Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Detellier, Christian' 'Moser, Arvin' 'Yap, Glenn P. A.' _publ_contact_author_name 'Dr Christian Detellier' _publ_contact_author_address ; Dr Christian Detellier The Ottawa-Carleton Chemistry Institute University of Ottawa Ottawa Ontario K1N 6N5 CANADA ; data_(Na,1)+ _database_code_CSD 159035 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C96.50 H126.50 B Cl1.50 N6 Na O8' _chemical_formula_weight 1585.51 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Na' 'Na' 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M P4cc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-y, x, z' 'y, -x, z' 'x, -y, z+1/2' '-x, y, z+1/2' '-y, -x, z+1/2' 'y, x, z+1/2' _cell_length_a 18.128(2) _cell_length_b 18.128(2) _cell_length_c 29.457(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 9680(2) _cell_formula_units_Z 4 _cell_measurement_temperature 236(2) _cell_measurement_reflns_used 'reflections from 60 data frames' _cell_measurement_theta_min 1.47 _cell_measurement_theta_max 28.29 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.088 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3412 _exptl_absorpt_coefficient_mu 0.112 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.720475 _exptl_absorpt_correction_T_max 0.928075 _exptl_absorpt_process_details 'Blessing,R., Acta Cryst. (1995) A51 33-38.' _exptl_special_details ; Data collection is performed with three batch runs at phi = 0.00 deg (606 frames), at phi = 90.00 deg (435 frames), and at phi = 180 deg (230 frames) A fourth batch run is collected at phi = 0.00 deg (50 frames) to monitor crystal and diffractometer stability. Frame width = 0.30 deg in omega. Data is merged, corrected for decay (if any), and treated with multi-scan absorption corrections (if required). All symmetry-equivalent reflections are merged for centrosymmetric data. Friedel pairs are not merged for noncentrosymmetric data. ; _diffrn_ambient_temperature 236(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number '50 standard frames at start and end' _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% <1 _diffrn_reflns_number 75446 _diffrn_reflns_av_R_equivalents 0.2253 _diffrn_reflns_av_sigmaI/netI 0.2502 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.38 _diffrn_reflns_theta_max 20.82 _reflns_number_total 5085 _reflns_number_gt 3571 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1300P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0077(8) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.6(4) _refine_ls_number_reflns 5085 _refine_ls_number_parameters 525 _refine_ls_number_restraints 13 _refine_ls_R_factor_all 0.1062 _refine_ls_R_factor_gt 0.0759 _refine_ls_wR_factor_ref 0.2055 _refine_ls_wR_factor_gt 0.1901 _refine_ls_goodness_of_fit_ref 1.061 _refine_ls_restrained_S_all 1.061 _refine_ls_shift/su_max 0.016 _refine_ls_shift/su_mean 0.004 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 Na1 Na 0.5000 0.5000 0.06407(19) 0.0393(14) Uani 1 4 d S . . Na2 Na 0.0000 0.0000 0.15975(19) 0.0392(14) Uani 1 4 d S . . O1 O 0.3899(2) 0.4400(2) 0.02227(15) 0.0320(12) Uani 1 1 d . . . O2 O 0.4377(3) 0.3972(3) 0.10313(17) 0.0437(13) Uani 1 1 d . . . O3 O 0.1052(2) 0.0661(2) 0.12108(16) 0.0383(13) Uani 1 1 d . . . O4 O 0.1205(3) -0.0027(3) 0.19934(17) 0.0450(13) Uani 1 1 d . . . B1 B 0.5000 0.0000 0.1614(5) 0.052(3) Uani 1 2 d S . . N1 N 0.3244(3) 0.3777(3) 0.1324(2) 0.0395(16) Uani 1 1 d . . . N2 N 0.1920(3) 0.0842(3) 0.2313(2) 0.0454(17) Uani 1 1 d . . . C1 C 0.4412(3) 0.3103(4) -0.0235(2) 0.0318(17) Uani 1 1 d . . . H1A H 0.4255 0.2595 -0.0297 0.038 Uiso 1 1 calc R . . H1B H 0.4430 0.3173 0.0094 0.038 Uiso 1 1 calc R . . C2 C 0.3866(4) 0.3643(4) -0.0445(2) 0.0326(18) Uani 1 1 d . . . C3 C 0.3599(4) 0.3509(4) -0.0885(2) 0.0331(18) Uani 1 1 d . . . H3A H 0.3742 0.3077 -0.1038 0.040 Uiso 1 1 calc R . . C4 C 0.3123(4) 0.4010(4) -0.1100(2) 0.0352(19) Uani 1 1 d . . . C5 C 0.2950(4) 0.4665(4) -0.0867(3) 0.0355(18) Uani 1 1 d . . . H5A H 0.2630 0.5007 -0.1004 0.043 Uiso 1 1 calc R . . C6 C 0.3236(3) 0.4824(4) -0.0439(2) 0.0303(17) Uani 1 1 d . . . C7 C 0.3667(4) 0.4296(4) -0.0220(2) 0.0287(17) Uani 1 1 d . . . C8 C 0.2786(4) 0.3851(4) -0.1566(2) 0.039(2) Uani 1 1 d . . . C9 C 0.1946(5) 0.3767(5) -0.1520(3) 0.070(3) Uani 1 1 d . . . H9A H 0.1742 0.4206 -0.1379 0.105 Uiso 1 1 calc R . . H9B H 0.1835 0.3340 -0.1334 0.105 Uiso 1 1 calc R . . H9C H 0.1730 0.3703 -0.1819 0.105 Uiso 1 1 calc R . . C10 C 0.3088(5) 0.3145(4) -0.1785(3) 0.061(2) Uani 1 1 d . . . H10A H 0.2985 0.2727 -0.1589 0.092 Uiso 1 1 calc R . . H10B H 0.3617 0.3191 -0.1827 0.092 Uiso 1 1 calc R . . H10C H 0.2853 0.3070 -0.2077 0.092 Uiso 1 1 calc R . . C11 C 0.2976(5) 0.4496(5) -0.1893(3) 0.069(3) Uani 1 1 d . . . H11A H 0.2787 0.4954 -0.1769 0.104 Uiso 1 1 calc R . . H11B H 0.2752 0.4405 -0.2186 0.104 Uiso 1 1 calc R . . H11C H 0.3507 0.4531 -0.1927 0.104 Uiso 1 1 calc R . . C12 C 0.3352(4) 0.4188(4) 0.0534(2) 0.042(2) Uani 1 1 d . . . H12A H 0.3074 0.3769 0.0413 0.050 Uiso 1 1 calc R . . H12B H 0.3007 0.4598 0.0581 0.050 Uiso 1 1 calc R . . C13 C 0.3704(5) 0.3973(4) 0.0989(3) 0.0357(18) Uani 1 1 d . . . C14 C 0.2446(4) 0.3725(4) 0.1285(3) 0.051(2) Uani 1 1 d . . . H14A H 0.2275 0.4090 0.1064 0.062 Uiso 1 1 calc R . . H14B H 0.2224 0.3848 0.1579 0.062 Uiso 1 1 calc R . . C15 C 0.2174(5) 0.2943(5) 0.1136(4) 0.086(3) Uani 1 1 d . . . H15A H 0.1640 0.2942 0.1117 0.129 Uiso 1 1 calc R . . H15B H 0.2332 0.2580 0.1358 0.129 Uiso 1 1 calc R . . H15C H 0.2381 0.2822 0.0842 0.129 Uiso 1 1 calc R . . C16 C 0.3553(5) 0.3630(5) 0.1774(3) 0.053(2) Uani 1 1 d . . . H16A H 0.4030 0.3381 0.1739 0.064 Uiso 1 1 calc R . . H16B H 0.3223 0.3294 0.1937 0.064 Uiso 1 1 calc R . . C17 C 0.3661(6) 0.4318(6) 0.2054(3) 0.081(3) Uani 1 1 d . . . H17A H 0.3864 0.4186 0.2348 0.122 Uiso 1 1 calc R . . H17B H 0.3190 0.4562 0.2096 0.122 Uiso 1 1 calc R . . H17C H 0.3998 0.4648 0.1898 0.122 Uiso 1 1 calc R . . C18 C 0.0400(4) 0.1944(4) 0.0757(3) 0.044(2) Uani 1 1 d . . . H18A H 0.0504 0.2466 0.0700 0.053 Uiso 1 1 calc R . . H18B H 0.0381 0.1865 0.1085 0.053 Uiso 1 1 calc R . . C19 C 0.1002(4) 0.1462(4) 0.0545(2) 0.038(2) Uani 1 1 d . . . C20 C 0.1270(4) 0.1619(5) 0.0117(3) 0.048(2) Uani 1 1 d . . . H20A H 0.1117 0.2058 -0.0024 0.058 Uiso 1 1 calc R . . C21 C 0.1753(4) 0.1162(4) -0.0116(2) 0.041(2) Uani 1 1 d . . . C22 C 0.1972(4) 0.0513(5) 0.0108(3) 0.048(2) Uani 1 1 d . . . H22A H 0.2296 0.0188 -0.0040 0.058 Uiso 1 1 calc R . . C23 C 0.1726(4) 0.0337(4) 0.0539(2) 0.0359(19) Uani 1 1 d . . . C24 C 0.1268(4) 0.0819(4) 0.0764(2) 0.0358(19) Uani 1 1 d . . . C25 C 0.2070(5) 0.1363(5) -0.0578(3) 0.050(2) Uani 1 1 d . . . C26 C 0.2839(6) 0.1694(7) -0.0530(3) 0.111(5) Uani 1 1 d . . . H26A H 0.3160 0.1342 -0.0379 0.166 Uiso 1 1 calc R . . H26B H 0.2812 0.2143 -0.0351 0.166 Uiso 1 1 calc R . . H26C H 0.3036 0.1806 -0.0828 0.166 Uiso 1 1 calc R . . C27 C 0.1603(7) 0.1900(7) -0.0820(4) 0.127(5) Uani 1 1 d . . . H27A H 0.1110 0.1699 -0.0855 0.191 Uiso 1 1 calc R . . H27B H 0.1812 0.2000 -0.1116 0.191 Uiso 1 1 calc R . . H27C H 0.1577 0.2354 -0.0646 0.191 Uiso 1 1 calc R . . C28 C 0.2110(7) 0.0698(6) -0.0881(4) 0.104(4) Uani 1 1 d . . . H28A H 0.2418 0.0325 -0.0740 0.155 Uiso 1 1 calc R . . H28B H 0.2320 0.0838 -0.1172 0.155 Uiso 1 1 calc R . . H28C H 0.1618 0.0501 -0.0927 0.155 Uiso 1 1 calc R . . C29 C 0.1535(4) 0.1000(4) 0.1541(2) 0.0400(19) Uani 1 1 d . . . H29A H 0.1369 0.1505 0.1604 0.048 Uiso 1 1 calc R . . H29B H 0.2038 0.1025 0.1420 0.048 Uiso 1 1 calc R . . C30 C 0.1533(4) 0.0563(5) 0.1970(3) 0.040(2) Uani 1 1 d . . . C31 C 0.2319(4) 0.1549(4) 0.2296(3) 0.054(2) Uani 1 1 d . . . H31A H 0.2279 0.1795 0.2591 0.065 Uiso 1 1 calc R . . H31B H 0.2088 0.1869 0.2068 0.065 Uiso 1 1 calc R . . C32 C 0.3132(5) 0.1445(5) 0.2177(3) 0.074(3) Uani 1 1 d . . . H32A H 0.3375 0.1922 0.2169 0.112 Uiso 1 1 calc R . . H32B H 0.3173 0.1211 0.1882 0.112 Uiso 1 1 calc R . . H32C H 0.3365 0.1136 0.2405 0.112 Uiso 1 1 calc R . . C33 C 0.1897(5) 0.0459(5) 0.2750(3) 0.061(2) Uani 1 1 d . . . H33A H 0.2358 0.0553 0.2914 0.074 Uiso 1 1 calc R . . H33B H 0.1861 -0.0073 0.2697 0.074 Uiso 1 1 calc R . . C34 C 0.1265(6) 0.0697(6) 0.3036(3) 0.090(3) Uani 1 1 d . . . H34A H 0.1277 0.0433 0.3323 0.135 Uiso 1 1 calc R . . H34B H 0.0807 0.0591 0.2880 0.135 Uiso 1 1 calc R . . H34C H 0.1300 0.1223 0.3093 0.135 Uiso 1 1 calc R . . C35 C 0.4692(5) -0.0902(5) 0.2297(3) 0.064(3) Uani 1 1 d . . . H35A H 0.5204 -0.0917 0.2347 0.077 Uiso 1 1 calc R . . C36 C 0.4230(6) -0.1344(6) 0.2577(4) 0.085(3) Uani 1 1 d . . . H36A H 0.4424 -0.1642 0.2809 0.102 Uiso 1 1 calc R . . C37 C 0.3471(6) -0.1312(6) 0.2489(4) 0.084(3) Uani 1 1 d . . . H37A H 0.3147 -0.1601 0.2663 0.101 Uiso 1 1 calc R . . C38 C 0.3197(6) -0.0879(5) 0.2162(4) 0.068(3) Uani 1 1 d . . . H38A H 0.2685 -0.0870 0.2113 0.081 Uiso 1 1 calc R . . C39 C 0.3644(4) -0.0451(4) 0.1899(3) 0.047(2) Uani 1 1 d . . . H39A H 0.3429 -0.0149 0.1676 0.056 Uiso 1 1 calc R . . C40 C 0.4425(4) -0.0447(4) 0.1952(3) 0.052(2) Uani 1 1 d . . . C41 C 0.4571(5) 0.1339(5) 0.1340(3) 0.051(2) Uani 1 1 d . . . H41A H 0.4885 0.1543 0.1561 0.061 Uiso 1 1 calc R . . C42 C 0.4170(6) 0.1825(6) 0.1076(4) 0.078(3) Uani 1 1 d . . . H42A H 0.4198 0.2336 0.1130 0.093 Uiso 1 1 calc R . . C43 C 0.3734(6) 0.1561(7) 0.0739(5) 0.094(4) Uani 1 1 d . . . H43A H 0.3458 0.1885 0.0557 0.112 Uiso 1 1 calc R . . C44 C 0.3703(6) 0.0819(8) 0.0667(3) 0.089(3) Uani 1 1 d . . . H44A H 0.3411 0.0628 0.0431 0.107 Uiso 1 1 calc R . . C45 C 0.4122(5) 0.0326(5) 0.0955(3) 0.068(3) Uani 1 1 d . . . H45A H 0.4102 -0.0184 0.0901 0.082 Uiso 1 1 calc R . . C46 C 0.4552(4) 0.0589(5) 0.1307(3) 0.046(2) Uani 1 1 d . . . C47 C 0.0842(8) 0.3984(6) 1.0095(5) 0.43(10) Uiso 0.25 1 d PDU . . H47A H 0.0557 0.3846 1.0368 0.518 Uiso 0.25 1 calc PR . . Cl1 Cl 0.0416(7) 0.3873(7) 0.9552(4) 0.117(4) Uiso 0.25 1 d PDU . . Cl2 Cl 0.1684(8) 0.3505(7) 0.9983(5) 0.126(5) Uiso 0.25 1 d PDU . . Cl3 Cl 0.1185(5) 0.4906(6) 1.0053(3) 0.079(3) Uiso 0.25 1 d PDU . . N3 N 0.4430(8) 0.1199(8) 0.8823(5) 0.068(4) Uiso 0.50 1 d PU . . C48 C 0.4205(9) 0.0702(9) 0.8665(5) 0.049(4) Uiso 0.50 1 d PU . . C49 C 0.3921(8) 0.0034(9) 0.8414(5) 0.055(4) Uiso 0.50 1 d PU . . H49A H 0.3921 0.0134 0.8090 0.082 Uiso 0.50 1 calc PR . . H49B H 0.3423 -0.0075 0.8513 0.082 Uiso 0.50 1 calc PR . . H49C H 0.4238 -0.0385 0.8477 0.082 Uiso 0.50 1 calc PR . . N4 N 0.5000 0.5000 0.7987(8) 0.125(7) Uiso 1 4 d SU . . C50 C 0.0000 0.0000 0.4408(7) 0.074(5) Uiso 1 4 d SU . . C51 C 0.0000 0.0000 0.4860(5) 0.051(4) Uiso 1 4 d SU . . H51A H 0.0502 -0.0048 0.4970 0.076 Uiso 0.25 1 calc PR . . H51B H -0.0293 -0.0411 0.4970 0.076 Uiso 0.25 1 calc PR . . H51C H -0.0209 0.0459 0.4970 0.076 Uiso 0.25 1 calc PR . . N5 N 0.0000 0.0000 0.4005(9) 0.145(8) Uiso 1 4 d SU . . C52 C 0.5000 0.5000 0.8400(7) 0.079(6) Uiso 1 4 d SU . . C53 C 0.5000 0.5000 0.8864(5) 0.053(4) Uiso 1 4 d SU . . H53A H 0.5230 0.5449 0.8973 0.079 Uiso 0.25 1 calc PR . . H53B H 0.5274 0.4576 0.8973 0.079 Uiso 0.25 1 calc PR . . H53C H 0.4496 0.4975 0.8973 0.079 Uiso 0.25 1 calc PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Na1 0.0366(19) 0.0366(19) 0.045(3) 0.000 0.000 0.000 Na2 0.037(2) 0.037(2) 0.043(3) 0.000 0.000 0.000 O1 0.036(3) 0.032(3) 0.028(3) 0.001(2) 0.002(2) -0.002(2) O2 0.037(3) 0.052(3) 0.042(3) 0.011(3) -0.002(3) -0.004(2) O3 0.039(3) 0.041(3) 0.034(3) 0.003(2) -0.007(3) -0.006(2) O4 0.052(3) 0.038(3) 0.045(3) 0.007(3) -0.007(3) -0.003(3) B1 0.044(8) 0.066(9) 0.045(7) 0.000 0.000 -0.007(8) N1 0.047(4) 0.048(4) 0.024(4) 0.006(3) 0.005(3) -0.006(3) N2 0.049(4) 0.049(4) 0.039(4) 0.001(4) -0.016(4) -0.008(3) C1 0.029(4) 0.033(4) 0.033(4) 0.003(3) -0.002(4) -0.006(3) C2 0.026(4) 0.032(4) 0.039(5) 0.003(4) 0.003(4) -0.007(3) C3 0.038(5) 0.029(4) 0.032(4) 0.005(4) 0.000(4) 0.003(3) C4 0.028(4) 0.041(5) 0.036(5) 0.006(4) 0.007(4) -0.012(4) C5 0.028(4) 0.034(4) 0.044(5) 0.002(4) 0.004(4) 0.003(3) C6 0.022(4) 0.034(4) 0.035(4) -0.001(4) 0.005(4) -0.002(3) C7 0.033(4) 0.034(4) 0.019(4) 0.002(4) -0.010(3) -0.001(3) C8 