# 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_vb5 _database_code_depnum_ccdc_archive 'CCDC 916806' #TrackingRef 'All7.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C37 H58 Mg N2 O' _chemical_formula_weight 571.16 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Mg Mg 0.0486 0.0363 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _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 9.1792(4) _cell_length_b 12.1190(4) _cell_length_c 15.8077(6) _cell_angle_alpha 85.527(3) _cell_angle_beta 77.912(3) _cell_angle_gamma 87.404(3) _cell_volume 1713.51(11) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 6793 _cell_measurement_theta_min 2.7822 _cell_measurement_theta_max 30.2932 _exptl_crystal_description 'fragment from plate' _exptl_crystal_colour colourless _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.107 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 628 _exptl_absorpt_coefficient_mu 0.082 _exptl_absorpt_correction_T_min 0.85976 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _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 'Oxford Diffraction Gemini S' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20725 _diffrn_reflns_av_R_equivalents 0.0499 _diffrn_reflns_av_sigmaI/netI 0.0915 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.79 _diffrn_reflns_theta_max 29.00 _reflns_number_total 8803 _reflns_number_gt 5110 _reflns_threshold_expression I>2\s(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0586P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8803 _refine_ls_number_parameters 381 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0998 _refine_ls_R_factor_gt 0.0513 _refine_ls_wR_factor_ref 0.1217 _refine_ls_wR_factor_gt 0.1110 _refine_ls_goodness_of_fit_ref 0.900 _refine_ls_restrained_S_all 0.900 _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 0.97385(6) 0.72505(4) 0.21542(3) 0.02006(14) Uani 1 1 d . . . O1 O 1.18457(12) 0.76197(10) 0.14787(7) 0.0266(3) Uani 1 1 d . . . N1 N 1.00116(14) 0.56414(11) 0.26441(8) 0.0200(3) Uani 1 1 d . . . N2 N 0.97339(14) 0.78941(10) 0.33227(8) 0.0198(3) Uani 1 1 d . . . C1 C 0.95529(18) 0.47127(13) 0.22552(10) 0.0211(4) Uani 1 1 d . . . C2 C 1.05395(19) 0.41579(13) 0.16072(10) 0.0243(4) Uani 1 1 d . . . C3 C 1.0032(2) 0.32536(14) 0.12709(11) 0.0296(4) Uani 1 1 d . . . H3 H 1.0693 0.2871 0.0837 0.036 Uiso 1 1 calc R . . C4 C 0.8597(2) 0.29022(14) 0.15530(11) 0.0296(4) Uani 1 1 d . . . H4 H 0.8287 0.2263 0.1335 0.036 Uiso 1 1 calc R . . C5 C 0.7609(2) 0.34832(14) 0.21545(11) 0.0278(4) Uani 1 1 d . . . H5 H 0.6609 0.3252 0.2331 0.033 Uiso 1 1 calc R . . C6 C 0.80465(18) 0.43975(13) 0.25059(10) 0.0231(4) Uani 1 1 d . . . C7 C 0.69439(18) 0.50395(14) 0.31564(12) 0.0289(4) Uani 1 1 d . . . H7 H 0.7249 0.5829 0.3074 0.035 Uiso 1 1 calc R . . C8 C 1.21058(19) 0.45461(15) 0.12316(11) 0.0329(4) Uani 1 1 d . . . H8 H 1.2302 0.5171 0.1566 0.039 Uiso 1 1 calc R . . C9 C 0.90158(17) 0.89582(13) 0.35000(10) 0.0208(3) Uani 1 1 d . . . C10 C 0.74616(18) 0.89947(13) 0.38424(10) 0.0226(4) Uani 1 1 d . . . C11 C 0.67442(19) 1.00218(14) 0.39500(11) 0.0288(4) Uani 1 1 d . . . H11 H 0.5705 1.0057 0.4189 0.035 Uiso 1 1 calc R . . C12 C 0.74976(19) 1.09916(14) 0.37196(11) 0.0284(4) Uani 1 1 d . . . H12 H 0.6980 1.1686 0.3792 0.034 Uiso 1 1 calc R . . C13 C 0.90147(19) 1.09476(14) 0.33814(10) 0.0258(4) Uani 1 1 d . . . H13 H 0.9532 1.1618 0.3222 0.031 Uiso 1 1 calc R . . C14 C 0.97981(18) 0.99446(13) 0.32701(10) 0.0215(4) Uani 1 1 d . . . C15 C 0.66097(18) 0.79317(14) 0.41132(12) 0.0293(4) Uani 1 1 d . . . H15 H 0.7167 0.7332 0.3768 0.035 Uiso 1 1 calc R . . C16 C 1.14699(18) 0.99521(14) 0.28887(11) 0.0260(4) Uani 1 1 d . . . H16 H 1.1861 0.9169 0.2903 0.031 Uiso 1 1 calc R . . C17 C 1.04584(17) 0.73686(13) 0.38882(10) 0.0205(3) Uani 1 1 d . . . C18 C 1.09777(17) 0.62567(13) 0.38347(10) 0.0210(3) Uani 1 1 d . . . H18 H 1.1636 0.6024 0.4208 0.025 Uiso 1 1 calc R . . C19 C 1.06757(17) 0.54410(13) 0.33169(10) 0.0209(3) Uani 1 1 d . . . C20 C 1.07377(18) 0.79457(14) 0.46499(10) 0.0248(4) Uani 1 1 d . . . H20A H 0.9815 0.8319 0.4933 0.037 Uiso 1 1 calc R . . H20B H 1.1510 0.8494 0.4446 0.037 Uiso 1 1 calc R . . H20C H 1.1070 0.7399 0.5065 0.037 Uiso 1 1 calc R . . C21 C 1.11280(19) 0.42665(14) 0.35795(11) 0.0282(4) Uani 1 1 d . . . H21A H 1.0352 0.3762 0.3527 0.042 Uiso 1 1 calc R . . H21B H 1.1254 0.4223 0.4182 0.042 Uiso 1 1 calc R . . H21C H 1.2070 0.4055 0.3200 0.042 Uiso 1 1 calc R . . C22 C 1.32499(18) 0.74141(16) 0.17605(11) 0.0300(4) Uani 1 1 d . . . H22A H 1.3191 0.6761 0.2182 0.036 Uiso 1 1 calc R . . H22B H 1.3517 0.8064 0.2032 0.036 Uiso 1 1 calc R . . C23 C 1.43693(19) 0.72066(16) 0.09414(11) 0.0341(4) Uani 1 1 d . . . H23A H 1.4346 0.6433 0.0785 0.041 Uiso 1 1 calc R . . H23B H 1.5392 0.7367 0.0997 0.041 Uiso 1 1 calc R . . C24 C 1.3831(2) 0.80223(18) 0.02808(12) 0.0412(5) Uani 1 1 d . . . H24A H 1.4213 0.8770 0.0296 0.049 Uiso 1 1 calc R . . H24B H 1.4153 0.7774 -0.0313 0.049 Uiso 1 1 calc R . . C25 C 1.21523(19) 0.80192(16) 0.05681(10) 0.0308(4) Uani 1 1 d . . . H25A H 1.1720 0.8775 0.0496 0.037 Uiso 1 1 calc R . . H25B H 1.1720 0.7525 0.0221 0.037 Uiso 1 1 calc R . . C26 C 0.8140(2) 0.76058(15) 0.13646(12) 0.0320(4) Uani 1 1 d . . . H26A H 0.8171 0.6965 0.1008 0.038 Uiso 1 1 calc R . . H26B H 0.7150 0.7611 0.1761 0.038 Uiso 1 1 calc R . . C27 C 0.8174(2) 0.86432(16) 0.07487(12) 0.0363(5) Uani 1 1 d . . . H27A H 0.9146 0.8659 0.0335 0.044 Uiso 1 1 calc R . . H27B H 0.7386 0.8602 0.0411 0.044 Uiso 1 1 calc R . . C28 C 0.7948(2) 0.97023(16) 0.12032(13) 0.0401(5) Uani 1 1 d . . . H28A H 0.8286 1.0325 0.0774 0.048 Uiso 1 1 calc R . . H28B H 0.8580 0.9666 0.1641 0.048 Uiso 1 1 calc R . . C29 C 0.6344(2) 0.99404(19) 0.16494(14) 0.0517(6) Uani 1 1 d . . . H29A H 0.6283 1.0634 0.1936 0.078 Uiso 1 1 calc R . . H29B H 0.6001 0.9333 0.2082 0.078 Uiso 1 1 calc R . . H29C H 0.5713 1.0008 0.1218 0.078 Uiso 1 1 calc R . . C30 C 1.1776(2) 1.04151(16) 0.19474(12) 0.0368(5) Uani 1 1 d . . . H30A H 1.1230 0.9995 0.1615 0.055 Uiso 1 1 calc R . . H30B H 1.2847 1.0352 0.1702 0.055 Uiso 1 1 calc R . . H30C H 1.1448 1.1196 0.1919 0.055 Uiso 1 1 calc R . . C31 C 1.2311(2) 1.06057(15) 0.34149(13) 0.0368(5) Uani 1 1 d . . . H31A H 1.3386 1.0507 0.3197 0.055 Uiso 1 1 calc R . . H31B H 1.2057 1.0335 0.4027 0.055 Uiso 1 1 calc R . . H31C H 1.2027 1.1393 0.3357 0.055 Uiso 1 1 calc R . . C32 C 0.5030(2) 0.80102(18) 0.39421(13) 0.0438(5) Uani 1 1 d . . . H32A H 0.4567 0.7288 0.4090 0.066 Uiso 1 1 calc R . . H32B H 0.5068 0.8228 0.3328 0.066 Uiso 1 1 calc R . . H32C H 0.4440 0.8564 0.4299 0.066 Uiso 1 1 calc R . . C33 C 0.6542(2) 0.75921(16) 0.50691(13) 0.0433(5) Uani 1 1 d . . . H33A H 0.6018 0.6895 0.5225 0.065 Uiso 1 1 calc R . . H33B H 0.6007 0.8170 0.5423 0.065 Uiso 1 1 calc R . . H33C H 0.7556 0.7493 0.5174 0.065 Uiso 1 1 calc R . . C34 C 0.6990(2) 0.46364(17) 0.40891(12) 0.0409(5) Uani 1 1 d . . . H34A H 0.6251 0.5058 0.4488 0.061 Uiso 1 1 calc R . . H34B H 0.7986 0.4744 0.4197 0.061 Uiso 1 1 calc R . . H34C H 0.6764 0.3848 0.4182 0.061 Uiso 1 1 calc R . . C35 C 0.5343(2) 0.50231(18) 0.30156(14) 0.0469(5) Uani 1 1 d . . . H35A H 0.4706 0.5526 0.3401 0.070 Uiso 1 1 calc R . . H35B H 0.4974 0.4270 0.3145 0.070 Uiso 1 1 calc R . . H35C H 0.5327 0.5263 0.2411 0.070 Uiso 1 1 calc R . . C36 C 1.2221(3) 0.49793(18) 0.02827(12) 0.0519(6) Uani 1 1 d . . . H36A H 1.3204 0.5293 0.0058 0.078 Uiso 1 1 calc R . . H36B H 1.1446 0.5553 0.0246 0.078 Uiso 1 1 calc R . . H36C H 1.2087 0.4368 -0.0063 0.078 Uiso 1 1 calc R . . C37 C 1.3292(2) 0.36319(18) 0.12924(16) 0.0534(6) Uani 1 1 d . . . H37A H 1.4285 0.3935 0.1082 0.080 Uiso 1 1 calc R . . H37B H 1.3158 0.3032 0.0936 0.080 Uiso 1 1 calc R . . H37C H 1.3193 0.3343 0.1898 0.080 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 0.0178(3) 0.0229(3) 0.0198(3) -0.0032(2) -0.0042(2) 0.0005(2) O1 0.0177(6) 0.0403(7) 0.0211(6) 0.0012(5) -0.0036(5) 0.0000(5) N1 0.0174(7) 0.0226(7) 0.0195(7) -0.0035(6) -0.0017(6) 0.0003(6) N2 0.0162(7) 0.0228(7) 0.0199(7) -0.0030(6) -0.0017(5) -0.0008(6) C1 0.0243(9) 0.0200(8) 0.0200(8) -0.0009(7) -0.0069(7) 0.0001(7) C2 0.0261(9) 0.0231(9) 0.0232(9) -0.0033(7) -0.0036(7) -0.0003(7) C3 0.0364(11) 0.0270(9) 0.0246(9) -0.0067(8) -0.0029(8) 0.0003(8) C4 0.0399(11) 0.0238(9) 0.0276(9) -0.0048(8) -0.0103(8) -0.0058(8) C5 0.0269(9) 0.0280(9) 0.0295(9) 0.0002(8) -0.0078(8) -0.0053(8) C6 0.0240(9) 0.0241(9) 0.0217(8) 0.0013(7) -0.0067(7) -0.0009(7) C7 0.0199(9) 0.0283(9) 0.0373(10) -0.0060(8) -0.0015(8) -0.0033(7) C8 0.0283(10) 0.0344(10) 0.0332(10) -0.0149(9) 0.0050(8) -0.0045(8) C9 0.0216(8) 0.0244(8) 0.0173(8) -0.0047(7) -0.0051(7) 0.0009(7) C10 0.0213(9) 0.0268(9) 0.0198(8) -0.0057(7) -0.0028(7) -0.0009(7) C11 0.0219(9) 0.0357(10) 0.0280(9) -0.0080(8) -0.0022(7) 0.0023(8) C12 0.0283(10) 0.0259(9) 0.0310(10) -0.0077(8) -0.0060(8) 0.0074(8) C13 0.0290(10) 0.0232(9) 0.0256(9) -0.0033(8) -0.0053(7) -0.0032(7) C14 0.0224(9) 0.0242(9) 0.0189(8) -0.0047(7) -0.0050(7) -0.0006(7) C15 0.0186(9) 0.0295(9) 0.0376(10) -0.0111(8) 0.0025(8) -0.0011(7) C16 0.0210(9) 0.0236(9) 0.0323(10) -0.0053(8) -0.0017(7) -0.0011(7) C17 0.0147(8) 0.0275(9) 0.0183(8) -0.0019(7) -0.0006(6) -0.0023(7) C18 0.0175(8) 0.0273(9) 0.0190(8) -0.0016(7) -0.0060(6) 0.0005(7) C19 0.0150(8) 0.0236(9) 0.0223(8) -0.0004(7) -0.0004(7) -0.0002(7) C20 0.0233(9) 0.0304(9) 0.0220(8) -0.0049(7) -0.0069(7) 0.0000(7) C21 0.0252(9) 0.0289(9) 0.0305(10) -0.0013(8) -0.0069(8) 0.0038(8) C22 0.0205(9) 0.0413(11) 0.0302(10) -0.0054(8) -0.0089(7) 0.0000(8) C23 0.0196(9) 0.0479(12) 0.0348(10) -0.0087(9) -0.0035(8) -0.0013(8) C24 0.0265(10) 0.0614(13) 0.0320(10) 0.0013(10) 0.0020(8) -0.0060(10) C25 0.0281(10) 0.0434(11) 0.0189(8) 0.0024(8) -0.0021(7) 0.0007(8) C26 0.0304(10) 0.0353(10) 0.0348(10) -0.0061(9) -0.0157(8) 0.0012(8) C27 0.0283(10) 0.0509(12) 0.0310(10) 0.0036(9) -0.0115(8) -0.0005(9) C28 0.0375(11) 0.0450(12) 0.0394(11) 0.0086(10) -0.0146(9) -0.0053(10) C29 0.0500(14) 0.0543(13) 0.0481(13) -0.0054(11) -0.0045(11) 0.0059(11) C30 0.0297(10) 0.0397(11) 0.0366(11) -0.0020(9) 0.0026(8) -0.0018(9) C31 0.0255(10) 0.0381(11) 0.0489(12) -0.0094(10) -0.0094(9) -0.0041(8) C32 0.0324(11) 0.0564(13) 0.0446(12) 0.0014(11) -0.0112(9) -0.0161(10) C33 0.0360(11) 0.0411(12) 0.0530(13) 0.0146(10) -0.0138(10) -0.0101(9) C34 0.0282(10) 0.0591(13) 0.0316(10) -0.0080(10) 0.0042(8) -0.0008(10) C35 0.0251(10) 0.0560(13) 0.0601(14) -0.0115(11) -0.0086(10) 0.0057(10) C36 0.0615(15) 0.0571(14) 0.0333(11) -0.0083(11) 0.0066(10) -0.0274(12) C37 0.0278(11) 0.0543(13) 0.0735(16) -0.0204(12) 0.0051(11) 0.0022(10) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mg1 O1 2.0544(12) . ? Mg1 N2 2.0594(14) . ? Mg1 N1 2.0657(14) . ? Mg1 C26 2.1268(16) . ? O1 C22 1.4546(18) . ? O1 C25 1.4559(19) . ? N1 C19 1.3340(19) . ? N1 C1 1.4426(19) . ? N2 C17 1.3300(19) . ? N2 C9 1.442(2) . ? C1 C2 1.409(2) . ? C1 C6 1.418(2) . ? C2 C3 1.393(2) . ? C2 C8 1.517(2) . ? C3 C4 1.375(2) . ? C3 H3 0.9500 . ? C4 C5 1.381(2) . ? C4 H4 0.9500 . ? C5 C6 1.388(2) . ? C5 H5 0.9500 . ? C6 C7 1.518(2) . ? C7 C34 1.525(2) . ? C7 C35 1.533(2) . ? C7 H7 1.0000 . ? C8 C37 1.530(3) . ? C8 C36 1.534(3) . ? C8 H8 1.0000 . ? C9 C14 1.406(2) . ? C9 C10 1.416(2) . ? C10 C11 1.387(2) . ? C10 C15 1.523(2) . ? C11 C12 1.376(2) . ? C11 H11 0.9500 . ? C12 C13 1.383(2) . ? C12 H12 0.9500 . ? C13 C14 1.388(2) . ? C13 H13 0.9500 . ? C14 C16 1.527(2) . ? C15 C33 1.524(2) . ? C15 C32 1.528(2) . ? C15 H15 1.0000 . ? C16 C30 1.522(2) . ? C16 C31 1.530(2) . ? C16 H16 1.0000 . ? C17 C18 1.412(2) . ? C17 C20 1.510(2) . ? C18 C19 1.404(2) . ? C18 H18 0.9500 . ? C19 C21 1.516(2) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 C23 1.505(2) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.524(3) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 C25 1.513(2) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 C27 1.526(2) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 C28 1.505(3) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 C29 1.519(3) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 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 N2 101.10(5) . . ? O1 Mg1 N1 102.70(5) . . ? N2 Mg1 N1 92.96(5) . . ? O1 Mg1 C26 110.95(6) . . ? N2 Mg1 C26 126.35(7) . . ? N1 Mg1 C26 118.96(6) . . ? C22 O1 C25 109.06(12) . . ? C22 O1 Mg1 127.97(10) . . ? C25 O1 Mg1 122.56(9) . . ? C19 N1 C1 118.48(13) . . ? C19 N1 Mg1 119.85(10) . . ? C1 N1 Mg1 121.62(9) . . ? C17 N2 C9 120.03(13) . . ? C17 N2 Mg1 120.60(10) . . ? C9 N2 Mg1 119.24(10) . . ? C2 C1 C6 119.82(14) . . ? C2 C1 N1 121.69(14) . . ? C6 C1 N1 118.41(14) . . ? C3 C2 C1 118.73(16) . . ? C3 C2 C8 118.90(15) . . ? C1 C2 C8 122.30(14) . . ? C4 C3 C2 121.47(17) . . ? C4 C3 H3 119.3 . . ? C2 C3 H3 119.3 . . ? C3 C4 C5 119.68(16) . . ? C3 C4 H4 120.2 . . ? C5 C4 H4 120.2 . . ? C4 C5 C6 121.37(16) . . ? C4 C5 H5 119.3 . . ? C6 C5 H5 119.3 . . ? C5 C6 C1 118.69(15) . . ? C5 C6 C7 120.87(15) . . ? C1 C6 C7 120.44(14) . . ? C6 C7 C34 111.90(14) . . ? C6 C7 C35 112.96(15) . . ? C34 C7 C35 109.97(15) . . ? C6 C7 H7 107.2 . . ? C34 C7 H7 107.2 . . ? C35 C7 H7 107.2 . . ? C2 C8 C37 112.46(15) . . ? C2 C8 C36 109.64(15) . . ? C37 C8 C36 109.84(17) . . ? C2 C8 H8 108.3 . . ? C37 C8 H8 108.3 . . ? C36 C8 H8 108.3 . . ? C14 C9 C10 120.31(15) . . ? C14 C9 N2 121.35(14) . . ? C10 C9 N2 118.10(14) . . ? C11 C10 C9 118.35(15) . . ? C11 C10 C15 120.87(15) . . ? C9 C10 C15 120.75(14) . . ? C12 C11 C10 121.76(16) . . ? C12 C11 H11 119.1 . . ? C10 C11 H11 119.1 . . ? C11 C12 C13 119.46(16) . . ? C11 C12 H12 120.3 . . ? C13 C12 H12 120.3 . . ? C12 C13 C14 121.44(16) . . ? C12 C13 H13 119.3 . . ? C14 C13 H13 119.3 . . ? C13 C14 C9 118.67(15) . . ? C13 C14 C16 118.89(15) . . ? C9 C14 C16 122.43(14) . . ? C10 C15 C33 110.84(14) . . ? C10 C15 C32 113.34(15) . . ? C33 C15 C32 109.21(15) . . ? C10 C15 H15 107.8 . . ? C33 C15 H15 107.8 . . ? C32 C15 H15 107.8 . . ? C30 C16 C14 110.96(13) . . ? C30 C16 C31 109.92(15) . . ? C14 C16 C31 112.10(14) . . ? C30 C16 H16 107.9 . . ? C14 C16 H16 107.9 . . ? C31 C16 H16 107.9 . . ? N2 C17 C18 123.38(14) . . ? N2 C17 C20 120.50(14) . . ? C18 C17 C20 116.10(13) . . ? C19 C18 C17 130.26(14) . . ? C19 C18 H18 114.9 . . ? C17 C18 H18 114.9 . . ? N1 C19 C18 124.35(14) . . ? N1 C19 C21 120.16(14) . . ? C18 C19 C21 115.48(13) . . ? C17 C20 H20A 109.5 . . ? C17 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C17 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? O1 C22 C23 104.46(13) . . ? O1 C22 H22A 110.9 . . ? C23 C22 H22A 110.9 . . ? O1 C22 H22B 110.9 . . ? C23 C22 H22B 110.9 . . ? H22A C22 H22B 108.9 . . ? C22 C23 C24 102.02(14) . . ? C22 C23 H23A 111.4 . . ? C24 C23 H23A 111.4 . . ? C22 C23 H23B 111.4 . . ? C24 C23 H23B 111.4 . . ? H23A C23 H23B 109.2 . . ? C25 C24 C23 103.54(14) . . ? C25 C24 H24A 111.1 . . ? C23 C24 H24A 111.1 . . ? C25 C24 H24B 111.1 . . ? C23 C24 H24B 111.1 . . ? H24A C24 H24B 109.0 . . ? O1 C25 C24 106.19(13) . . ? O1 C25 H25A 110.5 . . ? C24 C25 H25A 110.5 . . ? O1 C25 H25B 110.5 . . ? C24 C25 H25B 110.5 . . ? H25A C25 H25B 108.7 . . ? C27 C26 Mg1 122.90(12) . . ? C27 C26 H26A 106.6 . . ? Mg1 C26 H26A 106.6 . . ? C27 C26 H26B 106.6 . . ? Mg1 C26 H26B 106.6 . . ? H26A C26 H26B 106.6 . . ? C28 C27 C26 113.55(15) . . ? C28 C27 H27A 108.9 . . ? C26 C27 H27A 108.9 . . ? C28 C27 H27B 108.9 . . ? C26 C27 H27B 108.9 . . ? H27A C27 H27B 107.7 . . ? C27 C28 C29 114.00(17) . . ? C27 C28 H28A 108.8 . . ? C29 C28 H28A 108.8 . . ? C27 C28 H28B 108.8 . . ? C29 C28 H28B 108.8 . . ? H28A C28 H28B 107.6 . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C16 C30 H30A 109.5 . . ? C16 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C16 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C16 C31 H31A 109.5 . . ? C16 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C16 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C15 C32 H32A 109.5 . . ? C15 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C15 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C15 C33 H33A 109.5 . . ? C15 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C15 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C7 C34 H34A 109.5 . . ? C7 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C7 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C7 C35 H35A 109.5 . . ? C7 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C7 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C8 C36 H36A 109.5 . . ? C8 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C8 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C8 C37 H37A 109.5 . . ? C8 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C8 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Mg1 O1 C22 49.24(14) . . . . ? N1 Mg1 O1 C22 -46.40(13) . . . . ? C26 Mg1 O1 C22 -174.55(13) . . . . ? N2 Mg1 O1 C25 -138.93(12) . . . . ? N1 Mg1 O1 C25 125.43(12) . . . . ? C26 Mg1 O1 C25 -2.72(14) . . . . ? O1 Mg1 N1 C19 75.58(12) . . . . ? N2 Mg1 N1 C19 -26.51(12) . . . . ? C26 Mg1 N1 C19 -161.49(12) . . . . ? O1 Mg1 N1 C1 -101.95(12) . . . . ? N2 Mg1 N1 C1 155.97(12) . . . . ? C26 Mg1 N1 C1 20.98(14) . . . . ? O1 Mg1 N2 C17 -75.70(12) . . . . ? N1 Mg1 N2 C17 27.86(12) . . . . ? C26 Mg1 N2 C17 157.66(11) . . . . ? O1 Mg1 N2 C9 100.35(11) . . . . ? N1 Mg1 N2 C9 -156.08(11) . . . . ? C26 Mg1 N2 C9 -26.28(14) . . . . ? C19 N1 C1 C2 -85.81(19) . . . . ? Mg1 N1 C1 C2 91.74(16) . . . . ? C19 N1 C1 C6 97.53(17) . . . . ? Mg1 N1 C1 C6 -84.92(16) . . . . ? C6 C1 C2 C3 -4.6(2) . . . . ? N1 C1 C2 C3 178.78(14) . . . . ? C6 C1 C2 C8 172.20(15) . . . . ? N1 C1 C2 C8 -4.4(2) . . . . ? C1 C2 C3 C4 0.5(2) . . . . ? C8 C2 C3 C4 -176.43(15) . . . . ? C2 C3 C4 C5 3.0(3) . . . . ? C3 C4 C5 C6 -2.3(2) . . . . ? C4 C5 C6 C1 -1.8(2) . . . . ? C4 C5 C6 C7 179.08(15) . . . . ? C2 C1 C6 C5 5.3(2) . . . . ? N1 C1 C6 C5 -178.01(13) . . . . ? C2 C1 C6 C7 -175.65(15) . . . . ? N1 C1 C6 C7 1.1(2) . . . . ? C5 C6 C7 C34 94.02(18) . . . . ? C1 C6 C7 C34 -85.05(19) . . . . ? C5 C6 C7 C35 -30.7(2) . . . . ? C1 C6 C7 C35 150.20(16) . . . . ? C3 C2 C8 C37 -57.5(2) . . . . ? C1 C2 C8 C37 125.68(18) . . . . ? C3 C2 C8 C36 65.0(2) . . . . ? C1 C2 C8 C36 -111.80(18) . . . . ? C17 N2 C9 C14 86.73(18) . . . . ? Mg1 N2 C9 C14 -89.34(15) . . . . ? C17 N2 C9 C10 -98.88(17) . . . . ? Mg1 N2 C9 C10 85.04(15) . . . . ? C14 C9 C10 C11 -0.5(2) . . . . ? N2 C9 C10 C11 -174.98(14) . . . . ? C14 C9 C10 C15 -178.57(14) . . . . ? N2 C9 C10 C15 7.0(2) . . . . ? C9 C10 C11 C12 1.1(2) . . . . ? C15 C10 C11 C12 179.17(15) . . . . ? C10 C11 C12 C13 -0.8(3) . . . . ? C11 C12 C13 C14 -0.1(2) . . . . ? C12 C13 C14 C9 0.7(2) . . . . ? C12 C13 C14 C16 179.66(15) . . . . ? C10 C9 C14 C13 -0.4(2) . . . . ? N2 C9 C14 C13 173.90(14) . . . . ? C10 C9 C14 C16 -179.29(14) . . . . ? N2 C9 C14 C16 -5.0(2) . . . . ? C11 C10 C15 C33 -86.25(19) . . . . ? C9 C10 C15 C33 91.73(18) . . . . ? C11 C10 C15 C32 37.0(2) . . . . ? C9 C10 C15 C32 -145.07(16) . . . . ? C13 C14 C16 C30 -66.76(19) . . . . ? C9 C14 C16 C30 112.16(17) . . . . ? C13 C14 C16 C31 56.6(2) . . . . ? C9 C14 C16 C31 -124.52(16) . . . . ? C9 N2 C17 C18 169.28(14) . . . . ? Mg1 N2 C17 C18 -14.7(2) . . . . ? C9 N2 C17 C20 -9.3(2) . . . . ? Mg1 N2 C17 C20 166.76(11) . . . . ? N2 C17 C18 C19 -11.4(3) . . . . ? C20 C17 C18 C19 167.20(16) . . . . ? C1 N1 C19 C18 -170.15(15) . . . . ? Mg1 N1 C19 C18 12.3(2) . . . . ? C1 N1 C19 C21 8.5(2) . . . . ? Mg1 N1 C19 C21 -169.11(11) . . . . ? C17 C18 C19 N1 12.8(3) . . . . ? C17 C18 C19 C21 -165.93(16) . . . . ? C25 O1 C22 C23 -24.68(18) . . . . ? Mg1 O1 C22 C23 148.05(12) . . . . ? O1 C22 C23 C24 37.16(18) . . . . ? C22 C23 C24 C25 -35.76(19) . . . . ? C22 O1 C25 C24 1.68(19) . . . . ? Mg1 O1 C25 C24 -171.51(12) . . . . ? C23 C24 C25 O1 21.57(19) . . . . ? O1 Mg1 C26 C27 -41.45(17) . . . . ? N2 Mg1 C26 C27 81.08(17) . . . . ? N1 Mg1 C26 C27 -160.20(13) . . . . ? Mg1 C26 C27 C28 -63.7(2) . . . . ? C26 C27 C28 C29 -75.7(2) . . . . ? _diffrn_measured_fraction_theta_max 0.965 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.315 _refine_diff_density_min -0.249 _refine_diff_density_rms 0.048 data_sbjemma1 _database_code_depnum_ccdc_archive 'CCDC 916807' #TrackingRef 'All7.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H59 Mg N3' _chemical_formula_weight 582.19 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Mg Mg 0.0486 0.0363 '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' 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/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 9.0121(2) _cell_length_b 20.1333(5) _cell_length_c 19.8758(4) _cell_angle_alpha 90.00 _cell_angle_beta 91.504(2) _cell_angle_gamma 90.00 _cell_volume 3605.09(14) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 8431 _cell_measurement_theta_min 3.0283 _cell_measurement_theta_max 29.3850 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.073 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1280 _exptl_absorpt_coefficient_mu 0.077 _exptl_absorpt_correction_T_min 0.71637 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _diffrn_ambient_temperature 120(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 'Oxford diffraction Xcalibur E' _diffrn_measurement_method 'Omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20209 _diffrn_reflns_av_R_equivalents 0.0299 _diffrn_reflns_av_sigmaI/netI 0.0406 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 3.03 _diffrn_reflns_theta_max 27.00 _reflns_number_total 7869 _reflns_number_gt 6088 _reflns_threshold_expression I>2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _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^)+(0.0494P)^2^+1.2467P] 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 7869 _refine_ls_number_parameters 393 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0673 _refine_ls_R_factor_gt 0.0478 _refine_ls_wR_factor_ref 0.1216 _refine_ls_wR_factor_gt 0.1115 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.054 _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 1.19072(5) 0.24280(2) -0.13136(2) 0.01776(12) Uani 1 1 d . . . N1 N 1.10298(13) 0.16041(6) -0.08722(6) 0.0173(3) Uani 1 1 d . . . N2 N 1.08704(13) 0.30694(6) -0.06954(6) 0.0171(3) Uani 1 1 d . . . N3 N 1.32527(14) 0.25192(6) -0.20551(6) 0.0222(3) Uani 1 1 d . . . C1 C 0.99484(15) 0.16329(7) -0.04312(7) 0.0191(3) Uani 1 1 d . . . C2 C 0.92785(16) 0.22275(7) -0.02291(8) 0.0209(3) Uani 1 1 d . . . H2 H 0.8388 0.2175 0.0010 0.025 Uiso 1 1 calc R . . C3 C 0.97223(15) 0.28862(7) -0.03265(7) 0.0188(3) Uani 1 1 d . . . C4 C 1.17566(16) 0.09783(7) -0.09894(7) 0.0189(3) Uani 1 1 d . . . C5 C 1.31727(17) 0.08854(7) -0.06819(8) 0.0215(3) Uani 1 1 d . . . C6 C 1.39320(19) 0.02990(8) -0.08115(8) 0.0291(4) Uani 1 1 d . . . H6 H 1.4886 0.0229 -0.0610 0.035 Uiso 1 1 calc R . . C7 C 1.3322(2) -0.01824(9) -0.12284(9) 0.0337(4) Uani 1 1 d . . . H7 H 1.3852 -0.0582 -0.1307 0.040 Uiso 1 1 calc R . . C8 C 1.1946(2) -0.00845(8) -0.15301(9) 0.0318(4) Uani 1 1 d . . . H8 H 1.1539 -0.0419 -0.1818 0.038 Uiso 1 1 calc R . . C9 C 1.11373(18) 0.04951(7) -0.14221(8) 0.0241(3) Uani 1 1 d . . . C10 C 1.38269(17) 0.14030(8) -0.02039(8) 0.0244(3) Uani 1 1 d . . . H10 H 1.3504 0.1847 -0.0379 0.029 Uiso 1 1 calc R . . C13 C 1.13911(16) 0.37443(7) -0.06425(7) 0.0202(3) Uani 1 1 d . . . C14 C 1.25332(17) 0.38839(8) -0.01645(8) 0.0239(3) Uani 1 1 d . . . C15 C 1.31025(19) 0.45281(8) -0.01372(10) 0.0343(4) Uani 1 1 d . . . H15 H 1.3869 0.4633 0.0182 0.041 Uiso 1 1 calc R . . C16 C 1.2569(2) 0.50147(9) -0.05668(11) 0.0407(5) Uani 1 1 d . . . H16 H 1.2977 0.5449 -0.0543 0.049 Uiso 1 1 calc R . . C17 C 1.1449(2) 0.48749(8) -0.10302(10) 0.0366(4) Uani 1 1 d . . . H17 H 1.1088 0.5216 -0.1322 0.044 Uiso 1 1 calc R . . C18 C 1.08345(18) 0.42374(8) -0.10770(8) 0.0261(4) Uani 1 1 d . . . C19 C 1.31191(17) 0.33536(9) 0.03137(8) 0.0270(4) Uani 1 1 d . . . H19 H 1.2943 0.2914 0.0092 0.032 Uiso 1 1 calc R . . C20 C 1.2289(2) 0.33504(11) 0.09725(9) 0.0404(5) Uani 1 1 d . . . H20A H 1.2387 0.3786 0.1189 0.061 Uiso 1 1 calc R . . H20B H 1.2710 0.3008 0.1272 0.061 Uiso 1 1 calc R . . H20C H 