# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Robert E. Mulvey' _publ_contact_author_address ; Department of Pure & Applied Chemistry University of Strathclyde 295 Cathedral Street Glasgow G1 1XL UNITED KINGDOM ; _publ_contact_author_email R.E.MULVEY@STRATH.AC.UK _publ_section_title ; Structurally-defined direct C-magnesiation and C-zincation of N-heterocyclic aromatic compounds using alkali-metal-mediated metallation ; _publ_contact_letter ; File altered as per the crystallographic referee's suggestions. This cif contains the supplementary data for the ms entitled Structurally-defined direct C-magnesiation and C-zincation of N-heterocyclic aromatic compounds using alkali-metal-mediated metallation by Conway, Hevia, Kennedy & Mulvey. If there are any problems with the file please contact me a.r.kennedy@strath.ac.uk 0141 552 2016 Yours, Alan Kennedy ; loop_ _publ_author_name 'R. E. Mulvey' 'Ben Conway' 'Eva Hevia' 'Alan R. Kennedy' data_grem225 _database_code_depnum_ccdc_archive 'CCDC 641398' ################################################################## ################ COMPOUND 2 ###################################### ################################################################# _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H64 Mg N8 Na2' _chemical_formula_weight 823.36 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/a loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x-1/2, -y-1/2, z' _cell_length_a 15.8300(3) _cell_length_b 16.8625(3) _cell_length_c 17.9095(4) _cell_angle_alpha 90.00 _cell_angle_beta 91.237(1) _cell_angle_gamma 90.00 _cell_volume 4779.53(16) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 9735 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 26.37 _exptl_crystal_description fragment _exptl_crystal_colour colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.144 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1768 _exptl_absorpt_coefficient_mu 0.096 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method 'omega and phi scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 90776 _diffrn_reflns_av_R_equivalents 0.084 _diffrn_reflns_av_sigmaI/netI 0.0549 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.66 _diffrn_reflns_theta_max 26.00 _reflns_number_total 9374 _reflns_number_gt 6015 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Denzo & Collect' _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^)+(0.0398P)^2^+2.3277P] 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 9374 _refine_ls_number_parameters 544 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0964 _refine_ls_R_factor_gt 0.0496 _refine_ls_wR_factor_ref 0.1161 _refine_ls_wR_factor_gt 0.0989 _refine_ls_goodness_of_fit_ref 1.015 _refine_ls_restrained_S_all 1.015 _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 0.62376(4) 0.98543(4) 0.80876(4) 0.02678(17) Uani 1 1 d . . . Na1 Na 0.72363(5) 1.14667(5) 0.75412(4) 0.0344(2) Uani 1 1 d . . . Na2 Na 0.53741(5) 0.83720(5) 0.71048(5) 0.0381(2) Uani 1 1 d . . . N1 N 0.82499(11) 0.99454(9) 0.77916(9) 0.0292(4) Uani 1 1 d . . . N2 N 0.66536(10) 1.11535(10) 0.94088(9) 0.0286(4) Uani 1 1 d . . . N3 N 0.71071(13) 1.23727(11) 0.64639(10) 0.0426(5) Uani 1 1 d . . . N4 N 0.83783(11) 1.23961(10) 0.77595(10) 0.0384(5) Uani 1 1 d . . . N5 N 0.42983(11) 0.99564(9) 0.74745(9) 0.0290(4) Uani 1 1 d . . . N6 N 0.57582(11) 0.82687(10) 0.90862(9) 0.0297(4) Uani 1 1 d . . . N7 N 0.55123(13) 0.76162(12) 0.59202(11) 0.0464(5) Uani 1 1 d . . . N8 N 0.41827(12) 0.74768(10) 0.71098(11) 0.0396(5) Uani 1 1 d . . . C1 C 0.74387(13) 0.99471(11) 0.74541(11) 0.0295(5) Uani 1 1 d . . . C2 C 0.75891(13) 1.00703(12) 0.67028(11) 0.0310(5) Uani 1 1 d . . . H2 H 0.7161 1.0105 0.6325 0.037 Uiso 1 1 calc R . . C3 C 0.84761(13) 1.01378(12) 0.65728(11) 0.0282(5) Uani 1 1 d . . . C4 C 0.89922(14) 1.02679(13) 0.59552(12) 0.0357(5) Uani 1 1 d . . . H4 H 0.8746 1.0327 0.5470 0.043 Uiso 1 1 calc R . . C5 C 0.98562(14) 1.03093(14) 0.60575(13) 0.0394(6) Uani 1 1 d . . . H5 H 1.0203 1.0403 0.5640 0.047 Uiso 1 1 calc R . . C6 C 1.02301(14) 1.02150(13) 0.67671(13) 0.0380(5) Uani 1 1 d . . . H6 H 1.0827 1.0244 0.6824 0.046 Uiso 1 1 calc R . . C7 C 0.97462(14) 1.00804(12) 0.73843(12) 0.0346(5) Uani 1 1 d . . . H7 H 1.0000 1.0011 0.7865 0.042 Uiso 1 1 calc R . . C8 C 0.88716(13) 1.00500(11) 0.72795(11) 0.0286(5) Uani 1 1 d . . . C9 C 0.84241(15) 0.98597(14) 0.85880(11) 0.0411(6) Uani 1 1 d . . . H9A H 0.8858 0.9453 0.8670 0.062 Uiso 1 1 calc R . . H9B H 0.7906 0.9702 0.8839 0.062 Uiso 1 1 calc R . . H9C H 0.8626 1.0366 0.8793 0.062 Uiso 1 1 calc R . . C10 C 0.62178(12) 1.09544(12) 0.87467(11) 0.0277(5) Uani 1 1 d . . . C11 C 0.59510(13) 1.16752(12) 0.84496(11) 0.0298(5) Uani 1 1 d . . . H11 H 0.5630 1.1734 0.7999 0.036 Uiso 1 1 calc R . . C12 C 0.62273(13) 1.23204(12) 0.89187(11) 0.0308(5) Uani 1 1 d . . . C13 C 0.61671(15) 1.31526(13) 0.89082(13) 0.0401(6) Uani 1 1 d . . . H13 H 0.5871 1.3415 0.8513 0.048 Uiso 1 1 calc R . . C14 C 0.65478(16) 1.35852(14) 0.94840(14) 0.0483(7) Uani 1 1 d . . . H14 H 0.6510 1.4147 0.9479 0.058 Uiso 1 1 calc R . . C15 C 0.69843(16) 1.32096(15) 1.00687(14) 0.0484(7) Uani 1 1 d . . . H15 H 0.7245 1.3521 1.0451 0.058 Uiso 1 1 calc R . . C16 C 0.70454(14) 1.23971(14) 1.01023(12) 0.0396(6) Uani 1 1 d . . . H16 H 0.7335 1.2142 1.0505 0.048 Uiso 1 1 calc R . . C17 C 0.66679(13) 1.19610(12) 0.95252(11) 0.0299(5) Uani 1 1 d . . . C18 C 0.70119(15) 1.05891(14) 0.99415(12) 0.0398(6) Uani 1 1 d . . . H18A H 0.7624 1.0672 0.9988 0.060 Uiso 1 1 calc R . . H18B H 0.6898 1.0048 0.9767 0.060 Uiso 1 1 calc R . . H18C H 0.6755 1.0667 1.0429 0.060 Uiso 1 1 calc R . . C19 C 0.70380(18) 1.19791(16) 0.57368(13) 0.0558(7) Uani 1 1 d . . . H19A H 0.7016 1.2379 0.5340 0.084 Uiso 1 1 calc R . . H19B H 0.6522 1.1659 0.5714 0.084 Uiso 1 1 calc R . . H19C H 0.7530 1.1636 0.5669 0.084 Uiso 1 1 calc R . . C20 C 0.6360(2) 1.28709(19) 0.65599(16) 0.0747(10) Uani 1 1 d . . . H20A H 0.6340 1.3279 0.6170 0.112 Uiso 1 1 calc R . . H20B H 0.6390 1.3125 0.7052 0.112 Uiso 1 1 calc R . . H20C H 0.5851 1.2542 0.6522 0.112 Uiso 1 1 calc R . . C21 C 0.78872(18) 1.28491(14) 0.65048(13) 0.0513(7) Uani 1 1 d . . . H21A H 0.7801 1.3339 0.6208 0.062 Uiso 1 1 calc R . . H21B H 0.8349 1.2545 0.6275 0.062 Uiso 1 1 calc R . . C22 C 0.81571(17) 1.30759(13) 0.72904(13) 0.0473(6) Uani 1 1 d . . . H22A H 0.8651 1.3435 0.7268 0.057 Uiso 1 1 calc R . . H22B H 0.7692 1.3372 0.7524 0.057 Uiso 1 1 calc R . . C23 C 0.85101(17) 1.26642(16) 0.85356(14) 0.0529(7) Uani 1 1 d . . . H23A H 0.8663 1.2210 0.8852 0.079 Uiso 1 1 calc R . . H23B H 0.7989 1.2905 0.8715 0.079 Uiso 1 1 calc R . . H23C H 0.8966 1.3057 0.8557 0.079 Uiso 1 1 calc R . . C24 C 0.91584(17) 1.20248(17) 0.75152(18) 0.0689(9) Uani 1 1 d . . . H24A H 0.9600 1.2429 0.7475 0.103 Uiso 1 1 calc R . . H24B H 0.9060 1.1775 0.7027 0.103 Uiso 1 1 calc R . . H24C H 0.9338 1.1622 0.7879 0.103 Uiso 1 1 calc R . . C25 C 0.51535(13) 0.99272(11) 0.72763(11) 0.0297(5) Uani 1 1 d . . . C26 C 0.51289(13) 0.98847(13) 0.65044(11) 0.0341(5) Uani 1 1 d . . . H26 H 0.5613 0.9858 0.6202 0.041 Uiso 1 1 calc R . . C27 C 0.42740(13) 0.98871(12) 0.62227(11) 0.0296(5) Uani 1 1 d . . . C28 C 0.38744(14) 0.98433(14) 0.55168(12) 0.0405(6) Uani 1 1 d . . . H28 H 0.4201 0.9814 0.5079 0.049 Uiso 1 1 calc R . . C29 C 0.30063(14) 0.98428(14) 0.54642(12) 0.0418(6) Uani 1 1 d . . . H29 H 0.2737 0.9815 0.4986 0.050 Uiso 1 1 calc R . . C30 C 0.25146(14) 0.98816(13) 0.60969(12) 0.0373(5) Uani 1 1 d . . . H30 H 0.1916 0.9876 0.6044 0.045 Uiso 1 1 calc R . . C31 C 0.28835(14) 0.99288(12) 0.68009(12) 0.0333(5) Uani 1 1 d . . . H31 H 0.2548 0.9958 0.7234 0.040 Uiso 1 1 calc R . . C32 C 0.37628(13) 0.99326(11) 0.68580(11) 0.0270(5) Uani 1 1 d . . . C33 C 0.40073(15) 0.99621(15) 0.82389(12) 0.0430(6) Uani 1 1 d . . . H33A H 0.3524 1.0321 0.8277 0.064 Uiso 1 1 calc R . . H33B H 0.4465 1.0143 0.8574 0.064 Uiso 1 1 calc R . . H33C H 0.3837 0.9425 0.8381 0.064 Uiso 1 1 calc R . . C34 C 0.62032(13) 0.86333(12) 0.85143(11) 0.0298(5) Uani 1 1 d . . . C35 C 0.65624(13) 0.80150(12) 0.81247(12) 0.0322(5) Uani 1 1 d . . . H35 H 0.6907 0.8078 0.7701 0.039 Uiso 1 1 calc R . . C36 C 0.63445(14) 0.72670(12) 0.84467(12) 0.0326(5) Uani 1 1 d . . . C37 C 0.65118(15) 0.64653(13) 0.82942(13) 0.0424(6) Uani 1 1 d . . . H37 H 0.6849 0.6323 0.7883 0.051 Uiso 1 1 calc R . . C38 C 0.61829(17) 0.58891(15) 0.87470(15) 0.0505(7) Uani 1 1 d . . . H38 H 0.6300 0.5347 0.8648 0.061 Uiso 1 1 calc R . . C39 C 0.56781(17) 0.60871(15) 0.93522(15) 0.0510(7) Uani 1 1 d . . . H39 H 0.5456 0.5676 0.9653 0.061 Uiso 1 1 calc R . . C40 C 0.54954(15) 0.68710(14) 0.95208(13) 0.0413(6) Uani 1 1 d . . . H40 H 0.5152 0.7005 0.9931 0.050 Uiso 1 1 calc R . . C41 C 0.58367(13) 0.74537(12) 0.90630(12) 0.0322(5) Uani 1 1 d . . . C42 C 0.53144(16) 0.86876(14) 0.96638(13) 0.0454(6) Uani 1 1 d . . . H42A H 0.4726 0.8509 0.9669 0.068 Uiso 1 1 calc R . . H42B H 0.5331 0.9259 0.9564 0.068 Uiso 1 1 calc R . . H42C H 0.5586 0.8579 1.0150 0.068 Uiso 1 1 calc R . . C43 C 0.5681(2) 0.81043(19) 0.52628(15) 0.0710(9) Uani 1 1 d . . . H43A H 0.5658 0.7772 0.4814 0.106 Uiso 1 1 calc R . . H43B H 0.6244 0.8344 0.5317 0.106 Uiso 1 1 calc R . . H43C H 0.5255 0.8524 0.5218 0.106 Uiso 1 1 calc R . . C44 C 0.6168(2) 0.7006(2) 0.59994(18) 0.0871(11) Uani 1 1 d . . . H44A H 0.6150 0.6659 0.5560 0.131 Uiso 1 1 calc R . . H44B H 0.6068 0.6690 0.6449 0.131 Uiso 1 1 calc R . . H44C H 0.6724 0.7259 0.6043 0.131 Uiso 1 1 calc R . . C45 C 0.46818(18) 0.72443(15) 0.58254(14) 0.0545(7) Uani 1 1 d . . . H45A H 0.4718 0.6823 0.5443 0.065 Uiso 1 1 calc R . . H45B H 0.4275 0.7647 0.5637 0.065 Uiso 1 1 calc R . . C46 C 0.43502(18) 0.68894(14) 0.65312(14) 0.0535(7) Uani 1 1 d . . . H46A H 0.3821 0.6599 0.6411 0.064 Uiso 1 1 calc R . . H46B H 0.4767 0.6501 0.6730 0.064 Uiso 1 1 calc R . . C47 C 0.34149(17) 0.79217(17) 0.69281(19) 0.0722(9) Uani 1 1 d . . . H47A H 0.2943 0.7552 0.6852 0.108 Uiso 1 1 calc R . . H47B H 0.3497 0.8228 0.6471 0.108 Uiso 1 1 calc R . . H47C H 0.3290 0.8283 0.7340 0.108 Uiso 1 1 calc R . . C48 C 0.40769(16) 0.70719(15) 0.78284(14) 0.0513(7) Uani 1 1 d . . . H48A H 0.3969 0.7465 0.8218 0.077 Uiso 1 1 calc R . . H48B H 0.4592 0.6776 0.7958 0.077 Uiso 1 1 calc R . . H48C H 0.3598 0.6704 0.7789 0.077 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 0.0268(4) 0.0286(4) 0.0251(4) 0.0005(3) 0.0021(3) -0.0024(3) Na1 0.0334(5) 0.0319(5) 0.0381(5) 0.0039(4) 0.0031(4) -0.0045(4) Na2 0.0377(5) 0.0382(5) 0.0384(5) -0.0063(4) 