057(7) 0.049(7) 0.094(9) 0.000(7) 0.025(7) -0.023(6) C15 0.057(8) 0.078(9) 0.077(8) -0.029(7) 0.022(7) -0.056(7) C16 0.042(6) 0.079(8) 0.054(6) -0.030(6) 0.004(5) -0.018(6) C17 0.041(6) 0.043(6) 0.081(8) -0.033(6) 0.008(5) -0.017(5) C18 0.024(5) 0.037(5) 0.052(6) -0.028(5) -0.013(4) 0.012(4) C19 0.036(5) 0.031(5) 0.022(4) -0.014(4) 0.004(4) 0.006(4) C20 0.047(6) 0.048(6) 0.047(6) -0.011(5) -0.002(5) -0.006(5) C21 0.089(10) 0.053(8) 0.071(9) -0.006(7) -0.027(8) 0.003(7) C22 0.163(16) 0.041(7) 0.043(7) -0.019(6) 0.026(9) -0.030(9) C23 0.072(8) 0.058(8) 0.059(7) -0.012(6) 0.021(7) -0.031(7) C24 0.043(6) 0.047(7) 0.098(9) -0.015(7) 0.008(6) 0.002(5) C25 0.041(6) 0.086(9) 0.019(5) 0.009(5) 0.001(4) -0.008(6) C26 0.009(5) 0.224(18) 0.055(7) 0.053(9) 0.000(5) -0.010(7) C27 0.116(12) 0.075(10) 0.079(9) -0.003(8) 0.029(8) -0.058(9) C28 0.010(4) 0.068(7) 0.019(4) 0.006(4) -0.001(3) -0.006(4) C29 0.033(5) 0.055(6) 0.051(6) -0.005(5) 0.000(5) 0.005(5) C30 0.050(7) 0.065(7) 0.064(7) -0.011(6) 0.008(6) -0.008(6) C31 0.070(8) 0.088(10) 0.036(6) -0.023(7) 0.000(6) -0.009(8) C32 0.057(7) 0.097(10) 0.022(5) 0.016(6) -0.006(5) -0.021(7) C33 0.032(6) 0.086(9) 0.065(8) -0.007(7) -0.008(5) -0.002(6) C34 0.030(5) 0.040(6) 0.038(5) 0.007(4) -0.003(4) -0.010(4) C35 0.032(5) 0.059(7) 0.030(5) -0.001(5) 0.008(4) -0.006(5) C36 0.047(6) 0.055(7) 0.062(7) -0.001(6) 0.030(5) 0.005(6) C37 0.065(7) 0.059(7) 0.043(6) 0.017(6) 0.028(5) -0.008(6) C38 0.073(9) 0.116(12) 0.056(7) 0.057(8) 0.033(7) 0.021(8) C39 0.035(6) 0.067(8) 0.059(7) 0.031(6) 0.004(5) -0.007(5) N1 0.039(5) 0.066(6) 0.049(5) 0.019(4) -0.005(4) 0.010(5) N2 0.023(4) 0.036(4) 0.040(4) -0.010(3) 0.006(3) -0.007(3) N3 0.034(4) 0.047(5) 0.038(4) -0.008(4) -0.010(3) 0.006(4) Rh1 0.0287(4) 0.0489(4) 0.0351(4) -0.0104(3) 0.0077(3) 0.0023(3) B1 0.023(5) 0.026(5) 0.027(5) -0.005(4) 0.005(4) 0.006(4) C40 0.014(4) 0.032(4) 0.036(5) -0.004(4) 0.008(4) 0.000(4) C41 0.030(5) 0.022(4) 0.037(5) 0.001(4) 0.016(4) 0.000(4) C42 0.023(4) 0.035(5) 0.036(5) 0.007(4) -0.001(4) -0.003(4) C43 0.026(5) 0.022(4) 0.049(5) 0.002(4) 0.011(4) -0.007(4) C44 0.021(5) 0.043(6) 0.054(6) 0.008(4) 0.003(4) 0.017(5) C45 0.025(5) 0.041(5) 0.030(4) -0.007(4) 0.003(4) -0.008(4) C46 0.049(6) 0.040(6) 0.049(6) -0.015(5) -0.001(5) -0.004(5) C47 0.037(6) 0.045(7) 0.053(7) 0.013(5) 0.015(6) 0.016(5) C48 0.024(4) 0.028(5) 0.007(4) 0.005(3) 0.004(3) 0.001(3) C49 0.026(4) 0.038(5) 0.027(4) 0.004(4) 0.009(4) -0.004(4) C50 0.014(4) 0.066(7) 0.046(6) -0.011(5) 0.003(4) 0.012(4) C51 0.045(6) 0.055(7) 0.034(5) 0.016(5) -0.002(5) 0.021(5) C52 0.028(5) 0.044(6) 0.059(6) 0.024(5) 0.002(5) 0.004(5) C53 0.017(4) 0.041(6) 0.041(5) 0.007(4) -0.002(4) -0.002(4) C54 0.026(5) 0.077(8) 0.065(7) 0.004(7) 0.012(5) 0.002(6) C55 0.039(8) 0.064(9) 0.121(12) 0.050(9) -0.003(8) 0.008(7) C56 0.032(5) 0.030(5) 0.036(5) -0.014(4) 0.001(4) 0.004(4) C57 0.041(6) 0.029(4) 0.032(4) -0.004(4) 0.015(4) -0.001(4) C58 0.065(7) 0.025(5) 0.034(5) -0.005(4) 0.000(5) 0.016(5) C59 0.068(7) 0.051(7) 0.033(5) 0.002(5) 0.032(5) 0.021(6) C60 0.045(5) 0.053(6) 0.033(5) -0.001(5) 0.010(4) -0.011(5) C61 0.038(5) 0.043(6) 0.025(5) 0.000(4) 0.013(4) -0.004(4) C62 0.107(10) 0.041(6) 0.036(6) -0.012(5) 0.012(6) -0.002(7) C63 0.063(8) 0.088(10) 0.076(9) -0.023(8) 0.046(8) -0.009(7) C64 0.031(4) 0.011(4) 0.014(4) -0.002(3) 0.000(3) 0.003(3) C65 0.029(4) 0.020(4) 0.010(4) 0.001(3) 0.000(3) 0.004(3) C66 0.031(4) 0.023(4) 0.013(4) 0.006(3) 0.001(3) -0.003(4) C67 0.026(4) 0.027(4) 0.015(4) 0.005(3) 0.000(3) 0.001(4) C68 0.022(4) 0.031(5) 0.025(4) -0.003(4) -0.002(3) -0.005(3) C69 0.043(5) 0.019(4) 0.017(4) -0.008(3) 0.007(4) 0.000(4) C70 0.028(5) 0.047(6) 0.032(5) 0.003(5) 0.007(4) -0.005(4) C71 0.028(5) 0.054(6) 0.033(5) -0.004(5) -0.002(4) -0.005(5) F1 0.127(6) 0.045(4) 0.052(4) -0.003(3) -0.003(4) -0.045(4) F2 0.109(5) 0.057(4) 0.050(3) -0.007(3) -0.022(4) -0.009(4) F3 0.097(5) 0.101(5) 0.055(4) -0.042(4) 0.039(4) -0.036(5) F4 0.106(17) 0.23(3) 0.096(16) 0.103(19) 0.081(14) 0.134(19) F5 0.18(2) 0.024(6) 0.035(8) 0.006(5) -0.056(13) -0.033(11) F6 0.097(13) 0.093(13) 0.041(9) 0.056(9) -0.035(9) -0.064(12) F4A 0.109(15) 0.068(11) 0.059(11) 0.021(8) -0.057(12) 0.005(10) F5A 0.121(18) 0.14(2) 0.056(14) 0.063(14) 0.041(13) 0.050(16) F6A 0.143(19) 0.020(7) 0.112(15) 0.022(7) -0.061(16) -0.011(10) F7 0.039(3) 0.157(7) 0.053(4) -0.018(4) 0.006(3) -0.038(4) F8 0.055(4) 0.142(8) 0.133(7) -0.097(6) -0.011(4) -0.003(5) F9 0.062(5) 0.166(9) 0.123(7) 0.065(7) -0.059(5) -0.032(5) F10 0.17(3) 0.074(11) 0.073(12) 0.061(10) 0.032(14) 0.009(16) F11 0.025(9) 0.041(11) 0.19(2) 0.072(13) -0.017(10) -0.004(7) F12 0.070(10) 0.021(6) 0.102(13) -0.012(8) 0.028(9) -0.002(7) F10A 0.12(2) 0.038(10) 0.27(4) -0.004(14) 0.15(3) 0.006(11) F11A 0.46(6) 0.062(13) 0.070(13) -0.006(11) -0.06(2) -0.12(2) F12A 0.086(17) 0.16(3) 0.14(3) 0.10(3) -0.017(17) -0.015(16) F13 0.202(9) 0.093(5) 0.059(4) -0.047(4) 0.045(6) -0.069(7) F14 0.114(8) 0.103(8) 0.259(14) -0.094(9) -0.077(9) 0.006(6) F15 0.213(11) 0.072(5) 0.072(5) -0.011(4) 0.000(6) -0.061(6) F16 0.098(7) 0.216(13) 0.291(16) 0.207(13) 0.104(9) 0.046(8) F17 0.084(5) 0.214(11) 0.085(6) -0.052(7) 0.057(5) -0.019(7) F18 0.087(5) 0.141(8) 0.086(6) -0.014(6) 0.041(5) -0.045(6) F19 0.085(5) 0.087(5) 0.031(3) 0.013(3) -0.002(3) -0.023(4) F20 0.104(5) 0.056(4) 0.056(4) 0.032(3) 0.030(4) 0.013(4) F21 0.037(3) 0.114(6) 0.054(4) 0.037(4) 0.011(3) -0.006(3) F22 0.052(3) 0.052(4) 0.043(3) 0.018(3) -0.018(3) 0.006(3) F23 0.071(4) 0.086(5) 0.019(3) 0.002(3) -0.016(3) -0.014(3) F24 0.031(3) 0.120(6) 0.053(3) 0.033(4) -0.003(3) 0.003(3) C1' 0.073(7) 0.021(4) 0.024(4) 0.007(3) 0.011(5) 0.006(5) C2' 0.055(6) 0.040(6) 0.034(5) 0.009(4) 0.014(5) 0.025(5) C3' 0.060(7) 0.059(7) 0.033(5) 0.001(5) 0.020(5) 0.034(6) C4' 0.053(6) 0.044(6) 0.047(6) 0.001(5) 0.021(5) 0.027(5) C5' 0.041(6) 0.022(5) 0.030(5) 0.004(4) 0.007(4) 0.001(4) C6' 0.049(6) 0.017(4) 0.012(4) 0.002(3) 0.000(4) 0.008(4) C7' 0.066(7) 0.031(5) 0.022(5) -0.006(4) -0.001(4) 0.007(5) C8' 0.084(8) 0.029(5) 0.030(5) -0.007(4) 0.012(5) 0.013(6) C9' 0.032(4) 0.006(3) 0.037(4) 0.000(3) 0.006(4) 0.012(4) C10' 0.028(4) 0.012(4) 0.023(4) -0.002(3) 0.000(3) 0.013(3) C11' 0.023(4) 0.015(4) 0.038(5) 0.001(3) 0.000(4) -0.006(4) C12' 0.023(4) 0.027(5) 0.044(5) -0.007(4) 0.009(4) -0.003(4) C13' 0.025(5) 0.058(6) 0.023(4) -0.011(4) 0.010(4) -0.008(4) C14' 0.023(4) 0.050(6) 0.048(6) -0.013(5) 0.010(4) -0.018(5) C15' 0.040(5) 0.024(5) 0.050(6) -0.008(4) 0.021(4) -0.005(4) C16' 0.033(5) 0.029(5) 0.032(5) -0.005(4) 0.014(4) -0.011(4) C17' 0.034(5) 0.026(4) 0.025(4) 0.004(4) 0.004(3) 0.001(4) C18' 0.032(5) 0.025(5) 0.036(5) -0.010(4) 0.004(4) -0.004(4) C19' 0.029(4) 0.020(4) 0.023(4) -0.003(4) 0.006(4) 0.001(3) C20' 0.032(5) 0.014(4) 0.070(7) 0.015(4) 0.016(5) 0.001(4) C21' 0.045(6) 0.056(7) 0.029(5) 0.018(5) 0.002(4) -0.002(5) C22' 0.032(5) 0.059(7) 0.033(5) -0.002(5) 0.002(4) 0.004(5) C23' 0.036(5) 0.031(5) 0.051(6) -0.019(5) 0.011(5) -0.012(4) C24' 0.030(4) 0.039(5) 0.013(4) 0.007(4) 0.006(4) 0.001(4) C25' 0.060(6) 0.011(4) 0.031(5) 0.000(4) -0.015(4) -0.004(4) C26' 0.075(7) 0.019(5) 0.056(6) 0.003(4) -0.003(6) 0.007(5) C27' 0.052(6) 0.049(6) 0.024(5) -0.003(4) -0.006(4) -0.022(5) C28' 0.019(4) 0.038(5) 0.020(4) -0.002(4) 0.003(3) -0.009(4) C29' 0.044(5) 0.038(5) 0.029(4) -0.004(4) 0.000(4) -0.005(5) C30' 0.063(7) 0.049(6) 0.052(6) -0.022(5) 0.023(6) -0.024(5) C31' 0.061(7) 0.072(8) 0.036(6) -0.032(6) 0.020(5) -0.042(7) C32' 0.046(6) 0.108(11) 0.024(5) -0.005(6) -0.009(5) -0.010(7) C33' 0.047(6) 0.064(7) 0.015(4) -0.001(4) 