data_global #TrackingRef '- C0CC03234D_ccdc_784396_784398_cif.txt' _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Hill, Michael' _publ_contact_author_email m.s.hill@bath.ac.uk _publ_section_title ; Magnesium hydride-promoted dearomatisation of pyridine ; _publ_author_name M.Hill # Attachment 'bigcif.cif' data_h10msh7 #TrackingRef '- C0CC03234D_ccdc_784396_784398_cif.txt' _database_code_depnum_ccdc_archive 'CCDC 784396' #TrackingRef 'bigcif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H55 Mg N3' _chemical_formula_weight 578.16 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' _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 12.7380(4) _cell_length_b 12.9120(5) _cell_length_c 22.1870(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.308(2) _cell_angle_gamma 90.00 _cell_volume 3649.1(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 159651 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 27.485 _exptl_crystal_description block _exptl_crystal_colour ? _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.052 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1264 _exptl_absorpt_coefficient_mu 0.076 # Absorption correction _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.510 _exptl_absorpt_correction_T_max 0.996 _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 50456 _diffrn_reflns_av_R_equivalents 0.1170 _diffrn_reflns_av_sigmaI/netI 0.0689 _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 -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 3.56 _diffrn_reflns_theta_max 27.47 _reflns_number_total 8271 _reflns_number_gt 5146 _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. Crystal was not a strong diffractor and this is evidenced in the R(int) value and in the final residuals. ; _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^)+(0.1061P)^2^+2.2078P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.021(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 8271 _refine_ls_number_parameters 380 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1312 _refine_ls_R_factor_gt 0.0801 _refine_ls_wR_factor_ref 0.2424 _refine_ls_wR_factor_gt 0.2098 _refine_ls_goodness_of_fit_ref 1.105 _refine_ls_restrained_S_all 1.105 _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 C1 C 0.4061(3) 0.3446(3) 0.50972(13) 0.0580(9) Uani 1 1 d . . . H1A H 0.4487 0.3953 0.4879 0.087 Uiso 1 1 calc R . . H1B H 0.4519 0.3011 0.5347 0.087 Uiso 1 1 calc R . . H1C H 0.3558 0.3809 0.5355 0.087 Uiso 1 1 calc R . . C2 C 0.3472(2) 0.2773(2) 0.46496(11) 0.0405(7) Uani 1 1 d . . . C3 C 0.2823(2) 0.2007(2) 0.48954(11) 0.0386(6) Uani 1 1 d . . . H3 H 0.2934 0.1873 0.5312 0.046 Uiso 1 1 calc R . . C4 C 0.2032(2) 0.1405(2) 0.46202(11) 0.0352(6) Uani 1 1 d . . . C5 C 0.1287(2) 0.0868(3) 0.50481(12) 0.0496(8) Uani 1 1 d . . . H5A H 0.0768 0.0472 0.4816 0.074 Uiso 1 1 calc R . . H5B H 0.0928 0.1387 0.5295 0.074 Uiso 1 1 calc R . . H5C H 0.1684 0.0397 0.5310 0.074 Uiso 1 1 calc R . . C6 C 0.4071(2) 0.3884(2) 0.38689(12) 0.0461(7) Uani 1 1 d . . . C7 C 0.5151(3) 0.3912(3) 0.37626(13) 0.0575(9) Uani 1 1 d . . . C8 C 0.5596(3) 0.4866(4) 0.35947(14) 0.0705(12) Uani 1 1 d . . . H8 H 0.6331 0.4905 0.3528 0.085 Uiso 1 1 calc R . . C9 C 0.4996(4) 0.5741(3) 0.35244(15) 0.0736(12) Uani 1 1 d . . . H9 H 0.5318 0.6380 0.3421 0.088 Uiso 1 1 calc R . . C10 C 0.3942(4) 0.5691(3) 0.36033(16) 0.0693(10) Uani 1 1 d . . . H10 H 0.3529 0.6296 0.3543 0.083 Uiso 1 1 calc R . . C11 C 0.3449(3) 0.4762(2) 0.37723(14) 0.0558(8) Uani 1 1 d . . . C12 C 0.5818(3) 0.2955(4) 0.38101(17) 0.0733(12) Uani 1 1 d . . . H12 H 0.5369 0.2392 0.3979 0.088 Uiso 1 1 calc R . . C13 C 0.6199(3) 0.2595(4) 0.3189(2) 0.0919(14) Uani 1 1 d . . . H13A H 0.6632 0.1972 0.3236 0.138 Uiso 1 1 calc R . . H13B H 0.6616 0.3145 0.3002 0.138 Uiso 1 1 calc R . . H13C H 0.5591 0.2437 0.2932 0.138 Uiso 1 1 calc R . . C14 C 0.6772(3) 0.3089(5) 0.4239(2) 0.121(2) Uani 1 1 d . . . H14A H 0.7175 0.2443 0.4252 0.182 Uiso 1 1 calc R . . H14B H 0.6524 0.3258 0.4645 0.182 Uiso 1 1 calc R . . H14C H 0.7220 0.3650 0.4091 0.182 Uiso 1 1 calc R . . C15 C 0.2272(3) 0.4735(3) 0.3841(2) 0.0702(10) Uani 1 1 d . . . H15 H 0.2058 0.3990 0.3845 0.084 Uiso 1 1 calc R . . C16 C 0.1696(4) 0.5250(4) 0.3311(2) 0.0889(13) Uani 1 1 d . . . H16A H 0.0937 0.5209 0.3376 0.133 Uiso 1 1 calc R . . H16B H 0.1875 0.4892 0.2936 0.133 Uiso 1 1 calc R . . H16C H 0.1908 0.5978 0.3283 0.133 Uiso 1 1 calc R . . C17 C 0.1906(4) 0.5212(3) 0.4436(2) 0.0896(14) Uani 1 1 d . . . H17A H 0.2272 0.4877 0.4772 0.134 Uiso 1 1 calc R . . H17B H 0.1147 0.5110 0.4478 0.134 Uiso 1 1 calc R . . H17C H 0.2063 0.5955 0.4437 0.134 Uiso 1 1 calc R . . C18 C 0.1014(2) 0.0786(2) 0.37882(11) 0.0385(6) Uani 1 1 d . . . C19 C 0.0152(2) 0.1371(3) 0.35711(12) 0.0457(7) Uani 1 1 d . . . C20 C -0.0707(3) 0.0836(3) 0.33359(14) 0.0584(9) Uani 1 1 d . . . H20 H -0.1299 0.1216 0.3197 0.070 Uiso 1 1 calc R . . C21 C -0.0721(3) -0.0232(3) 0.32990(15) 0.0636(10) Uani 1 1 d . . . H21 H -0.1322 -0.0580 0.3145 0.076 Uiso 1 1 calc R . . C22 C 0.0137(3) -0.0786(3) 0.34866(14) 0.0578(9) Uani 1 1 d . . . H22 H 0.0134 -0.1518 0.3448 0.069 Uiso 1 1 calc R . . C23 C 0.1023(3) -0.0295(2) 0.37355(12) 0.0480(7) Uani 1 1 d . . . C24 C 0.0171(2) 0.2537(2) 0.35878(14) 0.0497(7) Uani 1 1 d . . . H24 H 0.0916 0.2753 0.3521 0.060 Uiso 1 1 calc R . . C25 C -0.0486(3) 0.3046(3) 0.30920(18) 0.0718(11) Uani 1 1 d . . . H25A H -0.0435 0.3801 0.3127 0.108 Uiso 1 1 calc R . . H25B H -0.1221 0.2834 0.3133 0.108 Uiso 1 1 calc R . . H25C H -0.0225 0.2829 0.2697 0.108 Uiso 1 1 calc R . . C26 C -0.0153(3) 0.2969(3) 0.42051(16) 0.0661(10) Uani 1 1 d . . . H26A H -0.0125 0.3728 0.4195 0.099 Uiso 1 1 calc R . . H26B H 0.0329 0.2711 