# Electronic Supplementary Material (ESI) for Chemical Science # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_vb15 #TrackingRef 'hevia5.cif' #--------------------------------------------------------------------- #---------- COMPOUND 2--------------------------------------------- #--------------------------------------------------------------------- _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C47 H77 N2 Na O3 Zn' _chemical_formula_weight 806.47 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M P212121 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 11.9480(6) _cell_length_b 15.8780(8) _cell_length_c 24.9404(11) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4731.5(4) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 8572 _cell_measurement_theta_min 3.0356 _cell_measurement_theta_max 28.8594 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.132 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1752 _exptl_absorpt_coefficient_mu 0.567 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.67848 _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 'OD Xcalibur, Eos' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30717 _diffrn_reflns_av_R_equivalents 0.0552 _diffrn_reflns_av_sigmaI/netI 0.0883 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 3.04 _diffrn_reflns_theta_max 28.00 _reflns_number_total 10854 _reflns_number_gt 7909 _reflns_threshold_expression I>2\s(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; 3 THF modelled as disordered. 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^ > 2\s(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^)+(0.0310P)^2^+1.8399P] 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 0.143(11) _refine_ls_number_reflns 10854 _refine_ls_number_parameters 493 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0928 _refine_ls_R_factor_gt 0.0557 _refine_ls_wR_factor_ref 0.1010 _refine_ls_wR_factor_gt 0.0895 _refine_ls_goodness_of_fit_ref 1.011 _refine_ls_restrained_S_all 1.014 _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 0.35903(3) 1.00978(2) -0.039365(14) 0.02458(9) Uani 1 1 d . . . Na1 Na 0.71210(11) 1.03879(9) 0.16128(5) 0.0370(3) Uani 1 1 d . . . O1 O 0.8096(2) 0.91045(17) 0.16689(11) 0.0537(8) Uani 1 1 d . C . O2 O 0.6965(2) 1.07664(19) 0.25038(10) 0.0524(8) Uani 1 1 d . A . O3 O 0.8800(2) 1.10977(15) 0.15395(11) 0.0480(7) Uani 1 1 d . D . N1 N 0.4379(2) 1.10294(15) 0.11524(9) 0.0199(6) Uani 1 1 d . . . N2 N 0.5312(2) 1.04500(14) 0.05344(9) 0.0194(6) Uani 1 1 d . . . C1 C 0.5407(3) 1.06898(18) 0.10637(12) 0.0207(7) Uani 1 1 d . . . C3 C 0.3694(3) 1.09697(18) 0.06973(11) 0.0205(7) Uani 1 1 d . C . C2 C 0.4255(2) 1.06014(18) 0.02968(12) 0.0208(7) Uani 1 1 d . C . C4 C 0.3968(2) 1.1285(2) 0.16710(12) 0.0222(7) Uani 1 1 d . . . C5 C 0.3978(3) 1.2143(2) 0.17997(12) 0.0262(8) Uani 1 1 d . . . C6 C 0.3575(3) 1.2370(2) 0.23039(12) 0.0326(8) Uani 1 1 d . . . H6 H 0.3592 1.2944 0.2411 0.039 Uiso 1 1 calc R . . C7 C 0.3152(3) 1.1770(3) 0.26497(14) 0.0422(10) Uani 1 1 d . . . H7 H 0.2874 1.1936 0.2991 0.051 Uiso 1 1 calc R C . C8 C 0.3128(3) 1.0935(2) 0.25052(13) 0.0380(9) Uani 1 1 d . . . H8 H 0.2824 1.0532 0.2747 0.046 Uiso 1 1 calc R . . C9 C 0.3541(3) 1.06677(19) 0.20127(12) 0.0275(7) Uani 1 1 d . . . C10 C 0.4472(3) 1.2784(2) 0.14164(13) 0.0337(8) Uani 1 1 d . . . H10 H 0.4333 1.2575 0.1044 0.040 Uiso 1 1 calc R . . C11 C 0.3933(4) 1.3657(2) 0.14594(15) 0.0487(11) Uani 1 1 d . . . H11A H 0.4112 1.3905 0.1809 0.073 Uiso 1 1 calc R C . H11B H 0.3119 1.3604 0.1423 0.073 Uiso 1 1 calc R . . H11C H 0.4222 1.4020 0.1174 0.073 Uiso 1 1 calc R . . C12 C 0.5734(3) 1.2842(2) 0.14903(16) 0.0493(11) Uani 1 1 d . . . H12A H 0.6073 1.2291 0.1419 0.074 Uiso 1 1 calc R C . H12B H 0.5902 1.3013 0.1859 0.074 Uiso 1 1 calc R . . H12C H 0.6040 1.3259 0.1241 0.074 Uiso 1 1 calc R . . C13 C 0.3550(3) 0.97372(19) 0.18628(12) 0.0334(8) Uani 1 1 d . . . H13 H 0.3830 0.9690 0.1486 0.040 Uiso 1 1 calc R . . C14 C 0.4364(4) 0.9262(3) 0.22247(17) 0.0578(12) Uani 1 1 d . . . H14A H 0.4111 0.9302 0.2598 0.087 Uiso 1 1 calc R C . H14B H 0.5112 0.9510 0.2192 0.087 Uiso 1 1 calc R . . H14C H 0.4391 0.8669 0.2117 0.087 Uiso 1 1 calc R . . C15 C 0.2395(3) 0.9346(3) 0.18829(17) 0.0533(11) Uani 1 1 d . . . H15A H 0.1903 0.9636 0.1628 0.080 Uiso 1 1 calc R C . H15B H 0.2090 0.9401 0.2246 0.080 Uiso 1 1 calc R . . H15C H 0.2445 0.8749 0.1788 0.080 Uiso 1 1 calc R . . C16 C 0.2023(3) 0.9615(2) -0.02460(13) 0.0346(9) Uani 1 1 d . . . C17 C 0.1562(4) 0.9078(3) -0.06977(17) 0.0812(17) Uani 1 1 d . . . H17A H 0.1518 0.9416 -0.1026 0.122 Uiso 1 1 calc R . . H17B H 0.0813 0.8877 -0.0602 0.122 Uiso 1 1 calc R . . H17C H 0.2057 0.8595 -0.0757 0.122 Uiso 1 1 calc R . . C18 C 0.1971(3) 0.9102(3) 0.02634(18) 0.0607(13) Uani 1 1 d . . . H18A H 0.2465 0.8611 0.0230 0.091 Uiso 1 1 calc R . . H18B H 0.1201 0.8912 0.0324 0.091 Uiso 1 1 calc R . . H18C H 0.2215 0.9449 0.0567 0.091 Uiso 1 1 calc R . . C19 C 0.1246(3) 1.0366(3) -0.01646(19) 0.0657(13) Uani 1 1 d . . . H19A H 0.0488 1.0164 -0.0088 0.098 Uiso 1 1 calc R . . H19B H 0.1237 1.0710 -0.0491 0.098 Uiso 1 1 calc R . . H19C H 0.1515 1.0705 0.0137 0.098 Uiso 1 1 calc R . . C20 C 0.7149(3) 1.0538(2) 0.01097(12) 0.0250(7) Uani 1 1 d . . . C21 C 0.8008(3) 1.0118(2) -0.01611(12) 0.0365(8) Uani 1 1 d . . . H21 H 0.8653 1.0424 -0.0270 0.044 Uiso 1 1 calc R . . C22 C 0.6224(2) 1.00515(18) 0.02607(10) 0.0216(6) Uani 1 1 d . . . C23 C 0.6144(3) 0.91884(19) 0.01541(13) 0.0286(8) Uani 1 1 d . . . C24 C 0.7022(3) 0.8804(2) -0.01195(14) 0.0389(9) Uani 1 1 d . . . H24 H 0.6989 0.8220 -0.0200 0.047 Uiso 1 1 calc R . . C25 C 0.7940(3) 0.9272(2) -0.02736(14) 0.0439(10) Uani 1 1 d . . . H25 H 0.8535 0.9005 -0.0460 0.053 Uiso 1 1 calc R C . C26 C 0.7226(3) 1.1469(2) 0.02314(13) 0.0286(8) Uani 1 1 d . . . H26 H 0.6970 1.1546 0.0610 0.034 Uiso 1 1 calc R . . C27 C 0.6445(3) 1.1994(2) -0.01210(14) 0.0421(9) Uani 1 1 d . . . H27A H 0.5681 1.1775 -0.0093 0.063 Uiso 1 1 calc R C . H27B H 0.6695 1.1962 -0.0495 0.063 Uiso 1 1 calc R . . H27C H 0.6460 1.2582 -0.0001 0.063 Uiso 1 1 calc R . . C28 C 0.8408(3) 1.1833(2) 0.01958(14) 0.0467(10) Uani 1 1 d . . . H28A H 0.8651 1.1839 -0.0179 0.070 Uiso 1 1 calc R C . H28B H 0.8921 1.1483 0.0407 0.070 Uiso 1 1 calc R . . H28C H 0.8410 1.2409 0.0337 0.070 Uiso 1 1 calc R . . C29 C 0.5166(3) 0.86624(19) 0.03588(16) 0.0366(8) Uani 1 1 d . . . H29 H 0.4525 0.9055 0.0422 0.044 Uiso 1 1 calc R . . C30 C 0.4773(4) 0.7996(2) -0.00385(17) 0.0530(11) Uani 1 1 d . . . H30A H 0.4122 0.7700 0.0109 0.080 Uiso 1 1 calc R C . H30B H 0.5378 0.7592 -0.0103 0.080 Uiso 1 1 calc R . . H30C H 0.4566 0.8267 -0.0377 0.080 Uiso 1 1 calc R . . C31 C 0.5461(4) 0.8268(3) 0.08936(16) 0.0589(12) Uani 1 1 d . . . H31A H 0.5663 0.8711 0.1150 0.088 Uiso 1 1 calc R C . H31B H 0.6096 0.7884 0.0847 0.088 Uiso 1 1 calc R . . H31C H 0.4815 0.7953 0.1030 0.088 Uiso 1 1 calc R . . C32 C 0.4234(3) 1.0167(2) -0.11470(12) 0.0323(8) Uani 1 1 d . . . C33 C 0.5379(3) 1.0590(3) -0.11767(15) 0.0469(10) Uani 1 1 d . . . H33A H 0.5334 1.1153 -0.1017 0.070 Uiso 1 1 calc R . . H33B H 0.5611 1.0637 -0.1552 0.070 Uiso 1 1 calc R . . H33C H 0.5927 1.0251 -0.0979 0.070 Uiso 1 1 calc R . . C34 C 0.4319(3) 0.9309(2) -0.14213(15) 0.0449(10) Uani 1 1 d . . . H34A H 0.4894 0.8970 -0.1243 0.067 Uiso 1 1 calc R . . H34B H 0.4521 0.9387 -0.1799 0.067 Uiso 1 1 calc R . . H34C H 0.3596 0.9019 -0.1398 0.067 Uiso 1 1 calc R . . C35 C 0.3410(3) 1.0708(2) -0.14651(14) 0.0427(10) Uani 1 1 d . . . H35A H 0.3680 1.0772 -0.1834 0.064 Uiso 1 1 calc R . . H35B H 0.3347 1.1264 -0.1297 0.064 Uiso 1 1 calc R . . H35C H 0.2675 1.0434 -0.1468 0.064 Uiso 1 1 calc R . . C36 C 0.6009(5) 1.1063(4) 0.2793(3) 0.0465(16) Uiso 0.67 1 d P A 1 H36A H 0.5652 1.0602 0.2998 0.056 Uiso 0.67 1 calc PR A 1 H36B H 0.5450 1.1315 0.2547 0.056 Uiso 0.67 1 calc PR A 1 C37 C 0.6506(6) 1.1731(5) 0.3170(3) 0.064(2) Uiso 0.67 1 d P A 1 H37A H 0.6413 1.2301 0.3015 0.077 Uiso 0.67 1 calc PR A 1 H37B H 0.6128 1.1714 0.3523 0.077 Uiso 0.67 1 calc PR A 1 C38 C 0.7711(6) 1.1524(5) 0.3228(3) 0.0534(19) Uiso 0.67 1 d P A 1 H38A H 0.8183 1.2004 0.3114 0.064 Uiso 0.67 1 calc PR A 1 H38B H 0.7891 1.1383 0.3605 0.064 Uiso 0.67 1 calc PR A 1 C39 C 0.7894(6) 1.0790(4) 0.2877(3) 0.0414(19) Uiso 0.67 1 d P A 1 H39A H 0.8611 1.0848 0.2681 0.050 Uiso 0.67 1 calc PR A 1 H39B H 0.7919 1.0266 0.3092 0.050 Uiso 0.67 1 calc PR A 1 C40 C 0.8752(3) 0.8830(2) 0.21151(15) 0.0481(10) Uani 1 1 d . . . H40A H 0.8260 0.8610 0.2402 0.058 Uiso 1 1 calc R C . H40B H 0.9191 0.9307 0.2262 0.058 Uiso 1 1 calc R . . C41 C 0.9521(4) 0.8150(3) 0.19196(18) 0.0571(12) Uani 1 1 d D C . H41A H 1.0244 0.8169 0.2114 0.069 Uiso 1 1 calc R B 1 H41B H 0.9180 0.7588 0.1971 0.069 Uiso 1 1 calc R B 1 C42 C 0.9683(5) 0.8325(4) 0.1356(2) 0.0517(15) Uiso 0.75 1 d P C 1 H42A H 0.9917 0.7818 0.1154 0.062 Uiso 0.75 1 calc PR C 1 H42B H 1.0228 0.8785 0.1296 0.062 Uiso 0.75 1 calc PR C 1 C43 C 0.8487(6) 0.8592(3) 0.1219(2) 0.0525(15) Uiso 0.75 1 d P C 1 H43A H 0.8475 0.8923 0.0883 0.063 Uiso 0.75 1 calc PR C 1 H43B H 0.8003 0.8091 0.1173 0.063 Uiso 0.75 1 calc PR C 1 C44 C 0.9869(5) 1.0747(4) 0.1358(3) 0.0475(18) Uiso 0.75 1 d P D 1 H44A H 0.9805 1.0528 0.0988 0.057 Uiso 0.75 1 calc PR D 1 H44B H 1.0116 1.0285 0.1597 0.057 Uiso 0.75 1 calc PR D 1 C45 C 1.0674(5) 1.1476(3) 0.1382(2) 0.0431(14) Uiso 0.75 1 d P D 1 H45A H 1.0707 1.1776 0.1034 0.052 Uiso 0.75 1 calc PR D 1 H45B H 1.1435 1.1285 0.1480 0.052 Uiso 0.75 1 calc PR D 1 C46 C 1.0172(5) 1.2041(4) 0.1822(3) 0.0592(17) Uiso 0.75 1 d PD D 1 H46A H 1.0450 1.2627 0.1798 0.071 Uiso 0.75 1 calc PR D 1 H46B H 1.0317 1.1815 0.2185 0.071 Uiso 0.75 1 calc PR D 1 C47 C 0.8899(5) 1.1972(4) 0.1662(3) 0.047(2) Uiso 0.75 1 d PD D 1 H47A H 0.8405 1.2134 0.1964 0.056 Uiso 0.75 1 calc PR D 1 H47B H 0.8723 1.2327 0.1347 0.056 Uiso 0.75 1 calc PR D 1 C36A C 0.6241(11) 1.1502(8) 0.2677(5) 0.046(3) Uiso 0.33 1 d P A 2 H36C H 0.5474 1.1463 0.2529 0.056 Uiso 0.33 1 calc PR A 2 H36D H 0.6577 1.2050 0.2576 0.056 Uiso 0.33 1 calc PR A 2 C37A C 0.6260(10) 1.1361(8) 0.3292(5) 0.043(3) Uiso 0.33 1 d PD A 2 H37C H 0.5797 1.0874 0.3404 0.052 Uiso 0.33 1 calc PR A 2 H37D H 0.6038 1.1870 0.3495 0.052 Uiso 0.33 1 calc PR A 2 C38A C 0.7550(12) 1.1175(10) 0.3332(7) 0.063(5) Uiso 0.33 1 d PD A 2 H38C H 0.7996 1.1687 0.3254 0.076 Uiso 0.33 1 calc PR A 2 H38D H 0.7753 1.0962 0.3692 0.076 Uiso 0.33 1 calc PR A 2 C39A C 0.7721(11) 1.0527(9) 0.2920(5) 0.034(3) Uiso 0.33 1 d P A 2 H39C H 0.8504 1.0528 0.2789 0.041 Uiso 0.33 1 calc PR A 2 H39D H 0.7538 0.9960 0.3060 0.041 Uiso 0.33 1 calc PR A 2 C44A C 0.9952(15) 1.0823(10) 0.1556(8) 0.045(5) Uiso 0.25 1 d PD D 2 H44C H 1.0159 1.0556 0.1211 0.054 Uiso 0.25 1 calc PR D 2 H44D H 1.0055 1.0403 0.1845 0.054 Uiso 0.25 1 calc PR D 2 C45A C 1.0697(14) 1.1592(9) 0.1659(8) 0.053(5) Uiso 0.25 1 d PD D 2 H45C H 1.1018 1.1564 0.2024 0.064 Uiso 0.25 1 calc PR D 2 H45D H 1.1319 1.1606 0.1397 0.064 Uiso 0.25 1 calc PR D 2 C46A C 1.0031(14) 1.2315(10) 0.1605(8) 0.0592(17) Uiso 0.25 1 d PD D 2 H46C H 0.9958 1.2506 0.1229 0.071 Uiso 0.25 1 calc PR D 2 H46D H 1.0279 1.2785 0.1837 0.071 Uiso 0.25 1 calc PR D 2 C47A C 0.9001(17) 1.1885(15) 0.1809(10) 0.061(8) Uiso 0.25 1 d PD D 2 H47C H 0.9083 1.1781 0.2199 0.073 Uiso 0.25 1 calc PR D 2 H47D H 0.8348 1.2260 0.1757 0.073 Uiso 0.25 1 calc PR D 2 C42A C 0.9297(17) 0.8234(12) 0.1280(6) 0.0517(15) Uiso 0.25 1 d PD C 2 H42C H 1.0023 0.8303 0.1094 0.062 Uiso 0.25 1 calc PR C 2 H42D H 0.8951 0.7706 0.1149 0.062 Uiso 0.25 1 calc PR C 2 C43A C 0.8557(17) 0.8955(10) 0.1138(7) 0.0525(15) Uiso 0.25 1 d PD C 2 H43C H 0.8984 0.9444 0.1003 0.063 Uiso 0.25 1 calc PR C 2 H43D H 0.7973 0.8795 0.0876 0.063 Uiso 0.25 1 calc PR C 2 H2 H 0.296(3) 1.1183(19) 0.0715(12) 0.029(9) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.02066(17) 0.03216(18) 0.02091(16) -0.00467(16) -0.00187(17) -0.00228(17) Na1 0.0243(8) 0.0531(9) 0.0336(8) 0.0021(6) -0.0074(6) 0.0047(6) O1 0.0478(19) 0.0659(19) 0.0475(17) -0.0104(15) -0.0129(14) 0.0176(14) O2 0.0368(16) 0.087(2) 0.0335(15) -0.0171(14) -0.0139(13) 0.0153(15) O3 0.0317(17) 0.0483(15) 0.0639(19) 0.0059(13) 0.0032(14) 0.0029(12) N1 0.0183(14) 0.0283(14) 0.0129(13) -0.0005(11) 0.0002(11) 0.0014(11) N2 0.0166(14) 0.0236(13) 0.0182(14) -0.0013(10) 0.0006(10) 