# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name "Charles T O'Hara" _publ_contact_author_email CHARLIE.OHARA@STRATH.AC.UK _publ_section_title ; cis-2,6-Dimethylpiperidide: a structural mimic for TMP or DA? ; loop_ _publ_author_name "Charles T O'Hara" 'Ross Campbell' 'Ben Conway' 'Graham S. Fairweather' ; P.Garcia-Alvarez ; 'Alan R Kennedy' 'Jan Klett' 'R E Mulvey' 'Gemma M Robertson' # Attachment 'Revised_cif.cif.cif' data_jkgem2 _database_code_depnum_ccdc_archive 'CCDC 734661' #------------------------------------------------------- #------------------COMPOUND 1-------------------------- #----------------------------------------------------- _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H48 Li N3 Zn' _chemical_formula_weight 414.93 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Li Li -0.0003 0.0001 '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' Zn Zn 0.2839 1.4301 '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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 8.3990(3) _cell_length_b 16.7308(4) _cell_length_c 9.5282(4) _cell_angle_alpha 90.00 _cell_angle_beta 108.761(4) _cell_angle_gamma 90.00 _cell_volume 1267.78(8) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 7953 _cell_measurement_theta_min 2.54 _cell_measurement_theta_max 30.75 _exptl_crystal_description fragment _exptl_crystal_colour colourless _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.087 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 456 _exptl_absorpt_coefficient_mu 0.977 _exptl_absorpt_correction_T_min 0.86814 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET) (compiled Jun 10 2008,16:49:55) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'x-ray tube ' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Gemini S' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12776 _diffrn_reflns_av_R_equivalents 0.0204 _diffrn_reflns_av_sigmaI/netI 0.0338 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.56 _diffrn_reflns_theta_max 30.46 _reflns_number_total 6035 _reflns_number_gt 5446 _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^)+(0.0286P)^2^+0.0000P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.036(7) _chemical_absolute_configuration ad _refine_ls_number_reflns 6035 _refine_ls_number_parameters 248 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0298 _refine_ls_R_factor_gt 0.0252 _refine_ls_wR_factor_ref 0.0512 _refine_ls_wR_factor_gt 0.0504 _refine_ls_goodness_of_fit_ref 0.975 _refine_ls_restrained_S_all 0.975 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Li1 Li 0.1514(3) 0.55719(15) 0.3006(3) 0.0230(5) Uani 1 1 d . . . Zn1 Zn 0.418770(17) 0.492925(13) 0.611238(16) 0.01832(4) Uani 1 1 d . . . C1 C 0.49642(18) 0.60918(9) 0.61555(17) 0.0216(3) Uani 1 1 d . . . C11 C 0.4465(2) 0.65879(11) 0.7291(2) 0.0351(4) Uani 1 1 d . . . H11A H 0.4883 0.7135 0.7297 0.053 Uiso 1 1 calc R . . H11B H 0.4955 0.6351 0.8277 0.053 Uiso 1 1 calc R . . H11C H 0.3237 0.6596 0.7028 0.053 Uiso 1 1 calc R . . C12 C 0.68807(19) 0.60967(11) 0.6572(2) 0.0314(4) Uani 1 1 d . . . H12A H 0.7280 0.6649 0.6612 0.047 Uiso 1 1 calc R . . H12B H 0.7216 0.5799 0.5826 0.047 Uiso 1 1 calc R . . H12C H 0.7375 0.5845 0.7544 0.047 Uiso 1 1 calc R . . C13 C 0.4279(2) 0.64992(10) 0.4649(2) 0.0287(4) Uani 1 1 d . . . H13A H 0.4781 0.7032 0.4700 0.043 Uiso 1 1 calc R . . H13B H 0.3054 0.6550 0.4378 0.043 Uiso 1 1 calc R . . H13C H 0.4560 0.6178 0.3901 0.043 Uiso 1 1 calc R . . C2 C 0.52836(18) 0.41356(9) 0.77849(17) 0.0212(3) Uani 1 1 d . . . C21 C 0.6889(2) 0.38162(11) 0.7544(2) 0.0321(4) Uani 1 1 d . . . H21A H 0.7489 0.3469 0.8374 0.048 Uiso 1 1 calc R . . H21B H 0.7614 0.4265 0.7484 0.048 Uiso 1 1 calc R . . H21C H 0.6590 0.3510 0.6618 0.048 Uiso 1 1 calc R . . C22 C 0.5822(2) 0.45826(11) 0.92646(18) 0.0294(4) Uani 1 1 d . . . H22A H 0.6432 0.4217 1.0060 0.044 Uiso 1 1 calc R . . H22B H 0.4824 0.4787 0.9467 0.044 Uiso 1 1 calc R . . H22C H 0.6555 0.5030 0.9215 0.044 Uiso 1 1 calc R . . C23 C 0.4219(2) 0.34224(11) 0.7932(2) 0.0339(4) Uani 1 1 d . . . H23A H 0.4843 0.3103 0.8795 0.051 Uiso 1 1 calc R . . H23B H 0.3958 0.3093 0.7036 0.051 Uiso 1 1 calc R . . H23C H 0.3170 0.3613 0.8059 0.051 Uiso 1 1 calc R . . N3 N 0.23351(14) 0.45682(7) 0.42120(14) 0.0180(2) Uani 1 1 d . . . C31 C 0.10199(18) 0.41695(9) 0.46753(17) 0.0208(3) Uani 1 1 d . . . H31D H 0.1535 0.3687 0.5267 0.025 Uiso 1 1 calc R . . C311 C 0.04165(19) 0.47173(10) 0.56734(19) 0.0290(4) Uani 1 1 d . . . H31A H 0.1348 0.4826 0.6583 0.044 Uiso 1 1 calc R . . H31B H -0.0503 0.4458 0.5924 0.044 Uiso 1 1 calc R . . H31C H 0.0016 0.5221 0.5156 0.044 Uiso 1 1 calc R . . C32 C -0.04305(19) 0.38862(10) 0.3336(2) 0.0276(4) Uani 1 1 d . . . H32A H -0.1292 0.3620 0.3678 0.033 Uiso 1 1 calc R . . H32B H -0.0960 0.4352 0.2722 0.033 Uiso 1 1 calc R . . C33 C 0.0206(2) 0.33073(10) 0.2412(2) 0.0328(4) Uani 1 1 d . . . H33A H -0.0707 0.3191 0.1477 0.039 Uiso 1 1 calc R . . H33B H 0.0531 0.2799 0.2960 0.039 Uiso 1 1 calc R . . C34 C 0.1720(2) 0.36495(10) 0.2054(2) 0.0311(4) Uani 1 1 d . . . H34A H 0.1339 0.4086 0.1320 0.037 Uiso 1 1 calc R . . H34B H 0.2224 0.3226 0.1605 0.037 Uiso 1 1 calc R . . C35 C 0.30531(19) 0.39723(9) 0.34459(18) 0.0233(3) Uani 1 1 d . . . H35D H 0.3483 0.3514 0.4139 0.028 Uiso 1 1 calc R . . C351 C 0.4531(2) 0.43273(11) 0.3059(2) 0.0329(4) Uani 1 1 d . . . H35A H 0.5392 0.4507 0.3967 0.049 Uiso 1 1 calc R . . H35B H 0.4141 0.4783 0.2389 0.049 Uiso 1 1 calc R . . H35C H 0.5008 0.3920 0.2571 0.049 Uiso 1 1 calc R . . N41 N 0.13140(15) 0.60279(8) 0.07780(14) 0.0219(3) Uani 1 1 d . . . C411 C 0.2796(2) 0.65055(12) 0.0816(2) 0.0313(4) Uani 1 1 d . . . H41D H 0.3779 0.6155 0.1014 0.047 Uiso 1 1 calc R . . H41E H 0.3003 0.6908 0.1602 0.047 Uiso 1 1 calc R . . H41F H 0.2596 0.6772 -0.0141 0.047 Uiso 1 1 calc R . . C412 C 0.1018(2) 0.54526(11) -0.0438(2) 0.0311(4) Uani 1 1 d . . . H41A H 0.2020 0.5120 -0.0280 0.047 Uiso 1 1 calc R . . H41B H 0.0779 0.5741 -0.1379 0.047 Uiso 1 1 calc R . . H41C H 0.0057 0.5113 -0.0469 0.047 Uiso 1 1 calc R . . C42 C -0.0183(2) 0.65557(10) 0.04512(19) 0.0280(4) Uani 1 1 d . . . H42A H -0.1211 0.6228 0.0050 0.034 Uiso 1 1 calc R . . H42B H -0.0153 0.6946 -0.0321 0.034 Uiso 1 1 calc R . . C43 C -0.0276(2) 0.70025(10) 0.1798(2) 0.0285(4) Uani 1 1 d . . . H43A H 0.0749 0.7332 0.2201 0.034 Uiso 1 1 calc R . . H43B H -0.1256 0.7367 0.1502 0.034 Uiso 1 1 calc R . . N44 N -0.04316(16) 0.64582(8) 0.29647(15) 0.0219(3) Uani 1 1 d . . . C441 C -0.0269(2) 0.69368(10) 0.4303(2) 0.0303(4) Uani 1 1 d . . . H44A H 0.0795 0.7232 0.4585 0.046 Uiso 1 1 calc R . . H44B H -0.0287 0.6582 0.5116 0.046 Uiso 1 1 calc R . . H44C H -0.1208 0.7315 0.4098 0.046 Uiso 1 1 calc R . . C442 C -0.21205(19) 0.60895(11) 0.2505(2) 0.0293(4) Uani 1 1 d . . . H44D H -0.2241 0.5733 0.1661 0.044 Uiso 1 1 calc R . . H44E H -0.2979 0.6509 0.2217 0.044 Uiso 1 1 calc R . . H44F H -0.2261 0.5782 0.3333 0.044 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 Li1 0.0252(13) 0.0202(12) 0.0237(14) 0.0014(11) 0.0081(11) 0.0039(10) Zn1 0.01834(7) 0.01834(7) 0.01685(7) 0.00017(10) 0.00368(5) -0.00139(9) C1 0.0215(7) 0.0207(7) 0.0203(8) 0.0005(6) 0.0033(6) -0.0029(6) C11 0.0443(10) 0.0288(9) 0.0325(11) -0.0056(8) 0.0128(9) -0.0039(8) C12 0.0243(8) 0.0359(9) 0.0300(10) 0.0020(8) 0.0031(7) -0.0097(7) C13 0.0303(8) 0.0243(8) 0.0276(9) 0.0040(7) 0.0039(7) -0.0032(7) C2 0.0192(7) 0.0236(7) 0.0190(8) 0.0021(6) 0.0035(6) -0.0011(6) C21 0.0315(9) 0.0301(9) 0.0320(10) 0.0013(8) 0.0067(8) 0.0070(7) C22 0.0333(8) 0.0336(8) 0.0195(8) 0.0026(7) 0.0061(7) 0.0003(7) C23 0.0326(9) 0.0272(9) 0.0354(11) 0.0123(8) 0.0018(8) -0.0036(7) N3 0.0187(5) 0.0174(5) 0.0172(6) -0.0027(5) 0.0050(5) -0.0010(5) C31 0.0193(7) 0.0190(7) 0.0220(8) 0.0008(6) 0.0037(6) -0.0022(6) C311 0.0256(7) 0.0350(11) 0.0298(9) -0.0021(7) 0.0135(6) -0.0010(6) C32 0.0219(7) 0.0218(8) 0.0335(10) -0.0017(7) 0.0009(7) -0.0033(6) C33 0.0385(10) 0.0213(8) 0.0289(10) -0.0057(7) -0.0028(8) -0.0007(8) C34 0.0428(10) 0.0244(8) 0.0230(9) -0.0065(7) 0.0063(7) 0.0071(7) C35 0.0275(8) 0.0204(7) 0.0212(8) -0.0006(6) 0.0065(6) 0.0054(6) C351 0.0340(8) 0.0383(10) 0.0317(10) -0.0024(8) 0.0178(7) 0.0057(8) N41 0.0224(6) 0.0251(6) 0.0178(7) 0.0018(5) 0.0057(5) 0.0025(5) C411 0.0291(8) 0.0409(10) 0.0236(9) 0.0058(7) 0.0083(7) -0.0047(8) C412 0.0333(9) 0.0355(9) 0.0230(9) -0.0031(8) 0.0068(7) 0.0041(7) C42 0.0290(8) 0.0305(8) 0.0230(9) 0.0075(7) 0.0060(7) 0.0087(7) C43 0.0305(8) 0.0222(8) 0.0318(10) 0.0043(7) 0.0086(7) 0.0063(7) N44 0.0229(6) 0.0211(7) 0.0221(7) -0.0014(5) 0.0080(5) 0.0021(5) C441 0.0317(8) 0.0258(8) 0.0331(10) -0.0080(7) 0.0098(7) 0.0044(7) C442 0.0228(7) 0.0317(9) 0.0319(10) -0.0029(7) 0.0065(7) 0.0008(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Li1 N3 2.027(3) . ? Li1 N44 2.198(3) . ? Li1 N41 2.211(3) . ? Li1 Zn1 3.269(3) . ? Zn1 C1 2.0476(15) . ? Zn1 C2 2.0510(15) . ? Zn1 N3 2.0622(12) . ? C1 C13 1.525(2) . ? C1 C11 1.526(2) . ? C1 C12 1.529(2) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C2 C23 1.524(2) . ? C2 C22 1.530(2) . ? C2 C21 1.535(2) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? N3 C31 1.4742(19) . ? N3 C35 1.4743(19) . ? C31 C311 1.520(2) . ? C31 C32 1.529(2) . ? C31 H31D 1.0000 . ? C311 H31A 0.9800 . ? C311 H31B 0.9800 . ? C311 H31C 0.9800 . ? C32 C33 1.517(3) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C34 