Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'R. E. Mulvey' 'Joaquin Garcia-Alvarez' 'David V. Graham' 'Eva Hevia' 'Alan R. Kennedy' _publ_contact_author_name 'R. E. Mulvey' _publ_contact_author_address ; Department of Pure & Applied Chemistry University of Strathclyde 295 Cathedral Street Glasgow G1 1XL UNITED KINGDOM ; _publ_contact_author_email R.E.MULVEY@STRATH.AC.UK _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Synthesis and Characterisation of New Bimetallic Alkali Metal-Magnesium Mixed Diisopropylamide-Acetylides: Structural Variations in Bimetallic Lithium- and Sodium-Heteroleptic Magnesiates ; data_dvgrem201 _database_code_depnum_ccdc_archive 'CCDC 664919' #--------------------------------------------- # --------- COMPOUND 3------------------------ #--------------------------------------------- _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H66 Li2 Mg2 N4' _chemical_formula_weight 665.47 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mg Mg 0.0486 0.0363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.5591(3) _cell_length_b 20.3606(6) _cell_length_c 19.3002(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.8884(16) _cell_angle_gamma 90.00 _cell_volume 4148.8(2) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 9581 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.3 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.065 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1456 _exptl_absorpt_coefficient_mu 0.088 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method 'Omega and Phi scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 18288 _diffrn_reflns_av_R_equivalents 0.0564 _diffrn_reflns_av_sigmaI/netI 0.0752 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.45 _diffrn_reflns_theta_max 27.48 _reflns_number_total 9760 _reflns_number_gt 5876 _reflns_threshold_expression I>2\s(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0470P)^2^+1.7397P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9479 _refine_ls_number_parameters 481 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1065 _refine_ls_R_factor_gt 0.0514 _refine_ls_wR_factor_ref 0.1286 _refine_ls_wR_factor_gt 0.1065 _refine_ls_goodness_of_fit_ref 1.014 _refine_ls_restrained_S_all 1.014 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Li1 Li 0.5554(3) 0.09116(16) 0.69908(18) 0.0335(8) Uani 1 1 d . . . Li2 Li 0.9255(3) 0.15590(16) 0.81715(17) 0.0317(8) Uani 1 1 d . . . Mg1 Mg 0.74054(6) 0.05900(3) 0.79845(3) 0.02217(15) Uani 1 1 d . . . Mg2 Mg 0.72775(6) 0.19155(3) 0.72521(3) 0.02114(15) Uani 1 1 d . . . C1 C 0.85498(17) 0.10221(9) 0.71167(9) 0.0215(4) Uani 1 1 d . . . C2 C 0.93349(17) 0.08682(8) 0.66932(9) 0.0197(4) Uani 1 1 d . . . C3 C 1.02312(16) 0.06771(9) 0.61761(9) 0.0212(4) Uani 1 1 d . . . C4 C 1.11324(18) 0.01882(9) 0.63161(10) 0.0278(4) Uani 1 1 d . . . H4 H 1.1172 -0.0011 0.6761 0.033 Uiso 1 1 calc R . . C5 C 1.19624(19) -0.00059(10) 0.58105(10) 0.0323(5) Uani 1 1 d . . . H5 H 1.2575 -0.0335 0.5911 0.039 Uiso 1 1 calc R . . C6 C 1.19103(19) 0.02748(10) 0.51571(10) 0.0324(5) Uani 1 1 d . . . H6 H 1.2475 0.0135 0.4808 0.039 Uiso 1 1 calc R . . C7 C 1.1031(2) 0.07585(11) 0.50190(10) 0.0354(5) Uani 1 1 d . . . H7 H 1.0994 0.0954 0.4572 0.042 Uiso 1 1 calc R . . C8 C 1.02034(19) 0.09629(10) 0.55213(10) 0.0306(5) Uani 1 1 d . . . H8 H 0.9610 0.1301 0.5419 0.037 Uiso 1 1 calc R . . C9 C 0.9628(2) -0.03050(10) 0.84263(11) 0.0408(6) Uani 1 1 d . . . H9A H 0.8880 -0.0537 0.8595 0.061 Uiso 1 1 calc R . . H9B H 1.0377 -0.0585 0.8486 0.061 Uiso 1 1 calc R . . H9C H 0.9506 -0.0200 0.7934 0.061 Uiso 1 1 calc R . . C11 C 1.10431(19) 0.06553(12) 0.86142(11) 0.0414(6) Uani 1 1 d . . . H11A H 1.0993 0.0757 0.8118 0.062 Uiso 1 1 calc R . . H11B H 1.1755 0.0357 0.8704 0.062 Uiso 1 1 calc R . . H11C H 1.1170 0.1062 0.8878 0.062 Uiso 1 1 calc R . . C12 C 0.9318(2) 0.13758(12) 0.98572(11) 0.0452(6) Uani 1 1 d . . . H12A H 0.9946 0.1054 1.0020 0.068 Uiso 1 1 calc R . . H12B H 0.8941 0.1594 1.0257 0.068 Uiso 1 1 calc R . . H12C H 0.9732 0.1703 0.9565 0.068 Uiso 1 1 calc R . . C13 C 0.8276(2) 0.10238(11) 0.94340(10) 0.0353(5) Uani 1 1 d . . . C14 C 0.7638(2) 0.05103(13) 0.98880(11) 0.0489(7) Uani 1 1 d . . . H14A H 0.6891 0.0334 0.9644 0.073 Uiso 1 1 calc R . . H14B H 0.7379 0.0714 1.0323 0.073 Uiso 1 1 calc R . . H14C H 0.8234 0.0153 0.9988 0.073 Uiso 1 1 calc R . . C15 C 1.0956(2) 0.23797(12) 0.76481(13) 0.0462(6) Uani 1 1 d . . . H15A H 1.1054 0.2374 0.8154 0.069 Uiso 1 1 calc R . . H15B H 1.1676 0.2610 0.7445 0.069 Uiso 1 1 calc R . . H15C H 1.0925 0.1928 0.7474 0.069 Uiso 1 1 calc R . . C16 C 0.97235(19) 0.27354(11) 0.74474(10) 0.0309(5) Uani 1 1 d . . . C17 C 0.9559(3) 0.27508(12) 0.66606(11) 0.0502(7) Uani 1 1 d . . . H17A H 0.9453 0.2302 0.6486 0.075 Uiso 1 1 calc R . . H17B H 1.0310 0.2949 0.6454 0.075 Uiso 1 1 calc R . . H17C H 0.8809 0.3011 0.6537 0.075 Uiso 1 1 calc R . . C18 C 0.9032(2) 0.31139(11) 0.88782(10) 0.0364(5) Uani 1 1 d . . . H18A H 0.9419 0.2728 0.9099 0.055 Uiso 1 1 calc R . . H18B H 0.8587 0.3372 0.9227 0.055 Uiso 1 1 calc R . . H18C H 0.9693 0.3384 0.8670 0.055 Uiso 1 1 calc R . . C19 C 0.8087(2) 0.28914(10) 0.83137(11) 0.0320(5) Uani 1 1 d . . . C20 C 0.7464(2) 0.35006(12) 0.79875(15) 0.0639(9) Uani 1 1 d . . . H20A H 0.8113 0.3772 0.7769 0.096 Uiso 1 1 calc R . . H20B H 0.7045 0.3756 0.8348 0.096 Uiso 1 1 calc R . . H20C H 0.6837 0.3363 0.7637 0.096 Uiso 1 1 calc R . . C21 C 0.7386(2) -0.09712(10) 0.70019(12) 0.0398(5) Uani 1 1 d . . . H21A H 0.8093 -0.0857 0.7315 0.060 Uiso 1 1 calc R . . H21B H 0.7715 -0.1179 0.6584 0.060 Uiso 1 1 calc R . . H21C H 0.6816 -0.1276 0.7236 0.060 Uiso 1 1 calc R . . C22 C 0.66582(19) -0.03464(10) 0.68012(10) 0.0270(4) Uani 1 1 d . . . C23 C 0.5631(2) -0.05232(11) 0.62623(11) 0.0365(5) Uani 1 1 d . . . H23A H 0.5031 -0.0832 0.6466 0.055 Uiso 1 1 calc R . . H23B H 0.6025 -0.0726 0.5859 0.055 Uiso 1 1 calc R . . H23C H 0.5181 -0.0124 0.6118 0.055 Uiso 1 1 calc R . . C24 C 0.5496(2) -0.03850(11) 0.85409(11) 0.0420(6) Uani 1 1 d . . . H24A H 0.6313 -0.0607 0.8603 0.063 Uiso 1 1 calc R . . H24B H 0.4835 -0.0638 0.8771 0.063 Uiso 1 1 calc R . . H24C H 0.5544 0.0056 0.8744 0.063 Uiso 1 1 calc R . . C25 C 0.51779(19) -0.03306(10) 0.77703(10) 0.0286(5) Uani 1 1 d . . . C26 C 0.38755(19) -0.00089(11) 0.76784(12) 0.0413(6) Uani 1 1 d . . . H26A H 0.3892 0.0431 0.7885 0.062 Uiso 1 1 calc R . . H26B H 0.3236 -0.0277 0.7908 0.062 Uiso 1 1 calc R . . H26C H 0.3665 0.0026 0.7183 0.062 Uiso 1 1 calc R . . C27 C 0.5903(2) 0.12545(11) 0.52836(11) 0.0421(6) Uani 1 1 d . . . H27A H 0.5887 0.0816 0.5492 0.063 Uiso 1 1 calc R . . H27B H 0.6357 0.1237 0.4845 0.063 Uiso 1 1 calc R . . H27C H 0.5033 0.1405 0.5197 0.063 Uiso 1 1 calc R . . C28 C 0.65765(19) 0.17321(11) 0.57791(10) 0.0301(5) Uani 1 1 d . . . C29 C 0.6739(2) 0.23978(12) 0.54206(11) 0.0428(6) Uani 1 1 d . . . H29A H 0.5907 0.2570 0.5282 0.064 Uiso 1 1 calc R . . H29B H 0.7261 0.2343 0.5009 0.064 Uiso 1 1 calc R . . H29C H 0.7155 0.2706 0.5741 0.064 Uiso 1 1 calc R . . C30 C 0.4624(2) 0.27144(10) 0.68215(11) 0.0356(5) Uani 1 1 d . . . H30A H 0.4787 0.2628 0.7314 0.053 Uiso 1 1 calc R . . H30B H 0.3774 0.2902 0.6761 0.053 Uiso 1 1 calc R . . H30C H 0.5254 0.3025 0.6650 0.053 Uiso 1 1 calc R . . C31 C 0.47098(18) 0.20739(9) 0.64158(10) 0.0248(4) Uani 1 1 d . . . C32 C 0.36672(18) 