0.4516 0.099 Uiso 1 1 calc R . . H26C H -0.0869 0.2745 0.4297 0.099 Uiso 1 1 calc R . . C27 C 0.1970(3) -0.0930(2) 0.39031(15) 0.0561(8) Uani 1 1 d . . . H27 H 0.2493 -0.0460 0.4100 0.067 Uiso 1 1 calc R . . C28 C 0.2480(4) -0.1394(3) 0.33346(18) 0.0759(11) Uani 1 1 d . . . H28A H 0.3097 -0.1802 0.3451 0.114 Uiso 1 1 calc R . . H28B H 0.2695 -0.0833 0.3065 0.114 Uiso 1 1 calc R . . H28C H 0.1973 -0.1841 0.3127 0.114 Uiso 1 1 calc R . . C29 C 0.1711(4) -0.1796(3) 0.4346(2) 0.0835(13) Uani 1 1 d . . . H29A H 0.2351 -0.2184 0.4443 0.125 Uiso 1 1 calc R . . H29B H 0.1193 -0.2265 0.4164 0.125 Uiso 1 1 calc R . . H29C H 0.1422 -0.1497 0.4716 0.125 Uiso 1 1 calc R . . C30 C 0.2768(2) 0.2256(2) 0.25183(11) 0.0381(6) Uani 1 1 d . . . H30A H 0.2478 0.2967 0.2506 0.046 Uiso 1 1 calc R . . H30B H 0.3461 0.2279 0.2319 0.046 Uiso 1 1 calc R . . C31 C 0.2053(2) 0.1571(2) 0.21347(11) 0.0410(7) Uani 1 1 d . . . H31A H 0.2314 0.0850 0.2160 0.049 Uiso 1 1 calc R . . H31B H 0.1342 0.1582 0.2313 0.049 Uiso 1 1 calc R . . C32 C 0.1957(2) 0.1865(2) 0.14739(12) 0.0434(7) Uani 1 1 d . . . H32A H 0.2664 0.1833 0.1291 0.052 Uiso 1 1 calc R . . H32B H 0.1713 0.2592 0.1448 0.052 Uiso 1 1 calc R . . C33 C 0.1218(3) 0.1194(3) 0.11015(16) 0.0707(10) Uani 1 1 d . . . H33A H 0.1203 0.1445 0.0685 0.106 Uiso 1 1 calc R . . H33B H 0.0510 0.1229 0.1271 0.106 Uiso 1 1 calc R . . H33C H 0.1465 0.0475 0.1109 0.106 Uiso 1 1 calc R . . C34 C 0.4650(3) 0.0278(3) 0.30017(13) 0.0520(8) Uani 1 1 d . . . H34 H 0.4384 0.0512 0.2625 0.062 Uiso 1 1 calc R . . C35 C 0.5436(3) -0.0434(3) 0.29969(15) 0.0642(10) Uani 1 1 d . . . H35 H 0.5710 -0.0684 0.2627 0.077 Uiso 1 1 calc R . . C36 C 0.5827(3) -0.0783(3) 0.35400(16) 0.0737(11) Uani 1 1 d . . . H36 H 0.6376 -0.1280 0.3554 0.088 Uiso 1 1 calc R . . C37 C 0.5403(3) -0.0397(4) 0.40607(16) 0.0838(14) Uani 1 1 d . . . H37 H 0.5651 -0.0629 0.4442 0.101 Uiso 1 1 calc R . . C38 C 0.4618(3) 0.0325(3) 0.40247(13) 0.0649(10) Uani 1 1 d . . . H38 H 0.4339 0.0592 0.4389 0.078 Uiso 1 1 calc R . . N1 N 0.35715(17) 0.29402(18) 0.40574(9) 0.0382(5) Uani 1 1 d . . . N2 N 0.19087(16) 0.13305(17) 0.40256(9) 0.0345(5) Uani 1 1 d . . . N3 N 0.4225(2) 0.0672(2) 0.35029(10) 0.0470(6) Uani 1 1 d . . . Mg1 Mg 0.30301(7) 0.18694(7) 0.34401(4) 0.0334(3) 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 0.067(2) 0.081(2) 0.0257(14) -0.0088(14) -0.0031(13) -0.0231(18) C2 0.0426(15) 0.0549(17) 0.0241(12) -0.0059(11) -0.0012(11) -0.0027(13) C3 0.0458(15) 0.0509(16) 0.0191(12) -0.0007(11) -0.0004(10) 0.0028(13) C4 0.0424(14) 0.0389(14) 0.0244(12) 0.0028(10) 0.0031(10) 0.0038(12) C5 0.0618(19) 0.0581(19) 0.0290(14) 0.0033(13) 0.0054(13) -0.0107(15) C6 0.0567(18) 0.0582(19) 0.0234(13) -0.0059(12) -0.0021(12) -0.0182(15) C7 0.0545(19) 0.092(3) 0.0259(14) 0.0040(15) -0.0063(13) -0.0261(19) C8 0.068(2) 0.115(3) 0.0280(16) -0.0019(18) -0.0009(14) -0.050(2) C9 0.110(3) 0.077(3) 0.0340(17) -0.0018(17) -0.0028(19) -0.047(3) C10 0.103(3) 0.055(2) 0.050(2) -0.0080(16) 0.0013(19) -0.026(2) C11 0.076(2) 0.0463(18) 0.0448(17) -0.0078(14) 0.0029(15) -0.0162(17) C12 0.0427(18) 0.121(4) 0.057(2) 0.016(2) -0.0023(15) -0.015(2) C13 0.068(2) 0.122(4) 0.086(3) 0.009(3) 0.017(2) 0.002(3) C14 0.060(3) 0.216(7) 0.089(3) 0.027(4) -0.022(2) -0.006(3) C15 0.077(2) 0.0383(18) 0.095(3) -0.0087(18) 0.006(2) -0.0011(17) C16 0.094(3) 0.080(3) 0.093(3) -0.019(2) -0.014(3) 0.012(2) C17 0.108(3) 0.080(3) 0.081(3) 0.013(2) 0.025(3) 0.020(3) C18 0.0451(15) 0.0464(16) 0.0240(12) 0.0013(11) 0.0027(11) -0.0080(13) C19 0.0439(16) 0.0597(19) 0.0335(14) 0.0069(13) -0.0008(12) -0.0087(14) C20 0.0485(18) 0.083(3) 0.0441(17) 0.0147(16) -0.0093(14) -0.0142(17) C21 0.067(2) 0.081(3) 0.0427(18) 0.0032(17) -0.0087(16) -0.036(2) C22 0.083(2) 0.0531(19) 0.0369(16) -0.0005(14) 0.0016(16) -0.0262(18) C23 0.067(2) 0.0492(18) 0.0280(14) 0.0036(12) 0.0027(13) -0.0127(15) C24 0.0408(15) 0.0553(19) 0.0529(18) 0.0128(15) -0.0029(13) 0.0012(14) C25 0.069(2) 0.079(3) 0.067(2) 0.027(2) -0.0069(19) 0.007(2) C26 0.069(2) 0.068(2) 0.061(2) 0.0026(17) -0.0028(17) 0.0138(18) C27 0.079(2) 0.0394(17) 0.0502(18) -0.0001(14) -0.0004(16) -0.0032(16) C28 0.099(3) 0.055(2) 0.073(3) -0.0148(19) 0.010(2) 0.002(2) C29 0.122(4) 0.053(2) 0.076(3) 0.0220(19) -0.006(2) -0.002(2) C30 0.0456(15) 0.0431(15) 0.0254(12) 0.0025(11) -0.0004(11) 0.0005(12) C31 0.0471(16) 0.0491(16) 0.0268(13) 0.0013(11) 0.0020(11) -0.0016(13) C32 0.0505(16) 0.0530(17) 0.0265(13) 0.0003(12) -0.0039(11) 0.0022(14) C33 0.078(2) 0.089(3) 0.0454(19) -0.0047(18) -0.0158(17) -0.017(2) C34 0.0636(19) 0.063(2) 0.0289(14) -0.0023(13) -0.0011(13) 0.0162(16) C35 0.073(2) 0.080(2) 0.0402(17) -0.0083(16) 0.0060(16) 0.026(2) C36 0.080(3) 0.092(3) 0.049(2) -0.0043(19) -0.0055(17) 0.046(2) C37 0.103(3) 0.109(3) 0.0387(18) -0.0005(19) -0.0085(19) 0.059(3) C38 0.083(2) 0.087(3) 0.0246(14) -0.0017(15) -0.0021(14) 0.036(2) N1 0.0423(12) 0.0484(14) 0.0238(10) -0.0025(9) -0.0008(9) -0.0064(10) N2 0.0407(12) 0.0393(12) 0.0236(10) 0.0009(9) -0.0009(9) -0.0006(10) N3 0.0555(14) 0.0581(15) 0.0273(11) -0.0015(10) -0.0007(10) 0.0163(12) Mg1 0.0396(5) 0.0404(5) 0.0203(4) -0.0006(3) -0.0014(3) 0.0016(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.515(4) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 N1 1.338(3) . ? C2 C3 1.401(4) . ? C3 C4 1.409(4) . ? C3 H3 0.9500 . ? C4 N2 1.331(3) . ? C4 C5 1.514(4) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 C7 1.397(4) . ? C6 C11 1.400(5) . ? C6 N1 1.438(4) . ? C7 C8 1.407(5) . ? C7 C12 1.503(6) . ? C8 C9 1.373(6) . ? C8 H8 0.9500 . ? C9 C10 1.356(6) . ? C9 H9 0.9500 . ? C10 C11 1.406(5) . ? C10 H10 0.9500 . ? C11 C15 1.507(5) . ? C12 C13 1.536(6) . ? C12 C14 1.549(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 