1.530(3) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 C35 1.533(2) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 C351 1.524(2) . ? C35 H35D 1.0000 . ? C351 H35A 0.9800 . ? C351 H35B 0.9800 . ? C351 H35C 0.9800 . ? N41 C412 1.465(2) . ? N41 C411 1.470(2) . ? N41 C42 1.485(2) . ? C411 H41D 0.9800 . ? C411 H41E 0.9800 . ? C411 H41F 0.9800 . ? C412 H41A 0.9800 . ? C412 H41B 0.9800 . ? C412 H41C 0.9800 . ? C42 C43 1.509(2) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 N44 1.475(2) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? N44 C441 1.474(2) . ? N44 C442 1.478(2) . ? C441 H44A 0.9800 . ? C441 H44B 0.9800 . ? C441 H44C 0.9800 . ? C442 H44D 0.9800 . ? C442 H44E 0.9800 . ? C442 H44F 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 N3 Li1 N44 133.22(14) . . ? N3 Li1 N41 137.52(14) . . ? N44 Li1 N41 85.62(10) . . ? N3 Li1 Zn1 37.30(6) . . ? N44 Li1 Zn1 121.90(11) . . ? N41 Li1 Zn1 143.22(11) . . ? C1 Zn1 C2 122.61(6) . . ? C1 Zn1 N3 116.19(6) . . ? C2 Zn1 N3 121.06(5) . . ? C1 Zn1 Li1 80.06(6) . . ? C2 Zn1 Li1 157.29(6) . . ? N3 Zn1 Li1 36.54(6) . . ? C13 C1 C11 108.52(14) . . ? C13 C1 C12 106.80(13) . . ? C11 C1 C12 108.64(14) . . ? C13 C1 Zn1 112.61(10) . . ? C11 C1 Zn1 111.88(11) . . ? C12 C1 Zn1 108.19(11) . . ? C1 C11 H11A 109.5 . . ? C1 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C1 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C1 C12 H12A 109.5 . . ? C1 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C1 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C1 C13 H13A 109.5 . . ? C1 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C1 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C23 C2 C22 107.84(14) . . ? C23 C2 C21 108.12(14) . . ? C22 C2 C21 107.13(13) . . ? C23 C2 Zn1 116.62(11) . . ? C22 C2 Zn1 108.98(11) . . ? C21 C2 Zn1 107.78(11) . . ? C2 C21 H21A 109.5 . . ? C2 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C2 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C2 C22 H22A 109.5 . . ? C2 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C2 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C2 C23 H23A 109.5 . . ? C2 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C2 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C31 N3 C35 107.91(12) . . ? C31 N3 Li1 113.18(11) . . ? C35 N3 Li1 113.47(12) . . ? C31 N3 Zn1 107.22(9) . . ? C35 N3 Zn1 108.63(9) . . ? Li1 N3 Zn1 106.16(9) . . ? N3 C31 C311 110.31(12) . . ? N3 C31 C32 111.27(13) . . ? C311 C31 C32 111.88(13) . . ? N3 C31 H31D 107.7 . . ? C311 C31 H31D 107.7 . . ? C32 C31 H31D 107.7 . . ? C31 C311 H31A 109.5 . . ? C31 C311 H31B 109.5 . . ? H31A C311 H31B 109.5 . . ? C31 C311 H31C 109.5 . . ? H31A C311 H31C 109.5 . . ? H31B C311 H31C 109.5 . . ? C33 C32 C31 110.33(13) . . ? C33 C32 H32A 109.6 . . ? C31 C32 H32A 109.6 . . ? C33 C32 H32B 109.6 . . ? C31 C32 H32B 109.6 . . ? H32A C32 H32B 108.1 . . ? C32 C33 C34 111.33(14) . . ? C32 C33 H33A 109.4 . . ? C34 C33 H33A 109.4 . . ? C32 C33 H33B 109.4 . . ? C34 C33 H33B 109.4 . . ? H33A C33 H33B 108.0 . . ? C33 C34 C35 111.53(14) . . ? C33 C34 H34A 109.3 . . ? C35 C34 H34A 109.3 . . ? C33 C34 H34B 109.3 . . ? C35 C34 H34B 109.3 . . ? H34A C34 H34B 108.0 . . ? N3 C35 C351 110.54(13) . . ? N3 C35 C34 111.43(12) . . ? C351 C35 C34 110.66(14) . . ? N3 C35 H35D 108.0 . . ? C351 C35 H35D 108.0 . . ? C34 C35 H35D 108.0 . . ? C35 C351 H35A 109.5 . . ? C35 C351 H35B 109.5 . . ? H35A C351 H35B 109.5 . . ? C35 C351 H35C 109.5 . . ? H35A C351 H35C 109.5 . . ? H35B C351 H35C 109.5 . . ? C412 N41 C411 107.68(13) . . ? C412 N41 C42 107.94(12) . . ? C411 N41 C42 109.59(13) . . ? C412 N41 Li1 118.30(12) . . ? C411 N41 Li1 111.20(12) . . ? C42 N41 Li1 101.79(11) . . ? N41 C411 H41D 109.5 . . ? N41 C411 H41E 109.5 . . ? H41D C411 H41E 109.5 . . ? N41 C411 H41F 109.5 . . ? H41D C411 H41F 109.5 . . ? H41E C411 H41F 109.5 . . ? N41 C412 H41A 109.5 . . ? N41 C412 H41B 109.5 . . ? H41A C412 H41B 109.5 . . ? N41 C412 H41C 109.5 . . ? H41A C412 H41C 109.5 . . ? H41B C412 H41C 109.5 . . ? N41 C42 C43 112.85(13) . . ? N41 C42 H42A 109.0 . . ? C43 C42 H42A 109.0 . . ? N41 C42 H42B 109.0 . . ? C43 C42 H42B 109.0 . . ? H42A C42 H42B 107.8 . . ? N44 C43 C42 112.12(14) . . ? N44 C43 H43A 109.2 . . ? C42 C43 H43A 109.2 . . ? N44 C43 H43B 109.2 . . ? C42 C43 H43B 109.2 . . ? H43A C43 H43B 107.9 . . ? C441 N44 C43 108.10(13) . . ? C441 N44 C442 107.20(13) . . ? C43 N44 C442 110.09(13) . . ? C441 N44 Li1 119.32(12) . . ? C43 N44 Li1 100.64(12) . . ? C442 N44 Li1 111.15(12) . . ? N44 C441 H44A 109.5 . . ? N44 C441 H44B 109.5 . . ? H44A C441 H44B 109.5 . . ? N44 C441 H44C 109.5 . . ? H44A C441 H44C 109.5 . . ? H44B C441 H44C 109.5 . . ? N44 C442 H44D 109.5 . . ? N44 C442 H44E 109.5 . . ? H44D C442 H44E 109.5 . . ? N44 C442 H44F 109.5 . . ? H44D C442 H44F 109.5 . . ? H44E C442 H44F 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 N3 Li1 Zn1 C1 171.51(10) . . . . ? N44 Li1 Zn1 C1 -67.56(12) . . . . ? N41 Li1 Zn1 C1 65.45(18) . . . . ? N3 Li1 Zn1 C2 -11.6(2) . . . . ? N44 Li1 Zn1 C2 109.35(17) . . . . ? N41 Li1 Zn1 C2 -117.6(2) . . . . ? N44 Li1 Zn1 N3 120.93(17) . . . . ? N41 Li1 Zn1 N3 -106.1(2) . . . . ? C2 Zn1 C1 C13 165.54(10) . . . . ? N3 Zn1 C1 C13 -10.26(13) . . . . ? Li1 Zn1 C1 C13 -15.88(11) . . . . ? C2 Zn1 C1 C11 -71.92(13) . . . . ? N3 Zn1 C1 C11 112.29(12) . . . . ? Li1 Zn1 C1 C11 106.67(12) . . . . ? C2 Zn1 C1 C12 47.73(14) . . . . ? N3 Zn1 C1 C12 -128.06(11) . . . . ? Li1 Zn1 C1 C12 -133.69(12) . . . . ? C1 Zn1 C2 C23 156.90(12) . . . . ? N3 Zn1 C2 C23 -27.51(15) . . . . ? Li1 Zn1 C2 C23 -19.5(2) . . . . ? C1 Zn1 C2 C22 34.57(13) . . . . ? N3 Zn1 C2 C22 -149.83(9) . . . . ? Li1 Zn1 C2 C22 -141.81(15) . . . . ? C1 Zn1 C2 C21 -81.36(13) . . . . ? N3 Zn1 C2 C21 94.23(11) . . . . ? Li1 Zn1 C2 C21 102.26(18) . . . . ? N44 Li1 N3 C31 29.5(2) . . . . ? N41 Li1 N3 C31 -121.09(19) . . . . ? Zn1 Li1 N3 C31 117.35(12) . . . . ? N44 Li1 N3 C35 152.88(16) . . . . ? N41 Li1 N3 C35 2.3(2) . . . . ? Zn1 Li1 N3 C35 -119.24(12) . . . . ? N44 Li1 N3 Zn1 -87.88(18) . . . . ? N41 Li1 N3 Zn1 121.57(18) . . . . ? C1 Zn1 N3 C31 -130.58(9) . . . . ? C2 Zn1 N3 C31 53.56(11) . . . . ? Li1 Zn1 N3 C31 -121.25(13) . . . . ? C1 Zn1 N3 C35 113.04(10) . . . . ? C2 Zn1 N3 C35 -62.82(11) . . . . ? Li1 Zn1 N3 C35 122.37(14) . . . . ? C1 Zn1 N3 Li1 -9.33(11) . . . . ? C2 Zn1 N3 Li1 174.81(9) . . . . ? C35 N3 C31 C311 171.41(13) . . . . ? Li1 N3 C31 C311 -62.16(16) . . . . ? Zn1 N3 C31 C311 54.56(13) . . . . ? C35 N3 C31 C32 -63.79(15) . . . . ? Li1 N3 C31 C32 62.63(16) . . . . ? Zn1 N3 C31 C32 179.35(10) . . . . ? N3 C31 C32 C33 59.10(17) . . . . ? C311 C31 C32 C33 -176.99(14) . . . . ? C31 C32 C33 C34 -50.77(19) . . . . ? C32 C33 C34 C35 49.31(19) . . . . ? C31 N3 C35 C351 -174.94(13) . . . . ? Li1 N3 C35 C351 58.81(16) . . . . ? Zn1 N3 C35 C351 -59.01(14) . . . . ? C31 N3 C35 C34 61.56(16) . . . . ? Li1 N3 C35 C34 -64.69(16) . . . . ? Zn1 N3 C35 C34 177.49(11) . . . . ? C33 C34 C35 N3 -55.27(18) . . . . ? C33 C34 C35 C351 -178.70(13) . . . . ? N3 Li1 N41 C412 31.8(3) . . . . ? N44 Li1 N41 C412 -127.10(12) . . . . ? Zn1 Li1 N41 C412 91.4(2) . . . . ? N3 Li1 N41 C411 -93.5(2) . . . . ? N44 Li1 N41 C411 107.55(12) . . . . ? Zn1 Li1 N41 C411 -33.9(2) . . . . ? N3 Li1 N41 C42 149.86(19) . . . . ? N44 Li1 N41 C42 -9.09(12) . . . . ? Zn1 Li1 N41 C42 -150.58(17) . . . . ? C412 N41 C42 C43 162.64(14) . . . . ? C411 N41 C42 C43 -80.36(17) . . . . ? Li1 N41 C42 C43 37.44(16) . . . . ? N41 C42 C43 N44 -62.27(18) . . . . ? C42 C43 N44 C441 172.02(13) . . . . ? C42 C43 N44 C442 -71.19(16) . . . . ? C42 C43 N44 Li1 46.18(15) . . . . ? N3 Li1 N44 C441 62.3(2) . . . . ? N41 Li1 N44 C441 -137.19(13) . . . . ? Zn1 Li1 N44 C441 16.76(19) . . . . ? N3 Li1 N44 C43 -179.84(18) . . . . ? N41 Li1 N44 C43 -19.29(12) . . . . ? Zn1 Li1 N44 C43 134.66(12) . . . . ? N3 Li1 N44 C442 -63.3(2) . . . . ? N41 Li1 N44 C442 97.29(13) . . . . ? Zn1 Li1 N44 C442 -108.76(14) . . . . ? _diffrn_measured_fraction_theta_max 0.933 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.433 _refine_diff_density_min -0.195 _refine_diff_density_rms 0.041 #===END #------------------------------------------------------- #------------------COMPOUND 2-------------------------- #----------------------------------------------------- data_coh0409 _database_code_depnum_ccdc_archive 'CCDC 734662' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H48 N3 Na Zn' _chemical_formula_weight 430.98 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Zn Zn -1.5491 0.6778 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Na Na 0.1353 0.1239 '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' 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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' _cell_length_a 8.3370(4) _cell_length_b 9.6409(5) _cell_length_c 9.7024(4) _cell_angle_alpha 61.815(4) _cell_angle_beta 78.623(4) _cell_angle_gamma 73.435(5) _cell_volume 657.03(5) _cell_formula_units_Z 1 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 6995 _cell_measurement_theta_min 3.31 _cell_measurement_theta_max 71.66 _exptl_crystal_description lump _exptl_crystal_colour colourless _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.33 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.089 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 236 _exptl_absorpt_coefficient_mu 1.502 _exptl_absorpt_correction_T_min 0.864 _exptl_absorpt_correction_T_max 0.948 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET) (compiled Jun 10 2008,16:49:55) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 1.54180 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Gemini S' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6022 _diffrn_reflns_av_R_equivalents 0.0418 _diffrn_reflns_av_sigmaI/netI 0.0229 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 5.34 _diffrn_reflns_theta_max 71.69 _reflns_number_total 3312 _reflns_number_gt 3302 _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 ; Note use of 3 restraint equivalents to "fix" origin in P1. 