Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _publ_contact_author_email V.GIBSON@IMPERIAL.AC.UK _publ_contact_author_name 'Andrew White' loop_ _publ_author_name 'Vernon Gibson ' 'Andrew R. F. Cox' 'Edward L. Marshall ' 'A White ' 'David Yeldon ' data_Compound_2a _database_code_depnum_ccdc_archive 'CCDC 293279' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C54 H100 K2 N6 O2' _chemical_formula_weight 943.60 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' K K 0.2009 0.2494 '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 11.0251(6) _cell_length_b 16.2531(7) _cell_length_c 17.4691(8) _cell_angle_alpha 77.252(4) _cell_angle_beta 77.205(4) _cell_angle_gamma 84.064(4) _cell_volume 2972.4(2) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 4.0420 _cell_measurement_theta_max 32.6208 _exptl_crystal_description blocks _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.37 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.054 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1040 _exptl_absorpt_coefficient_mu 0.200 _exptl_absorpt_correction_type 'numeric analytical' _exptl_absorpt_correction_T_min 0.93782 _exptl_absorpt_correction_T_max 0.96251 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'OD Xcalibur 3' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 15.9863 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 31328 _diffrn_reflns_av_R_equivalents 0.0170 _diffrn_reflns_av_sigmaI/netI 0.0181 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 4.05 _diffrn_reflns_theta_max 32.69 _reflns_number_total 19557 _reflns_number_gt 17872 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd' _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^)+(0.0647P)^2^+1.4438P] 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 SHELXL _refine_ls_extinction_coef 0.0009(12) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 19557 _refine_ls_number_parameters 651 _refine_ls_number_restraints 151 _refine_ls_R_factor_all 0.0769 _refine_ls_R_factor_gt 0.0710 _refine_ls_wR_factor_ref 0.1708 _refine_ls_wR_factor_gt 0.1657 _refine_ls_goodness_of_fit_ref 1.106 _refine_ls_restrained_S_all 1.127 _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 K1 K 1.15032(3) 0.13510(2) 0.20403(2) 0.03568(8) Uani 1 1 d . . . K2 K 0.87871(3) 0.27504(2) 0.25597(2) 0.03616(9) Uani 1 1 d . B . O1 O 0.91293(11) 0.11448(7) 0.23929(7) 0.0368(2) Uani 1 1 d . . . C1 C 0.87875(14) 0.03643(9) 0.25705(9) 0.0315(3) Uani 1 1 d . . . C2 C 0.91572(15) -0.01729(10) 0.20008(9) 0.0334(3) Uani 1 1 d . . . C3 C 0.87647(16) -0.09939(10) 0.21729(10) 0.0371(3) Uani 1 1 d . . . H3A H 0.8996 -0.1322 0.1770 0.045 Uiso 1 1 calc R . . C4 C 0.80494(17) -0.13526(10) 0.29087(10) 0.0379(3) Uani 1 1 d . A . C5 C 0.77166(16) -0.08366(10) 0.34759(9) 0.0362(3) Uani 1 1 d . . . H5A H 0.7243 -0.1069 0.3989 0.043 Uiso 1 1 calc R . . C6 C 0.80422(14) -0.00001(9) 0.33301(9) 0.0328(3) Uani 1 1 d . . . C7 C 0.99983(15) 0.01272(11) 0.12011(9) 0.0370(3) Uani 1 1 d . . . H7A H 0.9869 -0.0209 0.0821 0.044 Uiso 1 1 calc R . . H7B H 0.9748 0.0723 0.0994 0.044 Uiso 1 1 calc R . . N8 N 1.13550(13) 0.00678(8) 0.12163(8) 0.0341(3) Uani 1 1 d . . . C9 C 1.17746(17) -0.07772(10) 0.16087(11) 0.0406(3) Uani 1 1 d . . . H9A H 1.1923 -0.1156 0.1220 0.049 Uiso 1 1 calc R . . H9B H 1.1103 -0.1007 0.2061 0.049 Uiso 1 1 calc R . . C10 C 1.29570(18) -0.07818(11) 0.19229(12) 0.0440(4) Uani 1 1 d . . . H10A H 1.3212 -0.1374 0.2140 0.053 Uiso 1 1 calc R . . H10B H 1.3628 -0.0558 0.1467 0.053 Uiso 1 1 calc R . . N11 N 1.28466(15) -0.02870(9) 0.25498(9) 0.0419(3) Uani 1 1 d . . . C12 C 1.1782(2) -0.05063(13) 0.32237(12) 0.0495(4) Uani 1 1 d . . . H12A H 1.1007 -0.0348 0.3015 0.059 Uiso 1 1 calc R . . H12B H 1.1783 -0.0152 0.3617 0.059 Uiso 1 1 calc R . . C13 C 1.1728(3) -0.14256(17) 0.36704(15) 0.0721(7) Uani 1 1 d . . . H13A H 1.0977 -0.1490 0.4096 0.108 Uiso 1 1 calc R . . H13B H 1.2466 -0.1589 0.3907 0.108 Uiso 1 1 calc R . . H13C H 1.1704 -0.1789 0.3295 0.108 Uiso 1 1 calc R . . C14 C 1.4027(2) -0.03683(13) 0.28350(14) 0.0540(5) Uani 1 1 d . . . H14A H 1.4261 -0.0976 0.3001 0.065 Uiso 1 1 calc R . . H14B H 1.3889 -0.0114 0.3315 0.065 Uiso 1 1 calc R . . C15 C 1.5102(2) 0.00439(18) 0.22219(16) 0.0651(6) Uani 1 1 d . . . H15A H 1.5846 -0.0034 0.2456 0.098 Uiso 1 1 calc R . . H15B H 1.4889 0.0649 0.2062 0.098 Uiso 1 1 calc R . . H15C H 1.5266 -0.0216 0.1751 0.098 Uiso 1 1 calc R . . C16 C 1.20715(17) 0.02741(12) 0.03872(10) 0.0420(4) Uani 1 1 d . . . H16A H 1.1763 -0.0054 0.0062 0.050 Uiso 1 1 calc R . . H16B H 1.2954 0.0083 0.0388 0.050 Uiso 1 1 calc R . . C17 C 1.20222(18) 0.11993(13) -0.00222(10) 0.0451(4) Uani 1 1 d . . . H17A H 1.2472 0.1252 -0.0587 0.054 Uiso 1 1 calc R . . H17B H 1.1141 0.1391 -0.0027 0.054 Uiso 1 1 calc R . . N18 N 1.25564(13) 0.17672(9) 0.03493(8) 0.0390(3) Uani 1 1 d . . . C19 C 1.38394(18) 0.15257(14) 0.04349(14) 0.0510(4) Uani 1 1 d . . . H19A H 1.3857 0.0953 0.0778 0.061 Uiso 1 1 calc R . . H19B H 1.4096 0.1918 0.0723 0.061 Uiso 1 1 calc R . . C20 C 1.4795(2) 0.1520(2) -0.0331(2) 0.0926(11) Uani 1 1 d . . . H20A H 1.5617 0.1348 -0.0203 0.139 Uiso 1 1 calc R . . H20B H 1.4815 0.2088 -0.0670 0.139 Uiso 1 1 calc R . . H20C H 1.4572 0.1121 -0.0617 0.139 Uiso 1 1 calc R . . C21 C 1.23746(19) 0.26482(13) -0.00706(12) 0.0495(4) Uani 1 1 d . . . H21A H 1.1470 0.2793 -0.0020 0.059 Uiso 1 1 calc R . . H21B H 1.2744 0.2692 -0.0648 0.059 Uiso 1 1 calc R . . C22 C 1.2940(2) 0.32882(13) 0.02382(13) 0.0507(4) Uani 1 1 d . . . H22A H 1.2785 0.3856 -0.0070 0.076 Uiso 1 1 calc R . . H22B H 1.3840 0.3159 0.0179 0.076 Uiso 1 1 calc R . . H22C H 1.2562 0.3263 0.0805 0.076 Uiso 1 1 calc R . . C23 C 0.7717(2) -0.22791(11) 0.30956(12) 0.0475(4) Uani 1 1 d D . . C24 C 0.8966(6) -0.2836(3) 0.3102(7) 0.085(2) Uani 0.597(12) 1 d PDU A 1 H24A H 0.9537 -0.2680 0.2583 0.128 Uiso 0.597(12) 1 calc PR A 1 H24B H 0.8793 -0.3433 0.3198 0.128 Uiso 0.597(12) 1 calc PR A 1 H24C H 0.9349 -0.2741 0.3528 0.128 Uiso 0.597(12) 1 calc PR A 1 C25 C 0.7186(7) -0.2474(5) 0.2425(4) 0.0659(17) Uani 0.597(12) 1 d PDU A 1 H25A H 0.7757 -0.2298 0.1910 0.099 Uiso 0.597(12) 1 calc PR A 1 H25B H 0.6375 -0.2167 0.2412 0.099 Uiso 0.597(12) 1 calc PR A 1 H25C H 0.7083 -0.3082 0.2521 0.099 Uiso 0.597(12) 1 calc PR A 1 C26 C 0.6845(10) -0.2529(4) 0.3865(4) 0.099(3) Uani 0.597(12) 1 d PDU A 1 H26A H 0.6673 -0.3125 0.3944 0.148 Uiso 0.597(12) 1 calc PR A 1 H26B H 0.6066 -0.2180 0.3861 0.148 Uiso 0.597(12) 1 calc PR A 1 H26C H 0.7216 -0.2449 0.4302 0.148 Uiso 0.597(12) 1 calc PR A 1 C24' C 0.8481(9) -0.2795(4) 0.3659(7) 0.077(3) Uani 0.403(12) 1 d PDU A 2 H24D H 0.8270 -0.3387 0.3776 0.116 Uiso 0.403(12) 1 calc PR A 2 H24E H 0.8305 -0.2584 0.4159 0.116 Uiso 0.403(12) 1 calc PR A 2 H24F H 0.9368 -0.2752 0.3412 0.116 Uiso 0.403(12) 1 calc PR A 2 C25' C 0.7769(17) -0.2621(8) 0.2366(6) 0.102(5) Uani 0.403(12) 1 d PDU A 2 H25D H 0.7204 -0.2276 0.2045 0.153 Uiso 0.403(12) 1 calc PR A 2 H25E H 0.7516 -0.3205 0.2523 0.153 Uiso 0.403(12) 1 calc PR A 2 H25F H 0.8622 -0.2607 0.2047 0.153 Uiso 0.403(12) 1 calc PR A 2 C26' C 0.6318(7) -0.2352(5) 0.3590(7) 0.075(3) Uani 0.403(12) 1 d PDU A 2 H26D H 0.5754 -0.2004 0.3271 0.113 Uiso 0.403(12) 1 calc PR A 2 H26E H 0.6242 -0.2154 0.4091 0.113 Uiso 0.403(12) 1 calc PR A 2 H26F H 0.6098 -0.2943 0.3714 0.113 Uiso 0.403(12) 1 calc PR A 2 C27 C 0.75876(17) 0.05374(10) 0.39728(11) 0.0399(3) Uani 1 1 d . . . C28 C 0.6866(2) 0.00369(14) 0.47645(13) 0.0601(6) Uani 1 1 d . . . H28A H 0.7411 -0.0425 0.4989 0.090 Uiso 1 1 calc R . . H28B H 0.6144 -0.0197 0.4665 0.090 Uiso 1 1 calc R . . H28C H 0.6580 0.0413 0.5145 0.090 Uiso 1 1 calc R . . C29 C 0.66891(19) 0.12546(12) 0.36515(14) 0.0523(5) Uani 1 1 d . . . H29A H 0.7120 0.1590 0.3145 0.078 Uiso 1 1 calc R . . H29B H 0.6408 0.1617 0.4044 0.078 Uiso 1 1 calc R . . H29C H 0.5968 0.1012 0.3561 0.078 Uiso 1 1 calc R . . C30 C 0.8695(2) 0.08890(13) 0.41722(13) 0.0498(4) Uani 1 1 d . . . H30A H 0.9181 0.1217 0.3681 0.075 Uiso 1 1 calc R . . H30B H 0.9225 0.0420 0.4402 0.075 Uiso 1 1 calc R . . H30C H 0.8386 0.1254 0.4560 0.075 Uiso 1 1 calc R . . O31 O 1.11891(11) 0.28717(7) 0.23199(8) 0.0375(2) Uani 1 1 d . . . C31 C 1.16870(14) 0.35514(9) 0.23612(9) 0.0317(3) Uani 1 1 d . . . C32 C 1.14000(14) 0.43469(9) 0.18821(9) 0.0326(3) Uani 1 1 d . . . C33 C 1.19475(15) 0.50747(10) 0.18973(10) 0.0371(3) Uani 1 1 d . . . H33A H 1.1752 0.5588 0.1554 0.045 Uiso 1 1 calc R . . C34 C 1.27655(16) 0.50802(10) 0.23934(11) 0.0397(3) Uani 1 1 d . C . C35 C 1.30304(16) 0.43017(10) 0.28796(11) 0.0393(3) Uani 1 1 d . . . H35A H 1.3581 0.4289 0.3231 0.047 Uiso 1 1 calc R . . C36 C 1.25371(14) 0.35446(9) 0.28803(10) 0.0343(3) Uani 1 1 d . . . C37 C 1.04673(15) 0.44180(11) 0.13557(9) 0.0367(3) Uani 1 1 d . . . H37A H 1.0617 0.4932 0.0929 0.044 Uiso 1 1 calc R . . H37B H 1.0615 0.3926 0.1092 0.044 Uiso 1 1 calc R . . N38 N 0.91352(12) 0.44580(8) 0.17772(8) 0.0328(2) Uani 1 1 d . . . C39 C 0.88822(17) 0.50656(10) 0.23132(11) 0.0398(3) Uani 1 1 d . . . H39A H 0.8768 0.5641 0.1992 0.048 Uiso 1 1 calc R . . H39B H 0.9615 0.5057 0.2556 0.048 Uiso 1 1 calc R . . C40 C 0.77327(17) 0.48826(11) 0.29810(11) 0.0421(4) Uani 1 1 d . B . H40A H 0.7574 0.5350 0.3277 0.051 Uiso 1 1 calc R . . H40B H 0.7007 0.4882 0.2733 0.051 Uiso 1 1 calc R . . N41 N 0.78094(14) 0.40818(9) 0.35590(9) 0.0407(3) Uani 1 1 d D . . C42 C 0.8938(3) 0.3937(2) 0.38896(19) 0.0484(7) Uani 0.704(4) 1 d PD B 1 H42A H 0.9664 0.3925 0.3442 0.058 Uiso 0.704(4) 1 calc PR B 1 H42B H 0.8918 0.3372 0.4247 0.058 Uiso 0.704(4) 1 calc PR B 1 C43 C 0.9146(4) 0.4582(3) 0.4360(2) 0.0726(11) Uani 0.704(4) 1 d PD B 1 H43A H 0.9926 0.4426 0.4552 0.109 Uiso 0.704(4) 1 calc PR B 1 H43B H 0.8451 0.4588 0.4819 0.109 Uiso 0.704(4) 1 calc PR B 1 H43C H 0.9194 0.5144 0.4011 0.109 Uiso 0.704(4) 1 calc PR B 1 C44 C 0.6659(3) 0.4024(2) 0.4184(2) 0.0518(7) Uani 0.704(4) 1 d PD B 1 H44A H 0.5938 0.4087 0.3920 0.062 Uiso 0.704(4) 1 calc PR B 1 H44B H 0.6595 0.4505 0.4456 0.062 Uiso 0.704(4) 1 calc PR B 1 C45 C 0.6564(4) 0.3217(2) 0.4810(2) 0.0641(9) Uani 0.704(4) 1 d PD B 1 H45A H 0.5774 0.3237 0.5197 0.096 Uiso 0.704(4) 1 calc PR B 1 H45B H 0.7258 0.3154 0.5088 0.096 Uiso 0.704(4) 1 calc PR B 1 H45C H 0.6597 0.2736 0.4551 0.096 Uiso 0.704(4) 1 calc PR B 1 C42' C 0.8643(9) 0.4173(6) 0.4097(6) 0.064(3) Uiso 0.296(4) 1 d PD B 2 H42C H 0.8332 0.4664 0.4348 0.077 Uiso 0.296(4) 1 calc PR B 2 H42D H 0.9490 0.4283 0.3774 0.077 Uiso 0.296(4) 1 calc PR B 2 C43' C 0.8709(12) 0.3386(7) 0.4750(7) 0.096(4) Uiso 0.296(4) 1 d PD B 2 H43D H 0.9268 0.3470 0.5088 0.144 Uiso 0.296(4) 1 calc PR B 2 H43E H 0.9028 0.2899 0.4503 0.144 Uiso 0.296(4) 1 calc PR B 2 H43F H 0.7875 0.3282 0.5079 0.144 Uiso 0.296(4) 1 calc PR B 2 C44' C 0.6538(8) 0.3866(7) 0.3991(6) 0.062(3) Uiso 0.296(4) 1 d PD B 2 H44C H 0.6596 0.3291 0.4323 0.074 Uiso 0.296(4) 1 calc PR B 2 H44D H 0.6050 0.3837 0.3587 0.074 Uiso 0.296(4) 1 calc PR B 2 C45' C 0.5803(9) 0.4427(6) 0.4523(6) 0.077(3) Uiso 0.296(4) 1 d PD B 2 H45D H 0.4974 0.4213 0.4752 0.116 Uiso 0.296(4) 1 calc PR B 2 H45E H 0.5722 0.5002 0.4209 0.116 Uiso 0.296(4) 1 calc PR B 2 H45F H 0.6233 0.4433 0.4956 0.116 Uiso 0.296(4) 1 calc PR B 2 C46 C 0.83607(17) 0.47080(11) 0.11681(11) 0.0431(4) Uani 1 1 d . . . H46A H 0.8695 0.5219 0.0786 0.052 Uiso 1 1 calc R . . H46B H 0.7507 0.4865 0.1438 0.052 Uiso 1 1 calc R . . C47 C 0.82787(18) 0.40452(13) 0.06959(11) 0.0466(4) Uani 1 1 d . B . H47A H 0.7826 0.4305 0.0264 0.056 Uiso 1 1 calc R . . H47B H 0.9134 0.3876 0.0438 0.056 Uiso 1 1 calc R . . N48 N 0.76615(16) 0.32847(11) 0.11630(9) 0.0466(3) Uani 1 1 d . . . C49 C 0.6373(2) 0.34715(17) 0.15525(14) 0.0622(6) Uani 1 1 d . B . H49A H 0.6389 0.3835 0.1936 0.075 Uiso 1 1 calc R . . H49B H 0.6022 0.2934 0.1869 0.075 Uiso 1 1 calc R . . C50 C 0.5498(3) 0.3896(3) 0.1017(2) 0.0947(11) Uani 1 1 d . . . H50A H 0.4670 0.3987 0.1344 0.142 Uiso 1 1 calc R B . H50B H 0.5444 0.3536 0.0644 0.142 Uiso 1 1 calc R . . H50C H 0.5810 0.4441 0.0712 0.142 Uiso 1 1 calc R . . C51 C 0.7775(3) 0.26640(17) 0.06449(15) 0.0658(6) Uani 1 1 d . B . H51A H 0.8670 0.2552 0.0425 0.079 Uiso 1 1 calc R . . H51B H 0.7372 0.2918 0.0188 0.079 Uiso 1 1 calc R . . C52 C 0.7211(3) 0.18353(18) 0.1056(2) 0.0794(8) Uani 1 1 d . . . H52A H 0.7336 0.1460 0.0673 0.119 Uiso 1 1 calc R B . H52B H 0.6317 0.1935 0.1258 0.119 Uiso 1 1 calc R . . H52C H 0.7613 0.1571 0.1504 0.119 Uiso 1 1 calc R . . C53 C 1.3351(2) 0.58880(12) 0.24195(15) 0.0534(5) Uani 1 1 d D . . C54 C 1.4329(15) 0.6129(10) 0.1720(7) 0.120(7) Uani 0.270(7) 1 d PDU C 1 H54A H 1.5027 0.5704 0.1732 0.181 Uiso 0.270(7) 1 calc PR C 1 H54B H 1.4615 0.6679 0.1721 0.181 Uiso 0.270(7) 1 calc PR C 1 H54C H 1.4005 0.6165 0.1233 0.181 Uiso 0.270(7) 1 calc PR C 1 C55 C 1.2333(12) 0.6555(7) 0.2593(12) 0.120(6) Uani 0.270(7) 1 d PDU C 1 H55A H 1.2702 0.7062 0.2635 0.179 Uiso 0.270(7) 1 calc PR C 1 H55B H 1.1764 0.6341 0.3099 0.179 Uiso 0.270(7) 1 calc PR C 1 H55C H 1.1873 0.6696 0.2157 0.179 Uiso 0.270(7) 1 calc PR C 1 C56 C 1.4009(12) 0.5739(6) 0.3191(7) 0.077(3) Uani 0.270(7) 1 d PDU C 1 H56A H 1.4411 0.5169 0.3274 0.116 Uiso 0.270(7) 1 calc PR C 1 H56B H 1.3376 0.5802 0.3670 0.116 Uiso 0.270(7) 1 calc PR C 1 H56C H 1.4635 0.6157 0.3095 0.116 Uiso 0.270(7) 1 calc PR C 1 C54' C 1.4749(3) 0.5804(3) 0.2103(5) 0.100(2) Uani 0.730(7) 1 d PDU C 2 H54D H 1.4910 0.5676 0.1566 0.150 Uiso 0.730(7) 1 calc PR C 2 H54E H 1.5120 0.5345 0.2463 0.150 Uiso 0.730(7) 1 calc PR C 2 H54F H 1.5118 0.6335 0.2078 0.150 Uiso 0.730(7) 1 calc PR C 2 C55' C 1.2879(4) 0.66791(18) 0.1854(3) 0.0703(13) Uani 0.730(7) 1 d PDU C 2 H55D H 1.1967 0.6736 0.1989 0.106 Uiso 0.730(7) 1 calc PR C 2 H55E H 1.3150 0.6614 0.1296 0.106 Uiso 0.730(7) 1 calc PR C 2 H55F H 1.3222 0.7185 0.1920 0.106 Uiso 0.730(7) 1 calc PR C 2 C56' C 1.3020(8) 0.6059(3) 0.3243(3) 0.117(3) Uani 0.730(7) 1 d PDU C 2 H56D H 1.2112 0.6129 0.3407 0.176 Uiso 0.730(7) 1 calc PR C 2 H56E H 1.3396 0.6577 0.3253 0.176 Uiso 0.730(7) 1 calc PR C 2 H56F H 1.3335 0.5584 0.3615 0.176 Uiso 0.730(7) 1 calc PR C 2 C57 C 1.28747(17) 0.27130(11) 0.34285(12) 0.0439(4) Uani 1 1 d . . . C58 C 1.3777(2) 0.28300(15) 0.39455(15) 0.0614(6) Uani 1 1 d . . . H58A H 1.4542 0.3062 0.3597 0.092 Uiso 1 1 calc R . . H58B H 1.3980 0.2283 0.4274 0.092 Uiso 1 1 calc R . . H58C H 1.3386 0.3220 0.4296 0.092 Uiso 1 1 calc R . . C59 C 1.35386(19) 0.20792(12) 0.29138(15) 0.0540(5) Uani 1 1 d . . . H59A H 1.4295 0.2318 0.2561 0.081 Uiso 1 1 calc R . . H59B H 1.2981 0.1963 0.2589 0.081 Uiso 1 1 calc R . . H59C H 1.3762 0.1552 0.3264 0.081 Uiso 1 1 calc R . . C60 C 1.1688(2) 0.23528(15) 0.39899(15) 0.0654(6) Uani 1 1 d . . . H60A H 1.1280 0.2763 0.4314 0.098 Uiso 1 1 calc R . . H60B H 1.1907 0.1827 0.4343 0.098 Uiso 1 1 calc R . . H60C H 1.1121 0.2239 0.3671 0.098 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 K1 0.03794(17) 0.03199(15) 0.03991(17) -0.01272(12) -0.00881(13) -0.00125(12) K2 0.03892(17) 0.02677(14) 0.04042(17) -0.00397(12) -0.00536(13) -0.00336(11) O1 0.0383(6) 0.0260(5) 0.0453(6) -0.0071(4) -0.0061(5) -0.0046(4) C1 0.0324(7) 0.0262(6) 0.0365(7) -0.0052(5) -0.0094(5) -0.0013(5) C2 0.0379(7) 0.0324(7) 0.0308(6) -0.0047(5) -0.0091(5) -0.0052(5) C3 0.0469(9) 0.0323(7) 0.0352(7) -0.0102(6) -0.0099(6) -0.0052(6) C4 0.0498(9) 0.0274(6) 0.0370(7) -0.0045(5) -0.0097(6) -0.0067(6) C5 0.0451(8) 0.0291(6) 0.0323(7) -0.0026(5) -0.0063(6) -0.0043(6) C6 0.0360(7) 0.0274(6) 0.0356(7) -0.0065(5) -0.0096(6) 0.0000(5) C7 0.0401(8) 0.0412(8) 0.0307(7) -0.0053(6) -0.0094(6) -0.0069(6) N8 0.0372(6) 0.0345(6) 0.0323(6) -0.0099(5) -0.0076(5) -0.0025(5) C9 0.0481(9) 0.0349(7) 0.0439(8) -0.0164(6) -0.0143(7) 0.0026(6) C10 0.0479(9) 0.0394(8) 0.0505(9) -0.0205(7) -0.0166(8) 0.0093(7) N11 0.0482(8) 0.0399(7) 0.0438(7) -0.0162(6) -0.0190(6) 0.0068(6) C12 0.0611(11) 0.0480(10) 0.0424(9) -0.0144(8) -0.0144(8) 0.0032(8) C13 0.100(2) 0.0619(14) 0.0532(12) 0.0008(10) -0.0224(13) -0.0107(13) C14 0.0616(12) 0.0492(10) 0.0611(12) -0.0156(9) -0.0354(10) 0.0105(9) C15 0.0509(12) 0.0826(16) 0.0751(15) -0.0309(13) -0.0290(11) 0.0025(11) C16 0.0433(9) 0.0512(9) 0.0352(8) -0.0177(7) -0.0049(6) -0.0066(7) C17 0.0448(9) 0.0583(11) 0.0323(7) -0.0062(7) -0.0068(6) -0.0132(8) N18 0.0358(7) 0.0433(7) 0.0368(7) -0.0054(5) -0.0079(5) -0.0028(5) C19 0.0432(9) 0.0521(10) 0.0638(12) -0.0201(9) -0.0178(8) 0.0023(8) C20 0.0462(13) 0.117(3) 0.119(3) -0.066(2) 0.0142(14) -0.0045(14) C21 0.0488(10) 0.0519(10) 0.0452(9) 0.0019(8) -0.0149(8) -0.0052(8) C22 0.0518(10) 0.0459(10) 0.0509(10) -0.0045(8) -0.0085(8) -0.0024(8) C23 0.0674(12) 0.0290(7) 0.0474(9) -0.0057(7) -0.0125(8) -0.0114(7) C24 0.085(4) 0.0318(17) 0.149(7) -0.009(3) -0.054(4) -0.0034(19) C25 0.093(4) 0.048(3) 0.068(3) -0.006(2) -0.033(3) -0.032(3) C26 0.170(8) 0.048(3) 0.061(3) -0.011(2) 0.037(4) -0.057(4) C24' 0.090(6) 0.033(3) 0.104(7) 0.012(3) -0.035(5) 0.001(3) C25' 0.187(13) 0.050(5) 0.069(5) -0.021(4) 0.001(7) -0.049(8) C26' 0.078(5) 0.043(3) 0.107(7) -0.008(4) -0.025(4) -0.018(3) C27 0.0433(8) 0.0338(7) 0.0425(8) -0.0126(6) -0.0053(7) 0.0014(6) C28 0.0774(15) 0.0528(11) 0.0434(10) -0.0158(9) 0.0078(10) -0.0046(10) C29 0.0432(9) 0.0416(9) 0.0721(13) -0.0201(9) -0.0074(9) 0.0068(7) C30 0.0579(11) 0.0477(10) 0.0513(10) -0.0228(8) -0.0169(9) 0.0026(8) O31 0.0354(5) 0.0274(5) 0.0521(7) -0.0101(4) -0.0108(5) -0.0040(4) C31 0.0302(6) 0.0279(6) 0.0363(7) -0.0074(5) -0.0043(5) -0.0021(5) C32 0.0308(7) 0.0312(6) 0.0337(7) -0.0046(5) -0.0034(5) -0.0039(5) C33 0.0347(7) 0.0290(6) 0.0443(8) -0.0036(6) -0.0039(6) -0.0040(5) C34 0.0361(8) 0.0303(7) 0.0543(9) -0.0128(6) -0.0079(7) -0.0030(6) C35 0.0377(8) 0.0358(7) 0.0489(9) -0.0141(7) -0.0131(7) -0.0007(6) C36 0.0338(7) 0.0303(6) 0.0389(7) -0.0074(6) -0.0085(6) 0.0000(5) C37 0.0363(7) 0.0390(8) 0.0320(7) -0.0018(6) -0.0054(6) -0.0048(6) N38 0.0338(6) 0.0285(5) 0.0347(6) -0.0030(5) -0.0075(5) -0.0014(4) C39 0.0435(8) 0.0267(6) 0.0464(9) -0.0056(6) -0.0047(7) -0.0030(6) C40 0.0401(8) 0.0346(7) 0.0489(9) -0.0090(7) -0.0049(7) 0.0022(6) N41 0.0429(7) 0.0360(7) 0.0413(7) -0.0093(6) -0.0027(6) -0.0029(5) C42 0.0455(14) 0.0520(16) 0.0470(15) -0.0104(13) -0.0100(11) 0.0029(12) C43 0.073(2) 0.085(3) 0.070(2) -0.0220(19) -0.0278(18) -0.0135(19) C44 0.0442(15) 0.0580(18) 0.0500(17) -0.0130(15) 0.0031(12) -0.0117(13) C45 0.076(2) 0.0631(19) 0.0497(16) -0.0109(14) 0.0047(15) -0.0253(16) C46 0.0402(8) 0.0396(8) 0.0453(9) 0.0064(7) -0.0140(7) -0.0045(6) C47 0.0443(9) 0.0597(11) 0.0343(8) 0.0001(7) -0.0112(7) -0.0105(8) N48 0.0533(9) 0.0509(8) 0.0381(7) -0.0076(6) -0.0112(6) -0.0131(7) C49 0.0604(13) 0.0724(14) 0.0551(12) -0.0193(11) 0.0027(10) -0.0283(11) C50 0.0467(13) 0.140(3) 0.109(2) -0.046(2) -0.0206(15) -0.0038(16) C51 0.0765(16) 0.0711(15) 0.0590(13) -0.0235(11) -0.0206(12) -0.0095(12) C52 0.094(2) 0.0647(15) 0.098(2) -0.0259(14) -0.0510(18) -0.0043(14) C53 0.0526(11) 0.0332(8) 0.0818(14) -0.0161(9) -0.0227(10) -0.0069(7) C54 0.135(13) 0.112(11) 0.121(10) -0.007(8) -0.014(9) -0.098(10) C55 0.132(11) 0.048(5) 0.209(17) -0.053(8) -0.079(11) 0.011(6) C56 0.087(7) 0.051(5) 0.116(8) -0.039(5) -0.035(6) -0.022(5) C54' 0.0483(19) 0.053(2) 0.208(7) -0.027(3) -0.039(3) -0.0136(15) C55' 0.081(2) 0.0300(12) 0.107(3) -0.0025(15) -0.041(2) -0.0135(13) C56' 0.222(8) 0.067(3) 0.082(3) -0.034(2) -0.036(4) -0.046(4) C57 0.0428(9) 0.0354(8) 0.0526(10) -0.0024(7) -0.0165(7) 0.0016(6) C58 0.0710(14) 0.0559(12) 0.0636(13) -0.0096(10) -0.0364(11) 0.0110(10) C59 0.0448(10) 0.0366(8) 0.0856(15) -0.0156(9) -0.0253(10) 0.0068(7) C60 0.0545(12) 0.0583(12) 0.0648(13) 0.0201(10) -0.0086(10) 0.0027(10) _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 K1 O1 2.5919(12) . ? K1 O31 2.5977(11) . ? K1 N8 2.8193(13) . ? K1 N18 2.8798(15) . ? K1 N11 2.9659(15) . ? K2 O31 2.6092(12) . ? K2 O1 2.6684(11) . ? K2 N38 2.8340(13) . ? K2 N48 2.9035(16) . ? K2 N41 3.0402(15) . ? O1 C1 1.3119(17) . ? C1 C2 1.431(2) . ? C1 C6 1.434(2) . ? C2 C3 1.394(2) . ? C2 C7 1.506(2) . ? C3 C4 1.389(2) . ? C4 C5 1.401(2) . ? C4 C23 1.534(2) . ? C5 C6 1.396(2) . ? C6 C27 1.539(2) . ? C7 N8 1.495(2) . ? N8 C9 1.471(2) . ? N8 C16 1.472(2) . ? C9 C10 1.521(2) . ? C10 N11 1.473(2) . ? N11 C12 1.476(3) . ? N11 C14 1.477(2) . ? C12 C13 1.526(3) . ? C14 C15 1.511(4) . ? C16 C17 1.517(3) . ? C17 N18 1.472(2) . ? N18 C19 1.460(2) . ? N18 C21 1.473(2) . ? C19 C20 1.509(3) . ? C21 C22 1.514(3) . ? C23 C26 1.471(5) . ? C23 C25' 1.487(8) . ? C23 C24' 1.496(6) . ? C23 C25 1.524(5) . ? C23 C24 1.568(5) . ? C23 C26' 1.595(8) . ? C27 C28 1.535(3) . ? C27 C30 1.536(3) . ? C27 C29 1.541(3) . ? O31 C31 1.3058(17) . ? C31 C32 1.424(2) . ? C31 C36 1.439(2) . ? C32 C33 1.390(2) . ? C32 C37 1.504(2) . ? C33 C34 1.384(2) . ? C34 C35 1.403(2) . ? C34 C53 1.535(2) . ? C35 C36 1.396(2) . ? C36 C57 1.538(2) . ? C37 N38 1.492(2) . ? N38 C39 1.471(2) . ? N38 C46 1.472(2) . ? C39 C40 1.525(2) . ? C40 N41 1.468(2) . ? N41 C42 1.461(3) . ? N41 C44' 1.474(9) . ? N41 C44 1.475(3) . ? N41 C42' 1.490(8) . ? C42 C43 1.529(5) . ? C44 C45 1.507(5) . ? C42' C43' 1.522(11) . ? C44' C45' 1.496(11) . ? C46 C47 1.515(3) . ? C47 N48 1.463(2) . ? N48 C49 1.466(3) . ? N48 C51 1.476(3) . ? C49 C50 1.503(4) . ? C51 C52 1.505(4) . ? C53 C54 1.450(9) . ? C53 C56' 1.485(5) . ? C53 C55 1.506(9) . ? C53 C54' 1.521(4) . ? C53 C55' 1.559(4) . ? C53 C56 1.629(8) . ? C57 C60 1.534(3) . ? C57 C58 1.534(3) . ? C57 C59 1.538(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 K1 O31 92.63(4) . . ? O1 K1 N8 78.59(4) . . ? O31 K1 N8 155.91(4) . . ? O1 K1 N18 114.77(4) . . ? O31 K1 N18 98.35(4) . . ? N8 K1 N18 66.24(4) . . ? O1 K1 N11 109.05(4) . . ? O31 K1 N11 139.90(4) . . ? N8 K1 N11 63.84(4) . . ? N18 K1 N11 102.15(4) . . ? O31 K2 O1 90.64(4) . . ? O31 K2 N38 76.31(4) . . ? O1 K2 N38 145.40(4) . . ? O31 K2 N48 116.52(4) . . ? O1 K2 N48 93.18(4) . . ? N38 K2 N48 65.90(4) . . ? O31 K2 N41 101.56(4) . . ? O1 K2 N41 151.30(4) . . ? N38 K2 N41 63.29(4) . . ? N48 K2 N41 104.06(5) . . ? C1 O1 K1 116.79(9) . . ? C1 O1 K2 151.74(10) . . ? K1 O1 K2 87.61(3) . . ? O1 C1 C2 120.59(14) . . ? O1 C1 C6 122.98(14) . . ? C2 C1 C6 116.43(13) . . ? O1 C1 K1 43.02(7) . . ? C2 C1 K1 94.46(9) . . ? C6 C1 K1 133.02(10) . . ? C3 C2 C1 121.08(14) . . ? C3 C2 C7 117.91(14) . . ? C1 C2 C7 121.01(13) . . ? C4 C3 C2 122.76(14) . . ? C3 C4 C5 116.25(14) . . ? C3 C4 C23 121.11(15) . . ? C5 C4 C23 122.54(15) . . ? C6 C5 C4 123.71(15) . . ? C5 C6 C1 119.69(14) . . ? C5 C6 C27 120.45(14) . . ? C1 C6 C27 119.84(13) . . ? N8 C7 C2 114.80(13) . . ? N8 C7 K1 53.11(7) . . ? C2 C7 K1 90.74(9) . . ? C9 N8 C16 109.50(13) . . ? C9 N8 C7 112.26(13) . . ? C16 N8 C7 108.89(12) . . ? C9 N8 K1 113.81(9) . . ? C16 N8 K1 110.31(9) . . ? C7 N8 K1 101.80(9) . . ? N8 C9 C10 113.46(14) . . ? N11 C10 C9 114.86(14) . . ? C10 N11 C12 113.26(15) . . ? C10 N11 C14 110.14(15) . . ? C12 N11 C14 111.22(16) . . ? C10 N11 K1 107.86(10) . . ? C12 N11 K1 88.96(10) . . ? C14 N11 K1 123.93(11) . . ? N11 C12 C13 117.43(19) . . ? N11 C12 K1 64.38(9) . . ? C13 C12 K1 167.55(16) . . ? N11 C14 C15 114.35(17) . . ? N8 C16 C17 115.93(14) . . ? N18 C17 C16 115.10(15) . . ? C19 N18 C17 114.06(15) . . ? C19 N18 C21 113.67(15) . . ? C17 N18 C21 109.58(14) . . ? C19 N18 K1 95.16(11) . . ? C17 N18 