Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2003 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Kenneth Henderson' 'Gordon W. Honeyman' 'Alan R. Kennedy' 'Robert E. Mulvey' 'John A. Parkinson' 'David Colin Sherrington' _publ_contact_author_name 'Prof Kenneth Henderson' _publ_contact_author_address ; Chemistry and Biochemistry University of Notre Dame 251 Nieuwland Science Hall Notre Dame IN 46556 UNITED STATES OF AMERICA ; _publ_contact_author_email KHENDERS@ND.EDU _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Magnesium Aryloxides: Synthesis, Structure, Solution Behavior and Magnesiate Ion Formation ; data_he14 _database_code_CSD 200471 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H60 Mg2 O2' _chemical_formula_weight 573.46 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Mg Mg 0.0486 0.0363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.9509(3) _cell_length_b 10.4326(2) _cell_length_c 14.2307(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.392(1) _cell_angle_gamma 90.00 _cell_volume 1774.23(7) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 4255 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.48 _exptl_crystal_description 'cut from large tablet' _exptl_crystal_colour colourless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.073 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 632 _exptl_absorpt_coefficient_mu 0.095 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details scalepacked _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method 'phi and omega scans to fill Ewald sphere' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 7848 _diffrn_reflns_av_R_equivalents 0.0198 _diffrn_reflns_av_sigmaI/netI 0.0286 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.23 _diffrn_reflns_theta_max 27.43 _reflns_number_total 4036 _reflns_number_gt 3037 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution shelxs _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material shelxl-97 _refine_special_details ; The Butyl groups are modeled as disordered. The disordered C atoms were treated isotropically. Their occupancies were refined so as to total 1. 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^)+(0.0696P)^2^+0.7105P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4036 _refine_ls_number_parameters 187 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0706 _refine_ls_R_factor_gt 0.0498 _refine_ls_wR_factor_ref 0.1464 _refine_ls_wR_factor_gt 0.1329 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.034 _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 -0.04949(5) 0.12413(6) 0.02300(4) 0.03731(18) Uani 1 1 d . . . O1 O 0.09624(9) 0.03818(11) 0.03626(7) 0.0327(3) Uani 1 1 d . . . C1 C 0.20350(13) 0.05312(16) 0.07184(11) 0.0338(4) Uani 1 1 d . . . C2 C 0.22860(13) 0.00548(16) 0.16300(12) 0.0358(4) Uani 1 1 d . B . C3 C 0.34050(15) 0.01095(19) 0.19292(13) 0.0438(4) Uani 1 1 d . . . H3 H 0.3596 -0.0206 0.2536 0.053 Uiso 1 1 calc R B . C4 C 0.42308(15) 0.0604(2) 0.13736(15) 0.0498(5) Uani 1 1 d . B . H4 H 0.4985 0.0600 0.1588 0.060 Uiso 1 1 calc R . . C5 C 0.39672(15) 0.11064(19) 0.05031(14) 0.0461(5) Uani 1 1 d . . . H5 H 0.4545 0.1463 0.0130 0.055 Uiso 1 1 calc R B . C6 C 0.28709(14) 0.11035(17) 0.01569(12) 0.0380(4) Uani 1 1 d . B . C7 C 0.13953(15) -0.04887(18) 0.22938(12) 0.0404(4) Uani 1 1 d . . . C8 C 0.07693(17) -0.1633(2) 0.18569(14) 0.0476(5) Uani 1 1 d . B . H8A H 0.0229 -0.1321 0.1389 0.071 Uiso 1 1 calc R . . H8B H 0.0374 -0.2102 0.2350 0.071 Uiso 1 1 calc R . . H8C H 0.1307 -0.2206 0.1553 0.071 Uiso 1 1 calc R . . C9 C 0.05641(16) 0.0568(2) 0.25709(13) 0.0478(5) Uani 1 1 d . B . H9A H 0.0961 0.1243 0.2917 0.072 Uiso 1 1 calc R . . H9B H -0.0020 0.0202 0.2969 0.072 Uiso 1 1 calc R . . H9C H 0.0222 0.0933 0.2003 0.072 Uiso 1 1 calc R . . C10 C 0.19080(18) -0.1001(2) 0.32227(14) 0.0539(5) Uani 1 1 d . B . H10A H 0.2428 -0.1702 0.3084 0.081 Uiso 1 1 calc R . . H10B H 0.1309 -0.1318 0.3629 0.081 Uiso 1 1 calc R . . H10C H 0.2311 -0.0308 0.3543 0.081 Uiso 1 1 calc R . . C11 C 0.26260(15) 0.17254(19) -0.08023(13) 0.0437(4) Uani 1 1 d . . . C12 C 0.36760(18) 0.2366(2) -0.12199(16) 0.0595(6) Uani 1 1 d . B . H12A H 0.4256 0.1717 -0.1318 0.089 Uiso 1 1 calc R . . H12B H 0.3956 0.3022 -0.0785 0.089 Uiso 1 1 calc R . . H12C H 0.3482 0.2766 -0.1822 0.089 Uiso 1 1 calc R . . C13 C 0.17659(17) 0.28152(19) -0.06939(14) 0.0488(5) Uani 1 1 d . B . H13A H 0.2088 0.3498 -0.0304 0.073 Uiso 1 1 calc R . . H13B H 0.1090 0.2481 -0.0394 0.073 Uiso 1 1 calc R . . H13C H 0.1572 0.3159 -0.1315 0.073 Uiso 1 1 calc R . . C14 C 0.22409(17) 0.0720(2) -0.15265(13) 0.0488(5) Uani 1 1 d . B . H14A H 0.2138 0.1131 -0.2140 0.073 Uiso 1 1 calc R . . H14B H 0.1531 0.0342 -0.1325 0.073 Uiso 1 1 calc R . . H14C H 0.2809 0.0046 -0.1576 0.073 Uiso 1 1 calc R . . C15 C -0.03492(17) 0.3790(2) 0.12591(16) 0.0536(5) Uani 1 1 d . A 2 H15A H 0.0041 0.4114 0.0704 0.080 Uiso 1 1 d R A 2 H15B H 0.0188 0.3364 0.1678 0.080 Uiso 1 1 d R A 2 H15C H -0.0700 0.4506 0.1591 0.080 Uiso 1 1 d R A 2 C16A C -0.1062(4) 0.3119(6) 0.0580(4) 0.0488(14) Uiso 0.431(7) 1 d P B 1 H16A H -0.1020 0.3629 -0.0014 0.059 Uiso 0.431(7) 1 d PR B 1 C17A C -0.2251(4) 0.3234(5) 0.0908(5) 0.0509(15) Uiso 0.431(7) 1 d P B 1 H17A H -0.2405 0.4149 0.1040 0.061 Uiso 0.431(7) 1 d PR B 1 H17B H -0.2320 0.2763 0.1509 0.061 Uiso 0.431(7) 1 d PR B 1 C16B C -0.1279(3) 0.2794(3) 0.0936(3) 0.0379(9) Uiso 0.569(7) 1 d P A 2 H16B H -0.1613 0.2433 0.1521 0.045 Uiso 0.569(7) 1 calc PR B 2 C17B C -0.2226(3) 0.3500(4) 0.0413(3) 0.0450(11) Uiso 0.569(7) 1 d P A 2 H17C H -0.2464 0.4240 0.0798 0.054 Uiso 0.569(7) 1 calc PR B 2 H17D H -0.1928 0.3841 -0.0184 0.054 Uiso 0.569(7) 1 calc PR B 2 C18 C -0.31926(18) 0.2723(2) 0.02050(19) 0.0661(6) Uani 1 1 d . A 2 H18A H -0.2992 0.2062 -0.0253 0.099 Uiso 1 1 calc R A 2 H18B H -0.3788 0.3264 -0.0056 0.099 Uiso 1 1 calc R A 2 H18C H -0.3455 0.2314 0.0783 0.099 Uiso 1 1 calc R A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mg1 0.0349(3) 0.0347(3) 0.0423(3) -0.0067(2) -0.0092(2) 0.0071(2) O1 0.0295(5) 0.0350(6) 0.0334(6) -0.0018(5) -0.0079(4) 0.0021(5) C1 0.0306(8) 0.0328(9) 0.0381(8) -0.0069(7) -0.0078(6) 0.0045(6) C2 0.0361(8) 0.0338(9) 0.0375(9) -0.0053(7) -0.0087(7) 0.0070(7) C3 0.0394(9) 0.0458(10) 0.0459(10) -0.0035(8) -0.0145(8) 0.0090(8) C4 0.0324(9) 0.0570(12) 0.0598(12) -0.0067(10) -0.0143(8) 0.0064(8) C5 0.0332(9) 0.0505(11) 0.0546(11) -0.0078(9) -0.0016(8) -0.0007(8) C6 0.0354(9) 0.0385(9) 0.0399(9) -0.0063(7) -0.0030(7) 0.0012(7) C7 0.0431(9) 0.0436(10) 0.0342(8) 0.0009(7) -0.0096(7) 0.0047(8) C8 0.0484(11) 0.0480(11) 0.0464(10) 0.0052(8) -0.0090(8) -0.0038(9) C9 0.0505(11) 0.0573(12) 0.0355(9) -0.0042(8) -0.0028(8) 0.0082(9) C10 0.0600(12) 0.0599(13) 0.0417(10) 0.0089(9) -0.0178(9) 0.0006(10) C11 0.0427(10) 0.0483(11) 0.0401(9) -0.0004(8) -0.0021(8) -0.0067(8) C12 0.0542(12) 0.0727(15) 0.0517(12) 0.0017(11) 0.0022(9) -0.0194(11) C13 0.0552(11) 0.0423(10) 0.0489(11) 0.0068(8) -0.0085(9) -0.0037(9) C14 0.0484(11) 0.0591(12) 0.0387(10) -0.0036(9) -0.0028(8) -0.0060(9) C15 0.0504(11) 0.0503(12) 0.0600(12) -0.0111(10) -0.0113(9) 0.0037(9) C18 0.0518(12) 0.0673(15) 0.0789(16) -0.0070(12) -0.0193(11) 0.0071(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mg1 O1 1.9668(12) . ? Mg1 O1 1.9708(12) 3 ? Mg1 C16B 2.126(3) . ? Mg1 C16A 2.133(5) . ? Mg1 Mg1 2.9235(11) 3 ? O1 C1 1.3839(18) . ? O1 Mg1 1.9708(12) 3 ? C1 C6 1.416(2) . ? C1 C2 1.419(2) . ? C2 C3 1.402(2) . ? C2 C7 1.536(3) . ? C3 C4 1.369(3) . ? C3 H3 0.9500 . ? C4 C5 1.380(3) . ? C4 H4 0.9500 . ? C5 C6 1.397(2) . ? C5 H5 0.9500 . ? C6 C11 1.538(3) . ? C7 C9 1.537(3) . ? C7 C8 1.538(3) . ? C7 C10 1.548(2) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C14 1.539(3) . ? C11 C13 1.541(3) . ? C11 C12 1.544(3) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? 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 C16B 1.587(4) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16A C17A 1.505(8) . ? C16A H16A 1.0000 . ? C17A H17A 0.9900 . ? C17A H17B 0.9900 . ? C16B C17B 1.538(5) . ? C16B H17B 1.4932 . ? C16B H16B 1.0000 . ? C17B C18 1.440(4) . ? C17B H16A 1.5738 . ? C17B H17A 1.1421 . ? C17B H17C 0.9900 . ? C17B H17D 0.9900 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Mg1 O1 84.12(5) . 