# Electronic Supplementary Material (ESI) for Chemical Science # 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_compound1(benzene) _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C65 H88 Mg2 N4 O3' _chemical_formula_weight 1022.01 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' Mg Mg 0.1719 0.1771 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 10.8296(2) _cell_length_b 22.4623(2) _cell_length_c 24.9069(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6058.80(14) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.35 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.120 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2216 _exptl_absorpt_coefficient_mu 0.708 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.741 _exptl_absorpt_correction_T_max 0.789 _exptl_absorpt_process_details 'SCALE3 ABSPACK' _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'Enhance (Cu) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Gemini Ultra' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 55425 _diffrn_reflns_av_R_equivalents 0.0230 _diffrn_reflns_av_sigmaI/netI 0.0167 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 2.65 _diffrn_reflns_theta_max 66.99 _reflns_number_total 10721 _reflns_number_gt 10622 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. A molecule of benzene of crystallisation in the asymmetric unit was located and its carbon atoms refined anisotropically. ; _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^)+(0.0399P)^2^+1.2523P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00(2) _refine_ls_number_reflns 10721 _refine_ls_number_parameters 687 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0286 _refine_ls_R_factor_gt 0.0283 _refine_ls_wR_factor_ref 0.0732 _refine_ls_wR_factor_gt 0.0730 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.052 _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 Mg1 Mg 0.91962(4) 0.042119(17) 0.079350(16) 0.01842(9) Uani 1 1 d . . . O1 O 0.99549(8) -0.04077(4) 0.08072(4) 0.01907(17) Uani 1 1 d . . . N1 N 0.92162(10) 0.09394(5) 0.14551(4) 0.0196(2) Uani 1 1 d . . . C1 C 0.92936(16) 0.18749(6) 0.19571(6) 0.0312(3) Uani 1 1 d . . . H1A H 0.8488 0.1827 0.2131 0.047 Uiso 1 1 calc R . . H1B H 0.9439 0.2298 0.1882 0.047 Uiso 1 1 calc R . . H1C H 0.9943 0.1725 0.2195 0.047 Uiso 1 1 calc R . . Mg2 Mg 1.05330(4) -0.126648(17) 0.081665(16) 0.01817(9) Uani 1 1 d . . . O2 O 0.80003(9) -0.02251(4) 0.05981(4) 0.0237(2) Uani 1 1 d . . . N2 N 0.94301(10) 0.11050(4) 0.02741(4) 0.0186(2) Uani 1 1 d . . . C2 C 0.93096(13) 0.15297(6) 0.14383(5) 0.0221(3) Uani 1 1 d . . . O3 O 0.87455(9) -0.11714(4) 0.05958(4) 0.0234(2) Uani 1 1 d . . . N3 N 1.17656(10) -0.16240(5) 0.02996(4) 0.0184(2) Uani 1 1 d . . . C3 C 0.94211(13) 0.18627(5) 0.09641(5) 0.0243(3) Uani 1 1 d . . . H3 H 0.9463 0.2282 0.1014 0.029 Uiso 1 1 calc R . . N4 N 1.09054(10) -0.18368(5) 0.14246(4) 0.0200(2) Uani 1 1 d . . . C4 C 0.94806(13) 0.16729(5) 0.04273(5) 0.0215(3) Uani 1 1 d . . . C5 C 0.96337(15) 0.21570(6) 0.00113(6) 0.0295(3) Uani 1 1 d . . . H5A H 1.0500 0.2176 -0.0101 0.044 Uiso 1 1 calc R . . H5B H 0.9388 0.2540 0.0166 0.044 Uiso 1 1 calc R . . H5C H 0.9113 0.2068 -0.0300 0.044 Uiso 1 1 calc R . . C6 C 0.91647(13) 0.06474(5) 0.19700(5) 0.0208(3) Uani 1 1 d . . . C7 C 0.80209(14) 0.05314(6) 0.22145(6) 0.0257(3) Uani 1 1 d . . . C8 C 0.80104(15) 0.01965(7) 0.26866(6) 0.0343(3) Uani 1 1 d . . . H8 H 0.7246 0.0114 0.2859 0.041 Uiso 1 1 calc R . . C9 C 0.90947(17) -0.00178(7) 0.29079(6) 0.0359(4) Uani 1 1 d . . . H9 H 0.9068 -0.0257 0.3222 0.043 Uiso 1 1 calc R . . C10 C 1.02110(15) 0.01152(7) 0.26737(6) 0.0311(3) Uani 1 1 d . . . H10 H 1.0950 -0.0030 0.2832 0.037 Uiso 1 1 calc R . . C11 C 1.02775(14) 0.04588(6) 0.22093(5) 0.0250(3) Uani 1 1 d . . . C12 C 0.68189(14) 0.07642(7) 0.19820(6) 0.0302(3) Uani 1 1 d . . . H12 H 0.7032 0.1045 0.1684 0.036 Uiso 1 1 calc R . . C13 C 0.60413(15) 0.02641(8) 0.17427(8) 0.0409(4) Uani 1 1 d . . . H13A H 0.6514 0.0061 0.1462 0.061 Uiso 1 1 calc R . . H13B H 0.5285 0.0431 0.1588 0.061 Uiso 1 1 calc R . . H13C H 0.5825 -0.0021 0.2025 0.061 Uiso 1 1 calc R . . C14 C 0.60673(17) 0.11125(8) 0.23984(8) 0.0454(4) Uani 1 1 d . . . H14A H 0.5761 0.0839 0.2674 0.068 Uiso 1 1 calc R . . H14B H 0.5367 0.1307 0.2221 0.068 Uiso 1 1 calc R . . H14C H 0.6593 0.1415 0.2566 0.068 Uiso 1 1 calc R . . C15 C 1.15253(14) 0.06358(7) 0.19848(6) 0.0314(3) Uani 1 1 d . . . H15 H 1.1383 0.0973 0.1730 0.038 Uiso 1 1 calc R . . C16 C 1.21294(17) 0.01388(10) 0.16690(8) 0.0513(5) Uani 1 1 d . . . H16A H 1.2222 -0.0212 0.1899 0.077 Uiso 1 1 calc R . . H16B H 1.2944 0.0269 0.1544 0.077 Uiso 1 1 calc R . . H16C H 1.1613 0.0038 0.1359 0.077 Uiso 1 1 calc R . . C17 C 1.24109(18) 0.08597(10) 0.24187(8) 0.0500(5) Uani 1 1 d . . . H17A H 1.1994 0.1160 0.2640 0.075 Uiso 1 1 calc R . . H17B H 1.3139 0.1038 0.2249 0.075 Uiso 1 1 calc R . . H17C H 1.2667 0.0525 0.2646 0.075 Uiso 1 1 calc R . . C18 C 0.95122(12) 0.09678(5) -0.02911(5) 0.0193(3) Uani 1 1 d . . . C19 C 0.84224(13) 0.08748(6) -0.05861(5) 0.0221(3) Uani 1 1 d . . . C20 C 0.85260(15) 0.07160(6) -0.11236(5) 0.0281(3) Uani 1 1 d . . . H20 H 0.7798 0.0655 -0.1329 0.034 Uiso 1 1 calc R . . C21 C 0.96631(16) 0.06454(7) -0.13651(6) 0.0312(3) Uani 1 1 d . . . H21 H 0.9713 0.0532 -0.1732 0.037 Uiso 1 1 calc R . . C22 C 1.07322(14) 0.07398(6) -0.10709(6) 0.0282(3) Uani 1 1 d . . . H22 H 1.1513 0.0690 -0.1239 0.034 Uiso 1 1 calc R . . C23 C 1.06803(13) 0.09064(6) -0.05325(5) 0.0225(3) Uani 1 1 d . . . C24 C 0.71556(13) 0.09652(7) -0.03383(6) 0.0280(3) Uani 1 1 d . . . H24 H 0.7273 0.1027 0.0056 0.034 Uiso 1 1 calc R . . C25 C 0.63123(15) 0.04274(7) -0.04119(7) 0.0354(3) Uani 1 1 d . . . H25A H 0.5534 0.0495 -0.0221 0.053 Uiso 1 1 calc R . . H25B H 0.6717 0.0072 -0.0267 0.053 Uiso 1 1 calc R . . H25C H 0.6144 0.0370 -0.0795 0.053 Uiso 1 1 calc R . . C26 C 0.65505(16) 0.15241(8) -0.05644(10) 0.0532(5) Uani 1 1 d . . . H26A H 0.6453 0.1482 -0.0954 0.080 Uiso 1 1 calc R . . H26B H 0.7071 0.1870 -0.0487 0.080 Uiso 1 1 calc R . . H26C H 0.5738 0.1579 -0.0398 0.080 Uiso 1 1 calc R . . C27 C 1.18522(13) 0.10080(6) -0.02099(6) 0.0260(3) Uani 1 1 d . . . H27 H 1.1647 0.1285 0.0091 0.031 Uiso 1 1 calc R . . C28 C 1.23067(15) 0.04243(7) 0.00361(7) 0.0369(4) Uani 1 1 d . . . H28A H 1.1656 0.0254 0.0262 0.055 Uiso 1 1 calc R . . H28B H 1.3042 0.0501 0.0255 0.055 Uiso 1 1 calc R . . H28C H 1.2514 0.0143 -0.0251 0.055 Uiso 1 1 calc R . . C29 C 1.28808(16) 0.12933(9) -0.05393(8) 0.0467(4) Uani 1 1 d . . . H29A H 1.3170 0.1011 -0.0811 0.070 Uiso 1 1 calc R . . H29B H 1.3568 0.1400 -0.0302 0.070 Uiso 1 1 calc R . . H29C H 1.2566 0.1652 -0.0716 0.070 Uiso 1 1 calc R . . C30 C 1.28305(14) -0.25022(6) -0.00743(6) 0.0260(3) Uani 1 1 d . . . H30A H 1.2548 -0.2394 -0.0435 0.039 Uiso 1 1 calc R . . H30B H 1.2779 -0.2935 -0.0029 0.039 Uiso 1 1 calc R . . H30C H 1.3688 -0.2373 -0.0027 0.039 Uiso 1 1 calc R . . C31 C 1.20223(12) -0.22006(6) 0.03395(5) 0.0202(3) Uani 1 1 d . . . C32 C 1.15903(13) -0.25613(5) 0.07646(5) 0.0228(3) Uani 1 1 d . . . H32 H 1.1617 -0.2978 0.0698 0.027 Uiso 1 1 calc R . . C33 C 1.11286(13) -0.23993(6) 0.12685(5) 0.0230(3) Uani 1 1 d . . . C34 C 1.08632(17) -0.29092(6) 0.16483(6) 0.0350(3) Uani 1 1 d . . . H34A H 1.1145 -0.2804 0.2010 0.052 Uiso 1 1 calc R . . H34B H 1.1300 -0.3266 0.1526 0.052 Uiso 1 1 calc R . . H34C H 0.9973 -0.2987 0.1655 0.052 Uiso 1 1 calc R . . C35 C 1.23443(13) -0.13024(6) -0.01324(5) 0.0207(3) Uani 1 1 d . . . C36 C 1.16508(13) -0.11742(6) -0.05965(5) 0.0249(3) Uani 1 1 d . . . C37 C 1.22548(16) -0.08883(7) -0.10200(6) 0.0340(3) Uani 1 1 d . . . H37 H 1.1810 -0.0799 -0.1338 0.041 Uiso 1 1 calc R . . C38 C 1.34837(17) -0.07338(7) -0.09845(6) 0.0388(4) Uani 1 1 d . . . H38 H 1.3883 -0.0551 -0.1281 0.047 Uiso 1 1 calc R . . C39 C 1.41416(15) -0.08447(7) -0.05160(6) 0.0323(3) Uani 1 1 d . . . H39 H 1.4983 -0.0728 -0.0493 0.039 Uiso 1 1 calc R . . C40 C 1.35838(13) -0.11249(6) -0.00812(5) 0.0231(3) Uani 1 1 d . . . C41 C 1.03045(13) -0.13551(6) -0.06499(5) 0.0265(3) Uani 1 1 d . . . H41 H 1.0034 -0.1515 -0.0294 0.032 Uiso 1 1 calc R . . C42 C 0.94737(17) -0.08273(8) -0.07830(8) 0.0426(4) Uani 1 1 d . . . H42A H 0.9611 -0.0509 -0.0521 0.064 Uiso 1 1 calc R . . H42B H 0.8608 -0.0953 -0.0770 0.064 Uiso 1 1 calc R . . H42C H 0.9669 -0.0681 -0.1144 0.064 Uiso 1 1 calc R . . C43 C 1.01339(17) -0.18500(8) -0.10626(7) 0.0433(4) Uani 1 1 d . . . H43A H 1.0410 -0.1710 -0.1415 0.065 Uiso 1 1 calc R . . H43B H 0.9259 -0.1960 -0.1081 0.065 Uiso 1 1 calc R . . H43C H 1.0623 -0.2198 -0.0956 0.065 Uiso 1 1 calc R . . C44 C 1.42846(13) -0.12182(6) 0.04420(6) 0.0254(3) Uani 1 1 d . . . H44 H 1.3854 -0.1541 0.0646 0.031 Uiso 1 1 calc R . . C45 C 1.42358(18) -0.06562(7) 0.07832(7) 0.0402(4) Uani 1 1 d . . . H45A H 1.4642 -0.0730 0.1128 0.060 Uiso 1 1 calc R . . H45B H 1.3373 -0.0544 0.0845 0.060 Uiso 1 1 calc R . . H45C H 1.4661 -0.0332 0.0596 0.060 Uiso 1 1 calc R . . C46 C 1.56165(16) -0.14121(9) 0.03613(8) 0.0468(4) Uani 1 1 d . . . H46A H 1.5642 -0.1753 0.0116 0.070 Uiso 1 1 calc R . . H46B H 1.5974 -0.1526 0.0708 0.070 Uiso 1 1 calc R . . H46C H 1.6092 -0.1082 0.0208 0.070 Uiso 1 1 calc R . . C47 C 1.07298(13) -0.17198(5) 0.19878(5) 0.0209(3) Uani 1 1 d . . . C48 C 0.95458(13) -0.17027(6) 0.22147(5) 0.0245(3) Uani 1 1 d . . . C49 C 0.94228(14) -0.15819(6) 0.27612(6) 0.0297(3) Uani 1 1 d . . . H49 H 0.8623 -0.1573 0.2918 0.036 Uiso 1 1 calc R . . C50 C 1.04520(15) -0.14746(6) 0.30797(6) 0.0304(3) Uani 1 1 d . . . H50 H 1.0358 -0.1400 0.3453 0.036 Uiso 1 1 calc R . . C51 C 1.16097(15) -0.14777(6) 0.28508(6) 0.0275(3) Uani 1 1 d . . . H51 H 1.2309 -0.1399 0.3070 0.033 Uiso 1 1 calc R . . C52 C 1.17805(13) -0.15931(6) 0.23048(5) 0.0242(3) Uani 1 1 d . . . C53 C 0.83869(14) -0.17974(7) 0.18800(6) 0.0325(3) Uani 1 1 d . . . H53 H 0.8650 -0.1892 0.1505 0.039 Uiso 1 1 calc R . . C54 C 0.76238(17) -0.12230(10) 0.18629(7) 0.0474(4) Uani 1 1 d . . . H54A H 0.7291 -0.1140 0.2221 0.071 Uiso 1 1 calc R . . H54B H 0.6942 -0.1270 0.1608 0.071 Uiso 1 1 calc R . . H54C H 0.8151 -0.0892 0.1749 0.071 Uiso 1 1 calc R . . C55 C 0.76090(19) -0.23188(11) 0.20853(8) 0.0550(5) Uani 1 1 d . . . H55A H 0.8105 -0.2684 0.2079 0.083 Uiso 1 1 calc R . . H55B H 0.6884 -0.2369 0.1854 0.083 Uiso 1 1 calc R . . H55C H 0.7340 -0.2237 0.2454 0.083 Uiso 1 1 calc R . . C56 C 1.30672(14) -0.15834(8) 0.20637(6) 0.0339(3) Uani 1 1 d . . . H56 H 1.2991 -0.1448 0.1683 0.041 Uiso 1 1 calc R . . C57 C 1.39565(16) -0.11557(9) 0.23513(7) 0.0436(4) Uani 1 1 d . . . H57A H 1.3569 -0.0763 0.2385 0.065 Uiso 1 1 calc R . . H57B H 1.4721 -0.1120 0.2143 0.065 Uiso 1 1 calc R . . H57C H 1.4147 -0.1311 0.2710 0.065 Uiso 1 1 calc R . . C58 C 1.36527(17) -0.22024(10) 0.20583(9) 0.0554(5) Uani 1 1 d . . . H58A H 1.3693 -0.2357 0.2426 0.083 Uiso 1 1 calc R . . H58B H 1.4488 -0.2177 0.1909 0.083 Uiso 1 1 calc R . . H58C H 1.3152 -0.2470 0.1837 0.083 Uiso 1 1 calc R . . C59 C 0.88333(12) -0.06138(5) 0.06568(5) 0.0189(3) Uani 1 1 d . . . C60 C 0.4832(2) 0.15513(9) 0.09013(8) 0.0554(5) Uani 1 1 d . . . H60 H 0.4990 0.1201 0.0698 0.066 Uiso 1 1 calc R . . C61 C 0.5785(2) 0.19208(11) 0.10364(8) 0.0618(6) Uani 1 1 d . . . H61 H 0.6604 0.1829 0.0928 0.074 Uiso 1 1 calc R . . C62 C 0.5548(3) 0.24284(11) 0.13316(8) 0.0671(7) Uani 1 1 d . . . H62 H 0.6208 0.2685 0.1428 0.081 Uiso 1 1 calc R . . C63 C 0.4364(3) 0.25639(9) 0.14858(8) 0.0651(6) Uani 1 1 d . . . H63 H 0.4205 0.2915 0.1686 0.078 Uiso 1 1 calc R . . C64 C 0.3413(2) 0.21914(11) 0.13503(8) 0.0598(5) Uani 1 1 d . . . H64 H 0.2593 0.2283 0.1458 0.072 Uiso 1 1 calc R . . C65 C 0.3649(2) 0.16829(10) 0.10570(8) 0.0555(5) Uani 1 1 d . . . H65 H 0.2991 0.1424 0.0963 0.067 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 Mg1 0.0242(2) 0.01398(18) 0.01710(19) -0.00060(15) -0.00044(17) -0.00077(16) O1 0.0186(4) 0.0161(4) 0.0225(4) -0.0013(3) -0.0015(3) -0.0020(3) N1 0.0235(6) 0.0182(5) 0.0169(5) -0.0012(4) 0.0001(4) -0.0009(4) C1 0.0463(9) 0.0235(6) 0.0238(7) -0.0067(5) 0.0011(6) -0.0035(6) Mg2 0.0208(2) 0.01600(19) 0.01775(19) -0.00019(15) 0.00073(16) 0.00054(16) O2 0.0214(5) 0.0174(4) 0.0322(5) -0.0018(4) -0.0041(4) 0.0021(4) N2 0.0218(5) 0.0170(5) 0.0170(5) -0.0008(4) -0.0015(4) -0.0012(4) C2 0.0241(7) 0.0203(6) 0.0220(6) -0.0031(5) 0.0002(5) -0.0019(5) O3 0.0234(5) 0.0152(4) 0.0316(5) -0.0031(4) -0.0019(4) -0.0016(4) N3 0.0200(5) 0.0168(5) 0.0183(5) -0.0002(4) 0.0009(4) -0.0010(4) C3 0.0331(7) 0.0144(6) 0.0254(7) -0.0021(5) 0.0001(6) -0.0020(5) N4 0.0224(5) 0.0193(5) 0.0184(5) 0.0001(4) -0.0006(4) 0.0001(4) C4 0.0241(7) 0.0175(6) 0.0229(6) 0.0016(5) -0.0003(5) -0.0013(5) C5 0.0427(8) 0.0194(6) 0.0265(7) 0.0039(5) 0.0009(6) -0.0035(6) C6 0.0265(7) 0.0187(6) 0.0171(6) -0.0024(5) -0.0009(5) -0.0031(5) C7 0.0282(7) 0.0250(7) 0.0239(7) -0.0004(5) -0.0007(6) -0.0060(6) C8 0.0330(8) 0.0420(8) 0.0279(7) 0.0076(7) 0.0029(6) -0.0107(7) C9 0.0456(9) 0.0383(8) 0.0237(7) 0.0112(6) -0.0031(7) -0.0067(7) C10 0.0351(8) 0.0344(7) 0.0237(7) 0.0016(6) -0.0065(6) 0.0013(6) C11 0.0300(7) 0.0234(6) 0.0214(6) -0.0041(5) -0.0015(5) 0.0026(6) C12 0.0257(7) 0.0328(8) 0.0321(7) 0.0021(6) 0.0024(6) -0.0051(6) C13 0.0271(8) 0.0452(9) 0.0504(10) -0.0049(8) -0.0067(7) -0.0031(7) C14 0.0363(9) 0.0466(10) 0.0534(11) -0.0082(8) 0.0040(8) 0.0038(8) C15 0.0269(8) 0.0413(8) 0.0261(7) 0.0013(6) 0.0002(6) 0.0045(6) C16 0.0291(9) 0.0706(13) 0.0541(11) -0.0302(10) -0.0005(8) 0.0061(8) C17 0.0385(9) 0.0642(12) 0.0475(10) -0.0193(9) 0.0057(8) -0.0145(9) C18 0.0236(7) 0.0167(6) 0.0176(6) 0.0006(5) -0.0008(5) -0.0010(5) C19 0.0229(7) 0.0208(6) 0.0227(6) 0.0018(5) -0.0008(5) -0.0030(5) C20 0.0327(8) 0.0308(7) 0.0208(7) -0.0002(5) -0.0054(6) -0.0060(6) C21 0.0414(9) 0.0335(7) 0.0186(6) -0.0023(6) 0.0039(6) -0.0074(7) C22 0.0293(8) 0.0276(7) 0.0277(7) -0.0001(5) 0.0088(6) -0.0038(6) C23 0.0247(7) 0.0183(6) 0.0244(6) 0.0018(5) 0.0015(6) -0.0026(5) C24 0.0224(7) 0.0350(8) 0.0265(7) -0.0030(6) -0.0009(6) -0.0025(6) C25 0.0270(7) 0.0404(8) 0.0386(8) 0.0031(7) 0.0019(6) -0.0073(7) C26 0.0236(8) 0.0416(9) 0.0945(16) 0.0102(10) 0.0022(9) 0.0038(7) C27 0.0216(7) 0.0254(7) 0.0310(7) 0.0015(5) 0.0003(6) -0.0021(5) C28 0.0320(8) 0.0345(8) 0.0443(9) 0.0077(7) -0.0064(7) 0.0004(7) C29 0.0270(8) 0.0594(11) 0.0537(10) 0.0214(9) -0.0034(7) -0.0158(8) C30 0.0291(7) 0.0218(6) 0.0271(7) -0.0056(5) 0.0027(6) 0.0010(5) C31 0.0202(6) 0.0193(6) 0.0210(6) -0.0029(5) -0.0033(5) -0.0013(5) C32 0.0307(7) 0.0153(6) 0.0225(6) -0.0014(5) -0.0018(6) 0.0003(5) C33 0.0264(7) 0.0201(6) 0.0224(6) 0.0023(5) -0.0041(5) -0.0032(5) C34 0.0541(10) 0.0238(7) 0.0269(7) 0.0055(6) 0.0037(7) -0.0013(7) C35 0.0248(7) 0.0179(6) 0.0195(6) -0.0022(5) 0.0045(5) -0.0011(5) C36 0.0314(7) 0.0243(7) 0.0190(6) -0.0030(5) 0.0012(5) -0.0028(6) C37 0.0436(9) 0.0379(8) 0.0205(7) 0.0033(6) 0.0009(6) -0.0079(7) C38 0.0488(10) 0.0417(9) 0.0260(7) 0.0055(7) 0.0115(7) -0.0121(8) C39 0.0307(8) 0.0327(7) 0.0335(8) -0.0025(6) 0.0087(6) -0.0095(6) C40 0.0254(7) 0.0188(6) 0.0253(7) -0.0042(5) 0.0041(5) -0.0022(5) C41 0.0295(7) 0.0282(7) 0.0217(6) 0.0005(5) -0.0032(5) -0.0038(6) C42 0.0393(9) 0.0389(8) 0.0497(9) 0.0022(8) -0.0064(8) 0.0044(7) C43 0.0404(9) 0.0447(9) 0.0448(9) -0.0153(8) -0.0048(8) -0.0071(8) C44 0.0216(7) 0.0242(6) 0.0306(7) -0.0035(5) -0.0002(5) -0.0015(6) C45 0.0574(10) 0.0331(8) 0.0299(7) -0.0096(6) -0.0072(8) 0.0091(8) C46 0.0264(8) 0.0667(12) 0.0472(10) -0.0179(9) -0.0041(7) 0.0103(8) C47 0.0260(7) 0.0174(6) 0.0194(6) 0.0013(5) 0.0000(5) 0.0006(5) C48 0.0263(7) 0.0246(6) 0.0225(6) 0.0030(5) 0.0000(5) 0.0008(6) C49 0.0302(8) 0.0341(7) 0.0247(7) 0.0016(6) 0.0035(6) 0.0043(6) C50 0.0416(9) 0.0310(7) 0.0186(6) -0.0007(5) 0.0005(6) 0.0043(6) C51 0.0346(8) 0.0267(7) 0.0210(7) -0.0013(5) -0.0060(6) -0.0010(6) C52 0.0280(7) 0.0224(6) 0.0223(6) 0.0013(5) -0.0031(6) -0.0006(5) C53 0.0237(7) 0.0474(9) 0.0263(7) -0.0002(6) -0.0004(6) -0.0017(7) C54 0.0349(9) 0.0725(13) 0.0347(9) -0.0037(9) -0.0029(7) 0.0202(9) C55 0.0399(10) 0.0796(14) 0.0455(10) 0.0057(10) -0.0028(8) -0.0252(10) C56 0.0262(8) 0.0526(10) 0.0230(7) -0.0001(7) -0.0024(6) -0.0047(7) C57 0.0323(9) 0.0557(10) 0.0429(9) 0.0035(8) -0.0071(7) -0.0112(8) C58 0.0315(9) 0.0688(13) 0.0659(12) -0.0354(11) -0.0064(9) 0.0130(9) C59 0.0209(6) 0.0172(6) 0.0185(6) -0.0010(5) 0.0003(5) -0.0023(5) C60 0.0767(15) 0.0492(11) 0.0403(10) 0.0084(8) 0.0003(10) 0.0093(10) C61 0.0552(12) 0.0856(16) 0.0446(11) 0.0277(11) -0.0052(9) 0.0058(12) C62 0.0830(17) 0.0803(16) 0.0381(10) 0.0192(10) -0.0135(11) -0.0361(14) C63 0.106(2) 0.0488(11) 0.0402(10) -0.0002(8) 0.0072(12) -0.0123(13) C64 0.0653(14) 0.0703(14) 0.0438(11) 0.0081(10) 0.0081(10) 0.0046(11) C65 0.0711(14) 0.0567(11) 0.0386(10) 0.0088(9) -0.0075(9) -0.0164(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mg1 O2 2.0054(10) . ? Mg1 N1 2.0176(11) . ? Mg1 N2 2.0240(11) . ? Mg1 O1 2.0355(9) . ? O1 C59 1.3527(15) . ? O1 Mg2 2.0281(9) . ? N1 C2 1.3303(16) . ? N1 C6 1.4416(16) . ? C1 C2 1.5073(18) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? Mg2 N3 2.0212(11) . ? Mg2 O3 2.0237(10) . ? Mg2 N4 2.0240(11) . ? O2 C59 1.2639(16) . ? N2 C4 1.3327(16) . ? N2 C18 1.4439(16) . ? C2 C3 1.4033(19) . ? O3 C59 1.2652(15) . ? N3 C31 1.3283(17) . ? N3 C35 1.4397(16) . ? C3 C4 1.4048(19) . ? C3 H3 0.9500 . ? N4 C33 1.3438(17) . ? N4 C47 1.4398(16) . ? C4 C5 1.5110(18) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 C7 1.405(2) . ? C6 C11 1.410(2) . ? C7 C8 1.396(2) . ? C7 C12 1.518(2) . ? C8 C9 1.384(2) . ? C8 H8 0.9500 . ? C9 C10 1.375(2) . ? C9 H9 0.9500 . ? C10 C11 1.393(2) . ? C10 H10 0.9500 . ? C11 C15 1.515(2) . ? C12 C13 1.525(2) . ? C12 C14 1.533(2) . ? C12 H12 1.0000 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C16 1.514(2) . ? C15 C17 1.530(2) . ? C15 H15 1.0000 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C19 1.4059(18) . ? C18 C23 1.408(2) . ? C19 C20 1.390(2) . ? C19 C24 1.518(2) . ? C20 C21 1.380(2) . ? C20 H20 0.9500 . ? C21 C22 1.386(2) . ? C21 H21 0.9500 . ? C22 C23 1.3933(19) . ? C22 H22 0.9500 . ? C23 C27 1.519(2) . ? C24 C26 1.524(2) . ? C24 C25 1.525(2) . ? C24 H24 1.0000 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C29 1.525(2) . ? C27 C28 1.529(2) . ? C27 H27 1.0000 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 C31 1.5123(19) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 C32 1.4130(19) . ? C32 C33 1.3991(19) . ? C32 H32 0.9500 . ? C33 C34 1.5129(18) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 C40 1.4061(19) . ? C35 C36 1.408(2) . ? C36 C37 1.397(2) . ? C36 C41 1.519(2) . ? C37 C38 1.378(2) . ? C37 H37 0.9500 . ? C38 C39 1.390(2) . ? C38 H38 0.9500 . ? C39 C40 1.391(2) . ? C39 H39 0.9500 . ? C40 C44 1.522(2) . ? C41 C42 1.525(2) . ? C41 C43 1.526(2) . ? C41 H41 1.0000 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 C46 1.520(2) . ? C44 C45 1.5226(19) . ? C44 H44 1.0000 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 C48 1.402(2) . ? C47 C52 1.4138(19) . ? C48 C49 1.394(2) . ? C48 C53 1.522(2) . ? C49 C50 1.389(2) . ? C49 H49 0.9500 . ? C50 C51 1.377(2) . ? C50 H50 0.9500 . ? C51 C52 1.397(2) . ? C51 H51 0.9500 . ? C52 C56 1.518(2) . ? C53 C55 1.531(2) . ? C53 C54 1.533(2) . ? C53 H53 1.0000 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? C56 C58 1.528(3) . ? C56 C57 1.537(2) . ? C56 H56 1.0000 . ? C57 H57A 0.9800 . ? C57 H57B 0.9800 . ? C57 H57C 0.9800 . ? C58 H58A 0.9800 . ? C58 H58B 0.9800 . ? C58 H58C 0.9800 . ? C60 C61 1.367(3) . ? C60 C65 1.371(3) . ? C60 H60 0.9500 . ? C61 C62 1.381(4) . ? C61 H61 0.9500 . ? C62 C63 1.372(4) . ? C62 H62 0.9500 . ? C63 C64 1.369(4) . ? C63 H63 0.9500 . ? C64 C65 1.380(3) . ? C64 H64 0.9500 . ? C65 H65 0.9500 . ? 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 Mg1 N1 128.52(5) . . ? O2 Mg1 N2 118.37(4) . . ? N1 Mg1 N2 94.75(4) . . ? O2 Mg1 O1 66.58(4) . . ? N1 Mg1 O1 120.65(4) . . ? N2 Mg1 O1 130.87(4) . . ? C59 O1 Mg2 87.42(7) . . ? C59 O1 Mg1 86.90(7) . . ? Mg2 O1 Mg1 174.16(5) . . ? C2 N1 C6 118.97(10) . . ? C2 N1 Mg1 123.38(9) . . ? C6 N1 Mg1 117.63(8) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N3 Mg2 O3 120.03(4) . . ? N3 Mg2 N4 95.37(5) . . ? O3 Mg2 N4 117.44(4) . . ? N3 Mg2 O1 125.05(4) . . ? O3 Mg2 O1 66.50(4) . . ? N4 Mg2 O1 132.24(4) . . ? C59 O2 Mg1 90.63(8) . . ? C4 N2 C18 118.74(10) . . ? C4 N2 Mg1 123.28(8) . . ? C18 N2 Mg1 117.96(8) . . ? N1 C2 C3 124.35(12) . . ? N1 C2 C1 119.01(12) . . ? C3 C2 C1 116.63(11) . . ? C59 O3 Mg2 89.99(8) . . ? C31 N3 C35 117.01(11) . . ? C31 N3 Mg2 118.56(9) . . ? C35 N3 Mg2 124.35(8) . . ? C2 C3 C4 130.03(12) . . ? C2 C3 H3 115.0 . . ? C4 C3 H3 115.0 . . ? C33 N4 C47 118.50(10) . . ? C33 N4 Mg2 114.50(9) . . ? C47 N4 Mg2 125.95(8) . . ? N2 C4 C3 124.12(11) . . ? N2 C4 C5 119.82(11) . . ? C3 C4 C5 116.06(11) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C7 C6 C11 120.99(12) . . ? C7 C6 N1 120.28(12) . . ? C11 C6 N1 118.67(12) . . ? C8 C7 C6 118.18(13) . . ? C8 C7 C12 120.01(13) . . ? C6 C7 C12 121.81(12) . . ? C9 C8 C7 121.07(14) . . ? C9 C8 H8 119.5 . . ? C7 C8 H8 119.5 . . ? C10 C9 C8 120.11(13) . . ? C10 C9 H9 119.9 . . ? C8 C9 H9 119.9 . . ? C9 C10 C11 121.21(14) . . ? C9 C10 H10 119.4 . . ? C11 C10 H10 119.4 . . ? C10 C11 C6 118.27(14) . . ? C10 C11 C15 119.86(13) . . ? C6 C11 C15 121.84(12) . . ? C7 C12 C13 111.65(13) . . ? C7 C12 C14 111.91(13) . . ? C13 C12 C14 110.31(14) . . ? C7 C12 H12 107.6 . . ? C13 C12 H12 107.6 . . ? C14 C12 H12 107.6 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C16 C15 C11 112.55(14) . . ? C16 C15 C17 109.79(14) . . ? C11 C15 C17 112.62(13) . . ? C16 C15 H15 107.2 . . ? C11 C15 H15 107.2 . . ? C17 C15 H15 107.2 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C19 C18 C23 121.11(11) . . ? C19 C18 N2 119.32(12) . . ? C23 C18 N2 119.53(11) . . ? C20 C19 C18 118.28(13) . . ? C20 C19 C24 119.93(12) . . ? C18 C19 C24 121.75(12) . . ? C21 C20 C19 121.43(13) . . ? C21 C20 H20 119.3 . . ? C19 C20 H20 119.3 . . ? C20 C21 C22 119.82(12) . . ? C20 C21 H21 120.1 . . ? C22 C21 H21 120.1 . . ? C21 C22 C23 121.07(14) . . ? C21 C22 H22 119.5 . . ? C23 C22 H22 119.5 . . ? C22 C23 C18 118.28(13) . . ? C22 C23 C27 121.05(13) . . ? C18 C23 C27 120.66(11) . . ? C19 C24 C26 110.40(13) . . ? C19 C24 C25 112.72(12) . . ? C26 C24 C25 110.52(13) . . ? C19 C24 H24 107.7 . . ? C26 C24 H24 107.7 . . ? C25 C24 H24 107.7 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C23 C27 C29 112.88(13) . . ? C23 C27 C28 110.62(12) . . ? C29 C27 C28 109.93(13) . . ? C23 C27 H27 107.7 . . ? C29 C27 H27 107.7 . . ? C28 C27 H27 107.7 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C31 C30 H30A 109.5 . . ? C31 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C31 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? N3 C31 C32 123.08(12) . . ? N3 C31 C30 120.47(12) . . ? C32 C31 C30 116.44(11) . . ? C33 C32 C31 129.89(12) . . ? C33 C32 H32 115.1 . . ? C31 C32 H32 115.1 . . ? N4 C33 C32 124.63(12) . . ? N4 C33 C34 119.79(12) . . ? C32 C33 C34 115.58(12) . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C40 C35 C36 121.71(12) . . ? C40 C35 N3 119.34(12) . . ? C36 C35 N3 118.94(12) . . ? C37 C36 C35 117.64(13) . . ? C37 C36 C41 120.39(13) . . ? C35 C36 C41 121.94(12) . . ? C38 C37 C36 121.28(15) . . ? C38 C37 H37 119.4 . . ? C36 C37 H37 119.4 . . ? C37 C38 C39 120.26(14) . . ? C37 C38 H38 119.9 . . ? C39 C38 H38 119.9 . . ? C38 C39 C40 120.81(14) . . ? C38 C39 H39 119.6 . . ? C40 C39 H39 119.6 . . ? C39 C40 C35 118.19(13) . . ? C39 C40 C44 120.82(13) . . ? C35 C40 C44 120.97(12) . . ? C36 C41 C42 112.17(12) . . ? C36 C41 C43 111.73(12) . . ? C42 C41 C43 110.40(13) . . ? C36 C41 H41 107.4 . . ? C42 C41 H41 107.4 . . ? C43 C41 H41 107.4 . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C41 C43 H43A 109.5 . . ? C41 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C41 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C46 C44 C40 113.54(13) . . ? C46 C44 C45 110.14(13) . . ? C40 C44 C45 110.26(12) . . ? C46 C44 H44 107.6 . . ? C40 C44 H44 107.6 . . ? C45 C44 H44 107.6 . . ? C44 C45 H45A 109.5 . . ? C44 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C44 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C44 C46 H46A 109.5 . . ? C44 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C44 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C48 C47 C52 120.36(12) . . ? C48 C47 N4 121.24(12) . . ? C52 C47 N4 118.33(12) . . ? C49 C48 C47 119.10(13) . . ? C49 C48 C53 118.90(13) . . ? C47 C48 C53 121.99(12) . . ? C50 C49 C48 120.97(14) . . ? C50 C49 H49 119.5 . . ? C48 C49 H49 119.5 . . ? C51 C50 C49 119.55(13) . . ? C51 C50 H50 120.2 . . ? C49 C50 H50 120.2 . . ? C50 C51 C52 121.63(13) . . ? C50 C51 H51 119.2 . . ? C52 C51 H51 119.2 . . ? C51 C52 C47 118.32(13) . . ? C51 C52 C56 120.28(13) . . ? C47 C52 C56 121.40(12) . . ? C48 C53 C55 112.20(13) . . ? C48 C53 C54 110.01(13) . . ? C55 C53 C54 110.89(15) . . ? C48 C53 H53 107.9 . . ? C55 C53 H53 107.9 . . ? C54 C53 H53 107.9 . . ? C53 C54 H54A 109.5 . . ? C53 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C53 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C53 C55 H55A 109.5 . . ? C53 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? C53 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? C52 C56 C58 111.79(14) . . ? C52 C56 C57 113.57(13) . . ? C58 C56 C57 108.23(14) . . ? C52 C56 H56 107.7 . . ? C58 C56 H56 107.7 . . ? C57 C56 H56 107.7 . . ? C56 C57 H57A 109.5 . . ? C56 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? C56 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? C56 C58 H58A 109.5 . . ? C56 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? C56 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? O2 C59 O3 128.04(12) . . ? O2 C59 O1 115.89(10) . . ? O3 C59 O1 116.07(11) . . ? C61 C60 C65 120.3(2) . . ? C61 C60 H60 119.8 . . ? C65 C60 H60 119.8 . . ? C60 C61 C62 119.5(2) . . ? C60 C61 H61 120.3 . . ? C62 C61 H61 120.3 . . ? C63 C62 C61 120.4(2) . . ? C63 C62 H62 119.8 . . ? C61 C62 H62 119.8 . . ? C64 C63 C62 119.9(2) . . ? C64 C63 H63 120.1 . . ? C62 C63 H63 120.1 . . ? C63 C64 C65 119.8(2) . . ? C63 C64 H64 120.1 . . ? C65 C64 H64 120.1 . . ? C60 C65 C64 120.1(2) . . ? C60 C65 H65 119.9 . . ? C64 C65 H65 119.9 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 66.99 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.194 _refine_diff_density_min -0.239 _refine_diff_density_rms 0.032 _database_code_depnum_ccdc_archive 'CCDC 955167' ####################################################################### # # 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_ccompound1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C59 H82 Mg2 N4 O3' _chemical_formula_weight 943.91 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mg Mg 0.0486 0.0363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 48.559(3) _cell_length_b 13.6700(9) _cell_length_c 17.5247(11) _cell_angle_alpha 90.00 _cell_angle_beta 103.460(3) _cell_angle_gamma 90.00 _cell_volume 11313.4(12) _cell_formula_units_Z 8 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.108 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4096 _exptl_absorpt_coefficient_mu 0.087 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.974 _exptl_absorpt_correction_T_max 0.987 _exptl_absorpt_process_details 'Sortav (Blessing, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(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 'Bruker Apex' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 48150 _diffrn_reflns_av_R_equivalents 0.0645 _diffrn_reflns_av_sigmaI/netI 0.0612 _diffrn_reflns_limit_h_min -57 _diffrn_reflns_limit_h_max 49 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.39 _diffrn_reflns_theta_max 25.00 _reflns_number_total 9945 _reflns_number_gt 6542 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0549P)^2^+10.8219P] 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 9945 _refine_ls_number_parameters 633 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0948 _refine_ls_R_factor_gt 0.0524 _refine_ls_wR_factor_ref 0.1347 _refine_ls_wR_factor_gt 0.1137 _refine_ls_goodness_of_fit_ref 1.005 _refine_ls_restrained_S_all 1.005 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mg1 Mg 0.135549(15) 0.68495(6) 0.06257(4) 0.0232(2) Uani 1 1 d . . . O1 O 0.12481(3) 0.76714(12) 0.14713(9) 0.0235(4) Uani 1 1 d . . . N1 N 0.17379(4) 0.62503(15) 0.06827(10) 0.0223(5) Uani 1 1 d . . . C1 C 0.20820(5) 0.5663(2) -0.00435(15) 0.0337(7) Uani 1 1 d . . . H1A H 0.2210 0.6198 0.0178 0.051 Uiso 1 1 calc R . . H1B H 0.2085 0.5571 -0.0596 0.051 Uiso 1 1 calc R . . H1C H 0.2144 0.5059 0.0247 0.051 Uiso 1 1 calc R . . Mg2 Mg 0.113946(15) 0.86395(6) 0.22404(4) 0.0247(2) Uani 1 1 d . . . O2 O 0.13298(4) 0.82811(13) 0.03742(9) 0.0313(4) Uani 1 1 d . . . N2 N 0.11379(4) 0.59441(14) -0.02096(11) 0.0226(5) Uani 1 1 d . . . C2 C 0.17843(4) 0.59103(18) 0.00184(13) 0.0234(5) Uani 1 1 d . . . O3 O 0.12114(3) 0.92727(13) 0.12809(9) 0.0303(4) Uani 1 1 d . . . N3 N 0.07550(4) 0.86287(15) 0.24748(10) 0.0236(5) Uani 1 1 d . . . C3 C 0.15707(5) 0.57301(18) -0.06532(13) 0.0249(6) Uani 1 1 d . . . H3 H 0.1636 0.5605 -0.1115 0.030 Uiso 1 1 calc R . . N4 N 0.13457(4) 0.90668(14) 0.33175(11) 0.0227(4) Uani 1 1 d . . . C4 C 0.12753(5) 0.57038(18) -0.07562(13) 0.0249(5) Uani 1 1 d . . . C5 C 0.11132(5) 0.5377(2) -0.15567(14) 0.0394(7) Uani 1 1 d . . . H5A H 0.0975 0.4877 -0.1500 0.059 Uiso 1 1 calc R . . H5B H 0.1245 0.5105 -0.1847 0.059 Uiso 1 1 calc R . . H5C H 0.1014 0.5939 -0.1844 0.059 Uiso 1 1 calc R . . C6 C 0.19705(4) 0.6282(2) 0.13605(13) 0.0280(6) Uani 1 1 d . . . C7 C 0.21208(5) 0.7159(2) 0.15591(15) 0.0394(7) Uani 1 1 d . . . C8 C 0.23386(6) 0.7152(3) 0.22292(19) 0.0576(10) Uani 1 1 d . . . H8 H 0.2443 0.7736 0.2381 0.069 Uiso 1 1 calc R . . C9 C 0.24078(6) 0.6330(3) 0.26784(19) 0.0658(12) Uani 1 1 d . . . H9 H 0.2561 0.6348 0.3128 0.079 Uiso 1 1 calc R . . C10 C 0.22568(6) 0.5477(3) 0.24838(16) 0.0532(9) Uani 1 1 d . . . H10 H 0.2304 0.4914 0.2805 0.064 Uiso 1 1 calc R . . C11 C 0.20339(5) 0.5435(2) 0.18152(14) 0.0349(7) Uani 1 1 d . . . C12 C 0.20555(6) 0.8076(2) 0.10809(17) 0.0459(8) Uani 1 1 d . . . H12 H 0.1887 0.7940 0.0644 0.055 Uiso 1 1 calc R . . C13 C 0.19785(6) 0.8932(2) 0.15616(19) 0.0551(9) Uani 1 1 d . . . H13A H 0.1827 0.8728 0.1812 0.083 Uiso 1 1 calc R . . H13B H 0.1914 0.9488 0.1214 0.083 Uiso 1 1 calc R . . H13C H 0.2146 0.9124 0.1965 0.083 Uiso 1 1 calc R . . C14 C 0.22986(8) 0.8384(3) 0.0710(2) 0.0772(13) Uani 1 1 d . . . H14A H 0.2467 0.8528 0.1125 0.116 Uiso 1 1 calc R . . H14B H 0.2243 0.8970 0.0389 0.116 Uiso 1 1 calc R . . H14C H 0.2341 0.7852 0.0381 0.116 Uiso 1 1 calc R . . C15 C 0.18597(5) 0.4514(2) 0.16149(15) 0.0367(7) Uani 1 1 d . . . H15 H 0.1775 0.4528 0.1038 0.044 Uiso 1 1 calc R . . C16 C 0.16147(6) 0.4505(2) 0.20282(17) 0.0491(8) Uani 1 1 d . . . H16A H 0.1690 0.4488 0.2598 0.074 Uiso 1 1 calc R . . H16B H 0.1497 0.3926 0.1865 0.074 Uiso 1 1 calc R . . H16C H 0.1500 0.5096 0.1887 0.074 Uiso 1 1 calc R . . C17 C 0.20297(7) 0.3570(2) 0.17897(19) 0.0572(9) Uani 1 1 d . . . H17A H 0.2195 0.3604 0.1558 0.086 Uiso 1 1 calc R . . H17B H 0.1911 0.3015 0.1564 0.086 Uiso 1 1 calc R . . H17C H 0.2093 0.3484 0.2359 0.086 Uiso 1 1 calc R . . C18 C 0.08373(4) 0.57550(19) -0.03694(13) 0.0241(6) Uani 1 1 d . . . C19 C 0.06456(5) 0.6483(2) -0.07150(14) 0.0290(6) Uani 1 1 d . . . C20 C 0.03561(5) 0.6270(2) -0.08398(15) 0.0368(7) Uani 1 1 d . . . H20 H 0.0221 0.6752 -0.1070 0.044 Uiso 1 1 calc R . . C21 C 0.02634(5) 0.5383(2) -0.06367(15) 0.0362(7) Uani 1 1 d . . . H21 H 0.0066 0.5253 -0.0736 0.043 Uiso 1 1 calc R . . C22 C 0.04543(5) 0.4680(2) -0.02898(15) 0.0339(6) Uani 1 1 d . . . H22 H 0.0387 0.4068 -0.0150 0.041 Uiso 1 1 calc R . . C23 C 0.07451(5) 0.48522(19) -0.01413(14) 0.0275(6) Uani 1 1 d . . . C24 C 0.07382(5) 0.7477(2) -0.09360(15) 0.0370(7) Uani 1 1 d . . . H24 H 0.0950 0.7478 -0.0826 0.044 Uiso 1 1 calc R . . C25 C 0.06492(6) 0.8275(2) -0.0434(2) 0.0515(8) Uani 1 1 d . . . H25A H 0.0442 0.8329 -0.0563 0.077 Uiso 1 1 calc R . . H25B H 0.0732 0.8901 -0.0540 0.077 Uiso 1 1 calc R . . H25C H 0.0717 0.8109 0.0122 0.077 Uiso 1 1 calc R . . C26 C 0.06259(7) 0.7704(3) -0.18036(19) 0.0655(10) Uani 1 1 d . . . H26A H 0.0687 0.7193 -0.2119 0.098 Uiso 1 1 calc R . . H26B H 0.0700 0.8338 -0.1925 0.098 Uiso 1 1 calc R . . H26C H 0.0419 0.7728 -0.1924 0.098 Uiso 1 1 calc R . . C27 C 0.09522(6) 0.4080(2) 0.02657(17) 0.0405(7) Uani 1 1 d . . . H27 H 0.1125 0.4435 0.0556 0.049 Uiso 1 1 calc R . . C28 C 0.08459(8) 0.3487(3) 0.0866(2) 0.0681(10) Uani 1 1 d . . . H28A H 0.0693 0.3052 0.0598 0.102 Uiso 1 1 calc R . . H28B H 0.0774 0.3929 0.1215 0.102 Uiso 1 1 calc R . . H28C H 0.1002 0.3095 0.1176 0.102 Uiso 1 1 calc R . . C29 C 0.10462(10) 0.3397(3) -0.0290(3) 0.1025(17) Uani 1 1 d . . . H29A H 0.0882 0.3047 -0.0600 0.154 Uiso 1 1 calc R . . H29B H 0.1182 0.2925 0.0008 0.154 Uiso 1 1 calc R . . H29C H 0.1137 0.3770 -0.0641 0.154 Uiso 1 1 calc R . . C30 C 0.04150(5) 0.8835(2) 0.33022(15) 0.0408(7) Uani 1 1 d . . . H30A H 0.0299 0.9313 0.2952 0.061 Uiso 1 1 calc R . . H30B H 0.0420 0.9005 0.3848 0.061 Uiso 1 1 calc R . . H30C H 0.0333 0.8181 0.3187 0.061 Uiso 1 1 calc R . . C31 C 0.07122(5) 0.88427(19) 0.31781(13) 0.0263(6) Uani 1 1 d . . . C32 C 0.09262(5) 0.90867(19) 0.38308(13) 0.0272(6) Uani 1 1 d . . . H32 H 0.0864 0.9190 0.4300 0.033 Uiso 1 1 calc R . . C33 C 0.12184(5) 0.92041(18) 0.39040(13) 0.0242(5) Uani 1 1 d . . . C34 C 0.13892(5) 0.9496(2) 0.47013(14) 0.0331(6) Uani 1 1 d . . . H34A H 0.1530 0.8990 0.4901 0.050 Uiso 1 1 calc R . . H34B H 0.1263 0.9570 0.5061 0.050 Uiso 1 1 calc R . . H34C H 0.1485 1.0118 0.4662 0.050 Uiso 1 1 calc R . . C35 C 0.05132(5) 0.83985(19) 0.18502(13) 0.0246(6) Uani 1 1 d . . . C36 C 0.03700(5) 0.91557(19) 0.13752(14) 0.0275(6) Uani 1 1 d . . . C37 C 0.01464(5) 0.8898(2) 0.07586(14) 0.0323(6) Uani 1 1 d . . . H37 H 0.0046 0.9398 0.0432 0.039 Uiso 1 1 calc R . . C38 C 0.00654(5) 0.7940(2) 0.06069(14) 0.0315(6) Uani 1 1 d . . . H38 H -0.0089 0.7787 0.0181 0.038 Uiso 1 1 calc R . . C39 C 0.02077(5) 0.7206(2) 0.10708(14) 0.0294(6) Uani 1 1 d . . . H39 H 0.0152 0.6546 0.0960 0.035 Uiso 1 1 calc R . . C40 C 0.04339(5) 0.74192(19) 0.17057(13) 0.0260(6) Uani 1 1 d . . . C41 C 0.04548(5) 1.0218(2) 0.15026(15) 0.0354(7) Uani 1 1 d . . . H41 H 0.0597 1.0267 0.2016 0.043 Uiso 1 1 calc R . . C42 C 0.05961(6) 1.0586(2) 0.08649(18) 0.0457(8) Uani 1 1 d . . . H42A H 0.0760 1.0172 0.0851 0.069 Uiso 1 1 calc R . . H42B H 0.0659 1.1263 0.0979 0.069 Uiso 1 1 calc R . . H42C H 0.0460 1.0559 0.0355 0.069 Uiso 1 1 calc R . . C43 C 0.02043(6) 1.0876(2) 0.15490(16) 0.0433(7) Uani 1 1 d . . . H43A H 0.0063 1.0855 0.1048 0.065 Uiso 1 1 calc R . . H43B H 0.0271 1.1549 0.1660 0.065 Uiso 1 1 calc R . . H43C H 0.0118 1.0644 0.1969 0.065 Uiso 1 1 calc R . . C44 C 0.05853(5) 0.65844(19) 0.21944(14) 0.0295(6) Uani 1 1 d . . . H44 H 0.0737 0.6870 0.2623 0.035 Uiso 1 1 calc R . . C45 C 0.07269(6) 0.5928(2) 0.17012(16) 0.0404(7) Uani 1 1 d . . . H45A H 0.0582 0.5626 0.1283 0.061 Uiso 1 1 calc R . . H45B H 0.0834 0.5415 0.2034 0.061 Uiso 1 1 calc R . . H45C H 0.0856 0.6317 0.1468 0.061 Uiso 1 1 calc R . . C46 C 0.03869(6) 0.5995(2) 0.25760(17) 0.0453(8) Uani 1 1 d . . . H46A H 0.0303 0.6426 0.2908 0.068 Uiso 1 1 calc R . . H46B H 0.0494 0.5473 0.2898 0.068 Uiso 1 1 calc R . . H46C H 0.0236 0.5706 0.2167 0.068 Uiso 1 1 calc R . . C47 C 0.16442(5) 0.92834(19) 0.34564(13) 0.0250(6) Uani 1 1 d . . . C48 C 0.17265(5) 1.0210(2) 0.32480(15) 0.0351(7) Uani 1 1 d . . . C49 C 0.20147(6) 1.0391(3) 0.33540(18) 0.0493(8) Uani 1 1 d . . . H49 H 0.2077 1.1014 0.3220 0.059 Uiso 1 1 calc R . . C50 C 0.22105(6) 0.9686(3) 0.36478(18) 0.0529(9) Uani 1 1 d . . . H50 H 0.2406 0.9825 0.3714 0.064 Uiso 1 1 calc R . . C51 C 0.21275(5) 0.8778(3) 0.38482(16) 0.0469(8) Uani 1 1 d . . . H51 H 0.2267 0.8299 0.4051 0.056 Uiso 1 1 calc R . . C52 C 0.18415(5) 0.8549(2) 0.37594(14) 0.0302(6) Uani 1 1 d . . . C53 C 0.15155(7) 1.1001(2) 0.29242(18) 0.0499(8) Uani 1 1 d . . . H53 H 0.1321 1.0724 0.2873 0.060 Uiso 1 1 calc R . . C54 C 0.15406(8) 1.1333(3) 0.21092(19) 0.0684(10) Uani 1 1 d . . . H54A H 0.1732 1.1588 0.2140 0.103 Uiso 1 1 calc R . . H54B H 0.1401 1.1847 0.1918 0.103 Uiso 1 1 calc R . . H54C H 0.1505 1.0776 0.1747 0.103 Uiso 1 1 calc R . . C55 C 0.15477(10) 1.1879(3) 0.3481(2) 0.0810(12) Uani 1 1 d . . . H55A H 0.1517 1.1668 0.3989 0.122 Uiso 1 1 calc R . . H55B H 0.1408 1.2380 0.3256 0.122 Uiso 1 1 calc R . . H55C H 0.1739 1.2151 0.3553 0.122 Uiso 1 1 calc R . . C56 C 0.17476(6) 0.7557(2) 0.39733(15) 0.0366(7) Uani 1 1 d . . . H56 H 0.1557 0.7642 0.4088 0.044 Uiso 1 1 calc R . . C57 C 0.17126(7) 0.6842(2) 0.32914(17) 0.0481(8) Uani 1 1 d . . . H57A H 0.1579 0.7112 0.2833 0.072 Uiso 1 1 calc R . . H57B H 0.1640 0.6218 0.3439 0.072 Uiso 1 1 calc R . . H57C H 0.1896 0.6735 0.3163 0.072 Uiso 1 1 calc R . . C58 C 0.19407(9) 0.7123(3) 0.4706(2) 0.0805(12) Uani 1 1 d . . . H58A H 0.2120 0.6926 0.4588 0.121 Uiso 1 1 calc R . . H58B H 0.1849 0.6551 0.4876 0.121 Uiso 1 1 calc R . . H58C H 0.1977 0.7614 0.5125 0.121 Uiso 1 1 calc R . . C59 C 0.12648(5) 0.8455(2) 0.10137(13) 0.0256(6) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mg1 0.0196(4) 0.0264(5) 0.0241(4) -0.0027(4) 0.0058(3) -0.0005(3) O1 0.0235(8) 0.0242(10) 0.0236(8) -0.0011(8) 0.0073(7) 0.0004(7) N1 0.0171(9) 0.0288(13) 0.0210(10) -0.0049(9) 0.0046(8) -0.0024(8) C1 0.0222(13) 0.0470(19) 0.0336(14) -0.0114(13) 0.0096(11) -0.0041(12) Mg2 0.0210(4) 0.0302(5) 0.0232(4) -0.0029(4) 0.0055(3) 0.0002(3) O2 0.0430(10) 0.0299(11) 0.0253(9) -0.0022(8) 0.0166(8) -0.0011(8) N2 0.0172(9) 0.0250(12) 0.0248(10) 0.0009(9) 0.0031(8) -0.0008(8) C2 0.0196(12) 0.0243(15) 0.0275(13) 0.0002(11) 0.0079(10) -0.0042(10) O3 0.0390(10) 0.0239(11) 0.0299(9) -0.0025(8) 0.0121(8) 0.0033(8) N3 0.0204(10) 0.0293(13) 0.0201(10) -0.0013(9) 0.0027(8) 0.0018(8) C3 0.0252(12) 0.0305(16) 0.0209(12) -0.0038(11) 0.0092(10) -0.0005(11) N4 0.0194(10) 0.0232(12) 0.0257(10) -0.0008(9) 0.0055(8) -0.0021(8) C4 0.0263(13) 0.0251(15) 0.0227(12) -0.0029(11) 0.0042(10) -0.0007(10) C5 0.0264(14) 0.061(2) 0.0291(14) -0.0108(14) 0.0037(11) -0.0024(13) C6 0.0129(11) 0.0464(18) 0.0247(13) -0.0107(12) 0.0042(10) 0.0006(11) C7 0.0213(13) 0.063(2) 0.0358(15) -0.0204(15) 0.0113(12) -0.0119(13) C8 0.0238(15) 0.097(3) 0.051(2) -0.033(2) 0.0067(14) -0.0127(17) C9 0.0214(15) 0.122(4) 0.0456(19) -0.039(2) -0.0101(14) 0.0107(19) C10 0.0342(16) 0.086(3) 0.0344(16) -0.0108(17) -0.0010(13) 0.0274(17) C11 0.0235(13) 0.056(2) 0.0237(13) -0.0072(13) 0.0031(11) 0.0120(12) C12 0.0425(17) 0.054(2) 0.0475(17) -0.0219(16) 0.0223(14) -0.0289(15) C13 0.0502(19) 0.059(2) 0.060(2) -0.0255(18) 0.0210(16) -0.0168(16) C14 0.082(3) 0.074(3) 0.098(3) -0.037(2) 0.066(2) -0.043(2) C15 0.0374(15) 0.047(2) 0.0253(13) 0.0046(13) 0.0065(12) 0.0147(13) C16 0.0449(17) 0.061(2) 0.0438(17) -0.0029(16) 0.0143(14) 0.0064(15) C17 0.059(2) 0.059(2) 0.056(2) 0.0168(17) 0.0172(16) 0.0278(17) C18 0.0173(11) 0.0305(16) 0.0234(12) -0.0039(11) 0.0027(10) -0.0030(10) C19 0.0230(13) 0.0351(17) 0.0278(13) 0.0002(12) 0.0042(11) -0.0013(11) C20 0.0209(13) 0.048(2) 0.0387(15) -0.0016(14) 0.0022(11) 0.0028(12) C21 0.0194(13) 0.047(2) 0.0416(16) -0.0090(14) 0.0058(12) -0.0068(12) C22 0.0320(14) 0.0342(17) 0.0372(15) -0.0071(13) 0.0115(12) -0.0116(12) C23 0.0271(13) 0.0275(16) 0.0282(13) -0.0040(11) 0.0072(11) -0.0026(11) C24 0.0263(14) 0.0391(19) 0.0432(16) 0.0114(14) 0.0035(12) 0.0059(12) C25 0.0364(16) 0.035(2) 0.084(2) 0.0080(17) 0.0159(16) 0.0043(13) C26 0.053(2) 0.080(3) 0.057(2) 0.035(2) 0.0008(17) 0.0024(18) C27 0.0332(15) 0.0284(17) 0.0566(18) 0.0063(14) 0.0037(13) -0.0054(12) C28 0.088(3) 0.044(2) 0.077(2) 0.0208(19) 0.029(2) 0.0189(19) C29 0.145(4) 0.076(3) 0.103(3) 0.023(3) 0.063(3) 0.063(3) C30 0.0259(14) 0.067(2) 0.0315(15) -0.0054(14) 0.0100(12) -0.0005(13) C31 0.0248(12) 0.0301(16) 0.0251(13) 0.0001(11) 0.0080(10) 0.0035(11) C32 0.0268(13) 0.0350(17) 0.0216(12) -0.0044(11) 0.0093(10) 0.0038(11) C33 0.0271(13) 0.0225(15) 0.0233(12) -0.0018(11) 0.0064(10) 0.0030(10) C34 0.0307(14) 0.0413(18) 0.0262(13) -0.0071(12) 0.0047(11) 0.0000(12) C35 0.0190(12) 0.0333(17) 0.0218(12) -0.0006(11) 0.0052(10) -0.0010(10) C36 0.0248(12) 0.0301(16) 0.0267(13) 0.0020(11) 0.0042(10) -0.0004(11) C37 0.0268(13) 0.0384(18) 0.0280(13) 0.0083(12) -0.0009(11) 0.0003(12) C38 0.0262(13) 0.0379(18) 0.0266(13) 0.0022(12) -0.0018(11) -0.0051(12) C39 0.0246(13) 0.0310(16) 0.0307(14) 0.0016(12) 0.0024(11) -0.0059(11) C40 0.0201(12) 0.0334(17) 0.0247(13) 0.0027(11) 0.0053(10) 0.0003(11) C41 0.0329(14) 0.0315(17) 0.0347(15) 0.0015(13) -0.0067(12) -0.0014(12) C42 0.0375(16) 0.0297(18) 0.070(2) 0.0119(15) 0.0134(15) 0.0013(13) C43 0.0473(17) 0.0396(19) 0.0414(16) -0.0062(14) 0.0073(14) 0.0032(14) C44 0.0265(13) 0.0323(17) 0.0271(13) 0.0046(12) 0.0008(11) -0.0022(11) C45 0.0445(16) 0.0379(19) 0.0397(16) 0.0072(14) 0.0114(13) 0.0091(13) C46 0.0384(16) 0.053(2) 0.0445(17) 0.0198(15) 0.0093(13) 0.0063(14) C47 0.0226(12) 0.0302(16) 0.0222(12) -0.0085(11) 0.0053(10) -0.0052(11) C48 0.0389(15) 0.0335(18) 0.0358(15) -0.0101(13) 0.0146(12) -0.0108(12) C49 0.0489(19) 0.051(2) 0.0523(19) -0.0225(16) 0.0215(16) -0.0273(16) C50 0.0268(16) 0.082(3) 0.0511(19) -0.0251(19) 0.0107(14) -0.0225(17) C51 0.0243(14) 0.075(3) 0.0392(16) -0.0104(16) 0.0025(12) 0.0056(15) C52 0.0248(13) 0.0412(18) 0.0237(13) -0.0040(12) 0.0040(10) 0.0027(11) C53 0.064(2) 0.0274(19) 0.062(2) 0.0013(16) 0.0227(17) -0.0049(15) C54 0.104(3) 0.040(2) 0.059(2) 0.0057(18) 0.016(2) -0.0049(19) C55 0.139(4) 0.040(2) 0.075(3) -0.005(2) 0.048(3) 0.012(2) C56 0.0392(15) 0.0394(19) 0.0311(14) 0.0071(13) 0.0080(12) 0.0162(13) C57 0.0588(19) 0.043(2) 0.0456(17) 0.0029(15) 0.0178(15) 0.0026(15) C58 0.105(3) 0.072(3) 0.052(2) 0.017(2) -0.007(2) 0.020(2) C59 0.0233(12) 0.0286(16) 0.0244(13) 0.0031(12) 0.0045(10) -0.0007(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mg1 O2 2.0035(19) . ? Mg1 N1 2.0107(19) . ? Mg1 N2 2.018(2) . ? Mg1 O1 2.0223(17) . ? O1 C59 1.352(3) . ? O1 Mg2 2.0440(17) . ? N1 C2 1.321(3) . ? N1 C6 1.437(3) . ? C1 C2 1.513(3) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? Mg2 O3 1.9930(18) . ? Mg2 N3 2.0027(19) . ? Mg2 N4 2.007(2) . ? O2 C59 1.256(3) . ? N2 C4 1.330(3) . ? N2 C18 1.444(3) . ? C2 C3 1.398(3) . ? O3 C59 1.262(3) . ? N3 C31 1.329(3) . ? N3 C35 1.441(3) . ? C3 C4 1.404(3) . ? C3 H3 0.9500 . ? N4 C33 1.330(3) . ? N4 C47 1.443(3) . ? C4 C5 1.507(3) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 C11 1.400(4) . ? C6 C7 1.404(4) . ? C7 C8 1.386(4) . ? C7 C12 1.500(4) . ? C8 C9 1.368(5) . ? C8 H8 0.9500 . ? C9 C10 1.378(5) . ? C9 H9 0.9500 . ? C10 C11 1.399(4) . ? C10 H10 0.9500 . ? C11 C15 1.511(4) . ? C12 C14 1.532(4) . ? C12 C13 1.537(4) . ? C12 H12 1.0000 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C17 1.524(4) . ? C15 C16 1.530(4) . ? C15 H15 1.0000 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C19 1.400(3) . ? C18 C23 1.402(3) . ? C19 C20 1.402(3) . ? C19 C24 1.510(4) . ? C20 C21 1.369(4) . ? C20 H20 0.9500 . ? C21 C22 1.376(4) . ? C21 H21 0.9500 . ? C22 C23 1.395(3) . ? C22 H22 0.9500 . ? C23 C27 1.517(4) . ? C24 C26 1.523(4) . ? C24 C25 1.525(4) . ? C24 H24 1.0000 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C29 1.495(5) . ? C27 C28 1.512(4) . ? C27 H27 1.0000 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 C31 1.509(3) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 C32 1.395(3) . ? C32 C33 1.404(3) . ? C32 H32 0.9500 . ? C33 C34 1.503(3) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 C40 1.400(3) . ? C35 C36 1.407(3) . ? C36 C37 1.388(3) . ? C36 C41 1.512(4) . ? C37 C38 1.375(4) . ? C37 H37 0.9500 . ? C38 C39 1.372(3) . ? C38 H38 0.9500 . ? C39 C40 1.400(3) . ? C39 H39 0.9500 . ? C40 C44 1.511(3) . ? C41 C42 1.526(4) . ? C41 C43 1.530(4) . ? C41 H41 1.0000 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 C45 1.517(4) . ? C44 C46 1.525(3) . ? C44 H44 1.0000 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 C48 1.402(4) . ? C47 C52 1.404(3) . ? C48 C49 1.390(4) . ? C48 C53 1.507(4) . ? C49 C50 1.367(5) . ? C49 H49 0.9500 . ? C50 C51 1.376(4) . ? C50 H50 0.9500 . ? C51 C52 1.397(3) . ? C51 H51 0.9500 . ? C52 C56 1.506(4) . ? C53 C54 1.530(4) . ? C53 C55 1.531(4) . ? C53 H53 1.0000 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? C56 C57 1.522(4) . ? C56 C58 1.522(4) . ? C56 H56 1.0000 . ? C57 H57A 0.9800 . ? C57 H57B 0.9800 . ? C57 H57C 0.9800 . ? C58 H58A 0.9800 . ? C58 H58B 0.9800 . ? C58 H58C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Mg1 N1 114.74(8) . . ? O2 Mg1 N2 116.38(8) . . ? N1 Mg1 N2 96.18(8) . . ? O2 Mg1 O1 66.74(7) . . ? N1 Mg1 O1 125.63(8) . . ? N2 Mg1 O1 133.76(7) . . ? C59 O1 Mg1 86.81(13) . . ? C59 O1 Mg2 86.46(13) . . ? Mg1 O1 Mg2 173.26(9) . . ? C2 N1 C6 118.49(18) . . ? C2 N1 Mg1 116.40(15) . . ? C6 N1 Mg1 124.60(14) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? O3 Mg2 N3 122.07(8) . . ? O3 Mg2 N4 121.34(8) . . ? N3 Mg2 N4 95.41(8) . . ? O3 Mg2 O1 66.55(7) . . ? N3 Mg2 O1 121.77(8) . . ? N4 Mg2 O1 131.28(8) . . ? C59 O2 Mg1 90.26(15) . . ? C4 N2 C18 118.04(18) . . ? C4 N2 Mg1 114.10(15) . . ? C18 N2 Mg1 125.83(15) . . ? N1 C2 C3 124.0(2) . . ? N1 C2 C1 120.3(2) . . ? C3 C2 C1 115.8(2) . . ? C59 O3 Mg2 91.15(14) . . ? C31 N3 C35 118.47(18) . . ? C31 N3 Mg2 122.88(15) . . ? C35 N3 Mg2 118.63(14) . . ? C2 C3 C4 130.4(2) . . ? C2 C3 H3 114.8 . . ? C4 C3 H3 114.8 . . ? C33 N4 C47 118.01(19) . . ? C33 N4 Mg2 123.22(15) . . ? C47 N4 Mg2 118.70(14) . . ? N2 C4 C3 124.8(2) . . ? N2 C4 C5 120.2(2) . . ? C3 C4 C5 115.1(2) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C11 C6 C7 122.2(2) . . ? C11 C6 N1 118.2(2) . . ? C7 C6 N1 119.6(2) . . ? C8 C7 C6 117.0(3) . . ? C8 C7 C12 120.0(3) . . ? C6 C7 C12 123.0(2) . . ? C9 C8 C7 122.0(3) . . ? C9 C8 H8 119.0 . . ? C7 C8 H8 119.0 . . ? C8 C9 C10 120.5(3) . . ? C8 C9 H9 119.7 . . ? C10 C9 H9 119.7 . . ? C9 C10 C11 120.4(3) . . ? C9 C10 H10 119.8 . . ? C11 C10 H10 119.8 . . ? C10 C11 C6 117.9(3) . . ? C10 C11 C15 120.7(3) . . ? C6 C11 C15 121.4(2) . . ? C7 C12 C14 112.5(3) . . ? C7 C12 C13 112.1(2) . . ? C14 C12 C13 109.4(2) . . ? C7 C12 H12 107.5 . . ? C14 C12 H12 107.5 . . ? C13 C12 H12 107.5 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C11 C15 C17 114.2(2) . . ? C11 C15 C16 110.6(2) . . ? C17 C15 C16 110.0(2) . . ? C11 C15 H15 107.2 . . ? C17 C15 H15 107.2 . . ? C16 C15 H15 107.2 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C19 C18 C23 121.6(2) . . ? C19 C18 N2 119.8(2) . . ? C23 C18 N2 118.5(2) . . ? C18 C19 C20 117.5(2) . . ? C18 C19 C24 122.9(2) . . ? C20 C19 C24 119.6(2) . . ? C21 C20 C19 121.4(3) . . ? C21 C20 H20 119.3 . . ? C19 C20 H20 119.3 . . ? C20 C21 C22 120.4(2) . . ? C20 C21 H21 119.8 . . ? C22 C21 H21 119.8 . . ? C21 C22 C23 120.9(3) . . ? C21 C22 H22 119.6 . . ? C23 C22 H22 119.6 . . ? C22 C23 C18 118.2(2) . . ? C22 C23 C27 120.1(2) . . ? C18 C23 C27 121.7(2) . . ? C19 C24 C26 112.4(2) . . ? C19 C24 C25 110.8(2) . . ? C26 C24 C25 110.2(3) . . ? C19 C24 H24 107.7 . . ? C26 C24 H24 107.7 . . ? C25 C24 H24 107.7 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C29 C27 C28 108.9(3) . . ? C29 C27 C23 113.5(3) . . ? C28 C27 C23 113.8(2) . . ? C29 C27 H27 106.7 . . ? C28 C27 H27 106.7 . . ? C23 C27 H27 106.7 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C31 C30 H30A 109.5 . . ? C31 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C31 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? N3 C31 C32 124.4(2) . . ? N3 C31 C30 119.6(2) . . ? C32 C31 C30 116.0(2) . . ? C31 C32 C33 130.3(2) . . ? C31 C32 H32 114.9 . . ? C33 C32 H32 114.9 . . ? N4 C33 C32 123.7(2) . . ? N4 C33 C34 120.1(2) . . ? C32 C33 C34 116.2(2) . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C40 C35 C36 121.3(2) . . ? C40 C35 N3 119.2(2) . . ? C36 C35 N3 119.5(2) . . ? C37 C36 C35 117.6(2) . . ? C37 C36 C41 119.7(2) . . ? C35 C36 C41 122.7(2) . . ? C38 C37 C36 121.9(2) . . ? C38 C37 H37 119.0 . . ? C36 C37 H37 119.0 . . ? C39 C38 C37 120.0(2) . . ? C39 C38 H38 120.0 . . ? C37 C38 H38 120.0 . . ? C38 C39 C40 120.8(2) . . ? C38 C39 H39 119.6 . . ? C40 C39 H39 119.6 . . ? C35 C40 C39 118.3(2) . . ? C35 C40 C44 122.9(2) . . ? C39 C40 C44 118.8(2) . . ? C36 C41 C42 111.2(2) . . ? C36 C41 C43 112.3(2) . . ? C42 C41 C43 110.1(2) . . ? C36 C41 H41 107.7 . . ? C42 C41 H41 107.7 . . ? C43 C41 H41 107.7 . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C41 C43 H43A 109.5 . . ? C41 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C41 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C40 C44 C45 110.4(2) . . ? C40 C44 C46 112.0(2) . . ? C45 C44 C46 110.7(2) . . ? C40 C44 H44 107.9 . . ? C45 C44 H44 107.9 . . ? C46 C44 H44 107.9 . . ? C44 C45 H45A 109.5 . . ? C44 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C44 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C44 C46 H46A 109.5 . . ? C44 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C44 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C48 C47 C52 122.2(2) . . ? C48 C47 N4 118.5(2) . . ? C52 C47 N4 119.2(2) . . ? C49 C48 C47 117.7(3) . . ? C49 C48 C53 119.8(3) . . ? C47 C48 C53 122.4(2) . . ? C50 C49 C48 121.0(3) . . ? C50 C49 H49 119.5 . . ? C48 C49 H49 119.5 . . ? C49 C50 C51 120.8(3) . . ? C49 C50 H50 119.6 . . ? C51 C50 H50 119.6 . . ? C50 C51 C52 121.1(3) . . ? C50 C51 H51 119.4 . . ? C52 C51 H51 119.4 . . ? C51 C52 C47 117.1(3) . . ? C51 C52 C56 121.7(2) . . ? C47 C52 C56 121.3(2) . . ? C48 C53 C54 111.7(3) . . ? C48 C53 C55 111.3(3) . . ? C54 C53 C55 110.1(3) . . ? C48 C53 H53 107.9 . . ? C54 C53 H53 107.9 . . ? C55 C53 H53 107.9 . . ? C53 C54 H54A 109.5 . . ? C53 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C53 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C53 C55 H55A 109.5 . . ? C53 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? C53 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? C52 C56 C57 111.6(2) . . ? C52 C56 C58 113.4(3) . . ? C57 C56 C58 110.3(3) . . ? C52 C56 H56 107.1 . . ? C57 C56 H56 107.1 . . ? C58 C56 H56 107.1 . . ? C56 C57 H57A 109.5 . . ? C56 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? C56 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? C56 C58 H58A 109.5 . . ? C56 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? C56 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? O2 C59 O3 128.0(2) . . ? O2 C59 O1 116.2(2) . . ? O3 C59 O1 115.8(2) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.483 _refine_diff_density_min -0.299 _refine_diff_density_rms 0.047 _database_code_depnum_ccdc_archive 'CCDC 955168' ####################################################################### # # 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_compound1S _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C60 H82 Mg2 N4 O4' _chemical_formula_weight 971.92 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mg Mg 0.0486 0.0363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pccn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' 'x+1/2, -y, -z+1/2' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' '-x-1/2, y, z-1/2' 'x, -y-1/2, z-1/2' _cell_length_a 14.5246(9) _cell_length_b 15.6210(9) _cell_length_c 25.9215(14) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5881.3(6) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.098 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2104 _exptl_absorpt_coefficient_mu 0.087 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.974 _exptl_absorpt_correction_T_max 0.991 _exptl_absorpt_process_details 'SCALE3 ABSPACK' _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Gemini Ultra' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 35432 _diffrn_reflns_av_R_equivalents 0.0513 _diffrn_reflns_av_sigmaI/netI 0.0347 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 2.07 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5177 _reflns_number_gt 3987 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0424P)^2^+3.1446P] 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 5177 _refine_ls_number_parameters 326 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0647 _refine_ls_R_factor_gt 0.0466 _refine_ls_wR_factor_ref 0.1159 _refine_ls_wR_factor_gt 0.1053 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.032 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mg1 Mg 0.36005(4) 0.11933(4) 0.30770(2) 0.02664(17) Uani 1 1 d . . . O1 O 0.37008(8) 0.24605(8) 0.30569(5) 0.0313(3) Uani 1 1 d . . . O2 O 0.27446(9) 0.35911(8) 0.30336(5) 0.0315(3) Uani 1 1 d . . . C30 C 0.29186(12) 0.28061(12) 0.30447(6) 0.0251(4) Uani 1 1 d . . . N1 N 0.39588(11) 0.05033(10) 0.36966(5) 0.0322(4) Uani 1 1 d . . . N2 N 0.43196(10) 0.05225(9) 0.25615(5) 0.0253(3) Uani 1 1 d . . . C19 C 0.53899(13) 0.12595(12) 0.19757(7) 0.0313(4) Uani 1 1 d . . . C4 C 0.46233(12) -0.02656(11) 0.26732(7) 0.0267(4) Uani 1 1 d . . . C3 C 0.45824(12) -0.06279(12) 0.31664(7) 0.0297(4) Uani 1 1 d . . . H3 H 0.4744 -0.1217 0.3181 0.036 Uiso 1 1 calc R . . C23 C 0.38108(14) 0.09642(13) 0.16961(7) 0.0329(5) Uani 1 1 d . . . C18 C 0.45165(13) 0.08967(11) 0.20651(7) 0.0271(4) Uani 1 1 d . . . C24 C 0.61516(13) 0.12270(13) 0.23784(7) 0.0343(5) Uani 1 1 d . . . H24 H 0.5993 0.0765 0.2630 0.041 Uiso 1 1 calc R . . C6 C 0.37903(15) 0.08715(14) 0.41968(7) 0.0381(5) Uani 1 1 d . . . C2 C 0.43408(14) -0.02643(13) 0.36452(7) 0.0342(5) Uani 1 1 d . . . C22 C 0.40045(15) 0.13870(14) 0.12361(7) 0.0407(5) Uani 1 1 d . . . H22 H 0.3539 0.1430 0.0980 0.049 Uiso 1 1 calc R . . C27 C 0.28634(15) 0.05846(16) 0.17812(8) 0.0464(6) Uani 1 1 d . . . H27 H 0.2823 0.0413 0.2152 0.056 Uiso 1 1 calc R . . C20 C 0.55339(15) 0.16810(14) 0.15093(8) 0.0431(5) Uani 1 1 d . . . H20 H 0.6118 0.1931 0.1442 0.052 Uiso 1 1 calc R . . C5 C 0.50661(15) -0.07945(13) 0.22553(8) 0.0387(5) Uani 1 1 d . . . H5A H 0.4686 -0.0772 0.1943 0.058 Uiso 1 1 calc R . . H5B H 0.5121 -0.1389 0.2372 0.058 Uiso 1 1 calc R . . H5C H 0.5679 -0.0566 0.2179 0.058 Uiso 1 1 calc R . . C25 C 0.61872(15) 0.20730(14) 0.26745(8) 0.0422(5) Uani 1 1 d . . . H25A H 0.6336 0.2539 0.2436 0.063 Uiso 1 1 calc R . . H25B H 0.6661 0.2039 0.2943 0.063 Uiso 1 1 calc R . . H25C H 0.5587 0.2183 0.2834 0.063 Uiso 1 1 calc R . . C7 C 0.44344(16) 0.14630(15) 0.43937(7) 0.0422(5) Uani 1 1 d . . . C11 C 0.29602(15) 0.07014(16) 0.44587(7) 0.0449(6) Uani 1 1 d . . . C21 C 0.48510(16) 0.17437(15) 0.11434(8) 0.0468(6) Uani 1 1 d . . . H21 H 0.4966 0.2033 0.0828 0.056 Uiso 1 1 calc R . . C12 C 0.53386(16) 0.16620(15) 0.41282(8) 0.0457(6) Uani 1 1 d . . . H12 H 0.5342 0.1355 0.3790 0.055 Uiso 1 1 calc R . . C26 C 0.70952(14) 0.10159(14) 0.21498(8) 0.0419(5) Uani 1 1 d . . . H26A H 0.7066 0.0463 0.1971 0.063 Uiso 1 1 calc R . . H26B H 0.7552 0.0986 0.2427 0.063 Uiso 1 1 calc R . . H26C H 0.7272 0.1463 0.1904 0.063 Uiso 1 1 calc R . . C1 C 0.45594(18) -0.07906(16) 0.41175(8) 0.0545(7) Uani 1 1 d . . . H1A H 0.4922 -0.0446 0.4359 0.082 Uiso 1 1 calc R . . H1B H 0.4913 -0.1298 0.4016 0.082 Uiso 1 1 calc R . . H1C H 0.3985 -0.0970 0.4284 0.082 Uiso 1 1 calc R . . C10 C 0.28071(18) 0.11271(18) 0.49267(8) 0.0558(7) Uani 1 1 d . . . H10 H 0.2256 0.1017 0.5113 0.067 Uiso 1 1 calc R . . C8 C 0.42314(18) 0.18651(16) 0.48593(8) 0.0513(6) Uani 1 1 d . . . H8 H 0.4658 0.2265 0.4998 0.062 Uiso 1 1 calc R . . C9 C 0.34328(19) 0.17005(18) 0.51243(8) 0.0593(7) Uani 1 1 d . . . H9 H 0.3313 0.1981 0.5442 0.071 Uiso 1 1 calc R . . C13 C 0.54602(18) 0.26179(16) 0.40194(9) 0.0568(6) Uani 1 1 d . . . H13A H 0.4951 0.2820 0.3803 0.085 Uiso 1 1 calc R . . H13B H 0.6045 0.2711 0.3839 0.085 Uiso 1 1 calc R . . H13C H 0.5462 0.2934 0.4346 0.085 Uiso 1 1 calc R . . C15 C 0.22302(15) 0.00954(17) 0.42558(8) 0.0503(6) Uani 1 1 d . . . H15 H 0.2461 -0.0146 0.3923 0.060 Uiso 1 1 calc R . . C16 C 0.13233(17) 0.0557(2) 0.41431(10) 0.0643(8) Uani 1 1 d . . . H16A H 0.1063 0.0776 0.4466 0.096 Uiso 1 1 calc R . . H16B H 0.0889 0.0156 0.3984 0.096 Uiso 1 1 calc R . . H16C H 0.1437 0.1035 0.3907 0.096 Uiso 1 1 calc R . . C17 C 0.2043(2) -0.06593(19) 0.46212(10) 0.0715(8) Uani 1 1 d . . . H17A H 0.2613 -0.0983 0.4674 0.107 Uiso 1 1 calc R . . H17B H 0.1575 -0.1034 0.4469 0.107 Uiso 1 1 calc R . . H17C H 0.1821 -0.0442 0.4953 0.107 Uiso 1 1 calc R . . C14 C 0.61543(18) 0.13357(19) 0.44429(9) 0.0636(7) Uani 1 1 d . . . H14A H 0.6168 0.1627 0.4778 0.095 Uiso 1 1 calc R . . H14B H 0.6727 0.1453 0.4256 0.095 Uiso 1 1 calc R . . H14C H 0.6092 0.0718 0.4497 0.095 Uiso 1 1 calc R . . C29 C 0.2734(2) -0.0223(2) 0.14594(11) 0.1000(13) Uani 1 1 d . . . H29A H 0.2816 -0.0085 0.1093 0.150 Uiso 1 1 calc R . . H29B H 0.2113 -0.0450 0.1515 0.150 Uiso 1 1 calc R . . H29C H 0.3190 -0.0652 0.1563 0.150 Uiso 1 1 calc R . . C28 C 0.21002(17) 0.1232(3) 0.16820(12) 0.0946(13) Uani 1 1 d . . . H28A H 0.2208 0.1745 0.1891 0.142 Uiso 1 1 calc R . . H28B H 0.1505 0.0979 0.1776 0.142 Uiso 1 1 calc R . . H28C H 0.2096 0.1387 0.1316 0.142 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 Mg1 0.0282(4) 0.0262(3) 0.0255(3) 0.0010(2) -0.0015(2) 0.0064(3) O1 0.0228(7) 0.0291(7) 0.0422(7) 0.0011(6) 0.0005(6) 0.0037(6) O2 0.0288(7) 0.0223(7) 0.0434(8) -0.0004(5) 0.0038(6) 0.0037(6) C30 0.0263(10) 0.0278(11) 0.0213(9) 0.0006(7) 0.0014(7) 0.0018(8) N1 0.0360(9) 0.0353(10) 0.0252(8) 0.0015(7) -0.0013(7) 0.0107(8) N2 0.0256(8) 0.0247(8) 0.0256(8) 0.0005(6) -0.0002(6) 0.0005(7) C19 0.0294(11) 0.0281(10) 0.0363(10) 0.0046(8) 0.0011(8) 0.0004(8) C4 0.0221(10) 0.0241(10) 0.0339(10) -0.0011(8) 0.0018(8) -0.0022(8) C3 0.0265(10) 0.0234(10) 0.0391(11) 0.0034(8) 0.0016(8) 0.0045(8) C23 0.0333(11) 0.0353(11) 0.0300(10) -0.0001(8) -0.0014(8) -0.0025(9) C18 0.0294(11) 0.0245(10) 0.0273(9) -0.0013(7) 0.0030(8) 0.0007(8) C24 0.0300(11) 0.0315(11) 0.0414(11) 0.0071(8) -0.0013(9) -0.0031(9) C6 0.0427(12) 0.0477(13) 0.0238(10) 0.0053(9) -0.0034(9) 0.0175(10) C2 0.0318(11) 0.0353(12) 0.0357(11) 0.0079(8) -0.0008(8) 0.0084(9) C22 0.0399(13) 0.0490(14) 0.0332(11) 0.0078(9) -0.0069(9) -0.0009(11) C27 0.0370(12) 0.0720(17) 0.0304(11) 0.0055(10) -0.0065(9) -0.0164(11) C20 0.0338(12) 0.0445(13) 0.0509(13) 0.0190(10) 0.0003(10) -0.0072(10) C5 0.0437(13) 0.0265(11) 0.0460(12) -0.0010(9) 0.0154(10) 0.0013(9) C25 0.0350(12) 0.0442(13) 0.0473(12) -0.0006(10) -0.0027(10) 0.0017(10) C7 0.0505(14) 0.0502(14) 0.0259(10) 0.0013(9) -0.0059(9) 0.0141(11) C11 0.0431(13) 0.0635(16) 0.0281(11) 0.0043(10) -0.0015(9) 0.0196(12) C21 0.0471(14) 0.0514(14) 0.0417(12) 0.0212(10) 0.0014(10) -0.0043(11) C12 0.0538(14) 0.0540(14) 0.0293(11) -0.0066(10) -0.0072(10) 0.0049(11) C26 0.0315(12) 0.0423(13) 0.0520(13) 0.0028(10) 0.0008(10) 0.0017(10) C1 0.0690(17) 0.0547(15) 0.0397(12) 0.0128(11) 0.0009(11) 0.0270(13) C10 0.0544(16) 0.0812(19) 0.0319(12) 0.0010(12) 0.0060(10) 0.0212(14) C8 0.0632(16) 0.0617(16) 0.0288(11) -0.0070(10) -0.0054(11) 0.0122(13) C9 0.0748(19) 0.0762(19) 0.0270(11) -0.0079(11) 0.0008(12) 0.0242(15) C13 0.0559(16) 0.0591(16) 0.0556(14) -0.0048(12) -0.0087(12) -0.0013(13) C15 0.0378(13) 0.0784(18) 0.0348(11) 0.0022(11) 0.0023(9) 0.0125(12) C16 0.0437(15) 0.095(2) 0.0542(15) 0.0229(14) 0.0041(11) 0.0155(14) C17 0.0689(19) 0.080(2) 0.0661(17) 0.0159(15) -0.0155(14) 0.0056(16) C14 0.0598(17) 0.081(2) 0.0502(14) -0.0026(13) -0.0019(12) 0.0240(15) C29 0.109(3) 0.129(3) 0.0627(18) -0.0296(18) 0.0121(17) -0.083(2) C28 0.0290(14) 0.175(4) 0.080(2) 0.061(2) -0.0029(13) 0.0059(18) _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 Mg1 O1 1.9855(15) . ? Mg1 O2 1.9858(14) 2 ? Mg1 N2 1.9936(15) . ? Mg1 N1 2.0029(16) . ? Mg1 C30 2.7052(19) 2 ? Mg1 C30 2.7084(19) . ? O1 C30 1.258(2) . ? O2 C30 1.252(2) . ? O2 Mg1 1.9858(14) 2 ? C30 C30 1.547(4) 2 ? C30 Mg1 2.7052(19) 2 ? N1 C2 1.328(3) . ? N1 C6 1.439(2) . ? N2 C4 1.339(2) . ? N2 C18 1.442(2) . ? C19 C20 1.392(3) . ? C19 C18 1.409(3) . ? C19 C24 1.522(3) . ? C4 C3 1.399(3) . ? C4 C5 1.507(3) . ? C3 C2 1.409(3) . ? C3 H3 0.9500 . ? C23 C22 1.392(3) . ? C23 C18 1.406(3) . ? C23 C27 1.515(3) . ? C24 C25 1.529(3) . ? C24 C26 1.529(3) . ? C24 H24 1.0000 . ? C6 C11 1.409(3) . ? C6 C7 1.411(3) . ? C2 C1 1.509(3) . ? C22 C21 1.371(3) . ? C22 H22 0.9500 . ? C27 C28 1.522(4) . ? C27 C29 1.523(4) . ? C27 H27 1.0000 . ? C20 C21 1.376(3) . ? C20 H20 0.9500 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C7 C8 1.392(3) . ? C7 C12 1.515(3) . ? C11 C10 1.401(3) . ? C11 C15 1.516(3) . ? C21 H21 0.9500 . ? C12 C14 1.526(3) . ? C12 C13 1.530(3) . ? C12 H12 1.0000 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C10 C9 1.375(4) . ? C10 H10 0.9500 . ? C8 C9 1.372(3) . ? C8 H8 0.9500 . ? C9 H9 0.9500 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C15 C16 1.530(3) . ? C15 C17 1.536(4) . ? C15 H15 1.0000 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Mg1 O2 84.35(5) . 2 ? O1 Mg1 N2 117.90(6) . . ? O2 Mg1 N2 124.52(6) 2 . ? O1 Mg1 N1 122.58(7) . . ? O2 Mg1 N1 113.10(7) 2 . ? N2 Mg1 N1 96.80(7) . . ? O1 Mg1 C30 58.87(5) . 2 ? O2 Mg1 C30 25.55(5) 2 2 ? N2 Mg1 C30 135.26(6) . 2 ? N1 Mg1 C30 123.21(6) . 2 ? O1 Mg1 C30 25.66(5) . . ? O2 Mg1 C30 58.71(5) 2 . ? N2 Mg1 C30 131.29(6) . . ? N1 Mg1 C30 128.34(6) . . ? C30 Mg1 C30 33.21(7) 2 . ? C30 O1 Mg1 111.24(11) . . ? C30 O2 Mg1 111.30(12) . 2 ? O2 C30 O1 127.08(17) . . ? O2 C30 C30 116.54(19) . 2 ? O1 C30 C30 116.38(19) . 2 ? O2 C30 Mg1 43.15(8) . 2 ? O1 C30 Mg1 169.60(13) . 2 ? C30 C30 Mg1 73.51(13) 2 2 ? O2 C30 Mg1 170.17(13) . . ? O1 C30 Mg1 43.10(9) . . ? C30 C30 Mg1 73.28(13) 2 . ? Mg1 C30 Mg1 146.59(7) 2 . ? C2 N1 C6 121.49(15) . . ? C2 N1 Mg1 120.93(12) . . ? C6 N1 Mg1 117.58(12) . . ? C4 N2 C18 120.01(15) . . ? C4 N2 Mg1 120.72(12) . . ? C18 N2 Mg1 119.27(11) . . ? C20 C19 C18 117.93(18) . . ? C20 C19 C24 120.13(17) . . ? C18 C19 C24 121.91(16) . . ? N2 C4 C3 123.72(16) . . ? N2 C4 C5 119.28(16) . . ? C3 C4 C5 116.96(17) . . ? C4 C3 C2 130.71(18) . . ? C4 C3 H3 114.6 . . ? C2 C3 H3 114.6 . . ? C22 C23 C18 118.11(18) . . ? C22 C23 C27 119.62(18) . . ? C18 C23 C27 122.27(17) . . ? C23 C18 C19 120.97(16) . . ? C23 C18 N2 119.54(16) . . ? C19 C18 N2 119.23(16) . . ? C19 C24 C25 109.87(16) . . ? C19 C24 C26 113.13(16) . . ? C25 C24 C26 110.52(17) . . ? C19 C24 H24 107.7 . . ? C25 C24 H24 107.7 . . ? C26 C24 H24 107.7 . . ? C11 C6 C7 121.11(19) . . ? C11 C6 N1 120.3(2) . . ? C7 C6 N1 118.36(18) . . ? N1 C2 C3 123.80(17) . . ? N1 C2 C1 119.91(17) . . ? C3 C2 C1 116.27(18) . . ? C21 C22 C23 121.61(19) . . ? C21 C22 H22 119.2 . . ? C23 C22 H22 119.2 . . ? C23 C27 C28 112.2(2) . . ? C23 C27 C29 110.9(2) . . ? C28 C27 C29 111.5(3) . . ? C23 C27 H27 107.3 . . ? C28 C27 H27 107.3 . . ? C29 C27 H27 107.3 . . ? C21 C20 C19 121.6(2) . . ? C21 C20 H20 119.2 . . ? C19 C20 H20 119.2 . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C8 C7 C6 118.0(2) . . ? C8 C7 C12 119.0(2) . . ? C6 C7 C12 123.02(18) . . ? C10 C11 C6 117.6(2) . . ? C10 C11 C15 119.1(2) . . ? C6 C11 C15 123.31(19) . . ? C22 C21 C20 119.78(19) . . ? C22 C21 H21 120.1 . . ? C20 C21 H21 120.1 . . ? C7 C12 C14 111.20(19) . . ? C7 C12 C13 112.59(19) . . ? C14 C12 C13 109.6(2) . . ? C7 C12 H12 107.8 . . ? C14 C12 H12 107.8 . . ? C13 C12 H12 107.8 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C9 C10 C11 121.8(2) . . ? C9 C10 H10 119.1 . . ? C11 C10 H10 119.1 . . ? C9 C8 C7 121.9(2) . . ? C9 C8 H8 119.0 . . ? C7 C8 H8 119.0 . . ? C8 C9 C10 119.6(2) . . ? C8 C9 H9 120.2 . . ? C10 C9 H9 120.2 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C11 C15 C16 112.0(2) . . ? C11 C15 C17 112.90(19) . . ? C16 C15 C17 109.1(2) . . ? C11 C15 H15 107.5 . . ? C16 C15 H15 107.5 . . ? C17 C15 H15 107.5 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.317 _refine_diff_density_min -0.233 _refine_diff_density_rms 0.039 _database_code_depnum_ccdc_archive 'CCDC 955169' ####################################################################### # # 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_compound2S _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C58 H84 Mg2 N4 O2' _chemical_formula_weight 917.91 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mg Mg 0.0486 0.0363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 22.886(5) _cell_length_b 14.823(3) _cell_length_c 16.196(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.65(3) _cell_angle_gamma 90.00 _cell_volume 5493.9(19) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.110 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2000 _exptl_absorpt_coefficient_mu 0.087 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.990 _exptl_absorpt_correction_T_max 0.993 _exptl_absorpt_process_details 'Sortav (Blessing, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(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 'Bruker Apex' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8993 _diffrn_reflns_av_R_equivalents 0.1005 _diffrn_reflns_av_sigmaI/netI 0.1360 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.99 _diffrn_reflns_theta_max 24.96 _reflns_number_total 4748 _reflns_number_gt 2295 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1227P)^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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4748 _refine_ls_number_parameters 312 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1761 _refine_ls_R_factor_gt 0.0775 _refine_ls_wR_factor_ref 0.2258 _refine_ls_wR_factor_gt 0.1822 _refine_ls_goodness_of_fit_ref 0.957 _refine_ls_restrained_S_all 0.957 _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 Mg1 Mg 0.20159(4) 0.68222(6) 0.00130(7) 0.0348(3) Uani 1 1 d . . . N1 N 0.11577(10) 0.67914(16) -0.04353(15) 0.0345(7) Uani 1 1 d . . . O1 O 0.23422(9) 0.77907(14) 0.06976(14) 0.0444(6) Uani 1 1 d . . . C6 C 0.08273(12) 0.76060(19) -0.0621(2) 0.0358(8) Uani 1 1 d . . . N2 N 0.19516(10) 0.55130(16) 0.04778(16) 0.0367(7) Uani 1 1 d . . . C18 C 0.23157(14) 0.5172(2) 0.1139(2) 0.0401(9) Uani 1 1 d . . . C2 C 0.08842(13) 0.6014(2) -0.0595(2) 0.0385(9) Uani 1 1 d . . . C11 C 0.08575(13) 0.7985(2) -0.1416(2) 0.0396(9) Uani 1 1 d . . . C7 C 0.04700(13) 0.7981(2) -0.0014(2) 0.0439(9) Uani 1 1 d . . . C3 C 0.11061(13) 0.5166(2) -0.0364(2) 0.0406(9) Uani 1 1 d . . . H3 H 0.0910 0.4669 -0.0612 0.049 Uiso 1 1 calc R . . C23 C 0.28180(14) 0.4667(2) 0.0980(2) 0.0438(9) Uani 1 1 d . . . C5 C 0.15887(15) 0.3936(2) 0.0391(2) 0.0514(10) Uani 1 1 d . . . H5A H 0.1912 0.3648 0.0100 0.077 Uiso 1 1 calc R . . H5B H 0.1220 0.3646 0.0231 0.077 Uiso 1 1 calc R . . H5C H 0.1650 0.3874 0.0988 0.077 Uiso 1 1 calc R . . C12 C 0.04451(15) 0.7571(2) 0.0853(2) 0.0564(11) Uani 1 1 d . . . H12 H 0.0710 0.7035 0.0860 0.068 Uiso 1 1 calc R . . C1 C 0.02857(14) 0.6003(2) -0.0998(2) 0.0521(10) Uani 1 1 d . . . H1A H 0.0013 0.6353 -0.0664 0.078 Uiso 1 1 calc R . . H1B H 0.0147 0.5379 -0.1042 0.078 Uiso 1 1 calc R . . H1C H 0.0308 0.6268 -0.1551 0.078 Uiso 1 1 calc R . . C15 C 0.12097(14) 0.7565(2) -0.2096(2) 0.0475(10) Uani 1 1 d . . . H15 H 0.1358 0.6971 -0.1890 0.057 Uiso 1 1 calc R . . C19 C 0.21355(14) 0.5342(2) 0.1956(2) 0.0458(10) Uani 1 1 d . . . C4 C 0.15643(13) 0.4930(2) 0.0165(2) 0.0384(9) Uani 1 1 d . . . C8 C 0.01385(15) 0.8731(2) -0.0212(2) 0.0527(10) Uani 1 1 d . . . H8 H -0.0111 0.8983 0.0192 0.063 Uiso 1 1 calc R . . C22 C 0.31289(16) 0.4315(2) 0.1645(2) 0.0582(11) Uani 1 1 d . . . H22 H 0.3475 0.3979 0.1547 0.070 Uiso 1 1 calc R . . C10 C 0.05245(15) 0.8757(2) -0.1571(2) 0.0537(10) Uani 1 1 d . . . H10 H 0.0548 0.9040 -0.2096 0.064 Uiso 1 1 calc R . . C24 C 0.15966(15) 0.5911(2) 0.2129(2) 0.0528(10) Uani 1 1 d . . . H24 H 0.1534 0.6320 0.1645 0.063 Uiso 1 1 calc R . . C20 C 0.24539(17) 0.4944(2) 0.2600(3) 0.0610(12) Uani 1 1 d . . . H20 H 0.2329 0.5020 0.3153 0.073 Uiso 1 1 calc R . . C27 C 0.30199(14) 0.4491(2) 0.0105(2) 0.0496(10) Uani 1 1 d . . . H27 H 0.2681 0.4615 -0.0274 0.060 Uiso 1 1 calc R . . C28 C 0.35080(17) 0.5120(3) -0.0135(3) 0.0707(13) Uani 1 1 d . . . H28A H 0.3368 0.5744 -0.0118 0.106 Uiso 1 1 calc R . . H28B H 0.3636 0.4975 -0.0695 0.106 Uiso 1 1 calc R . . H28C H 0.3837 0.5047 0.0252 0.106 Uiso 1 1 calc R . . C9 C 0.01606(16) 0.9121(2) -0.0981(3) 0.0582(11) Uani 1 1 d . . . H9 H -0.0072 0.9635 -0.1106 0.070 Uiso 1 1 calc R . . C21 C 0.29466(17) 0.4441(3) 0.2444(3) 0.0663(12) Uani 1 1 d . . . H21 H 0.3161 0.4181 0.2890 0.080 Uiso 1 1 calc R . . C26 C 0.16616(17) 0.6506(3) 0.2897(3) 0.0727(13) Uani 1 1 d . . . H26A H 0.1327 0.6917 0.2930 0.109 Uiso 1 1 calc R . . H26B H 0.2023 0.6857 0.2862 0.109 Uiso 1 1 calc R . . H26C H 0.1676 0.6124 0.3391 0.109 Uiso 1 1 calc R . . C16 C 0.08494(17) 0.7388(3) -0.2864(3) 0.0771(14) Uani 1 1 d . . . H16A H 0.0515 0.7005 -0.2725 0.116 Uiso 1 1 calc R . . H16B H 0.1090 0.7081 -0.3274 0.116 Uiso 1 1 calc R . . H16C H 0.0708 0.7962 -0.3091 0.116 Uiso 1 1 calc R . . C29 C 0.3211(2) 0.3514(3) -0.0040(3) 0.0801(14) Uani 1 1 d . . . H29A H 0.3585 0.3405 0.0245 0.120 Uiso 1 1 calc R . . H29B H 0.3257 0.3410 -0.0633 0.120 Uiso 1 1 calc R . . H29C H 0.2914 0.3103 0.0176 0.120 Uiso 1 1 calc R . . C17 C 0.17334(17) 0.8132(3) -0.2312(3) 0.0845(15) Uani 1 1 d . . . H17A H 0.1602 0.8722 -0.2516 0.127 Uiso 1 1 calc R . . H17B H 0.1959 0.7827 -0.2741 0.127 Uiso 1 1 calc R . . H17C H 0.1980 0.8216 -0.1819 0.127 Uiso 1 1 calc R . . C13 C 0.0658(2) 0.8202(4) 0.1505(3) 0.1081(19) Uani 1 1 d . . . H13A H 0.0382 0.8704 0.1557 0.162 Uiso 1 1 calc R . . H13B H 0.1042 0.8437 0.1354 0.162 Uiso 1 1 calc R . . H13C H 0.0689 0.7881 0.2033 0.162 Uiso 1 1 calc R . . C14 C -0.0160(2) 0.7240(4) 0.1058(3) 0.131(2) Uani 1 1 d . . . H14A H -0.0153 0.6957 0.1605 0.196 Uiso 1 1 calc R . . H14B H -0.0287 0.6797 0.0644 0.196 Uiso 1 1 calc R . . H14C H -0.0432 0.7750 0.1059 0.196 Uiso 1 1 calc R . . C25 C 0.10558(17) 0.5324(3) 0.2206(3) 0.0778(14) Uani 1 1 d . . . H25A H 0.1000 0.4975 0.1697 0.117 Uiso 1 1 calc R . . H25B H 0.0713 0.5707 0.2295 0.117 Uiso 1 1 calc R . . H25C H 0.1106 0.4911 0.2674 0.117 Uiso 1 1 calc R . . H1 H 0.2222(9) 0.8017(14) 0.1180(13) 0.000(6) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mg1 0.0311(5) 0.0312(5) 0.0421(7) 0.0011(5) 0.0001(5) -0.0014(4) N1 0.0320(13) 0.0310(13) 0.0403(16) 0.0002(12) -0.0046(12) -0.0026(11) O1 0.0430(12) 0.0442(13) 0.0462(15) -0.0080(11) 0.0083(11) -0.0080(10) C6 0.0272(16) 0.0325(17) 0.048(2) -0.0010(16) -0.0053(15) -0.0051(14) N2 0.0327(13) 0.0356(14) 0.0418(16) 0.0025(13) -0.0005(12) -0.0039(12) C18 0.0428(18) 0.0318(16) 0.046(2) 0.0080(16) -0.0065(17) -0.0043(15) C2 0.0341(17) 0.0431(19) 0.038(2) -0.0013(16) -0.0028(15) -0.0034(15) C11 0.0364(17) 0.0343(17) 0.048(2) -0.0025(17) -0.0106(16) -0.0021(14) C7 0.0341(18) 0.0407(19) 0.057(2) -0.0076(18) -0.0033(17) 0.0004(15) C3 0.0433(19) 0.0296(16) 0.049(2) -0.0069(16) 0.0009(17) -0.0061(15) C23 0.0386(18) 0.0362(18) 0.057(2) -0.0024(17) -0.0016(17) 0.0002(15) C5 0.056(2) 0.0328(18) 0.066(3) 0.0058(18) -0.010(2) -0.0086(16) C12 0.051(2) 0.059(2) 0.059(3) -0.004(2) 0.0141(19) 0.0108(18) C1 0.0420(19) 0.044(2) 0.069(3) -0.0038(19) -0.0097(19) -0.0059(16) C15 0.051(2) 0.047(2) 0.044(2) 0.0066(17) -0.0047(18) 0.0029(17) C19 0.046(2) 0.0424(19) 0.049(2) 0.0074(17) 0.0003(18) -0.0058(16) C4 0.0354(18) 0.0338(17) 0.046(2) 0.0006(16) 0.0008(16) -0.0020(14) C8 0.043(2) 0.053(2) 0.062(3) -0.012(2) -0.0080(18) 0.0098(17) C22 0.059(2) 0.047(2) 0.068(3) -0.001(2) -0.016(2) 0.0086(18) C10 0.062(2) 0.0389(19) 0.060(3) -0.0009(18) -0.017(2) 0.0057(17) C24 0.055(2) 0.056(2) 0.048(2) 0.0038(19) 0.0038(19) 0.0006(18) C20 0.071(3) 0.064(2) 0.048(2) 0.015(2) -0.007(2) -0.008(2) C27 0.0435(19) 0.0395(18) 0.066(3) -0.0018(19) -0.0045(18) 0.0056(16) C28 0.069(3) 0.065(3) 0.078(3) -0.003(2) 0.009(2) -0.010(2) C9 0.066(2) 0.0386(19) 0.069(3) -0.012(2) -0.026(2) 0.0109(18) C21 0.070(3) 0.061(2) 0.067(3) 0.012(2) -0.028(2) 0.005(2) C26 0.066(3) 0.070(3) 0.082(3) -0.019(2) 0.013(2) -0.004(2) C16 0.057(2) 0.111(3) 0.063(3) -0.036(3) -0.009(2) 0.004(2) C29 0.087(3) 0.053(2) 0.100(4) -0.011(2) 0.010(3) 0.012(2) C17 0.061(3) 0.104(3) 0.088(3) -0.018(3) 0.001(2) -0.021(2) C13 0.143(4) 0.125(4) 0.056(3) 0.020(3) -0.032(3) -0.064(3) C14 0.121(4) 0.182(5) 0.089(4) 0.003(4) 0.010(3) -0.095(4) C25 0.054(2) 0.093(3) 0.087(3) -0.021(3) 0.008(2) -0.010(2) _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 Mg1 O1 1.957(2) . ? Mg1 O1 1.962(2) 7_565 ? Mg1 N1 2.087(3) . ? Mg1 N2 2.087(3) . ? N1 C2 1.335(4) . ? N1 C6 1.454(4) . ? O1 Mg1 1.962(2) 7_565 ? C6 C7 1.400(4) . ? C6 C11 1.408(4) . ? N2 C4 1.334(4) . ? N2 C18 1.441(4) . ? C18 C23 1.398(4) . ? C18 C19 1.412(5) . ? C2 C3 1.405(4) . ? C2 C1 1.511(4) . ? C11 C10 1.395(4) . ? C11 C15 1.507(5) . ? C7 C8 1.381(5) . ? C7 C12 1.532(5) . ? C3 C4 1.391(4) . ? C23 C22 1.386(5) . ? C23 C27 1.519(5) . ? C5 C4 1.519(4) . ? C12 C13 1.488(6) . ? C12 C14 1.509(6) . ? C15 C16 1.507(5) . ? C15 C17 1.508(5) . ? C19 C20 1.397(5) . ? C19 C24 1.523(5) . ? C8 C9 1.373(5) . ? C22 C21 1.378(5) . ? C10 C9 1.385(5) . ? C24 C25 1.520(5) . ? C24 C26 1.530(5) . ? C20 C21 1.377(5) . ? C27 C28 1.509(5) . ? C27 C29 1.532(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Mg1 O1 80.47(11) . 7_565 ? O1 Mg1 N1 124.39(10) . . ? O1 Mg1 N1 120.69(11) 7_565 . ? O1 Mg1 N2 120.38(11) . . ? O1 Mg1 N2 122.66(10) 7_565 . ? N1 Mg1 N2 92.02(10) . . ? C2 N1 C6 115.8(2) . . ? C2 N1 Mg1 121.6(2) . . ? C6 N1 Mg1 122.60(17) . . ? Mg1 O1 Mg1 99.53(11) . 7_565 ? C7 C6 C11 121.2(3) . . ? C7 C6 N1 119.5(3) . . ? C11 C6 N1 119.3(3) . . ? C4 N2 C18 115.6(2) . . ? C4 N2 Mg1 121.0(2) . . ? C18 N2 Mg1 123.48(19) . . ? C23 C18 C19 121.2(3) . . ? C23 C18 N2 121.4(3) . . ? C19 C18 N2 117.4(3) . . ? N1 C2 C3 123.6(3) . . ? N1 C2 C1 121.0(3) . . ? C3 C2 C1 115.3(3) . . ? C10 C11 C6 117.4(3) . . ? C10 C11 C15 120.2(3) . . ? C6 C11 C15 122.4(3) . . ? C8 C7 C6 118.7(3) . . ? C8 C7 C12 120.4(3) . . ? C6 C7 C12 120.9(3) . . ? C4 C3 C2 131.0(3) . . ? C22 C23 C18 118.3(3) . . ? C22 C23 C27 120.1(3) . . ? C18 C23 C27 121.6(3) . . ? C13 C12 C14 110.0(4) . . ? C13 C12 C7 112.7(3) . . ? C14 C12 C7 112.0(3) . . ? C11 C15 C16 112.5(3) . . ? C11 C15 C17 111.9(3) . . ? C16 C15 C17 109.6(3) . . ? C20 C19 C18 117.9(3) . . ? C20 C19 C24 120.9(3) . . ? C18 C19 C24 121.2(3) . . ? N2 C4 C3 124.4(3) . . ? N2 C4 C5 120.9(3) . . ? C3 C4 C5 114.7(3) . . ? C9 C8 C7 121.6(3) . . ? C21 C22 C23 121.3(3) . . ? C9 C10 C11 121.8(4) . . ? C25 C24 C19 111.0(3) . . ? C25 C24 C26 109.6(3) . . ? C19 C24 C26 113.4(3) . . ? C21 C20 C19 120.9(4) . . ? C28 C27 C23 111.6(3) . . ? C28 C27 C29 109.3(3) . . ? C23 C27 C29 113.3(3) . . ? C8 C9 C10 119.4(3) . . ? C20 C21 C22 120.2(4) . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 24.96 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.290 _refine_diff_density_min -0.290 _refine_diff_density_rms 0.062 _database_code_depnum_ccdc_archive 'CCDC 955170' ####################################################################### # # 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_compound3 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C72 H104 Mg2 N4 O3' _chemical_formula_weight 1122.21 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mg Mg 0.0486 0.0363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.1680(13) _cell_length_b 12.6241(14) _cell_length_c 13.176(2) _cell_angle_alpha 98.046(11) _cell_angle_beta 111.433(12) _cell_angle_gamma 109.680(10) _cell_volume 1692.2(4) _cell_formula_units_Z 1 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.45 _exptl_crystal_size_min 0.35 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.101 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 612 _exptl_absorpt_coefficient_mu 0.083 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.959 _exptl_absorpt_correction_T_max 0.971 _exptl_absorpt_process_details 'SCALE3 ABSPACK' _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Enhance (Mo) X-ray Source' _diffrn_measurement_method 'Oxford Gemini Ultra' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15548 _diffrn_reflns_av_R_equivalents 0.0228 _diffrn_reflns_av_sigmaI/netI 0.0357 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.98 _diffrn_reflns_theta_max 28.00 _reflns_number_total 8169 _reflns_number_gt 6647 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. A half molecule of benzene of crystallisation, sitting on an inversion centre was located in the asymmetric unit and its carbon atoms refined anisotropically. ; _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^)+(0.0544P)^2^+0.6949P] 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 8169 _refine_ls_number_parameters 377 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0587 _refine_ls_R_factor_gt 0.0448 _refine_ls_wR_factor_ref 0.1230 _refine_ls_wR_factor_gt 0.1120 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.023 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mg1 Mg 0.43082(4) 0.46921(4) 0.34643(3) 0.01588(11) Uani 1 1 d . . . O1 O 0.5000 0.5000 0.5000 0.0277(3) Uani 1 2 d S . . N1 N 0.23939(10) 0.36276(9) 0.22060(9) 0.0169(2) Uani 1 1 d . . . C1 C 0.09621(14) 0.25017(13) 0.01599(11) 0.0263(3) Uani 1 1 d . . . H1A H 0.1087 0.1776 0.0177 0.039 Uiso 1 1 calc R . . H1B H 0.0853 0.2638 -0.0578 0.039 Uiso 1 1 calc R . . H1C H 0.0184 0.2424 0.0264 0.039 Uiso 1 1 calc R . . O2 O 0.52648(9) 0.37623(9) 0.29899(8) 0.0224(2) Uani 1 1 d . . . N2 N 0.44962(10) 0.59024(9) 0.25283(9) 0.0169(2) Uani 1 1 d . . . C2 C 0.21459(12) 0.35373(11) 0.11174(10) 0.0184(2) Uani 1 1 d . . . C3 C 0.29221(13) 0.43544(12) 0.07567(10) 0.0193(3) Uani 1 1 d . . . H3 H 0.2739 0.4104 -0.0024 0.023 Uiso 1 1 calc R . . C4 C 0.39287(12) 0.54873(11) 0.13899(10) 0.0176(2) Uani 1 1 d . . . C5 C 0.43440(15) 0.62496(13) 0.06841(11) 0.0257(3) Uani 1 1 d . . . H5A H 0.4288 0.7000 0.0891 0.039 Uiso 1 1 calc R . . H5B H 0.3769 0.5839 -0.0130 0.039 Uiso 1 1 calc R . . H5C H 0.5243 0.6402 0.0836 0.039 Uiso 1 1 calc R . . C6 C 0.13903(12) 0.28323(11) 0.24154(10) 0.0183(2) Uani 1 1 d . . . C7 C 0.13644(13) 0.17318(12) 0.25244(11) 0.0205(3) Uani 1 1 d . . . C8 C 0.03567(14) 0.09733(13) 0.26998(13) 0.0276(3) Uani 1 1 d . . . H8 H 0.0337 0.0232 0.2781 0.033 Uiso 1 1 calc R . . C9 C -0.06120(14) 0.12801(14) 0.27569(14) 0.0313(3) Uani 1 1 d . . . H9 H -0.1305 0.0745 0.2853 0.038 Uiso 1 1 calc R . . C10 C -0.05637(14) 0.23741(14) 0.26731(13) 0.0298(3) Uani 1 1 d . . . H10 H -0.1222 0.2588 0.2727 0.036 Uiso 1 1 calc R . . C11 C 0.04313(13) 0.31704(13) 0.25105(12) 0.0233(3) Uani 1 1 d . . . C12 C 0.24217(13) 0.13737(12) 0.24869(12) 0.0228(3) Uani 1 1 d . . . H12 H 0.2960 0.1957 0.2226 0.027 Uiso 1 1 calc R . . C13 C 0.33070(16) 0.14384(17) 0.36893(14) 0.0378(4) Uani 1 1 d . . . H13A H 0.3688 0.2242 0.4199 0.057 Uiso 1 1 calc R . . H13B H 0.4004 0.1227 0.3667 0.057 Uiso 1 1 calc R . . H13C H 0.2797 0.0888 0.3974 0.057 Uiso 1 1 calc R . . C14 C 0.18785(18) 0.01474(15) 0.16503(16) 0.0405(4) Uani 1 1 d . . . H14A H 0.1382 -0.0447 0.1909 0.061 Uiso 1 1 calc R . . H14B H 0.2599 -0.0018 0.1620 0.061 Uiso 1 1 calc R . . H14C H 0.1307 0.0123 0.0888 0.061 Uiso 1 1 calc R . . C15 C 0.04401(14) 0.43615(14) 0.24166(14) 0.0295(3) Uani 1 1 d . . . H15 H 0.1300 0.4859 0.2456 0.035 Uiso 1 1 calc R . . C16 C 0.02982(17) 0.50044(16) 0.34045(15) 0.0405(4) Uani 1 1 d . . . H16A H -0.0556 0.4553 0.3365 0.061 Uiso 1 1 calc R . . H16B H 0.0376 0.5790 0.3348 0.061 Uiso 1 1 calc R . . H16C H 0.0983 0.5082 0.4133 0.061 Uiso 1 1 calc R . . C17 C -0.06240(19) 0.42275(18) 0.12653(15) 0.0433(4) Uani 1 1 d . . . H17A H -0.0444 0.3925 0.0645 0.065 Uiso 1 1 calc R . . H17B H -0.0636 0.4997 0.1247 0.065 Uiso 1 1 calc R . . H17C H -0.1471 0.3675 0.1168 0.065 Uiso 1 1 calc R . . C18 C 0.53088(13) 0.71499(11) 0.30284(10) 0.0183(2) Uani 1 1 d . . . C19 C 0.66367(13) 0.76140(12) 0.32865(11) 0.0210(3) Uani 1 1 d . . . C20 C 0.73608(14) 0.88408(12) 0.37272(12) 0.0251(3) Uani 1 1 d . . . H20 H 0.8260 0.9168 0.3909 0.030 Uiso 1 1 calc R . . C21 C 0.67887(15) 0.95837(12) 0.39027(12) 0.0267(3) Uani 1 1 d . . . H21 H 0.7283 1.0414 0.4167 0.032 Uiso 1 1 calc R . . C22 C 0.54895(14) 0.91104(12) 0.36911(12) 0.0246(3) Uani 1 1 d . . . H22 H 0.5107 0.9623 0.3833 0.030 Uiso 1 1 calc R . . C23 C 0.47359(13) 0.78927(11) 0.32735(11) 0.0202(3) Uani 1 1 d . . . C24 C 0.73083(14) 0.68246(13) 0.31404(12) 0.0244(3) Uani 1 1 d . . . H24 H 0.6617 0.6020 0.2651 0.029 Uiso 1 1 calc R . . C25 C 0.80851(19) 0.67232(17) 0.43022(15) 0.0419(4) Uani 1 1 d . . . H25A H 0.8767 0.7503 0.4803 0.063 Uiso 1 1 calc R . . H25B H 0.8485 0.6185 0.4202 0.063 Uiso 1 1 calc R . . H25C H 0.7502 0.6416 0.4647 0.063 Uiso 1 1 calc R . . C26 C 0.81821(18) 0.72440(16) 0.25509(16) 0.0392(4) Uani 1 1 d . . . H26A H 0.7686 0.7367 0.1838 0.059 Uiso 1 1 calc R . . H26B H 0.8487 0.6646 0.2380 0.059 Uiso 1 1 calc R . . H26C H 0.8932 0.7987 0.3058 0.059 Uiso 1 1 calc R . . C27 C 0.33328(14) 0.73754(12) 0.31061(11) 0.0228(3) Uani 1 1 d . . . H27 H 0.3159 0.6598 0.3263 0.027 Uiso 1 1 calc R . . C28 C 0.30880(15) 0.81341(13) 0.39421(13) 0.0295(3) Uani 1 1 d . . . H28A H 0.3748 0.8323 0.4724 0.044 Uiso 1 1 calc R . . H28B H 0.2222 0.7698 0.3886 0.044 Uiso 1 1 calc R . . H28C H 0.3137 0.8866 0.3750 0.044 Uiso 1 1 calc R . . C29 C 0.23474(15) 0.71347(14) 0.18768(13) 0.0312(3) Uani 1 1 d . . . H29A H 0.2536 0.7868 0.1668 0.047 Uiso 1 1 calc R . . H29B H 0.1466 0.6834 0.1821 0.047 Uiso 1 1 calc R . . H29C H 0.2411 0.6548 0.1356 0.047 Uiso 1 1 calc R . . C30 C 0.51658(14) 0.32716(14) 0.18768(12) 0.0268(3) Uani 1 1 d . . . H30A H 0.5210 0.3859 0.1451 0.032 Uiso 1 1 calc R . . H30B H 0.4334 0.2564 0.1420 0.032 Uiso 1 1 calc R . . C31 C 0.63030(17) 0.29527(17) 0.21132(15) 0.0367(4) Uani 1 1 d . . . H31A H 0.7085 0.3627 0.2211 0.044 Uiso 1 1 calc R . . H31B H 0.6094 0.2269 0.1493 0.044 Uiso 1 1 calc R . . C32 C 0.6496(2) 0.26454(18) 0.32284(15) 0.0414(4) Uani 1 1 d . . . H32A H 0.5870 0.1834 0.3085 0.050 Uiso 1 1 calc R . . H32B H 0.7393 0.2722 0.3651 0.050 Uiso 1 1 calc R . . C33 C 0.62412(15) 0.35522(14) 0.38722(13) 0.0290(3) Uani 1 1 d . . . H33A H 0.5910 0.3247 0.4404 0.035 Uiso 1 1 calc R . . H33B H 0.7046 0.4288 0.4314 0.035 Uiso 1 1 calc R . . C34 C 0.62417(17) 1.01550(17) 0.01683(15) 0.0396(4) Uani 1 1 d . . . H34 H 0.7094 1.0261 0.0281 0.048 Uiso 1 1 calc R . . C35 C 0.57384(17) 0.96736(16) 0.08699(14) 0.0376(4) Uani 1 1 d . . . H35 H 0.6245 0.9451 0.1467 0.045 Uiso 1 1 calc R . . C36 C 0.45018(18) 0.95189(16) 0.06987(14) 0.0390(4) Uani 1 1 d . . . H36 H 0.4156 0.9186 0.1178 0.047 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 Mg1 0.0159(2) 0.0170(2) 0.0156(2) 0.00564(16) 0.00730(16) 0.00717(17) O1 0.0298(8) 0.0324(8) 0.0175(6) 0.0075(6) 0.0082(6) 0.0117(6) N1 0.0148(5) 0.0186(5) 0.0166(5) 0.0059(4) 0.0064(4) 0.0067(4) C1 0.0240(7) 0.0259(7) 0.0173(6) 0.0034(5) 0.0046(5) 0.0037(6) O2 0.0223(5) 0.0285(5) 0.0207(5) 0.0075(4) 0.0093(4) 0.0158(4) N2 0.0189(5) 0.0159(5) 0.0163(5) 0.0050(4) 0.0078(4) 0.0076(4) C2 0.0180(6) 0.0194(6) 0.0160(6) 0.0041(5) 0.0049(5) 0.0089(5) C3 0.0216(6) 0.0222(6) 0.0133(5) 0.0053(5) 0.0067(5) 0.0096(5) C4 0.0193(6) 0.0196(6) 0.0173(6) 0.0075(5) 0.0093(5) 0.0101(5) C5 0.0305(7) 0.0257(7) 0.0183(6) 0.0091(5) 0.0109(6) 0.0080(6) C6 0.0140(6) 0.0202(6) 0.0153(6) 0.0044(5) 0.0039(5) 0.0043(5) C7 0.0176(6) 0.0212(6) 0.0181(6) 0.0050(5) 0.0063(5) 0.0053(5) C8 0.0241(7) 0.0250(7) 0.0305(7) 0.0118(6) 0.0116(6) 0.0059(6) C9 0.0197(7) 0.0355(8) 0.0371(8) 0.0165(7) 0.0146(6) 0.0054(6) C10 0.0187(7) 0.0385(8) 0.0347(8) 0.0140(7) 0.0132(6) 0.0121(6) C11 0.0172(6) 0.0272(7) 0.0237(6) 0.0086(5) 0.0072(5) 0.0091(6) C12 0.0231(7) 0.0196(6) 0.0272(7) 0.0087(5) 0.0127(6) 0.0085(5) C13 0.0329(9) 0.0552(11) 0.0357(9) 0.0218(8) 0.0154(7) 0.0268(8) C14 0.0430(10) 0.0268(8) 0.0499(10) 0.0028(7) 0.0230(8) 0.0135(7) C15 0.0206(7) 0.0303(8) 0.0427(9) 0.0141(7) 0.0148(6) 0.0143(6) C16 0.0333(9) 0.0375(9) 0.0418(9) 0.0031(7) 0.0078(7) 0.0179(8) C17 0.0491(11) 0.0533(11) 0.0412(9) 0.0223(8) 0.0194(8) 0.0344(9) C18 0.0236(6) 0.0172(6) 0.0144(5) 0.0068(5) 0.0088(5) 0.0078(5) C19 0.0253(7) 0.0208(6) 0.0169(6) 0.0065(5) 0.0107(5) 0.0081(5) C20 0.0256(7) 0.0219(7) 0.0240(7) 0.0065(5) 0.0122(6) 0.0047(6) C21 0.0338(8) 0.0159(6) 0.0249(7) 0.0055(5) 0.0129(6) 0.0045(6) C22 0.0326(8) 0.0192(6) 0.0232(6) 0.0069(5) 0.0121(6) 0.0122(6) C23 0.0249(7) 0.0187(6) 0.0159(6) 0.0065(5) 0.0077(5) 0.0087(5) C24 0.0224(7) 0.0238(7) 0.0251(7) 0.0046(5) 0.0111(6) 0.0081(6) C25 0.0526(11) 0.0481(10) 0.0341(9) 0.0153(8) 0.0167(8) 0.0329(9) C26 0.0400(9) 0.0445(10) 0.0454(10) 0.0145(8) 0.0301(8) 0.0191(8) C27 0.0255(7) 0.0208(6) 0.0237(6) 0.0067(5) 0.0104(5) 0.0122(6) C28 0.0328(8) 0.0274(7) 0.0324(8) 0.0068(6) 0.0173(6) 0.0149(6) C29 0.0287(8) 0.0342(8) 0.0284(7) 0.0070(6) 0.0085(6) 0.0162(7) C30 0.0264(7) 0.0330(8) 0.0257(7) 0.0067(6) 0.0148(6) 0.0148(6) C31 0.0401(9) 0.0524(10) 0.0408(9) 0.0226(8) 0.0274(8) 0.0320(8) C32 0.0573(11) 0.0588(11) 0.0469(10) 0.0319(9) 0.0364(9) 0.0473(10) C33 0.0264(7) 0.0360(8) 0.0297(7) 0.0128(6) 0.0092(6) 0.0212(7) C34 0.0319(9) 0.0497(10) 0.0352(9) 0.0101(8) 0.0153(7) 0.0154(8) C35 0.0415(9) 0.0436(10) 0.0274(8) 0.0144(7) 0.0116(7) 0.0203(8) C36 0.0444(10) 0.0429(10) 0.0325(8) 0.0160(7) 0.0222(8) 0.0139(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mg1 O1 1.8080(5) . ? Mg1 O2 2.0905(10) . ? Mg1 N2 2.0990(11) . ? Mg1 N1 2.1039(12) . ? Mg1 Mg1 3.6160(11) 2_666 ? O1 Mg1 1.8080(5) 2_666 ? N1 C2 1.3328(16) . ? N1 C6 1.4399(16) . ? C1 C2 1.5224(18) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? O2 C30 1.4545(16) . ? O2 C33 1.4570(16) . ? N2 C4 1.3345(16) . ? N2 C18 1.4410(16) . ? C2 C3 1.4110(18) . ? C3 C4 1.4075(18) . ? C3 H3 0.9500 . ? C4 C5 1.5207(17) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 C7 1.4076(18) . ? C6 C11 1.4095(18) . ? C7 C8 1.3972(19) . ? C7 C12 1.5145(18) . ? C8 C9 1.382(2) . ? C8 H8 0.9500 . ? C9 C10 1.384(2) . ? C9 H9 0.9500 . ? C10 C11 1.397(2) . ? C10 H10 0.9500 . ? C11 C15 1.523(2) . ? C12 C13 1.528(2) . ? C12 C14 1.533(2) . ? C12 H12 1.0000 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C16 1.532(2) . ? C15 C17 1.533(2) . ? C15 H15 1.0000 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C19 1.4052(19) . ? C18 C23 1.4105(18) . ? C19 C20 1.4027(19) . ? C19 C24 1.5191(19) . ? C20 C21 1.384(2) . ? C20 H20 0.9500 . ? C21 C22 1.389(2) . ? C21 H21 0.9500 . ? C22 C23 1.3971(19) . ? C22 H22 0.9500 . ? C23 C27 1.524(2) . ? C24 C25 1.527(2) . ? C24 C26 1.534(2) . ? C24 H24 1.0000 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C29 1.5334(19) . ? C27 C28 1.5350(19) . ? C27 H27 1.0000 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 C31 1.506(2) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 C32 1.528(2) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 C33 1.512(2) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 C35 1.385(2) . ? C34 C36 1.386(2) 2_675 ? C34 H34 0.9500 . ? C35 C36 1.376(2) . ? C35 H35 0.9500 . ? C36 C34 1.386(2) 2_675 ? C36 H36 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Mg1 O2 103.20(3) . . ? O1 Mg1 N2 127.83(4) . . ? O2 Mg1 N2 99.93(4) . . ? O1 Mg1 N1 130.08(4) . . ? O2 Mg1 N1 99.27(4) . . ? N2 Mg1 N1 90.36(5) . . ? O1 Mg1 Mg1 0.0 . 2_666 ? O2 Mg1 Mg1 103.20(3) . 2_666 ? N2 Mg1 Mg1 127.83(4) . 2_666 ? N1 Mg1 Mg1 130.08(4) . 2_666 ? Mg1 O1 Mg1 180.000(1) 2_666 . ? C2 N1 C6 116.91(11) . . ? C2 N1 Mg1 117.81(9) . . ? C6 N1 Mg1 124.37(8) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C30 O2 C33 109.65(10) . . ? C30 O2 Mg1 131.13(8) . . ? C33 O2 Mg1 119.20(8) . . ? C4 N2 C18 116.84(10) . . ? C4 N2 Mg1 118.39(9) . . ? C18 N2 Mg1 124.45(8) . . ? N1 C2 C3 124.39(12) . . ? N1 C2 C1 120.46(12) . . ? C3 C2 C1 115.15(11) . . ? C4 C3 C2 129.18(12) . . ? C4 C3 H3 115.4 . . ? C2 C3 H3 115.4 . . ? N2 C4 C3 124.16(11) . . ? N2 C4 C5 120.53(12) . . ? C3 C4 C5 115.31(11) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C7 C6 C11 120.30(12) . . ? C7 C6 N1 120.61(11) . . ? C11 C6 N1 119.09(12) . . ? C8 C7 C6 118.87(13) . . ? C8 C7 C12 119.77(12) . . ? C6 C7 C12 121.34(12) . . ? C9 C8 C7 121.29(14) . . ? C9 C8 H8 119.4 . . ? C7 C8 H8 119.4 . . ? C8 C9 C10 119.44(13) . . ? C8 C9 H9 120.3 . . ? C10 C9 H9 120.3 . . ? C9 C10 C11 121.50(14) . . ? C9 C10 H10 119.2 . . ? C11 C10 H10 119.2 . . ? C10 C11 C6 118.55(13) . . ? C10 C11 C15 119.64(13) . . ? C6 C11 C15 121.80(12) . . ? C7 C12 C13 109.56(12) . . ? C7 C12 C14 112.81(12) . . ? C13 C12 C14 110.83(13) . . ? C7 C12 H12 107.8 . . ? C13 C12 H12 107.8 . . ? C14 C12 H12 107.8 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C11 C15 C16 111.88(13) . . ? C11 C15 C17 111.07(13) . . ? C16 C15 C17 110.46(13) . . ? C11 C15 H15 107.7 . . ? C16 C15 H15 107.7 . . ? C17 C15 H15 107.7 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C19 C18 C23 120.80(12) . . ? C19 C18 N2 121.28(11) . . ? C23 C18 N2 117.90(11) . . ? C20 C19 C18 118.42(13) . . ? C20 C19 C24 119.66(12) . . ? C18 C19 C24 121.88(12) . . ? C21 C20 C19 121.19(13) . . ? C21 C20 H20 119.4 . . ? C19 C20 H20 119.4 . . ? C20 C21 C22 119.75(13) . . ? C20 C21 H21 120.1 . . ? C22 C21 H21 120.1 . . ? C21 C22 C23 121.06(13) . . ? C21 C22 H22 119.5 . . ? C23 C22 H22 119.5 . . ? C22 C23 C18 118.54(13) . . ? C22 C23 C27 120.79(12) . . ? C18 C23 C27 120.65(12) . . ? C19 C24 C25 109.57(12) . . ? C19 C24 C26 113.10(12) . . ? C25 C24 C26 110.71(14) . . ? C19 C24 H24 107.8 . . ? C25 C24 H24 107.8 . . ? C26 C24 H24 107.8 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C23 C27 C29 112.64(12) . . ? C23 C27 C28 113.12(12) . . ? C29 C27 C28 109.65(12) . . ? C23 C27 H27 107.0 . . ? C29 C27 H27 107.0 . . ? C28 C27 H27 107.0 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? O2 C30 C31 105.83(12) . . ? O2 C30 H30A 110.6 . . ? C31 C30 H30A 110.6 . . ? O2 C30 H30B 110.6 . . ? C31 C30 H30B 110.6 . . ? H30A C30 H30B 108.7 . . ? C30 C31 C32 102.07(12) . . ? C30 C31 H31A 111.4 . . ? C32 C31 H31A 111.4 . . ? C30 C31 H31B 111.4 . . ? C32 C31 H31B 111.4 . . ? H31A C31 H31B 109.2 . . ? C33 C32 C31 102.59(12) . . ? C33 C32 H32A 111.2 . . ? C31 C32 H32A 111.2 . . ? C33 C32 H32B 111.2 . . ? C31 C32 H32B 111.2 . . ? H32A C32 H32B 109.2 . . ? O2 C33 C32 104.80(12) . . ? O2 C33 H33A 110.8 . . ? C32 C33 H33A 110.8 . . ? O2 C33 H33B 110.8 . . ? C32 C33 H33B 110.8 . . ? H33A C33 H33B 108.9 . . ? C35 C34 C36 119.75(16) . 2_675 ? C35 C34 H34 120.1 . . ? C36 C34 H34 120.1 2_675 . ? C36 C35 C34 119.79(15) . . ? C36 C35 H35 120.1 . . ? C34 C35 H35 120.1 . . ? C35 C36 C34 120.46(15) . 2_675 ? C35 C36 H36 119.8 . . ? C34 C36 H36 119.8 2_675 . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.041 _refine_diff_density_min -0.215 _refine_diff_density_rms 0.046 _database_code_depnum_ccdc_archive 'CCDC 955171' ####################################################################### # # 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_compound3S _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C73 H106 Mg2 N4 O4' _chemical_formula_weight 1152.24 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mg Mg 0.0486 0.0363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.749(3) _cell_length_b 14.372(3) _cell_length_c 18.802(4) _cell_angle_alpha 90.00 _cell_angle_beta 95.03(3) _cell_angle_gamma 90.00 _cell_volume 3431.7(12) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.115 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1256 _exptl_absorpt_coefficient_mu 0.084 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.959 _exptl_absorpt_correction_T_max 0.975 _exptl_absorpt_process_details 'Sortav (Blessing)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(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 'Bruker Apex' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12479 _diffrn_reflns_av_R_equivalents 0.0210 _diffrn_reflns_av_sigmaI/netI 0.0341 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.95 _diffrn_reflns_theta_max 26.00 _reflns_number_total 6667 _reflns_number_gt 5153 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. A molecule of toluene of crystallisation was located in the asymmetric unit. Attempts to model disorder in this molecule were not successful. As a result, its atomic positions were refined isotropically at 50% occupancy. The apparent poorly ordered nature of the atomic sites of the toluene molecule gave rise to the Level A alert in the cifcheck file for the structure. Using the SQUEEZE command of Platon to deal with this alert was considered, but rejected as it was thought best to present the refinement of the structure with unaltered data in this case. ; _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^)+(0.1144P)^2^+3.7969P] 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 6667 _refine_ls_number_parameters 382 _refine_ls_number_restraints 39 _refine_ls_R_factor_all 0.0973 _refine_ls_R_factor_gt 0.0786 _refine_ls_wR_factor_ref 0.2273 _refine_ls_wR_factor_gt 0.2112 _refine_ls_goodness_of_fit_ref 1.062 _refine_ls_restrained_S_all 1.150 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mg1 Mg 0.11975(6) 0.93799(6) 0.02429(5) 0.0246(2) Uani 1 1 d . . . O1 O -0.01889(15) 0.99019(15) 0.03844(10) 0.0354(5) Uani 1 1 d . . . O2 O 0.21401(15) 1.04569(14) 0.06573(13) 0.0397(5) Uani 1 1 d . . . N1 N 0.22273(18) 0.87134(18) -0.04061(12) 0.0332(6) Uani 1 1 d . . . N2 N 0.15238(16) 0.83572(15) 0.10262(11) 0.0246(5) Uani 1 1 d . . . C1 C 0.4035(3) 0.8132(3) -0.05252(19) 0.0563(11) Uani 1 1 d . . . H1A H 0.3879 0.7590 -0.0833 0.084 Uiso 1 1 calc R . . H1B H 0.4659 0.8003 -0.0198 0.084 Uiso 1 1 calc R . . H1C H 0.4170 0.8674 -0.0820 0.084 Uiso 1 1 calc R . . C2 C 0.3105(2) 0.8331(2) -0.00995(16) 0.0355(7) Uani 1 1 d . . . C3 C 0.3242(2) 0.8075(2) 0.06221(15) 0.0318(6) Uani 1 1 d . . . H3 H 0.3943 0.7922 0.0796 0.038 Uiso 1 1 calc R . . C4 C 0.2491(2) 0.80118(19) 0.11255(14) 0.0273(6) Uani 1 1 d . . . C5 C 0.2857(2) 0.7499(2) 0.18081(15) 0.0370(7) Uani 1 1 d . . . H5A H 0.2891 0.7934 0.2211 0.056 Uiso 1 1 calc R . . H5B H 0.3557 0.7234 0.1765 0.056 Uiso 1 1 calc R . . H5C H 0.2360 0.6998 0.1889 0.056 Uiso 1 1 calc R . . C6 C 0.2125(2) 0.8776(3) -0.11777(16) 0.0447(9) Uani 1 1 d . . . C7 C 0.2504(2) 0.9555(3) -0.15156(19) 0.0587(12) Uani 1 1 d . . . C8 C 0.2390(3) 0.9561(5) -0.2278(2) 0.0833(19) Uani 1 1 d . . . H8 H 0.2650 1.0077 -0.2525 0.100 Uiso 1 1 calc R . . C9 C 0.1914(4) 0.8838(5) -0.2664(2) 0.0791(15) Uani 1 1 d U . . H9 H 0.1849 0.8855 -0.3171 0.095 Uiso 1 1 calc R . . C10 C 0.1540(4) 0.8108(4) -0.2316(2) 0.0755(15) Uani 1 1 d . . . H10 H 0.1213 0.7612 -0.2587 0.091 Uiso 1 1 calc R . . C11 C 0.1616(3) 0.8053(3) -0.15719(17) 0.0548(10) Uani 1 1 d . . . C12 C 0.3014(3) 1.0362(4) -0.1111(2) 0.0714(14) Uani 1 1 d . . . H12 H 0.3099 1.0191 -0.0594 0.086 Uiso 1 1 calc R . . C13 C 0.2326(3) 1.1227(4) -0.1190(3) 0.0775(14) Uani 1 1 d . . . H13A H 0.2249 1.1419 -0.1692 0.116 Uiso 1 1 calc R . . H13B H 0.2656 1.1730 -0.0898 0.116 Uiso 1 1 calc R . . H13C H 0.1631 1.1088 -0.1031 0.116 Uiso 1 1 calc R . . C14 C 0.4116(4) 1.0572(4) -0.1350(3) 0.0978(17) Uani 1 1 d U . . H14A H 0.4537 1.0000 -0.1329 0.147 Uiso 1 1 calc R . . H14B H 0.4465 1.1039 -0.1031 0.147 Uiso 1 1 calc R . . H14C H 0.4047 1.0810 -0.1840 0.147 Uiso 1 1 calc R . . C15 C 0.1168(4) 0.7221(3) -0.1212(2) 0.0712(13) Uani 1 1 d . . . H15 H 0.1020 0.7421 -0.0721 0.085 Uiso 1 1 calc R . . C16 C 0.1963(5) 0.6427(4) -0.1127(4) 0.111(2) Uani 1 1 d U . . H16A H 0.2235 0.6297 -0.1589 0.167 Uiso 1 1 calc R . . H16B H 0.1619 0.5869 -0.0959 0.167 Uiso 1 1 calc R . . H16C H 0.2547 0.6604 -0.0780 0.167 Uiso 1 1 calc R . . C17 C 0.0134(4) 0.6859(4) -0.1586(3) 0.0847(15) Uani 1 1 d . . . H17A H -0.0368 0.7373 -0.1660 0.127 Uiso 1 1 calc R . . H17B H -0.0160 0.6381 -0.1288 0.127 Uiso 1 1 calc R . . H17C H 0.0266 0.6589 -0.2048 0.127 Uiso 1 1 calc R . . C18 C 0.0798(2) 0.80993(19) 0.15380(14) 0.0279(6) Uani 1 1 d . . . C19 C 0.0709(2) 0.8629(2) 0.21522(15) 0.0338(6) Uani 1 1 d . . . C20 C -0.0003(3) 0.8324(3) 0.26342(17) 0.0484(9) Uani 1 1 d . . . H20 H -0.0076 0.8677 0.3054 0.058 Uiso 1 1 calc R . . C21 C -0.0591(3) 0.7538(3) 0.25163(19) 0.0522(9) Uani 1 1 d . . . H21 H -0.1049 0.7337 0.2858 0.063 Uiso 1 1 calc R . . C22 C -0.0516(3) 0.7040(3) 0.1901(2) 0.0486(9) Uani 1 1 d . . . H22 H -0.0937 0.6499 0.1817 0.058 Uiso 1 1 calc R . . C23 C 0.0163(2) 0.7307(2) 0.13944(18) 0.0390(7) Uani 1 1 d . . . C24 C 0.1323(2) 0.9518(2) 0.22925(17) 0.0393(7) Uani 1 1 d . . . H24 H 0.1802 0.9592 0.1903 0.047 Uiso 1 1 calc R . . C25 C 0.0590(3) 1.0357(3) 0.2265(2) 0.0536(9) Uani 1 1 d . . . H25A H 0.0137 1.0349 0.1816 0.080 Uiso 1 1 calc R . . H25B H 0.1009 1.0929 0.2293 0.080 Uiso 1 1 calc R . . H25C H 0.0153 1.0332 0.2668 0.080 Uiso 1 1 calc R . . C26 C 0.2008(3) 0.9503(3) 0.3003(2) 0.0654(11) Uani 1 1 d . . . H26A H 0.1561 0.9412 0.3395 0.098 Uiso 1 1 calc R . . H26B H 0.2385 1.0095 0.3068 0.098 Uiso 1 1 calc R . . H26C H 0.2517 0.8992 0.3000 0.098 Uiso 1 1 calc R . . C27 C 0.0192(3) 0.6773(3) 0.0701(2) 0.0618(11) Uani 1 1 d . . . H27 H 0.0437 0.7221 0.0343 0.074 Uiso 1 1 calc R . . C28 C -0.0876(4) 0.6419(3) 0.0396(2) 0.0667(11) Uani 1 1 d . . . H28A H -0.0824 0.6190 -0.0091 0.100 Uiso 1 1 calc R . . H28B H -0.1390 0.6926 0.0386 0.100 Uiso 1 1 calc R . . H28C H -0.1103 0.5911 0.0695 0.100 Uiso 1 1 calc R . . C29 C 0.0964(4) 0.5992(4) 0.0750(4) 0.0987(18) Uani 1 1 d U . . H29A H 0.1675 0.6239 0.0865 0.148 Uiso 1 1 calc R . . H29B H 0.0933 0.5662 0.0293 0.148 Uiso 1 1 calc R . . H29C H 0.0791 0.5560 0.1126 0.148 Uiso 1 1 calc R . . C30 C 0.3214(2) 1.0457(2) 0.0986(2) 0.0454(8) Uani 1 1 d . . . H30A H 0.3723 1.0461 0.0617 0.055 Uiso 1 1 calc R . . H30B H 0.3347 0.9901 0.1291 0.055 Uiso 1 1 calc R . . C31 C 0.3311(3) 1.1316(3) 0.1419(3) 0.0666(12) Uani 1 1 d . . . H31A H 0.4048 1.1542 0.1471 0.080 Uiso 1 1 calc R . . H31B H 0.3068 1.1214 0.1898 0.080 Uiso 1 1 calc R . . C32 C 0.2599(4) 1.1994(3) 0.0987(3) 0.0707(12) Uani 1 1 d . . . H32A H 0.2347 1.2491 0.1295 0.085 Uiso 1 1 calc R . . H32B H 0.2968 1.2282 0.0601 0.085 Uiso 1 1 calc R . . C33 C 0.1702(3) 1.1392(2) 0.0687(2) 0.0488(9) Uani 1 1 d . . . H33A H 0.1116 1.1407 0.0999 0.059 Uiso 1 1 calc R . . H33B H 0.1437 1.1606 0.0204 0.059 Uiso 1 1 calc R . . C34 C -0.0762(7) 1.0194(7) 0.4970(6) 0.096(3) Uiso 0.50 1 d PD A -1 C35 C 0.0036(9) 1.0728(10) 0.4665(10) 0.146(6) Uiso 0.50 1 d PD A -1 H35 H -0.0123 1.1301 0.4427 0.175 Uiso 0.50 1 calc PR A -1 C36 C 0.1066(9) 1.0367(10) 0.4734(9) 0.143(6) Uiso 0.50 1 d PD A -1 H36 H 0.1608 1.0712 0.4539 0.171 Uiso 0.50 1 calc PR A -1 C37 C 0.1332(7) 0.9517(9) 0.5080(8) 0.107(4) Uiso 0.50 1 d PD A -1 H37 H 0.2032 0.9284 0.5100 0.128 Uiso 0.50 1 calc PR A -1 C38 C 0.0528(7) 0.9010(8) 0.5401(7) 0.105(4) Uiso 0.50 1 d PD A -1 H38 H 0.0682 0.8446 0.5651 0.126 Uiso 0.50 1 calc PR A -1 C39 C -0.0539(6) 0.9392(5) 0.5329(4) 0.0527(17) Uiso 0.50 1 d PD A -1 H39 H -0.1086 0.9072 0.5539 0.063 Uiso 0.50 1 calc PR A -1 C40 C -0.1844(10) 1.0609(18) 0.4873(19) 0.285(17) Uiso 0.50 1 d PD A -1 H40A H -0.2140 1.0513 0.4380 0.427 Uiso 0.50 1 calc PR A -1 H40B H -0.1804 1.1277 0.4976 0.427 Uiso 0.50 1 calc PR A -1 H40C H -0.2296 1.0307 0.5201 0.427 Uiso 0.50 1 calc PR A -1 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 Mg1 0.0213(4) 0.0273(5) 0.0252(5) 0.0042(3) 0.0021(3) 0.0007(3) O1 0.0290(10) 0.0489(13) 0.0290(11) 0.0090(9) 0.0062(8) 0.0065(9) O2 0.0275(10) 0.0274(11) 0.0626(14) 0.0037(10) -0.0054(9) -0.0023(8) N1 0.0284(11) 0.0454(15) 0.0265(12) 0.0074(10) 0.0064(9) 0.0084(10) N2 0.0253(11) 0.0239(11) 0.0250(11) 0.0015(9) 0.0044(8) -0.0005(9) C1 0.0394(17) 0.088(3) 0.0432(19) 0.0231(19) 0.0149(14) 0.0291(18) C2 0.0291(14) 0.0439(17) 0.0345(15) 0.0072(13) 0.0080(11) 0.0082(12) C3 0.0235(12) 0.0376(16) 0.0340(15) 0.0054(12) 0.0005(11) 0.0073(11) C4 0.0288(13) 0.0256(13) 0.0268(13) 0.0019(11) -0.0010(10) 0.0020(11) C5 0.0380(15) 0.0424(17) 0.0305(15) 0.0088(13) 0.0019(12) 0.0111(13) C6 0.0312(15) 0.075(2) 0.0293(15) 0.0143(16) 0.0106(12) 0.0252(16) C7 0.0251(15) 0.108(3) 0.0439(19) 0.036(2) 0.0082(13) 0.0147(18) C8 0.040(2) 0.157(5) 0.056(3) 0.064(3) 0.0237(19) 0.035(3) C9 0.064(2) 0.139(4) 0.035(2) 0.009(3) 0.0096(19) 0.043(3) C10 0.089(3) 0.110(4) 0.0289(18) -0.005(2) 0.0084(19) 0.059(3) C11 0.064(2) 0.073(3) 0.0274(16) -0.0066(16) 0.0044(15) 0.038(2) C12 0.0378(18) 0.107(4) 0.068(3) 0.059(3) -0.0034(18) -0.014(2) C13 0.047(2) 0.110(4) 0.075(3) 0.037(3) 0.003(2) -0.014(2) C14 0.051(2) 0.114(4) 0.129(4) 0.065(3) 0.006(2) -0.006(2) C15 0.127(4) 0.048(2) 0.0355(19) -0.0157(17) -0.009(2) 0.025(2) C16 0.121(4) 0.071(3) 0.130(4) -0.009(3) -0.054(3) 0.019(3) C17 0.102(4) 0.082(3) 0.069(3) -0.024(3) -0.003(3) 0.022(3) C18 0.0276(13) 0.0285(14) 0.0279(13) 0.0069(11) 0.0039(10) 0.0037(11) C19 0.0316(14) 0.0425(17) 0.0274(14) 0.0022(12) 0.0026(11) 0.0083(12) C20 0.0442(18) 0.075(3) 0.0268(15) 0.0073(16) 0.0088(13) 0.0123(18) C21 0.0389(17) 0.077(3) 0.0423(19) 0.0280(18) 0.0121(14) 0.0004(17) C22 0.0414(17) 0.046(2) 0.059(2) 0.0206(17) 0.0093(15) -0.0071(15) C23 0.0390(16) 0.0309(16) 0.0483(18) 0.0069(13) 0.0104(13) -0.0039(13) C24 0.0391(16) 0.0445(18) 0.0341(16) -0.0123(13) 0.0013(12) 0.0060(13) C25 0.056(2) 0.046(2) 0.056(2) -0.0117(17) -0.0080(17) 0.0125(17) C26 0.068(3) 0.065(3) 0.059(2) -0.016(2) -0.021(2) 0.011(2) C27 0.070(2) 0.042(2) 0.077(3) -0.0201(19) 0.028(2) -0.0237(18) C28 0.083(3) 0.044(2) 0.070(3) -0.0025(19) -0.009(2) -0.006(2) C29 0.076(3) 0.083(3) 0.135(4) -0.054(3) -0.002(3) 0.004(3) C30 0.0279(15) 0.0462(19) 0.060(2) -0.0001(16) -0.0060(14) -0.0070(13) C31 0.050(2) 0.064(3) 0.084(3) -0.024(2) -0.003(2) -0.0111(19) C32 0.072(3) 0.035(2) 0.101(3) -0.006(2) -0.013(2) -0.0123(19) C33 0.0479(18) 0.0257(16) 0.071(2) 0.0017(15) -0.0030(17) -0.0009(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mg1 O1 1.960(2) . ? Mg1 O1 1.961(2) 3_575 ? Mg1 O2 2.069(2) . ? Mg1 N2 2.096(2) . ? Mg1 N1 2.100(3) . ? O1 O1 1.588(4) 3_575 ? O1 Mg1 1.961(2) 3_575 ? O2 C30 1.452(3) . ? O2 C33 1.458(4) . ? N1 C2 1.332(4) . ? N1 C6 1.448(4) . ? N2 C4 1.328(3) . ? N2 C18 1.441(3) . ? C1 C2 1.515(4) . ? C2 C3 1.402(4) . ? C3 C4 1.407(4) . ? C4 C5 1.518(4) . ? C6 C7 1.394(5) . ? C6 C11 1.403(6) . ? C7 C8 1.428(6) . ? C7 C12 1.502(7) . ? C8 C9 1.378(8) . ? C9 C10 1.346(8) . ? C10 C11 1.397(5) . ? C11 C15 1.510(6) . ? C12 C13 1.521(7) . ? C12 C14 1.542(6) . ? C15 C16 1.526(7) . ? C15 C17 1.531(7) . ? C18 C19 1.396(4) . ? C18 C23 1.409(4) . ? C19 C20 1.408(4) . ? C19 C24 1.508(5) . ? C20 C21 1.364(6) . ? C21 C22 1.370(6) . ? C22 C23 1.396(4) . ? C23 C27 1.517(5) . ? C24 C25 1.524(5) . ? C24 C26 1.531(5) . ? C27 C29 1.490(7) . ? C27 C28 1.518(6) . ? C30 C31 1.478(5) . ? C31 C32 1.517(6) . ? C32 C33 1.504(5) . ? C34 C39 1.353(7) . ? C34 C35 1.434(8) . ? C34 C40 1.499(8) . ? C35 C36 1.408(9) . ? C36 C37 1.412(9) . ? C37 C38 1.434(8) . ? C38 C39 1.462(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Mg1 O1 47.81(10) . 3_575 ? O1 Mg1 O2 99.41(10) . . ? O1 Mg1 O2 99.28(10) 3_575 . ? O1 Mg1 N2 107.38(9) . . ? O1 Mg1 N2 150.57(9) 3_575 . ? O2 Mg1 N2 100.78(9) . . ? O1 Mg1 N1 150.54(10) . . ? O1 Mg1 N1 107.52(9) 3_575 . ? O2 Mg1 N1 100.83(10) . . ? N2 Mg1 N1 89.59(9) . . ? O1 O1 Mg1 66.13(13) 3_575 . ? O1 O1 Mg1 66.07(13) 3_575 3_575 ? Mg1 O1 Mg1 132.19(10) . 