# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_coden_Cambridge 182 loop_ _publ_author_name 'Andrew Wilson' 'Fred Campbell' 'Christopher Carruthers' 'Michaele J. Hardie' 'Jeffrey Plante' 'Timothy J. Prior' _publ_contact_author_name 'Andrew J. Wilson' _publ_contact_author_address ; Department of Chemistry University of Leeds Woodhouse Lane Leeds LS2 9JT UNITED KINGDOM ; _publ_contact_author_email A.J.WILSON@LEEDS.AC.UK _publ_requested_journal 'Chemical Communications' _publ_section_title ; Macrocyclic scaffolds derived from para-aminobenzoic acid ; data_1a _database_code_depnum_ccdc_archive 'CCDC 641457' _chemical_name_systematic ; 2,8,14, Tri-n-propyl-2,8-14-triazatetracyclo[142,24,7,210,13] tetracosa-4,6,10,12,16,18,19,21,23-nonaene-3,9,15trione ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety (trimer)4(toluene)4 _chemical_formula_sum 'C37 H41 N3 O3' _chemical_formula_weight 575.73 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' _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 26.934(3) _cell_length_b 9.8762(12) _cell_length_c 47.994(6) _cell_angle_alpha 90.00 _cell_angle_beta 94.7120(10) _cell_angle_gamma 90.00 _cell_volume 12723(3) _cell_formula_units_Z 16 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9325 _cell_measurement_theta_min 4.612 _cell_measurement_theta_max 26.58 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.202 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4928 _exptl_absorpt_coefficient_mu 0.076 _exptl_absorpt_correction_type multiscan _exptl_absorpt_correction_T_min 0.9901 _exptl_absorpt_correction_T_max 0.9985 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.79770 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'Daresbury SRS, Station 16.2SMX' _diffrn_radiation_monochromator 'silicon 111' _diffrn_measurement_device_type 'Bruker D8 diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_type 'APEXII CCD' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 66070 _diffrn_reflns_av_R_equivalents 0.0690 _diffrn_reflns_av_sigmaI/netI 0.0650 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -52 _diffrn_reflns_limit_l_max 52 _diffrn_reflns_theta_min 4.61 _diffrn_reflns_theta_max 26.00 _reflns_number_total 17528 _reflns_number_gt 12870 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX-II (Bruker)' _computing_cell_refinement 'APEX-II (Bruker)' _computing_data_reduction 'APEX-II (Bruker)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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. Crystal has a small twin component and the 12 worst affected reflections were omitted from the data. One alkyl arm was disordered over two positions and the disordered atoms were refined isotropically and the C-C bond lengths were restrained to be chemically reasonable. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type block _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0783P)^2^+15.0367P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 17528 _refine_ls_number_parameters 1564 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0939 _refine_ls_R_factor_gt 0.0674 _refine_ls_wR_factor_ref 0.1831 _refine_ls_wR_factor_gt 0.1679 _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_restrained_S_all 1.060 _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 O1 O 0.19413(10) 0.5316(3) 0.55438(5) 0.0480(7) Uani 1 1 d . . . N1 N 0.25279(11) 0.6243(3) 0.58494(6) 0.0318(7) Uani 1 1 d . . . C1 C 0.40105(14) 0.7598(4) 0.60101(7) 0.0353(9) Uani 1 1 d . . . O2 O 0.43859(10) 0.6384(3) 0.45566(6) 0.0464(7) Uani 1 1 d . . . N2 N 0.35883(11) 0.6517(3) 0.46847(6) 0.0304(7) Uani 1 1 d . . . C2 C 0.36136(15) 0.8485(4) 0.60282(8) 0.0407(10) Uani 1 1 d . . . H2 H 0.3677 0.9404 0.6077 0.049 Uiso 1 1 calc R . . O3 O 0.46746(11) 0.8646(3) 0.62869(6) 0.0594(9) Uani 1 1 d . . . N3 N 0.48361(11) 0.7973(3) 0.58539(6) 0.0365(8) Uani 1 1 d . . . C3 C 0.31287(15) 0.8044(4) 0.59759(8) 0.0388(9) Uani 1 1 d . . . H3 H 0.2861 0.8665 0.5984 0.047 Uiso 1 1 calc R . . O4 O 0.06037(9) 0.1341(3) 0.54780(5) 0.0351(6) Uani 1 1 d . . . N4 N 0.14097(10) 0.1503(3) 0.53670(5) 0.0246(6) Uani 1 1 d . . . C4 C 0.30329(13) 0.6703(4) 0.59112(7) 0.0307(8) Uani 1 1 d . . . O5 O 0.04284(9) 0.3183(3) 0.37228(5) 0.0384(6) Uani 1 1 d . . . N5 N 0.02472(10) 0.2793(3) 0.41690(5) 0.0253(6) Uani 1 1 d . . . C5 C 0.34267(13) 0.5794(4) 0.59079(8) 0.0340(9) Uani 1 1 d . . . H5 H 0.3361 0.4860 0.5875 0.041 Uiso 1 1 calc R . . O6 O 0.31497(8) 0.0366(3) 0.45616(5) 0.0362(6) Uani 1 1 d . . . N6 N 0.24889(10) 0.0499(3) 0.42334(5) 0.0255(6) Uani 1 1 d . . . C6 C 0.39119(14) 0.6243(4) 0.59520(8) 0.0378(9) Uani 1 1 d . . . H6 H 0.4179 0.5622 0.5943 0.045 Uiso 1 1 calc R . . O7 O -0.06510(9) 0.9130(3) 0.31212(5) 0.0427(7) Uani 1 1 d . . . N7 N -0.00578(10) 0.7893(3) 0.33721(6) 0.0267(7) Uani 1 1 d . . . C7 C 0.23561(13) 0.5817(4) 0.55901(7) 0.0314(8) Uani 1 1 d . . . O8 O 0.18800(10) 0.9268(3) 0.21430(5) 0.0447(7) Uani 1 1 d . . . N8 N 0.10942(11) 0.9339(3) 0.22781(6) 0.0297(7) Uani 1 1 d . . . C8 C 0.26868(12) 0.6034(4) 0.53569(7) 0.0278(8) Uani 1 1 d . . . O9 O 0.21704(10) 0.6024(3) 0.37992(5) 0.0477(7) Uani 1 1 d . . . N9 N 0.23295(10) 0.7144(3) 0.34035(6) 0.0305(7) Uani 1 1 d . . . C9 C 0.26719(13) 0.7228(4) 0.52056(7) 0.0311(8) Uani 1 1 d . . . H9 H 0.2459 0.7941 0.5255 0.037 Uiso 1 1 calc R . . O10 O 0.25944(10) 0.4038(3) 0.13248(5) 0.0466(7) Uani 1 1 d . . . N10 N 0.24966(10) 0.3565(3) 0.17800(6) 0.0261(6) Uani 1 1 d . . . C10 C 0.29641(13) 0.7401(4) 0.49823(7) 0.0318(9) Uani 1 1 d . . . H10 H 0.2951 0.8223 0.4879 0.038 Uiso 1 1 calc R . . O11 O 0.54872(9) 0.1417(3) 0.19970(5) 0.0471(7) Uani 1 1 d . . . N11 N 0.48271(10) 0.2132(3) 0.17122(6) 0.0296(7) Uani 1 1 d . B . C11 C 0.32758(12) 0.6353(3) 0.49119(7) 0.0261(8) Uani 1 1 d . . . O12 O 0.31050(9) 0.1955(3) 0.30603(5) 0.0407(7) Uani 1 1 d . . . N12 N 0.38824(10) 0.2106(3) 0.29092(6) 0.0274(7) Uani 1 1 d . . . C12 C 0.32852(13) 0.5150(3) 0.50594(7) 0.0287(8) Uani 1 1 d . . . H12 H 0.3496 0.4433 0.5010 0.034 Uiso 1 1 calc R . . C13 C 0.29895(13) 0.4986(4) 0.52780(7) 0.0296(8) Uani 1 1 d . . . H13 H 0.2993 0.4149 0.5376 0.036 Uiso 1 1 calc R . . C14 C 0.40967(14) 0.6564(4) 0.47382(8) 0.0339(9) Uani 1 1 d . . . C15 C 0.42802(13) 0.6914(4) 0.50314(8) 0.0319(9) Uani 1 1 d . . . C16 C 0.45935(13) 0.6036(4) 0.51903(8) 0.0349(9) Uani 1 1 d . . . H16 H 0.4683 0.5194 0.5113 0.042 Uiso 1 1 calc R . . C17 C 0.47760(13) 0.6371(4) 0.54582(8) 0.0344(9) Uani 1 1 d . . . H17 H 0.4987 0.5759 0.5565 0.041 Uiso 1 1 calc R . . C18 C 0.46507(13) 0.7605(4) 0.55716(8) 0.0327(9) Uani 1 1 d . . . C19 C 0.43427(13) 0.8506(4) 0.54156(8) 0.0360(9) Uani 1 1 d . . . H19 H 0.4257 0.9352 0.5493 0.043 Uiso 1 1 calc R . . C20 C 0.41616(14) 0.8158(4) 0.51462(8) 0.0346(9) Uani 1 1 d . . . H20 H 0.3954 0.8775 0.5039 0.042 Uiso 1 1 calc R . . C21 C 0.45348(15) 0.8122(4) 0.60634(8) 0.0396(10) Uani 1 1 d . . . C22 C 0.22134(14) 0.6066(4) 0.60843(7) 0.0361(9) Uani 1 1 d . . . H22A H 0.1862 0.6250 0.6018 0.043 Uiso 1 1 calc R . . H22B H 0.2314 0.6736 0.6232 0.043 Uiso 1 1 calc R . . C23 C 0.22513(17) 0.4656(4) 0.62087(8) 0.0492(11) Uani 1 1 d . . . H23A H 0.2605 0.4444 0.6265 0.059 Uiso 1 1 calc R . . H23B H 0.2127 0.3986 0.6066 0.059 Uiso 1 1 calc R . . C24 C 0.19493(19) 0.4549(5) 0.64617(9) 0.0574(12) Uani 1 1 d . . . H24A H 0.2084 0.5178 0.6607 0.086 Uiso 1 1 calc R . . H24B H 0.1969 0.3622 0.6535 0.086 Uiso 1 1 calc R . . H24C H 0.1601 0.4779 0.6407 0.086 Uiso 1 1 calc R . . C25 C 0.33576(14) 0.6341(4) 0.43985(7) 0.0350(9) Uani 1 1 d . . . H25A H 0.3603 0.6582 0.4264 0.042 Uiso 1 1 calc R . . H25B H 0.3072 