0.0005(10) C1 0.0189(17) 0.0238(16) 0.0194(16) 0.0020(13) 0.0027(13) 0.0001(13) C3 0.0157(18) 0.0281(16) 0.0177(15) 0.0005(12) 0.0013(15) 0.0003(15) C2 0.0153(16) 0.0280(16) 0.0191(17) 0.0006(13) -0.0015(13) -0.0024(13) C4 0.0163(17) 0.0356(18) 0.0146(16) -0.0002(14) 0.0013(13) 0.0059(13) C5 0.0225(19) 0.0393(19) 0.0168(17) -0.0020(14) -0.0028(14) 0.0031(14) C6 0.033(2) 0.0412(19) 0.0239(17) -0.0095(14) -0.0006(18) 0.0065(18) C7 0.038(2) 0.065(3) 0.024(2) -0.0058(19) 0.0090(17) 0.0054(19) C8 0.034(2) 0.057(3) 0.0229(19) 0.0115(17) 0.0085(16) -0.0014(18) C9 0.0198(17) 0.0417(18) 0.0208(16) 0.0055(14) 0.0001(16) 0.0017(17) C10 0.045(2) 0.0331(19) 0.0228(18) -0.0064(15) -0.0005(17) -0.0010(17) C11 0.071(3) 0.038(2) 0.038(2) -0.0027(17) -0.013(2) 0.003(2) C12 0.048(3) 0.045(2) 0.055(3) -0.0113(19) 0.012(2) -0.013(2) C13 0.037(2) 0.0371(19) 0.0263(17) 0.0090(14) 0.0058(17) 0.0018(18) C14 0.073(3) 0.046(3) 0.054(3) 0.015(2) -0.010(2) 0.005(2) C15 0.049(3) 0.055(3) 0.055(3) -0.001(2) 0.010(2) -0.009(2) C16 0.0268(19) 0.043(2) 0.034(2) -0.0038(16) 0.0025(16) -0.0069(15) C17 0.060(3) 0.123(4) 0.061(3) -0.034(3) 0.008(3) -0.054(3) C18 0.041(3) 0.068(3) 0.073(3) 0.014(2) 0.006(2) -0.024(2) C19 0.028(2) 0.064(3) 0.105(4) -0.016(2) -0.013(2) -0.0013(19) C20 0.0182(17) 0.0382(19) 0.0187(17) 0.0013(14) -0.0020(14) 0.0031(14) C21 0.0204(17) 0.059(2) 0.0301(17) 0.0051(18) 0.0033(14) 0.0046(18) C22 0.0170(15) 0.0299(16) 0.0180(14) -0.0022(13) -0.0027(11) 0.0005(14) C23 0.025(2) 0.0327(18) 0.0278(17) -0.0041(14) -0.0038(14) 0.0093(14) C24 0.035(2) 0.041(2) 0.041(2) -0.0092(18) -0.0047(19) 0.0124(18) C25 0.033(2) 0.062(3) 0.038(2) -0.0051(19) 0.0049(18) 0.0225(19) C26 0.0190(18) 0.044(2) 0.0234(18) 0.0031(15) 0.0009(14) -0.0085(14) C27 0.041(2) 0.0374(19) 0.048(2) 0.0005(16) -0.008(2) -0.011(2) C28 0.036(2) 0.065(2) 0.039(2) 0.0016(18) -0.0009(18) -0.023(2) C29 0.035(2) 0.0232(16) 0.052(2) -0.0040(19) 0.000(2) 0.0040(14) C30 0.055(3) 0.037(2) 0.067(3) -0.008(2) -0.018(2) -0.0030(19) C31 0.071(3) 0.057(3) 0.048(3) 0.012(2) 0.001(2) -0.018(2) C32 0.0283(19) 0.046(2) 0.0226(17) -0.0082(17) -0.0037(14) -0.0023(17) C33 0.040(3) 0.073(3) 0.027(2) -0.009(2) 0.0029(18) -0.014(2) C34 0.043(3) 0.053(2) 0.038(2) -0.0150(19) 0.0034(19) 0.004(2) C35 0.049(3) 0.048(2) 0.032(2) -0.0039(17) -0.0039(19) -0.001(2) C40 0.047(3) 0.055(2) 0.042(2) 0.0106(19) 0.005(2) -0.003(2) C41 0.043(3) 0.050(3) 0.078(3) 0.009(2) -0.008(2) 0.002(2) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 C32 2.033(3) . ? Zn1 C16 2.056(3) . ? Zn1 C2 2.058(3) . ? Na1 O3 2.308(3) . ? Na1 O2 2.309(3) . ? Na1 O1 2.352(3) . ? Na1 C1 2.510(3) . ? Na1 C43A 3.086(16) . ? O1 C40 1.429(4) . ? O1 C43A 1.452(17) . ? O1 C43 1.462(6) . ? O2 C39A 1.427(13) . ? O2 C36 1.430(6) . ? O2 C39 1.450(7) . ? O2 C36A 1.516(12) . ? O3 C47 1.427(7) . ? O3 C47A 1.44(2) . ? O3 C44A 1.445(19) . ? O3 C44 1.465(7) . ? N1 C1 1.359(4) . ? N1 C3 1.403(4) . ? N1 C4 1.442(4) . ? N2 C1 1.379(4) . ? N2 C2 1.416(4) . ? N2 C22 1.432(3) . ? C3 C2 1.338(4) . ? C3 H2 0.94(3) . ? C4 C9 1.396(4) . ? C4 C5 1.399(4) . ? C5 C6 1.394(4) . ? C5 C10 1.517(5) . ? C6 C7 1.381(5) . ? C6 H6 0.9500 . ? C7 C8 1.375(5) . ? C7 H7 0.9500 . ? C8 C9 1.390(4) . ? C8 H8 0.9500 . ? C9 C13 1.524(4) . ? C10 C12 1.522(5) . ? C10 C11 1.531(5) . ? C10 H10 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C15 1.514(5) . ? C13 C14 1.526(5) . ? C13 H13 1.0000 . ? 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 C18 1.511(5) . ? C16 C17 1.516(5) . ? C16 C19 1.524(5) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 C21 1.398(4) . ? C20 C22 1.400(4) . ? C20 C26 1.513(4) . ? C21 C25 1.375(5) . ? C21 H21 0.9500 . ? C22 C23 1.399(4) . ? C23 C24 1.392(5) . ? C23 C29 1.524(4) . ? C24 C25 1.379(5) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? C26 C28 1.529(4) . ? C26 C27 1.529(4) . ? C26 H26 1.0000 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 C31 1.515(5) . ? C29 C30 1.524(5) . ? C29 H29 1.0000 . ? 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 1.526(5) . ? C32 C35 1.528(5) . ? C32 C34 1.528(5) . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? 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 1.536(9) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 C38 1.484(9) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 C39 1.473(10) . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 C41 1.500(5) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 C42 1.446(7) . ? C41 C42A 1.623(14) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 C43 1.528(8) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 C45 1.506(8) . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C45 C46 1.539(8) . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C46 C47 1.576(8) . ? C46 H46A 0.9900 . ? C46 H46B 0.9900 . ? C47 H47A 0.9900 . ? C47 H47B 0.9900 . ? C36A C37A 1.552(16) . ? C36A H36C 0.9900 . ? C36A H36D 0.9900 . ? C37A C38A 1.572(14) . ? C37A H37C 0.9900 . ? C37A H37D 0.9900 . ? C38A C39A 1.47(2) . ? C38A H38C 0.9900 . ? C38A H38D 0.9900 . ? C39A H39C 0.9900 . ? C39A H39D 0.9900 . ? C44A C45A 1.532(16) . ? C44A H44C 0.9900 . ? C44A H44D 0.9900 . ? C45A C46A 1.403(16) . ? C45A H45C 0.9900 . ? C45A H45D 0.9900 . ? C46A C47A 1.496(17) . ? C46A H46C 0.9900 . ? C46A H46D 0.9900 . ? C47A H47C 0.9900 . ? C47A H47D 0.9900 . ? C42A C43A 1.489(16) . ? C42A H42C 0.9900 . ? C42A H42D 0.9900 . ? C43A H43C 0.9900 . ? C43A H43D 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 C32 Zn1 C16 122.01(13) . . ? C32 Zn1 C2 127.33(12) . . ? C16 Zn1 C2 110.25(12) . . ? O3 Na1 O2 91.10(10) . . ? O3 Na1 O1 89.84(10) . . ? O2 Na1 O1 102.02(11) . . ? O3 Na1 C1 124.93(11) . . ? O2 Na1 C1 114.17(10) . . ? O1 Na1 C1 127.03(11) . . ? O3 Na1 C43A 81.2(4) . . ? O2 Na1 C43A 127.3(3) . . ? O1 Na1 C43A 26.9(3) . . ? C1 Na1 C43A 112.7(3) . . ? C40 O1 C43A 116.9(7) . . ? C40 O1 C43 104.6(3) . . ? C43A O1 C43 24.4(7) . . ? C40 O1 Na1 125.6(2) . . ? C43A O1 Na1 106.0(6) . . ? C43 O1 Na1 126.5(3) . . ? C39A O2 C36 103.1(6) . . ? C39A O2 C39 19.1(6) . . ? C36 O2 C39 106.2(4) . . ? C39A O2 C36A 111.1(7) . . ? C36 O2 C36A 31.5(5) . . ? C39 O2 C36A 103.5(6) . . ? C39A O2 Na1 125.4(6) . . ? C36 O2 Na1 129.4(3) . . ? C39 O2 Na1 124.3(3) . . ? C36A O2 Na1 121.3(5) . . ? C47 O3 C47A 16.5(11) . . ? C47 O3 C44A 102.1(7) . . ? C47A O3 C44A 95.2(11) . . ? C47 O3 C44 111.3(4) . . ? C47A O3 C44 109.2(9) . . ? C44A O3 C44 20.5(8) . . ? C47 O3 Na1 122.0(3) . . ? C47A O3 Na1 122.2(8) . . ? C44A O3 Na1 132.7(7) . . ? C44 O3 Na1 126.6(3) . . ? C1 N1 C3 111.7(2) . . ? C1 N1 C4 124.4(2) . . ? C3 N1 C4 123.1(2) . . ? C1 N2 C2 115.3(2) . . ? C1 N2 C22 121.1(2) . . ? C2 N2 C22 123.6(2) . . ? N1 C1 N2 101.0(2) . . ? N1 C1 Na1 136.4(2) . . ? N2 C1 Na1 122.5(2) . . ? C2 C3 N1 109.9(3) . . ? C2 C3 H2 131.3(18) . . ? N1 C3 H2 118.8(18) . . ? C3 C2 N2 102.1(3) . . ? C3 C2 Zn1 127.0(2) . . ? N2 C2 Zn1 128.9(2) . . ? C9 C4 C5 123.1(3) . . ? C9 C4 N1 118.3(3) . . ? C5 C4 N1 118.5(3) . . ? C6 C5 C4 117.2(3) . . ? C6 C5 C10 121.9(3) . . ? C4 C5 C10 120.8(3) . . ? C7 C6 C5 120.7(3) . . ? C7 C6 H6 119.6 . . ? C5 C6 H6 119.6 . . ? C8 C7 C6 120.6(3) . . ? C8 C7 H7 119.7 . . ? C6 C7 H7 119.7 . . ? C7 C8 C9 121.2(3) . . ? C7 C8 H8 119.4 . . ? C9 C8 H8 119.4 . . ? C8 C9 C4 117.1(3) . . ? C8 C9 C13 121.0(3) . . ? C4 C9 C13 121.9(3) . . ? C5 C10 C12 110.5(3) . . ? C5 C10 C11 113.5(3) . . ? C12 C10 C11 110.7(3) . . ? C5 C10 H10 107.3 . . ? C12 C10 H10 107.3 . . ? C11 C10 H10 107.3 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C15 C13 C9 112.5(3) . . ? C15 C13 C14 111.0(3) . . ? C9 C13 C14 109.8(3) . . ? C15 C13 H13 107.8 . . ? C9 C13 H13 107.8 . . ? C14 C13 H13 107.8 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C18 C16 C17 107.9(3) . . ? C18 C16 C19 106.5(3) . . ? C17 C16 C19 108.5(3) . . ? C18 C16 Zn1 112.9(2) . . ? C17 C16 Zn1 114.0(2) . . ? C19 C16 Zn1 106.7(2) . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C16 C19 H19A 109.5 . . ? C16 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C16 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C21 C20 C22 116.6(3) . . ? C21 C20 C26 121.2(3) . . ? C22 C20 C26 122.2(3) . . ? C25 C21 C20 121.4(3) . . ? C25 C21 H21 119.3 . . ? C20 C21 H21 119.3 . . ? C23 C22 C20 122.9(3) . . ? C23 C22 N2 118.1(2) . . ? C20 C22 N2 119.0(3) . . ? C24 C23 C22 118.1(3) . . ? C24 C23 C29 120.1(3) . . ? C22 C23 C29 121.7(3) . . ? C25 C24 C23 120.0(3) . . ? C25 C24 H24 120.0 . . ? C23 C24 H24 120.0 . . ? C21 C25 C24 121.1(3) . . ? C21 C25 H25 119.5 . . ? C24 C25 H25 119.5 . . ? C20 C26 C28 114.4(3) . . ? C20 C26 C27 112.4(3) . . ? C28 C26 C27 108.9(3) . . ? C20 C26 H26 106.9 . . ? C28 C26 H26 106.9 . . ? C27 C26 H26 106.9 . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C26 C28 H28A 109.5 . . ? C26 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C26 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C31 C29 C23 110.1(3) . . ? C31 C29 C30 110.9(3) . . ? C23 C29 C30 113.5(3) . . ? C31 C29 H29 107.4 . . ? C23 C29 H29 107.4 . . ? C30 C29 H29 107.4 . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C29 C31 H31A 109.5 . . ? C29 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C29 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C33 C32 C35 107.8(3) . . ? C33 C32 C34 108.2(3) . . ? C35 C32 C34 108.1(3) . . ? C33 C32 Zn1 114.1(2) . . ? C35 C32 Zn1 105.4(2) . . ? C34 C32 Zn1 113.0(2) . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C32 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C32 C34 H34A 109.5 . . ? C32 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C32 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C32 C35 H35A 109.5 . . ? C32 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C32 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? O2 C36 C37 103.1(5) . . ? O2 C36 H36A 111.1 . . ? C37 C36 H36A 111.1 . . ? O2 C36 H36B 111.1 . . ? C37 C36 H36B 111.1 . . ? H36A C36 H36B 109.1 . . ? C38 C37 C36 106.4(6) . . ? C38 C37 H37A 110.4 . . ? C36 C37 H37A 110.4 . . ? C38 C37 H37B 110.4 . . ? C36 C37 H37B 110.4 . . ? H37A C37 H37B 108.6 . . ? C39 C38 C37 105.1(6) . . ? C39 C38 H38A 110.7 . . ? C37 C38 H38A 110.7 . . ? C39 C38 H38B 110.7 . . ? C37 C38 H38B 110.7 . . ? H38A C38 H38B 108.8 . . ? O2 C39 C38 106.8(5) . . ? O2 C39 H39A 110.4 . . ? C38 C39 H39A 110.4 . . ? O2 C39 H39B 110.4 . . ? C38 C39 H39B 110.4 . . ? H39A C39 H39B 108.6 . . ? O1 C40 C41 107.6(3) . . ? O1 C40 H40A 110.2 . . ? C41 C40 H40A 110.2 . . ? O1 C40 H40B 110.2 . . ? C41 C40 H40B 110.2 . . ? H40A C40 H40B 108.5 . . ? C42 C41 C40 105.1(4) . . ? C42 C41 C42A 18.3(8) . . ? C40 C41 C42A 99.2(7) . . ? C42 C41 H41A 110.7 . . ? C40 C41 H41A 110.7 . . ? C42A C41 H41A 128.5 . . ? C42 C41 H41B 110.7 . . ? C40 C41 H41B 110.7 . . ? C42A C41 H41B 97.6 . . ? H41A C41 H41B 108.8 . . ? C41 C42 C43 98.3(5) . . ? C41 C42 H42A 112.1 . . ? C43 C42 H42A 112.1 . . ? C41 C42 H42B 112.1 . . ? C43 C42 H42B 112.1 . . ? H42A C42 H42B 109.7 . . ? O1 C43 C42 106.4(5) . . ? O1 C43 H43A 110.4 . . ? C42 C43 H43A 110.4 . . ? O1 C43 H43B 110.4 . . ? C42 C43 H43B 110.4 . . ? H43A C43 H43B 108.6 . . ? O3 C44 C45 104.7(4) . . ? O3 C44 H44A 110.8 . . ? C45 C44 H44A 110.8 . . ? O3 C44 H44B 110.8 . . ? C45 C44 H44B 110.8 . . ? H44A C44 H44B 108.9 . . ? C44 C45 C46 103.1(5) . . ? C44 C45 H45A 111.1 . . ? C46 C45 H45A 111.1 . . ? C44 C45 H45B 111.1 . . ? C46 C45 H45B 111.1 . . ? H45A C45 H45B 109.1 . . ? C45 C46 C47 99.0(5) . . ? C45 C46 H46A 112.0 . . ? C47 C46 H46A 112.0 . . ? C45 C46 H46B 112.0 . . ? C47 C46 H46B 112.0 . . ? H46A C46 H46B 109.7 . . ? O3 C47 C46 101.6(5) . . ? O3 C47 H47A 111.4 . . ? C46 C47 H47A 111.4 . . ? O3 C47 H47B 111.4 . . ? C46 C47 H47B 111.4 . . ? H47A C47 H47B 109.3 . . ? O2 C36A C37A 99.3(8) . . ? O2 C36A H36C 111.9 . . ? C37A C36A H36C 111.9 . . ? O2 C36A H36D 111.9 . . ? C37A C36A H36D 111.9 . . ? H36C C36A H36D 109.6 . . ? C36A C37A C38A 96.0(10) . . ? C36A C37A H37C 112.6 . . ? C38A C37A H37C 112.6 . . ? C36A C37A H37D 112.6 . . ? C38A C37A H37D 112.6 . . ? H37C C37A H37D 110.1 . . ? C39A C38A C37A 102.9(11) . . ? C39A C38A H38C 111.2 . . ? C37A C38A H38C 111.2 . . ? C39A C38A H38D 111.2 . . ? C37A C38A H38D 111.2 . . ? H38C C38A H38D 109.1 . . ? O2 C39A C38A 103.5(10) . . ? O2 C39A H39C 111.1 . . ? C38A C39A H39C 111.1 . . ? O2 C39A H39D 111.1 . . ? C38A C39A H39D 111.1 . . ? H39C C39A H39D 109.0 . . ? O3 C44A C45A 108.5(13) . . ? O3 C44A H44C 110.0 . . ? C45A C44A H44C 110.0 . . ? O3 C44A H44D 110.0 . . ? C45A C44A H44D 110.0 . . ? H44C C44A H44D 108.4 . . ? C46A C45A C44A 107.9(14) . . ? C46A C45A H45C 110.1 . . ? C44A C45A H45C 110.1 . . ? C46A C45A H45D 110.1 . . ? C44A C45A H45D 110.1 . . ? H45C C45A H45D 108.4 . . ? C45A C46A C47A 93.5(16) . . ? C45A C46A H46C 113.0 . . ? C47A C46A H46C 113.0 . . ? C45A C46A H46D 113.0 . . ? C47A C46A H46D 113.0 . . ? H46C C46A H46D 110.4 . . ? O3 C47A C46A 112.0(16) . . ? O3 C47A H47C 109.2 . . ? C46A C47A H47C 109.2 . . ? O3 C47A H47D 109.2 . . ? C46A C47A H47D 109.2 . . ? H47C C47A H47D 107.9 . . ? C43A C42A C41 113.2(12) . . ? C43A C42A H42C 108.9 . . ? C41 C42A H42C 108.9 . . ? C43A C42A H42D 108.9 . . ? C41 C42A H42D 108.9 . . ? H42C C42A H42D 107.7 . . ? O1 C43A C42A 97.7(12) . . ? O1 C43A Na1 47.1(5) . . ? C42A C43A Na1 143.7(11) . . ? O1 C43A H43C 112.2 . . ? C42A C43A H43C 112.2 . . ? Na1 C43A H43C 80.7 . . ? O1 C43A H43D 112.2 . . ? C42A C43A H43D 112.2 . . ? Na1 C43A H43D 93.0 . . ? H43C C43A H43D 109.8 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O3 Na1 O1 C40 71.0(3) . . . . ? O2 Na1 O1 C40 -20.1(3) . . . . ? C1 Na1 O1 C40 -153.3(3) . . . . ? C43A Na1 O1 C40 141.5(9) . . . . ? O3 Na1 O1 C43A -70.5(9) . . . . ? O2 Na1 O1 C43A -161.6(9) . . . . ? C1 Na1 O1 C43A 65.1(9) . . . . ? O3 Na1 O1 C43 -85.4(4) . . . . ? O2 Na1 O1 C43 -176.5(4) . . . . ? C1 Na1 O1 C43 50.3(4) . . . . ? C43A Na1 O1 C43 -14.8(10) . . . . ? O3 Na1 O2 C39A -62.7(7) . . . . ? O1 Na1 O2 C39A 27.3(8) . . . . ? C1 Na1 O2 C39A 167.7(7) . . . . ? C43A Na1 O2 C39A 17.0(9) . . . . ? O3 Na1 O2 C36 136.5(4) . . . . ? O1 Na1 O2 C36 -133.4(4) . . . . ? C1 Na1 O2 C36 7.0(4) . . . . ? C43A Na1 O2 C36 -143.7(6) . . . . ? O3 Na1 O2 C39 -39.4(4) . . . . ? O1 Na1 O2 C39 50.7(4) . . . . ? C1 Na1 O2 C39 -168.9(4) . . . . ? C43A Na1 O2 C39 40.3(6) . . . . ? O3 Na1 O2 C36A 98.9(6) . . . . ? O1 Na1 O2 C36A -171.0(6) . . . . ? C1 Na1 O2 C36A -30.6(7) . . . . ? C43A Na1 O2 C36A 178.6(8) . . . . ? O2 Na1 O3 C47 -56.9(4) . . . . ? O1 Na1 O3 C47 -158.9(4) . . . . ? C1 Na1 O3 C47 64.0(5) . . . . ? C43A Na1 O3 C47 175.5(5) . . . . ? O2 Na1 O3 C47A -37.4(13) . . . . ? O1 Na1 O3 C47A -139.4(13) . . . . ? C1 Na1 O3 C47A 83.4(13) . . . . ? C43A Na1 O3 C47A -165.0(13) . . . . ? O2 Na1 O3 C44A 99.1(11) . . . . ? O1 Na1 O3 C44A -3.0(11) . . . . ? C1 Na1 O3 C44A -140.1(11) . . . . ? C43A Na1 O3 C44A -28.5(11) . . . . ? O2 Na1 O3 C44 124.6(4) . . . . ? O1 Na1 O3 C44 22.5(4) . . . . ? C1 Na1 O3 C44 -114.6(4) . . . . ? C43A Na1 O3 C44 -3.0(5) . . . . ? C3 N1 C1 N2 1.7(3) . . . . ? C4 N1 C1 N2 171.5(3) . . . . ? C3 N1 C1 Na1 -174.2(2) . . . . ? C4 N1 C1 Na1 -4.4(5) . . . . ? C2 N2 C1 N1 -2.1(3) . . . . ? C22 N2 C1 N1 179.9(2) . . . . ? C2 N2 C1 Na1 174.60(18) . . . . ? C22 N2 C1 Na1 -3.4(4) . . . . ? O3 Na1 C1 N1 -109.6(3) . . . . ? O2 Na1 C1 N1 0.2(3) . . . . ? O1 Na1 C1 N1 128.9(3) . . . . ? C43A Na1 C1 N1 155.3(5) . . . . ? O3 Na1 C1 N2 75.2(3) . . . . ? O2 Na1 C1 N2 -175.0(2) . . . . ? O1 Na1 C1 N2 -46.3(3) . . . . ? C43A Na1 C1 N2 -19.9(5) . . . . ? C1 N1 C3 C2 -0.8(3) . . . . ? C4 N1 C3 C2 -170.8(3) . . . . ? N1 C3 C2 N2 -0.4(3) . . . . ? N1 C3 C2 Zn1 164.4(2) . . . . ? C1 N2 C2 C3 1.6(3) . . . . ? C22 N2 C2 C3 179.6(3) . . . . ? C1 N2 C2 Zn1 -162.8(2) . . . . ? C22 N2 C2 Zn1 15.2(4) . . . . ? C32 Zn1 C2 C3 140.7(3) . . . . ? C16 Zn1 C2 C3 -32.0(3) . . . . ? C32 Zn1 C2 N2 -58.6(3) . . . . ? C16 Zn1 C2 N2 128.7(3) . . . . ? C1 N1 C4 C9 -80.7(4) . . . . ? C3 N1 C4 C9 88.0(4) . . . . ? C1 N1 C4 C5 101.7(3) . . . . ? C3 N1 C4 C5 -89.6(4) . . . . ? C9 C4 C5 C6 2.5(5) . . . . ? N1 C4 C5 C6 180.0(3) . . . . ? C9 C4 C5 C10 178.9(3) . . . . ? N1 C4 C5 C10 -3.6(4) . . . . ? C4 C5 C6 C7 -2.2(5) . . . . ? C10 C5 C6 C7 -178.6(3) . . . . ? C5 C6 C7 C8 0.6(6) . . . . ? C6 C7 C8 C9 0.9(6) . . . . ? C7 C8 C9 C4 -0.6(5) . . . . ? C7 C8 C9 C13 177.9(3) . . . . ? C5 C4 C9 C8 -1.1(5) . . . . ? N1 C4 C9 C8 -178.6(3) . . . . ? C5 C4 C9 C13 -179.6(3) . . . . ? N1 C4 C9 C13 2.9(5) . . . . ? C6 C5 C10 C12 92.3(4) . . . . ? C4 C5 C10 C12 -83.9(4) . . . . ? C6 C5 C10 C11 -32.8(5) . . . . ? C4 C5 C10 C11 151.0(3) . . . . ? C8 C9 C13 C15 57.6(4) . . . . ? C4 C9 C13 C15 -124.1(4) . . . . ? C8 C9 C13 C14 -66.6(5) . . . . ? C4 C9 C13 C14 111.8(4) . . . . ? C32 Zn1 C16 C18 142.0(3) . . . . ? C2 Zn1 C16 C18 -44.8(3) . . . . ? C32 Zn1 C16 C17 18.4(4) . . . . ? C2 Zn1 C16 C17 -168.4(3) . . . . ? C32 Zn1 C16 C19 -101.3(3) . . . . ? C2 Zn1 C16 C19 71.9(3) . . . . ? C22 C20 C21 C25 0.2(5) . . . . ? C26 C20 C21 C25 -179.8(3) . . . . ? C21 C20 C22 C23 0.4(4) . . . . ? C26 C20 C22 C23 -179.6(3) . . . . ? C21 C20 C22 N2 -179.3(3) . . . . ? C26 C20 C22 N2 0.7(4) . . . . ? C1 N2 C22 C23 106.5(3) . . . . ? C2 N2 C22 C23 -71.3(3) . . . . ? C1 N2 C22 C20 -73.7(3) . . . . ? C2 N2 C22 C20 108.4(3) . . . . ? C20 C22 C23 C24 -0.7(4) . . . . ? N2 C22 C23 C24 179.0(3) . . . . ? C20 C22 C23 C29 175.5(3) . . . . ? N2 C22 C23 C29 -4.8(4) . . . . ? C22 C23 C24 C25 0.5(5) . . . . ? C29 C23 C24 C25 -175.8(3) . . . . ? C20 C21 C25 C24 -0.4(5) . . . . ? C23 C24 C25 C21 0.1(5) . . . . ? C21 C20 C26 C28 -17.8(4) . . . . ? C22 C20 C26 C28 162.1(3) . . . . ? C21 C20 C26 C27 107.1(3) . . . . ? C22 C20 C26 C27 -73.0(4) . . . . ? C24 C23 C29 C31 83.1(4) . . . . ? C22 C23 C29 C31 -93.0(4) . . . . ? C24 C23 C29 C30 -41.8(4) . . . . ? C22 C23 C29 C30 142.0(3) . . . . ? C16 Zn1 C32 C33 176.7(3) . . . . ? C2 Zn1 C32 C33 4.8(3) . . . . ? C16 Zn1 C32 C35 58.6(3) . . . . ? C2 Zn1 C32 C35 -113.3(2) . . . . ? C16 Zn1 C32 C34 -59.3(3) . . . . ? C2 Zn1 C32 C34 128.8(2) . . . . ? C39A O2 C36 C37 54.0(8) . . . . ? C39 O2 C36 C37 34.5(6) . . . . ? C36A O2 C36 C37 -55.1(10) . . . . ? Na1 O2 C36 C37 -142.0(4) . . . . ? O2 C36 C37 C38 -22.6(7) . . . . ? C36 C37 C38 C39 2.4(8) . . . . ? C39A O2 C39 C38 -118(2) . . . . ? C36 O2 C39 C38 -34.3(7) . . . . ? C36A O2 C39 C38 -1.8(8) . . . . ? Na1 O2 C39 C38 142.4(4) . . . . ? C37 C38 C39 O2 18.7(8) . . . . ? C43A O1 C40 C41 -23.0(9) . . . . ? C43 O1 C40 C41 -0.3(4) . . . . ? Na1 O1 C40 C41 -160.9(3) . . . . ? O1 C40 C41 C42 26.9(5) . . . . ? O1 C40 C41 C42A 9.1(9) . . . . ? C40 C41 C42 C43 -39.4(5) . . . . ? C42A C41 C42 C43 34(2) . . . . ? C40 O1 C43 C42 -25.0(5) . . . . ? C43A O1 C43 C42 99(2) . . . . ? Na1 O1 C43 C42 135.4(4) . . . . ? C41 C42 C43 O1 40.5(5) . . . . ? C47 O3 C44 C45 0.7(7) . . . . ? C47A O3 C44 C45 -16.7(12) . . . . ? C44A O3 C44 C45 -65(2) . . . . ? Na1 O3 C44 C45 179.4(3) . . . . ? O3 C44 C45 C46 27.1(6) . . . . ? C44 C45 C46 C47 -42.0(6) . . . . ? C47A O3 C47 C46 58(3) . . . . ? C44A O3 C47 C46 -8.3(10) . . . . ? C44 O3 C47 C46 -27.4(6) . . . . ? Na1 O3 C47 C46 153.9(3) . . . . ? C45 C46 C47 O3 42.0(6) . . . . ? C39A O2 C36A C37A -26.4(12) . . . . ? C36 O2 C36A C37A 54.2(9) . . . . ? C39 O2 C36A C37A -44.8(9) . . . . ? Na1 O2 C36A C37A 169.6(6) . . . . ? O2 C36A C37A C38A 44.3(11) . . . . ? C36A C37A C38A C39A -50.8(13) . . . . ? C36 O2 C39A C38A -37.8(11) . . . . ? C39 O2 C39A C38A 64(2) . . . . ? C36A O2 C39A C38A -5.9(13) . . . . ? Na1 O2 C39A C38A 157.3(8) . . . . ? C37A C38A C39A O2 35.8(14) . . . . ? C47 O3 C44A C45A -3.4(16) . . . . ? C47A O3 C44A C45A -18.5(17) . . . . ? C44 O3 C44A C45A 116(3) . . . . ? Na1 O3 C44A C45A -162.7(9) . . . . ? O3 C44A C45A C46A -11(2) . . . . ? C44A C45A C46A C47A 32(2) . . . . ? C47 O3 C47A C46A -72(3) . . . . ? C44A O3 C47A C46A 43(2) . . . . ? C44 O3 C47A C46A 28(2) . . . . ? Na1 O3 C47A C46A -167.0(12) . . . . ? C45A C46A C47A O3 -50(2) . . . . ? C42 C41 C42A C43A -105(3) . . . . ? C40 C41 C42A C43A 5.4(17) . . . . ? C40 O1 C43A C42A 24.3(16) . . . . ? C43 O1 C43A C42A -40.1(16) . . . . ? Na1 O1 C43A C42A 169.8(11) . . . . ? C40 O1 C43A Na1 -145.5(7) . . . . ? C43 O1 C43A Na1 150.2(18) . . . . ? C41 C42A C43A O1 -16.7(19) . . . . ? C41 C42A C43A Na1 -4(3) . . . . ? O3 Na1 C43A O1 107.4(8) . . . . ? O2 Na1 C43A O1 22.8(10) . . . . ? C1 Na1 C43A O1 -128.3(7) . . . . ? O3 Na1 C43A C42A 90(2) . . . . ? O2 Na1 C43A C42A 6(3) . . . . ? O1 Na1 C43A C42A -17.3(19) . . . . ? C1 Na1 C43A C42A -146(2) . . . . ? _diffrn_measured_fraction_theta_max 0.974 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.423 _refine_diff_density_min -0.385 _refine_diff_density_rms 0.058 _database_code_depnum_ccdc_archive 'CCDC 923037' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_seb549r #TrackingRef 'hevia5.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C35 H54 N2 Zn' _chemical_formula_weight 568.17 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Zn Zn -1.5491 0.6778 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.7795(5) _cell_length_b 10.1033(5) _cell_length_c 20.1669(8) _cell_angle_alpha 90.336(4) _cell_angle_beta 103.989(4) _cell_angle_gamma 118.932(5) _cell_volume 1674.40(14) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 8451 _cell_measurement_theta_min 3.9471 _cell_measurement_theta_max 69.1158 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.127 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 616 _exptl_absorpt_coefficient_mu 1.173 _exptl_absorpt_correction_T_min 0.82536 _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. ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 1.54180 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Gemini S' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11997 _diffrn_reflns_av_R_equivalents 0.0157 _diffrn_reflns_av_sigmaI/netI 0.0312 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 5.05 _diffrn_reflns_theta_max 69.04 _reflns_number_total 6087 _reflns_number_gt 5646 _reflns_threshold_expression I>2\s(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^ > 2\s(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^)+(0.0347P)^2^+1.2491P] 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 6087 _refine_ls_number_parameters 365 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0425 _refine_ls_R_factor_gt 0.0388 _refine_ls_wR_factor_ref 0.0989 _refine_ls_wR_factor_gt 0.0963 _refine_ls_goodness_of_fit_ref 1.094 _refine_ls_restrained_S_all 1.094 _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 1.05894(3) 0.37619(3) 0.235952(14) 0.02509(9) Uani 1 1 d . . . N1 N 0.8027(2) 0.02483(18) 0.21322(8) 0.0222(3) Uani 1 1 d . . . N2 N 0.73903(19) 0.14822(19) 0.27420(8) 0.0241(4) Uani 1 1 d . . . C1 C 0.8572(2) 0.1683(2) 0.24427(10) 0.0214(4) Uani 1 1 d . . . C2 C 0.6545(3) -0.0806(2) 0.22342(11) 0.0265(4) Uani 1 1 d . . . C3 C 0.6140(3) -0.0034(2) 0.26116(11) 0.0288(5) Uani 1 1 d . . . C4 C 0.8929(3) -0.0180(2) 0.17903(11) 0.0271(4) Uani 1 1 d . . . C5 C 0.8244(3) -0.0826(2) 0.10969(12) 0.0353(5) Uani 1 1 d . . . C6 C 0.9140(4) -0.1253(3) 0.07917(15) 0.0496(7) Uani 1 1 d . . . H6 H 0.8711 -0.1697 0.0320 0.060 Uiso 1 1 calc R . . C7 C 1.0622(4) -0.1044(3) 0.11582(17) 0.0553(8) Uani 1 1 d . . . H7 H 1.1213 -0.1333 0.0937 0.066 Uiso 1 1 calc R . . C8 C 1.1261(3) -0.0420(3) 0.18444(16) 0.0465(7) Uani 1 1 d . . . H8 H 1.2289 -0.0288 0.2091 0.056 Uiso 1 1 calc R . . C9 C 1.0435(3) 0.0025(2) 0.21873(12) 0.0319(5) Uani 1 1 d . . . C10 C 1.1110(3) 0.0623(3) 0.29553(13) 0.0367(5) Uani 1 1 d . . . H10 H 1.0967 0.1524 0.3028 0.044 Uiso 1 1 calc R . . C11 C 1.0148(3) -0.0578(3) 0.33706(13) 0.0441(6) Uani 1 1 d . . . H11A H 0.8989 -0.0909 0.3192 0.066 Uiso 1 1 calc R . . H11B H 1.0534 -0.0134 0.3858 0.066 Uiso 1 1 calc R . . H11C H 1.0305 -0.1458 0.3328 0.066 Uiso 1 1 calc R . . C12 C 1.2920(3) 0.1157(3) 0.32462(18) 0.0593(8) Uani 1 1 d . . . H12A H 1.3083 0.0275 0.3234 0.089 Uiso 1 1 calc R . . H12B H 1.3302 0.1655 0.3724 0.089 Uiso 1 1 calc R . . H12C H 1.3535 0.1885 0.2967 0.089 Uiso 1 1 calc R . . C13 C 0.6588(3) -0.1131(3) 0.06652(12) 0.0437(6) Uani 1 1 d . . . H13 H 0.6214 -0.0588 0.0928 0.052 Uiso 1 1 calc R . . C14 C 0.5339(4) -0.2846(3) 0.05423(15) 0.0546(7) Uani 1 1 d . . . H14A H 0.5667 -0.3399 0.0274 0.082 Uiso 1 1 calc R . . H14B H 0.4266 -0.3013 0.0287 0.082 Uiso 1 1 calc R . . H14C H 0.5285 -0.3222 0.0988 0.082 Uiso 1 1 calc R . . C15 C 0.6652(5) -0.0536(4) -0.00323(14) 0.0719(10) Uani 1 1 d . . . H15A H 0.7448 0.0559 0.0046 0.108 Uiso 1 1 calc R . . H15B H 0.5576 -0.0702 -0.0282 0.108 Uiso 1 1 calc R . . H15C H 0.6972 -0.1085 -0.0307 0.108 Uiso 1 1 calc R . . C16 C 