3_575 ? C30 O2 C33 109.5(2) . . ? C30 O2 Mg1 130.93(19) . . ? C33 O2 Mg1 119.46(18) . . ? C2 N1 C6 117.2(2) . . ? C2 N1 Mg1 118.76(19) . . ? C6 N1 Mg1 123.23(18) . . ? C4 N2 C18 116.9(2) . . ? C4 N2 Mg1 119.05(18) . . ? C18 N2 Mg1 123.37(16) . . ? N1 C2 C3 123.8(2) . . ? N1 C2 C1 121.1(3) . . ? C3 C2 C1 115.1(3) . . ? C2 C3 C4 129.3(2) . . ? N2 C4 C3 124.1(2) . . ? N2 C4 C5 120.9(2) . . ? C3 C4 C5 115.0(2) . . ? C7 C6 C11 121.1(3) . . ? C7 C6 N1 120.2(4) . . ? C11 C6 N1 118.7(3) . . ? C6 C7 C8 117.0(5) . . ? C6 C7 C12 122.7(3) . . ? C8 C7 C12 120.3(4) . . ? C9 C8 C7 121.7(5) . . ? C10 C9 C8 119.4(4) . . ? C9 C10 C11 122.3(5) . . ? C10 C11 C6 118.4(4) . . ? C10 C11 C15 119.9(4) . . ? C6 C11 C15 121.7(3) . . ? C7 C12 C13 111.2(3) . . ? C7 C12 C14 111.7(5) . . ? C13 C12 C14 110.1(4) . . ? C11 C15 C16 111.4(5) . . ? C11 C15 C17 114.1(4) . . ? C16 C15 C17 109.3(4) . . ? C19 C18 C23 120.8(3) . . ? C19 C18 N2 121.0(2) . . ? C23 C18 N2 118.1(2) . . ? C18 C19 C20 117.8(3) . . ? C18 C19 C24 121.9(3) . . ? C20 C19 C24 120.3(3) . . ? C21 C20 C19 122.0(3) . . ? C20 C21 C22 119.5(3) . . ? C21 C22 C23 121.7(3) . . ? C22 C23 C18 118.1(3) . . ? C22 C23 C27 120.7(3) . . ? C18 C23 C27 121.1(3) . . ? C19 C24 C25 110.9(3) . . ? C19 C24 C26 112.9(3) . . ? C25 C24 C26 110.0(3) . . ? C29 C27 C23 113.1(4) . . ? C29 C27 C28 109.7(3) . . ? C23 C27 C28 113.9(3) . . ? O2 C30 C31 105.3(3) . . ? C30 C31 C32 103.0(3) . . ? C33 C32 C31 103.4(3) . . ? O2 C33 C32 105.3(3) . . ? C39 C34 C35 122.0(6) . . ? C39 C34 C40 123.3(8) . . ? C35 C34 C40 114.6(8) . . ? C36 C35 C34 117.0(7) . . ? C35 C36 C37 123.2(7) . . ? C36 C37 C38 118.8(7) . . ? C37 C38 C39 117.7(6) . . ? C34 C39 C38 121.2(6) . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 1.244 _refine_diff_density_min -0.520 _refine_diff_density_rms 0.063 _database_code_depnum_ccdc_archive 'CCDC 955172' ####################################################################### # # 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_compound4 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C59 H82 Mg2 N4 O S2' _chemical_formula_weight 976.03 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mg Mg 0.0486 0.0363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 14.860(3) _cell_length_b 17.210(3) _cell_length_c 45.300(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 11585(4) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.119 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4224 _exptl_absorpt_coefficient_mu 0.154 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.992 _exptl_absorpt_correction_T_max 0.996 _exptl_absorpt_process_details XDS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71080 _diffrn_radiation_type Synchrotron _diffrn_radiation_source 'Australian Synchrotron' _diffrn_radiation_monochromator ? _diffrn_measurement_device_type 'ADSC Quantum 210r' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 146059 _diffrn_reflns_av_R_equivalents 0.1193 _diffrn_reflns_av_sigmaI/netI 0.0408 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -54 _diffrn_reflns_limit_l_max 54 _diffrn_reflns_theta_min 2.97 _diffrn_reflns_theta_max 25.20 _reflns_number_total 10405 _reflns_number_gt 8925 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Blu-Ice (McPhillips, 2002)' _computing_cell_refinement 'XDS (Kabsch, 1993)' _computing_data_reduction 'XDS (Kabsch, 1993)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics X-Seed _computing_publication_material CifTAB _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. The atoms of two isopropyl groups of the compound were found to be disordered over two sites each. This dosorder was successfully modelled and the carbon atoms of both disordered sets refined anisotropically. ; _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^)+(0.0200P)^2^+65.1041P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0049(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 10405 _refine_ls_number_parameters 694 _refine_ls_number_restraints 80 _refine_ls_R_factor_all 0.1105 _refine_ls_R_factor_gt 0.0989 _refine_ls_wR_factor_ref 0.2218 _refine_ls_wR_factor_gt 0.2167 _refine_ls_goodness_of_fit_ref 1.220 _refine_ls_restrained_S_all 1.241 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group S1 S 0.72608(8) 0.51602(7) 0.09835(3) 0.0251(3) Uani 1 1 d . . . Mg1 Mg 0.70451(10) 0.65639(9) 0.09127(3) 0.0188(4) Uani 1 1 d . . . O1 O 0.6272(2) 0.61758(19) 0.12552(7) 0.0211(7) Uani 1 1 d . . . N1 N 0.6524(3) 0.7284(2) 0.06057(8) 0.0184(8) Uani 1 1 d . . . C1 C 0.6540(3) 0.8479(3) 0.03060(11) 0.0284(11) Uani 1 1 d . . . H1A H 0.6500 0.8204 0.0117 0.043 Uiso 1 1 calc R . . H1B H 0.6919 0.8941 0.0283 0.043 Uiso 1 1 calc R . . H1C H 0.5937 0.8637 0.0369 0.043 Uiso 1 1 calc R . . S2 S 0.62482(9) 0.48837(8) 0.15522(3) 0.0280(3) Uani 1 1 d . . . Mg2 Mg 0.53708(11) 0.60902(11) 0.15939(4) 0.0266(4) Uani 1 1 d . . . N2 N 0.8272(3) 0.7077(2) 0.09246(8) 0.0199(8) Uani 1 1 d . . . C2 C 0.6947(3) 0.7951(3) 0.05347(10) 0.0205(10) Uani 1 1 d . . . N3 N 0.5184(3) 0.7029(3) 0.18563(9) 0.0330(11) Uani 1 1 d . . . C3 C 0.7769(3) 0.8195(3) 0.06539(11) 0.0226(10) Uani 1 1 d . . . H3 H 0.7919 0.8722 0.0615 0.027 Uiso 1 1 calc R . . N4 N 0.4051(3) 0.5793(3) 0.15771(10) 0.0325(11) Uani 1 1 d . . . C4 C 0.8407(3) 0.7787(3) 0.08210(10) 0.0222(10) Uani 1 1 d . . . C5 C 0.9303(4) 0.8197(3) 0.08701(13) 0.0341(13) Uani 1 1 d . . . H5A H 0.9198 0.8697 0.0967 0.051 Uiso 1 1 calc R . . H5B H 0.9599 0.8283 0.0680 0.051 Uiso 1 1 calc R . . H5C H 0.9689 0.7873 0.0995 0.051 Uiso 1 1 calc R . . C6 C 0.5719(3) 0.7091(3) 0.04412(9) 0.0174(9) Uani 1 1 d . . . C7 C 0.4883(3) 0.7413(3) 0.05239(10) 0.0223(10) Uani 1 1 d . . . C8 C 0.4120(3) 0.7203(3) 0.03614(11) 0.0251(11) Uani 1 1 d . . . H8 H 0.3553 0.7415 0.0415 0.030 Uiso 1 1 calc R . . C9 C 0.4171(4) 0.6694(3) 0.01246(11) 0.0284(11) Uani 1 1 d . . . H9 H 0.3647 0.6563 0.0015 0.034 Uiso 1 1 calc R . . C10 C 0.5001(3) 0.6378(3) 0.00507(11) 0.0261(11) Uani 1 1 d . . . H10 H 0.5040 0.6031 -0.0112 0.031 Uiso 1 1 calc R . . C11 C 0.5776(3) 0.6555(3) 0.02082(10) 0.0231(10) Uani 1 1 d . . . C12 C 0.4786(3) 0.7960(3) 0.07842(11) 0.0230(10) Uani 1 1 d . . . H12 H 0.5399 0.8158 0.0835 0.028 Uiso 1 1 calc R . . C13 C 0.4425(4) 0.7527(3) 0.10525(11) 0.0329(12) Uani 1 1 d . . . H13A H 0.3833 0.7308 0.1006 0.049 Uiso 1 1 calc R . . H13B H 0.4370 0.7887 0.1219 0.049 Uiso 1 1 calc R . . H13C H 0.4840 0.7106 0.1105 0.049 Uiso 1 1 calc R . . C14 C 0.4188(4) 0.8665(3) 0.07192(12) 0.0347(13) Uani 1 1 d . . . H14A H 0.4378 0.8905 0.0533 0.052 Uiso 1 1 calc R . . H14B H 0.4245 0.9043 0.0880 0.052 Uiso 1 1 calc R . . H14C H 0.3560 0.8497 0.0703 0.052 Uiso 1 1 calc R . . C15 C 0.6666(3) 0.6196(3) 0.01166(11) 0.0259(11) Uani 1 1 d . . . H15 H 0.7124 0.6329 0.0270 0.031 Uiso 1 1 calc R . . C16 C 0.6598(4) 0.5306(3) 0.00983(12) 0.0329(12) Uani 1 1 d . . . H16A H 0.6414 0.5099 0.0291 0.049 Uiso 1 1 calc R . . H16B H 0.7185 0.5090 0.0044 0.049 Uiso 1 1 calc R . . H16C H 0.6152 0.5162 -0.0051 0.049 Uiso 1 1 calc R . . C17 C 0.6990(5) 0.6528(4) -0.01791(14) 0.0482(17) Uani 1 1 d . . . H17A H 0.6567 0.6380 -0.0335 0.072 Uiso 1 1 calc R . . H17B H 0.7587 0.6320 -0.0225 0.072 Uiso 1 1 calc R . . H17C H 0.7021 0.7095 -0.0166 0.072 Uiso 1 1 calc R . . C18 C 0.9039(3) 0.6621(3) 0.10209(11) 0.0222(10) Uani 1 1 d . . . C19 C 0.9236(3) 0.6553(3) 0.13218(11) 0.0303(12) Uani 1 1 d . . . C20 C 0.9954(4) 0.6077(4) 0.14000(12) 0.0358(13) Uani 1 1 d . . . H20 H 1.0105 0.6026 0.1603 0.043 Uiso 1 1 calc R . . C21 C 1.0457(3) 0.5673(3) 0.11928(12) 0.0336(13) Uani 1 1 d . . . H21 H 1.0938 0.5347 0.1254 0.040 Uiso 1 1 calc R . . C22 C 1.0250(3) 0.5750(3) 0.08983(12) 0.0276(11) Uani 1 1 d . . . H22 H 1.0588 0.5470 0.0756 0.033 Uiso 1 1 calc R . . C23 C 0.9548(3) 0.6235(3) 0.08058(11) 0.0235(10) Uani 1 1 d . . . C24 C 0.8694(4) 0.6970(4) 0.15542(12) 0.0400(14) Uani 1 1 d . . . H24 H 0.8194 0.7250 0.1451 0.048 Uiso 1 1 calc R . . C25 C 0.8273(4) 0.6419(4) 0.17733(14) 0.0444(16) Uani 1 1 d . . . H25A H 0.7928 0.6022 0.1668 0.067 Uiso 1 1 calc R . . H25B H 0.7871 0.6709 0.1905 0.067 Uiso 1 1 calc R . . H25C H 0.8747 0.6169 0.1890 0.067 Uiso 1 1 calc R . . C26 C 0.9265(5) 0.7578(4) 0.17129(14) 0.0480(16) Uani 1 1 d . . . H26A H 0.9792 0.7326 0.1801 0.072 Uiso 1 1 calc R . . H26B H 0.8906 0.7825 0.1868 0.072 Uiso 1 1 calc R . . H26C H 0.9463 0.7972 0.1571 0.072 Uiso 1 1 calc R . . C27 C 0.9349(4) 0.6311(3) 0.04768(11) 0.0307(12) Uani 1 1 d . . . H27 H 0.8834 0.6680 0.0453 0.037 Uiso 1 1 calc R . . C28 C 0.9072(5) 0.5531(4) 0.03444(13) 0.0449(15) Uani 1 1 d . . . H28A H 0.9580 0.5169 0.0354 0.067 Uiso 1 1 calc R . . H28B H 0.8895 0.5606 0.0138 0.067 Uiso 1 1 calc R . . H28C H 0.8563 0.5319 0.0456 0.067 Uiso 1 1 calc R . . C29 C 1.0150(5) 0.6638(4) 0.03093(15) 0.0541(18) Uani 1 1 d . . . H29A H 1.0660 0.6280 0.0326 0.081 Uiso 1 1 calc R . . H29B H 1.0316 0.7144 0.0393 0.081 Uiso 1 1 calc R . . H29C H 0.9991 0.6702 0.0101 0.081 Uiso 1 1 calc R . . C30 C 0.6582(3) 0.5446(3) 0.12647(10) 0.0206(10) Uani 1 1 d . . . C31 C 0.4267(5) 0.8050(4) 0.20892(14) 0.0543(19) Uani 1 1 d . . . H31A H 0.4466 0.7932 0.2290 0.081 Uiso 1 1 calc R . . H31B H 0.3635 0.8211 0.2093 0.081 Uiso 1 1 calc R . . H31C H 0.4636 0.8470 0.2008 0.081 Uiso 1 1 calc R . . C32 C 0.4365(4) 0.7332(4) 0.18983(11) 0.0359(14) Uani 1 1 d . . . C33 C 0.3575(4) 0.7026(4) 0.17819(12) 0.0374(14) Uani 1 1 d . . . H33 H 0.3066 0.7358 0.1794 0.045 Uiso 1 1 calc R . . C34 C 0.3413(4) 0.6300(4) 0.16498(12) 0.0358(14) Uani 1 1 d . . . C35 C 0.2433(4) 0.6101(4) 0.15896(16) 0.0490(17) Uani 1 1 d . . . H35A H 0.2326 0.6096 0.1376 0.073 Uiso 1 1 calc R . . H35B H 0.2044 0.6491 0.1682 0.073 Uiso 1 1 calc R . . H35C H 0.2296 0.5587 0.1672 0.073 Uiso 1 1 calc R . . C36 C 0.5944(4) 0.7369(4) 0.20159(12) 0.0494(19) Uani 1 1 d D A . C37 C 0.6371(4) 0.8038(4) 0.19153(15) 0.0502(18) Uani 1 1 d D . . C38 C 0.7108(5) 0.8329(5) 0.20704(18) 0.080(3) Uani 1 1 d D . . H38 H 0.7394 0.8789 0.2003 0.096 Uiso 1 1 calc R . . C39 C 0.7427(7) 0.7968(6) 0.23161(19) 0.087(3) Uani 1 1 d DU . . H39 H 0.7939 0.8166 0.2416 0.105 Uiso 1 1 calc R . . C40 C 0.7003(5) 0.7322(6) 0.24159(15) 0.072(2) Uani 1 1 d DU A . H40 H 0.7227 0.7092 0.2592 0.087 Uiso 1 1 calc R . . C41 C 0.6230(5) 0.6950(5) 0.22752(12) 0.076(3) Uani 1 1 d D . . C42 C 0.6072(4) 0.8456(4) 0.16406(15) 0.0435(16) Uani 1 1 d . . . H42 H 0.5457 0.8263 0.1590 0.052 Uiso 1 1 calc R . . C43 C 0.6692(4) 0.8267(3) 0.13797(14) 0.0420(15) Uani 1 1 d . . . H43A H 0.7305 0.8442 0.1425 0.063 Uiso 1 1 calc R . . H43B H 0.6474 0.8534 0.1202 0.063 Uiso 1 1 calc R . . H43C H 0.6695 0.7705 0.1345 0.063 Uiso 1 1 calc R . . C44 C 0.6014(5) 0.9346(4) 0.1675(2) 0.066(2) Uani 1 1 d . . . H44A H 0.5654 0.9473 0.1849 0.099 Uiso 1 1 calc R . . H44B H 0.5730 0.9570 0.1499 0.099 Uiso 1 1 calc R . . H44C H 0.6621 0.9560 0.1697 0.099 Uiso 1 1 calc R . . C45 C 0.5714(11) 0.6214(7) 0.2343(5) 0.116(12) Uani 0.55(2) 1 d PDU A 1 H45 H 0.5447 0.6008 0.2156 0.139 Uiso 0.55(2) 1 calc PR A 1 C46 C 0.6307(19) 0.5588(9) 0.2481(6) 0.124(10) Uani 0.55(2) 1 d PDU A 1 H46D H 0.6873 0.5551 0.2370 0.186 Uiso 0.55(2) 1 calc PR A 1 H46E H 0.5994 0.5087 0.2473 0.186 Uiso 0.55(2) 1 calc PR A 1 H46F H 0.6436 0.5723 0.2686 0.186 Uiso 0.55(2) 1 calc PR A 1 C47 C 0.4965(17) 0.6342(14) 0.2568(7) 0.154(12) Uani 0.55(2) 1 d PDU A 1 H47A H 0.5198 0.6641 0.2735 0.230 Uiso 0.55(2) 1 calc PR A 1 H47B H 0.4744 0.5838 0.2638 0.230 Uiso 0.55(2) 1 calc PR A 1 H47C H 0.4470 0.6628 0.2475 0.230 Uiso 0.55(2) 1 calc PR A 1 C48 C 0.3795(3) 0.5009(3) 0.14967(14) 0.0361(14) Uani 1 1 d . B . C49 C 0.3598(4) 0.4816(3) 0.12040(14) 0.0394(14) Uani 1 1 d . . . C50 C 0.3363(4) 0.4046(4) 0.11400(19) 0.0563(19) Uani 1 1 d . . . H50 H 0.3228 0.3902 0.0942 0.068 Uiso 1 1 calc R . . C51 C 0.3325(5) 0.3496(5) 0.1360(3) 0.082(3) Uani 1 1 d . . . H51 H 0.3140 0.2982 0.1314 0.098 Uiso 1 1 calc R . . C52 C 0.3548(5) 0.3679(4) 0.1643(2) 0.071(3) Uani 1 1 d . B . H52 H 0.3537 0.3285 0.1790 0.085 Uiso 1 1 calc R . . C53 C 0.3791(4) 0.4433(4) 0.17213(15) 0.0515(19) Uani 1 1 d D . . C54 C 0.3680(4) 0.5395(3) 0.09549(13) 0.0350(13) Uani 1 1 d . . . H54 H 0.3758 0.5921 0.1045 0.042 Uiso 1 1 calc R . . C55 C 0.4511(4) 0.5231(4) 0.07706(13) 0.0379(13) Uani 1 1 d . . . H55A H 0.5044 0.5233 0.0898 0.057 Uiso 1 1 calc R . . H55B H 0.4575 0.5633 0.0619 0.057 Uiso 1 1 calc R . . H55C H 0.4452 0.4721 0.0676 0.057 Uiso 1 1 calc R . . C56 C 0.2836(4) 0.5425(4) 0.07609(14) 0.0428(15) Uani 1 1 d . . . H56A H 0.2725 0.4910 0.0676 0.064 Uiso 1 1 calc R . . H56B H 0.2925 0.5803 0.0602 0.064 Uiso 1 1 calc R . . H56C H 0.2318 0.5580 0.0881 0.064 Uiso 1 1 calc R . . C57 C 0.4108(9) 0.4676(8) 0.2043(2) 0.051(3) Uani 0.72(3) 1 d PDU B 1 H57 H 0.4494 0.5147 0.2017 0.061 Uiso 0.72(3) 1 calc PR B 1 C58 C 0.4680(13) 0.4086(10) 0.2212(4) 0.051(4) Uani 0.72(3) 1 d PD B 1 H58D H 0.4315 0.3627 0.2257 0.077 Uiso 0.72(3) 1 calc PR B 1 H58E H 0.4896 0.4321 0.2396 0.077 Uiso 0.72(3) 1 calc PR B 1 H58F H 0.5195 0.3932 0.2090 0.077 Uiso 0.72(3) 1 calc PR B 1 C59 C 0.3330(13) 0.4924(14) 0.2244(3) 0.097(9) Uani 0.72(3) 1 d PD B 1 H59A H 0.3065 0.5408 0.2169 0.146 Uiso 0.72(3) 1 calc PR B 1 H59B H 0.3556 0.5008 0.2445 0.146 Uiso 0.72(3) 1 calc PR B 1 H59C H 0.2870 0.4516 0.2247 0.146 Uiso 0.72(3) 1 calc PR B 1 C45A C 0.5813(9) 0.6212(6) 0.2386(3) 0.041(5) Uani 0.45(2) 1 d PDU A 2 H45A H 0.5273 0.6039 0.2272 0.050 Uiso 0.45(2) 1 calc PR A 2 C46A C 0.6610(11) 0.5648(10) 0.2372(4) 0.055(5) Uani 0.45(2) 1 d PDU A 2 H46A H 0.7109 0.5855 0.2490 0.082 Uiso 0.45(2) 1 calc PR A 2 H46B H 0.6802 0.5587 0.2167 0.082 Uiso 0.45(2) 1 calc PR A 2 H46C H 0.6427 0.5142 0.2451 0.082 Uiso 0.45(2) 1 calc PR A 2 C47A C 0.5605(14) 0.6468(10) 0.2704(3) 0.060(6) Uani 0.45(2) 1 d PDU A 2 H47D H 0.6168 0.6583 0.2807 0.090 Uiso 0.45(2) 1 calc PR A 2 H47E H 0.5287 0.6049 0.2807 0.090 Uiso 0.45(2) 1 calc PR A 2 H47F H 0.5226 0.6934 0.2700 0.090 Uiso 0.45(2) 1 calc PR A 2 C57A C 0.3826(17) 0.4525(16) 0.2038(4) 0.035(8) Uani 0.28(3) 1 d PDU B 2 H57A H 0.4084 0.5048 0.2084 0.042 Uiso 0.28(3) 1 calc PR B 2 C58A C 0.448(3) 0.390(2) 0.2147(11) 0.042(10) Uani 0.28(3) 1 d PD B 2 H58A H 0.4195 0.3393 0.2137 0.063 Uiso 0.28(3) 1 calc PR B 2 H58B H 0.4653 0.4016 0.2352 0.063 Uiso 0.28(3) 1 calc PR B 2 H58C H 0.5022 0.3907 0.2023 0.063 Uiso 0.28(3) 1 calc PR B 2 C59A C 0.2895(18) 0.4469(17) 0.2179(5) 0.043(7) Uani 0.28(3) 1 d PD B 2 H59D H 0.2474 0.4803 0.2071 0.064 Uiso 0.28(3) 1 calc PR B 2 H59E H 0.2929 0.4639 0.2385 0.064 Uiso 0.28(3) 1 calc PR B 2 H59F H 0.2685 0.3930 0.2171 0.064 Uiso 0.28(3) 1 calc PR B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 S1 0.0273(6) 0.0200(6) 0.0279(6) -0.0012(5) 0.0088(5) 0.0005(5) Mg1 0.0182(8) 0.0201(8) 0.0179(8) 0.0014(6) -0.0007(6) 0.0002(6) O1 0.0209(16) 0.0202(17) 0.0222(17) 0.0026(14) 0.0026(13) 0.0039(14) N1 0.0188(19) 0.0174(19) 0.0191(19) 0.0008(16) -0.0033(16) -0.0049(16) C1 0.027(3) 0.026(3) 0.032(3) 0.009(2) -0.002(2) -0.002(2) S2 0.0267(6) 0.0279(7) 0.0293(7) 0.0096(5) 0.0076(5) 0.0045(5) Mg2 0.0244(8) 0.0370(10) 0.0184(8) 0.0039(7) 0.0054(7) 0.0105(8) N2 0.0171(19) 0.022(2) 0.0205(19) -0.0007(16) -0.0027(16) 0.0015(16) C2 0.023(2) 0.018(2) 0.021(2) -0.0009(19) 0.0023(19) -0.0010(19) N3 0.037(3) 0.045(3) 0.017(2) 0.000(2) -0.0005(18) 0.022(2) C3 0.023(2) 0.017(2) 0.028(2) 0.0002(19) 0.001(2) -0.0022(19) N4 0.027(2) 0.042(3) 0.029(2) 0.015(2) 0.0108(19) 0.008(2) C4 0.022(2) 0.022(2) 0.022(2) -0.004(2) 0.001(2) -0.002(2) C5 0.025(3) 0.027(3) 0.050(3) 0.005(2) -0.008(2) -0.004(2) C6 0.019(2) 0.017(2) 0.015(2) 0.0023(18) -0.0044(18) -0.0038(18) C7 0.021(2) 0.027(3) 0.020(2) 0.005(2) -0.0044(19) 0.000(2) C8 0.020(2) 0.027(3) 0.028(3) -0.002(2) -0.004(2) 0.002(2) C9 0.028(3) 0.029(3) 0.028(3) 0.000(2) -0.011(2) -0.005(2) C10 0.030(3) 0.028(3) 0.020(2) -0.009(2) -0.002(2) -0.002(2) C11 0.024(2) 0.024(3) 0.021(2) 0.004(2) -0.001(2) -0.004(2) C12 0.022(2) 0.021(2) 0.026(2) -0.001(2) -0.001(2) -0.001(2) C13 0.044(3) 0.033(3) 0.022(3) 0.000(2) -0.002(2) 0.002(3) C14 0.040(3) 0.029(3) 0.035(3) -0.002(2) -0.003(2) 0.007(2) C15 0.025(3) 0.025(3) 0.027(3) -0.008(2) 0.000(2) 0.000(2) C16 0.036(3) 0.026(3) 0.036(3) -0.005(2) 0.000(2) 0.004(2) C17 0.054(4) 0.035(3) 0.055(4) 0.004(3) 0.031(3) -0.004(3) C18 0.016(2) 0.024(2) 0.027(2) -0.002(2) -0.0005(19) 0.000(2) C19 0.026(3) 0.039(3) 0.026(3) -0.010(2) -0.007(2) 0.009(2) C20 0.029(3) 0.048(4) 0.030(3) -0.005(3) -0.008(2) 0.010(3) C21 0.019(3) 0.042(3) 0.040(3) 0.006(3) -0.006(2) 0.006(2) C22 0.020(2) 0.028(3) 0.035(3) 0.001(2) 0.004(2) 0.002(2) C23 0.021(2) 0.022(2) 0.028(3) 0.000(2) 0.002(2) -0.004(2) C24 0.039(3) 0.050(4) 0.031(3) -0.016(3) -0.008(3) 0.019(3) C25 0.028(3) 0.060(4) 0.045(4) -0.026(3) 0.001(3) -0.002(3) C26 0.070(5) 0.035(3) 0.039(3) -0.013(3) -0.002(3) 0.009(3) C27 0.030(3) 0.038(3) 0.024(3) 0.002(2) 0.003(2) 0.010(2) C28 0.051(4) 0.050(4) 0.034(3) -0.007(3) 0.000(3) -0.002(3) C29 0.059(4) 0.060(4) 0.043(4) 0.020(3) 0.016(3) 0.002(4) C30 0.018(2) 0.021(2) 0.022(2) 0.0011(19) 0.0006(19) -0.0011(19) C31 0.052(4) 0.068(5) 0.042(4) -0.013(3) 0.010(3) 0.032(4) C32 0.037(3) 0.050(4) 0.021(3) 0.008(2) 0.010(2) 0.019(3) C33 0.031(3) 0.050(4) 0.031(3) 0.017(3) 0.013(2) 0.021(3) C34 0.026(3) 0.047(3) 0.034(3) 0.017(3) 0.014(2) 0.011(3) C35 0.026(3) 0.053(4) 0.069(4) 0.019(3) 0.014(3) 0.006(3) C36 0.043(4) 0.083(5) 0.021(3) -0.025(3) -0.009(3) 0.037(4) C37 0.039(4) 0.059(4) 0.052(4) -0.034(4) -0.017(3) 0.020(3) C38 0.053(4) 0.104(7) 0.083(6) -0.066(5) -0.043(4) 0.036(5) C39 0.079(5) 0.105(6) 0.078(5) -0.044(4) -0.031(4) 0.030(4) C40 0.073(4) 0.110(5) 0.034(3) -0.025(4) -0.023(3) 0.052(4) C41 0.069(5) 0.135(8) 0.023(3) -0.036(4) -0.017(3) 0.074(5) C42 0.029(3) 0.039(3) 0.062(4) -0.028(3) -0.013(3) 0.010(3) C43 0.031(3) 0.033(3) 0.062(4) -0.018(3) -0.010(3) 0.004(3) C44 0.049(4) 0.038(4) 0.110(7) -0.039(4) -0.001(4) 0.008(3) C45 0.122(13) 0.125(13) 0.100(13) 0.007(7) 0.000(7) 0.025(7) C46 0.123(11) 0.124(11) 0.125(11) -0.001(7) -0.012(7) 0.012(7) C47 0.155(14) 0.156(14) 0.149(14) -0.003(7) 0.011(7) 0.006(7) C48 0.021(3) 0.031(3) 0.056(4) 0.023(3) 0.011(2) 0.002(2) C49 0.024(3) 0.036(3) 0.059(4) 0.018(3) 0.000(3) -0.005(2) C50 0.043(4) 0.035(4) 0.090(6) 0.013(4) -0.014(4) -0.014(3) C51 0.053(5) 0.050(5) 0.143(9) 0.045(6) -0.021(5) -0.024(4) C52 0.044(4) 0.050(5) 0.118(8) 0.054(5) 0.017(5) -0.006(3) C53 0.037(3) 0.051(4) 0.067(4) 0.032(3) 0.027(3) 0.013(3) C54 0.030(3) 0.032(3) 0.044(3) 0.005(3) -0.003(2) -0.005(2) C55 0.028(3) 0.038(3) 0.047(3) 0.004(3) -0.007(3) 0.001(2) C56 0.025(3) 0.052(4) 0.052(4) 0.005(3) -0.007(3) 0.002(3) C57 0.056(6) 0.052(6) 0.045(5) 0.024(4) 0.031(4) 0.013(5) C58 0.052(10) 0.052(8) 0.050(12) 0.005(7) 0.007(7) 0.010(8) C59 0.090(13) 0.129(19) 0.073(9) 0.046(11) 0.048(9) 0.068(14) C45A 0.058(7) 0.057(7) 0.010(5) 0.010(4) -0.002(4) 0.041(5) C46A 0.052(7) 0.054(7) 0.057(7) 0.000(5) 0.006(6) 0.018(5) C47A 0.070(8) 0.061(8) 0.050(7) 0.004(5) 0.011(5) 0.001(6) C57A 0.034(10) 0.030(9) 0.040(9) 0.006(6) 0.009(6) -0.005(6) C58A 0.038(17) 0.07(2) 0.019(15) 0.000(15) -0.014(11) -0.011(16) C59A 0.061(17) 0.039(14) 0.028(11) -0.011(10) 0.018(11) -0.009(13) _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 S1 C30 1.698(5) . ? S1 Mg1 2.458(2) . ? Mg1 N1 2.017(4) . ? Mg1 N2 2.026(4) . ? Mg1 O1 2.043(4) . ? Mg1 C30 2.592(5) . ? O1 C30 1.339(6) . ? O1 Mg2 2.042(4) . ? N1 C2 1.348(6) . ? N1 C6 1.448(6) . ? C1 C2 1.506(7) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? S2 C30 1.696(5) . ? S2 Mg2 2.459(2) . ? Mg2 N3 2.025(5) . ? Mg2 N4 2.028(5) . ? Mg2 C30 2.587(5) . ? N2 C4 1.324(6) . ? N2 C18 1.452(6) . ? C2 C3 1.400(7) . ? N3 C32 1.338(7) . ? N3 C36 1.462(8) . ? C3 C4 1.402(7) . ? C3 H3 0.9500 . ? N4 C34 1.330(7) . ? N4 C48 1.448(8) . ? C4 C5 1.523(7) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 C11 1.404(7) . ? C6 C7 1.411(7) . ? C7 C8 1.399(7) . ? C7 C12 1.516(7) . ? C8 C9 1.388(7) . ? C8 H8 0.9500 . ? C9 C10 1.390(7) . ? C9 H9 0.9500 . ? C10 C11 1.389(7) . ? C10 H10 0.9500 . ? C11 C15 1.517(7) . ? C12 C13 1.523(7) . ? C12 C14 1.532(7) . ? C12 H12 1.0000 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C17 1.533(7) . ? C15 C16 1.538(7) . ? C15 H15 1.0000 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C19 1.399(7) . ? C18 C23 1.401(7) . ? C19 C20 1.391(7) . ? C19 C24 1.506(7) . ? C20 C21 1.387(8) . ? C20 H20 0.9500 . ? C21 C22 1.376(7) . ? C21 H21 0.9500 . ? C22 C23 1.400(7) . ? C22 H22 0.9500 . ? C23 C27 1.525(7) . ? C24 C25 1.508(9) . ? C24 C26 1.527(8) . ? C24 H24 1.0000 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C29 1.520(8) . ? C27 C28 1.526(8) . ? C27 H27 1.0000 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C31 C32 1.515(9) . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 C33 1.391(9) . ? C33 C34 1.406(9) . ? C33 H33 0.9500 . ? C34 C35 1.521(8) . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 C37 1.392(9) . ? C36 C41 1.442(8) . ? C37 C38 1.393(8) . ? C37 C42 1.504(10) . ? C38 C39 1.360(11) . ? C38 H38 0.9500 . ? C39 C40 1.355(11) . ? C39 H39 0.9500 . ? C40 C41 1.462(10) . ? C40 H40 0.9500 . ? C41 C45A 1.500(8) . ? C41 C45 1.512(8) . ? C42 C43 1.534(9) . ? C42 C44 1.542(8) . ? C42 H42 1.0000 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 C46 1.524(7) . ? C45 C47 1.525(7) . ? C45 H45 1.0000 . ? C46 H46D 0.9800 . ? C46 H46E 0.9800 . ? C46 H46F 0.9800 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 C49 1.398(9) . ? C48 C53 1.421(8) . ? C49 C50 1.400(9) . ? C49 C54 1.511(8) . ? C50 C51 1.376(11) . ? C50 H50 0.9500 . ? C51 C52 1.360(13) . ? C51 H51 0.9500 . ? C52 C53 1.393(11) . ? C52 H52 0.9500 . ? C53 C57A 1.444(17) . ? C53 C57 1.587(13) . ? C54 C55 1.517(8) . ? C54 C56 1.533(8) . ? C54 H54 1.0000 . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? C57 C58 1.530(7) . ? C57 C59 1.533(7) . ? C57 H57 1.0000 . ? C58 H58D 0.9800 . ? C58 H58E 0.9800 . ? C58 H58F 0.9800 . ? C59 H59A 0.9800 . ? C59 H59B 0.9800 . ? C59 H59C 0.9800 . ? C45A C46A 1.532(7) . ? C45A C47A 1.534(7) . ? C45A H45A 1.0000 . ? C46A H46A 0.9800 . ? C46A H46B 0.9800 . ? C46A H46C 0.9800 . ? C47A H47D 0.9800 . ? C47A H47E 0.9800 . ? C47A H47F 0.9800 . ? C57A C59A 1.527(7) . ? C57A C58A 1.529(7) . ? C57A H57A 1.0000 . ? C58A H58A 0.9800 . ? C58A H58B 0.9800 . ? C58A H58C 0.9800 . ? C59A H59D 0.9800 . ? C59A H59E 0.9800 . ? C59A H59F 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C30 S1 Mg1 74.69(17) . . ? N1 Mg1 N2 95.50(16) . . ? N1 Mg1 O1 120.59(16) . . ? N2 Mg1 O1 128.91(16) . . ? N1 Mg1 S1 138.04(13) . . ? N2 Mg1 S1 107.93(13) . . ? O1 Mg1 S1 69.69(10) . . ? N1 Mg1 C30 141.09(16) . . ? N2 Mg1 C30 123.11(16) . . ? O1 Mg1 C30 30.76(14) . . ? S1 Mg1 C30 39.17(11) . . ? C30 O1 Mg2 97.7(3) . . ? C30 O1 Mg1 97.9(3) . . ? Mg2 O1 Mg1 164.39(19) . . ? C2 N1 C6 117.3(4) . . ? C2 N1 Mg1 120.6(3) . . ? C6 N1 Mg1 122.1(3) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C30 S2 Mg2 74.48(17) . . ? N3 Mg2 N4 95.2(2) . . ? N3 Mg2 O1 118.23(19) . . ? N4 Mg2 O1 128.64(18) . . ? N3 Mg2 S2 142.31(15) . . ? N4 Mg2 S2 107.26(16) . . ? O1 Mg2 S2 69.85(10) . . ? N3 Mg2 C30 140.86(19) . . ? N4 Mg2 C30 122.88(19) . . ? O1 Mg2 C30 30.86(14) . . ? S2 Mg2 C30 39.19(11) . . ? C4 N2 C18 119.0(4) . . ? C4 N2 Mg1 122.0(3) . . ? C18 N2 Mg1 118.6(3) . . ? N1 C2 C3 124.8(4) . . ? N1 C2 C1 119.4(4) . . ? C3 C2 C1 115.8(4) . . ? C32 N3 C36 118.4(5) . . ? C32 N3 Mg2 121.3(4) . . ? C36 N3 Mg2 120.2(3) . . ? C2 C3 C4 130.4(4) . . ? C2 C3 H3 114.8 . . ? C4 C3 H3 114.8 . . ? C34 N4 C48 119.1(5) . . ? C34 N4 Mg2 120.9(4) . . ? C48 N4 Mg2 119.9(3) . . ? N2 C4 C3 123.4(4) . . ? N2 C4 C5 120.6(4) . . ? C3 C4 C5 116.0(4) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C11 C6 C7 120.7(4) . . ? C11 C6 N1 119.2(4) . . ? C7 C6 N1 120.1(4) . . ? C8 C7 C6 118.2(4) . . ? C8 C7 C12 119.4(4) . . ? C6 C7 C12 122.3(4) . . ? C9 C8 C7 121.7(5) . . ? C9 C8 H8 119.1 . . ? C7 C8 H8 119.1 . . ? C8 C9 C10 118.8(5) . . ? C8 C9 H9 120.6 . . ? C10 C9 H9 120.6 . . ? C11 C10 C9 121.8(4) . . ? C11 C10 H10 119.1 . . ? C9 C10 H10 119.1 . . ? C10 C11 C6 118.7(4) . . ? C10 C11 C15 119.5(4) . . ? C6 C11 C15 121.7(4) . . ? C7 C12 C13 110.5(4) . . ? C7 C12 C14 113.4(4) . . ? C13 C12 C14 109.7(4) . . ? C7 C12 H12 107.7 . . ? C13 C12 H12 107.7 . . ? C14 C12 H12 107.7 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C11 C15 C17 111.2(5) . . ? C11 C15 C16 111.3(4) . . ? C17 C15 C16 110.1(4) . . ? C11 C15 H15 108.0 . . ? C17 C15 H15 108.0 . . ? C16 C15 H15 108.0 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C19 C18 C23 121.7(5) . . ? C19 C18 N2 120.1(4) . . ? C23 C18 N2 118.1(4) . . ? C20 C19 C18 117.2(5) . . ? C20 C19 C24 120.8(5) . . ? C18 C19 C24 122.0(5) . . ? C21 C20 C19 122.4(5) . . ? C21 C20 H20 118.8 . . ? C19 C20 H20 118.8 . . ? C22 C21 C20 119.2(5) . . ? C22 C21 H21 120.4 . . ? C20 C21 H21 120.4 . . ? C21 C22 C23 120.9(5) . . ? C21 C22 H22 119.5 . . ? C23 C22 H22 119.5 . . ? C22 C23 C18 118.5(5) . . ? C22 C23 C27 119.2(4) . . ? C18 C23 C27 122.3(4) . . ? C19 C24 C25 112.5(5) . . ? C19 C24 C26 111.0(5) . . ? C25 C24 C26 110.5(5) . . ? C19 C24 H24 107.5 . . ? C25 C24 H24 107.5 . . ? C26 C24 H24 107.5 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C29 C27 C23 111.6(5) . . ? C29 C27 C28 109.9(5) . . ? C23 C27 C28 111.2(5) . . ? C29 C27 H27 108.0 . . ? C23 C27 H27 108.0 . . ? C28 C27 H27 108.0 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? O1 C30 S2 117.3(3) . . ? O1 C30 S1 116.9(3) . . ? S2 C30 S1 125.8(3) . . ? O1 C30 Mg2 51.5(2) . . ? S2 C30 Mg2 66.34(16) . . ? S1 C30 Mg2 165.9(3) . . ? O1 C30 Mg1 51.3(2) . . ? S2 C30 Mg1 166.7(3) . . ? S1 C30 Mg1 66.14(16) . . ? Mg2 C30 Mg1 102.77(17) . . ? C32 C31 H31A 109.5 . . ? C32 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C32 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? N3 C32 C33 124.5(5) . . ? N3 C32 C31 119.2(6) . . ? C33 C32 C31 116.4(5) . . ? C32 C33 C34 130.0(5) . . ? C32 C33 H33 115.0 . . ? C34 C33 H33 115.0 . . ? N4 C34 C33 124.5(5) . . ? N4 C34 C35 119.4(6) . . ? C33 C34 C35 116.1(5) . . ? C34 C35 H35A 109.5 . . ? C34 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C34 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C37 C36 C41 123.1(6) . . ? C37 C36 N3 121.4(5) . . ? C41 C36 N3 115.5(7) . . ? C36 C37 C38 119.3(7) . . ? C36 C37 C42 122.1(5) . . ? C38 C37 C42 118.6(7) . . ? C39 C38 C37 121.5(10) . . ? C39 C38 H38 119.2 . . ? C37 C38 H38 119.2 . . ? C40 C39 C38 119.1(9) . . ? C40 C39 H39 120.5 . . ? C38 C39 H39 120.5 . . ? C39 C40 C41 125.4(7) . . ? C39 C40 H40 117.3 . . ? C41 C40 H40 117.3 . . ? C36 C41 C40 111.6(7) . . ? C36 C41 C45A 125.1(8) . . ? C40 C41 C45A 123.3(9) . . ? C36 C41 C45 115.9(10) . . ? C40 C41 C45 132.5(10) . . ? C45A C41 C45 9.3(12) . . ? C37 