# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email R.E.MULVEY@STRATH.AC.UK _publ_contact_author_name R.E.Mulvey loop_ _publ_author_name 'Jennifer Garden' A.R.Kennedy R.E.Mulvey 'Stuart Robertson' data_srjg06 _database_code_depnum_ccdc_archive 'CCDC 837241' #TrackingRef '- combined.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C14 H29 N3 Zn, C4 H5 N' _chemical_formula_sum 'C18 H34 N4 Zn' _chemical_formula_weight 371.86 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 Pna21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z+1/2' _cell_length_a 15.6099(2) _cell_length_b 9.65630(10) _cell_length_c 27.2685(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4110.29(9) _cell_formula_units_Z 8 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 31347 _cell_measurement_theta_min 2.7089 _cell_measurement_theta_max 29.1454 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.202 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1600 _exptl_absorpt_coefficient_mu 1.200 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.81230 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET) (compiled Apr 28 2010,14:27:37) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Sapphire3, Gemini' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 48155 _diffrn_reflns_av_R_equivalents 0.0214 _diffrn_reflns_av_sigmaI/netI 0.0236 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 2.71 _diffrn_reflns_theta_max 29.21 _reflns_number_total 10490 _reflns_number_gt 9180 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET) (compiled Apr 28 2010,14:27:37) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET) (compiled Apr 28 2010,14:27:37) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET) (compiled Apr 28 2010,14:27:37) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _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^)+(0.0354P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment 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 0.294(7) _refine_ls_number_reflns 10490 _refine_ls_number_parameters 438 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0299 _refine_ls_R_factor_gt 0.0241 _refine_ls_wR_factor_ref 0.0573 _refine_ls_wR_factor_gt 0.0564 _refine_ls_goodness_of_fit_ref 1.010 _refine_ls_restrained_S_all 1.010 _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 0.859042(13) 0.23000(2) 0.879110(7) 0.01761(6) Uani 1 1 d . . . Zn2 Zn 0.605340(13) 0.76903(2) 0.683922(7) 0.01823(6) Uani 1 1 d . . . N1 N 0.79374(9) 0.35766(15) 0.92338(6) 0.0202(3) Uani 1 1 d . . . N2 N 0.83140(9) 0.02512(15) 0.90913(7) 0.0224(3) Uani 1 1 d . . . N3 N 0.98516(9) 0.19844(15) 0.91202(6) 0.0205(3) Uani 1 1 d . . . N4 N 0.66228(11) 0.38461(16) 0.60540(7) 0.0257(3) Uani 1 1 d . . . N5 N 0.53985(9) 0.64560(15) 0.63943(6) 0.0198(3) Uani 1 1 d . . . N6 N 0.73103(9) 0.80354(15) 0.65090(6) 0.0214(3) Uani 1 1 d . . . N7 N 0.57737(9) 0.97692(15) 0.65680(7) 0.0244(3) Uani 1 1 d . . . N8 N 0.91536(11) 0.61752(16) 0.95763(7) 0.0291(4) Uani 1 1 d . . . C1 C 0.75233(11) 0.4728(2) 0.90632(8) 0.0230(4) Uani 1 1 d . . . H1 H 0.7504 0.5006 0.8729 0.028 Uiso 1 1 calc R . . C2 C 0.71387(12) 0.5427(2) 0.94448(9) 0.0308(5) Uani 1 1 d . . . H2 H 0.6819 0.6262 0.9423 0.037 Uiso 1 1 calc R . . C3 C 0.73113(12) 0.4666(2) 0.98720(8) 0.0326(5) Uani 1 1 d . . . H3 H 0.7128 0.4878 1.0196 0.039 Uiso 1 1 calc R . . C4 C 0.77989(12) 0.3553(2) 0.97289(7) 0.0264(4) Uani 1 1 d . . . H4 H 0.8011 0.2861 0.9945 0.032 Uiso 1 1 calc R . . C5 C 0.84886(18) 0.2571(2) 0.80649(16) 0.0273(8) Uani 1 1 d . . . C6 C 0.89790(15) 0.1528(3) 0.77350(9) 0.0427(6) Uani 1 1 d . . . H6A H 0.8898 0.1778 0.7390 0.064 Uiso 1 1 calc R . . H6B H 0.8758 0.0592 0.7792 0.064 Uiso 1 1 calc R . . H6C H 0.9591 0.1556 0.7815 0.064 Uiso 1 1 calc R . . C7 C 0.75441(19) 0.24749(18) 0.79134(12) 0.0283(8) Uani 1 1 d . . . H7A H 0.7493 0.2641 0.7560 0.042 Uiso 1 1 calc R . . H7B H 0.7212 0.3173 0.8092 0.042 Uiso 1 1 calc R . . H7C H 0.7324 0.1550 0.7991 0.042 Uiso 1 1 calc R . . C8 C 0.88170(13) 0.4015(2) 0.79159(9) 0.0299(5) Uani 1 1 d . . . H8A H 0.8713 0.4162 0.7565 0.045 Uiso 1 1 calc R . . H8B H 0.9433 0.4078 0.7982 0.045 Uiso 1 1 calc R . . H8C H 0.8514 0.4725 0.8105 0.045 Uiso 1 1 calc R . . C10 C 0.83247(14) -0.07869(19) 0.86889(8) 0.0342(5) Uani 1 1 d . . . H10A H 0.8206 -0.1708 0.8824 0.051 Uiso 1 1 calc R . . H10B H 0.8889 -0.0788 0.8532 0.051 Uiso 1 1 calc R . . H10C H 0.7886 -0.0549 0.8446 0.051 Uiso 1 1 calc R . . C11 C 0.74791(13) 0.0121(2) 0.93424(9) 0.0342(5) Uani 1 1 d . . . H11A H 0.7422 -0.0814 0.9478 0.051 Uiso 1 1 calc R . . H11B H 0.7016 0.0292 0.9107 0.051 Uiso 1 1 calc R . . H11C H 0.7446 0.0801 0.9609 0.051 Uiso 1 1 calc R . . C12 C 0.90256(11) -0.0012(2) 0.94366(8) 0.0245(4) Uani 1 1 d . . . H12A H 0.9059 -0.1016 0.9508 0.029 Uiso 1 1 calc R . . H12B H 0.8914 0.0479 0.9749 0.029 Uiso 1 1 calc R . . C13 C 0.98716(11) 0.04759(18) 0.92247(7) 0.0224(4) Uani 1 1 d . . . H13A H 1.0338 0.0275 0.9460 0.027 Uiso 1 1 calc R . . H13B H 0.9992 -0.0037 0.8918 0.027 Uiso 1 1 calc R . . C14 C 1.05496(13) 0.2343(2) 0.87854(17) 0.0307(6) Uani 1 1 d . . . H14A H 1.1098 0.2081 0.8933 0.046 Uiso 1 1 calc R . . H14B H 1.0543 0.3342 0.8723 0.046 Uiso 1 1 calc R . . H14C H 1.0474 0.1845 0.8475 0.046 Uiso 1 1 calc R . . C15 C 0.99988(16) 0.2779(2) 0.95828(10) 0.0276(5) Uani 1 1 d . . . H15A H 1.0552 0.2512 0.9724 0.041 Uiso 1 1 calc R . . H15B H 0.9540 0.2572 0.9817 0.041 Uiso 1 1 calc R . . H15C H 1.0001 0.3773 0.9510 0.041 Uiso 1 1 calc R . . C16 C 0.70500(11) 0.37448(19) 0.64881(8) 0.0257(4) Uani 1 1 d . . . H16 H 0.6825 0.3957 0.6803 0.031 Uiso 1 1 calc R . . C17 C 0.78599(12) 0.3284(2) 0.63909(7) 0.0272(4) Uani 1 1 d . . . H17 H 0.8299 0.3111 0.6624 0.033 Uiso 1 1 calc R . . C18 C 0.79213(13) 0.3113(2) 0.58816(8) 0.0342(5) Uani 1 1 d . . . H18 H 0.8413 0.2808 0.5707 0.041 Uiso 1 1 calc R . . C19 C 0.71507(12) 0.3460(2) 0.56798(8) 0.0318(4) Uani 1 1 d . . . H19 H 0.7008 0.3438 0.5341 0.038 Uiso 1 1 calc R . . C21 C 0.52476(12) 0.6478(2) 0.58974(7) 0.0260(4) Uani 1 1 d . . . H21 H 0.5450 0.7172 0.5679 0.031 Uiso 1 1 calc R . . C22 C 0.47615(12) 0.5350(2) 0.57599(8) 0.0321(4) Uani 1 1 d . . . H22 H 0.4573 0.5132 0.5438 0.039 Uiso 1 1 calc R . . C23 C 0.45989(12) 0.4587(2) 0.61874(8) 0.0301(4) Uani 1 1 d . . . H23 H 0.4278 0.3754 0.6212 0.036 Uiso 1 1 calc R . . C24 C 0.49967(12) 0.52826(19) 0.65633(9) 0.0235(4) Uani 1 1 d . . . H24 H 0.4994 0.4991 0.6896 0.028 Uiso 1 1 calc R . . C25 C 0.59852(17) 0.7368(2) 0.75775(13) 0.0243(7) Uani 1 1 d . . . C26 C 0.50349(19) 0.7394(3) 0.77259(13) 0.0360(9) Uani 1 1 d . . . H26A H 0.4984 0.7205 0.8078 0.054 Uiso 1 1 calc R . . H26B H 0.4722 0.6686 0.7541 0.054 Uiso 1 1 calc R . . H26C H 0.4793 0.8309 0.7654 0.054 Uiso 1 1 calc R . . C27 C 0.64636(17) 0.8438(3) 0.78824(10) 0.0527(8) Uani 1 1 d . . . H27A H 0.6434 0.8181 0.8230 0.079 Uiso 1 1 calc R . . H27B H 0.6201 0.9350 0.7836 0.079 Uiso 1 1 calc R . . H27C H 0.7064 0.8471 0.7778 0.079 Uiso 1 1 calc R . . C28 C 0.63388(15) 0.5932(3) 0.77030(10) 0.0416(6) Uani 1 1 d . . . H28A H 0.6311 0.5788 0.8058 0.062 Uiso 1 1 calc R . . H28B H 0.6936 0.5866 0.7594 0.062 Uiso 1 1 calc R . . H28C H 0.5996 0.5222 0.7537 0.062 Uiso 1 1 calc R . . C30 C 0.80221(14) 0.7656(2) 0.68549(18) 0.0333(6) Uani 1 1 d . . . H30A H 0.8575 0.7864 0.6702 0.050 Uiso 1 1 calc R . . H30B H 0.7991 0.6665 0.6930 0.050 Uiso 1 1 calc R . . H30C H 0.7964 0.8191 0.7158 0.050 Uiso 1 1 calc R . . C31 C 0.74503(16) 0.7293(2) 0.60505(11) 0.0276(5) Uani 1 1 d . . . H31A H 0.8013 0.7539 0.5917 0.041 Uiso 1 1 calc R . . H31B H 0.7003 0.7546 0.5815 0.041 Uiso 1 1 calc R . . H31C H 0.7429 0.6293 0.6112 0.041 Uiso 1 1 calc R . . C32 C 0.73310(11) 0.95510(19) 0.64197(8) 0.0248(4) Uani 1 1 d . . . H32A H 0.7793 0.9770 0.6183 0.030 Uiso 1 1 calc R . . H32B H 0.7458 1.0039 0.6731 0.030 Uiso 1 1 calc R . . C33 C 0.64809(11) 1.0054(2) 0.62182(8) 0.0245(4) Uani 1 1 d . . . H33A H 0.6514 1.1062 0.6155 0.029 Uiso 1 1 calc R . . H33B H 0.6361 0.9583 0.5903 0.029 Uiso 1 1 calc R . . C34 C 0.49399(14) 0.9885(3) 0.63138(11) 0.0373(6) Uani 1 1 d . . . H34A H 0.4861 1.0837 0.6198 0.056 Uiso 1 1 calc R . . H34B H 0.4477 0.9646 0.6542 0.056 Uiso 1 1 calc R . . H34C H 0.4929 0.9250 0.6034 0.056 Uiso 1 1 calc R . . C35 C 0.57807(15) 1.0800(2) 0.69679(9) 0.0398(6) Uani 1 1 d . . . H35A H 0.5684 1.1725 0.6831 0.060 Uiso 1 1 calc R . . H35B H 0.6337 1.0776 0.7135 0.060 Uiso 1 1 calc R . . H35C H 0.5326 1.0582 0.7203 0.060 Uiso 1 1 calc R . . C36 C 0.96688(13) 0.6535(2) 0.99544(8) 0.0327(5) Uani 1 1 d . . . H36 H 0.9516 0.6526 1.0292 0.039 Uiso 1 1 calc R . . C37 C 1.04390(14) 0.6910(3) 0.97698(8) 0.0380(5) Uani 1 1 d . . . H37 H 1.0920 0.7221 0.9953 0.046 Uiso 1 1 calc R . . C38 C 1.03971(12) 0.6756(2) 0.92581(8) 0.0293(4) Uani 1 1 d . . . H38 H 1.0844 0.6935 0.9030 0.035 Uiso 1 1 calc R . . C39 C 0.95988(12) 0.63060(18) 0.91514(8) 0.0258(4) Uani 1 1 d . . . H39 H 0.9385 0.6113 0.8832 0.031 Uiso 1 1 calc R . . H98 H 0.8630(16) 0.598(3) 0.9593(11) 0.070(10) Uiso 1 1 d . . . H99 H 0.6119(12) 0.416(2) 0.5997(7) 0.021(5) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.01839(13) 0.01721(8) 0.01724(14) 0.0008(2) -0.00018(10) 0.00332(8) Zn2 0.01870(13) 0.01870(9) 0.01729(14) 0.0015(2) 0.00112(10) -0.00456(8) N1 0.0187(7) 0.0185(7) 0.0234(8) -0.0014(6) 0.0023(6) 0.0020(6) N2 0.0198(8) 0.0187(7) 0.0288(9) 0.0031(6) -0.0048(7) -0.0003(6) N3 0.0182(7) 0.0190(9) 0.0244(8) 0.0008(6) -0.0002(6) -0.0003(6) N4 0.0178(8) 0.0208(8) 0.0384(10) 0.0023(7) -0.0031(7) 0.0035(7) N5 0.0162(7) 0.0215(7) 0.0216(8) 0.0002(6) -0.0011(6) -0.0025(6) N6 0.0176(7) 0.0223(9) 0.0243(8) 0.0032(6) 0.0000(6) -0.0024(6) N7 0.0170(8) 0.0209(8) 0.0351(10) -0.0010(6) 0.0039(7) -0.0021(6) N8 0.0201(8) 0.0213(8) 0.0459(11) 0.0022(7) 0.0014(8) -0.0015(7) C1 0.0184(9) 0.0234(9) 0.0272(11) -0.0009(8) -0.0029(8) -0.0007(7) C2 0.0169(9) 0.0231(10) 0.0525(14) -0.0087(9) 0.0018(9) 0.0026(8) C3 0.0259(10) 0.0408(11) 0.0310(11) -0.0131(9) 0.0100(9) -0.0047(9) C4 0.0249(10) 0.0304(10) 0.0237(10) 0.0008(8) 0.0040(8) -0.0007(8) C5 0.0284(14) 0.0256(15) 0.028(2) -0.0004(7) 0.0009(11) 0.0056(7) C6 0.0564(16) 0.0485(17) 0.0231(14) -0.0049(11) 0.0012(10) 0.0190(11) C7 0.0373(14) 0.0308(17) 0.0169(17) 0.0026(6) -0.0071(12) -0.0003(8) C8 0.0317(11) 0.0359(12) 0.0220(12) 0.0063(9) 0.0041(9) -0.0015(9) C10 0.0409(11) 0.0221(9) 0.0398(13) -0.0001(8) -0.0174(10) -0.0011(8) C11 0.0222(10) 0.0314(12) 0.0492(15) 0.0078(11) 0.0031(10) -0.0050(9) C12 0.0236(9) 0.0201(9) 0.0298(12) 0.0054(8) -0.0061(8) 0.0015(7) C13 0.0185(9) 0.0183(8) 0.0304(10) 0.0015(7) -0.0039(7) 0.0041(7) C14 0.0215(10) 0.0366(11) 0.0340(15) 0.0083(11) 0.0021(14) 0.0002(7) C15 0.0273(11) 0.0244(8) 0.0310(13) -0.0064(12) -0.0082(9) 0.0017(10) C16 0.0266(10) 0.0226(9) 0.0279(10) -0.0017(7) 0.0069(8) -0.0026(7) C17 0.0241(10) 0.0305(9) 0.0268(10) 0.0071(8) -0.0026(8) 0.0017(8) C18 0.0285(11) 0.0446(13) 0.0295(11) 0.0052(9) 0.0093(8) 0.0119(9) C19 0.0362(11) 0.0380(11) 0.0213(11) 0.0066(8) -0.0010(9) 0.0023(9) C21 0.0248(10) 0.0305(10) 0.0228(10) 0.0005(8) -0.0025(8) 0.0017(8) C22 0.0215(9) 0.0407(11) 0.0341(11) -0.0138(9) -0.0098(9) 0.0029(8) C23 0.0167(9) 0.0286(10) 0.0451(13) -0.0110(9) 0.0011(9) -0.0046(8) C24 0.0177(9) 0.0191(9) 0.0336(11) 0.0007(8) 0.0044(8) -0.0010(7) C25 0.0280(14) 0.0342(14) 0.0109(16) 0.0024(8) 0.0022(10) -0.0100(8) C26 0.0349(15) 0.0364(18) 0.037(2) -0.0032(8) 0.0119(15) -0.0052(9) C27 0.0607(18) 0.078(2) 0.0195(14) -0.0082(13) 0.0020(11) -0.0363(14) C28 0.0358(12) 0.0630(18) 0.0260(14) 0.0170(12) -0.0019(10) 0.0022(11) C30 0.0178(10) 0.0417(12) 0.0403(17) 0.0046(12) -0.0054(14) -0.0005(7) C31 0.0266(11) 0.0252(9) 0.0308(13) 0.0024(11) 0.0081(9) -0.0002(9) C32 0.0208(10) 0.0207(9) 0.0329(11) 0.0019(8) 0.0060(8) -0.0051(8) C33 0.0267(10) 0.0171(9) 0.0298(12) 0.0040(8) 0.0057(8) -0.0005(7) C34 0.0228(10) 0.0280(11) 0.0611(16) 0.0119(11) 0.0041(11) 0.0033(9) C35 0.0449(12) 0.0245(10) 0.0501(15) -0.0085(9) 0.0212(11) -0.0037(9) C36 0.0372(11) 0.0343(11) 0.0265(11) 0.0067(8) 0.0053(9) -0.0013(9) C37 0.0263(11) 0.0625(16) 0.0251(11) 0.0044(10) -0.0069(8) -0.0095(11) C38 0.0247(10) 0.0378(10) 0.0255(10) 0.0040(8) 0.0030(8) -0.0018(8) C39 0.0324(10) 0.0205(8) 0.0244(10) -0.0010(7) -0.0047(8) 0.0014(8) _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 C5 2.004(4) . ? Zn1 N1 2.0040(15) . ? Zn1 N2 2.1841(15) . ? Zn1 N3 2.1850(15) . ? Zn2 N5 1.9843(15) . ? Zn2 C25 2.040(4) . ? Zn2 N7 2.1835(16) . ? Zn2 N6 2.1843(15) . ? N1 C4 1.367(2) . ? N1 C1 1.368(2) . ? N2 C11 1.478(3) . ? N2 C12 1.478(2) . ? N2 C10 1.486(2) . ? N3 C14 1.463(4) . ? N3 C13 1.485(2) . ? N3 C15 1.494(3) . ? N4 C16 1.362(2) . ? N4 C19 1.363(2) . ? N4 H99 0.857(19) . ? N5 C24 1.375(2) . ? N5 C21 1.376(2) . ? N6 C31 1.458(3) . ? N6 C32 1.484(2) . ? N6 C30 1.503(4) . ? N7 C35 1.476(2) . ? N7 C34 1.479(3) . ? N7 C33 1.485(2) . ? N8 C36 1.353(3) . ? N8 C39 1.357(2) . ? N8 H98 0.84(3) . ? C1 C2 1.378(3) . ? C1 H1 0.9500 . ? C2 C3 1.404(3) . ? C2 H2 0.9500 . ? C3 C4 1.373(3) . ? C3 H3 0.9500 . ? C4 H4 0.9500 . ? C5 C7 1.534(4) . ? C5 C8 1.541(3) . ? C5 C6 1.552(4) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? 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 C13 1.516(3) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.366(2) . ? C16 H16 0.9500 . ? C17 C18 1.402(3) . ? C17 H17 0.9500 . ? C18 C19 1.365(3) . ? C18 H18 0.9500 . ? C19 H19 0.9500 . ? C21 C22 1.379(3) . ? C21 H21 0.9500 . ? C22 C23 1.402(3) . ? C22 H22 0.9500 . ? C23 C24 1.374(3) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C25 C27 1.522(4) . ? C25 C28 1.532(4) . ? C25 C26 1.538(4) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 C33 1.516(3) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 C37 1.353(3) . ? C36 H36 0.9500 . ? C37 C38 1.405(3) . ? C37 H37 0.9500 . ? C38 C39 1.352(3) . ? C38 H38 0.9500 . ? C39 H39 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C5 Zn1 N1 118.34(8) . . ? C5 Zn1 N2 118.22(8) . . ? N1 Zn1 N2 103.35(7) . . ? C5 Zn1 N3 119.71(9) . . ? N1 Zn1 N3 107.26(7) . . ? N2 Zn1 N3 84.13(6) . . ? N5 Zn2 C25 119.01(9) . . ? N5 Zn2 N7 104.01(6) . . ? C25 Zn2 N7 117.64(8) . . ? N5 Zn2 N6 107.59(7) . . ? C25 Zn2 N6 118.49(9) . . ? N7 Zn2 N6 84.25(6) . . ? C4 N1 C1 105.93(16) . . ? C4 N1 Zn1 131.68(13) . . ? C1 N1 Zn1 122.39(13) . . ? C11 N2 C12 110.67(16) . . ? C11 N2 C10 107.15(16) . . ? C12 N2 C10 110.25(14) . . ? C11 N2 Zn1 115.14(12) . . ? C12 N2 Zn1 104.23(11) . . ? C10 N2 Zn1 109.39(12) . . ? C14 N3 C13 109.65(14) . . ? C14 N3 C15 106.9(2) . . ? C13 N3 C15 109.78(16) . . ? C14 N3 Zn1 112.44(16) . . ? C13 N3 Zn1 103.57(10) . . ? C15 N3 Zn1 114.43(12) . . ? C16 N4 C19 109.56(16) . . ? C16 N4 H99 129.1(13) . . ? C19 N4 H99 121.1(13) . . ? C24 N5 C21 105.35(16) . . ? C24 N5 Zn2 121.68(13) . . ? C21 N5 Zn2 132.95(13) . . ? C31 N6 C32 109.95(16) . . ? C31 N6 C30 107.9(2) . . ? C32 N6 C30 109.11(15) . . ? C31 N6 Zn2 114.40(13) . . ? C32 N6 Zn2 103.75(10) . . ? C30 N6 Zn2 111.60(17) . . ? C35 N7 C34 107.56(17) . . ? C35 N7 C33 110.14(15) . . ? C34 N7 C33 109.84(17) . . ? C35 N7 Zn2 111.59(13) . . ? C34 N7 Zn2 113.85(12) . . ? C33 N7 Zn2 103.83(10) . . ? C36 N8 C39 108.81(17) . . ? C36 N8 H98 126(2) . . ? C39 N8 H98 125(2) . . ? N1 C1 C2 110.33(18) . . ? N1 C1 H1 124.8 . . ? C2 C1 H1 124.8 . . ? C1 C2 C3 106.65(18) . . ? C1 C2 H2 126.7 . . ? C3 C2 H2 126.7 . . ? C4 C3 C2 106.27(18) . . ? C4 C3 H3 126.9 . . ? C2 C3 H3 126.9 . . ? N1 C4 C3 110.81(18) . . ? N1 C4 H4 124.6 . . ? C3 C4 H4 124.6 . . ? C7 C5 C8 107.7(2) . . ? C7 C5 C6 106.2(3) . . ? C8 C5 C6 105.7(2) . . ? C7 C5 Zn1 109.6(2) . . ? C8 C5 Zn1 110.6(2) . . ? C6 C5 Zn1 116.68(19) . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C5 C7 H7A 109.5 . . ? C5 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C5 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C5 C8 H8A 109.5 . . ? C5 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C5 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N2 C10 H10A 109.5 . . ? N2 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? N2 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N2 C11 H11A 109.5 . . ? N2 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? N2 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N2 C12 C13 110.99(16) . . ? N2 C12 H12A 109.4 . . ? C13 C12 H12A 109.4 . . ? N2 C12 H12B 109.4 . . ? C13 C12 H12B 109.4 . . ? H12A C12 H12B 108.0 . . ? N3 C13 C12 111.08(14) . . ? N3 C13 H13A 109.4 . . ? C12 C13 H13A 109.4 . . ? N3 C13 H13B 109.4 . . ? C12 C13 H13B 109.4 . . ? H13A C13 H13B 108.0 . . ? N3 C14 H14A 109.5 . . ? N3 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? N3 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N3 C15 H15A 109.5 . . ? N3 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? N3 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N4 C16 C17 107.94(17) . . ? N4 C16 H16 126.0 . . ? C17 C16 H16 126.0 . . ? C16 C17 C18 107.08(17) . . ? C16 C17 H17 126.5 . . ? C18 C17 H17 126.5 . . ? C19 C18 C17 108.07(18) . . ? C19 C18 H18 126.0 . . ? C17 C18 H18 126.0 . . ? N4 C19 C18 107.35(18) . . ? N4 C19 H19 126.3 . . ? C18 C19 H19 126.3 . . ? N5 C21 C22 110.48(17) . . ? N5 C21 H21 124.8 . . ? C22 C21 H21 124.8 . . ? C21 C22 C23 106.78(17) . . ? C21 C22 H22 126.6 . . ? C23 C22 H22 126.6 . . ? C24 C23 C22 106.35(18) . . ? C24 C23 H23 126.8 . . ? C22 C23 H23 126.8 . . ? C23 C24 N5 111.05(19) . . ? C23 C24 H24 124.5 . . ? N5 C24 H24 124.5 . . ? C27 C25 C28 108.4(2) . . ? C27 C25 C26 108.6(2) . . ? C28 C25 C26 107.7(2) . . ? C27 C25 Zn2 114.22(19) . . ? C28 C25 Zn2 109.9(2) . . ? C26 C25 Zn2 107.9(2) . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C25 C28 H28A 109.5 . . ? C25 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C25 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? N6 C30 H30A 109.5 . . ? N6 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? N6 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? N6 C31 H31A 109.5 . . ? N6 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? N6 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? N6 C32 C33 110.87(14) . . ? N6 C32 H32A 109.5 . . ? C33 C32 H32A 109.5 . . ? N6 C32 H32B 109.5 . . ? C33 C32 H32B 109.5 . . ? H32A C32 H32B 108.1 . . ? N7 C33 C32 111.03(16) . . ? N7 C33 H33A 109.4 . . ? C32 C33 H33A 109.4 . . ? N7 C33 H33B 109.4 . . ? C32 C33 H33B 109.4 . . ? H33A C33 H33B 108.0 . . ? N7 C34 H34A 109.5 . . ? N7 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? N7 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? N7 C35 H35A 109.5 . . ? N7 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? N7 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C37 C36 N8 108.27(18) . . ? C37 C36 H36 125.9 . . ? N8 C36 H36 125.9 . . ? C36 C37 C38 107.45(19) . . ? C36 C37 H37 126.3 . . ? C38 C37 H37 126.3 . . ? C39 C38 C37 106.90(18) . . ? C39 C38 H38 126.5 . . ? C37 C38 H38 126.5 . . ? C38 C39 N8 108.56(17) . . ? C38 C39 H39 125.7 . . ? N8 C39 H39 125.7 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C5 Zn1 N1 C4 171.22(17) . . . . ? N2 Zn1 N1 C4 38.36(17) . . . . ? N3 Zn1 N1 C4 -49.56(17) . . . . ? C5 Zn1 N1 C1 -9.07(17) . . . . ? N2 Zn1 N1 C1 -141.93(13) . . . . ? N3 Zn1 N1 C1 130.15(13) . . . . ? C5 Zn1 N2 C11 -104.39(16) . . . . ? N1 Zn1 N2 C11 28.54(15) . . . . ? N3 Zn1 N2 C11 134.93(15) . . . . ? C5 Zn1 N2 C12 134.19(14) . . . . ? N1 Zn1 N2 C12 -92.87(12) . . . . ? N3 Zn1 N2 C12 13.52(12) . . . . ? C5 Zn1 N2 C10 16.30(15) . . . . ? N1 Zn1 N2 C10 149.23(12) . . . . ? N3 Zn1 N2 C10 -104.37(12) . . . . ? C5 Zn1 N3 C14 14.37(17) . . . . ? N1 Zn1 N3 C14 -124.19(15) . . . . ? N2 Zn1 N3 C14 133.62(15) . . . . ? C5 Zn1 N3 C13 -103.92(12) . . . . ? N1 Zn1 N3 C13 117.52(11) . . . . ? N2 Zn1 N3 C13 15.33(11) . . . . ? C5 Zn1 N3 C15 136.60(14) . . . . ? N1 Zn1 N3 C15 -1.95(15) . . . . ? N2 Zn1 N3 C15 -104.15(14) . . . . ? C25 Zn2 N5 C24 -9.01(17) . . . . ? N7 Zn2 N5 C24 -142.26(13) . . . . ? N6 Zn2 N5 C24 129.41(13) . . . . ? C25 Zn2 N5 C21 172.89(17) . . . . ? N7 Zn2 N5 C21 39.63(18) . . . . ? N6 Zn2 N5 C21 -48.69(17) . . . . ? N5 Zn2 N6 C31 -2.01(16) . . . . ? C25 Zn2 N6 C31 136.66(15) . . . . ? N7 Zn2 N6 C31 -104.92(15) . . . . ? N5 Zn2 N6 C32 117.77(11) . . . . ? C25 Zn2 N6 C32 -103.55(14) . . . . ? N7 Zn2 N6 C32 14.87(12) . . . . ? N5 Zn2 N6 C30 -124.88(14) . . . . ? C25 Zn2 N6 C30 13.80(17) . . . . ? N7 Zn2 N6 C30 132.22(15) . . . . ? N5 Zn2 N7 C35 148.74(12) . . . . ? C25 Zn2 N7 C35 14.72(15) . . . . ? N6 Zn2 N7 C35 -104.52(13) . . . . ? N5 Zn2 N7 C34 26.75(16) . . . . ? C25 Zn2 N7 C34 -107.27(17) . . . . ? N6 Zn2 N7 C34 133.49(15) . . . . ? N5 Zn2 N7 C33 -92.65(12) . . . . ? C25 Zn2 N7 C33 133.32(13) . . . . ? N6 Zn2 N7 C33 14.09(12) . . . . ? C4 N1 C1 C2 0.7(2) . . . . ? Zn1 N1 C1 C2 -179.10(12) . . . . ? N1 C1 C2 C3 -0.8(2) . . . . ? C1 C2 C3 C4 0.6(2) . . . . ? C1 N1 C4 C3 -0.3(2) . . . . ? Zn1 N1 C4 C3 179.48(13) . . . . ? C2 C3 C4 N1 -0.2(2) . . . . ? N1 Zn1 C5 C7 -57.27(14) . . . . ? N2 Zn1 C5 C7 68.69(15) . . . . ? N3 Zn1 C5 C7 168.63(11) . . . . ? N1 Zn1 C5 C8 61.26(19) . . . . ? N2 Zn1 C5 C8 -172.78(13) . . . . ? N3 Zn1 C5 C8 -72.84(18) . . . . ? N1 Zn1 C5 C6 -177.91(16) . . . . ? N2 Zn1 C5 C6 -51.9(2) . . . . ? N3 Zn1 C5 C6 48.0(2) . . . . ? C11 N2 C12 C13 -165.22(16) . . . . ? C10 N2 C12 C13 76.42(19) . . . . ? Zn1 N2 C12 C13 -40.88(17) . . . . ? C14 N3 C13 C12 -162.7(2) . . . . ? C15 N3 C13 C12 80.2(2) . . . . ? Zn1 N3 C13 C12 -42.46(17) . . . . ? N2 C12 C13 N3 60.0(2) . . . . ? C19 N4 C16 C17 -0.2(2) . . . . ? N4 C16 C17 C18 0.4(2) . . . . ? C16 C17 C18 C19 -0.5(3) . . . . ? C16 N4 C19 C18 -0.1(2) . . . . ? C17 C18 C19 N4 0.3(3) . . . . ? C24 N5 C21 C22 0.2(2) . . . . ? Zn2 N5 C21 C22 178.54(13) . . . . ? N5 C21 C22 C23 0.0(2) . . . . ? C21 C22 C23 C24 -0.3(2) . . . . ? C22 C23 C24 N5 0.4(2) . . . . ? C21 N5 C24 C23 -0.4(2) . . . . ? Zn2 N5 C24 C23 -178.96(12) . . . . ? N5 Zn2 C25 C27 -175.99(18) . . . . ? N7 Zn2 C25 C27 -48.9(2) . . . . ? N6 Zn2 C25 C27 50.0(2) . . . . ? N5 Zn2 C25 C28 61.97(19) . . . . ? N7 Zn2 C25 C28 -170.94(14) . . . . ? N6 Zn2 C25 C28 -71.99(19) . . . . ? N5 Zn2 C25 C26 -55.16(17) . . . . ? N7 Zn2 C25 C26 71.92(17) . . . . ? N6 Zn2 C25 C26 170.87(13) . . . . ? C31 N6 C32 C33 80.6(2) . . . . ? C30 N6 C32 C33 -161.2(2) . . . . ? Zn2 N6 C32 C33 -42.17(17) . . . . ? C35 N7 C33 C32 78.0(2) . . . . ? C34 N7 C33 C32 -163.69(17) . . . . ? Zn2 N7 C33 C32 -41.57(16) . . . . ? N6 C32 C33 N7 60.3(2) . . . . ? C39 N8 C36 C37 0.7(2) . . . . ? N8 C36 C37 C38 -0.8(3) . . . . ? C36 C37 C38 C39 0.6(3) . . . . ? C37 C38 C39 N8 -0.2(2) . . . . ? C36 N8 C39 C38 -0.3(2) . . . . ? _diffrn_measured_fraction_theta_max 0.962 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.288 _refine_diff_density_min -0.312 _refine_diff_density_rms 0.042 #===END #----------------------------------------------- #---------------COMPOUND 2---------------------- #----------------------------------------------- data_jag114sr _database_code_depnum_ccdc_archive 'CCDC 837242' #TrackingRef '- combined.