1.532(6) . ? C15 C16 1.533(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 C23 1.400(4) . ? C18 C19 1.415(4) . ? C18 N2 1.437(3) . ? C19 C20 1.393(4) . ? C19 C24 1.506(5) . ? C20 C21 1.382(5) . ? C20 H20 0.9500 . ? C21 C22 1.369(5) . ? C21 H21 0.9500 . ? C22 C23 1.404(4) . ? C22 H22 0.9500 . ? C23 C27 1.504(5) . ? C24 C25 1.528(4) . ? C24 C26 1.537(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 1.527(5) . ? C27 C28 1.543(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 1.526(4) . ? C30 Mg1 2.130(3) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 C32 1.519(4) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 C33 1.520(4) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 N3 1.339(4) . ? C34 C35 1.359(4) . ? C34 H34 0.9500 . ? C35 C36 1.377(5) . ? C35 H35 0.9500 . ? C36 C37 1.372(5) . ? C36 H36 0.9500 . ? C37 C38 1.369(5) . ? C37 H37 0.9500 . ? C38 N3 1.336(4) . ? C38 H38 0.9500 . ? N1 Mg1 2.062(2) . ? N2 Mg1 2.057(2) . ? N3 Mg1 2.174(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag 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 123.7(2) . . ? N1 C2 C1 120.1(3) . . ? C3 C2 C1 116.1(2) . . ? C2 C3 C4 130.0(2) . . ? C2 C3 H3 115.0 . . ? C4 C3 H3 115.0 . . ? N2 C4 C3 123.3(2) . . ? N2 C4 C5 121.1(2) . . ? C3 C4 C5 115.5(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 120.7(3) . . ? C7 C6 N1 120.6(3) . . ? C11 C6 N1 118.7(3) . . ? C6 C7 C8 117.8(4) . . ? C6 C7 C12 121.6(3) . . ? C8 C7 C12 120.6(3) . . ? C9 C8 C7 121.7(4) . . ? C9 C8 H8 119.2 . . ? C7 C8 H8 119.2 . . ? C10 C9 C8 119.9(4) . . ? C10 C9 H9 120.1 . . ? C8 C9 H9 120.1 . . ? C9 C10 C11 121.2(4) . . ? C9 C10 H10 119.4 . . ? C11 C10 H10 119.4 . . ? C6 C11 C10 118.6(3) . . ? C6 C11 C15 121.9(3) . . ? C10 C11 C15 119.5(3) . . ? C7 C12 C13 111.5(3) . . ? C7 C12 C14 113.2(4) . . ? C13 C12 C14 109.6(4) . . ? C7 C12 H12 107.4 . . ? C13 C12 H12 107.4 . . ? C14 C12 H12 107.4 . . ? 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 112.7(3) . . ? C11 C15 C16 112.7(4) . . ? C17 C15 C16 109.8(3) . . ? C11 C15 H15 107.1 . . ? C17 C15 H15 107.1 . . ? C16 C15 H15 107.1 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C23 C18 C19 120.7(3) . . ? C23 C18 N2 120.8(3) . . ? C19 C18 N2 118.4(2) . . ? C20 C19 C18 118.0(3) . . ? C20 C19 C24 121.2(3) . . ? C18 C19 C24 120.9(3) . . ? C21 C20 C19 121.8(3) . . ? C21 C20 H20 119.1 . . ? C19 C20 H20 119.1 . . ? C22 C21 C20 119.5(3) . . ? C22 C21 H21 120.3 . . ? C20 C21 H21 120.3 . . ? C21 C22 C23 121.5(3) . . ? C21 C22 H22 119.2 . . ? C23 C22 H22 119.2 . . ? C18 C23 C22 118.4(3) . . ? C18 C23 C27 122.0(3) . . ? C22 C23 C27 119.5(3) . . ? C19 C24 C25 113.8(3) . . ? C19 C24 C26 112.4(3) . . ? C25 C24 C26 109.7(3) . . ? C19 C24 H24 106.9 . . ? C25 C24 H24 106.9 . . ? C26 C24 H24 106.9 . . ? 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 112.5(3) . . ? C23 C27 C28 110.5(3) . . ? C29 C27 C28 109.6(3) . . ? 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 . . ? C31 C30 Mg1 119.36(18) . . ? C31 C30 H30A 107.5 . . ? Mg1 C30 H30A 107.5 . . ? C31 C30 H30B 107.5 . . ? Mg1 C30 H30B 107.5 . . ? H30A C30 H30B 107.0 . . ? C32 C31 C30 116.0(2) . . ? C32 C31 H31A 108.3 . . ? C30 C31 H31A 108.3 . . ? C32 C31 H31B 108.3 . . ? C30 C31 H31B 108.3 . . ? H31A C31 H31B 107.4 . . ? C31 C32 C33 115.4(3) . . ? C31 C32 H32A 108.4 . . ? C33 C32 H32A 108.4 . . ? C31 C32 H32B 108.4 . . ? C33 C32 H32B 108.4 . . ? H32A C32 H32B 107.5 . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C32 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? N3 C34 C35 124.3(3) . . ? N3 C34 H34 117.8 . . ? C35 C34 H34 117.8 . . ? C34 C35 C36 118.5(3) . . ? C34 C35 H35 120.7 . . ? C36 C35 H35 120.7 . . ? C37 C36 C35 118.4(3) . . ? C37 C36 H36 120.8 . . ? C35 C36 H36 120.8 . . ? C38 C37 C36 119.3(3) . . ? C38 C37 H37 120.4 . . ? C36 C37 H37 120.4 . . ? N3 C38 C37 123.3(3) . . ? N3 C38 H38 118.4 . . ? C37 C38 H38 118.4 . . ? C2 N1 C6 117.8(2) . . ? C2 N1 Mg1 120.70(19) . . ? C6 N1 Mg1 121.46(16) . . ? C4 N2 C18 119.2(2) . . ? C4 N2 Mg1 121.50(18) . . ? C18 N2 Mg1 119.10(15) . . ? C38 N3 C34 116.2(3) . . ? C38 N3 Mg1 123.6(2) . . ? C34 N3 Mg1 120.16(19) . . ? N2 Mg1 N1 92.19(9) . . ? N2 Mg1 C30 125.43(10) . . ? N1 Mg1 C30 122.07(11) . . ? N2 Mg1 N3 101.96(10) . . ? N1 Mg1 N3 101.70(10) . . ? C30 Mg1 N3 109.53(10) . . ? 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 -12.6(5) . . . . ? C1 C2 C3 C4 166.0(3) . . . . ? C2 C3 C4 N2 14.0(5) . . . . ? C2 C3 C4 C5 -163.7(3) . . . . ? C11 C6 C7 C8 4.1(4) . . . . ? N1 C6 C7 C8 -178.3(2) . . . . ? C11 C6 C7 C12 -174.5(3) . . . . ? N1 C6 C7 C12 3.1(4) . . . . ? C6 C7 C8 C9 -1.3(4) . . . . ? C12 C7 C8 C9 177.3(3) . . . . ? C7 C8 C9 C10 -1.6(5) . . . . ? C8 C9 C10 C11 1.7(5) . . . . ? C7 C6 C11 C10 -4.0(4) . . . . ? N1 C6 C11 C10 178.3(3) . . . . ? C7 C6 C11 C15 175.6(3) . . . . ? N1 C6 C11 C15 -2.0(4) . . . . ? C9 C10 C11 C6 1.1(5) . . . . ? C9 C10 C11 C15 -178.5(3) . . . . ? C6 C7 C12 C13 109.7(4) . . . . ? C8 C7 C12 C13 -68.9(4) . . . . ? C6 C7 C12 C14 -126.2(4) . . . . ? C8 C7 C12 C14 55.2(4) . . . . ? C6 C11 C15 C17 102.2(4) . . . . ? C10 C11 C15 C17 -78.2(4) . . . . ? C6 C11 C15 C16 -132.9(3) . . . . ? C10 C11 C15 C16 46.7(4) . . . . ? C23 C18 C19 C20 3.6(4) . . . . ? N2 C18 C19 C20 179.3(2) . . . . ? C23 C18 C19 C24 -175.7(3) . . . . ? N2 C18 C19 C24 0.0(4) . . . . ? C18 C19 C20 C21 -1.5(5) . . . . ? C24 C19 C20 C21 177.8(3) . . . . ? C19 C20 C21 C22 -1.3(5) . . . . ? C20 C21 C22 C23 2.2(5) . . . . ? C19 C18 C23 C22 -2.8(4) . . . . ? N2 C18 C23 C22 -178.4(2) . . . . ? C19 C18 C23 C27 173.6(3) . . . . ? N2 C18 C23 C27 -2.0(4) . . . . ? C21 C22 C23 C18 -0.1(4) . . . . ? C21 C22 C23 C27 -176.6(3) . . . . ? C20 C19 C24 C25 -27.9(4) . . . . ? C18 