# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_q6_isopr_100 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C47 H78 Cl N25 O27' _chemical_formula_weight 1460.73 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 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' _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M R-3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 50.5752(14) _cell_length_b 50.5752(14) _cell_length_c 12.5528(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 27806.5(12) _cell_formula_units_Z 18 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 11574 _cell_measurement_theta_min 3.492 _cell_measurement_theta_max 71.303 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.542 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 13361 _exptl_absorpt_coefficient_mu 1.491 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.59288 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET) (compiled Aug 3 2011,13:03:54) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'SuperNova (Cu) X-ray Source' _diffrn_radiation_monochromator mirror _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Eos' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.2974 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18723 _diffrn_reflns_av_R_equivalents 0.0283 _diffrn_reflns_av_sigmaI/netI 0.0295 _diffrn_reflns_limit_h_min -61 _diffrn_reflns_limit_h_max 44 _diffrn_reflns_limit_k_min -45 _diffrn_reflns_limit_k_max 59 _diffrn_reflns_limit_l_min -5 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.50 _diffrn_reflns_theta_max 71.44 _reflns_number_total 11534 _reflns_number_gt 9551 _reflns_threshold_expression >2\s(I) _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET) (compiled Aug 3 2011,13:03:54) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET) (compiled Aug 3 2011,13:03:54) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET) (compiled Aug 3 2011,13:03:54) ; _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(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^)+(0.1044P)^2^+99.5990P] 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 11534 _refine_ls_number_parameters 1179 _refine_ls_number_restraints 421 _refine_ls_R_factor_all 0.0836 _refine_ls_R_factor_gt 0.0722 _refine_ls_wR_factor_ref 0.2047 _refine_ls_wR_factor_gt 0.1960 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.024 _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 O3W O 0.33080(18) 0.19260(16) 1.3254(7) 0.0636(19) Uani 0.663(5) 1 d P A 1 O7W O 0.31661(15) 0.1118(2) 1.8227(6) 0.081(2) Uani 0.663(5) 1 d P A 1 O8W O 0.29851(11) 0.21147(14) 0.6085(4) 0.0856(17) Uani 0.663(5) 1 d P A 1 O12W O 0.3460(2) 0.0383(2) 1.1936(8) 0.137(3) Uani 0.663(5) 1 d P A 1 O14W O 0.3083(2) -0.0192(3) 1.1871(16) 0.243(9) Uani 0.663(5) 1 d P A 1 C10X C 0.21070(15) 0.08529(11) 1.4030(4) 0.0481(12) Uani 0.68 1 d P A 1 H10A H 0.1928 0.0651 1.4146 0.072 Uiso 0.68 1 calc PR A 1 H10B H 0.2087 0.1005 1.4450 0.072 Uiso 0.68 1 calc PR A 1 H10C H 0.2291 0.0850 1.4251 0.072 Uiso 0.68 1 calc PR A 1 C11X C 0.21236(13) 0.07006(11) 1.2153(4) 0.0445(11) Uani 0.68 1 d P A 1 H11A H 0.2159 0.0768 1.1409 0.067 Uiso 0.68 1 calc PR A 1 H11B H 0.1923 0.0515 1.2218 0.067 Uiso 0.68 1 calc PR A 1 H11C H 0.2283 0.0657 1.2386 0.067 Uiso 0.68 1 calc PR A 1 C3X C 0.28437(13) 0.21624(13) 1.0633(6) 0.0484(13) Uani 0.663(5) 1 d PU A 1 H3X H 0.2844 0.2252 1.1299 0.058 Uiso 0.663(5) 1 calc PR A 1 C2X C 0.29101(11) 0.23352(12) 0.9693(6) 0.0496(13) Uani 0.663(5) 1 d PU A 1 C1X C 0.2912(4) 0.2203(3) 0.8711(7) 0.048(2) Uani 0.663(5) 1 d PU A 1 C6X C 0.28474(12) 0.19051(14) 0.8685(5) 0.0453(13) Uani 0.663(5) 1 d PU A 1 H6X H 0.2844 0.1813 0.8023 0.054 Uiso 0.663(5) 1 calc PR A 1 C5X C 0.2787(2) 0.17375(17) 0.9618(6) 0.0473(16) Uani 0.663(5) 1 d PU A 1 H5X H 0.2750 0.1534 0.9590 0.057 Uiso 0.663(5) 1 calc PR A 1 C4X C 0.2779(4) 0.1863(3) 1.0589(8) 0.051(3) Uani 0.663(5) 1 d PU A 1 C7X C 0.27630(12) 0.16803(10) 1.1565(4) 0.0387(10) Uani 0.663(5) 1 d PU A 1 H7X H 0.2934 0.1636 1.1596 0.046 Uiso 0.663(5) 1 calc PR A 1 C8X C 0.2450(3) 0.1392(4) 1.1655(17) 0.042(3) Uani 0.663(5) 1 d PU A 1 H8X1 H 0.2286 0.1444 1.1613 0.050 Uiso 0.663(5) 1 calc PR A 1 H8X2 H 0.2420 0.1249 1.1068 0.050 Uiso 0.663(5) 1 calc PR A 1 C9X C 0.2131(2) 0.0937(3) 1.2810(8) 0.0418(19) Uani 0.663(5) 1 d PU A 1 H9X H 0.1957 0.0968 1.2612 0.050 Uiso 0.663(5) 1 calc PR A 1 O1X O 0.29894(11) 0.23884(11) 0.7830(4) 0.0724(15) Uani 0.663(5) 1 d PU A 1 H1X H 0.2990 0.2291 0.7289 0.109 Uiso 0.663(5) 1 calc PR A 1 O2X O 0.29810(16) 0.26315(16) 0.9666(7) 0.0544(17) Uani 0.35 1 d PU A 1 H2X H 0.2974 0.2690 1.0286 0.082 Uiso 0.35 1 calc PR A 1 O3X O 0.27796(17) 0.18796(19) 1.2389(6) 0.0529(15) Uani 0.663(5) 1 d PU A 1 H3X1 H 0.2963 0.2007 1.2517 0.079 Uiso 0.663(5) 1 calc PR A 1 N1X N 0.24382(16) 0.1249(3) 1.2692(9) 0.050(2) Uani 0.663(5) 1 d PU A 1 H1X1 H 0.2454 0.1379 1.3233 0.060 Uiso 0.663(5) 1 calc PR A 1 H1X2 H 0.2601 0.1216 1.2746 0.060 Uiso 0.663(5) 1 calc PR A 1 C3XA C 0.2822(3) 0.2093(3) 1.0076(12) 0.056(3) Uani 0.337(5) 1 d PU A 2 H3XA H 0.2789 0.2210 1.0593 0.067 Uiso 0.337(5) 1 calc PR A 2 C1XA C 0.2928(3) 0.2025(6) 0.8259(13) 0.091(4) Uani 0.337(5) 1 d PU A 2 C2XA C 0.2900(8) 0.2202(8) 0.9040(18) 0.065(4) Uani 0.337(5) 1 d PU A 2 C6XA C 0.2906(4) 0.1728(4) 0.8558(13) 0.099(5) Uani 0.337(5) 1 d PU A 2 H6XA H 0.2957 0.1616 0.8076 0.119 Uiso 0.337(5) 1 calc PR A 2 C5XA C 0.2810(5) 0.1632(4) 0.9537(17) 0.072(5) Uani 0.337(5) 1 d PU A 2 H5XA H 0.2747 0.1425 0.9697 0.087 Uiso 0.337(5) 1 calc PR A 2 C4XA C 0.2793(6) 0.1811(6) 1.0365(18) 0.043(3) Uani 0.337(5) 1 d PU A 2 C7XA C 0.2602(3) 0.1705(3) 1.1552(9) 0.058(3) Uani 0.337(5) 1 d PU A 2 H7XA H 0.2421 0.1734 1.1560 0.070 Uiso 0.337(5) 1 calc PR A 2 C8XA C 0.2518(7) 0.1392(9) 1.165(4) 0.045(5) Uani 0.337(5) 1 d PU A 2 H8X3 H 0.2706 0.1377 1.1676 0.054 Uiso 0.337(5) 1 calc PR A 2 H8X4 H 0.2401 0.1280 1.1015 0.054 Uiso 0.337(5) 1 calc PR A 2 C9XA C 0.2204(6) 0.0930(6) 1.303(2) 0.065(6) Uani 0.337(5) 1 d PU A 2 O1XA O 0.3003(3) 0.2120(4) 0.7224(8) 0.150(7) Uani 0.337(5) 1 d PU A 2 H1XA H 0.3025 0.2295 0.7157 0.226 Uiso 0.337(5) 1 calc PR A 2 O2XB O 0.2949(2) 0.2483(3) 0.8739(15) 0.120(5) Uani 0.337(5) 1 d PU A 2 H2XB H 0.2927 0.2572 0.9269 0.180 Uiso 0.337(5) 1 calc PR A 2 O3XA O 0.2817(7) 0.1851(6) 1.2608(17) 0.119(10) Uani 0.337(5) 1 d PU A 2 H3X2 H 0.2994 0.1883 1.2480 0.178 Uiso 0.337(5) 1 calc PR A 2 N1XA N 0.2329(4) 0.1238(4) 1.2636(16) 0.046(4) Uani 0.337(5) 1 d PU A 2 H1X3 H 0.2443 0.1359 1.3194 0.055 Uiso 0.337(5) 1 calc PR A 2 H1X4 H 0.2163 0.1266 1.2583 0.055 Uiso 0.337(5) 1 calc PR A 2 C10A C 0.1889(5) 0.0790(5) 1.350(2) 0.050(5) Uani 0.16 1 d P A 2 H10D H 0.1762 0.0583 1.3219 0.075 Uiso 0.16 1 calc PR A 2 H10E H 0.1796 0.0914 1.3312 0.075 Uiso 0.16 1 calc PR A 2 H10F H 0.1902 0.0781 1.4277 0.075 Uiso 0.16 1 calc PR A 2 C11A C 0.2344(4) 0.0770(6) 1.2948(19) 0.053(6) Uani 0.16 1 d P A 2 H11D H 0.2205 0.0570 1.2638 0.080 Uiso 0.16 1 calc PR A 2 H11E H 0.2408 0.0744 1.3657 0.080 Uiso 0.16 1 calc PR A 2 H11F H 0.2524 0.0879 1.2489 0.080 Uiso 0.16 1 calc PR A 2 O7WA O 0.3277(5) 0.1172(4) 1.7800(14) 0.140(9) Uani 0.337(5) 1 d P A 2 O8WA O 0.3107(3) 0.2866(3) 1.0386(14) 0.109(5) Uani 0.337(5) 1 d P A 2 O3WA O 0.3354(6) 0.1897(6) 1.326(3) 0.125(10) Uani 0.337(5) 1 d P A 2 O14A O 0.3342(10) -0.0166(7) 1.152(2) 0.271(17) Uani 0.337(5) 1 d P A 2 O2XA O 0.2864(3) 0.1773(3) 0.7756(9) 0.093(4) Uani 0.30 1 d P B 3 C10B C 0.2258(8) 0.0787(8) 1.390(3) 0.080(10) Uani 0.16 1 d P C 3 C11B C 0.1986(6) 0.0777(6) 1.218(2) 0.058(6) Uani 0.16 1 d P D 3 O1W O 0.20573(7) -0.01638(8) 1.7747(2) 0.0766(9) Uani 1 1 d . . . O2W O 0.27036(7) 0.21737(6) 1.4341(2) 0.0648(7) Uani 1 1 d . . . O5W O 0.16645(9) 0.17712(8) 1.5630(3) 0.0963(12) Uani 1 1 d . . . O6W O 0.06124(10) 0.03323(9) 1.6513(3) 0.0705(15) Uani 0.720(9) 1 d P E 1 O6WA O 0.0300(5) 0.0363(4) 1.802(3) 0.25(2) Uani 0.280(9) 1 d P E 2 O10W O 0.0000 0.0000 1.3910(10) 0.173(4) Uani 1 3 d S . . Cl1 Cl 0.04788(9) 0.07041(13) 1.1184(3) 0.1374(19) Uani 0.50 1 d P F 1 Cl1A Cl 0.06025(17) 0.09550(17) 1.1878(6) 0.128(2) Uani 0.30 1 d P G 2 Cl1B Cl 0.009(2) 0.0404(7) 1.016(3) 0.43(3) Uani 0.20 1 d P . 3 O11W O 0.3246(7) 0.2667(10) 1.315(2) 0.167(18) Uani 0.23(4) 1 d P H 1 O111 O 0.3135(4) 0.2680(2) 1.3408(16) 0.179(7) Uani 0.77(4) 1 d P H 2 O9W O 0.29955(15) 0.0571(4) 0.8905(14) 0.085(4) Uani 0.61(4) 1 d P I 1 O13W O 0.2676(2) 0.0034(2) 0.7940(10) 0.100(4) Uani 0.426(14) 1 d P J 1 O9WA O 0.30018(16) 0.0446(5) 0.8634(9) 0.058(4) Uani 0.39(4) 1 d P I 2 O13A O 0.3234(14) 0.0433(13) 0.654(3) 0.26(3) Uani 0.33(3) 1 d P K 2 O13B O 0.2892(12) 0.0161(7) 0.680(4) 0.20(4) Uani 0.25(3) 1 d P L 3 O2 O 0.21453(5) 0.09644(4) 0.94673(15) 0.0394(5) Uani 1 1 d . . . O11 O 0.13696(4) -0.02773(4) 1.17370(15) 0.0352(4) Uani 1 1 d . . . O10 O 0.09836(5) 0.00256(5) 1.32826(17) 0.0471(5) Uani 1 1 d . . . N15 N 0.17323(5) -0.00173(5) 1.04379(17) 0.0299(5) Uani 1 1 d . . . O7 O 0.18976(6) 0.03533(5) 1.67270(18) 0.0500(6) Uani 1 1 d . . . O3 O 0.17926(5) 0.12679(5) 1.11037(17) 0.0444(5) Uani 1 1 d . . . O1 O 0.27711(5) 0.09831(5) 1.06719(19) 0.0488(5) Uani 1 1 d . . . N3 N 0.20264(5) 0.04593(5) 0.94443(17) 0.0324(5) Uani 1 1 d . . . O12 O 0.20089(5) -0.02500(6) 1.2711(2) 0.0575(7) Uani 1 1 d . . . O9 O 0.22699(6) 0.00454(5) 1.51948(19) 0.0508(6) Uani 1 1 d . . . N4 N 0.16543(6) 0.05629(5) 0.97447(18) 0.0346(5) Uani 1 1 d . . . O8 O 0.12436(6) 0.03451(6) 1.58319(19) 0.0560(6) Uani 1 1 d . . . C27 C 0.14706(6) -0.00957(6) 1.1008(2) 0.0303(5) Uani 1 1 d . . . N21 N 0.20330(6) 0.08601(5) 1.68568(18) 0.0387(5) Uani 1 1 d . . . N16 N 0.13404(5) 0.00632(5) 1.05906(18) 0.0349(5) Uani 1 1 d . . . N17 N 0.11096(6) 0.02883(6) 1.16849(19) 0.0383(5) Uani 1 1 d . . . O4 O 0.30434(6) 0.12905(5) 1.3181(2) 0.0613(7) Uani 1 1 d . . . N14 N 0.21721(5) -0.00421(5) 1.10457(19) 0.0354(5) Uani 1 1 d . . . N2 N 0.24622(5) 0.04712(5) 1.02935(19) 0.0357(5) Uani 1 1 d . . . N5 N 0.14015(6) 0.07774(6) 1.07823(19) 0.0406(6) Uani 1 1 d . . . N13 N 0.25066(6) 0.01142(6) 1.2372(2) 0.0406(6) Uani 1 1 d . . . O5 O 0.20959(7) 0.15604(5) 1.36891(18) 0.0573(7) Uani 1 1 d . . . N6 N 0.13927(6) 0.10052(6) 1.22766(19) 0.0415(6) Uani 1 1 d . . . N22 N 0.24004(7) 0.07439(6) 1.6700(2) 0.0444(6) Uani 1 1 d . . . C33 C 0.20889(7) 0.06246(7) 1.6749(2) 0.0387(6) Uani 1 1 d . . . N18 N 0.10610(6) 0.05144(6) 1.31256(19) 0.0428(6) Uani 1 1 d . . . C3 C 0.19629(7) 0.06917(6) 0.95488(19) 0.0327(6) Uani 1 1 d . . . N24 N 0.26957(6) 0.03081(7) 1.4131(2) 0.0432(6) Uani 1 1 d . . . N20 N 0.15793(7) 0.08545(6) 1.61797(19) 0.0422(6) Uani 1 1 d . . . N8 N 0.19178(7) 0.13420(6) 1.5337(2) 0.0485(7) Uani 1 1 d . . . N1 N 0.28238(6) 0.06046(6) 1.1512(2) 0.0416(6) Uani 1 1 d . . . N12 N 0.29873(6) 0.08091(6) 1.3291(2) 0.0453(6) Uani 1 1 d . . . C5 C 0.15565(7) 0.10407(7) 1.1365(2) 0.0366(6) Uani 1 1 d . . . N7 N 0.15876(8) 0.12208(7) 1.4008(2) 0.0482(7) Uani 1 1 d . . . C26 C 0.18809(6) -0.01990(6) 1.0513(2) 0.0337(6) Uani 1 1 d . . . H26A H 0.1746 -0.0390 1.0904 0.040 Uiso 1 1 calc R . . H26B H 0.1911 -0.0256 0.9786 0.040 Uiso 1 1 calc R . . N19 N 0.12468(6) 0.07356(6) 1.48665(19) 0.0431(6) Uani 1 1 d . . . C2 C 0.23328(6) 0.05123(6) 0.9322(2) 0.0356(6) Uani 1 1 d . . . H2A H 0.2465 0.0723 0.9061 0.043 Uiso 1 1 calc R . . H2B H 0.2332 0.0371 0.8774 0.043 Uiso 1 1 calc R . . N23 N 0.26406(6) 0.05431(7) 1.5531(2) 0.0458(6) Uani 1 1 d . . . O6 O 0.26940(8) 0.15692(7) 1.4676(2) 0.0777(9) Uani 1 1 d . . . C15 C 0.17561(6) 0.01605(6) 0.9497(2) 0.0301(5) Uani 1 1 d . . . H15 H 0.1729 0.0041 0.8830 0.036 Uiso 1 1 calc R . . N11 N 0.29885(6) 0.10432(7) 1.4785(2) 0.0513(7) Uani 1 1 d . . . C29 C 0.10465(6) 0.02529(7) 1.2755(2) 0.0394(6) Uani 1 1 d . . . C25 C 0.22055(7) -0.00780(7) 1.2100(2) 0.0401(6) Uani 1 1 d . . . C14 C 0.24515(6) 0.01839(6) 1.0549(2) 0.0352(6) Uani 1 1 d . . . H14 H 0.2505 0.0099 0.9919 0.042 Uiso 1 1 calc R . . C28 C 0.10619(6) 0.00352(7) 1.1016(2) 0.0378(6) Uani 1 1 d . . . H28A H 0.0955 -0.0156 1.1437 0.045 Uiso 1 1 calc R . . H28B H 0.0927 0.0018 1.0417 0.045 Uiso 1 1 calc R . . C18 C 0.11025(7) 0.07253(8) 1.2278(2) 0.0429(7) Uani 1 1 d . . . H18 H 0.0929 0.0766 1.2245 0.051 Uiso 1 1 calc R . . C7 C 0.18867(9) 0.13905(7) 1.4290(2) 0.0483(8) Uani 1 1 d . . . N10 N 0.27282(7) 0.12392(7) 1.5876(2) 0.0542(7) Uani 1 1 d . . . C16 C 0.14939(6) 0.02330(6) 0.9645(2) 0.0321(6) Uani 1 1 d . . . H16 H 0.1353 0.0163 0.9017 0.039 Uiso 1 1 calc R . . C35 C 0.25116(7) 0.02754(7) 1.4971(2) 0.0410(7) Uani 1 1 d . . . N9 N 0.23685(7) 0.13649(6) 1.6105(2) 0.0517(7) Uani 1 1 d . . . C31 C 0.13462(7) 0.06154(7) 1.5641(2) 0.0421(7) Uani 1 1 d . . . C32 C 0.17319(8) 0.08139(7) 1.7085(2) 0.0412(7) Uani 1 1 d . . . H32A H 0.1603 0.0605 1.7366 0.049 Uiso 1 1 calc R . . H32B H 0.1750 0.0958 1.7651 0.049 Uiso 1 1 calc R . . C4 C 0.15035(8) 0.07434(7) 0.9738(2) 0.0403(7) Uani 1 1 d . . . H4A H 0.1646 0.0949 0.9449 0.048 Uiso 1 1 calc R . . H4B H 0.1325 0.0646 0.9255 0.048 Uiso 1 1 calc R . . C24 C 0.29737(7) 