# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'R. E. Mulvey' _publ_contact_author_address ; Department of Pure & Applied Chemistry University of Strathclyde 295 Cathedral Street Glasgow G1 1XL UNITED KINGDOM ; _publ_contact_author_email R.E.MULVEY@STRATH.AC.UK _publ_section_title ; Structural variations in bimetallic sodium-magnesium and sodium-zinc ketimides, and a sodium-zinc alkide-alkoxide-amide: connections to ring-stacking, ring-laddering, and inverse crown concepts ; loop_ _publ_author_name R.E.Mulvey W.Clegg S.Dale D.V.Graham R.W.Harrington E.Hevia ; L.M.Hogg ; A.R.Kennedy data_dvgrem89_compound1 _database_code_depnum_ccdc_archive 'CCDC 631656' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C104 H82 Mg2 N8 Na2' _chemical_formula_sum 'C104 H82 Mg2 N8 Na2' _chemical_formula_weight 1538.38 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Mg Mg 0.0486 0.0363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.9334(3) _cell_length_b 13.9081(4) _cell_length_c 14.1940(4) _cell_angle_alpha 65.832(1) _cell_angle_beta 85.235(2) _cell_angle_gamma 65.586(1) _cell_volume 2109.69(10) _cell_formula_units_Z 1 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 8920 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.10 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.211 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 808 _exptl_absorpt_coefficient_mu 0.093 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 36668 _diffrn_reflns_av_R_equivalents 0.045 _diffrn_reflns_av_sigmaI/netI 0.0604 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.74 _diffrn_reflns_theta_max 27.12 _reflns_number_total 9261 _reflns_number_gt 6055 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'DENZO & COLLECT' _computing_cell_refinement 'DENZO & COLLECT' _computing_data_reduction 'DENZO & COLLECT' _computing_structure_solution SHELXS-97 _computing_structure_refinement SHELXL-97 _computing_molecular_graphics SHELXTL _computing_publication_material 'SHELXTL and local programs' _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^)+(0.0352P)^2^+0.6029P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9261 _refine_ls_number_parameters 527 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0894 _refine_ls_R_factor_gt 0.0457 _refine_ls_wR_factor_ref 0.1030 _refine_ls_wR_factor_gt 0.0872 _refine_ls_goodness_of_fit_ref 1.020 _refine_ls_restrained_S_all 1.020 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mg1 Mg 0.54893(4) 0.49803(4) 0.40164(4) 0.02223(13) Uani 1 1 d . . . Na1 Na 0.73648(6) 0.35417(6) 0.61293(5) 0.03469(18) Uani 1 1 d . . . N1 N 0.41990(11) 0.56373(12) 0.29476(11) 0.0273(3) Uani 1 1 d . . . N2 N 0.72229(11) 0.41886(11) 0.42723(10) 0.0251(3) Uani 1 1 d . . . N4 N 0.50195(10) 0.38380(11) 0.53031(10) 0.0229(3) Uani 1 1 d . . . C1 C 0.36732(13) 0.59894(14) 0.20814(13) 0.0252(4) Uani 1 1 d . . . C2 C 0.25422(14) 0.59188(15) 0.20118(13) 0.0282(4) Uani 1 1 d . . . C3 C 0.16773(14) 0.67248(16) 0.12090(15) 0.0343(4) Uani 1 1 d . . . H3 H 0.1802 0.7329 0.0652 0.041 Uiso 1 1 calc R . . C4 C 0.06321(16) 0.66585(19) 0.12103(18) 0.0447(5) Uani 1 1 d . . . H4 H 0.0048 0.7216 0.0658 0.054 Uiso 1 1 calc R . . C5 C 0.04468(17) 0.5785(2) 0.2011(2) 0.0527(6) Uani 1 1 d . . . H5 H -0.0269 0.5744 0.2015 0.063 Uiso 1 1 calc R . . C6 C 0.12953(18) 0.49685(19) 0.28090(19) 0.0502(6) Uani 1 1 d . . . H6 H 0.1167 0.4361 0.3357 0.060 Uiso 1 1 calc R . . C7 C 0.23380(16) 0.50340(17) 0.28114(15) 0.0388(5) Uani 1 1 d . . . H7 H 0.2919 0.4470 0.3364 0.047 Uiso 1 1 calc R . . C8 C 0.41030(13) 0.65235(14) 0.10615(12) 0.0250(4) Uani 1 1 d . . . C9 C 0.40308(14) 0.62882(15) 0.02140(13) 0.0281(4) Uani 1 1 d . . . H9 H 0.3674 0.5797 0.0260 0.034 Uiso 1 1 calc R . . C10 C 0.44724(14) 0.67603(15) -0.07014(13) 0.0324(4) Uani 1 1 d . . . H10 H 0.4433 0.6578 -0.1270 0.039 Uiso 1 1 calc R . . C11 C 0.49684(15) 0.74959(16) -0.07787(14) 0.0355(4) Uani 1 1 d . . . H11 H 0.5257 0.7835 -0.1407 0.043 Uiso 1 1 calc R . . C12 C 0.50453(15) 0.77396(16) 0.00588(14) 0.0366(4) Uani 1 1 d . . . H12 H 0.5391 0.8242 0.0005 0.044 Uiso 1 1 calc R . . C13 C 0.46209(14) 0.72539(15) 0.09759(14) 0.0306(4) Uani 1 1 d . . . H13 H 0.4683 0.7420 0.1550 0.037 Uiso 1 1 calc R . . C14 C 0.81558(13) 0.38339(13) 0.38889(13) 0.0227(4) Uani 1 1 d . . . C15 C 0.82369(13) 0.40530(13) 0.27543(13) 0.0233(4) Uani 1 1 d . . . C16 C 0.72476(14) 0.45847(16) 0.20825(14) 0.0336(4) Uani 1 1 d . . . H16 H 0.6529 0.4755 0.2354 0.040 Uiso 1 1 calc R . . C17 C 0.72841(15) 0.48709(16) 0.10333(14) 0.0380(5) Uani 1 1 d . . . H17 H 0.6594 0.5243 0.0592 0.046 Uiso 1 1 calc R . . C18 C 0.83198(15) 0.46203(16) 0.06192(14) 0.0355(4) Uani 1 1 d . . . H18 H 0.8346 0.4819 -0.0105 0.043 Uiso 1 1 calc R . . C19 C 0.93099(15) 0.40801(16) 0.12693(14) 0.0354(4) Uani 1 1 d . . . H19 H 1.0026 0.3900 0.0993 0.043 Uiso 1 1 calc R . . C20 C 0.92719(14) 0.37960(15) 0.23258(14) 0.0297(4) Uani 1 1 d . . . H20 H 0.9965 0.3419 0.2764 0.036 Uiso 1 1 calc R . . C21 C 0.92736(13) 0.31829(14) 0.45813(13) 0.0266(4) Uani 1 1 d . . . C22 C 0.99860(16) 0.20400(17) 0.47718(15) 0.0427(5) Uani 1 1 d . . . H22 H 0.9797 0.1660 0.4435 0.051 Uiso 1 1 calc R . . C23 C 1.09781(17) 0.14474(19) 0.54560(17) 0.0550(6) Uani 1 1 d . . . H23 H 1.1453 0.0661 0.5591 0.066 Uiso 1 1 calc R . . C24 C 1.12743(17) 0.1991(2) 0.59363(16) 0.0510(6) Uani 1 1 d . . . H24 H 1.1962 0.1590 0.6387 0.061 Uiso 1 1 calc R . . C25 C 1.05726(16) 0.31169(19) 0.57620(16) 0.0459(5) Uani 1 1 d . . . H25 H 1.0768 0.3493 0.6100 0.055 Uiso 1 1 calc R . . C26 C 0.95743(15) 0.37076(16) 0.50912(14) 0.0355(4) Uani 1 1 d . . . H26 H 0.9090 0.4485 0.4981 0.043 Uiso 1 1 calc R . . N3 N 0.77149(14) 0.15109(14) 0.69629(13) 0.0430(4) Uani 1 1 d . . . C27 C 0.83865(15) 0.04371(16) 0.74607(14) 0.0340(4) Uani 1 1 d . . . C28 C 0.95450(14) 0.01059(15) 0.79006(13) 0.0311(4) Uani 1 1 d . . . C29 C 1.04181(14) -0.09792(15) 0.80715(14) 0.0326(4) Uani 1 1 d . . . H29 H 1.0263 -0.1511 0.7913 0.039 Uiso 1 1 calc R . . C30 C 1.15046(15) -0.12892(16) 0.84678(14) 0.0376(5) Uani 1 1 d . . . H30 H 1.2093 -0.2027 0.8572 0.045 Uiso 1 1 calc R . . C31 C 1.17377(17) -0.05358(18) 0.87115(16) 0.0459(5) Uani 1 1 d . . . H31 H 1.2483 -0.0753 0.8990 0.055 Uiso 1 1 calc R . . C32 C 1.08832(18) 0.05376(19) 0.85498(18) 0.0540(6) Uani 1 1 d . . . H32 H 1.1044 0.1060 0.8717 0.065 Uiso 1 1 calc R . . C33 C 0.97936(16) 0.08615(17) 0.81457(16) 0.0441(5) Uani 1 1 d . . . H33 H 0.9213 0.1605 0.8036 0.053 Uiso 1 1 calc R . . C34 C 0.80627(14) -0.05259(16) 0.76167(16) 0.0371(5) Uani 1 1 d . . . C35 C 0.78680(15) -0.07177(18) 0.67735(18) 0.0461(5) Uani 1 1 d . . . H35 H 0.7921 -0.0220 0.6091 0.055 Uiso 1 1 calc R . . C36 C 0.75961(16) -0.1635(2) 0.6927(2) 0.0574(7) Uani 1 1 d . . . H36 H 0.7485 -0.1777 0.6351 0.069 Uiso 1 1 calc R . . C37 C 0.74880(18) -0.2340(2) 0.7913(3) 0.0649(7) Uani 1 1 d . . . H37 H 0.7290 -0.2959 0.8014 0.078 Uiso 1 1 calc R . . C38 C 0.76651(17) -0.2152(2) 0.8754(2) 0.0587(6) Uani 1 1 d . . . H38 H 0.7581 -0.2636 0.9431 0.070 Uiso 1 1 calc R . . C39 C 0.79672(16) -0.12536(17) 0.86129(18) 0.0463(5) Uani 1 1 d . . . H39 H 0.8108 -0.1137 0.9196 0.056 Uiso 1 1 calc R . . C40 C 0.49350(13) 0.28983(13) 0.54975(12) 0.0223(4) Uani 1 1 d . . . C41 C 0.44153(13) 0.23327(14) 0.64459(13) 0.0239(4) Uani 1 1 d . . . C42 C 0.49096(15) 0.11416(14) 0.70323(13) 0.0309(4) Uani 1 1 d . . . H42 H 0.5540 0.0663 0.6801 0.037 Uiso 1 1 calc R . . C43 C 0.44945(17) 0.06422(16) 0.79513(15) 0.0401(5) Uani 1 1 d . . . H43 H 0.4854 -0.0172 0.8352 0.048 Uiso 1 1 calc R . . C44 C 0.35627(17) 0.13211(17) 0.82870(15) 0.0410(5) Uani 1 1 d . . . H44 H 0.3279 0.0978 0.8917 0.049 Uiso 1 1 calc R . . C45 C 0.30444(16) 0.25053(17) 0.76997(15) 0.0394(5) Uani 1 1 d . . . H45 H 0.2394 0.2976 0.7919 0.047 Uiso 1 1 calc R . . C46 C 0.34726(14) 0.30056(15) 0.67922(14) 0.0321(4) Uani 1 1 d . . . H46 H 0.3117 0.3821 0.6399 0.039 Uiso 1 1 calc R . . C47 C 0.53781(13) 0.22491(13) 0.48149(12) 0.0242(4) Uani 1 1 d . . . C48 C 0.48047(15) 0.16978(15) 0.45981(14) 0.0319(4) Uani 1 1 d . . . H48 H 0.4126 0.1696 0.4910 0.038 Uiso 1 1 calc R . . C49 C 0.52114(16) 0.11507(16) 0.39320(15) 0.0381(5) Uani 1 1 d . . . H49 H 0.4806 0.0784 0.3787 0.046 Uiso 1 1 calc R . . C50 C 0.62002(16) 0.11355(15) 0.34792(14) 0.0364(4) Uani 1 1 d . . . H50 H 0.6477 0.0758 0.3025 0.044 Uiso 1 1 calc R . . C51 C 0.67842(16) 0.16714(15) 0.36904(14) 0.0347(4) Uani 1 1 d . . . H51 H 0.7467 0.1663 0.3382 0.042 Uiso 1 1 calc R . . C52 C 0.63748(14) 0.22226(14) 0.43522(13) 0.0300(4) Uani 1 1 d . . . H52 H 0.6783 0.2589 0.4492 0.036 Uiso 1 1 calc R . . H1N H 0.7022(19) 0.1587(19) 0.6756(17) 0.060(7) 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 Mg1 0.0200(3) 0.0227(3) 0.0210(3) -0.0072(2) 