0.6971 0.4368 0.042 Uiso 1 1 calc R . . C26 C 0.31749(16) 0.4897(4) 0.43389(8) 0.0441(10) Uani 1 1 d . . . H26A H 0.2932 0.4655 0.4475 0.053 Uiso 1 1 calc R . . H26B H 0.2998 0.4867 0.4150 0.053 Uiso 1 1 calc R . . C27 C 0.35856(18) 0.3859(4) 0.43551(10) 0.0583(12) Uani 1 1 d . . . H27A H 0.3810 0.4038 0.4208 0.087 Uiso 1 1 calc R . . H27B H 0.3441 0.2953 0.4329 0.087 Uiso 1 1 calc R . . H27C H 0.3773 0.3912 0.4539 0.087 Uiso 1 1 calc R . . C28 C 0.53429(16) 0.8522(4) 0.58899(10) 0.0523(12) Uani 1 1 d . . . H28A H 0.5557 0.8057 0.5762 0.063 Uiso 1 1 calc R . . H28B H 0.5485 0.8366 0.6084 0.063 Uiso 1 1 calc R . . C29 C 0.53294(17) 1.0107(5) 0.58248(11) 0.0664(14) Uani 1 1 d . . . H29A H 0.5203 1.0257 0.5628 0.080 Uiso 1 1 calc R . . H29B H 0.5099 1.0561 0.5946 0.080 Uiso 1 1 calc R . . C30 C 0.5829(2) 1.0699(6) 0.58745(13) 0.0814(17) Uani 1 1 d . . . H30A H 0.5947 1.0585 0.6072 0.122 Uiso 1 1 calc R . . H30B H 0.5815 1.1665 0.5828 0.122 Uiso 1 1 calc R . . H30C H 0.6057 1.0241 0.5757 0.122 Uiso 1 1 calc R . . C31 C 0.23631(12) 0.0933(3) 0.47214(7) 0.0245(8) Uani 1 1 d . . . C32 C 0.20112(13) -0.0033(3) 0.47760(7) 0.0276(8) Uani 1 1 d . . . H32 H 0.1978 -0.0826 0.4664 0.033 Uiso 1 1 calc R . . C33 C 0.17076(12) 0.0142(3) 0.49911(7) 0.0255(8) Uani 1 1 d . . . H33 H 0.1476 -0.0543 0.5031 0.031 Uiso 1 1 calc R . . C34 C 0.17408(12) 0.1324(3) 0.51489(6) 0.0229(8) Uani 1 1 d . . . C35 C 0.20901(12) 0.2307(3) 0.50963(7) 0.0260(8) Uani 1 1 d . . . H35 H 0.2113 0.3116 0.5204 0.031 Uiso 1 1 calc R . . C36 C 0.24050(12) 0.2099(3) 0.48860(7) 0.0257(8) Uani 1 1 d . . . H36 H 0.2651 0.2755 0.4854 0.031 Uiso 1 1 calc R . . C37 C 0.09065(12) 0.1504(3) 0.53033(7) 0.0258(8) Uani 1 1 d . . . C38 C 0.07410(12) 0.1808(3) 0.50035(7) 0.0236(8) Uani 1 1 d . . . C39 C 0.04612(12) 0.0882(3) 0.48370(7) 0.0274(8) Uani 1 1 d . . . H39 H 0.0381 0.0027 0.4912 0.033 Uiso 1 1 calc R . . C40 C 0.02992(12) 0.1196(3) 0.45634(7) 0.0248(8) Uani 1 1 d . . . H40 H 0.0109 0.0561 0.4451 0.030 Uiso 1 1 calc R . . C41 C 0.04170(12) 0.2450(3) 0.44550(7) 0.0238(8) Uani 1 1 d . . . C42 C 0.06909(12) 0.3389(3) 0.46189(7) 0.0260(8) Uani 1 1 d . . . H42 H 0.0767 0.4248 0.4544 0.031 Uiso 1 1 calc R . . C43 C 0.08532(12) 0.3061(3) 0.48933(7) 0.0264(8) Uani 1 1 d . . . H43 H 0.1042 0.3699 0.5006 0.032 Uiso 1 1 calc R . . C44 C 0.05534(12) 0.2770(3) 0.39607(7) 0.0254(8) Uani 1 1 d . . . C45 C 0.10608(12) 0.2169(3) 0.40320(7) 0.0251(8) Uani 1 1 d . . . C46 C 0.14691(12) 0.3010(4) 0.40954(7) 0.0280(8) Uani 1 1 d . . . H46 H 0.1428 0.3965 0.4095 0.034 Uiso 1 1 calc R . . C47 C 0.19372(13) 0.2443(4) 0.41586(7) 0.0295(8) Uani 1 1 d . . . H47 H 0.2216 0.3017 0.4202 0.035 Uiso 1 1 calc R . . C48 C 0.20019(12) 0.1055(3) 0.41594(7) 0.0258(8) Uani 1 1 d . . . C49 C 0.15997(13) 0.0214(4) 0.40885(7) 0.0293(8) Uani 1 1 d . . . H49 H 0.1645 -0.0739 0.4082 0.035 Uiso 1 1 calc R . . C50 C 0.11313(13) 0.0770(3) 0.40277(7) 0.0286(8) Uani 1 1 d . . . H50 H 0.0855 0.0192 0.3982 0.034 Uiso 1 1 calc R . . C51 C 0.27070(12) 0.0616(3) 0.44989(7) 0.0261(8) Uani 1 1 d . . . C52 C 0.16279(14) 0.1420(4) 0.56585(7) 0.0326(9) Uani 1 1 d . . . H52A H 0.1368 0.1641 0.5786 0.039 Uiso 1 1 calc R . . H52B H 0.1896 0.2103 0.5688 0.039 Uiso 1 1 calc R . . C53 C 0.18400(14) 0.0029(4) 0.57319(8) 0.0376(9) Uani 1 1 d . . . H53A H 0.2095 -0.0194 0.5602 0.045 Uiso 1 1 calc R . . H53B H 0.2007 0.0058 0.5923 0.045 Uiso 1 1 calc R . . C54 C 0.14520(16) -0.1079(4) 0.57176(9) 0.0494(11) Uani 1 1 d . . . H54A H 0.1219 -0.0922 0.5861 0.074 Uiso 1 1 calc R . . H54B H 0.1616 -0.1957 0.5751 0.074 Uiso 1 1 calc R . . H54C H 0.1270 -0.1077 0.5532 0.074 Uiso 1 1 calc R . . C55 C -0.02577(12) 0.3360(3) 0.41220(7) 0.0290(8) Uani 1 1 d . . . H55A H -0.0489 0.2805 0.4224 0.035 Uiso 1 1 calc R . . H55B H -0.0367 0.3304 0.3920 0.035 Uiso 1 1 calc R . . C56 C -0.02911(13) 0.4819(4) 0.42158(8) 0.0327(9) Uani 1 1 d . . . H56A H -0.0072 0.5387 0.4108 0.039 Uiso 1 1 calc R . . H56B H -0.0171 0.4888 0.4416 0.039 Uiso 1 1 calc R . . C57 C -0.08270(14) 0.5354(4) 0.41742(10) 0.0468(11) Uani 1 1 d . . . H57A H -0.0946 0.5292 0.3976 0.070 Uiso 1 1 calc R . . H57B H -0.0835 0.6301 0.4234 0.070 Uiso 1 1 calc R . . H57C H -0.1042 0.4811 0.4285 0.070 Uiso 1 1 calc R . . C58 C 0.27350(14) -0.0271(4) 0.40191(7) 0.0328(9) Uani 1 1 d . . . H58A H 0.2548 -0.1121 0.3978 0.039 Uiso 1 1 calc R . . H58B H 0.3076 -0.0517 0.4095 0.039 Uiso 1 1 calc R . . C59 C 0.27669(14) 0.0505(4) 0.37498(7) 0.0359(9) Uani 1 1 d . . . H59A H 0.2919 -0.0091 0.3614 0.043 Uiso 1 1 calc R . . H59B H 0.2424 0.0717 0.3671 0.043 Uiso 1 1 calc R . . C60 C 0.30597(16) 0.1803(4) 0.37746(8) 0.0457(10) Uani 1 1 d . . . H60A H 0.2895 0.2440 0.3894 0.069 Uiso 1 1 calc R . . H60B H 0.3078 0.2199 0.3589 0.069 Uiso 1 1 calc R . . H60C H 0.3397 0.1615 0.3858 0.069 Uiso 1 1 calc R . . C61 C 0.14750(12) 0.7022(4) 0.35394(7) 0.0276(8) Uani 1 1 d . . . C62 C 0.13167(13) 0.8353(4) 0.34837(7) 0.0280(8) Uani 1 1 d . . . H62 H 0.1556 0.9058 0.3477 0.034 Uiso 1 1 calc R . . C63 C 0.08118(12) 0.8649(4) 0.34387(7) 0.0267(8) Uani 1 1 d . . . H63 H 0.0705 0.9559 0.3411 0.032 Uiso 1 1 calc R . . C64 C 0.04624(12) 0.7602(3) 0.34350(6) 0.0233(8) Uani 1 1 d . . . C65 C 0.06158(13) 0.6304(3) 0.35002(7) 0.0285(8) Uani 1 1 d . . . H65 H 0.0377 0.5600 0.3508 0.034 Uiso 1 1 calc R . . C66 C 0.11191(13) 0.6019(4) 0.35550(7) 0.0310(8) Uani 1 1 d . . . H66 H 0.1221 0.5123 0.3604 0.037 Uiso 1 1 calc R . . C67 C -0.02268(13) 0.8643(4) 0.31450(7) 0.0302(8) Uani 1 1 d . . . C68 C 0.01153(12) 0.8817(3) 0.29154(7) 0.0268(8) Uani 1 1 d . . . C69 C 0.02496(13) 1.0100(4) 0.28334(7) 0.0334(9) Uani 1 1 d . . . H69 H 0.0118 1.0874 0.2919 0.040 Uiso 1 1 calc R . . C70 C 0.05749(14) 1.0262(4) 0.26265(7) 0.0345(9) Uani 1 1 d . . . H70 H 0.0677 1.1145 0.2578 0.041 Uiso 1 1 calc R . . C71 C 0.07513(13) 0.9149(4) 0.24906(7) 0.0288(8) Uani 1 1 d . . . C72 C 0.05948(13) 0.7865(4) 0.25610(7) 0.0297(8) Uani 1 1 d . . . H72 H 0.0698 0.7099 0.2461 0.036 Uiso 1 1 calc R . . C73 C 0.02906(13) 0.7693(4) 0.27760(7) 0.0293(8) Uani 1 1 d . . . H73 H 0.0200 0.6807 0.2830 0.035 Uiso 1 1 calc R . . C74 C 0.15884(13) 0.9062(3) 0.23214(7) 0.0282(8) Uani 1 1 d . . . C75 C 0.17744(12) 0.8523(3) 0.26025(7) 0.0260(8) Uani 1 1 d . . . C76 C 0.20082(13) 0.9406(3) 0.27967(7) 0.0288(8) Uani 1 1 d . . . H76 H 0.2035 1.0338 0.2751 0.035 Uiso 1 1 calc R . . C77 C 0.22012(12) 0.8954(3) 0.30549(7) 0.0276(8) Uani 1 1 d . . . H77 H 0.2371 0.9564 0.3183 0.033 Uiso 1 1 calc R . . C78 C 0.21470(12) 0.7610(3) 0.31278(7) 0.0262(8) Uani 1 1 d . . . C79 C 0.19273(13) 0.6703(4) 0.29339(7) 0.0316(9) Uani 1 1 d . . . H79 H 0.1901 0.5772 0.2980 0.038 Uiso 1 1 calc R . . C80 C 0.17467(13) 0.7166(3) 0.26716(7) 0.0296(8) Uani 1 1 d . . . H80 H 0.1602 0.6542 0.2538 0.035 Uiso 1 1 calc R . . C81 C 0.20160(13) 0.6678(4) 0.35916(7) 0.0330(9) Uani 1 1 d . . . C82 C -0.03994(14) 0.7600(4) 0.35910(7) 0.0339(9) Uani 1 1 d . . . H82A H -0.0363 0.6639 0.3647 0.041 Uiso 1 1 calc R . . H82B H -0.0747 0.7740 0.3513 0.041 Uiso 1 1 calc R . . C83 C -0.02973(15) 0.8494(4) 0.38477(8) 0.0424(10) Uani 1 1 d . . . H83A H -0.0517 0.8208 0.3992 0.051 Uiso 1 1 calc R . . H83B H 0.0051 0.8355 0.3924 0.051 Uiso 1 1 calc R . . C84 C -0.03770(17) 0.9963(4) 0.37901(9) 0.0508(11) Uani 1 1 d . . . H84A H -0.0135 1.0280 0.3663 0.076 Uiso 1 1 calc R . . H84B H -0.0333 1.0471 0.3966 0.076 Uiso 1 1 calc R . . H84C H -0.0715 1.0106 0.3703 0.076 Uiso 1 1 calc R . . C85 C 0.08994(15) 1.0008(4) 0.20153(8) 0.0397(10) Uani 1 1 d . . . H85A H 0.1180 1.0186 0.1899 0.048 Uiso 1 1 calc R . . H85B H 0.0752 1.0890 0.2061 0.048 Uiso 1 1 