# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _publ_contact_author G.K.Fukin _publ_contact_author_email gera@iomc.ras.ru _publ_contact_author_name G.K.Fukin loop_ _publ_author_name 'Charlotte E. Willans' 'Mikhail A. Sinenkov' 'Georgy K. Fukin' 'Kristina Sheridan' 'Jason M. Lynam' ; A.A.Trifonov ; 'Francesca M. Kerton' data_ynoclm _database_code_depnum_ccdc_archive 'CCDC 676933' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H62 Cl N2 O3 Y' _chemical_formula_weight 719.26 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' Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 48.5157(14) _cell_length_b 11.9131(3) _cell_length_c 35.9372(10) _cell_angle_alpha 90.00 _cell_angle_beta 130.9340(10) _cell_angle_gamma 90.00 _cell_volume 15691.5(7) _cell_formula_units_Z 16 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 900 _cell_measurement_theta_min 2 _cell_measurement_theta_max 58 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.218 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6144 _exptl_absorpt_coefficient_mu 1.590 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6557 _exptl_absorpt_correction_T_max 0.7113 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1998a)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type '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 46613 _diffrn_reflns_av_R_equivalents 0.0436 _diffrn_reflns_av_sigmaI/netI 0.0515 _diffrn_reflns_limit_h_min -59 _diffrn_reflns_limit_h_max 44 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -44 _diffrn_reflns_limit_l_max 44 _diffrn_reflns_theta_min 1.68 _diffrn_reflns_theta_max 26.00 _reflns_number_total 15386 _reflns_number_gt 10955 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _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^)+(0.0477P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 15386 _refine_ls_number_parameters 839 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0701 _refine_ls_R_factor_gt 0.0398 _refine_ls_wR_factor_ref 0.0894 _refine_ls_wR_factor_gt 0.0820 _refine_ls_goodness_of_fit_ref 0.981 _refine_ls_restrained_S_all 0.980 _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 Y1A Y 0.143284(3) -0.087652(11) -0.000210(4) 0.01711(4) Uani 1 1 d . . . O1A O 0.15554(2) 0.00439(8) -0.04562(3) 0.0224(3) Uani 1 1 d . . . N1A N 0.07611(3) -0.12606(10) -0.05310(4) 0.0175(3) Uani 1 1 d . . . C1A C 0.16437(3) 0.12454(12) -0.03877(5) 0.0230(4) Uani 1 1 d . . . H1AA H 0.1764 0.1478 -0.0047 0.028 Uiso 1 1 calc R . . H1AB H 0.1420 0.1699 -0.0620 0.028 Uiso 1 1 calc R . . Cl1A Cl 0.211187(9) -0.08192(3) 0.077862(12) 0.02776(11) Uani 1 1 d . . . N2A N 0.13211(3) -0.20275(10) 0.04871(4) 0.0228(3) Uani 1 1 d . . . C2A C 0.18987(3) 0.13958(12) -0.04892(5) 0.0239(4) Uani 1 1 d . . . H2AA H 0.2081 0.1989 -0.0277 0.029 Uiso 1 1 calc R . . H2AB H 0.1762 0.1591 -0.0839 0.029 Uiso 1 1 calc R . . O2A O 0.12392(2) 0.07006(8) 0.00290(3) 0.0205(3) Uani 1 1 d . . . C3A C 0.20797(3) 0.02518(13) -0.03655(5) 0.0272(4) Uani 1 1 d . . . H3AA H 0.2178 0.0132 -0.0532 0.033 Uiso 1 1 calc R . . H3AB H 0.2279 0.0157 -0.0006 0.033 Uiso 1 1 calc R . . O3A O 0.13926(2) -0.23455(8) -0.03812(3) 0.0232(3) Uani 1 1 d . . . C4A C 0.17667(4) -0.05219(13) -0.05623(5) 0.0329(4) Uani 1 1 d . . . H4AA H 0.1616 -0.0635 -0.0921 0.040 Uiso 1 1 calc R . . H4AB H 0.1856 -0.1261 -0.0396 0.040 Uiso 1 1 calc R . . C5A C 0.06522(3) -0.19115(12) -0.09681(4) 0.0206(4) Uani 1 1 d . . . H5AA H 0.0734 -0.1488 -0.1118 0.025 Uiso 1 1 calc R . . H5AB H 0.0383 -0.1948 -0.1215 0.025 Uiso 1 1 calc R . . C6A C 0.07987(3) -0.30896(12) -0.08662(4) 0.0183(4) Uani 1 1 d . . . C7A C 0.05641(3) -0.39969(12) -0.10544(4) 0.0193(4) Uani 1 1 d . . . H7AA H 0.0313 -0.3871 -0.1229 0.023 Uiso 1 1 calc R . . C8A C 0.06891(3) -0.50935(12) -0.09936(4) 0.0185(4) Uani 1 1 d . . . C9A C 0.04224(3) -0.60831(12) -0.11853(5) 0.0231(4) Uani 1 1 d . . . C10A C 0.00926(4) -0.59156(13) -0.17362(5) 0.0326(5) Uani 1 1 d . . . H10A H -0.0025 -0.5198 -0.1784 0.049 Uiso 1 1 calc R . . H10B H -0.0082 -0.6528 -0.1853 0.049 Uiso 1 1 calc R . . H10C H 0.0175 -0.5914 -0.1923 0.049 Uiso 1 1 calc R . . C11A C 0.05982(4) -0.72088(12) -0.11260(5) 0.0285(5) Uani 1 1 d . . . H11A H 0.0686 -0.7191 -0.1305 0.043 Uiso 1 1 calc R . . H11B H 0.0418 -0.7809 -0.1258 0.043 Uiso 1 1 calc R . . H11C H 0.0804 -0.7348 -0.0776 0.043 Uiso 1 1 calc R . . C12A C 0.02850(4) -0.61234(14) -0.09055(5) 0.0323(5) Uani 1 1 d . . . H12A H 0.0172 -0.5404 -0.0942 0.048 Uiso 1 1 calc R . . H12B H 0.0490 -0.6267 -0.0556 0.048 Uiso 1 1 calc R . . H12C H 0.0105 -0.6726 -0.1040 0.048 Uiso 1 1 calc R . . C13A C 0.10572(3) -0.52235(12) -0.07518(4) 0.0197(4) Uani 1 1 d . . . H13A H 0.1145 -0.5963 -0.0717 0.024 Uiso 1 1 calc R . . C14A C 0.13065(3) -0.43383(12) -0.05568(4) 0.0189(4) Uani 1 1 d . . . C15A C 0.17056(3) -0.45347(13) -0.03242(5) 0.0240(4) Uani 1 1 d . . . C16A C 0.17823(3) -0.57716(12) -0.03471(5) 0.0277(4) Uani 1 1 d . . . H16A H 0.1741 -0.6230 -0.0161 0.041 Uiso 1 1 calc R . . H16B H 0.2036 -0.5854 -0.0204 0.041 Uiso 1 1 calc R . . H16C H 0.1619 -0.6020 -0.0691 0.041 Uiso 1 1 calc R . . C17A C 0.19744(4) -0.41811(14) 0.02197(5) 0.0316(5) Uani 1 1 d . . . H17A H 0.1934 -0.3390 0.0247 0.047 Uiso 1 1 calc R . . H17B H 0.2225 -0.4282 0.0352 0.047 Uiso 1 1 calc R . . H17C H 0.1935 -0.4645 0.0407 0.047 Uiso 1 1 calc R . . C18A C 0.17773(4) -0.38606(13) -0.06191(5) 0.0329(5) Uani 1 1 d . . . H18A H 0.1733 -0.3062 -0.0612 0.049 Uiso 1 1 calc R . . H18B H 0.1614 -0.4124 -0.0961 0.049 Uiso 1 1 calc R . . H18C H 0.2031 -0.3967 -0.0472 0.049 Uiso 1 1 calc R . . C19A C 0.11744(3) -0.32444(12) -0.05959(4) 0.0182(4) Uani 1 1 d . . . C20A C 0.05526(3) -0.01794(12) -0.07341(5) 0.0209(4) Uani 1 1 d . . . H20A H 0.0289 -0.0359 -0.0978 0.025 Uiso 1 1 calc R . . H20B H 0.0617 0.0204 -0.0913 0.025 Uiso 1 1 calc R . . C21A C 0.06146(3) 0.06332(12) -0.03616(4) 0.0193(4) Uani 1 1 d . . . C22A C 0.03260(3) 0.09538(11) -0.03907(5) 0.0196(4) Uani 1 1 d . . . H22A H 0.0094 0.0615 -0.0631 0.023 Uiso 1 1 calc R . . C23A C 0.03700(3) 0.17611(12) -0.00755(4) 0.0197(4) Uani 1 1 d . . . C24A C 0.00611(3) 0.21653(12) -0.00925(5) 0.0226(4) Uani 1 1 d . . . C25A C -0.00125(4) 0.34235(12) -0.02246(5) 0.0282(4) Uani 1 1 d . . . H25A H -0.0084 0.3540 -0.0548 0.042 Uiso 1 1 calc R . . H25B H 0.0209 0.3854 0.0025 0.042 Uiso 1 1 calc R . . H25C H -0.0209 0.3676 -0.0235 0.042 Uiso 1 1 calc R . . C26A C 0.01745(4) 0.20163(14) 0.04179(5) 0.0302(4) Uani 1 1 d . . . H26A H 0.0223 0.1221 0.0510 0.045 Uiso 1 1 calc R . . H26B H -0.0023 0.2277 0.0406 0.045 Uiso 1 1 calc R . . H26C H 0.0395 0.2456 0.0662 0.045 Uiso 1 1 calc R . . C27A C -0.02926(3) 0.15222(13) -0.04692(5) 0.0291(5) Uani 1 1 d . . . H27A H -0.0251 0.0720 -0.0389 0.044 Uiso 1 1 calc R . . H27B H -0.0375 0.1638 -0.0799 0.044 Uiso 1 1 calc R . . H27C H -0.0480 0.1795 -0.0462 0.044 Uiso 1 1 calc R . . C28A C 0.07158(3) 0.22424(12) 0.02615(4) 0.0188(4) Uani 1 1 d . . . H28A H 0.0749 0.2806 0.0475 0.023 Uiso 1 1 calc R . . C29A C 0.10138(3) 0.19585(12) 0.03073(4) 0.0182(4) Uani 1 1 d . . . C30A C 0.13803(3) 0.25785(12) 0.06697(5) 0.0215(4) Uani 1 1 d . . . C31A C 0.13596(4) 0.35261(13) 0.09389(5) 0.0290(5) Uani 1 1 d . . . H31A H 0.1169 0.4060 0.0698 0.044 Uiso 1 1 calc R . . H31B H 0.1595 0.3914 0.1159 0.044 Uiso 1 1 calc R . . H31C H 0.1301 0.3211 0.1132 0.044 Uiso 1 1 calc R . . C32A C 0.16835(4) 0.17654(13) 0.10616(5) 0.0290(5) Uani 1 1 d . . . H32A H 0.1617 0.1428 0.1243 0.044 Uiso 1 1 calc R . . H32B H 0.1913 0.2177 0.1291 0.044 Uiso 1 1 