0.0040(2) -0.0083(2) Na1 0.0325(4) 0.0336(4) 0.0269(4) -0.0093(3) 0.0036(3) -0.0069(3) N1 0.0266(8) 0.0250(7) 0.0249(8) -0.0079(6) 0.0013(6) -0.0080(6) N2 0.0235(7) 0.0206(7) 0.0287(8) -0.0086(6) 0.0037(6) -0.0087(6) N4 0.0192(7) 0.0204(7) 0.0240(7) -0.0063(6) 0.0001(6) -0.0062(6) C1 0.0241(9) 0.0231(9) 0.0255(9) -0.0092(7) 0.0026(7) -0.0082(7) C2 0.0259(9) 0.0334(10) 0.0310(10) -0.0184(8) 0.0075(8) -0.0132(8) C3 0.0263(10) 0.0435(11) 0.0368(11) -0.0226(9) 0.0049(8) -0.0125(9) C4 0.0265(10) 0.0558(13) 0.0598(14) -0.0372(12) 0.0030(9) -0.0111(10) C5 0.0318(12) 0.0682(16) 0.0866(18) -0.0547(15) 0.0216(12) -0.0273(12) C6 0.0503(13) 0.0536(14) 0.0663(15) -0.0323(12) 0.0265(12) -0.0359(12) C7 0.0387(11) 0.0417(11) 0.0421(12) -0.0192(10) 0.0103(9) -0.0217(9) C8 0.0207(8) 0.0238(9) 0.0231(9) -0.0060(7) -0.0014(7) -0.0056(7) C9 0.0235(9) 0.0294(9) 0.0277(10) -0.0104(8) 0.0006(7) -0.0087(8) C10 0.0277(10) 0.0377(10) 0.0226(9) -0.0098(8) -0.0010(7) -0.0073(8) C11 0.0300(10) 0.0382(11) 0.0246(10) -0.0020(9) 0.0030(8) -0.0128(9) C12 0.0376(11) 0.0351(10) 0.0329(11) -0.0049(9) 0.0007(8) -0.0199(9) C13 0.0320(10) 0.0306(10) 0.0259(9) -0.0065(8) -0.0002(7) -0.0147(8) C14 0.0207(8) 0.0195(8) 0.0273(9) -0.0099(7) 0.0038(7) -0.0080(7) C15 0.0219(8) 0.0198(8) 0.0278(9) -0.0102(7) 0.0043(7) -0.0082(7) C16 0.0226(9) 0.0431(11) 0.0340(11) -0.0213(9) 0.0042(8) -0.0076(8) C17 0.0300(10) 0.0438(11) 0.0335(11) -0.0198(9) -0.0040(8) -0.0043(9) C18 0.0402(11) 0.0363(10) 0.0264(10) -0.0149(9) 0.0044(8) -0.0110(9) C19 0.0299(10) 0.0418(11) 0.0336(11) -0.0177(9) 0.0098(8) -0.0133(9) C20 0.0225(9) 0.0330(10) 0.0314(10) -0.0123(8) 0.0021(7) -0.0104(8) C21 0.0197(8) 0.0295(9) 0.0249(9) -0.0093(8) 0.0045(7) -0.0075(7) C22 0.0384(11) 0.0374(11) 0.0411(12) -0.0193(10) -0.0064(9) -0.0007(9) C23 0.0417(12) 0.0427(12) 0.0490(13) -0.0175(11) -0.0116(10) 0.0126(10) C24 0.0326(11) 0.0641(15) 0.0375(12) -0.0185(11) -0.0082(9) -0.0033(11) C25 0.0390(12) 0.0560(14) 0.0419(12) -0.0192(11) -0.0046(9) -0.0186(11) C26 0.0304(10) 0.0364(11) 0.0371(11) -0.0143(9) -0.0001(8) -0.0117(9) N3 0.0312(9) 0.0342(10) 0.0506(11) -0.0102(8) -0.0081(8) -0.0069(8) C27 0.0298(10) 0.0320(10) 0.0336(10) -0.0123(9) 0.0019(8) -0.0078(8) C28 0.0288(10) 0.0296(10) 0.0284(10) -0.0077(8) 0.0011(8) -0.0102(8) C29 0.0311(10) 0.0299(10) 0.0321(10) -0.0107(8) 0.0024(8) -0.0104(8) C30 0.0298(10) 0.0339(10) 0.0374(11) -0.0088(9) 0.0010(8) -0.0079(9) C31 0.0318(11) 0.0462(12) 0.0506(13) -0.0132(11) -0.0094(9) -0.0123(10) C32 0.0503(13) 0.0463(13) 0.0674(16) -0.0254(12) -0.0138(11) -0.0165(11) C33 0.0373(11) 0.0331(11) 0.0543(13) -0.0178(10) -0.0098(10) -0.0054(9) C34 0.0186(9) 0.0335(10) 0.0530(13) -0.0175(10) -0.0017(8) -0.0045(8) C35 0.0276(10) 0.0457(12) 0.0656(15) -0.0299(12) 0.0025(10) -0.0087(9) C36 0.0269(11) 0.0604(15) 0.101(2) -0.0531(16) 0.0082(12) -0.0136(11) C37 0.0309(12) 0.0542(15) 0.124(2) -0.0488(17) 0.0195(14) -0.0211(11) C38 0.0351(12) 0.0484(14) 0.0869(19) -0.0222(13) 0.0176(12) -0.0201(11) C39 0.0321(11) 0.0427(12) 0.0598(14) -0.0164(11) 0.0051(10) -0.0164(10) C40 0.0174(8) 0.0206(8) 0.0239(9) -0.0056(7) -0.0025(7) -0.0060(7) C41 0.0216(8) 0.0240(9) 0.0264(9) -0.0082(7) 0.0001(7) -0.0114(7) C42 0.0322(10) 0.0240(9) 0.0314(10) -0.0074(8) 0.0015(8) -0.0108(8) C43 0.0493(12) 0.0293(10) 0.0334(11) -0.0019(9) 0.0035(9) -0.0195(10) C44 0.0497(12) 0.0479(12) 0.0328(11) -0.0118(10) 0.0135(9) -0.0337(11) C45 0.0355(11) 0.0433(12) 0.0483(12) -0.0228(10) 0.0185(9) -0.0232(9) C46 0.0280(9) 0.0277(9) 0.0396(11) -0.0111(9) 0.0064(8) -0.0139(8) C47 0.0261(9) 0.0180(8) 0.0222(9) -0.0040(7) -0.0010(7) -0.0072(7) C48 0.0299(10) 0.0336(10) 0.0339(10) -0.0142(9) 0.0022(8) -0.0143(8) C49 0.0440(12) 0.0373(11) 0.0380(11) -0.0189(9) -0.0036(9) -0.0167(9) C50 0.0430(11) 0.0311(10) 0.0280(10) -0.0132(9) -0.0013(8) -0.0072(9) C51 0.0368(10) 0.0289(10) 0.0324(10) -0.0120(8) 0.0080(8) -0.0097(8) C52 0.0303(10) 0.0240(9) 0.0333(10) -0.0105(8) 0.0042(8) -0.0106(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 Mg1 N1 1.9864(14) . ? Mg1 N2 2.0343(14) . ? Mg1 N4 2.0899(14) 2_666 ? Mg1 N4 2.1134(14) . ? Na1 N2 2.4069(15) . ? Na1 N3 2.4244(17) . ? Na1 N1 2.4467(15) 2_666 ? Na1 C1 2.9569(18) 2_666 ? Na1 C2 3.0475(18) 2_666 ? Na1 C7 3.082(2) 2_666 ? N1 C1 1.259(2) . ? N1 Na1 2.4467(15) 2_666 ? N2 C14 1.270(2) . ? N4 C40 1.2704(19) . ? N4 Mg1 2.0899(14) 2_666 ? C1 C8 1.511(2) . ? C1 C2 1.520(2) . ? C1 Na1 2.9569(18) 2_666 ? C2 C3 1.391(2) . ? C2 C7 1.396(2) . ? C2 Na1 3.0475(18) 2_666 ? C3 C4 1.392(2) . ? C3 H3 0.950 . ? C4 C5 1.375(3) . ? C4 H4 0.950 . ? C5 C6 1.378(3) . ? C5 H5 0.950 . ? C6 C7 1.389(3) . ? C6 H6 0.950 . ? C7 Na1 3.082(2) 2_666 ? C7 H7 0.950 . ? C8 C9 1.389(2) . ? C8 C13 1.394(2) . ? C9 C10 1.391(2) . ? C9 H9 0.950 . ? C10 C11 1.382(3) . ? C10 H10 0.950 . ? C11 C12 1.384(3) . ? C11 H11 0.950 . ? C12 C13 1.386(2) . ? C12 H12 0.950 . ? C13 H13 0.950 . ? C14 C15 1.514(2) . ? C14 C21 1.517(2) . ? C15 C16 1.392(2) . ? C15 C20 1.392(2) . ? C16 C17 1.377(2) . ? C16 H16 0.950 . ? C17 C18 1.383(2) . ? C17 H17 0.950 . ? C18 C19 1.374(2) . ? C18 H18 0.950 . ? C19 C20 1.388(2) . ? C19 H19 0.950 . ? C20 H20 0.950 . ? C21 C26 1.386(2) . ? C21 C22 1.388(2) . ? C22 C23 1.395(3) . ? C22 H22 0.950 . ? C23 C24 1.374(3) . ? C23 H23 0.950 . ? C24 C25 1.372(3) . ? C24 H24 0.950 . ? C25 C26 1.391(3) . ? C25 H25 0.950 . ? C26 H26 0.950 . ? N3 C27 1.284(2) . ? N3 H1N 0.92(2) . ? C27 C28 1.482(2) . ? C27 C34 1.491(3) . ? C28 C33 1.388(3) . ? C28 C29 1.396(2) . ? C29 C30 1.382(2) . ? C29 H29 0.950 . ? C30 C31 1.373(3) . ? C30 H30 0.950 . ? C31 C32 1.379(3) . ? C31 H31 0.950 . ? C32 C33 1.384(3) . ? C32 H32 0.950 . ? C33 H33 0.950 . ? C34 C35 1.391(3) . ? C34 C39 1.393(3) . ? C35 C36 1.390(3) . ? C35 H35 0.950 . ? C36 C37 1.378(4) . ? C36 H36 0.950 . ? C37 C38 1.377(4) . ? C37 H37 0.950 . ? C38 C39 1.393(3) . ? C38 H38 0.950 . ? C39 H39 0.950 . ? C40 C47 1.509(2) . ? C40 C41 1.517(2) . ? C41 C42 1.389(2) . ? C41 C46 1.392(2) . ? C42 C43 1.386(3) . ? C42 H42 0.950 . ? C43 C44 1.380(3) . ? C43 H43 0.950 . ? C44 C45 1.383(3) . ? C44 H44 0.950 . ? C45 C46 1.384(2) . ? C45 H45 0.950 . ? C46 H46 0.950 . ? C47 C48 1.391(2) . ? C47 C52 1.391(2) . ? C48 C49 1.388(2) . ? C48 H48 0.950 . ? C49 C50 1.379(3) . ? C49 H49 0.950 . ? C50 C51 1.379(3) . ? C50 H50 0.950 . ? C51 C52 1.386(2) . ? C51 H51 0.950 . ? C52 H52 0.950 . ? 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 Mg1 N2 142.49(6) . . ? N1 Mg1 N4 103.34(6) . 2_666 ? N2 Mg1 N4 105.59(6) . 2_666 ? N1 Mg1 N4 101.66(6) . . ? N2 Mg1 N4 101.85(5) . . ? N4 Mg1 N4 89.69(5) 2_666 . ? N2 Na1 N3 109.98(6) . . ? N2 Na1 N1 123.15(5) . 2_666 ? N3 Na1 N1 100.96(6) . 2_666 ? N2 Na1 C1 146.33(5) . 2_666 ? N3 Na1 C1 93.30(6) . 2_666 ? N1 Na1 C1 24.70(4) 2_666 2_666 ? N2 Na1 C2 147.97(5) . 2_666 ? N3 Na1 C2 101.87(6) . 2_666 ? N1 Na1 C2 50.87(5) 2_666 2_666 ? C1 Na1 C2 29.27(4) 2_666 2_666 ? N2 Na1 C7 122.18(5) . 2_666 ? N3 Na1 C7 126.13(6) . 2_666 ? N1 Na1 C7 62.05(5) 2_666 2_666 ? C1 Na1 C7 49.04(5) 2_666 2_666 ? C2 Na1 C7 26.31(5) 2_666 2_666 ? C1 N1 Mg1 159.68(12) . . ? C1 N1 Na1 100.97(10) . 2_666 ? Mg1 N1 Na1 98.68(6) . 2_666 ? C14 N2 Mg1 146.35(12) . . ? C14 N2 Na1 115.81(11) . . ? Mg1 N2 Na1 97.23(6) . . ? C40 N4 Mg1 135.18(12) . 2_666 ? C40 N4 Mg1 133.84(12) . . ? Mg1 N4 Mg1 90.31(5) 2_666 . ? N1 C1 C8 122.79(14) . . ? N1 C1 C2 120.96(15) . . ? C8 C1 C2 116.23(14) . . ? N1 C1 Na1 54.33(9) . 2_666 ? C8 C1 Na1 142.32(11) . 2_666 ? C2 C1 Na1 78.67(9) . 2_666 ? C3 C2 C7 118.15(16) . . ? C3 C2 C1 123.10(16) . . ? C7 C2 C1 118.69(15) . . ? C3 C2 Na1 117.95(11) . 2_666 ? C7 C2 Na1 78.21(11) . 2_666 ? C1 C2 Na1 72.06(9) . 2_666 ? C2 C3 C4 120.90(18) . . ? C2 C3 H3 119.5 . . ? C4 C3 H3 119.5 . . ? C5 C4 C3 119.91(19) . . ? C5 C4 H4 120.0 . . ? C3 C4 H4 120.0 . . ? C4 C5 C6 120.25(18) . . ? C4 C5 H5 119.9 . . ? C6 C5 H5 119.9 . . ? C5 C6 C7 120.0(2) . . ? C5 C6 H6 120.0 . . ? C7 C6 H6 120.0 . . ? C6 C7 C2 120.80(19) . . ? C6 C7 Na1 118.61(13) . 2_666 ? C2 C7 Na1 75.48(10) . 