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^)+(0.1642P)^2^+0.2479P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.15(5) _chemical_absolute_configuration ad _refine_ls_number_reflns 3312 _refine_ls_number_parameters 248 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0658 _refine_ls_R_factor_gt 0.0658 _refine_ls_wR_factor_ref 0.1841 _refine_ls_wR_factor_gt 0.1841 _refine_ls_goodness_of_fit_ref 1.061 _refine_ls_restrained_S_all 1.060 _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 Zn1 Zn 0.1766(2) 0.4733(2) 0.1227(2) 0.0290(2) Uani 1 1 d . . . Na1 Na -0.0732(3) 0.8568(3) -0.0138(3) 0.0323(5) Uani 1 1 d . . . N1 N -0.2892(7) 0.9774(7) -0.2016(6) 0.0372(11) Uani 1 1 d . . . N2 N -0.0995(7) 1.1494(6) -0.1191(6) 0.0352(10) Uani 1 1 d . . . N3 N 0.0052(6) 0.6157(6) 0.2105(5) 0.0279(9) Uani 1 1 d . . . C1 C -0.4541(9) 0.9659(10) -0.1171(10) 0.0507(16) Uani 1 1 d . . . H1A H -0.4702 1.0110 -0.0423 0.076 Uiso 1 1 calc R . . H1B H -0.4615 0.8524 -0.0604 0.076 Uiso 1 1 calc R . . H1C H -0.5412 1.0265 -0.1918 0.076 Uiso 1 1 calc R . . C2 C -0.2676(10) 0.8973(12) -0.3048(10) 0.057(2) Uani 1 1 d . . . H2A H -0.2569 0.7809 -0.2403 0.085 Uiso 1 1 calc R . . H2B H -0.1663 0.9169 -0.3755 0.085 Uiso 1 1 calc R . . H2C H -0.3655 0.9412 -0.3666 0.085 Uiso 1 1 calc R . . C3 C -0.2707(10) 1.1432(9) -0.3002(8) 0.0480(16) Uani 1 1 d . . . H3A H -0.3703 1.2059 -0.3617 0.058 Uiso 1 1 calc R . . H3B H -0.1710 1.1430 -0.3750 0.058 Uiso 1 1 calc R . . C4 C -0.2516(10) 1.2255(8) -0.2065(9) 0.0463(15) Uani 1 1 d . . . H4A H -0.2489 1.3395 -0.2789 0.056 Uiso 1 1 calc R . . H4B H -0.3511 1.2250 -0.1314 0.056 Uiso 1 1 calc R . . C5 C -0.1193(10) 1.2154(9) -0.0070(8) 0.0480(15) Uani 1 1 d . . . H5A H -0.0198 1.1679 0.0532 0.072 Uiso 1 1 calc R . . H5B H -0.2189 1.1898 0.0646 0.072 Uiso 1 1 calc R . . H5C H -0.1325 1.3328 -0.0637 0.072 Uiso 1 1 calc R . . C6 C 0.0496(10) 1.1843(9) -0.2235(10) 0.0502(16) Uani 1 1 d . . . H6A H 0.0337 1.3011 -0.2887 0.075 Uiso 1 1 calc R . . H6B H 0.0693 1.1300 -0.2909 0.075 Uiso 1 1 calc R . . H6C H 0.1464 1.1456 -0.1615 0.075 Uiso 1 1 calc R . . C7 C -0.1432(8) 0.5500(7) 0.2907(7) 0.0336(11) Uani 1 1 d . . . H7 H -0.1086 0.4487 0.3876 0.040 Uiso 1 1 calc R . . C8 C -0.2789(8) 0.6670(10) 0.3385(9) 0.0449(15) Uani 1 1 d . . . H8A H -0.3746 0.6158 0.3961 0.054 Uiso 1 1 calc R . . H8B H -0.3201 0.7650 0.2433 0.054 Uiso 1 1 calc R . . C9 C -0.2120(10) 0.7148(9) 0.4424(9) 0.0470(15) Uani 1 1 d . . . H9A H -0.2967 0.8026 0.4584 0.056 Uiso 1 1 calc R . . H9B H -0.1911 0.6212 0.5461 0.056 Uiso 1 1 calc R . . C10 C -0.0510(9) 0.7708(9) 0.3661(8) 0.0421(14) Uani 1 1 d . . . H10A H -0.0003 0.7859 0.4408 0.051 Uiso 1 1 calc R . . H10B H -0.0765 0.8763 0.2730 0.051 Uiso 1 1 calc R . . C11 C 0.0763(8) 0.6482(8) 0.3155(7) 0.0360(12) Uani 1 1 d . . . H11 H 0.1052 0.5445 0.4119 0.043 Uiso 1 1 calc R . . C12 C -0.2129(9) 0.5075(9) 0.1841(9) 0.0451(15) Uani 1 1 d . . . H12A H -0.2452 0.6051 0.0874 0.068 Uiso 1 1 calc R . . H12B H -0.3113 0.4620 0.2384 0.068 Uiso 1 1 calc R . . H12C H -0.1266 0.4281 0.1585 0.068 Uiso 1 1 calc R . . C13 C 0.2356(9) 0.7070(10) 0.2402(9) 0.0484(16) Uani 1 1 d . . . H13A H 0.3190 0.6232 0.2188 0.073 Uiso 1 1 calc R . . H13B H 0.2794 0.7311 0.3111 0.073 Uiso 1 1 calc R . . H13C H 0.2118 0.8049 0.1416 0.073 Uiso 1 1 calc R . . C14 C 0.2731(7) 0.5796(7) -0.1045(6) 0.0304(11) Uani 1 1 d . . . C15 C 0.2075(10) 0.7617(8) -0.1953(8) 0.0467(15) Uani 1 1 d . . . H15A H 0.2140 0.8150 -0.1326 0.070 Uiso 1 1 calc R . . H15B H 0.0905 0.7837 -0.2168 0.070 Uiso 1 1 calc R . . H15C H 0.2758 0.8030 -0.2944 0.070 Uiso 1 1 calc R . . C16 C 0.4634(8) 0.5533(9) -0.1025(9) 0.0448(14) Uani 1 1 d . . . H16A H 0.5152 0.5868 -0.2098 0.067 Uiso 1 1 calc R . . H16B H 0.5108 0.4388 -0.0387 0.067 Uiso 1 1 calc R . . H16C H 0.4855 0.6176 -0.0576 0.067 Uiso 1 1 calc R . . C17 C 0.2469(12) 0.4993(12) -0.2009(9) 0.0565(19) Uani 1 1 d . . . H17A H 0.3054 0.5440 -0.3052 0.085 Uiso 1 1 calc R . . H17B H 0.1268 0.5202 -0.2115 0.085 Uiso 1 1 calc R . . H17C H 0.2920 0.3826 -0.1473 0.085 Uiso 1 1 calc R . . C18 C 0.2571(9) 0.2332(7) 0.2740(7) 0.0410(14) Uani 1 1 d . . . C19 C 0.1139(12) 0.1494(10) 0.3674(9) 0.0531(17) Uani 1 1 d . . . H19A H 0.1601 0.0348 0.4322 0.080 Uiso 1 1 calc R . . H19B H 0.0393 0.1599 0.2949 0.080 Uiso 1 1 calc R . . H19C H 0.0505 0.1996 0.4349 0.080 Uiso 1 1 calc R . . C20 C 0.3581(15) 0.2264(12) 0.3942(14) 0.083(4) Uani 1 1 d . . . H20A H 0.2894 0.2931 0.4448 0.125 Uiso 1 1 calc R . . H20B H 0.4595 0.2671 0.3409 0.125 Uiso 1 1 calc R . . H20C H 0.3900 0.1145 0.4737 0.125 Uiso 1 1 calc R . . C21 C 0.3579(13) 0.1320(10) 0.1856(11) 0.059(2) Uani 1 1 d . . . H21A H 0.4213 0.0289 0.2599 0.089 Uiso 1 1 calc R . . H21B H 0.4358 0.1918 0.1040 0.089 Uiso 1 1 calc R . . H21C H 0.2799 0.1116 0.1373 0.089 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 Zn1 0.0283(3) 0.0281(3) 0.0258(3) -0.0117(2) 0.0017(2) -0.0023(2) Na1 0.0302(11) 0.0330(11) 0.0317(11) -0.0138(9) -0.0038(9) -0.0039(9) N1 0.030(2) 0.045(3) 0.043(3) -0.024(2) -0.007(2) -0.007(2) N2 0.035(3) 0.037(2) 0.038(2) -0.021(2) -0.002(2) -0.007(2) N3 0.026(2) 0.032(2) 0.030(2) -0.0204(18) 0.0024(18) -0.0041(18) C1 0.033(3) 0.059(4) 0.065(4) -0.036(4) 0.007(3) -0.009(3) C2 0.042(4) 0.087(6) 0.058(4) -0.048(4) -0.011(3) -0.004(4) C3 0.046(4) 0.053(4) 0.042(3) -0.015(3) -0.012(3) -0.010(3) C4 0.053(4) 0.035(3) 0.050(3) -0.014(3) -0.014(3) -0.009(3) C5 0.056(4) 0.048(4) 0.045(3) -0.027(3) -0.010(3) -0.004(3) C6 0.045(4) 0.047(4) 0.061(4) -0.030(3) 0.012(3) -0.014(3) C7 0.030(3) 0.035(3) 0.034(3) -0.018(2) 0.007(2) -0.007(2) C8 0.029(3) 0.060(4) 0.051(4) -0.034(3) 0.013(3) -0.010(3) C9 0.049(4) 0.050(4) 0.046(3) -0.033(3) 0.011(3) -0.006(3) C10 0.048(4) 0.045(3) 0.041(3) -0.029(3) 0.003(3) -0.010(3) C11 0.036(3) 0.041(3) 0.036(3) -0.021(2) -0.002(2) -0.009(2) C12 0.035(3) 0.055(4) 0.059(4) -0.039(3) 0.004(3) -0.009(3) C13 0.039(3) 0.065(4) 0.055(4) -0.036(3) 0.001(3) -0.019(3) C14 0.028(3) 0.035(3) 0.026(2) -0.015(2) 0.011(2) -0.010(2) C15 0.044(4) 0.041(3) 0.034(3) -0.010(3) 0.005(3) 0.004(3) C16 0.032(3) 0.046(3) 0.053(4) -0.024(3) 0.013(3) -0.010(3) C17 0.067(5) 0.074(5) 0.046(4) -0.037(4) 0.010(3) -0.032(4) C18 0.047(4) 0.030(3) 0.028(3) -0.007(2) 0.006(3) 0.001(2) C19 0.060(5) 0.043(4) 0.041(4) -0.011(3) 0.000(3) -0.009(3) C20 0.085(7) 0.055(5) 0.091(7) 0.002(4) -0.065(6) -0.012(5) C21 0.063(5) 0.038(3) 0.057(5) -0.013(3) 0.012(4) -0.007(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 Zn1 N3 2.039(5) . ? Zn1 C14 2.048(5) . ? Zn1 C18 2.063(6) . ? Zn1 Na1 3.440(2) . ? Na1 N3 2.342(5) . ? Na1 N1 2.452(5) . ? Na1 N2 2.462(6) . ? N1 C1 1.459(9) . ? N1 C3 1.460(9) . ? N1 C2 1.488(8) . ? N2 C6 1.451(9) . ? N2 C5 1.462(8) . ? N2 C4 1.473(9) . ? N3 C11 1.461(6) . ? N3 C7 1.462(7) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 C4 1.514(10) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? 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 1.525(9) . ? C7 C12 1.533(8) . ? C7 H7 1.0000 . ? C8 C9 1.531(9) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.512(10) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C11 1.546(9) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C13 1.508(9) . ? C11 H11 1.0000 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 C15 1.529(8) . ? C14 C16 1.536(8) . ? C14 C17 1.544(8) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C19 1.527(11) . ? C18 C20 1.535(10) . ? C18 C21 1.560(11) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 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 N3 Zn1 C14 118.4(2) . . ? N3 Zn1 C18 117.8(2) . . ? C14 Zn1 C18 123.7(2) . . ? N3 Zn1 Na1 41.49(14) . . ? C14 Zn1 Na1 77.90(17) . . ? C18 Zn1 Na1 158.10(19) . . ? N3 Na1 N1 137.69(19) . . ? N3 Na1 N2 140.64(18) . . ? N1 Na1 N2 75.93(18) . . ? N3 Na1 Zn1 35.24(12) . . ? N1 Na1 Zn1 127.90(15) . . ? N2 Na1 Zn1 149.02(15) . . ? C1 N1 C3 113.6(6) . . ? C1 N1 C2 106.9(5) . . ? C3 N1 C2 108.0(6) . . ? C1 N1 Na1 109.6(4) . . ? C3 N1 Na1 105.2(3) . . ? C2 N1 Na1 113.7(4) . . ? C6 N2 C5 109.7(6) . . ? C6 N2 C4 111.1(6) . . ? C5 N2 C4 107.1(6) . . ? C6 N2 Na1 105.8(4) . . ? C5 N2 Na1 117.8(4) . . ? C4 N2 Na1 105.3(4) . . ? C11 N3 C7 109.2(4) . . ? C11 N3 Zn1 112.8(4) . . ? C7 N3 Zn1 112.9(3) . . ? C11 N3 Na1 109.3(3) . . ? C7 N3 Na1 109.1(3) . . ? Zn1 N3 Na1 103.3(2) . . ? N1 C1 H1A 109.5 . . ? N1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? N1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N1 C2 H2A 109.5 . . ? N1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? N1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? N1 C3 C4 112.8(6) . . ? N1 C3 H3A 109.0 . . ? C4 C3 H3A 109.0 . . ? N1 C3 H3B 109.0 . . ? C4 C3 H3B 109.0 . . ? H3A C3 H3B 107.8 . . ? N2 C4 C3 113.8(6) . . ? N2 C4 H4A 108.8 . . ? C3 C4 H4A 108.8 . . ? N2 C4 H4B 108.8 . . ? C3 C4 H4B 108.8 . . ? H4A C4 H4B 107.7 . . ? N2 C5 H5A 109.5 . . ? N2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? N2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N2 C6 H6A 109.5 . . ? N2 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? N2 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? N3 C7 C8 112.2(5) . . ? N3 C7 C12 109.4(5) . . ? C8 C7 C12 110.1(5) . . ? N3 C7 H7 108.4 . . ? C8 C7 H7 108.4 . . ? C12 C7 H7 108.4 . . ? C7 C8 C9 111.4(6) . . ? C7 C8 H8A 109.4 . . ? C9 C8 H8A 109.4 . . ? C7 C8 H8B 109.4 . . ? C9 C8 H8B 109.4 . . ? H8A C8 H8B 108.0 . . ? C10 C9 C8 110.1(5) . . ? C10 C9 H9A 109.6 . . ? C8 C9 H9A 109.6 . . ? C10 C9 H9B 109.6 . . ? C8 C9 H9B 109.6 . . ? H9A C9 H9B 108.2 . . ? C9 C10 C11 111.7(5) . . ? C9 C10 H10A 109.3 . . ? C11 C10 H10A 109.3 . . ? C9 C10 H10B 109.3 . . ? C11 C10 H10B 109.3 . . ? H10A C10 H10B 107.9 . . ? N3 C11 C13 110.8(5) . . ? N3 C11 C10 111.6(5) . . ? C13 C11 C10 110.5(5) . . ? N3 C11 H11 107.9 . . ? C13 C11 H11 107.9 . . ? C10 C11 H11 107.9 . . ? C7 C12 H12A 109.5 . . ? C7 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C7 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C15 C14 C16 106.1(5) . . ? C15 C14 C17 107.7(6) . . ? C16 C14 C17 107.0(6) . . ? C15 C14 Zn1 116.3(4) . . ? C16 C14 Zn1 107.9(4) . . ? C17 C14 Zn1 111.4(4) . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C14 C16 H16A 109.5 . . ? C14 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C14 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C14 C17 H17A 109.5 . . ? C14 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C14 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C19 C18 C20 106.5(7) . . ? C19 C18 C21 104.3(6) . . ? C20 C18 C21 113.1(8) . . ? C19 C18 Zn1 113.5(5) . . ? C20 C18 Zn1 107.3(5) . . ? C21 C18 Zn1 112.1(4) . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C18 C20 H20A 109.5 . . ? C18 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C18 C21 H21A 109.5 . . ? C18 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C18 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 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 C14 Zn1 Na1 N3 -167.4(2) . . . . ? C18 Zn1 Na1 N3 22.0(6) . . . . ? N3 Zn1 Na1 N1 -121.5(3) . . . . ? C14 Zn1 Na1 N1 71.1(2) . . . . ? C18 Zn1 Na1 N1 -99.4(6) . . . . ? N3 Zn1 Na1 N2 104.2(3) . . . . ? C14 Zn1 Na1 N2 -63.2(3) . . . . ? C18 Zn1 Na1 N2 126.3(6) . . . . ? N3 Na1 N1 C1 50.3(5) . . . . ? N2 Na1 N1 C1 -105.1(4) . . . . ? Zn1 Na1 N1 C1 97.2(4) . . . . ? N3 Na1 N1 C3 172.7(4) . . . . ? N2 Na1 N1 C3 17.4(4) . . . . ? Zn1 Na1 N1 C3 -140.3(4) . . . . ? N3 Na1 N1 C2 -69.3(6) . . . . ? N2 Na1 N1 C2 135.3(5) . . . . ? Zn1 Na1 N1 C2 -22.3(6) . . . . ? N3 Na1 N2 C6 100.0(5) . . . . ? N1 Na1 N2 C6 -106.3(4) . . . . ? Zn1 Na1 N2 C6 38.1(5) . . . . ? N3 Na1 N2 C5 -23.0(6) . . . . ? N1 Na1 N2 C5 130.8(5) . . . . ? Zn1 Na1 N2 C5 -84.9(6) . . . . ? N3 Na1 N2 C4 -142.2(5) . . . . ? N1 Na1 N2 C4 11.5(4) . . . . ? Zn1 Na1 N2 C4 155.9(4) . . . . ? C14 Zn1 N3 C11 -103.8(4) . . . . ? C18 Zn1 N3 C11 71.2(5) . . . . ? Na1 Zn1 N3 C11 -117.9(4) . . . . ? C14 Zn1 N3 C7 131.7(4) . . . . ? C18 Zn1 N3 C7 -53.2(4) . . . . ? Na1 Zn1 N3 C7 117.7(4) . . . . ? C14 Zn1 N3 Na1 14.0(3) . . . . ? C18 Zn1 N3 Na1 -170.9(3) . . . . ? N1 Na1 N3 C11 -148.2(4) . . . . ? N2 Na1 N3 C11 -7.8(5) . . . . ? Zn1 Na1 N3 C11 120.3(4) . . . . ? N1 Na1 N3 C7 -28.8(5) . . . . ? N2 Na1 N3 C7 111.6(4) . . . . ? Zn1 Na1 N3 C7 -120.3(4) . . . . ? N1 Na1 N3 Zn1 91.5(3) . . . . ? N2 Na1 N3 Zn1 -128.1(3) . . . . ? C1 N1 C3 C4 74.4(7) . . . . ? C2 N1 C3 C4 -167.2(6) . . . . ? Na1 N1 C3 C4 -45.5(7) . . . . ? C6 N2 C4 C3 73.8(7) . . . . ? C5 N2 C4 C3 -166.4(6) . . . . ? Na1 N2 C4 C3 -40.3(7) . . . . ? N1 C3 C4 N2 63.1(9) . . . . ? C11 N3 C7 C8 60.5(7) . . . . ? Zn1 N3 C7 C8 -173.2(4) . . . . ? Na1 N3 C7 C8 -59.0(5) . . . . ? C11 N3 C7 C12 -177.1(5) . . . . ? Zn1 N3 C7 C12 -50.7(6) . . . . ? Na1 N3 C7 C12 63.5(5) . . . . ? N3 C7 C8 C9 -56.7(8) . . . . ? C12 C7 C8 C9 -178.8(6) . . . . ? C7 C8 C9 C10 50.9(8) . . . . ? C8 C9 C10 C11 -50.7(8) . . . . ? C7 N3 C11 C13 176.7(6) . . . . ? Zn1 N3 C11 C13 50.3(6) . . . . ? Na1 N3 C11 C13 -64.0(6) . . . . ? C7 N3 C11 C10 -59.7(6) . . . . ? Zn1 N3 C11 C10 173.9(4) . . . . ? Na1 N3 C11 C10 59.6(5) . . . . ? C9 C10 C11 N3 56.3(7) . . . . ? C9 C10 C11 C13 -179.9(6) . . . . ? N3 Zn1 C14 C15 -0.7(5) . . . . ? C18 Zn1 C14 C15 -175.4(5) . . . . ? Na1 Zn1 C14 C15 8.8(4) . . . . ? N3 Zn1 C14 C16 118.3(4) . . . . ? C18 Zn1 C14 C16 -56.4(5) . . . . ? Na1 Zn1 C14 C16 127.8(4) . . . . ? N3 Zn1 C14 C17 -124.6(5) . . . . ? C18 Zn1 C14 C17 60.7(6) . . . . ? Na1 Zn1 C14 C17 -115.1(5) . . . . ? N3 Zn1 C18 C19 50.3(6) . . . . ? C14 Zn1 C18 C19 -134.9(5) . . . . ? Na1 Zn1 C18 C19 34.0(9) . . . . ? N3 Zn1 C18 C20 -67.1(7) . . . . ? C14 Zn1 C18 C20 107.7(7) . . . . ? Na1 Zn1 C18 C20 -83.4(9) . . . . ? N3 Zn1 C18 C21 168.2(5) . . . . ? C14 Zn1 C18 C21 -17.0(7) . . . . ? Na1 Zn1 C18 C21 151.9(5) . . . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 65.00 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.021 _refine_diff_density_min -1.187 _refine_diff_density_rms 0.115 #===END #------------------------------------------------------- #------------------COMPOUND 4-------------------------- #----------------------------------------------------- data_pgaross6 _database_code_depnum_ccdc_archive 'CCDC 734663' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H61 N4 Na Zn' _chemical_formula_weight 518.15 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Zn Zn -1.5491 0.6778 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Na Na 0.1353 0.1239 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0181 0.0091 '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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting MONOCLINIC _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.7987(1) _cell_length_b 19.5516(2) _cell_length_c 16.5289(2) _cell_angle_alpha 90.00 _cell_angle_beta 91.279(1) _cell_angle_gamma 90.00 _cell_volume 3165.82(6) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 11572 _cell_measurement_theta_min 3.5035 _cell_measurement_theta_max 68.9839 _exptl_crystal_description fragment _exptl_crystal_colour colourless _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.087 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1144 _exptl_absorpt_coefficient_mu 1.327 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.47280 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET) (compiled Jun 10 2008,16:49:55) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 1.54180 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Gemini S' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19219 _diffrn_reflns_av_R_equivalents 0.0187 _diffrn_reflns_av_sigmaI/netI 0.0297 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.50 _diffrn_reflns_theta_max 69.26 _reflns_number_total 5797 _reflns_number_gt 4569 _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^)+(0.0490P)^2^+0.0000P] 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 5797 _refine_ls_number_parameters 304 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0433 _refine_ls_R_factor_gt 0.0304 _refine_ls_wR_factor_ref 0.0791 _refine_ls_wR_factor_gt 0.0764 _refine_ls_goodness_of_fit_ref 1.002 _refine_ls_restrained_S_all 1.002 _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 Zn1 Zn -0.05566(2) 0.111216(11) 0.260411(13) 0.02228(8) Uani 1 1 d . . . Na1 Na 0.12538(6) 0.24134(3) 0.28959(4) 0.02548(16) Uani 1 1 d . . . N1 N 0.00171(14) 0.18312(7) 0.17954(8) 0.0229(3) Uani 1 1 d . . . N2 N 0.02918(14) 0.14469(7) 0.36300(8) 0.0231(3) Uani 1 1 d . . . N3 N 0.37899(15) 0.27098(8) 0.28557(9) 0.0307(3) Uani 1 1 d . . . N4 N 0.16564(15) 0.34809(7) 0.38008(9) 0.0317(4) Uani 1 1 d . . . C1 C 0.03780(18) 0.15735(9) 0.09992(10) 0.0269(4) Uani 1 1 d . . . H1A H 0.0780 0.1952 0.0686 0.032 Uiso 1 1 calc R . . H1B H -0.0467 0.1427 0.0709 0.032 Uiso 1 1 calc R . . C2 C 0.13754(19) 0.09799(9) 0.10187(11) 0.0306(4) Uani 1 1 d . . . H2 H 0.0980 0.0610 0.1359 0.037 Uiso 1 1 calc R . . C3 C 0.2746(2) 0.11774(11) 0.13891(13) 0.0445(5) Uani 1 1 d . . . H3A H 0.3173 0.1526 0.1052 0.067 Uiso 1 1 calc R . . H3C H 0.3336 0.0773 0.1421 0.067 Uiso 1 1 calc R . . H3B H 0.2617 0.1361 0.1934 0.067 Uiso 1 1 calc R . . C4 C 0.1555(2) 0.06952(10) 0.01668(11) 0.0395(5) Uani 1 1 d . . . H4A H 0.1920 0.1053 -0.0182 0.059 Uiso 1 1 calc R . . H4C H 0.0670 0.0542 -0.0053 0.059 Uiso 1 1 calc R . . H4B H 0.2190 0.0308 0.0189 0.059 Uiso 1 1 calc R . . C5 C -0.12035(17) 0.22675(9) 0.17097(10) 0.0253(4) Uani 1 1 d . . . H5A H -0.1516 0.2379 0.2260 0.030 Uiso 1 1 calc R . . H5B H -0.1933 0.1994 0.1442 0.030 Uiso 1 1 calc R . . C6 C -0.10692(17) 0.29397(9) 0.12404(10) 0.0258(4) Uani 1 1 d . . . H6 H -0.0836 0.2828 0.0669 0.031 Uiso 1 1 calc R . . C7 C 0.00569(19) 0.33879(9) 0.15986(11) 0.0331(4) Uani 1 1 d . . . H7A H 0.0097 0.3818 0.1296 0.050 Uiso 1 1 calc R . . H7B H 0.0934 0.3150 0.1564 0.050 Uiso 1 1 calc R . . H7C H -0.0133 0.3485 0.2167 0.050 Uiso 1 1 calc R . . C8 C -0.24297(19) 0.33139(10) 0.12316(12) 0.0361(5) Uani 1 1 d . . . H8A H -0.2671 0.3431 0.1787 0.054 Uiso 1 1 calc R . . H8C H -0.3138 0.3019 0.0991 0.054 Uiso 1 1 calc R . . H8B H -0.2357 0.3733 0.0911 0.054 Uiso 1 1 calc R . . C9 C -0.05785(17) 0.14143(9) 0.43303(10) 