calc R . . H32C H 0.1713 0.1173 0.0900 0.044 Uiso 1 1 calc R . . C33A C 0.14838(4) 0.31131(13) 0.03868(5) 0.0263(4) Uani 1 1 d . . . H33A H 0.1291 0.3633 0.0139 0.040 Uiso 1 1 calc R . . H33B H 0.1512 0.2524 0.0224 0.040 Uiso 1 1 calc R . . H33C H 0.1714 0.3524 0.0617 0.040 Uiso 1 1 calc R . . C34A C 0.09648(3) 0.10892(12) -0.00050(4) 0.0173(4) Uani 1 1 d . . . C35A C 0.06631(3) -0.18875(12) -0.02749(4) 0.0206(4) Uani 1 1 d . . . H35A H 0.0446 -0.2358 -0.0517 0.025 Uiso 1 1 calc R . . H35B H 0.0598 -0.1346 -0.0135 0.025 Uiso 1 1 calc R . . C36A C 0.09715(3) -0.26312(12) 0.01352(5) 0.0236(4) Uani 1 1 d . . . H36A H 0.0902 -0.2959 0.0316 0.028 Uiso 1 1 calc R . . H36B H 0.1006 -0.3257 -0.0012 0.028 Uiso 1 1 calc R . . C37A C 0.13051(4) -0.12488(13) 0.07933(5) 0.0281(4) Uani 1 1 d . . . H37A H 0.1262 -0.1676 0.0984 0.042 Uiso 1 1 calc R . . H37B H 0.1106 -0.0712 0.0580 0.042 Uiso 1 1 calc R . . H37C H 0.1537 -0.0842 0.1018 0.042 Uiso 1 1 calc R . . C38A C 0.16108(4) -0.28650(14) 0.08165(5) 0.0353(5) Uani 1 1 d . . . H38A H 0.1553 -0.3279 0.0994 0.053 Uiso 1 1 calc R . . H38B H 0.1845 -0.2480 0.1054 0.053 Uiso 1 1 calc R . . H38C H 0.1626 -0.3390 0.0620 0.053 Uiso 1 1 calc R . . Cl1B Cl 0.038079(9) 0.21127(4) 0.171573(13) 0.03598(13) Uani 1 1 d . . . C1B C 0.08711(4) 0.42130(13) 0.28586(5) 0.0321(5) Uani 1 1 d . A . H1BA H 0.0747 0.4385 0.2511 0.038 Uiso 1 1 calc R . . H1BB H 0.1080 0.4731 0.3073 0.038 Uiso 1 1 calc R . . Y1B Y 0.106716(3) 0.207764(12) 0.247778(4) 0.01697(4) Uani 1 1 d . A . N1B N 0.17429(3) 0.17389(10) 0.30067(4) 0.0169(3) Uani 1 1 d . A . O1B O 0.12370(2) 0.36356(8) 0.23944(3) 0.0205(3) Uani 1 1 d . . . C2B C 0.06133(4) 0.43362(16) 0.29467(6) 0.0461(6) Uani 1 1 d . . . H2BA H 0.0406 0.4828 0.2696 0.055 Uiso 1 1 calc R . . H2BB H 0.0737 0.4650 0.3278 0.055 Uiso 1 1 calc R . . N2B N 0.118263(6) 0.08915(2) 0.200329(10) 0.0231(4) Uani 1 1 d D . . O2B O 0.11335(2) 0.06520(8) 0.28966(3) 0.0218(3) Uani 1 1 d . . . C3B C 0.04862(4) 0.3142(2) 0.29053(6) 0.0640(7) Uani 1 1 d . . . H3BA H 0.0392 0.3049 0.3079 0.077 Uiso 1 1 calc R . . H3BB H 0.0296 0.2909 0.2557 0.077 Uiso 1 1 calc R . . O3B O 0.09951(2) 0.30535(8) 0.29725(3) 0.0297(3) Uani 1 1 d . . . C4B C 0.08328(4) 0.25140(15) 0.31548(6) 0.0629(5) Uani 1 1 d . A . H4BA H 0.0994 0.2583 0.3517 0.076 Uiso 1 1 calc R . . H4BB H 0.0785 0.1709 0.3064 0.076 Uiso 1 1 calc R . . C5B C 0.18706(3) 0.10968(12) 0.34536(4) 0.0199(4) Uani 1 1 d . A . H5BA H 0.1799 0.1518 0.3616 0.024 Uiso 1 1 calc R . . H5BB H 0.2140 0.1067 0.3687 0.024 Uiso 1 1 calc R . . C6B C 0.17276(3) -0.00857(12) 0.33612(4) 0.0181(4) Uani 1 1 d . . . C7B C 0.19601(3) -0.09889(12) 0.35290(4) 0.0187(4) Uani 1 1 d . A . H7BA H 0.2210 -0.0858 0.3697 0.022 Uiso 1 1 calc R . . C8B C 0.18358(3) -0.20924(12) 0.34574(4) 0.0200(4) Uani 1 1 d . . . C9B C 0.20980(3) -0.30786(12) 0.36302(5) 0.0216(4) Uani 1 1 d . A . C10B C 0.22155(4) -0.31216(14) 0.33252(5) 0.0326(5) Uani 1 1 d . . . H10D H 0.2327 -0.2404 0.3354 0.049 Uiso 1 1 calc R A . H10E H 0.2002 -0.3262 0.2979 0.049 Uiso 1 1 calc R . . H10F H 0.2393 -0.3727 0.3448 0.049 Uiso 1 1 calc R . . C11B C 0.24370(4) -0.29388(13) 0.41744(5) 0.0326(5) Uani 1 1 d . . . H11D H 0.2364 -0.2904 0.4372 0.049 Uiso 1 1 calc R A . H11E H 0.2564 -0.2244 0.4218 0.049 Uiso 1 1 calc R . . H11F H 0.2601 -0.3579 0.4282 0.049 Uiso 1 1 calc R . . C12B C 0.19248(4) -0.42149(13) 0.35735(5) 0.0311(5) Uani 1 1 d . . . H12D H 0.1846 -0.4211 0.3765 0.047 Uiso 1 1 calc R A . H12E H 0.2104 -0.4814 0.3695 0.047 Uiso 1 1 calc R . . H12F H 0.1713 -0.4345 0.3225 0.047 Uiso 1 1 calc R . . C13B C 0.14701(3) -0.22253(12) 0.32281(4) 0.0195(4) Uani 1 1 d . A . H13B H 0.1382 -0.2968 0.3186 0.023 Uiso 1 1 calc R . . C14B C 0.12239(3) -0.13422(12) 0.30566(4) 0.0191(4) Uani 1 1 d . . . C15B C 0.08315(3) -0.15469(12) 0.28453(5) 0.0229(4) Uani 1 1 d . A . C16B C 0.07648(4) -0.27824(12) 0.28866(5) 0.0276(4) Uani 1 1 d . . . H16D H 0.0803 -0.3251 0.2699 0.041 Uiso 1 1 calc R A . H16E H 0.0514 -0.2875 0.2753 0.041 Uiso 1 1 calc R . . H16F H 0.0935 -0.3011 0.3233 0.041 Uiso 1 1 calc R . . C17B C 0.07628(4) -0.08563(13) 0.31402(5) 0.0300(4) Uani 1 1 d . . . H17D H 0.0513 -0.0986 0.3006 0.045 Uiso 1 1 calc R A . H17E H 0.0796 -0.0057 0.3115 0.045 Uiso 1 1 calc R . . H17F H 0.0936 -0.1087 0.3487 0.045 Uiso 1 1 calc R . . C18B C 0.05487(4) -0.12192(13) 0.22981(5) 0.0299(5) Uani 1 1 d . . . H18D H 0.0590 -0.1662 0.2109 0.045 Uiso 1 1 calc R A . H18E H 0.0573 -0.0419 0.2262 0.045 Uiso 1 1 calc R . . H18F H 0.0303 -0.1368 0.2175 0.045 Uiso 1 1 calc R . . C19B C 0.13527(3) -0.02458(12) 0.30985(4) 0.0189(4) Uani 1 1 d . A . C20B C 0.19299(3) 0.28570(11) 0.31874(4) 0.0199(4) Uani 1 1 d . . . H20C H 0.2196 0.2728 0.3445 0.024 Uiso 1 1 calc R . . H20D H 0.1850 0.3251 0.3345 0.024 Uiso 1 1 calc R . . C21B C 0.18630(3) 0.36171(12) 0.27997(4) 0.0187(4) Uani 1 1 d . . . C22B C 0.21511(3) 0.39362(12) 0.28289(4) 0.0193(4) Uani 1 1 d . . . H22B H 0.2388 0.3643 0.3086 0.023 Uiso 1 1 calc R . . C23B C 0.21024(3) 0.46766(12) 0.24906(5) 0.0195(4) Uani 1 1 d . . . C24B C 0.24163(3) 0.50267(13) 0.25094(5) 0.0219(4) Uani 1 1 d . . . C25B C 0.24427(4) 0.63184(13) 0.25155(5) 0.0298(5) Uani 1 1 d . . . H25D H 0.2492 0.6614 0.2808 0.045 Uiso 1 1 calc R . . H25E H 0.2212 0.6627 0.2219 0.045 Uiso 1 1 calc R . . H25F H 0.2641 0.6535 0.2523 0.045 Uiso 1 1 calc R . . C26B C 0.23403(4) 0.45730(14) 0.20492(5) 0.0311(5) Uani 1 1 d . . . H26D H 0.2323 0.3752 0.2043 0.047 Uiso 1 1 calc R . . H26E H 0.2539 0.4793 0.2058 0.047 Uiso 1 1 calc R . . H26F H 0.2110 0.4884 0.1753 0.047 Uiso 1 1 calc R . . C27B C 0.27820(3) 0.45790(13) 0.29672(5) 0.0290(5) Uani 1 1 d . . . H27D H 0.2832 0.4867 0.3262 0.043 Uiso 1 1 calc R . . H27E H 0.2975 0.4825 0.2968 0.043 Uiso 1 1 calc R . . H27F H 0.2775 0.3757 0.2967 0.043 Uiso 1 1 calc R . . C28B C 0.17517(3) 0.51087(12) 0.21326(4) 0.0201(4) Uani 1 1 d . . . H28B H 0.1714 0.5626 0.1902 0.024 Uiso 1 1 calc R . . C29B C 0.14540(3) 0.48351(12) 0.20903(4) 0.0188(4) Uani 1 1 d . . . C30B C 0.10799(3) 0.54104(12) 0.17067(5) 0.0221(4) Uani 1 1 d . . . C31B C 0.09783(4) 0.60352(13) 0.19794(5) 0.0292(5) Uani 1 1 d . . . H31D H 0.1169 0.6582 0.2208 0.044 Uiso 1 1 calc R . . H31E H 0.0956 0.5493 0.2163 0.044 Uiso 1 1 calc R . . H31F H 0.0746 0.6427 0.1739 0.044 Uiso 1 1 calc R . . C32B C 0.10899(4) 0.62865(14) 0.14025(5) 0.0301(5) Uani 1 1 d . . . H32D H 0.1278 0.6847 0.1624 0.045 Uiso 1 1 calc R . . H32E H 0.0852 0.6657 0.1174 0.045 Uiso 1 1 calc R . . H32F H 0.1146 0.5915 0.1216 0.045 Uiso 1 1 calc R . . C33B C 0.07826(4) 0.45520(13) 0.13480(5) 0.0271(5) Uani 1 1 d . . . H33D H 0.0770 0.3983 0.1533 0.041 Uiso 1 1 calc R . . H33E H 0.0841 0.4190 0.1162 0.041 Uiso 1 1 calc R . . H33F H 0.0547 0.4934 0.1119 0.041 Uiso 1 1 calc R . . C34B C 0.15089(3) 0.40278(12) 0.24253(4) 0.0185(4) Uani 1 1 d . . . C35B C 0.18396(3) 0.11268(12) 0.27436(4) 0.0213(4) Uani 1 1 d . . . H35C H 0.1985 0.0486 0.2937 0.026 Uiso 1 1 d R A . H35D H 0.1987 0.1611 0.2722 0.026 Uiso 1 1 d R . . C36B C 0.153994(12) 0.03295(7) 0.23579(5) 0.0212(5) Uani 0.8188(16) 1 d PD A 1 H36C H 0.1608 -0.0012 0.2176 0.025 Uiso 0.8188(16) 1 calc PR A 1 H36D H 0.1519 -0.0282 0.2524 0.025 Uiso 0.8188(16) 1 calc PR A 1 C37B C 0.117957(17) 0.16338(7) 0.16715(2) 0.0298(6) Uani 0.8188(16) 1 d PD A 1 H37D H 0.1223 0.1187 0.1486 0.045 Uiso 0.8188(16) 1 calc PR A 1 H37E H 0.1371 0.2202 0.1867 0.045 Uiso 0.8188(16) 1 calc PR A 1 H37F H 0.0942 0.2005 0.1442 0.045 Uiso 0.8188(16) 1 calc PR A 1 C38B C 0.090390(17) 0.00089(5) 0.17064(5) 