Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2003 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Vernon Gibson' 'Andrew P. Dove' 'Pimpa Horminum' 'Edward L. Marshall' 'John A. Segal' 'Andrew J.P. White' 'David J. Williams' _publ_contact_author_name 'Prof Vernon Gibson' _publ_contact_author_address ; Department of Chemistry Imperial College Exhibition Road South Kensington London SW7 2AZ UNITED KINGDOM ; _publ_contact_author_email V.GIBSON@IMPERIAL.AC.UK _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Low coordinate magnesium chemistry supported by a bulky beta-diketiminate ligand ; data_Compound_4 _database_code_CSD 207267 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C39 H56 N2 Mg' _chemical_formula_weight 577.17 _chemical_melting_point ? _chemical_compound_source ? 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 P2(1)/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 9.9099(6) _cell_length_b 20.430(2) _cell_length_c 18.414(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.832(4) _cell_angle_gamma 90.00 _cell_volume 3727.7(6) _cell_formula_units_Z 4 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 21 _cell_measurement_theta_min 10.79 _cell_measurement_theta_max 24.01 _exptl_crystal_description rhombs _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.83 _exptl_crystal_size_mid 0.77 _exptl_crystal_size_min 0.73 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.028 _exptl_crystal_density_method ? _exptl_crystal_F_000 1264 _exptl_absorpt_coefficient_mu 0.590 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(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 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 197 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5882 _diffrn_reflns_av_R_equivalents 0.0506 _diffrn_reflns_av_sigmaI/netI 0.0343 _diffrn_reflns_limit_h_min -3 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.23 _diffrn_reflns_theta_max 60.00 _reflns_number_total 5522 _reflns_number_observed 4226 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 373 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0801P)^2^+1.4198P] 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 ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0034(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 5149 _refine_ls_number_parameters 396 _refine_ls_number_restraints 26 _refine_ls_R_factor_all 0.0769 _refine_ls_R_factor_obs 0.0562 _refine_ls_wR_factor_all 0.1606 _refine_ls_wR_factor_obs 0.1435 _refine_ls_goodness_of_fit_all 1.050 _refine_ls_goodness_of_fit_obs 1.102 _refine_ls_restrained_S_all 1.075 _refine_ls_restrained_S_obs 1.109 _refine_ls_shift/esd_max 0.018 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Mg Mg 0.11847(9) 0.23310(4) 0.16926(4) 0.0434(2) Uani 1 d D . C1 C -0.0449(2) 0.30550(11) 0.05820(12) 0.0393(5) Uani 1 d . . N1 N 0.0034(2) 0.30502(9) 0.12599(10) 0.0362(4) Uani 1 d . . C2 C -0.0249(3) 0.25436(12) 0.00839(12) 0.0439(6) Uani 1 d . . H2A H -0.0610(3) 0.26170(12) -0.03898(12) 0.053 Uiso 1 calc R . C3 C 0.0403(3) 0.19445(11) 0.01834(12) 0.0391(5) Uani 1 d . . N3 N 0.1031(2) 0.17643(9) 0.07954(10) 0.0365(4) Uani 1 d . . C4 C -0.1268(3) 0.36304(13) 0.03181(15) 0.0574(8) Uani 1 d . . H4A H -0.1510(3) 0.35695(13) -0.01954(15) 0.086 Uiso 1 d R . H4B H -0.0737(3) 0.40322(13) 0.03752(15) 0.086 Uiso 1 d R . H4C H -0.2092(3) 0.36643(13) 0.06039(15) 0.086 Uiso 1 d R . C5 C 0.0356(3) 0.14760(13) -0.04532(13) 0.0561(7) Uani 1 d . . H5A H -0.0117(3) 0.16834(13) -0.08638(13) 0.084 Uiso 1 d R . H5B H -0.0123(3) 0.10762(13) -0.03149(13) 0.084 Uiso 1 d R . H5C H 0.1278(3) 0.13654(13) -0.05936(13) 0.084 Uiso 1 d R . C6 C -0.0243(2) 0.35910(11) 0.17356(11) 0.0355(5) Uani 1 d . . C7 C 0.0642(2) 0.41260(12) 0.17644(12) 0.0390(5) Uani 1 d . . C8 C 0.0440(3) 0.46023(13) 0.22911(14) 0.0481(6) Uani 1 d . . H8A H 0.1038(3) 0.49647(13) 0.23231(14) 0.058 Uiso 1 calc R . C9 C -0.0614(3) 0.45566(14) 0.27664(14) 0.0534(7) Uani 1 d . . H9A H -0.0735(3) 0.48848(14) 0.31251(14) 0.064 Uiso 1 calc R . C10 C -0.1492(3) 0.40391(14) 0.27239(14) 0.0500(6) Uani 1 d . . H10A H -0.2224(3) 0.40179(14) 0.30505(14) 0.060 Uiso 1 calc R . C11 C -0.1334(2) 0.35440(12) 0.22133(13) 0.0422(6) Uani 1 d . . C12 C 0.1814(3) 0.41892(13) 0.12438(14) 0.0480(6) Uani 1 d . . H12A H 0.1682(3) 0.38522(13) 0.08553(14) 0.058 Uiso 1 calc R . C13 C 0.3142(3) 0.4040(2) 0.1629(2) 0.0925(13) Uani 1 d . . H13A H 0.3089(3) 0.3610(2) 0.1862(2) 0.139 Uiso 1 calc R . H13B H 0.3324(3) 0.4375(2) 0.1999(2) 0.139 Uiso 1 calc R . H13C H 0.3872(3) 0.4038(2) 0.1276(2) 0.139 Uiso 1 calc R . C14 C 0.1856(4) 0.4850(2) 0.0877(2) 0.0698(9) Uani 1 d . . H14A H 0.0989(4) 0.4935(2) 0.0632(2) 0.105 Uiso 1 calc R . H14B H 0.2578(4) 0.4854(2) 0.0518(2) 0.105 Uiso 1 calc R . H14C H 0.2029(4) 0.5191(2) 0.1241(2) 0.105 Uiso 1 calc R . C15 C -0.2327(3) 0.29793(14) 0.2180(2) 0.0549(7) Uani 1 d . . H15A H -0.2118(3) 0.27079(14) 0.1744(2) 0.066 Uiso 1 calc R . C16 C -0.3774(3) 0.3221(2) 0.2104(3) 0.0952(13) Uani 1 d . . H16A H -0.4388(3) 0.2845(2) 0.2084(3) 0.143 Uiso 1 calc R . H16B H -0.3874(3) 0.3478(2) 0.1657(3) 0.143 Uiso 1 calc R . H16C H -0.3994(3) 0.3495(2) 0.2523(3) 0.143 Uiso 1 calc R . C17 C -0.2192(5) 0.2545(2) 0.2853(2) 0.1011(14) Uani 1 d . . H17A H -0.2843(5) 0.2184(2) 0.2819(2) 0.152 Uiso 1 calc R . H17B H -0.2372(5) 0.2805(2) 0.3288(2) 0.152 Uiso 1 calc R . H17C H -0.1275(5) 0.2367(2) 0.2884(2) 0.152 Uiso 1 calc R . C18 C 0.1529(3) 0.11063(11) 0.08706(12) 0.0395(6) Uani 1 d . . C19 C 0.0663(3) 0.06257(12) 0.11436(13) 0.0463(6) Uani 1 d . . C20 C 0.1193(3) 0.00042(13) 0.12831(14) 0.0575(8) Uani 1 d . . H20A H 0.0625(3) -0.03266(13) 0.14739(14) 0.069 Uiso 1 calc R . C21 C 0.2525(4) -0.01371(14) 0.1149(2) 0.0650(9) Uani 1 d . . H21A H 0.2871(4) -0.05621(14) 0.1248(2) 0.078 Uiso 1 calc R . C22 C 0.3352(3) 0.03357(14) 0.0872(2) 0.0600(8) Uani 1 d . . H22A H 0.4267(3) 0.02313(14) 0.0776(2) 0.072 Uiso 1 calc R . C23 C 0.2885(3) 0.09650(13) 0.07260(13) 0.0475(6) Uani 1 d . . C24 C -0.0809(3) 0.07677(14) 0.1291(2) 0.0597(8) Uani 1 d . . H24A H -0.1012(3) 0.12156(14) 0.1099(2) 0.072 Uiso 1 calc R . C25 C -0.1096(5) 0.0772(3) 0.2098(2) 0.113(2) Uani 1 d . . H25A H -0.2054(5) 0.0865(3) 0.2173(2) 0.170 Uiso 1 calc R . H25B H -0.0546(5) 0.1110(3) 0.2337(2) 0.170 Uiso 1 calc R . H25C H -0.0871(5) 0.0343(3) 0.2306(2) 0.170 Uiso 1 calc R . C26 C -0.1751(3) 0.0290(2) 0.0900(2) 0.0741(9) Uani 1 d . . H26A H -0.2689(3) 0.0399(2) 0.1010(2) 0.111 Uiso 1 calc R . H26B H -0.1554(3) -0.0157(2) 0.1064(2) 0.111 Uiso 1 calc R . H26C H -0.1615(3) 0.0320(2) 0.0375(2) 0.111 Uiso 1 calc R . C27 C 0.3838(3) 0.1475(2) 0.0435(2) 0.0600(7) Uani 1 d . . H27A H 0.3285(3) 0.1863(2) 0.0284(2) 0.072 Uiso 1 calc R . C28 C 0.4603(5) 0.1242(2) -0.0229(2) 0.0949(13) Uani 1 d . . H28A H 0.5204(5) 0.1591(2) -0.0395(2) 0.142 Uiso 1 calc R . H28B H 0.3960(5) 0.1131(2) -0.0619(2) 0.142 Uiso 1 calc R . H28C H 0.5139(5) 0.0855(2) -0.0101(2) 0.142 Uiso 1 calc R . C29 C 0.4832(4) 0.1700(2) 0.1020(2) 0.1010(14) Uani 1 d . . H29A H 0.5438(4) 0.2030(2) 0.0819(2) 0.152 Uiso 1 calc R . H29B H 0.5362(4) 0.1325(2) 0.1194(2) 0.152 Uiso 1 calc R . H29C H 0.4336(4) 0.1890(2) 0.1426(2) 0.152 Uiso 1 calc R . C30 C 0.2366(6) 0.2273(2) 0.2659(2) 0.0463(12) Uani 0.55 d PD 1 H30A H 0.3305(6) 0.2419(2) 0.2550(2) 0.056 Uiso 0.55 calc PR 1 C31 C 0.1803(9) 0.2712(4) 0.3279(3) 0.067(2) Uani 0.55 d PDU 1 H31A H 0.1744(9) 0.3167(4) 0.3111(3) 0.101 Uiso 0.55 calc PR 1 H31B H 0.2408(9) 0.2688(4) 0.3704(3) 0.101 Uiso 0.55 calc PR 1 H31C H 0.0903(9) 0.2558(4) 0.3412(3) 0.101 Uiso 0.55 calc PR 1 C32 C 0.2428(9) 0.1552(3) 0.2964(4) 0.081(2) Uani 0.55 d PDU 1 H32A H 0.2774(9) 0.1258(3) 0.2589(4) 0.121 Uiso 0.55 calc PR 1 H32B H 0.1520(9) 0.1411(3) 0.3100(4) 0.121 Uiso 0.55 calc PR 1 H32C H 0.3027(9) 0.1537(3) 0.3391(4) 0.121 Uiso 0.55 calc PR 1 C30' C 0.1768(8) 0.2144(4) 0.2786(4) 0.062(2) Uiso 0.45 d PD 2 H30B H 0.0975(8) 0.1961(4) 0.3047(4) 0.075 Uiso 0.45 calc PR 2 C31' C 0.2249(11) 0.2779(5) 0.3193(6) 0.075(4) Uiso 0.45 d PD 2 H31D H 0.1543(11) 0.3114(5) 0.3158(6) 0.112 Uiso 0.45 calc PR 2 H31E H 0.3075(11) 0.2943(5) 0.2970(6) 0.112 Uiso 0.45 calc PR 2 H31F H 0.2430(11) 0.2677(5) 0.3705(6) 0.112 Uiso 0.45 calc PR 2 C32' C 0.2988(9) 0.1661(5) 0.2886(6) 0.079(3) Uiso 0.45 d PD 2 H32D H 0.2778(9) 0.1245(5) 0.2643(6) 0.118 Uiso 0.45 calc PR 2 H32E H 0.3152(9) 0.1582(5) 0.3404(6) 0.118 Uiso 0.45 calc PR 2 H32F H 0.3797(9) 0.1853(5) 0.2671(6) 0.118 Uiso 0.45 calc PR 2 C40 C -0.4454(13) 0.6836(4) 0.0168(5) 0.131(4) Uani 0.60 d P 1 H40A H -0.3862(13) 0.6982(4) -0.0222(5) 0.196 Uiso 0.60 d PR 1 H40B H -0.4559(13) 0.7191(4) 0.0521(5) 0.196 Uiso 0.60 d PR 1 H40C H -0.5339(13) 0.6719(4) -0.0037(5) 0.196 Uiso 0.60 d PR 1 C41 C -0.2481(6) 0.6362(2) 0.0708(3) 0.077(2) Uani 0.60 d PG 1 H41A H -0.2039(6) 0.6764(2) 0.0606(3) 0.092 Uiso 0.60 calc PR 1 C42 C -0.1777(3) 0.5857(4) 0.1049(3) 0.091(2) Uani 0.60 d PG 1 H42A H -0.0854(3) 0.5914(6) 0.1180(5) 0.109 Uiso 0.60 calc PR 1 C43 C -0.2424(7) 0.5270(3) 0.1198(2) 0.073(2) Uani 0.60 d PG 1 H43A H -0.1943(11) 0.4925(4) 0.1431(3) 0.088 Uiso 0.60 calc PR 1 C44 C -0.3775(7) 0.5187(2) 0.1006(3) 0.078(2) Uani 0.60 d PG 1 H44A H -0.4217(11) 0.4786(2) 0.1108(4) 0.093 Uiso 0.60 calc PR 1 C45 C -0.4479(3) 0.5692(3) 0.0665(3) 0.0684(15) Uani 0.60 d PG 1 H45A H -0.5402(3) 0.5636(5) 0.0534(4) 0.082 Uiso 0.60 calc PR 1 C46 C -0.3832(6) 0.6280(2) 0.0516(2) 0.0574(14) Uani 0.60 d PG 1 C40' C -0.5044(25) 0.6525(11) 0.0230(13) 0.181(10) Uiso 0.40 d P 2 H40D H -0.4812(25) 0.6534(11) -0.0285(13) 0.271 Uiso 0.40 d PR 2 H40E H -0.4854(25) 0.6953(11) 0.0448(13) 0.271 Uiso 0.40 d PR 2 H40F H -0.6005(25) 0.6423(11) 0.0279(13) 0.271 Uiso 0.40 d PR 2 C41' C -0.3047(15) 0.6468(4) 0.0580(5) 0.074(3) Uiso 0.40 d PG 2 H41B H -0.3057(15) 0.6898(4) 0.0383(5) 0.088 Uiso 0.40 calc PR 2 C42' C -0.1866(10) 0.6217(5) 0.0887(5) 0.084(4) Uiso 0.40 d PG 2 H42B H -0.1070(14) 0.6476(9) 0.0900(8) 0.101 Uiso 0.40 calc PR 2 C43' C -0.1851(9) 0.5588(6) 0.1174(5) 0.078(4) Uiso 0.40 d PG 2 H43B H -0.1044(13) 0.5416(10) 0.1384(7) 0.093 Uiso 0.40 calc PR 2 C44' C -0.3017(15) 0.5209(3) 0.1155(7) 0.105(5) Uiso 0.40 d PG 2 H44B H -0.3007(25) 0.4779(4) 0.1351(10) 0.126 Uiso 0.40 calc PR 2 C45' C -0.4198(10) 0.5460(7) 0.0847(7) 0.105(5) Uiso 0.40 d PG 2 H45B H -0.4994(14) 0.5202(11) 0.0834(10) 0.126 Uiso 0.40 calc PR 2 C46' C -0.4212(9) 0.6089(8) 0.0560(5) 0.088(4) Uiso 0.40 d PG 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 Mg 0.0612(5) 0.0402(4) 0.0285(4) -0.0048(3) -0.0112(3) 0.0123(4) C1 0.0489(14) 0.0361(12) 0.0329(12) 0.0002(10) -0.0054(10) 0.0014(10) N1 0.0447(11) 0.0360(10) 0.0277(9) -0.0033(8) -0.0034(8) 0.0035(8) C2 0.064(2) 0.0407(13) 0.0265(11) -0.0010(10) -0.0130(11) 0.0035(12) C3 0.0529(14) 0.0375(13) 0.0268(11) -0.0025(9) -0.0009(10) -0.0030(11) N3 0.0475(11) 0.0332(10) 0.0288(10) -0.0004(8) -0.0015(8) 0.0027(8) C4 0.083(2) 0.0461(15) 0.0427(14) -0.0034(12) -0.0211(14) 0.0185(14) C5 0.089(2) 0.047(2) 0.0324(13) -0.0088(11) -0.0114(13) 0.0064(14) C6 0.0425(13) 0.0361(12) 0.0278(11) -0.0021(9) -0.0073(9) 0.0074(10) C7 0.0441(13) 0.0403(13) 0.0326(12) -0.0032(10) -0.0048(10) 0.0046(10) C8 0.054(2) 0.0452(14) 0.0455(14) -0.0118(11) -0.0057(12) -0.0018(12) C9 0.059(2) 0.061(2) 0.0403(13) -0.0192(12) -0.0018(12) 0.0077(14) C10 0.0493(15) 0.063(2) 0.0372(13) -0.0098(12) 0.0036(11) 0.0073(13) C11 0.0439(13) 0.0462(14) 0.0365(12) -0.0011(10) -0.0036(10) 0.0046(11) C12 0.0496(15) 0.0482(15) 0.0463(14) -0.0062(11) 0.0061(11) -0.0016(12) C13 0.048(2) 0.141(4) 0.090(3) 0.026(3) 0.008(2) 0.015(2) C14 0.089(2) 0.058(2) 0.064(2) 0.0037(15) 0.018(2) -0.006(2) C15 0.056(2) 0.056(2) 0.053(2) -0.0045(13) 0.0073(13) -0.0078(13) C16 0.054(2) 0.098(3) 0.134(4) -0.011(3) -0.009(2) -0.013(2) C17 0.113(3) 0.085(3) 0.106(3) 0.033(2) -0.007(3) -0.025(2) C18 0.0541(15) 0.0373(12) 0.0269(11) -0.0051(9) -0.0059(10) 0.0056(11) C19 0.066(2) 0.0374(13) 0.0350(12) -0.0024(10) -0.0045(11) 0.0004(12) C20 0.091(2) 0.0410(15) 0.0399(14) 0.0000(11) -0.0106(14) -0.0032(14) C21 0.092(2) 0.042(2) 0.060(2) -0.0016(13) -0.028(2) 0.015(2) C22 0.066(2) 0.053(2) 0.061(2) -0.0095(14) -0.0191(14) 0.0178(14) C23 0.055(2) 0.0483(15) 0.0388(13) -0.0073(11) -0.0107(11) 0.0096(12) C24 0.073(2) 0.047(2) 0.060(2) -0.0013(13) 0.0172(15) -0.0075(14) C25 0.114(3) 0.159(5) 0.067(2) -0.045(3) 0.030(2) -0.031(3) C26 0.070(2) 0.091(2) 0.062(2) -0.007(2) 0.005(2) -0.013(2) C27 0.053(2) 0.061(2) 0.067(2) -0.0091(15) 0.0040(14) 0.0042(14) C28 0.101(3) 0.110(3) 0.075(2) -0.014(2) 0.027(2) -0.004(2) C29 0.093(3) 0.116(3) 0.093(3) -0.029(3) 0.003(2) -0.037(3) C30 0.052(3) 0.055(3) 0.032(2) 0.002(2) -0.014(2) 0.005(3) C31 0.078(5) 0.098(5) 0.025(3) -0.017(3) -0.016(3) -0.003(4) C32 0.099(5) 0.078(4) 0.064(4) 0.030(3) -0.036(4) 0.009(4) C40 0.219(13) 0.076(5) 0.097(6) 0.014(4) -0.005(7) 0.034(7) C41 0.044(4) 0.109(5) 0.077(4) -0.042(4) 0.012(3) -0.013(4) C42 0.126(7) 0.077(6) 0.070(4) -0.023(4) 0.015(4) 0.001(4) C43 0.084(5) 0.089(5) 0.046(3) -0.016(3) -0.008(3) -0.001(4) C44 0.090(5) 0.086(4) 0.057(3) 0.007(3) 0.014(3) 0.010(4) C45 0.078(4) 0.047(3) 0.081(4) -0.003(3) 0.021(3) -0.018(3) C46 0.058(3) 0.057(3) 0.058(3) -0.014(2) 0.010(2) -0.026(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 Mg N1 2.017(2) . ? Mg N3 2.021(2) . ? Mg C30 2.120(4) . ? Mg C30' 2.122(8) . ? C1 N1 1.330(3) . ? C1 C2 1.406(3) . ? C1 C4 1.505(3) . ? N1 C6 1.439(3) . ? C2 C3 1.395(3) . ? C3 N3 1.331(3) . ? C3 C5 1.514(3) . ? N3 C18 1.438(3) . ? C6 C7 1.402(3) . ? C6 C11 1.407(3) . ? C7 C8 1.390(3) . ? C7 C12 1.522(3) . ? C8 C9 1.376(4) . ? C9 C10 1.370(4) . ? C10 C11 1.391(4) . ? C11 C15 1.517(4) . ? C12 C14 1.511(4) . ? C12 C13 1.517(4) . ? C15 C16 1.521(5) . ? C15 C17 1.530(5) . ? C18 C19 1.402(4) . ? C18 C23 1.404(4) . ? C19 C20 1.396(4) . ? C19 C24 1.516(4) . ? C20 C21 1.378(5) . ? C21 C22 1.370(5) . ? C22 C23 1.391(4) . ? C23 C27 1.510(4) . ? C24 C25 1.518(5) . ? C24 C26 1.523(4) . ? C27 C29 1.521(5) . ? C27 C28 1.524(4) . ? C30 C31 1.562(6) . ? C30 C32 1.577(6) . ? C30' C31' 1.568(7) . ? C30' C32' 1.571(7) . ? C40 C46 1.439(9) . ? C41 C42 1.39 . ? C41 C46 1.39 . ? C42 C43 1.39 . ? C43 C44 1.39 . ? C44 C45 1.39 . ? C45 C46 1.39 . ? C40' C46' 1.35(2) . ? C41' C42' 1.39 . ? C41' C46' 1.39 . ? C42' C43' 1.39 . ? C43' C44' 1.39 . ? C44' C45' 1.39 . ? C45' C46' 1.39 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Mg N3 93.38(8) . . ? N1 Mg C30 132.44(14) . . ? N3 Mg C30 133.50(14) . . ? N1 Mg C30' 130.6(2) . . ? N3 Mg C30' 133.6(2) . . ? N1 C1 C2 123.7(2) . . ? N1 C1 C4 119.6(2) . . ? C2 C1 C4 116.7(2) . . ? C1 N1 C6 119.8(2) . . ? C1 N1 Mg 124.7(2) . . ? C6 N1 Mg 115.51(13) . . ? C3 C2 C1 129.5(2) . . ? N3 C3 C2 124.3(2) . . ? N3 C3 C5 119.3(2) . . ? C2 C3 C5 116.4(2) . . ? C3 N3 C18 119.7(2) . . ? C3 N3 Mg 124.2(2) . . ? C18 N3 Mg 115.79(14) . . ? C7 C6 C11 121.0(2) . . ? C7 C6 N1 119.8(2) . . ? C11 C6 N1 118.9(2) . . ? C8 C7 C6 118.4(2) . . ? C8 C7 C12 119.9(2) . . ? C6 C7 C12 121.7(2) . . ? C9 C8 C7 121.0(2) . . ? C10 C9 C8 120.2(2) . . ? C9 C10 C11 121.5(2) . . ? C10 C11 C6 117.9(2) . . ? C10 C11 C15 120.1(2) . . ? C6 C11 C15 122.0(2) . . ? C14 C12 C13 111.1(3) . . ? C14 C12 C7 112.6(2) . . ? C13 C12 C7 110.7(2) . . ? C11 C15 C16 111.5(3) . . ? C11 C15 C17 111.0(3) . . ? C16 C15 C17 109.5(3) . . ? C19 C18 C23 121.1(2) . . ? C19 C18 N3 118.6(2) . . ? C23 C18 N3 120.1(2) . . ? C20 C19 C18 118.2(3) . . ? C20 C19 C24 120.1(3) . . ? C18 C19 C24 121.7(2) . . ? C21 C20 C19 121.1(3) . . ? C22 C21 C20 120.0(3) . . ? C21 C22 C23 121.6(3) . . ? C22 C23 C18 118.0(3) . . ? C22 C23 C27 119.9(3) . . ? C18 C23 C27 122.1(2) . . ? C19 C24 C25 111.7(3) . . ? C19 C24 C26 112.2(2) . . ? C25 C24 C26 110.1(3) . . ? C23 C27 C29 111.0(3) . . ? C23 C27 C28 113.0(3) . . ? C29 C27 C28 109.8(3) . . ? C31 C30 C32 106.8(5) . . ? C31 C30 Mg 112.5(4) . . ? C32 C30 Mg 111.6(4) . . ? C31' C30' C32' 103.7(6) . . ? C31' C30' Mg 112.4(6) . . ? C32' C30' Mg 115.0(6) . . ? C42 C41 C46 120.0 . . ? C41 C42 C43 120.0 . . ? C44 C43 C42 120.0 . . ? C45 C44 C43 120.0 . . ? C44 C45 C46 120.0 . . ? C45 C46 C41 120.0 . . ? C45 C46 C40 125.1(7) . . ? C41 C46 C40 114.9(7) . . ? C42' C41' C46' 120.0 . . ? C41' C42' C43' 120.0 . . ? C44' C43' C42' 120.0 . . ? C43' C44' C45' 120.0 . . ? C46' C45' C44' 120.0 . . ? C40' C46' C45' 141.6(16) . . ? C40' C46' C41' 98.4(16) . . ? C45' C46' C41' 120.0 . . ? _refine_diff_density_max 0.318 _refine_diff_density_min -0.205 _refine_diff_density_rms 0.039 #===END data_Compound_5 _database_code_CSD 207268 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C39 H56 N2 O Mg' _chemical_formula_weight 593.17 _chemical_melting_point ? _chemical_compound_source ? 