0.7461(2) 0.2638(2) 0.32034(11) 0.0296(5) Uani 1 1 d . . . C17 C 0.7305(2) 0.3844(2) 0.29318(13) 0.0340(5) Uani 1 1 d . . . C18 C 0.7311(3) 0.4884(3) 0.33972(16) 0.0479(7) Uani 1 1 d . . . H18 H 0.7219 0.5727 0.3236 0.057 Uiso 1 1 calc R . . C19 C 0.7449(3) 0.4713(3) 0.40795(16) 0.0553(8) Uani 1 1 d . . . H19 H 0.7424 0.5422 0.4381 0.066 Uiso 1 1 calc R . . C20 C 0.7622(3) 0.3532(3) 0.43311(14) 0.0498(7) Uani 1 1 d . . . H20 H 0.7729 0.3440 0.4807 0.060 Uiso 1 1 calc R . . C21 C 0.7645(3) 0.2458(3) 0.39004(12) 0.0365(5) Uani 1 1 d . . . C22 C 0.7839(3) 0.1170(3) 0.42078(12) 0.0418(6) Uani 1 1 d . . . H22 H 0.7902 0.0558 0.3836 0.050 Uiso 1 1 calc R . . C23 C 0.6371(4) 0.0106(4) 0.44602(17) 0.0646(9) Uani 1 1 d . . . H23A H 0.6335 0.0660 0.4850 0.097 Uiso 1 1 calc R . . H23B H 0.6468 -0.0775 0.4608 0.097 Uiso 1 1 calc R . . H23C H 0.5370 -0.0250 0.4084 0.097 Uiso 1 1 calc R . . C24 C 0.9388(3) 0.1750(4) 0.48044(15) 0.0626(9) Uani 1 1 d . . . H24A H 1.0340 0.2360 0.4637 0.094 Uiso 1 1 calc R . . H24B H 0.9444 0.0878 0.4990 0.094 Uiso 1 1 calc R . . H24C H 0.9372 0.2385 0.5169 0.094 Uiso 1 1 calc R . . C25 C 0.7065(3) 0.3996(3) 0.21731(13) 0.0372(5) Uani 1 1 d . . . H25 H 0.7760 0.3675 0.2008 0.045 Uiso 1 1 calc R . . C26 C 0.5329(4) 0.2914(4) 0.17693(16) 0.0793(11) Uani 1 1 d . . . H26A H 0.5034 0.1869 0.1856 0.119 Uiso 1 1 calc R . . H26B H 0.5213 0.2968 0.1275 0.119 Uiso 1 1 calc R . . H26C H 0.4609 0.3201 0.1914 0.119 Uiso 1 1 calc R . . C27 C 0.7592(4) 0.5611(3) 0.20262(18) 0.0731(10) Uani 1 1 d . . . H27A H 0.6833 0.5913 0.2117 0.110 Uiso 1 1 calc R . . H27B H 0.7594 0.5664 0.1541 0.110 Uiso 1 1 calc R . . H27C H 0.8689 0.6305 0.2325 0.110 Uiso 1 1 calc R . . C28 C 1.2257(3) 0.5207(2) 0.32239(12) 0.0307(5) Uani 1 1 d . . . C29 C 1.2039(3) 0.6605(3) 0.32713(15) 0.0499(7) Uani 1 1 d . . . H29A H 1.0957 0.6286 0.3324 0.075 Uiso 1 1 calc R . . H29B H 1.2148 0.7073 0.2849 0.075 Uiso 1 1 calc R . . H29C H 1.2872 0.7348 0.3671 0.075 Uiso 1 1 calc R . . C30 C 1.2155(3) 0.4562(3) 0.39005(12) 0.0444(6) Uani 1 1 d . . . H30A H 1.2291 0.3664 0.3885 0.067 Uiso 1 1 calc R . . H30B H 1.1091 0.4267 0.3970 0.067 Uiso 1 1 calc R . . H30C H 1.3016 0.5341 0.4283 0.067 Uiso 1 1 calc R . . C31 C 1.3957(3) 0.5736(3) 0.31515(15) 0.0468(6) Uani 1 1 d . . . H31A H 1.4771 0.6513 0.3544 0.070 Uiso 1 1 calc R . . H31B H 1.4056 0.6171 0.2721 0.070 Uiso 1 1 calc R . . H31C H 1.4136 0.4862 0.3143 0.070 Uiso 1 1 calc R . . C32 C 1.0594(3) 0.4122(3) 0.13697(12) 0.0383(6) Uani 1 1 d . . . C33 C 0.8888(4) 0.3428(4) 0.08769(14) 0.0697(9) Uani 1 1 d . . . H33A H 0.8955 0.3474 0.0400 0.104 Uiso 1 1 calc R . . H33B H 0.8373 0.4003 0.0975 0.104 Uiso 1 1 calc R . . H33C H 0.8238 0.2360 0.0939 0.104 Uiso 1 1 calc R . . C34 C 1.1501(4) 0.5838(3) 0.13308(15) 0.0568(8) Uani 1 1 d . . . H34A H 1.2616 0.6302 0.1633 0.085 Uiso 1 1 calc R . . H34B H 1.0939 0.6315 0.1481 0.085 Uiso 1 1 calc R . . H34C H 1.1529 0.5996 0.0854 0.085 Uiso 1 1 calc R . . C35 C 1.1495(5) 0.3437(4) 0.11127(17) 0.0685(10) Uani 1 1 d . . . H35A H 1.1517 0.3636 0.0639 0.103 Uiso 1 1 calc R . . H35B H 1.0934 0.2331 0.1121 0.103 Uiso 1 1 calc R . . H35C H 1.2611 0.3903 0.1413 0.103 Uiso 1 1 calc R . . H2 H 0.604(3) -0.181(3) 0.2058(12) 0.026(6) Uiso 1 1 d . . . H3 H 0.528(3) -0.037(3) 0.2793(13) 0.036(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 Zn1 0.03022(16) 0.02290(15) 0.02480(16) 0.00522(11) 0.01090(11) 0.01382(12) N1 0.0268(8) 0.0224(8) 0.0197(8) 0.0032(6) 0.0082(7) 0.0133(7) N2 0.0217(8) 0.0247(9) 0.0233(9) -0.0040(7) 0.0050(7) 0.0103(7) C1 0.0244(10) 0.0243(10) 0.0170(9) 0.0028(7) 0.0040(7) 0.0142(8) C2 0.0270(10) 0.0224(10) 0.0255(11) -0.0006(8) 0.0069(8) 0.0091(9) C3 0.0220(10) 0.0284(11) 0.0298(12) -0.0025(9) 0.0080(9) 0.0077(9) C4 0.0366(11) 0.0193(9) 0.0335(12) 0.0081(8) 0.0205(9) 0.0152(9) C5 0.0558(15) 0.0239(11) 0.0323(12) 0.0066(9) 0.0241(11) 0.0192(11) C6 0.083(2) 0.0319(13) 0.0494(16) 0.0074(11) 0.0441(15) 0.0286(14) C7 0.078(2) 0.0342(14) 0.085(2) 0.0177(14) 0.0630(19) 0.0329(14) C8 0.0442(14) 0.0295(12) 0.084(2) 0.0176(13) 0.0389(14) 0.0224(11) C9 0.0341(12) 0.0188(10) 0.0499(14) 0.0108(9) 0.0222(10) 0.0137(9) C10 0.0309(12) 0.0288(11) 0.0512(15) 0.0053(10) 0.0059(10) 0.0181(10) C11 0.0476(15) 0.0464(15) 0.0396(14) 0.0098(11) 0.0081(11) 0.0262(12) C12 0.0338(14) 0.0467(16) 0.091(2) 0.0086(15) 0.0031(14) 0.0214(13) C13 0.0689(18) 0.0399(13) 0.0218(12) -0.0009(10) 0.0100(11) 0.0281(13) C14 0.0622(18) 0.0475(16) 0.0401(15) -0.0082(12) 0.0075(13) 0.0202(14) C15 0.123(3) 0.0614(19) 0.0233(14) 0.0037(13) 0.0146(16) 0.043(2) C16 0.0181(9) 0.0300(11) 0.0351(12) -0.0112(9) 0.0068(8) 0.0082(9) C17 0.0192(10) 0.0278(11) 0.0500(14) -0.0084(10) 0.0094(9) 0.0082(9) C18 0.0290(12) 0.0312(13) 0.079(2) -0.0154(12) 0.0169(12) 0.0108(10) C19 0.0380(14) 0.0495(16) 0.066(2) -0.0312(14) 0.0180(13) 0.0116(12) C20 0.0349(13) 0.0576(17) 0.0439(15) -0.0222(13) 0.0126(11) 0.0129(12) C21 0.0213(10) 0.0445(13) 0.0329(12) -0.0113(10) 0.0083(9) 0.0082(10) C22 0.0375(13) 0.0526(15) 0.0263(12) -0.0026(11) 0.0105(10) 0.0152(12) C23 0.0477(17) 0.0572(18) 0.064(2) -0.0027(15) 0.0233(15) 0.0041(14) C24 0.0470(16) 0.073(2) 0.0398(16) 0.0190(14) 0.0059(12) 0.0117(15) C25 0.0331(12) 0.0284(11) 0.0521(15) -0.0007(10) 0.0121(11) 0.0168(10) C26 0.0508(18) 0.093(3) 0.0431(18) -0.0065(17) -0.0013(14) 0.0038(18) C27 0.089(2) 0.0370(16) 0.074(2) 0.0090(15) -0.0103(18) 0.0314(17) C28 0.0272(11) 0.0262(11) 0.0346(12) -0.0016(9) 0.0085(9) 0.0103(9) C29 0.0407(14) 0.0349(13) 0.0648(18) -0.0117(12) 0.0033(13) 0.0172(12) C30 0.0414(14) 0.0508(15) 0.0312(13) -0.0028(11) 0.0072(10) 0.0172(12) C31 0.0303(12) 0.0450(15) 0.0577(17) 0.0020(12) 0.0138(11) 0.0126(11) C32 0.0654(16) 0.0344(12) 0.0255(12) 0.0121(9) 0.0225(11) 0.0282(12) C33 0.093(3) 0.080(2) 0.0211(14) 0.0107(14) 0.0081(14) 0.036(2) C34 0.099(2) 0.0404(15) 0.0462(16) 0.0231(12) 0.0380(16) 0.0378(16) C35 0.129(3) 0.0561(18) 0.066(2) 0.0333(16) 0.072(2) 0.060(2) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 C28 2.030(2) . ? Zn1 C32 2.032(2) . ? Zn1 C1 2.118(2) . ? N1 C1 1.363(2) . ? N1 C2 1.390(3) . ? N1 C4 1.450(2) . ? N2 C1 1.361(2) . ? N2 C3 1.392(3) . ? N2 C16 1.454(2) . ? C2 C3 1.335(3) . ? C2 H2 0.91(2) . ? C3 H3 0.91(3) . ? C4 C5 1.394(3) . ? C4 C9 1.409(3) . ? C5 C6 1.398(3) . ? C5 C13 1.519(4) . ? C6 C7 1.370(4) . ? C6 H6 0.9500 . ? C7 C8 1.376(4) . ? C7 H7 0.9500 . ? C8 C9 1.396(3) . ? C8 H8 0.9500 . ? C9 C10 1.519(3) . ? C10 C12 1.530(3) . ? C10 C11 1.532(3) . ? C10 H10 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.536(4) . ? C13 C15 1.536(4) . ? C13 H13 1.0000 . ? 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 C21 1.398(3) . ? C16 C17 1.398(3) . ? C17 C18 1.402(3) . ? C17 C25 1.511(4) . ? C18 C19 1.370(4) . ? C18 H18 0.9500 . ? C19 C20 1.368(4) . ? C19 H19 0.9500 . ? C20 C21 1.398(3) . ? C20 H20 0.9500 . ? C21 C22 1.518(4) . ? C22 C24 1.529(3) . ? C22 C23 1.531(4) . ? C22 H22 1.0000 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C26 1.506(4) . ? C25 C27 1.511(3) . ? C25 H25 1.0000 . ? 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 C30 1.520(3) . ? C28 C31 1.526(3) . ? C28 C29 1.533(3) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 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 1.524(4) . ? C32 C35 1.526(4) . ? C32 C34 1.532(3) . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 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 C28 Zn1 C32 126.14(10) . . ? C28 Zn1 C1 120.08(8) . . ? C32 Zn1 C1 113.75(9) . . ? C1 N1 C2 111.74(16) . . ? C1 N1 C4 125.02(16) . . ? C2 N1 C4 123.01(16) . . ? C1 N2 C3 111.63(16) . . ? C1 N2 C16 125.58(16) . . ? C3 N2 C16 122.49(17) . . ? N2 C1 N1 103.20(16) . . ? N2 C1 Zn1 128.19(14) . . ? N1 C1 Zn1 128.10(14) . . ? C3 C2 N1 106.66(18) . . ? C3 C2 H2 131.9(14) . . ? N1 C2 H2 121.4(14) . . ? C2 C3 N2 106.76(18) . . ? C2 C3 H3 130.2(16) . . ? N2 C3 H3 122.9(16) . . ? C5 C4 C9 123.3(2) . . ? C5 C4 N1 118.80(19) . . ? C9 C4 N1 117.88(19) . . ? C4 C5 C6 116.9(2) . . ? C4 C5 C13 124.5(2) . . ? C6 C5 C13 118.6(2) . . ? C7 C6 C5 121.4(3) . . ? C7 C6 H6 119.3 . . ? C5 C6 H6 119.3 . . ? C6 C7 C8 120.4(2) . . ? C6 C7 H7 119.8 . . ? C8 C7 H7 119.8 . . ? C7 C8 C9 121.6(3) . . ? C7 C8 H8 119.2 . . ? C9 C8 H8 119.2 . . ? C8 C9 C4 116.4(2) . . ? C8 C9 C10 120.9(2) . . ? C4 C9 C10 122.67(19) . . ? C9 C10 C12 114.1(2) . . ? C9 C10 C11 110.94(19) . . ? C12 C10 C11 109.1(2) . . ? C9 C10 H10 107.5 . . ? C12 C10 H10 107.5 . . ? C11 C10 H10 107.5 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C5 C13 C14 110.7(2) . . ? C5 C13 C15 112.2(2) . . ? C14 C13 C15 109.5(2) . . ? C5 C13 H13 108.1 . . ? C14 C13 H13 108.1 . . ? C15 C13 H13 108.1 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C21 C16 C17 123.3(2) . . ? C21 C16 N2 117.5(2) . . ? C17 C16 N2 119.1(2) . . ? C16 C17 C18 116.4(2) . . ? C16 C17 C25 122.47(19) . . ? C18 C17 C25 121.1(2) . . ? C19 C18 C17 121.5(3) . . ? C19 C18 H18 119.3 . . ? C17 C18 H18 119.3 . . ? C20 C19 C18 120.7(2) . . ? C20 C19 H19 119.7 . . ? C18 C19 H19 119.7 . . ? C19 C20 C21 121.2(3) . . ? C19 C20 H20 119.4 . . ? C21 C20 H20 119.4 . . ? C16 C21 C20 116.9(2) . . ? C16 C21 C22 124.2(2) . . ? C20 C21 C22 118.9(2) . . ? C21 C22 C24 112.7(2) . . ? C21 C22 C23 111.1(2) . . ? C24 C22 C23 109.0(2) . . ? C21 C22 H22 108.0 . . ? C24 C22 H22 108.0 . . ? C23 C22 H22 108.0 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C26 C25 C27 111.1(3) . . ? C26 C25 C17 110.4(2) . . ? C27 C25 C17 113.7(2) . . ? C26 C25 H25 107.1 . . ? C27 C25 H25 107.1 . . ? C17 C25 H25 107.1 . . ? 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 . . ? C30 C28 C31 108.1(2) . . ? C30 C28 C29 107.6(2) . . ? C31 C28 C29 108.4(2) . . ? C30 C28 Zn1 115.92(15) . . ? C31 C28 Zn1 108.72(16) . . ? C29 C28 Zn1 107.84(16) . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C28 C30 H30A 109.5 . . ? C28 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C28 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C28 C31 H31A 109.5 . . ? C28 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C28 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C33 C32 C35 108.4(3) . . ? C33 C32 C34 108.1(2) . . ? C35 C32 C34 107.1(2) . . ? C33 C32 Zn1 112.93(18) . . ? C35 C32 Zn1 109.82(17) . . ? C34 C32 Zn1 110.30(16) . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C32 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C32 C34 H34A 109.5 . . ? C32 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C32 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C32 C35 H35A 109.5 . . ? C32 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C32 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 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 C3 N2 C1 N1 -0.7(2) . . . . ? C16 N2 C1 N1 173.06(18) . . . . ? C3 N2 C1 Zn1 171.54(14) . . . . ? C16 N2 C1 Zn1 -14.6(3) . . . . ? C2 N1 C1 N2 0.3(2) . . . . ? C4 N1 C1 N2 -174.23(17) . . . . ? C2 N1 C1 Zn1 -171.95(14) . . . . ? C4 N1 C1 Zn1 13.5(3) . . . . ? C28 Zn1 C1 N2 59.66(19) . . . . ? C32 Zn1 C1 N2 -118.64(17) . . . . ? C28 Zn1 C1 N1 -129.90(16) . . . . ? C32 Zn1 C1 N1 51.81(19) . . . . ? C1 N1 C2 C3 0.2(2) . . . . ? C4 N1 C2 C3 174.89(18) . . . . ? N1 C2 C3 N2 -0.6(2) . . . . ? C1 N2 C3 C2 0.9(2) . . . . ? C16 N2 C3 C2 -173.14(19) . . . . ? C1 N1 C4 C5 -121.8(2) . . . . ? C2 N1 C4 C5 64.2(3) . . . . ? C1 N1 C4 C9 60.6(3) . . . . ? C2 N1 C4 C9 -113.3(2) . . . . ? C9 C4 C5 C6 -1.3(3) . . . . ? N1 C4 C5 C6 -178.66(18) . . . . ? C9 C4 C5 C13 176.9(2) . . . . ? N1 C4 C5 C13 -0.4(3) . . . . ? C4 C5 C6 C7 0.0(3) . . . . ? C13 C5 C6 C7 -178.3(2) . . . . ? C5 C6 C7 C8 0.7(4) . . . . ? C6 C7 C8 C9 -0.3(4) . . . . ? C7 C8 C9 C4 -0.9(3) . . . . ? C7 C8 C9 C10 176.3(2) . . . . ? C5 C4 C9 C8 1.7(3) . . . . ? N1 C4 C9 C8 179.12(18) . . . . ? C5 C4 C9 C10 -175.4(2) . . . . ? N1 C4 C9 C10 2.0(3) . . . . ? C8 C9 C10 C12 18.3(3) . . . . ? C4 C9 C10 C12 -164.6(2) . . . . ? C8 C9 C10 C11 -105.4(2) . . . . ? C4 C9 C10 C11 71.6(3) . . . . ? C4 C5 C13 C14 -105.9(3) . . . . ? C6 C5 C13 C14 72.3(3) . . . . ? C4 C5 C13 C15 131.4(2) . . . . ? C6 C5 C13 C15 -50.4(3) . . . . ? C1 N2 C16 C21 -109.1(2) . . . . ? C3 N2 C16 C21 64.0(3) . . . . ? C1 N2 C16 C17 72.4(3) . . . . ? C3 N2 C16 C17 -114.5(2) . . . . ? C21 C16 C17 C18 -1.1(3) . . . . ? N2 C16 C17 C18 177.29(18) . . . . ? C21 C16 C17 C25 -178.5(2) . . . . ? N2 C16 C17 C25 -0.1(3) . . . . ? C16 C17 C18 C19 -0.6(3) . . . . ? C25 C17 C18 C19 176.8(2) . . . . ? C17 C18 C19 C20 1.5(4) . . . . ? C18 C19 C20 C21 -0.8(4) . . . . ? C17 C16 C21 C20 1.8(3) . . . . ? N2 C16 C21 C20 -176.61(19) . . . . ? C17 C16 C21 C22 -179.2(2) . . . . ? N2 C16 C21 C22 2.4(3) . . . . ? C19 C20 C21 C16 -0.8(3) . . . . ? C19 C20 C21 C22 -179.9(2) . . . . ? C16 C21 C22 C24 123.7(2) . . . . ? C20 C21 C22 C24 -57.2(3) . . . . ? C16 C21 C22 C23 -113.6(3) . . . . ? C20 C21 C22 C23 65.4(3) . . . . ? C16 C17 C25 C26 77.8(3) . . . . ? C18 C17 C25 C26 -99.5(3) . . . . ? C16 C17 C25 C27 -156.6(2) . . . . ? C18 C17 C25 C27 26.2(3) . . . . ? C32 Zn1 C28 C30 -169.70(16) . . . . ? C1 Zn1 C28 C30 12.2(2) . . . . ? C32 Zn1 C28 C31 -47.7(2) . . . . ? C1 Zn1 C28 C31 134.20(16) . . . . ? C32 Zn1 C28 C29 69.7(2) . . . . ? C1 Zn1 C28 C29 -108.41(17) . . . . ? C28 Zn1 C32 C33 -146.77(19) . . . . ? C1 Zn1 C32 C33 31.4(2) . . . . ? C28 Zn1 C32 C35 92.2(2) . . . . ? C1 Zn1 C32 C35 -89.7(2) . . . . ? C28 Zn1 C32 C34 -25.7(2) . . . . ? C1 Zn1 C32 C34 152.52(18) . . . . ? _diffrn_measured_fraction_theta_max 0.973 _diffrn_reflns_theta_full 69.04 _diffrn_measured_fraction_theta_full 0.973 _refine_diff_density_max 0.792 _refine_diff_density_min -0.405 _refine_diff_density_rms 0.049 _database_code_depnum_ccdc_archive 'CCDC 923038' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_vb22 #TrackingRef 'hevia5.