0.0320(6) Uani 0.8188(16) 1 d PD A 1 H38D H 0.0959 -0.0425 0.1530 0.048 Uiso 0.8188(16) 1 calc PR A 1 H38E H 0.0663 0.0357 0.1468 0.048 Uiso 0.8188(16) 1 calc PR A 1 H38F H 0.0905 -0.0491 0.1924 0.048 Uiso 0.8188(16) 1 calc PR A 1 C36" C 0.154320(10) 0.12772(14) 0.21905(5) 0.045(3) Uani 0.1812(16) 1 d PD A 2 H36E H 0.1527 0.2081 0.2108 0.054 Uiso 0.1812(16) 1 calc PR A 2 H36F H 0.1611 0.0852 0.2024 0.054 Uiso 0.1812(16) 1 calc PR A 2 C37" C 0.0942(2) 0.13179(11) 0.14926(2) 0.049(3) Uani 0.1812(16) 1 d PD A 2 H37G H 0.0987 0.0896 0.1303 0.074 Uiso 0.1812(16) 1 calc PR A 2 H37H H 0.0993 0.2115 0.1495 0.074 Uiso 0.1812(16) 1 calc PR A 2 H37I H 0.0687 0.1225 0.1341 0.074 Uiso 0.1812(16) 1 calc PR A 2 C38" C 0.11675(10) -0.03429(4) 0.20249(17) 0.051(3) Uani 0.1812(16) 1 d PD A 2 H38G H 0.1220 -0.0687 0.1829 0.076 Uiso 0.1812(16) 1 calc PR A 2 H38H H 0.0924 -0.0569 0.1892 0.076 Uiso 0.1812(16) 1 calc PR A 2 H38I H 0.1349 -0.0592 0.2368 0.076 Uiso 0.1812(16) 1 calc PR A 2 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 Y1A 0.01625(4) 0.01661(7) 0.01981(4) -0.00040(5) 0.01239(3) -0.00014(5) O1A 0.0288(3) 0.0173(5) 0.0292(3) -0.0018(3) 0.0225(3) -0.0002(4) N1A 0.0189(4) 0.0152(6) 0.0212(4) -0.0019(4) 0.0143(3) 0.0005(4) C1A 0.0260(5) 0.0176(7) 0.0262(5) -0.0005(5) 0.0175(4) 0.0001(6) Cl1A 0.01791(13) 0.0311(2) 0.02420(14) 0.00105(14) 0.00942(10) -0.00098(15) N2A 0.0216(4) 0.0246(7) 0.0236(4) 0.0050(4) 0.0153(3) 0.0025(5) C2A 0.0281(5) 0.0219(8) 0.0262(5) -0.0011(5) 0.0196(4) -0.0029(6) O2A 0.0193(3) 0.0209(5) 0.0236(3) -0.0033(3) 0.0150(3) 0.0002(4) C3A 0.0333(5) 0.0270(8) 0.0328(5) 0.0017(5) 0.0267(4) 0.0026(6) O3A 0.0211(3) 0.0194(5) 0.0318(4) -0.0046(4) 0.0185(3) -0.0023(4) C4A 0.0483(6) 0.0255(8) 0.0507(6) -0.0041(6) 0.0436(4) 0.0009(6) C5A 0.0186(5) 0.0224(8) 0.0194(5) -0.0024(5) 0.0120(4) 0.0005(6) C6A 0.0212(5) 0.0182(7) 0.0191(5) -0.0028(5) 0.0147(4) -0.0019(5) C7A 0.0175(5) 0.0250(8) 0.0148(5) -0.0008(5) 0.0104(4) 0.0014(6) C8A 0.0223(5) 0.0176(7) 0.0165(5) -0.0006(5) 0.0130(4) -0.0022(6) C9A 0.0223(5) 0.0210(8) 0.0216(5) -0.0011(5) 0.0124(4) -0.0025(6) C10A 0.0298(6) 0.0279(9) 0.0264(6) -0.0021(6) 0.0124(5) -0.0078(7) C11A 0.0313(6) 0.0207(8) 0.0292(6) -0.0017(6) 0.0180(5) -0.0043(7) C12A 0.0341(6) 0.0304(9) 0.0397(6) -0.0002(6) 0.0274(5) -0.0057(7) C13A 0.0257(5) 0.0181(7) 0.0191(5) 0.0003(5) 0.0163(4) 0.0020(6) C14A 0.0186(5) 0.0195(7) 0.0207(5) -0.0013(5) 0.0137(4) -0.0007(5) C15A 0.0204(5) 0.0209(8) 0.0308(6) -0.0031(5) 0.0168(4) 0.0017(6) C16A 0.0220(5) 0.0235(8) 0.0380(6) -0.0013(6) 0.0199(4) 0.0005(6) C17A 0.0180(5) 0.0324(9) 0.0349(7) -0.0074(6) 0.0132(5) 0.0019(7) C18A 0.0338(5) 0.0245(8) 0.0533(7) -0.0006(6) 0.0342(5) -0.0010(6) C19A 0.0198(5) 0.0194(7) 0.0197(5) -0.0030(5) 0.0148(4) -0.0035(5) C20A 0.0173(5) 0.0201(7) 0.0202(5) -0.0003(5) 0.0100(4) 0.0020(6) C21A 0.0208(5) 0.0158(7) 0.0214(5) 0.0025(5) 0.0138(4) 0.0038(5) C22A 0.0162(5) 0.0164(7) 0.0227(5) -0.0002(5) 0.0113(4) 0.0000(5) C23A 0.0216(5) 0.0171(7) 0.0228(5) 0.0041(5) 0.0156(4) 0.0039(6) C24A 0.0198(5) 0.0203(8) 0.0305(5) -0.0010(5) 0.0177(4) 0.0002(6) C25A 0.0273(5) 0.0232(8) 0.0402(6) 0.0014(6) 0.0248(4) 0.0062(6) C26A 0.0322(5) 0.0343(9) 0.0361(6) 0.0010(6) 0.0275(4) 0.0024(7) C27A 0.0231(5) 0.0280(9) 0.0405(6) -0.0045(6) 0.0227(4) 0.0017(6) C28A 0.0230(5) 0.0162(7) 0.0182(5) 0.0012(5) 0.0139(4) 0.0040(6) C29A 0.0201(5) 0.0168(7) 0.0161(5) 0.0016(5) 0.0111(4) 0.0018(6) C30A 0.0203(5) 0.0226(8) 0.0194(5) -0.0024(5) 0.0120(4) 0.0008(6) C31A 0.0243(6) 0.0301(9) 0.0298(6) -0.0113(6) 0.0164(4) -0.0051(6) C32A 0.0215(6) 0.0322(9) 0.0228(6) -0.0034(6) 0.0099(5) 0.0021(7) C33A 0.0249(5) 0.0251(8) 0.0279(6) -0.0046(6) 0.0168(4) -0.0043(6) C34A 0.0184(5) 0.0164(7) 0.0199(5) 0.0031(5) 0.0137(4) 0.0029(5) C35A 0.0199(5) 0.0215(8) 0.0247(5) -0.0035(5) 0.0165(4) -0.0018(6) C36A 0.0267(5) 0.0200(8) 0.0296(5) 0.0022(5) 0.0209(4) -0.0001(6) C37A 0.0289(6) 0.0318(9) 0.0231(5) -0.0002(6) 0.0168(4) -0.0051(7) C38A 0.0299(6) 0.0365(9) 0.0416(6) 0.0186(7) 0.0243(5) 0.0085(7) Cl1B 0.01788(14) 0.0460(2) 0.02972(16) 0.00138(17) 0.00934(12) -0.00093(18) C1B 0.0402(6) 0.0215(8) 0.0402(6) 0.0015(6) 0.0289(5) 0.0053(7) Y1B 0.01599(4) 0.01732(7) 0.01742(4) 0.00133(5) 0.01086(3) 0.00041(5) N1B 0.0179(4) 0.0164(6) 0.0179(4) 0.0013(4) 0.0124(3) 0.0001(4) O1B 0.0196(3) 0.0207(5) 0.0230(3) 0.0039(3) 0.0147(3) 0.0010(4) C2B 0.0487(7) 0.0582(12) 0.0412(7) 0.0193(7) 0.0337(5) 0.0246(8) N2B 0.0221(4) 0.0262(7) 0.0200(4) -0.0018(4) 0.0133(3) -0.0007(5) O2B 0.0216(3) 0.0199(5) 0.0259(4) 0.0051(4) 0.0164(3) 0.0040(4) C3B 0.0529(6) 0.1162(18) 0.0505(6) -0.0443(9) 0.0459(5) -0.0432(10) O3B 0.0497(4) 0.0167(5) 0.0452(4) 0.0018(4) 0.0409(3) 0.0016(4) C4B 0.1305(7) 0.0212(9) 0.1213(8) -0.0042(7) 0.1192(5) -0.0075(8) C5B 0.0205(5) 0.0191(7) 0.0164(5) 0.0027(5) 0.0105(4) -0.0001(6) C6B 0.0216(5) 0.0178(7) 0.0147(5) 0.0006(5) 0.0118(4) -0.0017(6) C7B 0.0182(5) 0.0216(8) 0.0143(5) 0.0030(5) 0.0097(4) 0.0003(6) C8B 0.0244(5) 0.0231(8) 0.0139(4) 0.0025(5) 0.0132(4) 0.0032(6) C9B 0.0232(5) 0.0193(8) 0.0206(5) -0.0009(5) 0.0136(4) 0.0030(6) C10B 0.0383(6) 0.0286(9) 0.0386(6) 0.0021(6) 0.0285(5) 0.0079(7) C11B 0.0297(6) 0.0257(9) 0.0255(6) 0.0021(6) 0.0107(5) 0.0095(7) C12B 0.0324(6) 0.0220(8) 0.0386(6) 0.0032(6) 0.0232(5) 0.0037(7) C13B 0.0247(5) 0.0179(7) 0.0157(5) -0.0013(5) 0.0132(4) -0.0016(6) C14B 0.0212(5) 0.0207(7) 0.0165(5) 0.0004(5) 0.0129(4) -0.0012(6) C15B 0.0210(5) 0.0219(8) 0.0254(5) 0.0023(5) 0.0150(4) 0.0003(6) C16B 0.0243(5) 0.0243(8) 0.0315(6) 0.0018(6) 0.0172(4) -0.0019(6) C17B 0.0327(5) 0.0250(8) 0.0446(6) 0.0028(6) 0.0306(4) 0.0008(6) C18B 0.0226(6) 0.0271(8) 0.0302(6) 0.0079(6) 0.0130(5) -0.0024(6) C19B 0.0241(5) 0.0179(7) 0.0175(5) 0.0029(5) 0.0148(4) 0.0026(6) C20B 0.0201(5) 0.0158(7) 0.0206(5) 0.0002(5) 0.0120(4) -0.0021(6) C21B 0.0208(5) 0.0168(7) 0.0177(5) 0.0000(5) 0.0123(4) -0.0011(6) C22B 0.0181(5) 0.0164(7) 0.0209(5) 0.0002(5) 0.0117(4) -0.0010(5) C23B 0.0220(5) 0.0161(7) 0.0232(5) -0.0045(5) 0.0160(4) -0.0044(5) C24B 0.0247(5) 0.0196(8) 0.0272(5) -0.0028(5) 0.0195(4) -0.0041(6) C25B 0.0315(6) 0.0252(8) 0.0375(6) -0.0028(6) 0.0247(5) -0.0068(6) C26B 0.0297(6) 0.0363(9) 0.0338(6) -0.0091(6) 0.0237(4) -0.0118(7) C27B 0.0234(5) 0.0312(9) 0.0354(6) -0.0012(6) 0.0205(4) -0.0058(6) C28B 0.0270(5) 0.0158(7) 0.0183(5) 0.0004(5) 0.0152(4) -0.0001(6) C29B 0.0214(5) 0.0173(7) 0.0190(5) -0.0005(5) 0.0138(4) 0.0003(6) C30B 0.0225(5) 0.0212(8) 0.0242(5) 0.0086(5) 0.0160(4) 0.0047(6) C31B 0.0300(6) 0.0256(8) 0.0324(6) 0.0074(6) 0.0206(5) 0.0090(6) C32B 0.0264(6) 0.0332(9) 0.0285(6) 0.0121(6) 0.0171(4) 0.0051(7) C33B 0.0192(6) 0.0291(8) 0.0230(6) 0.0067(6) 0.0095(5) 0.0038(6) C34B 0.0202(5) 0.0171(7) 0.0203(5) -0.0023(5) 0.0143(4) -0.0010(5) C35B 0.0240(5) 0.0215(8) 0.0260(5) 0.0022(5) 0.0198(4) 0.0023(6) C36B 0.0264(6) 0.0219(9) 0.0221(6) -0.0002(6) 0.0189(5) 0.0025(7) C37B 0.0341(7) 0.0342(11) 0.0259(7) 0.0021(7) 0.0218(5) 0.0015(8) C38B 0.0296(7) 0.0337(11) 0.0335(7) -0.0097(8) 0.0211(6) -0.0074(8) C36" 0.096(4) 0.017(4) 0.071(3) 0.010(3) 0.076(3) 0.010(4) C37" 0.086(4) 0.038(6) 0.057(4) 0.010(4) 0.062(3) 0.021(5) C38" 0.081(4) 0.020(5) 0.095(4) -0.011(4) 0.077(3) -0.001(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Y1A O2A 2.1360(10) . ? Y1A O3A 2.1467(10) . ? Y1A O1A 2.3433(11) . ? Y1A N1A 2.5153(10) . ? Y1A N2A 2.5523(14) . ? Y1A Cl1A 2.5725(3) . ? O1A C1A 1.4680(17) . ? O1A C4A 1.470(2) . ? N1A C35A 1.484(2) . ? N1A C20A 1.4991(17) . ? N1A C5A 1.5034(18) . ? C1A C2A 1.513(2) . ? N2A C36A 1.4773(16) . ? N2A