calc R . . C86 C 0.05135(15) 0.9177(5) 0.18492(8) 0.0496(11) Uani 1 1 d . . . H86A H 0.0232 0.9013 0.1965 0.060 Uiso 1 1 calc R . . H86B H 0.0385 0.9705 0.1683 0.060 Uiso 1 1 calc R . . C87 C 0.07001(19) 0.7838(5) 0.17529(9) 0.0624(13) Uani 1 1 d . . . H87A H 0.0974 0.7988 0.1634 0.094 Uiso 1 1 calc R . . H87B H 0.0429 0.7357 0.1646 0.094 Uiso 1 1 calc R . . H87C H 0.0820 0.7295 0.1916 0.094 Uiso 1 1 calc R . . C88 C 0.28590(13) 0.6811(4) 0.34462(8) 0.0353(9) Uani 1 1 d . . . H88A H 0.2960 0.6812 0.3649 0.042 Uiso 1 1 calc R . . H88B H 0.3053 0.7522 0.3358 0.042 Uiso 1 1 calc R . . C89 C 0.29860(14) 0.5440(4) 0.33250(10) 0.0473(11) Uani 1 1 d . . . H89A H 0.2791 0.4723 0.3410 0.057 Uiso 1 1 calc R . . H89B H 0.2896 0.5438 0.3121 0.057 Uiso 1 1 calc R . . C90 C 0.35383(16) 0.5147(5) 0.33817(12) 0.0660(14) Uani 1 1 d . . . H90A H 0.3731 0.5860 0.3298 0.099 Uiso 1 1 calc R . . H90B H 0.3615 0.4270 0.3300 0.099 Uiso 1 1 calc R . . H90C H 0.3625 0.5121 0.3584 0.099 Uiso 1 1 calc R . . C91 C 0.31580(12) 0.2538(3) 0.25822(7) 0.0270(8) Uani 1 1 d . . . C92 C 0.32496(13) 0.3788(4) 0.24666(7) 0.0316(9) Uani 1 1 d . . . H92 H 0.3465 0.4411 0.2567 0.038 Uiso 1 1 calc R . . C93 C 0.30281(13) 0.4138(4) 0.22036(7) 0.0306(8) Uani 1 1 d . . . H93 H 0.3089 0.5003 0.2127 0.037 Uiso 1 1 calc R . . C94 C 0.27207(12) 0.3225(3) 0.20555(7) 0.0248(8) Uani 1 1 d . . . C95 C 0.26201(12) 0.1980(3) 0.21716(7) 0.0280(8) Uani 1 1 d . . . H95 H 0.2403 0.1360 0.2071 0.034 Uiso 1 1 calc R . . C96 C 0.28361(12) 0.1641(3) 0.24336(7) 0.0287(8) Uani 1 1 d . . . H96 H 0.2765 0.0789 0.2513 0.034 Uiso 1 1 calc R . . C97 C 0.27696(13) 0.3650(4) 0.15561(7) 0.0310(8) Uani 1 1 d . . . C98 C 0.33040(13) 0.3229(4) 0.15999(7) 0.0293(8) Uani 1 1 d . . . C99 C 0.36768(14) 0.4194(4) 0.15953(8) 0.0361(9) Uani 1 1 d . . . H99 H 0.3589 0.5117 0.1566 0.043 Uiso 1 1 calc R . . C100 C 0.41756(14) 0.3837(4) 0.16328(8) 0.0354(9) Uani 1 1 d . . . H100 H 0.4426 0.4514 0.1632 0.042 Uiso 1 1 calc R . . C101 C 0.43066(13) 0.2499(4) 0.16721(7) 0.0282(8) Uani 1 1 d . . . C102 C 0.39377(13) 0.1513(4) 0.16668(8) 0.0346(9) Uani 1 1 d . . . H102 H 0.4027 0.0585 0.1685 0.042 Uiso 1 1 calc R . . C103 C 0.34417(13) 0.1878(4) 0.16354(8) 0.0354(9) Uani 1 1 d . . . H103 H 0.3192 0.1200 0.1638 0.042 Uiso 1 1 calc R . . C104 C 0.50510(13) 0.1784(4) 0.19661(7) 0.0313(8) Uani 1 1 d . . . C105 C 0.47396(12) 0.1877(4) 0.22119(7) 0.0285(8) Uani 1 1 d . . . C106 C 0.47468(13) 0.3044(4) 0.23753(7) 0.0331(9) Uani 1 1 d . . . H106 H 0.4942 0.3796 0.2327 0.040 Uiso 1 1 calc R . . C107 C 0.44743(13) 0.3124(4) 0.26057(7) 0.0309(8) Uani 1 1 d . . . H107 H 0.4487 0.3918 0.2718 0.037 Uiso 1 1 calc R . . C108 C 0.41830(12) 0.2038(3) 0.26717(7) 0.0263(8) Uani 1 1 d . . . C109 C 0.41782(13) 0.0858(4) 0.25144(7) 0.0306(8) Uani 1 1 d . . . H109 H 0.3984 0.0106 0.2563 0.037 Uiso 1 1 calc R . . C110 C 0.44582(13) 0.0784(4) 0.22862(7) 0.0328(9) Uani 1 1 d . . . H110 H 0.4457 -0.0026 0.2179 0.039 Uiso 1 1 calc R . . C111 C 0.33758(13) 0.2166(4) 0.28714(7) 0.0300(8) Uani 1 1 d . . . C112 C 0.19615(12) 0.3927(4) 0.17565(8) 0.0319(8) Uani 1 1 d . . . H11A H 0.1777 0.3256 0.1861 0.038 Uiso 1 1 calc R . . H11B H 0.1832 0.3881 0.1558 0.038 Uiso 1 1 calc R . . C113 C 0.18657(14) 0.5335(4) 0.18684(8) 0.0355(9) Uani 1 1 d . . . H11C H 0.2029 0.5415 0.2060 0.043 Uiso 1 1 calc R . . H11D H 0.1503 0.5457 0.1879 0.043 Uiso 1 1 calc R . . C114 C 0.20585(15) 0.6457(4) 0.16878(9) 0.0474(11) Uani 1 1 d . . . H11E H 0.2415 0.6326 0.1671 0.071 Uiso 1 1 calc R . . H11F H 0.2004 0.7337 0.1775 0.071 Uiso 1 1 calc R . . H11G H 0.1880 0.6429 0.1502 0.071 Uiso 1 1 calc R . . C115 C 0.51066(14) 0.2074(4) 0.14635(8) 0.0385(9) Uani 1 1 d D . . H11H H 0.5456 0.2361 0.1510 0.046 Uiso 1 1 calc R A 1 H11I H 0.4954 0.2680 0.1316 0.046 Uiso 1 1 calc R A 1 C118 C 0.41369(13) 0.1824(4) 0.31862(7) 0.0314(8) Uani 1 1 d . . . H11O H 0.3909 0.2044 0.3331 0.038 Uiso 1 1 calc R . . H11P H 0.4431 0.2423 0.3216 0.038 Uiso 1 1 calc R . . C119 C 0.43054(13) 0.0360(4) 0.32230(8) 0.0330(9) Uani 1 1 d . . . H11Q H 0.4515 0.0271 0.3401 0.040 Uiso 1 1 calc R . . H11R H 0.4512 0.0113 0.3069 0.040 Uiso 1 1 calc R . . C120 C 0.38666(15) -0.0618(4) 0.32237(9) 0.0474(11) Uani 1 1 d . . . H12A H 0.3678 -0.0429 0.3385 0.071 Uiso 1 1 calc R . . H12B H 0.3991 -0.1550 0.3235 0.071 Uiso 1 1 calc R . . H12C H 0.3649 -0.0502 0.3051 0.071 Uiso 1 1 calc R . . C121 C 0.09454(14) 0.6806(4) 0.48303(8) 0.0369(9) Uani 1 1 d . . . C122 C 0.07449(16) 0.7189(4) 0.45624(8) 0.0424(10) Uani 1 1 d . . . H122 H 0.0415 0.7534 0.4537 0.051 Uiso 1 1 calc R . . C123 C 0.10277(18) 0.7065(4) 0.43360(9) 0.0515(12) Uani 1 1 d . . . H123 H 0.0887 0.7320 0.4156 0.062 Uiso 1 1 calc R . . C124 C 0.15067(18) 0.6579(4) 0.43663(9) 0.0511(12) Uani 1 1 d . . . H124 H 0.1697 0.6497 0.4209 0.061 Uiso 1 1 calc R . . C125 C 0.17057(16) 0.6212(4) 0.46301(9) 0.0436(10) Uani 1 1 d . . . H125 H 0.2037 0.5874 0.4654 0.052 Uiso 1 1 calc R . . C126 C 0.14300(14) 0.6330(4) 0.48591(8) 0.0366(9) Uani 1 1 d . . . H126 H 0.1575 0.6081 0.5039 0.044 Uiso 1 1 calc R . . C127 C 0.06360(18) 0.6869(5) 0.50746(10) 0.0600(13) Uani 1 1 d . . . H12D H 0.0789 0.6306 0.5227 0.090 Uiso 1 1 calc R . . H12E H 0.0300 0.6533 0.5019 0.090 Uiso 1 1 calc R . . H12F H 0.0616 0.7808 0.5139 0.090 Uiso 1 1 calc R . . C128 C 0.14838(15) 0.2997(4) 0.30701(8) 0.0369(9) Uani 1 1 d . . . C129 C 0.09930(15) 0.3416(4) 0.30145(9) 0.0416(10) Uani 1 1 d . . . H129 H 0.0773 0.3401 0.3160 0.050 Uiso 1 1 calc R . . C130 C 0.08207(15) 0.3855(4) 0.27506(8) 0.0416(10) Uani 1 1 d . . . H130 H 0.0484 0.4139 0.2716 0.050 Uiso 1 1 calc R . . C131 C 0.11304(16) 0.3885(4) 0.25378(8) 0.0433(10) Uani 1 1 d . . . H131 H 0.1011 0.4188 0.2357 0.052 Uiso 1 1 calc R . . C132 C 0.16153(15) 0.3474(4) 0.25898(8) 0.0404(10) Uani 1 1 d . . . H132 H 0.1831 0.3486 0.2443 0.048 Uiso 1 1 calc R . . C133 C 0.17932(14) 0.3043(3) 0.28525(8) 0.0344(9) Uani 1 1 d . . . H133 H 0.2132 0.2774 0.2885 0.041 Uiso 1 1 calc R . . C134 C 0.1672(2) 0.2491(5) 0.33551(9) 0.0703(15) Uani 1 1 d . . . H13A H 0.1392 0.2409 0.3473 0.105 Uiso 1 1 calc R . . H13B H 0.1917 0.3130 0.3441 0.105 Uiso 1 1 calc R . . H13C H 0.1829 0.1603 0.3337 0.105 Uiso 1 1 calc R . . C135 C 0.40278(15) 0.3039(4) 0.03126(10) 0.0504(12) Uani 1 1 d . . . C136 C 0.35554(14) 0.3572(4) 0.02742(9) 0.0382(9) Uani 1 1 d . . . H136 H 0.3434 0.3879 0.0094 0.046 Uiso 1 1 calc R . . C137 C 0.32569(18) 0.3668(4) 0.04909(10) 0.0561(12) Uani 1 1 d . . . H137 H 0.2935 0.4054 0.0456 0.067 Uiso 1 1 calc R . . C138 C 0.3401(3) 0.3240(5) 0.07490(11) 0.0799(18) Uani 1 1 d . . . H138 H 0.3183 0.3311 0.0894 0.096 Uiso 1 1 calc R . . C139 C 0.3859(3) 0.2708(6) 0.08005(12) 0.095(2) Uani 1 1 d . . . H139 H 0.3963 0.2414 0.0985 0.114 Uiso 1 1 calc R . . C140 C 0.4188(2) 0.2574(4) 0.05894(14) 0.083(2) Uani 1 1 d . . . H140 H 0.4508 0.2185 0.0629 0.100 Uiso 1 1 calc R . . C141 C 0.4360(2) 0.2976(6) 0.00777(15) 0.096(2) Uani 1 1 d . . . H14A H 0.4380 0.2040 0.0012 0.144 Uiso 1 1 calc R . . H14B H 0.4694 0.3293 0.0144 0.144 Uiso 1 1 calc R . . H14C H 0.4224 0.3554 -0.0076 0.144 Uiso 1 1 calc R . . C142 C 0.65398(15) 0.2595(4) 0.26913(9) 0.0463(11) Uani 1 1 d . . . C143 C 0.60562(15) 0.2123(4) 0.26806(9) 0.0425(10) Uani 1 1 d . . . H143 H 0.5899 0.1806 0.2508 0.051 Uiso 1 1 calc R . . C144 C 0.57977(18) 0.2108(4) 0.29191(11) 0.0596(13) Uani 1 1 d . . . H144 H 0.5465 0.1784 0.2908 0.072 Uiso 1 1 calc R . . C145 C 0.6020(2) 0.2559(5) 0.31717(10) 0.0754(17) Uani 1 1 d . . . H145 H 0.5846 0.2544 0.3336 0.090 Uiso 1 1 calc R . . C146 C 0.6503(2) 0.3033(5) 0.31776(12) 0.0799(18) Uani 1 1 