2_666 ? C6 C7 H7 119.6 . . ? C2 C7 H7 119.6 . . ? Na1 C7 H7 76.6 2_666 . ? C9 C8 C13 118.66(15) . . ? C9 C8 C1 122.45(15) . . ? C13 C8 C1 118.86(15) . . ? C8 C9 C10 121.03(16) . . ? C8 C9 H9 119.5 . . ? C10 C9 H9 119.5 . . ? C11 C10 C9 119.57(17) . . ? C11 C10 H10 120.2 . . ? C9 C10 H10 120.2 . . ? C10 C11 C12 120.04(17) . . ? C10 C11 H11 120.0 . . ? C12 C11 H11 120.0 . . ? C11 C12 C13 120.31(17) . . ? C11 C12 H12 119.8 . . ? C13 C12 H12 119.8 . . ? C12 C13 C8 120.37(17) . . ? C12 C13 H13 119.8 . . ? C8 C13 H13 119.8 . . ? N2 C14 C15 123.95(14) . . ? N2 C14 C21 119.40(15) . . ? C15 C14 C21 116.62(13) . . ? C16 C15 C20 117.19(16) . . ? C16 C15 C14 120.01(14) . . ? C20 C15 C14 122.73(14) . . ? C17 C16 C15 121.67(16) . . ? C17 C16 H16 119.2 . . ? C15 C16 H16 119.2 . . ? C16 C17 C18 120.35(17) . . ? C16 C17 H17 119.8 . . ? C18 C17 H17 119.8 . . ? C19 C18 C17 119.08(17) . . ? C19 C18 H18 120.5 . . ? C17 C18 H18 120.5 . . ? C18 C19 C20 120.53(16) . . ? C18 C19 H19 119.7 . . ? C20 C19 H19 119.7 . . ? C19 C20 C15 121.18(16) . . ? C19 C20 H20 119.4 . . ? C15 C20 H20 119.4 . . ? C26 C21 C22 118.21(16) . . ? C26 C21 C14 119.87(15) . . ? C22 C21 C14 121.81(16) . . ? C21 C22 C23 120.33(19) . . ? C21 C22 H22 119.8 . . ? C23 C22 H22 119.8 . . ? C24 C23 C22 120.57(19) . . ? C24 C23 H23 119.7 . . ? C22 C23 H23 119.7 . . ? C25 C24 C23 119.67(18) . . ? C25 C24 H24 120.2 . . ? C23 C24 H24 120.2 . . ? C24 C25 C26 120.0(2) . . ? C24 C25 H25 120.0 . . ? C26 C25 H25 120.0 . . ? C21 C26 C25 121.18(18) . . ? C21 C26 H26 119.4 . . ? C25 C26 H26 119.4 . . ? C27 N3 Na1 151.07(14) . . ? C27 N3 H1N 110.7(14) . . ? Na1 N3 H1N 97.9(14) . . ? N3 C27 C28 120.23(17) . . ? N3 C27 C34 122.86(16) . . ? C28 C27 C34 116.91(15) . . ? C33 C28 C29 118.36(16) . . ? C33 C28 C27 121.27(16) . . ? C29 C28 C27 120.37(16) . . ? C30 C29 C28 120.77(17) . . ? C30 C29 H29 119.6 . . ? C28 C29 H29 119.6 . . ? C31 C30 C29 120.28(18) . . ? C31 C30 H30 119.9 . . ? C29 C30 H30 119.9 . . ? C30 C31 C32 119.61(18) . . ? C30 C31 H31 120.2 . . ? C32 C31 H31 120.2 . . ? C31 C32 C33 120.65(19) . . ? C31 C32 H32 119.7 . . ? C33 C32 H32 119.7 . . ? C32 C33 C28 120.34(18) . . ? C32 C33 H33 119.8 . . ? C28 C33 H33 119.8 . . ? C35 C34 C39 119.29(19) . . ? C35 C34 C27 120.50(18) . . ? C39 C34 C27 120.21(18) . . ? C36 C35 C34 120.2(2) . . ? C36 C35 H35 119.9 . . ? C34 C35 H35 119.9 . . ? C37 C36 C35 120.1(2) . . ? C37 C36 H36 120.0 . . ? C35 C36 H36 120.0 . . ? C38 C37 C36 120.3(2) . . ? C38 C37 H37 119.8 . . ? C36 C37 H37 119.8 . . ? C37 C38 C39 120.1(2) . . ? C37 C38 H38 119.9 . . ? C39 C38 H38 119.9 . . ? C38 C39 C34 119.9(2) . . ? C38 C39 H39 120.0 . . ? C34 C39 H39 120.0 . . ? N4 C40 C47 122.12(14) . . ? N4 C40 C41 122.47(15) . . ? C47 C40 C41 115.39(13) . . ? C42 C41 C46 118.11(16) . . ? C42 C41 C40 121.14(15) . . ? C46 C41 C40 120.60(14) . . ? C43 C42 C41 120.86(17) . . ? C43 C42 H42 119.6 . . ? C41 C42 H42 119.6 . . ? C44 C43 C42 120.34(17) . . ? C44 C43 H43 119.8 . . ? C42 C43 H43 119.8 . . ? C43 C44 C45 119.50(17) . . ? C43 C44 H44 120.2 . . ? C45 C44 H44 120.2 . . ? C44 C45 C46 120.10(18) . . ? C44 C45 H45 119.9 . . ? C46 C45 H45 119.9 . . ? C45 C46 C41 121.05(16) . . ? C45 C46 H46 119.5 . . ? C41 C46 H46 119.5 . . ? C48 C47 C52 117.88(16) . . ? C48 C47 C40 122.36(15) . . ? C52 C47 C40 119.73(14) . . ? C49 C48 C47 120.82(17) . . ? C49 C48 H48 119.6 . . ? C47 C48 H48 119.6 . . ? C50 C49 C48 120.44(17) . . ? C50 C49 H49 119.8 . . ? C48 C49 H49 119.8 . . ? C49 C50 C51 119.55(18) . . ? C49 C50 H50 120.2 . . ? C51 C50 H50 120.2 . . ? C50 C51 C52 119.99(17) . . ? C50 C51 H51 120.0 . . ? C52 C51 H51 120.0 . . ? C51 C52 C47 121.32(16) . . ? C51 C52 H52 119.3 . . ? C47 C52 H52 119.3 . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.12 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.197 _refine_diff_density_min -0.203 _refine_diff_density_rms 0.042 #===END data_rem324_compound2 _database_code_depnum_ccdc_archive 'CCDC 631657' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C86 H80 N6 Na2 Zn2' _chemical_formula_sum 'C86 H80 N6 Na2 Zn2' _chemical_formula_weight 1374.28 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/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 13.2031(12) _cell_length_b 27.339(3) _cell_length_c 20.0914(18) _cell_angle_alpha 90.00 _cell_angle_beta 92.909(2) _cell_angle_gamma 90.00 _cell_volume 7242.8(11) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 7617 _cell_measurement_theta_min 2.41 _cell_measurement_theta_max 28.23 _exptl_crystal_description Block _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.58 _exptl_crystal_size_mid 0.53 _exptl_crystal_size_min 0.32 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.260 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2880 _exptl_absorpt_coefficient_mu 0.724 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.679 _exptl_absorpt_correction_T_max 0.801 _exptl_absorpt_process_details 'Bruker SHELXTL' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1K CCD diffractometer' _diffrn_measurement_method 'thin-slice \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 63519 _diffrn_reflns_av_R_equivalents 0.0285 _diffrn_reflns_av_sigmaI/netI 0.0275 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -34 _diffrn_reflns_limit_k_max 35 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.26 _diffrn_reflns_theta_max 27.50 _reflns_number_total 16561 _reflns_number_gt 14269 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL and local programs' _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^)+(0.0000P)^2^+34.2827P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 16561 _refine_ls_number_parameters 976 _refine_ls_number_restraints 551 _refine_ls_R_factor_all 0.0881 _refine_ls_R_factor_gt 0.0780 _refine_ls_wR_factor_ref 0.1850 _refine_ls_wR_factor_gt 0.1809 _refine_ls_goodness_of_fit_ref 1.328 _refine_ls_restrained_S_all 1.320 _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 0.58549(4) 0.188444(19) 0.84128(3) 0.02415(12) Uani 1 1 d . . . Zn2 Zn 0.58856(4) 0.197989(19) 0.68753(3) 0.02446(12) Uani 1 1 d . C . Na1 Na 0.49044(15) 0.09713(7) 0.74868(10) 0.0328(4) Uani 1 1 d . . . Na2 Na 0.72290(14) 0.11202(7) 0.76875(10) 0.0318(4) Uani 1 1 d . . . N1 N 0.6104(3) 0.12419(14) 0.67245(19) 0.0268(8) Uani 1 1 d . . . C1 C 0.6047(3) 0.09996(18) 0.6189(2) 0.0284(10) Uani 1 1 d . . . C2 C 0.5790(4) 0.12246(18) 0.5519(3) 0.0350(11) Uani 1 1 d . . . C3 C 0.4903(5) 0.1481(2) 0.5393(3) 0.0490(15) Uani 1 1 d . . . H3 H 0.4428 0.1503 0.5731 0.059 Uiso 1 1 calc R . . C4 C 0.4688(6) 0.1708(2) 0.4789(4) 0.065(2) Uani 1 1 d . . . H4 H 0.4068 0.1881 0.4713 0.078 Uiso 1 1 calc R . . C5 C 0.5382(7) 0.1683(2) 0.4291(3) 0.068(2) Uani 1 1 d . . . H5 H 0.5241 0.1841 0.3876 0.082 Uiso 1 1 calc R . . C6 C 0.6270(6) 0.1428(2) 0.4403(3) 0.0576(18) Uani 1 1 d . . . H6 H 0.6747 0.1412 0.4065 0.069 Uiso 1 1 calc R . . C7 C 0.6472(5) 0.1194(2) 0.5011(3) 0.0426(13) Uani 1 1 d . . . H7 H 0.7080 0.1012 0.5082 0.051 Uiso 1 1 calc R . . C8 C 0.6210(4) 0.04512(18) 0.6180(3) 0.0319(11) Uani 1 1 d . . . C9 C 0.5512(4) 0.01466(19) 0.5846(3) 0.0365(11) Uani 1 1 d . . . H9 H 0.4970 0.0286 0.5580 0.044 Uiso 1 1 calc R . . C10 C 0.5596(5) -0.0358(2) 0.5894(3) 0.0425(13) Uani 1 1 d . . . H10 H 0.5099 -0.0561 0.5676 0.051 Uiso 1 1 calc R . . C11 C 0.6399(5) -0.0566(2) 0.6256(3) 0.0479(14) Uani 1 1 d . . . H11 H 0.6461 -0.0912 0.6284 0.057 Uiso 1 1 calc R . . C12 C 0.7114(5) -0.0268(2) 0.6579(3) 0.0480(15) Uani 1 1 d . . . H12 H 0.7672 -0.0409 0.6827 0.058 Uiso 1 1 calc R . . C13 C 0.7019(4) 0.0236(2) 0.6542(3) 0.0393(12) Uani 1 1 d . . . H13 H 0.7512 0.0437 0.6767 0.047 Uiso 1 1 calc R . . N2 N 0.5935(3) 0.11344(14) 0.8482(2) 0.0298(9) Uani 1 1 d D A . C14 C 0.6213(4) 0.08521(18) 0.8952(2) 0.0315(10) Uani 1 1 d D . . C15 C 0.6003(11) 0.0310(3) 0.8923(9) 0.042(2) Uani 0.548(15) 1 d PDU A 1 C16 C 0.5126(10) 0.0133(4) 0.9186(8) 0.045(2) Uani 0.548(15) 1 d PDU A 1 H16 H 0.4682 0.0354 0.9391 0.054 Uiso 0.548(15) 1 calc PR A 1 C17 C 0.4883(11) -0.0363(4) 0.9157(7) 0.050(2) Uani 0.548(15) 1 d PDU A 1 H17 H 0.4277 -0.0480 0.9336 0.060 Uiso 0.548(15) 1 calc PR A 1 C18 C 0.5539(11) -0.0678(4) 0.8864(7) 0.053(3) Uani 0.548(15) 1 d PDU A 1 H18 H 0.5382 -0.1017 0.8842 0.064 Uiso 0.548(15) 1 calc PR A 1 C19 C 0.6413(12) -0.0514(3) 0.8603(7) 0.056(2) Uani 0.548(15) 1 d PDU A 1 H19 H 0.6861 -0.0737 0.8405 0.067 Uiso 0.548(15) 1 calc PR A 1 C20 C 0.6641(12) -0.0015(3) 0.8632(8) 0.051(2) Uani 0.548(15) 1 d PDU A 1 H20 H 0.7245 0.0101 0.8448 0.062 Uiso 0.548(15) 1 calc PR A 1 C15X C 0.6159(13) 0.0301(3) 0.8863(10) 0.041(2) Uani 0.452(15) 1 d PDU A 2 C16X C 0.5399(13) 0.0029(4) 0.9136(10) 0.049(2) Uani 0.452(15) 1 d PDU A 2 H16X H 0.4905 0.0192 0.9384 0.058 Uiso 0.452(15) 1 calc PR A 2 C17X C 0.5336(14) -0.0477(4) 0.9057(9) 0.055(3) Uani 0.452(15) 1 d PDU A 2 H17X H 0.4792 -0.0653 0.9234 0.066 Uiso 0.452(15) 1 calc PR A 2 C18X C 0.6065(14) -0.0717(4) 0.8723(8) 0.054(3) Uani 0.452(15) 1 d PDU A 2 H18X H 0.6049 -0.1064 0.8692 0.065 Uiso 0.452(15) 1 calc PR A 2 C19X C 0.6821(14) -0.0461(4) 0.8431(9) 0.057(3) Uani 0.452(15) 1 d PDU A 2 H19X H 0.7319 -0.0627 0.8191 0.068 Uiso 0.452(15) 1 calc PR A 2 C20X C 0.6841(14) 0.0047(4) 0.8496(10) 0.051(2) Uani 0.452(15) 1 d PDU A 2 H20X H 0.7344 0.0226 0.8277 0.061 Uiso 0.452(15) 1 calc PR A 2 C21 C 0.6644(4) 0.10091(18) 0.9630(2) 0.0339(11) Uani 1 1 d . A . C22 C 0.6234(4) 0.1395(2) 0.9971(3) 0.0377(12) Uani 1 1 d . . . H22 H 0.5660 0.1564 0.9782 0.045 Uiso 1 1 calc R