C37A 1.480(2) . ? N2A C38A 1.4805(17) . ? C2A C3A 1.521(2) . ? O2A C34A 1.3372(18) . ? C3A C4A 1.499(2) . ? O3A C19A 1.3389(16) . ? C5A C6A 1.5059(19) . ? C6A C7A 1.3829(19) . ? C6A C19A 1.4072(18) . ? C7A C8A 1.396(2) . ? C8A C13A 1.3909(19) . ? C8A C9A 1.540(2) . ? C9A C11A 1.527(2) . ? C9A C12A 1.529(3) . ? C9A C10A 1.5391(17) . ? C13A C14A 1.3984(19) . ? C14A C19A 1.418(2) . ? C14A C15A 1.543(2) . ? C15A C16A 1.535(2) . ? C15A C17A 1.5356(19) . ? C15A C18A 1.540(3) . ? C20A C21A 1.514(2) . ? C21A C22A 1.388(2) . ? C21A C34A 1.4041(16) . ? C22A C23A 1.392(2) . ? C23A C28A 1.3956(17) . ? C23A C24A 1.537(2) . ? C24A C27A 1.5232(18) . ? C24A C26A 1.541(2) . ? C24A C25A 1.542(2) . ? C28A C29A 1.386(2) . ? C29A C34A 1.428(2) . ? C29A C30A 1.5393(17) . ? C30A C31A 1.532(2) . ? C30A C33A 1.536(3) . ? C30A C32A 1.5398(18) . ? C35A C36A 1.5186(17) . ? Cl1B Y1B 2.5769(3) . ? C1B O3B 1.4542(18) . ? C1B C2B 1.485(3) . ? Y1B O1B 2.1300(10) . ? Y1B O2B 2.1492(10) . ? Y1B O3B 2.3343(12) . ? Y1B N1B 2.5216(10) . ? Y1B N2B 2.5437(4) . ? N1B C35B 1.492(2) . ? N1B C5B 1.4982(18) . ? N1B C20B 1.4990(17) . ? O1B C34B 1.3340(19) . ? C2B C3B 1.519(3) . ? N2B C37B 1.4768(5) . ? N2B C38" 1.4769(5) . ? N2B C37" 1.4771(5) . ? N2B C38B 1.4771(4) . ? N2B C36" 1.4771(5) . ? N2B C36B 1.4773(4) . ? O2B C19B 1.3378(16) . ? C3B C4B 1.488(3) . ? O3B C4B 1.462(2) . ? C5B C6B 1.508(2) . ? C6B C7B 1.3793(19) . ? C6B C19B 1.4092(18) . ? C7B C8B 1.398(2) . ? C8B C13B 1.3918(19) . ? C8B C9B 1.532(2) . ? C9B C11B 1.5305(17) . ? C9B C10B 1.533(3) . ? C9B C12B 1.535(2) . ? C13B C14B 1.396(2) . ? C14B C19B 1.413(2) . ? C14B C15B 1.539(2) . ? C15B C16B 1.535(2) . ? C15B C18B 1.5385(18) . ? C15B C17B 1.541(2) . ? C20B C21B 1.508(2) . ? C21B C22B 1.385(2) . ? C21B C34B 1.4043(16) . ? C22B C23B 1.391(2) . ? C23B C28B 1.3952(17) . ? C23B C24B 1.537(2) . ? C24B C27B 1.5211(17) . ? C24B C26B 1.538(2) . ? C24B C25B 1.543(2) . ? C28B C29B 1.389(2) . ? C29B C34B 1.423(2) . ? C29B C30B 1.5446(17) . ? C30B C33B 1.5334(18) . ? C30B C32B 1.535(2) . ? C30B C31B 1.546(3) . ? C35B C36B 1.5155(15) . ? C35B C36" 1.5183(17) . ? 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 O2A Y1A O3A 152.88(3) . . ? O2A Y1A O1A 86.90(4) . . ? O3A Y1A O1A 84.17(4) . . ? O2A Y1A N1A 78.64(4) . . ? O3A Y1A N1A 80.69(4) . . ? O1A Y1A N1A 110.68(3) . . ? O2A Y1A N2A 97.89(4) . . ? O3A Y1A N2A 91.56(4) . . ? O1A Y1A N2A 175.21(4) . . ? N1A Y1A N2A 70.61(4) . . ? O2A Y1A Cl1A 102.27(2) . . ? O3A Y1A Cl1A 103.46(2) . . ? O1A Y1A Cl1A 91.10(2) . . ? N1A Y1A Cl1A 158.19(3) . . ? N2A Y1A Cl1A 87.78(2) . . ? C1A O1A C4A 108.31(12) . . ? C1A O1A Y1A 121.24(9) . . ? C4A O1A Y1A 120.27(8) . . ? C35A N1A C20A 110.26(12) . . ? C35A N1A C5A 110.62(11) . . ? C20A N1A C5A 105.75(9) . . ? C35A N1A Y1A 113.93(6) . . ? C20A N1A Y1A 109.78(8) . . ? C5A N1A Y1A 106.11(9) . . ? O1A C1A C2A 105.66(13) . . ? C36A N2A C37A 110.60(13) . . ? C36A N2A C38A 108.20(11) . . ? C37A N2A C38A 108.22(11) . . ? C36A N2A Y1A 108.33(9) . . ? C37A N2A Y1A 108.29(9) . . ? C38A N2A Y1A 113.21(11) . . ? C1A C2A C3A 103.28(13) . . ? C34A O2A Y1A 138.19(9) . . ? C4A C3A C2A 101.59(12) . . ? C19A O3A Y1A 136.59(10) . . ? O1A C4A C3A 104.98(12) . . ? N1A C5A C6A 116.10(10) . . ? C7A C6A C19A 120.93(13) . . ? C7A C6A C5A 120.23(11) . . ? C19A C6A C5A 118.78(12) . . ? C6A C7A C8A 121.40(12) . . ? C13A C8A C7A 116.76(13) . . ? C13A C8A C9A 123.56(13) . . ? C7A C8A C9A 119.67(12) . . ? C11A C9A C12A 108.97(14) . . ? C11A C9A C10A 107.95(12) . . ? C12A C9A C10A 108.43(13) . . ? C11A C9A C8A 112.41(12) . . ? C12A C9A C8A 109.31(13) . . ? C10A C9A C8A 109.69(12) . . ? C8A C13A C14A 124.33(13) . . ? C13A C14A C19A 117.20(12) . . ? C13A C14A C15A 121.56(13) . . ? C19A C14A C15A 121.21(12) . . ? C16A C15A C17A 107.34(11) . . ? C16A C15A C18A 106.95(15) . . ? C17A C15A C18A 110.27(12) . . ? C16A C15A C14A 112.25(12) . . ? C17A C15A C14A 111.44(14) . . ? C18A C15A C14A 108.49(11) . . ? O3A C19A C6A 118.07(13) . . ? O3A C19A C14A 122.86(11) . . ? C6A C19A C14A 119.06(12) . . ? N1A C20A C21A 116.05(10) . . ? C22A C21A C34A 121.35(14) . . ? C22A C21A C20A 120.22(11) . . ? C34A C21A C20A 118.35(14) . . ? C21A C22A C23A 121.32(12) . . ? C22A C23A C28A 116.52(15) . . ? C22A C23A C24A 123.97(11) . . ? C28A C23A C24A 119.48(13) . . ? C27A C24A C23A 112.28(13) . . ? C27A C24A C26A 108.39(14) . . ? C23A C24A C26A 109.77(10) . . ? C27A C24A C25A 108.45(10) . . ? C23A C24A C25A 109.88(14) . . ? C26A C24A C25A 107.96(13) . . ? C29A C28A C23A 124.77(14) . . ? C28A C29A C34A 117.41(11) . . ? C28A C29A C30A 121.37(13) . . ? C34A C29A C30A 121.20(14) . . ? C31A C30A C33A 107.31(13) . . ? C31A C30A C29A 111.74(13) . . ? C33A C30A C29A 109.65(11) . . ? C31A C30A C32A 107.73(11) . . ? C33A C30A C32A 109.61(13) . . ? C29A C30A C32A 110.71(12) . . ? O2A C34A C21A 119.11(13) . . ? O2A C34A C29A 122.43(11) . . ? C21A C34A C29A 118.46(14) . . ? N1A C35A C36A 112.53(12) . . ? N2A C36A C35A 113.28(12) . . ? O3B C1B C2B 106.55(15) . . ? O1B Y1B O2B 153.24(3) . . ? O1B Y1B O3B 86.45(4) . . ? O2B Y1B O3B 83.60(4) . . ? O1B Y1B N1B 79.27(4) . . ? O2B Y1B N1B 79.71(4) . . ? O3B Y1B N1B 105.97(3) . . ? O1B Y1B N2B 96.56(3) . . ? O2B Y1B N2B 91.88(3) . . ? O3B Y1B N2B 174.82(2) . . ? N1B Y1B N2B 70.59(3) . . ? O1B Y1B Cl1B 100.72(2) . . ? O2B Y1B Cl1B 104.68(2) . . ? O3B Y1B Cl1B 93.86(2) . . ? N1B Y1B Cl1B 160.10(3) . . ? N2B Y1B Cl1B 89.737(13) . . ? C35B N1B C5B 110.41(11) . . ? C35B N1B C20B 110.88(12) . . ? C5B N1B C20B 106.34(9) . . ? C35B N1B Y1B 113.19(6) . . ? C5B N1B Y1B 108.06(9) . . ? C20B N1B Y1B 107.66(8) . . ? C34B O1B Y1B 138.26(9) . . ? C1B C2B C3B 103.37(16) . . ? C37B N2B C38" 131.6(2) . . ? C37B N2B C37" 37.7(3) . . ? C38" N2B C37" 112.44(19) . . ? C37B N2B C38B 108.84(7) . . ? C38" N2B C38B 43.59(14) . . ? C37" N2B C38B 75.13(19) . . ? C37B N2B C36" 64.14(5) . . ? C38" N2B C36" 111.75(18) . . ? C37" N2B C36" 101.2(3) . . ? C38B N2B C36" 143.23(11) . . ? C37B N2B C36B 110.68(7) . . ? C38" N2B C36B 64.79(14) . . ? C37" N2B C36B 138.8(4) . . ? C38B N2B C36B 107.58(5) . . ? C36" N2B C36B 51.53(7) . . ? C37B N2B Y1B 108.57(4) . . ? C38" N2B Y1B 118.5(2) . . ? C37" N2B Y1B 107.5(3) . . ? C38B N2B Y1B 112.34(7) . . ? C36" N2B Y1B 103.72(8) . . ? C36B N2B Y1B 108.84(7) . . ? C19B O2B Y1B 135.45(11) . . ? C4B C3B C2B 100.72(14) . . ? C1B O3B C4B 107.37(13) . . ? C1B O3B Y1B 119.97(10) . . ? C4B O3B Y1B 121.05(9) . . ? O3B C4B C3B 103.68(15) . . ? N1B C5B C6B 115.69(10) . . ? C7B C6B C19B 120.94(13) . . ? C7B C6B C5B 120.39(12) . . ? C19B C6B C5B 118.66(12) . . ? C6B C7B C8B 121.51(13) . . ? C13B C8B C7B 116.40(13) . . ? C13B C8B C9B 123.39(13) . . ? C7B C8B C9B 120.21(12) . . ? C11B C9B C10B 109.00(13) . . ? C11B C9B C8B 110.26(12) . . ? C10B C9B C8B 109.55(12) . . ? C11B C9B C12B 107.59(12) . . ? C10B C9B C12B 107.67(13) . . ? C8B C9B C12B 112.68(12) . . ? C8B C13B C14B 124.45(14) . . ? C13B C14B C19B 117.35(13) . . ? C13B C14B C15B 121.50(13) . . ? C19B C14B C15B 121.12(12) . . ? C16B C15B C14B 112.04(12) . . ? C16B C15B C18B 107.40(11) . . ? C14B C15B C18B 111.67(14) . . ? C16B C15B C17B 106.95(14) . . ? C14B C15B C17B 109.35(11) . . ? C18B C15B C17B 109.28(12) . . ? O2B C19B C6B 118.26(13) . . ? O2B C19B C14B 122.86(12) . . ? C6B C19B C14B 118.88(12) . . ? N1B C20B C21B 115.50(10) . . ? C22B C21B C34B 121.15(14) . . ? C22B C21B C20B 119.96(11) . . ? C34B C21B C20B 118.84(14) . . ? C21B C22B C23B 121.53(11) . . ? C22B C23B C28B 116.48(15) . . ? C22B C23B C24B 122.52(11) . . ? C28B C23B C24B 120.99(13) . . ? C27B C24B C23B 111.85(13) . . ? C27B C24B C26B 109.15(13) . . ? C23B C24B C26B 108.96(11) . . ? C27B C24B C25B 107.89(11) . . ? C23B C24B C25B 109.99(13) . . ? C26B C24B C25B 108.96(13) . . ? C29B C28B C23B 124.54(14) . . ? C28B C29B C34B 117.46(11) . . ? C28B C29B C30B 121.57(13) . . ? C34B C29B C30B 120.95(14) . . ? C33B C30B C32B 107.80(11) . . ? C33B C30B C29B 111.24(12) . . ? C32B C30B C29B 111.73(13) . . ? C33B C30B C31B 109.84(13) . . ? C32B C30B C31B 107.23(13) . . ? C29B C30B C31B 108.91(11) . . ? O1B C34B C21B 118.68(13) . . ? O1B C34B C29B 122.65(11) . . ? C21B C34B C29B 118.67(14) . . ? N1B C35B C36B 111.98(12) . . ? N1B C35B C36" 110.51(11) . . ? C36B C35B C36" 50.08(8) . . ? N2B C36B C35B 112.66(8) . . ? N2B C36" C35B 112.51(11) . . ? 