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C14 H24 N4 Zn' _chemical_formula_sum 'C14 H24 N4 Zn' _chemical_formula_weight 313.74 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pna21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z+1/2' _cell_length_a 15.4350(3) _cell_length_b 10.3607(2) _cell_length_c 9.7566(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1560.25(5) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 18684 _cell_measurement_theta_min 3.1508 _cell_measurement_theta_max 29.4172 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.336 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 664 _exptl_absorpt_coefficient_mu 1.568 _exptl_absorpt_correction_T_min 0.57036 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Eos' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29629 _diffrn_reflns_av_R_equivalents 0.0300 _diffrn_reflns_av_sigmaI/netI 0.0186 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.16 _diffrn_reflns_theta_max 29.48 _reflns_number_total 4140 _reflns_number_gt 3913 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _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^)+(0.0336P)^2^+0.3547P] 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 0.248(9) _refine_ls_number_reflns 4140 _refine_ls_number_parameters 177 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0264 _refine_ls_R_factor_gt 0.0239 _refine_ls_wR_factor_ref 0.0582 _refine_ls_wR_factor_gt 0.0569 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.029 _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 0.186027(10) 0.314446(14) 0.26180(3) 0.01567(5) Uani 1 1 d . . . N1 N 0.17045(10) 0.32699(13) 0.06431(15) 0.0169(3) Uani 1 1 d . . . C1 C 0.22104(11) 0.38860(15) -0.03193(17) 0.0196(3) Uani 1 1 d . . . H1A H 0.2742 0.4312 -0.0132 0.024 Uiso 1 1 calc R . . C2 C 0.18314(11) 0.37935(19) -0.15929(18) 0.0233(4) Uani 1 1 d . . . H2A H 0.2051 0.4136 -0.2427 0.028 Uiso 1 1 calc R . . C3 C 0.10518(13) 0.30900(17) -0.14217(19) 0.0241(4) Uani 1 1 d . . . H3A H 0.0645 0.2868 -0.2114 0.029 Uiso 1 1 calc R . . C4 C 0.10021(11) 0.27919(16) -0.00466(17) 0.0193(3) Uani 1 1 d . . . H4A H 0.0543 0.2320 0.0366 0.023 Uiso 1 1 calc R . . N2 N 0.12605(10) 0.17217(14) 0.35016(15) 0.0202(3) Uani 1 1 d . . . C5 C 0.10476(10) 0.05950(15) 0.28487(17) 0.0196(4) Uani 1 1 d . . . H5A H 0.1184 0.0400 0.1922 0.024 Uiso 1 1 calc R . . C6 C 0.06080(11) -0.02149(18) 0.3727(2) 0.0254(4) Uani 1 1 d . . . H6A H 0.0386 -0.1048 0.3520 0.030 Uiso 1 1 calc R . . C7 C 0.05514(11) 0.04355(18) 0.4996(2) 0.0268(4) Uani 1 1 d . . . H7A H 0.0283 0.0129 0.5809 0.032 Uiso 1 1 calc R . . C8 C 0.09636(13) 0.16074(18) 0.48171(18) 0.0249(4) Uani 1 1 d . . . H8A H 0.1031 0.2244 0.5510 0.030 Uiso 1 1 calc R . . N3 N 0.16637(10) 0.49969(14) 0.35083(15) 0.0188(3) Uani 1 1 d . . . N4 N 0.31448(9) 0.33123(14) 0.32976(17) 0.0175(3) Uani 1 1 d . . . C10 C 0.38046(12) 0.28180(17) 0.23279(18) 0.0251(4) Uani 1 1 d . . . H10A H 0.4385 0.2997 0.2689 0.038 Uiso 1 1 calc R . . H10B H 0.3734 0.3245 0.1439 0.038 Uiso 1 1 calc R . . H10C H 0.3731 0.1884 0.2215 0.038 Uiso 1 1 calc R . . C11 C 0.32642(12) 0.26257(19) 0.46143(19) 0.0254(4) Uani 1 1 d . . . H11A H 0.3844 0.2808 0.4975 0.038 Uiso 1 1 calc R . . H11B H 0.3201 0.1695 0.4467 0.038 Uiso 1 1 calc R . . H11C H 0.2827 0.2920 0.5272 0.038 Uiso 1 1 calc R . . C12 C 0.24828(12) 0.53075(16) 0.42368(18) 0.0221(3) Uani 1 1 d . . . H12A H 0.2458 0.4961 0.5181 0.027 Uiso 1 1 calc R . . H12B H 0.2552 0.6256 0.4296 0.027 Uiso 1 1 calc R . . C13 C 0.32596(11) 0.47257(17) 0.3483(2) 0.0213(3) Uani 1 1 d . . . H13A H 0.3322 0.5144 0.2575 0.026 Uiso 1 1 calc R . . H13B H 0.3795 0.4891 0.4013 0.026 Uiso 1 1 calc R . . C14 C 0.15300(15) 0.59379(17) 0.2387(2) 0.0303(4) Uani 1 1 d . . . H14A H 0.1461 0.6804 0.2774 0.045 Uiso 1 1 calc R . . H14B H 0.1008 0.5707 0.1871 0.045 Uiso 1 1 calc R . . H14C H 0.2032 0.5926 0.1772 0.045 Uiso 1 1 calc R . . C15 C 0.09212(12) 0.5094(2) 0.4462(2) 0.0296(4) Uani 1 1 d . . . H15A H 0.0873 0.5982 0.4798 0.044 Uiso 1 1 calc R . . H15B H 0.1012 0.4509 0.5238 0.044 Uiso 1 1 calc R . . H15C H 0.0387 0.4854 0.3981 0.044 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.01936(8) 0.01551(8) 0.01214(8) 0.00003(9) 0.00013(10) -0.00376(6) N1 0.0213(6) 0.0173(7) 0.0121(7) -0.0002(5) -0.0001(5) -0.0021(5) C1 0.0227(8) 0.0180(7) 0.0183(8) 0.0005(6) 0.0017(6) -0.0028(6) C2 0.0303(10) 0.0253(9) 0.0144(8) 0.0029(7) 0.0026(6) 0.0014(7) C3 0.0248(9) 0.0311(10) 0.0163(8) -0.0012(7) -0.0042(7) 0.0016(7) C4 0.0180(7) 0.0224(8) 0.0175(8) -0.0019(6) -0.0003(6) 0.0003(6) N2 0.0238(7) 0.0204(7) 0.0164(7) 0.0021(5) 0.0015(6) -0.0048(5) C5 0.0182(7) 0.0183(7) 0.0223(11) 0.0008(6) -0.0026(6) -0.0017(5) C6 0.0182(8) 0.0213(8) 0.0367(10) 0.0079(7) -0.0024(7) -0.0035(6) C7 0.0189(8) 0.0328(9) 0.0287(9) 0.0153(8) 0.0024(7) -0.0006(7) C8 0.0281(9) 0.0290(9) 0.0177(8) 0.0029(7) 0.0036(7) -0.0011(7) N3 0.0220(6) 0.0189(7) 0.0155(6) -0.0007(5) -0.0005(5) 0.0013(5) N4 0.0195(7) 0.0163(7) 0.0167(7) 0.0018(5) 0.0009(5) -0.0014(5) C10 0.0248(8) 0.0235(8) 0.0271(11) 0.0011(7) 0.0052(7) 0.0029(6) C11 0.0285(9) 0.0268(9) 0.0208(9) 0.0073(7) -0.0030(7) -0.0004(7) C12 0.0254(8) 0.0181(7) 0.0228(8) -0.0040(6) -0.0033(7) -0.0015(6) C13 0.0200(8) 0.0167(8) 0.0273(9) 0.0000(7) -0.0011(6) -0.0053(6) C14 0.0452(10) 0.0208(8) 0.0249(12) 0.0033(7) -0.0065(8) 0.0076(7) C15 0.0239(9) 0.0338(10) 0.0310(10) -0.0087(8) 0.0038(8) 0.0045(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 N2 1.9425(14) . ? Zn1 N1 1.9461(15) . ? Zn1 N4 2.0978(14) . ? Zn1 N3 2.1284(15) . ? N1 C4 1.369(2) . ? N1 C1 1.378(2) . ? C1 C2 1.377(2) . ? C1 H1A 0.9500 . ? C2 C3 1.417(3) . ? C2 H2A 0.9500 . ? C3 C4 1.379(2) . ? C3 H3A 0.9500 . ? C4 H4A 0.9500 . ? N2 C8 1.368(2) . ? N2 C5 1.370(2) . ? C5 C6 1.378(2) . ? C5 H5A 0.9500 . ? C6 C7 1.412(3) . ? C6 H6A 0.9500 . ? C7 C8 1.382(2) . ? C7 H7A 0.9500 . ? C8 H8A 0.9500 . ? N3 C15 1.480(2) . ? N3 C14 1.480(2) . ? N3 C12 1.486(2) . ? N4 C11 1.480(2) . ? N4 C10 1.481(2) . ? N4 C13 1.486(2) . ? 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 C13 1.530(2) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Zn1 N1 115.55(6) . . ? N2 Zn1 N4 111.90(6) . . ? N1 Zn1 N4 115.10(6) . . ? N2 Zn1 N3 115.80(6) . . ? N1 Zn1 N3 109.04(6) . . ? N4 Zn1 N3 86.04(6) . . ? C4 N1 C1 106.35(14) . . ? C4 N1 Zn1 124.08(12) . . ? C1 N1 Zn1 129.46(12) . . ? C2 C1 N1 110.00(15) . . ? C2 C1 H1A 125.0 . . ? N1 C1 H1A 125.0 . . ? C1 C2 C3 106.87(15) . . ? C1 C2 H2A 126.6 . . ? C3 C2 H2A 126.6 . . ? C4 C3 C2 106.10(16) . . ? C4 C3 H3A 127.0 . . ? C2 C3 H3A 127.0 . . ? N1 C4 C3 110.68(16) . . ? N1 C4 H4A 124.7 . . ? C3 C4 H4A 124.7 . . ? C8 N2 C5 106.39(14) . . ? C8 N2 Zn1 129.93(13) . . ? C5 N2 Zn1 123.68(12) . . ? N2 C5 C6 110.35(15) . . ? N2 C5 H5A 124.8 . . ? C6 C5 H5A 124.8 . . ? C5 C6 C7 106.56(16) . . ? C5 C6 H6A 126.7 . . ? C7 C6 H6A 126.7 . . ? C8 C7 C6 106.29(16) . . ? C8 C7 H7A 126.9 . . ? C6 C7 H7A 126.9 . . ? N2 C8 C7 110.40(17) . . ? N2 C8 H8A 124.8 . . ? C7 C8 H8A 124.8 . . ? C15 N3 C14 108.19(15) . . ? C15 N3 C12 110.10(14) . . ? C14 N3 C12 109.25(15) . . ? C15 N3 Zn1 115.36(12) . . ? C14 N3 Zn1 108.19(10) . . ? C12 N3 Zn1 105.62(10) . . ? C11 N4 C10 107.61(13) . . ? C11 N4 C13 110.69(15) . . ? C10 N4 C13 109.65(13) . . ? C11 N4 Zn1 110.62(11) . . ? C10 N4 Zn1 114.78(11) . . ? C13 N4 Zn1 103.46(10) . . ? N4 C10 H10A 109.5 . . ? N4 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? N4 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N4 C11 H11A 109.5 . . ? N4 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? N4 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N3 C12 C13 110.57(14) . . ? N3 C12 H12A 109.5 . . ? C13 C12 H12A 109.5 . . ? N3 C12 H12B 109.5 . . ? C13 C12 H12B 109.5 . . ? H12A C12 H12B 108.1 . . ? N4 C13 C12 110.68(14) . . ? N4 C13 H13A 109.5 . . ? C12 C13 H13A 109.5 . . ? N4 C13 H13B 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 108.1 . . ? N3 C14 H14A 109.5 . . ? N3 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? N3 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N3 C15 H15A 109.5 . . ? N3 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? N3 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Zn1 N1 C4 25.30(15) . . . . ? N4 Zn1 N1 C4 158.18(13) . . . . ? N3 Zn1 N1 C4 -107.17(13) . . . . ? N2 Zn1 N1 C1 -158.92(14) . . . . ? N4 Zn1 N1 C1 -26.04(16) . . . . ? N3 Zn1 N1 C1 68.60(16) . . . . ? C4 N1 C1 C2 -0.10(19) . . . . ? Zn1 N1 C1 C2 -176.46(12) . . . . ? N1 C1 C2 C3 0.1(2) . . . . ? C1 C2 C3 C4 -0.1(2) . . . . ? C1 N1 C4 C3 0.05(19) . . . . ? Zn1 N1 C4 C3 176.65(12) . . . . ? C2 C3 C4 N1 0.0(2) . . . . ? N1 Zn1 N2 C8 -153.01(16) . . . . ? N4 Zn1 N2 C8 72.65(18) . . . . ? N3 Zn1 N2 C8 -23.76(19) . . . . ? N1 Zn1 N2 C5 26.43(16) . . . . ? N4 Zn1 N2 C5 -107.91(14) . . . . ? N3 Zn1 N2 C5 155.68(13) . . . . ? C8 N2 C5 C6 1.09(19) . . . . ? Zn1 N2 C5 C6 -178.47(12) . . . . ? N2 C5 C6 C7 -0.57(19) . . . . ? C5 C6 C7 C8 -0.2(2) . . . . ? C5 N2 C8 C7 -1.2(2) . . . . ? Zn1 N2 C8 C7 178.32(13) . . . . ? C6 C7 C8 N2 0.8(2) . . . . ? N2 Zn1 N3 C15 -15.73(15) . . . . ? N1 Zn1 N3 C15 116.61(13) . . . . ? N4 Zn1 N3 C15 -128.18(13) . . . . ? N2 Zn1 N3 C14 -137.02(12) . . . . ? N1 Zn1 N3 C14 -4.67(14) . . . . ? N4 Zn1 N3 C14 110.53(13) . . . . ? N2 Zn1 N3 C12 106.10(11) . . . . ? N1 Zn1 N3 C12 -121.56(11) . . . . ? N4 Zn1 N3 C12 -6.35(11) . . . . ? N2 Zn1 N4 C11 -18.79(14) . . . . ? N1 Zn1 N4 C11 -153.35(11) . . . . ? N3 Zn1 N4 C11 97.46(12) . . . . ? N2 Zn1 N4 C10 103.20(12) . . . . ? N1 Zn1 N4 C10 -31.35(13) . . . . ? N3 Zn1 N4 C10 -140.55(12) . . . . ? N2 Zn1 N4 C13 -137.37(11) . . . . ? N1 Zn1 N4 C13 88.08(12) . . . . ? N3 Zn1 N4 C13 -21.11(11) . . . . ? C15 N3 C12 C13 157.99(15) . . . . ? C14 N3 C12 C13 -83.34(17) . . . . ? Zn1 N3 C12 C13 32.83(16) . . . . ? C11 N4 C13 C12 -73.04(18) . . . . ? C10 N4 C13 C12 168.38(14) . . . . ? Zn1 N4 C13 C12 45.48(16) . . . . ? N3 C12 C13 N4 -55.42(19) . . . . ? _diffrn_measured_fraction_theta_max 0.970 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.730 _refine_diff_density_min -0.299 _refine_diff_density_rms 0.045 #===END #----------------------------------------------- #---------------COMPOUND 3---------------------- #----------------------------------------------- data_srjg1102 _database_code_depnum_ccdc_archive 'CCDC 837243' #TrackingRef '- combined.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H36 N3 Na O3 Zn' _chemical_formula_sum 'C24 H36 N3 Na O3 Zn' _chemical_formula_weight 502.92 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.3429(2) _cell_length_b 11.0909(3) _cell_length_c 14.1002(3) _cell_angle_alpha 94.178(2) _cell_angle_beta 104.038(2) _cell_angle_gamma 95.994(2) _cell_volume 1252.28(5) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 6835 _cell_measurement_theta_min 3.2484 _cell_measurement_theta_max 30.1203 _exptl_crystal_description brick _exptl_crystal_colour colourless _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.334 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 532 _exptl_absorpt_coefficient_mu 1.027 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.75096 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Eos' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14316 _diffrn_reflns_av_R_equivalents 0.0303 _diffrn_reflns_av_sigmaI/netI 0.0467 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.25 _diffrn_reflns_theta_max 30.19 _reflns_number_total 6611 _reflns_number_gt 5404 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _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^)+(0.0336P)^2^+0.2404P] 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 6611 _refine_ls_number_parameters 289 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0507 _refine_ls_R_factor_gt 0.0364 _refine_ls_wR_factor_ref 0.0822 _refine_ls_wR_factor_gt 0.0763 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.037 _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 -0.15580(2) 0.639457(19) 0.232632(13) 0.02016(7) Uani 1 1 d . . . Na1 Na 0.45930(8) 0.73424(7) 0.38693(5) 0.02393(16) Uani 1 1 d . . . O1 O -0.11792(14) 0.45940(11) 0.18553(8) 0.0223(3) Uani 1 1 d . . . C1 C -0.2440(2) 0.35620(18) 0.17970(14) 0.0291(4) Uani 1 1 d . . . H1A H -0.3564 0.3825 0.1658 0.035 Uiso 1 1 calc R . . H1B H -0.2240 0.3184 0.2423 0.035 Uiso 1 1 calc R . . C2 C -0.2290(3) 0.26676(19) 0.09646(14) 0.0325(4) Uani 1 1 d . . . H2A H -0.1505 0.2082 0.1208 0.039 Uiso 1 1 calc R . . H2B H -0.3386 0.2212 0.0620 0.039 Uiso 1 1 calc R . . C3 C -0.1627(2) 0.34940(18) 0.03019(13) 0.0282(4) Uani 1 1 d . . . H3A H -0.1059 0.3045 -0.0125 0.034 Uiso 1 1 calc R . . H3B H -0.2527 0.3881 -0.0112 0.034 Uiso 1 1 calc R . . C4 C -0.0419(2) 0.44180(19) 0.10361(13) 0.0293(4) Uani 1 1 d . . . H4A H 0.0670 0.4112 0.1255 0.035 Uiso 1 1 calc R . . H4B H -0.0249 0.5193 0.0746 0.035 Uiso 1 1 calc R . . N2 N -0.35420(17) 0.59139(14) 0.27977(10) 0.0215(3) Uani 1 1 d . . . C5 C -0.3559(2) 0.53630(17) 0.36347(12) 0.0225(4) Uani 1 1 d . . . H5A H -0.2600 0.5306 0.4147 0.027 Uiso 1 1 calc R . . C6 C -0.5161(2) 0.49031(18) 0.36303(14) 0.0289(4) Uani 1 1 d . . . H6A H -0.5502 0.4485 0.4127 0.035 Uiso 1 1 calc R . . C7 C -0.6192(2) 0.5176(2) 0.27422(14) 0.0325(5) Uani 1 1 d . . . H7A H -0.7367 0.4980 0.2523 0.039 Uiso 1 1 calc R . . C8 C -0.5168(2) 0.57795(19) 0.22559(13) 0.0279(4) Uani 1 1 d . . . H8A H -0.5534 0.6065 0.1630 0.033 Uiso 1 1 calc R . . N3 N -0.18862(18) 0.71847(14) 0.11143(10) 0.0230(3) Uani 1 1 d . . . C9 C -0.3004(2) 0.67483(18) 0.02406(12) 0.0257(4) Uani 1 1 d . . . H9A H -0.3754 0.6018 0.0141 0.031 Uiso 1 1 calc R . . C10 C -0.2890(2) 0.75151(19) -0.04703(13) 0.0281(4) Uani 1 1 d . . . H10A H -0.3527 0.7414 -0.1134 0.034 Uiso 1 1 calc R . . C11 C -0.1647(2) 0.8475(2) -0.00219(13) 0.0295(4) Uani 1 1 d . . . H11A H -0.1277 0.9154 -0.0322 0.035 Uiso 1 1 calc R . . C12 C -0.1068(2) 0.82423(18) 0.09398(13) 0.0258(4) Uani 1 1 d . . . H12A H -0.0216 0.8749 0.1416 0.031 Uiso 1 1 calc R . . N4 N 0.03988(17) 0.69894(14) 0.34067(10) 0.0202(3) Uani 1 1 d . . . C13 C 0.1042(2) 0.63655(17) 0.41878(12) 0.0226(4) Uani 1 1 d . . . H13A H 0.0753 0.5521 0.4222 0.027 Uiso 1 1 calc R . . C14 C 0.2167(2) 0.71338(18) 0.49162(12) 0.0237(4) Uani 1 1 d . . . H14A H 0.2780 0.6922 0.5528 0.028 Uiso 1 1 calc R . . C15 C 0.2227(2) 0.83003(18) 0.45718(12) 0.0237(4) Uani 1 1 d . . . H15A H 0.2885 0.9028 0.4906 0.028 Uiso 1 1 calc R . . C16 C 0.1135(2) 0.81664(17) 0.36523(13) 0.0229(4) Uani 1 1 d . . . H16A H 0.0924 0.8807 0.3245 0.027 Uiso 1 1 calc R . . O9 O 0.66832(15) 0.81406(14) 0.52567(9) 0.0311(3) Uani 1 1 d . . . C33 C 0.6528(2) 0.84665(19) 0.62363(12) 0.0280(4) Uani 1 1 d . . . H33A H 0.5570 0.7957 0.6364 0.034 Uiso 1 1 calc R . . H33B H 0.6351 0.9333 0.6317 0.034 Uiso 1 1 calc R . . C34 C 0.8142(2) 0.8250(2) 0.69424(14) 0.0341(5) Uani 1 1 d . . . H34A H 0.7926 0.7654 0.7400 0.041 Uiso 1 1 calc R . . H34B H 0.8727 0.9020 0.7329 0.041 Uiso 1 1 calc R . . C35 C 0.9161(3) 0.7751(2) 0.62755(15) 0.0412(5) Uani 1 1 d . . . H35A H 1.0356 0.8072 0.6522 0.049 Uiso 1 1 calc R . . H35B H 0.9041 0.6849 0.6223 0.049 Uiso 1 1 calc R . . C36 C 0.8432(2) 0.8195(2) 0.53158(14) 0.0324(5) Uani 1 1 d . . . H36A H 0.8923 0.9041 0.5291 0.039 Uiso 1 1 calc R . . H36B H 0.8629 0.7668 0.4768 0.039 Uiso 1 1 calc R . . O10 O 0.49906(15) 0.88527(13) 0.28879(9) 0.0278(3) Uani 1 1 d . . . C37 C 0.6655(2) 0.9397(2) 0.29401(13) 0.0308(4) Uani 1 1 d . . . H37A H 0.7377 0.8761 0.2867 0.037 Uiso 1 1 calc R . . H37B H 0.7138 0.9893 0.3578 0.037 Uiso 1 1 calc R . . C38 C 0.6503(3) 1.0187(2) 0.21079(15) 0.0384(5) Uani 1 1 d . . . H38A H 0.7542 1.0285 0.1884 0.046 Uiso 1 1 calc R . . H38B H 0.6220 1.1000 0.2296 0.046 Uiso 1 1 calc R . . C39 C 0.5084(3) 0.9456(2) 0.13271(14) 0.0387(5) Uani 1 1 d . . . H39A H 0.4529 0.9982 0.0843 0.046 Uiso 1 1 calc R . . H39B H 0.5479 0.8786 0.0978 0.046 Uiso 1 1 calc R . . C40 C 0.3936(2) 0.8970(2) 0.19308(13) 0.0323(4) Uani 1 1 d . . . H40A H 0.3119 0.9541 0.1985 0.039 Uiso 1 1 calc R . . H40B H 0.3323 0.8169 0.1623 0.039 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.02331(11) 0.01981(12) 0.01742(10) 0.00200(7) 0.00519(7) 0.00283(8) Na1 0.0265(4) 0.0256(4) 0.0204(3) 0.0016(3) 0.0073(3) 0.0041(3) O1 0.0255(6) 0.0204(7) 0.0210(6) -0.0009(5) 0.0075(5) 0.0013(5) C1 0.0351(10) 0.0206(10) 0.0324(10) 0.0030(8) 0.0124(8) -0.0021(8) C2 0.0378(11) 0.0222(11) 0.0365(10) -0.0027(8) 0.0113(9) -0.0016(8) C3 0.0335(10) 0.0264(11) 0.0231(9) -0.0027(7) 0.0060(7) 0.0029(8) C4 0.0287(9) 0.0286(11) 0.0316(9) -0.0057(8) 0.0139(8) -0.0007(8) N2 0.0214(7) 0.0250(9) 0.0182(7) 0.0016(6) 0.0041(5) 0.0057(6) C5 0.0249(9) 0.0225(10) 0.0204(8) 0.0029(7) 0.0049(7) 0.0054(7) C6 0.0314(10) 0.0250(11) 0.0319(9) 0.0004(8) 0.0135(8) -0.0003(8) C7 0.0206(9) 0.0393(13) 0.0331(10) -0.0118(9) 0.0039(7) 0.0009(8) C8 0.0251(9) 0.0363(12) 0.0195(8) -0.0043(8) -0.0002(7) 0.0099(8) N3 0.0264(7) 0.0230(9) 0.0202(7) 0.0035(6) 0.0061(6) 0.0037(6) C9 0.0277(9) 0.0250(10) 0.0221(8) 0.0014(7) 0.0030(7) 0.0018(8) C10 0.0270(9) 0.0386(12) 0.0201(8) 0.0065(8) 0.0056(7) 0.0089(8) C11 0.0291(10) 0.0337(12) 0.0292(9) 0.0124(8) 0.0105(8) 0.0055(8) C12 0.0264(9) 0.0242(10) 0.0267(9) 0.0032(7) 0.0068(7) 0.0017(8) N4 0.0214(7) 0.0185(8) 0.0213(7) 0.0023(6) 0.0064(6) 0.0031(6) C13 0.0209(8) 0.0223(10) 0.0270(9) 0.0050(7) 0.0089(7) 0.0051(7) C14 0.0190(8) 0.0312(11) 0.0218(8) 0.0044(7) 0.0053(7) 0.0057(7) C15 0.0222(8) 0.0243(10) 0.0238(8) -0.0019(7) 0.0062(7) 0.0016(7) C16 0.0240(8) 0.0204(10) 0.0253(8) 0.0038(7) 0.0078(7) 0.0031(7) O9 0.0217(6) 0.0480(9) 0.0223(6) -0.0076(6) 0.0059(5) 0.0047(6) C33 0.0290(9) 0.0323(11) 0.0237(9) -0.0043(8) 0.0105(7) 0.0032(8) C34 0.0370(11) 0.0407(13) 0.0248(9) 0.0035(9) 0.0071(8) 0.0073(9) C35 0.0346(11) 0.0521(16) 0.0399(11) 0.0053(10) 0.0092(9) 0.0186(11) C36 0.0256(9) 0.0430(13) 0.0299(10) -0.0019(9) 0.0108(8) 0.0045(9) O10 0.0296(7) 0.0313(8) 0.0240(6) 0.0074(5) 0.0084(5) 0.0040(6) C37 0.0327(10) 0.0315(12) 0.0268(9) -0.0002(8) 0.0081(8) -0.0011(9) C38 0.0510(13) 0.0260(12) 0.0462(12) 0.0083(9) 0.0265(10) 0.0044(10) C39 0.0507(13) 0.0482(15) 0.0243(9) 0.0097(9) 0.0140(9) 0.0235(11) C40 0.0321(10) 0.0371(12) 0.0268(9) 0.0038(8) 0.0030(8) 0.0102(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 N3 1.9506(14) . ? Zn1 N4 1.9604(14) . ? Zn1 N2 1.9664(14) . ? Zn1 O1 2.1376(12) . ? Na1 O10 2.2967(15) . ? Na1 O9 2.3285(14) . ? Na1 C15 2.6908(18) . ? Na1 C7 2.709(2) 1_655 ? Na1 C6 2.737(2) 1_655 ? Na1 C14 2.7806(18) . ? Na1 C8 2.8172(19) 1_655 ? Na1 C5 2.8554(19) 1_655 ? Na1 N2 2.9191(15) 1_655 ? Na1 C16 3.0681(19) . ? O1 C1 1.455(2) . ? O1 C4 1.457(2) . ? C1 C2 1.518(3) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C3 1.513(3) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.504(2) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? N2 C5 1.370(2) . ? N2 C8 1.373(2) . ? N2 Na1 2.9191(15) 1_455 ? C5 C6 1.378(3) . ? C5 Na1 2.8554(19) 1_455 ? C5 H5A 0.9500 . ? C6 C7 1.410(3) . ? C6 Na1 2.737(2) 1_455 ? C6 H6A 0.9500 . ? C7 C8 1.371(3) . ? C7 Na1 2.709(2) 1_455 ? C7 H7A 0.9500 . ? C8 Na1 2.8172(19) 1_455 ? C8 H8A 0.9500 . ? N3 C12 1.363(2) . ? N3 C9 1.372(2) . ? C9 C10 1.375(3) . ? C9 H9A 0.9500 . ? C10 C11 1.400(3) . ? C10 H10A 0.9500 . ? C11 C12 1.378(2) . ? C11 H11A 0.9500 . ? C12 H12A 0.9500 . ? N4 C16 1.366(2) . ? N4 C13 1.372(2) . ? C13 C14 1.378(2) . ? C13 H13A 0.9500 . ? C14 C15 1.415(3) . ? C14 H14A 0.9500 . ? C15 C16 1.380(2) . ? C15 H15A 0.9500 . ? C16 H16A 0.9500 . ? O9 C36 1.436(2) . ? O9 C33 1.442(2) . ? C33 C34 1.521(3) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 C35 1.524(3) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 C36 1.485(3) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? O10 C37 1.438(2) . ? O10 C40 1.444(2) . ? C37 C38 1.504(3) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 C39 1.519(3) . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C39 C40 1.512(3) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 H40A 0.9900 . ? C40 H40B 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 N3 Zn1 N4 118.76(6) . . ? N3 Zn1 N2 117.39(6) . . ? N4 Zn1 N2 112.27(6) . . ? N3 Zn1 O1 102.56(6) . . ? N4 Zn1 O1 105.15(5) . . ? N2 Zn1 O1 96.48(5) . . ? O10 Na1 O9 97.55(6) . . ? O10 Na1 C15 96.44(6) . . ? O9 Na1 C15 92.50(5) . . ? O10 Na1 C7 108.61(6) . 1_655 ? O9 Na1 C7 134.90(6) . 1_655 ? C15 Na1 C7 119.27(6) . 1_655 ? O10 Na1 C6 130.41(6) . 1_655 ? O9 Na1 C6 106.13(6) . 1_655 ? C15 Na1 C6 124.61(6) . 1_655 ? C7 Na1 C6 29.99(6) 1_655 1_655 ? O10 Na1 C14 125.86(6) . . ? O9 Na1 C14 93.05(5) . . ? C15 Na1 C14 29.92(6) . . ? C7 Na1 C14 99.95(6) 1_655 . ? C6 Na1 C14 96.09(6) 1_655 . ? O10 Na1 C8 83.89(6) . 1_655 ? O9 Na1 C8 128.45(5) . 1_655 ? C15 Na1 C8 138.80(6) . 1_655 ? C7 Na1 C8 28.64(6) 1_655 1_655 ? C6 Na1 C8 47.30(6) 1_655 1_655 ? C14 Na1 C8 127.43(6) . 1_655 ? O10 Na1 C5 112.77(5) . 1_655 ? O9 Na1 C5 89.16(5) . 1_655 ? C15 Na1 C5 150.26(6) . 