0.037(5) 0.046(5) 0.035(5) 0.005(4) -0.009(4) 0.001(4) C9 0.059(6) 0.087(7) 0.064(6) -0.012(5) -0.019(5) -0.017(5) C10 0.076(6) 0.057(6) 0.051(5) -0.020(5) -0.022(5) 0.011(5) C11 0.102(7) 0.065(6) 0.042(5) 0.021(5) -0.019(5) -0.017(5) C12 0.038(5) 0.054(5) 0.034(5) 0.006(4) 0.011(4) -0.006(4) C13 0.049(5) 0.029(4) 0.030(4) 0.006(4) 0.000(5) 0.002(4) C14 0.037(5) 0.069(6) 0.048(5) 0.009(5) 0.010(4) -0.003(4) C15 0.062(6) 0.077(7) 0.120(8) 0.000(7) 0.012(6) -0.032(5) C16 0.059(6) 0.064(6) 0.036(5) 0.009(5) 0.015(4) 0.001(4) C17 0.102(8) 0.094(8) 0.048(6) -0.002(6) -0.003(6) 0.000(6) C18 0.054(5) 0.032(4) 0.047(5) 0.000(4) -0.012(4) -0.003(4) C19 0.034(4) 0.047(5) 0.033(5) -0.002(4) -0.008(4) -0.003(4) C20 0.043(5) 0.059(5) 0.043(6) 0.010(5) -0.003(4) -0.002(4) C21 0.040(5) 0.048(5) 0.034(5) 0.013(4) 0.002(4) -0.019(4) C22 0.029(4) 0.058(6) 0.058(6) 0.000(5) 0.004(4) 0.000(4) C23 0.032(4) 0.050(5) 0.026(4) 0.012(4) 0.011(4) 0.001(4) C24 0.032(4) 0.045(5) 0.030(4) 0.015(4) -0.002(4) -0.004(4) C25 0.059(6) 0.056(5) 0.035(5) 0.011(5) -0.004(4) -0.003(4) C26 0.079(8) 0.181(12) 0.071(7) 0.002(8) 0.014(6) -0.084(8) C27 0.167(12) 0.157(12) 0.058(7) 0.063(8) 0.035(8) 0.076(10) C28 0.149(11) 0.103(9) 0.059(7) 0.026(7) 0.028(7) -0.009(8) C29 0.036(4) 0.045(5) 0.039(5) -0.006(4) -0.009(4) -0.007(4) C30 0.043(5) 0.046(5) 0.032(5) 0.003(4) -0.002(4) -0.001(4) C31 0.048(5) 0.063(6) 0.052(5) -0.011(5) -0.005(4) -0.009(5) C32 0.065(7) 0.063(6) 0.095(8) -0.017(5) 0.013(6) -0.025(5) C33 0.073(6) 0.065(6) 0.045(5) 0.012(5) -0.009(5) -0.004(5) C34 0.125(9) 0.098(8) 0.047(6) 0.013(6) 0.026(6) 0.017(7) C35 0.058(6) 0.075(6) 0.058(6) 0.017(6) 0.012(5) 0.013(5) C36 0.075(8) 0.092(8) 0.089(8) 0.033(7) 0.008(6) 0.002(6) C37 0.072(8) 0.080(8) 0.100(9) 0.019(7) 0.013(7) -0.020(6) C38 0.064(7) 0.060(6) 0.078(7) -0.001(6) 0.017(6) -0.005(6) C39 0.038(5) 0.038(5) 0.065(6) -0.005(4) 0.014(5) -0.009(4) C40 0.053(6) 0.037(5) 0.065(6) -0.010(5) 0.002(5) 0.002(4) C41 0.055(6) 0.048(6) 0.050(5) -0.001(5) -0.007(5) 0.011(5) C42 0.091(8) 0.069(7) 0.073(7) -0.005(6) -0.005(7) -0.012(6) C43 0.091(9) 0.066(8) 0.123(11) 0.046(8) 0.032(8) 0.009(6) C44 0.070(7) 0.137(12) 0.060(7) 0.020(7) -0.005(6) -0.019(7) C45 0.049(5) 0.068(6) 0.088(7) 0.022(6) 0.000(6) -0.014(5) C46 0.029(5) 0.064(6) 0.045(5) -0.001(5) -0.006(4) -0.004(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Na1 O2 2.464(5) 3_655 ? Na1 O2 2.464(5) 2_665 ? Na1 O2 2.464(5) 4_565 ? Na1 O2 2.464(5) . ? Na1 O1 2.584(5) . ? Na1 O1 2.584(5) 3_655 ? Na1 O1 2.584(5) 4_565 ? Na1 O1 2.584(5) 2_665 ? Na2 O4 2.477(5) 4 ? Na2 O4 2.477(5) . ? Na2 O4 2.477(5) 3 ? Na2 O4 2.477(5) 2 ? Na2 O3 2.524(5) 2 ? Na2 O3 2.524(5) . ? Na2 O3 2.524(5) 4 ? Na2 O3 2.524(5) 3 ? O1 C7 1.383(8) . ? O1 C12 1.406(8) . ? O2 C13 1.225(8) . ? O3 C24 1.402(8) . ? O3 C29 1.447(8) . ? O4 C30 1.227(8) . ? B1 C46 1.618(11) 2_655 ? B1 C46 1.618(11) . ? B1 C40 1.653(12) 2_655 ? B1 C40 1.653(12) . ? N1 C13 1.341(9) . ? N1 C14 1.454(9) . ? N1 C16 1.463(10) . ? N2 C30 1.330(9) . ? N2 C33 1.464(10) . ? N2 C31 1.473(10) . ? C1 C2 1.522(9) . ? C1 C6 1.529(9) 3_655 ? C2 C7 1.404(9) . ? C2 C3 1.406(10) . ? C3 C4 1.404(10) . ? C4 C5 1.407(9) . ? C4 C8 1.530(10) . ? C5 C6 1.392(10) . ? C6 C7 1.394(9) . ? C6 C1 1.529(9) 4_565 ? C8 C10 1.535(10) . ? C8 C9 1.537(11) . ? C8 C11 1.552(10) . ? C12 C13 1.534(10) . ? C14 C15 1.564(11) . ? C16 C17 1.507(12) . ? C18 C19 1.529(10) . ? C18 C23 1.535(10) 3 ? C19 C20 1.383(10) . ? C19 C24 1.418(10) . ? C20 C21 1.386(10) . ? C21 C22 1.406(10) . ? C21 C25 1.522(11) . ? C22 C23 1.382(10) . ? C23 C24 1.375(10) . ? C23 C18 1.535(10) 4 ? C25 C27 1.473(12) . ? C25 C28 1.502(13) . ? C25 C26 1.525(12) . ? C29 C30 1.491(10) . ? C31 C32 1.527(11) . ? C33 C34 1.486(12) . ? C35 C40 1.396(11) . ? C35 C36 1.423(12) . ? C36 C37 1.402(14) . ? C37 C38 1.337(13) . ? C38 C39 1.363(11) . ? C39 C40 1.425(11) . ? C41 C46 1.364(10) . ? C41 C42 1.382(12) . ? C42 C43 1.357(15) . ? C43 C44 1.362(15) . ? C44 C45 1.447(14) . ? C45 C46 1.382(11) . ? C47 Cl2 1.787(5) . ? C47 Cl3 1.787(5) . ? C47 Cl1 1.788(5) . ? N3 C48 1.093(18) . ? C48 C49 1.51(2) . ? N4 C52 1.22(3) . ? C50 N5 1.18(3) . ? C50 C51 1.33(2) . ? C52 C53 1.37(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 O2 Na1 O2 77.41(14) 3_655 2_665 ? O2 Na1 O2 124.3(3) 3_655 4_565 ? O2 Na1 O2 77.41(14) 2_665 4_565 ? O2 Na1 O2 77.41(14) 3_655 . ? O2 Na1 O2 124.3(3) 2_665 . ? O2 Na1 O2 77.41(14) 4_565 . ? O2 Na1 O1 127.82(15) 3_655 . ? O2 Na1 O1 153.46(15) 2_665 . ? O2 Na1 O1 80.31(15) 4_565 . ? O2 Na1 O1 63.28(15) . . ? O2 Na1 O1 63.28(15) 3_655 3_655 ? O2 Na1 O1 127.82(15) 2_665 3_655 ? O2 Na1 O1 153.46(15) 4_565 3_655 ? O2 Na1 O1 80.31(15) . 3_655 ? O1 Na1 O1 76.88(12) . 3_655 ? O2 Na1 O1 153.46(15) 3_655 4_565 ? O2 Na1 O1 80.31(15) 2_665 4_565 ? O2 Na1 O1 63.28(15) 4_565 4_565 ? O2 Na1 O1 127.82(15) . 4_565 ? O1 Na1 O1 76.88(12) . 4_565 ? O1 Na1 O1 123.1(3) 3_655 4_565 ? O2 Na1 O1 80.31(15) 3_655 2_665 ? O2 Na1 O1 63.28(15) 2_665 2_665 ? O2 Na1 O1 127.82(15) 4_565 2_665 ? O2 Na1 O1 153.46(15) . 2_665 ? O1 Na1 O1 123.1(3) . 2_665 ? O1 Na1 O1 76.88(12) 3_655 2_665 ? O1 Na1 O1 76.88(12) 4_565 2_665 ? O4 Na2 O4 77.19(14) 4 . ? O4 Na2 O4 123.8(3) 4 3 ? O4 Na2 O4 77.19(14) . 3 ? O4 Na2 O4 77.19(14) 4 2 ? O4 Na2 O4 123.8(3) . 2 ? O4 Na2 O4 77.19(14) 3 2 ? O4 Na2 O3 77.20(16) 4 2 ? O4 Na2 O3 150.37(16) . 2 ? O4 Na2 O3 130.29(16) 3 2 ? O4 Na2 O3 63.63(15) 2 2 ? O4 Na2 O3 130.29(16) 4 . ? O4 Na2 O3 63.63(15) . . ? O4 Na2 O3 77.20(16) 3 . ? O4 Na2 O3 150.37(16) 2 . ? O3 Na2 O3 126.3(3) 2 . ? O4 Na2 O3 63.63(15) 4 4 ? O4 Na2 O3 77.20(16) . 4 ? O4 Na2 O3 150.37(16) 3 4 ? O4 Na2 O3 130.29(16) 2 4 ? O3 Na2 O3 78.25(12) 2 4 ? O3 Na2 O3 78.25(12) . 4 ? O4 Na2 O3 150.37(16) 4 3 ? O4 Na2 O3 130.29(16) . 3 ? O4 Na2 O3 63.63(15) 3 3 ? O4 Na2 O3 77.20(16) 2 3 ? O3 Na2 O3 78.25(12) 2 3 ? O3 Na2 O3 78.25(12) . 3 ? O3 Na2 O3 126.3(3) 4 3 ? C7 O1 C12 111.3(5) . . ? C7 O1 Na1 137.9(4) . . ? C12 O1 Na1 110.4(4) . . ? C13 O2 Na1 114.1(4) . . ? C24 O3 C29 112.0(5) . . ? C24 O3 Na2 137.0(4) . . ? C29 O3 Na2 110.9(4) . . ? C30 O4 Na2 112.6(5) . . ? C46 B1 C46 112.0(10) 2_655 . ? C46 B1 C40 110.1(4) 2_655 2_655 ? C46 B1 C40 109.2(4) . 