# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/1919 data_sfa110 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety MgL2 _chemical_formula_sum 'C26 H38 Mg N4' _chemical_formula_weight 430.91 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Mg' 'Mg' 0.1719 0.1771 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.5281(6) _cell_length_b 18.3692(13) _cell_length_c 14.2891(10) _cell_angle_alpha 90.00 _cell_angle_beta 93.154(7) _cell_angle_gamma 90.00 _cell_volume 2497.1(3) _cell_formula_units_Z 4 _cell_measurement_temperature 220(2) _cell_measurement_reflns_used 48 _cell_measurement_theta_min 20 _cell_measurement_theta_max 22 _exptl_crystal_description block _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.62 _exptl_crystal_size_mid 0.41 _exptl_crystal_size_min 0.27 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.146 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 936 _exptl_absorpt_coefficient_mu 0.747 _exptl_absorpt_correction_type 'Optimised numerical' _exptl_absorpt_correction_T_min 0.805 _exptl_absorpt_correction_T_max 0.900 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 220(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method Omega-theta _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% ? _diffrn_reflns_number 9321 _diffrn_reflns_av_R_equivalents 0.0147 _diffrn_reflns_av_sigmaI/netI 0.0181 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.92 _diffrn_reflns_theta_max 70.11 _reflns_number_total 4652 _reflns_number_gt 4010 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Stoe DIF4' _computing_cell_refinement 'Stoe DIF4' _computing_data_reduction 'Stoe REDU4' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0436P)^2^+0.6382P] 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 riding _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0033(2) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 4652 _refine_ls_number_parameters 281 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0418 _refine_ls_R_factor_gt 0.0346 _refine_ls_wR_factor_ref 0.0931 _refine_ls_wR_factor_gt 0.0888 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.028 _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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mg1 Mg 0.51417(4) 0.19659(2) 0.86954(3) 0.03229(13) Uani 1 1 d . . . C1A C 0.26647(13) 0.28557(7) 0.86566(8) 0.0327(3) Uani 1 1 d . . . N1A N 0.30179(11) 0.21598(6) 0.85703(7) 0.0322(2) Uani 1 1 d . . . C11A C 0.19634(14) 0.16194(8) 0.82413(9) 0.0383(3) Uani 1 1 d . . . H11A H 0.1453 0.1808 0.7670 0.046 Uiso 1 1 calc R . . C12A C 0.09071(17) 0.14741(10) 0.89864(12) 0.0556(4) Uani 1 1 d . . . H12A H 0.0433 0.1924 0.9132 0.083 Uiso 1 1 calc R . . H12B H 0.1397 0.1287 0.9549 0.083 Uiso 1 1 calc R . . H12C H 0.0221 0.1120 0.8751 0.083 Uiso 1 1 calc R . . C13A C 0.27139(17) 0.09204(8) 0.79980(11) 0.0480(4) Uani 1 1 d . . . H13A H 0.3382 0.1021 0.7526 0.072 Uiso 1 1 calc R . . H13B H 0.2031 0.0566 0.7756 0.072 Uiso 1 1 calc R . . H13C H 0.3207 0.0728 0.8556 0.072 Uiso 1 1 calc R . . C2A C 0.38067(14) 0.33288(7) 0.90902(9) 0.0344(3) Uani 1 1 d . . . N2A N 0.50559(11) 0.30101(6) 0.91876(7) 0.0341(2) Uani 1 1 d . . . C21A C 0.62735(15) 0.34090(8) 0.96054(10) 0.0408(3) Uani 1 1 d . . . H21A H 0.6228 0.3921 0.9389 0.049 Uiso 1 1 calc R . . C22A C 0.62879(17) 0.33956(9) 1.06723(10) 0.0479(4) Uani 1 1 d . . . H22A H 0.5442 0.3627 1.0877 0.072 Uiso 1 1 calc R . . H22B H 0.7106 0.3656 1.0929 0.072 Uiso 1 1 calc R . . H22C H 0.6324 0.2895 1.0889 0.072 Uiso 1 1 calc R . . C23A C 0.76025(16) 0.30626(11) 0.92787(12) 0.0604(5) Uani 1 1 d . . . H23A H 0.7585 0.3071 0.8599 0.091 Uiso 1 1 calc R . . H23B H 0.7661 0.2563 0.9496 0.091 Uiso 1 1 calc R . . H23C H 0.8413 0.3332 0.9531 0.091 Uiso 1 1 calc R . . C3A C 0.35621(17) 0.40451(8) 0.94124(11) 0.0471(4) Uani 1 1 d . . . H3A H 0.4332 0.4243 0.9765 0.057 Uiso 1 1 calc R . . C4A C 0.2425(2) 0.45153(9) 0.93166(13) 0.0602(5) Uani 1 1 d . . . H4A H 0.2551 0.4963 0.9628 0.072 Uiso 1 1 calc R . . C5A C 0.1150(2) 0.44325(9) 0.88415(14) 0.0603(5) Uani 1 1 d . . . H5A H 0.0532 0.4832 0.8828 0.072 Uiso 1 1 calc R . . C6A C 0.07018(17) 0.38062(9) 0.83798(11) 0.0513(4) Uani 1 1 d . . . H6A H -0.0177 0.3845 0.8051 0.062 Uiso 1 1 calc R . . C7A C 0.13344(15) 0.31342(8) 0.83239(10) 0.0429(3) Uani 1 1 d . . . H7A H 0.0770 0.2787 0.7998 0.051 Uiso 1 1 calc R . . C1B C 0.70407(14) 0.10478(7) 0.77310(9) 0.0338(3) Uani 1 1 d . . . N1B N 0.62625(11) 0.16407(6) 0.75846(7) 0.0331(2) Uani 1 1 d . . . C11B C 0.62117(15) 0.19976(8) 0.66596(9) 0.0381(3) Uani 1 1 d . . . H11B H 0.6104 0.1620 0.6167 0.046 Uiso 1 1 calc R . . C12B C 0.49464(17) 0.25017(10) 0.65807(11) 0.0521(4) Uani 1 1 d . . . H12D H 0.4099 0.2225 0.6678 0.078 Uiso 1 1 calc R . . H12E H 0.4878 0.2721 0.5962 0.078 Uiso 1 1 calc R . . H12F H 0.5054 0.2881 0.7052 0.078 Uiso 1 1 calc R . . C13B C 0.75346(17) 0.24345(9) 0.65084(11) 0.0521(4) Uani 1 1 d . . . H13D H 0.8345 0.2115 0.6558 0.078 Uiso 1 1 calc R . . H13E H 0.7638 0.2813 0.6980 0.078 Uiso 1 1 calc R . . H13F H 0.7465 0.2654 0.5890 0.078 Uiso 1 1 calc R . . C2B C 0.70323(13) 0.07415(7) 0.87039(9) 0.0325(3) Uani 1 1 d . . . N2B N 0.62415(11) 0.11106(6) 0.92808(7) 0.0322(2) Uani 1 1 d . . . C21B C 0.61496(14) 0.08784(8) 1.02602(9) 0.0362(3) Uani 1 1 d . . . H21B H 0.6030 0.0343 1.0277 0.043 Uiso 1 1 calc R . . C22B C 0.48703(15) 0.12356(9) 1.06489(10) 0.0449(3) Uani 1 1 d . . . H22D H 0.4038 0.1104 1.0265 0.067 Uiso 1 1 calc R . . H22E H 0.4985 0.1760 1.0644 0.067 Uiso 1 1 calc R . . H22F H 0.4769 0.1072 1.1287 0.067 Uiso 1 1 calc R . . C23B C 0.74619(16) 0.10842(10) 1.08622(11) 0.0511(4) Uani 1 1 d . . . H23D H 0.8278 0.0854 1.0612 0.077 Uiso 1 1 calc R . . H23E H 0.7362 0.0920 1.1500 0.077 Uiso 1 1 calc R . . H23F H 0.7580 0.1609 1.0857 0.077 Uiso 1 1 calc R . . C3B C 0.77970(15) 0.01110(8) 0.89926(10) 0.0411(3) Uani 1 1 d . . . H3B H 0.7676 -0.0016 0.9620 0.049 Uiso 1 1 calc R . . C4B C 0.86803(17) -0.03571(8) 0.85522(11) 0.0490(4) Uani 1 1 d . . . H4B H 0.9030 -0.0744 0.8928 0.059 Uiso 1 1 calc R . . C5B C 0.91333(19) -0.03529(9) 0.76580(12) 0.0545(4) Uani 1 1 d . . . H5B H 0.9765 -0.0719 0.7495 0.065 Uiso 1 1 calc R . . C6B C 0.8728(2) 0.01480(9) 0.69864(12) 0.0577(4) Uani 1 1 d . . . H6B H 0.9132 0.0081 0.6407 0.069 Uiso 1 1 calc R . . C7B C 0.78260(19) 0.07349(8) 0.70165(11) 0.0512(4) Uani 1 1 d . . . H7B H 0.7706 0.0980 0.6440 0.061 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 0.0314(2) 0.0343(2) 0.0313(2) -0.00016(17) 0.00288(16) 0.00028(17) C1A 0.0344(7) 0.0380(7) 0.0263(6) 0.0035(5) 0.0075(5) -0.0002(5) N1A 0.0323(5) 0.0352(6) 0.0293(5) 0.0010(4) 0.0025(4) -0.0035(4) C11A 0.0375(7) 0.0437(8) 0.0333(7) 0.0003(6) -0.0026(5) -0.0069(6) C12A 0.0474(9) 0.0657(11) 0.0545(9) -0.0008(8) 0.0090(7) -0.0218(8) C13A 0.0517(9) 0.0411(8) 