0.0272(4) Uani 1 1 d . . . H9A H -0.0101 0.1631 0.4798 0.033 Uiso 1 1 calc R . . H9B H -0.0743 0.0929 0.4469 0.033 Uiso 1 1 calc R . . C10 C -0.19492(17) 0.17716(9) 0.41818(10) 0.0284(4) Uani 1 1 d . . . H10 H -0.2323 0.1615 0.3645 0.034 Uiso 1 1 calc R . . C11 C -0.1810(2) 0.25468(10) 0.41490(12) 0.0378(5) Uani 1 1 d . . . H11B H -0.1539 0.2720 0.4686 0.057 Uiso 1 1 calc R . . H11C H -0.2686 0.2749 0.3982 0.057 Uiso 1 1 calc R . . H11A H -0.1113 0.2670 0.3758 0.057 Uiso 1 1 calc R . . C12 C -0.2968(2) 0.15695(12) 0.48248(12) 0.0435(5) Uani 1 1 d . . . H12C H -0.3139 0.1076 0.4795 0.065 Uiso 1 1 calc R . . H12B H -0.3826 0.1818 0.4731 0.065 Uiso 1 1 calc R . . H12A H -0.2592 0.1685 0.5362 0.065 Uiso 1 1 calc R . . C13 C 0.16944(17) 0.12558(9) 0.38467(10) 0.0260(4) Uani 1 1 d . . . H13A H 0.2042 0.1595 0.4245 0.031 Uiso 1 1 calc R . . H13B H 0.2245 0.1308 0.3355 0.031 Uiso 1 1 calc R . . C14 C 0.19915(19) 0.05435(9) 0.41950(11) 0.0325(4) Uani 1 1 d . . . H14 H 0.1533 0.0509 0.4728 0.039 Uiso 1 1 calc R . . C15 C 0.1432(2) -0.00191(10) 0.36559(14) 0.0535(6) Uani 1 1 d . . . H15C H 0.0438 0.0027 0.3602 0.080 Uiso 1 1 calc R . . H15B H 0.1658 -0.0465 0.3895 0.080 Uiso 1 1 calc R . . H15A H 0.1836 0.0015 0.3121 0.080 Uiso 1 1 calc R . . C16 C 0.3525(2) 0.04668(11) 0.43499(13) 0.0440(5) Uani 1 1 d . . . H16B H 0.3709 0.0031 0.4625 0.066 Uiso 1 1 calc R . . H16C H 0.3855 0.0845 0.4691 0.066 Uiso 1 1 calc R . . H16A H 0.3996 0.0475 0.3833 0.066 Uiso 1 1 calc R . . C17 C 0.47956(19) 0.21533(11) 0.29051(13) 0.0424(5) Uani 1 1 d . . . H17C H 0.5715 0.2342 0.2849 0.064 Uiso 1 1 calc R . . H17A H 0.4611 0.1824 0.2470 0.064 Uiso 1 1 calc R . . H17B H 0.4732 0.1923 0.3430 0.064 Uiso 1 1 calc R . . C18 C 0.3905(2) 0.30508(11) 0.20651(12) 0.0424(5) Uani 1 1 d . . . H18B H 0.3253 0.3431 0.2030 0.064 Uiso 1 1 calc R . . H18A H 0.3703 0.2722 0.1632 0.064 Uiso 1 1 calc R . . H18C H 0.4834 0.3227 0.2008 0.064 Uiso 1 1 calc R . . C19 C 0.40867(19) 0.31956(10) 0.35152(12) 0.0372(5) Uani 1 1 d . . . H19A H 0.4976 0.3417 0.3416 0.045 Uiso 1 1 calc R . . H19B H 0.4176 0.2938 0.4030 0.045 Uiso 1 1 calc R . . C20 C 0.3015(2) 0.37454(10) 0.36092(13) 0.0388(5) Uani 1 1 d . . . H20B H 0.3318 0.4062 0.4045 0.047 Uiso 1 1 calc R . . H20A H 0.2945 0.4012 0.3100 0.047 Uiso 1 1 calc R . . C21 C 0.0683(2) 0.40515(10) 0.37716(14) 0.0445(5) Uani 1 1 d . . . H21C H -0.0236 0.3880 0.3874 0.067 Uiso 1 1 calc R . . H21A H 0.0697 0.4266 0.3236 0.067 Uiso 1 1 calc R . . H21B H 0.0940 0.4390 0.4185 0.067 Uiso 1 1 calc R . . C22 C 0.1676(2) 0.31941(11) 0.46215(12) 0.0413(5) Uani 1 1 d . . . H22B H 0.1977 0.3546 0.5009 0.062 Uiso 1 1 calc R . . H22A H 0.2308 0.2806 0.4648 0.062 Uiso 1 1 calc R . . H22C H 0.0757 0.3039 0.4755 0.062 Uiso 1 1 calc R . . C23 C -0.19781(18) 0.03789(9) 0.23599(11) 0.0284(4) Uani 1 1 d . . . C24 C -0.13252(19) -0.02858(9) 0.20868(12) 0.0355(4) Uani 1 1 d . . . H24A H -0.0727 -0.0463 0.2521 0.053 Uiso 1 1 calc R . . H24C H -0.0788 -0.0201 0.1604 0.053 Uiso 1 1 calc R . . H24B H -0.2040 -0.0622 0.1959 0.053 Uiso 1 1 calc R . . C25 C -0.2930(2) 0.06138(11) 0.16618(15) 0.0551(7) Uani 1 1 d . . . H25A H -0.2392 0.0700 0.1180 0.083 Uiso 1 1 calc R . . H25B H -0.3399 0.1035 0.1818 0.083 Uiso 1 1 calc R . . H25C H -0.3606 0.0256 0.1543 0.083 Uiso 1 1 calc R . . C26 C -0.2855(2) 0.02144(11) 0.30829(14) 0.0545(6) Uani 1 1 d . . . H26B H -0.3499 -0.0151 0.2937 0.082 Uiso 1 1 calc R . . H26C H -0.3361 0.0624 0.3240 0.082 Uiso 1 1 calc R . . H26A H -0.2268 0.0064 0.3537 0.082 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 Zn1 0.02353(12) 0.02176(13) 0.02151(12) 0.00031(10) -0.00080(8) -0.00198(10) Na1 0.0240(3) 0.0250(4) 0.0273(3) 0.0004(3) -0.0039(3) -0.0025(3) N1 0.0242(7) 0.0241(7) 0.0203(7) 0.0017(6) -0.0005(6) 0.0002(6) N2 0.0229(7) 0.0268(8) 0.0194(7) 0.0015(6) -0.0024(6) 0.0033(6) N3 0.0235(8) 0.0305(8) 0.0379(9) 0.0026(7) -0.0048(6) -0.0018(7) N4 0.0333(8) 0.0258(8) 0.0356(9) -0.0037(7) -0.0098(7) 0.0019(7) C1 0.0303(9) 0.0281(9) 0.0223(9) 0.0005(7) -0.0003(7) -0.0002(8) C2 0.0356(10) 0.0284(10) 0.0281(10) 0.0011(8) 0.0037(8) 0.0024(8) C3 0.0346(10) 0.0595(14) 0.0393(11) -0.0089(10) -0.0022(9) 0.0126(10) C4 0.0485(12) 0.0354(11) 0.0348(11) -0.0054(9) 0.0035(9) 0.0052(10) C5 0.0240(9) 0.0294(9) 0.0225(9) 0.0002(7) 0.0000(7) -0.0015(7) C6 0.0275(9) 0.0281(9) 0.0217(8) -0.0005(7) 0.0003(7) 0.0034(8) C7 0.0372(10) 0.0281(10) 0.0340(10) 0.0034(8) 0.0007(8) -0.0020(8) C8 0.0354(10) 0.0374(11) 0.0352(11) 0.0028(9) -0.0023(8) 0.0086(9) C9 0.0293(9) 0.0323(10) 0.0199(9) -0.0005(8) -0.0013(7) 0.0000(8) C10 0.0260(9) 0.0362(10) 0.0230(9) -0.0049(8) -0.0014(7) 0.0005(8) C11 0.0317(10) 0.0403(11) 0.0411(11) -0.0121(9) -0.0041(8) 0.0061(9) C12 0.0330(10) 0.0629(14) 0.0349(11) -0.0034(10) 0.0065(9) 0.0017(10) C13 0.0241(8) 0.0286(10) 0.0250(9) 0.0012(7) -0.0032(7) -0.0006(7) C14 0.0325(10) 0.0291(10) 0.0354(10) 0.0011(8) -0.0100(8) 0.0026(8) C15 0.0638(15) 0.0304(11) 0.0650(15) -0.0043(11) -0.0302(12) 0.0102(11) C16 0.0349(11) 0.0411(12) 0.0557(13) 0.0046(10) -0.0098(10) 0.0094(10) C17 0.0267(10) 0.0412(12) 0.0588(14) -0.0002(10) -0.0095(9) 0.0040(9) C18 0.0314(10) 0.0521(13) 0.0438(12) 0.0083(10) 0.0020(9) -0.0057(10) C19 0.0299(10) 0.0344(11) 0.0469(12) 0.0013(9) -0.0086(9) -0.0080(8) C20 0.0381(11) 0.0296(11) 0.0483(12) -0.0027(9) -0.0065(9) -0.0067(9) C21 0.0453(12) 0.0328(11) 0.0547(14) -0.0125(10) -0.0137(10) 0.0059(9) C22 0.0416(11) 0.0459(12) 0.0359(11) -0.0038(10) -0.0087(9) -0.0046(10) C23 0.0291(9) 0.0224(9) 0.0338(10) 0.0001(8) -0.0014(7) -0.0059(8) C24 0.0367(10) 0.0298(10) 0.0399(11) -0.0092(9) -0.0033(8) -0.0048(8) C25 0.0449(13) 0.0349(12) 0.0841(18) 0.0075(12) -0.0308(12) -0.0129(10) C26 0.0578(14) 0.0393(12) 0.0676(15) -0.0163(11) 0.0269(12) -0.0247(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 N2 1.9830(14) . ? Zn1 N1 2.0281(14) . ? Zn1 C23 2.0330(17) . ? Zn1 Na1 3.1328(7) . ? Na1 N1 2.4444(14) . ? Na1 N2 2.4460(15) . ? Na1 N3 2.5540(16) . ? Na1 N4 2.5927(16) . ? N1 C1 1.460(2) . ? N1 C5 1.473(2) . ? N2 C9 1.454(2) . ? N2 C13 1.461(2) . ? N3 C17 1.469(2) . ? N3 C19 1.470(2) . ? N3 C18 1.474(2) . ? N4 C22 1.468(2) . ? N4 C21 1.468(2) . ? N4 C20 1.470(2) . ? C1 C2 1.517(2) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C3 1.514(3) . ? C2 C4 1.528(2) . ? C2 H2 1.0000 . ? C3 H3A 0.9800 . ? C3 H3C 0.9800 . ? C3 H3B 0.9800 . ? C4 H4A 0.9800 . ? C4 H4C 0.9800 . ? C4 H4B 0.9800 . ? C5 C6 1.533(2) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C7 1.519(2) . ? C6 C8 1.520(2) . ? C6 H6 1.0000 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8C 0.9800 . ? C8 H8B 0.9800 . ? C9 C10 1.529(2) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C11 1.523(3) . ? C10 C12 1.526(2) . ? C10 H10 1.0000 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C11 H11A 0.9800 . ? C12 H12C 0.9800 . ? C12 H12B 0.9800 . ? C12 H12A 0.9800 . ? C13 C14 1.532(2) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.511(3) . ? C14 C16 1.526(2) . ? C14 H14 1.0000 . ? C15 H15C 0.9800 . ? C15 H15B 0.9800 . ? C15 H15A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C16 H16A 0.9800 . ? C17 H17C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C18 H18B 0.9800 . ? C18 H18A 0.9800 . ? C18 H18C 0.9800 . ? C19 C20 1.513(3) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 H20B 0.9900 . ? C20 H20A 0.9900 . ? C21 H21C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C22 H22B 0.9800 . ? C22 H22A 0.9800 . ? C22 H22C 0.9800 . ? C23 C24 1.521(2) . ? C23 C26 1.522(3) . ? C23 C25 1.538(3) . ? C24 H24A 0.9800 . ? C24 H24C 0.9800 . ? C24 H24B 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C26 H26A 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 Zn1 N1 102.58(6) . . ? N2 Zn1 C23 132.44(6) . . ? N1 Zn1 C23 123.83(6) . . ? N2 Zn1 Na1 51.33(4) . . ? N1 Zn1 Na1 51.26(4) . . ? C23 Zn1 Na1 170.52(5) . . ? N1 Na1 N2 79.59(5) . . ? N1 Na1 N3 123.56(5) . . ? N2 Na1 N3 125.04(5) . . ? N1 Na1 N4 150.54(5) . . ? N2 Na1 N4 113.02(5) . . ? N3 Na1 N4 72.35(5) . . ? N1 Na1 Zn1 40.32(3) . . ? N2 Na1 Zn1 39.27(3) . . ? N3 Na1 Zn1 136.74(4) . . ? N4 Na1 Zn1 145.17(4) . . ? C1 N1 C5 109.00(13) . . ? C1 N1 Zn1 115.54(10) . . ? C5 N1 Zn1 103.20(10) . . ? C1 N1 Na1 134.87(11) . . ? C5 N1 Na1 100.95(10) . . ? Zn1 N1 Na1 88.42(5) . . ? C9 N2 C13 111.03(13) . . ? C9 N2 Zn1 115.09(10) . . ? C13 N2 Zn1 119.95(11) . . ? C9 N2 Na1 131.92(11) . . ? C13 N2 Na1 87.04(9) . . ? Zn1 N2 Na1 89.41(5) . . ? C17 N3 C19 108.42(14) . . ? C17 N3 C18 108.67(16) . . ? C19 N3 C18 110.33(15) . . ? C17 N3 Na1 118.85(11) . . ? C19 N3 Na1 107.69(11) . . ? C18 N3 Na1 102.67(11) . . ? C22 N4 C21 108.43(16) . . ? C22 N4 C20 109.89(15) . . ? C21 N4 C20 108.45(15) . . ? C22 N4 Na1 102.96(11) . . ? C21 N4 Na1 120.17(11) . . ? C20 N4 Na1 106.61(11) . . ? N1 C1 C2 114.44(14) . . ? N1 C1 H1A 108.7 . . ? C2 C1 H1A 108.7 . . ? N1 C1 H1B 108.7 . . ? C2 C1 H1B 108.7 . . ? H1A C1 H1B 107.6 . . ? C3 C2 C1 112.26(15) . . ? C3 C2 C4 110.26(16) . . ? C1 C2 C4 110.27(15) . . ? C3 C2 H2 108.0 . . ? C1 C2 H2 108.0 . . ? C4 C2 H2 108.0 . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? H3C C3 H3B 109.5 . . ? C2 C4 H4A 109.5 . . ? C2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? C2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? H4C C4 H4B 109.5 . . ? N1 C5 C6 117.79(14) . . ? N1 C5 H5A 107.9 . . ? C6 C5 H5A 107.9 . . ? N1 C5 H5B 107.9 . . ? C6 C5 H5B 107.9 . . ? H5A C5 H5B 107.2 . . ? C7 C6 C8 110.81(15) . . ? C7 C6 C5 111.55(14) . . ? C8 C6 C5 109.41(14) . . ? C7 C6 H6 108.3 . . ? C8 C6 H6 108.3 . . ? C5 C6 H6 108.3 . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C6 C8 H8A 109.5 . . ? C6 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? C6 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? H8C C8 H8B 109.5 . . ? N2 C9 C10 112.38(14) . . ? N2 C9 H9A 109.1 . . ? C10 C9 H9A 109.1 . . ? N2 C9 H9B 109.1 . . ? C10 C9 H9B 109.1 . . ? H9A C9 H9B 107.9 . . ? C11 C10 C12 110.07(16) . . ? C11 C10 C9 112.40(15) . . ? C12 C10 C9 110.83(15) . . ? C11 C10 H10 107.8 . . ? C12 C10 H10 107.8 . . ? C9 C10 H10 107.8 . . ? C10 C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C11 H11A 109.5 . . ? H11B C11 H11A 109.5 . . ? H11C C11 H11A 109.5 . . ? C10 C12 H12C 109.5 . . ? C10 C12 H12B 109.5 . . ? H12C C12 H12B 109.5 . . ? C10 C12 H12A 109.5 . . ? H12C C12 H12A 109.5 . . ? H12B C12 H12A 109.5 . . ? N2 C13 C14 119.62(14) . . ? N2 C13 H13A 107.4 . . ? C14 C13 H13A 107.4 . . ? N2 C13 H13B 107.4 . . ? C14 C13 H13B 107.4 . . ? H13A C13 H13B 106.9 . . ? C15 C14 C16 111.76(17) . . ? C15 C14 C13 112.12(15) . . ? C16 C14 C13 109.29(15) . . ? C15 C14 H14 107.8 . . ? C16 C14 H14 107.8 . . ? C13 C14 H14 107.8 . . ? C14 C15 H15C 109.5 . . ? C14 C15 H15B 109.5 . . ? H15C C15 H15B 109.5 . . ? C14 C15 H15A 109.5 . . ? H15C C15 H15A 109.5 . . ? H15B C15 H15A 109.5 . . ? C14 C16 H16B 109.5 . . ? C14 C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C14 C16 H16A 109.5 . . ? H16B C16 H16A 109.5 . . ? H16C C16 H16A 109.5 . . ? N3 C17 H17C 109.5 . . ? N3 C17 H17A 109.5 . . ? H17C C17 H17A 109.5 . . ? N3 C17 H17B 109.5 . . ? H17C C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? N3 C18 H18B 109.5 . . ? N3 C18 H18A 109.5 . . ? H18B C18 H18A 109.5 . . ? N3 C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? N3 C19 C20 114.15(15) . . ? N3 C19 H19A 108.7 . . ? C20 C19 H19A 108.7 . . ? N3 C19 H19B 108.7 . . ? C20 C19 H19B 108.7 . . ? H19A C19 H19B 107.6 . . ? N4 C20 C19 113.96(15) . . ? N4 C20 H20B 108.8 . . ? C19 C20 H20B 108.8 . . ? N4 C20 H20A 108.8 . . ? C19 C20 H20A 108.8 . . ? H20B C20 H20A 107.7 . . ? N4 C21 H21C 109.5 . . ? N4 C21 H21A 109.5 . . ? H21C C21 H21A 109.5 . . ? N4 C21 H21B 109.5 . . ? H21C C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? N4 C22 H22B 109.5 . . ? N4 C22 H22A 109.5 . . ? H22B C22 H22A 109.5 . . ? N4 C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? C24 C23 C26 107.51(16) . . ? C24 C23 C25 106.54(16) . . ? C26 C23 C25 107.99(18) . . ? C24 C23 Zn1 111.75(12) . . ? C26 C23 Zn1 112.91(13) . . ? C25 C23 Zn1 109.87(12) . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? H24C C24 H24B 109.5 . . ? C23 C25 H25A 109.5 . . ? C23 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C23 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C23 C26 H26B 109.5 . . ? C23 C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C23 C26 H26A 109.5 . . ? H26B C26 H26A 109.5 . . ? H26C C26 H26A 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 Zn1 Na1 N1 -178.93(7) . . . . ? C23 Zn1 Na1 N1 -61.9(3) . . . . ? N1 Zn1 Na1 N2 178.93(7) . . . . ? C23 Zn1 Na1 N2 117.1(3) . . . . ? N2 Zn1 Na1 N3 91.37(8) . . . . ? N1 Zn1 Na1 N3 -89.69(8) . . . . ? C23 Zn1 Na1 N3 -151.6(3) . . . . ? N2 Zn1 Na1 N4 -47.44(8) . . . . ? N1 Zn1 Na1 N4 131.49(9) . . . . ? C23 Zn1 Na1 N4 69.6(3) . . . . ? N2 Zn1 N1 C1 141.11(11) . . . . ? C23 Zn1 N1 C1 -49.81(14) . . . . ? Na1 Zn1 N1 C1 140.26(13) . . . . ? N2 Zn1 N1 C5 -100.02(10) . . . . ? C23 Zn1 N1 C5 69.06(12) . . . . ? Na1 Zn1 N1 C5 -100.87(10) . . . . ? N2 Zn1 N1 Na1 0.85(6) . . . . ? C23 Zn1 N1 Na1 169.93(6) . . . . ? N2 Na1 N1 C1 -126.21(15) . . . . ? N3 Na1 N1 C1 -0.86(17) . . . . ? N4 Na1 N1 C1 114.90(16) . . . . ? Zn1 Na1 N1 C1 -125.53(16) . . . . ? N2 Na1 N1 C5 102.45(10) . . . . ? N3 Na1 N1 C5 -132.19(9) . . . . ? N4 Na1 N1 C5 -16.43(16) . . . . ? Zn1 Na1 N1 C5 103.14(10) . . . . ? N2 Na1 N1 Zn1 -0.69(5) . . . . ? N3 Na1 N1 Zn1 124.67(6) . . . . ? N4 Na1 N1 Zn1 -119.57(10) . . . . ? N1 Zn1 N2 C9 136.27(12) . . . . ? C23 Zn1 N2 C9 -31.41(16) . . . . ? Na1 Zn1 N2 C9 137.12(13) . . . . ? N1 Zn1 N2 C13 -87.09(12) . . . . ? C23 Zn1 N2 C13 105.23(13) . . . . ? Na1 Zn1 N2 C13 -86.24(12) . . . . ? N1 Zn1 N2 Na1 -0.85(6) . . . . ? C23 Zn1 N2 Na1 -168.54(7) . . . . ? N1 Na1 N2 C9 -123.39(14) . . . . ? N3 Na1 N2 C9 112.72(14) . . . . ? N4 Na1 N2 C9 28.71(15) . . . . ? Zn1 Na1 N2 C9 -124.10(15) . . . . ? N1 Na1 N2 C13 120.73(10) . . . . ? N3 Na1 N2 C13 -3.16(11) . . . . ? N4 Na1 N2 C13 -87.17(10) . . . . ? Zn1 Na1 N2 C13 120.03(11) . . . . ? N1 Na1 N2 Zn1 0.70(5) . . . . ? N3 Na1 N2 Zn1 -123.19(6) . . . . ? N4 Na1 N2 Zn1 152.80(5) . . . . ? N1 Na1 N3 C17 -70.02(14) . . . . ? N2 Na1 N3 C17 31.53(16) . . . . ? N4 Na1 N3 C17 137.68(14) . . . . ? Zn1 Na1 N3 C17 -19.08(16) . . . . ? N1 Na1 N3 C19 166.32(11) . . . . ? N2 Na1 N3 C19 -92.13(12) . . . . ? N4 Na1 N3 C19 14.02(11) . . . . ? Zn1 Na1 N3 C19 -142.74(10) . . . . ? N1 Na1 N3 C18 49.87(13) . . . . ? N2 Na1 N3 C18 151.42(11) . . . . ? N4 Na1 N3 C18 -102.43(12) . . . . ? Zn1 Na1 N3 C18 100.81(12) . . . . ? N1 Na1 N4 C22 130.42(13) . . . . ? N2 Na1 N4 C22 19.76(13) . . . . ? N3 Na1 N4 C22 -101.54(12) . . . . ? Zn1 Na1 N4 C22 50.19(14) . . . . ? N1 Na1 N4 C21 9.8(2) . . . . ? N2 Na1 N4 C21 -100.84(15) . . . . ? N3 Na1 N4 C21 137.86(15) . . . . ? Zn1 Na1 N4 C21 -70.41(16) . . . . ? N1 Na1 N4 C20 -113.92(14) . . . . ? N2 Na1 N4 C20 135.41(11) . . . . ? N3 Na1 N4 C20 14.11(11) . . . . ? Zn1 Na1 N4 C20 165.85(10) . . . . ? C5 N1 C1 C2 -164.99(14) . . . . ? Zn1 N1 C1 C2 -49.38(18) . . . . ? Na1 N1 C1 C2 66.2(2) . . . . ? N1 C1 C2 C3 -63.3(2) . . . . ? N1 C1 C2 C4 173.34(15) . . . . ? C1 N1 C5 C6 -66.22(18) . . . . ? Zn1 N1 C5 C6 170.47(12) . . . . ? Na1 N1 C5 C6 79.52(14) . . . . ? N1 C5 C6 C7 -56.36(19) . . . . ? N1 C5 C6 C8 -179.32(14) . . . . ? C13 N2 C9 C10 166.08(14) . . . . ? Zn1 N2 C9 C10 -53.51(17) . . . . ? Na1 N2 C9 C10 60.38(19) . . . . ? N2 C9 C10 C11 -71.45(19) . . . . ? N2 C9 C10 C12 164.90(15) . . . . ? C9 N2 C13 C14 59.9(2) . . . . ? Zn1 N2 C13 C14 -78.28(18) . . . . ? Na1 N2 C13 C14 -165.89(15) . . . . ? N2 C13 C14 C15 54.1(2) . . . . ? N2 C13 C14 C16 178.64(16) . . . . ? C17 N3 C19 C20 -172.04(17) . . . . ? C18 N3 C19 C20 69.1(2) . . . . ? Na1 N3 C19 C20 -42.26(18) . . . . ? C22 N4 C20 C19 68.9(2) . . . . ? C21 N4 C20 C19 -172.76(16) . . . . ? Na1 N4 C20 C19 -42.04(18) . . . . ? N3 C19 C20 N4 61.4(2) . . . . ? N2 Zn1 C23 C24 -99.62(14) . . . . ? N1 Zn1 C23 C24 94.89(13) . . . . ? Na1 Zn1 C23 C24 150.8(3) . . . . ? N2 Zn1 C23 C26 21.73(19) . . . . ? N1 Zn1 C23 C26 -143.76(14) . . . . ? Na1 Zn1 C23 C26 -87.9(4) . . . . ? N2 Zn1 C23 C25 142.34(13) . . . . ? N1 Zn1 C23 C25 -23.15(17) . . . . ? Na1 Zn1 C23 C25 32.7(4) . . . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 67.50 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.497 _refine_diff_density_min -0.216 _refine_diff_density_rms 0.044 #===END #------------------------------------------------------- #------------------COMPOUND 5-------------------------- #----------------------------------------------------- data_pgagf4 _database_code_depnum_ccdc_archive 'CCDC 734664' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27 H58 Mg N5 Na' _chemical_formula_weight 500.08 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Mg Mg 0.0486 0.0363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting MONOCLINIC _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 14.1862(4) _cell_length_b 15.1005(5) _cell_length_c 14.6621(4) _cell_angle_alpha 90.00 _cell_angle_beta 97.090(3) _cell_angle_gamma 90.00 _cell_volume 3116.88(16) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 8352 _cell_measurement_theta_min 2.5162 _cell_measurement_theta_max 30.3485 _exptl_crystal_description fragment _exptl_crystal_colour colourless _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.066 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1112 _exptl_absorpt_coefficient_mu 0.093 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.99393 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.24 (release 21-04-2008 CrysAlis171 .NET) (compiled Apr 21 2008,18:23:10) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _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 'Oxford Diffraction Gemini S' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25234 _diffrn_reflns_av_R_equivalents 0.0370 _diffrn_reflns_av_sigmaI/netI 0.0730 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.52 _diffrn_reflns_theta_max 30.47 _reflns_number_total 8635 _reflns_number_gt 5421 _reflns_threshold_expression >2sigma(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^)+(0.0506P)^2^+0.0000P] 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 8635 _refine_ls_number_parameters 317 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0987 _refine_ls_R_factor_gt 0.0475 _refine_ls_wR_factor_ref 0.1045 _refine_ls_wR_factor_gt 0.0931 _refine_ls_goodness_of_fit_ref 0.949 _refine_ls_restrained_S_all 0.949 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mg1 Mg 0.67976(3) 0.12754(3) 0.80275(3) 0.01645(11) Uani 1 1 d . . . Na1 Na 0.47972(4) 0.20600(4) 0.82822(4) 0.02167(14) Uani 1 1 d . . . N1 N 0.55765(8) 0.09716(8) 0.71954(8) 0.0196(3) Uani 1 1 d . . . N2 N 0.80904(8) 0.08483(8) 0.78711(7) 0.0188(3) Uani 1 1 d . . . N3 N 0.64685(7) 