0.013(4) -0.004(5) C34' 0.037(5) 0.022(5) 0.025(4) 0.004(4) 0.003(4) -0.011(4) C35' 0.040(5) 0.045(5) 0.019(4) 0.012(4) 0.023(4) -0.006(5) C36' 0.048(6) 0.066(7) 0.043(6) 0.004(6) 0.003(5) -0.010(6) C37' 0.077(8) 0.071(8) 0.028(5) 0.008(6) 0.012(6) -0.041(7) C38' 0.096(10) 0.057(8) 0.064(8) 0.032(6) 0.010(7) 0.009(7) C39' 0.073(8) 0.052(7) 0.039(6) 0.024(5) 0.014(5) 0.020(6) F1' 0.042(4) 0.229(11) 0.092(6) -0.002(7) 0.018(4) -0.023(5) F2' 0.044(4) 0.087(5) 0.162(8) -0.058(6) -0.023(4) -0.009(4) F3' 0.039(4) 0.057(5) 0.372(17) 0.080(7) -0.071(7) -0.010(3) F4' 0.100(5) 0.043(4) 0.081(5) -0.009(3) 0.038(4) -0.028(4) F5' 0.105(5) 0.040(3) 0.033(3) -0.002(3) 0.006(3) -0.040(3) F6' 0.087(5) 0.056(4) 0.143(7) 0.056(4) -0.058(5) -0.022(4) F7' 0.036(4) 0.141(7) 0.076(4) -0.021(4) -0.012(3) 0.032(4) F8' 0.133(6) 0.050(4) 0.056(4) -0.009(3) -0.062(4) 0.015(4) F9' 0.065(5) 0.122(7) 0.137(7) 0.096(6) -0.047(5) -0.050(5) F10' 0.038(4) 0.135(6) 0.051(3) -0.001(4) 0.009(3) -0.039(4) F11' 0.144(7) 0.095(5) 0.045(4) -0.042(4) 0.056(4) -0.041(5) F12' 0.058(4) 0.111(6) 0.042(3) 0.028(4) 0.000(3) -0.013(4) F13' 0.040(3) 0.053(3) 0.040(3) 0.022(3) -0.011(2) -0.008(3) F14' 0.094(5) 0.098(5) 0.071(4) 0.063(4) 0.055(4) 0.054(4) F15' 0.084(5) 0.023(3) 0.124(6) 0.019(3) -0.039(4) -0.007(3) F16' 0.031(3) 0.206(9) 0.066(4) -0.082(5) -0.015(3) 0.019(4) F17' 0.208(9) 0.058(4) 0.040(4) 0.003(3) -0.038(5) -0.086(5) F18' 0.043(3) 0.053(3) 0.032(3) 0.009(2) -0.001(2) -0.013(3) F19' 0.141(8) 0.101(7) 0.068(5) -0.043(5) 0.008(5) -0.053(6) F20' 0.104(7) 0.200(11) 0.253(13) -0.186(11) -0.113(8) 0.065(7) F21' 0.172(8) 0.098(6) 0.035(4) -0.026(4) -0.013(4) 0.007(6) F22' 0.076(6) 0.126(8) 0.260(14) 0.117(9) 0.061(7) 0.012(6) F23' 0.050(4) 0.151(8) 0.102(6) 0.063(6) -0.001(4) -0.030(5) F24' 0.195(11) 0.323(17) 0.102(7) -0.124(9) 0.118(8) -0.169(12) N1' 0.040(4) 0.011(3) 0.017(3) 0.001(3) 0.007(3) 0.000(3) N2' 0.023(4) 0.031(4) 0.023(4) -0.002(3) 0.012(3) 0.000(3) N3' 0.024(4) 0.029(4) 0.035(4) -0.002(3) 0.014(3) 0.001(3) Rh1' 0.0332(3) 0.0217(3) 0.0255(3) 0.0017(3) 0.0080(3) 0.0039(3) B1' 0.017(4) 0.027(5) 0.026(5) 0.009(4) 0.002(4) 0.000(4) C40' 0.027(4) 0.023(4) 0.016(4) -0.005(3) 0.004(4) -0.007(4) C41' 0.027(5) 0.019(4) 0.027(4) -0.004(3) 0.002(4) 0.005(4) C42' 0.025(5) 0.031(5) 0.044(5) -0.003(4) 0.004(4) -0.002(4) C43' 0.041(5) 0.014(4) 0.041(5) -0.009(4) -0.007(4) 0.008(4) C44' 0.041(5) 0.030(4) 0.031(4) 0.001(4) -0.013(4) -0.014(4) C45' 0.015(4) 0.030(5) 0.030(4) -0.004(4) -0.004(3) -0.008(4) C46' 0.025(5) 0.033(5) 0.071(7) -0.003(5) -0.006(5) 0.008(4) C47' 0.031(5) 0.021(5) 0.052(5) -0.009(4) -0.014(4) 0.001(4) C48' 0.025(4) 0.017(4) 0.026(4) -0.008(3) 0.002(3) 0.001(3) C49' 0.029(4) 0.010(4) 0.023(4) 0.001(3) 0.003(3) -0.003(3) C50' 0.023(4) 0.018(4) 0.023(4) -0.003(3) -0.009(3) -0.005(3) C51' 0.026(4) 0.020(5) 0.044(5) -0.009(4) -0.001(4) 0.002(4) C52' 0.029(5) 0.028(4) 0.033(5) -0.007(4) 0.010(4) -0.008(4) C53' 0.033(5) 0.027(4) 0.013(4) -0.010(3) -0.006(3) -0.003(4) C54' 0.023(5) 0.019(5) 0.068(7) 0.018(5) -0.003(4) -0.005(4) C55' 0.039(6) 0.065(7) 0.029(5) -0.013(5) 0.013(4) -0.023(5) C56' 0.016(4) 0.020(4) 0.013(4) -0.001(3) 0.007(3) -0.001(3) C57' 0.026(4) 0.026(5) 0.025(4) -0.007(4) -0.001(3) -0.008(4) C58' 0.021(4) 0.023(4) 0.021(4) 0.006(3) 0.004(3) 0.003(3) C59' 0.025(5) 0.026(4) 0.039(5) -0.013(4) 0.014(4) -0.003(4) C60' 0.019(4) 0.040(5) 0.040(4) -0.005(4) 0.024(4) -0.014(4) C61' 0.021(4) 0.033(4) 0.001(3) 0.003(3) -0.002(3) -0.009(4) C62' 0.027(5) 0.032(6) 0.063(7) 0.005(5) 0.017(5) 0.004(4) C63' 0.033(5) 0.041(6) 0.040(5) -0.008(5) 0.008(4) -0.016(5) C64' 0.028(4) 0.020(4) 0.027(4) 0.009(3) 0.001(3) 0.000(3) C65' 0.029(5) 0.040(5) 0.034(5) -0.019(4) -0.007(4) 0.005(4) C66' 0.031(5) 0.051(6) 0.035(5) -0.022(5) -0.001(4) 0.023(5) C67' 0.065(7) 0.071(7) 0.019(4) -0.026(5) -0.008(5) 0.056(6) C68' 0.030(5) 0.054(6) 0.024(5) 0.009(5) 0.003(4) 0.012(5) C69' 0.027(5) 0.036(5) 0.044(5) -0.001(4) -0.002(4) 0.009(4) C70' 0.064(8) 0.086(10) 0.068(9) -0.044(8) -0.010(7) 0.013(8) C71' 0.048(7) 0.081(9) 0.022(5) 0.022(5) 0.013(5) 0.019(6) C72 0.077(10) 0.106(13) 0.070(9) -0.030(9) -0.029(8) 0.028(9) C73 0.131(15) 0.123(15) 0.063(9) 0.011(9) -0.012(9) 0.025(13) C74 0.121(13) 0.090(12) 0.090(11) 0.008(9) 0.000(10) -0.024(11) C75 0.059(9) 0.106(13) 0.117(13) -0.058(11) 0.006(9) -0.030(9) C76 0.137(18) 0.053(10) 0.20(2) -0.039(12) -0.068(16) 0.015(11) C77 0.111(13) 0.081(11) 0.090(11) 0.010(9) -0.012(9) -0.001(11) C78 0.075(9) 0.096(11) 0.095(10) 0.008(9) 0.007(8) -0.002(8) C79 0.12(3) 0.15(3) 0.13(3) 0.08(2) -0.07(2) 0.04(2) C80 0.026(10) 0.073(16) 0.080(16) 0.033(13) -0.014(10) 0.004(11) C81 0.28(3) 0.18(3) 0.040(15) 0.036(18) -0.07(2) 0.07(3) C82 0.14(3) 0.068(17) 0.052(15) -0.006(13) 0.006(16) 0.042(17) C83 0.07(2) 0.22(4) 0.11(2) 0.08(3) 0.022(19) 0.01(2) C84 0.17(3) 0.09(2) 0.055(15) -0.033(15) 0.009(18) 0.08(2) C85 0.045(14) 0.070(17) 0.15(2) 0.055(17) 0.017(15) -0.012(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.399(16) . ? C1 C8 1.528(15) . ? C1 Rh1 2.143(9) . ? C1 H1 0.9800 . ? C2 C3 1.500(17) . ? C2 Rh1 2.073(11) . ? C2 H2 0.9800 . ? C3 C4 1.607(19) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 C5 1.480(17) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C6 1.347(16) . ? C5 Rh1 2.245(9) . ? C5 H5 0.9800 . ? C6 C7 1.494(14) . ? C6 Rh1 2.168(9) . ? C6 H6 0.9800 . ? C7 C8 1.482(17) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C11 1.353(11) . ? C9 N1 1.418(10) . ? C9 C25 1.464(12) . ? C10 N1 1.358(11) . ? C10 N2 1.397(10) . ? C10 C34 1.496(12) . ? C11 N2 1.382(11) . ? C11 Rh1 2.025(8) . ? C12 N2 1.476(11) . ? C12 C13 1.523(13) . ? C12 C17 1.529(14) . ? C12 H12 0.9800 . ? C13 C14 1.509(15) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 C15 1.511(17) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 C16 1.553(16) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 C17 1.541(13) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 N3 1.503(13) . ? C17 H17 0.9800 . ? C18 C19 1.478(13) . ? C18 N3 1.506(11) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 C24 1.365(13) . ? C19 C20 1.381(13) . ? C20 C21 1.357(16) . ? C20 H20 0.9300 . ? C21 C22 1.37(2) . ? C21 H21 0.9300 . ? C22 C23 1.389(19) . ? C22 H22 0.9300 . ? C23 C24 1.379(16) . ? C23 H23 0.9300 . ? C24 H24 0.9300 . ? C25 C27 1.508(17) . ? C25 C26 1.517(14) . ? C25 H25 0.9800 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C28 C29 1.365(13) . ? C28 C33 1.376(14) . ? C28 N1 1.497(12) . ? C29 C30 1.380(14) . ? C29 H29 0.9300 . ? C30 C31 1.345(16) . ? C30 H30 0.9300 . ? C31 C32 1.337(17) . ? C31 H31 0.9300 . ? C32 C33 1.385(16) . ? C32 H32 0.9300 . ? C33 H33 0.9300 . ? C34 C35 1.366(13) . ? C34 C39 1.371(13) . ? C35 C36 1.410(13) . ? C35 H35 0.9300 . ? C36 C37 1.373(15) . ? C36 H36 0.9300 . ? C37 C38 1.361(16) . ? C37 H37 0.9300 . ? C38 C39 1.402(14) . ? C38 H38 0.9300 . ? C39 H39 0.9300 . ? N3 Rh1 2.206(7) . ? N3 H3 0.9100 . ? B1 C64 1.628(12) . ? B1 C40 1.630(11) . ? B1 C56 1.640(11) . ? B1 C48 1.653(11) . ? C40 C41 1.389(11) . ? C40 C45 1.391(11) . ? C41 C42 1.384(11) . ? C41 H41 0.9300 . ? C42 C43 1.381(12) . ? C42 C46 1.499(13) . ? C43 C44 1.384(12) . ? C43 H43 0.9300 . ? C44 C45 1.385(11) . ? C44 C47 1.498(13) . ? C45 H45 0.9300 . ? C46 F1 1.308(11) . ? C46 F3 1.332(12) . ? C46 F2 1.351(12) . ? C47 F4 1.238(18) . ? C47 F5A 1.257(18) . ? C47 F6A 1.265(18) . ? C47 F4A 1.31(2) . ? C47 F5 1.35(2) . ? C47 F6 1.389(17) . ? C48 C53 1.402(11) . ? C48 C49 1.406(11) . ? C49 C50 1.358(13) . ? C49 H49 0.9300 . ? C50 C51 1.420(14) . ? C50 C54 