C19 C24 C25 151.4(3) . . . . ? C20 C19 C24 C26 97.4(3) . . . . ? C18 C19 C24 C26 -83.3(3) . . . . ? C18 C23 C27 C29 127.0(3) . . . . ? C22 C23 C27 C29 -56.6(4) . . . . ? C18 C23 C27 C28 -110.1(3) . . . . ? C22 C23 C27 C28 66.3(4) . . . . ? Mg1 C30 C31 C32 -176.6(2) . . . . ? C30 C31 C32 C33 -178.4(3) . . . . ? N3 C34 C35 C36 0.3(6) . . . . ? C34 C35 C36 C37 0.0(7) . . . . ? C35 C36 C37 C38 -0.6(7) . . . . ? C36 C37 C38 N3 0.9(7) . . . . ? C3 C2 N1 C6 166.5(3) . . . . ? C1 C2 N1 C6 -12.1(4) . . . . ? C3 C2 N1 Mg1 -13.9(4) . . . . ? C1 C2 N1 Mg1 167.5(2) . . . . ? C7 C6 N1 C2 92.3(3) . . . . ? C11 C6 N1 C2 -90.1(3) . . . . ? C7 C6 N1 Mg1 -87.3(3) . . . . ? C11 C6 N1 Mg1 90.3(3) . . . . ? C3 C4 N2 C18 -173.5(2) . . . . ? C5 C4 N2 C18 4.0(4) . . . . ? C3 C4 N2 Mg1 11.7(4) . . . . ? C5 C4 N2 Mg1 -170.8(2) . . . . ? C23 C18 N2 C4 -82.6(3) . . . . ? C19 C18 N2 C4 101.6(3) . . . . ? C23 C18 N2 Mg1 92.2(3) . . . . ? C19 C18 N2 Mg1 -83.5(3) . . . . ? C37 C38 N3 C34 -0.5(6) . . . . ? C37 C38 N3 Mg1 -177.1(3) . . . . ? C35 C34 N3 C38 -0.1(5) . . . . ? C35 C34 N3 Mg1 176.6(3) . . . . ? C4 N2 Mg1 N1 -26.3(2) . . . . ? C18 N2 Mg1 N1 158.9(2) . . . . ? C4 N2 Mg1 C30 -159.1(2) . . . . ? C18 N2 Mg1 C30 26.1(2) . . . . ? C4 N2 Mg1 N3 76.1(2) . . . . ? C18 N2 Mg1 N3 -98.6(2) . . . . ? C2 N1 Mg1 N2 27.2(2) . . . . ? C6 N1 Mg1 N2 -153.1(2) . . . . ? C2 N1 Mg1 C30 162.4(2) . . . . ? C6 N1 Mg1 C30 -18.0(3) . . . . ? C2 N1 Mg1 N3 -75.4(2) . . . . ? C6 N1 Mg1 N3 104.2(2) . . . . ? C31 C30 Mg1 N2 -40.2(3) . . . . ? C31 C30 Mg1 N1 -160.26(19) . . . . ? C31 C30 Mg1 N3 81.3(2) . . . . ? C38 N3 Mg1 N2 -50.6(3) . . . . ? C34 N3 Mg1 N2 133.0(2) . . . . ? C38 N3 Mg1 N1 44.2(3) . . . . ? C34 N3 Mg1 N1 -132.2(2) . . . . ? C38 N3 Mg1 C30 174.6(3) . . . . ? C34 N3 Mg1 C30 -1.8(3) . . . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.456 _refine_diff_density_min -0.332 _refine_diff_density_rms 0.080 #=== end data_k10msh6 _database_code_depnum_ccdc_archive 'CCDC 784397' #TrackingRef 'bigcif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C39 H52 Mg N4' _chemical_formula_weight 601.16 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' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbnm 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 9.6737(2) _cell_length_b 18.2623(4) _cell_length_c 20.6525(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3648.55(13) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 50345 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 27.485 _exptl_crystal_description needle _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.094 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1304 _exptl_absorpt_coefficient_mu 0.079 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.704 _exptl_absorpt_correction_T_max 0.997 _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 39041 _diffrn_reflns_av_R_equivalents 0.0918 _diffrn_reflns_av_sigmaI/netI 0.0341 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 4.08 _diffrn_reflns_theta_max 25.03 _reflns_number_total 3303 _reflns_number_gt 2613 _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. Asymmetric unit = 1/2 of a molecule, with atoms the magnesium, nitrogen, carbons 18-23 (plus associated hydrogens) located on a mirror plane implicit in the space group. Hydrogens 3, 16, 17, 18a and 18b were all evident in the penultimate difference Fourier map, but ultimately included at calculated positions. The methyl protons attached to C1 are modeled as being disordered over 2 sites. ; _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^)+(0.0465P)^2^+2.1798P] 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 3303 _refine_ls_number_parameters 218 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0662 _refine_ls_R_factor_gt 0.0476 _refine_ls_wR_factor_ref 0.1268 _refine_ls_wR_factor_gt 0.1111 _refine_ls_goodness_of_fit_ref 1.068 _refine_ls_restrained_S_all 1.068 _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 0.63507(9) 0.08988(4) 0.2500 0.0280(2) Uani 1 2 d S . . N1 N 0.65883(16) 0.16361(8) 0.17691(7) 0.0298(4) Uani 1 1 d . . . N2 N 0.4901(2) 0.01229(12) 0.2500 0.0347(5) Uani 1 2 d S . . N3 N 0.8244(2) 0.02949(12) 0.2500 0.0333(5) Uani 1 2 d S . . C1 C 0.7696(2) 0.27426(12) 0.13188(10) 0.0468(5) Uani 1 1 d . . . H1A H 0.7385 0.2524 0.0911 0.070 Uiso 0.50 1 calc PR . . H1B H 0.8704 0.2795 0.1312 0.070 Uiso 0.50 1 calc PR . . H1C H 0.7269 0.3225 0.1372 0.070 Uiso 0.50 1 calc PR . . H1D H 0.8187 0.3172 0.1486 0.070 Uiso 0.50 1 calc PR . . H1E H 0.6868 0.2901 0.1085 0.070 Uiso 0.50 1 calc PR . . H1F H 0.8303 0.2471 0.1024 0.070 Uiso 0.50 1 calc PR . . C2 C 0.7280(2) 0.22524(10) 0.18787(9) 0.0324(4) Uani 1 1 d . . . C3 C 0.7661(3) 0.25003(14) 0.2500 0.0341(6) Uani 1 2 d S . . H3 H 0.8282 0.2903 0.2500 0.041 Uiso 1 2 calc SR . . C4 C 0.6070(2) 0.14819(10) 0.11260(8) 0.0333(4) Uani 1 1 d . . . C5 C 0.6857(2) 0.10697(11) 0.06849(9) 0.0416(5) Uani 1 1 d . . . C6 C 0.6276(3) 0.08987(13) 0.00866(10) 0.0524(6) Uani 1 1 d . . . H6 H 0.6802 0.0625 -0.0217 0.063 Uiso 1 1 calc R . . C7 C 0.4963(3) 0.11168(14) -0.00746(10) 0.0546(6) Uani 1 1 d . . . H7 H 0.4587 0.0994 -0.0485 0.065 Uiso 1 1 calc R . . C8 C 0.4193(2) 0.15150(13) 0.03632(10) 0.0497(6) Uani 1 1 d . . . H8 H 0.3284 0.1664 0.0250 0.060 Uiso 1 1 calc R . . C9 C 0.4725(2) 0.17027(11) 0.09679(9) 0.0397(5) Uani 1 1 d . . . C10 C 0.8297(2) 0.07927(14) 0.08442(10) 0.0508(6) Uani 1 1 d . . . H10 H 0.8544 0.0978 0.1285 0.061 Uiso 1 1 calc R . . C11 C 0.9384(3) 0.10730(17) 0.03717(12) 0.0681(8) Uani 1 1 d . . . H11A H 0.9169 0.0898 -0.0065 0.102 Uiso 1 1 calc R . . H11B H 1.0297 0.0892 0.0501 0.102 Uiso 1 1 calc R . . H11C H 0.9387 0.1610 0.0375 0.102 Uiso 1 1 calc R . . C12 