1_655 ? C7 Na1 C5 47.18(5) 1_655 1_655 ? C6 Na1 C5 28.43(5) 1_655 1_655 ? C14 Na1 C5 120.34(6) . 1_655 ? C8 Na1 C5 45.38(5) 1_655 1_655 ? O10 Na1 N2 86.54(5) . 1_655 ? O9 Na1 N2 100.82(5) . 1_655 ? C15 Na1 N2 165.87(6) . 1_655 ? C7 Na1 N2 47.10(5) 1_655 1_655 ? C6 Na1 N2 46.95(5) 1_655 1_655 ? C14 Na1 N2 142.80(6) . 1_655 ? C8 Na1 N2 27.62(4) 1_655 1_655 ? C5 Na1 N2 27.43(4) 1_655 1_655 ? O10 Na1 C16 84.66(5) . . ? O9 Na1 C16 117.80(5) . . ? C15 Na1 C16 26.70(5) . . ? C7 Na1 C16 101.03(6) 1_655 . ? C6 Na1 C16 118.86(6) 1_655 . ? C14 Na1 C16 44.56(5) . . ? C8 Na1 C16 113.65(5) 1_655 . ? C5 Na1 C16 146.48(6) 1_655 . ? N2 Na1 C16 141.16(5) 1_655 . ? C1 O1 C4 108.53(13) . . ? C1 O1 Zn1 120.88(10) . . ? C4 O1 Zn1 118.99(11) . . ? O1 C1 C2 105.92(15) . . ? O1 C1 H1A 110.6 . . ? C2 C1 H1A 110.6 . . ? O1 C1 H1B 110.6 . . ? C2 C1 H1B 110.6 . . ? H1A C1 H1B 108.7 . . ? C3 C2 C1 102.54(16) . . ? C3 C2 H2A 111.3 . . ? C1 C2 H2A 111.3 . . ? C3 C2 H2B 111.3 . . ? C1 C2 H2B 111.3 . . ? H2A C2 H2B 109.2 . . ? C4 C3 C2 101.76(15) . . ? C4 C3 H3A 111.4 . . ? C2 C3 H3A 111.4 . . ? C4 C3 H3B 111.4 . . ? C2 C3 H3B 111.4 . . ? H3A C3 H3B 109.3 . . ? O1 C4 C3 105.36(14) . . ? O1 C4 H4A 110.7 . . ? C3 C4 H4A 110.7 . . ? O1 C4 H4B 110.7 . . ? C3 C4 H4B 110.7 . . ? H4A C4 H4B 108.8 . . ? C5 N2 C8 105.82(15) . . ? C5 N2 Zn1 125.88(11) . . ? C8 N2 Zn1 126.50(12) . . ? C5 N2 Na1 73.70(9) . 1_455 ? C8 N2 Na1 72.06(9) . 1_455 ? Zn1 N2 Na1 130.94(7) . 1_455 ? N2 C5 C6 110.58(16) . . ? N2 C5 Na1 78.87(10) . 1_455 ? C6 C5 Na1 71.01(11) . 1_455 ? N2 C5 H5A 124.7 . . ? C6 C5 H5A 124.7 . . ? Na1 C5 H5A 117.1 1_455 . ? C5 C6 C7 106.31(17) . . ? C5 C6 Na1 80.56(12) . 1_455 ? C7 C6 Na1 73.90(12) . 1_455 ? C5 C6 H6A 126.8 . . ? C7 C6 H6A 126.8 . . ? Na1 C6 H6A 111.6 1_455 . ? C8 C7 C6 106.61(16) . . ? C8 C7 Na1 80.07(12) . 1_455 ? C6 C7 Na1 76.11(11) . 1_455 ? C8 C7 H7A 126.7 . . ? C6 C7 H7A 126.7 . . ? Na1 C7 H7A 110.2 1_455 . ? C7 C8 N2 110.67(16) . . ? C7 C8 Na1 71.29(11) . 1_455 ? N2 C8 Na1 80.32(10) . 1_455 ? C7 C8 H8A 124.7 . . ? N2 C8 H8A 124.7 . . ? Na1 C8 H8A 115.5 1_455 . ? C12 N3 C9 105.75(15) . . ? C12 N3 Zn1 128.65(12) . . ? C9 N3 Zn1 125.59(13) . . ? N3 C9 C10 110.61(17) . . ? N3 C9 H9A 124.7 . . ? C10 C9 H9A 124.7 . . ? C9 C10 C11 106.41(16) . . ? C9 C10 H10A 126.8 . . ? C11 C10 H10A 126.8 . . ? C12 C11 C10 106.53(17) . . ? C12 C11 H11A 126.7 . . ? C10 C11 H11A 126.7 . . ? N3 C12 C11 110.70(17) . . ? N3 C12 H12A 124.7 . . ? C11 C12 H12A 124.7 . . ? C16 N4 C13 106.03(14) . . ? C16 N4 Zn1 126.74(12) . . ? C13 N4 Zn1 125.66(12) . . ? N4 C13 C14 110.57(17) . . ? N4 C13 H13A 124.7 . . ? C14 C13 H13A 124.7 . . ? C13 C14 C15 106.41(15) . . ? C13 C14 Na1 94.24(11) . . ? C15 C14 Na1 71.53(10) . . ? C13 C14 H14A 126.8 . . ? C15 C14 H14A 126.8 . . ? Na1 C14 H14A 101.7 . . ? C16 C15 C14 106.09(16) . . ? C16 C15 Na1 92.09(11) . . ? C14 C15 Na1 78.56(10) . . ? C16 C15 H15A 127.0 . . ? C14 C15 H15A 127.0 . . ? Na1 C15 H15A 97.7 . . ? N4 C16 C15 110.90(16) . . ? N4 C16 Na1 90.78(10) . . ? C15 C16 Na1 61.21(9) . . ? N4 C16 H16A 124.6 . . ? C15 C16 H16A 124.6 . . ? Na1 C16 H16A 114.4 . . ? C36 O9 C33 106.87(13) . . ? C36 O9 Na1 124.08(10) . . ? C33 O9 Na1 128.26(10) . . ? O9 C33 C34 106.90(14) . . ? O9 C33 H33A 110.3 . . ? C34 C33 H33A 110.3 . . ? O9 C33 H33B 110.3 . . ? C34 C33 H33B 110.3 . . ? H33A C33 H33B 108.6 . . ? C33 C34 C35 104.14(15) . . ? C33 C34 H34A 110.9 . . ? C35 C34 H34A 110.9 . . ? C33 C34 H34B 110.9 . . ? C35 C34 H34B 110.9 . . ? H34A C34 H34B 108.9 . . ? C36 C35 C34 103.37(17) . . ? C36 C35 H35A 111.1 . . ? C34 C35 H35A 111.1 . . ? C36 C35 H35B 111.1 . . ? C34 C35 H35B 111.1 . . ? H35A C35 H35B 109.1 . . ? O9 C36 C35 104.88(16) . . ? O9 C36 H36A 110.8 . . ? C35 C36 H36A 110.8 . . ? O9 C36 H36B 110.8 . . ? C35 C36 H36B 110.8 . . ? H36A C36 H36B 108.8 . . ? C37 O10 C40 109.03(14) . . ? C37 O10 Na1 119.34(11) . . ? C40 O10 Na1 125.68(12) . . ? O10 C37 C38 105.89(16) . . ? O10 C37 H37A 110.6 . . ? C38 C37 H37A 110.6 . . ? O10 C37 H37B 110.6 . . ? C38 C37 H37B 110.6 . . ? H37A C37 H37B 108.7 . . ? C37 C38 C39 101.62(17) . . ? C37 C38 H38A 111.4 . . ? C39 C38 H38A 111.4 . . ? C37 C38 H38B 111.4 . . ? C39 C38 H38B 111.4 . . ? H38A C38 H38B 109.3 . . ? C40 C39 C38 102.11(15) . . ? C40 C39 H39A 111.3 . . ? C38 C39 H39A 111.3 . . ? C40 C39 H39B 111.3 . . ? C38 C39 H39B 111.3 . . ? H39A C39 H39B 109.2 . . ? O10 C40 C39 106.10(15) . . ? O10 C40 H40A 110.5 . . ? C39 C40 H40A 110.5 . . ? O10 C40 H40B 110.5 . . ? C39 C40 H40B 110.5 . . ? H40A C40 H40B 108.7 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N3 Zn1 O1 C1 -108.98(12) . . . . ? N4 Zn1 O1 C1 126.20(12) . . . . ? N2 Zn1 O1 C1 10.99(12) . . . . ? N3 Zn1 O1 C4 30.02(12) . . . . ? N4 Zn1 O1 C4 -94.80(12) . . . . ? N2 Zn1 O1 C4 150.00(12) . . . . ? C4 O1 C1 C2 6.1(2) . . . . ? Zn1 O1 C1 C2 148.90(12) . . . . ? O1 C1 C2 C3 -28.4(2) . . . . ? C1 C2 C3 C4 38.90(19) . . . . ? C1 O1 C4 C3 18.9(2) . . . . ? Zn1 O1 C4 C3 -124.70(14) . . . . ? C2 C3 C4 O1 -36.0(2) . . . . ? N3 Zn1 N2 C5 -179.28(14) . . . . ? N4 Zn1 N2 C5 -36.37(16) . . . . ? O1 Zn1 N2 C5 72.94(15) . . . . ? N3 Zn1 N2 C8 18.18(18) . . . . ? N4 Zn1 N2 C8 161.10(15) . . . . ? O1 Zn1 N2 C8 -89.59(16) . . . . ? N3 Zn1 N2 Na1 -79.55(9) . . . 1_455 ? N4 Zn1 N2 Na1 63.36(10) . . . 1_455 ? O1 Zn1 N2 Na1 172.67(7) . . . 1_455 ? C8 N2 C5 C6 -0.7(2) . . . . ? Zn1 N2 C5 C6 -166.21(13) . . . . ? Na1 N2 C5 C6 64.65(14) 1_455 . . . ? C8 N2 C5 Na1 -65.39(12) . . . 1_455 ? Zn1 N2 C5 Na1 129.14(12) . . . 1_455 ? N2 C5 C6 C7 0.3(2) . . . . ? Na1 C5 C6 C7 70.03(14) 1_455 . . . ? N2 C5 C6 Na1 -69.68(13) . . . 1_455 ? C5 C6 C7 C8 0.2(2) . . . . ? Na1 C6 C7 C8 74.98(15) 1_455 . . . ? C5 C6 C7 Na1 -74.79(13) . . . 1_455 ? C6 C7 C8 N2 -0.7(2) . . . . ? Na1 C7 C8 N2 71.49(14) 1_455 . . . ? C6 C7 C8 Na1 -72.15(13) . . . 1_455 ? C5 N2 C8 C7 0.9(2) . . . . ? Zn1 N2 C8 C7 166.22(13) . . . . ? Na1 N2 C8 C7 -65.66(14) 1_455 . . . ? C5 N2 C8 Na1 66.52(12) . . . 1_455 ? Zn1 N2 C8 Na1 -128.12(12) . . . 1_455 ? N4 Zn1 N3 C12 -10.96(18) . . . . ? N2 Zn1 N3 C12 129.51(15) . . . . ? O1 Zn1 N3 C12 -126.28(15) . . . . ? N4 Zn1 N3 C9 167.62(13) . . . . ? N2 Zn1 N3 C9 -51.92(16) . . . . ? O1 Zn1 N3 C9 52.30(15) . . . . ? C12 N3 C9 C10 0.1(2) . . . . ? Zn1 N3 C9 C10 -178.70(12) . . . . ? N3 C9 C10 C11 -0.1(2) . . . . ? C9 C10 C11 C12 0.1(2) . . . . ? C9 N3 C12 C11 -0.1(2) . . . . ? Zn1 N3 C12 C11 178.70(13) . . . . ? C10 C11 C12 N3 0.0(2) . . . . ? N3 Zn1 N4 C16 34.09(16) . . . . ? N2 Zn1 N4 C16 -108.26(14) . . . . ? O1 Zn1 N4 C16 148.02(13) . . . . ? N3 Zn1 N4 C13 -162.21(13) . . . . ? N2 Zn1 N4 C13 55.44(15) . . . . ? O1 Zn1 N4 C13 -48.28(14) . . . . ? C16 N4 C13 C14 0.03(18) . . . . ? Zn1 N4 C13 C14 -166.44(11) . . . . ? N4 C13 C14 C15 0.08(19) . . . . ? N4 C13 C14 Na1 -71.90(13) . . . . ? O10 Na1 C14 C13 94.02(13) . . . . ? O9 Na1 C14 C13 -164.39(12) . . . . ? C15 Na1 C14 C13 105.90(15) . . . . ? C7 Na1 C14 C13 -27.75(13) 1_655 . . . ? C6 Na1 C14 C13 -57.80(12) 1_655 . . . ? C8 Na1 C14 C13 -18.81(15) 1_655 . . . ? C5 Na1 C14 C13 -73.58(13) 1_655 . . . ? N2 Na1 C14 C13 -51.99(15) 1_655 . . . ? C16 Na1 C14 C13 67.90(12) . . . . ? O10 Na1 C14 C15 -11.87(12) . . . . ? O9 Na1 C14 C15 89.72(10) . . . . ? C7 Na1 C14 C15 -133.65(11) 1_655 . . . ? C6 Na1 C14 C15 -163.70(10) 1_655 . . . ? C8 Na1 C14 C15 -124.71(11) 1_655 . . . ? C5 Na1 C14 C15 -179.47(10) 1_655 . . . ? N2 Na1 C14 C15 -157.89(10) 1_655 . . . ? C16 Na1 C14 C15 -38.00(10) . . . . ? C13 C14 C15 C16 -0.15(19) . . . . ? Na1 C14 C15 C16 88.87(12) . . . . ? C13 C14 C15 Na1 -89.02(12) . . . . ? O10 Na1 C15 C16 64.34(12) . . . . ? O9 Na1 C15 C16 162.23(12) . . . . ? C7 Na1 C15 C16 -51.22(14) 1_655 . . . ? C6 Na1 C15 C16 -86.18(13) 1_655 . . . ? C14 Na1 C15 C16 -106.00(16) . . . . ? C8 Na1 C15 C16 -23.74(17) 1_655 . . . ? C5 Na1 C15 C16 -105.09(15) 1_655 . . . ? N2 Na1 C15 C16 -37.2(3) 1_655 . . . ? O10 Na1 C15 C14 170.34(10) . . . . ? O9 Na1 C15 C14 -91.77(10) . . . . ? C7 Na1 C15 C14 54.78(12) 1_655 . . . ? C6 Na1 C15 C14 19.82(13) 1_655 . . . ? C8 Na1 C15 C14 82.26(13) 1_655 . . . ? C5 Na1 C15 C14 0.91(17) 1_655 . . . ? N2 Na1 C15 C14 68.8(3) 1_655 . . . ? C16 Na1 C15 C14 106.00(16) . . . . ? C13 N4 C16 C15 -0.13(19) . . . . ? Zn1 N4 C16 C15 166.15(11) . . . . ? C13 N4 C16 Na1 59.19(11) . . . . ? Zn1 N4 C16 Na1 -134.54(10) . . . . ? C14 C15 C16 N4 0.17(19) . . . . ? Na1 C15 C16 N4 78.86(13) . . . . ? C14 C15 C16 Na1 -78.69(12) . . . . ? O10 Na1 C16 N4 130.55(10) . . . . ? O9 Na1 C16 N4 -133.71(10) . . . . ? C15 Na1 C16 N4 -113.55(16) . . . . ? C7 Na1 C16 N4 22.60(11) 1_655 . . . ? C6 Na1 C16 N4 -3.23(12) 1_655 . . . ? C14 Na1 C16 N4 -70.45(11) . . . . ? C8 Na1 C16 N4 49.62(11) 1_655 . . . ? C5 Na1 C16 N4 6.30(15) 1_655 . . . ? N2 Na1 C16 N4 52.84(13) 1_655 . . . ? O10 Na1 C16 C15 -115.90(12) . . . . ? O9 Na1 C16 C15 -20.16(13) . . . . ? C7 Na1 C16 C15 136.15(12) 1_655 . . . ? C6 Na1 C16 C15 110.32(12) 1_655 . . . ? C14 Na1 C16 C15 43.10(12) . . . . ? C8 Na1 C16 C15 163.17(12) 1_655 . . . ? C5 Na1 C16 C15 119.85(13) 1_655 . . . ? N2 Na1 C16 C15 166.39(12) 1_655 . . . ? O10 Na1 O9 C36 -69.81(16) . . . . ? C15 Na1 O9 C36 -166.65(16) . . . . ? C7 Na1 O9 C36 56.10(19) 1_655 . . . ? C6 Na1 O9 C36 66.17(16) 1_655 . . . ? C14 Na1 O9 C36 163.40(16) . . . . ? C8 Na1 O9 C36 18.37(19) 1_655 . . . ? C5 Na1 O9 C36 43.06(16) 1_655 . . . ? N2 Na1 O9 C36 18.09(16) 1_655 . . . ? C16 Na1 O9 C36 -157.73(15) . . . . ? O10 Na1 O9 C33 121.74(16) . . . . ? C15 Na1 O9 C33 24.89(16) . . . . ? C7 Na1 O9 C33 -112.35(16) 1_655 . . . ? C6 Na1 O9 C33 -102.29(16) 1_655 . . . ? C14 Na1 O9 C33 -5.05(16) . . . . ? C8 Na1 O9 C33 -150.08(15) 1_655 . . . ? C5 Na1 O9 C33 -125.40(16) 1_655 . . . ? N2 Na1 O9 C33 -150.36(15) 1_655 . . . ? C16 Na1 O9 C33 33.81(17) . . . . ? C36 O9 C33 C34 -21.3(2) . . . . ? Na1 O9 C33 C34 148.74(14) . . . . ? O9 C33 C34 C35 -1.5(2) . . . . ? C33 C34 C35 C36 22.6(2) . . . . ? C33 O9 C36 C35 36.3(2) . . . . ? Na1 O9 C36 C35 -134.21(15) . . . . ? C34 C35 C36 O9 -36.2(2) . . . . ? O9 Na1 O10 C37 37.45(13) . . . . ? C15 Na1 O10 C37 130.85(13) . . . . ? C7 Na1 O10 C37 -105.29(13) 1_655 . . . ? C6 Na1 O10 C37 -81.29(14) 1_655 . . . ? C14 Na1 O10 C37 136.78(12) . . . . ? C8 Na1 O10 C37 -90.61(13) 1_655 . . . ? C5 Na1 O10 C37 -54.82(13) 1_655 . . . ? N2 Na1 O10 C37 -63.02(12) 1_655 . . . ? C16 Na1 O10 C37 154.85(13) . . . . ? O9 Na1 O10 C40 -172.77(13) . . . . ? C15 Na1 O10 C40 -79.37(14) . . . . ? C7 Na1 O10 C40 44.49(14) 1_655 . . . ? C6 Na1 O10 C40 68.49(15) 1_655 . . . ? C14 Na1 O10 C40 -73.45(15) . . . . ? C8 Na1 O10 C40 59.16(13) 1_655 . . . ? C5 Na1 O10 C40 94.96(14) 1_655 . . . ? N2 Na1 O10 C40 86.76(13) 1_655 . . . ? C16 Na1 O10 C40 -55.37(13) . . . . ? C40 O10 C37 C38 16.8(2) . . . . ? Na1 O10 C37 C38 171.14(12) . . . . ? O10 C37 C38 C39 -34.4(2) . . . . ? C37 C38 C39 C40 38.2(2) . . . . ? C37 O10 C40 C39 8.1(2) . . . . ? Na1 O10 C40 C39 -144.21(14) . . . . ? C38 C39 C40 O10 -29.2(2) . . . . ? _diffrn_measured_fraction_theta_max 0.888 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.544 _refine_diff_density_min -0.268 _refine_diff_density_rms 0.063 #===END #----------------------------------------------- #---------------COMPOUND 4---------------------- #----------------------------------------------- data_srjg1103 _database_code_depnum_ccdc_archive 'CCDC 837244' #TrackingRef '- combined.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H48 N8 Na2 Zn' _chemical_formula_sum 'C28 H48 N8 Na2 Zn' _chemical_formula_weight 608.09 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 '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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'P -4 n 2' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'y, -x, -z' '-y, x, -z' 'x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, z+1/2' 'y+1/2, x+1/2, -z+1/2' '-y+1/2, -x+1/2, -z+1/2' _cell_length_a 12.2787(6) _cell_length_b 12.2787(6) _cell_length_c 11.2091(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1689.96(18) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 1475 _cell_measurement_theta_min 2.9617 _cell_measurement_theta_max 29.6415 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.195 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 648 _exptl_absorpt_coefficient_mu 0.781 _exptl_absorpt_correction_T_min 0.98325 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.34.46 (release 25-11-2010 CrysAlis171 .NET) (compiled Nov 25 2010,17:55:46) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Sapphire3, Gemini' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4944 _diffrn_reflns_av_R_equivalents 0.0440 _diffrn_reflns_av_sigmaI/netI 0.0578 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.97 _diffrn_reflns_theta_max 27.99 _reflns_number_total 1938 _reflns_number_gt 1532 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.34.46 (release 25-11-2010 CrysAlis171 .NET) (compiled Nov 25 2010,17:55:46) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.34.46 (release 25-11-2010 CrysAlis171 .NET) (compiled Nov 25 2010,17:55:46) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.34.46 (release 25-11-2010 CrysAlis171 .NET) (compiled Nov 25 2010,17:55:46) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _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^)+(0.0283P)^2^+0.5242P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary patterson _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 0.01(2) _refine_ls_number_reflns 1938 _refine_ls_number_parameters 104 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.0672 _refine_ls_R_factor_gt 0.0464 _refine_ls_wR_factor_ref 0.0902 _refine_ls_wR_factor_gt 0.0825 _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_restrained_S_all 1.070 _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 1.0000 0.5000 0.2500 0.02623(17) Uani 1 4 d S . . N1 N 1.0054(2) 0.6344(2) 0.1519(2) 0.0277(6) Uani 1 1 d . A . C1 C 1.0691(3) 0.6491(3) 0.0536(3) 0.0358(8) Uani 1 1 d . A . H1A H 1.1043 0.5922 0.0109 0.043 Uiso 1 1 calc R . . C2 C 1.0750(3) 0.7581(3) 0.0248(3) 0.0448(10) Uani 1 1 d . A . H2A H 1.1146 0.7896 -0.0393 0.054 Uiso 1 1 calc R . . C3 C 1.0114(3) 0.8128(3) 0.1080(4) 0.0475(10) Uani 1 1 d . . . H3A H 0.9994 0.8891 0.1118 0.057 Uiso 1 1 calc R . . C4 C 0.9694(3) 0.7356(3) 0.1834(3) 0.0328(8) Uani 1 1 d . A . H4A H 0.9220 0.7505 0.2484 0.039 Uiso 1 1 calc R . . Na1 Na 1.19888(8) 0.69888(8) 0.2500 0.0298(3) Uani 1 2 d S . . N2 N 1.3772(2) 0.7459(2) 0.1599(2) 0.0322(6) Uani 1 1 d D A . C10 C 1.3935(4) 0.8636(4) 0.1889(4) 0.0538(19) Uani 0.782(7) 1 d PD A 1 H10A H 1.4710 0.8823 0.1759 0.065 Uiso 0.782(7) 1 calc PR A 1 H10B H 1.3497 0.9079 0.1328 0.065 Uiso 0.782(7) 1 calc PR A 1 C11 C 1.3765(8) 0.7387(6) 0.0291(6) 0.055(3) Uani 0.782(7) 1 d PD A 1 H11A H 1.4477 0.7610 -0.0020 0.083 Uiso 0.782(7) 1 calc PR A 1 H11B H 1.3199 0.7868 -0.0029 0.083 Uiso 0.782(7) 1 calc PR A 1 H11C H 1.3614 0.6635 0.0050 0.083 Uiso 0.782(7) 1 calc PR A 1 C12 C 1.4682(4) 0.6842(5) 0.2048(5) 0.0474(16) Uani 0.782(7) 1 d PD A 1 H12A H 1.5363 0.7160 0.1752 0.071 Uiso 0.782(7) 1 calc PR A 1 H12B H 1.4625 0.6086 0.1775 0.071 Uiso 0.782(7) 1 calc PR A 1 H12C H 1.4678 0.6860 0.2922 0.071 Uiso 0.782(7) 1 calc PR A 1 C10A C 1.4147(10) 0.8264(10) 0.247(2) 0.0538(19) Uani 0.22 1 d PD A 2 H10C H 1.4848 0.8585 0.2208 0.065 Uiso 0.218(7) 1 calc PR A 2 H10D H 1.4251 0.7921 0.3257 0.065 Uiso 0.218(7) 1 calc PR A 2 C12A C 1.4472(17) 0.6444(15) 0.158(2) 0.0474(16) Uani 0.22 1 d PD A 2 H12D H 1.5204 0.6630 0.1296 0.071 Uiso 0.218(7) 1 calc PR A 2 H12E H 1.4146 0.5904 0.1046 0.071 Uiso 0.218(7) 1 calc PR A 2 H12F H 1.4520 0.6142 0.2388 0.071 Uiso 0.218(7) 1 calc PR A 2 C11A C 1.356(3) 0.777(3) 0.0352(19) 0.055(3) Uani 0.22 1 d PD A 2 H11D H 1.4246 0.7943 -0.0045 0.083 Uiso 0.218(7) 1 calc PR A 2 H11E H 1.3077 0.8403 0.0333 0.083 Uiso 0.218(7) 1 calc PR A 2 H11F H 1.3206 0.7157 -0.0063 0.083 Uiso 0.218(7) 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0228(2) 0.0228(2) 0.0331(3) 0.000 0.000 -0.0027(3) N1 0.0266(13) 0.0291(14) 0.0275(12) 0.0007(12) -0.0024(13) 0.0007(11) C1 0.0323(18) 0.046(2) 0.0295(16) 0.0003(17) -0.0017(16) 0.0044(16) C2 0.040(2) 0.053(2) 0.0420(19) 0.023(2) -0.0141(18) -0.0134(18) C3 0.048(2) 0.0251(17) 0.069(3) 0.0083(19) -0.025(2) -0.0014(18) C4 0.0315(17) 0.0287(17) 0.0382(18) -0.0035(15) -0.0088(15) 0.0056(13) Na1 0.0297(5) 0.0297(5) 0.0302(7) 0.0009(9) -0.0009(9) -0.0075(6) N2 0.0318(15) 0.0379(16) 0.0270(13) 0.0016(13) 0.0003(13) -0.0015(12) C10 0.045(3) 0.045(4) 0.071(4) -0.008(3) 0.028(3) -0.017(3) C11 0.046(5) 0.082(7) 0.036(2) 0.013(3) -0.003(3) -0.017(5) C12 0.035(3) 0.062(4) 0.046(3) 0.006(3) 0.005(2) 0.009(2) C10A 0.045(3) 0.045(4) 0.071(4) -0.008(3) 0.028(3) -0.017(3) C12A 0.035(3) 0.062(4) 0.046(3) 0.006(3) 0.005(2) 0.009(2) C11A 0.046(5) 0.082(7) 0.036(2) 0.013(3) -0.003(3) -0.017(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 N1 1.984(2) 7_545 ? Zn1 N1 1.984(2) 2_765 ? Zn1 N1 1.984(2) . ? Zn1 N1 1.984(2) 8_665 ? Zn1 Na1 3.4534(14) 2_765 ? Zn1 Na1 3.4534(14) . ? N1 C1 1.363(4) . ? N1 C4 1.365(4) . ? N1 Na1 2.735(3) . ? C1 C2 1.379(5) . ? C1 Na1 2.786(3) . ? C1 H1A 0.9500 . ? C2 C3 1.389(5) . ? C2 Na1 3.036(3) . ? C2 H2A 0.9500 . ? C3 C4 1.371(5) . ? C3 Na1 3.129(3) . ? C3 H3A 0.9500 . ? C4 Na1 2.950(3) . ? C4 H4A 0.9500 . ? Na1 N2 2.480(3) 7_545 ? Na1 N2 2.480(3) . ? Na1 N1 2.735(3) 7_545 ? Na1 C1 2.786(3) 7_545 ? Na1 C4 2.950(3) 7_545 ? Na1 C2 3.036(3) 7_545 ? Na1 C10A 3.078(16) . ? Na1 C10A 3.078(16) 7_545 ? N2 C12 1.440(5) . ? N2 C10A 1.461(16) . ? N2 C11 1.468(7) . ? N2 C11A 1.472(19) . ? N2 C10 1.495(5) . ? N2 C12A 1.514(15) . ? C10 C10 1.465(7) 7_545 ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C10A C10A 1.534(10) 7_545 ? C10A H10C 0.9900 . ? C10A H10D 0.9900 . ? C12A H12D 0.9800 . ? C12A H12E 0.9800 . ? C12A H12F 0.9800 . ? C11A H11D 0.9800 . ? C11A H11E 0.9800 . ? C11A H11F 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 N1 111.26(14) 7_545 2_765 ? N1 Zn1 N1 104.55(14) 7_545 . ? N1 Zn1 N1 112.71(14) 2_765 . ? N1 Zn1 N1 112.71(14) 7_545 8_665 ? N1 Zn1 N1 104.55(14) 2_765 8_665 ? N1 Zn1 N1 111.26(14) . 8_665 ? N1 Zn1 Na1 127.72(7) 7_545 2_765 ? N1 Zn1 Na1 52.28(7) 2_765 2_765 ? N1 Zn1 Na1 127.72(7) . 2_765 ? N1 Zn1 Na1 52.28(7) 8_665 2_765 ? N1 Zn1 Na1 52.28(7) 7_545 . ? N1 Zn1 Na1 127.72(7) 2_765 . ? N1 Zn1 Na1 52.28(7) . . ? N1 Zn1 Na1 127.72(7) 8_665 . ? Na1 Zn1 Na1 180.0 2_765 . ? C1 N1 C4 106.0(3) . . ? C1 N1 Zn1 125.2(2) . . ? C4 N1 Zn1 127.1(2) . . ? C1 N1 Na1 77.82(16) . . ? C4 N1 Na1 85.06(17) . . ? Zn1 N1 Na1 92.70(9) . . ? N1 C1 C2 110.3(3) . . ? N1 C1 Na1 73.61(16) . . ? C2 C1 Na1 86.7(2) . . ? N1 C1 H1A 124.8 . . ? C2 C1 H1A 124.8 . . ? Na1 C1 H1A 107.3 . . ? C1 C2 C3 106.4(3) . . ? C1 C2 Na1 66.38(19) . . ? C3 C2 Na1 80.7(2) . . ? C1 C2 H2A 126.8 . . ? C3 C2 H2A 126.8 . . ? Na1 C2 H2A 118.0 . . ? C4 C3 C2 107.0(3) . . ? C4 C3 Na1 69.76(19) . . ? C2 C3 Na1 73.28(19) . . ? C4 C3 H3A 126.5 . . ? C2 C3 H3A 126.5 . . ? Na1 C3 H3A 122.2 . . ? N1 C4 C3 110.3(3) . . ? N1 C4 Na1 67.47(16) . . ? C3 C4 Na1 84.4(2) . . ? N1 C4 H4A 124.8 . . ? C3 C4 H4A 124.8 . . ? Na1 C4 H4A 114.9 . . ? N2 Na1 N2 75.81(13) 7_545 . ? N2 Na1 N1 128.43(8) 7_545 . ? N2 Na1 N1 132.12(8) . . ? N2 Na1 N1 132.12(8) 7_545 7_545 ? N2 Na1 N1 128.43(8) . 7_545 ? N1 Na1 N1 70.05(11) . 7_545 ? N2 Na1 C1 130.46(10) 7_545 . ? N2 Na1 C1 103.56(9) . . ? N1 Na1 C1 28.57(8) . . ? N1 Na1 C1 87.79(10) 7_545 . ? N2 Na1 C1 103.56(9) 7_545 7_545 ? N2 Na1 C1 130.46(10) . 7_545 ? N1 Na1 C1 87.79(10) . 7_545 ? N1 Na1 C1 28.57(8) 7_545 7_545 ? C1 Na1 C1 111.92(15) . 7_545 ? N2 Na1 C4 100.97(9) 7_545 . ? N2 Na1 C4 134.82(9) . . ? N1 Na1 C4 27.47(8) . . ? N1 Na1 C4 87.60(9) 7_545 . ? C1 Na1 C4 44.53(9) . . ? C1 Na1 C4 94.46(10) 7_545 . ? N2 Na1 C4 134.82(9) 7_545 7_545 ? N2 Na1 C4 100.97(9) . 7_545 ? N1 Na1 C4 87.60(9) . 7_545 ? N1 Na1 C4 27.47(8) 7_545 7_545 ? C1 Na1 C4 94.46(10) . 7_545 ? C1 Na1 C4 44.53(9) 7_545 7_545 ? C4 Na1 C4 110.88(13) . 7_545 ? N2 Na1 C2 104.12(10) 7_545 . ? N2 Na1 C2 92.75(9) . . ? N1 Na1 C2 45.54(8) . . ? N1 Na1 C2 113.41(10) 7_545 . ? C1 Na1 C2 26.97(9) . . ? C1 Na1 C2 133.17(11) 7_545 . ? C4 Na1 C2 43.46(10) . . ? C4 Na1 C2 121.06(11) 7_545 . ? N2 Na1 C2 92.75(9) 7_545 7_545 ? N2 Na1 C2 104.12(10) . 7_545 ? N1 Na1 C2 113.41(10) . 7_545 ? N1 Na1 C2 45.54(8) 7_545 7_545 ? C1 Na1 C2 133.17(11) . 7_545 ? C1 Na1 C2 26.97(9) 7_545 7_545 ? C4 Na1 C2 121.06(11) . 7_545 ? C4 Na1 C2 43.46(10) 7_545 7_545 ? C2 Na1 C2 158.68(14) . 7_545 ? N2 Na1 C10A 49.9(2) 7_545 . ? N2 Na1 C10A 27.9(3) . . ? N1 Na1 C10A 152.9(4) . . ? N1 Na1 C10A 134.1(3) 7_545 . ? C1 Na1 C10A 126.5(4) . . ? C1 Na1 C10A 119.3(4) 7_545 . ? C4 Na1 C10A 137.8(2) . . ? C4 Na1 C10A 110.9(2) 7_545 . ? C2 Na1 C10A 107.4(4) . . ? C2 Na1 C10A 93.4(4) 7_545 . ? N2 Na1 C10A 27.9(3) 7_545 7_545 ? N2 Na1 C10A 49.9(2) . 7_545 ? N1 Na1 C10A 134.1(3) . 7_545 ? N1 Na1 C10A 152.9(4) 7_545 7_545 ? C1 Na1 C10A 119.3(4) . 7_545 ? C1 Na1 C10A 126.5(4) 7_545 7_545 ? C4 Na1 C10A 110.9(2) . 7_545 ? C4 Na1 C10A 137.8(2) 7_545 7_545 ? C2 Na1 C10A 93.4(4) . 7_545 ? C2 Na1 C10A 107.4(4) 7_545 7_545 ? C10A Na1 C10A 28.9(2) . 7_545 ? C12 N2 C10A 83.1(4) . . ? C12 N2 C11 108.8(4) . . ? C10A N2 C11 135.0(10) . . ? C12 N2 C11A 127.3(16) . . ? C10A N2 C11A 121.0(18) . . ? C12 N2 C10 109.2(4) . . ? C11 N2 C10 106.0(4) . . ? C11A N2 C10 89.0(16) . . ? C10A N2 C12A 112.8(10) . . ? C11 N2 C12A 86.6(9) . . ? C11A N2 C12A 107.5(17) . . ? C10 N2 C12A 136.3(9) . . ? C12 N2 Na1 114.8(3) . . ? C10A N2 Na1 99.5(7) . . ? C11 N2 Na1 112.8(4) . . ? C11A N2 Na1 106.7(17) . . ? C10 N2 Na1 104.7(2) . . ? C12A N2 Na1 108.4(9) . . ? C10 C10 N2 114.4(3) 7_545 . ? C10 C10 H10A 108.7 7_545 . ? N2 C10 H10A 108.7 . . ? C10 C10 H10B 108.7 7_545 . ? N2 C10 H10B 108.7 . . ? H10A C10 H10B 107.6 . . ? N2 C11 H11A 109.5 . . ? N2 C11 H11B 109.5 . . ? N2 C11 H11C 109.5 . . ? N2 C12 H12A 109.5 . . ? N2 C12 H12B 109.5 . . ? N2 C12 H12C 109.5 . . ? N2 C10A C10A 106.8(14) . 