1.1237 0.3255 0.0880 0.061 Uiso 1 1 calc R . . C21 C 1.47857(19) 0.34106(12) 0.04697(9) 0.0420(5) Uani 1 1 d . . . H21A H 1.5316 0.3461 0.0049 0.063 Uiso 1 1 calc R . . H21B H 1.5132 0.3009 0.0704 0.063 Uiso 1 1 calc R . . H21C H 1.4976 0.3799 0.0757 0.063 Uiso 1 1 calc R . . C22 C 0.9593(2) 0.41052(8) -0.15901(8) 0.0298(4) Uani 1 1 d . . . H22 H 0.9274 0.3632 -0.1540 0.036 Uiso 1 1 calc R . . C23 C 0.8239(2) 0.45495(10) -0.14789(10) 0.0430(5) Uani 1 1 d . . . H23A H 0.7926 0.4506 -0.1012 0.065 Uiso 1 1 calc R . . H23B H 0.7424 0.4413 -0.1785 0.065 Uiso 1 1 calc R . . H23C H 0.8500 0.5013 -0.1568 0.065 Uiso 1 1 calc R . . C24 C 1.0134(3) 0.41986(10) -0.23069(9) 0.0471(5) Uani 1 1 d . . . H24A H 1.0381 0.4667 -0.2379 0.071 Uiso 1 1 calc R . . H24B H 0.9350 0.4064 -0.2630 0.071 Uiso 1 1 calc R . . H24C H 1.1018 0.3925 -0.2372 0.071 Uiso 1 1 calc R . . C30 C 0.96306(19) 0.05737(8) -0.17793(9) 0.0310(4) Uani 1 1 d . . . H30 H 0.9214 0.1016 -0.1655 0.037 Uiso 1 1 calc R . . C31 C 0.9764(2) 0.05486(9) -0.25483(9) 0.0415(5) Uani 1 1 d . . . H31A H 1.0500 0.0875 -0.2689 0.062 Uiso 1 1 calc R . . H31B H 0.8799 0.0652 -0.2762 0.062 Uiso 1 1 calc R . . H31C H 1.0077 0.0103 -0.2683 0.062 Uiso 1 1 calc R . . C32 C 0.8531(2) 0.00330(9) -0.15669(10) 0.0414(5) Uani 1 1 d . . . H32A H 0.8864 -0.0400 -0.1730 0.062 Uiso 1 1 calc R . . H32B H 0.7544 0.0132 -0.1760 0.062 Uiso 1 1 calc R . . H32C H 0.8484 0.0023 -0.1075 0.062 Uiso 1 1 calc R . . C33 C 1.55220(18) 0.14081(10) -0.01677(9) 0.0352(4) Uani 1 1 d . . . H33A H 1.5881 0.0998 0.0046 0.053 Uiso 1 1 calc R . . H33B H 1.5867 0.1791 0.0097 0.053 Uiso 1 1 calc R . . H33C H 1.5905 0.1439 -0.0624 0.053 Uiso 1 1 calc R . . C34 C 1.32242(18) 0.13360(9) 0.05045(8) 0.0315(4) Uani 1 1 d . . . H34A H 1.2147 0.1405 0.0489 0.047 Uiso 1 1 calc R . . H34B H 1.3693 0.1669 0.0800 0.047 Uiso 1 1 calc R . . H34C H 1.3445 0.0891 0.0679 0.047 Uiso 1 1 calc R . . C35 C 0.93819(18) 0.10093(8) -0.00993(8) 0.0259(3) Uani 1 1 d . . . H35A H 0.8568 0.0821 -0.0375 0.039 Uiso 1 1 calc R . . H35B H 0.9021 0.1118 0.0348 0.039 Uiso 1 1 calc R . . H35C H 1.0189 0.0685 -0.0056 0.039 Uiso 1 1 calc R . . C36 C 0.88112(17) 0.34096(8) 0.00203(8) 0.0253(3) Uani 1 1 d . . . H36A H 0.9463 0.3770 0.0178 0.038 Uiso 1 1 calc R . . H36B H 0.8319 0.3211 0.0405 0.038 Uiso 1 1 calc R . . H36C H 0.8061 0.3587 -0.0297 0.038 Uiso 1 1 calc R . . C37 C 1.48119(18) 0.27252(8) -0.20164(8) 0.0259(3) Uani 1 1 d . . . C38 C 1.5134(2) 0.32599(9) -0.25477(8) 0.0318(4) Uani 1 1 d . . . H38A H 1.4634 0.3678 -0.2423 0.038 Uiso 1 1 calc R . . H38B H 1.6215 0.3346 -0.2549 0.038 Uiso 1 1 calc R . . C39 C 1.4607(2) 0.30547(9) -0.32512(8) 0.0332(4) Uani 1 1 d . . . H39A H 1.5190 0.2668 -0.3402 0.040 Uiso 1 1 calc R . . H39B H 1.4764 0.3425 -0.3570 0.040 Uiso 1 1 calc R . . C40 C 1.2964(2) 0.28738(8) -0.32499(8) 0.0306(4) Uani 1 1 d . . . H40A H 1.2656 0.2707 -0.3701 0.037 Uiso 1 1 calc R . . H40B H 1.2376 0.3278 -0.3158 0.037 Uiso 1 1 calc R . . C41 C 1.26202(19) 0.23410(8) -0.27188(8) 0.0259(3) Uani 1 1 d . . . C42 C 1.5067(2) 0.30350(9) -0.13203(8) 0.0332(4) Uani 1 1 d . . . H42A H 1.4386 0.3409 -0.1266 0.050 Uiso 1 1 calc R . . H42B H 1.6094 0.3193 -0.1276 0.050 Uiso 1 1 calc R . . H42C H 1.4885 0.2701 -0.0973 0.050 Uiso 1 1 calc R . . C43 C 1.5941(2) 0.21495(9) -0.20744(10) 0.0371(4) Uani 1 1 d . . . H43A H 1.5636 0.1778 -0.1791 0.056 Uiso 1 1 calc R . . H43B H 1.6927 0.2303 -0.1925 0.056 Uiso 1 1 calc R . . H43C H 1.5974 0.2003 -0.2544 0.056 Uiso 1 1 calc R . . C44 C 1.3112(2) 0.16502(8) -0.29777(9) 0.0345(4) Uani 1 1 d . . . H44A H 1.4143 0.1674 -0.3121 0.052 Uiso 1 1 calc R . . H44B H 1.2470 0.1518 -0.3360 0.052 Uiso 1 1 calc R . . H44C H 1.3034 0.1323 -0.2616 0.052 Uiso 1 1 calc R . . C45 C 1.09342(19) 0.23162(9) -0.26394(8) 0.0322(4) Uani 1 1 d . . . H45A H 1.0689 0.1973 -0.2311 0.048 Uiso 1 1 calc R . . H45B H 1.0453 0.2212 -0.3074 0.048 Uiso 1 1 calc R . . H45C H 1.0583 0.2748 -0.2482 0.048 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 0.0194(2) 0.0157(2) 0.0183(2) 0.0002(2) 0.00298(19) -0.00082(19) N1 0.0165(6) 0.0159(6) 0.0194(6) 0.0011(5) -0.0020(5) -0.0016(5) N2 0.0152(6) 0.0162(6) 0.0198(6) -0.0009(5) 0.0004(5) -0.0011(5) N3 0.0256(7) 0.0219(7) 0.0192(6) -0.0012(5) 0.0060(5) -0.0033(5) C1 0.0143(7) 0.0209(7) 0.0220(7) 0.0018(6) -0.0034(5) -0.0045(6) C2 0.0144(7) 0.0239(8) 0.0246(8) 0.0010(6) 0.0027(6) -0.0027(6) C3 0.0141(7) 0.0229(8) 0.0192(7) -0.0001(6) -0.0025(5) 0.0004(6) C4 0.0207(7) 0.0157(7) 0.0203(7) 0.0035(6) 0.0015(6) -0.0012(6) C5 0.0218(7) 0.0200(8) 0.0229(7) 0.0044(6) 0.0016(6) 0.0004(6) C6 0.0280(9) 0.0316(9) 0.0278(8) 0.0044(7) 0.0021(7) 0.0089(7) C7 0.0469(11) 0.0254(9) 0.0289(9) 0.0003(7) 0.0036(8) 0.0141(8) C8 0.0480(11) 0.0200(8) 0.0271(8) -0.0031(7) -0.0023(7) 0.0012(8) C9 0.0305(8) 0.0179(7) 0.0237(8) 0.0028(6) -0.0020(6) -0.0031(6) C10 0.0194(7) 0.0222(8) 0.0312(8) 0.0044(7) -0.0058(6) -0.0008(6) C13 0.0201(7) 0.0173(7) 0.0237(8) -0.0038(6) 0.0069(6) -0.0010(6) C14 0.0188(7) 0.0238(8) 0.0294(8) -0.0076(7) 0.0073(6) -0.0025(6) C15 0.0256(9) 0.0285(9) 0.0493(11) -0.0153(8) 0.0078(8) -0.0084(7) C16 0.0404(11) 0.0182(8) 0.0644(13) -0.0084(9) 0.0162(9) -0.0092(8) C17 0.0442(11) 0.0183(8) 0.0480(11) 0.0032(8) 0.0136(9) 0.0017(8) C18 0.0304(9) 0.0189(8) 0.0296(9) 0.0001(7) 0.0098(7) 0.0031(7) C19 0.0191(8) 0.0320(9) 0.0298(8) -0.0071(7) -0.0040(6) -0.0029(7) C20 0.0286(9) 0.0541(12) 0.0386(10) 0.0056(9) 0.0044(8) -0.0038(9) C21 0.0223(9) 0.0716(14) 0.0319(9) -0.0015(10) -0.0030(7) -0.0042(9) C22 0.0393(10) 0.0223(8) 0.0280(9) 0.0040(7) 0.0013(7) 0.0085(7) C23 0.0443(11) 0.0399(11) 0.0446(11) 0.0020(9) -0.0029(9) 0.0167(9) C24 0.0707(15) 0.0388(11) 0.0322(10) 0.0038(9) 0.0080(10) 0.0112(10) C30 0.0340(9) 0.0215(8) 0.0366(9) -0.0003(7) -0.0117(7) -0.0066(7) C31 0.0546(12) 0.0319(10) 0.0370(10) 0.0027(8) -0.0186(9) -0.0146(9) C32 0.0414(11) 0.0347(10) 0.0477(11) -0.0027(9) -0.0065(9) -0.0136(9) C33 0.0205(8) 0.0418(10) 0.0430(10) 0.0127(9) -0.0053(7) -0.0035(8) C34 0.0253(8) 0.0371(10) 0.0318(9) -0.0055(8) -0.0047(7) -0.0017(7) C35 0.0227(8) 0.0227(8) 0.0326(9) 0.0044(7) 0.0040(6) -0.0038(6) C36 0.0213(8) 0.0244(8) 0.0307(8) -0.0026(7) 0.0066(6) 0.0008(6) C37 0.0260(8) 0.0281(9) 0.0241(8) 0.0015(7) 0.0082(6) -0.0026(7) C38 0.0358(10) 0.0274(9) 0.0329(9) 0.0020(7) 0.0125(7) -0.0068(7) C39 0.0458(11) 0.0271(9) 0.0275(9) 0.0053(7) 0.0148(8) 0.0002(8) C40 0.0439(10) 0.0268(9) 0.0215(8) 0.0010(7) 0.0056(7) 0.0022(8) C41 0.0337(9) 0.0242(8) 0.0202(7) -0.0016(7) 0.0060(6) -0.0015(7) C42 0.0314(9) 0.0395(10) 0.0288(9) -0.0007(8) 0.0044(7) -0.0095(8) C43 0.0334(10) 0.0413(10) 0.0371(10) 0.0051(9) 0.0085(8) 0.0063(8) C44 0.0493(11) 0.0257(9) 0.0290(9) -0.0057(7) 0.0071(8) -0.0022(8) C45 0.0364(10) 0.0350(10) 0.0250(8) -0.0025(7) -0.0012(7) -0.0059(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 N3 1.9417(13) . ? Mg1 N2 2.0273(13) . ? Mg1 N1 2.0451(13) . ? N1 C1 1.3291(19) . ? N1 C4 1.4418(18) . ? N2 C3 1.3357(18) . ? N2 C13 1.4406(18) . ? N3 C37 1.465(2) . ? N3 C41 1.468(2) . ? C1 C2 1.404(2) . ? C1 C35 1.513(2) . ? C2 C3 1.400(2) . ? C2 H2 0.9500 . ? C3 C36 1.513(2) . ? C4 C9 1.404(2) . ? C4 C5 1.413(2) . ? C5 C6 1.392(2) . ? C5 C10 1.519(2) . ? C6 C7 1.380(2) . ? C6 H6 0.9500 . ? C7 C8 1.378(3) . ? C7 H7 0.9500 . ? C8 C9 1.395(2) . ? C8 H8 0.9500 . ? C9 C30 1.524(2) . ? C10 C33 1.527(2) . ? C10 C34 1.528(2) . ? C10 H10 1.0000 . ? C13 C18 1.400(2) . ? C13 C14 1.411(2) . ? C14 C15 1.395(2) . ? C14 C19 1.515(2) . ? C15 C16 1.378(3) . ? C15 H15 0.9500 . ? C16 C17 1.378(3) . ? C16 H16 0.9500 . ? C17 C18 1.400(2) . ? C17 H17 0.9500 . ? C18 C22 1.518(2) . ? C19 C20 1.525(2) . ? C19 C21 1.530(2) . ? C19 H19 1.0000 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 C24 1.530(2) . ? C22 C23 1.534(2) . ? C22 H22 1.0000 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C30 C31 1.537(3) . ? C30 C32 1.539(2) . ? C30 H30 1.0000 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 C42 1.529(2) . ? C37 C38 1.541(2) . ? C37 C43 1.549(2) . ? C38 C39 1.522(2) . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C39 C40 1.525(2) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 C41 1.542(2) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 C45 1.533(2) . ? C41 C44 1.552(2) . ? 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 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 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 N3 Mg1 N2 134.97(6) . . ? N3 Mg1 N1 131.18(6) . . ? N2 Mg1 N1 93.85(5) . . ? C1 N1 C4 119.26(12) . . ? C1 N1 Mg1 123.09(10) . . ? C4 N1 Mg1 117.20(9) . . ? C3 N2 C13 118.42(12) . . ? C3 N2 Mg1 122.19(10) . . ? C13 N2 Mg1 119.38(9) . . ? C37 N3 C41 117.75(12) . . ? C37 N3 Mg1 127.16(10) . . ? C41 N3 Mg1 115.06(10) . . ? N1 C1 C2 123.64(13) . . ? N1 C1 C35 120.86(13) . . ? C2 C1 C35 115.48(13) . . ? C3 C2 C1 129.90(13) . . ? C3 C2 H2 115.0 . . ? C1 C2 H2 115.0 . . ? N2 C3 C2 124.45(13) . . ? N2 C3 C36 119.68(13) . . ? C2 C3 C36 115.87(13) . . ? C9 C4 C5 120.87(14) . . ? C9 C4 N1 121.96(13) . . ? C5 C4 N1 117.06(13) . . ? C6 C5 C4 118.37(14) . . ? C6 C5 C10 120.87(14) . . ? C4 C5 C10 120.74(13) . . ? C7 C6 C5 121.12(16) . . ? C7 C6 H6 119.4 . . ? C5 C6 H6 119.4 . . ? C8 C7 C6 120.06(15) . . ? C8 C7 H7 120.0 . . ? C6 C7 H7 120.0 . . ? C7 C8 C9 121.36(16) . . ? C7 C8 H8 119.3 . . ? C9 C8 H8 119.3 . . ? C8 C9 C4 118.22(15) . . ? C8 C9 C30 118.53(15) . . ? C4 C9 C30 123.25(14) . . ? C5 C10 C33 113.91(14) . . ? C5 C10 C34 111.98(13) . . ? C33 C10 C34 109.66(13) . . ? C5 C10 H10 107.0 . . ? C33 C10 H10 107.0 . . ? C34 C10 H10 107.0 . . ? C18 C13 C14 121.16(14) . . ? C18 C13 N2 120.87(14) . . ? C14 C13 N2 117.88(13) . . ? C15 C14 C13 118.19(16) . . ? C15 C14 C19 120.59(15) . . ? C13 C14 C19 121.22(14) . . ? C16 C15 C14 120.99(17) . . ? C16 C15 H15 119.5 . . ? C14 C15 H15 119.5 . . ? C15 C16 C17 120.44(16) . . ? C15 C16 H16 119.8 . . ? C17 C16 H16 119.8 . . ? C16 C17 C18 120.88(17) . . ? C16 C17 H17 119.6 . . ? C18 C17 H17 119.6 . . ? C17 C18 C13 118.32(16) . . ? C17 C18 C22 119.26(16) . . ? C13 C18 C22 122.42(14) . . ? C14 C19 C20 111.78(14) . . ? C14 C19 C21 113.48(14) . . ? C20 C19 C21 109.11(14) . . ? C14 C19 H19 107.4 . . ? C20 C19 H19 107.4 . . ? C21 C19 H19 107.4 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C18 C22 C24 110.90(16) . . ? C18 C22 C23 112.11(14) . . ? C24 C22 C23 109.69(15) . . ? C18 C22 H22 108.0 . . ? C24 C22 H22 108.0 . . ? C23 C22 H22 108.0 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C9 C30 C31 111.58(15) . . ? C9 C30 C32 111.79(14) . . ? C31 C30 C32 108.50(14) . . ? C9 C30 H30 108.3 . . ? C31 C30 H30 108.3 . . ? C32 C30 H30 108.3 . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C30 C32 H32A 109.5 . . ? C30 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C30 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C10 C33 H33A 109.5 . . ? C10 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C10 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C10 C34 H34A 109.5 . . ? C10 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C10 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C1 C35 H35A 109.5 . . ? C1 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C1 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C3 C36 H36A 109.5 . . ? C3 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C3 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? N3 C37 C42 106.52(12) . . ? N3 C37 C38 111.06(13) . . ? C42 C37 C38 107.97(14) . . ? N3 C37 C43 114.53(14) . . ? C42 C37 C43 106.79(14) . . ? C38 C37 C43 109.63(13) . . ? C39 C38 C37 112.35(14) . . ? C39 C38 H38A 109.1 . . ? C37 C38 H38A 109.1 . . ? C39 C38 H38B 109.1 . . ? C37 C38 H38B 109.1 . . ? H38A C38 H38B 107.9 . . ? C38 C39 C40 110.05(13) . . ? C38 C39 H39A 109.6 . . ? C40 C39 H39A 109.6 . . ? C38 C39 H39B 109.6 . . ? C40 C39 H39B 109.6 . . ? H39A C39 H39B 108.2 . . ? C39 C40 C41 112.31(14) . . ? C39 C40 H40A 109.1 . . ? C41 C40 H40A 109.1 . . ? C39 C40 H40B 109.1 . . ? C41 C40 H40B 109.1 . . ? H40A C40 H40B 107.9 . . ? N3 C41 C45 106.15(12) . . ? N3 C41 C40 111.41(13) . . ? C45 C41 C40 108.09(14) . . ? N3 C41 C44 114.18(14) . . ? C45 C41 C44 107.30(14) . . ? C40 C41 C44 109.41(13) . . ? C37 C42 H42A 109.5 . . ? C37 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C37 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C37 C43 H43A 109.5 . . ? C37 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C37 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C41 C44 H44A 109.5 . . ? C41 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C41 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C41 C45 H45A 109.5 . . ? C41 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C41 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N3 Mg1 N1 C1 -169.70(11) . . . . ? N2 Mg1 N1 C1 10.56(12) . . . . ? N3 Mg1 N1 C4 18.07(13) . . . . ? N2 Mg1 N1 C4 -161.66(10) . . . . ? N3 Mg1 N2 C3 163.64(11) . . . . ? N1 Mg1 N2 C3 -16.64(12) . . . . ? N3 Mg1 N2 C13 -17.10(14) . . . . ? N1 Mg1 N2 C13 162.62(10) . . . . ? N2 Mg1 N3 C37 71.12(15) . . . . ? N1 Mg1 N3 C37 -108.51(13) . . . . ? N2 Mg1 N3 C41 -110.71(11) . . . . ? N1 Mg1 N3 C41 69.66(13) . . . . ? C4 N1 C1 C2 173.10(13) . . . . ? Mg1 N1 C1 C2 1.0(2) . . . . ? C4 N1 C1 C35 -5.5(2) . . . . ? Mg1 N1 C1 C35 -177.58(10) . . . . ? N1 C1 C2 C3 -13.0(2) . . . . ? C35 C1 C2 C3 165.71(15) . . . . ? C13 N2 C3 C2 -167.43(13) . . . . ? Mg1 N2 C3 C2 11.8(2) . . . . ? C13 N2 C3 C36 12.4(2) . . . . ? Mg1 N2 C3 C36 -168.35(10) . . . . ? C1 C2 C3 N2 5.6(3) . . . . ? C1 C2 C3 C36 -174.18(15) . . . . ? C1 N1 C4 C9 81.37(18) . . . . ? Mg1 N1 C4 C9 -106.09(14) . . . . ? C1 N1 C4 C5 -102.47(16) . . . . ? Mg1 N1 C4 C5 70.07(15) . . . . ? C9 C4 C5 C6 -0.8(2) . . . . ? N1 C4 C5 C6 -177.01(13) . . . . ? C9 C4 C5 C10 -178.84(14) . . . . ? N1 C4 C5 C10 5.0(2) . . . . ? C4 C5 C6 C7 -0.1(2) . . . . ? C10 C5 C6 C7 177.89(15) . . . . ? C5 C6 C7 C8 0.7(3) . . . . ? C6 C7 C8 C9 -0.3(3) . . . . ? C7 C8 C9 C4 -0.7(2) . . . . ? C7 C8 C9 C30 179.24(16) . . . . ? C5 C4 C9 C8 1.2(2) . . . . ? N1 C4 C9 C8 177.21(14) . . . . ? C5 C4 C9 C30 -178.70(14) . . . . ? N1 C4 C9 C30 -2.7(2) . . . . ? C6 C5 C10 C33 28.5(2) . . . . ? C4 C5 C10 C33 -153.50(14) . . . . ? C6 C5 C10 C34 -96.64(17) . . . . ? C4 C5 C10 C34 81.35(18) . . . . ? C3 N2 C13 C18 -91.52(17) . . . . ? Mg1 N2 C13 C18 89.20(15) . . . . ? C3 N2 C13 C14 91.82(16) . . . . ? Mg1 N2 C13 C14 -87.46(14) . . . . ? C18 C13 C14 C15 -0.3(2) . . . . ? N2 C13 C14 C15 176.35(13) . . . . ? C18 C13 C14 C19 178.98(14) . . . . ? N2 C13 C14 C19 -4.4(2) . . . . ? C13 C14 C15 C16 -0.3(2) . . . . ? C19 C14 C15 C16 -179.54(15) . . . . ? C14 C15 C16 C17 0.6(3) . . . . ? C15 C16 C17 C18 -0.3(3) . . . . ? C16 C17 C18 C13 -0.2(3) . . . . ? C16 C17 C18 C22 179.49(16) . . . . ? C14 C13 C18 C17 0.5(2) . . . . ? N2 C13 C18 C17 -176.02(14) . . . . ? C14 C13 C18 C22 -179.16(14) . . . . ? N2 C13 C18 C22 4.3(2) . . . . ? C15 C14 C19 C20 87.85(18) . . . . ? C13 C14 C19 C20 -91.41(18) . . . . ? C15 C14 C19 C21 -36.1(2) . . . . ? C13 C14 C19 C21 144.67(15) . . . . ? C17 C18 C22 C24 63.8(2) . . . . ? C13 C18 C22 C24 -116.55(17) . . . . ? C17 C18 C22 C23 -59.2(2) . . . . ? C13 C18 C22 C23 120.46(17) . . . . ? C8 C9 C30 C31 -59.8(2) . . . . ? C4 C9 C30 C31 120.09(17) . . . . ? C8 C9 C30 C32 61.9(2) . . . . ? C4 C9 C30 C32 -118.20(17) . . . . ? C41 N3 C37 C42 166.77(13) . . . . ? Mg1 N3 C37 C42 -15.10(18) . . . . ? C41 N3 C37 C38 49.44(18) . . . . ? Mg1 N3 C37 C38 -132.43(12) . . . . ? C41 N3 C37 C43 -75.41(18) . . . . ? Mg1 N3 C37 C43 102.72(15) . . . . ? N3 C37 C38 C39 -51.48(18) . . . . ? C42 C37 C38 C39 -167.92(15) . . . . ? C43 C37 C38 C39 76.09(18) . . . . ? C37 C38 C39 C40 54.98(19) . . . . ? C38 C39 C40 C41 -54.32(19) . . . . ? C37 N3 C41 C45 -166.44(13) . . . . ? Mg1 N3 C41 C45 15.20(15) . . . . ? C37 N3 C41 C40 -49.00(18) . . . . ? Mg1 N3 C41 C40 132.64(12) . . . . ? C37 N3 C41 C44 75.57(17) . . . . ? Mg1 N3 C41 C44 -102.79(13) . . . . ? C39 C40 C41 N3 50.35(18) . . . . ? C39 C40 C41 C45 166.60(14) . . . . ? C39 C40 C41 C44 -76.85(18) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.332 _refine_diff_density_min -0.207 _refine_diff_density_rms 0.042 data_eh8 _database_code_depnum_ccdc_archive 'CCDC 916808' #TrackingRef 'All7.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C40 H53 Mg N3 O2' _chemical_formula_sum 'C40 H53 Mg N3 O2' _chemical_formula_weight 632.16 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 0.0000 '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 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mg Mg 0.0419 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M 'R 3 m' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-y, -x, z' '-x+y, y, z' 'x, x-y, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' '-y+2/3, -x+1/3, z+1/3' '-x+y+2/3, y+1/3, z+1/3' 'x+2/3, x-y+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-y+1/3, -x+2/3, z+2/3' '-x+y+1/3, y+2/3, z+2/3' 'x+1/3, x-y+2/3, z+2/3' _cell_length_a 32.394(6) _cell_length_b 32.394(6) _cell_length_c 11.017(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 10012(3) _cell_formula_units_Z 9 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9875 _cell_measurement_theta_min 2.44 _cell_measurement_theta_max 23.96 _exptl_crystal_description rod _exptl_crystal_colour colourless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.944 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3078 _exptl_absorpt_coefficient_mu 0.069 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.990 _exptl_absorpt_correction_T_max 0.999 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.6889 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'Diamond beamline I19' _diffrn_radiation_monochromator 'silicon double crystal' _diffrn_measurement_device_type 'Crystal Logic diffractometer and Rigaku Saturn 724+ CCD' _diffrn_measurement_method 'thick-slice \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 23375 _diffrn_reflns_av_R_equivalents 0.0588 _diffrn_reflns_av_sigmaI/netI 0.0270 _diffrn_reflns_limit_h_min -38 _diffrn_reflns_limit_h_max 38 _diffrn_reflns_limit_k_min -38 _diffrn_reflns_limit_k_max 38 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 3.55 _diffrn_reflns_theta_max 24.01 _reflns_number_total 1967 _reflns_number_gt 1919 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Rigaku CrystalClear' _computing_cell_refinement 'Bruker APEX2' _computing_data_reduction 'Bruker APEX2' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL and local programs' _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^)+(0.1634P)^2^+0.9982P] 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 0.46(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 1967 _refine_ls_number_parameters 232 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0759 _refine_ls_R_factor_gt 0.0751 _refine_ls_wR_factor_ref 0.1877 _refine_ls_wR_factor_gt 0.1859 _refine_ls_goodness_of_fit_ref 1.112 _refine_ls_restrained_S_all 1.111 _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 Mg Mg 0.79222(3) 0.20778(3) 0.74992(13) 0.0405(6) Uani 1 2 d S . . O1 O 0.78818(8) 0.21182(8) 0.5819(4) 0.0565(10) Uani 1 2 d S . . O2 O 0.82806(6) 0.17194(6) 0.7460(3) 0.0489(10) Uani 1 2 d S . . N1 N 0.73079(10) 0.17613(10) 0.8485(3) 0.0423(8) Uani 1 1 d . . . N2 N 0.80776(13) 0.19224(13) 0.3558(5) 0.0749(16) Uani 1 2 d S . . C1 C 0.74794(9) 0.25206(9) 0.9326(5) 0.0468(11) Uani 1 2 d S . . H1 H 0.7324 0.2676 0.9664 0.056 Uiso 1 2 calc SR . . C2 C 0.71826(11) 0.20307(12) 0.9117(3) 0.0442(9) Uani 1 1 d . . . C3 C 0.66941(15) 0.18112(15) 0.9692(5) 0.0630(12) Uani 1 1 d . . . H3A H 0.6452 0.1606 0.9099 0.095 Uiso 1 1 calc R . . H3B H 0.6632 0.2064 0.9952 0.095 Uiso 1 1 calc R . . H3C H 0.6681 0.1621 1.0397 0.095 Uiso 1 1 calc R . . C4 C 0.69888(12) 0.12595(12) 0.8427(3) 0.0457(9) Uani 1 1 d . . . C5 C 0.69844(13) 0.09641(13) 0.9404(4) 0.0528(10) Uani 1 1 d . . . C6 C 0.66878(17) 0.04728(14) 0.9285(5) 0.0659(12) Uani 1 1 d . . . H6 H 0.6680 0.0269 0.9916 0.079 Uiso 1 1 calc R . . C7 C 0.64084(17) 0.02767(15) 0.8281(6) 0.0745(15) Uani 1 1 d . . . H7 H 0.6207 -0.0059 0.8232 0.089 Uiso 1 1 calc R . . C8 C 0.64157(15) 0.05564(16) 0.7356(5) 0.0654(12) Uani 1 1 d . . . H8 H 0.6221 0.0412 0.6664 0.079 Uiso 1 1 calc R . . C9 C 0.67029(12) 0.10518(13) 0.7398(4) 0.0518(10) Uani 1 1 d . . . C10 C 0.72935(17) 0.11730(15) 1.0526(4) 0.0600(11) Uani 1 1 d . . . H10 H 0.7426 0.1526 1.0521 0.072 Uiso 1 1 calc R . . C11 C 0.7003(3) 0.0969(2) 1.1695(6) 0.0884(18) Uani 1 1 d . . . H11A H 0.6782 0.1090 1.1792 0.133 Uiso 1 1 calc R . . H11B H 0.7220 0.1067 1.2392 0.133 Uiso 1 1 calc R . . H11C H 0.6823 0.0621 1.1646 0.133 Uiso 1 1 calc R . . C12 C 0.7713(2) 0.1076(2) 1.0486(5) 0.0832(15) Uani 1 1 d . . . H12A H 0.7900 0.1216 0.9746 0.125 Uiso 1 1 calc R . . H12B H 0.7590 0.0732 1.0490 0.125 Uiso 1 1 calc R . . H12C H 0.7917 0.1220 1.1198 0.125 Uiso 1 1 calc R . . C13 C 0.66782(14) 0.13546(16) 0.6377(4) 0.0571(10) Uani 1 1 d . . . H13 H 0.6927 0.1694 0.6527 0.068 Uiso 1 1 calc R . . C14 C 0.6192(2) 0.1322(3) 0.6380(7) 0.0874(17) Uani 1 1 d . . . H14A H 0.6184 0.1531 0.5750 0.131 Uiso 1 1 calc R . . H14B H 0.6136 0.1420 0.7175 0.131 Uiso 1 1 calc R . . H14C H 0.5943 0.0992 0.6216 0.131 Uiso 1 1 calc R . . C15 C 0.67762(16) 0.12071(17) 0.5148(4) 0.0658(12) Uani 1 1 d . . . H15A H 0.7083 0.1217 0.5172 0.099 Uiso 1 1 calc R . . H15B H 0.6786 0.1427 0.4522 0.099 Uiso 1 1 calc R . . H15C H 0.6523 0.0883 0.4957 0.099 Uiso 1 1 calc R . . C16 C 0.77390(12) 0.22610(12) 0.4889(5) 0.0565(13) Uani 1 2 d S . . C17 C 0.74931(14) 0.25069(14) 0.4978(6) 0.0680(16) Uani 1 2 d S . . H17 H 0.7423 0.2577 0.5763 0.082 Uiso 1 2 calc SR . . C18 C 0.73450(15) 0.26550(15) 0.3984(8) 0.081(2) Uani 1 2 d S . . H18 H 0.7177 0.2823 0.4083 0.097 Uiso 1 2 calc SR . . C19 C 0.7446(2) 0.2554(2) 0.2823(8) 0.093(3) Uani 1 2 d S . . H19 H 0.7346 0.2654 0.2131 0.111 Uiso 1 2 calc SR . . C20 C 0.76839(17) 0.23161(17) 0.2672(6) 0.0751(19) Uani 1 2 d S . . H20 H 0.7751 0.2249 0.1880 0.090 Uiso 1 2 calc SR . . C21 C 0.78320(15) 0.21680(15) 0.3696(6) 0.0647(16) Uani 1 2 d S . . C22 C 0.8279(2) 0.1721(2) 0.3462(9) 0.122(4) Uani 1 2 d S . . C23 C 0.80327(19) 0.12410(17) 0.6933(6) 0.0745(14) Uani 1 1 d . . . H23B H 0.7881 0.0999 0.7580 0.112 Uiso 1 1 calc R . . H23A H 0.7782 0.1210 0.6364 0.112 Uiso 1 1 calc R . . C24 C 0.8386(3) 0.1174(3) 0.6297(8) 0.104(2) Uani 1 1 d . . . H24A H 0.8427 0.0925 0.6704 0.125 Uiso 1 1 calc R . . H24B H 0.8281 0.1071 0.5452 0.125 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mg 0.0366(7) 0.0366(7) 0.0458(9) -0.0018(3) 0.0018(3) 0.0165(6) O1 0.0571(16) 0.0571(16) 0.0474(19) 0.0020(8) -0.0020(8) 0.0227(18) O2 0.0451(14) 0.0451(14) 0.056(2) -0.0025(7) 0.0025(7) 0.0218(15) N1 0.0390(14) 0.0371(14) 0.0510(15) 0.0005(11) 0.0036(11) 0.0191(11) N2 0.089(3) 0.089(3) 0.047(3) -0.0034(13) 0.0034(13) 0.045(4) C1 0.0430(18) 0.0430(18) 0.055(3) -0.0063(9) 0.0063(9) 0.022(2) C2 0.0364(16) 0.0438(17) 0.0537(19) 0.0018(13) 0.0047(13) 0.0211(14) C3 0.046(2) 0.049(2) 0.089(3) 0.0008(19) 0.0198(19) 0.0202(17) C4 0.0329(15) 0.0357(16) 0.065(2) -0.0001(14) 0.0088(13) 0.0144(12) C5 0.049(2) 0.0417(18) 0.065(2) 0.0052(15) 0.0105(16) 0.0208(16) C6 0.068(2) 0.0403(19) 0.085(3) 0.0083(19) 0.022(2) 0.0230(18) C7 0.061(2) 0.0365(19) 0.110(4) -0.006(2) 0.027(3) 0.0126(18) C8 0.045(2) 0.048(2) 0.090(3) -0.014(2) 0.0095(19) 0.0132(17) C9 0.0362(16) 0.0468(19) 0.070(2) -0.0096(16) 0.0041(15) 0.0191(15) C10 0.066(2) 0.046(2) 0.066(2) 0.0111(16) 0.0084(19) 0.0259(18) C11 0.109(4) 0.075(3) 0.075(3) 0.014(2) 0.027(3) 0.042(3) C12 0.089(3) 0.102(4) 0.072(3) 0.010(3) 0.004(3) 0.057(3) C13 0.0429(18) 0.061(2) 0.071(2) -0.0149(18) -0.0088(16) 0.0291(16) C14 0.063(3) 0.117(5) 0.101(4) -0.004(3) -0.004(3) 0.059(3) C15 0.059(2) 0.064(2) 0.069(3) -0.019(2) -0.0091(19) 0.0267(19) C16 0.0505(19) 0.0505(19) 0.055(3) 0.0016(13) -0.0016(13) 0.015(2) C17 0.067(3) 0.067(3) 0.060(3) 0.0033(15) -0.0033(15) 0.027(3) C18 0.081(3) 0.081(3) 0.082(5) 0.0064(18) -0.0064(18) 0.042(4) C19 0.100(4) 0.100(4) 0.069(5) 0.013(2) -0.013(2) 0.044(5) C20 0.080(3) 0.080(3) 0.052(3) 0.0021(16) -0.0021(16) 0.030(4) C21 0.064(2) 0.064(2) 0.050(3) 0.0013(14) -0.0013(14) 0.019(3) C22 0.176(10) 0.176(10) 0.062(5) -0.015(2) 0.015(2) 0.123(11) C23 0.074(3) 0.047(2) 0.104(4) -0.024(2) -0.005(3) 0.031(2) C24 0.130(6) 0.095(4) 0.107(5) -0.029(3) 0.009(4) 0.072(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mg O1 1.865(4) . ? Mg O2 2.011(4) . ? Mg N1 2.037(3) . ? Mg N1 2.037(3) 4_665 ? O1 C16 1.300(8) . ? O2 C23 1.462(5) . ? O2 C23 1.462(5) 4_665 ? N1 C2 1.329(5) . ? N1 C4 1.426(4) . ? N2 C21 1.386(11) . ? N2 C22 1.132(14) . ? C1 H1 0.950 . ? C1 C2 1.404(4) . ? C1 C2 1.404(4) 4_665 ? C2 C3 1.512(5) . ? C3 H3A 0.980 . ? C3 H3B 0.980 . ? C3 H3C 0.980 . ? C4 C5 1.436(6) . ? C4 C9 1.404(6) . ? C5 C6 1.394(5) . ? C5 C10 1.520(7) . ? C6 H6 0.950 . ? C6 C7 1.368(9) . ? C7 H7 0.950 . ? C7 C8 1.356(9) . ? C8 H8 0.950 . ? C8 C9 1.397(6) . ? C9 C13 1.521(7) . ? C10 H10 1.000 . ? C10 C11 1.536(7) . ? C10 C12 1.540(8) . ? C11 H11A 0.980 . ? C11 H11B 0.980 . ? C11 H11C 0.980 . ? C12 H12A 0.980 . ? C12 H12B 0.980 . ? C12 H12C 0.980 . ? C13 H13 1.000 . ? C13 C14 1.524(6) . ? C13 C15 1.521(6) . ? C14 H14A 0.980 . ? C14 H14B 0.980 . ? C14 H14C 0.980 . ? C15 H15A 0.980 . ? C15 H15B 0.980 . ? C15 H15C 0.980 . ? C16 C17 1.384(10) . ? C16 C21 1.414(9) . ? C17 H17 0.950 . ? C17 C18 1.374(11) . ? C18 H18 0.950 . ? C18 C19 1.400(14) . ? C19 H19 0.950 . ? C19 C20 1.343(15) . ? C20 H20 0.950 . ? C20 C21 1.401(11) . ? C23 H23B 0.990 . ? C23 H23A 0.990 . ? C23 C24 1.448(8) . ? C24 C24 1.424(17) 4_665 ? C24 H24A 0.990 . ? C24 H24B 0.990 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Mg O2 95.73(18) . . ? O1 Mg N1 118.64(12) . . ? O1 Mg N1 118.64(12) . 