K1 106.16(10) . . ? C21 N18 K1 117.52(11) . . ? N18 C19 C20 116.4(2) . . ? N18 C19 K1 59.07(9) . . ? C20 C19 K1 171.79(17) . . ? N18 C21 C22 114.25(16) . . ? C26 C23 C25' 124.9(6) . . ? C26 C23 C24' 74.0(5) . . ? C25' C23 C24' 114.0(6) . . ? C26 C23 C25 109.3(4) . . ? C25' C23 C25 25.2(6) . . ? C24' C23 C25 133.0(5) . . ? C26 C23 C4 113.9(2) . . ? C25' C23 C4 113.3(5) . . ? C24' C23 C4 109.6(3) . . ? C25 C23 C4 110.8(3) . . ? C26 C23 C24 109.5(4) . . ? C25' C23 C24 81.4(6) . . ? C24' C23 C24 38.6(4) . . ? C25 C23 C24 105.8(4) . . ? C4 C23 C24 107.2(2) . . ? C26 C23 C26' 30.9(4) . . ? C25' C23 C26' 106.2(6) . . ? C24' C23 C26' 104.2(4) . . ? C25 C23 C26' 84.2(4) . . ? C4 C23 C26' 108.9(3) . . ? C24 C23 C26' 135.8(4) . . ? C28 C27 C30 106.77(17) . . ? C28 C27 C6 113.05(14) . . ? C30 C27 C6 110.63(14) . . ? C28 C27 C29 107.12(17) . . ? C30 C27 C29 111.29(15) . . ? C6 C27 C29 107.97(15) . . ? C27 C29 K2 100.58(11) . . ? C31 O31 K1 148.38(10) . . ? C31 O31 K2 122.84(9) . . ? K1 O31 K2 88.76(3) . . ? O31 C31 C32 120.41(14) . . ? O31 C31 C36 122.88(13) . . ? C32 C31 C36 116.70(13) . . ? O31 C31 K2 38.86(7) . . ? C32 C31 K2 95.06(9) . . ? C36 C31 K2 136.08(10) . . ? C33 C32 C31 121.46(14) . . ? C33 C32 C37 118.42(14) . . ? C31 C32 C37 120.11(13) . . ? C34 C33 C32 122.59(15) . . ? C33 C34 C35 116.16(14) . . ? C33 C34 C53 122.46(16) . . ? C35 C34 C53 121.38(16) . . ? C36 C35 C34 124.19(15) . . ? C35 C36 C31 118.85(14) . . ? C35 C36 C57 121.30(15) . . ? C31 C36 C57 119.85(14) . . ? N38 C37 C32 115.13(13) . . ? N38 C37 K2 53.19(7) . . ? C32 C37 K2 94.69(9) . . ? C39 N38 C46 109.28(13) . . ? C39 N38 C37 112.36(13) . . ? C46 N38 C37 108.24(13) . . ? C39 N38 K2 114.85(9) . . ? C46 N38 K2 109.89(9) . . ? C37 N38 K2 101.88(9) . . ? N38 C39 C40 113.34(13) . . ? N41 C40 C39 115.47(14) . . ? C42 N41 C40 114.66(17) . . ? C42 N41 C44' 126.8(5) . . ? C40 N41 C44' 108.6(5) . . ? C42 N41 C44 112.9(2) . . ? C40 N41 C44 108.56(18) . . ? C44' N41 C44 20.0(4) . . ? C42 N41 C42' 23.6(4) . . ? C40 N41 C42' 108.6(4) . . ? C44' N41 C42' 113.4(6) . . ? C44 N41 C42' 95.4(5) . . ? C42 N41 K2 89.90(16) . . ? C40 N41 K2 105.71(10) . . ? C44' N41 K2 106.9(4) . . ? C44 N41 K2 124.35(18) . . ? C42' N41 K2 113.3(4) . . ? N41 C42 C43 116.3(3) . . ? N41 C42 K2 64.41(14) . . ? C43 C42 K2 169.4(2) . . ? N41 C44 C45 115.4(3) . . ? N41 C42' C43' 112.0(7) . . ? N41 C44' C45' 119.1(8) . . ? N38 C46 C47 115.64(14) . . ? N48 C47 C46 115.28(15) . . ? C47 N48 C49 112.40(17) . . ? C47 N48 C51 108.98(17) . . ? C49 N48 C51 113.33(18) . . ? C47 N48 K2 105.81(10) . . ? C49 N48 K2 100.12(12) . . ? C51 N48 K2 115.83(14) . . ? N48 C49 C50 117.0(2) . . ? N48 C49 K2 55.35(11) . . ? C50 C49 K2 169.37(18) . . ? N48 C51 C52 114.8(2) . . ? C54 C53 C56' 135.5(6) . . ? C54 C53 C55 116.4(8) . . ? C56' C53 C55 61.9(7) . . ? C54 C53 C54' 36.6(7) . . ? C56' C53 C54' 113.1(4) . . ? C55 C53 C54' 140.1(6) . . ? C54 C53 C34 111.4(5) . . ? C56' C53 C34 110.2(2) . . ? C55 C53 C34 109.3(5) . . ? C54' C53 C34 109.1(2) . . ? C54 C53 C55' 70.8(8) . . ? C56' C53 C55' 107.0(3) . . ? C55 C53 C55' 49.3(7) . . ? C54' C53 C55' 105.2(3) . . ? C34 C53 C55' 112.15(19) . . ? C54 C53 C56 106.0(6) . . ? C56' C53 C56 43.1(4) . . ? C55 C53 C56 102.7(6) . . ? C54' C53 C56 73.1(5) . . ? C34 C53 C56 110.6(3) . . ? C55' C53 C56 134.8(4) . . ? C60 C57 C58 108.17(19) . . ? C60 C57 C36 109.60(15) . . ? C58 C57 C36 112.49(15) . . ? C60 C57 C59 110.56(18) . . ? C58 C57 C59 106.39(16) . . ? C36 C57 C59 109.60(16) . . ? C57 C59 K1 110.99(11) . . ? _diffrn_measured_fraction_theta_max 0.894 _diffrn_reflns_theta_full 32.69 _diffrn_measured_fraction_theta_full 0.894 _refine_diff_density_max 0.349 _refine_diff_density_min -0.350 _refine_diff_density_rms 0.047 #===END data_Compound_3b _database_code_depnum_ccdc_archive 'CCDC 293280' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H53 Mg N3 O' _chemical_formula_weight 472.04 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' Mg Mg 0.0486 0.0363 '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)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.9731(4) _cell_length_b 12.3098(4) _cell_length_c 19.0286(6) _cell_angle_alpha 90.00 _cell_angle_beta 96.436(3) _cell_angle_gamma 90.00 _cell_volume 3019.64(17) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 4.2528 _cell_measurement_theta_max 32.5687 _exptl_crystal_description 'hexagonal plates' _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.29 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.038 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1048 _exptl_absorpt_coefficient_mu 0.081 _exptl_absorpt_correction_type 'numeric analytical' _exptl_absorpt_correction_T_min 0.97966 _exptl_absorpt_correction_T_max 0.98431 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'OD Xcalibur 3' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 15.9863 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26900 _diffrn_reflns_av_R_equivalents 0.0224 _diffrn_reflns_av_sigmaI/netI 0.0197 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 4.35 _diffrn_reflns_theta_max 32.64 _reflns_number_total 10268 _reflns_number_gt 9996 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd' _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^)+(0.0433P)^2^+1.6966P] 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 10268 _refine_ls_number_parameters 323 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.0797 _refine_ls_R_factor_gt 0.0767 _refine_ls_wR_factor_ref 0.1621 _refine_ls_wR_factor_gt 0.1605 _refine_ls_goodness_of_fit_ref 1.215 _refine_ls_restrained_S_all 1.220 _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 Mg Mg 0.90159(4) 0.51240(4) 0.17751(2) 0.02270(11) Uani 1 1 d . . . O1 O 0.93988(8) 0.39215(8) 0.12292(6) 0.0272(2) Uani 1 1 d . . . C1 C 0.87514(10) 0.32770(10) 0.08328(7) 0.0218(2) Uani 1 1 d . . . C2 C 0.89083(10) 0.21324(10) 0.08043(7) 0.0231(2) Uani 1 1 d . . . C3 C 0.82221(11) 0.15187(11) 0.03444(8) 0.0270(3) Uani 1 1 d . . . H3A H 0.8339 0.0758 0.0319 0.032 Uiso 1 1 calc R . . C4 C 0.73767(11) 0.19553(12) -0.00797(8) 0.0276(3) Uani 1 1 d . . . C5 C 0.72199(10) 0.30707(12) -0.00279(7) 0.0259(3) Uani 1 1 d . . . H5A H 0.6643 0.3394 -0.0302 0.031 Uiso 1 1 calc R . . C6 C 0.78830(10) 0.37249(11) 0.04140(7) 0.0223(2) Uani 1 1 d . . . C7 C 0.77157(11) 0.49393(11) 0.04003(7) 0.0246(2) Uani 1 1 d . . . H7A H 0.8314 0.5289 0.0211 0.030 Uiso 1 1 calc R . . H7B H 0.7089 0.5104 0.0071 0.030 Uiso 1 1 calc R . . N8 N 0.75894(9) 0.54313(9) 0.11072(6) 0.0232(2) Uani 1 1 d D A . C9 C 0.73512(12) 0.66092(12) 0.10342(9) 0.0321(3) Uani 1 1 d . . . H9A H 0.7178 0.6885 0.1496 0.038 Uiso 1 1 calc R . . H9B H 0.6727 0.6699 0.0689 0.038 Uiso 1 1 calc R . . C10 C 0.82211(14) 0.73111(12) 0.07967(9) 0.0361(3) Uani 1 1 d . . . H10A H 0.8437 0.6990 0.0359 0.043 Uiso 1 1 calc R . . H10B H 0.7933 0.8040 0.0673 0.043 Uiso 1 1 calc R . . C11 C 0.91846(14) 0.74566(12) 0.13218(10) 0.0376(4) Uani 1 1 d . . . H11A H 0.9590 0.8073 0.1162 0.045 Uiso 1 1 calc R . . H11B H 0.8962 0.7659 0.1785 0.045 Uiso 1 1 calc R . . N12 N 0.98807(10) 0.64958(10) 0.14261(7) 0.0289(2) Uani 1 1 d . . . C13 C 1.06993(14) 0.67348(16) 0.20103(10) 0.0423(4) Uani 1 1 d . . . H13A H 1.1114 0.7353 0.1880 0.064 Uiso 1 1 calc R . . H13B H 1.1148 0.6098 0.2099 0.064 Uiso 1 1 calc R . . H13C H 1.0379 0.6912 0.2438 0.064 Uiso 1 1 calc R . . C14 C 1.04000(14) 0.62944(14) 0.07824(9) 0.0369(3) Uani 1 1 d . . . H14A H 1.0767 0.6952 0.0661 0.055 Uiso 1 1 calc R . . H14B H 0.9879 0.6101 0.0389 0.055 Uiso 1 1 calc R . . H14C H 1.0897 0.5697 0.0871 0.055 Uiso 1 1 calc R . . C15 C 0.67656(10) 0.48671(12) 0.14526(7) 0.0257(2) Uani 1 1 d D . . H15A H 0.6681 0.5254 0.1899 0.031 Uiso 0.637(6) 1 calc PR A 1 H15B H 0.7016 0.4126 0.1582 0.031 Uiso 0.637(6) 1 calc PR A 1 H15C H 0.6793 0.5126 0.1930 0.031 Uiso 0.363(6) 1 d PR A 2 H15D H 0.6926 0.4106 0.1475 0.031 Uiso 0.363(6) 1 d PR A 2 C16 C 0.5673(2) 0.4764(4) 0.1022(2) 0.0312(7) Uani 0.637(6) 1 d PD A 1 H16A H 0.5479 0.5460 0.0783 0.037 Uiso 0.637(6) 1 calc PR A 1 H16B H 0.5687 0.4194 0.0656 0.037 Uiso 0.637(6) 1 calc PR A 1 C17 C 0.48743(19) 0.4468(3) 0.15232(14) 0.0377(7) Uani 0.637(6) 1 d PD A 1 H17A H 0.5139 0.3851 0.1824 0.045 Uiso 0.637(6) 1 calc PR A 1 H17B H 0.4783 0.5094 0.1837 0.045 Uiso 0.637(6) 1 calc PR A 1 N18 N 0.3870(3) 0.4176(5) 0.1146(4) 0.0368(13) Uani 0.637(6) 1 d PD A 1 C19 C 0.3800(4) 0.3038(3) 0.0934(2) 0.0502(9) Uani 0.637(6) 1 d PD A 1 H19A H 0.4359 0.2868 0.0646 0.075 Uiso 0.637(6) 1 calc PR A 1 H19B H 0.3128 0.2905 0.0658 0.075 Uiso 0.637(6) 1 calc PR A 1 H19C H 0.3866 0.2577 0.1357 0.075 Uiso 0.637(6) 1 calc PR A 1 C20 C 0.3044(3) 0.4396(4) 0.1605(3) 0.0648(11) Uani 0.637(6) 1 d PD A 1 H20A H 0.3168 0.3960 0.2037 0.097 Uiso 0.637(6) 1 calc PR A 1 H20B H 0.2368 0.4206 0.1353 0.097 Uiso 0.637(6) 1 calc PR A 1 H20C H 0.3050 0.5169 0.1730 0.097 Uiso 0.637(6) 1 calc PR A 1 C16' C 0.5674(5) 0.4989(6) 0.1120(4) 0.0278(16) Uiso 0.363(6) 1 d PD A 2 H16C H 0.5657 0.5039 0.0600 0.033 Uiso 0.363(6) 1 calc PR A 2 H16D H 0.5365 0.5660 0.1293 0.033 Uiso 0.363(6) 1 calc PR A 2 C17' C 0.5067(3) 0.4006(4) 0.1317(3) 0.0296(10) Uiso 0.363(6) 1 d PD A 2 H17C H 0.5328 0.3352 0.1091 0.035 Uiso 0.363(6) 1 calc PR A 2 H17D H 0.5179 0.3900 0.1836 0.035 Uiso 0.363(6) 1 calc PR A 2 N18' N 0.3941(7) 0.4124(10) 0.1093(8) 0.049(3) Uiso 0.363(6) 1 d PD A 2 C19' C 0.3465(7) 0.3065(7) 0.1073(5) 0.058(2) Uiso 0.363(6) 1 d PD A 2 H19D H 0.3810 0.2589 0.0759 0.087 Uiso 0.363(6) 1 calc PR A 2 H19E H 0.2729 0.3130 0.0896 0.087 Uiso 0.363(6) 1 calc PR A 2 H19F H 0.3533 0.2756 0.1551 0.087 Uiso 0.363(6) 1 calc PR A 2 C20' C 0.3412(5) 0.4837(5) 0.1505(3) 0.0459(14) Uiso 0.363(6) 1 d PD A 2 H20D H 0.2688 0.4903 0.1299 0.069 Uiso 0.363(6) 1 calc PR A 2 H20E H 0.3744 0.5553 0.1517 0.069 Uiso 0.363(6) 1 calc PR A 2 H20F H 0.3436 0.4552 0.1988 0.069 Uiso 0.363(6) 1 calc PR A 2 C21 C 0.98225(11) 0.16052(11) 0.12632(8) 0.0292(3) Uani 1 1 d . . . C22 C 0.97826(15) 0.18720(15) 0.20489(9) 0.0420(4) Uani 1 1 d . . . H22A H 1.0367 0.1521 0.2333 0.063 Uiso 1 1 calc R . . H22B H 0.9129 0.1605 0.2198 0.063 Uiso 1 1 calc R . . H22C H 0.9827 0.2660 0.2118 0.063 Uiso 1 1 calc R . . C23 C 1.08490(13) 0.20221(15) 0.10277(12) 0.0436(4) Uani 1 1 d . . . H23A H 1.1433 0.1679 0.1316 0.065 Uiso 1 1 calc R . . H23B H 1.0890 0.2812 0.1089 0.065 Uiso 1 1 calc R . . H23C H 1.0877 0.1841 0.0529 0.065 Uiso 1 1 calc R . . C24 C 0.98187(15) 0.03613(13) 0.11970(11) 0.0433(4) Uani 1 1 d . . . H24A H 1.0414 0.0061 0.1497 0.065 Uiso 1 1 calc R . . H24B H 0.9865 0.0158 0.0704 0.065 Uiso 1 1 calc R . . H24C H 0.9175 0.0072 0.1348 0.065 Uiso 1 1 calc R . . C25 C 0.66298(13) 0.12635(14) -0.05805(9) 0.0365(3) Uani 1 1 d . . . C26 C 0.6867(2) 0.00488(18) -0.05200(14) 0.0625(6) Uani 1 1 d . . . H26A H 0.6898 -0.0175 -0.0024 0.094 Uiso 1 1 calc R . . H26B H 0.7535 -0.0098 -0.0695 0.094 Uiso 1 1 calc R . . H26C H 0.6320 -0.0360 -0.0802 0.094 Uiso 1 1 calc R . . C27 C 0.6674(3) 0.1627(3) -0.13395(11) 0.0869(11) Uani 1 1 d . . . H27A H 0.7196 0.1199 -0.1551 0.130 Uiso 1 1 calc R . . H27B H 0.6860 0.2398 -0.1346 0.130 Uiso 1 1 calc R . . H27C H 0.5994 0.1519 -0.1611 0.130 Uiso 1 1 calc R . . C28 C 0.55228(17) 0.1407(2) -0.03876(15) 0.0658(7) Uani 1 1 d . . . H28A H 0.5476 0.1110 0.0086 0.099 Uiso 1 1 calc R . . H28B H 0.5037 0.1021 -0.0733 0.099 Uiso 1 1 calc R . . H28C H 0.5347 0.2181 -0.0392 0.099 Uiso 1 1 calc R . . C30 C 0.89006(13) 0.52308(15) 0.28920(8) 0.0360(3) Uani 1 1 d . . . H30A H 0.9626 0.5189 0.3132 0.043 Uiso 1 1 calc R . . C31 C 0.83078(17) 0.4278(2) 0.31757(10) 0.0546(6) Uani 1 1 d . . . H31A H 0.8283 0.4370 0.3685 0.082 Uiso 1 1 calc R . . H31B H 0.8662 0.3596 0.3089 0.082 Uiso 1 1 calc R . . H31C H 0.7600 0.4260 0.2934 0.082 Uiso 1 1 calc R . . C32 C 0.84412(18) 0.6303(2) 0.31329(11) 0.0553(5) Uani 1 1 d . . . H32A H 0.8417 0.6284 0.3646 0.083 Uiso 1 1 calc R . . H32B H 0.7738 0.6396 0.2893 0.083 Uiso 1 1 calc R . . H32C H 0.8877 0.6911 0.3013 0.083 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mg 0.0243(2) 0.0211(2) 0.0230(2) -0.00052(16) 0.00367(16) -0.00275(16) O1 0.0252(5) 0.0204(4) 0.0344(5) -0.0052(4) -0.0037(4) 0.0004(3) C1 0.0216(5) 0.0203(5) 0.0234(5) -0.0011(4) 0.0029(4) 0.0000(4) C2 0.0235(6) 0.0200(5) 0.0262(6) 0.0000(4) 0.0042(4) -0.0005(4) C3 0.0298(6) 0.0212(6) 0.0305(6) -0.0029(5) 0.0062(5) -0.0034(5) C4 0.0272(6) 0.0288(6) 0.0274(6) -0.0049(5) 0.0048(5) -0.0069(5) C5 0.0222(6) 0.0321(7) 0.0233(6) -0.0015(5) 0.0012(4) -0.0013(5) C6 0.0234(5) 0.0227(5) 0.0212(5) -0.0010(4) 0.0040(4) 0.0010(4) C7 0.0280(6) 0.0239(6) 0.0220(5) 0.0010(4) 0.0032(4) 0.0046(5) N8 0.0254(5) 0.0197(5) 0.0250(5) 0.0006(4) 0.0049(4) 0.0025(4) C9 0.0345(7) 0.0234(6) 0.0393(8) 0.0008(5) 0.0082(6) 0.0073(5) C10 0.0460(9) 0.0200(6) 0.0443(9) 0.0053(6) 0.0138(7) 0.0046(6) C11 0.0456(9) 0.0201(6) 0.0498(9) -0.0049(6) 0.0171(7) -0.0041(6) N12 0.0315(6) 0.0246(5) 0.0326(6) -0.0041(4) 0.0113(5) -0.0053(4) C13 0.0376(8) 0.0454(9) 0.0446(9) -0.0095(7) 0.0070(7) -0.0168(7) C14 0.0391(8) 0.0371(8) 0.0379(8) -0.0031(6) 0.0194(7) -0.0046(6) C15 0.0230(6) 0.0301(6) 0.0241(6) 0.0010(5) 0.0028(4) 0.0013(5) C16 0.0208(12) 0.043(2) 0.0290(16) -0.0002(14) -0.0003(9) 0.0020(11) C17 0.0263(11) 0.0548(18) 0.0316(12) -0.0047(12) 0.0019(9) -0.0077(11) N18 0.0181(11) 0.048(2) 0.041(2) 0.0127(12) -0.0100(10) -0.0093(10) C19 0.055(2) 0.055(2) 0.0380(17) -0.0035(14) -0.0065(16) 0.0045(17) C20 0.0421(18) 0.069(3) 0.084(3) -0.006(2) 0.0106(18) -0.0024(18) C21 0.0290(7) 0.0203(6) 0.0377(7) 0.0035(5) 0.0012(5) 0.0021(5) C22 0.0486(10) 0.0392(9) 0.0358(8) 0.0061(7) -0.0052(7) 0.0069(7) C23 0.0277(7) 0.0348(8) 0.0685(12) 0.0117(8) 0.0065(7) 0.0051(6) C24 0.0483(10) 0.0227(7) 0.0574(11) 0.0053(7) -0.0010(8) 0.0056(6) C25 0.0374(8) 0.0371(8) 0.0340(7) -0.0076(6) -0.0003(6) -0.0119(6) C26 0.0659(14) 0.0427(11) 0.0750(15) -0.0213(10) -0.0097(12) -0.0141(10) C27 0.127(3) 0.098(2) 0.0315(10) -0.0058(11) -0.0065(12) -0.071(2) C28 0.0369(10) 0.0752(16) 0.0838(17) -0.0227(13) -0.0001(10) -0.0194(10) C30 0.0310(7) 0.0523(10) 0.0247(6) 0.0020(6) 0.0032(5) -0.0092(7) C31 0.0524(11) 0.0763(15) 0.0344(9) 0.0183(9) 0.0022(8) -0.0218(10) C32 0.0545(12) 0.0753(15) 0.0397(9) -0.0161(10) 0.0211(9) -0.0065(11) _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 Mg O1 1.9060(11) . ? Mg C30 2.1512(16) . ? Mg N8 2.1577(12) . ? Mg N12 2.1721(13) . ? O1 C1 1.3273(15) . ? C1 C6 1.4167(18) . ? C1 C2 1.4255(18) . ? C2 C3 1.3979(19) . ? C2 C21 1.5356(19) . ? C3 C4 1.395(2) . ? C4 C5 1.393(2) . ? C4 C25 1.538(2) . ? C5 C6 1.3905(18) . ? C6 C7 1.5103(18) . ? C7 N8 1.5008(17) . ? N8 C9 1.4858(18) . ? N8 C15 1.4880(17) . ? C9 C10 1.529(2) . ? C10 C11 1.521(3) . ? C11 N12 1.488(2) . ? N12 C13 1.478(2) . ? N12 C14 1.4835(19) . ? C15 C16' 1.492(7) . ? C15 C16 1.561(3) . ? C16 C17 1.528(4) . ? C17 N18 1.461(4) . ? N18 C19 1.457(6) . ? N18 C20 1.481(7) . ? C16' C17' 1.513(8) . ? C17' N18' 1.482(10) . ? N18' C20' 1.406(11) . ? N18' C19' 1.441(11) . ? C21 C24 1.536(2) . ? C21 C22 1.537(2) . ? C21 C23 1.540(2) . ? C25 C27 1.519(3) . ? C25 C26 1.528(3) . ? C25 C28 1.532(3) . ? C30 C31 1.533(3) . ? C30 C32 1.539(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Mg C30 129.58(6) . . ? O1 Mg N8 94.23(5) . . ? C30 Mg N8 114.91(6) . . ? O1 Mg N12 105.19(5) . . ? C30 Mg N12 110.49(6) . . ? N8 Mg N12 97.00(5) . . ? C1 O1 Mg 125.94(9) . . ? O1 C1 C6 119.98(11) . . ? O1 C1 C2 121.91(12) . . ? C6 C1 C2 118.11(12) . . ? C3 C2 C1 118.32(12) . . ? C3 C2 C21 121.64(12) . . ? C1 C2 C21 120.03(12) . . ? C4 C3 C2 123.94(13) . . ? C5 C4 C3 116.78(12) . . ? C5 C4 C25 120.18(14) . . ? C3 C4 C25 123.04(14) . . ? C6 C5 C4 121.89(13) . . ? C5 C6 C1 120.92(12) . . ? C5 C6 C7 119.00(12) . . ? C1 C6 C7 119.91(12) . . ? N8 C7 C6 114.44(11) . . ? C9 N8 C15 110.16(11) . . ? C9 N8 C7 110.64(11) . . ? C15 N8 C7 111.32(11) . . ? C9 N8 Mg 112.44(9) . . ? C15 N8 Mg 105.61(8) . . ? C7 N8 Mg 106.54(8) . . ? N8 C9 C10 115.24(12) . . ? C11 C10 C9 116.86(14) . . ? N12 C11 C10 115.84(13) . . ? C13 N12 C14 107.44(13) . . ? C13 N12 C11 108.44(13) . . ? C14 N12 C11 110.35(13) . . ? C13 N12 Mg 106.08(10) . . ? C14 N12 Mg 114.86(9) . . ? C11 N12 Mg 109.40(9) . . ? N8 C15 C16' 117.4(3) . . ? N8 C15 C16 117.48(17) . . ? C16' C15 C16 12.3(3) . . ? C17 C16 C15 109.3(2) . . ? N18 C17 C16 112.4(3) . . ? C19 N18 C17 113.4(4) . . ? C19 N18 C20 108.2(4) . . ? C17 N18 C20 109.2(5) . . ? C15 C16' C17' 108.1(5) . . ? N18' C17' C16' 111.9(6) . . ? C20' N18' C19' 110.2(9) . . ? C20' N18' C17' 115.3(9) . . ? C19' N18' C17' 108.9(9) . . ? C2 C21 C24 112.29(13) . . ? C2 C21 C22 110.77(12) . . ? C24 C21 C22 107.01(14) . . ? C2 C21 C23 109.37(12) . . ? C24 C21 C23 107.65(14) . . ? C22 C21 C23 109.65(15) . . ? C27 C25 C26 109.3(2) . . ? C27 C25 C28 109.3(2) . . ? C26 C25 C28 106.31(18) . . ? C27 C25 C4 109.74(14) . . ? C26 C25 C4 112.80(15) . . ? C28 C25 C4 109.28(15) . . ? C31 C30 C32 108.94(16) . . ? C31 C30 Mg 113.22(12) . . ? C32 C30 Mg 114.76(12) . . ? _diffrn_measured_fraction_theta_max 0.929 _diffrn_reflns_theta_full 32.64 _diffrn_measured_fraction_theta_full 0.929 _refine_diff_density_max 0.356 _refine_diff_density_min -0.299 _refine_diff_density_rms 0.044 #===END data_Compound_6c _database_code_depnum_ccdc_archive 'CCDC 293281' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C23 H42 Al N O3' _chemical_formula_weight 407.56 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' Al Al 0.0645 0.0514 '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 10.3132(4) _cell_length_b 11.9611(5) _cell_length_c 20.6126(9) _cell_angle_alpha 86.978(3) _cell_angle_beta 86.976(3) _cell_angle_gamma 89.506(3) _cell_volume 2535.60(18) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 3.9796 _cell_measurement_theta_max 32.6455 _exptl_crystal_description 'blocky needles' _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.068 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 896 _exptl_absorpt_coefficient_mu 0.100 _exptl_absorpt_correction_type 'numeric analytical' _exptl_absorpt_correction_T_min 0.97861 _exptl_absorpt_correction_T_max 0.99133 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'OD Xcalibur 3' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 15.9863 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27740 _diffrn_reflns_av_R_equivalents 0.0383 _diffrn_reflns_av_sigmaI/netI 0.0629 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 3.99 _diffrn_reflns_theta_max 32.72 _reflns_number_total 16761 _reflns_number_gt 10237 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd' _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^)+(0.1102P)^2^+0.5083P] 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 16761 _refine_ls_number_parameters 546 _refine_ls_number_restraints 60 _refine_ls_R_factor_all 0.1156 _refine_ls_R_factor_gt 0.0739 _refine_ls_wR_factor_ref 0.2299 _refine_ls_wR_factor_gt 0.2055 _refine_ls_goodness_of_fit_ref 1.085 _refine_ls_restrained_S_all 1.108 _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 Al Al 0.45875(6) 0.62962(5) 0.14468(3) 0.02886(14) Uani 1 1 d . . . O1 O 0.41917(14) 0.54184(13) 0.21484(7) 0.0340(3) Uani 1 1 d . . . C1 C 0.48924(19) 0.48813(16) 0.25962(10) 0.0279(4) Uani 1 1 d . . . C2 C 0.4351(2) 0.45688(16) 0.32255(10) 0.0292(4) Uani 1 1 d . . . C3 C 0.5172(2) 0.40239(18) 0.36585(10) 0.0340(4) Uani 1 1 d . . . H3A H 0.4818 0.3802 0.4080 0.041 Uiso 1 1 calc R . . C4 C 0.6478(2) 0.37838(18) 0.35143(10) 0.0331(4) Uani 1 1 d . A . C5 C 0.6970(2) 0.40880(16) 0.28897(10) 0.0301(4) Uani 1 1 d . . . H5A H 0.7855 0.3936 0.2773 0.036 Uiso 1 1 calc R . . C6 C 0.6191(2) 0.46108(16) 0.24327(9) 0.0278(4) Uani 1 1 d . . . C7 C 0.66922(19) 0.48167(15) 0.17392(9) 0.0273(4) Uani 1 1 d . . . H7A H 0.6219 0.4326 0.1462 0.033 Uiso 1 1 calc R . . H7B H 0.7621 0.4598 0.1706 0.033 Uiso 1 1 calc R . . N8 N 0.65624(16) 0.60127(13) 0.14748(8) 0.0254(3) Uani 1 1 d . . . C9 C 0.7237(2) 0.60561(17) 0.08124(9) 0.0307(4) Uani 1 1 d . . . H9A H 0.6851 0.5487 0.0550 0.037 Uiso 1 1 calc R . . H9B H 0.8163 0.5857 0.0857 0.037 Uiso 1 1 calc R . . C10 C 0.7153(2) 0.71874(19) 0.04528(11) 0.0351(4) Uani 1 1 d . . . H10A H 0.7631 0.7752 0.0679 0.042 Uiso 1 1 calc R . . H10B H 0.7540 0.7149 0.0005 0.042 Uiso 1 1 calc R . . O11 O 0.58348(16) 0.74821(14) 0.04378(10) 0.0486(4) Uani 1 1 d . . . C12 C 0.5605(3) 0.8534(2) 0.01346(13) 0.0459(6) Uani 1 1 d . . . H12A H 0.4669 0.8684 0.0145 0.069 Uiso 1 1 calc R . . H12B H 0.5949 0.8545 -0.0318 0.069 Uiso 1 1 calc R . . H12C H 0.6037 0.9110 0.0365 0.069 Uiso 1 1 calc R . . C13 C 0.71238(19) 0.68034(16) 0.19218(10) 0.0288(4) Uani 1 1 d . . . H13A H 0.6609 0.6739 0.2341 0.035 Uiso 1 1 calc R . . H13B H 0.6994 0.7574 0.1735 0.035 Uiso 1 1 calc R . . C14 C 0.8536(2) 0.66735(19) 0.20664(11) 0.0362(5) Uani 1 1 d . . . H14A H 0.8704 0.7046 0.2471 0.043 Uiso 1 1 calc R . . H14B H 0.8755 0.5869 0.2132 0.043 Uiso 1 1 calc R . . O15 O 0.93219(15) 0.71582(16) 0.15416(9) 0.0461(4) Uani 1 1 d . . . C16 C 1.0636(3) 0.7260(3) 0.17039(17) 0.0628(8) Uani 1 1 d . . . H16A H 1.1146 0.7593 0.1329 0.094 Uiso 1 1 calc R . . H16B H 1.0988 0.6517 0.1821 0.094 Uiso 1 1 calc R . . H16C H 1.0681 0.7739 0.2073 0.094 Uiso 1 1 calc R . . C17 C 0.2920(2) 0.48210(18) 0.34137(11) 0.0344(4) Uani 1 1 d . . . C18 C 0.2701(2) 0.6091(2) 0.33935(13) 0.0444(5) Uani 1 1 d . . . H18A H 0.3270 0.6428 0.3694 0.067 Uiso 1 1 calc R . . H18B H 0.1793 0.6252 0.3522 0.067 Uiso 1 1 calc R . . H18C H 0.2899 0.6405 0.2951 0.067 Uiso 1 1 calc R . . C19 C 0.2033(2) 0.4291(2) 0.29413(13) 0.0443(6) Uani 1 1 d . . . H19A H 0.2172 0.3479 0.2956 0.066 Uiso 1 1 calc R . . H19B H 0.2235 0.4602 0.2499 0.066 Uiso 1 1 calc R . . H19C H 0.1124 0.4453 0.3068 0.066 Uiso 1 1 calc R . . C20 C 0.2519(3) 0.4352(3) 0.40956(12) 0.0497(6) Uani 1 1 d . . . H20A H 0.3068 0.4672 0.4411 0.075 Uiso 1 1 calc R . . H20B H 0.2620 0.3536 0.4115 0.075 Uiso 1 1 calc R . . H20C H 0.1609 0.4546 0.4199 0.075 Uiso 1 1 calc R . . C21 C 0.7338(2) 0.3190(2) 0.40156(11) 0.0449(6) Uani 1 1 d D . . C22 C 0.6638(4) 0.2957(5) 0.46717(18) 0.0634(14) Uani 0.713(6) 1 d PD A 1 H22A H 0.6630 0.3634 0.4919 0.095 Uiso 0.713(6) 1 calc PR A 1 H22B H 0.7087 0.2353 0.4911 0.095 Uiso 0.713(6) 1 calc PR A 1 H22C H 0.5744 0.2731 0.4610 0.095 Uiso 0.713(6) 1 calc PR A 1 C23 C 0.7981(6) 0.2184(4) 0.3763(2) 0.083(2) Uani 0.713(6) 1 d PD A 1 H23A H 0.8836 0.2386 0.3563 0.125 Uiso 0.713(6) 1 calc PR A 1 H23B H 0.7449 0.1873 0.3437 0.125 Uiso 0.713(6) 1 calc PR A 1 H23C H 0.8087 0.1625 0.4122 0.125 Uiso 0.713(6) 1 calc PR A 1 C24 C 0.8449(4) 0.4040(5) 0.4166(2) 0.0736(17) Uani 0.713(6) 1 d PD A 1 H24A H 0.8155 0.4809 0.4069 0.110 Uiso 0.713(6) 1 calc PR A 1 H24B H 0.9233 0.3887 0.3895 0.110 Uiso 0.713(6) 1 calc PR A 1 H24C H 0.8643 0.3947 0.4626 0.110 Uiso 0.713(6) 1 calc PR A 1 C22A C 0.7099(12) 0.3627(10) 0.4652(5) 0.066(3) Uiso 0.287(6) 1 d PD A 2 H22D H 0.7370 0.4411 0.4640 0.100 Uiso 0.287(6) 1 calc PR A 2 H22E H 0.7595 0.3189 0.4970 0.100 Uiso 0.287(6) 1 calc PR A 2 H22F H 0.6171 0.3577 0.4777 0.100 Uiso 0.287(6) 1 calc PR A 2 C23A C 0.6804(11) 0.1911(8) 0.4063(6) 0.069(3) Uiso 0.287(6) 1 d PD A 2 H23D H 0.5919 0.1902 0.3913 0.103 Uiso 0.287(6) 1 calc PR A 2 H23E H 0.6803 0.1615 