7_545 ? N2 C10A Na1 52.6(5) . . ? C10A C10A Na1 75.57(12) 7_545 . ? N2 C10A H10C 110.4 . . ? C10A C10A H10C 110.4 7_545 . ? Na1 C10A H10C 162.7 . . ? N2 C10A H10D 110.4 . . ? C10A C10A H10D 110.4 7_545 . ? Na1 C10A H10D 83.3 . . ? H10C C10A H10D 108.6 . . ? N2 C12A H12D 109.5 . . ? N2 C12A H12E 109.5 . . ? H12D C12A H12E 109.5 . . ? N2 C12A H12F 109.5 . . ? H12D C12A H12F 109.5 . . ? H12E C12A H12F 109.5 . . ? N2 C11A H11D 109.5 . . ? N2 C11A H11E 109.5 . . ? H11D C11A H11E 109.5 . . ? N2 C11A H11F 109.5 . . ? H11D C11A H11F 109.5 . . ? H11E C11A H11F 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 N1 Zn1 N1 C1 77.0(2) 7_545 . . . ? N1 Zn1 N1 C1 -44.0(2) 2_765 . . . ? N1 Zn1 N1 C1 -161.1(3) 8_665 . . . ? Na1 Zn1 N1 C1 -103.0(2) 2_765 . . . ? Na1 Zn1 N1 C1 77.0(2) . . . . ? N1 Zn1 N1 C4 -85.8(2) 7_545 . . . ? N1 Zn1 N1 C4 153.2(3) 2_765 . . . ? N1 Zn1 N1 C4 36.1(2) 8_665 . . . ? Na1 Zn1 N1 C4 94.2(2) 2_765 . . . ? Na1 Zn1 N1 C4 -85.8(2) . . . . ? N1 Zn1 N1 Na1 0.0 7_545 . . . ? N1 Zn1 N1 Na1 -120.99(9) 2_765 . . . ? N1 Zn1 N1 Na1 121.94(9) 8_665 . . . ? Na1 Zn1 N1 Na1 180.0 2_765 . . . ? C4 N1 C1 C2 1.2(3) . . . . ? Zn1 N1 C1 C2 -164.6(2) . . . . ? Na1 N1 C1 C2 -80.0(2) . . . . ? C4 N1 C1 Na1 81.2(2) . . . . ? Zn1 N1 C1 Na1 -84.63(18) . . . . ? N1 C1 C2 C3 -0.7(4) . . . . ? Na1 C1 C2 C3 -71.8(3) . . . . ? N1 C1 C2 Na1 71.2(2) . . . . ? C1 C2 C3 C4 -0.1(4) . . . . ? Na1 C2 C3 C4 -62.0(2) . . . . ? C1 C2 C3 Na1 61.9(2) . . . . ? C1 N1 C4 C3 -1.3(3) . . . . ? Zn1 N1 C4 C3 164.2(2) . . . . ? Na1 N1 C4 C3 74.5(2) . . . . ? C1 N1 C4 Na1 -75.82(19) . . . . ? Zn1 N1 C4 Na1 89.7(2) . . . . ? C2 C3 C4 N1 0.9(4) . . . . ? Na1 C3 C4 N1 -63.4(2) . . . . ? C2 C3 C4 Na1 64.3(2) . . . . ? C1 N1 Na1 N2 106.0(2) . . . 7_545 ? C4 N1 Na1 N2 -1.5(2) . . . 7_545 ? Zn1 N1 Na1 N2 -128.52(10) . . . 7_545 ? C1 N1 Na1 N2 -1.2(2) . . . . ? C4 N1 Na1 N2 -108.7(2) . . . . ? Zn1 N1 Na1 N2 124.28(11) . . . . ? C1 N1 Na1 N1 -125.5(2) . . . 7_545 ? C4 N1 Na1 N1 127.0(2) . . . 7_545 ? Zn1 N1 Na1 N1 0.0 . . . 7_545 ? C4 N1 Na1 C1 -107.5(3) . . . . ? Zn1 N1 Na1 C1 125.5(2) . . . . ? C1 N1 Na1 C1 -148.43(15) . . . 7_545 ? C4 N1 Na1 C1 104.06(19) . . . 7_545 ? Zn1 N1 Na1 C1 -22.93(10) . . . 7_545 ? C1 N1 Na1 C4 107.5(3) . . . . ? Zn1 N1 Na1 C4 -127.0(2) . . . . ? C1 N1 Na1 C4 -103.86(19) . . . 7_545 ? C4 N1 Na1 C4 148.63(15) . . . 7_545 ? Zn1 N1 Na1 C4 21.63(9) . . . 7_545 ? C1 N1 Na1 C2 35.99(19) . . . . ? C4 N1 Na1 C2 -71.5(2) . . . . ? Zn1 N1 Na1 C2 161.49(16) . . . . ? C1 N1 Na1 C2 -139.79(19) . . . 7_545 ? C4 N1 Na1 C2 112.7(2) . . . 7_545 ? Zn1 N1 Na1 C2 -14.30(13) . . . 7_545 ? C1 N1 Na1 C10A 30.8(4) . . . . ? C4 N1 Na1 C10A -76.7(4) . . . . ? Zn1 N1 Na1 C10A 156.3(4) . . . . ? C1 N1 Na1 C10A 69.3(5) . . . 7_545 ? C4 N1 Na1 C10A -38.2(5) . . . 7_545 ? Zn1 N1 Na1 C10A -165.2(5) . . . 7_545 ? N1 C1 Na1 N2 -98.1(2) . . . 7_545 ? C2 C1 Na1 N2 14.2(3) . . . 7_545 ? N1 C1 Na1 N2 179.07(18) . . . . ? C2 C1 Na1 N2 -68.6(2) . . . . ? C2 C1 Na1 N1 112.3(3) . . . . ? N1 C1 Na1 N1 50.0(2) . . . 7_545 ? C2 C1 Na1 N1 162.3(2) . . . 7_545 ? N1 C1 Na1 C1 34.33(15) . . . 7_545 ? C2 C1 Na1 C1 146.7(2) . . . 7_545 ? N1 C1 Na1 C4 -38.85(17) . . . . ? C2 C1 Na1 C4 73.5(2) . . . . ? N1 C1 Na1 C4 76.65(19) . . . 7_545 ? C2 C1 Na1 C4 -171.0(2) . . . 7_545 ? N1 C1 Na1 C2 -112.3(3) . . . . ? N1 C1 Na1 C2 54.3(2) . . . 7_545 ? C2 C1 Na1 C2 166.64(13) . . . 7_545 ? N1 C1 Na1 C10A -163.1(2) . . . . ? C2 C1 Na1 C10A -50.8(3) . . . . ? N1 C1 Na1 C10A -129.6(3) . . . 7_545 ? C2 C1 Na1 C10A -17.3(3) . . . 7_545 ? N1 C4 Na1 N2 178.78(18) . . . 7_545 ? C3 C4 Na1 N2 64.0(2) . . . 7_545 ? N1 C4 Na1 N2 97.9(2) . . . . ? C3 C4 Na1 N2 -16.8(3) . . . . ? C3 C4 Na1 N1 -114.8(3) . . . . ? N1 C4 Na1 N1 -48.7(2) . . . 7_545 ? C3 C4 Na1 N1 -163.5(2) . . . 7_545 ? N1 C4 Na1 C1 40.57(17) . . . . ? C3 C4 Na1 C1 -74.2(2) . . . . ? N1 C4 Na1 C1 -76.47(19) . . . 7_545 ? C3 C4 Na1 C1 168.8(2) . . . 7_545 ? N1 C4 Na1 C4 -33.83(15) . . . 7_545 ? C3 C4 Na1 C4 -148.6(2) . . . 7_545 ? N1 C4 Na1 C2 79.8(2) . . . . ? C3 C4 Na1 C2 -35.0(2) . . . . ? N1 C4 Na1 C2 -81.2(2) . . . 7_545 ? C3 C4 Na1 C2 164.0(2) . . . 7_545 ? N1 C4 Na1 C10A 138.6(6) . . . . ? C3 C4 Na1 C10A 23.9(6) . . . . ? N1 C4 Na1 C10A 151.6(5) . . . 7_545 ? C3 C4 Na1 C10A 36.8(5) . . . 7_545 ? C1 C2 Na1 N2 -168.9(2) . . . 7_545 ? C3 C2 Na1 N2 -56.3(2) . . . 7_545 ? C1 C2 Na1 N2 115.0(2) . . . . ? C3 C2 Na1 N2 -132.4(2) . . . . ? C1 C2 Na1 N1 -38.30(19) . . . . ? C3 C2 Na1 N1 74.3(2) . . . . ? C1 C2 Na1 N1 -19.3(2) . . . 7_545 ? C3 C2 Na1 N1 93.3(2) . . . 7_545 ? C3 C2 Na1 C1 112.6(3) . . . . ? C1 C2 Na1 C1 -44.4(3) . . . 7_545 ? C3 C2 Na1 C1 68.2(3) . . . 7_545 ? C1 C2 Na1 C4 -77.8(2) . . . . ? C3 C2 Na1 C4 34.8(2) . . . . ? C1 C2 Na1 C4 10.5(3) . . . 7_545 ? C3 C2 Na1 C4 123.0(2) . . . 7_545 ? C1 C2 Na1 C2 -27.6(2) . . . 7_545 ? C3 C2 Na1 C2 85.0(2) . . . 7_545 ? C1 C2 Na1 C10A 139.2(3) . . . . ? C3 C2 Na1 C10A -108.2(3) . . . . ? C1 C2 Na1 C10A 165.0(3) . . . 7_545 ? C3 C2 Na1 C10A -82.5(3) . . . 7_545 ? N2 Na1 N2 C12 106.1(3) 7_545 . . . ? N1 Na1 N2 C12 -124.4(3) . . . . ? N1 Na1 N2 C12 -26.9(3) 7_545 . . . ? C1 Na1 N2 C12 -125.0(3) . . . . ? C1 Na1 N2 C12 10.3(3) 7_545 . . . ? C4 Na1 N2 C12 -162.4(3) . . . . ? C4 Na1 N2 C12 -27.6(3) 7_545 . . . ? C2 Na1 N2 C12 -150.0(3) . . . . ? C2 Na1 N2 C12 16.8(3) 7_545 . . . ? C10A Na1 N2 C12 86.7(7) . . . . ? C10A Na1 N2 C12 117.9(6) 7_545 . . . ? N2 Na1 N2 C10A 19.4(6) 7_545 . . . ? N1 Na1 N2 C10A 148.9(6) . . . . ? N1 Na1 N2 C10A -113.6(6) 7_545 . . . ? C1 Na1 N2 C10A 148.3(6) . . . . ? C1 Na1 N2 C10A -76.4(6) 7_545 . . . ? C4 Na1 N2 C10A 110.9(6) . . . . ? C4 Na1 N2 C10A -114.3(6) 7_545 . . . ? C2 Na1 N2 C10A 123.3(6) . . . . ? C2 Na1 N2 C10A -69.8(6) 7_545 . . . ? C10A Na1 N2 C10A 31.2(11) 7_545 . . . ? N2 Na1 N2 C11 -128.5(4) 7_545 . . . ? N1 Na1 N2 C11 1.0(4) . . . . ? N1 Na1 N2 C11 98.5(4) 7_545 . . . ? C1 Na1 N2 C11 0.4(4) . . . . ? C1 Na1 N2 C11 135.7(4) 7_545 . . . ? C4 Na1 N2 C11 -37.0(4) . . . . ? C4 Na1 N2 C11 97.8(4) 7_545 . . . ? C2 Na1 N2 C11 -24.6(4) . . . . ? C2 Na1 N2 C11 142.2(4) 7_545 . . . ? C10A Na1 N2 C11 -147.9(7) . . . . ? C10A Na1 N2 C11 -116.7(6) 7_545 . . . ? N2 Na1 N2 C11A -107.1(16) 7_545 . . . ? N1 Na1 N2 C11A 22.4(16) . . . . ? N1 Na1 N2 C11A 119.9(16) 7_545 . . . ? C1 Na1 N2 C11A 21.8(16) . . . . ? C1 Na1 N2 C11A 157.0(16) 7_545 . . . ? C4 Na1 N2 C11A -15.6(16) . . . . ? C4 Na1 N2 C11A 119.2(16) 7_545 . . . ? C2 Na1 N2 C11A -3.2(16) . . . . ? C2 Na1 N2 C11A 163.6(16) 7_545 . . . ? C10A Na1 N2 C11A -126.5(17) . . . . ? C10A Na1 N2 C11A -95.3(17) 7_545 . . . ? N2 Na1 N2 C10 -13.6(2) 7_545 . . . ? N1 Na1 N2 C10 115.8(2) . . . . ? N1 Na1 N2 C10 -146.7(2) 7_545 . . . ? C1 Na1 N2 C10 115.3(3) . . . . ? C1 Na1 N2 C10 -109.5(3) 7_545 . . . ? C4 Na1 N2 C10 77.8(3) . . . . ? C4 Na1 N2 C10 -147.4(2) 7_545 . . . ? C2 Na1 N2 C10 90.2(3) . . . . ? C2 Na1 N2 C10 -102.9(3) 7_545 . . . ? C10A Na1 N2 C10 -33.1(6) . . . . ? C10A Na1 N2 C10 -1.9(6) 7_545 . . . ? N2 Na1 N2 C12A 137.4(10) 7_545 . . . ? N1 Na1 N2 C12A -93.1(10) . . . . ? N1 Na1 N2 C12A 4.4(10) 7_545 . . . ? C1 Na1 N2 C12A -93.7(10) . . . . ? C1 Na1 N2 C12A 41.6(10) 7_545 . . . ? C4 Na1 N2 C12A -131.1(10) . . . . ? C4 Na1 N2 C12A 3.7(10) 7_545 . . . ? C2 Na1 N2 C12A -118.7(10) . . . . ? C2 Na1 N2 C12A 48.1(10) 7_545 . . . ? C10A Na1 N2 C12A 118.0(11) . . . . ? C10A Na1 N2 C12A 149.2(11) 7_545 . . . ? C12 N2 C10 C10 -80.9(6) . . . 7_545 ? C10A N2 C10 C10 -42.0(11) . . . 7_545 ? C11 N2 C10 C10 162.1(6) . . . 7_545 ? C11A N2 C10 C10 149.7(17) . . . 7_545 ? C12A N2 C10 C10 -95.7(14) . . . 7_545 ? Na1 N2 C10 C10 42.6(6) . . . 7_545 ? C12 N2 C10A C10A -170.2(17) . . . 7_545 ? C11 N2 C10A C10A 80.1(17) . . . 7_545 ? C11A N2 C10A C10A 60(3) . . . 7_545 ? C10 N2 C10A C10A 46.5(11) . . . 7_545 ? C12A N2 C10A C10A -170.7(16) . . . 7_545 ? Na1 N2 C10A C10A -56.1(17) . . . 7_545 ? C12 N2 C10A Na1 -114.1(3) . . . . ? C11 N2 C10A Na1 136.2(7) . . . . ? C11A N2 C10A Na1 116.2(19) . . . . ? C10 N2 C10A Na1 102.6(12) . . . . ? C12A N2 C10A Na1 -114.6(11) . . . . ? N2 Na1 C10A N2 -155.0(9) 7_545 . . . ? N1 Na1 C10A N2 -57.2(5) . . . . ? N1 Na1 C10A N2 91.1(8) 7_545 . . . ? C1 Na1 C10A N2 -39.4(6) . . . . ? C1 Na1 C10A N2 122.0(6) 7_545 . . . ? C4 Na1 C10A N2 -99.1(3) . . . . ? C4 Na1 C10A N2 73.3(7) 7_545 . . . ? C2 Na1 C10A N2 -61.0(5) . . . . ? C2 Na1 C10A N2 114.2(6) 7_545 . . . ? C10A Na1 C10A N2 -125(2) 7_545 . . . ? N2 Na1 C10A C10A -30.2(13) 7_545 . . 7_545 ? N2 Na1 C10A C10A 125(2) . . . 7_545 ? N1 Na1 C10A C10A 68(2) . . . 7_545 ? N1 Na1 C10A C10A -144.0(14) 7_545 . . 7_545 ? C1 Na1 C10A C10A 85.5(17) . . . 7_545 ? C1 Na1 C10A C10A -113.1(16) 7_545 . . 7_545 ? C4 Na1 C10A C10A 26(2) . . . 7_545 ? C4 Na1 C10A C10A -161.8(15) 7_545 . . 7_545 ? C2 Na1 C10A C10A 63.9(17) . . . 7_545 ? C2 Na1 C10A C10A -120.9(17) 7_545 . . 7_545 ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.356 _refine_diff_density_min -0.336 _refine_diff_density_rms 0.053 #===END #----------------------------------------------- #---------------COMPOUND 5---------------------- #----------------------------------------------- data_jg1104 _database_code_depnum_ccdc_archive 'CCDC 837245' #TrackingRef '- combined.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C34 H62 N10 Na2 Zn' _chemical_formula_sum 'C34 H62 N10 Na2 Zn' _chemical_formula_weight 722.29 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 '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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 19.0953(9) _cell_length_b 25.2534(13) _cell_length_c 17.1703(8) _cell_angle_alpha 90.00 _cell_angle_beta 102.034(5) _cell_angle_gamma 90.00 _cell_volume 8097.9(7) _cell_formula_units_Z 8 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 9635 _cell_measurement_theta_min 3.0080 _cell_measurement_theta_max 30.0958 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.185 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3104 _exptl_absorpt_coefficient_mu 0.664 _exptl_absorpt_correction_T_min 0.88446 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Eos' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 41267 _diffrn_reflns_av_R_equivalents 0.0378 _diffrn_reflns_av_sigmaI/netI 0.0633 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 27.00 _reflns_number_total 17641 _reflns_number_gt 12360 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _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^)+(0.0311P)^2^+2.9766P] 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 17641 _refine_ls_number_parameters 882 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0774 _refine_ls_R_factor_gt 0.0439 _refine_ls_wR_factor_ref 0.0984 _refine_ls_wR_factor_gt 0.0847 _refine_ls_goodness_of_fit_ref 1.015 _refine_ls_restrained_S_all 1.016 _refine_ls_shift/su_max 0.190 _refine_ls_shift/su_mean 0.003 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 0.340672(14) 0.363829(11) 0.555517(14) 0.02223(7) Uani 1 1 d . . . Na1 Na 0.44250(5) 0.27254(4) 0.70627(5) 0.0239(2) Uani 1 1 d . . . N1 N 0.53767(10) 0.31686(8) 0.80155(10) 0.0246(4) Uani 1 1 d . . . N2 N 0.50363(10) 0.19905(8) 0.78856(10) 0.0243(4) Uani 1 1 d . . . N3 N 0.35274(10) 0.23847(8) 0.77867(11) 0.0241(4) Uani 1 1 d . . . C1 C 0.51422(14) 0.34107(11) 0.86996(13) 0.0338(6) Uani 1 1 d . . . H1A H 0.5560 0.3547 0.9078 0.051 Uiso 1 1 calc R . . H1B H 0.4899 0.3144 0.8963 0.051 Uiso 1 1 calc R . . H1C H 0.4811 0.3702 0.8513 0.051 Uiso 1 1 calc R . . C2 C 0.57189(14) 0.35761(11) 0.76109(14) 0.0355(6) Uani 1 1 d . . . H2A H 0.6135 0.3721 0.7983 0.053 Uiso 1 1 calc R . . H2B H 0.5376 0.3861 0.7427 0.053 Uiso 1 1 calc R . . H2C H 0.5874 0.3419 0.7153 0.053 Uiso 1 1 calc R . . C3 C 0.58829(12) 0.27359(10) 0.82764(14) 0.0295(6) Uani 1 1 d . . . H3A H 0.6262 0.2863 0.8721 0.035 Uiso 1 1 calc R . . H3B H 0.6114 0.2637 0.7832 0.035 Uiso 1 1 calc R . . C4 C 0.55361(13) 0.22470(10) 0.85469(13) 0.0290(6) Uani 1 1 d . . . H4A H 0.5914 0.1991 0.8783 0.035 Uiso 1 1 calc R . . H4B H 0.5274 0.2349 0.8965 0.035 Uiso 1 1 calc R . . C5 C 0.54303(14) 0.16307(10) 0.74581(14) 0.0346(6) Uani 1 1 d . . . H5A H 0.5815 0.1826 0.7286 0.052 Uiso 1 1 calc R . . H5B H 0.5102 0.1485 0.6991 0.052 Uiso 1 1 calc R . . H5C H 0.5637 0.1341 0.7812 0.052 Uiso 1 1 calc R . . C6 C 0.44755(13) 0.16932(10) 0.81717(15) 0.0322(6) Uani 1 1 d . . . H6A H 0.4705 0.1470 0.8628 0.039 Uiso 1 1 calc R . . H6B H 0.4233 0.1454 0.7742 0.039 Uiso 1 1 calc R . . C7 C 0.39203(13) 0.20391(10) 0.84264(13) 0.0300(6) Uani 1 1 d . . . H7A H 0.3572 0.1810 0.8620 0.036 Uiso 1 1 calc R . . H7B H 0.4159 0.2264 0.8877 0.036 Uiso 1 1 calc R . . C8 C 0.31214(14) 0.27735(11) 0.81433(15) 0.0371(6) Uani 1 1 d . . . H8A H 0.3452 0.2990 0.8529 0.056 Uiso 1 1 calc R . . H8B H 0.2789 0.2589 0.8415 0.056 Uiso 1 1 calc R . . H8C H 0.2851 0.3002 0.7725 0.056 Uiso 1 1 calc R . . C9 C 0.30263(14) 0.20797(11) 0.71923(15) 0.0380(7) Uani 1 1 d . . . H9A H 0.2751 0.2321 0.6797 0.057 Uiso 1 1 calc R . . H9B H 0.2699 0.1883 0.7455 0.057 Uiso 1 1 calc R . . H9C H 0.3294 0.1831 0.6927 0.057 Uiso 1 1 calc R . . N4 N 0.40518(10) 0.30123(8) 0.55871(10) 0.0209(4) Uani 1 1 d . . . C10 C 0.47800(12) 0.30373(10) 0.56681(12) 0.0242(5) Uani 1 1 d . . . H10A H 0.5050 0.3356 0.5736 0.029 Uiso 1 1 calc R . . C11 C 0.50680(13) 0.25410(10) 0.56380(13) 0.0277(6) Uani 1 1 d . . . H11A H 0.5560 0.2456 0.5685 0.033 Uiso 1 1 calc R . . C12 C 0.44904(13) 0.21829(10) 0.55241(12) 0.0269(5) Uani 1 1 d . . . H12A H 0.4515 0.1809 0.5478 0.032 Uiso 1 1 calc R . . C13 C 0.38831(12) 0.24837(9) 0.54936(12) 0.0228(5) Uani 1 1 d . . . H13A H 0.3412 0.2345 0.5418 0.027 Uiso 1 1 calc R . . N5 N 0.24647(10) 0.33878(8) 0.57149(11) 0.0300(5) Uani 1 1 d . . . C14 C 0.20700(13) 0.29817(11) 0.53197(16) 0.0397(7) Uani 1 1 d . . . H14A H 0.2197 0.2788 0.4896 0.048 Uiso 1 1 calc R . . C15 C 0.14706(14) 0.28916(12) 0.56134(18) 0.0446(7) Uani 1 1 d . . . H15A H 0.1112 0.2632 0.5437 0.054 Uiso 1 1 calc R . . C16 C 0.14900(14) 0.32591(13) 0.62288(17) 0.0458(8) Uani 1 1 d . . . H16A H 0.1147 0.3297 0.6554 0.055 Uiso 1 1 calc R . . C17 C 0.21024(13) 0.35546(11) 0.62720(14) 0.0348(6) Uani 1 1 d . . . H17A H 0.2250 0.3835 0.6638 0.042 Uiso 1 1 calc R . . N6 N 0.38733(10) 0.41540(8) 0.63867(11) 0.0266(5) Uani 1 1 d . . . C18 C 0.38378(13) 0.41594(10) 0.71727(13) 0.0282(6) Uani 1 1 d . . . H18A H 0.3573 0.3913 0.7415 0.034 Uiso 1 1 calc R . . C19 C 0.42366(14) 0.45682(11) 0.75664(14) 0.0352(6) Uani 1 1 d . . . H19A H 0.4295 0.4654 0.8115 0.042 Uiso 1 1 calc R . . C20 C 0.45391(14) 0.48321(11) 0.70041(15) 0.0387(7) Uani 1 1 d . . . H20A H 0.4844 0.5133 0.7093 0.046 Uiso 1 1 calc R . . C21 C 0.43077(14) 0.45688(11) 0.62933(15) 0.0350(6) Uani 1 1 d . . . H21A H 0.4433 0.4663 0.5805 0.042 Uiso 1 1 calc R . . N7 N 0.32659(11) 0.40056(8) 0.44979(10) 0.0275(5) Uani 1 1 d . . . C22 C 0.37381(15) 0.43046(10) 0.41785(13) 0.0348(6) Uani 1 1 d . . . H22A H 0.4219 0.4375 0.4438 0.042 Uiso 1 1 calc R . . C23 C 0.34228(19) 0.44884(12) 0.34356(15) 0.0497(8) Uani 1 1 d . . . H23A H 0.3636 0.4706 0.3098 0.060 Uiso 1 1 calc R . . C24 C 0.27305(19) 0.42914(12) 0.32793(15) 0.0517(9) Uani 1 1 d . . . H24A H 0.2377 0.4350 0.2809 0.062 Uiso 1 1 calc R . . C25 C 0.26471(15) 0.39938(11) 0.39305(14) 0.0400(7) Uani 1 1 d . . . H25A H 0.2224 0.3809 0.3976 0.048 Uiso 1 1 calc R . . Na2 Na 0.27116(5) 0.48822(4) 0.47958(6) 0.0318(2) Uani 1 1 d . . . N8 N 0.13648(11) 0.48476(8) 0.46346(12) 0.0313(5) Uani 1 1 d . . . N9 N 0.24111(10) 0.54622(8) 0.58308(10) 0.0247(4) Uani 1 1 d . . . N10 N 0.32856(11) 0.57560(8) 0.46295(11) 0.0301(5) Uani 1 1 d . . . C30 C 0.11129(16) 0.51824(13) 0.39388(16) 0.0528(8) Uani 1 1 d . . . H30A H 0.1368 0.5521 0.4010 0.079 Uiso 1 1 calc R . . H30B H 0.0598 0.5246 0.3878 0.079 Uiso 1 1 calc R . . H30C H 0.1203 0.5005 0.3462 0.079 Uiso 1 1 calc R . . C31 C 0.10137(14) 0.43235(11) 0.45036(17) 0.0450(7) Uani 1 1 d . . . H31A H 0.1080 0.4178 0.3995 0.068 Uiso 1 1 calc R . . H31B H 0.0501 0.4362 0.4492 0.068 Uiso 1 1 calc R . . H31C H 0.1228 0.4084 0.4937 0.068 Uiso 1 1 calc R . . C32 C 0.12010(13) 0.50838(11) 0.53527(15) 0.0350(6) Uani 1 1 d . . . H32A H 0.1286 0.4817 0.5784 0.042 Uiso 1 1 calc R . . H32B H 0.0687 0.5179 0.5247 0.042 Uiso 1 1 calc R . . C33 C 0.16400(13) 0.55732(10) 0.56358(14) 0.0306(6) Uani 1 1 d . . . H33A H 0.1542 0.5847 0.5215 0.037 Uiso 1 1 calc R . . H33B H 0.1491 0.5716 0.6113 0.037 Uiso 1 1 calc R . . C34 C 0.25987(15) 0.51917(12) 0.66076(14) 0.0442(7) Uani 1 1 d . . . H34A H 0.3114 0.5118 0.6735 0.066 Uiso 1 1 calc R . . H34B H 0.2333 0.4858 0.6583 0.066 Uiso 1 1 calc R . . H34C H 0.2474 0.5419 0.7021 0.066 Uiso 1 1 calc R . . C35 C 0.28284(14) 0.59521(11) 0.58556(15) 0.0354(6) Uani 1 1 d . . . H35A H 0.3312 0.5893 0.6186 0.042 Uiso 1 1 calc R . . H35B H 0.2595 0.6233 0.6114 0.042 Uiso 1 1 calc R . . C36 C 0.28991(16) 0.61388(11) 0.50475(16) 0.0437(7) Uani 1 1 d . . . H36A H 0.2415 0.6201 0.4718 0.052 Uiso 1 1 calc R . . H36B H 0.3158 0.6481 0.5103 0.052 Uiso 1 1 calc R . . C37 C 0.31783(18) 0.59304(13) 0.38016(16) 0.0572(9) Uani 1 1 d . . . H37A H 0.3454 0.5703 0.3513 0.086 Uiso 1 1 calc R . . H37B H 0.3340 0.6298 0.3784 0.086 Uiso 1 1 calc R . . H37C H 0.2669 0.5908 0.3552 0.086 Uiso 1 1 calc R . . C38 C 0.40423(15) 0.57556(13) 0.49777(18) 0.0516(8) Uani 1 1 d . . . H38A H 0.4293 0.5530 0.4660 0.077 Uiso 1 1 calc R . . H38B H 0.4119 0.5619 0.5523 0.077 Uiso 1 1 calc R . . H38C H 0.4228 0.6118 0.4986 0.077 Uiso 1 1 calc R . . Zn2 Zn 0.162407(14) 0.619098(10) 0.952520(14) 0.02153(7) Uani 1 1 d . . . Na3 Na 0.22160(5) 0.48529(4) 1.02289(5) 0.0290(2) Uani 1 1 d . . . N11 N 0.15359(11) 0.40192(8) 1.03501(11) 0.0282(5) Uani 1 1 d . . . N12 N 0.23936(11) 0.42561(8) 0.91080(11) 0.0294(5) Uani 1 1 d . . . N13 N 0.35419(11) 0.46881(8) 1.04586(11) 0.0289(5) Uani 1 1 d . . . C51 C 0.07719(14) 0.41147(11) 1.00438(16) 0.0406(7) Uani 1 1 d . . . H51A H 0.0592 0.4361 1.0397 0.061 Uiso 1 1 calc R . . H51B H 0.0510 0.3779 1.0020 0.061 Uiso 1 1 calc R . . H51C H 0.0702 0.4268 0.9509 0.061 Uiso 1 1 calc R . . C52 C 0.16331(17) 0.38256(12) 1.11713(15) 0.0493(8) Uani 1 1 d . . . H52A H 0.2146 0.3799 1.1406 0.074 Uiso 1 1 calc R . . H52B H 0.1411 0.3476 1.1172 0.074 Uiso 1 1 calc R . . H52C H 0.1408 0.4073 1.1485 0.074 Uiso 1 1 calc R . . C53 C 0.18081(16) 0.36165(10) 0.98762(16) 0.0400(7) Uani 1 1 d . . . H53A H 0.1478 0.3310 0.9804 0.048 Uiso 1 1 calc R . . H53B H 0.2280 0.3492 1.0175 0.048 Uiso 1 1 calc R . . C54 C 0.18891(16) 0.38095(10) 0.90704(15) 0.0394(7) Uani 1 1 d . . . H54A H 0.2057 0.3513 0.8780 0.047 Uiso 1 1 calc R . . H54B H 0.1414 0.3921 0.8763 0.047 Uiso 1 1 calc R . . C55 C 0.22516(16) 0.45168(11) 0.83231(14) 0.0428(7) Uani 1 1 d . . . H55A H 0.1776 0.4680 0.8224 0.064 Uiso 1 1 calc R . . H55B H 0.2271 0.4253 0.7909 0.064 Uiso 1 1 calc R . . H55C H 0.2614 0.4790 0.8314 0.064 Uiso 1 1 calc R . . C56 C 0.31416(14) 0.40744(11) 0.93145(16) 0.0388(7) Uani 1 1 d . . . H56A H 0.3284 0.3943 0.8827 0.047 Uiso 1 1 calc R . . H56B H 0.3176 0.3774 0.9692 0.047 Uiso 1 1 calc R . . C57 C 0.36543(14) 0.45023(11) 0.96829(15) 0.0370(6) Uani 1 1 d . . . H57A H 0.4150 0.4366 0.9750 0.044 Uiso 1 1 calc R . . H57B H 0.3606 0.4807 0.9313 0.044 Uiso 1 1 calc R . . C58 C 0.39548(14) 0.51747(11) 1.06691(17) 0.0430(7) Uani 1 1 d . . . H58A H 0.3899 0.5296 1.1195 0.064 Uiso 1 1 calc R . . H58B H 0.3780 0.5449 1.0272 0.064 Uiso 1 1 calc R . . H58C H 0.4462 0.5105 1.0681 0.064 Uiso 1 1 calc R . . C59 C 0.37725(17) 0.42949(12) 1.10811(17) 0.0545(8) Uani 1 1 d . . . H59A H 0.3501 0.3967 1.0942 0.082 Uiso 1 1 calc R . . H59B H 0.3686 0.4430 1.1588 0.082 Uiso 1 1 calc R . . H59C H 0.4285 0.4224 1.1132 0.082 Uiso 1 1 calc R . . N14 N 0.17328(10) 0.57966(7) 1.05585(10) 0.0221(4) Uani 1 1 d . . . C60 C 0.12582(13) 0.55026(9) 1.08798(13) 0.0257(5) Uani 1 1 d . . . H60A H 0.0765 0.5461 1.0644 0.031 Uiso 1 1 calc R . . C61 C 0.15920(15) 0.52768(10) 1.15886(13) 0.0327(6) Uani 1 1 d . . . H61A H 0.1380 0.5055 1.1921 0.039 Uiso 1 1 calc R . . C62 C 0.23067(15) 0.54398(10) 1.17219(13) 0.0350(6) Uani 1 1 d . . . H62A H 0.2676 0.5349 1.2164 0.042 Uiso 1 1 calc R . . C63 C 0.23730(13) 0.57592(9) 1.10861(13) 0.0274(5) Uani 1 1 d . . . H63A H 0.2803 0.5928 1.1026 0.033 Uiso 1 1 calc R . . N15 N 0.25866(10) 0.62072(8) 0.92508(10) 0.0253(4) Uani 1 1 d . . . C64 C 0.32012(13) 0.64707(10) 0.95781(14) 0.0304(6) Uani 1 1 d . . . H64A H 0.3241 0.6722 0.9996 0.037 Uiso 1 1 calc R . . C65 C 0.37544(13) 0.63264(10) 0.92269(14) 0.0308(6) Uani 1 1 d . . . H65A H 0.4233 0.6454 0.9355 0.037 Uiso 1 1 calc R . . C66 C 0.34733(13) 0.59541(11) 0.86418(14) 0.0335(6) Uani 1 1 d . . . H66A H 0.3721 0.5779 0.8291 0.040 Uiso 1 1 calc R . . C67 C 0.27653(13) 0.58930(10) 0.86774(13) 0.0296(6) Uani 1 1 d . . . H67A H 0.2442 0.5661 0.8345 0.036 Uiso 1 1 calc R . . N16 N 0.12607(10) 0.69320(8) 0.95773(10) 0.0221(4) Uani 1 1 d . . . C68 C 0.16619(13) 0.73830(9) 0.97347(12) 0.0251(5) Uani 1 1 d . . . H68A H 0.2170 0.7393 0.9840 0.030 Uiso 1 1 calc R . . C69 C 0.12286(14) 0.78192(10) 0.97196(14) 0.0318(6) Uani 1 1 d . . . H69A H 0.1379 0.8177 0.9806 0.038 Uiso 1 1 calc R . . C70 C 0.05198(14) 0.76333(10) 0.95516(14) 0.0330(6) Uani 1 1 d . . . H70A H 0.0097 0.7840 0.9502 0.040 Uiso 1 1 calc R . . C71 C 0.05600(13) 0.70937(10) 0.94735(13) 0.0273(6) Uani 1 1 d . . . H71A H 0.0158 0.6863 0.9363 0.033 Uiso 1 1 calc R . . N17 N 0.09905(10) 0.57802(8) 0.86749(11) 0.0257(4) Uani 1 1 d . . . C72 C 0.05834(13) 0.53474(10) 0.87484(14) 0.0313(6) Uani 1 1 d . . . H72A H 0.0516 0.5207 0.9241 0.038 Uiso 1 1 calc R . . C73 C 0.02830(14) 0.51402(11) 0.80112(15) 0.0389(7) Uani 1 1 d . . . H73A H -0.0025 0.4842 0.7905 0.047 Uiso 1 1 calc R . . C74 C 0.05225(14) 0.54576(12) 0.74502(15) 0.0415(7) Uani 1 1 d . . . H74A H 0.0411 0.5416 0.6888 0.050 Uiso 1 1 calc R . . C75 C 0.09495(14) 0.58397(11) 0.78755(14) 0.0369(7) Uani 1 1 d . . . H75A H 0.1186 0.6110 0.7645 0.044 Uiso 1 1 calc R . . Na4 Na 0.09497(5) 0.73259(4) 0.81113(5) 0.0261(2) Uani 1 1 d . A . N18 N 0.20114(11) 0.74510(8) 0.75207(12) 0.0339(5) Uani 1 1 d D . . N19 N 0.07164(12) 0.81485(9) 0.73381(13) 