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 Monoclinic _symmetry_space_group_name_H-M P2(1)/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' '-x, -y, -z' 'x, -y-1/2, z' _cell_length_a 9.3526(6) _cell_length_b 19.746(2) _cell_length_c 10.4848(6) _cell_angle_alpha 90.00 _cell_angle_beta 112.124(5) _cell_angle_gamma 90.00 _cell_volume 1793.7(2) _cell_formula_units_Z 2 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used 48 _cell_measurement_theta_min 11.12 _cell_measurement_theta_max 27.89 _exptl_crystal_description plates _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.47 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.098 _exptl_crystal_density_method ? _exptl_crystal_F_000 648 _exptl_absorpt_coefficient_mu 0.647 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 203(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 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2946 _diffrn_reflns_av_R_equivalents 0.0530 _diffrn_reflns_av_sigmaI/netI 0.0456 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 4.48 _diffrn_reflns_theta_max 59.98 _reflns_number_total 2752 _reflns_number_observed 2139 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 189 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0876P)^2^+0.4171P] 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 ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0015(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 2563 _refine_ls_number_parameters 224 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0760 _refine_ls_R_factor_obs 0.0567 _refine_ls_wR_factor_all 0.1604 _refine_ls_wR_factor_obs 0.1421 _refine_ls_goodness_of_fit_all 1.044 _refine_ls_goodness_of_fit_obs 1.083 _refine_ls_restrained_S_all 1.068 _refine_ls_restrained_S_obs 1.083 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Mg Mg 0.48312(11) 0.7500 0.30348(10) 0.0315(3) Uani 1 d S . N1 N 0.4770(2) 0.67338(10) 0.1678(2) 0.0333(4) Uani 1 d . . C1 C 0.5129(2) 0.68537(12) 0.0584(2) 0.0338(5) Uani 1 d . . C2 C 0.5389(4) 0.7500 0.0162(3) 0.0362(7) Uani 1 d S . H2A H 0.5811(4) 0.7500 -0.0522(3) 0.043 Uiso 1 calc SR . C3 C 0.5249(3) 0.62773(14) -0.0324(3) 0.0472(6) Uani 1 d . . H3A H 0.6284(3) 0.60902(14) 0.0048(3) 0.071 Uiso 1 d R . H3B H 0.5032(3) 0.64452(14) -0.1247(3) 0.071 Uiso 1 d R . H3C H 0.4509(3) 0.59275(14) -0.0353(3) 0.071 Uiso 1 d R . C4 C 0.4259(3) 0.60692(13) 0.1870(2) 0.0387(6) Uani 1 d . . C5 C 0.5301(3) 0.55543(14) 0.2553(3) 0.0488(6) Uani 1 d . . C6 C 0.4722(4) 0.4931(2) 0.2755(4) 0.0635(8) Uani 1 d . . H6A H 0.5412(4) 0.4586(2) 0.3222(4) 0.076 Uiso 1 calc R . C7 C 0.3155(5) 0.4811(2) 0.2283(4) 0.0712(10) Uani 1 d . . H7A H 0.2784(5) 0.4383(2) 0.2406(4) 0.085 Uiso 1 calc R . C8 C 0.2143(4) 0.5318(2) 0.1634(4) 0.0661(9) Uani 1 d . . H8A H 0.1077(4) 0.5234(2) 0.1333(4) 0.079 Uiso 1 calc R . C9 C 0.2647(3) 0.59533(14) 0.1406(3) 0.0498(7) Uani 1 d . . C10 C 0.7037(4) 0.5655(2) 0.3076(4) 0.0618(8) Uani 1 d . . H10A H 0.7234(4) 0.6114(2) 0.2798(4) 0.074 Uiso 1 calc R . C11 C 0.7751(6) 0.5618(3) 0.4640(5) 0.117(2) Uani 1 d . . H11A H 0.8858(6) 0.5683(3) 0.4948(5) 0.176 Uiso 1 calc R . H11B H 0.7541(6) 0.5178(3) 0.4941(5) 0.176 Uiso 1 calc R . H11C H 0.7311(6) 0.5969(3) 0.5028(5) 0.176 Uiso 1 calc R . C12 C 0.7824(4) 0.5145(2) 0.2459(5) 0.0757(10) Uani 1 d . . H12A H 0.8927(4) 0.5228(2) 0.2822(5) 0.113 Uiso 1 calc R . H12B H 0.7417(4) 0.5193(2) 0.1465(5) 0.113 Uiso 1 calc R . H12C H 0.7627(4) 0.4689(2) 0.2698(5) 0.113 Uiso 1 calc R . C13 C 0.1499(3) 0.6495(2) 0.0665(4) 0.0614(8) Uani 1 d . . H13A H 0.1996(3) 0.6940(2) 0.0982(4) 0.074 Uiso 1 calc R . C14 C 0.0027(4) 0.6471(2) 0.0977(5) 0.0839(12) Uani 1 d . . H14A H -0.0667(4) 0.6829(2) 0.0475(5) 0.126 Uiso 1 calc R . H14B H 0.0289(4) 0.6532(2) 0.1957(5) 0.126 Uiso 1 calc R . H14C H -0.0473(4) 0.6035(2) 0.0696(5) 0.126 Uiso 1 calc R . C15 C 0.1087(5) 0.6456(3) -0.0875(4) 0.0886(13) Uani 1 d . . H15A H 0.0349(5) 0.6809(3) -0.1328(4) 0.133 Uiso 1 calc R . H15B H 0.0637(5) 0.6017(3) -0.1210(4) 0.133 Uiso 1 calc R . H15C H 0.2011(5) 0.6517(3) -0.1073(4) 0.133 Uiso 1 calc R . C16 C 0.3381(3) 0.7500 0.4199(3) 0.0380(8) Uani 1 d S . C17 C 0.3052(3) 0.69050(15) 0.4763(3) 0.0443(6) Uani 1 d . . H17A H 0.3195(3) 0.64874(15) 0.4397(3) 0.053 Uiso 1 calc R . C18 C 0.2526(3) 0.6902(2) 0.5837(3) 0.0553(8) Uani 1 d . . H18A H 0.2324(3) 0.6488(2) 0.6180(3) 0.066 Uiso 1 calc R . C19 C 0.2300(4) 0.7500 0.6402(4) 0.0558(11) Uani 1 d S . H19A H 0.1995(4) 0.7500 0.7160(4) 0.067 Uiso 1 calc SR . O20 O 0.6960(3) 0.7334(2) 0.4697(3) 0.046(2) Uani 0.50 d P -1 C21 C 0.8528(5) 0.7385(10) 0.4767(5) 0.052(5) Uani 0.50 d P -1 H21A H 0.9099(5) 0.6979(10) 0.5218(5) 0.062 Uiso 0.50 calc PR -1 H21B H 0.9025(5) 0.7777(10) 0.5335(5) 0.062 Uiso 0.50 calc PR -1 C22 C 0.8619(5) 0.7457(27) 0.3406(5) 0.052(4) Uani 0.50 d P -1 H22A H 0.9692(5) 0.7488(27) 0.3510(5) 0.077 Uiso 1 calc SR -1 H22B H 0.8076(5) 0.7863(27) 0.2963(5) 0.077 Uiso 0.50 calc PR -1 H22C H 0.8149(5) 0.7065(27) 0.2845(5) 0.077 Uiso 0.50 calc PR -1 C23 C 0.6963(6) 0.7174(4) 0.6043(6) 0.057(2) Uani 0.50 d P -1 H23A H 0.7826(6) 0.6867(4) 0.6512(6) 0.069 Uiso 0.50 calc PR -1 H23B H 0.6006(6) 0.6935(4) 0.5932(6) 0.069 Uiso 0.50 calc PR -1 C24 C 0.7101(7) 0.7778(4) 0.6918(8) 0.073(2) Uani 0.50 d P -1 H24A H 0.7097(7) 0.7639(4) 0.7803(8) 0.110 Uiso 0.50 calc PR -1 H24B H 0.6237(7) 0.8080(4) 0.6471(8) 0.110 Uiso 0.50 calc PR -1 H24C H 0.8058(7) 0.8012(4) 0.7051(8) 0.110 Uiso 0.50 calc PR -1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mg 0.0247(5) 0.0447(6) 0.0276(5) 0.000 0.0127(4) 0.000 N1 0.0291(9) 0.0394(10) 0.0347(10) -0.0005(8) 0.0158(8) 0.0006(8) C1 0.0241(10) 0.0452(13) 0.0332(11) -0.0021(9) 0.0121(9) 0.0014(9) C2 0.030(2) 0.052(2) 0.032(2) 0.000 0.0172(13) 0.000 C3 0.0499(14) 0.0534(15) 0.0462(14) -0.0086(12) 0.0271(12) 0.0015(12) C4 0.0434(13) 0.0401(12) 0.0413(13) -0.0031(10) 0.0259(11) -0.0010(10) C5 0.057(2) 0.0432(14) 0.0509(15) 0.0009(11) 0.0262(13) 0.0031(12) C6 0.088(2) 0.043(2) 0.072(2) 0.0064(14) 0.044(2) 0.005(2) C7 0.093(3) 0.046(2) 0.102(3) 0.001(2) 0.067(2) -0.010(2) C8 0.063(2) 0.056(2) 0.101(3) -0.015(2) 0.054(2) -0.016(2) C9 0.0477(14) 0.0465(14) 0.069(2) -0.0118(13) 0.0371(14) -0.0079(12) C10 0.053(2) 0.050(2) 0.071(2) 0.0083(14) 0.0100(14) 0.0118(13) C11 0.102(4) 0.139(5) 0.074(3) -0.001(3) -0.010(2) 0.039(3) C12 0.058(2) 0.066(2) 0.109(3) 0.013(2) 0.040(2) 0.014(2) C13 0.0353(14) 0.056(2) 0.095(2) -0.013(2) 0.0265(15) -0.0074(12) C14 0.046(2) 0.108(3) 0.104(3) -0.024(2) 0.035(2) 0.006(2) C15 0.064(2) 0.115(3) 0.094(3) 0.030(3) 0.038(2) 0.021(2) C16 0.0237(15) 0.058(2) 0.033(2) 0.000 0.0115(13) 0.000 C17 0.0346(12) 0.0542(15) 0.0458(14) 0.0080(12) 0.0173(11) 0.0049(11) C18 0.0394(13) 0.077(2) 0.052(2) 0.0215(15) 0.0205(12) 0.0007(13) C19 0.034(2) 0.104(4) 0.035(2) 0.000 0.0187(15) 0.000 O20 0.0220(13) 0.079(5) 0.037(2) 0.004(2) 0.0103(11) -0.0022(15) C21 0.022(2) 0.081(14) 0.051(2) 0.002(3) 0.013(2) -0.002(3) C22 0.032(2) 0.070(12) 0.057(2) -0.013(10) 0.021(2) -0.014(10) C23 0.036(3) 0.101(4) 0.032(3) 0.015(3) 0.007(2) -0.001(3) C24 0.044(3) 0.130(7) 0.043(3) -0.016(3) 0.012(3) -0.001(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 Mg N1 2.063(2) . ? Mg N1 2.063(2) 4_575 ? Mg O20 2.120(3) . ? Mg O20 2.120(3) 4_575 ? Mg C16 2.139(3) . ? N1 C1 1.332(3) . ? N1 C4 1.437(3) . ? C1 C2 1.401(3) . ? C1 C3 1.515(3) . ? C2 C1 1.401(3) 4_575 ? C4 C5 1.404(4) . ? C4 C9 1.418(4) . ? C5 C6 1.393(4) . ? C5 C10 1.518(4) . ? C6 C7 1.379(5) . ? C7 C8 1.370(5) . ? C8 C9 1.392(4) . ? C9 C13 1.508(5) . ? C10 C11 1.522(5) . ? C10 C12 1.527(5) . ? C13 C15 1.514(5) . ? C13 C14 1.531(4) . ? C16 C17 1.401(3) . ? C16 C17 1.401(3) 4_575 ? C17 C18 1.389(4) . ? C18 C19 1.372(4) . ? C19 C18 1.372(4) 4_575 ? O20 C21 1.444(5) . ? O20 C23 1.445(7) . ? C21 C22 1.469(9) . ? C23 C24 1.481(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Mg N1 94.36(12) . 4_575 ? N1 Mg O20 103.13(12) . . ? N1 Mg O20 116.97(12) 4_575 . ? N1 Mg O20 116.97(12) . 4_575 ? N1 Mg O20 103.13(12) 4_575 4_575 ? O20 Mg O20 17.8(2) . 4_575 ? N1 Mg C16 122.32(7) . . ? N1 Mg C16 122.32(7) 4_575 . ? O20 Mg C16 97.59(12) . . ? O20 Mg C16 97.59(12) 4_575 . ? C1 N1 C4 119.2(2) . . ? C1 N1 Mg 120.9(2) . . ? C4 N1 Mg 119.82(14) . . ? N1 C1 C2 124.3(2) . . ? N1 C1 C3 120.6(2) . . ? C2 C1 C3 115.0(2) . . ? C1 C2 C1 131.2(3) 4_575 . ? C5 C4 C9 120.2(2) . . ? C5 C4 N1 122.0(2) . . ? C9 C4 N1 117.8(2) . . ? C6 C5 C4 118.8(3) . . ? C6 C5 C10 119.0(3) . . ? C4 C5 C10 122.2(2) . . ? C7 C6 C5 121.3(3) . . ? C8 C7 C6 119.6(3) . . ? C7 C8 C9 121.9(3) . . ? C8 C9 C4 118.1(3) . . ? C8 C9 C13 120.4(3) . . ? C4 C9 C13 121.4(2) . . ? C5 C10 C11 111.0(4) . . ? C5 C10 C12 112.4(3) . . ? C11 C10 C12 109.8(3) . . ? C9 C13 C15 111.0(3) . . ? C9 C13 C14 113.0(3) . . ? C15 C13 C14 109.8(3) . . ? C17 C16 C17 114.0(3) . 4_575 ? C17 C16 Mg 121.9(2) . . ? C17 C16 Mg 121.9(2) 4_575 . ? C18 C17 C16 123.2(3) . . ? C19 C18 C17 120.4(3) . . ? C18 C19 C18 118.7(3) 4_575 . ? C21 O20 C23 109.7(4) . . ? C21 O20 Mg 130.8(4) . . ? C23 O20 Mg 119.5(3) . . ? O20 C21 C22 112.7(4) . . ? O20 C23 C24 113.3(5) . . ? _refine_diff_density_max 0.309 _refine_diff_density_min -0.325 _refine_diff_density_rms 0.046 #===END data_Compound_6 _database_code_CSD 207269 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C35 H46 N2 Mg' _chemical_formula_weight 519.05 _chemical_melting_point ? _chemical_compound_source ? 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 Orthorhombic _symmetry_space_group_name_H-M Pnma loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z' '-x-1/2, y-1/2, z-1/2' _cell_length_a 16.8417(9) _cell_length_b 20.974(3) _cell_length_c 9.1888(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3245.9(6) _cell_formula_units_Z 4 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used 28 _cell_measurement_theta_min 10.58 _cell_measurement_theta_max 25.36 _exptl_crystal_description blocks _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.60 _exptl_crystal_size_min 0.47 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.062 _exptl_crystal_density_method ? _exptl_crystal_F_000 1128 _exptl_absorpt_coefficient_mu 0.633 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 183(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 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2776 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0224 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 0 _diffrn_reflns_theta_min 4.22 _diffrn_reflns_theta_max 64.00 _reflns_number_total 2776 _reflns_number_observed 2331 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 125 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0582P)^2^+1.2396P] 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 ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0029(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 2651 _refine_ls_number_parameters 179 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0595 _refine_ls_R_factor_obs 0.0445 _refine_ls_wR_factor_all 0.1284 _refine_ls_wR_factor_obs 0.1117 _refine_ls_goodness_of_fit_all 1.018 _refine_ls_goodness_of_fit_obs 1.049 _refine_ls_restrained_S_all 1.101 _refine_ls_restrained_S_obs 1.049 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Mg Mg 0.11499(5) 0.2500 0.11299(9) 0.0346(2) Uani 1 d S . N1 N 0.17578(8) 0.31971(6) 0.2110(2) 0.0308(3) Uani 1 d . . C1 C 0.23713(10) 0.31040(7) 0.2996(2) 0.0317(4) Uani 1 d . . C2 C 0.26741(14) 0.2500 0.3352(3) 0.0354(6) Uani 1 d S . H2A H 0.31492(14) 0.2500 0.3909(3) 0.043 Uiso 1 calc SR . C3 C 0.27620(11) 0.36688(8) 0.3716(2) 0.0430(5) Uani 1 d . . H3A H 0.32501(11) 0.35303(8) 0.4203(2) 0.064 Uiso 1 d R . H3B H 0.23987(11) 0.38534(8) 0.4435(2) 0.064 Uiso 1 d R . H3C H 0.28912(11) 0.39899(8) 0.2978(2) 0.064 Uiso 1 d R . C4 C 0.14341(10) 0.38286(7) 0.1910(2) 0.0325(4) Uani 1 d . . C5 C 0.17268(10) 0.42195(8) 0.0794(2) 0.0389(4) Uani 1 d . . C6 C 0.13416(13) 0.48005(9) 0.0543(3) 0.0515(5) Uani 1 d . . H6A H 0.15298(13) 0.50735(9) -0.0206(3) 0.062 Uiso 1 calc R . C7 C 0.06980(13) 0.49839(8) 0.1356(3) 0.0551(6) Uani 1 d . . H7A H 0.04449(13) 0.53802(8) 0.1167(3) 0.066 Uiso 1 calc R . C8 C 0.04194(12) 0.45936(9) 0.2445(3) 0.0509(5) Uani 1 d . . H8A H -0.00273(12) 0.47246(9) 0.3001(3) 0.061 Uiso 1 calc R . C9 C 0.07786(11) 0.40097(8) 0.2750(2) 0.0406(4) Uani 1 d . . C10 C 0.24101(12) 0.40137(9) -0.0170(2) 0.0469(5) Uani 1 d . . H10A H 0.26814(12) 0.36492(9) 0.0325(2) 0.056 Uiso 1 calc R . C11 C 0.2099(2) 0.3770(2) -0.1624(3) 0.0864(9) Uani 1 d . . H11A H 0.2547(2) 0.3638(2) -0.2236(3) 0.130 Uiso 1 calc R . H11B H 0.1803(2) 0.4110(2) -0.2113(3) 0.130 Uiso 1 calc R . H11C H 0.1748(2) 0.3404(2) -0.1458(3) 0.130 Uiso 1 calc R . C12 C 0.30273(14) 0.45370(11) -0.0391(3) 0.0776(8) Uani 1 d . . H12A H 0.34536(14) 0.43784(11) -0.1020(3) 0.116 Uiso 1 calc R . H12B H 0.32491(14) 0.46612(11) 0.0553(3) 0.116 Uiso 1 calc R . H12C H 0.27757(14) 0.49077(11) -0.0848(3) 0.116 Uiso 1 calc R . C13 C 0.04547(13) 0.35970(10) 0.3965(3) 0.0558(5) Uani 1 d . . H13A H 0.07907(13) 0.32049(10) 0.4030(3) 0.067 Uiso 1 calc R . C14 C -0.0396(2) 0.33915(13) 0.3685(3) 0.0778(8) Uani 1 d . . H14A H -0.0581(2) 0.31264(13) 0.4495(3) 0.117 Uiso 1 calc R . H14B H -0.0421(2) 0.31460(13) 0.2779(3) 0.117 Uiso 1 calc R . H14C H -0.0735(2) 0.37695(13) 0.3601(3) 0.117 Uiso 1 calc R . C15 C 0.0500(2) 0.3945(2) 0.5426(3) 0.0905(10) Uani 1 d . . H15A H 0.0288(2) 0.3670(2) 0.6195(3) 0.136 Uiso 1 calc R . H15B H 0.0187(2) 0.4338(2) 0.5376(3) 0.136 Uiso 1 calc R . H15C H 0.1055(2) 0.4050(2) 0.5642(3) 0.136 Uiso 1 calc R . C16 C 0.01778(14) 0.2500 -0.0292(3) 0.0368(6) Uani 1 d S . C17 C -0.01702(11) 0.30627(9) -0.0802(2) 0.0448(5) Uani 1 d . . H17A H 0.00404(11) 0.34588(9) -0.0483(2) 0.054 Uiso 1 calc R . C18 C -0.08071(12) 0.30683(10) -0.1752(2) 0.0523(5) Uani 1 d . . H18A H -0.10229(12) 0.34624(10) -0.2073(2) 0.063 Uiso 1 calc R . C19 C -0.1130(2) 0.2500 -0.2233(3) 0.0543(8) Uani 1 d S . H19A H -0.1567(2) 0.2500 -0.2886(3) 0.065 Uiso 1 calc SR . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mg 0.0367(4) 0.0187(4) 0.0485(5) 0.000 -0.0120(4) 0.000 N1 0.0325(7) 0.0161(6) 0.0437(8) 0.0006(5) -0.0033(6) 0.0014(5) C1 0.0334(8) 0.0211(8) 0.0408(9) -0.0010(6) -0.0031(7) -0.0018(6) C2 0.0345(12) 0.0237(11) 0.0481(14) 0.000 -0.0108(11) 0.000 C3 0.0471(10) 0.0237(8) 0.0582(12) -0.0055(8) -0.0140(9) -0.0030(7) C4 0.0343(8) 0.0170(7) 0.0462(9) -0.0025(7) -0.0090(7) 0.0014(6) C5 0.0413(9) 0.0223(8) 0.0530(11) 0.0033(7) -0.0083(8) -0.0009(7) C6 0.0579(12) 0.0265(9) 0.0701(14) 0.0098(9) -0.0125(11) 0.0006(8) C7 0.0590(12) 0.0233(9) 0.083(2) -0.0040(9) -0.0222(12) 0.0130(8) C8 0.0477(11) 0.0358(9) 0.0691(13) -0.0142(10) -0.0093(10) 0.0151(9) C9 0.0398(10) 0.0305(9) 0.0513(11) -0.0073(8) -0.0051(8) 0.0061(7) C10 0.0455(10) 0.0372(9) 0.0580(12) 0.0132(9) 0.0012(9) -0.0002(8) C11 0.068(2) 0.125(3) 0.066(2) -0.020(2) 0.0061(13) 0.010(2) C12 0.0573(14) 0.0558(14) 0.120(2) 0.0318(15) 0.0135(14) -0.0077(11) C13 0.0501(11) 0.0515(11) 0.0659(14) 0.0034(10) 0.0142(11) 0.0105(10) C14 0.075(2) 0.071(2) 0.087(2) -0.0141(14) 0.0117(15) -0.0213(14) C15 0.081(2) 0.131(3) 0.059(2) -0.001(2) 0.0031(14) -0.030(2) C16 0.0362(13) 0.0302(11) 0.0439(14) 0.000 -0.0053(11) 0.000 C17 0.0419(10) 0.0330(9) 0.0596(12) 0.0058(8) -0.0076(9) -0.0003(8) C18 0.0430(11) 0.0529(12) 0.0610(13) 0.0156(10) -0.0085(9) 0.0056(9) C19 0.0384(15) 0.075(2) 0.050(2) 0.000 -0.0120(13) 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mg N1 1.9992(14) . ? Mg N1 1.9992(14) 7_565 ? Mg C16 2.095(3) . ? N1 C1 1.330(2) . ? N1 C4 1.444(2) . ? C1 C2 1.404(2) . ? C1 C3 1.508(2) . ? C2 C1 1.404(2) 7_565 ? C4 C9 1.399(3) . ? C4 C5 1.403(2) . ? C5 C6 1.400(2) . ? C5 C10 1.515(3) . ? C6 C7 1.371(3) . ? C7 C8 1.375(3) . ? C8 C9 1.394(3) . ? C9 C13 1.514(3) . ? C10 C11 1.523(3) . ? C10 C12 1.525(3) . ? C13 C14 1.518(3) . ? C13 C15 1.530(3) . ? C16 C17 1.399(2) 7_565 ? C16 C17 1.399(2) . ? C17 C18 1.383(3) . ? C18 C19 1.383(3) . ? C19 C18 1.383(3) 7_565 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Mg N1 93.99(8) . 