2_655 ? C46 B1 C40 109.2(4) 2_655 . ? C46 B1 C40 110.1(4) . . ? C40 B1 C40 106.1(10) 2_655 . ? C13 N1 C14 125.3(6) . . ? C13 N1 C16 118.6(6) . . ? C14 N1 C16 116.1(6) . . ? C30 N2 C33 118.3(6) . . ? C30 N2 C31 124.3(7) . . ? C33 N2 C31 117.3(6) . . ? C2 C1 C6 109.2(5) . 3_655 ? C7 C2 C3 119.5(6) . . ? C7 C2 C1 121.2(6) . . ? C3 C2 C1 119.1(6) . . ? C4 C3 C2 121.1(7) . . ? C3 C4 C5 117.6(7) . . ? C3 C4 C8 121.9(7) . . ? C5 C4 C8 120.5(7) . . ? C6 C5 C4 122.2(7) . . ? C7 C6 C5 119.1(6) . . ? C7 C6 C1 121.9(6) . 4_565 ? C5 C6 C1 118.9(6) . 4_565 ? O1 C7 C6 120.9(6) . . ? O1 C7 C2 118.8(6) . . ? C6 C7 C2 120.3(6) . . ? C4 C8 C10 113.1(6) . . ? C4 C8 C9 109.6(6) . . ? C10 C8 C9 107.9(6) . . ? C4 C8 C11 109.0(6) . . ? C10 C8 C11 106.8(6) . . ? C9 C8 C11 110.4(7) . . ? O1 C12 C13 110.2(6) . . ? O2 C13 N1 122.9(7) . . ? O2 C13 C12 120.3(7) . . ? N1 C13 C12 116.8(7) . . ? N1 C14 C15 113.3(6) . . ? N1 C16 C17 113.2(7) . . ? C19 C18 C23 107.7(6) . 3 ? C20 C19 C24 117.7(7) . . ? C20 C19 C18 120.4(7) . . ? C24 C19 C18 121.9(7) . . ? C19 C20 C21 123.4(7) . . ? C20 C21 C22 116.5(7) . . ? C20 C21 C25 122.5(7) . . ? C22 C21 C25 120.9(7) . . ? C23 C22 C21 122.2(7) . . ? C24 C23 C22 119.5(7) . . ? C24 C23 C18 120.4(6) . 4 ? C22 C23 C18 120.1(7) . 4 ? C23 C24 O3 119.6(6) . . ? C23 C24 C19 120.5(7) . . ? O3 C24 C19 119.9(7) . . ? C27 C25 C28 105.8(8) . . ? C27 C25 C26 108.2(9) . . ? C28 C25 C26 109.1(9) . . ? C27 C25 C21 111.9(8) . . ? C28 C25 C21 111.0(7) . . ? C26 C25 C21 110.8(7) . . ? O3 C29 C30 110.0(6) . . ? O4 C30 N2 123.0(7) . . ? O4 C30 C29 120.9(7) . . ? N2 C30 C29 116.1(7) . . ? N2 C31 C32 112.0(7) . . ? N2 C33 C34 112.5(7) . . ? C40 C35 C36 123.4(9) . . ? C37 C36 C35 116.6(9) . . ? C38 C37 C36 121.4(10) . . ? C37 C38 C39 121.6(10) . . ? C38 C39 C40 122.1(8) . . ? C35 C40 C39 114.9(8) . . ? C35 C40 B1 120.6(7) . . ? C39 C40 B1 124.3(7) . . ? C46 C41 C42 125.6(9) . . ? C43 C42 C41 119.5(10) . . ? C42 C43 C44 119.1(11) . . ? C43 C44 C45 119.8(11) . . ? C46 C45 C44 121.5(9) . . ? C41 C46 C45 114.3(8) . . ? C41 C46 B1 127.3(7) . . ? C45 C46 B1 118.4(8) . . ? Cl2 C47 Cl3 98.3(8) . . ? Cl2 C47 Cl1 98.6(9) . . ? Cl3 C47 Cl1 101.2(8) . . ? N3 C48 C49 175.6(18) . . ? N5 C50 C51 180.000(4) . . ? N4 C52 C53 180.000(9) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 20.82 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.886 _refine_diff_density_min -0.281 _refine_diff_density_rms 0.081 #===END data_(MeCN,1) _database_code_CSD 159036 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C72 H106 N6 O8' _chemical_formula_weight 1183.63 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 11.380(2) _cell_length_b 26.899(5) _cell_length_c 11.468(2) _cell_angle_alpha 90.00 _cell_angle_beta 96.382(3) _cell_angle_gamma 90.00 _cell_volume 3489(1) _cell_formula_units_Z 2 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used 'reflections from 60 data frames' _cell_measurement_theta_min 1.47 _cell_measurement_theta_max 28.29 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.127 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1288 _exptl_absorpt_coefficient_mu 0.073 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.615225 _exptl_absorpt_correction_T_max 0.928075 _exptl_absorpt_process_details 'Blessing,R., Acta Cryst. (1995) A51 33-38.' _exptl_special_details ; Data collection is performed with three batch runs at phi = 0.00 deg (606 frames), at phi = 90.00 deg (435 frames), and at phi = 180 deg (230 frames) A fourth batch run is collected at phi = 0.00 deg (50 frames) to monitor crystal and diffractometer stability. Frame width = 0.30 deg in omega. Data is merged, corrected for decay (if any), and treated with multi-scan absorption corrections (if required). All symmetry-equivalent reflections are merged for centrosymmetric data. Friedel pairs are not merged for noncentrosymmetric data. ; _diffrn_ambient_temperature 203(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number '50 standard frames at start and end' _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% <1 _diffrn_reflns_number 27031 _diffrn_reflns_av_R_equivalents 0.0420 _diffrn_reflns_av_sigmaI/netI 0.1010 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.79 _diffrn_reflns_theta_max 23.25 _reflns_number_total 9863 _reflns_number_gt 7643 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.017(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 1(2) _refine_ls_number_reflns 9863 _refine_ls_number_parameters 814 _refine_ls_number_restraints 968 _refine_ls_R_factor_all 0.1258 _refine_ls_R_factor_gt 0.1090 _refine_ls_wR_factor_ref 0.2963 _refine_ls_wR_factor_gt 0.2855 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.059 _refine_ls_shift/su_max 0.018 _refine_ls_shift/su_mean 0.005 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 N1 N 1.1376(7) 0.5686(3) 0.8746(8) 0.125(3) Uani 1 1 d DU . . N2 N 1.0656(8) 0.6416(4) 0.3883(7) 0.141(3) Uani 1 1 d DU . . N3 N 0.5731(10) 0.5639(3) 0.3329(6) 0.137(4) Uani 1 1 d DU . . N4 N 0.6301(10) 0.4878(2) 0.8542(8) 0.126(3) Uani 1 1 d U . . N5 N 0.5919(12) 0.8842(5) 0.8749(14) 0.179(5) Uani 1 1 d U . . N6 N 0.8597(14) 0.4888(5) 0.6773(14) 0.182(6) Uani 1 1 d U . . O1 O 0.9201(4) 0.66757(16) 0.8470(4) 0.0634(11) Uani 1 1 d U A . O2 O 1.1346(7) 0.6444(3) 0.7708(8) 0.083(2) Uani 0.648(12) 1 d PU A 1 O2' O 0.9443(13) 0.5688(5) 0.9585(15) 0.083(2) Uani 0.35 1 d PU A 2 O3 O 0.8873(4) 0.70689(13) 0.5833(3) 0.0522(10) Uani 1 1 d U . . O4 O 0.8652(7) 0.6702(3) 0.3538(6) 0.076(2) Uani 0.639(10) 1 d PU B 1 O4' O 1.1117(11) 0.6607(6) 0.5975(11) 0.076(2) Uani 0.36 1 d PU B 2 O5 O 0.6241(3) 0.66458(13) 0.5520(3) 0.0500(9) Uani 1 1 d U . . O6 O 0.5422(11) 0.5676(3) 0.5282(7) 0.097(3) Uani 0.584(10) 1 d PU C 1 O6' O 0.6837(16) 0.6476(4) 0.3334(10) 0.097(3) Uani 0.42 1 d PU C 2 O7 O 0.6570(3) 0.62259(12) 0.8221(3) 0.0453(9) Uani 1 1 d U . . O8 