0.4515 0.103 Uiso 0.287(6) 1 calc PR A 2 H23F H 0.7370 0.1447 0.3789 0.103 Uiso 0.287(6) 1 calc PR A 2 C24A C 0.8690(9) 0.3098(10) 0.3793(5) 0.061(3) Uiso 0.287(6) 1 d PD A 2 H24D H 0.9088 0.3841 0.3768 0.092 Uiso 0.287(6) 1 calc PR A 2 H24E H 0.8748 0.2787 0.3362 0.092 Uiso 0.287(6) 1 calc PR A 2 H24F H 0.9149 0.2603 0.4100 0.092 Uiso 0.287(6) 1 calc PR A 2 C25 C 0.4128(2) 0.7831(2) 0.16715(14) 0.0458(6) Uani 1 1 d . . . H25A H 0.3188 0.7939 0.1655 0.069 Uiso 1 1 calc R . . H25B H 0.4574 0.8365 0.1360 0.069 Uiso 1 1 calc R . . H25C H 0.4395 0.7956 0.2111 0.069 Uiso 1 1 calc R . . C26 C 0.3858(2) 0.5536(2) 0.07299(11) 0.0405(5) Uani 1 1 d . . . H26A H 0.2922 0.5684 0.0728 0.061 Uiso 1 1 calc R . . H26B H 0.4010 0.4727 0.0788 0.061 Uiso 1 1 calc R . . H26C H 0.4276 0.5815 0.0316 0.061 Uiso 1 1 calc R . . Al' Al 1.01125(6) 1.12584(5) 0.14658(3) 0.02957(15) Uani 1 1 d . . . O1' O 1.03415(14) 1.04084(13) 0.21833(7) 0.0348(3) Uani 1 1 d . . . C1' C 0.95279(19) 0.98884(16) 0.26239(10) 0.0280(4) Uani 1 1 d . . . C2' C 0.9898(2) 0.95946(17) 0.32646(10) 0.0303(4) Uani 1 1 d . . . C3' C 0.8972(2) 0.90765(18) 0.36893(11) 0.0357(4) Uani 1 1 d . . . H3'A H 0.9219 0.8867 0.4117 0.043 Uiso 1 1 calc R . . C4' C 0.7704(2) 0.88413(18) 0.35340(10) 0.0349(4) Uani 1 1 d . B . C5' C 0.7385(2) 0.91209(16) 0.28980(10) 0.0296(4) Uani 1 1 d . . . H5'A H 0.6537 0.8967 0.2768 0.035 Uiso 1 1 calc R . . C6' C 0.82807(19) 0.96205(16) 0.24491(9) 0.0279(4) Uani 1 1 d . . . C7' C 0.79553(19) 0.98100(16) 0.17481(9) 0.0278(4) Uani 1 1 d . . . H7'A H 0.7039 0.9596 0.1707 0.033 Uiso 1 1 calc R . . H7'B H 0.8504 0.9306 0.1482 0.033 Uiso 1 1 calc R . . N8' N 0.81369(16) 1.09927(13) 0.14717(8) 0.0257(3) Uani 1 1 d . . . C9' C 0.7628(2) 1.10272(17) 0.08040(9) 0.0304(4) Uani 1 1 d . . . H9'A H 0.6696 1.0829 0.0841 0.037 Uiso 1 1 calc R . . H9'B H 0.8089 1.0452 0.0550 0.037 Uiso 1 1 calc R . . C10' C 0.7775(2) 1.21455(19) 0.04361(10) 0.0350(4) Uani 1 1 d . . . H10C H 0.7501 1.2094 -0.0014 0.042 Uiso 1 1 calc R . . H10D H 0.7229 1.2717 0.0652 0.042 Uiso 1 1 calc R . . O11' O 0.90942(16) 1.24428(14) 0.04305(9) 0.0461(4) Uani 1 1 d . . . C12' C 0.9361(3) 1.3507(2) 0.01235(14) 0.0478(6) Uani 1 1 d . . . H12D H 1.0289 1.3666 0.0137 0.072 Uiso 1 1 calc R . . H12E H 0.8857 1.4080 0.0351 0.072 Uiso 1 1 calc R . . H12F H 0.9120 1.3513 -0.0330 0.072 Uiso 1 1 calc R . . C13' C 0.74586(19) 1.18010(16) 0.19044(10) 0.0291(4) Uani 1 1 d . . . H13C H 0.7624 1.2565 0.1711 0.035 Uiso 1 1 calc R . . H13D H 0.7873 1.1747 0.2328 0.035 Uiso 1 1 calc R . . C14' C 0.6017(2) 1.16853(19) 0.20391(11) 0.0361(5) Uani 1 1 d . . . H14C H 0.5791 1.0884 0.2108 0.043 Uiso 1 1 calc R . . H14D H 0.5750 1.2067 0.2440 0.043 Uiso 1 1 calc R . . O15' O 0.53481(16) 1.21671(16) 0.15058(9) 0.0483(4) Uani 1 1 d . . . C16' C 0.4006(3) 1.2294(3) 0.16588(18) 0.0657(9) Uani 1 1 d . . . H16D H 0.3584 1.2628 0.1279 0.099 Uiso 1 1 calc R . . H16E H 0.3877 1.2783 0.2024 0.099 Uiso 1 1 calc R . . H16F H 0.3625 1.1560 0.1779 0.099 Uiso 1 1 calc R . . C17' C 1.1275(2) 0.98335(19) 0.34699(11) 0.0360(5) Uani 1 1 d . . . C18' C 1.1528(3) 1.1097(2) 0.34356(14) 0.0480(6) Uani 1 1 d . . . H18D H 1.0888 1.1466 0.3722 0.072 Uiso 1 1 calc R . . H18E H 1.1456 1.1397 0.2987 0.072 Uiso 1 1 calc R . . H18F H 1.2403 1.1235 0.3576 0.072 Uiso 1 1 calc R . . C19' C 1.2288(2) 0.9267(2) 0.30158(14) 0.0482(6) Uani 1 1 d . . . H19D H 1.2184 0.9547 0.2566 0.072 Uiso 1 1 calc R . . H19E H 1.2162 0.8455 0.3050 0.072 Uiso 1 1 calc R . . H19F H 1.3163 0.9441 0.3143 0.072 Uiso 1 1 calc R . . C20' C 1.1497(3) 0.9381(3) 0.41618(13) 0.0537(7) Uani 1 1 d . . . H20D H 1.0872 0.9727 0.4466 0.081 Uiso 1 1 calc R . . H20E H 1.2382 0.9557 0.4273 0.081 Uiso 1 1 calc R . . H20F H 1.1379 0.8567 0.4190 0.081 Uiso 1 1 calc R . . C21' C 0.6724(3) 0.8285(2) 0.40320(12) 0.0482(6) Uani 1 1 d D . . C22' C 0.7258(9) 0.7976(10) 0.4668(4) 0.079(3) Uani 0.486(10) 1 d PD B 1 H22G H 0.7923 0.7393 0.4614 0.119 Uiso 0.486(10) 1 calc PR B 1 H22H H 0.6559 0.7693 0.4972 0.119 Uiso 0.486(10) 1 calc PR B 1 H22I H 0.7647 0.8636 0.4841 0.119 Uiso 0.486(10) 1 calc PR B 1 C23' C 0.6030(10) 0.7387(8) 0.3751(3) 0.084(4) Uani 0.486(10) 1 d PD B 1 H23G H 0.6633 0.6770 0.3659 0.126 Uiso 0.486(10) 1 calc PR B 1 H23H H 0.5658 0.7670 0.3346 0.126 Uiso 0.486(10) 1 calc PR B 1 H23I H 0.5331 0.7117 0.4059 0.126 Uiso 0.486(10) 1 calc PR B 1 C24' C 0.5657(8) 0.9244(8) 0.4174(4) 0.084(3) Uani 0.486(10) 1 d PD B 1 H24G H 0.6054 0.9982 0.4088 0.125 Uiso 0.486(10) 1 calc PR B 1 H24H H 0.5335 0.9165 0.4630 0.125 Uiso 0.486(10) 1 calc PR B 1 H24I H 0.4933 0.9168 0.3890 0.125 Uiso 0.486(10) 1 calc PR B 1 C22B C 0.6872(9) 0.8666(9) 0.4701(3) 0.075(3) Uani 0.514(10) 1 d PD B 2 H22J H 0.7578 0.8245 0.4903 0.113 Uiso 0.514(10) 1 calc PR B 2 H22K H 0.6060 0.8536 0.4962 0.113 Uiso 0.514(10) 1 calc PR B 2 H22L H 0.7074 0.9466 0.4678 0.113 Uiso 0.514(10) 1 calc PR B 2 C23B C 0.7067(11) 0.6979(5) 0.4060(4) 0.095(4) Uani 0.514(10) 1 d PD B 2 H23J H 0.7983 0.6873 0.3924 0.143 Uiso 0.514(10) 1 calc PR B 2 H23K H 0.6521 0.6597 0.3767 0.143 Uiso 0.514(10) 1 calc PR B 2 H23L H 0.6907 0.6665 0.4506 0.143 Uiso 0.514(10) 1 calc PR B 2 C24B C 0.5358(6) 0.8392(10) 0.3848(4) 0.099(5) Uani 0.514(10) 1 d PD B 2 H24J H 0.5136 0.7753 0.3598 0.148 Uiso 0.514(10) 1 calc PR B 2 H24K H 0.5249 0.9088 0.3583 0.148 Uiso 0.514(10) 1 calc PR B 2 H24L H 0.4784 0.8407 0.4242 0.148 Uiso 0.514(10) 1 calc PR B 2 C25' C 1.0500(3) 1.2802(2) 0.16657(14) 0.0472(6) Uani 1 1 d . . . H25D H 1.1443 1.2901 0.1660 0.071 Uiso 1 1 calc R . . H25E H 1.0118 1.2954 0.2098 0.071 Uiso 1 1 calc R . . H25F H 1.0133 1.3321 0.1340 0.071 Uiso 1 1 calc R . . C26' C 1.1012(2) 1.0481(2) 0.07573(12) 0.0413(5) Uani 1 1 d . . . H26D H 1.1948 1.0615 0.0762 0.062 Uiso 1 1 calc R . . H26E H 1.0692 1.0764 0.0340 0.062 Uiso 1 1 calc R . . H26F H 1.0846 0.9676 0.0816 0.062 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Al 0.0293(3) 0.0290(3) 0.0282(3) -0.0003(2) -0.0017(2) 0.0020(2) O1 0.0315(7) 0.0394(8) 0.0303(7) 0.0052(6) -0.0008(6) 0.0002(6) C1 0.0303(9) 0.0245(8) 0.0287(9) -0.0008(7) -0.0015(7) -0.0019(7) C2 0.0321(9) 0.0272(9) 0.0280(9) -0.0011(7) 0.0020(7) -0.0048(7) C3 0.0390(11) 0.0342(10) 0.0278(10) 0.0018(8) 0.0033(8) -0.0020(8) C4 0.0404(11) 0.0309(10) 0.0274(10) 0.0031(8) -0.0009(8) 0.0019(8) C5 0.0331(10) 0.0284(9) 0.0284(9) -0.0006(7) 0.0006(7) 0.0031(7) C6 0.0352(10) 0.0228(8) 0.0250(9) 0.0005(7) 0.0005(7) -0.0013(7) C7 0.0314(9) 0.0221(8) 0.0280(9) -0.0006(7) 0.0018(7) 0.0022(7) N8 0.0314(8) 0.0210(7) 0.0233(7) 0.0001(6) 0.0021(6) -0.0015(6) C9 0.0350(10) 0.0338(10) 0.0226(9) -0.0005(7) 0.0024(7) 0.0026(8) C10 0.0339(10) 0.0397(11) 0.0306(10) 0.0067(8) 0.0009(8) 0.0002(9) O11 0.0351(8) 0.0386(9) 0.0696(12) 0.0164(8) 0.0006(8) 0.0013(7) C12 0.0443(13) 0.0412(12) 0.0517(15) 0.0086(11) -0.0100(11) 0.0015(10) C13 0.0337(10) 0.0247(9) 0.0280(9) -0.0034(7) 0.0002(7) -0.0006(7) C14 0.0380(11) 0.0332(10) 0.0379(11) -0.0018(9) -0.0065(9) -0.0031(8) O15 0.0310(8) 0.0577(11) 0.0496(10) -0.0013(8) -0.0028(7) -0.0083(7) C16 0.0328(13) 0.078(2) 0.079(2) -0.0129(17) -0.0101(13) -0.0066(13) C17 0.0310(10) 0.0370(11) 0.0346(11) -0.0038(8) 0.0053(8) -0.0051(8) C18 0.0402(12) 0.0413(12) 0.0512(14) -0.0065(10) 0.0073(10) 0.0028(10) C19 0.0352(11) 0.0505(14) 0.0471(14) -0.0047(11) 0.0025(10) -0.0144(10) C20 0.0446(13) 0.0634(17) 0.0392(13) 0.0025(11) 0.0105(10) -0.0032(12) C21 0.0463(13) 0.0574(15) 0.0301(11) 0.0070(10) -0.0027(9) 0.0108(11) C22 0.051(2) 0.100(4) 0.037(2) 0.023(2) -0.0034(16) 0.005(2) C23 0.115(5) 0.087(4) 0.049(3) -0.002(2) -0.025(3) 0.063(3) C24 0.055(3) 0.111(4) 0.054(3) 0.023(3) -0.020(2) -0.027(3) C25 0.0423(13) 0.0363(12) 0.0574(15) -0.0009(11) 0.0077(11) 0.0077(10) C26 0.0413(12) 0.0467(13) 0.0339(11) -0.0005(9) -0.0081(9) -0.0044(10) Al' 0.0283(3) 0.0297(3) 0.0306(3) -0.0015(2) -0.0002(2) -0.0025(2) O1' 0.0288(7) 0.0414(8) 0.0335(8) 0.0055(6) -0.0020(6) -0.0017(6) C1' 0.0297(9) 0.0240(9) 0.0297(9) 0.0015(7) -0.0005(7) 0.0015(7) C2' 0.0321(10) 0.0292(9) 0.0301(10) -0.0016(7) -0.0067(8) 0.0035(7) C3' 0.0423(12) 0.0359(11) 0.0292(10) 0.0013(8) -0.0072(8) 0.0003(9) C4' 0.0422(11) 0.0335(10) 0.0289(10) 0.0020(8) -0.0026(8) -0.0048(8) C5' 0.0321(10) 0.0268(9) 0.0298(10) 0.0012(7) -0.0036(7) -0.0040(7) C6' 0.0331(10) 0.0234(8) 0.0270(9) 0.0003(7) -0.0034(7) -0.0013(7) C7' 0.0315(9) 0.0242(8) 0.0278(9) -0.0015(7) -0.0029(7) -0.0033(7) N8' 0.0314(8) 0.0237(7) 0.0223(7) -0.0027(6) -0.0023(6) -0.0007(6) C9' 0.0356(10) 0.0326(10) 0.0235(9) -0.0014(7) -0.0044(7) -0.0021(8) C10' 0.0345(10) 0.0406(11) 0.0298(10) 0.0050(8) -0.0066(8) -0.0020(9) O11' 0.0353(8) 0.0368(8) 0.0650(12) 0.0135(8) -0.0062(8) -0.0037(7) C12' 0.0432(13) 0.0420(13) 0.0559(16) 0.0112(11) 0.0059(11) -0.0026(10) C13' 0.0325(10) 0.0255(9) 0.0294(9) -0.0038(7) -0.0014(7) 0.0012(7) C14' 0.0360(11) 0.0338(10) 0.0385(11) -0.0051(9) 0.0021(9) -0.0008(8) O15' 0.0311(8) 0.0636(11) 0.0505(10) -0.0062(8) -0.0049(7) 0.0107(8) C16' 0.0309(12) 0.088(2) 0.080(2) -0.0189(18) -0.0052(13) 0.0107(13) C17' 0.0348(11) 0.0389(11) 0.0351(11) -0.0030(9) -0.0098(8) 0.0046(9) C18' 0.0427(13) 0.0429(13) 0.0608(16) -0.0112(11) -0.0151(12) -0.0034(10) C19' 0.0363(12) 0.0564(15) 0.0530(15) -0.0077(12) -0.0101(11) 0.0141(11) C20' 0.0491(15) 0.0702(18) 0.0432(14) 0.0002(13) -0.0185(11) 0.0025(13) C21' 0.0530(14) 0.0601(16) 0.0307(11) 0.0077(11) -0.0020(10) -0.0183(12) C22' 0.076(6) 0.121(9) 0.037(4) 0.040(5) -0.010(3) -0.031(6) C23' 0.110(8) 0.097(7) 0.044(4) 0.011(4) 0.004(4) -0.071(6) C24' 0.061(5) 0.109(7) 0.073(5) 0.025(5) 0.035(4) 0.017(5) C22B 0.076(6) 0.105(7) 0.044(4) -0.006(4) 0.013(3) -0.036(5) C23B 0.164(10) 0.041(3) 0.074(6) 0.013(3) 0.048(6) -0.019(4) C24B 0.044(3) 0.166(12) 0.079(6) 0.061(7) -0.005(3) -0.031(5) C25' 0.0475(14) 0.0366(12) 0.0589(16) -0.0014(11) -0.0151(12) -0.0090(10) C26' 0.0408(12) 0.0454(13) 0.0368(12) -0.0033(10) 0.0063(9) 0.0040(10) _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 Al O1 1.7735(15) . ? Al C26 1.962(2) . ? Al C25 1.965(2) . ? Al N8 2.0652(17) . ? O1 C1 1.337(2) . ? C1 C6 1.403(3) . ? C1 C2 1.418(3) . ? C2 C3 1.396(3) . ? C2 C17 1.537(3) . ? C3 C4 1.394(3) . ? C4 C5 1.390(3) . ? C4 C21 1.539(3) . ? C5 C6 1.390(3) . ? C6 C7 1.503(3) . ? C7 N8 1.511(2) . ? N8 C13 1.495(2) . ? N8 C9 1.498(2) . ? C9 C10 1.512(3) . ? C10 O11 1.403(3) . ? O11 C12 1.399(3) . ? C13 C14 1.507(3) . ? C14 O15 1.419(3) . ? O15 C16 1.421(3) . ? C17 C20 1.524(3) . ? C17 C18 1.533(3) . ? C17 C19 1.536(3) . ? C21 C22A 1.445(9) . ? C21 C24A 1.449(8) . ? C21 C23 1.474(5) . ? C21 C22 1.513(4) . ? C21 C24 1.591(5) . ? C21 C23A 1.626(9) . ? Al' O1' 1.7752(16) . ? Al' C26' 1.961(2) . ? Al' C25' 1.961(2) . ? Al' N8' 2.0641(17) . ? O1' C1' 1.336(2) . ? C1' C6' 1.398(3) . ? C1' C2' 1.419(3) . ? C2' C3' 1.388(3) . ? C2' C17' 1.536(3) . ? C3' C4' 1.397(3) . ? C4' C5' 1.391(3) . ? C4' C21' 1.532(3) . ? C5' C6' 1.388(3) . ? C6' C7' 1.506(3) . ? C7' N8' 1.506(2) . ? N8' C13' 1.494(3) . ? N8' C9' 1.497(2) . ? C9' C10' 1.507(3) . ? C10' O11' 1.408(3) . ? O11' C12' 1.414(3) . ? C13' C14' 1.504(3) . ? C14' O15' 1.422(3) . ? O15' C16' 1.412(3) . ? C17' C20' 1.527(3) . ? C17' C18' 1.533(3) . ? C17' C19' 1.542(3) . ? C21' C23' 1.459(6) . ? C21' C22' 1.476(6) . ? C21' C24B 1.481(6) . ? C21' C22B 1.490(7) . ? C21' C23B 1.598(6) . ? C21' C24' 1.610(7) . ? 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 O1 Al C26 104.61(9) . . ? O1 Al C25 106.65(10) . . ? C26 Al C25 123.96(12) . . ? O1 Al N8 94.45(7) . . ? C26 Al N8 111.13(9) . . ? C25 Al N8 111.40(9) . . ? C1 O1 Al 133.94(13) . . ? O1 C1 C6 118.79(17) . . ? O1 C1 C2 121.65(18) . . ? C6 C1 C2 119.55(18) . . ? C3 C2 C1 116.98(19) . . ? C3 C2 C17 122.14(18) . . ? C1 C2 C17 120.88(18) . . ? C4 C3 C2 124.42(19) . . ? C5 C4 C3 116.98(19) . . ? C5 C4 C21 121.0(2) . . ? C3 C4 C21 121.99(19) . . ? C4 C5 C6 121.21(19) . . ? C5 C6 C1 120.80(18) . . ? C5 C6 C7 120.55(18) . . ? C1 C6 C7 118.49(17) . . ? C6 C7 N8 114.69(15) . . ? C13 N8 C9 112.96(15) . . ? C13 N8 C7 110.70(15) . . ? C9 N8 C7 105.87(14) . . ? C13 N8 Al 109.16(12) . . ? C9 N8 Al 112.81(12) . . ? C7 N8 Al 105.02(11) . . ? N8 C9 C10 113.69(17) . . ? O11 C10 C9 107.52(17) . . ? C12 O11 C10 114.09(18) . . ? N8 C13 C14 118.32(17) . . ? O15 C14 C13 109.73(18) . . ? C14 O15 C16 112.0(2) . . ? C20 C17 C18 108.0(2) . . ? C20 C17 C19 107.20(19) . . ? C18 C17 C19 109.6(2) . . ? C20 C17 C2 112.24(19) . . ? C18 C17 C2 109.47(17) . . ? C19 C17 C2 110.22(18) . . ? C22A C21 C24A 115.9(6) . . ? C22A C21 C23 135.3(6) . . ? C24A C21 C23 53.9(5) . . ? C22A C21 C22 36.7(5) . . ? C24A C21 C22 132.5(5) . . ? C23 C21 C22 112.4(3) . . ? C22A C21 C4 111.0(5) . . ? C24A C21 C4 113.8(5) . . ? C23 C21 C4 112.2(2) . . ? C22 C21 C4 113.1(2) . . ? C22A C21 C24 69.3(5) . . ? C24A C21 C24 55.0(5) . . ? C23 C21 C24 107.3(4) . . ? C22 C21 C24 103.6(3) . . ? C4 C21 C24 107.5(2) . . ? C22A C21 C23A 106.7(6) . . ? C24A C21 C23A 104.9(6) . . ? C23 C21 C23A 52.0(5) . . ? C22 C21 C23A 70.7(5) . . ? C4 C21 C23A 103.3(5) . . ? C24 C21 C23A 148.1(5) . . ? O1' Al' C26' 105.76(10) . . ? O1' Al' C25' 106.94(10) . . ? C26' Al' C25' 123.25(12) . . ? O1' Al' N8' 94.81(7) . . ? C26' Al' N8' 110.51(9) . . ? C25' Al' N8' 111.44(10) . . ? C1' O1' Al' 133.49(13) . . ? O1' C1' C6' 119.21(18) . . ? O1' C1' C2' 121.76(18) . . ? C6' C1' C2' 119.04(18) . . ? C3' C2' C1' 117.28(18) . . ? C3' C2' C17' 121.93(19) . . ? C1' C2' C17' 120.79(19) . . ? C2' C3' C4' 124.7(2) . . ? C5' C4' C3' 116.34(19) . . ? C5' C4' C21' 121.7(2) . . ? C3' C4' C21' 121.9(2) . . ? C6' C5' C4' 121.34(19) . . ? C5' C6' C1' 121.20(18) . . ? C5' C6' C7' 120.22(17) . . ? C1' C6' C7' 118.44(17) . . ? C6' C7' N8' 115.00(15) . . ? C13' N8' C9' 112.81(15) . . ? C13' N8' C7' 110.52(15) . . ? C9' N8' C7' 106.39(14) . . ? C13' N8' Al' 108.98(11) . . ? C9' N8' Al' 113.06(12) . . ? C7' N8' Al' 104.75(11) . . ? N8' C9' C10' 114.20(16) . . ? O11' C10' C9' 107.46(17) . . ? C10' O11' C12' 113.41(18) . . ? N8' C13' C14' 118.42(16) . . ? O15' C14' C13' 109.85(18) . . ? C16' O15' C14' 112.2(2) . . ? C20' C17' C18' 108.0(2) . . ? C20' C17' C2' 112.3(2) . . ? C18' C17' C2' 110.52(18) . . ? C20' C17' C19' 107.1(2) . . ? C18' C17' C19' 108.7(2) . . ? C2' C17' C19' 110.07(18) . . ? C23' C21' C22' 114.3(5) . . ? C23' C21' C24B 56.9(5) . . ? C22' C21' C24B 130.0(5) . . ? C23' C21' C22B 135.5(4) . . ? C22' C21' C22B 36.0(4) . . ? C24B C21' C22B 111.0(5) . . ? C23' C21' C4' 111.3(3) . . ? C22' C21' C4' 114.3(4) . . ? C24B C21' C4' 113.9(3) . . ? C22B C21' C4' 112.3(4) . . ? C23' C21' C23B 52.1(5) . . ? C22' C21' C23B 71.3(5) . . ? C24B C21' C23B 106.7(5) . . ? C22B C21' C23B 106.2(5) . . ? C4' C21' C23B 106.2(3) . . ? C23' C21' C24' 105.8(5) . . ? C22' C21' C24' 105.4(5) . . ? C24B C21' C24' 49.4(5) . . ? C22B C21' C24' 71.3(5) . . ? C4' C21' C24' 104.6(3) . . ? C23B C21' C24' 147.3(4) . . ? _diffrn_measured_fraction_theta_max 0.896 _diffrn_reflns_theta_full 32.72 _diffrn_measured_fraction_theta_full 0.896 _refine_diff_density_max 0.449 _refine_diff_density_min -0.376 _refine_diff_density_rms 0.061 #===END data_Compound_7a _database_code_depnum_ccdc_archive 'CCDC 293282' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C29 H55 N3 O Zn' _chemical_formula_weight 527.13 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' Zn Zn 0.2839 1.4301 '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 14.7846(16) _cell_length_b 15.365(2) _cell_length_c 17.136(2) _cell_angle_alpha 67.774(13) _cell_angle_beta 72.413(10) _cell_angle_gamma 71.161(12) _cell_volume 3337.8(8) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 4.1273 _cell_measurement_theta_max 32.6685 _exptl_crystal_description blocks _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.33 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.049 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1152 _exptl_absorpt_coefficient_mu 0.757 _exptl_absorpt_correction_type 'numeric analytical' _exptl_absorpt_correction_T_min 0.76295 _exptl_absorpt_correction_T_max 0.81570 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'OD Xcalibur 3' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 15.9863 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 35768 _diffrn_reflns_av_R_equivalents 0.0209 _diffrn_reflns_av_sigmaI/netI 0.0401 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 4.14 _diffrn_reflns_theta_max 32.74 _reflns_number_total 22006 _reflns_number_gt 12530 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd' _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^)+(0.1814P)^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 22006 _refine_ls_number_parameters 663 _refine_ls_number_restraints 624 _refine_ls_R_factor_all 0.1112 _refine_ls_R_factor_gt 0.0812 _refine_ls_wR_factor_ref 0.2795 _refine_ls_wR_factor_gt 0.2410 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.106 _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 Zn Zn 0.53476(2) 0.82705(2) 0.705637(19) 0.04221(12) Uani 1 1 d . . . O1 O 0.58114(14) 0.93938(14) 0.62164(13) 0.0483(4) Uani 1 1 d . . . C1 C 0.6628(2) 0.9130(2) 0.56769(16) 0.0417(5) Uani 1 1 d . . . C2 C 0.7501(2) 0.9401(2) 0.5563(2) 0.0518(7) Uani 1 1 d . . . C3 C 0.8314(2) 0.9091(3) 0.4977(2) 0.0592(8) Uani 1 1 d . . . H3A H 0.8896 0.9278 0.4897 0.071 Uiso 1 1 calc R . . C4 C 0.8327(2) 0.8525(3) 0.45021(19) 0.0594(8) Uani 1 1 d . . . C5 C 0.7466(2) 0.8281(2) 0.46171(18) 0.0525(7) Uani 1 1 d . . . H5A H 0.7447 0.7898 0.4301 0.063 Uiso 1 1 calc R . . C6 C 0.6628(2) 0.8579(2) 0.51801(17) 0.0450(6) Uani 1 1 d . . . C7 C 0.5675(2) 0.8376(3) 0.52347(17) 0.0525(7) Uani 1 1 d . . . H7A H 0.5181 0.8997 0.5106 0.063 Uiso 1 1 calc R . . H7B H 0.5766 0.8074 0.4790 0.063 Uiso 1 1 calc R . . N8 N 0.52987(17) 0.77297(19) 0.60921(14) 0.0475(5) Uani 1 1 d D A . C9 C 0.4238(3) 0.7811(4) 0.6193(2) 0.0725(12) Uani 1 1 d . . . H9A H 0.4049 0.7242 0.6664 0.087 Uiso 1 1 calc R . . H9B H 0.4124 0.7804 0.5656 0.087 Uiso 1 1 calc R . . C10 C 0.3607(3) 0.8717(4) 0.6391(3) 0.0825(14) Uani 1 1 d . . . H10A H 0.3731 0.9286 0.5887 0.099 Uiso 1 1 calc R . . H10B H 0.2912 0.8713 0.6500 0.099 Uiso 1 1 calc R . . N11 N 0.38036(18) 0.88020(19) 0.71535(18) 0.0582(7) Uani 1 1 d . . . C12 C 0.3326(3) 0.8176(3) 0.7972(2) 0.0667(9) Uani 1 1 d . . . H12A H 0.3587 0.8156 0.8449 0.080 Uiso 1 1 calc R . . H12B H 0.3511 0.7510 0.7939 0.080 Uiso 1 1 calc R . . C13 C 0.2210(3) 0.8492(3) 0.8195(3) 0.0921(14) Uani 1 1 d . . . H13A H 0.1962 0.8038 0.8741 0.138 Uiso 1 1 calc R . . H13B H 0.1939 0.8499 0.7736 0.138 Uiso 1 1 calc R . . H13C H 0.2015 0.9143 0.8252 0.138 Uiso 1 1 calc R . . C14 C 0.3526(3) 0.9823(3) 0.7080(3) 0.0929(14) Uani 1 1 d U . . H14A H 0.2813 1.0067 0.7111 0.111 Uiso 1 1 calc R . . H14B H 0.3861 1.0190 0.6514 0.111 Uiso 1 1 calc R . . C15 C 0.3794(5) 0.9984(4) 0.7793(4) 0.124(2) Uani 1 1 d U . . H15A H 0.3604 1.0677 0.7728 0.186 Uiso 1 1 calc R . . H15B H 0.4501 0.9748 0.7759 0.186 Uiso 1 1 calc R . . H15C H 0.3451 0.9632 0.8353 0.186 Uiso 1 1 calc R . . C16 C 0.5894(3) 0.6720(3) 0.6238(2) 0.0655(9) Uani 1 1 d D . . H16A H 0.6571 0.6760 0.6165 0.079 Uiso 0.507(6) 1 calc PR A 1 H16B H 0.5682 0.6381 0.6856 0.079 Uiso 0.507(6) 1 calc PR A 1 H16C H 0.5730 0.6331 0.6826 0.079 Uiso 0.493(6) 1 d PR A 2 H16D H 0.6579 0.6700 0.6087 0.079 Uiso 0.493(6) 1 d PR A 2 C17 C 0.5974(5) 0.6045(4) 0.5779(4) 0.0534(15) Uani 0.507(6) 1 d PDU A 1 H17A H 0.6060 0.6403 0.5155 0.064 Uiso 0.507(6) 1 calc PR A 1 H17B H 0.5345 0.5855 0.5958 0.064 Uiso 0.507(6) 1 calc PR A 1 N18 N 0.6779(7) 0.5134(5) 0.5903(6) 0.092(4) Uani 0.507(6) 1 d PDU A 1 C19 C 0.7687(7) 0.5397(7) 0.5265(7) 0.105(3) Uani 0.507(6) 1 d PDU A 1 H19A H 0.7640 0.5447 0.4684 0.127 Uiso 0.507(6) 1 calc PR A 1 H19B H 0.7717 0.6039 0.5245 0.127 Uiso 0.507(6) 1 calc PR A 1 C20 C 0.8589(8) 0.4691(10) 0.5478(9) 0.137(4) Uani 0.507(6) 1 d PDU A 1 H20A H 0.9150 0.4896 0.5042 0.206 Uiso 0.507(6) 1 calc PR A 1 H20B H 0.8569 0.4055 0.5489 0.206 Uiso 0.507(6) 1 calc PR A 1 H20C H 0.8650 0.4651 0.6045 0.206 Uiso 0.507(6) 1 calc PR A 1 C21 C 0.6498(10) 0.4429(7) 0.5676(8) 0.127(3) Uani 0.507(6) 1 d PDU A 1 H21A H 0.7080 0.4070 0.5357 0.152 Uiso 0.507(6) 1 calc PR A 1 H21B H 0.6015 0.4775 0.5301 0.152 Uiso 0.507(6) 1 calc PR A 1 C22 C 0.6056(13) 0.3717(10) 0.6502(9) 0.161(5) Uani 0.507(6) 1 d PDU A 1 H22A H 0.5866 0.3255 0.6352 0.242 Uiso 0.507(6) 1 calc PR A 1 H22B H 0.5480 0.4074 0.6815 0.242 Uiso 0.507(6) 1 calc PR A 1 H22C H 0.6541 0.3366 0.6867 0.242 Uiso 0.507(6) 1 calc PR A 1 C17A C 0.5606(5) 0.6368(6) 0.5571(5) 0.0590(18) Uiso 0.493(6) 1 d PDU A 2 H17C H 0.5153 0.5935 0.5881 0.071 Uiso 0.493(6) 1 calc PR A 2 H17D H 0.5304 0.6929 0.5127 0.071 Uiso 0.493(6) 1 calc PR A 2 N18A N 0.6554(5) 0.5852(5) 0.5187(5) 0.084(2) Uiso 0.493(6) 1 d PDU A 2 C19A C 0.6466(10) 0.5580(8) 0.4480(6) 0.117(3) Uiso 0.493(6) 1 d PDU A 2 H19C H 0.5870 0.5334 0.4655 0.140 Uiso 0.493(6) 1 calc PR A 2 H19D H 0.7035 0.5053 0.4368 0.140 Uiso 0.493(6) 1 calc PR A 2 C20A C 0.6413(12) 0.6466(10) 0.3626(7) 0.133(4) Uiso 0.493(6) 1 d PDU A 2 H20D H 0.6350 0.6261 0.3172 0.200 Uiso 0.493(6) 1 calc PR A 2 H20E H 0.7010 0.6701 0.3442 0.200 Uiso 0.493(6) 1 calc PR A 2 H20F H 0.5846 0.6987 0.3732 0.200 Uiso 0.493(6) 1 calc PR A 2 C21A C 0.6816(10) 0.4948(10) 0.5904(9) 0.113(5) Uiso 0.493(6) 1 d PDU A 2 H21C H 0.6376 0.4523 0.6030 0.136 Uiso 0.493(6) 1 calc PR A 2 H21D H 0.6731 0.5114 0.6431 0.136 Uiso 0.493(6) 1 calc PR A 2 C22A C 0.7860(11) 0.4423(12) 0.5657(12) 0.164(6) Uiso 0.493(6) 1 d PDU A 2 H22D H 0.8022 0.3830 0.6129 0.245 Uiso 0.493(6) 1 calc PR A 2 H22E H 0.8295 0.4841 0.5545 0.245 Uiso 0.493(6) 1 calc PR A 2 H22F H 0.7941 0.4257 0.5137 0.245 Uiso 0.493(6) 1 calc PR A 2 C23 C 0.7543(3) 1.0014(2) 0.6073(2) 0.0599(8) Uani 1 1 d . . . C24 C 0.7301(3) 0.9483(3) 0.7033(2) 0.0725(11) Uani 1 1 d . . . H24A H 0.6656 0.9346 0.7182 0.109 Uiso 1 1 calc R . . H24B H 0.7297 0.9888 0.7360 0.109 Uiso 1 1 calc R . . H24C H 0.7794 0.8874 0.7175 0.109 Uiso 1 1 calc R . . C25 C 0.6816(4) 1.0978(3) 0.5857(3) 0.0883(14) Uani 1 1 d . . . H25A H 0.6159 1.0872 0.5997 0.132 Uiso 1 1 calc R . . H25B H 0.6985 1.1324 0.5242 0.132 Uiso 1 1 calc R . . H25C H 0.6833 1.1364 0.6194 0.132 Uiso 1 1 calc R . . C26 C 0.8555(4) 1.0226(4) 0.5848(4) 0.1051(17) Uani 1 1 d . . . H26A H 0.9049 0.9615 0.5972 0.158 Uiso 1 1 calc R . . H26B H 0.8555 1.0608 0.6195 0.158 Uiso 1 1 calc R . . H26C H 0.8706 1.0590 0.5235 0.158 Uiso 1 1 calc R . . C27 C 0.9269(3) 0.8224(4) 0.3877(2) 0.0818(12) Uani 1 1 d . . . C28 C 1.0107(3) 0.7739(5) 0.4361(4) 0.1070(17) Uani 1 1 d . . . H28A H 0.9979 0.7141 0.4809 0.160 Uiso 1 1 calc R . . H28B H 1.0161 0.8178 0.4628 0.160 Uiso 1 1 calc R . . H28C H 1.0719 0.7587 0.3957 0.160 Uiso 1 1 calc R . . C29 C 0.9541(4) 0.9164(5) 0.3189(3) 0.117(2) Uani 1 1 d . . . H29A H 0.9026 0.9515 0.2856 0.175 Uiso 1 1 calc R . . H29B H 1.0161 0.8991 0.2801 0.175 Uiso 1 1 calc R . . H29C H 0.9607 0.9575 0.3478 0.175 Uiso 1 1 calc R . . C30 C 0.9152(4) 0.7614(6) 0.3447(4) 0.127(2) Uani 1 1 d U . . H30A H 0.8980 0.7025 0.3880 0.191 Uiso 1 1 calc R . . H30B H 0.9765 0.7440 0.3053 0.191 Uiso 1 1 calc R . . H30C H 0.8631 0.7971 0.3121 0.191 Uiso 1 1 calc R . . C31 C 0.5833(4) 0.7411(4) 0.8107(3) 0.0979(16) Uani 