# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email m.s.hill@bath.ac.uk _publ_contact_author_name 'Michael Hill' loop_ _publ_author_name M.S.Hill G.Kociok-Kohn D.J.MacDougall M.F.Mahon C.Weetman data_2-h10msh19 _database_code_depnum_ccdc_archive 'CCDC 831736' #TrackingRef '- bigcif.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C39 H57 Mg N3' _chemical_formula_weight 592.19 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 0.0486 0.0363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 15.8710(2) _cell_length_b 24.1760(4) _cell_length_c 19.3490(3) _cell_angle_alpha 90.00 _cell_angle_beta 98.312(1) _cell_angle_gamma 90.00 _cell_volume 7346.17(19) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 205787 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 27.485 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.071 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2592 _exptl_absorpt_coefficient_mu 0.077 # Absorption correction _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.882 _exptl_absorpt_correction_T_max 0.993 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_measurement_device_type '95mm CCD camera on \k-goniostat' _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 133599 _diffrn_reflns_av_R_equivalents 0.1155 _diffrn_reflns_av_sigmaI/netI 0.0702 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 4.27 _diffrn_reflns_theta_max 27.48 _reflns_number_total 16753 _reflns_number_gt 8649 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Collect (Bruker AXS BV 1997-2004)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo & Scalepack (Otwinowski, Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick 1990)' _computing_structure_refinement 'SHELXL-97/2 (Sheldrick 1997)' _computing_molecular_graphics 'ORTEX (P.McArdle 1995)' _computing_publication_material 'SHELXL-97/2 (Sheldrick 1997)' _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. Asymmetric unit consists of 2 molecules. Disorder was modeled as follows: The ligand based on N3 was modeled over 2 positions in a 50:50 ratio, while that based on N6 in addition to the butyl group based on C30 were modeled over 2 sites in a 70:30 split. Disordered aromatic groups were treated as rigid hexagons in the refinement and only partial atoms with 50% occupancy or above were refined anisotropically. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0594P)^2^+5.3631P] 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 16753 _refine_ls_number_parameters 862 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1506 _refine_ls_R_factor_gt 0.0663 _refine_ls_wR_factor_ref 0.1919 _refine_ls_wR_factor_gt 0.1442 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.029 _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 C1 C 0.29470(18) 0.03743(13) 0.68137(17) 0.0571(8) Uani 1 1 d . . . H1A H 0.3129 0.0064 0.7125 0.086 Uiso 1 1 calc R . . H1B H 0.2768 0.0236 0.6339 0.086 Uiso 1 1 calc R . . H1C H 0.2469 0.0565 0.6979 0.086 Uiso 1 1 calc R . . C2 C 0.36844(16) 0.07760(11) 0.68101(14) 0.0423(6) Uani 1 1 d . . . C3 C 0.37003(16) 0.10609(11) 0.61763(15) 0.0457(7) Uani 1 1 d . . . H3 H 0.3193 0.1036 0.5851 0.055 Uiso 1 1 calc R . . C4 C 0.43557(16) 0.13760(11) 0.59549(14) 0.0433(6) Uani 1 1 d . . . C5 C 0.4242(2) 0.15176(14) 0.51864(15) 0.0602(8) Uani 1 1 d . . . H5A H 0.4356 0.1912 0.5130 0.090 Uiso 1 1 calc R . . H5B H 0.3657 0.1434 0.4976 0.090 Uiso 1 1 calc R . . H5C H 0.4640 0.1299 0.4955 0.090 Uiso 1 1 calc R . . C6 C 0.42667(17) 0.04769(11) 0.79533(15) 0.0455(6) Uani 1 1 d . . . C7 C 0.3770(2) 0.05995(12) 0.84789(16) 0.0541(7) Uani 1 1 d . . . C8 C 0.3837(2) 0.02482(14) 0.90569(18) 0.0679(9) Uani 1 1 d . . . H8 H 0.3505 0.0321 0.9417 0.081 Uiso 1 1 calc R . . C9 C 0.4375(2) -0.02018(15) 0.91172(19) 0.0708(10) Uani 1 1 d . . . H9 H 0.4408 -0.0437 0.9514 0.085 Uiso 1 1 calc R . . C10 C 0.4862(2) -0.03094(13) 0.86049(18) 0.0642(9) Uani 1 1 d . . . H10 H 0.5232 -0.0621 0.8652 0.077 Uiso 1 1 calc R . . C11 C 0.48308(18) 0.00239(11) 0.80172(15) 0.0506(7) Uani 1 1 d . . . C12 C 0.3186(2) 0.10959(13) 0.84428(18) 0.0627(8) Uani 1 1 d . . . H12 H 0.3205 0.1283 0.7985 0.075 Uiso 1 1 calc R . . C13 C 0.2257(2) 0.09309(17) 0.8473(2) 0.0852(11) Uani 1 1 d . . . H13A H 0.2061 0.0679 0.8086 0.128 Uiso 1 1 calc R . . H13B H 0.1899 0.1263 0.8434 0.128 Uiso 1 1 calc R . . H13C H 0.2219 0.0746 0.8918 0.128 Uiso 1 1 calc R . . C14 C 0.3495(3) 0.15112(15) 0.9021(2) 0.0831(11) Uani 1 1 d . . . H14A H 0.3471 0.1341 0.9477 0.125 Uiso 1 1 calc R . . H14B H 0.3130 0.1840 0.8968 0.125 Uiso 1 1 calc R . . H14C H 0.4083 0.1619 0.8986 0.125 Uiso 1 1 calc R . . C15 C 0.53989(18) -0.00866(12) 0.74598(16) 0.0540(7) Uani 1 1 d . . . H15 H 0.5554 0.0281 0.7276 0.065 Uiso 1 1 calc R . . C16 C 0.4940(2) -0.04145(14) 0.68434(18) 0.0675(9) Uani 1 1 d . . . H16A H 0.4766 -0.0775 0.7007 0.101 Uiso 1 1 calc R . . H16B H 0.5324 -0.0470 0.6496 0.101 Uiso 1 1 calc R . . H16C H 0.4435 -0.0210 0.6632 0.101 Uiso 1 1 calc R . . C17 C 0.6234(2) -0.03789(14) 0.7753(2) 0.0734(10) Uani 1 1 d . . . H17A H 0.6110 -0.0757 0.7891 0.110 Uiso 1 1 calc R . . H17B H 0.6513 -0.0176 0.8162 0.110 Uiso 1 1 calc R . . H17C H 0.6611 -0.0390 0.7395 0.110 Uiso 1 1 calc R . . C18 C 0.57412(16) 0.17594(11) 0.60384(13) 0.0432(6) Uani 1 1 d . . . C19 C 0.63135(17) 0.13957(13) 0.57818(15) 0.0503(7) Uani 1 1 d . . . C20 C 0.6977(2) 0.16197(16) 0.54731(17) 0.0659(9) Uani 1 1 d . . . H20 H 0.7364 0.1378 0.5293 0.079 Uiso 1 1 calc R . . C21 C 0.7087(2) 0.21786(17) 0.5422(2) 0.0783(11) Uani 1 1 d . . . H21 H 0.7543 0.2321 0.5208 0.094 Uiso 1 1 calc R . . C22 C 0.6533(2) 0.25333(15) 0.56836(18) 0.0709(10) Uani 1 1 d . . . H22 H 0.6616 0.2921 0.5652 0.085 Uiso 1 1 calc R . . C23 C 0.58512(19) 0.23350(12) 0.59949(15) 0.0528(7) Uani 1 1 d . . . C24 C 0.6231(2) 0.07714(13) 0.58322(16) 0.0578(8) Uani 1 1 d . . . H24 H 0.5708 0.0691 0.6047 0.069 Uiso 1 1 calc R . . C25 C 0.6994(3) 0.05232(17) 0.6310(2) 0.0867(12) Uani 1 1 d . . . H25A H 0.7518 0.0597 0.6113 0.130 Uiso 1 1 calc R . . H25B H 0.6915 0.0123 0.6348 0.130 Uiso 1 1 calc R . . H25C H 0.7035 0.0691 0.6775 0.130 Uiso 1 1 calc R . . C26 C 0.6129(3) 0.04887(15) 0.51185(19) 0.0792(11) Uani 1 1 d . . . H26A H 0.5654 0.0658 0.4811 0.119 Uiso 1 1 calc R . . H26B H 0.6013 0.0094 0.5174 0.119 Uiso 1 1 calc R . . H26C H 0.6654 0.0532 0.4913 0.119 Uiso 1 1 calc R . . C27 C 0.5256(2) 0.27442(12) 0.62690(16) 0.0594(8) Uani 1 1 d . . . H27 H 0.4820 0.2524 0.6475 0.071 Uiso 1 1 calc R . . C28 C 0.5721(3) 0.30978(15) 0.68508(18) 0.0784(11) Uani 1 1 d . . . H28A H 0.6042 0.2859 0.7204 0.118 Uiso 1 1 calc R . . H28B H 0.5307 0.3315 0.7066 0.118 Uiso 1 1 calc R . . H28C H 0.6114 0.3348 0.6658 0.118 Uiso 1 1 calc R . . C29 C 0.4776(3) 0.31092(16) 0.5693(2) 0.0864(12) Uani 1 1 d . . . H29A H 0.5183 0.3345 0.5494 0.130 Uiso 1 1 calc R . . H29B H 0.4365 0.3341 0.5891 0.130 Uiso 1 1 calc R . . H29C H 0.4474 0.2874 0.5325 0.130 Uiso 1 1 calc R . . C30 C 0.6283(3) 0.1298(2) 0.8191(3) 0.0478(12) Uani 0.70 1 d P A 1 H30A H 0.6600 0.0992 0.8006 0.057 Uiso 0.70 1 calc PR A 1 H30B H 0.6653 0.1629 0.8222 0.057 Uiso 0.70 1 calc PR A 1 C31 C 0.6126(3) 0.1141(2) 0.8942(2) 0.0565(11) Uani 0.70 1 d P A 1 H31A H 0.5724 0.1414 0.9093 0.068 Uiso 0.70 1 calc PR A 1 H31B H 0.5841 0.0776 0.8920 0.068 Uiso 0.70 1 calc PR A 1 C32 C 0.6904(3) 0.11145(19) 0.9499(2) 0.0594(11) Uani 0.70 1 d P A 1 H32A H 0.7212 0.1471 0.9502 0.071 Uiso 0.70 1 calc PR A 1 H32B H 0.6710 0.1072 0.9960 0.071 Uiso 0.70 1 calc PR A 1 C33 C 0.7512(4) 0.0656(3) 0.9410(4) 0.0784(17) Uani 0.70 1 d P A 1 H33A H 0.7214 0.0301 0.9400 0.118 Uiso 0.70 1 calc PR A 1 H33B H 0.7980 0.0660 0.9800 0.118 Uiso 0.70 1 calc PR A 1 H33C H 0.7741 0.0707 0.8970 0.118 Uiso 0.70 1 calc PR A 1 C30A C 0.6448(12) 0.1363(9) 0.7969(9) 0.077(6) Uiso 0.30 1 d P A 2 H30C H 0.6779 0.1154 0.7660 0.093 Uiso 0.30 1 calc PR A 2 H30D H 0.6715 0.1731 0.8053 0.093 Uiso 0.30 1 calc PR A 2 C31A C 0.6489(8) 0.1049(5) 0.8684(7) 0.059(3) Uiso 0.30 1 d P A 2 H31C H 0.6235 0.1290 0.9012 0.071 Uiso 0.30 1 calc PR A 2 H31D H 0.6127 0.0715 0.8606 0.071 Uiso 0.30 1 calc PR A 2 C32A C 0.7338(7) 0.0875(5) 0.9028(6) 0.059(3) Uiso 0.30 1 d P A 2 H32C H 0.7695 0.1206 0.9151 0.071 Uiso 0.30 1 calc PR A 2 H32D H 0.7616 0.0648 0.8700 0.071 Uiso 0.30 1 calc PR A 2 C33A C 0.7270(12) 0.0536(8) 0.9697(9) 0.089(6) Uiso 0.30 1 d P A 2 H33D H 0.7124 0.0783 1.0063 0.134 Uiso 0.30 1 calc PR A 2 H33E H 0.7816 0.0356 0.9857 0.134 Uiso 0.30 1 calc PR A 2 H33F H 0.6826 0.0254 0.9595 0.134 Uiso 0.30 1 calc PR A 2 C40 C 0.91465(19) 0.30265(13) 0.51146(14) 0.0503(7) Uani 1 1 d . . . H40A H 0.9586 0.3192 0.4873 0.075 Uiso 1 1 calc R . . H40B H 0.8583 0.3139 0.4882 0.075 Uiso 1 1 calc R . . H40C H 0.9194 0.2623 0.5101 0.075 Uiso 1 1 calc R . . C41 C 0.92650(16) 0.32196(10) 0.58664(12) 0.0370(6) Uani 1 1 d . . . C42 C 0.85908(16) 0.35228(10) 0.60743(13) 0.0395(6) Uani 1 1 d . . . H42 H 0.8078 0.3519 0.5754 0.047 Uiso 1 1 calc R . . C43 C 0.85604(15) 0.38324(10) 0.66874(13) 0.0382(6) Uani 1 1 d . . . C44 C 0.78009(17) 0.42179(12) 0.66751(15) 0.0489(7) Uani 1 1 d . . . H44A H 0.7339 0.4024 0.6860 0.073 Uiso 1 1 calc R . . H44B H 0.7605 0.4334 0.6194 0.073 Uiso 1 1 calc R . . H44C H 0.7969 0.4544 0.6964 0.073 Uiso 1 1 calc R . . C45 C 1.06919(16) 0.29076(11) 0.59586(13) 0.0422(6) Uani 1 1 d . . . C46 C 1.08614(19) 0.23381(12) 0.59154(15) 0.0508(7) Uani 1 1 d . . . C47 C 1.1556(2) 0.21727(15) 0.55924(18) 0.0674(9) Uani 1 1 d . . . H47 H 1.1679 0.1790 0.5559 0.081 Uiso 1 1 calc R . . C48 C 1.2066(2) 0.25584(17) 0.53208(18) 0.0720(10) Uani 1 1 d . . . H48 H 1.2524 0.2439 0.5091 0.086 Uiso 1 1 calc R . . C49 C 1.1910(2) 0.31125(16) 0.53848(16) 0.0632(9) Uani 1 1 d . . . H49 H 1.2271 0.3374 0.5207 0.076 Uiso 1 1 calc R . . C50 C 1.12304(17) 0.33014(12) 0.57067(14) 0.0484(7) Uani 1 1 d . . . C51 C 1.0327(2) 0.19040(12) 0.62117(17) 0.0606(8) Uani 1 1 d . . . H51 H 0.9853 0.2099 0.6399 0.073 Uiso 1 1 calc R . . C52 C 0.9925(3) 0.14853(15) 0.5661(2) 0.0802(11) Uani 1 1 d . . . H52A H 0.9623 0.1684 0.5259 0.120 Uiso 1 1 calc R . . H52B H 0.9523 0.1249 0.5865 0.120 Uiso 1 1 calc R . . H52C H 1.0373 0.1256 0.5510 0.120 Uiso 1 1 calc R . . C53 C 1.0853(3) 0.15994(15) 0.68227(18) 0.0775(10) Uani 1 1 d . . . H53A H 1.1306 0.1388 0.6651 0.116 Uiso 1 1 calc R . . H53B H 1.0483 0.1347 0.7038 0.116 Uiso 1 1 calc R . . H53C H 1.1106 0.1869 0.7171 0.116 Uiso 1 1 calc R . . C54 C 1.1092(2) 0.39174(12) 0.57871(15) 0.0549(8) Uani 1 1 d . . . H54 H 1.0658 0.3964 0.6109 0.066 Uiso 1 1 calc R . . C55 C 1.1904(2) 0.42029(16) 0.6125(2) 0.0858(12) Uani 1 1 d . . . H55A H 1.2131 0.4009 0.6558 0.129 Uiso 1 1 calc R . . H55B H 1.1777 0.4587 0.6233 0.129 Uiso 1 1 calc R . . H55C H 1.2327 0.4195 0.5803 0.129 Uiso 1 1 calc R . . C56 C 1.0743(3) 0.41959(15) 0.50995(19) 0.0810(11) Uani 1 1 d . . . H56A H 1.1133 0.4132 0.4758 0.121 Uiso 1 1 calc R . . H56B H 1.0688 0.4594 0.5175 0.121 Uiso 1 1 calc R . . H56C H 1.0183 0.4040 0.4922 0.121 Uiso 1 1 calc R . . C57 C 0.91177(16) 0.41752(10) 0.78245(14) 0.0402(6) Uani 1 1 d . . . C58 C 0.96545(17) 0.46419(11) 0.78762(15) 0.0468(7) Uani 1 1 d . . . C59 C 0.9663(2) 0.49822(12) 0.84624(17) 0.0561(8) Uani 1 1 d . . . H59 H 1.0008 0.5305 0.8502 0.067 Uiso 1 1 calc R . . C60 C 0.9188(2) 0.48631(13) 0.89788(17) 0.0610(8) Uani 1 1 d . . . H60 H 0.9210 0.5100 0.9373 0.073 Uiso 1 1 calc R . . C61 C 0.86752(19) 0.43972(12) 0.89284(15) 0.0531(7) Uani 1 1 d . . . H61 H 0.8355 0.4313 0.9294 0.064 Uiso 1 1 calc R . . C62 C 0.86229(17) 0.40509(11) 0.83481(14) 0.0436(6) Uani 1 1 d . . . C63 C 1.02236(17) 0.47647(11) 0.73269(16) 0.0500(7) Uani 1 1 d . . . H63 H 1.0407 0.4400 0.7155 0.060 Uiso 1 1 calc R . . C64 C 0.9756(2) 0.50693(14) 0.66968(17) 0.0661(9) Uani 1 1 d . . . H64A H 0.9262 0.4852 0.6492 0.099 Uiso 1 1 calc R . . H64B H 1.0141 0.5122 0.6349 0.099 Uiso 1 1 calc R . . H64C H 0.9566 0.5431 0.6844 0.099 Uiso 1 1 calc R . . C65 C 1.1033(2) 0.50825(14) 0.76097(19) 0.0696(9) Uani 1 1 d . . . H65A H 1.1412 0.5095 0.7253 0.104 Uiso 1 1 calc R . . H65B H 1.1322 0.4896 0.8028 0.104 Uiso 1 1 calc R . . H65C H 1.0883 0.5460 0.7730 0.104 Uiso 1 1 calc R . . C66 C 0.80529(18) 0.35438(11) 0.83145(14) 0.0466(6) Uani 1 1 d . . . H66 H 0.8061 0.3364 0.7850 0.056 Uiso 1 1 calc R . . C67 C 0.8386(2) 0.31226(13) 0.88806(15) 0.0605(8) Uani 1 1 d . . . H67A H 0.8984 0.3039 0.8852 0.091 Uiso 1 1 calc R . . H67B H 0.8049 0.2782 0.8810 0.091 Uiso 1 1 calc R . . H67C H 0.8338 0.3277 0.9342 0.091 Uiso 1 1 calc R . . C68 C 0.71262(19) 0.36945(14) 0.83709(18) 0.0644(8) Uani 1 1 d . . . H68A H 0.7096 0.3859 0.8829 0.097 Uiso 1 1 calc R . . H68B H 0.6774 0.3360 0.8315 0.097 Uiso 1 1 calc R . . H68C H 0.6916 0.3960 0.8004 0.097 Uiso 1 1 calc R . . C69 C 1.12892(18) 0.34054(13) 0.79586(16) 0.0549(8) Uani 1 1 d . B . H69A H 1.1621 0.3060 0.8050 0.066 Uiso 1 1 calc R . . H69B H 1.1608 0.3648 0.7676 0.066 Uiso 1 1 calc R . . C70 C 1.12463(19) 0.36966(13) 0.86722(17) 0.0597(8) Uani 1 1 d . . . H70A H 1.0805 0.3988 0.8598 0.072 Uiso 1 1 calc R . . H70B H 1.1058 0.3421 0.8996 0.072 Uiso 1 1 calc R . . C71 C 1.2062(2) 0.39554(15) 0.90217(18) 0.0712(10) Uani 1 1 d . . . H71A H 1.2466 0.3659 0.9200 0.085 Uiso 1 1 calc R . . H71B H 1.2322 0.4170 0.8671 0.085 Uiso 1 1 calc R . . C72 C 1.1928(2) 0.43312(15) 0.96171(18) 0.0760(10) Uani 1 1 d . . . H72A H 1.1545 0.4633 0.9441 0.114 Uiso 1 1 calc R . . H72B H 1.2477 0.4485 0.9829 0.114 Uiso 1 1 calc R . . H72C H 1.1677 0.4120 0.9968 0.114 Uiso 1 1 calc R . . N3 N 0.4640(3) 0.22296(18) 0.7852(3) 0.055(3) Uani 0.50 1 d PG A 1 C34 C 0.5202(3) 0.2447(2) 0.8403(3) 0.059(2) Uani 0.50 1 d PG A 1 H34 H 0.5721 0.2261 0.8562 0.071 Uiso 0.50 1 calc PR A 1 C35 C 0.5002(3) 0.2935(2) 0.8722(2) 0.0616(17) Uani 0.50 1 d PG A 1 H35 H 0.5386 0.3084 0.9098 0.074 Uiso 0.50 1 calc PR A 1 C36 C 0.4242(4) 0.3207(2) 0.8489(3) 0.075(3) Uani 0.50 1 d PG A 1 H36 H 0.4106 0.3541 0.8707 0.090 Uiso 0.50 1 calc PR A 1 C37 C 0.3681(3) 0.2990(2) 0.7938(3) 0.065(2) Uani 0.50 1 d PG A 1 H37 H 0.3161 0.3175 0.7779 0.078 Uiso 0.50 1 calc PR A 1 C38 C 0.3880(3) 0.2501(2) 0.7619(2) 0.0537(15) Uani 0.50 1 d PG A 1 C39 C 0.3277(5) 0.2269(4) 0.7059(5) 0.079(3) Uani 0.50 1 d P A 1 H39A H 0.2718 0.2235 0.7213 0.118 Uiso 0.50 1 calc PR A 1 H39B H 0.3474 0.1902 0.6935 0.118 Uiso 0.50 1 calc PR A 1 H39C H 0.3232 0.2512 0.6650 0.118 Uiso 0.50 1 calc PR A 1 N3A N 0.4446(3) 0.21929(16) 0.7742(3) 0.0329(16) Uani 0.50 1 d PG A 2 C34A C 0.3692(3) 0.22498(16) 0.7283(2) 0.0436(16) Uani 0.50 1 d PG A 2 H34A H 0.3527 0.1973 0.6942 0.052 Uiso 0.50 1 calc PR A 2 C35A C 0.3180(2) 0.27120(18) 0.7322(3) 0.0528(15) Uani 0.50 1 d PG A 2 H35A H 0.2665 0.2751 0.7008 0.063 Uiso 0.50 1 calc PR A 2 C36A C 0.3422(3) 0.31173(19) 0.7821(3) 0.068(3) Uani 0.50 1 d PG A 2 H36A H 0.3072 0.3433 0.7848 0.081 Uiso 0.50 1 calc PR A 2 C37A C 0.4176(3) 0.30605(19) 0.8280(3) 0.063(2) Uani 0.50 1 d PG A 2 H37A H 0.4341 0.3338 0.8621 0.075 Uiso 0.50 1 calc PR A 2 C38A C 0.4688(2) 0.25983(18) 0.8241(2) 0.0477(16) Uani 0.50 1 d PG A 2 C39A C 0.5472(5) 0.2531(4) 0.8748(4) 0.069(2) Uani 0.50 1 d P A 2 H39D H 0.5679 0.2895 0.8919 0.103 Uiso 0.50 1 calc PR A 2 H39E H 0.5909 0.2347 0.8520 0.103 Uiso 0.50 1 calc PR A 2 H39F H 0.5348 0.2305 0.9142 0.103 Uiso 0.50 1 calc PR A 2 N6 N 0.94291(16) 0.24721(8) 0.76690(13) 0.0395(9) Uani 0.70 1 d PG B 1 C73 C 0.86554(17) 0.23969(9) 0.72411(12) 0.0440(9) Uani 0.70 1 d PG B 1 H73 H 0.8462 0.2664 0.6894 0.053 Uiso 0.70 1 calc PR B 1 C74 C 0.81654(14) 0.19310(10) 0.73209(13) 0.0510(10) Uani 0.70 1 d PG B 1 H74 H 0.7637 0.1880 0.7028 0.061 Uiso 0.70 1 calc PR B 1 C75 C 0.84490(16) 0.15403(9) 0.78286(15) 0.0509(10) Uani 0.70 1 d PG B 1 H75 H 0.8114 0.1222 0.7883 0.061 Uiso 0.70 1 calc PR B 1 C76 C 0.92226(17) 0.16155(9) 0.82565(13) 0.0461(10) Uani 0.70 1 d PG B 1 H76 H 0.9416 0.1348 0.8604 0.055 Uiso 0.70 1 calc PR B 1 C77 C 0.97127(14) 0.20814(10) 0.81767(12) 0.0425(9) Uani 0.70 1 d PG B 1 C78 C 1.0527(3) 0.21911(19) 0.8645(2) 0.0557(11) Uani 0.70 1 d P B 1 H78A H 1.0734 0.1847 0.8879 0.084 Uiso 0.70 1 calc PR B 1 H78B H 1.0430 0.2467 0.8996 0.084 Uiso 0.70 1 calc PR B 1 H78C H 1.0952 0.2331 0.8369 0.084 Uiso 0.70 1 calc PR B 1 N6A N 0.9663(4) 0.2447(2) 0.7791(3) 0.036(2) Uiso 0.30 1 d PG B 2 C73A C 1.0271(3) 0.2273(2) 0.8337(3) 0.036(2) Uiso 0.30 1 d PG B 2 H73A H 1.0764 0.2492 0.8477 0.043 Uiso 0.30 1 calc PR B 2 C74A C 1.0160(4) 0.1779(3) 0.8679(3) 0.047(2) Uiso 0.30 1 d PG B 2 H74A H 1.0576 0.1660 0.9053 0.057 Uiso 0.30 1 calc PR B 2 C75A C 0.9440(4) 0.1458(2) 0.8475(4) 0.058(3) Uiso 0.30 1 d PG B 2 H75A H 0.9364 0.1120 0.8709 0.070 Uiso 0.30 1 calc PR B 2 C76A C 0.8831(4) 0.1632(3) 0.7929(4) 0.046(3) Uiso 0.30 1 d PG B 2 H76A H 0.8339 0.1413 0.7790 0.056 Uiso 0.30 1 calc PR B 2 C77A C 0.8942(4) 0.2127(3) 0.7587(3) 0.042(2) Uiso 0.30 1 d PG B 2 C78A C 0.8281(7) 0.2306(5) 0.7008(6) 0.060(3) Uiso 0.30 1 d P B 2 H78D H 0.7724 0.2312 0.7171 0.091 Uiso 0.30 1 calc PR B 2 H78E H 0.8265 0.2048 0.6616 0.091 Uiso 0.30 1 calc PR B 2 H78F H 0.8417 0.2678 0.6855 0.091 Uiso 0.30 1 calc PR B 2 N1 N 0.42627(13) 0.08416(8) 0.73644(11) 0.0403(5) Uani 1 1 d . A . N2 N 0.50587(13) 0.15382(8) 0.63739(11) 0.0398(5) Uani 1 1 d . A . N4 N 0.99875(12) 0.31002(8) 0.62823(10) 0.0359(5) Uani 1 1 d . B . N5 N 0.91489(12) 0.38012(8) 0.72466(10) 0.0357(5) Uani 1 1 d . B . Mg1 Mg 0.51696(5) 0.14648(4) 0.74517(5) 0.0411(2) Uani 1 1 d . . . Mg2 Mg 1.01064(5) 0.32065(3) 0.73550(4) 0.0365(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0409(15) 0.0554(18) 0.074(2) -0.0090(16) 0.0036(14) -0.0140(14) C2 0.0349(13) 0.0364(14) 0.0548(16) -0.0066(12) 0.0043(12) -0.0022(11) C3 0.0338(14) 0.0460(15) 0.0542(17) -0.0066(13) -0.0048(12) -0.0023(12) C4 0.0410(15) 0.0423(15) 0.0452(15) -0.0027(12) 0.0009(12) 0.0022(12) C5 0.0552(18) 0.075(2) 0.0473(17) 0.0004(16) -0.0038(14) -0.0061(16) C6 0.0461(15) 0.0373(14) 0.0518(16) -0.0024(12) 0.0023(13) -0.0103(12) C7 0.0615(18) 0.0467(16) 0.0551(18) -0.0008(14) 0.0122(15) -0.0161(14) C8 0.081(2) 0.063(2) 0.061(2) -0.0014(17) 0.0150(18) -0.0241(19) C9 0.083(2) 0.064(2) 0.063(2) 0.0129(18) 0.0038(19) -0.021(2) C10 0.066(2) 0.0459(17) 0.076(2) 0.0111(16) -0.0065(18) -0.0096(15) C11 0.0504(16) 0.0398(15) 0.0580(18) -0.0010(14) -0.0041(14) -0.0095(13) C12 0.073(2) 0.0521(18) 0.069(2) -0.0052(16) 0.0325(17) -0.0099(16) C13 0.072(2) 0.083(3) 0.108(3) -0.001(2) 0.040(2) -0.003(2) C14 0.106(3) 0.068(2) 0.085(3) -0.018(2) 0.046(2) -0.017(2) C15 0.0474(16) 0.0403(15) 0.071(2) 0.0006(14) -0.0017(15) 0.0011(13) C16 0.0568(19) 0.066(2) 0.078(2) -0.0164(18) 0.0031(17) 0.0061(16) C17 0.057(2) 0.061(2) 0.098(3) -0.0026(19) -0.0022(19) 0.0133(16) C18 0.0408(14) 0.0491(16) 0.0398(14) -0.0035(12) 0.0057(11) -0.0073(12) C19 0.0428(15) 0.0603(18) 0.0477(16) -0.0080(14) 0.0072(13) -0.0041(14) C20 0.0585(19) 0.079(2) 