O 0.7780(8) 0.5491(3) 0.9512(8) 0.080(2) Uani 0.604(10) 1 d PU D 1 O8' O 0.5523(12) 0.5446(4) 0.6981(11) 0.080(2) Uani 0.40 1 d PU D 2 C1 C 0.8510(4) 0.7084(2) 1.0137(4) 0.0451(12) Uani 1 1 d U . . C2 C 0.8553(5) 0.7499(2) 1.0843(5) 0.0537(14) Uani 1 1 d U . . H2A H 0.8148 0.7491 1.1514 0.064 Uiso 1 1 calc R . . C3 C 0.9172(5) 0.7935(3) 1.0613(5) 0.0621(16) Uani 1 1 d U . . C4 C 0.9728(5) 0.7934(3) 0.9608(6) 0.0630(17) Uani 1 1 d U . . H4A H 1.0119 0.8224 0.9405 0.076 Uiso 1 1 calc R . . C5 C 0.9732(5) 0.7519(2) 0.8876(5) 0.0544(14) Uani 1 1 d U . . C6 C 0.9149(5) 0.7094(2) 0.9164(5) 0.0497(13) Uani 1 1 d U . . C7 C 0.9274(7) 0.8364(3) 1.1501(8) 0.092(2) Uani 1 1 d U . . C8 C 0.8076(12) 0.8499(4) 1.1771(14) 0.152(5) Uani 1 1 d U . . H8A H 0.7642 0.8651 1.1088 0.228 Uiso 1 1 calc R . . H8B H 0.8135 0.8731 1.2421 0.228 Uiso 1 1 calc R . . H8C H 0.7665 0.8202 1.1982 0.228 Uiso 1 1 calc R . . C9 C 0.9702(16) 0.8100(7) 1.2809(10) 0.182(5) Uani 1 1 d U . . H9A H 0.9098 0.7870 1.3004 0.274 Uiso 1 1 calc R . . H9B H 0.9816 0.8356 1.3406 0.274 Uiso 1 1 calc R . . H9C H 1.0439 0.7923 1.2770 0.274 Uiso 1 1 calc R . . C10 C 1.0204(14) 0.8676(5) 1.1406(13) 0.182(7) Uani 1 1 d U . . H10A H 1.0099 0.8841 1.0649 0.274 Uiso 1 1 calc R . . H10B H 1.0933 0.8486 1.1475 0.274 Uiso 1 1 calc R . . H10C H 1.0241 0.8922 1.2026 0.274 Uiso 1 1 calc R . . C11 C 0.9898(10) 0.6314(3) 0.8823(7) 0.097(2) Uani 1 1 d U . . H11A H 0.9402 0.6015 0.8785 0.116 Uiso 1 1 calc R A 1 H11B H 1.0139 0.6375 0.9658 0.116 Uiso 1 1 calc R A 1 C12 C 1.0887(10) 0.6183(4) 0.8362(9) 0.068(2) Uani 0.648(12) 1 d PU A 1 C12' C 1.0329(19) 0.5864(7) 0.9149(17) 0.068(2) Uani 0.35 1 d PU A 2 C13 C 1.1003(15) 0.5264(6) 0.9302(19) 0.192(7) Uani 1 1 d DU A . H13A H 1.0149 0.5282 0.9344 0.230 Uiso 1 1 calc R . . H13B H 1.1164 0.4967 0.8850 0.230 Uiso 1 1 calc R . . C14 C 1.158(3) 0.5230(12) 1.040(2) 0.324(18) Uani 1 1 d DU . . H14A H 1.1305 0.4940 1.0792 0.486 Uiso 1 1 calc R A . H14B H 1.1427 0.5526 1.0842 0.486 Uiso 1 1 calc R . . H14C H 1.2424 0.5201 1.0354 0.486 Uiso 1 1 calc R . . C15 C 1.2456(9) 0.5653(4) 0.8315(11) 0.111(3) Uani 1 1 d DU A . H15A H 1.3000 0.5456 0.8851 0.134 Uiso 1 1 calc R . . H15B H 1.2793 0.5987 0.8262 0.134 Uiso 1 1 calc R . . C16 C 1.2331(15) 0.5435(6) 0.7217(13) 0.168(5) Uani 1 1 d DU . . H16A H 1.3095 0.5419 0.6919 0.251 Uiso 1 1 calc R A . H16B H 1.1791 0.5630 0.6687 0.251 Uiso 1 1 calc R . . H16C H 1.2019 0.5101 0.7274 0.251 Uiso 1 1 calc R . . C17 C 1.0278(5) 0.7573(2) 0.7714(5) 0.0555(14) Uani 1 1 d U B . H17A H 1.0458 0.7243 0.7422 0.067 Uiso 1 1 calc R . . H17B H 1.1022 0.7759 0.7856 0.067 Uiso 1 1 calc R . . C18 C 0.9462(5) 0.7839(2) 0.6799(6) 0.0559(14) Uani 1 1 d U . . C19 C 0.9415(6) 0.8356(3) 0.6820(7) 0.0684(17) Uani 1 1 d U B . H19A H 0.9938 0.8531 0.7364 0.082 Uiso 1 1 calc R . . C20 C 0.8607(7) 0.8617(2) 0.6051(7) 0.0727(18) Uani 1 1 d U . . C21 C 0.7825(7) 0.8353(2) 0.5257(6) 0.0647(16) Uani 1 1 d U B . H21A H 0.7267 0.8525 0.4741 0.078 Uiso 1 1 calc R . . C22 C 0.7867(5) 0.7826(2) 0.5224(5) 0.0474(12) Uani 1 1 d U . . C23 C 0.8744(5) 0.7582(2) 0.5935(5) 0.0488(13) Uani 1 1 d U B . C24 C 0.8615(9) 0.9190(3) 0.6051(9) 0.103(3) Uani 1 1 d U B . C25 C 0.885(3) 0.9384(4) 0.7257(13) 0.246(9) Uani 1 1 d U . . H25A H 0.8843 0.9745 0.7237 0.369 Uiso 1 1 calc R B . H25B H 0.9613 0.9269 0.7607 0.369 Uiso 1 1 calc R . . H25C H 0.8239 0.9268 0.7719 0.369 Uiso 1 1 calc R . . C26 C 0.9575(16) 0.9374(3) 0.5335(15) 0.198(8) Uani 1 1 d U . . H26A H 0.9401 0.9264 0.4529 0.298 Uiso 1 1 calc R B . H26B H 1.0333 0.9241 0.5661 0.298 Uiso 1 1 calc R . . H26C H 0.9602 0.9734 0.5358 0.298 Uiso 1 1 calc R . . C27 C 0.7432(14) 0.9378(3) 0.571(3) 0.257(10) Uani 1 1 d U . . H27A H 0.7142 0.9252 0.4943 0.385 Uiso 1 1 calc R B . H27B H 0.7451 0.9738 0.5692 0.385 Uiso 1 1 calc R . . H27C H 0.6913 0.9270 0.6280 0.385 Uiso 1 1 calc R . . C28 C 0.9856(10) 0.6949(3) 0.5292(9) 0.053(2) Uani 0.639(10) 1 d PU B 1 H28A H 1.0368 0.6735 0.5819 0.063 Uiso 0.639(10) 1 calc PR B 1 H28B H 1.0295 0.7255 0.5176 0.063 Uiso 0.639(10) 1 calc PR B 1 C29 C 0.9595(11) 0.6685(4) 0.4099(9) 0.067(2) Uani 0.639(10) 1 d PU B 1 C28' C 0.9228(19) 0.6868(7) 0.4898(18) 0.053(2) Uani 0.36 1 d PU B 2 H28C H 0.9240 0.7130 0.4305 0.063 Uiso 0.361(10) 1 calc PR B 2 H28D H 0.8628 0.6626 0.4594 0.063 Uiso 0.361(10) 1 calc PR B 2 C29' C 1.0387(18) 0.6615(7) 0.4994(16) 0.067(2) Uani 0.36 1 d PU B 2 C30 C 1.1859(17) 0.6129(10) 0.4333(14) 0.240(10) Uani 1 1 d DU B . H30A H 1.2014 0.6147 0.5190 0.288 Uiso 1 1 calc R . . H30B H 1.1806 0.5779 0.4100 0.288 Uiso 1 1 calc R . . C31 C 1.2734(16) 0.6362(11) 0.382(3) 0.294(14) Uani 1 1 d DU . . H31A H 1.3491 0.6213 0.4094 0.440 Uiso 1 1 calc R B . H31B H 1.2748 0.6712 0.4027 0.440 Uiso 1 1 calc R . . H31C H 1.2587 0.6328 0.2975 0.440 Uiso 1 1 calc R . . C32 C 1.0327(15) 0.6253(5) 0.2527(10) 0.162(6) Uani 1 1 d DU B . H32A H 0.9852 0.6510 0.2089 0.195 Uiso 1 1 calc R . . H32B H 1.1044 0.6195 0.2146 0.195 Uiso 1 1 calc R . . C33 C 0.967(3) 0.5808(7) 0.2586(15) 0.274(13) Uani 1 1 d DU . . H33A H 0.9420 0.5691 0.1799 0.412 Uiso 1 1 calc R B . H33B H 0.8982 0.5872 0.2991 0.412 Uiso 1 1 calc R . . H33C H 1.0162 0.5558 0.3011 0.412 Uiso 1 1 calc R . . C34 C 0.6919(6) 0.7556(2) 0.4395(5) 0.0521(13) Uani 1 1 d U B . H34A H 0.6746 0.7747 0.3669 0.063 Uiso 1 1 calc R . . H34B H 0.7211 0.7228 0.4193 0.063 Uiso 1 1 calc R . . C35 C 0.5814(5) 0.7499(2) 0.4986(4) 0.0485(13) Uani 1 1 d U . . C36 C 0.5037(6) 0.7895(2) 0.4981(5) 0.0634(16) Uani 1 1 d U B . H36A H 0.5192 0.8185 0.4568 0.076 Uiso 1 1 calc R . . C37 C 0.4039(6) 0.7876(3) 0.5568(5) 0.0657(17) Uani 1 1 d U . . C38 C 0.3830(5) 0.7456(2) 0.6181(5) 0.0562(15) Uani 1 1 d U B . H38A H 0.3154 0.7445 0.6582 0.067 Uiso 1 1 calc R . . C39 C 0.4575(4) 0.7043(2) 0.6238(4) 0.0400(11) Uani 1 1 d U . . C40 C 0.5537(5) 0.7062(2) 0.5571(4) 0.0409(11) Uani 1 1 d U B . C41 C 0.3120(10) 0.8324(4) 0.5480(9) 0.119(3) Uani 1 1 d U B . C42 C 0.3361(15) 0.8687(5) 0.4667(13) 0.192(7) Uani 1 1 d U . . H42A H 0.4107 0.8847 