0.21072(8) 0.90525(7) 0.0168(2) Uani 1 1 d . . . N4 N 0.37071(8) 0.34299(8) 0.78571(8) 0.0240(3) Uani 1 1 d . . . N5 N 0.31958(8) 0.18517(8) 0.90039(8) 0.0230(3) Uani 1 1 d . . . C1 C 0.52624(10) 0.14086(11) 0.63207(10) 0.0271(3) Uani 1 1 d . . . H1 H 0.5594 0.1113 0.5839 0.033 Uiso 1 1 calc R . . C2 C 0.41890(11) 0.12876(13) 0.60454(12) 0.0416(5) Uani 1 1 d . . . H2A H 0.3839 0.1576 0.6508 0.050 Uiso 1 1 calc R . . H2B H 0.3999 0.1578 0.5446 0.050 Uiso 1 1 calc R . . C3 C 0.39265(12) 0.03165(14) 0.59762(13) 0.0475(5) Uani 1 1 d . . . H3A H 0.3226 0.0257 0.5903 0.057 Uiso 1 1 calc R . . H3B H 0.4160 0.0059 0.5425 0.057 Uiso 1 1 calc R . . C4 C 0.43458(10) -0.01921(12) 0.68192(12) 0.0367(4) Uani 1 1 d . . . H4A H 0.4267 -0.0835 0.6702 0.044 Uiso 1 1 calc R . . H4B H 0.3999 -0.0038 0.7343 0.044 Uiso 1 1 calc R . . C5 C 0.54019(10) 0.00186(10) 0.70691(10) 0.0239(3) Uani 1 1 d . . . H5 H 0.5739 -0.0179 0.6545 0.029 Uiso 1 1 calc R . . C6 C 0.57971(11) -0.05091(10) 0.79047(11) 0.0296(4) Uani 1 1 d . . . H6A H 0.6480 -0.0397 0.8041 0.044 Uiso 1 1 calc R . . H6B H 0.5689 -0.1142 0.7784 0.044 Uiso 1 1 calc R . . H6C H 0.5478 -0.0331 0.8432 0.044 Uiso 1 1 calc R . . C7 C 0.55326(12) 0.23784(11) 0.63324(11) 0.0348(4) Uani 1 1 d . . . H7A H 0.5246 0.2682 0.6821 0.052 Uiso 1 1 calc R . . H7B H 0.5301 0.2647 0.5738 0.052 Uiso 1 1 calc R . . H7C H 0.6225 0.2435 0.6445 0.052 Uiso 1 1 calc R . . C8 C 0.84606(9) 0.08025(10) 0.69894(9) 0.0190(3) Uani 1 1 d . . . H8 H 0.8756 0.0205 0.6944 0.023 Uiso 1 1 calc R . . C9 C 0.92320(10) 0.14949(11) 0.69117(10) 0.0272(3) Uani 1 1 d . . . H9A H 0.9489 0.1418 0.6319 0.033 Uiso 1 1 calc R . . H9B H 0.8949 0.2094 0.6918 0.033 Uiso 1 1 calc R . . C10 C 1.00357(10) 0.14187(12) 0.76928(11) 0.0329(4) Uani 1 1 d . . . H10A H 1.0463 0.1936 0.7683 0.039 Uiso 1 1 calc R . . H10B H 1.0410 0.0878 0.7609 0.039 Uiso 1 1 calc R . . C11 C 0.96513(10) 0.13768(11) 0.86178(11) 0.0311(4) Uani 1 1 d . . . H11A H 0.9399 0.1964 0.8764 0.037 Uiso 1 1 calc R . . H11B H 1.0173 0.1225 0.9105 0.037 Uiso 1 1 calc R . . C12 C 0.88617(9) 0.06821(10) 0.85986(10) 0.0235(3) Uani 1 1 d . . . H12 H 0.9144 0.0094 0.8474 0.028 Uiso 1 1 calc R . . C13 C 0.84996(11) 0.06266(13) 0.95271(10) 0.0370(4) Uani 1 1 d . . . H13A H 0.8219 0.1196 0.9669 0.055 Uiso 1 1 calc R . . H13B H 0.9029 0.0488 1.0001 0.055 Uiso 1 1 calc R . . H13C H 0.8017 0.0161 0.9513 0.055 Uiso 1 1 calc R . . C14 C 0.76817(10) 0.08932(10) 0.61927(9) 0.0228(3) Uani 1 1 d . . . H14A H 0.7192 0.0445 0.6246 0.034 Uiso 1 1 calc R . . H14B H 0.7949 0.0808 0.5614 0.034 Uiso 1 1 calc R . . H14C H 0.7399 0.1485 0.6202 0.034 Uiso 1 1 calc R . . C15 C 0.63674(9) 0.18004(9) 0.99836(9) 0.0189(3) Uani 1 1 d . . . H15 H 0.7022 0.1714 1.0311 0.023 Uiso 1 1 calc R . . C16 C 0.58679(10) 0.24795(10) 1.05327(10) 0.0233(3) Uani 1 1 d . . . H16A H 0.5215 0.2581 1.0228 0.028 Uiso 1 1 calc R . . H16B H 0.5824 0.2246 1.1157 0.028 Uiso 1 1 calc R . . C17 C 0.64079(11) 0.33478(10) 1.06023(10) 0.0268(3) Uani 1 1 d . . . H17A H 0.7018 0.3271 1.1002 0.032 Uiso 1 1 calc R . . H17B H 0.6033 0.3803 1.0883 0.032 Uiso 1 1 calc R . . C18 C 0.65985(11) 0.36524(10) 0.96503(10) 0.0266(3) Uani 1 1 d . . . H18A H 0.5994 0.3840 0.9293 0.032 Uiso 1 1 calc R . . H18B H 0.7029 0.4170 0.9713 0.032 Uiso 1 1 calc R . . C19 C 0.70449(10) 0.29196(10) 0.91318(10) 0.0221(3) Uani 1 1 d . . . H19 H 0.7673 0.2770 0.9485 0.026 Uiso 1 1 calc R . . C20 C 0.72285(12) 0.32592(11) 0.81911(11) 0.0344(4) Uani 1 1 d . . . H20A H 0.7534 0.2793 0.7866 0.052 Uiso 1 1 calc R . . H20B H 0.7645 0.3778 0.8268 0.052 Uiso 1 1 calc R . . H20C H 0.6624 0.3425 0.7834 0.052 Uiso 1 1 calc R . . C21 C 0.58667(11) 0.09145(10) 0.99683(10) 0.0265(3) Uani 1 1 d . . . H21A H 0.5237 0.0966 0.9614 0.040 Uiso 1 1 calc R . . H21B H 0.5799 0.0733 1.0599 0.040 Uiso 1 1 calc R . . H21C H 0.6240 0.0471 0.9682 0.040 Uiso 1 1 calc R . . C22 C 0.37178(13) 0.38096(12) 0.69320(12) 0.0383(4) Uani 1 1 d . . . H22A H 0.3249 0.4288 0.6837 0.057 Uiso 1 1 calc R . . H22B H 0.3560 0.3348 0.6469 0.057 Uiso 1 1 calc R . . H22C H 0.4351 0.4046 0.6875 0.057 Uiso 1 1 calc R . . C23 C 0.39517(12) 0.41281(12) 0.85327(12) 0.0397(4) Uani 1 1 d . . . H23A H 0.3434 0.4561 0.8499 0.060 Uiso 1 1 calc R . . H23B H 0.4536 0.4423 0.8403 0.060 Uiso 1 1 calc R . . H23C H 0.4050 0.3869 0.9150 0.060 Uiso 1 1 calc R . . C24 C 0.27423(10) 0.30895(11) 0.79041(11) 0.0310(4) Uani 1 1 d . . . H24A H 0.2585 0.2657 0.7401 0.037 Uiso 1 1 calc R . . H24B H 0.2287 0.3587 0.7800 0.037 Uiso 1 1 calc R . . C25 C 0.26102(10) 0.26495(10) 0.88025(11) 0.0300(4) Uani 1 1 d . . . H25A H 0.2766 0.3082 0.9306 0.036 Uiso 1 1 calc R . . H25B H 0.1933 0.2486 0.8792 0.036 Uiso 1 1 calc R . . C26 C 0.32370(11) 0.16527(11) 0.99828(11) 0.0316(4) Uani 1 1 d . . . H26A H 0.2592 0.1556 1.0138 0.047 Uiso 1 1 calc R . . H26B H 0.3529 0.2151 1.0342 0.047 Uiso 1 1 calc R . . H26C H 0.3618 0.1118 1.0125 0.047 Uiso 1 1 calc R . . C27 C 0.27658(11) 0.10965(11) 0.84834(12) 0.0341(4) Uani 1 1 d . . . H27A H 0.3164 0.0571 0.8619 0.051 Uiso 1 1 calc R . . H27B H 0.2714 0.1227 0.7824 0.051 Uiso 1 1 calc R . . H27C H 0.2132 0.0986 0.8659 0.051 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mg1 0.0140(2) 0.0196(3) 0.0161(2) -0.00048(19) 0.00299(18) 0.00096(19) Na1 0.0169(3) 0.0240(3) 0.0240(3) -0.0008(2) 0.0020(2) 0.0025(2) N1 0.0167(5) 0.0235(7) 0.0181(6) -0.0025(5) 0.0004(5) 0.0024(5) N2 0.0155(5) 0.0257(7) 0.0156(6) 0.0011(5) 0.0034(5) 0.0021(5) N3 0.0156(5) 0.0183(6) 0.0163(6) -0.0001(5) 0.0015(5) -0.0022(5) N4 0.0221(6) 0.0208(7) 0.0289(7) 0.0026(5) 0.0028(5) 0.0032(5) N5 0.0204(6) 0.0212(7) 0.0275(7) -0.0005(5) 0.0034(5) 0.0007(5) C1 0.0241(7) 0.0362(10) 0.0205(7) -0.0023(7) 0.0004(6) 0.0103(7) C2 0.0256(8) 0.0635(14) 0.0327(9) -0.0048(9) -0.0083(7) 0.0129(9) C3 0.0204(8) 0.0704(15) 0.0483(11) -0.0266(10) -0.0094(8) 0.0013(9) C4 0.0198(8) 0.0419(11) 0.0492(11) -0.0218(9) 0.0077(7) -0.0076(7) C5 0.0178(7) 0.0273(9) 0.0276(8) -0.0095(7) 0.0070(6) -0.0015(6) C6 0.0321(8) 0.0218(9) 0.0366(9) -0.0019(7) 0.0115(7) -0.0028(7) C7 0.0385(9) 0.0387(11) 0.0275(8) 0.0092(7) 0.0054(7) 0.0151(8) C8 0.0178(6) 0.0201(8) 0.0201(7) -0.0016(6) 0.0064(6) 0.0008(6) C9 0.0230(7) 0.0333(9) 0.0266(8) 0.0029(7) 0.0077(6) -0.0045(7) C10 0.0210(7) 0.0425(11) 0.0354(9) 0.0018(8) 0.0044(7) -0.0101(7) C11 0.0206(7) 0.0426(11) 0.0287(8) -0.0060(7) -0.0025(6) 0.0010(7) C12 0.0182(7) 0.0302(9) 0.0220(7) 0.0007(6) 0.0028(6) 0.0058(6) C13 0.0275(8) 0.0617(13) 0.0214(8) 0.0074(8) 0.0023(7) 0.0138(8) C14 0.0222(7) 0.0274(9) 0.0195(7) -0.0007(6) 0.0061(6) -0.0008(6) C15 0.0177(6) 0.0220(8) 0.0174(7) -0.0013(6) 0.0034(5) 0.0017(6) C16 0.0245(7) 0.0257(9) 0.0210(7) -0.0031(6) 0.0077(6) -0.0001(6) C17 0.0262(8) 0.0286(9) 0.0267(8) -0.0109(7) 0.0073(7) -0.0039(7) C18 0.0288(8) 0.0199(8) 0.0315(8) -0.0050(7) 0.0052(7) -0.0062(6) C19 0.0188(7) 0.0235(8) 0.0242(8) -0.0024(6) 0.0039(6) -0.0043(6) C20 0.0444(10) 0.0274(9) 0.0345(9) -0.0016(7) 0.0178(8) -0.0096(8) C21 0.0326(8) 0.0203(8) 0.0287(8) 0.0015(6) 0.0117(7) 0.0014(7) C22 0.0429(10) 0.0351(10) 0.0364(10) 0.0079(8) 0.0030(8) 0.0137(8) C23 0.0405(10) 0.0324(10) 0.0446(11) -0.0057(8) -0.0010(8) -0.0004(8) C24 0.0224(7) 0.0291(10) 0.0408(10) 0.0003(7) 0.0006(7) 0.0065(7) C25 0.0221(7) 0.0276(9) 0.0416(10) -0.0011(7) 0.0092(7) 0.0051(6) C26 0.0297(8) 0.0358(10) 0.0302(9) 0.0016(7) 0.0070(7) -0.0042(7) C27 0.0322(8) 0.0294(10) 0.0401(10) -0.0077(8) 0.0024(8) 0.0018(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mg1 N2 1.9840(11) . ? Mg1 N1 2.0441(12) . ? Mg1 N3 2.0560(12) . ? Mg1 Na1 3.1397(7) . ? Na1 N3 2.4982(12) . ? Na1 N4 2.6117(13) . ? Na1 N1 2.6263(12) . ? Na1 N5 2.6406(12) . ? N1 C1 1.4620(18) . ? N1 C5 1.4680(18) . ? N2 C12 1.4526(17) . ? N2 C8 1.4558(16) . ? N3 C15 1.4653(17) . ? N3 C19 1.4710(18) . ? N4 C23 1.459(2) . ? N4 C24 1.4716(19) . ? N4 C22 1.474(2) . ? N5 C26 1.4605(19) . ? N5 C27 1.4630(19) . ? N5 C25 1.4725(18) . ? C1 C7 1.513(2) . ? C1 C2 1.537(2) . ? C1 H1 1.0000 . ? C2 C3 1.513(3) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.513(3) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.5311(19) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.510(2) . ? C5 H5 1.0000 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 C14 1.5118(19) . ? C8 C9 1.5278(19) . ? C8 H8 1.0000 . ? C9 C10 1.517(2) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C11 1.524(2) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.532(2) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C13 1.515(2) . ? C12 H12 1.0000 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C21 1.514(2) . ? C15 C16 1.5307(19) . ? C15 H15 1.0000 . ? C16 C17 1.516(2) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.525(2) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C19 1.524(2) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.524(2) . ? C19 H19 1.0000 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 C25 1.508(2) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 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 Mg1 N1 125.83(5) . . ? N2 Mg1 N3 125.43(5) . . ? N1 Mg1 N3 108.74(5) . . ? N2 Mg1 Na1 176.79(4) . . ? N1 Mg1 Na1 56.21(3) . . ? N3 Mg1 Na1 52.59(3) . . ? N3 Na1 N4 125.90(4) . . ? N3 Na1 N1 81.09(4) . . ? N4 Na1 N1 129.20(4) . . ? N3 Na1 N5 129.62(4) . . ? N4 Na1 N5 71.13(4) . . ? N1 Na1 N5 128.02(4) . . ? N3 Na1 Mg1 40.82(3) . . ? N4 Na1 Mg1 141.97(3) . . ? N1 