0.16032(11) 0.66462(12) 0.0370(5) Uani 1 1 d . . . H32A H 0.3728 0.1192 0.6386 0.055 Uiso 1 1 calc R . . H32B H 0.2837 0.1804 0.6558 0.055 Uiso 1 1 calc R . . H32C H 0.3769 0.1512 0.7143 0.055 Uiso 1 1 calc R . . C33 C 0.61072(17) 0.14726(9) 0.81040(9) 0.0224(4) Uani 1 1 d . . . C34 C 0.53127(17) 0.16224(9) 0.85262(9) 0.0208(4) Uani 1 1 d . . . C35 C 0.43747(17) 0.18102(9) 0.90236(9) 0.0226(4) Uani 1 1 d . . . C36 C 0.3973(2) 0.13733(11) 0.95280(11) 0.0354(5) Uani 1 1 d . . . H36 H 0.4317 0.0942 0.9546 0.043 Uiso 1 1 calc R . . C37 C 0.3077(2) 0.15605(12) 1.00047(11) 0.0415(6) Uani 1 1 d . . . H37 H 0.2807 0.1257 1.0346 0.050 Uiso 1 1 calc R . . C38 C 0.2574(2) 0.21832(12) 0.99883(11) 0.0373(5) Uani 1 1 d . . . H38 H 0.1960 0.2310 1.0317 0.045 Uiso 1 1 calc R . . C39 C 0.2963(2) 0.26205(11) 0.94945(11) 0.0403(6) Uani 1 1 d . . . H39 H 0.2616 0.3051 0.9482 0.048 Uiso 1 1 calc R . . C40 C 0.3857(2) 0.24391(10) 0.90159(11) 0.0345(5) Uani 1 1 d . . . H40 H 0.4121 0.2747 0.8678 0.041 Uiso 1 1 calc R . . C10 C 0.98134(19) 0.03280(10) 0.88359(10) 0.0293(5) Uani 1 1 d . . . N1 N 0.87019(14) 0.07677(8) 0.87577(8) 0.0246(4) Uani 1 1 d . . . N2 N 0.86192(14) 0.24428(7) 0.77933(8) 0.0215(3) Uani 1 1 d . . . N3 N 0.61767(14) 0.00322(7) 0.73965(8) 0.0225(3) Uani 1 1 d . . . N4 N 0.59867(14) 0.17696(7) 0.64678(7) 0.0218(3) Uani 1 1 d . . . H10 H 0.9920(18) 0.0188(9) 0.9342(10) 0.030(5) Uiso 1 1 d . . . H13 H 0.7637(19) 0.1353(10) 0.9331(10) 0.037(6) Uiso 1 1 d . . . H16 H 0.9847(18) 0.3198(10) 0.7594(10) 0.032(6) Uiso 1 1 d . . . H19 H 0.743(2) 0.2631(11) 0.8556(11) 0.042(6) Uiso 1 1 d . . . H22 H 0.7269(17) -0.0054(9) 0.6565(9) 0.022(5) Uiso 1 1 d . . . H25 H 0.5117(17) -0.0787(9) 0.7592(9) 0.023(5) Uiso 1 1 d . . . H28 H 0.7477(19) 0.1547(9) 0.5839(10) 0.032(5) Uiso 1 1 d . . . H31 H 0.4532(17) 0.2183(9) 0.5927(10) 0.025(5) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Li1 0.038(2) 0.0241(18) 0.039(2) 0.0006(15) -0.0014(16) 0.0012(15) Li2 0.0365(19) 0.0287(19) 0.0297(18) -0.0003(15) -0.0032(15) 0.0012(15) Mg1 0.0250(3) 0.0201(3) 0.0214(3) 0.0004(3) 0.0003(3) 0.0011(3) Mg2 0.0223(3) 0.0196(3) 0.0215(3) -0.0005(3) -0.0016(3) -0.0003(3) C1 0.0233(10) 0.0180(10) 0.0230(10) -0.0010(8) -0.0014(8) -0.0006(8) C2 0.0207(9) 0.0171(9) 0.0213(9) 0.0016(7) -0.0021(8) -0.0012(7) C3 0.0189(9) 0.0236(10) 0.0212(9) -0.0028(8) 0.0013(7) -0.0016(8) C4 0.0287(10) 0.0275(11) 0.0271(10) 0.0029(9) 0.0033(9) 0.0041(9) C5 0.0298(11) 0.0297(12) 0.0376(12) -0.0001(9) 0.0071(9) 0.0099(9) C6 0.0312(11) 0.0351(12) 0.0314(11) -0.0037(9) 0.0126(9) 0.0021(9) C7 0.0393(12) 0.0422(13) 0.0250(10) 0.0065(10) 0.0102(9) 0.0043(10) C8 0.0296(11) 0.0329(12) 0.0294(11) 0.0058(9) 0.0039(9) 0.0083(9) C9 0.0473(14) 0.0331(13) 0.0418(13) -0.0009(10) -0.0042(11) 0.0175(11) C11 0.0310(12) 0.0560(15) 0.0373(12) -0.0064(11) 0.0017(10) 0.0098(11) C12 0.0556(15) 0.0506(15) 0.0290(12) -0.0121(11) -0.0084(11) 0.0164(12) C13 0.0377(12) 0.0459(14) 0.0222(10) -0.0029(10) -0.0013(9) 0.0190(11) C14 0.0375(13) 0.085(2) 0.0243(11) 0.0068(12) 0.0035(10) 0.0053(13) C15 0.0266(12) 0.0533(16) 0.0590(16) -0.0155(12) 0.0134(11) -0.0086(11) C16 0.0356(12) 0.0266(11) 0.0305(11) -0.0053(9) 0.0047(9) -0.0109(9) C17 0.0783(19) 0.0413(14) 0.0314(12) -0.0021(11) 0.0134(12) -0.0250(13) C18 0.0445(13) 0.0358(13) 0.0290(11) -0.0127(9) 0.0005(10) -0.0038(10) C19 0.0276(11) 0.0302(12) 0.0384(12) -0.0154(10) 0.0036(9) -0.0042(9) C20 0.0534(16) 0.0437(16) 0.093(2) -0.0373(15) -0.0351(15) 0.0239(13) C21 0.0404(13) 0.0328(13) 0.0466(13) -0.0140(10) 0.0059(11) 0.0035(10) C22 0.0298(11) 0.0239(11) 0.0275(11) -0.0050(8) 0.0081(9) -0.0071(9) C23 0.0415(13) 0.0358(13) 0.0324(11) -0.0075(10) 0.0050(10) -0.0122(10) C24 0.0507(14) 0.0406(14) 0.0349(12) 0.0044(10) 0.0123(11) -0.0087(11) C25 0.0332(11) 0.0195(11) 0.0333(11) -0.0038(9) 0.0090(9) -0.0061(9) C26 0.0309(12) 0.0370(13) 0.0563(15) -0.0072(11) 0.0113(11) -0.0065(10) C27 0.0548(15) 0.0430(14) 0.0284(12) -0.0107(10) -0.0007(11) 0.0106(11) C28 0.0276(11) 0.0406(13) 0.0221(10) -0.0001(9) 0.0011(8) 0.0076(9) C29 0.0455(14) 0.0553(16) 0.0276(12) 0.0079(11) 0.0010(10) -0.0069(12) C30 0.0380(12) 0.0298(12) 0.0388(12) -0.0027(10) -0.0002(10) 0.0093(10) C31 0.0243(10) 0.0260(11) 0.0241(10) -0.0016(8) -0.0035(8) 0.0063(8) C32 0.0222(11) 0.0370(13) 0.0517(14) -0.0046(11) 0.0001(10) 0.0042(9) C33 0.0248(10) 0.0204(10) 0.0219(10) 0.0007(8) -0.0030(8) 0.0002(8) C34 0.0222(10) 0.0174(9) 0.0226(10) 0.0003(8) -0.0034(8) -0.0008(7) C35 0.0200(9) 0.0274(11) 0.0202(9) -0.0043(8) -0.0029(8) -0.0004(8) C36 0.0407(13) 0.0329(12) 0.0329(12) 0.0037(9) 0.0075(10) 0.0035(10) C37 0.0451(14) 0.0484(15) 0.0315(12) 0.0050(11) 0.0143(10) -0.0027(11) C38 0.0273(11) 0.0571(15) 0.0276(11) -0.0104(11) 0.0060(9) 0.0028(10) C39 0.0400(13) 0.0412(14) 0.0398(13) -0.0013(11) 0.0079(11) 0.0167(11) C40 0.0388(12) 0.0317(12) 0.0333(12) 0.0040(9) 0.0092(10) 0.0092(10) C10 0.0317(11) 0.0317(12) 0.0244(10) 0.0013(9) -0.0023(9) 0.0111(9) N1 0.0260(8) 0.0272(9) 0.0205(8) -0.0001(7) -0.0011(7) 0.0099(7) N2 0.0208(8) 0.0208(8) 0.0230(8) -0.0034(6) 0.0011(6) -0.0020(6) N3 0.0224(8) 0.0190(8) 0.0262(8) -0.0018(7) 0.0055(7) -0.0023(6) N4 0.0201(8) 0.0246(9) 0.0206(8) -0.0009(7) -0.0014(6) 0.0030(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Li1 N3 2.058(4) . ? Li1 N4 2.072(4) . ? Li1 C33 2.495(4) . ? Li1 C31 2.756(4) . ? Li1 Mg2 2.778(3) . ? Li1 Mg1 2.795(3) . ? Li2 N2 2.051(4) . ? Li2 N1 2.058(4) . ? Li2 C1 2.418(4) . ? Li2 Mg1 2.795(3) . ? Li2 Mg2 2.814(3) . ? Mg1 N1 2.0417(16) . ? Mg1 N3 2.0532(16) . ? Mg1 C1 2.259(2) . ? Mg1 C33 2.2741(19) . ? Mg1 Mg2 3.0485(9) . ? Mg2 N4 2.0428(15) . ? Mg2 N2 2.0506(15) . ? Mg2 C33 2.260(2) . ? Mg2 C1 2.2787(19) . ? C1 C2 1.214(2) . ? C2 C3 1.440(3) . ? C3 C8 1.391(3) . ? C3 C4 1.400(3) . ? C4 C5 1.380(3) . ? C4 H4 0.9500 . ? C5 C6 1.385(3) . ? C5 H5 0.9500 . ? C6 C7 1.376(3) . ? C6 H6 0.9500 . ? C7 C8 1.380(3) . ? C7 H7 0.9500 . ? C8 H8 0.9500 . ? C9 C10 1.523(3) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C11 C10 1.527(3) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C13 1.537(3) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 N1 1.482(2) . ? C13 C14 1.528(3) . ? C13 H13 0.97(2) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C16 1.534(3) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 N2 1.478(2) . ? C16 C17 1.526(3) . ? C16 H16 0.99(2) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C19 1.534(3) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 N2 1.475(2) . ? C19 C20 1.535(3) . ? C19 H19 0.99(2) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C22 1.533(3) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 N3 1.480(2) . ? C22 C23 1.534(3) . ? C22 H22 0.994(19) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 C25 1.524(3) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 N3 1.484(2) . ? C25 C26 1.531(3) . ? C25 H25 0.992(19) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C28 1.531(3) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 N4 1.479(2) . ? C28 C29 1.533(3) . ? C28 H28 1.03(2) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 C31 1.525(3) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 N4 1.486(2) . ? C31 C32 1.531(3) . ? C31 H31 0.985(19) . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 C34 1.217(3) . ? C34 C35 1.442(3) . ? C35 C36 1.390(3) . ? C35 C40 1.392(3) . ? C36 C37 1.384(3) . ? C36 H36 0.9500 . ? C37 C38 1.375(3) . ? C37 H37 0.9500 . ? C38 C39 1.372(3) . ? C38 H38 0.9500 . ? C39 C40 1.381(3) . ? C39 H39 0.9500 . ? C40 H40 0.9500 . ? C10 N1 1.482(2) . ? C10 H10 1.022(19) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Li1 N4 147.9(2) . . ? N3 Li1 C33 90.08(14) . . ? N4 Li1 C33 89.02(13) . . ? N3 Li1 C31 178.56(18) . . ? N4 Li1 C31 32.04(8) . . ? C33 Li1 C31 91.35(12) . . ? N3 Li1 Mg2 111.49(14) . . ? N4 Li1 Mg2 47.09(8) . . ? C33 Li1 Mg2 50.41(8) . . ? C31 Li1 Mg2 69.40(9) . . ? N3 Li1 Mg1 47.09(8) . . ? N4 Li1 Mg1 111.98(14) . . ? C33 Li1 Mg1 50.53(8) . . ? C31 Li1 Mg1 134.09(13) . . ? Mg2 Li1 Mg1 66.32(8) . . ? N2 Li2 N1 142.03(19) . . ? N2 Li2 C1 90.12(13) . . ? N1 Li2 C1 91.30(14) . . ? N2 Li2 Mg1 110.44(14) . . ? N1 Li2 Mg1 46.77(8) . . ? C1 Li2 Mg1 50.72(8) . . ? N2 Li2 Mg2 46.67(8) . . ? N1 Li2 Mg2 109.54(14) . . ? C1 Li2 Mg2 50.95(8) . . ? Mg1 Li2 Mg2 65.84(8) . . ? N1 Mg1 N3 155.90(7) . . ? N1 Mg1 C1 96.47(7) . . ? N3 Mg1 C1 98.41(6) . . ? N1 Mg1 C33 100.62(7) . . ? N3 Mg1 C33 96.68(7) . . ? C1 Mg1 C33 95.61(7) . . ? N1 Mg1 Li2 47.27(8) . . ? N3 Mg1 Li2 153.64(9) . . ? C1 Mg1 Li2 55.96(8) . . ? C33 Mg1 Li2 81.38(9) . . ? N1 Mg1 Li1 156.05(9) . . ? N3 Mg1 Li1 47.24(8) . . ? C1 Mg1 Li1 77.09(9) . . ? C33 Mg1 Li1 57.87(8) . . ? Li2 Mg1 Li1 113.77(10) . . ? N1 Mg1 Mg2 101.91(5) . . ? N3 Mg1 Mg2 102.14(5) . . ? C1 Mg1 Mg2 48.07(5) . . ? C33 Mg1 Mg2 47.55(5) . . ? Li2 Mg1 Mg2 57.38(7) . . ? Li1 Mg1 Mg2 56.57(7) . . ? N4 Mg2 N2 154.33(7) . . ? N4 Mg2 C33 96.60(7) . . ? N2 Mg2 C33 102.68(7) . . ? N4 Mg2 C1 100.76(6) . . ? N2 Mg2 C1 94.15(6) . . ? C33 Mg2 C1 95.45(7) . . ? N4 Mg2 Li1 47.99(8) . . ? N2 Mg2 Li1 157.41(9) . . ? C33 Mg2 Li1 58.28(9) . . ? C1 Mg2 Li1 77.15(9) . . ? N4 Mg2 Li2 155.46(9) . . ? N2 Mg2 Li2 46.68(8) . . ? C33 Mg2 Li2 81.20(9) . . ? C1 Mg2 Li2 55.49(8) . . ? Li1 Mg2 Li2 113.72(10) . . ? N4 Mg2 Mg1 103.83(5) . . ? N2 Mg2 Mg1 101.65(5) . . ? C33 Mg2 Mg1 47.95(5) . . ? C1 Mg2 Mg1 47.51(5) . . ? Li1 Mg2 Mg1 57.11(7) . . ? Li2 Mg2 Mg1 56.78(7) . . ? C2 C1 Mg1 141.01(15) . . ? C2 C1 Mg2 133.87(15) . . ? Mg1 C1 Mg2 84.42(7) . . ? C2 C1 Li2 118.61(16) . . ? Mg1 C1 Li2 73.32(10) . . ? Mg2 C1 Li2 73.56(10) . . ? C1 C2 C3 178.03(19) . . ? C8 C3 C4 118.51(17) . . ? C8 C3 C2 120.78(16) . . ? C4 C3 C2 120.70(16) . . ? C5 C4 C3 120.29(18) . . ? C5 C4 H4 119.9 . . ? C3 C4 H4 119.9 . . ? C4 C5 C6 120.61(18) . . ? C4 C5 H5 119.7 . . ? C6 C5 H5 119.7 . . ? C7 C6 C5 119.25(19) . . ? C7 C6 H6 120.4 . . ? C5 C6 H6 120.4 . . ? C6 C7 C8 120.84(19) . . ? C6 C7 H7 119.6 . . ? C8 C7 H7 119.6 . . ? C7 C8 C3 120.48(18) . . ? C7 C8 H8 119.8 . . ? C3 C8 H8 119.8 . . ? C10 C9 H9A 109.5 . . ? C10 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C10 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C13 C12 H12A 109.5 . . ? C13 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C13 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N1 C13 C14 114.02(19) . . ? N1 C13 C12 114.06(18) . . ? C14 C13 C12 109.43(17) . . ? N1 C13 H13 106.5(12) . . ? C14 C13 H13 106.2(12) . . ? C12 C13 H13 106.0(12) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C16 C15 H15A 109.5 . . ? C16 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C16 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N2 C16 C17 112.29(17) . . ? N2 C16 C15 111.58(17) . . ? C17 C16 C15 110.14(19) . . ? N2 C16 H16 110.8(12) . . ? C17 C16 H16 106.1(11) . . ? C15 C16 H16 105.6(11) . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C19 C18 H18A 109.5 . . ? C19 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C19 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N2 C19 C18 114.61(17) . . ? N2 C19 C20 112.73(18) . . ? C18 C19 C20 108.82(17) . . ? N2 C19 H19 105.3(13) . . ? C18 C19 H19 105.7(12) . . ? C20 C19 H19 109.2(12) . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C22 C21 H21A 109.5 . . ? C22 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C22 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? N3 C22 C21 114.39(16) . . ? N3 C22 C23 113.62(16) . . ? C21 C22 C23 108.86(16) . . ? N3 C22 H22 106.1(10) . . ? C21 C22 H22 106.7(10) . . ? C23 C22 H22 106.6(10) . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C25 C24 H24A 109.5 . . ? C25 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C25 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N3 C25 C24 111.30(16) . . ? N3 C25 C26 112.00(16) . . ? C24 C25 C26 109.16(18) . . ? N3 C25 H25 109.9(11) . . ? C24 C25 H25 106.4(10) . . ? C26 C25 H25 107.9(11) . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C28 C27 H27A 109.5 . . ? C28 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C28 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? N4 C28 C27 113.33(17) . . ? N4 C28 C29 114.32(17) . . ? C27 C28 C29 109.51(17) . . ? N4 C28 H28 108.7(11) . . ? C27 C28 H28 104.9(11) . . ? C29 C28 H28 105.4(11) . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C31 C30 H30A 109.5 . . ? C31 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C31 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? N4 C31 C30 112.54(15) . . ? N4 C31 C32 112.05(15) . . ? C30 C31 C32 109.72(17) . . ? N4 C31 Li1 47.73(11) . . ? C30 C31 Li1 123.31(15) . . ? C32 C31 Li1 64.85(13) . . ? N4 C31 H31 108.6(11) . . ? C30 C31 H31 106.6(11) . . ? C32 C31 H31 107.0(11) . . ? Li1 C31 H31 129.5(11) . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C34 C33 Mg2 141.02(15) . . ? C34 C33 Mg1 133.52(15) . . ? Mg2 C33 Mg1 84.50(7) . . ? C34 C33 Li1 122.45(16) . . ? Mg2 C33 Li1 71.31(10) . . ? Mg1 C33 Li1 71.60(9) . . ? C33 C34 C35 179.1(2) . . ? C36 C35 C40 118.16(18) . . ? C36 C35 C34 121.13(18) . . ? C40 C35 C34 120.71(18) . . ? C37 C36 C35 120.6(2) . . ? C37 C36 H36 119.7 . . ? C35 C36 H36 119.7 . . ? C38 C37 C36 120.4(2) . . ? C38 C37 H37 119.8 . . ? C36 C37 H37 119.8 . . ? C39 C38 C37 119.6(2) . . ? C39 C38 H38 120.2 . . ? C37 C38 H38 120.2 . . ? C38 C39 C40 120.4(2) . . ? C38 C39 H39 119.8 . . ? C40 C39 H39 119.8 . . ? C39 C40 C35 120.7(2) . . ? C39 C40 H40 119.6 . . ? C35 C40 H40 119.6 . . ? N1 C10 C9 111.28(16) . . ? N1 C10 C11 112.54(17) . . ? C9 C10 C11 109.10(18) . . ? N1 C10 H10 110.0(11) . . ? C9 C10 H10 105.7(11) . . ? C11 C10 H10 107.9(11) . . ? C13 N1 C10 111.93(14) . . ? C13 N1 Mg1 119.80(12) . . ? C10 N1 Mg1 119.23(12) . . ? C13 N1 Li2 107.53(16) . . ? C10 N1 Li2 107.34(15) . . ? Mg1 N1 Li2 85.97(11) . . ? C19 N2 C16 111.67(15) . . ? C19 N2 Mg2 113.81(12) . . ? C16 N2 Mg2 121.64(12) . . ? C19 N2 Li2 115.27(16) . . ? C16 N2 Li2 104.97(15) . . ? Mg2 N2 Li2 86.66(11) . . ? C22 N3 C25 111.92(14) . . ? C22 N3 Mg1 119.70(11) . . ? C25 N3 Mg1 117.03(12) . . ? C22 N3 Li1 105.63(15) . . ? C25 N3 Li1 113.12(15) . . ? Mg1 N3 Li1 85.68(11) . . ? C28 N4 C31 110.81(14) . . ? C28 N4 Mg2 112.84(11) . . ? C31 N4 Mg2 125.72(12) . . ? C28 N4 Li1 119.57(15) . . ? C31 N4 Li1 100.22(15) . . ? Mg2 N4 Li1 84.92(11) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Li2 Mg1 N1 -143.6(2) . . . . ? C1 Li2 Mg1 N1 144.01(13) . . . . ? Mg2 Li2 Mg1 N1 -157.66(12) . . . . ? N2 Li2 Mg1 N3 57.3(3) . . . . ? N1 Li2 Mg1 N3 -159.14(15) . . . . ? C1 Li2 Mg1 N3 -15.1(2) . . . . ? Mg2 Li2 Mg1 N3 43.2(2) . . . . ? N2 Li2 Mg1 C1 72.43(14) . . . . ? N1 Li2 Mg1 C1 -144.01(13) . . . . ? Mg2 Li2 Mg1 C1 58.32(7) . . . . ? N2 Li2 Mg1 C33 -30.37(14) . . . . ? N1 Li2 Mg1 C33 113.18(10) . . . . ? C1 