A . C23 C 0.6658(5) 0.1540(2) 1.0590(3) 0.0481(15) Uani 1 1 d . A . H23 H 0.6364 0.1800 1.0826 0.058 Uiso 1 1 calc R . . C24 C 0.7507(5) 0.1302(2) 1.0857(3) 0.0538(16) Uani 1 1 d . . . H24 H 0.7802 0.1403 1.1275 0.065 Uiso 1 1 calc R A . C25 C 0.7930(6) 0.0919(3) 1.0522(3) 0.0577(18) Uani 1 1 d . A . H25 H 0.8517 0.0758 1.0707 0.069 Uiso 1 1 calc R . . C26 C 0.7491(5) 0.0770(2) 0.9911(3) 0.0445(14) Uani 1 1 d . . . H26 H 0.7773 0.0502 0.9683 0.053 Uiso 1 1 calc R A . N3 N 0.6946(3) 0.20051(13) 0.76973(18) 0.0239(8) Uani 1 1 d . . . C27 C 0.7869(3) 0.21221(17) 0.7696(2) 0.0276(9) Uani 1 1 d U . . C28 C 0.8339(4) 0.2283(2) 0.7046(3) 0.0360(11) Uani 1 1 d U . . C29 C 0.8236(4) 0.1989(2) 0.6486(3) 0.0419(12) Uani 1 1 d U . . H29 H 0.7878 0.1689 0.6509 0.050 Uiso 1 1 calc R . . C30 C 0.8650(4) 0.2126(3) 0.5884(3) 0.0501(14) Uani 1 1 d U . . H30 H 0.8583 0.1918 0.5506 0.060 Uiso 1 1 calc R . . C31 C 0.9142(5) 0.2554(3) 0.5848(3) 0.0537(15) Uani 1 1 d U . . H31 H 0.9437 0.2643 0.5444 0.064 Uiso 1 1 calc R . . C32 C 0.9226(5) 0.2860(3) 0.6378(4) 0.0577(15) Uani 1 1 d U . . H32 H 0.9542 0.3170 0.6334 0.069 Uiso 1 1 calc R . . C33 C 0.8843(5) 0.2721(2) 0.6999(3) 0.0525(14) Uani 1 1 d U . . H33 H 0.8933 0.2929 0.7377 0.063 Uiso 1 1 calc R . . C34 C 0.8611(4) 0.20771(18) 0.8294(2) 0.0283(9) Uani 1 1 d U . . C35 C 0.9653(4) 0.2028(2) 0.8209(3) 0.0360(11) Uani 1 1 d U . . H35 H 0.9906 0.2065 0.7777 0.043 Uiso 1 1 calc R . . C36 C 1.0319(4) 0.1925(2) 0.8748(3) 0.0448(13) Uani 1 1 d U . . H36 H 1.1022 0.1884 0.8682 0.054 Uiso 1 1 calc R . . C37 C 0.9968(4) 0.1883(2) 0.9378(3) 0.0451(13) Uani 1 1 d U . . H37 H 1.0426 0.1815 0.9746 0.054 Uiso 1 1 calc R . . C38 C 0.8943(4) 0.1940(2) 0.9474(3) 0.0429(12) Uani 1 1 d U . . H38 H 0.8698 0.1915 0.9909 0.051 Uiso 1 1 calc R . . C39 C 0.8274(4) 0.2034(2) 0.8934(3) 0.0368(11) Uani 1 1 d U . . H39 H 0.7572 0.2070 0.9004 0.044 Uiso 1 1 calc R . . N4 N 0.4776(3) 0.18968(13) 0.76064(19) 0.0243(8) Uani 1 1 d . . . C40 C 0.3837(3) 0.19604(16) 0.7686(2) 0.0266(9) Uani 1 1 d . . . C41 C 0.3420(3) 0.19531(18) 0.8372(2) 0.0288(10) Uani 1 1 d . . . C42 C 0.2966(4) 0.2367(2) 0.8638(3) 0.0413(13) Uani 1 1 d . . . H42 H 0.2880 0.2653 0.8373 0.050 Uiso 1 1 calc R . . C43 C 0.2641(4) 0.2365(3) 0.9283(3) 0.0513(17) Uani 1 1 d . . . H43 H 0.2343 0.2651 0.9457 0.062 Uiso 1 1 calc R . . C44 C 0.2745(4) 0.1957(3) 0.9671(3) 0.0478(15) Uani 1 1 d . . . H44 H 0.2511 0.1957 1.0111 0.057 Uiso 1 1 calc R . . C45 C 0.3186(5) 0.1550(2) 0.9426(3) 0.0465(14) Uani 1 1 d . . . H45 H 0.3262 0.1265 0.9695 0.056 Uiso 1 1 calc R . . C46 C 0.3528(4) 0.1548(2) 0.8781(3) 0.0364(11) Uani 1 1 d . . . H46 H 0.3842 0.1262 0.8619 0.044 Uiso 1 1 calc R . . C47 C 0.3052(3) 0.20488(17) 0.7124(2) 0.0278(10) Uani 1 1 d . . . C48 C 0.2033(4) 0.19365(19) 0.7182(3) 0.0336(11) Uani 1 1 d . . . H48 H 0.1812 0.1808 0.7590 0.040 Uiso 1 1 calc R . . C49 C 0.1336(4) 0.2010(2) 0.6652(3) 0.0385(12) Uani 1 1 d . . . H49 H 0.0640 0.1937 0.6701 0.046 Uiso 1 1 calc R . . C50 C 0.1642(4) 0.2189(2) 0.6052(3) 0.0387(12) Uani 1 1 d . . . H50 H 0.1163 0.2236 0.5689 0.046 Uiso 1 1 calc R . . C51 C 0.2652(4) 0.2300(2) 0.5985(3) 0.0413(13) Uani 1 1 d . . . H51 H 0.2868 0.2425 0.5574 0.050 Uiso 1 1 calc R . . C52 C 0.3352(4) 0.22291(19) 0.6513(3) 0.0355(11) Uani 1 1 d . . . H52 H 0.4046 0.2304 0.6460 0.043 Uiso 1 1 calc R . . N5 N 0.8792(4) 0.0877(2) 0.8250(3) 0.0515(13) Uani 1 1 d D . . H5A H 0.869(5) 0.095(3) 0.8676(15) 0.062 Uiso 1 1 d D . . C53 C 0.9596(4) 0.06509(19) 0.8101(3) 0.0404(13) Uani 1 1 d . . . C54 C 1.0464(4) 0.0541(2) 0.8586(3) 0.0413(13) Uani 1 1 d . . . C55 C 1.0331(5) 0.0540(3) 0.9268(3) 0.0575(17) Uani 1 1 d . . . H55 H 0.9672 0.0590 0.9427 0.069 Uiso 1 1 calc R . . C56 C 1.1147(6) 0.0467(3) 0.9722(4) 0.0620(18) Uani 1 1 d . . . H56 H 1.1055 0.0479 1.0188 0.074 Uiso 1 1 calc R . . C57 C 1.2097(5) 0.0378(2) 0.9486(4) 0.0580(18) Uani 1 1 d . . . H57 H 1.2659 0.0324 0.9791 0.070 Uiso 1 1 calc R . . C58 C 1.2227(5) 0.0368(2) 0.8819(3) 0.0535(16) Uani 1 1 d . . . H58 H 1.2881 0.0303 0.8662 0.064 Uiso 1 1 calc R . . C59 C 1.1428(4) 0.0451(2) 0.8366(3) 0.0468(14) Uani 1 1 d . . . H59 H 1.1535 0.0446 0.7902 0.056 Uiso 1 1 calc R . . C60 C 0.9683(4) 0.0515(2) 0.7387(3) 0.0419(13) Uani 1 1 d . . . C61 C 0.9567(5) 0.0879(3) 0.6905(3) 0.0552(17) Uani 1 1 d . . . H61 H 0.9458 0.1207 0.7041 0.066 Uiso 1 1 calc R . . C62 C 0.9606(6) 0.0778(4) 0.6251(4) 0.080(3) Uani 1 1 d . . . H62 H 0.9516 0.1031 0.5929 0.096 Uiso 1 1 calc R . . C63 C 0.9775(6) 0.0309(4) 0.6057(4) 0.081(3) Uani 1 1 d . . . H63 H 0.9805 0.0237 0.5595 0.097 Uiso 1 1 calc R . . C64 C 0.9905(6) -0.0066(3) 0.6517(4) 0.073(2) Uani 1 1 d . . . H64 H 1.0020 -0.0392 0.6374 0.088 Uiso 1 1 calc R . . C65 C 0.9866(5) 0.0041(3) 0.7188(3) 0.0537(16) Uani 1 1 d . . . H65 H 0.9964 -0.0210 0.7510 0.064 Uiso 1 1 calc R . . N6 N 0.4056(4) 0.01931(19) 0.7504(2) 0.0436(11) Uani 1 1 d D . . H6A H 0.417(5) 0.001(2) 0.787(2) 0.052 Uiso 1 1 d D . . C66 C 0.3484(4) -0.00620(19) 0.7104(3) 0.0346(11) Uani 1 1 d . . . C67 C 0.3309(5) -0.0594(2) 0.7210(3) 0.0406(12) Uani 1 1 d U . . C68 C 0.2362(5) -0.0792(2) 0.7151(3) 0.0463(13) Uani 1 1 d U . . H68 H 0.1804 -0.0590 0.7014 0.056 Uiso 1 1 calc R . . C69 C 0.2191(7) -0.1288(2) 0.7287(3) 0.0648(17) Uani 1 1 d U . . H69 H 0.1524 -0.1419 0.7265 0.078 Uiso 1 1 calc R . . C70 C 0.3019(8) -0.1582(3) 0.7455(3) 0.0737(19) Uani 1 1 d U . . H70 H 0.2921 -0.1919 0.7548 0.088 Uiso 1 1 calc R . . C71 C 0.3971(7) -0.1392(3) 0.7487(3) 0.0723(19) Uani 1 1 d U . . H71 H 0.4535 -0.1599 0.7591 0.087 Uiso 1 1 calc R . . C72 C 0.4127(6) -0.0901(2) 0.7369(3) 0.0587(16) Uani 1 1 d U . . H72 H 0.4796 -0.0772 0.7395 0.070 Uiso 1 1 calc R . . C73 C 0.2997(4) 0.01760(19) 0.6504(3) 0.0336(11) Uani 1 1 d . . . C74 C 0.2845(4) -0.0087(2) 0.5918(3) 0.0380(12) Uani 1 1 d . . . H74 H 0.2988 -0.0428 0.5913 0.046 Uiso 1 1 calc R . . C75 C 0.2485(5) 0.0143(2) 0.5339(3) 0.0502(15) Uani 1 1 d . . . H75 H 0.2393 -0.0038 0.4937 0.060 Uiso 1 1 calc R . . C76 C 0.2259(5) 0.0636(3) 0.5347(4) 0.0577(18) Uani 1 1 d . . . H76 H 0.2025 0.0796 0.4950 0.069 Uiso 1 1 calc R . . C77 C 0.2378(5) 0.0897(2) 0.5942(4) 0.0604(19) Uani 1 1 d . . . H77 H 0.2199 0.1233 0.5953 0.073 Uiso 1 1 calc R . . C78 C 0.2753(5) 0.0671(2) 0.6513(3) 0.0471(14) Uani 1 1 d . . . H78 H 0.2845 0.0852 0.6915 0.056 Uiso 1 1 calc R . . C79 C 0.5879(4) 0.25633(18) 0.6275(3) 0.0378(11) Uani 1 1 d DU . . H79A H 0.6532 0.2582 0.6056 0.045 Uiso 1 1 calc R B 1 H79B H 0.5331 0.2527 0.5923 0.045 Uiso 1 1 calc R B 1 C80 C 0.5712(6) 0.3041(2) 0.6670(3) 0.0389(14) Uani 0.826(8) 1 d PDU C 1 H80A H 0.5044 0.3020 0.6871 0.047 Uiso 0.826(8) 1 calc PR C 1 H80B H 0.6235 0.3057 0.7040 0.047 Uiso 0.826(8) 1 calc PR C 1 C81 C 0.5748(7) 0.3512(3) 0.6277(4) 0.0496(17) Uani 0.826(8) 1 d PU C 1 H81A H 0.6418 0.3536 0.6078 0.060 Uiso 0.826(8) 1 calc PR C 1 H81B H 0.5226 0.3497 0.5906 0.060 Uiso 0.826(8) 1 calc PR C 1 C82 C 0.5580(9) 0.3970(3) 0.6672(5) 0.072(3) Uani 0.826(8) 1 d PU C 1 H82A H 0.4868 0.3987 0.6786 0.108 Uiso 0.826(8) 1 calc PR C 1 H82B H 0.5747 0.4256 0.6406 0.108 Uiso 0.826(8) 1 calc PR C 1 H82C H 0.6016 0.3964 0.7082 0.108 Uiso 0.826(8) 1 calc PR C 1 C80X C 0.619(2) 0.3095(5) 0.6406(17) 0.044(3) Uani 0.174(8) 1 d PDU C 2 H80C H 0.6299 0.3279 0.5991 0.052 Uiso 0.174(8) 1 calc PR C 2 H80D H 0.6790 0.3125 0.6718 0.052 Uiso 0.174(8) 1 calc PR C 2 C81X C 0.520(2) 0.3238(13) 0.6725(18) 0.046(3) Uani 0.174(8) 1 d PDU C 2 H81C H 0.5032 0.2996 0.7069 0.055 Uiso 0.174(8) 1 calc PR C 2 H81D H 0.4633 0.3247 0.6382 0.055 Uiso 0.174(8) 1 calc PR C 2 C82X C 0.536(4) 0.3778(15) 0.706(2) 0.064(6) Uani 0.174(8) 1 d PU C 2 H82D H 0.6057 0.3804 0.7256 0.096 Uiso 0.174(8) 1 calc PR C 2 H82E H 0.4880 0.3823 0.7410 0.096 Uiso 0.174(8) 1 calc PR C 2 H82F H 0.5251 0.4030 0.6718 0.096 Uiso 0.174(8) 1 calc PR C 2 C83 C 0.5730(4) 0.24494(19) 0.9054(3) 0.0348(11) Uani 1 1 d U E . H83A H 0.5047 0.2447 0.9236 0.042 Uiso 1 1 calc R . . H83B H 0.6237 0.2412 0.9431 0.042 Uiso 1 1 calc R . . C84 C 0.5899(6) 0.2937(2) 0.8703(3) 0.0585(16) Uani 1 1 d DU . . H84A H 0.5338 0.2980 0.8362 0.070 Uiso 1 1 calc R D 1 H84B H 0.6533 0.2908 0.8463 0.070 Uiso 1 1 calc R D 1 C85 C 0.5971(7) 0.3407(3) 0.9121(4) 0.063(2) Uani 0.835(11) 1 d PDU E 1 H85A H 0.6482 0.3363 0.9494 0.075 Uiso 0.835(11) 1 calc PR E 1 H85B H 0.6192 0.3681 0.8841 0.075 Uiso 0.835(11) 1 calc PR E 1 C86 C 0.4941(7) 0.3526(4) 0.9396(5) 0.077(3) Uani 0.835(11) 1 d PDU E 1 H86A H 0.4485 0.3652 0.9036 0.116 Uiso 0.835(11) 1 calc PR E 1 H86B H 0.5028 0.3773 0.9747 0.116 Uiso 0.835(11) 1 calc PR E 1 H86C H 0.4651 0.3229 0.9581 0.116 Uiso 0.835(11) 1 calc PR E 1 C85X C 0.541(4) 0.3244(11) 0.9245(16) 0.064(4) Uani 0.165(11) 1 d PDU E 2 H85C H 0.4731 0.3110 0.9331 0.077 