Na1 Mg1 40.30(3) . . ? N5 Na1 Mg1 146.89(3) . . ? C1 N1 C5 107.66(11) . . ? C1 N1 Mg1 124.49(9) . . ? C5 N1 Mg1 114.37(9) . . ? C1 N1 Na1 98.30(8) . . ? C5 N1 Na1 127.80(8) . . ? Mg1 N1 Na1 83.49(4) . . ? C12 N2 C8 108.80(10) . . ? C12 N2 Mg1 126.48(9) . . ? C8 N2 Mg1 123.92(9) . . ? C15 N3 C19 107.90(10) . . ? C15 N3 Mg1 123.03(9) . . ? C19 N3 Mg1 113.14(8) . . ? C15 N3 Na1 102.45(8) . . ? C19 N3 Na1 123.14(9) . . ? Mg1 N3 Na1 86.59(4) . . ? C23 N4 C24 111.42(12) . . ? C23 N4 C22 108.36(13) . . ? C24 N4 C22 107.11(12) . . ? C23 N4 Na1 109.03(9) . . ? C24 N4 Na1 103.82(9) . . ? C22 N4 Na1 117.04(9) . . ? C26 N5 C27 108.41(12) . . ? C26 N5 C25 108.58(12) . . ? C27 N5 C25 110.15(12) . . ? C26 N5 Na1 119.09(9) . . ? C27 N5 Na1 101.99(9) . . ? C25 N5 Na1 108.32(8) . . ? N1 C1 C7 112.17(12) . . ? N1 C1 C2 111.18(13) . . ? C7 C1 C2 111.05(13) . . ? N1 C1 H1 107.4 . . ? C7 C1 H1 107.4 . . ? C2 C1 H1 107.4 . . ? C3 C2 C1 111.12(14) . . ? C3 C2 H2A 109.4 . . ? C1 C2 H2A 109.4 . . ? C3 C2 H2B 109.4 . . ? C1 C2 H2B 109.4 . . ? H2A C2 H2B 108.0 . . ? C4 C3 C2 111.61(14) . . ? C4 C3 H3A 109.3 . . ? C2 C3 H3A 109.3 . . ? C4 C3 H3B 109.3 . . ? C2 C3 H3B 109.3 . . ? H3A C3 H3B 108.0 . . ? C3 C4 C5 111.37(14) . . ? C3 C4 H4A 109.4 . . ? C5 C4 H4A 109.4 . . ? C3 C4 H4B 109.4 . . ? C5 C4 H4B 109.4 . . ? H4A C4 H4B 108.0 . . ? N1 C5 C6 112.02(12) . . ? N1 C5 C4 112.26(12) . . ? C6 C5 C4 109.80(13) . . ? N1 C5 H5 107.5 . . ? C6 C5 H5 107.5 . . ? C4 C5 H5 107.5 . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C1 C7 H7A 109.5 . . ? C1 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C1 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N2 C8 C14 111.86(11) . . ? N2 C8 C9 111.96(11) . . ? C14 C8 C9 110.02(12) . . ? N2 C8 H8 107.6 . . ? C14 C8 H8 107.6 . . ? C9 C8 H8 107.6 . . ? C10 C9 C8 111.72(12) . . ? C10 C9 H9A 109.3 . . ? C8 C9 H9A 109.3 . . ? C10 C9 H9B 109.3 . . ? C8 C9 H9B 109.3 . . ? H9A C9 H9B 107.9 . . ? C9 C10 C11 110.90(12) . . ? C9 C10 H10A 109.5 . . ? C11 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? C11 C10 H10B 109.5 . . ? H10A C10 H10B 108.0 . . ? C10 C11 C12 110.68(13) . . ? C10 C11 H11A 109.5 . . ? C12 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? C12 C11 H11B 109.5 . . ? H11A C11 H11B 108.1 . . ? N2 C12 C13 111.17(11) . . ? N2 C12 C11 112.20(12) . . ? C13 C12 C11 110.45(13) . . ? N2 C12 H12 107.6 . . ? C13 C12 H12 107.6 . . ? C11 C12 H12 107.6 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C8 C14 H14A 109.5 . . ? C8 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C8 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N3 C15 C21 111.43(11) . . ? N3 C15 C16 112.53(11) . . ? C21 C15 C16 110.68(11) . . ? N3 C15 H15 107.3 . . ? C21 C15 H15 107.3 . . ? C16 C15 H15 107.3 . . ? C17 C16 C15 110.61(11) . . ? C17 C16 H16A 109.5 . . ? C15 C16 H16A 109.5 . . ? C17 C16 H16B 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 108.1 . . ? C16 C17 C18 110.16(12) . . ? C16 C17 H17A 109.6 . . ? C18 C17 H17A 109.6 . . ? C16 C17 H17B 109.6 . . ? C18 C17 H17B 109.6 . . ? H17A C17 H17B 108.1 . . ? C19 C18 C17 111.66(13) . . ? C19 C18 H18A 109.3 . . ? C17 C18 H18A 109.3 . . ? C19 C18 H18B 109.3 . . ? C17 C18 H18B 109.3 . . ? H18A C18 H18B 107.9 . . ? N3 C19 C20 111.38(12) . . ? N3 C19 C18 112.57(11) . . ? C20 C19 C18 109.59(13) . . ? N3 C19 H19 107.7 . . ? C20 C19 H19 107.7 . . ? C18 C19 H19 107.7 . . ? 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 . . ? C15 C21 H21A 109.5 . . ? C15 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C15 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? N4 C22 H22A 109.5 . . ? N4 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? N4 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? N4 C23 H23A 109.5 . . ? N4 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? N4 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? N4 C24 C25 114.30(13) . . ? N4 C24 H24A 108.7 . . ? C25 C24 H24A 108.7 . . ? N4 C24 H24B 108.7 . . ? C25 C24 H24B 108.7 . . ? H24A C24 H24B 107.6 . . ? N5 C25 C24 114.07(12) . . ? N5 C25 H25A 108.7 . . ? C24 C25 H25A 108.7 . . ? N5 C25 H25B 108.7 . . ? C24 C25 H25B 108.7 . . ? H25A C25 H25B 107.6 . . ? N5 C26 H26A 109.5 . . ? N5 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? N5 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? N5 C27 H27A 109.5 . . ? N5 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? N5 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 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 Mg1 Na1 N3 -52.8(7) . . . . ? N1 Mg1 Na1 N3 176.90(6) . . . . ? N2 Mg1 Na1 N4 35.8(7) . . . . ? N1 Mg1 Na1 N4 -94.50(7) . . . . ? N3 Mg1 Na1 N4 88.60(7) . . . . ? N2 Mg1 Na1 N1 130.3(7) . . . . ? N3 Mg1 Na1 N1 -176.90(6) . . . . ? N2 Mg1 Na1 N5 -143.4(7) . . . . ? N1 Mg1 Na1 N5 86.30(7) . . . . ? N3 Mg1 Na1 N5 -90.60(7) . . . . ? N2 Mg1 N1 C1 -81.37(12) . . . . ? N3 Mg1 N1 C1 98.21(11) . . . . ? Na1 Mg1 N1 C1 95.61(11) . . . . ? N2 Mg1 N1 C5 54.31(11) . . . . ? N3 Mg1 N1 C5 -126.12(9) . . . . ? Na1 Mg1 N1 C5 -128.72(10) . . . . ? N2 Mg1 N1 Na1 -176.98(5) . . . . ? N3 Mg1 N1 Na1 2.60(5) . . . . ? N3 Na1 N1 C1 -126.06(9) . . . . ? N4 Na1 N1 C1 3.57(10) . . . . ? N5 Na1 N1 C1 99.77(9) . . . . ? Mg1 Na1 N1 C1 -124.01(10) . . . . ? N3 Na1 N1 C5 113.87(11) . . . . ? N4 Na1 N1 C5 -116.50(11) . . . . ? N5 Na1 N1 C5 -20.30(13) . . . . ? Mg1 Na1 N1 C5 115.92(12) . . . . ? N3 Na1 N1 Mg1 -2.05(4) . . . . ? N4 Na1 N1 Mg1 127.58(5) . . . . ? N5 Na1 N1 Mg1 -136.22(5) . . . . ? N1 Mg1 N2 C12 -148.79(11) . . . . ? N3 Mg1 N2 C12 31.70(14) . . . . ? Na1 Mg1 N2 C12 82.6(7) . . . . ? N1 Mg1 N2 C8 42.58(13) . . . . ? N3 Mg1 N2 C8 -136.93(10) . . . . ? Na1 Mg1 N2 C8 -86.0(7) . . . . ? N2 Mg1 N3 C15 -80.49(11) . . . . ? N1 Mg1 N3 C15 99.93(10) . . . . ? Na1 Mg1 N3 C15 102.65(10) . . . . ? N2 Mg1 N3 C19 52.09(11) . . . . ? N1 Mg1 N3 C19 -127.49(9) . . . . ? Na1 Mg1 N3 C19 -124.77(10) . . . . ? N2 Mg1 N3 Na1 176.86(5) . . . . ? N1 Mg1 N3 Na1 -2.72(5) . . . . ? N4 Na1 N3 C15 106.39(8) . . . . ? N1 Na1 N3 C15 -121.07(8) . . . . ? N5 Na1 N3 C15 11.75(10) . . . . ? Mg1 Na1 N3 C15 -123.10(9) . . . . ? N4 Na1 N3 C19 -14.96(11) . . . . ? N1 Na1 N3 C19 117.59(9) . . . . ? N5 Na1 N3 C19 -109.60(10) . . . . ? Mg1 Na1 N3 C19 115.56(10) . . . . ? N4 Na1 N3 Mg1 -130.52(5) . . . . ? N1 Na1 N3 Mg1 2.03(4) . . . . ? N5 Na1 N3 Mg1 134.84(5) . . . . ? N3 Na1 N4 C23 -31.68(11) . . . . ? N1 Na1 N4 C23 -141.77(10) . . . . ? N5 Na1 N4 C23 94.09(10) . . . . ? Mg1 Na1 N4 C23 -85.46(11) . . . . ? N3 Na1 N4 C24 -150.55(9) . . . . ? N1 Na1 N4 C24 99.37(10) . . . . ? N5 Na1 N4 C24 -24.78(9) . . . . ? Mg1 Na1 N4 C24 155.68(8) . . . . ? N3 Na1 N4 C22 91.69(11) . . . . ? N1 Na1 N4 C22 -18.40(13) . . . . ? N5 Na1 N4 C22 -142.54(12) . . . . ? Mg1 Na1 N4 C22 37.92(13) . . . . ? N3 Na1 N5 C26 -6.26(13) . . . . ? N4 Na1 N5 C26 -127.69(11) . . . . ? N1 Na1 N5 C26 106.82(11) . . . . ? Mg1 Na1 N5 C26 51.80(13) . . . . ? N3 Na1 N5 C27 -125.44(9) . . . . ? N4 Na1 N5 C27 113.13(9) . . . . ? N1 Na1 N5 C27 -12.36(11) . . . . ? Mg1 Na1 N5 C27 -67.39(11) . . . . ? N3 Na1 N5 C25 118.37(10) . . . . ? N4 Na1 N5 C25 -3.06(9) . . . . ? N1 Na1 N5 C25 -128.55(9) . . . . ? Mg1 Na1 N5 C25 176.42(8) . . . . ? C5 N1 C1 C7 -172.12(11) . . . . ? Mg1 N1 C1 C7 -34.03(16) . . . . ? Na1 N1 C1 C7 53.74(12) . . . . ? C5 N1 C1 C2 62.85(15) . . . . ? Mg1 N1 C1 C2 -159.06(11) . . . . ? Na1 N1 C1 C2 -71.29(13) . . . . ? N1 C1 C2 C3 -57.84(18) . . . . ? C7 C1 C2 C3 176.50(14) . . . . ? C1 C2 C3 C4 49.46(19) . . . . ? C2 C3 C4 C5 -48.20(18) . . . . ? C1 N1 C5 C6 173.93(11) . . . . ? Mg1 N1 C5 C6 31.12(13) . . . . ? Na1 N1 C5 C6 -70.06(14) . . . . ? C1 N1 C5 C4 -61.99(15) . . . . ? Mg1 N1 C5 C4 155.20(10) . . . . ? Na1 N1 C5 C4 54.03(16) . . . . ? C3 C4 C5 N1 55.41(17) . . . . ? C3 C4 C5 C6 -179.29(13) . . . . ? C12 N2 C8 C14 175.23(12) . . . . ? Mg1 N2 C8 C14 -14.41(17) . . . . ? C12 N2 C8 C9 -60.75(15) . . . . ? Mg1 N2 C8 C9 109.61(12) . . . . ? N2 C8 C9 C10 55.73(16) . . . . ? C14 C8 C9 C10 -179.23(12) . . . . ? C8 C9 C10 C11 -49.38(18) . . . . ? C9 C10 C11 C12 49.53(18) . . . . ? C8 N2 C12 C13 -174.09(13) . . . . ? Mg1 N2 C12 C13 15.86(18) . . . . ? C8 N2 C12 C11 61.67(15) . . . . ? Mg1 N2 C12 C11 -108.38(12) . . . . ? C10 C11 C12 N2 -56.80(16) . . . . ? C10 C11 C12 C13 178.55(13) . . . . ? C19 N3 C15 C21 -174.24(11) . . . . ? Mg1 N3 C15 C21 -39.59(14) . . . . ? Na1 N3 C15 C21 54.48(11) . . . . ? C19 N3 C15 C16 60.77(14) . . . . ? Mg1 N3 C15 C16 -164.59(9) . . . . ? Na1 N3 C15 C16 -70.51(11) . . . . ? N3 C15 C16 C17 -58.44(16) . . . . ? C21 C15 C16 C17 176.15(12) . . . . ? C15 C16 C17 C18 51.54(16) . . . . ? C16 C17 C18 C19 -50.82(17) . . . . ? C15 N3 C19 C20 177.08(12) . . . . ? Mg1 N3 C19 C20 37.53(14) . . . . ? Na1 N3 C19 C20 -64.13(14) . . . . ? C15 N3 C19 C18 -59.36(15) . . . . ? Mg1 N3 C19 C18 161.08(10) . . . . ? Na1 N3 C19 C18 59.43(14) . . . . ? C17 C18 C19 N3 55.95(16) . . . . ? C17 C18 C19 C20 -179.51(12) . . . . ? C23 N4 C24 C25 -63.37(17) . . . . ? C22 N4 C24 C25 178.29(13) . . . . ? Na1 N4 C24 C25 53.84(14) . . . . ? C26 N5 C25 C24 162.46(13) . . . . ? C27 N5 C25 C24 -78.97(16) . . . . ? Na1 N5 C25 C24 31.80(15) . . . . ? N4 C24 C25 N5 -63.00(18) . . . . ? _diffrn_measured_fraction_theta_max 0.911 _diffrn_reflns_theta_full 29.00 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.428 _refine_diff_density_min -0.183 _refine_diff_density_rms 0.041 #===END