0.065(2) -0.0169(18) 0.0262(16) -0.0091(17) C21 0.073(2) 0.088(3) 0.083(3) -0.016(2) 0.039(2) -0.030(2) C22 0.086(2) 0.060(2) 0.074(2) -0.0091(18) 0.035(2) -0.0277(19) C23 0.0573(18) 0.0524(17) 0.0497(17) -0.0064(14) 0.0116(14) -0.0123(14) C24 0.0538(18) 0.0569(18) 0.065(2) -0.0044(16) 0.0171(15) 0.0076(15) C25 0.086(3) 0.080(3) 0.089(3) -0.007(2) -0.004(2) 0.025(2) C26 0.096(3) 0.063(2) 0.077(2) -0.0153(19) 0.007(2) 0.002(2) C27 0.076(2) 0.0435(16) 0.0622(19) -0.0016(14) 0.0223(17) -0.0081(15) C28 0.108(3) 0.063(2) 0.069(2) -0.0180(18) 0.027(2) -0.019(2) C29 0.112(3) 0.063(2) 0.083(3) -0.002(2) 0.011(2) 0.009(2) C30 0.038(2) 0.044(3) 0.057(3) -0.003(2) -0.009(3) -0.006(2) C31 0.056(3) 0.066(3) 0.045(2) 0.000(2) -0.002(2) -0.003(2) C32 0.060(3) 0.063(3) 0.053(3) 0.001(2) 0.000(2) 0.002(2) C33 0.080(4) 0.069(4) 0.081(5) -0.017(4) -0.007(4) 0.016(3) C40 0.0525(17) 0.0588(18) 0.0390(15) -0.0019(13) 0.0044(13) 0.0000(14) C41 0.0403(14) 0.0337(13) 0.0358(13) 0.0041(11) 0.0015(11) -0.0050(11) C42 0.0373(14) 0.0384(14) 0.0404(14) 0.0041(11) -0.0028(11) -0.0039(11) C43 0.0373(13) 0.0319(13) 0.0444(15) 0.0060(11) 0.0027(11) -0.0011(11) C44 0.0445(15) 0.0469(16) 0.0534(17) -0.0003(13) 0.0004(13) 0.0082(13) C45 0.0409(14) 0.0512(16) 0.0341(13) 0.0005(12) 0.0044(11) 0.0018(12) C46 0.0551(17) 0.0505(17) 0.0490(16) 0.0028(13) 0.0146(14) 0.0106(14) C47 0.072(2) 0.065(2) 0.069(2) -0.0004(17) 0.0258(18) 0.0197(18) C48 0.058(2) 0.095(3) 0.069(2) -0.005(2) 0.0292(17) 0.012(2) C49 0.0533(18) 0.085(3) 0.0543(18) -0.0003(17) 0.0188(15) -0.0077(17) C50 0.0459(16) 0.0588(18) 0.0405(15) 0.0014(13) 0.0064(12) -0.0072(14) C51 0.079(2) 0.0402(16) 0.068(2) 0.0045(15) 0.0297(17) 0.0129(15) C52 0.098(3) 0.061(2) 0.081(2) 0.0039(19) 0.008(2) -0.004(2) C53 0.113(3) 0.060(2) 0.060(2) 0.0068(17) 0.014(2) 0.005(2) C54 0.0589(18) 0.0546(18) 0.0525(17) -0.0027(14) 0.0126(14) -0.0191(15) C55 0.085(3) 0.079(3) 0.090(3) 0.001(2) -0.002(2) -0.035(2) C56 0.101(3) 0.062(2) 0.075(2) 0.0042(19) -0.003(2) -0.002(2) C57 0.0387(14) 0.0319(13) 0.0479(15) -0.0009(11) -0.0008(12) 0.0072(11) C58 0.0465(15) 0.0330(13) 0.0582(17) -0.0043(13) -0.0019(13) 0.0032(12) C59 0.0593(18) 0.0351(15) 0.071(2) -0.0137(15) 0.0001(16) 0.0021(14) C60 0.068(2) 0.0505(18) 0.062(2) -0.0224(15) -0.0013(17) 0.0087(16) C61 0.0593(18) 0.0512(17) 0.0483(16) -0.0095(14) 0.0065(14) 0.0128(15) C62 0.0453(15) 0.0392(14) 0.0446(15) -0.0011(12) 0.0008(12) 0.0083(12) C63 0.0478(16) 0.0351(14) 0.0658(19) -0.0016(13) 0.0037(14) -0.0040(12) C64 0.063(2) 0.062(2) 0.071(2) 0.0116(17) 0.0026(17) -0.0061(16) C65 0.060(2) 0.058(2) 0.087(2) 0.0049(18) -0.0013(18) -0.0165(16) C66 0.0529(16) 0.0422(15) 0.0460(15) -0.0049(12) 0.0109(13) 0.0005(13) C67 0.081(2) 0.0532(18) 0.0508(17) 0.0042(14) 0.0220(16) 0.0081(16) C68 0.0555(19) 0.070(2) 0.070(2) -0.0075(17) 0.0145(16) -0.0040(16) C69 0.0495(17) 0.0496(16) 0.0616(19) 0.0075(14) -0.0052(14) -0.0044(14) C70 0.0567(18) 0.0523(18) 0.067(2) 0.0035(15) -0.0031(15) -0.0017(15) C71 0.069(2) 0.067(2) 0.070(2) 0.0040(18) -0.0151(18) -0.0025(18) C72 0.093(3) 0.065(2) 0.064(2) 0.0072(18) -0.0071(19) -0.008(2) N3 0.042(3) 0.071(6) 0.051(4) 0.009(4) 0.001(3) -0.017(3) C34 0.065(6) 0.046(4) 0.074(6) -0.005(4) 0.033(5) -0.002(4) C35 0.067(4) 0.057(4) 0.064(4) -0.014(3) 0.019(3) -0.010(4) C36 0.074(6) 0.065(6) 0.091(7) 0.006(5) 0.035(5) 0.002(5) C37 0.081(7) 0.043(4) 0.080(6) -0.009(5) 0.045(5) 0.010(5) C38 0.048(4) 0.054(4) 0.061(4) 0.012(3) 0.014(3) -0.006(3) C39 0.052(5) 0.091(6) 0.089(6) 0.010(5) -0.003(4) -0.007(5) N3A 0.037(3) 0.025(3) 0.037(3) -0.011(2) 0.008(2) 0.002(2) C34A 0.042(4) 0.039(3) 0.051(4) -0.009(3) 0.012(3) -0.004(3) C35A 0.048(3) 0.039(3) 0.073(4) -0.008(3) 0.013(3) 0.007(3) C36A 0.074(5) 0.035(4) 0.107(7) -0.014(4) 0.053(5) 0.003(4) C37A 0.064(6) 0.049(5) 0.083(6) -0.008(5) 0.035(5) -0.009(4) C38A 0.068(4) 0.035(3) 0.047(4) -0.016(3) 0.030(3) -0.020(3) C39A 0.080(6) 0.075(6) 0.052(5) -0.016(4) 0.010(4) -0.028(4) N6 0.045(2) 0.0384(19) 0.0355(18) 0.0015(14) 0.0067(17) 0.0070(16) C73 0.049(3) 0.035(2) 0.049(2) 0.0024(19) 0.011(2) -0.0019(19) C74 0.054(2) 0.044(2) 0.056(2) 0.000(2) 0.010(2) -0.0063(19) C75 0.059(3) 0.035(2) 0.062(3) 0.0054(19) 0.021(2) -0.002(2) C76 0.058(3) 0.033(2) 0.050(3) 0.001(2) 0.018(2) 0.001(2) C77 0.057(2) 0.037(2) 0.036(2) 0.0047(16) 0.0150(18) 0.0131(18) C78 0.061(3) 0.058(3) 0.046(3) 0.013(2) 0.002(2) 0.011(2) N1 0.0377(11) 0.0349(11) 0.0481(13) -0.0031(10) 0.0055(10) -0.0026(9) N2 0.0347(11) 0.0384(12) 0.0458(12) -0.0042(10) 0.0043(9) -0.0031(9) N4 0.0373(11) 0.0332(11) 0.0375(11) 0.0019(9) 0.0064(9) 0.0001(9) N5 0.0382(11) 0.0291(10) 0.0393(12) 0.0003(9) 0.0039(9) -0.0001(9) Mg1 0.0386(5) 0.0391(5) 0.0446(5) -0.0047(4) 0.0020(4) -0.0044(4) Mg2 0.0377(4) 0.0330(4) 0.0378(5) 0.0015(4) 0.0018(4) 0.0023(4) _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 C1 C2 1.522(4) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 N1 1.317(3) . ? C2 C3 1.410(4) . ? C3 C4 1.405(4) . ? C3 H3 0.9500 . ? C4 N2 1.340(3) . ? C4 C5 1.511(4) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 C7 1.406(4) . ? C6 C11 1.409(4) . ? C6 N1 1.440(3) . ? C7 C8 1.396(4) . ? C7 C12 1.512(4) . ? C8 C9 1.377(5) . ? C8 H8 0.9500 . ? C9 C10 1.367(5) . ? C9 H9 0.9500 . ? C10 C11 1.389(4) . ? C10 H10 0.9500 . ? C11 C15 1.526(4) . ? C12 C14 1.530(5) . ? C12 C13 1.535(5) . ? C12 H12 1.0000 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C16 1.527(4) . ? C15 C17 1.536(4) . ? C15 H15 1.0000 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C19 1.405(4) . ? C18 C23 1.406(4) . ? C18 N2 1.444(3) . ? C19 C20 1.393(4) . ? C19 C24 1.519(4) . ? C20 C21 1.368(5) . ? C20 H20 0.9500 . ? C21 C22 1.375(5) . ? C21 H21 0.9500 . ? C22 C23 1.397(4) . ? C22 H22 0.9500 . ? C23 C27 1.515(4) . ? C24 C26 1.528(4) . ? C24 C25 1.535(4) . ? C24 H24 1.0000 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C28 1.517(4) . ? C27 C29 1.535(5) . ? C27 H27 1.0000 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 C31 1.557(8) . ? C30 Mg1 2.144(5) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 C32 1.519(6) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 C33 1.497(7) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C30A C31A 1.572(19) . ? C30A Mg1 2.142(19) . ? C30A H30C 0.9900 . ? C30A H30D 0.9900 . ? C31A C32A 1.474(16) . ? C31A H31C 0.9900 . ? C31A H31D 0.9900 . ? C32A C33A 1.551(19) . ? C32A H32C 0.9900 . ? C32A H32D 0.9900 . ? C33A H33D 0.9800 . ? C33A H33E 0.9800 . ? C33A H33F 0.9800 . ? C40 C41 1.513(3) . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 N4 1.334(3) . ? C41 C42 1.403(4) . ? C42 C43 1.409(4) . ? C42 H42 0.9500 . ? C43 N5 1.325(3) . ? C43 C44 1.521(3) . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 C46 1.408(4) . ? C45 C50 1.412(4) . ? C45 N4 1.436(3) . ? C46 C47 1.401(4) . ? C46 C51 1.513(4) . ? C47 C48 1.388(5) . ? C47 H47 0.9500 . ? C48 C49 1.371(5) . ? C48 H48 0.9500 . ? C49 C50 1.398(4) . ? C49 H49 0.9500 . ? C50 C54 1.517(4) . ? C51 C53 1.533(5) . ? C51 C52 1.539(5) . ? C51 H51 1.0000 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C54 C56 1.522(4) . ? C54 C55 1.524(4) . ? C54 H54 1.0000 . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? C57 C62 1.401(4) . ? C57 C58 1.409(4) . ? C57 N5 1.444(3) . ? C58 C59 1.400(4) . ? C58 C63 1.520(4) . ? C59 C60 1.366(4) . ? C59 H59 0.9500 . ? C60 C61 1.385(4) . ? C60 H60 0.9500 . ? C61 C62 1.394(4) . ? C61 H61 0.9500 . ? C62 C66 1.519(4) . ? C63 C64 1.522(4) . ? C63 C65 1.528(4) . ? C63 H63 1.0000 . ? C64 H64A 0.9800 . ? C64 H64B 0.9800 . ? C64 H64C 0.9800 . ? C65 H65A 0.9800 . ? C65 H65B 0.9800 . ? C65 H65C 0.9800 . ? C66 C67 1.533(4) . ? C66 C68 1.534(4) . ? C66 H66 1.0000 . ? C67 H67A 0.9800 . ? C67 H67B 0.9800 . ? C67 H67C 0.9800 . ? C68 H68A 0.9800 . ? C68 H68B 0.9800 . ? C68 H68C 0.9800 . ? C69 C70 1.560(4) . ? C69 Mg2 2.118(3) . ? C69 H69A 0.9900 . ? C69 H69B 0.9900 . ? C70 C71 1.507(4) . ? C70 H70A 0.9900 . ? C70 H70B 0.9900 . ? C71 C72 1.506(5) . ? C71 H71A 0.9900 . ? C71 H71B 0.9900 . ? C72 H72A 0.9800 . ? C72 H72B 0.9800 . ? C72 H72C 0.9800 . ? N3 C34 1.3900 . ? N3 C38 1.3900 . ? N3 Mg1 2.216(4) . ? C34 C35 1.3900 . ? C34 H34 0.9500 . ? C35 C36 1.3900 . ? C35 H35 0.9500 . ? C36 C37 1.3900 . ? C36 H36 0.9500 . ? C37 C38 1.3900 . ? C37 H37 0.9500 . ? C38 C39 1.452(8) . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? N3A C34A 1.3900 . ? N3A C38A 1.3900 . ? N3A Mg1 2.218(3) . ? C34A C35A 1.3900 . ? C34A H34A 0.9500 . ? C35A C36A 1.3900 . ? C35A H35A 0.9500 . ? C36A C37A 1.3900 . ? C36A H36A 0.9500 . ? C37A C38A 1.3900 . ? C37A H37A 0.9500 . ? C38A C39A 1.479(8) . ? C39A H39D 0.9800 . ? C39A H39E 0.9800 . ? C39A H39F 0.9800 . ? N6 C73 1.3900 . ? N6 C77 1.3900 . ? N6 Mg2 2.2058(18) . ? C73 C74 1.3900 . ? C73 H73 0.9500 . ? C74 C75 1.3900 . ? C74 H74 0.9500 . ? C75 C76 1.3900 . ? C75 H75 0.9500 . ? C76 C77 1.3900 . ? C76 H76 0.9500 . ? C77 C78 1.491(5) . ? C78 H78A 0.9800 . ? C78 H78B 0.9800 . ? C78 H78C 0.9800 . ? N6A C73A 1.3900 . ? N6A C77A 1.3900 . ? N6A Mg2 2.179(5) . ? C73A C74A 1.3900 . ? C73A H73A 0.9500 . ? C74A C75A 1.3900 . ? C74A H74A 0.9500 . ? C75A C76A 1.3900 . ? C75A H75A 0.9500 . ? C76A C77A 1.3900 . ? C76A H76A 0.9500 . ? C77A C78A 1.485(12) . ? C78A H78D 0.9800 . ? C78A H78E 0.9800 . ? C78A H78F 0.9800 . ? N1 Mg1 2.074(2) . ? N2 Mg1 2.075(2) . ? N4 Mg2 2.073(2) . ? N5 Mg2 2.081(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N1 C2 C3 123.5(2) . . ? N1 C2 C1 121.3(2) . . ? C3 C2 C1 115.2(2) . . ? C4 C3 C2 129.6(2) . . ? C4 C3 H3 115.2 . . ? C2 C3 H3 115.2 . . ? N2 C4 C3 124.2(2) . . ? N2 C4 C5 120.0(2) . . ? C3 C4 C5 115.8(2) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C7 C6 C11 121.1(3) . . ? C7 C6 N1 120.3(2) . . ? C11 C6 N1 118.4(3) . . ? C8 C7 C6 117.7(3) . . ? C8 C7 C12 119.7(3) . . ? C6 C7 C12 122.6(3) . . ? C9 C8 C7 121.6(3) . . ? C9 C8 H8 119.2 . . ? C7 C8 H8 119.2 . . ? C10 C9 C8 119.8(3) . . ? C10 C9 H9 120.1 . . ? C8 C9 H9 120.1 . . ? C9 C10 C11 121.7(3) . . ? C9 C10 H10 119.1 . . ? C11 C10 H10 119.1 . . ? C10 C11 C6 118.0(3) . . ? C10 C11 C15 121.5(3) . . ? C6 C11 C15 120.5(3) . . ? C7 C12 C14 110.9(3) . . ? C7 C12 C13 112.2(3) . . ? C14 C12 C13 110.6(3) . . ? C7 C12 H12 107.7 . . ? C14 C12 H12 107.7 . . ? C13 C12 H12 107.7 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C11 C15 C16 112.3(2) . . ? C11 C15 C17 112.7(3) . . ? C16 C15 C17 109.8(3) . . ? C11 C15 H15 107.3 . . ? C16 C15 H15 107.3 . . ? C17 C15 H15 107.3 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C19 C18 C23 120.4(3) . . ? C19 C18 N2 119.5(2) . . ? C23 C18 N2 120.1(2) . . ? C20 C19 C18 118.4(3) . . ? C20 C19 C24 119.4(3) . . ? C18 C19 C24 122.2(3) . . ? C21 C20 C19 121.8(3) . . ? C21 C20 H20 119.1 . . ? C19 C20 H20 119.1 . . ? C20 C21 C22 119.7(3) . . ? C20 C21 H21 120.2 . . ? C22 C21 H21 120.2 . . ? C21 C22 C23 121.3(3) . . ? C21 C22 H22 119.3 . . ? C23 C22 H22 119.3 . . ? C22 C23 C18 118.4(3) . . ? C22 C23 C27 119.2(3) . . ? C18 C23 C27 122.4(3) . . ? C19 C24 C26 112.7(3) . . ? C19 C24 C25 111.1(3) . . ? C26 C24 C25 110.0(3) . . ? C19 C24 H24 107.6 . . ? C26 C24 H24 107.6 . . ? C25 C24 H24 107.6 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C23 C27 C28 111.5(3) . . ? C23 C27 C29 113.0(3) . . ? C28 C27 C29 110.6(3) . . ? C23 C27 H27 107.1 . . ? C28 C27 H27 107.1 . . ? C29 C27 H27 107.1 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C31 C30 Mg1 116.1(3) . . ? C31 C30 H30A 108.3 . . ? Mg1 C30 H30A 108.3 . . ? C31 C30 H30B 108.3 . . ? Mg1 C30 H30B 108.3 . . ? H30A C30 H30B 107.4 . . ? C32 C31 C30 116.7(4) . . ? C32 C31 H31A 108.1 . . ? C30 C31 H31A 108.1 . . ? C32 C31 H31B 108.1 . . ? C30 C31 H31B 108.1 . . ? H31A C31 H31B 107.3 . . ? C33 C32 C31 114.9(4) . . ? C33 C32 H32A 108.5 . . ? C31 C32 H32A 108.5 . . ? C33 C32 H32B 108.5 . . ? C31 C32 H32B 108.5 . . ? H32A C32 H32B 107.5 . . ? C31A C30A Mg1 112.5(10) . . ? C31A C30A H30C 109.1 . . ? Mg1 C30A H30C 109.1 . . ? C31A C30A H30D 109.1 . . ? Mg1 C30A H30D 109.1 . . ? H30C C30A H30D 107.8 . . ? C32A C31A C30A 117.0(12) . . ? C32A C31A H31C 108.1 . . ? C30A C31A H31C 108.1 . . ? C32A C31A H31D 108.1 . . ? C30A C31A H31D 108.1 . . ? H31C C31A H31D 107.3 . . ? C31A C32A C33A 111.0(11) . . ? C31A C32A H32C 109.4 . . ? C33A C32A H32C 109.4 . . ? C31A C32A H32D 109.4 . . ? C33A C32A H32D 109.4 . . ? H32C C32A H32D 108.0 . . ? C32A C33A H33D 109.5 . . ? C32A C33A H33E 109.5 . . ? H33D C33A H33E 109.5 . . ? C32A C33A H33F 109.5 . . ? H33D C33A H33F 109.5 . . ? H33E C33A H33F 109.5 . . ? C41 C40 H40A 109.5 . . ? C41 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C41 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? N4 C41 C42 124.4(2) . . ? N4 C41 C40 119.3(2) . . ? C42 C41 C40 116.3(2) . . ? C41 C42 C43 129.7(2) . . ? C41 C42 H42 115.1 . . ? C43 C42 H42 115.1 . . ? N5 C43 C42 123.4(2) . . ? N5 C43 C44 120.7(2) . . ? C42 C43 C44 115.8(2) . . ? C43 C44 H44A 109.5 . . ? C43 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C43 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C46 C45 C50 120.6(2) . . ? C46 C45 N4 120.7(2) . . ? C50 C45 N4 118.7(2) . . ? C47 C46 C45 118.3(3) . . ? C47 C46 C51 119.4(3) . . ? C45 C46 C51 122.2(2) . . ? C48 C47 C46 121.1(3) . . ? C48 C47 H47 119.4 . . ? C46 C47 H47 119.4 . . ? C49 C48 C47 119.9(3) . . ? C49 C48 H48 120.0 . . ? C47 C48 H48 120.0 . . ? C48 C49 C50 121.4(3) . . ? C48 C49 H49 119.3 . . ? C50 C49 H49 119.3 . . ? C49 C50 C45 118.5(3) . . ? C49 C50 C54 119.9(3) . . ? C45 C50 C54 121.5(2) . . ? C46 C51 C53 110.7(3) . . ? C46 C51 C52 113.1(3) . . ? C53 C51 C52 110.0(3) . . ? C46 C51 H51 107.6 . . ? C53 C51 H51 107.6 . . ? C52 C51 H51 107.6 . . ? C51 C52 H52A 109.5 . . ? C51 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C51 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C51 C53 H53A 109.5 . . ? C51 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C51 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C50 C54 C56 112.6(3) . . ? C50 C54 C55 111.3(3) . . ? C56 C54 C55 110.7(3) . . ? C50 C54 H54 107.3 . . ? C56 C54 H54 107.3 . . ? C55 C54 H54 107.3 . . ? C54 C55 H55A 109.5 . . ? C54 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? C54 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? C54 C56 H56A 109.5 . . ? C54 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C54 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? C62 C57 C58 121.1(2) . . ? C62 C57 N5 120.7(2) . . ? C58 C57 N5 117.9(2) . . ? C59 C58 C57 117.6(3) . . ? C59 C58 C63 121.0(3) . . ? C57 C58 C63 121.4(2) . . ? C60 C59 C58 121.8(3) . . ? C60 C59 H59 119.1 . . ? C58 C59 H59 119.1 . . ? C59 C60 C61 120.0(3) . . ? C59 C60 H60 120.0 . . ? C61 C60 H60 120.0 . . ? C60 C61 C62 120.8(3) . . ? C60 C61 H61 119.6 . . ? C62 C61 H61 119.6 . . ? C61 C62 C57 118.6(3) . . ? C61 C62 C66 119.0(3) . . ? C57 C62 C66 122.3(2) . . ? C58 C63 C64 112.6(2) . . ? C58 C63 C65 113.7(3) . . ? C64 C63 C65 109.3(2) . . ? C58 C63 H63 107.0 . . ? C64 C63 H63 107.0 . . ? C65 C63 H63 107.0 . . ? C63 C64 H64A 109.5 . . ? C63 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? C63 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? C63 C65 H65A 109.5 . . ? C63 C65 H65B 109.5 . . ? H65A C65 H65B 109.5 . . ? C63 C65 H65C 109.5 . . ? H65A C65 H65C 109.5 . . ? H65B C65 H65C 109.5 . . ? C62 C66 C67 111.3(2) . . ? C62 C66 C68 112.1(2) . . ? C67 C66 C68 110.0(2) . . ? C62 C66 H66 107.7 . . ? C67 C66 H66 107.7 . . ? C68 C66 H66 107.7 . . ? C66 C67 H67A 109.5 . . ? C66 C67 H67B 109.5 . . ? H67A C67 H67B 109.5 . . ? C66 C67 H67C 109.5 . . ? H67A C67 H67C 109.5 . . ? H67B C67 H67C 109.5 . . ? C66 C68 H68A 109.5 . . ? C66 C68 H68B 109.5 . . ? H68A C68 H68B 109.5 . . ? C66 C68 H68C 109.5 . . ? H68A C68 H68C 109.5 . . ? H68B C68 H68C 109.5 . . ? C70 C69 Mg2 116.2(2) . . ? C70 C69 H69A 108.2 . . ? Mg2 C69 H69A 108.2 . . ? C70 C69 H69B 108.2 . . ? Mg2 C69 H69B 108.2 . . ? H69A C69 H69B 107.4 . . ? C71 C70 C69 116.1(3) . . ? C71 C70 H70A 108.3 . . ? C69 C70 H70A 108.3 . . ? C71 C70 H70B 108.3 . . ? C69 C70 H70B 108.3 . . ? H70A C70 H70B 107.4 . . ? C72 C71 C70 112.8(3) . . ? C72 C71 H71A 109.0 . . ? C70 C71 H71A 109.0 . . ? C72 C71 H71B 109.0 . . ? C70 C71 H71B 109.0 . . ? H71A C71 H71B 107.8 . . ? C71 C72 H72A 109.5 . . ? C71 C72 H72B 109.5 . . ? H72A C72 H72B 109.5 . . ? C71 C72 H72C 109.5 . . ? H72A C72 H72C 109.5 . . ? H72B C72 H72C 109.5 . . ? C34 N3 C38 120.0 . . ? C34 N3 Mg1 110.5(3) . . ? C38 N3 Mg1 129.5(3) . . ? N3 C34 C35 120.0 . . ? N3 C34 H34 120.0 . . ? C35 C34 H34 120.0 . . ? C36 C35 C34 120.0 . . ? C36 C35 H35 120.0 . . ? C34 C35 H35 120.0 . . ? C35 C36 C37 120.0 . . ? C35 C36 H36 120.0 . . ? C37 C36 H36 120.0 . . ? C38 C37 C36 120.0 . . ? C38 C37 H37 120.0 . . ? C36 C37 H37 120.0 . . ? C37 C38 N3 120.0 . . ? C37 C38 C39 119.5(5) . . ? N3 C38 C39 120.5(5) . . ? C34A N3A C38A 120.0 . . ? C34A N3A Mg1 110.2(2) . . ? C38A N3A Mg1 129.4(2) . . ? N3A C34A C35A 120.0 . . ? N3A C34A H34A 120.0 . . ? C35A C34A H34A 120.0 . . ? C34A C35A C36A 120.0 . . ? C34A C35A H35A 120.0 . . ? C36A C35A H35A 120.0 . . ? C37A C36A C35A 120.0 . . ? C37A C36A H36A 120.0 . . ? C35A C36A H36A 120.0 . . ? C38A C37A C36A 120.0 . . ? C38A C37A H37A 120.0 . . ? C36A C37A H37A 120.0 . . ? C37A C38A N3A 120.0 . . ? C37A C38A C39A 119.7(4) . . ? N3A C38A C39A 120.3(4) . . ? C38A C39A H39D 109.5 . . ? C38A C39A H39E 109.5 . . ? H39D C39A H39E 109.5 . . ? C38A C39A H39F 109.5 . . ? H39D C39A H39F 109.5 . . ? H39E C39A H39F 109.5 . . ? C73 N6 C77 120.0 . . ? C73 N6 Mg2 111.40(13) . . ? C77 N6 Mg2 128.37(13) . . ? C74 C73 N6 120.0 . . ? C74 C73 H73 120.0 . . ? N6 C73 H73 120.0 . . ? C73 C74 C75 120.0 . . ? C73 C74 H74 120.0 . . ? C75 C74 H74 120.0 . . ? C76 C75 C74 120.0 . . ? C76 C75 H75 120.0 . . ? C74 C75 H75 120.0 . . ? C75 C76 C77 120.0 . . ? C75 C76 H76 120.0 . . ? C77 C76 H76 120.0 . . ? C76 C77 N6 120.0 . . ? C76 C77 C78 121.7(2) . . ? N6 C77 C78 118.2(2) . . ? C73A N6A C77A 120.0 . . ? C73A N6A Mg2 108.7(3) . . ? C77A N6A Mg2 131.1(3) . . ? C74A C73A N6A 120.0 . . ? C74A C73A H73A 120.0 . . ? N6A C73A H73A 120.0 . . ? C75A C74A C73A 120.0 . . ? C75A C74A H74A 120.0 . . ? C73A C74A H74A 120.0 . . ? C74A C75A C76A 120.0 . . ? C74A C75A H75A 120.0 . . ? C76A C75A H75A 120.0 . . ? C75A C76A C77A 120.0 . . ? C75A C76A H76A 120.0 . . ? C77A C76A H76A 120.0 . . ? C76A C77A N6A 120.0 . . ? C76A C77A C78A 119.1(6) . . ? N6A C77A C78A 120.9(6) . . ? C77A C78A H78D 109.5 . . ? C77A C78A H78E 109.5 . . ? H78D C78A H78E 109.5 . . ? C77A C78A H78F 109.5 . . ? H78D C78A H78F 109.5 . . ? H78E C78A H78F 109.5 . . ? C2 N1 C6 119.6(2) . . ? C2 N1 Mg1 123.21(18) . . ? C6 N1 Mg1 117.17(16) . . ? C4 N2 C18 116.7(2) . . ? C4 N2 Mg1 121.70(18) . . ? C18 N2 Mg1 121.56(16) . . ? C41 N4 C45 117.6(2) . . ? C41 N4 Mg2 121.55(17) . . ? C45 N4 Mg2 120.87(15) . . ? C43 N5 C57 119.8(2) . . ? C43 N5 Mg2 122.68(17) . . ? C57 N5 Mg2 117.44(15) . . ? N1 Mg1 N2 91.32(9) . . ? N1 Mg1 C30A 123.6(5) . . ? N2 Mg1 C30A 114.6(5) . . ? N1 Mg1 C30 114.40(17) . . ? N2 Mg1 C30 128.91(19) . . ? C30A Mg1 C30 14.9(5) . . ? N1 Mg1 N3 109.94(17) . . ? N2 Mg1 N3 107.35(17) . . ? C30A Mg1 N3 108.3(6) . . ? C30 Mg1 N3 104.0(2) . . ? N1 Mg1 N3A 102.62(15) . . ? N2 Mg1 N3A 102.41(15) . . ? C30A Mg1 N3A 117.6(6) . . ? C30 Mg1 N3A 112.80(19) . . ? N3 Mg1 N3A 9.30(18) . . ? N4 Mg2 N5 91.45(8) . . ? N4 Mg2 C69 121.70(11) . . ? N5 Mg2 C69 118.35(11) . . ? N4 Mg2 N6A 107.19(19) . . ? N5 Mg2 N6A 110.42(19) . . ? C69 Mg2 N6A 106.75(18) . . ? N4 Mg2 N6 101.46(9) . . ? N5 Mg2 N6 101.89(10) . . ? C69 Mg2 N6 117.34(11) . . ? N6A Mg2 N6 10.81(17) . . ? 