Li2 Mg1 C33 -102.80(9) . . . . ? Mg2 Li2 Mg1 C33 -44.48(6) . . . . ? N2 Li2 Mg1 Li1 18.75(19) . . . . ? N1 Li2 Mg1 Li1 162.30(11) . . . . ? C1 Li2 Mg1 Li1 -53.69(12) . . . . ? Mg2 Li2 Mg1 Li1 4.64(11) . . . . ? N2 Li2 Mg1 Mg2 14.11(10) . . . . ? N1 Li2 Mg1 Mg2 157.66(12) . . . . ? C1 Li2 Mg1 Mg2 -58.32(7) . . . . ? N3 Li1 Mg1 N1 -168.77(18) . . . . ? N4 Li1 Mg1 N1 40.5(3) . . . . ? C33 Li1 Mg1 N1 -28.6(3) . . . . ? C31 Li1 Mg1 N1 12.4(4) . . . . ? Mg2 Li1 Mg1 N1 28.7(2) . . . . ? N4 Li1 Mg1 N3 -150.7(2) . . . . ? C33 Li1 Mg1 N3 140.18(14) . . . . ? C31 Li1 Mg1 N3 -178.8(3) . . . . ? Mg2 Li1 Mg1 N3 -162.53(13) . . . . ? N3 Li1 Mg1 C1 114.61(11) . . . . ? N4 Li1 Mg1 C1 -36.08(14) . . . . ? C33 Li1 Mg1 C1 -105.21(9) . . . . ? C31 Li1 Mg1 C1 -64.24(19) . . . . ? Mg2 Li1 Mg1 C1 -47.92(6) . . . . ? N3 Li1 Mg1 C33 -140.18(14) . . . . ? N4 Li1 Mg1 C33 69.13(14) . . . . ? C31 Li1 Mg1 C33 40.97(17) . . . . ? Mg2 Li1 Mg1 C33 57.29(7) . . . . ? N3 Li1 Mg1 Li2 157.85(11) . . . . ? N4 Li1 Mg1 Li2 7.16(19) . . . . ? C33 Li1 Mg1 Li2 -61.97(12) . . . . ? C31 Li1 Mg1 Li2 -21.0(2) . . . . ? Mg2 Li1 Mg1 Li2 -4.68(11) . . . . ? N3 Li1 Mg1 Mg2 162.53(13) . . . . ? N4 Li1 Mg1 Mg2 11.84(10) . . . . ? C33 Li1 Mg1 Mg2 -57.29(7) . . . . ? C31 Li1 Mg1 Mg2 -16.32(15) . . . . ? N3 Li1 Mg2 N4 151.3(2) . . . . ? C33 Li1 Mg2 N4 -137.61(13) . . . . ? C31 Li1 Mg2 N4 -27.51(8) . . . . ? Mg1 Li1 Mg2 N4 164.94(13) . . . . ? N3 Li1 Mg2 N2 -35.5(3) . . . . ? N4 Li1 Mg2 N2 173.18(19) . . . . ? C33 Li1 Mg2 N2 35.6(3) . . . . ? C31 Li1 Mg2 N2 145.67(19) . . . . ? Mg1 Li1 Mg2 N2 -21.9(3) . . . . ? N3 Li1 Mg2 C33 -71.12(15) . . . . ? N4 Li1 Mg2 C33 137.61(13) . . . . ? C31 Li1 Mg2 C33 110.10(11) . . . . ? Mg1 Li1 Mg2 C33 -57.45(7) . . . . ? N3 Li1 Mg2 C1 33.68(14) . . . . ? N4 Li1 Mg2 C1 -117.59(11) . . . . ? C33 Li1 Mg2 C1 104.80(9) . . . . ? C31 Li1 Mg2 C1 -145.10(9) . . . . ? Mg1 Li1 Mg2 C1 47.35(6) . . . . ? N3 Li1 Mg2 Li2 -9.02(19) . . . . ? N4 Li1 Mg2 Li2 -160.29(11) . . . . ? C33 Li1 Mg2 Li2 62.09(12) . . . . ? C31 Li1 Mg2 Li2 172.19(9) . . . . ? Mg1 Li1 Mg2 Li2 4.65(11) . . . . ? N3 Li1 Mg2 Mg1 -13.67(10) . . . . ? N4 Li1 Mg2 Mg1 -164.94(13) . . . . ? C33 Li1 Mg2 Mg1 57.45(7) . . . . ? C31 Li1 Mg2 Mg1 167.55(11) . . . . ? N2 Li2 Mg2 N4 156.54(17) . . . . ? N1 Li2 Mg2 N4 -58.8(3) . . . . ? C1 Li2 Mg2 N4 16.3(2) . . . . ? Mg1 Li2 Mg2 N4 -41.8(2) . . . . ? N1 Li2 Mg2 N2 144.6(2) . . . . ? C1 Li2 Mg2 N2 -140.28(14) . . . . ? Mg1 Li2 Mg2 N2 161.70(13) . . . . ? N2 Li2 Mg2 C33 -116.83(11) . . . . ? N1 Li2 Mg2 C33 27.77(13) . . . . ? C1 Li2 Mg2 C33 102.89(9) . . . . ? Mg1 Li2 Mg2 C33 44.86(6) . . . . ? N2 Li2 Mg2 C1 140.28(14) . . . . ? N1 Li2 Mg2 C1 -75.11(14) . . . . ? Mg1 Li2 Mg2 C1 -58.02(7) . . . . ? N2 Li2 Mg2 Li1 -166.36(11) . . . . ? N1 Li2 Mg2 Li1 -21.75(18) . . . . ? C1 Li2 Mg2 Li1 53.36(12) . . . . ? Mg1 Li2 Mg2 Li1 -4.66(11) . . . . ? N2 Li2 Mg2 Mg1 -161.70(13) . . . . ? N1 Li2 Mg2 Mg1 -17.09(9) . . . . ? C1 Li2 Mg2 Mg1 58.02(7) . . . . ? N1 Mg1 Mg2 N4 -179.98(7) . . . . ? N3 Mg1 Mg2 N4 1.56(7) . . . . ? C1 Mg1 Mg2 N4 92.02(8) . . . . ? C33 Mg1 Mg2 N4 -86.41(8) . . . . ? Li2 Mg1 Mg2 N4 163.45(10) . . . . ? Li1 Mg1 Mg2 N4 -11.47(10) . . . . ? N1 Mg1 Mg2 N2 3.09(7) . . . . ? N3 Mg1 Mg2 N2 -175.37(6) . . . . ? C1 Mg1 Mg2 N2 -84.92(8) . . . . ? C33 Mg1 Mg2 N2 96.65(8) . . . . ? Li2 Mg1 Mg2 N2 -13.49(10) . . . . ? Li1 Mg1 Mg2 N2 171.60(10) . . . . ? N1 Mg1 Mg2 C33 -93.57(8) . . . . ? N3 Mg1 Mg2 C33 87.97(8) . . . . ? C1 Mg1 Mg2 C33 178.43(9) . . . . ? Li2 Mg1 Mg2 C33 -110.14(11) . . . . ? Li1 Mg1 Mg2 C33 74.94(11) . . . . ? N1 Mg1 Mg2 C1 88.01(8) . . . . ? N3 Mg1 Mg2 C1 -90.46(8) . . . . ? C33 Mg1 Mg2 C1 -178.43(9) . . . . ? Li2 Mg1 Mg2 C1 71.43(10) . . . . ? Li1 Mg1 Mg2 C1 -103.49(11) . . . . ? N1 Mg1 Mg2 Li1 -168.51(10) . . . . ? N3 Mg1 Mg2 Li1 13.03(10) . . . . ? C1 Mg1 Mg2 Li1 103.49(11) . . . . ? C33 Mg1 Mg2 Li1 -74.94(11) . . . . ? Li2 Mg1 Mg2 Li1 174.91(12) . . . . ? N1 Mg1 Mg2 Li2 16.58(10) . . . . ? N3 Mg1 Mg2 Li2 -161.89(10) . . . . ? C1 Mg1 Mg2 Li2 -71.43(10) . . . . ? C33 Mg1 Mg2 Li2 110.14(11) . . . . ? Li1 Mg1 Mg2 Li2 -174.91(12) . . . . ? N1 Mg1 C1 C2 89.4(2) . . . . ? N3 Mg1 C1 C2 -71.6(2) . . . . ? C33 Mg1 C1 C2 -169.2(2) . . . . ? Li2 Mg1 C1 C2 115.1(2) . . . . ? Li1 Mg1 C1 C2 -114.0(2) . . . . ? Mg2 Mg1 C1 C2 -170.4(3) . . . . ? N1 Mg1 C1 Mg2 -100.22(6) . . . . ? N3 Mg1 C1 Mg2 98.80(6) . . . . ? C33 Mg1 C1 Mg2 1.17(6) . . . . ? Li2 Mg1 C1 Mg2 -74.48(9) . . . . ? Li1 Mg1 C1 Mg2 56.36(8) . . . . ? N1 Mg1 C1 Li2 -25.74(10) . . . . ? N3 Mg1 C1 Li2 173.27(10) . . . . ? C33 Mg1 C1 Li2 75.64(10) . . . . ? Li1 Mg1 C1 Li2 130.84(12) . . . . ? Mg2 Mg1 C1 Li2 74.48(10) . . . . ? N4 Mg2 C1 C2 72.7(2) . . . . ? N2 Mg2 C1 C2 -86.4(2) . . . . ? C33 Mg2 C1 C2 170.47(19) . . . . ? Li1 Mg2 C1 C2 114.8(2) . . . . ? Li2 Mg2 C1 C2 -114.1(2) . . . . ? Mg1 Mg2 C1 C2 171.6(2) . . . . ? N4 Mg2 C1 Mg1 -98.97(6) . . . . ? N2 Mg2 C1 Mg1 102.01(6) . . . . ? C33 Mg2 C1 Mg1 -1.17(6) . . . . ? Li1 Mg2 C1 Mg1 -56.88(8) . . . . ? Li2 Mg2 C1 Mg1 74.23(10) . . . . ? N4 Mg2 C1 Li2 -173.20(10) . . . . ? N2 Mg2 C1 Li2 27.78(10) . . . . ? C33 Mg2 C1 Li2 -75.40(10) . . . . ? Li1 Mg2 C1 Li2 -131.11(12) . . . . ? Mg1 Mg2 C1 Li2 -74.23(10) . . . . ? N2 Li2 C1 C2 103.76(19) . . . . ? N1 Li2 C1 C2 -114.18(18) . . . . ? Mg1 Li2 C1 C2 -139.54(18) . . . . ? Mg2 Li2 C1 C2 131.46(18) . . . . ? N2 Li2 C1 Mg1 -116.70(13) . . . . ? N1 Li2 C1 Mg1 25.36(10) . . . . ? Mg2 Li2 C1 Mg1 -89.00(7) . . . . ? N2 Li2 C1 Mg2 -27.70(10) . . . . ? N1 Li2 C1 Mg2 114.36(13) . . . . ? Mg1 Li2 C1 Mg2 89.00(7) . . . . ? Mg1 C1 C2 C3 82(6) . . . . ? Mg2 C1 C2 C3 -85(6) . . . . ? Li2 C1 C2 C3 -179(100) . . . . ? C1 C2 C3 C8 64(6) . . . . ? C1 C2 C3 C4 -115(6) . . . . ? C8 C3 C4 C5 -0.5(3) . . . . ? C2 C3 C4 C5 178.01(18) . . . . ? C3 C4 C5 C6 -0.5(3) . . . . ? C4 C5 C6 C7 1.0(3) . . . . ? C5 C6 C7 C8 -0.3(3) . . . . ? C6 C7 C8 C3 -0.8(3) . . . . ? C4 C3 C8 C7 1.2(3) . . . . ? C2 C3 C8 C7 -177.33(18) . . . . ? N3 Li1 C31 N4 -89(7) . . . . ? C33 Li1 C31 N4 86.00(15) . . . . ? Mg2 Li1 C31 N4 39.62(10) . . . . ? Mg1 Li1 C31 N4 55.58(19) . . . . ? N3 Li1 C31 C30 -180(100) . . . . ? N4 Li1 C31 C30 -91.3(2) . . . . ? C33 Li1 C31 C30 -5.3(2) . . . . ? Mg2 Li1 C31 C30 -51.66(18) . . . . ? Mg1 Li1 C31 C30 -35.7(3) . . . . ? N3 Li1 C31 C32 82(7) . . . . ? N4 Li1 C31 C32 170.8(2) . . . . ? C33 Li1 C31 C32 -103.19(16) . . . . ? Mg2 Li1 C31 C32 -149.56(15) . . . . ? Mg1 Li1 C31 C32 -133.6(2) . . . . ? N4 Mg2 C33 C34 -88.6(2) . . . . ? N2 Mg2 C33 C34 74.4(2) . . . . ? C1 Mg2 C33 C34 169.9(2) . . . . ? Li1 Mg2 C33 C34 -118.8(2) . . . . ? Li2 Mg2 C33 C34 116.1(2) . . . . ? Mg1 Mg2 C33 C34 168.8(3) . . . . ? N4 Mg2 C33 Mg1 102.69(6) . . . . ? N2 Mg2 C33 Mg1 -94.35(6) . . . . ? C1 Mg2 C33 Mg1 1.17(6) . . . . ? Li1 Mg2 C33 Mg1 72.41(9) . . . . ? Li2 Mg2 C33 Mg1 -52.63(8) . . . . ? N4 Mg2 C33 Li1 30.28(10) . . . . ? N2 Mg2 C33 Li1 -166.76(10) . . . . ? C1 Mg2 C33 Li1 -71.25(10) . . . . ? Li2 Mg2 C33 Li1 -125.05(11) . . . . ? Mg1 Mg2 C33 Li1 -72.41(9) . . . . ? N1 Mg1 C33 C34 -73.8(2) . . . . ? N3 Mg1 C33 C34 89.4(2) . . . . ? C1 Mg1 C33 C34 -171.43(19) . . . . ? Li2 Mg1 C33 C34 -117.1(2) . . . . ? Li1 Mg1 C33 C34 117.6(2) . . . . ? Mg2 Mg1 C33 C34 -170.3(2) . . . . ? N1 Mg1 C33 Mg2 96.50(7) . . . . ? N3 Mg1 C33 Mg2 -100.36(6) . . . . ? C1 Mg1 C33 Mg2 -1.18(7) . . . . ? Li2 Mg1 C33 Mg2 53.11(8) . . . . ? Li1 