0.0503(8) -0.0047(7) -0.0070(7) -0.0075(7) C2A 0.0409(7) 0.0347(7) 0.0282(6) 0.0035(5) 0.0076(5) -0.0028(5) N2A 0.0353(6) 0.0366(6) 0.0308(5) -0.0006(4) 0.0036(4) -0.0062(5) C21A 0.0440(8) 0.0426(8) 0.0358(7) -0.0011(6) 0.0014(6) -0.0131(6) C22A 0.0546(9) 0.0509(9) 0.0377(8) -0.0044(6) -0.0020(7) -0.0088(7) C23A 0.0394(8) 0.0866(13) 0.0557(10) -0.0143(9) 0.0066(7) -0.0178(8) C3A 0.0561(9) 0.0354(8) 0.0499(9) -0.0006(6) 0.0038(7) -0.0009(7) C4A 0.0741(12) 0.0366(8) 0.0707(11) -0.0019(8) 0.0094(9) 0.0080(8) C5A 0.0633(11) 0.0454(9) 0.0731(12) 0.0087(8) 0.0131(9) 0.0189(8) C6A 0.0439(8) 0.0609(10) 0.0497(9) 0.0144(7) 0.0090(7) 0.0124(7) C7A 0.0381(7) 0.0501(8) 0.0406(7) 0.0038(6) 0.0036(6) 0.0038(6) C1B 0.0365(7) 0.0316(6) 0.0334(6) 0.0001(5) 0.0033(5) -0.0015(5) N1B 0.0350(6) 0.0341(6) 0.0302(5) 0.0023(4) 0.0028(4) 0.0003(4) C11B 0.0450(8) 0.0397(7) 0.0298(6) 0.0036(5) 0.0040(5) 0.0020(6) C12B 0.0495(9) 0.0629(10) 0.0441(8) 0.0182(7) 0.0034(7) 0.0101(7) C13B 0.0515(9) 0.0573(10) 0.0487(9) 0.0142(7) 0.0137(7) 0.0012(7) C2B 0.0313(6) 0.0317(7) 0.0347(7) 0.0010(5) 0.0022(5) -0.0047(5) N2B 0.0321(5) 0.0352(6) 0.0294(5) 0.0022(4) 0.0020(4) -0.0027(4) C21B 0.0379(7) 0.0398(7) 0.0308(6) 0.0044(5) 0.0012(5) -0.0036(6) C22B 0.0456(8) 0.0556(9) 0.0343(7) 0.0014(6) 0.0083(6) -0.0016(7) C23B 0.0464(9) 0.0652(10) 0.0405(8) 0.0016(7) -0.0083(7) -0.0043(7) C3B 0.0428(7) 0.0385(7) 0.0424(7) 0.0093(6) 0.0063(6) 0.0024(6) C4B 0.0510(9) 0.0391(8) 0.0576(9) 0.0112(7) 0.0093(7) 0.0099(7) C5B 0.0652(10) 0.0393(8) 0.0608(10) 0.0003(7) 0.0186(8) 0.0155(7) C6B 0.0826(12) 0.0455(9) 0.0471(9) -0.0008(7) 0.0238(8) 0.0169(8) C7B 0.0741(11) 0.0439(8) 0.0369(8) 0.0035(6) 0.0149(7) 0.0146(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 N2B 2.0420(12) . ? Mg1 N2A 2.0461(12) . ? Mg1 N1B 2.0502(11) . ? Mg1 N1A 2.0528(11) . ? Mg1 C1A 2.8688(14) . ? C1A N1A 1.3294(17) . ? C1A C7A 1.4240(19) . ? C1A C2A 1.4997(18) . ? N1A C11A 1.4710(16) . ? C11A C13A 1.519(2) . ? C11A C12A 1.528(2) . ? C2A N2A 1.3268(17) . ? C2A C3A 1.4176(19) . ? N2A C21A 1.4707(17) . ? C21A C23A 1.514(2) . ? C21A C22A 1.5240(19) . ? C3A C4A 1.386(2) . ? C4A C5A 1.367(3) . ? C5A C6A 1.382(3) . ? C6A C7A 1.378(2) . ? C1B N1B 1.3276(17) . ? C1B C7B 1.4202(19) . ? C1B C2B 1.5002(18) . ? N1B C11B 1.4737(16) . ? C11B C12B 1.520(2) . ? C11B C13B 1.520(2) . ? C2B N2B 1.3325(17) . ? C2B C3B 1.4175(19) . ? N2B C21B 1.4701(16) . ? C21B C22B 1.5164(19) . ? C21B C23B 1.5258(19) . ? C3B C4B 1.379(2) . ? C4B C5B 1.371(2) . ? C5B C6B 1.370(2) . ? C6B C7B 1.381(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 N2B Mg1 N2A 127.58(5) . . ? N2B Mg1 N1B 79.37(4) . . ? N2A Mg1 N1B 124.86(5) . . ? N2B Mg1 N1A 130.56(5) . . ? N2A Mg1 N1A 79.02(4) . . ? N1B Mg1 N1A 122.42(5) . . ? N2B Mg1 C1A 148.14(4) . . ? N2A Mg1 C1A 54.84(4) . . ? N1B Mg1 C1A 127.88(4) . . ? N1A Mg1 C1A 24.97(4) . . ? N1A C1A C7A 122.67(12) . . ? N1A C1A C2A 114.45(11) . . ? C7A C1A C2A 122.82(12) . . ? N1A C1A Mg1 40.69(6) . . ? C7A C1A Mg1 158.02(10) . . ? C2A C1A Mg1 75.21(7) . . ? C1A N1A C11A 120.44(11) . . ? C1A N1A Mg1 114.34(8) . . ? C11A N1A Mg1 124.30(9) . . ? N1A C11A C13A 108.76(11) . . ? N1A C11A C12A 111.07(11) . . ? C13A C11A C12A 110.37(13) . . ? N2A C2A C3A 122.55(13) . . ? N2A C2A C1A 114.45(11) . . ? C3A C2A C1A 122.93(13) . . ? C2A N2A C21A 120.38(11) . . ? C2A N2A Mg1 115.48(9) . . ? C21A N2A Mg1 124.12(9) . . ? N2A C21A C23A 108.66(12) . . ? N2A C21A C22A 111.19(11) . . ? C23A C21A C22A 109.89(13) . . ? C4A C3A C2A 133.45(16) . . ? C5A C4A C3A 130.38(17) . . ? C4A C5A C6A 124.92(16) . . ? C7A C6A C5A 130.44(16) . . ? C6A C7A C1A 133.37(15) . . ? N1B C1B C7B 122.04(12) . . ? N1B C1B C2B 114.99(11) . . ? C7B C1B C2B 122.98(12) . . ? C1B N1B C11B 119.79(11) . . ? C1B N1B Mg1 115.29(8) . . ? C11B N1B Mg1 124.89(8) . . ? N1B C11B C12B 108.93(11) . . ? N1B C11B C13B 112.08(12) . . ? C12B C11B C13B 109.17(12) . . ? N2B C2B C3B 122.34(12) . . ? N2B C2B C1B 114.48(11) . . ? C3B C2B C1B 123.18(12) . . ? C2B N2B C21B 120.44(11) . . ? C2B N2B Mg1 115.66(8) . . ? C21B N2B Mg1 123.85(8) . . ? N2B C21B C22B 108.32(11) . . ? N2B C21B C23B 112.02(11) . . ? C22B C21B C23B 109.67(12) . . ? C4B C3B C2B 133.91(14) . . ? C5B C4B C3B 130.77(15) . . ? C6B C5B C4B 124.46(15) . . ? C5B C6B C7B 130.89(15) . . ? C6B C7B C1B 133.77(15) . . ? _diffrn_measured_fraction_theta_max 0.977 _diffrn_reflns_theta_full 70.11 _diffrn_measured_fraction_theta_full 0.977 _refine_diff_density_max 0.183 _refine_diff_density_min -0.162 _refine_diff_density_rms 0.029 data_sfa104 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety [MgL(OMe)]2 _chemical_formula_sum 'C28 H44 Mg2 N4 O2' _chemical_formula_weight 517.29 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Mg' 'Mg' 0.1719 0.1771 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 15.560(11) _cell_length_b 8.838(7) _cell_length_c 22.162(16) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3048(4) _cell_formula_units_Z 4 _cell_measurement_temperature 220(2) _cell_measurement_reflns_used 72 _cell_measurement_theta_min 20 _cell_measurement_theta_max 22 _exptl_crystal_description block _exptl_crystal_colour Orange _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.26 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.127 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1120 _exptl_absorpt_coefficient_mu 0.927 _exptl_absorpt_correction_type Psi-scans _exptl_absorpt_correction_T_min 0.625 _exptl_absorpt_correction_T_max 0.717 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 220(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method Omega-theta _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 5 _diffrn_reflns_number 4130 _diffrn_reflns_av_R_equivalents 0.0205 _diffrn_reflns_av_sigmaI/netI 0.0362 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.99 _diffrn_reflns_theta_max 69.96 _reflns_number_total 2715 _reflns_number_gt 1631 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Stoe DIF4' _computing_cell_refinement 'Stoe DIF4' _computing_data_reduction 'Stoe REDU4' _computing_structure_solution SIR92 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0893P)^2^+0.8468P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geometric _refine_ls_hydrogen_treatment riding _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0007(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 2715 _refine_ls_number_parameters 176 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0995 _refine_ls_R_factor_gt 0.0582 _refine_ls_wR_factor_ref 0.1871 _refine_ls_wR_factor_gt 0.1586 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.038 _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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mg1 Mg 0.98156(7) 0.45011(13) 0.56160(4) 0.0707(4) Uani 1 1 d . . . O1M O 0.93525(15) 0.4272(3) 0.48079(10) 