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 O2A Y1A O1A C1A 28.76(8) . . . . ? O3A Y1A O1A C1A -176.88(8) . . . . ? N1A Y1A O1A C1A 105.39(8) . . . . ? N2A Y1A O1A C1A -149.8(3) . . . . ? Cl1A Y1A O1A C1A -73.46(7) . . . . ? O2A Y1A O1A C4A 169.98(8) . . . . ? O3A Y1A O1A C4A -35.66(8) . . . . ? N1A Y1A O1A C4A -113.40(8) . . . . ? N2A Y1A O1A C4A -8.6(4) . . . . ? Cl1A Y1A O1A C4A 67.76(7) . . . . ? O2A Y1A N1A C35A -100.26(10) . . . . ? O3A Y1A N1A C35A 97.39(10) . . . . ? O1A Y1A N1A C35A 177.49(9) . . . . ? N2A Y1A N1A C35A 2.40(9) . . . . ? Cl1A Y1A N1A C35A -5.61(15) . . . . ? O2A Y1A N1A C20A 23.95(9) . . . . ? O3A Y1A N1A C20A -138.40(10) . . . . ? O1A Y1A N1A C20A -58.30(10) . . . . ? N2A Y1A N1A C20A 126.61(10) . . . . ? Cl1A Y1A N1A C20A 118.59(10) . . . . ? O2A Y1A N1A C5A 137.78(9) . . . . ? O3A Y1A N1A C5A -24.56(8) . . . . ? O1A Y1A N1A C5A 55.53(9) . . . . ? N2A Y1A N1A C5A -119.56(9) . . . . ? Cl1A Y1A N1A C5A -127.57(9) . . . . ? C4A O1A C1A C2A 3.57(12) . . . . ? Y1A O1A C1A C2A 148.84(7) . . . . ? O2A Y1A N2A C36A 98.09(9) . . . . ? O3A Y1A N2A C36A -56.42(9) . . . . ? O1A Y1A N2A C36A -83.3(4) . . . . ? N1A Y1A N2A C36A 23.14(9) . . . . ? Cl1A Y1A N2A C36A -159.83(9) . . . . ? O2A Y1A N2A C37A -21.91(7) . . . . ? O3A Y1A N2A C37A -176.42(7) . . . . ? O1A Y1A N2A C37A 156.7(3) . . . . ? N1A Y1A N2A C37A -96.86(8) . . . . ? Cl1A Y1A N2A C37A 80.17(7) . . . . ? O2A Y1A N2A C38A -141.91(9) . . . . ? O3A Y1A N2A C38A 63.58(9) . . . . ? O1A Y1A N2A C38A 36.7(4) . . . . ? N1A Y1A N2A C38A 143.14(10) . . . . ? Cl1A Y1A N2A C38A -39.83(9) . . . . ? O1A C1A C2A C3A -26.66(11) . . . . ? O3A Y1A O2A C34A 68.72(17) . . . . ? O1A Y1A O2A C34A 139.52(12) . . . . ? N1A Y1A O2A C34A 27.70(12) . . . . ? N2A Y1A O2A C34A -40.60(12) . . . . ? Cl1A Y1A O2A C34A -130.03(11) . . . . ? C1A C2A C3A C4A 39.02(14) . . . . ? O2A Y1A O3A C19A -67.13(16) . . . . ? O1A Y1A O3A C19A -138.55(11) . . . . ? N1A Y1A O3A C19A -26.42(11) . . . . ? N2A Y1A O3A C19A 43.63(11) . . . . ? Cl1A Y1A O3A C19A 131.72(11) . . . . ? C1A O1A C4A C3A 21.42(13) . . . . ? Y1A O1A C4A C3A -124.24(10) . . . . ? C2A C3A C4A O1A -37.24(14) . . . . ? C35A N1A C5A C6A -54.93(15) . . . . ? C20A N1A C5A C6A -174.30(13) . . . . ? Y1A N1A C5A C6A 69.11(14) . . . . ? N1A C5A C6A C7A 113.21(15) . . . . ? N1A C5A C6A C19A -69.6(2) . . . . ? C19A C6A C7A C8A -1.5(2) . . . . ? C5A C6A C7A C8A 175.64(14) . . . . ? C6A C7A C8A C13A -2.4(2) . . . . ? C6A C7A C8A C9A 176.78(14) . . . . ? C13A C8A C9A C11A -5.7(2) . . . . ? C7A C8A C9A C11A 175.18(14) . . . . ? C13A C8A C9A C12A 115.43(16) . . . . ? C7A C8A C9A C12A -63.69(16) . . . . ? C13A C8A C9A C10A -125.81(16) . . . . ? C7A C8A C9A C10A 55.1(2) . . . . ? C7A C8A C13A C14A 2.0(2) . . . . ? C9A C8A C13A C14A -177.13(15) . . . . ? C8A C13A C14A C19A 2.2(2) . . . . ? C8A C13A C14A C15A -175.76(14) . . . . ? C13A C14A C15A C16A 1.2(2) . . . . ? C19A C14A C15A C16A -176.73(14) . . . . ? C13A C14A C15A C17A -119.28(16) . . . . ? C19A C14A C15A C17A 62.83(19) . . . . ? C13A C14A C15A C18A 119.14(15) . . . . ? C19A C14A C15A C18A -58.76(18) . . . . ? Y1A O3A C19A C6A 38.77(19) . . . . ? Y1A O3A C19A C14A -140.41(13) . . . . ? C7A C6A C19A O3A -173.36(14) . . . . ? C5A C6A C19A O3A 9.5(2) . . . . ? C7A C6A C19A C14A 5.9(2) . . . . ? C5A C6A C19A C14A -171.33(14) . . . . ? C13A C14A C19A O3A 173.12(14) . . . . ? C15A C14A C19A O3A -8.9(2) . . . . ? C13A C14A C19A C6A -6.1(2) . . . . ? C15A C14A C19A C6A 171.93(14) . . . . ? C35A N1A C20A C21A 60.13(15) . . . . ? C5A N1A C20A C21A 179.75(13) . . . . ? Y1A N1A C20A C21A -66.18(15) . . . . ? N1A C20A C21A C22A -119.11(14) . . . . ? N1A C20A C21A C34A 63.94(19) . . . . ? C34A C21A C22A C23A 1.6(2) . . . . ? C20A C21A C22A C23A -175.22(13) . . . . ? C21A C22A C23A C28A 1.3(2) . . . . ? C21A C22A C23A C24A 179.15(14) . . . . ? C22A C23A C24A C27A 4.1(2) . . . . ? C28A C23A C24A C27A -178.09(13) . . . . ? C22A C23A C24A C26A 124.74(15) . . . . ? C28A C23A C24A C26A -57.45(18) . . . . ? C22A C23A C24A C25A -116.69(15) . . . . ? C28A C23A C24A C25A 61.13(16) . . . . ? C22A C23A C28A C29A -1.2(2) . . . . ? C24A C23A C28A C29A -179.18(14) . . . . ? C23A C28A C29A C34A -1.7(2) . . . . ? C23A C28A C29A C30A 176.53(13) . . . . ? C28A C29A C30A C31A -2.07(19) . . . . ? C34A C29A C30A C31A 176.12(13) . . . . ? C28A C29A C30A C33A -120.92(15) . . . . ? C34A C29A C30A C33A 57.27(17) . . . . ? C28A C29A C30A C32A 118.01(16) . . . . ? C34A C29A C30A C32A -63.80(19) . . . . ? Y1A O2A C34A C21A -40.94(19) . . . . ? Y1A O2A C34A C29A 139.35(11) . . . . ? C22A C21A C34A O2A 175.68(13) . . . . ? C20A C21A C34A O2A -7.4(2) . . . . ? C22A C21A C34A C29A -4.6(2) . . . . ? C20A C21A C34A C29A 172.32(13) . . . . ? C28A C29A C34A O2A -175.75(13) . . . . ? C30A C29A C34A O2A 6.0(2) . . . . ? C28A C29A C34A C21A 4.5(2) . . . . ? C30A C29A C34A C21A -173.73(13) . . . . ? C20A N1A C35A C36A -151.64(11) . . . . ? C5A N1A C35A C36A 91.74(12) . . . . ? Y1A N1A C35A C36A -27.69(14) . . . . ? C37A N2A C36A C35A 70.89(17) . . . . ? C38A N2A C36A C35A -170.74(15) . . . . ? Y1A N2A C36A C35A -47.65(16) . . . . ? N1A C35A C36A N2A 52.22(18) . . . . ? O1B Y1B N1B C35B -96.28(10) . . . . ? O2B Y1B N1B C35B 100.37(10) . . . . ? O3B Y1B N1B C35B -179.40(9) . . . . ? N2B Y1B N1B C35B 4.68(8) . . . . ? Cl1B Y1B N1B C35B -4.43(16) . . . . ? O1B Y1B N1B C5B 141.11(9) . . . . ? O2B Y1B N1B C5B -22.23(8) . . . . ? O3B Y1B N1B C5B 58.00(9) . . . . ? N2B Y1B N1B C5B -117.93(8) . . . . ? Cl1B Y1B N1B C5B -127.03(9) . . . . ? O1B Y1B N1B C20B 26.63(9) . . . . ? O2B Y1B N1B C20B -136.71(10) . . . . ? O3B Y1B N1B C20B -56.48(10) . . . . ? N2B Y1B N1B C20B 127.59(9) . . . . ? Cl1B Y1B N1B C20B 118.48(10) . . . . ? O2B Y1B O1B C34B 63.47(17) . . . . ? O3B Y1B O1B C34B 131.69(12) . . . . ? N1B Y1B O1B C34B 24.69(12) . . . . ? N2B Y1B O1B C34B -44.08(12) . . . . ? Cl1B Y1B O1B C34B -135.06(12) . . . . ? O3B C1B C2B C3B -22.50(14) . . . . ? O1B Y1B N2B C37B -22.24(3) . . . . ? O2B Y1B N2B C37B -176.80(3) . . . . ? O3B Y1B N2B C37B -147.5(3) . . . . ? N1B Y1B N2B C37B -98.40(4) . . . . ? Cl1B Y1B N2B C37B 78.52(3) . . . . ? O1B Y1B N2B C38" 169.24(16) . . . . ? O2B Y1B N2B C38" 14.68(16) . . . . ? O3B Y1B N2B C38" 43.9(3) . . . . ? N1B Y1B N2B C38" 93.08(16) . . . . ? Cl1B Y1B N2B C38" -90.01(16) . . . . ? O1B Y1B N2B C37" -62.0(3) . . . . ? O2B Y1B N2B C37" 143.5(3) . . . . ? O3B Y1B N2B C37" 172.7(4) . . . . ? N1B Y1B N2B C37" -138.1(3) . . . . ? Cl1B Y1B N2B C37" 38.8(3) . . . . ? O1B Y1B N2B C38B -142.67(5) . . . . ? O2B Y1B N2B C38B 62.77(6) . . . . ? O3B Y1B N2B C38B 92.0(3) . . . . ? N1B Y1B N2B C38B 141.18(6) . . . . ? Cl1B Y1B N2B C38B -41.91(5) . . . . ? O1B Y1B N2B C36" 44.70(5) . . . . ? O2B Y1B N2B C36" -109.86(5) . . . . ? O3B