1 1 d U . . H31A H 0.5539 0.6845 0.8342 0.117 Uiso 1 1 calc R . . H31B H 0.6547 0.7168 0.7941 0.117 Uiso 1 1 calc R . . C32 C 0.5641(6) 0.7834(6) 0.8818(4) 0.132(2) Uani 1 1 d U . . H32A H 0.5914 0.7340 0.9304 0.198 Uiso 1 1 calc R . . H32B H 0.4935 0.8059 0.9007 0.198 Uiso 1 1 calc R . . H32C H 0.5948 0.8381 0.8606 0.198 Uiso 1 1 calc R . . Zn' Zn 0.93415(3) 0.34204(2) 0.21767(2) 0.05366(13) Uani 1 1 d . . . O1' O 0.87242(15) 0.45266(14) 0.13210(14) 0.0523(5) Uani 1 1 d . . . C1' C 0.8452(2) 0.4250(2) 0.07983(19) 0.0523(7) Uani 1 1 d . . . C2' C 0.7464(2) 0.4504(2) 0.0709(2) 0.0573(8) Uani 1 1 d . . . C3' C 0.7249(2) 0.4181(3) 0.0144(2) 0.0654(9) Uani 1 1 d . . . H3'A H 0.6588 0.4347 0.0092 0.078 Uiso 1 1 calc R . . C4' C 0.7949(3) 0.3623(3) -0.0356(2) 0.0647(9) Uani 1 1 d . . . C5' C 0.8904(2) 0.3375(2) -0.0243(2) 0.0607(8) Uani 1 1 d . . . H5'A H 0.9396 0.2984 -0.0555 0.073 Uiso 1 1 calc R . . C6' C 0.9166(2) 0.3680(2) 0.03126(18) 0.0506(7) Uani 1 1 d . . . C7' C 1.0221(2) 0.3478(2) 0.03514(18) 0.0593(8) Uani 1 1 d . . . H7'A H 1.0635 0.3158 -0.0084 0.071 Uiso 1 1 calc R . . H7'B H 1.0397 0.4100 0.0200 0.071 Uiso 1 1 calc R . . N8' N 1.0439(2) 0.2849(2) 0.12220(15) 0.0616(7) Uani 1 1 d D B . C9' C 1.1352(3) 0.2944(3) 0.1318(2) 0.0846(14) Uani 1 1 d . . . H9'A H 1.1852 0.2922 0.0786 0.101 Uiso 1 1 calc R . . H9'B H 1.1590 0.2387 0.1799 0.101 Uiso 1 1 calc R . . C10' C 1.1242(3) 0.3853(3) 0.1490(2) 0.0715(11) Uani 1 1 d . . . H10C H 1.1087 0.4410 0.0979 0.086 Uiso 1 1 calc R . . H10D H 1.1868 0.3857 0.1586 0.086 Uiso 1 1 calc R . . N11' N 1.0452(2) 0.3967(2) 0.22613(16) 0.0594(7) Uani 1 1 d . . . C12' C 1.0789(3) 0.3345(3) 0.3092(2) 0.0738(11) Uani 1 1 d . . . H12C H 1.1049 0.2672 0.3073 0.089 Uiso 1 1 calc R . . H12D H 1.0212 0.3349 0.3571 0.089 Uiso 1 1 calc R . . C13' C 1.1556(4) 0.3631(5) 0.3299(3) 0.1115(19) Uani 1 1 d U . . H13D H 1.1720 0.3178 0.3847 0.167 Uiso 1 1 calc R . . H13E H 1.1302 0.4287 0.3343 0.167 Uiso 1 1 calc R . . H13F H 1.2142 0.3612 0.2840 0.167 Uiso 1 1 calc R . . C14' C 1.0081(3) 0.5005(3) 0.2208(3) 0.0700(9) Uani 1 1 d . . . H14C H 0.9886 0.5377 0.1646 0.084 Uiso 1 1 calc R . . H14D H 1.0615 0.5246 0.2229 0.084 Uiso 1 1 calc R . . C15' C 0.9227(4) 0.5184(3) 0.2916(3) 0.0811(11) Uani 1 1 d . . . H15D H 0.9014 0.5878 0.2845 0.122 Uiso 1 1 calc R . . H15E H 0.9420 0.4832 0.3474 0.122 Uiso 1 1 calc R . . H15F H 0.8690 0.4958 0.2893 0.122 Uiso 1 1 calc R . . C16' C 1.0427(4) 0.1832(3) 0.1400(2) 0.0856(15) Uani 1 1 d D . . H16E H 1.0294 0.1554 0.2035 0.103 Uiso 0.593(6) 1 calc PR B 1 H16F H 0.9837 0.1868 0.1218 0.103 Uiso 0.593(6) 1 calc PR B 1 H16G H 0.9899 0.1810 0.1196 0.103 Uiso 0.407(6) 1 d PR B 2 H16H H 1.0358 0.1482 0.2004 0.103 Uiso 0.407(6) 1 d PR B 2 C17' C 1.1195(6) 0.1082(5) 0.1086(4) 0.078(2) Uani 0.593(6) 1 d PDU B 1 H17E H 1.1769 0.0938 0.1335 0.093 Uiso 0.593(6) 1 calc PR B 1 H17F H 1.0955 0.0484 0.1303 0.093 Uiso 0.593(6) 1 calc PR B 1 N18' N 1.1509(6) 0.1326(5) 0.0155(4) 0.095(3) Uani 0.593(6) 1 d PDU B 1 C19' C 1.0846(6) 0.0984(7) -0.0158(5) 0.110(3) Uani 0.593(6) 1 d PDU B 1 H19E H 1.0998 0.0269 0.0020 0.132 Uiso 0.593(6) 1 calc PR B 1 H19F H 1.0150 0.1224 0.0082 0.132 Uiso 0.593(6) 1 calc PR B 1 C20' C 1.1066(11) 0.1411(11) -0.1151(6) 0.168(5) Uani 0.593(6) 1 d PDU B 1 H20G H 1.0663 0.1220 -0.1390 0.253 Uiso 0.593(6) 1 calc PR B 1 H20H H 1.1758 0.1166 -0.1377 0.253 Uiso 0.593(6) 1 calc PR B 1 H20I H 1.0917 0.2119 -0.1315 0.253 Uiso 0.593(6) 1 calc PR B 1 C21' C 1.2514(7) 0.0771(9) -0.0096(8) 0.142(4) Uani 0.593(6) 1 d PDU B 1 H21E H 1.2658 0.0866 -0.0722 0.171 Uiso 0.593(6) 1 calc PR B 1 H21F H 1.2555 0.0074 0.0211 0.171 Uiso 0.593(6) 1 calc PR B 1 C22' C 1.3285(8) 0.1078(11) 0.0108(11) 0.175(5) Uani 0.593(6) 1 d PDU B 1 H22G H 1.3936 0.0695 -0.0073 0.263 Uiso 0.593(6) 1 calc PR B 1 H22H H 1.3157 0.0968 0.0729 0.263 Uiso 0.593(6) 1 calc PR B 1 H22I H 1.3255 0.1766 -0.0201 0.263 Uiso 0.593(6) 1 calc PR B 1 C17B C 1.1464(7) 0.1428(8) 0.0803(8) 0.078(3) Uiso 0.407(6) 1 d PDU B 2 H17G H 1.1832 0.1939 0.0489 0.094 Uiso 0.407(6) 1 calc PR B 2 H17H H 1.1875 0.0862 0.1160 0.094 Uiso 0.407(6) 1 calc PR B 2 N18B N 1.1171(10) 0.1162(10) 0.0218(7) 0.105(5) Uiso 0.407(6) 1 d PDU B 2 C19B C 1.0881(14) 0.0203(12) 0.0773(10) 0.162(5) Uiso 0.407(6) 1 d PDU B 2 H19G H 1.1452 -0.0343 0.0720 0.195 Uiso 0.407(6) 1 calc PR B 2 H19H H 1.0679 0.0181 0.1385 0.195 Uiso 0.407(6) 1 calc PR B 2 C20B C 1.0065(14) 0.0093(15) 0.0506(14) 0.164(5) Uiso 0.407(6) 1 d PDU . 2 H20J H 0.9916 -0.0536 0.0853 0.246 Uiso 0.407(6) 1 calc PR B 2 H20K H 1.0256 0.0133 -0.0104 0.246 Uiso 0.407(6) 1 calc PR B 2 H20L H 0.9485 0.0610 0.0592 0.246 Uiso 0.407(6) 1 calc PR B 2 C21B C 1.1861(12) 0.1086(10) -0.0556(7) 0.120(4) Uiso 0.407(6) 1 d PDU B 2 H21G H 1.1756 0.0583 -0.0724 0.143 Uiso 0.407(6) 1 calc PR B 2 H21H H 1.2523 0.0855 -0.0427 0.143 Uiso 0.407(6) 1 calc PR B 2 C22B C 1.1842(11) 0.2005(9) -0.1330(8) 0.104(4) Uiso 0.407(6) 1 d PDU B 2 H22J H 1.2369 0.1875 -0.1810 0.156 Uiso 0.407(6) 1 calc PR B 2 H22K H 1.1931 0.2518 -0.1173 0.156 Uiso 0.407(6) 1 calc PR B 2 H22L H 1.1212 0.2212 -0.1503 0.156 Uiso 0.407(6) 1 calc PR B 2 C23' C 0.6668(2) 0.5131(3) 0.1218(3) 0.0650(9) Uani 1 1 d . . . C24' C 0.6646(4) 0.4639(3) 0.2196(3) 0.0953(16) Uani 1 1 d . . . H24D H 0.7295 0.4517 0.2306 0.143 Uiso 1 1 calc R . . H24E H 0.6457 0.4024 0.2384 0.143 Uiso 1 1 calc R . . H24F H 0.6171 0.5064 0.2515 0.143 Uiso 1 1 calc R . . C25' C 0.6903(3) 0.6113(3) 0.0970(3) 0.0710(10) Uani 1 1 d . . . H25D H 0.7548 0.6014 0.1080 0.107 Uiso 1 1 calc R . . H25E H 0.6408 0.6500 0.1313 0.107 Uiso 1 1 calc R . . H25F H 0.6905 0.6452 0.0357 0.107 Uiso 1 1 calc R . . C26' C 0.5654(3) 0.5310(4) 0.1049(4) 0.111(2) Uani 1 1 d . . . H26D H 0.5667 0.5614 0.0431 0.167 Uiso 1 1 calc R . . H26E H 0.5178 0.5739 0.1364 0.167 Uiso 1 1 calc R . . H26F H 0.5469 0.4692 0.1245 0.167 Uiso 1 1 calc R . . C27' C 0.7641(3) 0.3310(4) -0.0936(3) 0.0898(14) Uani 1 1 d . . . C28' C 0.6896(5) 0.2673(5) -0.0430(4) 0.126(2) Uani 1 1 d U . . H28D H 0.6327 0.3032 -0.0112 0.189 Uiso 1 1 calc R . . H28E H 0.7202 0.2082 -0.0024 0.189 Uiso 1 1 calc R . . H28F H 0.6688 0.2502 -0.0834 0.189 Uiso 1 1 calc R . . C29' C 0.7134(4) 0.4231(5) -0.1610(3) 0.1062(18) Uani 1 1 d . . . H29D H 0.6577 0.4613 -0.1303 0.159 Uiso 1 1 calc R . . H29E H 0.6907 0.4024 -0.1979 0.159 Uiso 1 1 calc R . . H29F H 0.7605 0.4625 -0.1966 0.159 Uiso 1 1 calc R . . C30' C 0.8499(4) 0.2742(5) -0.1454(4) 0.1124(19) Uani 1 1 d . . . H30D H 0.8958 0.3148 -0.1812 0.169 Uiso 1 1 calc R . . H30E H 0.8255 0.2552 -0.1823 0.169 Uiso 1 1 calc R . . H30F H 0.8833 0.2161 -0.1057 0.169 Uiso 1 1 calc R . . C31' C 0.8688(4) 0.2565(3) 0.3247(2) 0.0846(14) Uani 1 1 d . . . H31C H 0.8244 0.2325 0.3089 0.102 Uiso 1 1 calc R . . H31D H 0.9194 0.1996 0.3483 0.102 Uiso 1 1 calc R . . C32' C 0.8107(4) 0.3007(3) 0.3956(3) 0.0950(16) Uani 1 1 d . . . H32D H 0.7819 0.2522 0.4447 0.143 Uiso 1 1 calc R . . H32E H 0.7587 0.3559 0.3741 0.143 Uiso 1 1 calc R . . H32F H 0.8540 0.3227 0.4138 0.143 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn 0.03945(18) 0.0457(2) 0.03597(17) -0.01142(13) -0.00837(12) -0.00387(13) O1 0.0423(10) 0.0491(10) 0.0526(11) -0.0129(9) -0.0121(9) -0.0110(8) C1 0.0419(13) 0.0453(13) 0.0352(11) -0.0023(10) -0.0106(10) -0.0166(11) C2 0.0494(15) 0.0598(16) 0.0475(14) -0.0026(13) -0.0182(12) -0.0239(13) C3 0.0484(16) 0.078(2) 0.0493(16) -0.0021(15) -0.0112(13) -0.0328(15) C4 0.0493(16) 0.086(2) 0.0387(14) -0.0074(15) -0.0027(12) -0.0304(16) C5 0.0548(16) 0.0694(19) 0.0335(12) -0.0101(12) -0.0023(11) -0.0283(15) C6 0.0418(13) 0.0613(16) 0.0327(11) -0.0049(11) -0.0063(10) -0.0261(12) C7 0.0521(16) 0.079(2) 0.0330(12) -0.0115(13) -0.0027(11) -0.0361(15) N8 0.0466(12) 0.0656(15) 0.0360(10) -0.0143(10) 0.0002(9) -0.0305(11) C9 0.063(2) 0.124(3) 0.0409(15) -0.0076(18) -0.0053(14) -0.061(2) C10 0.0382(16) 0.114(3) 0.059(2) 0.019(2) -0.0153(15) -0.0216(19) N11 0.0398(12) 0.0501(13) 0.0545(14) 0.0008(11) 0.0001(11) -0.0009(10) C12 0.0580(19) 0.0593(18) 0.0518(17) -0.0054(15) 0.0134(14) -0.0109(15) C13 0.057(2) 0.083(3) 0.099(3) -0.018(2) 0.025(2) -0.020(2) C14 0.0534(19) 0.0580(19) 0.109(3) -0.002(2) 0.017(2) 0.0023(15) C15 0.121(4) 0.078(3) 0.136(5) -0.056(3) 0.045(4) -0.015(3) C16 0.080(2) 0.065(2) 0.0573(18) -0.0293(16) 0.0144(16) -0.0394(18) C17 0.057(4) 0.050(3) 0.056(3) -0.021(3) -0.017(3) -0.004(3) N18 0.141(8) 0.050(4) 0.091(6) -0.046(4) -0.025(5) 0.001(4) C19 0.133(7) 0.094(6) 0.097(6) -0.042(5) -0.011(6) -0.035(6) C20 0.137(9) 0.149(9) 0.141(9) -0.085(8) 0.027(8) -0.056(8) C21 0.180(8) 0.082(5) 0.134(7) -0.058(5) -0.011(7) -0.044(6) C22 0.182(11) 0.166(10) 0.163(10) -0.099(8) 0.014(9) -0.065(9) C23 0.068(2) 0.0509(16) 0.071(2) -0.0116(15) -0.0343(17) -0.0172(15) C24 0.104(3) 0.0563(19) 0.066(2) -0.0190(17) -0.048(2) -0.0030(19) C25 0.115(4) 0.0452(18) 0.122(4) -0.004(2) -0.070(3) -0.024(2) C26 0.088(3) 0.131(4) 0.137(5) -0.057(4) -0.028(3) -0.056(3) C27 0.054(2) 0.131(4) 0.0480(18) -0.016(2) 0.0052(15) -0.034(2) C28 0.060(2) 0.149(5) 0.100(4) -0.044(4) 0.001(2) -0.019(3) C29 0.083(3) 0.167(6) 0.069(3) -0.003(3) 0.015(2) -0.059(4) C30 0.087(3) 0.211(7) 0.115(4) -0.112(5) 0.042(3) -0.062(4) C31 0.133(4) 0.087(3) 0.074(3) 0.004(2) -0.070(3) -0.016(3) C32 0.161(6) 0.182(6) 0.074(3) -0.010(4) -0.036(4) -0.092(5) Zn' 0.0592(2) 0.0429(2) 0.03619(18) -0.00511(14) 0.00726(15) -0.00717(15) O1' 0.0477(11) 0.0425(10) 0.0501(11) -0.0090(9) -0.0008(9) -0.0041(8) C1' 0.0458(14) 0.0401(13) 0.0441(14) 0.0011(11) 0.0063(11) -0.0070(11) C2' 0.0454(15) 0.0484(16) 0.0593(18) -0.0124(14) 0.0107(13) -0.0122(12) C3' 0.0437(16) 0.067(2) 0.070(2) -0.0199(17) 0.0123(15) -0.0170(14) C4' 0.0559(18) 0.072(2) 0.0576(18) -0.0211(17) 0.0151(15) -0.0271(16) C5' 0.0545(17) 0.0531(17) 0.0471(16) -0.0096(13) 0.0157(13) -0.0086(14) C6' 0.0476(15) 0.0448(14) 0.0347(12) -0.0019(11) 0.0036(11) -0.0027(11) C7' 0.0500(16) 0.0569(17) 0.0351(13) -0.0009(12) 0.0017(11) 0.0078(13) N8' 0.0565(15) 0.0558(14) 0.0329(11) -0.0009(10) -0.0001(10) 0.0141(12) C9' 0.0548(19) 0.100(3) 0.0400(16) 0.0006(18) -0.0035(14) 0.0249(19) C10' 0.0536(18) 0.082(2) 0.0404(15) 0.0118(16) -0.0062(13) -0.0067(17) N11' 0.0556(15) 0.0571(15) 0.0394(12) 0.0058(11) -0.0059(11) -0.0081(12) C12' 0.069(2) 0.076(2) 0.0401(15) 0.0040(16) -0.0075(15) -0.0011(18) C13' 0.082(3) 0.156(5) 0.064(2) 0.013(3) -0.031(2) -0.027(3) C14' 0.071(2) 0.059(2) 0.073(2) -0.0007(17) -0.0198(19) -0.0257(17) C15' 0.091(3) 0.064(2) 0.082(3) -0.026(2) -0.011(2) -0.013(2) C16' 0.124(4) 0.0547(19) 0.0368(15) -0.0119(14) -0.0105(19) 0.023(2) C17' 0.078(4) 0.069(4) 0.060(4) -0.019(3) -0.016(3) 0.016(4) N18' 0.120(7) 0.070(4) 0.056(3) -0.033(3) 0.015(4) 0.014(4) C19' 0.119(6) 0.130(6) 0.106(5) -0.076(5) -0.058(4) 0.019(5) C20' 0.166(9) 0.216(10) 0.093(6) -0.080(7) -0.029(6) 0.034(8) C21' 0.141(7) 0.129(7) 0.133(7) -0.053(6) -0.016(6) 0.002(6) C22' 0.149(9) 0.156(9) 0.188(10) -0.081(8) 0.031(8) -0.022(8) C23' 0.0422(15) 0.0577(18) 0.076(2) -0.0211(17) 0.0132(15) -0.0099(13) C24' 0.101(3) 0.062(2) 0.075(3) -0.0196(19) 0.046(2) -0.018(2) C25' 0.0512(18) 0.0518(18) 0.086(3) -0.0143(18) 0.0001(17) -0.0034(14) C26' 0.0383(18) 0.129(4) 0.177(6) -0.093(4) 0.018(3) -0.018(2) C27' 0.074(3) 0.123(4) 0.084(3) -0.052(3) 0.026(2) -0.055(3) C28' 0.119(4) 0.171(6) 0.116(4) -0.074(4) 0.044(3) -0.099(4) C29' 0.089(3) 0.173(6) 0.080(3) -0.046(4) 0.000(3) -0.068(4) C30' 0.102(4) 0.148(5) 0.111(4) -0.083(4) 0.026(3) -0.053(4) C31' 0.119(4) 0.059(2) 0.0532(19) -0.0124(17) 0.026(2) -0.038(2) C32' 0.124(4) 0.083(3) 0.060(2) -0.024(2) 0.037(2) -0.050(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 Zn O1 1.952(2) . ? Zn C31 1.967(4) . ? Zn N11 2.139(3) . ? Zn N8 2.139(2) . ? O1 C1 1.331(3) . ? C1 C6 1.410(4) . ? C1 C2 1.418(4) . ? C2 C3 1.393(5) . ? C2 C23 1.533(5) . ? C3 C4 1.389(5) . ? C4 C5 1.379(4) . ? C4 C27 1.535(5) . ? C5 C6 1.386(4) . ? C6 C7 1.508(4) . ? C7 N8 1.488(4) . ? N8 C16 1.483(5) . ? N8 C9 1.494(4) . ? C9 C10 1.500(7) . ? C10 N11 1.480(5) . ? N11 C14 1.453(5) . ? N11 C12 1.487(4) . ? C12 C13 1.532(5) . ? C14 C15 1.515(9) . ? C16 C17 1.480(6) . ? C16 C17A 1.640(7) . ? C17 N18 1.508(9) . ? N18 C21 1.485(10) . ? N18 C19 1.514(10) . ? C19 C20 1.466(12) . ? C21 C22 1.535(12) . ? C17A N18A 1.465(9) . ? N18A C19A 1.473(10) . ? N18A C21A 1.496(11) . ? C19A C20A 1.580(12) . ? C21A C22A 1.508(13) . ? C23 C25 1.512(5) . ? C23 C24 1.522(5) . ? C23 C26 1.538(6) . ? C27 C30 1.469(7) . ? C27 C28 1.529(7) . ? C27 C29 1.562(7) . ? C31 C32 1.503(8) . ? Zn' O1' 1.948(2) . ? Zn' C31' 1.987(3) . ? Zn' N11' 2.133(3) . ? Zn' N8' 2.155(2) . ? O1' C1' 1.326(4) . ? C1' C6' 1.413(4) . ? C1' C2' 1.426(5) . ? C2' C3' 1.391(5) . ? C2' C23' 1.535(5) . ? C3' C4' 1.411(5) . ? C4' C5' 1.392(5) . ? C4' C27' 1.484(6) . ? C5' C6' 1.397(5) . ? C6' C7' 1.507(5) . ? C7' N8' 1.504(4) . ? N8' C9' 1.468(6) . ? N8' C16' 1.480(5) . ? C9' C10' 1.482(7) . ? C10' N11' 1.500(4) . ? N11' C14' 1.485(5) . ? N11' C12' 1.509(4) . ? C12' C13' 1.511(7) . ? C14' C15' 1.498(6) . ? C16' C17' 1.469(6) . ? C16' C17B 1.643(10) . ? C17' N18' 1.453(8) . ? N18' C21' 1.481(10) . ? N18' C19' 1.547(10) . ? C19' C20' 1.545(11) . ? C21' C22' 1.535(12) . ? C17B N18B 1.432(12) . ? N18B C21B 1.426(11) . ? N18B C19B 1.537(13) . ? C19B C20B 1.489(14) . ? C20B C20B 1.93(4) 2_755 ? C21B C22B 1.529(12) . ? C23' C26' 1.529(6) . ? C23' C25' 1.530(5) . ? C23' C24' 1.551(6) . ? C27' C30' 1.533(7) . ? C27' C28' 1.550(6) . ? C27' C29' 1.580(8) . ? C31' C32' 1.514(5) . ? 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 O1 Zn C31 127.12(18) . . ? O1 Zn N11 100.98(9) . . ? C31 Zn N11 118.2(2) . . ? O1 Zn N8 93.67(9) . . ? C31 Zn N8 121.97(17) . . ? N11 Zn N8 85.26(11) . . ? C1 O1 Zn 111.28(16) . . ? O1 C1 C6 119.2(2) . . ? O1 C1 C2 122.6(3) . . ? C6 C1 C2 118.2(3) . . ? C3 C2 C1 118.0(3) . . ? C3 C2 C23 121.4(3) . . ? C1 C2 C23 120.7(3) . . ? C4 C3 C2 124.3(3) . . ? C5 C4 C3 116.6(3) . . ? C5 C4 C27 123.8(3) . . ? C3 C4 C27 119.6(3) . . ? C4 C5 C6 121.9(3) . . ? C5 C6 C1 121.0(2) . . ? C5 C6 C7 120.7(3) . . ? C1 C6 C7 118.2(3) . . ? N8 C7 C6 113.4(2) . . ? C16 N8 C7 111.4(2) . . ? C16 N8 C9 113.2(3) . . ? C7 N8 C9 110.1(2) . . ? C16 N8 Zn 109.48(19) . . ? C7 N8 Zn 108.02(17) . . ? C9 N8 Zn 104.3(2) . . ? N8 C9 C10 112.3(3) . . ? N11 C10 C9 111.5(3) . . ? C14 N11 C10 107.5(3) . . ? C14 N11 C12 114.4(3) . . ? C10 N11 C12 111.9(3) . . ? C14 N11 Zn 109.9(2) . . ? C10 N11 Zn 105.3(2) . . ? C12 N11 Zn 107.4(2) . . ? N11 C12 C13 115.3(3) . . ? N11 C14 C15 111.0(4) . . ? C17 C16 N8 127.1(4) . . ? C17 C16 C17A 24.9(3) . . ? N8 C16 C17A 102.4(4) . . ? C16 C17 N18 117.5(5) . . ? C21 N18 C17 107.3(8) . . ? C21 N18 C19 108.8(7) . . ? C17 N18 C19 106.6(7) . . ? C20 C19 N18 113.1(9) . . ? N18 C21 C22 109.5(9) . . ? N18A C17A C16 102.7(5) . . ? C17A N18A C19A 110.9(7) . . ? C17A N18A C21A 103.9(7) . . ? C19A N18A C21A 108.6(8) . . ? N18A C19A C20A 111.8(9) . . ? N18A C21A C22A 110.1(11) . . ? C25 C23 C24 109.8(4) . . ? C25 C23 C2 109.5(3) . . ? C24 C23 C2 109.4(3) . . ? C25 C23 C26 107.1(4) . . ? C24 C23 C26 109.0(4) . . ? C2 C23 C26 112.0(3) . . ? C30 C27 C28 112.7(5) . . ? C30 C27 C4 111.9(3) . . ? C28 C27 C4 109.1(3) . . ? C30 C27 C29 109.6(4) . . ? C28 C27 C29 105.3(4) . . ? C4 C27 C29 108.0(4) . . ? C32 C31 Zn 117.1(4) . . ? O1' Zn' C31' 127.46(18) . . ? O1' Zn' N11' 100.68(9) . . ? C31' Zn' N11' 118.24(18) . . ? O1' Zn' N8' 93.52(9) . . ? C31' Zn' N8' 121.64(14) . . ? N11' Zn' N8' 85.57(12) . . ? C1' O1' Zn' 111.53(17) . . ? O1' C1' C6' 119.0(3) . . ? O1' C1' C2' 122.5(3) . . ? C6' C1' C2' 118.5(3) . . ? C3' C2' C1' 118.3(3) . . ? C3' C2' C23' 121.4(3) . . ? C1' C2' C23' 120.2(3) . . ? C2' C3' C4' 124.2(3) . . ? C5' C4' C3' 115.9(3) . . ? C5' C4' C27' 124.1(3) . . ? C3' C4' C27' 119.9(4) . . ? C4' C5' C6' 122.5(3) . . ? C5' C6' C1' 120.5(3) . . ? C5' C6' C7' 120.7(3) . . ? C1' C6' C7' 118.6(3) . . ? N8' C7' C6' 113.2(2) . . ? C9' N8' C16' 112.9(3) . . ? C9' N8' C7' 110.7(3) . . ? C16' N8' C7' 111.9(3) . . ? C9' N8' Zn' 103.8(2) . . ? C16' N8' Zn' 109.3(2) . . ? C7' N8' Zn' 107.80(16) . . ? N8' C9' C10' 113.0(3) . . ? C9' C10' N11' 112.1(3) . . ? C14' N11' C10' 110.2(3) . . ? C14' N11' C12' 112.6(3) . . ? C10' N11' C12' 111.6(3) . . ? C14' N11' Zn' 110.5(2) . . ? C10' N11' Zn' 103.9(2) . . ? C12' N11' Zn' 107.7(2) . . ? N11' C12' C13' 116.5(4) . . ? N11' C14' C15' 113.2(3) . . ? C17' C16' N8' 128.1(5) . . ? C17' C16' C17B 25.5(4) . . ? N8' C16' C17B 102.8(5) . . ? N18' C17' C16' 115.4(5) . . ? C17' N18' C21' 111.5(7) . . ? C17' N18' C19' 106.6(7) . . ? C21' N18' C19' 105.5(6) . . ? C20' C19' N18' 105.6(8) . . ? N18' C21' C22' 112.6(9) . . ? N18B C17B C16' 103.8(8) . . ? C21B N18B C17B 117.1(11) . . ? C21B N18B C19B 112.4(11) . . ? C17B N18B C19B 103.5(9) . . ? C20B C19B N18B 111.4(12) . . ? C19B C20B C20B 134(2) . 2_755 ? N18B C21B C22B 116.8(11) . . ? C26' C23' C25' 108.2(3) . . ? C26' C23' C2' 112.5(4) . . ? C25' C23' C2' 109.7(3) . . ? C26' C23' C24' 109.2(4) . . ? C25' C23' C24' 107.4(4) . . ? C2' C23' C24' 109.7(3) . . ? C4' C27' C30' 112.9(4) . . ? C4' C27' C28' 111.6(4) . . ? C30' C27' C28' 107.9(4) . . ? C4' C27' C29' 109.5(4) . . ? C30' C27' C29' 106.9(4) . . ? C28' C27' C29' 107.8(5) . . ? C32' C31' Zn' 116.7(3) . . ? _diffrn_measured_fraction_theta_max 0.892 _diffrn_reflns_theta_full 32.74 _diffrn_measured_fraction_theta_full 0.892 _refine_diff_density_max 2.186 _refine_diff_density_min -1.273 _refine_diff_density_rms 0.096 #===END data_Compound_7b _database_code_depnum_ccdc_archive 'CCDC 293283' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27 H51 N3 O Zn' _chemical_formula_weight 499.08 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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 11.6696(3) _cell_length_b 19.4177(6) _cell_length_c 25.5282(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5784.6(3) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 3.9426 _cell_measurement_theta_max 32.6693 _exptl_crystal_description blocks _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.146 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2176 _exptl_absorpt_coefficient_mu 0.870 _exptl_absorpt_correction_type 'numeric analytical' _exptl_absorpt_correction_T_min 0.75992 _exptl_absorpt_correction_T_max 0.87826 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'OD Xcalibur 3' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 15.9863 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 58532 _diffrn_reflns_av_R_equivalents 0.0336 _diffrn_reflns_av_sigmaI/netI 0.0268 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -38 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 4.27 _diffrn_reflns_theta_max 32.77 _reflns_number_total 10193 _reflns_number_gt 7777 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd' _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^)+(0.0631P)^2^+1.3580P] 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 10193 _refine_ls_number_parameters 289 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0686 _refine_ls_R_factor_gt 0.0492 _refine_ls_wR_factor_ref 0.1372 _refine_ls_wR_factor_gt 0.1256 _refine_ls_goodness_of_fit_ref 1.167 _refine_ls_restrained_S_all 1.167 _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 Zn Zn 0.524613(16) 0.521335(10) 0.857945(8) 0.02794(7) Uani 1 1 d . . . O1 O 0.41220(10) 0.47753(5) 0.90331(5) 0.0295(2) Uani 1 1 d . . . C1 C 0.40627(12) 0.40910(8) 0.90524(6) 0.0246(3) Uani 1 1 d . . . C2 C 0.30061(13) 0.37309(8) 0.89981(6) 0.0247(3) Uani 1 1 d . . . C3 C 0.30071(14) 0.30171(8) 0.90656(7) 0.0290(3) Uani 1 1 d . . . H3A H 0.2297 0.2781 0.9038 0.035 Uiso 1 1 calc R . . C4 C 0.39894(14) 0.26284(8) 0.91709(7) 0.0309(3) Uani 1 1 d . . . C5 C 0.50214(14) 0.29881(9) 0.91983(7) 0.0298(3) Uani 1 1 d . . . H5A H 0.5712 0.2740 0.9255 0.036 Uiso 1 1 calc R . . C6 C 0.50659(13) 0.36990(9) 0.91447(6) 0.0265(3) Uani 1 1 d . . . C7 C 0.61885(13) 0.40684(9) 0.92111(6) 0.0294(3) Uani 1 1 d . . . H7A H 0.6122 0.4394 0.9508 0.035 Uiso 1 1 calc R . . H7B H 0.6788 0.3728 0.9301 0.035 Uiso 1 1 calc R . . N8 N 0.65548(11) 0.44548(7) 0.87380(6) 0.0279(3) Uani 1 1 d . . . C9 C 0.77028(15) 0.47620(10) 0.88170(8) 0.0374(4) Uani 1 1 d . . . H9A H 0.7979 0.4941 0.8477 0.045 Uiso 1 1 calc R . . H9B H 0.8236 0.4393 0.8928 0.045 Uiso 1 1 calc R . . C10 C 0.77548(16) 0.53411(11) 0.92170(8) 0.0410(4) Uani 1 1 d . . . H10A H 0.8570 0.5433 0.9299 0.049 Uiso 1 1 calc R . . H10B H 0.7385 0.5179 0.9544 0.049 Uiso 1 1 calc R . . C11 C 0.71946(16) 0.60189(10) 0.90568(8) 0.0413(4) Uani 1 1 d . . . H11A H 0.7476 0.6386 0.9293 0.050 Uiso 1 1 calc R . . H11B H 0.7449 0.6135 0.8698 0.050 Uiso 1 1 calc R . . N12 N 0.59241(13) 0.60226(8) 0.90677(6) 0.0334(3) Uani 1 1 d . . . C13 C 0.55402(19) 0.66892(10) 0.88506(9) 0.0434(4) Uani 1 1 d . . . H13A H 0.5840 0.7065 0.9067 0.065 Uiso 1 1 calc R . . H13B H 0.4701 0.6706 0.8850 0.065 Uiso 1 1 calc R . . H13C H 0.5825 0.6738 0.8491 0.065 Uiso 1 1 calc R . . C14 C 0.55085(19) 0.59793(11) 0.96149(8) 0.0428(4) Uani 1 1 d . . . H14A H 0.5839 0.6356 0.9820 0.064 Uiso 1 1 calc R . . H14B H 0.5740 0.5537 0.9767 0.064 Uiso 1 1 calc R . . H14C H 0.4671 0.6015 0.9619 0.064 Uiso 1 1 calc R . . C15 C 0.65594(14) 0.40079(9) 0.82653(7) 0.0316(3) Uani 1 1 d . . . H15A H 0.6713 0.4303 0.7957 0.038 Uiso 1 1 calc R . . H15B H 0.5780 0.3814 0.8222 0.038 Uiso 1 1 calc R . . C16 C 0.74123(16) 0.34121(10) 0.82570(8) 0.0382(4) Uani 1 1 d . . . H16A H 0.8194 0.3589 0.8190 0.046 Uiso 1 1 calc R . . H16B H 0.7413 0.3175 0.8600 0.046 Uiso 1 1 calc R . . C17 C 0.70673(16) 0.29132(10) 0.78285(8) 0.0379(4) Uani 1 1 d . . . H17A H 0.6303 0.2721 0.7913 0.046 Uiso 1 1 calc R . . H17B H 0.6998 0.3169 0.7495 0.046 Uiso 1 1 calc R . . N18 N 0.78685(14) 0.23466(8) 0.77554(7) 0.0381(3) Uani 1 1 d . . . C19 C 0.7330(2) 0.18137(12) 0.74398(11) 0.0574(6) Uani 1 1 d . . . H19A H 0.7866 0.1430 0.7393 0.086 Uiso 1 1 calc R . . H19B H 0.7124 0.2004 0.7097 0.086 Uiso 1 1 calc R . . H19C H 0.6638 0.1648 0.7617 0.086 Uiso 1 1 calc R . . C20 C 0.89218(19) 0.25750(12) 0.75082(10) 0.0519(5) Uani 1 1 d . . . H20A H 0.9443 0.2183 0.7468 0.078 Uiso 1 1 calc R . . H20B H 0.9286 0.2928 0.7727 0.078 Uiso 1 1 calc R . . H20C H 0.8748 0.2769 0.7163 0.078 Uiso 1 1 calc R . . C21 C 0.18873(13) 0.41170(8) 0.88872(7) 0.0270(3) Uani 1 1 d . . . C22 C 0.20110(17) 0.45763(10) 0.84010(8) 0.0386(4) Uani 1 1 d . . . H22A H 0.2204 0.4291 0.8097 0.058 Uiso 1 1 calc R . . H22B H 0.2621 0.4914 0.8460 0.058 Uiso 1 1 calc R . . H22C H 0.1287 0.4817 0.8336 0.058 Uiso 1 1 calc R . . C23 C 0.15869(16) 0.45582(9) 0.93657(8) 0.0354(4) Uani 1 1 d . . . H23A H 0.2217 0.4878 0.9438 0.053 Uiso 1 1 calc R . . H23B H 0.1466 0.4259 0.9670 0.053 Uiso 1 1 calc R . . H23C H 0.0886 0.4820 0.9295 0.053 Uiso 1 1 calc R . . C24 C 0.08762(14) 0.36287(9) 0.87856(9) 0.0375(4) Uani 1 1 d . . . H24A H 0.1044 0.3340 0.8480 0.056 Uiso 1 1 calc R . . H24B H 0.0182 0.3899 0.8719 0.056 Uiso 1 1 calc R . . H24C H 0.0757 0.3335 0.9093 0.056 Uiso 1 1 calc R . . C25 C 0.39620(17) 0.18479(9) 0.92488(9) 0.0402(4) Uani 1 1 d . . . C26 C 0.2742(2) 0.15589(10) 0.92318(12) 0.0597(7) Uani 1 1 d . . . H26A H 0.2282 0.1774 0.9508 0.090 Uiso 1 1 calc R . . H26B