0.0814(7) Uani 1 1 d . . . C1M C 0.8625(3) 0.3438(7) 0.4625(2) 0.144(2) Uani 1 1 d . . . H1M1 H 0.8368 0.2950 0.4973 0.215 Uiso 1 1 calc R . . H1M2 H 0.8796 0.2676 0.4334 0.215 Uiso 1 1 calc R . . H1M3 H 0.8209 0.4115 0.4441 0.215 Uiso 1 1 calc R . . C1 C 0.9571(2) 0.2596(4) 0.66528(14) 0.0699(8) Uani 1 1 d . A . N1 N 1.00636(18) 0.2713(4) 0.61668(13) 0.0887(9) Uani 1 1 d D . . C11 C 1.0638(3) 0.1387(7) 0.6007(3) 0.0797(14) Uani 0.75 1 d PD A 1 H11 H 1.0370 0.0419 0.6129 0.096 Uiso 0.75 1 calc PR A 1 C12 C 1.0814(4) 0.1406(7) 0.5341(3) 0.1015(17) Uani 0.75 1 d PD A 1 H12A H 1.0286 0.1198 0.5123 0.152 Uiso 0.75 1 calc PR A 1 H12B H 1.1238 0.0639 0.5245 0.152 Uiso 0.75 1 calc PR A 1 H12C H 1.1031 0.2393 0.5226 0.152 Uiso 0.75 1 calc PR A 1 C13 C 1.1445(3) 0.1662(9) 0.6353(3) 0.116(2) Uani 0.75 1 d PD A 1 H13A H 1.1323 0.1626 0.6782 0.175 Uiso 0.75 1 calc PR A 1 H13B H 1.1673 0.2650 0.6249 0.175 Uiso 0.75 1 calc PR A 1 H13C H 1.1864 0.0890 0.6253 0.175 Uiso 0.75 1 calc PR A 1 C11' C 1.0979(8) 0.2109(15) 0.6164(6) 0.058(3) Uiso 0.25 1 d PD A 2 H11' H 1.1138 0.1787 0.6577 0.069 Uiso 0.25 1 calc PR A 2 C12' C 1.0802(13) 0.0708(19) 0.5776(9) 0.102(7) Uiso 0.25 1 d PD A 2 H12D H 1.0339 0.0126 0.5954 0.152 Uiso 0.25 1 calc PR A 2 H12E H 1.1316 0.0090 0.5756 0.152 Uiso 0.25 1 calc PR A 2 H12F H 1.0640 0.1022 0.5373 0.152 Uiso 0.25 1 calc PR A 2 C13' C 1.1679(7) 0.3039(13) 0.5907(5) 0.064(3) Uiso 0.25 1 d PD A 2 H13D H 1.1804 0.3874 0.6177 0.096 Uiso 0.25 1 calc PR A 2 H13E H 1.1502 0.3433 0.5518 0.096 Uiso 0.25 1 calc PR A 2 H13F H 1.2189 0.2421 0.5858 0.096 Uiso 0.25 1 calc PR A 2 C2 C 0.89472(19) 0.3883(4) 0.67327(13) 0.0649(8) Uani 1 1 d . . . N2 N 0.90334(17) 0.4982(3) 0.63328(12) 0.0713(7) Uani 1 1 d . A . C21 C 0.8544(3) 0.6406(5) 0.63918(17) 0.0902(11) Uani 1 1 d . . . H21 H 0.8347 0.6511 0.6814 0.108 Uiso 1 1 calc R A . C22 C 0.7771(3) 0.6345(5) 0.5985(2) 0.1181(16) Uani 1 1 d . A . H22A H 0.7408 0.5503 0.6102 0.177 Uiso 1 1 calc R . . H22B H 0.7957 0.6212 0.5571 0.177 Uiso 1 1 calc R . . H22C H 0.7450 0.7282 0.6020 0.177 Uiso 1 1 calc R . . C23 C 0.9143(3) 0.7717(5) 0.6243(2) 0.1271(18) Uani 1 1 d . A . H23A H 0.9620 0.7722 0.6525 0.191 Uiso 1 1 calc R . . H23B H 0.8831 0.8663 0.6274 0.191 Uiso 1 1 calc R . . H23C H 0.9361 0.7599 0.5836 0.191 Uiso 1 1 calc R . . C3 C 0.8321(3) 0.3922(4) 0.71865(16) 0.0882(11) Uani 1 1 d . A . H3 H 0.7971 0.4787 0.7171 0.106 Uiso 1 1 calc R . . C4 C 0.8115(3) 0.2955(6) 0.76495(18) 0.1085(14) Uani 1 1 d . . . H4 H 0.7643 0.3267 0.7884 0.130 Uiso 1 1 calc R A . C5 C 0.8477(3) 0.1612(6) 0.78300(17) 0.1044(14) Uani 1 1 d . A . H5 H 0.8234 0.1121 0.8165 0.125 Uiso 1 1 calc R . . C6 C 0.9169(3) 0.0936(5) 0.75562(18) 0.0986(13) Uani 1 1 d . . . H6 H 0.9352 0.0029 0.7737 0.118 Uiso 1 1 calc R A . C7 C 0.9642(2) 0.1377(5) 0.70566(15) 0.0839(10) Uani 1 1 d . A . H7 H 1.0105 0.0729 0.6970 0.101 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 0.0718(7) 0.0776(7) 0.0625(6) 0.0133(5) 0.0087(5) 0.0094(6) O1M 0.0758(14) 0.0995(18) 0.0688(13) 0.0076(13) 0.0027(11) -0.0125(13) C1M 0.113(4) 0.206(6) 0.111(3) -0.021(4) 0.008(3) -0.063(4) C1 0.0723(18) 0.076(2) 0.0615(17) 0.0081(17) -0.0060(15) -0.0014(18) N1 0.0852(18) 0.102(2) 0.0786(18) 0.0294(17) 0.0202(15) 0.0346(18) C11 0.076(3) 0.080(4) 0.083(3) 0.021(3) -0.001(3) 0.004(3) C12 0.114(4) 0.091(4) 0.099(4) -0.009(3) 0.004(3) 0.027(3) C13 0.075(3) 0.161(6) 0.113(4) 0.023(4) -0.006(3) 0.006(4) C2 0.0679(18) 0.075(2) 0.0515(15) -0.0005(15) -0.0033(13) -0.0084(17) N2 0.0761(17) 0.0718(17) 0.0661(15) 0.0046(13) 0.0072(13) 0.0103(14) C21 0.100(3) 0.089(3) 0.082(2) 0.007(2) 0.025(2) 0.016(2) C22 0.089(3) 0.098(3) 0.168(4) 0.001(3) -0.001(3) 0.017(2) C23 0.139(4) 0.073(3) 0.169(5) -0.004(3) 0.004(4) 0.001(3) C3 0.104(3) 0.086(3) 0.075(2) 0.0000(19) 0.023(2) 0.002(2) C4 0.128(3) 0.118(4) 0.080(2) 0.008(2) 0.041(2) -0.007(3) C5 0.118(3) 0.123(4) 0.072(2) 0.023(2) 0.010(2) -0.023(3) C6 0.102(3) 0.112(3) 0.082(2) 0.033(3) -0.018(2) -0.018(3) C7 0.083(2) 0.095(3) 0.074(2) 0.022(2) -0.0059(18) -0.005(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 O1M 1.932(3) 5_766 ? Mg1 O1M 1.941(3) . ? Mg1 N1 2.034(3) . ? Mg1 N2 2.046(3) . ? Mg1 Mg1 2.926(3) 5_766 ? O1M C1M 1.411(5) . ? O1M Mg1 1.932(3) 5_766 ? C1 N1 1.326(4) . ? C1 C7 1.405(5) . ? C1 C2 1.506(5) . ? N1 C11 1.516(6) . ? N1 C11' 1.521(12) . ? C11 C13 1.492(7) . ? C11 C12 1.500(7) . ? C11' C13' 1.479(14) . ? C11' C12' 1.533(16) . ? C2 N2 1.321(4) . ? C2 C3 1.401(4) . ? N2 C21 1.477(5) . ? C21 C22 1.504(6) . ? C21 C23 1.523(6) . ? C3 C4 1.373(5) . ? C4 C5 1.373(6) . ? C5 C6 1.373(6) . ? C6 C7 1.385(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1M Mg1 O1M 81.88(12) 5_766 . ? O1M Mg1 N1 126.92(13) 5_766 . ? O1M Mg1 N1 122.90(14) . . ? O1M Mg1 N2 131.26(13) 5_766 . ? O1M Mg1 N2 121.15(12) . . ? N1 Mg1 N2 78.94(12) . . ? O1M Mg1 Mg1 41.05(7) 5_766 5_766 ? O1M Mg1 Mg1 40.82(8) . 5_766 ? N1 Mg1 Mg1 139.21(11) . 5_766 ? N2 Mg1 Mg1 141.14(11) . 5_766 ? C1M O1M Mg1 133.7(3) . 5_766 ? C1M O1M Mg1 128.2(3) . . ? Mg1 O1M Mg1 98.12(12) 5_766 . ? N1 C1 C7 122.1(3) . . ? N1 C1 C2 114.2(3) . . ? C7 C1 C2 123.7(3) . . ? C1 N1 C11 118.1(3) . . ? C1 N1 C11' 121.1(5) . . ? C11 N1 C11' 34.5(5) . . ? C1 N1 Mg1 116.0(2) . . ? C11 N1 Mg1 124.9(2) . . ? C11' N1 Mg1 116.6(5) . . ? C13 C11 C12 110.5(5) . . ? C13 C11 N1 104.5(6) . . ? C12 C11 N1 109.2(4) . . ? C13' C11' N1 119.7(10) . . ? C13' C11' C12' 111.4(11) . . ? N1 C11' C12' 96.7(12) . . ? N2 C2 C3 122.3(3) . . ? N2 C2 C1 114.3(3) . . ? C3 C2 C1 123.4(3) . . ? C2 N2 C21 121.0(3) . . ? C2 N2 Mg1 115.4(2) . . ? C21 N2 Mg1 123.5(2) . . ? N2 C21 C22 109.2(3) . . ? N2 C21 C23 108.2(3) . . ? C22 C21 C23 112.8(4) . . ? C4 C3 C2 133.2(4) . . ? C5 C4 C3 131.2(4) . . ? C6 C5 C4 124.7(4) . . ? C5 C6 C7 130.3(4) . . ? C6 C7 C1 133.1(4) . . ? _diffrn_measured_fraction_theta_max 0.938 _diffrn_reflns_theta_full 69.96 _diffrn_measured_fraction_theta_full 0.938 _refine_diff_density_max 0.284 _refine_diff_density_min -0.218 _refine_diff_density_rms 0.037 data_sfa84b _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety [Mg2(mu-Me)2L2] _chemical_formula_sum 'C60 H88 Mg2 N4' _chemical_formula_weight 913.96 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Mg' 'Mg' 0.1719 0.1771 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 14.068(5) _cell_length_b 14.903(7) _cell_length_c 14.110(5) _cell_angle_alpha 90.00 _cell_angle_beta 108.02(3) _cell_angle_gamma 90.00 _cell_volume 2813(2) _cell_formula_units_Z 2 _cell_measurement_temperature 220(2) _cell_measurement_reflns_used 50 _cell_measurement_theta_min 20 _cell_measurement_theta_max 22 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.29 _exptl_crystal_size_min 0.27 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.079 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1000 _exptl_absorpt_coefficient_mu 0.666 _exptl_absorpt_correction_type 'Optimised numerical' _exptl_absorpt_correction_T_min 0.701 _exptl_absorpt_correction_T_max 0.865 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 220(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method Omega-theta _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% +/-1 _diffrn_reflns_number 4881 _diffrn_reflns_av_R_equivalents 0.0872 _diffrn_reflns_av_sigmaI/netI 0.0378 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 4 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.88 _diffrn_reflns_theta_max 70.23 _reflns_number_total 4807 _reflns_number_gt 3228 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Stoe DIF4' _computing_cell_refinement 'Stoe DIF4' _computing_data_reduction 'Stoe REDU4' _computing_structure_solution SIR92 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1225P)^2^+1.1723P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geometric _refine_ls_hydrogen_treatment riding _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0012(4) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 4807 _refine_ls_number_parameters 343 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1054 _refine_ls_R_factor_gt 0.0720 _refine_ls_wR_factor_ref 0.2189 _refine_ls_wR_factor_gt 0.1910 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.021 _refine_ls_shift/su_max 0.022 _refine_ls_shift/su_mean 0.001 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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mg1 Mg 0.45491(7) 0.06369(6) 0.04763(7) 0.0339(3) Uani 0.929(3) 1 d P . 1 C1M C 0.4388(2) 0.0484(2) -0.1185(2) 0.0437(7) Uani 0.929(3) 1 d P . 1 H1M1 H 0.4848 0.0487 -0.1575 0.066 Uiso 0.929(3) 1 d PR . 1 H1M2 H 0.4188 0.1085 -0.1092 0.066 Uiso 0.929(3) 1 d PR . 1 H1M3 H 0.3810 0.0121 -0.1516 0.066 Uiso 0.929(3) 1 d PR . 1 N1 N 0.48926(19) 0.19454(17) 0.09654(19) 0.0416(6) Uani 0.929(3) 1 d P . 1 C11 C 0.5893(3) 0.2309(2) 0.1241(3) 0.0529(9) Uani 0.929(3) 1 d P . 1 C12 C 0.6505(3) 0.2179(3) 0.2231(3) 0.0634(10) Uani 0.929(3) 1 d P . 1 C13 C 0.7442(4) 0.2590(5) 0.2508(4) 0.0855(16) Uani 0.929(3) 1 d P . 1 H13 H 0.7857 0.2545 0.3172 0.103 Uiso 0.929(3) 1 calc PR . 1 C14 C 0.7769(4) 0.3058(4) 0.1833(5) 0.1038(19) Uani 0.929(3) 1 d P . 1 H14 H 0.8411 0.3313 0.2035 0.125 Uiso 0.929(3) 1 calc PR . 1 C15 C 0.7178(4) 0.3157(4) 0.0873(4) 0.0932(16) Uani 0.929(3) 1 d P . 1 H15 H 0.7423 0.3475 0.0422 0.112 Uiso 0.929(3) 1 calc PR . 1 C16 C 0.6215(3) 0.2798(3) 0.0544(3) 0.0674(11) Uani 0.929(3) 1 d P . 1 C17 C 0.6150(3) 0.1664(3) 0.2979(3) 0.0699(12) Uani 0.929(3) 1 d P . 1 H17 H 0.5584 0.1283 0.2600 0.084 Uiso 0.929(3) 1 calc PR . 1 C18 C 0.5763(4) 0.2292(4) 0.3623(4) 0.0964(17) Uani 0.929(3) 1 d P . 1 H18A H 0.5532 0.1943 0.4089 0.145 Uiso 0.929(3) 1 calc PR . 1 H18B H 0.5214 0.2644 0.3203 0.145 Uiso 0.929(3) 1 calc PR . 1 H18C H 0.6297 0.2689 0.3989 0.145 Uiso 0.929(3) 1 calc PR . 1 C19 C 0.6942(4) 0.1047(4) 0.3640(4) 0.0991(17) Uani 0.929(3) 1 d P . 1 H19A H 0.6665 0.0729 0.4094 0.149 Uiso 0.929(3) 1 calc PR . 1 H19B H 0.7512 0.1401 0.4019 0.149 Uiso 0.929(3) 1 calc PR . 1 H19C H 0.7154 0.0618 0.3229 0.149 Uiso 0.929(3) 1 calc PR . 1 C20 C 0.5546(4) 0.2981(3) -0.0521(3) 0.0756(12) Uani 0.929(3) 1 d P . 1 H20 H 0.4877 0.2722 -0.0603 0.091 Uiso 0.929(3) 1 calc PR . 1 C21 C 0.5955(5) 0.2567(4) -0.1272(5) 0.0997(18) Uani 0.929(3) 1 d P . 1 H21A H 0.5513 0.2694 -0.1936 0.149 Uiso 0.929(3) 1 calc PR . 1 H21B H 0.6008 0.1923 -0.1170 0.149 Uiso 0.929(3) 1 calc PR . 1 H21C H 0.6612 0.2813 -0.1199 0.149 Uiso 0.929(3) 1 calc PR . 1 C22 C 0.5421(6) 0.4003(4) -0.0782(5) 0.120(2) Uani 0.929(3) 1 d P . 1 H22A H 0.4979 0.4078 -0.1457 0.180 Uiso 0.929(3) 1 calc PR . 1 H22B H 0.6069 0.4262 -0.0728 0.180 Uiso 0.929(3) 1 calc PR . 1 H22C H 0.5138 0.4305 -0.0322 0.180 Uiso 0.929(3) 1 calc PR . 1 C2 C 0.4193(3) 0.2510(2) 0.1018(3) 0.0443(8) Uani 0.929(3) 1 d P . 1 C2M C 0.4385(3) 0.3504(2) 0.1232(3) 0.0621(10) Uani 0.929(3) 1 d P . 1 H2M1 H 0.5098 0.3607 0.1512 0.093 Uiso 0.929(3) 1 calc PR . 1 H2M2 H 0.4050 0.3698 0.1703 0.093 Uiso 0.929(3) 1 calc PR . 1 H2M3 H 0.4128 0.3841 0.0618 0.093 Uiso 0.929(3) 1 calc PR . 1 C3 C 0.3198(2) 0.2260(2) 0.0908(2) 0.0433(7) Uani 0.929(3) 1 d P . 1 H3 H 0.2740 0.2738 0.0798 0.052 Uiso 0.929(3) 1 calc PR . 1 C4 C 0.2788(2) 0.1411(2) 0.0938(2) 0.0396(7) Uani 0.929(3) 1 d P . 1 C4M C 0.1762(3) 0.1417(3) 0.1068(3) 0.0557(9) Uani 0.929(3) 1 d P . 1 H4M1 H 0.1291 0.1121 0.0504 0.083 Uiso 0.929(3) 1 calc PR . 1 H4M2 H 0.1551 0.2032 0.1107 0.083 Uiso 0.929(3) 1 calc PR . 1 H4M3 H 0.1784 0.1102 0.1676 0.083 Uiso 0.929(3) 1 calc PR . 1 N5 N 0.32455(18) 0.06414(16) 0.08727(18) 0.0371(6) Uani 0.929(3) 1 d P . 1 C51 C 0.2762(2) -0.0165(3) 0.1044(3) 0.0451(8) Uani 0.929(3) 1 d P . 1 C52 C 0.3027(3) -0.0514(3) 0.2008(3) 0.0583(10) Uani 0.929(3) 1 d P . 1 C53 C 0.2520(4) -0.1274(3) 0.2165(4) 0.0845(15) Uani 0.929(3) 1 d P . 1 H53 H 0.2676 -0.1515 0.2811 0.101 Uiso 0.929(3) 1 calc PR . 1 C54 C 0.1806(4) -0.1677(3) 0.1407(6) 0.0929(18) Uani 0.929(3) 1 d P . 1 H54 H 0.1484 -0.2195 0.1532 0.111 Uiso 0.929(3) 1 calc PR . 1 C55 C 0.1554(3) -0.1331(3) 0.0464(5) 0.0835(15) Uani 0.929(3) 1 d P . 1 H55 H 0.1064 -0.1621 -0.0054 0.100 Uiso 0.929(3) 1 calc PR . 1 C56 C 0.2008(3) -0.0560(3) 0.0256(3) 0.0616(10) Uani 0.929(3) 1 d P . 1 C57 C 0.3820(4) -0.0077(5) 0.2872(4) 0.083(2) Uani 0.929(3) 1 d P . 1 H57 H 0.4200 0.0348 0.2589 0.099 Uiso 0.929(3) 1 calc PR . 1 C58 C 0.4560(4) -0.0741(5) 0.3515(4) 0.111(2) Uani 0.929(3) 1 d P . 1 H58A H 0.5046 -0.0422 0.4048 0.167 Uiso 0.929(3) 1 calc PR . 1 H58B H 0.4900 -0.1054 0.3111 0.167 Uiso 0.929(3) 1 calc PR . 1 H58C H 0.4206 -0.1171 0.3798 0.167 Uiso 0.929(3) 1 calc PR . 1 C59 C 0.3334(5) 0.0467(5) 0.3537(4) 0.123(2) Uani 0.929(3) 1 d P . 1 H59A H 0.3852 0.0753 0.4071 0.185 Uiso 0.929(3) 1 calc PR . 1 H59B H 0.2949 0.0066 0.3819 0.185 Uiso 0.929(3) 1 calc PR . 1 H59C H 0.2896 0.0921 0.3138 0.185 Uiso 0.929(3) 1 calc PR . 1 C60 C 0.1648(3) -0.0141(4) -0.0799(4) 0.0770(15) Uani 0.929(3) 1 d P . 1 H60 H 0.1962 0.0458 -0.0763 0.092 Uiso 0.929(3) 1 calc PR . 1 C61 C 0.1976(5) -0.0686(5) -0.1500(5) 0.122(2) Uani 0.929(3) 1 d P . 1 H61A H 0.1752 -0.0411 -0.2155 0.183 Uiso 0.929(3) 1 calc PR . 1 H61B H 0.1693 -0.1283 -0.1534 0.183 Uiso 0.929(3) 1 calc PR . 1 H61C H 0.2699 -0.0725 -0.1277 0.183 Uiso 0.929(3) 1 calc PR . 1 C62 C 0.0493(3) -0.0015(4) -0.1224(4) 0.0823(13) Uani 0.929(3) 1 d P . 1 H62A H 0.0268 0.0370 -0.0781 0.123 Uiso 0.929(3) 1 calc PR . 1 H62B H 0.0168 -0.0594 -0.1275 0.123 Uiso 0.929(3) 1 calc PR . 1 H62C H 0.0326 0.0259 -0.1879 0.123 Uiso 0.929(3) 1 calc PR . 1 Mg1' Mg 0.4538(6) -0.0632(5) 0.0484(5) 0.035(4) Uani 0.071(3) 1 d P . 2 C1M' C 0.5827(6) 0.0199(5) 0.1510(5) 0.15(4) Uiso 0.071(3) 1 d PR . 2 H1M4 H 0.6492 0.0411 0.1555 0.232 Uiso 0.071(3) 1 d PR . 