7_565 ? N1 Mg C16 132.94(4) . . ? N1 Mg C16 132.94(4) 7_565 . ? C1 N1 C4 120.38(13) . . ? C1 N1 Mg 124.49(10) . . ? C4 N1 Mg 114.85(10) . . ? N1 C1 C2 123.8(2) . . ? N1 C1 C3 119.49(14) . . ? C2 C1 C3 116.6(2) . . ? C1 C2 C1 128.9(2) 7_565 . ? C9 C4 C5 121.46(15) . . ? C9 C4 N1 118.5(2) . . ? C5 C4 N1 119.8(2) . . ? C6 C5 C4 117.8(2) . . ? C6 C5 C10 120.3(2) . . ? C4 C5 C10 121.87(15) . . ? C7 C6 C5 121.4(2) . . ? C6 C7 C8 119.9(2) . . ? C7 C8 C9 121.4(2) . . ? C8 C9 C4 118.0(2) . . ? C8 C9 C13 119.6(2) . . ? C4 C9 C13 122.4(2) . . ? C5 C10 C11 110.3(2) . . ? C5 C10 C12 113.0(2) . . ? C11 C10 C12 111.1(2) . . ? C9 C13 C14 112.2(2) . . ? C9 C13 C15 110.8(2) . . ? C14 C13 C15 109.4(2) . . ? C17 C16 C17 115.1(2) 7_565 . ? C17 C16 Mg 122.46(12) 7_565 . ? C17 C16 Mg 122.46(12) . . ? C18 C17 C16 122.9(2) . . ? C17 C18 C19 120.0(2) . . ? C18 C19 C18 119.1(3) . 7_565 ? _refine_diff_density_max 0.210 _refine_diff_density_min -0.221 _refine_diff_density_rms 0.034 #===END data_Compound_7a _database_code_CSD 207270 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C72 H114 N4 Cl2 Mg2' _chemical_formula_weight 1155.19 _chemical_melting_point ? _chemical_compound_source ? 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' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M I2/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z+1/2' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 12.2182(3) _cell_length_b 17.9539(10) _cell_length_c 16.4195(6) _cell_angle_alpha 90.00 _cell_angle_beta 97.653(2) _cell_angle_gamma 90.00 _cell_volume 3569.8(3) _cell_formula_units_Z 2 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used 22 _cell_measurement_theta_min 11.06 _cell_measurement_theta_max 24.91 _exptl_crystal_description prisms _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.075 _exptl_crystal_density_method ? _exptl_crystal_F_000 1264 _exptl_absorpt_coefficient_mu 1.285 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 183(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 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3183 _diffrn_reflns_av_R_equivalents 0.0361 _diffrn_reflns_av_sigmaI/netI 0.0301 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 3.67 _diffrn_reflns_theta_max 63.99 _reflns_number_total 3082 _reflns_number_observed 2560 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 158 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0691P)^2^+2.0001P] 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 ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00032(9) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 2924 _refine_ls_number_parameters 266 _refine_ls_number_restraints 112 _refine_ls_R_factor_all 0.0596 _refine_ls_R_factor_obs 0.0470 _refine_ls_wR_factor_all 0.1317 _refine_ls_wR_factor_obs 0.1174 _refine_ls_goodness_of_fit_all 1.073 _refine_ls_goodness_of_fit_obs 1.092 _refine_ls_restrained_S_all 1.109 _refine_ls_restrained_S_obs 1.094 _refine_ls_shift/esd_max -0.002 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Mg Mg 0.42999(6) 1.0000 0.58400(5) 0.0260(2) Uani 1 d S . Cl Cl 0.37997(5) 1.0000 0.43704(4) 0.0370(2) Uani 1 d S . N1 N 0.37264(12) 0.91702(8) 0.65095(9) 0.0281(3) Uani 1 d . . C1 C 0.29186(15) 0.92940(11) 0.69700(11) 0.0316(4) Uani 1 d . . C2 C 0.2511(2) 1.0000 0.7122(2) 0.0346(6) Uani 1 d S . H2A H 0.1850(2) 1.0000 0.7368(2) 0.041 Uiso 1 calc SR . C3 C 0.2404(2) 0.86553(12) 0.7386(2) 0.0466(5) Uani 1 d . . H3A H 0.2123(2) 0.88375(12) 0.7881(2) 0.070 Uiso 1 d R . H3B H 0.2962(2) 0.82702(12) 0.7538(2) 0.070 Uiso 1 d R . H3C H 0.1794(2) 0.84444(12) 0.7007(2) 0.070 Uiso 1 d R . C4 C 0.4167(2) 0.84234(10) 0.65167(12) 0.0322(4) Uani 1 d . . C5 C 0.3704(2) 0.79032(11) 0.59358(14) 0.0390(5) Uani 1 d . . C6 C 0.4151(2) 0.71845(12) 0.5974(2) 0.0516(6) Uani 1 d . . H6A H 0.3857(2) 0.68234(12) 0.5582(2) 0.062 Uiso 1 calc R . C7 C 0.5006(2) 0.69888(12) 0.6568(2) 0.0558(6) Uani 1 d . . H7A H 0.5288(2) 0.64949(12) 0.6588(2) 0.067 Uiso 1 calc R . C8 C 0.5455(2) 0.75083(13) 0.7132(2) 0.0522(6) Uani 1 d . . H8A H 0.6041(2) 0.73678(13) 0.7543(2) 0.063 Uiso 1 calc R . C9 C 0.5060(2) 0.82396(12) 0.71098(14) 0.0402(5) Uani 1 d . . C10 C 0.2727(2) 0.80883(13) 0.52922(15) 0.0487(5) Uani 1 d . . H10A H 0.2543(2) 0.86263(13) 0.53541(15) 0.058 Uiso 1 calc R . C11 C 0.2998(3) 0.7974(2) 0.4430(2) 0.0659(7) Uani 1 d . . H11A H 0.2351(3) 0.8099(2) 0.4033(2) 0.099 Uiso 1 calc R . H11B H 0.3202(3) 0.7453(2) 0.4358(2) 0.099 Uiso 1 calc R . H11C H 0.3616(3) 0.8298(2) 0.4338(2) 0.099 Uiso 1 calc R . C12 C 0.1695(2) 0.7627(2) 0.5416(2) 0.0769(9) Uani 1 d . . H12A H 0.1521(2) 0.7702(2) 0.5976(2) 0.115 Uiso 1 calc R . H12B H 0.1841(2) 0.7098(2) 0.5331(2) 0.115 Uiso 1 calc R . H12C H 0.1068(2) 0.7789(2) 0.5021(2) 0.115 Uiso 1 calc R . C13 C 0.5584(2) 0.88060(14) 0.7733(2) 0.0520(6) Uani 1 d . . H13A H 0.5291(2) 0.93075(14) 0.7552(2) 0.062 Uiso 1 calc R . C14 C 0.6830(2) 0.8837(2) 0.7775(2) 0.0743(9) Uani 1 d . . H14A H 0.7027(2) 0.8927(2) 0.7224(2) 0.111 Uiso 1 calc R . H14B H 0.7148(2) 0.8362(2) 0.7984(2) 0.111 Uiso 1 calc R . H14C H 0.7120(2) 0.9241(2) 0.8143(2) 0.111 Uiso 1 calc R . C15 C 0.5274(3) 0.8667(3) 0.8578(2) 0.108(2) Uani 1 d U . H15A H 0.4469(3) 0.8648(3) 0.8548(2) 0.162 Uiso 1 calc R . H15B H 0.5562(3) 0.9071(3) 0.8947(2) 0.162 Uiso 1 calc R . H15C H 0.5591(3) 0.8192(3) 0.8789(2) 0.162 Uiso 1 calc R . C21 C 0.7678(8) 0.5194(10) 0.4656(8) 0.095(6) Uani 0.25 d PGDU -1 H21A H 0.8120(9) 0.5137(14) 0.4203(9) 0.143 Uiso 0.25 d PG -1 H21B H 0.7972(7) 0.4868(15) 0.5112(11) 0.143 Uiso 0.25 d PG -1 H21C H 0.7711(10) 0.5713(11) 0.4842(15) 0.143 Uiso 0.25 d PG -1 C22 C 0.6515(8) 0.4989(10) 0.4368(8) 0.096(6) Uani 0.50 d SPGDU -1 H22A H 0.6494(11) 0.4481(14) 0.4131(17) 0.115 Uiso 0.25 d PG -1 H22B H 0.6210(9) 0.5337(17) 0.3928(8) 0.115 Uiso 0.25 d PG -1 C23 C 0.5800(7) 0.5011(8) 0.5057(6) 0.093(6) Uani 0.50 d SPGDU -1 H23A H 0.6046(8) 0.4618(15) 0.5463(13) 0.111 Uiso 0.25 d PG -1 H23B H 0.5896(8) 0.5498(12) 0.5339(11) 0.111 Uiso 0.25 d PG -1 C24 C 0.4631(7) 0.4901(6) 0.4754(7) 0.094(6) Uani 0.25 d PGDU -1 H24A H 0.4549(10) 0.4404(10) 0.4491(17) 0.113 Uiso 0.25 d PG -1 H24B H 0.4415(8) 0.5275(13) 0.4319(7) 0.113 Uiso 0.25 d PG -1 C25 C 0.3822(6) 0.4910(11) 0.5373(6) 0.070(6) Uani 0.25 d PGDU -1 H25A H 0.3785(8) 0.4460(15) 0.5643(15) 0.085 Uiso 0.25 d PG -1 H25B H 0.4099(7) 0.5317(18) 0.5800(8) 0.085 Uiso 0.25 d PG -1 C26 C 0.2676(7) 0.5173(10) 0.4999(6) 0.082(6) Uani 0.25 d PGDU -1 H26A H 0.2496(7) 0.4930(15) 0.4457(5) 0.099 Uiso 0.25 d PG -1 H26B H 0.2651(10) 0.5719(10) 0.4913(17) 0.099 Uiso 0.25 d PG -1 C27 C 0.1836(6) 0.4957(15) 0.5540(6) 0.101(5) Uani 0.25 d PGDU -1 H27A H 0.1093(6) 0.5019(14) 0.5239(6) 0.152 Uiso 0.50 d SPG -1 H27B H 0.1918(8) 0.5274(21) 0.6030(8) 0.152 Uiso 0.25 d PG -1 H27C H 0.1946(8) 0.4435(17) 0.5705(15) 0.152 Uiso 0.25 d PG -1 C31 C 0.4251(36) 0.5048(31) 1.2193(20) 0.095(10) Uani 0.25 d PDU -1 H31A H 0.4085(36) 0.4702(31) 1.2621(20) 0.143 Uiso 0.25 calc PR -1 H31B H 0.3630(36) 0.5392(31) 1.2058(20) 0.143 Uiso 0.25 calc PR -1 H31C H 0.4919(36) 0.5332(31) 1.2392(20) 0.143 Uiso 0.25 calc PR -1 C32 C 0.4433(21) 0.4623(13) 1.1449(15) 0.062(4) Uani 0.25 d PDU -1 H32A H 0.3763(21) 0.4329(13) 1.1259(15) 0.074 Uiso 0.25 calc PR -1 H32B H 0.5050(21) 0.4270(13) 1.1594(15) 0.074 Uiso 0.25 calc PR -1 C33 C 0.4691(13) 0.5106(16) 1.0766(11) 0.067(6) Uani 0.25 d PDU -1 H33A H 0.4012(13) 0.5373(16) 1.0532(11) 0.081 Uiso 0.25 calc PR -1 H33B H 0.5241(13) 0.5484(16) 1.0987(11) 0.081 Uiso 0.25 calc PR -1 C34 C 0.5127(28) 0.4689(7) 1.0103(16) 0.097(7) Uani 0.25 d PDU -1 H34A H 0.4574(28) 0.4315(7) 0.9874(16) 0.116 Uiso 0.25 calc PR -1 H34B H 0.5803(28) 0.4419(7) 1.0336(16) 0.116 Uiso 0.25 calc PR -1 C35 C 0.5390(27) 0.5184(20) 0.9429(16) 0.143(13) Uani 0.25 d PDU -1 H35A H 0.6050(27) 0.5489(20) 0.9617(16) 0.171 Uiso 0.25 calc PR -1 H35B H 0.4762(27) 0.5522(20) 0.9254(16) 0.171 Uiso 0.25 calc PR -1 C36 C 0.5604(37) 0.4693(21) 0.8728(18) 0.118(15) Uani 0.25 d PDU -1 H36A H 0.6265(37) 0.4381(21) 0.8891(18) 0.142 Uiso 0.25 calc PR -1 H36B H 0.4965(37) 0.4360(21) 0.8569(18) 0.142 Uiso 0.25 calc PR -1 C37 C 0.5785(41) 0.5184(26) 0.8025(20) 0.108(13) Uani 0.25 d PDU -1 H37A H 0.5928(41) 0.4876(26) 0.7557(20) 0.162 Uiso 0.25 calc PR -1 H37B H 0.6421(41) 0.5509(26) 0.8188(20) 0.162 Uiso 0.25 calc PR -1 H37C H 0.5126(41) 0.5489(26) 0.7867(20) 0.162 Uiso 0.25 calc PR -1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mg 0.0280(4) 0.0211(4) 0.0302(4) 0.000 0.0086(3) 0.000 Cl 0.0271(3) 0.0507(4) 0.0335(3) 0.000 0.0047(2) 0.000 N1 0.0300(7) 0.0207(7) 0.0343(8) 0.0002(6) 0.0067(6) 0.0014(6) C1 0.0292(9) 0.0297(10) 0.0366(9) 0.0028(7) 0.0071(7) -0.0030(7) C2 0.0276(13) 0.0344(14) 0.0443(15) 0.000 0.0143(11) 0.000 C3 0.0460(11) 0.0365(11) 0.0616(14) 0.0076(10) 0.0236(10) -0.0051(9) C4 0.0344(9) 0.0210(8) 0.0429(10) 0.0047(7) 0.0116(8) -0.0003(7) C5 0.0403(10) 0.0260(9) 0.0523(12) -0.0025(8) 0.0122(9) -0.0038(8) C6 0.0588(14) 0.0254(10) 0.073(2) -0.0069(10) 0.0186(12) -0.0043(10) C7 0.0594(14) 0.0252(10) 0.086(2) 0.0081(11) 0.0205(13) 0.0085(10) C8 0.0519(13) 0.0360(12) 0.069(2) 0.0134(11) 0.0095(11) 0.0120(10) C9 0.0408(10) 0.0308(10) 0.0491(12) 0.0083(9) 0.0064(9) 0.0041(8) C10 0.0485(12) 0.0396(11) 0.0568(14) -0.0115(10) 0.0030(10) -0.0061(10) C11 0.071(2) 0.068(2) 0.059(2) -0.0105(13) 0.0096(13) -0.0109(14) C12 0.0476(15) 0.100(3) 0.083(2) -0.015(2) 0.0084(13) -0.022(2) C13 0.0518(13) 0.0431(13) 0.0564(14) 0.0020(10) -0.0105(10) 0.0092(10) C14 0.062(2) 0.085(2) 0.075(2) -0.009(2) 0.0058(14) -0.022(2) C15 0.081(2) 0.174(5) 0.072(2) -0.046(3) 0.021(2) -0.035(3) C21 0.121(14) 0.065(13) 0.107(13) 0.011(10) 0.038(11) 0.006(9) C22 0.114(10) 0.071(10) 0.102(10) -0.046(13) 0.019(8) -0.040(13) C23 0.111(11) 0.078(10) 0.088(9) -0.008(18) 0.013(9) -0.034(17) C24 0.114(12) 0.079(12) 0.085(8) -0.009(9) 0.001(8) -0.023(11) C25 0.107(10) 0.012(10) 0.090(10) -0.006(7) 0.006(8) 0.002(7) C26 0.115(11) 0.072(14) 0.057(6) -0.006(7) -0.001(7) -0.002(8) C27 0.133(12) 0.100(12) 0.066(7) -0.004(22) -0.001(8) 0.009(28) C31 0.064(14) 0.116(22) 0.111(14) 0.020(26) 0.027(13) 0.017(21) C32 0.046(8) 0.068(9) 0.070(9) 0.003(8) 0.001(7) -0.008(7) C33 0.046(5) 0.073(16) 0.079(9) 0.002(9) -0.009(6) -0.009(8) C34 0.112(14) 0.073(6) 0.105(14) 0.009(9) 0.012(12) 0.041(11) C35 0.139(18) 0.170(24) 0.132(17) -0.021(16) 0.065(14) 0.007(16) C36 0.091(16) 0.135(23) 0.121(20) -0.025(15) -0.012(13) -0.008(13) C37 0.072(16) 0.107(25) 0.138(25) 0.033(23) -0.011(18) 0.000(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mg N1 2.031(2) . ? Mg N1 2.031(2) 6_575 ? Mg Cl 2.3926(10) 5_676 ? Mg Cl 2.4091(10) . ? Mg Mg 3.434(2) 5_676 ? Cl Mg 2.3926(10) 5_676 ? N1 C1 1.339(2) . ? N1 C4 1.444(2) . ? C1 C2 1.397(2) . ? C1 C3 1.513(3) . ? C2 C1 1.397(2) 6_575 ? C4 C5 1.400(3) . ? C4 C9 1.402(3) . ? C5 C6 1.399(3) . ? C5 C10 1.522(3) . ? C6 C7 1.376(4) . ? C7 C8 1.376(4) . ? C8 C9 1.397(3) . ? C9 C13 1.522(3) . ? C10 C11 1.511(4) . ? C10 C12 1.544(4) . ? C13 C15 1.507(4) . ? C13 C14 1.515(4) . ? C21 C22 1.48 . ? C22 C23 1.52 . ? C23 C24 1.46 . ? C24 C25 1.51 . ? C25 C26 1.53 . ? C26 C27 1.50 . ? C31 C32 1.48(2) . ? C32 C33 1.48(2) . ? C33 C34 1.48(2) . ? C34 C35 1.49(2) . ? C35 C36 1.50(2) . ? C36 C37 1.49(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 N1 Mg N1 94.38(9) . 6_575 ? N1 Mg Cl 119.32(5) . 5_676 ? N1 Mg Cl 119.32(5) 6_575 5_676 ? N1 Mg Cl 118.84(5) . . ? N1 Mg Cl 118.84(5) 6_575 . ? Cl Mg Cl 88.68(3) 5_676 . ? N1 Mg Mg 132.81(4) . 5_676 ? N1 Mg Mg 132.81(4) 6_575 5_676 ? Cl Mg Mg 44.54(2) 5_676 5_676 ? Cl Mg Mg 44.15(2) . 5_676 ? Mg Cl Mg 91.32(3) 5_676 . ? C1 N1 C4 116.82(15) . . ? C1 N1 Mg 121.14(12) . . ? C4 N1 Mg 122.04(11) . . ? N1 C1 C2 124.0(2) . . ? N1 C1 C3 120.7(2) . . ? C2 C1 C3 115.3(2) . . ? C1 C2 C1 130.4(2) . 6_575 ? C5 C4 C9 121.5(2) . . ? C5 C4 N1 119.8(2) . . ? C9 C4 N1 118.6(2) . . ? C6 C5 C4 117.7(2) . . ? C6 C5 C10 119.9(2) . . ? C4 C5 C10 122.4(2) . . ? C7 C6 C5 121.5(2) . . ? C8 C7 C6 120.0(2) . . ? C7 C8 C9 121.0(2) . . ? C8 C9 C4 118.2(2) . . ? C8 C9 C13 119.8(2) . . ? C4 C9 C13 121.9(2) . . ? C11 C10 C5 111.8(2) . . ? C11 C10 C12 109.6(2) . . ? C5 C10 C12 111.7(2) . . ? C15 C13 C14 109.8(2) . . ? C15 C13 C9 112.0(2) . . ? C14 C13 C9 112.6(2) . . ? C21 C22 C23 112.2 . . ? C24 C23 C22 112.1 . . ? C23 C24 C25 117.8 . . ? C24 C25 C26 112.4 . . ? C27 C26 C25 110.3 . . ? C31 C32 C33 113.1(22) . . ? C34 C33 C32 113.2(21) . . ? C33 C34 C35 112.3(14) . . ? C34 C35 C36 107.2(22) . . ? C37 C36 C35 107.8(22) . . ? _refine_diff_density_max 0.373 _refine_diff_density_min -0.237 _refine_diff_density_rms 0.045 #===END data_Compound_7b _database_code_CSD 207271 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C58 H82 N4 Cl2 Mg2' _chemical_formula_weight 954.80 _chemical_melting_point ? _chemical_compound_source ? 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' Cl Cl 0.3639 0.7018 '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 C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 22.889(3) _cell_length_b 14.9573(5) _cell_length_c 16.3492(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.270(7) _cell_angle_gamma 90.00 _cell_volume 5597.2(8) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 26 _cell_measurement_theta_min 10.85 _cell_measurement_theta_max 27.99 _exptl_crystal_description rhombs _exptl_crystal_colour Clear _exptl_crystal_size_max 0.70 _exptl_crystal_size_mid 0.57 _exptl_crystal_size_min 0.57 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.133 _exptl_crystal_density_method ? _exptl_crystal_F_000 2064 _exptl_absorpt_coefficient_mu 1.548 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4275 _diffrn_reflns_av_R_equivalents 0.0576 _diffrn_reflns_av_sigmaI/netI 0.0256 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.53 _diffrn_reflns_theta_max 60.00 _reflns_number_total 4157 _reflns_number_observed 3617 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 138 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.1307P)^2^+4.9971P] 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 ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00115(14) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4019 _refine_ls_number_parameters 299 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0725 _refine_ls_R_factor_obs 0.0648 _refine_ls_wR_factor_all 0.1900 _refine_ls_wR_factor_obs 0.1767 _refine_ls_goodness_of_fit_all 1.064 _refine_ls_goodness_of_fit_obs 1.095 _refine_ls_restrained_S_all 1.094 _refine_ls_restrained_S_obs 1.095 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Mg Mg 0.19528(4) 0.17354(6) 0.00036(5) 0.0241(3) Uani 1 d . . Cl Cl 0.22657(3) 0.28932(5) 0.09045(4) 0.0352(3) Uani 1 d . . N2 N 0.19204(10) 0.0458(2) 0.04255(13) 0.0263(5) Uani 1 d . . C3 C 0.15267(12) -0.0106(2) 0.0119(2) 0.0276(6) Uani 1 d . . C4 C 0.10613(12) 0.0146(2) -0.0397(2) 0.0296(6) Uani 1 d . . H4A H 0.08652(12) -0.0337(2) -0.0658(2) 0.036 Uiso 1 calc R . C5 C 0.08429(12) 0.0989(2) -0.0586(2) 0.0270(6) Uani 1 d . . N6 N 0.11182(10) 0.17587(15) -0.04252(14) 0.0257(5) Uani 1 d . . C7 C 0.15532(14) -0.1093(2) 0.0319(2) 0.0383(7) Uani 1 d . . H7A H 0.18229(14) -0.1391(2) -0.0057(2) 0.057 Uiso 1 d R . H7B H 0.11628(14) -0.1355(2) 0.0260(2) 0.057 Uiso 1 d R . H7C H 0.16911(14) -0.1173(2) 0.0882(2) 0.057 Uiso 1 d R . C8 C 0.02498(13) 