H 0.2765 0.1060 0.9286 0.090 Uiso 1 1 calc R . . H26C H 0.2399 0.1659 0.8890 0.090 Uiso 1 1 calc R . . C27 C 0.4654(2) 0.14983(11) 0.88090(11) 0.0517(6) Uani 1 1 d . . . H27A H 0.5442 0.1672 0.8813 0.078 Uiso 1 1 calc R . . H27B H 0.4300 0.1602 0.8470 0.078 Uiso 1 1 calc R . . H27C H 0.4659 0.0999 0.8865 0.078 Uiso 1 1 calc R . . C28 C 0.4502(3) 0.16614(12) 0.97737(11) 0.0605(7) Uani 1 1 d . . . H28A H 0.5286 0.1842 0.9788 0.091 Uiso 1 1 calc R . . H28B H 0.4519 0.1159 0.9812 0.091 Uiso 1 1 calc R . . H28C H 0.4049 0.1863 1.0058 0.091 Uiso 1 1 calc R . . C29 C 0.51507(17) 0.55024(11) 0.78316(8) 0.0393(4) Uani 1 1 d . . . H29A H 0.4887 0.5987 0.7824 0.047 Uiso 1 1 calc R . . H29B H 0.5937 0.5495 0.7686 0.047 Uiso 1 1 calc R . . C30 C 0.4389(2) 0.50922(13) 0.74651(8) 0.0511(5) Uani 1 1 d . . . H30A H 0.4427 0.5291 0.7113 0.077 Uiso 1 1 calc R . . H30B H 0.3597 0.5108 0.7592 0.077 Uiso 1 1 calc R . . H30C H 0.4651 0.4613 0.7454 0.077 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn 0.02535(11) 0.03107(11) 0.02739(11) 0.00030(7) 0.00011(7) -0.00466(7) O1 0.0242(5) 0.0259(5) 0.0385(6) 0.0003(4) 0.0036(5) -0.0029(4) C1 0.0200(6) 0.0268(7) 0.0271(7) 0.0005(5) 0.0015(6) -0.0005(5) C2 0.0204(6) 0.0252(6) 0.0286(7) 0.0016(5) -0.0002(6) 0.0008(5) C3 0.0231(7) 0.0267(7) 0.0373(9) 0.0033(6) -0.0008(6) -0.0012(5) C4 0.0283(7) 0.0262(7) 0.0381(9) 0.0040(6) -0.0020(7) 0.0021(6) C5 0.0245(7) 0.0317(8) 0.0331(8) 0.0038(6) -0.0016(6) 0.0051(6) C6 0.0212(6) 0.0325(8) 0.0258(7) 0.0011(6) 0.0008(6) -0.0008(6) C7 0.0207(6) 0.0407(8) 0.0268(7) 0.0004(6) -0.0012(6) -0.0017(6) N8 0.0206(6) 0.0380(7) 0.0251(6) -0.0010(5) 0.0016(5) -0.0040(5) C9 0.0223(7) 0.0503(10) 0.0395(10) -0.0037(8) 0.0055(7) -0.0081(7) C10 0.0266(8) 0.0583(12) 0.0381(10) -0.0047(8) -0.0020(7) -0.0134(8) C11 0.0329(9) 0.0496(11) 0.0416(10) -0.0082(8) 0.0060(8) -0.0158(8) N12 0.0314(7) 0.0385(7) 0.0303(7) -0.0026(6) 0.0061(6) -0.0096(6) C13 0.0478(11) 0.0354(9) 0.0469(12) -0.0017(8) 0.0075(9) -0.0080(8) C14 0.0460(10) 0.0501(11) 0.0322(9) -0.0050(8) 0.0110(8) -0.0065(9) C15 0.0265(7) 0.0419(9) 0.0266(8) -0.0031(6) 0.0009(6) 0.0012(6) C16 0.0279(8) 0.0498(10) 0.0370(9) -0.0055(8) -0.0012(7) 0.0062(7) C17 0.0304(8) 0.0430(9) 0.0403(10) -0.0067(8) -0.0055(8) 0.0075(7) N18 0.0324(7) 0.0382(8) 0.0437(9) -0.0022(6) -0.0030(7) 0.0073(6) C19 0.0516(13) 0.0436(11) 0.0769(18) -0.0155(11) -0.0128(12) 0.0107(9) C20 0.0427(11) 0.0547(12) 0.0581(14) -0.0059(10) 0.0120(10) 0.0071(9) C21 0.0199(6) 0.0271(7) 0.0339(8) 0.0011(6) -0.0005(6) 0.0014(5) C22 0.0336(9) 0.0423(9) 0.0398(10) 0.0096(8) -0.0059(8) 0.0032(7) C23 0.0317(8) 0.0327(8) 0.0419(10) -0.0024(7) 0.0058(7) 0.0013(7) C24 0.0220(7) 0.0359(8) 0.0547(11) -0.0017(8) -0.0048(8) -0.0004(6) C25 0.0360(9) 0.0282(8) 0.0564(12) 0.0090(7) -0.0062(9) 0.0038(7) C26 0.0455(12) 0.0282(9) 0.105(2) 0.0158(11) -0.0026(13) -0.0038(8) C27 0.0532(13) 0.0339(10) 0.0679(16) -0.0012(10) -0.0074(11) 0.0103(9) C28 0.0756(17) 0.0447(12) 0.0611(15) 0.0200(11) -0.0162(13) 0.0021(11) C29 0.0422(10) 0.0442(10) 0.0313(9) 0.0070(8) -0.0045(8) -0.0051(8) C30 0.0438(11) 0.0778(15) 0.0316(10) -0.0026(10) -0.0044(9) -0.0101(11) _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 Zn O1 1.9456(12) . ? Zn C29 1.9930(19) . ? Zn N12 2.1560(15) . ? Zn N8 2.1599(14) . ? O1 C1 1.3315(18) . ? C1 C6 1.416(2) . ? C1 C2 1.424(2) . ? C2 C3 1.397(2) . ? C2 C21 1.532(2) . ? C3 C4 1.399(2) . ? C4 C5 1.394(2) . ? C4 C25 1.529(2) . ? C5 C6 1.388(2) . ? C6 C7 1.503(2) . ? C7 N8 1.485(2) . ? N8 C9 1.480(2) . ? N8 C15 1.486(2) . ? C9 C10 1.520(3) . ? C10 C11 1.525(3) . ? C11 N12 1.483(2) . ? N12 C13 1.478(3) . ? N12 C14 1.481(2) . ? C15 C16 1.526(2) . ? C16 C17 1.516(3) . ? C17 N18 1.456(2) . ? N18 C20 1.451(3) . ? N18 C19 1.454(3) . ? C21 C23 1.532(2) . ? C21 C22 1.535(2) . ? C21 C24 1.536(2) . ? C25 C28 1.525(3) . ? C25 C26 1.531(3) . ? C25 C27 1.541(3) . ? C29 C30 1.517(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Zn C29 130.97(7) . . ? O1 Zn N12 102.82(5) . . ? C29 Zn N12 111.65(7) . . ? O1 Zn N8 93.85(5) . . ? C29 Zn N8 114.27(7) . . ? N12 Zn N8 97.43(6) . . ? C1 O1 Zn 119.56(10) . . ? O1 C1 C6 119.97(14) . . ? O1 C1 C2 122.10(13) . . ? C6 C1 C2 117.91(14) . . ? C3 C2 C1 118.33(14) . . ? C3 C2 C21 120.61(13) . . ? C1 C2 C21 121.03(13) . . ? C2 C3 C4 124.05(15) . . ? C5 C4 C3 116.58(14) . . ? C5 C4 C25 120.54(15) . . ? C3 C4 C25 122.87(15) . . ? C6 C5 C4 121.71(15) . . ? C5 C6 C1 121.33(15) . . ? C5 C6 C7 119.73(15) . . ? C1 C6 C7 118.88(14) . . ? N8 C7 C6 113.58(13) . . ? C9 N8 C7 110.69(14) . . ? C9 N8 C15 110.03(13) . . ? C7 N8 C15 111.50(13) . . ? C9 N8 Zn 112.99(11) . . ? C7 N8 Zn 107.07(10) . . ? C15 N8 Zn 104.40(10) . . ? N8 C9 C10 115.19(15) . . ? C9 C10 C11 116.17(17) . . ? N12 C11 C10 115.32(15) . . ? C13 N12 C14 107.70(15) . . ? C13 N12 C11 107.48(15) . . ? C14 N12 C11 110.17(16) . . ? C13 N12 Zn 108.09(12) . . ? C14 N12 Zn 112.56(11) . . ? C11 N12 Zn 110.65(11) . . ? N8 C15 C16 117.15(14) . . ? C17 C16 C15 108.74(15) . . ? N18 C17 C16 113.89(15) . . ? C20 N18 C19 110.03(19) . . ? C20 N18 C17 111.64(16) . . ? C19 N18 C17 109.35(16) . . ? C2 C21 C23 108.74(14) . . ? C2 C21 C22 110.71(13) . . ? C23 C21 C22 109.95(15) . . ? C2 C21 C24 112.57(13) . . ? C23 C21 C24 107.69(14) . . ? C22 C21 C24 107.11(15) . . ? C28 C25 C4 109.95(17) . . ? C28 C25 C26 108.8(2) . . ? C4 C25 C26 112.28(15) . . ? C28 C25 C27 108.61(18) . . ? C4 C25 C27 109.32(17) . . ? C26 C25 C27 107.76(19) . . ? C30 C29 Zn 118.41(14) . . ? _diffrn_measured_fraction_theta_max 0.952 _diffrn_reflns_theta_full 32.77 _diffrn_measured_fraction_theta_full 0.952 _refine_diff_density_max 1.043 _refine_diff_density_min -0.516 _refine_diff_density_rms 0.063 #===END data_Compound_9c _database_code_depnum_ccdc_archive 'CCDC 293284' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C56 H88 Cl2 Fe2 N2 O6' _chemical_formula_weight 1067.88 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' Fe Fe 0.3463 0.8444 '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 10.6902(4) _cell_length_b 13.6702(4) _cell_length_c 19.5952(6) _cell_angle_alpha 90.00 _cell_angle_beta 94.272(3) _cell_angle_gamma 90.00 _cell_volume 2855.63(16) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 3.7778 _cell_measurement_theta_max 32.7079 _exptl_crystal_description needles _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.242 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1144 _exptl_absorpt_coefficient_mu 0.649 _exptl_absorpt_correction_type 'numeric analytical' _exptl_absorpt_correction_T_min 0.87399 _exptl_absorpt_correction_T_max 0.96717 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'OD Xcalibur 3' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 15.9863 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29044 _diffrn_reflns_av_R_equivalents 0.0349 _diffrn_reflns_av_sigmaI/netI 0.0507 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 4.10 _diffrn_reflns_theta_max 32.78 _reflns_number_total 9871 _reflns_number_gt 6715 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd' _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^)+(0.0538P)^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 9871 _refine_ls_number_parameters 308 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0718 _refine_ls_R_factor_gt 0.0413 _refine_ls_wR_factor_ref 0.1072 _refine_ls_wR_factor_gt 0.0969 _refine_ls_goodness_of_fit_ref 1.014 _refine_ls_restrained_S_all 1.014 _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 Fe Fe 0.389775(19) 0.028023(15) 0.429209(11) 0.02154(6) Uani 1 1 d . . . Cl Cl 0.61505(3) 0.04071(3) 0.450296(18) 0.02556(9) Uani 1 1 d . . . O1 O 0.32434(9) 0.15809(8) 0.44526(6) 0.0276(2) Uani 1 1 d . . . C1 C 0.21309(13) 0.19952(11) 0.43239(7) 0.0226(3) Uani 1 1 d . . . C2 C 0.20022(13) 0.30248(11) 0.42396(7) 0.0221(3) Uani 1 1 d . . . C3 C 0.07941(13) 0.34149(11) 0.41296(7) 0.0225(3) Uani 1 1 d . . . H3A H 0.0714 0.4104 0.4084 0.027 Uiso 1 1 calc R . . C4 C -0.02999(13) 0.28551(11) 0.40822(7) 0.0226(3) Uani 1 1 d . . . C5 C -0.01456(13) 0.18478(11) 0.41469(8) 0.0229(3) Uani 1 1 d . . . H5A H -0.0867 0.1440 0.4111 0.027 Uiso 1 1 calc R . . C6 C 0.10267(13) 0.14194(10) 0.42619(7) 0.0219(3) Uani 1 1 d . . . C7 C 0.11164(14) 0.03250(10) 0.43532(8) 0.0233(3) Uani 1 1 d . . . H7A H 0.1390 0.0183 0.4837 0.028 Uiso 1 1 calc R . . H7B H 0.0270 0.0039 0.4259 0.028 Uiso 1 1 calc R . . N8 N 0.19940(11) -0.01643(9) 0.39069(6) 0.0215(2) Uani 1 1 d . . . C9 C 0.19176(14) -0.12338(11) 0.40272(9) 0.0271(3) Uani 1 1 d . . . H9A H 0.1110 -0.1484 0.3817 0.033 Uiso 1 1 calc R . . H9B H 0.1942 -0.1360 0.4526 0.033 Uiso 1 1 calc R . . C10 C 0.29828(14) -0.17710(12) 0.37294(9) 0.0300(3) Uani 1 1 d . . . H10A H 0.2987 -0.2465 0.3873 0.036 Uiso 1 1 calc R . . H10B H 0.2885 -0.1746 0.3223 0.036 Uiso 1 1 calc R . . O11 O 0.41227(10) -0.13109(8) 0.39718(6) 0.0287(2) Uani 1 1 d . . . C12 C 0.51709(16) -0.17070(14) 0.36582(11) 0.0429(5) Uani 1 1 d . . . H12A H 0.5036 -0.2407 0.3574 0.064 Uiso 1 1 calc R . . H12B H 0.5932 -0.1615 0.3962 0.064 Uiso 1 1 calc R . . H12C H 0.5266 -0.1372 0.3223 0.064 Uiso 1 1 calc R . . C13 C 0.17159(15) 0.00807(12) 0.31721(8) 0.0276(3) Uani 1 1 d . . . H13A H 0.0865 0.0368 0.3109 0.033 Uiso 1 1 calc R . . H13B H 0.1718 -0.0529 0.2899 0.033 Uiso 1 1 calc R . . C14 C 0.26422(16) 0.07874(14) 0.29056(9) 0.0349(4) Uani 1 1 d . . . H14A H 0.2547 0.0804 0.2399 0.042 Uiso 1 1 calc R . . H14B H 0.2488 0.1454 0.3079 0.042 Uiso 1 1 calc R . . O15 O 0.38766(10) 0.04777(9) 0.31305(6) 0.0342(3) Uani 1 1 d . . . C16 C 0.48312(17) 0.09752(15) 0.27940(10) 0.0421(4) Uani 1 1 d . . . H16A H 0.4623 0.0965 0.2298 0.063 Uiso 1 1 calc R . . H16B H 0.5638 0.0648 0.2899 0.063 Uiso 1 1 calc R . . H16C H 0.4888 0.1654 0.2953 0.063 Uiso 1 1 calc R . . C17 C 0.31643(14) 0.36890(11) 0.42782(8) 0.0276(3) Uani 1 1 d . . . C18 C 0.38636(17) 0.36101(13) 0.49881(10) 0.0391(4) Uani 1 1 d . . . H18A H 0.3303 0.3805 0.5338 0.059 Uiso 1 1 calc R . . H18B H 0.4597 0.4042 0.5011 0.059 Uiso 1 1 calc R . . H18C H 0.4137 0.2933 0.5069 0.059 Uiso 1 1 calc R . . C19 C 0.40497(16) 0.33846(13) 0.37297(10) 0.0366(4) Uani 1 1 d . . . H19A H 0.4285 0.2696 0.3795 0.055 Uiso 1 1 calc R . . H19B H 0.4805 0.3793 0.3771 0.055 Uiso 1 1 calc R . . H19C H 0.3621 0.3471 0.3274 0.055 Uiso 1 1 calc R . . C20 C 0.28265(17) 0.47679(12) 0.41500(11) 0.0386(4) Uani 1 1 d . . . H20A H 0.2260 0.4988 0.4490 0.058 Uiso 1 1 calc R . . H20B H 0.2411 0.4841 0.3690 0.058 Uiso 1 1 calc R . . H20C H 0.3593 0.5164 0.4188 0.058 Uiso 1 1 calc R . . C21 C -0.16160(14) 0.32996(11) 0.39756(8) 0.0250(3) Uani 1 1 d . . . C22 C -0.15836(16) 0.44089(13) 0.38734(10) 0.0388(4) Uani 1 1 d . . . H22A H -0.1112 0.4562 0.3477 0.058 Uiso 1 1 calc R . . H22B H -0.1176 0.4718 0.4283 0.058 Uiso 1 1 calc R . . H22C H -0.2442 0.4657 0.3795 0.058 Uiso 1 1 calc R . . C23 C -0.23223(16) 0.28484(14) 0.33380(9) 0.0374(4) Uani 1 1 d . . . H23A H -0.1862 0.2985 0.2934 0.056 Uiso 1 1 calc R . . H23B H -0.3164 0.3134 0.3275 0.056 Uiso 1 1 calc R . . H23C H -0.2390 0.2139 0.3399 0.056 Uiso 1 1 calc R . . C24 C -0.23608(15) 0.30774(13) 0.45981(9) 0.0323(4) Uani 1 1 d . . . H24A H -0.1927 0.3361 0.5010 0.048 Uiso 1 1 calc R . . H24B H -0.2429 0.2368 0.4655 0.048 Uiso 1 1 calc R . . H24C H -0.3202 0.3362 0.4527 0.048 Uiso 1 1 calc R . . C30 C 0.19498(19) 0.44822(17) 0.19994(12) 0.0549(6) Uani 1 1 d . . . H30A H 0.2755 0.4375 0.2262 0.082 Uiso 1 1 calc R . . H30B H 0.1392 0.4857 0.2276 0.082 Uiso 1 1 calc R . . H30C H 0.2089 0.4847 0.1581 0.082 Uiso 1 1 calc R . . C31 C 0.13559(15) 0.35092(15) 0.18129(9) 0.0372(4) Uani 1 1 d . . . C32 C 0.14230(16) 0.31200(16) 0.11601(9) 0.0409(4) Uani 1 1 d . . . H32A H 0.1868 0.3463 0.0833 0.049 Uiso 1 1 calc R . . C33 C 0.08497(17) 0.22401(16) 0.09831(10) 0.0456(5) Uani 1 1 d . . . H33A H 0.0910 0.1980 0.0537 0.055 Uiso 1 1 calc R . . C34 C 0.01906(19) 0.17379(15) 0.14510(12) 0.0485(5) Uani 1 1 d . . . H34A H -0.0214 0.1139 0.1326 0.058 Uiso 1 1 calc R . . C35 C 0.01232(19) 0.21136(15) 0.21034(11) 0.0472(5) Uani 1 1 d . . . H35A H -0.0325 0.1769 0.2429 0.057 Uiso 1 1 calc R . . C36 C 0.07053(17) 0.29857(15) 0.22819(9) 0.0416(4) Uani 1 1 d . . . H36A H 0.0662 0.3233 0.2732 0.050 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe 0.01864(10) 0.02275(11) 0.02274(11) -0.00011(8) -0.00162(8) 0.00110(8) Cl 0.01979(16) 0.0324(2) 0.02403(18) 0.00177(14) -0.00120(13) -0.00155(14) O1 0.0196(5) 0.0241(5) 0.0384(6) -0.0019(5) -0.0038(4) 0.0018(4) C1 0.0202(7) 0.0243(7) 0.0228(7) -0.0025(6) -0.0006(5) 0.0008(6) C2 0.0214(7) 0.0230(7) 0.0218(7) -0.0028(5) 0.0006(5) -0.0004(6) C3 0.0256(7) 0.0208(7) 0.0210(7) -0.0005(5) 0.0028(6) 0.0020(6) C4 0.0210(7) 0.0257(7) 0.0211(7) 0.0015(6) 0.0012(5) 0.0026(6) C5 0.0189(7) 0.0252(7) 0.0242(7) 0.0003(6) 0.0002(5) -0.0012(6) C6 0.0212(7) 0.0212(7) 0.0231(7) -0.0004(5) -0.0003(5) 0.0006(5) C7 0.0209(7) 0.0210(7) 0.0279(8) 0.0001(6) 0.0010(6) -0.0001(6) N8 0.0212(6) 0.0204(6) 0.0226(6) 0.0001(5) -0.0012(5) -0.0003(5) C9 0.0243(7) 0.0201(7) 0.0366(9) 0.0009(6) -0.0012(6) -0.0024(6) C10 0.0292(8) 0.0238(8) 0.0361(9) -0.0045(6) -0.0028(7) -0.0007(6) O11 0.0227(5) 0.0285(6) 0.0346(6) -0.0075(5) -0.0001(4) 0.0018(4) C12 0.0290(9) 0.0411(10) 0.0595(13) -0.0123(9) 0.0088(8) 0.0060(8) C13 0.0266(8) 0.0304(8) 0.0249(8) -0.0008(6) -0.0047(6) 0.0003(6) C14 0.0330(9) 0.0429(10) 0.0282(9) 0.0045(7) -0.0023(7) 0.0008(7) O15 0.0248(6) 0.0479(7) 0.0298(6) 0.0095(5) 0.0017(5) -0.0005(5) C16 0.0363(10) 0.0524(12) 0.0388(10) 0.0076(8) 0.0101(8) -0.0038(9) C17 0.0222(7) 0.0243(8) 0.0360(9) -0.0017(6) 0.0003(6) -0.0020(6) C18 0.0356(9) 0.0373(10) 0.0429(10) -0.0063(8) -0.0071(8) -0.0075(8) C19 0.0277(8) 0.0351(9) 0.0480(11) 0.0013(8) 0.0103(7) -0.0024(7) C20 0.0314(9) 0.0233(8) 0.0608(12) -0.0013(8) 0.0023(8) -0.0034(7) C21 0.0217(7) 0.0259(8) 0.0273(8) 0.0045(6) 0.0014(6) 0.0028(6) C22 0.0292(9) 0.0297(9) 0.0577(12) 0.0120(8) 0.0045(8) 0.0067(7) C23 0.0270(8) 0.0502(11) 0.0340(9) -0.0004(8) -0.0048(7) 0.0084(8) C24 0.0270(8) 0.0348(9) 0.0358(9) 0.0042(7) 0.0070(7) 0.0064(7) C30 0.0366(11) 0.0711(15) 0.0559(14) -0.0062(11) -0.0042(9) -0.0005(10) C31 0.0249(8) 0.0550(12) 0.0311(9) 0.0015(8) -0.0018(7) 0.0093(8) C32 0.0263(8) 0.0682(13) 0.0285(9) 0.0048(8) 0.0040(7) 0.0088(8) C33 0.0356(10) 0.0644(14) 0.0366(10) -0.0094(9) 0.0021(8) 0.0179(9) C34 0.0429(11) 0.0409(11) 0.0615(14) -0.0029(10) 0.0018(10) 0.0176(9) C35 0.0460(11) 0.0493(12) 0.0472(12) 0.0206(9) 0.0096(9) 0.0181(9) C36 0.0388(10) 0.0604(13) 0.0255(9) 0.0045(8) 0.0026(7) 0.0163(9) _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 Fe O1 1.9449(10) . ? Fe N8 2.2027(12) . ? Fe O11 2.2815(11) . ? Fe O15 2.2905(12) . ? Fe Cl 2.4192(4) . ? Fe Cl 2.5453(4) 3_656 ? Cl Fe 2.5453(4) 3_656 ? O1 C1 1.3243(17) . ? C1 C6 1.416(2) . ? C1 C2 1.423(2) . ? C2 C3 1.399(2) . ? C2 C17 1.536(2) . ? C3 C4 1.395(2) . ? C4 C5 1.391(2) . ? C4 C21 1.532(2) . ? C5 C6 1.386(2) . ? C6 C7 1.509(2) . ? C7 N8 1.4882(19) . ? N8 C9 1.4842(18) . ? N8 C13 1.487(2) . ? C9 C10 1.508(2) . ? C10 O11 1.4212(18) . ? O11 C12 1.4245(19) . ? C13 C14 1.505(2) . ? C14 O15 1.424(2) . ? O15 C16 1.428(2) . ? C17 C18 1.533(2) . ? C17 C20 1.535(2) . ? C17 C19 1.541(2) . ? C21 C22 1.530(2) . ? C21 C24 1.536(2) . ? C21 C23 1.540(2) . ? C30 C31 1.507(3) . ? C31 C36 1.391(3) . ? C31 C32 1.392(3) . ? C32 C33 1.382(3) . ? C33 C34 1.380(3) . ? C34 C35 1.385(3) . ? C35 C36 1.378(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Fe N8 88.47(4) . . ? O1 Fe O11 164.29(4) . . ? N8 Fe O11 75.90(4) . . ? O1 Fe O15 94.35(5) . . ? N8 Fe O15 75.62(4) . . ? O11 Fe O15 80.36(4) . . ? O1 Fe Cl 105.80(3) . . ? N8 Fe Cl 163.93(3) . . ? O11 Fe Cl 89.50(3) . . ? O15 Fe Cl 95.58(3) . . ? O1 Fe Cl 98.92(4) . 3_656 ? N8 Fe Cl 97.70(3) . 3_656 ? O11 Fe Cl 85.02(3) . 3_656 ? O15 Fe Cl 165.01(3) . 3_656 ? Cl Fe Cl 87.520(14) . 3_656 ? Fe Cl Fe 92.480(14) . 3_656 ? C1 O1 Fe 133.54(9) . . ? O1 C1 C6 120.63(13) . . ? O1 C1 C2 121.52(13) . . ? C6 C1 C2 117.85(13) . . ? C3 C2 C1 118.37(13) . . ? C3 C2 C17 121.08(13) . . ? C1 C2 C17 120.55(13) . . ? C4 C3 C2 124.12(14) . . ? C5 C4 C3 116.34(13) . . ? C5 C4 C21 120.41(13) . . ? C3 C4 C21 123.24(13) . . ? C6 C5 C4 122.17(13) . . ? C5 C6 C1 121.10(13) . . ? C5 C6 C7 119.13(13) . . ? C1 C6 C7 119.71(13) . . ? N8 C7 C6 114.41(12) . . ? C9 N8 C13 111.49(12) . . ? C9 N8 C7 107.75(11) . . ? C13 N8 C7 112.25(12) . . ? C9 N8 Fe 106.12(8) . . ? C13 N8 Fe 112.50(9) . . ? C7 N8 Fe 106.35(8) . . ? N8 C9 C10 111.47(13) . . ? O11 C10 C9 107.97(12) . . ? C10 O11 C12 111.71(13) . . ? C10 O11 Fe 114.11(9) . . ? C12 O11 Fe 125.70(10) . . ? N8 C13 C14 113.05(13) . . ? O15 C14 C13 108.68(13) . . ? C14 O15 C16 113.14(13) . . ? C14 O15 Fe 106.44(9) . . ? C16 O15 Fe 124.10(11) . . ? C18 C17 C20 108.01(14) . . ? C18 C17 C2 109.94(13) . . ? C20 C17 C2 112.36(13) . . ? C18 C17 C19 109.30(14) . . ? C20 C17 C19 107.12(14) . . ? C2 C17 C19 110.03(13) . . ? C22 C21 C4 112.41(13) . . ? C22 C21 C24 108.54(14) . . ? C4 C21 C24 109.78(12) . . ? C22 C21 C23 107.77(14) . . ? C4 C21 C23 109.96(13) . . ? C24 C21 C23 108.25(13) . . ? C36 C31 C32 118.21(19) . . ? C36 C31 C30 121.07(18) . . ? C32 C31 C30 120.70(18) . . ? C33 C32 C31 120.72(18) . . ? C34 C33 C32 120.33(19) . . ? C33 C34 C35 119.5(2) . . ? C36 C35 C34 120.12(19) . . ? C35 C36 C31 121.06(18) . . ? _diffrn_measured_fraction_theta_max 0.933 _diffrn_reflns_theta_full 32.78 _diffrn_measured_fraction_theta_full 0.933 _refine_diff_density_max 0.721 _refine_diff_density_min -0.348 _refine_diff_density_rms 0.059 #===END data_Compound_8a _database_code_depnum_ccdc_archive 'CCDC 293285' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27 H50 Cl2 Cr N3 O' _chemical_formula_weight 555.60 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cr Cr -0.1635 2.4439 '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 28.367(4) _cell_length_b 13.2626(18) _cell_length_c 16.275(2) _cell_angle_alpha 90.00 _cell_angle_beta 98.509(11) _cell_angle_gamma 90.00 _cell_volume 6055.5(14) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 2.9537 _cell_measurement_theta_max 71.0181 _exptl_crystal_description needles _exptl_crystal_colour 'Pale green' _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.219 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2392 _exptl_absorpt_coefficient_mu 4.896 _exptl_absorpt_correction_type 'numeric analytical' _exptl_absorpt_correction_T_min 0.52728 _exptl_absorpt_correction_T_max 0.94031 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 1.54248 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'Enhance Ultra (Cu) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'OD Xcalibur PX Ultra' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 8.2556 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28161 _diffrn_reflns_av_R_equivalents 0.1052 _diffrn_reflns_av_sigmaI/netI 0.1141 _diffrn_reflns_limit_h_min -34 _diffrn_reflns_limit_h_max 34 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 4.46 _diffrn_reflns_theta_max 71.21 _reflns_number_total 5728 _reflns_number_gt 3537 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd' _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^)+(0.0140P)^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 5728 _refine_ls_number_parameters 307 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1159 _refine_ls_R_factor_gt 0.0516 _refine_ls_wR_factor_ref 0.0829 _refine_ls_wR_factor_gt 0.0646 _refine_ls_goodness_of_fit_ref 0.954 _refine_ls_restrained_S_all 0.954 _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 Cr Cr 0.17366(2) 0.54920(5) 0.25734(3) 0.02420(15) Uani 1 1 d . . . Cl1 Cl 0.19637(3) 0.71998(7) 0.25083(6) 0.0345(2) Uani 1 1 d . . . Cl2 Cl 0.14144(3) 0.57683(7) 0.37930(5) 0.0319(2) Uani 1 1 d . . . O1 O 0.15895(8) 0.40964(17) 0.27003(13) 0.0265(6) Uani 1 1 d . . . C1 C 0.14216(12) 0.3387(3) 0.2138(2) 0.0241(8) Uani 1 1 d . . . C2 C 0.11119(12) 0.2608(3) 0.2339(2) 0.0256(9) Uani 1 1 d . . . C3 C 0.09161(12) 0.1977(3) 0.1688(2) 0.0283(9) Uani 1 1 d . . . H3A H 0.0705 0.1460 0.1811 0.034 Uiso 1 1 calc R . . C4 C 0.10078(12) 0.2052(3) 0.0873(2) 0.0271(9) Uani 1 1 d . . . C5 C 0.13344(12) 0.2782(3) 0.0718(2) 0.0253(9) Uani 1 1 d . . . H5A H 0.1415 0.2846 0.0174 0.030 Uiso 1 1 calc R . . C6 C 0.15467(12) 0.3420(3) 0.1344(2) 0.0251(9) Uani 1 1 d . . . C7 C 0.19653(13) 0.4050(3) 0.1183(2) 0.0301(9) Uani 1 1 d . . . H7A H 0.1972 0.4042 0.0577 0.036 Uiso 1 1 calc R . . H7B H 0.2258 0.3706 0.1449 0.036 Uiso 1 1 calc R . . N8 N 0.19964(10) 0.5135(2) 0.14610(16) 0.0260(7) Uani 1 1 d . . . C9 C 0.25105(12) 0.5415(3) 0.1616(2) 0.0308(9) Uani 1 1 d . . . H9A H 0.2542 0.6157 0.1663 0.037 Uiso 1 1 calc R . . H9B H 0.2668 0.5192 0.1144 0.037 Uiso 1 1 calc R . . C10 C 0.27505(13) 0.4925(3) 0.2412(2) 0.0316(10) Uani 1 1 d . . . H10A H 0.2749 0.4183 0.2340 0.038 Uiso 1 1 calc R . . H10B H 0.3086 0.5150 0.2529 0.038 Uiso 1 1 calc R . . N11 N 0.25000(10) 0.5190(2) 0.31360(17) 0.0256(7) Uani 1 1 d . . . C12 C 0.25049(13) 0.4292(3) 0.3705(2) 0.0322(9) Uani 1 1 d . . . H12A H 0.2367 0.3711 0.3370 0.039 Uiso 1 1 calc R . . H12B H 0.2291 0.4440 0.4119 0.039 Uiso 1 1 calc R . . C13 C 0.29851(13) 0.3971(3) 0.4171(2) 0.0407(11) Uani 1 1 d . . . H13A H 0.2943 0.3381 0.4515 0.061 Uiso 1 1 calc R . . H13B H 0.3123 0.4526 0.4526 0.061 Uiso 1 1 calc R . . H13C H 0.3200 0.3799 0.3772 0.061 Uiso 1 1 calc R . . C14 C 0.27828(12) 0.6034(3) 0.3586(2) 0.0288(9) Uani 1 1 d . . . H14A H 0.2791 0.6603 0.3195 0.035 Uiso 1 1 calc R . . H14B H 0.3115 0.5800 0.3750 0.035 Uiso 1 1 calc R . . C15 C 0.25967(13) 0.6419(3) 0.4353(2) 0.0350(10) Uani 1 1 d . . . H15A H 0.2800 0.6972 0.4599 0.052 Uiso 1 1 calc R . . H15B H 0.2601 0.5871 0.4758 0.052 Uiso 1 1 calc R . . H15C H 0.2270 0.6664 0.4200 0.052 Uiso 1 1 calc R . . C16 C 0.17182(13) 0.5765(3) 0.0812(2) 0.0320(9) Uani 1 1 d . . . H16A H 0.1796 0.5576 0.0259 0.038 Uiso 1 1 calc R . . H16B H 0.1801 0.6484 0.0912 0.038 Uiso 1 1 calc R . . C17 C 0.11930(12) 0.5607(3) 0.08354(19) 0.0321(9) Uani 1 1 d . . . H17A H 0.1005 0.6023 0.0400 0.039 Uiso 1 1 calc R . . H17B H 0.1111 0.4890 0.0718 0.039 Uiso 1 1 calc R . . N18 N 0.10675(10) 0.5890(2) 0.16717(17) 0.0282(7) Uani 1 1 d . . . C19 C 0.09193(14) 0.6983(3) 0.1611(2) 0.0374(10) Uani 1 1 d . . . H19A H 0.1190 0.7384 0.1469 0.045 Uiso 1 1 calc R . . H19B H 0.0654 0.7053 0.1145 0.045 Uiso 1 1 calc R . . C20 C 0.07632(14) 0.7435(3) 0.2378(2) 0.0488(12) Uani 1 1 d . . . H20A H 0.0676 0.8143 0.2272 0.073 Uiso 1 1 calc R . . H20B H 0.1025 0.7392 0.2842 0.073 Uiso 1 1 calc R . . H20C H 0.0487 0.7062 0.2517 0.073 Uiso 1 1 calc R . . C21 C 0.06582(12) 0.5263(3) 0.1860(2) 0.0339(10) Uani 1 1 d . . . H21A H 0.0600 0.5423 0.2431 0.041 Uiso 1 1 calc R . . H21B H 0.0752 0.4544 0.1853 0.041 Uiso 1 1 calc R . . C22 C 0.01892(13) 0.5400(3) 0.1267(2) 0.0488(12) Uani 1 1 d . . . H22A H -0.0055 0.4954 0.1437 0.073 Uiso 1 1 calc R . . H22B H 0.0239 0.5230 0.0700 0.073 Uiso 1 1 calc R . . H22C H 0.0084 0.6102 0.1285 0.073 Uiso 1 1 calc R . . C23 C 0.09938(13) 0.2450(3) 0.3222(2) 0.0287(9) Uani 1 1 d . . . C24 C 0.14537(13) 0.2410(3) 0.3854(2) 0.0423(11) Uani 1 1 d . . . H24A H 0.1654 0.1854 0.3712 0.063 Uiso 1 1 calc R . . H24B H 