2 H1M5 H 0.5864 -0.0355 0.1862 0.232 Uiso 0.071(3) 1 d PR . 2 H1M6 H 0.5496 0.0654 0.1798 0.232 Uiso 0.071(3) 1 d PR . 2 N1' N 0.4886(6) -0.1963(5) 0.0921(5) 0.031(7) Uiso 0.071(3) 1 d PR . 2 C11' C 0.5898(6) -0.2293(5) 0.1289(5) 0.057(12) Uiso 0.071(3) 1 d PR . 2 C12' C 0.6209(6) -0.2887(5) 0.0653(5) 0.083(17) Uiso 0.071(3) 1 d PR . 2 C13' C 0.7215(6) -0.3114(5) 0.0964(5) 0.064(13) Uiso 0.071(3) 1 d PR . 2 H13' H 0.7504 -0.3359 0.0503 0.077 Uiso 0.071(3) 1 calc PR . 2 C14' C 0.7795(6) -0.2987(5) 0.1931(5) 0.077(16) Uiso 0.071(3) 1 d PR . 2 H14' H 0.8477 -0.3138 0.2120 0.092 Uiso 0.071(3) 1 calc PR . 2 C15' C 0.7391(6) -0.2636(5) 0.2645(5) 0.07(3) Uiso 0.071(3) 1 d PR . 2 H15' H 0.7693 -0.2735 0.3330 0.089 Uiso 0.071(3) 1 calc PR . 2 C16' C 0.6508(6) -0.2125(5) 0.2281(5) 0.037(9) Uiso 0.071(3) 1 d PR . 2 C17' C 0.5598(6) -0.2944(5) -0.0425(5) 0.079(16) Uiso 0.071(3) 1 d PR . 2 H17' H 0.4967 -0.2618 -0.0495 0.095 Uiso 0.071(3) 1 calc PR . 2 C18' C 0.5311(6) -0.3909(5) -0.0762(5) 0.066(14) Uiso 0.071(3) 1 d PR . 2 H18D H 0.4918 -0.3912 -0.1461 0.099 Uiso 0.071(3) 1 calc PR . 2 H18E H 0.4920 -0.4164 -0.0369 0.099 Uiso 0.071(3) 1 calc PR . 2 H18F H 0.5912 -0.4262 -0.0668 0.099 Uiso 0.071(3) 1 calc PR . 2 C19' C 0.6091(6) -0.2486(5) -0.1112(5) 0.020(12) Uiso 0.071(3) 1 d PR . 2 H19D H 0.5665 -0.2543 -0.1797 0.030 Uiso 0.071(3) 1 calc PR . 2 H19E H 0.6732 -0.2765 -0.1040 0.030 Uiso 0.071(3) 1 calc PR . 2 H19F H 0.6190 -0.1855 -0.0938 0.030 Uiso 0.071(3) 1 calc PR . 2 C20' C 0.6131(6) -0.1589(5) 0.3007(5) 0.069(14) Uiso 0.071(3) 1 d PR . 2 H20' H 0.5599 -0.1183 0.2611 0.083 Uiso 0.071(3) 1 calc PR . 2 C21' C 0.6922(6) -0.1023(5) 0.3687(5) 0.091(19) Uiso 0.071(3) 1 d PR . 2 H21D H 0.6644 -0.0695 0.4134 0.136 Uiso 0.071(3) 1 calc PR . 2 H21E H 0.7173 -0.0602 0.3298 0.136 Uiso 0.071(3) 1 calc PR . 2 H21F H 0.7464 -0.1402 0.4073 0.136 Uiso 0.071(3) 1 calc PR . 2 C22' C 0.5674(6) -0.2178(5) 0.3669(5) 0.10(2) Uiso 0.071(3) 1 d PR . 2 H22D H 0.5153 -0.2558 0.3247 0.152 Uiso 0.071(3) 1 calc PR . 2 H22E H 0.5391 -0.1794 0.4067 0.152 Uiso 0.071(3) 1 calc PR . 2 H22F H 0.6193 -0.2551 0.4105 0.152 Uiso 0.071(3) 1 calc PR . 2 C2' C 0.4181(6) -0.2498(5) 0.0997(5) 0.057(19) Uiso 0.071(3) 1 d PR . 2 C2M' C 0.4348(6) -0.3484(5) 0.1305(5) 0.042(9) Uiso 0.071(3) 1 d PR . 2 H2M4 H 0.5043 -0.3640 0.1413 0.063 Uiso 0.071(3) 1 calc PR . 2 H2M5 H 0.3925 -0.3859 0.0781 0.063 Uiso 0.071(3) 1 calc PR . 2 H2M6 H 0.4182 -0.3578 0.1915 0.063 Uiso 0.071(3) 1 calc PR . 2 C3' C 0.3173(6) -0.2264(5) 0.0838(5) 0.046(10) Uiso 0.071(3) 1 d PR . 2 H3' H 0.2704 -0.2729 0.0623 0.055 Uiso 0.071(3) 1 calc PR . 2 C4' C 0.2789(6) -0.1425(5) 0.0961(5) 0.046(10) Uiso 0.071(3) 1 d PR . 2 C4M' C 0.1751(6) -0.1444(5) 0.1074(5) 0.07(3) Uiso 0.071(3) 1 d PR . 2 H4M4 H 0.1541 -0.0837 0.1156 0.112 Uiso 0.071(3) 1 calc PR . 2 H4M5 H 0.1762 -0.1798 0.1654 0.112 Uiso 0.071(3) 1 calc PR . 2 H4M6 H 0.1286 -0.1710 0.0484 0.112 Uiso 0.071(3) 1 calc PR . 2 N5' N 0.3224(6) -0.0648(5) 0.0863(5) 0.035(7) Uiso 0.071(3) 1 d PR . 2 C51' C 0.2742(6) 0.0151(5) 0.1064(5) 0.015(10) Uiso 0.071(3) 1 d PR . 2 C52' C 0.1949(6) 0.0517(5) 0.0301(5) 0.060(12) Uiso 0.071(3) 1 d PR . 2 C53' C 0.1469(6) 0.1273(5) 0.0504(5) 0.11(3) Uiso 0.071(3) 1 d PR . 2 H53' H 0.0957 0.1540 -0.0011 0.129 Uiso 0.071(3) 1 calc PR . 2 C54' C 0.1730(6) 0.1637(5) 0.1445(5) 0.047(13) Uiso 0.071(3) 1 d PR . 2 H54' H 0.1363 0.2119 0.1582 0.057 Uiso 0.071(3) 1 calc PR . 2 C55' C 0.2520(6) 0.1296(5) 0.2177(5) 0.11(2) Uiso 0.071(3) 1 d PR . 2 H55' H 0.2706 0.1562 0.2811 0.131 Uiso 0.071(3) 1 calc PR . 2 C56' C 0.3060(6) 0.0562(5) 0.2009(5) 0.055(11) Uiso 0.071(3) 1 d PR . 2 C57' C 0.1673(6) 0.0127(5) -0.0740(5) 0.008(7) Uiso 0.071(3) 1 d PR . 2 H57' H 0.0970 -0.0079 -0.0924 0.010 Uiso 0.071(3) 1 calc PR . 2 C58' C 0.1762(6) 0.0789(5) -0.1527(5) 0.19(5) Uiso 0.071(3) 1 d PR . 2 H58D H 0.1575 0.0496 -0.2172 0.279 Uiso 0.071(3) 1 calc PR . 2 H58E H 0.2446 0.1000 -0.1361 0.279 Uiso 0.071(3) 1 calc PR . 2 H58F H 0.1321 0.1295 -0.1550 0.279 Uiso 0.071(3) 1 calc PR . 2 C59' C 0.2332(6) -0.0690(5) -0.0751(5) 0.038(9) Uiso 0.071(3) 1 d PR . 2 H59D H 0.2151 -0.0936 -0.1420 0.057 Uiso 0.071(3) 1 calc PR . 2 H59E H 0.2233 -0.1142 -0.0296 0.057 Uiso 0.071(3) 1 calc PR . 2 H59F H 0.3028 -0.0509 -0.0545 0.057 Uiso 0.071(3) 1 calc PR . 2 C60' C 0.3766(6) 0.0070(5) 0.2939(5) 0.034(16) Uiso 0.071(3) 1 d PR . 2 H60' H 0.4136 -0.0404 0.2709 0.041 Uiso 0.071(3) 1 calc PR . 2 C61' C 0.4487(6) 0.0720(5) 0.3542(5) 0.065(13) Uiso 0.071(3) 1 d PR . 2 H61D H 0.4853 0.0994 0.3137 0.098 Uiso 0.071(3) 1 calc PR . 2 H61E H 0.4951 0.0414 0.4103 0.098 Uiso 0.071(3) 1 calc PR . 2 H61F H 0.4133 0.1180 0.3785 0.098 Uiso 0.071(3) 1 calc PR . 2 C62' C 0.3181(6) -0.0368(5) 0.3590(5) 0.11(2) Uiso 0.071(3) 1 d PR . 2 H62D H 0.2705 -0.0797 0.3193 0.160 Uiso 0.071(3) 1 calc PR . 2 H62E H 0.2828 0.0093 0.3833 0.160 Uiso 0.071(3) 1 calc PR . 2 H62F H 0.3646 -0.0673 0.4152 0.160 Uiso 0.071(3) 1 calc PR . 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mg1 0.0326(5) 0.0342(5) 0.0357(5) -0.0024(4) 0.0115(4) -0.0004(4) C1M 0.0478(19) 0.0377(16) 0.0509(18) -0.0062(14) 0.0231(15) 0.0083(14) N1 0.0380(14) 0.0417(14) 0.0459(14) -0.0084(11) 0.0141(11) -0.0060(12) C11 0.0455(19) 0.0500(19) 0.065(2) -0.0192(17) 0.0200(17) -0.0143(16) C12 0.052(2) 0.064(2) 0.067(2) -0.022(2) 0.0081(18) -0.0122(19) C13 0.059(3) 0.097(4) 0.089(3) -0.036(4) 0.004(3) -0.021(3) C14 0.062(3) 0.117(5) 0.133(5) -0.041(4) 0.030(3) -0.043(3) C15 0.084(3) 0.094(4) 0.111(4) -0.024(3) 0.044(3) -0.048(3) C16 0.059(2) 0.062(2) 0.089(3) -0.012(2) 0.033(2) -0.022(2) C17 0.061(2) 0.081(3) 0.052(2) -0.012(2) -0.0055(18) -0.009(2) C18 0.085(3) 0.128(5) 0.076(3) 0.001(3) 0.024(3) 0.026(3) C19 0.104(4) 0.107(4) 0.067(3) -0.011(3) -0.002(3) 0.021(3) C20 0.083(3) 0.073(3) 0.082(3) 0.003(2) 0.040(3) -0.013(2) C21 0.113(5) 0.099(4) 0.103(4) -0.001(3) 0.056(4) 0.005(3) C22 0.174(6) 0.069(3) 0.128(5) 0.023(3) 0.064(5) 0.024(4) C2 0.047(2) 0.040(2) 0.0450(19) -0.0039(14) 0.0134(18) -0.0049(15) C2M 0.067(3) 0.0409(19) 0.077(3) -0.0125(18) 0.021(2) -0.0072(18) C3 0.0457(18) 0.0371(16) 0.0484(17) -0.0011(13) 0.0163(14) 0.0066(14) C4 0.0370(16) 0.0451(17) 0.0382(15) 0.0024(13) 0.0141(13) 0.0032(14) C4M 0.047(2) 0.062(2) 0.066(3) 0.000(2) 0.0295(19) 0.0079(18) N5 0.0373(14) 0.0355(13) 0.0409(13) 0.0028(11) 0.0156(11) 0.0005(11) C51 0.046(2) 0.036(2) 0.062(2) 0.0050(15) 0.0291(17) 0.0010(15) C52 0.059(2) 0.057(2) 0.070(2) 0.0205(18) 0.0355(19) 0.0043(18) C53 0.081(3) 0.079(3) 0.111(4) 0.046(3) 0.054(3) 0.008(3) C54 0.068(3) 0.060(3) 0.164(6) 0.033(4) 0.055(4) -0.005(2) C55 0.059(3) 0.061(3) 0.135(5) -0.001(3) 0.036(3) -0.020(2) C56 0.053(2) 0.056(2) 0.079(3) -0.006(2) 0.024(2) -0.0125(19) C57 0.095(4) 0.100(4) 0.055(3) 0.025(2) 0.026(3) 0.001(3) C58 0.098(4) 0.163(6) 0.073(3) 0.033(3) 