C 0.8316(3) -0.00459(15) 0.08707(12) 0.0653(7) Uani 1 1 d . . . H12A H 0.8149 -0.0243 0.0436 0.098 Uiso 1 1 calc R . . H12B H 0.7591 -0.0218 0.1166 0.098 Uiso 1 1 calc R . . H12C H 0.9219 -0.0213 0.1027 0.098 Uiso 1 1 calc R . . C13 C 0.3840(2) 0.21507(13) 0.14355(10) 0.0475(6) Uani 1 1 d . . . H13 H 0.4331 0.2162 0.1861 0.057 Uiso 1 1 calc R . . C14 C 0.2450(4) 0.18126(19) 0.15465(19) 0.0991(12) Uani 1 1 d . . . H14A H 0.1952 0.2092 0.1878 0.149 Uiso 1 1 calc R . . H14B H 0.2567 0.1306 0.1693 0.149 Uiso 1 1 calc R . . H14C H 0.1922 0.1818 0.1142 0.149 Uiso 1 1 calc R . . C15 C 0.3687(4) 0.29344(16) 0.12067(18) 0.0888(11) Uani 1 1 d . . . H15A H 0.3126 0.2945 0.0812 0.133 Uiso 1 1 calc R . . H15B H 0.4602 0.3140 0.1116 0.133 Uiso 1 1 calc R . . H15C H 0.3233 0.3225 0.1544 0.133 Uiso 1 1 calc R . . C16 C 0.4644(2) -0.02788(11) 0.19405(9) 0.0400(5) Uani 1 1 d . . . H16 H 0.4760 -0.0031 0.1540 0.048 Uiso 1 1 calc R . . C17 C 0.4251(2) -0.09792(12) 0.19126(11) 0.0462(5) Uani 1 1 d . . . H17 H 0.4129 -0.1197 0.1499 0.055 Uiso 1 1 calc R . . C18 C 0.3994(3) -0.14363(16) 0.2500 0.0436(7) Uani 1 2 d S . . H18A H 0.3028 -0.1615 0.2500 0.052 Uiso 1 2 calc SR . . H18B H 0.4618 -0.1866 0.2500 0.052 Uiso 1 2 calc SR . . C19 C 0.9482(3) 0.06310(16) 0.2500 0.0387(7) Uani 1 2 d S . . H19 H 0.9502 0.1151 0.2500 0.046 Uiso 1 2 calc SR . . C20 C 1.0713(3) 0.02632(17) 0.2500 0.0477(8) Uani 1 2 d S . . H20 H 1.1566 0.0521 0.2500 0.057 Uiso 1 2 calc SR . . C21 C 1.0685(4) -0.04940(19) 0.2500 0.0574(9) Uani 1 2 d S . . H21 H 1.1523 -0.0765 0.2500 0.069 Uiso 1 2 calc SR . . C22 C 0.9440(3) -0.08496(17) 0.2500 0.0515(8) Uani 1 2 d S . . H22 H 0.9404 -0.1369 0.2500 0.062 Uiso 1 2 calc SR . . C23 C 0.8244(3) -0.04438(15) 0.2500 0.0396(7) Uani 1 2 d S . . H23 H 0.7383 -0.0693 0.2500 0.047 Uiso 1 2 calc SR . . 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 0.0318(5) 0.0269(4) 0.0253(4) 0.000 0.000 -0.0007(4) N1 0.0349(9) 0.0307(8) 0.0239(7) 0.0010(6) 0.0018(6) 0.0017(7) N2 0.0355(13) 0.0361(12) 0.0325(11) 0.000 0.000 -0.0062(10) N3 0.0350(13) 0.0295(11) 0.0353(12) 0.000 0.000 0.0010(10) C1 0.0514(13) 0.0435(12) 0.0455(12) 0.0112(10) 0.0076(10) -0.0074(10) C2 0.0314(10) 0.0311(10) 0.0347(10) 0.0041(8) 0.0068(8) 0.0034(8) C3 0.0310(14) 0.0284(13) 0.0428(15) 0.000 0.000 -0.0037(11) C4 0.0427(11) 0.0328(10) 0.0245(9) 0.0026(7) 0.0029(8) 0.0009(8) C5 0.0476(12) 0.0465(12) 0.0308(10) -0.0014(8) 0.0023(9) 0.0088(10) C6 0.0637(16) 0.0629(15) 0.0306(11) -0.0101(10) 0.0026(10) 0.0122(12) C7 0.0617(15) 0.0723(16) 0.0296(10) -0.0072(10) -0.0070(10) 0.0048(13) C8 0.0483(13) 0.0685(15) 0.0322(11) 0.0004(10) -0.0054(9) 0.0095(11) C9 0.0451(12) 0.0462(11) 0.0278(9) 0.0044(8) 0.0015(9) 0.0056(9) C10 0.0499(14) 0.0693(15) 0.0333(11) -0.0091(10) 0.0016(9) 0.0185(12) C11 0.0523(15) 0.102(2) 0.0498(14) -0.0092(14) 0.0075(12) 0.0155(15) C12 0.0743(18) 0.0728(17) 0.0489(14) -0.0105(12) 0.0000(12) 0.0315(14) C13 0.0442(12) 0.0672(15) 0.0313(10) -0.0007(9) -0.0017(9) 0.0169(11) C14 0.095(2) 0.086(2) 0.116(3) -0.023(2) 0.070(2) -0.0216(19) C15 0.093(2) 0.0597(17) 0.113(3) -0.0044(16) 0.054(2) 0.0114(16) C16 0.0394(11) 0.0473(12) 0.0334(10) -0.0029(9) 0.0021(9) -0.0107(9) C17 0.0416(12) 0.0516(13) 0.0455(12) -0.0145(10) 0.0095(10) -0.0135(10) C18 0.0271(15) 0.0356(15) 0.068(2) 0.000 0.000 -0.0003(12) C19 0.0420(17) 0.0333(15) 0.0407(15) 0.000 0.000 -0.0029(12) C20 0.0334(17) 0.0465(18) 0.063(2) 0.000 0.000 -0.0036(13) C21 0.0421(19) 0.0477(19) 0.083(2) 0.000 0.000 0.0114(15) C22 0.0470(19) 0.0321(16) 0.075(2) 0.000 0.000 0.0075(14) C23 0.0382(16) 0.0314(15) 0.0490(17) 0.000 0.000 -0.0005(12) _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 N2 1.993(2) . ? Mg1 N1 2.0358(15) 6_556 ? Mg1 N1 2.0358(15) . ? Mg1 N3 2.138(2) . ? N1 C2 1.329(2) . ? N1 C4 1.447(2) . ? N2 C16 1.391(2) 6_556 ? N2 C16 1.391(2) . ? N3 C19 1.346(4) . ? N3 C23 1.349(3) . ? C1 C2 1.517(3) . ? 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 C2 1.410(2) 6_556 ? C3 H3 0.9500 . ? C4 C9 1.401(3) . ? C4 C5 1.405(3) . ? C5 C6 1.392(3) . ? C5 C10 1.518(3) . ? C6 C7 1.372(3) . ? C6 H6 0.9500 . ? C7 C8 1.379(3) . ? C7 H7 0.9500 . ? C8 C9 1.393(3) . ? C8 H8 0.9500 . ? C9 C13 1.528(3) . ? C10 C11 1.524(3) . ? C10 C12 1.533(4) . ? C10 H10 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.497(4) . ? C13 C15 1.514(4) . ? C13 H13 1.0000 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.336(3) . ? C16 H16 0.9500 . ? C17 C18 1.493(3) . ? C17 H17 0.9500 . ? C18 C17 1.493(3) 6_556 ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.367(4) . ? C19 H19 0.9500 . ? C20 C21 1.383(5) . ? C20 H20 0.9500 . ? C21 C22 1.368(5) . ? C21 H21 0.9500 . ? C22 C23 1.374(4) . ? C22 H22 0.9500 . ? C23 H23 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 N2 Mg1 N1 123.34(6) . 6_556 ? N2 Mg1 N1 123.34(6) . . ? N1 Mg1 N1 95.72(9) 6_556 . ? N2 Mg1 N3 103.65(10) . . ? N1 Mg1 N3 104.15(6) 6_556 . ? N1 Mg1 N3 104.15(6) . . ? C2 N1 C4 119.70(15) . . ? C2 N1 Mg1 119.39(12) . . ? C4 N1 Mg1 120.84(11) . . ? C16 N2 C16 112.3(2) 6_556 . ? C16 N2 Mg1 120.03(12) 6_556 . ? C16 N2 Mg1 120.03(12) . . ? C19 N3 C23 117.1(2) . . ? C19 N3 Mg1 121.81(18) . . ? C23 N3 Mg1 121.0(2) . . ? 