Y1B N2B C36" -80.6(3) . . . . ? N1B Y1B N2B C36" -31.45(6) . . . . ? Cl1B Y1B N2B C36" 145.46(5) . . . . ? O1B Y1B N2B C36B 98.31(5) . . . . ? O2B Y1B N2B C36B -56.25(5) . . . . ? O3B Y1B N2B C36B -27.0(3) . . . . ? N1B Y1B N2B C36B 22.16(6) . . . . ? Cl1B Y1B N2B C36B -160.93(5) . . . . ? O1B Y1B O2B C19B -70.26(15) . . . . ? O3B Y1B O2B C19B -139.10(11) . . . . ? N1B Y1B O2B C19B -31.54(10) . . . . ? N2B Y1B O2B C19B 38.35(10) . . . . ? Cl1B Y1B O2B C19B 128.57(10) . . . . ? C1B C2B C3B C4B 39.17(17) . . . . ? C2B C1B O3B C4B -3.47(14) . . . . ? C2B C1B O3B Y1B 140.06(10) . . . . ? O1B Y1B O3B C1B 34.86(9) . . . . ? O2B Y1B O3B C1B -170.02(9) . . . . ? N1B Y1B O3B C1B 112.63(9) . . . . ? N2B Y1B O3B C1B 160.5(2) . . . . ? Cl1B Y1B O3B C1B -65.65(9) . . . . ? O1B Y1B O3B C4B 173.40(9) . . . . ? O2B Y1B O3B C4B -31.48(9) . . . . ? N1B Y1B O3B C4B -108.83(9) . . . . ? N2B Y1B O3B C4B -60.9(3) . . . . ? Cl1B Y1B O3B C4B 72.88(9) . . . . ? C1B O3B C4B C3B 28.70(15) . . . . ? Y1B O3B C4B C3B -114.36(12) . . . . ? C2B C3B C4B O3B -41.49(17) . . . . ? C35B N1B C5B C6B -57.26(16) . . . . ? C20B N1B C5B C6B -177.62(13) . . . . ? Y1B N1B C5B C6B 67.03(14) . . . . ? N1B C5B C6B C7B 112.15(15) . . . . ? N1B C5B C6B C19B -67.5(2) . . . . ? C19B C6B C7B C8B -1.7(2) . . . . ? C5B C6B C7B C8B 178.63(14) . . . . ? C6B C7B C8B C13B -2.8(2) . . . . ? C6B C7B C8B C9B 177.56(14) . . . . ? C13B C8B C9B C11B -126.34(16) . . . . ? C7B C8B C9B C11B 53.3(2) . . . . ? C13B C8B C9B C10B 113.71(16) . . . . ? C7B C8B C9B C10B -66.65(16) . . . . ? C13B C8B C9B C12B -6.1(2) . . . . ? C7B C8B C9B C12B 173.51(14) . . . . ? C7B C8B C13B C14B 2.0(2) . . . . ? C9B C8B C13B C14B -178.33(14) . . . . ? C8B C13B C14B C19B 3.2(2) . . . . ? C8B C13B C14B C15B -174.87(14) . . . . ? C13B C14B C15B C16B 4.2(2) . . . . ? C19B C14B C15B C16B -173.78(14) . . . . ? C13B C14B C15B C18B -116.32(15) . . . . ? C19B C14B C15B C18B 65.69(18) . . . . ? C13B C14B C15B C17B 122.60(15) . . . . ? C19B C14B C15B C17B -55.39(18) . . . . ? Y1B O2B C19B C6B 44.62(18) . . . . ? Y1B O2B C19B C14B -134.96(13) . . . . ? C7B C6B C19B O2B -172.51(14) . . . . ? C5B C6B C19B O2B 7.1(2) . . . . ? C7B C6B C19B C14B 7.1(2) . . . . ? C5B C6B C19B C14B -173.27(14) . . . . ? C13B C14B C19B O2B 171.97(14) . . . . ? C15B C14B C19B O2B -10.0(2) . . . . ? C13B C14B C19B C6B -7.6(2) . . . . ? C15B C14B C19B C6B 170.46(14) . . . . ? C35B N1B C20B C21B 55.43(15) . . . . ? C5B N1B C20B C21B 175.48(13) . . . . ? Y1B N1B C20B C21B -68.90(14) . . . . ? N1B C20B C21B C22B -117.10(14) . . . . ? N1B C20B C21B C34B 65.62(19) . . . . ? C34B C21B C22B C23B 0.2(2) . . . . ? C20B C21B C22B C23B -177.04(13) . . . . ? C21B C22B C23B C28B 2.2(2) . . . . ? C21B C22B C23B C24B -178.84(14) . . . . ? C22B C23B C24B C27B -6.6(2) . . . . ? C28B C23B C24B C27B 172.31(13) . . . . ? C22B C23B C24B C26B 114.15(15) . . . . ? C28B C23B C24B C26B -66.94(17) . . . . ? C22B C23B C24B C25B -126.48(14) . . . . ? C28B C23B C24B C25B 52.44(17) . . . . ? C22B C23B C28B C29B -1.1(2) . . . . ? C24B C23B C28B C29B 179.94(14) . . . . ? C23B C28B C29B C34B -2.3(2) . . . . ? C23B C28B C29B C30B 175.66(14) . . . . ? C28B C29B C30B C33B 119.96(16) . . . . ? C34B C29B C30B C33B -62.11(19) . . . . ? C28B C29B C30B C32B -0.6(2) . . . . ? C34B C29B C30B C32B 177.36(13) . . . . ? C28B C29B C30B C31B -118.83(16) . . . . ? C34B C29B C30B C31B 59.10(17) . . . . ? Y1B O1B C34B C21B -39.1(2) . . . . ? Y1B O1B C34B C29B 140.11(12) . . . . ? C22B C21B C34B O1B 175.54(13) . . . . ? C20B C21B C34B O1B -7.2(2) . . . . ? C22B C21B C34B C29B -3.7(2) . . . . ? C20B C21B C34B C29B 173.57(13) . . . . ? C28B C29B C34B O1B -174.56(13) . . . . ? C30B C29B C34B O1B 7.4(2) . . . . ? C28B C29B C34B C21B 4.6(2) . . . . ? C30B C29B C34B C21B -173.39(13) . . . . ? C5B N1B C35B C36B 90.33(11) . . . . ? C20B N1B C35B C36B -152.06(10) . . . . ? Y1B N1B C35B C36B -30.95(13) . . . . ? C5B N1B C35B C36" 144.33(11) . . . . ? C20B N1B C35B C36" -98.06(11) . . . . ? Y1B N1B C35B C36" 23.05(14) . . . . ? C37B N2B C36B C35B 71.30(14) . . . . ? C38" N2B C36B C35B -161.3(3) . . . . ? C37" N2B C36B C35B 102.8(2) . . . . ? C38B N2B C36B C35B -169.90(13) . . . . ? C36" N2B C36B C35B 44.87(14) . . . . ? Y1B N2B C36B C35B -47.94(13) . . . . ? N1B C35B C36B N2B 54.45(16) . . . . ? C36" C35B C36B N2B -44.47(12) . . . . ? C37B N2B C36" C35B 162.87(17) . . . . ? C38" N2B C36" C35B -70.2(3) . . . . ? C37" N2B C36" C35B 170.0(2) . . . . ? C38B N2B C36" C35B -109.93(17) . . . . ? C36B N2B C36" C35B -44.70(12) . . . . ? Y1B N2B C36" C35B 58.63(13) . . . . ? N1B C35B C36" N2B -57.59(17) . . . . ? C36B C35B C36" N2B 44.42(11) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.531 _refine_diff_density_min -0.364 _refine_diff_density_rms 0.070 _publ_section_references ; Bruker (2000) SAINTPlus Data Reduction and Correction Program v. 6.02a, Bruker AXS, Madison, Wisconsin, USA. Bruker (2000) SMART. Bruker Molecular Analysis Research Tool, v. 5.625 Bruker AXS, Madison, Wisconsin, USA. Sheldrick G.M. (1998a). SADABS v.2.01, Bruker/Siemens Area Detector Absorption Correction Program, Bruker AXS, Madison, Wisconsin, USA. Sheldrick G.M. (2000). SHELXTL v. 6.12, Structure Determination Software Suite, Bruker AXS, Madison, Wisconsin, USA. ; #===# END data_smnoclm _database_code_depnum_ccdc_archive 'CCDC 676934' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C41.50 H68 Cl N2 O4 Sm' _chemical_formula_weight 844.78 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' Sm Sm -0.1638 3.4418 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.6169(4) _cell_length_b 19.9748(6) _cell_length_c 17.6003(5) _cell_angle_alpha 90.00 _cell_angle_beta 94.0440(10) _cell_angle_gamma 90.00 _cell_volume 4424.6(2) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 900 _cell_measurement_theta_min 2 _cell_measurement_theta_max 28 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.268 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1768 _exptl_absorpt_coefficient_mu 1.425 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6353 _exptl_absorpt_correction_T_max 0.9321 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1998a)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type '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 24314 _diffrn_reflns_av_R_equivalents 0.0224 _diffrn_reflns_av_sigmaI/netI 0.0233 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.91 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7752 _reflns_number_gt 6750 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _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^)+(0.0382P)^2^+3.3000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7752 _refine_ls_number_parameters 451 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0319 _refine_ls_R_factor_gt 0.0259 _refine_ls_wR_factor_ref 0.0661 _refine_ls_wR_factor_gt 0.0636 _refine_ls_goodness_of_fit_ref 1.009 _refine_ls_restrained_S_all 1.009 _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 Sm1 Sm 0.419852(8) -0.164728(5) 0.636307(5) 0.01704(3) Uani 1 1 d . . . O1 O 0.55768(10) -0.10699(7) 0.60109(8) 0.0214(3) Uani 1 1 d . . . O2 O 0.27738(11) -0.22397(7) 0.60748(8) 0.0221(3) Uani 1 1 d . . . O3 O 0.39724(12) -0.04674(7) 0.69935(8) 0.0262(3) Uani 1 1 d . . . O4 O 0.29814(11) -0.08012(7) 0.56589(8) 0.0222(3) Uani 1 1 d . . . N1 N 0.44015(12) -0.20655(8) 0.49673(9) 0.0158(4) Uani 1 1 d . . . N2 N 0.54336(14) -0.27403(9) 0.63320(10) 0.0245(4) Uani 1 1 d . . . C1 C 0.49877(15) -0.15434(10) 0.45551(11) 