0.026(3) 0.040(4) C59 0.154(6) 0.118(5) 0.083(4) -0.001(3) 0.016(4) 0.044(4) C60 0.070(3) 0.075(3) 0.091(4) -0.026(3) 0.032(2) -0.025(2) C61 0.092(4) 0.162(6) 0.118(5) -0.043(4) 0.042(4) 0.009(4) C62 0.054(2) 0.108(4) 0.086(3) 0.001(3) 0.023(2) 0.005(3) Mg1' 0.051(8) 0.029(6) 0.025(6) -0.001(5) 0.010(5) 0.000(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 N1 2.075(3) . ? Mg1 N5 2.076(3) . ? Mg1 C1M 2.259(3) 3_655 ? Mg1 C1M 2.296(3) . ? Mg1 Mg1 2.8416(19) 3_655 ? C1M Mg1 2.259(3) 3_655 ? N1 C2 1.315(5) . ? N1 C11 1.444(4) . ? C11 C16 1.407(5) . ? C11 C12 1.409(5) . ? C12 C13 1.395(6) . ? C12 C17 1.508(6) . ? C13 C14 1.371(8) . ? C14 C15 1.360(8) . ? C15 C16 1.396(6) . ? C16 C20 1.531(6) . ? C17 C18 1.518(6) . ? C17 C19 1.521(6) . ? C20 C21 1.488(7) . ? C20 C22 1.565(7) . ? C2 C3 1.410(5) . ? C2 C2M 1.519(5) . ? C3 C4 1.397(4) . ? C4 N5 1.332(4) . ? C4 C4M 1.511(4) . ? N5 C51 1.438(4) . ? C51 C52 1.395(5) . ? C51 C56 1.406(5) . ? C52 C53 1.393(6) . ? C52 C57 1.521(7) . ? C53 C54 1.360(7) . ? C54 C55 1.368(9) . ? C55 C56 1.390(6) . ? C56 C60 1.548(6) . ? C57 C58 1.517(7) . ? C57 C59 1.551(9) . ? C60 C61 1.460(7) . ? C60 C62 1.560(6) . ? Mg1' N5' 2.0781 . ? Mg1' N1' 2.0906 . ? Mg1' C1M' 2.3008 . ? Mg1' C1M' 2.775(14) 3_655 ? Mg1' Mg1' 2.863(15) 3_655 ? C1M' Mg1' 2.775(14) 3_655 ? N1' C2' 1.3013 . ? N1' C11' 1.4428 . ? C11' C16' 1.4195 . ? C11' C12' 1.4231 . ? C12' C13' 1.3883 . ? C12' C17' 1.5002 . ? C13' C14' 1.3688 . ? C14' C15' 1.4024 . ? C15' C16' 1.4107 . ? C16' C20' 1.5183 . ? C17' C19' 1.5166 . ? C17' C18' 1.5287 . ? C20' C21' 1.4864 . ? C20' C22' 1.5588 . ? C2' C3' 1.4097 . ? C2' C2M' 1.5302 . ? C3' C4' 1.3936 . ? C4' N5' 1.3366 . ? C4' C4M' 1.5173 . ? N5' C51' 1.4414 . ? C51' C52' 1.3996 . ? C51' C56' 1.4084 . ? C52' C53' 1.3883 . ? C52' C57' 1.5137 . ? C53' C54' 1.3749 . ? C54' C55' 1.3594 . ? C55' C56' 1.3932 . ? C56' C60' 1.5617 . ? C57' C58' 1.5195 . ? C57' C59' 1.5323 . ? C60' C61' 1.4680 . ? C60' C62' 1.5542 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Mg1 N5 92.39(10) . . ? N1 Mg1 C1M 119.55(12) . 3_655 ? N5 Mg1 C1M 113.72(11) . 3_655 ? N1 Mg1 C1M 111.87(11) . . ? N5 Mg1 C1M 117.31(12) . . ? C1M Mg1 C1M 102.80(11) 3_655 . ? N1 Mg1 Mg1 133.87(9) . 3_655 ? N5 Mg1 Mg1 133.66(9) . 3_655 ? C1M Mg1 Mg1 51.99(8) 3_655 3_655 ? C1M Mg1 Mg1 50.82(8) . 3_655 ? Mg1 C1M Mg1 77.20(11) 3_655 . ? C2 N1 C11 115.4(3) . . ? C2 N1 Mg1 121.3(2) . . ? C11 N1 Mg1 123.3(2) . . ? C16 C11 C12 122.3(3) . . ? C16 C11 N1 120.3(3) . . ? C12 C11 N1 117.4(3) . . ? C13 C12 C11 116.9(4) . . ? C13 C12 C17 121.0(4) . . ? C11 C12 C17 122.0(3) . . ? C14 C13 C12 121.3(5) . . ? C15 C14 C13 121.0(5) . . ? C14 C15 C16 121.4(5) . . ? C15 C16 C11 117.1(4) . . ? C15 C16 C20 119.8(4) . . ? C11 C16 C20 123.0(3) . . ? C12 C17 C18 111.3(4) . . ? C12 C17 C19 113.5(4) . . ? C18 C17 C19 109.6(4) . . ? C21 C20 C16 111.7(4) . . ? C21 C20 C22 106.0(4) . . ? C16 C20 C22 113.2(4) . . ? N1 C2 C3 124.0(3) . . ? N1 C2 C2M 123.1(4) . . ? C3 C2 C2M 112.9(3) . . ? C4 C3 C2 129.9(3) . . ? N5 C4 C3 124.5(3) . . ? N5 C4 C4M 120.9(3) . . ? C3 C4 C4M 114.6(3) . . ? C4 N5 C51 116.4(3) . . ? C4 N5 Mg1 120.5(2) . . ? C51 N5 Mg1 123.1(2) . . ? C52 C51 C56 121.6(4) . . ? C52 C51 N5 118.5(3) . . ? C56 C51 N5 119.9(3) . . ? C53 C52 C51 117.6(4) . . ? C53 C52 C57 120.3(4) . . ? C51 C52 C57 122.1(3) . . ? C54 C53 C52 121.6(5) . . ? C53 C54 C55 120.4(4) . . ? C54 C55 C56 121.2(5) . . ? C55 C56 C51 117.6(4) . . ? C55 C56 C60 120.1(4) . . ? C51 C56 C60 122.2(4) . . ? C58 C57 C52 113.5(6) . . ? C58 C57 C59 109.1(4) . . ? C52 C57 C59 110.9(5) . . ? C61 C60 C56 110.5(5) . . ? C61 C60 C62 108.4(4) . . ? C56 C60 C62 114.1(4) . . ? N5' Mg1' N1' 93.3 . . ? N5' Mg1' C1M' 115.8 . . ? N1' Mg1' C1M' 105.0 . . ? N5' Mg1' C1M' 111.3(3) . 3_655 ? N1' Mg1' C1M' 118.2(3) . 3_655 ? C1M' Mg1' C1M' 112.1(3) . 3_655 ? N5' Mg1' Mg1' 134.6(3) . 3_655 ? N1' Mg1' Mg1' 131.7(3) . 3_655 ? C1M' Mg1' Mg1' 63.9(3) . 3_655 ? C1M' Mg1' Mg1' 48.1(2) 3_655 3_655 ? Mg1' C1M' Mg1' 67.9(3) . 3_655 ? C2' N1' C11' 116.9 . . ? C2' N1' Mg1' 119.4 . . ? C11' N1' Mg1' 123.0 . . ? C16' C11' C12' 121.4 . . ? C16' C11' N1' 121.6 . . ? C12' C11' N1' 116.5 . . ? C13' C12' C11' 115.8 . . ? C13' C12' C17' 121.0 . . ? C11' C12' C17' 118.9 . . ? C14' C13' C12' 121.1 . . ? C13' C14' C15' 121.3 . . ? C14' C15' C16' 116.5 . . ? C15' C16' C11' 117.4 . . ? C15' C16' C20' 119.3 . . ? C11' C16' C20' 121.8 . . ? C12' C17' C19' 113.0 . . ? C12' C17' C18' 112.5 . . ? C19' C17' C18' 110.8 . . ? C21' C20' C16' 112.7 . . ? C21' C20' C22' 107.4 . . ? C16' C20' C22' 113.8 . . ? N1' C2' C3' 126.2 . . ? N1' C2' C2M' 123.9 . . ? C3' C2' C2M' 109.9 . . ? C4' C3' C2' 127.7 . . ? N5' C4' C3' 123.8 . . ? N5' C4' C4M' 120.9 . . ? C3' C4' C4M' 114.8 . . ? C4' N5' C51' 116.0 . . ? C4' N5' Mg1' 120.6 . . ? C51' N5' Mg1' 123.4 . . ? C52' C51' C56' 120.2 . . ? C52' C51' N5' 118.8 . . ? C56' C51' N5' 121.0 . . ? C53' C52' C51' 118.6 . . ? C53' C52' C57' 121.1 . . ? C51' C52' C57' 120.1 . . ? C54' C53' C52' 121.2 . . ? C55' C54' C53' 119.8 . . ? C54' C55' C56' 121.7 . . ? C55' C56' C51' 118.1 . . ? C55' C56' C60' 117.7 . . ? C51' C56' C60' 121.7 . . ? C52' C57' C58' 113.9 . . ? C52' C57' C59' 109.9 . . ? C58' C57' C59' 108.8 . . ? C61' C60' C62' 109.3 . . ? C61' C60' C56' 108.9 . . ? C62' C60' C56' 112.2 . . ? _diffrn_measured_fraction_theta_max 0.898 _diffrn_reflns_theta_full 70.23 _diffrn_measured_fraction_theta_full 0.898 _refine_diff_density_max 0.407 _refine_diff_density_min -0.249 _refine_diff_density_rms 0.050 data_mgsf68 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety [MgLMe(thf)].0.5C6H14 _chemical_formula_sum 'C37 H59 Mg N2 O' _chemical_formula_weight 572.17 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Mg' 'Mg' 0.1719 0.1771 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.136(3) _cell_length_b 12.690(5) _cell_length_c 16.004(6) _cell_angle_alpha 99.00(3) _cell_angle_beta 96.17(3) _cell_angle_gamma 95.19(2) _cell_volume 1811.2(11) _cell_formula_units_Z 2 _cell_measurement_temperature 220(2) _cell_measurement_reflns_used 64 _cell_measurement_theta_min 20 _cell_measurement_theta_max 22 _exptl_crystal_description plate _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.54 _exptl_crystal_size_mid 0.45 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.049 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 630 _exptl_absorpt_coefficient_mu 0.621 _exptl_absorpt_correction_type Psi-scans _exptl_absorpt_correction_T_min 0.825 _exptl_absorpt_correction_T_max 0.981 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 220(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method Omega-theta _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% -2 _diffrn_reflns_number 5022 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.1242 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.82 _diffrn_reflns_theta_max 60.08 _reflns_number_total 5022 _reflns_number_gt 2393 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Stoe DIF4' _computing_cell_refinement 'Stoe DIF4' _computing_data_reduction 'Stoe REDU4' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1204P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geometric _refine_ls_hydrogen_treatment riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5022 _refine_ls_number_parameters 375 _refine_ls_number_restraints 402 _refine_ls_R_factor_all 0.1767 _refine_ls_R_factor_gt 0.0840 _refine_ls_wR_factor_ref 0.2445 _refine_ls_wR_factor_gt 0.1912 _refine_ls_goodness_of_fit_ref 0.961 _refine_ls_restrained_S_all 0.932 _refine_ls_shift/su_max 0.002 _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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mg1 Mg 0.06144(17) 0.63400(14) 0.72390(11) 0.0398(5) Uani 1 1 d U . . C1M C 0.2436(6) 0.6358(6) 0.6536(4) 0.0676(18) Uani 1 1 d U . . H1M1 H 0.2528 0.5633 0.6261 0.101 Uiso 1 1 d R . . H1M2 H 0.3333 0.6636 0.6917 0.101 Uiso 1 1 d R . . H1M3 H 0.2286 0.6811 0.6107 0.101 Uiso 1 1 d R . . N1 N 0.0451(4) 0.7411(3) 0.8325(3) 0.0377(10) Uani 1 1 d U . . C1A C 0.1210(5) 0.8477(4) 0.8470(3) 0.0424(13) Uani 1 1 d U . . C2A C 0.2733(6) 0.8628(4) 0.8799(4) 0.0537(15) Uani 1 1 d U . . C3A C 0.3473(7) 0.9641(5) 0.8904(4) 0.0673(18) Uani 1 1 d U . . H3A H 0.4478 0.9747 0.9131 0.081 Uiso 1 1 calc R . . C4A C 0.2798(7) 1.0513(5) 0.8689(4) 0.0690(18) Uani 1 1 d U . . H4A H 0.3331 1.1198 0.8768 0.083 Uiso 1 1 calc R . . C5A C 0.1326(7) 1.0352(5) 0.8358(4) 0.0596(16) Uani 1 1 d U . . H5A H 0.0859 1.0938 0.8209 0.072 Uiso 1 1 calc R . . C6A C 0.0509(6) 0.9352(4) 0.8237(4) 0.0483(14) Uani 1 1 d U . . C7A C 0.3525(6) 0.7708(5) 0.9054(5) 0.0679(18) Uani 1 1 d U . . H7A H 0.2965 0.7035 0.8735 0.081 Uiso 1 1 calc R . . C8A C 0.3498(8) 0.7677(6) 1.0005(6) 0.098(3) Uani 1 1 d U . . H8A1 H 0.3981 0.7070 1.0154 0.147 Uiso 1 1 calc R . . H8A2 H 0.2479 0.7605 1.0127 0.147 Uiso 1 1 calc R . . H8A3 H 0.4015 0.8336 1.0337 0.147 Uiso 1 1 calc R . . C9A C 0.5092(7) 0.7729(7) 0.8826(6) 0.102(3) Uani 1 1 d U . . H9A1 H 0.5535 0.7115 0.8993 0.153 Uiso 1 1 calc R . . H9A2 H 0.5671 0.8385 0.9123 0.153 Uiso 1 1 calc R . . H9A3 H 0.5075 0.7701 0.8216 0.153 Uiso 1 1 calc R . . C10A C -0.1099(7) 0.9235(5) 0.7852(4) 0.0671(18) Uani 1 1 d U . . H10A H -0.1541 0.8508 0.7898 0.081 Uiso 1 1 calc R . . C11A C -0.1182(9) 0.9312(6) 0.6906(5) 0.099(3) Uani 1 1 d U . . H11A H -0.2211 0.9221 0.6657 0.148 Uiso 1 1 calc R . . H11B H -0.0665 0.8754 0.6620 0.148 Uiso 1 1 calc R . . H11C H -0.0724 1.0009 0.6841 0.148 Uiso 1 1 calc R . . C12A C -0.1997(7) 1.0049(6) 0.8327(6) 0.094(2) Uani 1 1 d U . . H12A H -0.1938 0.9967 0.8922 0.141 Uiso 1 1 calc R . . H12B H -0.3024 0.9923 0.8073 0.141 Uiso 1 1 calc R . . H12C H -0.1598 1.0771 0.8285 0.141 Uiso 1 1 calc R . . C2 C -0.0365(5) 0.7135(4) 0.8923(3) 0.0393(12) Uani 1 1 d U . . C2M C -0.0636(6) 0.7971(5) 0.9662(4) 0.0541(15) Uani 1 1 d U . . H2M1 H -0.0940 0.8601 0.9448 0.081 Uiso 1 1 d R . . H2M2 H 0.0267 0.8168 1.0055 0.081 Uiso 1 1 d R . . H2M3 H -0.1411 0.7677 0.9957 0.081 Uiso 1 1 d R . . C3 C -0.0956(5) 0.6086(4) 0.8940(3) 0.0411(12) Uani 1 1 d U . . H3 H -0.1669 0.6028 0.9317 0.049 Uiso 1 1 calc R . . C4 C -0.0662(5) 0.5099(4) 0.8485(3) 0.0388(12) Uani 1 1 d U . . C4M C -0.1179(6) 0.4122(4) 0.8842(4) 0.0493(14) Uani 1 1 d U . . H4M1 H -0.2251 0.4048 0.8806 0.074 Uiso 1 1 d R . . H4M2 H -0.0755 0.4198 0.9434 0.074 Uiso 1 1 d R . . H4M3 H -0.0863 0.3490 0.8517 0.074 Uiso 1 1 d R . . N5 N 0.0069(4) 0.5024(3) 0.7799(3) 0.0384(10) Uani 1 1 d U . . C1B C 0.0453(6) 0.3994(4) 0.7422(4) 0.0435(12) Uani 1 1 d U . . C2B C 0.1963(6) 0.3790(4) 0.7578(4) 0.0458(13) Uani 1 1 d U . . C3B C 0.2361(7) 0.2840(5) 0.7184(4) 0.0628(17) Uani 1 1 d U . . H3B H 0.3345 0.2689 0.7295 0.075 Uiso 1 1 calc R . . C4B C 0.1378(7) 0.2099(5) 0.6633(5) 0.0698(19) Uani 1 1 d U . . H4B H 0.1690 0.1462 0.6360 0.084 Uiso 1 1 calc R . . C5B C -0.0066(7) 0.2305(5) 0.6486(4) 0.0626(17) Uani 1 1 d U . . H5B H -0.0740 0.1803 0.6106 0.075 Uiso 1 1 calc R . . C6B C -0.0557(6) 0.3228(4) 0.6882(4) 0.0455(13) Uani 1 1 d U . . C7B C 0.3070(6) 0.4581(5) 0.8192(4) 0.0548(15) Uani 1 1 d U . . H7B H 0.2766 0.5306 0.8167 0.066 Uiso 1 1 calc R . . C8B C 0.3048(8) 0.4394(7) 0.9100(5) 0.096(3) Uani 1 1 d U . . H8B1 H 0.3748 0.4927 0.9477 0.144 Uiso 1 1 calc R . . H8B2 H 0.3320 0.3683 0.9146 0.144 Uiso 1 1 calc R . . H8B3 H 0.2061 0.4454 0.9261 0.144 Uiso 1 1 calc R . . C9B C 0.4666(7) 0.4589(6) 0.7955(5) 0.089(2) Uani 1 1 d U . . H9B1 H 0.5318 0.5121 0.8362 0.133 Uiso 1 1 calc R . . H9B2 H 0.4684 0.4765 0.7387 0.133 Uiso 1 1 calc R . . H9B3 H 0.4997 0.3886 0.7966 0.133 Uiso 1 1 calc R . . C10B C -0.2172(6) 0.3405(5) 0.6706(4) 0.0547(15) Uani 1 1 d U . . H10B H -0.2354 0.4064 0.7083 0.066 Uiso 1 1 calc R . . C11B C -0.3211(6) 0.2441(5) 0.6878(5) 0.076(2) Uani 1 1 d U . . H11D H -0.4234 0.2585 0.6777 0.114 Uiso 1 1 calc R . . H11E H -0.2986 0.2342 0.7465 0.114 Uiso 1 1 calc R . . H11F H -0.3061 0.1795 0.6499 0.114 Uiso 1 1 calc R . . C12B C -0.2526(8) 0.3547(6) 0.5789(4) 0.085(2) Uani 1 1 d U . . H12D H -0.3554 0.3680 0.5685 0.128 Uiso 1 1 calc R . . H12E H -0.2362 0.2902 0.5414 0.128 Uiso 1 1 calc R . . H12F H -0.1890 0.4152 0.5679 0.128 Uiso 1 1 calc R . . O1T O -0.1246(4) 0.6446(3) 0.6413(2) 0.0511(10) Uani 1 1 d DU B . C2T C -0.2753(5) 0.6429(5) 0.6624(4) 0.0573(16) Uani 1 1 d DU . . H2T1 H -0.2797 0.6919 0.7157 0.069 Uiso 0.50 1 calc PR A 1 H2T2 H -0.3143 0.5703 0.6687 0.069 Uiso 0.50 1 calc PR A 1 H2T3 H -0.2908 0.7117 0.6958 0.069 Uiso 0.50 1 calc PR A 2 H2T4 H -0.2973 0.5856 0.6953 0.069 Uiso 0.50 1 calc PR A 2 C3T C -0.3606(13) 0.6784(16) 0.5896(9) 0.085(4) Uani 0.50 1 d PDU B 1 H3T1 H -0.4481 0.6268 0.5683 0.102 Uiso 0.50 1 calc PR B 1 H3T2 H -0.3944 0.7483 0.6087 0.102 Uiso 0.50 1 calc PR B 1 C4T C -0.2726(12) 0.6866(15) 0.5236(8) 0.065(4) Uani 0.50 1 d PDU B 1 H4T1 H -0.2608 0.7607 0.5131 0.078 Uiso 0.50 1 calc PR B 1 H4T2 H -0.3188 0.6401 0.4709 0.078 Uiso 0.50 1 calc PR B 1 C5T C -0.1233(6) 0.6519(6) 0.5519(4) 0.0631(17) Uani 1 1 d DU . . H5T1 H -0.1102 0.5823 0.5190 0.076 Uiso 0.50 1 calc PR B 1 H5T2 H -0.0429 0.7049 0.5444 0.076 Uiso 0.50 1 calc PR B 1 H5T3 H -0.0724 0.5943 0.5235 0.076 Uiso 0.50 1 calc PR B 2 H5T4 H -0.0728 0.7211 0.5455 0.076 Uiso 0.50 1 calc PR B 2 C3T' C -0.3722(14) 0.6223(12) 0.5769(8) 0.066(5) Uiso 0.50 1 d PDU B 2 H3T3 H -0.4186 0.5479 0.5648 0.079 Uiso 0.50 1 calc PR B 2 H3T4 H -0.4506 0.6701 0.5779 0.079 Uiso 0.50 1 calc PR B 2 C4T' C -0.2833(13) 0.6411(15) 0.5146(9) 0.074(6) Uiso 0.50 1 d PDU B 2 H4T3 H -0.3059 0.7070 0.4936 0.089 Uiso 0.50 1 calc PR B 2 H4T4 H -0.3027 0.5815 0.4666 0.089 Uiso 0.50 1 calc PR B 2 C1S C 0.4286(11) 0.0036(13) 0.5189(10) 0.091(5) Uiso 0.50 1 d PDU . 