0.06030(8) 1.4119(3) 0.0469(7) Uani 1 1 d . . . H24 H 0.3160 0.0582 1.4123 0.056 Uiso 1 1 calc R . . C22 C 0.25696(8) 0.10724(8) 1.6820(2) 0.0462(7) Uani 1 1 d . . . H22 H 0.2709 0.1136 1.7451 0.055 Uiso 1 1 calc R . . C21 C 0.23137(8) 0.11539(7) 1.6966(2) 0.0450(7) Uani 1 1 d . . . H21 H 0.2327 0.1249 1.7677 0.054 Uiso 1 1 calc R . . C13 C 0.26900(7) 0.02755(7) 1.1452(2) 0.0386(6) Uani 1 1 d . . . H13 H 0.2846 0.0215 1.1287 0.046 Uiso 1 1 calc R . . C34 C 0.25357(10) 0.05537(9) 1.6600(3) 0.0547(9) Uani 1 1 d . . . H34A H 0.2384 0.0344 1.6822 0.066 Uiso 1 1 calc R . . H34B H 0.2711 0.0629 1.7096 0.066 Uiso 1 1 calc R . . C36 C 0.26293(7) 0.00731(8) 1.3357(3) 0.0444(7) Uani 1 1 d . . . H36A H 0.2481 -0.0127 1.3668 0.053 Uiso 1 1 calc R . . H36B H 0.2819 0.0069 1.3201 0.053 Uiso 1 1 calc R . . C9 C 0.26046(9) 0.14086(8) 1.5472(3) 0.0581(9) Uani 1 1 d . . . C12 C 0.30745(7) 0.07972(9) 1.2201(3) 0.0497(8) Uani 1 1 d . . . H12A H 0.3180 0.1007 1.1907 0.060 Uiso 1 1 calc R . . H12B H 0.3222 0.0723 1.2201 0.060 Uiso 1 1 calc R . . C1 C 0.26944(6) 0.07141(7) 1.0813(2) 0.0386(6) Uani 1 1 d . . . C11 C 0.30113(7) 0.10703(8) 1.3702(3) 0.0497(8) Uani 1 1 d . . . C19 C 0.13944(9) 0.10655(8) 1.4921(2) 0.0469(8) Uani 1 1 d . . . H19 H 0.1245 0.1136 1.5062 0.056 Uiso 1 1 calc R . . C17 C 0.11179(7) 0.05599(7) 1.1265(2) 0.0390(6) Uani 1 1 d . . . H17 H 0.0941 0.0507 1.0780 0.047 Uiso 1 1 calc R . . C8 C 0.21965(10) 0.15192(7) 1.5937(3) 0.0591(10) Uani 1 1 d . . . H8A H 0.2327 0.1713 1.5555 0.071 Uiso 1 1 calc R . . H8B H 0.2145 0.1571 1.6639 0.071 Uiso 1 1 calc R . . C20 C 0.16238(9) 0.11483(7) 1.5841(2) 0.0470(8) Uani 1 1 d . . . H20 H 0.1584 0.1256 1.6432 0.056 Uiso 1 1 calc R . . C30 C 0.09839(8) 0.05487(9) 1.4211(2) 0.0496(8) Uani 1 1 d . . . H30A H 0.0851 0.0641 1.4195 0.059 Uiso 1 1 calc R . . H30B H 0.0866 0.0344 1.4539 0.059 Uiso 1 1 calc R . . C6 C 0.14711(9) 0.12560(8) 1.3006(2) 0.0496(8) Uani 1 1 d . . . H6A H 0.1626 0.1448 1.2667 0.060 Uiso 1 1 calc R . . H6B H 0.1287 0.1273 1.3139 0.060 Uiso 1 1 calc R . . C10 C 0.30155(8) 0.12797(9) 1.5497(3) 0.0600(10) Uani 1 1 d . . . H101 H 0.3140 0.1288 1.6119 0.072 Uiso 1 1 calc R . . H102 H 0.3127 0.1478 1.5124 0.072 Uiso 1 1 calc R . . C23 C 0.29457(8) 0.07544(9) 1.5154(3) 0.0507(8) Uani 1 1 d . . . H23 H 0.3104 0.0783 1.5688 0.061 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 O3W 0.039(3) 0.035(3) 0.086(4) 0.017(3) 0.015(3) -0.005(3) O7W 0.058(3) 0.111(5) 0.082(5) -0.007(4) -0.009(3) 0.048(3) O8W 0.056(3) 0.128(5) 0.056(3) 0.014(3) 0.004(2) 0.033(3) O12W 0.163(8) 0.139(7) 0.148(7) -0.007(5) -0.003(6) 0.104(6) O14W 0.096(6) 0.197(11) 0.44(2) -0.179(14) -0.067(10) 0.072(7) C10X 0.064(4) 0.037(2) 0.036(2) -0.0060(19) 0.011(2) 0.020(2) C11X 0.057(3) 0.034(2) 0.033(2) -0.0014(17) 0.006(2) 0.016(2) C3X 0.030(2) 0.045(3) 0.057(3) -0.002(2) 0.001(3) 0.009(2) C2X 0.029(2) 0.039(3) 0.072(4) 0.014(2) -0.009(2) 0.011(2) C1X 0.031(3) 0.053(3) 0.051(5) 0.021(4) -0.005(5) 0.014(3) C6X 0.028(2) 0.050(3) 0.039(3) 0.014(2) -0.001(2) 0.004(2) C5X 0.049(3) 0.042(4) 0.039(3) 0.008(3) 0.001(3) 0.014(3) C4X 0.045(4) 0.045(4) 0.046(4) 0.010(3) 0.012(3) 0.009(3) C7X 0.035(2) 0.036(2) 0.040(2) -0.0031(17) 0.0006(19) 0.014(2) C8X 0.041(6) 0.032(3) 0.038(4) 0.003(2) 0.006(5) 0.008(4) C9X 0.039(3) 0.042(3) 0.037(5) 0.012(3) 0.000(3) 0.015(3) O1X 0.059(3) 0.064(3) 0.068(3) 0.034(2) -0.008(2) 0.011(2) O2X 0.044(4) 0.044(3) 0.078(5) 0.004(3) -0.016(4) 0.024(3) O3X 0.056(3) 0.030(2) 0.058(4) -0.008(3) 0.007(3) 0.010(2) N1X 0.045(4) 0.045(3) 0.039(3) 0.0010(19) 0.000(3) 0.008(3) C3XA 0.042(5) 0.062(7) 0.062(6) 0.026(5) 0.016(6) 0.024(5) C1XA 0.030(6) 0.126(9) 0.051(6) 0.012(6) 0.001(5) -0.010(7) C2XA 0.024(6) 0.081(8) 0.055(8) 0.036(7) -0.006(9) 0.002(6) C6XA 0.065(8) 0.094(8) 0.071(7) -0.038(6) 0.022(7) -0.010(7) C5XA 0.051(8) 0.056(8) 0.068(7) -0.018(6) 0.006(6) -0.004(7) C4XA 0.037(6) 0.053(8) 0.049(6) 0.012(6) 0.006(7) 0.029(6) C7XA 0.068(7) 0.057(6) 0.051(5) 0.018(4) 0.016(5) 0.033(6) C8XA 0.044(11) 0.053(6) 0.035(7) -0.001(5) 0.019(8) 0.023(7) C9XA 0.098(15) 0.033(6) 0.048(9) 0.000(5) -0.020(9) 0.019(9) O1XA 0.084(8) 0.191(14) 0.050(5) 0.015(6) 0.016(5) -0.026(8) O2XB 0.038(5) 0.124(8) 0.186(14) 0.113(9) 0.031(7) 0.032(6) O3XA 0.176(18) 0.064(9) 0.043(6) 0.002(6) 0.007(7) 0.005(11) N1XA 0.067(9) 0.032(5) 0.032(6) 0.001(4) 0.018(8) 0.019(7) C10A 0.038(10) 0.043(11) 0.080(15) -0.004(10) 0.012(11) 0.028(9) C11A 0.029(9) 0.077(15) 0.061(14) -0.027(11) -0.007(9) 0.032(10) O7WA 0.21(2) 0.064(8) 0.097(12) -0.032(8) -0.109(13) 0.030(11) O8WA 0.085(8) 0.111(10) 0.158(13) 0.012(9) 0.013(8) 0.068(8) O3WA 0.094(13) 0.106(14) 0.19(2) -0.014(12) 0.051(12) 0.062(11) O14A 0.39(5) 0.21(3) 0.22(2) -0.15(2) -0.11(3) 0.15(3) O2XA 0.070(7) 0.113(10) 0.049(6) 0.005(6) 0.001(5) 0.011(6) C10B 0.07(2) 0.08(2) 0.064(18) -0.001(15) -0.041(16) 0.018(16) C11B 0.058(14) 0.058(14) 0.068(16) -0.001(12) -0.006(13) 0.037(13) O1W 0.0580(16) 0.091(2) 0.0554(16) -0.0037(15) 0.0063(13) 0.0182(16) O2W 0.0655(17) 0.0573(15) 0.0800(18) 0.0014(13) 0.0082(14) 0.0369(14) O5W 0.107(3) 0.074(2) 0.129(3) 0.028(2) 0.039(2) 0.061(2) O6W 0.069(3) 0.063(3) 0.073(3) -0.0212(19) 0.0021(19) 0.028(2) O6WA 0.129(16) 0.075(11) 0.41(4) 0.115(19) -0.11(2) -0.052(11) O10W 0.159(6) 0.159(6) 0.201(11) 0.000 0.000 0.080(3) Cl1 0.110(2) 0.243(5) 0.114(2) 0.103(3) 0.052(2) 0.129(3) Cl1A 0.131(5) 0.120(5) 0.155(6) -0.018(4) -0.025(4) 0.079(4) Cl1B 0.83(8) 0.137(14) 0.35(3) 0.082(17) 0.19(4) 0.27(3) O11W 0.069(15) 0.30(5) 0.100(16) -0.04(2) 0.031(11) 0.071(18) O111 0.135(9) 0.135(7) 0.235(12) 0.104(7) 0.019(9) 0.043(6) O9W 0.057(3) 0.074(7) 0.109(6) 0.006(6) 0.033(3) 0.022(3) O13W 0.097(7) 0.107(7) 0.099(8) -0.033(6) -0.029(5) 0.053(6) O9WA 0.025(3) 0.063(8) 0.073(5) -0.023(5) 0.014(3) 0.013(3) O13A 0.41(7) 0.35(6) 0.22(3) 0.10(3) 0.03(3) 0.35(6) O13B 0.31(6) 0.12(2) 0.25(5) -0.13(3) -0.23(5) 0.17(3) O2 0.0530(12) 0.0265(10) 0.0287(9) 0.0033(7) 0.0080(8) 0.0123(9) O11 0.0361(10) 0.0321(10) 0.0322(10) 0.0064(8) 0.0058(8) 0.0130(8) O10 0.0449(12) 0.0560(13) 0.0405(11) 0.0173(10) 0.0109(9) 0.0253(11) N15 0.0313(11) 0.0251(10) 0.0300(11) -0.0008(8) 0.0031(9) 0.0118(9) O7 0.0608(14) 0.0304(11) 0.0481(12) 0.0036(9) 0.0100(10) 0.0148(10) O3 0.0576(13) 0.0369(11) 0.0460(12) 0.0038(9) 0.0171(10) 0.0292(11) O1 0.0403(12) 0.0322(11) 0.0539(13) 0.0023(9) 0.0005(10) 0.0032(9) N3 0.0337(12) 0.0255(11) 0.0303(11) 0.0015(8) 0.0042(9) 0.0091(9) O12 0.0374(12) 0.0687(16) 0.0542(14) 0.0269(12) 0.0101(10) 0.0173(11) O9 0.0557(14) 0.0438(12) 0.0548(13) 0.0185(10) 0.0208(11) 0.0263(11) N4 0.0447(13) 0.0294(11) 0.0296(11) 0.0022(9) 0.0059(9) 0.0185(10) O8 0.0586(15) 0.0447(13) 0.0486(13) 0.0103(10) -0.0053(11) 0.0136(11) C27 0.0300(13) 0.0263(12) 0.0279(12) -0.0011(10) 0.0006(10) 0.0091(10) N21 0.0491(14) 0.0284(11) 0.0295(11) 0.0025(9) 0.0055(10) 0.0126(11) N16 0.0319(11) 0.0364(12) 0.0345(12) 0.0073(9) 0.0057(9) 0.0157(10) N17 0.0401(13) 0.0466(14) 0.0333(12) 0.0096(10) 0.0078(10) 0.0254(11) O4 0.0585(15) 0.0369(12) 0.0525(14) 0.0031(10) -0.0022(11) -0.0033(11) N14 0.0330(12) 0.0317(12) 0.0405(13) 0.0061(10) 0.0074(10) 0.0154(10) N2 0.0330(12) 0.0305(11) 0.0357(12) 0.0009(9) 0.0053(9) 0.0101(10) N5 0.0527(15) 0.0427(13) 0.0292(12) 0.0039(10) 0.0107(10) 0.0261(12) N13 0.0339(12) 0.0496(15) 0.0377(13) 0.0084(11) 0.0079(10) 0.0205(11) O5 0.0886(19) 0.0395(12) 0.0390(12) 0.0061(9) 0.0194(12) 0.0284(13) N6 0.0584(16) 0.0468(14) 0.0308(12) 0.0056(10) 0.0138(11) 0.0351(13) N22 0.0546(16) 0.0397(14) 0.0345(13) 0.0061(10) 0.0073(11) 0.0204(12) C33 0.0530(17) 0.0352(15) 0.0229(12) 0.0021(10) 0.0053(11) 0.0183(13) N18 0.0451(14) 0.0532(15) 0.0314(12) 0.0086(11) 0.0077(10) 0.0255(12) C3 0.0463(15) 0.0271(13) 0.0195(11) 0.0012(9) 0.0054(10) 0.0144(12) N24 0.0335(12) 0.0548(16) 0.0420(13) 0.0050(11) 0.0047(10) 0.0226(12) N20 0.0635(17) 0.0383(13) 0.0291(12) 0.0037(10) 0.0059(11) 0.0285(13) N8 0.077(2) 0.0399(14) 0.0353(13) 0.0044(11) 0.0133(13) 0.0337(14) N1 0.0311(12) 0.0422(13) 0.0401(13) 0.0010(11) 0.0021(10) 0.0097(11) N12 0.0347(13) 0.0494(15) 0.0387(13) 0.0004(11) 0.0003(10) 0.0112(11) C5 0.0499(17) 0.0436(16) 0.0309(13) 0.0058(12) 0.0068(12) 0.0342(14) N7 0.076(2) 0.0529(16) 0.0291(12) 0.0072(11) 0.0157(12) 0.0425(16) C26 0.0345(14) 0.0222(12) 0.0411(14) 0.0008(10) 0.0052(11) 0.0118(11) N19 0.0547(15) 0.0549(16) 0.0312(12) 0.0045(11) 0.0095(11) 0.0361(13) C2 0.0352(14) 0.0323(13) 0.0301(13) 0.0051(11) 0.0081(11) 0.0101(11) N23 0.0469(15) 0.0546(16) 0.0358(13) 0.0068(11) 0.0054(11) 0.0253(13) O6 0.093(2) 0.0584(16) 0.0656(17) 0.0315(14) 0.0322(16) 0.0259(16) C15 0.0334(13) 0.0247(12) 0.0268(12) -0.0006(9) 0.0029(10) 0.0105(11) N11 0.0405(14) 0.0484(16) 0.0428(14) -0.0008(12) 0.0011(11) 0.0056(12) C29 0.0303(14) 0.0538(18) 0.0356(14) 0.0115(13) 0.0069(11) 0.0222(13) C25 0.0338(14) 0.0419(16) 0.0471(16) 0.0100(13) 0.0099(12) 0.0209(13) C14 0.0331(14) 0.0319(13) 0.0378(14) 0.0018(11) 0.0072(11) 0.0141(11) C28 0.0294(13) 0.0393(15) 0.0412(15) 0.0063(12) 0.0042(11) 0.0145(12) C18 0.0474(17) 0.063(2) 0.0342(14) 0.0119(13) 0.0116(13) 0.0392(16) C7 0.083(3) 0.0371(16) 0.0349(15) 0.0030(13) 0.0159(16) 0.0375(17) N10 0.0526(16) 0.0442(15) 0.0473(15) 0.0073(12) 0.0099(13) 0.0104(13) C16 0.0365(14) 0.0313(13) 0.0231(12) 0.0003(10) 0.0012(10) 0.0129(11) C35 0.0442(16) 0.0485(17) 0.0387(15) 0.0113(13) 0.0054(12) 0.0293(15) N9 0.0638(18) 0.0351(13) 0.0419(14) 0.0100(11) 0.0098(13) 0.0141(13) C31 0.0499(17) 0.0478(18) 0.0319(14) 0.0050(12) 0.0111(12) 0.0268(15) C32 0.0577(18) 0.0384(15) 0.0254(13) 0.0058(11) 0.0103(12) 0.0224(14) C4 0.0623(19) 0.0413(15) 0.0267(13) 0.0080(11) 0.0114(12) 0.0330(15) C24 0.0299(14) 0.063(2) 0.0434(16) 0.0029(14) -0.0017(12) 0.0197(14) C22 0.0499(18) 0.0448(17) 0.0307(14) 0.0003(12) 0.0011(13) 0.0137(14) C21 0.0577(19) 0.0308(14) 0.0320(14) 0.0018(11) 0.0023(13) 0.0111(14) C13 0.0329(14) 0.0453(16) 0.0376(15) 0.0048(12) 0.0100(11) 0.0195(13) C34 0.073(2) 0.066(2) 0.0340(16) 0.0149(15) 0.0104(15) 0.042(2) C36 0.0422(16) 0.0511(18) 0.0473(17) 0.0093(14) 0.0075(13) 0.0288(15) C9 0.066(2) 0.0384(17) 0.0469(18) 0.0087(14) 0.0132(17) 0.0087(16) C12 0.0280(14) 0.059(2) 0.0422(17) 0.0009(14) 0.0036(12) 0.0069(14) C1 0.0312(14) 0.0360(15) 0.0381(14) 0.0011(12) 0.0076(11) 0.0090(12) C11 0.0304(15) 0.0467(18) 0.0467(17) -0.0011(15) -0.0022(13) 0.0004(13) C19 0.074(2) 0.0577(19) 0.0297(14) 0.0070(13) 0.0163(14) 0.0490(18) C17 0.0399(15) 0.0505(17) 0.0336(14) 0.0086(12) 0.0026(11) 0.0278(14) C8 0.094(3) 0.0280(15) 0.0467(18) 0.0005(13) 0.0060(18) 0.0239(17) C20 0.081(2) 0.0438(17) 0.0304(14) 0.0031(12) 0.0145(14) 0.0419(17) C30 0.0439(17) 0.075(2) 0.0351(15) 0.0116(15) 0.0141(13) 0.0339(17) C6 0.088(3) 0.0498(18) 0.0312(14) 0.0066(13) 0.0155(15) 0.0499(19) C10 0.0448(18) 0.051(2) 0.052(2) -0.0062(16) 0.0054(15) -0.0005(16) C23 0.0366(16) 0.069(2) 0.0419(17) -0.0004(15) -0.0070(13) 0.0226(16) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 C10X C9X 1.578(10) . ? C11X C9X 1.438(14) . ? C3X C4X 1.379(13) . ? C3X C2X 1.406(9) . ? C2X O2X 1.356(9) . ? C2X C1X 1.404(13) . ? C1X C6X 1.372(13) . ? C1X O1X 1.375(9) . ? C6X C5X 1.386(9) . ? C5X C4X 1.384(10) . ? C4X C7X 1.514(13) . ? C7X O3X 1.417(9) . ? C7X C8X 1.531(14) . ? C8X N1X 1.47(2) . ? C9X N1X 1.571(14) . ? C3XA C2XA 1.39(2) . ? C3XA C4XA 1.40(3) . ? C1XA O1XA 1.37(2) . ? C1XA C2XA 1.38(4) . ? C1XA C6XA 1.50(3) . ? C2XA O2XB 1.37(3) . ? C6XA C5XA 1.32(3) . ? C5XA C4XA 1.41(2) . ? C4XA C7XA 1.71(3) . ? C7XA C8XA 1.43(4) . ? C7XA O3XA 1.64(3) . ? C8XA N1XA 1.52(5) . ? C9XA C11A 1.32(3) . ? C9XA N1XA 1.44(3) . ? C9XA C10A 1.51(3) . ? Cl1B Cl1B 1.90(2) 11_557 ? Cl1B Cl1B 1.90(2) 12_557 ? O2 C3 1.221(3) . ? O11 C27 1.214(3) . ? O10 C29 1.223(4) . ? N15 C27 1.377(3) . ? N15 C26 1.452(3) . ? N15 C15 1.453(3) . ? O7 C33 1.222(4) . ? O3 C5 1.217(4) . ? O1 C1 1.227(4) . ? N3 C3 1.371(4) . ? N3 C2 1.443(4) . ? N3 C15 1.446(3) . ? O12 C25 1.212(4) . ? O9 C35 1.226(4) . ? N4 C3 1.380(4) . ? N4 C16 1.451(3) . ? N4 C4 1.453(4) . ? O8 C31 1.219(4) . ? C27 N16 1.372(4) . ? N21 C33 1.362(4) . ? N21 C32 1.449(4) . ? N21 C21 1.461(4) . ? N16 C16 1.443(3) . ? N16 C28 1.446(4) . ? N17 C29 1.372(4) . ? N17 C28 1.446(4) . ? N17 C17 1.453(4) . ? O4 C11 1.230(4) . ? N14 C25 1.358(4) . ? N14 C14 1.441(3) . ? N14 C26 1.441(4) . ? N2 C1 1.368(4) . ? N2 C2 1.448(4) . ? N2 C14 1.462(4) . ? N5 C5 1.371(4) . ? N5 C17 1.434(4) . ? N5 C4 1.450(3) . ? N13 C25 1.379(4) . ? N13 C36 1.444(4) . ? N13 C13 1.451(4) . ? O5 C7 1.232(4) . ? N6 C5 1.371(4) . ? N6 C18 1.442(4) . ? N6 C6 1.450(4) . ? N22 C33 1.378(4) . ? N22 C34 1.438(5) . ? N22 C22 1.447(4) . ? N18 C29 1.369(4) . ? N18 C18 1.446(4) . ? N18 C30 1.451(4) . ? N24 C35 1.361(4) . ? N24 C36 1.439(4) . ? N24 C24 1.450(4) . ? N20 C31 1.372(4) . ? N20 C32 1.445(4) . ? N20 C20 1.451(4) . ? N8 C7 1.361(4) . ? N8 C8 1.447(5) . ? N8 C20 1.454(5) . ? N1 C1 1.367(4) . ? N1 C12 1.439(4) . ? N1 C13 1.452(4) . ? N12 C11 1.366(5) . ? N12 C12 1.448(4) . ? N12 C24 1.449(4) . ? N7 C7 1.361(5) . ? N7 C6 1.437(4) . ? N7 C19 1.455(4) . ? N19 