d . . . H146 H 0.6663 0.3347 0.3349 0.096 Uiso 1 1 calc R . . C147 C 0.67555(19) 0.3062(4) 0.29426(11) 0.0627(14) Uani 1 1 d . . . H147 H 0.7085 0.3409 0.2953 0.075 Uiso 1 1 calc R . . C148 C 0.6824(2) 0.2582(5) 0.24344(12) 0.0777(16) Uani 1 1 d . . . H14D H 0.6934 0.3503 0.2395 0.117 Uiso 1 1 calc R . . H14E H 0.6607 0.2245 0.2275 0.117 Uiso 1 1 calc R . . H14F H 0.7115 0.1989 0.2466 0.117 Uiso 1 1 calc R . . C116 C 0.5088(3) 0.0549(9) 0.13595(17) 0.0359(18) Uiso 0.50 1 d PD B 1 H11J H 0.5247 -0.0044 0.1507 0.043 Uiso 0.50 1 calc PR B 1 H11K H 0.4736 0.0261 0.1323 0.043 Uiso 0.50 1 calc PR B 1 C16A C 0.5000(3) 0.1064(9) 0.12457(19) 0.050(2) Uiso 0.50 1 d PD B 2 H16A H 0.5215 0.1208 0.1090 0.060 Uiso 0.50 1 calc PR B 2 H16B H 0.4647 0.1118 0.1171 0.060 Uiso 0.50 1 calc PR B 2 C117 C 0.5354(3) 0.0401(9) 0.10957(16) 0.046(2) Uiso 0.50 1 d PD B 1 H11L H 0.5169 0.0890 0.0943 0.068 Uiso 0.50 1 calc PR B 1 H11M H 0.5374 -0.0560 0.1047 0.068 Uiso 0.50 1 calc PR B 1 H11N H 0.5690 0.0776 0.1127 0.068 Uiso 0.50 1 calc PR B 1 C17A C 0.5108(3) -0.0285(10) 0.13810(18) 0.051(2) Uiso 0.50 1 d PD B 2 H17A H 0.5450 -0.0296 0.1467 0.076 Uiso 0.50 1 calc PR B 2 H17B H 0.5066 -0.1000 0.1239 0.076 Uiso 0.50 1 calc PR B 2 H17C H 0.4876 -0.0441 0.1525 0.076 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 O1 0.0354(16) 0.074(2) 0.0347(15) 0.0021(14) 0.0042(12) -0.0137(15) N1 0.0309(17) 0.0379(18) 0.0264(17) -0.0004(14) 0.0011(13) 0.0033(14) C1 0.043(2) 0.033(2) 0.028(2) -0.0014(17) -0.0106(17) -0.0017(18) O2 0.0408(16) 0.0540(18) 0.0465(17) -0.0108(14) 0.0159(14) -0.0058(13) N2 0.0344(18) 0.0282(17) 0.0291(17) -0.0008(13) 0.0057(14) -0.0054(13) C2 0.058(3) 0.027(2) 0.035(2) -0.0037(17) -0.0124(19) 0.0027(19) O3 0.060(2) 0.076(2) 0.0399(17) -0.0106(16) -0.0134(15) -0.0272(17) N3 0.0346(18) 0.0302(18) 0.0421(19) -0.0001(15) -0.0126(15) -0.0032(14) C3 0.045(2) 0.034(2) 0.036(2) -0.0026(18) -0.0057(18) 0.0059(19) O4 0.0349(14) 0.0434(16) 0.0281(14) 0.0045(12) 0.0087(12) 0.0047(12) N4 0.0306(17) 0.0234(16) 0.0200(15) -0.0025(12) 0.0031(12) 0.0035(12) C4 0.036(2) 0.033(2) 0.0221(19) 0.0000(16) -0.0029(16) 0.0059(17) O5 0.0341(15) 0.0518(17) 0.0283(14) 0.0114(12) -0.0038(11) 0.0039(12) N5 0.0240(15) 0.0277(16) 0.0233(16) 0.0007(12) -0.0038(13) 0.0033(12) C5 0.035(2) 0.028(2) 0.038(2) -0.0032(17) -0.0053(17) -0.0001(17) O6 0.0236(14) 0.0510(17) 0.0338(14) 0.0005(12) 0.0008(11) 0.0048(12) N6 0.0239(15) 0.0281(16) 0.0246(16) 0.0009(13) 0.0037(12) 0.0071(13) C6 0.036(2) 0.039(2) 0.037(2) -0.0049(18) -0.0034(18) 0.0056(18) O7 0.0325(15) 0.0594(18) 0.0357(15) -0.0015(13) 0.0007(12) 0.0130(13) N7 0.0243(16) 0.0309(17) 0.0252(16) -0.0012(13) 0.0044(12) -0.0040(13) C7 0.028(2) 0.033(2) 0.032(2) 0.0011(17) -0.0025(17) 0.0031(17) O8 0.0412(16) 0.0583(19) 0.0360(15) 0.0111(13) 0.0112(13) -0.0062(14) N8 0.0341(18) 0.0306(17) 0.0251(16) 0.0080(13) 0.0058(13) 0.0027(13) C8 0.0260(19) 0.032(2) 0.0248(19) -0.0003(16) -0.0031(15) -0.0002(16) O9 0.0392(16) 0.071(2) 0.0324(15) 0.0165(14) -0.0008(12) 0.0112(14) N9 0.0270(16) 0.0347(18) 0.0293(17) -0.0001(13) -0.0015(13) 0.0004(13) C9 0.032(2) 0.032(2) 0.029(2) -0.0002(16) 0.0000(16) 0.0072(16) O10 0.0430(16) 0.0662(19) 0.0296(15) 0.0118(13) -0.0036(12) 0.0152(14) N10 0.0252(16) 0.0266(16) 0.0259(16) 0.0024(12) -0.0018(12) 0.0020(12) C10 0.034(2) 0.027(2) 0.034(2) 0.0053(16) -0.0018(17) -0.0001(16) O11 0.0256(14) 0.075(2) 0.0408(16) 0.0046(14) 0.0018(12) 0.0087(13) N11 0.0261(16) 0.0328(17) 0.0298(16) -0.0042(13) 0.0011(13) -0.0001(13) C11 0.0271(19) 0.026(2) 0.0253(19) -0.0015(15) -0.0009(15) -0.0053(15) O12 0.0355(15) 0.0585(18) 0.0284(14) 0.0089(13) 0.0053(11) 0.0102(13) N12 0.0294(16) 0.0302(17) 0.0221(15) 0.0015(13) -0.0014(12) 0.0012(13) C12 0.0271(19) 0.024(2) 0.035(2) -0.0024(16) 0.0031(16) 0.0030(15) C13 0.030(2) 0.028(2) 0.030(2) 0.0053(16) -0.0003(16) -0.0021(16) C14 0.039(2) 0.026(2) 0.038(2) -0.0021(17) 0.0089(18) -0.0023(17) C15 0.027(2) 0.029(2) 0.041(2) -0.0020(17) 0.0089(17) -0.0018(16) C16 0.033(2) 0.027(2) 0.045(2) -0.0046(18) 0.0092(18) 0.0017(17) C17 0.027(2) 0.029(2) 0.047(2) 0.0045(18) 0.0011(17) 0.0037(16) C18 0.029(2) 0.028(2) 0.040(2) 0.0016(17) -0.0036(17) -0.0026(16) C19 0.038(2) 0.024(2) 0.045(2) -0.0072(17) -0.0074(18) 0.0008(17) C20 0.035(2) 0.025(2) 0.042(2) 0.0017(17) -0.0059(18) 0.0038(16) C21 0.046(2) 0.033(2) 0.037(2) 0.0002(18) -0.013(2) -0.0073(18) C22 0.042(2) 0.039(2) 0.029(2) 0.0021(17) 0.0058(17) 0.0075(18) C23 0.066(3) 0.048(3) 0.034(2) 0.008(2) 0.007(2) 0.016(2) C24 0.089(4) 0.045(3) 0.039(3) 0.011(2) 0.011(2) 0.005(2) C25 0.044(2) 0.035(2) 0.026(2) 0.0064(16) 0.0017(17) -0.0030(18) C26 0.055(3) 0.047(3) 0.029(2) -0.0017(18) -0.0054(19) -0.013(2) C27 0.081(3) 0.043(3) 0.050(3) -0.012(2) -0.004(2) -0.005(2) C28 0.045(3) 0.050(3) 0.058(3) 0.007(2) -0.016(2) -0.019(2) C29 0.042(3) 0.086(4) 0.070(3) 0.024(3) -0.003(2) -0.002(3) C30 0.076(4) 0.066(4) 0.101(4) 0.014(3) -0.003(3) -0.020(3) C31 0.0229(18) 0.027(2) 0.0227(18) 0.0049(15) -0.0037(14) 0.0020(15) C32 0.033(2) 0.0225(19) 0.0267(19) -0.0017(15) 0.0019(16) 0.0008(16) C33 0.0282(19) 0.0230(19) 0.0257(19) 0.0042(15) 0.0048(15) -0.0038(15) C34 0.0264(19) 0.0243(19) 0.0178(17) 0.0012(14) -0.0004(14) 0.0076(15) C35 0.0277(19) 0.0215(19) 0.0279(19) -0.0038(15) -0.0027(16) 0.0003(15) C36 0.0213(18) 0.027(2) 0.0282(19) 0.0018(15) -0.0010(15) -0.0047(15) C37 0.031(2) 0.0213(19) 0.0255(19) -0.0003(15) 0.0069(16) 0.0003(15) C38 0.0235(18) 0.0223(19) 0.0252(19) 0.0003(15) 0.0044(15) 0.0051(15) C39 0.0278(19) 0.0200(19) 0.035(2) 0.0049(16) 0.0071(16) -0.0012(15) C40 0.0228(18) 0.0217(19) 0.030(2) -0.0009(15) 0.0016(15) 0.0013(14) C41 0.0219(18) 0.0260(19) 0.0233(18) -0.0007(15) 0.0007(14) 0.0028(15) C42 0.0295(19) 0.0198(18) 0.028(2) 0.0048(15) -0.0025(15) -0.0031(15) C43 0.0279(19) 0.0233(19) 0.0275(19) -0.0027(15) 0.0003(15) -0.0032(15) C44 0.0286(19) 0.0206(19) 0.026(2) 0.0028(15) -0.0040(16) -0.0034(15) C45 0.0250(19) 0.033(2) 0.0178(18) -0.0002(15) 0.0024(14) 0.0007(16) C46 0.028(2) 0.0240(19) 0.031(2) 0.0000(15) -0.0005(16) 0.0006(16) C47 0.027(2) 0.028(2) 0.034(2) -0.0051(16) -0.0002(16) -0.0052(16) C48 0.029(2) 0.032(2) 0.0171(17) 0.0010(15) 0.0038(15) 0.0042(16) C49 0.031(2) 0.0233(19) 0.034(2) 0.0010(16) -0.0004(16) -0.0001(16) C50 0.027(2) 0.026(2) 0.032(2) -0.0004(16) 0.0004(16) -0.0047(16) C51 0.027(2) 0.0253(19) 0.025(2) 0.0027(15) 0.0004(16) 0.0004(15) C52 0.036(2) 0.038(2) 0.0226(19) -0.0049(16) -0.0025(16) -0.0028(17) C53 0.035(2) 0.053(3) 0.024(2) 0.0043(18) -0.0027(16) 0.0128(19) C54 0.062(3) 0.039(2) 0.046(3) 0.015(2) -0.001(2) 0.007(2) C55 0.0249(19) 0.030(2) 0.031(2) 0.0028(16) -0.0050(15) 0.0008(15) C56 0.026(2) 0.028(2) 0.044(2) 0.0058(17) 0.0043(17) 0.0009(16) C57 0.032(2) 0.038(2) 0.069(3) 0.007(2) 0.003(2) 0.0078(18) C58 0.034(2) 0.033(2) 0.032(2) -0.0062(17) 0.0046(16) 0.0072(17) C59 0.032(2) 0.047(2) 0.028(2) -0.0080(18) -0.0005(16) 0.0059(18) C60 0.054(3) 0.053(3) 0.031(2) 0.0012(19) 0.0110(19) 0.003(2) C61 0.0269(19) 0.035(2) 0.0209(18) -0.0001(15) 0.0007(15) 0.0000(16) C62 0.030(2) 0.030(2) 0.0244(19) -0.0038(15) 0.0017(15) -0.0070(16) C63 0.029(2) 0.027(2) 0.0248(19) -0.0035(15) 0.0021(15) 0.0014(16) C64 0.0260(19) 0.027(2) 0.0163(17) -0.0013(14) 0.0009(14) -0.0015(15) C65 0.031(2) 0.028(2) 0.0265(19) -0.0003(15) 0.0016(16) -0.0061(16) C66 0.037(2) 0.030(2) 0.0253(19) 0.0044(16) -0.0007(16) 0.0034(17) C67 0.026(2) 0.036(2) 0.028(2) -0.0067(17) -0.0017(16) 0.0004(17) C68 0.0287(19) 0.030(2) 0.0211(18) -0.0018(15) -0.0007(15) 0.0006(16) C69 0.037(2) 0.029(2) 0.035(2) -0.0050(17) 0.0044(17) 0.0045(17) C70 0.045(2) 0.025(2) 