1 H1S1 H 0.3449 -0.0257 0.4754 0.109 Uiso 0.50 1 calc PR . 1 H1S2 H 0.4169 0.0788 0.5399 0.109 Uiso 0.50 1 calc PR . 1 C2S C 0.431(2) -0.0617(17) 0.5939(13) 0.131(7) Uiso 0.50 1 d PDU C 1 H2S1 H 0.4668 -0.1317 0.5774 0.157 Uiso 0.50 1 calc PR C 1 H2S2 H 0.4953 -0.0225 0.6442 0.157 Uiso 0.50 1 calc PR C 1 C3S C 0.268(2) -0.0755(18) 0.6120(15) 0.145(8) Uiso 0.50 1 d PDU C 1 H3S1 H 0.2611 -0.1151 0.6588 0.218 Uiso 0.50 1 calc PR C 1 H3S2 H 0.2070 -0.1146 0.5615 0.218 Uiso 0.50 1 calc PR C 1 H3S3 H 0.2348 -0.0054 0.6270 0.218 Uiso 0.50 1 calc PR C 1 C1S' C 0.507(3) -0.031(2) 0.5357(13) 0.199(11) Uiso 0.50 1 d PDU . 2 H1S3 H 0.5827 0.0041 0.5821 0.239 Uiso 0.50 1 calc PR . 2 H1S4 H 0.5283 -0.1047 0.5165 0.239 Uiso 0.50 1 calc PR . 2 C2S' C 0.348(3) -0.028(3) 0.5620(16) 0.207(11) Uiso 0.50 1 d PDU D 2 H2S3 H 0.2789 -0.0866 0.5286 0.249 Uiso 0.50 1 calc PR D 2 H2S4 H 0.3104 0.0409 0.5571 0.249 Uiso 0.50 1 calc PR D 2 C3S' C 0.381(3) -0.0429(19) 0.6567(14) 0.160(9) Uiso 0.50 1 d PDU D 2 H3S4 H 0.2905 -0.0418 0.6831 0.240 Uiso 0.50 1 calc PR D 2 H3S5 H 0.4535 0.0148 0.6870 0.240 Uiso 0.50 1 calc PR D 2 H3S6 H 0.4202 -0.1112 0.6590 0.240 Uiso 0.50 1 calc PR D 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mg1 0.0301(9) 0.0483(11) 0.0439(11) 0.0133(9) 0.0080(8) 0.0063(8) C1M 0.051(3) 0.099(5) 0.060(4) 0.023(4) 0.022(3) 0.014(3) N1 0.026(2) 0.042(2) 0.045(3) 0.009(2) -0.0007(18) 0.0058(18) C1A 0.033(3) 0.042(3) 0.053(3) 0.008(3) 0.004(2) 0.010(2) C2A 0.041(3) 0.048(3) 0.069(4) 0.007(3) 0.000(3) 0.006(2) C3A 0.043(3) 0.057(4) 0.097(5) 0.004(4) 0.001(3) 0.002(3) C4A 0.059(4) 0.051(4) 0.091(5) 0.003(4) 0.003(4) -0.009(3) C5A 0.056(3) 0.052(3) 0.071(4) 0.010(3) 0.005(3) 0.007(3) C6A 0.043(3) 0.047(3) 0.054(4) 0.009(3) 0.003(3) 0.004(2) C7A 0.034(3) 0.055(4) 0.112(5) 0.015(4) -0.009(3) 0.011(3) C8A 0.073(5) 0.101(6) 0.133(6) 0.061(6) 0.006(5) 0.014(4) C9A 0.054(4) 0.114(6) 0.141(7) 0.011(6) 0.016(4) 0.038(4) C10A 0.054(3) 0.058(4) 0.087(5) 0.013(4) -0.010(3) 0.013(3) C11A 0.113(6) 0.081(5) 0.093(5) 0.018(5) -0.036(5) 0.007(5) C12A 0.054(4) 0.080(5) 0.149(7) 0.016(5) 0.000(4) 0.030(4) C2 0.024(3) 0.050(3) 0.043(3) 0.007(3) 0.001(2) 0.009(2) C2M 0.051(4) 0.064(4) 0.046(3) 0.004(3) 0.008(3) 0.008(3) C3 0.031(3) 0.059(3) 0.037(3) 0.015(3) 0.008(2) 0.008(2) C4 0.026(3) 0.050(3) 0.043(3) 0.016(3) 0.002(2) 0.007(2) C4M 0.043(3) 0.059(3) 0.052(4) 0.019(3) 0.014(3) 0.010(3) N5 0.031(2) 0.045(2) 0.041(3) 0.009(2) 0.0047(19) 0.0112(19) C1B 0.039(3) 0.044(3) 0.053(3) 0.015(3) 0.015(2) 0.011(2) C2B 0.038(3) 0.045(3) 0.061(4) 0.017(3) 0.015(3) 0.014(2) C3B 0.048(3) 0.054(4) 0.096(5) 0.019(3) 0.024(3) 0.023(3) C4B 0.065(4) 0.045(4) 0.103(6) 0.003(3) 0.033(4) 0.019(3) C5B 0.063(4) 0.048(3) 0.077(5) 0.003(3) 0.018(3) 0.007(3) C6B 0.045(3) 0.040(3) 0.053(3) 0.006(3) 0.013(3) 0.006(2) C7B 0.029(3) 0.072(4) 0.068(4) 0.016(3) 0.011(3) 0.020(3) C8B 0.068(5) 0.155(8) 0.066(4) 0.021(5) 0.004(4) 0.020(5) C9B 0.046(4) 0.100(6) 0.122(6) 0.011(5) 0.025(4) 0.009(4) C10B 0.040(3) 0.061(4) 0.059(4) 0.003(3) 0.000(3) 0.009(3) C11B 0.040(3) 0.072(4) 0.110(6) -0.003(4) 0.011(4) 0.004(3) C12B 0.083(5) 0.099(6) 0.069(5) 0.005(4) -0.011(4) 0.024(4) O1T 0.0351(19) 0.076(3) 0.047(2) 0.020(2) 0.0085(16) 0.0105(18) C2T 0.032(3) 0.077(4) 0.066(4) 0.017(3) 0.012(3) 0.007(3) C3T 0.042(6) 0.120(13) 0.105(10) 0.047(10) 0.004(6) 0.030(8) C4T 0.058(7) 0.084(11) 0.052(7) 0.017(8) -0.016(5) 0.014(7) C5T 0.053(3) 0.101(5) 0.040(3) 0.020(3) 0.008(3) 0.017(3) _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 N1 2.061(5) . ? Mg1 N5 2.063(5) . ? Mg1 O1T 2.066(4) . ? Mg1 C1M 2.107(6) . ? N1 C2 1.344(6) . ? N1 C1A 1.435(6) . ? C1A C6A 1.411(7) . ? C1A C2A 1.418(7) . ? C2A C3A 1.375(8) . ? C2A C7A 1.514(8) . ? C3A C4A 1.386(8) . ? C4A C5A 1.376(8) . ? C5A C6A 1.388(8) . ? C6A C10A 1.516(8) . ? C7A C9A 1.514(9) . ? C7A C8A 1.532(10) . ? C10A C11A 1.526(10) . ? C10A C12A 1.536(9) . ? C2 C3 1.396(7) . ? C2 C2M 1.518(7) . ? C3 C4 1.410(7) . ? C4 N5 1.341(6) . ? C4 C4M 1.504(7) . ? N5 C1B 1.442(6) . ? C1B C6B 1.396(7) . ? C1B C2B 1.429(7) . ? C2B C3B 1.369(8) . ? C2B C7B 1.513(8) . ? C3B C4B 1.373(9) . ? C4B C5B 1.371(8) . ? C5B C6B 1.377(8) . ? C6B C10B 1.515(7) . ? C7B C8B 1.510(9) . ? C7B C9B 1.545(8) . ? C10B C12B 1.511(9) . ? C10B C11B 1.558(8) . ? O1T C5T 1.448(6) . ? O1T C2T 1.453(6) . ? C2T C3T 1.484(11) . ? C2T C3T' 1.520(12) . ? C3T C4T 1.405(13) . ? C4T C5T 1.515(10) . ? C5T C4T' 1.504(12) . ? C3T' C4T' 1.386(14) . ? C1S C1S 1.500(10) 2_656 ? C1S C2S 1.561(15) . ? C2S C3S 1.546(16) . ? C1S' C1S' 1.490(10) 2_656 ? C1S' C2S' 1.552(17) . ? C2S' C3S' 1.557(17) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Mg1 N5 93.09(18) . . ? N1 Mg1 O1T 105.12(16) . . ? N5 Mg1 O1T 104.74(16) . . ? N1 Mg1 C1M 124.7(2) . . ? N5 Mg1 C1M 119.5(2) . . ? O1T Mg1 C1M 107.3(2) . . ? C2 N1 C1A 117.7(4) . . ? C2 N1 Mg1 121.1(3) . . ? C1A N1 Mg1 121.1(3) . . ? C6A C1A C2A 119.7(5) . . ? C6A C1A N1 121.6(4) . . ? C2A C1A N1 118.6(4) . . ? C3A C2A C1A 118.5(5) . . ? C3A C2A C7A 120.3(5) . . ? C1A C2A C7A 121.2(5) . . ? C2A C3A C4A 122.6(6) . . ? C5A C4A C3A 118.3(6) . . ? C4A C5A C6A 122.2(6) . . ? C5A C6A C1A 118.7(5) . . ? C5A C6A C10A 118.9(5) . . ? C1A C6A C10A 122.3(5) . . ? C2A C7A C9A 113.2(6) . . ? C2A C7A C8A 110.5(6) . . ? C9A C7A C8A 111.0(6) . . ? C6A C10A C11A 109.4(6) . . ? C6A C10A C12A 112.6(6) . . ? C11A C10A C12A 111.7(6) . . ? N1 C2 C3 123.9(5) . . ? N1 C2 C2M 120.5(5) . . ? C3 C2 C2M 115.5(5) . . ? C2 C3 C4 130.7(5) . . ? N5 C4 C3 123.2(5) . . ? N5 C4 C4M 121.6(5) . . ? C3 C4 C4M 115.2(5) . . ? C4 N5 C1B 119.6(4) . . ? C4 N5 Mg1 121.8(3) . . ? C1B N5 Mg1 118.6(3) . . ? C6B C1B C2B 119.5(5) . . ? C6B C1B N5 122.9(5) . . ? C2B C1B N5 117.5(5) . . ? C3B C2B C1B 118.0(5) . . ? C3B C2B C7B 121.1(5) . . ? C1B C2B C7B 120.8(5) . . ? C2B C3B C4B 122.5(6) . . ? C5B C4B C3B 118.9(6) . . ? C4B C5B C6B 121.8(6) . . ? C5B C6B C1B 119.2(5) . . ? C5B C6B C10B 119.5(5) . . ? C1B C6B C10B 121.3(5) . . ? C8B C7B C2B 111.7(5) . . ? C8B C7B C9B 110.0(5) . . ? C2B C7B C9B 113.2(5) . . ? C12B C10B C6B 109.9(5) . . ? C12B C10B C11B 109.0(5) . . ? C6B C10B C11B 111.3(5) . . ? C5T O1T C2T 109.8(4) . . ? C5T O1T Mg1 124.3(3) . . ? C2T O1T Mg1 125.9(3) . . ? O1T C2T C3T 104.8(6) . . ? O1T C2T C3T' 104.8(6) . . ? C3T C2T C3T' 27.1(9) . . ? C4T C3T C2T 110.5(8) . . ? C3T C4T C5T 107.2(8) . . ? O1T C5T C4T' 105.7(6) . . ? O1T C5T C4T 105.3(6) . . ? C4T' C5T C4T 21.7(11) . . ? C4T' C3T' C2T 108.2(9) . . ? C3T' C4T' C5T 109.2(10) . . ? C1S C1S C2S 108.7(16) 2_656 . ? C3S C2S C1S 104.6(13) . . ? C1S' C1S' C2S' 99(2) 2_656 . ? C1S' C2S' C3S' 99.4(16) . . ? _diffrn_measured_fraction_theta_max 0.934 _diffrn_reflns_theta_full 60.08 _diffrn_measured_fraction_theta_full 0.934 _refine_diff_density_max 0.285 _refine_diff_density_min -0.335 _refine_diff_density_rms 0.064