C31 1.369(4) . ? N19 C30 1.443(5) . ? N19 C19 1.449(4) . ? N23 C35 1.367(4) . ? N23 C23 1.449(4) . ? N23 C34 1.454(4) . ? O6 C9 1.223(4) . ? C15 C16 1.554(4) . ? N11 C11 1.366(4) . ? N11 C23 1.441(5) . ? N11 C10 1.444(5) . ? C14 C13 1.547(4) . ? C18 C17 1.546(4) . ? N10 C9 1.385(5) . ? N10 C22 1.443(4) . ? N10 C10 1.443(5) . ? N9 C9 1.358(5) . ? N9 C21 1.445(4) . ? N9 C8 1.445(5) . ? C24 C23 1.549(5) . ? C22 C21 1.553(5) . ? C19 C20 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 C4X C3X C2X 120.0(7) . . ? O2X C2X C1X 116.4(7) . . ? O2X C2X C3X 123.8(7) . . ? C1X C2X C3X 119.8(6) . . ? C6X C1X O1X 124.1(9) . . ? C6X C1X C2X 119.3(7) . . ? O1X C1X C2X 116.6(9) . . ? C1X C6X C5X 120.6(7) . . ? C4X C5X C6X 120.7(8) . . ? C3X C4X C5X 119.6(9) . . ? C3X C4X C7X 123.3(7) . . ? C5X C4X C7X 115.9(9) . . ? O3X C7X C4X 100.9(6) . . ? O3X C7X C8X 106.8(9) . . ? C4X C7X C8X 110.9(10) . . ? N1X C8X C7X 107.5(12) . . ? C11X C9X N1X 112.6(8) . . ? C11X C9X C10X 111.4(7) . . ? N1X C9X C10X 105.5(8) . . ? C8X N1X C9X 110.6(9) . . ? C2XA C3XA C4XA 121(2) . . ? O1XA C1XA C2XA 123(3) . . ? O1XA C1XA C6XA 117(2) . . ? C2XA C1XA C6XA 119.3(18) . . ? O2XB C2XA C1XA 117(2) . . ? O2XB C2XA C3XA 123(3) . . ? C1XA C2XA C3XA 121(3) . . ? C5XA C6XA C1XA 115.6(18) . . ? C6XA C5XA C4XA 125(2) . . ? C3XA C4XA C5XA 116.9(19) . . ? C3XA C4XA C7XA 107.8(15) . . ? C5XA C4XA C7XA 130.2(19) . . ? C8XA C7XA O3XA 101(2) . . ? C8XA C7XA C4XA 103.8(19) . . ? O3XA C7XA C4XA 114.9(16) . . ? C7XA C8XA N1XA 114(3) . . ? C11A C9XA N1XA 124(3) . . ? C11A C9XA C10A 121(2) . . ? N1XA C9XA C10A 116(2) . . ? C9XA N1XA C8XA 131(2) . . ? Cl1B Cl1B Cl1B 115.5(16) 11_557 12_557 ? C27 N15 C26 120.8(2) . . ? C27 N15 C15 111.8(2) . . ? C26 N15 C15 122.4(2) . . ? C3 N3 C2 122.8(2) . . ? C3 N3 C15 112.8(2) . . ? C2 N3 C15 124.4(2) . . ? C3 N4 C16 112.2(2) . . ? C3 N4 C4 121.8(2) . . ? C16 N4 C4 123.7(2) . . ? O11 C27 N16 126.0(3) . . ? O11 C27 N15 126.1(3) . . ? N16 C27 N15 107.9(2) . . ? C33 N21 C32 122.7(2) . . ? C33 N21 C21 112.2(3) . . ? C32 N21 C21 123.6(3) . . ? C27 N16 C16 112.9(2) . . ? C27 N16 C28 122.1(2) . . ? C16 N16 C28 124.8(2) . . ? C29 N17 C28 121.9(3) . . ? C29 N17 C17 111.9(2) . . ? C28 N17 C17 122.6(2) . . ? C25 N14 C14 112.9(2) . . ? C25 N14 C26 122.7(2) . . ? C14 N14 C26 124.3(2) . . ? C1 N2 C2 121.3(2) . . ? C1 N2 C14 112.1(2) . . ? C2 N2 C14 122.2(2) . . ? C5 N5 C17 112.7(2) . . ? C5 N5 C4 122.2(3) . . ? C17 N5 C4 124.7(3) . . ? C25 N13 C36 120.9(3) . . ? C25 N13 C13 111.6(2) . . ? C36 N13 C13 124.3(2) . . ? C5 N6 C18 112.4(3) . . ? C5 N6 C6 122.0(3) . . ? C18 N6 C6 123.8(3) . . ? C33 N22 C34 122.2(3) . . ? C33 N22 C22 112.9(3) . . ? C34 N22 C22 124.8(3) . . ? O7 C33 N21 126.2(3) . . ? O7 C33 N22 125.5(3) . . ? N21 C33 N22 108.3(3) . . ? C29 N18 C18 112.4(2) . . ? C29 N18 C30 123.1(3) . . ? C18 N18 C30 123.5(3) . . ? O2 C3 N3 126.3(3) . . ? O2 C3 N4 125.9(3) . . ? N3 C3 N4 107.9(2) . . ? C35 N24 C36 124.0(3) . . ? C35 N24 C24 112.7(3) . . ? C36 N24 C24 123.2(3) . . ? C31 N20 C32 123.1(3) . . ? C31 N20 C20 112.6(3) . . ? C32 N20 C20 123.7(3) . . ? C7 N8 C8 123.8(3) . . ? C7 N8 C20 111.7(3) . . ? C8 N8 C20 122.8(3) . . ? C1 N1 C12 123.4(3) . . ? C1 N1 C13 112.8(2) . . ? C12 N1 C13 123.7(3) . . ? C11 N12 C12 121.0(3) . . ? C11 N12 C24 112.0(3) . . ? C12 N12 C24 123.6(3) . . ? O3 C5 N5 126.0(3) . . ? O3 C5 N6 126.3(3) . . ? N5 C5 N6 107.7(3) . . ? C7 N7 C6 123.0(3) . . ? C7 N7 C19 111.7(3) . . ? C6 N7 C19 123.3(3) . . ? N14 C26 N15 113.0(2) . . ? C31 N19 C30 122.5(3) . . ? C31 N19 C19 112.7(3) . . ? C30 N19 C19 123.8(3) . . ? N3 C2 N2 113.9(2) . . ? C35 N23 C23 111.5(3) . . ? C35 N23 C34 120.6(3) . . ? C23 N23 C34 123.3(3) . . ? N3 C15 N15 115.3(2) . . ? N3 C15 C16 103.4(2) . . ? N15 C15 C16 103.5(2) . . ? C11 N11 C23 112.6(3) . . ? C11 N11 C10 124.4(3) . . ? C23 N11 C10 123.0(3) . . ? O10 C29 N18 126.0(3) . . ? O10 C29 N17 126.0(3) . . ? N18 C29 N17 108.1(3) . . ? O12 C25 N14 126.9(3) . . ? O12 C25 N13 124.7(3) . . ? N14 C25 N13 108.4(2) . . ? N14 C14 N2 114.7(2) . . ? N14 C14 C13 103.2(2) . . ? N2 C14 C13 103.1(2) . . ? N16 C28 N17 113.9(2) . . ? N6 C18 N18 115.2(3) . . ? N6 C18 C17 103.2(2) . . ? N18 C18 C17 103.6(2) . . ? O5 C7 N8 125.5(4) . . ? O5 C7 N7 125.2(3) . . ? N8 C7 N7 109.3(3) . . ? C9 N10 C22 111.8(3) . . ? C9 N10 C10 121.7(3) . . ? C22 N10 C10 125.4(3) . . ? N16 C16 N4 116.0(2) . . ? N16 C16 C15 103.1(2) . . ? N4 C16 C15 103.2(2) . . ? O9 C35 N24 126.1(3) . . ? O9 C35 N23 125.3(3) . . ? N24 C35 N23 108.6(3) . . ? C9 N9 C21 112.7(3) . . ? C9 N9 C8 123.0(3) . . ? C21 N9 C8 124.3(3) . . ? O8 C31 N19 126.3(3) . . ? O8 C31 N20 126.0(3) . . ? N19 C31 N20 107.6(3) . . ? N20 C32 N21 114.5(2) . . ? N5 C4 N4 113.5(2) . . ? N12 C24 N24 114.9(3) . . ? N12 C24 C23 103.2(3) . . ? N24 C24 C23 102.6(3) . . ? N10 C22 N22 115.0(3) . . ? N10 C22 C21 103.6(3) . . ? N22 C22 C21 103.0(3) . . ? N9 C21 N21 114.3(3) . . ? N9 C21 C22 103.3(3) . . ? N21 C21 C22 103.5(3) . . ? N13 C13 N1 113.8(2) . . ? N13 C13 C14 103.4(2) . . ? N1 C13 C14 103.2(2) . . ? N22 C34 N23 114.1(3) . . ? N24 C36 N13 113.5(3) . . ? O6 C9 N9 126.1(4) . . ? O6 C9 N10 125.4(4) . . ? N9 C9 N10 108.5(3) . . ? N1 C12 N12 114.4(2) . . ? O1 C1 N1 126.3(3) . . ? O1 C1 N2 125.5(3) . . ? N1 C1 N2 108.2(3) . . ? O4 C11 N12 125.6(3) . . ? O4 C11 N11 125.9(4) . . ? N12 C11 N11 108.4(3) . . ? N19 C19 N7 113.9(2) . . ? N19 C19 C20 103.5(2) . . ? N7 C19 C20 103.5(3) . . ? N5 C17 N17 115.1(2) . . ? N5 C17 C18 103.5(3) . . ? N17 C17 C18 103.2(2) . . ? N9 C8 N8 113.8(3) . . ? N20 C20 N8 113.6(3) . . ? N20 C20 C19 103.4(3) . . ? N8 C20 C19 103.5(2) . . ? N19 C30 N18 113.5(3) . . ? N7 C6 N6 113.2(3) . . ? N10 C10 N11 114.5(3) . . ? N11 C23 N23 114.7(3) . . ? N11 C23 C24 103.1(3) . . ? N23 C23 C24 103.7(3) . . ? _diffrn_measured_fraction_theta_max 0.957 _diffrn_reflns_theta_full 71.44 _diffrn_measured_fraction_theta_full 0.957 _refine_diff_density_max 0.872 _refine_diff_density_min -0.523 _refine_diff_density_rms 0.071 _database_code_depnum_ccdc_archive 'CCDC 946817' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_q6_isopr_old_s _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C47 H78 Cl2 Mg0.50 N25 O27' _chemical_formula_weight 1508.34 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' Mg Mg 0.1719 0.1771 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/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 18.1241(3) _cell_length_b 16.4081(2) _cell_length_c 21.0869(3) _cell_angle_alpha 90.00 _cell_angle_beta 98.9170(10) _cell_angle_gamma 90.00 _cell_volume 6195.07(15) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 12199 _cell_measurement_theta_min 3.4259 _cell_measurement_theta_max 71.8391 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.587 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3060 _exptl_absorpt_coefficient_mu 1.937 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.64208 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'SuperNova (Cu) X-ray Source' _diffrn_radiation_monochromator mirror _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Eos' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.2974 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23986 _diffrn_reflns_av_R_equivalents 0.0240 _diffrn_reflns_av_sigmaI/netI 0.0284 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.65 _diffrn_reflns_theta_max 71.98 _reflns_number_total 11906 _reflns_number_gt 10347 _reflns_threshold_expression >2\s(I) _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(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^)+(0.1281P)^2^+5.5924P] 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 11906 _refine_ls_number_parameters 1185 _refine_ls_number_restraints 554 _refine_ls_R_factor_all 0.0743 _refine_ls_R_factor_gt 0.0676 _refine_ls_wR_factor_ref 0.2010 _refine_ls_wR_factor_gt 0.1934 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.035 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O8W O 0.1234(3) 0.2899(4) -0.0083(3) 0.0821(15) Uani 0.64 1 d P A 1 C1X C 0.2962(3) 0.1650(4) 0.0664(2) 0.0307(4) Uani 0.688(3) 1 d PU B 1 C2X C 0.3328(3) 0.2090(4) 0.0243(3) 0.0306(4) Uani 0.688(3) 1 d PU B 1 C3X C 0.4113(4) 0.2037(4) 0.0304(4) 0.0303(4) Uani 0.688(3) 1 d PU B 1 H3X H 0.4373 0.2334 0.0020 0.036 Uiso 0.688(3) 1 calc PR B 1 C4X C 0.4508(3) 0.1547(3) 0.0782(2) 0.0300(3) Uani 0.688(3) 1 d PU B 1 C5X C 0.4117(3) 0.1139(3) 0.1200(3) 0.0304(4) Uani 0.688(3) 1 d PU B 1 H5X H 0.4383 0.0802 0.1523 0.036 Uiso 0.688(3) 1 calc PR B 1 C6X C 0.3372(3) 0.1207(4) 0.1159(2) 0.0309(4) Uani 0.688(3) 1 d PU B 1 H6X H 0.3124 0.0951 0.1471 0.037 Uiso 0.688(3) 1 calc PR B 1 O1X O 0.2196(2) 0.1739(3) 0.05795(17) 0.0340(6) Uani 0.688(3) 1 d PU B 1 H1X H 0.2012 0.1386 0.0798 0.051 Uiso 0.688(3) 1 calc PR B 1 O2X O 0.5653(2) 0.1780(2) 0.03125(18) 0.0311(5) Uani 0.688(3) 1 d PU B 1 H2X H 0.5715 0.1436 0.0030 0.047 Uiso 0.688(3) 1 calc PR B 1 O3X O 0.29003(15) 0.25587(18) -0.02144(14) 0.0353(5) Uani 0.688(3) 1 d PU B 1 H3X1 H 0.3173 0.2905 -0.0358 0.053 Uiso 0.688(3) 1 calc PR B 1 C7X C 0.5347(2) 0.1386(2) 0.08179(18) 0.0298(3) Uani 0.688(3) 1 d PU B 1 H7X H 0.5422 0.0785 0.0781 0.036 Uiso 0.688(3) 1 calc PR B 1 C8X C 0.5792(2) 0.1671(3) 0.1438(2) 0.0304(4) Uani 0.688(3) 1 d PU B 1 H8X1 H 0.5780 0.2273 0.1457 0.036 Uiso 0.688(3) 1 calc PR B 1 H8X2 H 0.5566 0.1455 0.1802 0.036 Uiso 0.688(3) 1 calc PR B 1 C9X C 0.7012(2) 0.1302(3) 0.2161(2) 0.0322(4) Uani 0.688(3) 1 d PU B 1 H9X H 0.6924 0.1830 0.2373 0.039 Uiso 0.688(3) 1 calc PR B 1 C10X C 0.7840(2) 0.1266(3) 0.2193(2) 0.0338(6) Uani 0.688(3) 1 d PU B 1 H10A H 0.7982 0.0734 0.2038 0.051 Uiso 0.688(3) 1 calc PR B 1 H10B H 0.8081 0.1343 0.2638 0.051 Uiso 0.688(3) 1 calc PR B 1 H10C H 0.8002 0.1697 0.1923 0.051 Uiso 0.688(3) 1 calc PR B 1 C11X C 0.6696(2) 0.0681(3) 0.25535(18) 0.0313(5) Uani 0.688(3) 1 d PU B 1 H11A H 0.6155 0.0760 0.2517 0.047 Uiso 0.688(3) 1 calc PR B 1 H11B H 0.6926 0.0737 0.3004 0.047 Uiso 0.688(3) 1 calc PR B 1 H11C H 0.6798 0.0135 0.2399 0.047 Uiso 0.688(3) 1 calc PR B 1 N1X N 0.6586(2) 0.1388(2) 0.14960(19) 0.0307(4) Uani 0.688(3) 1 d PU B 1 H1X1 H 0.6588 0.0891 0.1295 0.037 Uiso 0.688(3) 1 calc PR B 1 H1X2 H 0.6840 0.1748 0.1274 0.037 Uiso 0.688(3) 1 calc PR B 1 O8WA O 0.1752(10) 0.3244(10) -0.0065(7) 0.067(3) Uani 0.20 1 d PU C 2 O8WB O 0.2155(11) 0.3252(13) -0.0352(9) 0.067(3) Uani 0.16 1 d PU C 2 C1XA C 0.3011(7) 0.1697(9) 0.0546(5) 0.0308(4) Uani 0.312(3) 1 d PU B 2 C2XA C 0.3424(7) 0.2130(9) 0.0167(6) 0.0307(4) Uani 0.312(3) 1 d PU B 2 H2XA H 0.3171 0.2431 -0.0185 0.037 Uiso 0.312(3) 1 calc PR B 2 C3XA C 0.4174(9) 0.2141(9) 0.0278(8) 0.0304(4) Uani 0.312(3) 1 d PU B 2 H3XA H 0.4432 0.2419 -0.0017 0.036 Uiso 0.312(3) 1 calc PR B 2 C4XA C 0.4585(6) 0.1766(6) 0.0803(5) 0.0301(3) Uani 0.312(3) 1 d PU B 2 C5XA C 0.4220(6) 0.1317(6) 0.1224(6) 0.0303(4) Uani 0.312(3) 1 d PU B 2 H5XA H 0.4481 0.1082 0.1606 0.036 Uiso 0.312(3) 1 calc PR B 2 C6XA C 0.3364(8) 0.1223(9) 0.1030(5) 0.0308(4) Uani 0.312(3) 1 d PU B 2 O1XA O 0.2246(5) 0.1614(6) 0.0435(4) 0.0321(7) Uani 0.312(3) 1 d PU B 2 H1XA H 0.2050 0.2061 0.0307 0.048 Uiso 0.312(3) 1 calc PR B 2 O2XA O 0.5741(5) 0.1997(5) 0.0381(4) 0.0301(6) Uani 0.312(3) 1 d PU B 2 H2X1 H 0.6112 0.1683 0.0428 0.045 Uiso 0.312(3) 1 calc PR B 2 O3XA O 0.2993(3) 0.0792(4) 0.1468(3) 0.0350(7) Uani 0.312(3) 1 d PU B 2 H3X2 H 0.2968 0.1086 0.1791 0.052 Uiso 0.312(3) 1 calc PR B 2 C7XA C 0.5413(4) 0.1988(6) 0.0940(4) 0.0298(4) Uani 0.312(3) 1 d PU B 2 H7XA H 0.5463 0.2543 0.1138 0.036 Uiso 0.312(3) 1 calc PR B 2 C8XA C 0.5809(5) 0.1349(6) 0.1444(4) 0.0302(4) Uani 0.312(3) 1 d PU B 2 H8X3 H 0.5573 0.1352 0.1837 0.036 Uiso 0.312(3) 1 calc PR B 2 H8X4 H 0.5771 0.0793 0.1260 0.036 Uiso 0.312(3) 1 calc PR B 2 C9XA C 0.7040(5) 0.0950(7) 0.2066(4) 0.0321(4) Uani 0.312(3) 1 d PU B 2 H9XA H 0.6795 0.0404 0.2000 0.038 Uiso 0.312(3) 1 calc PR B 2 C10A C 0.7780(5) 0.0895(7) 0.2068(5) 0.0342(7) Uani 0.312(3) 1 d PU B 2 H10D H 0.7948 0.1361 0.1837 0.051 Uiso 0.312(3) 1 calc PR B 2 H10E H 0.7892 0.0388 0.1856 0.051 Uiso 0.312(3) 1 calc PR B 2 H10F H 0.8039 0.0895 0.2511 0.051 Uiso 0.312(3) 1 calc PR B 2 C11A C 0.6882(5) 0.1360(6) 0.2712(4) 0.0343(6) Uani 0.312(3) 1 d PU B 2 H11D H 0.6896 0.0942 0.3046 0.051 Uiso 0.312(3) 1 calc PR B 2 H11E H 0.6388 0.1616 0.2640 0.051 Uiso 0.312(3) 1 calc PR B 2 H11F H 0.7263 0.1774 0.2849 0.051 Uiso 0.312(3) 1 calc PR B 2 N1XA N 0.6616(5) 0.1611(6) 0.1597(4) 0.0310(4) Uani 0.312(3) 1 d PU B 2 H1X3 H 0.6650 0.2115 0.1790 0.037 Uiso 0.312(3) 1 calc PR B 2 H1X4 H 0.6824 0.1642 0.1226 0.037 Uiso 0.312(3) 1 calc PR B 2 Cl1 Cl 0.37965(5) 0.37911(6) -0.08374(4) 0.0536(2) Uani 1 1 d . . . Cl2 Cl 0.12653(4) 0.05132(5) 0.12617(5) 0.0547(2) Uani 1 1 d . . . O1W O 0.60940(12) 0.42244(15) 0.08405(10) 0.0465(5) Uani 1 1 d . . . O2W O 0.57380(16) 0.05936(15) -0.05032(12) 0.0590(7) Uani 1 1 d . . . O3W O 0.04863(14) 0.1399(2) -0.00558(13) 0.0674(8) Uani 1 1 d . . . O4W O 0.33023(18) 0.0877(2) 0.27388(15) 0.0720(8) Uani 1 1 d . . . O5W O 1.1817(2) 0.0771(3) 0.2751(3) 0.0501(11) Uani 0.592(5) 1 d P D -1 O6W O 1.1305(2) 0.1829(2) 0.36675(17) 0.0256(7) Uiso 0.47 1 d P E -1 O6W1 O 1.1134(9) 0.1191(10) 0.3726(8) 0.025(3) Uiso 0.10 1 d P E -1 O7W O 1.1856(3) -0.0264(3) 0.3963(3) 0.0741(17) Uani 0.592(5) 1 d P D -1 O9W O 0.9312(5) -0.1916(6) 0.4161(5) 0.058(2) Uiso 0.30 1 d P F -1 O9W1 O 0.9551(6) -0.1609(7) 0.4033(5) 0.055(2) Uiso 0.27 1 d P F -1 O10W O 0.9042(4) 0.0361(5) 0.3496(3) 0.105(2) Uani 0.592(5) 1 d P D -1 Mg1A Mg 0.9915(2) -0.0143(2) 0.46462(19) 0.0424(9) Uani 0.296(2) 1 d P D -1 O1A O 1.0062(4) -0.1364(6) 0.4829(4) 0.0436(17) Uani 0.296(2) 1 d PU D -1 O2A O 1.0415(4) -0.0206(5) 0.3827(3) 0.0427(17) Uani 0.296(2) 1 d PU D -1 O3A O 0.8887(6) -0.0372(7) 0.4150(9) 0.084(4) Uani 0.296(2) 1 d P D -1 O4A O 0.9782(5) 0.1099(5) 0.4512(4) 0.053(2) Uani 0.296(2) 1 d P D -1 O5A O 1.0979(5) 0.0015(6) 0.5224(5) 0.0499(19) Uani 0.296(2) 1 d PU D -1 O6A O 0.9399(16) 0.0081(16) 0.5441(13) 0.202(16) Uani 0.296(2) 1 d P D -1 Mg1B Mg 1.0500(3) 0.0170(4) 0.4595(3) 0.0352(14) Uani 0.204(2) 1 d PU . 