0.033(2) 0.0000(17) 0.0049(18) 0.0000(17) C71 0.031(2) 0.031(2) 0.0241(19) 0.0016(16) 0.0027(16) 0.0037(16) C72 0.037(2) 0.027(2) 0.0245(19) -0.0030(15) 0.0044(16) 0.0055(16) C73 0.033(2) 0.026(2) 0.029(2) 0.0005(16) 0.0031(16) 0.0001(16) C74 0.038(2) 0.0230(19) 0.0250(19) -0.0017(15) 0.0088(17) -0.0090(16) C75 0.0253(19) 0.0251(19) 0.0285(19) -0.0029(15) 0.0079(15) -0.0033(15) C76 0.037(2) 0.0203(19) 0.030(2) -0.0027(16) 0.0074(16) -0.0035(16) C77 0.030(2) 0.0226(19) 0.030(2) -0.0088(16) 0.0055(16) -0.0060(15) C78 0.0245(19) 0.027(2) 0.0278(19) -0.0015(15) 0.0054(15) 0.0009(15) C79 0.040(2) 0.0193(19) 0.036(2) -0.0033(16) 0.0025(17) -0.0039(16) C80 0.038(2) 0.0228(19) 0.027(2) -0.0062(15) -0.0023(16) -0.0060(16) C81 0.037(2) 0.037(2) 0.025(2) -0.0007(16) 0.0013(16) 0.0007(17) C82 0.034(2) 0.033(2) 0.036(2) -0.0025(17) 0.0136(17) -0.0062(17) C83 0.046(2) 0.048(3) 0.035(2) -0.0020(19) 0.0131(19) 0.003(2) C84 0.064(3) 0.042(3) 0.048(3) -0.013(2) 0.013(2) -0.005(2) C85 0.050(2) 0.039(2) 0.032(2) 0.0139(18) 0.0081(18) 0.0104(19) C86 0.043(2) 0.069(3) 0.036(2) 0.017(2) -0.0009(19) 0.015(2) C87 0.077(3) 0.067(3) 0.039(3) -0.005(2) -0.018(2) 0.005(3) C88 0.026(2) 0.036(2) 0.043(2) 0.0022(18) -0.0020(17) -0.0003(16) C89 0.030(2) 0.033(2) 0.079(3) 0.001(2) 0.004(2) 0.0038(18) C90 0.039(3) 0.044(3) 0.115(4) -0.001(3) 0.004(3) 0.006(2) C91 0.0267(19) 0.029(2) 0.0255(19) 0.0026(16) 0.0035(15) 0.0084(16) C92 0.032(2) 0.029(2) 0.033(2) -0.0005(16) -0.0035(16) -0.0026(16) C93 0.034(2) 0.0243(19) 0.033(2) 0.0056(16) -0.0020(17) 0.0012(16) C94 0.0243(18) 0.0226(19) 0.0270(19) -0.0011(15) -0.0014(15) 0.0026(15) C95 0.029(2) 0.025(2) 0.030(2) 0.0020(16) -0.0019(16) -0.0056(15) C96 0.0279(19) 0.0234(19) 0.034(2) 0.0058(16) 0.0012(16) -0.0014(15) C97 0.033(2) 0.030(2) 0.029(2) -0.0005(16) -0.0067(16) 0.0038(16) C98 0.034(2) 0.031(2) 0.0230(19) 0.0004(15) 0.0001(15) 0.0021(17) C99 0.039(2) 0.027(2) 0.041(2) 0.0021(17) -0.0054(18) 0.0011(18) C100 0.037(2) 0.025(2) 0.044(2) -0.0014(17) 0.0011(18) -0.0077(17) C101 0.0279(19) 0.032(2) 0.0241(19) -0.0023(16) -0.0002(15) 0.0020(16) C102 0.033(2) 0.029(2) 0.041(2) 0.0011(17) -0.0021(17) -0.0014(17) C103 0.027(2) 0.030(2) 0.048(2) 0.0046(18) -0.0026(17) -0.0020(16) C104 0.029(2) 0.030(2) 0.035(2) -0.0037(16) -0.0004(16) -0.0038(16) C105 0.0256(19) 0.030(2) 0.029(2) 0.0010(16) 0.0000(15) 0.0046(16) C106 0.033(2) 0.030(2) 0.036(2) -0.0023(17) 0.0026(17) -0.0081(16) C107 0.031(2) 0.027(2) 0.034(2) -0.0038(16) -0.0015(17) -0.0021(16) C108 0.0259(19) 0.026(2) 0.0261(19) 0.0014(15) -0.0024(15) 0.0045(15) C109 0.033(2) 0.025(2) 0.033(2) -0.0004(16) 0.0010(17) -0.0015(16) C110 0.037(2) 0.028(2) 0.034(2) -0.0047(16) 0.0014(17) -0.0024(17) C111 0.033(2) 0.028(2) 0.029(2) 0.0005(16) 0.0027(16) 0.0030(16) C112 0.0256(19) 0.032(2) 0.037(2) 0.0045(17) -0.0038(16) 0.0016(16) C113 0.029(2) 0.033(2) 0.044(2) 0.0037(18) -0.0006(17) 0.0054(16) C114 0.046(3) 0.029(2) 0.067(3) 0.005(2) 0.008(2) 0.0017(19) C115 0.030(2) 0.055(3) 0.031(2) -0.0115(19) 0.0013(17) -0.0006(18) C118 0.033(2) 0.034(2) 0.0256(19) 0.0017(16) -0.0069(16) -0.0022(16) C119 0.032(2) 0.039(2) 0.028(2) 0.0021(17) -0.0041(16) 0.0073(17) C120 0.048(3) 0.038(2) 0.055(3) 0.009(2) -0.007(2) 0.005(2) C121 0.044(2) 0.024(2) 0.043(2) -0.0025(17) 0.0043(19) -0.0061(17) C122 0.052(3) 0.025(2) 0.048(3) 0.0018(18) -0.011(2) -0.0020(18) C123 0.079(3) 0.034(2) 0.040(3) 0.0043(19) -0.007(2) -0.016(2) C124 0.080(3) 0.034(2) 0.042(3) -0.010(2) 0.021(2) -0.019(2) C125 0.047(2) 0.030(2) 0.055(3) -0.0055(19) 0.013(2) -0.0086(18) C126 0.041(2) 0.027(2) 0.041(2) -0.0002(17) -0.0045(19) -0.0041(17) C127 0.061(3) 0.056(3) 0.066(3) -0.005(2) 0.025(2) 0.004(2) C128 0.057(3) 0.021(2) 0.033(2) -0.0013(16) 0.0023(19) 0.0026(18) C129 0.045(2) 0.032(2) 0.050(3) -0.0103(19) 0.014(2) -0.0046(19) C130 0.039(2) 0.031(2) 0.053(3) -0.0083(19) -0.008(2) -0.0015(18) C131 0.066(3) 0.029(2) 0.033(2) -0.0006(17) -0.009(2) -0.006(2) C132 0.057(3) 0.026(2) 0.040(2) -0.0044(18) 0.017(2) -0.0058(19) C133 0.041(2) 0.021(2) 0.041(2) -0.0041(17) 0.0062(19) 0.0027(16) C134 0.111(4) 0.064(3) 0.035(3) 0.006(2) 0.000(3) 0.028(3) C135 0.041(3) 0.027(2) 0.082(3) -0.013(2) -0.004(2) -0.0049(19) C136 0.038(2) 0.027(2) 0.048(2) -0.0020(18) -0.0085(19) -0.0045(17) C137 0.065(3) 0.044(3) 0.059(3) -0.017(2) 0.005(3) -0.016(2) C138 0.129(5) 0.053(3) 0.058(3) -0.015(3) 0.010(3) -0.040(3) C139 0.170(7) 0.052(4) 0.056(4) 0.005(3) -0.035(4) -0.045(4) C140 0.077(4) 0.024(2) 0.138(5) 0.000(3) -0.063(4) -0.002(2) C141 0.066(4) 0.059(4) 0.168(6) -0.041(4) 0.044(4) -0.012(3) C142 0.045(3) 0.032(2) 0.061(3) 0.010(2) -0.003(2) 0.0064(19) C143 0.044(2) 0.030(2) 0.052(3) 0.0066(19) -0.006(2) 0.0044(18) C144 0.055(3) 0.043(3) 0.082(4) 0.020(3) 0.014(3) 0.017(2) C145 0.133(5) 0.047(3) 0.048(3) 0.017(2) 0.019(3) 0.043(3) C146 0.127(5) 0.038(3) 0.067(4) -0.002(3) -0.040(4) 0.021(3) C147 0.065(3) 0.035(3) 0.083(4) 0.006(3) -0.028(3) 0.003(2) C148 0.075(4) 0.057(3) 0.105(4) 0.027(3) 0.034(3) 0.009(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 O1 C7 1.225(4) . ? N1 C7 1.359(4) . ? N1 C4 1.442(5) . ? N1 C22 1.475(5) . ? C1 C6 1.389(5) . ? C1 C2 1.390(5) . ? C1 C21 1.506(5) . ? O2 C14 1.229(4) . ? N2 C14 1.373(5) . ? N2 C11 1.440(4) . ? N2 C25 1.471(4) . ? C2 C3 1.380(5) . ? O3 C21 1.222(4) . ? N3 C21 1.351(5) . ? N3 C18 1.451(5) . ? N3 C28 1.466(5) . ? C3 C4 1.381(5) . ? O4 C37 1.227(4) . ? N4 C37 1.365(4) . ? N4 C34 1.441(4) . ? N4 C52 1.475(4) . ? C4 C5 1.390(5) . ? O5 C44 1.233(4) . ? N5 C44 1.347(4) . ? N5 C41 1.451(4) . ? N5 C55 1.471(4) . ? C5 C6 1.380(5) . ? O6 C51 1.231(4) . ? N6 C51 1.364(4) . ? N6 C48 1.439(4) . ? N6 C58 1.479(4) . ? O7 C67 1.236(4) . ? N7 C67 1.365(4) . ? N7 C64 1.438(4) . ? N7 C82 1.481(4) . ? C7 C8 1.502(5) . ? O8 C74 1.226(4) . ? N8 C74 1.358(4) . ? N8 C71 1.443(4) . ? N8 C85 1.481(4) . ? C8 C9 1.384(5) . ? C8 C13 1.389(5) . ? O9 C81 1.231(4) . ? N9 C81 1.365(5) . ? N9 C78 1.448(4) . ? N9 C88 1.461(4) . ? C9 C10 1.391(5) . ? O10 C97 1.231(4) . ? N10 C97 1.353(4) . ? N10 C94 1.448(4) . ? N10 C112 1.480(4) . ? C10 C11 1.391(5) . ? O11 C104 1.227(4) . ? N11 C104 1.359(4) . ? N11 C101 1.445(4) . ? N11 C115 1.464(5) . ? C11 C12 1.383(5) . ? O12 C111 1.227(4) . ? N12 C111 1.363(4) . ? N12 C108 1.453(4) . ? N12 C118 1.471(4) . ? C12 C13 1.377(5) . ? C14 C15 1.493(5) . ? C15 C16 1.393(5) . ? C15 C20 1.394(5) . ? C16 C17 1.379(5) . ? C17 C18 1.388(5) . ? C18 C19 1.392(5) . ? C19 C20 1.387(5) . ? C22 C23 1.515(5) . ? C23 C24 1.520(6) . ? C25 C26 1.527(5) . ? C26 C27 1.505(6) . ? C28 C29 1.596(7) . ? C29 C30 1.468(7) . ? C31 C32 1.385(5) . ? C31 C36 1.395(5) . ? C31 C51 1.503(5) . ? C32 C33 1.380(5) . ? C33 C34 1.390(5) . ? C34 C35 1.390(5) . ? C35 C36 1.386(5) . ? C37 C38 1.501(5) . ? C38 C43 1.389(5) . ? C38 C39 1.394(5) . ? C39 C40 1.385(5) . ? C40 C41 1.389(5) . ? C41 C42 1.388(5) . ? C42 C43 1.391(5) . ? C44 C45 1.503(5) . ? C45 C46 1.392(5) . ? C45 C50 1.395(5) . ? C46 C47 1.390(5) . ? C47 C48 1.382(5) . ? C48 C49 1.385(5) . ? C49 C50 1.385(5) . ? C52 C53 1.518(5) . ? C53 C54 1.511(6) . ? C55 C56 1.515(5) . ? C56 C57 1.535(5) . ? C58 C59 1.511(5) . ? C59 C60 1.505(6) . ? C61 C66 1.385(5) . ? C61 C62 1.402(5) . ? C61 C81 1.497(5) . ? C62 C63 1.390(5) . ? C63 C64 1.397(5) . ? C64 C65 1.375(5) . ? C65 C66 1.388(5) . ? C67 C68 1.503(5) . ? C68 C69 1.384(5) . ? C68 C73 1.398(5) . ? C69 C70 1.386(5) . ? C70 C71 1.382(5) . ? C71 C72 1.387(5) . ? C72 C73 1.380(5) . ? C74 C75 1.498(5) . ? C75 C80 1.384(5) . ? C75 C76 1.389(5) . ? C76 C77 1.378(5) . ? C77 C78 1.383(5) . ? C78 C79 1.389(5) . ? C79 C80 1.389(5) . ? C82 C83 