0.0998(2) -0.0999(2) 0.0377(7) Uani 1 d . . H8A H 0.00722(13) 0.0404(2) -0.0958(2) 0.057 Uiso 1 d R . H8B H 0.02951(13) 0.1158(2) -0.1576(2) 0.057 Uiso 1 d R . H8C H -0.00018(13) 0.1438(2) -0.0730(2) 0.057 Uiso 1 d R . C9 C 0.22984(12) 0.0122(2) 0.1061(2) 0.0284(6) Uani 1 d . . C10 C 0.21280(14) 0.0264(2) 0.1877(2) 0.0347(7) Uani 1 d . . C11 C 0.2465(2) -0.0130(3) 0.2498(2) 0.0475(9) Uani 1 d . . H11A H 0.2352(2) -0.0060(3) 0.3053(2) 0.057 Uiso 1 calc R . C12 C 0.2959(2) -0.0619(3) 0.2313(2) 0.0533(9) Uani 1 d . . H12A H 0.3178(2) -0.0895(3) 0.2739(2) 0.064 Uiso 1 calc R . C13 C 0.31353(15) -0.0707(2) 0.1515(2) 0.0454(8) Uani 1 d . . H13A H 0.34871(15) -0.1018(2) 0.1399(2) 0.054 Uiso 1 calc R . C14 C 0.28072(13) -0.0348(2) 0.0872(2) 0.0325(7) Uani 1 d . . C15 C 0.15897(14) 0.0806(2) 0.2089(2) 0.0400(8) Uani 1 d . . H15A H 0.15017(14) 0.1201(2) 0.1611(2) 0.048 Uiso 1 calc R . C16 C 0.1676(2) 0.1412(3) 0.2833(2) 0.0586(10) Uani 1 d . . H16A H 0.1315(2) 0.1743(3) 0.2939(2) 0.088 Uiso 1 calc R . H16B H 0.1994(2) 0.1835(3) 0.2726(2) 0.088 Uiso 1 calc R . H16C H 0.1775(2) 0.1047(3) 0.3312(2) 0.088 Uiso 1 calc R . C17 C 0.1062(2) 0.0203(3) 0.2214(3) 0.0611(11) Uani 1 d . . H17A H 0.0721(2) 0.0569(3) 0.2350(3) 0.092 Uiso 1 calc R . H17B H 0.1142(2) -0.0216(3) 0.2661(3) 0.092 Uiso 1 calc R . H17C H 0.0983(2) -0.0132(3) 0.1710(3) 0.092 Uiso 1 calc R . C18 C 0.30140(13) -0.0481(2) -0.0005(2) 0.0366(7) Uani 1 d . . H18A H 0.26980(13) -0.0267(2) -0.0382(2) 0.044 Uiso 1 calc R . C19 C 0.3138(2) -0.1463(3) -0.0205(3) 0.0654(11) Uani 1 d . . H19A H 0.2788(2) -0.1821(3) -0.0100(3) 0.098 Uiso 1 calc R . H19B H 0.3460(2) -0.1679(3) 0.0140(3) 0.098 Uiso 1 calc R . H19C H 0.3247(2) -0.1518(3) -0.0782(3) 0.098 Uiso 1 calc R . C20 C 0.3559(2) 0.0070(3) -0.0168(2) 0.0503(9) Uani 1 d . . H20A H 0.3685(2) -0.0024(3) -0.0734(2) 0.075 Uiso 1 calc R . H20B H 0.3871(2) -0.0116(3) 0.0207(2) 0.075 Uiso 1 calc R . H20C H 0.3472(2) 0.0705(3) -0.0083(2) 0.075 Uiso 1 calc R . C21 C 0.07983(12) 0.2572(2) -0.0586(2) 0.0273(6) Uani 1 d . . C22 C 0.08284(13) 0.2978(2) -0.1359(2) 0.0316(7) Uani 1 d . . C23 C 0.04933(15) 0.3742(2) -0.1500(2) 0.0395(7) Uani 1 d . . H23A H 0.05129(15) 0.4031(2) -0.2016(2) 0.047 Uiso 1 calc R . C24 C 0.01361(15) 0.4083(2) -0.0906(2) 0.0424(8) Uani 1 d . . H24A H -0.00985(15) 0.4593(2) -0.1020(2) 0.051 Uiso 1 calc R . C25 C 0.01165(14) 0.3689(2) -0.0145(2) 0.0406(8) Uani 1 d . . H25A H -0.01328(14) 0.3931(2) 0.0262(2) 0.049 Uiso 1 calc R . C26 C 0.04567(13) 0.2942(2) 0.0038(2) 0.0323(7) Uani 1 d . . C27 C 0.12050(13) 0.2603(2) -0.2040(2) 0.0355(7) Uani 1 d . . H27A H 0.13978(13) 0.2048(2) -0.1831(2) 0.043 Uiso 1 calc R . C28 C 0.0847(2) 0.2352(3) -0.2799(2) 0.0528(9) Uani 1 d . . H28A H 0.1108(2) 0.2115(3) -0.3221(2) 0.079 Uiso 1 calc R . H28B H 0.0647(2) 0.2884(3) -0.3010(2) 0.079 Uiso 1 calc R . H28C H 0.0558(2) 0.1897(3) -0.2654(2) 0.079 Uiso 1 calc R . C29 C 0.1682(2) 0.3262(3) -0.2270(2) 0.0566(10) Uani 1 d . . H29A H 0.1920(2) 0.3009(3) -0.2709(2) 0.085 Uiso 1 calc R . H29B H 0.1929(2) 0.3380(3) -0.1791(2) 0.085 Uiso 1 calc R . H29C H 0.1503(2) 0.3822(3) -0.2457(2) 0.085 Uiso 1 calc R . C30 C 0.0436(2) 0.2536(2) 0.0890(2) 0.0422(8) Uani 1 d . . H30A H 0.0739(2) 0.2054(2) 0.0916(2) 0.051 Uiso 1 calc R . C31 C 0.0581(2) 0.3208(3) 0.1546(2) 0.0681(13) Uani 1 d . . H31A H 0.0960(2) 0.3483(3) 0.1430(2) 0.102 Uiso 1 calc R . H31B H 0.0598(2) 0.2907(3) 0.2078(2) 0.102 Uiso 1 calc R . H31C H 0.0278(2) 0.3671(3) 0.1558(2) 0.102 Uiso 1 calc R . C32 C -0.0149(3) 0.2112(4) 0.1070(3) 0.097(2) Uani 1 d . . H32A H -0.0242(3) 0.1674(4) 0.0643(3) 0.145 Uiso 1 calc R . H32B H -0.0451(3) 0.2575(4) 0.1081(3) 0.145 Uiso 1 calc R . H32C H -0.0131(3) 0.1810(4) 0.1602(3) 0.145 Uiso 1 calc R . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mg 0.0250(5) 0.0258(5) 0.0213(5) 0.0006(3) 0.0033(3) -0.0028(4) Cl 0.0384(4) 0.0417(5) 0.0256(4) -0.0101(3) 0.0128(3) -0.0116(3) N2 0.0288(12) 0.0266(12) 0.0237(12) 0.0024(9) 0.0044(9) -0.0021(9) C3 0.0318(15) 0.0292(15) 0.0219(14) 0.0000(11) 0.0054(11) -0.0029(11) C4 0.0322(15) 0.0294(15) 0.0272(14) -0.0038(11) 0.0038(11) -0.0059(12) C5 0.0270(14) 0.035(2) 0.0193(13) -0.0021(11) 0.0042(10) -0.0044(12) N6 0.0256(12) 0.0274(13) 0.0241(12) 0.0000(9) 0.0043(9) -0.0015(9) C7 0.046(2) 0.031(2) 0.037(2) 0.0036(13) -0.0011(13) -0.0064(14) C8 0.032(2) 0.038(2) 0.043(2) -0.0036(14) -0.0053(13) -0.0028(13) C9 0.0335(15) 0.0294(15) 0.0224(14) 0.0053(11) -0.0015(11) -0.0039(12) C10 0.040(2) 0.040(2) 0.0247(15) 0.0054(12) 0.0030(12) -0.0062(13) C11 0.059(2) 0.059(2) 0.025(2) 0.0128(15) 0.0002(14) -0.004(2) C12 0.059(2) 0.058(2) 0.042(2) 0.020(2) -0.012(2) 0.003(2) C13 0.042(2) 0.047(2) 0.048(2) 0.011(2) -0.0065(15) 0.0061(15) C14 0.037(2) 0.030(2) 0.030(2) 0.0040(12) 0.0007(12) 0.0003(12) C15 0.047(2) 0.053(2) 0.0201(14) 0.0038(13) 0.0095(12) -0.002(2) C16 0.056(2) 0.072(3) 0.047(2) -0.016(2) 0.015(2) -0.009(2) C17 0.047(2) 0.078(3) 0.059(2) -0.013(2) 0.012(2) -0.013(2) C18 0.036(2) 0.039(2) 0.035(2) -0.0011(13) 0.0046(13) 0.0024(13) C19 0.073(3) 0.047(2) 0.076(3) -0.019(2) 0.016(2) 0.002(2) C20 0.045(2) 0.052(2) 0.054(2) 0.004(2) 0.015(2) -0.002(2) C21 0.0266(14) 0.0262(14) 0.0292(15) -0.0050(11) 0.0006(11) -0.0017(11) C22 0.033(2) 0.033(2) 0.029(2) -0.0036(12) -0.0005(12) -0.0008(12) C23 0.048(2) 0.034(2) 0.036(2) -0.0005(13) -0.0078(14) 0.0028(14) C24 0.047(2) 0.033(2) 0.047(2) -0.0082(14) -0.0107(15) 0.0110(14) C25 0.037(2) 0.040(2) 0.045(2) -0.0142(14) 0.0026(14) 0.0059(14) C26 0.032(2) 0.033(2) 0.033(2) -0.0057(12) 0.0059(12) -0.0004(12) C27 0.039(2) 0.042(2) 0.026(2) 0.0019(13) 0.0031(13) 0.0041(14) C28 0.050(2) 0.072(3) 0.036(2) -0.017(2) 0.000(2) 0.005(2) C29 0.053(2) 0.076(3) 0.040(2) 0.006(2) 0.006(2) -0.015(2) C30 0.047(2) 0.046(2) 0.034(2) -0.0020(14) 0.0150(14) 0.0070(15) C31 0.082(3) 0.093(3) 0.030(2) 0.003(2) 0.002(2) -0.039(3) C32 0.121(4) 0.118(4) 0.051(3) 0.003(3) 0.013(3) -0.077(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mg N6 2.032(2) . ? Mg N2 2.033(2) . ? Mg Cl 2.3815(11) . ? Mg Cl 2.3952(11) 7 ? Mg Mg 3.392(2) 7 ? Cl Mg 2.3952(11) 7 ? N2 C3 1.330(4) . ? N2 C9 1.440(4) . ? C3 C4 1.407(4) . ? C3 C7 1.513(4) . ? C4 C5 1.392(4) . ? C5 N6 1.337(4) . ? C5 C8 1.513(4) . ? N6 C21 1.444(4) . ? C9 C14 1.396(4) . ? C9 C10 1.408(4) . ? C10 C11 1.401(5) . ? C10 C15 1.517(5) . ? C11 C12 1.382(5) . ? C12 C13 1.372(5) . ? C13 C14 1.396(4) . ? C14 C18 1.526(4) . ? C15 C17 1.522(5) . ? C15 C16 1.528(5) . ? C18 C20 1.519(5) . ? C18 C19 1.532(5) . ? C21 C26 1.402(4) . ? C21 C22 1.404(4) . ? C22 C23 1.395(4) . ? C22 C27 1.518(4) . ? C23 C24 1.370(5) . ? C24 C25 1.378(5) . ? C25 C26 1.394(5) . ? C26 C30 1.521(4) . ? C27 C29 1.518(5) . ? C27 C28 1.531(4) . ? C30 C31 1.505(5) . ? C30 C32 1.512(6) . ? 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 N6 Mg N2 95.59(9) . . ? N6 Mg Cl 118.70(8) . . ? N2 Mg Cl 119.01(8) . . ? N6 Mg Cl 119.06(8) . 7 ? N2 Mg Cl 117.19(7) . 7 ? Cl Mg Cl 89.51(4) . 7 ? N6 Mg Mg 132.86(8) . 7 ? N2 Mg Mg 131.54(8) . 7 ? Cl Mg Mg 44.92(3) . 7 ? Cl Mg Mg 44.59(3) 7 7 ? Mg Cl Mg 90.49(4) . 7 ? C3 N2 C9 117.0(2) . . ? C3 N2 Mg 119.6(2) . . ? C9 N2 Mg 123.4(2) . . ? N2 C3 C4 124.5(3) . . ? N2 C3 C7 120.7(3) . . ? C4 C3 C7 114.8(2) . . ? C5 C4 C3 130.2(3) . . ? N6 C5 C4 124.6(2) . . ? N6 C5 C8 120.1(3) . . ? C4 C5 C8 115.3(2) . . ? C5 N6 C21 116.8(2) . . ? C5 N6 Mg 119.6(2) . . ? C21 N6 Mg 123.5(2) . . ? C14 C9 C10 121.4(3) . . ? C14 C9 N2 121.0(2) . . ? C10 C9 N2 117.6(3) . . ? C11 C10 C9 117.9(3) . . ? C11 C10 C15 120.3(3) . . ? C9 C10 C15 121.8(3) . . ? C12 C11 C10 120.8(3) . . ? C13 C12 C11 120.2(3) . . ? C12 C13 C14 121.3(3) . . ? C9 C14 C13 118.2(3) . . ? C9 C14 C18 122.4(3) . . ? C13 C14 C18 119.3(3) . . ? C10 C15 C17 111.1(3) . . ? C10 C15 C16 113.4(3) . . ? C17 C15 C16 110.2(3) . . ? C20 C18 C14 110.7(3) . . ? C20 C18 C19 109.2(3) . . ? C14 C18 C19 112.6(3) . . ? C26 C21 C22 121.0(3) . . ? C26 C21 N6 118.9(3) . . ? C22 C21 N6 120.1(2) . . ? C23 C22 C21 118.2(3) . . ? C23 C22 C27 119.7(3) . . ? C21 C22 C27 122.1(3) . . ? C24 C23 C22 121.2(3) . . ? C23 C24 C25 120.1(3) . . ? C24 C25 C26 121.1(3) . . ? C25 C26 C21 118.2(3) . . ? C25 C26 C30 119.8(3) . . ? C21 C26 C30 121.9(3) . . ? C22 C27 C29 110.7(3) . . ? C22 C27 C28 112.4(3) . . ? C29 C27 C28 109.9(3) . . ? C31 C30 C32 109.5(3) . . ? C31 C30 C26 112.2(3) . . ? C32 C30 C26 112.1(3) . . ? _refine_diff_density_max 0.426 _refine_diff_density_min -0.494 _refine_diff_density_rms 0.078 #===END data_Compound_8 _database_code_CSD 207272 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C58 H82 N4 Br2 Mg2' _chemical_formula_weight 1043.72 _chemical_melting_point ? _chemical_compound_source ? 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' Br Br -0.6763 1.2805 '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 C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 22.9835(11) _cell_length_b 15.0629(5) _cell_length_c 16.4637(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.497(3) _cell_angle_gamma 90.00 _cell_volume 5699.5(4) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 26 _cell_measurement_theta_min 11.16 _cell_measurement_theta_max 27.98 _exptl_crystal_description rhombs _exptl_crystal_colour Clear _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.216 _exptl_crystal_density_method ? _exptl_crystal_F_000 2208 _exptl_absorpt_coefficient_mu 2.301 _exptl_absorpt_correction_type Ellipsoidal _exptl_absorpt_correction_T_min 0.5428 _exptl_absorpt_correction_T_max 0.8512 _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4348 _diffrn_reflns_av_R_equivalents 0.0251 _diffrn_reflns_av_sigmaI/netI 0.0351 _diffrn_reflns_limit_h_min -2 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.51 _diffrn_reflns_theta_max 59.99 _reflns_number_total 4228 _reflns_number_observed 3661 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 157 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0429P)^2^+2.9771P] 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 ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00008(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4071 _refine_ls_number_parameters 299 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0415 _refine_ls_R_factor_obs 0.0323 _refine_ls_wR_factor_all 0.0802 _refine_ls_wR_factor_obs 0.0742 _refine_ls_goodness_of_fit_all 1.044 _refine_ls_goodness_of_fit_obs 1.067 _refine_ls_restrained_S_all 1.067 _refine_ls_restrained_S_obs 1.067 _refine_ls_shift/esd_max 0.001 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Mg Mg 0.19328(3) 0.17125(4) 0.00093(4) 0.0172(2) Uani 1 d . . Br Br 0.225645(10) 0.29171(2) 0.098242(14) 0.02717(10) Uani 1 d . . N2 N 0.19075(8) 0.04435(12) 0.04185(11) 0.0197(4) Uani 1 d . . C3 C 0.15147(10) -0.01179(15) 0.01139(13) 0.0207(4) Uani 1 d . . C4 C 0.10454(10) 0.01352(15) -0.03883(14) 0.0233(5) Uani 1 d . . H4A H 0.08416(10) -0.03434(15) -0.06363(14) 0.028 Uiso 1 calc R . C5 C 0.08301(9) 0.0980(2) -0.05819(13) 0.0205(4) Uani 1 d . . N6 N 0.11012(8) 0.17403(12) -0.04170(11) 0.0193(4) Uani 1 d . . C7 C 0.15415(12) -0.1099(2) 0.0311(2) 0.0321(5) Uani 1 d . . H7A H 0.17970(12) -0.1398(2) -0.0076(2) 0.048 Uiso 1 d R . H7B H 0.11499(12) -0.1354(2) 0.0273(2) 0.048 Uiso 1 d R . H7C H 0.16949(12) -0.1180(2) 0.0863(2) 0.048 Uiso 1 d R . C8 C 0.02370(10) 0.0984(2) -0.0997(2) 0.0307(5) Uani 1 d . . H8A H 0.00422(10) 0.0415(2) -0.0901(2) 0.046 Uiso 1 d R . H8B H 0.02858(10) 0.1072(2) -0.1583(2) 0.046 Uiso 1 d R . H8C H 0.00006(10) 0.1467(2) -0.0776(2) 0.046 Uiso 1 d R . C9 C 0.22965(10) 0.01096(15) 0.10366(14) 0.0228(5) Uani 1 d . . C10 C 0.21443(11) 0.0240(2) 0.18567(15) 0.0284(5) Uani 1 d . . C11 C 0.24971(14) -0.0136(2) 0.2456(2) 0.0424(7) Uani 1 d . . H11A H 0.23948(14) -0.0070(2) 0.3011(2) 0.051 Uiso 1 calc R . C12 C 0.29920(14) -0.0601(2) 0.2258(2) 0.0466(7) Uani 1 d . . H12A H 0.32226(14) -0.0863(2) 0.2675(2) 0.056 Uiso 1 calc R . C13 C 0.31540(12) -0.0688(2) 0.1460(2) 0.0387(6) Uani 1 d . . H13A H 0.35049(12) -0.0989(2) 0.1335(2) 0.046 Uiso 1 calc R . C14 C 0.28132(11) -0.0341(2) 0.0831(2) 0.0274(5) Uani 1 d . . C15 C 0.16015(12) 0.0758(2) 0.2083(2) 0.0346(6) Uani 1 d . . H15A H 0.15039(12) 0.1154(2) 0.1614(2) 0.042 Uiso 1 calc R . C16 C 0.16912(15) 0.1356(2) 0.2827(2) 0.0507(8) Uani 1 d . . H16A H 0.13287(15) 0.1672(2) 0.2944(2) 0.076 Uiso 1 calc R . H16B H 0.20001(15) 0.1786(2) 0.2717(2) 0.076 Uiso 1 calc R . H16C H 0.18023(15) 0.0991(2) 0.3296(2) 0.076 Uiso 1 calc R . C17 C 0.10812(14) 0.0146(3) 0.2210(2) 0.0540(8) Uani 1 d . . H17A H 0.07401(14) 0.0501(3) 0.2355(2) 0.081 Uiso 1 calc R . H17B H 0.11694(14) -0.0274(3) 0.2649(2) 0.081 Uiso 1 calc R . H17C H 0.09999(14) -0.0182(3) 0.1708(2) 0.081 Uiso 1 calc R . C18 C 0.30039(11) -0.0462(2) -0.0043(2) 0.0310(5) Uani 1 d . . H18A H 0.26922(11) -0.0220(2) -0.0408(2) 0.037 Uiso 1 calc R . C19 C 0.3103(2) -0.1438(2) -0.0265(3) 0.0600(9) Uani 1 d . . H19A H 0.3225(2) -0.1480(2) -0.0833(3) 0.090 Uiso 1 calc R . H19B H 0.2741(2) -0.1771(2) -0.0193(3) 0.090 Uiso 1 calc R . H19C H 0.3407(2) -0.1688(2) 0.0088(3) 0.090 Uiso 1 calc R . C20 C 0.35657(13) 0.0057(2) -0.0197(2) 0.0430(7) Uani 1 d . . H20A H 0.36842(13) -0.0026(2) -0.0762(2) 0.065 Uiso 1 calc R . H20B H 0.38737(13) -0.0160(2) 0.0167(2) 0.065 Uiso 1 calc R . H20C H 0.34985(13) 0.0690(2) -0.0095(2) 0.065 Uiso 1 calc R . C21 C 0.07859(9) 0.25529(15) -0.05682(14) 0.0207(4) Uani 1 d . . C22 C 0.08150(10) 0.2963(2) -0.13343(15) 0.0243(5) Uani 1 d . . C23 C 0.04779(12) 0.3728(2) -0.1465(2) 0.0334(6) Uani 1 d . . H23A H 0.04943(12) 0.4020(2) -0.1976(2) 0.040 Uiso 1 calc R . C24 C 0.01251(12) 0.4065(2) -0.0871(2) 0.0375(6) Uani 1 d . . H24A H -0.01125(12) 0.4568(2) -0.0980(2) 0.045 Uiso 1 calc R . C25 C 0.01167(11) 0.3671(2) -0.0115(2) 0.0352(6) Uani 1 d . . H25A H -0.01215(11) 0.3917(2) 0.0297(2) 0.042 Uiso 1 calc R . C26 C 0.04498(10) 0.2921(2) 0.0058(2) 0.0272(5) Uani 1 d . . C27 C 0.11897(11) 0.2609(2) -0.20130(15) 0.0289(5) Uani 1 d . . H27A H 0.13961(11) 0.2067(2) -0.18094(15) 0.035 Uiso 1 calc R . C28 C 0.08326(13) 0.2348(2) -0.2767(2) 0.0436(7) Uani 1 d . . H28A H 0.10937(13) 0.2123(2) -0.3187(2) 0.065 Uiso 1 calc R . H28B H 0.06233(13) 0.2869(2) -0.2974(2) 0.065 Uiso 1 calc R . H28C H 0.05527(13) 0.1885(2) -0.2622(2) 0.065 Uiso 1 calc R . C29 C 0.16451(14) 0.3287(2) -0.2256(2) 0.0485(7) Uani 1 d . . H29A H 0.18826(14) 0.3045(2) -0.2695(2) 0.073 Uiso 1 calc R . H29B H 0.18948(14) 0.3423(2) -0.1787(2) 0.073 Uiso 1 calc R . H29C H 0.14517(14) 0.3831(2) -0.2443(2) 0.073 Uiso 1 calc R . C30 C 0.04413(12) 0.2519(2) 0.0904(2) 0.0364(6) Uani 1 d . . H30A H 0.07637(12) 0.2074(2) 0.0933(2) 0.044 Uiso 1 calc R . C31 C 0.0554(2) 0.3198(3) 0.1564(2) 0.0553(9) Uani 1 d . . H31A H 0.0918(2) 0.3513(3) 0.1452(2) 0.083 Uiso 1 calc R . H31B H 0.0586(2) 0.2897(3) 0.2090(2) 0.083 Uiso 1 calc R . H31C H 0.0232(2) 0.3624(3) 0.1577(2) 0.083 Uiso 1 calc R . C32 C -0.0119(3) 0.2029(4) 0.1070(3) 0.091(2) Uani 1 d . . H32A H -0.0189(3) 0.1591(4) 0.0640(3) 0.137 Uiso 1 calc R . H32B H -0.0442(3) 0.2452(4) 0.1082(3) 0.137 Uiso 1 calc R . H32C H -0.0088(3) 0.1726(4) 0.1595(3) 0.137 Uiso 1 calc R . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mg 0.0146(3) 0.0165(3) 0.0204(3) 0.0003(3) 0.0017(3) -0.0035(2) Br 0.02697(14) 0.02997(15) 0.02475(14) -0.00941(9) 0.01061(9) -0.01053(9) N2 0.0183(9) 0.0202(9) 0.0205(9) 0.0030(7) 0.0025(7) -0.0021(7) C3 0.0217(11) 0.0187(11) 0.0217(10) 0.0009(8) 0.0074(8) -0.0031(8) C4 0.0240(11) 0.0201(11) 0.0257(11) -0.0026(9) 0.0012(9) -0.0065(9) C5 0.0174(10) 0.0234(11) 0.0206(10) -0.0022(8) 0.0025(8) -0.0036(8) N6 0.0182(9) 0.0193(9) 0.0205(9) -0.0005(7) 0.0028(7) -0.0021(7) C7 0.0372(13) 0.0200(12) 0.0391(14) 0.0047(10) -0.0021(11) -0.0058(10) C8 0.0208(11) 0.0298(12) 0.0414(14) -0.0052(11) -0.0060(10) -0.0037(9) C9 0.0229(11) 0.0208(10) 0.0247(11) 0.0059(9) 0.0002(9) -0.0041(9) C10 0.0319(13) 0.0304(12) 0.0230(11) 0.0078(9) 0.0030(10) -0.0054(10) C11 0.050(2) 0.051(2) 0.0260(12) 0.0143(12) -0.0020(11) -0.0072(13) C12 0.044(2) 0.052(2) 0.043(2) 0.0227(14) -0.0086(13) 0.0033(13) C13 0.0335(14) 0.0388(14) 0.044(2) 0.0121(12) -0.0031(12) 0.0075(11) C14 0.0235(11) 0.0231(11) 0.0358(13) 0.0054(10) -0.0005(10) -0.0017(9) C15 0.0361(14) 0.0429(15) 0.0250(12) 0.0032(11) 0.0099(10) -0.0029(12) C16 0.046(2) 0.062(2) 0.043(2) -0.0130(15) 0.0169(14) -0.0100(15) C17 0.037(2) 0.071(2) 0.054(2) -0.013(2) 0.0138(14) -0.016(2) C18 0.0278(12) 0.0313(13) 0.0340(13) -0.0020(10) 0.0038(10) 0.0041(10) C19 0.068(2) 0.041(2) 0.071(2) -0.016(2) 0.017(2) -0.001(2) C20 0.0327(14) 0.044(2) 0.053(2) 0.0057(13) 0.0123(12) 0.0021(12) C21 0.0153(9) 0.0196(10) 0.0272(11) -0.0031(9) -0.0008(8) -0.0022(8) C22 0.0211(10) 0.0231(11) 0.0287(12) -0.0013(9) -0.0034(9) -0.0002(9) C23 0.0380(14) 0.0237(12) 0.0383(14) 0.0007(10) -0.0101(11) 0.0036(10) C24 0.0349(13) 0.0264(12) 0.051(2) -0.0066(11) -0.0110(12) 0.0096(10) C25 0.0262(12) 0.0317(13) 0.048(2) -0.0146(12) -0.0004(11) 0.0065(10) C26 0.0203(10) 0.0260(11) 0.0352(13) -0.0079(10) 0.0028(9) -0.0014(9) C27 0.0271(12) 0.0330(13) 0.0265(12) 0.0051(10) 0.0022(10) 0.0011(10) C28 0.0389(14) 0.057(2) 0.0345(14) -0.0146(13) -0.0031(12) 0.0054(13) C29 0.040(2) 0.063(2) 0.043(2) 0.0100(14) 0.0067(13) -0.0129(14) C30 0.0363(14) 0.0376(14) 0.0355(14) -0.0038(11) 0.0145(11) 0.0025(11) C31 0.062(2) 0.070(2) 0.035(2) -0.0057(15) 0.0076(14) -0.028(2) C32 0.121(4) 0.101(4) 0.051(2) -0.002(2) 0.015(2) -0.082(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 Mg N2 2.028(2) . ? Mg N6 2.031(2) . ? Mg Br 2.5282(7) . ? Mg Br 2.5498(7) 7 ? Mg Mg 3.5253(13) 7 ? Br Mg 2.5498(7) 7 ? N2 C3 1.332(3) . ? N2 C9 1.440(3) . ? C3 C4 1.406(3) . ? C3 C7 1.514(3) . ? C4 C5 1.401(3) . ? C5 N6 1.331(3) . ? C5 C8 1.520(3) . ? N6 C21 1.443(3) . ? C9 C10 1.411(3) . ? C9 C14 1.412(4) . ? C10 C11 1.392(4) . ? C10 C15 1.521(4) . ? C11 C12 1.378(5) . ? C12 C13 1.375(5) . ? C13 C14 1.395(4) . ? C14 C18 1.518(4) . ? C15 C17 1.526(4) . ? C15 C16 1.532(4) . ? C18 C20 1.533(4) . ? C18 C19 1.533(4) . ? C21 C22 1.407(3) . ? C21 C26 1.408(3) . ? C22 C23 1.404(4) . ? C22 C27 1.514(3) . ? C23 C24 1.373(4) . ? C24 C25 1.379(4) . ? C25 C26 1.394(4) . ? C26 C30 1.518(4) . ? C27 C29 1.519(4) . ? C27 C28 1.534(4) . ? C30 C32 1.510(5) . ? C30 C31 1.513(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Mg N6 96.00(8) . . ? N2 Mg Br 118.36(6) . . ? N6 Mg Br 118.36(6) . . ? N2 Mg Br 116.25(6) . 7 ? N6 Mg Br 117.72(6) . 7 ? Br Mg Br 92.07(2) . 7 ? N2 Mg Mg 131.35(6) . 7 ? N6 Mg Mg 132.61(6) . 7 ? Br Mg Mg 46.29(2) . 7 ? Br Mg Mg 45.78(2) 7 7 ? Mg Br Mg 87.93(2) . 7 ? C3 N2 C9 117.3(2) . . ? C3 N2 Mg 119.7(2) . . ? C9 N2 Mg 123.01(14) . . ? N2 C3 C4 124.3(2) . . ? N2 C3 C7 120.9(2) . . ? C4 C3 C7 114.8(2) . . ? C5 C4 C3 130.4(2) . . ? N6 C5 C4 124.8(2) . . ? N6 C5 C8 120.3(2) . . ? C4 C5 C8 114.8(2) . . ? C5 N6 C21 117.5(2) . . ? C5 N6 Mg 119.37(15) . . ? C21 N6 Mg 123.15(14) . . ? C10 C9 C14 120.9(2) . . ? C10 C9 N2 118.0(2) . . ? C14 C9 N2 121.1(2) . . ? C11 C10 C9 118.3(3) . . ? C11 C10 C15 120.6(2) . . ? C9 C10 C15 121.1(2) . . ? C12 C11 C10 121.1(3) . . ? C13 C12 C11 120.4(3) . . ? C12 C13 C14 121.3(3) . . ? C13 C14 C9 118.0(2) . . ? C13 C14 C18 119.6(2) . . ? C9 C14 C18 122.4(2) . . ? C10 C15 C17 111.6(2) . . ? C10 C15 C16 113.1(2) . . ? C17 C15 C16 110.2(2) . . ? C14 C18 C20 110.3(2) . . ? C14 C18 C19 112.7(2) . . ? C20 C18 C19 108.8(2) . . ? C22 C21 C26 121.0(2) . . ? C22 C21 N6 120.0(2) . . ? C26 C21 N6 119.0(2) . . ? C23 C22 C21 117.9(2) . . ? C23 C22 C27 119.5(2) . . ? C21 C22 C27 122.6(2) . . ? C24 C23 C22 121.5(3) . . ? C23 C24 C25 119.8(2) . . ? C24 C25 C26 121.4(2) . . ? C25 C26 C21 118.2(2) . . ? C25 C26 C30 120.0(2) . . ? C21 C26 C30 121.8(2) . . ? C22 C27 C29 110.8(2) . . ? C22 C27 C28 112.6(2) . . ? C29 C27 C28 108.9(2) . . ? C32 C30 C31 110.0(3) . . ? C32 C30 C26 112.2(3) . . ? C31 C30 C26 112.7(2) . . ? _refine_diff_density_max 0.261 _refine_diff_density_min -0.407 _refine_diff_density_rms 0.053 #===END data_Compound_12 _database_code_CSD 207273 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C35 H55 N3 Mg' _chemical_formula_weight 542.13 _chemical_melting_point ? _chemical_compound_source ? 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.7023(3) _cell_length_b 11.1726(4) _cell_length_c 15.4779(3) _cell_angle_alpha 88.885(2) _cell_angle_beta 78.697(2) _cell_angle_gamma 70.353(2) _cell_volume 1707.02(8) _cell_formula_units_Z 2 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used 23 _cell_measurement_theta_min 11.24 _cell_measurement_theta_max 23.98 _exptl_crystal_description prisms _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.43 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.27 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.055 _exptl_crystal_density_method ? _exptl_crystal_F_000 596 _exptl_absorpt_coefficient_mu 0.622 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 183(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 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5374 _diffrn_reflns_av_R_equivalents 0.0197 _diffrn_reflns_av_sigmaI/netI 0.0330 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.92 _diffrn_reflns_theta_max 59.98 _reflns_number_total 5058 _reflns_number_observed 4216 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 252 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0571P)^2^+0.7810P] 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 ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0071(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4806 _refine_ls_number_parameters 353 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0590 _refine_ls_R_factor_obs 0.0474 _refine_ls_wR_factor_all 0.1245 _refine_ls_wR_factor_obs 0.1156 _refine_ls_goodness_of_fit_all 1.048 _refine_ls_goodness_of_fit_obs 1.084 _refine_ls_restrained_S_all 1.058 _refine_ls_restrained_S_obs 1.084 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Mg Mg 0.20908(7) 0.72145(6) 0.21359(4) 0.0246(2) Uani 1 d . . C1 C 0.4706(2) 0.6527(2) 0.26682(14) 0.0288(5) Uani 1 d . . N1 N 0.3386(2) 0.6787(2) 0.29821(11) 0.0254(4) Uani 1 d . . C2 C 0.5241(2) 0.6830(2) 0.18257(14) 0.0303(5) Uani 1 d . . H2A H 0.6199(2) 0.6474(2) 0.16546(14) 0.036 Uiso 1 calc R . C3 C 0.4597(2) 0.7572(2) 0.11918(13) 0.0275(5) Uani 1 d . . N3 N 0.3266(2) 0.7930(2) 0.12275(10) 0.0241(4) Uani 1 d . . C4 C 0.5720(2) 0.5884(3) 0.3234(2) 0.0450(6) Uani 1 d . . H4A H 0.5242(2) 0.5715(3) 0.3806(2) 0.067 Uiso 1 calc R . H4B H 0.6226(2) 0.6440(3) 0.3326(2) 0.067 Uiso 1 calc R . H4C H 0.6350(2) 0.5079(3) 0.2938(2) 0.067 Uiso 1 calc R . C5 C 0.5509(2) 0.7980(2) 0.0462(2) 0.0396(6) Uani 1 d . . H5A H 0.4970(2) 0.8489(2) 0.0056(2) 0.059 Uiso 1 calc R . H5B H 0.6202(2) 0.7225(2) 0.0140(2) 0.059 Uiso 1 calc R . H5C H 0.5948(2) 0.8489(2) 0.0717(2) 0.059 Uiso 1 calc R . C6 C 0.2932(2) 0.6734(2) 0.39179(13) 0.0276(5) Uani 1 d . . C7 C 0.2710(2) 0.5642(2) 0.42806(14) 0.0313(5) Uani 1 d . . C8 C 0.2204(2) 0.5673(2) 0.51814(15) 0.0405(6) Uani 1 d . . H8A H 0.2046(2) 0.4942(2) 0.54333(15) 0.049 Uiso 1 calc R . C9 C 0.1928(3) 0.6736(2) 0.5717(2) 0.0461(6) Uani 1 d . . H9A H 0.1581(3) 0.6736(2) 0.6331(2) 0.055 Uiso 1 calc R . C10 C 0.2157(3) 0.7800(2) 0.5357(2) 0.0436(6) Uani 1 d . . H10A H 0.1975(3) 0.8528(2) 0.5731(2) 0.052 Uiso 1 calc R . C11 C 0.2649(2) 0.7832(2) 0.44582(14) 0.0338(5) Uani 1 d . . C12 C 0.3021(3) 0.4429(2) 0.3733(2) 0.0386(6) Uani 1 d . . H12A H 0.3390(3) 0.4572(2) 0.3109(2) 0.046 Uiso 1 calc R . C13 C 0.1734(3) 0.4105(3) 0.3745(2) 0.0544(7) Uani 1 d . . H13A H 0.1963(3) 0.3319(3) 0.3387(2) 0.082 Uiso 1 calc R . H13B H 0.1081(3) 0.4802(3) 0.3503(2) 0.082 Uiso 1 calc R . H13C H 0.1336(3) 0.3989(3) 0.4353(2) 0.082 Uiso 1 calc R . C14 C 0.4099(3) 0.3305(3) 0.4045(2) 0.0581(7) Uani 1 d . . H14A H 0.4275(3) 0.2539(3) 0.3678(2) 0.087 Uiso 1 calc R . H14B H 0.3771(3) 0.3161(3) 0.4661(2) 0.087 Uiso 1 calc R . H14C H 0.4937(3) 0.3499(3) 0.3995(2) 0.087 Uiso 1 calc R . C15 C 0.2906(3) 0.9025(2) 0.4094(2) 0.0397(6) Uani 1 d . . H15A H 0.3117(3) 0.8919(2) 0.3436(2) 0.048 Uiso 1 calc R . C16 C 0.4122(4) 0.9193(3) 0.4382(3) 0.0837(12) Uani 1 d . . H16A H 0.4914(4) 0.8422(3) 0.4211(3) 0.126 Uiso 1 calc R . H16B H 0.3923(4) 0.9344(3) 0.5024(3) 0.126 Uiso 1 calc R . H16C H 0.4311(4) 0.9921(3) 0.4096(3) 0.126 Uiso 1 calc R . C17 C 0.1677(3) 1.0218(2) 0.4357(2) 0.0536(7) Uani 1 d . . H17A H 0.0896(3) 1.0107(2) 0.4172(2) 0.080 Uiso 1 calc R . H17B H 0.1865(3) 1.0947(2) 0.4071(2) 0.080 Uiso 1 calc R . H17C H 0.1477(3) 1.0369(2) 0.4999(2) 0.080 Uiso 1 calc R . C18 C 0.2675(2) 0.8827(2) 0.06116(13) 0.0257(4) Uani 1 d . . C19 C 0.2011(2) 1.0109(2) 0.09117(13) 0.0289(5) Uani 1 d . . C20 C 0.1403(2) 1.0974(2) 0.03303(15) 0.0354(5) Uani 1 d . . H20A H 0.0963(2) 1.1844(2) 0.05214(15) 0.042 Uiso 1 calc R . C21 C 0.1426(3) 1.0594(2) -0.0517(2) 0.0413(6) Uani 1 d . . H21A H 0.1001(3) 1.1196(2) -0.0904(2) 0.050 Uiso 1 calc R . C22 C 0.2070(2) 0.9336(2) -0.07985(15) 0.0386(6) Uani 1 d . . H22A H 0.2086(2) 0.9080(2) -0.13834(15) 0.046 Uiso 1 calc R . C23 C 0.2701(2) 0.8427(2) -0.02477(14) 0.0300(5) Uani 1 d . . C24 C 0.1985(2) 1.0553(2) 0.18402(14) 0.0306(5) Uani 1 d . . H24A H 0.1985(2) 0.9828(2) 0.22296(14) 0.037 Uiso 1 calc R . C25 C 0.0722(2) 1.1683(2) 0.2220(2) 0.0408(6) Uani 1 d . . H25A H 0.0767(2) 1.1921(2) 0.2816(2) 0.061 Uiso 1 calc R . H25B H -0.0086(2) 1.1446(2) 0.2243(2) 0.061 Uiso 1 calc R . H25C H 0.0676(2) 1.2405(2) 0.1843(2) 0.061 Uiso 1 calc R . C26 C 0.3256(3) 1.0867(2) 0.1880(2) 0.0450(6) Uani 1 d . . H26A H 0.3212(3) 1.1150(2) 0.2484(2) 0.068 Uiso 1 calc R . H26B H 0.3313(3) 1.1547(2) 0.1480(2) 0.068 Uiso 1 calc R . H26C H 0.4058(3) 1.0107(2) 0.1701(2) 0.068 Uiso 1 calc R . C27 C 0.3340(2) 0.7043(2) -0.05896(14) 0.0336(5) Uani 1 d . . H27A H 0.3784(2) 0.6538(2) -0.01249(14) 0.040 Uiso 1 calc R . C28 C 0.4422(3) 0.6858(3) -0.1437(2) 0.0565(7) Uani 1 d . . H28A H 0.5116(3) 0.7197(3) -0.1332(2) 0.085 Uiso 1 calc R . H28B H 0.3999(3) 0.7310(3) -0.1911(2) 0.085 Uiso 1 calc R . H28C H 0.4841(3) 0.5949(3) -0.1608(2) 0.085 Uiso 1 calc R . C29 C 0.2271(3) 0.6515(2) -0.0761(2) 0.0470(6) Uani 1 d . . H29A H 0.2705(3) 0.5625(2) -0.0980(2) 0.071 Uiso 1 calc R . H29B H 0.1801(3) 0.7013(2) -0.1202(2) 0.071 Uiso 1 calc R . H29C H 0.1616(3) 0.6565(2) -0.0211(2) 0.071 Uiso 1 calc R . N30 N 0.0400(2) 0.6909(2) 0.21885(11) 0.0288(4) Uani 1 d . . C31 C -0.0859(2) 0.7782(2) 0.26923(14) 0.0339(5) Uani 1 d . . H31A H -0.1569(2) 0.7948(2) 0.23275(14) 0.041 Uiso 1 calc R . C32 C -0.0646(3) 0.9025(2) 0.2857(2) 0.0485(6) Uani 1 d . . H32A H -0.0318(3) 0.9341(2) 0.2294(2) 0.073 Uiso 1 calc R . H32B H 0.0024(3) 0.8886(2) 0.3233(2) 0.073 Uiso 1 calc R . H32C H -0.1506(3) 0.9653(2) 0.3152(2) 0.073 Uiso 1 calc R . C33 C -0.1368(3) 0.7292(3) 0.3569(2) 0.0517(7) Uani 1 d . . H33A H -0.1506(3) 0.6487(3) 0.3463(2) 0.078 Uiso 1 calc R . H33B H -0.2227(3) 0.7920(3) 0.3864(2) 0.078 Uiso 1 calc R . H33C H -0.0698(3) 0.7153(3) 0.3945(2) 0.078 Uiso 1 calc R . C34 C 0.0322(2) 0.5735(2) 0.18473(15) 0.0345(5) Uani 1 d . . H34A H -0.0022(2) 0.5291(2) 0.23576(15) 0.041 Uiso 1 calc R . C35 C -0.0618(3) 0.5937(3) 0.1190(2) 0.0467(6) Uani 1 d . . H35A H -0.1531(3) 0.6484(3) 0.1470(2) 0.070 Uiso 1 calc R . H35B H -0.0645(3) 0.5113(3) 0.1007(2) 0.070 Uiso 1 calc R . H35C H -0.0279(3) 0.6342(3) 0.0673(2) 0.070 Uiso 1 calc R . C36 C 0.1743(3) 0.4888(2) 0.1424(2) 0.0458(6) Uani 1 d . . H36A H 0.2336(3) 0.4766(2) 0.1851(2) 0.069 Uiso 1 calc R . H36B H 0.2088(3) 0.5291(2) 0.0908(2) 0.069 Uiso 1 calc R . H36C H 0.1722(3) 0.4062(2) 0.1241(2) 0.069 Uiso 1 calc R . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mg 0.0240(4) 0.0290(4) 0.0246(4) 0.0055(3) -0.0061(3) -0.0136(3) C1 0.0269(11) 0.0265(11) 0.0350(12) 0.0032(9) -0.0101(9) -0.0095(9) N1 0.0272(9) 0.0268(9) 0.0240(9) 0.0028(7) -0.0064(7) -0.0110(7) C2 0.0202(10) 0.0318(11) 0.0376(12) 0.0025(9) -0.0047(9) -0.0078(9) C3 0.0256(11) 0.0283(11) 0.0293(11) 0.0014(8) -0.0022(9) -0.0121(9) N3 0.0250(9) 0.0248(9) 0.0240(9) 0.0042(7) -0.0048(7) -0.0106(7) C4 0.0305(12) 0.059(2) 0.0462(14) 0.0147(12) -0.0156(11) -0.0120(12) C5 0.0310(12) 0.0500(14) 0.0383(13) 0.0084(11) -0.0011(10) -0.0179(11) C6 0.0287(11) 0.0308(11) 0.0249(10) 0.0045(8) -0.0101(9) -0.0095(9) C7 0.0326(12) 0.0323(12) 0.0292(11) 0.0062(9) -0.0079(9) -0.0104(10) C8 0.0470(14) 0.0395(13) 0.0323(12) 0.0122(10) -0.0047(11) -0.0135(11) C9 0.055(2) 0.0473(15) 0.0253(12) 0.0052(11) -0.0028(11) -0.0073(12) C10 0.054(2) 0.0384(13) 0.0318(13) -0.0022(10) -0.0095(11) -0.0068(12) C11 0.0382(12) 0.0333(12) 0.0312(12) 0.0035(9) -0.0124(10) -0.0108(10) C12 0.0532(15) 0.0303(12) 0.0332(12) 0.0070(9) -0.0081(11) -0.0159(11) C13 0.069(2) 0.048(2) 0.058(2) 0.0107(13) -0.0216(14) -0.0316(14) C14 0.068(2) 0.0371(14) 0.063(2) 0.0060(13) -0.0181(15) -0.0070(13) C15 0.0495(14) 0.0357(13) 0.0379(13) 0.0015(10) -0.0135(11) -0.0169(11) C16 0.082(2) 0.060(2) 0.137(3) 0.030(2) -0.057(2) -0.042(2) C17 0.072(2) 0.0348(14) 0.052(2) 0.0021(12) -0.0147(14) -0.0135(13) C18 0.0256(11) 0.0295(11) 0.0260(10) 0.0073(8) -0.0047(8) -0.0150(9) C19 0.0312(11) 0.0276(11) 0.0290(11) 0.0057(9) -0.0033(9) -0.0133(9) C20 0.0438(13) 0.0273(11) 0.0357(12) 0.0071(9) -0.0090(10) -0.0126(10) C21 0.0531(15) 0.0362(13) 0.0365(13) 0.0139(10) -0.0149(11) -0.0151(11) C22 0.0501(15) 0.0428(14) 0.0275(11) 0.0074(10) -0.0120(10) -0.0195(12) C23 0.0323(11) 0.0322(11) 0.0288(11) 0.0029(9) -0.0044(9) -0.0161(10) C24 0.0375(12) 0.0265(11) 0.0294(11) 0.0035(9) -0.0063(9) -0.0134(10) C25 0.0443(14) 0.0353(13) 0.0399(13) -0.0020(10) -0.0049(11) -0.0115(11) C26 0.0464(15) 0.0490(15) 0.0448(14) -0.0055(11) -0.0087(11) -0.0226(12) C27 0.0354(12) 0.0340(12) 0.0322(12) -0.0030(9) -0.0069(10) -0.0123(10) C28 0.051(2) 0.060(2) 0.055(2) -0.0159(14) 0.0096(13) -0.0253(14) C29 0.0430(14) 0.0417(14) 0.059(2) -0.0021(12) -0.0099(12) -0.0183(12) N30 0.0269(9) 0.0341(10) 0.0305(9) 0.0015(7) -0.0051(7) -0.0171(8) C31 0.0326(12) 0.0401(13) 0.0328(12) 0.0027(10) -0.0060(9) -0.0175(10) C32 0.059(2) 0.0413(14) 0.0460(14) -0.0058(11) -0.0048(12) -0.0205(13) C33 0.050(2) 0.060(2) 0.0433(15) 0.0022(12) 0.0077(12) -0.0247(14) C34 0.0378(13) 0.0337(12) 0.0369(12) 0.0031(10) -0.0053(10) -0.0199(10) C35 0.0430(14) 0.054(2) 0.053(2) -0.0094(12) -0.0137(12) -0.0259(12) C36 0.0459(15) 0.0382(14) 0.0502(15) 0.0021(11) -0.0097(12) -0.0104(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mg N30 1.938(2) . ? Mg N1 2.026(2) . ? Mg N3 2.034(2) . ? C1 N1 1.333(3) . ? C1 C2 1.401(3) . ? C1 C4 1.512(3) . ? N1 C6 1.441(3) . ? C2 C3 1.405(3) . ? C3 N3 1.333(3) . ? C3 C5 1.511(3) . ? N3 C18 1.444(3) . ? C6 C7 1.406(3) . ? C6 C11 1.409(3) . ? C7 C8 1.390(3) . ? C7 C12 1.515(3) . ? C8 C9 1.375(3) . ? C9 C10 1.379(4) . ? C10 C11 1.392(3) . ? C11 C15 1.525(3) . ? C12 C13 1.534(4) . ? C12 C14 1.537(3) . ? C15 C17 1.518(4) . ? C15 C16 1.525(4) . ? C18 C23 1.403(3) . ? C18 C19 1.409(3) . ? C19 C20 1.393(3) . ? C19 C24 1.521(3) . ? C20 C21 1.380(3) . ? C21 C22 1.376(3) . ? C22 C23 1.394(3) . ? C23 C27 1.522(3) . ? C24 C26 1.527(3) . ? C24 C25 1.528(3) . ? C27 C29 1.519(3) . ? C27 C28 1.535(3) . ? N30 C31 1.452(3) . ? N30 C34 1.457(3) . ? C31 C32 1.516(3) . ? C31 C33 1.523(3) . ? C34 C36 1.518(3) . ? C34 C35 1.528(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N30 Mg N1 130.67(8) . . ? N30 Mg N3 134.56(8) . . ? N1 Mg N3 94.65(7) . . ? N1 C1 C2 123.7(2) . . ? N1 C1 C4 120.1(2) . . ? C2 C1 C4 116.2(2) . . ? C1 N1 C6 118.4(2) . . ? C1 N1 Mg 119.41(14) . . ? C6 N1 Mg 122.20(13) . . ? C1 C2 C3 130.8(2) . . ? N3 C3 C2 123.3(2) . . ? N3 C3 C5 121.1(2) . . ? C2 C3 C5 115.6(2) . . ? C3 N3 C18 119.1(2) . . ? C3 N3 Mg 120.27(13) . . ? C18 N3 Mg 120.60(12) . . ? C7 C6 C11 120.6(2) . . ? C7 C6 N1 121.2(2) . . ? C11 C6 N1 118.2(2) . . ? C8 C7 C6 118.5(2) . . ? C8 C7 C12 118.8(2) . . ? C6 C7 C12 122.7(2) . . ? C9 C8 C7 121.6(2) . . ? C8 C9 C10 119.6(2) . . ? C9 C10 C11 121.5(2) . . ? C10 C11 C6 118.3(2) . . ? C10 C11 C15 119.5(2) . . ? C6 C11 C15 122.2(2) . . ? C7 C12 C13 111.1(2) . . ? C7 C12 C14 111.6(2) . . ? C13 C12 C14 110.2(2) . . ? C17 C15 C16 109.6(2) . . ? C17 C15 C11 112.4(2) . . ? C16 C15 C11 111.4(2) . . ? C23 C18 C19 120.7(2) . . ? C23 C18 N3 121.2(2) . . ? C19 C18 N3 118.0(2) . . ? C20 C19 C18 118.4(2) . . ? C20 C19 C24 120.4(2) . . ? C18 C19 C24 121.1(2) . . ? C21 C20 C19 121.4(2) . . ? C22 C21 C20 119.5(2) . . ? C21 C22 C23 121.7(2) . . ? C22 C23 C18 118.2(2) . . ? C22 C23 C27 118.9(2) . . ? C18 C23 C27 122.9(2) . . ? C19 C24 C26 111.2(2) . . ? C19 C24 C25 113.5(2) . . ? C26 C24 C25 109.9(2) . . ? C29 C27 C23 111.0(2) . . ? C29 C27 C28 108.9(2) . . ? C23 C27 C28 112.7(2) . . ? C31 N30 C34 115.6(2) . . ? C31 N30 Mg 120.51(13) . . ? C34 N30 Mg 123.31(14) . . ? N30 C31 C32 108.2(2) . . ? N30 C31 C33 114.1(2) . . ? C32 C31 C33 109.4(2) . . ? N30 C34 C36 108.3(2) . . ? N30 C34 C35 114.0(2) . . ? C36 C34 C35 110.2(2) . . ? _refine_diff_density_max 0.357 _refine_diff_density_min -0.278 _refine_diff_density_rms 0.039 #===END data_Compound_13 _database_code_CSD 207274 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C35 H59 N3 Si2 Mg' _chemical_formula_weight 602.34 _chemical_melting_point ? _chemical_compound_source ? 