Mg1 C33 Mg2 -72.11(10) . . . . ? N1 Mg1 C33 Li1 168.60(10) . . . . ? N3 Mg1 C33 Li1 -28.25(10) . . . . ? C1 Mg1 C33 Li1 70.93(10) . . . . ? Li2 Mg1 C33 Li1 125.21(12) . . . . ? Mg2 Mg1 C33 Li1 72.11(10) . . . . ? N3 Li1 C33 C34 -102.5(2) . . . . ? N4 Li1 C33 C34 109.64(19) . . . . ? C31 Li1 C33 C34 77.68(19) . . . . ? Mg2 Li1 C33 C34 139.24(19) . . . . ? Mg1 Li1 C33 C34 -130.42(19) . . . . ? N3 Li1 C33 Mg2 118.31(13) . . . . ? N4 Li1 C33 Mg2 -29.59(9) . . . . ? C31 Li1 C33 Mg2 -61.56(9) . . . . ? Mg1 Li1 C33 Mg2 90.34(7) . . . . ? N3 Li1 C33 Mg1 27.97(10) . . . . ? N4 Li1 C33 Mg1 -119.94(13) . . . . ? C31 Li1 C33 Mg1 -151.90(12) . . . . ? Mg2 Li1 C33 Mg1 -90.34(7) . . . . ? Mg2 C33 C34 C35 -8(12) . . . . ? Mg1 C33 C34 C35 156(12) . . . . ? Li1 C33 C34 C35 -109(12) . . . . ? C33 C34 C35 C36 -165(100) . . . . ? C33 C34 C35 C40 14(12) . . . . ? C40 C35 C36 C37 0.4(3) . . . . ? C34 C35 C36 C37 179.67(19) . . . . ? C35 C36 C37 C38 -0.3(3) . . . . ? C36 C37 C38 C39 0.1(3) . . . . ? C37 C38 C39 C40 -0.1(3) . . . . ? C38 C39 C40 C35 0.2(3) . . . . ? C36 C35 C40 C39 -0.4(3) . . . . ? C34 C35 C40 C39 -179.64(19) . . . . ? C14 C13 N1 C10 -71.5(2) . . . . ? C12 C13 N1 C10 55.2(2) . . . . ? C14 C13 N1 Mg1 75.30(19) . . . . ? C12 C13 N1 Mg1 -157.98(14) . . . . ? C14 C13 N1 Li2 170.80(17) . . . . ? C12 C13 N1 Li2 -62.5(2) . . . . ? C9 C10 N1 C13 132.23(19) . . . . ? C11 C10 N1 C13 -105.0(2) . . . . ? C9 C10 N1 Mg1 -14.8(2) . . . . ? C11 C10 N1 Mg1 107.99(17) . . . . ? C9 C10 N1 Li2 -110.01(19) . . . . ? C11 C10 N1 Li2 12.8(2) . . . . ? N3 Mg1 N1 C13 -94.9(2) . . . . ? C1 Mg1 N1 C13 137.26(15) . . . . ? C33 Mg1 N1 C13 40.29(16) . . . . ? Li2 Mg1 N1 C13 107.91(18) . . . . ? Li1 Mg1 N1 C13 64.6(3) . . . . ? Mg2 Mg1 N1 C13 88.82(14) . . . . ? N3 Mg1 N1 C10 49.6(2) . . . . ? C1 Mg1 N1 C10 -78.28(15) . . . . ? C33 Mg1 N1 C10 -175.25(14) . . . . ? Li2 Mg1 N1 C10 -107.63(18) . . . . ? Li1 Mg1 N1 C10 -150.9(2) . . . . ? Mg2 Mg1 N1 C10 -126.72(13) . . . . ? N3 Mg1 N1 Li2 157.22(17) . . . . ? C1 Mg1 N1 Li2 29.34(12) . . . . ? C33 Mg1 N1 Li2 -67.62(12) . . . . ? Li1 Mg1 N1 Li2 -43.3(3) . . . . ? Mg2 Mg1 N1 Li2 -19.10(11) . . . . ? N2 Li2 N1 C13 -55.2(3) . . . . ? C1 Li2 N1 C13 -147.08(13) . . . . ? Mg1 Li2 N1 C13 -120.02(13) . . . . ? Mg2 Li2 N1 C13 -98.43(15) . . . . ? N2 Li2 N1 C10 -175.8(3) . . . . ? C1 Li2 N1 C10 92.33(15) . . . . ? Mg1 Li2 N1 C10 119.39(13) . . . . ? Mg2 Li2 N1 C10 140.99(14) . . . . ? N2 Li2 N1 Mg1 64.8(3) . . . . ? C1 Li2 N1 Mg1 -27.06(10) . . . . ? Mg2 Li2 N1 Mg1 21.59(12) . . . . ? C18 C19 N2 C16 -57.0(2) . . . . ? C20 C19 N2 C16 68.2(2) . . . . ? C18 C19 N2 Mg2 160.63(14) . . . . ? C20 C19 N2 Mg2 -74.2(2) . . . . ? C18 C19 N2 Li2 62.7(2) . . . . ? C20 C19 N2 Li2 -172.08(18) . . . . ? C17 C16 N2 C19 -124.41(19) . . . . ? C15 C16 N2 C19 111.38(19) . . . . ? C17 C16 N2 Mg2 14.6(2) . . . . ? C15 C16 N2 Mg2 -109.58(16) . . . . ? C17 C16 N2 Li2 110.01(19) . . . . ? C15 C16 N2 Li2 -14.2(2) . . . . ? N4 Mg2 N2 C19 86.2(2) . . . . ? C33 Mg2 N2 C19 -51.54(14) . . . . ? C1 Mg2 N2 C19 -148.08(13) . . . . ? Li1 Mg2 N2 C19 -82.0(3) . . . . ? Li2 Mg2 N2 C19 -116.21(17) . . . . ? Mg1 Mg2 N2 C19 -100.65(13) . . . . ? N4 Mg2 N2 C16 -52.0(2) . . . . ? C33 Mg2 N2 C16 170.21(14) . . . . ? C1 Mg2 N2 C16 73.67(15) . . . . ? Li1 Mg2 N2 C16 139.7(2) . . . . ? Li2 Mg2 N2 C16 105.54(18) . . . . ? Mg1 Mg2 N2 C16 121.10(14) . . . . ? N4 Mg2 N2 Li2 -157.56(17) . . . . ? C33 Mg2 N2 Li2 64.67(12) . . . . ? C1 Mg2 N2 Li2 -31.87(12) . . . . ? Li1 Mg2 N2 Li2 34.2(3) . . . . ? Mg1 Mg2 N2 Li2 15.56(11) . . . . ? N1 Li2 N2 C19 52.3(3) . . . . ? C1 Li2 N2 C19 144.56(14) . . . . ? Mg1 Li2 N2 C19 97.01(16) . . . . ? Mg2 Li2 N2 C19 114.81(14) . . . . ? N1 Li2 N2 C16 175.6(3) . . . . ? C1 Li2 N2 C16 -92.14(14) . . . . ? Mg1 Li2 N2 C16 -139.70(14) . . . . ? Mg2 Li2 N2 C16 -121.89(13) . . . . ? N1 Li2 N2 Mg2 -62.5(3) . . . . ? C1 Li2 N2 Mg2 29.75(10) . . . . ? Mg1 Li2 N2 Mg2 -17.80(12) . . . . ? C21 C22 N3 C25 -66.8(2) . . . . ? C23 C22 N3 C25 59.0(2) . . . . ? C21 C22 N3 Mg1 75.70(19) . . . . ? C23 C22 N3 Mg1 -158.45(13) . . . . ? C21 C22 N3 Li1 169.68(17) . . . . ? C23 C22 N3 Li1 -64.5(2) . . . . ? C24 C25 N3 C22 126.24(18) . . . . ? C26 C25 N3 C22 -111.25(18) . . . . ? C24 C25 N3 Mg1 -17.3(2) . . . . ? C26 C25 N3 Mg1 105.15(16) . . . . ? C24 C25 N3 Li1 -114.57(19) . . . . ? C26 C25 N3 Li1 7.9(2) . . . . ? N1 Mg1 N3 C22 -85.6(2) . . . . ? C1 Mg1 N3 C22 41.93(14) . . . . ? C33 Mg1 N3 C22 138.63(13) . . . . ? Li2 Mg1 N3 C22 54.6(2) . . . . ? Li1 Mg1 N3 C22 105.54(17) . . . . ? Mg2 Mg1 N3 C22 90.69(13) . . . . ? N1 Mg1 N3 C25 55.0(2) . . . . ? C1 Mg1 N3 C25 -177.41(13) . . . . ? C33 Mg1 N3 C25 -80.70(13) . . . . ? Li2 Mg1 N3 C25 -164.78(19) . . . . ? Li1 Mg1 N3 C25 -113.79(17) . . . . ? Mg2 Mg1 N3 C25 -128.64(12) . . . . ? N1 Mg1 N3 Li1 168.84(18) . . . . ? C1 Mg1 N3 Li1 -63.61(12) . . . . ? C33 Mg1 N3 Li1 33.09(12) . . . . ? Li2 Mg1 N3 Li1 -51.0(2) . . . . ? Mg2 Mg1 N3 Li1 -14.85(11) . . . . ? N4 Li1 N3 C22 -61.0(4) . . . . ? C33 Li1 N3 C22 -149.28(13) . . . . ? C31 Li1 N3 C22 25(7) . . . . ? Mg2 Li1 N3 C22 -102.47(16) . . . . ? Mg1 Li1 N3 C22 -119.65(13) . . . . ? N4 Li1 N3 C25 176.3(3) . . . . ? C33 Li1 N3 C25 87.98(15) . . . . ? C31 Li1 N3 C25 -97(7) . . . . ? Mg2 Li1 N3 C25 134.79(15) . . . . ? Mg1 Li1 N3 C25 117.60(14) . . . . ? N4 Li1 N3 Mg1 58.7(3) . . . . ? C33 Li1 N3 Mg1 -29.62(10) . . . . ? C31 Li1 N3 Mg1 145(7) . . . . ? Mg2 Li1 N3 Mg1 17.19(13) . . . . ? C27 C28 N4 C31 -67.4(2) . . . . ? C29 C28 N4 C31 59.1(2) . . . . ? C27 C28 N4 Mg2 145.75(14) . . . . ? C29 C28 N4 Mg2 -87.80(17) . . . . ? C27 C28 N4 Li1 48.4(2) . . . . ? C29 C28 N4 Li1 174.82(17) . . . . ? C30 C31 N4 C28 -117.53(18) . . . . ? C32 C31 N4 C28 118.26(18) . . . . ? Li1 C31 N4 C28 127.23(18) . . . . ? C30 C31 N4 Mg2 24.2(2) . . . . ? C32 C31 N4 Mg2 -100.05(17) . . . . ? Li1 C31 N4 Mg2 -91.08(16) . . . . ? C30 C31 N4 Li1 115.24(18) . . . . ? C32 C31 N4 Li1 -8.97(19) . . . . ? N2 Mg2 N4 C28 66.0(2) . . . . ? C33 Mg2 N4 C28 -155.27(13) . . . . ? C1 Mg2 N4 C28 -58.42(14) . . . . ? Li1 Mg2 N4 C28 -120.01(17) . . . . ? Li2 Mg2 N4 C28 -72.0(3) . . . . ? Mg1 Mg2 N4 C28 -107.03(12) . . . . ? N2 Mg2 N4 C31 -75.0(2) . . . . ? C33 Mg2 N4 C31 63.69(15) . . . . ? C1 Mg2 N4 C31 160.54(14) . . . . ? Li1 Mg2 N4 C31 98.95(18) . . . . ? Li2 Mg2 N4 C31 146.9(2) . . . . ? Mg1 Mg2 N4 C31 111.93(14) . . . . ? N2 Mg2 N4 Li1 -173.96(17) . . . . ? C33 Mg2 N4 Li1 -35.26(12) . . . . ? C1 Mg2 N4 Li1 61.59(12) . . . . ? Li2 Mg2 N4 Li1 48.0(2) . . . . ? Mg1 Mg2 N4 Li1 12.99(11) . . . . ? N3 Li1 N4 C28 56.1(4) . . . . ? C33 Li1 N4 C28 144.73(14) . . . . ? C31 Li1 N4 C28 -121.16(18) . . . . ? Mg2 Li1 N4 C28 113.43(15) . . . . ? Mg1 Li1 N4 C28 98.56(17) . . . . ? N3 Li1 N4 C31 177.3(3) . . . . ? C33 Li1 N4 C31 -94.11(13) . . . . ? Mg2 Li1 N4 C31 -125.41(12) . . . . ? Mg1 Li1 N4 C31 -140.28(14) . . . . ? N3 Li1 N4 Mg2 -57.3(3) . . . . ? C33 Li1 N4 Mg2 31.30(9) . . . . ? C31 Li1 N4 Mg2 125.41(12) . . . . ? Mg1 Li1 N4 Mg2 -14.87(12) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.360 _refine_diff_density_min -0.236 _refine_diff_density_rms 0.046 #===END #--------------------------------------------- # --------- COMPOUND 4------------------------ #--------------------------------------------- data_grem205 _database_code_depnum_ccdc_archive 'CCDC 664920' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C56 