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 123.98(17) . . ? N1 C2 C1 120.25(17) . . ? C3 C2 C1 115.77(18) . . ? C2 C3 C2 131.0(2) 6_556 . ? C2 C3 H3 114.5 6_556 . ? C2 C3 H3 114.5 . . ? C9 C4 C5 120.38(18) . . ? C9 C4 N1 118.65(16) . . ? C5 C4 N1 120.79(17) . . ? C6 C5 C4 118.5(2) . . ? C6 C5 C10 119.17(19) . . ? C4 C5 C10 122.31(18) . . ? C7 C6 C5 121.6(2) . . ? C7 C6 H6 119.2 . . ? C5 C6 H6 119.2 . . ? C6 C7 C8 119.6(2) . . ? C6 C7 H7 120.2 . . ? C8 C7 H7 120.2 . . ? C7 C8 C9 121.2(2) . . ? C7 C8 H8 119.4 . . ? C9 C8 H8 119.4 . . ? C8 C9 C4 118.73(19) . . ? C8 C9 C13 119.45(19) . . ? C4 C9 C13 121.82(18) . . ? C5 C10 C11 112.52(19) . . ? C5 C10 C12 110.6(2) . . ? C11 C10 C12 110.5(2) . . ? C5 C10 H10 107.7 . . ? C11 C10 H10 107.7 . . ? C12 C10 H10 107.7 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C14 C13 C15 110.5(2) . . ? C14 C13 C9 112.3(2) . . ? C15 C13 C9 111.33(19) . . ? C14 C13 H13 107.5 . . ? C15 C13 H13 107.5 . . ? C9 C13 H13 107.5 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C17 C16 N2 126.28(19) . . ? C17 C16 H16 116.9 . . ? N2 C16 H16 116.9 . . ? C16 C17 C18 123.2(2) . . ? C16 C17 H17 118.4 . . ? C18 C17 H17 118.4 . . ? C17 C18 C17 108.6(2) 6_556 . ? C17 C18 H18A 110.0 6_556 . ? C17 C18 H18A 110.0 . . ? C17 C18 H18B 110.0 6_556 . ? C17 C18 H18B 110.0 . . ? H18A C18 H18B 108.3 . . ? N3 C19 C20 123.4(3) . . ? N3 C19 H19 118.3 . . ? C20 C19 H19 118.3 . . ? C19 C20 C21 118.3(3) . . ? C19 C20 H20 120.8 . . ? C21 C20 H20 120.8 . . ? C22 C21 C20 119.5(3) . . ? C22 C21 H21 120.3 . . ? C20 C21 H21 120.3 . . ? C21 C22 C23 119.0(3) . . ? C21 C22 H22 120.5 . . ? C23 C22 H22 120.5 . . ? N3 C23 C22 122.6(3) . . ? N3 C23 H23 118.7 . . ? C22 C23 H23 118.7 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Mg1 N1 C2 160.57(14) . . . . ? N1 Mg1 N1 C2 23.94(17) 6_556 . . . ? N3 Mg1 N1 C2 -82.23(14) . . . . ? N2 Mg1 N1 C4 -22.31(18) . . . . ? N1 Mg1 N1 C4 -158.94(11) 6_556 . . . ? N3 Mg1 N1 C4 94.89(14) . . . . ? N1 Mg1 N2 C16 -43.8(2) 6_556 . . 6_556 ? N1 Mg1 N2 C16 -168.93(16) . . . 6_556 ? N3 Mg1 N2 C16 73.63(18) . . . 6_556 ? N1 Mg1 N2 C16 168.93(16) 6_556 . . . ? N1 Mg1 N2 C16 43.8(2) . . . . ? N3 Mg1 N2 C16 -73.63(18) . . . . ? N2 Mg1 N3 C19 180.0 . . . . ? N1 Mg1 N3 C19 -49.88(5) 6_556 . . . ? N1 Mg1 N3 C19 49.88(5) . . . . ? N2 Mg1 N3 C23 0.0 . . . . ? N1 Mg1 N3 C23 130.12(5) 6_556 . . . ? N1 Mg1 N3 C23 -130.12(5) . . . . ? C4 N1 C2 C3 171.0(2) . . . . ? Mg1 N1 C2 C3 -11.8(3) . . . . ? C4 N1 C2 C1 -8.3(3) . . . . ? Mg1 N1 C2 C1 168.81(15) . . . . ? N1 C2 C3 C2 -10.1(4) . . . 6_556 ? C1 C2 C3 C2 169.3(2) . . . 6_556 ? C2 N1 C4 C9 -92.0(2) . . . . ? Mg1 N1 C4 C9 90.93(19) . . . . ? C2 N1 C4 C5 92.9(2) . . . . ? Mg1 N1 C4 C5 -84.2(2) . . . . ? C9 C4 C5 C6 1.1(3) . . . . ? N1 C4 C5 C6 176.12(19) . . . . ? C9 C4 C5 C10 -177.6(2) . . . . ? N1 C4 C5 C10 -2.5(3) . . . . ? C4 C5 C6 C7 -0.6(4) . . . . ? C10 C5 C6 C7 178.1(2) . . . . ? C5 C6 C7 C8 0.0(4) . . . . ? C6 C7 C8 C9 0.1(4) . . . . ? C7 C8 C9 C4 0.3(3) . . . . ? C7 C8 C9 C13 179.4(2) . . . . ? C5 C4 C9 C8 -0.9(3) . . . . ? N1 C4 C9 C8 -176.07(18) . . . . ? C5 C4 C9 C13 179.96(19) . . . . ? N1 C4 C9 C13 4.8(3) . . . . ? C6 C5 C10 C11 60.2(3) . . . . ? C4 C5 C10 C11 -121.2(2) . . . . ? C6 C5 C10 C12 -63.9(3) . . . . ? C4 C5 C10 C12 114.7(2) . . . . ? C8 C9 C13 C14 53.3(3) . . . . ? C4 C9 C13 C14 -127.6(3) . . . . ? C8 C9 C13 C15 -71.2(3) . . . . ? C4 C9 C13 C15 107.9(3) . . . . ? C16 N2 C16 C17 -2.7(4) 6_556 . . . ? Mg1 N2 C16 C17 146.9(2) . . . . ? N2 C16 C17 C18 1.5(4) . . . . ? C16 C17 C18 C17 0.0(4) . . . 6_556 ? C23 N3 C19 C20 0.0 . . . . ? Mg1 N3 C19 C20 180.0 . . . . ? N3 C19 C20 C21 0.0 . . . . ? C19 C20 C21 C22 0.0 . . . . ? C20 C21 C22 C23 0.0 . . . . ? C19 N3 C23 C22 0.0 . . . . ? Mg1 N3 C23 C22 180.0 . . . . ? C21 C22 C23 N3 0.0 . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.217 _refine_diff_density_min -0.278 _refine_diff_density_rms 0.039 #===end data_h10msh24 _database_code_depnum_ccdc_archive 'CCDC 784398' #TrackingRef 'bigcif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C39 H52 Mg N4' _chemical_formula_weight 601.16 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' '-x, -y, -z' 'x, -y-1/2, z' _cell_length_a 9.4213(2) _cell_length_b 20.5902(6) _cell_length_c 9.9732(2) _cell_angle_alpha 90.00 _cell_angle_beta 109.844(2) _cell_angle_gamma 90.00 _cell_volume 1819.79(8) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 45768 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 27.485 _exptl_crystal_description block _exptl_crystal_colour ? _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.097 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 652 _exptl_absorpt_coefficient_mu 0.080 # Absorption correction _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.830 _exptl_absorpt_correction_T_max 0.992 _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 32152 _diffrn_reflns_av_R_equivalents 0.0617 _diffrn_reflns_av_sigmaI/netI 0.0350 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 3.93 _diffrn_reflns_theta_max 27.47 _reflns_number_total 4267 _reflns_number_gt 3118 _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 in this structure consists of half of a molecule. Atoms Mg1, N2, C18 and C3 are located on a mirror plane -- intrinsic to the space group symmetry. The combination of symmetry within the molecule, and possible disorder, meant that treatment of the dearomatised pyridine provided that challenges in this structure. However, there is ample crystallographic evidence for the dearomatisation. Larger than normal ADPs are recorded for C16-18 -- a combination of asymmetry with the ring based on N3, and some disorder. The hydrogens on C16 were readily located, and have been refined at 0.98\%A from the parent atom. It was evident that one of these hydrogens is present at full occupancy, and one at half-occupancy. The full occupancy candidate (H16B) presents at an average position for an aromatic CH, or one hydrogen of a CH2 pair. The half occupancy H16A is clearly only present half of the time -- i.e. only one half of the pyridine ring has been reduced. H16a-H16b are closer to each other than one would expect for a CH2 group -- however, this is reasonable considering the comments herein. No