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' Si Si 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/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 9.1369(5) _cell_length_b 20.3728(7) _cell_length_c 20.235(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.148(4) _cell_angle_gamma 90.00 _cell_volume 3766.5(6) _cell_formula_units_Z 4 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used 37 _cell_measurement_theta_min 11.13 _cell_measurement_theta_max 28.01 _exptl_crystal_description prisms _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.67 _exptl_crystal_size_mid 0.63 _exptl_crystal_size_min 0.53 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.062 _exptl_crystal_density_method ? _exptl_crystal_F_000 1320 _exptl_absorpt_coefficient_mu 1.195 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 183(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 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5987 _diffrn_reflns_av_R_equivalents 0.0274 _diffrn_reflns_av_sigmaI/netI 0.0255 _diffrn_reflns_limit_h_min -5 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.08 _diffrn_reflns_theta_max 59.99 _reflns_number_total 5590 _reflns_number_observed 4786 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 201 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0602P)^2^+1.2948P] 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 ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0045(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 5389 _refine_ls_number_parameters 373 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0495 _refine_ls_R_factor_obs 0.0400 _refine_ls_wR_factor_all 0.1113 _refine_ls_wR_factor_obs 0.1042 _refine_ls_goodness_of_fit_all 1.071 _refine_ls_goodness_of_fit_obs 1.099 _refine_ls_restrained_S_all 1.081 _refine_ls_restrained_S_obs 1.099 _refine_ls_shift/esd_max -0.001 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Mg Mg 0.31107(6) 0.25477(3) 0.87245(3) 0.0218(2) Uani 1 d . . C1 C 0.5255(2) 0.20523(9) 0.96764(9) 0.0238(4) Uani 1 d . . N1 N 0.4054(2) 0.18911(7) 0.93346(7) 0.0215(3) Uani 1 d . . C2 C 0.5741(2) 0.26948(9) 0.97772(9) 0.0259(4) Uani 1 d . . H2A H 0.6668(2) 0.27324(9) 0.99878(9) 0.031 Uiso 1 calc R . C3 C 0.5066(2) 0.32963(9) 0.96141(9) 0.0241(4) Uani 1 d . . N3 N 0.3976(2) 0.33524(7) 0.91848(7) 0.0217(3) Uani 1 d . . C4 C 0.6176(2) 0.15170(10) 0.99893(10) 0.0315(5) Uani 1 d . . H4A H 0.6876(11) 0.17139(12) 1.0299(6) 0.047 Uiso 1 calc R . H4B H 0.6708(13) 0.1279(5) 0.96440(12) 0.047 Uiso 1 calc R . H4C H 0.5539(3) 0.1211(4) 1.0228(6) 0.047 Uiso 1 calc R . C5 C 0.5648(2) 0.38868(10) 0.99842(11) 0.0345(5) Uani 1 d . . H5A H 0.6542(10) 0.4044(5) 0.9770(5) 0.052 Uiso 1 calc R . H5B H 0.5869(16) 0.3762(2) 1.0442(2) 0.052 Uiso 1 calc R . H5C H 0.4911(7) 0.4236(3) 0.9981(7) 0.052 Uiso 1 calc R . C6 C 0.3490(2) 0.12353(9) 0.94015(9) 0.0254(4) Uani 1 d . . C7 C 0.3921(2) 0.07365(10) 0.89644(10) 0.0324(5) Uani 1 d . . C8 C 0.3284(3) 0.01201(11) 0.90292(13) 0.0446(6) Uani 1 d . . H8A H 0.3555(3) -0.02215(11) 0.87344(13) 0.053 Uiso 1 calc R . C9 C 0.2271(3) -0.00022(11) 0.95114(14) 0.0491(6) Uani 1 d . . H9A H 0.1850(3) -0.04270(11) 0.95486(14) 0.059 Uiso 1 calc R . C10 C 0.1859(2) 0.04859(11) 0.99423(12) 0.0417(6) Uani 1 d . . H10A H 0.1159(2) 0.03922(11) 1.02756(12) 0.050 Uiso 1 calc R . C11 C 0.2448(2) 0.11148(10) 0.98991(10) 0.0288(4) Uani 1 d . . C12 C 0.5044(3) 0.08501(11) 0.84231(11) 0.0417(5) Uani 1 d . . H12A H 0.5454(3) 0.13013(11) 0.84826(11) 0.050 Uiso 1 calc R . C13 C 0.4320(4) 0.08200(15) 0.77419(13) 0.0675(9) Uani 1 d . . H13A H 0.5060(4) 0.08942(15) 0.73999(13) 0.101 Uiso 1 calc R . H13B H 0.3563(4) 0.11594(15) 0.77107(13) 0.101 Uiso 1 calc R . H13C H 0.3874(4) 0.03870(15) 0.76783(13) 0.101 Uiso 1 calc R . C14 C 0.6314(3) 0.03626(15) 0.8460(2) 0.0664(8) Uani 1 d . . H14A H 0.7009(3) 0.04539(15) 0.8103(2) 0.100 Uiso 1 calc R . H14B H 0.5937(3) -0.00853(15) 0.8413(2) 0.100 Uiso 1 calc R . H14C H 0.6812(3) 0.04070(15) 0.8888(2) 0.100 Uiso 1 calc R . C15 C 0.1983(2) 0.16502(11) 1.03779(11) 0.0337(5) Uani 1 d . . H15A H 0.2073(2) 0.20787(11) 1.01404(11) 0.040 Uiso 1 calc R . C16 C 0.2975(3) 0.16849(14) 1.09837(12) 0.0530(7) Uani 1 d . . H16A H 0.2636(3) 0.20354(14) 1.12775(12) 0.079 Uiso 1 calc R . H16B H 0.3980(3) 0.17770(14) 1.08442(12) 0.079 Uiso 1 calc R . H16C H 0.2946(3) 0.12645(14) 1.12188(12) 0.079 Uiso 1 calc R . C17 C 0.0394(2) 0.15875(14) 1.06045(13) 0.0491(6) Uani 1 d . . H17A H 0.0163(2) 0.19453(14) 1.09107(13) 0.074 Uiso 1 calc R . H17B H 0.0258(2) 0.11653(14) 1.08281(13) 0.074 Uiso 1 calc R . H17C H -0.0258(2) 0.16118(14) 1.02199(13) 0.074 Uiso 1 calc R . C18 C 0.3300(2) 0.39800(9) 0.90780(9) 0.0243(4) Uani 1 d . . C19 C 0.1893(2) 0.40823(10) 0.93518(10) 0.0278(4) Uani 1 d . . C20 C 0.1182(2) 0.46705(11) 0.92199(11) 0.0378(5) Uani 1 d . . H20A H 0.0236(2) 0.47443(11) 0.93980(11) 0.045 Uiso 1 calc R . C21 C 0.1822(3) 0.51492(11) 0.88360(11) 0.0425(6) Uani 1 d . . H21A H 0.1317(3) 0.55481(11) 0.87510(11) 0.051 Uiso 1 calc R . C22 C 0.3193(3) 0.50482(10) 0.85761(11) 0.0390(5) Uani 1 d . . H22A H 0.3627(3) 0.53827(10) 0.83149(11) 0.047 Uiso 1 calc R . C23 C 0.3962(2) 0.44672(10) 0.86864(10) 0.0299(4) Uani 1 d . . C24 C 0.1207(2) 0.35657(10) 0.97990(10) 0.0320(5) Uani 1 d . . H24A H 0.1482(2) 0.31260(10) 0.96181(10) 0.038 Uiso 1 calc R . C25 C -0.0465(2) 0.35954(13) 0.98194(13) 0.0455(6) Uani 1 d . . H25A H -0.0834(2) 0.32520(13) 1.01144(13) 0.068 Uiso 1 calc R . H25B H -0.0858(2) 0.35272(13) 0.93736(13) 0.068 Uiso 1 calc R . H25C H -0.0774(2) 0.40262(13) 0.99834(13) 0.068 Uiso 1 calc R . C26 C 0.1810(3) 0.36046(13) 1.05019(11) 0.0468(6) Uani 1 d . . H26A H 0.1346(3) 0.32666(13) 1.07750(11) 0.070 Uiso 1 calc R . H26B H 0.1601(3) 0.40388(13) 1.06873(11) 0.070 Uiso 1 calc R . H26C H 0.2871(3) 0.35332(13) 1.04947(11) 0.070 Uiso 1 calc R . C27 C 0.5475(2) 0.43959(10) 0.83785(11) 0.0354(5) Uani 1 d . . H27A H 0.5872(2) 0.39558(10) 0.85050(11) 0.042 Uiso 1 calc R . C28 C 0.6546(3) 0.49205(13) 0.86305(14) 0.0532(7) Uani 1 d . . H28A H 0.7502(3) 0.48575(13) 0.84213(14) 0.080 Uiso 1 calc R . H28B H 0.6651(3) 0.48815(13) 0.91110(14) 0.080 Uiso 1 calc R . H28C H 0.6169(3) 0.53574(13) 0.85200(14) 0.080 Uiso 1 calc R . C29 C 0.5417(3) 0.44311(13) 0.76202(12) 0.0495(6) Uani 1 d . . H29A H 0.6408(3) 0.43835(13) 0.74419(12) 0.074 Uiso 1 calc R . H29B H 0.5011(3) 0.48556(13) 0.74844(12) 0.074 Uiso 1 calc R . H29C H 0.4795(3) 0.40768(13) 0.74508(12) 0.074 Uiso 1 calc R . N30 N 0.1769(2) 0.24697(8) 0.79702(8) 0.0249(4) Uani 1 d . . Si31 Si -0.00628(6) 0.23349(3) 0.80326(3) 0.0352(2) Uani 1 d . . C32 C -0.1150(3) 0.3110(2) 0.79527(14) 0.0634(8) Uani 1 d . . H32A H -0.0955(3) 0.3312(2) 0.75222(14) 0.095 Uiso 1 calc R . H32B H -0.0869(3) 0.3415(2) 0.83054(14) 0.095 Uiso 1 calc R . H32C H -0.2195(3) 0.3008(2) 0.79885(14) 0.095 Uiso 1 calc R . C33 C -0.0470(3) 0.19704(14) 0.88570(13) 0.0524(6) Uani 1 d . . H33A H -0.0097(3) 0.22606(14) 0.92052(13) 0.079 Uiso 1 calc R . H33B H 0.0004(3) 0.15404(14) 0.88930(13) 0.079 Uiso 1 calc R . H33C H -0.1530(3) 0.19187(14) 0.89063(13) 0.079 Uiso 1 calc R . C34 C -0.0804(3) 0.1755(2) 0.7399(2) 0.0719(9) Uani 1 d . . H34A H -0.0612(3) 0.1929(2) 0.6956(2) 0.108 Uiso 1 calc R . H34B H -0.1862(3) 0.1705(2) 0.7461(2) 0.108 Uiso 1 calc R . H34C H -0.0327(3) 0.1327(2) 0.7448(2) 0.108 Uiso 1 calc R . Si35 Si 0.26825(6) 0.26859(3) 0.72726(3) 0.0277(2) Uani 1 d . . C36 C 0.4688(2) 0.26891(11) 0.74981(11) 0.0359(5) Uani 1 d . . H36A H 0.4851(2) 0.29879(11) 0.78706(11) 0.054 Uiso 1 calc R . H36B H 0.5263(2) 0.28363(11) 0.71177(11) 0.054 Uiso 1 calc R . H36C H 0.4992(2) 0.22446(11) 0.76229(11) 0.054 Uiso 1 calc R . C37 C 0.2138(3) 0.35146(12) 0.69531(12) 0.0450(6) Uani 1 d . . H37A H 0.2225(3) 0.38390(12) 0.73086(12) 0.068 Uiso 1 calc R . H37B H 0.1123(3) 0.34995(12) 0.67967(12) 0.068 Uiso 1 calc R . H37C H 0.2781(3) 0.36385(12) 0.65871(12) 0.068 Uiso 1 calc R . C38 C 0.2479(3) 0.21052(13) 0.65611(11) 0.0485(6) Uani 1 d . . H38A H 0.2752(3) 0.16617(13) 0.67027(11) 0.073 Uiso 1 calc R . H38B H 0.3119(3) 0.22445(13) 0.61993(11) 0.073 Uiso 1 calc R . H38C H 0.1460(3) 0.21055(13) 0.64090(11) 0.073 Uiso 1 calc R . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mg 0.0217(3) 0.0202(3) 0.0235(3) -0.0006(2) -0.0043(2) -0.0002(2) C1 0.0201(9) 0.0286(10) 0.0226(9) 0.0021(8) 0.0020(7) 0.0009(8) N1 0.0217(8) 0.0207(8) 0.0222(8) 0.0003(6) -0.0011(6) -0.0011(6) C2 0.0177(9) 0.0306(10) 0.0294(10) -0.0001(8) -0.0044(8) -0.0025(8) C3 0.0203(9) 0.0259(10) 0.0260(10) -0.0014(8) 0.0021(7) -0.0045(7) N3 0.0195(8) 0.0209(8) 0.0247(8) -0.0014(6) -0.0006(6) -0.0005(6) C4 0.0252(10) 0.0332(11) 0.0360(11) 0.0047(9) -0.0062(8) 0.0027(8) C5 0.0323(11) 0.0294(11) 0.0419(12) -0.0054(9) -0.0112(9) -0.0036(9) C6 0.0245(9) 0.0216(9) 0.0301(10) 0.0039(8) -0.0077(8) 0.0013(7) C7 0.0369(11) 0.0258(10) 0.0344(11) -0.0004(8) -0.0085(9) 0.0040(8) C8 0.0510(14) 0.0240(11) 0.0587(15) -0.0059(10) -0.0118(12) 0.0015(10) C9 0.0451(14) 0.0232(11) 0.079(2) 0.0071(11) -0.0134(13) -0.0063(10) C10 0.0311(11) 0.0337(12) 0.0602(15) 0.0145(11) -0.0016(10) -0.0054(9) C11 0.0236(10) 0.0277(10) 0.0350(11) 0.0070(8) -0.0051(8) -0.0017(8) C12 0.0594(15) 0.0317(12) 0.0341(12) -0.0046(9) 0.0034(11) 0.0089(11) C13 0.107(3) 0.056(2) 0.0392(14) -0.0049(13) -0.009(2) 0.003(2) C14 0.073(2) 0.062(2) 0.064(2) 0.0011(14) 0.020(2) 0.032(2) C15 0.0282(11) 0.0355(11) 0.0375(11) 0.0047(9) 0.0051(9) -0.0026(9) C16 0.0431(14) 0.072(2) 0.0437(14) -0.0102(13) -0.0018(11) 0.0004(13) C17 0.0337(13) 0.066(2) 0.0474(14) 0.0017(12) 0.0094(10) -0.0013(11) C18 0.0253(10) 0.0202(9) 0.0275(10) -0.0059(7) -0.0042(8) 0.0003(7) C19 0.0268(10) 0.0274(10) 0.0293(10) -0.0053(8) -0.0011(8) 0.0011(8) C20 0.0345(11) 0.0354(12) 0.0436(12) -0.0056(10) 0.0007(9) 0.0117(9) C21 0.0520(14) 0.0309(12) 0.0447(13) 0.0013(10) -0.0013(11) 0.0165(10) C22 0.0515(14) 0.0258(11) 0.0396(12) 0.0029(9) 0.0014(10) 0.0030(10) C23 0.0340(11) 0.0236(10) 0.0322(11) -0.0027(8) 0.0004(8) -0.0024(8) C24 0.0246(10) 0.0308(11) 0.0407(12) -0.0063(9) 0.0064(9) -0.0016(8) C25 0.0271(11) 0.0547(15) 0.0548(15) -0.0137(12) 0.0084(10) -0.0039(10) C26 0.0412(13) 0.059(2) 0.0407(13) 0.0080(11) 0.0032(10) -0.0091(11) C27 0.0350(11) 0.0273(11) 0.0438(12) 0.0022(9) 0.0076(9) -0.0058(9) C28 0.0459(14) 0.0447(14) 0.069(2) 0.0006(12) 0.0025(12) -0.0189(11) C29 0.056(2) 0.0450(14) 0.0479(14) 0.0003(11) 0.0171(12) -0.0088(12) N30 0.0232(8) 0.0283(8) 0.0231(8) -0.0005(7) -0.0040(6) -0.0013(6) Si31 0.0241(3) 0.0490(4) 0.0324(3) -0.0043(3) -0.0043(2) -0.0056(2) C32 0.0399(14) 0.093(2) 0.058(2) 0.003(2) -0.0029(12) 0.0228(14) C33 0.0431(14) 0.064(2) 0.0502(15) 0.0055(13) 0.0080(11) -0.0132(12) C34 0.048(2) 0.100(3) 0.067(2) -0.027(2) -0.0041(14) -0.032(2) Si35 0.0298(3) 0.0304(3) 0.0229(3) 0.0020(2) -0.0031(2) -0.0012(2) C36 0.0313(11) 0.0403(12) 0.0360(12) 0.0033(9) 0.0038(9) -0.0006(9) C37 0.0426(13) 0.0431(13) 0.0494(14) 0.0176(11) -0.0046(11) 0.0007(10) C38 0.060(2) 0.057(2) 0.0293(11) -0.0079(11) 0.0018(11) -0.0073(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mg N30 1.961(2) . ? Mg N1 2.013(2) . ? Mg N3 2.044(2) . ? C1 N1 1.337(2) . ? C1 C2 1.397(3) . ? C1 C4 1.515(3) . ? N1 C6 1.438(2) . ? C2 C3 1.411(3) . ? C3 N3 1.325(2) . ? C3 C5 1.513(3) . ? N3 C18 1.436(2) . ? C6 C7 1.404(3) . ? C6 C11 1.409(3) . ? C7 C8 1.391(3) . ? C7 C12 1.520(3) . ? C8 C9 1.369(4) . ? C9 C10 1.376(4) . ? C10 C11 1.392(3) . ? C11 C15 1.520(3) . ? C12 C13 1.528(3) . ? C12 C14 1.529(3) . ? C15 C16 1.524(3) . ? C15 C17 1.529(3) . ? C18 C23 1.408(3) . ? C18 C19 1.416(3) . ? C19 C20 1.389(3) . ? C19 C24 1.524(3) . ? C20 C21 1.378(3) . ? C21 C22 1.375(3) . ? C22 C23 1.394(3) . ? C23 C27 1.525(3) . ? C24 C26 1.526(3) . ? C24 C25 1.530(3) . ? C27 C28 1.535(3) . ? C27 C29 1.537(3) . ? N30 Si35 1.700(2) . ? N30 Si31 1.701(2) . ? Si31 C33 1.864(3) . ? Si31 C34 1.869(3) . ? Si31 C32 1.872(3) . ? Si35 C38 1.872(2) . ? Si35 C37 1.874(2) . ? Si35 C36 1.888(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 N30 Mg N1 133.57(7) . . ? N30 Mg N3 131.28(7) . . ? N1 Mg N3 95.11(6) . . ? N1 C1 C2 124.5(2) . . ? N1 C1 C4 119.6(2) . . ? C2 C1 C4 116.0(2) . . ? C1 N1 C6 118.24(15) . . ? C1 N1 Mg 120.25(12) . . ? C6 N1 Mg 121.48(12) . . ? C1 C2 C3 129.9(2) . . ? N3 C3 C2 123.8(2) . . ? N3 C3 C5 121.3(2) . . ? C2 C3 C5 114.9(2) . . ? C3 N3 C18 119.85(15) . . ? C3 N3 Mg 121.26(12) . . ? C18 N3 Mg 118.68(11) . . ? C7 C6 C11 121.0(2) . . ? C7 C6 N1 120.8(2) . . ? C11 C6 N1 118.1(2) . . ? C8 C7 C6 118.4(2) . . ? C8 C7 C12 119.3(2) . . ? C6 C7 C12 122.3(2) . . ? C9 C8 C7 121.0(2) . . ? C8 C9 C10 120.4(2) . . ? C9 C10 C11 121.2(2) . . ? C10 C11 C6 117.8(2) . . ? C10 C11 C15 120.8(2) . . ? C6 C11 C15 121.4(2) . . ? C7 C12 C13 110.6(2) . . ? C7 C12 C14 112.3(2) . . ? C13 C12 C14 110.2(2) . . ? C11 C15 C16 112.3(2) . . ? C11 C15 C17 113.5(2) . . ? C16 C15 C17 109.0(2) . . ? C23 C18 C19 120.5(2) . . ? C23 C18 N3 121.8(2) . . ? C19 C18 N3 117.6(2) . . ? C20 C19 C18 118.4(2) . . ? C20 C19 C24 121.1(2) . . ? C18 C19 C24 120.4(2) . . ? C21 C20 C19 121.3(2) . . ? C22 C21 C20 119.8(2) . . ? C21 C22 C23 121.7(2) . . ? C22 C23 C18 118.1(2) . . ? C22 C23 C27 118.2(2) . . ? C18 C23 C27 123.7(2) . . ? C19 C24 C26 111.7(2) . . ? C19 C24 C25 113.7(2) . . ? C26 C24 C25 109.3(2) . . ? C23 C27 C28 112.1(2) . . ? C23 C27 C29 112.0(2) . . ? C28 C27 C29 108.6(2) . . ? Si35 N30 Si31 126.05(9) . . ? Si35 N30 Mg 108.56(8) . . ? Si31 N30 Mg 124.63(9) . . ? N30 Si31 C33 109.22(10) . . ? N30 Si31 C34 113.95(11) . . ? C33 Si31 C34 106.80(14) . . ? N30 Si31 C32 112.30(12) . . ? C33 Si31 C32 107.83(13) . . ? C34 Si31 C32 106.4(2) . . ? N30 Si35 C38 115.28(10) . . ? N30 Si35 C37 112.92(10) . . ? C38 Si35 C37 106.16(12) . . ? N30 Si35 C36 106.17(9) . . ? C38 Si35 C36 106.39(11) . . ? C37 Si35 C36 109.69(10) . . ? _refine_diff_density_max 0.290 _refine_diff_density_min -0.235 _refine_diff_density_rms 0.043 #===END data_Compound_14 _database_code_CSD 207275 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C62 H88 Mg2 N4 O4' _chemical_formula_weight 1001.98 _chemical_melting_point ? _chemical_compound_source ? 