0.0001(4) -0.0082(4) N1 0.0294(10) 0.0305(10) 0.0280(9) 0.0041(8) 0.0050(8) 0.0033(8) N2 0.0260(10) 0.0356(10) 0.0243(9) 0.0001(8) -0.0001(7) 0.0011(8) N3 0.0543(14) 0.0400(11) 0.0335(11) 0.0003(9) 0.0012(9) 0.0114(10) N4 0.0315(11) 0.0337(10) 0.0498(12) 0.0015(9) 0.0007(9) -0.0022(8) N5 0.0315(10) 0.0298(10) 0.0257(9) -0.0003(7) 0.0025(8) 0.0011(8) N6 0.0272(10) 0.0328(10) 0.0293(10) 0.0051(8) 0.0029(8) 0.0004(8) N7 0.0472(13) 0.0503(12) 0.0417(12) -0.0076(10) 0.0009(10) 0.0089(10) N8 0.0317(11) 0.0302(10) 0.0568(13) -0.0009(9) 0.0019(9) -0.0024(8) C1 0.0285(12) 0.0256(11) 0.0344(12) -0.0003(9) 0.0023(9) 0.0011(9) C2 0.0268(12) 0.0362(12) 0.0301(11) 0.0004(9) -0.0012(9) -0.0008(9) C3 0.0298(12) 0.0264(11) 0.0286(11) -0.0011(9) 0.0025(9) -0.0006(9) C4 0.0342(14) 0.0441(13) 0.0290(12) 0.0000(10) 0.0042(10) -0.0017(10) C5 0.0339(14) 0.0469(14) 0.0381(13) -0.0021(11) 0.0141(11) -0.0046(11) C6 0.0257(12) 0.0406(13) 0.0478(14) -0.0051(11) 0.0039(11) 0.0014(10) C7 0.0311(13) 0.0379(13) 0.0348(12) 0.0008(10) 0.0004(10) 0.0045(10) C8 0.0308(12) 0.0239(11) 0.0312(11) 0.0015(9) 0.0052(9) 0.0028(9) C9 0.0435(15) 0.0497(14) 0.0302(12) 0.0070(11) 0.0039(10) 0.0036(11) C10 0.0195(11) 0.0385(12) 0.0252(11) -0.0016(9) 0.0022(9) -0.0005(9) C11 0.0269(12) 0.0376(12) 0.0249(11) -0.0007(9) -0.0014(9) 0.0015(9) C12 0.0268(12) 0.0352(12) 0.0306(12) -0.0011(10) 0.0027(9) -0.0008(9) C13 0.0393(14) 0.0356(13) 0.0454(14) 0.0005(11) 0.0024(11) 0.0021(11) C14 0.0509(16) 0.0325(13) 0.0617(17) -0.0110(12) 0.0067(14) -0.0031(12) C15 0.0459(16) 0.0523(16) 0.0470(15) -0.0193(13) -0.0005(13) -0.0083(12) C16 0.0358(14) 0.0509(15) 0.0322(12) -0.0085(11) -0.0004(10) -0.0027(11) C17 0.0225(12) 0.0384(13) 0.0291(11) -0.0039(10) 0.0039(9) -0.0020(9) C18 0.0406(14) 0.0504(14) 0.0284(12) 0.0039(10) 0.0022(10) 0.0083(11) C19 0.070(2) 0.0585(17) 0.0388(14) -0.0022(13) -0.0075(13) 0.0108(14) C20 0.086(2) 0.086(2) 0.0523(17) 0.0096(16) 0.0049(16) 0.0454(19) C21 0.081(2) 0.0356(14) 0.0380(14) 0.0066(11) 0.0104(13) -0.0067(13) C22 0.0659(18) 0.0316(13) 0.0448(14) 0.0022(11) 0.0083(13) -0.0053(12) C23 0.0461(16) 0.0593(17) 0.0530(16) 0.0034(13) -0.0071(13) -0.0090(13) C24 0.0385(17) 0.0567(18) 0.111(3) -0.0346(17) -0.0052(16) -0.0015(13) C25 0.0326(12) 0.0248(11) 0.0317(12) 0.0026(9) 0.0037(9) -0.0033(9) C26 0.0272(12) 0.0468(13) 0.0284(11) -0.0001(10) 0.0038(9) -0.0058(10) C27 0.0308(12) 0.0315(11) 0.0265(11) 0.0006(9) 0.0014(9) -0.0042(9) C28 0.0335(14) 0.0626(16) 0.0257(12) -0.0012(11) 0.0030(10) -0.0039(12) C29 0.0324(13) 0.0604(16) 0.0322(12) -0.0053(11) -0.0057(10) -0.0014(11) C30 0.0280(12) 0.0403(13) 0.0434(14) -0.0050(11) -0.0030(10) 0.0000(10) C31 0.0338(13) 0.0314(12) 0.0349(12) -0.0018(10) 0.0074(10) 0.0017(10) C32 0.0301(12) 0.0219(10) 0.0288(11) -0.0002(9) 0.0000(9) 0.0009(9) C33 0.0443(15) 0.0569(16) 0.0279(12) 0.0007(11) 0.0057(10) 0.0086(12) C34 0.0241(12) 0.0361(12) 0.0292(11) 0.0033(9) 0.0005(9) -0.0016(9) C35 0.0274(12) 0.0377(13) 0.0317(12) 0.0016(10) 0.0028(9) -0.0009(10) C36 0.0293(12) 0.0325(12) 0.0357(12) 0.0012(10) -0.0067(10) -0.0006(10) C37 0.0422(15) 0.0393(14) 0.0451(14) -0.0023(11) -0.0133(12) 0.0023(11) C38 0.0548(17) 0.0342(14) 0.0611(17) 0.0024(12) -0.0261(15) -0.0022(12) C39 0.0502(17) 0.0407(15) 0.0609(17) 0.0211(13) -0.0243(14) -0.0166(12) C40 0.0369(14) 0.0483(15) 0.0384(13) 0.0130(11) -0.0083(11) -0.0087(11) C41 0.0261(12) 0.0348(12) 0.0352(12) 0.0077(10) -0.0087(10) -0.0019(9) C42 0.0450(15) 0.0525(15) 0.0391(14) 0.0079(12) 0.0119(12) 0.0072(12) C43 0.080(2) 0.085(2) 0.0490(17) -0.0034(16) 0.0185(16) 0.0001(18) C44 0.078(2) 0.112(3) 0.072(2) -0.017(2) -0.0045(18) 0.048(2) C45 0.0685(19) 0.0461(15) 0.0483(16) -0.0119(13) -0.0141(14) -0.0016(14) C46 0.0629(18) 0.0351(14) 0.0620(17) -0.0055(13) -0.0097(14) -0.0078(12) C47 0.0431(17) 0.0558(18) 0.118(3) 0.0406(18) 0.0159(17) 0.0078(14) C48 0.0429(16) 0.0519(16) 0.0593(17) 0.0028(13) 0.0024(13) -0.0083(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mg1 C34 2.197(2) . ? Mg1 C10 2.199(2) . ? Mg1 C25 2.228(2) . ? Mg1 C1 2.241(2) . ? Mg1 Na1 3.3041(10) . ? Mg1 Na2 3.3331(10) . ? Na1 N4 2.418(2) . ? Na1 N3 2.466(2) . ? Na1 C1 2.587(2) . ? Na1 C11 2.656(2) . ? Na1 C2 2.854(2) . ? Na1 C10 2.856(2) . ? Na1 N1 3.0538(18) . ? Na1 C22 3.117(2) . ? Na2 N8 2.416(2) . ? Na2 N7 2.489(2) . ? Na2 C35 2.662(2) . ? Na2 C25 2.664(2) . ? Na2 C26 2.792(2) . ? Na2 C34 2.854(2) . ? N1 C8 1.371(3) . ? N1 C1 1.407(3) . ? N1 C9 1.454(3) . ? N2 C17 1.378(3) . ? N2 C10 1.400(2) . ? N2 C18 1.454(3) . ? N3 C20 1.463(3) . ? N3 C19 1.464(3) . ? N3 C21 1.474(3) . ? N4 C22 1.459(3) . ? N4 C24 1.460(3) . ? N4 C23 1.472(3) . ? N5 C32 1.378(3) . ? N5 C25 1.408(3) . ? N5 C33 1.454(3) . ? N6 C41 1.381(3) . ? N6 C34 1.398(3) . ? N6 C42 1.447(3) . ? N7 C45 1.463(3) . ? N7 C43 1.466(3) . ? N7 C44 1.466(3) . ? N8 C47 1.459(3) . ? N8 C46 1.462(3) . ? N8 C48 1.470(3) . ? C1 C2 1.387(3) . ? C2 C3 1.433(3) . ? C2 H2 0.9500 . ? C3 C4 1.406(3) . ? C3 C8 1.408(3) . ? C4 C5 1.378(3) . ? C4 H4 0.9500 . ? C5 C6 1.399(3) . ? C5 H5 0.9500 . ? C6 C7 1.377(3) . ? C6 H6 0.9500 . ? C7 C8 1.394(3) . ? C7 H7 0.9500 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C11 1.389(3) . ? C11 C12 1.437(3) . ? C11 H11 0.9500 . ? C12 C13 1.407(3) . ? C12 C17 1.414(3) . ? C13 C14 1.390(3) . ? C13 H13 0.9500 . ? C14 C15 1.394(3) . ? C14 H14 0.9500 . ? C15 C16 1.375(3) . ? C15 H15 0.9500 . ? C16 C17 1.393(3) . ? C16 H16 0.9500 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? 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 C22 1.511(3) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C26 1.384(3) . ? C26 C27 1.434(3) . ? C26 H26 0.9500 . ? C27 C28 1.403(3) . ? C27 C32 1.412(3) . ? C28 C29 1.375(3) . ? C28 H28 0.9500 . ? C29 C30 1.390(3) . ? C29 H29 0.9500 . ? C30 C31 1.380(3) . ? C30 H30 0.9500 . ? C31 C32 1.394(3) . ? C31 H31 0.9500 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 C35 1.384(3) . ? C35 C36 1.432(3) . ? C35 H35 0.9500 . ? C36 C37 1.405(3) . ? C36 C41 1.415(3) . ? C37 C38 1.375(3) . ? C37 H37 0.9500 . ? C38 C39 1.401(4) . ? C38 H38 0.9500 . ? C39 C40 1.388(3) . ? C39 H39 0.9500 . ? C40 C41 1.396(3) . ? C40 H40 0.9500 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 C46 1.503(4) . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C46 H46A 0.9900 . ? C46 H46B 0.9900 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 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 C34 Mg1 C10 127.08(8) . . ? C34 Mg1 C25 104.71(8) . . ? C10 Mg1 C25 106.49(8) . . ? C34 Mg1 C1 105.62(8) . . ? C10 Mg1 C1 103.58(8) . . ? C25 Mg1 C1 108.42(8) . . ? C34 Mg1 Na1 152.84(6) . . ? C10 Mg1 Na1 58.49(6) . . ? C25 Mg1 Na1 97.36(6) . . ? C1 Mg1 Na1 51.37(5) . . ? C34 Mg1 Na2 57.86(6) . . ? C10 Mg1 Na2 154.89(6) . . ? C25 Mg1 Na2 52.82(5) . . ? C1 Mg1 Na2 97.34(6) . . ? Na1 Mg1 Na2 130.85(3) . . ? N4 Na1 N3 76.94(7) . . ? N4 Na1 C1 123.95(7) . . ? N3 Na1 C1 125.07(7) . . ? N4 Na1 C11 113.27(7) . . ? N3 Na1 C11 110.22(7) . . ? C1 Na1 C11 105.40(7) . . ? N4 Na1 C2 117.75(7) . . ? N3 Na1 C2 96.51(6) . . ? C1 Na1 C2 29.01(6) . . ? C11 Na1 C2 126.35(7) . . ? N4 Na1 C10 120.40(7) . . ? N3 Na1 C10 137.75(7) . . ? C1 Na1 C10 79.55(7) . . ? C11 Na1 C10 28.90(6) . . ? C2 Na1 C10 105.56(6) . . ? N4 Na1 N1 97.59(6) . . ? N3 Na1 N1 132.05(6) . . ? C1 Na1 N1 27.33(6) . . ? C11 Na1 N1 115.36(6) . . ? C2 Na1 N1 43.62(5) . . ? C10 Na1 N1 86.46(6) . . ? N4 Na1 C22 26.98(6) . . ? N3 Na1 C22 51.62(7) . . ? C1 Na1 C22 142.61(8) . . ? C11 Na1 C22 109.86(7) . . ? C2 Na1 C22 123.02(7) . . ? C10 Na1 C22 130.20(7) . . ? N1 Na1 C22 120.43(7) . . ? N4 Na1 Mg1 147.81(5) . . ? N3 Na1 Mg1 135.19(6) . . ? C1 Na1 Mg1 42.57(5) . . ? C11 Na1 Mg1 63.24(5) . . ? C2 Na1 Mg1 64.99(5) . . ? C10 Na1 Mg1 41.03(4) . . ? N1 Na1 Mg1 61.21(4) . . ? C22 Na1 Mg1 170.82(5) . . ? N8 Na2 N7 76.47(7) . . ? N8 Na2 C35 113.34(7) . . ? N7 Na2 C35 113.28(7) . . ? N8 Na2 C25 120.68(7) . . ? N7 Na2 C25 128.06(7) . . ? C35 Na2 C25 103.65(7) . . ? N8 Na2 C26 118.05(7) . . ? N7 Na2 C26 98.83(7) . . ? C35 Na2 C26 124.13(7) . . ? C25 Na2 C26 29.27(6) . . ? N8 Na2 C34 115.93(7) . . ? N7 Na2 C34 141.80(7) . . ? C35 Na2 C34 28.78(6) . . ? C25 Na2 C34 78.76(6) . . ? C26 Na2 C34 104.90(6) . . ? N8 Na2 Mg1 141.07(6) . . ? N7 Na2 Mg1 142.34(6) . . ? C35 Na2 Mg1 62.07(5) . . ? C25 Na2 Mg1 41.78(5) . . ? C26 Na2 Mg1 64.56(5) . . ? C34 Na2 Mg1 40.68(4) . . ? C8 N1 C1 111.96(17) . . ? C8 N1 C9 123.05(18) . . ? C1 N1 C9 124.98(17) . . ? C8 N1 Na1 100.14(11) . . ? C1 N1 Na1 57.55(10) . . ? C9 N1 Na1 108.39(12) . . ? C17 N2 C10 111.80(16) . . ? C17 N2 C18 122.87(17) . . ? C10 N2 C18 125.24(17) . . ? C20 N3 C19 108.7(2) . . ? C20 N3 C21 111.1(2) . . ? C19 N3 C21 109.8(2) . . ? C20 N3 Na1 108.50(15) . . ? C19 N3 Na1 114.74(14) . . ? C21 N3 Na1 104.10(13) . . ? C22 N4 C24 111.0(2) . . ? C22 N4 C23 109.25(18) . . ? C24 N4 C23 108.1(2) . . ? C22 N4 Na1 104.28(14) . . ? C24 N4 Na1 107.93(14) . . ? C23 N4 Na1 116.23(14) . . ? C32 N5 C25 112.04(16) . . ? C32 N5 C33 123.56(18) . . ? C25 N5 C33 124.30(17) . . ? C41 N6 C34 111.64(17) . . ? C41 N6 C42 123.55(18) . . ? C34 N6 C42 124.70(18) . . ? C45 N7 C43 109.1(2) . . ? C45 N7 C44 110.0(2) . . ? C43 N7 C44 109.3(2) . . ? C45 N7 Na2 102.89(14) . . ? C43 N7 Na2 114.71(16) . . ? C44 N7 Na2 110.62(16) . . ? C47 N8 C46 110.7(2) . . ? C47 N8 C48 108.9(2) . . ? C46 N8 C48 109.37(19) . . ? C47 N8 Na2 108.93(15) . . ? C46 N8 Na2 105.50(14) . . ? C48 N8 Na2 113.41(14) . . ? C2 C1 N1 104.05(17) . . ? C2 C1 Mg1 131.83(16) . . ? N1 C1 Mg1 123.97(14) . . ? C2 C1 Na1 86.23(12) . . ? N1 C1 Na1 95.12(12) . . ? Mg1 C1 Na1 86.05(7) . . ? C1 C2 C3 111.03(19) . . ? C1 C2 Na1 64.76(11) . . ? C3 C2 Na1 102.92(13) . . ? C1 C2 H2 124.5 . . ? C3 C2 H2 124.5 . . ? Na1 C2 H2 100.3 . . ? C4 C3 C8 117.96(19) . . ? C4 C3 C2 136.7(2) . . ? C8 C3 C2 105.31(18) . . ? C5 C4 C3 119.7(2) . . ? C5 C4 H4 120.2 . . ? C3 C4 H4 120.2 . . ? C4 C5 C6 120.9(2) . . ? C4 C5 H5 119.5 . . ? C6 C5 H5 119.5 . . ? C7 C6 C5 121.1(2) . . ? C7 C6 H6 119.5 . . ? C5 C6 H6 119.5 . . ? C6 C7 C8 117.8(2) . . ? C6 C7 H7 121.1 . . ? C8 C7 H7 121.1 . . ? N1 C8 C7 129.78(19) . . ? N1 C8 C3 107.65(18) . . ? C7 C8 C3 122.57(19) . . ? N1 C9 H9A 109.5 . . ? N1 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? N1 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C11 C10 N2 104.77(17) . . ? C11 C10 Mg1 122.70(14) . . ? N2 C10 Mg1 130.13(14) . . ? C11 C10 Na1 67.52(11) . . ? N2 C10 Na1 106.98(12) . . ? Mg1 C10 Na1 80.48(6) . . ? C10 C11 C12 110.63(18) . . ? C10 C11 Na1 83.58(12) . . ? C12 C11 Na1 103.35(13) . . ? C10 C11 H11 124.7 . . ? C12 C11 H11 124.7 . . ? Na1 C11 H11 84.0 . . ? C13 C12 C17 118.0(2) . . ? C13 C12 C11 136.7(2) . . ? C17 C12 C11 105.27(18) . . ? C14 C13 C12 119.0(2) . . ? C14 C13 H13 120.5 . . ? C12 C13 H13 120.5 . . ? C13 C14 C15 121.3(2) . . ? C13 C14 H14 119.4 . . ? C15 C14 H14 119.4 . . ? C16 C15 C14 121.2(2) . . ? C16 C15 H15 119.4 . . ? C14 C15 H15 119.4 . . ? C15 C16 C17 117.7(2) . . ? C15 C16 H16 121.1 . . ? C17 C16 H16 121.1 . . ? N2 C17 C16 129.8(2) . . ? N2 C17 C12 107.52(17) . . ? C16 C17 C12 122.7(2) . . ? N2 C18 H18A 109.5 . . ? N2 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? N2 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N3 C19 H19A 109.5 . . ? N3 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? N3 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? N3 C20 H20A 109.5 . . ? N3 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? N3 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? N3 C21 C22 113.8(2) . . ? N3 C21 H21A 108.8 . . ? C22 C21 H21A 108.8 . . ? N3 C21 H21B 108.8 . . ? C22 C21 H21B 108.8 . . ? H21A C21 H21B 107.7 . . ? N4 C22 C21 113.38(19) . . ? N4 C22 Na1 48.74(10) . . ? C21 C22 Na1 77.89(13) . . ? N4 C22 H22A 108.9 . . ? C21 C22 H22A 108.9 . . ? Na1 C22 H22A 155.5 . . ? N4 C22 H22B 108.9 . . ? C21 C22 H22B 108.9 . . ? Na1 C22 H22B 91.4 . . ? H22A C22 H22B 107.7 . . ? 