3 ? O1 Mg1 C16B 133.99(9) . . ? O1 Mg1 C16B 137.05(10) 3 . ? O1 Mg1 C16A 132.74(14) . . ? O1 Mg1 C16A 143.10(13) 3 . ? C16B Mg1 C16A 17.91(14) . . ? O1 Mg1 Mg1 42.11(3) . 3 ? O1 Mg1 Mg1 42.01(3) 3 3 ? C16B Mg1 Mg1 163.89(13) . 3 ? C16A Mg1 Mg1 174.64(15) . 3 ? C1 O1 Mg1 143.25(10) . . ? C1 O1 Mg1 120.83(10) . 3 ? Mg1 O1 Mg1 95.88(5) . 3 ? O1 C1 C6 119.77(14) . . ? O1 C1 C2 118.97(15) . . ? C6 C1 C2 121.20(14) . . ? C3 C2 C1 117.29(16) . . ? C3 C2 C7 119.46(15) . . ? C1 C2 C7 123.24(14) . . ? C4 C3 C2 121.98(17) . . ? C4 C3 H3 119.0 . . ? C2 C3 H3 119.0 . . ? C3 C4 C5 120.04(16) . . ? C3 C4 H4 120.0 . . ? C5 C4 H4 120.0 . . ? C4 C5 C6 121.58(18) . . ? C4 C5 H5 119.2 . . ? C6 C5 H5 119.2 . . ? C5 C6 C1 117.76(16) . . ? C5 C6 C11 118.99(16) . . ? C1 C6 C11 123.25(15) . . ? C2 C7 C9 110.16(15) . . ? C2 C7 C8 112.02(15) . . ? C9 C7 C8 110.30(15) . . ? C2 C7 C10 112.37(15) . . ? C9 C7 C10 106.34(15) . . ? C8 C7 C10 105.41(15) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C6 C11 C14 111.16(16) . . ? C6 C11 C13 110.21(15) . . ? C14 C11 C13 111.92(16) . . ? C6 C11 C12 111.96(15) . . ? C14 C11 C12 106.11(16) . . ? C13 C11 C12 105.28(17) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C11 C14 H14A 109.5 . . ? C11 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C11 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C16B C15 H15A 109.2 . . ? C16B C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C16B C15 H15C 109.8 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C17A C16A Mg1 116.6(4) . . ? C17A C16A H16A 105.9 . . ? Mg1 C16A H16A 105.8 . . ? C16A C17A H17A 108.2 . . ? C16A C17A H17B 108.2 . . ? H17A C17A H17B 107.4 . . ? C17B C16B C15 109.8(3) . . ? C17B C16B Mg1 117.5(3) . . ? C15 C16B Mg1 109.03(19) . . ? C17B C16B H16B 106.7 . . ? C15 C16B H16B 106.7 . . ? Mg1 C16B H16B 106.7 . . ? C18 C17B C16B 114.6(3) . . ? C18 C17B H17A 109.9 . . ? C18 C17B H17C 108.6 . . ? C16B C17B H17C 108.6 . . ? C18 C17B H17D 108.6 . . ? C16B C17B H17D 108.6 . . ? H17C C17B H17D 107.6 . . ? C17B C18 H18A 109.5 . . ? C17B C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17B C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Mg1 O1 C1 -177.2(2) 3 . . . ? C16B Mg1 O1 C1 -19.8(3) . . . . ? C16A Mg1 O1 C1 4.9(3) . . . . ? Mg1 Mg1 O1 C1 -177.2(2) 3 . . . ? O1 Mg1 O1 Mg1 0.0 3 . . 3 ? C16B Mg1 O1 Mg1 157.43(18) . . . 3 ? C16A Mg1 O1 Mg1 -177.9(3) . . . 3 ? Mg1 O1 C1 C6 -88.2(2) . . . . ? Mg1 O1 C1 C6 95.04(16) 3 . . . ? Mg1 O1 C1 C2 94.5(2) . . . . ? Mg1 O1 C1 C2 -82.31(16) 3 . . . ? O1 C1 C2 C3 173.85(14) . . . . ? C6 C1 C2 C3 -3.5(2) . . . . ? O1 C1 C2 C7 -7.1(2) . . . . ? C6 C1 C2 C7 175.60(15) . . . . ? C1 C2 C3 C4 0.2(3) . . . . ? C7 C2 C3 C4 -178.90(17) . . . . ? C2 C3 C4 C5 2.2(3) . . . . ? C3 C4 C5 C6 -1.4(3) . . . . ? C4 C5 C6 C1 -1.8(3) . . . . ? C4 C5 C6 C11 177.67(18) . . . . ? O1 C1 C6 C5 -173.05(15) . . . . ? C2 C1 C6 C5 4.2(3) . . . . ? O1 C1 C6 C11 7.5(2) . . . . ? C2 C1 C6 C11 -175.21(16) . . . . ? C3 C2 C7 C9 114.59(17) . . . . ? C1 C2 C7 C9 -64.5(2) . . . . ? C3 C2 C7 C8 -122.23(18) . . . . ? C1 C2 C7 C8 58.7(2) . . . . ? C3 C2 C7 C10 -3.8(2) . . . . ? C1 C2 C7 C10 177.18(16) . . . . ? C5 C6 C11 C14 114.50(19) . . . . ? C1 C6 C11 C14 -66.1(2) . . . . ? C5 C6 C11 C13 -120.81(18) . . . . ? C1 C6 C11 C13 58.6(2) . . . . ? C5 C6 C11 C12 -4.0(3) . . . . ? C1 C6 C11 C12 175.46(17) . . . . ? O1 Mg1 C16A C17A -145.4(4) . . . . ? O1 Mg1 C16A C17A 38.1(7) 3 . . . ? C16B Mg1 C16A C17A -42.9(6) . . . . ? Mg1 Mg1 C16A C17A -160.7(16) 3 . . . ? O1 Mg1 C16B C17B 158.2(2) . . . . ? O1 Mg1 C16B C17B -55.9(4) 3 . . . ? C16A Mg1 C16B C17B 63.6(6) . . . . ? Mg1 Mg1 C16B C17B -133.7(3) 3 . . . ? O1 Mg1 C16B C15 32.5(3) . . . . ? O1 Mg1 C16B C15 178.47(13) 3 . . . ? C16A Mg1 C16B C15 -62.0(5) . . . . ? Mg1 Mg1 C16B C15 100.6(4) 3 . . . ? C15 C16B C17B C18 -171.4(3) . . . . ? Mg1 C16B C17B C18 63.3(5) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.43 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.462 _refine_diff_density_min -0.291 _refine_diff_density_rms 0.041 #===END data_hend13 _database_code_CSD 200472 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C47 H78 Mg2 N2 O2' _chemical_formula_weight 751.73 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Mg Mg 0.0486 0.0363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M P212121 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 12.88850(10) _cell_length_b 15.4780(2) _cell_length_c 22.8343(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4555.17(9) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 5742 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description 'plate like fragment from big prism' _exptl_crystal_colour colourless _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.096 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1656 _exptl_absorpt_coefficient_mu 0.090 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details 'usual scalepack treatment' _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method 'phi and omega scans to fill Ewald sphere' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 52199 _diffrn_reflns_av_R_equivalents 0.046 _diffrn_reflns_av_sigmaI/netI 0.0378 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 2.98 _diffrn_reflns_theta_max 27.49 _reflns_number_total 10408 _reflns_number_gt 8815 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution SHELXS _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0276P)^2^+1.1826P] 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 calc _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.06(13) _refine_ls_number_reflns 10408 _refine_ls_number_parameters 499 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0548 _refine_ls_R_factor_gt 0.0388 _refine_ls_wR_factor_ref 0.0809 _refine_ls_wR_factor_gt 0.0747 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.046 _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 0.37479(4) 0.07497(3) 0.24922(2) 0.02139(11) Uani 1 1 d . . . Mg2 Mg 0.18865(4) 0.10895(3) 0.18529(2) 0.02245(11) Uani 1 1 d . . . O1 O 0.47767(8) 0.03477(7) 0.29721(4) 0.0226(2) Uani 1 1 d . . . O2 O 0.06664(8) 0.10868(7) 0.14496(5) 0.0247(2) Uani 1 1 d . . . N1 N 0.24354(10) 0.15307(8) 0.26597(6) 0.0222(3) Uani 1 1 d . . . N2 N 0.32650(10) 0.04657(8) 0.16410(5) 0.0227(3) Uani 1 1 d . . . C1 C 0.14809(15) 0.02758(11) 0.30336(8) 0.0354(4) Uani 1 1 d . . . H1A H 0.1121 0.0204 0.2659 0.053 Uiso 1 1 calc R . . H1B H 0.1038 0.0063 0.3351 0.053 Uiso 1 1 calc R . . H1C H 0.2131 -0.0053 0.3028 0.053 Uiso 1 1 calc R . . C2 C 0.17172(12) 0.12237(10) 0.31309(7) 0.0262(3) Uani 1 1 d . . . H2 H 0.2083 0.1282 0.3515 0.031 Uiso 1 1 calc R . . C3 C 0.06995(14) 0.17249(13) 0.31676(9) 0.0392(4) Uani 1 1 d . . . H3A H 0.0848 0.2338 0.3235 0.059 Uiso 1 1 calc R . . H3B H 0.0281 0.1499 0.3492 0.059 Uiso 1 1 calc R . . H3C H 0.0317 0.1660 0.2799 0.059 Uiso 1 1 calc R . . C4 C 0.33660(14) 0.27829(11) 0.22407(8) 0.0323(4) Uani 1 1 d . . . H4A H 0.3989 0.2429 0.2186 0.048 Uiso 1 1 calc R . . H4B H 0.3569 0.3384 0.2312 0.048 Uiso 1 1 calc R . . H4C H 0.2935 0.2752 0.1888 0.048 Uiso 1 1 calc R . . C5 C 0.27541(12) 0.24468(10) 0.27618(7) 0.0258(4) Uani 1 1 d . . . H5 H 0.2110 0.2803 0.2798 0.031 Uiso 1 1 calc R . . C6 C 0.33813(14) 0.25600(12) 0.33249(8) 0.0335(4) Uani 1 1 d . . . H6A H 0.2956 0.2390 0.3662 0.050 Uiso 1 1 calc R . . H6B H 0.3587 0.3167 0.3366 0.050 Uiso 1 1 calc R . . H6C H 0.4003 0.2196 0.3308 0.050 Uiso 1 1 calc R . . C7 C 0.25150(13) -0.09686(11) 0.18430(8) 0.0338(4) Uani 1 1 d . . . H7A H 0.2733 -0.0959 0.2254 0.051 Uiso 1 1 calc R . . H7B H 0.2486 -0.1568 0.1705 0.051 Uiso 1 1 calc R . . H7C H 0.1827 -0.0704 0.1807 0.051 Uiso 1 1 calc R . . C8 C 0.32890(13) -0.04641(10) 0.14752(7) 0.0258(3) Uani 1 1 d . . . H8 H 0.3068 -0.0510 0.1056 0.031 Uiso 1 1 calc R . . C9 C 0.43505(13) -0.08909(11) 0.15314(9) 0.0335(4) Uani 1 1 d . . . H9A H 0.4847 -0.0595 0.1276 0.050 Uiso 1 1 calc R . . H9B H 0.4299 -0.1499 0.1416 0.050 Uiso 1 1 calc R . . H9C H 0.4588 -0.0852 0.1938 0.050 Uiso 1 1 calc R . . C10 C 0.31604(15) 0.08790(12) 0.05611(7) 0.0330(4) Uani 1 1 d . . . H10A H 0.3503 0.0374 0.0389 0.050 Uiso 1 1 calc R . . H10B H 0.3263 0.1381 0.0306 0.050 Uiso 1 1 calc R . . H10C H 0.2416 0.0763 0.0602 0.050 Uiso 1 1 calc R . . C11 C 0.36263(13) 0.10642(11) 0.11640(7) 0.0270(3) Uani 1 1 d . . . H11 H 0.3353 0.1646 0.1276 0.032 