Uiso 0.165(11) 1 calc PR E 2 H85D H 0.5833 0.3228 0.9665 0.077 Uiso 0.165(11) 1 calc PR E 2 C86X C 0.531(4) 0.3778(12) 0.901(2) 0.069(6) Uani 0.165(11) 1 d PDU E 2 H86D H 0.5108 0.3982 0.9386 0.104 Uiso 0.165(11) 1 calc PR E 2 H86E H 0.4789 0.3801 0.8648 0.104 Uiso 0.165(11) 1 calc PR E 2 H86F H 0.5958 0.3892 0.8859 0.104 Uiso 0.165(11) 1 calc PR E 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 0.0248(3) 0.0247(3) 0.0227(3) -0.0024(2) -0.00107(19) -0.0010(2) Zn2 0.0247(3) 0.0240(3) 0.0243(3) 0.0005(2) -0.0022(2) -0.0002(2) Na1 0.0301(10) 0.0356(11) 0.0325(10) -0.0071(8) -0.0001(8) -0.0064(8) Na2 0.0286(10) 0.0328(10) 0.0338(10) 0.0010(8) -0.0004(8) 0.0030(8) N1 0.0243(19) 0.028(2) 0.028(2) -0.0013(16) 0.0006(16) -0.0023(15) C1 0.023(2) 0.032(2) 0.030(2) -0.0045(19) 0.0014(18) -0.0035(18) C2 0.046(3) 0.027(2) 0.031(3) -0.007(2) -0.009(2) -0.003(2) C3 0.055(4) 0.048(3) 0.042(3) -0.010(3) -0.011(3) 0.011(3) C4 0.093(6) 0.047(4) 0.051(4) -0.009(3) -0.029(4) 0.019(4) C5 0.125(7) 0.035(3) 0.042(4) 0.001(3) -0.029(4) 0.000(4) C6 0.101(6) 0.039(3) 0.032(3) -0.002(3) 0.002(3) -0.016(3) C7 0.060(4) 0.032(3) 0.036(3) -0.004(2) -0.001(3) -0.006(2) C8 0.033(3) 0.031(2) 0.032(3) -0.008(2) 0.001(2) 0.000(2) C9 0.039(3) 0.035(3) 0.035(3) -0.005(2) -0.004(2) -0.003(2) C10 0.047(3) 0.033(3) 0.047(3) -0.011(2) -0.002(3) -0.007(2) C11 0.062(4) 0.029(3) 0.052(4) -0.004(2) -0.002(3) 0.000(3) C12 0.049(3) 0.038(3) 0.055(4) -0.005(3) -0.011(3) 0.010(3) C13 0.038(3) 0.035(3) 0.043(3) -0.006(2) -0.009(2) -0.001(2) N2 0.030(2) 0.028(2) 0.031(2) 0.0033(17) -0.0010(17) -0.0048(16) C14 0.033(3) 0.029(2) 0.031(3) 0.000(2) -0.002(2) -0.002(2) C15 0.059(5) 0.030(3) 0.036(4) 0.004(3) -0.008(4) -0.008(3) C16 0.059(5) 0.032(4) 0.042(4) 0.005(4) -0.006(4) -0.010(4) C17 0.069(6) 0.034(4) 0.047(4) 0.002(4) -0.001(4) -0.012(4) C18 0.076(6) 0.031(4) 0.051(5) 0.003(4) 0.002(5) -0.013(4) C19 0.078(6) 0.032(4) 0.058(5) 0.005(4) 0.009(4) -0.014(4) C20 0.070(5) 0.031(4) 0.053(5) 0.007(4) 0.006(4) -0.009(4) C15X 0.059(5) 0.028(4) 0.036(4) 0.007(3) -0.011(4) -0.009(3) C16X 0.065(6) 0.036(4) 0.043(4) 0.003(4) -0.005(4) -0.011(4) C17X 0.072(6) 0.036(5) 0.055(5) 0.003(4) -0.002(5) -0.017(5) C18X 0.074(6) 0.031(4) 0.056(5) 0.008(4) 0.000(5) -0.017(4) C19X 0.078(6) 0.032(4) 0.062(6) 0.008(4) 0.006(5) -0.012(4) C20X 0.072(5) 0.028(4) 0.052(5) 0.008(4) 0.004(4) -0.010(4) C21 0.043(3) 0.030(2) 0.028(2) 0.007(2) -0.002(2) -0.006(2) C22 0.042(3) 0.040(3) 0.032(3) 0.007(2) 0.009(2) -0.002(2) C23 0.067(4) 0.044(3) 0.034(3) -0.003(2) 0.007(3) -0.008(3) C24 0.071(4) 0.056(4) 0.033(3) -0.006(3) -0.011(3) -0.007(3) C25 0.066(4) 0.057(4) 0.048(4) 0.005(3) -0.023(3) 0.001(3) C26 0.053(4) 0.039(3) 0.040(3) -0.001(2) -0.009(3) 0.003(3) N3 0.0244(18) 0.0220(18) 0.0251(18) -0.0036(15) -0.0006(15) -0.0010(14) C27 0.026(2) 0.027(2) 0.030(2) 0.0007(18) -0.0019(18) -0.0026(17) C28 0.021(2) 0.045(3) 0.041(2) 0.017(2) -0.0030(19) -0.0036(19) C29 0.028(2) 0.061(3) 0.037(3) 0.010(2) 0.002(2) 0.000(2) C30 0.030(3) 0.081(4) 0.039(3) 0.013(3) 0.005(2) 0.005(3) C31 0.036(3) 0.080(4) 0.046(3) 0.026(3) 0.000(2) 0.005(3) C32 0.046(3) 0.057(3) 0.071(4) 0.021(3) 0.011(3) -0.012(3) C33 0.047(3) 0.053(3) 0.057(3) 0.015(3) -0.005(3) -0.012(3) C34 0.025(2) 0.032(2) 0.027(2) -0.0029(18) -0.0004(17) -0.0033(17) C35 0.024(2) 0.054(3) 0.030(2) -0.002(2) 0.0007(18) -0.002(2) C36 0.026(2) 0.069(4) 0.038(3) -0.001(3) -0.006(2) -0.004(2) C37 0.037(3) 0.064(3) 0.033(2) -0.004(3) -0.012(2) 0.004(3) C38 0.037(3) 0.062(3) 0.028(2) -0.011(2) -0.004(2) 0.005(2) C39 0.031(2) 0.046(3) 0.033(2) -0.008(2) -0.0028(19) 0.002(2) N4 0.0225(18) 0.0218(18) 0.0287(19) -0.0013(15) 0.0003(15) -0.0007(14) C40 0.030(2) 0.021(2) 0.029(2) 0.0007(18) -0.0017(19) -0.0011(18) C41 0.023(2) 0.033(2) 0.030(2) -0.006(2) -0.0037(18) -0.0004(19) C42 0.035(3) 0.044(3) 0.043(3) -0.012(2) -0.009(2) 0.011(2) C43 0.034(3) 0.072(4) 0.047(3) -0.032(3) -0.004(3) 0.013(3) C44 0.029(3) 0.083(5) 0.031(3) -0.020(3) 0.001(2) -0.004(3) C45 0.047(3) 0.061(4) 0.033(3) 0.001(3) 0.012(2) -0.013(3) C46 0.038(3) 0.037(3) 0.036(3) -0.001(2) 0.015(2) -0.002(2) C47 0.026(2) 0.025(2) 0.033(2) 0.0010(19) -0.0010(19) 0.0015(18) C48 0.028(2) 0.039(3) 0.033(3) 0.003(2) -0.004(2) -0.002(2) C49 0.024(2) 0.050(3) 0.041(3) 0.007(2) -0.004(2) -0.005(2) C50 0.030(3) 0.049(3) 0.036(3) 0.014(2) -0.004(2) 0.001(2) C51 0.032(3) 0.050(3) 0.041(3) 0.020(3) 0.000(2) 0.000(2) C52 0.023(2) 0.037(3) 0.045(3) 0.009(2) -0.003(2) 0.001(2) N5 0.050(3) 0.048(3) 0.056(3) -0.007(3) -0.009(3) 0.013(2) C53 0.035(3) 0.029(3) 0.057(4) 0.002(2) -0.007(3) 0.003(2) C54 0.039(3) 0.031(3) 0.053(3) 0.004(2) -0.007(3) 0.004(2) C55 0.053(4) 0.063(4) 0.055(4) 0.003(3) -0.005(3) 0.014(3) C56 0.065(5) 0.069(5) 0.050(4) 0.000(3) -0.008(3) 0.012(4) C57 0.053(4) 0.051(4) 0.068(5) 0.007(3) -0.022(3) 0.003(3) C58 0.044(3) 0.057(4) 0.059(4) 0.004(3) -0.008(3) 0.007(3) C59 0.038(3) 0.047(3) 0.054(4) 0.004(3) -0.006(3) 0.003(3) C60 0.028(3) 0.043(3) 0.054(3) 0.008(3) -0.006(2) -0.002(2) C61 0.047(4) 0.062(4) 0.057(4) 0.018(3) -0.001(3) -0.007(3) C62 0.068(5) 0.113(8) 0.059(5) 0.028(5) 0.002(4) -0.016(5) C63 0.056(5) 0.143(9) 0.043(4) -0.011(5) -0.001(3) 0.000(5) C64 0.053(4) 0.092(6) 0.075(5) -0.028(5) -0.005(4) 0.010(4) C65 0.047(4) 0.056(4) 0.056(4) -0.005(3) -0.010(3) 0.006(3) N6 0.046(3) 0.047(3) 0.037(3) -0.005(2) -0.001(2) -0.012(2) C66 0.032(3) 0.035(3) 0.037(3) -0.008(2) 0.003(2) 0.000(2) C67 0.057(3) 0.033(2) 0.031(2) -0.006(2) -0.011(2) 0.002(2) C68 0.071(3) 0.038(3) 0.029(3) -0.001(2) -0.006(3) -0.011(3) C69 0.110(5) 0.045(3) 0.038(3) -0.004(3) -0.008(3) -0.023(3) C70 0.147(6) 0.038(3) 0.034(3) -0.001(3) -0.020(4) 0.003(3) C71 0.124(5) 0.052(3) 0.038(3) -0.005(3) -0.022(4) 0.032(4) C72 0.079(4) 0.052(3) 0.042(3) -0.008(3) -0.019(3) 0.021(3) C73 0.029(2) 0.033(3) 0.040(3) 0.000(2) 0.006(2) -0.002(2) C74 0.038(3) 0.038(3) 0.038(3) 0.002(2) 0.002(2) 0.001(2) C75 0.047(3) 0.060(4) 0.043(3) 0.012(3) -0.001(3) 0.007(3) C76 0.052(4) 0.062(4) 0.059(4) 0.032(4) 0.007(3) 0.010(3) C77 0.063(4) 0.037(3) 0.081(5) 0.020(3) 0.011(4) 0.010(3) C78 0.047(3) 0.038(3) 0.057(4) 0.001(3) 0.008(3) -0.002(3) C79 0.038(3) 0.033(2) 0.041(3) 0.009(2) -0.005(2) -0.002(2) C80 0.046(4) 0.033(3) 0.037(3) 0.006(3) 0.002(3) -0.004(3) C81 0.067(4) 0.035(3) 0.047(4) 0.006(3) 0.007(3) -0.003(3) C82 0.118(8) 0.041(4) 0.056(5) -0.010(4) -0.007(5) 0.002(5) C80X 0.053(6) 0.036(5) 0.043(5) 0.006(5) 0.002(5) -0.004(5) C81X 0.058(6) 0.036(6) 0.043(6) 0.004(5) 0.005(6) -0.003(5) C82X 0.098(14) 0.045(11) 0.051(13) -0.008(10) 0.015(12) 0.001(11) C83 0.034(3) 0.040(3) 0.030(2) -0.013(2) -0.001(2) 0.003(2) C84 0.086(4) 0.039(3) 0.051(3) -0.012(2) 0.001(3) 0.005(3) C85 0.095(5) 0.034(3) 0.060(4) -0.009(3) 0.007(4) -0.012(4) C86 0.104(7) 0.059(5) 0.071(6) -0.022(5) 0.024(5) 0.005(5) C85X 0.092(7) 0.041(6) 0.062(7) -0.014(6) 0.007(7) 0.001(6) C86X 0.099(12) 0.045(8) 0.065(11) -0.015(9) 0.005(11) 0.005(10) _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 2.058(4) . ? Zn1 N3 2.112(4) . ? Zn1 N4 2.103(4) . ? Zn1 C83 2.024(5) . ? Zn2 N1 2.063(4) . ? Zn2 N3 2.111(4) . ? Zn2 N4 2.139(4) . ? Zn2 C79 2.000(5) . ? Na1 N1 2.377(4) . ? Na1 N2 2.403(4) . ? Na1 N4 2.548(4) . ? Na1 N6 2.406(5) . ? Na2 N1 2.402(4) . ? Na2 N2 2.398(5) . ? Na2 N3 2.448(4) . ? Na2 N5 2.397(5) . ? N1 C1 1.262(6) . ? C1 C2 1.504(7) . ? C1 C8 1.515(7) . ? C2 C3 1.377(8) . ? C2 C7 1.396(8) . ? C3 C4 1.380(9) . ? C4 C5 1.392(11) . ? C5 C6 1.372(11) . ? C6 C7 1.394(8) . ? C8 C9 1.390(7) . ? C8 C13 1.392(7) . ? C9 C10 1.387(7) . ? C10 C11 1.378(8) . ? C11 C12 1.384(8) . ? C12 C13 1.385(8) . ? N2 C14 1.259(6) . ? C14 C15 1.509(8) . ? C14 C15X 1.519(9) . ? C14 C21 1.512(7) . ? C15 C16 1.385(8) . ? C15 C20 1.375(8) . ? C16 C17 1.392(9) . ? C17 C18 1.375(10) . ? C18 C19 1.367(10) . ? C19 C20 1.397(9) . ? C15X C16X 1.384(8) . ? C15X C20X 1.379(9) . ? C16X C17X 1.394(9) . ? C17X C18X 1.370(11) . ? C18X C19X 1.373(11) . ? C19X C20X 1.397(9) . ? C21 C22 1.384(8) . ? C21 C26 1.389(8) . ? C22 C23 1.393(8) . ? C23 C24 1.381(9) . ? C24 C25 1.376(10) . ? C25 C26 1.393(8) . ? N3 C27 1.260(6) . ? C27 C28 1.538(7) . ? C27 C34 1.517(6) . ? C28 C29 1.384(8) . ? C28 C33 1.376(8) . ? C29 C30 1.403(8) . ? C30 C31 1.341(9) . ? C31 C32 1.354(10) . ? C32 C33 1.422(9) . ? C34 C35 1.402(7) . ? C34 C39 1.386(7) . ? C35 C36 1.390(7) . ? C36 C37 1.375(8) . ? C37 C38 1.385(8) . ? C38 C39 1.388(7) . ? N4 C40 1.270(6) . ? C40 C41 1.509(7) . ? C40 C47 1.513(6) . ? C41 C42 1.399(7) . ? C41 C46 1.382(7) . ? C42 C43 1.387(8) . ? C43 C44 1.365(10) . ? C44 C45 1.361(9) . ? C45 C46 1.393(7) . ? C47 C48 1.390(7) . ? C47 C52 1.399(7) . ? C48 C49 1.388(7) . ? C49 C50 1.380(7) . ? C50 C51 1.380(7) . ? C51 C52 1.385(7) . ? N5 C53 1.277(7) . ? C53 C54 