C42 C43 111.0(5) . . ? C37 C42 C44 114.1(6) . . ? C43 C42 C44 108.7(6) . . ? C37 C42 H42 107.6 . . ? C43 C42 H42 107.6 . . ? C44 C42 H42 107.6 . . ? C42 C43 H43A 109.5 . . ? C42 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C42 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C42 C44 H44A 109.5 . . ? C42 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C42 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C41 C45 C46 112.5(8) . . ? C41 C45 C47 112.7(8) . . ? C46 C45 C47 105(2) . . ? C41 C45 H45 109.0 . . ? C46 C45 H45 109.0 . . ? C47 C45 H45 109.0 . . ? C49 C48 C53 120.8(6) . . ? C49 C48 N4 121.0(5) . . ? C53 C48 N4 118.1(6) . . ? C48 C49 C50 118.3(6) . . ? C48 C49 C54 122.3(5) . . ? C50 C49 C54 119.3(6) . . ? C51 C50 C49 120.7(8) . . ? C51 C50 H50 119.6 . . ? C49 C50 H50 119.6 . . ? C52 C51 C50 120.9(8) . . ? C52 C51 H51 119.6 . . ? C50 C51 H51 119.6 . . ? C51 C52 C53 121.3(7) . . ? C51 C52 H52 119.4 . . ? C53 C52 H52 119.4 . . ? C52 C53 C48 117.9(7) . . ? C52 C53 C57A 111.4(13) . . ? C48 C53 C57A 129.4(13) . . ? C52 C53 C57 123.8(8) . . ? C48 C53 C57 118.2(7) . . ? C57A C53 C57 18.0(10) . . ? C49 C54 C55 110.7(5) . . ? C49 C54 C56 112.6(5) . . ? C55 C54 C56 110.9(5) . . ? C49 C54 H54 107.5 . . ? C55 C54 H54 107.5 . . ? C56 C54 H54 107.5 . . ? C54 C55 H55A 109.5 . . ? C54 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? C54 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? C54 C56 H56A 109.5 . . ? C54 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C54 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? C58 C57 C59 107.9(11) . . ? C58 C57 C53 116.6(9) . . ? C59 C57 C53 113.3(10) . . ? C58 C57 H57 106.1 . . ? C59 C57 H57 106.1 . . ? C53 C57 H57 106.1 . . ? C41 C45A C46A 101.7(11) . . ? C41 C45A C47A 98.9(10) . . ? C46A C45A C47A 112.1(13) . . ? C41 C45A H45A 114.2 . . ? C46A C45A H45A 114.2 . . ? C47A C45A H45A 114.2 . . ? C45A C46A H46A 109.5 . . ? C45A C46A H46B 109.5 . . ? H46A C46A H46B 109.5 . . ? C45A C46A H46C 109.5 . . ? H46A C46A H46C 109.5 . . ? H46B C46A H46C 109.5 . . ? C45A C47A H47D 109.5 . . ? C45A C47A H47E 109.5 . . ? H47D C47A H47E 109.5 . . ? C45A C47A H47F 109.5 . . ? H47D C47A H47F 109.5 . . ? H47E C47A H47F 109.5 . . ? C53 C57A C59A 112.1(16) . . ? C53 C57A C58A 106(2) . . ? C59A C57A C58A 114(3) . . ? C53 C57A H57A 108.5 . . ? C59A C57A H57A 108.5 . . ? C58A C57A H57A 108.5 . . ? C57A C58A H58A 109.5 . . ? C57A C58A H58B 109.5 . . ? H58A C58A H58B 109.5 . . ? C57A C58A H58C 109.5 . . ? H58A C58A H58C 109.5 . . ? H58B C58A H58C 109.5 . . ? C57A C59A H59D 109.5 . . ? C57A C59A H59E 109.5 . . ? H59D C59A H59E 109.5 . . ? C57A C59A H59F 109.5 . . ? H59D C59A H59F 109.5 . . ? H59E C59A H59F 109.5 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.20 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.086 _refine_diff_density_min -0.604 _refine_diff_density_rms 0.084 _database_code_depnum_ccdc_archive 'CCDC 955173' ####################################################################### # # 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_compound5 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C83 H116 Mg2 N6 O' _chemical_formula_weight 1262.44 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mg Mg 0.0486 0.0363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M P3(1)21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z+1/3' '-x+y, -x, z+2/3' 'x-y, -y, -z+2/3' '-x, -x+y, -z+1/3' 'y, x, -z' _cell_length_a 12.0374(17) _cell_length_b 12.0374(17) _cell_length_c 44.799(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 5621.6(16) _cell_formula_units_Z 3 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.119 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2064 _exptl_absorpt_coefficient_mu 0.080 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.972 _exptl_absorpt_correction_T_max 0.984 _exptl_absorpt_process_details 'SCALE3 ABSPACK' _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Gemini Ultra' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30360 _diffrn_reflns_av_R_equivalents 0.0413 _diffrn_reflns_av_sigmaI/netI 0.0400 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -56 _diffrn_reflns_limit_l_max 49 _diffrn_reflns_theta_min 1.95 _diffrn_reflns_theta_max 27.96 _reflns_number_total 8072 _reflns_number_gt 7357 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. A molecule of benzene of crystallisation was located in the asymmetric unit and its C-atoms refined anisotropically. ; _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^)+(0.0416P)^2^+0.7012P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.05(17) _refine_ls_number_reflns 8072 _refine_ls_number_parameters 426 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0457 _refine_ls_R_factor_gt 0.0389 _refine_ls_wR_factor_ref 0.0900 _refine_ls_wR_factor_gt 0.0868 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.051 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mg1 Mg 0.10624(5) 0.14196(5) 0.044619(10) 0.01701(11) Uani 1 1 d . . . O1 O 0.12586(11) 0.12586(11) 0.0000 0.0185(3) Uani 1 2 d S . . N1 N -0.07636(12) 0.08754(12) 0.05877(3) 0.0178(3) Uani 1 1 d . . . C1 C -0.27749(14) -0.05176(16) 0.08601(3) 0.0239(3) Uani 1 1 d . . . H1A H -0.2868 0.0233 0.0899 0.036 Uiso 1 1 calc R . . H1B H -0.3020 -0.1061 0.1039 0.036 Uiso 1 1 calc R . . H1C H -0.3331 -0.1008 0.0693 0.036 Uiso 1 1 calc R . . N2 N 0.14023(12) 0.06150(12) 0.08171(3) 0.0181(3) Uani 1 1 d . . . C2 C -0.13918(14) -0.00800(14) 0.07817(3) 0.0193(3) Uani 1 1 d . . . N3 N 0.26277(12) 0.29643(12) 0.02653(3) 0.0190(3) Uani 1 1 d . . . C3 C -0.08533(15) -0.07337(15) 0.09248(3) 0.0208(3) Uani 1 1 d . . . H3 H -0.1448 -0.1519 0.1018 0.025 Uiso 1 1 calc R . . C4 C 0.04465(15) -0.03926(15) 0.09506(3) 0.0200(3) Uani 1 1 d . . . C5 C 0.07097(16) -0.12706(16) 0.11444(4) 0.0285(4) Uani 1 1 d . . . H5A H 0.0624 -0.1989 0.1024 0.043 Uiso 1 1 calc R . . H5B H 0.0093 -0.1600 0.1309 0.043 Uiso 1 1 calc R . . H5C H 0.1582 -0.0789 0.1225 0.043 Uiso 1 1 calc R . . C6 C -0.14396(14) 0.14681(15) 0.04621(3) 0.0190(3) Uani 1 1 d . . . C7 C -0.11728(14) 0.26772(15) 0.05696(3) 0.0215(3) Uani 1 1 d . . . C8 C -0.18403(16) 0.32348(16) 0.04497(4) 0.0252(3) Uani 1 1 d . . . H8 H -0.1697 0.4032 0.0527 0.030 Uiso 1 1 calc R . . C9 C -0.27114(16) 0.26519(16) 0.02202(4) 0.0275(4) Uani 1 1 d . . . H9 H -0.3152 0.3052 0.0139 0.033 Uiso 1 1 calc R . . C10 C -0.29379(15) 0.14871(16) 0.01101(3) 0.0250(3) Uani 1 1 d . . . H10 H -0.3527 0.1100 -0.0050 0.030 Uiso 1 1 calc R . . C11 C -0.23242(14) 0.08636(15) 0.02275(3) 0.0202(3) Uani 1 1 d . . . C12 C -0.01913(16) 0.33474(15) 0.08173(4) 0.0261(4) Uani 1 1 d . . . H12 H 0.0513 0.3149 0.0785 0.031 Uiso 1 1 calc R . . C13 C 0.0420(2) 0.48058(18) 0.08120(5) 0.0399(5) Uani 1 1 d . . . H13A H -0.0218 0.5043 0.0871 0.060 Uiso 1 1 calc R . . H13B H 0.0727 0.5123 0.0610 0.060 Uiso 1 1 calc R . . H13C H 0.1143 0.5187 0.0952 0.060 Uiso 1 1 calc R . . C14 C -0.07641(19) 0.2826(2) 0.11269(4) 0.0383(4) Uani 1 1 d . . . H14A H -0.0113 0.3288 0.1280 0.058 Uiso 1 1 calc R . . H14B H -0.1045 0.1910 0.1137 0.058 Uiso 1 1 calc R . . H14C H -0.1500 0.2949 0.1161 0.058 Uiso 1 1 calc R . . C15 C -0.26297(15) -0.04353(16) 0.01022(3) 0.0227(3) Uani 1 1 d . . . H15 H -0.2295 -0.0836 0.0245 0.027 Uiso 1 1 calc R . . C16 C -0.19706(17) -0.02882(17) -0.01993(3) 0.0294(4) Uani 1 1 d . . . H16A H -0.2297 0.0089 -0.0344 0.044 Uiso 1 1 calc R . . H16B H -0.2151 -0.1132 -0.0270 0.044 Uiso 1 1 calc R . . H16C H -0.1042 0.0273 -0.0176 0.044 Uiso 1 1 calc R . . C17 C -0.40739(16) -0.13445(17) 0.00659(4) 0.0298(4) Uani 1 1 d . . . H17A H -0.4508 -0.1398 0.0255 0.045 Uiso 1 1 calc R . . H17B H -0.4233 -0.2199 0.0010 0.045 Uiso 1 1 calc R . . H17C H -0.4405 -0.1018 -0.0090 0.045 Uiso 1 1 calc R . . C18 C 0.26911(15) 0.10796(14) 0.09207(3) 0.0185(3) Uani 1 1 d . . . C19 C 0.31541(15) 0.19721(15) 0.11592(3) 0.0212(3) Uani 1 1 d . . . C20 C 0.44416(16) 0.25169(16) 0.12404(4) 0.0270(4) Uani 1 1 d . . . H20 H 0.4766 0.3119 0.1400 0.032 Uiso 1 1 calc R . . C21 C 0.52512(16) 0.21984(17) 0.10942(4) 0.0292(4) Uani 1 1 d . . . H21 H 0.6128 0.2591 0.1151 0.035 Uiso 1 1 calc R . . C22 C 0.47890(15) 0.13088(16) 0.08654(4) 0.0262(3) Uani 1 1 d . . . H22 H 0.5352 0.1089 0.0767 0.031 Uiso 1 1 calc R . . C23 C 0.35064(15) 0.07283(15) 0.07772(3) 0.0210(3) Uani 1 1 d . . . C24 C 0.22661(17) 0.22884(17) 0.13370(4) 0.0306(4) Uani 1 1 d . . . H24 H 0.1495 0.2060 0.1211 0.037 Uiso 1 1 calc R . . C25 C 0.2868(2) 0.36988(18) 0.14229(4) 0.0396(5) Uani 1 1 d . . . H25A H 0.3545 0.3913 0.1571 0.059 Uiso 1 1 calc R . . H25B H 0.2209 0.3857 0.1508 0.059 Uiso 1 1 calc R . . H25C H 0.3238 0.4233 0.1245 0.059 Uiso 1 1 calc R . . C26 C 0.1815(3) 0.1483(2) 0.16193(5) 0.0710(9) Uani 1 1 d . . . H26A H 0.1380 0.0571 0.1566 0.106 Uiso 1 1 calc R . . H26B H 0.1218 0.1669 0.1727 0.106 Uiso 1 1 calc R . . H26C H 0.2555 0.1689 0.1747 0.106 Uiso 1 1 calc R . . C27 C 0.30188(15) -0.02658(15) 0.05282(3) 0.0226(3) Uani 1 1 d . . . H27 H 0.2074 -0.0615 0.0509 0.027 Uiso 1 1 calc R . . C28 C 0.36333(16) 0.03329(16) 0.02294(4) 0.0279(4) Uani 1 1 d . . . H28A H 0.4559 0.0662 0.0240 0.042 Uiso 1 1 calc R . . H28B H 0.3477 0.1039 0.0184 0.042 Uiso 1 1 calc R . . H28C H 0.3259 -0.0318 0.0072 0.042 Uiso 1 1 calc R . . C29 C 0.3230(2) -0.13869(18) 0.06066(4) 0.0347(4) Uani 1 1 d . . . H29A H 0.2884 -0.2028 0.0447 0.052 Uiso 1 1 calc R . . H29B H 0.2789 -0.1780 0.0794 0.052 Uiso 1 1 calc R . . H29C H 0.4150 -0.1070 0.0629 0.052 Uiso 1 1 calc R . . C30 C 0.23988(17) 0.23988(17) 0.0000 0.0179(4) Uani 1 2 d S . . C31 C 0.37744(15) 0.41736(14) 0.03420(3) 0.0207(3) Uani 1 1 d . . . H31 H 0.4058 0.4748 0.0163 0.025 Uiso 1 1 calc R . . C32 C 0.34161(17) 0.48002(16) 0.05906(4) 0.0296(4) Uani 1 1 d . . . H32A H 0.3038 0.4190 0.0759 0.036 Uiso 1 1 calc R . . H32B H 0.2758 0.4995 0.0516 0.036 Uiso 1 1 calc R . . C33 C 0.45795(19) 0.60419(17) 0.07034(4) 0.0368(4) Uani 1 1 d . . . H33A H 0.4884 0.6696 0.0543 0.044 Uiso 1 1 calc R . . H33B H 0.4318 0.6375 0.0875 0.044 Uiso 1 1 calc R . . C34 C 0.56636(19) 0.58236(18) 0.07972(4) 0.0399(5) Uani 1 1 d . . . H34A H 0.6417 0.6653 0.0855 0.048 Uiso 1 1 calc R . . H34B H 0.5395 0.5251 0.0973 0.048 Uiso 1 1 calc R . . C35 C 0.60329(17) 0.52288(18) 0.05473(4) 0.0367(4) Uani 1 1 d . . . H35A H 0.6715 0.5060 0.0617 0.044 Uiso 1 1 calc R . . H35B H 0.6376 0.5834 0.0377 0.044 Uiso 1 1 calc R . . C36 C 0.48731(16) 0.39735(16) 0.04441(4) 0.0270(4) Uani 1 1 d . . . H36A H 0.5132 0.3612 0.0277 0.032 Uiso 1 1 calc R . . H36B H 0.4573 0.3347 0.0610 0.032 Uiso 1 1 calc R . . C37 C -0.2620(3) -0.3986(2) 0.15245(6) 0.0655(8) Uani 1 1 d D . . H37 H -0.2436 -0.3301 0.1391 0.079 Uiso 1 1 calc R . . C38 C -0.3579(2) -0.4352(2) 0.17326(7) 0.0626(7) Uani 1 1 d D . . H38 H -0.4055 -0.3919 0.1746 0.075 Uiso 1 1 calc R . . C39 C -0.3840(2) -0.5354(3) 0.19205(5) 0.0602(7) Uani 1 1 d D . . H39 H -0.4501 -0.5622 0.2065 0.072 Uiso 1 1 calc R . . C40 C -0.3143(3) -0.5962(3) 0.18982(5) 0.0650(7) Uani 1 1 d D . . H40 H -0.3328 -0.6660 0.2027 0.078 Uiso 1 1 calc R . . C41 C -0.2196(3) -0.5584(2) 0.16953(5) 0.0619(7) Uani 1 1 d D . . H41 H -0.1715 -0.6012 0.1684 0.074 Uiso 1 1 calc R . . C42 C -0.1924(3) -0.4609(2) 0.15086(5) 0.0596(6) Uani 1 1 d D . . H42 H -0.1255 -0.4349 0.1366 0.072 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 Mg1 0.0158(2) 0.0182(3) 0.0152(2) 0.00023(19) 0.00082(18) 0.0071(2) O1 0.0168(5) 0.0168(5) 0.0164(6) -0.0004(3) 0.0004(3) 0.0043(6) N1 0.0176(6) 0.0198(6) 0.0164(6) 0.0005(5) 0.0009(5) 0.0095(5) C1 0.0195(8) 0.0271(9) 0.0231(7) 0.0050(7) 0.0042(6) 0.0102(7) N2 0.0182(6) 0.0203(6) 0.0150(6) -0.0008(5) -0.0011(5) 0.0089(5) C2 0.0176(7) 0.0193(7) 0.0180(7) -0.0024(6) 0.0010(6) 0.0069(6) N3 0.0180(6) 0.0176(6) 0.0174(6) -0.0016(5) 0.0009(5) 0.0058(5) C3 0.0182(8) 0.0190(8) 0.0202(7) 0.0038(6) 0.0026(6) 0.0056(6) C4 0.0216(8) 0.0205(8) 0.0174(7) -0.0003(6) -0.0006(6) 0.0102(6) C5 0.0258(9) 0.0284(9) 0.0303(8) 0.0093(7) -0.0008(7) 0.0128(7) C6 0.0156(7) 0.0211(8) 0.0198(7) 0.0039(6) 0.0042(6) 0.0088(6) C7 0.0210(8) 0.0228(8) 0.0200(7) 0.0032(6) 0.0059(6) 0.0106(7) C8 0.0277(9) 0.0227(8) 0.0283(8) 0.0032(7) 0.0065(7) 0.0149(7) C9 0.0251(9) 0.0315(9) 0.0322(8) 0.0082(7) 0.0045(7) 0.0189(8) C10 0.0186(8) 0.0314(9) 0.0239(8) 0.0050(7) 0.0014(6) 0.0117(7) C11 0.0175(8) 0.0231(8) 0.0188(7) 0.0048(6) 0.0044(6) 0.0093(7) C12 0.0268(9) 0.0240(8) 0.0274(8) -0.0043(6) 0.0006(7) 0.0125(7) C13 0.0401(11) 0.0305(10) 0.0477(11) -0.0099(9) -0.0047(9) 0.0166(9) C14 0.0402(11) 0.0447(12) 0.0260(9) -0.0049(8) -0.0011(8) 0.0182(10) C15 0.0199(8) 0.0252(8) 0.0207(7) 0.0016(6) -0.0008(6) 0.0095(7) C16 0.0278(9) 0.0320(9) 0.0258(8) -0.0015(7) 0.0037(7) 0.0131(8) C17 0.0240(9) 0.0287(9) 0.0298(8) -0.0021(7) 0.0005(7) 0.0079(7) C18 0.0177(7) 0.0184(7) 0.0181(7) 0.0005(6) -0.0014(6) 0.0080(6) C19 0.0242(8) 0.0226(8) 0.0169(7) -0.0008(6) -0.0013(6) 0.0117(7) C20 0.0284(9) 0.0249(8) 0.0248(8) -0.0053(7) -0.0080(7) 0.0111(7) C21 0.0196(8) 0.0321(9) 0.0334(9) -0.0053(7) -0.0093(7) 0.0110(7) C22 0.0215(8) 0.0294(9) 0.0303(8) -0.0028(7) -0.0014(7) 0.0147(7) C23 0.0200(8) 0.0206(8) 0.0209(7) -0.0003(6) -0.0002(6) 0.0091(7) C24 0.0287(9) 0.0368(10) 0.0270(8) -0.0109(7) -0.0016(7) 0.0169(8) C25 0.0551(13) 0.0374(11) 0.0320(9) -0.0030(8) 0.0080(9) 0.0275(10) C26 0.107(2) 0.0419(13) 0.0579(14) 0.0080(11) 0.0548(15) 0.0326(14) C27 0.0188(8) 0.0243(8) 0.0241(8) -0.0061(6) -0.0016(6) 0.0104(7) C28 0.0305(9) 0.0290(9) 0.0256(8) -0.0043(7) -0.0017(7) 0.0161(8) C29 0.0484(11) 0.0312(9) 0.0279(9) -0.0056(7) -0.0033(8) 0.0225(9) C30 0.0176(7) 0.0176(7) 0.0184(10) 0.0007(4) -0.0007(4) 0.0087(9) C31 0.0208(8) 0.0178(8) 0.0179(7) -0.0017(6) 0.0012(6) 0.0054(6) C32 0.0283(9) 0.0259(9) 0.0282(8) -0.0069(7) 0.0040(7) 0.0088(7) C33 0.0424(11) 0.0252(9) 0.0316(9) -0.0109(7) 0.0032(8) 0.0083(9) C34 0.0384(11) 0.0265(10) 0.0318(9) -0.0066(8) -0.0081(8) -0.0012(8) C35 0.0238(9) 0.0315(10) 0.0435(11) -0.0035(8) -0.0068(8) 0.0053(8) C36 0.0220(8) 0.0241(8) 0.0308(8) -0.0029(7) -0.0031(7) 0.0084(7) C37 0.0798(19) 0.0313(12) 0.0670(16) 0.0054(11) -0.0227(15) 0.0139(12) C38 0.0470(14) 0.0472(14) 0.092(2) -0.0377(14) -0.0301(14) 0.0226(12) C39 0.0477(14) 0.0760(18) 0.0363(12) -0.0209(12) -0.0053(10) 0.0156(13) C40 0.0776(18) 0.0691(17) 0.0404(12) 0.0164(12) -0.0030(12) 0.0307(15) C41 0.0798(18) 0.0590(16) 0.0602(14) 0.0010(12) 0.0060(13) 0.0448(14) C42 0.0704(17) 0.0566(15) 0.0439(12) -0.0009(11) 0.0111(11) 0.0257(13) _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 Mg1 O1 2.0334(6) . ? Mg1 N3 2.0398(14) . ? Mg1 N1 2.0548(13) . ? Mg1 N2 2.0646(13) . ? Mg1 C30 2.4650(13) . ? O1 C30 1.372(2) . ? O1 Mg1 2.0334(6) 6 ? N1 C2 1.3341(19) . ? N1 C6 1.4382(19) . ? C1 C2 1.515(2) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? N2 C4 1.3257(19) . ? N2 C18 1.4379(19) . ? C2 C3 1.400(2) . ? N3 C30 1.3282(14) . ? N3 C31 1.4606(19) . ? C3 C4 1.410(2) . ? C3 H3 0.9500 . ? C4 C5 1.519(2) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 C7 1.409(2) . ? C6 C11 1.412(2) . ? C7 C8 1.387(2) . ? C7 C12 1.525(2) . ? C8 C9 1.383(2) . ? C8 H8 0.9500 . ? C9 C10 1.379(2) . ? C9 H9 0.9500 . ? C10 C11 1.393(2) . ? C10 H10 0.9500 . ? C11 C15 1.523(2) . ? C12 C13 1.527(2) . ? C12 C14 1.536(2) . ? C12 H12 1.0000 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C17 1.531(2) . ? C15 C16 1.531(2) . ? C15 H15 1.0000 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C23 1.404(2) . ? C18 C19 1.417(2) . ? C19 C20 1.396(2) . ? C19 C24 1.526(2) . ? C20 C21 1.378(2) . ? C20 H20 0.9500 . ? C21 C22 1.382(2) . ? C21 H21 0.9500 . ? C22 C23 1.396(2) . ? C22 H22 0.9500 . ? C23 C27 1.523(2) . ? C24 C26 1.519(3) . ? C24 C25 1.525(3) . ? C24 H24 1.0000 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C28 1.525(2) . ? C27 C29 1.534(2) . ? C27 H27 1.0000 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 N3 1.3282(14) 6 ? C30 Mg1 2.4650(13) 6 ? C31 C32 1.523(2) . ? C31 C36 1.528(2) . ? C31 H31 1.0000 . ? C32 C33 1.535(2) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C34 1.514(3) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 C35 1.510(3) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 C36 1.529(2) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 C38 1.374(4) . ? C37 C42 1.377(4) . ? C37 H37 0.9500 . ? C38 C39 1.372(4) . ? C38 H38 0.9500 . ? C39 C40 1.365(4) . ? C39 H39 0.9500 . ? C40 C41 1.346(3) . ? C40 H40 0.9500 . ? C41 C42 1.342(3) . ? C41 H41 0.9500 . ? C42 H42 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Mg1 N3 66.30(5) . . ? O1 Mg1 N1 115.44(5) . . ? N3 Mg1 N1 140.04(6) . . ? O1 Mg1 N2 133.37(4) . . ? N3 Mg1 N2 115.98(5) . . ? N1 Mg1 N2 91.92(5) . . ? O1 Mg1 C30 33.83(6) . . ? N3 Mg1 C30 32.59(5) . . ? N1 Mg1 C30 137.81(4) . . ? N2 Mg1 C30 129.93(4) . . ? C30 O1 Mg1 90.60(4) . 6 ? C30 O1 Mg1 90.60(4) . . ? Mg1 O1 Mg1 178.81(9) 6 . ? C2 N1 C6 117.71(12) . . ? C2 N1 Mg1 122.06(10) . . ? C6 N1 Mg1 120.10(9) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C4 N2 C18 118.96(12) . . ? C4 N2 Mg1 120.50(10) . . ? C18 N2 Mg1 120.38(9) . . ? N1 C2 C3 124.09(14) . . ? N1 C2 C1 120.10(13) . . ? C3 C2 C1 115.80(13) . . ? C30 N3 C31 124.88(14) . . ? C30 N3 Mg1 91.60(11) . . ? C31 N3 Mg1 142.84(10) . . ? C2 C3 C4 129.20(14) . . ? C2 C3 H3 115.4 . . ? C4 C3 H3 115.4 . . ? N2 C4 C3 123.96(14) . . ? N2 C4 C5 120.47(14) . . ? C3 C4 C5 115.57(14) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C7 C6 C11 120.68(14) . . ? C7 C6 N1 119.05(13) . . ? C11 C6 N1 120.24(13) . . ? C8 C7 C6 118.65(14) . . ? C8 C7 C12 120.59(14) . . ? C6 C7 C12 120.74(14) . . ? C9 C8 C7 121.20(15) . . ? C9 C8 H8 119.4 . . ? C7 C8 H8 119.4 . . ? C10 C9 C8 119.75(15) . . ? C10 C9 H9 120.1 . . ? C8 C9 H9 120.1 . . ? C9 C10 C11 121.61(15) . . ? C9 C10 H10 119.2 . . ? C11 C10 H10 119.2 . . ? C10 C11 C6 118.04(14) . . ? C10 C11 C15 119.54(14) . . ? C6 C11 C15 122.42(13) . . ? C7 C12 C13 113.42(14) . . ? C7 C12 C14 111.73(14) . . ? C13 C12 C14 110.06(15) . . ? C7 C12 H12 107.1 . . ? C13 C12 H12 107.1 . . ? C14 C12 H12 107.1 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C11 C15 C17 112.21(14) . . ? C11 C15 C16 111.17(13) . . ? C17 C15 C16 109.06(13) . . ? C11 C15 H15 108.1 . . ? C17 C15 H15 108.1 . . ? C16 C15 H15 108.1 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C23 C18 C19 120.30(14) . . ? C23 C18 N2 121.05(13) . . ? C19 C18 N2 118.51(13) . . ? C20 C19 C18 118.45(15) . . ? C20 C19 C24 119.89(14) . . ? C18 C19 C24 121.58(14) . . ? C21 C20 C19 121.26(15) . . ? C21 C20 H20 119.4 . . ? C19 C20 H20 119.4 . . ? C20 C21 C22 120.08(15) . . ? C20 C21 H21 120.0 . . ? C22 C21 H21 120.0 . . ? C21 C22 C23 120.90(15) . . ? C21 C22 H22 119.6 . . ? C23 C22 H22 119.6 . . ? C22 C23 C18 118.98(14) . . ? C22 C23 C27 119.73(14) . . ? C18 C23 C27 121.29(14) . . ? C26 C24 C25 108.67(15) . . ? C26 C24 C19 110.30(16) . . ? C25 C24 C19 114.02(15) . . ? C26 C24 H24 107.9 . . ? C25 C24 H24 107.9 . . ? C19 C24 H24 107.9 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C23 C27 C28 111.49(13) . . ? C23 C27 C29 110.82(13) . . ? C28 C27 C29 111.24(13) . . ? C23 C27 H27 107.7 . . ? C28 C27 H27 107.7 . . ? C29 C27 H27 107.7 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? N3 C30 N3 137.8(2) 6 . ? N3 C30 O1 111.10(10) 6 . ? N3 C30 O1 111.10(10) . . ? N3 C30 Mg1 55.81(7) 6 6 ? N3 C30 Mg1 165.69(13) . 6 ? O1 C30 Mg1 55.57(4) . 6 ? N3 C30 Mg1 165.69(13) 6 . ? N3 C30 Mg1 55.81(7) . . ? O1 C30 Mg1 55.57(4) . . ? Mg1 C30 Mg1 111.14(8) 6 . ? N3 C31 C32 107.76(12) . . ? N3 C31 C36 112.00(13) . . ? C32 C31 C36 109.93(13) . . ? N3 C31 H31 109.0 . . ? C32 C31 H31 109.0 . . ? C36 C31 H31 109.0 . . ? C31 C32 C33 112.11(14) . . ? C31 C32 H32A 109.2 . . ? C33 C32 H32A 109.2 . . ? C31 C32 H32B 109.2 . . ? C33 C32 H32B 109.2 . . ? H32A C32 H32B 107.9 . . ? C34 C33 C32 111.61(16) . . ? C34 C33 H33A 109.3 . . ? C32 C33 H33A 109.3 . . ? C34 C33 H33B 109.3 . . ? C32 C33 H33B 109.3 . . ? H33A C33 H33B 108.0 . . ? C35 C34 C33 111.11(15) . . ? C35 C34 H34A 109.4 . . ? C33 C34 H34A 109.4 . . ? C35 C34 H34B 109.4 . . ? C33 C34 H34B 109.4 . . ? H34A C34 H34B 108.0 . . ? C34 C35 C36 110.67(15) . . ? C34 C35 H35A 109.5 . . ? C36 C35 H35A 109.5 . . ? C34 C35 H35B 109.5 . . ? C36 C35 H35B 109.5 . . ? H35A C35 H35B 108.1 . . ? C31 C36 C35 111.68(14) . . ? C31 C36 H36A 109.3 . . ? C35 C36 H36A 109.3 . . ? C31 C36 H36B 109.3 . . ? C35 C36 H36B 109.3 . . ? H36A C36 H36B 107.9 . . ? C38 C37 C42 120.2(2) . . ? C38 C37 H37 119.9 . . ? C42 C37 H37 119.9 . . ? C39 C38 C37 119.0(2) . . ? C39 C38 H38 120.5 . . ? C37 C38 H38 120.5 . . ? C40 C39 C38 119.6(2) . . ? C40 C39 H39 120.2 . . ? C38 C39 H39 120.2 . . ? C41 C40 C39 120.7(2) . . ? C41 C40 H40 119.6 . . ? C39 C40 H40 119.6 . . ? C42 C41 C40 120.8(3) . . ? C42 C41 H41 119.6 . . ? C40 C41 H41 119.6 . . ? C41 C42 C37 119.6(2) . . ? C41 C42 H42 120.2 . . ? C37 C42 H42 120.2 . . ? _diffrn_measured_fraction_theta_max 0.929 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.220 _refine_diff_density_min -0.188 _refine_diff_density_rms 0.034 _database_code_depnum_ccdc_archive 'CCDC 955174' ####################################################################### # # 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_compound6 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C63 H92 Mg2 N4 O2 S2' _chemical_formula_weight 1050.15 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mg Mg 0.0486 0.0363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.1816(5) _cell_length_b 16.2050(6) _cell_length_c 31.9827(11) _cell_angle_alpha 79.216(3) _cell_angle_beta 83.332(3) _cell_angle_gamma 68.828(3) _cell_volume 6249.3(4) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.116 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2280 _exptl_absorpt_coefficient_mu 0.148 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.949 _exptl_absorpt_correction_T_max 0.978 _exptl_absorpt_process_details 'SCALE3 ABSPACK' _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Gemini Ultra' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 46789 _diffrn_reflns_av_R_equivalents 0.0344 _diffrn_reflns_av_sigmaI/netI 0.0656 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -39 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_theta_min 1.95 _diffrn_reflns_theta_max 26.00 _reflns_number_total 24528 _reflns_number_gt 17596 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. two crystallographically independent molecules were refined in the asymmetric unit. There are no significant geometric differences between them. The carbon atoms of one of the diethyl ether molecules were found to be disordered over two sites. This disorder was successfully modelled and both sets of carbon atoms refined anisotropically. ; _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^)+(0.0404P)^2^+2.9706P] 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 24528 _refine_ls_number_parameters 1398 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.0827 _refine_ls_R_factor_gt 0.0511 _refine_ls_wR_factor_ref 0.1186 _refine_ls_wR_factor_gt 0.1042 _refine_ls_goodness_of_fit_ref 1.014 _refine_ls_restrained_S_all 1.014 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group S1 S 0.72107(5) 0.26487(3) 0.202435(18) 0.02567(13) Uani 1 1 d . . . Mg1 Mg 0.64725(5) 0.54264(4) 0.12584(2) 0.01684(15) Uani 1 1 d . . . O1 O 0.67840(12) 0.42433(9) 0.15827(5) 0.0239(3) Uani 1 1 d . . . N1 N 0.74080(13) 0.56784(11) 0.07392(5) 0.0183(4) Uani 1 1 d . . . C1 C 0.79796(19) 0.53761(16) 0.00028(7) 0.0319(6) Uani 1 1 d . . . H1A H 0.8561 0.5601 0.0033 0.048 Uiso 1 1 calc R . . H1B H 0.7642 0.5662 -0.0269 0.048 Uiso 1 1 calc R . . H1C H 0.8287 0.4726 0.0010 0.048 Uiso 1 1 calc R . . S2 S 0.68430(5) 0.30953(3) 0.109151(18) 0.02511(13) Uani 1 1 d . . . Mg2 Mg 0.72311(5) 0.16251(4) 0.15536(2) 0.01922(16) Uani 1 1 d . . . O2 O 0.65771(13) 0.60080(10) 0.17511(5) 0.0277(4) Uani 1 1 d . . . N2 N 0.50712(13) 0.59819(11) 0.09479(5) 0.0183(4) Uani 1 1 d . . . C2 C 0.71311(17) 0.55921(13) 0.03641(7) 0.0210(5) Uani 1 1 d . . . S3 S 0.66068(5) -0.24088(4) 0.296964(18) 0.02669(13) Uani 1 1 d . . . Mg3 Mg 0.91140(6) -0.51141(5) 0.34132(2) 0.02165(16) Uani 1 1 d . A . O3 O 0.80195(12) -0.40504(9) 0.30956(5) 0.0252(3) Uani 1 1 d . . . N3 N 0.62190(13) 0.08930(11) 0.16815(5) 0.0186(4) Uani 1 1 d . . . C3 C 0.60751(17) 0.56786(13) 0.02814(7) 0.0216(5) Uani 1 1 d . . . H3 H 0.6004 0.5550 0.0011 0.026 Uiso 1 1 calc R . . S4 S 0.76797(5) -0.33244(3) 0.378874(18) 0.02411(13) Uani 1 1 d . . . Mg4 Mg 0.62876(6) -0.18179(4) 0.36547(2) 0.01990(16) Uani 1 1 d . . . O4 O 0.96238(12) -0.57637(10) 0.29018(5) 0.0277(4) Uani 1 1 d D . . N4 N 0.85696(14) 0.05568(11) 0.14294(6) 0.0205(4) Uani 1 1 d . . . C4 C 0.51057(17) 0.59262(13) 0.05360(7) 0.0207(5) Uani 1 1 d . . . N5 N 0.86478(14) -0.58748(11) 0.39266(6) 0.0209(4) Uani 1 1 d . . . C5 C 0.40589(18) 0.61382(15) 0.03183(8) 0.0295(5) Uani 1 1 d . . . H5A H 0.3675 0.5738 0.0463 0.044 Uiso 1 1 calc R . . H5B H 0.4230 0.6052 0.0020 0.044 Uiso 1 1 calc R . . H5C H 0.3595 0.6762 0.0332 0.044 Uiso 1 1 calc R . . N6 N 1.04574(14) -0.51522(11) 0.36805(6) 0.0209(4) Uani 1 1 d . . . C6 C 0.84471(17) 0.57619(14) 0.07699(7) 0.0207(5) Uani 1 1 d . . . N7 N 0.67059(14) -0.08546(11) 0.38428(5) 0.0199(4) Uani 1 1 d . . . C7 C 0.85215(17) 0.66259(14) 0.06947(7) 0.0234(5) Uani 1 1 d . . . N8 N 0.47349(14) -0.13587(11) 0.39183(6) 0.0207(4) Uani 1 1 d . . . C8 C 0.95120(19) 0.67016(15) 0.07493(8) 0.0300(5) Uani 1 1 d . . . H8 H 0.9578 0.7277 0.0696 0.036 Uiso 1 1 calc R . . C9 C 1.04061(19) 0.59568(16) 0.08802(8) 0.0346(6) Uani 1 1 d . . . H9 H 1.1074 0.6024 0.0919 0.041 Uiso 1 1 calc R . . C10 C 1.03220(18) 0.51192(15) 0.09531(8) 0.0304(6) Uani 1 1 d . . . H10 H 1.0939 0.4611 0.1041 0.036 Uiso 1 1 calc R . . C11 C 0.93514(17) 0.50001(14) 0.09004(7) 0.0243(5) Uani 1 1 d . . . C12 C 0.75465(18) 0.74559(14) 0.05483(7) 0.0262(5) Uani 1 1 d . . . H12 H 0.6869 0.7321 0.0653 0.031 Uiso 1 1 