2 O1B O 1.1414(4) -0.0304(5) 0.4292(4) 0.0230(17) Uani 0.204(2) 1 d PU D 2 O2B O 1.0290(4) -0.0844(4) 0.4999(3) 0.0512(16) Uani 0.408(5) 1 d PU . 2 O3B O 0.9825(5) -0.0030(7) 0.3742(5) 0.039(2) Uani 0.204(2) 1 d PU D 2 O4B O 1.0794(8) 0.1306(8) 0.4281(9) 0.079(5) Uani 0.204(2) 1 d PU D 2 O5B O 1.1211(6) 0.0413(8) 0.5466(6) 0.034(2) Uani 0.204(2) 1 d PU D 2 O5W1 O 1.1677(9) 0.0548(10) 0.3026(8) 0.139(6) Uiso 0.408(5) 1 d P D 2 O11W O 1.1660(5) -0.0145(7) 0.6290(5) 0.098(3) Uani 0.408(5) 1 d P D 2 O2 O 0.48806(9) 0.13613(11) 0.26982(8) 0.0272(4) Uani 1 1 d . . . O3 O 0.51905(10) -0.03577(11) 0.17275(8) 0.0271(4) Uani 1 1 d . . . O4 O 0.65126(10) -0.01578(12) 0.06982(9) 0.0336(4) Uani 1 1 d . . . O5 O 0.75206(10) 0.15868(12) 0.05101(8) 0.0299(4) Uani 1 1 d . . . O10 O 1.00304(11) 0.03982(14) 0.25415(10) 0.0409(5) Uani 1 1 d . . . O6 O 0.72609(10) 0.31213(13) 0.14358(9) 0.0352(4) Uani 1 1 d . . . O9 O 0.90020(11) -0.13019(13) 0.27509(11) 0.0394(5) Uani 1 1 d . . . O11 O 0.97577(11) 0.20282(14) 0.34715(9) 0.0398(5) Uani 1 1 d . . . O7 O 0.74191(11) 0.00529(13) 0.47266(10) 0.0399(5) Uani 1 1 d . . . O12 O 0.84881(10) 0.18468(14) 0.45173(9) 0.0360(4) Uani 1 1 d . . . O1 O 0.59625(11) 0.30866(12) 0.25225(9) 0.0363(4) Uani 1 1 d . . . O8 O 0.76718(12) -0.14709(15) 0.38414(11) 0.0467(5) Uani 1 1 d . . . N1 N 0.70903(12) 0.34547(13) 0.31279(10) 0.0266(4) Uani 1 1 d . . . N6 N 0.59810(12) -0.14481(13) 0.20132(10) 0.0265(4) Uani 1 1 d . . . N25 N 0.95769(11) 0.26041(14) 0.24615(10) 0.0274(4) Uani 1 1 d . . . N8 N 0.77379(12) -0.06054(14) 0.08456(11) 0.0314(5) Uani 1 1 d . . . N3 N 0.55376(12) 0.15910(14) 0.37118(10) 0.0273(4) Uani 1 1 d . . . N5 N 0.54568(12) -0.08336(13) 0.27700(10) 0.0255(4) Uani 1 1 d . . . N12 N 0.79604(11) 0.35905(14) 0.23723(10) 0.0285(4) Uani 1 1 d . . . N26 N 0.89532(11) 0.31089(14) 0.31995(10) 0.0270(4) Uani 1 1 d . . . N10 N 0.87428(11) 0.18898(13) 0.09272(10) 0.0251(4) Uani 1 1 d . . . N24 N 0.96867(11) 0.14156(13) 0.17967(10) 0.0269(4) Uani 1 1 d . . . N4 N 0.52179(11) 0.03225(13) 0.34253(9) 0.0251(4) Uani 1 1 d . . . N2 N 0.62368(11) 0.28340(13) 0.36081(10) 0.0264(4) Uani 1 1 d . . . N15 N 0.80951(11) 0.30331(15) 0.39746(10) 0.0298(5) Uani 1 1 d . . . N7 N 0.69072(12) -0.12951(13) 0.13046(11) 0.0293(5) Uani 1 1 d . . . N23 N 0.94188(11) 0.01307(14) 0.15172(11) 0.0299(5) Uani 1 1 d . . . N17 N 0.65426(11) 0.10657(14) 0.44993(10) 0.0284(4) Uani 1 1 d . . . N16 N 0.72604(11) 0.22695(13) 0.43601(10) 0.0265(4) Uani 1 1 d . . . N18 N 0.62101(13) -0.01942(14) 0.42387(11) 0.0341(5) Uani 1 1 d . . . N9 N 0.84492(11) 0.06123(14) 0.06718(11) 0.0291(5) Uani 1 1 d . . . N21 N 0.79073(13) -0.17491(15) 0.21317(12) 0.0357(5) Uani 1 1 d . . . C1 C 0.63856(14) 0.31185(15) 0.30323(12) 0.0268(5) Uani 1 1 d . . . C25 C 0.79978(14) 0.23292(17) 0.43029(11) 0.0278(5) Uani 1 1 d . . . C4 C 0.49005(13) -0.03520(16) 0.30275(12) 0.0266(5) Uani 1 1 d . . . H4A H 0.4623 -0.0710 0.3286 0.032 Uiso 1 1 calc R . . H4B H 0.4539 -0.0134 0.2667 0.032 Uiso 1 1 calc R . . C9 C 0.81731(13) 0.13839(16) 0.06879(11) 0.0258(5) Uani 1 1 d . . . C5 C 0.55108(13) -0.08289(15) 0.21309(12) 0.0245(5) Uani 1 1 d . . . C2 C 0.55307(13) 0.24640(16) 0.36853(12) 0.0280(5) Uani 1 1 d . . . H2A H 0.5378 0.2675 0.4085 0.034 Uiso 1 1 calc R . . H2B H 0.5148 0.2637 0.3323 0.034 Uiso 1 1 calc R . . C7 C 0.70023(14) -0.06381(16) 0.09241(13) 0.0290(5) Uani 1 1 d . . . C3 C 0.51812(13) 0.11159(15) 0.32232(11) 0.0236(5) Uani 1 1 d . . . C21 C 0.92403(13) 0.05688(16) 0.09177(12) 0.0274(5) Uani 1 1 d . . . H21 H 0.9534 0.0363 0.0587 0.033 Uiso 1 1 calc R . . N20 N 0.70015(13) -0.18323(14) 0.28588(11) 0.0327(5) Uani 1 1 d . . . N19 N 0.63840(14) -0.14003(15) 0.36223(11) 0.0346(5) Uani 1 1 d . . . C27 C 0.67891(15) 0.02858(17) 0.45073(12) 0.0305(5) Uani 1 1 d . . . C12 C 0.73580(14) 0.39583(16) 0.26482(12) 0.0278(5) Uani 1 1 d . . . H12A H 0.6938 0.4073 0.2300 0.033 Uiso 1 1 calc R . . H12B H 0.7532 0.4485 0.2846 0.033 Uiso 1 1 calc R . . N22 N 0.87390(12) -0.11071(14) 0.16505(12) 0.0339(5) Uani 1 1 d . . . C35 C 0.94544(13) 0.25259(17) 0.30776(12) 0.0282(5) Uani 1 1 d . . . N11 N 0.85444(12) 0.30072(14) 0.16404(10) 0.0296(5) Uani 1 1 d . . . C14 C 0.68420(13) 0.29868(15) 0.41289(11) 0.0249(5) Uani 1 1 d . . . H14 H 0.6669 0.3297 0.4487 0.030 Uiso 1 1 calc R . . C22 C 0.94409(13) 0.14657(15) 0.11080(12) 0.0250(5) Uani 1 1 d . . . H22 H 0.9841 0.1684 0.0878 0.030 Uiso 1 1 calc R . . C26 C 0.69978(14) 0.17131(17) 0.48112(12) 0.0287(5) Uani 1 1 d . . . H26A H 0.7434 0.1473 0.5090 0.034 Uiso 1 1 calc R . . H26B H 0.6704 0.2022 0.5089 0.034 Uiso 1 1 calc R . . C15 C 0.57457(13) 0.11293(16) 0.42977(11) 0.0267(5) Uani 1 1 d . . . H15 H 0.5484 0.1331 0.4651 0.032 Uiso 1 1 calc R . . C18 C 0.62248(14) -0.19383(15) 0.25779(13) 0.0293(5) Uani 1 1 d . . . H18 H 0.6096 -0.2526 0.2502 0.035 Uiso 1 1 calc R . . C20 C 0.81576(15) -0.13045(16) 0.11244(14) 0.0319(6) Uani 1 1 d . . . H20 H 0.8349 -0.1644 0.0791 0.038 Uiso 1 1 calc R . . C36 C 0.88176(14) 0.33015(19) 0.38438(12) 0.0324(6) Uani 1 1 d . . . H36A H 0.9212 0.3044 0.4157 0.039 Uiso 1 1 calc R . . H36B H 0.8856 0.3899 0.3907 0.039 Uiso 1 1 calc R . . C32 C 0.94418(15) -0.07431(17) 0.15695(15) 0.0358(6) Uani 1 1 d . . . H32A H 0.9822 -0.0896 0.1940 0.043 Uiso 1 1 calc R . . H32B H 0.9602 -0.0971 0.1178 0.043 Uiso 1 1 calc R . . C11 C 0.78639(15) 0.32338(16) 0.17801(12) 0.0287(5) Uani 1 1 d . . . C23 C 0.91508(14) 0.32644(16) 0.21284(12) 0.0265(5) Uani 1 1 d . . . H23 H 0.9481 0.3671 0.1958 0.032 Uiso 1 1 calc R . . C13 C 0.74088(13) 0.34850(16) 0.38037(11) 0.0263(5) Uani 1 1 d . . . H13 H 0.7457 0.4058 0.3967 0.032 Uiso 1 1 calc R . . C10 C 0.86526(15) 0.27603(16) 0.10022(12) 0.0290(5) Uani 1 1 d . . . H101 H 0.9101 0.3040 0.0893 0.035 Uiso 1 1 calc R . . H102 H 0.8218 0.2945 0.0692 0.035 Uiso 1 1 calc R . . C19 C 0.75829(15) -0.17768(16) 0.14633(14) 0.0315(5) Uani 1 1 d . . . H19 H 0.7511 -0.2349 0.1303 0.038 Uiso 1 1 calc R . . C8 C 0.80007(14) -0.00626(17) 0.03840(13) 0.0312(5) Uani 1 1 d . . . H8A H 0.8300 -0.0382 0.0118 0.037 Uiso 1 1 calc R . . H8B H 0.7563 0.0158 0.0096 0.037 Uiso 1 1 calc R . . C33 C 0.97393(14) 0.06249(17) 0.20076(13) 0.0308(5) Uani 1 1 d . . . C31 C 0.85883(15) -0.13734(16) 0.22335(14) 0.0335(6) Uani 1 1 d . . . C29 C 0.70752(16) -0.15510(17) 0.34798(14) 0.0355(6) Uani 1 1 d . . . C16 C 0.55155(14) 0.02490(17) 0.40995(11) 0.0285(5) Uani 1 1 d . . . H16 H 0.5133 0.0034 0.4351 0.034 Uiso 1 1 calc R . . C17 C 0.57981(14) -0.15585(15) 0.30881(12) 0.0285(5) Uani 1 1 d . . . H17 H 0.5414 -0.1941 0.3210 0.034 Uiso 1 1 calc R . . C24 C 0.87402(13) 0.36431(16) 0.26533(12) 0.0264(5) Uani 1 1 d . . . H24 H 0.8899 0.4219 0.2752 0.032 Uiso 1 1 calc R . . C34 C 1.00692(13) 0.20791(16) 0.21643(12) 0.0280(5) Uani 1 1 d . . . H34A H 1.0332 0.2412 0.1877 0.034 Uiso 1 1 calc R . . H34B H 1.0451 0.1849 0.2503 0.034 Uiso 1 1 calc R . . C6 C 0.61777(14) -0.15965(16) 0.13839(12) 0.0283(5) Uani 1 1 d . . . H6A H 0.6161 -0.2191 0.1302 0.034 Uiso 1 1 calc R . . H6B H 0.5799 -0.1337 0.1058 0.034 Uiso 1 1 calc R . . C30 C 0.76174(16) -0.22232(18) 0.26191(15) 0.0374(6) Uani 1 1 d . . . H30A H 0.7450 -0.2760 0.2437 0.045 Uiso 1 1 calc R . . H30B H 0.8025 -0.2320 0.2982 0.045 Uiso 1 1 calc R . . C28 C 0.62646(18) -0.10707(17) 0.42289(13) 0.0364(6) Uani 1 1 d . . . H28A H 0.6681 -0.1243 0.4562 0.044 Uiso 1 1 calc R . . H28B H 0.5799 -0.1305 0.4342 0.044 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 O8W 0.061(3) 0.100(4) 0.080(3) 0.009(3) -0.006(3) 0.030(3) C1X 0.0251(6) 0.0379(7) 0.0289(8) -0.0037(7) 0.0038(6) -0.0018(6) C2X 0.0258(7) 0.0375(7) 0.0283(7) -0.0032(6) 0.0033(6) -0.0010(6) C3X 0.0259(6) 0.0377(8) 0.0275(7) -0.0024(7) 0.0043(6) -0.0013(6) C4X 0.0254(6) 0.0378(8) 0.0273(6) -0.0019(7) 0.0051(5) -0.0010(6) C5X 0.0255(6) 0.0379(8) 0.0281(7) -0.0019(7) 0.0051(6) -0.0012(6) C6X 0.0258(6) 0.0383(8) 0.0288(8) -0.0025(7) 0.0046(6) -0.0017(6) O1X 0.0244(8) 0.0433(12) 0.0336(13) -0.0056(10) 0.0022(9) -0.0021(9) O2X 0.0283(10) 0.0390(13) 0.0270(9) 0.0005(10) 0.0077(8) -0.0029(10) O3X 0.0300(9) 0.0401(11) 0.0345(10) 0.0000(8) 0.0011(8) 0.0004(8) C7X 0.0256(6) 0.0377(8) 0.0266(6) -0.0003(6) 0.0061(5) -0.0013(6) C8X 0.0251(6) 0.0394(9) 0.0272(7) 0.0006(7) 0.0059(6) -0.0010(7) C9X 0.0264(7) 0.0411(10) 0.0293(8) 0.0038(8) 0.0054(6) -0.0009(8) C10X 0.0260(8) 0.0424(14) 0.0332(12) 0.0076(11) 0.0056(8) -0.0024(11) C11X 0.0249(10) 0.0409(12) 0.0294(10) 0.0053(9) 0.0083(9) 0.0015(10) N1X 0.0252(6) 0.0398(9) 0.0279(7) 0.0021(7) 0.0063(6) -0.0006(7) O8WA 0.058(8) 0.082(7) 0.052(7) -0.010(6) -0.021(5) 0.004(7) O8WB 0.058(8) 0.081(7) 0.052(7) -0.010(6) -0.021(5) 0.004(7) C1XA 0.0252(7) 0.0381(8) 0.0289(8) -0.0035(7) 0.0038(6) -0.0016(6) C2XA 0.0258(7) 0.0377(8) 0.0284(7) -0.0029(7) 0.0036(6) -0.0013(6) C3XA 0.0258(7) 0.0377(8) 0.0276(7) -0.0024(7) 0.0042(6) -0.0012(6) C4XA 0.0255(6) 0.0378(8) 0.0272(6) -0.0018(6) 0.0052(5) -0.0011(6) C5XA 0.0253(6) 0.0379(8) 0.0280(7) -0.0021(7) 0.0050(6) -0.0014(6) C6XA 0.0256(6) 0.0383(8) 0.0288(8) -0.0026(7) 0.0048(6) -0.0018(6) O1XA 0.0246(9) 0.0415(13) 0.0303(14) -0.0075(12) 0.0040(11) -0.0017(11) O2XA 0.0273(11) 0.0379(15) 0.0259(11) -0.0014(11) 0.0065(9) -0.0024(13) O3XA 0.0281(12) 0.0431(14) 0.0343(13) 0.0012(11) 0.0064(12) -0.0041(12) C7XA 0.0254(6) 0.0380(9) 0.0266(7) -0.0004(7) 0.0059(6) -0.0010(7) C8XA 0.0253(7) 0.0387(9) 0.0274(7) 0.0009(7) 0.0061(6) -0.0010(7) C9XA 0.0264(7) 0.0408(10) 0.0294(8) 0.0031(8) 0.0055(7) -0.0002(8) C10A 0.0266(10) 0.0446(15) 0.0316(13) 0.0047(13) 0.0054(10) 0.0006(12) C11A 0.0296(13) 0.0437(14) 0.0300(10) 0.0034(11) 0.0058(11) 0.0010(13) N1XA 0.0254(7) 0.0399(9) 0.0284(8) 0.0023(8) 0.0059(6) -0.0008(8) Cl1 0.0564(5) 0.0616(5) 0.0478(4) 0.0130(4) 0.0235(4) -0.0059(4) Cl2 0.0379(4) 0.0495(4) 0.0791(6) 0.0194(4) 0.0166(4) 0.0055(3) O1W 0.0407(11) 0.0614(14) 0.0371(11) -0.0065(10) 0.0053(9) 0.0174(10) O2W 0.0779(18) 0.0411(13) 0.0496(14) 0.0070(10) -0.0164(12) -0.0132(12) O3W 0.0402(13) 0.117(3) 0.0486(14) -0.0042(15) 0.0195(11) 0.0119(14) O4W 0.0677(18) 0.081(2) 0.0641(17) -0.0003(15) 0.0005(14) -0.0017(15) O5W 0.0311(18) 0.040(2) 0.082(3) -0.018(2) 0.0189(19) -0.0061(15) O7W 0.076(4) 0.051(3) 0.083(4) -0.012(2) -0.024(3) 0.014(2) O10W 0.115(5) 0.133(6) 0.066(4) 0.018(4) 0.012(3) -0.037(5) Mg1A 0.0376(19) 0.0367(18) 0.057(2) 0.0126(15) 0.0205(16) 0.0102(14) O1A 0.036(4) 0.051(5) 0.045(4) 0.006(4) 0.008(3) 0.005(3) O2A 0.048(5) 0.047(4) 0.034(4) 0.002(3) 0.008(3) 0.004(3) O3A 0.039(5) 0.065(7) 0.137(12) 0.040(8) -0.023(7) -0.012(4) O4A 0.053(5) 0.056(5) 0.054(5) 0.003(4) 0.022(4) 0.009(4) O5A 0.045(4) 0.055(5) 0.052(5) -0.003(4) 0.013(4) 0.000(4) O6A 0.29(3) 0.19(2) 0.18(2) 0.109(18) 0.20(2) 0.14(2) Mg1B 0.0115(19) 0.058(3) 0.034(3) 0.019(2) -0.0040(18) 0.0153(19) O1B 0.017(3) 0.029(4) 0.018(4) -0.008(3) -0.012(3) 0.010(3) O2B 0.051(3) 0.055(4) 0.047(3) 0.008(3) 0.006(3) 0.021(3) O3B 0.023(4) 0.065(6) 0.029(4) 0.008(4) 0.004(3) 0.007(4) O4B 0.059(8) 0.051(6) 0.110(11) 0.044(7) -0.037(8) 0.000(5) O5B 0.032(5) 0.040(6) 0.031(5) 0.008(4) 0.007(4) 0.008(4) O11W 0.077(6) 0.117(8) 0.100(7) 0.037(6) 0.013(5) 0.002(5) O2 0.0244(8) 0.0361(9) 0.0213(8) -0.0007(7) 0.0038(6) 0.0013(7) O3 0.0281(8) 0.0306(9) 0.0228(8) -0.0004(7) 0.0042(7) 0.0020(7) O4 0.0302(9) 0.0340(10) 0.0388(10) 0.0011(8) 0.0123(8) 0.0082(8) O5 0.0216(8) 0.0405(10) 0.0272(9) 0.0039(7) 0.0020(7) 0.0062(7) O10 0.0328(10) 0.0485(12) 0.0387(11) 0.0137(9) -0.0024(8) 0.0023(9) O6 0.0263(9) 0.0453(11) 0.0313(9) -0.0077(8) -0.0044(7) 0.0107(8) O9 0.0283(9) 0.0398(11) 0.0485(12) 0.0078(9) 0.0007(8) 0.0043(8) O11 0.0291(9) 0.0586(13) 0.0320(10) 0.0092(9) 0.0059(8) 0.0126(9) O7 0.0335(10) 0.0406(11) 0.0427(11) 0.0001(9) -0.0038(8) 0.0050(8) O12 0.0258(9) 0.0541(12) 0.0285(9) 0.0057(8) 0.0056(7) 0.0110(8) O1 0.0385(10) 0.0352(10) 0.0309(10) 0.0067(8) -0.0081(8) -0.0084(8) O8 0.0386(11) 0.0538(13) 0.0430(12) 0.0041(10) -0.0081(9) -0.0016(10) N1 0.0246(10) 0.0282(10) 0.0259(10) 0.0003(8) 0.0010(8) -0.0006(8) N6 