0.4930 0.288 Uiso 1 1 calc R B . H42B H 0.2733 0.8932 0.4597 0.288 Uiso 1 1 calc R . . H42C H 0.3410 0.8532 0.3910 0.288 Uiso 1 1 calc R . . C43 C 0.2963(13) 0.8486(4) 0.6684(10) 0.137(4) Uani 1 1 d U . . H43A H 0.3680 0.8646 0.7034 0.205 Uiso 1 1 calc R B . H43B H 0.2797 0.8198 0.7151 0.205 Uiso 1 1 calc R . . H43C H 0.2308 0.8718 0.6659 0.205 Uiso 1 1 calc R . . C44 C 0.1878(11) 0.8077(6) 0.4995(11) 0.160(4) Uani 1 1 d U . . H44A H 0.1266 0.8329 0.4930 0.240 Uiso 1 1 calc R B . H44B H 0.1681 0.7820 0.5533 0.240 Uiso 1 1 calc R . . H44C H 0.1938 0.7932 0.4229 0.240 Uiso 1 1 calc R . . C45 C 0.6105(11) 0.6402(4) 0.4371(10) 0.059(2) Uani 0.584(10) 1 d PU C 1 H45A H 0.6863 0.6415 0.4041 0.071 Uiso 0.584(10) 1 calc PR C 1 H45B H 0.5527 0.6589 0.3845 0.071 Uiso 0.584(10) 1 calc PR C 1 C46 C 0.5709(12) 0.5867(4) 0.4399(10) 0.068(2) Uani 0.584(10) 1 d PU C 1 C45' C 0.5706(16) 0.6288(6) 0.4902(13) 0.059(2) Uani 0.42 1 d PU C 2 H45C H 0.4867 0.6375 0.4744 0.071 Uiso 0.416(10) 1 calc PR C 2 H45D H 0.5755 0.5986 0.5384 0.071 Uiso 0.416(10) 1 calc PR C 2 C46' C 0.6157(17) 0.6164(7) 0.3747(14) 0.068(2) Uani 0.42 1 d PU C 2 C47 C 0.6001(18) 0.5766(6) 0.2205(11) 0.204(7) Uani 1 1 d DU C . H47A H 0.6483 0.5505 0.1895 0.245 Uiso 1 1 calc R . . H47B H 0.6441 0.6079 0.2227 0.245 Uiso 1 1 calc R . . C48 C 0.474(2) 0.5822(13) 0.1385(14) 0.316(15) Uani 1 1 d DU . . H48A H 0.4878 0.5905 0.0590 0.474 Uiso 1 1 calc R C . H48B H 0.4274 0.6083 0.1697 0.474 Uiso 1 1 calc R . . H48C H 0.4306 0.5510 0.1382 0.474 Uiso 1 1 calc R . . C49 C 0.528(2) 0.5163(6) 0.3464(13) 0.218(8) Uani 1 1 d DU C . H49A H 0.4826 0.5051 0.2733 0.262 Uiso 1 1 calc R . . H49B H 0.4753 0.5160 0.4088 0.262 Uiso 1 1 calc R . . C50 C 0.640(3) 0.4806(10) 0.380(2) 0.355(18) Uani 1 1 d DU . . H50A H 0.6132 0.4477 0.3992 0.533 Uiso 1 1 calc R C . H50B H 0.6887 0.4943 0.4476 0.533 Uiso 1 1 calc R . . H50C H 0.6865 0.4785 0.3143 0.533 Uiso 1 1 calc R . . C51 C 0.4381(5) 0.6609(2) 0.7024(5) 0.0446(12) Uani 1 1 d U B . H51A H 0.4800 0.6317 0.6770 0.054 Uiso 1 1 calc R . . H51B H 0.3536 0.6530 0.6965 0.054 Uiso 1 1 calc R . . C52 C 0.4832(4) 0.67318(19) 0.8296(4) 0.0397(11) Uani 1 1 d U . . C53 C 0.4200(5) 0.7043(2) 0.8953(5) 0.0523(14) Uani 1 1 d U B . H53A H 0.3451 0.7151 0.8620 0.063 Uiso 1 1 calc R . . C54 C 0.4593(6) 0.7204(3) 1.0054(6) 0.0673(18) Uani 1 1 d U . . C55 C 0.5744(6) 0.7061(2) 1.0508(5) 0.0580(15) Uani 1 1 d U B . H55A H 0.6056 0.7177 1.1251 0.070 Uiso 1 1 calc R . . C56 C 0.6424(5) 0.6756(2) 0.9892(4) 0.0435(12) Uani 1 1 d U . . C57 C 0.5937(4) 0.65695(18) 0.8810(4) 0.0368(11) Uani 1 1 d U B . C58 C 0.3805(8) 0.7528(5) 1.0761(7) 0.113(3) Uani 1 1 d U B . C59 C 0.3327(13) 0.7968(6) 1.0026(11) 0.164(5) Uani 1 1 d U . . H59A H 0.2836 0.8170 1.0478 0.246 Uiso 1 1 calc R B . H59B H 0.2858 0.7848 0.9324 0.246 Uiso 1 1 calc R . . H59C H 0.3980 0.8166 0.9807 0.246 Uiso 1 1 calc R . . C60 C 0.2574(12) 0.7254(7) 1.0758(14) 0.181(5) Uani 1 1 d U . . H60A H 0.2679 0.6953 1.1223 0.272 Uiso 1 1 calc R B . H60B H 0.2271 0.7169 0.9959 0.272 Uiso 1 1 calc R . . H60C H 0.2019 0.7471 1.1090 0.272 Uiso 1 1 calc R . . C61 C 0.4338(14) 0.7630(9) 1.1904(12) 0.277(11) Uani 1 1 d U . . H61A H 0.4575 0.7320 1.2296 0.415 Uiso 1 1 calc R B . H61B H 0.3778 0.7801 1.2340 0.415 Uiso 1 1 calc R . . H61C H 0.5028 0.7838 1.1862 0.415 Uiso 1 1 calc R . . C62 C 0.6164(12) 0.5742(4) 0.8125(11) 0.059(2) Uani 0.604(10) 1 d PU D 1 H62A H 0.6153 0.5637 0.7306 0.070 Uiso 0.604(10) 1 calc PR D 1 H62B H 0.5347 0.5735 0.8319 0.070 Uiso 0.604(10) 1 calc PR D 1 C63 C 0.6883(11) 0.5367(4) 0.8900(10) 0.063(2) Uani 0.604(10) 1 d PU D 1 C62' C 0.6645(19) 0.5739(7) 0.8705(17) 0.059(2) Uani 0.40 1 d PU D 2 H62C H 0.6339 0.5745 0.9470 0.070 Uiso 0.396(10) 1 calc PR D 2 H62D H 0.7479 0.5641 0.8834 0.070 Uiso 0.396(10) 1 calc PR D 2 C63' C 0.5973(16) 0.5354(7) 0.7943(15) 0.063(2) Uani 0.40 1 d PU D 2 C64 C 0.5623(17) 0.4473(5) 0.7514(14) 0.161(5) Uani 1 1 d U D . H64A H 0.5447 0.4641 0.6757 0.193 Uiso 1 1 calc R . . H64B H 0.6140 0.4189 0.7410 0.193 Uiso 1 1 calc R . . C65 C 0.4699(18) 0.4333(6) 0.788(3) 0.236(10) Uani 1 1 d U . . H65A H 0.4277 0.4111 0.7314 0.354 Uiso 1 1 calc R D . H65B H 0.4207 0.4618 0.8006 0.354 Uiso 1 1 calc R . . H65C H 0.4887 0.4158 0.8620 0.354 Uiso 1 1 calc R . . C66 C 0.7435(11) 0.4528(4) 0.9487(14) 0.142(4) Uani 1 1 d U D . H66A H 0.7614 0.4221 0.9082 0.170 Uiso 1 1 calc R . . H66B H 0.8161 0.4727 0.9594 0.170 Uiso 1 1 calc R . . C67 C 0.7128(17) 0.4411(6) 1.0532(18) 0.204(8) Uani 1 1 d U . . H67A H 0.7751 0.4216 1.0958 0.306 Uiso 1 1 calc R D . H67B H 0.6401 0.4220 1.0438 0.306 Uiso 1 1 calc R . . H67C H 0.7007 0.4713 1.0966 0.306 Uiso 1 1 calc R . . C68 C 0.7695(5) 0.6641(2) 1.0378(5) 0.0512(13) Uani 1 1 d U B . H68A H 0.7962 0.6340 1.0006 0.061 Uiso 1 1 calc R . . H68B H 0.7738 0.6581 1.1224 0.061 Uiso 1 1 calc R . . C69 C 0.6551(7) 0.7986(3) 0.8140(7) 0.0770(19) Uani 1 1 d U . . H69A H 0.6834 0.8004 0.7374 0.116 Uiso 1 1 calc R . . H69B H 0.5876 0.7764 0.8105 0.116 Uiso 1 1 calc R . . H69C H 0.7176 0.7862 0.8709 0.116 Uiso 1 1 calc R . . C70 C 0.6211(9) 0.8465(4) 0.8480(9) 0.098(3) Uani 1 1 d U . . C71 C 0.8516(11) 0.5818(4) 0.6267(10) 0.116(3) Uani 1 1 d U . . H71A H 0.8021 0.5869 0.5532 0.174 Uiso 1 1 calc R . . H71B H 0.9304 0.5944 0.6198 0.174 Uiso 1 1 calc R . . H71C H 0.8181 0.5993 0.6891 0.174 Uiso 1 1 calc R . . C72 C 0.8581(10) 0.5297(4) 0.6530(10) 0.108(3) Uani 1 1 d U . . 