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 N1 C2 C3 C4 12.3(5) . . . . ? C1 C2 C3 C4 -167.1(3) . . . . ? C2 C3 C4 N2 -11.8(5) . . . . ? C2 C3 C4 C5 166.5(3) . . . . ? C11 C6 C7 C8 -1.7(4) . . . . ? N1 C6 C7 C8 -176.3(2) . . . . ? C11 C6 C7 C12 177.3(3) . . . . ? N1 C6 C7 C12 2.7(4) . . . . ? C6 C7 C8 C9 0.5(5) . . . . ? C12 C7 C8 C9 -178.6(3) . . . . ? C7 C8 C9 C10 0.5(5) . . . . ? C8 C9 C10 C11 -0.1(5) . . . . ? C9 C10 C11 C6 -1.1(4) . . . . ? C9 C10 C11 C15 177.8(3) . . . . ? C7 C6 C11 C10 2.0(4) . . . . ? N1 C6 C11 C10 176.8(2) . . . . ? C7 C6 C11 C15 -176.9(2) . . . . ? N1 C6 C11 C15 -2.1(4) . . . . ? C8 C7 C12 C14 65.0(4) . . . . ? C6 C7 C12 C14 -114.0(3) . . . . ? C8 C7 C12 C13 -59.2(4) . . . . ? C6 C7 C12 C13 121.8(3) . . . . ? C10 C11 C15 C16 97.1(3) . . . . ? C6 C11 C15 C16 -84.1(3) . . . . ? C10 C11 C15 C17 -27.5(4) . . . . ? C6 C11 C15 C17 151.3(3) . . . . ? C23 C18 C19 C20 -1.3(4) . . . . ? N2 C18 C19 C20 -178.7(2) . . . . ? C23 C18 C19 C24 178.6(3) . . . . ? N2 C18 C19 C24 1.2(4) . . . . ? C18 C19 C20 C21 0.7(5) . . . . ? C24 C19 C20 C21 -179.2(3) . . . . ? C19 C20 C21 C22 0.3(6) . . . . ? C20 C21 C22 C23 -0.7(6) . . . . ? C21 C22 C23 C18 0.2(5) . . . . ? C21 C22 C23 C27 -179.5(3) . . . . ? C19 C18 C23 C22 0.8(4) . . . . ? N2 C18 C23 C22 178.3(3) . . . . ? C19 C18 C23 C27 -179.5(3) . . . . ? N2 C18 C23 C27 -2.1(4) . . . . ? C20 C19 C24 C26 -59.0(4) . . . . ? C18 C19 C24 C26 121.1(3) . . . . ? C20 C19 C24 C25 64.9(4) . . . . ? C18 C19 C24 C25 -115.0(3) . . . . ? C22 C23 C27 C28 -62.4(4) . . . . ? C18 C23 C27 C28 117.9(3) . . . . ? C22 C23 C27 C29 62.9(4) . . . . ? C18 C23 C27 C29 -116.8(3) . . . . ? Mg1 C30 C31 C32 -170.3(3) . . . . ? C30 C31 C32 C33 -67.4(6) . . . . ? Mg1 C30A C31A C32A 170.2(10) . . . . ? C30A C31A C32A C33A -176.0(14) . . . . ? N4 C41 C42 C43 11.1(4) . . . . ? C40 C41 C42 C43 -168.3(3) . . . . ? C41 C42 C43 N5 -13.3(4) . . . . ? C41 C42 C43 C44 166.3(3) . . . . ? C50 C45 C46 C47 -2.5(4) . . . . ? N4 C45 C46 C47 179.8(3) . . . . ? C50 C45 C46 C51 176.8(3) . . . . ? N4 C45 C46 C51 -0.9(4) . . . . ? C45 C46 C47 C48 0.0(5) . . . . ? C51 C46 C47 C48 -179.3(3) . . . . ? C46 C47 C48 C49 1.9(5) . . . . ? C47 C48 C49 C50 -1.4(5) . . . . ? C48 C49 C50 C45 -1.0(4) . . . . ? C48 C49 C50 C54 178.2(3) . . . . ? C46 C45 C50 C49 3.0(4) . . . . ? N4 C45 C50 C49 -179.3(2) . . . . ? C46 C45 C50 C54 -176.2(3) . . . . ? N4 C45 C50 C54 1.5(4) . . . . ? C47 C46 C51 C53 65.2(4) . . . . ? C45 C46 C51 C53 -114.1(3) . . . . ? C47 C46 C51 C52 -58.8(4) . . . . ? C45 C46 C51 C52 121.9(3) . . . . ? C49 C50 C54 C56 73.3(4) . . . . ? C45 C50 C54 C56 -107.5(3) . . . . ? C49 C50 C54 C55 -51.7(4) . . . . ? C45 C50 C54 C55 127.5(3) . . . . ? C62 C57 C58 C59 -1.2(4) . . . . ? N5 C57 C58 C59 -175.8(2) . . . . ? C62 C57 C58 C63 177.1(2) . . . . ? N5 C57 C58 C63 2.5(4) . . . . ? C57 C58 C59 C60 1.7(4) . . . . ? C63 C58 C59 C60 -176.6(3) . . . . ? C58 C59 C60 C61 -0.5(5) . . . . ? C59 C60 C61 C62 -1.2(4) . . . . ? C60 C61 C62 C57 1.7(4) . . . . ? C60 C61 C62 C66 179.9(3) . . . . ? C58 C57 C62 C61 -0.5(4) . . . . ? N5 C57 C62 C61 174.0(2) . . . . ? C58 C57 C62 C66 -178.7(2) . . . . ? N5 C57 C62 C66 -4.2(4) . . . . ? C59 C58 C63 C64 -98.2(3) . . . . ? C57 C58 C63 C64 83.5(3) . . . . ? C59 C58 C63 C65 26.7(4) . . . . ? C57 C58 C63 C65 -151.5(3) . . . . ? C61 C62 C66 C67 -66.3(3) . . . . ? C57 C62 C66 C67 111.9(3) . . . . ? C61 C62 C66 C68 57.4(3) . . . . ? C57 C62 C66 C68 -124.4(3) . . . . ? Mg2 C69 C70 C71 -166.3(2) . . . . ? C69 C70 C71 C72 167.3(3) . . . . ? C38 N3 C34 C35 0.0 . . . . ? Mg1 N3 C34 C35 178.5(5) . . . . ? N3 C34 C35 C36 0.0 . . . . ? C34 C35 C36 C37 0.0 . . . . ? C35 C36 C37 C38 0.0 . . . . ? C36 C37 C38 N3 0.0 . . . . ? C36 C37 C38 C39 178.0(6) . . . . ? C34 N3 C38 C37 0.0 . . . . ? Mg1 N3 C38 C37 -178.2(6) . . . . ? C34 N3 C38 C39 -178.0(6) . . . . ? Mg1 N3 C38 C39 3.7(8) . . . . ? C38A N3A C34A C35A 0.0 . . . . ? Mg1 N3A C34A C35A -173.3(4) . . . . ? N3A C34A C35A C36A 0.0 . . . . ? C34A C35A C36A C37A 0.0 . . . . ? C35A C36A C37A C38A 0.0 . . . . ? C36A C37A C38A N3A 0.0 . . . . ? C36A C37A C38A C39A -177.7(5) . . . . ? C34A N3A C38A C37A 0.0 . . . . ? Mg1 N3A C38A C37A 171.9(5) . . . . ? C34A N3A C38A C39A 177.7(6) . . . . ? Mg1 N3A C38A C39A -10.4(7) . . . . ? C77 N6 C73 C74 0.0 . . . . ? Mg2 N6 C73 C74 174.92(18) . . . . ? N6 C73 C74 C75 0.0 . . . . ? C73 C74 C75 C76 0.0 . . . . ? C74 C75 C76 C77 0.0 . . . . ? C75 C76 C77 N6 0.0 . . . . ? C75 C76 C77 C78 177.2(3) . . . . ? C73 N6 C77 C76 0.0 . . . . ? Mg2 N6 C77 C76 -174.0(2) . . . . ? C73 N6 C77 C78 -177.3(3) . . . . ? Mg2 N6 C77 C78 8.8(3) . . . . ? C77A N6A C73A C74A 0.0 . . . . ? Mg2 N6A C73A C74A -176.5(5) . . . . ? N6A C73A C74A C75A 0.0 . . . . ? C73A C74A C75A C76A 0.0 . . . . ? C74A C75A C76A C77A 0.0 . . . . ? C75A C76A C77A N6A 0.0 . . . . ? C75A C76A C77A C78A -179.6(8) . . . . ? C73A N6A C77A C76A 0.0 . . . . ? Mg2 N6A C77A C76A 175.6(6) . . . . ? C73A N6A C77A C78A 179.6(8) . . . . ? Mg2 N6A C77A C78A -4.8(9) . . . . ? C3 C2 N1 C6 -171.0(2) . . . . ? C1 C2 N1 C6 8.3(4) . . . . ? C3 C2 N1 Mg1 10.6(4) . . . . ? C1 C2 N1 Mg1 -170.04(19) . . . . ? C7 C6 N1 C2 -87.5(3) . . . . ? C11 C6 N1 C2 97.7(3) . . . . ? C7 C6 N1 Mg1 90.9(3) . . . . ? C11 C6 N1 Mg1 -83.8(3) . . . . ? C3 C4 N2 C18 167.7(2) . . . . ? C5 C4 N2 C18 -10.5(4) . . . . ? C3 C4 N2 Mg1 -11.4(4) . . . . ? C5 C4 N2 Mg1 170.4(2) . . . . ? C19 C18 N2 C4 -83.0(3) . . . . ? C23 C18 N2 C4 99.5(3) . . . . ? C19 C18 N2 Mg1 96.1(3) . . . . ? C23 C18 N2 Mg1 -81.4(3) . . . . ? C42 C41 N4 C45 -165.2(2) . . . . ? C40 C41 N4 C45 14.1(3) . . . . ? C42 C41 N4 Mg2 13.2(3) . . . . ? C40 C41 N4 Mg2 -167.42(18) . . . . ? C46 C45 N4 C41 -97.1(3) . . . . ? C50 C45 N4 C41 85.1(3) . . . . ? C46 C45 N4 Mg2 84.4(3) . . . . ? C50 C45 N4 Mg2 -93.3(2) . . . . ? C42 C43 N5 C57 173.4(2) . . . . ? C44 C43 N5 C57 -6.2(3) . . . . ? C42 C43 N5 Mg2 -9.3(3) . . . . ? C44 C43 N5 Mg2 171.05(18) . . . . ? C62 C57 N5 C43 85.8(3) . . . . ? C58 C57 N5 C43 -99.5(3) . . . . ? C62 C57 N5 Mg2 -91.6(2) . . . . ? C58 C57 N5 Mg2 83.1(2) . . . . ? C2 N1 Mg1 N2 -23.1(2) . . . . ? C6 N1 Mg1 N2 158.43(19) . . . . ? C2 N1 Mg1 C30A -144.1(6) . . . . ? C6 N1 Mg1 C30A 37.4(6) . . . . ? C2 N1 Mg1 C30 -157.6(3) . . . . ? C6 N1 Mg1 C30 24.0(3) . . . . ? C2 N1 Mg1 N3 85.9(3) . . . . ? C6 N1 Mg1 N3 -92.6(2) . . . . ? C2 N1 Mg1 N3A 79.9(2) . . . . ? C6 N1 Mg1 N3A -98.5(2) . . . . ? C4 N2 Mg1 N1 23.2(2) . . . . ? C18 N2 Mg1 N1 -155.89(19) . . . . ? C4 N2 Mg1 C30A 151.5(6) . . . . ? C18 N2 Mg1 C30A -27.6(6) . . . . ? C4 N2 Mg1 C30 146.5(2) . . . . ? C18 N2 Mg1 C30 -32.5(3) . . . . ? C4 N2 Mg1 N3 -88.2(2) . . . . ? C18 N2 Mg1 N3 92.7(2) . . . . ? C4 N2 Mg1 N3A -80.0(2) . . . . ? C18 N2 Mg1 N3A 100.9(2) . . . . ? C31A C30A Mg1 N1 -44.2(15) . . . . ? C31A C30A Mg1 N2 -153.8(10) . . . . ? C31A C30A Mg1 C30 11.1(16) . . . . ? C31A C30A Mg1 N3 86.4(12) . . . . ? C31A C30A Mg1 N3A 85.8(13) . . . . ? C31 C30 Mg1 N1 -53.6(4) . . . . ? C31 C30 Mg1 N2 -167.1(3) . . . . ? C31 C30 Mg1 C30A 175(3) . . . . ? C31 C30 Mg1 N3 66.4(4) . . . . ? C31 C30 Mg1 N3A 63.2(4) . . . . ? C34 N3 Mg1 N1 131.0(2) . . . . ? C38 N3 Mg1 N1 -50.6(5) . . . . ? C34 N3 Mg1 N2 -131.0(2) . . . . ? C38 N3 Mg1 N2 47.4(5) . . . . ? C34 N3 Mg1 C30A -6.7(5) . . . . ? C38 N3 Mg1 C30A 171.6(6) . . . . ? C34 N3 Mg1 C30 8.1(3) . . . . ? C38 N3 Mg1 C30 -173.5(4) . . . . ? C34 N3 Mg1 N3A 170.0(19) . . . . ? C38 N3 Mg1 N3A -11.6(15) . . . . ? C34A N3A Mg1 N1 -50.8(2) . . . . ? C38A N3A Mg1 N1 136.7(4) . . . . ? C34A N3A Mg1 N2 43.4(2) . . . . ? C38A N3A Mg1 N2 -129.1(4) . . . . ? C34A N3A Mg1 C30A 170.0(5) . . . . ? C38A N3A Mg1 C30A -2.5(7) . . . . ? C34A N3A Mg1 C30 -174.4(2) . . . . ? C38A N3A Mg1 C30 13.1(5) . . . . ? C34A N3A Mg1 N3 166.5(19) . . . . ? C38A N3A Mg1 N3 -6.0(15) . . . . ? C41 N4 Mg2 N5 -24.48(19) . . . . ? C45 N4 Mg2 N5 153.91(19) . . . . ? C41 N4 Mg2 C69 -149.51(19) . . . . ? C45 N4 Mg2 C69 28.9(2) . . . . ? C41 N4 Mg2 N6A 87.4(3) . . . . ? C45 N4 Mg2 N6A -94.2(3) . . . . ? C41 N4 Mg2 N6 78.0(2) . . . . ? C45 N4 Mg2 N6 -103.65(19) . . . . ? C43 N5 Mg2 N4 22.8(2) . . . . ? C57 N5 Mg2 N4 -159.83(17) . . . . ? C43 N5 Mg2 C69 150.50(19) . . . . ? C57 N5 Mg2 C69 -32.2(2) . . . . ? C43 N5 Mg2 N6A -86.1(3) . . . . ? C57 N5 Mg2 N6A 91.2(3) . . . . ? C43 N5 Mg2 N6 -79.2(2) . . . . ? C57 N5 Mg2 N6 98.14(18) . . . . ? C70 C69 Mg2 N4 156.64(19) . . . . ? C70 C69 Mg2 N5 45.1(3) . . . . ? C70 C69 Mg2 N6A -80.1(3) . . . . ? C70 C69 Mg2 N6 -77.8(2) . . . . ? C73A N6A Mg2 N4 130.0(3) . . . . ? C77A N6A Mg2 N4 -46.0(5) . . . . ? C73A N6A Mg2 N5 -131.8(3) . . . . ? C77A N6A Mg2 N5 52.3(5) . . . . ? C73A N6A Mg2 C69 -1.9(3) . . . . ? C77A N6A Mg2 C69 -177.8(4) . . . . ? C73A N6A Mg2 N6 -170.7(14) . . . . ? C77A N6A Mg2 N6 13.3(10) . . . . ? C73 N6 Mg2 N4 -46.35(13) . . . . ? C77 N6 Mg2 N4 128.04(16) . . . . ? C73 N6 Mg2 N5 47.61(13) . . . . ? C77 N6 Mg2 N5 -138.00(16) . . . . ? C73 N6 Mg2 C69 178.54(14) . . . . ? C77 N6 Mg2 C69 -7.1(2) . . . . ? C73 N6 Mg2 N6A -169.4(13) . . . . ? C77 N6 Mg2 N6A 4.9(12) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.354 _refine_diff_density_min -0.347 _refine_diff_density_rms 0.043 #===end data_6-h10msh25 _database_code_depnum_ccdc_archive 'CCDC 831737' #TrackingRef '- bigcif.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C41 H56 Mg N4' _chemical_formula_weight 629.21 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mg Mg 0.0486 0.0363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 35.9897(12) _cell_length_b 15.3126(3) _cell_length_c 14.6944(5) _cell_angle_alpha 90.00 _cell_angle_beta 105.416(1) _cell_angle_gamma 90.00 _cell_volume 7806.7(4) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 44826 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 27.485 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.071 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2736 _exptl_absorpt_coefficient_mu 0.077 # Absorption correction _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.936 _exptl_absorpt_correction_T_max 0.986 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_measurement_device_type '95mm CCD camera on \k-goniostat' _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 55881 _diffrn_reflns_av_R_equivalents 0.0882 _diffrn_reflns_av_sigmaI/netI 0.0529 _diffrn_reflns_limit_h_min -42 _diffrn_reflns_limit_h_max 42 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 4.04 _diffrn_reflns_theta_max 25.02 _reflns_number_total 6839 _reflns_number_gt 4207 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Bruker AXS BV 1997-2004)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo & Scalepack (Otwinowski, Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick 1990)' _computing_structure_refinement 'SHELXL-97/2 (Sheldrick 1997)' _computing_molecular_graphics 'ORTEX (P.McArdle 1995)' _computing_publication_material 'SHELXL-97/2 (Sheldrick 1997)' _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. Data truncated to a Bragg angle of 25o due to decline of diffraction intensity beyond this point. This is most likely to be related to the smallest crystal dimension. The electron density in the reduced picoline moiety based on N3 is quite smeared, and suggests that this functionality may be disordered. However, ardent efforts to model same over 2 sites did not improve convergence. The hydrogens attached to C30 and C34 have been omitted from the refinement -- because of the inability to determine precisely which of these best represents a CH2 moiety. ; _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^)+(0.0730P)^2^+12.1547P] 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 6839 _refine_ls_number_parameters 427 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1199 _refine_ls_R_factor_gt 0.0663 _refine_ls_wR_factor_ref 0.1913 _refine_ls_wR_factor_gt 0.1561 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.043 _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 0.62931(3) 0.22013(6) 0.50262(7) 0.0447(3) Uani 1 1 d . . . N1 N 0.60345(7) 0.29042(14) 0.38421(17) 0.0425(6) Uani 1 1 d . . . N2 N 0.58050(7) 0.15045(14) 0.49896(16) 0.0400(6) Uani 1 1 d . . . N4 N 0.66910(7) 0.13179(16) 0.46604(18) 0.0501(6) Uani 1 1 d . . . C1 C 0.55796(10) 0.3034(2) 0.2254(2) 0.0582(9) Uani 1 1 d . . . H1A H 0.5554 0.3663 0.2350 0.087 Uiso 1 1 calc R . . H1B H 0.5327 0.2791 0.1932 0.087 Uiso 1 1 calc R . . H1 H 0.5759 0.2937 0.1866 0.087 Uiso 1 1 calc R . . C2 C 0.57318(8) 0.25872(18) 0.3205(2) 0.0420(7) Uani 1 1 d . . . C3 C 0.55240(8) 0.18516(18) 0.3354(2) 0.0422(7) Uani 1 1 d . . . H3 H 0.5352 0.1619 0.2801 0.051 Uiso 1 1 calc R . . C4 C 0.55301(8) 0.14028(17) 0.4193(2) 0.0390(7) Uani 1 1 d . . . C5 C 0.51922(9) 0.0800(2) 0.4158(2) 0.0492(8) Uani 1 1 d . . . H5A H 0.5288 0.0212 0.4355 0.074 Uiso 1 1 calc R . . H5B H 0.5025 0.0779 0.3512 0.074 Uiso 1 1 calc R . . H5C H 0.5045 0.1020 0.4584 0.074 Uiso 1 1 calc R . . C6 C 0.61866(9) 0.37464(19) 0.3681(2) 0.0504(8) Uani 1 1 d . . . C7 C 0.64636(9) 0.3814(2) 0.3170(3) 0.0570(9) Uani 1 1 d . . . C8 C 0.66103(12) 0.4637(2) 0.3068(3) 0.0841(13) Uani 1 1 d . . . H8 H 0.6800 0.4694 0.2729 0.101 Uiso 1 1 calc R . . C9 C 0.64879(15) 0.5369(3) 0.3444(4) 0.1027(16) Uani 1 1 d . . . H9 H 0.6590 0.5926 0.3360 0.123 Uiso 1 1 calc R . . C10 C 0.62163(14) 0.5290(2) 0.3942(4) 0.0923(14) Uani 1 1 d . . . H10 H 0.6134 0.5799 0.4204 0.111 Uiso 1 1 calc R . . C11 C 0.60578(11) 0.4488(2) 0.4073(3) 0.0649(10) Uani 1 1 d . . . C12 C 0.66107(9) 0.3028(2) 0.2747(3) 0.0573(9) Uani 1 1 d . . . H12 H 0.6452 0.2514 0.2831 0.069 Uiso 1 1 calc R . . C13 C 0.70294(11) 0.2833(3) 0.3275(3) 0.0794(12) Uani 1 1 d . . . H13A H 0.7195 0.3307 0.3166 0.119 Uiso 1 1 calc R . . H13B H 0.7109 0.2282 0.3044 0.119 Uiso 1 1 calc R . . H13C H 0.7052 0.2785 0.3952 0.119 Uiso 1 1 calc R . . C14 C 0.65736(12) 0.3125(3) 0.1695(3) 0.0785(11) Uani 1 1 d . . . H14A H 0.6303 0.3228 0.1359 0.118 Uiso 1 1 calc R . . H14B H 0.6663 0.2589 0.1457 0.118 Uiso 1 1 calc R . . H14C H 0.6730 0.3619 0.1591 0.118 Uiso 1 1 calc R . . C15 C 0.57465(12) 0.4431(2) 0.4597(3) 0.0749(11) Uani 1 1 d . . . H15 H 0.5722 0.3803 0.4759 0.090 Uiso 1 1 calc R . . C16 C 0.53601(15) 0.4722(5) 0.3972(4) 0.132(2) Uani 1 1 d . . . H16A H 0.5370 0.5346 0.3835 0.198 Uiso 1 1 calc R . . H16B H 0.5159 0.4616 0.4298 0.198 Uiso 1 1 calc R . . H16C H 0.5301 0.4390 0.3381 0.198 Uiso 1 1 calc R . . C17 C 0.58387(19) 0.4944(4) 0.5508(4) 0.132(2) Uani 1 1 d . . . H17A H 0.6086 0.4748 0.5917 0.198 Uiso 1 1 calc R . . H17B H 0.5635 0.4851 0.5829 0.198 Uiso 1 1 calc R . . H17C H 0.5854 0.5567 0.5370 0.198 Uiso 1 1 calc R . . C18 C 0.57541(8) 0.10927(19) 0.58292(19) 0.0428(7) Uani 1 1 d . . . C19 C 0.58644(8) 0.0216(2) 0.6031(2) 0.0459(7) Uani 1 1 d . . . C20 C 0.58123(9) -0.0151(2) 0.6857(2) 0.0527(8) Uani 1 1 d . . . H20 H 0.5879 -0.0745 0.6997 0.063 Uiso 1 1 calc R . . C21 C 0.56656(10) 0.0331(2) 0.7471(2) 0.0597(9) Uani 1 1 d . . . H21 H 0.5630 0.0068 0.8027 0.072 Uiso 1 1 calc R . . C22 C 0.55700(10) 0.1193(2) 0.7280(2) 0.0596(9) Uani 1 1 d . . . H22 H 0.5472 0.1522 0.7713 0.072 Uiso 1 1 calc R . . C23 C 0.56139(9) 0.1594(2) 0.6467(2) 0.0510(8) Uani 1 1 d . . . C24 C 0.60480(9) -0.03299(19) 0.5402(2) 0.0503(8) Uani 1 1 d . . . H24 H 0.6035 0.0018 0.4818 0.060 Uiso 1 1 calc R . . C25 C 0.58389(12) -0.1193(2) 0.5096(3) 0.0716(10) Uani 1 1 d . . . H25A H 0.5854 -0.1558 0.5652 0.107 Uiso 1 1 calc R . . H25B H 0.5960 -0.1498 0.4663 0.107 Uiso 1 1 calc R . . H25C H 0.5568 -0.1076 0.4775 0.107 Uiso 1 1 calc R . . C26 C 0.64744(10) -0.0498(2) 0.5889(3) 0.0693(10) Uani 1 1 d . . . H26A H 0.6607 0.0061 0.6061 0.104 Uiso 1 1 calc R . . H26B H 0.6593 -0.0815 0.5458 0.104 Uiso 1 1 calc R . . H26C H 0.6496 -0.0847 0.6460 0.104 Uiso 1 1 calc R . . C27 C 0.55163(11) 0.2560(2) 0.6287(2) 0.0609(9) Uani 1 1 d . . . H27 H 0.5685 0.2788 0.5898 0.073 Uiso 1 1 calc R . . C28 C 0.56011(15) 0.3105(3) 0.7186(3) 0.0940(14) Uani 1 1 d . . . H28A H 0.5596 0.3726 0.7023 0.141 Uiso 1 1 calc R . . H28B H 0.5856 0.2952 0.7590 0.141 Uiso 1 1 calc R . . H28C H 0.5406 0.2987 0.7524 0.141 Uiso 1 1 calc R . . C29 C 0.51027(14) 0.2691(3) 0.5713(3) 0.0918(14) Uani 1 1 d . . . H29A H 0.5070 0.2459 0.5075 0.138 Uiso 1 1 calc R . . H29B H 0.5041 0.3316 0.5676 0.138 Uiso 1 1 calc R . . H29C H 0.4929 0.2383 0.6017 0.138 Uiso 1 1 calc R . . C36 C 0.70587(9) 0.1254(2) 0.5181(3) 0.0588(9) Uani 1 1 d . . . H36 H 0.7143 0.1615 0.5723 0.071 Uiso 1 1 calc R . . C37 C 0.73193(10) 0.0682(2) 0.4959(3) 0.0688(10) Uani 1 1 d . . . H37 H 0.7577 0.0662 0.5344 0.083 Uiso 1 1 calc R . . C38 C 0.72081(12) 0.0142(2) 0.4184(3) 0.0669(10) Uani 1 1 d . . . C39 C 0.68271(12) 0.0198(2) 0.3655(3) 0.0658(10) Uani 1 1 d . . . H39 H 0.6735 -0.0169 0.3121 0.079 Uiso 1 1 calc R . . C40 C 0.65840(10) 0.0786(2) 0.3909(2) 0.0552(8) Uani 1 1 d . . . H40 H 0.6325 0.0819 0.3532 0.066 Uiso 1 1 calc R . . C41 C 0.74893(14) -0.0479(3) 0.3928(4) 0.0986(15) Uani 1 1 d . . . H41A H 0.7454 -0.1065 0.4158 0.148 Uiso 1 1 calc R . . H41B H 0.7753 -0.0281 0.4218 0.148 Uiso 1 1 calc R . . H41C H 0.7444 -0.0494 0.3240 0.148 Uiso 1 1 calc R . . N3 N 0.65944(8) 0.27000(18) 0.6254(2) 0.0610(8) Uani 1 1 d . . . C30 C 0.66152(11) 0.2291(2) 0.7131(3) 0.0701(10) Uani 1 1 d . . . C31 C 0.68821(12) 0.2458(3) 0.7942(3) 0.0760(11) Uani 1 1 d . . . H31 H 0.6856 0.2205 0.8512 0.091 Uiso 1 1 calc R . . C32 C 0.72067(15) 0.3015(4) 0.7965(3) 0.1040(16) Uani 1 1 d . . . C33 C 0.71611(13) 0.3496(3) 0.7112(3) 0.0897(13) Uani 1 1 d . . . H33 H 0.7352 0.3909 0.7069 0.108 Uiso 1 1 calc R . . C34 C 0.68627(12) 0.3382(3) 0.6387(3) 0.0753(12) Uani 1 1 d . . . C35 C 0.7466(2) 0.3256(5) 0.8775(5) 0.174(3) Uani 1 1 d . . . H35A H 0.7727 0.3217 0.8692 0.261 Uiso 1 1 calc R . . H35B H 0.7445 0.2867 0.9289 0.261 Uiso 1 1 calc R . . H35C H 0.7415 0.3858 0.8932 0.261 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 0.0404(6) 0.0413(5) 0.0495(6) -0.0003(4) 0.0069(4) -0.0041(4) N1 0.0393(14) 0.0367(13) 0.0522(15) 0.0024(11) 0.0133(12) -0.0020(10) N2 0.0422(14) 0.0400(13) 0.0372(13) -0.0027(10) 0.0094(11) -0.0026(10) N4 0.0434(15) 0.0473(15) 0.0566(16) 