Uiso 1 1 calc R . . C12 C 0.48037(14) 0.11834(13) 0.11100(9) 0.0414(5) Uani 1 1 d . . . H12A H 0.5097 0.1310 0.1496 0.062 Uiso 1 1 calc R . . H12B H 0.4951 0.1664 0.0843 0.062 Uiso 1 1 calc R . . H12C H 0.5115 0.0652 0.0956 0.062 Uiso 1 1 calc R . . C13 C 0.55377(11) 0.01649(9) 0.33533(7) 0.0205(3) Uani 1 1 d . . . C14 C 0.53250(12) -0.03453(10) 0.38623(7) 0.0211(3) Uani 1 1 d . . . C15 C 0.61239(13) -0.04905(10) 0.42618(7) 0.0268(4) Uani 1 1 d . . . H15 H 0.5985 -0.0820 0.4604 0.032 Uiso 1 1 calc R . . C16 C 0.71116(13) -0.01693(11) 0.41744(7) 0.0295(4) Uani 1 1 d . . . H16 H 0.7639 -0.0266 0.4458 0.035 Uiso 1 1 calc R . . C17 C 0.73263(12) 0.02946(10) 0.36706(7) 0.0275(4) Uani 1 1 d . . . H17 H 0.8012 0.0499 0.3608 0.033 Uiso 1 1 calc R . . C18 C 0.65684(12) 0.04700(10) 0.32537(7) 0.0225(3) Uani 1 1 d . . . C19 C 0.42430(12) -0.07198(10) 0.39830(7) 0.0234(3) Uani 1 1 d . . . C20 C 0.39005(13) -0.13010(11) 0.34704(7) 0.0283(4) Uani 1 1 d . . . H20A H 0.3921 -0.0969 0.3105 0.042 Uiso 1 1 calc R . . H20B H 0.3192 -0.1507 0.3540 0.042 Uiso 1 1 calc R . . H20C H 0.4371 -0.1797 0.3440 0.042 Uiso 1 1 calc R . . C21 C 0.34716(13) 0.00185(11) 0.40917(7) 0.0284(4) Uani 1 1 d . . . H21A H 0.3665 0.0327 0.4450 0.043 Uiso 1 1 calc R . . H21B H 0.2771 -0.0219 0.4135 0.043 Uiso 1 1 calc R . . H21C H 0.3487 0.0419 0.3760 0.043 Uiso 1 1 calc R . . C22 C 0.42153(14) -0.12967(11) 0.45321(7) 0.0288(4) Uani 1 1 d . . . H22A H 0.4718 -0.1768 0.4488 0.043 Uiso 1 1 calc R . . H22B H 0.3518 -0.1538 0.4580 0.043 Uiso 1 1 calc R . . H22C H 0.4393 -0.0951 0.4877 0.043 Uiso 1 1 calc R . . C23 C 0.68612(12) 0.09626(10) 0.26916(7) 0.0260(3) Uani 1 1 d . . . C24 C 0.62358(14) 0.18057(11) 0.26361(8) 0.0341(4) Uani 1 1 d . . . H24A H 0.5493 0.1672 0.2630 0.051 Uiso 1 1 calc R . . H24B H 0.6427 0.2101 0.2272 0.051 Uiso 1 1 calc R . . H24C H 0.6389 0.2181 0.2970 0.051 Uiso 1 1 calc R . . C25 C 0.66877(13) 0.03716(12) 0.21601(7) 0.0318(4) Uani 1 1 d . . . H25A H 0.7136 -0.0138 0.2193 0.048 Uiso 1 1 calc R . . H25B H 0.6857 0.0687 0.1800 0.048 Uiso 1 1 calc R . . H25C H 0.5960 0.0189 0.2148 0.048 Uiso 1 1 calc R . . C26 C 0.80107(13) 0.12302(12) 0.26783(8) 0.0363(4) Uani 1 1 d . . . H26A H 0.8156 0.1618 0.3007 0.054 Uiso 1 1 calc R . . H26B H 0.8161 0.1528 0.2309 0.054 Uiso 1 1 calc R . . H26C H 0.8448 0.0714 0.2710 0.054 Uiso 1 1 calc R . . C27 C -0.02231(12) 0.12706(10) 0.11751(7) 0.0215(3) Uani 1 1 d . . . C28 C -0.04743(12) 0.21428(10) 0.10266(7) 0.0242(3) Uani 1 1 d . . . C29 C -0.14443(13) 0.23066(11) 0.07803(7) 0.0300(4) Uani 1 1 d . . . H29 H -0.1627 0.2885 0.0688 0.036 Uiso 1 1 calc R . . C30 C -0.21483(14) 0.16545(12) 0.06665(8) 0.0323(4) Uani 1 1 d . . . H30 H -0.2815 0.1788 0.0514 0.039 Uiso 1 1 calc R . . C31 C -0.18746(13) 0.08086(11) 0.07760(7) 0.0283(4) Uani 1 1 d . . . H31 H -0.2351 0.0361 0.0682 0.034 Uiso 1 1 calc R . . C32 C -0.09184(12) 0.05898(10) 0.10213(7) 0.0231(3) Uani 1 1 d . . . C33 C 0.02911(13) 0.28915(10) 0.11290(7) 0.0265(4) Uani 1 1 d . . . C34 C 0.13361(14) 0.27132(11) 0.08281(8) 0.0312(4) Uani 1 1 d . . . H34A H 0.1828 0.3173 0.0927 0.047 Uiso 1 1 calc R . . H34B H 0.1237 0.2696 0.0403 0.047 Uiso 1 1 calc R . . H34C H 0.1610 0.2157 0.0962 0.047 Uiso 1 1 calc R . . C35 C 0.04433(15) 0.30543(12) 0.17881(8) 0.0349(4) Uani 1 1 d . . . H35A H 0.0933 0.3531 0.1844 0.052 Uiso 1 1 calc R . . H35B H 0.0718 0.2531 0.1974 0.052 Uiso 1 1 calc R . . H35C H -0.0224 0.3204 0.1966 0.052 Uiso 1 1 calc R . . C36 C -0.00961(15) 0.37473(11) 0.08662(8) 0.0375(4) Uani 1 1 d . . . H36A H -0.0759 0.3905 0.1047 0.056 Uiso 1 1 calc R . . H36B H -0.0192 0.3679 0.0443 0.056 Uiso 1 1 calc R . . H36C H 0.0415 0.4203 0.0941 0.056 Uiso 1 1 calc R . . C37 C -0.06321(12) -0.03691(10) 0.11111(7) 0.0247(3) Uani 1 1 d . . . C38 C -0.14777(14) -0.09803(12) 0.08819(8) 0.0352(4) Uani 1 1 d . . . H38A H -0.2122 -0.0882 0.1099 0.053 Uiso 1 1 calc R . . H38B H -0.1254 -0.1580 0.0935 0.053 Uiso 1 1 calc R . . H38C H -0.1596 -0.0869 0.0465 0.053 Uiso 1 1 calc R . . C39 C 0.03601(13) -0.05828(11) 0.07638(8) 0.0301(4) Uani 1 1 d . . . H39A H 0.0561 -0.1183 0.0839 0.045 Uiso 1 1 calc R . . H39B H 0.0921 -0.0197 0.0888 0.045 Uiso 1 1 calc R . . H39C H 0.0229 -0.0504 0.0344 0.045 Uiso 1 1 calc R . . C40 C -0.04875(13) -0.05712(11) 0.17655(7) 0.0278(4) Uani 1 1 d . . . H40A H -0.1160 -0.0537 0.1965 0.042 Uiso 1 1 calc R . . H40B H -0.0008 -0.0151 0.1939 0.042 Uiso 1 1 calc R . . H40C H -0.0202 -0.1155 0.1810 0.042 Uiso 1 1 calc R . . C41 C -0.0612(2) 0.1098(2) 0.47830(13) 0.0838(9) Uani 1 1 d . . . H41A H -0.0338 0.0522 0.4695 0.126 Uiso 1 1 calc R . . H41B H -0.0898 0.1355 0.4425 0.126 Uiso 1 1 calc R . . H41C H -0.1160 0.1051 0.5079 0.126 Uiso 1 1 calc R . . C42 C 0.02487(16) 0.16623(13) 0.50133(8) 0.0397(5) Uani 1 1 d . . . C43 C 0.12763(17) 0.14505(12) 0.49257(9) 0.0422(5) Uani 1 1 d . . . H43 H 0.1447 0.0955 0.4699 0.051 Uiso 1 1 calc R . . C44 C 0.20527(18) 0.19428(16) 0.51596(10) 0.0563(6) Uani 1 1 d . . . H44 H 0.2756 0.1781 0.5099 0.068 Uiso 1 1 calc R . . C45 C 0.1828(2) 0.26680(17) 0.54805(11) 0.0650(7) Uani 1 1 d . . . H45 H 0.2372 0.3001 0.5648 0.078 Uiso 1 1 calc R . . C46 C 0.0815(3) 0.29091(14) 0.55584(9) 0.0598(7) Uani 1 1 d . . . H46 H 0.0655 0.3418 0.5772 0.072 Uiso 1 1 calc R . . C47 C 0.00295(18) 0.24118(14) 0.53263(9) 0.0478(5) Uani 1 1 d . . . H47 H -0.0672 0.2583 0.5381 0.057 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 0.0201(2) 0.0235(3) 0.0205(2) -0.0004(2) -0.0031(2) 0.0029(2) Mg2 0.0204(3) 0.0248(3) 0.0222(3) -0.0002(2) -0.0037(2) 0.0026(2) O1 0.0188(5) 0.0282(6) 0.0207(5) 0.0024(4) -0.0027(5) 0.0012(5) O2 0.0219(6) 0.0241(6) 0.0281(6) 0.0003(5) -0.0068(5) 0.0010(5) N1 0.0210(7) 0.0231(7) 0.0223(7) -0.0011(5) -0.0019(6) 0.0009(5) N2 0.0237(7) 0.0234(7) 0.0211(6) -0.0008(5) -0.0020(6) 0.0030(5) C1 0.0402(10) 0.0360(10) 0.0300(9) 0.0062(8) -0.0029(8) -0.0085(8) C2 0.0249(8) 0.0320(9) 0.0217(8) 0.0020(7) -0.0015(7) 0.0005(7) C3 0.0255(9) 0.0476(11) 0.0444(11) 0.0115(9) 0.0085(9) 0.0046(8) C4 0.0326(10) 0.0259(9) 0.0383(10) -0.0031(7) 0.0030(8) -0.0021(7) C5 0.0221(8) 0.0228(8) 0.0325(9) -0.0067(7) -0.0008(7) 0.0023(6) C6 0.0292(9) 0.0348(10) 0.0364(10) -0.0109(8) -0.0018(8) -0.0020(7) C7 0.0285(9) 0.0286(9) 0.0442(10) 0.0019(8) -0.0028(8) 0.0008(7) C8 0.0302(9) 0.0251(8) 0.0221(8) -0.0017(6) -0.0034(7) 0.0017(7) C9 0.0302(9) 0.0257(9) 0.0445(11) -0.0056(8) 0.0042(8) 0.0035(7) C10 0.0377(10) 0.0387(10) 0.0227(8) 0.0031(7) 0.0004(8) 0.0007(8) C11 0.0289(9) 0.0265(8) 0.0256(8) 0.0015(7) -0.0013(7) 0.0039(7) C12 0.0335(10) 0.0468(11) 0.0440(11) 0.0121(9) -0.0011(9) -0.0050(9) C13 0.0220(8) 0.0184(7) 0.0212(8) -0.0040(6) -0.0019(6) 0.0033(6) C14 0.0223(8) 0.0195(7) 0.0215(8) -0.0044(6) -0.0014(7) 0.0039(6) C15 0.0305(9) 0.0265(8) 0.0234(8) 0.0013(7) -0.0036(7) 0.0043(7) C16 0.0247(9) 0.0342(9) 0.0298(9) 0.0002(7) -0.0107(7) 0.0044(7) C17 0.0186(8) 0.0300(9) 0.0340(10) -0.0025(7) -0.0032(7) 0.0021(7) C18 0.0231(8) 0.0204(7) 0.0240(8) -0.0037(6) 0.0001(7) 0.0023(6) C19 0.0249(8) 0.0248(8) 0.0206(8) 0.0009(6) -0.0002(7) -0.0006(7) C20 0.0305(9) 0.0300(9) 0.0245(8) -0.0014(7) -0.0008(7) -0.0053(7) C21 0.0261(9) 0.0337(9) 0.0255(9) 0.0004(7) 0.0008(7) 0.0019(7) C22 0.0331(9) 0.0303(9) 0.0231(8) 0.0019(7) -0.0004(7) -0.0017(8) C23 0.0213(8) 0.0287(8) 0.0280(8) 0.0020(6) 0.0003(7) -0.0014(7) C24 0.0333(10) 0.0277(9) 0.0412(11) 0.0075(7) 0.0010(9) -0.0035(8) C25 0.0251(9) 0.0436(10) 0.0266(9) -0.0026(8) 0.0053(7) -0.0031(8) C26 0.0266(9) 0.0438(10) 0.0383(10) 0.0024(8) 0.0019(8) -0.0086(8) C27 0.0189(7) 0.0295(8) 0.0162(7) 0.0000(6) 0.0002(6) 0.0023(6) C28 0.0269(9) 0.0291(9) 0.0166(8) -0.0008(6) 0.0017(7) 0.0056(7) C29 0.0304(10) 0.0352(9) 0.0244(8) 0.0049(7) 0.0026(7) 0.0091(7) C30 0.0221(9) 0.0473(11) 0.0274(9) 0.0052(8) -0.0036(7) 0.0044(8) C31 0.0241(8) 0.0418(10) 0.0189(8) 0.0010(7) -0.0001(7) -0.0045(8) C32 0.0221(8) 0.0313(9) 0.0158(7) -0.0012(6) 0.0026(6) 0.0006(6) C33 0.0320(9) 0.0225(8) 0.0250(8) -0.0014(7) -0.0013(7) 0.0044(7) C34 0.0344(10) 0.0261(8) 0.0330(9) 0.0018(7) 0.0003(8) -0.0029(7) C35 0.0462(11) 0.0318(9) 0.0268(9) -0.0040(7) -0.0050(9) 0.0037(8) C36 0.0471(11) 0.0258(9) 0.0396(10) 0.0004(8) -0.0101(9) 0.0043(8) C37 0.0239(8) 0.0277(8) 0.0226(8) -0.0004(7) 0.0008(7) -0.0032(7) C38 0.0344(10) 0.0365(10) 0.0348(10) -0.0014(8) -0.0019(8) -0.0088(8) C39 0.0309(9) 