0.1373 0.2303 0.4412 0.063 Uiso 1 1 calc R . . H24C H 0.1627 0.3048 0.3840 0.063 Uiso 1 1 calc R . . C25 C 0.06872(13) 0.3330(3) 0.3460(2) 0.0350(10) Uani 1 1 d . . . H25A H 0.0391 0.3367 0.3065 0.053 Uiso 1 1 calc R . . H25B H 0.0864 0.3963 0.3446 0.053 Uiso 1 1 calc R . . H25C H 0.0611 0.3221 0.4022 0.053 Uiso 1 1 calc R . . C26 C 0.07200(15) 0.1476(3) 0.3306(2) 0.0474(12) Uani 1 1 d . . . H26A H 0.0425 0.1480 0.2908 0.071 Uiso 1 1 calc R . . H26B H 0.0643 0.1422 0.3871 0.071 Uiso 1 1 calc R . . H26C H 0.0916 0.0899 0.3192 0.071 Uiso 1 1 calc R . . C27 C 0.07487(14) 0.1396(3) 0.0173(2) 0.0344(10) Uani 1 1 d . . . C28 C 0.02890(16) 0.1927(4) -0.0197(3) 0.0759(17) Uani 1 1 d . . . H28A H 0.0091 0.2040 0.0239 0.114 Uiso 1 1 calc R . . H28B H 0.0115 0.1506 -0.0636 0.114 Uiso 1 1 calc R . . H28C H 0.0366 0.2576 -0.0433 0.114 Uiso 1 1 calc R . . C29 C 0.06325(15) 0.0354(3) 0.0492(2) 0.0522(12) Uani 1 1 d . . . H29A H 0.0433 0.0428 0.0931 0.078 Uiso 1 1 calc R . . H29B H 0.0929 0.0008 0.0715 0.078 Uiso 1 1 calc R . . H29C H 0.0461 -0.0042 0.0034 0.078 Uiso 1 1 calc R . . C30 C 0.10581(15) 0.1215(3) -0.0515(2) 0.0543(13) Uani 1 1 d . . . H30A H 0.0884 0.0788 -0.0949 0.081 Uiso 1 1 calc R . . H30B H 0.1355 0.0879 -0.0278 0.081 Uiso 1 1 calc R . . H30C H 0.1132 0.1863 -0.0756 0.081 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cr 0.0289(4) 0.0225(4) 0.0211(3) -0.0006(3) 0.0038(3) -0.0011(3) Cl1 0.0427(6) 0.0232(5) 0.0363(5) 0.0015(4) 0.0013(4) -0.0051(5) Cl2 0.0357(6) 0.0347(6) 0.0264(5) -0.0039(4) 0.0080(4) 0.0020(4) O1 0.0309(15) 0.0254(15) 0.0227(13) -0.0015(11) 0.0029(11) -0.0004(12) C1 0.024(2) 0.021(2) 0.026(2) 0.0001(16) -0.0007(17) 0.0015(17) C2 0.026(2) 0.021(2) 0.029(2) 0.0012(17) 0.0006(17) 0.0041(17) C3 0.030(2) 0.021(2) 0.033(2) 0.0007(17) 0.0029(18) -0.0059(17) C4 0.026(2) 0.022(2) 0.031(2) -0.0019(17) -0.0035(17) -0.0001(17) C5 0.028(2) 0.028(2) 0.0194(19) -0.0020(16) 0.0009(16) -0.0009(18) C6 0.027(2) 0.025(2) 0.023(2) 0.0040(16) 0.0043(17) -0.0019(18) C7 0.038(2) 0.027(2) 0.026(2) -0.0067(17) 0.0084(18) -0.0049(19) N8 0.0313(19) 0.0233(18) 0.0237(17) -0.0031(13) 0.0045(14) -0.0071(15) C9 0.033(2) 0.030(2) 0.031(2) -0.0064(18) 0.0089(17) -0.0092(19) C10 0.034(2) 0.030(2) 0.031(2) -0.0099(17) 0.0065(18) -0.0020(18) N11 0.0291(18) 0.0203(18) 0.0277(17) -0.0038(13) 0.0057(14) -0.0021(14) C12 0.035(2) 0.030(3) 0.029(2) 0.0005(18) 0.0000(18) 0.0000(19) C13 0.042(3) 0.036(3) 0.040(2) -0.0029(19) -0.008(2) 0.003(2) C14 0.027(2) 0.026(2) 0.033(2) -0.0035(17) 0.0019(17) -0.0049(18) C15 0.039(3) 0.035(3) 0.031(2) -0.0094(19) 0.0049(19) -0.0063(19) C16 0.044(2) 0.029(2) 0.023(2) 0.0024(17) 0.0039(18) -0.0059(19) C17 0.039(2) 0.032(2) 0.022(2) 0.0053(17) -0.0032(17) -0.002(2) N18 0.0324(19) 0.0226(18) 0.0292(17) 0.0024(14) 0.0030(14) -0.0029(15) C19 0.042(3) 0.029(3) 0.038(2) 0.0041(19) -0.003(2) 0.001(2) C20 0.048(3) 0.039(3) 0.057(3) -0.005(2) 0.002(2) 0.014(2) C21 0.033(2) 0.031(2) 0.037(2) 0.0065(19) 0.0031(19) -0.0011(19) C22 0.033(2) 0.055(3) 0.054(3) 0.013(2) -0.006(2) -0.006(2) C23 0.031(2) 0.028(2) 0.026(2) 0.0082(17) 0.0014(17) -0.0003(18) C24 0.043(3) 0.050(3) 0.033(2) 0.012(2) 0.003(2) 0.005(2) C25 0.036(2) 0.040(3) 0.031(2) 0.0049(18) 0.0084(19) 0.002(2) C26 0.063(3) 0.041(3) 0.039(2) 0.009(2) 0.011(2) -0.017(2) C27 0.033(3) 0.031(2) 0.035(2) -0.0043(19) -0.0061(19) -0.0041(19) C28 0.065(4) 0.068(4) 0.078(4) -0.019(3) -0.045(3) 0.011(3) C29 0.065(3) 0.042(3) 0.047(3) -0.012(2) 0.000(2) -0.023(2) C30 0.072(3) 0.053(3) 0.037(2) -0.018(2) 0.005(2) -0.023(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 Cr O1 1.915(2) . ? Cr N8 2.107(3) . ? Cr N11 2.259(3) . ? Cr N18 2.283(3) . ? Cr Cl2 2.3337(10) . ? Cr Cl1 2.3615(11) . ? O1 C1 1.349(4) . ? C1 C6 1.390(4) . ? C1 C2 1.426(5) . ? C2 C3 1.398(5) . ? C2 C23 1.538(4) . ? C3 C4 1.392(5) . ? C4 C5 1.388(5) . ? C4 C27 1.533(5) . ? C5 C6 1.391(4) . ? C6 C7 1.506(5) . ? C7 N8 1.507(4) . ? N8 C16 1.480(4) . ? N8 C9 1.490(4) . ? C9 C10 1.518(5) . ? C10 N11 1.505(4) . ? N11 C14 1.502(4) . ? N11 C12 1.507(4) . ? C12 C13 1.519(5) . ? C14 C15 1.515(4) . ? C16 C17 1.510(5) . ? C17 N18 1.505(4) . ? N18 C21 1.496(4) . ? N18 C19 1.508(4) . ? C19 C20 1.508(5) . ? C21 C22 1.534(4) . ? C23 C26 1.524(5) . ? C23 C24 1.538(5) . ? C23 C25 1.540(5) . ? C27 C28 1.525(5) . ? C27 C29 1.530(5) . ? C27 C30 1.540(5) . ? 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 O1 Cr N8 89.13(10) . . ? O1 Cr N11 89.78(10) . . ? N8 Cr N11 82.66(11) . . ? O1 Cr N18 96.83(10) . . ? N8 Cr N18 82.11(11) . . ? N11 Cr N18 163.29(10) . . ? O1 Cr Cl2 86.62(7) . . ? N8 Cr Cl2 175.44(9) . . ? N11 Cr Cl2 98.96(7) . . ? N18 Cr Cl2 96.74(7) . . ? O1 Cr Cl1 175.56(8) . . ? N8 Cr Cl1 92.56(8) . . ? N11 Cr Cl1 86.37(8) . . ? N18 Cr Cl1 87.47(8) . . ? Cl2 Cr Cl1 91.79(4) . . ? C1 O1 Cr 131.4(2) . . ? O1 C1 C6 119.7(3) . . ? O1 C1 C2 121.2(3) . . ? C6 C1 C2 119.1(3) . . ? C3 C2 C1 116.7(3) . . ? C3 C2 C23 120.6(3) . . ? C1 C2 C23 122.7(3) . . ? C4 C3 C2 124.7(3) . . ? C5 C4 C3 116.5(3) . . ? C5 C4 C27 121.3(3) . . ? C3 C4 C27 122.1(3) . . ? C4 C5 C6 121.3(3) . . ? C1 C6 C5 121.2(3) . . ? C1 C6 C7 119.7(3) . . ? C5 C6 C7 118.5(3) . . ? C6 C7 N8 119.3(3) . . ? C16 N8 C9 112.7(3) . . ? C16 N8 C7 108.9(3) . . ? C9 N8 C7 107.6(3) . . ? C16 N8 Cr 105.6(2) . . ? C9 N8 Cr 104.82(19) . . ? C7 N8 Cr 117.4(2) . . ? N8 C9 C10 110.0(3) . . ? N11 C10 C9 111.3(3) . . ? C14 N11 C10 106.0(3) . . ? C14 N11 C12 109.5(3) . . ? C10 N11 C12 109.5(3) . . ? C14 N11 Cr 118.4(2) . . ? C10 N11 Cr 105.0(2) . . ? C12 N11 Cr 108.1(2) . . ? N11 C12 C13 117.0(3) . . ? N11 C14 C15 115.3(3) . . ? N8 C16 C17 109.1(3) . . ? N18 C17 C16 110.7(3) . . ? C21 N18 C17 110.0(3) . . ? C21 N18 C19 109.3(3) . . ? C17 N18 C19 106.4(3) . . ? C21 N18 Cr 109.6(2) . . ? C17 N18 Cr 103.79(19) . . ? C19 N18 Cr 117.5(2) . . ? C20 C19 N18 116.2(3) . . ? N18 C21 C22 115.6(3) . . ? C26 C23 C24 107.7(3) . . ? C26 C23 C2 112.5(3) . . ? C24 C23 C2 110.4(3) . . ? C26 C23 C25 107.8(3) . . ? C24 C23 C25 108.2(3) . . ? C2 C23 C25 110.0(3) . . ? C28 C27 C29 109.7(3) . . ? C28 C27 C4 108.6(3) . . ? C29 C27 C4 111.3(3) . . ? C28 C27 C30 109.3(3) . . ? C29 C27 C30 106.3(3) . . ? C4 C27 C30 111.5(3) . . ? _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 71.21 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 0.254 _refine_diff_density_min -0.270 _refine_diff_density_rms 0.051 #===END data_Compound_10c _database_code_depnum_ccdc_archive 'CCDC 293286' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H36 Cl Co N O3' _chemical_formula_weight 444.89 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' Co Co 0.3494 0.9721 '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 11.9832(5) _cell_length_b 12.9061(7) _cell_length_c 15.6009(7) _cell_angle_alpha 90.00 _cell_angle_beta 106.512(4) _cell_angle_gamma 90.00 _cell_volume 2313.28(19) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 3.9580 _cell_measurement_theta_max 32.6383 _exptl_crystal_description 'platy needles' _exptl_crystal_colour Lilac _exptl_crystal_size_max 0.39 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.277 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 948 _exptl_absorpt_coefficient_mu 0.877 _exptl_absorpt_correction_type 'numeric analytical' _exptl_absorpt_correction_T_min 0.77156 _exptl_absorpt_correction_T_max 0.97924 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'OD Xcalibur 3' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 15.9863 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24396 _diffrn_reflns_av_R_equivalents 0.0240 _diffrn_reflns_av_sigmaI/netI 0.0271 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 4.12 _diffrn_reflns_theta_max 32.70 _reflns_number_total 7904 _reflns_number_gt 6268 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd' _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^)+(0.0519P)^2^+0.1551P] 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 7904 _refine_ls_number_parameters 246 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0485 _refine_ls_R_factor_gt 0.0363 _refine_ls_wR_factor_ref 0.1001 _refine_ls_wR_factor_gt 0.0939 _refine_ls_goodness_of_fit_ref 1.137 _refine_ls_restrained_S_all 1.137 _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 Co Co 0.447271(15) 0.670944(13) 0.272269(11) 0.02123(6) Uani 1 1 d . . . Cl Cl 0.39656(4) 0.74145(3) 0.39085(3) 0.04472(11) Uani 1 1 d . . . O1 O 0.60876(8) 0.70325(7) 0.30152(6) 0.02384(18) Uani 1 1 d . . . C1 C 0.69256(11) 0.65667(9) 0.27536(8) 0.0210(2) Uani 1 1 d . . . C2 C 0.80517(11) 0.64172(10) 0.33585(8) 0.0228(2) Uani 1 1 d . . . C3 C 0.88912(11) 0.59282(10) 0.30444(9) 0.0267(3) Uani 1 1 d . . . H3A H 0.9646 0.5842 0.3447 0.032 Uiso 1 1 calc R . . C4 C 0.86905(11) 0.55542(11) 0.21678(9) 0.0259(2) Uani 1 1 d . . . C5 C 0.75856(11) 0.57122(10) 0.15937(9) 0.0252(2) Uani 1 1 d . . . H5A H 0.7416 0.5471 0.0995 0.030 Uiso 1 1 calc R . . C6 C 0.67166(11) 0.62151(10) 0.18686(8) 0.0232(2) Uani 1 1 d . . . C7 C 0.55537(11) 0.64055(11) 0.12035(9) 0.0261(3) Uani 1 1 d . . . H7A H 0.5444 0.7161 0.1109 0.031 Uiso 1 1 calc R . . H7B H 0.5553 0.6090 0.0625 0.031 Uiso 1 1 calc R . . N8 N 0.45496(9) 0.59793(8) 0.14826(7) 0.0232(2) Uani 1 1 d . . . C9 C 0.34506(12) 0.62156(12) 0.07854(9) 0.0304(3) Uani 1 1 d . . . H9A H 0.2826 0.5754 0.0862 0.037 Uiso 1 1 calc R . . H9B H 0.3554 0.6081 0.0188 0.037 Uiso 1 1 calc R . . C10 C 0.30970(13) 0.73244(13) 0.08388(9) 0.0332(3) Uani 1 1 d . . . H10A H 0.3634 0.7794 0.0646 0.040 Uiso 1 1 calc R . . H10B H 0.2298 0.7440 0.0448 0.040 Uiso 1 1 calc R . . O11 O 0.31487(9) 0.75165(8) 0.17555(7) 0.0309(2) Uani 1 1 d . . . C12 C 0.26372(17) 0.84865(14) 0.18692(13) 0.0480(5) Uani 1 1 d . . . H12A H 0.1818 0.8492 0.1516 0.072 Uiso 1 1 calc R . . H12B H 0.3052 0.9048 0.1667 0.072 Uiso 1 1 calc R . . H12C H 0.2690 0.8586 0.2502 0.072 Uiso 1 1 calc R . . C13 C 0.46784(13) 0.48531(11) 0.16333(11) 0.0319(3) Uani 1 1 d . . . H13A H 0.5509 0.4684 0.1910 0.038 Uiso 1 1 calc R . . H13B H 0.4417 0.4486 0.1053 0.038 Uiso 1 1 calc R . . C14 C 0.39720(14) 0.44938(11) 0.22348(12) 0.0364(3) Uani 1 1 d . . . H14A H 0.3130 0.4554 0.1926 0.044 Uiso 1 1 calc R . . H14B H 0.4150 0.3761 0.2407 0.044 Uiso 1 1 calc R . . O15 O 0.42817(11) 0.51465(8) 0.30113(7) 0.0364(2) Uani 1 1 d . . . C16 C 0.3821(2) 0.47822(15) 0.37093(14) 0.0553(5) Uani 1 1 d . . . H16A H 0.4156 0.4103 0.3916 0.083 Uiso 1 1 calc R . . H16B H 0.2973 0.4721 0.3481 0.083 Uiso 1 1 calc R . . H16C H 0.4019 0.5273 0.4209 0.083 Uiso 1 1 calc R . . C17 C 0.83068(12) 0.67488(10) 0.43438(9) 0.0258(3) Uani 1 1 d . . . C18 C 0.79767(13) 0.78859(11) 0.44348(10) 0.0335(3) Uani 1 1 d . . . H18A H 0.7151 0.7989 0.4121 0.050 Uiso 1 1 calc R . . H18B H 0.8451 0.8337 0.4173 0.050 Uiso 1 1 calc R . . H18C H 0.8117 0.8057 0.5069 0.050 Uiso 1 1 calc R . . C19 C 0.76071(16) 0.60652(14) 0.48053(11) 0.0413(4) Uani 1 1 d . . . H19A H 0.6777 0.6122 0.4489 0.062 Uiso 1 1 calc R . . H19B H 0.7741 0.6293 0.5426 0.062 Uiso 1 1 calc R . . H19C H 0.7855 0.5343 0.4797 0.062 Uiso 1 1 calc R . . C20 C 0.96030(14) 0.66411(12) 0.48539(11) 0.0369(3) Uani 1 1 d . . . H20A H 0.9853 0.5925 0.4811 0.055 Uiso 1 1 calc R . . H20B H 0.9720 0.6822 0.5484 0.055 Uiso 1 1 calc R . . H20C H 1.0062 0.7108 0.4593 0.055 Uiso 1 1 calc R . . C21 C 0.96736(12) 0.50291(12) 0.18788(10) 0.0322(3) Uani 1 1 d . . . C22 C 1.02394(16) 0.41690(14) 0.25343(12) 0.0455(4) Uani 1 1 d . . . H22A H 0.9653 0.3647 0.2553 0.068 Uiso 1 1 calc R . . H22B H 1.0563 0.4465 0.3132 0.068 Uiso 1 1 calc R . . H22C H 1.0864 0.3845 0.2338 0.068 Uiso 1 1 calc R . . C23 C 1.05943(16) 0.58381(16) 0.18425(15) 0.0532(5) Uani 1 1 d . . . H23A H 1.0898 0.6160 0.2432 0.080 Uiso 1 1 calc R . . H23B H 1.0242 0.6371 0.1401 0.080 Uiso 1 1 calc R . . H23C H 1.1232 0.5501 0.1671 0.080 Uiso 1 1 calc R . . C24 C 0.92190(16) 0.45433(16) 0.09474(12) 0.0490(4) Uani 1 1 d . . . H24A H 0.8635 0.4015 0.0957 0.073 Uiso 1 1 calc R . . H24B H 0.9867 0.4222 0.0778 0.073 Uiso 1 1 calc R . . H24C H 0.8865 0.5082 0.0512 0.073 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co 0.02131(9) 0.02296(9) 0.02031(9) -0.00239(6) 0.00734(6) -0.00141(6) Cl 0.0596(3) 0.0496(2) 0.03320(19) -0.01019(16) 0.02662(18) 0.00094(19) O1 0.0203(4) 0.0260(4) 0.0249(4) -0.0053(3) 0.0059(3) -0.0009(3) C1 0.0197(5) 0.0207(5) 0.0225(6) 0.0020(4) 0.0056(4) -0.0016(4) C2 0.0219(5) 0.0225(5) 0.0224(6) 0.0015(4) 0.0039(4) -0.0030(4) C3 0.0203(6) 0.0304(6) 0.0277(6) 0.0036(5) 0.0038(5) 0.0008(5) C4 0.0219(6) 0.0306(6) 0.0266(6) 0.0040(5) 0.0092(5) 0.0022(5) C5 0.0233(6) 0.0314(6) 0.0221(6) 0.0017(5) 0.0085(4) 0.0019(5) C6 0.0192(5) 0.0304(6) 0.0200(5) 0.0011(5) 0.0055(4) -0.0005(5) C7 0.0213(6) 0.0364(7) 0.0205(6) 0.0011(5) 0.0060(4) 0.0029(5) N8 0.0197(5) 0.0263(5) 0.0226(5) -0.0042(4) 0.0042(4) 0.0018(4) C9 0.0209(6) 0.0452(8) 0.0228(6) -0.0086(5) 0.0021(5) 0.0036(5) C10 0.0271(7) 0.0463(8) 0.0247(6) 0.0014(6) 0.0047(5) 0.0106(6) O11 0.0291(5) 0.0362(5) 0.0269(5) -0.0034(4) 0.0073(4) 0.0103(4) C12 0.0430(9) 0.0431(9) 0.0483(10) -0.0132(7) -0.0026(7) 0.0203(7) C13 0.0301(7) 0.0251(6) 0.0410(8) -0.0095(6) 0.0108(6) -0.0003(5) C14 0.0371(8) 0.0231(6) 0.0514(9) -0.0072(6) 0.0165(7) -0.0057(6) O15 0.0499(7) 0.0282(5) 0.0347(6) 0.0011(4) 0.0176(5) -0.0087(5) C16 0.0795(15) 0.0447(10) 0.0511(11) 0.0138(8) 0.0336(11) -0.0084(10) C17 0.0249(6) 0.0276(6) 0.0222(6) 0.0008(5) 0.0023(5) -0.0021(5) C18 0.0317(7) 0.0316(7) 0.0321(7) -0.0076(6) 0.0007(5) -0.0013(6) C19 0.0503(10) 0.0471(9) 0.0262(7) 0.0055(6) 0.0105(6) -0.0132(7) C20 0.0300(7) 0.0416(8) 0.0307(7) -0.0032(6) -0.0047(6) 0.0038(6) C21 0.0243(6) 0.0427(8) 0.0314(7) 0.0060(6) 0.0111(5) 0.0091(6) C22 0.0408(9) 0.0549(10) 0.0432(9) 0.0118(8) 0.0158(7) 0.0209(8) C23 0.0320(8) 0.0640(12) 0.0718(13) 0.0122(10) 0.0281(9) 0.0035(8) C24 0.0397(9) 0.0703(12) 0.0384(9) -0.0037(8) 0.0134(7) 0.0235(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co O1 1.9040(9) . ? Co O15 2.0934(10) . ? Co O11 2.1256(10) . ? Co N8 2.1773(10) . ? Co Cl 2.2932(4) . ? O1 C1 1.3301(15) . ? C1 C6 1.4066(17) . ? C1 C2 1.4229(17) . ? C2 C3 1.3895(18) . ? C2 C17 1.5402(18) . ? C3 C4 1.4051(19) . ? C4 C5 1.3865(18) . ? C4 C21 1.5338(19) . ? C5 C6 1.3941(17) . ? C6 C7 1.5023(18) . ? C7 N8 1.4958(17) . ? N8 C13 1.4734(17) . ? N8 C9 1.4820(17) . ? C9 C10 1.501(2) . ? C10 O11 1.4355(17) . ? O11 C12 1.4270(18) . ? C13 C14 1.505(2) . ? C14 O15 1.4351(18) . ? O15 C16 1.433(2) . ? C17 C19 1.531(2) . ? C17 C18 1.537(2) . ? C17 C20 1.537(2) . ? C21 C22 1.531(2) . ? C21 C23 1.532(2) . ? C21 C24 1.533(2) . ? 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 O1 Co O15 108.98(4) . . ? O1 Co O11 124.44(4) . . ? O15 Co O11 121.31(4) . . ? O1 Co N8 90.62(4) . . ? O15 Co N8 78.98(4) . . ? O11 Co N8 78.05(4) . . ? O1 Co Cl 101.78(3) . . ? O15 Co Cl 97.96(3) . . ? O11 Co Cl 93.60(3) . . ? N8 Co Cl 167.53(3) . . ? C1 O1 Co 129.20(8) . . ? O1 C1 C6 120.50(11) . . ? O1 C1 C2 120.95(11) . . ? C6 C1 C2 118.55(11) . . ? C3 C2 C1 118.23(12) . . ? C3 C2 C17 121.32(12) . . ? C1 C2 C17 120.40(12) . . ? C2 C3 C4 123.95(12) . . ? C5 C4 C3 116.49(12) . . ? C5 C4 C21 123.19(12) . . ? C3 C4 C21 120.30(12) . . ? C4 C5 C6 121.97(12) . . ? C5 C6 C1 120.79(11) . . ? C5 C6 C7 119.41(11) . . ? C1 C6 C7 119.78(11) . . ? N8 C7 C6 113.81(10) . . ? C13 N8 C9 110.55(11) . . ? C13 N8 C7 110.66(10) . . ? C9 N8 C7 109.34(10) . . ? C13 N8 Co 108.31(8) . . ? C9 N8 Co 108.05(8) . . ? C7 N8 Co 109.89(8) . . ? N8 C9 C10 111.18(11) . . ? O11 C10 C9 106.68(11) . . ? C12 O11 C10 112.15(12) . . ? C12 O11 Co 127.02(9) . . ? C10 O11 Co 115.77(8) . . ? N8 C13 C14 110.58(11) . . ? O15 C14 C13 106.81(11) . . ? C16 O15 C14 112.69(13) . . ? C16 O15 Co 124.67(11) . . ? C14 O15 Co 113.70(9) . . ? C19 C17 C18 108.49(13) . . ? C19 C17 C20 108.20(12) . . ? C18 C17 C20 106.69(11) . . ? C19 C17 C2 109.24(11) . . ? C18 C17 C2 111.97(11) . . ? C20 C17 C2 112.11(12) . . ? C22 C21 C23 109.39(14) . . ? C22 C21 C24 107.88(14) . . ? C23 C21 C24 108.03(15) . . ? C22 C21 C4 110.82(12) . . ? C23 C21 C4 109.35(13) . . ? C24 C21 C4 111.31(12) . . ? _diffrn_measured_fraction_theta_max 0.928 _diffrn_reflns_theta_full 32.70 _diffrn_measured_fraction_theta_full 0.928 _refine_diff_density_max 0.581 _refine_diff_density_min -0.518 _refine_diff_density_rms 0.059 #===END #===END data_Compound_4c _database_code_depnum_ccdc_archive 'CCDC 293483' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H72 Mg N2 O6' _chemical_formula_weight 725.33 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' Mg Mg 0.0486 0.0363 '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)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 15.7123(6) _cell_length_b 30.5819(12) _cell_length_c 18.7720(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.923(3) _cell_angle_gamma 90.00 _cell_volume 9019.0(6) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 3.8832 _cell_measurement_theta_max 32.6826 _exptl_crystal_description 'blocky needles' _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.068 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3184 _exptl_absorpt_coefficient_mu 0.082 _exptl_absorpt_correction_type 'numeric analytical' _exptl_absorpt_correction_T_min 0.98889 _exptl_absorpt_correction_T_max 0.99420 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'OD Xcalibur 3' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 15.9863 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 90554 _diffrn_reflns_av_R_equivalents 0.1039 _diffrn_reflns_av_sigmaI/netI 0.1516 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -45 _diffrn_reflns_limit_k_max 45 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.95 _diffrn_reflns_theta_max 32.75 _reflns_number_total 30993 _reflns_number_gt 24491 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd' _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^)+(0.1000P)^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 30993 _refine_ls_number_parameters 949 _refine_ls_number_restraints 78 _refine_ls_R_factor_all 0.3374 _refine_ls_R_factor_gt 0.2975 _refine_ls_wR_factor_ref 0.4586 _refine_ls_wR_factor_gt 0.4465 _refine_ls_goodness_of_fit_ref 2.088 _refine_ls_restrained_S_all 2.097 _refine_ls_shift/su_max 0.066 _refine_ls_shift/su_mean 0.007 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 Mg Mg 0.22458(10) -0.00030(5) 0.71892(9) 0.0231(4) Uani 1 1 d . . . O1 O 0.1738(2) 0.04208(12) 0.65095(18) 0.0271(8) Uani 1 1 d . . . C1 C 0.0991(3) 0.06207(16) 0.6441(2) 0.0210(10) Uani 1 1 d U . . C2 C 0.0687(3) 0.08047(16) 0.5791(2) 0.0215(10) Uani 1 1 d . . . C3 C -0.0091(3) 0.10218(19) 0.5777(3) 0.0325(13) Uani 1 1 d . . . H3A H -0.0277 0.1149 0.5339 0.039 Uiso 1 1 calc R . . C4 C -0.0623(3) 0.10653(17) 0.6373(3) 0.0248(11) Uani 1 1 d U . . C5 C -0.0330(3) 0.08623(16) 0.6994(3) 0.0253(11) Uani 1 1 d . . . H5A H -0.0680 0.0872 0.7402 0.030 Uiso 1 1 calc R . . C6 C 0.0442(3) 0.06474(17) 0.7048(3) 0.0235(11) Uani 1 1 d . . . C7 C 0.0715(3) 0.04436(17) 0.7731(3) 0.0262(11) Uani 1 1 d . . . H7A H 0.0256 0.0479 0.8081 0.031 Uiso 1 1 calc R . . H7B H 0.1223 0.0600 0.7918 0.031 Uiso 1 1 calc R . . N8 N 0.0923(3) -0.00309(13) 0.7668(2) 0.0235(9) Uani 1 1 d . . . C9 C 0.1087(4) -0.02157(17) 0.8383(3) 0.0307(13) Uani 1 1 d . . . H9A H 0.0542 -0.0250 0.8634 0.037 Uiso 1 1 calc R . . H9B H 0.1450 -0.0012 0.8663 0.037 Uiso 1 1 calc R . . C10 C 0.1524(4) -0.06540(19) 0.8333(3) 0.0378(14) Uani 1 1 d . . . H10A H 0.1785 -0.0733 0.8799 0.045 Uiso 1 1 calc R . . H10B H 0.1107 -0.0883 0.8198 0.045 Uiso 1 1 calc R . . O11 O 0.2173(2) -0.06183(12) 0.7797(2) 0.0355(10) Uani 1 1 d . . . C12 C 0.2697(4) -0.0997(2) 0.7783(4) 0.0476(17) Uani 1 1 d . . . H12A H 0.3048 -0.1009 0.8219 0.071 Uiso 1 1 calc R . . H12B H 0.3066 -0.0985 0.7367 0.071 Uiso 1 1 calc R . . H12C H 0.2338 -0.1259 0.7754 0.071 Uiso 1 1 calc R . . C13 C 0.0248(4) -0.02741(18) 0.7263(3) 0.0330(13) Uani 1 1 d . . . H13A H 0.0399 -0.0588 0.7275 0.040 Uiso 1 1 calc R . . H13B H 0.0271 -0.0179 0.6760 0.040 Uiso 1 1 calc R . . C14 C -0.0664(4) -0.0231(2) 0.7501(4) 0.0496(17) Uani 1 1 d . . . H14A H -0.0790 0.0080 0.7602 0.060 Uiso 1 1 calc R . . H14B H -0.1053 -0.0330 0.7114 0.060 Uiso 1 1 calc R . . O15 O -0.0802(3) -0.0479(2) 0.8107(3) 0.0801(18) Uani 1 1 d . . . C16 C -0.1660(5) -0.0453(4) 0.8343(6) 0.106(4) Uani 1 1 d . . . H16A H -0.1724 -0.0632 0.8772 0.160 Uiso 1 1 calc R . . H16B H -0.2045 -0.0562 0.7967 0.160 Uiso 1 1 calc R . . H16C H -0.1801 -0.0149 0.8451 0.160 Uiso 1 1 calc R . . C17 C 0.1214(3) 0.07588(18) 0.5102(3) 0.0277(12) Uani 1 1 d . . . C18 C 0.1333(4) 0.0266(2) 0.4933(3) 0.0413(15) Uani 1 1 d . . . H18A H 0.1664 0.0234 0.4498 0.062 Uiso 1 1 calc R . . H18B H 0.0774 0.0128 0.4863 0.062 Uiso 1 1 calc R . . H18C H 0.1635 0.0124 0.5330 0.062 Uiso 1 1 calc R . . C19 C 0.2088(4) 0.0987(2) 0.5202(3) 0.0365(14) Uani 1 1 d . . . H19A H 0.2416 0.0957 0.4765 0.055 Uiso 1 1 calc R . . H19B H 0.2401 0.0851 0.5599 0.055 Uiso 1 1 calc R . . H19C H 0.2001 0.1298 0.5304 0.055 Uiso 1 1 calc R . . C20 C 0.0780(4) 0.0973(2) 0.4448(3) 0.0465(17) Uani 1 1 d . . . H20A H 0.1139 0.0934 0.4030 0.070 Uiso 1 1 calc R . . H20B H 0.0700 0.1286 0.4538 0.070 Uiso 1 1 calc R . . H20C H 0.0226 0.0835 0.4359 0.070 Uiso 1 1 calc R . . C21 C -0.1499(3) 0.1291(2) 0.6342(3) 0.0426(16) Uani 1 1 d . . . C22 C -0.1641(4) 0.1555(3) 0.5661(3) 0.059(2) Uani 1 1 d . . . H22A H -0.2208 0.1689 0.5666 0.088 Uiso 1 1 calc R . . H22B H -0.1599 0.1362 0.5247 0.088 Uiso 1 1 calc R . . H22C H -0.1208 0.1785 0.5632 0.088 Uiso 1 1 calc R . . C23 C -0.2175(4) 0.0944(3) 0.6417(5) 0.072(2) Uani 1 1 d . . . H23A H -0.2739 0.1081 0.6402 0.108 Uiso 1 1 calc R . . H23B H -0.2093 0.0792 0.6872 0.108 Uiso 1 1 calc R . . H23C H -0.2131 0.0734 0.6025 0.108 Uiso 1 1 calc R . . C24 C -0.1569(5) 0.1609(2) 0.6972(4) 0.0522(18) Uani 1 1 d . . . H24A H -0.2130 0.1750 0.6959 0.078 Uiso 1 1 calc R . . H24B H -0.1125 0.1833 0.6940 0.078 Uiso 1 1 calc R . . H24C H -0.1497 0.1448 0.7420 0.078 Uiso 1 1 calc R . . O31 O 0.2752(2) 0.03006(12) 0.80235(18) 0.0281(8) Uani 1 1 d . . . C31 C 0.3479(3) 0.05007(17) 0.8162(3) 0.0246(11) Uani 1 1 d . . . C32 C 0.3770(4) 0.05904(19) 0.8864(3) 0.0328(13) Uani 1 1 d . . . C33 C 0.4527(4) 0.0827(2) 0.8977(3) 0.0383(14) Uani 1 1 d . . . H33A H 0.4700 0.0892 0.9452 0.046 Uiso 1 1 calc R . . C34 C 0.5032(4) 0.0969(2) 0.8423(3) 0.0429(16) Uani 1 1 d . A . C35 C 0.4775(4) 0.08550(19) 0.7738(3) 0.0355(13) Uani 1 1 d . . . H35A H 0.5117 0.0938 0.7349 0.043 Uiso 1 1 calc R . . C36 C 0.4024(3) 0.06213(17) 0.7607(3) 0.0269(11) Uani 1 1 d . . . C37 C 0.3783(3) 0.05090(16) 0.6846(3) 0.0241(11) Uani 1 1 d . . . H37A H 0.3280 0.0684 0.6702 0.029 Uiso 1 1 calc R . . H37B H 0.4258 0.0592 0.6533 0.029 Uiso 1 1 calc R . . N38 N 0.3588(3) 0.00410(14) 0.6737(2) 0.0257(9) Uani 1 1 d . . . C39 C 0.3451(3) -0.00439(18) 0.5975(3) 0.0299(12) Uani 1 1 d . . . H39A H 0.4008 -0.0047 0.5736 0.036 Uiso 1 1 calc R . . H39B H 0.3109 0.0197 0.5765 0.036 Uiso 1 1 calc R . . C40 C 0.3006(3) -0.04685(17) 0.5834(3) 0.0290(12) Uani 1 1 d . . . H40A H 0.2801 -0.0482 0.5333 0.035 Uiso 1 1 calc R . . H40B H 0.3398 -0.0717 0.5922 0.035 Uiso 1 1 calc R . . O41 O 0.2298(2) -0.04890(12) 0.6311(2) 0.0320(9) Uani 1 1 d . . . C42 C 