1.496(7) . ? C53 C60 1.492(9) . ? C54 C55 1.392(9) . ? C54 C59 1.389(8) . ? C55 C56 1.391(9) . ? C56 C57 1.384(10) . ? C57 C58 1.362(10) . ? C58 C59 1.376(8) . ? C60 C61 1.393(8) . ? C60 C65 1.380(9) . ? C61 C62 1.346(11) . ? C62 C63 1.364(13) . ? C63 C64 1.385(13) . ? C64 C65 1.383(10) . ? N6 C66 1.281(7) . ? C66 C67 1.489(7) . ? C66 C73 1.488(7) . ? C67 C68 1.362(8) . ? C67 C72 1.393(8) . ? C68 C69 1.406(8) . ? C69 C70 1.384(11) . ? C70 C71 1.358(12) . ? C71 C72 1.381(10) . ? C73 C74 1.386(7) . ? C73 C78 1.391(8) . ? C74 C75 1.385(8) . ? C75 C76 1.379(9) . ? C76 C77 1.394(10) . ? C77 C78 1.373(9) . ? C79 C80 1.549(7) . ? C79 C80X 1.531(9) . ? C80 C81 1.515(9) . ? C81 C82 1.504(11) . ? C80X C81X 1.536(10) . ? C81X C82X 1.63(5) . ? C83 C84 1.530(8) . ? C84 C85 1.534(7) . ? C84 C85X 1.543(10) . ? C85 C86 1.529(8) . ? C85X C86X 1.537(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Zn1 N3 99.64(15) . . ? N2 Zn1 N4 95.67(15) . . ? N2 Zn1 C83 136.3(2) . . ? N3 Zn1 N4 86.09(14) . . ? N3 Zn1 C83 113.26(19) . . ? N4 Zn1 C83 113.85(18) . . ? N1 Zn2 N3 93.13(15) . . ? N1 Zn2 N4 95.91(15) . . ? N1 Zn2 C79 133.46(19) . . ? N3 Zn2 N4 85.20(14) . . ? N3 Zn2 C79 115.38(18) . . ? N4 Zn2 C79 121.11(19) . . ? N1 Na1 N2 96.37(15) . . ? N1 Na1 N4 78.55(14) . . ? N1 Na1 N6 127.64(17) . . ? N2 Na1 N4 76.99(14) . . ? N2 Na1 N6 113.37(17) . . ? N4 Na1 N6 147.52(18) . . ? N1 Na2 N2 95.85(15) . . ? N1 Na2 N3 77.35(14) . . ? N1 Na2 N5 154.30(19) . . ? N2 Na2 N3 82.20(14) . . ? N2 Na2 N5 108.41(19) . . ? N3 Na2 N5 113.51(17) . . ? Zn2 N1 Na1 96.14(16) . . ? Zn2 N1 Na2 95.89(15) . . ? Zn2 N1 C1 129.5(3) . . ? Na1 N1 Na2 80.96(14) . . ? Na1 N1 C1 111.9(3) . . ? Na2 N1 C1 128.4(3) . . ? N1 C1 C2 123.4(4) . . ? N1 C1 C8 121.8(5) . . ? C2 C1 C8 114.9(4) . . ? C1 C2 C3 121.5(5) . . ? C1 C2 C7 120.4(5) . . ? C3 C2 C7 118.1(5) . . ? C2 C3 C4 121.7(7) . . ? C3 C4 C5 119.7(7) . . ? C4 C5 C6 119.7(6) . . ? C5 C6 C7 120.0(7) . . ? C2 C7 C6 120.8(6) . . ? C1 C8 C9 120.5(5) . . ? C1 C8 C13 121.3(4) . . ? C9 C8 C13 118.1(5) . . ? C8 C9 C10 120.9(5) . . ? C9 C10 C11 120.3(5) . . ? C10 C11 C12 119.6(5) . . ? C11 C12 C13 120.1(5) . . ? C8 C13 C12 121.0(5) . . ? Zn1 N2 Na1 95.93(16) . . ? Zn1 N2 Na2 90.39(15) . . ? Zn1 N2 C14 132.4(4) . . ? Na1 N2 Na2 80.50(14) . . ? Na1 N2 C14 129.9(3) . . ? Na2 N2 C14 107.4(3) . . ? N2 C14 C15 121.8(9) . . ? N2 C14 C15X 120.7(10) . . ? N2 C14 C21 125.7(5) . . ? C15 C14 C15X 9.3(7) . . ? C15 C14 C21 112.0(8) . . ? C15X C14 C21 113.6(10) . . ? C14 C15 C16 118.9(7) . . ? C14 C15 C20 122.4(7) . . ? C16 C15 C20 118.7(8) . . ? C15 C16 C17 121.2(9) . . ? C16 C17 C18 118.6(9) . . ? C17 C18 C19 121.4(9) . . ? C18 C19 C20 119.3(10) . . ? C15 C20 C19 120.8(9) . . ? C14 C15X C16X 121.1(8) . . ? C14 C15X C20X 122.2(8) . . ? C16X C15X C20X 116.7(9) . . ? C15X C16X C17X 121.8(10) . . ? C16X C17X C18X 119.5(11) . . ? C17X C18X C19X 120.6(10) . . ? C18X C19X C20X 118.6(10) . . ? C15X C20X C19X 122.7(10) . . ? C14 C21 C22 121.6(5) . . ? C14 C21 C26 119.3(5) . . ? C22 C21 C26 119.0(5) . . ? C21 C22 C23 120.5(5) . . ? C22 C23 C24 119.6(6) . . ? C23 C24 C25 120.7(6) . . ? C24 C25 C26 119.5(6) . . ? C21 C26 C25 120.7(6) . . ? Zn1 N3 Zn2 94.56(15) . . ? Zn1 N3 Na2 87.76(14) . . ? Zn1 N3 C27 137.3(3) . . ? Zn2 N3 Na2 93.26(14) . . ? Zn2 N3 C27 127.5(3) . . ? Na2 N3 C27 95.9(3) . . ? N3 C27 C28 120.5(4) . . ? N3 C27 C34 124.3(4) . . ? C28 C27 C34 115.0(4) . . ? C27 C28 C29 119.8(5) . . ? C27 C28 C33 121.6(5) . . ? C29 C28 C33 118.5(5) . . ? C28 C29 C30 121.3(6) . . ? C29 C30 C31 119.4(7) . . ? C30 C31 C32 121.2(6) . . ? C31 C32 C33 120.4(6) . . ? C28 C33 C32 119.2(7) . . ? C27 C34 C35 120.6(4) . . ? C27 C34 C39 121.1(4) . . ? C35 C34 C39 117.9(4) . . ? C34 C35 C36 120.7(5) . . ? C35 C36 C37 120.3(5) . . ? C36 C37 C38 119.8(5) . . ? C37 C38 C39 119.9(5) . . ? C34 C39 C38 121.3(5) . . ? Zn1 N4 Zn2 94.00(14) . . ? Zn1 N4 Na1 90.62(14) . . ? Zn1 N4 C40 122.2(3) . . ? Zn2 N4 Na1 89.39(14) . . ? Zn2 N4 C40 141.2(3) . . ? Na1 N4 C40 102.6(3) . . ? N4 C40 C41 121.2(4) . . ? N4 C40 C47 124.3(4) . . ? C41 C40 C47 114.5(4) . . ? C40 C41 C42 121.4(5) . . ? C40 C41 C46 121.5(4) . . ? C42 C41 C46 117.0(5) . . ? C41 C42 C43 120.8(6) . . ? C42 C43 C44 120.7(6) . . ? C43 C44 C45 119.6(5) . . ? C44 C45 C46 120.3(6) . . ? C41 C46 C45 121.5(5) . . ? C40 C47 C48 122.1(4) . . ? C40 C47 C52 119.8(4) . . ? C48 C47 C52 118.1(4) . . ? C47 C48 C49 120.7(5) . . ? C48 C49 C50 120.6(5) . . ? C49 C50 C51 119.4(5) . . ? C50 C51 C52 120.3(5) . . ? C47 C52 C51 120.9(5) . . ? Na2 N5 C53 136.9(5) . . ? N5 C53 C54 124.3(6) . . ? N5 C53 C60 116.9(5) . . ? C54 C53 C60 118.8(5) . . ? C53 C54 C55 120.7(6) . . ? C53 C54 C59 120.9(6) . . ? C55 C54 C59 118.4(5) . . ? C54 C55 C56 120.9(7) . . ? C55 C56 C57 119.1(7) . . ? C56 C57 C58 120.2(6) . . ? C57 C58 C59 121.1(7) . . ? C54 C59 C58 120.3(6) . . ? C53 C60 C61 118.7(6) . . ? C53 C60 C65 122.5(5) . . ? C61 C60 C65 118.9(6) . . ? C60 C61 C62 121.7(8) . . ? C61 C62 C63 119.1(8) . . ? C62 C63 C64 121.5(8) . . ? C63 C64 C65 118.9(8) . . ? C60 C65 C64 119.9(7) . . ? Na1 N6 C66 137.1(4) . . ? N6 C66 C67 122.2(5) . . ? N6 C66 C73 119.2(5) . . ? C67 C66 C73 118.6(4) . . ? C66 C67 C68 121.6(5) . . ? C66 C67 C72 119.8(6) . . ? C68 C67 C72 118.6(6) . . ? C67 C68 C69 121.5(7) . . ? C68 C69 C70 118.3(8) . . ? C69 C70 C71 120.5(7) . . ? C70 C71 C72 120.6(7) . . ? C67 C72 C71 120.3(8) . . ? C66 C73 C74 120.0(5) . . ? C66 C73 C78 120.3(5) . . ? C74 C73 C78 119.6(5) . . ? C73 C74 C75 120.4(6) . . ? C74 C75 C76 120.0(6) . . ? C75 C76 C77 119.7(6) . . ? C76 C77 C78 120.4(6) . . ? C73 C78 C77 120.0(6) . . ? Zn2 C79 C80 111.0(4) . . ? Zn2 C79 C80X 131.4(14) . . ? C80 C79 C80X 32.3(11) . . ? C79 C80 C81 116.1(5) . . ? C80 C81 C82 115.1(7) . . ? C79 C80X C81X 95.0(18) . . ? C80X C81X C82X 108(3) . . ? Zn1 C83 C84 110.6(4) . . ? C83 C84 C85 118.9(6) . . ? C83 C84 C85X 94.1(14) . . ? C85 C84 C85X 34.5(17) . . ? C84 C85 C86 110.1(7) . . ? C84 C85X C86X 110(2) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.966 _refine_diff_density_min -0.982 _refine_diff_density_rms 0.092 #===END data_rem366_compound3 _database_code_depnum_ccdc_archive 'CCDC 631658' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C34 H74 N4 Na2 O2 Zn2' _chemical_formula_sum 'C34 H74 N4 Na2 O2 Zn2' _chemical_formula_weight 747.69 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 10.380(2) _cell_length_b 17.783(3) _cell_length_c 22.035(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4067.2(14) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 7538 _cell_measurement_theta_min 2.25 _cell_measurement_theta_max 28.23 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.221 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1616 _exptl_absorpt_coefficient_mu 1.233 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.626 _exptl_absorpt_correction_T_max 0.695 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1K CCD diffractometer' _diffrn_measurement_method 'thin-slice \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28407 _diffrn_reflns_av_R_equivalents 0.0690 _diffrn_reflns_av_sigmaI/netI 0.0600 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.47 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7155 _reflns_number_gt 6357 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution SIR97 _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL and local programs' _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^)+(0.0504P)^2^+2.5961P] 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 0.107(15) _refine_ls_number_reflns 7155 _refine_ls_number_parameters 416 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0588 _refine_ls_R_factor_gt 0.0493 _refine_ls_wR_factor_ref 0.1134 _refine_ls_wR_factor_gt 0.1090 _refine_ls_goodness_of_fit_ref 1.152 _refine_ls_restrained_S_all 1.152 _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 0.06891(5) 0.96501(3) 0.44266(2) 0.01673(14) Uani 1 1 d . . . Zn2 Zn 0.22006(5) 1.13179(3) 0.64922(2) 0.01644(14) Uani 1 1 d . . . Na1 Na -0.00721(18) 1.04036(11) 0.60709(8) 0.0202(4) Uani 1 1 d . . . Na2 Na 0.20875(18) 0.93624(9) 0.56086(8) 0.0195(4) Uani 1 1 d . . . O1 O 0.1964(3) 1.01853(16) 0.64171(14) 0.0180(7) Uani 1 1 d . . . O2 O 0.0013(3) 0.95319(18) 0.52836(14) 0.0183(7) Uani 1 1 d . . . N1 N 0.2781(4) 0.8555(2) 0.64326(18) 0.0253(9) Uani 1 1 d . . . N2 N -0.1888(4) 0.9615(3) 0.63059(19) 0.0281(10) Uani 1 1 d . . . N3 N 0.0445(4) 1.1686(2) 0.63313(16) 0.0148(9) Uani 1 1 d . . . N4 N 0.2462(4) 0.9278(2) 0.45194(17) 0.0173(9) Uani 1 1 d . . . C1 C 0.4011(4) 1.1683(3) 0.6637(2) 0.0226(12) Uani 1 1 d . . . C2 C 0.4732(5) 1.1173(4) 0.7063(3) 0.0386(15) Uani 1 1 d . . . H2A H 0.5606 1.1368 0.7125 0.058 Uiso 1 1 calc R . . H2B H 0.4779 1.0667 0.6889 0.058 Uiso 1 1 