0.0271(9) 0.0323(9) -0.0032(7) 0.0045(8) 0.0001(7) C40 0.0278(9) 0.0275(8) 0.0281(9) 0.0027(7) 0.0011(7) -0.0019(7) C41 0.0672(18) 0.115(2) 0.0695(18) -0.0248(17) -0.0141(15) -0.0174(17) C42 0.0468(12) 0.0456(11) 0.0267(9) -0.0010(8) -0.0049(9) 0.0025(9) C43 0.0555(13) 0.0360(10) 0.0352(10) 0.0066(8) 0.0092(10) 0.0097(10) C44 0.0434(13) 0.0679(16) 0.0575(14) 0.0243(13) 0.0039(11) -0.0084(11) C45 0.083(2) 0.0589(16) 0.0531(14) 0.0162(12) -0.0119(14) -0.0351(15) C46 0.116(2) 0.0308(11) 0.0327(11) 0.0018(9) -0.0023(13) -0.0011(13) C47 0.0592(14) 0.0534(13) 0.0307(10) 0.0041(9) 0.0035(10) 0.0231(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mg1 O1 1.8292(11) . ? Mg1 N2 2.0878(14) . ? Mg1 N1 2.1139(14) . ? Mg1 Mg2 2.8572(7) . ? Mg2 O2 1.8223(11) . ? Mg2 N2 2.0791(14) . ? Mg2 N1 2.0882(14) . ? O1 C13 1.3415(18) . ? O2 C27 1.3373(18) . ? N1 C5 1.495(2) . ? N1 C2 1.497(2) . ? N2 C8 1.489(2) . ? N2 C11 1.504(2) . ? C1 C2 1.515(2) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C3 1.526(2) . ? C2 H2 1.0000 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 C5 1.519(2) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 C6 1.529(2) . ? C5 H5 1.0000 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 C8 1.520(2) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 C9 1.525(2) . ? C8 H8 1.0000 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C11 1.529(2) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.534(2) . ? C11 H11 1.0000 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C18 1.428(2) . ? C13 C14 1.432(2) . ? C14 C15 1.394(2) . ? C14 C19 1.535(2) . ? C15 C16 1.381(2) . ? C15 H15 0.9500 . ? C16 C17 1.384(2) . ? C16 H16 0.9500 . ? C17 C18 1.391(2) . ? C17 H17 0.9500 . ? C18 C23 1.540(2) . ? C19 C21 1.535(2) . ? C19 C22 1.540(2) . ? C19 C20 1.541(2) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 C25 1.536(2) . ? C23 C26 1.539(2) . ? C23 C24 1.539(2) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? 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 C32 1.427(2) . ? C27 C28 1.429(2) . ? C28 C29 1.394(2) . ? C28 C33 1.540(2) . ? C29 C30 1.382(3) . ? C29 H29 0.9500 . ? C30 C31 1.379(2) . ? C30 H30 0.9500 . ? C31 C32 1.395(2) . ? C31 H31 0.9500 . ? C32 C37 1.543(2) . ? C33 C34 1.537(2) . ? C33 C36 1.537(2) . ? C33 C35 1.538(2) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 C38 1.535(2) . ? C37 C40 1.538(2) . ? C37 C39 1.541(2) . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 C42 1.507(3) . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 C43 1.379(3) . ? C42 C47 1.392(3) . ? C43 C44 1.367(3) . ? C43 H43 0.9500 . ? C44 C45 1.371(4) . ? C44 H44 0.9500 . ? C45 C46 1.369(4) . ? C45 H45 0.9500 . ? C46 C47 1.378(3) . ? C46 H46 0.9500 . ? C47 H47 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Mg1 N2 134.61(5) . . ? O1 Mg1 N1 131.77(6) . . ? N2 Mg1 N1 92.88(5) . . ? O1 Mg1 Mg2 167.78(4) . . ? N2 Mg1 Mg2 46.58(4) . . ? N1 Mg1 Mg2 46.78(4) . . ? O2 Mg2 N2 128.23(6) . . ? O2 Mg2 N1 137.64(6) . . ? N2 Mg2 N1 93.88(5) . . ? O2 Mg2 Mg1 169.22(4) . . ? N2 Mg2 Mg1 46.84(4) . . ? N1 Mg2 Mg1 47.54(4) . . ? C13 O1 Mg1 172.05(10) . . ? C27 O2 Mg2 167.48(11) . . ? C5 N1 C2 111.04(12) . . ? C5 N1 Mg2 122.75(10) . . ? C2 N1 Mg2 108.72(9) . . ? C5 N1 Mg1 110.54(9) . . ? C2 N1 Mg1 116.32(9) . . ? Mg2 N1 Mg1 85.67(5) . . ? C8 N2 C11 113.89(12) . . ? C8 N2 Mg2 121.73(10) . . ? C11 N2 Mg2 98.46(9) . . ? C8 N2 Mg1 115.73(10) . . ? C11 N2 Mg1 116.89(10) . . ? Mg2 N2 Mg1 86.58(5) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N1 C2 C1 109.04(14) . . ? N1 C2 C3 114.17(13) . . ? C1 C2 C3 109.13(14) . . ? N1 C2 H2 108.1 . . ? C1 C2 H2 108.1 . . ? C3 C2 H2 108.1 . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C5 C4 H4A 109.5 . . ? C5 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C5 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N1 C5 C4 110.20(13) . . ? N1 C5 C6 112.66(13) . . ? C4 C5 C6 110.19(14) . . ? N1 C5 H5 107.9 . . ? C4 C5 H5 107.9 . . ? C6 C5 H5 107.9 . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C8 C7 H7A 109.5 . . ? C8 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C8 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N2 C8 C7 110.03(13) . . ? N2 C8 C9 114.59(13) . . ? C7 C8 C9 108.66(13) . . ? N2 C8 H8 107.8 . . ? C7 C8 H8 107.8 . . ? C9 C8 H8 107.8 . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C11 C10 H10A 109.5 . . ? C11 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C11 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N2 C11 C10 114.52(13) . . ? N2 C11 C12 116.03(13) . . ? C10 C11 C12 109.80(15) . . ? N2 C11 H11 105.1 . . ? C10 C11 H11 105.1 . . ? C12 C11 H11 105.1 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? O1 C13 C18 120.47(13) . . ? O1 C13 C14 120.20(13) . . ? C18 C13 C14 119.32(13) . . ? C15 C14 C13 118.61(14) . . ? C15 C14 C19 119.52(14) . . ? C13 C14 C19 121.87(13) . . ? C16 C15 C14 121.89(15) . . ? C16 C15 H15 119.1 . . ? C14 C15 H15 119.1 . . ? C15 C16 C17 119.41(15) . . ? C15 C16 H16 120.3 . . ? C17 C16 H16 120.3 . . ? C16 C17 C18 121.99(15) . . ? C16 C17 H17 119.0 . . ? C18 C17 H17 119.0 . . ? C17 C18 C13 118.68(14) . . ? C17 C18 C23 119.67(14) . . ? C13 C18 C23 121.63(13) . . ? C21 C19 C14 109.66(13) . . ? C21 C19 C22 106.56(13) . . ? C14 C19 C22 112.72(13) . . ? C21 C19 C20 111.84(13) . . ? C14 C19 C20 110.14(13) . . ? C22 C19 C20 105.87(13) . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C19 C22 H22A 109.5 . . ? C19 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C19 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C25 C23 C26 106.55(14) . . ? C25 C23 C24 111.32(14) . . ? C26 C23 C24 105.93(13) . . ? C25 C23 C18 109.15(13) . . ? C26 C23 C18 112.69(13) . . ? C24 C23 C18 111.11(13) . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C23 C25 H25A 109.5 . . ? C23 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C23 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C23 C26 H26A 109.5 . . ? C23 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C23 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? O2 C27 C32 119.78(14) . . ? O2 C27 C28 120.42(14) . . ? C32 C27 C28 119.80(14) . . ? C29 C28 C27 118.07(15) . . ? C29 C28 C33 119.93(15) . . ? C27 C28 C33 122.00(14) . . ? C30 C29 C28 122.13(16) . . ? C30 C29 H29 118.9 . . ? C28 C29 H29 118.9 . . ? C31 C30 C29 119.44(16) . . ? C31 C30 H30 120.3 . . ? C29 C30 H30 120.3 . . ? C30 C31 C32 121.94(16) . . ? C30 C31 H31 119.0 . . ? C32 C31 H31 119.0 . . ? C31 C32 C27 118.30(15) . . ? C31 C32 C37 119.87(14) . . ? C27 C32 C37 121.82(14) . . ? C34 C33 C36 105.34(14) . . ? C34 C33 C35 110.79(14) . . ? C36 C33 C35 106.39(14) . . ? C34 C33 C28 111.00(13) . . ? C36 C33 C28 112.41(14) . . ? C35 C33 C28 110.71(14) . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C33 C35 H35A 109.5 . . ? C33 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C33 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C33 C36 H36A 109.5 . . ? C33 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C33 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C38 C37 C40 106.97(13) . . ? C38 C37 C39 106.35(13) . . ? C40 C37 C39 110.84(13) . . ? C38 C37 C32 112.19(14) . . ? C40 C37 C32 110.72(13) . . ? C39 C37 C32 109.67(13) . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C37 C39 H39A 109.5 . . ? C37 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C37 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C37 C40 H40A 109.5 . . ? C37 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C37 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C42 C41 H41A 109.5 . . ? C42 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C42 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C43 C42 C47 117.88(19) . . ? C43 C42 C41 121.3(2) . . ? C47 C42 C41 120.9(2) . . ? C44 C43 C42 120.9(2) . . ? C44 C43 H43 119.5 . . ? C42 C43 H43 119.5 . . ? C43 C44 C45 120.7(2) . . ? C43 C44 H44 119.7 . . ? C45 C44 H44 119.7 . . ? C46 C45 C44 119.6(2) . . ? C46 C45 H45 120.2 . . ? C44 C45 H45 120.2 . . ? C45 C46 C47 119.9(2) . . ? C45 C46 H46 120.1 . . ? C47 C46 H46 120.1 . . ? C46 C47 C42 120.9(2) . . ? C46 C47 H47 119.5 . . ? C42 C47 H47 119.5 . . ? 