0.0174(4) Uani 1 1 d . . . H1A H 0.4605 -0.1113 0.4592 0.021 Uiso 1 1 calc R . . H1B H 0.4962 -0.1667 0.4009 0.021 Uiso 1 1 calc R . . C2 C 0.61329(15) -0.14337(10) 0.48308(11) 0.0181(4) Uani 1 1 d . . . C3 C 0.69384(16) -0.16009(9) 0.43635(12) 0.0187(4) Uani 1 1 d . . . H3A H 0.6760 -0.1792 0.3877 0.022 Uiso 1 1 calc R . . C4 C 0.80029(16) -0.14917(10) 0.45993(12) 0.0210(5) Uani 1 1 d . . . C5 C 0.82135(16) -0.11794(10) 0.53044(12) 0.0217(5) Uani 1 1 d . . . H5A H 0.8934 -0.1087 0.5464 0.026 Uiso 1 1 calc R . . C6 C 0.74376(16) -0.09950(10) 0.57875(11) 0.0207(5) Uani 1 1 d . . . C7 C 0.63687(16) -0.11619(10) 0.55576(11) 0.0190(4) Uani 1 1 d . . . C8 C 0.89221(16) -0.17035(11) 0.41250(13) 0.0266(5) Uani 1 1 d . . . C9 C 0.85261(19) -0.20429(14) 0.33807(14) 0.0391(6) Uani 1 1 d . . . H9A H 0.8113 -0.2442 0.3494 0.059 Uiso 1 1 calc R . . H9B H 0.9135 -0.2174 0.3098 0.059 Uiso 1 1 calc R . . H9C H 0.8076 -0.1731 0.3073 0.059 Uiso 1 1 calc R . . Cl1 Cl 0.44058(5) -0.19582(3) 0.78469(3) 0.02949(13) Uani 1 1 d . . . C10 C 0.95800(18) -0.10868(12) 0.39358(14) 0.0334(6) Uani 1 1 d . . . H10A H 1.0166 -0.1224 0.3633 0.050 Uiso 1 1 calc R . . H10B H 0.9868 -0.0876 0.4409 0.050 Uiso 1 1 calc R . . H10C H 0.9126 -0.0766 0.3644 0.050 Uiso 1 1 calc R . . C11 C 0.96351(19) -0.21975(13) 0.45944(16) 0.0410(7) Uani 1 1 d . . . H11A H 0.9221 -0.2595 0.4713 0.062 Uiso 1 1 calc R . . H11B H 0.9907 -0.1982 0.5069 0.062 Uiso 1 1 calc R . . H11C H 1.0232 -0.2331 0.4301 0.062 Uiso 1 1 calc R . . C12 C 0.77142(17) -0.05952(11) 0.65222(12) 0.0268(5) Uani 1 1 d . . . C13 C 0.70755(19) 0.00627(12) 0.64876(14) 0.0352(6) Uani 1 1 d . . . H13A H 0.7240 0.0316 0.6034 0.053 Uiso 1 1 calc R . . H13B H 0.7266 0.0329 0.6944 0.053 Uiso 1 1 calc R . . H13C H 0.6314 -0.0039 0.6462 0.053 Uiso 1 1 calc R . . C14 C 0.74553(19) -0.09936(13) 0.72322(13) 0.0366(6) Uani 1 1 d . . . H14A H 0.7865 -0.1411 0.7256 0.055 Uiso 1 1 calc R . . H14B H 0.6695 -0.1098 0.7205 0.055 Uiso 1 1 calc R . . H14C H 0.7642 -0.0726 0.7689 0.055 Uiso 1 1 calc R . . C15 C 0.88999(18) -0.04098(13) 0.66169(13) 0.0344(6) Uani 1 1 d . . . H15A H 0.9094 -0.0156 0.6171 0.052 Uiso 1 1 calc R . . H15B H 0.9327 -0.0819 0.6664 0.052 Uiso 1 1 calc R . . H15C H 0.9034 -0.0136 0.7076 0.052 Uiso 1 1 calc R . . C16 C 0.33221(14) -0.21115(10) 0.45550(11) 0.0169(4) Uani 1 1 d . . . H16A H 0.3415 -0.2177 0.4006 0.020 Uiso 1 1 calc R . . H16B H 0.2955 -0.1678 0.4610 0.020 Uiso 1 1 calc R . . C17 C 0.26131(15) -0.26587(10) 0.48141(11) 0.0174(4) Uani 1 1 d . . . C18 C 0.22094(15) -0.31256(10) 0.42842(12) 0.0188(4) Uani 1 1 d . . . H18A H 0.2418 -0.3104 0.3776 0.023 Uiso 1 1 calc R . . C19 C 0.15098(16) -0.36224(10) 0.44791(11) 0.0200(5) Uani 1 1 d . . . C20 C 0.12091(16) -0.36226(11) 0.52289(12) 0.0230(5) Uani 1 1 d . . . H20A H 0.0717 -0.3953 0.5368 0.028 Uiso 1 1 calc R . . C21 C 0.15873(16) -0.31679(10) 0.57852(12) 0.0220(5) Uani 1 1 d . . . C22 C 0.23289(16) -0.26796(10) 0.55736(12) 0.0200(5) Uani 1 1 d . . . C23 C 0.10485(16) -0.41493(10) 0.39121(12) 0.0231(5) Uani 1 1 d . . . C24 C 0.14655(19) -0.40640(12) 0.31195(13) 0.0328(6) Uani 1 1 d . . . H24A H 0.1276 -0.3618 0.2922 0.049 Uiso 1 1 calc R . . H24B H 0.1146 -0.4405 0.2775 0.049 Uiso 1 1 calc R . . H24C H 0.2240 -0.4114 0.3156 0.049 Uiso 1 1 calc R . . C25 C -0.01695(18) -0.40891(12) 0.38300(14) 0.0337(6) Uani 1 1 d . . . H25A H -0.0368 -0.3640 0.3648 0.051 Uiso 1 1 calc R . . H25B H -0.0456 -0.4166 0.4326 0.051 Uiso 1 1 calc R . . H25C H -0.0460 -0.4423 0.3464 0.051 Uiso 1 1 calc R . . C26 C 0.1351(2) -0.48549(11) 0.41995(14) 0.0341(6) Uani 1 1 d . . . H26A H 0.1092 -0.4922 0.4706 0.051 Uiso 1 1 calc R . . H26B H 0.2126 -0.4904 0.4229 0.051 Uiso 1 1 calc R . . H26C H 0.1028 -0.5189 0.3847 0.051 Uiso 1 1 calc R . . C27 C 0.1193(2) -0.31727(12) 0.65905(13) 0.0333(6) Uani 1 1 d . . . C28 C 0.0358(2) -0.37264(13) 0.66822(14) 0.0410(6) Uani 1 1 d . . . H28A H 0.0674 -0.4164 0.6588 0.061 Uiso 1 1 calc R . . H28B H -0.0253 -0.3652 0.6316 0.061 Uiso 1 1 calc R . . H28C H 0.0123 -0.3714 0.7201 0.061 Uiso 1 1 calc R . . C29 C 0.0662(2) -0.25045(13) 0.67506(14) 0.0407(6) Uani 1 1 d . . . H29A H 0.1171 -0.2140 0.6699 0.061 Uiso 1 1 calc R . . H29B H 0.0426 -0.2507 0.7269 0.061 Uiso 1 1 calc R . . H29C H 0.0047 -0.2439 0.6386 0.061 Uiso 1 1 calc R . . C30 C 0.2110(2) -0.33048(13) 0.71906(14) 0.0429(7) Uani 1 1 d . . . H30A H 0.2446 -0.3734 0.7083 0.064 Uiso 1 1 calc R . . H30B H 0.1834 -0.3321 0.7697 0.064 Uiso 1 1 calc R . . H30C H 0.2635 -0.2945 0.7175 0.064 Uiso 1 1 calc R . . C31 C 0.49441(16) -0.27258(10) 0.49309(11) 0.0195(4) Uani 1 1 d . . . H31A H 0.5255 -0.2766 0.4432 0.023 Uiso 1 1 calc R . . H31B H 0.4409 -0.3085 0.4962 0.023 Uiso 1 1 calc R . . C32 C 0.58156(16) -0.28297(10) 0.55593(12) 0.0234(5) Uani 1 1 d . . . H32A H 0.6108 -0.3287 0.5517 0.028 Uiso 1 1 calc R . . H32B H 0.6398 -0.2508 0.5490 0.028 Uiso 1 1 calc R . . C33 C 0.4779(2) -0.33183(11) 0.65291(14) 0.0320(6) Uani 1 1 d . . . H33A H 0.5206 -0.3728 0.6523 0.048 Uiso 1 1 calc R . . H33B H 0.4167 -0.3358 0.6157 0.048 Uiso 1 1 calc R . . H33C H 0.4530 -0.3254 0.7039 0.048 Uiso 1 1 calc R . . C34 C 0.63812(19) -0.27198(13) 0.68755(14) 0.0358(6) Uani 1 1 d . . . H34A H 0.6793 -0.3132 0.6830 0.054 Uiso 1 1 calc R . . H34B H 0.6157 -0.2680 0.7396 0.054 Uiso 1 1 calc R . . H34C H 0.6822 -0.2334 0.6761 0.054 Uiso 1 1 calc R . . C35 C 0.4382(2) -0.02478(12) 0.77334(13) 0.0406(7) Uani 1 1 d . . . H35A H 0.4174 0.0219 0.7811 0.061 Uiso 1 1 calc R . . H35B H 0.5159 -0.0282 0.7770 0.061 Uiso 1 1 calc R . . H35C H 0.4094 -0.0530 0.8125 0.061 Uiso 1 1 calc R . . C36 C 0.34911(18) 0.00722(11) 0.65634(12) 0.0278(5) Uani 1 1 d . . . H36A H 0.3929 0.0482 0.6633 0.033 Uiso 1 1 calc R . . H36B H 0.2776 0.0167 0.6735 0.033 Uiso 1 1 calc R . . C37 C 0.34109(17) -0.01351(10) 0.57412(12) 0.0250(5) Uani 1 1 d . . . H37A H 0.2947 0.0183 0.5441 0.030 Uiso 1 1 calc R . . H37B H 0.4124 -0.0122 0.5541 0.030 Uiso 1 1 calc R . . C38 C 0.18481(17) -0.08173(12) 0.56679(15) 0.0348(6) Uani 1 1 d . . . H38A H 0.1541 -0.0447 0.5360 0.052 Uiso 1 1 calc R . . H38B H 0.1647 -0.0772 0.6193 0.052 Uiso 1 1 calc R . . H38C H 0.1580 -0.1244 0.5457 0.052 Uiso 1 1 calc R . . C1S C 0.4187(2) -0.45389(12) 0.49823(15) 0.0420(7) Uani 1 1 d . . . H1SA H 0.3627 -0.4220 0.4965 0.050 Uiso 1 1 calc R . . C2S C 0.5050(2) -0.44332(12) 0.45639(14) 0.0416(7) Uani 1 1 d . B . H2SA H 0.5084 -0.4039 0.4265 0.050 Uiso 1 1 calc R . . C3S C 0.5872(2) -0.48936(12) 0.45714(15) 0.0415(7) Uani 1 1 d . . . H3SA H 0.6464 -0.4821 0.4276 0.050 Uiso 0.50 1 calc PR A 1 C4S C 0.6739(5) -0.4793(3) 0.4143(3) 0.0531(16) Uani 0.50 1 d P B 2 H4SA H 0.7235 -0.5168 0.4222 0.080 Uiso 0.50 1 calc PR B 2 H4SB H 0.7097 -0.4376 0.4302 0.080 Uiso 0.50 1 calc PR B 2 H4SC H 0.6497 -0.4765 0.3602 0.080 Uiso 0.50 1 calc PR B 2 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 Sm1 0.02066(6) 0.01843(5) 0.01217(5) -0.00014(4) 0.00209(4) -0.00302(4) O1 0.0209(7) 0.0270(7) 0.0167(7) -0.0040(6) 0.0046(6) -0.0042(6) O2 0.0275(7) 0.0229(7) 0.0163(7) -0.0028(6) 0.0036(6) -0.0078(6) O3 0.0376(8) 0.0238(7) 0.0170(7) -0.0032(6) -0.0006(6) 0.0007(6) O4 0.0226(7) 0.0206(7) 0.0233(7) -0.0009(6) 0.0002(6) -0.0026(6) N1 0.0184(8) 0.0154(8) 0.0138(8) 0.0005(6) 0.0031(6) -0.0025(6) N2 0.0306(9) 0.0243(9) 0.0178(9) 0.0019(7) -0.0037(7) 0.0020(8) C1 0.0174(9) 0.0205(10) 0.0143(10) 0.0017(8) 0.0021(7) -0.0024(7) C2 0.0192(9) 0.0183(9) 0.0168(10) 0.0031(8) 0.0006(8) -0.0031(8) C3 0.0219(10) 0.0188(10) 0.0156(10) 0.0012(8) 0.0021(8) -0.0008(8) C4 