1.509(14) . ? C51 C52 1.363(14) . ? C51 H51 0.9300 . ? C52 C53 1.389(12) . ? C52 C55 1.529(15) . ? C53 H53 0.9300 . ? C54 F7 1.284(11) . ? C54 F9 1.317(13) . ? C54 F8 1.326(14) . ? C55 F11 1.21(2) . ? C55 F12 1.223(18) . ? C55 F12A 1.25(2) . ? C55 F11A 1.34(2) . ? C55 F10A 1.35(2) . ? C55 F10 1.43(3) . ? C56 C61 1.391(12) . ? C56 C57 1.397(12) . ? C57 C58 1.380(12) . ? C57 H57 0.9300 . ? C58 C59 1.385(14) . ? C58 C62 1.461(15) . ? C59 C60 1.359(14) . ? C59 H59 0.9300 . ? C60 C61 1.369(12) . ? C60 C63 1.496(15) . ? C61 H61 0.9300 . ? C62 F14 1.304(15) . ? C62 F13 1.309(11) . ? C62 F15 1.336(13) . ? C63 F16 1.228(17) . ? C63 F17 1.292(14) . ? C63 F18 1.337(15) . ? C64 C69 1.404(11) . ? C64 C65 1.418(10) . ? C65 C66 1.390(11) . ? C65 H65 0.9300 . ? C66 C67 1.381(11) . ? C66 C70 1.466(12) . ? C67 C68 1.402(11) . ? C67 H67 0.9300 . ? C68 C69 1.382(11) . ? C68 C71 1.495(12) . ? C69 H69 0.9300 . ? C70 F20 1.317(11) . ? C70 F21 1.327(10) . ? C70 F19 1.334(11) . ? C71 F24 1.323(10) . ? C71 F23 1.323(10) . ? C71 F22 1.349(11) . ? C1' C2' 1.370(14) . ? C1' C8' 1.529(12) . ? C1' Rh1' 2.114(8) . ? C1' H1' 0.9800 . ? C2' C3' 1.531(14) . ? C2' Rh1' 2.125(9) . ? C2' H2' 0.9800 . ? C3' C4' 1.498(13) . ? C3' H3'1 0.9700 . ? C3' H3'2 0.9700 . ? C4' C5' 1.512(12) . ? C4' H4'1 0.9700 . ? C4' H4'2 0.9700 . ? C5' C6' 1.377(12) . ? C5' Rh1' 2.212(8) . ? C5' H5' 0.9800 . ? C6' C7' 1.518(11) . ? C6' Rh1' 2.189(7) . ? C6' H6' 0.9800 . ? C7' C8' 1.501(12) . ? C7' H7'1 0.9700 . ? C7' H7'2 0.9700 . ? C8' H8'1 0.9700 . ? C8' H8'2 0.9700 . ? C9' N2' 1.338(10) . ? C9' N1' 1.363(10) . ? C9' Rh1' 2.066(7) . ? C10' C11' 1.347(10) . ? C10' N1' 1.381(9) . ? C10' C34' 1.514(11) . ? C11' N2' 1.401(10) . ? C11' C28' 1.473(11) . ? C12' N2' 1.468(10) . ? C12' C17' 1.500(12) . ? C12' C13' 1.523(12) . ? C12' H12' 0.9800 . ? C13' C14' 1.536(12) . ? C13' H13C 0.9700 . ? C13' H13D 0.9700 . ? C14' C15' 1.508(13) . ? C14' H14C 0.9700 . ? C14' H14D 0.9700 . ? C15' C16' 1.501(12) . ? C15' H15C 0.9700 . ? C15' H15D 0.9700 . ? C16' C17' 1.527(11) . ? C16' H16C 0.9700 . ? C16' H16D 0.9700 . ? C17' N3' 1.504(10) . ? C17' H17' 0.9800 . ? C18' C19' 1.485(11) . ? C18' N3' 1.496(10) . ? C18' H18C 0.9700 . ? C18' H18D 0.9700 . ? C19' C24' 1.386(11) . ? C19' C20' 1.418(12) . ? C20' C21' 1.386(13) . ? C20' H20' 0.9300 . ? C21' C22' 1.362(14) . ? C21' H21' 0.9300 . ? C22' C23' 1.352(13) . ? C22' H22' 0.9300 . ? C23' C24' 1.391(12) . ? C23' H23' 0.9300 . ? C24' H24' 0.9300 . ? C25' C27' 1.477(13) . ? C25' N1' 1.486(10) . ? C25' C26' 1.519(12) . ? C25' H25' 0.9800 . ? C26' H26D 0.9600 . ? C26' H26E 0.9600 . ? C26' H26F 0.9600 . ? C27' H27D 0.9600 . ? C27' H27E 0.9600 . ? C27' H27F 0.9600 . ? C28' C29' 1.382(12) . ? C28' C33' 1.398(12) . ? C29' C30' 1.333(13) . ? C29' H29' 0.9300 . ? C30' C31' 1.376(16) . ? C30' H30' 0.9300 . ? C31' C32' 1.390(17) . ? C31' H31' 0.9300 . ? C32' C33' 1.425(14) . ? C32' H32' 0.9300 . ? C33' H33' 0.9300 . ? C34' C35' 1.344(12) . ? C34' C39' 1.369(13) . ? C35' C36' 1.410(13) . ? C35' H35' 0.9300 . ? C36' C37' 1.366(16) . ? C36' H36' 0.9300 . ? C37' C38' 1.369(17) . ? C37' H37' 0.9300 . ? C38' C39' 1.363(15) . ? C38' H38' 0.9300 . ? C39' H39' 0.9300 . ? F1' C46' 1.341(13) . ? F2' C46' 1.270(11) . ? F3' C46' 1.222(11) . ? F4' C47' 1.328(11) . ? F5' C47' 1.328(9) . ? F6' C47' 1.309(10) . ? F7' C54' 1.328(10) . ? F8' C54' 1.269(11) . ? F9' C54' 1.283(10) . ? F10' C55' 1.321(11) . ? F11' C55' 1.305(11) . ? F12' C55' 1.344(12) . ? F13' C62' 1.335(10) . ? F14' C62' 1.328(11) . ? F15' C62' 1.322(11) . ? F16' C63' 1.332(11) . ? F17' C63' 1.309(11) . ? F18' C63' 1.308(10) . ? F19' C70' 1.337(16) . ? F20' C70' 1.296(14) . ? F21' C70' 1.273(14) . ? F22' C71' 1.288(14) . ? F23' C71' 1.278(12) . ? F24' C71' 1.300(12) . ? N3' Rh1' 2.218(7) . ? N3' H3' 0.91(8) . ? B1' C40' 1.621(11) . ? B1' C64' 1.637(11) . ? B1' C56' 1.640(12) . ? B1' C48' 1.654(11) . ? C40' C41' 1.393(11) . ? C40' C45' 1.410(11) . ? C41' C42' 1.409(12) . ? C41' H41' 0.9300 . ? C42' C43' 1.374(12) . ? C42' C46' 1.499(12) . ? C43' C44' 1.370(12) . ? C43' H43' 0.9300 . ? C44' C45' 1.381(11) . ? C44' C47' 1.488(12) . ? C45' H45' 0.9300 . ? C48' C53' 1.379(11) . ? C48' C49' 1.403(11) . ? C49' C50' 1.391(11) . ? C49' H49' 0.9300 . ? C50' C51' 1.360(11) . ? C50' C54' 1.528(11) . ? C51' C52' 1.363(12) . ? C51' H51' 0.9300 . ? C52' C53' 1.388(11) . ? C52' C55' 1.557(12) . ? C53' H53' 0.9300 . ? C56' C61' 1.392(10) . ? C56' C57' 1.403(11) . ? C57' C58' 1.389(11) . ? C57' H57' 0.9300 . ? C58' C59' 1.375(11) . ? C58' C62' 1.471(12) . ? C59' C60' 1.424(12) . ? C59' H59' 0.9300 . ? C60' C61' 1.390(11) . ? C60' C63' 1.498(12) . ? C61' H61' 0.9300 . ? C64' C69' 1.389(11) . ? C64' C65' 1.414(11) . ? C65' C66' 1.403(12) . ? C65' H65' 0.9300 . ? C66' C67' 1.364(14) . ? C66' C70' 1.502(15) . ? C67' C68' 1.362(14) . ? C67' H67' 0.9300 . ? C68' C69' 1.390(12) . ? C68' C71' 1.481(14) . ? C69' H69' 0.9300 . ? C72 C77 1.289(19) . ? C72 C73 1.31(2) . ? C72 C78 1.57(2) . ? C73 C74 1.35(2) . ? C73 H73 0.9300 . ? C74 C75 1.46(2) . ? C74 H74 0.9300 . ? C75 C76 1.23(2) . ? C75 H75 0.9300 . ? C76 C77 1.44(3) . ? C76 H76 0.9300 . ? C77 H77 0.9300 . ? C78 H78A 0.9600 . ? C78 H78B 0.9600 . ? C78 H78C 0.9600 . ? C79 C85 1.13(3) . ? C79 C80 1.3900 . ? C79 C84 1.3900 . ? C80 C81 1.3900 . ? C80 H80 0.9300 . ? C81 C82 1.3900 . ? C81 H81 0.9300 . ? C82 C83 1.3900 . ? C82 H82 0.9300 . ? C83 C84 1.3900 . ? C83 H83 0.9300 . ? C84 H84 0.9300 . ? C85 H85A 0.9600 . ? C85 H85B 0.9600 . ? C85 H85C 0.9600 . ? 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 C1 C8 124.3(11) . . ? C2 C1 Rh1 67.9(6) . . ? C8 C1 Rh1 112.5(7) . . ? C2 C1 H1 114.5 . . ? C8 C1 H1 114.5 . . ? Rh1 C1 H1 114.5 . . ? C1 C2 C3 129.2(12) . . ? C1 C2 Rh1 73.4(6) . . ? C3 C2 Rh1 110.6(9) . . ? C1 C2 H2 112.2 . . ? C3 C2 H2 112.2 . . ? Rh1 C2 H2 112.2 . . ? C2 C3 C4 110.7(10) . . ? C2 C3 H3A 109.5 . . ? C4 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? C4 C3 H3B 109.5 . . ? H3A C3 H3B 108.1 . . ? C5 C4 C3 111.0(9) . . ? C5 C4 H4A 109.4 . . ? C3 C4 H4A 109.4 . . ? C5 C4 H4B 109.4 . . ? C3 C4 H4B 109.4 . . ? H4A C4 H4B 108.0 . . ? C6 C5 C4 127.0(10) . . ? C6 C5 Rh1 69.2(5) . . ? C4 C5 Rh1 111.1(9) . . ? C6 C5 H5 113.6 . . ? C4 C5 H5 113.6 . . ? Rh1 C5 H5 113.6 . . ? C5 C6 C7 124.0(11) . . ? C5 C6 Rh1 75.4(6) . . ? C7 C6 Rh1 108.3(6) . . ? C5 C6 H6 114.1 . . ? C7 C6 H6 114.1 . . ? Rh1 C6 H6 114.1 . . ? C8 C7 C6 115.0(9) . . ? C8 C7 H7A 108.5 . . ? C6 C7 H7A 108.5 . . ? C8 C7 H7B 108.5 . . ? C6 C7 H7B 108.5 . . ? H7A C7 H7B 107.5 . . ? C7 C8 C1 112.5(8) . . ? C7 C8 H8A 109.1 . . ? C1 C8 H8A 109.1 . . ? C7 C8 H8B 109.1 . . ? C1 C8 H8B 109.1 . . ? H8A C8 H8B 107.8 . . ? C11 C9 N1 111.1(7) . . ? C11 C9 C25 120.7(7) . . ? N1 C9 C25 127.7(7) . . ? N1 C10 N2 107.4(7) . . ? N1 C10 C34 126.8(8) . . ? N2 C10 C34 125.6(7) . . ? C9 C11 N2 105.0(7) . . ? C9 C11 Rh1 136.3(6) . . ? N2 C11 Rh1 117.1(6) . . ? N2 C12 C13 115.1(8) . . ? N2 C12 C17 109.9(7) . . ? C13 C12 C17 112.1(8) . . ? N2 C12 H12 106.4 . . ? C13 C12 H12 106.4 . . ? C17 C12 H12 106.4 . . ? C14 C13 C12 108.4(9) . . ? C14 C13 H13A 110.0 . . ? C12 C13 H13A 110.0 . . ? C14 C13 H13B 110.0 . . ? C12 C13 H13B 110.0 . . ? H13A C13 H13B 108.4 . . ? C13 C14 C15 109.9(10) . . ? C13 C14 H14A 109.7 . . ? C15 C14 H14A 109.7 . . ? C13 C14 H14B 109.7 . . ? C15 C14 H14B 109.7 . . ? H14A C14 H14B 108.2 . . ? C14 C15 C16 113.5(9) . . ? C14 C15 H15A 108.9 . . ? C16 C15 H15A 108.9 . . ? C14 C15 H15B 108.9 . . ? C16 C15 H15B 108.9 . . ? H15A C15 H15B 107.7 . . ? C17 C16 C15 110.1(9) . . ? C17 C16 H16A 109.6 . . ? C15 C16 H16A 