0.0035(13) 0.0078(12) -0.0031(12) C1 0.054(2) 0.061(2) 0.056(2) 0.0168(16) 0.0092(16) 0.0021(16) C2 0.0411(17) 0.0430(16) 0.0428(17) 0.0021(13) 0.0128(14) 0.0028(13) C3 0.0404(17) 0.0460(16) 0.0375(16) -0.0048(13) 0.0053(13) -0.0023(13) C4 0.0403(16) 0.0363(15) 0.0417(17) -0.0050(13) 0.0128(14) -0.0015(12) C5 0.0461(18) 0.0536(18) 0.0481(18) -0.0007(14) 0.0132(14) -0.0098(14) C6 0.0511(19) 0.0381(16) 0.060(2) 0.0064(14) 0.0118(16) -0.0042(14) C7 0.051(2) 0.0444(18) 0.077(2) 0.0062(16) 0.0185(18) -0.0056(15) C8 0.083(3) 0.055(2) 0.128(4) 0.010(2) 0.054(3) -0.012(2) C9 0.122(4) 0.046(2) 0.161(5) -0.002(3) 0.075(4) -0.021(2) C10 0.114(4) 0.040(2) 0.137(4) -0.003(2) 0.058(3) -0.004(2) C11 0.074(2) 0.0404(18) 0.084(3) 0.0035(17) 0.027(2) -0.0021(16) C12 0.049(2) 0.055(2) 0.073(2) 0.0107(17) 0.0256(17) -0.0035(15) C13 0.057(2) 0.078(3) 0.106(3) 0.015(2) 0.027(2) 0.0045(19) C14 0.079(3) 0.075(3) 0.089(3) 0.004(2) 0.036(2) -0.007(2) C15 0.098(3) 0.0416(19) 0.099(3) -0.0035(19) 0.049(3) 0.0045(19) C16 0.092(4) 0.180(6) 0.134(5) -0.017(4) 0.048(4) 0.021(4) C17 0.151(5) 0.151(5) 0.107(4) -0.036(4) 0.058(4) -0.017(4) C18 0.0425(17) 0.0491(17) 0.0358(16) -0.0006(13) 0.0088(13) -0.0067(13) C19 0.0438(17) 0.0512(18) 0.0395(17) 0.0025(14) 0.0053(13) -0.0056(14) C20 0.056(2) 0.0560(19) 0.0428(18) 0.0070(15) 0.0084(15) -0.0057(15) C21 0.067(2) 0.072(2) 0.0406(19) 0.0049(17) 0.0148(16) -0.0062(18) C22 0.065(2) 0.072(2) 0.046(2) -0.0059(17) 0.0207(17) -0.0056(18) C23 0.054(2) 0.0549(19) 0.0454(19) -0.0049(15) 0.0151(15) -0.0069(15) C24 0.058(2) 0.0462(18) 0.0477(18) 0.0059(14) 0.0160(15) 0.0009(15) C25 0.096(3) 0.053(2) 0.070(2) -0.0059(18) 0.030(2) -0.0087(19) C26 0.067(2) 0.073(2) 0.069(2) 0.0150(19) 0.0188(19) 0.0160(19) C27 0.076(2) 0.0525(19) 0.063(2) -0.0071(16) 0.0339(19) -0.0005(17) C28 0.117(4) 0.072(3) 0.098(3) -0.034(2) 0.038(3) -0.007(2) C29 0.102(4) 0.067(3) 0.099(3) -0.009(2) 0.016(3) 0.020(2) C36 0.044(2) 0.0539(19) 0.073(2) -0.0033(17) 0.0044(17) -0.0012(15) C37 0.045(2) 0.057(2) 0.102(3) 0.005(2) 0.015(2) 0.0055(16) C38 0.073(3) 0.0449(19) 0.092(3) 0.0064(19) 0.038(2) 0.0032(17) C39 0.083(3) 0.051(2) 0.067(2) -0.0039(17) 0.026(2) -0.0051(19) C40 0.055(2) 0.055(2) 0.054(2) 0.0024(16) 0.0121(16) -0.0055(16) C41 0.107(4) 0.059(2) 0.150(4) 0.004(3) 0.070(3) 0.016(2) N3 0.0553(17) 0.0565(17) 0.0644(19) -0.0086(14) 0.0039(14) -0.0062(13) C30 0.073(3) 0.072(2) 0.060(2) 0.0003(19) 0.008(2) -0.0034(19) C31 0.079(3) 0.088(3) 0.052(2) -0.001(2) 0.004(2) -0.004(2) C32 0.106(4) 0.124(4) 0.074(3) -0.003(3) 0.008(3) -0.049(3) C33 0.078(3) 0.088(3) 0.102(4) -0.003(3) 0.022(3) -0.025(2) C34 0.083(3) 0.075(3) 0.064(2) -0.0051(19) 0.012(2) -0.045(2) C35 0.167(7) 0.192(7) 0.124(5) 0.005(5) -0.031(5) -0.079(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mg1 N3 1.993(3) . ? Mg1 N2 2.044(2) . ? Mg1 N1 2.047(3) . ? Mg1 N4 2.140(3) . ? N1 C2 1.326(4) . ? N1 C6 1.445(4) . ? N2 C4 1.325(3) . ? N2 C18 1.440(4) . ? N4 C40 1.343(4) . ? N4 C36 1.345(4) . ? C1 C2 1.522(4) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1 0.9800 . ? C2 C3 1.401(4) . ? C3 C4 1.407(4) . ? C3 H3 0.9500 . ? C4 C5 1.516(4) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 C7 1.402(4) . ? C6 C11 1.407(5) . ? C7 C8 1.390(5) . ? C7 C12 1.513(5) . ? C8 C9 1.373(6) . ? C8 H8 0.9500 . ? C9 C10 1.373(6) . ? C9 H9 0.9500 . ? C10 C11 1.389(5) . ? C10 H10 0.9500 . ? C11 C15 1.520(5) . ? C12 C14 1.524(5) . ? C12 C13 1.530(5) . ? C12 H12 1.0000 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C17 1.512(6) . ? C15 C16 1.515(7) . ? C15 H15 1.0000 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C23 1.405(4) . ? C18 C19 1.409(4) . ? C19 C20 1.393(4) . ? C19 C24 1.522(4) . ? C20 C21 1.375(5) . ? C20 H20 0.9500 . ? C21 C22 1.374(5) . ? C21 H21 0.9500 . ? C22 C23 1.388(4) . ? C22 H22 0.9500 . ? C23 C27 1.526(5) . ? C24 C25 1.528(4) . ? C24 C26 1.533(5) . ? C24 H24 1.0000 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C29 1.517(5) . ? C27 C28 1.524(5) . ? C27 H27 1.0000 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C36 C37 1.384(5) . ? C36 H36 0.9500 . ? C37 C38 1.378(5) . ? C37 H37 0.9500 . ? C38 C39 1.387(5) . ? C38 C41 1.508(5) . ? C39 C40 1.376(5) . ? C39 H39 0.9500 . ? C40 H40 0.9500 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? N3 C34 1.401(4) . ? N3 C30 1.418(5) . ? C30 C31 1.341(5) . ? C31 C32 1.439(6) . ? C31 H31 0.9500 . ? C32 C35 1.355(7) . ? C32 C33 1.426(6) . ? C33 C34 1.308(5) . ? C33 H33 0.9500 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 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 118.74(12) . . ? N3 Mg1 N1 125.65(11) . . ? N2 Mg1 N1 93.36(10) . . ? N3 Mg1 N4 103.30(12) . . ? N2 Mg1 N4 106.94(10) . . ? N1 Mg1 N4 107.60(10) . . ? C2 N1 C6 119.2(2) . . ? C2 N1 Mg1 120.69(18) . . ? C6 N1 Mg1 120.14(19) . . ? C4 N2 C18 118.0(2) . . ? C4 N2 Mg1 121.28(18) . . ? C18 N2 Mg1 120.69(17) . . ? C40 N4 C36 116.6(3) . . ? C40 N4 Mg1 121.6(2) . . ? C36 N4 Mg1 121.8(2) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1 109.5 . . ? H1A C1 H1 109.5 . . ? H1B C1 H1 109.5 . . ? N1 C2 C3 123.8(3) . . ? N1 C2 C1 120.8(3) . . ? C3 C2 C1 115.4(3) . . ? C2 C3 C4 130.2(3) . . ? C2 C3 H3 114.9 . . ? C4 C3 H3 114.9 . . ? N2 C4 C3 123.4(3) . . ? N2 C4 C5 120.4(2) . . ? C3 C4 C5 116.2(3) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C7 C6 C11 121.2(3) . . ? C7 C6 N1 120.5(3) . . ? C11 C6 N1 118.2(3) . . ? C8 C7 C6 118.0(3) . . ? C8 C7 C12 119.5(3) . . ? C6 C7 C12 122.5(3) . . ? C9 C8 C7 121.6(4) . . ? C9 C8 H8 119.2 . . ? C7 C8 H8 119.2 . . ? C10 C9 C8 119.5(4) . . ? C10 C9 H9 120.2 . . ? C8 C9 H9 120.2 . . ? C9 C10 C11 121.9(4) . . ? C9 C10 H10 119.0 . . ? C11 C10 H10 119.0 . . ? C10 C11 C6 117.7(3) . . ? C10 C11 C15 120.4(3) . . ? C6 C11 C15 121.9(3) . . ? C7 C12 C14 113.2(3) . . ? C7 C12 C13 110.7(3) . . ? C14 C12 C13 110.0(3) . . ? C7 C12 H12 107.6 . . ? C14 C12 H12 107.6 . . ? C13 C12 H12 107.6 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C17 C15 C16 109.5(4) . . ? C17 C15 C11 113.6(4) . . ? C16 C15 C11 111.0(4) . . ? C17 C15 H15 107.5 . . ? C16 C15 H15 107.5 . . ? C11 C15 H15 107.5 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C23 C18 C19 120.7(3) . . ? C23 C18 N2 118.8(3) . . ? C19 C18 N2 120.3(3) . . ? C20 C19 C18 118.1(3) . . ? C20 C19 C24 119.2(3) . . ? C18 C19 C24 122.6(3) . . ? C21 C20 C19 121.3(3) . . ? C21 C20 H20 119.4 . . ? C19 C20 H20 119.4 . . ? C22 C21 C20 120.0(3) . . ? C22 C21 H21 120.0 . . ? C20 C21 H21 120.0 . . ? C21 C22 C23 121.4(3) . . ? C21 C22 H22 119.3 . . ? C23 C22 H22 119.3 . . ? C22 C23 C18 118.4(3) . . ? C22 C23 C27 120.3(3) . . ? C18 C23 C27 121.3(3) . . ? C19 C24 C25 113.2(3) . . ? C19 C24 C26 110.5(3) . . ? C25 C24 C26 110.3(3) . . ? C19 C24 H24 107.5 . . ? C25 C24 H24 107.5 . . ? C26 C24 H24 107.5 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C29 C27 C28 110.5(3) . . ? C29 C27 C23 111.8(3) . . ? C28 C27 C23 113.3(3) . . ? C29 C27 H27 106.9 . . ? C28 C27 H27 106.9 . . ? C23 C27 H27 106.9 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? N4 C36 C37 122.6(3) . . ? N4 C36 H36 118.7 . . ? C37 C36 H36 118.7 . . ? C38 C37 C36 120.5(3) . . ? C38 C37 H37 119.7 . . ? C36 C37 H37 119.7 . . ? C37 C38 C39 117.0(3) . . ? C37 C38 C41 121.2(4) . . ? C39 C38 C41 121.9(4) . . ? C40 C39 C38 119.5(3) . . ? C40 C39 H39 120.2 . . ? C38 C39 H39 120.2 . . ? N4 C40 C39 123.8(3) . . ? N4 C40 H40 118.1 . . ? C39 C40 H40 118.1 . . ? C38 C41 H41A 109.5 . . ? C38 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C38 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C34 N3 C30 109.6(3) . . ? C34 N3 Mg1 126.9(2) . . ? C30 N3 Mg1 122.6(2) . . ? C31 C30 N3 125.1(4) . . ? C30 C31 C32 121.3(4) . . ? C30 C31 H31 119.3 . . ? C32 C31 H31 119.3 . . ? C35 C32 C33 121.6(5) . . ? C35 C32 C31 123.3(5) . . ? C33 C32 C31 112.5(4) . . ? C34 C33 C32 121.7(4) . . ? C34 C33 H33 119.1 . . ? C32 C33 H33 119.1 . . ? C33 C34 N3 126.8(4) . . ? C32 C35 H35A 109.5 . . ? C32 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C32 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 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 C2 -154.2(2) . . . . ? N2 Mg1 N1 C2 -24.8(2) . . . . ? N4 Mg1 N1 C2 84.1(2) . . . . ? N3 Mg1 N1 C6 27.2(3) . . . . ? N2 Mg1 N1 C6 156.6(2) . . . . ? N4 Mg1 N1 C6 -94.4(2) . . . . ? N3 Mg1 N2 C4 157.7(2) . . . . ? N1 Mg1 N2 C4 23.4(2) . . . . ? N4 Mg1 N2 C4 -86.1(2) . . . . ? N3 Mg1 N2 C18 -23.7(2) . . . . ? N1 Mg1 N2 C18 -158.0(2) . . . . ? N4 Mg1 N2 C18 92.5(2) . . . . ? N3 Mg1 N4 C40 173.8(2) . . . . ? N2 Mg1 N4 C40 47.7(2) . . . . ? N1 Mg1 N4 C40 -51.5(2) . . . . ? N3 Mg1 N4 C36 -4.8(3) . . . . ? N2 Mg1 N4 C36 -130.9(2) . . . . ? N1 Mg1 N4 C36 129.8(2) . . . . ? C6 N1 C2 C3 -169.4(3) . . . . ? Mg1 N1 C2 C3 12.0(4) . . . . ? C6 N1 C2 C1 8.6(4) . . . . ? Mg1 N1 C2 C1 -169.9(2) . . . . ? N1 C2 C3 C4 13.3(5) . . . . ? C1 C2 C3 C4 -164.9(3) . . . . ? C18 N2 C4 C3 172.4(3) . . . . ? Mg1 N2 C4 C3 -9.0(4) . . . . ? C18 N2 C4 C5 -5.6(4) . . . . ? Mg1 N2 C4 C5 173.1(2) . . . . ? C2 C3 C4 N2 -15.1(5) . . . . ? C2 C3 C4 C5 163.0(3) . . . . ? C2 N1 C6 C7 -87.7(4) . . . . ? Mg1 N1 C6 C7 90.9(3) . . . . ? C2 N1 C6 C11 94.2(4) . . . . ? Mg1 N1 C6 C11 -87.3(3) . . . . ? C11 C6 C7 C8 0.5(5) . . . . ? N1 C6 C7 C8 -177.6(3) . . . . ? C11 C6 C7 C12 179.4(3) . . . . ? N1 C6 C7 C12 1.3(5) . . . . ? C6 C7 C8 C9 -0.6(6) . . . . ? C12 C7 C8 C9 -179.6(4) . . . . ? C7 C8 C9 C10 0.6(8) . . . . ? C8 C9 C10 C11 -0.5(8) . . . . ? C9 C10 C11 C6 0.4(7) . . . . ? C9 C10 C11 C15 -177.6(5) . . . . ? C7 C6 C11 C10 -0.4(5) . . . . ? N1 C6 C11 C10 177.8(3) . . . . ? C7 C6 C11 C15 177.6(3) . . . . ? N1 C6 C11 C15 -4.3(5) . . . . ? C8 C7 C12 C14 -55.1(5) . . . . ? C6 C7 C12 C14 126.0(4) . . . . ? C8 C7 C12 C13 68.9(4) . . . . ? C6 C7 C12 C13 -110.0(4) . . . . ? C10 C11 C15 C17 -46.8(6) . . . . ? C6 C11 C15 C17 135.3(4) . . . . ? C10 C11 C15 C16 77.0(5) . . . . ? C6 C11 C15 C16 -100.9(5) . . . . ? C4 N2 C18 C23 -98.2(3) . . . . ? Mg1 N2 C18 C23 83.1(3) . . . . ? C4 N2 C18 C19 85.4(3) . . . . ? Mg1 N2 C18 C19 -93.2(3) . . . . ? C23 C18 C19 C20 3.2(4) . . . . ? N2 C18 C19 C20 179.5(3) . . . . ? C23 C18 C19 C24 -174.9(3) . . . . ? N2 C18 C19 C24 1.4(4) . . . . ? C18 C19 C20 C21 -1.5(4) . . . . ? C24 C19 C20 C21 176.7(3) . . . . ? C19 C20 C21 C22 -0.5(5) . . . . ? C20 C21 C22 C23 0.8(5) . . . . ? C21 C22 C23 C18 0.9(5) . . . . ? C21 C22 C23 C27 -178.2(3) . . . . ? C19 C18 C23 C22 -3.0(4) . . . . ? N2 C18 C23 C22 -179.3(3) . . . . ? C19 C18 C23 C27 176.2(3) . . . . ? N2 C18 C23 C27 -0.1(4) . . . . ? C20 C19 C24 C25 55.5(4) . . . . ? C18 C19 C24 C25 -126.5(3) . . . . ? C20 C19 C24 C26 -68.8(4) . . . . ? C18 C19 C24 C26 109.3(3) . . . . ? C22 C23 C27 C29 -92.1(4) . . . . ? C18 C23 C27 C29 88.7(4) . . . . ? C22 C23 C27 C28 33.5(5) . . . . ? C18 C23 C27 C28 -145.6(3) . . . . ? C40 N4 C36 C37 0.9(5) . . . . ? Mg1 N4 C36 C37 179.6(3) . . . . ? N4 C36 C37 C38 -0.5(5) . . . . ? C36 C37 C38 C39 -0.6(5) . . . . ? C36 C37 C38 C41 179.5(3) . . . . ? C37 C38 C39 C40 1.2(5) . . . . ? C41 C38 C39 C40 -178.9(3) . . . . ? C36 N4 C40 C39 -0.2(5) . . . . ? Mg1 N4 C40 C39 -178.9(2) . . . . ? C38 C39 C40 N4 -0.9(5) . . . . ? N2 Mg1 N3 C34 -160.3(3) . . . . ? N1 Mg1 N3 C34 -41.9(4) . . . . ? N4 Mg1 N3 C34 81.6(3) . . . . ? N2 Mg1 N3 C30 31.7(3) . . . . ? N1 Mg1 N3 C30 150.1(3) . . . . ? N4 Mg1 N3 C30 -86.4(3) . . . . ? C34 N3 C30 C31 -7.6(5) . . . . ? Mg1 N3 C30 C31 162.2(3) . . . . ? N3 C30 C31 C32 -7.5(7) . . . . ? C30 C31 C32 C35 174.7(6) . . . . ? C30 C31 C32 C33 13.2(7) . . . . ? C35 C32 C33 C34 -165.6(6) . . . . ? C31 C32 C33 C34 -3.8(7) . . . . ? C32 C33 C34 N3 -13.1(8) . . . . ? C30 N3 C34 C33 18.2(6) . . . . ? Mg1 N3 C34 C33 -151.0(4) . . . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.341 _refine_diff_density_min -0.201 _refine_diff_density_rms 0.042 #===end data_7-k10msh13 _database_code_depnum_ccdc_archive 'CCDC 831738' #TrackingRef '- bigcif.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C43 H60 Mg N4' _chemical_formula_weight 657.26 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 0.0486 0.0363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P212121 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 10.5988(1) _cell_length_b 18.1105(2) _cell_length_c 21.0057(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4032.04(7) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 63184 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 27.485 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.083 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1432 _exptl_absorpt_coefficient_mu 0.077 # Absorption correction _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.825 _exptl_absorpt_correction_T_max 0.985 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_measurement_device_type '95mm CCD camera on \k-goniostat' _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 55112 _diffrn_reflns_av_R_equivalents 0.0481 _diffrn_reflns_av_sigmaI/netI 0.0250 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 3.54 _diffrn_reflns_theta_max 27.52 _reflns_number_total 9226 _reflns_number_gt 8599 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Bruker AXS BV 1997-2004)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo & Scalepack (Otwinowski, Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick 1990)' _computing_structure_refinement 'SHELXL-97/2 (Sheldrick 1997)' _computing_molecular_graphics 'ORTEX (P.McArdle 1995)' _computing_publication_material 'SHELXL-97/2 (Sheldrick 1997)' _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^)+(0.0518P)^2^+0.7753P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.06(16) _refine_ls_number_reflns 9226 _refine_ls_number_parameters 447 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0426 _refine_ls_R_factor_gt 0.0384 _refine_ls_wR_factor_ref 0.1014 _refine_ls_wR_factor_gt 0.0980 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.055 _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 0.45681(4) 0.55155(2) 0.22832(2) 0.02663(10) Uani 1 1 d . . . N1 N 0.56019(11) 0.58013(6) 0.14948(5) 0.0278(2) Uani 1 1 d . . . N2 N 0.43919(11) 0.65888(6) 0.25887(5) 0.0255(2) Uani 1 1 d . . . N3 N 0.31742(12) 0.47862(7) 0.22522(6) 0.0358(3) Uani 1 1 d . . . N4 N 0.58501(12) 0.50863(7) 0.29696(6) 0.0308(3) Uani 1 1 d . . . C1 C 0.71645(16) 0.65758(9) 0.09357(8) 0.0397(4) Uani 1 1 d . . . H1A H 0.7955 0.6315 0.1026 0.060 Uiso 1 1 calc R . . H1B H 0.7330 0.7107 0.0903 0.060 Uiso 1 1 calc R . . H1C H 0.6812 0.6396 0.0533 0.060 Uiso 1 1 calc R . . C2 C 0.62329(13) 0.64357(8) 0.14683(7) 0.0287(3) Uani 1 1 d . . . C3 C 0.60855(14) 0.70142(8) 0.19087(7) 0.0294(3) Uani 1 1 d . . . H3 H 0.6696 0.7397 0.1878 0.035 Uiso 1 1 calc R . . C4 C 0.51674(13) 0.71138(8) 0.23897(6) 0.0270(3) Uani 1 1 d . . . C5 C 0.50796(16) 0.78843(8) 0.26636(8) 0.0386(3) Uani 1 1 d . . . H5A H 0.4305 0.8122 0.2512 0.058 Uiso 1 1 calc R . . H5B H 0.5812 0.8174 0.2527 0.058 Uiso 1 1 calc R . . H5C H 0.5065 0.7856 0.3129 0.058 Uiso 1 1 calc R . . C6 C 0.56893(14) 0.52761(8) 0.09836(7) 0.0310(3) Uani 1 1 d . . . C7 C 0.66874(16) 0.47711(8) 0.09527(7) 0.0352(3) Uani 1 1 d . . . C8 C 0.6646(2) 0.42160(10) 0.04895(8) 0.0468(4) Uani 1 1 d . . . H8 H 0.7312 0.3866 0.0466 0.056 Uiso 1 1 calc R . . C9 C 0.5651(2) 0.41689(10) 0.00655(8) 0.0517(5) Uani 1 1 d . . . H9 H 0.5636 0.3788 -0.0246 0.062 Uiso 1 1 calc R . . C10 C 0.46815(19) 0.46749(10) 0.00950(8) 0.0445(4) Uani 1 1 d . . . H10 H 0.4007 0.4640 -0.0201 0.053 Uiso 1 1 calc R . . C11 C 0.46660(16) 0.52369(9) 0.05487(7) 0.0365(3) Uani 1 1 d . . . C12 C 0.77836(15) 0.47769(9) 0.14186(8) 0.0366(3) Uani 1 1 d . . . H12 H 0.7721 0.5238 0.1678 0.044 Uiso 1 1 calc R . . C13 C 0.90742(18) 0.47779(12) 0.10846(10) 0.0537(5) Uani 1 1 d . . . H13A H 0.9172 0.4321 0.0839 0.080 Uiso 1 1 calc R . . H13B H 0.9745 0.4810 0.1404 0.080 Uiso 1 1 calc R . . H13C H 0.9128 0.5203 0.0797 0.080 Uiso 1 1 calc R . . C14 C 0.76940(19) 0.41177(10) 0.18746(9) 0.0460(4) Uani 1 1 d . . . H14A H 0.6848 0.4100 0.2062 0.069 Uiso 1 1 calc R . . H14B H 0.8323 0.4172 0.2214 0.069 Uiso 1 1 calc R . . H14C H 0.7854 0.3660 0.1640 0.069 Uiso 1 1 calc R . . C15 C 0.35738(18) 0.57798(11) 0.05919(8) 0.0452(4) Uani 1 1 d . . . H15 H 0.3392 0.5852 0.1055 0.054 Uiso 1 1 calc R . . C16 C 0.23507(19) 0.55021(15) 0.02848(9) 0.0585(5) Uani 1 1 d . . . H16A H 0.2477 0.5446 -0.0175 0.088 Uiso 1 1 calc R . . H16B H 0.1673 0.5859 0.0363 0.088 Uiso 1 1 calc R . . H16C H 0.2121 0.5024 0.0470 0.088 Uiso 1 1 calc R . . C17 C 0.3913(2) 0.65346(12) 0.03218(10) 0.0576(5) Uani 1 1 d . . . H17A H 0.4572 0.6761 0.0584 0.086 Uiso 1 1 calc R . . H17B H 0.3163 0.6851 0.0323 0.086 Uiso 1 1 calc R . . H17C H 0.4221 0.6478 -0.0115 0.086 Uiso 1 1 calc R . . C18 C 0.33772(14) 0.67804(7) 0.30151(7) 0.0276(3) Uani 1 1 d . . . C19 C 0.21743(14) 0.69146(8) 0.27536(7) 0.0304(3) Uani 1 1 d . . . C20 C 0.11852(15) 0.70922(9) 0.31627(8) 0.0350(3) Uani 1 1 d . . . H20 H 0.0377 0.7198 0.2990 0.042 Uiso 1 1 calc R . . C21 C 0.13569(16) 0.71175(9) 0.38149(8) 0.0383(3) Uani 1 1 d . . . H21 H 0.0671 0.7240 0.4086 0.046 Uiso 1 1 calc R . . C22 C 0.25252(16) 0.69640(9) 0.40705(7) 0.0366(3) Uani 1 1 d . . . H22 H 0.2633 0.6973 0.4519 0.044 Uiso 1 1 calc R . . C23 C 0.35553(14) 0.67951(8) 0.36804(7) 0.0309(3) Uani 1 1 d . . . C24 C 0.19456(15) 0.68838(9) 0.20382(7) 0.0350(3) Uani 1 1 d . . . H24 H 0.2744 0.6707 0.1835 0.042 Uiso 1 1 calc R . . C25 C 0.0914(3) 0.63338(16) 0.18674(10) 0.0735(7) Uani 1 1 d . . . H25A H 0.0113 0.6494 0.2055 0.110 Uiso 1 1 calc R . . H25B H 0.1137 0.5845 0.2034 0.110 Uiso 1 1 calc R . . H25C H 0.0827 0.6308 0.1403 0.110 Uiso 1 1 calc R . . C26 C 0.1667(3) 0.76413(13) 0.17708(10) 0.0725(7) Uani 1 1 d . . . H26A H 0.1570 0.7608 0.1308 0.109 Uiso 1 1 calc R . . H26B H 0.2366 0.7976 0.1872 0.109 Uiso 1 1 calc R . . H26C H 0.0886 0.7831 0.1959 0.109 Uiso 1 1 calc R . . C27 C 0.48180(16) 0.66195(9) 0.39912(7) 0.0374(3) Uani 1 1 d . . . H27 H 0.5455 0.6539 0.3647 0.045 Uiso 1 1 calc R . . C28 C 0.5284(2) 0.72535(12) 0.44173(9) 0.0507(4) Uani 1 1 d . . . H28A H 0.5339 0.7708 0.4166 0.076 Uiso 1 1 calc R . . H28B H 0.6119 0.7131 0.4587 0.076 Uiso 1 1 calc R . . H28C H 0.4691 0.7325 0.4770 0.076 Uiso 1 1 calc R . . C29 C 0.4727(2) 0.59132(11) 0.43847(8) 0.0491(4) Uani 1 1 d . . . H29A H 0.4190 0.6001 0.4757 0.074 Uiso 1 1 calc R . . H29B H 0.5572 0.5767 0.4526 0.074 Uiso 1 1 calc R . . H29C H 0.4361 0.5519 0.4124 0.074 Uiso 1 1 calc R . . C30 C 0.28832(15) 0.43188(9) 0.17457(7) 0.0336(3) Uani 1 1 d . . . H30 H 0.3309 0.4412 0.1356 0.040 Uiso 1 1 calc R . . C31 C 0.20724(15) 0.37555(9) 0.17489(7) 0.0340(3) Uani 1 1 d . . . C32 C 0.13714(14) 0.35458(9) 0.23442(8) 0.0358(3) Uani 1 1 d . . . H32A H 0.1588 0.3032 0.2464 0.043 Uiso 1 1 calc R . . H32B H 0.0452 0.3568 0.2263 0.043 Uiso 1 1 calc R . . C33 C 