H80 Mg2 N6 Na2' _chemical_formula_weight 931.86 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mg Mg 0.0486 0.0363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.7683(5) _cell_length_b 12.0499(6) _cell_length_c 12.3553(6) _cell_angle_alpha 75.407(2) _cell_angle_beta 78.428(2) _cell_angle_gamma 65.633(2) _cell_volume 1404.75(12) _cell_formula_units_Z 1 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 5441 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 26.02 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.33 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.102 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 504 _exptl_absorpt_coefficient_mu 0.098 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method 'omega and phi scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23308 _diffrn_reflns_av_R_equivalents 0.037 _diffrn_reflns_av_sigmaI/netI 0.0356 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.71 _diffrn_reflns_theta_max 26.00 _reflns_number_total 5482 _reflns_number_gt 4424 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Collect and Denzo' _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution Shelxs97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0637P)^2^+0.7378P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5482 _refine_ls_number_parameters 306 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0636 _refine_ls_R_factor_gt 0.0479 _refine_ls_wR_factor_ref 0.1313 _refine_ls_wR_factor_gt 0.1212 _refine_ls_goodness_of_fit_ref 1.020 _refine_ls_restrained_S_all 1.020 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Na1 Na 0.05420(8) 0.27084(7) 0.71454(6) 0.0362(2) Uani 1 1 d . . . Mg1 Mg 0.02113(5) 0.43551(5) 0.90703(4) 0.02133(15) Uani 1 1 d . . . N1 N 0.11253(14) 0.54764(13) 0.93845(12) 0.0248(3) Uani 1 1 d . . . N2 N 0.1466(2) 0.13589(16) 0.57400(14) 0.0425(4) Uani 1 1 d . . . N3 N -0.10253(18) 0.15986(16) 0.74781(15) 0.0407(4) Uani 1 1 d . . . C1 C 0.0941(2) 0.67204(17) 0.86548(16) 0.0330(4) Uani 1 1 d . . . H1 H 0.1069 0.7239 0.9107 0.040 Uiso 1 1 calc R . . C2 C 0.1882(2) 0.6739(2) 0.75653(18) 0.0473(5) Uani 1 1 d . . . H2A H 0.2826 0.6469 0.7734 0.071 Uiso 1 1 calc R . . H2B H 0.1593 0.7583 0.7119 0.071 Uiso 1 1 calc R . . H2C H 0.1836 0.6175 0.7138 0.071 Uiso 1 1 calc R . . C3 C -0.0533(2) 0.73344(17) 0.83565(17) 0.0362(4) Uani 1 1 d . . . H3A H -0.0667 0.6869 0.7874 0.054 Uiso 1 1 calc R . . H3B H -0.0710 0.8189 0.7957 0.054 Uiso 1 1 calc R . . H3C H -0.1167 0.7339 0.9047 0.054 Uiso 1 1 calc R . . C4 C 0.25435(19) 0.47931(18) 0.97571(16) 0.0318(4) Uani 1 1 d . . . H4 H 0.2447 0.4154 1.0427 0.038 Uiso 1 1 calc R . . C5 C 0.3061(2) 0.5593(2) 1.01916(17) 0.0394(5) Uani 1 1 d . . . H5A H 0.3319 0.6160 0.9555 0.059 Uiso 1 1 calc R . . H5B H 0.3862 0.5056 1.0595 0.059 Uiso 1 1 calc R . . H5C H 0.2333 0.6074 1.0703 0.059 Uiso 1 1 calc R . . C6 C 0.3664(2) 0.4058(2) 0.89353(17) 0.0395(5) Uani 1 1 d . . . H6A H 0.3322 0.3561 0.8650 0.059 Uiso 1 1 calc R . . H6B H 0.4473 0.3509 0.9325 0.059 Uiso 1 1 calc R . . H6C H 0.3915 0.4635 0.8305 0.059 Uiso 1 1 calc R . . C7 C 0.15467(19) 0.24580(17) 0.89142(15) 0.0296(4) Uani 1 1 d . . . C8 C 0.24411(18) 0.14643(17) 0.87676(15) 0.0295(4) Uani 1 1 d . . . C9 C 0.36030(19) 0.03496(16) 0.85594(15) 0.0306(4) Uani 1 1 d . . . C10 C 0.4875(2) 0.0421(2) 0.8146(3) 0.0614(7) Uani 1 1 d . . . H10 H 0.4977 0.1188 0.8047 0.074 Uiso 1 1 calc R . . C11 C 0.5993(2) -0.0611(2) 0.7876(3) 0.0724(9) Uani 1 1 d . . . H11 H 0.6852 -0.0544 0.7591 0.087 Uiso 1 1 calc R . . C12 C 0.5871(2) -0.1730(2) 0.8018(2) 0.0500(6) Uani 1 1 d . . . H12 H 0.6644 -0.2439 0.7847 0.060 Uiso 1 1 calc R . . C13 C 0.4627(2) -0.18110(19) 0.84099(19) 0.0454(5) Uani 1 1 d . . . H13 H 0.4532 -0.2579 0.8497 0.054 Uiso 1 1 calc R . . C14 C 0.3501(2) -0.07851(18) 0.86817(18) 0.0398(5) Uani 1 1 d . . . H14 H 0.2645 -0.0862 0.8957 0.048 Uiso 1 1 calc R . . C15 C -0.08541(18) 0.48929(16) 0.75659(14) 0.0253(4) Uani 1 1 d . . . C16 C -0.15751(17) 0.51480(15) 0.68213(14) 0.0248(4) Uani 1 1 d . . . C17 C -0.24956(18) 0.55442(16) 0.59698(14) 0.0257(4) Uani 1 1 d . . . C18 C -0.3910(2) 0.5979(2) 0.62587(17) 0.0396(5) Uani 1 1 d . . . H18 H -0.4272 0.5989 0.7025 0.047 Uiso 1 1 calc R . . C19 C -0.4797(2) 0.6398(3) 0.54376(19) 0.0537(6) Uani 1 1 d . . . H19 H -0.5760 0.6687 0.5647 0.064 Uiso 1 1 calc R . . C20 C -0.4290(2) 0.6398(2) 0.43225(19) 0.0501(6) Uani 1 1 d . . . H20 H -0.4900 0.6700 0.3762 0.060 Uiso 1 1 calc R . . C21 C -0.2892(2) 0.5959(2) 0.40214(16) 0.0387(5) Uani 1 1 d . . . H21 H -0.2541 0.5951 0.3253 0.046 Uiso 1 1 calc R . . C22 C -0.19993(19) 0.55296(18) 0.48329(15) 0.0299(4) Uani 1 1 d . . . H22 H -0.1038 0.5221 0.4617 0.036 Uiso 1 1 calc R . . C23 C 0.2969(3) 0.0811(2) 0.5545(2) 0.0578(6) Uani 1 1 d . . . H23A H 0.3343 0.0341 0.6257 0.087 Uiso 1 1 calc R . . H23B H 0.3320 0.1472 0.5240 0.087 Uiso 1 1 calc R . . H23C H 0.3247 0.0254 0.5008 0.087 Uiso 1 1 calc R . . C24 C 0.0925(3) 0.2034(2) 0.46659(18) 0.0554(7) Uani 1 1 d . . . H24A H 0.1070 0.1443 0.4190 0.083 Uiso 1 1 calc R . . H24B H 0.1403 0.2590 0.4287 0.083 Uiso 1 1 calc R . . H24C H -0.0058 0.2523 0.4801 0.083 Uiso 1 1 calc R . . C25 C 0.0936(3) 0.03786(19) 0.62402(17) 0.0461(6) Uani 1 1 d . . . H25A H 0.1416 -0.0134 0.6908 0.055 Uiso 1 1 calc R . . H25B H 0.1155 -0.0165 0.5690 0.055 Uiso 1 1 calc R . . C26 C -0.0592(3) 0.0855(2) 0.65901(18) 0.0468(6) Uani 1 1 d . . . H26A H -0.1073 0.1369 0.5923 0.056 Uiso 1 1 calc R . . H26B H -0.0876 0.0140 0.6861 0.056 Uiso 1 1 calc R . . C27 C -0.0768(3) 0.0794(2) 0.85821(19) 0.0524(6) Uani 1 1 d . . . H27A H -0.1000 0.1304 0.9154 0.079 Uiso 1 1 calc R . . H27B H 0.0203 0.0242 0.8569 0.079 Uiso 1 1 calc R . . H27C H -0.1334 0.0296 0.8763 0.079 Uiso 1 1 calc R . . C28 C -0.2495(2) 0.2383(2) 0.7491(3) 0.0625(7) Uani 1 1 d . . . H28A H -0.3026 0.1857 0.7648 0.094 Uiso 1 1 calc R . . H28B H -0.2672 0.2934 0.6757 0.094 Uiso 1 1 calc R . . H28C H -0.2767 0.2882 0.8077 0.094 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Na1 0.0448(5) 0.0323(4) 0.0374(4) -0.0146(3) -0.0100(3) -0.0134(3) Mg1 0.0221(3) 0.0231(3) 0.0195(3) -0.0069(2) -0.0023(2) -0.0076(2) N1 0.0264(8) 0.0250(7) 0.0227(7) -0.0062(6) -0.0051(6) -0.0074(6) N2 0.0672(13) 0.0382(9) 0.0290(9) -0.0055(7) -0.0071(8) -0.0267(9) N3 0.0467(10) 0.0373(9) 0.0481(10) -0.0112(8) -0.0122(8) -0.0209(8) C1 0.0413(11) 0.0302(10) 0.0322(10) -0.0061(8) -0.0033(8) -0.0186(8) C2 0.0547(14) 0.0421(12) 0.0396(12) 0.0002(9) -0.0010(10) -0.0197(10) C3 0.0463(12) 0.0264(9) 0.0340(10) 0.0000(8) -0.0108(9) -0.0125(8) C4 0.0284(10) 0.0380(10) 0.0318(10) -0.0073(8) -0.0034(8) -0.0149(8) C5 0.0353(11) 0.0543(13) 0.0374(11) -0.0128(9) -0.0026(9) -0.0242(10) C6 0.0273(10) 0.0548(13) 0.0400(11) -0.0165(10) -0.0010(8) -0.0159(9) C7 0.0307(10) 0.0294(9) 0.0282(9) -0.0076(7) -0.0053(7) -0.0088(8) C8 0.0301(10) 0.0287(9) 0.0289(9) -0.0064(7) -0.0056(7) -0.0089(8) C9 0.0297(10) 0.0266(9) 0.0323(10) -0.0073(7) -0.0061(8) -0.0053(7) C10 0.0316(12) 0.0369(12) 0.118(2) -0.0254(14) -0.0035(13) -0.0115(10) C11 0.0302(12) 0.0473(14) 0.137(3) -0.0313(16) 0.0049(14) -0.0110(11) C12 0.0349(11) 0.0321(11) 0.0724(16) -0.0154(11) -0.0011(11) -0.0015(9) C13 0.0453(13) 0.0256(10) 0.0569(14) -0.0084(9) 0.0060(10) -0.0103(9) C14 0.0354(11) 0.0330(10) 0.0449(12) -0.0075(9) 0.0076(9) -0.0127(9) C15 0.0277(9) 