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 N1 0.089(5) 0.102(5) 0.186(8) 0.003(5) 0.029(5) 0.040(4) N2 0.146(6) 0.168(7) 0.117(5) -0.065(5) 0.050(5) 0.067(6) N3 0.211(9) 0.127(6) 0.086(4) -0.068(4) 0.068(5) -0.082(6) N4 0.204(8) 0.034(3) 0.146(6) 0.016(3) 0.048(5) 0.015(3) N5 0.168(11) 0.116(7) 0.259(15) -0.041(8) 0.048(10) 0.019(7) N6 0.232(14) 0.110(6) 0.218(13) 0.035(8) 0.088(11) 0.020(8) O1 0.045(2) 0.075(3) 0.068(3) -0.036(2) -0.0048(19) 0.010(2) O2 0.063(4) 0.073(4) 0.117(6) 0.010(4) 0.023(4) 0.017(3) O2' 0.063(4) 0.073(4) 0.117(6) 0.010(4) 0.023(4) 0.017(3) O3 0.059(2) 0.0377(19) 0.064(2) -0.0116(17) 0.0217(19) -0.0030(16) O4 0.059(4) 0.111(5) 0.061(3) -0.027(3) 0.020(3) -0.010(3) O4' 0.059(4) 0.111(5) 0.061(3) -0.027(3) 0.020(3) -0.010(3) O5 0.054(2) 0.052(2) 0.0433(19) -0.0067(16) 0.0030(17) 0.0085(17) O6 0.175(8) 0.061(4) 0.061(4) -0.007(3) 0.040(4) -0.041(4) O6' 0.175(8) 0.061(4) 0.061(4) -0.007(3) 0.040(4) -0.041(4) O7 0.054(2) 0.0383(18) 0.0447(19) -0.0023(15) 0.0110(17) 0.0035(16) O8 0.080(5) 0.067(4) 0.087(4) 0.016(3) -0.016(3) 0.010(3) O8' 0.080(5) 0.067(4) 0.087(4) 0.016(3) -0.016(3) 0.010(3) C1 0.032(3) 0.060(3) 0.040(3) -0.010(2) -0.013(2) 0.012(2) C2 0.053(4) 0.076(4) 0.030(3) -0.017(2) -0.006(2) 0.002(3) C3 0.037(3) 0.090(4) 0.059(3) -0.041(3) 0.001(3) -0.006(3) C4 0.038(3) 0.080(4) 0.071(4) -0.034(3) 0.005(3) -0.012(3) C5 0.025(3) 0.081(4) 0.058(3) -0.032(3) 0.007(2) -0.003(3) C6 0.031(3) 0.066(3) 0.049(3) -0.027(3) -0.009(2) 0.007(2) C7 0.071(5) 0.099(5) 0.109(5) -0.067(4) 0.022(4) -0.014(4) C8 0.150(8) 0.103(7) 0.222(13) -0.072(8) 0.105(8) -0.014(6) C9 0.205(14) 0.251(15) 0.087(6) -0.072(6) -0.003(7) -0.058(10) C10 0.218(12) 0.149(9) 0.206(12) -0.135(9) 0.138(11) -0.112(9) C11 0.135(7) 0.069(4) 0.083(5) -0.010(4) 0.001(4) 0.044(4) C12 0.075(5) 0.065(4) 0.065(5) -0.006(4) 0.008(4) -0.014(3) C12' 0.075(5) 0.065(4) 0.065(5) -0.006(4) 0.008(4) -0.014(3) C13 0.159(13) 0.154(10) 0.277(18) 0.060(12) 0.089(13) 0.019(9) C14 0.30(3) 0.40(4) 0.28(2) 0.18(3) 0.067(19) -0.10(3) C15 0.094(6) 0.081(6) 0.160(8) 0.034(5) 0.018(6) -0.004(4) C16 0.167(13) 0.174(13) 0.168(11) -0.009(9) 0.049(10) 0.041(10) C17 0.034(3) 0.069(3) 0.065(3) -0.032(3) 0.011(2) -0.011(3) C18 0.045(3) 0.059(3) 0.069(3) -0.024(3) 0.025(3) -0.005(3) C19 0.057(4) 0.060(3) 0.095(5) -0.034(3) 0.040(3) -0.021(3) C20 0.090(5) 0.045(3) 0.095(5) -0.019(3) 0.064(4) -0.009(3) C21 0.087(5) 0.042(3) 0.072(4) -0.003(3) 0.039(3) 0.001(3) C22 0.055(3) 0.045(3) 0.047(3) -0.003(2) 0.025(2) -0.004(2) C23 0.049(3) 0.047(3) 0.055(3) -0.014(2) 0.027(2) -0.008(2) C24 0.138(7) 0.041(3) 0.145(7) -0.028(4) 0.083(6) -0.012(4) C25 0.57(3) 0.050(5) 0.132(8) -0.017(6) 0.095(11) -0.005(11) C26 0.302(16) 0.039(4) 0.299(17) 0.006(7) 0.233(15) 0.003(7) C27 0.155(9) 0.035(5) 0.58(3) -0.061(11) 0.032(13) 0.019(5) C28 0.059(6) 0.038(4) 0.065(5) -0.008(3) 0.025(4) 0.009(4) C29 0.071(5) 0.075(5) 0.056(4) 0.007(4) 0.016(3) 0.009(4) C28' 0.059(6) 0.038(4) 0.065(5) -0.008(3) 0.025(4) 0.009(4) C29' 0.071(5) 0.075(5) 0.056(4) 0.007(4) 0.016(3) 0.009(4) C30 0.164(14) 0.42(3) 0.134(11) -0.079(15) -0.012(9) 0.135(14) C31 0.125(10) 0.46(4) 0.28(3) -0.09(2) -0.042(14) 0.076(18) C32 0.224(14) 0.131(9) 0.118(7) -0.057(7) -0.045(8) 0.082(9) C33 0.52(4) 0.151(14) 0.139(13) -0.052(10) -0.033(17) 0.005(15) C34 0.061(4) 0.059(3) 0.039(3) 0.001(2) 0.016(2) -0.001(3) C35 0.043(3) 0.069(3) 0.033(3) 0.009(2) 0.002(2) 0.010(2) C36 0.077(4) 0.066(4) 0.050(3) 0.018(3) 0.019(3) 0.027(3) C37 0.068(4) 0.077(4) 0.053(3) 0.023(3) 0.012(3) 0.030(3) C38 0.047(4) 0.082(4) 0.039(3) 0.013(3) 0.004(3) 0.022(3) C39 0.036(3) 0.056(3) 0.026(2) 0.001(2) -0.0080(19) 0.004(2) C40 0.040(3) 0.052(3) 0.030(2) 0.003(2) -0.003(2) 0.009(2) C41 0.123(6) 0.136(7) 0.110(6) 0.056(5) 0.070(5) 0.089(5) C42 0.237(12) 0.159(9) 0.207(12) 0.128(9) 0.145(11) 0.155(9) C43 0.223(13) 0.075(6) 0.124(6) 0.025(5) 0.073(7) 0.068(6) C44 0.096(6) 0.263(13) 0.124(8) 0.048(8) 0.019(6) 0.115(6) C45 0.083(7) 0.048(4) 0.051(5) -0.002(4) 0.027(4) -0.011(4) C46 0.086(7) 0.070(5) 0.050(4) 0.000(3) 0.016(4) -0.015(4) C45' 0.083(7) 0.048(4) 0.051(5) -0.002(4) 0.027(4) -0.011(4) C46' 0.086(7) 0.070(5) 0.050(4) 0.000(3) 0.016(4) -0.015(4) C47 0.335(18) 0.187(12) 0.108(7) -0.048(7) 0.105(9) -0.178(13) C48 0.38(3) 0.48(4) 0.105(10) 0.013(16) 0.058(11) -0.17(3) C49 0.39(2) 0.148(10) 0.122(9) -0.009(7) 0.058(13) -0.145(13) C50 0.63(5) 0.212(17) 0.20(2) 0.062(18) -0.06(3) 0.00(2) C51 0.033(3) 0.055(3) 0.047(3) -0.002(2) 0.007(2) -0.006(2) C52 0.035(3) 0.046(3) 0.039(2) 0.004(2) 0.006(2) -0.001(2) C53 0.045(3) 0.065(4) 0.045(3) -0.004(3) -0.002(2) 0.013(3) C54 0.053(4) 0.091(5) 0.057(3) -0.016(3) 0.005(3) 0.015(3) C55 0.060(4) 0.076(4) 0.034(3) -0.009(3) -0.011(2) 0.022(3) C56 0.040(3) 0.050(3) 0.040(3) -0.002(2) 0.004(2) 0.003(2) C57 0.037(3) 0.041(3) 0.033(2) 0.0059(19) 0.005(2) -0.002(2) C58 0.079(5) 0.196(9) 0.065(4) -0.027(5) 0.011(4) 0.077(5) C59 0.169(12) 0.186(10) 0.135(8) -0.049(7) 0.007(8) 0.110(8) C60 0.097(7) 0.292(15) 0.162(11) -0.010(11) 0.046(7) 0.070(8) C61 0.153(10) 0.53(3) 0.126(8) -0.183(12) -0.069(8) 0.229(14) C62 0.074(7) 0.041(3) 0.062(7) 0.005(4) 0.010(4) 0.009(4) C63 0.072(6) 0.059(4) 0.062(5) 0.003(4) 0.019(4) -0.004(4) C62' 0.074(7) 0.041(3) 0.062(7) 0.005(4) 0.010(4) 0.009(4) C63' 0.072(6) 0.059(4) 0.062(5) 0.003(4) 0.019(4) -0.004(4) C64 0.228(14) 0.099(7) 0.163(11) -0.032(7) 0.053(8) -0.040(8) C65 0.182(16) 0.127(12) 0.41(3) 0.029(15) 0.071(15) -0.027(10) C66 0.135(9) 0.077(6) 0.219(11) 0.042(7) 0.046(7) 0.015(6) C67 0.208(16) 0.151(13) 0.259(16) 0.127(14) 0.054(12) 0.021(11) C68 0.046(3) 0.069(3) 0.037(3) 0.002(3) -0.005(2) 0.012(3) C69 0.071(5) 0.088(5) 0.073(4) -0.009(4) 0.012(4) 0.001(4) C70 0.112(7) 0.081(5) 0.105(6) -0.006(5) 0.033(5) -0.003(5) C71 0.134(9) 0.112(6) 0.106(7) -0.007(5) 0.027(6) -0.019(6) C72 0.115(7) 0.102(5) 0.119(7) -0.001(6) 0.060(6) 0.011(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N1 C15 1.377(11) . ? N1 C13 1.391(14) . ? N1 C12' 1.41(2) . ? N1 C12 1.498(15) . ? N2 C29 1.452(14) . ? N2 C29' 1.45(2) . ? N2 C30 1.606(15) . ? N2 C32 1.619(12) . ? N3 C46 1.375(13) . ? N3 C47 1.400(11) . ? N3 C49 1.397(12) . ? N3 C46' 1.55(2) . ? N4 C63 1.510(15) . ? N4 C63' 1.48(2) . ? N4 C64 1.722(17) . ? N4 C66 1.847(16) . ? N5 C70 1.121(13) . ? N6 C72 1.133(13) . ? O1 C11 1.293(9) . ? O1 C6 1.382(7) . ? O2 C12 1.188(13) . ? O2' C12' 1.27(2) . ? O3 C28' 1.305(18) . ? O3 C28 1.375(10) . ? O3 C23 1.394(7) . ? O4 C29 1.189(12) . ? O4' C29' 1.32(2) . ? O5 C45' 1.307(16) . ? O5 C40 1.382(6) . ? O5 C45 1.465(12) . ? O6 C46 1.212(13) . ? O6' C46' 1.27(2) . ? O7 