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 H24A 109.5 . . ? N4 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? N4 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C26 C25 N5 104.31(17) . . ? C26 C25 Mg1 130.79(16) . . ? N5 C25 Mg1 124.67(14) . . ? C26 C25 Na2 80.49(13) . . ? N5 C25 Na2 101.11(12) . . ? Mg1 C25 Na2 85.40(7) . . ? C25 C26 C27 110.93(19) . . ? C25 C26 Na2 70.24(12) . . ? C27 C26 Na2 105.09(13) . . ? C25 C26 H26 124.5 . . ? C27 C26 H26 124.5 . . ? Na2 C26 H26 93.9 . . ? C28 C27 C32 118.27(19) . . ? C28 C27 C26 136.1(2) . . ? C32 C27 C26 105.64(17) . . ? C29 C28 C27 119.5(2) . . ? C29 C28 H28 120.3 . . ? C27 C28 H28 120.3 . . ? C28 C29 C30 121.4(2) . . ? C28 C29 H29 119.3 . . ? C30 C29 H29 119.3 . . ? C31 C30 C29 120.9(2) . . ? C31 C30 H30 119.5 . . ? C29 C30 H30 119.5 . . ? C30 C31 C32 118.0(2) . . ? C30 C31 H31 121.0 . . ? C32 C31 H31 121.0 . . ? N5 C32 C31 130.93(19) . . ? N5 C32 C27 107.09(18) . . ? C31 C32 C27 121.97(18) . . ? N5 C33 H33A 109.5 . . ? N5 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? N5 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C35 C34 N6 104.90(18) . . ? C35 C34 Mg1 121.15(15) . . ? N6 C34 Mg1 133.12(15) . . ? C35 C34 Na2 67.90(12) . . ? N6 C34 Na2 110.54(13) . . ? Mg1 C34 Na2 81.46(6) . . ? C34 C35 C36 110.83(19) . . ? C34 C35 Na2 83.31(13) . . ? C36 C35 Na2 107.62(13) . . ? C34 C35 H35 124.6 . . ? C36 C35 H35 124.6 . . ? Na2 C35 H35 80.6 . . ? C37 C36 C41 118.6(2) . . ? C37 C36 C35 136.1(2) . . ? C41 C36 C35 105.30(18) . . ? C38 C37 C36 119.3(2) . . ? C38 C37 H37 120.3 . . ? C36 C37 H37 120.3 . . ? C37 C38 C39 121.2(2) . . ? C37 C38 H38 119.4 . . ? C39 C38 H38 119.4 . . ? C40 C39 C38 121.4(2) . . ? C40 C39 H39 119.3 . . ? C38 C39 H39 119.3 . . ? C39 C40 C41 117.2(2) . . ? C39 C40 H40 121.4 . . ? C41 C40 H40 121.4 . . ? N6 C41 C40 130.3(2) . . ? N6 C41 C36 107.33(18) . . ? C40 C41 C36 122.3(2) . . ? N6 C42 H42A 109.5 . . ? N6 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? N6 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? N7 C43 H43A 109.5 . . ? N7 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? N7 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? N7 C44 H44A 109.5 . . ? N7 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? N7 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? N7 C45 C46 113.7(2) . . ? N7 C45 H45A 108.8 . . ? C46 C45 H45A 108.8 . . ? N7 C45 H45B 108.8 . . ? C46 C45 H45B 108.8 . . ? H45A C45 H45B 107.7 . . ? N8 C46 C45 113.5(2) . . ? N8 C46 H46A 108.9 . . ? C45 C46 H46A 108.9 . . ? N8 C46 H46B 108.9 . . ? C45 C46 H46B 108.9 . . ? H46A C46 H46B 107.7 . . ? N8 C47 H47A 109.5 . . ? N8 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? N8 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? N8 C48 H48A 109.5 . . ? N8 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? N8 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 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 C34 Mg1 Na1 N4 -43.00(18) . . . . ? C10 Mg1 Na1 N4 67.76(12) . . . . ? C25 Mg1 Na1 N4 172.62(11) . . . . ? C1 Mg1 Na1 N4 -79.65(12) . . . . ? Na2 Mg1 Na1 N4 -141.32(10) . . . . ? C34 Mg1 Na1 N3 132.93(14) . . . . ? C10 Mg1 Na1 N3 -116.31(10) . . . . ? C25 Mg1 Na1 N3 -11.45(10) . . . . ? C1 Mg1 Na1 N3 96.28(10) . . . . ? Na2 Mg1 Na1 N3 34.61(9) . . . . ? C34 Mg1 Na1 C1 36.65(15) . . . . ? C10 Mg1 Na1 C1 147.41(10) . . . . ? C25 Mg1 Na1 C1 -107.73(9) . . . . ? Na2 Mg1 Na1 C1 -61.67(8) . . . . ? C34 Mg1 Na1 C11 -134.68(14) . . . . ? C10 Mg1 Na1 C11 -23.93(8) . . . . ? C25 Mg1 Na1 C11 80.93(8) . . . . ? C1 Mg1 Na1 C11 -171.33(9) . . . . ? Na2 Mg1 Na1 C11 127.00(6) . . . . ? C34 Mg1 Na1 C2 59.92(14) . . . . ? C10 Mg1 Na1 C2 170.68(8) . . . . ? C25 Mg1 Na1 C2 -84.47(7) . . . . ? C1 Mg1 Na1 C2 23.27(8) . . . . ? Na2 Mg1 Na1 C2 -38.40(6) . . . . ? C34 Mg1 Na1 C10 -110.76(15) . . . . ? C25 Mg1 Na1 C10 104.86(9) . . . . ? C1 Mg1 Na1 C10 -147.41(10) . . . . ? Na2 Mg1 Na1 C10 150.92(7) . . . . ? C34 Mg1 Na1 N1 10.84(14) . . . . ? C10 Mg1 Na1 N1 121.60(7) . . . . ? C25 Mg1 Na1 N1 -133.54(7) . . . . ? C1 Mg1 Na1 N1 -25.80(8) . . . . ? Na2 Mg1 Na1 N1 -87.47(5) . . . . ? C34 Mg1 Na1 C22 -92.0(4) . . . . ? C10 Mg1 Na1 C22 18.7(4) . . . . ? C25 Mg1 Na1 C22 123.6(4) . . . . ? C1 Mg1 Na1 C22 -128.7(4) . . . . ? Na2 Mg1 Na1 C22 169.6(4) . . . . ? C34 Mg1 Na2 N8 68.13(11) . . . . ? C10 Mg1 Na2 N8 -41.59(18) . . . . ? C25 Mg1 Na2 N8 -80.41(11) . . . . ? C1 Mg1 Na2 N8 172.00(10) . . . . ? Na1 Mg1 Na2 N8 -144.10(8) . . . . ? C34 Mg1 Na2 N7 -117.77(11) . . . . ? C10 Mg1 Na2 N7 132.51(16) . . . . ? C25 Mg1 Na2 N7 93.69(11) . . . . ? C1 Mg1 Na2 N7 -13.89(11) . . . . ? Na1 Mg1 Na2 N7 30.00(11) . . . . ? C34 Mg1 Na2 C35 -25.16(8) . . . . ? C10 Mg1 Na2 C35 -134.88(15) . . . . ? C25 Mg1 Na2 C35 -173.71(9) . . . . ? C1 Mg1 Na2 C35 78.71(8) . . . . ? Na1 Mg1 Na2 C35 122.61(6) . . . . ? C34 Mg1 Na2 C25 148.54(10) . . . . ? C10 Mg1 Na2 C25 38.82(15) . . . . ? C1 Mg1 Na2 C25 -107.59(9) . . . . ? Na1 Mg1 Na2 C25 -63.69(7) . . . . ? C34 Mg1 Na2 C26 171.99(8) . . . . ? C10 Mg1 Na2 C26 62.27(15) . . . . ? C25 Mg1 Na2 C26 23.45(8) . . . . ? C1 Mg1 Na2 C26 -84.13(7) . . . . ? Na1 Mg1 Na2 C26 -40.24(6) . . . . ? C10 Mg1 Na2 C34 -109.72(15) . . . . ? C25 Mg1 Na2 C34 -148.54(10) . . . . ? C1 Mg1 Na2 C34 103.87(9) . . . . ? Na1 Mg1 Na2 C34 147.77(8) . . . . ? N4 Na1 N1 C8 -56.16(13) . . . . ? N3 Na1 N1 C8 23.08(16) . . . . ? C1 Na1 N1 C8 109.66(17) . . . . ? C11 Na1 N1 C8 -176.44(12) . . . . ? C2 Na1 N1 C8 66.60(13) . . . . ? C10 Na1 N1 C8 -176.37(13) . . . . ? C22 Na1 N1 C8 -40.83(14) . . . . ? Mg1 Na1 N1 C8 149.56(13) . . . . ? N4 Na1 N1 C1 -165.81(13) . . . . ? N3 Na1 N1 C1 -86.57(14) . . . . ? C11 Na1 N1 C1 73.91(13) . . . . ? C2 Na1 N1 C1 -43.05(12) . . . . ? C10 Na1 N1 C1 73.97(12) . . . . ? C22 Na1 N1 C1 -150.49(12) . . . . ? Mg1 Na1 N1 C1 39.90(11) . . . . ? N4 Na1 N1 C9 73.88(14) . . . . ? N3 Na1 N1 C9 153.12(14) . . . . ? C1 Na1 N1 C9 -120.31(19) . . . . ? C11 Na1 N1 C9 -46.40(15) . . . . ? C2 Na1 N1 C9 -163.36(16) . . . . ? C10 Na1 N1 C9 -46.33(14) . . . . ? C22 Na1 N1 C9 89.21(14) . . . . ? Mg1 Na1 N1 C9 -80.40(13) . . . . ? N4 Na1 N3 C20 -107.87(19) . . . . ? C1 Na1 N3 C20 129.60(18) . . . . ? C11 Na1 N3 C20 2.4(2) . . . . ? C2 Na1 N3 C20 135.08(18) . . . . ? C10 Na1 N3 C20 13.3(2) . . . . ? N1 Na1 N3 C20 163.65(17) . . . . ? C22 Na1 N3 C20 -97.38(19) . . . . ? Mg1 Na1 N3 C20 74.35(19) . . . . ? N4 Na1 N3 C19 130.42(18) . . . . ? C1 Na1 N3 C19 7.9(2) . . . . ? C11 Na1 N3 C19 -119.29(17) . . . . ? C2 Na1 N3 C19 13.38(18) . . . . ? C10 Na1 N3 C19 -108.43(18) . . . . ? N1 Na1 N3 C19 41.9(2) . . . . ? C22 Na1 N3 C19 140.9(2) . . . . ? Mg1 Na1 N3 C19 -47.4(2) . . . . ? N4 Na1 N3 C21 10.46(14) . . . . ? C1 Na1 N3 C21 -112.07(15) . . . . ? C11 Na1 N3 C21 120.75(14) . . . . ? C2 Na1 N3 C21 -106.59(14) . . . . ? C10 Na1 N3 C21 131.61(14) . . . . ? N1 Na1 N3 C21 -78.02(16) . . . . ? C22 Na1 N3 C21 20.95(13) . . . . ? Mg1 Na1 N3 C21 -167.32(12) . . . . ? N3 Na1 N4 C22 18.34(14) . . . . ? C1 Na1 N4 C22 142.05(14) . . . . ? C11 Na1 N4 C22 -88.31(15) . . . . ? C2 Na1 N4 C22 108.88(14) . . . . ? C10 Na1 N4 C22 -119.81(14) . . . . ? N1 Na1 N4 C22 149.85(14) . . . . ? Mg1 Na1 N4 C22 -164.60(12) . . . . ? N3 Na1 N4 C24 -99.75(18) . . . . ? C1 Na1 N4 C24 24.0(2) . . . . ? C11 Na1 N4 C24 153.60(17) . . . . ? C2 Na1 N4 C24 -9.21(19) . . . . ? C10 Na1 N4 C24 122.09(18) . . . . ? N1 Na1 N4 C24 31.75(18) . . . . ? C22 Na1 N4 C24 -118.1(2) . . . . ? Mg1 Na1 N4 C24 77.3(2) . . . . ? N3 Na1 N4 C23 138.65(17) . . . . ? C1 Na1 N4 C23 -97.64(17) . . . . ? C11 Na1 N4 C23 32.00(17) . . . . ? C2 Na1 N4 C23 -130.81(16) . . . . ? C10 Na1 N4 C23 0.50(18) . . . . ? N1 Na1 N4 C23 -89.85(16) . . . . ? C22 Na1 N4 C23 120.3(2) . . . . ? Mg1 Na1 N4 C23 -44.3(2) . . . . ? N8 Na2 N7 C45 15.16(14) . . . . ? C35 Na2 N7 C45 125.05(15) . . . . ? C25 Na2 N7 C45 -103.41(16) . . . . ? C26 Na2 N7 C45 -101.71(15) . . . . ? C34 Na2 N7 C45 130.10(15) . . . . ? Mg1 Na2 N7 C45 -161.03(13) . . . . ? N8 Na2 N7 C43 133.47(19) . . . . ? C35 Na2 N7 C43 -116.65(18) . . . . ? C25 Na2 N7 C43 14.9(2) . . . . ? C26 Na2 N7 C43 16.59(19) . . . . ? C34 Na2 N7 C43 -111.60(19) . . . . ? Mg1 Na2 N7 C43 -42.7(2) . . . . ? N8 Na2 N7 C44 -102.3(2) . . . . ? C35 Na2 N7 C44 7.6(2) . . . . ? C25 Na2 N7 C44 139.1(2) . . . . ? C26 Na2 N7 C44 140.8(2) . . . . ? C34 Na2 N7 C44 12.6(3) . . . . ? Mg1 Na2 N7 C44 81.5(2) . . . . ? N7 Na2 N8 C47 -104.95(18) . . . . ? C35 Na2 N8 C47 145.24(18) . . . . ? C25 Na2 N8 C47 21.5(2) . . . . ? C26 Na2 N8 C47 -12.0(2) . . . . ? C34 Na2 N8 C47 113.62(18) . . . . ? Mg1 Na2 N8 C47 71.3(2) . . . . ? N7 Na2 N8 C46 13.92(14) . . . . ? C35 Na2 N8 C46 -95.90(15) . . . . ? C25 Na2 N8 C46 140.40(14) . . . . ? C26 Na2 N8 C46 106.83(15) . . . . ? C34 Na2 N8 C46 -127.51(14) . . . . ? Mg1 Na2 N8 C46 -169.78(12) . . . . ? N7 Na2 N8 C48 133.60(16) . . . . ? C35 Na2 N8 C48 23.79(17) . . . . ? C25 Na2 N8 C48 -99.92(16) . . . . ? C26 Na2 N8 C48 -133.49(15) . . . . ? C34 Na2 N8 C48 -7.83(18) . . . . ? Mg1 Na2 N8 C48 -50.10(19) . . . . ? C8 N1 C1 C2 -0.8(2) . . . . ? C9 N1 C1 C2 178.04(18) . . . . ? Na1 N1 C1 C2 87.38(14) . . . . ? C8 N1 C1 Mg1 -176.89(13) . . . . ? C9 N1 C1 Mg1 2.0(3) . . . . ? Na1 N1 C1 Mg1 -88.69(13) . . . . ? C8 N1 C1 Na1 -88.21(15) . . . . ? C9 N1 C1 Na1 90.65(19) . . . . ? C34 Mg1 C1 C2 115.07(19) . . . . ? C10 Mg1 C1 C2 -109.55(19) . . . . ? C25 Mg1 C1 C2 3.3(2) . . . . ? Na1 Mg1 C1 C2 -81.36(19) . . . . ? Na2 Mg1 C1 C2 56.47(19) . . . . ? C34 Mg1 C1 N1 -70.05(17) . . . . ? C10 Mg1 C1 N1 65.33(17) . . . . ? C25 Mg1 C1 N1 178.17(15) . . . . ? Na1 Mg1 C1 N1 93.52(16) . . . . ? Na2 Mg1 C1 N1 -128.65(15) . . . . ? C34 Mg1 C1 Na1 -163.57(7) . . . . ? C10 Mg1 C1 Na1 -28.19(8) . . . . ? C25 Mg1 C1 Na1 84.65(8) . . . . ? Na2 Mg1 C1 Na1 137.83(5) . . . . ? N4 Na1 C1 C2 -86.76(14) . . . . ? N3 Na1 C1 C2 11.29(16) . . . . ? C11 Na1 C1 C2 140.44(13) . . . . ? C10 Na1 C1 C2 153.50(13) . . . . ? N1 Na1 C1 C2 -103.79(17) . . . . ? C22 Na1 C1 C2 -59.41(18) . . . . ? Mg1 Na1 C1 C2 132.42(15) . . . . ? N4 Na1 C1 N1 17.03(15) . . . . ? N3 Na1 C1 N1 115.08(13) . . . . ? C11 Na1 C1 N1 -115.77(12) . . . . ? C2 Na1 C1 N1 103.79(17) . . . . ? C10 Na1 C1 N1 -102.72(12) . . . . ? C22 Na1 C1 N1 44.38(18) . . . . ? Mg1 Na1 C1 N1 -123.79(14) . . . . ? N4 Na1 C1 Mg1 140.82(7) . . . . ? N3 Na1 C1 Mg1 -121.13(8) . . . . ? C11 Na1 C1 Mg1 8.02(8) . . . . ? C2 Na1 C1 Mg1 -132.42(15) . . . . ? C10 Na1 C1 Mg1 21.08(6) . . . . ? N1 Na1 C1 Mg1 123.79(14) . . . . ? C22 Na1 C1 Mg1 168.17(9) . . . . ? N1 C1 C2 C3 0.5(2) . . . . ? Mg1 C1 C2 C3 176.08(14) . . . . ? Na1 C1 C2 C3 94.79(15) . . . . ? N1 C1 C2 Na1 -94.34(13) . . . . ? Mg1 C1 C2 Na1 81.28(16) . . . . ? N4 Na1 C2 C1 110.63(13) . . . . ? N3 Na1 C2 C1 -170.72(13) . . . . ? C11 Na1 C2 C1 -49.67(15) . . . . ? C10 Na1 C2 C1 -27.10(14) . . . . ? N1 Na1 C2 C1 40.26(12) . . . . ? C22 Na1 C2 C1 141.43(13) . . . . ? Mg1 Na1 C2 C1 -33.44(11) . . . . ? N4 Na1 C2 C3 3.24(15) . . . . ? N3 Na1 C2 C3 81.89(14) . . . . ? C1 Na1 C2 C3 -107.39(19) . . . . ? C11 Na1 C2 C3 -157.06(12) . . . . ? C10 Na1 C2 C3 -134.49(13) . . . . ? N1 Na1 C2 C3 -67.13(13) . . . . ? C22 Na1 C2 C3 34.04(16) . . . . ? Mg1 Na1 C2 C3 -140.83(14) . . . . ? C1 C2 C3 C4 -179.2(2) . . . . ? Na1 C2 C3 C4 -111.6(2) . . . . ? C1 C2 C3 C8 0.0(2) . . . . ? Na1 C2 C3 C8 67.68(16) . . . . ? C8 C3 C4 C5 -0.3(3) . . . . ? C2 C3 C4 C5 178.9(2) . . . . ? C3 C4 C5 C6 0.7(3) . . . . ? C4 C5 C6 C7 -0.2(3) . . . . ? C5 C6 C7 C8 -0.7(3) . . . . ? C1 N1 C8 C7 -179.7(2) . . . . ? C9 N1 C8 C7 1.4(3) . . . . ? Na1 N1 C8 C7 121.3(2) . . . . ? C1 N1 C8 C3 0.9(2) . . . . ? C9 N1 C8 C3 -178.00(18) . . . . ? Na1 N1 C8 C3 -58.09(16) . . . . ? C6 C7 C8 N1 -178.3(2) . . . . ? C6 C7 C8 C3 1.1(3) . . . . ? C4 C3 C8 N1 178.88(17) . . . . ? C2 C3 C8 N1 -0.6(2) . . . . ? C4 C3 C8 C7 -0.6(3) . . . . ? C2 C3 C8 C7 179.99(19) . . . . ? C17 N2 C10 C11 -0.4(2) . . . . ? C18 N2 C10 C11 176.31(18) . . . . ? C17 N2 C10 Mg1 161.99(15) . . . . ? C18 N2 C10 Mg1 -21.3(3) . . . . ? C17 N2 C10 Na1 70.20(17) . . . . ? C18 N2 C10 Na1 -113.13(18) . . . . ? C34 Mg1 C10 C11 -156.98(16) . . . . ? C25 Mg1 C10 C11 -33.22(19) . . . . ? C1 Mg1 C10 C11 81.02(18) . . . . ? Na1 Mg1 C10 C11 55.37(15) . . . . ? Na2 Mg1 C10 C11 -64.6(2) . . . . ? C34 Mg1 C10 N2 43.4(2) . . . . ? C25 Mg1 C10 N2 167.18(17) . . . . ? C1 Mg1 C10 N2 -78.58(18) . . . . ? Na1 Mg1 C10 N2 -104.23(18) . . . . ? Na2 Mg1 C10 N2 135.79(15) . . . . ? C34 Mg1 C10 Na1 147.66(8) . . . . ? C25 Mg1 C10 Na1 -88.58(7) . . . . ? C1 Mg1 C10 Na1 25.65(7) . . . . ? Na2 Mg1 C10 Na1 -119.98(12) . . . . ? N4 Na1 C10 C11 83.40(13) . . . . ? N3 Na1 C10 C11 -21.45(17) . . . . ? C1 Na1 C10 C11 -153.22(13) . . . . ? C2 Na1 C10 C11 -140.24(12) . . . . ? N1 Na1 C10 C11 -179.87(12) . . . . ? C22 Na1 C10 C11 52.37(15) . . . . ? Mg1 Na1 C10 C11 -131.47(14) . . . . ? N4 Na1 C10 N2 -15.93(16) . . . . ? N3 Na1 C10 N2 -120.78(14) . . . . ? C1 Na1 C10 N2 107.45(14) . . . . ? C11 Na1 C10 N2 -99.33(18) . . . . ? C2 Na1 C10 N2 120.43(13) . . . . ? N1 Na1 C10 N2 80.79(13) . . . . ? C22 Na1 C10 N2 -46.96(16) . . . . ? Mg1 Na1 C10 N2 129.20(15) . . . . ? N4 Na1 C10 Mg1 -145.13(7) . . . . ? N3 Na1 C10 Mg1 110.01(10) . . . . ? C1 Na1 C10 Mg1 -21.75(6) . . . . ? C11 Na1 C10 Mg1 131.47(14) . . . . ? C2 Na1 C10 Mg1 -8.77(8) . . . . ? N1 Na1 C10 Mg1 -48.41(6) . . . . ? C22 Na1 C10 Mg1 -176.16(8) . . . . ? N2 C10 C11 C12 0.7(2) . . . . ? Mg1 C10 C11 C12 -163.31(14) . . . . ? Na1 C10 C11 C12 -101.88(16) . . . . ? N2 C10 C11 Na1 102.58(13) . . . . ? Mg1 C10 C11 Na1 -61.42(14) . . . . ? N4 Na1 C11 C10 -111.14(12) . . . . ? N3 Na1 C11 C10 164.81(12) . . . . ? C1 Na1 C11 C10 27.36(13) . . . . ? C2 Na1 C11 C10 49.91(15) . . . . ? N1 Na1 C11 C10 0.14(14) . . . . ? C22 Na1 C11 C10 -139.97(12) . . . . ? Mg1 Na1 C11 C10 33.43(10) . . . . ? N4 Na1 C11 C12 -1.40(15) . . . . ? N3 Na1 C11 C12 -85.46(14) . . . . ? C1 Na1 C11 C12 137.10(13) . . . . ? C2 Na1 C11 C12 159.65(12) . . . . ? C10 Na1 C11 C12 109.74(19) . . . . ? N1 Na1 C11 C12 109.88(13) . . . . ? C22 Na1 C11 C12 -30.23(15) . . . . ? Mg1 Na1 C11 C12 143.17(14) . . . . ? C10 C11 C12 C13 178.8(2) . . . . ? Na1 C11 C12 C13 90.7(3) . . . . ? C10 C11 C12 C17 -0.8(2) . . . . ? Na1 C11 C12 C17 -88.86(16) . . . . ? C17 C12 C13 C14 0.7(3) . . . . ? C11 C12 C13 C14 -178.8(2) . . . . ? C12 C13 C14 C15 -0.1(4) . . . . ? C13 C14 C15 C16 -0.8(4) . . . . ? C14 C15 C16 C17 1.0(4) . . . . ? C10 N2 C17 C16 -178.6(2) . . . . ? C18 N2 C17 C16 4.6(3) . . . . ? C10 N2 C17 C12 -0.1(2) . . . . ? C18 N2 C17 C12 -176.88(18) . . . . ? C15 C16 C17 N2 177.9(2) . . . . ? C15 C16 C17 C12 -0.4(3) . . . . ? C13 C12 C17 N2 -179.13(19) . . . . ? C11 C12 C17 N2 0.5(2) . . . . ? C13 C12 C17 C16 -0.5(3) . . . . ? C11 C12 C17 C16 179.2(2) . . . . ? C20 N3 C21 C22 77.3(3) . . . . ? C19 N3 C21 C22 -162.5(2) . . . . ? Na1 N3 C21 C22 -39.2(2) . . . . ? C24 N4 C22 C21 69.1(3) . . . . ? C23 N4 C22 C21 -171.8(2) . . . . ? Na1 N4 C22 C21 -46.9(2) . . . . ? C24 N4 C22 Na1 115.97(19) . . . . ? C23 N4 C22 Na1 -124.89(19) . . . . ? N3 C21 C22 N4 63.9(3) . . . . ? N3 C21 C22 Na1 29.75(17) . . . . ? N3 Na1 C22 N4 -156.98(17) . . . . ? C1 Na1 C22 N4 -57.14(18) . . . . ? C11 Na1 C22 N4 102.49(14) . . . . ? C2 Na1 C22 N4 -87.00(15) . . . . ? C10 Na1 C22 N4 78.48(16) . . . . ? N1 Na1 C22 N4 -35.28(15) . . . . ? Mg1 Na1 C22 N4 62.5(4) . . . . ? N4 Na1 C22 C21 136.7(2) . . . . ? N3 Na1 C22 C21 -20.24(14) . . . . ? C1 Na1 C22 C21 79.61(19) . . . . ? C11 Na1 C22 C21 -120.77(15) . . . . ? C2 Na1 C22 C21 49.75(17) . . . . ? C10 Na1 C22 C21 -144.78(14) . . . . ? N1 Na1 C22 C21 101.47(15) . . . . ? Mg1 Na1 C22 C21 -160.8(3) . . . . ? C32 N5 C25 C26 0.1(2) . . . . ? C33 N5 C25 C26 176.53(19) . . . . ? C32 N5 C25 Mg1 -174.92(13) . . . . ? C33 N5 C25 Mg1 1.5(3) . . . . ? C32 N5 C25 Na2 -82.83(15) . . . . ? C33 N5 C25 Na2 93.63(19) . . . . ? C34 Mg1 C25 C26 -100.4(2) . . . . ? C10 Mg1 C25 C26 122.86(19) . . . . ? C1 Mg1 C25 C26 12.0(2) . . . . ? Na1 Mg1 C25 C26 63.62(19) . . . . ? Na2 Mg1 C25 C26 -73.25(19) . . . . ? C34 Mg1 C25 N5 73.15(17) . . . . ? C10 Mg1 C25 N5 -63.56(17) . . . . ? C1 Mg1 C25 N5 -174.46(15) . . . . ? Na1 Mg1 C25 N5 -122.80(15) . . . . ? Na2 Mg1 C25 N5 100.34(16) . . . . ? C34 Mg1 C25 Na2 -27.18(8) . . . . ? C10 Mg1 C25 Na2 -163.89(7) . . . . ? C1 Mg1 C25 Na2 85.21(7) . . . . ? Na1 Mg1 C25 Na2 136.86(4) . . . . ? N8 Na2 C25 C26 -93.41(14) . . . . ? N7 Na2 C25 C26 3.44(16) . . . . ? C35 Na2 C25 C26 138.41(13) . . . . ? C34 Na2 C25 C26 152.98(13) . . . . ? Mg1 Na2 C25 C26 132.69(15) . . . . ? N8 Na2 C25 N5 9.45(15) . . . . ? N7 Na2 C25 N5 106.29(13) . . . . ? C35 Na2 C25 N5 -118.74(12) . . . . ? C26 Na2 C25 N5 102.86(18) . . . . ? C34 Na2 C25 N5 -104.16(12) . . . . ? Mg1 Na2 C25 N5 -124.46(14) . . . . ? N8 Na2 C25 Mg1 133.90(8) . . . . ? N7 Na2 C25 Mg1 -129.25(8) . . . . ? C35 Na2 C25 Mg1 5.72(8) . . . . ? C26 Na2 C25 Mg1 -132.69(15) . . . . ? C34 Na2 C25 Mg1 20.29(6) . . . . ? N5 C25 C26 C27 0.0(2) . . . . ? Mg1 C25 C26 C27 174.54(15) . . . . ? Na2 C25 C26 C27 99.14(16) . . . . ? N5 C25 C26 Na2 -99.15(13) . . . . ? Mg1 C25 C26 Na2 75.41(16) . . . . ? N8 Na2 C26 C25 103.42(13) . . . . ? N7 Na2 C26 C25 -177.26(13) . . . . ? C35 Na2 C26 C25 -51.20(15) . . . . ? C34 Na2 C26 C25 -27.46(13) . . . . ? Mg1 Na2 C26 C25 -32.85(11) . . . . ? N8 Na2 C26 C27 -3.81(16) . . . . ? N7 Na2 C26 C27 75.50(14) . . . . ? C35 Na2 C26 C27 -158.44(13) . . . . ? C25 Na2 C26 C27 -107.23(19) . . . . ? C34 Na2 C26 C27 -134.69(13) . . . . ? Mg1 Na2 C26 C27 -140.08(14) . . . . ? C25 C26 C27 C28 -178.7(2) . . . . ? Na2 C26 C27 C28 -104.5(3) . . . . ? C25 C26 C27 C32 0.0(2) . . . . ? Na2 C26 C27 C32 74.18(16) . . . . ? C32 C27 C28 C29 -0.3(3) . . . . ? C26 C27 C28 C29 178.3(2) . . . . ? C27 C28 C29 C30 -0.3(4) . . . . ? C28 C29 C30 C31 0.6(4) . . . . ? C29 C30 C31 C32 -0.3(3) . . . . ? C25 N5 C32 C31 178.3(2) . . . . ? C33 N5 C32 C31 1.8(3) . . . . ? C25 N5 C32 C27 -0.1(2) . . . . ? C33 N5 C32 C27 -176.59(18) . . . . ? C30 C31 C32 N5 -178.4(2) . . . . ? C30 C31 C32 C27 -0.2(3) . . . . ? C28 C27 C32 N5 179.05(18) . . . . ? C26 C27 C32 N5 0.1(2) . . . . ? C28 C27 C32 C31 0.5(3) . . . . ? C26 C27 C32 C31 -178.45(19) . . . . ? C41 N6 C34 C35 0.4(2) . . . . ? C42 N6 C34 C35 176.55(19) . . . . ? C41 N6 C34 Mg1 169.63(15) . . . . ? C42 N6 C34 Mg1 -14.2(3) . . . . ? C41 N6 C34 Na2 71.96(18) . . . . ? C42 N6 C34 Na2 -111.87(19) . . . . ? C10 Mg1 C34 C35 -152.41(16) . . . . ? C25 Mg1 C34 C35 83.10(18) . . . . ? C1 Mg1 C34 C35 -31.27(18) . . . . ? Na1 Mg1 C34 C35 -60.2(2) . . . . ? Na2 Mg1 C34 C35 57.64(15) . . . . ? C10 Mg1 C34 N6 39.7(2) . . . . ? C25 Mg1 C34 N6 -84.7(2) . . . . ? C1 Mg1 C34 N6 160.88(18) . . . . ? Na1 Mg1 C34 N6 131.92(16) . . . . ? Na2 Mg1 C34 N6 -110.2(2) . . . . ? C10 Mg1 C34 Na2 149.95(8) . . . . ? C25 Mg1 C34 Na2 25.46(8) . . . . ? C1 Mg1 C34 Na2 -88.91(7) . . . . ? Na1 Mg1 C34 Na2 -117.88(11) . . . . ? N8 Na2 C34 C35 91.71(14) . . . . ? N7 Na2 C34 C35 -9.68(18) . . . . ? C25 Na2 C34 C35 -149.48(14) . . . . ? C26 Na2 C34 C35 -136.19(13) . . . . ? Mg1 Na2 C34 C35 -128.72(15) . . . . ? N8 Na2 C34 N6 -6.58(16) . . . . ? N7 Na2 C34 N6 -107.97(16) . . . . ? C35 Na2 C34 N6 -98.29(19) . . . . ? C25 Na2 C34 N6 112.23(14) . . . . ? C26 Na2 C34 N6 125.51(14) . . . . ? Mg1 Na2 C34 N6 132.99(16) . . . . ? N8 Na2 C34 Mg1 -139.57(7) . . . . ? N7 Na2 C34 Mg1 119.04(11) . . . . ? C35 Na2 C34 Mg1 128.72(15) . . . . ? C25 Na2 C34 Mg1 -20.76(6) . . . . ? C26 Na2 C34 Mg1 -7.48(8) . . . . ? N6 C34 C35 C36 0.1(2) . . . . ? Mg1 C34 C35 C36 -170.71(14) . . . . ? Na2 C34 C35 C36 -106.35(16) . . . . ? N6 C34 C35 Na2 106.49(14) . . . . ? Mg1 C34 C35 Na2 -64.36(13) . . . . ? N8 Na2 C35 C34 -101.75(13) . . . . ? N7 Na2 C35 