additional attempts were made to restrain the H...H distance herein. ; _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^)+(0.0644P)^2^+0.8362P] 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 0.026(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4267 _refine_ls_number_parameters 227 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0806 _refine_ls_R_factor_gt 0.0537 _refine_ls_wR_factor_ref 0.1456 _refine_ls_wR_factor_gt 0.1292 _refine_ls_goodness_of_fit_ref 1.005 _refine_ls_restrained_S_all 1.005 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.5481(2) 0.13175(9) 0.5838(2) 0.0456(5) Uani 1 1 d . . . H1A H 0.4985 0.0909 0.5436 0.068 Uiso 0.50 1 calc PR . . H1B H 0.5457 0.1372 0.6806 0.068 Uiso 0.50 1 calc PR . . H1C H 0.6531 0.1309 0.5867 0.068 Uiso 0.50 1 calc PR . . H1D H 0.6330 0.1485 0.6636 0.068 Uiso 0.50 1 calc PR . . H1E H 0.5859 0.1021 0.5267 0.068 Uiso 0.50 1 calc PR . . H1F H 0.4784 0.1084 0.6206 0.068 Uiso 0.50 1 calc PR . . C2 C 0.46617(18) 0.18779(8) 0.49166(16) 0.0321(4) Uani 1 1 d . . . C3 C 0.5255(3) 0.2500 0.5369(2) 0.0335(5) Uani 1 2 d S . . H3 H 0.6215 0.2500 0.6101 0.040 Uiso 1 2 calc SR . . C4 C 0.27913(19) 0.11354(8) 0.34698(18) 0.0370(4) Uani 1 1 d . . . C5 C 0.3287(2) 0.06806(8) 0.2681(2) 0.0429(4) Uani 1 1 d . . . C6 C 0.2492(3) 0.00963(10) 0.2313(3) 0.0619(6) Uani 1 1 d . . . H6 H 0.2812 -0.0219 0.1780 0.074 Uiso 1 1 calc R . . C7 C 0.1257(3) -0.00315(11) 0.2706(4) 0.0862(9) Uani 1 1 d . . . H7 H 0.0732 -0.0431 0.2443 0.103 Uiso 1 1 calc R . . C8 C 0.0784(3) 0.04163(11) 0.3476(4) 0.0826(9) Uani 1 1 d . . . H8 H -0.0072 0.0322 0.3741 0.099 Uiso 1 1 calc R . . C9 C 0.1526(2) 0.10050(9) 0.3880(3) 0.0551(6) Uani 1 1 d . . . C10 C 0.4618(2) 0.08029(9) 0.2193(2) 0.0490(5) Uani 1 1 d . . . H10 H 0.5064 0.1233 0.2579 0.059 Uiso 1 1 calc R . . C11 C 0.5849(3) 0.02860(10) 0.2753(3) 0.0589(6) Uani 1 1 d . . . H11A H 0.6170 0.0270 0.3796 0.088 Uiso 1 1 calc R . . H11B H 0.6714 0.0396 0.2462 0.088 Uiso 1 1 calc R . . H11C H 0.5449 -0.0139 0.2359 0.088 Uiso 1 1 calc R . . C12 C 0.4108(4) 0.08363(11) 0.0560(2) 0.0779(8) Uani 1 1 d . . . H12A H 0.3734 0.0410 0.0158 0.117 Uiso 1 1 calc R . . H12B H 0.4964 0.0962 0.0269 0.117 Uiso 1 1 calc R . . H12C H 0.3301 0.1159 0.0211 0.117 Uiso 1 1 calc R . . C13 C 0.0989(3) 0.14845(10) 0.4769(3) 0.0688(7) Uani 1 1 d . . . H13 H 0.1396 0.1923 0.4665 0.083 Uiso 1 1 calc R . . C14 C 0.1581(3) 0.13035(15) 0.6319(3) 0.0884(9) Uani 1 1 d . . . H14A H 0.1210 0.0871 0.6445 0.133 Uiso 1 1 calc R . . H14B H 0.1234 0.1622 0.6870 0.133 Uiso 1 1 calc R . . H14C H 0.2687 0.1300 0.6654 0.133 Uiso 1 1 calc R . . C15 C -0.0737(3) 0.15318(19) 0.4255(3) 0.1003(11) Uani 1 1 d . . . H15A H -0.1128 0.1567 0.3213 0.150 Uiso 1 1 calc R . . H15B H -0.1035 0.1917 0.4674 0.150 Uiso 1 1 calc R . . H15C H -0.1152 0.1142 0.4548 0.150 Uiso 1 1 calc R . . C16 C -0.0094(2) 0.19335(11) 0.0224(2) 0.0535(5) Uani 1 1 d D . . H16A H -0.103(3) 0.182(3) 0.039(5) 0.088(17) Uiso 0.50 1 d PD . . H16B H 0.028(2) 0.1539(6) 0.078(2) 0.060(6) Uiso 1 1 d D . . C17 C -0.0647(3) 0.19302(16) -0.1258(3) 0.0809(8) Uani 1 1 d . . . H17 H -0.0906 0.1529 -0.1753 0.097 Uiso 1 1 calc R . . C18 C -0.0825(3) 0.2500 -0.2016(4) 0.0841(14) Uani 1 2 d S . . H18 H -0.1061 0.2500 -0.3021 0.101 Uiso 1 2 calc SR . . C19 C 0.3421(3) 0.2500 -0.0390(2) 0.0352(5) Uani 1 2 d S . . H19 H 0.2355 0.2500 -0.0832 0.042 Uiso 1 2 calc SR . . C20 C 0.4306(3) 0.2500 -0.1244(3) 0.0418(6) Uani 1 2 d S . . H20 H 0.3855 0.2500 -0.2253 0.050 Uiso 1 2 calc SR . . C21 C 0.5851(3) 0.2500 -0.0615(3) 0.0492(7) Uani 1 2 d S . . H21 H 0.6484 0.2500 -0.1181 0.059 Uiso 1 2 calc SR . . C22 C 0.6469(3) 0.2500 0.0863(3) 0.0502(7) Uani 1 2 d S . . H22 H 0.7532 0.2500 0.1327 0.060 Uiso 1 2 calc SR . . C23 C 0.5512(3) 0.2500 0.1641(3) 0.0388(6) Uani 1 2 d S . . H23 H 0.5941 0.2500 0.2651 0.047 Uiso 1 2 calc SR . . N1 N 0.34598(14) 0.17704(6) 0.37657(13) 0.0300(3) Uani 1 1 d . . . N2 N 0.0504(2) 0.2500 0.0976(2) 0.0352(4) Uani 1 2 d S . . N3 N 0.4004(2) 0.2500 0.10447(19) 0.0311(4) Uani 1 2 d S . . Mg1 Mg 0.26159(8) 0.2500 0.23420(7) 0.0273(2) Uani 1 2 d S . . 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 0.0436(10) 0.0404(10) 0.0472(10) 0.0126(8) 0.0083(8) 0.0025(8) C2 0.0345(8) 0.0341(9) 0.0306(8) 0.0052(6) 0.0147(7) 0.0035(7) C3 0.0310(12) 0.0388(13) 0.0295(11) 0.000 0.0084(9) 0.000 C4 0.0379(9) 0.0258(8) 0.0440(9) 0.0068(7) 0.0097(7) 0.0008(7) C5 0.0512(11) 0.0261(9) 0.0470(10) 0.0015(7) 0.0109(8) 0.0008(7) C6 0.0656(14) 0.0284(10) 0.0820(16) -0.0067(10) 0.0124(12) -0.0006(9) C7 0.0559(14) 0.0307(12) 0.162(3) -0.0051(14) 0.0238(16) -0.0123(10) C8 0.0533(13) 0.0331(11) 0.170(3) 0.0116(14) 0.0497(16) -0.0025(10) C9 0.0465(11) 0.0286(10) 0.0953(16) 0.0130(10) 0.0309(11) 0.0023(8) C10 0.0740(13) 0.0290(9) 0.0520(11) -0.0038(8) 0.0317(10) 0.0014(9) C11 0.0711(14) 0.0410(11) 0.0754(15) -0.0025(10) 0.0388(12) 0.0058(10) C12 0.144(3) 0.0443(13) 0.0553(13) -0.0019(10) 0.0462(15) 0.0115(14) C13 0.0634(14) 0.0358(11) 0.132(2) 0.0161(12) 0.0652(15) 0.0041(10) C14 0.0658(16) 0.0783(19) 0.107(2) -0.0298(17) 0.0113(15) 0.0050(14) C15 0.0783(18) 0.143(3) 0.089(2) 0.030(2) 0.0412(16) 0.058(2) C16 0.0377(10) 0.0601(14) 0.0563(12) -0.0158(10) 0.0076(9) 0.0050(9) C17 0.0668(16) 0.111(2) 0.0595(15) -0.0360(15) 0.0144(12) -0.0343(15) C18 0.0346(16) 0.168(5) 0.0451(18) 0.000 0.0073(14) 0.000 C19 0.0334(12) 0.0410(13) 0.0310(11) 0.000 0.0105(9) 0.000 C20 0.0421(14) 0.0551(16) 0.0304(12) 0.000 0.0152(10) 0.000 C21 0.0429(15) 0.072(2) 0.0402(14) 0.000 0.0242(12) 0.000 C22 0.0319(13) 0.077(2) 0.0420(14) 0.000 0.0136(11) 0.000 C23 0.0368(13) 0.0474(15) 0.0314(12) 0.000 0.0106(10) 0.000 N1 0.0343(7) 0.0252(7) 0.0319(7) 0.0013(5) 0.0130(5) 