0.17008(15) 0.40568(10) 0.28838(7) 0.0375(3) Uani 1 1 d . . . C34 C 0.25140(15) 0.46152(10) 0.28023(7) 0.0374(3) Uani 1 1 d . . . H34 H 0.2653 0.4927 0.3159 0.045 Uiso 1 1 calc R . . C35 C 0.18375(18) 0.32860(10) 0.11786(9) 0.0454(4) Uani 1 1 d . . . H35A H 0.2342 0.3468 0.0821 0.068 Uiso 1 1 calc R . . H35B H 0.0940 0.3306 0.1067 0.068 Uiso 1 1 calc R . . H35C H 0.2076 0.2775 0.1273 0.068 Uiso 1 1 calc R . . C36 C 0.1083(2) 0.39006(13) 0.35115(9) 0.0553(5) Uani 1 1 d . . . H36A H 0.1362 0.4265 0.3826 0.083 Uiso 1 1 calc R . . H36B H 0.1318 0.3405 0.3655 0.083 Uiso 1 1 calc R . . H36C H 0.0164 0.3930 0.3463 0.083 Uiso 1 1 calc R . . C37 C 0.56087(14) 0.45223(8) 0.33634(7) 0.0318(3) Uani 1 1 d . . . H37 H 0.4817 0.4280 0.3330 0.038 Uiso 1 1 calc R . . C38 C 0.64574(16) 0.42752(9) 0.38169(7) 0.0363(3) Uani 1 1 d . . . C39 C 0.76334(16) 0.46127(10) 0.38400(8) 0.0398(4) Uani 1 1 d . . . H39 H 0.8242 0.4453 0.4142 0.048 Uiso 1 1 calc R . . C40 C 0.79215(16) 0.51849(10) 0.34214(8) 0.0392(3) Uani 1 1 d . . . C41 C 0.69832(15) 0.54121(9) 0.30074(7) 0.0341(3) Uani 1 1 d . . . H41 H 0.7151 0.5820 0.2736 0.041 Uiso 1 1 calc R . . C42 C 0.6085(2) 0.36698(12) 0.42732(9) 0.0526(5) Uani 1 1 d . . . H42A H 0.5589 0.3880 0.4623 0.079 Uiso 1 1 calc R . . H42B H 0.6845 0.3436 0.4445 0.079 Uiso 1 1 calc R . . H42C H 0.5578 0.3300 0.4048 0.079 Uiso 1 1 calc R . . C43 C 0.92007(19) 0.55430(15) 0.33947(10) 0.0614(6) Uani 1 1 d . . . H43A H 0.9694 0.5323 0.3049 0.092 Uiso 1 1 calc R . . H43B H 0.9639 0.5466 0.3800 0.092 Uiso 1 1 calc R . . H43C H 0.9103 0.6074 0.3318 0.092 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 0.0331(2) 0.0244(2) 0.0224(2) -0.00108(17) 0.00066(18) -0.00386(19) N1 0.0324(6) 0.0281(6) 0.0229(5) -0.0011(4) 0.0017(4) -0.0022(5) N2 0.0275(6) 0.0258(5) 0.0230(5) -0.0015(4) 0.0005(4) -0.0005(4) N3 0.0371(7) 0.0378(7) 0.0327(6) -0.0011(5) 0.0015(5) -0.0093(5) N4 0.0394(7) 0.0257(6) 0.0272(6) -0.0022(5) -0.0006(5) 0.0017(5) C1 0.0458(9) 0.0372(8) 0.0362(8) 0.0001(7) 0.0138(7) -0.0078(7) C2 0.0296(7) 0.0318(7) 0.0249(6) 0.0015(5) 0.0014(5) -0.0016(6) C3 0.0314(7) 0.0269(7) 0.0300(7) 0.0011(5) 0.0019(5) -0.0066(6) C4 0.0316(7) 0.0249(6) 0.0246(6) -0.0004(5) -0.0025(5) -0.0009(5) C5 0.0477(9) 0.0256(7) 0.0424(8) -0.0039(6) 0.0103(7) -0.0042(6) C6 0.0385(8) 0.0313(7) 0.0232(6) -0.0009(5) 0.0055(5) -0.0076(6) C7 0.0459(8) 0.0297(7) 0.0300(7) -0.0028(6) 0.0070(6) -0.0043(6) C8 0.0681(12) 0.0344(8) 0.0378(9) -0.0076(7) 0.0048(8) 0.0035(8) C9 0.0833(14) 0.0362(9) 0.0355(8) -0.0120(7) 0.0012(9) -0.0065(9) C10 0.0595(11) 0.0473(10) 0.0268(7) -0.0053(6) -0.0011(7) -0.0122(8) C11 0.0466(9) 0.0400(8) 0.0230(6) -0.0017(6) 0.0031(6) -0.0076(7) C12 0.0399(8) 0.0330(8) 0.0370(8) -0.0040(6) 0.0056(6) 0.0032(6) C13 0.0465(10) 0.0583(12) 0.0562(12) -0.0061(9) 0.0133(8) 0.0042(9) C14 0.0561(11) 0.0355(9) 0.0463(10) 0.0002(7) 0.0034(8) 0.0089(8) C15 0.0478(9) 0.0606(11) 0.0271(7) -0.0046(7) -0.0056(7) 0.0010(8) C16 0.0505(11) 0.0861(15) 0.0391(9) -0.0006(10) -0.0075(8) -0.0054(11) C17 0.0684(13) 0.0519(11) 0.0526(11) -0.0050(9) -0.0197(10) 0.0055(10) C18 0.0335(7) 0.0219(6) 0.0275(7) -0.0001(5) 0.0044(5) -0.0018(5) C19 0.0347(7) 0.0257(7) 0.0308(7) 0.0004(6) 0.0026(6) -0.0011(5) C20 0.0317(7) 0.0322(7) 0.0411(8) 0.0008(6) 0.0039(6) -0.0004(6) C21 0.0389(8) 0.0360(8) 0.0400(8) -0.0006(7) 0.0146(7) -0.0014(7) C22 0.0476(9) 0.0353(8) 0.0269(7) -0.0003(6) 0.0096(6) 0.0005(7) C23 0.0376(7) 0.0284(7) 0.0267(7) -0.0004(5) 0.0033(6) 0.0000(6) C24 0.0323(7) 0.0421(8) 0.0304(7) -0.0009(6) -0.0008(6) 0.0022(6) C25 0.0813(16) 0.0962(18) 0.0431(11) 0.0051(11) -0.0188(11) -0.0401(14) C26 0.126(2) 0.0539(13) 0.0374(10) 0.0126(9) 0.0043(12) 0.0103(14) C27 0.0421(8) 0.0479(9) 0.0221(6) -0.0028(6) 0.0010(6) 0.0061(7) C28 0.0535(11) 0.0616(12) 0.0370(9) -0.0073(8) -0.0055(8) -0.0061(9) C29 0.0674(12) 0.0487(10) 0.0312(8) 0.0007(7) -0.0001(8) 0.0156(9) C30 0.0329(7) 0.0381(8) 0.0297(7) 0.0012(6) 0.0014(6) -0.0002(6) C31 0.0320(7) 0.0367(8) 0.0333(8) -0.0021(6) -0.0034(6) 0.0019(6) C32 0.0308(7) 0.0381(8) 0.0385(8) 0.0026(6) -0.0024(6) -0.0046(6) C33 0.0337(7) 0.0478(9) 0.0311(8) 0.0012(6) -0.0001(6) -0.0073(7) C34 0.0352(7) 0.0466(9) 0.0304(7) -0.0055(6) -0.0006(6) -0.0061(7) C35 0.0463(9) 0.0473(10) 0.0425(9) -0.0101(7) -0.0008(7) -0.0082(8) C36 0.0570(11) 0.0713(13) 0.0376(9) -0.0015(9) 0.0103(8) -0.0182(10) C37 0.0369(7) 0.0273(7) 0.0312(7) -0.0011(5) 0.0047(6) 0.0010(6) C38 0.0459(9) 0.0335(8) 0.0295(7) 0.0035(6) 0.0040(6) 0.0057(6) C39 0.0406(8) 0.0490(10) 0.0299(7) 0.0053(7) -0.0034(6) 0.0044(7) C40 0.0389(8) 0.0478(9) 0.0308(8) -0.0005(7) -0.0015(6) -0.0048(7) C41 0.0432(8) 0.0318(8) 0.0272(7) -0.0001(6) 0.0007(6) -0.0037(6) C42 0.0584(11) 0.0527(11) 0.0468(10) 0.0207(9) 0.0028(8) 0.0018(9) C43 0.0501(11) 0.0843(15) 0.0497(11) 0.0146(11) -0.0097(8) -0.0225(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mg1 N3 1.9827(13) . ? Mg1 N1 2.0521(12) . ? Mg1 N2 2.0555(12) . ? Mg1 N4 2.1282(13) . ? N1 C2 1.3306(18) . ? N1 C6 1.4375(18) . ? N2 C4 1.3246(18) . ? N2 C18 1.4420(17) . ? N3 C34 1.386(2) . ? N3 C30 1.394(2) . ? N4 C37 1.3390(19) . ? N4 C41 1.340(2) . ? C1 C2 1.5135(19) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C3 1.406(2) . ? C3 C4 1.4144(19) . ? C3 H3 0.9500 . ? C4 C5 1.512(2) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 C7 1.400(2) . ? C6 C11 1.420(2) . ? C7 C8 1.400(2) . ? C7 C12 1.519(2) . ? C8 C9 1.383(3) . ? C8 H8 0.9500 . ? C9 C10 1.378(3) . ? C9 H9 0.9500 . ? C10 C11 1.394(2) . ? C10 H10 0.9500 . ? C11 C15 1.521(3) . ? C12 C14 1.534(2) . ? C12 C13 1.537(2) . ? C12 H12 1.0000 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C17 1.523(3) . ? C15 C16 1.533(3) . ? C15 H15 1.0000 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C19 1.409(2) . ? C18 C23 1.410(2) . ? C19 C20 1.393(2) . ? C19 C24 1.523(2) . ? C20 C21 1.383(2) . ? C20 H20 0.9500 . ? C21 C22 1.378(2) . ? C21 H21 0.9500 . ? C22 C23 1.399(2) . ? C22 H22 0.9500 . ? C23 C27 1.523(2) . ? C24 C26 1.511(3) . ? C24 C25 1.522(3) . ? C24 H24 1.0000 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C29 1.526(2) . ? C27 C28 1.537(2) . ? C27 H27 1.0000 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 C31 1.334(2) . ? C30 H30 0.9500 . ? C31 C35 1.490(2) . ? C31 C32 1.503(2) . ? C32 C33 1.504(2) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C34 1.340(2) . ? C33 C36 1.499(2) . ? C34 H34 0.9500 . ? 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 C38 1.385(2) . ? C37 H37 0.9500 . ? C38 C39 1.389(2) . ? C38 C42 1.509(2) . ? C39 C40 1.393(2) . ? C39 H39 0.9500 . ? C40 C41 1.384(2) . ? C40 C43 1.504(3) . ? C41 H41 0.9500 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 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 N1 122.64(5) . . ? N3 Mg1 N2 124.93(6) . . ? N1 Mg1 N2 93.55(5) . . ? N3 Mg1 N4 104.75(6) . . ? N1 Mg1 N4 107.33(5) . . ? N2 Mg1 N4 101.06(5) . . ? C2 N1 C6 120.51(12) . . ? C2 N1 Mg1 121.33(9) . . ? C6 N1 Mg1 118.06(9) . . ? C4 N2 C18 119.08(11) . . ? C4 N2 Mg1 121.60(9) . . ? C18 N2 Mg1 119.30(9) . . ? C34 N3 C30 112.89(12) . . ? C34 N3 Mg1 119.85(10) . . ? C30 N3 Mg1 126.46(10) . . ? C37 N4 C41 118.05(13) . . ? C37 N4 Mg1 125.11(10) . . ? C41 N4 Mg1 116.83(10) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N1 C2 C3 124.05(13) . . ? N1 C2 C1 120.24(13) . . ? C3 C2 C1 115.71(13) . . ? C2 C3 C4 129.90(13) . . ? C2 C3 H3 115.1 . . ? C4 C3 H3 115.1 . . ? N2 C4 C3 124.11(12) . . ? N2 C4 C5 120.27(12) . . ? C3 C4 C5 115.59(12) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C7 C6 C11 120.98(14) . . ? C7 C6 N1 121.03(13) . . ? C11 C6 N1 117.68(14) . . ? C8 C7 C6 118.52(16) . . ? C8 C7 C12 118.48(15) . . ? C6 C7 C12 122.93(13) . . ? C9 C8 C7 121.08(18) . . ? C9 C8 H8 119.5 . . ? C7 C8 H8 119.5 . . ? C10 C9 C8 119.90(15) . . ? C10 C9 H9 120.1 . . ? C8 C9 H9 120.1 . . ? C9 C10 C11 121.66(17) . . ? C9 C10 H10 119.2 . . ? C11 C10 H10 119.2 . . ? C10 C11 C6 117.85(16) . . ? C10 C11 C15 121.44(15) . . ? C6 C11 C15 120.69(14) . . ? C7 C12 C14 110.46(14) . . ? C7 C12 C13 112.74(14) . . ? C14 C12 C13 109.94(15) . . ? C7 C12 H12 107.8 . . ? C14 C12 H12 107.8 . . ? C13 C12 H12 107.8 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C11 C15 C17 112.23(16) . . ? C11 C15 C16 113.97(16) . . ? C17 C15 C16 109.70(17) . . ? C11 C15 H15 106.8 . . ? C17 C15 H15 106.8 . . ? C16 C15 H15 106.8 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C19 C18 C23 120.26(13) . . ? C19 C18 N2 118.30(12) . . ? C23 C18 N2 121.35(13) . . ? C20 C19 C18 118.70(14) . . ? C20 C19 C24 119.82(14) . . ? C18 C19 C24 121.47(13) . . ? C21 C20 C19 121.31(15) . . ? C21 C20 H20 119.3 . . ? C19 C20 H20 119.3 . . ? C22 C21 C20 119.84(15) . . ? C22 C21 H21 120.1 . . ? C20 C21 H21 120.1 . . ? C21 C22 C23 121.15(14) . . ? C21 C22 H22 119.4 . . ? C23 C22 H22 119.4 . . ? C22 C23 C18 118.69(14) . . ? C22 C23 C27 118.71(13) . . ? C18 C23 C27 122.58(13) . . ? C26 C24 C25 111.48(19) . . ? C26 C24 C19 111.37(14) . . ? C25 C24 C19 111.77(14) . . ? C26 C24 H24 107.3 . . ? C25 C24 H24 107.3 . . ? C19 C24 H24 107.3 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C23 C27 C29 110.61(15) . . ? C23 C27 C28 112.08(14) . . ? C29 C27 C28 109.33(13) . . ? C23 C27 H27 108.2 . . ? C29 C27 H27 108.2 . . ? C28 C27 H27 108.2 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C31 C30 N3 127.09(14) . . ? C31 C30 H30 116.5 . . ? N3 C30 H30 116.5 . . ? C30 C31 C35 122.69(15) . . ? C30 C31 C32 121.05(14) . . ? C35 C31 C32 116.23(14) . . ? C31 C32 C33 110.89(13) . . ? C31 C32 H32A 109.5 . . ? C33 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? C33 C32 H32B 109.5 . . ? H32A C32 H32B 108.0 . . ? C34 C33 C36 122.41(15) . . ? C34 C33 C32 121.16(14) . . ? C36 C33 C32 116.43(15) . . ? C33 C34 N3 126.87(15) . . ? C33 C34 H34 116.6 . . ? N3 C34 H34 116.6 . . ? C31 C35 H35A 109.5 . . ? C31 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C31 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C33 C36 H36A 109.5 . . ? C33 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C33 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? N4 C37 C38 123.19(14) . . ? N4 C37 H37 118.4 . . ? C38 C37 H37 118.4 . . ? C37 C38 C39 117.69(14) . . ? C37 C38 C42 120.12(16) . . ? C39 C38 C42 122.18(15) . . ? C38 C39 C40 120.14(15) . . ? C38 C39 H39 119.9 . . ? C40 C39 H39 119.9 . . ? C41 C40 C39 117.41(15) . . ? C41 C40 C43 119.76(16) . . ? C39 C40 C43 122.81(16) . . ? N4 C41 C40 123.39(14) . . ? N4 C41 H41 118.3 . . ? C40 C41 H41 118.3 . . ? C38 C42 H42A 109.5 . . ? C38 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C38 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C40 C43 H43A 109.5 . . ? C40 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C40 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 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 C2 158.20(11) . . . . ? N2 Mg1 N1 C2 22.07(12) . . . . ? N4 Mg1 N1 C2 -80.68(12) . . . . ? N3 Mg1 N1 C6 -25.45(13) . . . . ? N2 Mg1 N1 C6 -161.58(11) . . . . ? N4 Mg1 N1 C6 95.66(11) . . . . ? N3 Mg1 N2 C4 -154.48(10) . . . . ? N1 Mg1 N2 C4 -19.86(11) . . . . ? N4 Mg1 N2 C4 88.58(11) . . . . ? N3 Mg1 N2 C18 23.63(13) . . . . ? N1 Mg1 N2 C18 158.26(10) . . . . ? N4 Mg1 N2 C18 -93.31(10) . . . . ? N1 Mg1 N3 C34 179.80(11) . . . . ? N2 Mg1 N3 C34 -57.72(14) . . . . ? N4 Mg1 N3 C34 57.49(13) . . . . ? N1 Mg1 N3 C30 10.80(16) . . . . ? N2 Mg1 N3 C30 133.28(12) . . . . ? N4 Mg1 N3 C30 -111.51(13) . . . . ? N3 Mg1 N4 C37 -10.96(13) . . . . ? N1 Mg1 N4 C37 -142.76(11) . . . . ? N2 Mg1 N4 C37 119.94(12) . . . . ? N3 Mg1 N4 C41 169.26(11) . . . . ? N1 Mg1 N4 C41 37.46(12) . . . . ? N2 Mg1 N4 C41 -59.84(11) . . . . ? C6 N1 C2 C3 172.19(14) . . . . ? Mg1 N1 C2 C3 -11.55(19) . . . . ? C6 N1 C2 C1 -6.9(2) . . . . ? Mg1 N1 C2 C1 169.35(11) . . . . ? N1 C2 C3 C4 -10.7(3) . . . . ? C1 C2 C3 C4 168.44(15) . . . . ? C18 N2 C4 C3 -171.18(13) . . . . ? Mg1 N2 C4 C3 6.94(19) . . . . ? C18 N2 C4 C5 6.8(2) . . . . ? Mg1 N2 C4 C5 -175.04(11) . . . . ? C2 C3 C4 N2 13.4(2) . . . . ? C2 C3 C4 C5 -164.72(15) . . . . ? C2 N1 C6 C7 83.83(18) . . . . ? Mg1 N1 C6 C7 -92.55(14) . . . . ? C2 N1 C6 C11 -102.44(16) . . . . ? Mg1 N1 C6 C11 81.19(14) . . . . ? C11 C6 C7 C8 -1.1(2) . . . . ? N1 C6 C7 C8 172.41(14) . . . . ? C11 C6 C7 C12 -178.21(14) . . . . ? N1 C6 C7 C12 -4.7(2) . . . . ? C6 C7 C8 C9 0.7(3) . . . . ? C12 C7 C8 C9 177.96(16) . . . . ? C7 C8 C9 C10 0.1(3) . . . . ? C8 C9 C10 C11 -0.6(3) . . . . ? C9 C10 C11 C6 0.2(2) . . . . ? C9 C10 C11 C15 -178.12(16) . . . . ? C7 C6 C11 C10 0.7(2) . . . . ? N1 C6 C11 C10 -173.06(14) . . . . ? C7 C6 C11 C15 178.98(15) . . . . ? N1 C6 C11 C15 5.2(2) . . . . ? C8 C7 C12 C14 -69.11(19) . . . . ? C6 C7 C12 C14 107.98(17) . . . . ? C8 C7 C12 C13 54.3(2) . . . . ? C6 C7 C12 C13 -128.57(17) . . . . ? C10 C11 C15 C17 -104.71(19) . . . . ? C6 C11 C15 C17 77.04(19) . . . . ? C10 C11 C15 C16 20.8(2) . . . . ? C6 C11 C15 C16 -157.49(15) . . . . ? C4 N2 C18 C19 96.28(16) . . . . ? Mg1 N2 C18 C19 -81.88(14) . . . . ? C4 N2 C18 C23 -87.18(17) . . . . ? Mg1 N2 C18 C23 94.66(14) . . . . ? C23 C18 C19 C20 2.7(2) . . . . ? N2 C18 C19 C20 179.31(13) . . . . ? C23 C18 C19 C24 -178.47(13) . . . . ? N2 C18 C19 C24 -1.9(2) . . . . ? C18 C19 C20 C21 -1.9(2) . . . . ? C24 C19 C20 C21 179.32(15) . . . . ? C19 C20 C21 C22 -0.1(2) . . . . ? C20 C21 C22 C23 1.2(2) . . . . ? C21 C22 C23 C18 -0.3(2) . . . . ? C21 C22 C23 C27 -179.12(15) . . . . ? C19 C18 C23 C22 -1.7(2) . . . . ? N2 C18 C23 C22 -178.13(13) . . . . ? C19 C18 C23 C27 177.09(14) . . . . ? N2 C18 C23 C27 0.6(2) . . . . ? C20 C19 C24 C26 67.6(2) . . . . ? C18 C19 C24 C26 -111.23(19) . . . . ? C20 C19 C24 C25 -57.9(2) . . . . ? C18 C19 C24 C25 123.35(19) . . . . ? C22 C23 C27 C29 64.59(19) . . . . ? C18 C23 C27 C29 -114.16(15) . . . . ? C22 C23 C27 C28 -57.7(2) . . . . ? C18 C23 C27 C28 123.55(16) . . . . ? C34 N3 C30 C31 -0.1(2) . . . . ? Mg1 N3 C30 C31 169.57(13) . . . . ? N3 C30 C31 C35 -179.59(16) . . . . ? N3 C30 C31 C32 -1.6(3) . . . . ? C30 C31 C32 C33 1.3(2) . . . . ? C35 C31 C32 C33 179.44(15) . . . . ? C31 C32 C33 C34 0.5(2) . . . . ? C31 C32 C33 C36 -178.93(16) . . . . ? C36 C33 C34 N3 177.01(18) . . . . ? C32 C33 C34 N3 -2.3(3) . . . . ? C30 N3 C34 C33 2.1(2) . . . . ? Mg1 N3 C34 C33 -168.27(14) . . . . ? C41 N4 C37 C38 1.8(2) . . . . ? Mg1 N4 C37 C38 -177.94(11) . . . . ? N4 C37 C38 C39 -2.9(2) . . . . ? N4 C37 C38 C42 175.89(15) . . . . ? C37 C38 C39 C40 0.8(2) . . . . ? C42 C38 C39 C40 -178.04(17) . . . . ? C38 C39 C40 C41 2.2(2) . . . . ? C38 C39 C40 C43 -176.25(18) . . . . ? C37 N4 C41 C40 1.5(2) . . . . ? Mg1 N4 C41 C40 -178.70(12) . . . . ? C39 C40 C41 N4 -3.5(2) . . . . ? C43 C40 C41 N4 175.05(17) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.52 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.351 _refine_diff_density_min -0.223 _refine_diff_density_rms 0.035 #===end data_10-k10msh20 _database_code_depnum_ccdc_archive 'CCDC 831739' #TrackingRef '- bigcif.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C47 H56 Mg N4' _chemical_formula_weight 701.27 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 0.0486 0.0363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2/a loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y, -z' '-x, -y, -z' 'x-1/2, -y, z' _cell_length_a 18.3245(2) _cell_length_b 10.8579(1) _cell_length_c 22.0748(3) _cell_angle_alpha 90.00 _cell_angle_beta 108.966(1) _cell_angle_gamma 90.00 _cell_volume 4153.68(8) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 72928 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 27.485 _exptl_crystal_description blcok _exptl_crystal_colour orange _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.121 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1512 _exptl_absorpt_coefficient_mu 0.079 # Absorption correction _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.893 _exptl_absorpt_correction_T_max 0.985 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_measurement_device_type '95mm CCD camera on \k-goniostat' _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 61721 _diffrn_reflns_av_R_equivalents 0.0599 _diffrn_reflns_av_sigmaI/netI 0.0405 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 3.98 _diffrn_reflns_theta_max 27.48 _reflns_number_total 9439 _reflns_number_gt 6789 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Bruker AXS BV 1997-2004)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo & Scalepack (Otwinowski, Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick 1990)' _computing_structure_refinement 'SHELXL-97/2 (Sheldrick 1997)' _computing_molecular_graphics 'ORTEX (P.McArdle 1995)' _computing_publication_material 'SHELXL-97/2 (Sheldrick 1997)' _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^)+(0.0533P)^2^+1.9860P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0034(7) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 9439 _refine_ls_number_parameters 478 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0812 _refine_ls_R_factor_gt 0.0523 _refine_ls_wR_factor_ref 0.1403 _refine_ls_wR_factor_gt 0.1217 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.039 _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 -0.05700(3) 0.25224(5) 0.26816(3) 0.02972(14) Uani 1 1 d . . . N1 N -0.05235(8) 0.16124(13) 0.34961(6) 0.0317(3) Uani 1 1 d . . . N2 N -0.00297(8) 0.11937(12) 0.23349(6) 0.0303(3) Uani 1 1 d . . . N3 N -0.02904(9) 0.42897(14) 0.26522(8) 0.0430(4) Uani 1 1 d . . . N4 N -0.17582(8) 0.24257(13) 0.21185(7) 0.0330(3) Uani 1 1 d . . . C1 C -0.05702(13) -0.03242(18) 0.40644(9) 0.0455(5) Uani 1 1 d . . . H1A H -0.0688 0.0247 0.4364 0.068 Uiso 0.50 1 calc PR . . H1B H -0.0095 -0.0775 0.4286 0.068 Uiso 0.50 1 calc PR . . H1C H -0.0997 -0.0908 0.3901 0.068 Uiso 0.50 1 calc PR . . H1D H -0.0499 -0.1205 0.4004 0.068 Uiso 0.50 1 calc PR . . H1E H -0.1091 -0.0183 0.4081 0.068 Uiso 0.50 1 calc PR . . H1F H -0.0190 -0.0049 0.4466 0.068 Uiso 0.50 1 calc PR . . C2 C -0.04636(10) 0.03906(16) 0.35128(8) 0.0333(4) Uani 1 1 d . . . C3 C -0.02906(10) -0.03215(16) 0.30430(8) 0.0348(4) Uani 1 1 d . . . H3 H -0.0367 -0.1182 0.3071 0.042 Uiso 1 1 calc R . . C4 C -0.00235(9) 0.00342(15) 0.25394(8) 0.0318(4) Uani 1 1 d . . . C5 C 0.02935(11) -0.09881(16) 0.22308(9) 0.0401(4) Uani 1 1 d . . . H5A H 0.0460 -0.0646 0.1886 0.060 Uiso 0.50 1 calc PR . . H5B H -0.0109 -0.1607 0.2054 0.060 Uiso 0.50 1 calc PR . . H5C H 0.0735 -0.1373 0.2553 0.060 Uiso 0.50 1 calc PR . . H5D H 0.0264 -0.1771 0.2442 0.060 Uiso 0.50 1 calc PR . . H5E H 0.0833 -0.0810 0.2274 0.060 Uiso 0.50 1 calc PR . . H5F H -0.0011 -0.1045 0.1776 0.060 Uiso 0.50 1 calc PR . . C6 C -0.05232(10) 0.22533(15) 0.40697(8) 0.0341(4) Uani 1 1 d . . . C7 C 0.01944(11) 0.26690(17) 0.44844(8) 0.0396(4) Uani 1 1 d . . . C8 C 0.02091(12) 0.32770(19) 0.50446(9) 0.0482(5) Uani 1 1 d . . . H8 H 0.0688 0.3556 0.5332 0.058 Uiso 1 1 calc R . . C9 C -0.04548(13) 0.34804(19) 0.51901(10) 0.0497(5) Uani 1 1 d . . . H9 H -0.0431 0.3873 0.5581 0.060 Uiso 1 1 calc R . . C10 C -0.11586(12) 0.31132(19) 0.47667(9) 0.0454(5) Uani 1 1 d . . . H10 H -0.1617 0.3280 0.4865 0.054 Uiso 1 1 calc R . . C11 C -0.12094(11) 0.25016(17) 0.41980(8) 0.0375(4) Uani 1 1 d . . . C12 C 0.09370(11) 0.2465(2) 0.43326(9) 0.0463(5) Uani 1 1 d . . . H12 H 0.0786 0.2245 0.3868 0.056 Uiso 1 1 calc R . . C13 C 0.13924(16) 0.1388(3) 0.47053(16) 0.0813(8) Uani 1 1 d . . . H13A H 0.1551 0.1569 0.5165 0.122 Uiso 1 1 calc R . . H13B H 0.1851 0.1251 0.4578 0.122 Uiso 1 1 calc R . . H13C H 0.1070 0.0647 0.4614 0.122 Uiso 1 1 calc R . . C14 C 0.14334(16) 0.3609(3) 0.44269(18) 0.0892(9) Uani 1 1 d . . . H14A H 0.1146 0.4263 0.4143 0.134 Uiso 1 1 calc R . . H14B H 0.1904 0.3422 0.4325 0.134 Uiso 1 1 calc R . . H14C H 0.1572 0.3881 0.4873 0.134 Uiso 1 1 calc R . . C15 C -0.19989(11) 0.21643(19) 0.37342(9) 0.0431(4) Uani 1 1 d . . . H15 H -0.1919 0.1606 0.3401 0.052 Uiso 1 1 calc R . . C16 C -0.25047(13) 0.1482(2) 0.40600(11) 0.0563(6) Uani 1 1 d . . . H16A H -0.2229 0.0753 0.4283 0.084 Uiso 1 1 calc R . . H16B H -0.2987 0.1226 0.3736 0.084 Uiso 1 1 calc R . . H16C H -0.2620 0.2030 0.4370 0.084 Uiso 1 1 calc R . . C17 C -0.24177(13) 0.3321(2) 0.33945(11) 0.0607(6) Uani 1 1 d . . . H17A H -0.2534 0.3860 0.3707 0.091 Uiso 1 1 calc R . . H17B H -0.2899 0.3082 0.3064 0.091 Uiso 1 1 calc R . . H17C H -0.2087 0.3760 0.3196 0.091 Uiso 1 1 calc R . . C18 C 0.03256(9) 0.14550(15) 0.18546(8) 0.0319(4) Uani 1 1 d . . . C19 C 0.10753(10) 0.19541(16) 0.20462(9) 0.0372(4) Uani 1 1 d . . . C20 C 0.14088(10) 0.22206(16) 0.15763(10) 0.0399(4) Uani 1 1 d . . . H20 H 0.1915 0.2554 0.1700 0.048 Uiso 1 1 calc R . . C21 C 0.10211(11) 0.20119(18) 0.09373(9) 0.0424(4) Uani 1 1 d . . . H21 H 0.1264 0.2177 0.0626 0.051 Uiso 1 1 calc R . . C22 C 0.02762(10) 0.15607(18) 0.07511(9) 0.0401(4) Uani 1 1 d . . . H22 H 0.0007 0.1434 0.0309 0.048 Uiso 1 1 calc R . . C23 C -0.00894(10) 0.12873(16) 0.11991(8) 0.0346(4) Uani 1 1 d . . . C24 C 0.15277(12) 0.2202(2) 0.27445(10) 0.0518(5) Uani 1 1 d . . . H24 H 0.1156 0.2198 0.2991 0.062 Uiso 1 1 calc R . . C25 C 0.19265(15) 0.3454(2) 0.28412(14) 0.0753(8) Uani 1 1 d . . . H25A H 0.2353 0.3436 0.2665 0.113 Uiso 1 1 calc R . . H25B H 0.2128 0.3643 0.3300 0.113 Uiso 1 1 calc R . . H25C H 0.1555 0.4089 0.2621 0.113 Uiso 1 1 calc R . . C26 C 0.2116(2) 0.1215(3) 0.30169(13) 0.1068(13) Uani 1 1 d . . . H26A H 0.2365 0.1359 0.3476 0.160 Uiso 1 1 calc R . . H26B H 0.2506 0.1233 0.2800 0.160 Uiso 1 1 calc R . . H26C H 0.1862 0.0409 0.2952 0.160 Uiso 1 1 calc R . . C27 C -0.09336(10) 0.09078(18) 0.09602(8) 0.0385(4) Uani 1 1 d . . . H27 H -0.1072 0.0591 0.1334 0.046 Uiso 1 1 calc R . . C28 C -0.14382(11) 0.2035(2) 0.06932(10) 0.0492(5) Uani 1 1 d . . . H28A H -0.1316 0.2690 0.1016 0.074 Uiso 1 1 calc R . . H28B H -0.1983 0.1808 0.0585 0.074 Uiso 1 1 calc R . . H28C H -0.1338 0.2327 0.0307 0.074 Uiso 1 1 calc R . . C29 C -0.11079(12) -0.0104(2) 0.04530(10) 0.0490(5) Uani 1 1 d . . . H29A H -0.0976 0.0186 0.0081 0.073 Uiso 1 1 calc R . . H29B H -0.1658 -0.0310 0.0320 0.073 Uiso 1 1 calc R . . H29C H -0.0802 -0.0837 0.0632 0.073 Uiso 1 1 calc R . . C30 C -0.01220(12) 0.48189(19) 0.21003(11) 0.0515(5) Uani 1 1 d . . . H30A H -0.0051 0.4145 0.1822 0.062 Uiso 1 1 calc R . . H30B H 0.0366 0.5292 0.2253 0.062 Uiso 1 1 calc R . . C31 C -0.07596(12) 0.5652(2) 0.17172(12) 0.0568(6) Uani 1 1 d . . . C32 C -0.10248(11) 0.64973(19) 0.20913(15) 0.0624(7) Uani 1 1 d . . . C33 C -0.07941(13) 0.62980(19) 0.27684(14) 0.0621(6) Uani 1 1 d . . . H33 H -0.0826 0.6937 0.3053 0.075 Uiso 1 1 calc R . . C34 C -0.05260(12) 0.51549(18) 0.29911(11) 0.0504(5) Uani 1 1 d . . . H34 H -0.0503 0.4951 0.3415 0.060 Uiso 1 1 calc R . . C35 C -0.10635(14) 0.5643(3) 0.10578(14) 0.0762(8) Uani 1 1 d . . . H35 H -0.0903 0.5032 0.0820 0.091 Uiso 1 1 calc R . . C36 C -0.16029(16) 0.6523(4) 0.07391(18) 0.1029(14) Uani 1 1 d . . . H36 H -0.1806 0.6528 0.0285 0.123 Uiso 1 1 calc R . . C37 C -0.18373(15) 0.7387(3) 0.1094(2) 0.1080(15) Uani 1 1 d . . . H37 H -0.2200 0.7998 0.0878 0.130 Uiso 1 1 calc R . . C38 C -0.15599(14) 0.7391(2) 0.1757(2) 0.0860(10) Uani 1 1 d . . . H38 H -0.1732 0.8001 0.1987 0.103 Uiso 1 1 calc R . . C39 C -0.21487(10) 0.34178(16) 0.18541(8) 0.0343(4) Uani 1 1 d . . . H39 H -0.1888 0.4188 0.1929 0.041 Uiso 1 1 calc R . . C40 C -0.29331(10) 0.33987(16) 0.14656(8) 0.0334(4) Uani 1 1 d . . . C41 C -0.33182(9) 0.22504(16) 0.13600(8) 0.0324(4) Uani 1 1 d . . . C42 C -0.28911(10) 0.11958(16) 0.16451(8) 0.0370(4) Uani 1 1 d . . . H42 H -0.3129 0.0408 0.1583 0.044 Uiso 1 1 calc R . . C43 C -0.21374(10) 0.13170(16) 0.20094(8) 0.0359(4) Uani 1 1 d . . . H43 H -0.1860 0.0598 0.2197 0.043 Uiso 1 1 calc R . . C44 C -0.33292(11) 0.44830(18) 0.11927(9) 0.0430(4) Uani 1 1 d . . . H44 H -0.3067 0.5251 0.1258 0.052 Uiso 1 1 calc R . . C45 C -0.40935(12) 0.4420(2) 0.08327(10) 0.0507(5) Uani 1 1 d . . . H45 H -0.4363 0.5149 0.0651 0.061 Uiso 1 1 calc R . . C46 C -0.44806(11) 0.3284(2) 0.07300(9) 0.0469(5) Uani 1 1 d . . . H46 H -0.5012 0.3255 0.0482 0.056 Uiso 1 1 calc R . . C47 C -0.41064(10) 0.22174(19) 0.09810(9) 0.0407(4) Uani 1 1 d . . . H47 H -0.4375 0.1455 0.0901 0.049 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 0.0313(3) 0.0265(3) 0.0311(3) 0.0009(2) 0.0099(2) -0.0003(2) N1 0.0354(8) 0.0301(7) 0.0301(7) -0.0011(6) 0.0115(6) 0.0007(6) N2 0.0310(7) 0.0289(7) 0.0321(7) 0.0004(6) 0.0117(6) -0.0017(5) N3 0.0408(9) 0.0312(8) 0.0553(10) 0.0026(7) 0.0133(7) -0.0026(6) N4 0.0329(7) 0.0323(7) 0.0343(7) 0.0006(6) 0.0117(6) -0.0012(6) C1 0.0660(13) 0.0363(10) 0.0368(10) 0.0039(8) 0.0204(9) -0.0014(9) C2 0.0341(9) 0.0323(9) 0.0325(9) 0.0033(7) 0.0095(7) -0.0011(7) C3 0.0411(10) 0.0262(8) 0.0378(9) 0.0006(7) 0.0139(7) -0.0022(7) C4 0.0304(8) 0.0288(8) 0.0355(9) -0.0025(7) 0.0099(7) -0.0016(6) C5 0.0456(10) 0.0312(9) 0.0490(11) -0.0016(8) 0.0227(8) 0.0014(8) C6 0.0437(10) 0.0304(9) 0.0283(8) 0.0011(7) 0.0119(7) -0.0001(7) C7 0.0436(10) 0.0388(10) 0.0340(9) 0.0012(8) 0.0093(7) -0.0024(8) C8 0.0543(12) 0.0492(12) 0.0366(10) -0.0058(9) 0.0085(9) -0.0089(9) C9 0.0661(13) 0.0462(11) 0.0382(10) -0.0122(9) 0.0187(9) -0.0072(10) C10 0.0541(12) 0.0448(11) 0.0417(10) -0.0078(8) 0.0218(9) -0.0003(9) C11 0.0440(10) 0.0353(9) 0.0350(9) -0.0027(7) 0.0155(7) -0.0007(8) C12 0.0394(10) 0.0605(13) 0.0370(10) -0.0005(9) 0.0096(8) -0.0049(9) C13 0.0655(16) 0.0772(18) 0.115(2) 0.0253(17) 0.0489(16) 0.0222(14) C14 0.0604(16) 0.0734(19) 0.144(3) 0.0012(19) 0.0472(18) -0.0111(14) C15 0.0422(10) 0.0504(11) 0.0403(10) -0.0080(8) 0.0181(8) 0.0002(8) C16 0.0538(13) 0.0648(14) 0.0569(13) -0.0121(11) 0.0272(10) -0.0119(11) C17 0.0555(13) 0.0725(16) 0.0523(13) 0.0033(11) 0.0150(10) 0.0168(12) C18 0.0346(9) 0.0281(8) 0.0364(9) 0.0011(7) 0.0161(7) 0.0008(7) C19 0.0369(9) 0.0342(9) 0.0429(10) -0.0040(8) 0.0162(8) -0.0030(7) C20 0.0351(9) 0.0339(9) 0.0558(11) 0.0014(8) 0.0218(8) -0.0027(7) C21 0.0443(10) 0.0434(11) 0.0469(11) 0.0084(8) 0.0251(8) 0.0018(8) C22 0.0403(10) 0.0461(11) 0.0363(9) 0.0068(8) 0.0159(8) 0.0025(8) C23 0.0341(9) 0.0333(9) 0.0379(9) 0.0038(7) 0.0141(7) 0.0025(7) C24 0.0429(11) 0.0683(14) 0.0478(11) -0.0165(10) 0.0200(9) -0.0219(10) C25 0.0647(15) 0.0498(14) 0.0852(18) -0.0194(13) -0.0118(13) 0.0010(11) C26 0.168(3) 0.0500(15) 0.0527(15) 0.0090(12) -0.0320(18) -0.0041(18) C27 0.0356(9) 0.0496(11) 0.0319(9) 0.0031(8) 0.0129(7) -0.0011(8) C28 0.0410(11) 0.0638(13) 0.0431(11) 0.0056(10) 0.0142(8) 0.0081(9) C29 0.0462(11) 0.0569(13) 0.0451(11) -0.0051(9) 0.0167(9) -0.0096(9) C30 0.0428(11) 0.0387(11) 0.0762(15) 0.0155(10) 0.0239(10) 0.0008(8) C31 0.0358(10) 0.0478(12) 0.0872(17) 0.0290(12) 0.0207(10) -0.0051(9) C32 0.0325(10) 0.0317(10) 0.122(2) 0.0204(12) 0.0233(12) -0.0033(8) C33 0.0525(13) 0.0294(10) 0.103(2) -0.0054(11) 0.0236(13) -0.0061(9) C34 0.0462(11) 0.0335(10) 0.0671(14) -0.0095(9) 0.0126(10) -0.0091(8) C35 0.0489(13) 0.093(2) 0.0885(19) 0.0467(16) 0.0242(13) -0.0081(13) C36 0.0437(15) 0.145(3) 0.118(3) 0.084(3) 0.0235(16) -0.0017(18) C37 0.0320(13) 0.108(3) 0.182(4) 0.099(3) 0.0317(19) 0.0130(14) C38 0.0389(12) 0.0519(14) 0.168(3) 0.0478(18) 0.0344(16) 0.0083(10) C39 0.0336(9) 0.0320(9) 0.0381(9) -0.0001(7) 0.0126(7) -0.0025(7) C40 0.0325(9) 0.0353(9) 0.0344(9) -0.0014(7) 0.0137(7) 0.0000(7) C41 0.0312(8) 0.0394(9) 0.0296(8) -0.0027(7) 0.0139(7) -0.0024(7) C42 0.0400(10) 0.0327(9) 0.0405(10) -0.0015(7) 0.0162(8) -0.0076(7) C43 0.0378(9) 0.0330(9) 0.0381(9) 0.0027(7) 0.0138(7) 0.0007(7) C44 0.0411(10) 0.0355(10) 0.0496(11) 0.0001(8) 0.0110(8) 0.0038(8) C45 0.0434(11) 0.0474(12) 0.0547(12) -0.0014(9) 0.0068(9) 0.0128(9) C46 0.0331(10) 0.0602(13) 0.0440(11) -0.0085(9) 0.0080(8) 0.0051(9) C47 0.0344(9) 0.0501(11) 0.0396(10) -0.0083(8) 0.0148(8) -0.0061(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 1.9926(16) . ? Mg1 N1 2.0289(15) . ? Mg1 N2 2.0347(15) . ? Mg1 N4 2.1301(15) . ? N1 C2 1.331(2) . ? N1 C6 1.445(2) . ? N2 C4 1.336(2) . ? N2 C18 1.441(2) . ? N3 C34 1.356(3) . ? N3 C30 1.468(3) . ? N4 C39 1.320(2) . ? N4 C43 1.372(2) . ? C1 C2 1.509(2) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C1 H1D 0.9800 . ? C1 H1E 0.9800 . ? C1 H1F 0.9800 . ? C2 C3 1.410(2) . ? C3 C4 1.406(2) . ? C3 H3 0.9500 . ? C4 C5 1.514(2) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C5 H5D 0.9800 . ? C5 H5E 0.9800 . ? C5 H5F 0.9800 . ? C6 C11 1.402(3) . ? C6 C7 1.410(2) . ? C7 C8 1.394(3) . ? C7 C12 1.520(3) . ? C8 C9 1.373(3) . ? C8 H8 0.9500 . ? C9 C10 1.383(3) . ? C9 H9 0.9500 . ? C10 C11 1.396(3) . ? C10 H10 0.9500 . ? C11 C15 1.521(3) . ? C12 C14 1.513(3) . ? C12 C13 1.515(3) . ? C12 H12 1.0000 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C17 1.535(3) . ? C15 C16 1.536(3) . ? C15 H15 1.0000 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C19 1.408(2) . ? C18 C23 1.411(2) . ? C19 C20 1.395(3) . ? C19 C24 1.518(3) . ? C20 C21 1.376(3) . ? C20 H20 0.9500 . ? C21 C22 1.381(3) . ? C21 H21 0.9500 . ? C22 C23 1.395(2) . ? C22 H22 0.9500 . ? C23 C27 1.520(2) . ? C24 C26 1.500(4) . ? C24 C25 1.526(3) . ? C24 H24 1.0000 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C29 1.526(3) . ? C27 C28 1.531(3) . ? C27 H27 1.0000 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 C31 1.502(3) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 C35 1.379(4) . ? C31 C32 1.422(4) . ? C32 C38 1.406(3) . ? C32 C33 1.431(4) . ? C33 C34 1.366(3) . ? C33 H33 0.9500 . ? C34 H34 0.9500 . ? C35 C36 1.390(4) . ? C35 H35 0.9500 . ? C36 C37 1.377(6) . ? C36 H36 0.9500 . ? C37 C38 1.384(5) . ? C37 H37 0.9500 . ? C38 H38 0.9500 . ? C39 C40 1.415(2) . ? C39 H39 0.9500 . ? C40 C44 1.411(3) . ? C40 C41 1.414(2) . ? C41 C42 1.414(2) . ? C41 C47 1.415(2) . ? C42 C43 1.360(2) . ? C42 H42 0.9500 . ? C43 H43 0.9500 . ? C44 C45 1.369(3) . ? C44 H44 0.9500 . ? C45 C46 1.404(3) . ? C45 H45 0.9500 . ? C46 C47 1.368(3) . ? C46 H46 0.9500 . ? C47 H47 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Mg1 N1 124.10(7) . . ? N3 Mg1 N2 120.59(7) . . ? N1 Mg1 N2 95.89(6) . . ? N3 Mg1 N4 104.68(6) . . ? N1 Mg1 N4 103.52(6) . . ? N2 Mg1 N4 106.00(6) . . ? C2 N1 C6 118.64(14) . . ? C2 N1 Mg1 119.30(11) . . ? C6 N1 Mg1 122.01(11) . . ? C4 N2 C18 118.53(14) . . ? C4 N2 Mg1 119.52(11) . . ? C18 N2 Mg1 121.90(10) . . ? C34 N3 C30 112.17(17) . . ? C34 N3 Mg1 121.19(13) . . ? C30 N3 Mg1 121.98(13) . . ? C39 N4 C43 117.89(15) . . ? C39 N4 Mg1 121.49(12) . . ? C43 N4 Mg1 120.61(11) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C2 C1 H1D 109.5 . . ? H1A C1 H1D 141.1 . . ? H1B C1 H1D 56.3 . . ? H1C C1 H1D 56.3 . . ? C2 C1 H1E 109.5 . . ? H1A C1 H1E 56.3 . . ? H1B C1 H1E 141.1 . . ? H1C C1 H1E 56.3 . . ? H1D C1 H1E 109.5 . . ? C2 C1 H1F 109.5 . . ? H1A C1 H1F 56.3 . . ? H1B C1 H1F 56.3 . . ? H1C C1 H1F 141.1 . . ? H1D C1 H1F 109.5 . . ? H1E C1 H1F 109.5 . . ? N1 C2 C3 124.23(15) . . ? N1 C2 C1 120.26(15) . . ? C3 C2 C1 115.50(15) . . ? C4 C3 C2 130.55(16) . . ? C4 C3 H3 114.7 . . ? C2 C3 H3 114.7 . . ? N2 C4 C3 123.97(15) . . ? N2 C4 C5 120.09(15) . . ? C3 C4 C5 115.94(15) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C4 C5 H5D 109.5 . . ? H5A C5 H5D 141.1 . . ? H5B C5 H5D 56.3 . . ? H5C C5 H5D 56.3 . . ? C4 C5 H5E 109.5 . . ? H5A C5 H5E 56.3 . . ? H5B C5 H5E 141.1 . . ? H5C C5 H5E 56.3 . . ? H5D C5 H5E 109.5 . . ? C4 C5 H5F 109.5 . . ? H5A C5 H5F 56.3 . . ? H5B C5 H5F 56.3 . . ? H5C C5 H5F 141.1 . . ? H5D C5 H5F 109.5 . . ? H5E C5 H5F 109.5 . . ? C11 C6 C7 121.05(16) . . ? C11 C6 N1 121.65(15) . . ? C7 C6 N1 117.24(15) . . ? C8 C7 C6 118.19(17) . . ? C8 C7 C12 120.26(17) . . ? C6 C7 C12 121.55(16) . . ? C9 C8 C7 121.35(18) . . ? C9 C8 H8 119.3 . . ? C7 C8 H8 119.3 . . ? C8 C9 C10 119.88(18) . . ? C8 C9 H9 120.1 . . ? C10 C9 H9 120.1 . . ? C9 C10 C11 121.32(18) . . ? C9 C10 H10 119.3 . . ? C11 C10 H10 119.3 . . ? C10 C11 C6 118.10(17) . . ? C10 C11 C15 119.38(16) . . ? C6 C11 C15 122.50(15) . . ? C14 C12 C13 111.0(2) . . ? C14 C12 C7 113.06(19) . . ? C13 C12 C7 111.54(17) . . ? C14 C12 H12 106.9 . . ? C13 C12 H12 106.9 . . ? C7 C12 H12 106.9 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C11 C15 C17 110.31(17) . . ? C11 C15 C16 112.82(16) . . ? C17 C15 C16 109.99(17) . . ? C11 C15 H15 107.9 . . ? C17 C15 H15 107.9 . . ? C16 C15 H15 107.9 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C19 C18 C23 120.39(15) . . ? C19 C18 N2 119.00(15) . . ? C23 C18 N2 120.48(14) . . ? C20 C19 C18 118.50(17) . . ? C20 C19 C24 119.46(16) . . ? C18 C19 C24 122.05(16) . . ? C21 C20 C19 121.54(17) . . ? C21 C20 H20 119.2 . . ? C19 C20 H20 119.2 . . ? C20 C21 C22 119.62(17) . . ? C20 C21 H21 120.2 . . ? C22 C21 H21 120.2 . . ? C21 C22 C23 121.37(17) . . ? C21 C22 H22 119.3 . . ? C23 C22 H22 119.3 . . ? C22 C23 C18 118.47(16) . . ? C22 C23 C27 118.74(16) . . ? C18 C23 C27 122.65(15) . . ? C26 C24 C19 111.39(19) . . ? C26 C24 C25 109.3(2) . . ? C19 C24 C25 112.24(19) . . ? C26 C24 H24 107.9 . . ? C19 C24 H24 107.9 . . ? C25 C24 H24 107.9 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C23 C27 C29 113.35(15) . . ? C23 C27 C28 109.64(16) . . ? C29 C27 C28 109.66(16) . . ? C23 C27 H27 108.0 . . ? C29 C27 H27 108.0 . . ? C28 C27 H27 108.0 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? N3 C30 C31 111.60(17) . . ? N3 C30 H30A 109.3 . . ? C31 C30 H30A 109.3 . . ? N3 C30 H30B 109.3 . . ? C31 C30 H30B 109.3 . . ? H30A C30 H30B 108.0 . . ? C35 C31 C32 121.4(2) . . ? C35 C31 C30 124.3(2) . . ? C32 C31 C30 114.3(2) . . ? C38 C32 C31 116.9(3) . . ? C38 C32 C33 124.8(3) . . ? C31 C32 C33 117.91(19) . . ? C34 C33 C32 117.6(2) . . ? C34 C33 H33 121.2 . . ? C32 C33 H33 121.2 . . ? N3 C34 C33 124.9(2) . . ? N3 C34 H34 117.5 . . ? C33 C34 H34 117.5 . . ? C31 C35 C36 120.4(3) . . ? C31 C35 H35 119.8 . . ? C36 C35 H35 119.8 . . ? C37 C36 C35 118.8(3) . . ? C37 C36 H36 120.6 . . ? C35 C36 H36 120.6 . . ? C36 C37 C38 121.9(3) . . ? C36 C37 H37 119.1 . . ? C38 C37 H37 119.1 . . ? C37 C38 C32 120.4(3) . . ? C37 C38 H38 119.8 . . ? C32 C38 H38 119.8 . . ? N4 C39 C40 123.66(16) . . ? N4 C39 H39 118.2 . . ? C40 C39 H39 118.2 . . ? C44 C40 C41 120.36(16) . . ? C44 C40 C39 121.80(16) . . ? C41 C40 C39 117.85(16) . . ? C42 C41 C40 117.79(15) . . ? C42 C41 C47 123.61(16) . . ? C40 C41 C47 118.59(16) . . ? C43 C42 C41 119.58(16) . . ? C43 C42 H42 120.2 . . ? C41 C42 H42 120.2 . . ? C42 C43 N4 123.23(16) . . ? C42 C43 H43 118.4 . . ? N4 C43 H43 118.4 . . ? C45 C44 C40 119.56(18) . . ? C45 C44 H44 120.2 . . ? C40 C44 H44 120.2 . . ? C44 C45 C46 120.36(19) . . ? C44 C45 H45 119.8 . . ? C46 C45 H45 119.8 . . ? C47 C46 C45 121.19(18) . . ? C47 C46 H46 119.4 . . ? C45 C46 H46 119.4 . . ? C46 C47 C41 119.94(18) . . ? C46 C47 H47 120.0 . . ? C41 C47 H47 120.0 . . ? 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 C2 -157.44(12) . . . . ? N2 Mg1 N1 C2 -24.00(13) . . . . ? N4 Mg1 N1 C2 84.05(13) . . . . ? N3 Mg1 N1 C6 20.12(15) . . . . ? N2 Mg1 N1 C6 153.56(12) . . . . ? N4 Mg1 N1 C6 -98.40(13) . . . . ? N3 Mg1 N2 C4 157.79(12) . . . . ? N1 Mg1 N2 C4 22.09(13) . . . . ? N4 Mg1 N2 C4 -83.81(13) . . . . ? N3 Mg1 N2 C18 -24.52(15) . . . . ? N1 Mg1 N2 C18 -160.21(12) . . . . ? N4 Mg1 N2 C18 93.89(13) . . . . ? N1 Mg1 N3 C34 -43.65(18) . . . . ? N2 Mg1 N3 C34 -166.61(14) . . . . ? N4 Mg1 N3 C34 74.33(16) . . . . ? N1 Mg1 N3 C30 162.45(13) . . . . ? N2 Mg1 N3 C30 39.49(16) . . . . ? N4 Mg1 N3 C30 -79.58(15) . . . . ? N3 Mg1 N4 C39 -1.67(15) . . . . ? N1 Mg1 N4 C39 129.55(13) . . . . ? N2 Mg1 N4 C39 -130.16(13) . . . . ? N3 Mg1 N4 C43 177.00(13) . . . . ? N1 Mg1 N4 C43 -51.78(14) . . . . ? N2 Mg1 N4 C43 48.51(14) . . . . ? C6 N1 C2 C3 -165.71(16) . . . . ? Mg1 N1 C2 C3 11.9(2) . . . . ? C6 N1 C2 C1 13.3(2) . . . . ? Mg1 N1 C2 C1 -169.07(13) . . . . ? N1 C2 C3 C4 11.9(3) . . . . ? C1 C2 C3 C4 -167.11(18) . . . . ? C18 N2 C4 C3 174.33(16) . . . . ? Mg1 N2 C4 C3 -7.9(2) . . . . ? C18 N2 C4 C5 -4.9(2) . . . . ? Mg1 N2 C4 C5 172.89(12) . . . . ? C2 C3 C4 N2 -14.3(3) . . . . ? C2 C3 C4 C5 164.95(18) . . . . ? C2 N1 C6 C11 -90.4(2) . . . . ? Mg1 N1 C6 C11 91.98(18) . . . . ? C2 N1 C6 C7 92.25(19) . . . . ? Mg1 N1 C6 C7 -85.32(17) . . . . ? C11 C6 C7 C8 3.4(3) . . . . ? N1 C6 C7 C8 -179.25(16) . . . . ? C11 C6 C7 C12 -176.68(17) . . . . ? N1 C6 C7 C12 0.6(2) . . . . ? C6 C7 C8 C9 -0.6(3) . . . . ? C12 C7 C8 C9 179.50(19) . . . . ? C7 C8 C9 C10 -2.0(3) . . . . ? C8 C9 C10 C11 1.9(3) . . . . ? C9 C10 C11 C6 0.8(3) . . . . ? C9 C10 C11 C15 -177.42(19) . . . . ? C7 C6 C11 C10 -3.5(3) . . . . ? N1 C6 C11 C10 179.29(16) . . . . ? C7 C6 C11 C15 174.66(17) . . . . ? N1 C6 C11 C15 -2.5(3) . . . . ? C8 C7 C12 C14 -46.7(3) . . . . ? C6 C7 C12 C14 133.4(2) . . . . ? C8 C7 C12 C13 79.3(3) . . . . ? C6 C7 C12 C13 -100.6(2) . . . . ? C10 C11 C15 C17 72.7(2) . . . . ? C6 C11 C15 C17 -105.5(2) . . . . ? C10 C11 C15 C16 -50.8(2) . . . . ? C6 C11 C15 C16 131.07(19) . . . . ? C4 N2 C18 C19 -99.68(19) . . . . ? Mg1 N2 C18 C19 82.61(18) . . . . ? C4 N2 C18 C23 84.3(2) . . . . ? Mg1 N2 C18 C23 -93.39(17) . . . . ? C23 C18 C19 C20 -3.0(3) . . . . ? N2 C18 C19 C20 -179.04(15) . . . . ? C23 C18 C19 C24 177.26(18) . . . . ? N2 C18 C19 C24 1.3(3) . . . . ? C18 C19 C20 C21 0.3(3) . . . . ? C24 C19 C20 C21 180.00(18) . . . . ? C19 C20 C21 C22 1.8(3) . . . . ? C20 C21 C22 C23 -1.3(3) . . . . ? C21 C22 C23 C18 -1.4(3) . . . . ? C21 C22 C23 C27 174.35(17) . . . . ? C19 C18 C23 C22 3.6(3) . . . . ? N2 C18 C23 C22 179.54(16) . . . . ? C19 C18 C23 C27 -172.02(16) . . . . ? N2 C18 C23 C27 3.9(2) . . . . ? C20 C19 C24 C26 -78.3(3) . . . . ? C18 C19 C24 C26 101.4(3) . . . . ? C20 C19 C24 C25 44.7(3) . . . . ? C18 C19 C24 C25 -135.6(2) . . . . ? C22 C23 C27 C29 49.5(2) . . . . ? C18 C23 C27 C29 -134.93(18) . . . . ? C22 C23 C27 C28 -73.4(2) . . . . ? C18 C23 C27 C28 102.17(19) . . . . ? C34 N3 C30 C31 -48.2(2) . . . . ? Mg1 N3 C30 C31 107.87(18) . . . . ? N3 C30 C31 C35 -135.1(2) . . . . ? N3 C30 C31 C32 46.4(2) . . . . ? C35 C31 C32 C38 -5.4(3) . . . . ? C30 C31 C32 C38 173.13(18) . . . . ? C35 C31 C32 C33 168.1(2) . . . . ? C30 C31 C32 C33 -13.3(3) . . . . ? C38 C32 C33 C34 155.0(2) . . . . ? C31 C32 C33 C34 -18.0(3) . . . . ? C30 N3 C34 C33 17.9(3) . . . . ? Mg1 N3 C34 C33 -138.32(18) . . . . ? C32 C33 C34 N3 16.3(3) . . . . ? C32 C31 C35 C36 4.5(3) . . . . ? C30 C31 C35 C36 -174.0(2) . . . . ? C31 C35 C36 C37 -1.1(4) . . . . ? C35 C36 C37 C38 -1.0(4) . . . . ? C36 C37 C38 C32 -0.2(4) . . . . ? C31 C32 C38 C37 3.3(3) . . . . ? C33 C32 C38 C37 -169.7(2) . . . . ? C43 N4 C39 C40 -0.1(3) . . . . ? Mg1 N4 C39 C40 178.64(13) . . . . ? N4 C39 C40 C44 179.92(17) . . . . ? N4 C39 C40 C41 0.4(3) . . . . ? C44 C40 C41 C42 179.91(16) . . . . ? C39 C40 C41 C42 -0.6(2) . . . . ? C44 C40 C41 C47 -0.5(2) . . . . ? C39 C40 C41 C47 179.01(15) . . . . ? C40 C41 C42 C43 0.4(2) . . . . ? C47 C41 C42 C43 -179.14(16) . . . . ? C41 C42 C43 N4 -0.1(3) . . . . ? C39 N4 C43 C42 -0.1(3) . . . . ? Mg1 N4 C43 C42 -178.83(13) . . . . ? C41 C40 C44 C45 1.0(3) . . . . ? C39 C40 C44 C45 -178.44(18) . . . . ? C40 C44 C45 C46 -0.6(3) . . . . ? C44 C45 C46 C47 -0.5(3) . . . . ? C45 C46 C47 C41 1.0(3) . . . . ? C42 C41 C47 C46 179.04(17) . . . . ? C40 C41 C47 C46 -0.5(3) . . . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.276 _refine_diff_density_min -0.282 _refine_diff_density_rms 0.039 #===end data_11-h10msh27 _database_code_depnum_ccdc_archive 'CCDC 831740' #TrackingRef '- bigcif.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C71.50 H96 Mg2 N6 O2' _chemical_formula_weight 1120.16 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 0.0016 '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 0.0486 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' _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 13.0076(2) _cell_length_b 14.3714(2) _cell_length_c 18.6803(3) _cell_angle_alpha 90.00 _cell_angle_beta 94.299(1) _cell_angle_gamma 90.00 _cell_volume 3482.22(9) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 47542 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 27.485 _exptl_crystal_description block _exptl_crystal_colour ? _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.068 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1214 _exptl_absorpt_coefficient_mu 0.080 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_measurement_device_type '95mm CCD camera on \k-goniostat' _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 55826 _diffrn_reflns_av_R_equivalents 0.0477 _diffrn_reflns_av_sigmaI/netI 0.0305 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.53 _diffrn_reflns_theta_max 27.48 _reflns_number_total 7938 _reflns_number_gt 6115 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Bruker AXS BV 1997-2004)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo & Scalepack (Otwinowski, Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick 1990)' _computing_structure_refinement 'SHELXL-97/2 (Sheldrick 1997)' _computing_molecular_graphics 'ORTEX (P.McArdle 1995)' _computing_publication_material 'SHELXL-97/2 (Sheldrick 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The asymmetric unit = 1/2 of a dimer molecule plus a small region of disordered solvent. Both fragments straddle inversion centres. The solvent bore a resemblance to toluene, but because of the symmetry imposed disorder and its diffuse nature, it could not be modeled in any logical way. Hence PLATON SQUEEZE was employed, and allowance has been made herein for the presence of one molecule of toluene per unit cell based on the results from using this algorithm. ; _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^)+(0.1150P)^2^+2.3352P] 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 7938 _refine_ls_number_parameters 359 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0909 _refine_ls_R_factor_gt 0.0723 _refine_ls_wR_factor_ref 0.2128 _refine_ls_wR_factor_gt 0.2008 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.042 _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 C1 C 0.22312(17) 0.24411(17) 0.81175(12) 0.0377(5) Uani 1 1 d . . . H1A H 0.2767 0.2879 0.7993 0.057 Uiso 1 1 calc R . . H1B H 0.1588 0.2780 0.8173 0.057 Uiso 1 1 calc R . . H1C H 0.2119 0.1978 0.7735 0.057 Uiso 1 1 calc R . . C2 C 0.25700(15) 0.19558(14) 0.88158(11) 0.0275(4) Uani 1 1 d . . . C3 C 0.18151(15) 0.19067(15) 0.93187(11) 0.0313(4) Uani 1 1 d . . . H3 H 0.1137 0.2079 0.9143 0.038 Uiso 1 1 calc R . . C4 C 0.19282(16) 0.16382(16) 1.00445(11) 0.0323(5) Uani 1 1 d . . . C5 C 0.10016(19) 0.1836(2) 1.04679(13) 0.0474(6) Uani 1 1 d . . . H5A H 0.1146 0.1628 1.0965 0.071 Uiso 0.50 1 calc PR . . H5B H 0.0400 0.1502 1.0251 0.071 Uiso 0.50 1 calc PR . . H5C H 0.0860 0.2506 1.0462 0.071 Uiso 0.50 1 calc PR . . H5D H 0.0458 0.2129 1.0153 0.071 Uiso 0.50 1 calc PR . . H5E H 0.1204 0.2255 1.0867 0.071 Uiso 0.50 1 calc PR . . H5F H 0.0744 0.1251 1.0656 0.071 Uiso 0.50 1 calc PR . . C6 C 0.42420(15) 0.18401(14) 0.84038(11) 0.0273(4) Uani 1 1 d . . . C7 C 0.43757(16) 0.12621(15) 0.78202(11) 0.0308(4) Uani 1 1 d . . . C8 C 0.51141(18) 0.15074(19) 0.73478(12) 0.0410(5) Uani 1 1 d . . . H8 H 0.5227 0.1111 0.6954 0.049 Uiso 1 1 calc R . . C9 C 0.56798(18) 0.2313(2) 0.74423(13) 0.0467(6) Uani 1 1 d . . . H9 H 0.6166 0.2476 0.7109 0.056 Uiso 1 1 calc R . . C10 C 0.55428(18) 0.28786(18) 0.80162(15) 0.0458(6) Uani 1 1 d . . . H10 H 0.5933 0.3436 0.8074 0.055 Uiso 1 1 calc R . . C11 C 0.48436(17) 0.26540(16) 0.85174(14) 0.0391(5) Uani 1 1 d . . . C12 C 0.37457(18) 0.03859(16) 0.76899(12) 0.0370(5) Uani 1 1 d . . . H12 H 0.3221 0.0368 0.8054 0.044 Uiso 1 1 calc R . . C13 C 0.4417(2) -0.04815(19) 0.77989(16) 0.0532(7) Uani 1 1 d . . . H13A H 0.4916 -0.0502 0.7432 0.080 Uiso 1 1 calc R . . H13B H 0.3980 -0.1037 0.7759 0.080 Uiso 1 1 calc R . . H13C H 0.4784 -0.0462 0.8276 0.080 Uiso 1 1 calc R . . C14 C 0.3165(3) 0.0361(2) 0.69473(16) 0.0601(8) Uani 1 1 d . . . H14A H 0.2719 0.0910 0.6887 0.090 Uiso 1 1 calc R . . H14B H 0.2742 -0.0203 0.6902 0.090 Uiso 1 1 calc R . . H14C H 0.3661 0.0361 0.6577 0.090 Uiso 1 1 calc R . . C15 C 0.4754(3) 0.3264(2) 0.9179(2) 0.0724(11) Uani 1 1 d . . . H15 H 0.4406 0.2881 0.9537 0.087 Uiso 1 1 calc R . . C16 C 0.5762(4) 0.3567(3) 0.9534(2) 0.0893(13) Uani 1 1 d . . . H16A H 0.6041 0.4075 0.9257 0.134 Uiso 1 1 calc R . . H16B H 0.6244 0.3043 0.9556 0.134 Uiso 1 1 calc R . . H16C H 0.5663 0.3783 1.0021 0.134 Uiso 1 1 calc R . . C17 C 0.4114(5) 0.4090(5) 0.9034(5) 0.220(5) Uani 1 1 d . . . H17A H 0.4136 0.4482 0.9464 0.330 Uiso 1 1 calc R . . H17B H 0.3402 0.3899 0.8903 0.330 Uiso 1 1 calc R . . H17C H 0.4377 0.4442 0.8637 0.330 Uiso 1 1 calc R . . C18 C 0.28336(17) 0.11516(18) 1.11277(12) 0.0381(5) Uani 1 1 d . . . C19 C 0.24468(18) 0.0362(2) 1.14489(13) 0.0462(6) Uani 1 1 d . . . C20 C 0.2517(2) 0.0309(3) 1.22000(15) 0.0630(9) Uani 1 1 d . . . H20 H 0.2264 -0.0226 1.2428 0.076 Uiso 1 1 calc R . . C21 C 0.2948(2) 0.1020(3) 1.26116(15) 0.0711(11) Uani 1 1 d . . . H21 H 0.2972 0.0980 1.3120 0.085 Uiso 1 1 calc R . . C22 C 0.3349(2) 0.1803(3) 1.22869(14) 0.0615(9) Uani 1 1 d . . . H22 H 0.3651 0.2289 1.2577 0.074 Uiso 1 1 calc R . . C23 C 0.3313(2) 0.1879(2) 1.15396(13) 0.0483(7) Uani 1 1 d . . . C24 C 0.19699(19) -0.0447(2) 1.10198(15) 0.0489(6) Uani 1 1 d . . . H24 H 0.1935 -0.0269 1.0501 0.059 Uiso 1 1 calc R . . C25 C 0.2649(2) -0.1310(2) 1.11138(19) 0.0657(9) Uani 1 1 d . . . H25A H 0.2688 -0.1506 1.1617 0.099 Uiso 1 1 calc R . . H25B H 0.3342 -0.1165 1.0974 0.099 Uiso 1 1 calc R . . H25C H 0.2351 -0.1813 1.0810 0.099 Uiso 1 1 calc R . . C26 C 0.0869(2) -0.0672(3) 1.1210(2) 0.0726(10) Uani 1 1 d . . . H26A H 0.0602 -0.1201 1.0920 0.109 Uiso 1 1 calc R . . H26B H 0.0425 -0.0129 1.1110 0.109 Uiso 1 1 calc R . . H26C H 0.0875 -0.0831 1.1720 0.109 Uiso 1 1 calc R . . C27 C 0.3778(3) 0.2713(2) 1.11919(15) 0.0577(7) Uani 1 1 d . . . H27 H 0.3963 0.2513 1.0705 0.069 Uiso 1 1 calc R . . C28 C 0.4767(3) 0.3067(3) 1.1597(2) 0.0810(11) Uani 1 1 d . . . H28A H 0.5083 0.3544 1.1310 0.121 Uiso 1 1 calc R . . H28B H 0.5249 0.2548 1.1685 0.121 Uiso 1 1 calc R . . H28C H 0.4601 0.3335 1.2057 0.121 Uiso 1 1 calc R . . C29 C 0.3026(4) 0.3514(3) 1.1084(3) 0.1137(19) Uani 1 1 d . . . H29A H 0.2850 0.3747 1.1553 0.171 Uiso 1 1 calc R . . H29B H 0.2399 0.3298 1.0810 0.171 Uiso 1 1 calc R . . H29C H 0.3342 0.4014 1.0820 0.171 Uiso 1 1 calc R . . C30 C 0.19255(17) -0.04687(17) 0.89150(13) 0.0383(5) Uani 1 1 d . . . H30 H 0.1637 0.0138 0.8868 0.046 Uiso 1 1 calc R . . C31 C 0.13673(18) -0.12045(19) 0.86228(15) 0.0452(6) Uani 1 1 d . . . H31 H 0.0712 -0.1105 0.8375 0.054 Uiso 1 1 calc R . . C32 C 0.1769(2) -0.20866(19) 0.86931(15) 0.0488(6) Uani 1 1 d . . . H32 H 0.1394 -0.2606 0.8497 0.059 Uiso 1 1 calc R . . C33 C 0.2725(2) -0.22053(18) 0.90521(16) 0.0512(6) Uani 1 1 d . . . H33 H 0.3019 -0.2808 0.9113 0.061 Uiso 1 1 calc R . . C34 C 0.32467(19) -0.14249(17) 0.93228(14) 0.0422(6) Uani 1 1 d . . . H34 H 0.3911 -0.1505 0.9562 0.051 Uiso 1 1 calc R . . N1 N 0.35142(12) 0.16047(11) 0.89241(9) 0.0254(3) Uani 1 1 d . . . N2 N 0.27687(13) 0.12425(13) 1.03540(9) 0.0308(4) Uani 1 1 d . . . N3 N 0.28590(14) -0.05666(13) 0.92631(10) 0.0330(4) Uani 1 1 d . . . Mg1 Mg 0.38198(4) 0.05771(4) 0.97176(3) 0.02482(18) Uani 1 1 d . . . O1 O 0.52298(4) 0.01170(4) 0.96176(3) 0.0366(4) Uani 1 1 d R . -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 C1 0.0323(11) 0.0454(13) 0.0354(12) 0.0101(10) 0.0021(9) 0.0080(9) C2 0.0270(10) 0.0274(9) 0.0278(10) -0.0011(8) 0.0012(7) 0.0004(7) C3 0.0227(9) 0.0387(11) 0.0325(11) 0.0029(9) 0.0018(8) 0.0055(8) C4 0.0262(10) 0.0395(11) 0.0319(11) -0.0010(9) 0.0062(8) 0.0052(8) C5 0.0339(12) 0.0734(18) 0.0363(12) 0.0085(12) 0.0127(10) 0.0209(12) C6 0.0244(9) 0.0291(10) 0.0287(10) 0.0060(8) 0.0039(8) 0.0026(7) C7 0.0279(10) 0.0399(11) 0.0249(10) 0.0060(8) 0.0028(8) 0.0057(8) C8 0.0337(11) 0.0634(15) 0.0268(11) 0.0059(10) 0.0076(9) 0.0079(11) C9 0.0282(11) 0.0723(18) 0.0401(13) 0.0242(12) 0.0069(9) -0.0015(11) C10 0.0324(12) 0.0462(14) 0.0594(16) 0.0166(12) 0.0070(11) -0.0056(10) C11 0.0337(11) 0.0339(11) 0.0507(14) 0.0031(10) 0.0096(10) -0.0045(9) C12 0.0406(12) 0.0391(12) 0.0317(11) -0.0069(9) 0.0041(9) 0.0021(9) C13 0.0633(17) 0.0437(14) 0.0519(16) -0.0068(12) -0.0013(13) 0.0117(12) C14 0.0634(18) 0.0583(17) 0.0552(17) -0.0095(14) -0.0191(14) 0.0006(14) C15 0.068(2) 0.0493(16) 0.105(3) -0.0347(17) 0.0426(19) -0.0291(15) C16 0.114(3) 0.077(2) 0.071(2) -0.0231(19) -0.033(2) 0.035(2) C17 0.153(5) 0.170(6) 0.312(10) -0.184(7) -0.150(6) 0.117(5) C18 0.0286(10) 0.0593(15) 0.0273(11) 0.0022(10) 0.0083(8) 0.0178(10) C19 0.0277(11) 0.0781(18) 0.0341(12) 0.0168(12) 0.0104(9) 0.0155(11) C20 0.0410(14) 0.116(3) 0.0338(14) 0.0247(16) 0.0119(11) 0.0203(16) C21 0.0496(16) 0.137(3) 0.0277(13) 0.0087(17) 0.0100(12) 0.0378(19) C22 0.0530(16) 0.098(2) 0.0331(13) -0.0145(15) 0.0030(12) 0.0302(16) C23 0.0477(14) 0.0668(17) 0.0308(12) -0.0081(11) 0.0054(10) 0.0245(13) C24 0.0346(12) 0.0664(17) 0.0465(14) 0.0228(13) 0.0079(10) 0.0015(11) C25 0.0534(17) 0.075(2) 0.070(2) 0.0218(17) 0.0127(15) 0.0118(15) C26 0.0394(15) 0.093(3) 0.087(2) 0.029(2) 0.0149(15) -0.0014(15) C27 0.080(2) 0.0537(16) 0.0388(14) -0.0187(12) -0.0013(13) 0.0105(15) C28 0.067(2) 0.086(3) 0.088(3) -0.012(2) -0.0017(19) 0.0060(19) C29 0.103(3) 0.060(2) 0.169(5) 0.003(3) -0.050(3) 0.015(2) C30 0.0310(11) 0.0409(12) 0.0430(13) -0.0024(10) 0.0032(9) -0.0020(9) C31 0.0300(11) 0.0532(15) 0.0522(15) -0.0099(12) 0.0011(10) -0.0064(10) C32 0.0423(13) 0.0473(14) 0.0563(16) -0.0170(12) 0.0012(11) -0.0129(11) C33 0.0520(15) 0.0345(12) 0.0657(17) -0.0072(12) -0.0053(13) -0.0056(11) C34 0.0399(12) 0.0362(12) 0.0490(14) 0.0010(10) -0.0072(10) -0.0042(10) N1 0.0235(8) 0.0272(8) 0.0260(8) 0.0006(6) 0.0053(6) 0.0003(6) N2 0.0271(8) 0.0407(10) 0.0253(8) 0.0014(7) 0.0052(7) 0.0058(7) N3 0.0309(9) 0.0331(9) 0.0349(9) -0.0001(7) 0.0018(7) -0.0056(7) Mg1 0.0222(3) 0.0281(3) 0.0244(3) -0.0007(3) 0.0033(2) -0.0007(2) O1 0.0285(7) 0.0479(9) 0.0337(8) 0.0045(7) 0.0044(6) 0.0082(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 C1 C2 1.515(3) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 N1 1.329(3) . ? C2 C3 1.411(3) . ? C3 C4 1.407(3) . ? C3 H3 0.9500 . ? C4 N2 1.326(3) . ? C4 C5 1.517(3) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C5 H5D 0.9800 . ? C5 H5E 0.9800 . ? C5 H5F 0.9800 . ? C6 C7 1.392(3) . ? C6 C11 1.415(3) . ? C6 N1 1.447(2) . ? C7 C8 1.397(3) . ? C7 C12 1.512(3) . ? C8 C9 1.376(4) . ? C8 H8 0.9500 . ? C9 C10 1.368(4) . ? C9 H9 0.9500 . ? C10 C11 1.391(3) . ? C10 H10 0.9500 . ? C11 C15 1.527(4) . ? C12 C13 1.527(3) . ? C12 C14 1.530(4) . ? C12 H12 1.0000 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C17 1.463(6) . ? C15 C16 1.489(5) . ? C15 H15 1.0000 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C19 1.395(4) . ? C18 C23 1.414(4) . ? C18 N2 1.447(3) . ? C19 C20 1.401(4) . ? C19 C24 1.518(4) . ? C20 C21 1.373(5) . ? C20 H20 0.9500 . ? C21 C22 1.398(5) . ? C21 H21 0.9500 . ? C22 C23 1.397(4) . ? C22 H22 0.9500 . ? C23 C27 1.511(4) . ? C24 C25 1.525(4) . ? C24 C26 1.536(4) . ? C24 H24 1.0000 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C29 1.514(5) . ? C27 C28 1.530(5) . ? C27 H27 1.0000 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 N3 1.341(3) . ? C30 C31 1.372(3) . ? C30 H30 0.9500 . ? C31 C32 1.374(4) . ? C31 H31 0.9500 . ? C32 C33 1.378(4) . ? C32 H32 0.9500 . ? C33 C34 1.387(3) . ? C33 H33 0.9500 . ? C34 N3 1.334(3) . ? C34 H34 0.9500 . ? N1 Mg1 2.1090(17) . ? N2 Mg1 2.1073(18) . ? N3 Mg1 2.1966(19) . ? Mg1 O1 1.9583(12) 3_657 ? Mg1 O1 1.9716 . ? O1 Mg1 1.9583(12) 3_657 ? 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 C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N1 C2 C3 124.13(18) . . ? N1 C2 C1 120.77(18) . . ? C3 C2 C1 115.10(18) . . ? C4 C3 C2 128.89(19) . . ? C4 C3 H3 115.6 . . ? C2 C3 H3 115.6 . . ? N2 C4 C3 124.13(18) . . ? N2 C4 C5 120.95(19) . . ? C3 C4 C5 114.92(19) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C4 C5 H5D 109.5 . . ? H5A C5 H5D 141.1 . . ? H5B C5 H5D 56.3 . . ? H5C C5 H5D 56.3 . . ? C4 C5 H5E 109.5 . . ? H5A C5 H5E 56.3 . . ? H5B C5 H5E 141.1 . . ? H5C C5 H5E 56.3 . . ? H5D C5 H5E 109.5 . . ? C4 C5 H5F 109.5 . . ? H5A C5 H5F 56.3 . . ? H5B C5 H5F 56.3 . . ? H5C C5 H5F 141.1 . . ? H5D C5 H5F 109.5 . . ? H5E C5 H5F 109.5 . . ? C7 C6 C11 120.72(19) . . ? C7 C6 N1 120.87(18) . . ? C11 C6 N1 118.36(18) . . ? C6 C7 C8 118.4(2) . . ? C6 C7 C12 121.67(18) . . ? C8 C7 C12 119.9(2) . . ? C9 C8 C7 121.2(2) . . ? C9 C8 H8 119.4 . . ? C7 C8 H8 119.4 . . ? C10 C9 C8 120.1(2) . . ? C10 C9 H9 120.0 . . ? C8 C9 H9 120.0 . . ? C9 C10 C11 121.3(2) . . ? C9 C10 H10 119.3 . . ? C11 C10 H10 119.3 . . ? C10 C11 C6 118.2(2) . . ? C10 C11 C15 120.3(2) . . ? C6 C11 C15 121.4(2) . . ? C7 C12 C13 111.2(2) . . ? C7 C12 C14 113.0(2) . . ? C13 C12 C14 109.9(2) . . ? C7 C12 H12 107.5 . . ? C13 C12 H12 107.5 . . ? C14 C12 H12 107.5 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C17 C15 C16 108.3(3) . . ? C17 C15 C11 113.1(4) . . ? C16 C15 C11 114.2(3) . . ? C17 C15 H15 106.9 . . ? C16 C15 H15 106.9 . . ? C11 C15 H15 106.9 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C19 C18 C23 121.7(2) . . ? C19 C18 N2 120.5(2) . . ? C23 C18 N2 117.8(2) . . ? C18 C19 C20 118.4(3) . . ? C18 C19 C24 122.8(2) . . ? C20 C19 C24 118.8(3) . . ? C21 C20 C19 121.0(3) . . ? C21 C20 H20 119.5 . . ? C19 C20 H20 119.5 . . ? C20 C21 C22 120.4(3) . . ? C20 C21 H21 119.8 . . ? C22 C21 H21 119.8 . . ? C23 C22 C21 120.7(3) . . ? C23 C22 H22 119.7 . . ? C21 C22 H22 119.7 . . ? C22 C23 C18 117.8(3) . . ? C22 C23 C27 120.4(3) . . ? C18 C23 C27 121.8(2) . . ? C19 C24 C25 110.6(2) . . ? C19 C24 C26 113.0(3) . . ? C25 C24 C26 110.1(2) . . ? C19 C24 H24 107.6 . . ? C25 C24 H24 107.6 . . ? C26 C24 H24 107.6 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C23 C27 C29 112.6(3) . . ? C23 C27 C28 113.6(3) . . ? C29 C27 C28 108.9(3) . . ? C23 C27 H27 107.1 . . ? C29 C27 H27 107.1 . . ? C28 C27 H27 107.1 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? N3 C30 C31 123.0(2) . . ? N3 C30 H30 118.5 . . ? C31 C30 H30 118.5 . . ? C30 C31 C32 119.1(2) . . ? C30 C31 H31 120.4 . . ? C32 C31 H31 120.4 . . ? C31 C32 C33 118.9(2) . . ? C31 C32 H32 120.5 . . ? C33 C32 H32 120.5 . . ? C32 C33 C34 118.5(2) . . ? C32 C33 H33 120.8 . . ? C34 C33 H33 120.8 . . ? N3 C34 C33 123.1(2) . . ? N3 C34 H34 118.5 . . ? C33 C34 H34 118.5 . . ? C2 N1 C6 116.92(16) . . ? C2 N1 Mg1 119.74(13) . . ? C6 N1 Mg1 122.51(12) . . ? C4 N2 C18 117.30(17) . . ? C4 N2 Mg1 119.82(14) . . ? C18 N2 Mg1 122.05(13) . . ? C34 N3 C30 117.4(2) . . ? C34 N3 Mg1 117.32(15) . . ? C30 N3 Mg1 125.25(16) . . ? O1 Mg1 O1 48.8 3_657 . ? O1 Mg1 N2 106.19(6) 3_657 . ? O1 Mg1 N2 148.55(5) . . ? O1 Mg1 N1 151.54(7) 3_657 . ? O1 Mg1 N1 107.21(5) . . ? N2 Mg1 N1 89.00(7) . . ? O1 Mg1 N3 100.24(6) 3_657 . ? O1 Mg1 N3 102.64(5) . . ? N2 Mg1 N3 100.55(7) . . ? N1 Mg1 N3 100.40(7) . . ? Mg1 O1 Mg1 131.16(3) 3_657 . ? 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 N1 C2 C3 C4 11.3(4) . . . . ? C1 C2 C3 C4 -169.2(2) . . . . ? C2 C3 C4 N2 -10.8(4) . . . . ? C2 C3 C4 C5 169.1(2) . . . . ? C11 C6 C7 C8 -0.3(3) . . . . ? N1 C6 C7 C8 -177.86(18) . . . . ? C11 C6 C7 C12 179.7(2) . . . . ? N1 C6 C7 C12 2.1(3) . . . . ? C6 C7 C8 C9 -1.7(3) . . . . ? C12 C7 C8 C9 178.3(2) . . . . ? C7 C8 C9 C10 1.6(4) . . . . ? C8 C9 C10 C11 0.6(4) . . . . ? C9 C10 C11 C6 -2.6(4) . . . . ? C9 C10 C11 C15 176.0(3) . . . . ? C7 C6 C11 C10 2.4(3) . . . . ? N1 C6 C11 C10 180.0(2) . . . . ? C7 C6 C11 C15 -176.2(3) . . . . ? N1 C6 C11 C15 1.4(3) . . . . ? C6 C7 C12 C13 -112.0(2) . . . . ? C8 C7 C12 C13 68.0(3) . . . . ? C6 C7 C12 C14 123.9(2) . . . . ? C8 C7 C12 C14 -56.1(3) . . . . ? C10 C11 C15 C17 81.3(5) . . . . ? C6 C11 C15 C17 -100.1(5) . . . . ? C10 C11 C15 C16 -43.2(4) . . . . ? C6 C11 C15 C16 135.4(3) . . . . ? C23 C18 C19 C20 1.7(3) . . . . ? N2 C18 C19 C20 -179.3(2) . . . . ? C23 C18 C19 C24 -177.4(2) . . . . ? N2 C18 C19 C24 1.7(3) . . . . ? C18 C19 C20 C21 0.6(4) . . . . ? C24 C19 C20 C21 179.6(2) . . . . ? C19 C20 C21 C22 -1.7(4) . . . . ? C20 C21 C22 C23 0.5(4) . . . . ? C21 C22 C23 C18 1.6(4) . . . . ? C21 C22 C23 C27 -178.1(3) . . . . ? C19 C18 C23 C22 -2.7(3) . . . . ? N2 C18 C23 C22 178.2(2) . . . . ? C19 C18 C23 C27 177.0(2) . . . . ? N2 C18 C23 C27 -2.1(3) . . . . ? C18 C19 C24 C25 112.1(3) . . . . ? C20 C19 C24 C25 -66.9(3) . . . . ? C18 C19 C24 C26 -123.9(3) . . . . ? C20 C19 C24 C26 57.1(3) . . . . ? C22 C23 C27 C29 -87.9(4) . . . . ? C18 C23 C27 C29 92.4(3) . . . . ? C22 C23 C27 C28 36.5(4) . . . . ? C18 C23 C27 C28 -143.2(3) . . . . ? N3 C30 C31 C32 0.7(4) . . . . ? C30 C31 C32 C33 -0.4(4) . . . . ? C31 C32 C33 C34 -0.6(4) . . . . ? C32 C33 C34 N3 1.2(4) . . . . ? C3 C2 N1 C6 -170.63(19) . . . . ? C1 C2 N1 C6 9.9(3) . . . . ? C3 C2 N1 Mg1 19.5(3) . . . . ? C1 C2 N1 Mg1 -159.97(16) . . . . ? C7 C6 N1 C2 -93.2(2) . . . . ? C11 C6 N1 C2 89.2(2) . . . . ? C7 C6 N1 Mg1 76.3(2) . . . . ? C11 C6 N1 Mg1 -101.3(2) . . . . ? C3 C4 N2 C18 169.8(2) . . . . ? C5 C4 N2 C18 -10.1(3) . . . . ? C3 C4 N2 Mg1 -20.5(3) . . . . ? C5 C4 N2 Mg1 159.66(19) . . . . ? C19 C18 N2 C4 89.4(3) . . . . ? C23 C18 N2 C4 -91.6(2) . . . . ? C19 C18 N2 Mg1 -80.1(2) . . . . ? C23 C18 N2 Mg1 98.9(2) . . . . ? C33 C34 N3 C30 -0.9(4) . . . . ? C33 C34 N3 Mg1 -179.3(2) . . . . ? C31 C30 N3 C34 -0.1(3) . . . . ? C31 C30 N3 Mg1 178.11(18) . . . . ? C4 N2 Mg1 O1 -168.66(16) . . . 