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'C71 H127 N2 Na O7 Zn2' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C71 H127 N2 Na O7 Zn2' _chemical_formula_weight 1274.48 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' 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' 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/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 12.5177(2) _cell_length_b 33.2445(6) _cell_length_c 18.2146(3) _cell_angle_alpha 90.00 _cell_angle_beta 100.694(2) _cell_angle_gamma 90.00 _cell_volume 7448.3(2) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 39605 _cell_measurement_theta_min 3.2620 _cell_measurement_theta_max 29.3651 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.137 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2776 _exptl_absorpt_coefficient_mu 0.698 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.88234 _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 'OD Xcalibur, Eos' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 106036 _diffrn_reflns_av_R_equivalents 0.0636 _diffrn_reflns_av_sigmaI/netI 0.0444 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -43 _diffrn_reflns_limit_k_max 43 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.27 _diffrn_reflns_theta_max 28.00 _reflns_number_total 17954 _reflns_number_gt 14402 _reflns_threshold_expression I>2\s(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Disorder modelled in 5 THF groups and one But fragment. 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^ > 2\s(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^)+(0.0179P)^2^+20.4956P] 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 17954 _refine_ls_number_parameters 822 _refine_ls_number_restraints 121 _refine_ls_R_factor_all 0.0979 _refine_ls_R_factor_gt 0.0781 _refine_ls_wR_factor_ref 0.1585 _refine_ls_wR_factor_gt 0.1498 _refine_ls_goodness_of_fit_ref 1.178 _refine_ls_restrained_S_all 1.181 _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 Na1 Na 0.51121(11) 0.38522(4) 0.70408(8) 0.0298(3) Uani 1 1 d . B . Zn1 Zn 0.10924(3) 0.338451(13) 0.01991(2) 0.02713(10) Uani 1 1 d . . . Zn2 Zn -0.00028(4) 0.405104(14) 0.32514(2) 0.03257(11) Uani 1 1 d . . . O3 O 0.4866(3) 0.36331(11) 0.57606(17) 0.0539(9) Uani 1 1 d . . . O6 O 0.6967(2) 0.39177(9) 0.70331(19) 0.0469(8) Uani 1 1 d . . . N1 N -0.0957(2) 0.39046(8) 0.15551(14) 0.0199(5) Uani 1 1 d . A . N2 N 0.0719(2) 0.37402(8) 0.17841(14) 0.0195(5) Uani 1 1 d . . . C2 C 0.0368(3) 0.36265(10) 0.10243(17) 0.0210(6) Uani 1 1 d . A . C1 C -0.0070(2) 0.39102(9) 0.21120(17) 0.0201(6) Uani 1 1 d . A . C3 C -0.0697(3) 0.37384(10) 0.09081(18) 0.0214(6) Uani 1 1 d . . . H3 H -0.1193 0.3707 0.0449 0.026 Uiso 1 1 calc R A . C4 C -0.1976(2) 0.41054(10) 0.15569(17) 0.0220(6) Uani 1 1 d . . . C5 C -0.2939(3) 0.38800(11) 0.14387(19) 0.0272(7) Uani 1 1 d . A . C6 C -0.3916(3) 0.40879(13) 0.1414(2) 0.0345(9) Uani 1 1 d . . . H6 H -0.4580 0.3942 0.1343 0.041 Uiso 1 1 calc R A . C7 C -0.3933(3) 0.44993(13) 0.1489(2) 0.0387(9) Uani 1 1 d . A . H7 H -0.4606 0.4635 0.1470 0.046 Uiso 1 1 calc R . . C8 C -0.2982(3) 0.47155(12) 0.1592(2) 0.0362(9) Uani 1 1 d . . . H8 H -0.3007 0.4999 0.1649 0.043 Uiso 1 1 calc R A . C9 C -0.1980(3) 0.45273(11) 0.16149(19) 0.0277(7) Uani 1 1 d . A . C10 C -0.0958(3) 0.47784(11) 0.1638(2) 0.0336(8) Uani 1 1 d . . . H10 H -0.0328 0.4615 0.1894 0.040 Uiso 1 1 calc R A . C11 C -0.0963(5) 0.51693(15) 0.2074(3) 0.0627(14) Uani 1 1 d . A . H11A H -0.0285 0.5316 0.2071 0.094 Uiso 1 1 calc R . . H11B H -0.1026 0.5108 0.2591 0.094 Uiso 1 1 calc R . . H11C H -0.1582 0.5335 0.1842 0.094 Uiso 1 1 calc R . . C12 C -0.0789(4) 0.48576(14) 0.0840(3) 0.0492(11) Uani 1 1 d . A . H12A H -0.0128 0.5017 0.0854 0.074 Uiso 1 1 calc R . . H12B H -0.1415 0.5005 0.0565 0.074 Uiso 1 1 calc R . . H12C H -0.0717 0.4601 0.0590 0.074 Uiso 1 1 calc R . . C13 C -0.2976(3) 0.34273(12) 0.1318(2) 0.0334(8) Uani 1 1 d . . . H13 H -0.2217 0.3321 0.1442 0.040 Uiso 1 1 calc R A . C14 C -0.3661(3) 0.32166(14) 0.1825(3) 0.0496(12) Uani 1 1 d . A . H14A H -0.3666 0.2926 0.1734 0.074 Uiso 1 1 calc R . . H14B H -0.4408 0.3319 0.1714 0.074 Uiso 1 1 calc R . . H14C H -0.3346 0.3270 0.2349 0.074 Uiso 1 1 calc R . . C15 C -0.3440(3) 0.33271(13) 0.0501(3) 0.0461(11) Uani 1 1 d . A . H15A H -0.3458 0.3035 0.0434 0.069 Uiso 1 1 calc R . . H15B H -0.2981 0.3448 0.0179 0.069 Uiso 1 1 calc R . . H15C H -0.4180 0.3435 0.0367 0.069 Uiso 1 1 calc R . . C16 C 0.1848(2) 0.37478(10) 0.21434(18) 0.0215(6) Uani 1 1 d . A . C17 C 0.2235(3) 0.34702(11) 0.2709(2) 0.0291(8) Uani 1 1 d . . . C18 C 0.3330(3) 0.34948(13) 0.3047(2) 0.0376(9) Uani 1 1 d . A . H18 H 0.3612 0.3312 0.3436 0.045 Uiso 1 1 calc R . . C19 C 0.4008(3) 0.37787(13) 0.2828(2) 0.0357(9) Uani 1 1 d . . . H19 H 0.4749 0.3792 0.3066 0.043 Uiso 1 1 calc R A . C20 C 0.3604(3) 0.40446(11) 0.2261(2) 0.0283(7) Uani 1 1 d . A . H20 H 0.4079 0.4238 0.2110 0.034 Uiso 1 1 calc R . . C21 C 0.2527(3) 0.40366(10) 0.19063(18) 0.0218(6) Uani 1 1 d . . . C22 C 0.2132(3) 0.43296(10) 0.1270(2) 0.0265(7) Uani 1 1 d . A . H22 H 0.1330 0.4292 0.1109 0.032 Uiso 1 1 calc R . . C23 C 0.2674(3) 0.42390(13) 0.0600(2) 0.0369(9) Uani 1 1 d . . . H23A H 0.2410 0.4429 0.0196 0.055 Uiso 1 1 calc R A . H23B H 0.2495 0.3964 0.0426 0.055 Uiso 1 1 calc R . . H23C H 0.3464 0.4266 0.0751 0.055 Uiso 1 1 calc R . . C24 C 0.2337(4) 0.47692(12) 0.1500(2) 0.0411(10) Uani 1 1 d . . . H24A H 0.2067 0.4944 0.1073 0.062 Uiso 1 1 calc R A . H24B H 0.3119 0.4813 0.1666 0.062 Uiso 1 1 calc R . . H24C H 0.1956 0.4832 0.1910 0.062 Uiso 1 1 calc R . . C25 C 0.1530(3) 0.31410(13) 0.2947(2) 0.0426(10) Uani 1 1 d . A . H25 H 0.0769 0.3179 0.2669 0.051 Uiso 1 1 calc R . . C26 C 0.1512(5) 0.3155(2) 0.3775(3) 0.0745(19) Uani 1 1 d . . . H26A H 0.1042 0.2940 0.3902 0.112 Uiso 1 1 calc R A . H26B H 0.1232 0.3416 0.3902 0.112 Uiso 1 1 calc R . . H26C H 0.2251 0.3118 0.4058 0.112 Uiso 1 1 calc R . . C27 C 0.1921(5) 0.27247(16) 0.2755(4) 0.0803(19) Uani 1 1 d . . . H27A H 0.1454 0.2518 0.2914 0.120 Uiso 1 1 calc R A . H27B H 0.2672 0.2684 0.3013 0.120 Uiso 1 1 calc R . . H27C H 0.1886 0.2705 0.2214 0.120 Uiso 1 1 calc R . . C28 C -0.1163(4) 0.37602(16) 0.3709(2) 0.0489(12) Uani 1 1 d . . . C29 C -0.1439(4) 0.33422(17) 0.3378(3) 0.0593(14) Uani 1 1 d . . . H29A H -0.1658 0.3363 0.2834 0.089 Uiso 1 1 calc R . . H29B H -0.2037 0.3227 0.3589 0.089 Uiso 1 1 calc R . . H29C H -0.0799 0.3168 0.3499 0.089 Uiso 1 1 calc R . . C30 C -0.2195(4) 0.40185(19) 0.3562(3) 0.0657(16) Uani 1 1 d . . . H30A H -0.2432 0.4055 0.3023 0.099 Uiso 1 1 calc R . . H30B H -0.2042 0.4281 0.3803 0.099 Uiso 1 1 calc R . . H30C H -0.2771 0.3884 0.3768 0.099 Uiso 1 1 calc R . . C31 C -0.0833(4) 0.3712(2) 0.4560(2) 0.0702(18) Uani 1 1 d . . . H31A H -0.0651 0.3976 0.4788 0.105 Uiso 1 1 calc R . . H31B H -0.0198 0.3535 0.4674 0.105 Uiso 1 1 calc R . . H31C H -0.1438 0.3595 0.4760 0.105 Uiso 1 1 calc R . . C32 C 0.1063(4) 0.44473(15) 0.3836(2) 0.0461(11) Uani 1 1 d . . . C33 C 0.1864(5) 0.4221(2) 0.4439(3) 0.083(2) Uani 1 1 d . . . H33A H 0.1458 0.4063 0.4749 0.124 Uiso 1 1 calc R . . H33B H 0.2330 0.4415 0.4753 0.124 Uiso 1 1 calc R . . H33C H 0.2315 0.4041 0.4198 0.124 Uiso 1 1 calc R . . C34 C 0.1760(4) 0.46818(14) 0.3387(3) 0.0511(12) Uani 1 1 d . . . H34A H 0.2170 0.4494 0.3131 0.077 Uiso 1 1 calc R . . H34B H 0.2266 0.4854 0.3723 0.077 Uiso 1 1 calc R . . H34C H 0.1292 0.4849 0.3016 0.077 Uiso 1 1 calc R . . C35 C 0.0442(6) 0.4749(2) 0.4224(4) 0.092(2) Uani 1 1 d . . . H35A H -0.0015 0.4606 0.4519 0.138 Uiso 1 1 calc R . . H35B H -0.0016 0.4917 0.3848 0.138 Uiso 1 1 calc R . . H35C H 0.0959 0.4921 0.4554 0.138 Uiso 1 1 calc R . . C36 C 0.019(2) 0.3532(9) -0.083(2) 0.0450(12) Uani 0.190(5) 1 d PD A 1 C37 C -0.022(2) 0.3966(7) -0.0879(13) 0.073(2) Uani 0.190(5) 1 d PD A 1 H37A H -0.0604 0.4021 -0.1388 0.110 Uiso 0.190(5) 1 calc PR A 1 H37B H 0.0404 0.4150 -0.0757 0.110 Uiso 0.190(5) 1 calc PR A 1 H37C H -0.0709 0.4007 -0.0526 0.110 Uiso 0.190(5) 1 calc PR A 1 C38 C -0.081(2) 0.3259(8) -0.0994(14) 0.067(2) Uani 0.190(5) 1 d PD A 1 H38A H -0.1110 0.3225 -0.0540 0.101 Uiso 0.190(5) 1 calc PR A 1 H38B H -0.0593 0.2997 -0.1165 0.101 Uiso 0.190(5) 1 calc PR A 1 H38C H -0.1353 0.3382 -0.1385 0.101 Uiso 0.190(5) 1 calc PR A 1 C39 C 0.083(2) 0.3476(9) -0.1458(14) 0.072(2) Uani 0.190(5) 1 d PD A 1 H39A H 0.1212 0.3218 -0.1395 0.108 Uiso 0.190(5) 1 calc PR A 1 H39B H 0.1352 0.3695 -0.1446 0.108 Uiso 0.190(5) 1 calc PR A 1 H39C H 0.0322 0.3478 -0.1939 0.108 Uiso 0.190(5) 1 calc PR A 1 C40 C 0.2484(3) 0.30412(12) 0.0340(2) 0.0361(9) Uani 1 1 d . A . C41 C 0.3286(3) 0.31046(14) 0.1057(3) 0.0499(12) Uani 1 1 d . . . H41A H 0.3538 0.3384 0.1084 0.075 Uiso 1 1 calc R A . H41B H 0.3907 0.2924 0.1070 0.075 Uiso 1 1 calc R . . H41C H 0.2933 0.3047 0.1483 0.075 Uiso 1 1 calc R . . C42 C 0.2117(4) 0.26059(14) 0.0321(4) 0.0732(19) Uani 1 1 d . . . H42A H 0.1593 0.2556 -0.0140 0.110 Uiso 1 1 calc R A . H42B H 0.1773 0.2552 0.0753 0.110 Uiso 1 1 calc R . . H42C H 0.2748 0.2429 0.0339 0.110 Uiso 1 1 calc R . . C43 C 0.3102(4) 0.3106(2) -0.0302(3) 0.0741(18) Uani 1 1 d . . . H43A H 0.2606 0.3068 -0.0780 0.111 Uiso 1 1 calc R A . H43B H 0.3699 0.2911 -0.0260 0.111 Uiso 1 1 calc R . . H43C H 0.3398 0.3379 -0.0276 0.111 Uiso 1 1 calc R . . C52 C 0.5357(4) 0.37387(15) 0.5144(3) 0.0527(12) Uani 1 1 d . . . H52A H 0.6008 0.3908 0.5311 0.063 Uiso 1 1 calc R . . H52B H 0.4839 0.3891 0.4768 0.063 Uiso 1 1 calc R . . C53 C 0.5671(4) 0.33484(14) 0.4815(3) 0.0478(11) Uani 1 1 d . . . H53A H 0.6449 0.3287 0.4996 0.057 Uiso 1 1 calc R . . H53B H 0.5531 0.3361 0.4262 0.057 Uiso 1 1 calc R . . C54 C 0.4949(4) 0.30360(15) 0.5089(3) 0.0534(12) Uani 1 1 d . . . H54A H 0.5385 0.2839 0.5427 0.064 Uiso 1 1 calc R . . H54B H 0.4502 0.2891 0.4666 0.064 Uiso 1 1 calc R . . C55 C 0.4235(5) 0.32943(18) 0.5509(3) 0.0661(16) Uani 1 1 d . . . H55A H 0.3555 0.3375 0.5172 0.079 Uiso 1 1 calc R . . H55B H 0.4046 0.3143 0.5936 0.079 Uiso 1 1 calc R . . C64 C 0.7556(3) 0.35757(14) 0.6847(3) 0.0451(10) Uani 1 1 d . . . H64A H 0.7097 0.3415 0.6452 0.054 Uiso 1 1 calc R . . H64B H 0.7780 0.3403 0.7292 0.054 Uiso 1 1 calc R . . C65 C 0.8542(4) 0.37337(16) 0.6573(3) 0.0561(13) Uani 1 1 d . . . H65A H 0.9211 0.3685 0.6948 0.067 Uiso 1 1 calc R . . H65B H 0.8619 0.3602 0.6098 0.067 Uiso 1 1 calc R . . C66 C 0.8344(5) 0.41687(17) 0.6463(4) 0.0705(17) Uani 1 1 d . . . H66A H 0.8002 0.4228 0.5939 0.085 Uiso 1 1 calc R . . H66B H 0.9031 0.4322 0.6590 0.085 Uiso 1 1 calc R . . C67 C 0.7593(4) 0.42709(15) 0.6984(4) 0.0664(16) Uani 1 1 d . . . H67A H 0.8009 0.4346 0.7482 0.080 Uiso 1 1 calc R . . H67B H 0.7115 0.4499 0.6786 0.080 Uiso 1 1 calc R . . O1 O 0.5322(2) 0.41237(9) 0.82827(16) 0.0433(7) Uani 1 1 d D . . O2 O 0.4835(3) 0.45338(9) 0.65931(16) 0.0464(7) Uani 1 1 d D . . O4 O 