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 O1 Mg1 Mg2 O2 -34.4(3) . . . . ? N2 Mg1 Mg2 O2 67.0(2) . . . . ? N1 Mg1 Mg2 O2 -123.3(2) . . . . ? O1 Mg1 Mg2 N2 -101.4(2) . . . . ? N1 Mg1 Mg2 N2 169.69(7) . . . . ? O1 Mg1 Mg2 N1 88.9(2) . . . . ? N2 Mg1 Mg2 N1 -169.69(7) . . . . ? N2 Mg1 O1 C13 146.5(7) . . . . ? N1 Mg1 O1 C13 -46.2(8) . . . . ? Mg2 Mg1 O1 C13 -123.8(7) . . . . ? N2 Mg2 O2 C27 -134.0(5) . . . . ? N1 Mg2 O2 C27 53.6(5) . . . . ? Mg1 Mg2 O2 C27 167.3(4) . . . . ? O2 Mg2 N1 C5 -81.73(14) . . . . ? N2 Mg2 N1 C5 104.17(12) . . . . ? Mg1 Mg2 N1 C5 111.69(12) . . . . ? O2 Mg2 N1 C2 50.23(13) . . . . ? N2 Mg2 N1 C2 -123.87(10) . . . . ? Mg1 Mg2 N1 C2 -116.35(11) . . . . ? O2 Mg2 N1 Mg1 166.58(7) . . . . ? N2 Mg2 N1 Mg1 -7.52(5) . . . . ? O1 Mg1 N1 C5 73.05(12) . . . . ? N2 Mg1 N1 C5 -115.95(10) . . . . ? Mg2 Mg1 N1 C5 -123.43(11) . . . . ? O1 Mg1 N1 C2 -54.75(13) . . . . ? N2 Mg1 N1 C2 116.24(11) . . . . ? Mg2 Mg1 N1 C2 108.76(11) . . . . ? O1 Mg1 N1 Mg2 -163.52(6) . . . . ? N2 Mg1 N1 Mg2 7.48(5) . . . . ? O2 Mg2 N2 C8 -49.01(14) . . . . ? N1 Mg2 N2 C8 125.93(11) . . . . ? Mg1 Mg2 N2 C8 118.32(12) . . . . ? O2 Mg2 N2 C11 75.98(11) . . . . ? N1 Mg2 N2 C11 -109.08(9) . . . . ? Mg1 Mg2 N2 C11 -116.69(10) . . . . ? O2 Mg2 N2 Mg1 -167.33(6) . . . . ? N1 Mg2 N2 Mg1 7.61(5) . . . . ? O1 Mg1 N2 C8 39.27(14) . . . . ? N1 Mg1 N2 C8 -131.29(11) . . . . ? Mg2 Mg1 N2 C8 -123.79(12) . . . . ? O1 Mg1 N2 C11 -99.18(12) . . . . ? N1 Mg1 N2 C11 90.25(11) . . . . ? Mg2 Mg1 N2 C11 97.76(11) . . . . ? O1 Mg1 N2 Mg2 163.06(6) . . . . ? N1 Mg1 N2 Mg2 -7.51(5) . . . . ? C5 N1 C2 C1 -175.81(13) . . . . ? Mg2 N1 C2 C1 46.26(14) . . . . ? Mg1 N1 C2 C1 -48.25(15) . . . . ? C5 N1 C2 C3 61.86(18) . . . . ? Mg2 N1 C2 C3 -76.07(15) . . . . ? Mg1 N1 C2 C3 -170.59(12) . . . . ? C2 N1 C5 C4 -172.65(13) . . . . ? Mg2 N1 C5 C4 -41.64(17) . . . . ? Mg1 N1 C5 C4 56.71(14) . . . . ? C2 N1 C5 C6 63.85(17) . . . . ? Mg2 N1 C5 C6 -165.14(11) . . . . ? Mg1 N1 C5 C6 -66.79(14) . . . . ? C11 N2 C8 C7 -155.43(13) . . . . ? Mg2 N2 C8 C7 -37.84(16) . . . . ? Mg1 N2 C8 C7 64.88(15) . . . . ? C11 N2 C8 C9 81.80(17) . . . . ? Mg2 N2 C8 C9 -160.61(11) . . . . ? Mg1 N2 C8 C9 -57.90(16) . . . . ? C8 N2 C11 C10 46.73(18) . . . . ? Mg2 N2 C11 C10 -83.62(14) . . . . ? Mg1 N2 C11 C10 -174.07(11) . . . . ? C8 N2 C11 C12 -82.83(18) . . . . ? Mg2 N2 C11 C12 146.82(13) . . . . ? Mg1 N2 C11 C12 56.37(17) . . . . ? Mg1 O1 C13 C18 -72.5(8) . . . . ? Mg1 O1 C13 C14 108.0(7) . . . . ? O1 C13 C14 C15 -177.22(13) . . . . ? C18 C13 C14 C15 3.3(2) . . . . ? O1 C13 C14 C19 1.7(2) . . . . ? C18 C13 C14 C19 -177.77(13) . . . . ? C13 C14 C15 C16 -1.1(2) . . . . ? C19 C14 C15 C16 179.94(15) . . . . ? C14 C15 C16 C17 -1.4(2) . . . . ? C15 C16 C17 C18 1.8(2) . . . . ? C16 C17 C18 C13 0.4(2) . . . . ? C16 C17 C18 C23 -177.93(15) . . . . ? O1 C13 C18 C17 177.56(14) . . . . ? C14 C13 C18 C17 -3.0(2) . . . . ? O1 C13 C18 C23 -4.1(2) . . . . ? C14 C13 C18 C23 175.34(13) . . . . ? C15 C14 C19 C21 113.51(15) . . . . ? C13 C14 C19 C21 -65.40(18) . . . . ? C15 C14 C19 C22 -5.0(2) . . . . ? C13 C14 C19 C22 176.07(14) . . . . ? C15 C14 C19 C20 -123.01(15) . . . . ? C13 C14 C19 C20 58.08(18) . . . . ? C17 C18 C23 C25 116.36(16) . . . . ? C13 C18 C23 C25 -61.93(18) . . . . ? C17 C18 C23 C26 -1.8(2) . . . . ? C13 C18 C23 C26 179.90(14) . . . . ? C17 C18 C23 C24 -120.50(16) . . . . ? C13 C18 C23 C24 61.20(19) . . . . ? Mg2 O2 C27 C32 -166.6(4) . . . . ? Mg2 O2 C27 C28 14.4(6) . . . . ? O2 C27 C28 C29 -175.31(14) . . . . ? C32 C27 C28 C29 5.7(2) . . . . ? O2 C27 C28 C33 4.9(2) . . . . ? C32 C27 C28 C33 -174.12(14) . . . . ? C27 C28 C29 C30 -1.4(2) . . . . ? C33 C28 C29 C30 178.40(15) . . . . ? C28 C29 C30 C31 -2.7(3) . . . . ? C29 C30 C31 C32 2.6(2) . . . . ? C30 C31 C32 C27 1.7(2) . . . . ? C30 C31 C32 C37 -177.46(15) . . . . ? O2 C27 C32 C31 175.16(13) . . . . ? C28 C27 C32 C31 -5.8(2) . . . . ? O2 C27 C32 C37 -5.7(2) . . . . ? C28 C27 C32 C37 173.29(14) . . . . ? C29 C28 C33 C34 -124.59(16) . . . . ? C27 C28 C33 C34 55.20(19) . . . . ? C29 C28 C33 C36 -6.9(2) . . . . ? C27 C28 C33 C36 172.90(15) . . . . ? C29 C28 C33 C35 111.93(17) . . . . ? C27 C28 C33 C35 -68.28(19) . . . . ? C31 C32 C37 C38 2.3(2) . . . . ? C27 C32 C37 C38 -176.83(14) . . . . ? C31 C32 C37 C40 -117.16(16) . . . . ? C27 C32 C37 C40 63.75(18) . . . . ? C31 C32 C37 C39 120.21(15) . . . . ? C27 C32 C37 C39 -58.88(19) . . . . ? C47 C42 C43 C44 2.6(3) . . . . ? C41 C42 C43 C44 -176.8(2) . . . . ? C42 C43 C44 C45 -1.0(3) . . . . ? C43 C44 C45 C46 -1.1(3) . . . . ? C44 C45 C46 C47 1.5(3) . . . . ? C45 C46 C47 C42 0.2(3) . . . . ? C43 C42 C47 C46 -2.2(3) . . . . ? C41 C42 C47 C46 177.2(2) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.172 _refine_diff_density_min -0.176 _refine_diff_density_rms 0.035 #===END data_h15 _database_code_CSD 200473 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H58 Mg O4' _chemical_formula_weight 579.13 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Mg Mg 0.0486 0.0363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pccn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' 'x+1/2, -y, -z+1/2' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' '-x-1/2, y, z-1/2' 'x, -y-1/2, z-1/2' _cell_length_a 20.0212(6) _cell_length_b 9.8738(2) _cell_length_c 16.6859(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3298.56(15) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 4182 _cell_measurement_theta_min 1.02 _cell_measurement_theta_max 27.48 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.7 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.166 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1272 _exptl_absorpt_coefficient_mu 0.090 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 7089 _diffrn_reflns_av_R_equivalents 0.0539 _diffrn_reflns_av_sigmaI/netI 0.0681 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.03 _diffrn_reflns_theta_max 27.48 _reflns_number_total 3769 _reflns_number_gt 2527 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution SIR-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0414P)^2^+0.4159P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3769 _refine_ls_number_parameters 192 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0832 _refine_ls_R_factor_gt 0.0437 _refine_ls_wR_factor_ref 0.1002 _refine_ls_wR_factor_gt 0.0893 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.025 _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 0.2500 0.7500 0.23246(4) 0.01848(18) Uani 1 2 d S . . O1 O 0.16980(5) 0.78221(9) 0.28589(6) 0.0193(2) Uani 1 1 d . . . O2 O 0.22004(5) 0.61719(10) 0.14407(6) 0.0220(3) Uani 1 1 d . . . C1 C 0.11553(7) 0.79072(14) 0.33251(9) 0.0185(3) Uani 1 1 d . . . C2 C 0.07434(7) 0.90884(15) 0.33053(9) 0.0192(3) Uani 1 1 d . . . C3 C 0.01911(7) 0.91483(16) 0.38124(9) 0.0239(4) Uani 1 1 d . . . H3 H -0.0081 0.9936 0.3804 0.029 Uiso 1 1 calc R . . C4 C 0.00242(7) 0.81069(16) 0.43274(10) 0.0262(4) Uani 1 1 d . . . H4 H -0.0353 0.8181 0.4670 0.031 Uiso 1 1 calc R . . C5 C 0.04146(7) 0.69586(15) 0.43356(9) 0.0232(4) Uani 1 1 d . . . H5 H 0.0299 0.6241 0.4688 0.028 Uiso 1 1 calc R . . C6 C 0.09735(7) 0.68112(14) 0.38452(9) 0.0197(3) Uani 1 1 d . . . C7 C 0.08965(7) 1.02976(14) 0.27522(9) 0.0210(3) Uani 1 1 d . . . C8 C 0.08994(8) 0.98467(16) 0.18726(9) 0.0265(4) Uani 1 1 d . . . H8A H 0.1254 0.9178 0.1790 0.040 Uiso 1 1 calc R . . H8B H 0.0979 1.0633 0.1527 0.040 Uiso 1 1 calc R . . H8C H 0.0467 0.9441 0.1739 0.040 Uiso 1 1 calc R . . C9 C 0.15728(7) 1.09175(15) 0.29854(10) 0.0261(4) Uani 1 1 d . . . H9A H 0.1921 1.0223 0.2951 0.039 Uiso 1 1 calc R . . H9B H 0.1549 1.1263 0.3535 0.039 Uiso 1 1 calc R . . H9C H 0.1679 1.1663 0.2619 0.039 Uiso 1 1 calc R . . C10 C 0.03766(8) 1.14370(15) 0.28168(10) 0.0272(4) Uani 1 1 d . . . H10A H 0.0494 1.2169 0.2446 0.041 Uiso 1 1 calc R . . H10B H 0.0370 1.1788 0.3366 0.041 Uiso 1 1 calc R . . H10C H -0.0066 1.1081 0.2680 0.041 Uiso 1 1 calc R . . C11 C 0.13723(7) 0.54819(15) 0.38765(9) 0.0208(3) Uani 1 1 d . . . C12 C 0.13901(8) 0.48084(15) 0.30490(10) 0.0251(4) Uani 1 1 d . . . H12A H 0.0938 0.4521 0.2900 0.038 Uiso 1 1 calc R . . H12B H 0.1685 0.4017 0.3066 0.038 Uiso 1 1 calc R . . H12C H 0.1558 0.5456 0.2652 0.038 Uiso 1 1 calc R . . C13 C 0.20849(7) 0.57441(15) 0.41818(10) 0.0241(4) Uani 1 1 d . . . H13A H 0.2320 0.6338 0.3805 0.036 Uiso 1 1 calc R . . H13B H 0.2325 0.4882 0.4226 0.036 Uiso 1 1 calc R . . H13C H 0.2065 0.6179 0.4709 0.036 Uiso 1 1 calc R . . C14 C 0.10658(8) 