0.0275(10) 0.0251(10) 0.0270(10) -0.0026(8) 0.0047(8) 0.0002(8) N25 0.0203(9) 0.0359(11) 0.0262(10) -0.0004(8) 0.0040(8) 0.0043(8) N8 0.0261(11) 0.0307(11) 0.0388(12) 0.0028(9) 0.0094(9) 0.0031(8) N3 0.0255(10) 0.0340(11) 0.0217(10) 0.0002(8) 0.0019(8) -0.0051(8) N5 0.0271(10) 0.0263(10) 0.0234(10) 0.0010(8) 0.0049(8) -0.0025(8) N12 0.0224(10) 0.0355(11) 0.0270(10) -0.0065(8) 0.0022(8) 0.0046(8) N26 0.0217(9) 0.0358(11) 0.0236(10) -0.0005(8) 0.0043(8) -0.0009(8) N10 0.0222(10) 0.0294(11) 0.0240(10) 0.0017(8) 0.0046(8) 0.0044(8) N24 0.0225(9) 0.0319(11) 0.0257(10) 0.0012(8) 0.0021(8) 0.0019(8) N4 0.0246(10) 0.0325(11) 0.0187(9) -0.0022(8) 0.0049(7) -0.0010(8) N2 0.0207(9) 0.0305(11) 0.0272(10) -0.0026(8) 0.0006(8) -0.0029(8) N15 0.0202(10) 0.0432(12) 0.0265(10) 0.0012(9) 0.0055(8) 0.0016(9) N7 0.0258(10) 0.0254(10) 0.0379(12) -0.0037(8) 0.0089(9) 0.0002(8) N23 0.0217(10) 0.0311(11) 0.0365(12) 0.0052(9) 0.0030(8) 0.0015(8) N17 0.0221(10) 0.0356(11) 0.0269(10) -0.0057(8) 0.0018(8) -0.0003(8) N16 0.0223(10) 0.0329(11) 0.0245(10) -0.0008(8) 0.0043(8) 0.0025(8) N18 0.0357(12) 0.0310(12) 0.0326(12) 0.0059(9) -0.0034(9) -0.0022(9) N9 0.0191(10) 0.0329(11) 0.0351(11) -0.0023(9) 0.0031(8) 0.0026(8) N21 0.0298(11) 0.0356(12) 0.0421(13) 0.0032(10) 0.0066(10) -0.0021(9) C1 0.0292(12) 0.0210(11) 0.0294(12) -0.0010(9) 0.0017(10) 0.0019(9) C25 0.0237(11) 0.0415(14) 0.0189(11) -0.0054(9) 0.0052(9) 0.0037(10) C4 0.0231(11) 0.0337(13) 0.0235(11) -0.0020(9) 0.0048(9) -0.0056(9) C9 0.0250(12) 0.0336(13) 0.0205(11) 0.0035(9) 0.0087(9) 0.0039(9) C5 0.0228(11) 0.0241(11) 0.0270(11) -0.0038(9) 0.0051(9) -0.0059(9) C2 0.0199(11) 0.0322(13) 0.0318(12) -0.0043(10) 0.0039(9) 0.0020(9) C7 0.0284(12) 0.0277(12) 0.0330(13) -0.0070(10) 0.0113(10) -0.0008(10) C3 0.0198(10) 0.0315(12) 0.0209(11) -0.0019(9) 0.0079(8) -0.0015(9) C21 0.0195(11) 0.0314(13) 0.0327(13) -0.0012(10) 0.0088(9) 0.0024(9) N20 0.0281(11) 0.0334(11) 0.0361(12) 0.0056(9) 0.0031(9) -0.0018(9) N19 0.0375(12) 0.0352(12) 0.0294(11) 0.0051(9) -0.0001(9) -0.0013(9) C27 0.0322(13) 0.0341(13) 0.0250(12) 0.0023(10) 0.0034(10) 0.0004(10) C12 0.0265(12) 0.0292(12) 0.0286(12) -0.0002(9) 0.0069(9) 0.0044(10) N22 0.0266(11) 0.0296(11) 0.0456(13) 0.0045(9) 0.0056(9) -0.0005(9) C35 0.0178(10) 0.0396(14) 0.0268(12) 0.0008(10) 0.0027(9) -0.0001(9) N11 0.0251(10) 0.0392(12) 0.0234(10) -0.0038(9) 0.0006(8) 0.0085(9) C14 0.0199(11) 0.0306(12) 0.0242(11) -0.0063(9) 0.0033(9) 0.0011(9) C22 0.0196(11) 0.0314(12) 0.0250(11) 0.0013(9) 0.0070(9) 0.0025(9) C26 0.0260(12) 0.0379(14) 0.0219(11) -0.0031(10) 0.0024(9) -0.0033(10) C15 0.0238(11) 0.0372(13) 0.0199(11) -0.0008(9) 0.0063(9) -0.0022(10) C18 0.0303(13) 0.0230(12) 0.0343(13) 0.0025(10) 0.0043(10) -0.0038(9) C20 0.0272(12) 0.0271(12) 0.0432(15) -0.0051(11) 0.0106(11) 0.0013(10) C36 0.0214(12) 0.0505(16) 0.0252(12) -0.0078(11) 0.0036(9) -0.0061(11) C32 0.0229(12) 0.0317(14) 0.0536(17) 0.0066(12) 0.0088(11) 0.0067(10) C11 0.0282(12) 0.0304(12) 0.0266(12) -0.0024(9) 0.0016(10) 0.0058(10) C23 0.0232(11) 0.0298(12) 0.0266(12) -0.0005(9) 0.0037(9) -0.0003(9) C13 0.0240(11) 0.0307(12) 0.0239(11) -0.0059(9) 0.0032(9) 0.0001(9) C10 0.0338(13) 0.0307(13) 0.0224(12) 0.0021(9) 0.0041(9) 0.0064(10) C19 0.0274(12) 0.0266(12) 0.0419(15) -0.0035(10) 0.0095(11) 0.0008(10) C8 0.0269(12) 0.0353(14) 0.0316(13) -0.0015(10) 0.0050(10) -0.0028(10) C33 0.0209(11) 0.0384(14) 0.0335(13) 0.0059(11) 0.0054(10) 0.0022(10) C31 0.0269(12) 0.0268(13) 0.0472(16) 0.0016(11) 0.0074(11) 0.0046(10) C29 0.0372(14) 0.0319(13) 0.0357(14) 0.0079(11) -0.0001(11) -0.0031(11) C16 0.0277(12) 0.0388(14) 0.0193(11) 0.0021(9) 0.0049(9) -0.0069(10) C17 0.0304(12) 0.0257(12) 0.0289(12) 0.0031(9) 0.0035(10) -0.0047(10) C24 0.0232(11) 0.0295(12) 0.0262(12) -0.0028(9) 0.0032(9) -0.0012(9) C34 0.0170(10) 0.0377(14) 0.0291(12) -0.0032(10) 0.0029(9) 0.0023(9) C6 0.0267(12) 0.0277(12) 0.0313(13) -0.0078(10) 0.0065(10) -0.0039(9) C30 0.0308(13) 0.0336(14) 0.0483(16) 0.0113(12) 0.0078(12) 0.0032(11) C28 0.0483(16) 0.0317(14) 0.0273(13) 0.0067(10) 0.0003(11) -0.0020(12) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 C1X O1X 1.380(7) . ? C1X C2X 1.389(6) . ? C1X C6X 1.390(7) . ? C2X O3X 1.375(7) . ? C2X C3X 1.412(8) . ? C3X C4X 1.397(9) . ? C4X C5X 1.385(6) . ? C4X C7X 1.534(6) . ? C5X C6X 1.344(8) . ? O2X C7X 1.430(5) . ? C7X C8X 1.501(5) . ? C8X N1X 1.498(6) . ? C9X C11X 1.483(5) . ? C9X C10X 1.493(6) . ? C9X N1X 1.498(6) . ? O8WA O8WB 1.02(2) . ? C1XA C6XA 1.361(16) . ? C1XA C2XA 1.375(14) . ? C1XA O1XA 1.377(15) . ? C2XA C3XA 1.342(19) . ? C3XA C4XA 1.379(19) . ? C4XA C5XA 1.397(14) . ? C4XA C7XA 1.527(12) . ? C5XA C6XA 1.549(17) . ? C6XA O3XA 1.413(13) . ? O2XA C7XA 1.399(12) . ? C7XA C8XA 1.584(13) . ? C8XA N1XA 1.511(13) . ? C9XA C10A 1.342(13) . ? C9XA C11A 1.584(13) . ? C9XA N1XA 1.585(14) . ? O6W O6W1 1.103(17) . ? O9W O9W1 0.743(11) . ? Mg1A O3A 2.025(11) . ? Mg1A O1A 2.050(10) . ? Mg1A O4A 2.066(10) . ? Mg1A O2A 2.073(8) . ? Mg1A O6A 2.07(2) . ? Mg1A O5A 2.130(11) . ? Mg1B O2B 1.933(10) . ? Mg1B O1B 2.020(10) . ? Mg1B O3B 2.038(11) . ? Mg1B O4B 2.075(15) . ? Mg1B O2B 2.094(9) 3_756 ? Mg1B O5B 2.112(15) . ? Mg1B Mg1B 2.734(13) 3_756 ? O2B Mg1B 2.094(9) 3_756 ? O2 C3 1.224(3) . ? O3 C5 1.227(3) . ? O4 C7 1.227(3) . ? O5 C9 1.230(3) . ? O10 C33 1.225(3) . ? O6 C11 1.229(3) . ? O9 C31 1.230(4) . ? O11 C35 1.232(3) . ? O7 C27 1.225(3) . ? O12 C25 1.223(3) . ? O1 C1 1.221(3) . ? O8 C29 1.230(4) . ? N1 C1 1.377(3) . ? N1 C12 1.447(3) . ? N1 C13 1.453(3) . ? N6 C5 1.373(3) . ? N6 C6 1.447(3) . ? N6 C18 1.448(3) . ? N25 C35 1.357(3) . ? N25 C23 1.448(3) . ? N25 C34 1.451(3) . ? N8 C7 1.370(3) . ? N8 C20 1.450(3) . ? N8 C8 1.453(3) . ? N3 C3 1.371(3) . ? N3 C2 1.433(3) . ? N3 C15 1.449(3) . ? N5 C5 1.366(3) . ? N5 C4 1.451(3) . ? N5 C17 1.455(3) . ? N12 C11 1.366(3) . ? N12 C12 1.446(3) . ? N12 C24 1.448(3) . ? N26 C35 1.371(3) . ? N26 C24 1.451(3) . ? N26 C36 1.452(3) . ? N10 C9 1.359(3) . ? N10 C22 1.443(3) . ? N10 C10 1.449(3) . ? N24 C33 1.370(3) . ? N24 C34 1.449(3) . ? N24 C22 1.454(3) . ? N4 C3 1.368(3) . ? N4 C16 1.445(3) . ? N4 C4 1.453(3) . ? N2 C1 1.366(3) . ? N2 C2 1.448(3) . ? N2 C14 1.449(3) . ? N15 C25 1.372(4) . ? N15 C13 1.445(3) . ? N15 C36 1.448(3) . ? N7 C7 1.371(3) . ? N7 C6 1.445(3) . ? N7 C19 1.452(3) . ? N23 C33 1.371(4) . ? N23 C32 1.438(4) . ? N23 C21 1.446(3) . ? N17 C27 1.355(4) . ? N17 C26 1.440(3) . ? N17 C15 1.445(3) . ? N16 C25 1.364(3) . ? N16 C14 1.443(3) . ? N16 C26 1.451(3) . ? N18 C27 1.363(4) . ? N18 C28 1.442(4) . ? N18 C16 1.444(4) . ? N9 C9 1.364(3) . ? N9 C21 1.449(3) . ? N9 C8 1.450(3) . ? N21 C31 1.366(4) . ? N21 C19 1.441(4) . ? N21 C30 1.451(4) . ? C21 C22 1.554(3) . ? N20 C29 1.375(4) . ? N20 C30 1.445(4) . ? N20 C18 1.451(3) . ? N19 C29 1.356(4) . ? N19 C28 1.436(4) . ? N19 C17 1.447(3) . ? N22 C31 1.372(4) . ? N22 C32 1.441(3) . ? N22 C20 1.443(4) . ? N11 C11 1.363(3) . ? N11 C23 1.447(3) . ? N11 C10 1.448(3) . ? C14 C13 1.553(3) . ? C15 C16 1.543(4) . ? C18 C17 1.550(4) . ? C20 C19 1.558(4) . ? C23 C24 1.556(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 O1X C1X C2X 115.6(5) . . ? O1X C1X C6X 124.2(4) . . ? C2X C1X C6X 120.0(5) . . ? O3X C2X C1X 117.8(5) . . ? O3X C2X C3X 123.3(4) . . ? C1X C2X C3X 119.0(6) . . ? C4X C3X C2X 119.8(5) . . ? C5X C4X C3X 118.8(5) . . ? C5X C4X C7X 119.1(4) . . ? C3X C4X C7X 121.8(4) . . ? C6X C5X C4X 121.8(5) . . ? C5X C6X C1X 120.3(5) . . ? O2X C7X C8X 106.9(3) . . ? O2X C7X C4X 112.4(4) . . ? C8X C7X C4X 112.6(3) . . ? N1X C8X C7X 110.8(3) . . ? C11X C9X C10X 114.8(4) . . ? C11X C9X N1X 113.5(4) . . ? C10X C9X N1X 114.6(4) . . ? C9X N1X C8X 117.0(4) . . ? C6XA C1XA C2XA 119.7(12) . . ? C6XA C1XA O1XA 114.6(10) . . ? C2XA C1XA O1XA 125.2(11) . . ? C3XA C2XA C1XA 122.3(13) . . ? C2XA C3XA C4XA 122.6(11) . . ? C3XA C4XA C5XA 119.7(10) . . ? C3XA C4XA C7XA 116.0(9) . . ? C5XA C4XA C7XA 123.6(9) . . ? C4XA C5XA C6XA 116.0(10) . . ? C1XA C6XA O3XA 124.1(11) . . ? C1XA C6XA C5XA 118.4(11) . . ? O3XA C6XA C5XA 115.8(9) . . ? O2XA C7XA C4XA 112.1(8) . . ? O2XA C7XA C8XA 111.4(7) . . ? C4XA C7XA C8XA 107.4(7) . . ? N1XA C8XA C7XA 106.2(8) . . ? C10A C9XA C11A 109.9(8) . . ? C10A C9XA N1XA 115.8(8) . . ? C11A C9XA N1XA 96.4(8) . . ? C8XA N1XA C9XA 107.4(8) . . ? O3A Mg1A O1A 89.9(4) . . ? O3A Mg1A O4A 92.0(4) . . ? O1A Mg1A O4A 177.0(4) . . ? O3A Mg1A O2A 92.6(6) . . ? O1A Mg1A O2A 92.7(3) . . ? O4A Mg1A O2A 89.5(3) . . ? O3A Mg1A O6A 87.5(11) . . ? O1A Mg1A O6A 94.7(7) . . ? O4A Mg1A O6A 83.0(7) . . ? O2A Mg1A O6A 172.6(7) . . ? O3A Mg1A O5A 175.0(5) . . ? O1A Mg1A O5A 86.1(4) . . ? O4A Mg1A O5A 92.0(4) . . ? O2A Mg1A O5A 90.5(3) . . ? O6A Mg1A O5A 89.9(10) . . ? O2B Mg1B O1B 92.0(4) . . ? O2B Mg1B O3B 96.8(5) . . ? O1B Mg1B O3B 94.0(4) . . ? O2B Mg1B O4B 172.3(6) . . ? O1B Mg1B O4B 88.9(6) . . ? O3B Mg1B O4B 90.7(6) . . ? O2B Mg1B O2B 94.6(4) . 3_756 ? O1B Mg1B O2B 168.0(5) . 3_756 ? O3B Mg1B O2B 95.2(4) . 3_756 ? O4B Mg1B O2B 83.2(6) . 3_756 ? O2B Mg1B O5B 85.1(5) . . ? O1B Mg1B O5B 85.8(4) . . ? O3B Mg1B O5B 178.1(6) . . ? O4B Mg1B O5B 87.4(6) . . ? O2B Mg1B O5B 84.7(4) 3_756 . ? O2B Mg1B Mg1B 49.8(3) . 3_756 ? O1B Mg1B Mg1B 140.7(5) . 3_756 ? O3B Mg1B Mg1B 98.8(4) . 3_756 ? O4B Mg1B Mg1B 127.6(7) . 3_756 ? O2B Mg1B Mg1B 44.8(3) 3_756 3_756 ? O5B Mg1B Mg1B 82.5(4) . 3_756 ? Mg1B O2B Mg1B 85.4(4) . 3_756 ? C1 N1 C12 122.0(2) . . ? C1 N1 C13 112.1(2) . . ? C12 N1 C13 122.7(2) . . ? C5 N6 C6 122.6(2) . . ? C5 N6 C18 112.4(2) . . ? C6 N6 C18 125.0(2) . . ? C35 N25 C23 112.4(2) . . ? C35 N25 C34 124.1(2) . . ? C23 N25 C34 123.5(2) . . ? C7 N8 C20 112.3(2) . . ? C7 N8 C8 122.1(2) . . ? C20 N8 C8 123.4(2) . . ? C3 N3 C2 122.6(2) . . ? C3 N3 C15 111.9(2) . . ? C2 N3 C15 123.7(2) . . ? C5 N5 C4 121.7(2) . . ? C5 N5 C17 111.7(2) . . ? C4 N5 C17 122.9(2) . . ? C11 N12 C12 123.3(2) . . ? C11 N12 C24 112.2(2) . . ? C12 N12 C24 124.1(2) . . ? C35 N26 C24 112.0(2) . . ? C35 N26 C36 122.7(2) . . ? C24 N26 C36 123.2(2) . . ? C9 N10 C22 112.8(2) . . ? C9 N10 C10 123.4(2) . . ? C22 N10 C10 123.8(2) . . ? C33 N24 C34 122.3(2) . . ? C33 N24 C22 111.9(2) . . ? C34 N24 C22 122.6(2) . . ? C3 N4 C16 112.2(2) . . ? C3 N4 C4 123.3(2) . . ? C16 N4 C4 124.0(2) . . ? C1 N2 C2 122.9(2) . . ? C1 N2 C14 112.6(2) . . ? C2 N2 C14 124.5(2) . . ? C25 N15 C13 112.6(2) . . ? C25 N15 C36 122.9(2) . . ? C13 N15 C36 124.4(2) . . ? C7 N7 C6 122.5(2) . . ? C7 N7 C19 112.6(2) . . ? C6 N7 C19 122.7(2) . . ? C33 N23 C32 121.9(2) . . ? C33 N23 C21 112.1(2) . . ? C32 N23 C21 124.2(2) . . ? C27 N17 C26 121.8(2) . . ? C27 N17 C15 112.6(2) . . ? C26 N17 C15 123.8(2) . . ? C25 N16 C14 112.5(2) . . ? C25 N16 C26 121.9(2) . . ? C14 N16 C26 121.7(2) . . ? C27 N18 C28 122.2(2) . . ? C27 N18 C16 112.6(2) . . ? C28 N18 C16 124.0(2) . . ? C9 N9 C21 112.5(2) . . ? C9 N9 C8 122.4(2) . . ? C21 N9 C8 124.9(2) . . ? C31 N21 C19 112.9(2) . . ? C31 N21 C30 123.2(3) . . ? C19 N21 C30 122.6(2) . . ? O1 C1 N2 125.7(2) . . ? O1 C1 N1 126.0(2) . . ? N2 C1 N1 108.3(2) . . ? O12 C25 N16 125.9(3) . . ? O12 C25 N15 126.0(2) . . ? N16 C25 N15 108.0(2) . . ? N5 C4 N4 113.27(19) . . ? O5 C9 N10 125.9(2) . . ? O5 C9 N9 125.6(2) . . ? N10 C9 N9 108.4(2) . . ? O3 C5 N5 126.1(2) . . ? O3 C5 N6 125.5(2) . . ? N5 C5 N6 108.4(2) . . ? N3 C2 N2 114.9(2) . . ? O4 C7 N8 126.0(2) . . ? O4 C7 N7 125.7(2) . . ? N8 C7 N7 108.3(2) . . ? O2 C3 N4 126.0(2) . . ? O2 C3 N3 125.8(2) . . ? N4 C3 N3 108.2(2) . . ? N23 C21 N9 114.3(2) . . ? N23 C21 C22 103.5(2) . . ? N9 C21 C22 102.99(19) . . ? C29 N20 C30 121.0(2) . . ? C29 N20 C18 112.0(2) . . ? C30 N20 C18 123.9(2) . . ? C29 N19 C28 122.6(2) . . ? C29 N19 C17 112.8(2) . . ? C28 N19 C17 124.6(2) . . ? O7 C27 N17 125.9(3) . . ? O7 C27 N18 126.1(3) . . ? N17 C27 N18 108.0(2) . . ? N12 C12 N1 113.5(2) . . ? C31 N22 C32 122.7(2) . . ? C31 N22 C20 113.2(2) . . ? C32 N22 C20 123.7(2) . . ? O11 C35 N25 125.9(2) . . ? O11 C35 N26 125.1(2) . . ? N25 C35 N26 109.0(2) . . ? C11 N11 C23 112.3(2) . . ? C11 N11 C10 122.3(2) . . ? C23 N11 C10 123.0(2) . . ? N16 C14 N2 114.3(2) . . ? N16 C14 C13 103.27(18) . . ? N2 C14 C13 103.37(19) . . ? N10 C22 N24 114.31(19) . . ? N10 C22 C21 103.18(19) . . ? N24 C22 C21 103.2(2) . . ? N17 C26 N16 112.8(2) . . ? N17 C15 N3 113.9(2) . . ? N17 C15 C16 103.2(2) . . ? N3 C15 C16 103.58(19) . . ? N6 C18 N20 115.0(2) . . ? N6 C18 C17 103.1(2) . . ? N20 C18 C17 103.0(2) . . ? N22 C20 N8 114.1(2) . . ? N22 C20 C19 102.7(2) . . ? N8 C20 C19 103.5(2) . . ? N15 C36 N26 113.7(2) . . ? N23 C32 N22 114.0(2) . . ? O6 C11 N11 125.7(2) . . ? O6 C11 N12 125.5(2) . . ? N11 C11 N12 108.8(2) . . ? N11 C23 N25 114.6(2) . . ? N11 C23 C24 103.19(19) . . ? N25 C23 C24 103.40(19) . . ? N15 C13 N1 115.0(2) . . ? N15 C13 C14 102.9(2) . . ? N1 C13 C14 103.04(19) . . ? N11 C10 N10 114.3(2) . . ? N21 C19 N7 114.2(2) . . ? N21 C19 C20 103.4(2) . . ? N7 C19 C20 102.9(2) . . ? N9 C8 N8 114.1(2) . . ? O10 C33 N24 125.8(3) . . ? O10 C33 N23 125.9(3) . . ? N24 C33 N23 108.4(2) . . ? O9 C31 N21 126.4(3) . . ? O9 C31 N22 125.9(3) . . ? N21 C31 N22 107.7(2) . . ? O8 C29 N19 126.7(3) . . ? O8 C29 N20 124.9(3) . . ? N19 C29 N20 108.4(2) . . ? N18 C16 N4 115.0(2) . . ? N18 C16 C15 103.1(2) . . ? N4 C16 C15 103.4(2) . . ? N19 C17 N5 114.9(2) . . ? N19 C17 C18 103.2(2) . . ? N5 C17 C18 103.35(19) . . ? N12 C24 N26 114.3(2) . . ? N12 C24 C23 103.25(19) . . ? N26 C24 C23 103.04(19) . . ? N24 C34 N25 113.69(19) . . ? N7 C6 N6 114.1(2) . . ? N20 C30 N21 113.2(2) . . ? N19 C28 N18 114.1(2) . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 71.98 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 1.108 _refine_diff_density_min -1.011 _refine_diff_density_rms 0.085 _database_code_depnum_ccdc_archive 'CCDC 946818' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_q6_isopr_ca _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C94 H214 Ca2 Cl4 N50 O83' _chemical_formula_weight 3594.98 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' Ca Ca 0.3641 1.2855 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/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 22.1854(2) _cell_length_b 15.9734(2) _cell_length_c 22.9981(3) _cell_angle_alpha 90.00 _cell_angle_beta 105.0202(11) _cell_angle_gamma 90.00 _cell_volume 7871.54(16) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 19998 _cell_measurement_theta_min 3.70 _cell_measurement_theta_max 71.29 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.472 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3588 _exptl_absorpt_coefficient_mu 2.286 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.67848 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.21b (release 03-02-2012 CrysAlis171 .NET) (compiled Feb 3 2012,10:37:01) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'SuperNova (Cu) X-ray Source' _diffrn_radiation_monochromator mirror _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Eos' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.2974 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 34191 _diffrn_reflns_av_R_equivalents 0.0234 _diffrn_reflns_av_sigmaI/netI 0.0240 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 3.71 _diffrn_reflns_theta_max 71.43 _reflns_number_total 15017 _reflns_number_gt 13436 _reflns_threshold_expression >2\s(I) _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.35.21b (release 03-02-2012 CrysAlis171 .NET) (compiled Feb 3 2012,10:37:01) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.35.21b (release 03-02-2012 CrysAlis171 .NET) (compiled Feb 3 2012,10:37:01) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.35.21b (release 03-02-2012 CrysAlis171 .NET) (compiled Feb 3 2012,10:37:01) ; _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(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^)+(0.1568P)^2^+11.6050P] 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 15017 _refine_ls_number_parameters 1430 _refine_ls_number_restraints 178 _refine_ls_R_factor_all 0.0934 _refine_ls_R_factor_gt 0.0859 _refine_ls_wR_factor_ref 0.2505 _refine_ls_wR_factor_gt 0.2439 _refine_ls_goodness_of_fit_ref 1.012 _refine_ls_restrained_S_all 1.007 _refine_ls_shift/su_max 0.021 _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 Ca1 Ca 0.58855(4) 0.04409(5) 0.61649(4) 0.0259(3) Uani 0.661(2) 1 d P . 1 O1W O 0.5531(3) 0.1659(4) 0.5544(3) 0.0337(12) Uani 0.661(2) 1 d P . 1 O2W O 0.59200(15) 0.0103(2) 0.51060(17) 0.0288(7) Uani 0.661(2) 1 d P . 1 O3W O 0.5183(2) -0.0730(2) 0.57955(16) 0.0305(8) Uani 0.661(2) 1 d P . 1 O4W O 0.6118(2) -0.0190(5) 0.7152(2) 0.0667(16) Uani 0.661(2) 1 d P . 1 O5W O 0.6070(2) 0.1647(3) 0.6904(2) 0.0656(13) Uani 0.661(2) 1 d P . 1 O7WA O 0.4847(3) 0.2634(5) 0.4215(4) 0.099(2) Uani 0.661(2) 1 d P . 1 O22W O 0.4810(8) 0.3749(5) 0.5215(5) 0.193(6) Uani 0.661(2) 1 d P . 1 O27A O 0.6139(9) -0.0721(9) 0.9088(8) 0.154(7) Uani 0.40 1 d P A 1 O27B O 0.6568(7) -0.0534(13) 0.8975(9) 0.065(6) Uani 0.20 1 d P A 1 Ca2 Ca 0.52336(7) 0.17252(9) 0.46762(7) 0.0252(5) Uani 0.339(2) 1 d P . 2 O2W1 O 0.5784(3) 0.0335(4) 0.4819(3) 0.0289(13) Uani 0.339(2) 1 d P . 2 O1W1 O 0.5628(5) 0.1466(7) 0.5740(5) 0.029(2) Uani 0.339(2) 1 d P . 2 O6W O 0.5254(3) 0.3162(4) 0.5145(3) 0.0411(15) Uani 0.339(2) 1 d P . 2 O7W O 0.4709(4) 0.2662(5) 0.3868(3) 0.0375(16) Uani 0.339(2) 1 d P . 2 O3W1 O 0.5493(4) -0.0645(4) 0.5813(3) 0.0307(15) Uani 0.339(2) 1 d P . 2 O4W1 O 0.6191(6) 0.0324(9) 0.7112(6) 0.079(4) Uani 0.339(2) 1 d P . 2 O25W O 0.6180(4) -0.1287(7) 0.7662(4) 0.068(3) Uani 0.339(2) 1 d P . 2 O22A O 0.4172(5) 0.4055(6) 0.4838(6) 0.078(3) Uani 0.339(2) 1 d P . 2 O24W O 0.4365(8) 0.5304(13) 0.5549(8) 0.114(6) Uani 0.339(2) 1 d P . 2 O27W O 0.6392(11) -0.1014(10) 0.8764(8) 0.121(8) Uani 0.339(2) 1 d P . 2 C11X C 0.72386(15) 0.0017(2) 0.39172(15) 0.0428(7) Uani 1 1 d . B . H11A H 0.7271 0.0629 0.3924 0.064 Uiso 1 1 calc R . . H11B H 0.6811 -0.0147 0.3909 0.064 Uiso 1 1 calc R . . H11C H 0.7345 -0.0199 0.3558 0.064 Uiso 1 1 calc R . . N1X N 0.83529(11) -0.02261(17) 0.44463(12) 0.0360(6) Uani 1 1 d . B . H1X1 H 0.8421 0.0336 0.4402 0.043 Uiso 1 1 calc R . . H1X2 H 0.8611 -0.0391 0.4809 0.043 Uiso 1 1 calc R . . C10X C 0.75886(14) 0.0062(2) 0.50406(14) 0.0396(7) Uani 1 1 d . B . H10A H 0.7876 -0.0189 0.5394 0.059 Uiso 1 1 calc R . . H10B H 0.7158 -0.0028 0.5061 0.059 Uiso 1 1 calc R . . H10E H 0.7670 0.0665 0.5033 0.059 Uiso 1 1 calc R . . C8X C 0.85381(15) -0.0691(2) 0.39550(15) 0.0401(7) Uani 1 1 d G . . H8X1 H 0.8465 -0.0272 0.3639 0.048 Uiso 0.553(7) 1 d PG B 1 H8X2 H 0.8249 -0.1149 0.3819 0.048 Uiso 0.553(7) 1 d PG B 1 H8X3 H 0.8413 -0.1275 0.3930 0.048 Uiso 0.447(7) 1 d PG B 2 H8X4 H 0.8278 -0.0405 0.3608 0.048 Uiso 0.447(7) 1 d PG B 2 C9X C 0.76842(13) -0.0340(2) 0.44738(14) 0.0351(6) Uani 1 1 d . . . H9X H 0.7600 -0.0954 0.4490 0.042 Uiso 1 1 calc R B . O9W O 0.82257(15) -0.0344(3) 0.18994(15) 0.0784(10) Uani 1 1 d . . . O8W O 0.7380(6) 0.0291(5) 0.0772(5) 0.082(3) Uani 0.698(18) 1 d P . . O8WA O 0.7653(8) 0.0245(12) 0.0759(9) 0.070(6) Uani 0.302(18) 1 d P . . O10W O 0.9099(3) 0.1395(4) 0.3034(3) 0.074(3) Uani 0.695(16) 1 d P C 1 O10A O 0.9585(19) 0.1689(12) 0.3186(9) 0.204(18) Uani 0.305(16) 1 d P C 2 O26W O 0.5014(5) 0.1887(7) 0.9169(6) 0.122(4) Uani 0.519(10) 1 d P D 1 O28W O 0.6187(7) 0.0533(11) 0.8255(4) 0.192(8) Uani 0.519(10) 1 d P D 1 O30W O 0.5477(5) 0.0667(5) 0.8869(5) 0.108(4) Uani 0.481(10) 1 d P D 2 O26A O 0.4753(19) 0.1720(15) 0.9574(13) 0.308(19) Uani 0.481(10) 1 d P . 2 O31W O 0.5887(3) 0.3254(3) 0.6334(3) 0.1220(18) Uani 1 1 d . . . O11W O 0.7408(3) -0.4573(3) 0.6244(2) 0.0894(18) Uani 0.799(10) 1 d P E 1 O11A O 0.7321(15) -0.512(2) 0.622(3) 0.20(2) Uani 0.201(10) 1 d P E 2 O13W O 0.9273(4) 0.0738(4) 0.2034(4) 0.097(2) Uani 0.701(8) 1 d P F 1 O15W O 1.0510(4) 0.0247(6) 0.1912(3) 0.138(4) Uani 0.701(8) 1 d P F 1 O21W O 1.1067(8) -0.0863(11) 0.1503(7) 0.230(6) Uiso 0.701(8) 1 d P F 1 O13A O 0.9308(6) 0.0327(11) 0.1663(10) 0.096(6) Uani 0.299(8) 1 d P F 2 O15A O 1.0333(7) 0.1395(11) 0.2310(7) 0.115(7) Uani 0.299(8) 1 d P . 2 O21A O 1.1832(10) -0.1195(14) 0.1964(10) 0.136(7) Uiso 0.299(8) 1 d P F 2 O21B O 1.0507(11) -0.1396(16) 0.1571(11) 0.154(9) Uiso 0.299(8) 1 d P . 2 O18W O 0.8715(4) 0.3651(4) 0.3953(3) 0.095(3) Uani 0.698(18) 1 d P . . O18A O 0.9115(14) 0.3385(15) 0.3974(11) 0.127(8) Uiso 0.302(18) 1 d P . . O14W O 0.8027(5) -0.0445(3) -0.0072(4) 0.153(4) Uani 0.799(10) 1 d P . . O14A O 0.9144(11) -0.0564(14) 0.0400(10) 0.074(6) Uiso 0.201(10) 1 d P . . C1X C 1.0022(4) -0.2070(8) 0.2800(5) 0.0516(19) Uani 0.553(7) 1 d PDU B 1 C2X C 0.9993(7) -0.2466(7) 0.3319(6) 0.042(2) Uani 0.553(7) 1 d PDU B 1 C3X C 0.9713(4) -0.2077(6) 0.3715(4) 0.0375(16) Uani 0.553(7) 1 d PDU B 1 H3X H 0.9715 -0.2347 0.4083 0.045 Uiso 0.553(7) 1 calc PR B 1 C4X C 0.9421(11) -0.1283(8) 0.3589(7) 0.031(3) Uani 0.553(7) 1 d PDU B 1 C5X C 0.9488(11) -0.0882(10) 0.3082(7) 0.045(3) Uani 0.553(7) 1 d PDU B 1 H5X H 0.9334 -0.0328 0.3002 0.054 Uiso 0.553(7) 1 calc PR B 1 C6X C 0.9778(4) -0.1272(7) 0.2677(4) 0.052(2) Uani 0.553(7) 1 d PDU B 1 H6X H 0.9806 -0.0990 0.2322 0.063 Uiso 0.553(7) 1 calc PR B 1 C7X C 0.9232(4) -0.0835(6) 0.4117(4) 0.0425(18) Uani 0.553(7) 1 d PU B 1 H7X H 0.9340 -0.1214 0.4475 0.051 Uiso 0.553(7) 1 calc PR B 1 O1X O 0.9556(3) -0.0062(5) 0.4281(4) 0.0588(19) Uani 0.553(7) 1 d PU B 1 H1X H 0.9936 -0.0159 0.4432 0.088 Uiso 0.553(7) 1 calc PR B 1 O2X O 1.0313(3) -0.2445(5) 0.2397(3) 0.077(2) Uani 0.553(7) 1 d PU B 1 H2X H 1.0042 -0.2599 0.2088 0.116 Uiso 0.553(7) 1 calc PR B 1 O3X O 1.0260(3) -0.3231(4) 0.3400(3) 0.0664(19) Uani 0.553(7) 1 d PU B 1 H3X1 H 1.0580 -0.3215 0.3691 0.100 Uiso 0.553(7) 1 calc PR B 1 O12W O 1.0132(5) -0.1706(10) 0.5472(5) 0.103(4) Uani 0.553(7) 1 d P B 1 O17W O 1.0055(6) -0.4017(8) 0.4351(8) 0.185(7) Uani 0.553(7) 1 d P B 1 O16W O 0.8840(4) -0.3876(5) 0.4030(4) 0.093(3) Uani 0.553(7) 1 d P B 1 C1XA C 1.0023(10) -0.2409(12) 0.3108(8) 0.048(3) Uani 0.447(7) 1 d PDU B 2 C2XA C 0.9838(4) -0.2599(6) 0.3615(5) 0.0435(19) Uani 0.447(7) 1 d PDU B 2 C3XA C 0.9554(5) -0.2000(7) 0.3880(5) 0.041(2) Uani 0.447(7) 1 d PDU B 2 H3XA H 0.9397 -0.2143 0.4214 0.049 Uiso 0.447(7) 1 calc PR B 2 C4XA C 0.9495(15) -0.1167(10) 0.3655(9) 0.042(5) Uani 0.447(7) 1 d PDU B 2 C5XA C 0.9621(13) -0.1018(13) 0.3113(10) 0.050(4) Uani 0.447(7) 1 d PDU B 2 H5XA H 0.9510 -0.0496 0.2917 0.060 Uiso 0.447(7) 1 calc PR B 2 C6XA C 0.9913(6) -0.1631(10) 0.2842(6) 0.054(3) Uani 0.447(7) 1 d PDU B 2 H6XA H 1.0032 -0.1512 0.2482 0.064 Uiso 0.447(7) 1 calc PR B 2 C7XA C 0.9163(6) -0.0519(8) 0.3919(6) 0.050(2) Uani 0.447(7) 1 d PU B 2 H7XA H 0.9165 0.0020 0.3698 0.061 Uiso 0.447(7) 1 calc PR B 2 O1XA O 0.9546(4) -0.0425(9) 0.4529(4) 0.071(3) Uani 0.447(7) 1 d PU B 2 H1XA H 0.9922 -0.0377 0.4525 0.107 Uiso 0.447(7) 1 calc PR B 2 O2XA O 1.0334(3) -0.2990(6) 0.2856(4) 0.080(3) Uani 0.447(7) 1 d PU B 2 H2XA H 1.0681 -0.2795 0.2840 0.119 Uiso 0.447(7) 1 calc PR B 2 O3XA O 0.9964(4) -0.3384(6) 0.3836(5) 0.089(3) Uani 0.447(7) 1 d PU B 2 H3X2 H 0.9805 -0.3453 0.4127 0.134 Uiso 0.447(7) 1 calc PR B 2 O12A O 1.0147(5) -0.1484(9) 0.5741(5) 0.068(3) Uani 0.447(7) 1 d P B 2 O16A O 0.9204(6) -0.3632(8) 0.4602(7) 0.124(5) Uani 0.447(7) 1 d P B 2 O20W O 1.0740(10) -0.2116(13) 0.1844(9) 0.086(5) Uiso 0.20 1 d P . 2 O20A O 1.0903(6) -0.2882(9) 0.2048(6) 0.070(3) Uiso 0.25 1 d P G 2 O19W O 0.6314(5) -0.0220(7) 0.0206(6) 0.261(6) Uani 1 1 d . . . Cl2 Cl 0.7516(4) 0.2440(7) 0.7378(3) 0.231(6) Uani 0.40 1 d P H 1 O23A O 0.6365(7) 0.3535(7) 0.6638(5) 0.105(4) Uani 0.40 1 d P I 1 O23B O 0.6935(12) 0.4105(14) 0.6721(12) 0.175(11) Uani 0.40 1 d P I 1 O29W O 0.7276(5) 0.1591(8) 0.7639(6) 0.071(3) Uani 0.30 1 d P J 2 O29A O 0.7322(8) 0.1121(12) 0.8067(10) 0.082(6) Uani 0.20 1 d P J 2 Cl2A Cl 0.8139(14) 0.3071(12) 0.7422(8) 0.44(2) Uani 0.30 1 d P . 2 Cl2B Cl 0.8018(5) 0.2386(10) 0.7498(5) 0.216(7) Uani 0.30 1 d P K 3 O23W O 0.7103(8) 0.3709(10) 0.6941(7) 0.074(4) Uani 0.30 1 d P L 3 Cl1 Cl 0.56043(12) 0.2015(3) 0.80735(13) 0.0959(10) Uani 0.55 1 d P M 1 Cl1A Cl 0.5465(3) 0.2565(4) 0.7909(5) 0.161(5) Uani 0.30 1 d P . 2 Cl1B Cl 0.5758(4) 0.2071(6) 0.7349(7) 0.113(5) Uani 0.15 1 d P N 3 O2 O 0.92203(9) 0.05630(14) 0.54836(9) 0.0355(5) Uani 1 1 d . . . O1 O 0.88945(10) -0.13968(15) 0.54473(10) 0.0402(5) Uani 1 1 d . . . O3 O 0.85670(9) 0.14919(14) 0.41816(9) 0.0351(5) Uani 1 1 d . . . O11 O 0.51601(10) -0.06328(14) 0.36367(12) 0.0424(5) Uani 1 1 d . . . O12 O 0.57542(9) -0.17214(15) 0.49480(11) 0.0410(5) Uani 1 1 d . . . O6 O 0.81237(10) -0.25571(17) 0.41732(12) 0.0477(6) Uani 1 1 d . . . O5 O 0.75052(10) -0.13617(17) 0.28058(10) 0.0441(6) Uani 1 1 d . . . O4 O 0.78015(11) 0.07039(17) 0.27694(11) 0.0451(5) Uani 1 1 d . . . N3 N 0.88255(12) 0.04689(17) 0.63190(11) 0.0359(6) Uani 1 1 d . . . O7 O 0.66046(12) -0.07995(17) 0.62482(15) 0.0582(7) Uani 1 1 d . . . O8 O 0.68448(10) 0.11235(15) 0.61878(12) 0.0454(6) Uani 1 1 d . . . O10 O 0.54931(11) 0.14552(17) 0.36048(14) 0.0537(7) Uani 1 1 d . . . N6 N 0.76974(11) 0.23448(17) 0.38956(12) 0.0349(5) Uani 1 1 d . . . N25 N 0.57030(12) -0.17076(16) 0.33338(12) 0.0370(6) Uani 1 1 d . . . N4 N 0.86945(11) 0.16473(17) 0.57949(11) 0.0322(5) Uani 1 1 d . . . O9 O 0.62041(11) 0.24054(17) 0.48102(12) 0.0478(6) Uani 1 1 d . . . N19 N 0.72723(11) 0.25939(16) 0.51048(13) 0.0357(6) Uani 1 1 d . . . N15 N 0.72404(13) -0.19035(17) 0.61428(13) 0.0391(6) Uani 1 1 d . . . N18 N 0.76920(11) 0.18368(17) 0.60314(12) 0.0353(6) Uani 1 1 d . . . N5 N 0.82523(11) 0.23637(16) 0.48493(11) 0.0328(5) Uani 1 1 d . . . N7 N 0.71749(12) 0.18001(18) 0.29073(12) 0.0408(6) Uani 1 1 d . . . N20 N 0.67699(12) 0.28510(16) 0.41549(13) 0.0384(6) Uani 1 1 d . . . N17 N 0.78605(12) 0.07003(18) 0.66086(12) 0.0387(6) Uani 1 1 d . . . N26 N 0.61053(12) -0.24897(16) 0.42490(13) 0.0374(6) Uani 1 1 d . . . N24 N 0.55663(12) -0.05271(18) 0.28136(12) 0.0381(6) Uani 1 1 d . . . N22 N 0.58124(12) 0.09489(19) 0.27977(13) 0.0421(6) Uani 1 1 d . . . N9 N 0.65126(12) -0.0811(2) 0.24874(12) 0.0426(6) Uani 1 1 d . . . C5 C 0.82136(12) 0.20196(19) 0.42998(13) 0.0308(6) Uani 1 1 d . . . N1 N 0.81742(12) -0.21462(17) 0.57999(12) 0.0373(6) Uani 1 1 d . . . N11 N 