4_665 ? O2 Mg N1 114.93(11) . . ? O2 Mg N1 114.93(11) . 4_665 ? N1 Mg N1 95.48(17) . 4_665 ? Mg O1 C16 149.0(4) . . ? Mg O2 C23 116.8(2) . . ? Mg O2 C23 116.8(2) . 4_665 ? C23 O2 C23 107.1(5) . 4_665 ? Mg N1 C2 119.4(2) . . ? Mg N1 C4 121.2(2) . . ? C2 N1 C4 119.1(3) . . ? C21 N2 C22 179.1(8) . . ? H1 C1 C2 114.8 . . ? H1 C1 C2 114.8 . 4_665 ? C2 C1 C2 130.4(4) . 4_665 ? N1 C2 C1 124.6(3) . . ? N1 C2 C3 120.1(3) . . ? C1 C2 C3 115.3(3) . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3B 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? N1 C4 C5 119.1(3) . . ? N1 C4 C9 120.7(3) . . ? C5 C4 C9 120.1(3) . . ? C4 C5 C6 117.5(4) . . ? C4 C5 C10 121.9(3) . . ? C6 C5 C10 120.6(4) . . ? C5 C6 H6 119.2 . . ? C5 C6 C7 121.6(5) . . ? H6 C6 C7 119.2 . . ? C6 C7 H7 119.6 . . ? C6 C7 C8 120.7(4) . . ? H7 C7 C8 119.6 . . ? C7 C8 H8 119.3 . . ? C7 C8 C9 121.5(5) . . ? H8 C8 C9 119.3 . . ? C4 C9 C8 118.6(4) . . ? C4 C9 C13 121.5(3) . . ? C8 C9 C13 119.8(4) . . ? C5 C10 H10 108.4 . . ? C5 C10 C11 111.4(5) . . ? C5 C10 C12 109.8(4) . . ? H10 C10 C11 108.4 . . ? H10 C10 C12 108.4 . . ? C11 C10 C12 110.4(5) . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11B 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12B 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C9 C13 H13 108.2 . . ? C9 C13 C14 109.8(4) . . ? C9 C13 C15 111.7(4) . . ? H13 C13 C14 108.2 . . ? H13 C13 C15 108.2 . . ? C14 C13 C15 110.5(4) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14B 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15B 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? O1 C16 C17 124.0(6) . . ? O1 C16 C21 120.3(6) . . ? C17 C16 C21 115.7(6) . . ? C16 C17 H17 118.4 . . ? C16 C17 C18 123.1(7) . . ? H17 C17 C18 118.4 . . ? C17 C18 H18 120.6 . . ? C17 C18 C19 118.8(8) . . ? H18 C18 C19 120.6 . . ? C18 C19 H19 119.4 . . ? C18 C19 C20 121.1(8) . . ? H19 C19 C20 119.4 . . ? C19 C20 H20 120.4 . . ? C19 C20 C21 119.3(7) . . ? H20 C20 C21 120.4 . . ? N2 C21 C16 117.9(6) . . ? N2 C21 C20 120.1(6) . . ? C16 C21 C20 122.0(8) . . ? O2 C23 H23B 110.3 . . ? O2 C23 H23A 110.3 . . ? O2 C23 C24 107.1(5) . . ? H23B C23 H23A 108.5 . . ? H23B C23 C24 110.3 . . ? H23A C23 C24 110.3 . . ? C23 C24 C24 108.7(4) . 4_665 ? C23 C24 H24A 110.0 . . ? C23 C24 H24B 110.0 . . ? C24 C24 H24A 110.0 4_665 . ? C24 C24 H24B 110.0 4_665 . ? H24A C24 H24B 108.3 . . ? _diffrn_measured_fraction_theta_max 0.963 _diffrn_reflns_theta_full 24.01 _diffrn_measured_fraction_theta_full 0.963 _refine_diff_density_max 0.410 _refine_diff_density_min -0.514 _refine_diff_density_rms 0.056 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.000 0.010 769 46 ' ' 2 0.333 0.667 0.656 766 46 ' ' 3 0.667 0.333 0.323 770 46 ' ' _platon_squeeze_details ; ; # Contents of RES file _iucr_refine_instructions_details ; TITL eh8 in R3m CELL 0.6889 32.394 32.394 11.017 90.000 90.000 120.000 ZERR 9.00 0.006 0.006 0.002 0.000 0.000 0.000 LATT -3 SYMM -Y, X-Y, Z SYMM -X+Y, -X, Z SYMM -Y, -X, Z SYMM -X+Y, Y, Z SYMM X, X-Y, Z SFAC C H N O MG DISP Mg 0.04190 0.03438 148.53 UNIT 360 477 27 18 9 TEMP -123 SIZE 0.02 0.02 0.15 SHEL 5.8 0.84 MERG 4 OMIT -4 5 3 L.S. 8 ACTA BOND $H FMAP 2 PLAN 10 WGHT 0.163400 0.998200 EXTI 0.461430 FVAR 2.42301 MG 5 0.792219 0.207781 0.749915 10.50000 0.03662 0.03662 = 0.04582 -0.00177 0.00177 0.01647 O1 4 0.788180 0.211820 0.581889 10.50000 0.05711 0.05711 = 0.04743 0.00205 -0.00205 0.02269 O2 4 0.828059 0.171941 0.745951 10.50000 0.04513 0.04513 = 0.05557 -0.00246 0.00246 0.02184 N1 3 0.730786 0.176126 0.848479 11.00000 0.03896 0.03712 = 0.05100 0.00053 0.00361 0.01910 N2 3 0.807756 0.192244 0.355795 10.50000 0.08926 0.08926 = 0.04728 -0.00339 0.00339 0.04537 C1 1 0.747937 0.252063 0.932632 10.50000 0.04301 0.04301 = 0.05515 -0.00631 0.00631 0.02213 AFIX 43 H1 2 0.732358 0.267639 0.966423 10.50000 -1.20000 AFIX 0 C2 1 0.718259 0.203073 0.911689 11.00000 0.03636 0.04376 = 0.05371 0.00176 0.00474 0.02105 C3 1 0.669408 0.181122 0.969161 11.00000 0.04614 0.04887 = 0.08925 0.00077 0.01984 0.02015 AFIX 137 H3A 2 0.645241 0.160619 0.909893 11.00000 -1.50000 H3B 2 0.663200 0.206446 0.995161 11.00000 -1.50000 H3C 2 0.668115 0.162072 1.039685 11.00000 -1.50000 AFIX 0 C4 1 0.698884 0.125947 0.842666 11.00000 0.03294 0.03566 = 0.06479 -0.00012 0.00879 0.01435 C5 1 0.698440 0.096408 0.940425 11.00000 0.04901 0.04170 = 0.06507 0.00522 0.01046 0.02076 C6 1 0.668782 0.047276 0.928478 11.00000 0.06771 0.04028 = 0.08450 0.00835 0.02225 0.02300 AFIX 43 H6 2 0.667966 0.026913 0.991636 11.00000 -1.20000 AFIX 0 C7 1 0.640842 0.027670 0.828123 11.00000 0.06130 0.03645 = 0.10978 -0.00590 0.02680 0.01257 AFIX 43 H7 2 0.620702 -0.005916 0.823157 11.00000 -1.20000 AFIX 0 C8 1 0.641568 0.055636 0.735642 11.00000 0.04491 0.04815 = 0.08978 -0.01421 0.00954 0.01321 AFIX 43 H8 2 0.622102 0.041206 0.666448 11.00000 -1.20000 AFIX 0 C9 1 0.670291 0.105181 0.739813 11.00000 0.03624 0.04681 = 0.07020 -0.00957 0.00406 0.01906 C10 1 0.729349 0.117296 1.052563 11.00000 0.06565 0.04579 = 0.06603 0.01112 0.00837 0.02586 AFIX 13 H10 2 0.742556 0.152572 1.052137 11.00000 -1.20000 AFIX 0 C11 1 0.700320 0.096924 1.169476 11.00000 0.10943 0.07477 = 0.07485 0.01409 0.02668 0.04155 AFIX 137 H11A 2 0.678198 0.109039 1.179248 11.00000 -1.50000 H11B 2 0.721967 0.106680 1.239219 11.00000 -1.50000 H11C 2 0.682268 0.062052 1.164568 11.00000 -1.50000 AFIX 0 C12 1 0.771311 0.107638 1.048645 11.00000 0.08851 0.10180 = 0.07193 0.01012 0.00440 0.05705 AFIX 137 H12A 2 0.789956 0.121554 0.974644 11.00000 -1.50000 H12B 2 0.758992 0.073169 1.048966 11.00000 -1.50000 H12C 2 0.791683 0.122044 1.119834 11.00000 -1.50000 AFIX 0 C13 1 0.667819 0.135463 0.637679 11.00000 0.04287 0.06109 = 0.07146 -0.01492 -0.00881 0.02912 AFIX 13 H13 2 0.692698 0.169409 0.652739 11.00000 -1.20000 AFIX 0 C14 1 0.619197 0.132165 0.637958 11.00000 0.06330 0.11666 = 0.10143 -0.00398 -0.00438 0.05945 AFIX 137 H14A 2 0.618437 0.153147 0.575002 11.00000 -1.50000 H14B 2 0.613552 0.142008 0.717452 11.00000 -1.50000 H14C 2 0.594345 0.099219 0.621601 11.00000 -1.50000 AFIX 0 C15 1 0.677619 0.120710 0.514778 11.00000 0.05949 0.06373 = 0.06871 -0.01934 -0.00909 0.02671 AFIX 137 H15A 2 0.708326 0.121665 0.517248 11.00000 -1.50000 H15B 2 0.678590 0.142694 0.452243 11.00000 -1.50000 H15C 2 0.652255 0.088268 0.495669 11.00000 -1.50000 AFIX 0 C16 1 0.773904 0.226096 0.488899 10.50000 0.05051 0.05051 = 0.05490 0.00162 -0.00162 0.01510 C17 1 0.749305 0.250695 0.497767 10.50000 0.06744 0.06744 = 0.05968 0.00327 -0.00327 0.02665 AFIX 43 H17 2 0.742315 0.257685 0.576306 10.50000 -1.20000 AFIX 0 C18 1 0.734502 0.265498 0.398385 10.50000 0.08124 0.08124 = 0.08158 0.00638 -0.00638 0.04207 AFIX 43 H18 2 0.717683 0.282317 0.408286 10.50000 -1.20000 AFIX 0 C19 1 0.744647 0.255353 0.282325 10.50000 0.10020 0.10020 = 0.06905 0.01350 -0.01350 0.04353 AFIX 43 H19 2 0.734560 0.265440 0.213066 10.50000 -1.20000 AFIX 0 C20 1 0.768391 0.231609 0.267206 10.50000 0.07995 0.07995 = 0.05186 0.00209 -0.00209 0.02977 AFIX 43 H20 2 0.775072 0.224928 0.187973 10.50000 -1.20000 AFIX 0 C21 1 0.783204 0.216796 0.369563 10.50000 0.06356 0.06356 = 0.05044 0.00130 -0.00130 0.01947 C22 1 0.827850 0.172150 0.346210 10.50000 0.17572 0.17572 = 0.06168 -0.01473 0.01473 0.12337 C23 1 0.803269 0.124103 0.693315 11.00000 0.07373 0.04691 = 0.10375 -0.02408 -0.00482 0.03083 AFIX 23 H23B 2 0.788067 0.099865 0.757995 11.00000 -1.50000 H23A 2 0.778227 0.120998 0.636374 11.00000 -1.50000 AFIX 0 C24 1 0.838605 0.117422 0.629682 11.00000 0.13021 0.09477 = 0.10749 -0.02921 0.00898 0.07179 AFIX 23 H24A 2 0.842703 0.092468 0.670449 11.00000 -1.20000 H24B 2 0.828079 0.107093 0.545215 11.00000 -1.20000 HKLF 4 REM eh8 in R3m REM R1 = 0.0751 for 1919 Fo > 4sig(Fo) and 0.0759 for all 1967 data REM 232 parameters refined using 1 restraints END ; data_eh7 _database_code_depnum_ccdc_archive 'CCDC 916809' #TrackingRef 'All7.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C72 H90 Mg2 N6 S2, C6 H14' _chemical_formula_sum 'C78 H104 Mg2 N6 S2' _chemical_formula_weight 1238.41 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' Mg Mg 0.0419 0.0344 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1002 0.1169 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 13.5757(17) _cell_length_b 14.4034(18) _cell_length_c 18.932(2) _cell_angle_alpha 90.00 _cell_angle_beta 92.2137(13) _cell_angle_gamma 90.00 _cell_volume 3699.1(8) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9932 _cell_measurement_theta_min 2.23 _cell_measurement_theta_max 27.40 _exptl_crystal_description plate _exptl_crystal_colour green _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.112 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1340 _exptl_absorpt_coefficient_mu 0.126 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.994 _exptl_absorpt_correction_T_max 0.999 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.6889 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'Diamond beamline I19' _diffrn_radiation_monochromator 'silicon double crystal' _diffrn_measurement_device_type 'Crystal Logic diffractometer and Rigaku Saturn 724+ CCD' _diffrn_measurement_method 'thick-slice \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 26382 _diffrn_reflns_av_R_equivalents 0.0865 _diffrn_reflns_av_sigmaI/netI 0.0695 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.42 _diffrn_reflns_theta_max 24.21 _reflns_number_total 6415 _reflns_number_gt 5418 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Rigaku CrystalClear' _computing_cell_refinement 'Bruker APEX2' _computing_data_reduction 'Bruker APEX2' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL and local programs' _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^)+(0.1396P)^2^+0.4842P] 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 1.13(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 6415 _refine_ls_number_parameters 409 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0910 _refine_ls_R_factor_gt 0.0830 _refine_ls_wR_factor_ref 0.2099 _refine_ls_wR_factor_gt 0.1985 _refine_ls_goodness_of_fit_ref 1.157 _refine_ls_restrained_S_all 1.157 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mg Mg 0.39612(4) 0.58994(5) 0.47858(4) 0.0221(3) Uani 1 1 d . . . S S 0.42234(4) 0.27591(4) 0.45553(3) 0.0321(3) Uani 1 1 d . . . N1 N 0.38075(11) 0.44757(13) 0.45787(9) 0.0243(4) Uani 1 1 d . . . N2 N 0.35722(11) 0.66976(12) 0.39170(9) 0.0254(4) Uani 1 1 d . . . N3 N 0.27939(12) 0.63743(13) 0.53575(9) 0.0261(4) Uani 1 1 d . . . C1 C 0.30779(15) 0.30712(17) 0.42083(12) 0.0293(5) Uani 1 1 d . . . C2 C 0.23262(18) 0.2528(2) 0.39069(14) 0.0402(6) Uani 1 1 d . . . H2 H 0.2395 0.1873 0.3877 0.048 Uiso 1 1 calc R . . C3 C 0.14849(18) 0.2957(2) 0.36542(15) 0.0440(7) Uani 1 1 d . . . H3 H 0.0969 0.2598 0.3439 0.053 Uiso 1 1 calc R . . C4 C 0.13770(16) 0.3918(2) 0.37102(14) 0.0396(6) Uani 1 1 d . . . H4 H 0.0787 0.4203 0.3532 0.048 Uiso 1 1 calc R . . C5 C 0.21097(15) 0.44603(17) 0.40186(12) 0.0303(5) Uani 1 1 d . . . H5 H 0.2025 0.5112 0.4060 0.036 Uiso 1 1 calc R . . C6 C 0.29775(14) 0.40372(15) 0.42683(11) 0.0264(5) Uani 1 1 d . . . C7 C 0.45431(14) 0.39029(15) 0.47591(11) 0.0256(5) Uani 1 1 d . . . C8 C 0.22958(16) 0.72983(19) 0.30700(13) 0.0372(6) Uani 1 1 d . . . H8A H 0.2843 0.7605 0.2841 0.056 Uiso 1 1 calc R . . H8B H 0.1754 0.7741 0.3119 0.056 Uiso 1 1 calc R . . H8C H 0.2066 0.6771 0.2781 0.056 Uiso 1 1 calc R . . C9 C 0.26401(15) 0.69562(15) 0.37920(12) 0.0274(5) Uani 1 1 d . . . C10 C 0.19076(15) 0.69077(16) 0.42958(12) 0.0303(5) Uani 1 1 d . . . H10 H 0.1260 0.7048 0.4119 0.036 Uiso 1 1 calc R . . C11 C 0.19779(14) 0.66840(15) 0.50207(12) 0.0278(5) Uani 1 1 d . . . C12 C 0.10299(16) 0.68036(19) 0.54061(13) 0.0369(6) Uani 1 1 d . . . H12A H 0.1178 0.6823 0.5917 0.055 Uiso 1 1 calc R . . H12B H 0.0589 0.6281 0.5295 0.055 Uiso 1 1 calc R . . H12C H 0.0710 0.7384 0.5256 0.055 Uiso 1 1 calc R . . C13 C 0.42835(14) 0.68857(15) 0.33847(11) 0.0265(5) Uani 1 1 d . . . C14 C 0.44855(14) 0.62127(17) 0.28721(12) 0.0291(5) Uani 1 1 d . . . C15 C 0.52060(15) 0.64110(19) 0.23862(13) 0.0360(6) Uani 1 1 d . . . H15 H 0.5356 0.5961 0.2040 0.043 Uiso 1 1 calc R . . C16 C 0.56995(16) 0.72404(19) 0.23992(14) 0.0412(7) Uani 1 1 d . . . H16 H 0.6177 0.7367 0.2058 0.049 Uiso 1 1 calc R . . C17 C 0.55023(16) 0.78876(19) 0.29047(14) 0.0384(6) Uani 1 1 d . . . H17 H 0.5848 0.8461 0.2907 0.046 Uiso 1 1 calc R . . C18 C 0.48062(15) 0.77278(16) 0.34180(13) 0.0328(6) Uani 1 1 d . . . C19 C 0.39556(15) 0.52914(17) 0.28291(12) 0.0321(5) Uani 1 1 d . . . H19 H 0.3495 0.5265 0.3229 0.039 Uiso 1 1 calc R . . C20 C 0.3337(2) 0.5186(2) 0.21401(17) 0.0523(7) Uani 1 1 d . . . H20A H 0.2875 0.5707 0.2091 0.078 Uiso 1 1 calc R . . H20B H 0.2968 0.4602 0.2150 0.078 Uiso 1 1 calc R . . H20C H 0.3772 0.5182 0.1739 0.078 Uiso 1 1 calc R . . C21 C 0.46640(19) 0.44706(19) 0.29118(14) 0.0429(6) Uani 1 1 d . . . H21A H 0.5084 0.4554 0.3340 0.064 Uiso 1 1 calc R . . H21B H 0.5077 0.4437 0.2499 0.064 Uiso 1 1 calc R . . H21C H 0.4286 0.3894 0.2949 0.064 Uiso 1 1 calc R . . C22 C 0.46427(17) 0.84459(17) 0.39905(14) 0.0387(6) Uani 1 1 d . . . H22 H 0.4440 0.8105 0.4421 0.046 Uiso 1 1 calc R . . C23 C 0.3813(2) 0.9122(2) 0.3783(2) 0.0588(8) Uani 1 1 d . . . H23A H 0.3182 0.8791 0.3765 0.088 Uiso 1 1 calc R . . H23B H 0.3932 0.9387 0.3318 0.088 Uiso 1 1 calc R . . H23C H 0.3792 0.9621 0.4134 0.088 Uiso 1 1 calc R . . C24 C 0.5584(2) 0.8988(2) 0.41927(18) 0.0511(7) Uani 1 1 d . . . H24A H 0.6133 0.8554 0.4268 0.077 Uiso 1 1 calc R . . H24B H 0.5486 0.9338 0.4628 0.077 Uiso 1 1 calc R . . H24C H 0.5734 0.9419 0.3811 0.077 Uiso 1 1 calc R . . C25 C 0.27901(14) 0.62703(17) 0.61115(12) 0.0299(5) Uani 1 1 d . . . C26 C 0.24713(14) 0.54367(17) 0.64142(12) 0.0320(6) Uani 1 1 d . . . C27 C 0.24872(17) 0.5368(2) 0.71500(13) 0.0411(6) Uani 1 1 d . . . H27 H 0.2266 0.4813 0.7364 0.049 Uiso 1 1 calc R . . C28 C 0.28209(18) 0.6097(2) 0.75744(13) 0.0442(7) Uani 1 1 d . . . H28 H 0.2820 0.6042 0.8074 0.053 Uiso 1 1 calc R . . C29 C 0.31521(17) 0.6897(2) 0.72716(13) 0.0419(6) Uani 1 1 d . . . H29 H 0.3388 0.7388 0.7567 0.050 Uiso 1 1 calc R . . C30 C 0.31510(15) 0.70062(18) 0.65391(13) 0.0335(6) Uani 1 1 d . . . C31 C 0.35293(17) 0.79006(18) 0.62161(14) 0.0387(6) Uani 1 1 d . . . H31 H 0.3810 0.7733 0.5753 0.046 Uiso 1 1 calc R . . C32 C 0.4357(2) 0.8355(2) 0.66650(17) 0.0531(8) Uani 1 1 d . . . H32A H 0.4846 0.7884 0.6808 0.080 Uiso 1 1 calc R . . H32B H 0.4083 0.8633 0.7087 0.080 Uiso 1 1 calc R . . H32C H 0.4673 0.8838 0.6388 0.080 Uiso 1 1 calc R . . C33 C 0.2701(2) 0.8601(2) 0.60617(18) 0.0527(7) Uani 1 1 d . . . H33A H 0.2236 0.8346 0.5704 0.079 Uiso 1 1 calc R . . H33B H 0.2982 0.9180 0.5886 0.079 Uiso 1 1 calc R . . H33C H 0.2355 0.8727 0.6496 0.079 Uiso 1 1 calc R . . C34 C 0.21260(16) 0.46148(18) 0.59794(13) 0.0350(6) Uani 1 1 d . . . H34 H 0.2180 0.4783 0.5470 0.042 Uiso 1 1 calc R . . C35 C 0.10432(18) 0.4359(2) 0.60982(17) 0.0503(7) Uani 1 1 d . . . H35A H 0.0619 0.4889 0.5973 0.075 Uiso 1 1 calc R . . H35B H 0.0967 0.4199 0.6596 0.075 Uiso 1 1 calc R . . H35C H 0.0854 0.3826 0.5801 0.075 Uiso 1 1 calc R . . C36 C 0.27786(18) 0.37629(19) 0.61247(15) 0.0427(6) Uani 1 1 d . . . H36A H 0.3473 0.3941 0.6100 0.064 Uiso 1 1 calc R . . H36B H 0.2623 0.3284 0.5770 0.064 Uiso 1 1 calc R . . H36C H 0.2656 0.3519 0.6597 0.064 Uiso 1 1 calc R . . C37 C 0.3869(6) 0.6684(4) 0.9390(4) 0.137(2) Uani 1 1 d . . . H37A H 0.4027 0.6978 0.8941 0.206 Uiso 1 1 calc R . . H37B H 0.4107 0.7076 0.9784 0.206 Uiso 1 1 calc R . . H37C H 0.3153 0.6608 0.9410 0.206 Uiso 1 1 calc R . . C38 C 0.4313(11) 0.5836(6) 0.9437(5) 0.289(9) Uani 1 1 d . . . H38A H 0.3800 0.5394 0.9264 0.347 Uiso 1 1 calc R . . H38B H 0.4812 0.5848 0.9070 0.347 Uiso 1 1 calc R . . C39 C 0.4756(10) 0.5408(5) 0.9980(5) 0.229(6) Uani 1 1 d . . . H39A H 0.4241 0.5353 1.0334 0.275 Uiso 1 1 calc R . . H39B H 0.5234 0.5869 1.0176 0.275 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mg 0.0146(4) 0.0246(5) 0.0274(4) 0.0005(3) 0.0058(3) 0.0018(2) S 0.0258(4) 0.0258(4) 0.0447(4) -0.0032(2) 0.0021(2) 0.0017(2) N1 0.0162(8) 0.0277(10) 0.0293(9) -0.0002(7) 0.0051(6) -0.0005(6) N2 0.0173(8) 0.0270(10) 0.0323(10) 0.0018(7) 0.0064(7) 0.0012(6) N3 0.0212(8) 0.0305(10) 0.0270(9) -0.0008(7) 0.0074(6) 0.0024(7) C1 0.0250(10) 0.0310(12) 0.0323(12) -0.0033(9) 0.0072(8) -0.0018(8) C2 0.0348(12) 0.0382(14) 0.0480(15) -0.0108(11) 0.0060(10) -0.0077(10) C3 0.0305(12) 0.0522(17) 0.0492(15) -0.0134(13) 0.0015(10) -0.0107(11) C4 0.0215(10) 0.0564(17) 0.0409(14) -0.0057(12) 0.0020(9) -0.0008(10) C5 0.0220(10) 0.0354(13) 0.0337(12) -0.0011(10) 0.0055(8) 0.0017(8) C6 0.0207(10) 0.0315(13) 0.0275(11) -0.0024(9) 0.0071(8) -0.0014(8) C7 0.0203(10) 0.0275(12) 0.0296(11) -0.0004(9) 0.0078(8) 0.0005(8) C8 0.0255(11) 0.0506(16) 0.0356(13) 0.0096(11) 0.0041(9) 0.0089(9) C9 0.0225(10) 0.0277(12) 0.0323(12) 0.0014(9) 0.0054(8) 0.0020(8) C10 0.0185(9) 0.0352(13) 0.0374(13) 0.0008(10) 0.0036(8) 0.0055(8) C11 0.0206(9) 0.0284(12) 0.0349(12) -0.0009(9) 0.0085(8) 0.0038(8) C12 0.0230(10) 0.0502(16) 0.0384(13) 0.0025(11) 0.0110(9) 0.0087(10) C13 0.0173(9) 0.0325(12) 0.0301(11) 0.0083(9) 0.0060(8) 0.0023(8) C14 0.0196(9) 0.0382(13) 0.0297(11) 0.0050(9) 0.0047(8) 0.0045(8) C15 0.0242(10) 0.0510(16) 0.0333(12) 0.0063(10) 0.0080(9) 0.0061(10) C16 0.0233(11) 0.0618(18) 0.0391(14) 0.0186(12) 0.0093(9) 0.0006(10) C17 0.0239(11) 0.0453(15) 0.0462(14) 0.0178(11) 0.0037(9) -0.0065(9) C18 0.0233(10) 0.0366(14) 0.0385(13) 0.0102(10) 0.0021(9) -0.0011(8) C19 0.0255(10) 0.0377(14) 0.0338(12) -0.0023(10) 0.0086(8) 0.0034(9) C20 0.0497(15) 0.0498(17) 0.0563(18) -0.0025(14) -0.0113(13) -0.0031(12) C21 0.0415(13) 0.0415(15) 0.0464(15) 0.0029(12) 0.0125(11) 0.0105(11) C22 0.0354(12) 0.0309(13) 0.0499(15) 0.0033(11) 0.0019(10) -0.0031(10) C23 0.0556(17) 0.0410(17) 0.079(2) -0.0003(15) -0.0056(15) 0.0114(13) C24 0.0505(16) 0.0399(16) 0.0624(18) 0.0047(13) -0.0036(13) -0.0130(12) C25 0.0185(9) 0.0414(14) 0.0306(12) -0.0010(9) 0.0102(8) 0.0071(8) C26 0.0198(10) 0.0434(14) 0.0333(12) 0.0036(10) 0.0086(8) 0.0062(9) C27 0.0322(12) 0.0574(17) 0.0343(13) 0.0075(12) 0.0113(9) 0.0085(11) C28 0.0350(12) 0.0690(19) 0.0292(12) -0.0007(12) 0.0088(9) 0.0139(12) C29 0.0312(12) 0.0590(17) 0.0360(13) -0.0127(12) 0.0062(9) 0.0133(11) C30 0.0234(10) 0.0428(14) 0.0350(12) -0.0084(10) 0.0087(8) 0.0074(9) C31 0.0326(12) 0.0402(15) 0.0440(14) -0.0114(11) 0.0100(10) 0.0017(10) C32 0.0440(14) 0.0535(18) 0.0622(19) -0.0237(15) 0.0088(13) -0.0033(12) C33 0.0487(15) 0.0404(16) 0.070(2) -0.0043(14) 0.0086(13) 0.0045(12) C34 0.0297(11) 0.0401(14) 0.0357(12) 0.0073(10) 0.0094(9) 0.0017(9) C35 0.0319(13) 0.0567(18) 0.0626(18) 0.0032(14) 0.0060(12) -0.0026(12) C36 0.0383(13) 0.0413(15) 0.0492(15) 0.0073(12) 0.0118(11) 0.0047(10) C37 0.162(6) 0.113(5) 0.133(5) -0.037(4) -0.038(4) 0.032(4) C38 0.53(2) 0.147(7) 0.177(8) -0.068(6) -0.201(11) 0.158(10) C39 0.401(16) 0.103(5) 0.171(7) -0.033(5) -0.135(10) 0.089(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mg N1 2.097(2) . ? Mg N2 2.0587(19) . ? Mg N3 2.0696(18) . ? Mg C7 2.193(2) 3_666 ? S C1 1.724(2) . ? S C7 1.743(2) . ? N1 C6 1.401(3) . ? N1 C7 1.330(3) . ? N2 C9 1.331(3) . ? N2 C13 1.448(3) . ? N3 C11 1.333(3) . ? N3 C25 1.435(3) . ? C1 C2 1.391(3) . ? C1 C6 1.403(3) . ? C2 H2 0.950 . ? C2 C3 1.369(4) . ? C3 H3 0.950 . ? C3 C4 1.396(4) . ? C4 H4 0.950 . ? C4 C5 1.377(3) . ? C5 H5 0.950 . ? C5 C6 1.393(3) . ? C7 Mg 2.193(2) 3_666 ? C8 H8A 0.980 . ? C8 H8B 0.980 . ? C8 H8C 0.980 . ? C8 C9 1.510(3) . ? C9 C10 1.406(3) . ? C10 H10 0.950 . ? C10 C11 1.409(3) . ? C11 C12 1.514(3) . ? C12 H12A 0.980 . ? C12 H12B 0.980 . ? C12 H12C 0.980 . ? C13 C14 1.406(3) . ? C13 C18 1.405(3) . ? C14 C15 1.398(3) . ? C14 C19 1.510(3) . ? C15 H15 0.950 . ? C15 C16 1.369(4) . ? C16 H16 0.950 . ? C16 C17 1.370(4) . ? C17 H17 0.950 . ? C17 C18 1.401(3) . ? C18 C22 1.521(4) . ? C19 H19 1.000 . ? C19 C20 1.531(3) . ? C19 C21 1.528(3) . ? C20 H20A 0.980 . ? C20 H20B 0.980 . ? C20 H20C 0.980 . ? C21 H21A 0.980 . ? C21 H21B 0.980 . ? C21 H21C 0.980 . ? C22 H22 1.000 . ? C22 C23 1.529(4) . ? C22 C24 1.533(3) . ? C23 H23A 0.980 . ? C23 H23B 0.980 . ? C23 H23C 0.980 . ? C24 H24A 0.980 . ? C24 H24B 0.980 . ? C24 H24C 0.980 . ? C25 C26 1.406(3) . ? C25 C30 1.410(3) . ? C26 C27 1.396(3) . ? C26 C34 1.506(4) . ? C27 H27 0.950 . ? C27 C28 1.387(4) . ? C28 H28 0.950 . ? C28 C29 1.370(4) . ? C29 H29 0.950 . ? C29 C30 1.396(4) . ? C30 C31 1.524(4) . ? C31 H31 1.000 . ? C31 C32 1.529(4) . ? C31 C33 1.531(4) . ? C32 H32A 0.980 . ? C32 H32B 0.980 . ? C32 H32C 0.980 . ? C33 H33A 0.980 . ? C33 H33B 0.980 . ? C33 H33C 0.980 . ? C34 H34 1.000 . ? C34 C35 1.540(3) . ? C34 C36 1.532(3) . ? C35 H35A 0.980 . ? C35 H35B 0.980 . ? C35 H35C 0.980 . ? C36 H36A 0.980 . ? C36 H36B 0.980 . ? C36 H36C 0.980 . ? C37 H37A 0.980 . ? C37 H37B 0.980 . ? C37 H37C 0.980 . ? C37 C38 1.364(9) . ? C38 H38A 0.990 . ? C38 H38B 0.990 . ? C38 C39 1.323(9) . ? C39 C39 1.350(13) 3_667 ? C39 H39A 0.990 . ? C39 H39B 0.990 . ? 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 N1 Mg N2 112.09(8) . . ? N1 Mg N3 110.39(7) . . ? N1 Mg C7 106.52(8) . 3_666 ? N2 Mg N3 93.17(7) . . ? N2 Mg C7 116.51(8) . 3_666 ? N3 Mg C7 117.87(8) . 3_666 ? C1 S C7 92.93(10) . . ? Mg N1 C6 126.30(14) . . ? Mg N1 C7 119.37(14) . . ? C6 N1 C7 114.32(18) . . ? Mg N2 C9 120.73(14) . . ? Mg N2 C13 120.21(12) . . ? C9 N2 C13 118.59(17) . . ? Mg N3 C11 119.95(14) . . ? Mg N3 C25 121.18(13) . . ? C11 N3 C25 118.40(17) . . ? S C1 C2 130.3(2) . . ? S C1 C6 108.46(16) . . ? C2 C1 C6 121.3(2) . . ? C1 C2 H2 120.7 . . ? C1 C2 C3 118.6(2) . . ? H2 C2 C3 120.7 . . ? C2 C3 H3 119.7 . . ? C2 C3 C4 120.7(2) . . ? H3 C3 C4 119.7 . . ? C3 C4 H4 119.4 . . ? C3 C4 C5 121.2(2) . . ? H4 C4 C5 119.4 . . ? C4 C5 H5 120.5 . . ? C4 C5 C6 118.9(2) . . ? H5 C5 C6 120.5 . . ? N1 C6 C1 113.70(18) . . ? N1 C6 C5 126.9(2) . . ? C1 C6 C5 119.3(2) . . ? Mg C7 S 115.37(11) 3_666 . ? Mg C7 N1 134.02(16) 3_666 . ? S C7 N1 110.57(15) . . ? H8A C8 H8B 109.5 . . ? H8A C8 H8C 109.5 . . ? H8A C8 C9 109.5 . . ? H8B C8 H8C 109.5 . . ? H8B C8 C9 109.5 . . ? H8C C8 C9 109.5 . . ? N2 C9 C8 120.74(19) . . ? N2 C9 C10 123.9(2) . . ? C8 C9 C10 115.33(18) . . ? C9 C10 H10 114.8 . . ? C9 C10 C11 130.46(19) . . ? H10 C10 C11 114.8 . . ? N3 C11 C10 124.46(18) . . ? N3 C11 C12 120.9(2) . . ? C10 C11 C12 114.62(18) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12B 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N2 C13 C14 120.29(19) . . ? N2 C13 C18 118.7(2) . . ? C14 C13 C18 120.95(19) . . ? C13 C14 C15 118.3(2) . . ? C13 C14 C19 122.53(19) . . ? C15 C14 C19 119.2(2) . . ? C14 C15 H15 119.3 . . ? C14 C15 C16 121.4(2) . . ? H15 C15 C16 119.3 . . ? C15 C16 H16 120.1 . . ? C15 C16 C17 119.8(2) . . ? H16 C16 C17 120.1 . . ? C16 C17 H17 119.1 . . ? C16 C17 C18 121.9(2) . . ? H17 C17 C18 119.1 . . ? C13 C18 C17 117.6(2) . . ? C13 C18 C22 122.1(2) . . ? C17 C18 C22 120.2(2) . . ? C14 C19 H19 107.6 . . ? C14 C19 C20 112.2(2) . . ? C14 C19 C21 112.19(18) . . ? H19 C19 C20 107.6 . . ? H19 C19 C21 107.6 . . ? C20 C19 C21 109.4(2) . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20B 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21B 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C18 C22 H22 107.4 . . ? C18 C22 C23 112.1(2) . . ? C18 C22 C24 112.4(2) . . ? H22 C22 C23 107.4 . . ? H22 C22 C24 107.4 . . ? C23 C22 C24 109.8(2) . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23B 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24B 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N3 C25 C26 120.5(2) . . ? N3 C25 C30 118.6(2) . . ? C26 C25 C30 120.9(2) . . ? C25 C26 C27 118.3(2) . . ? C25 C26 C34 122.9(2) . . ? C27 C26 C34 118.8(2) . . ? C26 C27 H27 119.5 . . ? C26 C27 C28 121.1(3) . . ? H27 C27 C28 119.5 . . ? C27 C28 H28 120.0 . . ? C27 C28 C29 119.9(2) . . ? H28 C28 C29 120.0 . . ? C28 C29 H29 119.2 . . ? C28 C29 C30 121.5(3) . . ? H29 C29 C30 119.2 . . ? C25 C30 C29 118.2(2) . . ? C25 C30 C31 121.3(2) . . ? C29 C30 C31 120.5(2) . . ? C30 C31 H31 107.1 . . ? C30 C31 C32 113.0(2) . . ? C30 C31 C33 112.2(2) . . ? H31 C31 C32 107.1 . . ? H31 C31 C33 107.1 . . ? C32 C31 C33 110.1(2) . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32B 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C31 C33 H33A 109.5 . . ? C31 C33 H33B 109.5 . . ? C31 C33 H33C 109.5 . . ? H33A C33 H33B 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C26 C34 H34 107.7 . . ? C26 C34 C35 112.8(2) . . ? C26 C34 C36 111.5(2) . . ? H34 C34 C35 107.7 . . ? H34 C34 C36 107.7 . . ? C35 C34 C36 109.3(2) . . ? C34 C35 H35A 109.5 . . ? C34 C35 H35B 109.5 . . ? C34 C35 H35C 109.5 . . ? H35A C35 H35B 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C34 C36 H36A 109.5 . . ? C34 C36 H36B 109.5 . . ? C34 C36 H36C 109.5 . . ? H36A C36 H36B 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? H37A C37 H37B 109.5 . . ? H37A C37 H37C 109.5 . . ? H37A C37 C38 109.5 . . ? H37B C37 H37C 109.5 . . ? H37B C37 C38 109.5 . . ? H37C C37 C38 109.5 . . ? C37 C38 H38A 104.5 . . ? C37 C38 H38B 104.5 . . ? C37 C38 C39 130.9(8) . . ? H38A C38 H38B 105.7 . . ? H38A C38 C39 104.5 . . ? H38B C38 C39 104.5 . . ? C38 C39 C39 131.0(10) . 3_667 ? C38 C39 H39A 104.5 . . ? C38 C39 H39B 104.5 . . ? C39 C39 H39A 104.5 3_667 . ? C39 C39 H39B 104.5 3_667 . ? H39A C39 H39B 105.7 . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 24.21 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 0.683 _refine_diff_density_min -0.464 _refine_diff_density_rms 0.109 # Contents of RES file _iucr_refine_instructions_details ; TITL eh7 in P2(1)/n CELL 0.6889 13.5757 14.4034 18.9319 90.000 92.2137 90.000 ZERR 2.00 0.0017 0.0018 0.0024 0.000 0.0013 0.000 LATT 1 SYMM 0.5-X, 0.5+Y, 0.5-Z SFAC C H N MG S DISP Mg 0.04190 0.03438 148.53 DISP S 0.10019 0.11693 478.92 UNIT 156 208 12 4 4 TEMP -123 SIZE 0.01 0.05 0.05 REM green plate SHEL 5.8 0.84 L.S. 8 BOND $H ACTA FMAP 2 PLAN 10 WGHT 0.139600 0.484200 EXTI 1.131898 FVAR 0.39719 MG 4 0.396120 0.589939 0.478578 11.00000 0.01459 0.02458 = 0.02743 0.00052 0.00580 0.00184 S 5 0.422343 0.275914 0.455528 11.00000 0.02577 0.02578 = 0.04474 -0.00315 0.00214 0.00171 N1 3 0.380748 0.447569 0.457866 11.00000 0.01617 0.02770 = 0.02928 -0.00025 0.00514 -0.00048 N2 3 0.357220 0.669755 0.391704 11.00000 0.01734 0.02704 = 0.03226 0.00182 0.00636 0.00124 N3 3 0.279388 0.637431 0.535749 11.00000 0.02116 0.03048 = 0.02704 -0.00076 0.00744 0.00240 C1 1 0.307790 0.307121 0.420829 11.00000 0.02500 0.03104 = 0.03235 -0.00327 0.00721 -0.00182 C2 1 0.232622 0.252768 0.390687 11.00000 0.03483 0.03822 = 0.04798 -0.01085 0.00599 -0.00771 AFIX 43 H2 2 0.239531 0.187266 0.387701 11.00000 -1.20000 AFIX 0 C3 1 0.148489 0.295694 0.365422 11.00000 0.03054 0.05219 = 0.04918 -0.01338 0.00154 -0.01075 AFIX 43 H3 2 0.096926 0.259752 0.343864 11.00000 -1.20000 AFIX 0 C4 1 0.137699 0.391789 0.371020 11.00000 0.02153 0.05642 = 0.04087 -0.00569 0.00204 -0.00075 AFIX 43 H4 2 0.078706 0.420275 0.353217 11.00000 -1.20000 AFIX 0 C5 1 0.210967 0.446034 0.401863 11.00000 0.02203 0.03540 = 0.03368 -0.00110 0.00553 0.00170 AFIX 43 H5 2 0.202466 0.511245 0.406045 11.00000 -1.20000 AFIX 0 C6 1 0.297746 0.403717 0.426827 11.00000 0.02073 0.03149 = 0.02749 -0.00240 0.00708 -0.00136 C7 1 0.454313 0.390286 0.475910 11.00000 0.02034 0.02750 = 0.02961 -0.00037 0.00782 0.00049 C8 1 0.229575 0.729831 0.307002 11.00000 0.02551 0.05057 = 0.03563 0.00960 0.00411 0.00885 AFIX 137 H8A 2 0.284345 0.760512 0.284135 11.00000 -1.50000 H8B 2 0.175435 0.774082 0.311922 11.00000 -1.50000 H8C 2 0.206595 0.677105 0.278093 11.00000 -1.50000 AFIX 0 C9 1 0.264015 0.695616 0.379199 11.00000 0.02247 0.02773 = 0.03227 0.00140 0.00535 0.00196 C10 1 0.190763 0.690765 0.429579 11.00000 0.01852 0.03520 = 0.03741 0.00083 0.00357 0.00548 AFIX 43 H10 2 0.126044 0.704847 0.411890 11.00000 -1.20000 AFIX 0 C11 1 0.197790 0.668398 0.502068 11.00000 0.02057 0.02841 = 0.03488 -0.00090 0.00854 0.00376 C12 1 0.102993 0.680363 0.540606 11.00000 0.02295 0.05018 = 0.03840 0.00255 0.01104 0.00873 AFIX 137 H12A 2 0.117766 0.682321 0.591664 11.00000 -1.50000 H12B 2 0.058874 0.628067 0.529527 11.00000 -1.50000 H12C 2 0.070960 0.738447 0.525581 11.00000 -1.50000 AFIX 0 C13 1 0.428348 0.688571 0.338471 11.00000 0.01733 0.03253 = 0.03009 0.00826 0.00603 0.00228 C14 1 0.448549 0.621271 0.287210 11.00000 0.01961 0.03824 = 0.02968 0.00499 0.00474 0.00452 C15 1 0.520598 0.641104 0.238616 11.00000 0.02420 0.05103 = 0.03331 0.00626 0.00801 0.00614 AFIX 43 H15 2 0.535642 0.596102 0.203967 11.00000 -1.20000 AFIX 0 C16 1 0.569945 0.724042 0.239915 11.00000 0.02328 0.06181 = 0.03908 0.01857 0.00929 0.00057 AFIX 43 H16 2 0.617738 0.736663 0.205840 11.00000 -1.20000 AFIX 0 C17 1 0.550229 0.788763 0.290465 11.00000 0.02386 0.04529 = 0.04622 0.01775 0.00374 -0.00646 AFIX 43 H17 2 0.584762 0.846136 0.290711 11.00000 -1.20000 AFIX 0 C18 1 0.480617 0.772775 0.341797 11.00000 0.02332 0.03658 = 0.03852 0.01018 0.00210 -0.00106 C19 1 0.395558 0.529136 0.282906 11.00000 0.02545 0.03768 = 0.03379 -0.00231 0.00860 0.00337 AFIX 13 H19 2 0.349548 0.526525 0.322853 11.00000 -1.20000 AFIX 0 C20 1 0.333695 0.518588 0.214008 11.00000 0.04966 0.04983 = 0.05629 -0.00252 -0.01126 -0.00313 AFIX 137 H20A 2 0.287506 0.570680 0.209057 11.00000 -1.50000 H20B 2 0.296772 0.460165 0.214976 11.00000 -1.50000 H20C 2 0.377220 0.518168 0.173900 11.00000 -1.50000 AFIX 0 C21 1 0.466399 0.447064 0.291178 11.00000 0.04154 0.04151 = 0.04639 0.00286 0.01253 0.01047 AFIX 137 H21A 2 0.508351 0.455400 0.334001 11.00000 -1.50000 H21B 2 0.507688 0.443727 0.249921 11.00000 -1.50000 H21C 2 0.428587 0.389431 0.294916 11.00000 -1.50000 AFIX 0 C22 1 0.464268 0.844586 0.399053 11.00000 0.03544 0.03094 = 0.04987 0.00330 0.00192 -0.00306 AFIX 13 H22 2 0.444020 0.810458 0.442143 11.00000 -1.20000 AFIX 0 C23 1 0.381253 0.912209 0.378316 11.00000 0.05564 0.04103 = 0.07903 -0.00028 -0.00565 0.01139 AFIX 137 H23A 2 0.318153 0.879080 0.376512 11.00000 -1.50000 H23B 2 0.393200 0.938741 0.331755 11.00000 -1.50000 H23C 2 0.379207 0.962141 0.413392 11.00000 -1.50000 AFIX 0 C24 1 0.558368 0.898810 0.419268 11.00000 0.05054 0.03993 = 0.06245 0.00468 -0.00360 -0.01303 AFIX 137 H24A 2 0.613323 0.855360 0.426806 11.00000 -1.50000 H24B 2 0.548574 0.933820 0.462824 11.00000 -1.50000 H24C 2 0.573355 0.941910 0.381095 11.00000 -1.50000 AFIX 0 C25 1 0.279010 0.627034 0.611146 11.00000 0.01852 0.04140 = 0.03063 -0.00099 0.01021 0.00714 C26 1 0.247127 0.543669 0.641417 11.00000 0.01975 0.04342 = 0.03332 0.00356 0.00861 0.00622 C27 1 0.248719 0.536809 0.714998 11.00000 0.03225 0.05744 = 0.03425 0.00750 0.01126 0.00845 AFIX 43 H27 2 0.226582 0.481308 0.736371 11.00000 -1.20000 AFIX 0 C28 1 0.282093 0.609698 0.757437 11.00000 0.03501 0.06904 = 0.02922 -0.00067 0.00877 0.01387 AFIX 43 H28 2 0.281984 0.604166 0.807437 11.00000 -1.20000 AFIX 0 C29 1 0.315210 0.689667 0.727160 11.00000 0.03116 0.05901 = 0.03599 -0.01274 0.00616 0.01329 AFIX 43 H29 2 0.338795 0.738798 0.756714 11.00000 -1.20000 AFIX 0 C30 1 0.315099 0.700622 0.653912 11.00000 0.02338 0.04280 = 0.03503 -0.00841 0.00870 0.00743 C31 1 0.352927 0.790060 0.621612 11.00000 0.03257 0.04015 = 0.04401 -0.01142 0.01003 0.00174 AFIX 13 H31 2 0.381022 0.773288 0.575253 11.00000 -1.20000 AFIX 0 C32 1 0.435719 0.835457 0.666496 11.00000 0.04404 0.05351 = 0.06215 -0.02368 0.00877 -0.00333 AFIX 137 H32A 2 0.484648 0.788377 0.680791 11.00000 -1.50000 H32B 2 0.408271 0.863316 0.708672 11.00000 -1.50000 H32C 2 0.467289 0.883765 0.638787 11.00000 -1.50000 AFIX 0 C33 1 0.270099 0.860142 0.606166 11.00000 0.04869 0.04041 = 0.06958 -0.00433 0.00861 0.00451 AFIX 137 H33A 2 0.223602 0.834598 0.570354 11.00000 -1.50000 H33B 2 0.298169 0.918023 0.588616 11.00000 -1.50000 H33C 2 0.235501 0.872671 0.649638 11.00000 -1.50000 AFIX 0 C34 1 0.212600 0.461483 0.597941 11.00000 0.02975 0.04013 = 0.03574 0.00729 0.00945 0.00174 AFIX 13 H34 2 0.217952 0.478300 0.546986 11.00000 -1.20000 AFIX 0 C35 1 0.104324 0.435902 0.609822 11.00000 0.03191 0.05667 = 0.06263 0.00322 0.00604 -0.00260 AFIX 137 H35A 2 0.061913 0.488924 0.597301 11.00000 -1.50000 H35B 2 0.096722 0.419896 0.659628 11.00000 -1.50000 H35C 2 0.085449 0.382610 0.580097 11.00000 -1.50000 AFIX 0 C36 1 0.277859 0.376291 0.612470 11.00000 0.03829 0.04129 = 0.04918 0.00732 0.01180 0.00472 AFIX 137 H36A 2 0.347330 0.394054 0.610038 11.00000 -1.50000 H36B 2 0.262345 0.328391 0.576998 11.00000 -1.50000 H36C 2 0.265643 0.351935 0.659667 11.00000 -1.50000 AFIX 0 C37 1 0.386892 0.668420 0.938969 11.00000 0.16205 0.11269 = 0.13296 -0.03703 -0.03779 0.03249 AFIX 137 H37A 2 0.402723 0.697828 0.894127 11.00000 -1.50000 H37B 2 0.410738 0.707581 0.978358 11.00000 -1.50000 H37C 2 0.315323 0.660809 0.941003 11.00000 -1.50000 AFIX 0 C38 1 0.431266 0.583600 0.943724 11.00000 0.52774 0.14656 = 0.17652 -0.06843 -0.20143 0.15756 AFIX 23 H38A 2 0.379963 0.539405 0.926410 11.00000 -1.20000 H38B 2 0.481167 0.584773 0.906959 11.00000 -1.20000 AFIX 0 C39 1 0.475618 0.540808 0.998016 11.00000 0.40092 0.10322 = 0.17128 -0.03339 -0.13473 0.08934 AFIX 23 H39A 2 0.424093 0.535307 1.033384 11.00000 -1.20000 H39B 2 0.523372 0.586901 1.017612 11.00000 -1.20000 HKLF 4 REM eh7 in P2(1)/n REM R1 = 0.0830 for 5418 Fo > 4sig(Fo) and 0.0910 for all 6415 data REM 409 parameters refined using 0 restraints END ; data_eh3 _database_code_depnum_ccdc_archive 'CCDC 916810' #TrackingRef 'All7.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C43 H50 Mg N4 S2, 1.25 C4 H8 O' _chemical_formula_sum 'C48 H60 Mg N4 O1.25 S2' _chemical_formula_weight 801.43 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' Mg Mg 0.0419 0.0344 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1002 0.1169 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 18.964(5) _cell_length_b 12.505(3) _cell_length_c 38.624(10) _cell_angle_alpha 90.00 _cell_angle_beta 96.385(3) _cell_angle_gamma 90.00 _cell_volume 9103(4) _cell_formula_units_Z 8 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 9746 _cell_measurement_theta_min 2.36 _cell_measurement_theta_max 25.63 _exptl_crystal_description needle _exptl_crystal_colour green _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.170 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3440 _exptl_absorpt_coefficient_mu 0.159 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.984 _exptl_absorpt_correction_T_max 0.998 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.6889 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'Diamond beamline I19' _diffrn_radiation_monochromator 'silicon double crystal' _diffrn_measurement_device_type 'Crystal Logic diffractometer and Rigaku Saturn 724+ CCD' _diffrn_measurement_method 'thick-slice \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 69167 _diffrn_reflns_av_R_equivalents 0.0683 _diffrn_reflns_av_sigmaI/netI 0.0577 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -45 _diffrn_reflns_limit_l_max 45 _diffrn_reflns_theta_min 1.11 _diffrn_reflns_theta_max 24.21 _reflns_number_total 16016 _reflns_number_gt 11598 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Rigaku CrystalClear' _computing_cell_refinement 'Bruker APEX2' _computing_data_reduction 'Bruker APEX2' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL and local programs' _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^)+(0.0672P)^2^+17.1363P] 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 0.0020(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 16016 _refine_ls_number_parameters 1037 _refine_ls_number_restraints 186 _refine_ls_R_factor_all 0.1026 _refine_ls_R_factor_gt 0.0746 _refine_ls_wR_factor_ref 0.1956 _refine_ls_wR_factor_gt 0.1793 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.051 _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 0.78715(6) 0.72047(10) 0.52099(3) 0.0369(3) Uani 1 1 d . . . S1 S 0.69145(5) 0.77100(8) 0.55640(2) 0.0409(2) Uani 1 1 d . . . S2 S 0.78604(6) 0.77680(14) 0.39992(3) 0.0745(5) Uani 1 1 d . . . N1 N 0.69166(15) 0.7055(2) 0.48290(8) 0.0362(7) Uani 1 1 d . . . N2 N 0.82435(15) 0.7412(3) 0.46543(8) 0.0380(7) Uani 1 1 d . . . N3 N 0.83457(15) 0.5758(3) 0.53468(8) 0.0428(8) Uani 1 1 d . . . N4 N 0.86691(15) 0.8058(3) 0.55007(8) 0.0388(7) Uani 1 1 d . . . C1 C 0.61873(18) 0.7194(3) 0.52972(9) 0.0352(8) Uani 1 1 d . . . C2 C 0.55168(19) 0.7097(3) 0.54159(10) 0.0396(9) Uani 1 1 d . . . H2 H 0.5457 0.7311 0.5647 0.047 Uiso 1 1 calc R . . C3 C 0.49431(19) 0.6697(3) 0.52044(10) 0.0437(9) Uani 1 1 d . . . H3 H 0.4497 0.6631 0.5293 0.052 Uiso 1 1 calc R . . C4 C 0.5008(2) 0.6389(3) 0.48655(10) 0.0457(10) Uani 1 1 d . . . H4 H 0.4612 0.6103 0.4723 0.055 Uiso 1 1 calc R . . C5 C 0.56566(19) 0.6503(3) 0.47351(10) 0.0420(9) Uani 1 1 d . . . H5 H 0.5705 0.6304 0.4502 0.050 Uiso 1 1 calc R . . C6 C 0.62364(18) 0.6911(3) 0.49475(9) 0.0359(8) Uani 1 1 d . . . C7 C 0.69769(19) 0.7247(3) 0.45099(10) 0.0448(9) Uani 1 1 d . . . H7 H 0.6574 0.7272 0.4340 0.054 Uiso 1 1 calc R . . C8 C 0.7693(2) 0.7430(4) 0.44153(10) 0.0462(10) Uani 1 1 d . . . C9 C 0.88595(18) 0.7656(3) 0.45036(10) 0.0393(9) Uani 1 1 d . . . C10 C 0.8750(2) 0.7864(4) 0.41490(11) 0.0583(12) Uani 1 1 d . . . C11 C 0.9314(2) 0.8135(5) 0.39571(12) 0.0732(16) Uani 1 1 d . . . H11 H 0.9237 0.8265 0.3714 0.088 Uiso 1 1 calc R . . C12 C 0.9980(2) 0.8202(4) 0.41354(11) 0.0566(12) Uani 1 1 d . . . H12 H 1.0370 0.8388 0.4013 0.068 Uiso 1 1 calc R . . C13 C 1.00929(19) 0.8008(3) 0.44867(10) 0.0448(9) Uani 1 1 d . . . H13 H 1.0560 0.8068 0.4602 0.054 Uiso 1 1 calc R . . C14 C 0.95450(19) 0.7728(3) 0.46779(10) 0.0446(9) Uani 1 1 d . . . H14 H 0.9632 0.7587 0.4921 0.054 Uiso 1 1 calc R . . C15 C 0.7894(2) 0.4550(4) 0.47034(12) 0.0552(11) Uani 1 1 d . . . H15 H 0.8121 0.5272 0.4724 0.066 Uiso 1 1 calc R . . C16 C 0.8448(3) 0.3745(5) 0.45954(14) 0.0809(17) Uani 1 1 d . . . H16A H 0.8850 0.3709 0.4778 0.121 Uiso 1 1 calc R . . H16B H 0.8616 0.3979 0.4377 0.121 Uiso 1 1 calc R . . H16C H 0.8230 0.3036 0.4563 0.121 Uiso 1 1 calc R . . C17 C 0.7274(3) 0.4602(4) 0.44138(13) 0.0678(13) Uani 1 1 d . . . H17A H 0.6920 0.5114 0.4479 0.102 Uiso 1 1 calc R . . H17B H 0.7057 0.3893 0.4381 0.102 Uiso 1 1 calc R . . H17C H 0.7449 0.4833 0.4196 0.102 Uiso 1 1 calc R . . C18 C 0.79134(19) 0.4817(3) 0.53595(11) 0.0471(10) Uani 1 1 d . . . C19 C 0.7666(2) 0.4260(3) 0.50541(12) 0.0506(10) Uani 1 1 d . . . C20 C 0.7202(2) 0.3400(4) 0.50791(14) 0.0602(12) Uani 1 1 d . . . H20 H 0.7023 0.3028 0.4873 0.072 Uiso 1 1 calc R . . C21 C 0.6998(2) 0.3079(4) 0.53954(15) 0.0670(14) Uani 1 1 d . . . H21 H 0.6688 0.2486 0.5408 0.080 Uiso 1 1 calc R . . C22 C 0.7248(2) 0.3629(4) 0.56921(15) 0.0634(13) Uani 1 1 d . . . H22 H 0.7113 0.3400 0.5910 0.076 Uiso 1 1 calc R . . C23 C 0.7694(2) 0.4509(4) 0.56830(12) 0.0544(11) Uani 1 1 d . . . C24 C 0.7928(2) 0.5128(4) 0.60131(13) 0.0634(13) Uani 1 1 d . . . H24 H 0.8036 0.5875 0.5943 0.076 Uiso 1 1 calc R . . C25 C 0.8601(3) 0.4665(7) 0.62037(17) 0.122(3) Uani 1 1 d . . . H25A H 0.8970 0.4630 0.6045 0.182 Uiso 1 1 calc R . . H25B H 0.8506 0.3944 0.6286 0.182 Uiso 1 1 calc R . . H25C H 0.8764 0.5121 0.6403 0.182 Uiso 1 1 calc R . . C26 C 0.7366(2) 0.5193(4) 0.62649(13) 0.0638(13) Uani 1 1 d . . . H26A H 0.7552 0.5601 0.6472 0.096 Uiso 1 1 calc R . . H26B H 0.7241 0.4470 0.6334 0.096 Uiso 1 1 calc R . . H26C H 0.6942 0.5550 0.6151 0.096 Uiso 1 1 calc R . . C27 C 0.9422(2) 0.4624(4) 0.54388(14) 0.0639(13) Uani 1 1 d . . . H27A H 0.9071 0.4052 0.5393 0.096 Uiso 1 1 calc R . . H27B H 0.9680 0.4524 0.5671 0.096 Uiso 1 1 calc R . . H27C H 0.9757 0.4601 0.5263 0.096 Uiso 1 1 calc R . . C28 C 0.9047(2) 0.5700(3) 0.54228(11) 0.0473(10) Uani 1 1 d . . . C29 C 0.94909(19) 0.6592(3) 0.54883(10) 0.0470(10) Uani 1 1 d . . . H29 H 0.9983 0.6446 0.5491 0.056 Uiso 1 1 calc R . . C30 C 0.93263(19) 0.7658(3) 0.55507(9) 0.0428(9) Uani 1 1 d . . . C31 C 0.9946(2) 0.8376(4) 0.56742(11) 0.0530(11) Uani 1 1 d . . . H31A H 0.9773 0.9101 0.5711 0.079 Uiso 1 1 calc R . . H31B H 1.0280 0.8393 0.5498 0.079 Uiso 1 1 calc R . . H31C H 1.0187 0.8099 0.5894 0.079 Uiso 1 1 calc R . . C32 C 0.85290(18) 0.9087(3) 0.56430(9) 0.0392(9) Uani 1 1 d . . . C33 C 0.85490(19) 0.9237(3) 0.60082(10) 0.0436(9) Uani 1 1 d . . . C34 C 0.8351(2) 1.0222(4) 0.61308(11) 0.0500(10) Uani 1 1 d . . . H34 H 0.8361 1.0325 0.6375 0.060 Uiso 1 1 calc R . . C35 C 0.8140(2) 1.1057(4) 0.59100(11) 0.0499(10) Uani 1 1 d . . . H35 H 0.8009 1.1725 0.6001 0.060 Uiso 1 1 calc R . . C36 C 0.8122(2) 1.0910(3) 0.55533(10) 0.0461(10) Uani 1 1 d . . . H36 H 0.7984 1.1487 0.5400 0.055 Uiso 1 1 calc R . . C37 C 0.83040(19) 0.9933(3) 0.54154(10) 0.0409(9) Uani 1 1 d . . . C38 C 0.8755(2) 0.8352(4) 0.62701(10) 0.0515(11) Uani 1 1 d . . . H38 H 0.8932 0.7731 0.6142 0.062 Uiso 1 1 calc R . . C39 C 0.9346(3) 0.8700(5) 0.65511(12) 0.0684(14) Uani 1 1 d . . . H39A H 0.9763 0.8922 0.6440 0.103 Uiso 1 1 calc R . . H39B H 0.9473 0.8100 0.6709 0.103 Uiso 1 1 calc R . . H39C H 0.9179 0.9300 0.6683 0.103 Uiso 1 1 calc R . . C40 C 0.8101(2) 0.7983(4) 0.64413(12) 0.0633(13) Uani 1 1 d . . . H40A H 0.8239 0.7408 0.6608 0.095 Uiso 1 1 calc R . . H40B H 0.7738 0.7718 0.6262 0.095 Uiso 1 1 calc R . . H40C H 0.7911 0.8586 0.6564 0.095 Uiso 1 1 calc R . . C41 C 0.8255(2) 0.9796(3) 0.50227(10) 0.0451(9) Uani 1 1 d . . . H41 H 0.8380 0.9036 0.4977 0.054 Uiso 1 1 calc R . . C42 C 0.7495(3) 0.9978(4) 0.48531(13) 0.0694(14) Uani 1 1 d . . . H42A H 0.7170 0.9511 0.4963 0.104 Uiso 1 1 calc R . . H42B H 0.7467 0.9813 0.4604 0.104 Uiso 1 1 calc R . . H42C H 0.7362 1.0727 0.4884 0.104 Uiso 1 1 calc R . . C43 C 0.8779(3) 1.0501(4) 0.48538(11) 0.0614(12) Uani 1 1 d . . . H43A H 0.9261 1.0371 0.4966 0.092 Uiso 1 1 calc R . . H43B H 0.8656 1.1255 0.4882 0.092 Uiso 1 1 calc R . . H43C H 0.8757 1.0330 0.4605 0.092 Uiso 1 1 calc R . . Mg2 Mg 0.54416(6) 0.86895(10) 0.33232(3) 0.0356(3) Uani 1 1 d . . . S3 S 0.62861(5) 0.73092(8) 0.35928(2) 0.0415(2) Uani 1 1 d . . . S4 S 0.38783(6) 1.05241(8) 0.39714(3) 0.0468(3) Uani 1 1 d . . . N5 N 0.48567(15) 0.7919(2) 0.37204(8) 0.0363(7) Uani 1 1 d . . . N6 N 0.47038(15) 0.9959(2) 0.35081(8) 0.0379(7) Uani 1 1 d . . . N7 N 0.61630(16) 0.9632(3) 0.30983(8) 0.0398(7) Uani 1 1 d . . . N8 N 0.48921(16) 0.8290(3) 0.28492(8) 0.0397(7) Uani 1 1 d . . . C44 C 0.56582(19) 0.6445(3) 0.37401(9) 0.0366(8) Uani 1 1 d . . . C45 C 0.5797(2) 0.5366(3) 0.38135(10) 0.0433(9) Uani 1 1 d . . . H45 H 0.6239 0.5070 0.3769 0.052 Uiso 1 1 calc R . . C46 C 0.5304(2) 0.4721(3) 0.39488(10) 0.0471(10) Uani 1 1 d . . . H46 H 0.5415 0.3991 0.3997 0.056 Uiso 1 1 calc R . . C47 C 0.4646(2) 0.5126(3) 0.40153(11) 0.0486(10) Uani 1 1 d . . . H47 H 0.4310 0.4679 0.4110 0.058 Uiso 1 1 calc R . . C48 C 0.4494(2) 0.6178(3) 0.39423(10) 0.0414(9) Uani 1 1 d . . . H48 H 0.4046 0.6462 0.3984 0.050 Uiso 1 1 calc R . . C49 C 0.49900(19) 0.6836(3) 0.38071(9) 0.0369(8) Uani 1 1 d . . . C50 C 0.4499(2) 0.8532(3) 0.39011(10) 0.0424(9) Uani 1 1 d . . . H50 H 0.4311 0.8285 0.4105 0.051 Uiso 1 1 calc R . . C51 C 0.4397(2) 0.9624(3) 0.37785(10) 0.0406(9) Uani 1 1 d . . . C52 C 0.40612(19) 1.1465(3) 0.36640(9) 0.0383(8) Uani 1 1 d . . . C53 C 0.3838(2) 1.2518(3) 0.36296(10) 0.0436(9) Uani 1 1 d . . . H53 H 0.3539 1.2817 0.3786 0.052 Uiso 1 1 calc R . . C54 C 0.4059(2) 1.3122(4) 0.33634(11) 0.0499(10) Uani 1 1 d . . . H54 H 0.3917 1.3849 0.3338 0.060 Uiso 1 1 calc R . . C55 C 0.4493(2) 1.2672(3) 0.31304(11) 0.0523(11) Uani 1 1 d . . . H55 H 0.4636 1.3100 0.2947 0.063 Uiso 1 1 calc R . . C56 C 0.4716(2) 1.1630(3) 0.31608(10) 0.0490(10) Uani 1 1 d . . . H56 H 0.5005 1.1334 0.2999 0.059 Uiso 1 1 calc R . . C57 C 0.45118(19) 1.1012(3) 0.34339(9) 0.0384(8) Uani 1 1 d . . . C58 C 0.6415(2) 1.1258(4) 0.36440(13) 0.0614(12) Uani 1 1 d . . . H58 H 0.5972 1.1080 0.3489 0.074 Uiso 1 1 calc R . . C59 C 0.6282(3) 1.0971(6) 0.40116(14) 0.0911(19) Uani 1 1 d . . . H59A H 0.6199 1.0200 0.4027 0.137 Uiso 1 1 calc R . . H59B H 0.5865 1.1359 0.4073 0.137 Uiso 1 1 calc R . . H59C H 0.6697 1.1168 0.4173 0.137 Uiso 1 1 calc R . . C60 C 0.6541(3) 1.2464(4) 0.36063(18) 0.0899(19) Uani 1 1 d . . . H60A H 0.6617 1.2626 0.3365 0.135 Uiso 1 1 calc R . . H60B H 0.6961 1.2677 0.3762 0.135 Uiso 1 1 calc R . . H60C H 0.6127 1.2859 0.3668 0.135 Uiso 1 1 calc R . . C61 C 0.7311(2) 0.8359(4) 0.28713(11) 0.0536(11) Uani 1 1 d . . . H62 H 0.6787 0.8252 0.2821 0.064 Uiso 1 1 calc R . . C62 C 0.7595(3) 0.8684(5) 0.25291(14) 0.0875(18) Uani 1 1 d . . . H62A H 0.7382 0.9366 0.2448 0.131 Uiso 1 1 calc R . . H62B H 0.7473 0.8131 0.2353 0.131 Uiso 1 1 calc R . . H62C H 0.8112 0.8761 0.2568 0.131 Uiso 1 1 calc R . . C63 C 0.7641(2) 0.7288(4) 0.29948(11) 0.0570(11) Uani 1 1 d . . . H63A H 0.7458 0.7075 0.3212 0.085 Uiso 1 1 calc R . . H63B H 0.8158 0.7361 0.3035 0.085 Uiso 1 1 calc R . . H63C H 0.7517 0.6741 0.2816 0.085 Uiso 1 1 calc R . . C64 C 0.68745(19) 0.9828(3) 0.32584(10) 0.0423(9) Uani 1 1 d . . . C65 C 0.7008(2) 1.0589(4) 0.35202(12) 0.0533(11) Uani 1 1 d . . . C66 C 0.7704(3) 1.0769(4) 0.36637(14) 0.0723(15) Uani 1 1 d . . . H66 H 0.7798 1.1284 0.3844 0.087 Uiso 1 1 calc R . . C67 C 0.8260(2) 1.0206(4) 0.35474(16) 0.0758(15) Uani 1 1 d . . . H67 H 0.8734 1.0345 0.3644 0.091 Uiso 1 1 calc R . . C68 C 0.8125(2) 0.9449(4) 0.32930(13) 0.0635(13) Uani 1 1 d . . . H68 H 0.8510 0.9068 0.3214 0.076 Uiso 1 1 calc R . . C69 C 0.7435(2) 0.9224(3) 0.31473(11) 0.0470(10) Uani 1 1 d . . . C70 C 0.6410(2) 1.1005(4) 0.26683(12) 0.0584(12) Uani 1 1 d . . . H70A H 0.6813 1.1148 0.2844 0.088 Uiso 1 1 calc R . . H70B H 0.6113 1.1646 0.2635 0.088 Uiso 1 1 calc R . . H70C H 0.6585 1.0810 0.2448 0.088 Uiso 1 1 calc R . . C71 C 0.5976(2) 1.0095(3) 0.27897(10) 0.0426(9) Uani 1 1 d . . . C72 C 0.5375(2) 0.9802(3) 0.25639(10) 0.0453(10) Uani 1 1 d . . . H72 H 0.5259 1.0274 0.2373 0.054 Uiso 1 1 calc R . . C73 C 0.4914(2) 0.8919(3) 0.25753(10) 0.0431(9) Uani 1 1 d . . . C74 C 0.4434(3) 0.8720(4) 0.22384(11) 0.0584(12) Uani 1 1 d . . . H74A H 0.4129 0.8101 0.2268 0.088 Uiso 1 1 calc R . . H74B H 0.4725 0.8579 0.2049 0.088 Uiso 1 1 calc R . . H74C H 0.4138 0.9351 0.2181 0.088 Uiso 1 1 calc R . . C75 C 0.3381(2) 0.8345(4) 0.29786(13) 0.0657(13) Uani 1 1 d . . . H75 H 0.3749 0.8912 0.3031 0.079 Uiso 1 1 calc R . . C76 C 0.2831(3) 0.8767(6) 0.26887(17) 0.099(2) Uani 1 1 d . . . H76A H 0.3060 0.8885 0.2476 0.149 Uiso 1 1 calc R . . H76B H 0.2634 0.9443 0.2763 0.149 Uiso 1 1 calc R . . H76C H 