109.6 . . ? C17 C16 H16B 109.6 . . ? C15 C16 H16B 109.6 . . ? H16A C16 H16B 108.2 . . ? N3 C17 C12 112.3(8) . . ? N3 C17 C16 109.5(9) . . ? C12 C17 C16 109.2(9) . . ? N3 C17 H17 108.6 . . ? C12 C17 H17 108.6 . . ? C16 C17 H17 108.6 . . ? C19 C18 N3 111.1(7) . . ? C19 C18 H18A 109.4 . . ? N3 C18 H18A 109.4 . . ? C19 C18 H18B 109.4 . . ? N3 C18 H18B 109.4 . . ? H18A C18 H18B 108.0 . . ? C24 C19 C20 118.8(9) . . ? C24 C19 C18 120.6(9) . . ? C20 C19 C18 120.5(8) . . ? C21 C20 C19 121.3(11) . . ? C21 C20 H20 119.4 . . ? C19 C20 H20 119.4 . . ? C20 C21 C22 120.8(13) . . ? C20 C21 H21 119.6 . . ? C22 C21 H21 119.6 . . ? C21 C22 C23 118.2(12) . . ? C21 C22 H22 120.9 . . ? C23 C22 H22 120.9 . . ? C24 C23 C22 120.9(11) . . ? C24 C23 H23 119.6 . . ? C22 C23 H23 119.6 . . ? C19 C24 C23 120.1(11) . . ? C19 C24 H24 120.0 . . ? C23 C24 H24 120.0 . . ? C9 C25 C27 113.2(9) . . ? C9 C25 C26 110.8(9) . . ? C27 C25 C26 113.0(12) . . ? C9 C25 H25 106.4 . . ? C27 C25 H25 106.4 . . ? C26 C25 H25 106.4 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C29 C28 C33 119.4(9) . . ? C29 C28 N1 120.3(8) . . ? C33 C28 N1 119.8(9) . . ? C28 C29 C30 119.8(10) . . ? C28 C29 H29 120.1 . . ? C30 C29 H29 120.1 . . ? C31 C30 C29 120.8(11) . . ? C31 C30 H30 119.6 . . ? C29 C30 H30 119.6 . . ? C32 C31 C30 119.6(11) . . ? C32 C31 H31 120.2 . . ? C30 C31 H31 120.2 . . ? C31 C32 C33 121.6(11) . . ? C31 C32 H32 119.2 . . ? C33 C32 H32 119.2 . . ? C28 C33 C32 118.7(12) . . ? C28 C33 H33 120.6 . . ? C32 C33 H33 120.6 . . ? C35 C34 C39 120.5(9) . . ? C35 C34 C10 118.3(8) . . ? C39 C34 C10 121.2(8) . . ? C34 C35 C36 119.3(9) . . ? C34 C35 H35 120.4 . . ? C36 C35 H35 120.4 . . ? C37 C36 C35 119.2(9) . . ? C37 C36 H36 120.4 . . ? C35 C36 H36 120.4 . . ? C38 C37 C36 121.7(9) . . ? C38 C37 H37 119.1 . . ? C36 C37 H37 119.1 . . ? C37 C38 C39 118.4(10) . . ? C37 C38 H38 120.8 . . ? C39 C38 H38 120.8 . . ? C34 C39 C38 120.7(10) . . ? C34 C39 H39 119.7 . . ? C38 C39 H39 119.7 . . ? C10 N1 C9 106.1(7) . . ? C10 N1 C28 125.0(7) . . ? C9 N1 C28 128.8(7) . . ? C11 N2 C10 110.4(7) . . ? C11 N2 C12 117.6(7) . . ? C10 N2 C12 131.6(7) . . ? C17 N3 C18 113.1(7) . . ? C17 N3 Rh1 111.6(6) . . ? C18 N3 Rh1 113.5(5) . . ? C17 N3 H3 106.0 . . ? C18 N3 H3 106.0 . . ? Rh1 N3 H3 106.0 . . ? C11 Rh1 C2 94.2(4) . . ? C11 Rh1 C1 99.9(4) . . ? C2 Rh1 C1 38.7(4) . . ? C11 Rh1 C6 162.9(4) . . ? C2 Rh1 C6 97.0(5) . . ? C1 Rh1 C6 81.1(4) . . ? C11 Rh1 N3 81.6(3) . . ? C2 Rh1 N3 144.5(4) . . ? C1 Rh1 N3 176.6(4) . . ? C6 Rh1 N3 96.5(4) . . ? C11 Rh1 C5 160.7(4) . . ? C2 Rh1 C5 81.1(5) . . ? C1 Rh1 C5 88.2(4) . . ? C6 Rh1 C5 35.5(4) . . ? N3 Rh1 C5 91.4(3) . . ? C64 B1 C40 106.2(6) . . ? C64 B1 C56 111.4(6) . . ? C40 B1 C56 111.5(6) . . ? C64 B1 C48 112.9(6) . . ? C40 B1 C48 112.4(7) . . ? C56 B1 C48 102.6(6) . . ? C41 C40 C45 114.6(7) . . ? C41 C40 B1 124.3(7) . . ? C45 C40 B1 120.8(7) . . ? C42 C41 C40 122.7(8) . . ? C42 C41 H41 118.6 . . ? C40 C41 H41 118.6 . . ? C43 C42 C41 121.5(8) . . ? C43 C42 C46 117.5(8) . . ? C41 C42 C46 120.9(8) . . ? C42 C43 C44 117.0(8) . . ? C42 C43 H43 121.5 . . ? C44 C43 H43 121.5 . . ? C43 C44 C45 120.7(8) . . ? C43 C44 C47 118.8(8) . . ? C45 C44 C47 120.4(9) . . ? C44 C45 C40 123.3(8) . . ? C44 C45 H45 118.3 . . ? C40 C45 H45 118.3 . . ? F1 C46 F3 107.7(8) . . ? F1 C46 F2 106.2(8) . . ? F3 C46 F2 102.7(9) . . ? F1 C46 C42 114.2(9) . . ? F3 C46 C42 112.1(8) . . ? F2 C46 C42 113.1(8) . . ? F4 C47 F5A 131.8(14) . . ? F4 C47 F6A 52.6(19) . . ? F5A C47 F6A 109.3(18) . . ? F4 C47 F4A 54(2) . . ? F5A C47 F4A 108.2(18) . . ? F6A C47 F4A 105.5(15) . . ? F4 C47 F5 109(2) . . ? F5A C47 F5 43.6(15) . . ? F6A C47 F5 129.9(14) . . ? F4A C47 F5 65.8(13) . . ? F4 C47 F6 108(2) . . ? F5A C47 F6 56.2(16) . . ? F6A C47 F6 59.0(13) . . ? F4A C47 F6 142.3(12) . . ? F5 C47 F6 96.8(14) . . ? F4 C47 C44 116.8(11) . . ? F5A C47 C44 111.2(10) . . ? F6A C47 C44 115.0(12) . . ? F4A C47 C44 107.3(11) . . ? F5 C47 C44 114.5(10) . . ? F6 C47 C44 110.4(10) . . ? C53 C48 C49 115.2(7) . . ? C53 C48 B1 120.9(7) . . ? C49 C48 B1 123.6(7) . . ? C50 C49 C48 122.9(8) . . ? C50 C49 H49 118.6 . . ? C48 C49 H49 118.6 . . ? C49 C50 C51 120.9(9) . . ? C49 C50 C54 118.4(10) . . ? C51 C50 C54 120.7(9) . . ? C52 C51 C50 117.1(8) . . ? C52 C51 H51 121.4 . . ? C50 C51 H51 121.4 . . ? C51 C52 C53 121.7(9) . . ? C51 C52 C55 119.3(9) . . ? C53 C52 C55 118.9(9) . . ? C52 C53 C48 122.0(8) . . ? C52 C53 H53 119.0 . . ? C48 C53 H53 119.0 . . ? F7 C54 F9 108.0(9) . . ? F7 C54 F8 106.7(10) . . ? F9 C54 F8 104.3(11) . . ? F7 C54 C50 113.1(9) . . ? F9 C54 C50 113.4(10) . . ? F8 C54 C50 110.8(8) . . ? F11 C55 F12 113(2) . . ? F11 C55 F12A 127.6(17) . . ? F12 C55 F12A 61.9(18) . . ? F11 C55 F11A 65(2) . . ? F12 C55 F11A 56(2) . . ? F12A C55 F11A 113(3) . . ? F11 C55 F10A 44.3(17) . . ? F12 C55 F10A 141.5(15) . . ? F12A C55 F10A 104(2) . . ? F11A C55 F10A 109(3) . . ? F11 C55 F10 102.7(19) . . ? F12 C55 F10 98.3(17) . . ? F12A C55 F10 38.8(16) . . ? F11A C55 F10 135.5(16) . . ? F10A C55 F10 66.9(19) . . ? F11 C55 C52 118.4(11) . . ? F12 C55 C52 112.8(12) . . ? F12A C55 C52 109.3(17) . . ? F11A C55 C52 114.7(14) . . ? F10A C55 C52 105.6(13) . . ? F10 C55 C52 108.6(16) . . ? C61 C56 C57 112.7(7) . . ? C61 C56 B1 122.0(7) . . ? C57 C56 B1 125.1(7) . . ? C58 C57 C56 124.3(8) . . ? C58 C57 H57 117.8 . . ? C56 C57 H57 117.8 . . ? C57 C58 C59 118.6(9) . . ? C57 C58 C62 120.5(9) . . ? C59 C58 C62 121.0(9) . . ? C60 C59 C58 120.1(8) . . ? C60 C59 H59 119.9 . . ? C58 C59 H59 119.9 . . ? C59 C60 C61 119.0(8) . . ? C59 C60 C63 118.9(9) . . ? C61 C60 C63 122.1(10) . . ? C60 C61 C56 125.3(9) . . ? C60 C61 H61 117.3 . . ? C56 C61 H61 117.3 . . ? F14 C62 F13 107.3(12) . . ? F14 C62 F15 99.8(12) . . ? F13 C62 F15 105.6(9) . . ? F14 C62 C58 113.1(10) . . ? F13 C62 C58 116.2(10) . . ? F15 C62 C58 113.3(9) . . ? F16 C63 F17 111.3(13) . . ? F16 C63 F18 104.3(14) . . ? F17 C63 F18 100.3(11) . . ? F16 C63 C60 114.8(12) . . ? F17 C63 C60 113.6(12) . . ? F18 C63 C60 111.2(11) . . ? C69 C64 C65 114.5(7) . . ? C69 C64 B1 118.7(6) . . ? C65 C64 B1 126.4(7) . . ? C66 C65 C64 122.9(7) . . ? C66 C65 H65 118.6 . . ? C64 C65 H65 118.6 . . ? C67 C66 C65 120.6(7) . . ? C67 C66 C70 120.0(7) . . ? C65 C66 C70 119.4(7) . . ? C66 C67 C68 118.2(7) . . ? C66 C67 H67 120.9 . . ? C68 C67 H67 120.9 . . ? C69 C68 C67 120.6(7) . . ? C69 C68 C71 118.7(7) . . ? C67 C68 C71 120.7(7) . . ? C68 C69 C64 123.2(7) . . ? C68 C69 H69 118.4 . . ? C64 C69 H69 118.4 . . ? F20 C70 F21 106.5(8) . . ? F20 C70 F19 106.2(8) . . ? F21 C70 F19 106.0(8) . . ? F20 C70 C66 112.7(8) . . ? F21 C70 C66 112.5(8) . . ? F19 C70 C66 112.4(8) . . ? F24 C71 F23 107.2(7) . . ? F24 C71 F22 106.2(8) . . ? F23 C71 F22 103.9(7) . . ? F24 C71 C68 113.5(7) . . ? F23 C71 C68 113.5(8) . . ? F22 C71 C68 111.8(7) . . ? C2' C1' C8' 123.0(9) . . ? C2' C1' Rh1' 71.5(5) . . ? C8' C1' Rh1' 114.5(5) . . ? C2' C1' H1' 113.7 . . ? C8' C1' H1' 113.7 . . ? Rh1' C1' H1' 113.7 . . ? C1' C2' C3' 127.2(9) . . ? C1' C2' Rh1' 70.7(5) . . ? C3' C2' Rh1' 109.3(6) . . ? C1' C2' H2' 113.7 . . ? C3' C2' H2' 113.7 . . ? Rh1' C2' H2' 113.7 . . ? C4' C3' C2' 112.9(8) . . ? C4' C3' H3'1 109.0 . . ? C2' C3' H3'1 109.0 . . ? C4' C3' H3'2 109.0 . . ? C2' C3' H3'2 109.0 . . ? H3'1 C3' H3'2 107.8 . . ? C3' C4' C5' 114.1(7) . . ? C3' C4' H4'1 108.7 . . ? C5' C4' H4'1 108.7 . . ? C3' C4' H4'2 108.7 . . ? C5' C4' H4'2 108.7 . . ? H4'1 C4' H4'2 107.6 . . ? C6' C5' C4' 123.7(8) . . ? C6' C5' Rh1' 70.9(5) . . ? C4' C5' Rh1' 110.4(6) . . ? C6' C5' H5' 114.6 . . ? C4' C5' H5' 114.6 . . ? Rh1' C5' H5' 114.6 . . ? C5' C6' C7' 