calc R . . C13 C 0.7493(2) 0.82855(15) 0.07264(9) 0.0413(7) Uani 1 1 d . . . H13A H 0.7566 0.8134 0.1035 0.062 Uiso 1 1 calc R . . H13B H 0.6792 0.8764 0.0665 0.062 Uiso 1 1 calc R . . H13C H 0.8087 0.8489 0.0593 0.062 Uiso 1 1 calc R . . C14 C 0.7551(2) 0.76690(17) 0.00635(8) 0.0409(7) Uani 1 1 d . . . H14A H 0.8234 0.7760 -0.0049 0.061 Uiso 1 1 calc R . . H14B H 0.6935 0.8215 -0.0022 0.061 Uiso 1 1 calc R . . H14C H 0.7489 0.7169 -0.0050 0.061 Uiso 1 1 calc R . . C15 C 0.93002(18) 0.40599(14) 0.09834(8) 0.0291(6) Uani 1 1 d . . . H15 H 0.8554 0.4108 0.0920 0.035 Uiso 1 1 calc R . . C16 C 0.9480(2) 0.36379(18) 0.14497(9) 0.0470(8) Uani 1 1 d . . . H16A H 1.0216 0.3565 0.1518 0.071 Uiso 1 1 calc R . . H16B H 0.9394 0.3051 0.1498 0.071 Uiso 1 1 calc R . . H16C H 0.8944 0.4027 0.1633 0.071 Uiso 1 1 calc R . . C17 C 1.0119(2) 0.34575(17) 0.06915(10) 0.0493(8) Uani 1 1 d . . . H17A H 0.9986 0.3731 0.0393 0.074 Uiso 1 1 calc R . . H17B H 1.0034 0.2870 0.0741 0.074 Uiso 1 1 calc R . . H17C H 1.0860 0.3385 0.0753 0.074 Uiso 1 1 calc R . . C18 C 0.40314(16) 0.63368(13) 0.11683(7) 0.0204(5) Uani 1 1 d . . . C19 C 0.35765(18) 0.72686(14) 0.11785(8) 0.0278(5) Uani 1 1 d . . . C20 C 0.25936(19) 0.75939(15) 0.14055(9) 0.0356(6) Uani 1 1 d . . . H20 H 0.2272 0.8219 0.1411 0.043 Uiso 1 1 calc R . . C21 C 0.2071(2) 0.70313(16) 0.16229(9) 0.0380(6) Uani 1 1 d . . . H21 H 0.1395 0.7268 0.1776 0.046 Uiso 1 1 calc R . . C22 C 0.25341(18) 0.61204(15) 0.16176(8) 0.0306(6) Uani 1 1 d . . . H22 H 0.2175 0.5735 0.1773 0.037 Uiso 1 1 calc R . . C23 C 0.35080(17) 0.57546(14) 0.13920(7) 0.0219(5) Uani 1 1 d . . . C24 C 0.4143(2) 0.79093(15) 0.09504(10) 0.0414(7) Uani 1 1 d . . . H24 H 0.4874 0.7545 0.0835 0.050 Uiso 1 1 calc R . . C25 C 0.4317(3) 0.8456(2) 0.12559(11) 0.0630(10) Uani 1 1 d . . . H25A H 0.3613 0.8883 0.1340 0.095 Uiso 1 1 calc R . . H25B H 0.4792 0.8782 0.1115 0.095 Uiso 1 1 calc R . . H25C H 0.4657 0.8054 0.1510 0.095 Uiso 1 1 calc R . . C26 C 0.3514(3) 0.8548(2) 0.05798(9) 0.0623(9) Uani 1 1 d . . . H26A H 0.3414 0.8203 0.0377 0.094 Uiso 1 1 calc R . . H26B H 0.3922 0.8931 0.0437 0.094 Uiso 1 1 calc R . . H26C H 0.2800 0.8923 0.0687 0.094 Uiso 1 1 calc R . . C27 C 0.39782(18) 0.47477(14) 0.13902(7) 0.0244(5) Uani 1 1 d . . . H27 H 0.4680 0.4612 0.1214 0.029 Uiso 1 1 calc R . . C28 C 0.42191(19) 0.42220(15) 0.18399(8) 0.0329(6) Uani 1 1 d . . . H28A H 0.4721 0.4417 0.1966 0.049 Uiso 1 1 calc R . . H28B H 0.4552 0.3580 0.1825 0.049 Uiso 1 1 calc R . . H28C H 0.3538 0.4333 0.2017 0.049 Uiso 1 1 calc R . . C29 C 0.3213(2) 0.44288(16) 0.11908(9) 0.0373(6) Uani 1 1 d . . . H29A H 0.2532 0.4527 0.1367 0.056 Uiso 1 1 calc R . . H29B H 0.3561 0.3789 0.1174 0.056 Uiso 1 1 calc R . . H29C H 0.3054 0.4767 0.0904 0.056 Uiso 1 1 calc R . . C30 C 0.69283(16) 0.34342(13) 0.15659(7) 0.0197(5) Uani 1 1 d . . . C31 C 0.6151(2) 0.57667(16) 0.21829(7) 0.0357(6) Uani 1 1 d . . . H31A H 0.6553 0.5888 0.2393 0.043 Uiso 1 1 calc R . . H31B H 0.6269 0.5118 0.2237 0.043 Uiso 1 1 calc R . . C32 C 0.4962(2) 0.62856(19) 0.22400(8) 0.0456(7) Uani 1 1 d . . . H32A H 0.4845 0.6928 0.2190 0.068 Uiso 1 1 calc R . . H32B H 0.4701 0.6114 0.2531 0.068 Uiso 1 1 calc R . . H32C H 0.4561 0.6155 0.2037 0.068 Uiso 1 1 calc R . . C33 C 0.6942(2) 0.67625(15) 0.17099(8) 0.0337(6) Uani 1 1 d . . . H33A H 0.6431 0.7211 0.1878 0.040 Uiso 1 1 calc R . . H33B H 0.6926 0.7048 0.1407 0.040 Uiso 1 1 calc R . . C34 C 0.8071(2) 0.64994(19) 0.18580(9) 0.0447(7) Uani 1 1 d . . . H34A H 0.8076 0.6270 0.2164 0.067 Uiso 1 1 calc R . . H34B H 0.8299 0.7024 0.1804 0.067 Uiso 1 1 calc R . . H34C H 0.8575 0.6033 0.1703 0.067 Uiso 1 1 calc R . . C35 C 0.57985(18) -0.05074(14) 0.18500(8) 0.0282(5) Uani 1 1 d . . . H35A H 0.5805 -0.0714 0.2158 0.042 Uiso 1 1 calc R . . H35B H 0.6026 -0.1025 0.1700 0.042 Uiso 1 1 calc R . . H35C H 0.5061 -0.0114 0.1774 0.042 Uiso 1 1 calc R . . C36 C 0.65779(17) 0.00044(13) 0.17229(7) 0.0211(5) Uani 1 1 d . . . C37 C 0.76672(17) -0.05275(13) 0.16521(7) 0.0227(5) Uani 1 1 d . . . H37 H 0.7813 -0.1155 0.1717 0.027 Uiso 1 1 calc R . . C38 C 0.85765(17) -0.02832(13) 0.15011(7) 0.0226(5) Uani 1 1 d . . . C39 C 0.96078(19) -0.10533(14) 0.14165(9) 0.0337(6) Uani 1 1 d . . . H39A H 0.9948 -0.0896 0.1139 0.051 Uiso 1 1 calc R . . H39B H 0.9428 -0.1589 0.1416 0.051 Uiso 1 1 calc R . . H39C H 1.0114 -0.1173 0.1640 0.051 Uiso 1 1 calc R . . C40 C 0.50555(17) 0.13567(13) 0.16995(7) 0.0217(5) Uani 1 1 d . . . C41 C 0.44751(18) 0.15169(14) 0.20902(8) 0.0265(5) Uani 1 1 d . . . C42 C 0.33500(19) 0.19461(15) 0.20863(9) 0.0349(6) Uani 1 1 d . . . H42 H 0.2943 0.2066 0.2347 0.042 Uiso 1 1 calc R . . C43 C 0.2814(2) 0.22002(16) 0.17122(9) 0.0380(7) Uani 1 1 d . . . H43 H 0.2044 0.2474 0.1718 0.046 Uiso 1 1 calc R . . C44 C 0.33967(19) 0.20573(15) 0.13300(9) 0.0325(6) Uani 1 1 d . . . H44 H 0.3022 0.2243 0.1073 0.039 Uiso 1 1 calc R . . C45 C 0.45263(18) 0.16457(14) 0.13129(7) 0.0254(5) Uani 1 1 d . . . C46 C 0.5025(2) 0.12313(16) 0.25127(8) 0.0320(6) Uani 1 1 d . . . H46 H 0.5817 0.0902 0.2455 0.038 Uiso 1 1 calc R . . C47 C 0.4923(2) 0.20382(17) 0.27149(9) 0.0413(7) Uani 1 1 d . . . H47A H 0.5291 0.2406 0.2527 0.062 Uiso 1 1 calc R . . H47B H 0.5262 0.1833 0.2990 0.062 Uiso 1 1 calc R . . H47C H 0.4152 0.2395 0.2758 0.062 Uiso 1 1 calc R . . C48 C 0.4563(2) 0.05953(19) 0.28250(9) 0.0486(7) Uani 1 1 d . . . H48A H 0.3790 0.0910 0.2894 0.073 Uiso 1 1 calc R . . H48B H 0.4964 0.0395 0.3086 0.073 Uiso 1 1 calc R . . H48C H 0.4639 0.0075 0.2693 0.073 Uiso 1 1 calc R . . C49 C 0.5150(2) 0.14897(16) 0.08877(8) 0.0316(6) Uani 1 1 d . . . H49 H 0.5943 0.1291 0.0939 0.038 Uiso 1 1 calc R . . C50 C 0.4880(2) 0.23435(17) 0.05580(8) 0.0429(7) Uani 1 1 d . . . H50A H 0.4109 0.2552 0.0497 0.064 Uiso 1 1 calc R . . H50B H 0.5330 0.2217 0.0295 0.064 Uiso 1 1 calc R . . H50C H 0.5030 0.2808 0.0671 0.064 Uiso 1 1 calc R . . C51 C 0.4969(3) 0.07400(17) 0.07146(9) 0.0507(8) Uani 1 1 d . . . H51A H 0.5213 0.0184 0.0919 0.076 Uiso 1 1 calc R . . H51B H 0.5386 0.0651 0.0442 0.076 Uiso 1 1 calc R . . H51C H 0.4193 0.0903 0.0672 0.076 Uiso 1 1 calc R . . C52 C 0.95576(17) 0.06976(13) 0.12436(7) 0.0233(5) Uani 1 1 d . . . C53 C 1.04018(18) 0.05941(14) 0.15025(7) 0.0254(5) Uani 1 1 d . . . C54 C 1.13624(18) 0.06896(15) 0.13040(8) 0.0311(6) Uani 1 1 d . . . H54 H 1.1943 0.0620 0.1473 0.037 Uiso 1 1 calc R . . C55 C 1.14832(19) 0.08820(15) 0.08682(8) 0.0331(6) Uani 1 1 d . . . H55 H 1.2156 0.0915 0.0738 0.040 Uiso 1 1 calc R . . C56 C 1.06281(19) 0.10271(15) 0.06185(8) 0.0302(5) Uani 1 1 d . . . H56 H 1.0713 0.1179 0.0318 0.036 Uiso 1 1 calc R . . C57 C 0.96447(18) 0.09542(13) 0.07990(7) 0.0245(5) Uani 1 1 d . . . C58 C 1.02992(19) 0.03948(15) 0.19858(7) 0.0292(5) Uani 1 1 d . . . H58 H 0.9566 0.0344 0.2069 0.035 Uiso 1 1 calc R . . C59 C 1.0365(2) 0.11605(17) 0.21849(8) 0.0395(6) Uani 1 1 d . . . H59A H 1.1068 0.1237 0.2100 0.059 Uiso 1 1 calc R . . H59B H 1.0294 0.1019 0.2496 0.059 Uiso 1 1 calc R . . H59C H 0.9774 0.1716 0.2086 0.059 Uiso 1 1 calc R . . C60 C 1.1160(2) -0.04862(18) 0.21686(9) 0.0485(8) Uani 1 1 d . . . H60A H 1.1116 -0.0977 0.2041 0.073 Uiso 1 1 calc R . . H60B H 1.1029 -0.0604 0.2478 0.073 Uiso 1 1 calc R . . H60C H 1.1886 -0.0443 0.2103 0.073 Uiso 1 1 calc R . . C61 C 0.86892(19) 0.11603(15) 0.05225(7) 0.0296(5) Uani 1 1 d . . . H61 H 0.8013 0.1434 0.0698 0.035 Uiso 1 1 calc R . . C62 C 0.8690(2) 0.18505(18) 0.01238(9) 0.0474(7) Uani 1 1 d . . . H62A H 0.8747 0.2385 0.0206 0.071 Uiso 1 1 calc R . . H62B H 0.8012 0.2017 -0.0021 0.071 Uiso 1 1 calc R . . H62C H 0.9312 0.1592 -0.0069 0.071 Uiso 1 1 calc R . . C63 C 0.8597(2) 0.03211(17) 0.04020(9) 0.0426(7) Uani 1 1 d . . . H63A H 0.9273 0.0000 0.0250 0.064 Uiso 1 1 calc R . . H63B H 0.7986 0.0495 0.0218 0.064 Uiso 1 1 calc R . . H63C H 0.8472 -0.0069 0.0661 0.064 Uiso 1 1 calc R . . C64 C 0.8227(2) -0.60631(19) 0.47024(8) 0.0408(7) Uani 1 1 d . . . H64A H 0.7607 -0.5548 0.4778 0.061 Uiso 1 1 calc R A . H64B H 0.8717 -0.6311 0.4939 0.061 Uiso 1 1 calc R . . H64C H 0.7963 -0.6523 0.4646 0.061 Uiso 1 1 calc R . . C65 C 0.88360(18) -0.57676(14) 0.43084(7) 0.0239(5) Uani 1 1 d . A . C66 C 0.95841(17) -0.53736(14) 0.43769(7) 0.0231(5) Uani 1 1 d . . . H66 H 0.9545 -0.5244 0.4657 0.028 Uiso 1 1 calc R A . C67 C 1.03752(17) -0.51416(13) 0.40999(7) 0.0206(5) Uani 1 1 d . A . C68 C 1.11542(19) -0.48598(17) 0.43020(8) 0.0309(6) Uani 1 1 d . . . H68A H 1.1717 -0.4772 0.4088 0.046 Uiso 1 1 calc R A . H68B H 1.1497 -0.5327 0.4537 0.046 Uiso 1 1 calc R . . H68C H 1.0754 -0.4298 0.4412 0.046 Uiso 1 1 calc R . . C69 C 0.79902(18) -0.63978(14) 0.38831(7) 0.0233(5) Uani 1 1 d . A . C70 C 0.8485(2) -0.73308(15) 0.38894(8) 0.0347(6) Uani 1 1 d . . . C71 C 0.7865(2) -0.77996(16) 0.37896(9) 0.0407(7) Uani 1 1 d . A . H71 H 0.8185 -0.8429 0.3797 0.049 Uiso 1 1 calc R . . C72 C 0.6807(2) -0.73731(16) 0.36814(8) 0.0365(6) Uani 1 1 d . . . H72 H 0.6412 -0.7701 0.3601 0.044 Uiso 1 1 calc R A . C73 C 0.6318(2) -0.64739(15) 0.36894(8) 0.0316(6) Uani 1 1 d . A . H73 H 0.5577 -0.6186 0.3621 0.038 Uiso 1 1 calc R . . C74 C 0.68887(18) -0.59716(14) 0.37967(7) 0.0250(5) Uani 1 1 d . . . C75 C 0.9654(2) -0.78454(18) 0.40102(12) 0.0605(9) Uani 1 1 d . A . H75 H 1.0014 -0.7400 0.4016 0.073 Uiso 1 1 calc R . . C76 C 1.0304(3) -0.8457(2) 0.36831(15) 0.0922(14) Uani 1 1 d . . . H76A H 1.0021 -0.8944 0.3696 0.138 Uiso 1 1 calc R A . H76B H 1.1074 -0.8709 0.3749 0.138 Uiso 1 1 calc R . . H76C H 1.0230 -0.8106 0.3396 0.138 Uiso 1 1 calc R . . C77 C 0.9679(4) -0.8396(4) 0.44625(16) 0.142(2) Uani 1 1 d . . . H77A H 0.9255 -0.7998 0.4665 0.212 Uiso 1 1 calc R A . H77B H 1.0434 -0.8681 0.4547 0.212 Uiso 1 1 calc R . . H77C H 0.9363 -0.8858 0.4462 0.212 Uiso 1 1 calc R . . C78 C 0.62621(19) -0.50006(15) 0.38413(9) 0.0337(6) Uani 1 1 d . A . H78 H 0.6790 -0.4724 0.3896 0.040 Uiso 1 1 calc R . . C79 C 0.5665(2) -0.44574(17) 0.34417(9) 0.0452(7) Uani 1 1 d . . . H79A H 0.6177 -0.4536 0.3192 0.068 Uiso 1 1 calc R A . H79B H 0.5361 -0.3822 0.3472 0.068 Uiso 1 1 calc R . . H79C H 0.5074 -0.4666 0.3405 0.068 Uiso 1 1 calc R . . C80 C 0.5441(2) -0.49568(19) 0.42239(10) 0.0530(8) Uani 1 1 d . . . H80A H 0.4917 -0.5226 0.4176 0.080 Uiso 1 1 calc R A . H80B H 0.5054 -0.4330 0.4259 0.080 Uiso 1 1 calc R . . H80C H 0.5827 -0.5286 0.4482 0.080 Uiso 1 1 calc R . . C81 C 1.14342(17) -0.51098(14) 0.34393(7) 0.0204(5) Uani 1 1 d . A . C82 C 1.24142(18) -0.58533(15) 0.34864(7) 0.0260(5) Uani 1 1 d . . . C83 C 1.33124(19) -0.58204(16) 0.32209(8) 0.0301(6) Uani 1 1 d . A . H83 H 1.3975 -0.6317 0.3249 0.036 Uiso 1 1 calc R . . C84 C 1.32671(19) -0.50857(16) 0.29167(8) 0.0320(6) Uani 1 1 d . . . H84 H 1.3892 -0.5081 0.2737 0.038 Uiso 1 1 calc R A . C85 C 1.23156(19) -0.43588(16) 0.28744(8) 0.0308(6) Uani 1 1 d . A . H85 H 1.2294 -0.3850 0.2667 0.037 Uiso 1 1 calc R . . C86 C 1.13835(18) -0.43548(14) 0.31294(7) 0.0237(5) Uani 1 1 d . . . C87 C 1.2508(2) -0.66888(16) 0.38137(9) 0.0404(7) Uani 1 1 d . A . H87 H 1.1916 -0.6514 0.4040 0.049 Uiso 1 1 calc R . . C88 C 1.2339(4) -0.7408(2) 0.36178(14) 0.0938(14) Uani 1 1 d . . . H88A H 1.2923 -0.7609 0.3401 0.141 Uiso 1 1 calc R A . H88B H 1.1634 -0.7164 0.3486 0.141 Uiso 1 1 calc R . . H88C H 1.2349 -0.7917 0.3840 0.141 Uiso 1 1 calc R . . C89 C 1.3582(3) -0.7065(3) 0.40269(12) 0.0868(14) Uani 1 1 d . . . H89A H 1.3558 -0.7537 0.4265 0.130 Uiso 1 1 calc R A . H89B H 1.3714 -0.6586 0.4134 0.130 Uiso 1 1 calc R . . H89C H 1.4172 -0.7316 0.3820 0.130 Uiso 1 1 calc R . . C90 C 1.03522(18) -0.35286(14) 0.30869(7) 0.0265(5) Uani 1 1 d . A . H90 H 0.9734 -0.3723 0.3221 0.032 Uiso 1 1 calc R . . C91 C 1.0082(3) -0.3112(2) 0.26319(9) 0.0691(11) Uani 1 1 d . . . H91A H 0.9369 -0.2631 0.2628 0.104 Uiso 1 1 calc R A . H91B H 1.0062 -0.3570 0.2475 0.104 Uiso 1 1 calc R . . H91C H 1.0639 -0.2865 0.2497 0.104 Uiso 1 1 calc R . . C92 C 1.0407(3) -0.28361(19) 0.33308(12) 0.0689(11) Uani 1 1 d . . . H92A H 1.0577 -0.3112 0.3626 0.103 Uiso 1 1 calc R A . H92B H 0.9703 -0.2345 0.3327 0.103 Uiso 1 1 calc R . . H92C H 1.0976 -0.2602 0.3198 0.103 Uiso 1 1 calc R . . C93 C 0.74977(17) -0.33488(14) 0.32634(7) 0.0224(5) Uani 1 1 d . . . C94 C 0.8775(3) -0.5784(3) 0.26515(15) 0.0440(13) Uani 0.614(4) 1 d PD A 1 H94A H 0.8929 -0.5582 0.2347 0.053 Uiso 0.614(4) 1 calc PR A 1 H94B H 0.8064 -0.5359 0.2741 0.053 Uiso 0.614(4) 1 calc PR A 1 C95 C 0.8699(9) -0.6708(4) 0.2702(4) 0.078(3) Uani 0.614(4) 1 d PD A 1 H95A H 0.9355 -0.7110 0.2571 0.117 Uiso 0.614(4) 1 calc PR A 1 H95B H 0.8057 -0.6671 0.2562 0.117 Uiso 0.614(4) 1 calc PR A 1 H95C H 0.8635 -0.6942 0.3006 0.117 Uiso 0.614(4) 1 calc PR A 1 C96 C 1.0722(3) -0.6185(3) 0.27312(13) 0.0352(12) Uani 0.614(4) 1 d PD A 1 H96A H 1.0824 -0.6808 0.2703 0.042 Uiso 0.614(4) 1 calc PR A 1 H96B H 1.1245 -0.6211 0.2936 0.042 Uiso 0.614(4) 1 calc PR A 1 C97 C 1.0979(8) -0.5700(10) 0.2301(4) 0.058(4) Uani 0.614(4) 1 d PD A 1 H97A H 1.0519 -0.5730 0.2089 0.087 Uiso 0.614(4) 1 calc PR A 1 H97B H 1.1747 -0.5985 0.2215 0.087 Uiso 0.614(4) 1 calc PR A 1 H97C H 1.0835 -0.5072 0.2322 0.087 Uiso 0.614(4) 1 calc PR A 1 C98 C 0.6337(2) 0.06040(15) 0.40712(9) 0.0348(6) Uani 1 1 d . . . H98A H 0.6882 0.0352 0.4288 0.052 Uiso 1 1 calc R . . H98B H 0.5708 0.1077 0.4176 0.052 Uiso 1 1 calc R . . H98C H 0.6656 0.0856 0.3809 0.052 Uiso 1 1 calc R . . C99 C 0.59747(18) -0.01255(13) 0.39801(7) 0.0237(5) Uani 1 1 d . . . C100 C 0.48586(18) 0.00182(14) 0.40506(7) 0.0252(5) Uani 1 1 d . . . H100 H 0.4418 0.0601 0.4105 0.030 Uiso 1 1 calc R . . C101 C 0.42951(17) -0.05696(14) 0.40524(7) 0.0230(5) Uani 1 1 d . . . C102 C 0.31404(18) -0.02668(15) 0.42436(8) 0.0314(6) Uani 1 1 d . . . H10A H 0.2693 -0.0491 0.4103 0.047 Uiso 1 1 calc R . . H10B H 0.2840 0.0389 0.4203 0.047 Uiso 1 1 calc R . . H10C H 0.3140 -0.0502 0.4549 0.047 Uiso 1 1 calc R . . C103 C 0.78366(17) -0.09502(13) 0.38563(7) 0.0211(5) Uani 1 1 d . . . C104 C 0.84057(18) -0.14599(14) 0.42173(7) 0.0238(5) Uani 1 1 d . . . C105 C 0.94718(19) -0.15055(15) 0.42383(8) 0.0304(6) Uani 1 1 d . . . H105 H 0.9865 -0.1842 0.4482 0.037 Uiso 1 1 calc R . . C106 C 0.99746(19) -0.10744(16) 0.39142(8) 0.0319(6) Uani 1 1 d . . . H106 H 1.0698 -0.1101 0.3938 0.038 Uiso 1 1 calc R . . C107 C 0.94154(18) -0.06030(15) 0.35541(8) 0.0288(5) Uani 1 1 d . . . H107 H 0.9770 -0.0320 0.3328 0.035 Uiso 1 1 calc R . . C108 C 0.83466(18) -0.05335(14) 0.35157(7) 0.0237(5) Uani 1 1 d . . . C109 C 0.78575(19) -0.19193(15) 0.45857(7) 0.0290(5) Uani 1 1 d . . . H109 H 0.7228 -0.1995 0.4470 0.035 Uiso 1 1 calc R . . C110 C 0.8608(2) -0.28514(17) 0.47703(9) 0.0431(7) Uani 1 1 d . . . H11A H 0.8920 -0.3206 0.4540 0.065 Uiso 1 1 calc R . . H11B H 0.8190 -0.3148 0.4977 0.065 Uiso 1 1 calc R . . H11C H 0.9196 -0.2798 0.4913 0.065 Uiso 1 1 calc R . . C111 C 0.7398(3) -0.1338(2) 0.49352(9) 0.0552(8) Uani 1 1 d . . . H11D H 0.7986 -0.1210 0.5040 0.083 Uiso 1 1 calc R . . H11E H 0.7069 -0.1656 0.5170 0.083 Uiso 1 1 calc R . . H11F H 0.6843 -0.0774 0.4820 0.083 Uiso 1 1 calc R . . C112 C 0.77729(19) -0.00529(15) 0.31051(7) 0.0286(5) Uani 1 1 d . . . H112 H 0.6973 0.0090 0.3169 0.034 Uiso 1 1 calc R . . C113 C 0.8126(2) -0.06691(17) 0.27686(8) 0.0389(6) Uani 1 1 d . . . H11G H 0.7746 -0.0357 0.2507 0.058 Uiso 1 1 calc R . . H11H H 0.7944 -0.1209 0.2875 0.058 Uiso 1 1 calc R . . H11I H 0.8914 -0.0838 0.2707 0.058 Uiso 1 1 calc R . . C114 C 0.7961(2) 0.08244(16) 0.29272(9) 0.0404(7) Uani 1 1 d . . . H11J H 0.8732 0.0699 0.2839 0.061 Uiso 1 1 calc R . . H11K H 0.7753 0.1212 0.3147 0.061 Uiso 1 1 calc R . . H11L H 0.7517 0.1127 0.2680 0.061 Uiso 1 1 calc R . . C115 C 0.40793(17) -0.19254(14) 0.39891(7) 0.0233(5) Uani 1 1 d . . . C116 C 0.40284(19) -0.24293(15) 0.43950(8) 0.0306(6) Uani 1 1 d . . . C117 C 0.3369(2) -0.29555(16) 0.44535(9) 0.0397(7) Uani 1 1 d . . . H117 H 0.3308 -0.3291 0.4726 0.048 Uiso 1 1 calc R . . C118 C 0.2809(2) -0.30005(18) 0.41278(10) 0.0467(7) Uani 1 1 d . . . H118 H 0.2368 -0.3365 0.4176 0.056 Uiso 1 1 calc R . . C119 C 0.2886(2) -0.25175(17) 0.37311(10) 0.0426(7) Uani 1 1 d . . . H119 H 0.2504 -0.2559 0.3506 0.051 Uiso 1 1 calc R . . C120 C 0.35172(18) -0.19653(15) 0.36522(8) 0.0289(5) Uani 1 1 d . . . C121 C 0.4662(2) -0.24232(17) 0.47595(8) 0.0376(6) Uani 1 1 d . . . H121 H 0.4919 -0.1902 0.4681 0.045 Uiso 1 1 calc R . . C122 C 0.5672(2) -0.32770(19) 0.48270(9) 0.0465(7) Uani 1 1 d . . . H12A H 0.5443 -0.3798 0.4917 0.070 Uiso 1 1 calc R . . H12B H 0.6101 -0.3233 0.5047 0.070 Uiso 1 1 calc R . . H12C H 0.6117 -0.3345 0.4559 0.070 Uiso 1 1 calc R . . C123 C 0.3964(3) -0.2308(2) 0.51779(9) 0.0551(8) Uani 1 1 d . . . H12D H 0.3298 -0.1784 0.5128 0.083 Uiso 1 1 calc R . . H12E H 0.4377 -0.2221 0.5392 0.083 Uiso 1 1 calc R . . H12F H 0.3773 -0.2844 0.5281 0.083 Uiso 1 1 calc R . . C124 C 0.35313(19) -0.13964(16) 0.32184(8) 0.0337(6) Uani 1 1 d . . . H124 H 0.4184 -0.1211 0.3197 0.040 Uiso 1 1 calc R . . C125 C 0.3643(2) -0.18972(19) 0.28497(9) 0.0523(8) Uani 1 1 d . . . H12G H 0.4286 -0.2445 0.2882 0.078 Uiso 1 1 calc R . . H12H H 0.3723 -0.1516 0.2581 0.078 Uiso 1 1 calc R . . H12I H 0.2991 -0.2054 0.2849 0.078 Uiso 1 1 calc R . . C126 C 0.2527(2) -0.05385(18) 0.31756(9) 0.0459(7) Uani 1 1 d . . . H12J H 0.1866 -0.0695 0.3223 0.069 Uiso 1 1 calc R . . H12K H 0.2542 -0.0198 0.2889 0.069 Uiso 1 1 calc R . . H12L H 0.2530 -0.0174 0.3387 0.069 Uiso 1 1 calc R . . C96A C 0.9966(6) -0.5340(4) 0.25037(18) 0.041(2) Uani 0.386(4) 1 d PD A 2 H96C H 0.9838 -0.4707 0.2523 0.049 Uiso 0.386(4) 1 calc PR A 2 H96D H 0.9522 -0.5345 0.2276 0.049 Uiso 0.386(4) 1 calc PR A 2 C94A C 0.9418(7) -0.6575(4) 0.2875(3) 0.057(3) Uani 0.386(4) 1 d PD A 2 H94C H 0.9476 -0.6958 0.3158 0.068 Uiso 0.386(4) 1 calc PR A 2 H94D H 0.9951 -0.6919 0.2671 0.068 Uiso 0.386(4) 1 calc PR A 2 C95A C 0.8261(10) -0.6268(10) 0.2724(6) 0.097(6) Uani 0.386(4) 1 d PD A 2 H95D H 0.7749 -0.5901 0.2921 0.146 Uiso 0.386(4) 1 calc PR A 2 H95E H 0.8066 -0.6793 0.2714 0.146 Uiso 0.386(4) 1 calc PR A 2 H95F H 0.8227 -0.5913 0.2438 0.146 Uiso 0.386(4) 1 calc PR A 2 C97A C 1.1166(10) -0.5807(15) 0.2387(6) 0.050(4) Uani 0.386(4) 1 d PD A 2 H97D H 1.1611 -0.5759 0.2600 0.075 Uiso 0.386(4) 1 calc PR A 2 H97E H 1.1356 -0.5523 0.2106 0.075 Uiso 0.386(4) 1 calc PR A 2 H97F H 1.1302 -0.6441 0.2381 0.075 Uiso 0.386(4) 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 S1 0.0369(3) 0.0169(3) 0.0229(3) -0.0007(2) -0.0067(2) -0.0087(2) Mg1 0.0161(4) 0.0155(3) 0.0183(4) -0.0025(3) -0.0013(3) -0.0046(3) O1 0.0245(8) 0.0149(7) 0.0308(9) -0.0021(7) -0.0015(7) -0.0057(6) N1 0.0183(9) 0.0173(9) 0.0195(10) -0.0021(7) -0.0008(7) -0.0069(7) C1 0.0313(14) 0.0425(14) 0.0260(13) -0.0127(11) 0.0080(10) -0.0169(11) S2 0.0324(3) 0.0190(3) 0.0221(3) -0.0014(2) -0.0027(2) -0.0073(2) Mg2 0.0162(4) 0.0143(3) 0.0262(4) -0.0036(3) -0.0009(3) -0.0040(3) O2 0.0435(10) 0.0234(8) 0.0202(8) -0.0039(7) -0.0017(7) -0.0159(7) N2 0.0167(9) 0.0159(8) 0.0213(10) -0.0029(7) -0.0007(7) -0.0046(7) C2 0.0260(12) 0.0177(10) 0.0197(12) -0.0034(9) 0.0002(9) -0.0082(9) S3 0.0290(3) 0.0243(3) 0.0231(3) -0.0049(2) -0.0034(2) -0.0038(2) Mg3 0.0218(4) 0.0249(4) 0.0193(4) -0.0051(3) -0.0013(3) -0.0085(3) O3 0.0208(8) 0.0201(8) 0.0349(9) -0.0114(7) 0.0038(7) -0.0056(6) N3 0.0168(9) 0.0161(9) 0.0220(10) -0.0016(8) -0.0022(7) -0.0048(7) C3 0.0270(13) 0.0235(11) 0.0175(11) -0.0064(9) -0.0010(9) -0.0109(9) S4 0.0250(3) 0.0198(3) 0.0253(3) -0.0047(2) -0.0033(2) -0.0039(2) Mg4 0.0188(4) 0.0185(3) 0.0227(4) -0.0049(3) 0.0002(3) -0.0063(3) O4 0.0254(9) 0.0321(9) 0.0268(9) -0.0124(7) -0.0015(7) -0.0075(7) N4 0.0168(9) 0.0183(9) 0.0249(10) -0.0038(8) -0.0015(8) -0.0041(7) C4 0.0239(12) 0.0143(10) 0.0252(12) -0.0015(9) -0.0061(9) -0.0077(9) N5 0.0209(10) 0.0224(9) 0.0209(10) -0.0046(8) -0.0021(8) -0.0085(7) C5 0.0270(13) 0.0313(12) 0.0311(14) -0.0070(11) -0.0090(10) -0.0079(10) N6 0.0192(10) 0.0231(9) 0.0205(10) -0.0059(8) 0.0023(8) -0.0073(7) C6 0.0193(12) 0.0255(11) 0.0173(11) -0.0035(9) 0.0023(9) -0.0088(9) N7 0.0217(10) 0.0170(9) 0.0206(10) -0.0028(8) -0.0011(8) -0.0064(7) C7 0.0227(12) 0.0251(11) 0.0228(12) -0.0043(10) 0.0018(9) -0.0096(9) N8 0.0191(10) 0.0217(9) 0.0215(10) -0.0044(8) -0.0001(8) -0.0070(7) C8 0.0308(14) 0.0283(12) 0.0370(14) -0.0079(11) 0.0007(11) -0.0169(10) C9 0.0210(13) 0.0421(15) 0.0451(16) -0.0087(13) -0.0016(11) -0.0154(11) C10 0.0170(12) 0.0310(13) 0.0399(15) -0.0046(11) -0.0020(10) -0.0047(10) C11 0.0193(12) 0.0272(12) 0.0263(13) -0.0068(10) 0.0024(9) -0.0078(9) C12 0.0261(13) 0.0206(11) 0.0328(14) -0.0010(10) -0.0010(10) -0.0109(9) C13 0.0457(17) 0.0243(13) 0.0527(18) -0.0058(12) -0.0044(13) -0.0103(11) C14 0.0459(17) 0.0356(14) 0.0359(15) 0.0021(12) -0.0065(12) -0.0103(12) C15 0.0176(12) 0.0222(11) 0.0425(15) -0.0029(11) 0.0019(10) -0.0033(9) C16 0.0289(15) 0.0446(16) 0.0593(19) 0.0178(15) -0.0122(13) -0.0128(12) C17 0.0356(16) 0.0289(14) 0.081(2) -0.0161(15) 0.0152(15) -0.0095(12) C18 0.0146(11) 0.0216(11) 0.0233(12) -0.0040(9) -0.0037(9) -0.0033(8) C19 0.0207(12) 0.0201(11) 0.0398(15) -0.0048(11) -0.0027(10) -0.0032(9) C20 0.0265(14) 0.0190(11) 0.0534(17) -0.0084(12) 0.0040(12) 0.0012(10) C21 0.0238(14) 0.0308(13) 0.0470(16) -0.0057(12) 0.0119(12) 0.0008(10) C22 0.0224(13) 0.0267(12) 0.0378(15) -0.0005(11) 0.0052(11) -0.0071(10) C23 0.0175(11) 0.0210(11) 0.0241(12) -0.0023(9) -0.0025(9) -0.0032(9) C24 0.0278(14) 0.0204(12) 0.074(2) -0.0122(13) 0.0122(13) -0.0074(10) C25 0.081(2) 0.0459(17) 0.074(2) 0.0213(17) -0.0425(19) -0.0399(17) C26 0.111(3) 0.060(2) 0.0369(17) -0.0002(15) -0.0029(18) -0.059(2) C27 0.0194(12) 0.0211(11) 0.0302(13) -0.0031(10) 0.0025(10) -0.0057(9) C28 0.0247(13) 0.0293(13) 0.0381(15) 0.0028(11) 0.0012(11) -0.0065(10) C29 0.0369(15) 0.0283(13) 0.0501(17) -0.0057(12) -0.0064(12) -0.0146(11) C30 0.0141(11) 0.0169(10) 0.0271(12) -0.0037(9) -0.0003(9) -0.0044(8) C31 0.0565(18) 0.0322(13) 0.0210(13) -0.0047(11) 0.0018(12) -0.0197(12) C32 0.0570(19) 0.0546(17) 0.0282(15) -0.0111(13) 0.0044(13) -0.0228(15) C33 0.0538(17) 0.0248(12) 0.0297(14) -0.0038(11) -0.0067(12) -0.0210(11) C34 0.0549(19) 0.0520(17) 0.0393(16) -0.0059(14) -0.0101(14) -0.0311(14) C35 0.0285(13) 0.0203(11) 0.0370(14) -0.0002(10) -0.0033(11) -0.0118(10) C36 0.0253(12) 0.0200(11) 0.0190(11) 0.0003(9) -0.0046(9) -0.0096(9) C37 0.0269(13) 0.0130(10) 0.0272(13) -0.0016(9) -0.0065(10) -0.0050(9) C38 0.0230(12) 0.0182(11) 0.0247(12) -0.0060(9) -0.0074(9) -0.0019(9) C39 0.0278(14) 0.0200(11) 0.0493(16) -0.0090(11) -0.0034(12) -0.0014(10) C40 0.0196(12) 0.0147(10) 0.0320(13) -0.0009(9) -0.0040(10) -0.0080(8) C41 0.0239(13) 0.0212(11) 0.0325(14) -0.0014(10) 0.0028(10) -0.0083(9) C42 0.0264(14) 0.0293(13) 0.0441(16) -0.0036(12) 0.0076(12) -0.0078(10) C43 0.0190(13) 0.0289(13) 0.0606(19) -0.0015(13) -0.0016(12) -0.0049(10) C44 0.0265(14) 0.0253(12) 0.0448(16) 0.0036(11) -0.0151(12) -0.0085(10) C45 0.0240(12) 0.0192(11) 0.0337(14) -0.0002(10) -0.0060(10) -0.0090(9) C46 0.0309(14) 0.0334(13) 0.0275(13) -0.0033(11) 0.0052(11) -0.0089(11) C47 0.0423(16) 0.0445(15) 0.0384(16) -0.0109(13) 0.0036(12) -0.0163(13) C48 0.065(2) 0.0493(17) 0.0327(16) 0.0013(13) 0.0007(14) -0.0261(15) C49 0.0291(14) 0.0363(13) 0.0284(14) -0.0021(11) -0.0090(11) -0.0094(11) C50 0.0590(19) 0.0435(15) 0.0321(15) 0.0006(13) -0.0088(13) -0.0259(14) C51 0.075(2) 0.0354(15) 0.0418(17) -0.0052(13) -0.0106(15) -0.0168(14) C52 0.0190(12) 0.0154(10) 0.0318(13) -0.0055(10) 0.0015(10) -0.0017(8) C53 0.0206(12) 0.0208(11) 0.0308(13) -0.0026(10) -0.0029(10) -0.0028(9) C54 0.0186(12) 0.0331(13) 0.0392(15) -0.0031(11) -0.0034(11) -0.0070(10) C55 0.0240(13) 0.0301(13) 0.0430(16) -0.0058(12) 0.0084(11) -0.0096(10) C56 0.0329(14) 0.0261(12) 0.0293(14) -0.0056(11) 0.0047(11) -0.0087(10) C57 0.0261(13) 0.0165(10) 0.0289(13) -0.0068(10) 0.0016(10) -0.0042(9) C58 0.0225(13) 0.0345(13) 0.0306(14) -0.0032(11) -0.0045(10) -0.0100(10) C59 0.0402(16) 0.0416(15) 0.0357(15) -0.0056(12) -0.0025(12) -0.0131(12) C60 0.0558(19) 0.0421(16) 0.0389(17) 0.0026(13) -0.0151(14) -0.0075(14) C61 0.0294(14) 0.0303(12) 0.0264(13) -0.0082(11) -0.0023(10) -0.0053(10) C62 0.0571(19) 0.0416(15) 0.0405(17) 0.0033(13) -0.0167(14) -0.0141(14) C63 0.0534(18) 0.0426(15) 0.0374(16) -0.0117(13) -0.0061(13) -0.0195(13) C64 0.0443(16) 0.0634(18) 0.0285(14) -0.0066(13) 0.0032(12) -0.0368(14) C65 0.0225(12) 0.0272(12) 0.0219(12) -0.0043(10) 0.0006(9) -0.0087(9) C66 0.0233(12) 0.0316(12) 0.0169(11) -0.0088(10) -0.0005(9) -0.0101(10) C67 0.0188(11) 0.0215(11) 0.0220(12) -0.0077(9) -0.0020(9) -0.0051(9) C68 0.0287(14) 0.0452(14) 0.0261(13) -0.0083(11) -0.0011(10) -0.0202(11) C69 0.0280(13) 0.0229(11) 0.0208(12) -0.0026(10) -0.0027(10) -0.0109(9) C70 0.0310(14) 0.0266(12) 0.0466(16) -0.0079(12) -0.0117(12) -0.0062(10) C71 0.0457(17) 0.0211(12) 0.0582(19) -0.0090(12) -0.0120(14) -0.0109(11) C72 0.0405(16) 0.0325(13) 0.0457(16) -0.0072(12) -0.0093(12) -0.0212(12) C73 0.0295(14) 0.0310(13) 0.0387(15) -0.0045(11) -0.0069(11) -0.0149(10) C74 0.0280(13) 0.0245(11) 0.0257(13) -0.0017(10) -0.0031(10) -0.0136(10) C75 0.0409(18) 0.0337(15) 0.108(3) -0.0265(17) -0.0215(18) -0.0017(13) C76 0.043(2) 0.060(2) 0.169(4) -0.057(3) -0.030(2) 0.0149(16) C77 0.096(4) 0.164(5) 0.114(4) 0.013(4) -0.073(3) 0.018(3) C78 0.0259(13) 0.0258(12) 0.0530(17) -0.0070(12) -0.0088(12) -0.0107(10) C79 0.0350(16) 0.0327(14) 0.068(2) 0.0069(14) -0.0179(14) -0.0142(12) C80 0.0483(19) 0.0507(17) 0.059(2) -0.0238(15) -0.0014(15) -0.0083(14) C81 0.0199(12) 0.0271(11) 0.0178(11) -0.0083(9) 0.0010(9) -0.0107(9) C82 0.0232(13) 0.0282(12) 0.0261(13) -0.0061(10) 0.0019(10) -0.0082(10) C83 0.0228(13) 0.0338(13) 0.0316(14) -0.0092(11) 0.0014(10) -0.0061(10) C84 0.0260(13) 0.0438(15) 0.0288(14) -0.0071(12) 0.0072(10) -0.0171(11) C85 0.0296(14) 0.0365(13) 0.0279(13) -0.0015(11) 0.0022(10) -0.0163(11) C86 0.0234(12) 0.0277(12) 0.0238(12) -0.0071(10) -0.0015(9) -0.0118(9) C87 0.0301(14) 0.0315(14) 0.0438(16) 0.0028(12) 0.0127(12) -0.0006(11) C88 0.121(4) 0.042(2) 0.119(4) -0.002(2) 0.015(3) -0.042(2) C89 