0.2448 0.8242 0.2642 0.149 Uiso 1 1 calc R . . C77 C 0.3014(3) 0.8170(5) 0.33091(15) 0.0819(17) Uani 1 1 d . . . H77A H 0.3364 0.7923 0.3498 0.123 Uiso 1 1 calc R . . H77B H 0.2640 0.7632 0.3263 0.123 Uiso 1 1 calc R . . H77C H 0.2805 0.8845 0.3377 0.123 Uiso 1 1 calc R . . C78 C 0.5595(2) 0.6322(3) 0.27038(11) 0.0501(10) Uani 1 1 d . . . H78 H 0.5823 0.6929 0.2843 0.060 Uiso 1 1 calc R . . C79 C 0.5753(3) 0.6481(4) 0.23272(12) 0.0663(13) Uani 1 1 d . . . H79A H 0.5529 0.7144 0.2235 0.099 Uiso 1 1 calc R . . H79B H 0.5564 0.5875 0.2185 0.099 Uiso 1 1 calc R . . H79C H 0.6267 0.6528 0.2320 0.099 Uiso 1 1 calc R . . C80 C 0.5943(3) 0.5294(4) 0.28525(12) 0.0634(13) Uani 1 1 d . . . H80A H 0.5836 0.5198 0.3093 0.095 Uiso 1 1 calc R . . H80B H 0.6458 0.5341 0.2849 0.095 Uiso 1 1 calc R . . H80C H 0.5758 0.4684 0.2711 0.095 Uiso 1 1 calc R . . C81 C 0.4474(2) 0.7331(3) 0.28148(10) 0.0441(9) Uani 1 1 d . . . C82 C 0.3751(2) 0.7346(4) 0.28724(11) 0.0518(10) Uani 1 1 d . . . C83 C 0.3370(3) 0.6391(4) 0.28301(13) 0.0674(13) Uani 1 1 d . . . H83 H 0.2882 0.6386 0.2864 0.081 Uiso 1 1 calc R . . C84 C 0.3681(3) 0.5465(4) 0.27411(14) 0.0717(14) Uani 1 1 d . . . H84 H 0.3408 0.4830 0.2708 0.086 Uiso 1 1 calc R . . C85 C 0.4402(3) 0.5449(4) 0.26983(13) 0.0637(12) Uani 1 1 d . . . H85 H 0.4619 0.4797 0.2641 0.076 Uiso 1 1 calc R . . C86 C 0.4803(2) 0.6370(3) 0.27391(10) 0.0482(10) Uani 1 1 d . . . O101 O 0.9677(3) 0.7473(5) 0.31096(14) 0.1343(19) Uani 1 1 d DU . . C102 C 1.0239(3) 0.6805(6) 0.3253(2) 0.109(2) Uani 1 1 d DU . . H10A H 1.0102 0.6042 0.3230 0.130 Uiso 1 1 calc R . . H10B H 1.0368 0.6968 0.3503 0.130 Uiso 1 1 calc R . . C103 C 1.0853(5) 0.7054(8) 0.3044(4) 0.209(5) Uani 1 1 d DU . . H10C H 1.1310 0.6992 0.3194 0.250 Uiso 1 1 calc R . . H10D H 1.0857 0.6543 0.2848 0.250 Uiso 1 1 calc R . . C104 C 1.0767(4) 0.8055(8) 0.2921(3) 0.183(5) Uani 1 1 d DU . . H10E H 1.0906 0.8113 0.2682 0.219 Uiso 1 1 calc R . . H10F H 1.1047 0.8572 0.3074 0.219 Uiso 1 1 calc R . . C105 C 0.9975(4) 0.8232(9) 0.2925(3) 0.189(5) Uani 1 1 d DU . . H10G H 0.9896 0.8943 0.3027 0.227 Uiso 1 1 calc R . . H10H H 0.9742 0.8230 0.2682 0.227 Uiso 1 1 calc R . . O201 O 0.8745(4) 0.5325(6) 0.3610(3) 0.226(4) Uani 1 1 d DU . . C202 C 0.8235(4) 0.4566(8) 0.3440(2) 0.141(3) Uani 1 1 d DU . . H20B H 0.7886 0.4343 0.3598 0.169 Uiso 1 1 calc R . . H20C H 0.7979 0.4879 0.3226 0.169 Uiso 1 1 calc R . . C203 C 0.8671(6) 0.3671(9) 0.3356(3) 0.201(5) Uani 1 1 d DU . . H20D H 0.8420 0.2988 0.3386 0.241 Uiso 1 1 calc R . . H20E H 0.8776 0.3720 0.3111 0.241 Uiso 1 1 calc R . . C204 C 0.9286(6) 0.3710(10) 0.3576(3) 0.184(5) Uani 1 1 d DU . . H20F H 0.9696 0.3554 0.3447 0.221 Uiso 1 1 calc R . . H20G H 0.9274 0.3169 0.3763 0.221 Uiso 1 1 calc R . . C205 C 0.9352(4) 0.4735(8) 0.3722(3) 0.148(3) Uani 1 1 d DU . . H20H H 0.9412 0.4685 0.3979 0.178 Uiso 1 1 calc R . . H20I H 0.9776 0.5094 0.3648 0.178 Uiso 1 1 calc R . . O301 O 0.4656(4) 0.9283(6) 0.46656(18) 0.0772(19) Uani 0.50 1 d PDU A -1 C302 C 0.4259(6) 0.9695(15) 0.4921(3) 0.075(4) Uani 0.50 1 d PDU A -1 H30A H 0.3987 0.9116 0.5020 0.090 Uiso 0.50 1 calc PR A -1 H30B H 0.3921 1.0242 0.4819 0.090 Uiso 0.50 1 calc PR A -1 C303 C 0.4757(7) 1.017(2) 0.5194(5) 0.092(6) Uani 0.50 1 d PDU A -1 H30C H 0.4602 1.0907 0.5246 0.110 Uiso 0.50 1 calc PR A -1 H30D H 0.4773 0.9743 0.5410 0.110 Uiso 0.50 1 calc PR A -1 C304 C 0.5428(7) 1.020(2) 0.5077(5) 0.104(5) Uani 0.50 1 d PDU A -1 H30E H 0.5788 0.9885 0.5253 0.125 Uiso 0.50 1 calc PR A -1 H30F H 0.5567 1.0947 0.5032 0.125 Uiso 0.50 1 calc PR A -1 C305 C 0.5373(7) 0.9578(18) 0.4756(5) 0.079(4) Uani 0.50 1 d PDU A -1 H30G H 0.5542 1.0007 0.4567 0.094 Uiso 0.50 1 calc PR A -1 H30H H 0.5672 0.8929 0.4790 0.094 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 0.0279(6) 0.0416(8) 0.0423(7) 0.0021(5) 0.0092(5) 0.0032(5) S1 0.0310(4) 0.0507(6) 0.0423(5) -0.0055(4) 0.0098(4) 0.0018(4) S2 0.0334(5) 0.1512(14) 0.0405(6) 0.0073(7) 0.0110(4) -0.0135(7) N1 0.0285(14) 0.0385(19) 0.0430(17) -0.0005(13) 0.0112(12) 0.0020(13) N2 0.0289(15) 0.0425(19) 0.0439(17) -0.0015(14) 0.0103(13) -0.0006(13) N3 0.0316(16) 0.042(2) 0.0562(19) 0.0050(15) 0.0134(14) 0.0050(14) N4 0.0305(15) 0.045(2) 0.0421(17) 0.0067(14) 0.0082(13) 0.0035(14) C1 0.0315(17) 0.032(2) 0.0434(19) 0.0053(15) 0.0106(15) 0.0027(15) C2 0.0367(19) 0.041(2) 0.043(2) 0.0022(16) 0.0154(16) -0.0008(17) C3 0.0307(18) 0.051(3) 0.052(2) 0.0043(18) 0.0151(16) -0.0036(17) C4 0.0335(19) 0.051(3) 0.054(2) -0.0004(19) 0.0097(17) -0.0066(18) C5 0.0359(19) 0.050(3) 0.042(2) -0.0035(17) 0.0122(16) -0.0024(17) C6 0.0280(17) 0.036(2) 0.045(2) 0.0022(16) 0.0107(15) 0.0020(15) C7 0.0325(19) 0.063(3) 0.040(2) -0.0020(18) 0.0080(15) 0.0012(18) C8 0.038(2) 0.064(3) 0.039(2) -0.0029(18) 0.0127(16) -0.0007(19) C9 0.0302(18) 0.043(2) 0.047(2) -0.0042(17) 0.0129(15) -0.0016(16) C10 0.033(2) 0.096(4) 0.047(2) 0.000(2) 0.0110(17) -0.005(2) C11 0.041(2) 0.131(5) 0.050(3) 0.009(3) 0.015(2) -0.011(3) C12 0.032(2) 0.084(3) 0.056(3) 0.004(2) 0.0163(18) -0.003(2) C13 0.0302(18) 0.047(3) 0.058(2) -0.0068(19) 0.0110(17) -0.0023(17) C14 0.0348(19) 0.053(3) 0.047(2) -0.0021(18) 0.0117(16) -0.0006(18) C15 0.049(2) 0.044(3) 0.073(3) -0.001(2) 0.008(2) 0.006(2) C16 0.062(3) 0.099(5) 0.087(4) 0.014(3) 0.029(3) 0.031(3) C17 0.061(3) 0.063(3) 0.078(3) -0.016(3) 0.001(2) 0.013(2) C18 0.0301(19) 0.040(2) 0.073(3) 0.007(2) 0.0150(18) 0.0122(17) C19 0.034(2) 0.041(3) 0.078(3) 0.000(2) 0.0114(19) 0.0133(18) C20 0.041(2) 0.043(3) 0.098(4) -0.010(2) 0.014(2) 0.008(2) C21 0.043(2) 0.047(3) 0.116(4) -0.005(3) 0.032(3) 0.004(2) C22 0.044(2) 0.051(3) 0.102(4) 0.010(3) 0.038(2) 0.006(2) C23 0.037(2) 0.050(3) 0.080(3) 0.006(2) 0.022(2) 0.0089(19) C24 0.052(3) 0.067(3) 0.076(3) 0.009(2) 0.026(2) -0.007(2) C25 0.059(3) 0.218(9) 0.089(4) -0.016(5) 0.011(3) 0.028(5) C26 0.058(3) 0.057(3) 0.082(3) 0.008(2) 0.030(2) 0.007(2) C27 0.037(2) 0.050(3) 0.107(4) 0.009(3) 0.018(2) 0.012(2) C28 0.033(2) 0.047(3) 0.064(3) 0.0091(19) 0.0165(18) 0.0088(18) C29 0.0286(18) 0.053(3) 0.061(2) 0.011(2) 0.0112(17) 0.0092(18) C30 0.0315(18) 0.058(3) 0.040(2) 0.0073(18) 0.0075(15) -0.0016(18) C31 0.032(2) 0.073(3) 0.054(2) 0.005(2) 0.0051(17) -0.002(2) C32 0.0260(17) 0.047(2) 0.045(2) 0.0023(17) 0.0057(15) -0.0047(16) C33 0.0311(18) 0.056(3) 0.044(2) 0.0033(18) 0.0065(16) -0.0047(18) C34 0.040(2) 0.066(3) 0.045(2) -0.005(2) 0.0099(17) -0.003(2) C35 0.037(2) 0.054(3) 0.060(3) -0.010(2) 0.0112(18) -0.0009(19) C36 0.038(2) 0.049(3) 0.052(2) 0.0041(19) 0.0051(17) 0.0015(18) C37 0.0311(18) 0.046(2) 0.045(2) 0.0017(17) 0.0050(15) -0.0027(17) C38 0.049(2) 0.067(3) 0.039(2) 0.0069(19) 0.0058(17) -0.004(2) C39 0.058(3) 0.091(4) 0.053(3) 0.015(3) -0.006(2) -0.009(3) C40 0.062(3) 0.078(4) 0.050(2) 0.010(2) 0.009(2) -0.016(3) C41 0.051(2) 0.038(2) 0.045(2) 0.0049(17) 0.0003(17) -0.0001(18) C42 0.073(3) 0.068(3) 0.062(3) 0.006(2) -0.015(2) -0.004(3) C43 0.077(3) 0.064(3) 0.044(2) 0.002(2) 0.011(2) -0.015(3) Mg2 0.0320(6) 0.0371(7) 0.0394(6) 0.0000(5) 0.0115(5) -0.0003(5) S3 0.0314(5) 0.0511(6) 0.0434(5) 0.0062(4) 0.0099(4) 0.0007(4) S4 0.0520(6) 0.0385(6) 0.0546(6) 0.0015(4) 0.0273(5) 0.0063(5) N5 0.0313(15) 0.0337(18) 0.0451(17) 0.0001(13) 0.0101(13) 0.0013(13) N6 0.0340(15) 0.0366(19) 0.0453(17) -0.0011(14) 0.0140(13) -0.0002(14) N7 0.0356(16) 0.043(2) 0.0431(17) -0.0013(14) 0.0146(13) -0.0009(14) N8 0.0368(16) 0.0398(19) 0.0435(17) 0.0010(14) 0.0097(13) 0.0039(14) C44 0.0373(19) 0.038(2) 0.0357(18) -0.0007(15) 0.0078(15) 0.0011(16) C45 0.042(2) 0.045(3) 0.044(2) -0.0009(17) 0.0094(17) 0.0069(18) C46 0.059(3) 0.031(2) 0.052(2) 0.0021(17) 0.0115(19) 0.0008(19) C47 0.049(2) 0.042(3) 0.056(2) 0.0015(19) 0.0130(19) -0.0063(19) C48 0.039(2) 0.035(2) 0.053(2) -0.0005(17) 0.0146(17) -0.0047(17) C49 0.0374(19) 0.033(2) 0.042(2) -0.0002(15) 0.0109(15) -0.0013(16) C50 0.045(2) 0.039(2) 0.046(2) 0.0024(17) 0.0190(17) 0.0010(18) C51 0.040(2) 0.038(2) 0.046(2) 0.0012(17) 0.0163(16) 0.0014(17) C52 0.0378(19) 0.033(2) 0.046(2) -0.0027(16) 0.0105(16) -0.0003(16) C53 0.045(2) 0.041(2) 0.047(2) -0.0024(17) 0.0118(17) 0.0044(18) C54 0.055(2) 0.041(2) 0.055(2) 0.0048(19) 0.0123(19) 0.007(2) C55 0.060(3) 0.046(3) 0.055(2) 0.0116(19) 0.023(2) 0.009(2) C56 0.051(2) 0.052(3) 0.047(2) 0.0049(19) 0.0181(18) 0.009(2) C57 0.0370(19) 0.035(2) 0.045(2) -0.0028(16) 0.0114(16) 0.0022(16) C58 0.051(3) 0.058(3) 0.075(3) -0.021(2) 0.010(2) -0.001(2) C59 0.073(4) 0.125(6) 0.079(4) -0.013(4) 0.022(3) 0.017(4) C60 0.078(4) 0.064(4) 0.130(5) -0.032(3) 0.022(4) -0.001(3) C61 0.042(2) 0.065(3) 0.057(2) -0.001(2) 0.0206(19) 0.008(2) C62 0.116(5) 0.086(4) 0.068(3) 0.014(3) 0.041(3) 0.031(4) C63 0.055(3) 0.063(3) 0.057(3) -0.004(2) 0.025(2) 0.004(2) C64 0.0326(19) 0.041(2) 0.055(2) 0.0030(18) 0.0146(16) -0.0058(17) C65 0.041(2) 0.046(3) 0.074(3) -0.008(2) 0.012(2) -0.0041(19) C66 0.052(3) 0.069(4) 0.094(4) -0.028(3) 0.002(3) -0.008(2) C67 0.036(2) 0.077(4) 0.115(4) -0.019(3) 0.010(3) -0.007(2) C68 0.035(2) 0.068(3) 0.090(3) -0.006(3) 0.020(2) -0.003(2) C69 0.039(2) 0.048(3) 0.057(2) 0.0036(19) 0.0194(18) -0.0026(18) C70 0.056(3) 0.056(3) 0.067(3) 0.015(2) 0.025(2) -0.003(2) C71 0.045(2) 0.039(2) 0.047(2) 0.0022(17) 0.0196(18) 0.0034(18) C72 0.055(2) 0.040(2) 0.043(2) 0.0076(17) 0.0153(18) 0.0059(19) C73 0.048(2) 0.039(2) 0.043(2) -0.0005(17) 0.0112(17) 0.0091(18) C74 0.074(3) 0.055(3) 0.045(2) 0.001(2) 0.000(2) 0.002(2) C75 0.045(2) 0.065(3) 0.088(3) -0.001(3) 0.011(2) -0.001(2) C76 0.080(4) 0.102(5) 0.116(5) 0.020(4) 0.012(4) 0.035(4) C77 0.041(2) 0.114(5) 0.092(4) -0.008(3) 0.016(2) -0.001(3) C78 0.055(2) 0.042(3) 0.053(2) -0.0068(19) 0.0029(19) 0.007(2) C79 0.067(3) 0.072(4) 0.061(3) 0.002(2) 0.009(2) 0.007(3) C80 0.074(3) 0.056(3) 0.059(3) -0.006(2) 0.001(2) 0.017(2) C81 0.046(2) 0.042(2) 0.042(2) 0.0005(17) 0.0003(17) -0.0030(19) C82 0.044(2) 0.051(3) 0.059(3) 0.003(2) 0.0012(19) -0.006(2) C83 0.050(3) 0.072(4) 0.078(3) 0.006(3) -0.001(2) -0.011(3) C84 0.071(3) 0.051(3) 0.089(4) 0.005(3) -0.008(3) -0.022(3) C85 0.070(3) 0.044(3) 0.074(3) 0.002(2) -0.006(2) -0.004(2) C86 0.054(2) 0.042(3) 0.047(2) 0.0004(18) -0.0015(18) -0.001(2) O101 0.084(3) 0.189(6) 0.130(4) 0.036(4) 0.011(3) 0.018(3) C102 0.084(4) 0.109(5) 0.133(6) 0.015(4) 0.014(4) 0.006(4) C103 0.105(6) 0.164(9) 0.370(15) 0.130(10) 0.083(8) 0.027(6) C104 0.124(6) 0.191(9) 0.246(10) 0.146(8) 0.075(7) 0.050(6) C105 0.118(6) 0.217(10) 0.249(11) 0.149(9) 0.090(7) 0.063(6) O201 0.149(6) 0.161(6) 0.352(11) -0.036(7) -0.050(7) 0.017(5) C202 0.087(5) 0.172(8) 0.159(7) -0.052(6) -0.012(5) 0.009(5) C203 0.203(11) 0.154(9) 0.236(12) -0.049(8) -0.020(8) 0.056(8) C204 0.177(9) 0.213(10) 0.161(9) 0.013(8) 0.014(7) 0.115(9) C205 0.068(4) 0.178(8) 0.187(9) 0.064(7) -0.035(5) -0.013(5) O301 0.085(5) 0.078(5) 0.068(4) -0.012(4) 0.012(4) 0.014(4) C302 0.070(7) 0.093(10) 0.064(6) 0.006(6) 0.020(6) 0.023(7) C303 0.088(9) 0.108(15) 0.083(9) -0.033(8) 0.022(7) 0.030(10) C304 0.082(9) 0.121(13) 0.110(11) -0.032(9) 0.009(8) 0.004(11) C305 0.070(6) 0.068(10) 0.102(10) -0.007(7) 0.030(6) 0.031(7) _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 S1 2.4731(14) . ? Mg1 N1 2.211(3) . ? Mg1 N2 2.346(3) . ? Mg1 N3 2.063(3) . ? Mg1 N4 2.076(3) . ? S1 C1 1.750(4) . ? S2 C8 1.725(4) . ? S2 C10 1.726(4) . ? N1 C6 1.427(4) . ? N1 C7 1.273(5) . ? N2 C8 1.314(5) . ? N2 C9 1.396(4) . ? N3 C18 1.438(5) . ? N3 C28 1.332(5) . ? N4 C30 1.336(5) . ? N4 C32 1.436(5) . ? C1 C2 1.404(5) . ? C1 C6 1.409(5) . ? C2 H2 0.950 . ? C2 C3 1.380(5) . ? C3 H3 0.950 . ? C3 C4 1.383(5) . ? C4 H4 0.950 . ? C4 C5 1.388(5) . ? C5 H5 0.950 . ? C5 C6 1.393(5) . ? C7 H7 0.950 . ? C7 C8 1.464(5) . ? C9 C10 1.387(6) . ? C9 C14 1.399(5) . ? C10 C11 1.409(6) . ? C11 H11 0.950 . ? C11 C12 1.372(6) . ? C12 H12 0.950 . ? C12 C13 1.372(6) . ? C13 H13 0.950 . ? C13 C14 1.385(5) . ? C14 H14 0.950 . ? C15 H15 1.000 . ? C15 C16 1.546(6) . ? C15 C17 1.531(6) . ? C15 C19 1.511(6) . ? C16 H16A 0.980 . ? C16 H16B 0.980 . ? C16 H16C 0.980 . ? C17 H17A 0.980 . ? C17 H17B 0.980 . ? C17 H17C 0.980 . ? C18 C19 1.404(6) . ? C18 C23 1.414(6) . ? C19 C20 1.400(6) . ? C20 H20 0.950 . ? C20 C21 1.382(7) . ? C21 H21 0.950 . ? C21 C22 1.375(7) . ? C22 H22 0.950 . ? C22 C23 1.390(6) . ? C23 C24 1.515(7) . ? C24 H24 1.000 . ? C24 C25 1.517(8) . ? C24 C26 1.522(6) . ? C25 H25A 0.980 . ? C25 H25B 0.980 . ? C25 H25C 0.980 . ? C26 H26A 0.980 . ? C26 H26B 0.980 . ? C26 H26C 0.980 . ? C27 H27A 0.980 . ? C27 H27B 0.980 . ? C27 H27C 0.980 . ? C27 C28 1.521(6) . ? C28 C29 1.402(6) . ? C29 H29 0.950 . ? C29 C30 1.397(6) . ? C30 C31 1.514(6) . ? C31 H31A 0.980 . ? C31 H31B 0.980 . ? C31 H31C 0.980 . ? C32 C33 1.419(5) . ? C32 C37 1.411(5) . ? C33 C34 1.387(6) . ? C33 C38 1.520(6) . ? C34 H34 0.950 . ? C34 C35 1.379(6) . ? C35 H35 0.950 . ? C35 C36 1.386(6) . ? C36 H36 0.950 . ? C36 C37 1.392(6) . ? C37 C41 1.519(5) . ? C38 H38 1.000 . ? C38 C39 1.535(6) . ? C38 C40 1.539(6) . ? C39 H39A 0.980 . ? C39 H39B 0.980 . ? C39 H39C 0.980 . ? C40 H40A 0.980 . ? C40 H40B 0.980 . ? C40 H40C 0.980 . ? C41 H41 1.000 . ? C41 C42 1.533(6) . ? C41 C43 1.528(6) . ? C42 H42A 0.980 . ? C42 H42B 0.980 . ? C42 H42C 0.980 . ? C43 H43A 0.980 . ? C43 H43B 0.980 . ? C43 H43C 0.980 . ? Mg2 S3 2.5015(16) . ? Mg2 N5 2.211(3) . ? Mg2 N6 2.283(3) . ? Mg2 N7 2.069(3) . ? Mg2 N8 2.065(3) . ? S3 C44 1.750(4) . ? S4 C51 1.718(4) . ? S4 C52 1.734(4) . ? N5 C49 1.411(5) . ? N5 C50 1.280(5) . ? N6 C51 1.320(4) . ? N6 C57 1.387(5) . ? N7 C64 1.441(5) . ? N7 C71 1.337(5) . ? N8 C73 1.322(5) . ? N8 C81 1.436(5) . ? C44 C45 1.397(5) . ? C44 C49 1.409(5) . ? C45 H45 0.950 . ? C45 C46 1.380(5) . ? C46 H46 0.950 . ? C46 C47 1.397(6) . ? C47 H47 0.950 . ? C47 C48 1.370(6) . ? C48 H48 0.950 . ? C48 C49 1.394(5) . ? C50 H50 0.950 . ? C50 C51 1.451(5) . ? C52 C53 1.385(5) . ? C52 C57 1.418(5) . ? C53 H53 0.950 . ? C53 C54 1.379(5) . ? C54 H54 0.950 . ? C54 C55 1.403(6) . ? C55 H55 0.950 . ? C55 C56 1.371(6) . ? C56 H56 0.950 . ? C56 C57 1.397(5) . ? C58 H58 1.000 . ? C58 C59 1.513(7) . ? C58 C60 1.537(7) . ? C58 C65 1.519(6) . ? C59 H59A 0.980 . ? C59 H59B 0.980 . ? C59 H59C 0.980 . ? C60 H60A 0.980 . ? C60 H60B 0.980 . ? C60 H60C 0.980 . ? C61 H62 1.000 . ? C61 C62 1.536(6) . ? C61 C63 1.532(6) . ? C61 C69 1.519(6) . ? C62 H62A 0.980 . ? C62 H62B 0.980 . ? C62 H62C 0.980 . ? C63 H63A 0.980 . ? C63 H63B 0.980 . ? C63 H63C 0.980 . ? C64 C65 1.392(6) . ? C64 C69 1.409(5) . ? C65 C66 1.392(6) . ? C66 H66 0.950 . ? C66 C67 1.384(7) . ? C67 H67 0.950 . ? C67 C68 1.368(7) . ? C68 H68 0.950 . ? C68 C69 1.394(6) . ? C70 H70A 0.980 . ? C70 H70B 0.980 . ? C70 H70C 0.980 . ? C70 C71 1.508(5) . ? C71 C72 1.405(6) . ? C72 H72 0.950 . ? C72 C73 1.412(6) . ? C73 C74 1.524(6) . ? C74 H74A 0.980 . ? C74 H74B 0.980 . ? C74 H74C 0.980 . ? C75 H75 1.000 . ? C75 C76 1.536(7) . ? C75 C77 1.535(7) . ? C75 C82 1.512(7) . ? C76 H76A 0.980 . ? C76 H76B 0.980 . ? C76 H76C 0.980 . ? C77 H77A 0.980 . ? C77 H77B 0.980 . ? C77 H77C 0.980 . ? C78 H78 1.000 . ? C78 C79 1.531(6) . ? C78 C80 1.528(6) . ? C78 C86 1.524(6) . ? C79 H79A 0.980 . ? C79 H79B 0.980 . ? C79 H79C 0.980 . ? C80 H80A 0.980 . ? C80 H80B 0.980 . ? C80 H80C 0.980 . ? C81 C82 1.414(6) . ? C81 C86 1.400(6) . ? C82 C83 1.395(6) . ? C83 H83 0.950 . ? C83 C84 1.361(7) . ? C84 H84 0.950 . ? C84 C85 1.396(7) . ? C85 H85 0.950 . ? C85 C86 1.380(6) . ? O101 C102 1.418(7) . ? O101 C105 1.349(8) . ? C102 H10A 0.990 . ? C102 H10B 0.990 . ? C102 C103 1.524(9) . ? C103 H10C 0.990 . ? C103 H10D 0.990 . ? C103 C104 1.341(10) . ? C104 H10E 0.990 . ? C104 H10F 0.990 . ? C104 C105 1.521(9) . ? C105 H10G 0.990 . ? C105 H10H 0.990 . ? O201 C202 1.459(9) . ? O201 C205 1.396(9) . ? C202 H20B 0.990 . ? C202 H20C 0.990 . ? C202 C203 1.450(10) . ? C203 H20D 0.990 . ? C203 H20E 0.990 . ? C203 C204 1.367(11) . ? C204 H20F 0.990 . ? C204 H20G 0.990 . ? C204 C205 1.398(10) . ? C205 H20H 0.990 . ? C205 H20I 0.990 . ? O301 C302 1.405(11) . ? O301 C305 1.415(12) . ? C302 H30A 0.990 . ? C302 H30B 0.990 . ? C302 C303 1.461(13) . ? C303 H30C 0.990 . ? C303 H30D 0.990 . ? C303 C304 1.398(15) . ? C304 H30E 0.990 . ? C304 H30F 0.990 . ? C304 C305 1.456(13) . ? C305 H30G 0.990 . ? C305 H30H 0.990 . ? 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 S1 Mg1 N1 78.02(8) . . ? S1 Mg1 N2 142.31(9) . . ? S1 Mg1 N3 114.08(10) . . ? S1 Mg1 N4 96.01(10) . . ? N1 Mg1 N2 73.02(11) . . ? N1 Mg1 N3 113.45(14) . . ? N1 Mg1 N4 153.80(13) . . ? N2 Mg1 N3 99.46(12) . . ? N2 Mg1 N4 99.39(12) . . ? N3 Mg1 N4 92.37(13) . . ? Mg1 S1 C1 99.14(12) . . ? C8 S2 C10 88.77(19) . . ? Mg1 N1 C6 120.0(2) . . ? Mg1 N1 C7 118.2(2) . . ? C6 N1 C7 121.1(3) . . ? Mg1 N2 C8 110.4(2) . . ? Mg1 N2 C9 139.1(2) . . ? C8 N2 C9 109.8(3) . . ? Mg1 N3 C18 119.5(2) . . ? Mg1 N3 C28 120.0(3) . . ? C18 N3 C28 120.5(3) . . ? Mg1 N4 C30 119.9(3) . . ? Mg1 N4 C32 120.9(2) . . ? C30 N4 C32 119.3(3) . . ? S1 C1 C2 121.5(3) . . ? S1 C1 C6 121.7(3) . . ? C2 C1 C6 116.7(3) . . ? C1 C2 H2 119.3 . . ? C1 C2 C3 121.4(3) . . ? H2 C2 C3 119.3 . . ? C2 C3 H3 119.5 . . ? C2 C3 C4 120.9(3) . . ? H3 C3 C4 119.5 . . ? C3 C4 H4 120.3 . . ? C3 C4 C5 119.4(4) . . ? H4 C4 C5 120.3 . . ? C4 C5 H5 120.1 . . ? C4 C5 C6 119.8(3) . . ? H5 C5 C6 120.1 . . ? N1 C6 C1 115.7(3) . . ? N1 C6 C5 122.7(3) . . ? C1 C6 C5 121.6(3) . . ? N1 C7 H7 121.4 . . ? N1 C7 C8 117.2(3) . . ? H7 C7 C8 121.4 . . ? S2 C8 N2 116.4(3) . . ? S2 C8 C7 122.9(3) . . ? N2 C8 C7 120.5(3) . . ? N2 C9 C10 114.4(3) . . ? N2 C9 C14 126.1(3) . . ? C10 C9 C14 119.5(3) . . ? S2 C10 C9 110.6(3) . . ? S2 C10 C11 127.7(3) . . ? C9 C10 C11 121.7(4) . . ? C10 C11 H11 121.3 . . ? C10 C11 C12 117.5(4) . . ? H11 C11 C12 121.3 . . ? C11 C12 H12 119.4 . . ? C11 C12 C13 121.3(4) . . ? H12 C12 C13 119.4 . . ? C12 C13 H13 119.1 . . ? C12 C13 C14 121.9(4) . . ? H13 C13 C14 119.1 . . ? C9 C14 C13 118.1(4) . . ? C9 C14 H14 120.9 . . ? C13 C14 H14 120.9 . . ? H15 C15 C16 108.0 . . ? H15 C15 C17 108.0 . . ? H15 C15 C19 108.0 . . ? C16 C15 C17 108.7(4) . . ? C16 C15 C19 110.9(4) . . ? C17 C15 C19 113.1(4) . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16B 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17B 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N3 C18 C19 121.0(4) . . ? N3 C18 C23 118.6(4) . . ? C19 C18 C23 120.2(4) . . ? C15 C19 C18 122.2(4) . . ? C15 C19 C20 119.4(4) . . ? C18 C19 C20 118.4(4) . . ? C19 C20 H20 119.2 . . ? C19 C20 C21 121.6(5) . . ? H20 C20 C21 119.2 . . ? C20 C21 H21 120.4 . . ? C20 C21 C22 119.1(5) . . ? H21 C21 C22 120.4 . . ? C21 C22 H22 119.0 . . ? C21 C22 C23 122.0(5) . . ? H22 C22 C23 119.0 . . ? C18 C23 C22 118.5(5) . . ? C18 C23 C24 121.1(4) . . ? C22 C23 C24 120.3(4) . . ? C23 C24 H24 107.5 . . ? C23 C24 C25 111.4(5) . . ? C23 C24 C26 113.9(4) . . ? H24 C24 C25 107.5 . . ? H24 C24 C26 107.5 . . ? C25 C24 C26 108.8(4) . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25B 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26B 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? H27A C27 H27B 109.5 . . ? H27A C27 H27C 109.5 . . ? H27A C27 C28 109.5 . . ? H27B C27 H27C 109.5 . . ? H27B C27 C28 109.5 . . ? H27C C27 C28 109.5 . . ? N3 C28 C27 120.5(4) . . ? N3 C28 C29 124.2(4) . . ? C27 C28 C29 115.3(3) . . ? C28 C29 H29 114.8 . . ? C28 C29 C30 130.4(3) . . ? H29 C29 C30 114.8 . . ? N4 C30 C29 123.7(4) . . ? N4 C30 C31 120.2(4) . . ? C29 C30 C31 116.1(3) . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31B 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? N4 C32 C33 120.9(3) . . ? N4 C32 C37 119.3(3) . . ? C33 C32 C37 119.6(4) . . ? C32 C33 C34 118.6(4) . . ? C32 C33 C38 122.8(4) . . ? C34 C33 C38 118.6(4) . . ? C33 C34 H34 118.9 . . ? C33 C34 C35 122.2(4) . . ? H34 C34 C35 118.9 . . ? C34 C35 H35 120.4 . . ? C34 C35 C36 119.2(4) . . ? H35 C35 C36 120.4 . . ? C35 C36 H36 119.4 . . ? C35 C36 C37 121.1(4) . . ? H36 C36 C37 119.4 . . ? C32 C37 C36 119.4(3) . . ? C32 C37 C41 121.2(4) . . ? C36 C37 C41 119.4(3) . . ? C33 C38 H38 108.1 . . ? C33 C38 C39 112.2(4) . . ? C33 C38 C40 110.2(4) . . ? H38 C38 C39 108.1 . . ? H38 C38 C40 108.1 . . ? C39 C38 C40 109.9(3) . . ? C38 C39 H39A 109.5 . . ? C38 C39 H39B 109.5 . . ? C38 C39 H39C 109.5 . . ? H39A C39 H39B 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C38 C40 H40A 109.5 . . ? C38 C40 H40B 109.5 . . ? C38 C40 H40C 109.5 . . ? H40A C40 H40B 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C37 C41 H41 107.2 . . ? C37 C41 C42 111.1(3) . . ? C37 C41 C43 113.0(3) . . ? H41 C41 C42 107.2 . . ? H41 C41 C43 107.2 . . ? C42 C41 C43 110.9(4) . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42B 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C41 C43 H43A 109.5 . . ? C41 C43 H43B 109.5 . . ? C41 C43 H43C 109.5 . . ? H43A C43 H43B 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? S3 Mg2 N5 75.99(9) . . ? S3 Mg2 N6 137.40(9) . . ? S3 Mg2 N7 98.35(10) . . ? S3 Mg2 N8 116.04(10) . . ? N5 Mg2 N6 73.37(11) . . ? N5 Mg2 N7 161.02(13) . . ? N5 Mg2 N8 105.50(13) . . ? N6 Mg2 N7 101.07(12) . . ? N6 Mg2 N8 100.31(12) . . ? N7 Mg2 N8 93.30(13) . . ? Mg2 S3 C44 97.72(13) . . ? C51 S4 C52 88.86(18) . . ? Mg2 N5 C49 119.5(2) . . ? Mg2 N5 C50 117.0(3) . . ? C49 N5 C50 122.5(3) . . ? Mg2 N6 C51 111.5(2) . . ? Mg2 N6 C57 138.7(2) . . ? C51 N6 C57 109.7(3) . . ? Mg2 N7 C64 123.2(2) . . ? Mg2 N7 C71 119.9(3) . . ? C64 N7 C71 116.9(3) . . ? Mg2 N8 C73 120.5(3) . . ? Mg2 N8 C81 120.2(2) . . ? C73 N8 C81 119.3(3) . . ? S3 C44 C45 122.9(3) . . ? S3 C44 C49 120.2(3) . . ? C45 C44 C49 116.8(3) . . ? C44 C45 H45 119.3 . . ? C44 C45 C46 121.4(4) . . ? H45 C45 C46 119.3 . . ? C45 C46 H46 119.6 . . ? C45 C46 C47 120.9(4) . . ? H46 C46 C47 119.6 . . ? C46 C47 H47 120.5 . . ? C46 C47 C48 118.9(4) . . ? H47 C47 C48 120.5 . . ? C47 C48 H48 119.8 . . ? C47 C48 C49 120.5(4) . . ? H48 C48 C49 119.8 . . ? N5 C49 C44 115.5(3) . . ? N5 C49 C48 123.0(3) . . ? C44 C49 C48 121.5(3) . . ? N5 C50 H50 121.8 . . ? N5 C50 C51 116.4(3) . . ? H50 C50 C51 121.8 . . ? S4 C51 N6 117.3(3) . . ? S4 C51 C50 122.5(3) . . ? N6 C51 C50 120.2(3) . . ? S4 C52 C53 128.9(3) . . ? S4 C52 C57 109.8(3) . . ? C53 C52 C57 121.3(3) . . ? C52 C53 H53 120.8 . . ? C52 C53 C54 118.5(4) . . ? H53 C53 C54 120.8 . . ? C53 C54 H54 119.7 . . ? C53 C54 C55 120.5(4) . . ? H54 C54 C55 119.7 . . ? C54 C55 H55 119.2 . . ? C54 C55 C56 121.6(4) . . ? H55 C55 C56 119.2 . . ? C55 C56 H56 120.6 . . ? C55 C56 C57 118.8(4) . . ? H56 C56 C57 120.6 . . ? N6 C57 C52 114.4(3) . . ? N6 C57 C56 126.3(3) . . ? C52 C57 C56 119.3(4) . . ? H58 C58 C59 106.9 . . ? H58 C58 C60 106.9 . . ? H58 C58 C65 106.9 . . ? C59 C58 C60 111.4(5) . . ? C59 C58 C65 111.8(4) . . ? C60 C58 C65 112.4(4) . . ? C58 C59 H59A 109.5 . . ? C58 C59 H59B 109.5 . . ? C58 C59 H59C 109.5 . . ? H59A C59 H59B 109.5 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? C58 C60 H60A 109.5 . . ? C58 C60 H60B 109.5 . . ? C58 C60 H60C 109.5 . . ? H60A C60 H60B 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? H62 C61 C62 107.7 . . ? H62 C61 C63 107.7 . . ? H62 C61 C69 107.7 . . ? C62 C61 C63 109.2(4) . . ? C62 C61 C69 112.0(4) . . ? C63 C61 C69 112.2(4) . . ? C61 C62 H62A 109.5 . . ? C61 C62 H62B 109.5 . . ? C61 C62 H62C 109.5 . . ? H62A C62 H62B 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? C61 C63 H63A 109.5 . . ? C61 C63 H63B 109.5 . . ? C61 C63 H63C 109.5 . . ? H63A C63 H63B 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? N7 C64 C65 120.9(3) . . ? N7 C64 C69 118.7(4) . . ? C65 C64 C69 120.4(4) . . ? C58 C65 C64 121.6(4) . . ? C58 C65 C66 119.2(4) . . ? C64 C65 C66 119.2(4) . . ? C65 C66 H66 119.6 . . ? C65 C66 C67 120.8(5) . . ? H66 C66 C67 119.6 . . ? C66 C67 H67 120.1 . . ? C66 C67 C68 119.8(5) . . ? H67 C67 C68 120.1 . . ? C67 C68 H68 119.3 . . ? C67 C68 C69 121.5(4) . . ? H68 C68 C69 119.3 . . ? C61 C69 C64 122.1(4) . . ? C61 C69 C68 119.5(4) . . ? C64 C69 C68 118.4(4) . . ? H70A C70 H70B 109.5 . . ? H70A C70 H70C 109.5 . . ? H70A C70 C71 109.5 . . ? H70B C70 H70C 109.5 . . ? H70B C70 C71 109.5 . . ? H70C C70 C71 109.5 . . ? N7 C71 C70 120.3(4) . . ? N7 C71 C72 123.8(4) . . ? C70 C71 C72 115.9(4) . . ? C71 C72 H72 114.9 . . ? C71 C72 C73 130.3(4) . . ? H72 C72 C73 114.9 . . ? N8 C73 C72 124.4(4) . . ? N8 C73 C74 121.1(4) . . ? C72 C73 C74 114.5(3) . . ? C73 C74 H74A 109.5 . . ? C73 C74 H74B 109.5 . . ? C73 C74 H74C 109.5 . . ? H74A C74 H74B 109.5 . . ? H74A C74 H74C 109.5 . . ? H74B C74 H74C 109.5 . . ? H75 C75 C76 107.8 . . ? H75 C75 C77 107.8 . . ? H75 C75 C82 107.8 . . ? C76 C75 C77 108.8(4) . . ? C76 C75 C82 112.6(4) . . ? C77 C75 C82 112.0(4) . . ? C75 C76 H76A 109.5 . . ? C75 C76 H76B 109.5 . . ? C75 C76 H76C 109.5 . . ? H76A C76 H76B 109.5 . . ? H76A C76 H76C 109.5 . . ? H76B C76 H76C 109.5 . . ? C75 C77 H77A 109.5 . . ? C75 C77 H77B 109.5 . . ? C75 C77 H77C 109.5 . . ? H77A C77 H77B 109.5 . . ? H77A C77 H77C 109.5 . . ? H77B C77 H77C 109.5 . . ? H78 C78 C79 107.1 . . ? H78 C78 C80 107.1 . . ? H78 C78 C86 107.1 . . ? C79 C78 C80 110.2(4) . . ? C79 C78 C86 112.3(4) . . ? C80 C78 C86 112.9(4) . . ? C78 C79 H79A 109.5 . . ? C78 C79 H79B 109.5 . . ? C78 C79 H79C 109.5 . . ? H79A C79 H79B 109.5 . . ? H79A C79 H79C 109.5 . . ? H79B C79 H79C 109.5 . . ? C78 C80 H80A 109.5 . . ? C78 C80 H80B 109.5 . . ? C78 C80 H80C 109.5 . . ? H80A C80 H80B 109.5 . . ? H80A C80 H80C 109.5 . . ? H80B C80 H80C 109.5 . . ? N8 C81 C82 120.7(4) . . ? N8 C81 C86 118.8(3) . . ? C82 C81 C86 120.5(4) . . ? C75 C82 C81 122.7(4) . . ? C75 C82 C83 119.3(4) . . ? C81 C82 C83 117.9(4) . . ? C82 C83 H83 119.2 . . ? C82 C83 C84 121.6(5) . . ? H83 C83 C84 119.2 . . ? C83 C84 H84 120.0 . . ? C83 C84 C85 120.1(5) . . ? H84 C84 C85 120.0 . . ? C84 C85 H85 119.7 . . ? C84 C85 C86 120.6(5) . . ? H85 C85 C86 119.7 . . ? C78 C86 C81 121.3(4) . . ? C78 C86 C85 119.5(4) . . ? C81 C86 C85 119.2(4) . . ? C102 O101 C105 106.3(5) . . ? O101 C102 H10A 110.8 . . ? O101 C102 H10B 110.8 . . ? O101 C102 C103 104.9(6) . . ? H10A C102 H10B 108.8 . . ? H10A C102 C103 110.8 . . ? H10B C102 C103 110.8 . . ? C102 C103 H10C 110.1 . . ? C102 C103 H10D 110.1 . . ? C102 C103 C104 108.0(7) . . ? H10C C103 H10D 108.4 . . ? H10C C103 C104 110.1 . . ? H10D C103 C104 110.1 . . ? C103 C104 H10E 111.3 . . ? C103 C104 H10F 111.3 . . ? C103 C104 C105 102.4(7) . . ? H10E C104 H10F 109.2 . . ? H10E C104 C105 111.3 . . ? H10F C104 C105 111.3 . . ? O101 C105 C104 112.0(6) . . ? O101 C105 H10G 109.2 . . ? O101 C105 H10H 109.2 . . ? C104 C105 H10G 109.2 . . ? C104 C105 H10H 109.2 . . ? H10G C105 H10H 107.9 . . ? C202 O201 C205 106.1(7) . . ? O201 C202 H20B 111.0 . . ? O201 C202 H20C 111.0 . . ? O201 C202 C203 103.7(7) . . ? H20B C202 H20C 109.0 . . ? H20B C202 C203 111.0 . . ? H20C C202 C203 111.0 . . ? C202 C203 H20D 110.2 . . ? C202 C203 H20E 110.2 . . ? C202 C203 C204 107.5(8) . . ? H20D C203 H20E 108.5 . . ? H20D C203 C204 110.2 . . ? H20E C203 C204 110.2 . . ? C203 C204 H20F 110.0 . . ? C203 C204 H20G 110.0 . . ? C203 C204 C205 108.4(8) . . ? H20F C204 H20G 108.4 . . ? H20F C204 C205 110.0 . . ? H20G C204 C205 110.0 . . ? O201 C205 C204 109.1(7) . . ? O201 C205 H20H 109.9 . . ? O201 C205 H20I 109.9 . . ? C204 C205 H20H 109.9 . . ? C204 C205 H20I 109.9 . . ? H20H C205 H20I 108.3 . . ? C302 O301 C305 107.8(9) . . ? O301 C302 H30A 110.2 . . ? O301 C302 H30B 110.2 . . ? O301 C302 C303 107.7(10) . . ? H30A C302 H30B 108.5 . . ? H30A C302 C303 110.2 . . ? H30B C302 C303 110.2 . . ? C302 C303 H30C 110.0 . . ? C302 C303 H30D 110.0 . . ? C302 C303 C304 108.4(11) . . ? H30C C303 H30D 108.4 . . ? H30C C303 C304 110.0 . . ? H30D C303 C304 110.0 . . ? C303 C304 H30E 110.5 . . ? C303 C304 H30F 110.5 . . ? C303 C304 C305 106.3(11) . . ? H30E C304 H30F 108.7 . . ? H30E C304 C305 110.5 . . ? H30F C304 C305 110.5 . . ? O301 C305 C304 109.0(10) . . ? O301 C305 H30G 109.9 . . ? O301 C305 H30H 109.9 . . ? C304 C305 H30G 109.9 . . ? C304 C305 H30H 109.9 . . ? H30G C305 H30H 108.3 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 24.21 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.969 _refine_diff_density_min -0.551 _refine_diff_density_rms 0.059 # Contents of RES file _iucr_refine_instructions_details ; TITL eh3 in P2(1)/n CELL 0.6889 18.964 12.505 38.624 90.000 96.385 90.000 ZERR 8.00 0.005 0.003 0.010 0.000 0.003 0.000 LATT 1 SYMM 0.5-X, 0.5+Y, 0.5-Z SFAC C H N MG S O DISP Mg 0.04190 0.03438 148.53 DISP S 0.10019 0.11693 478.92 UNIT 384 480 32 8 16 10 TEMP -153 SIZE 0.01 0.02 0.10 L.S. 8 BOND $H ACTA FMAP 2 PLAN 10 SIMU O101 > C305 DELU O101 > C305 WGHT 0.067200 17.136303 EXTI 0.001985 FVAR 0.11852 MG1 4 0.787153 0.720465 0.520987 11.00000 0.02789 0.04161 = 0.04228 0.00214 0.00924 0.00325 S1 5 0.691455 0.771005 0.556401 11.00000 0.03098 0.05069 = 0.04232 -0.00548 0.00984 0.00178 S2 5 0.786043 0.776800 0.399918 11.00000 0.03340 0.15124 = 0.04047 0.00734 0.01100 -0.01346 N1 3 0.691656 0.705519 0.482895 11.00000 0.02855 0.03852 = 0.04301 -0.00046 0.01121 0.00199 N2 3 0.824351 0.741157 0.465430 11.00000 0.02895 0.04246 = 0.04390 -0.00150 0.01034 -0.00061 N3 3 0.834565 0.575798 0.534680 11.00000 0.03163 0.04240 = 0.05621 0.00502 0.01342 0.00505 N4 3 0.866912 0.805760 0.550071 11.00000 0.03045 0.04470 = 0.04211 0.00675 0.00818 0.00350 C1 1 0.618731 0.719433 0.529719 11.00000 0.03151 0.03209 = 0.04341 0.00533 0.01061 0.00274 C2 1 0.551682 0.709695 0.541595 11.00000 0.03673 0.04108 = 0.04335 0.00219 0.01538 -0.00079 AFIX 43 H2 2 0.545690 0.731122 0.564684 11.00000 -1.20000 AFIX 0 C3 1 0.494312 0.669666 0.520444 11.00000 0.03070 0.05062 = 0.05226 0.00427 0.01508 -0.00358 AFIX 43 H3 2 0.449730 0.663125 0.529291 11.00000 -1.20000 AFIX 0 C4 1 0.500791 0.638941 0.486555 11.00000 0.03355 0.05074 = 0.05401 -0.00040 0.00970 -0.00662 AFIX 43 H4 2 0.461187 0.610298 0.472328 11.00000 -1.20000 AFIX 0 C5 1 0.565664 0.650324 0.473515 11.00000 0.03591 0.04979 = 0.04211 -0.00354 0.01221 -0.00240 AFIX 43 H5 2 0.570532 0.630384 0.450166 11.00000 -1.20000 AFIX 0 C6 1 0.623636 0.691067 0.494751 11.00000 0.02796 0.03616 = 0.04518 0.00221 0.01074 0.00198 C7 1 0.697691 0.724742 0.450990 11.00000 0.03251 0.06285 = 0.04007 -0.00198 0.00803 0.00121 AFIX 43 H7 2 0.657386 0.727160 0.434039 11.00000 -1.20000 AFIX 0 C8 1 0.769347 0.742961 0.441526 11.00000 0.03752 0.06413 = 0.03887 -0.00294 0.01266 -0.00066 C9 1 0.885948 0.765649 0.450361 11.00000 0.03022 0.04257 = 0.04708 -0.00421 0.01289 -0.00161 C10 1 0.874997 0.786438 0.414903 11.00000 0.03281 0.09650 = 0.04715 0.00049 0.01104 -0.00474 C11 1 0.931415 0.813463 0.395714 11.00000 0.04061 0.13121 = 0.05009 0.00932 0.01540 -0.01053 AFIX 43 H11 2 0.923651 0.826495 0.371356 11.00000 -1.20000 AFIX 0 C12 1 0.997997 0.820244 0.413540 11.00000 0.03201 0.08428 = 0.05611 0.00374 0.01634 -0.00321 AFIX 43 H12 2 1.037041 0.838753 0.401316 11.00000 -1.20000 AFIX 0 C13 1 1.009285 0.800819 0.448670 11.00000 0.03019 0.04709 = 0.05835 -0.00680 0.01101 -0.00227 AFIX 43 H13 2 1.056030 0.806781 0.460223 11.00000 -1.20000 AFIX 0 C14 1 0.954498 0.772763 0.467786 11.00000 0.03479 0.05330 = 0.04739 -0.00205 0.01167 -0.00058 AFIX 43 H14 2 0.963237 0.758741 0.492058 11.00000 -1.20000 AFIX 0 C15 1 0.789374 0.454988 0.470340 11.00000 0.04875 0.04440 = 0.07272 -0.00076 0.00834 0.00561 AFIX 13 H15 2 0.812129 0.527185 0.472399 11.00000 -1.20000 AFIX 0 C16 1 0.844829 0.374474 0.459538 11.00000 0.06173 0.09882 = 0.08661 0.01354 0.02865 0.03057 AFIX 33 H16A 2 0.885023 0.370923 0.477789 11.00000 -1.50000 H16B 2 0.861563 0.397887 0.437656 11.00000 -1.50000 H16C 2 0.823045 0.303590 0.456324 11.00000 -1.50000 AFIX 0 C17 1 0.727398 0.460228 0.441382 11.00000 0.06069 0.06301 = 0.07801 -0.01567 0.00052 0.01306 AFIX 33 H17A 2 0.691982 0.511374 0.447872 11.00000 -1.50000 H17B 2 0.705671 0.389323 0.438099 11.00000 -1.50000 H17C 2 0.744871 0.483343 0.419641 11.00000 -1.50000 AFIX 0 C18 1 0.791338 0.481679 0.535946 11.00000 0.03005 0.04028 = 0.07302 0.00673 0.01497 0.01224 C19 1 0.766648 0.426015 0.505410 11.00000 0.03376 0.04137 = 0.07788 0.00007 0.01139 0.01329 C20 1 0.720206 0.340020 0.507911 11.00000 0.04071 0.04305 = 0.09811 -0.00959 0.01400 0.00836 AFIX 43 H20 2 0.702297 0.302826 0.487347 11.00000 -1.20000 AFIX 0 C21 1 0.699769 0.307897 0.539538 11.00000 0.04279 0.04697 = 0.11641 -0.00523 0.03225 0.00391 AFIX 43 H21 2 0.668805 0.248631 0.540766 11.00000 -1.20000 AFIX 0 C22 1 0.724845 0.362857 0.569211 11.00000 0.04382 0.05096 = 0.10225 0.01040 0.03798 0.00554 AFIX 43 H22 2 0.711323 0.340004 0.590982 11.00000 -1.20000 AFIX 0 C23 1 0.769387 0.450852 0.568305 11.00000 0.03723 0.04964 = 0.07993 0.00631 0.02233 0.00893 C24 1 0.792756 0.512782 0.601310 11.00000 0.05180 0.06656 = 0.07618 0.00927 0.02643 -0.00662 AFIX 13 H24 2 0.803553 0.587517 0.594342 11.00000 -1.20000 AFIX 0 C25 1 0.860142 0.466470 0.620374 11.00000 0.05895 0.21762 = 0.08883 -0.01637 0.01066 0.02765 AFIX 33 H25A 2 0.896951 0.463008 0.604498 11.00000 -1.50000 H25B 2 0.850605 0.394371 0.628641 11.00000 -1.50000 H25C 2 0.876401 0.512115 0.640300 11.00000 -1.50000 AFIX 0 C26 1 0.736579 0.519285 0.626485 11.00000 0.05784 0.05672 = 0.08164 0.00791 0.02950 0.00663 AFIX 33 H26A 2 0.755238 0.560098 0.647158 11.00000 -1.50000 H26B 2 0.724110 0.446958 0.633448 11.00000 -1.50000 H26C 2 0.694226 0.554984 0.615057 11.00000 -1.50000 AFIX 0 C27 1 0.942200 0.462384 0.543884 11.00000 0.03655 0.05032 = 0.10719 0.00909 0.01828 0.01207 AFIX 33 H27A 2 0.907070 0.405206 0.539274 11.00000 -1.50000 H27B 2 0.967988 0.452412 0.567087 11.00000 -1.50000 H27C 2 0.975702 0.460145 0.526322 11.00000 -1.50000 AFIX 0 C28 1 0.904713 0.570049 0.542285 11.00000 0.03321 0.04729 = 0.06382 0.00911 0.01649 0.00881 C29 1 0.949094 0.659159 0.548830 11.00000 0.02865 0.05271 = 0.06090 0.01136 0.01116 0.00918 AFIX 43 H29 2 0.998314 0.644639 0.549055 11.00000 -1.20000 AFIX 0 C30 1 0.932628 0.765839 0.555073 11.00000 0.03149 0.05774 = 0.03996 0.00726 0.00753 -0.00158 C31 1 0.994648 0.837624 0.567421 11.00000 0.03216 0.07312 = 0.05368 0.00547 0.00508 -0.00187 AFIX 33 H31A 2 0.977340 0.910124 0.571111 11.00000 -1.50000 H31B 2 1.028024 0.839347 0.549795 11.00000 -1.50000 H31C 2 1.018729 0.809871 0.589351 11.00000 -1.50000 AFIX 0 C32 1 0.852896 0.908707 0.564296 11.00000 0.02599 0.04717 = 0.04481 0.00234 0.00566 -0.00474 C33 1 0.854898 0.923671 0.600821 11.00000 0.03110 0.05598 = 0.04417 0.00333 0.00648 -0.00474 C34 1 0.835108 1.022195 0.613079 11.00000 0.04037 0.06597 = 0.04467 -0.00509 0.00986 -0.00329 AFIX 43 H34 2 0.836094 1.032504 0.637497 11.00000 -1.20000 AFIX 0 C35 1 0.814033 1.105746 0.590997 11.00000 0.03695 0.05385 = 0.06018 -0.01041 0.01122 -0.00093 AFIX 43 H35 2 0.800923 1.172520 0.600114 11.00000 -1.20000 AFIX 0 C36 1 0.812226 1.091037 0.555334 11.00000 0.03775 0.04871 = 0.05191 0.00412 0.00509 0.00147 AFIX 43 H36 2 0.798350 1.148658 0.540047 11.00000 -1.20000 AFIX 0 C37 1 0.830397 0.993275 0.541539 11.00000 0.03110 0.04633 = 0.04533 0.00168 0.00499 -0.00273 C38 1 0.875452 0.835238 0.627005 11.00000 0.04867 0.06692 = 0.03914 0.00693 0.00577 -0.00412 AFIX 13 H38 2 0.893203 0.773098 0.614171 11.00000 -1.20000 AFIX 0 C39 1 0.934590 0.870008 0.655115 11.00000 0.05779 0.09128 = 0.05338 0.01483 -0.00639 -0.00935 AFIX 33 H39A 2 0.976295 0.892186 0.644046 11.00000 -1.50000 H39B 2 0.947313 0.810006 0.670904 11.00000 -1.50000 H39C 2 0.917929 0.930039 0.668345 11.00000 -1.50000 AFIX 0 C40 1 0.810108 0.798263 0.644131 11.00000 0.06226 0.07815 = 0.05001 0.01016 0.00866 -0.01593 AFIX 33 H40A 2 0.823898 0.740830 0.660782 11.00000 -1.50000 H40B 2 0.773750 0.771839 0.626150 11.00000 -1.50000 H40C 2 0.791073 0.858577 0.656365 11.00000 -1.50000 AFIX 0 C41 1 0.825536 0.979575 0.502272 11.00000 0.05110 0.03810 = 0.04492 0.00489 0.00034 -0.00014 AFIX 13 H41 2 0.837999 0.903573 0.497675 11.00000 -1.20000 AFIX 0 C42 1 0.749502 0.997817 0.485310 11.00000 0.07268 0.06809 = 0.06213 0.00596 -0.01549 -0.00365 AFIX 33 H42A 2 0.716980 0.951128 0.496320 11.00000 -1.50000 H42B 2 0.746743 0.981327 0.460392 11.00000 -1.50000 H42C 2 0.736179 1.072658 0.488377 11.00000 -1.50000 AFIX 0 C43 1 0.877922 1.050119 0.485385 11.00000 0.07721 0.06398 = 0.04386 0.00230 0.01108 -0.01464 AFIX 33 H43A 2 0.926080 1.037073 0.496603 11.00000 -1.50000 H43B 2 0.865584 1.125484 0.488196 11.00000 -1.50000 H43C 2 0.875701 1.033043 0.460524 11.00000 -1.50000 AFIX 0 MG2 4 0.544163 0.868950 0.332320 11.00000 0.03199 0.03711 = 0.03937 0.00004 0.01147 -0.00033 S3 5 0.628613 0.730924 0.359281 11.00000 0.03136 0.05106 = 0.04336 0.00618 0.00991 0.00068 S4 5 0.387827 1.052410 0.397137 11.00000 0.05204 0.03847 = 0.05459 0.00147 0.02730 0.00634 N5 3 0.485668 0.791921 0.372039 11.00000 0.03130 0.03368 = 0.04510 0.00006 0.01012 0.00132 N6 3 0.470383 0.995943 0.350808 11.00000 0.03404 0.03662 = 0.04531 -0.00114 0.01398 -0.00016 N7 3 0.616300 0.963188 0.309831 11.00000 0.03559 0.04303 = 0.04310 -0.00131 0.01459 -0.00085 N8 3 0.489208 0.829042 0.284917 11.00000 0.03682 0.03984 = 0.04353 0.00104 0.00969 0.00392 C44 1 0.565819 0.644458 0.374011 11.00000 0.03733 0.03761 = 0.03569 -0.00072 0.00785 0.00107 C45 1 0.579675 0.536583 0.381352 11.00000 0.04222 0.04505 = 0.04367 -0.00092 0.00942 0.00691 AFIX 43 H45 2 0.623944 0.507017 0.376932 11.00000 -1.20000 AFIX 0 C46 1 0.530448 0.472086 0.394882 11.00000 0.05931 0.03066 = 0.05238 0.00208 0.01151 0.00079 AFIX 43 H46 2 0.541457 0.399129 0.399746 11.00000 -1.20000 AFIX 0 C47 1 0.464627 0.512612 0.401529 11.00000 0.04897 0.04224 = 0.05615 0.00151 0.01296 -0.00626 AFIX 43 H47 2 0.431017 0.467933 0.410952 11.00000 -1.20000 AFIX 0 C48 1 0.449358 0.617845 0.394232 11.00000 0.03861 0.03463 = 0.05304 -0.00045 0.01455 -0.00475 AFIX 43 H48 2 0.404614 0.646227 0.398413 11.00000 -1.20000 AFIX 0 C49 1 0.498998 0.683608 0.380715 11.00000 0.03741 0.03270 = 0.04190 -0.00024 0.01089 -0.00131 C50 1 0.449907 0.853196 0.390107 11.00000 0.04499 0.03908 = 0.04637 0.00240 0.01896 0.00096 AFIX 43 H50 2 0.431089 0.828498 0.410450 11.00000 -1.20000 AFIX 0 C51 1 0.439660 0.962366 0.377854 11.00000 0.04021 0.03797 = 0.04622 0.00115 0.01631 0.00142 C52 1 0.406124 1.146502 0.366397 11.00000 0.03776 0.03291 = 0.04555 -0.00268 0.01054 -0.00026 C53 1 0.383794 1.251789 0.362965 11.00000 0.04455 0.04113 = 0.04659 -0.00236 0.01184 0.00441 AFIX 43 H53 2 0.353895 1.281713 0.378603 11.00000 -1.20000 AFIX 0 C54 1 0.405944 1.312189 0.336338 11.00000 0.05496 0.04139 = 0.05460 0.00476 0.01226 0.00729 AFIX 43 H54 2 0.391722 1.384857 0.333751 11.00000 -1.20000 AFIX 0 C55 1 0.449309 1.267201 0.313038 11.00000 0.05964 0.04567 = 0.05516 0.01163 0.02264 0.00926 AFIX 43 H55 2 0.463559 1.309950 0.294710 11.00000 -1.20000 AFIX 0 C56 1 0.471626 1.162982 0.316084 11.00000 0.05114 0.05213 = 0.04661 0.00493 0.01808 0.00886 AFIX 43 H56 2 0.500472 1.133355 0.299916 11.00000 -1.20000 AFIX 0 C57 1 0.451180 1.101179 0.343387 11.00000 0.03699 0.03493 = 0.04488 -0.00281 0.01140 0.00217 C58 1 0.641519 1.125767 0.364395 11.00000 0.05128 0.05830 = 0.07522 -0.02084 0.00976 -0.00075 AFIX 13 H58 2 0.597230 1.107979 0.348933 11.00000 -1.20000 AFIX 0 C59 1 0.628216 1.097096 0.401159 11.00000 0.07281 0.12466 = 0.07891 -0.01283 0.02186 0.01719 AFIX 33 H59A 2 0.619866 1.019979 0.402650 11.00000 -1.50000 H59B 2 0.586482 1.135937 0.407303 11.00000 -1.50000 H59C 2 0.669683 1.116798 0.417340 11.00000 -1.50000 AFIX 0 C60 1 0.654149 1.246426 0.360630 11.00000 0.07831 0.06359 = 0.13009 -0.03247 0.02214 -0.00053 AFIX 33 H60A 2 0.661699 1.262596 0.336491 11.00000 -1.50000 H60B 2 0.696133 1.267736 0.376208 11.00000 -1.50000 H60C 2 0.612667 1.285869 0.366792 11.00000 -1.50000 AFIX 0 C61 1 0.731121 0.835935 0.287128 11.00000 0.04214 0.06524 = 0.05674 -0.00124 0.02060 0.00776 AFIX 13 H62 2 0.678728 0.825192 0.282110 11.00000 -1.20000 AFIX 0 C62 1 0.759529 0.868375 0.252909 11.00000 0.11623 0.08569 = 0.06768 0.01367 0.04120 0.03146 AFIX 33 H62A 2 0.738229 0.936570 0.244797 11.00000 -1.50000 H62B 2 0.747255 0.813145 0.235264 11.00000 -1.50000 H62C 2 0.811225 0.876105 0.256838 11.00000 -1.50000 AFIX 0 C63 1 0.764056 0.728769 0.299482 11.00000 0.05511 0.06297 = 0.05695 -0.00367 0.02471 0.00402 AFIX 33 H63A 2 0.745763 0.707493 0.321214 11.00000 -1.50000 H63B 2 0.815769 0.736118 0.303495 11.00000 -1.50000 H63C 2 0.751703 0.674147 0.281641 11.00000 -1.50000 AFIX 0 C64 1 0.687446 0.982774 0.325838 11.00000 0.03263 0.04149 = 0.05493 0.00304 0.01459 -0.00580 C65 1 0.700770 1.058938 0.352023 11.00000 0.04147 0.04605 = 0.07358 -0.00765 0.01153 -0.00410 C66 1 0.770397 1.076913 0.366375 11.00000 0.05247 0.06872 = 0.09440 -0.02751 0.00224 -0.00812 AFIX 43 H66 2 0.779842 1.128432 0.384369 11.00000 -1.20000 AFIX 0 C67 1 0.825993 1.020634 0.354741 11.00000 0.03589 0.07651 = 0.11518 -0.01866 0.00958 -0.00713 AFIX 43 H67 2 0.873393 1.034523 0.364388 11.00000 -1.20000 AFIX 0 C68 1 0.812488 0.944930 0.329305 11.00000 0.03550 0.06792 = 0.08991 -0.00570 0.01978 -0.00305 AFIX 43 H68 2 0.850971 0.906830 0.321395 11.00000 -1.20000 AFIX 0 C69 1 0.743522 0.922450 0.314733 11.00000 0.03880 0.04838 = 0.05711 0.00364 0.01941 -0.00257 C70 1 0.640969 1.100466 0.266831 11.00000 0.05586 0.05595 = 0.06745 0.01547 0.02506 -0.00287 AFIX 33 H70A 2 0.681252 1.114838 0.284386 11.00000 -1.50000 H70B 2 0.611309 1.164610 0.263469 11.00000 -1.50000 H70C 2 0.658532 1.081024 0.244753 11.00000 -1.50000 AFIX 0 C71 1 0.597586 1.009537 0.278970 11.00000 0.04538 0.03912 = 0.04655 0.00220 0.01962 0.00344 C72 1 0.537451 0.980237 0.256389 11.00000 0.05510 0.04020 = 0.04287 0.00762 0.01533 0.00593 AFIX 43 H72 2 0.525945 1.027378 0.237308 11.00000 -1.20000 AFIX 0 C73 1 0.491407 0.891925 0.257535 11.00000 0.04846 0.03924 = 0.04292 -0.00047 0.01116 0.00911 C74 1 0.443375 0.871969 0.223842 11.00000 0.07408 0.05479 = 0.04487 0.00107 0.00022 0.00165 AFIX 33 H74A 2 0.412945 0.810052 0.226811 11.00000 -1.50000 H74B 2 0.472512 0.857874 0.204919 11.00000 -1.50000 H74C 2 0.413778 0.935149 0.218128 11.00000 -1.50000 AFIX 0 C75 1 0.338076 0.834511 0.297863 11.00000 0.04527 0.06456 = 0.08810 -0.00117 0.01105 -0.00119 AFIX 13 H75 2 0.374934 0.891194 0.303053 11.00000 -1.20000 AFIX 0 C76 1 0.283087 0.876707 0.268866 11.00000 0.08033 0.10154 = 0.11633 0.02004 0.01164 0.03520 AFIX 33 H76A 2 0.305964 0.888455 0.247650 11.00000 -1.50000 H76B 2 0.263393 0.944338 0.276275 11.00000 -1.50000 H76C 2 0.244828 0.824243 0.264177 11.00000 -1.50000 AFIX 0 C77 1 0.301419 0.817021 0.330910 11.00000 0.04105 0.11412 = 0.09232 -0.00795 0.01596 -0.00148 AFIX 33 H77A 2 0.336355 0.792254 0.349815 11.00000 -1.50000 H77B 2 0.264004 0.763167 0.326326 11.00000 -1.50000 H77C 2 0.280504 0.884479 0.337682 11.00000 -1.50000 AFIX 0 C78 1 0.559508 0.632223 0.270385 11.00000 0.05505 0.04209 = 0.05251 -0.00683 0.00291 0.00679 AFIX 13 H78 2 0.582317 0.692896 0.284302 11.00000 -1.20000 AFIX 0 C79 1 0.575317 0.648144 0.232716 11.00000 0.06673 0.07166 = 0.06091 0.00213 0.00897 0.00693 AFIX 33 H79A 2 0.552896 0.714371 0.223470 11.00000 -1.50000 H79B 2 0.556442 0.587500 0.218515 11.00000 -1.50000 H79C 2 0.626735 0.652755 0.232046 11.00000 -1.50000 AFIX 0 C80 1 0.594308 0.529421 0.285250 11.00000 0.07403 0.05583 = 0.05889 -0.00591 0.00097 0.01739 AFIX 33 H80A 2 0.583641 0.519821 0.309306 11.00000 -1.50000 H80B 2 0.645796 0.534105 0.284850 11.00000 -1.50000 H80C 2 0.575814 0.468386 0.271131 11.00000 -1.50000 AFIX 0 C81 1 0.447413 0.733112 0.281477 11.00000 0.04644 0.04224 = 0.04245 0.00054 0.00034 -0.00295 C82 1 0.375063 0.734554 0.287237 11.00000 0.04401 0.05093 = 0.05942 0.00346 0.00115 -0.00620 C83 1 0.337020 0.639057 0.283010 11.00000 0.05034 0.07169 = 0.07818 0.00551 -0.00126 -0.01097 AFIX 43 H83 2 0.288183 0.638648 0.286434 11.00000 -1.20000 AFIX 0 C84 1 0.368148 0.546508 0.274105 11.00000 0.07086 0.05140 = 0.08897 0.00480 -0.00839 -0.02184 AFIX 43 H84 2 0.340779 0.482957 0.270797 11.00000 -1.20000 AFIX 0 C85 1 0.440250 0.544868 0.269827 11.00000 0.06975 0.04442 = 0.07375 0.00249 -0.00600 -0.00355 AFIX 43 H85 2 0.461925 0.479735 0.264052 11.00000 -1.20000 AFIX 0 C86 1 0.480343 0.637043 0.273913 11.00000 0.05414 0.04206 = 0.04688 0.00040 -0.00145 -0.00141 SAME O201 > C205 SAME O301 > C305 SAME O101 C105 < C102 O101 6 0.967680 0.747343 0.310956 11.00000 0.08378 0.18921 = 0.12953 0.03613 0.01062 0.01808 C102 1 1.023851 0.680526 0.325338 11.00000 0.08443 0.10873 = 0.13319 0.01459 0.01398 0.00640 AFIX 23 H10A 2 1.010228 0.604235 0.322951 11.00000 -1.20000 H10B 2 1.036791 0.696827 0.350319 11.00000 -1.20000 AFIX 0 C103 1 1.085328 0.705421 0.304370 11.00000 0.10475 0.16370 = 0.36985 0.13033 0.08298 0.02729 AFIX 23 H10C 2 1.130986 0.699212 0.319377 11.00000 -1.20000 H10D 2 1.085680 0.654288 0.284822 11.00000 -1.20000 AFIX 0 C104 1 1.076747 0.805464 0.292102 11.00000 0.12361 0.19078 = 0.24565 0.14608 0.07521 0.04954 AFIX 23 H10E 2 1.090613 0.811251 0.268208 11.00000 -1.20000 H10F 2 1.104710 0.857237 0.307408 11.00000 -1.20000 AFIX 0 C105 1 0.997494 0.823241 0.292467 11.00000 0.11785 0.21652 = 0.24916 0.14942 0.09026 0.06292 AFIX 23 H10G 2 0.989555 0.894261 0.302676 11.00000 -1.20000 H10H 2 0.974162 0.823017 0.268228 11.00000 -1.20000 AFIX 0 O201 6 0.874461 0.532501 0.361047 11.00000 0.14870 0.16109 = 0.35156 -0.03638 -0.04974 0.01733 C202 1 0.823475 0.456595 0.343960 11.00000 0.08686 0.17157 = 0.15941 -0.05179 -0.01176 0.00942 AFIX 23 H20B 2 0.788556 0.434343 0.359795 11.00000 -1.20000 H20C 2 0.797851 0.487910 0.322614 11.00000 -1.20000 AFIX 0 C203 1 0.867092 0.367051 0.335562 11.00000 0.20348 0.15427 = 0.23564 -0.04880 -0.02049 0.05643 AFIX 23 H20D 2 0.842005 0.298829 0.338583 11.00000 -1.20000 H20E 2 0.877597 0.372034 0.311073 11.00000 -1.20000 AFIX 0 C204 1 0.928600 0.371012 0.357649 11.00000 0.17704 0.21302 = 0.16126 0.01327 0.01383 0.11491 AFIX 23 H20F 2 0.969650 0.355391 0.344718 11.00000 -1.20000 H20G 2 0.927403 0.316944 0.376298 11.00000 -1.20000 AFIX 0 C205 1 0.935241 0.473457 0.372166 11.00000 0.06833 0.17778 = 0.18731 0.06418 -0.03451 -0.01282 AFIX 23 H20H 2 0.941151 0.468454 0.397907 11.00000 -1.20000 H20I 2 0.977601 0.509396 0.364765 11.00000 -1.20000 AFIX 0 PART -1 O301 6 0.465602 0.928310 0.466559 10.50000 0.08548 0.07831 = 0.06841 -0.01169 0.01161 0.01396 C302 1 0.425940 0.969516 0.492141 10.50000 0.06952 0.09303 = 0.06402 0.00617 0.01982 0.02264 AFIX 23 H30A 2 0.398715 0.911571 0.501994 10.50000 -1.20000 H30B 2 0.392090 1.024155 0.481853 10.50000 -1.20000 AFIX 0 C303 1 0.475670 1.017292 0.519397 10.50000 0.08775 0.10788 = 0.08281 -0.03264 0.02228 0.02979 AFIX 23 H30C 2 0.460234 1.090662 0.524553 10.50000 -1.20000 H30D 2 0.477275 0.974337 0.541001 10.50000 -1.20000 AFIX 0 C304 1 0.542809 1.020065 0.507686 10.50000 0.08164 0.12129 = 0.10958 -0.03213 0.00901 0.00424 AFIX 23 H30E 2 0.578751 0.988518 0.525304 10.50000 -1.20000 H30F 2 0.556698 1.094665 0.503181 10.50000 -1.20000 AFIX 0 C305 1 0.537308 0.957775 0.475635 10.50000 0.07005 0.06849 = 0.10202 -0.00685 0.03020 0.03094 AFIX 23 H30G 2 0.554249 1.000723 0.456678 10.50000 -1.20000 H30H 2 0.567213 0.892914 0.479021 10.50000 -1.20000 PART 0 HKLF 4 REM eh3 in P2(1)/n REM R1 = 0.0746 for 11598 Fo > 4sig(Fo) and 0.1026 for all 16016 data REM 1037 parameters refined using 186 restraints END ; data_sebtyne3 _database_code_depnum_ccdc_archive 'CCDC 916811' #TrackingRef 'All7.