124.3(8) . . ? C5' C6' Rh1' 72.7(5) . . ? C7' C6' Rh1' 108.3(5) . . ? C5' C6' H6' 114.6 . . ? C7' C6' H6' 114.6 . . ? Rh1' C6' H6' 114.6 . . ? C8' C7' C6' 115.1(7) . . ? C8' C7' H7'1 108.5 . . ? C6' C7' H7'1 108.5 . . ? C8' C7' H7'2 108.5 . . ? C6' C7' H7'2 108.5 . . ? H7'1 C7' H7'2 107.5 . . ? C7' C8' C1' 112.0(7) . . ? C7' C8' H8'1 109.2 . . ? C1' C8' H8'1 109.2 . . ? C7' C8' H8'2 109.2 . . ? C1' C8' H8'2 109.2 . . ? H8'1 C8' H8'2 107.9 . . ? N2' C9' N1' 107.2(6) . . ? N2' C9' Rh1' 115.5(5) . . ? N1' C9' Rh1' 136.4(6) . . ? C11' C10' N1' 107.9(7) . . ? C11' C10' C34' 125.4(7) . . ? N1' C10' C34' 126.7(7) . . ? C10' C11' N2' 106.7(6) . . ? C10' C11' C28' 128.1(7) . . ? N2' C11' C28' 125.0(6) . . ? N2' C12' C17' 112.0(7) . . ? N2' C12' C13' 116.6(7) . . ? C17' C12' C13' 112.9(7) . . ? N2' C12' H12' 104.7 . . ? C17' C12' H12' 104.7 . . ? C13' C12' H12' 104.7 . . ? C12' C13' C14' 107.3(7) . . ? C12' C13' H13C 110.2 . . ? C14' C13' H13C 110.2 . . ? C12' C13' H13D 110.2 . . ? C14' C13' H13D 110.2 . . ? H13C C13' H13D 108.5 . . ? C15' C14' C13' 110.8(7) . . ? C15' C14' H14C 109.5 . . ? C13' C14' H14C 109.5 . . ? C15' C14' H14D 109.5 . . ? C13' C14' H14D 109.5 . . ? H14C C14' H14D 108.1 . . ? C16' C15' C14' 111.3(7) . . ? C16' C15' H15C 109.4 . . ? C14' C15' H15C 109.4 . . ? C16' C15' H15D 109.4 . . ? C14' C15' H15D 109.4 . . ? H15C C15' H15D 108.0 . . ? C15' C16' C17' 113.2(7) . . ? C15' C16' H16C 108.9 . . ? C17' C16' H16C 108.9 . . ? C15' C16' H16D 108.9 . . ? C17' C16' H16D 108.9 . . ? H16C C16' H16D 107.7 . . ? C12' C17' N3' 111.2(7) . . ? C12' C17' C16' 110.8(7) . . ? N3' C17' C16' 111.4(6) . . ? C12' C17' H17' 107.8 . . ? N3' C17' H17' 107.8 . . ? C16' C17' H17' 107.8 . . ? C19' C18' N3' 108.9(7) . . ? C19' C18' H18C 109.9 . . ? N3' C18' H18C 109.9 . . ? C19' C18' H18D 109.9 . . ? N3' C18' H18D 109.9 . . ? H18C C18' H18D 108.3 . . ? C24' C19' C20' 117.3(8) . . ? C24' C19' C18' 122.9(7) . . ? C20' C19' C18' 119.4(7) . . ? C21' C20' C19' 119.2(8) . . ? C21' C20' H20' 120.4 . . ? C19' C20' H20' 120.4 . . ? C22' C21' C20' 121.8(9) . . ? C22' C21' H21' 119.1 . . ? C20' C21' H21' 119.1 . . ? C23' C22' C21' 120.1(9) . . ? C23' C22' H22' 119.9 . . ? C21' C22' H22' 119.9 . . ? C22' C23' C24' 119.9(8) . . ? C22' C23' H23' 120.1 . . ? C24' C23' H23' 120.1 . . ? C19' C24' C23' 121.8(8) . . ? C19' C24' H24' 119.1 . . ? C23' C24' H24' 119.1 . . ? C27' C25' N1' 114.5(7) . . ? C27' C25' C26' 113.5(8) . . ? N1' C25' C26' 109.5(7) . . ? C27' C25' H25' 106.2 . . ? N1' C25' H25' 106.2 . . ? C26' C25' H25' 106.2 . . ? C25' C26' H26D 109.5 . . ? C25' C26' H26E 109.5 . . ? H26D C26' H26E 109.5 . . ? C25' C26' H26F 109.5 . . ? H26D C26' H26F 109.5 . . ? H26E C26' H26F 109.5 . . ? C25' C27' H27D 109.5 . . ? C25' C27' H27E 109.5 . . ? H27D C27' H27E 109.5 . . ? C25' C27' H27F 109.5 . . ? H27D C27' H27F 109.5 . . ? H27E C27' H27F 109.5 . . ? C29' C28' C33' 118.7(8) . . ? C29' C28' C11' 121.5(7) . . ? C33' C28' C11' 119.8(8) . . ? C30' C29' C28' 122.0(9) . . ? C30' C29' H29' 119.0 . . ? C28' C29' H29' 119.0 . . ? C29' C30' C31' 121.2(10) . . ? C29' C30' H30' 119.4 . . ? C31' C30' H30' 119.4 . . ? C30' C31' C32' 119.5(9) . . ? C30' C31' H31' 120.2 . . ? C32' C31' H31' 120.2 . . ? C31' C32' C33' 119.2(10) . . ? C31' C32' H32' 120.4 . . ? C33' C32' H32' 120.4 . . ? C28' C33' C32' 119.1(10) . . ? C28' C33' H33' 120.5 . . ? C32' C33' H33' 120.5 . . ? C35' C34' C39' 120.2(8) . . ? C35' C34' C10' 119.6(7) . . ? C39' C34' C10' 120.1(8) . . ? C34' C35' C36' 120.1(9) . . ? C34' C35' H35' 119.9 . . ? C36' C35' H35' 119.9 . . ? C37' C36' C35' 119.1(10) . . ? C37' C36' H36' 120.4 . . ? C35' C36' H36' 120.4 . . ? C36' C37' C38' 119.7(10) . . ? C36' C37' H37' 120.1 . . ? C38' C37' H37' 120.1 . . ? C39' C38' C37' 120.6(11) . . ? C39' C38' H38' 119.7 . . ? C37' C38' H38' 119.7 . . ? C38' C39' C34' 120.2(10) . . ? C38' C39' H39' 119.9 . . ? C34' C39' H39' 119.9 . . ? C9' N1' C10' 108.9(6) . . ? C9' N1' C25' 122.7(6) . . ? C10' N1' C25' 128.5(6) . . ? C9' N2' C11' 109.3(6) . . ? C9' N2' C12' 121.2(6) . . ? C11' N2' C12' 129.4(7) . . ? C18' N3' C17' 113.2(6) . . ? C18' N3' Rh1' 112.9(5) . . ? C17' N3' Rh1' 112.9(5) . . ? C18' N3' H3' 101(5) . . ? C17' N3' H3' 105(5) . . ? Rh1' N3' H3' 110(5) . . ? C9' Rh1' C1' 100.3(3) . . ? C9' Rh1' C2' 94.2(3) . . ? C1' Rh1' C2' 37.7(4) . . ? C9' Rh1' C6' 164.1(3) . . ? C1' Rh1' C6' 81.4(3) . . ? C2' Rh1' C6' 96.5(3) . . ? C9' Rh1' C5' 158.1(3) . . ? C1' Rh1' C5' 89.4(3) . . ? C2' Rh1' C5' 81.5(3) . . ? C6' Rh1' C5' 36.5(3) . . ? C9' Rh1' N3' 81.7(3) . . ? C1' Rh1' N3' 174.7(3) . . ? C2' Rh1' N3' 147.4(3) . . ? C6' Rh1' N3' 95.3(3) . . ? C5' Rh1' N3' 90.4(3) . . ? C40' B1' C64' 104.4(6) . . ? C40' B1' C56' 113.5(6) . . ? C64' B1' C56' 107.6(6) . . ? C40' B1' C48' 114.9(6) . . ? C64' B1' C48' 112.1(6) . . ? C56' B1' C48' 104.4(6) . . ? C41' C40' C45' 115.1(7) . . ? C41' C40' B1' 120.2(7) . . ? C45' C40' B1' 124.5(7) . . ? C40' C41' C42' 121.9(8) . . ? C40' C41' H41' 119.1 . . ? C42' C41' H41' 119.1 . . ? C43' C42' C41' 120.3(8) . . ? C43' C42' C46' 120.1(8) . . ? C41' C42' C46' 119.6(8) . . ? C44' C43' C42' 119.6(8) . . ? C44' C43' H43' 120.2 . . ? C42' C43' H43' 120.2 . . ? C43' C44' C45' 119.9(7) . . ? C43' C44' C47' 121.0(8) . . ? C45' C44' C47' 119.2(7) . . ? C44' C45' C40' 123.3(7) . . ? C44' C45' H45' 118.3 . . ? C40' C45' H45' 118.3 . . ? F3' C46' F2' 110.0(10) . . ? F3' C46' F1' 106.7(10) . . ? F2' C46' F1' 97.3(9) . . ? F3' C46' C42' 116.1(8) . . ? F2' C46' C42' 112.7(8) . . ? F1' C46' C42' 112.3(9) . . ? F6' C47' F4' 106.1(8) . . ? F6' C47' F5' 105.7(7) . . ? F4' C47' F5' 104.6(7) . . ? F6' C47' C44' 114.4(7) . . ? F4' C47' C44' 113.0(7) . . ? F5' C47' C44' 112.2(7) . . ? C53' C48' C49' 114.7(7) . . ? C53' C48' B1' 122.1(7) . . ? C49' C48' B1' 123.1(7) . . ? C50' C49' C48' 121.9(7) . . ? C50' C49' H49' 119.0 . . ? C48' C49' H49' 119.0 . . ? C51' C50' C49' 121.9(7) . . ? C51' C50' C54' 120.5(7) . . ? C49' C50' C54' 117.5(7) . . ? C50' C51' C52' 116.8(7) . . ? C50' C51' H51' 121.6 . . ? C52' C51' H51' 121.6 . . ? C51' C52' C53' 122.2(7) . . ? C51' C52' C55' 119.3(7) . . ? C53' C52' C55' 118.5(8) . . ? C48' C53' C52' 122.3(7) . . ? C48' C53' H53' 118.8 . . ? C52' C53' H53' 118.8 . . ? F8' C54' F9' 108.1(9) . . ? F8' C54' F7' 106.0(8) . . ? F9' C54' F7' 106.2(8) . . ? F8' C54' C50' 113.1(7) . . ? F9' C54' C50' 112.3(7) . . ? F7' C54' C50' 110.7(8) . . ? F11' C55' F10' 108.2(8) . . ? F11' C55' F12' 106.6(8) . . ? F10' C55' F12' 106.1(8) . . ? F11' C55' C52' 113.0(8) . . ? F10' C55' C52' 110.1(8) . . ? F12' C55' C52' 112.5(8) . . ? C61' C56' C57' 114.1(7) . . ? C61' C56' B1' 126.7(6) . . ? C57' C56' B1' 119.2(6) . . ? C58' C57' C56' 124.0(7) . . ? C58' C57' H57' 118.0 . . ? C56' C57' H57' 118.0 . . ? C59' C58' C57' 120.5(7) . . ? C59' C58' C62' 119.8(7) . . ? C57' C58' C62' 119.7(7) . . ? C58' C59' C60' 118.0(7) . . ? C58' C59' H59' 121.0 . . ? C60' C59' H59' 121.0 . . ? C61' C60' C59' 119.3(7) . . ? C61' C60' C63' 121.7(8) . . ? C59' C60' C63' 119.1(7) . . ? C60' C61' C56' 124.1(7) . . ? C60' C61' H61' 117.9 . . ? C56' C61' H61' 117.9 . . ? F15' C62' F14' 105.9(8) . . ? F15' C62' F13' 105.0(7) . . ? F14' C62' F13' 104.6(8) . . ? F15' C62' C58' 114.3(8) . . ? F14' C62' C58' 112.1(7) . . ? F13' C62' C58' 114.1(7) . . ? F18' C63' F17' 108.3(8) . . ? F18' C63' F16' 104.3(8) . . ? F17' C63' F16' 107.3(8) . . ? F18' C63' C60' 113.9(7) . . ? F17' C63' C60' 113.3(8) . . ? F16' C63' C60' 109.3(7) . . ? C69' C64' C65' 114.3(8) . . ? C69' C64' B1' 123.1(7) . . ? C65' C64' B1' 121.9(7) . . ? C66' C65' C64' 