0.0186(10) 0.0222(10) 0.0224(11) 0.0025(9) 0.0026(8) -0.0001(8) C5 0.0187(10) 0.0230(10) 0.0231(11) 0.0045(9) -0.0017(8) -0.0030(8) C6 0.0237(10) 0.0219(10) 0.0160(10) 0.0032(8) -0.0011(8) -0.0039(8) C7 0.0215(10) 0.0185(9) 0.0171(10) 0.0020(8) 0.0025(8) -0.0013(8) C8 0.0163(10) 0.0333(12) 0.0306(12) -0.0051(10) 0.0045(9) 0.0017(8) C9 0.0264(12) 0.0554(15) 0.0371(13) -0.0174(12) 0.0138(10) -0.0045(11) Cl1 0.0425(3) 0.0318(3) 0.0143(2) 0.0025(2) 0.0032(2) -0.0035(2) C10 0.0248(11) 0.0450(14) 0.0317(13) -0.0031(11) 0.0117(9) -0.0068(10) C11 0.0288(12) 0.0427(14) 0.0524(16) -0.0004(13) 0.0085(11) 0.0111(11) C12 0.0250(11) 0.0357(12) 0.0195(11) -0.0027(9) 0.0000(9) -0.0086(9) C13 0.0399(13) 0.0335(12) 0.0322(13) -0.0140(11) 0.0015(10) -0.0080(10) C14 0.0386(13) 0.0514(15) 0.0189(11) -0.0007(11) -0.0036(10) -0.0162(11) C15 0.0321(12) 0.0455(14) 0.0247(12) -0.0043(11) -0.0041(10) -0.0141(11) C16 0.0158(9) 0.0196(9) 0.0151(9) 0.0002(8) 0.0011(7) -0.0001(7) C17 0.0154(9) 0.0189(9) 0.0180(10) 0.0002(8) 0.0008(7) 0.0005(7) C18 0.0179(9) 0.0220(10) 0.0166(10) -0.0003(8) 0.0022(8) 0.0023(8) C19 0.0209(10) 0.0202(10) 0.0185(10) -0.0004(8) -0.0006(8) 0.0006(8) C20 0.0235(10) 0.0218(10) 0.0238(11) 0.0021(9) 0.0025(8) -0.0065(8) C21 0.0250(10) 0.0228(10) 0.0185(10) -0.0003(9) 0.0028(8) -0.0051(8) C22 0.0233(10) 0.0178(9) 0.0190(10) 0.0003(8) 0.0009(8) -0.0020(8) C23 0.0233(10) 0.0210(10) 0.0250(11) -0.0029(9) 0.0010(8) -0.0054(8) C24 0.0390(13) 0.0325(12) 0.0273(12) -0.0094(10) 0.0048(10) -0.0110(10) C25 0.0288(12) 0.0357(12) 0.0358(13) -0.0084(11) -0.0029(10) -0.0068(10) C26 0.0437(13) 0.0202(11) 0.0375(13) -0.0047(10) -0.0035(11) -0.0058(10) C27 0.0461(13) 0.0357(12) 0.0195(11) 0.0021(10) 0.0126(10) -0.0212(11) C28 0.0514(14) 0.0470(14) 0.0264(13) -0.0046(11) 0.0153(11) -0.0268(12) C29 0.0513(14) 0.0440(14) 0.0299(13) -0.0114(11) 0.0241(11) -0.0174(12) C30 0.0588(16) 0.0494(15) 0.0205(12) 0.0091(11) 0.0024(11) -0.0263(12) C31 0.0223(10) 0.0188(9) 0.0172(10) -0.0011(8) 0.0001(8) 0.0003(8) C32 0.0245(10) 0.0210(10) 0.0242(11) -0.0019(9) -0.0014(9) 0.0031(8) C33 0.0467(14) 0.0254(11) 0.0242(12) 0.0046(9) 0.0032(10) 0.0011(10) C34 0.0386(13) 0.0389(13) 0.0278(12) -0.0023(11) -0.0130(10) 0.0094(11) C35 0.0662(17) 0.0333(13) 0.0210(12) -0.0070(10) -0.0065(11) -0.0027(12) C36 0.0354(12) 0.0217(10) 0.0262(12) -0.0024(9) 0.0013(9) 0.0033(9) C37 0.0313(11) 0.0186(10) 0.0247(11) 0.0020(9) 0.0000(9) -0.0020(8) C38 0.0243(11) 0.0342(12) 0.0453(15) 0.0005(11) -0.0025(10) 0.0005(10) C1S 0.0536(15) 0.0317(13) 0.0374(14) -0.0107(11) -0.0213(12) 0.0082(11) C2S 0.0678(17) 0.0240(12) 0.0300(13) -0.0037(10) -0.0186(12) 0.0007(12) C3S 0.0528(15) 0.0334(13) 0.0365(14) -0.0086(11) -0.0113(12) -0.0017(12) C4S 0.050(3) 0.068(4) 0.041(3) -0.003(3) 0.000(3) -0.005(3) _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 Sm1 O2 2.1819(13) . ? Sm1 O1 2.2113(14) . ? Sm1 O4 2.5459(14) . ? Sm1 N1 2.6243(16) . ? Sm1 O3 2.6290(14) . ? Sm1 Cl1 2.6792(5) . ? Sm1 N2 2.6852(17) . ? O1 C7 1.335(2) . ? O2 C22 1.340(2) . ? O3 C36 1.428(3) . ? O3 C35 1.436(3) . ? O4 C38 1.431(3) . ? O4 C37 1.440(2) . ? N1 C31 1.489(2) . ? N1 C1 1.496(2) . ? N1 C16 1.500(2) . ? N2 C33 1.475(3) . ? N2 C34 1.478(3) . ? N2 C32 1.485(3) . ? C1 C2 1.507(3) . ? C2 C3 1.392(3) . ? C2 C7 1.402(3) . ? C3 C4 1.395(3) . ? C4 C5 1.398(3) . ? C4 C8 1.535(3) . ? C5 C6 1.391(3) . ? C6 C7 1.420(3) . ? C6 C12 1.539(3) . ? C8 C9 1.527(3) . ? C8 C10 1.535(3) . ? C8 C11 1.536(3) . ? C12 C14 1.536(3) . ? C12 C15 1.539(3) . ? C12 C13 1.540(3) . ? C16 C17 1.503(3) . ? C17 C18 1.390(3) . ? C17 C22 1.409(3) . ? C18 C19 1.387(3) . ? C19 C20 1.399(3) . ? C19 C23 1.536(3) . ? C20 C21 1.395(3) . ? C21 C22 1.419(3) . ? C21 C27 1.535(3) . ? C23 C24 1.535(3) . ? C23 C26 1.536(3) . ? C23 C25 1.538(3) . ? C27 C29 1.528(4) . ? C27 C30 1.533(4) . ? C27 C28 1.543(3) . ? C31 C32 1.518(3) . ? C36 C37 1.502(3) . ? C1S C2S 1.373(4) . ? C1S C3S 1.384(4) 3_646 ? C2S C3S 1.386(4) . ? C3S C1S 1.384(4) 3_646 ? C3S C4S 1.386(6) . ? 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 O2 Sm1 O1 150.34(5) . . ? O2 Sm1 O4 77.77(5) . . ? O1 Sm1 O4 88.66(5) . . ? O2 Sm1 N1 75.10(5) . . ? O1 Sm1 N1 76.88(5) . . ? O4 Sm1 N1 81.43(5) . . ? O2 Sm1 O3 118.18(5) . . ? O1 Sm1 O3 76.21(5) . . ? O4 Sm1 O3 62.01(4) . . ? N1 Sm1 O3 134.51(5) . . ? O2 Sm1 Cl1 97.07(4) . . ? O1 Sm1 Cl1 111.68(4) . . ? O4 Sm1 Cl1 129.97(3) . . ? N1 Sm1 Cl1 146.04(4) . . ? O3 Sm1 Cl1 78.61(3) . . ? O2 Sm1 N2 91.38(5) . . ? O1 Sm1 N2 87.10(5) . . ? O4 Sm1 N2 149.41(5) . . ? N1 Sm1 N2 68.10(5) . . ? O3 Sm1 N2 144.88(5) . . ? Cl1 Sm1 N2 79.31(4) . . ? C7 O1 Sm1 137.10(12) . . ? C22 O2 Sm1 143.97(13) . . ? C36 O3 C35 111.28(16) . . ? C36 O3 Sm1 120.51(11) . . ? C35 O3 Sm1 127.87(13) . . ? C38 O4 C37 112.88(16) . . ? C38 O4 Sm1 123.25(13) . . ? C37 O4 Sm1 110.77(11) . . ? C31 N1 C1 110.62(15) . . ? C31 N1 C16 109.22(14) . . ? C1 N1 C16 105.73(14) . . ? C31 N1 Sm1 113.43(11) . . ? C1 N1 Sm1 108.45(11) . . ? C16 N1 Sm1 109.10(11) . . ? C33 N2 C34 108.07(18) . . ? C33 N2 C32 110.14(17) . . ? C34 N2 C32 107.22(17) . . ? C33 N2 Sm1 107.25(13) . . ? C34 N2 Sm1 114.10(13) . . ? C32 N2 Sm1 110.04(12) . . ? N1 C1 C2 116.15(16) . . ? C3 C2 C7 121.00(18) . . ? C3 C2 C1 119.87(18) . . ? C7 C2 C1 119.13(18) . . ? C2 C3 C4 120.96(19) . . ? C3 C4 C5 116.93(19) . . ? C3 C4 C8 122.92(19) . . ? C5 C4 C8 120.14(18) . . ? C6 C5 C4 124.27(18) . . ? C5 C6 C7 117.31(18) . . ? C5 C6 C12 121.57(18) . . ? C7 C6 C12 121.05(18) . . ? O1 C7 C2 118.63(17) . . ? O1 C7 C6 122.23(18) . . ? C2 C7 C6 119.14(18) . . ? C9 C8 C10 108.6(2) . . ? C9 C8 C4 112.01(17) . . ? C10 C8 C4 109.73(18) . . ? C9 C8 C11 108.7(2) . . ? C10 C8 C11 109.09(19) . . ? C4 C8 C11 108.70(19) . . ? C14 C12 C6 111.48(18) . . ? C14 C12 C15 107.30(18) . . ? C6 C12 C15 112.15(18) . . ? C14 C12 C13 109.48(19) . . ? C6 C12 C13 108.81(17) . . ? C15 C12 C13 107.51(19) . . ? N1 C16 C17 115.92(15) . . ? C18 C17 C22 120.72(18) . . ? C18 C17 C16 118.81(17) . . ? C22 C17 C16 120.41(17) . . ? C19 C18 C17 121.57(19) . . ? C18 C19 C20 116.95(18) . . ? C18 C19 C23 123.23(18) . . ? C20 C19 C23 119.81(18) . . ? C21 C20 C19 124.05(19) . . ? C20 C21 C22 117.55(19) . . ? C20 C21 C27 121.79(19) . . ? C22 C21 C27 120.62(18) . . ? O2 C22 C17 118.84(17) . . ? O2 C22 C21 122.08(18) . . ? C17 C22 C21 119.08(18) . . ? C24 C23 C19 112.08(17) . . ? C24 C23 C26 107.94(19) . . ? C19 C23 C26 109.91(17) . . ? C24 C23 C25 108.08(18) . . ? C19 C23 C25 109.73(17) . . ? C26 C23 C25 109.03(18) . . ? C29 C27 C30 110.0(2) . . ? C29 C27 C21 109.86(19) . . ? C30 C27 C21 111.0(2) . . ? C29 C27 C28 107.2(2) . . ? C30 C27 C28 107.0(2) . . ? C21 C27 C28 111.67(19) . . ? N1 C31 C32 113.66(16) . . ? N2 C32 C31 112.68(17) . . ? O3 C36 C37 107.46(17) . . ? O4 C37 C36 110.55(17) . . ? C2S C1S C3S 120.5(2) . 3_646 ? C1S C2S C3S 120.9(2) . . ? C1S C3S C2S 118.6(3) 3_646 . ? C1S C3S C4S 120.2(4) 3_646 . ? C2S C3S C4S 121.2(4) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.367 _refine_diff_density_min -0.523 _refine_diff_density_rms 0.074 _publ_section_references ; Bruker (2000) SAINTPlus Data Reduction and Correction Program v. 6.02a, Bruker AXS, Madison, Wisconsin, USA. Bruker (2000) SMART. Bruker Molecular Analysis Research Tool, v. 5.625 Bruker AXS, Madison, Wisconsin, USA. Sheldrick G.M. (1998a). SADABS v.2.01, Bruker/Siemens Area Detector Absorption Correction Program, Bruker AXS, Madison, Wisconsin, USA. Sheldrick G.M. (2000). SHELXTL v. 6.12, Structure Determination Software Suite, Bruker AXS, Madison, Wisconsin, USA. ;