0.0258(9) 0.0231(8) -0.0064(7) -0.0009(7) -0.0106(7) C16 0.0278(9) 0.0250(8) 0.0226(8) -0.0057(7) 0.0002(7) -0.0118(7) C17 0.0282(9) 0.0281(9) 0.0238(8) -0.0045(7) -0.0052(7) -0.0129(7) C18 0.0309(10) 0.0580(13) 0.0283(10) -0.0098(9) -0.0005(8) -0.0158(9) C19 0.0265(11) 0.0838(18) 0.0449(13) -0.0097(12) -0.0071(9) -0.0154(11) C20 0.0397(12) 0.0748(16) 0.0380(12) -0.0025(11) -0.0191(10) -0.0219(11) C21 0.0426(12) 0.0576(13) 0.0231(9) -0.0080(9) -0.0052(8) -0.0253(10) C22 0.0279(9) 0.0384(10) 0.0267(9) -0.0086(8) -0.0023(7) -0.0149(8) C23 0.0701(17) 0.0617(16) 0.0402(13) -0.0151(11) 0.0018(12) -0.0242(13) C24 0.096(2) 0.0478(13) 0.0350(12) 0.0023(10) -0.0157(12) -0.0424(14) C25 0.0816(17) 0.0330(11) 0.0295(10) -0.0077(8) -0.0043(10) -0.0273(11) C26 0.0798(17) 0.0384(11) 0.0397(11) -0.0029(9) -0.0175(11) -0.0373(12) C27 0.0640(16) 0.0604(15) 0.0397(12) -0.0136(11) -0.0015(11) -0.0300(12) C28 0.0459(14) 0.0541(15) 0.101(2) -0.0202(14) -0.0201(14) -0.0243(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 Na1 N2 2.4584(19) . ? Na1 N3 2.4724(18) . ? Na1 C7 2.5268(19) . ? Na1 C15 2.5631(18) . ? Na1 C8 2.8367(19) . ? Na1 C16 2.8710(19) . ? Na1 C25 3.118(2) . ? Na1 Mg1 3.3430(9) . ? Mg1 N1 2.1118(15) . ? Mg1 N1 2.1469(15) 2_567 ? Mg1 C7 2.1747(19) . ? Mg1 C15 2.1968(18) . ? Mg1 Mg1 2.9490(10) 2_567 ? N1 C1 1.498(2) . ? N1 C4 1.509(2) . ? N1 Mg1 2.1469(15) 2_567 ? N2 C24 1.462(3) . ? N2 C25 1.466(3) . ? N2 C23 1.468(3) . ? N3 C27 1.463(3) . ? N3 C28 1.470(3) . ? N3 C26 1.473(3) . ? C1 C2 1.515(3) . ? C1 C3 1.526(3) . ? C1 H1 1.0000 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 C6 1.534(3) . ? C4 C5 1.534(3) . ? C4 H4 1.0000 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 C8 1.217(3) . ? C8 C9 1.447(2) . ? C9 C14 1.385(3) . ? C9 C10 1.392(3) . ? C10 C11 1.386(3) . ? C10 H10 0.9500 . ? C11 C12 1.372(3) . ? C11 H11 0.9500 . ? C12 C13 1.365(3) . ? C12 H12 0.9500 . ? C13 C14 1.385(3) . ? C13 H13 0.9500 . ? C14 H14 0.9500 . ? C15 C16 1.221(2) . ? C16 C17 1.446(2) . ? C17 C18 1.393(3) . ? C17 C22 1.401(2) . ? C18 C19 1.389(3) . ? C18 H18 0.9500 . ? C19 C20 1.377(3) . ? C19 H19 0.9500 . ? C20 C21 1.378(3) . ? C20 H20 0.9500 . ? C21 C22 1.383(3) . ? C21 H21 0.9500 . ? C22 H22 0.9500 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C26 1.512(3) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Na1 N3 76.18(6) . . ? N2 Na1 C7 127.50(7) . . ? N3 Na1 C7 111.89(7) . . ? N2 Na1 C15 147.71(6) . . ? N3 Na1 C15 108.16(6) . . ? C7 Na1 C15 81.65(6) . . ? N2 Na1 C8 102.19(6) . . ? N3 Na1 C8 106.97(6) . . ? C7 Na1 C8 25.40(5) . . ? C15 Na1 C8 106.68(6) . . ? N2 Na1 C16 124.77(6) . . ? N3 Na1 C16 95.26(6) . . ? C7 Na1 C16 106.58(6) . . ? C15 Na1 C16 25.16(5) . . ? C8 Na1 C16 131.78(6) . . ? N2 Na1 C25 27.35(6) . . ? N3 Na1 C25 51.51(6) . . ? C7 Na1 C25 120.18(6) . . ? C15 Na1 C25 153.23(7) . . ? C8 Na1 C25 97.01(6) . . ? C16 Na1 C25 129.44(6) . . ? N2 Na1 Mg1 164.02(6) . . ? N3 Na1 Mg1 116.52(5) . . ? C7 Na1 Mg1 40.58(4) . . ? C15 Na1 Mg1 41.07(4) . . ? C8 Na1 Mg1 65.75(4) . . ? C16 Na1 Mg1 66.05(4) . . ? C25 Na1 Mg1 156.81(5) . . ? N1 Mg1 N1 92.36(6) . 2_567 ? N1 Mg1 C7 117.08(7) . . ? N1 Mg1 C7 114.38(7) 2_567 . ? N1 Mg1 C15 120.82(6) . . ? N1 Mg1 C15 114.19(6) 2_567 . ? C7 Mg1 C15 99.14(7) . . ? N1 Mg1 Mg1 46.67(4) . 2_567 ? N1 Mg1 Mg1 45.69(4) 2_567 2_567 ? C7 Mg1 Mg1 128.79(6) . 2_567 ? C15 Mg1 Mg1 131.70(5) . 2_567 ? N1 Mg1 Na1 138.73(5) . . ? N1 Mg1 Na1 128.84(5) 2_567 . ? C7 Mg1 Na1 49.10(5) . . ? C15 Mg1 Na1 50.05(5) . . ? Mg1 Mg1 Na1 174.17(3) 2_567 . ? C1 N1 C4 112.77(14) . . ? C1 N1 Mg1 120.88(11) . . ? C4 N1 Mg1 115.51(11) . . ? C1 N1 Mg1 111.49(11) . 2_567 ? C4 N1 Mg1 104.12(10) . 2_567 ? Mg1 N1 Mg1 87.64(6) . 2_567 ? C24 N2 C25 110.67(17) . . ? C24 N2 C23 108.72(19) . . ? C25 N2 C23 109.77(18) . . ? C24 N2 Na1 110.39(14) . . ? C25 N2 Na1 102.23(12) . . ? C23 N2 Na1 114.94(14) . . ? C27 N3 C28 109.1(2) . . ? C27 N3 C26 110.68(17) . . ? C28 N3 C26 110.30(18) . . ? C27 N3 Na1 104.61(13) . . ? C28 N3 Na1 115.85(13) . . ? C26 N3 Na1 106.14(13) . . ? N1 C1 C2 116.90(16) . . ? N1 C1 C3 108.07(15) . . ? C2 C1 C3 107.63(17) . . ? N1 C1 H1 108.0 . . ? C2 C1 H1 108.0 . . ? C3 C1 H1 108.0 . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? N1 C4 C6 116.87(15) . . ? N1 C4 C5 113.95(16) . . ? C6 C4 C5 109.87(16) . . ? N1 C4 H4 105.0 . . ? C6 C4 H4 105.0 . . ? C5 C4 H4 105.0 . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C4 C6 H6A 109.5 . . ? C4 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C4 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C8 C7 Mg1 170.56(17) . . ? C8 C7 Na1 91.68(13) . . ? Mg1 C7 Na1 90.32(6) . . ? C7 C8 C9 174.0(2) . . ? C7 C8 Na1 62.92(11) . . ? C9 C8 Na1 118.62(12) . . ? C14 C9 C10 117.46(18) . . ? C14 C9 C8 123.19(18) . . ? C10 C9 C8 119.22(18) . . ? C11 C10 C9 120.9(2) . . ? C11 C10 H10 119.5 . . ? C9 C10 H10 119.5 . . ? C12 C11 C10 120.5(2) . . ? C12 C11 H11 119.7 . . ? C10 C11 H11 119.7 . . ? C13 C12 C11 119.3(2) . . ? C13 C12 H12 120.4 . . ? C11 C12 H12 120.4 . . ? C12 C13 C14 120.7(2) . . ? C12 C13 H13 119.7 . . ? C14 C13 H13 119.7 . . ? C9 C14 C13 121.14(19) . . ? C9 C14 H14 119.4 . . ? C13 C14 H14 119.4 . . ? C16 C15 Mg1 171.66(15) . . ? C16 C15 Na1 91.67(12) . . ? Mg1 C15 Na1 88.88(6) . . ? C15 C16 C17 175.36(18) . . ? C15 C16 Na1 63.17(11) . . ? C17 C16 Na1 121.45(11) . . ? C18 C17 C22 118.05(16) . . ? C18 C17 C16 120.58(16) . . ? C22 C17 C16 121.35(16) . . ? C19 C18 C17 120.67(18) . . ? C19 C18 H18 119.7 . . ? C17 C18 H18 119.7 . . ? C20 C19 C18 120.4(2) . . ? C20 C19 H19 119.8 . . ? C18 C19 H19 119.8 . . ? C19 C20 C21 119.79(19) . . ? C19 C20 H20 120.1 . . ? C21 C20 H20 120.1 . . ? C20 C21 C22 120.31(18) . . ? C20 C21 H21 119.8 . . ? C22 C21 H21 119.8 . . ? C21 C22 C17 120.77(17) . . ? C21 C22 H22 119.6 . . ? C17 C22 H22 119.6 . . ? N2 C23 H23A 109.5 . . ? N2 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? N2 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? N2 C24 H24A 109.5 . . ? N2 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? N2 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N2 C25 C26 114.00(18) . . ? N2 C25 Na1 50.41(9) . . ? C26 C25 Na1 79.61(11) . . ? N2 C25 H25A 108.8 . . ? C26 C25 H25A 108.8 . . ? Na1 C25 H25A 87.5 . . ? N2 C25 H25B 108.8 . . ? C26 C25 H25B 108.8 . . ? Na1 C25 H25B 158.3 . . ? H25A C25 H25B 107.6 . . ? N3 C26 C25 113.61(17) . . ? N3 C26 H26A 108.8 . . ? C25 C26 H26A 108.8 . . ? N3 C26 H26B 108.8 . . ? C25 C26 H26B 108.8 . . ? H26A C26 H26B 107.7 . . ? N3 C27 H27A 109.5 . . ? N3 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? N3 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? N3 C28 H28A 109.5 . . ? N3 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? N3 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Na1 Mg1 N1 38.4(2) . . . . ? N3 Na1 Mg1 N1 179.06(8) . . . . ? C7 Na1 Mg1 N1 85.74(9) . . . . ? C15 Na1 Mg1 N1 -93.37(9) . . . . ? C8 Na1 Mg1 N1 81.42(8) . . . . ? C16 Na1 Mg1 N1 -97.23(8) . . . . ? C25 Na1 Mg1 N1 126.05(15) . . . . ? N2 Na1 Mg1 N1 -137.52(18) . . . 2_567 ? N3 Na1 Mg1 N1 3.11(8) . . . 2_567 ? C7 Na1 Mg1 N1 -90.21(9) . . . 2_567 ? C15 Na1 Mg1 N1 90.68(8) . . . 2_567 ? C8 Na1 Mg1 N1 -94.54(7) . . . 2_567 ? C16 Na1 Mg1 N1 86.82(7) . . . 2_567 ? C25 Na1 Mg1 N1 -49.90(15) . . . 