calc R . . H2C H 0.4282 1.1153 0.7454 0.058 Uiso 1 1 calc R . . C3 C 0.4048(7) 1.2468(4) 0.6925(4) 0.058(2) Uani 1 1 d . . . H3A H 0.3578 1.2461 0.7310 0.087 Uiso 1 1 calc R . . H3B H 0.3645 1.2832 0.6649 0.087 Uiso 1 1 calc R . . H3C H 0.4945 1.2614 0.6998 0.087 Uiso 1 1 calc R . . C4 C 0.4694(6) 1.1679(5) 0.6034(3) 0.052(2) Uani 1 1 d . . . H4A H 0.5600 1.1815 0.6094 0.079 Uiso 1 1 calc R . . H4B H 0.4286 1.2044 0.5762 0.079 Uiso 1 1 calc R . . H4C H 0.4641 1.1176 0.5855 0.079 Uiso 1 1 calc R . . C5 C -0.0614(5) 1.0023(3) 0.3828(2) 0.0232(11) Uani 1 1 d . . . C6 C -0.1523(6) 1.0600(3) 0.4113(3) 0.0377(15) Uani 1 1 d . . . H6A H -0.1046 1.1062 0.4202 0.057 Uiso 1 1 calc R . . H6B H -0.1881 1.0395 0.4490 0.057 Uiso 1 1 calc R . . H6C H -0.2226 1.0711 0.3830 0.057 Uiso 1 1 calc R . . C7 C 0.0022(6) 1.0383(4) 0.3284(2) 0.0354(13) Uani 1 1 d . . . H7A H 0.0532 1.0006 0.3067 0.053 Uiso 1 1 calc R . . H7B H 0.0587 1.0791 0.3420 0.053 Uiso 1 1 calc R . . H7C H -0.0640 1.0586 0.3013 0.053 Uiso 1 1 calc R . . C8 C -0.1426(6) 0.9356(4) 0.3604(3) 0.0398(15) Uani 1 1 d . . . H8A H -0.2092 0.9538 0.3325 0.060 Uiso 1 1 calc R . . H8B H -0.1834 0.9108 0.3952 0.060 Uiso 1 1 calc R . . H8C H -0.0869 0.8996 0.3393 0.060 Uiso 1 1 calc R . . C9 C 0.2279(7) 0.9786(3) 0.6951(2) 0.0318(13) Uani 1 1 d . . . H9A H 0.1770 0.9993 0.7292 0.038 Uiso 1 1 calc R . . H9B H 0.3201 0.9868 0.7044 0.038 Uiso 1 1 calc R . . C10 C 0.2030(6) 0.8947(3) 0.6907(2) 0.0304(13) Uani 1 1 d . . . H10A H 0.2229 0.8715 0.7304 0.036 Uiso 1 1 calc R . . H10B H 0.1101 0.8867 0.6827 0.036 Uiso 1 1 calc R . . C11 C 0.4133(6) 0.8572(4) 0.6552(3) 0.059(2) Uani 1 1 d . . . H11A H 0.4304 0.8346 0.6949 0.088 Uiso 1 1 calc R . . H11B H 0.4436 0.9094 0.6550 0.088 Uiso 1 1 calc R . . H11C H 0.4589 0.8286 0.6237 0.088 Uiso 1 1 calc R . . C12 C 0.2334(8) 0.7775(3) 0.6393(3) 0.0518(19) Uani 1 1 d . . . H12A H 0.2760 0.7525 0.6051 0.078 Uiso 1 1 calc R . . H12B H 0.1399 0.7769 0.6331 0.078 Uiso 1 1 calc R . . H12C H 0.2545 0.7511 0.6770 0.078 Uiso 1 1 calc R . . C13 C -0.1137(5) 0.9117(3) 0.5305(2) 0.0240(12) Uani 1 1 d . . . H13A H -0.1008 0.8637 0.5086 0.029 Uiso 1 1 calc R . . H13B H -0.1817 0.9402 0.5090 0.029 Uiso 1 1 calc R . . C14 C -0.1598(5) 0.8946(3) 0.5940(2) 0.0247(12) Uani 1 1 d . . . H14A H -0.2384 0.8632 0.5913 0.030 Uiso 1 1 calc R . . H14B H -0.0930 0.8647 0.6151 0.030 Uiso 1 1 calc R . . C15 C -0.2192(7) 0.9381(4) 0.6921(3) 0.057(2) Uani 1 1 d . . . H15A H -0.2941 0.9046 0.6915 0.086 Uiso 1 1 calc R . . H15B H -0.2387 0.9825 0.7168 0.086 Uiso 1 1 calc R . . H15C H -0.1452 0.9115 0.7095 0.086 Uiso 1 1 calc R . . C16 C -0.2971(6) 1.0028(4) 0.6042(3) 0.0495(18) Uani 1 1 d . . . H16A H -0.3736 0.9706 0.6037 0.074 Uiso 1 1 calc R . . H16B H -0.2755 1.0179 0.5627 0.074 Uiso 1 1 calc R . . H16C H -0.3146 1.0477 0.6287 0.074 Uiso 1 1 calc R . . C17 C 0.0830(5) 1.1735(3) 0.5255(2) 0.0247(11) Uani 1 1 d . . . H17A H 0.1746 1.1629 0.5320 0.037 Uiso 1 1 calc R . . H17B H 0.0725 1.2031 0.4883 0.037 Uiso 1 1 calc R . . H17C H 0.0358 1.1260 0.5215 0.037 Uiso 1 1 calc R . . C18 C 0.1070(5) 1.2915(3) 0.5811(2) 0.0270(12) Uani 1 1 d . . . H18A H 0.0727 1.3240 0.6132 0.040 Uiso 1 1 calc R . . H18B H 0.0994 1.3171 0.5419 0.040 Uiso 1 1 calc R . . H18C H 0.1979 1.2806 0.5893 0.040 Uiso 1 1 calc R . . C19 C 0.0302(4) 1.2176(3) 0.5794(2) 0.0155(10) Uani 1 1 d . . . C20 C -0.1114(5) 1.2338(3) 0.5674(2) 0.0230(12) Uani 1 1 d . . . H20A H -0.1546 1.1867 0.5548 0.028 Uiso 1 1 calc R . . H20B H -0.1186 1.2702 0.5336 0.028 Uiso 1 1 calc R . . C21 C -0.1803(5) 1.2656(3) 0.6229(2) 0.0264(12) Uani 1 1 d . . . H21A H -0.1432 1.3150 0.6338 0.032 Uiso 1 1 calc R . . H21B H -0.2730 1.2726 0.6138 0.032 Uiso 1 1 calc R . . C22 C -0.1641(5) 1.2109(3) 0.6751(2) 0.0223(11) Uani 1 1 d . . . H22A H -0.2092 1.1635 0.6651 0.027 Uiso 1 1 calc R . . H22B H -0.2051 1.2324 0.7118 0.027 Uiso 1 1 calc R . . C23 C -0.0227(5) 1.1935(3) 0.6890(2) 0.0195(11) Uani 1 1 d . . . C24 C -0.0201(5) 1.1274(3) 0.7332(2) 0.0267(12) Uani 1 1 d . . . H24A H -0.0609 1.0836 0.7143 0.040 Uiso 1 1 calc R . . H24B H -0.0671 1.1410 0.7702 0.040 Uiso 1 1 calc R . . H24C H 0.0694 1.1154 0.7435 0.040 Uiso 1 1 calc R . . C25 C 0.0407(5) 1.2609(3) 0.7225(2) 0.0295(13) Uani 1 1 d . . . H25A H 0.1342 1.2534 0.7243 0.044 Uiso 1 1 calc R . . H25B H 0.0062 1.2643 0.7638 0.044 Uiso 1 1 calc R . . H25C H 0.0219 1.3076 0.7006 0.044 Uiso 1 1 calc R . . C26 C 0.1544(5) 0.8033(3) 0.4646(2) 0.0262(12) Uani 1 1 d . . . H26A H 0.1548 0.8141 0.5082 0.039 Uiso 1 1 calc R . . H26B H 0.1680 0.7494 0.4581 0.039 Uiso 1 1 calc R . . H26C H 0.0713 0.8182 0.4473 0.039 Uiso 1 1 calc R . . C27 C 0.2497(6) 0.8319(3) 0.3654(2) 0.0324(14) Uani 1 1 d . . . H27A H 0.1748 0.8587 0.3492 0.049 Uiso 1 1 calc R . . H27B H 0.2392 0.7778 0.3586 0.049 Uiso 1 1 calc R . . H27C H 0.3278 0.8494 0.3448 0.049 Uiso 1 1 calc R . . C28 C 0.2613(5) 0.8472(2) 0.4341(2) 0.0191(11) Uani 1 1 d . . . C29 C 0.3916(5) 0.8187(3) 0.4567(2) 0.0311(14) Uani 1 1 d . . . H29A H 0.3884 0.8150 0.5015 0.037 Uiso 1 1 calc R . . H29B H 0.4057 0.7674 0.4406 0.037 Uiso 1 1 calc R . . C30 C 0.5049(5) 0.8669(3) 0.4393(3) 0.0347(12) Uani 1 1 d . . . H30A H 0.5168 0.8659 0.3947 0.042 Uiso 1 1 calc R . . H30B H 0.5842 0.8473 0.4585 0.042 Uiso 1 1 calc R . . C31 C 0.4799(5) 0.9482(3) 0.4606(2) 0.0278(13) Uani 1 1 d . . . H31A H 0.4779 0.9496 0.5055 0.033 Uiso 1 1 calc R . . H31B H 0.5515 0.9808 0.4468 0.033 Uiso 1 1 calc R . . C32 C 0.3519(4) 0.9791(2) 0.4356(2) 0.0167(10) Uani 1 1 d . . . C33 C 0.3229(5) 1.0536(3) 0.4679(2) 0.0252(12) Uani 1 1 d . . . H33A H 0.2435 1.0753 0.4514 0.038 Uiso 1 1 calc R . . H33B H 0.3945 1.0886 0.4615 0.038 Uiso 1 1 calc R . . H33C H 0.3121 1.0444 0.5115 0.038 Uiso 1 1 calc R . . C34 C 0.3665(5) 0.9984(3) 0.3686(2) 0.0254(12) Uani 1 1 d . . . H34A H 0.4029 0.9552 0.3470 0.038 Uiso 1 1 calc R . . H34B H 0.4242 1.0417 0.3643 0.038 Uiso 1 1 calc R . . H34C H 0.2819 1.0107 0.3516 0.038 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 0.0240(3) 0.0109(3) 0.0153(3) -0.0001(2) 0.0010(2) 0.0031(2) Zn2 0.0188(3) 0.0094(3) 0.0212(3) -0.0003(2) -0.0034(2) -0.0005(2) Na1 0.0237(10) 0.0118(9) 0.0250(10) -0.0050(8) 0.0034(8) -0.0038(8) Na2 0.0281(10) 0.0151(9) 0.0153(9) 0.0002(7) 0.0010(9) 0.0030(8) O1 0.0255(18) 0.0090(16) 0.0194(17) 0.0007(13) -0.0044(14) 0.0004(13) O2 0.0186(17) 0.0165(17) 0.0200(16) -0.0026(14) 0.0086(14) -0.0022(14) N1 0.039(2) 0.012(2) 0.024(2) 0.0053(18) 0.001(2) 0.0048(19) N2 0.026(2) 0.027(2) 0.031(2) -0.012(2) 0.0105(18) -0.010(2) N3 0.021(2) 0.0112(19) 0.012(2) 0.0021(15) -0.0033(16) 0.0017(16) N4 0.016(2) 0.015(2) 0.021(2) -0.0044(17) 0.0039(16) 0.0018(15) C1 0.012(2) 0.019(3) 0.037(3) 0.003(2) -0.006(2) -0.003(2) C2 0.024(3) 0.054(4) 0.038(3) 0.010(3) -0.002(2) -0.004(3) C3 0.044(4) 0.026(3) 0.104(6) -0.006(4) -0.029(4) -0.008(3) C4 0.029(3) 0.093(6) 0.035(4) 0.021(3) -0.003(3) -0.028(4) C5 0.019(3) 0.027(3) 0.024(3) 0.000(2) -0.007(2) 0.003(2) C6 0.042(4) 0.039(4) 0.033(3) 0.001(3) -0.005(3) 0.020(3) C7 0.046(3) 0.035(3) 0.025(3) 0.009(3) -0.011(3) 0.009(3) C8 0.039(3) 0.043(4) 0.037(3) -0.006(3) -0.008(3) -0.005(3) C9 0.061(4) 0.015(3) 0.019(3) 0.001(2) -0.005(3) 0.006(3) C10 0.043(3) 0.022(3) 0.026(3) 0.006(2) -0.002(3) -0.001(3) C11 0.039(4) 0.075(5) 0.062(5) 0.019(4) 0.001(3) 0.018(4) C12 0.097(6) 0.016(3) 0.043(4) 0.004(3) 0.010(4) 0.004(3) C13 0.024(3) 0.020(3) 0.029(3) -0.005(2) 0.002(2) -0.007(2) C14 0.021(3) 0.019(3) 0.034(3) -0.004(2) 0.005(2) -0.011(2) C15 0.065(4) 0.072(5) 0.034(4) -0.020(3) 0.034(3) -0.040(4) C16 0.023(3) 0.041(4) 0.085(5) -0.019(4) 0.011(3) -0.005(3) C17 0.032(3) 0.021(3) 0.020(3) 0.004(2) 0.004(2) 0.002(2) C18 0.032(3) 0.015(3) 0.034(3) 0.009(2) 0.000(2) 0.001(2) C19 0.016(2) 0.011(2) 0.019(2) -0.0006(19) -0.0024(18) -0.0018(18) C20 0.024(3) 0.013(2) 0.032(3) 0.005(2) -0.004(2) -0.005(2) C21 0.018(3) 0.025(3) 0.036(3) 0.002(2) 0.002(2) 0.005(2) C22 0.021(3) 0.021(3) 0.025(3) 0.000(2) 0.009(2) 0.000(2) C23 0.022(3) 0.019(3) 0.018(2) -0.004(2) -0.001(2) -0.006(2) C24 0.037(3) 0.025(3) 0.018(3) 0.000(2) 0.001(2) 0.005(3) C25 0.030(3) 0.027(3) 0.032(3) -0.012(2) -0.003(2) 0.003(2) C26 0.027(3) 0.012(3) 0.040(3) -0.006(2) 0.011(2) -0.002(2) C27 0.056(4) 0.018(3) 0.023(3) -0.006(2) 0.006(2) -0.003(3) C28 0.028(3) 0.008(2) 0.022(3) -0.0007(18) 0.004(2) 0.0055(18) C29 0.048(4) 0.016(3) 0.029(3) -0.002(2) 0.007(2) 0.007(2) C30 0.029(3) 0.023(3) 0.053(3) 0.008(3) -0.001(3) 0.007(3) C31 0.029(3) 0.024(3) 0.031(3) 0.004(2) 0.005(2) -0.005(2) C32 0.019(2) 0.009(2) 0.022(3) 0.000(2) 0.005(2) 0.0017(18) C33 0.035(3) 0.012(3) 0.028(3) -0.003(2) 0.004(2) -0.003(2) C34 0.033(3) 0.017(3) 0.026(3) 0.000(2) 0.007(2) -0.002(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O2 