0.5364(3) 0.31843(8) 0.75991(17) 0.0454(7) Uani 1 1 d D . . O5 O 0.3239(2) 0.37647(10) 0.69921(18) 0.0518(8) Uani 1 1 d D . . O7 O 0.7628(7) 0.2618(5) 0.6065(6) 0.094(3) Uani 0.617(4) 1 d PDU B 1 C44 C 0.4470(17) 0.4134(9) 0.8711(14) 0.066(5) Uani 0.617(4) 1 d PD B 1 H44A H 0.4213 0.3857 0.8775 0.079 Uiso 0.617(4) 1 calc PR B 1 H44B H 0.3850 0.4291 0.8438 0.079 Uiso 0.617(4) 1 calc PR B 1 C45 C 0.4845(11) 0.4315(5) 0.9447(9) 0.058(3) Uani 0.617(4) 1 d PD B 1 H45A H 0.4900 0.4110 0.9846 0.069 Uiso 0.617(4) 1 calc PR B 1 H45B H 0.4343 0.4530 0.9545 0.069 Uiso 0.617(4) 1 calc PR B 1 C46 C 0.5970(12) 0.4489(4) 0.9405(10) 0.059(4) Uani 0.617(4) 1 d PD B 1 H46A H 0.5925 0.4773 0.9239 0.070 Uiso 0.617(4) 1 calc PR B 1 H46B H 0.6480 0.4466 0.9888 0.070 Uiso 0.617(4) 1 calc PR B 1 C47 C 0.6286(9) 0.4209(7) 0.8814(6) 0.042(2) Uani 0.617(4) 1 d PD B 1 H47A H 0.6832 0.4341 0.8565 0.050 Uiso 0.617(4) 1 calc PR B 1 H47B H 0.6603 0.3957 0.9049 0.050 Uiso 0.617(4) 1 calc PR B 1 C48 C 0.4958(9) 0.4904(3) 0.7016(6) 0.060(3) Uani 0.617(4) 1 d PD B 1 H48A H 0.5732 0.4945 0.7244 0.072 Uiso 0.617(4) 1 calc PR B 1 H48B H 0.4534 0.4889 0.7423 0.072 Uiso 0.617(4) 1 calc PR B 1 C49 C 0.4578(9) 0.5239(3) 0.6529(7) 0.067(3) Uani 0.617(4) 1 d PD B 1 H49A H 0.5198 0.5383 0.6382 0.081 Uiso 0.617(4) 1 calc PR B 1 H49B H 0.4161 0.5431 0.6781 0.081 Uiso 0.617(4) 1 calc PR B 1 C50 C 0.3840(10) 0.5052(3) 0.5835(5) 0.074(3) Uani 0.617(4) 1 d PD B 1 H50A H 0.3090 0.5001 0.5914 0.089 Uiso 0.617(4) 1 calc PR B 1 H50B H 0.3825 0.5213 0.5375 0.089 Uiso 0.617(4) 1 calc PR B 1 C51 C 0.451(4) 0.4669(6) 0.5846(8) 0.083(7) Uani 0.617(4) 1 d PD B 1 H51A H 0.4067 0.4459 0.5546 0.100 Uiso 0.617(4) 1 calc PR B 1 H51B H 0.5155 0.4722 0.5622 0.100 Uiso 0.617(4) 1 calc PR B 1 C56 C 0.5612(11) 0.2798(3) 0.7335(6) 0.077(4) Uani 0.617(4) 1 d PD B 1 H56A H 0.6341 0.2800 0.7199 0.092 Uiso 0.617(4) 1 calc PR B 1 H56B H 0.5070 0.2722 0.6889 0.092 Uiso 0.617(4) 1 calc PR B 1 C57 C 0.5581(12) 0.2505(4) 0.7968(7) 0.102(3) Uiso 0.617(4) 1 d PD B 1 H57A H 0.4930 0.2330 0.7850 0.122 Uiso 0.617(4) 1 calc PR B 1 H57B H 0.6236 0.2332 0.8049 0.122 Uiso 0.617(4) 1 calc PR B 1 C58 C 0.5542(11) 0.2741(3) 0.8629(6) 0.089(3) Uiso 0.617(4) 1 d PD B 1 H58A H 0.6222 0.2708 0.9001 0.106 Uiso 0.617(4) 1 calc PR B 1 H58B H 0.4921 0.2658 0.8860 0.106 Uiso 0.617(4) 1 calc PR B 1 C59 C 0.5415(11) 0.3160(3) 0.8376(6) 0.091(3) Uiso 0.617(4) 1 d PD B 1 H59A H 0.4742 0.3273 0.8505 0.109 Uiso 0.617(4) 1 calc PR B 1 H59B H 0.6037 0.3321 0.8636 0.109 Uiso 0.617(4) 1 calc PR B 1 C60 C 0.2646(13) 0.3406(4) 0.7123(8) 0.077(4) Uani 0.617(4) 1 d PD B 1 H60A H 0.2544 0.3390 0.7648 0.092 Uiso 0.617(4) 1 calc PR B 1 H60B H 0.3021 0.3160 0.6999 0.092 Uiso 0.617(4) 1 calc PR B 1 C61 C 0.1563(14) 0.3466(4) 0.6587(10) 0.090(5) Uani 0.617(4) 1 d PD B 1 H61A H 0.1602 0.3361 0.6084 0.108 Uiso 0.617(4) 1 calc PR B 1 H61B H 0.0967 0.3328 0.6774 0.108 Uiso 0.617(4) 1 calc PR B 1 C62 C 0.1386(5) 0.3916(3) 0.6562(4) 0.0535(19) Uani 0.617(4) 1 d PD B 1 H62A H 0.1020 0.4007 0.6970 0.064 Uiso 0.617(4) 1 calc PR B 1 H62B H 0.0954 0.4002 0.6077 0.064 Uiso 0.617(4) 1 calc PR B 1 C63 C 0.2539(10) 0.4071(6) 0.6667(13) 0.137(9) Uani 0.617(4) 1 d PD B 1 H63A H 0.2715 0.4149 0.6179 0.164 Uiso 0.617(4) 1 calc PR B 1 H63B H 0.2622 0.4311 0.6995 0.164 Uiso 0.617(4) 1 calc PR B 1 C68 C 0.8539(9) 0.2560(10) 0.6691(8) 0.086(3) Uani 0.617(4) 1 d PDU B 1 H68A H 0.8417 0.2326 0.7002 0.104 Uiso 0.617(4) 1 calc PR B 1 H68B H 0.8669 0.2803 0.7009 0.104 Uiso 0.617(4) 1 calc PR B 1 C69 C 0.9595(17) 0.2474(8) 0.6220(13) 0.089(4) Uani 0.617(4) 1 d PDU B 1 H69A H 1.0072 0.2712 0.6235 0.107 Uiso 0.617(4) 1 calc PR B 1 H69B H 1.0035 0.2238 0.6425 0.107 Uiso 0.617(4) 1 calc PR B 1 C70 C 0.8998(8) 0.2397(3) 0.5463(8) 0.085(2) Uani 0.617(4) 1 d PDU B 1 H70A H 0.9456 0.2448 0.5085 0.102 Uiso 0.617(4) 1 calc PR B 1 H70B H 0.8721 0.2117 0.5410 0.102 Uiso 0.617(4) 1 calc PR B 1 C71 C 0.8148(15) 0.2675(7) 0.5407(7) 0.097(3) Uani 0.617(4) 1 d PDU B 1 H71A H 0.7614 0.2630 0.4941 0.116 Uiso 0.617(4) 1 calc PR B 1 H71B H 0.8434 0.2953 0.5400 0.116 Uiso 0.617(4) 1 calc PR B 1 C62A C 0.1578(10) 0.3619(5) 0.6243(8) 0.0535(19) Uani 0.383(4) 1 d PD B 2 H62C H 0.0833 0.3731 0.6138 0.064 Uiso 0.383(4) 1 calc PR B 2 H62D H 0.1715 0.3483 0.5787 0.064 Uiso 0.383(4) 1 calc PR B 2 O7A O 0.7843(15) 0.2696(9) 0.6021(12) 0.094(3) Uani 0.383(4) 1 d PU B 2 C61A C 0.168(3) 0.3329(10) 0.6865(14) 0.090(5) Uani 0.383(4) 1 d PD B 2 H61C H 0.1844 0.3054 0.6704 0.108 Uiso 0.383(4) 1 calc PR B 2 H61D H 0.1019 0.3321 0.7088 0.108 Uiso 0.383(4) 1 calc PR B 2 C48A C 0.4496(15) 0.4823(5) 0.7091(11) 0.060(3) Uani 0.383(4) 1 d PD B 2 H48C H 0.5117 0.4901 0.7486 0.072 Uiso 0.383(4) 1 calc PR B 2 H48D H 0.3916 0.4709 0.7332 0.072 Uiso 0.383(4) 1 calc PR B 2 C49A C 0.4089(16) 0.5172(5) 0.6630(11) 0.067(3) Uani 0.383(4) 1 d PD B 2 H49C H 0.4344 0.5427 0.6883 0.081 Uiso 0.383(4) 1 calc PR B 2 H49D H 0.3285 0.5173 0.6506 0.081 Uiso 0.383(4) 1 calc PR B 2 C56A C 0.4902(17) 0.2798(4) 0.7338(10) 0.077(4) Uani 0.383(4) 1 d PD B 2 H56C H 0.5320 0.2669 0.6991 0.092 Uiso 0.383(4) 1 calc PR B 2 H56D H 0.4132 0.2824 0.7089 0.092 Uiso 0.383(4) 1 calc PR B 2 C51A C 0.475(7) 0.4660(9) 0.5832(13) 0.083(7) Uani 0.383(4) 1 d PD B 2 H51C H 0.4127 0.4534 0.5498 0.100 Uiso 0.383(4) 1 calc PR B 2 H51D H 0.5429 0.4607 0.5640 0.100 Uiso 0.383(4) 1 calc PR B 2 C50A C 0.4574(16) 0.5109(5) 0.5947(9) 0.074(3) Uani 0.383(4) 1 d PD B 2 H50C H 0.5276 0.5253 0.6003 0.089 Uiso 0.383(4) 1 calc PR B 2 H50D H 0.4081 0.5220 0.5505 0.089 Uiso 0.383(4) 1 calc PR B 2 C63A C 0.2418(13) 0.3963(6) 0.6464(10) 0.072(7) Uani 0.383(4) 1 d PD B 2 H63C H 0.2709 0.4061 0.6027 0.086 Uiso 0.383(4) 1 calc PR B 2 H63D H 0.2096 0.4191 0.6696 0.086 Uiso 0.383(4) 1 calc PR B 2 C71A C 0.794(3) 0.2605(14) 0.5321(11) 0.097(3) Uani 0.383(4) 1 d PDU B 2 H71C H 0.7638 0.2814 0.4954 0.116 Uiso 0.383(4) 1 calc PR B 2 H71D H 0.7648 0.2337 0.5157 0.116 Uiso 0.383(4) 1 calc PR B 2 C68A C 0.8721(15) 0.2573(17) 0.6528(15) 0.086(3) Uani 0.383(4) 1 d PDU B 2 H68C H 0.9018 0.2819 0.6798 0.104 Uiso 0.383(4) 1 calc PR B 2 H68D H 0.8426 0.2407 0.6896 0.104 Uiso 0.383(4) 1 calc PR B 2 C58A C 0.6249(14) 0.2690(5) 0.8377(12) 0.089(3) Uiso 0.383(4) 1 d PD B 2 H58C H 0.6492 0.2602 0.8901 0.106 Uiso 0.383(4) 1 calc PR B 2 H58D H 0.6750 0.2583 0.8063 0.106 Uiso 0.383(4) 1 calc PR B 2 C59A C 0.6124(16) 0.3133(5) 0.8312(9) 0.091(3) Uiso 0.383(4) 1 d PD B 2 H59C H 0.5818 0.3245 0.8733 0.109 Uiso 0.383(4) 1 calc PR B 2 H59D H 0.6829 0.3265 0.8299 0.109 Uiso 0.383(4) 1 calc PR B 2 C60A C 0.264(2) 0.3508(8) 0.7402(14) 0.077(4) Uani 0.383(4) 1 d PD B 2 H60C H 0.2381 0.3664 0.7796 0.092 Uiso 0.383(4) 1 calc PR B 2 H60D H 0.3122 0.3290 0.7646 0.092 Uiso 0.383(4) 1 calc PR B 2 C69A C 0.943(3) 0.2406(14) 0.641(2) 0.089(4) Uani 0.383(4) 1 d PDU B 2 H69C H 0.9319 0.2111 0.6387 0.107 Uiso 0.383(4) 1 calc PR B 2 H69D H 1.0113 0.2472 0.6759 0.107 Uiso 0.383(4) 1 calc PR B 2 C57A C 0.5010(15) 0.2569(7) 0.8061(11) 0.102(3) Uiso 0.383(4) 1 d PD B 2 H57C H 0.4914 0.2275 0.7981 0.122 Uiso 0.383(4) 1 calc PR B 2 H57D H 0.4508 0.2668 0.8381 0.122 Uiso 0.383(4) 1 calc PR B 2 C46A C 0.626(2) 0.4365(8) 0.9425(16) 0.059(4) Uani 0.383(4) 1 d PD B 2 H46C H 0.6673 0.4616 0.9567 0.070 Uiso 0.383(4) 1 calc PR B 2 H46D H 0.6516 0.4157 0.9807 0.070 Uiso 0.383(4) 1 calc PR B 2 C70A C 0.9374(14) 0.2615(6) 0.5549(13) 0.085(2) Uani 0.383(4) 1 d PDU B 2 H70C H 0.9722 0.2446 0.5213 0.102 Uiso 0.383(4) 1 calc PR B 2 H70D H 0.9675 0.2891 0.5573 0.102 Uiso 0.383(4) 1 calc PR B 2 C47A C 0.6422(16) 0.4224(12) 0.8665(12) 0.042(2) Uani 0.383(4) 1 d PD B 2 H47C H 0.6738 0.4440 0.8398 0.050 Uiso 0.383(4) 1 calc PR B 2 H47D H 0.6903 0.3986 0.8707 0.050 Uiso 0.383(4) 1 calc PR B 2 C45A C 0.5051(19) 0.4439(8) 0.9375(16) 0.058(3) Uani 0.383(4) 1 d PD B 2 H45C H 0.4808 0.4330 0.9823 0.069 Uiso 0.383(4) 1 calc PR B 2 H45D H 0.4896 0.4731 0.9344 0.069 Uiso 0.383(4) 1 calc PR B 2 C44A C 0.448(3) 0.4232(17) 0.869(2) 0.066(5) Uani 0.383(4) 1 d PD B 2 H44C H 0.4094 0.3989 0.8823 0.079 Uiso 0.383(4) 1 calc PR B 2 H44D H 0.3939 0.4414 0.8390 0.079 Uiso 0.383(4) 1 calc PR B 2 C36A C 0.0239(7) 0.3492(2) -0.0873(5) 0.0450(12) Uani 0.810(5) 1 d PD A 2 C37A C -0.0915(5) 0.3655(3) -0.0939(3) 0.073(2) Uani 0.810(5) 1 d PD A 2 H37D H -0.0900 0.3904 -0.0649 0.110 Uiso 0.810(5) 1 calc PR A 2 H37E H -0.1368 0.3455 -0.0745 0.110 Uiso 0.810(5) 1 calc PR A 2 H37F H -0.1219 0.3710 -0.1465 0.110 Uiso 0.810(5) 1 calc PR A 2 C39A C 0.0150(6) 0.3115(2) -0.1347(3) 0.067(2) Uani 0.810(5) 1 d PD A 2 H39D H -0.0217 0.3179 -0.1857 0.101 Uiso 0.810(5) 1 calc PR A 2 H39E H -0.0271 0.2912 -0.1134 0.101 Uiso 0.810(5) 1 calc PR A 2 H39F H 0.0879 0.3011 -0.1357 0.101 Uiso 0.810(5) 1 calc PR A 2 C38A C 0.0899(6) 0.3801(2) -0.1213(4) 0.072(2) Uani 0.810(5) 1 d PD A 2 H38D H 0.1637 0.3699 -0.1199 0.108 Uiso 0.810(5) 1 calc PR A 2 H38E H 0.0935 0.4052 -0.0927 0.108 Uiso 0.810(5) 1 calc PR A 2 H38F H 0.0552 0.3853 -0.1732 0.108 Uiso 0.810(5) 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 0.0254(7) 0.0343(8) 0.0303(7) -0.0038(6) 0.0069(6) -0.0014(6) Zn1 0.02307(19) 0.0310(2) 0.0269(2) -0.00735(17) 0.00350(15) 0.00703(16) Zn2 0.0328(2) 0.0462(3) 0.0202(2) -0.00141(18) 0.00861(16) -0.00663(19) O3 0.0494(18) 0.076(2) 0.0380(17) -0.0203(16) 0.0131(14) -0.0223(17) O6 0.0339(15) 0.0416(17) 0.069(2) -0.0172(15) 0.0209(15) -0.0081(13) N1 0.0175(12) 0.0234(14) 0.0193(13) 0.0013(10) 0.0047(10) 0.0015(10) N2 0.0180(13) 0.0194(13) 0.0198(13) 0.0020(10) 0.0004(10) -0.0001(10) C2 0.0203(15) 0.0221(16) 0.0195(15) -0.0008(12) 0.0008(12) -0.0006(12) C1 0.0182(14) 0.0205(15) 0.0216(15) 0.0035(12) 0.0038(12) -0.0009(12) C3 0.0203(15) 0.0242(16) 0.0192(15) -0.0026(12) 0.0029(12) 0.0022(12) C4 0.0173(14) 0.0313(18) 0.0185(15) 0.0007(13) 0.0059(12) 0.0026(13) C5 0.0189(16) 0.0358(19) 0.0273(17) 0.0017(15) 0.0052(13) 0.0015(14) C6 0.0166(16) 0.050(2) 0.037(2) -0.0030(18) 0.0071(14) 0.0045(16) C7 0.0262(19) 0.053(3) 0.039(2) -0.0034(19) 0.0106(16) 0.0127(17) C8 0.037(2) 0.034(2) 0.038(2) -0.0035(17) 0.0105(17) 0.0109(17) C9 0.0275(17) 0.0320(19) 0.0252(17) -0.0007(14) 0.0090(14) 0.0043(14) C10 0.0304(19) 0.0236(18) 0.046(2) -0.0001(16) 0.0064(17) 0.0022(14) C11 0.069(3) 0.041(3) 0.081(4) -0.019(3) 0.022(3) -0.014(2) C12 0.045(3) 0.048(3) 0.059(3) 0.015(2) 0.023(2) 0.001(2) C13 0.0189(16) 0.035(2) 0.045(2) 0.0017(17) 0.0021(15) -0.0031(14) C14 0.0232(19) 0.050(3) 0.074(3) 0.013(2) 0.004(2) -0.0081(18) C15 0.034(2) 0.042(2) 0.057(3) -0.012(2) -0.0039(19) -0.0068(18) C16 0.0170(14) 0.0246(16) 0.0219(15) -0.0001(13) 0.0007(12) 0.0002(12) C17 0.0236(17) 0.033(2) 0.0277(18) 0.0073(15) -0.0025(14) -0.0039(14) C18 0.0282(19) 0.046(2) 0.034(2) 0.0127(17) -0.0063(15) 0.0006(17) C19 0.0179(16) 0.049(2) 0.036(2) 0.0037(18) -0.0037(14) -0.0015(16) C20 0.0191(16) 0.0333(19) 0.0323(18) -0.0012(15) 0.0045(14) -0.0048(14) C21 0.0193(15) 0.0236(16) 0.0230(16) -0.0011(13) 0.0054(12) -0.0010(12) C22 0.0238(16) 0.0248(17) 0.0313(18) 0.0045(14) 0.0058(14) -0.0033(13) C23 0.041(2) 0.040(2) 0.031(2) 0.0065(17) 0.0099(17) 0.0011(17) C24 0.052(3) 0.030(2) 0.041(2) 0.0045(17) 0.0105(19) -0.0051(18) C25 0.031(2) 0.047(2) 0.044(2) 0.025(2) -0.0065(17) -0.0065(18) C26 0.060(3) 0.109(5) 0.050(3) 0.039(3) 0.000(2) -0.032(3) C27 0.086(4) 0.045(3) 0.111(5) 0.021(3) 0.019(4) -0.016(3) C28 0.045(2) 0.079(3) 0.025(2) 0.009(2) 0.0103(18) -0.013(2) C29 0.043(3) 0.093(4) 0.043(3) 0.009(3) 0.014(2) -0.035(3) C30 0.048(3) 0.114(5) 0.042(3) 0.003(3) 0.025(2) -0.009(3) C31 0.067(3) 0.119(5) 0.028(2) 0.013(3) 0.017(2) -0.035(3) C32 0.058(3) 0.059(3) 0.0239(19) -0.0137(19) 0.0146(19) -0.014(2) C33 0.091(5) 0.100(5) 0.045(3) 0.010(3) -0.020(3) -0.041(4) C34 0.059(3) 0.051(3) 0.047(3) -0.017(2) 0.018(2) -0.015(2) C35 0.113(5) 0.100(5) 0.078(4) -0.056(4) 0.058(4) -0.041(4) C36 0.046(3) 0.063(3) 0.025(2) -0.009(2) 0.0041(18) 0.019(2) C37 0.062(4) 0.128(7) 0.024(3) -0.013(3) -0.007(3) 0.046(4) C38 0.068(4) 0.086(5) 0.041(3) -0.031(3) -0.010(3) 0.021(4) C39 0.092(5) 0.089(6) 0.033(3) 0.011(3) 0.003(3) 0.003(5) C40 0.0283(19) 0.036(2) 0.043(2) -0.0123(17) 0.0046(16) 0.0099(16) C41 0.033(2) 0.050(3) 0.060(3) -0.012(2) -0.006(2) 0.0171(19) C42 0.042(3) 0.039(3) 0.130(5) -0.033(3) -0.005(3) 0.014(2) C43 0.046(3) 0.113(5) 0.069(4) 0.001(3) 0.025(3) 