0.0372(5) Uani 1 1 d D . . N20 N -0.01588(11) 0.71424(9) 0.71034(12) 0.0367(5) Uani 1 1 d . . . C80 C 0.2249(6) 0.6995(5) 0.7132(8) 0.048(2) Uani 0.852(5) 1 d PD A 1 H80A H 0.2417 0.6719 0.7528 0.072 Uiso 0.852(5) 1 calc PR A 1 H80B H 0.2641 0.7099 0.6876 0.072 Uiso 0.852(5) 1 calc PR A 1 H80C H 0.1850 0.6857 0.6729 0.072 Uiso 0.852(5) 1 calc PR A 1 C81 C 0.2579(3) 0.7631(2) 0.8164(4) 0.0507(16) Uani 0.852(5) 1 d PD A 1 H81A H 0.2751 0.7334 0.8519 0.076 Uiso 0.852(5) 1 calc PR A 1 H81B H 0.2396 0.7910 0.8464 0.076 Uiso 0.852(5) 1 calc PR A 1 H81C H 0.2975 0.7771 0.7943 0.076 Uiso 0.852(5) 1 calc PR A 1 C82 C 0.1790(2) 0.78540(13) 0.6884(2) 0.0396(9) Uani 0.852(5) 1 d PD A 1 H82A H 0.1479 0.7682 0.6419 0.047 Uiso 0.852(5) 1 calc PR A 1 H82B H 0.2222 0.7987 0.6711 0.047 Uiso 0.852(5) 1 calc PR A 1 C83 C 0.13973(19) 0.83151(13) 0.7140(2) 0.0444(10) Uani 0.852(5) 1 d PD A 1 H83A H 0.1702 0.8484 0.7612 0.053 Uiso 0.852(5) 1 calc PR A 1 H83B H 0.1300 0.8580 0.6707 0.053 Uiso 0.852(5) 1 calc PR A 1 C81A C 0.2645(19) 0.7469(17) 0.819(2) 0.0507(16) Uani 0.15 1 d PD A 2 H81D H 0.3056 0.7613 0.8001 0.076 Uiso 0.148(5) 1 calc PR A 2 H81E H 0.2758 0.7110 0.8396 0.076 Uiso 0.148(5) 1 calc PR A 2 H81F H 0.2540 0.7694 0.8616 0.076 Uiso 0.148(5) 1 calc PR A 2 C80A C 0.213(4) 0.699(3) 0.703(5) 0.048(2) Uani 0.15 1 d PD A 2 H80D H 0.2620 0.7006 0.6937 0.072 Uiso 0.148(5) 1 calc PR A 2 H80E H 0.1789 0.7005 0.6519 0.072 Uiso 0.148(5) 1 calc PR A 2 H80F H 0.2065 0.6664 0.7310 0.072 Uiso 0.148(5) 1 calc PR A 2 C82A C 0.2037(12) 0.8040(8) 0.7294(12) 0.0396(9) Uani 0.15 1 d P A 2 H82C H 0.2401 0.8104 0.6970 0.047 Uiso 0.148(5) 1 calc PR A 2 H82D H 0.2141 0.8268 0.7773 0.047 Uiso 0.148(5) 1 calc PR A 2 C83A C 0.1248(10) 0.8137(9) 0.6790(12) 0.0444(10) Uani 0.15 1 d PD A 2 H83C H 0.1230 0.8478 0.6501 0.053 Uiso 0.148(5) 1 calc PR A 2 H83D H 0.1117 0.7851 0.6392 0.053 Uiso 0.148(5) 1 calc PR A 2 C84 C 0.05023(19) 0.85813(11) 0.78120(19) 0.0579(9) Uani 1 1 d . A . H84A H 0.0865 0.8626 0.8303 0.087 Uiso 1 1 calc R . . H84B H 0.0041 0.8496 0.7946 0.087 Uiso 1 1 calc R . . H84C H 0.0458 0.8910 0.7503 0.087 Uiso 1 1 calc R . . C85 C 0.01350(15) 0.80382(11) 0.66515(15) 0.0425(7) Uani 1 1 d . A . H85A H 0.0338 0.7874 0.6224 0.051 Uiso 1 1 calc R . . H85B H -0.0093 0.8376 0.6444 0.051 Uiso 1 1 calc R . . C86 C -0.04283(15) 0.76738(12) 0.68607(16) 0.0454(7) Uani 1 1 d . A . H86A H -0.0620 0.7835 0.7299 0.055 Uiso 1 1 calc R . . H86B H -0.0829 0.7642 0.6393 0.055 Uiso 1 1 calc R . . C87 C -0.00091(15) 0.68427(12) 0.64201(15) 0.0447(7) Uani 1 1 d . A . H87A H 0.0360 0.7027 0.6203 0.067 Uiso 1 1 calc R . . H87B H -0.0448 0.6815 0.6008 0.067 Uiso 1 1 calc R . . H87C H 0.0160 0.6487 0.6595 0.067 Uiso 1 1 calc R . . C88 C -0.06895(16) 0.68496(14) 0.74435(18) 0.0585(9) Uani 1 1 d . A . H88A H -0.0796 0.7047 0.7896 0.088 Uiso 1 1 calc R . . H88B H -0.0497 0.6501 0.7624 0.088 Uiso 1 1 calc R . . H88C H -0.1129 0.6806 0.7037 0.088 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.02461(14) 0.02352(15) 0.01841(13) -0.00137(11) 0.00415(11) 0.00435(13) Na1 0.0254(5) 0.0299(5) 0.0158(4) 0.0038(4) 0.0030(4) -0.0048(4) N1 0.0238(10) 0.0274(11) 0.0227(9) 0.0003(9) 0.0047(8) -0.0016(9) N2 0.0272(11) 0.0243(11) 0.0220(9) 0.0017(9) 0.0066(8) -0.0004(9) N3 0.0268(11) 0.0231(11) 0.0243(10) 0.0020(9) 0.0096(8) -0.0005(9) C1 0.0382(15) 0.0359(15) 0.0263(12) -0.0030(12) 0.0039(11) 0.0025(13) C2 0.0346(15) 0.0361(16) 0.0346(14) 0.0005(12) 0.0049(12) -0.0122(13) C3 0.0236(13) 0.0375(15) 0.0253(12) -0.0026(11) 0.0003(10) -0.0019(12) C4 0.0311(13) 0.0337(15) 0.0206(11) 0.0032(11) 0.0019(10) 0.0091(12) C5 0.0411(15) 0.0308(15) 0.0321(13) -0.0014(12) 0.0080(12) 0.0094(13) C6 0.0371(15) 0.0255(14) 0.0347(13) 0.0090(11) 0.0087(12) 0.0008(12) C7 0.0346(14) 0.0315(14) 0.0267(12) 0.0072(11) 0.0127(11) -0.0032(12) C8 0.0408(16) 0.0351(16) 0.0384(14) 0.0000(13) 0.0152(13) 0.0042(13) C9 0.0380(15) 0.0434(17) 0.0335(14) -0.0043(13) 0.0096(12) -0.0104(14) N4 0.0238(10) 0.0222(11) 0.0167(9) 0.0020(8) 0.0046(8) 0.0017(9) C10 0.0272(13) 0.0271(13) 0.0195(11) 0.0046(10) 0.0077(10) -0.0037(11) C11 0.0249(13) 0.0342(15) 0.0263(12) 0.0050(11) 0.0108(10) 0.0086(12) C12 0.0371(14) 0.0214(13) 0.0226(11) 0.0021(10) 0.0075(10) 0.0068(12) C13 0.0252(12) 0.0263(13) 0.0164(10) 0.0006(10) 0.0032(9) -0.0014(11) N5 0.0235(11) 0.0329(12) 0.0333(11) -0.0044(10) 0.0055(9) 0.0028(10) C14 0.0266(14) 0.0380(16) 0.0519(17) -0.0128(14) 0.0021(12) 0.0019(13) C15 0.0261(15) 0.0377(17) 0.067(2) 0.0004(16) 0.0019(14) -0.0013(13) C16 0.0296(15) 0.061(2) 0.0505(17) 0.0151(16) 0.0159(13) 0.0051(15) C17 0.0346(15) 0.0403(17) 0.0303(13) -0.0002(12) 0.0089(11) 0.0068(13) N6 0.0300(11) 0.0276(11) 0.0232(10) -0.0033(9) 0.0077(9) -0.0016(10) C18 0.0301(13) 0.0342(15) 0.0202(11) -0.0003(11) 0.0052(10) 0.0014(12) C19 0.0416(16) 0.0368(16) 0.0249(12) -0.0067(12) 0.0015(12) 0.0054(13) C20 0.0370(15) 0.0324(15) 0.0429(15) -0.0057(13) -0.0008(12) -0.0068(13) C21 0.0405(16) 0.0348(16) 0.0314(13) 0.0013(12) 0.0112(12) -0.0033(13) N7 0.0374(12) 0.0265(11) 0.0175(9) -0.0034(9) 0.0034(9) 0.0136(10) C22 0.0536(17) 0.0306(15) 0.0229(12) 0.0003(11) 0.0141(12) 0.0154(14) C23 0.088(3) 0.0369(17) 0.0268(14) 0.0059(13) 0.0177(16) 0.0240(18) C24 0.088(3) 0.0411(18) 0.0182(13) -0.0039(12) -0.0077(15) 0.0337(18) C25 0.0502(17) 0.0346(16) 0.0300(13) -0.0134(12) -0.0037(12) 0.0188(14) Na2 0.0336(5) 0.0228(5) 0.0426(5) -0.0083(5) 0.0159(5) 0.0011(5) N8 0.0274(11) 0.0302(12) 0.0335(11) -0.0043(10) 0.0002(9) -0.0024(10) N9 0.0256(11) 0.0251(11) 0.0240(10) -0.0053(9) 0.0064(8) -0.0011(9) N10 0.0317(12) 0.0306(12) 0.0303(11) -0.0003(10) 0.0121(9) -0.0045(10) C30 0.056(2) 0.051(2) 0.0418(16) 0.0041(15) -0.0107(14) -0.0047(17) C31 0.0325(15) 0.0376(17) 0.0583(18) -0.0057(15) -0.0057(13) -0.0053(14) C32 0.0236(13) 0.0376(16) 0.0441(15) 0.0002(13) 0.0080(11) 0.0012(12) C33 0.0312(14) 0.0274(14) 0.0352(13) -0.0052(11) 0.0113(11) 0.0058(12) C34 0.0485(17) 0.0519(19) 0.0286(13) 0.0039(13) -0.0005(13) -0.0002(15) C35 0.0388(15) 0.0314(15) 0.0383(14) -0.0152(12) 0.0134(12) -0.0068(13) C36 0.0526(19) 0.0283(15) 0.0537(17) -0.0052(14) 0.0192(15) -0.0075(14) C37 0.076(2) 0.054(2) 0.0426(17) 0.0127(16) 0.0132(16) 0.0031(19) C38 0.0408(18) 0.050(2) 0.065(2) 0.0133(17) 0.0120(15) -0.0093(16) Zn2 0.02476(14) 0.01879(14) 0.01953(13) -0.00003(11) 0.00119(11) -0.00206(12) Na3 0.0333(5) 0.0214(5) 0.0340(5) -0.0078(4) 0.0108(4) -0.0006(4) N11 0.0358(12) 0.0247(11) 0.0255(10) -0.0002(9) 0.0097(9) -0.0024(10) N12 0.0429(13) 0.0232(11) 0.0248(10) -0.0026(9) 0.0135(9) -0.0044(10) N13 0.0363(12) 0.0235(11) 0.0275(10) 0.0014(9) 0.0080(9) 0.0024(10) C51 0.0373(16) 0.0370(17) 0.0480(16) 0.0021(14) 0.0099(13) -0.0087(14) C52 0.069(2) 0.0444(18) 0.0343(15) 0.0084(14) 0.0103(15) -0.0027(17) C53 0.0576(18) 0.0199(13) 0.0476(16) -0.0043(13) 0.0228(14) -0.0078(14) C54 0.0587(18) 0.0262(14) 0.0389(14) -0.0144(12) 0.0229(14) -0.0115(14) C55 0.0609(19) 0.0403(17) 0.0288(13) -0.0025(13) 0.0127(13) -0.0071(15) C56 0.0510(18) 0.0317(15) 0.0393(15) -0.0056(13) 0.0228(13) 0.0083(14) C57 0.0392(16) 0.0355(16) 0.0400(15) -0.0011(13) 0.0169(13) 0.0051(13) C58 0.0343(15) 0.0393(17) 0.0539(17) -0.0060(15) 0.0055(13) -0.0012(14) C59 0.072(2) 0.0463(19) 0.0444(17) 0.0127(15) 0.0113(16) 0.0097(18) N14 0.0278(11) 0.0182(10) 0.0194(9) -0.0009(8) 0.0030(8) 0.0015(9) C60 0.0341(14) 0.0204(13) 0.0240(11) -0.0047(10) 0.0093(10) -0.0007(11) C61 0.0552(18) 0.0216(13) 0.0247(12) 0.0031(11) 0.0159(12) 0.0036(13) C62 0.0534(18) 0.0309(15) 0.0168(11) 0.0001(11) -0.0017(11) 0.0126(14) C63 0.0327(14) 0.0224(13) 0.0247(12) -0.0054(10) 0.0006(10) 0.0008(11) N15 0.0286(11) 0.0235(11) 0.0229(9) -0.0032(9) 0.0035(8) -0.0026(9) C64 0.0296(13) 0.0265(14) 0.0328(13) -0.0068(11) 0.0010(11) -0.0058(12) C65 0.0255(13) 0.0319(15) 0.0348(13) 0.0031(12) 0.0059(11) -0.0048(12) C66 0.0357(15) 0.0363(16) 0.0314(13) 0.0013(12) 0.0137(12) 0.0020(13) C67 0.0322(14) 0.0289(14) 0.0266(12) -0.0069(11) 0.0034(11) -0.0054(12) N16 0.0285(11) 0.0204(10) 0.0174(9) 0.0034(8) 0.0046(8) -0.0004(9) C68 0.0290(13) 0.0239(13) 0.0216(11) -0.0017(10) 0.0036(10) -0.0032(11) C69 0.0458(16) 0.0194(13) 0.0314(13) -0.0013(11) 0.0108(12) 0.0002(12) C70 0.0387(15) 0.0320(15) 0.0329(13) 0.0064(12) 0.0179(12) 0.0126(13) C71 0.0256(13) 0.0332(15) 0.0252(12) 0.0074(11) 0.0099(10) -0.0033(12) N17 0.0262(11) 0.0258(11) 0.0231(10) -0.0016(9) 0.0006(8) -0.0047(9) C72 0.0321(14) 0.0333(15) 0.0306(13) -0.0040(12) 0.0118(11) -0.0105(12) C73 0.0376(15) 0.0366(16) 0.0414(15) -0.0138(13) 0.0057(12) -0.0150(13) C74 0.0435(17) 0.0500(19) 0.0267(13) -0.0059(13) -0.0029(12) -0.0082(15) C75 0.0393(15) 0.0415(17) 0.0254(13) 0.0056(12) -0.0036(11) -0.0139(13) Na4 0.0297(5) 0.0284(5) 0.0207(4) 0.0058(4) 0.0064(4) -0.0013(4) N18 0.0426(13) 0.0238(12) 0.0422(12) 0.0102(10) 0.0244(11) 0.0064(11) N19 0.0379(13) 0.0269(12) 0.0476(13) 0.0139(11) 0.0111(11) 0.0054(11) N20 0.0363(13) 0.0427(14) 0.0287(11) 0.0054(10) 0.0008(10) -0.0081(11) C80 0.042(5) 0.0446(19) 0.064(4) -0.011(2) 0.027(4) -0.006(2) C81 0.052(2) 0.058(4) 0.0491(19) -0.010(3) 0.0269(17) -0.018(3) C82 0.054(2) 0.033(2) 0.040(2) 0.0039(15) 0.0286(18) -0.0028(17) C83 0.051(2) 0.023(2) 0.061(3) 0.0165(17) 0.0143(19) -0.0045(16) C81A 0.052(2) 0.058(4) 0.0491(19) -0.010(3) 0.0269(17) -0.018(3) C80A 0.042(5) 0.0446(19) 0.064(4) -0.011(2) 0.027(4) -0.006(2) C82A 0.054(2) 0.033(2) 0.040(2) 0.0039(15) 0.0286(18) -0.0028(17) C83A 0.051(2) 0.023(2) 0.061(3) 0.0165(17) 0.0143(19) -0.0045(16) C84 0.080(2) 0.0269(16) 0.062(2) 0.0020(15) 0.0036(18) 0.0037(17) C85 0.0572(19) 0.0366(16) 0.0335(14) 0.0156(13) 0.0094(13) 0.0196(15) C86 0.0358(16) 0.056(2) 0.0393(15) -0.0003(15) -0.0044(13) 0.0071(15) C87 0.0549(18) 0.0441(18) 0.0297(14) -0.0004(13) -0.0032(13) -0.0068(15) C88 0.0438(18) 0.076(3) 0.0543(19) 0.0003(18) 0.0072(15) -0.0273(18) _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 N5 1.9792(19) . ? Zn1 N4 1.9978(19) . ? Zn1 N6 1.9995(19) . ? Zn1 N7 2.0062(18) . ? Na1 N1 2.448(2) . ? Na1 N3 2.4722(19) . ? Na1 N2 2.473(2) . ? Na1 N4 2.5884(18) . ? Na1 C10 2.737(2) . ? Na1 C13 2.746(2) . ? Na1 C11 2.993(2) . ? Na1 C12 3.002(2) . ? Na1 C3 3.110(2) . ? N1 C3 1.466(3) . ? N1 C2 1.469(3) . ? N1 C1 1.474(3) . ? N2 C5 1.470(3) . ? N2 C4 1.472(3) . ? N2 C6 1.474(3) . ? N3 C8 1.462(3) . ? N3 C9 1.464(3) . ? N3 C7 1.479(3) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 C4 1.519(3) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 C7 1.507(3) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? N4 C10 1.370(3) . ? N4 C13 1.375(3) . ? C10 C11 1.374(3) . ? C10 H10A 0.9500 . ? C11 C12 1.408(3) . ? C11 H11A 0.9500 . ? C12 C13 1.378(3) . ? C12 H12A 0.9500 . ? C13 H13A 0.9500 . ? N5 C17 1.359(3) . ? N5 C14 1.366(3) . ? C14 C15 1.363(4) . ? C14 H14A 0.9500 . ? C15 C16 1.401(4) . ? C15 H15A 0.9500 . ? C16 C17 1.376(4) . ? C16 H16A 0.9500 . ? C17 H17A 0.9500 . ? N6 C18 1.365(3) . ? N6 C21 1.366(3) . ? C18 C19 1.374(3) . ? C18 H18A 0.9500 . ? C19 C20 1.394(3) . ? C19 H19A 0.9500 . ? C20 C21 1.379(3) . ? C20 H20A 0.9500 . ? C21 H21A 0.9500 . ? N7 C25 1.366(3) . ? N7 C22 1.375(3) . ? N7 Na2 2.551(2) . ? C22 C23 1.373(3) . ? C22 Na2 2.821(2) . ? C22 H22A 0.9500 . ? C23 C24 1.385(4) . ? C23 Na2 3.100(3) . ? C23 H23A 0.9500 . ? C24 C25 1.384(4) . ? C24 Na2 3.008(3) . ? C24 H24A 0.9500 . ? C25 Na2 2.680(3) . ? C25 H25A 0.9500 . ? Na2 N9 2.461(2) . ? Na2 N10 2.506(2) . ? Na2 N8 2.530(2) . ? N8 C30 1.461(3) . ? N8 C32 1.461(3) . ? N8 C31 1.479(3) . ? N9 C33 1.467(3) . ? N9 C35 1.467(3) . ? N9 C34 1.475(3) . ? N10 C38 1.444(3) . ? N10 C37 1.461(3) . ? N10 C36 1.488(3) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 C33 1.515(3) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 C36 1.498(3) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? Zn2 N17 1.9837(19) . ? Zn2 N15 1.9906(19) . ? Zn2 N16 2.0043(19) . ? Zn2 N14 2.0073(17) . ? Na3 N11 2.505(2) . ? Na3 N13 2.514(2) . ? Na3 N12 2.522(2) . ? Na3 N14 2.659(2) . ? Na3 C63 2.704(2) . ? Na3 C60 2.853(2) . ? Na3 C62 2.935(2) . ? Na3 C61 3.029(2) . ? N11 C53 1.464(3) . ? N11 C51 1.464(3) . ? N11 C52 1.467(3) . ? N12 C56 1.471(3) . ? N12 C55 1.473(3) . ? N12 C54 1.476(3) . ? N13 C59 1.458(3) . ? N13 C58 1.464(3) . ? N13 C57 1.470(3) . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C53 C54 1.505(3) . ? C53 H53A 0.9900 . ? C53 H53B 0.9900 . ? C54 H54A 0.9900 . ? C54 H54B 0.9900 . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? C56 C57 1.506(4) . ? C56 H56A 0.9900 . ? C56 H56B 0.9900 . ? C57 H57A 0.9900 . ? C57 H57B 0.9900 . ? C58 H58A 0.9800 . ? C58 H58B 0.9800 . ? C58 H58C 0.9800 . ? C59 H59A 0.9800 . ? C59 H59B 0.9800 . ? C59 H59C 0.9800 . ? N14 C63 1.365(3) . ? N14 C60 1.373(3) . ? C60 C61 1.374(3) . ? C60 H60A 0.9500 . ? C61 C62 1.398(4) . ? C61 H61A 0.9500 . ? C62 C63 1.384(3) . ? C62 H62A 0.9500 . ? C63 H63A 0.9500 . ? N15 C67 1.362(3) . ? N15 C64 1.364(3) . ? C64 C65 1.370(3) . ? C64 H64A 0.9500 . ? C65 C66 1.399(3) . ? C65 H65A 0.9500 . ? C66 C67 1.375(3) . ? C66 H66A 0.9500 . ? C67 H67A 0.9500 . ? N16 C68 1.368(3) . ? N16 C71 1.375(3) . ? N16 Na4 2.6562(19) . ? C68 C69 1.375(3) . ? C68 Na4 2.839(2) . ? C68 H68A 0.9500 . ? C69 C70 1.405(4) . ? C69 Na4 2.975(2) . ? C69 H69A 0.9500 . ? C70 C71 1.373(3) . ? C70 Na4 2.870(2) . ? C70 H70A 0.9500 . ? C71 Na4 2.663(2) . ? C71 H71A 0.9500 . ? N17 C72 1.362(3) . ? N17 C75 1.367(3) . ? C72 C73 1.379(3) . ? C72 H72A 0.9500 . ? C73 C74 1.401(4) . ? C73 H73A 0.9500 . ? C74 C75 1.371(4) . ? C74 H74A 0.9500 . ? C75 H75A 0.9500 . ? Na4 N19 2.456(2) . ? Na4 N18 2.469(2) . ? Na4 N20 2.482(2) . ? N18 C81 1.450(4) . ? N18 C80 1.452(4) . ? N18 C80A 1.476(10) . ? N18 C81A 1.486(10) . ? N18 C82 1.490(4) . ? N18 C82A 1.54(2) . ? N19 C85 1.468(3) . ? N19 C84 1.471(3) . ? N19 C83 1.472(4) . ? N19 C83A 1.522(10) . ? N20 C86 1.466(4) . ? N20 C88 1.470(3) . ? N20 C87 1.473(3) . ? C80 H80A 0.9800 . ? C80 H80B 0.9800 . ? C80 H80C 0.9800 . ? C81 H81A 0.9800 . ? C81 H81B 0.9800 . ? C81 H81C 0.9800 . ? C82 C83 1.500(4) . ? C82 H82A 0.9900 . ? C82 H82B 0.9900 . ? C83 H83A 0.9900 . ? C83 H83B 0.9900 . ? C81A H81D 0.9800 . ? C81A H81E 0.9800 . ? C81A H81F 0.9800 . ? C80A H80D 0.9800 . ? C80A H80E 0.9800 . ? C80A H80F 0.9800 . ? C82A C83A 1.59(3) . ? C82A H82C 0.9900 . ? C82A H82D 0.9900 . ? C83A H83C 0.9900 . ? C83A H83D 0.9900 . ? C84 H84A 0.9800 . ? C84 H84B 0.9800 . ? C84 H84C 0.9800 . ? C85 C86 1.515(4) . ? C85 H85A 0.9900 . ? C85 H85B 0.9900 . ? C86 H86A 0.9900 . ? C86 H86B 0.9900 . ? C87 H87A 0.9800 . ? C87 H87B 0.9800 . ? C87 H87C 0.9800 . ? C88 H88A 0.9800 . ? C88 H88B 0.9800 . ? C88 H88C 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 N5 Zn1 N4 108.44(8) . . ? N5 Zn1 N6 113.06(8) . . ? N4 Zn1 N6 108.38(8) . . ? N5 Zn1 N7 108.60(8) . . ? N4 Zn1 N7 110.87(7) . . ? N6 Zn1 N7 107.50(8) . . ? N5 Zn1 Na2 93.02(6) . . ? N4 Zn1 Na2 153.03(5) . . ? N6 Zn1 Na2 76.28(6) . . ? N7 Zn1 Na2 44.71(5) . . ? N1 Na1 N3 108.60(7) . . ? N1 Na1 N2 76.41(7) . . ? N3 Na1 N2 75.27(6) . . ? N1 Na1 N4 122.73(7) . . ? N3 Na1 N4 120.75(7) . . ? N2 Na1 N4 140.37(7) . . ? N1 Na1 C10 99.69(7) . . ? N3 Na1 C10 149.79(7) . . ? N2 Na1 C10 122.85(7) . . ? N4 Na1 C10 29.64(6) . . ? N1 Na1 C13 146.39(7) . . ? N3 Na1 C13 104.90(7) . . ? N2 Na1 C13 115.48(7) . . ? N4 Na1 C13 29.68(6) . . ? C10 Na1 C13 46.91(7) . . ? N1 Na1 C11 104.09(7) . . ? N3 Na1 C11 143.35(8) . . ? N2 Na1 C11 97.18(7) . . ? N4 Na1 C11 47.13(6) . . ? C10 Na1 C11 27.28(7) . . ? C13 Na1 C11 45.45(7) . . ? N1 Na1 C12 129.47(7) . . ? N3 Na1 C12 116.37(7) . . ? N2 Na1 C12 93.39(7) . . ? N4 Na1 C12 47.13(6) . . ? C10 Na1 C12 45.41(7) . . ? C13 Na1 C12 27.28(6) . . ? C11 Na1 C12 27.16(6) . . ? N1 Na1 C3 27.41(6) . . ? N3 Na1 C3 106.48(7) . . ? N2 Na1 C3 51.22(7) . . ? N4 Na1 C3 132.75(7) . . ? C10 Na1 C3 103.50(7) . . ? C13 Na1 C3 139.54(7) . . ? C11 Na1 C3 94.97(7) . . ? C12 Na1 C3 113.45(7) . . ? C3 N1 C2 109.68(18) . . ? C3 N1 C1 110.86(18) . . ? C2 N1 C1 108.97(19) . . ? C3 N1 Na1 102.35(14) . . ? C2 N1 Na1 110.23(13) . . ? C1 N1 Na1 114.57(14) . . ? C5 N2 C4 109.88(19) . . ? C5 N2 C6 109.55(19) . . ? C4 N2 C6 111.49(17) . . ? C5 N2 Na1 114.10(13) . . ? C4 N2 Na1 105.27(14) . . ? C6 N2 Na1 106.48(14) . . ? C8 N3 C9 108.6(2) . . ? C8 N3 C7 108.44(17) . . ? C9 N3 C7 111.3(2) . . ? C8 N3 Na1 117.43(15) . . ? C9 N3 Na1 104.68(13) . . ? C7 N3 Na1 106.34(13) . . ? N1 C1 H1A 109.5 . . ? N1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? N1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N1 C2 H2A 109.5 . . ? N1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? N1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? N1 C3 C4 113.43(19) . . ? N1 C3 Na1 50.24(10) . . ? C4 C3 Na1 79.13(13) . . ? N1 C3 H3A 108.9 . . ? C4 C3 H3A 108.9 . . ? Na1 C3 H3A 158.2 . . ? N1 C3 H3B 108.9 . . ? C4 C3 H3B 108.9 . . ? Na1 C3 H3B 87.8 . . ? H3A C3 H3B 107.7 . . ? N2 C4 C3 112.07(18) . . ? N2 C4 H4A 109.2 . . ? C3 C4 H4A 109.2 . . ? N2 C4 H4B 109.2 . . ? C3 C4 H4B 109.2 . . ? H4A C4 H4B 107.9 . . ? N2 C5 H5A 109.5 . . ? N2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? N2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N2 C6 C7 113.9(2) . . ? N2 C6 H6A 108.8 . . ? C7 C6 H6A 108.8 . . ? N2 C6 H6B 108.8 . . ? C7 C6 H6B 108.8 . . ? H6A C6 H6B 107.7 . . ? N3 C7 C6 113.89(18) . . ? N3 C7 H7A 108.8 . . ? C6 C7 H7A 108.8 . . ? N3 C7 H7B 108.8 . . ? C6 C7 H7B 108.8 . . ? H7A C7 H7B 107.7 . . ? N3 C8 H8A 109.5 . . ? N3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? N3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N3 C9 H9A 109.5 . . ? N3 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? N3 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C10 N4 C13 105.36(19) . . ? C10 N4 Zn1 124.99(16) . . ? C13 N4 Zn1 129.57(15) . . ? C10 N4 Na1 81.20(12) . . ? C13 N4 Na1 81.51(12) . . ? Zn1 N4 Na1 106.90(7) . . ? N4 C10 C11 111.1(2) . . ? N4 C10 Na1 69.16(11) . . ? C11 C10 Na1 86.81(14) . . ? N4 C10 H10A 124.5 . . ? C11 C10 H10A 124.5 . . ? Na1 C10 H10A 111.3 . . ? C10 C11 C12 106.4(2) . . ? C10 C11 Na1 65.91(12) . . ? C12 C11 Na1 76.74(12) . . ? C10 C11 H11A 126.8 . . ? C12 C11 H11A 126.8 . . ? Na1 C11 H11A 122.2 . . ? C13 C12 C11 106.3(2) . . ? C13 C12 Na1 65.97(12) . . ? C11 C12 Na1 76.10(13) . . ? C13 C12 H12A 126.9 . . ? C11 C12 H12A 126.9 . . ? Na1 C12 H12A 122.7 . . ? N4 C13 C12 110.8(2) . . ? N4 C13 Na1 68.81(11) . . ? C12 C13 Na1 86.75(14) . . ? N4 C13 H13A 124.6 . . ? C12 C13 H13A 124.6 . . ? Na1 C13 H13A 111.6 . . ? C17 N5 C14 105.9(2) . . ? C17 N5 Zn1 127.54(18) . . ? C14 N5 Zn1 126.45(17) . . ? C15 C14 N5 111.1(2) . . ? C15 C14 H14A 124.4 . . ? N5 C14 H14A 124.4 . . ? C14 C15 C16 106.0(3) . . ? C14 C15 H15A 127.0 . . ? C16 C15 H15A 127.0 . . ? C17 C16 C15 106.8(2) . . ? C17 C16 H16A 126.6 . . ? C15 C16 H16A 126.6 . . ? N5 C17 C16 110.2(2) . . ? N5 C17 H17A 124.9 . . ? C16 C17 H17A 124.9 . . ? C18 N6 C21 105.4(2) . . ? C18 N6 Zn1 127.29(17) . . ? C21 N6 Zn1 127.34(15) . . ? N6 C18 C19 110.9(2) . . ? N6 C18 H18A 124.5 . . ? C19 C18 H18A 124.5 . . ? C18 C19 C20 106.6(2) . . ? C18 C19 H19A 126.7 . . ? C20 C19 H19A 126.7 . . ? C21 C20 C19 106.3(2) . . ? C21 C20 H20A 126.9 . . ? C19 C20 H20A 126.9 . . ? N6 C21 C20 110.9(2) . . ? N6 C21 H21A 124.6 . . ? C20 C21 H21A 124.6 . . ? C25 N7 C22 105.6(2) . . ? C25 N7 Zn1 124.61(18) . . ? C22 N7 Zn1 129.76(17) . . ? C25 N7 Na2 80.13(14) . . ? C22 N7 Na2 86.41(14) . . ? Zn1 N7 Na2 101.70(7) . . ? C23 C22 N7 111.0(3) . . ? C23 C22 Na2 88.27(17) . . ? N7 C22 Na2 64.49(12) . . ? C23 C22 H22A 124.5 . . ? N7 C22 H22A 124.5 . . ? Na2 C22 H22A 114.0 . . ? C22 C23 C24 105.9(3) . . ? C22 C23 Na2 65.45(14) . . ? C24 C23 Na2 73.20(16) . . ? C22 C23 H23A 127.0 . . ? C24 C23 H23A 127.0 . . ? Na2 C23 H23A 125.8 . . ? C25 C24 C23 107.7(3) . . ? C25 C24 Na2 62.98(14) . . ? C23 C24 Na2 80.64(16) . . ? C25 C24 H24A 126.1 . . ? C23 C24 H24A 126.1 . . ? Na2 C24 H24A 121.5 . . ? N7 C25 C24 109.7(3) . . ? N7 C25 Na2 69.72(13) . . ? C24 C25 Na2 89.63(17) . . ? N7 C25 H25A 125.2 . . ? C24 C25 H25A 125.2 . . ? Na2 C25 H25A 107.8 . . ? N9 Na2 N10 74.44(7) . . ? N9 Na2 N8 73.43(7) . . ? N10 Na2 N8 118.46(8) . . ? N9 Na2 N7 146.11(7) . . ? N10 Na2 N7 122.11(7) . . ? N8 Na2 N7 113.76(8) . . ? N9 Na2 C25 155.22(9) . . ? N10 Na2 C25 130.13(9) . . ? N8 Na2 C25 88.98(8) . . ? N7 Na2 C25 30.15(7) . . ? N9 Na2 C22 149.74(8) . . ? N10 Na2 C22 93.31(8) . . ? N8 Na2 C22 135.32(8) . . ? N7 Na2 C22 29.10(7) . . ? C25 Na2 C22 46.69(9) . . ? N9 Na2 C24 165.23(8) . . ? N10 Na2 C24 104.69(8) . . ? N8 Na2 C24 94.79(9) . . ? N7 Na2 C24 46.81(7) . . ? C25 Na2 C24 27.39(8) . . ? C22 Na2 C24 44.24(8) . . ? N9 Na2 C23 159.98(9) . . ? N10 Na2 C23 85.75(8) . . ? N8 Na2 C23 120.09(9) . . ? N7 Na2 C23 46.00(7) . . ? C25 Na2 C23 44.79(9) . . ? C22 Na2 C23 26.27(7) . . ? C24 Na2 C23 26.16(8) . . ? N9 Na2 Zn1 112.77(6) . . ? N10 Na2 Zn1 132.99(6) . . ? N8 Na2 Zn1 107.65(6) . . ? N7 Na2 Zn1 33.59(4) . . ? C25 Na2 Zn1 55.48(6) . . ? C22 Na2 Zn1 56.27(5) . . ? C24 Na2 Zn1 78.93(6) . . ? C23 Na2 Zn1 78.69(6) . . ? C30 N8 C32 111.2(2) . . ? C30 N8 C31 109.4(2) . . ? C32 N8 C31 108.9(2) . . ? C30 N8 Na2 102.91(16) . . ? C32 N8 Na2 106.56(14) . . ? C31 N8 Na2 117.75(16) . . ? C33 N9 C35 111.0(2) . . ? C33 N9 C34 109.75(19) . . ? C35 N9 C34 109.6(2) . . ? C33 N9 Na2 108.83(13) . . ? C35 N9 Na2 108.41(13) . . ? C34 N9 Na2 109.15(16) . . ? C38 N10 C37 109.2(2) . . ? C38 N10 C36 110.8(2) . . ? C37 N10 C36 106.9(2) . . ? C38 N10 Na2 112.07(17) . . ? C37 N10 Na2 113.59(17) . . ? C36 N10 Na2 104.14(14) . . ? N8 C30 H30A 109.5 . . ? N8 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? N8 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? N8 C31 H31A 109.5 . . ? N8 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? N8 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? N8 C32 C33 113.7(2) . . ? N8 C32 H32A 108.8 . . ? C33 C32 H32A 108.8 . . ? N8 C32 H32B 108.8 . . ? C33 C32 H32B 108.8 . . ? H32A C32 H32B 107.7 . . ? N9 C33 C32 112.3(2) . . ? N9 C33 H33A 109.1 . . ? C32 C33 H33A 109.1 . . ? N9 