1.522(5) . ? C83 C84 1.489(6) . ? C85 C86 1.501(6) . ? C86 C87 1.501(6) . ? C88 C89 1.523(5) . ? C89 C90 1.518(5) . ? C91 C92 1.384(5) . ? C91 C96 1.394(5) . ? C91 C111 1.508(5) . ? C92 C93 1.395(5) . ? C93 C94 1.381(5) . ? C94 C95 1.386(5) . ? C95 C96 1.382(5) . ? C97 C98 1.496(5) . ? C98 C99 1.385(5) . ? C98 C103 1.392(5) . ? C99 C100 1.386(5) . ? C100 C101 1.377(5) . ? C101 C102 1.390(5) . ? C102 C103 1.380(5) . ? C104 C105 1.505(5) . ? C105 C110 1.383(5) . ? C105 C106 1.394(5) . ? C106 C107 1.379(5) . ? C107 C108 1.381(5) . ? C108 C109 1.388(5) . ? C109 C110 1.382(5) . ? C112 C113 1.520(5) . ? C113 C114 1.524(5) . ? C115 C16A 1.456(9) . ? C115 C116 1.586(9) . ? C118 C119 1.521(5) . ? C119 C120 1.526(5) . ? C121 C126 1.383(5) . ? C121 C122 1.405(5) . ? C121 C127 1.494(6) . ? C122 C123 1.383(6) . ? C123 C124 1.373(6) . ? C124 C125 1.382(6) . ? C125 C126 1.381(5) . ? C128 C133 1.389(5) . ? C128 C129 1.390(5) . ? C128 C134 1.504(6) . ? C129 C130 1.383(6) . ? C130 C131 1.371(6) . ? C131 C132 1.371(6) . ? C132 C133 1.379(5) . ? C135 C136 1.375(5) . ? C135 C140 1.438(7) . ? C135 C141 1.497(7) . ? C136 C137 1.369(6) . ? C137 C138 1.336(7) . ? C138 C139 1.345(9) . ? C139 C140 1.406(9) . ? C142 C147 1.374(6) . ? C142 C143 1.381(6) . ? C142 C148 1.503(6) . ? C143 C144 1.388(6) . ? C144 C145 1.381(7) . ? C145 C146 1.379(8) . ? C146 C147 1.365(8) . ? C116 C117 1.512(10) . ? C16A C17A 1.500(11) . ? 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 C7 N1 C4 122.0(3) . . ? C7 N1 C22 119.3(3) . . ? C4 N1 C22 118.1(3) . . ? C6 C1 C2 119.0(4) . . ? C6 C1 C21 121.8(3) . . ? C2 C1 C21 119.2(3) . . ? C14 N2 C11 119.9(3) . . ? C14 N2 C25 121.1(3) . . ? C11 N2 C25 117.7(3) . . ? C3 C2 C1 120.8(4) . . ? C21 N3 C18 122.7(3) . . ? C21 N3 C28 118.8(3) . . ? C18 N3 C28 116.6(3) . . ? C2 C3 C4 120.0(4) . . ? C37 N4 C34 120.0(3) . . ? C37 N4 C52 121.6(3) . . ? C34 N4 C52 117.4(3) . . ? C3 C4 C5 119.6(3) . . ? C3 C4 N1 120.3(3) . . ? C5 C4 N1 120.1(3) . . ? C44 N5 C41 122.2(3) . . ? C44 N5 C55 120.5(3) . . ? C41 N5 C55 116.7(3) . . ? C6 C5 C4 120.3(3) . . ? C51 N6 C48 120.8(3) . . ? C51 N6 C58 120.7(3) . . ? C48 N6 C58 118.4(3) . . ? C5 C6 C1 120.2(4) . . ? C67 N7 C64 122.1(3) . . ? C67 N7 C82 119.1(3) . . ? C64 N7 C82 117.6(3) . . ? O1 C7 N1 121.8(3) . . ? O1 C7 C8 120.7(3) . . ? N1 C7 C8 117.4(3) . . ? C74 N8 C71 122.8(3) . . ? C74 N8 C85 119.6(3) . . ? C71 N8 C85 117.2(3) . . ? C9 C8 C13 119.0(3) . . ? C9 C8 C7 121.3(3) . . ? C13 C8 C7 119.6(3) . . ? C81 N9 C78 122.0(3) . . ? C81 N9 C88 118.7(3) . . ? C78 N9 C88 117.0(3) . . ? C8 C9 C10 121.0(3) . . ? C97 N10 C94 121.8(3) . . ? C97 N10 C112 120.9(3) . . ? C94 N10 C112 117.1(3) . . ? C9 C10 C11 119.1(3) . . ? C104 N11 C101 122.5(3) . . ? C104 N11 C115 120.1(3) . . ? C101 N11 C115 117.3(3) . . ? C12 C11 C10 120.0(3) . . ? C12 C11 N2 119.8(3) . . ? C10 C11 N2 120.2(3) . . ? C111 N12 C108 120.9(3) . . ? C111 N12 C118 121.0(3) . . ? C108 N12 C118 116.9(3) . . ? C13 C12 C11 120.2(3) . . ? C12 C13 C8 120.6(3) . . ? O2 C14 N2 122.9(3) . . ? O2 C14 C15 121.5(3) . . ? N2 C14 C15 115.6(3) . . ? C16 C15 C20 118.7(3) . . ? C16 C15 C14 120.7(3) . . ? C20 C15 C14 120.5(3) . . ? C17 C16 C15 121.0(3) . . ? C16 C17 C18 119.8(3) . . ? C17 C18 C19 120.3(3) . . ? C17 C18 N3 120.6(3) . . ? C19 C18 N3 119.1(3) . . ? C20 C19 C18 119.4(3) . . ? C19 C20 C15 120.8(3) . . ? O3 C21 N3 122.6(4) . . ? O3 C21 C1 120.7(4) . . ? N3 C21 C1 116.6(3) . . ? N1 C22 C23 112.7(3) . . ? C22 C23 C24 110.8(3) . . ? N2 C25 C26 112.9(3) . . ? C27 C26 C25 113.7(3) . . ? N3 C28 C29 109.5(3) . . ? C30 C29 C28 110.7(4) . . ? C32 C31 C36 119.1(3) . . ? C32 C31 C51 117.5(3) . . ? C36 C31 C51 123.2(3) . . ? C33 C32 C31 120.8(3) . . ? C32 C33 C34 119.8(3) . . ? C35 C34 C33 120.1(3) . . ? C35 C34 N4 121.0(3) . . ? C33 C34 N4 118.9(3) . . ? C36 C35 C34 119.5(3) . . ? C35 C36 C31 120.6(3) . . ? O4 C37 N4 123.4(3) . . ? O4 C37 C38 121.3(3) . . ? N4 C37 C38 115.2(3) . . ? C43 C38 C39 119.4(3) . . ? C43 C38 C37 119.1(3) . . ? C39 C38 C37 121.5(3) . . ? C40 C39 C38 120.7(3) . . ? C39 C40 C41 119.4(3) . . ? C42 C41 C40 120.7(3) . . ? C42 C41 N5 119.4(3) . . ? C40 C41 N5 119.9(3) . . ? C41 C42 C43 119.5(3) . . ? C38 C43 C42 120.4(3) . . ? O5 C44 N5 123.0(3) . . ? O5 C44 C45 121.0(3) . . ? N5 C44 C45 116.0(3) . . ? C46 C45 C50 119.2(3) . . ? C46 C45 C44 120.1(3) . . ? C50 C45 C44 120.7(3) . . ? C47 C46 C45 119.6(3) . . ? C48 C47 C46 120.8(3) . . ? C47 C48 C49 119.9(3) . . ? C47 C48 N6 119.4(3) . . ? C49 C48 N6 120.7(3) . . ? C50 C49 C48 119.6(3) . . ? C49 C50 C45 120.8(3) . . ? O6 C51 N6 123.1(3) . . ? O6 C51 C31 120.6(3) . . ? N6 C51 C31 116.0(3) . . ? N4 C52 C53 112.6(3) . . ? C54 C53 C52 113.5(3) . . ? N5 C55 C56 113.2(3) . . ? C55 C56 C57 111.5(3) . . ? N6 C58 C59 113.2(3) . . ? C60 C59 C58 115.5(3) . . ? C66 C61 C62 118.7(3) . . ? C66 C61 C81 119.8(3) . . ? C62 C61 C81 121.4(3) . . ? C63 C62 C61 120.3(3) . . ? C62 C63 C64 119.7(3) . . ? C65 C64 C63 119.9(3) . . ? C65 C64 N7 120.2(3) . . ? C63 C64 N7 119.9(3) . . ? C64 C65 C66 120.1(3) . . ? C61 C66 C65 121.0(3) . . ? O7 C67 N7 122.0(3) . . ? O7 C67 C68 120.4(3) . . ? N7 C67 C68 117.6(3) . . ? C69 C68 C73 119.0(3) . . ? C69 C68 C67 120.2(3) . . ? C73 C68 C67 120.7(3) . . ? C68 C69 C70 120.3(3) . . ? C71 C70 C69 120.5(3) . . ? C70 C71 C72 119.3(3) . . ? C70 C71 N8 119.6(3) . . ? C72 C71 N8 121.1(3) . . ? C73 C72 C71 120.4(3) . . ? C72 C73 C68 120.3(3) . . ? O8 C74 N8 122.4(3) . . ? O8 C74 C75 120.1(3) . . ? N8 C74 C75 117.4(3) . . ? C80 C75 C76 118.5(3) . . ? C80 C75 C74 122.7(3) . . ? C76 C75 C74 118.7(3) . . ? C77 C76 C75 121.1(3) . . ? C76 C77 C78 119.9(3) . . ? C77 C78 C79 119.8(3) . . ? C77 C78 N9 120.1(3) . . ? C79 C78 N9 120.1(3) . . ? C78 C79 C80 119.5(3) . . ? C75 C80 C79 121.0(3) . . ? O9 C81 N9 121.7(3) . . ? O9 C81 C61 120.9(3) . . ? N9 C81 C61 117.3(3) . . ? N7 C82 C83 112.3(3) . . ? C84 C83 C82 113.7(3) . . ? N8 C85 C86 113.0(3) . . ? C87 C86 C85 114.2(3) . . ? N9 C88 C89 113.2(3) . . ? C90 C89 C88 110.4(3) . . ? C92 C91 C96 119.1(3) . . ? C92 C91 C111 121.2(3) . . ? C96 C91 C111 119.7(3) . . ? C91 C92 C93 120.5(3) . . ? C94 C93 C92 119.8(3) . . ? C93 C94 C95 120.1(3) . . ? C93 C94 N10 120.4(3) . . ? C95 C94 N10 119.5(3) . . ? C96 C95 C94 119.9(3) . . ? C95 C96 C91 120.6(3) . . ? O10 C97 N10 122.8(3) . . ? O10 C97 C98 120.4(3) . . ? N10 C97 C98 116.8(3) . . ? C99 C98 C103 118.4(3) . . ? C99 C98 C97 119.8(3) . . ? C103 C98 C97 121.8(3) . . ? C98 C99 C100 121.3(3) . . ? C101 C100 C99 119.8(3) . . ? C100 C101 C102 119.7(3) . . ? C100 C101 N11 119.6(3) . . ? C102 C101 N11 120.7(3) . . ? C103 C102 C101 120.2(3) . . ? C102 C103 C98 120.6(3) . . ? O11 C104 N11 122.2(3) . . ? O11 C104 C105 120.9(3) . . ? N11 C104 C105 116.9(3) . . ? C110 C105 C106 118.9(3) . . ? C110 C105 C104 120.5(3) . . ? C106 C105 C104 120.6(3) . . ? C107 C106 C105 121.0(3) . . ? C106 C107 C108 119.3(3) . . ? C107 C108 C109 120.5(3) . . ? C107 C108 N12 120.5(3) . . ? C109 C108 N12 119.0(3) . . ? C110 C109 C108 119.6(3) . . ? C109 C110 C105 120.6(3) . . ? O12 C111 N12 122.9(3) . . ? O12 C111 C91 120.8(3) . . ? N12 C111 C91 116.3(3) . . ? N10 C112 C113 112.7(3) . . ? C112 C113 C114 112.8(3) . . ? C16A C115 N11 121.9(5) . . ? C16A C115 C116 28.9(4) . . ? N11 C115 C116 106.8(4) . . ? N12 C118 C119 113.4(3) . . ? C118 C119 C120 112.2(3) . . ? C126 C121 C122 118.1(4) . . ? C126 C121 C127 121.2(4) . . ? C122 C121 C127 120.6(4) . . ? C123 C122 C121 120.0(4) . . ? C124 C123 C122 121.4(4) . . ? C123 C124 C125 118.6(4) . . ? C126 C125 C124 120.9(4) . . ? C125 C126 C121 120.9(4) . . ? C133 C128 C129 117.8(4) . . ? C133 C128 C134 121.1(4) . . ? C129 