121.9(9) . . ? C66' C65' H65' 119.1 . . ? C64' C65' H65' 119.1 . . ? C67' C66' C65' 119.7(9) . . ? C67' C66' C70' 120.9(9) . . ? C65' C66' C70' 119.4(10) . . ? C68' C67' C66' 121.1(8) . . ? C68' C67' H67' 119.5 . . ? C66' C67' H67' 119.5 . . ? C67' C68' C69' 118.5(9) . . ? C67' C68' C71' 123.8(9) . . ? C69' C68' C71' 117.6(9) . . ? C64' C69' C68' 124.4(9) . . ? C64' C69' H69' 117.8 . . ? C68' C69' H69' 117.8 . . ? F21' C70' F20' 111.3(12) . . ? F21' C70' F19' 104.7(10) . . ? F20' C70' F19' 102.9(14) . . ? F21' C70' C66' 115.4(12) . . ? F20' C70' C66' 111.0(10) . . ? F19' C70' C66' 110.5(11) . . ? F23' C71' F22' 99.7(12) . . ? F23' C71' F24' 106.6(10) . . ? F22' C71' F24' 105.1(11) . . ? F23' C71' C68' 117.7(8) . . ? F22' C71' C68' 114.0(9) . . ? F24' C71' C68' 112.2(10) . . ? C77 C72 C73 116.4(19) . . ? C77 C72 C78 124.1(15) . . ? C73 C72 C78 119.5(16) . . ? C72 C73 C74 121.6(18) . . ? C72 C73 H73 119.2 . . ? C74 C73 H73 119.2 . . ? C73 C74 C75 121.4(17) . . ? C73 C74 H74 119.3 . . ? C75 C74 H74 119.3 . . ? C76 C75 C74 114.9(19) . . ? C76 C75 H75 122.6 . . ? C74 C75 H75 122.6 . . ? C75 C76 C77 121.1(19) . . ? C75 C76 H76 119.4 . . ? C77 C76 H76 119.4 . . ? C72 C77 C76 124.3(18) . . ? C72 C77 H77 117.9 . . ? C76 C77 H77 117.9 . . ? C72 C78 H78A 109.5 . . ? C72 C78 H78B 109.5 . . ? H78A C78 H78B 109.5 . . ? C72 C78 H78C 109.5 . . ? H78A C78 H78C 109.5 . . ? H78B C78 H78C 109.5 . . ? C85 C79 C80 129(2) . . ? C85 C79 C84 111(2) . . ? C80 C79 C84 120.0 . . ? C79 C80 C81 120.0 . . ? C79 C80 H80 120.0 . . ? C81 C80 H80 120.0 . . ? C82 C81 C80 120.0 . . ? C82 C81 H81 120.0 . . ? C80 C81 H81 120.0 . . ? C81 C82 C83 120.0 . . ? C81 C82 H82 120.0 . . ? C83 C82 H82 120.0 . . ? C84 C83 C82 120.0 . . ? C84 C83 H83 120.0 . . ? C82 C83 H83 120.0 . . ? C83 C84 C79 120.0 . . ? C83 C84 H84 120.0 . . ? C79 C84 H84 120.0 . . ? C79 C85 H85A 109.5 . . ? C79 C85 H85B 109.5 . . ? H85A C85 H85B 109.5 . . ? C79 C85 H85C 109.5 . . ? H85A C85 H85C 109.5 . . ? H85B C85 H85C 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 C8 C1 C2 C3 -0.4(19) . . . . ? Rh1 C1 C2 C3 -103.3(13) . . . . ? C8 C1 C2 Rh1 102.9(10) . . . . ? C1 C2 C3 C4 41.4(16) . . . . ? Rh1 C2 C3 C4 -43.5(11) . . . . ? C2 C3 C4 C5 37.0(14) . . . . ? C3 C4 C5 C6 -92.7(14) . . . . ? C3 C4 C5 Rh1 -13.4(12) . . . . ? C4 C5 C6 C7 -1.2(17) . . . . ? Rh1 C5 C6 C7 -102.5(9) . . . . ? C4 C5 C6 Rh1 101.3(12) . . . . ? C5 C6 C7 C8 48.3(14) . . . . ? Rh1 C6 C7 C8 -36.1(12) . . . . ? C6 C7 C8 C1 32.0(15) . . . . ? C2 C1 C8 C7 -89.1(14) . . . . ? Rh1 C1 C8 C7 -11.3(13) . . . . ? N1 C9 C11 N2 0.4(9) . . . . ? C25 C9 C11 N2 -171.8(8) . . . . ? N1 C9 C11 Rh1 -163.9(7) . . . . ? C25 C9 C11 Rh1 23.8(13) . . . . ? N2 C12 C13 C14 171.0(8) . . . . ? C17 C12 C13 C14 -62.5(11) . . . . ? C12 C13 C14 C15 59.3(12) . . . . ? C13 C14 C15 C16 -56.6(13) . . . . ? C14 C15 C16 C17 53.0(13) . . . . ? N2 C12 C17 N3 -49.9(10) . . . . ? C13 C12 C17 N3 -179.2(7) . . . . ? N2 C12 C17 C16 -171.7(8) . . . . ? C13 C12 C17 C16 59.1(11) . . . . ? C15 C16 C17 N3 -175.7(9) . . . . ? C15 C16 C17 C12 -52.3(12) . . . . ? N3 C18 C19 C24 80.2(10) . . . . ? N3 C18 C19 C20 -94.8(9) . . . . ? C24 C19 C20 C21 -0.2(14) . . . . ? C18 C19 C20 C21 174.9(9) . . . . ? C19 C20 C21 C22 -1.5(17) . . . . ? C20 C21 C22 C23 2.6(18) . . . . ? C21 C22 C23 C24 -2.0(17) . . . . ? C20 C19 C24 C23 0.8(15) . . . . ? C18 C19 C24 C23 -174.3(9) . . . . ? C22 C23 C24 C19 0.4(17) . . . . ? C11 C9 C25 C27 -129.4(10) . . . . ? N1 C9 C25 C27 59.7(13) . . . . ? C11 C9 C25 C26 102.5(11) . . . . ? N1 C9 C25 C26 -68.4(13) . . . . ? C33 C28 C29 C30 -2.1(14) . . . . ? N1 C28 C29 C30 -174.0(8) . . . . ? C28 C29 C30 C31 2.7(16) . . . . ? C29 C30 C31 C32 -2.2(18) . . . . ? C30 C31 C32 C33 1.2(18) . . . . ? C29 C28 C33 C32 1.1(14) . . . . ? N1 C28 C33 C32 173.0(9) . . . . ? C31 C32 C33 C28 -0.6(17) . . . . ? N1 C10 C34 C35 -90.7(11) . . . . ? N2 C10 C34 C35 84.2(11) . . . . ? N1 C10 C34 C39 87.5(12) . . . . ? N2 C10 C34 C39 -97.6(11) . . . . ? C39 C34 C35 C36 -1.9(15) . . . . ? C10 C34 C35 C36 176.3(9) . . . . ? C34 C35 C36 C37 4.8(15) . . . . ? C35 C36 C37 C38 -5.3(18) . . . . ? C36 C37 C38 C39 3(2) . . . . ? C35 C34 C39 C38 -0.6(17) . . . . ? C10 C34 C39 C38 -178.8(11) . . . . ? C37 C38 C39 C34 0(2) . . . . ? N2 C10 N1 C9 -0.3(9) . . . . ? C34 C10 N1 C9 175.4(8) . . . . ? N2 C10 N1 C28 -177.6(7) . . . . ? C34 C10 N1 C28 -2.0(13) . . . . ? C11 C9 N1 C10 -0.1(9) . . . . ? C25 C9 N1 C10 171.5(8) . . . . ? C11 C9 N1 C28 177.1(8) . . . . ? C25 C9 N1 C28 -11.3(14) . . . . ? C29 C28 N1 C10 102.6(10) . . . . ? C33 C28 N1 C10 -69.3(11) . . . . ? C29 C28 N1 C9 -74.1(11) . . . . ? C33 C28 N1 C9 114.0(10) . . . . ? C9 C11 N2 C10 -0.6(9) . . . . ? Rh1 C11 N2 C10 167.3(6) . . . . ? C9 C11 N2 C12 -174.5(7) . . . . ? Rh1 C11 N2 C12 -6.6(10) . . . . ? N1 C10 N2 C11 0.6(9) . . . . ? C34 C10 N2 C11 -175.1(8) . . . . ? N1 C10 N2 C12 173.3(8) . . . . ? C34 C10 N2 C12 -2.4(14) . . . . ? C13 C12 N2 C11 -159.4(8) . . . . ? C17 C12 N2 C11 73.0(10) . . . . ? C13 C12 N2 C10 28.3(13) . . . . ? C17 C12 N2 C10 -99.3(11) . . . . ? C12 C17 N3 C18 107.3(8) . . . . ? C16 C17 N3 C18 -131.1(8) . . . . ? C12 C17 N3 Rh1 -22.0(9) . . . . ? C16 C17 N3 Rh1 99.6(8) . . . . ? C19 C18 N3 C17 166.2(7) . . . . ? C19 C18 N3 Rh1 -65.4(8) . . . . ? C9 C11 Rh1 C2 -100.8(10) . . . . ? N2 C11 Rh1 C2 96.2(7) . . . . ? C9 C11 Rh1 C1 -62.2(10) . . . . ? N2 C11 Rh1 C1 134.8(7) . . . . ? C9 C11 Rh1 C6 29.8(19) . . . . ? N2 C11 Rh1 C6 -133.1(12) . . . . ? C9 C11 Rh1 N3 114.6(9) . . . . ? N2 C11 Rh1 N3 -48.3(6) . . . . ? C9 C11 Rh1 C5 -175.8(10) . . . . ? N2 C11 Rh1 C5 21.3(16) . . . . ? C1 C2 Rh1 C11 100.6(7) . . . . ? C3 C2 Rh1 C11 -133.1(9) . . . . ? C3 C2 Rh1 C1 126.3(12) . . . . ? C1 C2 Rh1 C6 -66.4(8) . . . . ? C3 C2 Rh1 C6 59.9(9) . . . . ? C1 C2 Rh1 N3 -178.0(6) . . . . ? C3 C2 Rh1 N3 -51.7(12) . . . . ? C1 C2 Rh1 C5 -98.2(8) . . . . ? C3 C2 Rh1 C5 28.1(9) . . . . ? C2 C1 Rh1 C11 -84.3(8) . . . . ? C8 C1 Rh1 C11 156.4(8) . . . . ? C8 C1 Rh1 C2 -119.3(12) . . . . ? C2 C1 Rh1 C6 113.0(8) . . . . ? C8 C1 Rh1 C6 -6.3(9) . . . . ? C2 C1 Rh1 N3 160(6) . . . . ? C8 C1 Rh1 N3 41(7) . . . . ? C2 C1 Rh1 C5 78.1(8) . . . . ? C8 C1 Rh1 C5 -41.2(9) . . . . ? C5 C6 Rh1 C11 165.7(11) . . . . ? C7 C6 Rh1 C11 -72.7(16) . . . . ? C5 C6 Rh1 C2 -63.9(8) . . . . ? C7 C6 Rh1 C2 57.6(9) . . . . ? C5 C6 Rh1 C1 -99.4(7) . . . . ? C7 C6 Rh1 C1 22.2(8) . . . . ? C5 C6 Rh1 N3 83.2(7) . . . . ? C7 C6 Rh1 N3 -155.3(8) . . . . ? C7 C6 Rh1 C5 121.5(11) . . . . ? C17 N3 Rh1 C11 63.0(6) . . . . ? C18 N3 Rh1 C11 -66.2(6) . . . . ? C17 N3 Rh1 C2 -22.4(10) . . . . ? C18 N3 Rh1 C2 -151.5(8) . . . . ? C17 N3 Rh1 C1 179(100) . . . . ? C18 N3 Rh1 C1 50(7) . . . . ? C17 N3 Rh1 C6 -134.2(6) . . . . ? C18 N3 Rh1 C6 96.7(6) . . . . ? C17 N3 Rh1 C5 -99.0(7) . . . . ? C18 N3 Rh1 C5 131.9(7) . . . . ? C6 C5 Rh1 C11 -167.4(10) . . . . ? C4 C5 Rh1 C11 69.7(14) . . . . ? C6 C5 Rh1 C2 115.5(7) . . . . ? C4 C5 Rh1 C2 -7.4(8) . . . . ? C6 C5 Rh1 C1 77.3(7) . . . . ? C4 C5 Rh1 C1 -45.7(9) . . . . ? C4 C5 Rh1 C6 -122.9(11) . . . . ? C6 C5 Rh1 N3 -99.3(7) . . . . ? C4 C5 Rh1 N3 137.7(8) . . . . ? C64 B1 C40 C41 85.5(9) . . . . ? C56 B1 C40 C41 -153.0(7) . . . . ? C48 B1 C40 C41 -38.4(10) . . . . ? C64 B1 C40 C45 -87.0(8) . . . . ? C56 B1 C40 C45 34.4(11) . . . . ? C48 B1 C40 C45 149.0(7) . . . . ? C45 C40 C41 C42 -1.5(11) . . . . ? B1 C40 C41 C42 -174.5(8) . . . . ? C40 C41 C42 C43 1.4(13) . . . . ? C40 C41 C42 C46 -178.2(8) . . . . ? C41 C42 C43 C44 0.9(12) . . . . ? C46 C42 C43 C44 -179.6(8) . . . . ? C42 C43 C44 C45 -2.8(13) . . . . ? C42 C43 C44 C47 