C33 H33B 109.1 . . ? C32 C33 H33B 109.1 . . ? H33A C33 H33B 107.9 . . ? N9 C34 H34A 109.5 . . ? N9 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? N9 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? N9 C35 C36 113.1(2) . . ? N9 C35 H35A 109.0 . . ? C36 C35 H35A 109.0 . . ? N9 C35 H35B 109.0 . . ? C36 C35 H35B 109.0 . . ? H35A C35 H35B 107.8 . . ? N10 C36 C35 113.1(2) . . ? N10 C36 H36A 109.0 . . ? C35 C36 H36A 109.0 . . ? N10 C36 H36B 109.0 . . ? C35 C36 H36B 109.0 . . ? H36A C36 H36B 107.8 . . ? N10 C37 H37A 109.5 . . ? N10 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? N10 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? N10 C38 H38A 109.5 . . ? N10 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? N10 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? N17 Zn2 N15 106.75(8) . . ? N17 Zn2 N16 110.95(8) . . ? N15 Zn2 N16 109.67(8) . . ? N17 Zn2 N14 109.01(8) . . ? N15 Zn2 N14 106.80(8) . . ? N16 Zn2 N14 113.38(7) . . ? N17 Zn2 Na3 81.96(6) . . ? N15 Zn2 Na3 82.03(6) . . ? N16 Zn2 Na3 157.92(5) . . ? N14 Zn2 Na3 44.54(5) . . ? N11 Na3 N13 111.74(7) . . ? N11 Na3 N12 73.49(7) . . ? N13 Na3 N12 74.31(7) . . ? N11 Na3 N14 121.78(7) . . ? N13 Na3 N14 119.85(7) . . ? N12 Na3 N14 143.68(7) . . ? N11 Na3 C63 131.82(7) . . ? N13 Na3 C63 93.50(7) . . ? N12 Na3 C63 154.66(8) . . ? N14 Na3 C63 29.47(6) . . ? N11 Na3 C60 93.73(7) . . ? N13 Na3 C60 137.78(7) . . ? N12 Na3 C60 147.32(8) . . ? N14 Na3 C60 28.57(6) . . ? C63 Na3 C60 46.15(7) . . ? N11 Na3 C62 106.81(7) . . ? N13 Na3 C62 94.15(7) . . ? N12 Na3 C62 167.26(8) . . ? N14 Na3 C62 47.26(6) . . ? C63 Na3 C62 28.04(7) . . ? C60 Na3 C62 45.03(7) . . ? N11 Na3 C61 86.50(7) . . ? N13 Na3 C61 118.85(7) . . ? N12 Na3 C61 159.43(8) . . ? N14 Na3 C61 46.33(6) . . ? C63 Na3 C61 45.42(7) . . ? C60 Na3 C61 26.81(6) . . ? C62 Na3 C61 27.05(7) . . ? N11 Na3 Zn2 131.98(6) . . ? N13 Na3 Zn2 115.66(5) . . ? N12 Na3 Zn2 112.23(5) . . ? N14 Na3 Zn2 31.98(4) . . ? C63 Na3 Zn2 52.70(5) . . ? C60 Na3 Zn2 54.78(5) . . ? C62 Na3 Zn2 77.38(5) . . ? C61 Na3 Zn2 77.62(5) . . ? C53 N11 C51 111.0(2) . . ? C53 N11 C52 108.3(2) . . ? C51 N11 C52 108.5(2) . . ? C53 N11 Na3 106.70(14) . . ? C51 N11 Na3 109.07(15) . . ? C52 N11 Na3 113.33(16) . . ? C56 N12 C55 110.12(19) . . ? C56 N12 C54 111.4(2) . . ? C55 N12 C54 107.9(2) . . ? C56 N12 Na3 106.30(14) . . ? C55 N12 Na3 113.75(15) . . ? C54 N12 Na3 107.42(13) . . ? C59 N13 C58 109.0(2) . . ? C59 N13 C57 111.6(2) . . ? C58 N13 C57 108.6(2) . . ? C59 N13 Na3 111.59(17) . . ? C58 N13 Na3 111.88(15) . . ? C57 N13 Na3 104.08(15) . . ? N11 C51 H51A 109.5 . . ? N11 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? N11 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? N11 C52 H52A 109.5 . . ? N11 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? N11 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? N11 C53 C54 113.7(2) . . ? N11 C53 H53A 108.8 . . ? C54 C53 H53A 108.8 . . ? N11 C53 H53B 108.8 . . ? C54 C53 H53B 108.8 . . ? H53A C53 H53B 107.7 . . ? N12 C54 C53 113.5(2) . . ? N12 C54 H54A 108.9 . . ? C53 C54 H54A 108.9 . . ? N12 C54 H54B 108.9 . . ? C53 C54 H54B 108.9 . . ? H54A C54 H54B 107.7 . . ? N12 C55 H55A 109.5 . . ? N12 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? N12 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? N12 C56 C57 113.0(2) . . ? N12 C56 H56A 109.0 . . ? C57 C56 H56A 109.0 . . ? N12 C56 H56B 109.0 . . ? C57 C56 H56B 109.0 . . ? H56A C56 H56B 107.8 . . ? N13 C57 C56 113.9(2) . . ? N13 C57 H57A 108.8 . . ? C56 C57 H57A 108.8 . . ? N13 C57 H57B 108.8 . . ? C56 C57 H57B 108.8 . . ? H57A C57 H57B 107.7 . . ? N13 C58 H58A 109.5 . . ? N13 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? N13 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? N13 C59 H59A 109.5 . . ? N13 C59 H59B 109.5 . . ? H59A C59 H59B 109.5 . . ? N13 C59 H59C 109.5 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? C63 N14 C60 105.71(19) . . ? C63 N14 Zn2 122.30(15) . . ? C60 N14 Zn2 131.93(16) . . ? C63 N14 Na3 77.09(13) . . ? C60 N14 Na3 83.58(13) . . ? Zn2 N14 Na3 103.48(7) . . ? N14 C60 C61 110.9(2) . . ? N14 C60 Na3 67.85(12) . . ? C61 C60 Na3 83.78(14) . . ? N14 C60 H60A 124.5 . . ? C61 C60 H60A 124.5 . . ? Na3 C60 H60A 115.3 . . ? C60 C61 C62 106.2(2) . . ? C60 C61 Na3 69.41(13) . . ? C62 C61 Na3 72.71(13) . . ? C60 C61 H61A 126.9 . . ? C62 C61 H61A 126.9 . . ? Na3 C61 H61A 122.7 . . ? C63 C62 C61 106.8(2) . . ? C63 C62 Na3 66.66(13) . . ? C61 C62 Na3 80.24(14) . . ? C63 C62 H62A 126.6 . . ? C61 C62 H62A 126.6 . . ? Na3 C62 H62A 118.3 . . ? N14 C63 C62 110.3(2) . . ? N14 C63 Na3 73.44(12) . . ? C62 C63 Na3 85.30(15) . . ? N14 C63 H63A 124.8 . . ? C62 C63 H63A 124.8 . . ? Na3 C63 H63A 108.7 . . ? C67 N15 C64 104.96(19) . . ? C67 N15 Zn2 122.81(16) . . ? C64 N15 Zn2 132.07(16) . . ? N15 C64 C65 111.4(2) . . ? N15 C64 H64A 124.3 . . ? C65 C64 H64A 124.3 . . ? C64 C65 C66 106.2(2) . . ? C64 C65 H65A 126.9 . . ? C66 C65 H65A 126.9 . . ? C67 C66 C65 106.1(2) . . ? C67 C66 H66A 127.0 . . ? C65 C66 H66A 127.0 . . ? N15 C67 C66 111.3(2) . . ? N15 C67 H67A 124.3 . . ? C66 C67 H67A 124.3 . . ? C68 N16 C71 105.6(2) . . ? C68 N16 Zn2 126.98(16) . . ? C71 N16 Zn2 127.46(16) . . ? C68 N16 Na4 83.15(12) . . ? C71 N16 Na4 75.31(12) . . ? Zn2 N16 Na4 108.57(7) . . ? N16 C68 C69 110.7(2) . . ? N16 C68 Na4 68.27(11) . . ? C69 C68 Na4 81.89(14) . . ? N16 C68 H68A 124.7 . . ? C69 C68 H68A 124.7 . . ? Na4 C68 H68A 116.7 . . ? C68 C69 C70 106.6(2) . . ? C68 C69 Na4 70.88(13) . . ? C70 C69 Na4 72.00(13) . . ? C68 C69 H69A 126.7 . . ? C70 C69 H69A 126.7 . . ? Na4 C69 H69A 122.2 . . ? C71 C70 C69 106.3(2) . . ? C71 C70 Na4 67.39(13) . . ? C69 C70 Na4 80.27(14) . . ? C71 C70 H70A 126.8 . . ? C69 C70 H70A 126.8 . . ? Na4 C70 H70A 117.5 . . ? C70 C71 N16 110.8(2) . . ? C70 C71 Na4 84.20(14) . . ? N16 C71 Na4 74.73(11) . . ? C70 C71 H71A 124.6 . . ? N16 C71 H71A 124.6 . . ? Na4 C71 H71A 108.7 . . ? C72 N17 C75 105.48(19) . . ? C72 N17 Zn2 128.59(15) . . ? C75 N17 Zn2 125.46(17) . . ? N17 C72 C73 110.8(2) . . ? N17 C72 H72A 124.6 . . ? C73 C72 H72A 124.6 . . ? C72 C73 C74 106.3(2) . . ? C72 C73 H73A 126.8 . . ? C74 C73 H73A 126.8 . . ? C75 C74 C73 106.2(2) . . ? C75 C74 H74A 126.9 . . ? C73 C74 H74A 126.9 . . ? N17 C75 C74 111.1(2) . . ? N17 C75 H75A 124.4 . . ? C74 C75 H75A 124.4 . . ? N19 Na4 N18 75.03(7) . . ? N19 Na4 N20 75.45(8) . . ? N18 Na4 N20 113.04(8) . . ? N19 Na4 N16 143.97(8) . . ? N18 Na4 N16 113.37(7) . . ? N20 Na4 N16 125.48(7) . . ? N19 Na4 C71 127.49(8) . . ? N18 Na4 C71 142.42(8) . . ? N20 Na4 C71 102.56(8) . . ? N16 Na4 C71 29.95(6) . . ? N19 Na4 C68 118.92(8) . . ? N18 Na4 C68 97.50(8) . . ? N20 Na4 C68 149.12(7) . . ? N16 Na4 C68 28.58(6) . . ? C71 Na4 C68 46.63(7) . . ? N19 Na4 C70 100.65(8) . . ? N18 Na4 C70 136.56(8) . . ? N20 Na4 C70 107.20(8) . . ? N16 Na4 C70 48.12(7) . . ? C71 Na4 C70 28.41(7) . . ? C68 Na4 C70 45.96(7) . . ? N19 Na4 C69 97.17(8) . . ? N18 Na4 C69 108.92(8) . . ? N20 Na4 C69 133.39(8) . . ? N16 Na4 C69 46.82(6) . . ? C71 Na4 C69 46.03(7) . . ? C68 Na4 C69 27.23(7) . . ? C70 Na4 C69 27.73(7) . . ? C81 N18 C80 110.1(5) . . ? C81 N18 C80A 120(3) . . ? C80 N18 C81A 95.6(19) . . ? C80A N18 C81A 105(4) . . ? C81 N18 C82 113.4(3) . . ? C80 N18 C82 105.8(7) . . ? C80A N18 C82 100(4) . . ? C81A N18 C82 127.5(19) . . ? C81 N18 C82A 80.3(9) . . ? C80 N18 C82A 128.4(10) . . ? C80A N18 C82A 127(5) . . ? C81A N18 C82A 95.9(19) . . ? C81 N18 Na4 106.0(4) . . ? C80 N18 Na4 116.7(6) . . ? C80A N18 Na4 112(4) . . ? C81A N18 Na4 107(2) . . ? C82 N18 Na4 104.91(16) . . ? C82A N18 Na4 107.4(7) . . ? C85 N19 C84 109.5(2) . . ? C85 N19 C83 115.2(2) . . ? C84 N19 C83 106.0(2) . . ? C85 N19 C83A 89.4(9) . . ? C84 N19 C83A 130.9(9) . . ? C85 N19 Na4 107.17(16) . . ? C84 N19 Na4 111.69(16) . . ? C83 N19 Na4 107.28(17) . . ? C83A N19 Na4 104.4(9) . . ? C86 N20 C88 110.1(2) . . ? C86 N20 C87 111.0(2) . . ? C88 N20 C87 108.8(2) . . ? C86 N20 Na4 103.01(16) . . ? C88 N20 Na4 112.03(16) . . ? C87 N20 Na4 111.85(16) . . ? N18 C80 H80A 109.5 . . ? N18 C80 H80B 109.5 . . ? N18 C80 H80C 109.5 . . ? N18 C81 H81A 109.5 . . ? N18 C81 H81B 109.5 . . ? N18 C81 H81C 109.5 . . ? N18 C82 C83 113.4(2) . . ? N18 C82 H82A 108.9 . . ? C83 C82 H82A 108.9 . . ? N18 C82 H82B 108.9 . . ? C83 C82 H82B 108.9 . . ? H82A C82 H82B 107.7 . . ? N19 C83 C82 111.4(3) . . ? N19 C83 H83A 109.3 . . ? C82 C83 H83A 109.3 . . ? N19 C83 H83B 109.3 . . ? C82 C83 H83B 109.4 . . ? H83A C83 H83B 108.0 . . ? N18 C81A H81D 109.5 . . ? N18 C81A H81E 109.5 . . ? H81D C81A H81E 109.5 . . ? N18 C81A H81F 109.5 . . ? H81D C81A H81F 109.5 . . ? H81E C81A H81F 109.5 . . ? N18 C80A H80D 109.5 . . ? N18 C80A H80E 109.5 . . ? H80D C80A H80E 109.5 . . ? N18 C80A H80F 109.5 . . ? H80D C80A H80F 109.5 . . ? H80E C80A H80F 109.5 . . ? N18 C82A C83A 102.1(15) . . ? N18 C82A H82C 111.3 . . ? C83A C82A H82C 111.3 . . ? N18 C82A H82D 111.4 . . ? C83A C82A H82D 111.4 . . ? H82C C82A H82D 109.2 . . ? N19 C83A C82A 110.1(14) . . ? N19 C83A H83C 109.6 . . ? C82A C83A H83C 109.6 . . ? N19 C83A H83D 109.7 . . ? C82A C83A H83D 109.7 . . ? H83C C83A H83D 108.1 . . ? N19 C84 H84A 109.5 . . ? N19 C84 H84B 109.5 . . ? H84A C84 H84B 109.5 . . ? N19 C84 H84C 109.5 . . ? H84A C84 H84C 109.5 . . ? H84B C84 H84C 109.5 . . ? N19 C85 C86 112.4(2) . . ? N19 C85 H85A 109.1 . . ? C86 C85 H85A 109.1 . . ? N19 C85 H85B 109.1 . . ? C86 C85 H85B 109.1 . . ? H85A C85 H85B 107.9 . . ? N20 C86 C85 113.5(2) . . ? N20 C86 H86A 108.9 . . ? C85 C86 H86A 108.9 . . ? N20 C86 H86B 108.9 . . ? C85 C86 H86B 108.9 . . ? H86A C86 H86B 107.7 . . ? N20 C87 H87A 109.5 . . ? N20 C87 H87B 109.5 . . ? H87A C87 H87B 109.5 . . ? N20 C87 H87C 109.5 . . ? H87A C87 H87C 109.5 . . ? H87B C87 H87C 109.5 . . ? N20 C88 H88A 109.5 . . ? N20 C88 H88B 109.5 . . ? H88A C88 H88B 109.5 . . ? N20 C88 H88C 109.5 . . ? H88A C88 H88C 109.5 . . ? H88B C88 H88C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N3 Na1 N1 C3 90.06(14) . . . . ? N2 Na1 N1 C3 20.99(13) . . . . ? N4 Na1 N1 C3 -120.88(13) . . . . ? C10 Na1 N1 C3 -100.66(14) . . . . ? C13 Na1 N1 C3 -94.86(18) . . . . ? C11 Na1 N1 C3 -73.13(14) . . . . ? C12 Na1 N1 C3 -62.10(16) . . . . ? N3 Na1 N1 C2 -153.32(15) . . . . ? N2 Na1 N1 C2 137.61(16) . . . . ? N4 Na1 N1 C2 -4.26(18) . . . . ? C10 Na1 N1 C2 15.96(16) . . . . ? C13 Na1 N1 C2 21.8(2) . . . . ? C11 Na1 N1 C2 43.49(16) . . . . ? C12 Na1 N1 C2 54.52(18) . . . . ? C3 Na1 N1 C2 116.6(2) . . . . ? N3 Na1 N1 C1 -30.00(17) . . . . ? N2 Na1 N1 C1 -99.06(16) . . . . ? N4 Na1 N1 C1 119.07(16) . . . . ? C10 Na1 N1 C1 139.28(16) . . . . ? C13 Na1 N1 C1 145.09(17) . . . . ? C11 Na1 N1 C1 166.81(16) . . . . ? C12 Na1 N1 C1 177.84(15) . . . . ? C3 Na1 N1 C1 -120.1(2) . . . . ? N1 Na1 N2 C5 -111.58(16) . . . . ? N3 Na1 N2 C5 134.66(17) . . . . ? N4 Na1 N2 C5 13.9(2) . . . . ? C10 Na1 N2 C5 -18.71(19) . . . . ? C13 Na1 N2 C5 34.92(18) . . . . ? C11 Na1 N2 C5 -8.75(17) . . . . ? C12 Na1 N2 C5 18.27(16) . . . . ? C3 Na1 N2 C5 -99.37(17) . . . . ? N1 Na1 N2 C4 8.97(13) . . . . ? N3 Na1 N2 C4 -104.79(14) . . . . ? N4 Na1 N2 C4 134.45(14) . . . . ? C10 Na1 N2 C4 101.85(14) . . . . ? C13 Na1 N2 C4 155.47(13) . . . . ? C11 Na1 N2 C4 111.80(13) . . . . ? C12 Na1 N2 C4 138.82(13) . . . . ? C3 Na1 N2 C4 21.18(12) . . . . ? N1 Na1 N2 C6 127.44(14) . . . . ? N3 Na1 N2 C6 13.69(14) . . . . ? N4 Na1 N2 C6 -107.08(15) . . . . ? C10 Na1 N2 C6 -139.68(14) . . . . ? C13 Na1 N2 C6 -86.05(15) . . . . ? C11 Na1 N2 C6 -129.73(14) . . . . ? C12 Na1 N2 C6 -102.71(14) . . . . ? C3 Na1 N2 C6 139.66(16) . . . . ? N1 Na1 N3 C8 65.46(18) . . . . ? N2 Na1 N3 C8 135.29(17) . . . . ? N4 Na1 N3 C8 -84.33(17) . . . . ? C10 Na1 N3 C8 -93.2(2) . . . . ? C13 Na1 N3 C8 -111.72(17) . . . . ? C11 Na1 N3 C8 -142.57(16) . . . . ? C12 Na1 N3 C8 -138.27(16) . . . . ? C3 Na1 N3 C8 94.15(17) . . . . ? N1 Na1 N3 C9 -174.06(15) . . . . ? N2 Na1 N3 C9 -104.23(16) . . . . ? N4 Na1 N3 C9 36.15(18) . . . . ? C10 Na1 N3 C9 27.3(2) . . . . ? C13 Na1 N3 C9 8.76(17) . . . . ? C11 Na1 N3 C9 -22.1(2) . . . . ? C12 Na1 N3 C9 -17.79(17) . . . . ? C3 Na1 N3 C9 -145.37(15) . . . . ? N1 Na1 N3 C7 -56.11(15) . . . . ? N2 Na1 N3 C7 13.72(14) . . . . ? N4 Na1 N3 C7 154.10(14) . . . . ? C10 Na1 N3 C7 145.26(17) . . . . ? C13 Na1 N3 C7 126.71(14) . . . . ? C11 Na1 N3 C7 95.86(17) . . . . ? C12 Na1 N3 C7 100.16(15) . . . . ? C3 Na1 N3 C7 -27.42(16) . . . . ? C2 N1 C3 C4 -168.13(18) . . . . ? C1 N1 C3 C4 71.5(2) . . . . ? Na1 N1 C3 C4 -51.12(19) . . . . ? C2 N1 C3 Na1 -117.02(18) . . . . ? C1 N1 C3 Na1 122.60(19) . . . . ? N3 Na1 C3 N1 -98.76(13) . . . . ? N2 Na1 C3 N1 -153.47(16) . . . . ? N4 Na1 C3 N1 79.46(15) . . . . ? C10 Na1 C3 N1 85.02(14) . . . . ? C13 Na1 C3 N1 121.78(15) . . . . ? C11 Na1 C3 N1 111.30(13) . . . . ? C12 Na1 C3 N1 131.95(13) . . . . ? N1 Na1 C3 C4 133.3(2) . . . . ? N3 Na1 C3 C4 34.58(14) . . . . ? N2 Na1 C3 C4 -20.13(12) . . . . ? N4 Na1 C3 C4 -147.20(12) . . . . ? C10 Na1 C3 C4 -141.64(13) . . . . ? C13 Na1 C3 C4 -104.88(15) . . . . ? C11 Na1 C3 C4 -115.36(13) . . . . ? C12 Na1 C3 C4 -94.71(13) . . . . ? C5 N2 C4 C3 84.8(2) . . . . ? C6 N2 C4 C3 -153.55(19) . . . . ? Na1 N2 C4 C3 -38.5(2) . . . . ? N1 C3 C4 N2 66.6(2) . . . . ? Na1 C3 C4 N2 29.09(16) . . . . ? C5 N2 C6 C7 -164.9(2) . . . . ? C4 N2 C6 C7 73.2(3) . . . . ? Na1 N2 C6 C7 -41.1(2) . . . . ? C8 N3 C7 C6 -168.2(2) . . . . ? C9 N3 C7 C6 72.4(3) . . . . ? Na1 N3 C7 C6 -41.1(2) . . . . ? N2 C6 C7 N3 59.7(3) . . . . ? N5 Zn1 N4 C10 -165.38(16) . . . . ? N6 Zn1 N4 C10 -42.29(17) . . . . ? N7 Zn1 N4 C10 75.47(17) . . . . ? Na2 Zn1 N4 C10 53.6(2) . . . . ? N5 Zn1 N4 C13 18.54(19) . . . . ? N6 Zn1 N4 C13 141.63(17) . . . . ? N7 Zn1 N4 C13 -100.60(18) . . . . ? Na2 Zn1 N4 C13 -122.52(17) . . . . ? N5 Zn1 N4 Na1 -74.38(9) . . . . ? N6 Zn1 N4 Na1 48.71(9) . . . . ? N7 Zn1 N4 Na1 166.48(8) . . . . ? Na2 Zn1 N4 Na1 144.56(8) . . . . ? N1 Na1 N4 C10 43.53(16) . . . . ? N3 Na1 N4 C10 -171.00(14) . . . . ? N2 Na1 N4 C10 -66.25(17) . . . . ? C13 Na1 N4 C10 -107.10(19) . . . . ? C11 Na1 N4 C10 -34.83(13) . . . . ? C12 Na1 N4 C10 -72.21(14) . . . . ? C3 Na1 N4 C10 10.98(17) . . . . ? N1 Na1 N4 C13 150.63(13) . . . . ? N3 Na1 N4 C13 -63.90(14) . . . . ? N2 Na1 N4 C13 40.85(17) . . . . ? C10 Na1 N4 C13 107.10(19) . . . . ? C11 Na1 N4 C13 72.27(14) . . . . ? C12 Na1 N4 C13 34.89(12) . . . . ? C3 Na1 N4 C13 118.08(14) . . . . ? N1 Na1 N4 Zn1 -80.48(10) . . . . ? N3 Na1 N4 Zn1 64.98(11) . . . . ? N2 Na1 N4 Zn1 169.74(9) . . . . ? C10 Na1 N4 Zn1 -124.02(17) . . . . ? C13 Na1 N4 Zn1 128.88(16) . . . . ? C11 Na1 N4 Zn1 -158.85(12) . . . . ? C12 Na1 N4 Zn1 163.78(12) . . . . ? C3 Na1 N4 Zn1 -113.03(10) . . . . ? C13 N4 C10 C11 -0.8(2) . . . . ? Zn1 N4 C10 C11 -177.64(14) . . . . ? Na1 N4 C10 C11 77.84(16) . . . . ? C13 N4 C10 Na1 -78.62(13) . . . . ? Zn1 N4 C10 Na1 104.52(13) . . . . ? N1 Na1 C10 N4 -144.00(13) . . . . ? N3 Na1 C10 N4 15.5(2) . . . . ? N2 Na1 C10 N4 135.98(13) . . . . ? C13 Na1 C10 N4 40.40(12) . . . . ? C11 Na1 C10 N4 114.0(2) . . . . ? C12 Na1 C10 N4 78.51(14) . . . . ? C3 Na1 C10 N4 -171.73(13) . . . . ? N1 Na1 C10 C11 101.99(15) . . . . ? N3 Na1 C10 C11 -98.52(19) . . . . ? N2 Na1 C10 C11 21.97(17) . . . . ? N4 Na1 C10 C11 -114.0(2) . . . . ? C13 Na1 C10 C11 -73.62(16) . . . . ? C12 Na1 C10 C11 -35.50(14) . . . . ? C3 Na1 C10 C11 74.26(15) . . . . ? N4 C10 C11 C12 0.6(2) . . . . ? Na1 C10 C11 C12 66.80(16) . . . . ? N4 C10 C11 Na1 -66.21(14) . . . . ? N1 Na1 C11 C10 -83.80(15) . . . . ? N3 Na1 C11 C10 123.54(16) . . . . ? N2 Na1 C11 C10 -161.53(15) . . . . ? N4 Na1 C11 C10 38.05(14) . . . . ? C13 Na1 C11 C10 79.49(16) . . . . ? C12 Na1 C11 C10 115.1(2) . . . . ? C3 Na1 C11 C10 -110.04(15) . . . . ? N1 Na1 C11 C12 161.12(14) . . . . ? N3 Na1 C11 C12 8.5(2) . . . . ? N2 Na1 C11 C12 83.39(14) . . . . ? N4 Na1 C11 C12 -77.03(15) . . . . ? C10 Na1 C11 C12 -115.1(2) . . . . ? C13 Na1 C11 C12 -35.59(13) . . . . ? C3 Na1 C11 C12 134.88(14) . . . . ? C10 C11 C12 C13 -0.2(2) . . . . ? Na1 C11 C12 C13 59.39(15) . . . . ? C10 C11 C12 Na1 -59.55(15) . . . . ? N1 Na1 C12 C13 -139.20(15) . . . . ? N3 Na1 C12 C13 70.41(16) . . . . ? N2 Na1 C12 C13 145.64(15) . . . . ? N4 Na1 C12 C13 -38.17(13) . . . . ? C10 Na1 C12 C13 -79.56(15) . . . . ? C11 Na1 C12 C13 -115.2(2) . . . . ? C3 Na1 C12 C13 -165.53(14) . . . . ? N1 Na1 C12 C11 -23.98(17) . . . . ? N3 Na1 C12 C11 -174.38(14) . . . . ? N2 Na1 C12 C11 -99.15(14) . . . . ? N4 Na1 C12 C11 77.05(15) . . . . ? C10 Na1 C12 C11 35.65(13) . . . . ? C13 Na1 C12 C11 115.2(2) . . . . ? C3 Na1 C12 C11 -50.31(15) . . . . ? C10 N4 C13 C12 0.7(2) . . . . ? Zn1 N4 C13 C12 177.34(14) . . . . ? Na1 N4 C13 C12 -77.71(16) . . . . ? C10 N4 C13 Na1 78.38(13) . . . . ? Zn1 N4 C13 Na1 -104.95(15) . . . . ? C11 C12 C13 N4 -0.3(2) . . . . ? Na1 C12 C13 N4 65.85(14) . . . . ? C11 C12 C13 Na1 -66.17(16) . . . . ? N1 Na1 C13 N4 -48.2(2) . . . . ? N3 Na1 C13 N4 127.00(13) . . . . ? N2 Na1 C13 N4 -152.47(12) . . . . ? C10 Na1 C13 N4 -40.33(12) . . . . ? C11 Na1 C13 N4 -78.43(14) . . . . ? C12 Na1 C13 N4 -113.9(2) . . . . ? C3 Na1 C13 N4 -93.16(16) . . . . ? N1 Na1 C13 C12 65.7(2) . . . . ? N3 Na1 C13 C12 -119.14(14) . . . . ? N2 Na1 C13 C12 -38.62(16) . . . . ? N4 Na1 C13 C12 113.9(2) . . . . ? C10 Na1 C13 C12 73.52(15) . . . . ? C11 Na1 C13 C12 35.42(13) . . . . ? C3 Na1 C13 C12 20.7(2) . . . . ? N4 Zn1 N5 C17 125.3(2) . . . . ? N6 Zn1 N5 C17 5.1(2) . . . . ? N7 Zn1 N5 C17 -114.1(2) . . . . ? Na2 Zn1 N5 C17 -71.3(2) . . . . ? N4 Zn1 N5 C14 -49.5(2) . . . . ? N6 Zn1 N5 C14 -169.8(2) . . . . ? N7 Zn1 N5 C14 71.0(2) . . . . ? Na2 Zn1 N5 C14 113.9(2) . . . . ? C17 N5 C14 C15 0.2(3) . . . . ? Zn1 N5 C14 C15 175.92(18) . . . . ? N5 C14 C15 C16 -0.2(3) . . . . ? C14 C15 C16 C17 0.2(3) . . . . ? C14 N5 C17 C16 0.0(3) . . . . ? Zn1 N5 C17 C16 -175.70(18) . . . . ? C15 C16 C17 N5 -0.1(3) . . . . ? N5 Zn1 N6 C18 34.3(2) . . . . ? N4 Zn1 N6 C18 -86.0(2) . . . . ? N7 Zn1 N6 C18 154.12(19) . . . . ? Na2 Zn1 N6 C18 121.7(2) . . . . ? N5 Zn1 N6 C21 -147.3(2) . . . . ? N4 Zn1 N6 C21 92.5(2) . . . . ? N7 Zn1 N6 C21 -27.4(2) . . . . ? Na2 Zn1 N6 C21 -59.9(2) . . . . ? C21 N6 C18 C19 0.3(3) . . . . ? Zn1 N6 C18 C19 178.99(17) . . . . ? N6 C18 C19 C20 -0.2(3) . . . . ? C18 C19 C20 C21 0.0(3) . . . . ? C18 N6 C21 C20 -0.3(3) . . . . ? Zn1 N6 C21 C20 -179.00(17) . . . . ? C19 C20 C21 N6 0.2(3) . . . . ? N5 Zn1 N7 C25 -11.1(2) . . . . ? N4 Zn1 N7 C25 107.92(19) . . . . ? N6 Zn1 N7 C25 -133.78(18) . . . . ? Na2 Zn1 N7 C25 -86.00(19) . . . . ? N5 Zn1 N7 C22 169.98(19) . . . . ? N4 Zn1 N7 C22 -71.0(2) . . . . ? N6 Zn1 N7 C22 47.3(2) . . . . ? Na2 Zn1 N7 C22 95.1(2) . . . . ? N5 Zn1 N7 Na2 74.87(10) . . . . ? N4 Zn1 N7 Na2 -166.08(7) . . . . ? N6 Zn1 N7 Na2 -47.78(10) . . . . ? C25 N7 C22 C23 1.4(3) . . . . ? Zn1 N7 C22 C23 -179.57(17) . . . . ? Na2 N7 C22 C23 -77.3(2) . . . . ? C25 N7 C22 Na2 78.71(15) . . . . ? Zn1 N7 C22 Na2 -102.24(16) . . . . ? N7 C22 C23 C24 -0.8(3) . . . . ? Na2 C22 C23 C24 -62.6(2) . . . . ? N7 C22 C23 Na2 61.75(16) . . . . ? C22 C23 C24 C25 -0.1(3) . . . . ? Na2 C23 C24 C25 -57.59(18) . . . . ? C22 C23 C24 Na2 57.48(19) . . . . ? C22 N7 C25 C24 -1.4(3) . . . . ? Zn1 N7 C25 C24 179.46(16) . . . . ? Na2 N7 C25 C24 82.00(19) . . . . ? C22 N7 C25 Na2 -83.42(15) . . . . ? Zn1 N7 C25 Na2 97.47(14) . . . . ? C23 C24 C25 N7 1.0(3) . . . . ? Na2 C24 C25 N7 -68.26(17) . . . . ? C23 C24 C25 Na2 69.2(2) . . . . ? C25 N7 Na2 N9 132.76(18) . . . . ? C22 N7 Na2 N9 -120.70(17) . . . . ? Zn1 N7 Na2 N9 9.20(18) . . . . ? C25 N7 Na2 N10 -115.77(16) . . . . ? C22 N7 Na2 N10 -9.23(16) . . . . ? Zn1 N7 Na2 N10 120.68(9) . . . . ? C25 N7 Na2 N8 37.22(17) . . . . ? C22 N7 Na2 N8 143.76(14) . . . . ? Zn1 N7 Na2 N8 -86.34(9) . . . . ? C22 N7 Na2 C25 106.5(2) . . . . ? Zn1 N7 Na2 C25 -123.56(19) . . . . ? C25 N7 Na2 C22 -106.5(2) . . . . ? Zn1 N7 Na2 C22 129.90(17) . . . . ? C25 N7 Na2 C24 -36.04(16) . . . . ? C22 N7 Na2 C24 70.50(16) . . . . ? Zn1 N7 Na2 C24 -159.60(15) . . . . ? C25 N7 Na2 C23 -72.44(17) . . . . ? C22 N7 Na2 C23 34.10(15) . . . . ? Zn1 N7 Na2 C23 164.00(15) . . . . ? C25 N7 Na2 Zn1 123.56(19) . . . . ? C22 N7 Na2 Zn1 -129.90(17) . . . . ? N7 C25 Na2 N9 -102.3(2) . . . . ? C24 C25 Na2 N9 146.5(2) . . . . ? N7 C25 Na2 N10 86.14(17) . . . . ? C24 C25 Na2 N10 -25.0(2) . . . . ? N7 C25 Na2 N8 -146.38(15) . . . . ? C24 C25 Na2 N8 102.47(19) . . . . ? C24 C25 Na2 N7 -111.2(3) . . . . ? N7 C25 Na2 C22 39.85(13) . . . . ? C24 C25 Na2 C22 -71.3(2) . . . . ? N7 C25 Na2 C24 111.2(3) . . . . ? N7 C25 Na2 C23 76.76(17) . . . . ? C24 C25 Na2 C23 -34.39(17) . . . . ? N7 C25 Na2 Zn1 -34.03(12) . . . . ? C24 C25 Na2 Zn1 -145.2(2) . . . . ? C23 C22 Na2 N9 -137.7(2) . . . . ? N7 C22 Na2 N9 107.92(19) . . . . ? C23 C22 Na2 N10 -73.5(2) . . . . ? N7 C22 Na2 N10 172.18(14) . . . . ? C23 C22 Na2 N8 64.1(2) . . . . ? N7 C22 Na2 N8 -50.31(17) . . . . ? C23 C22 Na2 N7 114.4(3) . . . . ? C23 C22 Na2 C25 72.9(2) . . . . ? N7 C22 Na2 C25 -41.43(13) . . . . ? C23 C22 Na2 C24 34.28(18) . . . . ? N7 C22 Na2 C24 -80.08(17) . . . . ? N7 C22 Na2 C23 -114.4(3) . . . . ? C23 C22 Na2 Zn1 145.0(2) . . . . ? N7 C22 Na2 Zn1 30.69(11) . . . . ? C25 C24 Na2 N9 -114.9(3) . . . . ? C23 C24 Na2 N9 129.6(3) . . . . ? C25 C24 Na2 N10 160.48(18) . . . . ? C23 C24 Na2 N10 44.98(18) . . . . ? C25 C24 Na2 N8 -78.43(19) . . . . ? C23 C24 Na2 N8 166.07(17) . . . . ? C25 C24 Na2 N7 39.98(16) . . . . ? C23 C24 Na2 N7 -75.52(18) . . . . ? C23 C24 Na2 C25 -115.5(3) . . . . ? C25 C24 Na2 C22 81.05(19) . . . . ? C23 C24 Na2 C22 -34.44(16) . . . . ? C25 C24 Na2 C23 115.5(3) . . . . ? C25 C24 Na2 Zn1 28.64(18) . . . . ? C23 C24 Na2 Zn1 -86.85(16) . . . . ? C22 C23 Na2 N9 98.1(3) . . . . ? C24 C23 Na2 N9 -145.0(2) . . . . ? C22 C23 Na2 N10 106.3(2) . . . . ? C24 C23 Na2 N10 -136.72(17) . . . . ? C22 C23 Na2 N8 -133.05(19) . . . . ? C24 C23 Na2 N8 -16.1(2) . . . . ? C22 C23 Na2 N7 -38.02(17) . . . . ? C24 C23 Na2 N7 78.93(18) . . . . ? C22 C23 Na2 C25 -80.8(2) . . . . ? C24 C23 Na2 C25 36.11(16) . . . . ? C24 C23 Na2 C22 116.9(3) . . . . ? C22 C23 