2_567 ? N2 Na1 Mg1 C7 -47.31(19) . . . . ? N3 Na1 Mg1 C7 93.32(9) . . . . ? C15 Na1 Mg1 C7 -179.11(9) . . . . ? C8 Na1 Mg1 C7 -4.33(8) . . . . ? C16 Na1 Mg1 C7 177.03(8) . . . . ? C25 Na1 Mg1 C7 40.31(15) . . . . ? N2 Na1 Mg1 C15 131.8(2) . . . . ? N3 Na1 Mg1 C15 -87.57(8) . . . . ? C7 Na1 Mg1 C15 179.11(9) . . . . ? C8 Na1 Mg1 C15 174.78(8) . . . . ? C16 Na1 Mg1 C15 -3.86(7) . . . . ? C25 Na1 Mg1 C15 -140.58(15) . . . . ? N2 Na1 Mg1 Mg1 -118.4(3) . . . 2_567 ? N3 Na1 Mg1 Mg1 22.3(3) . . . 2_567 ? C7 Na1 Mg1 Mg1 -71.1(3) . . . 2_567 ? C15 Na1 Mg1 Mg1 109.8(3) . . . 2_567 ? C8 Na1 Mg1 Mg1 -75.4(3) . . . 2_567 ? C16 Na1 Mg1 Mg1 106.0(3) . . . 2_567 ? C25 Na1 Mg1 Mg1 -30.7(4) . . . 2_567 ? N1 Mg1 N1 C1 -113.75(14) 2_567 . . . ? C7 Mg1 N1 C1 127.24(13) . . . . ? C15 Mg1 N1 C1 6.40(15) . . . . ? Mg1 Mg1 N1 C1 -113.75(14) 2_567 . . . ? Na1 Mg1 N1 C1 69.41(14) . . . . ? N1 Mg1 N1 C4 104.53(12) 2_567 . . . ? C7 Mg1 N1 C4 -14.48(14) . . . . ? C15 Mg1 N1 C4 -135.33(12) . . . . ? Mg1 Mg1 N1 C4 104.53(12) 2_567 . . . ? Na1 Mg1 N1 C4 -72.32(13) . . . . ? N1 Mg1 N1 Mg1 0.0 2_567 . . 2_567 ? C7 Mg1 N1 Mg1 -119.01(7) . . . 2_567 ? C15 Mg1 N1 Mg1 120.14(7) . . . 2_567 ? Na1 Mg1 N1 Mg1 -176.85(5) . . . 2_567 ? N3 Na1 N2 C24 94.63(15) . . . . ? C7 Na1 N2 C24 -158.20(14) . . . . ? C15 Na1 N2 C24 -7.6(2) . . . . ? C8 Na1 N2 C24 -160.63(15) . . . . ? C16 Na1 N2 C24 7.83(18) . . . . ? C25 Na1 N2 C24 117.8(2) . . . . ? Mg1 Na1 N2 C24 -121.1(2) . . . . ? N3 Na1 N2 C25 -23.14(13) . . . . ? C7 Na1 N2 C25 84.03(16) . . . . ? C15 Na1 N2 C25 -125.35(15) . . . . ? C8 Na1 N2 C25 81.60(14) . . . . ? C16 Na1 N2 C25 -109.94(13) . . . . ? Mg1 Na1 N2 C25 121.1(2) . . . . ? N3 Na1 N2 C23 -141.98(16) . . . . ? C7 Na1 N2 C23 -34.81(18) . . . . ? C15 Na1 N2 C23 115.80(17) . . . . ? C8 Na1 N2 C23 -37.24(16) . . . . ? C16 Na1 N2 C23 131.22(14) . . . . ? C25 Na1 N2 C23 -118.8(2) . . . . ? Mg1 Na1 N2 C23 2.2(3) . . . . ? N2 Na1 N3 C27 112.17(14) . . . . ? C7 Na1 N3 C27 -13.05(15) . . . . ? C15 Na1 N3 C27 -101.17(14) . . . . ? C8 Na1 N3 C27 13.41(15) . . . . ? C16 Na1 N3 C27 -123.28(14) . . . . ? C25 Na1 N3 C27 98.83(15) . . . . ? Mg1 Na1 N3 C27 -57.47(14) . . . . ? N2 Na1 N3 C28 -127.72(18) . . . . ? C7 Na1 N3 C28 107.06(17) . . . . ? C15 Na1 N3 C28 18.95(18) . . . . ? C8 Na1 N3 C28 133.52(17) . . . . ? C16 Na1 N3 C28 -3.17(18) . . . . ? C25 Na1 N3 C28 -141.05(19) . . . . ? Mg1 Na1 N3 C28 62.64(18) . . . . ? N2 Na1 N3 C26 -4.92(13) . . . . ? C7 Na1 N3 C26 -130.14(13) . . . . ? C15 Na1 N3 C26 141.74(13) . . . . ? C8 Na1 N3 C26 -103.68(13) . . . . ? C16 Na1 N3 C26 119.63(13) . . . . ? C25 Na1 N3 C26 -18.26(12) . . . . ? Mg1 Na1 N3 C26 -174.56(11) . . . . ? C4 N1 C1 C2 59.9(2) . . . . ? Mg1 N1 C1 C2 -82.80(19) . . . . ? Mg1 N1 C1 C2 176.60(14) 2_567 . . . ? C4 N1 C1 C3 -178.59(14) . . . . ? Mg1 N1 C1 C3 38.73(18) . . . . ? Mg1 N1 C1 C3 -61.88(16) 2_567 . . . ? C1 N1 C4 C6 -83.7(2) . . . . ? Mg1 N1 C4 C6 61.14(19) . . . . ? Mg1 N1 C4 C6 155.33(14) 2_567 . . . ? C1 N1 C4 C5 46.3(2) . . . . ? Mg1 N1 C4 C5 -168.93(12) . . . . ? Mg1 N1 C4 C5 -74.74(16) 2_567 . . . ? N1 Mg1 C7 C8 -30.1(10) . . . . ? N1 Mg1 C7 C8 -136.5(9) 2_567 . . . ? C15 Mg1 C7 C8 101.6(9) . . . . ? Mg1 Mg1 C7 C8 -84.8(9) 2_567 . . . ? Na1 Mg1 C7 C8 102.3(9) . . . . ? N1 Mg1 C7 Na1 -132.38(6) . . . . ? N1 Mg1 C7 Na1 121.22(6) 2_567 . . . ? C15 Mg1 C7 Na1 -0.69(7) . . . . ? Mg1 Mg1 C7 Na1 172.92(4) 2_567 . . . ? N2 Na1 C7 C8 -5.55(17) . . . . ? N3 Na1 C7 C8 83.53(14) . . . . ? C15 Na1 C7 C8 -170.18(14) . . . . ? C16 Na1 C7 C8 -173.60(12) . . . . ? C25 Na1 C7 C8 26.37(16) . . . . ? Mg1 Na1 C7 C8 -170.77(17) . . . . ? N2 Na1 C7 Mg1 165.22(7) . . . . ? N3 Na1 C7 Mg1 -105.70(7) . . . . ? C15 Na1 C7 Mg1 0.59(6) . . . . ? C8 Na1 C7 Mg1 170.77(17) . . . . ? C16 Na1 C7 Mg1 -2.83(8) . . . . ? C25 Na1 C7 Mg1 -162.86(7) . . . . ? Mg1 C7 C8 C9 4(3) . . . . ? Na1 C7 C8 C9 106.3(18) . . . . ? Mg1 C7 C8 Na1 -102.2(9) . . . . ? N2 Na1 C8 C7 175.50(14) . . . . ? N3 Na1 C8 C7 -105.42(14) . . . . ? C15 Na1 C8 C7 10.15(14) . . . . ? C16 Na1 C8 C7 8.23(16) . . . . ? C25 Na1 C8 C7 -157.24(14) . . . . ? Mg1 Na1 C8 C7 6.57(12) . . . . ? N2 Na1 C8 C9 2.08(15) . . . . ? N3 Na1 C8 C9 81.16(15) . . . . ? C7 Na1 C8 C9 -173.4(2) . . . . ? C15 Na1 C8 C9 -163.28(14) . . . . ? C16 Na1 C8 C9 -165.19(13) . . . . ? C25 Na1 C8 C9 29.34(15) . . . . ? Mg1 Na1 C8 C9 -166.85(15) . . . . ? C7 C8 C9 C14 -179(100) . . . . ? Na1 C8 C9 C14 -75.6(2) . . . . ? C7 C8 C9 C10 -3.2(19) . . . . ? Na1 C8 C9 C10 100.0(2) . . . . ? C14 C9 C10 C11 -0.4(4) . . . . ? C8 C9 C10 C11 -176.3(3) . . . . ? C9 C10 C11 C12 -0.4(5) . . . . ? C10 C11 C12 C13 1.2(5) . . . . ? C11 C12 C13 C14 -1.2(4) . . . . ? C10 C9 C14 C13 0.5(3) . . . . ? C8 C9 C14 C13 176.2(2) . . . . ? C12 C13 C14 C9 0.3(4) . . . . ? N1 Mg1 C15 C16 -136.2(10) . . . . ? N1 Mg1 C15 C16 -27.5(10) 2_567 . . . ? C7 Mg1 C15 C16 94.6(10) . . . . ? Mg1 Mg1 C15 C16 -78.8(10) 2_567 . . . ? Na1 Mg1 C15 C16 93.9(10) . . . . ? N1 Mg1 C15 Na1 129.94(6) . . . . ? N1 Mg1 C15 Na1 -121.36(6) 2_567 . . . ? C7 Mg1 C15 Na1 0.68(7) . . . . ? Mg1 Mg1 C15 Na1 -172.65(5) 2_567 . . . ? N2 Na1 C15 C16 30.91(19) . . . . ? N3 Na1 C15 C16 -61.87(13) . . . . ? C7 Na1 C15 C16 -172.26(12) . . . . ? C8 Na1 C15 C16 -176.64(11) . . . . ? C25 Na1 C15 C16 -25.4(2) . . . . ? Mg1 Na1 C15 C16 -171.68(15) . . . . ? N2 Na1 C15 Mg1 -157.41(11) . . . . ? N3 Na1 C15 Mg1 109.81(7) . . . . ? C7 Na1 C15 Mg1 -0.58(6) . . . . ? C8 Na1 C15 Mg1 -4.96(7) . . . . ? C16 Na1 C15 Mg1 171.68(15) . . . . ? C25 Na1 C15 Mg1 146.27(12) . . . . ? Mg1 C15 C16 C17 81(3) . . . . ? Na1 C15 C16 C17 174(2) . . . . ? Mg1 C15 C16 Na1 -93.7(10) . . . . ? N2 Na1 C16 C15 -160.48(12) . . . . ? N3 Na1 C16 C15 122.70(12) . . . . ? C7 Na1 C16 C15 7.99(13) . . . . ? C8 Na1 C16 C15 4.32(15) . . . . ? C25 Na1 C16 C15 165.51(12) . . . . ? Mg1 Na1 C16 C15 5.97(11) . . . . ? N2 Na1 C16 C17 20.07(16) . . . . ? N3 Na1 C16 C17 -56.75(14) . . . . ? C7 Na1 C16 C17 -171.46(13) . . . . ? C15 Na1 C16 C17 -179.4(2) . . . . ? C8 Na1 C16 C17 -175.13(12) . . . . ? C25 Na1 C16 C17 -13.94(16) . . . . ? Mg1 Na1 C16 C17 -173.48(14) . . . . ? C15 C16 C17 C18 -50(2) . . . . ? Na1 C16 C17 C18 123.92(17) . . . . ? C15 C16 C17 C22 129(2) . . . . ? Na1 C16 C17 C22 -57.5(2) . . . . ? C22 C17 C18 C19 -0.8(3) . . . . ? C16 C17 C18 C19 177.8(2) . . . . ? C17 C18 C19 C20 -0.4(4) . . . . ? C18 C19 C20 C21 1.1(4) . . . . ? C19 C20 C21 C22 -0.6(4) . . . . ? C20 C21 C22 C17 -0.6(3) . . . . ? C18 C17 C22 C21 1.3(3) . . . . ? C16 C17 C22 C21 -177.32(18) . . . . ? C24 N2 C25 C26 -66.2(2) . . . . ? C23 N2 C25 C26 173.81(17) . . . . ? Na1 N2 C25 C26 51.37(18) . . . . ? C24 N2 C25 Na1 -117.6(2) . . . . ? C23 N2 C25 Na1 122.43(17) . . . . ? N3 Na1 C25 N2 150.82(16) . . . . ? C7 Na1 C25 N2 -114.10(14) . . . . ? C15 Na1 C25 N2 104.64(18) . . . . ? C8 Na1 C25 N2 -103.03(14) . . . . ? C16 Na1 C25 N2 90.98(15) . . . . ? Mg1 Na1 C25 N2 -143.23(14) . . . . ? N2 Na1 C25 C26 -133.48(19) . . . . ? N3 Na1 C25 C26 17.34(11) . . . . ? C7 Na1 C25 C26 112.42(12) . . . . ? C15 Na1 C25 C26 -28.8(2) . . . . ? C8 Na1 C25 C26 123.49(12) . . . . ? C16 Na1 C25 C26 -42.50(14) . . . . ? Mg1 Na1 C25 C26 83.29(18) . . . . ? C27 N3 C26 C25 -79.5(2) . . . . ? C28 N3 C26 C25 159.73(19) . . . . ? Na1 N3 C26 C25 33.50(19) . . . . ? N2 C25 C26 N3 -63.0(2) . . . . ? Na1 C25 C26 N3 -25.30(15) . . . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.480 _refine_diff_density_min -0.334 _refine_diff_density_rms 0.043 #===END