178.3(8) . . . . ? C43 C44 C45 C40 2.7(14) . . . . ? C47 C44 C45 C40 -178.4(8) . . . . ? C41 C40 C45 C44 -0.5(12) . . . . ? B1 C40 C45 C44 172.7(8) . . . . ? C43 C42 C46 F1 -25.7(12) . . . . ? C41 C42 C46 F1 153.9(8) . . . . ? C43 C42 C46 F3 97.1(10) . . . . ? C41 C42 C46 F3 -83.3(11) . . . . ? C43 C42 C46 F2 -147.3(8) . . . . ? C41 C42 C46 F2 32.3(12) . . . . ? C43 C44 C47 F4 -65(3) . . . . ? C45 C44 C47 F4 116(3) . . . . ? C43 C44 C47 F5A 119(2) . . . . ? C45 C44 C47 F5A -60(3) . . . . ? C43 C44 C47 F6A -6(2) . . . . ? C45 C44 C47 F6A 175(2) . . . . ? C43 C44 C47 F4A -122.8(17) . . . . ? C45 C44 C47 F4A 58.2(18) . . . . ? C43 C44 C47 F5 166.4(18) . . . . ? C45 C44 C47 F5 -12(2) . . . . ? C43 C44 C47 F6 58.5(18) . . . . ? C45 C44 C47 F6 -120.4(17) . . . . ? C64 B1 C48 C53 41.1(9) . . . . ? C40 B1 C48 C53 161.3(7) . . . . ? C56 B1 C48 C53 -78.8(9) . . . . ? C64 B1 C48 C49 -146.0(7) . . . . ? C40 B1 C48 C49 -25.9(10) . . . . ? C56 B1 C48 C49 94.0(8) . . . . ? C53 C48 C49 C50 -3.8(11) . . . . ? B1 C48 C49 C50 -177.0(8) . . . . ? C48 C49 C50 C51 -0.1(13) . . . . ? C48 C49 C50 C54 179.7(8) . . . . ? C49 C50 C51 C52 2.5(14) . . . . ? C54 C50 C51 C52 -177.3(9) . . . . ? C50 C51 C52 C53 -0.8(14) . . . . ? C50 C51 C52 C55 175.1(11) . . . . ? C51 C52 C53 C48 -3.4(15) . . . . ? C55 C52 C53 C48 -179.3(10) . . . . ? C49 C48 C53 C52 5.6(12) . . . . ? B1 C48 C53 C52 179.0(8) . . . . ? C49 C50 C54 F7 -67.6(13) . . . . ? C51 C50 C54 F7 112.2(11) . . . . ? C49 C50 C54 F9 169.0(10) . . . . ? C51 C50 C54 F9 -11.1(14) . . . . ? C49 C50 C54 F8 52.1(13) . . . . ? C51 C50 C54 F8 -128.1(11) . . . . ? C51 C52 C55 F11 169(2) . . . . ? C53 C52 C55 F11 -15(3) . . . . ? C51 C52 C55 F12 -55(2) . . . . ? C53 C52 C55 F12 121.0(17) . . . . ? C51 C52 C55 F12A 12(3) . . . . ? C53 C52 C55 F12A -172(2) . . . . ? C51 C52 C55 F11A -116(3) . . . . ? C53 C52 C55 F11A 60(3) . . . . ? C51 C52 C55 F10A 123(3) . . . . ? C53 C52 C55 F10A -61(3) . . . . ? C51 C52 C55 F10 53(2) . . . . ? C53 C52 C55 F10 -131.1(19) . . . . ? C64 B1 C56 C61 162.8(8) . . . . ? C40 B1 C56 C61 44.4(11) . . . . ? C48 B1 C56 C61 -76.1(9) . . . . ? C64 B1 C56 C57 -22.8(11) . . . . ? C40 B1 C56 C57 -141.3(8) . . . . ? C48 B1 C56 C57 98.2(9) . . . . ? C61 C56 C57 C58 -0.4(13) . . . . ? B1 C56 C57 C58 -175.2(8) . . . . ? C56 C57 C58 C59 -0.2(14) . . . . ? C56 C57 C58 C62 -179.5(9) . . . . ? C57 C58 C59 C60 0.1(14) . . . . ? C62 C58 C59 C60 179.3(10) . . . . ? C58 C59 C60 C61 0.7(15) . . . . ? C58 C59 C60 C63 -176.7(11) . . . . ? C59 C60 C61 C56 -1.3(16) . . . . ? C63 C60 C61 C56 176.0(11) . . . . ? C57 C56 C61 C60 1.1(14) . . . . ? B1 C56 C61 C60 176.1(9) . . . . ? C57 C58 C62 F14 54.9(14) . . . . ? C59 C58 C62 F14 -124.4(12) . . . . ? C57 C58 C62 F13 179.7(10) . . . . ? C59 C58 C62 F13 0.4(16) . . . . ? C57 C58 C62 F15 -57.8(14) . . . . ? C59 C58 C62 F15 123.0(11) . . . . ? C59 C60 C63 F16 97.3(16) . . . . ? C61 C60 C63 F16 -80.0(18) . . . . ? C59 C60 C63 F17 -32.4(18) . . . . ? C61 C60 C63 F17 150.3(12) . . . . ? C59 C60 C63 F18 -144.7(11) . . . . ? C61 C60 C63 F18 38.0(17) . . . . ? C40 B1 C64 C69 67.2(8) . . . . ? C56 B1 C64 C69 -54.4(9) . . . . ? C48 B1 C64 C69 -169.1(6) . . . . ? C40 B1 C64 C65 -104.4(8) . . . . ? C56 B1 C64 C65 134.0(8) . . . . ? C48 B1 C64 C65 19.3(10) . . . . ? C69 C64 C65 C66 3.9(11) . . . . ? B1 C64 C65 C66 175.9(7) . . . . ? C64 C65 C66 C67 -3.6(12) . . . . ? C64 C65 C66 C70 174.1(7) . . . . ? C65 C66 C67 C68 0.7(12) . . . . ? C70 C66 C67 C68 -177.0(8) . . . . ? C66 C67 C68 C69 1.5(12) . . . . ? C66 C67 C68 C71 179.2(8) . . . . ? C67 C68 C69 C64 -1.0(12) . . . . ? C71 C68 C69 C64 -178.8(7) . . . . ? C65 C64 C69 C68 -1.7(11) . . . . ? B1 C64 C69 C68 -174.2(7) . . . . ? C67 C66 C70 F20 113.5(9) . . . . ? C65 C66 C70 F20 -64.2(11) . . . . ? C67 C66 C70 F21 -6.9(12) . . . . ? C65 C66 C70 F21 175.3(8) . . . . ? C67 C66 C70 F19 -126.4(9) . . . . ? C65 C66 C70 F19 55.8(11) . . . . ? C69 C68 C71 F24 -172.6(8) . . . . ? C67 C68 C71 F24 9.6(12) . . . . ? C69 C68 C71 F23 64.7(11) . . . . ? C67 C68 C71 F23 -113.1(9) . . . . ? C69 C68 C71 F22 -52.4(10) . . . . ? C67 C68 C71 F22 129.8(8) . . . . ? C8' C1' C2' C3' 7.7(14) . . . . ? Rh1' C1' C2' C3' -100.0(9) . . . . ? C8' C1' C2' Rh1' 107.7(8) . . . . ? C1' C2' C3' C4' 41.8(13) . . . . ? Rh1' C2' C3' C4' -38.2(10) . . . . ? C2' C3' C4' C5' 33.8(13) . . . . ? C3' C4' C5' C6' -92.8(12) . . . . ? C3' C4' C5' Rh1' -12.7(11) . . . . ? C4' C5' C6' C7' 1.6(13) . . . . ? Rh1' C5' C6' C7' -100.6(7) . . . . ? C4' C5' C6' Rh1' 102.2(8) . . . . ? C5' C6' C7' C8' 48.2(12) . . . . ? Rh1' C6' C7' C8' -32.9(10) . . . . ? C6' C7' C8' C1' 28.9(13) . . . . ? C2' C1' C8' C7' -93.2(12) . . . . ? Rh1' C1' C8' C7' -10.0(12) . . . . ? N1' C10' C11' N2' -1.3(8) . . . . ? C34' C10' C11' N2' -178.1(7) . . . . ? N1' C10' C11' C28' 174.7(7) . . . . ? C34' C10' C11' C28' -2.2(13) . . . . ? N2' C12' C13' C14' 169.0(7) . . . . ? C17' C12' C13' C14' -59.3(9) . . . . ? C12' C13' C14' C15' 59.9(9) . . . . ? C13' C14' C15' C16' -57.7(9) . . . . ? C14' C15' C16' C17' 52.3(9) . . . . ? N2' C12' C17' N3' -46.9(9) . . . . ? C13' C12' C17' N3' 179.1(6) . . . . ? N2' C12' C17' C16' -171.3(6) . . . . ? C13' C12' C17' C16' 54.7(9) . . . . ? C15' C16' C17' C12' -50.3(9) . . . . ? C15' C16' C17' N3' -174.6(7) . . . . ? N3' C18' C19' C24' 85.2(9) . . . . ? N3' C18' C19' C20' -86.9(9) . . . . ? C24' C19' C20' C21' -0.4(12) . . . . ? C18' C19' C20' C21' 172.2(8) . . . . ? C19' C20' C21' C22' -0.6(13) . . . . ? C20' C21' C22' C23' 0.9(14) . . . . ? C21' C22' C23' C24' -0.1(14) . . . . ? C20' C19' C24' C23' 1.1(12) . . . . ? C18' C19' C24' C23' -171.1(8) . . . . ? C22' C23' C24' C19' -0.9(13) . . . . ? C10' C11' C28' C29' -103.9(10) . . . . ? N2' C11' C28' C29' 71.3(11) . . . . ? C10' C11' C28' C33' 75.1(11) . . . . ? N2' C11' C28' C33' -109.7(9) . . . . ? C33' C28' C29' C30' 6.0(13) . . . . ? C11' C28' C29' C30' -175.0(8) . . . . ? C28' C29' C30' C31' -6.6(14) . . . . ? C29' C30' C31' C32' 2.1(15) . . . . ? C30' C31' C32' C33' 2.7(15) . . . . ? C29' C28' C33' C32' -1.1(12) . . . . ? C11' C28' C33' C32' 179.9(8) . . . . ? C31' C32' C33' C28' -3.1(14) . . . . ? C11' C10' C34' C35' 84.3(11) . . . . ? N1' C10' C34' C35' -92.0(10) . . . . ? C11' C10' C34' C39' -91.7(11) . . . . ? N1' C10' C34' C39' 92.0(11) . . . . ? C39' C34' C35' C36' 1.1(14) . . . . ? C10' C34' C35' C36' -174.9(8) . . . . ? C34' C35' C36' C37' -1.1(15) . . . . ? C35' C36' C37' C38' 1.0(16) . . . . ? C36' C37' C38' C39' -1.1(19) . . . . ? C37' C38' C39' C34' 1.1(19) . . . . ? C35' C34' C39' C38' -1.1(16) . . . . ? C10' C34' C39' C38' 174.9(10) . . . . ? N2' C9' N1' C10' 0.7(8) . . . . ? Rh1' C9' N1' C10' -167.7(6) . . . . ? N2' C9' N1' C25' -177.3(7) . . . . ? Rh1' C9' N1' C25' 14.2(11) . . . . ? C11' C10' N1' C9' 0.4(8) . . . . ? C34' C10' N1' C9' 177.2(7) . . . . ? C11' C10' N1' C25' 178.3(7) . . . . ? C34' C10' N1' C25' -4.9(12) . . . . ? C27' C25' N1' C9' -131.2(8) . . . . ? C26' C25' N1' C9' 100.0(9) . . . . ? C27' C25' N1' C10' 51.1(11) . . . . ? C26' C25' N1' C10' -77.7(10) . . . . ? N1' C9' N2' C11' -1.5(8) . . . . ? Rh1' C9' N2' C11' 169.7(5) . . . . ? N1' C9' N2' C12' -179.3(6) . . . . ? Rh1' C9' N2' C12' -8.1(9) . . . . ? C10' C11' N2' C9' 1.8(8) . . . . ? C28' C11' N2' C9' -174.3(7) . . . . ? C10' C11' N2' C12' 179.3(7) . . . . ? C28' C11' N2' C12' 3.2(13) . . . . ? C17' C12' N2' C9' 73.2(9) . . . . ? C13' C12' N2' C9' -154.7(7) . . . . ? C17' C12' N2' C11' -104.1(9) . . . . ? C13' C12' N2' C11' 28.0(12) . . . . ? C19' C18' N3' C17' 169.2(7) . . . . ? C19' C18' N3' Rh1' -61.0(7) . . . . ? C12' C17' N3' C18' 