C128 C134 121.1(4) . . ? C130 C129 C128 120.8(4) . . ? C131 C130 C129 120.7(4) . . ? C132 C131 C130 119.1(4) . . ? C131 C132 C133 120.8(4) . . ? C132 C133 C128 120.8(4) . . ? C136 C135 C140 116.7(5) . . ? C136 C135 C141 121.3(5) . . ? C140 C135 C141 122.0(5) . . ? C137 C136 C135 121.3(4) . . ? C138 C137 C136 122.6(5) . . ? C137 C138 C139 119.1(6) . . ? C138 C139 C140 121.8(5) . . ? C139 C140 C135 118.5(5) . . ? C147 C142 C143 118.4(4) . . ? C147 C142 C148 121.1(4) . . ? C143 C142 C148 120.5(4) . . ? C142 C143 C144 120.6(4) . . ? C145 C144 C143 120.6(5) . . ? C146 C145 C144 117.9(5) . . ? C147 C146 C145 121.6(5) . . ? C146 C147 C142 121.0(5) . . ? C117 C116 C115 110.5(6) . . ? C115 C16A C17A 106.2(7) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.714 _refine_diff_density_min -0.368 _refine_diff_density_rms 0.065 #===END data_2a _database_code_depnum_ccdc_archive 'CCDC 641458' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Methyl-4-[{N-(4-N_propylaminobenzoyl}-N- (4-N--propylamido)benzoyl)-N--propylamido]-benzoate ; _chemical_name_common 'propyl trimer' _chemical_melting_point ? _chemical_formula_moiety trimer _chemical_formula_sum 'C31 H39 N3 O5' _chemical_formula_weight 533.65 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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.3830(2) _cell_length_b 12.3990(3) _cell_length_c 12.8450(3) _cell_angle_alpha 104.730(1) _cell_angle_beta 91.325(1) _cell_angle_gamma 114.224(1) _cell_volume 1443.150(57) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 16413 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 27.485 _exptl_crystal_description Block _exptl_crystal_colour Clear _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.165 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.228 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 572 _exptl_absorpt_coefficient_mu 0.083 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.523 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 KappaCCD _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 28977 _diffrn_reflns_av_R_equivalents 0.0757 _diffrn_reflns_av_sigmaI/netI 0.0522 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.12 _diffrn_reflns_theta_max 27.51 _reflns_number_total 6611 _reflns_number_gt 4603 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo and Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0975P)^2^+0.1305P] 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_number_reflns 6611 _refine_ls_number_parameters 368 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0819 _refine_ls_R_factor_gt 0.0512 _refine_ls_wR_factor_ref 0.1650 _refine_ls_wR_factor_gt 0.1408 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.026 _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 O1 O 0.18870(15) 0.37068(13) 0.79995(10) 0.0446(3) Uani 1 1 d . . . O2 O 0.02640(13) -0.14918(11) 1.18285(10) 0.0468(3) Uani 1 1 d . . . N3 N 0.15699(15) 0.02897(13) 1.14645(11) 0.0362(3) Uani 1 1 d . . . O4 O 0.64662(12) 0.46058(10) 1.00468(9) 0.0374(3) Uani 1 1 d . . . N5 N 0.60684(14) 0.30540(12) 0.85184(10) 0.0317(3) Uani 1 1 d . . . O6 O 0.30308(15) -0.20408(12) 0.47044(10) 0.0521(4) Uani 1 1 d . . . O7 O 0.12261(14) -0.15119(13) 0.49853(10) 0.0574(4) Uani 1 1 d . . . C8 C 0.34645(18) 0.27751(15) 1.02076(13) 0.0346(4) Uani 1 1 d . . . H8 H 0.3332 0.3427 1.0035 0.042 Uiso 1 1 calc R . . C9 C 0.49163(17) 0.16996(14) 1.03013(12) 0.0313(3) Uani 1 1 d . . . H9 H 0.5758 0.1592 1.0164 0.038 Uiso 1 1 calc R . . C10 C 0.46954(17) 0.26220(14) 1.00057(12) 0.0297(3) Uani 1 1 d . . . C11 C 0.24333(18) 0.19823(15) 1.06581(13) 0.0355(4) Uani 1 1 d . . . H11 H 0.1576 0.2070 1.0769 0.043 Uiso 1 1 calc R . . C12 C 0.56428(18) 0.10450(15) 0.73003(13) 0.0353(4) Uani 1 1 d . . . H12 H 0.6596 0.1201 0.7528 0.042 Uiso 1 1 calc R . . C13 C 0.58050(17) 0.35094(14) 0.95260(13) 0.0313(3) Uani 1 1 d . . . C14 C 0.13704(17) -0.34091(15) 0.82707(13) 0.0358(4) Uani 1 1 d . . . C15 C 0.15093(18) -0.22304(16) 0.82598(14) 0.0378(4) Uani 1 1 d . . . H15 H 0.1674 -0.1991 0.7611 0.045 Uiso 1 1 calc R . . C16 C 0.09764(18) -0.09732(15) 1.11911(14) 0.0369(4) Uani 1 1 d . . . C17 C 0.10893(17) -0.37293(15) 0.92432(14) 0.0362(4) Uani 1 1 d . . . H17 H 0.0964 -0.4524 0.9271 0.043 Uiso 1 1 calc R . . C18 C 0.26448(17) 0.10542(14) 1.09504(13) 0.0325(3) Uani 1 1 d . . . C19 C 0.37037(18) 0.16404(15) 0.74737(13) 0.0360(4) Uani 1 1 d . . . H19 H 0.3336 0.2209 0.7809 0.043 Uiso 1 1 calc R . . C20 C 0.39022(17) 0.09345(14) 1.07991(13) 0.0330(4) Uani 1 1 d . . . H20 H 0.4072 0.0331 1.1035 0.040 Uiso 1 1 calc R . . C21 C 0.71707(17) 0.38950(15) 0.80277(14) 0.0348(4) Uani 1 1 d . . . H21A H 0.7653 0.3439 0.7581 0.042 Uiso 1 1 calc R . . H21B H 0.7897 0.4580 0.8614 0.042 Uiso 1 1 calc R . . C22 C 0.33850(18) -0.02575(14) 0.61615(12) 0.0347(4) Uani 1 1 d . . . C23 C 0.47839(19) -0.00162(15) 0.64859(13) 0.0378(4) Uani 1 1 d . . . H23 H 0.5154 -0.0582 0.6148 0.045 Uiso 1 1 calc R . . N24 N 0.14307(17) -0.42665(15) 0.73796(12) 0.0431(4) Uani 1 1 d . . . C25 C 0.28402(18) 0.05608(16) 0.66698(13) 0.0374(4) Uani 1 1 d . . . H25 H 0.1872 0.0382 0.6467 0.045 Uiso 1 1 calc R . . C26 C 0.11621(17) -0.17321(15) 1.01568(13) 0.0344(4) Uani 1 1 d . . . C27 C 0.51080(17) 0.18818(14) 0.77842(12) 0.0314(3) Uani 1 1 d . . . C28 C 0.09926(17) -0.29204(15) 1.01484(14) 0.0356(4) Uani 1 1 d . . . H28 H 0.0805 -0.3167 1.0792 0.043 Uiso 1 1 calc R . . C29 C 0.65481(19) 0.44275(17) 0.73191(15) 0.0424(4) Uani 1 1 d . . . H29A H 0.5806 0.3744 0.6741 0.051 Uiso 1 1 calc R . . H29B H 0.6090 0.4906 0.7768 0.051 Uiso 1 1 calc R . . C30 C 0.2556(2) -0.13610(16) 0.52179(13) 0.0399(4) Uani 1 1 d . . . C31 C 0.1333(2) 0.09372(16) 1.25218(14) 0.0409(4) Uani 1 1 d . . . H31A H 0.0359 0.0452 1.2661 0.049 Uiso 1 1 calc R . . H31B H 0.1407 0.1752 1.2499 0.049 Uiso 1 1 calc R . . C32 C 0.14075(18) -0.14213(15) 0.91833(14) 0.0367(4) Uani 1 1 d . . . H32 H 0.1507 -0.0633 0.9156 0.044 Uiso 1 1 calc R . . C33 C 0.0396(2) -0.2524(2) 0.40254(17) 0.0635(6) Uani 1 1 d . . . H33A H 0.0807 -0.2341 0.3377 0.095 Uiso 1 1 calc R . . H33B H -0.0592 -0.2624 0.3960 0.095 Uiso 1 1 calc R . . H33C H 0.0412 -0.3288 0.4092 0.095 Uiso 1 1 calc R . . C34 C 0.1970(2) -0.39785(18) 0.64050(15) 0.0462(4) Uani 1 1 d . . . H34A H 0.1575 -0.3442 0.6207 0.055 Uiso 1 1 calc R . . H34B H 0.1617 -0.4755 0.5802 0.055 Uiso 1 1 calc R . . C35 C 0.4288(2) -0.4123(2) 0.6762(2) 0.0657(6) Uani 1 1 d . . . H35A H 0.4034 -0.4306 0.7447 0.099 Uiso 1 1 calc R . . H35B H 0.5326 -0.3664 0.6828 0.099 Uiso 1 1 calc R . . H35C H 0.3964 -0.4897 0.6173 0.099 Uiso 1 1 calc R . . C36 C 0.7695(2) 0.52613(19) 0.68017(18) 0.0542(5) Uani 1 1 d . . . H36A H 0.8399 0.5966 0.7372 0.081 Uiso 1 1 calc R . . H36B H 0.7259 0.5561 0.6324 0.081 Uiso 1 1 calc R . . H36C H 0.8169 0.4795 0.6375 0.081 Uiso 1 1 calc R . . C37 C 0.2419(2) 0.11173(18) 1.34409(15) 0.0472(4) Uani 1 1 d . . . H37A H 0.2300 0.0299 1.3492 0.057 Uiso 1 1 calc R . . H37B H 0.3393 0.1549 1.3273 0.057 Uiso 1 1 calc R . . C38 C 0.3571(2) -0.33455(19) 0.65077(17) 0.0528(5) Uani 1 1 d . . . H38A H 0.3928 -0.2553 0.7093 0.063 Uiso 1 1 calc R . . H38B H 0.3841 -0.3155 0.5819 0.063 Uiso 1 1 calc R . . C39 C 0.2261(3) 0.1856(2) 1.45229(18) 0.0705(7) Uani 1 1 d . . . H39A H 0.2280 0.2631 1.4456 0.106 Uiso 1 1 calc R . . H39B H 0.3048 0.2037 1.5073 0.106 Uiso 1 1 calc R . . H39C H 0.1351 0.1377 1.4742 0.106 Uiso 1 1 calc R . . H1 H 0.153(2) -0.493(2) 0.7541(16) 0.050(5) Uiso 1 1 d . . . H3 H 0.132(3) 0.304(2) 0.8184(19) 0.064(7) Uiso 1 1 d . . . H4 H 0.248(3) 0.422(2) 0.864(2) 0.064(6) Uiso 