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 Monoclinic _symmetry_space_group_name_H-M P2(1)/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 17.316(2) _cell_length_b 15.1884(13) _cell_length_c 23.294(3) _cell_angle_alpha 90.00 _cell_angle_beta 101.725(13) _cell_angle_gamma 90.00 _cell_volume 5998.5(11) _cell_formula_units_Z 4 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used 28 _cell_measurement_theta_min 11.23 _cell_measurement_theta_max 25.03 _exptl_crystal_description blocks _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.37 _exptl_crystal_size_min 0.33 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.109 _exptl_crystal_density_method ? _exptl_crystal_F_000 2176 _exptl_absorpt_coefficient_mu 0.717 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 183(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 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9232 _diffrn_reflns_av_R_equivalents 0.0495 _diffrn_reflns_av_sigmaI/netI 0.0481 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.61 _diffrn_reflns_theta_max 60.01 _reflns_number_total 8890 _reflns_number_observed 6539 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 725 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0740P)^2^+1.0806P] 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 ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00042(6) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 8165 _refine_ls_number_parameters 656 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0790 _refine_ls_R_factor_obs 0.0524 _refine_ls_wR_factor_all 0.1476 _refine_ls_wR_factor_obs 0.1263 _refine_ls_goodness_of_fit_all 1.038 _refine_ls_goodness_of_fit_obs 1.092 _refine_ls_restrained_S_all 1.083 _refine_ls_restrained_S_obs 1.092 _refine_ls_shift/esd_max -0.048 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Mg Mg 0.24122(5) 0.10614(5) 0.30213(3) 0.0280(2) Uani 1 d . . O1 O 0.14989(12) 0.03463(13) 0.26971(9) 0.0480(5) Uani 1 d . . O2 O 0.33888(11) 0.05105(13) 0.29601(9) 0.0466(5) Uani 1 d . . N1 N 0.23045(12) 0.23226(13) 0.27144(8) 0.0287(4) Uani 1 d . . C1 C 0.19674(14) 0.2932(2) 0.29893(10) 0.0297(5) Uani 1 d . . C2 C 0.17751(14) 0.2817(2) 0.35422(11) 0.0311(5) Uani 1 d . . H2A H 0.14410(14) 0.3256(2) 0.36506(11) 0.037 Uiso 1 calc R . C3 C 0.20033(13) 0.2150(2) 0.39567(10) 0.0284(5) Uani 1 d . . N3 N 0.23823(11) 0.14213(12) 0.38570(8) 0.0275(4) Uani 1 d . . C4 C 0.1771(2) 0.3830(2) 0.27117(12) 0.0424(6) Uani 1 d . . H4A H 0.2193(6) 0.4015(7) 0.2514(8) 0.064 Uiso 1 calc R . H4B H 0.1720(13) 0.4258(4) 0.3016(2) 0.064 Uiso 1 calc R . H4C H 0.1272(7) 0.3795(4) 0.2425(7) 0.064 Uiso 1 calc R . C5 C 0.1817(2) 0.2308(2) 0.45528(11) 0.0402(6) Uani 1 d . . H5A H 0.1521(11) 0.1806(7) 0.4661(4) 0.060 Uiso 1 calc R . H5B H 0.1500(11) 0.2845(8) 0.4542(3) 0.060 Uiso 1 calc R . H5C H 0.2310(2) 0.2378(14) 0.4843(2) 0.060 Uiso 1 calc R . C6 C 0.25255(15) 0.2563(2) 0.21734(11) 0.0332(5) Uani 1 d . . C7 C 0.1973(2) 0.2511(2) 0.16455(11) 0.0405(6) Uani 1 d . . C8 C 0.2195(2) 0.2797(2) 0.11337(13) 0.0545(8) Uani 1 d . . H8A H 0.1823(2) 0.2780(2) 0.07727(13) 0.065 Uiso 1 calc R . C9 C 0.2945(2) 0.3104(3) 0.11445(13) 0.0598(9) Uani 1 d . . H9A H 0.3081(2) 0.3319(3) 0.07949(13) 0.072 Uiso 1 calc R . C10 C 0.3500(2) 0.3100(2) 0.16586(14) 0.0527(7) Uani 1 d . . H10A H 0.4023(2) 0.3288(2) 0.16555(14) 0.063 Uiso 1 calc R . C11 C 0.3311(2) 0.2827(2) 0.21845(12) 0.0395(6) Uani 1 d . . C12 C 0.1144(2) 0.2156(2) 0.16037(12) 0.0455(7) Uani 1 d . . H12A H 0.1071(2) 0.2036(2) 0.20115(12) 0.055 Uiso 1 calc R . C13 C 0.1037(2) 0.1285(3) 0.1268(2) 0.0652(9) Uani 1 d . . H13A H 0.0500(2) 0.1067(3) 0.1246(2) 0.098 Uiso 1 calc R . H13B H 0.1416(2) 0.0852(3) 0.1472(2) 0.098 Uiso 1 calc R . H13C H 0.1129(2) 0.1378(3) 0.0871(2) 0.098 Uiso 1 calc R . C14 C 0.0506(2) 0.2810(3) 0.1323(2) 0.0684(10) Uani 1 d . . H14A H -0.0016(2) 0.2549(3) 0.1307(2) 0.103 Uiso 1 calc R . H14B H 0.0571(2) 0.2950(3) 0.0925(2) 0.103 Uiso 1 calc R . H14C H 0.0554(2) 0.3350(3) 0.1558(2) 0.103 Uiso 1 calc R . C15 C 0.3931(2) 0.2800(2) 0.27466(13) 0.0456(7) Uani 1 d . . H15A H 0.3772(2) 0.2327(2) 0.29985(13) 0.055 Uiso 1 calc R . C16 C 0.3964(2) 0.3661(3) 0.3088(2) 0.0636(9) Uani 1 d . . H16A H 0.4370(2) 0.3620(3) 0.3447(2) 0.095 Uiso 1 calc R . H16B H 0.3450(2) 0.3772(3) 0.3189(2) 0.095 Uiso 1 calc R . H16C H 0.4091(2) 0.4146(3) 0.2845(2) 0.095 Uiso 1 calc R . C17 C 0.4748(2) 0.2560(3) 0.2644(2) 0.0650(9) Uani 1 d . . H17A H 0.5125(2) 0.2552(3) 0.3020(2) 0.097 Uiso 1 calc R . H17B H 0.4915(2) 0.2998(3) 0.2385(2) 0.097 Uiso 1 calc R . H17C H 0.4730(2) 0.1977(3) 0.2462(2) 0.097 Uiso 1 calc R . C18 C 0.27484(15) 0.0905(2) 0.43526(10) 0.0305(5) Uani 1 d . . C19 C 0.3534(2) 0.1097(2) 0.46181(11) 0.0354(5) Uani 1 d . . C20 C 0.3900(2) 0.0594(2) 0.50952(12) 0.0448(6) Uani 1 d . . H20A H 0.4434(2) 0.0709(2) 0.52735(12) 0.054 Uiso 1 calc R . C21 C 0.3497(2) -0.0072(2) 0.53139(14) 0.0537(8) Uani 1 d . . H21A H 0.3748(2) -0.0401(2) 0.56464(14) 0.064 Uiso 1 calc R . C22 C 0.2733(2) -0.0253(2) 0.50478(15) 0.0537(8) Uani 1 d . . H22A H 0.2461(2) -0.0712(2) 0.52001(15) 0.064 Uiso 1 calc R . C23 C 0.2346(2) 0.0213(2) 0.45632(13) 0.0413(6) Uani 1 d . . C24 C 0.3982(2) 0.1845(2) 0.43974(12) 0.0437(6) Uani 1 d . . H24A H 0.3671(2) 0.2029(2) 0.40061(12) 0.052 Uiso 1 calc R . C25 C 0.4785(2) 0.1567(3) 0.4312(2) 0.0735(10) Uani 1 d . . H25A H 0.4732(2) 0.1053(3) 0.4053(2) 0.110 Uiso 1 calc R . H25B H 0.5116(2) 0.1416(3) 0.4692(2) 0.110 Uiso 1 calc R . H25C H 0.5028(2) 0.2052(3) 0.4135(2) 0.110 Uiso 1 calc R . C26 C 0.4053(3) 0.2636(3) 0.4795(3) 0.099(2) Uani 1 d . . H26A H 0.3528(3) 0.2812(3) 0.4848(3) 0.148 Uiso 1 calc R . H26B H 0.4295(3) 0.3123(3) 0.4619(3) 0.148 Uiso 1 calc R . H26C H 0.4383(3) 0.2487(3) 0.5176(3) 0.148 Uiso 1 calc R . C27 C 0.1512(2) -0.0038(2) 0.4270(2) 0.0551(8) Uani 1 d . . H27A H 0.1319(2) 0.0407(2) 0.3957(2) 0.066 Uiso 1 calc R . C28 C 0.0944(2) -0.0032(3) 0.4696(2) 0.0814(13) Uani 1 d . . H28A H 0.0415(2) -0.0198(3) 0.4486(2) 0.122 Uiso 1 calc R . H28B H 0.0928(2) 0.0560(3) 0.4861(2) 0.122 Uiso 1 calc R . H28C H 0.1127(2) -0.0454(3) 0.5013(2) 0.122 Uiso 1 calc R . C29 C 0.1503(2) -0.0939(2) 0.3975(2) 0.0758(11) Uani 1 d . . H29A H 0.0960(2) -0.1091(2) 0.3788(2) 0.114 Uiso 1 calc R . H29B H 0.1711(2) -0.1384(2) 0.4271(2) 0.114 Uiso 1 calc R . H29C H 0.1830(2) -0.0919(2) 0.3678(2) 0.114 Uiso 1 calc R . C30 C 0.1239(2) -0.0337(2) 0.24293(12) 0.0379(6) Uani 1 d . . C31 C 0.0388(2) -0.0555(3) 0.2389(2) 0.0743(12) Uani 1 d . . H31A H 0.0335(3) -0.1182(6) 0.2472(14) 0.111 Uiso 1 calc R . H31B H 0.0093(4) -0.0422(21) 0.1993(5) 0.111 Uiso 1 calc R . H31C H 0.0178(6) -0.0203(17) 0.2675(11) 0.111 Uiso 1 calc R . Mg' Mg 0.26015(5) -0.13602(5) 0.20729(3) 0.0292(2) Uani 1 d . . O1' O 0.35152(12) -0.07341(14) 0.24924(9) 0.0501(5) Uani 1 d . . O2' O 0.16348(12) -0.08497(13) 0.21885(9) 0.0473(5) Uani 1 d . . N1' N 0.26484(12) -0.26694(13) 0.22677(9) 0.0320(4) Uani 1 d . . C1' C 0.30282(14) -0.3215(2) 0.19743(11) 0.0320(5) Uani 1 d . . C2' C 0.32421(14) -0.3002(2) 0.14435(11) 0.0309(5) Uani 1 d . . H2'A H 0.35907(14) -0.3406(2) 0.13160(11) 0.037 Uiso 1 calc R . C3' C 0.30174(14) -0.2277(2) 0.10701(10) 0.0297(5) Uani 1 d . . N3' N 0.26576(11) -0.15618(12) 0.12211(8) 0.0279(4) Uani 1 d . . C4' C 0.3257(2) -0.4132(2) 0.22098(13) 0.0458(7) Uani 1 d . . H4'A H 0.2851(7) -0.4357(6) 0.2410(9) 0.069 Uiso 1 calc R . H4'B H 0.3764(7) -0.4105(3) 0.2487(8) 0.069 Uiso 1 calc R . H4'C H 0.3302(13) -0.4524(4) 0.1884(2) 0.069 Uiso 1 calc R . C5' C 0.3185(2) -0.2350(2) 0.04614(11) 0.0398(6) Uani 1 d . . H5'A H 0.2696(3) -0.2259(14) 0.01713(11) 0.060 Uiso 1 calc R . H5'B H 0.3396(12) -0.2936(5) 0.0408(3) 0.060 Uiso 1 calc R . H5'C H 0.3573(10) -0.1902(9) 0.0409(3) 0.060 Uiso 1 calc R . C6' C 0.2319(2) -0.3001(2) 0.27445(12) 0.0428(6) Uani 1 d . . C7' C 0.2760(2) -0.2984(2) 0.33178(13) 0.0549(8) Uani 1 d . . C8' C 0.2392(3) -0.3292(3) 0.3762(2) 0.0790(13) Uani 1 d . . H8'A H 0.2680(3) -0.3299(3) 0.4155(2) 0.095 Uiso 1 calc R . C9' C 0.1628(3) -0.3581(3) 0.3643(2) 0.092(2) Uani 1 d . . H9'A H 0.1395(3) -0.3789(3) 0.3953(2) 0.110 Uiso 1 calc R . C10' C 0.1200(3) -0.3573(3) 0.3084(2) 0.0756(12) Uani 1 d . . H10B H 0.0667(3) -0.3768(3) 0.3011(2) 0.091 Uiso 1 calc R . C11' C 0.1526(2) -0.3285(2) 0.2616(2) 0.0531(8) Uani 1 d . . C12' C 0.3595(2) -0.2651(3) 0.34668(14) 0.0692(10) Uani 1 d . . H12B H 0.3754(2) -0.2495(3) 0.30903(14) 0.083 Uiso 1 calc R . C13' C 0.3664(3) -0.1816(4) 0.3842(2) 0.0868(13) Uani 1 d . . H13D H 0.4214(3) -0.1618(4) 0.3931(2) 0.130 Uiso 1 calc R . H13E H 0.3491(3) -0.1942(4) 0.4209(2) 0.130 Uiso 1 calc R . H13F H 0.3331(3) -0.1352(4) 0.3628(2) 0.130 Uiso 1 calc R . C14' C 0.4174(3) -0.3352(4) 0.3774(2) 0.115(2) Uani 1 d . . H14D H 0.4709(3) -0.3106(4) 0.3862(2) 0.172 Uiso 1 calc R . H14E H 0.4162(3) -0.3863(4) 0.3516(2) 0.172 Uiso 1 calc R . H14F H 0.4022(3) -0.3533(4) 0.4139(2) 0.172 Uiso 1 calc R . C15' C 0.1043(2) -0.3301(2) 0.1997(2) 0.0644(10) Uani 1 d . . H15B H 0.1253(2) -0.2824(2) 0.1775(2) 0.077 Uiso 1 calc R . C16' C 0.1131(2) -0.4157(3) 0.1685(2) 0.0771(11) Uani 1 d . . H16D H 0.0809(2) -0.4137(3) 0.1287(2) 0.116 Uiso 1 calc R . H16E H 0.0955(2) -0.4647(3) 0.1901(2) 0.116 Uiso 1 calc R . H16F H 0.1686(2) -0.4244(3) 0.1664(2) 0.116 Uiso 1 calc R . C17' C 0.0166(2) -0.3110(3) 0.1958(3) 0.094(2) Uani 1 d . . H17D H 0.0106(2) -0.2556(3) 0.2159(3) 0.141 Uiso 1 calc R . H17E H -0.0071(2) -0.3591(3) 0.2143(3) 0.141 Uiso 1 calc R . H17F H -0.0099(2) -0.3063(3) 0.1545(3) 0.141 Uiso 1 calc R . C18' C 0.2359(2) -0.0934(2) 0.07694(10) 0.0315(5) Uani 1 d . . C19' C 0.1558(2) -0.0983(2) 0.04928(11) 0.0350(5) Uani 1 d . . C20' C 0.1272(2) -0.0401(2) 0.00424(12) 0.0446(6) Uani 1 d . . H20B H 0.0735(2) -0.0432(2) -0.01518(12) 0.054 Uiso 1 calc R . C21' C 0.1760(2) 0.0226(2) -0.01281(14) 0.0536(8) Uani 1 d . . H21B H 0.1563(2) 0.0607(2) -0.04474(14) 0.064 Uiso 1 calc R . C22' C 0.2530(2) 0.0295(2) 0.01653(15) 0.0533(8) Uani 1 d . . H22B H 0.2852(2) 0.0745(2) 0.00548(15) 0.064 Uiso 1 calc R . C23' C 0.2855(2) -0.0274(2) 0.06194(12) 0.0403(6) Uani 1 d . . C24' C 0.1014(2) -0.1664(2) 0.06774(12) 0.0403(6) Uani 1 d . . H24B H 0.1258(2) -0.1847(2) 0.10864(12) 0.048 Uiso 1 calc R . C25' C 0.0206(2) -0.1294(3) 0.0694(2) 0.0666(9) Uani 1 d . . H25D H 0.0264(2) -0.0766(3) 0.0941(2) 0.100 Uiso 1 calc R . H25E H -0.0103(2) -0.1736(3) 0.0856(2) 0.100 Uiso 1 calc R . H25F H -0.0066(2) -0.1140(3) 0.0295(2) 0.100 Uiso 1 calc R . C26' C 0.0951(3) -0.2480(2) 0.0301(2) 0.0802(12) Uani 1 d . . H26D H 0.1481(3) -0.2705(2) 0.0298(2) 0.120 Uiso 1 calc R . H26E H 0.0684(3) -0.2334(2) -0.0101(2) 0.120 Uiso 1 calc R . H26F H 0.0648(3) -0.2930(2) 0.0460(2) 0.120 Uiso 1 calc R . C27' C 0.3691(2) -0.0154(2) 0.09471(14) 0.0501(7) Uani 1 d . . H27B H 0.3829(2) -0.0672(2) 0.12130(14) 0.060 Uiso 1 calc R . C28' C 0.4290(2) -0.0115(3) 0.0542(2) 0.0663(9) Uani 1 d . . H28D H 0.4822(2) -0.0037(3) 0.0778(2) 0.099 Uiso 1 calc R . H28E H 0.4162(2) 0.0382(3) 0.0270(2) 0.099 Uiso 1 calc R . H28F H 0.4268(2) -0.0664(3) 0.0318(2) 0.099 Uiso 1 calc R . C29' C 0.3759(2) 0.0672(3) 0.1330(2) 0.0689(10) Uani 1 d . . H29D H 0.4306(2) 0.0742(3) 0.1541(2) 0.103 Uiso 1 calc R . H29E H 0.3413(2) 0.0615(3) 0.1613(2) 0.103 Uiso 1 calc R . H29F H 0.3602(2) 0.1189(3) 0.1081(2) 0.103 Uiso 1 calc R . C30' C 0.3792(2) -0.0083(2) 0.27898(12) 0.0405(6) Uani 1 d . . C31' C 0.4674(2) -0.0005(3) 0.2963(2) 0.0750(12) Uani 1 d . . H31D H 0.4912(2) -0.0188(21) 0.2635(5) 0.112 Uiso 1 calc R . H31E H 0.4867(3) -0.0385(17) 0.3302(9) 0.112 Uiso 1 calc R . H31F H 0.4817(2) 0.0607(5) 0.3066(14) 0.112 Uiso 1 calc R . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mg 0.0323(4) 0.0238(4) 0.0305(4) -0.0034(3) 0.0128(3) 0.0020(3) O1 0.0470(11) 0.0395(11) 0.0588(12) -0.0159(9) 0.0137(9) -0.0083(9) O2 0.0413(10) 0.0457(11) 0.0563(12) -0.0089(9) 0.0184(9) 0.0109(9) N1 0.0342(10) 0.0289(10) 0.0248(9) 0.0007(8) 0.0103(8) 0.0006(8) C1 0.0315(12) 0.0277(12) 0.0303(12) 0.0015(10) 0.0070(9) 0.0033(9) C2 0.0349(12) 0.0271(12) 0.0330(12) -0.0027(10) 0.0110(10) 0.0065(10) C3 0.0285(11) 0.0279(12) 0.0310(12) -0.0031(9) 0.0110(9) 0.0001(9) N3 0.0310(10) 0.0233(9) 0.0313(10) -0.0004(8) 0.0136(8) 0.0017(8) C4 0.056(2) 0.0320(13) 0.0422(14) 0.0087(11) 0.0158(12) 0.0088(12) C5 0.054(2) 0.0358(14) 0.0341(13) 0.0006(10) 0.0176(12) 0.0138(12) C6 0.0385(13) 0.0308(12) 0.0335(13) 0.0030(10) 0.0145(11) 0.0024(10) C7 0.0451(15) 0.0461(15) 0.0327(13) 0.0014(11) 0.0132(11) 0.0043(12) C8 0.059(2) 0.072(2) 0.0348(15) 0.0078(14) 0.0163(13) 0.002(2) C9 0.072(2) 0.075(2) 0.038(2) 0.011(2) 0.026(2) -0.005(2) C10 0.055(2) 0.058(2) 0.051(2) 0.0099(14) 0.0265(14) -0.0064(15) C11 0.0410(14) 0.0390(14) 0.0420(14) 0.0046(11) 0.0167(12) -0.0027(11) C12 0.0392(14) 0.061(2) 0.0357(14) 0.0003(13) 0.0070(11) 0.0009(13) C13 0.067(2) 0.070(2) 0.059(2) -0.014(2) 0.014(2) -0.011(2) C14 0.048(2) 0.082(3) 0.070(2) 0.000(2) -0.001(2) 0.011(2) C15 0.0420(15) 0.047(2) 0.049(2) 0.0104(13) 0.0121(12) -0.0085(13) C16 0.056(2) 0.068(2) 0.064(2) -0.009(2) 0.005(2) -0.007(2) C17 0.048(2) 0.067(2) 0.080(2) 0.015(2) 0.014(2) 0.002(2) C18 0.0392(13) 0.0245(11) 0.0311(12) 0.0022(9) 0.0150(10) 0.0060(10) C19 0.0402(14) 0.0340(13) 0.0343(13) 0.0016(10) 0.0134(11) 0.0073(11) C20 0.046(2) 0.048(2) 0.0398(14) 0.0074(12) 0.0073(12) 0.0111(13) C21 0.064(2) 0.047(2) 0.052(2) 0.0217(14) 0.0153(15) 0.0174(15) C22 0.066(2) 0.037(2) 0.065(2) 0.0222(14) 0.027(2) 0.0083(14) C23 0.048(2) 0.0308(13) 0.050(2) 0.0094(11) 0.0213(13) 0.0061(11) C24 0.0364(14) 0.050(2) 0.0435(15) 0.0082(12) 0.0048(11) -0.0045(12) C25 0.059(2) 0.083(3) 0.088(3) -0.006(2) 0.038(2) -0.009(2) C26 0.120(4) 0.046(2) 0.152(5) -0.027(2) 0.081(4) -0.027(2) C27 0.047(2) 0.045(2) 0.076(2) 0.020(2) 0.018(2) -0.0052(13) C28 0.056(2) 0.077(3) 0.122(4) 0.031(3) 0.044(2) 0.000(2) C29 0.075(2) 0.052(2) 0.099(3) 0.003(2) 0.014(2) -0.021(2) C30 0.0338(13) 0.0344(14) 0.0478(15) -0.0100(12) 0.0138(11) -0.0002(11) C31 0.040(2) 0.071(2) 0.117(3) -0.045(2) 0.030(2) -0.015(2) Mg' 0.0324(4) 0.0272(4) 0.0301(4) -0.0042(3) 0.0114(3) 0.0018(3) O1' 0.0455(11) 0.0500(12) 0.0539(12) -0.0192(10) 0.0082(9) -0.0063(9) O2' 0.0436(10) 0.0481(11) 0.0539(11) -0.0098(9) 0.0184(9) 0.0122(9) N1' 0.0360(11) 0.0321(11) 0.0303(10) 0.0032(8) 0.0122(8) 0.0047(9) C1' 0.0308(12) 0.0299(12) 0.0351(12) 0.0015(10) 0.0064(10) 0.0051(10) C2' 0.0323(12) 0.0264(12) 0.0357(12) -0.0039(10) 0.0109(10) 0.0064(10) C3' 0.0320(12) 0.0277(12) 0.0317(12) -0.0035(9) 0.0114(10) -0.0006(10) N3' 0.0333(10) 0.0233(9) 0.0284(9) 0.0001(8) 0.0097(8) 0.0010(8) C4' 0.057(2) 0.0346(14) 0.049(2) 0.0108(12) 0.0181(13) 0.0157(13) C5' 0.056(2) 0.0337(13) 0.0347(13) -0.0012(11) 0.0200(12) 0.0071(12) C6' 0.053(2) 0.0373(14) 0.0437(15) 0.0123(12) 0.0235(13) 0.0163(12) C7' 0.073(2) 0.060(2) 0.0366(15) 0.0086(13) 0.0203(14) 0.025(2) C8' 0.125(4) 0.077(3) 0.043(2) 0.014(2) 0.038(2) 0.026(3) C9' 0.139(4) 0.078(3) 0.082(3) 0.021(2) 0.080(3) 0.006(3) C10' 0.091(3) 0.064(2) 0.089(3) 0.023(2) 0.060(2) 0.003(2) C11' 0.058(2) 0.041(2) 0.070(2) 0.0183(14) 0.036(2) 0.0082(14) C12' 0.073(2) 0.098(3) 0.033(2) 0.000(2) 0.0048(15) 0.027(2) C13' 0.095(3) 0.114(4) 0.049(2) -0.012(2) 0.009(2) 0.005(3) C14' 0.110(4) 0.149(5) 0.071(3) 0.002(3) -0.017(3) 0.067(4) C15' 0.048(2) 0.059(2) 0.085(2) 0.033(2) 0.013(2) -0.007(2) C16' 0.060(2) 0.094(3) 0.077(3) 0.005(2) 0.014(2) -0.006(2) C17' 0.055(2) 0.057(2) 0.165(5) 0.028(3) 0.010(3) 0.002(2) C18' 0.0427(13) 0.0233(11) 0.0311(12) -0.0006(9) 0.0136(10) 0.0042(10) C19' 0.0455(14) 0.0285(12) 0.0318(12) -0.0008(10) 0.0098(11) 0.0044(11) C20' 0.057(2) 0.0362(14) 0.0393(14) 0.0043(11) 0.0057(12) 0.0090(13) C21' 0.078(2) 0.037(2) 0.046(2) 0.0160(13) 0.015(2) 0.0127(15) C22' 0.073(2) 0.0341(15) 0.059(2) 0.0112(13) 0.027(2) -0.0030(14) C23' 0.054(2) 0.0297(13) 0.0422(14) 0.0034(11) 0.0208(12) -0.0008(12) C24' 0.0372(13) 0.0396(14) 0.0419(14) 0.0079(11) 0.0027(11) 0.0001(11) C25' 0.051(2) 0.061(2) 0.091(3) 0.007(2) 0.022(2) 0.002(2) C26' 0.090(3) 0.048(2) 0.111(3) -0.023(2) 0.041(3) -0.019(2) C27' 0.054(2) 0.041(2) 0.058(2) 0.0044(13) 0.0190(14) -0.0097(13) C28' 0.059(2) 0.062(2) 0.086(3) 0.003(2) 0.035(2) -0.013(2) C29' 0.078(2) 0.060(2) 0.073(2) -0.014(2) 0.024(2) -0.021(2) C30' 0.0351(14) 0.0411(15) 0.0459(15) -0.0124(12) 0.0097(11) 0.0024(12) C31' 0.036(2) 0.070(2) 0.115(3) -0.045(2) 0.007(2) 0.004(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 Mg O2 1.918(2) . ? Mg O1 1.941(2) . ? Mg N3 2.033(2) . ? Mg N1 2.040(2) . ? O1 C30 1.247(3) . ? O2 C30' 1.253(3) . ? N1 C1 1.327(3) . ? N1 C6 1.437(3) . ? C1 C2 1.405(3) . ? C1 C4 1.517(3) . ? C2 C3 1.400(4) . ? C3 N3 1.331(3) . ? C3 C5 1.507(3) . ? N3 C18 1.432(3) . ? C6 C7 1.398(4) . ? C6 C11 1.413(4) . ? C7 C8 1.394(4) . ? C7 C12 1.519(4) . ? C8 C9 1.376(5) . ? C9 C10 1.375(5) . ? C10 C11 1.394(4) . ? C11 C15 1.516(4) . ? C12 C13 1.528(5) . ? C12 C14 1.530(5) . ? C15 C17 1.526(4) . ? C15 C16 1.526(5) . ? C18 C23 1.404(4) . ? C18 C19 1.406(4) . ? C19 C20 1.391(4) . ? C19 C24 1.523(4) . ? C20 C21 1.384(5) . ? C21 C22 1.369(5) . ? C22 C23 1.385(4) . ? C23 C27 1.516(4) . ? C24 C25 1.504(4) . ? C24 C26 1.507(5) . ? C27 C29 1.529(5) . ? C27 C28 1.533(5) . ? C30 O2' 1.244(3) . ? C30 C31 1.495(4) . ? Mg' O2' 1.913(2) . ? Mg' O1' 1.932(2) . ? Mg' N3' 2.029(2) . ? Mg' N1' 2.037(2) . ? O1' C30' 1.246(3) . ? N1' C1' 1.330(3) . ? N1' C6' 1.439(3) . ? C1' C2' 1.399(4) . ? C1' C4' 1.518(4) . ? C2' C3' 1.408(4) . ? C3' N3' 1.335(3) . ? C3' C5' 1.508(3) . ? N3' C18' 1.436(3) . ? C6' C7' 1.397(4) . ? C6' C11' 1.412(5) . ? C7' C8' 1.401(5) . ? C7' C12' 1.503(6) . ? C8' C9' 1.368(7) . ? C9' C10' 1.361(7) . ? C10' C11' 1.397(5) . ? C11' C15' 1.514(5) . ? C12' C13' 1.532(6) . ? C12' C14' 1.536(6) . ? C15' C16' 1.513(6) . ? C15' C17' 1.531(5) . ? C18' C19' 1.408(4) . ? C18' C23' 1.409(4) . ? C19' C20' 1.385(4) . ? C19' C24' 1.519(4) . ? C20' C21' 1.383(5) . ? C21' C22' 1.373(5) . ? C22' C23' 1.392(4) . ? C23' C27' 1.505(4) . ? C24' C26' 1.509(5) . ? C24' C25' 1.516(4) . ? C27' C29' 1.531(5) . ? C27' C28' 1.540(4) . ? C30' C31' 1.502(4) . ? 