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C80 H110 Mg2 N8' _chemical_formula_weight 1232.38 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Mg Mg 0.0486 0.0363 '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' 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/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 12.703(3) _cell_length_b 21.654(5) _cell_length_c 13.282(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.01(2) _cell_angle_gamma 90.00 _cell_volume 3653.5(15) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 787 _cell_measurement_theta_min 3.0612 _cell_measurement_theta_max 29.1840 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.120 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1340 _exptl_absorpt_coefficient_mu 0.081 _exptl_absorpt_correction_T_min 0.70154 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; Despit the near 90 degree beta angle, adding TWIN laws to the model, creating hklf 5 files using ROTAX and processing the raw data with a variety of twin laws present did NOT improve the final solution. Thus the present non-twinned model has been selected. Weak diffraction and very long data collection time resulting in loss of some data frames because of icing. Solvent modeled as disordered. ; _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 'Oxford Diffraction Xcalibur E' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9900 _diffrn_reflns_av_R_equivalents 0.1131 _diffrn_reflns_av_sigmaI/netI 0.2776 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.07 _diffrn_reflns_theta_max 24.99 _reflns_number_total 5404 _reflns_number_gt 1931 _reflns_threshold_expression I>2\s(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0368P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5404 _refine_ls_number_parameters 429 _refine_ls_number_restraints 36 _refine_ls_R_factor_all 0.2566 _refine_ls_R_factor_gt 0.0995 _refine_ls_wR_factor_ref 0.2343 _refine_ls_wR_factor_gt 0.1516 _refine_ls_goodness_of_fit_ref 1.026 _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 0.04254(16) 0.08344(12) 0.55144(15) 0.0279(6) Uani 1 1 d . . . C3 C -0.1736(6) 0.0822(4) 0.3030(5) 0.036(2) Uani 1 1 d . . . N3 N 0.1562(4) 0.1434(3) 0.4905(4) 0.0243(14) Uani 1 1 d . . . N1 N -0.0675(4) 0.0647(3) 0.4365(4) 0.0287(15) Uani 1 1 d . . . C4 C -0.1201(5) 0.1103(4) 0.3825(5) 0.0273(18) Uani 1 1 d . . . C16 C 0.2284(5) 0.1163(4) 0.3235(5) 0.034(2) Uani 1 1 d . . . N4 N -0.0030(4) 0.1491(3) 0.6587(4) 0.0261(15) Uani 1 1 d . . . C22 C 0.1239(6) 0.1280(4) 0.2734(5) 0.041(2) Uani 1 1 d . . . H009 H 0.0705 0.1326 0.3282 0.049 Uiso 1 1 calc R . . C8 C -0.2338(6) 0.1132(4) 0.2316(5) 0.044(2) Uani 1 1 d . . . H010 H -0.2700 0.0924 0.1790 0.052 Uiso 1 1 calc R . . C11 C 0.0734(5) 0.2338(3) 0.5641(4) 0.0281(18) Uani 1 1 d . . . H011 H 0.0682 0.2771 0.5546 0.034 Uiso 1 1 calc R . . C15 C 0.2428(5) 0.1226(4) 0.4290(5) 0.034(2) Uani 1 1 d . . . C5 C -0.1248(5) 0.1742(4) 0.3936(5) 0.036(2) Uani 1 1 d . . . H013 H -0.0891 0.1943 0.4472 0.043 Uiso 1 1 calc R . . C10 C 0.1480(5) 0.2046(4) 0.5029(5) 0.033(2) Uani 1 1 d . . . C19 C 0.4236(5) 0.0924(4) 0.4133(5) 0.041(2) Uani 1 1 d . . . H015 H 0.4898 0.0834 0.4432 0.049 Uiso 1 1 calc R . . C20 C 0.3385(5) 0.1075(4) 0.4731(5) 0.036(2) Uani 1 1 d . . . C28 C -0.1612(5) 0.1040(4) 0.7362(5) 0.034(2) Uani 1 1 d . . . C25 C 0.3498(5) 0.1077(4) 0.5869(5) 0.043(2) Uani 1 1 d . . . H018 H 0.2776 0.1041 0.6165 0.051 Uiso 1 1 calc R . . C13 C 0.2210(5) 0.2499(4) 0.4500(5) 0.037(2) Uani 1 1 d . . . H01A H 0.2742 0.2270 0.4118 0.055 Uiso 1 1 calc R . . H01B H 0.2557 0.2761 0.5001 0.055 Uiso 1 1 calc R . . H01C H 0.1799 0.2758 0.4039 0.055 Uiso 1 1 calc R . . C27 C -0.0621(6) 0.1315(4) 0.7477(5) 0.037(2) Uani 1 1 d . . . C31 C -0.0711(7) 0.1144(4) 0.9263(6) 0.060(3) Uani 1 1 d . . . H022 H -0.0414 0.1182 0.9917 0.072 Uiso 1 1 calc R . . C12 C 0.0050(5) 0.2097(4) 0.6371(5) 0.0328(19) Uani 1 1 d . . . C32 C -0.0173(6) 0.1386(4) 0.8447(5) 0.043(2) Uani 1 1 d . . . C17 C 0.3147(5) 0.1010(4) 0.2656(5) 0.040(2) Uani 1 1 d . . . H025 H 0.3070 0.0978 0.1946 0.048 Uiso 1 1 calc R . . C7 C -0.2369(6) 0.1780(4) 0.2435(5) 0.049(2) Uani 1 1 d . . . H027 H -0.2758 0.2021 0.1967 0.059 Uiso 1 1 calc R . . C34 C -0.2167(5) 0.1052(4) 0.6354(5) 0.037(2) Uani 1 1 d . . . H028 H -0.1636 0.1178 0.5838 0.045 Uiso 1 1 calc R . . C29 C -0.2125(6) 0.0806(4) 0.8207(5) 0.048(2) Uani 1 1 d . . . H029 H -0.2793 0.0614 0.8140 0.057 Uiso 1 1 calc R . . C24 C 0.4151(6) 0.0534(4) 0.6257(5) 0.049(2) Uani 1 1 d . . . H03A H 0.4847 0.0541 0.5939 0.074 Uiso 1 1 calc R . . H03B H 0.3795 0.0146 0.6091 0.074 Uiso 1 1 calc R . . H03C H 0.4230 0.0568 0.6989 0.074 Uiso 1 1 calc R . . C33 C -0.2596(6) 0.0418(4) 0.6038(5) 0.060(3) Uani 1 1 d . . . H03D H -0.3151 0.0291 0.6506 0.090 Uiso 1 1 calc R . . H03E H -0.2025 0.0114 0.6049 0.090 Uiso 1 1 calc R . . H03F H -0.2887 0.0446 0.5355 0.090 Uiso 1 1 calc R . . C30 C -0.1652(7) 0.0855(4) 0.9152(5) 0.052(3) Uani 1 1 d . . . H032 H -0.1992 0.0683 0.9725 0.062 Uiso 1 1 calc R . . C38 C 0.0524(6) 0.2385(4) 0.9221(5) 0.066(3) Uani 1 1 d . . . H03G H 0.0344 0.2283 0.9919 0.100 Uiso 1 1 calc R . . H03H H -0.0083 0.2579 0.8894 0.100 Uiso 1 1 calc R . . H03I H 0.1122 0.2670 0.9213 0.100 Uiso 1 1 calc R . . C36 C 0.1648(6) 0.1437(5) 0.9283(5) 0.072(3) Uani 1 1 d . . . H03J H 0.2183 0.1727 0.9524 0.108 Uiso 1 1 calc R . . H03K H 0.1983 0.1120 0.8865 0.108 Uiso 1 1 calc R . . H03L H 0.1303 0.1241 0.9860 0.108 Uiso 1 1 calc R . . C6 C -0.1831(6) 0.2079(4) 0.3240(5) 0.050(2) Uani 1 1 d . . . H035 H -0.1872 0.2515 0.3303 0.060 Uiso 1 1 calc R . . C18 C 0.4123(6) 0.0903(4) 0.3086(5) 0.044(2) Uani 1 1 d . . . H036 H 0.4713 0.0815 0.2671 0.053 Uiso 1 1 calc R . . C37 C 0.0820(6) 0.1789(4) 0.8651(5) 0.044(2) Uani 1 1 d . . . H037 H 0.1143 0.1905 0.7991 0.053 Uiso 1 1 calc R . . C21 C 0.0898(6) 0.0735(4) 0.2093(5) 0.048(2) Uani 1 1 d . . . H03M H 0.1384 0.0688 0.1524 0.071 Uiso 1 1 calc R . . H03N H 0.0184 0.0807 0.1839 0.071 Uiso 1 1 calc R . . H03O H 0.0907 0.0358 0.2501 0.071 Uiso 1 1 calc R . . C14 C -0.0632(5) 0.2572(4) 0.6886(5) 0.049(2) Uani 1 1 d . . . H03P H -0.0999 0.2380 0.7454 0.073 Uiso 1 1 calc R . . H03Q H -0.1149 0.2734 0.6406 0.073 Uiso 1 1 calc R . . H03R H -0.0190 0.2911 0.7132 0.073 Uiso 1 1 calc R . . C23 C 0.1215(6) 0.1880(4) 0.2109(5) 0.055(2) Uani 1 1 d . . . H04A H 0.1734 0.1853 0.1565 0.082 Uiso 1 1 calc R . . H04B H 0.1383 0.2232 0.2544 0.082 Uiso 1 1 calc R . . H04C H 0.0511 0.1936 0.1821 0.082 Uiso 1 1 calc R . . C35 C -0.3045(6) 0.1533(4) 0.6339(6) 0.067(3) Uani 1 1 d . . . H04D H -0.3585 0.1421 0.6833 0.101 Uiso 1 1 calc R . . H04E H -0.3361 0.1548 0.5666 0.101 Uiso 1 1 calc R . . H04F H -0.2754 0.1939 0.6508 0.101 Uiso 1 1 calc R . . C26 C 0.3981(6) 0.1700(4) 0.6239(5) 0.063(3) Uani 1 1 d . . . H04G H 0.4135 0.1672 0.6961 0.094 Uiso 1 1 calc R . . H04H H 0.3479 0.2035 0.6119 0.094 Uiso 1 1 calc R . . H04I H 0.4634 0.1782 0.5869 0.094 Uiso 1 1 calc R . . C1 C -0.0859(5) 0.0082(3) 0.3934(5) 0.0267(18) Uani 1 1 d . . . N2 N -0.1515(4) 0.0195(3) 0.3117(4) 0.0352(16) Uani 1 1 d . . . C2 C -0.1756(6) -0.0269(4) 0.2351(5) 0.051(2) Uani 1 1 d . . . H3A H -0.1341 -0.0186 0.1744 0.077 Uiso 1 1 calc R . . H3B H -0.2508 -0.0252 0.2187 0.077 Uiso 1 1 calc R . . H3C H -0.1580 -0.0680 0.2610 0.077 Uiso 1 1 calc R . . C1S C 0.9802(15) 0.3675(8) 0.3979(11) 0.075(4) Uani 0.713(13) 1 d PDU A 1 H1S1 H 0.9096 0.3712 0.3689 0.112 Uiso 0.713(13) 1 calc PR A 1 H1S2 H 0.9917 0.3250 0.4206 0.112 Uiso 0.713(13) 1 calc PR A 1 H1S3 H 1.0329 0.3782 0.3469 0.112 Uiso 0.713(13) 1 calc PR A 1 C3S C 0.9903(14) 0.4787(5) 0.4557(6) 0.070(4) Uani 0.713(13) 1 d PDU . 1 H3S1 H 1.0456 0.4854 0.4043 0.084 Uiso 0.713(13) 1 calc PR A 1 H3S2 H 0.9215 0.4889 0.4248 0.084 Uiso 0.713(13) 1 calc PR A 1 C2S C 0.9904(14) 0.4114(6) 0.4872(11) 0.070(4) Uani 0.713(13) 1 d PDU A 1 H2S1 H 0.9312 0.4041 0.5342 0.084 Uiso 0.713(13) 1 calc PR A 1 H2S2 H 1.0567 0.4023 0.5235 0.084 Uiso 0.713(13) 1 calc PR A 1 C4S C 0.964(3) 0.383(2) 0.428(3) 0.075(4) Uani 0.287(13) 1 d PDU A 2 H4S1 H 0.8942 0.4023 0.4324 0.112 Uiso 0.287(13) 1 calc PR A 2 H4S2 H 0.9577 0.3385 0.4376 0.112 Uiso 0.287(13) 1 calc PR A 2 H4S3 H 0.9949 0.3918 0.3621 0.112 Uiso 0.287(13) 1 calc PR A 2 C5S C 1.035(3) 0.4100(16) 0.510(3) 0.070(4) Uani 0.287(13) 1 d PDU A 2 H5S1 H 1.1047 0.3899 0.5062 0.084 Uiso 0.287(13) 1 calc PR A 2 H5S2 H 1.0042 0.3999 0.5768 0.084 Uiso 0.287(13) 1 calc PR A 2 C6S C 1.0491(18) 0.4798(15) 0.503(3) 0.070(4) Uani 0.287(13) 1 d PDU . 2 H6S1 H 1.0919 0.4883 0.4419 0.084 Uiso 0.287(13) 1 calc PR A 2 H6S2 H 1.0909 0.4933 0.5615 0.084 Uiso 0.287(13) 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 Mg1 0.0283(12) 0.0282(16) 0.0272(12) -0.0001(12) 0.0019(11) 0.0015(14) C3 0.039(4) 0.027(5) 0.042(5) 0.009(4) 0.001(4) 0.005(5) N3 0.028(3) 0.017(4) 0.028(3) -0.004(3) -0.003(3) 0.005(3) N1 0.037(3) 0.027(4) 0.023(3) 0.005(3) 0.001(3) 0.000(4) C4 0.030(4) 0.026(5) 0.026(4) 0.004(4) 0.000(3) 0.004(4) C16 0.034(4) 0.034(6) 0.034(4) -0.007(4) 0.009(4) -0.014(4) N4 0.029(3) 0.031(4) 0.019(3) -0.003(3) -0.001(3) 0.003(3) C22 0.049(5) 0.040(6) 0.032(4) 0.004(4) 0.011(4) 0.001(5) C8 0.046(5) 0.042(6) 0.043(5) 0.009(5) -0.015(4) 0.002(5) C11 0.030(4) 0.027(5) 0.027(4) 0.001(4) -0.001(3) 0.002(4) C15 0.036(4) 0.025(5) 0.041(4) -0.001(4) 0.009(4) -0.014(4) C5 0.033(4) 0.041(6) 0.034(4) 0.004(4) -0.004(4) 0.012(5) C10 0.025(4) 0.045(6) 0.031(4) 0.001(4) 0.002(3) -0.002(4) C19 0.029(4) 0.037(6) 0.056(5) -0.004(4) 0.004(4) -0.004(4) C20 0.031(4) 0.039(6) 0.038(4) -0.006(4) 0.000(4) -0.003(4) C28 0.031(4) 0.037(6) 0.034(4) -0.001(4) -0.001(4) 0.000(4) C25 0.033(4) 0.048(6) 0.047(5) -0.004(5) 0.002(4) 0.008(5) C13 0.039(4) 0.039(5) 0.033(4) -0.004(4) -0.002(4) -0.008(4) C27 0.050(5) 0.043(6) 0.018(4) 0.002(4) 0.006(4) 0.007(5) C31 0.068(6) 0.074(8) 0.039(5) 0.004(5) 0.011(5) 0.013(6) C12 0.033(4) 0.036(5) 0.029(4) -0.012(4) -0.005(4) 0.007(5) C32 0.061(5) 0.043(6) 0.026(4) -0.002(4) 0.008(4) 0.010(5) C17 0.045(4) 0.031(5) 0.044(4) 0.003(4) 0.014(4) -0.003(5) C7 0.056(5) 0.046(7) 0.046(5) 0.006(5) -0.014(5) 0.005(6) C34 0.034(4) 0.028(5) 0.050(5) -0.001(4) 0.010(4) -0.006(4) C29 0.053(5) 0.042(6) 0.048(5) 0.002(4) 0.023(4) 0.001(5) C24 0.056(5) 0.039(6) 0.053(5) 0.007(5) -0.001(4) 0.004(5) C33 0.067(6) 0.050(7) 0.063(5) 0.017(5) 0.002(5) -0.011(6) C30 0.075(6) 0.049(7) 0.032(5) 0.008(4) 0.029(5) 0.005(6) C38 0.072(6) 0.071(8) 0.056(5) -0.013(6) -0.003(5) 0.004(6) C36 0.069(6) 0.103(9) 0.045(5) -0.028(6) -0.016(5) 0.030(7) C6 0.060(5) 0.038(6) 0.050(5) -0.001(5) -0.006(5) 0.002(5) C18 0.042(5) 0.040(6) 0.050(5) -0.005(4) 0.021(4) 0.000(5) C37 0.047(5) 0.062(7) 0.023(4) 0.001(4) -0.001(4) 0.005(5) C21 0.056(5) 0.050(6) 0.037(4) -0.001(4) 0.004(4) -0.009(5) C14 0.045(5) 0.043(6) 0.059(5) -0.010(5) 0.010(4) 0.013(5) C23 0.083(6) 0.037(6) 0.044(5) -0.003(4) -0.007(5) 0.007(6) C35 0.069(6) 0.076(8) 0.057(5) 0.004(6) -0.004(5) 0.034(6) C26 0.086(7) 0.054(7) 0.048(5) -0.007(5) -0.013(5) 0.011(6) C1 0.029(4) 0.027(5) 0.023(4) -0.005(4) 0.003(3) -0.006(4) N2 0.038(3) 0.041(5) 0.026(3) 0.001(4) -0.002(3) 0.000(4) C2 0.075(6) 0.043(6) 0.036(4) -0.003(4) 0.003(4) -0.013(6) C1S 0.101(9) 0.071(9) 0.051(10) -0.009(6) -0.026(8) 0.027(8) C3S 0.100(10) 0.063(7) 0.048(8) 0.004(7) -0.019(7) 0.018(9) C2S 0.104(9) 0.059(6) 0.049(7) -0.001(6) -0.027(7) 0.015(8) C4S 0.101(9) 0.071(9) 0.051(10) -0.009(6) -0.026(8) 0.027(8) C5S 0.104(9) 0.059(6) 0.049(7) -0.001(6) -0.027(7) 0.015(8) C6S 0.100(10) 0.063(7) 0.048(8) 0.004(7) -0.019(7) 0.018(9) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mg1 N4 2.094(6) . ? Mg1 N3 2.103(6) . ? Mg1 N1 2.109(6) . ? Mg1 C1 2.186(8) 3_556 ? C3 C8 1.390(9) . ? C3 N2 1.391(9) . ? C3 C4 1.395(9) . ? N3 C10 1.341(9) . ? N3 C15 1.442(8) . ? N1 C1 1.371(8) . ? N1 C4 1.391(8) . ? C4 C5 1.394(10) . ? C16 C17 1.379(8) . ? C16 C15 1.420(8) . ? C16 C22 1.506(9) . ? N4 C12 1.347(9) . ? N4 C27 1.452(7) . ? C22 C21 1.518(9) . ? C22 C23 1.543(10) . ? C22 H009 1.0000 . ? C8 C7 1.412(11) . ? C8 H010 0.9500 . ? C11 C10 1.398(8) . ? C11 C12 1.402(8) . ? C11 H011 0.9500 . ? C15 C20 1.389(9) . ? C5 C6 1.391(9) . ? C5 H013 0.9500 . ? C10 C13 1.522(9) . ? C19 C20 1.381(9) . ? C19 C18 1.398(8) . ? C19 H015 0.9500 . ? C20 C25 1.519(9) . ? C28 C29 1.394(8) . ? C28 C27 1.401(9) . ? C28 C34 1.513(9) . ? C25 C24 1.528(9) . ? C25 C26 1.561(10) . ? C25 H018 1.0000 . ? C13 H01A 0.9800 . ? C13 H01B 0.9800 . ? C13 H01C 0.9800 . ? C27 C32 1.416(9) . ? C31 C30 1.357(10) . ? C31 C32 1.385(9) . ? C31 H022 0.9500 . ? C12 C14 1.509(9) . ? C32 C37 1.557(10) . ? C17 C18 1.384(9) . ? C17 H025 0.9500 . ? C7 C6 1.425(9) . ? C7 H027 0.9500 . ? C34 C35 1.527(9) . ? C34 C33 1.535(10) . ? C34 H028 1.0000 . ? C29 C30 1.396(9) . ? C29 H029 0.9500 . ? C24 H03A 0.9800 . ? C24 H03B 0.9800 . ? C24 H03C 0.9800 . ? C33 H03D 0.9800 . ? C33 H03E 0.9800 . ? C33 H03F 0.9800 . ? C30 H032 0.9500 . ? C38 C37 1.543(10) . ? C38 H03G 0.9800 . ? C38 H03H 0.9800 . ? C38 H03I 0.9800 . ? C36 C37 1.547(9) . ? C36 H03J 0.9800 . ? C36 H03K 0.9800 . ? C36 H03L 0.9800 . ? C6 H035 0.9500 . ? C18 H036 0.9500 . ? C37 H037 1.0000 . ? C21 H03M 0.9800 . ? C21 H03N 0.9800 . ? C21 H03O 0.9800 . ? C14 H03P 0.9800 . ? C14 H03Q 0.9800 . ? C14 H03R 0.9800 . ? C23 H04A 0.9800 . ? C23 H04B 0.9800 . ? C23 H04C 0.9800 . ? C35 H04D 0.9800 . ? C35 H04E 0.9800 . ? C35 H04F 0.9800 . ? C26 H04G 0.9800 . ? C26 H04H 0.9800 . ? C26 H04I 0.9800 . ? C1 N2 1.390(7) . ? C1 Mg1 2.186(8) 3_556 ? N2 C2 1.463(8) . ? C2 H3A 0.9800 . ? C2 H3B 0.9800 . ? C2 H3C 0.9800 . ? C1S C2S 1.524(9) . ? C1S H1S1 0.9800 . ? C1S H1S2 0.9800 . ? C1S H1S3 0.9800 . ? C3S C3S 1.517(9) 3_766 ? C3S C2S 1.517(9) . ? C3S H3S1 0.9900 . ? C3S H3S2 0.9900 . ? C2S H2S1 0.9900 . ? C2S H2S2 0.9900 . ? C4S C5S 1.525(10) . ? C4S H4S1 0.9800 . ? C4S H4S2 0.9800 . ? C4S H4S3 0.9800 . ? C5S C6S 1.526(10) . ? C5S H5S1 0.9900 . ? C5S H5S2 0.9900 . ? C6S C6S 1.527(10) 3_766 ? C6S H6S1 0.9900 . ? C6S H6S2 0.9900 . ? 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 N4 Mg1 N3 91.9(2) . . ? N4 Mg1 N1 116.1(2) . . ? N3 Mg1 N1 107.1(2) . . ? N4 Mg1 C1 117.3(2) . 3_556 ? N3 Mg1 C1 121.1(2) . 3_556 ? N1 Mg1 C1 103.6(2) . 3_556 ? C8 C3 N2 129.7(8) . . ? C8 C3 C4 125.0(7) . . ? N2 C3 C4 105.3(6) . . ? C10 N3 C15 116.0(6) . . ? C10 N3 Mg1 120.6(5) . . ? C15 N3 Mg1 123.3(5) . . ? C1 N1 C4 109.6(5) . . ? C1 N1 Mg1 126.0(5) . . ? C4 N1 Mg1 123.7(5) . . ? N1 C4 C5 132.2(7) . . ? N1 C4 C3 108.4(7) . . ? C5 C4 C3 119.4(7) . . ? C17 C16 C15 118.1(6) . . ? C17 C16 C22 119.7(6) . . ? C15 C16 C22 122.2(6) . . ? C12 N4 C27 117.9(6) . . ? C12 N4 Mg1 119.7(4) . . ? C27 N4 Mg1 121.2(5) . . ? C16 C22 C21 111.6(7) . . ? C16 C22 C23 113.4(7) . . ? C21 C22 C23 110.3(5) . . ? C16 C22 H009 107.1 . . ? C21 C22 H009 107.1 . . ? C23 C22 H009 107.1 . . ? C3 C8 C7 114.8(8) . . ? C3 C8 H010 122.6 . . ? C7 C8 H010 122.6 . . ? C10 C11 C12 130.9(7) . . ? C10 C11 H011 114.6 . . ? C12 C11 H011 114.6 . . ? C20 C15 C16 120.4(7) . . ? C20 C15 N3 120.2(6) . . ? C16 C15 N3 119.4(6) . . ? C6 C5 C4 118.3(7) . . ? C6 C5 H013 120.9 . . ? C4 C5 H013 120.9 . . ? N3 C10 C11 124.8(7) . . ? N3 C10 C13 122.2(6) . . ? C11 C10 C13 113.0(7) . . ? C20 C19 C18 120.0(7) . . ? C20 C19 H015 120.0 . . ? C18 C19 H015 120.0 . . ? C19 C20 C15 119.9(6) . . ? C19 C20 C25 120.0(6) . . ? C15 C20 C25 120.1(6) . . ? C29 C28 C27 119.1(6) . . ? C29 C28 C34 120.0(6) . . ? C27 C28 C34 120.6(6) . . ? C20 C25 C24 112.6(7) . . ? C20 C25 C26 110.7(7) . . ? C24 C25 C26 110.1(6) . . ? C20 C25 H018 107.8 . . ? C24 C25 H018 107.8 . . ? C26 C25 H018 107.8 . . ? C10 C13 H01A 109.5 . . ? C10 C13 H01B 109.5 . . ? H01A C13 H01B 109.5 . . ? C10 C13 H01C 109.5 . . ? H01A C13 H01C 109.5 . . ? H01B C13 H01C 109.5 . . ? C28 C27 C32 120.4(6) . . ? C28 C27 N4 119.2(6) . . ? C32 C27 N4 120.3(6) . . ? C30 C31 C32 121.6(8) . . ? C30 C31 H022 119.2 . . ? C32 C31 H022 119.2 . . ? N4 C12 C11 123.8(6) . . ? N4 C12 C14 121.6(6) . . ? C11 C12 C14 114.6(7) . . ? C31 C32 C27 118.2(8) . . ? C31 C32 C37 118.4(7) . . ? C27 C32 C37 123.0(7) . . ? C16 C17 C18 121.5(7) . . ? C16 C17 H025 119.3 . . ? C18 C17 H025 119.3 . . ? C8 C7 C6 121.4(8) . . ? C8 C7 H027 119.3 . . ? C6 C7 H027 119.3 . . ? C28 C34 C35 111.3(6) . . ? C28 C34 C33 113.2(7) . . ? C35 C34 C33 110.3(6) . . ? C28 C34 H028 107.3 . . ? C35 C34 H028 107.3 . . ? C33 C34 H028 107.3 . . ? C28 C29 C30 119.7(7) . . ? C28 C29 H029 120.1 . . ? C30 C29 H029 120.1 . . ? C25 C24 H03A 109.5 . . ? C25 C24 H03B 109.5 . . ? H03A C24 H03B 109.5 . . ? C25 C24 H03C 109.5 . . ? H03A C24 H03C 109.5 . . ? H03B C24 H03C 109.5 . . ? C34 C33 H03D 109.5 . . ? C34 C33 H03E 109.5 . . ? H03D C33 H03E 109.5 . . ? C34 C33 H03F 109.5 . . ? H03D C33 H03F 109.5 . . ? H03E C33 H03F 109.5 . . ? C31 C30 C29 120.8(7) . . ? C31 C30 H032 119.6 . . ? C29 C30 H032 119.6 . . ? C37 C38 H03G 109.5 . . ? C37 C38 H03H 109.5 . . ? H03G C38 H03H 109.5 . . ? C37 C38 H03I 109.5 . . ? H03G C38 H03I 109.5 . . ? H03H C38 H03I 109.5 . . ? C37 C36 H03J 109.5 . . ? C37 C36 H03K 109.5 . . ? H03J C36 H03K 109.5 . . ? C37 C36 H03L 109.5 . . ? H03J C36 H03L 109.5 . . ? H03K C36 H03L 109.5 . . ? C5 C6 C7 121.1(8) . . ? C5 C6 H035 119.5 . . ? C7 C6 H035 119.5 . . ? C17 C18 C19 119.8(7) . . ? C17 C18 H036 120.1 . . ? C19 C18 H036 120.1 . . ? C38 C37 C36 108.1(6) . . ? C38 C37 C32 110.9(6) . . ? C36 C37 C32 111.7(7) . . ? C38 C37 H037 108.7 . . ? C36 C37 H037 108.7 . . ? C32 C37 H037 108.7 . . ? C22 C21 H03M 109.5 . . ? C22 C21 H03N 109.5 . . ? H03M C21 H03N 109.5 . . ? C22 C21 H03O 109.5 . . ? H03M C21 H03O 109.5 . . ? H03N C21 H03O 109.5 . . ? C12 C14 H03P 109.5 . . ? C12 C14 H03Q 109.5 . . ? H03P C14 H03Q 109.5 . . ? C12 C14 H03R 109.5 . . ? H03P C14 H03R 109.5 . . ? H03Q C14 H03R 109.5 . . ? C22 C23 H04A 109.5 . . ? C22 C23 H04B 109.5 . . ? H04A C23 H04B 109.5 . . ? C22 C23 H04C 109.5 . . ? H04A C23 H04C 109.5 . . ? H04B C23 H04C 109.5 . . ? C34 C35 H04D 109.5 . . ? C34 C35 H04E 109.5 . . ? H04D C35 H04E 109.5 . . ? C34 C35 H04F 109.5 . . ? H04D C35 H04F 109.5 . . ? H04E C35 H04F 109.5 . . ? C25 C26 H04G 109.5 . . ? C25 C26 H04H 109.5 . . ? H04G C26 H04H 109.5 . . ? C25 C26 H04I 109.5 . . ? H04G C26 H04I 109.5 . . ? H04H C26 H04I 109.5 . . ? N1 C1 N2 105.7(6) . . ? N1 C1 Mg1 128.8(5) . 3_556 ? N2 C1 Mg1 125.0(5) . 3_556 ? C1 N2 C3 111.0(6) . . ? C1 N2 C2 123.2(7) . . ? C3 N2 C2 124.8(6) . . ? N2 C2 H3A 109.5 . . ? N2 C2 H3B 109.5 . . ? H3A C2 H3B 109.5 . . ? N2 C2 H3C 109.5 . . ? H3A C2 H3C 109.5 . . ? H3B C2 H3C 109.5 . . ? C3S C3S C2S 111.7(12) 3_766 . ? C3S C3S H3S1 109.3 3_766 . ? C2S C3S H3S1 109.3 . . ? C3S C3S H3S2 109.3 3_766 . ? C2S C3S H3S2 109.3 . . ? H3S1 C3S H3S2 107.9 . . ? C3S C2S C1S 112.6(11) . . ? C3S C2S H2S1 109.1 . . ? C1S C2S H2S1 109.1 . . ? C3S C2S H2S2 109.1 . . ? C1S C2S H2S2 109.1 . . ? H2S1 C2S H2S2 107.8 . . ? C5S C4S H4S1 109.5 . . ? C5S C4S H4S2 109.5 . . ? H4S1 C4S H4S2 109.5 . . ? C5S C4S H4S3 109.5 . . ? H4S1 C4S H4S3 109.5 . . ? H4S2 C4S H4S3 109.5 . . ? C4S C5S C6S 113(3) . . ? C4S C5S H5S1 108.9 . . ? C6S C5S H5S1 108.9 . . ? C4S C5S H5S2 108.9 . . ? C6S C5S H5S2 108.9 . . ? H5S1 C5S H5S2 107.7 . . ? C5S C6S C6S 118(4) . 3_766 ? C5S C6S H6S1 107.7 . . ? C6S C6S H6S1 107.7 3_766 . ? C5S C6S H6S2 107.7 . . ? C6S C6S H6S2 107.7 3_766 . ? H6S1 C6S H6S2 107.1 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N4 Mg1 N3 C10 -22.6(6) . . . . ? N1 Mg1 N3 C10 95.5(6) . . . . ? C1 Mg1 N3 C10 -146.3(5) 3_556 . . . ? N4 Mg1 N3 C15 161.0(5) . . . . ? N1 Mg1 N3 C15 -80.9(5) . . . . ? C1 Mg1 N3 C15 37.3(6) 3_556 . . . ? N4 Mg1 N1 C1 -143.5(5) . . . . ? N3 Mg1 N1 C1 115.6(5) . . . . ? C1 Mg1 N1 C1 -13.5(6) 3_556 . . . ? N4 Mg1 N1 C4 47.1(5) . . . . ? N3 Mg1 N1 C4 -53.8(5) . . . . ? C1 Mg1 N1 C4 177.2(4) 3_556 . . . ? C1 N1 C4 C5 -178.2(7) . . . . ? Mg1 N1 C4 C5 -7.4(10) . . . . ? C1 N1 C4 C3 0.0(7) . . . . ? Mg1 N1 C4 C3 170.9(4) . . . . ? C8 C3 C4 N1 -179.0(6) . . . . ? N2 C3 C4 N1 0.2(7) . . . . ? C8 C3 C4 C5 -0.5(10) . . . . ? N2 C3 C4 C5 178.7(6) . . . . ? N3 Mg1 N4 C12 30.1(6) . . . . ? N1 Mg1 N4 C12 -80.0(6) . . . . ? C1 Mg1 N4 C12 156.8(5) 3_556 . . . ? N3 Mg1 N4 C27 -162.2(5) . . . . ? N1 Mg1 N4 C27 87.6(5) . . . . ? C1 Mg1 N4 C27 -35.5(5) 3_556 . . . ? C17 C16 C22 C21 55.7(9) . . . . ? C15 C16 C22 C21 -126.5(8) . . . . ? C17 C16 C22 C23 -69.6(10) . . . . ? C15 C16 C22 C23 108.2(8) . . . . ? N2 C3 C8 C7 -178.0(7) . . . . ? C4 C3 C8 C7 1.0(11) . . . . ? C17 C16 C15 C20 -6.4(12) . . . . ? C22 C16 C15 C20 175.7(7) . . . . ? C17 C16 C15 N3 175.0(6) . . . . ? C22 C16 C15 N3 -2.8(11) . . . . ? C10 N3 C15 C20 92.1(9) . . . . ? Mg1 N3 C15 C20 -91.4(7) . . . . ? C10 N3 C15 C16 -89.3(9) . . . . ? Mg1 N3 C15 C16 87.2(8) . . . . ? N1 C4 C5 C6 178.0(6) . . . . ? C3 C4 C5 C6 -0.1(10) . . . . ? C15 N3 C10 C11 -176.3(6) . . . . ? Mg1 N3 C10 C11 7.2(10) . . . . ? C15 N3 C10 C13 3.9(10) . . . . ? Mg1 N3 C10 C13 -172.7(4) . . . . ? C12 C11 C10 N3 12.3(12) . . . . ? C12 C11 C10 C13 -167.9(6) . . . . ? C18 C19 C20 C15 -2.2(13) . . . . ? C18 C19 C20 C25 178.0(8) . . . . ? C16 C15 C20 C19 6.7(12) . . . . ? N3 C15 C20 C19 -174.8(7) . . . . ? C16 C15 C20 C25 -173.5(7) . . . . ? N3 C15 C20 C25 5.1(12) . . . . ? C19 C20 C25 C24 -40.8(11) . . . . ? C15 C20 C25 C24 139.4(7) . . . . ? C19 C20 C25 C26 82.9(10) . . . . ? C15 C20 C25 C26 -96.9(8) . . . . ? C29 C28 C27 C32 -3.6(12) . . . . ? C34 C28 C27 C32 170.5(7) . . . . ? C29 C28 C27 N4 172.6(7) . . . . ? C34 C28 C27 N4 -13.3(11) . . . . ? C12 N4 C27 C28 107.3(9) . . . . ? Mg1 N4 C27 C28 -60.5(8) . . . . ? C12 N4 C27 C32 -76.5(9) . . . . ? Mg1 N4 C27 C32 115.7(7) . . . . ? C27 N4 C12 C11 169.0(6) . . . . ? Mg1 N4 C12 C11 -23.0(10) . . . . ? C27 N4 C12 C14 -13.1(10) . . . . ? Mg1 N4 C12 C14 154.9(5) . . . . ? C10 C11 C12 N4 -2.9(12) . . . . ? C10 C11 C12 C14 179.0(6) . . . . ? C30 C31 C32 C27 -1.1(13) . . . . ? C30 C31 C32 C37 171.7(8) . . . . ? C28 C27 C32 C31 3.8(12) . . . . ? N4 C27 C32 C31 -172.4(7) . . . . ? C28 C27 C32 C37 -168.6(7) . . . . ? N4 C27 C32 C37 15.2(12) . . . . ? C15 C16 C17 C18 1.8(12) . . . . ? C22 C16 C17 C18 179.7(7) . . . . ? C3 C8 C7 C6 -1.0(11) . . . . ? C29 C28 C34 C35 70.8(10) . . . . ? C27 C28 C34 C35 -103.2(8) . . . . ? C29 C28 C34 C33 -54.0(9) . . . . ? C27 C28 C34 C33 131.9(7) . . . . ? C27 C28 C29 C30 0.8(12) . . . . ? C34 C28 C29 C30 -173.4(8) . . . . ? C32 C31 C30 C29 -1.8(14) . . . . ? C28 C29 C30 C31 2.0(13) . . . . ? C4 C5 C6 C7 0.1(10) . . . . ? C8 C7 C6 C5 0.5(11) . . . . ? C16 C17 C18 C19 2.6(13) . . . . ? C20 C19 C18 C17 -2.5(13) . . . . ? C31 C32 C37 C38 -64.1(9) . . . . ? C27 C32 C37 C38 108.3(8) . . . . ? C31 C32 C37 C36 56.5(9) . . . . ? C27 C32 C37 C36 -131.1(8) . . . . ? C4 N1 C1 N2 -0.3(7) . . . . ? Mg1 N1 C1 N2 -170.9(4) . . . . ? C4 N1 C1 Mg1 -172.5(4) . . . 3_556 ? Mg1 N1 C1 Mg1 16.9(8) . . . 3_556 ? N1 C1 N2 C3 0.4(7) . . . . ? Mg1 C1 N2 C3 173.0(4) 3_556 . . . ? N1 C1 N2 C2 169.1(6) . . . . ? Mg1 C1 N2 C2 -18.3(8) 3_556 . . . ? C8 C3 N2 C1 178.8(6) . . . . ? C4 C3 N2 C1 -0.4(7) . . . . ? C8 C3 N2 C2 10.3(12) . . . . ? C4 C3 N2 C2 -168.9(6) . . . . ? C3S C3S C2S C1S -175.1(19) 3_766 . . . ? C4S C5S C6S C6S 53(7) . . . 3_766 ? _diffrn_measured_fraction_theta_max 0.841 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.841 _refine_diff_density_max 0.290 _refine_diff_density_min -0.283 _refine_diff_density_rms 0.063 data_vb6 _database_code_depnum_ccdc_archive 'CCDC 916812' #TrackingRef 'All7.