0.0002(5) N2 0.0325(10) 0.0370(11) 0.0357(10) 0.000 0.0113(8) 0.000 N3 0.0338(10) 0.0309(10) 0.0300(9) 0.000 0.0124(8) 0.000 Mg1 0.0311(4) 0.0246(4) 0.0271(4) 0.000 0.0109(3) 0.000 _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 1.513(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 N1 1.329(2) . ? C2 C3 1.4091(19) . ? C3 C2 1.4091(19) 4_565 ? C3 H3 0.9500 . ? C4 C5 1.402(3) . ? C4 C9 1.411(3) . ? C4 N1 1.438(2) . ? C5 C6 1.399(3) . ? C5 C10 1.512(3) . ? C6 C7 1.373(4) . ? C6 H6 0.9500 . ? C7 C8 1.368(4) . ? C7 H7 0.9500 . ? C8 C9 1.389(3) . ? C8 H8 0.9500 . ? C9 C13 1.524(3) . ? C10 C11 1.533(3) . ? C10 C12 1.535(3) . ? C10 H10 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.502(4) . ? C13 C15 1.533(3) . ? C13 H13 1.0000 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.390(3) . ? C16 N2 1.398(2) . ? C16 H16A 0.981(3) . ? C16 H16B 0.981(3) . ? C17 C18 1.375(4) . ? C17 H17 0.9500 . ? C18 C17 1.375(4) 4_565 ? C18 H18 0.9500 . ? C19 N3 1.347(3) . ? C19 C20 1.380(3) . ? C19 H19 0.9500 . ? C20 C21 1.376(4) . ? C20 H20 0.9500 . ? C21 C22 1.389(4) . ? C21 H21 0.9500 . ? C22 C23 1.374(4) . ? C22 H22 0.9500 . ? C23 N3 1.341(3) . ? C23 H23 0.9500 . ? N1 Mg1 2.0344(13) . ? N2 C16 1.398(2) 4_565 ? N2 Mg1 1.993(2) . ? N3 Mg1 2.1289(19) . ? Mg1 N1 2.0343(13) 4_565 ? 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 . . ? 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 123.84(15) . . ? N1 C2 C1 120.45(15) . . ? C3 C2 C1 115.71(15) . . ? C2 C3 C2 130.8(2) . 4_565 ? C2 C3 H3 114.6 . . ? C2 C3 H3 114.6 4_565 . ? C5 C4 C9 120.74(17) . . ? C5 C4 N1 121.10(15) . . ? C9 C4 N1 117.90(16) . . ? C6 C5 C4 118.08(19) . . ? C6 C5 C10 119.19(18) . . ? C4 C5 C10 122.72(16) . . ? C7 C6 C5 121.4(2) . . ? C7 C6 H6 119.3 . . ? C5 C6 H6 119.3 . . ? C8 C7 C6 120.0(2) . . ? C8 C7 H7 120.0 . . ? C6 C7 H7 120.0 . . ? C7 C8 C9 121.5(2) . . ? C7 C8 H8 119.2 . . ? C9 C8 H8 119.2 . . ? C8 C9 C4 118.3(2) . . ? C8 C9 C13 120.0(2) . . ? C4 C9 C13 121.71(17) . . ? C5 C10 C11 111.97(16) . . ? C5 C10 C12 110.71(19) . . ? C11 C10 C12 110.11(17) . . ? C5 C10 H10 108.0 . . ? C11 C10 H10 108.0 . . ? C12 C10 H10 108.0 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C14 C13 C9 110.95(19) . . ? C14 C13 C15 110.0(2) . . ? C9 C13 C15 111.8(2) . . ? C14 C13 H13 108.0 . . ? C9 C13 H13 108.0 . . ? C15 C13 H13 108.0 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C17 C16 N2 120.8(2) . . ? C17 C16 H16A 98(3) . . ? N2 C16 H16A 109(3) . . ? C17 C16 H16B 122.2(13) . . ? N2 C16 H16B 112.5(13) . . ? H16A C16 H16B 84(3) . . ? C18 C17 C16 120.8(3) . . ? C18 C17 H17 119.6 . . ? C16 C17 H17 119.6 . . ? C17 C18 C17 117.2(3) . 4_565 ? C17 C18 H18 121.4 . . ? C17 C18 H18 121.4 4_565 . ? N3 C19 C20 122.8(2) . . ? N3 C19 H19 118.6 . . ? C20 C19 H19 118.6 . . ? C21 C20 C19 119.1(2) . . ? C21 C20 H20 120.5 . . ? C19 C20 H20 120.5 . . ? C20 C21 C22 118.8(2) . . ? C20 C21 H21 120.6 . . ? C22 C21 H21 120.6 . . ? C23 C22 C21 118.7(2) . . ? C23 C22 H22 120.6 . . ? C21 C22 H22 120.6 . . ? N3 C23 C22 123.3(2) . . ? N3 C23 H23 118.3 . . ? C22 C23 H23 118.3 . . ? C2 N1 C4 120.94(13) . . ? C2 N1 Mg1 119.76(11) . . ? C4 N1 Mg1 119.22(10) . . ? C16 N2 C16 113.1(2) 4_565 . ? C16 N2 Mg1 119.58(11) 4_565 . ? C16 N2 Mg1 119.58(11) . . ? C23 N3 C19 117.3(2) . . ? C23 N3 Mg1 120.51(15) . . ? C19 N3 Mg1 122.16(15) . . ? N2 Mg1 N1 122.67(5) . 4_565 ? N2 Mg1 N1 122.67(5) . . ? N1 Mg1 N1 95.20(8) 4_565 . ? N2 Mg1 N3 105.15(8) . . ? N1 Mg1 N3 104.42(5) 4_565 . ? N1 Mg1 N3 104.42(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 N1 C2 C3 C2 10.9(4) . . . 4_565 ? C1 C2 C3 C2 -168.80(18) . . . 4_565 ? C9 C4 C5 C6 0.1(3) . . . . ? N1 C4 C5 C6 -173.85(16) . . . . ? C9 C4 C5 C10 178.81(18) . . . . ? N1 C4 C5 C10 4.9(3) . . . . ? C4 C5 C6 C7 0.2(3) . . . . ? C10 C5 C6 C7 -178.6(2) . . . . ? C5 C6 C7 C8 -0.2(4) . . . . ? C6 C7 C8 C9 -0.1(5) . . . . ? C7 C8 C9 C4 0.3(4) . . . . ? C7 C8 C9 C13 -178.5(3) . . . . ? C5 C4 C9 C8 -0.3(3) . . . . ? N1 C4 C9 C8 173.8(2) . . . . ? C5 C4 C9 C13 178.5(2) . . . . ? N1 C4 C9 C13 -7.4(3) . . . . ? C6 C5 C10 C11 -59.4(2) . . . . ? C4 C5 C10 C11 121.88(19) . . . . ? C6 C5 C10 C12 63.9(2) . . . . ? C4 C5 C10 C12 -114.8(2) . . . . ? C8 C9 C13 C14 81.3(3) . . . . ? C4 C9 C13 C14 -97.4(2) . . . . ? C8 C9 C13 C15 -41.8(3) . . . . ? C4 C9 C13 C15 139.5(2) . . . . ? N2 C16 C17 C18 -9.6(4) . . . . ? C16 C17 C18 C17 -9.3(5) . . . 4_565 ? N3 C19 C20 C21 0.0 . . . . ? C19 C20 C21 C22 0.0 . . . . ? C20 C21 C22 C23 0.0 . . . . ? C21 C22 C23 N3 0.0 . . . . ? C3 C2 N1 C4 -171.52(17) . . . . ? C1 C2 N1 C4 8.2(2) . . . . ? C3 C2 N1 Mg1 11.8(2) . . . . ? C1 C2 N1 Mg1 -168.45(12) . . . . ? C5 C4 N1 C2 -88.6(2) . . . . ? C9 C4 N1 C2 97.33(19) . . . . ? C5 C4 N1 Mg1 88.10(17) . . . . ? C9 C4 N1 Mg1 -85.98(18) . . . . ? C17 C16 N2 C16 26.8(3) . . . 4_565 ? C17 C16 N2 Mg1 -122.4(2) . . . . ? C22 C23 N3 C19 0.0 . . . . ? C22 C23 N3 Mg1 180.0 . . . . ? C20 C19 N3 C23 0.0 . . . . ? C20 C19 N3 Mg1 180.0 . . . . ? C16 N2 Mg1 N1 45.1(2) 4_565 . . 4_565 ? C16 N2 Mg1 N1 -167.68(15) . . . 4_565 ? C16 N2 Mg1 N1 167.68(15) 4_565 . . . ? C16 N2 Mg1 N1 -45.1(2) . . . . ? C16 N2 Mg1 N3 -73.63(16) 4_565 . . . ? C16 N2 Mg1 N3 73.63(16) . . . . ? C2 N1 Mg1 N2 -159.01(12) . . . . ? C4 N1 Mg1 N2 24.26(15) . . . . ? C2 N1 Mg1 N1 -24.40(15) . . . 4_565 ? C4 N1 Mg1 N1 158.87(9) . . . 4_565 ? C2 N1 Mg1 N3 81.95(12) . . . . ? C4 N1 Mg1 N3 -94.77(12) . . . . ? C23 N3 Mg1 N2 180.0 . . . . ? C19 N3 Mg1 N2 0.0 . . . . ? C23 N3 Mg1 N1 49.68(4) . . . 4_565 ? C19 N3 Mg1 N1 -130.32(4) . . . 4_565 ? C23 N3 Mg1 N1 -49.68(4) . . . . ? C19 N3 Mg1 N1 130.32(4) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.338 _refine_diff_density_min -0.244 _refine_diff_density_rms 0.042