Na2 C24 -116.9(3) . . . . ? C22 C23 Na2 Zn1 -29.07(18) . . . . ? C24 C23 Na2 Zn1 87.88(17) . . . . ? N5 Zn1 Na2 N9 71.92(8) . . . . ? N4 Zn1 Na2 N9 -144.74(13) . . . . ? N6 Zn1 Na2 N9 -41.09(8) . . . . ? N7 Zn1 Na2 N9 -174.45(11) . . . . ? N5 Zn1 Na2 N10 161.54(9) . . . . ? N4 Zn1 Na2 N10 -55.12(15) . . . . ? N6 Zn1 Na2 N10 48.53(9) . . . . ? N7 Zn1 Na2 N10 -84.83(11) . . . . ? N5 Zn1 Na2 N8 -7.07(8) . . . . ? N4 Zn1 Na2 N8 136.27(13) . . . . ? N6 Zn1 Na2 N8 -120.08(8) . . . . ? N7 Zn1 Na2 N8 106.56(10) . . . . ? N5 Zn1 Na2 N7 -113.63(10) . . . . ? N4 Zn1 Na2 N7 29.71(15) . . . . ? N6 Zn1 Na2 N7 133.36(10) . . . . ? N5 Zn1 Na2 C25 -83.10(10) . . . . ? N4 Zn1 Na2 C25 60.24(15) . . . . ? N6 Zn1 Na2 C25 163.89(10) . . . . ? N7 Zn1 Na2 C25 30.53(11) . . . . ? N5 Zn1 Na2 C22 -140.28(9) . . . . ? N4 Zn1 Na2 C22 3.06(14) . . . . ? N6 Zn1 Na2 C22 106.71(9) . . . . ? N7 Zn1 Na2 C22 -26.65(11) . . . . ? N5 Zn1 Na2 C24 -98.62(9) . . . . ? N4 Zn1 Na2 C24 44.72(15) . . . . ? N6 Zn1 Na2 C24 148.37(9) . . . . ? N7 Zn1 Na2 C24 15.01(11) . . . . ? N5 Zn1 Na2 C23 -125.29(9) . . . . ? N4 Zn1 Na2 C23 18.05(14) . . . . ? N6 Zn1 Na2 C23 121.70(9) . . . . ? N7 Zn1 Na2 C23 -11.67(11) . . . . ? N9 Na2 N8 C30 103.82(17) . . . . ? N10 Na2 N8 C30 42.49(18) . . . . ? N7 Na2 N8 C30 -111.56(16) . . . . ? C25 Na2 N8 C30 -93.87(17) . . . . ? C22 Na2 N8 C30 -87.43(19) . . . . ? C24 Na2 N8 C30 -67.08(17) . . . . ? C23 Na2 N8 C30 -60.03(18) . . . . ? Zn1 Na2 N8 C30 -146.97(15) . . . . ? N9 Na2 N8 C32 -13.28(15) . . . . ? N10 Na2 N8 C32 -74.62(17) . . . . ? N7 Na2 N8 C32 131.34(15) . . . . ? C25 Na2 N8 C32 149.02(16) . . . . ? C22 Na2 N8 C32 155.47(15) . . . . ? C24 Na2 N8 C32 175.81(16) . . . . ? C23 Na2 N8 C32 -177.14(15) . . . . ? Zn1 Na2 N8 C32 95.92(15) . . . . ? N9 Na2 N8 C31 -135.82(19) . . . . ? N10 Na2 N8 C31 162.84(17) . . . . ? N7 Na2 N8 C31 8.8(2) . . . . ? C25 Na2 N8 C31 26.48(19) . . . . ? C22 Na2 N8 C31 32.9(2) . . . . ? C24 Na2 N8 C31 53.27(19) . . . . ? C23 Na2 N8 C31 60.3(2) . . . . ? Zn1 Na2 N8 C31 -26.62(18) . . . . ? N10 Na2 N9 C33 111.51(16) . . . . ? N8 Na2 N9 C33 -15.29(15) . . . . ? N7 Na2 N9 C33 -123.41(17) . . . . ? C25 Na2 N9 C33 -61.8(3) . . . . ? C22 Na2 N9 C33 -179.50(16) . . . . ? C24 Na2 N9 C33 22.9(4) . . . . ? C23 Na2 N9 C33 120.1(3) . . . . ? Zn1 Na2 N9 C33 -117.90(14) . . . . ? N10 Na2 N9 C35 -9.35(15) . . . . ? N8 Na2 N9 C35 -136.15(17) . . . . ? N7 Na2 N9 C35 115.74(18) . . . . ? C25 Na2 N9 C35 177.4(2) . . . . ? C22 Na2 N9 C35 59.6(2) . . . . ? C24 Na2 N9 C35 -98.0(4) . . . . ? C23 Na2 N9 C35 -0.8(3) . . . . ? Zn1 Na2 N9 C35 121.24(15) . . . . ? N10 Na2 N9 C34 -128.73(16) . . . . ? N8 Na2 N9 C34 104.47(16) . . . . ? N7 Na2 N9 C34 -3.6(2) . . . . ? C25 Na2 N9 C34 58.0(3) . . . . ? C22 Na2 N9 C34 -59.7(2) . . . . ? C24 Na2 N9 C34 142.6(3) . . . . ? C23 Na2 N9 C34 -120.2(3) . . . . ? Zn1 Na2 N9 C34 1.86(17) . . . . ? N9 Na2 N10 C38 100.72(18) . . . . ? N8 Na2 N10 C38 161.54(17) . . . . ? N7 Na2 N10 C38 -46.68(19) . . . . ? C25 Na2 N10 C38 -82.96(19) . . . . ? C22 Na2 N10 C38 -51.16(18) . . . . ? C24 Na2 N10 C38 -94.56(18) . . . . ? C23 Na2 N10 C38 -76.35(18) . . . . ? Zn1 Na2 N10 C38 -6.1(2) . . . . ? N9 Na2 N10 C37 -134.97(19) . . . . ? N8 Na2 N10 C37 -74.16(19) . . . . ? N7 Na2 N10 C37 77.6(2) . . . . ? C25 Na2 N10 C37 41.3(2) . . . . ? C22 Na2 N10 C37 73.14(19) . . . . ? C24 Na2 N10 C37 29.7(2) . . . . ? C23 Na2 N10 C37 47.96(19) . . . . ? Zn1 Na2 N10 C37 118.20(18) . . . . ? N9 Na2 N10 C36 -19.07(15) . . . . ? N8 Na2 N10 C36 41.74(18) . . . . ? N7 Na2 N10 C36 -166.48(15) . . . . ? C25 Na2 N10 C36 157.25(16) . . . . ? C22 Na2 N10 C36 -170.96(16) . . . . ? C24 Na2 N10 C36 145.65(16) . . . . ? C23 Na2 N10 C36 163.86(17) . . . . ? Zn1 Na2 N10 C36 -125.90(15) . . . . ? C30 N8 C32 C33 -70.2(3) . . . . ? C31 N8 C32 C33 169.2(2) . . . . ? Na2 N8 C32 C33 41.3(2) . . . . ? C35 N9 C33 C32 162.04(19) . . . . ? C34 N9 C33 C32 -76.6(2) . . . . ? Na2 N9 C33 C32 42.8(2) . . . . ? N8 C32 C33 N9 -60.4(3) . . . . ? C33 N9 C35 C36 -81.1(3) . . . . ? C34 N9 C35 C36 157.4(2) . . . . ? Na2 N9 C35 C36 38.3(3) . . . . ? C38 N10 C36 C35 -73.3(3) . . . . ? C37 N10 C36 C35 167.9(2) . . . . ? Na2 N10 C36 C35 47.4(2) . . . . ? N9 C35 C36 N10 -62.3(3) . . . . ? N17 Zn2 Na3 N11 -43.71(9) . . . . ? N15 Zn2 Na3 N11 -151.99(9) . . . . ? N16 Zn2 Na3 N11 84.03(16) . . . . ? N14 Zn2 Na3 N11 84.07(10) . . . . ? N17 Zn2 Na3 N13 126.36(8) . . . . ? N15 Zn2 Na3 N13 18.08(7) . . . . ? N16 Zn2 Na3 N13 -105.90(16) . . . . ? N14 Zn2 Na3 N13 -105.86(10) . . . . ? N17 Zn2 Na3 N12 43.69(8) . . . . ? N15 Zn2 Na3 N12 -64.58(8) . . . . ? N16 Zn2 Na3 N12 171.44(15) . . . . ? N14 Zn2 Na3 N12 171.48(10) . . . . ? N17 Zn2 Na3 N14 -127.78(10) . . . . ? N15 Zn2 Na3 N14 123.94(9) . . . . ? N16 Zn2 Na3 N14 -0.04(17) . . . . ? N17 Zn2 Na3 C63 -159.95(9) . . . . ? N15 Zn2 Na3 C63 91.77(9) . . . . ? N16 Zn2 Na3 C63 -32.21(16) . . . . ? N14 Zn2 Na3 C63 -32.17(10) . . . . ? N17 Zn2 Na3 C60 -101.84(8) . . . . ? N15 Zn2 Na3 C60 149.88(8) . . . . ? N16 Zn2 Na3 C60 25.90(16) . . . . ? N14 Zn2 Na3 C60 25.94(10) . . . . ? N17 Zn2 Na3 C62 -145.08(8) . . . . ? N15 Zn2 Na3 C62 106.64(8) . . . . ? N16 Zn2 Na3 C62 -17.34(16) . . . . ? N14 Zn2 Na3 C62 -17.30(10) . . . . ? N17 Zn2 Na3 C61 -117.36(8) . . . . ? N15 Zn2 Na3 C61 134.36(8) . . . . ? N16 Zn2 Na3 C61 10.38(16) . . . . ? N14 Zn2 Na3 C61 10.42(9) . . . . ? N13 Na3 N11 C53 -47.87(17) . . . . ? N12 Na3 N11 C53 17.18(16) . . . . ? N14 Na3 N11 C53 160.79(15) . . . . ? C63 Na3 N11 C53 -164.28(16) . . . . ? C60 Na3 N11 C53 166.55(16) . . . . ? C62 Na3 N11 C53 -149.52(16) . . . . ? C61 Na3 N11 C53 -167.61(17) . . . . ? Zn2 Na3 N11 C53 122.50(15) . . . . ? N13 Na3 N11 C51 -167.78(14) . . . . ? N12 Na3 N11 C51 -102.73(16) . . . . ? N14 Na3 N11 C51 40.88(17) . . . . ? C63 Na3 N11 C51 75.81(18) . . . . ? C60 Na3 N11 C51 46.64(16) . . . . ? C62 Na3 N11 C51 90.57(16) . . . . ? C61 Na3 N11 C51 72.47(15) . . . . ? Zn2 Na3 N11 C51 2.59(18) . . . . ? N13 Na3 N11 C52 71.26(18) . . . . ? N12 Na3 N11 C52 136.31(19) . . . . ? N14 Na3 N11 C52 -80.08(19) . . . . ? C63 Na3 N11 C52 -45.2(2) . . . . ? C60 Na3 N11 C52 -74.32(18) . . . . ? C62 Na3 N11 C52 -30.39(19) . . . . ? C61 Na3 N11 C52 -48.48(18) . . . . ? Zn2 Na3 N11 C52 -118.37(17) . . . . ? N11 Na3 N12 C56 -108.48(16) . . . . ? N13 Na3 N12 C56 10.50(15) . . . . ? N14 Na3 N12 C56 129.91(16) . . . . ? C63 Na3 N12 C56 74.1(2) . . . . ? C60 Na3 N12 C56 -178.81(15) . . . . ? C62 Na3 N12 C56 -15.3(4) . . . . ? C61 Na3 N12 C56 -122.2(2) . . . . ? Zn2 Na3 N12 C56 122.29(14) . . . . ? N11 Na3 N12 C55 130.18(18) . . . . ? N13 Na3 N12 C55 -110.84(17) . . . . ? N14 Na3 N12 C55 8.6(2) . . . . ? C63 Na3 N12 C55 -47.3(3) . . . . ? C60 Na3 N12 C55 59.8(2) . . . . ? C62 Na3 N12 C55 -136.6(3) . . . . ? C61 Na3 N12 C55 116.4(2) . . . . ? Zn2 Na3 N12 C55 0.95(18) . . . . ? N11 Na3 N12 C54 10.83(16) . . . . ? N13 Na3 N12 C54 129.81(17) . . . . ? N14 Na3 N12 C54 -110.79(18) . . . . ? C63 Na3 N12 C54 -166.62(19) . . . . ? C60 Na3 N12 C54 -59.5(2) . . . . ? C62 Na3 N12 C54 104.0(4) . . . . ? C61 Na3 N12 C54 -2.9(3) . . . . ? Zn2 Na3 N12 C54 -118.40(16) . . . . ? N11 Na3 N13 C59 -37.30(18) . . . . ? N12 Na3 N13 C59 -101.85(18) . . . . ? N14 Na3 N13 C59 114.66(17) . . . . ? C63 Na3 N13 C59 100.73(18) . . . . ? C60 Na3 N13 C59 85.6(2) . . . . ? C62 Na3 N13 C59 72.64(18) . . . . ? C61 Na3 N13 C59 61.02(19) . . . . ? Zn2 Na3 N13 C59 150.63(16) . . . . ? N11 Na3 N13 C58 -159.76(15) . . . . ? N12 Na3 N13 C58 135.70(17) . . . . ? N14 Na3 N13 C58 -7.80(18) . . . . ? C63 Na3 N13 C58 -21.73(17) . . . . ? C60 Na3 N13 C58 -36.8(2) . . . . ? C62 Na3 N13 C58 -49.82(17) . . . . ? C61 Na3 N13 C58 -61.44(18) . . . . ? Zn2 Na3 N13 C58 28.17(17) . . . . ? N11 Na3 N13 C57 83.18(16) . . . . ? N12 Na3 N13 C57 18.64(15) . . . . ? N14 Na3 N13 C57 -124.86(15) . . . . ? C63 Na3 N13 C57 -138.79(15) . . . . ? C60 Na3 N13 C57 -153.89(15) . . . . ? C62 Na3 N13 C57 -166.88(15) . . . . ? C61 Na3 N13 C57 -178.50(14) . . . . ? Zn2 Na3 N13 C57 -88.89(15) . . . . ? C51 N11 C53 C54 73.6(3) . . . . ? C52 N11 C53 C54 -167.5(2) . . . . ? Na3 N11 C53 C54 -45.1(3) . . . . ? C56 N12 C54 C53 77.3(3) . . . . ? C55 N12 C54 C53 -161.7(2) . . . . ? Na3 N12 C54 C53 -38.7(3) . . . . ? N11 C53 C54 N12 60.7(3) . . . . ? C55 N12 C56 C57 83.9(2) . . . . ? C54 N12 C56 C57 -156.4(2) . . . . ? Na3 N12 C56 C57 -39.7(2) . . . . ? C59 N13 C57 C56 72.3(3) . . . . ? C58 N13 C57 C56 -167.6(2) . . . . ? Na3 N13 C57 C56 -48.2(2) . . . . ? N12 C56 C57 N13 64.9(3) . . . . ? N17 Zn2 N14 C63 138.96(17) . . . . ? N15 Zn2 N14 C63 23.98(19) . . . . ? N16 Zn2 N14 C63 -96.92(18) . . . . ? Na3 Zn2 N14 C63 83.09(17) . . . . ? N17 Zn2 N14 C60 -37.6(2) . . . . ? N15 Zn2 N14 C60 -152.60(19) . . . . ? N16 Zn2 N14 C60 86.5(2) . . . . ? Na3 Zn2 N14 C60 -93.5(2) . . . . ? N17 Zn2 N14 Na3 55.87(9) . . . . ? N15 Zn2 N14 Na3 -59.12(9) . . . . ? N16 Zn2 N14 Na3 179.98(7) . . . . ? N11 Na3 N14 C63 119.86(14) . . . . ? N13 Na3 N14 C63 -29.23(15) . . . . ? N12 Na3 N14 C63 -133.98(15) . . . . ? C60 Na3 N14 C63 107.77(18) . . . . ? C62 Na3 N14 C63 36.14(13) . . . . ? C61 Na3 N14 C63 73.55(14) . . . . ? Zn2 Na3 N14 C63 -120.58(16) . . . . ? N11 Na3 N14 C60 12.08(15) . . . . ? N13 Na3 N14 C60 -137.01(13) . . . . ? N12 Na3 N14 C60 118.25(15) . . . . ? C63 Na3 N14 C60 -107.77(18) . . . . ? C62 Na3 N14 C60 -71.63(14) . . . . ? C61 Na3 N14 C60 -34.22(13) . . . . ? Zn2 Na3 N14 C60 131.64(16) . . . . ? N11 Na3 N14 Zn2 -119.56(8) . . . . ? N13 Na3 N14 Zn2 91.35(9) . . . . ? N12 Na3 N14 Zn2 -13.39(16) . . . . ? C63 Na3 N14 Zn2 120.58(16) . . . . ? C60 Na3 N14 Zn2 -131.64(16) . . . . ? C62 Na3 N14 Zn2 156.73(13) . . . . ? C61 Na3 N14 Zn2 -165.86(12) . . . . ? C63 N14 C60 C61 -0.9(3) . . . . ? Zn2 N14 C60 C61 176.06(16) . . . . ? Na3 N14 C60 C61 73.68(17) . . . . ? C63 N14 C60 Na3 -74.62(15) . . . . ? Zn2 N14 C60 Na3 102.38(17) . . . . ? N11 Na3 C60 N14 -169.73(13) . . . . ? N13 Na3 C60 N14 61.65(16) . . . . ? N12 Na3 C60 N14 -104.94(17) . . . . ? C63 Na3 C60 N14 40.52(12) . . . . ? C62 Na3 C60 N14 80.13(14) . . . . ? C61 Na3 C60 N14 115.6(2) . . . . ? Zn2 Na3 C60 N14 -28.97(10) . . . . ? N11 Na3 C60 C61 74.67(16) . . . . ? N13 Na3 C60 C61 -53.95(19) . . . . ? N12 Na3 C60 C61 139.45(17) . . . . ? N14 Na3 C60 C61 -115.6(2) . . . . ? C63 Na3 C60 C61 -75.09(16) . . . . ? C62 Na3 C60 C61 -35.48(14) . . . . ? Zn2 Na3 C60 C61 -144.58(17) . . . . ? N14 C60 C61 C62 0.5(3) . . . . ? Na3 C60 C61 C62 63.89(17) . . . . ? N14 C60 C61 Na3 -63.40(15) . . . . ? N11 Na3 C61 C60 -105.39(16) . . . . ? N13 Na3 C61 C60 141.66(15) . . . . ? N12 Na3 C61 C60 -92.2(3) . . . . ? N14 Na3 C61 C60 36.61(14) . . . . ? C63 Na3 C61 C60 78.10(16) . . . . ? C62 Na3 C61 C60 115.4(2) . . . . ? Zn2 Na3 C61 C60 29.00(14) . . . . ? N11 Na3 C61 C62 139.17(15) . . . . ? N13 Na3 C61 C62 26.21(17) . . . . ? N12 Na3 C61 C62 152.4(2) . . . . ? N14 Na3 C61 C62 -78.84(15) . . . . ? C63 Na3 C61 C62 -37.34(14) . . . . ? C60 Na3 C61 C62 -115.4(2) . . . . ? Zn2 Na3 C61 C62 -86.45(14) . . . . ? C60 C61 C62 C63 0.2(3) . . . . ? Na3 C61 C62 C63 61.84(16) . . . . ? C60 C61 C62 Na3 -61.69(16) . . . . ? N11 Na3 C62 C63 -156.17(15) . . . . ? N13 Na3 C62 C63 89.64(16) . . . . ? N12 Na3 C62 C63 114.4(4) . . . . ? N14 Na3 C62 C63 -38.13(14) . . . . ? C60 Na3 C62 C63 -78.04(16) . . . . ? C61 Na3 C62 C63 -113.2(2) . . . . ? Zn2 Na3 C62 C63 -25.75(14) . . . . ? N11 Na3 C62 C61 -42.98(16) . . . . ? N13 Na3 C62 C61 -157.18(15) . . . . ? N12 Na3 C62 C61 -132.4(3) . . . . ? N14 Na3 C62 C61 75.06(15) . . . . ? C63 Na3 C62 C61 113.2(2) . . . . ? C60 Na3 C62 C61 35.15(14) . . . . ? Zn2 Na3 C62 C61 87.44(14) . . . . ? C60 N14 C63 C62 1.0(3) . . . . ? Zn2 N14 C63 C62 -176.33(15) . . . . ? Na3 N14 C63 C62 -78.39(18) . . . . ? C60 N14 C63 Na3 79.42(14) . . . . ? Zn2 N14 C63 Na3 -97.94(13) . . . . ? C61 C62 C63 N14 -0.7(3) . . . . ? Na3 C62 C63 N14 70.40(16) . . . . ? C61 C62 C63 Na3 -71.15(18) . . . . ? N11 Na3 C63 N14 -81.57(15) . . . . ? N13 Na3 C63 N14 154.89(13) . . . . ? N12 Na3 C63 N14 95.2(2) . . . . ? C60 Na3 C63 N14 -39.16(12) . . . . ? C62 Na3 C63 N14 -112.8(2) . . . . ? C61 Na3 C63 N14 -76.89(14) . . . . ? Zn2 Na3 C63 N14 34.96(10) . . . . ? N11 Na3 C63 C62 31.3(2) . . . . ? N13 Na3 C63 C62 -92.28(16) . . . . ? N12 Na3 C63 C62 -152.02(19) . . . . ? N14 Na3 C63 C62 112.8(2) . . . . ? C60 Na3 C63 C62 73.67(16) . . . . ? C61 Na3 C63 C62 35.94(14) . . . . ? Zn2 Na3 C63 C62 147.80(18) . . . . ? N17 Zn2 N15 C67 -12.3(2) . . . . ? N16 Zn2 N15 C67 -132.53(18) . . . . ? N14 Zn2 N15 C67 104.24(19) . . . . ? Na3 Zn2 N15 C67 66.80(18) . . . . ? N17 Zn2 N15 C64 173.0(2) . . . . ? N16 Zn2 N15 C64 52.7(2) . . . . ? N14 Zn2 N15 C64 -70.5(2) . . . . ? Na3 Zn2 N15 C64 -107.9(2) . . . . ? C67 N15 C64 C65 -0.3(3) . . . . ? Zn2 N15 C64 C65 175.09(17) . . . . ? N15 C64 C65 C66 0.4(3) . . . . ? C64 C65 C66 C67 -0.3(3) . . . . ? C64 N15 C67 C66 0.1(3) . . . . ? Zn2 N15 C67 C66 -175.86(17) . . . . ? C65 C66 C67 N15 0.2(3) . . . . ? N17 Zn2 N16 C68 -143.07(17) . . . . ? N15 Zn2 N16 C68 -25.40(19) . . . . ? N14 Zn2 N16 C68 93.87(18) . . . . ? Na3 Zn2 N16 C68 93.9(2) . . . . ? N17 Zn2 N16 C71 37.85(19) . . . . ? N15 Zn2 N16 C71 155.52(16) . . . . ? N14 Zn2 N16 C71 -85.21(18) . . . . ? Na3 Zn2 N16 C71 -85.2(2) . . . . ? N17 Zn2 N16 Na4 -47.59(10) . . . . ? N15 Zn2 N16 Na4 70.08(9) . . . . ? N14 Zn2 N16 Na4 -170.65(7) . . . . ? Na3 Zn2 N16 Na4 -170.62(9) . . . . ? C71 N16 C68 C69 -0.9(2) . . . . ? Zn2 N16 C68 C69 179.89(14) . . . . ? Na4 N16 C68 C69 71.76(17) . . . . ? C71 N16 C68 Na4 -72.63(13) . . . . ? Zn2 N16 C68 Na4 108.13(14) . . . . ? N16 C68 C69 C70 0.6(3) . . . . ? Na4 C68 C69 C70 63.58(17) . . . . ? N16 C68 C69 Na4 -63.02(15) . . . . ? C68 C69 C70 C71 0.0(3) . . . . ? Na4 C69 C70 C71 62.83(16) . . . . ? C68 C69 C70 Na4 -62.84(16) . . . . ? C69 C70 C71 N16 -0.5(3) . . . . ? Na4 C70 C71 N16 71.24(15) . . . . ? C69 C70 C71 Na4 -71.78(17) . . . . ? C68 N16 C71 C70 0.9(2) . . . . ? Zn2 N16 C71 C70 -179.90(15) . . . . ? Na4 N16 C71 C70 -77.54(17) . . . . ? C68 N16 C71 Na4 78.41(14) . . . . ? Zn2 N16 C71 Na4 -102.35(14) . . . . ? N15 Zn2 N17 C72 125.2(2) . . . . ? N16 Zn2 N17 C72 -115.3(2) . . . . ? N14 Zn2 N17 C72 10.2(2) . . . . ? Na3 Zn2 N17 C72 46.1(2) . . . . ? N15 Zn2 N17 C75 -45.7(2) . . . . ? N16 Zn2 N17 C75 73.7(2) . . . . ? N14 Zn2 N17 C75 -160.7(2) . . . . ? Na3 Zn2 N17 C75 -124.8(2) . . . . ? C75 N17 C72 C73 -0.7(3) . . . . ? Zn2 N17 C72 C73 -173.06(18) . . . . ? N17 C72 C73 C74 0.7(3) . . . . ? C72 C73 C74 C75 -0.3(3) . . . . ? C72 N17 C75 C74 0.5(3) . . . . ? Zn2 N17 C75 C74 173.15(18) . . . . ? C73 C74 C75 N17 -0.1(3) . . . . ? C68 N16 Na4 N19 -36.37(19) . . . . ? C71 N16 Na4 N19 71.73(18) . . . . ? Zn2 N16 Na4 N19 -163.15(10) . . . . ? C68 N16 Na4 N18 60.26(15) . . . . ? C71 N16 Na4 N18 168.36(14) . . . . ? Zn2 N16 Na4 N18 -66.52(10) . . . . ? C68 N16 Na4 N20 -153.48(14) . . . . ? C71 N16 Na4 N20 -45.38(16) . . . . ? Zn2 N16 Na4 N20 79.74(11) . . . . ? C68 N16 Na4 C71 -108.10(19) . . . . ? Zn2 N16 Na4 C71 125.12(17) . . . . ? C71 N16 Na4 C68 108.10(19) . . . . ? Zn2 N16 Na4 C68 -126.78(16) . . . . ? C68 N16 Na4 C70 -72.19(14) . . . . ? C71 N16 Na4 C70 35.91(14) . . . . ? Zn2 N16 Na4 C70 161.03(13) . . . . ? C68 N16 Na4 C69 -34.27(13) . . . . ? C71 N16 Na4 C69 73.83(15) . . . . ? Zn2 N16 Na4 C69 -161.05(13) . . . . ? C70 C71 Na4 N19 -21.8(2) . . . . ? N16 C71 Na4 N19 -135.26(14) . . . . ? C70 C71 Na4 N18 95.75(19) . . . . ? N16 C71 Na4 N18 -17.7(2) . . . . ? C70 C71 Na4 N20 -103.00(16) . . . . ? N16 C71 Na4 N20 143.57(14) . . . . ? C70 C71 Na4 N16 113.4(2) . . . . ? C70 C71 Na4 C68 74.71(17) . . . . ? N16 C71 Na4 C68 -38.72(12) . . . . ? N16 C71 Na4 C70 -113.4(2) . . . . ? C70 C71 Na4 C69 36.74(15) . . . . ? N16 C71 Na4 C69 -76.69(14) . . . . ? N16 C68 Na4 N19 156.52(13) . . . . ? C69 C68 Na4 N19 40.34(17) . . . . ? N16 C68 Na4 N18 -126.49(13) . . . . ? C69 C68 Na4 N18 117.33(15) . . . . ? N16 C68 Na4 N20 45.1(2) . . . . ? C69 C68 Na4 N20 -71.1(2) . . . . ? C69 C68 Na4 N16 -116.2(2) . . . . ? N16 C68 Na4 C71 40.75(13) . . . . ? C69 C68 Na4 C71 -75.42(16) . . . . ? N16 C68 Na4 C70 80.43(14) . . . . ? C69 C68 Na4 C70 -35.74(14) . . . . ? N16 C68 Na4 C69 116.2(2) . . . . ? C71 C70 Na4 N19 162.53(16) . . . . ? C69 C70 Na4 N19 -85.13(15) . . . . ? C71 C70 Na4 N18 -118.06(17) . . . . ? C69 C70 Na4 N18 -5.7(2) . . . . ? C71 C70 Na4 N20 84.61(17) . . . . ? C69 C70 Na4 N20 -163.05(15) . . . . ? C71 C70 Na4 N16 -37.98(14) . . . . ? C69 C70 Na4 N16 74.36(15) . . . . ? C69 C70 Na4 C71 112.3(2) . . . . ? C71 C70 Na4 C68 -77.29(16) . . . . ? C69 C70 Na4 C68 35.05(14) . . . . ? C71 C70 Na4 C69 -112.3(2) . . . . ? C68 C69 Na4 N19 -145.18(15) . . . . ? C70 C69 Na4 N19 99.27(15) . . . . ? C68 C69 Na4 N18 -68.60(16) . . . . ? C70 C69 Na4 N18 175.85(15) . . . . ? C68 C69 Na4 N20 138.09(15) . . . . ? C70 C69 Na4 N20 22.54(19) . . . . ? C68 C69 Na4 N16 36.07(13) . . . . ? C70 C69 Na4 N16 -79.48(15) . . . . ? C68 C69 Na4 C71 77.85(16) . . . . ? C70 C69 Na4 C71 -37.70(14) . . . . ? C70 C69 Na4 C68 -115.5(2) . . . . ? C68 C69 Na4 C70 115.5(2) . . . . ? N19 Na4 N18 C81 105.0(2) . . . . ? N20 Na4 N18 C81 171.6(2) . . . . ? N16 Na4 N18 C81 -37.8(2) . . . . ? C71 Na4 N18 C81 -28.3(3) . . . . ? C68 Na4 N18 C81 -13.0(2) . . . . ? C70 Na4 N18 C81 15.2(3) . . . . ? C69 Na4 N18 C81 12.4(2) . . . . ? N19 Na4 N18 C80 -132.1(7) . . . . ? N20 Na4 N18 C80 -65.4(7) . . . . ? N16 Na4 N18 C80 85.1(7) . . . . ? C71 Na4 N18 C80 94.7(7) . . . . ? C68 Na4 N18 C80 109.9(7) . . . . ? C70 Na4 N18 C80 138.2(7) . . . . ? C69 Na4 N18 C80 135.4(7) . . . . ? N19 Na4 N18 C80A -123(4) . . . . ? N20 Na4 N18 C80A -56(4) . . . . ? N16 Na4 N18 C80A 95(4) . . . . ? C71 Na4 N18 C80A 104(4) . . . . ? C68 Na4 N18 C80A 119(4) . . . . ? C70 Na4 N18 C80A 148(4) . . . . ? C69 Na4 N18 C80A 145(4) . . . . ? N19 Na4 N18 C81A 122.4(18) . . . . ? N20 Na4 N18 C81A -170.9(18) . . . . ? N16 Na4 N18 C81A -20.4(18) . . . . ? C71 Na4 N18 C81A -10.9(18) . . . . ? C68 Na4 N18 C81A 4.4(18) . . . . ? C70 Na4 N18 C81A 32.6(18) . . . . ? C69 Na4 N18 C81A 29.8(18) . . . . ? N19 Na4 N18 C82 -15.30(18) . . . . ? N20 Na4 N18 C82 51.3(2) . . . . ? N16 Na4 N18 C82 -158.09(18) . . . . ? C71 Na4 N18 C82 -148.59(19) . . . . ? C68 Na4 N18 C82 -133.32(18) . . . . ? C70 Na4 N18 C82 -105.1(2) . . . . ? C69 Na4 N18 C82 -107.88(19) . . . . ? N19 Na4 N18 C82A 20.4(9) . . . . ? N20 Na4 N18 C82A 87.0(9) . . . . ? N16 Na4 N18 C82A -122.4(9) . . . . ? C71 Na4 N18 C82A -112.9(9) . . . . ? C68 Na4 N18 C82A -97.6(9) . . . . ? C70 Na4 N18 C82A -69.4(9) . . . . ? C69 Na4 N18 C82A -72.2(9) . . . . ? N18 Na4 N19 C85 110.23(16) . . . . ? N20 Na4 N19 C85 -8.98(15) . . . . ? N16 Na4 N19 C85 -140.49(16) . . . . ? C71 Na4 N19 C85 -103.80(17) . . . . ? C68 Na4 N19 C85 -159.40(15) . . . . ? C70 Na4 N19 C85 -114.17(16) . . . . ? C69 Na4 N19 C85 -142.04(16) . . . . ? N18 Na4 N19 C84 -129.8(2) . . . . ? N20 Na4 N19 C84 111.0(2) . . . . ? N16 Na4 N19 C84 -20.5(3) . . . . ? C71 Na4 N19 C84 16.2(2) . . . . ? C68 Na4 N19 C84 -39.4(2) . . . . ? C70 Na4 N19 C84 5.8(2) . . . . ? C69 Na4 N19 C84 -22.1(2) . . . . ? N18 Na4 N19 C83 -14.01(19) . . . . ? N20 Na4 N19 C83 -133.2(2) . . . . ? N16 Na4 N19 C83 95.3(2) . . . . ? C71 Na4 N19 C83 132.0(2) . . . . ? C68 Na4 N19 C83 76.4(2) . . . . ? C70 Na4 N19 C83 121.6(2) . . . . ? C69 Na4 N19 C83 93.7(2) . . . . ? N18 Na4 N19 C83A 16.3(10) . . . . ? N20 Na4 N19 C83A -102.9(10) . . . . ? N16 Na4 N19 C83A 125.6(10) . . . . ? C71 Na4 N19 C83A 162.3(10) . . . . ? C68 Na4 N19 C83A 106.7(10) . . . . ? C70 Na4 N19 C83A 151.9(10) . . . . ? C69 Na4 N19 C83A 124.0(10) . . . . ? N19 Na4 N20 C86 -20.26(15) . . . . ? N18 Na4 N20 C86 -86.66(17) . . . . ? N16 Na4 N20 C86 126.99(15) . . . . ? C71 Na4 N20 C86 105.64(16) . . . . ? C68 Na4 N20 C86 102.4(2) . . . . ? C70 Na4 N20 C86 76.61(17) . . . . ? C69 Na4 N20 C86 65.85(19) . . . . ? N19 Na4 N20 C88 -138.5(2) . . . . ? N18 Na4 N20 C88 155.09(19) . . . . ? N16 Na4 N20 C88 8.7(2) . . . . ? C71 Na4 N20 C88 -12.6(2) . . . . ? C68 Na4 N20 C88 -15.8(3) . . . . ? C70 Na4 N20 C88 -41.6(2) . . . . ? C69 Na4 N20 C88 -52.4(2) . . . . ? N19 Na4 N20 C87 99.02(17) . . . . ? N18 Na4 N20 C87 32.63(19) . . . . ? N16 Na4 N20 C87 -113.72(17) . . . . ? C71 Na4 N20 C87 -135.07(17) . . . . ? C68 Na4 N20 C87 -138.31(18) . . . . ? C70 Na4 N20 C87 -164.11(16) . . . . ? C69 Na4 N20 C87 -174.87(16) . . . . ? C81 N18 C82 C83 -70.2(5) . . . . ? C80 N18 C82 C83 169.0(6) . . . . ? C80A N18 C82 C83 161(3) . . . . ? C81A N18 C82 C83 -81(3) . . . . ? C82A N18 C82 C83 -54.2(13) . . . . ? Na4 N18 C82 C83 45.0(3) . . . . ? C85 N19 C83 C82 -76.4(3) . . . . ? C84 N19 C83 C82 162.3(3) . . . . ? C83A N19 C83 C82 -46.0(18) . . . . ? Na4 N19 C83 C82 42.8(3) . . . . ? N18 C82 C83 N19 -63.5(4) . . . . ? C81 N18 C82A C83A -155.0(12) . . . . ? C80 N18 C82A C83A 97.0(13) . . . . ? C80A N18 C82A C83A 85(4) . . . . ? C81A N18 C82A C83A -161(2) . . . . ? C82 N18 C82A C83A 39.8(10) . . . . ? Na4 N18 C82A C83A -51.2(12) . . . . ? C85 N19 C83A C82A -160.0(15) . . . . ? C84 N19 C83A C82A 84.3(17) . . . . ? C83 N19 C83A C82A 47.3(15) . . . . ? Na4 N19 C83A C82A -52.4(16) . . . . ? N18 C82A C83A N19 72.9(17) . . . . ? C84 N19 C85 C86 -83.4(3) . . . . ? C83 N19 C85 C86 157.2(2) . . . . ? C83A N19 C85 C86 142.9(9) . . . . ? Na4 N19 C85 C86 37.9(2) . . . . ? C88 N20 C86 C85 168.9(2) . . . . ? C87 N20 C86 C85 -70.5(3) . . . . ? Na4 N20 C86 C85 49.3(2) . . . . ? N19 C85 C86 N20 -64.3(3) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.703 _refine_diff_density_min -0.365 _refine_diff_density_rms 0.059 #===END #----------------------------------------------- #---------------COMPOUND 6---------------------- #----------------------------------------------- data_srjg1105 _database_code_depnum_ccdc_archive 'CCDC 837246' #TrackingRef '- combined.