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 O2 Mg O1 112.83(9) . . ? O2 Mg N3 112.52(9) . . ? O1 Mg N3 110.24(9) . . ? O2 Mg N1 113.75(9) . . ? O1 Mg N1 112.33(9) . . ? N3 Mg N1 93.72(8) . . ? C30 O1 Mg 147.5(2) . . ? C30' O2 Mg 153.4(2) . . ? C1 N1 C6 117.9(2) . . ? C1 N1 Mg 120.3(2) . . ? C6 N1 Mg 121.6(2) . . ? N1 C1 C2 124.3(2) . . ? N1 C1 C4 120.3(2) . . ? C2 C1 C4 115.4(2) . . ? C3 C2 C1 129.5(2) . . ? N3 C3 C2 124.1(2) . . ? N3 C3 C5 119.9(2) . . ? C2 C3 C5 115.9(2) . . ? C3 N3 C18 117.9(2) . . ? C3 N3 Mg 120.0(2) . . ? C18 N3 Mg 122.11(14) . . ? C7 C6 C11 121.0(2) . . ? C7 C6 N1 120.0(2) . . ? C11 C6 N1 118.9(2) . . ? C8 C7 C6 118.5(3) . . ? C8 C7 C12 118.5(3) . . ? C6 C7 C12 123.0(2) . . ? C9 C8 C7 120.8(3) . . ? C10 C9 C8 120.3(3) . . ? C9 C10 C11 121.3(3) . . ? C10 C11 C6 117.8(3) . . ? C10 C11 C15 121.0(3) . . ? C6 C11 C15 121.2(2) . . ? C7 C12 C13 110.7(3) . . ? C7 C12 C14 112.8(3) . . ? C13 C12 C14 110.0(3) . . ? C11 C15 C17 112.9(3) . . ? C11 C15 C16 111.8(3) . . ? C17 C15 C16 110.4(3) . . ? C23 C18 C19 120.4(2) . . ? C23 C18 N3 121.4(2) . . ? C19 C18 N3 118.1(2) . . ? C20 C19 C18 118.7(2) . . ? C20 C19 C24 119.9(2) . . ? C18 C19 C24 121.3(2) . . ? C21 C20 C19 120.9(3) . . ? C22 C21 C20 119.6(3) . . ? C21 C22 C23 122.0(3) . . ? C22 C23 C18 118.4(3) . . ? C22 C23 C27 119.9(3) . . ? C18 C23 C27 121.7(2) . . ? C25 C24 C26 110.1(3) . . ? C25 C24 C19 112.6(3) . . ? C26 C24 C19 111.8(3) . . ? C23 C27 C29 110.5(3) . . ? C23 C27 C28 112.6(3) . . ? C29 C27 C28 110.3(3) . . ? O2' C30 O1 124.8(2) . . ? O2' C30 C31 117.3(3) . . ? O1 C30 C31 117.8(2) . . ? O2' Mg' O1' 112.29(9) . . ? O2' Mg' N3' 114.58(9) . . ? O1' Mg' N3' 111.82(9) . . ? O2' Mg' N1' 111.15(9) . . ? O1' Mg' N1' 112.10(10) . . ? N3' Mg' N1' 93.60(8) . . ? C30' O1' Mg' 148.7(2) . . ? C30 O2' Mg' 153.5(2) . . ? C1' N1' C6' 119.5(2) . . ? C1' N1' Mg' 119.7(2) . . ? C6' N1' Mg' 120.6(2) . . ? N1' C1' C2' 123.8(2) . . ? N1' C1' C4' 120.4(2) . . ? C2' C1' C4' 115.8(2) . . ? C1' C2' C3' 129.6(2) . . ? N3' C3' C2' 124.0(2) . . ? N3' C3' C5' 119.8(2) . . ? C2' C3' C5' 116.2(2) . . ? C3' N3' C18' 117.7(2) . . ? C3' N3' Mg' 119.9(2) . . ? C18' N3' Mg' 122.32(15) . . ? C7' C6' C11' 121.8(3) . . ? C7' C6' N1' 120.4(3) . . ? C11' C6' N1' 117.7(3) . . ? C6' C7' C8' 117.2(4) . . ? C6' C7' C12' 122.7(3) . . ? C8' C7' C12' 120.2(3) . . ? C9' C8' C7' 121.7(4) . . ? C10' C9' C8' 120.4(3) . . ? C9' C10' C11' 121.4(4) . . ? C10' C11' C6' 117.5(4) . . ? C10' C11' C15' 120.4(3) . . ? C6' C11' C15' 122.1(3) . . ? C7' C12' C13' 111.8(3) . . ? C7' C12' C14' 112.4(4) . . ? C13' C12' C14' 109.9(3) . . ? C16' C15' C11' 112.4(3) . . ? C16' C15' C17' 109.2(3) . . ? C11' C15' C17' 113.8(4) . . ? C19' C18' C23' 121.1(2) . . ? C19' C18' N3' 118.3(2) . . ? C23' C18' N3' 120.5(2) . . ? C20' C19' C18' 118.7(2) . . ? C20' C19' C24' 120.2(2) . . ? C18' C19' C24' 121.1(2) . . ? C21' C20' C19' 120.8(3) . . ? C22' C21' C20' 119.8(3) . . ? C21' C22' C23' 122.1(3) . . ? C22' C23' C18' 117.2(3) . . ? C22' C23' C27' 120.6(3) . . ? C18' C23' C27' 122.1(2) . . ? C26' C24' C25' 111.2(3) . . ? C26' C24' C19' 111.7(3) . . ? C25' C24' C19' 112.6(2) . . ? C23' C27' C29' 110.3(3) . . ? C23' C27' C28' 113.1(3) . . ? C29' C27' C28' 110.1(3) . . ? O1' C30' O2 124.8(3) . . ? O1' C30' C31' 117.9(2) . . ? O2 C30' C31' 117.3(3) . . ? _refine_diff_density_max 0.263 _refine_diff_density_min -0.198 _refine_diff_density_rms 0.044 #===END data_Compound_15 _database_code_CSD 207276 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C79 H108 N4 O4 Mg2' _chemical_formula_weight 1226.31 _chemical_melting_point ? _chemical_compound_source ? 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 Cmca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y+1/2, z+1/2' '-x, y+1/2, -z+1/2' 'x, -y, -z' 'x+1/2, y+1/2, z' '-x+1/2, -y+1, z+1/2' '-x+1/2, y+1, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x, y-1/2, -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+1/2, -y, z-1/2' '-x+1/2, y+1/2, z' _cell_length_a 17.7581(5) _cell_length_b 19.4442(8) _cell_length_c 21.618(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7464.4(8) _cell_formula_units_Z 4 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used 28 _cell_measurement_theta_min 11.20 _cell_measurement_theta_max 25.00 _exptl_crystal_description prisms _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.53 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.091 _exptl_crystal_density_method ? _exptl_crystal_F_000 2664 _exptl_absorpt_coefficient_mu 0.659 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 183(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 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3221 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0245 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 3.94 _diffrn_reflns_theta_max 63.98 _reflns_number_total 3221 _reflns_number_observed 2670 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 149 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0798P)^2^+3.9085P] 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 ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00049(9) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 3072 _refine_ls_number_parameters 266 _refine_ls_number_restraints 184 _refine_ls_R_factor_all 0.0665 _refine_ls_R_factor_obs 0.0519 _refine_ls_wR_factor_all 0.1492 _refine_ls_wR_factor_obs 0.1368 _refine_ls_goodness_of_fit_all 1.074 _refine_ls_goodness_of_fit_obs 1.113 _refine_ls_restrained_S_all 1.089 _refine_ls_restrained_S_obs 1.101 _refine_ls_shift/esd_max 0.001 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Mg Mg 0.5000 0.05587(4) 0.08365(4) 0.0294(2) Uani 1 d S . C1 C 0.42799(11) 0.07497(10) 0.20547(9) 0.0403(4) Uani 1 d . . N1 N 0.41511(9) 0.07405(8) 0.14495(7) 0.0358(4) Uani 1 d . . C2 C 0.5000 0.07192(15) 0.23222(12) 0.0426(6) Uani 1 d S . H2A H 0.5000 0.06693(15) 0.27593(12) 0.051 Uiso 1 calc SR . C3 C 0.36327(13) 0.08113(14) 0.25097(12) 0.0610(6) Uani 1 d . . H3A H 0.36339(13) 0.12719(14) 0.26937(12) 0.091 Uiso 1 d R . H3B H 0.36909(13) 0.04660(14) 0.28365(12) 0.091 Uiso 1 d R . H3C H 0.31552(13) 0.07356(14) 0.22928(12) 0.091 Uiso 1 d R . C4 C 0.33900(11) 0.08386(11) 0.12344(9) 0.0432(5) Uani 1 d . . C5 C 0.31247(13) 0.15072(13) 0.11385(12) 0.0596(6) Uani 1 d . . C6 C 0.2386(2) 0.1592(2) 0.09302(14) 0.0758(8) Uani 1 d . . H6A H 0.2193(2) 0.2042(2) 0.08701(14) 0.091 Uiso 1 calc R . C7 C 0.19375(14) 0.1039(2) 0.08117(13) 0.0769(9) Uani 1 d . . H7A H 0.14336(14) 0.1108(2) 0.06778(13) 0.092 Uiso 1 calc R . C8 C 0.22098(13) 0.0385(2) 0.08847(12) 0.0667(7) Uani 1 d . . H8A H 0.18942(13) 0.0005(2) 0.07891(12) 0.080 Uiso 1 calc R . C9 C 0.29396(12) 0.02644(13) 0.10962(9) 0.0490(5) Uani 1 d . . C10 C 0.3616(2) 0.21332(14) 0.1240(2) 0.0851(10) Uani 1 d . . H10A H 0.4133(2) 0.19703(14) 0.1351(2) 0.102 Uiso 1 calc R . C11 C 0.3320(3) 0.2570(2) 0.1776(2) 0.133(2) Uani 1 d . . H11A H 0.3647(3) 0.2972(2) 0.1832(2) 0.200 Uiso 1 calc R . H11B H 0.3317(3) 0.2295(2) 0.2156(2) 0.200 Uiso 1 calc R . H11C H 0.2807(3) 0.2724(2) 0.1683(2) 0.200 Uiso 1 calc R . C12 C 0.3677(2) 0.2569(2) 0.0658(2) 0.1141(14) Uani 1 d . . H12A H 0.3998(2) 0.2969(2) 0.0741(2) 0.171 Uiso 1 calc R . H12B H 0.3175(2) 0.2725(2) 0.0534(2) 0.171 Uiso 1 calc R . H12C H 0.3898(2) 0.2294(2) 0.0325(2) 0.171 Uiso 1 calc R . C13 C 0.32256(14) -0.04658(12) 0.11760(10) 0.0541(6) Uani 1 d . . H13A H 0.37832(14) -0.04384(12) 0.12360(10) 0.065 Uiso 1 calc R . C14 C 0.3086(2) -0.0913(2) 0.06126(14) 0.0777(8) Uani 1 d . . H14A H 0.3281(2) -0.1377(2) 0.06897(14) 0.117 Uiso 1 calc R . H14B H 0.3343(2) -0.0714(2) 0.02535(14) 0.117 Uiso 1 calc R . H14C H 0.2544(2) -0.0938(2) 0.05306(14) 0.117 Uiso 1 calc R . C15 C 0.2896(3) -0.0801(2) 0.1753(2) 0.1078(14) Uani 1 d . . H15A H 0.2991(3) -0.0506(2) 0.2113(2) 0.162 Uiso 1 calc R . H15B H 0.3134(3) -0.1250(2) 0.1818(2) 0.162 Uiso 1 calc R . H15C H 0.2353(3) -0.0863(2) 0.1700(2) 0.162 Uiso 1 calc R . C16 C 0.5000 0.10102(12) -0.04402(12) 0.0349(6) Uani 1 d S . O16 O 0.5000 0.11753(9) 0.01208(8) 0.0401(4) Uani 1 d S . O17 O 0.5000 0.03983(9) -0.06214(9) 0.0434(5) Uani 1 d S . C18 C 0.5000 0.2251(2) -0.0741(2) 0.0589(9) Uani 1 d S . H18A H 0.5000 0.2369(2) -0.0314(2) 0.071 Uiso 1 calc SR . C19 C 0.5000 0.2766(2) -0.1188(2) 0.0825(13) Uani 1 d S . H19A H 0.5000 0.3235(2) -0.1067(2) 0.099 Uiso 1 calc SR . C20 C 0.5000 0.2595(2) -0.1803(2) 0.091(2) Uani 1 d S . H20A H 0.5000 0.2947(2) -0.2107(2) 0.110 Uiso 1 calc SR . C21 C 0.5000 0.1917(2) -0.1983(2) 0.0843(13) Uani 1 d S . H21A H 0.5000 0.1803(2) -0.2410(2) 0.101 Uiso 1 calc SR . C22 C 0.5000 0.1399(2) -0.15393(14) 0.0601(9) Uani 1 d S . H22A H 0.5000 0.0930(2) -0.16634(14) 0.072 Uiso 1 calc SR . C23 C 0.5000 0.15668(14) -0.09168(13) 0.0432(6) Uani 1 d S . C31 C -0.0371(21) 0.0773(21) -0.1448(13) 0.151(9) Uani 0.25 d PDU -1 H31A H -0.0324(21) 0.0656(21) -0.1888(13) 0.227 Uiso 0.25 calc PR -1 H31B H -0.0210(21) 0.1250(21) -0.1383(13) 0.227 Uiso 0.25 calc PR -1 H31C H -0.0897(21) 0.0722(21) -0.1319(13) 0.227 Uiso 0.25 calc PR -1 C32 C 0.0117(21) 0.0301(11) -0.1072(8) 0.162(8) Uani 0.25 d PDU -1 H32A H 0.0651(21) 0.0348(11) -0.1197(8) 0.195 Uiso 0.25 calc PR -1 H32B H -0.0038(21) -0.0183(11) -0.1133(8) 0.195 Uiso 0.25 calc PR -1 C33 C 0.0019(45) 0.0508(9) -0.0404(6) 0.167(7) Uani 0.50 d SPDU -1 H33A H 0.0490(45) 0.0704(9) -0.0234(6) 0.201 Uiso 0.25 calc PR -1 H33B H -0.0391(45) 0.0850(9) -0.0359(6) 0.201 Uiso 0.25 calc PR -1 C34 C -0.0179(14) -0.0153(12) -0.0089(7) 0.169(8) Uani 0.25 d PDU -1 H34A H -0.0721(14) -0.0257(12) -0.0141(7) 0.202 Uiso 0.25 calc PR -1 H34B H 0.0119(14) -0.0538(12) -0.0263(7) 0.202 Uiso 0.25 calc PR -1 C35 C 0.0006(36) -0.0052(9) 0.0579(7) 0.145(5) Uani 0.50 d SPDU -1 H35A H -0.0297(36) 0.0326(9) 0.0759(7) 0.174 Uiso 0.25 calc PR -1 H35B H 0.0547(36) 0.0053(9) 0.0635(7) 0.174 Uiso 0.25 calc PR -1 C36 C -0.0197(17) -0.0735(11) 0.0869(9) 0.175(8) Uani 0.25 d PDU -1 H36A H -0.0749(17) -0.0777(11) 0.0917(9) 0.210 Uiso 0.25 calc PR -1 H36B H -0.0014(17) -0.1120(11) 0.0610(9) 0.210 Uiso 0.50 calc SPR -1 C37 C 0.0186(23) -0.0736(18) 0.1489(11) 0.145(9) Uani 0.25 d PDU -1 H37A H 0.0077(23) -0.1169(18) 0.1704(11) 0.218 Uiso 0.25 calc PR -1 H37B H 0.0000(23) -0.0350(18) 0.1737(11) 0.218 Uiso 0.50 calc SPR -1 H37C H 0.0731(23) -0.0691(18) 0.1432(11) 0.218 Uiso 0.25 calc PR -1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mg 0.0313(4) 0.0281(4) 0.0288(4) -0.0024(3) 0.000 0.000 C1 0.0412(10) 0.0435(10) 0.0363(9) -0.0064(8) 0.0070(8) -0.0019(8) N1 0.0314(7) 0.0401(8) 0.0357(8) -0.0057(6) 0.0016(6) -0.0002(6) C2 0.048(2) 0.051(2) 0.0286(13) -0.0041(11) 0.000 0.000 C3 0.0511(12) 0.089(2) 0.0429(11) -0.0086(12) 0.0147(10) -0.0007(12) C4 0.0313(9) 0.0592(12) 0.0391(10) -0.0078(9) 0.0041(8) 0.0039(8) C5 0.0445(12) 0.0641(14) 0.0701(15) -0.0122(12) -0.0009(11) 0.0165(11) C6 0.0511(15) 0.095(2) 0.082(2) -0.010(2) -0.0024(13) 0.0324(14) C7 0.0337(12) 0.126(3) 0.071(2) -0.012(2) -0.0022(11) 0.0137(14) C8 0.0359(11) 0.106(2) 0.0585(14) -0.0120(14) -0.0004(10) -0.0113(13) C9 0.0357(10) 0.0707(14) 0.0404(10) -0.0051(9) 0.0055(8) -0.0085(9) C10 0.072(2) 0.0504(14) 0.133(3) -0.014(2) -0.021(2) 0.0237(13) C11 0.213(6) 0.076(2) 0.111(3) -0.028(2) -0.023(4) 0.002(3) C12 0.122(3) 0.076(2) 0.145(4) -0.017(2) 0.037(3) -0.005(2) C13 0.0521(12) 0.0598(13) 0.0504(12) -0.0001(10) 0.0031(10) -0.0210(10) C14 0.076(2) 0.081(2) 0.076(2) -0.0246(15) -0.0085(15) -0.0120(15) C15 0.147(4) 0.093(2) 0.083(2) 0.018(2) 0.035(2) -0.032(2) C16 0.0415(13) 0.0278(12) 0.0355(13) 0.0021(10) 0.000 0.000 O16 0.0540(11) 0.0339(9) 0.0323(9) -0.0005(7) 0.000 0.000 O17 0.0624(12) 0.0275(9) 0.0403(10) 0.0003(7) 0.000 0.000 C18 0.078(2) 0.0323(15) 0.067(2) 0.0093(14) 0.000 0.000 C19 0.109(3) 0.040(2) 0.099(3) 0.026(2) 0.000 0.000 C20 0.117(4) 0.069(3) 0.089(3) 0.051(2) 0.000 0.000 C21 0.117(4) 0.082(3) 0.053(2) 0.032(2) 0.000 0.000 C22 0.087(2) 0.054(2) 0.039(2) 0.0131(14) 0.000 0.000 C23 0.054(2) 0.0336(13) 0.0423(15) 0.0097(11) 0.000 0.000 C31 0.129(16) 0.144(15) 0.181(15) 0.004(14) 0.040(13) 0.019(14) C32 0.131(14) 0.189(12) 0.167(12) -0.073(10) -0.017(12) 0.029(12) C33 0.140(12) 0.190(13) 0.172(12) -0.026(11) 0.000(14) 0.012(14) C34 0.122(14) 0.187(14) 0.197(13) -0.039(12) 0.000(12) 0.022(11) C35 0.085(7) 0.158(11) 0.193(12) 0.025(11) 0.003(14) 0.025(13) C36 0.142(14) 0.153(12) 0.229(14) -0.019(12) -0.004(12) 0.019(11) C37 0.133(18) 0.104(11) 0.199(15) -0.008(11) 0.018(14) 0.042(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mg O17 1.918(2) 9_655 ? Mg O16 1.958(2) . ? Mg N1 2.038(2) 12_655 ? Mg N1 2.038(2) . ? C1 N1 1.328(2) . ? C1 C2 1.405(2) . ? C1 C3 1.518(3) . ? N1 C4 1.442(2) . ? C2 C1 1.405(2) 12_655 ? C4 C5 1.398(3) . ? C4 C9 1.406(3) . ? C5 C6 1.397(4) . ? C5 C10 1.513(4) . ? C6 C7 1.361(4) . ? C7 C8 1.370(4) . ? C8 C9 1.394(3) . ? C9 C13 1.518(3) . ? C10 C12 1.520(5) . ? C10 C11 1.530(5) . ? C13 C14 1.517(3) . ? C13 C15 1.524(4) . ? C16 O17 1.253(3) . ? C16 O16 1.254(3) . ? C16 C23 1.494(3) . ? O17 Mg 1.918(2) 9_655 ? C18 C23 1.383(4) . ? C18 C19 1.392(5) . ? C19 C20 1.370(7) . ? C20 C21 1.373(7) . ? C21 C22 1.391(5) . ? C22 C23 1.385(4) . ? C31 C32 1.502(10) . ? C32 C33 1.510(10) . ? C33 C34 1.497(10) . ? C34 C35 1.492(10) . ? C35 C36 1.512(10) . ? C36 C37 1.505(10) . ? 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 O17 Mg O16 113.74(9) 9_655 . ? O17 Mg N1 109.02(6) 9_655 12_655 ? O16 Mg N1 114.06(6) . 12_655 ? O17 Mg N1 109.02(6) 9_655 . ? O16 Mg N1 114.06(6) . . ? N1 Mg N1 95.42(9) 12_655 . ? N1 C1 C2 124.2(2) . . ? N1 C1 C3 120.6(2) . . ? C2 C1 C3 115.2(2) . . ? C1 N1 C4 118.5(2) . . ? C1 N1 Mg 121.02(13) . . ? C4 N1 Mg 120.45(12) . . ? C1 C2 C1 131.1(2) 12_655 . ? C5 C4 C9 121.0(2) . . ? C5 C4 N1 119.1(2) . . ? C9 C4 N1 119.8(2) . . ? C6 C5 C4 118.3(2) . . ? C6 C5 C10 119.6(2) . . ? C4 C5 C10 122.1(2) . . ? C7 C6 C5 121.2(3) . . ? C6 C7 C8 120.3(2) . . ? C7 C8 C9 121.5(3) . . ? C8 C9 C4 117.7(2) . . ? C8 C9 C13 120.4(2) . . ? C4 C9 C13 121.9(2) . . ? C5 C10 C12 111.7(3) . . ? C5 C10 C11 111.0(3) . . ? C12 C10 C11 110.0(3) . . ? C14 C13 C9 113.0(2) . . ? C14 C13 C15 110.4(2) . . ? C9 C13 C15 111.4(2) . . ? O17 C16 O16 123.1(2) . . ? O17 C16 C23 118.2(2) . . ? O16 C16 C23 118.8(2) . . ? C16 O16 Mg 127.4(2) . . ? C16 O17 Mg 175.8(2) . 9_655 ? C23 C18 C19 120.0(4) . . ? C20 C19 C18 120.0(4) . . ? C19 C20 C21 120.4(3) . . ? C20 C21 C22 120.0(4) . . ? C23 C22 C21 119.9(4) . . ? C18 C23 C22 119.6(3) . . ? C18 C23 C16 120.4(3) . . ? C22 C23 C16 120.0(3) . . ? C31 C32 C33 106.7(17) . . ? C34 C33 C32 103.5(14) . . ? C35 C34 C33 106.0(12) . . ? C34 C35 C36 103.4(15) . . ? C37 C36 C35 105.3(15) . . ? _refine_diff_density_max 0.253 _refine_diff_density_min -0.225 _refine_diff_density_rms 0.037 #===END