C34 173.50(12) . . . . ? C25 Na2 C35 C34 30.83(14) . . . . ? C26 Na2 C35 C34 53.92(15) . . . . ? Mg1 Na2 C35 C34 35.15(11) . . . . ? N8 Na2 C35 C36 8.02(17) . . . . ? N7 Na2 C35 C36 -76.72(16) . . . . ? C25 Na2 C35 C36 140.61(14) . . . . ? C26 Na2 C35 C36 163.70(13) . . . . ? C34 Na2 C35 C36 109.8(2) . . . . ? Mg1 Na2 C35 C36 144.92(16) . . . . ? C34 C35 C36 C37 179.4(2) . . . . ? Na2 C35 C36 C37 89.9(3) . . . . ? C34 C35 C36 C41 -0.6(2) . . . . ? Na2 C35 C36 C41 -90.01(16) . . . . ? C41 C36 C37 C38 -0.3(3) . . . . ? C35 C36 C37 C38 179.8(2) . . . . ? C36 C37 C38 C39 0.6(3) . . . . ? C37 C38 C39 C40 -0.4(4) . . . . ? C38 C39 C40 C41 -0.1(3) . . . . ? C34 N6 C41 C40 -179.6(2) . . . . ? C42 N6 C41 C40 4.2(4) . . . . ? C34 N6 C41 C36 -0.7(2) . . . . ? C42 N6 C41 C36 -176.97(19) . . . . ? C39 C40 C41 N6 179.1(2) . . . . ? C39 C40 C41 C36 0.4(3) . . . . ? C37 C36 C41 N6 -179.18(18) . . . . ? C35 C36 C41 N6 0.8(2) . . . . ? C37 C36 C41 C40 -0.2(3) . . . . ? C35 C36 C41 C40 179.72(19) . . . . ? C43 N7 C45 C46 -166.3(2) . . . . ? C44 N7 C45 C46 73.8(3) . . . . ? Na2 N7 C45 C46 -44.1(2) . . . . ? C47 N8 C46 C45 74.6(3) . . . . ? C48 N8 C46 C45 -165.5(2) . . . . ? Na2 N8 C46 C45 -43.1(2) . . . . ? N7 C45 C46 N8 64.9(3) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.202 _refine_diff_density_min -0.208 _refine_diff_density_rms 0.040 #===END ################################################################## ################ COMPOUND 4 ###################################### ################################################################# data_grem224 _database_code_depnum_ccdc_archive 'CCDC 641399' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H32 N4 Zn' _chemical_formula_weight 441.91 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ORTHORHOMBIC _symmetry_space_group_name_H-M P212121 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 12.2666(2) _cell_length_b 13.1709(2) _cell_length_c 14.3918(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2325.17(6) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 3018 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.262 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 936 _exptl_absorpt_coefficient_mu 1.073 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 54726 _diffrn_reflns_av_R_equivalents 0.064 _diffrn_reflns_av_sigmaI/netI 0.0333 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.09 _diffrn_reflns_theta_max 27.49 _reflns_number_total 5323 _reflns_number_gt 4616 _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^)+(0.0194P)^2^+1.0641P] 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 -0.019(10) _refine_ls_number_reflns 5323 _refine_ls_number_parameters 307 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0444 _refine_ls_R_factor_gt 0.0309 _refine_ls_wR_factor_ref 0.0601 _refine_ls_wR_factor_gt 0.0557 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.024 _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 0.050089(19) 0.836721(17) 0.620028(15) 0.02377(6) Uani 1 1 d . A . N1 N 0.20041(15) 0.75638(17) 0.76064(12) 0.0364(5) Uani 1 1 d . A . N2 N 0.02756(15) 0.65237(15) 0.50003(11) 0.0300(4) Uani 1 1 d . A . N3 N -0.10146(14) 0.92075(13) 0.61680(14) 0.0292(4) Uani 1 1 d . . . N4 N 0.12503(16) 0.98542(15) 0.59784(13) 0.0355(5) Uani 1 1 d . . . C1 C 0.09740(18) 0.79769(17) 0.74798(14) 0.0253(5) Uani 1 1 d . . . C2 C 0.0556(2) 0.80935(15) 0.83591(13) 0.0266(5) Uani 1 1 d . A . H2 H -0.0144 0.8365 0.8496 0.032 Uiso 1 1 calc R . . C3 C 0.13151(18) 0.77511(15) 0.90359(14) 0.0254(5) Uani 1 1 d . . . C4 C 0.1322(2) 0.76332(18) 1.00102(15) 0.0328(6) Uani 1 1 d . A . H4 H 0.0715 0.7844 1.0372 0.039 Uiso 1 1 calc R . . C5 C 0.2228(2) 0.72053(19) 1.04317(16) 0.0370(6) Uani 1 1 d . . . H5 H 0.2236 0.7120 1.1087 0.044 Uiso 1 1 calc R A . C6 C 0.3122(2) 0.6900(2) 0.99143(17) 0.0489(8) Uani 1 1 d . A . H6 H 0.3731 0.6607 1.0221 0.059 Uiso 1 1 calc R . . C7 C 0.3142(2) 0.7015(2) 0.89579(18) 0.0533(8) Uani 1 1 d . . . H7 H 0.3759 0.6816 0.8604 0.064 Uiso 1 1 calc R A . C8 C 0.22333(18) 0.74283(19) 0.85374(15) 0.0335(5) Uani 1 1 d . A . C9 C 0.2756(2) 0.7288(3) 0.68719(18) 0.0705(11) Uani 1 1 d . . . H9A H 0.3000 0.6586 0.6963 0.106 Uiso 1 1 calc R A . H9B H 0.3387 0.7744 0.6886 0.106 Uiso 1 1 calc R . . H9C H 0.2389 0.7346 0.6269 0.106 Uiso 1 1 calc R . . C10 C 0.0526(2) 0.75553(16) 0.50198(13) 0.0280(4) Uani 1 1 d . . . C11 C 0.0678(2) 0.78334(17) 0.41046(14) 0.0361(6) Uani 1 1 d . A . H11 H 0.0861 0.8497 0.3899 0.043 Uiso 1 1 calc R . . C12 C 0.0520(2) 0.69816(16) 0.35144(14) 0.0322(5) Uani 1 1 d . . . C13 C 0.0545(2) 0.6817(2) 0.25498(14) 0.0457(6) Uani 1 1 d . A . H13 H 0.0716 0.7358 0.2139 0.055 Uiso 1 1 calc R . . C14 C 0.0321(2) 0.5869(2) 0.22077(18) 0.0504(7) Uani 1 1 d . . . H14 H 0.0338 0.5759 0.1555 0.060 Uiso 1 1 calc R A . C15 C 0.0073(2) 0.5071(2) 0.2789(2) 0.0541(8) Uani 1 1 d . A . H15 H -0.0077 0.4421 0.2533 0.065 Uiso 1 1 calc R . . C16 C 0.0038(2) 0.52075(19) 0.3750(2) 0.0478(6) Uani 1 1 d . . . H16 H -0.0136 0.4660 0.4154 0.057 Uiso 1 1 calc R A . C17 C 0.02659(18) 0.61630(17) 0.40966(15) 0.0301(5) Uani 1 1 d . A . C18 C 0.0075(3) 0.5892(2) 0.58040(18) 0.0558(9) Uani 1 1 d . . . H18A H 0.0642 0.5370 0.5847 0.084 Uiso 1 1 calc R A . H18B H -0.0639 0.5567 0.5744 0.084 Uiso 1 1 calc R . . H18C H 0.0088 0.6312 0.6366 0.084 Uiso 1 1 calc R . . C19B C -0.1778(11) 0.8556(9) 0.5525(9) 0.041(3) Uiso 0.292(10) 1 d P A 2 H19D H -0.1948 0.7911 0.5833 0.061 Uiso 0.292(10) 1 calc PR A 2 H19E H -0.1407 0.8420 0.4935 0.061 Uiso 0.292(10) 1 calc PR A 2 H19F H -0.2454 0.8929 0.5406 0.061 Uiso 0.292(10) 1 calc PR A 2 C20B C -0.1493(10) 0.9409(9) 0.7013(8) 0.029(3) Uiso 0.292(10) 1 d P A 2 H20D H -0.2188 0.9761 0.6914 0.043 Uiso 0.292(10) 1 calc PR A 2 H20E H -0.1008 0.9839 0.7384 0.043 Uiso 0.292(10) 1 calc PR A 2 H20F H -0.1625 0.8770 0.7343 0.043 Uiso 0.292(10) 1 calc PR A 2 C23B C 0.2109(13) 1.0031(14) 0.6783(12) 0.053(5) Uiso 0.292(10) 1 d P A 2 H23D H 0.2760 0.9619 0.6665 0.079 Uiso 0.292(10) 1 calc PR A 2 H23E H 0.1787 0.9833 0.7380 0.079 Uiso 0.292(10) 1 calc PR A 2 H23F H 0.2312 1.0750 0.6804 0.079 Uiso 0.292(10) 1 calc PR A 2 C24B C 0.211(2) 0.971(2) 0.5152(19) 0.079(8) Uiso 0.292(10) 1 d P A 2 H24D H 0.2411 1.0367 0.4975 0.119 Uiso 0.292(10) 1 calc PR A 2 H24E H 0.1743 0.9400 0.4616 0.119 Uiso 0.292(10) 1 calc PR A 2 H24F H 0.2700 0.9260 0.5360 0.119 Uiso 0.292(10) 1 calc PR A 2 C22B C 0.0335(12) 1.0601(9) 0.6130(11) 0.045(3) Uani 0.292(10) 1 d P A 2 H22C H 0.0513 1.1273 0.5862 0.054 Uiso 0.292(10) 1 calc PR A 2 H22D H 0.0172 1.0682 0.6800 0.054 Uiso 0.292(10) 1 calc PR A 2 C21B C -0.0669(9) 1.0077(8) 0.5590(8) 0.034(3) Uani 0.292(10) 1 d P A 2 H21C H -0.1276 1.0566 0.5514 0.041 Uiso 0.292(10) 1 calc PR A 2 H21D H -0.0437 0.9843 0.4967 0.041 Uiso 0.292(10) 1 calc PR A 2 C19A C -0.1689(4) 0.8984(6) 0.5371(3) 0.0480(15) Uani 0.708(10) 1 d P A 1 H19A H -0.2360 0.9386 0.5404 0.072 Uiso 0.708(10) 1 calc PR A 1 H19B H -0.1871 0.8260 0.5368 0.072 Uiso 0.708(10) 1 calc PR A 1 H19C H -0.1292 0.9156 0.4801 0.072 Uiso 0.708(10) 1 calc PR A 1 C20A C -0.1735(4) 0.9051(5) 0.7010(3) 0.0419(12) Uani 0.708(10) 1 d P A 1 H20A H -0.1987 0.8346 0.7027 0.063 Uiso 0.708(10) 1 calc PR A 1 H20B H -0.2364 0.9507 0.6973 0.063 Uiso 0.708(10) 1 calc PR A 1 H20C H -0.1318 0.9200 0.7575 0.063 Uiso 0.708(10) 1 calc PR A 1 C23A C 0.1727(6) 1.0262(4) 0.6820(3) 0.0447(14) Uani 0.708(10) 1 d P A 1 H23A H 0.1959 1.0964 0.6712 0.067 Uiso 0.708(10) 1 calc PR A 1 H23B H 0.2360 0.9851 0.6998 0.067 Uiso 0.708(10) 1 calc PR A 1 H23C H 0.1186 1.0246 0.7321 0.067 Uiso 0.708(10) 1 calc PR A 1 C24A C 0.2009(8) 0.9930(7) 0.5217(5) 0.061(2) Uani 0.708(10) 1 d P A 1 H24A H 0.2599 0.9438 0.5305 0.091 Uiso 0.708(10) 1 calc PR A 1 H24B H 0.2314 1.0617 0.5197 0.091 Uiso 0.708(10) 1 calc PR A 1 H24C H 0.1630 0.9786 0.4632 0.091 Uiso 0.708(10) 1 calc PR A 1 C21A C -0.0679(4) 1.0298(3) 0.6164(7) 0.0616(19) Uani 0.708(10) 1 d P A 1 H21A H -0.1273 1.0714 0.5895 0.074 Uiso 0.708(10) 1 calc PR A 1 H21B H -0.0559 1.0528 0.6810 0.074 Uiso 0.708(10) 1 calc PR A 1 C22A C 0.0322(5) 1.0454(4) 0.5623(6) 0.0557(16) Uani 0.708(10) 1 d P A 1 H22A H 0.0517 1.1183 0.5636 0.067 Uiso 0.708(10) 1 calc PR A 1 H22B H 0.0184 1.0264 0.4968 0.067 Uiso 0.708(10) 1 calc PR A 1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.02714(11) 0.02729(11) 0.01689(10) 0.00077(10) 0.00035(11) 0.00220(11) N1 0.0225(10) 0.0672(14) 0.0196(9) 0.0083(10) 0.0012(8) 0.0057(10) N2 0.0369(11) 0.0333(10) 0.0199(8) -0.0002(8) -0.0008(7) 0.0005(9) N3 0.0277(9) 0.0301(9) 0.0297(9) 0.0004(9) -0.0022(9) 0.0018(7) N4 0.0341(11) 0.0392(11) 0.0330(11) 0.0023(9) 0.0014(9) -0.0101(9) C1 0.0250(11) 0.0295(11) 0.0214(11) 0.0005(9) -0.0008(9) -0.0001(9) C2 0.0330(12) 0.0280(11) 0.0189(9) 0.0006(8) 0.0017(10) 0.0046(11) C3 0.0309(12) 0.0231(11) 0.0222(11) -0.0007(8) -0.0018(9) -0.0064(9) C4 0.0471(16) 0.0303(13) 0.0210(11) -0.0029(9) -0.0027(11) -0.0004(11) C5 0.0487(16) 0.0400(15) 0.0223(12) 0.0030(10) -0.0092(11) -0.0126(12) C6 0.0307(14) 0.082(2) 0.0339(14) 0.0161(14) -0.0133(11) -0.0045(14) C7 0.0235(12) 0.103(2) 0.0336(15) 0.0182(14) -0.0025(11) 0.0041(13) C8 0.0260(12) 0.0503(15) 0.0240(11) 0.0101(10) -0.0025(9) -0.0065(11) C9 0.0357(17) 0.147(3) 0.0284(14) 0.0239(18) 0.0098(12) 0.0350(19) C10 0.0347(12) 0.0277(11) 0.0216(9) -0.0008(8) -0.0024(11) 0.0098(12) C11 0.0563(18) 0.0294(12) 0.0225(10) 0.0018(9) -0.0002(11) 0.0076(12) C12 0.0338(12) 0.0398(12) 0.0230(10) -0.0032(8) -0.0030(11) 0.0155(11) C13 0.0569(16) 0.0589(17) 0.0212(10) -0.0047(11) -0.0039(12) 0.0163(16) C14 0.0514(19) 0.0692(18) 0.0304(13) -0.0176(13) -0.0107(13) 0.0174(15) C15 0.0583(18) 0.0538(17) 0.0501(17) -0.0264(15) -0.0123(14) -0.0021(15) C16 0.0563(16) 0.0414(14) 0.0457(15) -0.0081(14) -0.0004(15) -0.0074(12) C17 0.0289(13) 0.0363(12) 0.0251(11) -0.0041(9) -0.0033(9) 0.0039(10) C18 0.092(2) 0.0433(15) 0.0317(13) 0.0088(12) 0.0003(14) -0.0221(15) C22B 0.055(7) 0.025(4) 0.054(7) -0.010(6) -0.012(8) 0.000(4) C21B 0.044(7) 0.022(5) 0.036(5) 0.012(4) 0.006(5) 0.021(4) C19A 0.032(2) 0.075(5) 0.036(2) -0.004(3) -0.0156(19) 0.013(3) C20A 0.027(2) 0.061(4) 0.037(2) 0.000(2) 0.0023(19) 0.007(2) C23A 0.059(4) 0.035(3) 0.040(2) -0.0023(19) -0.005(3) -0.019(3) C24A 0.086(5) 0.057(4) 0.040(3) -0.017(3) 0.040(3) -0.051(4) C21A 0.051(3) 0.025(2) 0.109(6) -0.001(3) 0.019(4) 0.0036(17) C22A 0.057(3) 0.029(3) 0.081(4) 0.020(3) -0.007(4) -0.006(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 C1 1.998(2) . ? Zn1 C10 2.008(2) . ? Zn1 N3 2.1640(17) . ? Zn1 N4 