106.2(8) . . . . ? C16' C17' N3' C18' -129.8(7) . . . . ? C12' C17' N3' Rh1' -23.6(8) . . . . ? C16' C17' N3' Rh1' 100.5(7) . . . . ? N2' C9' Rh1' C1' 139.6(6) . . . . ? N1' C9' Rh1' C1' -52.6(8) . . . . ? N2' C9' Rh1' C2' 102.1(6) . . . . ? N1' C9' Rh1' C2' -90.2(8) . . . . ? N2' C9' Rh1' C6' -125.6(10) . . . . ? N1' C9' Rh1' C6' 42.2(14) . . . . ? N2' C9' Rh1' C5' 24.5(11) . . . . ? N1' C9' Rh1' C5' -167.7(8) . . . . ? N2' C9' Rh1' N3' -45.4(5) . . . . ? N1' C9' Rh1' N3' 122.4(8) . . . . ? C2' C1' Rh1' C9' -83.5(5) . . . . ? C8' C1' Rh1' C9' 157.9(8) . . . . ? C8' C1' Rh1' C2' -118.6(10) . . . . ? C2' C1' Rh1' C6' 112.5(6) . . . . ? C8' C1' Rh1' C6' -6.1(8) . . . . ? C2' C1' Rh1' C5' 76.8(5) . . . . ? C8' C1' Rh1' C5' -41.8(8) . . . . ? C2' C1' Rh1' N3' 165(3) . . . . ? C8' C1' Rh1' N3' 46(4) . . . . ? C1' C2' Rh1' C9' 101.4(5) . . . . ? C3' C2' Rh1' C9' -134.8(7) . . . . ? C3' C2' Rh1' C1' 123.8(9) . . . . ? C1' C2' Rh1' C6' -66.8(5) . . . . ? C3' C2' Rh1' C6' 56.9(7) . . . . ? C1' C2' Rh1' C5' -100.1(5) . . . . ? C3' C2' Rh1' C5' 23.6(7) . . . . ? C1' C2' Rh1' N3' -177.4(5) . . . . ? C3' C2' Rh1' N3' -53.7(10) . . . . ? C5' C6' Rh1' C9' 161.8(9) . . . . ? C7' C6' Rh1' C9' -77.0(12) . . . . ? C5' C6' Rh1' C1' -100.7(6) . . . . ? C7' C6' Rh1' C1' 20.4(6) . . . . ? C5' C6' Rh1' C2' -66.1(6) . . . . ? C7' C6' Rh1' C2' 55.1(7) . . . . ? C7' C6' Rh1' C5' 121.2(8) . . . . ? C5' C6' Rh1' N3' 83.5(5) . . . . ? C7' C6' Rh1' N3' -155.3(6) . . . . ? C6' C5' Rh1' C9' -166.7(7) . . . . ? C4' C5' Rh1' C9' 73.4(11) . . . . ? C6' C5' Rh1' C1' 76.3(5) . . . . ? C4' C5' Rh1' C1' -43.6(7) . . . . ? C6' C5' Rh1' C2' 113.3(6) . . . . ? C4' C5' Rh1' C2' -6.6(7) . . . . ? C4' C5' Rh1' C6' -119.9(9) . . . . ? C6' C5' Rh1' N3' -98.4(5) . . . . ? C4' C5' Rh1' N3' 141.7(7) . . . . ? C18' N3' Rh1' C9' -67.6(6) . . . . ? C17' N3' Rh1' C9' 62.4(5) . . . . ? C18' N3' Rh1' C1' 45(3) . . . . ? C17' N3' Rh1' C1' 175(11) . . . . ? C18' N3' Rh1' C2' -152.4(6) . . . . ? C17' N3' Rh1' C2' -22.4(8) . . . . ? C18' N3' Rh1' C6' 96.7(6) . . . . ? C17' N3' Rh1' C6' -133.3(5) . . . . ? C18' N3' Rh1' C5' 132.9(6) . . . . ? C17' N3' Rh1' C5' -97.1(5) . . . . ? C64' B1' C40' C41' -69.9(8) . . . . ? C56' B1' C40' C41' 46.9(9) . . . . ? C48' B1' C40' C41' 167.0(7) . . . . ? C64' B1' C40' C45' 103.8(8) . . . . ? C56' B1' C40' C45' -139.4(7) . . . . ? C48' B1' C40' C45' -19.3(11) . . . . ? C45' C40' C41' C42' 1.7(11) . . . . ? B1' C40' C41' C42' 176.1(7) . . . . ? C40' C41' C42' C43' -2.0(13) . . . . ? C40' C41' C42' C46' 178.5(8) . . . . ? C41' C42' C43' C44' 1.2(13) . . . . ? C46' C42' C43' C44' -179.3(8) . . . . ? C42' C43' C44' C45' -0.2(12) . . . . ? C42' C43' C44' C47' -179.8(8) . . . . ? C43' C44' C45' C40' 0.0(12) . . . . ? C47' C44' C45' C40' 179.6(7) . . . . ? C41' C40' C45' C44' -0.8(11) . . . . ? B1' C40' C45' C44' -174.8(7) . . . . ? C43' C42' C46' F3' -8.9(16) . . . . ? C41' C42' C46' F3' 170.5(11) . . . . ? C43' C42' C46' F2' 119.2(10) . . . . ? C41' C42' C46' F2' -61.3(13) . . . . ? C43' C42' C46' F1' -132.1(10) . . . . ? C41' C42' C46' F1' 47.4(12) . . . . ? C43' C44' C47' F6' -3.9(12) . . . . ? C45' C44' C47' F6' 176.5(8) . . . . ? C43' C44' C47' F4' -125.5(9) . . . . ? C45' C44' C47' F4' 54.9(11) . . . . ? C43' C44' C47' F5' 116.5(9) . . . . ? C45' C44' C47' F5' -63.1(10) . . . . ? C40' B1' C48' C53' -42.1(10) . . . . ? C64' B1' C48' C53' -161.0(7) . . . . ? C56' B1' C48' C53' 82.8(8) . . . . ? C40' B1' C48' C49' 142.5(7) . . . . ? C64' B1' C48' C49' 23.6(10) . . . . ? C56' B1' C48' C49' -92.6(8) . . . . ? C53' C48' C49' C50' 1.1(11) . . . . ? B1' C48' C49' C50' 176.8(7) . . . . ? C48' C49' C50' C51' 0.2(12) . . . . ? C48' C49' C50' C54' 177.1(7) . . . . ? C49' C50' C51' C52' 0.7(12) . . . . ? C54' C50' C51' C52' -176.2(7) . . . . ? C50' C51' C52' C53' -2.9(12) . . . . ? C50' C51' C52' C55' -179.0(8) . . . . ? C49' C48' C53' C52' -3.3(11) . . . . ? B1' C48' C53' C52' -179.1(8) . . . . ? C51' C52' C53' C48' 4.5(13) . . . . ? C55' C52' C53' C48' -179.4(8) . . . . ? C51' C50' C54' F8' 94.1(10) . . . . ? C49' C50' C54' F8' -82.9(10) . . . . ? C51' C50' C54' F9' -143.2(9) . . . . ? C49' C50' C54' F9' 39.8(12) . . . . ? C51' C50' C54' F7' -24.7(11) . . . . ? C49' C50' C54' F7' 158.3(8) . . . . ? C51' C52' C55' F11' 94.0(10) . . . . ? C53' C52' C55' F11' -82.2(12) . . . . ? C51' C52' C55' F10' -27.1(12) . . . . ? C53' C52' C55' F10' 156.6(9) . . . . ? C51' C52' C55' F12' -145.2(8) . . . . ? C53' C52' C55' F12' 38.5(11) . . . . ? C40' B1' C56' C61' 18.4(10) . . . . ? C64' B1' C56' C61' 133.3(7) . . . . ? C48' B1' C56' C61' -107.4(8) . . . . ? C40' B1' C56' C57' -164.5(7) . . . . ? C64' B1' C56' C57' -49.6(9) . . . . ? C48' B1' C56' C57' 69.6(8) . . . . ? C61' C56' C57' C58' -2.7(11) . . . . ? B1' C56' C57' C58' 179.9(7) . . . . ? C56' C57' C58' C59' 0.9(12) . . . . ? C56' C57' C58' C62' -178.0(7) . . . . ? C57' C58' C59' C60' -0.3(11) . . . . ? C62' C58' C59' C60' 178.7(7) . . . . ? C58' C59' C60' C61' 1.6(11) . . . . ? C58' C59' C60' C63' -177.5(7) . . . . ? C59' C60' C61' C56' -3.8(11) . . . . ? C63' C60' C61' C56' 175.3(7) . . . . ? C57' C56' C61' C60' 4.2(11) . . . . ? B1' C56' C61' C60' -178.6(7) . . . . ? C59' C58' C62' F15' 5.7(11) . . . . ? C57' C58' C62' F15' -175.4(7) . . . . ? C59' C58' C62' F14' -114.8(9) . . . . ? C57' C58' C62' F14' 64.1(11) . . . . ? C59' C58' C62' F13' 126.6(8) . . . . ? C57' C58' C62' F13' -54.5(11) . . . . ? C61' C60' C63' F18' 61.5(11) . . . . ? C59' C60' C63' F18' -119.4(8) . . . . ? C61' C60' C63' F17' -174.2(8) . . . . ? C59' C60' C63' F17' 4.8(11) . . . . ? C61' C60' C63' F16' -54.7(10) . . . . ? C59' C60' C63' F16' 124.4(9) . . . . ? C40' B1' C64' C69' 86.3(9) . . . . ? C56' B1' C64' C69' -34.5(9) . . . . ? C48' B1' C64' C69' -148.8(7) . . . . ? C40' B1' C64' C65' -83.9(8) . . . . ? C56' B1' C64' C65' 155.3(7) . . . . ? C48' B1' C64' C65' 41.0(10) . . . . ? C69' C64' C65' C66' 5.1(12) . . . . ? B1' C64' C65' C66' 176.1(8) . . . . ? C64' C65' C66' C67' -3.2(13) . . . . ? C64' C65' C66' C70' 175.6(9) . . . . ? C65' C66' C67' C68' 0.2(13) . . . . ? C70' C66' C67' C68' -178.6(10) . . . . ? C66' C67' C68' C69' 0.6(13) . . . . ? C66' C67' C68' C71' -177.4(9) . . . . ? C65' C64' C69' C68' -4.4(12) . . . . ? B1' C64' C69' C68' -175.3(8) . . . . ? C67' C68' C69' C64' 1.7(13) . . . . ? C71' C68' C69' C64' 179.9(8) . . . . ? C67' C66' C70' F21' -9.8(17) . . . . ? C65' C66' C70' F21' 171.4(10) . . . . ? C67' C66' C70' F20' 118.1(14) . . . . ? C65' C66' C70' F20' -60.7(18) . . . . ? C67' C66' C70' F19' -128.3(11) . . . . ? C65' C66' C70' F19' 52.9(13) . . . . ? C67' C68' C71' F23' 127.6(11) . . . . ? C69' C68' C71' F23' -50.5(14) . . . . ? C67' C68' C71' F22' -116.1(12) . . . . ? C69' C68' C71' F22' 65.9(13) . . . . ? C67' C68' C71' F24' 3.2(16) . . . . ? C69' C68' C71' F24' -174.8(11) . . . . ? C77 C72 C73 C74 1(2) . . . . ? C78 C72 C73 C74 -179.9(14) . . . . ? C72 C73 C74 C75 -6(2) . . . . ? C73 C74 C75 C76 7(2) . . . . ? C74 C75 C76 C77 -2(3) . . . . ? C73 C72 C77 C76 3(2) . . . . ? C78 C72 C77 C76 -175.8(15) . . . . ? C75 C76 C77 C72 -2(3) . . . . ? C85 C79 C80 C81 -171(3) . . . . ? C84 C79 C80 C81 0.0 . . . . ? C79 C80 C81 C82 0.0 . . . . ? C80 C81 C82 C83 0.0 . . . . ? C81 C82 C83 C84 0.0 . . . . ? C82 C83 C84 C79 0.0 . . . . ? C85 C79 C84 C83 173(2) . . . . ? C80 C79 C84 C83 0.0 . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 22.55 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.975 _refine_diff_density_min -0.989 _refine_diff_density_rms 0.092 #====END====#