0.44346(15) 0.44498(10) 0.0279(4) Uani 1 1 d . . . H14A H 0.1060 0.4802 0.4995 0.042 Uiso 1 1 calc R . . H14B H 0.1333 0.3604 0.4439 0.042 Uiso 1 1 calc R . . H14C H 0.0608 0.4230 0.4281 0.042 Uiso 1 1 calc R . . C15 C 0.23555(8) 0.47555(15) 0.12612(10) 0.0253(4) Uani 1 1 d . . . H15A H 0.2440 0.4242 0.1761 0.030 Uiso 1 1 calc R . . H15B H 0.2755 0.4691 0.0913 0.030 Uiso 1 1 calc R . . C16 C 0.17436(8) 0.42107(16) 0.08331(11) 0.0307(4) Uani 1 1 d . . . H16A H 0.1417 0.3832 0.1219 0.037 Uiso 1 1 calc R . . H16B H 0.1867 0.3501 0.0441 0.037 Uiso 1 1 calc R . . C17 C 0.14635(8) 0.54563(16) 0.04143(10) 0.0263(4) Uani 1 1 d . . . H17A H 0.1704 0.5643 -0.0092 0.032 Uiso 1 1 calc R . . H17B H 0.0981 0.5351 0.0299 0.032 Uiso 1 1 calc R . . C18 C 0.15839(7) 0.65539(16) 0.10218(10) 0.0244(4) Uani 1 1 d . . . H18A H 0.1637 0.7442 0.0754 0.029 Uiso 1 1 calc R . . H18B H 0.1206 0.6612 0.1403 0.029 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 0.0155(4) 0.0202(4) 0.0197(4) 0.000 0.000 -0.0008(3) O1 0.0156(5) 0.0205(6) 0.0217(6) 0.0007(4) 0.0022(4) 0.0006(4) O2 0.0201(6) 0.0230(5) 0.0230(6) -0.0025(5) -0.0026(5) 0.0000(5) C1 0.0140(8) 0.0221(8) 0.0193(8) -0.0038(6) -0.0014(6) -0.0014(6) C2 0.0171(8) 0.0207(8) 0.0198(8) -0.0019(6) -0.0036(6) -0.0008(6) C3 0.0208(8) 0.0247(8) 0.0262(9) -0.0028(7) 0.0000(7) 0.0040(7) C4 0.0183(8) 0.0333(9) 0.0270(9) -0.0012(8) 0.0064(7) 0.0020(7) C5 0.0203(8) 0.0253(8) 0.0239(9) 0.0027(7) 0.0018(7) -0.0016(7) C6 0.0174(8) 0.0213(8) 0.0205(8) -0.0010(6) -0.0021(6) -0.0005(6) C7 0.0181(8) 0.0212(8) 0.0237(9) -0.0002(7) 0.0002(7) 0.0032(6) C8 0.0272(9) 0.0281(9) 0.0241(9) 0.0025(7) -0.0009(7) 0.0029(7) C9 0.0260(9) 0.0220(8) 0.0302(9) -0.0010(7) -0.0009(7) 0.0015(7) C10 0.0247(9) 0.0247(8) 0.0322(10) 0.0008(7) -0.0009(8) 0.0045(7) C11 0.0183(8) 0.0229(8) 0.0211(8) 0.0030(7) 0.0021(7) 0.0008(6) C12 0.0282(9) 0.0202(8) 0.0270(9) -0.0005(7) 0.0026(7) -0.0008(7) C13 0.0212(8) 0.0264(8) 0.0247(9) 0.0021(7) 0.0008(7) 0.0037(7) C14 0.0282(9) 0.0258(8) 0.0296(10) 0.0054(7) 0.0053(7) 0.0015(7) C15 0.0270(9) 0.0237(8) 0.0254(9) -0.0037(7) -0.0007(7) 0.0013(7) C16 0.0293(9) 0.0284(9) 0.0344(10) -0.0068(8) -0.0044(8) -0.0027(8) C17 0.0178(8) 0.0362(9) 0.0249(9) -0.0029(7) -0.0016(7) -0.0031(7) C18 0.0204(8) 0.0280(8) 0.0248(9) 0.0025(7) -0.0040(7) 0.0019(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mg1 O1 1.8639(10) 2_565 ? Mg1 O1 1.8639(10) . ? Mg1 O2 2.0627(11) . ? Mg1 O2 2.0627(11) 2_565 ? O1 C1 1.3389(16) . ? O2 C15 1.4636(17) . ? O2 C18 1.4678(17) . ? C1 C2 1.4288(19) . ? C1 C6 1.434(2) . ? C2 C3 1.394(2) . ? C2 C7 1.540(2) . ? C3 C4 1.381(2) . ? C3 H3 0.9500 . ? C4 C5 1.377(2) . ? C4 H4 0.9500 . ? C5 C6 1.394(2) . ? C5 H5 0.9500 . ? C6 C11 1.537(2) . ? C7 C8 1.534(2) . ? C7 C9 1.536(2) . ? C7 C10 1.536(2) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.533(2) . ? C11 C14 1.537(2) . ? C11 C13 1.537(2) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C16 1.517(2) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.522(2) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.503(2) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Mg1 O1 122.85(7) 2_565 . ? O1 Mg1 O2 118.95(4) 2_565 . ? O1 Mg1 O2 101.53(4) . . ? O1 Mg1 O2 101.53(4) 2_565 2_565 ? O1 Mg1 O2 118.95(4) . 2_565 ? O2 Mg1 O2 88.71(6) . 2_565 ? C1 O1 Mg1 170.99(9) . . ? C15 O2 C18 109.06(11) . . ? C15 O2 Mg1 133.80(9) . . ? C18 O2 Mg1 114.94(8) . . ? O1 C1 C2 120.41(13) . . ? O1 C1 C6 120.68(12) . . ? C2 C1 C6 118.91(13) . . ? C3 C2 C1 118.59(14) . . ? C3 C2 C7 119.27(13) . . ? C1 C2 C7 122.14(13) . . ? C4 C3 C2 122.55(15) . . ? C4 C3 H3 118.7 . . ? C2 C3 H3 118.7 . . ? C5 C4 C3 118.81(14) . . ? C5 C4 H4 120.6 . . ? C3 C4 H4 120.6 . . ? C4 C5 C6 122.39(14) . . ? C4 C5 H5 118.8 . . ? C6 C5 H5 118.8 . . ? C5 C6 C1 118.69(13) . . ? C5 C6 C11 119.09(13) . . ? C1 C6 C11 122.21(13) . . ? C8 C7 C9 110.77(13) . . ? C8 C7 C10 106.40(13) . . ? C9 C7 C10 106.72(12) . . ? C8 C7 C2 110.44(12) . . ? C9 C7 C2 109.42(12) . . ? C10 C7 C2 113.01(12) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C12 C11 C14 106.14(12) . . ? C12 C11 C13 110.49(12) . . ? C14 C11 C13 106.13(13) . . ? C12 C11 C6 110.60(12) . . ? C14 C11 C6 112.85(12) . . ? C13 C11 C6 110.46(12) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C11 C14 H14A 109.5 . . ? C11 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C11 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? O2 C15 C16 105.30(12) . . ? O2 C15 H15A 110.7 . . ? C16 C15 H15A 110.7 . . ? O2 C15 H15B 110.7 . . ? C16 C15 H15B 110.7 . . ? H15A C15 H15B 108.8 . . ? C15 C16 C17 103.14(12) . . ? C15 C16 H16A 111.1 . . ? C17 C16 H16A 111.1 . . ? C15 C16 H16B 111.1 . . ? C17 C16 H16B 111.1 . . ? H16A C16 H16B 109.1 . . ? C18 C17 C16 102.35(13) . . ? C18 C17 H17A 111.3 . . ? C16 C17 H17A 111.3 . . ? C18 C17 H17B 111.3 . . ? C16 C17 H17B 111.3 . . ? H17A C17 H17B 109.2 . . ? O2 C18 C17 105.70(12) . . ? O2 C18 H18A 110.6 . . ? C17 C18 H18A 110.6 . . ? O2 C18 H18B 110.6 . . ? C17 C18 H18B 110.6 . . ? H18A C18 H18B 108.7 . . ? 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 O1 Mg1 O1 C1 -37.9(6) 2_565 . . . ? O2 Mg1 O1 C1 98.2(6) . . . . ? O2 Mg1 O1 C1 -166.9(6) 2_565 . . . ? O1 Mg1 O2 C15 22.63(14) 2_565 . . . ? O1 Mg1 O2 C15 -115.58(12) . . . . ? O2 Mg1 O2 C15 125.11(13) 2_565 . . . ? O1 Mg1 O2 C18 -176.48(9) 2_565 . . . ? O1 Mg1 O2 C18 45.31(10) . . . . ? O2 Mg1 O2 C18 -74.00(9) 2_565 . . . ? Mg1 O1 C1 C2 158.3(5) . . . . ? Mg1 O1 C1 C6 -22.4(7) . . . . ? O1 C1 C2 C3 -178.65(13) . . . . ? C6 C1 C2 C3 2.0(2) . . . . ? O1 C1 C2 C7 0.5(2) . . . . ? C6 C1 C2 C7 -178.84(13) . . . . ? C1 C2 C3 C4 -0.5(2) . . . . ? C7 C2 C3 C4 -179.70(14) . . . . ? C2 C3 C4 C5 -0.6(2) . . . . ? C3 C4 C5 C6 0.2(2) . . . . ? C4 C5 C6 C1 1.3(2) . . . . ? C4 C5 C6 C11 -178.50(14) . . . . ? O1 C1 C6 C5 178.31(13) . . . . ? C2 C1 C6 C5 -2.4(2) . . . . ? O1 C1 C6 C11 -1.9(2) . . . . ? C2 C1 C6 C11 177.38(13) . . . . ? C3 C2 C7 C8 -121.39(15) . . . . ? C1 C2 C7 C8 59.49(18) . . . . ? C3 C2 C7 C9 116.43(15) . . . . ? C1 C2 C7 C9 -62.70(18) . . . . ? C3 C2 C7 C10 -2.3(2) . . . . ? C1 C2 C7 C10 178.54(13) . . . . ? C5 C6 C11 C12 121.02(15) . . . . ? C1 C6 C11 C12 -58.72(18) . . . . ? C5 C6 C11 C14 2.3(2) . . . . ? C1 C6 C11 C14 -177.46(14) . . . . ? C5 C6 C11 C13 -116.33(15) . . . . ? C1 C6 C11 C13 63.92(18) . . . . ? C18 O2 C15 C16 -9.74(16) . . . . ? Mg1 O2 C15 C16 151.96(11) . . . . ? O2 C15 C16 C17 29.63(16) . . . . ? C15 C16 C17 C18 -37.83(16) . . . . ? C15 O2 C18 C17 -14.43(16) . . . . ? Mg1 O2 C18 C17 -179.95(9) . . . . ? C16 C17 C18 O2 32.37(15) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.204 _refine_diff_density_min -0.219 _refine_diff_density_rms 0.044 #===END data_h16 _database_code_CSD 200474 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H58 Mg N2 O2' _chemical_formula_weight 551.13 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Mg Mg 0.0486 0.0363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 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 11.6257(2) _cell_length_b 15.3910(2) _cell_length_c 18.7651(3) _cell_angle_alpha 90.00 _cell_angle_beta 96.118(1) _cell_angle_gamma 90.00 _cell_volume 3338.54(9) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 7649 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.48 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.70 _exptl_crystal_size_mid 0.55 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.097 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1216 _exptl_absorpt_coefficient_mu 0.083 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; Most of sample heavily twinned. This was better, but still not entirely single. ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method 'phi and omega scans ' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 13620 _diffrn_reflns_av_R_equivalents 0.0182 _diffrn_reflns_av_sigmaI/netI 0.0298 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.72 _diffrn_reflns_theta_max 27.49 _reflns_number_total 7604 _reflns_number_gt 6245 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect and Denzo' _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution SIR-92 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0375P)^2^+1.1600P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7604 _refine_ls_number_parameters 368 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0516 _refine_ls_R_factor_gt 0.0379 _refine_ls_wR_factor_ref 0.0959 _refine_ls_wR_factor_gt 0.0886 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.040 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mg1 Mg 0.21443(3) 0.40620(2) 0.75255(2) 0.01758(9) Uani 1 1 d . . . O1 O 0.30897(7) 0.31909(5) 0.79808(4) 0.01947(17) Uani 1 1 d . . . O2 O 0.05306(7) 0.39022(5) 0.74372(4) 0.01995(17) Uani 1 1 d . . . N1 N 0.30885(9) 0.44406(7) 0.65784(6) 0.0248(2) Uani 1 1 d . . . N2 N 0.24235(8) 0.54911(6) 0.77877(6) 0.0232(2) Uani 1 1 d . . . C1 C 0.34996(9) 0.24903(7) 0.83413(6) 0.0179(2) Uani 1 1 d . . . C2 C 0.32912(9) 0.16331(7) 0.80547(6) 0.0194(2) Uani 1 1 d . . . C3 C 0.36250(11) 0.09205(8) 0.84884(7) 0.0242(3) Uani 1 1 d . . . H3 H 0.3451 0.0353 0.8309 0.029 Uiso 1 1 calc R . . C4 C 0.41979(11) 0.10089(8) 0.91681(7) 0.0277(3) Uani 1 1 d . . . H4 H 0.4393 0.0512 0.9456 0.033 Uiso 1 1 calc R . . C5 C 0.44824(11) 0.18319(8) 0.94211(7) 0.0257(3) Uani 1 1 d . . . H5 H 0.4911 0.1892 0.9879 0.031 Uiso 1 1 calc R . . C6 C 0.41622(10) 0.25783(8) 0.90278(6) 0.0205(2) Uani 1 1 d . . . C7 C 0.26829(10) 0.14618(7) 0.72994(7) 0.0226(2) Uani 1 1 d . . . C8 C 0.32404(13) 0.19865(9) 0.67368(7) 0.0334(3) Uani 1 1 d . . . H8A H 0.3170 0.2608 0.6837 0.050 Uiso 1 1 calc R . . H8B H 0.2849 0.1857 0.6260 0.050 Uiso 1 1 calc R . . H8C H 0.4060 0.1831 0.6753 0.050 Uiso 1 1 calc R . . C9 C 0.13948(11) 0.16857(9) 0.72743(8) 0.0301(3) Uani 1 1 d . . . H9A H 0.1308 0.2303 0.7383 0.045 Uiso 1 1 calc R . . H9B H 0.1042 0.1335 0.7629 0.045 Uiso 1 1 calc R . . H9C H 0.1010 0.1562 0.6795 0.045 Uiso 1 1 calc R . . C10 C 0.27587(12) 0.05010(8) 0.70752(8) 0.0325(3) Uani 1 1 d . . . H10A H 0.2416 0.0432 0.6578 0.049 Uiso 1 1 calc R . . H10B H 0.2337 0.0139 0.7390 0.049 Uiso 1 1 calc R . . H10C H 0.3572 0.0321 0.7115 0.049 Uiso 1 1 calc R . . C11 C 0.44785(10) 0.34715(8) 0.93620(6) 0.0229(2) Uani 1 1 d . . . C12 C 0.33769(11) 0.39056(8) 0.95760(7) 0.0265(3) Uani 1 1 d . . . H12A H 0.3036 0.3540 0.9926 0.040 Uiso 1 1 calc R . . H12B H 0.2820 0.3979 0.9150 0.040 Uiso 1 1 calc R . . H12C H 0.3571 0.4475 0.9789 0.040 Uiso 1 1 calc R . . C13 C 0.50775(11) 0.40471(8) 0.88441(7) 0.0267(3) Uani 1 1 d . . . H13A H 0.5270 0.4610 0.9071 0.040 Uiso 1 1 calc R . . H13B H 0.4557 0.4136 0.8404 0.040 Uiso 1 1 calc R . . H13C H 0.5788 0.3762 0.8727 0.040 Uiso 1 1 calc R . . C14 C 0.53299(12) 0.34030(10) 1.00469(7) 0.0355(3) Uani 1 1 d . . . H14A H 0.4968 0.3076 1.0412 0.053 Uiso 1 1 calc R . . H14B H 0.5530 0.3987 1.0227 0.053 Uiso 1 1 calc R . . H14C H 0.6033 0.3102 0.9937 0.053 Uiso 1 1 calc R . . C15 C -0.05760(9) 0.36864(7) 0.74577(6) 0.0177(2) Uani 1 1 d . . . C16 C -0.13540(10) 0.36480(7) 0.68093(6) 0.0203(2) Uani 1 1 d . . . C17 C -0.25018(10) 0.34032(8) 0.68463(7) 0.0241(3) Uani 1 1 d . . . H17 H -0.3013 0.3381 0.6417 0.029 Uiso 1 1 calc R . . C18 C -0.29201(10) 0.31921(8) 0.74838(7) 0.0259(3) Uani 1 1 d . . . H18 H -0.3702 0.3018 0.7493 0.031 Uiso 1 1 calc R . . C19 C -0.21789(10) 0.32378(7) 0.81093(7) 0.0234(3) Uani 1 1 d . . . H19 H -0.2467 0.3088 0.8548 0.028 Uiso 1 1 calc R . . C20 C -0.10260(10) 0.34942(7) 0.81232(6) 0.0190(2) Uani 1 1 d . . . C21 C -0.09550(11) 0.38595(8) 0.60734(6) 0.0244(3) Uani 1 1 d . . . C22 C -0.19444(12) 0.38157(10) 0.54598(7) 0.0356(3) Uani 1 1 d . . . H22A H -0.2272 0.3229 0.5434 0.053 Uiso 1 1 calc R . . H22B H -0.1643 0.3956 0.5005 0.053 Uiso 1 1 calc R . . H22C H -0.2547 0.4234 0.5550 0.053 Uiso 1 1 calc R . . C23 C -0.04735(12) 0.47884(8) 0.60707(7) 0.0290(3) Uani 1 1 d . . . H23A H -0.1080 0.5201 0.6166 0.043 Uiso 1 1 calc R . . H23B H -0.0214 0.4914 0.5601 0.043 Uiso 1 1 calc R . . H23C H 0.0181 0.4843 0.6443 0.043 Uiso 1 1 calc R . . C24 C -0.00485(12) 0.31874(9) 0.58995(7) 0.0308(3) Uani 1 1 d . . . H24A H 0.0615 0.3209 0.6268 0.046 Uiso 1 1 calc R . . H24B H 0.0209 0.3319 0.5431 0.046 Uiso 1 1 calc R . . H24C H -0.0391 0.2605 0.5889 0.046 Uiso 1 1 calc R . . C25 C -0.02937(10) 0.35537(8) 0.88563(6) 0.0231(2) Uani 1 1 d . . . C26 C -0.10308(12) 0.34628(10) 0.94887(7) 0.0346(3) Uani 1 1 d . . . H26A H -0.1645 0.3902 0.9446 0.052 Uiso 1 1 calc R . . H26B H -0.0539 0.3546 0.9941 0.052 Uiso 1 1 calc R . . H26C H -0.1378 0.2882 0.9481 0.052 Uiso 1 1 calc R . . C27 C 0.06138(11) 0.28222(8) 0.89280(7) 0.0278(3) Uani 1 1 d . . . H27A H 0.0223 0.2258 0.8875 0.042 Uiso 1 1 calc R . . H27B H 0.1060 0.2855 0.9401 0.042 Uiso 1 1 calc R . . H27C H 0.1136 0.2888 0.8554 0.042 Uiso 1 1 calc R . . C28 C 0.02934(11) 0.44457(8) 0.89571(7) 0.0266(3) Uani 1 1 d . . . H28A H 0.0815 0.4531 0.8586 0.040 Uiso 1 1 calc R . . H28B H 0.0737 0.4473 0.9431 0.040 Uiso 1 1 calc R . . H28C H -0.0297 0.4902 0.8919 0.040 Uiso 1 1 calc R . . C29 C 0.30338(12) 0.54073(8) 0.65639(8) 0.0316(3) Uani 1 1 d . . . H29A H 0.2255 0.5592 0.6353 0.038 Uiso 1 1 calc R . . H29B H 0.3605 0.5632 0.6255 0.038 Uiso 1 1 calc R . . C30 C 0.32786(11) 0.57911(8) 0.73022(8) 0.0313(3) Uani 1 1 d . . . H30A H 0.4067 0.5622 0.7507 0.038 Uiso 1 1 calc R . . H30B H 0.3253 0.6433 0.7268 0.038 Uiso 1 1 calc R . . C31 C 0.26504(12) 0.41281(10) 0.58513(7) 0.0339(3) Uani 1 1 d . . . H31A H 0.1847 0.4317 0.5735 0.051 Uiso 1 1 calc R . . H31B H 0.2687 0.3492 0.5839 0.051 Uiso 1 1 calc R . . H31C H 0.3128 0.4369 0.5499 0.051 Uiso 1 1 calc R . . C32 C 0.43230(10) 0.41721(8) 0.67128(8) 0.0277(3) Uani 1 1 d . . . H32A H 0.4761 0.4427 0.6346 0.042 Uiso 1 1 calc R . . H32B H 0.4376 0.3537 0.6694 0.042 Uiso 1 1 calc R . . H32C H 0.4645 0.4376 0.7187 0.042 Uiso 1 1 calc R . . C33 C 0.13170(10) 0.59675(8) 0.76065(7) 0.0252(3) Uani 1 1 d . . . H33A H 0.0746 0.5768 0.7919 0.038 Uiso 1 1 calc R . . H33B H 0.1027 0.5856 0.7105 0.038 Uiso 1 1 calc R . . H33C H 0.1449 0.6592 0.7676 0.038 Uiso 1 1 calc R . . C34 C 0.28616(12) 0.57559(8) 0.85253(8) 0.0331(3) Uani 1 1 d . . . H34A H 0.2966 0.6388 0.8543 0.050 Uiso 1 1 calc R . . H34B H 0.3605 0.5470 0.8666 0.050 Uiso 1 1 calc R . . H34C H 0.2304 0.5585 0.8856 0.050 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 0.01674(18) 0.01834(19) 0.01749(19) 0.00176(14) 0.00099(14) -0.00001(14) O1 0.0206(4) 0.0170(4) 0.0203(4) 0.0013(3) -0.0002(3) 0.0007(3) O2 0.0170(4) 0.0237(4) 0.0191(4) 0.0009(3) 0.0018(3) -0.0010(3) N1 0.0228(5) 0.0263(5) 0.0260(6) 0.0072(4) 0.0062(4) 0.0025(4) N2 0.0218(5) 0.0195(5) 0.0273(5) 0.0020(4) -0.0014(4) 0.0003(4) C1 0.0164(5) 0.0187(5) 0.0188(6) 0.0013(4) 0.0036(4) 0.0013(4) C2 0.0178(5) 0.0200(5) 0.0212(6) -0.0011(4) 0.0054(4) 0.0003(4) C3 0.0280(6) 0.0176(6) 0.0280(6) 0.0003(5) 0.0085(5) 0.0029(5) C4 0.0348(7) 0.0238(6) 0.0251(6) 0.0067(5) 0.0063(5) 0.0099(5) C5 0.0284(6) 0.0294(7) 0.0193(6) 0.0014(5) 0.0019(5) 0.0076(5) C6 0.0195(5) 0.0231(6) 0.0191(6) -0.0009(4) 0.0033(4) 0.0031(4) C7 0.0258(6) 0.0182(6) 0.0239(6) -0.0026(5) 0.0034(5) -0.0039(4) C8 0.0479(8) 0.0316(7) 0.0217(6) -0.0055(5) 0.0081(6) -0.0128(6) C9 0.0266(6) 0.0279(7) 0.0345(7) -0.0020(5) -0.0036(5) -0.0032(5) C10 0.0407(8) 0.0233(6) 0.0327(7) -0.0080(5) 0.0007(6) -0.0032(5) C11 0.0229(6) 0.0255(6) 0.0194(6) -0.0028(5) -0.0016(5) 0.0021(5) C12 0.0300(6) 0.0258(6) 0.0240(6) -0.0058(5) 0.0043(5) 0.0020(5) C13 0.0232(6) 0.0272(6) 0.0294(7) -0.0052(5) 0.0020(5) -0.0024(5) C14 0.0378(8) 0.0370(8) 0.0284(7) -0.0056(6) -0.0115(6) 0.0015(6) C15 0.0174(5) 0.0143(5) 0.0214(6) -0.0002(4) 0.0023(4) 0.0017(4) C16 0.0221(6) 0.0162(5) 0.0221(6) -0.0018(4) 0.0003(5) 0.0029(4) C17 0.0213(6) 0.0182(6) 0.0311(7) -0.0020(5) -0.0045(5) 0.0023(4) C18 0.0167(5) 0.0193(6) 0.0417(8) 0.0017(5) 0.0029(5) 0.0002(4) C19 0.0230(6) 0.0173(6) 0.0313(7) 0.0047(5) 0.0088(5) 0.0030(4) C20 0.0206(5) 0.0144(5) 0.0222(6) 0.0022(4) 0.0034(4) 0.0031(4) C21 0.0261(6) 0.0284(6) 0.0180(6) -0.0016(5) -0.0019(5) 0.0028(5) C22 0.0374(8) 0.0450(8) 0.0222(7) -0.0030(6) -0.0070(6) 0.0042(6) C23 0.0348(7) 0.0315(7) 0.0207(6) 0.0042(5) 0.0032(5) 0.0004(5) C24 0.0330(7) 0.0367(7) 0.0224(6) -0.0068(5) 0.0015(5) 0.0050(6) C25 0.0241(6) 0.0257(6) 0.0200(6) 0.0046(5) 0.0046(5) 0.0018(5) C26 0.0368(7) 0.0454(8) 0.0230(7) 0.0074(6) 0.0091(6) 0.0026(6) C27 0.0264(6) 0.0301(7) 0.0265(7) 0.0081(5) 0.0003(5) 0.0042(5) C28 0.0323(7) 0.0285(7) 0.0188(6) -0.0011(5) 0.0010(5) 0.0012(5) C29 0.0315(7) 0.0268(7) 0.0390(8) 0.0143(6) 0.0142(6) 0.0056(5) C30 0.0250(6) 0.0192(6) 0.0505(9) 0.0062(6) 0.0075(6) -0.0013(5) C31 0.0342(7) 0.0468(8) 0.0217(7) 0.0056(6) 0.0071(5) 0.0035(6) C32 0.0215(6) 0.0248(6) 0.0379(7) 0.0065(5) 0.0082(5) 0.0004(5) C33 0.0234(6) 0.0220(6) 0.0296(7) 0.0006(5) 0.0002(5) 0.0039(5) C34 0.0371(7) 0.0237(6) 0.0354(8) -0.0042(6) -0.0106(6) 0.0000(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mg1 O1 1.8803(8) . ? Mg1 O2 1.8817(9) . ? Mg1 N1 2.2625(11) . ? Mg1 N2 2.2695(11) . ? O1 C1 1.3337(13) . ? O2 C15 1.3333(13) . ? N1 C31 1.4846(17) . ? N1 C32 1.4890(15) . ? N1 C29 1.4894(16) . ? N2 C34 1.4803(16) . ? N2 C33 1.4881(15) . ? N2 C30 1.4916(17) . ? C1 C6 1.4352(16) . ? C1 C2 1.4355(16) . ? C2 C3 1.3958(17) . ? C2 C7 1.5379(16) . ? C3 C4 1.3814(18) . ? C3 H3 0.9500 . ? C4 C5 1.3806(18) . ? C4 H4 0.9500 . ? C5 C6 1.3944(17) . ? C5 H5 0.9500 . ? C6 C11 1.5392(16) . ? C7 C8 1.5272(17) . ? C7 C9 1.5324(17) . ? C7 C10 1.5427(17) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.5354(17) . ? C11 C13 1.5357(18) . ? C11 C14 1.5400(16) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? 