0.70552(12) -0.27425(17) 0.39396(13) 0.0384(6) Uani 1 1 d . . . C35 C 0.61324(13) -0.21929(18) 0.48111(14) 0.0334(6) Uani 1 1 d . . . N12 N 0.75976(12) -0.28480(18) 0.48910(13) 0.0394(6) Uani 1 1 d . . . N27 N 0.66543(12) -0.25042(16) 0.52008(12) 0.0357(6) Uani 1 1 d . . . N21 N 0.62377(12) 0.21197(19) 0.32392(14) 0.0436(6) Uani 1 1 d . . . N16 N 0.76792(14) -0.07873(19) 0.66462(13) 0.0435(6) Uani 1 1 d . . . C3 C 0.89392(12) 0.0866(2) 0.58316(12) 0.0320(6) Uani 1 1 d . . . N2 N 0.86168(12) -0.10260(18) 0.63107(11) 0.0371(6) Uani 1 1 d . . . C1 C 0.85930(14) -0.1512(2) 0.58201(13) 0.0358(6) Uani 1 1 d . . . C33 C 0.54483(13) -0.0922(2) 0.32943(15) 0.0360(6) Uani 1 1 d . . . C27 C 0.74115(14) 0.1207(2) 0.62685(14) 0.0375(7) Uani 1 1 d . . . C11 C 0.76444(14) -0.2704(2) 0.43225(15) 0.0378(7) Uani 1 1 d . . . N8 N 0.67272(13) 0.0677(2) 0.24214(13) 0.0468(7) Uani 1 1 d . . . C34 C 0.55818(14) -0.23362(19) 0.37372(15) 0.0367(7) Uani 1 1 d . . . H34A H 0.5468 -0.2866 0.3512 0.044 Uiso 1 1 calc R . . H34B H 0.5220 -0.2159 0.3884 0.044 Uiso 1 1 calc R . . N10 N 0.66410(12) -0.20076(19) 0.29999(12) 0.0395(6) Uani 1 1 d . . . C29 C 0.66964(14) 0.25920(19) 0.46995(15) 0.0371(7) Uani 1 1 d . . . C9 C 0.69441(15) -0.1389(2) 0.27733(13) 0.0399(7) Uani 1 1 d . . . C28 C 0.73510(15) 0.25627(19) 0.57481(15) 0.0378(7) Uani 1 1 d . . . H28A H 0.7574 0.3073 0.5932 0.045 Uiso 1 1 calc R . . H28B H 0.6934 0.2565 0.5830 0.045 Uiso 1 1 calc R . . C16 C 0.83694(14) 0.1804(2) 0.62561(13) 0.0348(6) Uani 1 1 d . . . H16 H 0.8538 0.2307 0.6504 0.042 Uiso 1 1 calc R . . C32 C 0.53372(14) 0.0306(2) 0.26241(16) 0.0421(7) Uani 1 1 d . . . H32A H 0.4988 0.0440 0.2802 0.050 Uiso 1 1 calc R . . H32B H 0.5172 0.0312 0.2181 0.050 Uiso 1 1 calc R . . C18 C 0.74120(13) 0.30084(19) 0.41677(15) 0.0362(7) Uani 1 1 d . . . H18 H 0.7470 0.3572 0.4000 0.043 Uiso 1 1 calc R . . C25 C 0.71235(16) -0.1128(2) 0.63355(16) 0.0428(7) Uani 1 1 d . . . C13 C 0.78986(15) -0.2115(2) 0.63087(14) 0.0383(7) Uani 1 1 d . . . H13 H 0.7985 -0.2635 0.6559 0.046 Uiso 1 1 calc R . . C7 C 0.72871(14) 0.1023(2) 0.27095(14) 0.0398(7) Uani 1 1 d . . . C24 C 0.66060(14) -0.30606(18) 0.42434(15) 0.0369(7) Uani 1 1 d . . . H24 H 0.6445 -0.3624 0.4088 0.044 Uiso 1 1 calc R . . C25B C 0.69757(14) -0.30987(18) 0.49086(15) 0.0363(6) Uani 1 1 d . . . H25B H 0.6973 -0.3675 0.5078 0.044 Uiso 1 1 calc R . . C23 C 0.59710(14) -0.1885(2) 0.28329(14) 0.0392(7) Uani 1 1 d . . . H23 H 0.5751 -0.2360 0.2582 0.047 Uiso 1 1 calc R . . C12 C 0.81342(15) -0.2862(2) 0.54092(16) 0.0409(7) Uani 1 1 d . . . H12A H 0.8117 -0.3376 0.5644 0.049 Uiso 1 1 calc R . . H12B H 0.8518 -0.2889 0.5266 0.049 Uiso 1 1 calc R . . C4 C 0.87864(13) 0.2257(2) 0.53640(13) 0.0347(6) Uani 1 1 d . . . H4A H 0.9150 0.2086 0.5218 0.042 Uiso 1 1 calc R . . H4B H 0.8887 0.2803 0.5570 0.042 Uiso 1 1 calc R . . C2 C 0.90658(14) -0.0359(2) 0.65055(14) 0.0390(7) Uani 1 1 d . . . H2A H 0.9212 -0.0371 0.6950 0.047 Uiso 1 1 calc R . . H2B H 0.9431 -0.0466 0.6344 0.047 Uiso 1 1 calc R . . C10 C 0.69539(16) -0.2745(2) 0.32904(16) 0.0435(8) Uani 1 1 d . . . H10C H 0.7362 -0.2796 0.3195 0.052 Uiso 1 1 calc R . . H10D H 0.6703 -0.3243 0.3124 0.052 Uiso 1 1 calc R . . C36 C 0.67506(15) -0.2466(2) 0.58478(15) 0.0381(7) Uani 1 1 d . . . H36A H 0.6357 -0.2289 0.5937 0.046 Uiso 1 1 calc R . . H36B H 0.6851 -0.3035 0.6016 0.046 Uiso 1 1 calc R . . C31 C 0.58173(14) 0.1498(2) 0.32491(16) 0.0422(7) Uani 1 1 d . . . C8 C 0.66634(17) -0.0133(3) 0.21301(15) 0.0483(8) Uani 1 1 d . . . H8A H 0.7059 -0.0270 0.2028 0.058 Uiso 1 1 calc R . . H8B H 0.6332 -0.0097 0.1748 0.058 Uiso 1 1 calc R . . C17 C 0.77482(14) 0.29379(19) 0.48412(15) 0.0356(6) Uani 1 1 d . . . H17 H 0.7904 0.3493 0.5020 0.043 Uiso 1 1 calc R . . C15 C 0.84814(14) 0.0993(2) 0.66346(13) 0.0368(7) Uani 1 1 d . . . H15 H 0.8725 0.1104 0.7058 0.044 Uiso 1 1 calc R . . C20 C 0.62060(15) 0.1222(2) 0.24159(15) 0.0452(8) Uani 1 1 d . . . H20 H 0.5955 0.1342 0.1996 0.054 Uiso 1 1 calc R . . C6 C 0.76627(14) 0.2343(2) 0.32574(14) 0.0390(7) Uani 1 1 d . . . H6A H 0.8070 0.2159 0.3200 0.047 Uiso 1 1 calc R . . H6B H 0.7587 0.2922 0.3102 0.047 Uiso 1 1 calc R . . C21 C 0.58816(14) -0.1062(2) 0.24756(14) 0.0409(7) Uani 1 1 d . . . H21 H 0.5623 -0.1147 0.2054 0.049 Uiso 1 1 calc R . . C19 C 0.65173(15) 0.2023(2) 0.27368(16) 0.0439(8) Uani 1 1 d . . . H19 H 0.6435 0.2520 0.2463 0.053 Uiso 1 1 calc R . . C14 C 0.82057(15) -0.1333(2) 0.66623(14) 0.0412(7) Uani 1 1 d . . . H14 H 0.8440 -0.1475 0.7084 0.049 Uiso 1 1 calc R . . C30 C 0.62729(15) 0.2864(2) 0.36037(18) 0.0465(8) Uani 1 1 d . . . H30A H 0.5870 0.2937 0.3707 0.056 Uiso 1 1 calc R . . H30B H 0.6333 0.3355 0.3362 0.056 Uiso 1 1 calc R . . C26 C 0.77257(17) 0.0009(2) 0.69565(15) 0.0444(8) Uani 1 1 d . . . H26A H 0.7327 0.0121 0.7061 0.053 Uiso 1 1 calc R . . H26B H 0.8058 -0.0029 0.7337 0.053 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 Ca1 0.0199(4) 0.0309(4) 0.0280(4) -0.0044(3) 0.0080(3) -0.0038(3) O1W 0.025(2) 0.035(3) 0.043(3) -0.001(2) 0.011(2) -0.0010(18) O2W 0.0273(16) 0.0294(17) 0.0291(17) 0.0004(14) 0.0062(14) 0.0008(13) O3W 0.0256(19) 0.0327(17) 0.0338(17) -0.0028(12) 0.0089(16) -0.0054(16) O4W 0.043(2) 0.123(5) 0.037(2) 0.016(3) 0.0144(17) 0.020(3) O5W 0.057(2) 0.089(3) 0.057(2) -0.038(2) 0.027(2) -0.029(2) O7WA 0.056(4) 0.113(5) 0.137(6) 0.033(5) 0.044(4) 0.014(3) O22W 0.359(19) 0.066(5) 0.197(10) -0.043(6) 0.148(12) -0.075(8) O27A 0.154(14) 0.076(8) 0.171(15) 0.006(9) -0.068(12) 0.002(9) O27B 0.020(6) 0.091(13) 0.074(11) 0.064(11) -0.006(6) 0.008(7) Ca2 0.0204(8) 0.0258(8) 0.0289(8) 0.0005(6) 0.0056(6) 0.0000(6) O2W1 0.031(3) 0.025(3) 0.029(3) 0.004(3) 0.004(3) 0.005(2) O1W1 0.021(4) 0.036(6) 0.030(5) -0.003(4) 0.007(4) -0.004(4) O6W 0.037(3) 0.040(3) 0.046(4) -0.006(3) 0.012(3) -0.004(3) O7W 0.037(4) 0.036(3) 0.039(4) 0.003(3) 0.009(3) 0.005(3) O3W1 0.024(4) 0.034(3) 0.033(3) -0.002(2) 0.006(3) 0.000(3) O4W1 0.075(7) 0.101(9) 0.079(7) 0.039(7) 0.053(6) 0.049(7) O25W 0.055(5) 0.103(7) 0.050(4) 0.005(4) 0.021(4) -0.046(5) O22A 0.061(6) 0.059(5) 0.115(8) 0.027(6) 0.026(5) 0.013(5) O24W 0.075(9) 0.143(14) 0.131(13) 0.035(11) 0.037(9) -0.007(9) O27W 0.190(19) 0.082(10) 0.123(13) 0.052(9) 0.102(13) 0.080(12) C11X 0.0320(16) 0.0536(19) 0.0374(16) -0.0036(14) -0.0009(12) 0.0023(14) N1X 0.0254(12) 0.0448(14) 0.0364(13) -0.0015(11) 0.0055(10) -0.0056(10) C10X 0.0287(15) 0.0516(18) 0.0367(15) 0.0031(13) 0.0054(12) -0.0032(13) C8X 0.0284(15) 0.0500(18) 0.0390(16) -0.0057(14) 0.0036(12) 0.0002(13) C9X 0.0222(13) 0.0402(15) 0.0413(16) -0.0008(12) 0.0051(11) -0.0053(11) O9W 0.0594(18) 0.109(3) 0.0659(19) -0.0259(18) 0.0142(15) 0.0261(18) O8W 0.126(7) 0.028(3) 0.110(5) 0.024(3) 0.061(6) 0.026(4) O8WA 0.053(8) 0.055(9) 0.083(10) 0.023(7) -0.016(7) -0.043(7) O10W 0.066(4) 0.088(4) 0.074(4) 0.031(3) 0.026(3) 0.015(3) O10A 0.31(4) 0.086(12) 0.119(14) 0.008(10) -0.118(19) 0.001(17) O26W 0.090(6) 0.118(8) 0.152(10) -0.010(7) 0.021(6) 0.001(5) O28W 0.233(14) 0.308(19) 0.047(4) -0.062(7) 0.054(6) -0.148(13) O30W 0.132(8) 0.068(5) 0.123(8) -0.048(5) 0.032(6) 0.005(5) O26A 0.55(5) 0.19(2) 0.27(3) 0.073(19) 0.26(4) 0.10(3) O31W 0.136(4) 0.094(3) 0.144(4) -0.043(3) 0.052(4) -0.042(3) O11W 0.114(4) 0.051(3) 0.082(3) 0.016(2) -0.011(3) 0.020(3) O11A 0.10(2) 0.08(2) 0.43(7) 0.00(3) 0.07(3) 0.021(16) O13W 0.113(5) 0.069(4) 0.096(5) 0.046(3) 0.004(4) -0.001(3) O15W 0.146(6) 0.214(9) 0.065(4) 0.058(5) 0.048(4) 0.049(6) O13A 0.057(7) 0.083(10) 0.143(15) 0.072(10) 0.018(8) -0.020(7) O15A 0.097(10) 0.118(12) 0.098(10) 0.057(9) -0.032(8) -0.007(9) O18W 0.093(5) 0.084(4) 0.105(4) 0.038(3) 0.018(3) -0.035(4) O14W 0.249(10) 0.055(3) 0.179(7) -0.016(4) 0.098(7) -0.048(4) C1X 0.031(4) 0.080(6) 0.040(5) -0.020(4) 0.002(3) -0.009(4) C2X 0.025(5) 0.051(4) 0.044(8) -0.017(4) -0.003(6) 0.003(3) C3X 0.028(4) 0.048(4) 0.033(4) -0.006(3) 0.003(3) -0.003(3) C4X 0.014(5) 0.038(4) 0.037(4) -0.017(3) -0.001(4) -0.012(4) C5X 0.026(9) 0.056(5) 0.044(4) 0.002(3) -0.008(4) -0.005(3) C6X 0.036(4) 0.080(5) 0.037(4) 0.000(4) 0.003(3) -0.014(4) C7X 0.026(3) 0.056(5) 0.041(4) -0.008(3) -0.001(3) 0.010(3) O1X 0.024(2) 0.073(4) 0.079(5) -0.041(3) 0.010(3) -0.004(3) O2X 0.045(3) 0.137(6) 0.051(3) -0.034(4) 0.013(2) 0.000(3) O3X 0.054(3) 0.062(3) 0.068(4) -0.023(3) -0.010(3) 0.015(2) O12W 0.040(4) 0.171(12) 0.106(8) 0.042(8) 0.032(6) 0.018(5) O17W 0.183(12) 0.123(9) 0.285(17) 0.113(10) 0.127(12) 0.061(8) O16W 0.133(7) 0.075(4) 0.087(5) -0.009(4) 0.055(5) 0.027(4) C1XA 0.026(4) 0.080(6) 0.037(9) -0.033(5) 0.009(7) -0.006(5) C2XA 0.029(4) 0.055(5) 0.043(5) -0.019(4) 0.003(3) 0.001(4) C3XA 0.034(5) 0.058(5) 0.032(5) -0.015(4) 0.011(3) -0.007(4) C4XA 0.024(8) 0.050(6) 0.044(6) -0.017(5) -0.006(5) -0.012(6) C5XA 0.021(10) 0.064(8) 0.060(7) -0.001(5) 0.001(7) -0.012(5) C6XA 0.039(7) 0.082(8) 0.039(6) -0.018(6) 0.008(5) -0.028(6) C7XA 0.041(6) 0.052(6) 0.061(6) -0.014(5) 0.016(5) -0.011(5) O1XA 0.028(3) 0.136(10) 0.053(5) -0.042(5) 0.015(3) -0.021(5) O2XA 0.041(3) 0.112(6) 0.092(7) -0.073(6) 0.027(4) -0.013(4) O3XA 0.071(5) 0.074(5) 0.106(7) -0.007(4) -0.006(5) 0.005(4) O12A 0.036(4) 0.104(7) 0.068(6) -0.003(5) 0.020(4) -0.011(4) O16A 0.102(8) 0.108(8) 0.180(13) 0.049(9) 0.070(9) 0.034(7) O19W 0.189(8) 0.242(11) 0.386(16) 0.015(11) 0.135(10) 0.100(8) Cl2 0.172(6) 0.388(13) 0.178(6) -0.220(8) 0.125(5) -0.166(8) O23A 0.150(11) 0.091(7) 0.083(7) -0.024(6) 0.049(7) -0.023(7) O23B 0.18(2) 0.131(17) 0.21(2) -0.104(16) 0.050(18) -0.044(15) O29W 0.061(6) 0.079(7) 0.076(7) -0.050(6) 0.024(5) -0.019(6) O29A 0.083(11) 0.068(10) 0.099(13) -0.073(11) 0.032(10) -0.021(9) Cl2A 0.80(5) 0.36(2) 0.32(2) -0.29(2) 0.43(3) -0.41(3) Cl2B 0.128(6) 0.333(17) 0.215(11) -0.184(12) 0.093(7) -0.108(9) O23W 0.090(10) 0.081(10) 0.068(7) -0.044(7) 0.050(7) -0.038(8) Cl1 0.0592(13) 0.149(3) 0.0814(15) -0.0476(18) 0.0218(11) -0.0320(17) Cl1A 0.080(4) 0.075(3) 0.291(12) -0.062(5) -0.021(5) 0.013(3) Cl1B 0.048(4) 0.073(5) 0.209(13) 0.055(7) 0.020(6) -0.006(4) O2 0.0228(9) 0.0502(12) 0.0340(10) -0.0018(9) 0.0084(8) -0.0032(9) O1 0.0317(11) 0.0512(13) 0.0389(11) 0.0062(10) 0.0111(9) 0.0007(9) O3 0.0258(10) 0.0453(12) 0.0346(10) 0.0052(9) 0.0087(8) 0.0039(9) O11 0.0345(11) 0.0352(11) 0.0662(15) -0.0055(10) 0.0289(11) 0.0005(9) O12 0.0229(10) 0.0467(12) 0.0530(13) -0.0197(10) 0.0093(9) 0.0021(9) O6 0.0283(11) 0.0614(15) 0.0568(14) -0.0066(12) 0.0171(10) 0.0026(10) O5 0.0261(11) 0.0663(15) 0.0405(12) -0.0204(11) 0.0097(9) -0.0014(10) O4 0.0317(12) 0.0577(14) 0.0465(13) 0.0026(11) 0.0114(9) -0.0036(10) N3 0.0306(13) 0.0479(15) 0.0298(12) -0.0013(10) 0.0089(10) -0.0072(11) O7 0.0393(14) 0.0483(14) 0.099(2) -0.0227(14) 0.0395(14) -0.0134(11) O8 0.0295(11) 0.0454(13) 0.0684(15) -0.0164(11) 0.0257(11) -0.0125(10) O10 0.0331(12) 0.0517(14) 0.0807(18) -0.0148(13) 0.0228(12) -0.0072(11) N6 0.0251(12) 0.0416(14) 0.0379(13) 0.0087(11) 0.0082(10) 0.0001(10) N25 0.0306(13) 0.0366(13) 0.0466(14) -0.0119(11) 0.0151(11) -0.0008(10) N4 0.0222(11) 0.0445(14) 0.0307(12) -0.0015(10) 0.0079(9) -0.0067(10) O9 0.0304(12) 0.0569(14) 0.0620(15) -0.0169(12) 0.0224(11) -0.0130(10) N19 0.0249(12) 0.0348(13) 0.0510(15) -0.0040(11) 0.0160(11) -0.0075(10) N15 0.0353(14) 0.0379(13) 0.0462(15) 0.0018(11) 0.0144(11) -0.0044(11) N18 0.0244(12) 0.0417(14) 0.0426(14) -0.0095(11) 0.0136(10) -0.0104(10) N5 0.0237(12) 0.0381(13) 0.0366(13) 0.0007(10) 0.0079(10) -0.0019(10) N7 0.0265(13) 0.0502(16) 0.0416(14) 0.0122(12) 0.0017(10) -0.0019(11) N20 0.0233(12) 0.0341(13) 0.0583(16) 0.0025(12) 0.0114(11) -0.0005(10) N17 0.0340(14) 0.0501(15) 0.0352(13) -0.0044(11) 0.0149(11) -0.0134(12) N26 0.0241(12) 0.0362(13) 0.0521(15) -0.0139(11) 0.0101(11) 0.0009(10) N24 0.0269(12) 0.0465(15) 0.0397(13) -0.0062(11) 0.0065(10) -0.0004(11) N22 0.0270(13) 0.0493(16) 0.0452(15) 0.0043(12) 0.0005(11) -0.0017(11) N9 0.0300(13) 0.0633(18) 0.0337(13) -0.0056(12) 0.0067(10) -0.0019(12) C5 0.0209(12) 0.0385(15) 0.0334(14) 0.0064(11) 0.0077(10) -0.0049(11) N1 0.0313(13) 0.0425(14) 0.0385(13) 0.0046(11) 0.0096(10) -0.0014(11) N11 0.0286(13) 0.0414(14) 0.0472(15) -0.0060(11) 0.0134(11) 0.0043(11) C35 0.0233(13) 0.0296(14) 0.0486(17) -0.0077(12) 0.0117(12) -0.0039(11) N12 0.0264(12) 0.0420(14) 0.0514(15) -0.0040(12) 0.0128(11) 0.0006(11) N27 0.0342(13) 0.0301(12) 0.0452(14) 0.0009(10) 0.0149(11) 0.0043(10) N21 0.0259(13) 0.0461(15) 0.0557(17) 0.0046(13) 0.0049(11) -0.0017(11) N16 0.0424(15) 0.0513(16) 0.0413(14) -0.0060(12) 0.0191(12) -0.0124(13) C3 0.0200(12) 0.0450(16) 0.0298(13) -0.0018(12) 0.0042(10) -0.0081(11) N2 0.0315(13) 0.0463(15) 0.0346(13) 0.0061(11) 0.0104(10) -0.0053(11) C1 0.0262(14) 0.0450(16) 0.0338(14) 0.0112(12) 0.0034(11) 0.0047(12) C33 0.0205(13) 0.0388(15) 0.0496(17) -0.0094(13) 0.0107(12) -0.0049(11) C27 0.0338(16) 0.0436(16) 0.0403(16) -0.0167(13) 0.0188(13) -0.0116(13) C11 0.0307(15) 0.0349(15) 0.0489(17) -0.0081(13) 0.0121(13) 0.0056(12) N8 0.0306(14) 0.0634(19) 0.0436(15) -0.0010(13) 0.0047(11) -0.0033(13) C34 0.0261(14) 0.0342(15) 0.0498(17) -0.0135(13) 0.0098(12) -0.0040(11) N10 