0.1738(4) -0.08454(19) 0.6140(4) 0.0416(15) Uani 1 1 d . . . H42A H 0.1372 -0.0764 0.5733 0.062 Uiso 1 1 calc R . . H42B H 0.1385 -0.0912 0.6551 0.062 Uiso 1 1 calc R . . H42C H 0.2075 -0.1104 0.6017 0.062 Uiso 1 1 calc R . . C43 C 0.4232(3) -0.02624(18) 0.7065(3) 0.0291(12) Uani 1 1 d . . . H43A H 0.4105 -0.0562 0.6894 0.035 Uiso 1 1 calc R . . H43B H 0.4150 -0.0261 0.7587 0.035 Uiso 1 1 calc R . . C44 C 0.5171(4) -0.0170(2) 0.6929(3) 0.0409(15) Uani 1 1 d . . . H44A H 0.5300 0.0137 0.7057 0.049 Uiso 1 1 calc R . . H44B H 0.5527 -0.0362 0.7237 0.049 Uiso 1 1 calc R . . O45 O 0.5375(3) -0.02412(15) 0.6216(2) 0.0497(12) Uani 1 1 d . . . C46 C 0.6253(4) -0.0166(3) 0.6088(5) 0.063(2) Uani 1 1 d . . . H46A H 0.6371 -0.0220 0.5584 0.094 Uiso 1 1 calc R . . H46B H 0.6598 -0.0364 0.6385 0.094 Uiso 1 1 calc R . . H46C H 0.6396 0.0138 0.6206 0.094 Uiso 1 1 calc R . . C47 C 0.3247(4) 0.0431(3) 0.9515(3) 0.0490(18) Uani 1 1 d . . . C48 C 0.2398(5) 0.0661(3) 0.9508(4) 0.071(2) Uani 1 1 d . . . H48A H 0.2068 0.0566 0.9918 0.106 Uiso 1 1 calc R . . H48B H 0.2086 0.0589 0.9067 0.106 Uiso 1 1 calc R . . H48C H 0.2488 0.0978 0.9534 0.106 Uiso 1 1 calc R . . C49 C 0.3150(5) -0.0066(3) 0.9466(4) 0.065(2) Uani 1 1 d . . . H49A H 0.2824 -0.0171 0.9873 0.097 Uiso 1 1 calc R . . H49B H 0.3714 -0.0203 0.9473 0.097 Uiso 1 1 calc R . . H49C H 0.2850 -0.0142 0.9022 0.097 Uiso 1 1 calc R . . C50 C 0.3689(6) 0.0535(4) 1.0241(4) 0.082(3) Uani 1 1 d . . . H50A H 0.3332 0.0431 1.0630 0.123 Uiso 1 1 calc R . . H50B H 0.3770 0.0852 1.0285 0.123 Uiso 1 1 calc R . . H50C H 0.4243 0.0389 1.0267 0.123 Uiso 1 1 calc R . . C51 C 0.5858(5) 0.1226(3) 0.8590(4) 0.069(2) Uani 1 1 d D . . C52 C 0.5597(8) 0.1641(4) 0.9070(6) 0.073(5) Uani 0.649(16) 1 d PD A 1 H52A H 0.5021 0.1737 0.8937 0.109 Uiso 0.649(16) 1 calc PR A 1 H52B H 0.5999 0.1881 0.8991 0.109 Uiso 0.649(16) 1 calc PR A 1 H52C H 0.5614 0.1558 0.9575 0.109 Uiso 0.649(16) 1 calc PR A 1 C53 C 0.6434(8) 0.0973(5) 0.9079(8) 0.090(6) Uani 0.649(16) 1 d PDU A 1 H53A H 0.6347 0.1067 0.9572 0.135 Uiso 0.649(16) 1 calc PR A 1 H53B H 0.7028 0.1025 0.8950 0.135 Uiso 0.649(16) 1 calc PR A 1 H53C H 0.6306 0.0660 0.9036 0.135 Uiso 0.649(16) 1 calc PR A 1 C54 C 0.6278(7) 0.1409(4) 0.7955(6) 0.056(4) Uani 0.649(16) 1 d PD A 1 H54A H 0.6038 0.1697 0.7845 0.084 Uiso 0.649(16) 1 calc PR A 1 H54B H 0.6184 0.1213 0.7548 0.084 Uiso 0.649(16) 1 calc PR A 1 H54C H 0.6890 0.1437 0.8051 0.084 Uiso 0.649(16) 1 calc PR A 1 C52A C 0.617(3) 0.1399(10) 0.9300(10) 0.157(18) Uiso 0.351(16) 1 d PD A 2 H52G H 0.5782 0.1625 0.9468 0.236 Uiso 0.351(16) 1 calc PR A 2 H52H H 0.6741 0.1524 0.9246 0.236 Uiso 0.351(16) 1 calc PR A 2 H52I H 0.6198 0.1159 0.9646 0.236 Uiso 0.351(16) 1 calc PR A 2 C53A C 0.6533(17) 0.0841(7) 0.8415(16) 0.100(11) Uiso 0.351(16) 1 d PD A 2 H53G H 0.6302 0.0655 0.8034 0.149 Uiso 0.351(16) 1 calc PR A 2 H53H H 0.6635 0.0664 0.8844 0.149 Uiso 0.351(16) 1 calc PR A 2 H53I H 0.7071 0.0971 0.8263 0.149 Uiso 0.351(16) 1 calc PR A 2 C54A C 0.6056(15) 0.1559(6) 0.8006(9) 0.038(6) Uiso 0.351(16) 1 d PD A 2 H54G H 0.5700 0.1819 0.8066 0.057 Uiso 0.351(16) 1 calc PR A 2 H54H H 0.5937 0.1428 0.7538 0.057 Uiso 0.351(16) 1 calc PR A 2 H54I H 0.6657 0.1642 0.8040 0.057 Uiso 0.351(16) 1 calc PR A 2 Mg' Mg 0.27485(11) -0.24145(5) 0.77687(8) 0.0231(4) Uani 1 1 d . . . O1' O 0.3618(2) -0.19771(11) 0.75417(18) 0.0274(8) Uani 1 1 d . . . C1' C 0.3919(3) -0.18191(15) 0.6939(3) 0.0233(11) Uani 1 1 d . . . C2' C 0.4763(3) -0.16466(17) 0.6882(3) 0.0233(11) Uani 1 1 d . . . C3' C 0.5026(3) -0.15050(17) 0.6209(3) 0.0303(12) Uani 1 1 d . . . H3'A H 0.5589 -0.1395 0.6176 0.036 Uiso 1 1 calc R . . C4' C 0.4538(3) -0.15124(16) 0.5596(3) 0.0265(11) Uani 1 1 d . . . C5' C 0.3706(3) -0.16651(17) 0.5673(3) 0.0258(11) Uani 1 1 d . . . H5'A H 0.3336 -0.1667 0.5268 0.031 Uiso 1 1 calc R . . C6' C 0.3402(3) -0.18134(16) 0.6318(2) 0.0221(10) Uani 1 1 d . . . C7' C 0.2502(3) -0.19928(15) 0.6352(3) 0.0217(10) Uani 1 1 d . . . H7'A H 0.2178 -0.1823 0.6706 0.026 Uiso 1 1 calc R . . H7'B H 0.2217 -0.1955 0.5882 0.026 Uiso 1 1 calc R . . N8' N 0.2490(3) -0.24640(13) 0.6552(2) 0.0233(9) Uani 1 1 d . . . C9' C 0.1609(3) -0.26276(18) 0.6548(3) 0.0292(12) Uani 1 1 d . . . H9'A H 0.1398 -0.2653 0.6050 0.035 Uiso 1 1 calc R . . H9'B H 0.1241 -0.2416 0.6798 0.035 Uiso 1 1 calc R . . C10' C 0.1553(4) -0.30682(18) 0.6910(3) 0.0341(13) Uani 1 1 d . . . H10C H 0.0953 -0.3140 0.7011 0.041 Uiso 1 1 calc R . . H10D H 0.1787 -0.3299 0.6600 0.041 Uiso 1 1 calc R . . O11' O 0.2044(3) -0.30364(12) 0.7565(2) 0.0359(9) Uani 1 1 d . . . C12' C 0.2024(5) -0.3443(2) 0.7951(4) 0.056(2) Uani 1 1 d . . . H12D H 0.1441 -0.3501 0.8104 0.084 Uiso 1 1 calc R . . H12E H 0.2403 -0.3423 0.8369 0.084 Uiso 1 1 calc R . . H12F H 0.2213 -0.3681 0.7642 0.084 Uiso 1 1 calc R . . C13' C 0.3068(3) -0.27317(17) 0.6113(3) 0.0267(11) Uani 1 1 d . . . H13C H 0.3069 -0.3034 0.6303 0.032 Uiso 1 1 calc R . . H13D H 0.3652 -0.2615 0.6174 0.032 Uiso 1 1 calc R . . C14' C 0.2864(4) -0.2753(2) 0.5325(3) 0.0402(14) Uani 1 1 d . . . H14C H 0.2672 -0.2463 0.5155 0.048 Uiso 1 1 calc R . . H14D H 0.3382 -0.2834 0.5062 0.048 Uiso 1 1 calc R . . O15' O 0.2221(4) -0.30656(19) 0.5195(2) 0.0667(15) Uani 1 1 d . . . C16' C 0.1937(8) -0.3094(4) 0.4492(4) 0.101(4) Uani 1 1 d . . . H16D H 0.1496 -0.3320 0.4452 0.152 Uiso 1 1 calc R . . H16E H 0.2415 -0.3170 0.4187 0.152 Uiso 1 1 calc R . . H16F H 0.1700 -0.2812 0.4342 0.152 Uiso 1 1 calc R . . C17' C 0.5386(3) -0.16507(18) 0.7517(3) 0.0299(12) Uani 1 1 d . . . C18' C 0.5546(4) -0.2128(2) 0.7733(3) 0.0421(15) Uani 1 1 d . . . H18D H 0.5002 -0.2270 0.7831 0.063 Uiso 1 1 calc R . . H18E H 0.5911 -0.2136 0.8161 0.063 Uiso 1 1 calc R . . H18F H 0.5827 -0.2281 0.7343 0.063 Uiso 1 1 calc R . . C19' C 0.5004(4) -0.13921(19) 0.8145(3) 0.0352(13) Uani 1 1 d . . . H19D H 0.4450 -0.1517 0.8265 0.053 Uiso 1 1 calc R . . H19E H 0.4931 -0.1085 0.8007 0.053 Uiso 1 1 calc R . . H19F H 0.5389 -0.1411 0.8560 0.053 Uiso 1 1 calc R . . C20' C 0.6247(4) -0.1435(3) 0.7364(4) 0.0529(18) Uani 1 1 d . . . H20D H 0.6518 -0.1587 0.6968 0.079 Uiso 1 1 calc R . . H20E H 0.6616 -0.1454 0.7790 0.079 Uiso 1 1 calc R . . H20F H 0.6158 -0.1128 0.7239 0.079 Uiso 1 1 calc R . . C21' C 0.4863(3) -0.13682(18) 0.4865(3) 0.0295(12) Uani 1 1 d . . . C22' C 0.5813(4) -0.1265(2) 0.4883(3) 0.0459(17) Uani 1 1 d . . . H22D H 0.5992 -0.1174 0.4408 0.069 Uiso 1 1 calc R . . H22E H 0.6131 -0.1527 0.5030 0.069 Uiso 1 1 calc R . . H22F H 0.5925 -0.1029 0.5224 0.069 Uiso 1 1 calc R . . C23' C 0.4401(4) -0.0958(3) 0.4618(3) 0.0528(19) Uani 1 1 d . . . H23D H 0.4614 -0.0869 0.4152 0.079 Uiso 1 1 calc R . . H23E H 0.4501 -0.0723 0.4963 0.079 Uiso 1 1 calc R . . H23F H 0.3789 -0.1018 0.4579 0.079 Uiso 1 1 calc R . . C24' C 0.4697(5) -0.1734(3) 0.4319(4) 0.059(2) Uani 1 1 d . . . H24D H 0.4903 -0.1642 0.3852 0.089 Uiso 1 1 calc R . . H24E H 0.4085 -0.1793 0.4285 0.089 Uiso 1 1 calc R . . H24F H 0.4997 -0.1999 0.4471 0.089 Uiso 1 1 calc R . . O31' O 0.1681(2) -0.20888(12) 0.79507(18) 0.0277(8) Uani 1 1 d . . . C31' C 0.1363(3) -0.18772(15) 0.8492(3) 0.0221(10) Uani 1 1 d . . . C32' C 0.0487(3) -0.17537(18) 0.8520(3) 0.0268(11) Uani 1 1 d . . . C33' C 0.0212(3) -0.15141(19) 0.9113(3) 0.0307(12) Uani 1 1 d . . . H33B H -0.0367 -0.1424 0.9117 0.037 Uiso 1 1 calc R . . C34' C 0.0721(3) -0.14000(18) 0.9691(3) 0.0295(12) Uani 1 1 d . B . C35' C 0.1562(3) -0.15363(17) 0.9651(3) 0.0267(11) Uani 1 1 d . . . H35B H 0.1940 -0.1466 1.0034 0.032 Uiso 1 1 calc R . . C36' C 0.1879(3) -0.17711(16) 0.9078(3) 0.0231(11) Uani 1 1 d . . . C37' C 0.2799(3) -0.18995(17) 0.9097(3) 0.0264(11) Uani 1 1 d . . . H37C H 0.3105 -0.1726 0.8738 0.032 Uiso 1 1 calc R . . H37D H 0.3043 -0.1825 0.9571 0.032 Uiso 1 1 calc R . . N38' N 0.2946(3) -0.23725(14) 0.8957(2) 0.0264(9) Uani 1 1 d . . . C39' C 0.3862(4) -0.24678(18) 0.9088(3) 0.0315(12) Uani 1 1 d . . . H39C H 0.3976 -0.2486 0.9607 0.038 Uiso 1 1 calc R . . H39D H 0.4210 -0.2227 0.8895 0.038 Uiso 1 1 calc R . . C40' C 0.4111(4) -0.28935(19) 0.8741(3) 0.0360(13) Uani 1 1 d . . . H40C H 0.4739 -0.2916 0.8718 0.043 Uiso 1 1 calc R . . H40D H 0.3897 -0.3144 0.9020 0.043 Uiso 1 1 calc R . . O41' O 0.3747(3) -0.28998(12) 0.8039(2) 0.0367(9) Uani 1 1 d . . . C42' C 0.4099(5) -0.3253(2) 0.7631(4) 0.056(2) Uani 1 1 d . . . H42D H 0.4703 -0.3196 0.7548 0.083 Uiso 1 1 calc R . . H42E H 0.3795 -0.3275 0.7173 0.083 Uiso 1 1 calc R . . H42F H 0.4039 -0.3527 0.7895 0.083 Uiso 1 1 calc R . . C43' C 0.2364(4) -0.26547(19) 0.9367(3) 0.0332(13) Uani 1 1 d . . . H43C H 0.2508 -0.2963 0.9261 0.040 Uiso 1 1 calc R . . H43D H 0.1778 -0.2603 0.9184 0.040 Uiso 1 1 calc R . . C44' C 0.2357(5) -0.2602(2) 1.0170(3) 0.0499(17) Uani 1 1 d . . . H44C H 0.2348 -0.2287 1.0294 0.060 Uiso 1 1 calc R . . H44D H 0.1838 -0.2739 1.0363 0.060 Uiso 1 1 calc R . . O45' O 0.3067(4) -0.2795(3) 1.0469(3) 0.093(2) Uani 1 1 d . . . C46' C 0.3057(8) -0.2791(5) 1.1217(4) 0.120(4) Uani 1 1 d . . . H46D H 0.3571 -0.2933 1.1406 0.179 Uiso 1 1 calc R . . H46E H 0.2553 -0.2948 1.1382 0.179 Uiso 1 1 calc R . . H46F H 0.3037 -0.2488 1.1387 0.179 Uiso 1 1 calc R . . C47' C -0.0133(3) -0.18736(17) 0.7916(3) 0.0279(11) Uani 1 1 d . . . C48' C 0.0145(4) -0.1659(2) 0.7221(3) 0.0344(13) Uani 1 1 d . . . H48D H 0.0159 -0.1341 0.7281 0.052 Uiso 1 1 calc R . . H48E H -0.0260 -0.1735 0.6837 0.052 Uiso 1 1 calc R . . H48F H 0.0713 -0.1764 0.7098 0.052 Uiso 1 1 calc R . . C49' C -0.0162(4) -0.2378(2) 0.7837(3) 0.0413(15) Uani 1 1 d . . . H49D H 0.0413 -0.2489 0.7753 0.062 Uiso 1 1 calc R . . H49E H -0.0535 -0.2456 0.7433 0.062 Uiso 1 1 calc R . . H49F H -0.0382 -0.2508 0.8274 0.062 Uiso 1 1 calc R . . C50' C -0.1055(4) -0.1717(2) 0.8047(3) 0.0468(16) Uani 1 1 d . . . H50D H -0.1060 -0.1398 0.8100 0.070 Uiso 1 1 calc R . . H50E H -0.1267 -0.1853 0.8482 0.070 Uiso 1 1 calc R . . H50F H -0.1420 -0.1801 0.7642 0.070 Uiso 1 1 calc R . . C51' C 0.0380(3) -0.1133(2) 1.0321(3) 0.0384(15) Uani 1 1 d D . . C52' C 0.0051(6) -0.0688(3) 1.0068(4) 0.057(3) Uani 0.809(11) 1 d PD B 1 H52D H -0.0165 -0.0524 1.0475 0.085 Uiso 0.809(11) 1 calc PR B 1 H52E H -0.0409 -0.0730 0.9716 0.085 Uiso 0.809(11) 1 calc PR B 1 H52F H 0.0515 -0.0524 0.9850 0.085 Uiso 0.809(11) 1 calc PR B 1 C53' C -0.0369(6) -0.1376(3) 1.0634(5) 0.066(3) Uani 0.809(11) 1 d PD B 1 H53D H -0.0179 -0.1662 1.0810 0.099 Uiso 0.809(11) 1 calc PR B 1 H53E H -0.0810 -0.1416 1.0265 0.099 Uiso 0.809(11) 1 calc PR B 1 H53F H -0.0601 -0.1206 1.1028 0.099 Uiso 0.809(11) 1 calc PR B 1 C54' C 0.1041(5) -0.1057(4) 1.0900(5) 0.088(5) Uani 0.809(11) 1 d PD B 1 H54D H 0.1251 -0.1340 1.1076 0.132 Uiso 0.809(11) 1 calc PR B 1 H54E H 0.0785 -0.0895 1.1292 0.132 Uiso 0.809(11) 1 calc PR B 1 H54F H 0.1515 -0.0889 1.0707 0.132 Uiso 0.809(11) 1 calc PR B 1 C52B C -0.0532(11) -0.0992(11) 1.0189(19) 0.064(12) Uiso 0.191(11) 1 d PD B 2 H52J H -0.0916 -0.1231 1.0311 0.096 Uiso 0.191(11) 1 calc PR B 2 H52K H -0.0612 -0.0916 0.9685 0.096 Uiso 0.191(11) 1 calc PR B 2 H52L H -0.0657 -0.0736 1.0484 0.096 Uiso 0.191(11) 1 calc PR B 2 C53B C 0.0418(19) -0.1407(9) 1.0995(13) 0.049(10) Uiso 0.191(11) 1 d PD B 2 H53J H 0.0702 -0.1685 1.0897 0.074 Uiso 0.191(11) 1 calc PR B 2 H53K H -0.0161 -0.1464 1.1158 0.074 Uiso 0.191(11) 1 calc PR B 2 H53L H 0.0738 -0.1249 1.1367 0.074 Uiso 0.191(11) 1 calc PR B 2 C54B C 0.0922(16) -0.0730(7) 1.0441(17) 0.045(9) Uiso 0.191(11) 1 d PD B 2 H54J H 0.1452 -0.0812 1.0689 0.068 Uiso 0.191(11) 1 calc PR B 2 H54K H 0.0610 -0.0520 1.0732 0.068 Uiso 0.191(11) 1 calc PR B 2 H54L H 0.1054 -0.0597 0.9981 0.068 Uiso 0.191(11) 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 Mg 0.0217(8) 0.0212(8) 0.0265(9) 0.0003(7) 0.0038(7) 0.0040(7) O1 0.0222(18) 0.035(2) 0.0241(18) 0.0033(15) 0.0018(15) 0.0009(16) C1 0.0208(13) 0.0211(13) 0.0212(13) -0.0011(9) 0.0004(9) -0.0012(9) C2 0.021(2) 0.029(3) 0.015(2) -0.0045(19) -0.0020(19) 0.003(2) C3 0.026(3) 0.045(3) 0.027(3) -0.004(2) -0.004(2) 0.004(2) C4 0.0242(13) 0.0254(13) 0.0247(13) -0.0011(9) -0.0004(9) -0.0003(9) C5 0.024(3) 0.018(2) 0.034(3) -0.014(2) 0.004(2) -0.003(2) C6 0.021(2) 0.026(3) 0.024(3) -0.006(2) 0.001(2) -0.006(2) C7 0.019(2) 0.030(3) 0.029(3) 0.004(2) -0.002(2) 0.002(2) N8 0.027(2) 0.0144(19) 0.029(2) -0.0026(17) 0.0069(18) 0.0053(17) C9 0.038(3) 0.024(3) 0.031(3) 0.014(2) 0.010(2) 0.006(2) C10 0.041(3) 0.032(3) 0.041(3) 0.007(3) 0.022(3) -0.007(3) O11 0.036(2) 0.027(2) 0.045(2) 0.0102(17) 0.0164(19) 0.0063(17) C12 0.039(4) 0.039(4) 0.065(4) 0.021(3) 0.010(3) 0.004(3) C13 0.042(3) 0.022(3) 0.035(3) -0.001(2) 0.003(3) -0.009(2) C14 0.029(3) 0.049(4) 0.071(5) -0.001(4) 0.005(3) -0.006(3) O15 0.050(3) 0.100(5) 0.092(4) 0.028(4) 0.034(3) 0.000(3) C16 0.050(5) 0.151(10) 0.121(8) 0.016(7) 0.059(6) 0.003(6) C17 0.034(3) 0.034(3) 0.015(2) -0.001(2) 0.003(2) -0.002(2) C18 0.031(3) 0.051(4) 0.042(3) -0.020(3) 0.007(3) 0.002(3) C19 0.029(3) 0.044(3) 0.037(3) 0.005(3) 0.005(2) -0.007(3) C20 0.037(3) 0.073(5) 0.030(3) 0.014(3) -0.003(3) 0.008(3) C21 0.017(3) 0.070(5) 0.041(3) -0.007(3) -0.002(2) 0.006(3) C22 0.045(4) 0.094(6) 0.037(4) 0.007(4) -0.008(3) 0.040(4) C23 0.022(3) 0.087(6) 0.107(7) -0.019(5) -0.015(4) -0.002(4) C24 0.050(4) 0.060(4) 0.047(4) -0.010(3) 0.001(3) 0.023(3) O31 0.0285(19) 0.035(2) 0.0209(17) -0.0001(15) 0.0000(15) -0.0059(16) C31 0.022(3) 0.026(3) 0.026(3) 0.002(2) 0.003(2) 0.000(2) C32 0.034(3) 0.039(3) 0.026(3) 0.002(2) 0.008(2) 0.002(3) C33 0.040(3) 0.052(4) 0.022(3) -0.001(3) -0.013(2) 0.001(3) C34 0.030(3) 0.063(4) 0.036(3) 0.007(3) -0.013(3) -0.015(3) C35 0.031(3) 0.039(3) 0.037(3) 0.009(3) 0.001(3) -0.004(3) C36 0.023(3) 0.029(3) 0.029(3) 0.004(2) -0.006(2) -0.001(2) C37 0.024(3) 0.025(3) 0.023(3) 0.006(2) 0.001(2) -0.002(2) N38 0.027(2) 0.028(2) 0.022(2) 0.0002(18) 0.0037(18) 0.0026(19) C39 0.024(3) 0.031(3) 0.035(3) 0.001(2) 0.010(2) 0.004(2) C40 0.037(3) 0.026(3) 0.024(3) -0.012(2) 0.012(2) 0.000(2) O41 0.028(2) 0.0260(19) 0.042(2) -0.0104(17) 0.0091(17) -0.0022(16) C42 0.035(3) 0.028(3) 0.063(4) -0.019(3) 0.009(3) -0.011(3) C43 0.031(3) 0.029(3) 0.028(3) 0.001(2) 0.009(2) 0.002(2) C44 0.029(3) 0.048(4) 0.045(4) 0.002(3) 0.007(3) 0.013(3) O45 0.036(2) 0.059(3) 0.054(3) -0.008(2) 0.017(2) 0.003(2) C46 0.029(3) 0.073(5) 0.086(6) 0.012(4) 0.022(4) 0.002(3) C47 0.049(4) 0.080(5) 0.019(3) -0.006(3) 0.006(3) -0.015(4) C48 0.051(4) 0.116(7) 0.046(4) -0.012(4) 0.024(4) 0.005(5) C49 0.055(4) 0.096(6) 0.044(4) 0.034(4) 0.002(3) -0.016(4) C50 0.067(5) 0.152(9) 0.027(4) 0.010(5) -0.005(4) -0.009(6) C51 0.051(4) 0.086(6) 0.069(5) 0.009(4) -0.035(4) -0.028(4) C52 0.061(8) 0.085(10) 0.071(8) -0.030(7) -0.026(7) -0.016(7) C53 0.052(7) 0.098(10) 0.118(12) 0.029(9) -0.044(8) -0.022(7) C54 0.031(6) 0.059(8) 0.078(9) -0.027(7) 0.019(6) -0.022(6) Mg' 0.0282(9) 0.0219(8) 0.0190(8) 0.0005(7) -0.0009(7) 0.0017(7) O1' 0.032(2) 0.0262(19) 0.0237(18) -0.0007(15) 0.0003(16) 0.0016(16) C1' 0.028(3) 0.014(2) 0.028(3) -0.0041(19) 0.005(2) 0.003(2) C2' 0.015(2) 0.028(3) 0.026(3) 0.001(2) -0.003(2) 0.006(2) C3' 0.018(2) 0.025(3) 0.048(3) -0.002(2) 0.008(2) -0.005(2) C4' 0.026(3) 0.020(3) 0.033(3) 0.001(2) 0.002(2) -0.001(2) C5' 0.019(2) 0.031(3) 0.027(3) -0.001(2) -0.005(2) 0.007(2) C6' 0.028(3) 0.021(2) 0.018(2) -0.0042(19) -0.002(2) 0.006(2) C7' 0.023(2) 0.021(2) 0.021(2) 0.0016(19) -0.004(2) 0.004(2) N8' 0.023(2) 0.017(2) 0.030(2) -0.0019(17) -0.0019(18) -0.0012(17) C9' 0.025(3) 0.033(3) 0.030(3) -0.001(2) -0.007(2) -0.008(2) C10' 0.040(3) 0.029(3) 0.033(3) -0.006(2) -0.002(3) -0.016(3) O11' 0.052(3) 0.0245(19) 0.031(2) 0.0030(16) -0.0019(19) -0.0091(18) C12' 0.095(6) 0.030(3) 0.044(4) 0.010(3) 0.010(4) -0.022(4) C13' 0.031(3) 0.020(2) 0.030(3) 0.002(2) 0.002(2) 0.007(2) C14' 0.051(4) 0.038(3) 0.032(3) -0.002(3) 0.003(3) 0.000(3) O15' 0.084(4) 0.079(4) 0.036(3) -0.022(3) -0.007(3) -0.023(3) C16' 0.128(9) 0.125(9) 0.051(5) -0.017(5) -0.023(5) -0.028(7) C17' 0.022(3) 0.033(3) 0.034(3) -0.004(2) -0.006(2) 0.000(2) C18' 0.042(3) 0.042(4) 0.043(3) 0.008(3) -0.009(3) 0.005(3) C19' 0.037(3) 0.039(3) 0.029(3) -0.007(2) -0.009(2) -0.001(3) C20' 0.029(3) 0.073(5) 0.057(4) 0.004(4) -0.001(3) -0.014(3) C21' 0.028(3) 0.038(3) 0.023(3) -0.002(2) 0.014(2) 0.004(2) C22' 0.022(3) 0.072(5) 0.044(4) 0.015(3) 0.013(3) 0.001(3) C23' 0.048(4) 0.080(5) 0.030(3) 0.025(3) 0.021(3) -0.003(4) C24' 0.076(5) 0.066(5) 0.037(4) -0.013(3) 0.021(4) -0.026(4) O31' 0.0288(19) 0.034(2) 0.0198(17) 0.0010(15) 0.0002(15) 0.0008(16) C31' 0.027(3) 0.016(2) 0.023(2) -0.0026(19) 0.004(2) -0.003(2) C32' 0.019(2) 0.036(3) 0.026(3) 0.001(2) 0.004(2) -0.006(2) C33' 0.019(3) 0.046(3) 0.027(3) 0.006(2) 0.001(2) -0.003(2) C34' 0.032(3) 0.033(3) 0.024(3) 0.001(2) 0.001(2) 0.001(2) C35' 0.031(3) 0.032(3) 0.017(2) -0.002(2) 0.004(2) 0.001(2) C36' 0.023(2) 0.022(3) 0.024(3) 0.007(2) -0.001(2) -0.004(2) C37' 0.033(3) 0.026(3) 0.020(2) -0.007(2) -0.009(2) 0.000(2) N38' 0.029(2) 0.024(2) 0.026(2) 0.0062(18) -0.0010(19) 0.0001(19) C39' 0.038(3) 0.031(3) 0.025(3) -0.002(2) -0.011(2) 0.006(2) C40' 0.038(3) 0.034(3) 0.036(3) 0.012(3) -0.007(3) 0.012(3) O41' 0.042(2) 0.030(2) 0.037(2) 0.0007(17) -0.0055(19) 0.0110(18) C42' 0.083(5) 0.040(4) 0.044(4) -0.017(3) -0.018(4) 0.032(4) C43' 0.034(3) 0.034(3) 0.031(3) 0.005(2) 0.001(2) -0.003(3) C44' 0.071(5) 0.050(4) 0.029(3) 0.004(3) 0.007(3) -0.007(4) O45' 0.095(5) 0.152(6) 0.033(3) 0.034(3) -0.011(3) 0.020(4) C46' 0.128(10) 0.190(13) 0.040(5) 0.034(6) -0.015(5) 0.000(9) C47' 0.022(3) 0.029(3) 0.032(3) 0.002(2) 0.003(2) -0.001(2) C48' 0.034(3) 0.038(3) 0.031(3) 0.002(2) -0.007(2) 0.003(3) C49' 0.037(3) 0.052(4) 0.035(3) 0.010(3) -0.003(3) -0.015(3) C50' 0.029(3) 0.068(5) 0.044(4) -0.007(3) -0.010(3) 0.002(3) C51' 0.037(3) 0.062(4) 0.017(3) -0.009(3) 0.009(2) 0.009(3) C52' 0.083(7) 0.043(5) 0.046(5) -0.004(4) 0.024(5) 0.003(5) C53' 0.081(7) 0.067(6) 0.052(6) -0.031(5) 0.042(5) -0.013(5) C54' 0.040(5) 0.155(12) 0.070(7) -0.069(8) -0.008(5) 0.039(6) _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 Mg O31 1.977(4) . ? Mg O1 1.978(4) . ? Mg O11 2.204(4) . ? Mg O41 2.221(4) . ? Mg N8 2.279(4) . ? Mg N38 2.290(4) . ? O1 C1 1.328(6) . ? C1 C2 1.418(7) . ? C1 C6 1.444(6) . ? C2 C3 1.392(7) . ? C2 C17 1.553(6) . ? C3 C4 1.414(7) . ? C4 C5 1.392(7) . ? C4 C21 1.541(8) . ? C5 C6 1.382(7) . ? C6 C7 1.483(7) . ? C7 N8 1.493(6) . ? N8 C9 1.476(6) . ? N8 C13 1.492(7) . ? C9 C10 1.509(8) . ? C10 O11 1.449(6) . ? O11 C12 1.421(7) . ? C13 C14 1.514(8) . ? C14 O15 1.387(8) . ? O15 C16 1.428(9) . ? C17 C20 1.541(8) . ? C17 C19 1.550(8) . ? C17 C18 1.553(8) . ? C21 C23 1.511(10) . ? C21 C22 1.525(9) . ? C21 C24 1.538(9) . ? O31 C31 1.318(6) . ? C31 C36 1.408(7) . ? C31 C32 1.415(8) . ? C32 C33 1.405(8) . ? C32 C47 1.561(8) . ? C33 C34 1.388(8) . ? C34 C35 1.385(8) . ? C34 C51 1.546(9) . ? C35 C36 1.398(8) . ? C36 C37 1.511(7) . ? C37 N38 1.477(7) . ? N38 C39 1.467(7) . ? N38 C43 1.498(7) . ? C39 C40 1.496(8) . ? C40 O41 1.441(6) . ? O41 C42 1.434(6) . ? C43 C44 1.527(8) . ? C44 O45 1.399(7) . ? O45 C46 1.422(7) . ? C47 C48 1.509(11) . ? C47 C49 1.530(11) . ? C47 C50 1.553(10) . ? C51 C54 1.481(10) . ? C51 C53 1.496(11) . ? C51 C52A 1.509(15) . ? C51 C54A 1.531(13) . ? C51 C52 1.613(11) . ? C51 C53A 1.623(14) . ? Mg' O1' 1.964(4) . ? Mg' O31' 1.985(4) . ? Mg' O41' 2.213(4) . ? Mg' O11' 2.230(4) . ? Mg' N38' 2.251(5) . ? Mg' N8' 2.319(4) . ? O1' C1' 1.324(6) . ? C1' C6' 1.411(7) . ? C1' C2' 1.432(7) . ? C2' C3' 1.403(7) . ? C2' C17' 1.531(7) . ? C3' C4' 1.373(8) . ? C4' C5' 1.397(7) . ? C4' C21' 1.537(7) . ? C5' C6' 1.386(7) . ? C6' C7' 1.519(7) . ? C7' N8' 1.489(6) . ? N8' C9' 1.472(6) . ? N8' C13' 1.482(6) . ? C9' C10' 1.512(8) . ? C10' O11' 1.445(7) . ? O11' C12' 1.439(7) . ? C13' C14' 1.509(8) . ? C14' O15' 1.409(8) . ? O15' C16' 1.389(9) . ? C17' C18' 1.533(8) . ? C17' C20' 1.535(8) . ? C17' C19' 1.548(7) . ? C21' C23' 1.518(9) . ? C21' C22' 1.525(8) . ? C21' C24' 1.536(9) . ? O31' C31' 1.311(6) . ? C31' C36' 1.393(7) . ? C31' C32' 1.428(7) . ? C32' C33' 1.408(7) . ? C32' C47' 1.528(7) . ? C33' C34' 1.381(8) . ? C34' C35' 1.388(8) . ? C34' C51' 1.542(7) . ? C35' C36' 1.392(7) . ? C36' C37' 1.497(7) . ? C37' N38' 1.489(6) . ? N38' C43' 1.481(7) . ? N38' C39' 1.485(7) . ? C39' C40' 1.511(8) . ? C40' O41' 1.428(7) . ? O41' C42' 1.438(7) . ? C43' C44' 1.517(8) . ? C44' O45' 1.375(9) . ? O45' C46' 1.405(10) . ? C47' C48' 1.531(7) . ? C47' C50' 1.548(8) . ? C47' C49' 1.550(8) . ? C51' C54' 1.509(9) . ? C51' C52B 1.513(14) . ? C51' C54B 1.513(14) . ? C51' C53' 1.516(9) . ? C51' C53B 1.518(14) . ? C51' C52' 1.530(9) . ? 