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 C20 1.4352(16) . ? C15 C16 1.4379(16) . ? C16 C17 1.3954(16) . ? C16 C21 1.5377(17) . ? C17 C18 1.3774(18) . ? C17 H17 0.9500 . ? C18 C19 1.3820(18) . ? C18 H18 0.9500 . ? C19 C20 1.3948(16) . ? C19 H19 0.9500 . ? C20 C25 1.5415(16) . ? C21 C23 1.5356(18) . ? C21 C24 1.5365(17) . ? C21 C22 1.5398(17) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C28 1.5358(17) . ? C25 C27 1.5389(17) . ? C25 C26 1.5424(17) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 C30 1.505(2) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Mg1 O2 118.41(4) . . ? O1 Mg1 N1 103.39(4) . . ? O2 Mg1 N1 121.81(4) . . ? O1 Mg1 N2 121.96(4) . . ? O2 Mg1 N2 105.30(4) . . ? N1 Mg1 N2 81.41(4) . . ? C1 O1 Mg1 165.23(8) . . ? C15 O2 Mg1 170.41(8) . . ? C31 N1 C32 107.21(10) . . ? C31 N1 C29 107.29(10) . . ? C32 N1 C29 108.59(10) . . ? C31 N1 Mg1 119.39(8) . . ? C32 N1 Mg1 109.58(7) . . ? C29 N1 Mg1 104.38(7) . . ? C34 N2 C33 106.31(10) . . ? C34 N2 C30 107.50(10) . . ? C33 N2 C30 108.91(10) . . ? C34 N2 Mg1 119.77(8) . . ? C33 N2 Mg1 109.13(7) . . ? C30 N2 Mg1 104.88(7) . . ? O1 C1 C6 120.50(10) . . ? O1 C1 C2 121.07(10) . . ? C6 C1 C2 118.42(10) . . ? C3 C2 C1 118.58(11) . . ? C3 C2 C7 118.33(10) . . ? C1 C2 C7 123.06(10) . . ? C4 C3 C2 122.53(11) . . ? C4 C3 H3 118.7 . . ? C2 C3 H3 118.7 . . ? C5 C4 C3 118.82(11) . . ? C5 C4 H4 120.6 . . ? C3 C4 H4 120.6 . . ? C4 C5 C6 122.23(11) . . ? C4 C5 H5 118.9 . . ? C6 C5 H5 118.9 . . ? C5 C6 C1 119.00(11) . . ? C5 C6 C11 118.78(10) . . ? C1 C6 C11 122.14(10) . . ? C8 C7 C9 110.20(11) . . ? C8 C7 C2 111.04(10) . . ? C9 C7 C2 109.98(10) . . ? C8 C7 C10 106.11(10) . . ? C9 C7 C10 106.93(10) . . ? C2 C7 C10 112.44(10) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C12 C11 C13 111.20(10) . . ? C12 C11 C6 109.00(10) . . ? C13 C11 C6 111.23(10) . . ? C12 C11 C14 106.94(10) . . ? C13 C11 C14 105.85(10) . . ? C6 C11 C14 112.54(10) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C11 C14 H14A 109.5 . . ? C11 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C11 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? O2 C15 C20 121.25(10) . . ? O2 C15 C16 120.51(10) . . ? C20 C15 C16 118.23(10) . . ? C17 C16 C15 119.18(11) . . ? C17 C16 C21 118.91(11) . . ? C15 C16 C21 121.90(10) . . ? C18 C17 C16 122.34(11) . . ? C18 C17 H17 118.8 . . ? C16 C17 H17 118.8 . . ? C17 C18 C19 118.67(11) . . ? C17 C18 H18 120.7 . . ? C19 C18 H18 120.7 . . ? C18 C19 C20 122.77(12) . . ? C18 C19 H19 118.6 . . ? C20 C19 H19 118.6 . . ? C19 C20 C15 118.73(11) . . ? C19 C20 C25 118.14(10) . . ? C15 C20 C25 123.12(10) . . ? C23 C21 C24 111.57(11) . . ? C23 C21 C16 110.18(10) . . ? C24 C21 C16 109.13(10) . . ? C23 C21 C22 106.37(10) . . ? C24 C21 C22 106.64(10) . . ? C16 C21 C22 112.92(11) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C21 C24 H24A 109.5 . . ? C21 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C21 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C28 C25 C27 110.59(10) . . ? C28 C25 C20 111.03(9) . . ? C27 C25 C20 110.05(10) . . ? C28 C25 C26 105.21(10) . . ? C27 C25 C26 107.36(10) . . ? C20 C25 C26 112.45(10) . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C25 C28 H28A 109.5 . . ? C25 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C25 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? N1 C29 C30 111.83(10) . . ? N1 C29 H29A 109.3 . . ? C30 C29 H29A 109.3 . . ? N1 C29 H29B 109.3 . . ? C30 C29 H29B 109.3 . . ? H29A C29 H29B 107.9 . . ? N2 C30 C29 111.58(10) . . ? N2 C30 H30A 109.3 . . ? C29 C30 H30A 109.3 . . ? N2 C30 H30B 109.3 . . ? C29 C30 H30B 109.3 . . ? H30A C30 H30B 108.0 . . ? N1 C31 H31A 109.5 . . ? N1 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? N1 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? N1 C32 H32A 109.5 . . ? N1 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? N1 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? N2 C33 H33A 109.5 . . ? N2 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? N2 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? N2 C34 H34A 109.5 . . ? N2 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? N2 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 Mg1 O1 C1 -7.9(3) . . . . ? N1 Mg1 O1 C1 -146.0(3) . . . . ? N2 Mg1 O1 C1 125.8(3) . . . . ? O1 Mg1 O2 C15 16.0(5) . . . . ? N1 Mg1 O2 C15 146.2(4) . . . . ? N2 Mg1 O2 C15 -124.5(5) . . . . ? O1 Mg1 N1 C31 103.62(9) . . . . ? O2 Mg1 N1 C31 -32.69(10) . . . . ? N2 Mg1 N1 C31 -135.43(9) . . . . ? O1 Mg1 N1 C32 -20.48(9) . . . . ? O2 Mg1 N1 C32 -156.80(7) . . . . ? N2 Mg1 N1 C32 100.47(8) . . . . ? O1 Mg1 N1 C29 -136.61(8) . . . . ? O2 Mg1 N1 C29 87.07(9) . . . . ? N2 Mg1 N1 C29 -15.66(8) . . . . ? O1 Mg1 N2 C34 -33.00(11) . . . . ? O2 Mg1 N2 C34 105.78(9) . . . . ? N1 Mg1 N2 C34 -133.47(10) . . . . ? O1 Mg1 N2 C33 -155.75(7) . . . . ? O2 Mg1 N2 C33 -16.97(9) . . . . ? N1 Mg1 N2 C33 103.78(8) . . . . ? O1 Mg1 N2 C30 87.69(8) . . . . ? O2 Mg1 N2 C30 -133.53(8) . . . . ? N1 Mg1 N2 C30 -12.77(8) . . . . ? Mg1 O1 C1 C6 -111.8(3) . . . . ? Mg1 O1 C1 C2 68.2(3) . . . . ? O1 C1 C2 C3 -172.78(10) . . . . ? C6 C1 C2 C3 7.23(16) . . . . ? O1 C1 C2 C7 5.29(17) . . . . ? C6 C1 C2 C7 -174.71(10) . . . . ? C1 C2 C3 C4 -3.27(18) . . . . ? C7 C2 C3 C4 178.58(11) . . . . ? C2 C3 C4 C5 -1.96(19) . . . . ? C3 C4 C5 C6 3.15(19) . . . . ? C4 C5 C6 C1 0.96(18) . . . . ? C4 C5 C6 C11 177.87(11) . . . . ? O1 C1 C6 C5 173.86(10) . . . . ? C2 C1 C6 C5 -6.14(16) . . . . ? O1 C1 C6 C11 -2.93(17) . . . . ? C2 C1 C6 C11 177.06(10) . . . . ? C3 C2 C7 C8 -130.72(12) . . . . ? C1 C2 C7 C8 51.21(15) . . . . ? C3 C2 C7 C9 107.04(12) . . . . ? C1 C2 C7 C9 -71.03(14) . . . . ? C3 C2 C7 C10 -11.99(15) . . . . ? C1 C2 C7 C10 169.94(11) . . . . ? C5 C6 C11 C12 -107.29(12) . . . . ? C1 C6 C11 C12 69.51(14) . . . . ? C5 C6 C11 C13 129.75(12) . . . . ? C1 C6 C11 C13 -53.45(14) . . . . ? C5 C6 C11 C14 11.17(16) . . . . ? C1 C6 C11 C14 -172.03(11) . . . . ? Mg1 O2 C15 C20 40.2(5) . . . . ? Mg1 O2 C15 C16 -140.4(4) . . . . ? O2 C15 C16 C17 178.73(10) . . . . ? C20 C15 C16 C17 -1.81(16) . . . . ? O2 C15 C16 C21 -0.58(16) . . . . ? C20 C15 C16 C21 178.88(10) . . . . ? C15 C16 C17 C18 -0.27(17) . . . . ? C21 C16 C17 C18 179.06(11) . . . . ? C16 C17 C18 C19 1.01(18) . . . . ? C17 C18 C19 C20 0.41(18) . . . . ? C18 C19 C20 C15 -2.50(17) . . . . ? C18 C19 C20 C25 177.74(11) . . . . ? O2 C15 C20 C19 -177.42(10) . . . . ? C16 C15 C20 C19 3.12(15) . . . . ? O2 C15 C20 C25 2.33(16) . . . . ? C16 C15 C20 C25 -177.13(10) . . . . ? C17 C16 C21 C23 122.02(12) . . . . ? C15 C16 C21 C23 -58.67(14) . . . . ? C17 C16 C21 C24 -115.16(12) . . . . ? C15 C16 C21 C24 64.15(14) . . . . ? C17 C16 C21 C22 3.25(16) . . . . ? C15 C16 C21 C22 -177.44(11) . . . . ? C19 C20 C25 C28 -127.36(11) . . . . ? C15 C20 C25 C28 52.89(14) . . . . ? C19 C20 C25 C27 109.86(12) . . . . ? C15 C20 C25 C27 -69.89(14) . . . . ? C19 C20 C25 C26 -9.77(15) . . . . ? C15 C20 C25 C26 170.48(11) . . . . ? C31 N1 C29 C30 170.92(10) . . . . ? C32 N1 C29 C30 -73.51(13) . . . . ? Mg1 N1 C29 C30 43.31(12) . . . . ? C34 N2 C30 C29 169.03(10) . . . . ? C33 N2 C30 C29 -76.18(12) . . . . ? Mg1 N2 C30 C29 40.53(11) . . . . ? N1 C29 C30 N2 -60.33(14) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.271 _refine_diff_density_min -0.207 _refine_diff_density_rms 0.036 #===END