0.063(2) 0.093(3) 0.078(3) 0.050(2) -0.021(2) -0.022(2) C90 0.0266(13) 0.0251(12) 0.0298(13) -0.0028(10) -0.0018(10) -0.0122(10) C91 0.066(2) 0.072(2) 0.0364(18) -0.0041(16) -0.0171(16) 0.0182(17) C92 0.059(2) 0.0447(17) 0.098(3) -0.0360(18) -0.040(2) 0.0120(15) C93 0.0189(12) 0.0243(11) 0.0268(13) -0.0066(10) 0.0036(9) -0.0111(9) C94 0.030(3) 0.060(3) 0.047(3) -0.026(2) -0.014(2) -0.008(2) C95 0.114(7) 0.067(5) 0.085(6) -0.015(5) -0.045(6) -0.056(5) C96 0.023(2) 0.042(2) 0.042(3) -0.019(2) -0.0003(19) -0.0072(18) C97 0.053(5) 0.075(6) 0.055(7) -0.019(5) 0.027(4) -0.036(4) C98 0.0336(14) 0.0217(12) 0.0512(17) -0.0139(12) 0.0024(12) -0.0097(10) C99 0.0274(13) 0.0174(11) 0.0247(12) -0.0006(9) -0.0032(10) -0.0067(9) C100 0.0270(13) 0.0174(11) 0.0284(13) -0.0057(10) -0.0016(10) -0.0033(9) C101 0.0209(12) 0.0232(11) 0.0212(12) -0.0030(10) -0.0018(9) -0.0033(9) C102 0.0221(13) 0.0286(12) 0.0412(15) -0.0117(11) 0.0038(11) -0.0048(10) C103 0.0213(12) 0.0161(10) 0.0270(12) -0.0064(9) -0.0007(9) -0.0067(9) C104 0.0263(13) 0.0215(11) 0.0241(12) -0.0057(10) -0.0045(10) -0.0067(9) C105 0.0306(14) 0.0311(13) 0.0296(14) -0.0058(11) -0.0097(11) -0.0077(10) C106 0.0236(13) 0.0357(13) 0.0415(15) -0.0125(12) -0.0030(11) -0.0127(10) C107 0.0249(13) 0.0284(12) 0.0352(14) -0.0054(11) 0.0035(10) -0.0130(10) C108 0.0251(13) 0.0194(11) 0.0267(13) -0.0042(10) 0.0002(10) -0.0081(9) C109 0.0336(14) 0.0318(13) 0.0221(13) -0.0005(10) -0.0055(10) -0.0124(11) C110 0.0455(17) 0.0391(15) 0.0395(16) 0.0066(13) -0.0085(13) -0.0129(13) C111 0.076(2) 0.0531(18) 0.0342(16) -0.0091(14) 0.0160(15) -0.0244(16) C112 0.0280(13) 0.0278(12) 0.0283(13) 0.0017(10) -0.0015(10) -0.0109(10) C113 0.0493(17) 0.0387(14) 0.0296(14) 0.0005(12) -0.0094(12) -0.0169(12) C114 0.0491(17) 0.0284(13) 0.0393(16) 0.0048(12) -0.0002(13) -0.0140(12) C115 0.0158(11) 0.0241(11) 0.0298(13) -0.0102(10) 0.0055(9) -0.0056(9) C116 0.0283(13) 0.0283(12) 0.0348(14) -0.0089(11) 0.0071(11) -0.0102(10) C117 0.0345(15) 0.0342(14) 0.0497(17) -0.0058(13) 0.0149(13) -0.0166(12) C118 0.0303(15) 0.0410(15) 0.077(2) -0.0137(16) 0.0027(14) -0.0216(12) C119 0.0250(14) 0.0448(16) 0.064(2) -0.0188(15) -0.0072(13) -0.0132(12) C120 0.0166(12) 0.0311(12) 0.0391(15) -0.0123(11) -0.0009(10) -0.0050(9) C121 0.0537(17) 0.0369(14) 0.0269(14) -0.0037(12) 0.0027(12) -0.0236(13) C122 0.0452(17) 0.0613(18) 0.0342(16) -0.0072(14) -0.0030(13) -0.0199(14) C123 0.074(2) 0.0496(17) 0.0346(17) -0.0126(14) 0.0108(15) -0.0147(16) C124 0.0240(13) 0.0439(14) 0.0326(14) -0.0116(12) -0.0065(11) -0.0067(11) C125 0.0503(19) 0.0539(17) 0.0439(18) -0.0197(14) -0.0135(14) 0.0015(14) C126 0.0438(17) 0.0431(15) 0.0436(17) -0.0093(13) -0.0078(13) -0.0039(13) C96A 0.058(5) 0.036(4) 0.032(4) -0.006(3) 0.001(3) -0.021(3) C94A 0.081(7) 0.053(5) 0.054(5) -0.035(4) 0.033(5) -0.043(5) C95A 0.151(17) 0.150(16) 0.057(8) -0.016(12) -0.012(10) -0.130(15) C97A 0.062(9) 0.063(9) 0.037(7) -0.029(6) 0.013(6) -0.029(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 S1 C30 1.731(2) . ? S1 Mg2 2.4313(9) . ? Mg1 O1 1.9253(14) . ? Mg1 N1 2.0197(18) . ? Mg1 O2 2.0225(17) . ? Mg1 N2 2.0245(17) . ? O1 C30 1.266(2) . ? N1 C2 1.339(3) . ? N1 C6 1.440(3) . ? C1 C2 1.509(3) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? S2 C30 1.736(2) . ? S2 Mg2 2.4697(8) . ? Mg2 N4 2.0387(18) . ? Mg2 N3 2.0468(18) . ? Mg2 C30 2.819(2) . ? O2 C33 1.447(3) . ? O2 C31 1.467(3) . ? N2 C4 1.332(3) . ? N2 C18 1.437(3) . ? C2 C3 1.399(3) . ? S3 C93 1.735(2) . ? S3 Mg4 2.4849(9) . ? Mg3 O3 1.9933(16) . ? Mg3 O4 2.0282(17) . ? Mg3 N6 2.0306(19) . ? Mg3 N5 2.0369(18) . ? O3 C93 1.277(3) . ? N3 C36 1.329(3) . ? N3 C40 1.443(3) . ? C3 C4 1.403(3) . ? C3 H3 0.9500 . ? S4 C93 1.734(2) . ? S4 Mg4 2.4629(8) . ? Mg4 N7 2.0379(19) . ? Mg4 N8 2.0462(19) . ? Mg4 C93 2.847(2) . ? O4 C96A 1.435(5) . ? O4 C96 1.449(4) . ? O4 C94A 1.453(5) . ? O4 C94 1.462(4) . ? N4 C38 1.334(3) . ? N4 C52 1.444(3) . ? C4 C5 1.516(3) . ? N5 C65 1.328(3) . ? N5 C69 1.446(3) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? N6 C67 1.336(3) . ? N6 C81 1.439(3) . ? C6 C11 1.407(3) . ? C6 C7 1.413(3) . ? N7 C99 1.338(3) . ? N7 C103 1.447(3) . ? C7 C8 1.388(3) . ? C7 C12 1.528(3) . ? N8 C101 1.329(3) . ? N8 C115 1.446(3) . ? C8 C9 1.385(3) . ? C8 H8 0.9500 . ? C9 C10 1.376(3) . ? C9 H9 0.9500 . ? C10 C11 1.394(3) . ? C10 H10 0.9500 . ? C11 C15 1.522(3) . ? C12 C14 1.524(3) . ? C12 C13 1.531(3) . ? C12 H12 1.0000 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C16 1.527(3) . ? C15 C17 1.528(4) . ? C15 H15 1.0000 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C23 1.407(3) . ? C18 C19 1.414(3) . ? C19 C20 1.384(3) . ? C19 C24 1.523(3) . ? C20 C21 1.376(3) . ? C20 H20 0.9500 . ? C21 C22 1.381(3) . ? C21 H21 0.9500 . ? C22 C23 1.384(3) . ? C22 H22 0.9500 . ? C23 C27 1.523(3) . ? C24 C25 1.521(4) . ? C24 C26 1.521(4) . ? C24 H24 1.0000 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C29 1.530(3) . ? C27 C28 1.532(3) . ? C27 H27 1.0000 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C31 C32 1.495(4) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 C34 1.500(4) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 C36 1.517(3) . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 C37 1.400(3) . ? C37 C38 1.401(3) . ? C37 H37 0.9500 . ? C38 C39 1.515(3) . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 C41 1.403(3) . ? C40 C45 1.408(3) . ? C41 C42 1.393(3) . ? C41 C46 1.522(3) . ? C42 C43 1.379(4) . ? C42 H42 0.9500 . ? C43 C44 1.377(4) . ? C43 H43 0.9500 . ? C44 C45 1.394(3) . ? C44 H44 0.9500 . ? C45 C49 1.519(3) . ? C46 C47 1.522(4) . ? C46 C48 1.535(3) . ? C46 H46 1.0000 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C49 C51 1.527(4) . ? C49 C50 1.529(3) . ? C49 H49 1.0000 . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C52 C53 1.407(3) . ? C52 C57 1.408(3) . ? C53 C54 1.396(3) . ? C53 C58 1.519(3) . ? C54 C55 1.374(3) . ? C54 H54 0.9500 . ? C55 C56 1.382(3) . ? C55 H55 0.9500 . ? C56 C57 1.392(3) . ? C56 H56 0.9500 . ? C57 C61 1.525(3) . ? C58 C59 1.529(3) . ? C58 C60 1.529(3) . ? C58 H58 1.0000 . ? C59 H59A 0.9800 . ? C59 H59B 0.9800 . ? C59 H59C 0.9800 . ? C60 H60A 0.9800 . ? C60 H60B 0.9800 . ? C60 H60C 0.9800 . ? C61 C63 1.529(3) . ? C61 C62 1.531(3) . ? C61 H61 1.0000 . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C62 H62C 0.9800 . ? C63 H63A 0.9800 . ? C63 H63B 0.9800 . ? C63 H63C 0.9800 . ? C64 C65 1.509(3) . ? C64 H64A 0.9800 . ? C64 H64B 0.9800 . ? C64 H64C 0.9800 . ? C65 C66 1.409(3) . ? C66 C67 1.399(3) . ? C66 H66 0.9500 . ? C67 C68 1.511(3) . ? C68 H68A 0.9800 . ? C68 H68B 0.9800 . ? C68 H68C 0.9800 . ? C69 C74 1.400(3) . ? C69 C70 1.411(3) . ? C70 C71 1.396(3) . ? C70 C75 1.519(4) . ? C71 C72 1.366(3) . ? C71 H71 0.9500 . ? C72 C73 1.368(3) . ? C72 H72 0.9500 . ? C73 C74 1.397(3) . ? C73 H73 0.9500 . ? C74 C78 1.515(3) . ? C75 C76 1.542(5) . ? C75 C77 1.548(5) . ? C75 H75 1.0000 . ? C76 H76A 0.9800 . ? C76 H76B 0.9800 . ? C76 H76C 0.9800 . ? C77 H77A 0.9800 . ? C77 H77B 0.9800 . ? C77 H77C 0.9800 . ? C78 C79 1.530(3) . ? C78 C80 1.530(4) . ? C78 H78 1.0000 . ? C79 H79A 0.9800 . ? C79 H79B 0.9800 . ? C79 H79C 0.9800 . ? C80 H80A 0.9800 . ? C80 H80B 0.9800 . ? C80 H80C 0.9800 . ? C81 C86 1.409(3) . ? C81 C82 1.413(3) . ? C82 C83 1.386(3) . ? C82 C87 1.524(3) . ? C83 C84 1.377(3) . ? C83 H83 0.9500 . ? C84 C85 1.375(3) . ? C84 H84 0.9500 . ? C85 C86 1.392(3) . ? C85 H85 0.9500 . ? C86 C90 1.523(3) . ? C87 C89 1.513(4) . ? C87 C88 1.515(5) . ? C87 H87 1.0000 . ? C88 H88A 0.9800 . ? C88 H88B 0.9800 . ? C88 H88C 0.9800 . ? C89 H89A 0.9800 . ? C89 H89B 0.9800 . ? C89 H89C 0.9800 . ? C90 C92 1.507(4) . ? C90 C91 1.510(3) . ? C90 H90 1.0000 . ? C91 H91A 0.9800 . ? C91 H91B 0.9800 . ? C91 H91C 0.9800 . ? C92 H92A 0.9800 . ? C92 H92B 0.9800 . ? C92 H92C 0.9800 . ? C94 C95 1.515(6) . ? C94 H94A 0.9900 . ? C94 H94B 0.9900 . ? C95 H95A 0.9800 . ? C95 H95B 0.9800 . ? C95 H95C 0.9800 . ? C96 C97 1.518(7) . ? C96 H96A 0.9900 . ? C96 H96B 0.9900 . ? C97 H97A 0.9800 . ? C97 H97B 0.9800 . ? C97 H97C 0.9800 . ? C98 C99 1.510(3) . ? C98 H98A 0.9800 . ? C98 H98B 0.9800 . ? C98 H98C 0.9800 . ? C99 C100 1.402(3) . ? C100 C101 1.403(3) . ? C100 H100 0.9500 . ? C101 C102 1.513(3) . ? C102 H10A 0.9800 . ? C102 H10B 0.9800 . ? C102 H10C 0.9800 . ? C103 C104 1.405(3) . ? C103 C108 1.406(3) . ? C104 C105 1.389(3) . ? C104 C109 1.526(3) . ? C105 C106 1.380(3) . ? C105 H105 0.9500 . ? C106 C107 1.384(3) . ? C106 H106 0.9500 . ? C107 C108 1.390(3) . ? C107 H107 0.9500 . ? C108 C112 1.525(3) . ? C109 C111 1.526(4) . ? C109 C110 1.527(3) . ? C109 H109 1.0000 . ? C110 H11A 0.9800 . ? C110 H11B 0.9800 . ? C110 H11C 0.9800 . ? C111 H11D 0.9800 . ? C111 H11E 0.9800 . ? C111 H11F 0.9800 . ? C112 C113 1.524(4) . ? C112 C114 1.525(3) . ? C112 H112 1.0000 . ? C113 H11G 0.9800 . ? C113 H11H 0.9800 . ? C113 H11I 0.9800 . ? C114 H11J 0.9800 . ? C114 H11K 0.9800 . ? C114 H11L 0.9800 . ? C115 C120 1.400(3) . ? C115 C116 1.407(3) . ? C116 C117 1.398(3) . ? C116 C121 1.514(3) . ? C117 C118 1.372(4) . ? C117 H117 0.9500 . ? C118 C119 1.374(4) . ? C118 H118 0.9500 . ? C119 C120 1.400(3) . ? C119 H119 0.9500 . ? C120 C124 1.518(3) . ? C121 C123 1.535(4) . ? C121 C122 1.536(4) . ? C121 H121 1.0000 . ? C122 H12A 0.9800 . ? C122 H12B 0.9800 . ? C122 H12C 0.9800 . ? C123 H12D 0.9800 . ? C123 H12E 0.9800 . ? C123 H12F 0.9800 . ? C124 C125 1.517(4) . ? C124 C126 1.531(3) . ? C124 H124 1.0000 . ? C125 H12G 0.9800 . ? C125 H12H 0.9800 . ? C125 H12I 0.9800 . ? C126 H12J 0.9800 . ? C126 H12K 0.9800 . ? C126 H12L 0.9800 . ? C96A C97A 1.522(7) . ? C96A H96C 0.9900 . ? C96A H96D 0.9900 . ? C94A C95A 1.531(7) . ? C94A H94C 0.9900 . ? C94A H94D 0.9900 . ? C95A H95D 0.9800 . ? C95A H95E 0.9800 . ? C95A H95F 0.9800 . ? C97A H97D 0.9800 . ? C97A H97E 0.9800 . ? C97A H97F 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C30 S1 Mg2 83.47(8) . . ? O1 Mg1 N1 121.78(7) . . ? O1 Mg1 O2 95.33(7) . . ? N1 Mg1 O2 112.98(7) . . ? O1 Mg1 N2 118.18(7) . . ? N1 Mg1 N2 93.85(7) . . ? O2 Mg1 N2 116.37(7) . . ? C30 O1 Mg1 144.96(15) . . ? C2 N1 C6 119.57(18) . . ? C2 N1 Mg1 116.78(14) . . ? C6 N1 Mg1 122.41(13) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C30 S2 Mg2 82.21(7) . . ? N4 Mg2 N3 93.89(7) . . ? N4 Mg2 S1 123.62(6) . . ? N3 Mg2 S1 120.77(6) . . ? N4 Mg2 S2 120.82(6) . . ? N3 Mg2 S2 125.87(5) . . ? S1 Mg2 S2 75.16(3) . . ? N4 Mg2 C30 132.48(7) . . ? N3 Mg2 C30 133.61(7) . . ? S1 Mg2 C30 37.58(5) . . ? S2 Mg2 C30 37.58(5) . . ? C33 O2 C31 113.17(18) . . ? C33 O2 Mg1 124.53(13) . . ? C31 O2 Mg1 121.88(13) . . ? C4 N2 C18 119.05(17) . . ? C4 N2 Mg1 118.58(14) . . ? C18 N2 Mg1 121.95(13) . . ? N1 C2 C3 123.7(2) . . ? N1 C2 C1 120.27(19) . . ? C3 C2 C1 116.1(2) . . ? C93 S3 Mg4 82.80(8) . . ? O3 Mg3 O4 94.09(7) . . ? O3 Mg3 N6 127.42(7) . . ? O4 Mg3 N6 107.68(7) . . ? O3 Mg3 N5 120.90(7) . . ? O4 Mg3 N5 112.30(7) . . ? N6 Mg3 N5 94.47(7) . . ? C93 O3 Mg3 121.61(14) . . ? C36 N3 C40 117.68(17) . . ? C36 N3 Mg2 123.09(14) . . ? C40 N3 Mg2 119.09(12) . . ? C2 C3 C4 130.0(2) . . ? C2 C3 H3 115.0 . . ? C4 C3 H3 115.0 . . ? C93 S4 Mg4 83.49(7) . . ? N7 Mg4 N8 93.08(8) . . ? N7 Mg4 S4 113.32(6) . . ? N8 Mg4 S4 128.85(6) . . ? N7 Mg4 S3 132.06(6) . . ? N8 Mg4 S3 119.37(6) . . ? S4 Mg4 S3 74.43(3) . . ? N7 Mg4 C93 132.97(7) . . ? N8 Mg4 C93 133.57(7) . . ? S4 Mg4 C93 37.25(5) . . ? S3 Mg4 C93 37.20(5) . . ? C96A O4 C96 62.0(3) . . ? C96A O4 C94A 114.4(4) . . ? C96 O4 C94A 87.8(4) . . ? C96A O4 C94 83.5(4) . . ? C96 O4 C94 113.9(3) . . ? C94A O4 C94 56.2(4) . . ? C96A O4 Mg3 121.3(3) . . ? C96 O4 Mg3 129.43(19) . . ? C94A O4 Mg3 122.6(3) . . ? C94 O4 Mg3 116.6(2) . . ? C38 N4 C52 117.15(17) . . ? C38 N4 Mg2 123.01(14) . . ? C52 N4 Mg2 119.82(13) . . ? N2 C4 C3 123.54(19) . . ? N2 C4 C5 120.0(2) . . ? C3 C4 C5 116.5(2) . . ? C65 N5 C69 120.95(18) . . ? C65 N5 Mg3 116.84(14) . . ? C69 N5 Mg3 121.50(14) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C67 N6 C81 119.37(18) . . ? C67 N6 Mg3 116.71(14) . . ? C81 N6 Mg3 123.67(14) . . ? C11 C6 C7 120.77(19) . . ? C11 C6 N1 120.30(18) . . ? C7 C6 N1 118.80(17) . . ? C99 N7 C103 115.80(17) . . ? C99 N7 Mg4 123.14(15) . . ? C103 N7 Mg4 120.98(13) . . ? C8 C7 C6 118.25(19) . . ? C8 C7 C12 120.64(19) . . ? C6 C7 C12 121.10(19) . . ? C101 N8 C115 116.60(18) . . ? C101 N8 Mg4 123.51(15) . . ? C115 N8 Mg4 119.80(13) . . ? C9 C8 C7 121.5(2) . . ? C9 C8 H8 119.3 . . ? C7 C8 H8 119.3 . . ? C10 C9 C8 119.7(2) . . ? C10 C9 H9 120.2 . . ? C8 C9 H9 120.2 . . ? C9 C10 C11 121.5(2) . . ? C9 C10 H10 119.3 . . ? C11 C10 H10 119.3 . . ? C10 C11 C6 118.4(2) . . ? C10 C11 C15 119.51(19) . . ? C6 C11 C15 122.13(19) . . ? C14 C12 C7 111.0(2) . . ? C14 C12 C13 109.13(19) . . ? C7 C12 C13 113.10(19) . . ? C14 C12 H12 107.8 . . ? C7 C12 H12 107.8 . . ? C13 C12 H12 107.8 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C11 C15 C16 111.3(2) . . ? C11 C15 C17 111.58(19) . . ? C16 C15 C17 110.3(2) . . ? C11 C15 H15 107.8 . . ? C16 C15 H15 107.8 . . ? C17 C15 H15 107.8 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C23 C18 C19 120.7(2) . . ? C23 C18 N2 120.07(18) . . ? C19 C18 N2 119.14(18) . . ? C20 C19 C18 118.3(2) . . ? C20 C19 C24 119.9(2) . . ? C18 C19 C24 121.7(2) . . ? C21 C20 C19 121.5(2) . . ? C21 C20 H20 119.3 . . ? C19 C20 H20 119.3 . . ? C20 C21 C22 119.7(2) . . ? C20 C21 H21 120.2 . . ? C22 C21 H21 120.2 . . ? C21 C22 C23 121.7(2) . . ? C21 C22 H22 119.2 . . ? C23 C22 H22 119.2 . . ? C22 C23 C18 118.18(19) . . ? C22 C23 C27 119.76(19) . . ? C18 C23 C27 122.06(19) . . ? C25 C24 C26 108.7(2) . . ? C25 C24 C19 111.2(2) . . ? C26 C24 C19 112.5(2) . . ? C25 C24 H24 108.1 . . ? C26 C24 H24 108.1 . . ? C19 C24 H24 108.1 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C23 C27 C29 111.40(18) . . ? C23 C27 C28 111.78(19) . . ? C29 C27 C28 109.31(18) . . ? C23 C27 H27 108.1 . . ? C29 C27 H27 108.1 . . ? C28 C27 H27 108.1 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? O1 C30 S1 119.55(17) . . ? O1 C30 S2 121.28(15) . . ? S1 C30 S2 119.16(12) . . ? O1 C30 Mg2 178.35(16) . . ? S1 C30 Mg2 58.95(6) . . ? S2 C30 Mg2 60.21(6) . . ? O2 C31 C32 111.25(19) . . ? O2 C31 H31A 109.4 . . ? C32 C31 H31A 109.4 . . ? O2 C31 H31B 109.4 . . ? C32 C31 H31B 109.4 . . ? H31A C31 H31B 108.0 . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? O2 C33 C34 112.70(19) . . ? O2 C33 H33A 109.1 . . ? C34 C33 H33A 109.1 . . ? O2 C33 H33B 109.1 . . ? C34 C33 H33B 109.1 . . ? H33A C33 H33B 107.8 . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C36 C35 H35A 109.5 . . ? C36 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C36 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? N3 C36 C37 124.20(19) . . ? N3 C36 C35 120.77(19) . . ? C37 C36 C35 115.03(18) . . ? C36 C37 C38 130.37(19) . . ? C36 C37 H37 114.8 . . ? C38 C37 H37 114.8 . . ? N4 C38 C37 124.36(19) . . ? N4 C38 C39 120.6(2) . . ? C37 C38 C39 115.07(19) . . ? C38 C39 H39A 109.5 . . ? C38 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C38 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C41 C40 C45 121.3(2) . . ? C41 C40 N3 120.89(19) . . ? C45 C40 N3 117.8(2) . . ? C42 C41 C40 118.0(2) . . ? C42 C41 C46 119.4(2) . . ? C40 C41 C46 122.6(2) . . ? C43 C42 C41 121.4(2) . . ? C43 C42 H42 119.3 . . ? C41 C42 H42 119.3 . . ? C44 C43 C42 120.0(2) . . ? C44 C43 H43 120.0 . . ? C42 C43 H43 120.0 . . ? C43 C44 C45 121.2(2) . . ? C43 C44 H44 119.4 . . ? C45 C44 H44 119.4 . . ? C44 C45 C40 118.1(2) . . ? C44 C45 C49 120.2(2) . . ? C40 C45 C49 121.7(2) . . ? C47 C46 C41 111.38(19) . . ? C47 C46 C48 110.0(2) . . ? C41 C46 C48 111.6(2) . . ? C47 C46 H46 107.9 . . ? C41 C46 H46 107.9 . . ? C48 C46 H46 107.9 . . ? C46 C47 H47A 109.5 . . ? C46 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C46 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C46 C48 H48A 109.5 . . ? C46 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C46 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C45 C49 C51 111.3(2) . . ? C45 C49 C50 112.5(2) . . ? C51 C49 C50 110.7(2) . . ? C45 C49 H49 107.3 . . ? C51 C49 H49 107.3 . . ? C50 C49 H49 107.3 . . ? C49 C50 H50A 109.5 . . ? C49 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C49 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C49 C51 H51A 109.5 . . ? C49 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C49 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C53 C52 C57 121.1(2) . . ? C53 C52 N4 120.6(2) . . ? C57 C52 N4 118.32(19) . . ? C54 C53 C52 118.2(2) . . ? C54 C53 C58 119.3(2) . . ? C52 C53 C58 122.6(2) . . ? C55 C54 C53 121.2(2) . . ? C55 C54 H54 119.4 . . ? C53 C54 H54 119.4 . . ? C54 C55 C56 120.1(2) . . ? C54 C55 H55 119.9 . . ? C56 C55 H55 119.9 . . ? C55 C56 C57 121.2(2) . . ? C55 C56 H56 119.4 . . ? C57 C56 H56 119.4 . . ? C56 C57 C52 118.0(2) . . ? C56 C57 C61 120.7(2) . . ? C52 C57 C61 121.3(2) . . ? C53 C58 C59 110.86(19) . . ? C53 C58 C60 112.7(2) . . ? C59 C58 C60 109.5(2) . . ? C53 C58 H58 107.9 . . ? C59 C58 H58 107.9 . . ? C60 C58 H58 107.9 . . ? C58 C59 H59A 109.5 . . ? C58 C59 H59B 109.5 . . ? H59A C59 H59B 109.5 . . ? C58 C59 H59C 109.5 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? C58 C60 H60A 109.5 . . ? C58 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? C58 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? C57 C61 C63 113.07(19) . . ? C57 C61 C62 113.0(2) . . ? C63 C61 C62 110.4(2) . . ? C57 C61 H61 106.6 . . ? C63 C61 H61 106.6 . . ? C62 C61 H61 106.6 . . ? C61 C62 H62A 109.5 . . ? C61 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C61 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? C61 C63 H63A 109.5 . . ? C61 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? C61 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? C65 C64 H64A 109.5 . . ? C65 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? C65 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? N5 C65 C66 123.8(2) . . ? N5 C65 C64 120.5(2) . . ? C66 C65 C64 115.7(2) . . ? C67 C66 C65 130.6(2) . . ? C67 C66 H66 114.7 . . ? C65 C66 H66 114.7 . . ? N6 C67 C66 123.7(2) . . ? N6 C67 C68 120.36(19) . . ? C66 C67 C68 115.89(19) . . ? C67 C68 H68A 109.5 . . ? C67 C68 H68B 109.5 . . ? H68A C68 H68B 109.5 . . ? C67 C68 H68C 109.5 . . ? H68A C68 H68C 109.5 . . ? H68B C68 H68C 109.5 . . ? C74 C69 C70 119.9(2) . . ? C74 C69 N5 120.16(19) . . ? C70 C69 N5 119.7(2) . . ? C71 C70 C69 118.4(2) . . ? C71 C70 C75 118.9(2) . . ? C69 C70 C75 122.7(2) . . ? C72 C71 C70 121.5(2) . . ? C72 C71 H71 119.2 . . ? C70 C71 H71 119.2 . . ? C71 C72 C73 119.9(2) . . ? C71 C72 H72 120.0 . . ? C73 C72 H72 120.0 . . ? C72 C73 C74 121.2(2) . . ? C72 C73 H73 119.4 . . ? C74 C73 H73 119.4 . . ? C73 C74 C69 118.8(2) . . ? C73 C74 C78 118.1(2) . . ? C69 C74 C78 123.0(2) . . ? C70 C75 C76 111.9(3) . . ? C70 C75 C77 110.3(3) . . ? C76 C75 C77 110.7(3) . . ? C70 C75 H75 107.9 . . ? C76 C75 H75 107.9 . . ? C77 C75 H75 107.9 . . ? C75 C76 H76A 109.5 . . ? C75 C76 H76B 109.5 . . ? H76A C76 H76B 109.5 . . ? C75 C76 H76C 109.5 . . ? H76A C76 H76C 109.5 . . ? H76B C76 H76C 109.5 . . ? C75 C77 H77A 109.5 . . ? C75 C77 H77B 109.5 . . ? H77A C77 H77B 109.5 . . ? C75 C77 H77C 109.5 . . ? H77A C77 H77C 109.5 . . ? H77B C77 H77C 109.5 . . ? C74 C78 C79 112.8(2) . . ? C74 C78 C80 109.4(2) . . ? C79 C78 C80 109.5(2) . . ? C74 C78 H78 108.3 . . ? C79 C78 H78 108.3 . . ? C80 C78 H78 108.3 . . ? C78 C79 H79A 109.5 . . ? C78 C79 H79B 109.5 . . ? H79A C79 H79B 109.5 . . ? C78 C79 H79C 109.5 . . ? H79A C79 H79C 109.5 . . ? H79B C79 H79C 109.5 . . ? C78 C80 H80A 109.5 . . ? C78 C80 H80B 109.5 . . ? H80A C80 H80B 109.5 . . ? C78 C80 H80C 109.5 . . ? H80A C80 H80C 109.5 . . ? H80B C80 H80C 109.5 . . ? C86 C81 C82 120.22(19) . . ? C86 C81 N6 119.48(18) . . ? C82 C81 N6 120.06(18) . . ? C83 C82 C81 118.5(2) . . ? C83 C82 C87 119.3(2) . . ? C81 C82 C87 122.2(2) . . ? C84 C83 C82 121.6(2) . . ? C84 C83 H83 119.2 . . ? C82 C83 H83 119.2 . . ? C85 C84 C83 119.8(2) . . ? C85 C84 H84 120.1 . . ? C83 C84 H84 120.1 . . ? C84 C85 C86 121.2(2) . . ? C84 C85 H85 119.4 . . ? C86 C85 H85 119.4 . . ? C85 C86 C81 118.6(2) . . ? C85 C86 C90 120.17(19) . . ? C81 C86 C90 121.11(19) . . ? C89 C87 C88 109.8(3) . . ? C89 C87 C82 112.6(2) . . ? C88 C87 C82 111.5(3) . . ? C89 C87 H87 107.6 . . ? C88 C87 H87 107.6 . . ? C82 C87 H87 107.6 . . ? C87 C88 H88A 109.5 . . ? C87 C88 H88B 109.5 . . ? H88A C88 H88B 109.5 . . ? C87 C88 H88C 109.5 . . ? H88A C88 H88C 109.5 . . ? H88B C88 H88C 109.5 . . ? C87 C89 H89A 109.5 . . ? C87 C89 H89B 109.5 . . ? H89A C89 H89B 109.5 . . ? C87 C89 H89C 109.5 . . ? H89A C89 H89C 109.5 . . ? H89B C89 H89C 109.5 . . ? C92 C90 C91 110.1(2) . . ? C92 C90 C86 111.07(19) . . ? C91 C90 C86 114.0(2) . . ? C92 C90 H90 107.1 . . ? C91 C90 H90 107.1 . . ? C86 C90 H90 107.1 . . ? C90 C91 H91A 109.5 . . ? C90 C91 H91B 109.5 . . ? H91A C91 H91B 109.5 . . ? C90 C91 H91C 109.5 . . ? H91A C91 H91C 109.5 . . ? H91B C91 H91C 109.5 . . ? C90 C92 H92A 109.5 . . ? C90 C92 H92B 109.5 . . ? H92A C92 H92B 109.5 . . ? C90 C92 H92C 109.5 . . ? H92A C92 H92C 109.5 . . ? H92B C92 H92C 109.5 . . ? O3 C93 S4 120.14(16) . . ? O3 C93 S3 120.65(17) . . ? S4 C93 S3 119.20(13) . . ? O3 C93 Mg4 177.96(16) . . ? S4 C93 Mg4 59.26(7) . . ? S3 C93 Mg4 59.99(7) . . ? O4 C94 C95 112.6(5) . . ? O4 C94 H94A 109.1 . . ? C95 C94 H94A 109.1 . . ? O4 C94 H94B 109.1 . . ? C95 C94 H94B 109.1 . . ? H94A C94 H94B 107.8 . . ? O4 C96 C97 113.4(4) . . ? O4 C96 H96A 108.9 . . ? C97 C96 H96A 108.9 . . ? O4 C96 H96B 108.9 . . ? C97 C96 H96B 108.9 . . ? H96A C96 H96B 107.7 . . ? C99 C98 H98A 109.5 . . ? C99 C98 H98B 109.5 . . ? H98A C98 H98B 109.5 . . ? C99 C98 H98C 109.5 . . ? H98A C98 H98C 109.5 . . ? H98B C98 H98C 109.5 . . ? N7 C99 C100 124.1(2) . . ? N7 C99 C98 120.0(2) . . ? C100 C99 C98 115.9(2) . . ? C99 C100 C101 129.7(2) . . ? C99 C100 H100 115.2 . . ? C101 C100 H100 115.2 . . ? N8 C101 C100 123.9(2) . . ? N8 C101 C102 121.0(2) . . ? C100 C101 C102 115.0(2) . . ? C101 C102 H10A 109.5 . . ? C101 C102 H10B 109.5 . . ? H10A C102 H10B 109.5 . . ? C101 C102 H10C 109.5 . . ? H10A C102 H10C 109.5 . . ? H10B C102 H10C 109.5 . . ? C104 C103 C108 121.1(2) . . ? C104 C103 N7 118.59(19) . . ? C108 C103 N7 120.36(18) . . ? C105 C104 C103 118.2(2) . . ? C105 C104 C109 120.60(19) . . ? C103 C104 C109 121.18(19) . . ? C106 C105 C104 121.6(2) . . ? C106 C105 H105 119.2 . . ? C104 C105 H105 119.2 . . ? C105 C106 C107 119.4(2) . . ? C105 C106 H106 120.3 . . ? C107 C106 H106 120.3 . . ? C106 C107 C108 121.5(2) . . ? C106 C107 H107 119.3 . . ? C108 C107 H107 119.3 . . ? C107 C108 C103 118.2(2) . . ? C107 C108 C112 120.2(2) . . ? C103 C108 C112 121.53(19) . . ? C104 C109 C111 111.3(2) . . ? C104 C109 C110 112.8(2) . . ? C111 C109 C110 110.6(2) . . ? C104 C109 H109 107.3 . . ? C111 C109 H109 107.3 . . ? C110 C109 H109 107.3 . . ? C109 C110 H11A 109.5 . . ? C109 C110 H11B 109.5 . . ? H11A C110 H11B 109.5 . . ? C109 C110 H11C 109.5 . . ? H11A C110 H11C 109.5 . . ? H11B C110 H11C 109.5 . . ? C109 C111 H11D 109.5 . . ? C109 C111 H11E 109.5 . . ? H11D C111 H11E 109.5 . . ? C109 C111 H11F 109.5 . . ? H11D C111 H11F 109.5 . . ? H11E C111 H11F 109.5 . . ? C113 C112 C114 109.7(2) . . ? C113 C112 C108 110.13(18) . . ? C114 C112 C108 113.5(2) . . ? C113 C112 H112 107.7 . . ? C114 C112 H112 107.7 . . ? C108 C112 H112 107.7 . . ? C112 C113 H11G 109.5 . . ? C112 C113 H11H 109.5 . . ? H11G C113 H11H 109.5 . . ? C112 C113 H11I 109.5 . . ? H11G C113 H11I 109.5 . . ? H11H C113 H11I 109.5 . . ? C112 C114 H11J 109.5 . . ? C112 C114 H11K 109.5 . . ? H11J C114 H11K 109.5 . . ? C112 C114 H11L 109.5 . . ? H11J C114 H11L 109.5 . . ? H11K C114 H11L 109.5 . . ? C120 C115 C116 121.6(2) . . ? C120 C115 N8 119.36(19) . . ? C116 C115 N8 119.1(2) . . ? C117 C116 C115 117.4(2) . . ? C117 C116 C121 120.1(2) . . ? C115 C116 C121 122.5(2) . . ? C118 C117 C116 121.9(2) . . ? C118 C117 H117 119.1 . . ? C116 C117 H117 119.1 . . ? C117 C118 C119 119.8(2) . . ? C117 C118 H118 120.1 . . ? C119 C118 H118 120.1 . . ? C118 C119 C120 121.3(3) . . ? C118 C119 H119 119.4 . . ? C120 C119 H119 119.4 . . ? C115 C120 C119 118.0(2) . . ? C115 C120 C124 121.9(2) . . ? C119 C120 C124 120.0(2) . . ? C116 C121 C123 112.7(2) . . ? C116 C121 C122 111.1(2) . . ? C123 C121 C122 109.9(2) . . ? C116 C121 H121 107.7 . . ? C123 C121 H121 107.7 . . ? C122 C121 H121 107.7 . . ? C121 C122 H12A 109.5 . . ? C121 C122 H12B 109.5 . . ? H12A C122 H12B 109.5 . . ? C121 C122 H12C 109.5 . . ? H12A C122 H12C 109.5 . . ? H12B C122 H12C 109.5 . . ? C121 C123 H12D 109.5 . . ? C121 C123 H12E 109.5 . . ? H12D C123 H12E 109.5 . . ? C121 C123 H12F 109.5 . . ? H12D C123 H12F 109.5 . . ? H12E C123 H12F 109.5 . . ? C125 C124 C120 113.4(2) . . ? C125 C124 C126 110.3(2) . . ? C120 C124 C126 111.3(2) . . ? C125 C124 H124 107.2 . . ? C120 C124 H124 107.2 . . ? C126 C124 H124 107.2 . . ? C124 C125 H12G 109.5 . . ? C124 C125 H12H 109.5 . . ? H12G C125 H12H 109.5 . . ? C124 C125 H12I 109.5 . . ? H12G C125 H12I 109.5 . . ? H12H C125 H12I 109.5 . . ? C124 C126 H12J 109.5 . . ? C124 C126 H12K 109.5 . . ? H12J C126 H12K 109.5 . . ? C124 C126 H12L 109.5 . . ? H12J C126 H12L 109.5 . . ? H12K C126 H12L 109.5 . . ? O4 C96A C97A 111.9(8) . . ? O4 C96A H96C 109.2 . . ? C97A C96A H96C 109.2 . . ? O4 C96A H96D 109.2 . . ? C97A C96A H96D 109.2 . . ? H96C C96A H96D 107.9 . . ? O4 C94A C95A 106.1(7) . . ? O4 C94A H94C 110.5 . . ? C95A C94A H94C 110.5 . . ? O4 C94A H94D 110.5 . . ? C95A C94A H94D 110.5 . . ? H94C C94A H94D 108.7 . . ? C94A C95A H95D 109.5 . . ? C94A C95A H95E 109.5 . . ? H95D C95A H95E 109.5 . . ? C94A C95A H95F 109.5 . . ? H95D C95A H95F 109.5 . . ? H95E C95A H95F 109.5 . . ? C96A C97A H97D 109.5 . . ? C96A C97A H97E 109.5 . . ? H97D C97A H97E 109.5 . . ? C96A C97A H97F 109.5 . . ? H97D C97A H97F 109.5 . . ? H97E C97A H97F 109.5 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.552 _refine_diff_density_min -0.330 _refine_diff_density_rms 0.051 _database_code_depnum_ccdc_archive 'CCDC 955175'