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 O31 Mg O1 110.88(17) . . ? O31 Mg O11 90.83(17) . . ? O1 Mg O11 150.40(17) . . ? O31 Mg O41 151.96(17) . . ? O1 Mg O41 88.81(16) . . ? O11 Mg O41 79.37(15) . . ? O31 Mg N8 93.63(16) . . ? O1 Mg N8 85.29(15) . . ? O11 Mg N8 73.08(15) . . ? O41 Mg N8 108.20(16) . . ? O31 Mg N38 84.53(16) . . ? O1 Mg N38 94.98(15) . . ? O11 Mg N38 107.32(16) . . ? O41 Mg N38 73.68(15) . . ? N8 Mg N38 178.11(18) . . ? C1 O1 Mg 135.3(3) . . ? O1 C1 C2 123.4(4) . . ? O1 C1 C6 119.2(4) . . ? C2 C1 C6 117.4(4) . . ? C3 C2 C1 119.3(4) . . ? C3 C2 C17 120.4(4) . . ? C1 C2 C17 120.2(4) . . ? C2 C3 C4 124.0(5) . . ? C5 C4 C3 115.5(5) . . ? C5 C4 C21 121.0(5) . . ? C3 C4 C21 123.4(5) . . ? C6 C5 C4 123.4(5) . . ? C5 C6 C1 120.3(5) . . ? C5 C6 C7 120.3(4) . . ? C1 C6 C7 119.4(4) . . ? C6 C7 N8 113.6(4) . . ? C9 N8 C13 112.6(4) . . ? C9 N8 C7 109.6(4) . . ? C13 N8 C7 111.8(4) . . ? C9 N8 Mg 103.0(3) . . ? C13 N8 Mg 117.6(3) . . ? C7 N8 Mg 101.4(3) . . ? N8 C9 C10 110.9(4) . . ? O11 C10 C9 107.6(4) . . ? C12 O11 C10 111.4(4) . . ? C12 O11 Mg 130.7(3) . . ? C10 O11 Mg 117.8(3) . . ? N8 C13 C14 118.3(5) . . ? O15 C14 C13 110.9(6) . . ? C14 O15 C16 112.7(7) . . ? C20 C17 C19 106.6(5) . . ? C20 C17 C2 113.0(4) . . ? C19 C17 C2 110.0(4) . . ? C20 C17 C18 107.6(5) . . ? C19 C17 C18 110.7(5) . . ? C2 C17 C18 109.0(4) . . ? C23 C21 C22 110.9(6) . . ? C23 C21 C24 108.3(6) . . ? C22 C21 C24 107.4(6) . . ? C23 C21 C4 108.0(6) . . ? C22 C21 C4 112.9(5) . . ? C24 C21 C4 109.2(5) . . ? C31 O31 Mg 135.3(3) . . ? O31 C31 C36 120.7(5) . . ? O31 C31 C32 122.6(4) . . ? C36 C31 C32 116.6(5) . . ? C33 C32 C31 120.0(5) . . ? C33 C32 C47 119.8(5) . . ? C31 C32 C47 120.2(5) . . ? C34 C33 C32 122.7(5) . . ? C35 C34 C33 117.1(5) . . ? C35 C34 C51 123.2(5) . . ? C33 C34 C51 119.7(5) . . ? C34 C35 C36 121.6(5) . . ? C35 C36 C31 121.6(5) . . ? C35 C36 C37 118.7(5) . . ? C31 C36 C37 119.6(4) . . ? N38 C37 C36 113.6(4) . . ? C39 N38 C37 109.5(4) . . ? C39 N38 C43 112.3(4) . . ? C37 N38 C43 113.9(4) . . ? C39 N38 Mg 103.3(3) . . ? C37 N38 Mg 101.3(3) . . ? C43 N38 Mg 115.5(3) . . ? N38 C39 C40 112.8(4) . . ? O41 C40 C39 106.9(4) . . ? C42 O41 C40 111.7(4) . . ? C42 O41 Mg 130.2(3) . . ? C40 O41 Mg 118.1(3) . . ? N38 C43 C44 117.7(4) . . ? O45 C44 C43 111.7(5) . . ? C44 O45 C46 112.0(6) . . ? C48 C47 C49 112.1(6) . . ? C48 C47 C50 107.1(6) . . ? C49 C47 C50 107.4(7) . . ? C48 C47 C32 108.9(6) . . ? C49 C47 C32 108.5(5) . . ? C50 C47 C32 112.9(6) . . ? C54 C51 C53 114.6(8) . . ? C54 C51 C52A 115.8(16) . . ? C53 C51 C52A 56.8(12) . . ? C54 C51 C54A 22.3(8) . . ? C53 C51 C54A 131.0(11) . . ? C52A C51 C54A 109.4(12) . . ? C54 C51 C34 114.3(6) . . ? C53 C51 C34 111.0(7) . . ? C52A C51 C34 128.3(16) . . ? C54A C51 C34 111.9(10) . . ? C54 C51 C52 105.9(7) . . ? C53 C51 C52 102.8(7) . . ? C52A C51 C52 46.7(13) . . ? C54A C51 C52 86.2(9) . . ? C34 C51 C52 107.2(7) . . ? C54 C51 C53A 79.0(10) . . ? C53 C51 C53A 49.9(10) . . ? C52A C51 C53A 103.1(11) . . ? C54A C51 C53A 101.3(10) . . ? C34 C51 C53A 98.0(13) . . ? C52 C51 C53A 148.9(12) . . ? O1' Mg' O31' 106.77(17) . . ? O1' Mg' O41' 90.75(16) . . ? O31' Mg' O41' 153.53(16) . . ? O1' Mg' O11' 152.70(16) . . ? O31' Mg' O11' 92.24(16) . . ? O41' Mg' O11' 79.37(16) . . ? O1' Mg' N38' 95.22(16) . . ? O31' Mg' N38' 84.49(16) . . ? O41' Mg' N38' 74.06(16) . . ? O11' Mg' N38' 106.19(16) . . ? O1' Mg' N8' 86.69(15) . . ? O31' Mg' N8' 93.86(15) . . ? O41' Mg' N8' 107.11(16) . . ? O11' Mg' N8' 72.34(14) . . ? N38' Mg' N8' 177.77(17) . . ? C1' O1' Mg' 133.9(3) . . ? O1' C1' C6' 120.1(4) . . ? O1' C1' C2' 122.9(5) . . ? C6' C1' C2' 117.0(4) . . ? C3' C2' C1' 117.9(5) . . ? C3' C2' C17' 120.6(4) . . ? C1' C2' C17' 121.3(4) . . ? C4' C3' C2' 125.5(5) . . ? C3' C4' C5' 115.5(5) . . ? C3' C4' C21' 123.7(5) . . ? C5' C4' C21' 120.8(5) . . ? C6' C5' C4' 122.4(5) . . ? C5' C6' C1' 121.6(5) . . ? C5' C6' C7' 119.3(4) . . ? C1' C6' C7' 119.0(4) . . ? N8' C7' C6' 112.0(4) . . ? C9' N8' C13' 113.2(4) . . ? C9' N8' C7' 110.1(4) . . ? C13' N8' C7' 112.6(4) . . ? C9' N8' Mg' 100.2(3) . . ? C13' N8' Mg' 119.0(3) . . ? C7' N8' Mg' 100.5(3) . . ? N8' C9' C10' 111.3(4) . . ? O11' C10' C9' 106.7(4) . . ? C12' O11' C10' 110.8(4) . . ? C12' O11' Mg' 131.7(4) . . ? C10' O11' Mg' 117.4(3) . . ? N8' C13' C14' 116.5(5) . . ? O15' C14' C13' 109.9(5) . . ? C16' O15' C14' 115.2(6) . . ? C2' C17' C18' 108.2(5) . . ? C2' C17' C20' 113.9(5) . . ? C18' C17' C20' 108.4(5) . . ? C2' C17' C19' 109.7(4) . . ? C18' C17' C19' 110.4(5) . . ? C20' C17' C19' 106.1(5) . . ? C23' C21' C22' 107.4(5) . . ? C23' C21' C24' 108.8(6) . . ? C22' C21' C24' 108.7(5) . . ? C23' C21' C4' 110.2(4) . . ? C22' C21' C4' 112.2(5) . . ? C24' C21' C4' 109.4(5) . . ? C31' O31' Mg' 135.6(3) . . ? O31' C31' C36' 120.1(4) . . ? O31' C31' C32' 122.5(5) . . ? C36' C31' C32' 117.3(4) . . ? C33' C32' C31' 118.3(5) . . ? C33' C32' C47' 120.8(4) . . ? C31' C32' C47' 120.9(4) . . ? C34' C33' C32' 124.8(5) . . ? C33' C34' C35' 114.9(5) . . ? C33' C34' C51' 122.1(5) . . ? C35' C34' C51' 122.9(5) . . ? C34' C35' C36' 123.3(5) . . ? C35' C36' C31' 121.2(5) . . ? C35' C36' C37' 118.3(5) . . ? C31' C36' C37' 120.5(4) . . ? N38' C37' C36' 113.8(4) . . ? C43' N38' C39' 113.8(4) . . ? C43' N38' C37' 112.1(4) . . ? C39' N38' C37' 108.3(4) . . ? C43' N38' Mg' 113.9(3) . . ? C39' N38' Mg' 105.7(3) . . ? C37' N38' Mg' 102.2(3) . . ? N38' C39' C40' 110.8(5) . . ? O41' C40' C39' 107.9(4) . . ? C40' O41' C42' 110.5(4) . . ? C40' O41' Mg' 118.3(3) . . ? C42' O41' Mg' 131.2(4) . . ? N38' C43' C44' 117.9(5) . . ? O45' C44' C43' 109.9(6) . . ? C44' O45' C46' 112.4(7) . . ? C32' C47' C48' 110.0(4) . . ? C32' C47' C50' 113.3(4) . . ? C48' C47' C50' 106.5(5) . . ? C32' C47' C49' 109.1(4) . . ? C48' C47' C49' 110.7(4) . . ? C50' C47' C49' 107.3(5) . . ? C54' C51' C52B 135.5(15) . . ? C54' C51' C54B 52.3(11) . . ? C52B C51' C54B 108.7(12) . . ? C54' C51' C53' 109.0(6) . . ? C52B C51' C53' 57.7(12) . . ? C54B C51' C53' 141.2(13) . . ? C54' C51' C53B 57.8(11) . . ? C52B C51' C53B 108.6(11) . . ? C54B C51' C53B 108.1(11) . . ? C53' C51' C53B 55.1(11) . . ? C54' C51' C52' 108.2(6) . . ? C52B C51' C52' 51.7(12) . . ? C54B C51' C52' 60.5(11) . . ? C53' C51' C52' 107.2(6) . . ? C53B C51' C52' 139.4(14) . . ? C54' C51' C34' 113.0(5) . . ? C52B C51' C34' 111.4(15) . . ? C54B C51' C34' 110.1(13) . . ? C53' C51' C34' 108.6(5) . . ? C53B C51' C34' 109.8(13) . . ? C52' C51' C34' 110.7(5) . . ? _diffrn_measured_fraction_theta_max 0.930 _diffrn_reflns_theta_full 32.75 _diffrn_measured_fraction_theta_full 0.930 _refine_diff_density_max 0.764 _refine_diff_density_min -0.480 _refine_diff_density_rms 0.080 #===END data_Compound_5a _database_code_depnum_ccdc_archive 'CCDC 293484' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C61 H108 Ca N6 O2' _chemical_formula_weight 997.61 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' Ca Ca 0.2262 0.3064 '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 10.8234(10) _cell_length_b 12.9659(12) _cell_length_c 13.1370(11) _cell_angle_alpha 110.331(8) _cell_angle_beta 107.408(8) _cell_angle_gamma 100.882(8) _cell_volume 1558.8(2) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 4.2931 _cell_measurement_theta_max 32.6590 _exptl_crystal_description 'tabular needles' _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.063 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 552 _exptl_absorpt_coefficient_mu 0.144 _exptl_absorpt_correction_type 'numeric analytical' _exptl_absorpt_correction_T_min 0.98468 _exptl_absorpt_correction_T_max 0.99444 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'OD Xcalibur 3' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 15.9863 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16621 _diffrn_reflns_av_R_equivalents 0.0534 _diffrn_reflns_av_sigmaI/netI 0.0863 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 4.30 _diffrn_reflns_theta_max 32.73 _reflns_number_total 10277 _reflns_number_gt 8941 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd' _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^)+(0.1000P)^2^+6.0000P] 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 10277 _refine_ls_number_parameters 372 _refine_ls_number_restraints 103 _refine_ls_R_factor_all 0.1908 _refine_ls_R_factor_gt 0.1754 _refine_ls_wR_factor_ref 0.3674 _refine_ls_wR_factor_gt 0.3555 _refine_ls_goodness_of_fit_ref 1.169 _refine_ls_restrained_S_all 1.172 _refine_ls_shift/su_max 0.000 _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 Ca Ca 0.5000 0.5000 0.0000 0.0159(2) Uani 1 2 d S . . O1 O 0.3487(3) 0.4067(3) 0.0446(3) 0.0318(7) Uani 1 1 d . . . C1 C 0.3403(4) 0.3589(4) 0.1176(4) 0.0274(8) Uani 1 1 d . . . C2 C 0.2145(4) 0.2805(4) 0.0991(4) 0.0271(8) Uani 1 1 d . . . C3 C 0.2151(5) 0.2322(4) 0.1791(4) 0.0299(8) Uani 1 1 d . . . H3A H 0.1311 0.1804 0.1659 0.036 Uiso 1 1 calc R . . C4 C 0.3310(5) 0.2549(4) 0.2770(4) 0.0316(9) Uani 1 1 d . B . C5 C 0.4523(4) 0.3330(4) 0.2943(4) 0.0311(9) Uani 1 1 d . . . H5A H 0.5330 0.3525 0.3613 0.037 Uiso 1 1 calc R . . C6 C 0.4594(4) 0.3830(4) 0.2175(4) 0.0282(8) Uani 1 1 d . . . C7 C 0.5923(4) 0.4740(4) 0.2500(4) 0.0300(8) Uani 1 1 d . . . H7A H 0.5772 0.5503 0.2709 0.036 Uiso 1 1 calc R . . H7B H 0.6610 0.4783 0.3221 0.036 Uiso 1 1 calc R . . N8 N 0.6528(4) 0.4580(3) 0.1602(3) 0.0282(7) Uani 1 1 d D A . C9 C 0.6528(5) 0.3380(4) 0.1050(4) 0.0370(10) Uani 1 1 d D . . H9A H 0.5645 0.2834 0.0891 0.044 Uiso 0.842(6) 1 calc PR A 1 H9B H 0.7266 0.3261 0.1613 0.044 Uiso 0.842(6) 1 calc PR A 1 H9C H 0.6332 0.2998 0.1520 0.044 Uiso 0.158(6) 1 d PR A 2 H9D H 0.7440 0.3416 0.1103 0.044 Uiso 0.158(6) 1 d PR A 2 C10 C 0.6735(6) 0.3095(5) -0.0091(5) 0.0359(12) Uani 0.842(6) 1 d PD A 1 H10A H 0.7578 0.3682 0.0057 0.043 Uiso 0.842(6) 1 calc PR A 1 H10B H 0.6874 0.2328 -0.0344 0.043 Uiso 0.842(6) 1 calc PR A 1 N11 N 0.5565(4) 0.3064(3) -0.1074(3) 0.0318(8) Uani 1 1 d D . . C12 C 0.4436(6) 0.1952(5) -0.1548(5) 0.0389(13) Uani 0.842(6) 1 d PD A 1 H12A H 0.4058 0.1976 -0.0944 0.047 Uiso 0.842(6) 1 calc PR A 1 H12B H 0.4817 0.1304 -0.1692 0.047 Uiso 0.842(6) 1 calc PR A 1 C13 C 0.3268(7) 0.1705(6) -0.2697(6) 0.0501(16) Uani 0.842(6) 1 d PD A 1 H13A H 0.2564 0.0963 -0.2961 0.075 Uiso 0.842(6) 1 calc PR A 1 H13B H 0.3628 0.1663 -0.3307 0.075 Uiso 0.842(6) 1 calc PR A 1 H13C H 0.2866 0.2332 -0.2558 0.075 Uiso 0.842(6) 1 calc PR A 1 C14 C 0.6066(7) 0.3146(5) -0.2000(5) 0.0394(13) Uani 0.842(6) 1 d PD A 1 H14A H 0.6829 0.3889 -0.1631 0.047 Uiso 0.842(6) 1 calc PR A 1 H14B H 0.5315 0.3191 -0.2619 0.047 Uiso 0.842(6) 1 calc PR A 1 C15 C 0.6557(7) 0.2170(6) -0.2605(6) 0.0478(15) Uani 0.842(6) 1 d PD A 1 H15A H 0.6857 0.2327 -0.3187 0.072 Uiso 0.842(6) 1 calc PR A 1 H15B H 0.5806 0.1428 -0.3006 0.072 Uiso 0.842(6) 1 calc PR A 1 H15C H 0.7325 0.2128 -0.2012 0.072 Uiso 0.842(6) 1 calc PR A 1 C10' C 0.5594(18) 0.2635(14) -0.0169(11) 0.027(5) Uiso 0.158(6) 1 d PD A 2 H10C H 0.4656 0.2438 -0.0187 0.033 Uiso 0.158(6) 1 calc PR A 2 H10D H 0.5808 0.1900 -0.0411 0.033 Uiso 0.158(6) 1 calc PR A 2 C12' C 0.426(2) 0.2374(17) -0.2136(15) 0.036(6) Uiso 0.158(6) 1 d PD A 2 H12C H 0.4143 0.2790 -0.2646 0.043 Uiso 0.158(6) 1 calc PR A 2 H12D H 0.3489 0.2335 -0.1877 0.043 Uiso 0.158(6) 1 calc PR A 2 C13' C 0.418(3) 0.1133(17) -0.287(2) 0.043(7) Uiso 0.158(6) 1 d PD A 2 H13D H 0.3291 0.0740 -0.3552 0.065 Uiso 0.158(6) 1 calc PR A 2 H13E H 0.4265 0.0705 -0.2385 0.065 Uiso 0.158(6) 1 calc PR A 2 H13F H 0.4918 0.1161 -0.3156 0.065 Uiso 0.158(6) 1 calc PR A 2 C14' C 0.6839(19) 0.319(2) -0.127(2) 0.031(6) Uiso 0.158(6) 1 d PD A 2 H14C H 0.7022 0.2443 -0.1455 0.037 Uiso 0.158(6) 1 calc PR A 2 H14D H 0.7604 0.3781 -0.0525 0.037 Uiso 0.158(6) 1 calc PR A 2 C15' C 0.682(2) 0.356(2) -0.227(2) 0.029(5) Uiso 0.158(6) 1 d PD A 2 H15D H 0.7708 0.3658 -0.2327 0.043 Uiso 0.158(6) 1 calc PR A 2 H15E H 0.6621 0.4294 -0.2096 0.043 Uiso 0.158(6) 1 calc PR A 2 H15F H 0.6101 0.2955 -0.3018 0.043 Uiso 0.158(6) 1 calc PR A 2 C16 C 0.7915(4) 0.5450(4) 0.2143(4) 0.0351(10) Uani 1 1 d . . . H16A H 0.7843 0.6231 0.2521 0.042 Uiso 1 1 calc R A . H16B H 0.8220 0.5439 0.1502 0.042 Uiso 1 1 calc R . . C17 C 0.9030(5) 0.5294(6) 0.3067(6) 0.0570(17) Uani 1 1 d D A . H17A H 0.8700 0.5216 0.3671 0.068 Uiso 1 1 calc R . . H17B H 0.9213 0.4570 0.2678 0.068 Uiso 1 1 calc R . . N18 N 1.0299(4) 0.6281(4) 0.3642(4) 0.0497(11) Uani 1 1 d D . . C19 C 1.1462(6) 0.6009(6) 0.4302(6) 0.0526(19) Uani 0.844(12) 1 d PDU A 1 H19A H 1.1189 0.5667 0.4800 0.063 Uiso 0.844(12) 1 calc PR A 1 H19B H 1.2241 0.6738 0.4832 0.063 Uiso 0.844(12) 1 calc PR A 1 C20 C 1.1908(10) 0.5174(9) 0.3485(11) 0.090(4) Uani 0.844(12) 1 d PD A 1 H20A H 1.2671 0.5008 0.3952 0.135 Uiso 0.844(12) 1 calc PR A 1 H20B H 1.2203 0.5521 0.3008 0.135 Uiso 0.844(12) 1 calc PR A 1 H20C H 1.1140 0.4449 0.2965 0.135 Uiso 0.844(12) 1 calc PR A 1 C21 C 1.0152(10) 0.7232(9) 0.4585(9) 0.098(4) Uani 0.844(12) 1 d PD A 1 H21A H 1.0352 0.7086 0.5299 0.118 Uiso 0.844(12) 1 calc PR A 1 H21B H 0.9194 0.7229 0.4315 0.118 Uiso 0.844(12) 1 calc PR A 1 C22 C 1.1094(14) 0.8402(9) 0.4897(13) 0.129(6) Uani 0.844(12) 1 d PDU A 1 H22A H 1.1022 0.8994 0.5565 0.194 Uiso 0.844(12) 1 calc PR A 1 H22B H 1.0837 0.8585 0.4215 0.194 Uiso 0.844(12) 1 calc PR A 1 H22C H 1.2039 0.8393 0.5116 0.194 Uiso 0.844(12) 1 calc PR A 1 C19' C 1.1473(19) 0.590(2) 0.352(3) 0.057(8) Uiso 0.156(12) 1 d PDU A 2 H19C H 1.2319 0.6585 0.3961 0.069 Uiso 0.156(12) 1 calc PR A 2 H19D H 1.1331 0.5575 0.2677 0.069 Uiso 0.156(12) 1 calc PR A 2 C20' C 1.166(3) 0.500(3) 0.398(3) 0.036(7) Uiso 0.156(12) 1 d PD A 2 H20D H 1.2462 0.4793 0.3898 0.054 Uiso 0.156(12) 1 calc PR A 2 H20E H 1.0842 0.4305 0.3518 0.054 Uiso 0.156(12) 1 calc PR A 2 H20F H 1.1793 0.5316 0.4811 0.054 Uiso 0.156(12) 1 calc PR A 2 C21' C 1.022(3) 0.7431(12) 0.400(4) 0.055(10) Uiso 0.156(12) 1 d PD A 2 H21C H 0.9998 0.7636 0.4703 0.066 Uiso 0.156(12) 1 calc PR A 2 H21D H 0.9466 0.7441 0.3355 0.066 Uiso 0.156(12) 1 calc PR A 2 C22' C 1.153(4) 0.835(2) 0.428(5) 0.074(12) Uiso 0.156(12) 1 d PDU A 2 H22D H 1.1510 0.9125 0.4740 0.111 Uiso 0.156(12) 1 calc PR A 2 H22E H 1.1601 0.8319 0.3544 0.111 Uiso 0.156(12) 1 calc PR A 2 H22F H 1.2322 0.8214 0.4743 0.111 Uiso 0.156(12) 1 calc PR A 2 C23 C 0.0810(4) 0.2534(4) -0.0052(4) 0.0322(9) Uani 1 1 d . . . C24 C 0.0962(5) 0.1953(5) -0.1225(4) 0.0446(12) Uani 1 1 d . . . H24A H 0.1156 0.1230 -0.1286 0.067 Uiso 1 1 calc R . . H24B H 0.1718 0.2481 -0.1250 0.067 Uiso 1 1 calc R . . H24C H 0.0110 0.1776 -0.1886 0.067 Uiso 1 1 calc R . . C25 C -0.0417(5) 0.1703(5) -0.0070(5) 0.0426(11) Uani 1 1 d . . . H25A H -0.0243 0.0973 -0.0136 0.064 Uiso 1 1 calc R . . H25B H -0.1242 0.1544 -0.0749 0.064 Uiso 1 1 calc R . . H25C H -0.0551 0.2062 0.0662 0.064 Uiso 1 1 calc R . . C26 C 0.0491(5) 0.3656(5) 0.0034(5) 0.0419(11) Uani 1 1 d . . . H26A H -0.0360 0.3471 -0.0632 0.063 Uiso 1 1 calc R . . H26B H 0.1244 0.4189 0.0011 0.063 Uiso 1 1 calc R . . H26C H 0.0385 0.4024 0.0778 0.063 Uiso 1 1 calc R . . C27 C 0.3255(5) 0.2031(4) 0.3644(4) 0.0364(10) Uani 1 1 d D . . C28 C 0.1841(9) 0.1178(8) 0.3280(7) 0.071(3) Uani 0.752(10) 1 d PD B 1 H28A H 0.1581 0.0539 0.2502 0.106 Uiso 0.752(10) 1 calc PR B 1 H28B H 0.1164 0.1585 0.3240 0.106 Uiso 0.752(10) 1 calc PR B 1 H28C H 0.1875 0.0865 0.3864 0.106 Uiso 0.752(10) 1 calc PR B 1 C29 C 0.4280(11) 0.1364(10) 0.3767(10) 0.082(4) Uani 0.752(10) 1 d PD B 1 H29A H 0.4053 0.0726 0.2997 0.124 Uiso 0.752(10) 1 calc PR B 1 H29B H 0.4232 0.1045 0.4335 0.124 Uiso 0.752(10) 1 calc PR B 1 H29C H 0.5209 0.1894 0.4048 0.124 Uiso 0.752(10) 1 calc PR B 1 C30 C 0.3616(12) 0.2991(7) 0.4852(7) 0.077(4) Uani 0.752(10) 1 d PD B 1 H30A H 0.3575 0.2650 0.5405 0.115 Uiso 0.752(10) 1 calc PR B 1 H30B H 0.2962 0.3419 0.4797 0.115 Uiso 0.752(10) 1 calc PR B 1 H30C H 0.4544 0.3524 0.5136 0.115 Uiso 0.752(10) 1 calc PR B 1 C28' C 0.270(2) 0.0721(11) 0.2991(18) 0.051(6) Uiso 0.248(10) 1 d PD B 2 H28D H 0.2660 0.0388 0.3551 0.077 Uiso 0.248(10) 1 calc PR B 2 H28E H 0.3294 0.0441 0.2608 0.077 Uiso 0.248(10) 1 calc PR B 2 H28F H 0.1772 0.0482 0.2390 0.077 Uiso 0.248(10) 1 calc PR B 2 C29' C 0.4658(14) 0.2385(18) 0.4629(16) 0.051(6) Uiso 0.248(10) 1 d PD B 2 H29D H 0.5060 0.3235 0.5022 0.077 Uiso 0.248(10) 1 calc PR B 2 H29E H 0.5261 0.2049 0.4291 0.077 Uiso 0.248(10) 1 calc PR B 2 H29F H 0.4551 0.2097 0.5207 0.077 Uiso 0.248(10) 1 calc PR B 2 C30' C 0.2313(19) 0.2457(19) 0.423(2) 0.057(7) Uiso 0.248(10) 1 d PD B 2 H30D H 0.2673 0.3307 0.4659 0.085 Uiso 0.248(10) 1 calc PR B 2 H30E H 0.2265 0.2116 0.4780 0.085 Uiso 0.248(10) 1 calc PR B 2 H30F H 0.1393 0.2221 0.3621 0.085 Uiso 0.248(10) 1 calc PR B 2 C40 C 0.249(4) -0.076(4) -0.162(3) 0.121(17) Uiso 0.269(15) 1 d PDU C -1 H40A H 0.2249 -0.1574 -0.2169 0.181 Uiso 0.269(15) 1 calc PR C -1 H40B H 0.2452 -0.0278 -0.2054 0.181 Uiso 0.269(15) 1 calc PR C -1 H40C H 0.1829 -0.0688 -0.1244 0.181 Uiso 0.269(15) 1 calc PR C -1 C41 C 0.3945(16) -0.0344(14) -0.0661(16) 0.052(6) Uiso 0.269(15) 1 d PGD C -1 C42 C 0.4250(18) 0.0434(14) 0.0491(17) 0.044(6) Uiso 0.269(15) 1 d PGD C -1 H42 H 0.3549 0.0675 0.0699 0.052 Uiso 0.269(15) 1 calc PR C -1 C43 C 0.5581(19) 0.0860(14) 0.1339(14) 0.041(5) Uiso 0.269(15) 1 d PG C -1 H43 H 0.5789 0.1392 0.2126 0.049 Uiso 0.269(15) 1 calc PR C -1 C44 C 0.6606(17) 0.0507(15) 0.1034(15) 0.063(8) Uiso 0.269(15) 1 d PG C -1 H44 H 0.7516 0.0797 0.1613 0.076 Uiso 0.269(15) 1 calc PR C -1 C45 C 0.6301(17) -0.0272(15) -0.0118(16) 0.040(4) Uiso 0.269(15) 1 d PG C -1 H45 H 0.7002 -0.0513 -0.0326 0.048 Uiso 0.269(15) 1 calc PR C -1 C46 C 0.4971(18) -0.0697(14) -0.0966(14) 0.045(7) Uiso 0.269(15) 1 d PGD C -1 H46 H 0.4762 -0.1229 -0.1753 0.054 Uiso 0.269(15) 1 calc PR C -1 C40' C 0.296(4) -0.051(4) -0.107(3) 0.076(12) Uiso 0.231(15) 1 d PDU C -2 H40D H 0.2381 -0.0996 -0.0851 0.114 Uiso 0.231(15) 1 calc PR C -2 H40E H 0.2877 -0.0960 -0.1874 0.114 Uiso 0.231(15) 1 calc PR C -2 H40F H 0.2659 0.0167 -0.1041 0.114 Uiso 0.231(15) 1 calc PR C -2 C41' C 0.4466(18) -0.0085(15) -0.0198(15) 0.041(5) Uiso 0.231(15) 1 d PGD C -2 C42' C 0.483(2) 0.0691(16) 0.0969(16) 0.043(8) Uiso 0.231(15) 1 d PGD C -2 H42' H 0.4165 0.0958 0.1213 0.051 Uiso 0.231(15) 1 calc PR C -2 C43' C 0.618(2) 0.1075(15) 0.1779(14) 0.052(7) Uiso 0.231(15) 1 d PG C -2 H43' H 0.6431 0.1605 0.2576 0.063 Uiso 0.231(15) 1 calc PR C -2 C44' C 0.7157(18) 0.0684(17) 0.1422(15) 0.046(7) Uiso 0.231(15) 1 d PGU C -2 H44' H 0.8077 0.0946 0.1975 0.055 Uiso 0.231(15) 1 calc PR C -2 C45' C 0.6789(19) -0.0092(15) 0.0255(16) 0.035(5) Uiso 0.231(15) 1 d PG C -2 H45' H 0.7458 -0.0360 0.0011 0.041 Uiso 0.231(15) 1 calc PR C -2 C46' C 0.544(2) -0.0477(13) -0.0555(13) 0.031(5) Uiso 0.231(15) 1 d PGD C -2 H46' H 0.5192 -0.1007 -0.1352 0.037 Uiso 0.231(15) 1 calc PR C -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 Ca 0.0161(4) 0.0192(5) 0.0187(5) 0.0119(4) 0.0087(4) 0.0087(3) O1 0.0261(14) 0.0351(16) 0.0352(16) 0.0196(14) 0.0091(12) 0.0089(12) C1 0.0253(18) 0.0248(18) 0.0290(19) 0.0099(16) 0.0083(15) 0.0085(15) C2 0.0241(18) 0.0279(19) 0.0284(19) 0.0123(16) 0.0094(15) 0.0082(15) C3 0.031(2) 0.029(2) 0.031(2) 0.0128(17) 0.0140(17) 0.0099(16) C4 0.035(2) 0.031(2) 0.031(2) 0.0146(17) 0.0143(18) 0.0089(17) C5 0.0275(19) 0.034(2) 0.028(2) 0.0133(17) 0.0062(16) 0.0089(17) C6 0.0242(18) 0.0280(19) 0.0287(19) 0.0112(16) 0.0077(15) 0.0067(15) C7 0.0262(19) 0.030(2) 0.0275(19) 0.0106(16) 0.0063(16) 0.0049(16) N8 0.0248(16) 0.0258(16) 0.0301(17) 0.0107(14) 0.0086(14) 0.0064(13) C9 0.041(2) 0.033(2) 0.037(2) 0.0178(19) 0.012(2) 0.0116(19) C10 0.031(3) 0.041(3) 0.035(3) 0.016(2) 0.011(2) 0.014(2) N11 0.0282(17) 0.0330(19) 0.0319(18) 0.0162(16) 0.0092(15) 0.0053(15) C12 0.036(3) 0.029(3) 0.042(3) 0.015(2) 0.010(2) 0.001(2) C13 0.042(3) 0.053(4) 0.043(3) 0.016(3) 0.011(3) 0.007(3) C14 0.048(3) 0.037(3) 0.036(3) 0.017(2) 0.020(3) 0.011(2) C15 0.055(4) 0.049(4) 0.040(3) 0.017(3) 0.020(3) 0.021(3) C16 0.025(2) 0.036(2) 0.034(2) 0.0165(19) 0.0040(17) -0.0002(17) C17 0.021(2) 0.079(4) 0.067(4) 0.047(4) 0.004(2) 0.001(2) N18 0.028(2) 0.050(3) 0.051(3) 0.015(2) 0.0025(19) 0.0055(19) C19 0.032(3) 0.059(4) 0.046(4) 0.021(3) 0.000(3) 0.002(3) C20 0.058(5) 0.079(7) 0.106(9) 0.020(6) 0.016(6) 0.033(5) C21 0.061(5) 0.121(9) 0.048(5) -0.017(5) 0.001(4) 0.030(6) C22 0.107(10) 0.076(7) 0.105(10) -0.023(7) -0.009(8) 0.023(7) C23 0.0257(19) 0.035(2) 0.031(2) 0.0140(18) 0.0078(16) 0.0056(17) C24 0.035(2) 0.053(3) 0.034(2) 0.016(2) 0.006(2) 0.009(2) C25 0.026(2) 0.046(3) 0.049(3) 0.024(2) 0.008(2) 0.0029(19) C26 0.029(2) 0.046(3) 0.047(3) 0.023(2) 0.008(2) 0.011(2) C27 0.040(2) 0.037(2) 0.031(2) 0.0168(19) 0.0117(19) 0.0083(19) C28 0.071(6) 0.069(6) 0.050(5) 0.037(5) 0.005(4) -0.018(5) C29 0.110(9) 0.110(9) 0.112(9) 0.095(8) 0.076(8) 0.074(8) C30 0.128(10) 0.056(5) 0.035(4) 0.016(4) 0.034(5) 0.005(6) _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 Ca O1 2.192(3) 2_665 ? Ca O1 2.192(3) . ? Ca N8 2.552(4) . ? Ca N8 2.552(4) 2_665 ? Ca N11 2.702(4) . ? Ca N11 2.702(4) 2_665 ? O1 C1 1.325(5) . ? C1 C6 1.425(6) . ? C1 C2 1.433(6) . ? C2 C3 1.397(6) . ? C2 C23 1.542(6) . ? C3 C4 1.395(6) . ? C4 C5 1.401(6) . ? C4 C27 1.528(6) . ? C5 C6 1.389(6) . ? C6 C7 1.512(6) . ? C7 N8 1.485(6) . ? N8 C9 1.471(6) . ? N8 C16 1.482(5) . ? C9 C10' 1.452(13) . ? C9 C10 1.511(7) . ? C10 N11 1.497(6) . ? N11 C14' 1.465(14) . ? N11 C10' 1.473(14) . ? N11 C12 1.488(6) . ? N11 C12' 1.489(14) . ? N11 C14 1.499(6) . ? C12 C13 1.532(8) . ? C14 C15 1.525(8) . ? C12' C13' 1.531(16) . ? C14' C15' 1.540(16) . ? C16 C17 1.535(7) . ? C17 N18 1.463(7) . ? N18 C21' 1.427(15) . ? N18 C19' 1.478(15) . ? N18 C19 1.479(7) . ? N18 C21 1.487(9) . ? C19 C20 1.503(11) . ? C21 C22 1.498(14) . ? C19' C20' 1.505(18) . ? C21' C22' 1.518(19) . ? C23 C26 1.531(7) . ? C23 C25 1.532(6) . ? C23 C24 1.536(7) . ? C27 C28' 1.509(12) . ? C27 C30 1.514(8) . ? C27 C30' 1.523(13) . ? C27 C29' 1.530(12) . ? C27 C28 1.533(8) . ? C27 C29 1.536(9) . ? C40 C41 1.55(4) . ? C41 C42 1.3900 . ? C41 C46 1.3900 . ? C42 C43 1.3900 . ? C43 C44 1.3900 . ? C44 C45 1.3900 . ? C45 C46 1.3900 . ? C40' C41' 1.54(4) . ? C41' C42' 1.3900 . ? C41' C46' 1.3900 . ? C42' C43' 1.3900 . ? C43' C44' 1.3900 . ? C44' C45' 1.3900 . ? C45' C46' 1.3900 . ? 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 O1 Ca O1 180.0 2_665 . ? O1 Ca N8 101.66(11) 2_665 . ? O1 Ca N8 78.34(11) . . ? O1 Ca N8 78.34(11) 2_665 2_665 ? O1 Ca N8 101.66(11) . 2_665 ? N8 Ca N8 180.0 . 2_665 ? O1 Ca N11 87.03(11) 2_665 . ? O1 Ca N11 92.97(11) . . ? N8 Ca N11 71.97(11) . . ? N8 Ca N11 108.03(11) 2_665 . ? O1 Ca N11 92.97(11) 2_665 2_665 ? O1 Ca N11 87.03(11) . 2_665 ? N8 Ca N11 108.03(11) . 2_665 ? N8 Ca N11 71.97(11) 2_665 2_665 ? N11 Ca N11 180.00(18) . 2_665 ? C1 O1 Ca 141.2(3) . . ? O1 C1 C6 120.1(4) . . ? O1 C1 C2 122.3(4) . . ? C6 C1 C2 117.6(4) . . ? C3 C2 C1 118.6(4) . . ? C3 C2 C23 121.1(4) . . ? C1 C2 C23 120.2(4) . . ? C4 C3 C2 124.3(4) . . ? C3 C4 C5 116.1(4) . . ? C3 C4 C27 122.4(4) . . ? C5 C4 C27 121.4(4) . . ? C6 C5 C4 122.6(4) . . ? C5 C6 C1 120.8(4) . . ? C5 C6 C7 118.2(4) . . ? C1 C6 C7 120.6(4) . . ? N8 C7 C6 117.7(4) . . ? C9 N8 C16 112.5(4) . . ? C9 N8 C7 112.1(3) . . ? C16 N8 C7 109.5(3) . . ? C9 N8 Ca 108.1(3) . . ? C16 N8 Ca 108.2(3) . . ? C7 N8 Ca 106.2(2) . . ? C10' C9 N8 119.1(8) . . ? C10' C9 C10 48.7(7) . . ? N8 C9 C10 113.1(4) . . ? N11 C10 C9 113.8(4) . . ? C14' N11 C10' 112.1(10) . . ? C14' N11 C12 126.0(12) . . ? C10' N11 C12 68.1(6) . . ? C14' N11 C12' 117.1(15) . . ? C10' N11 C12' 109.5(10) . . ? C12 N11 C12' 42.8(9) . . ? C14' N11 C10 66.7(8) . . ? C10' N11 C10 48.6(7) . . ? C12 N11 C10 108.1(4) . . ? C12' N11 C10 148.8(9) . . ? C14' N11 C14 41.2(8) . . ? C10' N11 C14 149.0(9) . . ? C12 N11 C14 111.5(4) . . ? C12' N11 C14 81.2(11) . . ? C10 N11 C14 107.9(4) . . ? C14' N11 Ca 118.8(11) . . ? C10' N11 Ca 95.4(7) . . ? C12 N11 Ca 114.8(3) . . ? C12' N11 Ca 101.3(9) . . ? C10 N11 Ca 102.7(3) . . ? C14 N11 Ca 111.2(3) . . ? N11 C12 C13 113.7(5) . . ? N11 C14 C15 117.5(5) . . ? C9 C10' N11 119.0(10) . . ? N11 C12' C13' 114.5(14) . . ? N11 C14' C15' 113.8(14) . . ? N8 C16 C17 116.6(4) . . ? N18 C17 C16 111.4(5) . . ? C21' N18 C17 118.9(11) . . ? C21' N18 C19' 128.0(15) . . ? C17 N18 C19' 111.5(11) . . ? C21' N18 C19 122.4(16) . . ? C17 N18 C19 111.3(5) . . ? C19' N18 C19 39.1(13) . . ? C21' N18 C21 36.6(18) . . ? C17 N18 C21 107.8(6) . . ? C19' N18 C21 133.6(15) . . ? C19 N18 C21 103.3(6) . . ? N18 C19 C20 111.7(6) . . ? N18 C21 C22 112.1(9) . . ? N18 C19' C20' 112.6(15) . . ? N18 C21' C22' 114.2(18) . . ? C26 C23 C25 107.9(4) . . ? C26 C23 C24 109.3(4) . . ? C25 C23 C24 107.8(4) . . ? C26 C23 C2 110.3(4) . . ? C25 C23 C2 111.8(4) . . ? C24 C23 C2 109.7(4) . . ? C28' C27 C30 139.9(10) . . ? C28' C27 C30' 109.0(10) . . ? C30 C27 C30' 50.6(9) . . ? C28' C27 C4 109.4(10) . . ? C30 C27 C4 110.1(5) . . ? C30' C27 C4 109.3(10) . . ? C28' C27 C29' 108.8(9) . . ? C30 C27 C29' 60.4(9) . . ? C30' C27 C29' 107.4(9) . . ? C4 C27 C29' 112.9(10) . . ? C28' C27 C28 49.3(8) . . ? C30 C27 C28 107.4(6) . . ? C30' C27 C28 61.3(9) . . ? C4 C27 C28 113.2(4) . . ? C29' C27 C28 133.6(10) . . ? C28' C27 C29 62.5(9) . . ? C30 C27 C29 108.1(6) . . ? C30' C27 C29 139.3(11) . . ? C4 C27 C29 110.9(5) . . ? C29' C27 C29 50.0(9) . . ? C28 C27 C29 106.9(6) . . ? C42 C41 C46 120.0 . . ? C42 C41 C40 119.9(8) . . ? C46 C41 C40 120.0(8) . . ? C41 C42 C43 120.0 . . ? C44 C43 C42 120.0 . . ? C43 C44 C45 120.0 . . ? C44 C45 C46 120.0 . . ? C45 C46 C41 120.0 . . ? C42' C41' C46' 120.0 . . ? C42' C41' C40' 118.6(7) . . ? C46' C41' C40' 121.4(7) . . ? C41' C42' C43' 120.0 . . ? C42' C43' C44' 120.0 . . ? C45' C44' C43' 120.0 . . ? C44' C45' C46' 120.0 . . ? C45' C46' C41' 120.0 . . ? _diffrn_measured_fraction_theta_max 0.893 _diffrn_reflns_theta_full 32.73 _diffrn_measured_fraction_theta_full 0.893 _refine_diff_density_max 0.665 _refine_diff_density_min -1.741 _refine_diff_density_rms 0.080