3_657 ? C18 N2 Mg1 O1 0.58(19) . . . 3_657 ? C4 N2 Mg1 O1 158.37(13) . . . . ? C18 N2 Mg1 O1 -32.4(2) . . . . ? C4 N2 Mg1 N1 35.76(17) . . . . ? C18 N2 Mg1 N1 -155.00(18) . . . . ? C4 N2 Mg1 N3 -64.63(18) . . . . ? C18 N2 Mg1 N3 104.61(18) . . . . ? C2 N1 Mg1 O1 -158.83(14) . . . 3_657 ? C6 N1 Mg1 O1 31.9(2) . . . 3_657 ? C2 N1 Mg1 O1 172.14(14) . . . . ? C6 N1 Mg1 O1 2.87(16) . . . . ? C2 N1 Mg1 N2 -35.25(16) . . . . ? C6 N1 Mg1 N2 155.48(15) . . . . ? C2 N1 Mg1 N3 65.30(16) . . . . ? C6 N1 Mg1 N3 -103.97(15) . . . . ? C34 N3 Mg1 O1 -19.87(18) . . . 3_657 ? C30 N3 Mg1 O1 161.89(17) . . . 3_657 ? C34 N3 Mg1 O1 29.96(18) . . . . ? C30 N3 Mg1 O1 -148.27(17) . . . . ? C34 N3 Mg1 N2 -128.65(18) . . . . ? C30 N3 Mg1 N2 53.11(19) . . . . ? C34 N3 Mg1 N1 140.42(17) . . . . ? C30 N3 Mg1 N1 -37.82(19) . . . . ? O1 Mg1 O1 Mg1 0.0 3_657 . . 3_657 ? N2 Mg1 O1 Mg1 43.96(10) . . . 3_657 ? N1 Mg1 O1 Mg1 162.11(8) . . . 3_657 ? N3 Mg1 O1 Mg1 -92.64(7) . . . 3_657 ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.743 _refine_diff_density_min -0.791 _refine_diff_density_rms 0.084 # 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 0.500 1.000 231 20 ' ' 2 0.076 0.039 0.756 16 2 ' ' 3 0.500 0.000 0.500 231 20 ' ' 4 0.423 0.539 0.744 16 2 ' ' 5 0.577 0.461 0.256 16 2 ' ' 6 0.923 0.961 0.244 16 2 ' ' _platon_squeeze_details ; ; #===end data_12-h11msh5 _database_code_depnum_ccdc_archive 'CCDC 831741' #TrackingRef '- bigcif.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C72 H102 Mg2 N8 O2' _chemical_formula_sum 'C72 H102 Mg2 N8 O2' _chemical_formula_weight 1160.24 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mg Mg 0.0486 0.0363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' 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 14.1320(7) _cell_length_b 13.7311(5) _cell_length_c 17.9409(11) _cell_angle_alpha 90.00 _cell_angle_beta 95.414(3) _cell_angle_gamma 90.00 _cell_volume 3465.9(3) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 28556 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 25.028 _exptl_crystal_description block _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.112 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1260 _exptl_absorpt_coefficient_mu 0.083 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Nonius Kappa CCD' _diffrn_measurement_method '145 1.9 degree images with \w scans' _diffrn_standards_number 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 24351 _diffrn_reflns_av_R_equivalents 0.1851 _diffrn_reflns_av_sigmaI/netI 0.1155 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 4.68 _diffrn_reflns_theta_max 25.15 _reflns_number_total 6008 _reflns_number_gt 3927 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinski & Minor, 1997)' _computing_data_reduction ; DENZO-SCALEPACK Z. Otwinowski and W. Minor, " Processing of X-ray Diffraction Data Collected in Oscillation Mode ", Methods in Enzymology, Volume 276: Macromolecular Crystallography, part A, p.307-326, 1997,C.W. Carter, Jr. & R. M. Sweet, Eds., Academic Press. ; _computing_structure_solution ; SIR97- Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C. , Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. (1999) J. Appl. Cryst. 32, 115-119 ; _computing_structure_refinement ; SHELXL97 -Program for Crystal Structure Analysis (Release 97-2). Sheldrick, G.M., Institut f\"ur Anorganische Chemie der Universit\"at, Tammanstrasse 4, D-3400 G\"ottingen, Germany, 1998 ; _computing_molecular_graphics 'ORTEP3 for Windows - Farrugia, L. J. J. Appl. Crystallogr. 1997, 30, 565' _computing_publication_material ; 'WinGX publication routines, Farrugia, L. J., J. Appl. Crystallogr., 1999, 32, 837-838 ; _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^)+(0.1021P)^2^+2.7472P] 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 6008 _refine_ls_number_parameters 391 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1291 _refine_ls_R_factor_gt 0.0845 _refine_ls_wR_factor_ref 0.2394 _refine_ls_wR_factor_gt 0.2027 _refine_ls_goodness_of_fit_ref 1.070 _refine_ls_restrained_S_all 1.070 _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 0.89241(8) 0.02941(8) 0.04048(7) 0.0369(3) Uani 1 1 d . . . O1 O 0.99407(19) -0.05710(17) 0.01194(16) 0.0498(7) Uani 1 1 d . . . N1 N 0.7716(2) -0.0605(2) 0.05451(17) 0.0379(7) Uani 1 1 d . . . N2 N 0.7988(2) 0.1470(2) 0.01405(17) 0.0367(7) Uani 1 1 d . . . N3 N 0.9332(2) 0.0593(2) 0.15728(18) 0.0422(7) Uani 1 1 d . . . N4 N 1.0230(2) 0.0864(2) 0.38672(19) 0.0471(8) Uani 1 1 d . . . C1 C 0.6935(3) -0.0237(3) 0.0781(2) 0.0402(8) Uani 1 1 d . . . C2 C 0.6155(3) -0.0895(3) 0.1024(3) 0.0555(11) Uani 1 1 d . . . H2A H 0.5755 -0.1119 0.0581 0.083 Uiso 1 1 calc R . . H2B H 0.5765 -0.0531 0.1352 0.083 Uiso 1 1 calc R . . H2C H 0.6441 -0.1458 0.1294 0.083 Uiso 1 1 calc R . . C3 C 0.6733(3) 0.0770(2) 0.0805(2) 0.0420(9) Uani 1 1 d . . . H3 H 0.6226 0.0946 0.1090 0.050 Uiso 1 1 calc R . . C4 C 0.7177(2) 0.1547(2) 0.0465(2) 0.0389(8) Uani 1 1 d . . . C5 C 0.6665(3) 0.2516(3) 0.0472(2) 0.0466(9) Uani 1 1 d . . . H5A H 0.7085 0.3003 0.0729 0.070 Uiso 1 1 calc R . . H5B H 0.6091 0.2445 0.0735 0.070 Uiso 1 1 calc R . . H5C H 0.6487 0.2728 -0.0044 0.070 Uiso 1 1 calc R . . C6 C 0.7741(2) -0.1647(2) 0.0438(2) 0.0375(8) Uani 1 1 d . . . C7 C 0.7319(3) -0.2050(3) -0.0231(2) 0.0433(9) Uani 1 1 d . . . C8 C 0.6849(3) -0.1401(3) -0.0851(2) 0.0469(9) Uani 1 1 d . . . H8 H 0.6659 -0.0777 -0.0619 0.056 Uiso 1 1 calc R . . C9 C 0.7566(4) -0.1167(3) -0.1403(3) 0.0613(12) Uani 1 1 d . . . H9A H 0.8116 -0.0838 -0.1141 0.092 Uiso 1 1 calc R . . H9B H 0.7272 -0.0739 -0.1796 0.092 Uiso 1 1 calc R . . H9C H 0.7773 -0.1771 -0.1628 0.092 Uiso 1 1 calc R . . C10 C 0.5962(3) -0.1858(4) -0.1261(3) 0.0770(15) Uani 1 1 d . . . H10A H 0.5689 -0.1409 -0.1648 0.115 Uiso 1 1 calc R . . H10B H 0.5494 -0.1989 -0.0904 0.115 Uiso 1 1 calc R . . H10C H 0.6135 -0.2470 -0.1496 0.115 Uiso 1 1 calc R . . C11 C 0.7394(3) -0.3048(3) -0.0346(2) 0.0471(9) Uani 1 1 d . . . H11 H 0.7130 -0.3322 -0.0806 0.057 Uiso 1 1 calc R . . C12 C 0.7846(3) -0.3649(3) 0.0195(3) 0.0505(10) Uani 1 1 d . . . H12 H 0.7889 -0.4329 0.0108 0.061 Uiso 1 1 calc R . . C13 C 0.8234(3) -0.3253(3) 0.0866(2) 0.0479(10) Uani 1 1 d . . . H13 H 0.8534 -0.3669 0.1240 0.057 Uiso 1 1 calc R . . C14 C 0.8192(2) -0.2252(3) 0.1001(2) 0.0406(8) Uani 1 1 d . . . C15 C 0.8642(3) -0.1852(3) 0.1739(2) 0.0470(9) Uani 1 1 d . . . H15 H 0.8558 -0.1128 0.1726 0.056 Uiso 1 1 calc R . . C16 C 0.9693(3) -0.2054(4) 0.1842(3) 0.0688(13) Uani 1 1 d . . . H16A H 0.9799 -0.2758 0.1884 0.103 Uiso 1 1 calc R . . H16B H 0.9972 -0.1732 0.2298 0.103 Uiso 1 1 calc R . . H16C H 0.9993 -0.1803 0.1410 0.103 Uiso 1 1 calc R . . C17 C 0.8152(4) -0.2241(4) 0.2414(3) 0.0748(14) Uani 1 1 d . . . H17A H 0.7465 -0.2134 0.2327 0.112 Uiso 1 1 calc R . . H17B H 0.8401 -0.1895 0.2869 0.112 Uiso 1 1 calc R . . H17C H 0.8280 -0.2939 0.2474 0.112 Uiso 1 1 calc R . . C18 C 0.8238(2) 0.2307(2) -0.0296(2) 0.0389(8) Uani 1 1 d . . . C19 C 0.8781(2) 0.3064(3) 0.0050(2) 0.0411(9) Uani 1 1 d . . . C20 C 0.9157(3) 0.3045(3) 0.0873(2) 0.0442(9) Uani 1 1 d . . . H20 H 0.8820 0.2505 0.1114 0.053 Uiso 1 1 calc R . . C21 C 1.0205(3) 0.2808(3) 0.0967(3) 0.0598(11) Uani 1 1 d . . . H21A H 1.0319 0.2202 0.0701 0.090 Uiso 1 1 calc R . . H21B H 1.0413 0.2728 0.1501 0.090 Uiso 1 1 calc R . . H21C H 1.0563 0.3339 0.0761 0.090 Uiso 1 1 calc R . . C22 C 0.8954(3) 0.3987(3) 0.1292(3) 0.0579(11) Uani 1 1 d . . . H22A H 0.9313 0.4525 0.1097 0.087 Uiso 1 1 calc R . . H22B H 0.9146 0.3903 0.1828 0.087 Uiso 1 1 calc R . . H22C H 0.8272 0.4133 0.1219 0.087 Uiso 1 1 calc R . . C23 C 0.9002(3) 0.3863(3) -0.0395(2) 0.0461(9) Uani 1 1 d . . . H23 H 0.9376 0.4380 -0.0173 0.055 Uiso 1 1 calc R . . C24 C 0.8690(3) 0.3910(3) -0.1142(2) 0.0502(10) Uani 1 1 d . . . H24 H 0.8831 0.4467 -0.1427 0.060 Uiso 1 1 calc R . . C25 C 0.8171(3) 0.3153(3) -0.1481(2) 0.0498(10) Uani 1 1 d . . . H25 H 0.7971 0.3183 -0.2001 0.060 Uiso 1 1 calc R . . C26 C 0.7937(3) 0.2334(2) -0.1063(2) 0.0401(8) Uani 1 1 d . . . C27 C 0.7370(3) 0.1498(3) -0.1452(2) 0.0484(9) Uani 1 1 d . . . H27 H 0.7578 0.0890 -0.1177 0.058 Uiso 1 1 calc R . . C28 C 0.6323(4) 0.1581(5) -0.1410(4) 0.092(2) Uani 1 1 d . . . H28A H 0.6090 0.2183 -0.1657 0.137 Uiso 1 1 calc R . . H28B H 0.6188 0.1592 -0.0884 0.137 Uiso 1 1 calc R . . H28C H 0.6004 0.1021 -0.1662 0.137 Uiso 1 1 calc R . . C29 C 0.7582(3) 0.1352(3) -0.2263(2) 0.0537(10) Uani 1 1 d . . . H29A H 0.7309 0.0732 -0.2449 0.081 Uiso 1 1 calc R . . H29B H 0.8271 0.1343 -0.2290 0.081 Uiso 1 1 calc R . . H29C H 0.7300 0.1886 -0.2571 0.081 Uiso 1 1 calc R . . C30 C 1.0203(3) 0.0366(3) 0.1863(2) 0.0479(10) Uani 1 1 d . . . H30 H 1.0628 0.0118 0.1529 0.058 Uiso 1 1 calc R . . C31 C 1.0545(3) 0.0455(3) 0.2601(2) 0.0499(10) Uani 1 1 d . . . H31 H 1.1185 0.0288 0.2758 0.060 Uiso 1 1 calc R . . C32 C 0.9936(3) 0.0799(3) 0.3123(2) 0.0415(9) Uani 1 1 d . . . C33 C 0.9019(3) 0.1066(3) 0.2823(2) 0.0445(9) Uani 1 1 d . . . H33 H 0.8580 0.1327 0.3140 0.053 Uiso 1 1 calc R . . C34 C 0.8754(3) 0.0949(3) 0.2072(2) 0.0440(9) Uani 1 1 d . . . H34 H 0.8125 0.1129 0.1889 0.053 Uiso 1 1 calc R . . C35 C 1.1130(3) 0.0471(3) 0.4155(3) 0.0550(10) Uani 1 1 d . . . H35A H 1.1167 -0.0215 0.4009 0.082 Uiso 1 1 calc R . . H35B H 1.1196 0.0521 0.4703 0.082 Uiso 1 1 calc R . . H35C H 1.1642 0.0838 0.3952 0.082 Uiso 1 1 calc R . . C36 C 0.9577(3) 0.1224(3) 0.4382(2) 0.0550(11) Uani 1 1 d . . . H36A H 0.9403 0.1898 0.4254 0.083 Uiso 1 1 calc R . . H36B H 0.9884 0.1197 0.4895 0.083 Uiso 1 1 calc R . . H36C H 0.9004 0.0818 0.4345 0.083 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mg1 0.0459(7) 0.0293(6) 0.0370(7) 0.0001(5) 0.0127(5) -0.0002(5) O1 0.0536(15) 0.0364(14) 0.0633(19) -0.0012(12) 0.0258(13) 0.0034(12) N1 0.0414(16) 0.0298(14) 0.0441(18) 0.0035(13) 0.0130(13) 0.0012(12) N2 0.0400(15) 0.0292(14) 0.0424(17) 0.0014(12) 0.0121(13) -0.0007(12) N3 0.0484(18) 0.0351(15) 0.0448(19) -0.0015(13) 0.0131(14) -0.0004(13) N4 0.0489(18) 0.0489(19) 0.044(2) -0.0069(15) 0.0059(14) 0.0089(14) C1 0.0430(19) 0.0365(19) 0.043(2) 0.0037(16) 0.0126(16) -0.0004(15) C2 0.053(2) 0.039(2) 0.080(3) 0.006(2) 0.035(2) 0.0013(17) C3 0.0414(19) 0.0351(18) 0.053(2) 0.0003(16) 0.0212(17) 0.0034(15) C4 0.0412(19) 0.0326(17) 0.045(2) -0.0001(15) 0.0132(16) 0.0053(14) C5 0.051(2) 0.0364(19) 0.055(2) 0.0013(17) 0.0193(18) 0.0057(16) C6 0.0356(17) 0.0347(18) 0.044(2) 0.0026(15) 0.0130(15) -0.0012(14) C7 0.0428(19) 0.0358(18) 0.054(2) 0.0029(17) 0.0190(17) -0.0022(15) C8 0.052(2) 0.042(2) 0.047(2) -0.0015(17) 0.0097(18) -0.0001(17) C9 0.081(3) 0.057(3) 0.048(3) 0.006(2) 0.017(2) 0.002(2) C10 0.063(3) 0.078(3) 0.088(4) 0.012(3) -0.002(3) -0.007(3) C11 0.052(2) 0.0360(19) 0.056(3) -0.0065(18) 0.0180(19) -0.0056(16) C12 0.056(2) 0.0303(18) 0.068(3) -0.0035(19) 0.019(2) -0.0005(16) C13 0.050(2) 0.0349(19) 0.060(3) 0.0083(18) 0.0137(19) 0.0033(16) C14 0.0415(19) 0.0376(19) 0.045(2) 0.0047(16) 0.0148(16) -0.0013(15) C15 0.058(2) 0.0381(19) 0.047(2) 0.0085(17) 0.0132(18) -0.0046(17) C16 0.061(3) 0.067(3) 0.078(4) 0.003(3) 0.002(2) -0.001(2) C17 0.088(3) 0.089(4) 0.049(3) 0.007(2) 0.017(2) -0.023(3) C18 0.0385(18) 0.0309(17) 0.050(2) 0.0066(15) 0.0166(16) 0.0040(14) C19 0.0432(19) 0.0347(18) 0.047(2) 0.0016(16) 0.0138(16) 0.0015(15) C20 0.052(2) 0.0315(18) 0.051(2) -0.0028(16) 0.0108(18) -0.0030(15) C21 0.056(2) 0.056(3) 0.067(3) -0.002(2) 0.004(2) -0.002(2) C22 0.073(3) 0.043(2) 0.059(3) -0.007(2) 0.016(2) 0.001(2) C23 0.051(2) 0.0331(19) 0.055(3) 0.0004(17) 0.0122(18) -0.0060(16) C24 0.057(2) 0.039(2) 0.056(3) 0.0101(18) 0.019(2) -0.0020(17) C25 0.057(2) 0.044(2) 0.051(3) 0.0049(18) 0.0170(19) -0.0030(18) C26 0.048(2) 0.0305(17) 0.044(2) 0.0006(15) 0.0127(16) 0.0008(15) C27 0.059(2) 0.045(2) 0.042(2) 0.0004(17) 0.0093(18) -0.0075(18) C28 0.065(3) 0.115(5) 0.098(5) -0.052(4) 0.027(3) -0.029(3) C29 0.066(3) 0.050(2) 0.045(2) -0.0018(19) 0.008(2) -0.0010(19) C30 0.047(2) 0.050(2) 0.049(2) -0.0082(18) 0.0179(18) 0.0018(17) C31 0.045(2) 0.056(2) 0.050(3) -0.0103(19) 0.0102(18) 0.0087(18) C32 0.046(2) 0.0355(18) 0.045(2) -0.0024(16) 0.0116(17) 0.0041(15) C33 0.049(2) 0.045(2) 0.040(2) -0.0002(16) 0.0106(17) 0.0059(17) C34 0.048(2) 0.042(2) 0.043(2) 0.0011(16) 0.0100(17) 0.0072(16) C35 0.064(3) 0.049(2) 0.051(3) -0.0029(19) 0.005(2) 0.0051(19) C36 0.063(3) 0.064(3) 0.040(2) -0.0043(19) 0.0124(19) 0.006(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mg1 O1 1.969(3) . ? Mg1 O1 1.972(3) 3_755 ? Mg1 N2 2.112(3) . ? Mg1 N1 2.141(3) . ? Mg1 N3 2.160(3) . ? Mg1 Mg1 3.584(2) 3_755 ? O1 O1 1.638(5) 3_755 ? O1 Mg1 1.972(3) 3_755 ? N1 C1 1.320(4) . ? N1 C6 1.444(4) . ? N2 C4 1.338(4) . ? N2 C18 1.454(4) . ? N3 C30 1.328(5) . ? N3 C34 1.358(5) . ? N4 C32 1.363(5) . ? N4 C35 1.432(5) . ? N4 C36 1.452(5) . ? C1 C3 1.413(5) . ? C1 C2 1.521(5) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 C4 1.405(5) . ? C3 H3 0.9500 . ? C4 C5 1.515(5) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 C7 1.403(5) . ? C6 C14 1.412(5) . ? C7 C11 1.392(5) . ? C7 C8 1.527(6) . ? C8 C9 1.517(6) . ? C8 C10 1.527(6) . ? C8 H8 1.0000 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.384(6) . ? C11 H11 0.9500 . ? C12 C13 1.385(6) . ? C12 H12 0.9500 . ? C13 C14 1.399(5) . ? C13 H13 0.9500 . ? C14 C15 1.517(6) . ? C15 C16 1.505(6) . ? C15 C17 1.546(6) . ? C15 H15 1.0000 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C19 1.401(5) . ? C18 C26 1.401(6) . ? C19 C23 1.409(5) . ? C19 C20 1.522(6) . ? C20 C21 1.511(6) . ? C20 C22 1.537(5) . ? C20 H20 1.0000 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 C24 1.373(6) . ? C23 H23 0.9500 . ? C24 C25 1.380(6) . ? C24 H24 0.9500 . ? C25 C26 1.409(5) . ? C25 H25 0.9500 . ? C26 C27 1.530(5) . ? C27 C28 1.493(6) . ? C27 C29 1.526(6) . ? C27 H27 1.0000 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 C31 1.370(6) . ? C30 H30 0.9500 . ? C31 C32 1.413(5) . ? C31 H31 0.9500 . ? C32 C33 1.405(5) . ? C33 C34 1.373(6) . ? C33 H33 0.9500 . ? C34 H34 0.9500 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 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 O1 49.14(13) . 3_755 ? O1 Mg1 N2 149.27(13) . . ? O1 Mg1 N2 105.44(11) 3_755 . ? O1 Mg1 N1 107.00(11) . . ? O1 Mg1 N1 149.44(13) 3_755 . ? N2 Mg1 N1 88.70(11) . . ? O1 Mg1 N3 103.46(13) . . ? O1 Mg1 N3 105.77(13) 3_755 . ? N2 Mg1 N3 100.17(12) . . ? N1 Mg1 N3 97.94(12) . . ? O1 Mg1 Mg1 24.59(7) . 3_755 ? O1 Mg1 Mg1 24.55(7) 3_755 3_755 ? N2 Mg1 Mg1 128.22(9) . 3_755 ? N1 Mg1 Mg1 129.37(9) . 3_755 ? N3 Mg1 Mg1 106.11(10) . 3_755 ? O1 O1 Mg1 65.52(16) 3_755 . ? O1 O1 Mg1 65.34(16) 3_755 3_755 ? Mg1 O1 Mg1 130.86(13) . 3_755 ? C1 N1 C6 117.0(3) . . ? C1 N1 Mg1 121.1(2) . . ? C6 N1 Mg1 121.7(2) . . ? C4 N2 C18 115.7(3) . . ? C4 N2 Mg1 120.5(2) . . ? C18 N2 Mg1 123.1(2) . . ? C30 N3 C34 114.7(3) . . ? C30 N3 Mg1 119.2(2) . . ? C34 N3 Mg1 125.9(3) . . ? C32 N4 C35 120.5(3) . . ? C32 N4 C36 119.5(3) . . ? C35 N4 C36 119.6(3) . . ? N1 C1 C3 124.2(3) . . ? N1 C1 C2 121.0(3) . . ? C3 C1 C2 114.8(3) . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C4 C3 C1 129.1(3) . . ? C4 C3 H3 115.5 . . ? C1 C3 H3 115.5 . . ? N2 C4 C3 124.3(3) . . ? N2 C4 C5 120.2(3) . . ? C3 C4 C5 115.5(3) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C7 C6 C14 120.4(3) . . ? C7 C6 N1 119.4(3) . . ? C14 C6 N1 120.2(3) . . ? C11 C7 C6 118.9(4) . . ? C11 C7 C8 120.0(4) . . ? C6 C7 C8 120.9(3) . . ? C9 C8 C7 109.1(3) . . ? C9 C8 C10 109.9(4) . . ? C7 C8 C10 113.1(3) . . ? C9 C8 H8 108.2 . . ? C7 C8 H8 108.2 . . ? C10 C8 H8 108.2 . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C8 C10 H10A 109.5 . . ? C8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C12 C11 C7 121.3(4) . . ? C12 C11 H11 119.3 . . ? C7 C11 H11 119.3 . . ? C11 C12 C13 119.6(4) . . ? C11 C12 H12 120.2 . . ? C13 C12 H12 120.2 . . ? C12 C13 C14 121.1(4) . . ? C12 C13 H13 119.5 . . ? C14 C13 H13 119.5 . . ? C13 C14 C6 118.6(4) . . ? C13 C14 C15 119.1(3) . . ? C6 C14 C15 122.3(3) . . ? C16 C15 C14 111.6(4) . . ? C16 C15 C17 110.5(4) . . ? C14 C15 C17 112.1(3) . . ? C16 C15 H15 107.5 . . ? C14 C15 H15 107.5 . . ? C17 C15 H15 107.5 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C19 C18 C26 121.2(3) . . ? C19 C18 N2 119.9(3) . . ? C26 C18 N2 118.8(3) . . ? C18 C19 C23 117.9(4) . . ? C18 C19 C20 122.9(3) . . ? C23 C19 C20 119.2(3) . . ? C21 C20 C19 111.2(3) . . ? C21 C20 C22 110.7(4) . . ? C19 C20 C22 113.3(3) . . ? C21 C20 H20 107.1 . . ? C19 C20 H20 107.1 . . ? C22 C20 H20 107.1 . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C20 C22 H22A 109.5 . . ? C20 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C20 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C24 C23 C19 121.5(4) . . ? C24 C23 H23 119.3 . . ? C19 C23 H23 119.3 . . ? C23 C24 C25 120.2(4) . . ? C23 C24 H24 119.9 . . ? C25 C24 H24 119.9 . . ? C24 C25 C26 120.5(4) . . ? C24 C25 H25 119.7 . . ? C26 C25 H25 119.7 . . ? C18 C26 C25 118.6(3) . . ? C18 C26 C27 121.7(3) . . ? C25 C26 C27 119.6(4) . . ? C28 C27 C29 110.0(4) . . ? C28 C27 C26 113.5(4) . . ? C29 C27 C26 113.2(3) . . ? C28 C27 H27 106.6 . . ? C29 C27 H27 106.6 . . ? C26 C27 H27 106.6 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? N3 C30 C31 126.0(3) . . ? N3 C30 H30 117.0 . . ? C31 C30 H30 117.0 . . ? C30 C31 C32 119.2(4) . . ? C30 C31 H31 120.4 . . ? C32 C31 H31 120.4 . . ? N4 C32 C33 123.0(3) . . ? N4 C32 C31 121.5(3) . . ? C33 C32 C31 115.5(4) . . ? C34 C33 C32 120.2(3) . . ? C34 C33 H33 119.9 . . ? C32 C33 H33 119.9 . . ? N3 C34 C33 124.3(4) . . ? N3 C34 H34 117.8 . . ? C33 C34 H34 117.8 . . ? N4 C35 H35A 109.5 . . ? N4 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? N4 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? N4 C36 H36A 109.5 . . ? N4 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? N4 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.967 _diffrn_reflns_theta_full 25.15 _diffrn_measured_fraction_theta_full 0.967 _refine_diff_density_max 0.320 _refine_diff_density_min -0.423 _refine_diff_density_rms 0.066 #===end