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42.50 H61.50 Mg N4' _chemical_formula_weight 652.77 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Mg Mg 0.0486 0.0363 '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' 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/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 14.0179(4) _cell_length_b 13.5976(3) _cell_length_c 21.7756(6) _cell_angle_alpha 90.00 _cell_angle_beta 96.842(3) _cell_angle_gamma 90.00 _cell_volume 4121.08(19) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 7478 _cell_measurement_theta_min 2.8207 _cell_measurement_theta_max 29.7144 _exptl_crystal_description ? _exptl_crystal_colour colourless _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.052 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1426 _exptl_absorpt_coefficient_mu 0.075 _exptl_absorpt_correction_T_min 0.96867 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _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 'Oxford Diffraction Gemini S' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21699 _diffrn_reflns_av_R_equivalents 0.0380 _diffrn_reflns_av_sigmaI/netI 0.0681 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 3.74 _diffrn_reflns_theta_max 26.00 _reflns_number_total 8074 _reflns_number_gt 5016 _reflns_threshold_expression I>2\s(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1205P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8074 _refine_ls_number_parameters 472 _refine_ls_number_restraints 77 _refine_ls_R_factor_all 0.1027 _refine_ls_R_factor_gt 0.0640 _refine_ls_wR_factor_ref 0.1953 _refine_ls_wR_factor_gt 0.1814 _refine_ls_goodness_of_fit_ref 0.978 _refine_ls_restrained_S_all 0.983 _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 0.03292(6) 0.69868(6) 0.24805(4) 0.0258(2) Uani 1 1 d . . . N1 N 0.00597(14) 0.64331(14) 0.15876(9) 0.0263(5) Uani 1 1 d . A . N2 N -0.10234(14) 0.65794(14) 0.26798(9) 0.0250(5) Uani 1 1 d . A . N3 N 0.03152(16) 0.85595(15) 0.24041(10) 0.0351(5) Uani 1 1 d . A . N5 N 0.09367(17) 1.00620(15) 0.25841(11) 0.0390(6) Uani 1 1 d . A . C1 C 0.08183(17) 0.61320(18) 0.12364(11) 0.0282(6) Uani 1 1 d . . . C2 C 0.10104(19) 0.51265(19) 0.11727(12) 0.0326(6) Uani 1 1 d . A . C3 C 0.1763(2) 0.4843(2) 0.08466(13) 0.0417(7) Uani 1 1 d . . . H3 H 0.1903 0.4164 0.0806 0.050 Uiso 1 1 calc R A . C4 C 0.2308(2) 0.5535(2) 0.05814(13) 0.0461(8) Uani 1 1 d . A . H4 H 0.2809 0.5333 0.0352 0.055 Uiso 1 1 calc R . . C5 C 0.2120(2) 0.6518(2) 0.06505(13) 0.0418(7) Uani 1 1 d . . . H5 H 0.2505 0.6989 0.0473 0.050 Uiso 1 1 calc R A . C6 C 0.13827(19) 0.6842(2) 0.09724(12) 0.0336(6) Uani 1 1 d . A . C7 C 0.1203(2) 0.79323(19) 0.10294(13) 0.0399(7) Uani 1 1 d . . . H7 H 0.0631 0.8013 0.1259 0.048 Uiso 1 1 calc R A . C8 C 0.2047(2) 0.8436(2) 0.14061(16) 0.0545(9) Uani 1 1 d . A . H8A H 0.2172 0.8120 0.1812 0.082 Uiso 1 1 calc R . . H8B H 0.1894 0.9132 0.1460 0.082 Uiso 1 1 calc R . . H8C H 0.2618 0.8381 0.1189 0.082 Uiso 1 1 calc R . . C9 C 0.0968(3) 0.8430(2) 0.04009(15) 0.0597(9) Uani 1 1 d . A . H9A H 0.1509 0.8346 0.0159 0.089 Uiso 1 1 calc R . . H9B H 0.0855 0.9133 0.0461 0.089 Uiso 1 1 calc R . . H9C H 0.0391 0.8130 0.0180 0.089 Uiso 1 1 calc R . . C10 C 0.0429(2) 0.43321(18) 0.14547(13) 0.0362(7) Uani 1 1 d . . . H10 H -0.0145 0.4656 0.1599 0.043 Uiso 1 1 calc R A . C11 C 0.0062(2) 0.3541(2) 0.09785(14) 0.0452(8) Uani 1 1 d . A . H11A H -0.0278 0.3857 0.0611 0.068 Uiso 1 1 calc R . . H11B H -0.0377 0.3096 0.1161 0.068 Uiso 1 1 calc R . . H11C H 0.0608 0.3165 0.0860 0.068 Uiso 1 1 calc R . . C12 C 0.1010(3) 0.3873(2) 0.20161(15) 0.0537(8) Uani 1 1 d . A . H12A H 0.1549 0.3502 0.1884 0.081 Uiso 1 1 calc R . . H12B H 0.0599 0.3429 0.2222 0.081 Uiso 1 1 calc R . . H12C H 0.1257 0.4392 0.2304 0.081 Uiso 1 1 calc R . . C14 C -0.08366(18) 0.63737(16) 0.13056(11) 0.0262(6) Uani 1 1 d . . . C15 C -0.16653(18) 0.64601(17) 0.16048(11) 0.0268(6) Uani 1 1 d . A . H15 H -0.2250 0.6524 0.1339 0.032 Uiso 1 1 calc R . . C16 C -0.17578(17) 0.64666(16) 0.22432(11) 0.0257(5) Uani 1 1 d . . . C17 C -0.1014(2) 0.6183(2) 0.06173(12) 0.0410(7) Uani 1 1 d . A . H17A H -0.0648 0.6656 0.0399 0.062 Uiso 1 1 calc R . . H17B H -0.1701 0.6257 0.0476 0.062 Uiso 1 1 calc R . . H17C H -0.0810 0.5514 0.0530 0.062 Uiso 1 1 calc R . . C18 C -0.27605(18) 0.63002(19) 0.24153(12) 0.0332(6) Uani 1 1 d . A . H18A H -0.2782 0.5671 0.2633 0.050 Uiso 1 1 calc R . . H18B H -0.3220 0.6287 0.2039 0.050 Uiso 1 1 calc R . . H18C H -0.2928 0.6834 0.2685 0.050 Uiso 1 1 calc R . . C19 C -0.11853(17) 0.64835(18) 0.33197(11) 0.0280(6) Uani 1 1 d . . . C20 C -0.15282(19) 0.72854(19) 0.36361(12) 0.0350(6) Uani 1 1 d . A . C21 C -0.1638(2) 0.7164(2) 0.42600(13) 0.0453(7) Uani 1 1 d . . . H21 H -0.1878 0.7695 0.4480 0.054 Uiso 1 1 calc R A . C22 C -0.1408(2) 0.6299(2) 0.45634(13) 0.0472(8) Uani 1 1 d . A . H22 H -0.1488 0.6235 0.4989 0.057 Uiso 1 1 calc R . . C23 C -0.1062(2) 0.5519(2) 0.42501(12) 0.0391(7) Uani 1 1 d . . . H23 H -0.0899 0.4922 0.4464 0.047 Uiso 1 1 calc R A . C24 C -0.09468(18) 0.55937(18) 0.36272(12) 0.0318(6) Uani 1 1 d . A . C25 C -0.0580(2) 0.47104(19) 0.32953(13) 0.0365(7) Uani 1 1 d . . . H25 H -0.0437 0.4935 0.2879 0.044 Uiso 1 1 calc R A . C26 C -0.1354(2) 0.3914(2) 0.31968(16) 0.0547(9) Uani 1 1 d . A . H26A H -0.1543 0.3715 0.3598 0.082 Uiso 1 1 calc R . . H26B H -0.1100 0.3344 0.2994 0.082 Uiso 1 1 calc R . . H26C H -0.1915 0.4174 0.2935 0.082 Uiso 1 1 calc R . . C27 C 0.0339(2) 0.4290(2) 0.36343(15) 0.0480(8) Uani 1 1 d . A . H27A H 0.0228 0.4095 0.4053 0.072 Uiso 1 1 calc R . . H27B H 0.0847 0.4789 0.3658 0.072 Uiso 1 1 calc R . . H27C H 0.0537 0.3713 0.3411 0.072 Uiso 1 1 calc R . . C28 C -0.1756(2) 0.82746(19) 0.33309(13) 0.0389(7) Uani 1 1 d . . . H28 H -0.1726 0.8198 0.2877 0.047 Uiso 1 1 calc R A . C29 C -0.1007(3) 0.9026(2) 0.35757(15) 0.0554(9) Uani 1 1 d . A . H29A H -0.1093 0.9195 0.4003 0.083 Uiso 1 1 calc R . . H29B H -0.1079 0.9619 0.3319 0.083 Uiso 1 1 calc R . . H29C H -0.0363 0.8750 0.3564 0.083 Uiso 1 1 calc R . . C30 C -0.2760(2) 0.8650(2) 0.34215(16) 0.0539(9) Uani 1 1 d . A . H30A H -0.3241 0.8162 0.3262 0.081 Uiso 1 1 calc R . . H30B H -0.2884 0.9270 0.3197 0.081 Uiso 1 1 calc R . . H30C H -0.2797 0.8758 0.3863 0.081 Uiso 1 1 calc R . . C31 C 0.0985(2) 0.91080(19) 0.27316(13) 0.0371(7) Uani 1 1 d . . . H31 H 0.1452 0.8844 0.3040 0.045 Uiso 1 1 calc R A . C32 C 0.01764(19) 1.01656(17) 0.21130(12) 0.0320(6) Uani 1 1 d . . . C33 C -0.02020(19) 0.92203(19) 0.20151(12) 0.0339(6) Uani 1 1 d . A . C34 C -0.0976(2) 0.9071(2) 0.15720(13) 0.0403(7) Uani 1 1 d . . . H34 H -0.1258 0.8439 0.1504 0.048 Uiso 1 1 calc R A . C35 C -0.1330(2) 0.9889(2) 0.12276(13) 0.0418(7) Uani 1 1 d . A . H35 H -0.1859 0.9806 0.0916 0.050 Uiso 1 1 calc R . . C36 C -0.0936(2) 1.0811(2) 0.13260(14) 0.0446(7) Uani 1 1 d . . . H36 H -0.1198 1.1346 0.1081 0.053 Uiso 1 1 calc R A . C37 C -0.0159(2) 1.0978(2) 0.17776(13) 0.0416(7) Uani 1 1 d . A . H37 H 0.0120 1.1611 0.1849 0.050 Uiso 1 1 calc R . . C38 C 0.1540(2) 1.0853(2) 0.28631(15) 0.0549(9) Uani 1 1 d . . . H38A H 0.2018 1.0582 0.3184 0.082 Uiso 1 1 calc R A . H38B H 0.1140 1.1335 0.3049 0.082 Uiso 1 1 calc R . . H38C H 0.1868 1.1175 0.2545 0.082 Uiso 1 1 calc R . . C39 C 0.162(2) 0.667(3) 0.3030(6) 0.0357(18) Uani 0.50 1 d PDU A 1 H39A H 0.1772 0.5971 0.2947 0.043 Uiso 0.50 1 calc PR A 1 H39B H 0.2123 0.7068 0.2869 0.043 Uiso 0.50 1 calc PR A 1 C40 C 0.1752(7) 0.6790(11) 0.3730(5) 0.047(2) Uani 0.50 1 d PDU A 1 H40A H 0.1203 0.6473 0.3899 0.056 Uiso 0.50 1 calc PR A 1 H40B H 0.1728 0.7501 0.3825 0.056 Uiso 0.50 1 calc PR A 1 C41 C 0.2694(6) 0.6361(6) 0.4069(3) 0.0758(17) Uani 0.50 1 d PDU A 1 H41A H 0.2706 0.5650 0.3973 0.091 Uiso 0.50 1 calc PR A 1 H41B H 0.3236 0.6667 0.3886 0.091 Uiso 0.50 1 calc PR A 1 C42 C 0.2888(9) 0.6467(7) 0.4742(4) 0.099(3) Uani 0.50 1 d PDU A 1 H42A H 0.3017 0.7159 0.4846 0.148 Uiso 0.50 1 calc PR A 1 H42B H 0.3449 0.6068 0.4895 0.148 Uiso 0.50 1 calc PR A 1 H42C H 0.2328 0.6244 0.4933 0.148 Uiso 0.50 1 calc PR A 1 C39A C 0.157(2) 0.668(3) 0.3162(6) 0.0357(18) Uani 0.50 1 d PDU A 2 H39C H 0.1708 0.5966 0.3155 0.043 Uiso 0.50 1 calc PR A 2 H39D H 0.2136 0.7026 0.3033 0.043 Uiso 0.50 1 calc PR A 2 C40A C 0.1463(6) 0.6977(10) 0.3827(5) 0.047(2) Uani 0.50 1 d PDU A 2 H40C H 0.0962 0.6559 0.3978 0.056 Uiso 0.50 1 calc PR A 2 H40D H 0.1235 0.7666 0.3827 0.056 Uiso 0.50 1 calc PR A 2 C41A C 0.2384(6) 0.6892(6) 0.4281(4) 0.0758(17) Uani 0.50 1 d PDU A 2 H41C H 0.2885 0.7284 0.4108 0.091 Uiso 0.50 1 d PR A 2 H41D H 0.2261 0.7218 0.4670 0.091 Uiso 0.50 1 d PR A 2 C42A C 0.2785(16) 0.5921(10) 0.4457(10) 0.099(3) Uani 0.25 1 d PDU A 2 H42G H 0.3360 0.6001 0.4757 0.148 Uiso 0.25 1 calc PR A 2 H42H H 0.2957 0.5582 0.4089 0.148 Uiso 0.25 1 calc PR A 2 H42I H 0.2306 0.5533 0.4644 0.148 Uiso 0.25 1 calc PR A 2 C42B C 0.2285(17) 0.6892(15) 0.4967(5) 0.099(3) Uani 0.25 1 d PDU A 2 H42D H 0.2110 0.6231 0.5094 0.148 Uiso 0.25 1 calc PR A 2 H42E H 0.1784 0.7360 0.5051 0.148 Uiso 0.25 1 calc PR A 2 H42F H 0.2898 0.7086 0.5200 0.148 Uiso 0.25 1 calc PR A 2 C1S C -0.0049(4) 0.9517(3) 0.5195(2) 0.0300(11) Uani 0.50 1 d PU . . H1S1 H -0.0170 0.9697 0.5619 0.036 Uiso 0.50 1 calc PR . . H1S2 H -0.0605 0.9130 0.5004 0.036 Uiso 0.50 1 calc PR . . C2S C 0.0834(4) 0.8905(4) 0.5225(3) 0.0427(14) Uani 0.50 1 d PU . . H2S1 H 0.1379 0.9269 0.5451 0.051 Uiso 0.50 1 calc PR . . H2S2 H 0.0990 0.8778 0.4801 0.051 Uiso 0.50 1 calc PR . . C3S C 0.0710(5) 0.7935(5) 0.5547(4) 0.080(3) Uani 0.50 1 d PU . . H3S1 H 0.0234 0.8010 0.5839 0.119 Uiso 0.50 1 calc PR . . H3S2 H 0.1326 0.7731 0.5771 0.119 Uiso 0.50 1 calc PR . . H3S3 H 0.0489 0.7434 0.5238 0.119 Uiso 0.50 1 calc PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mg1 0.0239(4) 0.0294(4) 0.0243(4) -0.0017(3) 0.0040(3) -0.0017(4) N1 0.0260(11) 0.0298(11) 0.0240(11) -0.0010(9) 0.0063(9) -0.0031(9) N2 0.0250(11) 0.0299(10) 0.0206(10) 0.0016(8) 0.0046(9) 0.0012(9) N3 0.0372(13) 0.0323(11) 0.0358(13) -0.0010(10) 0.0043(11) -0.0026(10) N5 0.0399(14) 0.0373(13) 0.0389(14) -0.0075(10) 0.0013(11) -0.0075(11) C1 0.0253(13) 0.0407(14) 0.0190(12) -0.0047(11) 0.0042(11) -0.0057(11) C2 0.0298(14) 0.0430(15) 0.0259(14) -0.0087(11) 0.0065(12) -0.0060(12) C3 0.0374(16) 0.0488(17) 0.0405(17) -0.0161(13) 0.0121(14) -0.0021(14) C4 0.0342(16) 0.069(2) 0.0385(17) -0.0166(15) 0.0193(14) -0.0082(15) C5 0.0370(16) 0.0570(18) 0.0346(16) -0.0048(14) 0.0175(13) -0.0156(14) C6 0.0312(14) 0.0456(16) 0.0247(13) 0.0003(11) 0.0062(12) -0.0058(12) C7 0.0419(16) 0.0428(16) 0.0373(16) 0.0035(13) 0.0147(14) -0.0106(13) C8 0.054(2) 0.0535(18) 0.057(2) -0.0069(16) 0.0112(18) -0.0182(16) C9 0.064(2) 0.067(2) 0.049(2) 0.0174(17) 0.0109(18) -0.0060(18) C10 0.0369(16) 0.0350(14) 0.0394(16) -0.0059(12) 0.0155(13) -0.0007(12) C11 0.0473(18) 0.0402(16) 0.0504(19) -0.0101(14) 0.0146(16) -0.0055(14) C12 0.069(2) 0.0484(17) 0.0444(19) -0.0011(14) 0.0078(17) -0.0024(17) C14 0.0304(14) 0.0251(12) 0.0232(13) 0.0017(10) 0.0031(11) -0.0044(11) C15 0.0230(13) 0.0332(13) 0.0231(13) 0.0032(10) -0.0021(10) -0.0006(11) C16 0.0242(13) 0.0263(12) 0.0269(13) 0.0009(10) 0.0048(11) 0.0001(10) C17 0.0366(16) 0.0591(18) 0.0268(14) -0.0033(13) 0.0012(13) -0.0047(14) C18 0.0252(14) 0.0435(15) 0.0308(14) 0.0042(12) 0.0031(12) -0.0017(12) C19 0.0212(12) 0.0391(14) 0.0241(13) 0.0027(11) 0.0041(11) -0.0004(11) C20 0.0309(15) 0.0464(16) 0.0288(14) -0.0014(12) 0.0089(12) 0.0004(13) C21 0.0473(18) 0.0612(19) 0.0290(15) -0.0071(14) 0.0110(14) 0.0039(15) C22 0.0451(18) 0.075(2) 0.0227(15) 0.0036(14) 0.0095(14) -0.0002(16) C23 0.0353(16) 0.0510(16) 0.0307(15) 0.0096(13) 0.0029(13) -0.0039(13) C24 0.0245(13) 0.0435(15) 0.0270(14) 0.0049(12) 0.0007(11) -0.0017(12) C25 0.0396(16) 0.0372(15) 0.0329(15) 0.0090(12) 0.0047(13) 0.0054(13) C26 0.052(2) 0.0483(18) 0.059(2) -0.0032(16) -0.0139(17) 0.0040(16) C27 0.0387(17) 0.0441(17) 0.060(2) 0.0089(15) 0.0008(16) 0.0040(14) C28 0.0450(17) 0.0390(15) 0.0342(15) -0.0032(12) 0.0116(14) 0.0067(13) C29 0.067(2) 0.0473(18) 0.054(2) -0.0063(15) 0.0142(18) 0.0036(17) C30 0.056(2) 0.0524(18) 0.055(2) -0.0053(15) 0.0164(17) 0.0197(16) C31 0.0383(16) 0.0387(15) 0.0339(15) 0.0007(12) 0.0018(13) 0.0006(13) C32 0.0346(15) 0.0312(13) 0.0313(15) -0.0023(11) 0.0082(12) -0.0022(12) C33 0.0326(15) 0.0386(15) 0.0311(15) -0.0004(12) 0.0058(12) 0.0012(12) C34 0.0349(16) 0.0404(15) 0.0458(18) -0.0073(13) 0.0054(14) -0.0044(13) C35 0.0395(17) 0.0471(17) 0.0380(17) -0.0051(13) 0.0010(14) 0.0022(14) C36 0.0485(19) 0.0440(17) 0.0416(17) 0.0063(14) 0.0070(15) 0.0095(15) C37 0.0472(18) 0.0353(15) 0.0437(18) 0.0006(13) 0.0117(15) 0.0005(14) C38 0.056(2) 0.0481(18) 0.056(2) -0.0066(15) -0.0120(17) -0.0126(16) C39 0.028(3) 0.0402(18) 0.038(4) 0.001(6) 0.003(5) -0.0049(18) C40 0.044(5) 0.055(5) 0.039(3) 0.002(3) -0.009(3) -0.007(3) C41 0.074(4) 0.082(5) 0.063(4) -0.004(3) -0.025(3) 0.006(3) C42 0.128(7) 0.085(6) 0.070(5) 0.018(4) -0.042(5) -0.002(5) C39A 0.028(3) 0.0402(18) 0.038(4) 0.001(6) 0.003(5) -0.0049(18) C40A 0.044(5) 0.055(5) 0.039(3) 0.002(3) -0.009(3) -0.007(3) C41A 0.074(4) 0.082(5) 0.063(4) -0.004(3) -0.025(3) 0.006(3) C42A 0.128(7) 0.085(6) 0.070(5) 0.018(4) -0.042(5) -0.002(5) C42B 0.128(7) 0.085(6) 0.070(5) 0.018(4) -0.042(5) -0.002(5) C1S 0.025(2) 0.036(3) 0.025(3) -0.014(2) -0.013(2) -0.011(2) C2S 0.033(3) 0.048(3) 0.045(3) 0.021(3) -0.002(3) -0.010(2) C3S 0.066(5) 0.051(4) 0.108(6) 0.056(4) -0.048(4) -0.035(3) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mg1 N2 2.070(2) . ? Mg1 N1 2.077(2) . ? Mg1 C39 2.09(3) . ? Mg1 N3 2.145(2) . ? Mg1 C39A 2.19(3) . ? N1 C14 1.334(3) . ? N1 C1 1.441(3) . ? N2 C16 1.324(3) . ? N2 C19 1.444(3) . ? N3 C31 1.337(3) . ? N3 C33 1.380(3) . ? N5 C31 1.336(3) . ? N5 C32 1.396(4) . ? N5 C38 1.456(4) . ? C1 C2 1.404(4) . ? C1 C6 1.413(3) . ? C2 C3 1.394(3) . ? C2 C10 1.526(4) . ? C3 C4 1.381(4) . ? C3 H3 0.9500 . ? C4 C5 1.374(4) . ? C4 H4 0.9500 . ? C5 C6 1.387(4) . ? C5 H5 0.9500 . ? C6 C7 1.512(4) . ? C7 C8 1.520(4) . ? C7 C9 1.527(4) . ? C7 H7 1.0000 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C12 1.520(4) . ? C10 C11 1.540(4) . ? C10 H10 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C14 C15 1.403(3) . ? C14 C17 1.512(3) . ? C15 C16 1.412(3) . ? C15 H15 0.9500 . ? C16 C18 1.514(3) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C24 1.404(3) . ? C19 C20 1.405(3) . ? C20 C21 1.395(4) . ? C20 C28 1.517(4) . ? C21 C22 1.369(4) . ? C21 H21 0.9500 . ? C22 C23 1.380(4) . ? C22 H22 0.9500 . ? C23 C24 1.389(4) . ? C23 H23 0.9500 . ? C24 C25 1.522(4) . ? C25 C27 1.519(4) . ? C25 C26 1.530(4) . ? C25 H25 1.0000 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 C29 1.516(4) . ? C28 C30 1.532(4) . ? C28 H28 1.0000 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31 0.9500 . ? C32 C37 1.376(4) . ? C32 C33 1.397(3) . ? C33 C34 1.379(4) . ? C34 C35 1.399(4) . ? C34 H34 0.9500 . ? C35 C36 1.377(4) . ? C35 H35 0.9500 . ? C36 C37 1.396(4) . ? C36 H36 0.9500 . ? C37 H37 0.9500 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 C40 1.523(8) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 C41 1.548(8) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 C42 1.464(8) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C41 H41C 1.2833 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C39A C40A 1.529(8) . ? C39A H39C 0.9900 . ? C39A H39D 0.9900 . ? C40A C41A 1.533(8) . ? C40A H40C 0.9900 . ? C40A H40D 0.9900 . ? C41A C42A 1.468(9) . ? C41A C42B 1.518(9) . ? C41A H41C 0.9900 . ? C41A H41D 0.9900 . ? C42A H42G 0.9800 . ? C42A H42H 0.9800 . ? C42A H42I 0.9800 . ? C42B H41D 0.7818 . ? C42B H42D 0.9800 . ? C42B H42E 0.9800 . ? C42B H42F 0.9800 . ? C1S C2S 1.487(8) . ? C1S C1S 1.578(10) 3_576 ? C1S H1S1 0.9900 . ? C1S H1S2 0.9900 . ? C2S C3S 1.513(7) . ? C2S H2S1 0.9900 . ? C2S H2S2 0.9900 . ? C3S H3S1 0.9800 . ? C3S H3S2 0.9800 . ? C3S H3S3 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 N2 Mg1 N1 91.73(8) . . ? N2 Mg1 C39 125.1(8) . . ? N1 Mg1 C39 120.5(6) . . ? N2 Mg1 N3 106.44(9) . . ? N1 Mg1 N3 106.85(9) . . ? C39 Mg1 N3 104.6(10) . . ? N2 Mg1 C39A 118.8(8) . . ? N1 Mg1 C39A 127.3(6) . . ? C39 Mg1 C39A 7.7(11) . . ? N3 Mg1 C39A 104.0(10) . . ? C14 N1 C1 116.9(2) . . ? C14 N1 Mg1 120.61(15) . . ? C1 N1 Mg1 122.43(16) . . ? C16 N2 C19 118.96(19) . . ? C16 N2 Mg1 122.24(15) . . ? C19 N2 Mg1 118.65(16) . . ? C31 N3 C33 104.4(2) . . ? C31 N3 Mg1 121.02(19) . . ? C33 N3 Mg1 134.12(19) . . ? C31 N5 C32 106.7(2) . . ? C31 N5 C38 127.3(3) . . ? C32 N5 C38 125.9(2) . . ? C2 C1 C6 120.1(2) . . ? C2 C1 N1 119.4(2) . . ? C6 C1 N1 120.4(2) . . ? C3 C2 C1 119.0(2) . . ? C3 C2 C10 118.8(2) . . ? C1 C2 C10 122.1(2) . . ? C4 C3 C2 121.0(3) . . ? C4 C3 H3 119.5 . . ? C2 C3 H3 119.5 . . ? C5 C4 C3 119.6(2) . . ? C5 C4 H4 120.2 . . ? C3 C4 H4 120.2 . . ? C4 C5 C6 121.9(2) . . ? C4 C5 H5 119.0 . . ? C6 C5 H5 119.0 . . ? C5 C6 C1 118.4(2) . . ? C5 C6 C7 119.6(2) . . ? C1 C6 C7 122.0(2) . . ? C6 C7 C8 111.1(3) . . ? C6 C7 C9 112.4(2) . . ? C8 C7 C9 110.8(2) . . ? C6 C7 H7 107.4 . . ? C8 C7 H7 107.4 . . ? C9 C7 H7 107.4 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C12 C10 C2 110.7(2) . . ? C12 C10 C11 111.0(2) . . ? C2 C10 C11 112.0(2) . . ? C12 C10 H10 107.6 . . ? C2 C10 H10 107.6 . . ? C11 C10 H10 107.6 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N1 C14 C15 124.6(2) . . ? N1 C14 C17 120.1(2) . . ? C15 C14 C17 115.3(2) . . ? C14 C15 C16 129.5(2) . . ? C14 C15 H15 115.2 . . ? C16 C15 H15 115.2 . . ? N2 C16 C15 123.6(2) . . ? N2 C16 C18 120.3(2) . . ? C15 C16 C18 116.1(2) . . ? C14 C17 H17A 109.5 . . ? C14 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C14 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C24 C19 C20 120.7(2) . . ? C24 C19 N2 118.8(2) . . ? C20 C19 N2 120.4(2) . . ? C21 C20 C19 118.0(2) . . ? C21 C20 C28 119.3(2) . . ? C19 C20 C28 122.6(2) . . ? C22 C21 C20 121.7(3) . . ? C22 C21 H21 119.2 . . ? C20 C21 H21 119.2 . . ? C21 C22 C23 119.9(3) . . ? C21 C22 H22 120.1 . . ? C23 C22 H22 120.1 . . ? C22 C23 C24 121.0(3) . . ? C22 C23 H23 119.5 . . ? C24 C23 H23 119.5 . . ? C23 C24 C19 118.7(2) . . ? C23 C24 C25 119.4(2) . . ? C19 C24 C25 121.9(2) . . ? C27 C25 C24 112.4(2) . . ? C27 C25 C26 110.4(2) . . ? C24 C25 C26 110.6(2) . . ? C27 C25 H25 107.8 . . ? C24 C25 H25 107.8 . . ? C26 C25 H25 107.8 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C29 C28 C20 110.1(3) . . ? C29 C28 C30 109.8(2) . . ? C20 C28 C30 112.8(2) . . ? C29 C28 H28 108.0 . . ? C20 C28 H28 108.0 . . ? C30 C28 H28 108.0 . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C28 C30 H30A 109.5 . . ? C28 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C28 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? N5 C31 N3 113.6(3) . . ? N5 C31 H31 123.2 . . ? N3 C31 H31 123.2 . . ? C37 C32 N5 130.9(2) . . ? C37 C32 C33 123.9(3) . . ? N5 C32 C33 105.2(2) . . ? C34 C33 N3 130.2(2) . . ? C34 C33 C32 119.7(2) . . ? N3 C33 C32 110.1(2) . . ? C33 C34 C35 117.2(3) . . ? C33 C34 H34 121.4 . . ? C35 C34 H34 121.4 . . ? C36 C35 C34 122.0(3) . . ? C36 C35 H35 119.0 . . ? C34 C35 H35 119.0 . . ? C35 C36 C37 121.5(3) . . ? C35 C36 H36 119.2 . . ? C37 C36 H36 119.2 . . ? C32 C37 C36 115.6(3) . . ? C32 C37 H37 122.2 . . ? C36 C37 H37 122.2 . . ? N5 C38 H38A 109.5 . . ? N5 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? N5 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C40 C39 Mg1 122.9(16) . . ? C40 C39 H39A 106.6 . . ? Mg1 C39 H39A 106.6 . . ? C40 C39 H39B 106.6 . . ? Mg1 C39 H39B 106.6 . . ? H39A C39 H39B 106.6 . . ? C39 C40 C41 115.5(13) . . ? C39 C40 H40A 108.4 . . ? C41 C40 H40A 108.4 . . ? C39 C40 H40B 108.4 . . ? C41 C40 H40B 108.4 . . ? H40A C40 H40B 107.5 . . ? C42 C41 C40 119.1(8) . . ? C42 C41 H41A 107.5 . . ? C40 C41 H41A 107.5 . . ? C42 C41 H41B 107.5 . . ? C40 C41 H41B 107.5 . . ? H41A C41 H41B 107.0 . . ? C42 C41 H41C 79.9 . . ? C40 C41 H41C 79.8 . . ? H41A C41 H41C 163.9 . . ? H41B C41 H41C 56.9 . . ? C41 C42 H41D 85.3 . . ? H42A C42 H41D 52.9 . . ? H42B C42 H41D 161.1 . . ? H42C C42 H41D 74.9 . . ? C40A C39A Mg1 115.5(16) . . ? C40A C39A H39C 108.4 . . ? Mg1 C39A H39C 108.4 . . ? C40A C39A H39D 108.4 . . ? Mg1 C39A H39D 108.4 . . ? H39C C39A H39D 107.5 . . ? C39A C40A C41A 114.8(12) . . ? C39A C40A H40C 108.6 . . ? C41A C40A H40C 108.6 . . ? C39A C40A H40D 108.6 . . ? C41A C40A H40D 108.6 . . ? H40C C40A H40D 107.5 . . ? C42A C41A C42B 79.6(11) . . ? C42A C41A C40A 120.2(11) . . ? C42B C41A C40A 117.8(11) . . ? C42A C41A H41C 108.4 . . ? C42B C41A H41C 121.7 . . ? C40A C41A H41C 107.2 . . ? C42A C41A H41D 106.2 . . ? C42B C41A H41D 27.2 . . ? C40A C41A H41D 107.5 . . ? H41C C41A H41D 106.7 . . ? C41A C42A H42G 109.5 . . ? C41A C42A H42H 109.5 . . ? H42G C42A H42H 109.5 . . ? C41A C42A H42I 109.5 . . ? H42G C42A H42I 109.5 . . ? H42H C42A H42I 109.5 . . ? C41A C42B H41D 35.4 . . ? C41A C42B H42D 109.5 . . ? H41D C42B H42D 140.0 . . ? C41A C42B H42E 109.5 . . ? H41D C42B H42E 79.9 . . ? H42D C42B H42E 109.5 . . ? C41A C42B H42F 109.5 . . ? H41D C42B H42F 103.0 . . ? H42D C42B H42F 109.5 . . ? H42E C42B H42F 109.5 . . ? C2S C1S C1S 111.4(5) . 3_576 ? C2S C1S H1S1 109.3 . . ? C1S C1S H1S1 109.3 3_576 . ? C2S C1S H1S2 109.3 . . ? C1S C1S H1S2 109.3 3_576 . ? H1S1 C1S H1S2 108.0 . . ? C1S C2S C3S 111.6(5) . . ? C1S C2S H2S1 109.3 . . ? C3S C2S H2S1 109.3 . . ? C1S C2S H2S2 109.3 . . ? C3S C2S H2S2 109.3 . . ? H2S1 C2S H2S2 108.0 . . ? C2S C3S H3S1 109.5 . . ? C2S C3S H3S2 109.5 . . ? H3S1 C3S H3S2 109.5 . . ? C2S C3S H3S3 109.5 . . ? H3S1 C3S H3S3 109.5 . . ? H3S2 C3S H3S3 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Mg1 N1 C14 26.30(18) . . . . ? C39 Mg1 N1 C14 159.6(11) . . . . ? N3 Mg1 N1 C14 -81.46(18) . . . . ? C39A Mg1 N1 C14 155.3(12) . . . . ? N2 Mg1 N1 C1 -156.05(18) . . . . ? C39 Mg1 N1 C1 -22.8(11) . . . . ? N3 Mg1 N1 C1 96.19(18) . . . . ? C39A Mg1 N1 C1 -27.1(12) . . . . ? N1 Mg1 N2 C16 -24.52(18) . . . . ? C39 Mg1 N2 C16 -154.5(10) . . . . ? N3 Mg1 N2 C16 83.61(19) . . . . ? C39A Mg1 N2 C16 -159.7(9) . . . . ? N1 Mg1 N2 C19 159.95(17) . . . . ? C39 Mg1 N2 C19 30.0(10) . . . . ? N3 Mg1 N2 C19 -91.92(17) . . . . ? C39A Mg1 N2 C19 24.8(9) . . . . ? N2 Mg1 N3 C31 127.0(2) . . . . ? N1 Mg1 N3 C31 -136.00(19) . . . . ? C39 Mg1 N3 C31 -7.1(6) . . . . ? C39A Mg1 N3 C31 0.8(6) . . . . ? N2 Mg1 N3 C33 -62.2(2) . . . . ? N1 Mg1 N3 C33 34.8(3) . . . . ? C39 Mg1 N3 C33 163.7(6) . . . . ? C39A Mg1 N3 C33 171.6(6) . . . . ? C14 N1 C1 C2 -79.2(3) . . . . ? Mg1 N1 C1 C2 103.1(2) . . . . ? C14 N1 C1 C6 102.6(3) . . . . ? Mg1 N1 C1 C6 -75.2(3) . . . . ? C6 C1 C2 C3 0.0(4) . . . . ? N1 C1 C2 C3 -178.3(2) . . . . ? C6 C1 C2 C10 179.4(2) . . . . ? N1 C1 C2 C10 1.1(4) . . . . ? C1 C2 C3 C4 -0.8(4) . . . . ? C10 C2 C3 C4 179.8(3) . . . . ? C2 C3 C4 C5 1.4(5) . . . . ? C3 C4 C5 C6 -1.1(5) . . . . ? C4 C5 C6 C1 0.3(4) . . . . ? C4 C5 C6 C7 -179.5(3) . . . . ? C2 C1 C6 C5 0.3(4) . . . . ? N1 C1 C6 C5 178.5(2) . . . . ? C2 C1 C6 C7 -180.0(2) . . . . ? N1 C1 C6 C7 -1.7(4) . . . . ? C5 C6 C7 C8 -65.2(3) . . . . ? C1 C6 C7 C8 115.1(3) . . . . ? C5 C6 C7 C9 59.6(4) . . . . ? C1 C6 C7 C9 -120.2(3) . . . . ? C3 C2 C10 C12 73.0(3) . . . . ? C1 C2 C10 C12 -106.4(3) . . . . ? C3 C2 C10 C11 -51.5(4) . . . . ? C1 C2 C10 C11 129.1(3) . . . . ? C1 N1 C14 C15 167.8(2) . . . . ? Mg1 N1 C14 C15 -14.4(3) . . . . ? C1 N1 C14 C17 -11.1(3) . . . . ? Mg1 N1 C14 C17 166.68(17) . . . . ? N1 C14 C15 C16 -11.1(4) . . . . ? C17 C14 C15 C16 167.8(2) . . . . ? C19 N2 C16 C15 -174.3(2) . . . . ? Mg1 N2 C16 C15 10.2(3) . . . . ? C19 N2 C16 C18 3.6(3) . . . . ? Mg1 N2 C16 C18 -171.91(17) . . . . ? C14 C15 C16 N2 13.7(4) . . . . ? C14 C15 C16 C18 -164.3(2) . . . . ? C16 N2 C19 C24 99.7(3) . . . . ? Mg1 N2 C19 C24 -84.6(2) . . . . ? C16 N2 C19 C20 -83.5(3) . . . . ? Mg1 N2 C19 C20 92.1(2) . . . . ? C24 C19 C20 C21 -1.0(4) . . . . ? N2 C19 C20 C21 -177.6(2) . . . . ? C24 C19 C20 C28 177.4(2) . . . . ? N2 C19 C20 C28 0.7(4) . . . . ? C19 C20 C21 C22 0.9(4) . . . . ? C28 C20 C21 C22 -177.5(3) . . . . ? C20 C21 C22 C23 -0.2(5) . . . . ? C21 C22 C23 C24 -0.5(5) . . . . ? C22 C23 C24 C19 0.4(4) . . . . ? C22 C23 C24 C25 -178.8(3) . . . . ? C20 C19 C24 C23 0.4(4) . . . . ? N2 C19 C24 C23 177.1(2) . . . . ? C20 C19 C24 C25 179.6(2) . . . . ? N2 C19 C24 C25 -3.7(4) . . . . ? C23 C24 C25 C27 -51.7(3) . . . . ? C19 C24 C25 C27 129.1(3) . . . . ? C23 C24 C25 C26 72.2(3) . . . . ? C19 C24 C25 C26 -107.1(3) . . . . ? C21 C20 C28 C29 70.1(3) . . . . ? C19 C20 C28 C29 -108.2(3) . . . . ? C21 C20 C28 C30 -52.9(4) . . . . ? C19 C20 C28 C30 128.8(3) . . . . ? C32 N5 C31 N3 -0.7(3) . . . . ? C38 N5 C31 N3 178.3(3) . . . . ? C33 N3 C31 N5 0.1(3) . . . . ? Mg1 N3 C31 N5 173.32(17) . . . . ? C31 N5 C32 C37 -177.0(3) . . . . ? C38 N5 C32 C37 4.1(4) . . . . ? C31 N5 C32 C33 0.9(3) . . . . ? C38 N5 C32 C33 -178.0(3) . . . . ? C31 N3 C33 C34 179.7(3) . . . . ? Mg1 N3 C33 C34 7.8(4) . . . . ? C31 N3 C33 C32 0.5(3) . . . . ? Mg1 N3 C33 C32 -171.39(18) . . . . ? C37 C32 C33 C34 -2.0(4) . . . . ? N5 C32 C33 C34 179.8(2) . . . . ? C37 C32 C33 N3 177.2(2) . . . . ? N5 C32 C33 N3 -0.9(3) . . . . ? N3 C33 C34 C35 -177.4(3) . . . . ? C32 C33 C34 C35 1.7(4) . . . . ? C33 C34 C35 C36 -0.7(4) . . . . ? C34 C35 C36 C37 -0.1(4) . . . . ? N5 C32 C37 C36 178.8(3) . . . . ? C33 C32 C37 C36 1.2(4) . . . . ? C35 C36 C37 C32 -0.2(4) . . . . ? N2 Mg1 C39 C40 -45(3) . . . . ? N1 Mg1 C39 C40 -162.1(18) . . . . ? N3 Mg1 C39 C40 78(2) . . . . ? C39A Mg1 C39 C40 -9(12) . . . . ? Mg1 C39 C40 C41 170.6(16) . . . . ? C39 C40 C41 C42 178.8(17) . . . . ? N2 Mg1 C39A C40A -48(2) . . . . ? N1 Mg1 C39A C40A -165.3(14) . . . . ? C39 Mg1 C39A C40A 166(17) . . . . ? N3 Mg1 C39A C40A 70(2) . . . . ? Mg1 C39A C40A C41A -171.8(14) . . . . ? C39A C40A C41A C42A -69(2) . . . . ? C39A C40A C41A C42B -163.2(18) . . . . ? C1S C1S C2S C3S -174.7(6) 3_576 . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.707 _refine_diff_density_min -0.331 _refine_diff_density_rms 0.060 #===END