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H54 N8 Na2' _chemical_formula_sum 'C26 H54 N8 Na2' _chemical_formula_weight 524.75 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.3617(5) _cell_length_b 9.6380(4) _cell_length_c 18.0907(8) _cell_angle_alpha 90.00 _cell_angle_beta 100.702(5) _cell_angle_gamma 90.00 _cell_volume 1603.90(13) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 3025 _cell_measurement_theta_min 3.0551 _cell_measurement_theta_max 30.0546 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.087 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 576 _exptl_absorpt_coefficient_mu 0.090 _exptl_absorpt_correction_T_min 0.99422 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Eos' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8124 _diffrn_reflns_av_R_equivalents 0.0224 _diffrn_reflns_av_sigmaI/netI 0.0381 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.06 _diffrn_reflns_theta_max 28.00 _reflns_number_total 3864 _reflns_number_gt 2857 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _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^)+(0.0645P)^2^+0.9049P] 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 3864 _refine_ls_number_parameters 210 _refine_ls_number_restraints 116 _refine_ls_R_factor_all 0.0843 _refine_ls_R_factor_gt 0.0595 _refine_ls_wR_factor_ref 0.1589 _refine_ls_wR_factor_gt 0.1431 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.031 _refine_ls_shift/su_max 0.033 _refine_ls_shift/su_mean 0.003 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Na1 Na 0.94812(7) 0.38094(7) 0.05538(4) 0.0251(2) Uani 1 1 d U . . N1 N 0.93518(19) 0.63284(16) 0.05679(9) 0.0333(4) Uani 1 1 d . . . C1 C 0.8003(2) 0.6915(2) 0.04503(11) 0.0331(4) Uani 1 1 d . . . H1A H 0.7232 0.6653 0.0056 0.040 Uiso 1 1 calc R A . C2 C 0.7892(2) 0.79283(19) 0.09699(11) 0.0339(4) Uani 1 1 d . A . H2A H 0.7060 0.8476 0.0999 0.041 Uiso 1 1 calc R . . C3 C 0.9244(2) 0.7991(2) 0.14458(12) 0.0360(5) Uani 1 1 d . . . H3A H 0.9524 0.8590 0.1864 0.043 Uiso 1 1 calc R A . C4 C 1.0089(2) 0.7007(2) 0.11843(12) 0.0357(5) Uani 1 1 d . A . H4A H 1.1072 0.6821 0.1407 0.043 Uiso 1 1 calc R . . N2 N 1.137(3) 0.264(3) 0.1622(17) 0.0401(13) Uani 0.345(3) 1 d PDU A 1 N4 N 0.7246(12) 0.2391(13) 0.0176(6) 0.0297(10) Uani 0.345(3) 1 d PD A 1 C10 C 1.287(3) 0.317(3) 0.177(2) 0.063(2) Uani 0.345(3) 1 d PDU A 1 H10A H 1.3523 0.2480 0.2051 0.095 Uiso 0.345(3) 1 calc PR A 1 H10B H 1.2916 0.4031 0.2063 0.095 Uiso 0.345(3) 1 calc PR A 1 H10C H 1.3182 0.3363 0.1290 0.095 Uiso 0.345(3) 1 calc PR A 1 C11 C 1.130(3) 0.131(3) 0.1215(17) 0.059(2) Uani 0.345(3) 1 d PDU A 1 H11A H 1.1855 0.0610 0.1537 0.089 Uiso 0.345(3) 1 calc PR A 1 H11B H 1.1702 0.1431 0.0757 0.089 Uiso 0.345(3) 1 calc PR A 1 H11C H 1.0280 0.1019 0.1080 0.089 Uiso 0.345(3) 1 calc PR A 1 N3 N 0.8299(13) 0.3425(19) 0.1733(14) 0.0404(10) Uani 0.345(3) 1 d PDU A 1 C15 C 0.6777(7) 0.3055(7) 0.1430(3) 0.0392(7) Uani 0.345(3) 1 d PD A 1 H15A H 0.6248 0.3905 0.1231 0.047 Uiso 0.345(3) 1 calc PR A 1 H15B H 0.6326 0.2708 0.1848 0.047 Uiso 0.345(3) 1 calc PR A 1 C12 C 1.074(3) 0.291(2) 0.2295(14) 0.0610(17) Uani 0.345(3) 1 d PDU A 1 H12A H 1.0703 0.3924 0.2388 0.073 Uiso 0.345(3) 1 calc PR A 1 H12B H 1.1326 0.2467 0.2742 0.073 Uiso 0.345(3) 1 calc PR A 1 C13 C 0.923(3) 0.232(3) 0.2144(18) 0.0570(14) Uani 0.345(3) 1 d PDU A 1 H13A H 0.9189 0.1471 0.1835 0.068 Uiso 0.345(3) 1 calc PR A 1 H13B H 0.8909 0.2093 0.2622 0.068 Uiso 0.345(3) 1 calc PR A 1 C14 C 0.8357(15) 0.4751(13) 0.2140(7) 0.0522(13) Uani 0.345(3) 1 d PD A 1 H14A H 0.7858 0.5469 0.1804 0.078 Uiso 0.345(3) 1 calc PR A 1 H14B H 0.9374 0.5020 0.2312 0.078 Uiso 0.345(3) 1 calc PR A 1 H14C H 0.7878 0.4648 0.2574 0.078 Uiso 0.345(3) 1 calc PR A 1 C16 C 0.6578(8) 0.1974(7) 0.0814(4) 0.0395(7) Uani 0.345(3) 1 d PD A 1 H16A H 0.7016 0.1089 0.1023 0.047 Uiso 0.345(3) 1 calc PR A 1 H16B H 0.5526 0.1813 0.0635 0.047 Uiso 0.345(3) 1 calc PR A 1 C17 C 0.6307(12) 0.3411(12) -0.0285(4) 0.0417(8) Uani 0.345(3) 1 d PD A 1 H17A H 0.6688 0.3601 -0.0744 0.063 Uiso 0.345(3) 1 calc PR A 1 H17B H 0.6290 0.4272 0.0001 0.063 Uiso 0.345(3) 1 calc PR A 1 H17C H 0.5319 0.3038 -0.0420 0.063 Uiso 0.345(3) 1 calc PR A 1 C18 C 0.720(5) 0.117(3) -0.0314(19) 0.0555(18) Uani 0.345(3) 1 d PD A 1 H18A H 0.7669 0.0383 -0.0022 0.083 Uiso 0.345(3) 1 calc PR A 1 H18B H 0.7709 0.1374 -0.0728 0.083 Uiso 0.345(3) 1 calc PR A 1 H18C H 0.6183 0.0933 -0.0520 0.083 Uiso 0.345(3) 1 calc PR A 1 N3A N 0.8292(7) 0.3154(9) 0.1650(7) 0.0404(10) Uani 0.65 1 d PDU A 2 C11A C 1.1686(14) 0.1368(13) 0.1344(8) 0.059(2) Uani 0.65 1 d PDU A 2 H11D H 1.2398 0.0932 0.1742 0.089 Uiso 0.655(3) 1 calc PR A 2 H11E H 1.2085 0.1416 0.0881 0.089 Uiso 0.655(3) 1 calc PR A 2 H11F H 1.0791 0.0817 0.1254 0.089 Uiso 0.655(3) 1 calc PR A 2 C12A C 1.0842(14) 0.2589(11) 0.2288(7) 0.0610(17) Uani 0.65 1 d PDU A 2 H12C H 1.1367 0.1795 0.2561 0.073 Uiso 0.655(3) 1 calc PR A 2 H12D H 1.1114 0.3427 0.2598 0.073 Uiso 0.655(3) 1 calc PR A 2 C15A C 0.7038(4) 0.2232(4) 0.14247(18) 0.0392(7) Uani 0.65 1 d PD A 2 H15C H 0.6425 0.2246 0.1816 0.047 Uiso 0.655(3) 1 calc PR A 2 H15D H 0.7383 0.1270 0.1381 0.047 Uiso 0.655(3) 1 calc PR A 2 C16A C 0.6138(4) 0.2683(4) 0.06780(18) 0.0395(7) Uani 0.65 1 d PD A 2 H16C H 0.5297 0.2049 0.0546 0.047 Uiso 0.655(3) 1 calc PR A 2 H16D H 0.5755 0.3626 0.0734 0.047 Uiso 0.655(3) 1 calc PR A 2 C10A C 1.2741(16) 0.3545(11) 0.1724(10) 0.063(2) Uani 0.65 1 d PDU A 2 H10D H 1.3436 0.3070 0.2114 0.095 Uiso 0.655(3) 1 calc PR A 2 H10E H 1.2560 0.4482 0.1897 0.095 Uiso 0.655(3) 1 calc PR A 2 H10F H 1.3141 0.3605 0.1262 0.095 Uiso 0.655(3) 1 calc PR A 2 N2A N 1.1367(18) 0.2763(16) 0.1576(9) 0.0401(13) Uani 0.65 1 d PDU A 2 C18A C 0.733(3) 0.1301(14) -0.0173(9) 0.0555(18) Uani 0.65 1 d PD A 2 H18D H 0.7986 0.0853 0.0242 0.083 Uiso 0.655(3) 1 calc PR A 2 H18E H 0.7801 0.1374 -0.0610 0.083 Uiso 0.655(3) 1 calc PR A 2 H18F H 0.6438 0.0746 -0.0306 0.083 Uiso 0.655(3) 1 calc PR A 2 C17A C 0.6145(5) 0.3465(6) -0.0579(2) 0.0417(8) Uani 0.65 1 d PD A 2 H17D H 0.5228 0.2986 -0.0773 0.063 Uiso 0.655(3) 1 calc PR A 2 H17E H 0.6725 0.3526 -0.0977 0.063 Uiso 0.655(3) 1 calc PR A 2 H17F H 0.5939 0.4401 -0.0416 0.063 Uiso 0.655(3) 1 calc PR A 2 N4A N 0.6954(5) 0.2691(6) 0.0059(3) 0.0297(10) Uani 0.65 1 d PD A 2 C13A C 0.9280(15) 0.2356(17) 0.2235(8) 0.0570(14) Uani 0.65 1 d PDU A 2 H13C H 0.9028 0.2577 0.2730 0.068 Uiso 0.655(3) 1 calc PR A 2 H13D H 0.9085 0.1355 0.2141 0.068 Uiso 0.655(3) 1 calc PR A 2 C14A C 0.7881(7) 0.4467(6) 0.1941(3) 0.0522(13) Uani 0.65 1 d PD A 2 H14D H 0.7163 0.4930 0.1556 0.078 Uiso 0.655(3) 1 calc PR A 2 H14E H 0.8743 0.5058 0.2072 0.078 Uiso 0.655(3) 1 calc PR A 2 H14F H 0.7460 0.4302 0.2390 0.078 Uiso 0.655(3) 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Na1 0.0273(4) 0.0267(4) 0.0236(3) 0.0016(3) 0.0105(3) 0.0007(3) N1 0.0453(10) 0.0292(8) 0.0311(8) -0.0006(7) 0.0217(7) 0.0002(7) C1 0.0396(11) 0.0341(10) 0.0257(9) 0.0032(8) 0.0063(8) -0.0014(8) C2 0.0383(11) 0.0279(9) 0.0397(10) 0.0033(8) 0.0179(9) 0.0061(8) C3 0.0399(11) 0.0335(10) 0.0378(10) -0.0102(8) 0.0158(9) -0.0079(9) C4 0.0296(10) 0.0401(11) 0.0409(11) -0.0004(9) 0.0154(8) -0.0024(8) N2 0.0436(10) 0.052(3) 0.0266(19) 0.0103(19) 0.0117(12) 0.0179(16) N4 0.024(2) 0.038(3) 0.0281(19) -0.0001(15) 0.0068(18) 0.0000(16) C10 0.059(3) 0.084(7) 0.042(2) 0.008(5) -0.005(2) 0.005(4) C11 0.088(8) 0.0431(16) 0.053(5) 0.014(2) 0.031(4) 0.016(4) N3 0.0395(10) 0.061(4) 0.025(3) 0.002(2) 0.0165(10) -0.0039(15) C15 0.0449(17) 0.0344(16) 0.0450(15) 0.0071(16) 0.0260(13) 0.0001(15) C12 0.065(2) 0.091(5) 0.0308(12) 0.021(3) 0.0197(14) 0.040(3) C13 0.0736(19) 0.0689(18) 0.035(4) 0.016(2) 0.026(2) 0.0009(15) C14 0.078(4) 0.044(3) 0.045(3) -0.004(2) 0.038(3) -0.012(2) C16 0.0342(18) 0.047(2) 0.0419(16) -0.0011(16) 0.0195(14) -0.0059(14) C17 0.0359(18) 0.0598(17) 0.029(2) 0.000(2) 0.005(2) -0.0005(13) C18 0.072(4) 0.036(3) 0.066(6) -0.005(2) 0.030(5) -0.010(3) N3A 0.0395(10) 0.061(4) 0.025(3) 0.002(2) 0.0165(10) -0.0039(15) C11A 0.088(8) 0.0431(16) 0.053(5) 0.014(2) 0.031(4) 0.016(4) C12A 0.065(2) 0.091(5) 0.0308(12) 0.021(3) 0.0197(14) 0.040(3) C15A 0.0449(17) 0.0344(16) 0.0450(15) 0.0071(16) 0.0260(13) 0.0001(15) C16A 0.0342(18) 0.047(2) 0.0419(16) -0.0011(16) 0.0195(14) -0.0059(14) C10A 0.059(3) 0.084(7) 0.042(2) 0.008(5) -0.005(2) 0.005(4) N2A 0.0436(10) 0.052(3) 0.0266(19) 0.0103(19) 0.0117(12) 0.0179(16) C18A 0.072(4) 0.036(3) 0.066(6) -0.005(2) 0.030(5) -0.010(3) C17A 0.0359(18) 0.0598(17) 0.029(2) 0.000(2) 0.005(2) -0.0005(13) N4A 0.024(2) 0.038(3) 0.0281(19) -0.0001(15) 0.0068(18) 0.0000(16) C13A 0.0736(19) 0.0689(18) 0.035(4) 0.016(2) 0.026(2) 0.0009(15) C14A 0.078(4) 0.044(3) 0.045(3) -0.004(2) 0.038(3) -0.012(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 Na1 N1 2.4312(17) . ? Na1 N1 2.4803(15) 3_765 ? Na1 N4 2.487(14) . ? Na1 N2A 2.518(19) . ? Na1 N3A 2.528(13) . ? Na1 N4A 2.603(6) . ? Na1 N3 2.61(3) . ? Na1 N2 2.62(4) . ? Na1 Na1 3.3088(13) 3_765 ? N1 C1 1.363(3) . ? N1 C4 1.365(3) . ? N1 Na1 2.4803(15) 3_765 ? C1 C2 1.373(3) . ? C1 H1A 0.9500 . ? C2 C3 1.394(3) . ? C2 H2A 0.9500 . ? C3 C4 1.374(3) . ? C3 H3A 0.9500 . ? C4 H4A 0.9500 . ? N2 C11 1.468(9) . ? N2 C10 1.473(9) . ? N2 C12 1.475(9) . ? N4 C16 1.468(8) . ? N4 C17 1.470(8) . ? N4 C18 1.471(10) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? N3 C14 1.471(9) . ? N3 C15 1.472(9) . ? N3 C13 1.484(9) . ? C15 C16 1.511(7) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C12 C13 1.499(10) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? N3A C14A 1.449(6) . ? N3A C15A 1.469(6) . ? N3A C13A 1.485(7) . ? C11A N2A 1.456(7) . ? C11A H11D 0.9800 . ? C11A H11E 0.9800 . ? C11A H11F 0.9800 . ? C12A C13A 1.465(7) . ? C12A N2A 1.471(7) . ? C12A H12C 0.9900 . ? C12A H12D 0.9900 . ? C15A C16A 1.517(4) . ? C15A H15C 0.9900 . ? C15A H15D 0.9900 . ? C16A N4A 1.468(5) . ? C16A H16C 0.9900 . ? C16A H16D 0.9900 . ? C10A N2A 1.472(6) . ? C10A H10D 0.9800 . ? C10A H10E 0.9800 . ? C10A H10F 0.9800 . ? C18A N4A 1.465(8) . ? C18A H18D 0.9800 . ? C18A H18E 0.9800 . ? C18A H18F 0.9800 . ? C17A N4A 1.463(4) . ? C17A H17D 0.9800 . ? C17A H17E 0.9800 . ? C17A H17F 0.9800 . ? C13A H13C 0.9900 . ? C13A H13D 0.9900 . ? C14A H14D 0.9800 . ? C14A H14E 0.9800 . ? C14A H14F 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 Na1 N1 95.30(5) . 3_765 ? N1 Na1 N4 120.7(2) . . ? N1 Na1 N4 102.8(2) 3_765 . ? N1 Na1 N2A 114.9(3) . . ? N1 Na1 N2A 102.9(3) 3_765 . ? N4 Na1 N2A 114.9(4) . . ? N1 Na1 N3A 102.19(16) . . ? N1 Na1 N3A 162.44(16) 3_765 . ? N4 Na1 N3A 66.9(3) . . ? N2A Na1 N3A 71.0(3) . . ? N1 Na1 N4A 111.93(10) . . ? N1 Na1 N4A 101.94(11) 3_765 . ? N4 Na1 N4A 9.2(3) . . ? N2A Na1 N4A 123.7(4) . . ? N3A Na1 N4A 70.22(17) . . ? N1 Na1 N3 96.0(4) . . ? N1 Na1 N3 168.7(4) 3_765 . ? N4 Na1 N3 71.5(3) . . ? N2A Na1 N3 71.8(5) . . ? N3A Na1 N3 6.5(4) . . ? N4A Na1 N3 74.0(3) . . ? N1 Na1 N2 116.7(6) . . ? N1 Na1 N2 103.9(5) 3_765 . ? N4 Na1 N2 112.6(7) . . ? N2A Na1 N2 2.3(10) . . ? N3A Na1 N2 69.5(6) . . ? N4A Na1 N2 121.5(7) . . ? N3 Na1 N2 70.6(6) . . ? N1 Na1 Na1 48.28(4) . 3_765 ? N1 Na1 Na1 47.02(4) 3_765 3_765 ? N4 Na1 Na1 122.8(2) . 3_765 ? N2A Na1 Na1 118.5(3) . 3_765 ? N3A Na1 Na1 150.45(17) . 3_765 ? N4A Na1 Na1 115.44(9) . 3_765 ? N3 Na1 Na1 144.2(4) . 3_765 ? N2 Na1 Na1 120.7(6) . 3_765 ? C1 N1 C4 104.00(16) . . ? C1 N1 Na1 117.31(13) . . ? C4 N1 Na1 117.95(13) . . ? C1 N1 Na1 115.49(12) . 3_765 ? C4 N1 Na1 117.48(12) . 3_765 ? Na1 N1 Na1 84.70(5) . 3_765 ? N1 C1 C2 111.97(18) . . ? N1 C1 H1A 124.0 . . ? C2 C1 H1A 124.0 . . ? C1 C2 C3 106.12(17) . . ? C1 C2 H2A 126.9 . . ? C3 C2 H2A 126.9 . . ? C4 C3 C2 105.81(18) . . ? C4 C3 H3A 127.1 . . ? C2 C3 H3A 127.1 . . ? N1 C4 C3 112.10(18) . . ? N1 C4 H4A 123.9 . . ? C3 C4 H4A 123.9 . . ? C11 N2 C10 111(2) . . ? C11 N2 C12 125(3) . . ? C10 N2 C12 108(3) . . ? C11 N2 Na1 92.3(17) . . ? C10 N2 Na1 118(2) . . ? C12 N2 Na1 102.0(18) . . ? C16 N4 C17 109.4(8) . . ? C16 N4 C18 107(2) . . ? C17 N4 C18 104.2(17) . . ? C16 N4 Na1 113.2(8) . . ? C17 N4 Na1 99.9(8) . . ? C18 N4 Na1 122(2) . . ? C14 N3 C15 109.9(9) . . ? C14 N3 C13 114(2) . . ? C15 N3 C13 116.8(17) . . ? C14 N3 Na1 107.7(13) . . ? C15 N3 Na1 105.0(12) . . ? C13 N3 Na1 102.3(15) . . ? N3 C15 C16 114.8(8) . . ? N3 C15 H15A 108.6 . . ? C16 C15 H15A 108.6 . . ? N3 C15 H15B 108.6 . . ? C16 C15 H15B 108.6 . . ? H15A C15 H15B 107.5 . . ? N2 C12 C13 107(2) . . ? N2 C12 H12A 110.3 . . ? C13 C12 H12A 110.3 . . ? N2 C12 H12B 110.3 . . ? C13 C12 H12B 110.3 . . ? H12A C12 H12B 108.6 . . ? N3 C13 C12 105.3(18) . . ? N3 C13 H13A 110.7 . . ? C12 C13 H13A 110.7 . . ? N3 C13 H13B 110.7 . . ? C12 C13 H13B 110.7 . . ? H13A C13 H13B 108.8 . . ? N4 C16 C15 112.3(7) . . ? N4 C16 H16A 109.2 . . ? C15 C16 H16A 109.1 . . ? N4 C16 H16B 109.2 . . ? C15 C16 H16B 109.2 . . ? H16A C16 H16B 107.9 . . ? C14A N3A C15A 112.1(5) . . ? C14A N3A C13A 111.5(10) . . ? C15A N3A C13A 104.1(9) . . ? C14A N3A Na1 104.6(7) . . ? C15A N3A Na1 112.3(6) . . ? C13A N3A Na1 112.5(7) . . ? N2A C11A H11D 109.5 . . ? N2A C11A H11E 109.5 . . ? H11D C11A H11E 109.5 . . ? N2A C11A H11F 109.5 . . ? H11D C11A H11F 109.5 . . ? H11E C11A H11F 109.5 . . ? C13A C12A N2A 116.9(12) . . ? C13A C12A H12C 108.1 . . ? N2A C12A H12C 108.1 . . ? C13A C12A H12D 108.1 . . ? N2A C12A H12D 108.1 . . ? H12C C12A H12D 107.3 . . ? N3A C15A C16A 110.9(6) . . ? N3A C15A H15C 109.5 . . ? C16A C15A H15C 109.5 . . ? N3A C15A H15D 109.5 . . ? C16A C15A H15D 109.5 . . ? H15C C15A H15D 108.0 . . ? N4A C16A C15A 113.5(3) . . ? N4A C16A H16C 108.9 . . ? C15A C16A H16C 108.9 . . ? N4A C16A H16D 108.9 . . ? C15A C16A H16D 108.9 . . ? H16C C16A H16D 107.7 . . ? N2A C10A H10D 109.5 . . ? N2A C10A H10E 109.5 . . ? H10D C10A H10E 109.5 . . ? N2A C10A H10F 109.5 . . ? H10D C10A H10F 109.5 . . ? H10E C10A H10F 109.5 . . ? C11A N2A C12A 105.4(14) . . ? C11A N2A C10A 107.8(10) . . ? C12A N2A C10A 108.7(14) . . ? C11A N2A Na1 108.2(9) . . ? C12A N2A Na1 112.7(9) . . ? C10A N2A Na1 113.5(10) . . ? N4A C18A H18D 109.5 . . ? N4A C18A H18E 109.5 . . ? H18D C18A H18E 109.5 . . ? N4A C18A H18F 109.5 . . ? H18D C18A H18F 109.5 . . ? H18E C18A H18F 109.5 . . ? N4A C17A H17D 109.5 . . ? N4A C17A H17E 109.5 . . ? H17D C17A H17E 109.5 . . ? N4A C17A H17F 109.5 . . ? H17D C17A H17F 109.5 . . ? H17E C17A H17F 109.5 . . ? C17A N4A C18A 110.8(8) . . ? C17A N4A C16A 109.8(3) . . ? C18A N4A C16A 113.5(10) . . ? C17A N4A Na1 111.4(4) . . ? C18A N4A Na1 103.2(9) . . ? C16A N4A Na1 108.0(3) . . ? C12A C13A N3A 116.7(10) . . ? C12A C13A H13C 108.1 . . ? N3A C13A H13C 108.1 . . ? C12A C13A H13D 108.1 . . ? N3A C13A H13D 108.1 . . ? H13C C13A H13D 107.3 . . ? N3A C14A H14D 109.5 . . ? N3A C14A H14E 109.5 . . ? H14D C14A H14E 109.5 . . ? N3A C14A H14F 109.5 . . ? H14D C14A H14F 109.5 . . ? H14E C14A H14F 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 N1 Na1 N1 C1 116.01(14) 3_765 . . . ? N4 Na1 N1 C1 7.7(3) . . . . ? N2A Na1 N1 C1 -137.1(3) . . . . ? N3A Na1 N1 C1 -62.5(2) . . . . ? N4A Na1 N1 C1 10.86(18) . . . . ? N3 Na1 N1 C1 -64.3(3) . . . . ? N2 Na1 N1 C1 -135.5(6) . . . . ? Na1 Na1 N1 C1 116.01(14) 3_765 . . . ? N1 Na1 N1 C4 -118.38(15) 3_765 . . . ? N4 Na1 N1 C4 133.3(3) . . . . ? N2A Na1 N1 C4 -11.4(3) . . . . ? N3A Na1 N1 C4 63.1(2) . . . . ? N4A Na1 N1 C4 136.46(16) . . . . ? N3 Na1 N1 C4 61.3(3) . . . . ? N2 Na1 N1 C4 -9.9(6) . . . . ? Na1 Na1 N1 C4 -118.38(15) 3_765 . . . ? N1 Na1 N1 Na1 0.0 3_765 . . 3_765 ? N4 Na1 N1 Na1 -108.3(3) . . . 3_765 ? N2A Na1 N1 Na1 106.9(3) . . . 3_765 ? N3A Na1 N1 Na1 -178.52(18) . . . 3_765 ? N4A Na1 N1 Na1 -105.15(12) . . . 3_765 ? N3 Na1 N1 Na1 179.7(3) . . . 3_765 ? N2 Na1 N1 Na1 108.5(6) . . . 3_765 ? C4 N1 C1 C2 0.2(2) . . . . ? Na1 N1 C1 C2 132.46(14) . . . . ? Na1 N1 C1 C2 -130.01(14) 3_765 . . . ? N1 C1 C2 C3 0.0(2) . . . . ? C1 C2 C3 C4 -0.1(2) . . . . ? C1 N1 C4 C3 -0.3(2) . . . . ? Na1 N1 C4 C3 -132.18(15) . . . . ? Na1 N1 C4 C3 128.73(15) 3_765 . . . ? C2 C3 C4 N1 0.3(2) . . . . ? N1 Na1 N2 C11 -163.8(17) . . . . ? N1 Na1 N2 C11 -60.5(19) 3_765 . . . ? N4 Na1 N2 C11 50.1(19) . . . . ? N2A Na1 N2 C11 -126(19) . . . . ? N3A Na1 N2 C11 102.5(19) . . . . ? N4A Na1 N2 C11 53.2(19) . . . . ? N3 Na1 N2 C11 109.3(19) . . . . ? Na1 Na1 N2 C11 -108.4(18) 3_765 . . . ? N1 Na1 N2 C10 -49(2) . . . . ? N1 Na1 N2 C10 54(2) 3_765 . . . ? N4 Na1 N2 C10 164.9(18) . . . . ? N2A Na1 N2 C10 -11(18) . . . . ? N3A Na1 N2 C10 -143(2) . . . . ? N4A Na1 N2 C10 168.1(18) . . . . ? N3 Na1 N2 C10 -136(2) . . . . ? Na1 Na1 N2 C10 6(2) 3_765 . . . ? N1 Na1 N2 C12 69.2(18) . . . . ? N1 Na1 N2 C12 172.6(16) 3_765 . . . ? N4 Na1 N2 C12 -76.9(18) . . . . ? N2A Na1 N2 C12 107(20) . . . . ? N3A Na1 N2 C12 -24.5(15) . . . . ? N4A Na1 N2 C12 -73.8(18) . . . . ? N3 Na1 N2 C12 -17.7(16) . . . . ? Na1 Na1 N2 C12 124.6(16) 3_765 . . . ? N1 Na1 N4 C16 -92.5(6) . . . . ? N1 Na1 N4 C16 163.3(6) 3_765 . . . ? N2A Na1 N4 C16 52.2(7) . . . . ? N3A Na1 N4 C16 -1.7(6) . . . . ? N4A Na1 N4 C16 -111(2) . . . . ? N3 Na1 N4 C16 -6.6(7) . . . . ? N2 Na1 N4 C16 52.1(8) . . . . ? Na1 Na1 N4 C16 -150.0(5) 3_765 . . . ? N1 Na1 N4 C17 23.8(7) . . . . ? N1 Na1 N4 C17 -80.5(6) 3_765 . . . ? N2A Na1 N4 C17 168.5(6) . . . . ? N3A Na1 N4 C17 114.5(7) . . . . ? N4A Na1 N4 C17 5.1(16) . . . . ? N3 Na1 N4 C17 109.7(8) . . . . ? N2 Na1 N4 C17 168.3(7) . . . . ? Na1 Na1 N4 C17 -33.7(7) 3_765 . . . ? N1 Na1 N4 C18 137.7(18) . . . . ? N1 Na1 N4 C18 33.5(19) 3_765 . . . ? N2A Na1 N4 C18 -77.6(19) . . . . ? N3A Na1 N4 C18 -131.6(19) . . . . ? N4A Na1 N4 C18 119(3) . . . . ? N3 Na1 N4 C18 -136.4(19) . . . . ? N2 Na1 N4 C18 -77.7(19) . . . . ? Na1 Na1 N4 C18 80.2(19) 3_765 . . . ? N1 Na1 N3 C14 -16.8(10) . . . . ? N1 Na1 N3 C14 161.6(10) 3_765 . . . ? N4 Na1 N3 C14 -137.2(11) . . . . ? N2A Na1 N3 C14 97.6(10) . . . . ? N3A Na1 N3 C14 179(5) . . . . ? N4A Na1 N3 C14 -127.9(10) . . . . ? N2 Na1 N3 C14 99.5(11) . . . . ? Na1 Na1 N3 C14 -16.3(13) 3_765 . . . ? N1 Na1 N3 C15 100.3(8) . . . . ? N1 Na1 N3 C15 -81(2) 3_765 . . . ? N4 Na1 N3 C15 -20.1(8) . . . . ? N2A Na1 N3 C15 -145.3(10) . . . . ? N3A Na1 N3 C15 -64(4) . . . . ? N4A Na1 N3 C15 -10.8(7) . . . . ? N2 Na1 N3 C15 -143.4(11) . . . . ? Na1 Na1 N3 C15 100.8(7) 3_765 . . . ? N1 Na1 N3 C13 -137.3(13) . . . . ? N1 Na1 N3 C13 41(2) 3_765 . . . ? N4 Na1 N3 C13 102.3(13) . . . . ? N2A Na1 N3 C13 -22.9(13) . . . . ? N3A Na1 N3 C13 59(5) . . . . ? N4A Na1 N3 C13 111.6(13) . . . . ? N2 Na1 N3 C13 -21.0(14) . . . . ? Na1 Na1 N3 C13 -136.8(13) 3_765 . . . ? C14 N3 C15 C16 162.3(13) . . . . ? C13 N3 C15 C16 -66(2) . . . . ? Na1 N3 C15 C16 46.7(12) . . . . ? C11 N2 C12 C13 -45(4) . . . . ? C10 N2 C12 C13 -178(2) . . . . ? Na1 N2 C12 C13 56.5(19) . . . . ? C14 N3 C13 C12 -57(3) . . . . ? C15 N3 C13 C12 172.7(18) . . . . ? Na1 N3 C13 C12 59(2) . . . . ? N2 C12 C13 N3 -85(3) . . . . ? C17 N4 C16 C15 -77.4(12) . . . . ? C18 N4 C16 C15 170.5(18) . . . . ? Na1 N4 C16 C15 33.0(8) . . . . ? N3 C15 C16 N4 -57.0(15) . . . . ? N1 Na1 N3A C14A 0.9(4) . . . . ? N1 Na1 N3A C14A -174.3(4) 3_765 . . . ? N4 Na1 N3A C14A -117.6(5) . . . . ? N2A Na1 N3A C14A 113.3(5) . . . . ? N4A Na1 N3A C14A -108.3(5) . . . . ? N3 Na1 N3A C14A 17(4) . . . . ? N2 Na1 N3A C14A 115.1(8) . . . . ? Na1 Na1 N3A C14A -1.4(7) 3_765 . . . ? N1 Na1 N3A C15A 122.7(4) . . . . ? N1 Na1 N3A C15A -52.4(10) 3_765 . . . ? N4 Na1 N3A C15A 4.2(5) . . . . ? N2A Na1 N3A C15A -124.9(6) . . . . ? N4A Na1 N3A C15A 13.5(4) . . . . ? N3 Na1 N3A C15A 139(5) . . . . ? N2 Na1 N3A C15A -123.1(8) . . . . ? Na1 Na1 N3A C15A 120.4(3) 3_765 . . . ? N1 Na1 N3A C13A -120.2(7) . . . . ? N1 Na1 N3A C13A 64.6(10) 3_765 . . . ? N4 Na1 N3A C13A 121.3(8) . . . . ? N2A Na1 N3A C13A -7.8(8) . . . . ? N4A Na1 N3A C13A 130.6(7) . . . . ? N3 Na1 N3A C13A -104(5) . . . . ? N2 Na1 N3A C13A -6.0(9) . . . . ? Na1 Na1 N3A C13A -122.5(7) 3_765 . . . ? C14A N3A C15A C16A 76.5(10) . . . . ? C13A N3A C15A C16A -162.9(8) . . . . ? Na1 N3A C15A C16A -40.9(5) . . . . ? N3A C15A C16A N4A 59.3(5) . . . . ? C13A C12A N2A C11A -88.4(13) . . . . ? C13A C12A N2A C10A 156.2(11) . . . . ? C13A C12A N2A Na1 29.5(13) . . . . ? N1 Na1 N2A C11A -159.5(9) . . . . ? N1 Na1 N2A C11A -57.3(11) 3_765 . . . ? N4 Na1 N2A C11A 53.6(11) . . . . ? N3A Na1 N2A C11A 105.5(11) . . . . ? N4A Na1 N2A C11A 56.8(11) . . . . ? N3 Na1 N2A C11A 112.3(11) . . . . ? N2 Na1 N2A C11A 57(19) . . . . ? Na1 Na1 N2A C11A -105.2(10) 3_765 . . . ? N1 Na1 N2A C12A 84.3(10) . . . . ? N1 Na1 N2A C12A -173.5(9) 3_765 . . . ? N4 Na1 N2A C12A -62.5(10) . . . . ? N3A Na1 N2A C12A -10.7(9) . . . . ? N4A Na1 N2A C12A -59.4(10) . . . . ? N3 Na1 N2A C12A -3.9(9) . . . . ? N2 Na1 N2A C12A -59(19) . . . . ? Na1 Na1 N2A C12A 138.7(9) 3_765 . . . ? N1 Na1 N2A C10A -39.9(9) . . . . ? N1 Na1 N2A C10A 62.3(9) 3_765 . . . ? N4 Na1 N2A C10A 173.3(9) . . . . ? N3A Na1 N2A C10A -134.8(10) . . . . ? N4A Na1 N2A C10A 176.4(8) . . . . ? N3 Na1 N2A C10A -128.1(10) . . . . ? N2 Na1 N2A C10A 177(19) . . . . ? Na1 Na1 N2A C10A 14.5(10) 3_765 . . . ? C15A C16A N4A C17A -165.4(4) . . . . ? C15A C16A N4A C18A 70.0(10) . . . . ? C15A C16A N4A Na1 -43.8(4) . . . . ? N1 Na1 N4A C17A 40.5(4) . . . . ? N1 Na1 N4A C17A -60.3(3) 3_765 . . . ? N4 Na1 N4A C17A -157(2) . . . . ? N2A Na1 N4A C17A -174.9(4) . . . . ? N3A Na1 N4A C17A 136.1(4) . . . . ? N3 Na1 N4A C17A 130.6(5) . . . . ? N2 Na1 N4A C17A -174.9(6) . . . . ? Na1 Na1 N4A C17A -12.4(4) 3_765 . . . ? N1 Na1 N4A C18A 159.5(8) . . . . ? N1 Na1 N4A C18A 58.7(8) 3_765 . . . ? N4 Na1 N4A C18A -38(2) . . . . ? N2A Na1 N4A C18A -55.9(9) . . . . ? N3A Na1 N4A C18A -104.9(9) . . . . ? N3 Na1 N4A C18A -110.4(9) . . . . ? N2 Na1 N4A C18A -55.9(10) . . . . ? Na1 Na1 N4A C18A 106.6(8) 3_765 . . . ? N1 Na1 N4A C16A -80.1(2) . . . . ? N1 Na1 N4A C16A 179.1(2) 3_765 . . . ? N4 Na1 N4A C16A 83(2) . . . . ? N2A Na1 N4A C16A 64.5(4) . . . . ? N3A Na1 N4A C16A 15.5(3) . . . . ? N3 Na1 N4A C16A 10.0(5) . . . . ? N2 Na1 N4A C16A 64.5(6) . . . . ? Na1 Na1 N4A C16A -133.0(2) 3_765 . . . ? N2A C12A C13A N3A -38.7(17) . . . . ? C14A N3A C13A C12A -90.5(15) . . . . ? C15A N3A C13A C12A 148.4(10) . . . . ? Na1 N3A C13A C12A 26.6(14) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.714 _refine_diff_density_min -0.378 _refine_diff_density_rms 0.047 #===END