2.1870(19) . ? N1 C8 1.381(3) . ? N1 C1 1.388(3) . ? N1 C9 1.449(3) . ? N2 C17 1.385(3) . ? N2 C10 1.393(3) . ? N2 C18 1.446(3) . ? N3 C20B 1.376(12) . ? N3 C19A 1.444(5) . ? N3 C21B 1.478(9) . ? N3 C21A 1.494(4) . ? N3 C20A 1.513(5) . ? N3 C19B 1.571(12) . ? N4 C24A 1.441(7) . ? N4 C23A 1.449(5) . ? N4 C22A 1.477(6) . ? N4 C22B 1.508(14) . ? N4 C23B 1.583(16) . ? N4 C24B 1.60(2) . ? C1 C2 1.374(3) . ? C2 C3 1.421(3) . ? C2 H2 0.9500 . ? C3 C8 1.401(3) . ? C3 C4 1.411(3) . ? C4 C5 1.386(3) . ? C4 H4 0.9500 . ? C5 C6 1.385(4) . ? C5 H5 0.9500 . ? C6 C7 1.385(3) . ? C6 H6 0.9500 . ? C7 C8 1.380(3) . ? C7 H7 0.9500 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C11 1.380(3) . ? C11 C12 1.420(3) . ? C11 H11 0.9500 . ? C12 C17 1.401(3) . ? C12 C13 1.405(3) . ? C13 C14 1.370(4) . ? C13 H13 0.9500 . ? C14 C15 1.377(4) . ? C14 H14 0.9500 . ? C15 C16 1.396(4) . ? C15 H15 0.9500 . ? C16 C17 1.382(3) . ? C16 H16 0.9500 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19B H19D 0.9800 . ? C19B H19E 0.9800 . ? C19B H19F 0.9800 . ? C20B H20D 0.9800 . ? C20B H20E 0.9800 . ? C20B H20F 0.9800 . ? C23B H23D 0.9800 . ? C23B H23E 0.9800 . ? C23B H23F 0.9800 . ? C24B H24D 0.9800 . ? C24B H24E 0.9800 . ? C24B H24F 0.9800 . ? C22B C21B 1.61(2) . ? C22B H22C 0.9900 . ? C22B H22D 0.9900 . ? C21B H21C 0.9900 . ? C21B H21D 0.9900 . ? C19A H19A 0.9800 . ? C19A H19B 0.9800 . ? C19A H19C 0.9800 . ? C20A H20A 0.9800 . ? C20A H20B 0.9800 . ? C20A H20C 0.9800 . ? C23A H23A 0.9800 . ? C23A H23B 0.9800 . ? C23A H23C 0.9800 . ? C24A H24A 0.9800 . ? C24A H24B 0.9800 . ? C24A H24C 0.9800 . ? C21A C22A 1.469(10) . ? C21A H21A 0.9900 . ? C21A H21B 0.9900 . ? C22A H22A 0.9900 . ? C22A H22B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Zn1 C10 129.68(8) . . ? C1 Zn1 N3 113.63(8) . . ? C10 Zn1 N3 105.50(9) . . ? C1 Zn1 N4 104.06(8) . . ? C10 Zn1 N4 110.31(8) . . ? N3 Zn1 N4 84.26(7) . . ? C8 N1 C1 111.31(18) . . ? C8 N1 C9 123.1(2) . . ? C1 N1 C9 125.59(19) . . ? C17 N2 C10 110.81(17) . . ? C17 N2 C18 123.6(2) . . ? C10 N2 C18 125.62(18) . . ? C20B N3 C19A 119.8(6) . . ? C20B N3 C21B 118.1(6) . . ? C19A N3 C21B 82.8(5) . . ? C20B N3 C21A 86.3(5) . . ? C19A N3 C21A 110.5(4) . . ? C21B N3 C21A 34.3(4) . . ? C20B N3 C20A 21.5(4) . . ? C19A N3 C20A 105.9(3) . . ? C21B N3 C20A 136.3(5) . . ? C21A N3 C20A 107.1(3) . . ? C20B N3 C19B 111.8(7) . . ? C19A N3 C19B 23.1(4) . . ? C21B N3 C19B 105.2(6) . . ? C21A N3 C19B 133.4(5) . . ? C20A N3 C19B 92.8(5) . . ? C20B N3 Zn1 116.5(5) . . ? C19A N3 Zn1 113.9(2) . . ? C21B N3 Zn1 99.3(4) . . ? C21A N3 Zn1 104.8(2) . . ? C20A N3 Zn1 114.5(2) . . ? C19B N3 Zn1 104.2(5) . . ? C24A N4 C23A 110.4(5) . . ? C24A N4 C22A 101.4(6) . . ? C23A N4 C22A 113.8(4) . . ? C24A N4 C22B 123.1(8) . . ? C23A N4 C22B 86.4(5) . . ? C22A N4 C22B 29.3(4) . . ? C24A N4 C23B 96.7(8) . . ? C23A N4 C23B 20.7(6) . . ? C22A N4 C23B 133.4(6) . . ? C22B N4 C23B 107.1(7) . . ? C24A N4 C24B 11.0(13) . . ? C23A N4 C24B 113.6(11) . . ? C22A N4 C24B 108.4(12) . . ? C22B N4 C24B 132.6(13) . . ? C23B N4 C24B 97.1(12) . . ? C24A N4 Zn1 116.4(3) . . ? C23A N4 Zn1 112.3(2) . . ? C22A N4 Zn1 101.9(2) . . ? C22B N4 Zn1 104.5(5) . . ? C23B N4 Zn1 107.7(7) . . ? C24B N4 Zn1 106.0(10) . . ? C2 C1 N1 105.24(19) . . ? C2 C1 Zn1 135.36(18) . . ? N1 C1 Zn1 119.10(15) . . ? C1 C2 C3 110.5(2) . . ? C1 C2 H2 124.7 . . ? C3 C2 H2 124.7 . . ? C8 C3 C4 118.1(2) . . ? C8 C3 C2 105.79(18) . . ? C4 C3 C2 136.1(2) . . ? C5 C4 C3 119.0(2) . . ? C5 C4 H4 120.5 . . ? C3 C4 H4 120.5 . . ? C6 C5 C4 121.2(2) . . ? C6 C5 H5 119.4 . . ? C4 C5 H5 119.4 . . ? C5 C6 C7 121.1(2) . . ? C5 C6 H6 119.4 . . ? C7 C6 H6 119.4 . . ? C8 C7 C6 117.7(2) . . ? C8 C7 H7 121.2 . . ? C6 C7 H7 121.2 . . ? C7 C8 N1 129.9(2) . . ? C7 C8 C3 123.0(2) . . ? N1 C8 C3 107.09(19) . . ? N1 C9 H9A 109.5 . . ? N1 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? N1 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C11 C10 N2 105.63(18) . . ? C11 C10 Zn1 131.95(17) . . ? N2 C10 Zn1 122.22(14) . . ? C10 C11 C12 110.0(2) . . ? C10 C11 H11 125.0 . . ? C12 C11 H11 125.0 . . ? C17 C12 C13 118.5(2) . . ? C17 C12 C11 106.29(18) . . ? C13 C12 C11 135.2(2) . . ? C14 C13 C12 119.4(2) . . ? C14 C13 H13 120.3 . . ? C12 C13 H13 120.3 . . ? C13 C14 C15 121.4(2) . . ? C13 C14 H14 119.3 . . ? C15 C14 H14 119.3 . . ? C14 C15 C16 120.7(3) . . ? C14 C15 H15 119.6 . . ? C16 C15 H15 119.6 . . ? C17 C16 C15 117.9(3) . . ? C17 C16 H16 121.0 . . ? C15 C16 H16 121.0 . . ? C16 C17 N2 130.8(2) . . ? C16 C17 C12 122.0(2) . . ? N2 C17 C12 107.21(18) . . ? N2 C18 H18A 109.5 . . ? N2 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? N2 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N3 C19B H19D 109.5 . . ? N3 C19B H19E 109.5 . . ? H19D C19B H19E 109.5 . . ? N3 C19B H19F 109.5 . . ? H19D C19B H19F 109.5 . . ? H19E C19B H19F 109.5 . . ? N3 C20B H20D 109.5 . . ? N3 C20B H20E 109.5 . . ? H20D C20B H20E 109.5 . . ? N3 C20B H20F 109.5 . . ? H20D C20B H20F 109.5 . . ? H20E C20B H20F 109.5 . . ? N4 C23B H23D 109.5 . . ? N4 C23B H23E 109.5 . . ? H23D C23B H23E 109.5 . . ? N4 C23B H23F 109.5 . . ? H23D C23B H23F 109.5 . . ? H23E C23B H23F 109.5 . . ? N4 C24B H24D 109.5 . . ? N4 C24B H24E 109.5 . . ? H24D C24B H24E 109.5 . . ? N4 C24B H24F 109.5 . . ? H24D C24B H24F 109.5 . . ? H24E C24B H24F 109.5 . . ? N4 C22B C21B 102.7(9) . . ? N4 C22B H22C 111.2 . . ? C21B C22B H22C 111.2 . . ? N4 C22B H22D 111.2 . . ? C21B C22B H22D 111.2 . . ? H22C C22B H22D 109.1 . . ? N3 C21B C22B 106.2(9) . . ? N3 C21B H21C 110.5 . . ? C22B C21B H21C 110.5 . . ? N3 C21B H21D 110.5 . . ? C22B C21B H21D 110.5 . . ? H21C C21B H21D 108.7 . . ? N3 C19A H19A 109.5 . . ? N3 C19A H19B 109.5 . . ? N3 C19A H19C 109.5 . . ? N3 C20A H20A 109.5 . . ? N3 C20A H20B 109.5 . . ? N3 C20A H20C 109.5 . . ? N4 C23A H23A 109.5 . . ? N4 C23A H23B 109.5 . . ? N4 C23A H23C 109.5 . . ? N4 C24A H24A 109.5 . . ? N4 C24A H24B 109.5 . . ? N4 C24A H24C 109.5 . . ? C22A C21A N3 111.5(5) . . ? C22A C21A H21A 109.3 . . ? N3 C21A H21A 109.3 . . ? C22A C21A H21B 109.3 . . ? N3 C21A H21B 109.3 . . ? H21A C21A H21B 108.0 . . ? C21A C22A N4 112.7(5) . . ? C21A C22A H22A 109.1 . . ? N4 C22A H22A 109.1 . . ? C21A C22A H22B 109.1 . . ? N4 C22A H22B 109.1 . . ? H22A C22A H22B 107.8 . . ? 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 C1 Zn1 N3 C20B 1.2(6) . . . . ? C10 Zn1 N3 C20B 148.8(6) . . . . ? N4 Zn1 N3 C20B -101.7(6) . . . . ? C1 Zn1 N3 C19A -144.7(4) . . . . ? C10 Zn1 N3 C19A 2.9(4) . . . . ? N4 Zn1 N3 C19A 112.5(4) . . . . ? C1 Zn1 N3 C21B 129.1(6) . . . . ? C10 Zn1 N3 C21B -83.3(6) . . . . ? N4 Zn1 N3 C21B 26.2(6) . . . . ? C1 Zn1 N3 C21A 94.5(4) . . . . ? C10 Zn1 N3 C21A -117.9(4) . . . . ? N4 Zn1 N3 C21A -8.4(4) . . . . ? C1 Zn1 N3 C20A -22.6(3) . . . . ? C10 Zn1 N3 C20A 125.0(3) . . . . ? N4 Zn1 N3 C20A -125.5(3) . . . . ? C1 Zn1 N3 C19B -122.5(5) . . . . ? C10 Zn1 N3 C19B 25.2(5) . . . . ? N4 Zn1 N3 C19B 134.7(5) . . . . ? C1 Zn1 N4 C24A 119.1(5) . . . . ? C10 Zn1 N4 C24A -23.5(5) . . . . ? N3 Zn1 N4 C24A -127.9(5) . . . . ? C1 Zn1 N4 C23A -9.6(4) . . . . ? C10 Zn1 N4 C23A -152.2(4) . . . . ? N3 Zn1 N4 C23A 103.4(4) . . . . ? C1 Zn1 N4 C22A -131.7(4) . . . . ? C10 Zn1 N4 C22A 85.7(4) . . . . ? N3 Zn1 N4 C22A -18.7(4) . . . . ? C1 Zn1 N4 C22B -101.7(6) . . . . ? C10 Zn1 N4 C22B 115.7(6) . . . . ? N3 Zn1 N4 C22B 11.3(6) . . . . ? C1 Zn1 N4 C23B 11.9(6) . . . . ? C10 Zn1 N4 C23B -130.7(6) . . . . ? N3 Zn1 N4 C23B 124.9(6) . . . . ? C1 Zn1 N4 C24B 115.1(12) . . . . ? C10 Zn1 N4 C24B -27.5(12) . . . . ? N3 Zn1 N4 C24B -132.0(12) . . . . ? C8 N1 C1 C2 -0.3(3) . . . . ? C9 N1 C1 C2 178.8(3) . . . . ? C8 N1 C1 Zn1 174.36(16) . . . . ? C9 N1 C1 Zn1 -6.5(4) . . . . ? C10 Zn1 C1 C2 -136.2(2) . . . . ? N3 Zn1 C1 C2 1.7(3) . . . . ? N4 Zn1 C1 C2 91.6(2) . . . . ? C10 Zn1 C1 N1 51.1(2) . . . . ? N3 Zn1 C1 N1 -170.96(16) . . . . ? N4 Zn1 C1 N1 -81.13(19) . . . . ? N1 C1 C2 C3 -0.3(3) . . . . ? Zn1 C1 C2 C3 -173.68(17) . . . . ? C1 C2 C3 C8 0.8(3) . . . . ? C1 C2 C3 C4 -175.8(2) . . . . ? C8 C3 C4 C5 -0.1(3) . . . . ? C2 C3 C4 C5 176.2(2) . . . . ? C3 C4 C5 C6 0.4(4) . . . . ? C4 C5 C6 C7 0.2(4) . . . . ? C5 C6 C7 C8 -1.0(4) . . . . ? C6 C7 C8 N1 -175.1(3) . . . . ? C6 C7 C8 C3 1.4(4) . . . . ? C1 N1 C8 C7 177.8(3) . . . . ? C9 N1 C8 C7 -1.4(5) . . . . ? C1 N1 C8 C3 0.8(3) . . . . ? C9 N1 C8 C3 -178.3(3) . . . . ? C4 C3 C8 C7 -0.8(4) . . . . ? C2 C3 C8 C7 -178.1(2) . . . . ? C4 C3 C8 N1 176.4(2) . . . . ? C2 C3 C8 N1 -0.9(3) . . . . ? C17 N2 C10 C11 -0.3(3) . . . . ? C18 N2 C10 C11 178.4(3) . . . . ? C17 N2 C10 Zn1 175.14(16) . . . . ? C18 N2 C10 Zn1 -6.2(3) . . . . ? C1 Zn1 C10 C11 -147.4(2) . . . . ? N3 Zn1 C10 C11 72.2(3) . . . . ? N4 Zn1 C10 C11 -17.3(3) . . . . ? C1 Zn1 C10 N2 38.6(3) . . . . ? N3 Zn1 C10 N2 -101.81(19) . . . . ? N4 Zn1 C10 N2 168.66(18) . . . . ? N2 C10 C11 C12 0.2(3) . . . . ? Zn1 C10 C11 C12 -174.55(19) . . . . ? C10 C11 C12 C17 -0.1(3) . . . . ? C10 C11 C12 C13 178.5(3) . . . . ? C17 C12 C13 C14 0.1(4) . . . . ? C11 C12 C13 C14 -178.4(3) . . . . ? C12 C13 C14 C15 -0.1(4) . . . . ? C13 C14 C15 C16 0.2(5) . . . . ? C14 C15 C16 C17 -0.3(4) . . . . ? C15 C16 C17 N2 178.7(2) . . . . ? C15 C16 C17 C12 0.3(4) . . . . ? C10 N2 C17 C16 -178.4(2) . . . . ? C18 N2 C17 C16 2.9(4) . . . . ? C10 N2 C17 C12 0.2(3) . . . . ? C18 N2 C17 C12 -178.5(2) . . . . ? C13 C12 C17 C16 -0.2(4) . . . . ? C11 C12 C17 C16 178.7(2) . . . . ? C13 C12 C17 N2 -178.9(2) . . . . ? C11 C12 C17 N2 -0.1(3) . . . . ? C24A N4 C22B C21B 92.5(10) . . . . ? C23A N4 C22B C21B -155.3(10) . . . . ? C22A N4 C22B C21B 45.4(10) . . . . ? C23B N4 C22B C21B -157.3(10) . . . . ? C24B N4 C22B C21B 85.5(18) . . . . ? Zn1 N4 C22B C21B -43.2(10) . . . . ? C20B N3 C21B C22B 68.3(12) . . . . ? C19A N3 C21B C22B -171.7(9) . . . . ? C21A N3 C21B C22B 44.0(9) . . . . ? C20A N3 C21B C22B 82.7(10) . . . . ? C19B N3 C21B C22B -166.2(9) . . . . ? Zn1 N3 C21B C22B -58.6(9) . . . . ? N4 C22B C21B N3 73.1(13) . . . . ? C20B N3 C21A C22A 152.3(9) . . . . ? C19A N3 C21A C22A -87.2(7) . . . . ? C21B N3 C21A C22A -49.1(9) . . . . ? C20A N3 C21A C22A 157.8(7) . . . . ? C19B N3 C21A C22A -90.9(9) . . . . ? Zn1 N3 C21A C22A 35.8(8) . . . . ? N3 C21A C22A N4 -58.8(10) . . . . ? C24A N4 C22A C21A 165.8(7) . . . . ? C23A N4 C22A C21A -75.6(8) . . . . ? C22B N4 C22A C21A -53.0(13) . . . . ? C23B N4 C22A C21A -83.4(12) . . . . ? C24B N4 C22A C21A 157.0(13) . . . . ? Zn1 N4 C22A C21A 45.4(8) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.359 _refine_diff_density_min -0.229 _refine_diff_density_rms 0.048 #===END ################################################################## ################ COMPOUND 6 ###################################### ################################################################# data_grem221 _database_code_depnum_ccdc_archive 'CCDC 641400' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H49 N4 Na Zn' _chemical_formula_weight 482.03 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Zn Zn 0.2839 1.4301 '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 orthorhombic _symmetry_space_group_name_H-M P212121 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 10.9318(3) _cell_length_b 14.4362(4) _cell_length_c 17.5664(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2772.22(13) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 3528 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.48 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.27 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.155 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1048 _exptl_absorpt_coefficient_mu 0.918 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 24509 _diffrn_reflns_av_R_equivalents 0.032 _diffrn_reflns_av_sigmaI/netI 0.0294 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.83 _diffrn_reflns_theta_max 27.50 _reflns_number_total 6275 _reflns_number_gt 5631 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Denzo & Collect' _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^)+(0.0172P)^2^+0.9941P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.514(8) _refine_ls_number_reflns 6275 _refine_ls_number_parameters 307 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0361 _refine_ls_R_factor_gt 0.0271 _refine_ls_wR_factor_ref 0.0560 _refine_ls_wR_factor_gt 0.0523 _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_restrained_S_all 1.057 _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 Zn1 Zn -0.029837(16) 0.996055(13) 0.984756(10) 0.01848(5) Uani 1 1 d . . . Na1 Na 0.20271(6) 0.97151(4) 0.87798(4) 0.02249(16) Uani 1 1 d . . . N1 N -0.00982(13) 0.92691(9) 0.88657(8) 0.0198(3) Uani 1 1 d . . . N2 N 0.15931(15) 1.14539(11) 1.03042(10) 0.0293(4) Uani 1 1 d . . . N3 N 0.38245(14) 0.88378(11) 0.81941(10) 0.0267(4) Uani 1 1 d . . . N4 N 0.31697(14) 1.08910(10) 0.80632(9) 0.0229(3) Uani 1 1 d . . . C1 C -0.17569(14) 1.00221(16) 1.05668(9) 0.0231(3) Uani 1 1 d . . . C2 C -0.1727(2) 1.09364(14) 1.10083(13) 0.0304(5) Uani 1 1 d . . . H2A H -0.2336 1.0918 1.1418 0.046 Uiso 1 1 calc R . . H2B H -0.1915 1.1450 1.0662 0.046 Uiso 1 1 calc R . . H2C H -0.0911 1.1027 1.1228 0.046 Uiso 1 1 calc R . . C3 C -0.1561(2) 0.92353(14) 1.11381(13) 0.0352(5) Uani 1 1 d . . . H3A H -0.1592 0.8639 1.0872 0.053 Uiso 1 1 calc R . . H3B H -0.2204 0.9255 1.1526 0.053 Uiso 1 1 calc R . . H3C H -0.0760 0.9307 1.1382 0.053 Uiso 1 1 calc R . . C4 C -0.30364(15) 0.99077(16) 1.02316(11) 0.0329(4) Uani 1 1 d . . . H4A H -0.3642 0.9915 1.0643 0.049 Uiso 1 1 calc R . . H4B H -0.3086 0.9317 0.9958 0.049 Uiso 1 1 calc R . . H4C H -0.3203 1.0418 0.9878 0.049 Uiso 1 1 calc R . . C5 C -0.07083(17) 0.97118(13) 0.82142(11) 0.0242(4) Uani 1 1 d . . . C6 C -0.0222(2) 0.93019(15) 0.74613(11) 0.0336(5) Uani 1 1 d . . . H6A H -0.0688 0.9567 0.7030 0.040 Uiso 1 1 calc R . . H6B H 0.0648 0.9477 0.7397 0.040 Uiso 1 1 calc R . . C7 C -0.0335(2) 0.82529(15) 0.74476(12) 0.0415(5) Uani 1 1 d . . . H7A H 0.0043 0.8008 0.6977 0.050 Uiso 1 1 calc R . . H7B H -0.1211 0.8077 0.7447 0.050 Uiso 1 1 calc R . . C8 C 0.0295(2) 0.78292(13) 0.81413(12) 0.0359(5) Uani 1 1 d . . . H8A H 0.1189 0.7923 0.8095 0.043 Uiso 1 1 calc R . . H8B H 0.0140 0.7154 0.8147 0.043 Uiso 1 1 calc R . . C9 C -0.01434(18) 0.82484(12) 0.89000(11) 0.0238(4) Uani 1 1 d . . . C10 C -0.0402(2) 1.07447(13) 0.82407(12) 0.0320(4) Uani 1 1 d . . . H10A H 0.0489 1.0825 0.8248 0.048 Uiso 1 1 calc R . . H10B H -0.0755 1.1019 0.8701 0.048 Uiso 1 1 calc R . . H10C H -0.0742 1.1052 0.7790 0.048 Uiso 1 1 calc R . . C11 C -0.21263(18) 0.96637(15) 0.82065(12) 0.0350(5) Uani 1 1 d . . . H11A H -0.2443 0.9838 0.8709 0.053 Uiso 1 1 calc R . . H11B H -0.2386 0.9031 0.8084 0.053 Uiso 1 1 calc R . . H11C H -0.2445 1.0092 0.7822 0.053 Uiso 1 1 calc R . . C12 C 0.0746(2) 0.79461(13) 0.95248(13) 0.0315(5) Uani 1 1 d . . . H12A H 0.0484 0.8207 1.0013 0.047 Uiso 1 1 calc R . . H12B H 0.1569 0.8169 0.9403 0.047 Uiso 1 1 calc R . . H12C H 0.0753 0.7268 0.9559 0.047 Uiso 1 1 calc R . . C13 C -0.13994(19) 0.78317(13) 0.91150(13) 0.0312(5) Uani 1 1 d . . . H13A H -0.1975 0.7922 0.8694 0.047 Uiso 1 1 calc R . . H13B H -0.1713 0.8141 0.9572 0.047 Uiso 1 1 calc R . . H13C H -0.1307 0.7168 0.9216 0.047 Uiso 1 1 calc R . . C14 C 0.13544(17) 1.05288(12) 1.01466(12) 0.0245(4) Uani 1 1 d . . . C15 C 0.24315(17) 1.00786(19) 1.03432(10) 0.0301(4) Uani 1 1 d . . . C16 C 0.3297(2) 1.07269(19) 1.06167(13) 0.0412(6) Uani 1 1 d . . . C17 C 0.2754(2) 1.15677(18) 1.05891(13) 0.0386(5) Uani 1 1 d . . . C18 C 0.0772(2) 1.22155(15) 1.01440(18) 0.0410(5) Uani 1 1 d . . . C19 C 0.4513(2) 0.85837(15) 0.88826(13) 0.0399(5) Uani 1 1 d . . . H19A H 0.5308 0.8325 0.8736 0.060 Uiso 1 1 calc R . . H19B H 0.4052 0.8121 0.9172 0.060 Uiso 1 1 calc R . . H19C H 0.4639 0.9136 0.9198 0.060 Uiso 1 1 calc R . . C20 C 0.3676(2) 0.80138(14) 0.77183(14) 0.0396(5) Uani 1 1 d . . . H20A H 0.3261 0.7528 0.8011 0.059 Uiso 1 1 calc R . . H20B H 0.4481 0.7791 0.7556 0.059 Uiso 1 1 calc R . . H20C H 0.3185 0.8170 0.7269 0.059 Uiso 1 1 calc R . . C21 C 0.44969(19) 0.95437(13) 0.77513(12) 0.0288(5) Uani 1 1 d . . . H21A H 0.4167 0.9557 0.7227 0.035 Uiso 1 1 calc R . . H21B H 0.5368 0.9359 0.7720 0.035 Uiso 1 1 calc R . . C22 C 0.44196(17) 1.05088(13) 0.80857(13) 0.0280(5) Uani 1 1 d . . . H22A H 0.4704 1.0491 0.8621 0.034 Uiso 1 1 calc R . . H22B H 0.4974 1.0925 0.7799 0.034 Uiso 1 1 calc R . . C23 C 0.2813(2) 1.11117(15) 0.72806(11) 0.0320(5) Uani 1 1 d . . . H23A H 0.2813 1.0544 0.6974 0.048 Uiso 1 1 calc R . . H23B H 0.3395 1.1556 0.7064 0.048 Uiso 1 1 calc R . . H23C H 0.1991 1.1383 0.7279 0.048 Uiso 1 1 calc R . . C24 C 0.3126(2) 1.17371(13) 0.85251(12) 0.0323(5) Uani 1 1 d . . . H24A H 0.2293 1.1988 0.8520 0.049 Uiso 1 1 calc R . . H24B H 0.3693 1.2196 0.8314 0.049 Uiso 1 1 calc R . . H24C H 0.3363 1.1592 0.9050 0.049 Uiso 1 1 calc R . . H15 H 0.2532(18) 0.9469(14) 1.0332(12) 0.023(6) Uiso 1 1 d . . . H17 H 0.305(2) 1.2184(17) 1.0699(14) 0.052(7) Uiso 1 1 d . . . H16 H 0.406(2) 1.0559(17) 1.0777(14) 0.051(8) Uiso 1 1 d . . . H18A H -0.010(3) 1.2002(18) 1.0100(16) 0.074(9) Uiso 1 1 d . . . H18B H 0.083(3) 1.268(2) 1.053(2) 0.094(11) Uiso 1 1 d . . . H18C H 0.095(3) 1.2468(19) 0.9656(18) 0.064(9) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.01868(8) 0.01826(8) 0.01849(8) -0.00085(9) -0.00005(8) 0.00039(10) Na1 0.0199(3) 0.0236(4) 0.0239(4) 0.0006(3) 0.0022(3) -0.0012(3) N1 0.0224(8) 0.0190(7) 0.0178(7) -0.0010(6) -0.0014(6) -0.0014(6) N2 0.0264(8) 0.0317(8) 0.0297(10) -0.0089(7) 0.0037(7) -0.0082(7) N3 0.0238(8) 0.0235(8) 0.0328(9) 0.0046(7) 0.0031(8) 0.0030(7) N4 0.0252(8) 0.0192(7) 0.0243(9) 0.0003(6) 0.0021(7) 0.0001(6) C1 0.0233(8) 0.0236(8) 0.0223(8) -0.0029(10) 0.0041(7) 0.0009(10) C2 0.0347(12) 0.0285(10) 0.0279(12) -0.0048(9) 0.0088(10) 0.0012(9) C3 0.0505(14) 0.0280(10) 0.0271(12) -0.0002(9) 0.0087(11) 0.0022(10) C4 0.0229(8) 0.0417(11) 0.0341(10) -0.0051(12) 0.0080(8) -0.0016(10) C5 0.0224(9) 0.0319(10) 0.0183(9) 0.0017(8) -0.0007(8) -0.0045(7) C6 0.0337(11) 0.0484(12) 0.0187(10) 0.0001(9) 0.0014(9) -0.0106(11) C7 0.0498(14) 0.0484(12) 0.0265(11) -0.0140(9) 0.0088(12) -0.0128(12) C8 0.0410(11) 0.0290(9) 0.0377(12) -0.0123(9) 0.0128(12) -0.0054(10) C9 0.0265(10) 0.0203(8) 0.0248(10) -0.0053(7) 0.0044(8) -0.0041(7) C10 0.0345(11) 0.0313(10) 0.0303(11) 0.0111(8) -0.0030(10) 0.0014(10) C11 0.0236(10) 0.0535(13) 0.0279(11) 0.0079(10) -0.0034(9) -0.0043(9) C12 0.0348(11) 0.0205(9) 0.0394(12) 0.0029(9) 0.0015(10) 0.0017(8) C13 0.0348(11) 0.0257(10) 0.0332(11) -0.0015(9) 0.0035(10) -0.0086(9) C14 0.0248(9) 0.0286(9) 0.0202(9) -0.0022(9) 0.0008(9) -0.0039(7) C15 0.0294(9) 0.0379(12) 0.0230(10) -0.0005(11) -0.0013(7) 0.0003(10) C16 0.0238(11) 0.0733(17) 0.0265(12) -0.0011(11) -0.0062(9) -0.0074(11) C17 0.0327(12) 0.0533(14) 0.0297(12) -0.0138(11) 0.0023(10) -0.0180(11) C18 0.0385(12) 0.0266(10) 0.0579(16) -0.0078(12) 0.0129(13) -0.0026(9) C19 0.0335(12) 0.0415(11) 0.0446(13) 0.0109(10) -0.0022(11) 0.0058(10) C20 0.0385(12) 0.0276(11) 0.0526(15) -0.0039(10) 0.0050(11) 0.0054(10) C21 0.0222(11) 0.0311(10) 0.0332(11) 0.0038(9) 0.0061(9) 0.0024(8) C22 0.0205(10) 0.0299(10) 0.0337(12) 0.0035(9) 0.0004(9) -0.0056(8) C23 0.0339(11) 0.0330(11) 0.0291(11) 0.0034(9) 0.0022(9) 0.0009(9) C24 0.0376(12) 0.0245(10) 0.0349(12) -0.0029(9) 0.0048(10) -0.0051(9) _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 N1 2.0048(15) . ? Zn1 C1 2.0363(16) . ? Zn1 C14 2.0527(18) . ? Zn1 Na1 3.1790(7) . ? Na1 N1 2.4156(16) . ? Na1 N4 2.4549(17) . ? Na1 N3 2.5541(17) . ? Na1 C14 2.772(2) . ? Na1 C15 2.831(2) . ? Na1 C22 3.105(2) . ? N1 C5 1.471(2) . ? N1 C9 1.476(2) . ? N2 C17 1.374(3) . ? N2 C14 1.389(2) . ? N2 C18 1.447(3) . ? N3 C20 1.463(3) . ? N3 C19 1.471(3) . ? N3 C21 1.478(3) . ? N4 C23 1.464(3) . ? N4 C24 1.467(2) . ? N4 C22 1.474(2) . ? C1 C4 1.527(2) . ? C1 C3 1.531(3) . ? C1 C2 1.531(3) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 C10 1.529(3) . ? C5 C6 1.544(3) . ? C5 C11 1.552(3) . ? C6 C7 1.520(3) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.528(3) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.540(3) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C12 1.530(3) . ? C9 C13 1.546(3) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? 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 . ? C14 C15 1.389(3) . ? C15 C16 1.415(3) . ? C15 H15 0.886(19) . ? C16 C17 1.352(4) . ? C16 H16 0.91(3) . ? C17 H17 0.97(3) . ? C18 H18A 1.00(3) . ? C18 H18B 0.95(4) . ? C18 H18C 0.95(3) . ? 