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 O1 0.0488(8) 0.0337(7) 0.0385(7) 0.0106(6) -0.0020(6) 0.0059(6) O2 0.0450(8) 0.0386(7) 0.0472(7) 0.0166(6) 0.0143(6) 0.0060(6) N3 0.0337(8) 0.0331(7) 0.0420(8) 0.0142(6) 0.0102(6) 0.0123(6) O4 0.0380(7) 0.0243(6) 0.0400(6) 0.0059(5) -0.0014(5) 0.0063(5) N5 0.0296(7) 0.0265(7) 0.0323(7) 0.0085(5) 0.0026(5) 0.0057(6) O6 0.0649(9) 0.0390(7) 0.0428(7) 0.0026(6) 0.0009(6) 0.0190(7) O7 0.0423(8) 0.0560(8) 0.0446(8) -0.0104(6) -0.0071(6) 0.0082(7) C8 0.0382(9) 0.0311(8) 0.0372(8) 0.0120(7) 0.0035(7) 0.0164(7) C9 0.0281(8) 0.0281(8) 0.0355(8) 0.0089(6) 0.0022(6) 0.0103(6) C10 0.0300(8) 0.0242(7) 0.0294(7) 0.0060(6) 0.0001(6) 0.0075(6) C11 0.0320(9) 0.0352(9) 0.0423(9) 0.0135(7) 0.0054(7) 0.0161(7) C12 0.0338(9) 0.0322(8) 0.0374(8) 0.0106(7) 0.0016(7) 0.0117(7) C13 0.0303(8) 0.0274(8) 0.0351(8) 0.0108(7) -0.0003(6) 0.0106(7) C14 0.0283(8) 0.0334(8) 0.0402(9) 0.0117(7) -0.0001(7) 0.0076(7) C15 0.0353(9) 0.0360(9) 0.0395(9) 0.0167(7) 0.0012(7) 0.0097(7) C16 0.0292(8) 0.0333(8) 0.0441(9) 0.0156(7) 0.0032(7) 0.0071(7) C17 0.0296(8) 0.0300(8) 0.0459(9) 0.0147(7) 0.0022(7) 0.0080(7) C18 0.0292(8) 0.0291(8) 0.0362(8) 0.0105(7) 0.0042(6) 0.0091(7) C19 0.0335(9) 0.0349(9) 0.0346(8) 0.0069(7) 0.0036(7) 0.0116(7) C20 0.0331(9) 0.0291(8) 0.0376(8) 0.0118(7) 0.0039(7) 0.0130(7) C21 0.0293(8) 0.0308(8) 0.0402(9) 0.0121(7) 0.0059(7) 0.0079(7) C22 0.0382(9) 0.0294(8) 0.0292(8) 0.0098(7) 0.0037(7) 0.0068(7) C23 0.0428(10) 0.0319(8) 0.0374(9) 0.0091(7) 0.0046(7) 0.0155(8) N24 0.0494(9) 0.0397(8) 0.0424(8) 0.0153(7) 0.0090(7) 0.0191(7) C25 0.0300(9) 0.0388(9) 0.0348(8) 0.0095(7) 0.0009(7) 0.0075(7) C26 0.0263(8) 0.0308(8) 0.0408(9) 0.0134(7) 0.0014(6) 0.0056(7) C27 0.0317(8) 0.0265(8) 0.0301(8) 0.0098(6) 0.0021(6) 0.0061(7) C28 0.0286(8) 0.0350(9) 0.0399(9) 0.0160(7) 0.0028(7) 0.0076(7) C29 0.0369(10) 0.0423(10) 0.0495(10) 0.0230(8) 0.0083(8) 0.0129(8) C30 0.0452(10) 0.0337(9) 0.0322(8) 0.0125(7) 0.0049(7) 0.0072(8) C31 0.0408(10) 0.0385(9) 0.0460(10) 0.0147(8) 0.0144(8) 0.0179(8) C32 0.0326(9) 0.0317(8) 0.0428(9) 0.0146(7) 0.0005(7) 0.0090(7) C33 0.0504(13) 0.0592(13) 0.0436(11) -0.0099(10) -0.0066(9) 0.0029(10) C34 0.0491(11) 0.0487(11) 0.0400(9) 0.0163(8) 0.0061(8) 0.0184(9) C35 0.0527(13) 0.0705(15) 0.0903(17) 0.0436(13) 0.0222(12) 0.0298(12) C36 0.0499(12) 0.0530(12) 0.0697(13) 0.0371(11) 0.0169(10) 0.0201(10) C37 0.0485(11) 0.0436(10) 0.0463(10) 0.0129(8) 0.0090(8) 0.0167(9) C38 0.0528(12) 0.0512(11) 0.0553(11) 0.0226(10) 0.0112(9) 0.0187(10) C39 0.106(2) 0.0621(14) 0.0480(12) 0.0162(11) 0.0161(12) 0.0403(14) _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 O1 H3 0.89(3) . ? O1 H4 0.92(3) . ? O2 C16 1.240(2) . ? N3 C16 1.369(2) . ? N3 C18 1.437(2) . ? N3 C31 1.474(2) . ? O4 C13 1.2318(19) . ? N5 C13 1.357(2) . ? N5 C27 1.4375(19) . ? N5 C21 1.477(2) . ? O6 C30 1.209(2) . ? O7 C30 1.331(2) . ? O7 C33 1.454(2) . ? C8 C11 1.379(2) . ? C8 C10 1.388(2) . ? C8 H8 0.9500 . ? C9 C10 1.392(2) . ? C9 C20 1.392(2) . ? C9 H9 0.9500 . ? C10 C13 1.502(2) . ? C11 C18 1.392(2) . ? C11 H11 0.9500 . ? C12 C23 1.384(2) . ? C12 C27 1.390(2) . ? C12 H12 0.9500 . ? C14 N24 1.372(2) . ? C14 C17 1.406(2) . ? C14 C15 1.412(2) . ? C15 C32 1.383(2) . ? C15 H15 0.9500 . ? C16 C26 1.488(2) . ? C17 C28 1.365(2) . ? C17 H17 0.9500 . ? C18 C20 1.386(2) . ? C19 C27 1.389(2) . ? C19 C25 1.390(2) . ? C19 H19 0.9500 . ? C20 H20 0.9500 . ? C21 C29 1.520(2) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C23 1.387(2) . ? C22 C25 1.388(2) . ? C22 C30 1.491(2) . ? C23 H23 0.9500 . ? N24 C34 1.451(2) . ? N24 H1 0.94(2) . ? C25 H25 0.9500 . ? C26 C32 1.399(2) . ? C26 C28 1.407(2) . ? C28 H28 0.9500 . ? C29 C36 1.518(3) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C31 C37 1.521(3) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 H32 0.9500 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 C38 1.504(3) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 C38 1.525(3) . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 C39 1.511(3) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag H3 O1 H4 103.3(19) . . ? C16 N3 C18 126.22(14) . . ? C16 N3 C31 116.74(14) . . ? C18 N3 C31 115.56(13) . . ? C13 N5 C27 123.04(13) . . ? C13 N5 C21 119.24(13) . . ? C27 N5 C21 115.84(12) . . ? C30 O7 C33 114.98(16) . . ? C11 C8 C10 120.11(14) . . ? C11 C8 H8 119.9 . . ? C10 C8 H8 119.9 . . ? C10 C9 C20 119.87(15) . . ? C10 C9 H9 120.1 . . ? C20 C9 H9 120.1 . . ? C8 C10 C9 119.89(15) . . ? C8 C10 C13 118.80(13) . . ? C9 C10 C13 121.22(14) . . ? C8 C11 C18 120.22(15) . . ? C8 C11 H11 119.9 . . ? C18 C11 H11 119.9 . . ? C23 C12 C27 119.84(15) . . ? C23 C12 H12 120.1 . . ? C27 C12 H12 120.1 . . ? O4 C13 N5 121.75(15) . . ? O4 C13 C10 120.53(14) . . ? N5 C13 C10 117.69(13) . . ? N24 C14 C17 118.83(15) . . ? N24 C14 C15 123.79(15) . . ? C17 C14 C15 117.31(15) . . ? C32 C15 C14 120.70(15) . . ? C32 C15 H15 119.6 . . ? C14 C15 H15 119.6 . . ? O2 C16 N3 118.58(16) . . ? O2 C16 C26 119.49(15) . . ? N3 C16 C26 121.93(15) . . ? C28 C17 C14 121.29(15) . . ? C28 C17 H17 119.4 . . ? C14 C17 H17 119.4 . . ? C20 C18 C11 119.89(15) . . ? C20 C18 N3 121.89(14) . . ? C11 C18 N3 118.11(14) . . ? C27 C19 C25 119.53(15) . . ? C27 C19 H19 120.2 . . ? C25 C19 H19 120.2 . . ? C18 C20 C9 119.89(14) . . ? C18 C20 H20 120.1 . . ? C9 C20 H20 120.1 . . ? N5 C21 C29 112.26(14) . . ? N5 C21 H21A 109.2 . . ? C29 C21 H21A 109.2 . . ? N5 C21 H21B 109.2 . . ? C29 C21 H21B 109.2 . . ? H21A C21 H21B 107.9 . . ? C23 C22 C25 119.72(15) . . ? C23 C22 C30 117.56(15) . . ? C25 C22 C30 122.60(16) . . ? C12 C23 C22 120.30(15) . . ? C12 C23 H23 119.9 . . ? C22 C23 H23 119.9 . . ? C14 N24 C34 123.74(16) . . ? C14 N24 H1 114.1(12) . . ? C34 N24 H1 116.2(13) . . ? C22 C25 C19 120.32(16) . . ? C22 C25 H25 119.8 . . ? C19 C25 H25 119.8 . . ? C32 C26 C28 116.87(15) . . ? C32 C26 C16 127.27(15) . . ? C28 C26 C16 115.76(15) . . ? C19 C27 C12 120.24(14) . . ? C19 C27 N5 120.49(14) . . ? C12 C27 N5 118.92(14) . . ? C17 C28 C26 122.00(15) . . ? C17 C28 H28 119.0 . . ? C26 C28 H28 119.0 . . ? C36 C29 C21 111.21(15) . . ? C36 C29 H29A 109.4 . . ? C21 C29 H29A 109.4 . . ? C36 C29 H29B 109.4 . . ? C21 C29 H29B 109.4 . . ? H29A C29 H29B 108.0 . . ? O6 C30 O7 123.09(16) . . ? O6 C30 C22 124.42(17) . . ? O7 C30 C22 112.48(16) . . ? N3 C31 C37 111.19(14) . . ? N3 C31 H31A 109.4 . . ? C37 C31 H31A 109.4 . . ? N3 C31 H31B 109.4 . . ? C37 C31 H31B 109.4 . . ? H31A C31 H31B 108.0 . . ? C15 C32 C26 121.80(15) . . ? C15 C32 H32 119.1 . . ? C26 C32 H32 119.1 . . ? O7 C33 H33A 109.5 . . ? O7 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? O7 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? N24 C34 C38 114.55(16) . . ? N24 C34 H34A 108.6 . . ? C38 C34 H34A 108.6 . . ? N24 C34 H34B 108.6 . . ? C38 C34 H34B 108.6 . . ? H34A C34 H34B 107.6 . . ? C38 C35 H35A 109.5 . . ? C38 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C38 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C29 C36 H36A 109.5 . . ? C29 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C29 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C39 C37 C31 112.15(17) . . ? C39 C37 H37A 109.2 . . ? C31 C37 H37A 109.2 . . ? C39 C37 H37B 109.2 . . ? C31 C37 H37B 109.2 . . ? H37A C37 H37B 107.9 . . ? C34 C38 C35 112.92(18) . . ? C34 C38 H38A 109.0 . . ? C35 C38 H38A 109.0 . . ? C34 C38 H38B 109.0 . . ? C35 C38 H38B 109.0 . . ? H38A C38 H38B 107.8 . . ? C37 C39 H39A 109.5 . . ? C37 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C37 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.517 _refine_diff_density_min -0.326 _refine_diff_density_rms 0.064