C62 1.382(12) . ? O7 C57 1.392(6) . ? O7 C62' 1.422(19) . ? O8 C63 1.219(14) . ? O8' C63' 1.19(2) . ? C1 C2 1.377(8) . ? C1 C6 1.398(8) . ? C1 C68 1.553(9) . ? C2 C3 1.408(9) . ? C3 C4 1.375(9) . ? C3 C7 1.535(9) . ? C4 C5 1.398(8) . ? C5 C6 1.380(9) . ? C5 C17 1.538(8) . ? C7 C10 1.364(13) . ? C7 C8 1.477(14) . ? C7 C9 1.68(2) . ? C11 C12' 1.34(2) . ? C11 C12 1.343(15) . ? C13 C14 1.36(2) . ? C15 C16 1.382(16) . ? C17 C18 1.503(10) . ? C18 C23 1.396(9) . ? C18 C19 1.391(9) . ? C19 C20 1.392(12) . ? C20 C21 1.395(11) . ? C20 C24 1.541(10) . ? C21 C22 1.419(8) . ? C22 C23 1.382(9) . ? C22 C34 1.539(9) . ? C24 C27 1.450(18) . ? C24 C26 1.520(13) . ? C24 C25 1.474(17) . ? C28 C29 1.543(16) . ? C28' C29' 1.48(3) . ? C30 C31 1.36(3) . ? C32 C33 1.41(2) . ? C34 C35 1.501(8) . ? C35 C36 1.383(8) . ? C35 C40 1.406(8) . ? C36 C37 1.384(9) . ? C37 C38 1.365(9) . ? C37 C41 1.592(10) . ? C38 C39 1.394(8) . ? C39 C40 1.404(7) . ? C39 C51 1.507(8) . ? C41 C42 1.397(14) . ? C41 C43 1.477(15) . ? C41 C44 1.60(2) . ? C45 C46 1.509(16) . ? C45' C46' 1.51(2) . ? C47 C48 1.64(3) . ? C49 C50 1.61(3) . ? C51 C52 1.528(7) . ? C52 C53 1.381(8) . ? C52 C57 1.398(7) . ? C53 C54 1.363(9) . ? C54 C55 1.408(9) . ? C54 C58 1.542(10) . ? C55 C56 1.376(8) . ? C56 C57 1.394(7) . ? C56 C68 1.523(8) . ? C58 C61 1.408(14) . ? C58 C59 1.519(18) . ? C58 C60 1.58(2) . ? C62 C63 1.521(18) . ? C62' C63' 1.51(3) . ? C64 C65 1.24(2) . ? C66 C67 1.32(2) . ? C69 C70 1.412(12) . ? C71 C72 1.435(15) . ? 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 C15 N1 C13 116.3(10) . . ? C15 N1 C12' 163.6(11) . . ? C13 N1 C12' 79.4(12) . . ? C15 N1 C12 105.5(8) . . ? C13 N1 C12 137.9(10) . . ? C12' N1 C12 59.4(10) . . ? C29 N2 C29' 53.4(9) . . ? C29 N2 C30 151.6(9) . . ? C29' N2 C30 98.7(11) . . ? C29 N2 C32 101.0(8) . . ? C29' N2 C32 153.9(11) . . ? C30 N2 C32 106.1(8) . . ? C46 N3 C47 137.8(9) . . ? C46 N3 C49 105.5(9) . . ? C47 N3 C49 116.6(9) . . ? C46 N3 C46' 49.8(8) . . ? C47 N3 C46' 88.3(8) . . ? C49 N3 C46' 155.2(10) . . ? C63 N4 C63' 56.8(9) . . ? C63 N4 C64 152.4(9) . . ? C63' N4 C64 99.1(11) . . ? C63 N4 C66 91.6(8) . . ? C63' N4 C66 146.7(11) . . ? C64 N4 C66 108.1(8) . . ? C11 O1 C6 119.8(5) . . ? C28' O3 C28 36.0(8) . . ? C28' O3 C23 121.6(9) . . ? C28 O3 C23 111.6(5) . . ? C45' O5 C40 112.5(9) . . ? C45' O5 C45 35.4(7) . . ? C40 O5 C45 113.4(6) . . ? C62 O7 C57 118.5(6) . . ? C62 O7 C62' 33.7(8) . . ? C57 O7 C62' 115.7(8) . . ? C2 C1 C6 117.8(5) . . ? C2 C1 C68 120.0(5) . . ? C6 C1 C68 122.0(5) . . ? C1 C2 C3 123.4(5) . . ? C4 C3 C2 116.2(5) . . ? C4 C3 C7 123.3(7) . . ? C2 C3 C7 120.3(6) . . ? C3 C4 C5 122.5(6) . . ? C4 C5 C6 118.9(5) . . ? C4 C5 C17 118.2(6) . . ? C6 C5 C17 122.5(5) . . ? O1 C6 C1 120.2(5) . . ? O1 C6 C5 118.9(5) . . ? C1 C6 C5 120.9(5) . . ? C10 C7 C8 127.5(10) . . ? C10 C7 C3 114.3(7) . . ? C8 C7 C3 108.6(7) . . ? C10 C7 C9 100.4(11) . . ? C8 C7 C9 95.7(10) . . ? C3 C7 C9 105.5(9) . . ? O1 C11 C12' 163.5(13) . . ? O1 C11 C12 125.8(9) . . ? C12' C11 C12 65.1(11) . . ? O2 C12 C11 122.8(11) . . ? O2 C12 N1 122.6(10) . . ? C11 C12 N1 114.7(9) . . ? O2' C12' C11 99.5(17) . . ? O2' C12' N1 137.7(17) . . ? C11 C12' N1 120.9(15) . . ? C14 C13 N1 109.7(15) . . ? N1 C15 C16 110.4(10) . . ? C5 C17 C18 111.9(5) . . ? C23 C18 C19 119.1(7) . . ? C23 C18 C17 121.9(5) . . ? C19 C18 C17 119.0(6) . . ? C20 C19 C18 121.2(7) . . ? C19 C20 C21 119.0(6) . . ? C19 C20 C24 120.1(8) . . ? C21 C20 C24 120.8(9) . . ? C22 C21 C20 120.3(7) . . ? C21 C22 C23 118.9(6) . . ? C21 C22 C34 117.7(6) . . ? C23 C22 C34 123.5(5) . . ? O3 C23 C18 119.4(6) . . ? O3 C23 C22 119.8(5) . . ? C18 C23 C22 120.7(5) . . ? C27 C24 C26 116.3(14) . . ? C27 C24 C25 101.0(15) . . ? C26 C24 C25 109.1(13) . . ? C27 C24 C20 110.1(8) . . ? C26 C24 C20 109.2(6) . . ? C25 C24 C20 110.8(9) . . ? O3 C28 C29 115.0(9) . . ? O4 C29 N2 130.1(10) . . ? O4 C29 C28 122.4(9) . . ? N2 C29 C28 107.4(9) . . ? O3 C28' C29' 119.0(17) . . ? O4' C29' C28' 122.9(16) . . ? O4' C29' N2 124.7(16) . . ? C28' C29' N2 112.3(15) . . ? C31 C30 N2 106.1(16) . . ? C33 C32 N2 104.4(12) . . ? C35 C34 C22 109.5(4) . . ? C36 C35 C40 117.9(5) . . ? C36 C35 C34 119.1(5) . . ? C40 C35 C34 122.9(5) . . ? C35 C36 C37 121.9(6) . . ? C38 C37 C36 118.7(6) . . ? C38 C37 C41 120.6(6) . . ? C36 C37 C41 120.7(6) . . ? C37 C38 C39 122.9(5) . . ? C38 C39 C40 116.9(5) . . ? C38 C39 C51 121.1(5) . . ? C40 C39 C51 121.9(5) . . ? O5 C40 C39 118.9(4) . . ? O5 C40 C35 119.7(4) . . ? C39 C40 C35 121.3(5) . . ? C42 C41 C43 118.2(11) . . ? C42 C41 C37 113.2(7) . . ? C43 C41 C37 108.1(7) . . ? C42 C41 C44 106.8(12) . . ? C43 C41 C44 104.6(9) . . ? C37 C41 C44 104.7(9) . . ? O5 C45 C46 114.1(8) . . ? O6 C46 N3 126.1(10) . . ? O6 C46 C45 122.1(10) . . ? N3 C46 C45 111.8(9) . . ? O5 C45' C46' 117.1(13) . . ? O6' C46' C45' 117.6(15) . . ? O6' C46' N3 132.0(14) . . ? C45' C46' N3 110.2(11) . . ? N3 C47 C48 106.4(12) . . ? N3 C49 C50 106.1(15) . . ? C39 C51 C52 110.3(4) . . ? C53 C52 C57 117.3(4) . . ? C53 C52 C51 120.8(5) . . ? C57 C52 C51 121.7(4) . . ? C54 C53 C52 124.1(5) . . ? C53 C54 C55 116.8(5) . . ? C53 C54 C58 121.1(6) . . ? C55 C54 C58 122.1(6) . . ? C56 C55 C54 121.8(5) . . ? C55 C56 C57 118.7(5) . . ? C55 C56 C68 119.9(5) . . ? C57 C56 C68 121.4(5) . . ? C52 C57 O7 119.5(4) . . ? C52 C57 C56 120.8(5) . . ? O7 C57 C56 119.6(4) . . ? C61 C58 C54 112.6(7) . . ? C61 C58 C59 117.1(13) . . ? C54 C58 C59 109.9(8) . . ? C61 C58 C60 112.5(13) . . ? C54 C58 C60 107.6(10) . . ? C59 C58 C60 95.7(10) . . ? O7 C62 C63 115.1(11) . . ? O8 C63 N4 135.1(11) . . ? O8 C63 C62 121.2(10) . . ? N4 C63 C62 103.2(10) . . ? O7 C62' C63' 113.7(15) . . ? O8' C63' N4 132.1(16) . . ? O8' C63' C62' 122.2(16) . . ? N4 C63' C62' 103.8(14) . . ? C65 C64 N4 107.0(16) . . ? C67 C66 N4 114.5(11) . . ? C56 C68 C1 110.0(4) . . ? N5 C70 C69 178.6(12) . . ? N6 C72 C71 177.0(12) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 23.25 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.748 _refine_diff_density_min -0.327 _refine_diff_density_rms 0.091