0.0270(12) 0.0532(16) 0.0388(13) -0.0143(12) 0.0095(10) 0.0003(11) C29 0.0282(15) 0.0322(14) 0.0540(18) -0.0073(13) 0.0160(13) -0.0049(12) C9 0.0334(16) 0.0558(19) 0.0298(14) -0.0191(13) 0.0069(12) -0.0001(14) C28 0.0319(15) 0.0352(15) 0.0510(18) -0.0143(13) 0.0190(13) -0.0076(12) C16 0.0274(14) 0.0453(17) 0.0326(14) -0.0102(12) 0.0095(11) -0.0122(12) C32 0.0222(14) 0.0512(18) 0.0473(18) 0.0019(14) -0.0010(12) -0.0016(13) C18 0.0245(14) 0.0319(14) 0.0532(18) 0.0072(13) 0.0117(12) -0.0031(11) C25 0.0399(18) 0.0462(18) 0.0505(18) -0.0047(15) 0.0264(14) -0.0107(14) C13 0.0359(16) 0.0430(17) 0.0366(15) 0.0109(13) 0.0105(12) -0.0017(13) C7 0.0288(15) 0.0562(19) 0.0334(15) 0.0090(14) 0.0063(12) -0.0022(14) C24 0.0308(15) 0.0267(13) 0.0557(18) -0.0092(13) 0.0158(13) 0.0005(11) C25B 0.0301(15) 0.0259(13) 0.0556(18) -0.0007(12) 0.0161(13) 0.0028(11) C23 0.0277(15) 0.0500(18) 0.0382(15) -0.0195(13) 0.0058(12) -0.0017(13) C12 0.0292(15) 0.0400(16) 0.0526(18) 0.0030(14) 0.0089(13) 0.0068(13) C4 0.0228(13) 0.0442(16) 0.0361(15) 0.0012(12) 0.0057(11) -0.0103(12) C2 0.0296(15) 0.0518(18) 0.0333(15) 0.0068(13) 0.0038(12) -0.0055(13) C10 0.0356(16) 0.0480(18) 0.0484(18) -0.0180(15) 0.0139(14) 0.0052(14) C36 0.0352(16) 0.0365(15) 0.0469(17) 0.0045(13) 0.0182(13) -0.0056(12) C31 0.0243(14) 0.0436(17) 0.0547(19) 0.0027(15) 0.0027(13) 0.0035(12) C8 0.0407(18) 0.070(2) 0.0340(16) -0.0046(15) 0.0100(13) -0.0087(17) C17 0.0286(14) 0.0308(14) 0.0504(17) 0.0006(12) 0.0158(13) -0.0054(11) C15 0.0312(15) 0.0511(18) 0.0283(13) -0.0054(12) 0.0082(11) -0.0114(13) C20 0.0310(16) 0.061(2) 0.0379(16) 0.0088(15) -0.0004(13) -0.0014(15) C6 0.0291(15) 0.0508(18) 0.0357(15) 0.0135(13) 0.0058(12) -0.0049(13) C21 0.0274(15) 0.059(2) 0.0343(15) -0.0132(14) 0.0037(12) -0.0037(14) C19 0.0283(15) 0.0529(19) 0.0452(17) 0.0149(15) 0.0001(13) -0.0011(14) C14 0.0396(17) 0.0527(19) 0.0319(15) 0.0095(13) 0.0105(13) -0.0085(14) C30 0.0271(15) 0.0396(17) 0.069(2) 0.0059(16) 0.0048(14) 0.0033(13) C26 0.0504(19) 0.0538(19) 0.0369(16) -0.0078(14) 0.0256(14) -0.0177(16) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 Ca1 O8 2.380(2) . ? Ca1 O4W 2.415(5) . ? Ca1 O1W 2.420(5) . ? Ca1 O3W 2.442(4) . ? Ca1 O11 2.496(2) 3_656 ? Ca1 O2W 2.515(4) . ? Ca1 O7 2.520(3) . ? Ca1 O5W 2.531(4) . ? O27A O27B 1.09(3) . ? Ca2 O9 2.360(3) . ? Ca2 O1W1 2.412(9) . ? Ca2 O3W1 2.430(8) 3_656 ? Ca2 O7W 2.435(8) . ? Ca2 O2W1 2.515(7) . ? Ca2 O6W 2.531(7) . ? Ca2 O12 2.556(3) 3_656 ? Ca2 O10 2.706(3) . ? O7W O20W 1.72(2) 2_655 ? O7W O21B 1.81(3) 2_655 ? O3W1 Ca2 2.430(8) 3_656 ? O25W Cl2A 1.878(19) 2_646 ? O24W O14A 0.67(2) 4_566 ? C11X C9X 1.512(4) . ? N1X C8X 1.496(4) . ? N1X C9X 1.512(4) . ? C10X C9X 1.517(4) . ? C8X C7XA 1.437(12) . ? C8X C7X 1.504(8) . ? O8W O8WA 0.617(16) . ? O26A O18A 1.71(4) 4_566 ? O31W O23A 1.196(13) . ? O15A Cl1A 2.13(2) 4_665 ? O21B O20W 1.35(3) . ? O21B O7W 1.81(3) 2_645 ? O18W O18A 0.97(3) . ? O18A O26A 1.71(4) 4_665 ? O14A O24W 0.67(2) 4_665 ? C1X C2X 1.367(14) . ? C1X C6X 1.384(14) . ? C1X O2X 1.396(10) . ? C2X O3X 1.350(11) . ? C2X C3X 1.377(13) . ? C3X C4X 1.418(11) . ? C4X C5X 1.372(10) . ? C4X C7X 1.557(13) . ? C5X C6X 1.407(12) . ? C7X O1X 1.430(12) . ? C1XA C2XA 1.365(14) . ? C1XA O2XA 1.372(14) . ? C1XA C6XA 1.379(18) . ? C2XA O3XA 1.354(14) . ? C2XA C3XA 1.374(12) . ? C3XA C4XA 1.422(14) . ? C4XA C5XA 1.368(13) . ? C4XA C7XA 1.49(2) . ? C5XA C6XA 1.406(15) . ? C7XA O1XA 1.448(16) . ? O20W O20A 1.33(2) . ? O20W O7W 1.72(2) 2_645 ? O23A O23B 1.53(3) . ? O29W O29A 1.22(2) . ? Cl2A O25W 1.878(19) 2_656 ? Cl1A O15A 2.13(2) 4_566 ? O2 C3 1.234(4) . ? O1 C1 1.230(4) . ? O3 C5 1.229(4) . ? O11 C33 1.226(4) . ? O11 Ca1 2.496(2) 3_656 ? O12 C35 1.228(4) . ? O12 Ca2 2.556(3) 3_656 ? O6 C11 1.222(4) . ? O5 C9 1.228(4) . ? O4 C7 1.224(4) . ? N3 C3 1.368(4) . ? N3 C2 1.448(4) . ? N3 C15 1.449(4) . ? O7 C25 1.233(5) . ? O8 C27 1.230(4) . ? O10 C31 1.223(4) . ? N6 C5 1.376(4) . ? N6 C6 1.450(4) . ? N6 C18 1.457(4) . ? N25 C33 1.369(4) . ? N25 C34 1.439(4) . ? N25 C23 1.455(4) . ? N4 C3 1.354(4) . ? N4 C4 1.441(4) . ? N4 C16 1.451(4) . ? O9 C29 1.221(4) . ? N19 C29 1.373(4) . ? N19 C28 1.445(4) . ? N19 C17 1.455(4) . ? N15 C25 1.363(4) . ? N15 C36 1.438(4) . ? N15 C13 1.450(4) . ? N18 C27 1.368(4) . ? N18 C28 1.444(4) . ? N18 C16 1.458(4) . ? N5 C5 1.360(4) . ? N5 C17 1.443(4) . ? N5 C4 1.452(4) . ? N7 C7 1.368(5) . ? N7 C19 1.454(4) . ? N7 C6 1.456(4) . ? N20 C29 1.368(4) . ? N20 C18 1.439(4) . ? N20 C30 1.449(4) . ? N17 C27 1.362(5) . ? N17 C26 1.440(4) . ? N17 C15 1.442(4) . ? N26 C35 1.363(4) . ? N26 C24 1.440(4) . ? N26 C34 1.444(4) . ? N24 C33 1.356(4) . ? N24 C32 1.451(4) . ? N24 C21 1.451(4) . ? N22 C31 1.357(5) . ? N22 C32 1.452(4) . ? N22 C20 1.456(4) . ? N9 C9 1.369(5) . ? N9 C8 1.449(5) . ? N9 C21 1.450(4) . ? N1 C1 1.367(4) . ? N1 C12 1.442(4) . ? N1 C13 1.455(4) . ? N11 C11 1.375(4) . ? N11 C24 1.449(4) . ? N11 C10 1.451(4) . ? C35 N27 1.361(4) . ? N12 C11 1.357(4) . ? N12 C25B 1.447(4) . ? N12 C12 1.450(4) . ? N27 C36 1.449(4) . ? N27 C25B 1.453(4) . ? N21 C31 1.366(4) . ? N21 C30 1.445(5) . ? N21 C19 1.454(5) . ? N16 C25 1.368(4) . ? N16 C26 1.449(5) . ? N16 C14 1.450(5) . ? N2 C1 1.360(4) . ? N2 C2 1.448(4) . ? N2 C14 1.452(4) . ? N8 C7 1.364(4) . ? N8 C20 1.445(5) . ? N8 C8 1.448(5) . ? N10 C9 1.372(5) . ? N10 C10 1.441(5) . ? N10 C23 1.449(4) . ? C16 C15 1.544(5) . ? C18 C17 1.539(5) . ? C13 C14 1.549(5) . ? C24 C25B 1.538(5) . ? C23 C21 1.536(5) . ? C20 C19 1.548(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 O8 Ca1 O4W 101.43(16) . . ? O8 Ca1 O1W 78.30(17) . . ? O4W Ca1 O1W 147.9(2) . . ? O8 Ca1 O3W 147.70(11) . . ? O4W Ca1 O3W 88.25(19) . . ? O1W Ca1 O3W 109.23(18) . . ? O8 Ca1 O11 143.88(8) . 3_656 ? O4W Ca1 O11 82.05(14) . 3_656 ? O1W Ca1 O11 80.41(17) . 3_656 ? O3W Ca1 O11 67.54(11) . 3_656 ? O8 Ca1 O2W 82.42(9) . . ? O4W Ca1 O2W 140.23(19) . . ? O1W Ca1 O2W 71.82(19) . . ? O3W Ca1 O2W 71.08(11) . . ? O11 Ca1 O2W 117.79(10) 3_656 . ? O8 Ca1 O7 79.26(8) . . ? O4W Ca1 O7 67.89(16) . . ? O1W Ca1 O7 141.22(18) . . ? O3W Ca1 O7 76.04(11) . . ? O11 Ca1 O7 133.05(8) 3_656 . ? O2W Ca1 O7 74.18(11) . . ? O8 Ca1 O5W 69.43(11) . . ? O4W Ca1 O5W 74.2(2) . . ? O1W Ca1 O5W 75.9(2) . . ? O3W Ca1 O5W 142.54(13) . . ? O11 Ca1 O5W 77.28(11) 3_656 . ? O2W Ca1 O5W 140.67(14) . . ? O7 Ca1 O5W 123.94(14) . . ? O9 Ca2 O1W1 82.4(3) . . ? O9 Ca2 O3W1 149.4(2) . 3_656 ? O1W1 Ca2 O3W1 111.8(3) . 3_656 ? O9 Ca2 O7W 93.2(2) . . ? O1W1 Ca2 O7W 148.9(4) . . ? O3W1 Ca2 O7W 87.4(3) 3_656 . ? O9 Ca2 O2W1 89.65(17) . . ? O1W1 Ca2 O2W1 71.3(3) . . ? O3W1 Ca2 O2W1 71.0(2) 3_656 . ? O7W Ca2 O2W1 139.7(3) . . ? O9 Ca2 O6W 67.14(17) . . ? O1W1 Ca2 O6W 76.2(3) . . ? O3W1 Ca2 O6W 141.1(2) 3_656 . ? O7W Ca2 O6W 73.8(2) . . ? O2W1 Ca2 O6W 142.2(2) . . ? O9 Ca2 O12 142.22(10) . 3_656 ? O1W1 Ca2 O12 76.9(3) . 3_656 ? O3W1 Ca2 O12 68.33(19) 3_656 3_656 ? O7W Ca2 O12 88.7(2) . 3_656 ? O2W1 Ca2 O12 112.55(17) . 3_656 ? O6W Ca2 O12 77.33(16) . 3_656 ? O9 Ca2 O10 77.88(9) . . ? O1W1 Ca2 O10 142.2(3) . . ? O3W1 Ca2 O10 74.77(18) 3_656 . ? O7W Ca2 O10 64.9(2) . . ? O2W1 Ca2 O10 76.57(18) . . ? O6W Ca2 O10 123.21(18) . . ? O12 Ca2 O10 135.31(9) 3_656 . ? O20W O7W O21B 44.9(10) 2_655 2_655 ? O20W O7W Ca2 154.0(8) 2_655 . ? O21B O7W Ca2 160.7(9) 2_655 . ? C8X N1X C9X 115.9(2) . . ? C7XA C8X N1X 114.0(5) . . ? C7XA C8X C7X 26.3(5) . . ? N1X C8X C7X 110.7(4) . . ? C11X C9X N1X 110.6(3) . . ? C11X C9X C10X 111.2(3) . . ? N1X C9X C10X 110.0(2) . . ? O20W O21B O7W 64.1(14) . 2_645 ? O18W O18A O26A 130(2) . 4_665 ? C2X C1X C6X 120.0(9) . . ? C2X C1X O2X 121.0(12) . . ? C6X C1X O2X 118.9(11) . . ? O3X C2X C1X 115.0(12) . . ? O3X C2X C3X 125.0(11) . . ? C1X C2X C3X 120.0(9) . . ? C2X C3X C4X 121.9(8) . . ? C5X C4X C3X 116.5(9) . . ? C5X C4X C7X 124.0(9) . . ? C3X C4X C7X 116.9(9) . . ? C4X C5X C6X 121.7(10) . . ? C1X C6X C5X 119.6(9) . . ? O1X C7X C8X 110.2(6) . . ? O1X C7X C4X 112.6(10) . . ? C8X C7X C4X 110.0(10) . . ? C2XA C1XA O2XA 120.3(16) . . ? C2XA C1XA C6XA 121.5(11) . . ? O2XA C1XA C6XA 118.2(15) . . ? O3XA C2XA C1XA 116.7(13) . . ? O3XA C2XA C3XA 123.4(11) . . ? C1XA C2XA C3XA 119.9(11) . . ? C2XA C3XA C4XA 120.0(11) . . ? C5XA C4XA C3XA 118.3(13) . . ? C5XA C4XA C7XA 119.4(13) . . ? C3XA C4XA C7XA 120.7(15) . . ? C4XA C5XA C6XA 120.7(14) . . ? C1XA C6XA C5XA 118.6(12) . . ? C8X C7XA O1XA 107.2(9) . . ? C8X C7XA C4XA 118.6(14) . . ? O1XA C7XA C4XA 103.8(15) . . ? O20A O20W O21B 171(2) . . ? O20A O20W O7W 100.6(14) . 2_645 ? O21B O20W O7W 71.0(14) . 2_645 ? O31W O23A O23B 151.1(15) . . ? C33 O11 Ca1 145.8(2) . 3_656 ? C35 O12 Ca2 142.0(2) . 3_656 ? C3 N3 C2 122.3(3) . . ? C3 N3 C15 112.0(3) . . ? C2 N3 C15 125.5(3) . . ? C25 O7 Ca1 153.2(2) . . ? C27 O8 Ca1 157.9(2) . . ? C31 O10 Ca2 154.2(2) . . ? C5 N6 C6 120.0(3) . . ? C5 N6 C18 111.3(3) . . ? C6 N6 C18 121.4(3) . . ? C33 N25 C34 122.6(3) . . ? C33 N25 C23 111.9(3) . . ? C34 N25 C23 123.9(3) . . ? C3 N4 C4 122.6(2) . . ? C3 N4 C16 112.4(2) . . ? C4 N4 C16 124.9(3) . . ? C29 O9 Ca2 157.0(2) . . ? C29 N19 C28 122.6(3) . . ? C29 N19 C17 111.5(3) . . ? C28 N19 C17 122.1(3) . . ? C25 N15 C36 122.5(3) . . ? C25 N15 C13 112.9(3) . . ? C36 N15 C13 124.4(3) . . ? C27 N18 C28 122.1(3) . . ? C27 N18 C16 111.5(3) . . ? C28 N18 C16 124.1(2) . . ? C5 N5 C17 112.5(2) . . ? C5 N5 C4 123.5(2) . . ? C17 N5 C4 123.5(3) . . ? C7 N7 C19 112.9(3) . . ? C7 N7 C6 123.5(3) . . ? C19 N7 C6 123.6(3) . . ? C29 N20 C18 112.7(3) . . ? C29 N20 C30 124.1(3) . . ? C18 N20 C30 122.7(3) . . ? C27 N17 C26 123.3(3) . . ? C27 N17 C15 112.3(3) . . ? C26 N17 C15 124.1(3) . . ? C35 N26 C24 112.6(3) . . ? C35 N26 C34 122.8(2) . . ? C24 N26 C34 124.0(3) . . ? C33 N24 C32 123.0(3) . . ? C33 N24 C21 112.6(3) . . ? C32 N24 C21 124.0(3) . . ? C31 N22 C32 121.9(3) . . ? C31 N22 C20 112.4(3) . . ? C32 N22 C20 123.5(3) . . ? C9 N9 C8 122.7(3) . . ? C9 N9 C21 111.9(3) . . ? C8 N9 C21 124.0(3) . . ? O3 C5 N5 126.3(3) . . ? O3 C5 N6 125.2(3) . . ? N5 C5 N6 108.4(3) . . ? C1 N1 C12 122.7(3) . . ? C1 N1 C13 111.8(3) . . ? C12 N1 C13 123.9(3) . . ? C11 N11 C24 111.4(3) . . ? C11 N11 C10 121.8(3) . . ? C24 N11 C10 123.5(3) . . ? O12 C35 N27 125.2(3) . . ? O12 C35 N26 126.2(3) . . ? N27 C35 N26 108.6(2) . . ? C11 N12 C25B 112.6(3) . . ? C11 N12 C12 122.9(3) . . ? C25B N12 C12 123.9(3) . . ? C35 N27 C36 122.3(3) . . ? C35 N27 C25B 111.7(3) . . ? C36 N27 C25B 122.9(3) . . ? C31 N21 C30 121.5(3) . . ? C31 N21 C19 111.7(3) . . ? C30 N21 C19 125.3(3) . . ? C25 N16 C26 123.1(3) . . ? C25 N16 C14 112.7(3) . . ? C26 N16 C14 124.1(3) . . ? O2 C3 N4 125.7(3) . . ? O2 C3 N3 125.5(3) . . ? N4 C3 N3 108.8(3) . . ? C1 N2 C2 123.6(3) . . ? C1 N2 C14 112.0(3) . . ? C2 N2 C14 123.8(3) . . ? O1 C1 N2 125.5(3) . . ? O1 C1 N1 125.1(3) . . ? N2 C1 N1 109.4(3) . . ? O11 C33 N24 126.2(3) . . ? O11 C33 N25 125.3(3) . . ? N24 C33 N25 108.5(3) . . ? O8 C27 N17 126.1(3) . . ? O8 C27 N18 124.9(3) . . ? N17 C27 N18 109.0(3) . . ? O6 C11 N12 126.3(3) . . ? O6 C11 N11 125.5(3) . . ? N12 C11 N11 108.2(3) . . ? C7 N8 C20 112.7(3) . . ? C7 N8 C8 123.7(3) . . ? C20 N8 C8 123.5(3) . . ? N25 C34 N26 113.5(2) . . ? C9 N10 C10 122.7(3) . . ? C9 N10 C23 111.9(3) . . ? C10 N10 C23 124.8(3) . . ? O9 C29 N20 126.1(3) . . ? O9 C29 N19 125.8(3) . . ? N20 C29 N19 108.1(3) . . ? O5 C9 N9 125.2(3) . . ? O5 C9 N10 126.3(3) . . ? N9 C9 N10 108.5(3) . . ? N18 C28 N19 113.6(2) . . ? N4 C16 N18 114.2(2) . . ? N4 C16 C15 103.3(2) . . ? N18 C16 C15 103.3(2) . . ? N24 C32 N22 113.2(2) . . ? N20 C18 N6 113.7(3) . . ? N20 C18 C17 103.1(2) . . ? N6 C18 C17 103.2(2) . . ? O7 C25 N15 125.6(3) . . ? O7 C25 N16 126.3(3) . . ? N15 C25 N16 108.1(3) . . ? N15 C13 N1 113.6(3) . . ? N15 C13 C14 103.1(3) . . ? N1 C13 C14 103.3(2) . . ? O4 C7 N8 126.3(3) . . ? O4 C7 N7 125.8(3) . . ? N8 C7 N7 107.9(3) . . ? N26 C24 N11 114.3(3) . . ? N26 C24 C25B 103.3(2) . . ? N11 C24 C25B 103.7(2) . . ? N12 C25B N27 114.7(3) . . ? N12 C25B C24 103.2(3) . . ? N27 C25B C24 103.6(2) . . ? N10 C23 N25 114.7(3) . . ? N10 C23 C21 103.8(3) . . ? N25 C23 C21 103.5(3) . . ? N1 C12 N12 113.9(3) . . ? N4 C4 N5 114.2(2) . . ? N3 C2 N2 114.2(2) . . ? N10 C10 N11 113.7(2) . . ? N15 C36 N27 113.8(2) . . ? O10 C31 N22 125.8(3) . . ? O10 C31 N21 125.0(3) . . ? N22 C31 N21 109.1(3) . . ? N8 C8 N9 114.5(3) . . ? N5 C17 N19 113.5(2) . . ? N5 C17 C18 103.4(2) . . ? N19 C17 C18 103.4(2) . . ? N17 C15 N3 114.4(3) . . ? N17 C15 C16 103.7(3) . . ? N3 C15 C16 103.4(2) . . ? N8 C20 N22 114.7(3) . . ? N8 C20 C19 103.7(3) . . ? N22 C20 C19 102.9(3) . . ? N6 C6 N7 113.5(2) . . ? N9 C21 N24 115.1(3) . . ? N9 C21 C23 103.7(3) . . ? N24 C21 C23 103.4(3) . . ? N7 C19 N21 114.6(3) . . ? N7 C19 C20 102.6(3) . . ? N21 C19 C20 103.7(3) . . ? N16 C14 N2 113.7(3) . . ? N16 C14 C13 103.3(3) . . ? N2 C14 C13 103.5(3) . . ? N21 C30 N20 114.2(3) . . ? N17 C26 N16 113.5(3) . . ? _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 71.43 _diffrn_measured_fraction_theta_full 0.979 _refine_diff_density_max 0.965 _refine_diff_density_min -0.983 _refine_diff_density_rms 0.093 _database_code_depnum_ccdc_archive 'CCDC 946819'