2.025(3) . ? Zn1 N4 1.967(4) . ? Zn1 C5 2.003(5) . ? Zn2 O1 2.036(3) . ? Zn2 N3 1.968(4) . ? Zn2 C1 2.013(5) . ? Na1 O1 2.280(4) . ? Na1 O2 2.328(4) . ? Na1 N2 2.406(5) . ? Na1 N3 2.413(4) . ? Na2 O1 2.309(4) . ? Na2 O2 2.289(4) . ? Na2 N1 2.424(4) . ? Na2 N4 2.436(4) . ? O1 C9 1.412(6) . ? O2 C13 1.404(6) . ? N1 C10 1.479(7) . ? N1 C11 1.429(8) . ? N1 C12 1.465(7) . ? N2 C14 1.468(7) . ? N2 C15 1.453(7) . ? N2 C16 1.463(8) . ? N3 C19 1.478(6) . ? N3 C23 1.483(6) . ? N4 C28 1.495(6) . ? N4 C32 1.471(6) . ? C1 C2 1.505(7) . ? C1 C3 1.535(8) . ? C1 C4 1.504(8) . ? C2 H2A 0.980 . ? C2 H2B 0.980 . ? C2 H2C 0.980 . ? C3 H3A 0.980 . ? C3 H3B 0.980 . ? C3 H3C 0.980 . ? C4 H4A 0.980 . ? C4 H4B 0.980 . ? C4 H4C 0.980 . ? C5 C6 1.528(7) . ? C5 C7 1.511(7) . ? C5 C8 1.536(8) . ? C6 H6A 0.980 . ? C6 H6B 0.980 . ? C6 H6C 0.980 . ? C7 H7A 0.980 . ? C7 H7B 0.980 . ? C7 H7C 0.980 . ? C8 H8A 0.980 . ? C8 H8B 0.980 . ? C8 H8C 0.980 . ? C9 H9A 0.990 . ? C9 H9B 0.990 . ? C9 C10 1.518(7) . ? C10 H10A 0.990 . ? C10 H10B 0.990 . ? C11 H11A 0.980 . ? C11 H11B 0.980 . ? C11 H11C 0.980 . ? C12 H12A 0.980 . ? C12 H12B 0.980 . ? C12 H12C 0.980 . ? C13 H13A 0.990 . ? C13 H13B 0.990 . ? C13 C14 1.510(7) . ? C14 H14A 0.990 . ? C14 H14B 0.990 . ? C15 H15A 0.980 . ? C15 H15B 0.980 . ? C15 H15C 0.980 . ? C16 H16A 0.980 . ? C16 H16B 0.980 . ? C16 H16C 0.980 . ? C17 H17A 0.980 . ? C17 H17B 0.980 . ? C17 H17C 0.980 . ? C17 C19 1.525(7) . ? C18 H18A 0.980 . ? C18 H18B 0.980 . ? C18 H18C 0.980 . ? C18 C19 1.538(7) . ? C19 C20 1.520(7) . ? C20 H20A 0.990 . ? C20 H20B 0.990 . ? C20 C21 1.524(7) . ? C21 H21A 0.990 . ? C21 H21B 0.990 . ? C21 C22 1.515(7) . ? C22 H22A 0.990 . ? C22 H22B 0.990 . ? C22 C23 1.531(7) . ? C23 C24 1.527(7) . ? C23 C25 1.554(7) . ? C24 H24A 0.980 . ? C24 H24B 0.980 . ? C24 H24C 0.980 . ? C25 H25A 0.980 . ? C25 H25B 0.980 . ? C25 H25C 0.980 . ? C26 H26A 0.980 . ? C26 H26B 0.980 . ? C26 H26C 0.980 . ? C26 C28 1.514(7) . ? C27 H27A 0.980 . ? C27 H27B 0.980 . ? C27 H27C 0.980 . ? C27 C28 1.542(7) . ? C28 C29 1.528(7) . ? C29 H29A 0.990 . ? C29 H29B 0.990 . ? C29 C30 1.505(8) . ? C30 H30A 0.990 . ? C30 H30B 0.990 . ? C30 C31 1.542(8) . ? C31 H31A 0.990 . ? C31 H31B 0.990 . ? C31 C32 1.540(7) . ? C32 C33 1.534(6) . ? C32 C34 1.523(7) . ? C33 H33A 0.980 . ? C33 H33B 0.980 . ? C33 H33C 0.980 . ? C34 H34A 0.980 . ? C34 H34B 0.980 . ? C34 H34C 0.980 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Zn1 N4 101.08(15) . . ? O2 Zn1 C5 114.50(18) . . ? N4 Zn1 C5 144.31(19) . . ? O1 Zn2 N3 101.70(14) . . ? O1 Zn2 C1 116.38(17) . . ? N3 Zn2 C1 141.75(18) . . ? O1 Na1 O2 95.78(13) . . ? O1 Na1 N2 123.70(16) . . ? O1 Na1 N3 82.82(13) . . ? O2 Na1 N2 78.58(14) . . ? O2 Na1 N3 142.96(14) . . ? N2 Na1 N3 132.41(16) . . ? O1 Na2 O2 96.06(13) . . ? O1 Na2 N1 79.28(13) . . ? O1 Na2 N4 143.92(14) . . ? O2 Na2 N1 126.28(16) . . ? O2 Na2 N4 81.38(13) . . ? N1 Na2 N4 130.85(15) . . ? Zn2 O1 Na1 88.33(12) . . ? Zn2 O1 Na2 133.08(16) . . ? Zn2 O1 C9 113.7(3) . . ? Na1 O1 Na2 84.34(12) . . ? Na1 O1 C9 125.4(3) . . ? Na2 O1 C9 108.1(3) . . ? Zn1 O2 Na1 129.70(16) . . ? Zn1 O2 Na2 88.83(12) . . ? Zn1 O2 C13 112.4(3) . . ? Na1 O2 Na2 83.70(12) . . ? Na1 O2 C13 107.0(3) . . ? Na2 O2 C13 136.1(3) . . ? Na2 N1 C10 95.4(3) . . ? Na2 N1 C11 114.6(4) . . ? Na2 N1 C12 115.0(4) . . ? C10 N1 C11 112.3(5) . . ? C10 N1 C12 108.7(4) . . ? C11 N1 C12 110.0(5) . . ? Na1 N2 C14 101.2(3) . . ? Na1 N2 C15 122.5(4) . . ? Na1 N2 C16 102.9(3) . . ? C14 N2 C15 109.0(5) . . ? C14 N2 C16 110.3(4) . . ? C15 N2 C16 110.3(5) . . ? Zn2 N3 Na1 86.23(14) . . ? Zn2 N3 C19 115.7(3) . . ? Zn2 N3 C23 112.7(3) . . ? Na1 N3 C19 110.1(3) . . ? Na1 N3 C23 112.0(3) . . ? C19 N3 C23 116.3(4) . . ? Zn1 N4 Na2 86.12(14) . . ? Zn1 N4 C28 113.2(3) . . ? Zn1 N4 C32 117.6(3) . . ? Na2 N4 C28 109.6(3) . . ? Na2 N4 C32 108.8(3) . . ? C28 N4 C32 116.9(3) . . ? Zn2 C1 C2 111.7(4) . . ? Zn2 C1 C3 112.4(4) . . ? Zn2 C1 C4 107.4(4) . . ? C2 C1 C3 106.1(5) . . ? C2 C1 C4 108.3(5) . . ? C3 C1 C4 110.9(5) . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2B 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3B 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C1 C4 H4A 109.5 . . ? C1 C4 H4B 109.5 . . ? C1 C4 H4C 109.5 . . ? H4A C4 H4B 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? Zn1 C5 C6 111.6(3) . . ? Zn1 C5 C7 111.6(4) . . ? Zn1 C5 C8 109.0(4) . . ? C6 C5 C7 108.2(5) . . ? C6 C5 C8 108.1(5) . . ? C7 C5 C8 108.2(4) . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6B 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C5 C7 H7A 109.5 . . ? C5 C7 H7B 109.5 . . ? C5 C7 H7C 109.5 . . ? H7A C7 H7B 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C5 C8 H8A 109.5 . . ? C5 C8 H8B 109.5 . . ? C5 C8 H8C 109.5 . . ? H8A C8 H8B 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? O1 C9 H9A 108.8 . . ? O1 C9 H9B 108.8 . . ? O1 C9 C10 113.7(4) . . ? H9A C9 H9B 107.7 . . ? H9A C9 C10 108.8 . . ? H9B C9 C10 108.8 . . ? N1 C10 C9 114.7(4) . . ? N1 C10 H10A 108.6 . . ? N1 C10 H10B 108.6 . . ? C9 C10 H10A 108.6 . . ? C9 C10 H10B 108.6 . . ? H10A C10 H10B 107.6 . . ? N1 C11 H11A 109.5 . . ? N1 C11 H11B 109.5 . . ? N1 C11 H11C 109.5 . . ? H11A C11 H11B 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N1 C12 H12A 109.5 . . ? N1 C12 H12B 109.5 . . ? N1 C12 H12C 109.5 . . ? H12A C12 H12B 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? O2 C13 H13A 108.7 . . ? O2 C13 H13B 108.7 . . ? O2 C13 C14 114.1(4) . . ? H13A C13 H13B 107.6 . . ? H13A C13 C14 108.7 . . ? H13B C13 C14 108.7 . . ? N2 C14 C13 114.2(4) . . ? N2 C14 H14A 108.7 . . ? N2 C14 H14B 108.7 . . ? C13 C14 H14A 108.7 . . ? C13 C14 H14B 108.7 . . ? H14A C14 H14B 107.6 . . ? N2 C15 H15A 109.5 . . ? N2 C15 H15B 109.5 . . ? N2 C15 H15C 109.5 . . ? H15A C15 H15B 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N2 C16 H16A 109.5 . . ? N2 C16 H16B 109.5 . . ? N2 C16 H16C 109.5 . . ? H16A C16 H16B 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? H17A C17 H17B 109.5 . . ? H17A C17 H17C 109.5 . . ? H17A C17 C19 109.5 . . ? H17B C17 H17C 109.5 . . ? H17B C17 C19 109.5 . . ? H17C C17 C19 109.5 . . ? H18A C18 H18B 109.5 . . ? H18A C18 H18C 109.5 . . ? H18A C18 C19 109.5 . . ? H18B C18 H18C 109.5 . . ? H18B C18 C19 109.5 . . ? H18C C18 C19 109.5 . . ? N3 C19 C17 106.5(4) . . ? N3 C19 C18 115.6(4) . . ? N3 C19 C20 110.3(4) . . ? C17 C19 C18 105.8(4) . . ? C17 C19 C20 108.1(4) . . ? C18 C19 C20 110.1(4) . . ? C19 C20 H20A 109.1 . . ? C19 C20 H20B 109.1 . . ? C19 C20 C21 112.7(4) . . ? H20A C20 H20B 107.8 . . ? H20A C20 C21 109.1 . . ? H20B C20 C21 109.1 . . ? C20 C21 H21A 110.0 . . ? C20 C21 H21B 110.0 . . ? C20 C21 C22 108.6(4) . . ? H21A C21 H21B 108.4 . . ? H21A C21 C22 110.0 . . ? H21B C21 C22 110.0 . . ? C21 C22 H22A 109.0 . . ? C21 C22 H22B 109.0 . . ? C21 C22 C23 112.9(4) . . ? H22A C22 H22B 107.8 . . ? H22A C22 C23 109.0 . . ? H22B C22 C23 109.0 . . ? N3 C23 C22 110.2(4) . . ? N3 C23 C24 107.0(4) . . ? N3 C23 C25 115.2(4) . . ? C22 C23 C24 107.5(4) . . ? C22 C23 C25 110.2(4) . . ? C24 C23 C25 106.4(4) . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24B 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C23 C25 H25A 109.5 . . ? C23 C25 H25B 109.5 . . ? C23 C25 H25C 109.5 . . ? H25A C25 H25B 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? H26A C26 H26B 109.5 . . ? H26A C26 H26C 109.5 . . ? H26A C26 C28 109.5 . . ? H26B C26 H26C 109.5 . . ? H26B C26 C28 109.5 . . ? H26C C26 C28 109.5 . . ? H27A C27 H27B 109.5 . . ? H27A C27 H27C 109.5 . . ? H27A C27 C28 109.5 . . ? H27B C27 H27C 109.5 . . ? H27B C27 C28 109.5 . . ? H27C C27 C28 109.5 . . ? N4 C28 C26 107.4(4) . . ? N4 C28 C27 114.8(4) . . ? N4 C28 C29 108.9(4) . . ? C26 C28 C27 106.8(4) . . ? C26 C28 C29 109.4(4) . . ? C27 C28 C29 109.3(4) . . ? C28 C29 H29A 108.6 . . ? C28 C29 H29B 108.6 . . ? C28 C29 C30 114.8(4) . . ? H29A C29 H29B 107.5 . . ? H29A C29 C30 108.6 . . ? H29B C29 C30 108.6 . . ? C29 C30 H30A 109.9 . . ? C29 C30 H30B 109.9 . . ? C29 C30 C31 109.0(5) . . ? H30A C30 H30B 108.3 . . ? H30A C30 C31 109.9 . . ? H30B C30 C31 109.9 . . ? C30 C31 H31A 109.3 . . ? C30 C31 H31B 109.3 . . ? C30 C31 C32 111.7(4) . . ? H31A C31 H31B 107.9 . . ? H31A C31 C32 109.3 . . ? H31B C31 C32 109.3 . . ? N4 C32 C31 109.6(4) . . ? N4 C32 C33 106.0(4) . . ? N4 C32 C34 116.8(4) . . ? C31 C32 C33 108.1(4) . . ? C31 C32 C34 109.9(4) . . ? C33 C32 C34 105.9(4) . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? C32 C33 H33C 109.5 . . ? H33A C33 H33B 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C32 C34 H34A 109.5 . . ? C32 C34 H34B 109.5 . . ? C32 C34 H34C 109.5 . . ? H34A C34 H34B 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.046 _refine_diff_density_min -0.514 _refine_diff_density_rms 0.093 #===END