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 C22 1.514(3) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 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 N1 Zn1 C1 129.87(7) . . ? N1 Zn1 C14 108.85(7) . . ? C1 Zn1 C14 120.86(7) . . ? N1 Zn1 Na1 49.43(4) . . ? C1 Zn1 Na1 175.64(6) . . ? C14 Zn1 Na1 59.45(6) . . ? N1 Na1 N4 134.88(6) . . ? N1 Na1 N3 129.27(6) . . ? N4 Na1 N3 75.22(5) . . ? N1 Na1 C14 78.68(5) . . ? N4 Na1 C14 106.62(6) . . ? N3 Na1 C14 139.74(6) . . ? N1 Na1 C15 97.99(6) . . ? N4 Na1 C15 106.85(7) . . ? N3 Na1 C15 111.26(6) . . ? C14 Na1 C15 28.67(6) . . ? N1 Na1 C22 158.92(6) . . ? N4 Na1 C22 27.73(5) . . ? N3 Na1 C22 51.45(5) . . ? C14 Na1 C22 114.03(6) . . ? C15 Na1 C22 100.43(6) . . ? N1 Na1 Zn1 39.08(4) . . ? N4 Na1 Zn1 129.22(4) . . ? N3 Na1 Zn1 155.25(4) . . ? C14 Na1 Zn1 39.62(4) . . ? C15 Na1 Zn1 62.08(4) . . ? C22 Na1 Zn1 149.79(4) . . ? C5 N1 C9 116.78(14) . . ? C5 N1 Zn1 113.81(11) . . ? C9 N1 Zn1 117.28(11) . . ? C5 N1 Na1 105.77(10) . . ? C9 N1 Na1 107.51(11) . . ? Zn1 N1 Na1 91.49(6) . . ? C17 N2 C14 111.17(18) . . ? C17 N2 C18 123.57(19) . . ? C14 N2 C18 125.13(17) . . ? C20 N3 C19 108.90(16) . . ? C20 N3 C21 108.38(17) . . ? C19 N3 C21 110.50(16) . . ? C20 N3 Na1 123.22(13) . . ? C19 N3 Na1 100.73(12) . . ? C21 N3 Na1 104.64(11) . . ? C23 N4 C24 109.24(15) . . ? C23 N4 C22 110.72(16) . . ? C24 N4 C22 109.07(16) . . ? C23 N4 Na1 119.75(12) . . ? C24 N4 Na1 106.00(11) . . ? C22 N4 Na1 101.48(11) . . ? C4 C1 C3 107.51(18) . . ? C4 C1 C2 107.95(16) . . ? C3 C1 C2 107.73(15) . . ? C4 C1 Zn1 118.25(12) . . ? C3 C1 Zn1 105.35(13) . . ? C2 C1 Zn1 109.59(13) . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C1 C4 H4A 109.5 . . ? C1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N1 C5 C10 107.50(16) . . ? N1 C5 C6 110.12(15) . . ? C10 C5 C6 108.93(16) . . ? N1 C5 C11 116.13(16) . . ? C10 C5 C11 105.25(16) . . ? C6 C5 C11 108.63(17) . . ? C7 C6 C5 111.56(16) . . ? C7 C6 H6A 109.3 . . ? C5 C6 H6A 109.3 . . ? C7 C6 H6B 109.3 . . ? C5 C6 H6B 109.3 . . ? H6A C6 H6B 108.0 . . ? C6 C7 C8 110.45(17) . . ? C6 C7 H7A 109.6 . . ? C8 C7 H7A 109.6 . . ? C6 C7 H7B 109.6 . . ? C8 C7 H7B 109.6 . . ? H7A C7 H7B 108.1 . . ? C7 C8 C9 113.10(17) . . ? C7 C8 H8A 109.0 . . ? C9 C8 H8A 109.0 . . ? C7 C8 H8B 109.0 . . ? C9 C8 H8B 109.0 . . ? H8A C8 H8B 107.8 . . ? N1 C9 C12 107.04(15) . . ? N1 C9 C8 110.28(15) . . ? C12 C9 C8 108.13(17) . . ? N1 C9 C13 115.35(15) . . ? C12 C9 C13 106.14(16) . . ? C8 C9 C13 109.58(16) . . ? C5 C10 H10A 109.5 . . ? C5 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C5 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C5 C11 H11A 109.5 . . ? C5 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C5 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C9 C12 H12A 109.5 . . ? C9 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C9 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C9 C13 H13A 109.5 . . ? C9 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C9 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C15 C14 N2 103.96(17) . . ? C15 C14 Zn1 128.53(15) . . ? N2 C14 Zn1 126.92(13) . . ? C15 C14 Na1 78.01(11) . . ? N2 C14 Na1 122.03(13) . . ? Zn1 C14 Na1 80.94(6) . . ? C14 C15 C16 110.0(2) . . ? C14 C15 Na1 73.32(11) . . ? C16 C15 Na1 123.81(14) . . ? C14 C15 H15 124.3(13) . . ? C16 C15 H15 125.5(13) . . ? Na1 C15 H15 79.3(14) . . ? C17 C16 C15 106.7(2) . . ? C17 C16 H16 130.5(16) . . ? C15 C16 H16 122.7(16) . . ? C16 C17 N2 108.1(2) . . ? C16 C17 H17 132.4(15) . . ? N2 C17 H17 119.4(15) . . ? N2 C18 H18A 111.7(16) . . ? N2 C18 H18B 110(2) . . ? H18A C18 H18B 110(2) . . ? N2 C18 H18C 110.1(17) . . ? H18A C18 H18C 104(2) . . ? H18B C18 H18C 111(3) . . ? N3 C19 H19A 109.5 . . ? N3 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? N3 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? N3 C20 H20A 109.5 . . ? N3 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? N3 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? N3 C21 C22 113.74(16) . . ? N3 C21 H21A 108.8 . . ? C22 C21 H21A 108.8 . . ? N3 C21 H21B 108.8 . . ? C22 C21 H21B 108.8 . . ? H21A C21 H21B 107.7 . . ? N4 C22 C21 112.68(17) . . ? N4 C22 Na1 50.79(9) . . ? C21 C22 Na1 81.94(11) . . ? N4 C22 H22A 109.1 . . ? C21 C22 H22A 109.1 . . ? Na1 C22 H22A 83.2 . . ? N4 C22 H22B 109.1 . . ? C21 C22 H22B 109.1 . . ? Na1 C22 H22B 159.8 . . ? H22A C22 H22B 107.8 . . ? 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 H24A 109.5 . . ? N4 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? N4 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 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 C1 Zn1 Na1 N1 82.6(7) . . . . ? C14 Zn1 Na1 N1 177.92(8) . . . . ? N1 Zn1 Na1 N4 116.09(8) . . . . ? C1 Zn1 Na1 N4 -161.3(7) . . . . ? C14 Zn1 Na1 N4 -65.98(8) . . . . ? N1 Zn1 Na1 N3 -74.16(12) . . . . ? C1 Zn1 Na1 N3 8.4(7) . . . . ? C14 Zn1 Na1 N3 103.76(13) . . . . ? N1 Zn1 Na1 C14 -177.92(8) . . . . ? C1 Zn1 Na1 C14 -95.3(7) . . . . ? N1 Zn1 Na1 C15 -154.42(8) . . . . ? C1 Zn1 Na1 C15 -71.8(7) . . . . ? C14 Zn1 Na1 C15 23.50(8) . . . . ? N1 Zn1 Na1 C22 145.76(11) . . . . ? C1 Zn1 Na1 C22 -131.7(7) . . . . ? C14 Zn1 Na1 C22 -36.32(11) . . . . ? C1 Zn1 N1 C5 77.67(14) . . . . ? C14 Zn1 N1 C5 -109.87(12) . . . . ? Na1 Zn1 N1 C5 -107.98(12) . . . . ? C1 Zn1 N1 C9 -63.75(16) . . . . ? C14 Zn1 N1 C9 108.72(13) . . . . ? Na1 Zn1 N1 C9 110.61(13) . . . . ? C1 Zn1 N1 Na1 -174.36(8) . . . . ? C14 Zn1 N1 Na1 -1.89(7) . . . . ? N4 Na1 N1 C5 14.36(14) . . . . ? N3 Na1 N1 C5 -96.08(12) . . . . ? C14 Na1 N1 C5 116.62(11) . . . . ? C15 Na1 N1 C5 137.93(12) . . . . ? C22 Na1 N1 C5 -12.8(2) . . . . ? Zn1 Na1 N1 C5 115.27(12) . . . . ? N4 Na1 N1 C9 139.81(11) . . . . ? N3 Na1 N1 C9 29.37(14) . . . . ? C14 Na1 N1 C9 -117.93(12) . . . . ? C15 Na1 N1 C9 -96.62(12) . . . . ? C22 Na1 N1 C9 112.63(17) . . . . ? Zn1 Na1 N1 C9 -119.28(13) . . . . ? N4 Na1 N1 Zn1 -100.91(8) . . . . ? N3 Na1 N1 Zn1 148.65(6) . . . . ? C14 Na1 N1 Zn1 1.35(5) . . . . ? C15 Na1 N1 Zn1 22.66(7) . . . . ? C22 Na1 N1 Zn1 -128.09(15) . . . . ? N1 Na1 N3 C20 11.48(19) . . . . ? N4 Na1 N3 C20 -125.15(16) . . . . ? C14 Na1 N3 C20 136.44(15) . . . . ? C15 Na1 N3 C20 132.20(16) . . . . ? C22 Na1 N3 C20 -141.34(18) . . . . ? Zn1 Na1 N3 C20 63.1(2) . . . . ? N1 Na1 N3 C19 -109.72(13) . . . . ? N4 Na1 N3 C19 113.65(12) . . . . ? C14 Na1 N3 C19 15.24(16) . . . . ? C15 Na1 N3 C19 11.00(13) . . . . ? C22 Na1 N3 C19 97.46(13) . . . . ? Zn1 Na1 N3 C19 -58.15(18) . . . . ? N1 Na1 N3 C21 135.59(12) . . . . ? N4 Na1 N3 C21 -1.05(12) . . . . ? C14 Na1 N3 C21 -99.46(14) . . . . ? C15 Na1 N3 C21 -103.70(13) . . . . ? C22 Na1 N3 C21 -17.23(11) . . . . ? Zn1 Na1 N3 C21 -172.85(11) . . . . ? N1 Na1 N4 C23 -37.19(17) . . . . ? N3 Na1 N4 C23 94.19(14) . . . . ? C14 Na1 N4 C23 -127.66(13) . . . . ? C15 Na1 N4 C23 -157.63(13) . . . . ? C22 Na1 N4 C23 122.13(19) . . . . ? Zn1 Na1 N4 C23 -90.23(14) . . . . ? N1 Na1 N4 C24 86.78(14) . . . . ? N3 Na1 N4 C24 -141.84(13) . . . . ? C14 Na1 N4 C24 -3.69(14) . . . . ? C15 Na1 N4 C24 -33.66(14) . . . . ? C22 Na1 N4 C24 -113.90(18) . . . . ? Zn1 Na1 N4 C24 33.74(14) . . . . ? N1 Na1 N4 C22 -159.32(11) . . . . ? N3 Na1 N4 C22 -27.94(12) . . . . ? C14 Na1 N4 C22 110.21(12) . . . . ? C15 Na1 N4 C22 80.24(12) . . . . ? Zn1 Na1 N4 C22 147.64(10) . . . . ? N1 Zn1 C1 C4 -29.4(2) . . . . ? C14 Zn1 C1 C4 158.94(15) . . . . ? Na1 Zn1 C1 C4 -108.3(6) . . . . ? N1 Zn1 C1 C3 90.75(14) . . . . ? C14 Zn1 C1 C3 -80.94(15) . . . . ? Na1 Zn1 C1 C3 11.8(8) . . . . ? N1 Zn1 C1 C2 -153.60(12) . . . . ? C14 Zn1 C1 C2 34.71(16) . . . . ? Na1 Zn1 C1 C2 127.5(7) . . . . ? C9 N1 C5 C10 -172.65(15) . . . . ? Zn1 N1 C5 C10 45.73(17) . . . . ? Na1 N1 C5 C10 -53.14(16) . . . . ? C9 N1 C5 C6 -54.1(2) . . . . ? Zn1 N1 C5 C6 164.26(12) . . . . ? Na1 N1 C5 C6 65.40(15) . . . . ? C9 N1 C5 C11 69.8(2) . . . . ? Zn1 N1 C5 C11 -71.77(18) . . . . ? Na1 N1 C5 C11 -170.64(14) . . . . ? N1 C5 C6 C7 54.3(2) . . . . ? C10 C5 C6 C7 171.92(19) . . . . ? C11 C5 C6 C7 -73.9(2) . . . . ? C5 C6 C7 C8 -54.8(3) . . . . ? C6 C7 C8 C9 53.2(2) . . . . ? C5 N1 C9 C12 169.22(15) . . . . ? Zn1 N1 C9 C12 -50.52(18) . . . . ? Na1 N1 C9 C12 50.63(16) . . . . ? C5 N1 C9 C8 51.8(2) . . . . ? Zn1 N1 C9 C8 -167.91(13) . . . . ? Na1 N1 C9 C8 -66.76(17) . . . . ? C5 N1 C9 C13 -72.9(2) . . . . ? Zn1 N1 C9 C13 67.32(19) . . . . ? Na1 N1 C9 C13 168.47(13) . . . . ? C7 C8 C9 N1 -50.1(2) . . . . ? C7 C8 C9 C12 -166.83(17) . . . . ? C7 C8 C9 C13 77.9(2) . . . . ? C17 N2 C14 C15 -0.5(2) . . . . ? C18 N2 C14 C15 175.5(2) . . . . ? C17 N2 C14 Zn1 171.37(15) . . . . ? C18 N2 C14 Zn1 -12.7(3) . . . . ? C17 N2 C14 Na1 -84.88(19) . . . . ? C18 N2 C14 Na1 91.1(2) . . . . ? N1 Zn1 C14 C15 -65.00(19) . . . . ? C1 Zn1 C14 C15 108.27(19) . . . . ? Na1 Zn1 C14 C15 -66.67(17) . . . . ? N1 Zn1 C14 N2 125.17(17) . . . . ? C1 Zn1 C14 N2 -61.6(2) . . . . ? Na1 Zn1 C14 N2 123.50(19) . . . . ? N1 Zn1 C14 Na1 1.67(7) . . . . ? C1 Zn1 C14 Na1 174.94(7) . . . . ? N1 Na1 C14 C15 131.42(13) . . . . ? N4 Na1 C14 C15 -94.85(13) . . . . ? N3 Na1 C14 C15 -8.26(16) . . . . ? C22 Na1 C14 C15 -66.29(13) . . . . ? Zn1 Na1 C14 C15 132.75(14) . . . . ? N1 Na1 C14 N2 -129.49(15) . . . . ? N4 Na1 C14 N2 4.24(16) . . . . ? N3 Na1 C14 N2 90.83(16) . . . . ? C15 Na1 C14 N2 99.09(19) . . . . ? C22 Na1 C14 N2 32.80(16) . . . . ? Zn1 Na1 C14 N2 -128.16(17) . . . . ? N1 Na1 C14 Zn1 -1.33(5) . . . . ? N4 Na1 C14 Zn1 132.40(6) . . . . ? N3 Na1 C14 Zn1 -141.01(7) . . . . ? C15 Na1 C14 Zn1 -132.75(14) . . . . ? C22 Na1 C14 Zn1 160.96(6) . . . . ? N2 C14 C15 C16 0.2(2) . . . . ? Zn1 C14 C15 C16 -171.42(16) . . . . ? Na1 C14 C15 C16 120.60(16) . . . . ? N2 C14 C15 Na1 -120.39(14) . . . . ? Zn1 C14 C15 Na1 67.97(15) . . . . ? N1 Na1 C15 C14 -47.95(13) . . . . ? N4 Na1 C15 C14 93.96(12) . . . . ? N3 Na1 C15 C14 174.28(11) . . . . ? C22 Na1 C15 C14 121.76(12) . . . . ? Zn1 Na1 C15 C14 -32.00(10) . . . . ? N1 Na1 C15 C16 -151.19(19) . . . . ? N4 Na1 C15 C16 -9.3(2) . . . . ? N3 Na1 C15 C16 71.0(2) . . . . ? C14 Na1 C15 C16 -103.2(3) . . . . ? C22 Na1 C15 C16 18.5(2) . . . . ? Zn1 Na1 C15 C16 -135.2(2) . . . . ? C14 C15 C16 C17 0.1(3) . . . . ? Na1 C15 C16 C17 83.0(2) . . . . ? C15 C16 C17 N2 -0.4(3) . . . . ? C14 N2 C17 C16 0.5(3) . . . . ? C18 N2 C17 C16 -175.5(2) . . . . ? C20 N3 C21 C22 164.38(17) . . . . ? C19 N3 C21 C22 -76.4(2) . . . . ? Na1 N3 C21 C22 31.26(19) . . . . ? C23 N4 C22 C21 -70.7(2) . . . . ? C24 N4 C22 C21 169.09(16) . . . . ? Na1 N4 C22 C21 57.51(16) . . . . ? C23 N4 C22 Na1 -128.19(16) . . . . ? C24 N4 C22 Na1 111.58(15) . . . . ? N3 C21 C22 N4 -66.0(2) . . . . ? N3 C21 C22 Na1 -24.65(15) . . . . ? N1 Na1 C22 N4 44.1(2) . . . . ? N3 Na1 C22 N4 144.60(15) . . . . ? C14 Na1 C22 N4 -79.92(13) . . . . ? C15 Na1 C22 N4 -106.45(12) . . . . ? Zn1 Na1 C22 N4 -55.50(16) . . . . ? N1 Na1 C22 C21 -84.12(19) . . . . ? N4 Na1 C22 C21 -128.19(18) . . . . ? N3 Na1 C22 C21 16.41(11) . . . . ? C14 Na1 C22 C21 151.89(11) . . . . ? C15 Na1 C22 C21 125.36(12) . . . . ? Zn1 Na1 C22 C21 176.32(10) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.312 _refine_diff_density_min -0.218 _refine_diff_density_rms 0.042 #===END