0.038(3) C52 0.058(3) 0.059(3) 0.042(3) -0.005(2) 0.010(2) -0.003(2) C53 0.041(2) 0.059(3) 0.045(2) -0.002(2) 0.0106(19) 0.001(2) C54 0.059(3) 0.050(3) 0.050(3) -0.001(2) 0.008(2) -0.011(2) C55 0.062(3) 0.084(4) 0.055(3) -0.024(3) 0.016(3) -0.029(3) C64 0.034(2) 0.048(3) 0.052(3) -0.006(2) 0.0068(19) 0.0038(19) C65 0.045(3) 0.069(3) 0.060(3) -0.006(3) 0.026(2) 0.002(2) C66 0.058(3) 0.057(3) 0.108(5) -0.007(3) 0.046(3) -0.009(3) C67 0.053(3) 0.045(3) 0.112(5) -0.026(3) 0.045(3) -0.020(2) O1 0.0395(16) 0.0554(19) 0.0355(15) -0.0071(14) 0.0084(12) 0.0007(14) O2 0.059(2) 0.0388(16) 0.0417(17) -0.0052(13) 0.0086(15) 0.0067(14) O4 0.061(2) 0.0319(15) 0.0439(17) 0.0011(13) 0.0117(15) 0.0031(14) O5 0.0274(15) 0.068(2) 0.060(2) 0.0084(17) 0.0064(14) -0.0040(14) O7 0.044(4) 0.061(7) 0.173(5) -0.027(4) 0.004(3) -0.004(4) C44 0.060(3) 0.076(15) 0.070(4) -0.019(7) 0.033(3) 0.005(5) C45 0.058(6) 0.082(10) 0.039(4) 0.001(6) 0.025(4) -0.011(5) C46 0.085(9) 0.057(9) 0.042(3) -0.022(6) 0.034(6) -0.026(6) C47 0.041(4) 0.058(3) 0.029(6) -0.003(5) 0.015(3) -0.013(3) C48 0.075(8) 0.042(5) 0.056(4) -0.019(4) -0.006(6) 0.010(5) C49 0.075(8) 0.044(5) 0.084(6) -0.009(4) 0.018(6) -0.002(5) C50 0.112(9) 0.050(5) 0.049(4) -0.002(3) -0.012(6) 0.019(6) C51 0.15(2) 0.053(4) 0.057(4) 0.003(3) 0.044(5) 0.028(5) C56 0.133(11) 0.047(4) 0.059(4) 0.004(3) 0.038(8) 0.018(7) C60 0.055(4) 0.086(9) 0.098(12) 0.009(7) 0.036(7) -0.008(6) C61 0.064(6) 0.115(14) 0.102(15) -0.028(9) 0.041(10) -0.047(9) C62 0.025(3) 0.092(6) 0.042(4) -0.003(3) -0.001(3) -0.002(3) C63 0.022(6) 0.142(15) 0.23(2) 0.030(14) -0.007(9) -0.005(8) C68 0.065(5) 0.050(4) 0.143(6) -0.014(7) 0.016(5) -0.007(5) C69 0.056(6) 0.070(8) 0.137(9) -0.008(7) 0.004(5) 0.008(6) C70 0.054(5) 0.060(6) 0.137(7) -0.002(6) 0.007(5) -0.002(4) C71 0.063(6) 0.060(8) 0.155(6) 0.010(5) -0.015(5) -0.014(5) C62A 0.025(3) 0.092(6) 0.042(4) -0.003(3) -0.001(3) -0.002(3) O7A 0.044(4) 0.061(7) 0.173(5) -0.027(4) 0.004(3) -0.004(4) C61A 0.064(6) 0.115(14) 0.102(15) -0.028(9) 0.041(10) -0.047(9) C48A 0.075(8) 0.042(5) 0.056(4) -0.019(4) -0.006(6) 0.010(5) C49A 0.075(8) 0.044(5) 0.084(6) -0.009(4) 0.018(6) -0.002(5) C56A 0.133(11) 0.047(4) 0.059(4) 0.004(3) 0.038(8) 0.018(7) C51A 0.15(2) 0.053(4) 0.057(4) 0.003(3) 0.044(5) 0.028(5) C50A 0.112(9) 0.050(5) 0.049(4) -0.002(3) -0.012(6) 0.019(6) C63A 0.042(10) 0.124(17) 0.047(8) 0.066(11) 0.003(6) 0.008(9) C71A 0.063(6) 0.060(8) 0.155(6) 0.010(5) -0.015(5) -0.014(5) C68A 0.065(5) 0.050(4) 0.143(6) -0.014(7) 0.016(5) -0.007(5) C60A 0.055(4) 0.086(9) 0.098(12) 0.009(7) 0.036(7) -0.008(6) C69A 0.056(6) 0.070(8) 0.137(9) -0.008(7) 0.004(5) 0.008(6) C46A 0.085(9) 0.057(9) 0.042(3) -0.022(6) 0.034(6) -0.026(6) C70A 0.054(5) 0.060(6) 0.137(7) -0.002(6) 0.007(5) -0.002(4) C47A 0.041(4) 0.058(3) 0.029(6) -0.003(5) 0.015(3) -0.013(3) C45A 0.058(6) 0.082(10) 0.039(4) 0.001(6) 0.025(4) -0.011(5) C44A 0.060(3) 0.076(15) 0.070(4) -0.019(7) 0.033(3) 0.005(5) C36A 0.046(3) 0.063(3) 0.025(2) -0.009(2) 0.0041(18) 0.019(2) C37A 0.062(4) 0.128(7) 0.024(3) -0.013(3) -0.007(3) 0.046(4) C39A 0.068(4) 0.086(5) 0.041(3) -0.031(3) -0.010(3) 0.021(4) C38A 0.092(5) 0.089(6) 0.033(3) 0.011(3) 0.003(3) 0.003(5) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 O6 2.335(3) . ? Na1 O5 2.348(3) . ? Na1 O1 2.404(3) . ? Na1 O3 2.408(3) . ? Na1 O2 2.411(3) . ? Na1 O4 2.438(3) . ? Zn1 C36 2.06(4) . ? Zn1 C2 2.058(3) . ? Zn1 C40 2.058(4) . ? Zn1 C36A 2.075(9) . ? Zn2 C32 2.030(4) . ? Zn2 C28 2.047(4) . ? Zn2 C1 2.114(3) . ? O3 C55 1.403(6) . ? O3 C52 1.421(5) . ? O6 C67 1.423(5) . ? O6 C64 1.429(5) . ? N1 C1 1.359(4) . ? N1 C3 1.394(4) . ? N1 C4 1.440(4) . ? N2 C1 1.367(4) . ? N2 C2 1.423(4) . ? N2 C16 1.443(4) . ? C2 C3 1.362(4) . ? C3 H3 0.9500 . ? C4 C5 1.402(5) . ? C4 C9 1.407(5) . ? C5 C6 1.398(5) . ? C5 C13 1.520(5) . ? C6 C7 1.375(6) . ? C6 H6 0.9500 . ? C7 C8 1.373(6) . ? C7 H7 0.9500 . ? C8 C9 1.395(5) . ? C8 H8 0.9500 . ? C9 C10 1.522(5) . ? C10 C11 1.524(6) . ? C10 C12 1.529(6) . ? C10 H10 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C15 1.530(6) . ? C13 C14 1.540(5) . ? C13 H13 1.0000 . ? 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 1.401(5) . ? C16 C21 1.403(4) . ? C17 C18 1.397(5) . ? C17 C25 1.520(5) . ? C18 C19 1.377(5) . ? C18 H18 0.9500 . ? C19 C20 1.383(5) . ? C19 H19 0.9500 . ? C20 C21 1.382(4) . ? C20 H20 0.9500 . ? C21 C22 1.524(5) . ? C22 C24 1.529(5) . ? C22 C23 1.532(5) . ? C22 H22 1.0000 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C26 1.513(7) . ? C25 C27 1.530(7) . ? C25 H25 1.0000 . ? 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 C29 1.528(7) . ? C28 C30 1.532(7) . ? C28 C31 1.536(6) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 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 C34 1.518(6) . ? C32 C35 1.521(7) . ? C32 C33 1.539(7) . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? 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 C39 1.53(2) . ? C36 C38 1.53(2) . ? C36 C37 1.53(2) . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 C41 1.507(6) . ? C40 C42 1.517(6) . ? C40 C43 1.533(6) . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C52 C53 1.511(6) . ? C52 H52A 0.9900 . ? C52 H52B 0.9900 . ? C53 C54 1.520(6) . ? C53 H53A 0.9900 . ? C53 H53B 0.9900 . ? C54 C55 1.542(7) . ? C54 H54A 0.9900 . ? C54 H54B 0.9900 . ? C55 H55A 0.9900 . ? C55 H55B 0.9900 . ? C64 C65 1.509(6) . ? C64 H64A 0.9900 . ? C64 H64B 0.9900 . ? C65 C66 1.475(7) . ? C65 H65A 0.9900 . ? C65 H65B 0.9900 . ? C66 C67 1.494(7) . ? C66 H66A 0.9900 . ? C66 H66B 0.9900 . ? C67 H67A 0.9900 . ? C67 H67B 0.9900 . ? O1 C47 1.428(11) . ? O1 C44 1.434(13) . ? O1 C44A 1.448(18) . ? O1 C47A 1.461(17) . ? O2 C51 1.420(13) . ? O2 C51A 1.434(18) . ? O2 C48A 1.439(15) . ? O2 C48 1.446(9) . ? O4 C59 1.408(10) . ? O4 C56 1.425(9) . ? O4 C56A 1.452(15) . ? O4 C59A 1.470(14) . ? O5 C63 1.402(14) . ? O5 C60A 1.431(17) . ? O5 C63A 1.432(13) . ? O5 C60 1.448(12) . ? O7 C68 1.468(10) . ? O7 C71 1.479(10) . ? C44 C45 1.464(13) . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C45 C46 1.538(13) . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C46 C47 1.528(13) . ? C46 H46A 0.9900 . ? C46 H46B 0.9900 . ? C47 H47A 0.9900 . ? C47 H47B 0.9900 . ? C48 C49 1.448(12) . ? C48 H48A 0.9900 . ? C48 H48B 0.9900 . ? C49 C50 1.550(12) . ? C49 H49A 0.9900 . ? C49 H49B 0.9900 . ? C50 C51 1.521(16) . ? C50 H50A 0.9900 . ? C50 H50B 0.9900 . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? C56 C57 1.516(12) . ? C56 H56A 0.9900 . ? C56 H56B 0.9900 . ? C57 C58 1.446(13) . ? C57 H57A 0.9900 . ? C57 H57B 0.9900 . ? C58 C59 1.466(12) . ? C58 H58A 0.9900 . ? C58 H58B 0.9900 . ? C59 H59A 0.9900 . ? C59 H59B 0.9900 . ? C60 C61 1.530(15) . ? C60 H60A 0.9900 . ? C60 H60B 0.9900 . ? C61 C62 1.510(15) . ? C61 H61A 0.9900 . ? C61 H61B 0.9900 . ? C62 C63 1.511(14) . ? C62 H62A 0.9900 . ? C62 H62B 0.9900 . ? C63 H63A 0.9900 . ? C63 H63B 0.9900 . ? C68 C69 1.73(3) . ? C68 H68A 0.9900 . ? C68 H68B 0.9900 . ? C69 C70 1.46(3) . ? C69 H69A 0.9900 . ? C69 H69B 0.9900 . ? C70 C71 1.40(3) . ? C70 H70A 0.9900 . ? C70 H70B 0.9900 . ? C71 H71A 0.9900 . ? C71 H71B 0.9900 . ? C62A C61A 1.476(17) . ? C62A C63A 1.554(17) . ? C62A H62C 0.9900 . ? C62A H62D 0.9900 . ? O7A C71A 1.34(3) . ? O7A C68A 1.36(3) . ? C61A C60A 1.525(18) . ? C61A H61C 0.9900 . ? C61A H61D 0.9900 . ? C48A C49A 1.469(17) . ? C48A H48C 0.9900 . ? C48A H48D 0.9900 . ? C49A C50A 1.496(16) . ? C49A H49C 0.9900 . ? C49A H49D 0.9900 . ? C56A C57A 1.505(16) . ? C56A H56C 0.9900 . ? C56A H56D 0.9900 . ? C51A C50A 1.53(2) . ? C51A H51C 0.9900 . ? C51A H51D 0.9900 . ? C50A H50C 0.9900 . ? C50A H50D 0.9900 . ? C63A H63C 0.9900 . ? C63A H63D 0.9900 . ? C71A C70A 1.76(4) . ? C71A H71C 0.9900 . ? C71A H71D 0.9900 . ? C68A C69A 1.11(6) . ? C68A H68C 0.9900 . ? C68A H68D 0.9900 . ? C58A C59A 1.486(16) . ? C58A C57A 1.603(17) . ? C58A H58C 0.9900 . ? C58A H58D 0.9900 . ? C59A H59C 0.9900 . ? C59A H59D 0.9900 . ? C60A H60C 0.9900 . ? C60A H60D 0.9900 . ? C69A C70A 1.70(4) . ? C69A H69C 0.9900 . ? C69A H69D 0.9900 . ? C57A H57C 0.9900 . ? C57A H57D 0.9900 . ? C46A C47A 1.512(17) . ? C46A C45A 1.517(18) . ? C46A H46C 0.9900 . ? C46A H46D 0.9900 . ? C70A H70C 0.9900 . ? C70A H70D 0.9900 . ? C47A H47C 0.9900 . ? C47A H47D 0.9900 . ? C45A C44A 1.488(18) . ? C45A H45C 0.9900 . ? C45A H45D 0.9900 . ? C44A H44C 0.9900 . ? C44A H44D 0.9900 . ? C36A C39A 1.514(9) . ? C36A C38A 1.522(10) . ? C36A C37A 1.527(9) . ? C37A H37D 0.9800 . ? C37A H37E 0.9800 . ? C37A H37F 0.9800 . ? C39A H39D 0.9800 . ? C39A H39E 0.9800 . ? C39A H39F 0.9800 . ? C38A H38D 0.9800 . ? C38A H38E 0.9800 . ? C38A H38F 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 O6 Na1 O5 176.97(13) . . ? O6 Na1 O1 92.02(11) . . ? O5 Na1 O1 90.93(12) . . ? O6 Na1 O3 88.35(12) . . ? O5 Na1 O3 88.76(12) . . ? O1 Na1 O3 175.48(14) . . ? O6 Na1 O2 89.48(12) . . ? O5 Na1 O2 91.37(12) . . ? O1 Na1 O2 87.09(11) . . ? O3 Na1 O2 88.41(12) . . ? O6 Na1 O4 92.04(12) . . ? O5 Na1 O4 87.36(12) . . ? O1 Na1 O4 88.07(11) . . ? O3 Na1 O4 96.42(12) . . ? O2 Na1 O4 174.98(12) . . ? C36 Zn1 C2 109.2(7) . . ? C36 Zn1 C40 123.7(7) . . ? C2 Zn1 C40 127.09(14) . . ? C36 Zn1 C36A 4.8(9) . . ? C2 Zn1 C36A 113.6(2) . . ? C40 Zn1 C36A 119.3(2) . . ? C32 Zn2 C28 122.64(17) . . ? C32 Zn2 C1 124.15(14) . . ? C28 Zn2 C1 113.17(15) . . ? C55 O3 C52 103.9(4) . . ? C55 O3 Na1 121.5(3) . . ? C52 O3 Na1 134.0(3) . . ? C67 O6 C64 109.1(3) . . ? C67 O6 Na1 129.5(3) . . ? C64 O6 Na1 118.9(2) . . ? C1 N1 C3 110.4(3) . . ? C1 N1 C4 126.4(3) . . ? C3 N1 C4 122.1(3) . . ? C1 N2 C2 114.7(3) . . ? C1 N2 C16 121.3(3) . . ? C2 N2 C16 123.0(3) . . ? C3 C2 N2 101.2(3) . . ? C3 C2 Zn1 123.0(2) . . ? N2 C2 Zn1 135.7(2) . . ? N1 C1 N2 103.0(3) . . ? N1 C1 Zn2 127.9(2) . . ? N2 C1 Zn2 128.3(2) . . ? C2 C3 N1 110.7(3) . . ? C2 C3 H3 124.7 . . ? N1 C3 H3 124.7 . . ? C5 C4 C9 122.0(3) . . ? C5 C4 N1 119.2(3) . . ? C9 C4 N1 118.6(3) . . ? C6 C5 C4 117.6(3) . . ? C6 C5 C13 118.8(3) . . ? C4 C5 C13 123.6(3) . . ? C7 C6 C5 121.2(4) . . ? C7 C6 H6 119.4 . . ? C5 C6 H6 119.4 . . ? C8 C7 C6 120.3(3) . . ? C8 C7 H7 119.8 . . ? C6 C7 H7 119.8 . . ? C7 C8 C9 121.4(4) . . ? C7 C8 H8 119.3 . . ? C9 C8 H8 119.3 . . ? C8 C9 C4 117.5(3) . . ? C8 C9 C10 120.1(3) . . ? C4 C9 C10 122.3(3) . . ? C9 C10 C11 113.4(3) . . ? C9 C10 C12 109.4(3) . . ? C11 C10 C12 111.3(4) . . ? C9 C10 H10 107.5 . . ? C11 C10 H10 107.5 . . ? C12 C10 H10 107.5 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C5 C13 C15 110.6(3) . . ? C5 C13 C14 111.6(3) . . ? C15 C13 C14 109.3(3) . . ? C5 C13 H13 108.4 . . ? C15 C13 H13 108.4 . . ? C14 C13 H13 108.4 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C17 C16 C21 122.0(3) . . ? C17 C16 N2 119.9(3) . . ? C21 C16 N2 118.1(3) . . ? C18 C17 C16 117.6(3) . . ? C18 C17 C25 119.4(3) . . ? C16 C17 C25 123.0(3) . . ? C19 C18 C17 121.2(3) . . ? C19 C18 H18 119.4 . . ? C17 C18 H18 119.4 . . ? C18 C19 C20 119.7(3) . . ? C18 C19 H19 120.1 . . ? C20 C19 H19 120.1 . . ? C21 C20 C19 121.8(3) . . ? C21 C20 H20 119.1 . . ? C19 C20 H20 119.1 . . ? C20 C21 C16 117.6(3) . . ? C20 C21 C22 119.6(3) . . ? C16 C21 C22 122.8(3) . . ? C21 C22 C24 112.8(3) . . ? C21 C22 C23 110.5(3) . . ? C24 C22 C23 109.2(3) . . ? C21 C22 H22 108.0 . . ? C24 C22 H22 108.0 . . ? C23 C22 H22 108.0 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C26 C25 C17 112.3(4) . . ? C26 C25 C27 108.7(4) . . ? C17 C25 C27 111.0(4) . . ? C26 C25 H25 108.2 . . ? C17 C25 H25 108.2 . . ? C27 C25 H25 108.2 . . ? 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 . . ? C29 C28 C30 108.6(4) . . ? C29 C28 C31 107.6(4) . . ? C30 C28 C31 107.2(4) . . ? C29 C28 Zn2 113.2(3) . . ? C30 C28 Zn2 107.6(3) . . ? C31 C28 Zn2 112.4(3) . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C28 C30 H30A 109.5 . . ? C28 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C28 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C28 C31 H31A 109.5 . . ? C28 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C28 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C34 C32 C35 107.8(4) . . ? C34 C32 C33 105.8(4) . . ? C35 C32 C33 108.3(5) . . ? C34 C32 Zn2 115.9(3) . . ? C35 C32 Zn2 109.3(4) . . ? C33 C32 Zn2 109.6(3) . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C32 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C32 C34 H34A 109.5 . . ? C32 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C32 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C32 C35 H35A 109.5 . . ? C32 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C32 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C39 C36 C38 107.3(19) . . ? C39 C36 C37 106.4(18) . . ? C38 C36 C37 107.4(19) . . ? C39 C36 Zn1 112.4(19) . . ? C38 C36 Zn1 109.3(18) . . ? C37 C36 Zn1 113.7(19) . . ? C41 C40 C42 107.7(4) . . ? C41 C40 C43 107.0(4) . . ? C42 C40 C43 108.1(4) . . ? C41 C40 Zn1 116.3(3) . . ? C42 C40 Zn1 106.3(3) . . ? C43 C40 Zn1 111.3(3) . . ? C40 C41 H41A 109.5 . . ? C40 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C40 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C40 C42 H42A 109.5 . . ? C40 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C40 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C40 C43 H43A 109.5 . . ? C40 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C40 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? O3 C52 C53 106.5(4) . . ? O3 C52 H52A 110.4 . . ? C53 C52 H52A 110.4 . . ? O3 C52 H52B 110.4 . . ? C53 C52 H52B 110.4 . . ? H52A C52 H52B 108.6 . . ? C52 C53 C54 104.0(4) . . ? C52 C53 H53A 111.0 . . ? C54 C53 H53A 111.0 . . ? C52 C53 H53B 111.0 . . ? C54 C53 H53B 111.0 . . ? H53A C53 H53B 109.0 . . ? C53 C54 C55 102.5(4) . . ? C53 C54 H54A 111.3 . . ? C55 C54 H54A 111.3 . . ? C53 C54 H54B 111.3 . . ? C55 C54 H54B 111.3 . . ? H54A C54 H54B 109.2 . . ? O3 C55 C54 105.4(4) . . ? O3 C55 H55A 110.7 . . ? C54 C55 H55A 110.7 . . ? O3 C55 H55B 110.7 . . ? C54 C55 H55B 110.7 . . ? H55A C55 H55B 108.8 . . ? O6 C64 C65 106.9(4) . . ? O6 C64 H64A 110.3 . . ? C65 C64 H64A 110.3 . . ? O6 C64 H64B 110.3 . . ? C65 C64 H64B 110.3 . . ? H64A C64 H64B 108.6 . . ? C66 C65 C64 105.0(4) . . ? C66 C65 H65A 110.7 . . ? C64 C65 H65A 110.7 . . ? C66 C65 H65B 110.7 . . ? C64 C65 H65B 110.7 . . ? H65A C65 H65B 108.8 . . ? C65 C66 C67 104.2(4) . . ? C65 C66 H66A 110.9 . . ? C67 C66 H66A 110.9 . . ? C65 C66 H66B 110.9 . . ? C67 C66 H66B 110.9 . . ? H66A C66 H66B 108.9 . . ? O6 C67 C66 105.7(4) . . ? O6 C67 H67A 110.6 . . ? C66 C67 H67A 110.6 . . ? O6 C67 H67B 110.6 . . ? C66 C67 H67B 110.6 . . ? H67A C67 H67B 108.7 . . ? C47 O1 C44 104.3(11) . . ? C47 O1 C44A 102.1(16) . . ? C44 O1 C44A 13(4) . . ? C47 O1 C47A 13.9(12) . . ? C44 O1 C47A 117.8(13) . . ? C44A O1 C47A 114.4(18) . . ? C47 O1 Na1 130.1(5) . . ? C44 O1 Na1 123.9(9) . . ? C44A O1 Na1 127.8(15) . . ? C47A O1 Na1 117.6(10) . . ? C51 O2 C51A 13(5) . . ? C51 O2 C48A 109.0(11) . . ? C51A O2 C48A 116.0(14) . . ? C51 O2 C48 102.9(10) . . ? C51A O2 C48 104.3(15) . . ? C48A O2 C48 27.1(8) . . ? C51 O2 Na1 128.3(9) . . ? C51A O2 Na1 125.6(10) . . ? C48A O2 Na1 117.0(8) . . ? C48 O2 Na1 128.7(5) . . ? C59 O4 C56 108.4(7) . . ? C59 O4 C56A 102.7(8) . . ? C56 O4 C56A 36.0(8) . . ? C59 O4 C59A 37.2(8) . . ? C56 O4 C59A 92.8(9) . . ? C56A O4 C59A 109.9(10) . . ? C59 O4 Na1 116.7(5) . . ? C56 O4 Na1 134.3(4) . . ? C56A O4 Na1 131.0(8) . . ? C59A O4 Na1 119.1(7) . . ? C63 O5 C60A 108.0(16) . . ? C63 O5 C63A 21.0(17) . . ? C60A O5 C63A 104.3(15) . . ? C63 O5 C60 111.7(9) . . ? C60A O5 C60 24.6(11) . . ? C63A O5 C60 99.4(10) . . ? C63 O5 Na1 117.9(6) . . ? C60A O5 Na1 131.8(14) . . ? C63A O5 Na1 123.8(7) . . ? C60 O5 Na1 129.4(7) . . ? C68 O7 C71 104.5(12) . . ? O1 C44 C45 111.3(14) . . ? O1 C44 H44A 109.4 . . ? C45 C44 H44A 109.4 . . ? O1 C44 H44B 109.4 . . ? C45 C44 H44B 109.4 . . ? H44A C44 H44B 108.0 . . ? C44 C45 C46 104.5(13) . . ? C44 C45 H45A 110.9 . . ? C46 C45 H45A 110.9 . . ? C44 C45 H45B 110.9 . . ? C46 C45 H45B 110.9 . . ? H45A C45 H45B 108.9 . . ? C47 C46 C45 99.5(12) . . ? C47 C46 H46A 111.9 . . ? C45 C46 H46A 111.9 . . ? C47 C46 H46B 111.9 . . ? C45 C46 H46B 111.9 . . ? H46A C46 H46B 109.6 . . ? O1 C47 C46 107.6(12) . . ? O1 C47 H47A 110.2 . . ? C46 C47 H47A 110.2 . . ? O1 C47 H47B 110.2 . . ? C46 C47 H47B 110.2 . . ? H47A C47 H47B 108.5 . . ? O2 C48 C49 109.7(8) . . ? O2 C48 H48A 109.7 . . ? C49 C48 H48A 109.7 . . ? O2 C48 H48B 109.7 . . ? C49 C48 H48B 109.7 . . ? H48A C48 H48B 108.2 . . ? C48 C49 C50 105.7(8) . . ? C48 C49 H49A 110.6 . . ? C50 C49 H49A 110.6 . . ? C48 C49 H49B 110.6 . . ? C50 C49 H49B 110.6 . . ? H49A C49 H49B 108.7 . . ? C51 C50 C49 94.7(15) . . ? C51 C50 H50A 112.8 . . ? C49 C50 H50A 112.8 . . ? C51 C50 H50B 112.8 . . ? C49 C50 H50B 112.8 . . ? H50A C50 H50B 110.2 . . ? O2 C51 C50 109.8(10) . . ? O2 C51 H51A 109.7 . . ? C50 C51 H51A 109.7 . . ? O2 C51 H51B 109.7 . . ? C50 C51 H51B 109.7 . . ? H51A C51 H51B 108.2 . . ? O4 C56 C57 106.5(8) . . ? O4 C56 H56A 110.4 . . ? C57 C56 H56A 110.4 . . ? O4 C56 H56B 110.4 . . ? C57 C56 H56B 110.4 . . ? H56A C56 H56B 108.6 . . ? C58 C57 C56 107.0(10) . . ? C58 C57 H57A 110.3 . . ? C56 C57 H57A 110.3 . . ? C58 C57 H57B 110.3 . . ? C56 C57 H57B 110.3 . . ? H57A C57 H57B 108.6 . . ? C57 C58 C59 105.9(10) . . ? C57 C58 H58A 110.6 . . ? C59 C58 H58A 110.6 . . ? C57 C58 H58B 110.6 . . ? C59 C58 H58B 110.6 . . ? H58A C58 H58B 108.7 . . ? O4 C59 C58 110.6(9) . . ? O4 C59 H59A 109.5 . . ? C58 C59 H59A 109.5 . . ? O4 C59 H59B 109.5 . . ? C58 C59 H59B 109.5 . . ? H59A C59 H59B 108.1 . . ? O5 C60 C61 101.9(11) . . ? O5 C60 H60A 111.4 . . ? C61 C60 H60A 111.4 . . ? O5 C60 H60B 111.4 . . ? C61 C60 H60B 111.4 . . ? H60A C60 H60B 109.2 . . ? C62 C61 C60 104.9(12) . . ? C62 C61 H61A 110.8 . . ? C60 C61 H61A 110.8 . . ? C62 C61 H61B 110.8 . . ? C60 C61 H61B 110.8 . . ? H61A C61 H61B 108.8 . . ? C61 C62 C63 101.7(11) . . ? C61 C62 H62A 111.4 . . ? C63 C62 H62A 111.4 . . ? C61 C62 H62B 111.4 . . ? C63 C62 H62B 111.4 . . ? H62A C62 H62B 109.3 . . ? O5 C63 C62 108.2(11) . . ? O5 C63 H63A 110.1 . . ? C62 C63 H63A 110.1 . . ? O5 C63 H63B 110.1 . . ? C62 C63 H63B 110.1 . . ? H63A C63 H63B 108.4 . . ? O7 C68 C69 101.0(13) . . ? O7 C68 H68A 111.6 . . ? C69 C68 H68A 111.6 . . ? O7 C68 H68B 111.6 . . ? C69 C68 H68B 111.6 . . ? H68A C68 H68B 109.4 . . ? C70 C69 C68 101.1(13) . . ? C70 C69 H69A 111.5 . . ? C68 C69 H69A 111.5 . . ? C70 C69 H69B 111.5 . . ? C68 C69 H69B 111.5 . . ? H69A C69 H69B 109.4 . . ? C71 C70 C69 101.6(13) . . ? C71 C70 H70A 111.5 . . ? C69 C70 H70A 111.5 . . ? C71 C70 H70B 111.5 . . ? C69 C70 H70B 111.5 . . ? H70A C70 H70B 109.3 . . ? C70 C71 O7 107.3(17) . . ? C70 C71 H71A 110.3 . . ? O7 C71 H71A 110.3 . . ? C70 C71 H71B 110.3 . . ? O7 C71 H71B 110.3 . . ? H71A C71 H71B 108.5 . . ? C61A C62A C63A 108.9(16) . . ? C61A C62A H62C 109.9 . . ? C63A C62A H62C 109.9 . . ? C61A C62A H62D 109.9 . . ? C63A C62A H62D 109.9 . . ? H62C C62A H62D 108.3 . . ? C71A O7A C68A 112(3) . . ? C62A C61A C60A 101(2) . . ? C62A C61A H61C 111.7 . . ? C60A C61A H61C 111.7 . . ? C62A C61A H61D 111.7 . . ? C60A C61A H61D 111.7 . . ? H61C C61A H61D 109.4 . . ? O2 C48A C49A 106.2(14) . . ? O2 C48A H48C 110.5 . . ? C49A C48A H48C 110.5 . . ? O2 C48A H48D 110.5 . . ? C49A C48A H48D 110.5 . . ? H48C C48A H48D 108.7 . . ? C48A C49A C50A 102.3(15) . . ? C48A C49A H49C 111.3 . . ? C50A C49A H49C 111.3 . . ? C48A C49A H49D 111.3 . . ? C50A C49A H49D 111.3 . . ? H49C C49A H49D 109.2 . . ? O4 C56A C57A 101.3(13) . . ? O4 C56A H56C 111.5 . . ? C57A C56A H56C 111.5 . . ? O4 C56A H56D 111.5 . . ? C57A C56A H56D 111.5 . . ? H56C C56A H56D 109.3 . . ? O2 C51A C50A 98.0(15) . . ? O2 C51A H51C 112.2 . . ? C50A C51A H51C 112.2 . . ? O2 C51A H51D 112.2 . . ? C50A C51A H51D 112.2 . . ? H51C C51A H51D 109.8 . . ? C49A C50A C51A 110(2) . . ? C49A C50A H50C 109.6 . . ? C51A C50A H50C 109.6 . . ? C49A C50A H50D 109.6 . . ? C51A C50A H50D 109.6 . . ? H50C C50A H50D 108.2 . . ? O5 C63A C62A 101.7(11) . . ? O5 C63A H63C 111.4 . . ? C62A C63A H63C 111.4 . . ? O5 C63A H63D 111.4 . . ? C62A C63A H63D 111.4 . . ? H63C C63A H63D 109.3 . . ? O7A C71A C70A 92(2) . . ? O7A C71A H71C 113.2 . . ? C70A C71A H71C 113.2 . . ? O7A C71A H71D 113.2 . . ? C70A C71A H71D 113.2 . . ? H71C C71A H71D 110.6 . . ? C69A C68A O7A 127(4) . . ? C69A C68A H68C 105.7 . . ? O7A C68A H68C 105.7 . . ? C69A C68A H68D 105.7 . . ? O7A C68A H68D 105.7 . . ? H68C C68A H68D 106.1 . . ? C59A C58A C57A 98.0(14) . . ? C59A C58A H58C 112.2 . . ? C57A C58A H58C 112.2 . . ? C59A C58A H58D 112.2 . . ? C57A C58A H58D 112.2 . . ? H58C C58A H58D 109.8 . . ? O4 C59A C58A 103.1(13) . . ? O4 C59A H59C 111.1 . . ? C58A C59A H59C 111.1 . . ? O4 C59A H59D 111.1 . . ? C58A C59A H59D 111.1 . . ? H59C C59A H59D 109.1 . . ? O5 C60A C61A 108.9(19) . . ? O5 C60A H60C 109.9 . . ? C61A C60A H60C 109.9 . . ? O5 C60A H60D 109.9 . . ? C61A C60A H60D 109.9 . . ? H60C C60A H60D 108.3 . . ? C68A C69A C70A 94(3) . . ? C68A C69A H69C 112.8 . . ? C70A C69A H69C 112.8 . . ? C68A C69A H69D 112.8 . . ? C70A C69A H69D 112.8 . . ? H69C C69A H69D 110.3 . . ? C56A C57A C58A 96.4(15) . . ? C56A C57A H57C 112.5 . . ? C58A C57A H57C 112.5 . . ? C56A C57A H57D 112.5 . . ? C58A C57A H57D 112.5 . . ? H57C C57A H57D 110.0 . . ? C47A C46A C45A 107(2) . . ? C47A C46A H46C 110.3 . . ? C45A C46A H46C 110.3 . . ? C47A C46A H46D 110.3 . . ? C45A C46A H46D 110.3 . . ? H46C C46A H46D 108.5 . . ? C69A C70A C71A 94.5(18) . . ? C69A C70A H70C 112.8 . . ? C71A C70A H70C 112.8 . . ? C69A C70A H70D 112.8 . . ? C71A C70A H70D 112.8 . . ? H70C C70A H70D 110.3 . . ? O1 C47A C46A 103.4(18) . . ? O1 C47A H47C 111.1 . . ? C46A C47A H47C 111.1 . . ? O1 C47A H47D 111.1 . . ? C46A C47A H47D 111.1 . . ? H47C C47A H47D 109.0 . . ? C44A C45A C46A 107(3) . . ? C44A C45A H45C 110.3 . . ? C46A C45A H45C 110.3 . . ? C44A C45A H45D 110.3 . . ? C46A C45A H45D 110.3 . . ? H45C C45A H45D 108.5 . . ? O1 C44A C45A 105(2) . . ? O1 C44A H44C 110.8 . . ? C45A C44A H44C 110.8 . . ? O1 C44A H44D 110.8 . . ? C45A C44A H44D 110.8 . . ? H44C C44A H44D 108.8 . . ? C39A C36A C38A 108.4(7) . . ? C39A C36A C37A 106.2(7) . . ? C38A C36A C37A 107.8(7) . . ? C39A C36A Zn1 111.4(5) . . ? C38A C36A Zn1 106.0(5) . . ? C37A C36A Zn1 116.7(5) . . ? C36A C37A H37D 109.5 . . ? C36A C37A H37E 109.5 . . ? H37D C37A H37E 109.5 . . ? C36A C37A H37F 109.5 . . ? H37D C37A H37F 109.5 . . ? H37E C37A H37F 109.5 . . ? C36A C39A H39D 109.5 . . ? C36A C39A H39E 109.5 . . ? H39D C39A H39E 109.5 . . ? C36A C39A H39F 109.5 . . ? H39D C39A H39F 109.5 . . ? H39E C39A H39F 109.5 . . ? C36A C38A H38D 109.5 . . ? C36A C38A H38E 109.5 . . ? H38D C38A H38E 109.5 . . ? C36A C38A H38F 109.5 . . ? H38D C38A H38F 109.5 . . ? H38E C38A H38F 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 O6 Na1 O3 C55 133.7(4) . . . . ? O5 Na1 O3 C55 -45.4(4) . . . . ? O1 Na1 O3 C55 -131.5(15) . . . . ? O2 Na1 O3 C55 -136.8(4) . . . . ? O4 Na1 O3 C55 41.8(4) . . . . ? O6 Na1 O3 C52 -35.7(4) . . . . ? O5 Na1 O3 C52 145.3(4) . . . . ? O1 Na1 O3 C52 59.2(17) . . . . ? O2 Na1 O3 C52 53.9(4) . . . . ? O4 Na1 O3 C52 -127.5(4) . . . . ? O5 Na1 O6 C67 121(3) . . . . ? O1 Na1 O6 C67 -72.0(4) . . . . ? O3 Na1 O6 C67 103.5(4) . . . . ? O2 Na1 O6 C67 15.1(4) . . . . ? O4 Na1 O6 C67 -160.1(4) . . . . ? O5 Na1 O6 C64 -39(3) . . . . ? O1 Na1 O6 C64 127.6(3) . . . . ? O3 Na1 O6 C64 -56.9(3) . . . . ? O2 Na1 O6 C64 -145.4(3) . . . . ? O4 Na1 O6 C64 39.4(3) . . . . ? C1 N2 C2 C3 -0.1(4) . . . . ? C16 N2 C2 C3 -168.9(3) . . . . ? C1 N2 C2 Zn1 177.1(3) . . . . ? C16 N2 C2 Zn1 8.3(5) . . . . ? C36 Zn1 C2 C3 20.5(9) . . . . ? C40 Zn1 C2 C3 -158.7(3) . . . . ? C36A Zn1 C2 C3 18.5(4) . . . . ? C36 Zn1 C2 N2 -156.3(9) . . . . ? C40 Zn1 C2 N2 24.5(4) . . . . ? C36A Zn1 C2 N2 -158.3(4) . . . . ? C3 N1 C1 N2 -0.6(3) . . . . ? C4 N1 C1 N2 -169.4(3) . . . . ? C3 N1 C1 Zn2 -171.0(2) . . . . ? C4 N1 C1 Zn2 20.3(5) . . . . ? C2 N2 C1 N1 0.5(3) . . . . ? C16 N2 C1 N1 169.5(3) . . . . ? C2 N2 C1 Zn2 170.7(2) . . . . ? C16 N2 C1 Zn2 -20.2(4) . . . . ? C32 Zn2 C1 N1 -130.3(3) . . . . ? C28 Zn2 C1 N1 47.7(3) . . . . ? C32 Zn2 C1 N2 61.7(3) . . . . ? C28 Zn2 C1 N2 -120.2(3) . . . . ? N2 C2 C3 N1 -0.3(3) . . . . ? Zn1 C2 C3 N1 -178.0(2) . . . . ? C1 N1 C3 C2 0.6(4) . . . . ? C4 N1 C3 C2 170.0(3) . . . . ? C1 N1 C4 C5 -124.0(3) . . . . ? C3 N1 C4 C5 68.4(4) . . . . ? C1 N1 C4 C9 61.3(4) . . . . ? C3 N1 C4 C9 -106.3(4) . . . . ? C9 C4 C5 C6 -2.9(5) . . . . ? N1 C4 C5 C6 -177.4(3) . . . . ? C9 C4 C5 C13 175.5(3) . . . . ? N1 C4 C5 C13 1.0(5) . . . . ? C4 C5 C6 C7 1.1(6) . . . . ? C13 C5 C6 C7 -177.4(4) . . . . ? C5 C6 C7 C8 0.0(6) . . . . ? C6 C7 C8 C9 0.7(6) . . . . ? C7 C8 C9 C4 -2.3(6) . . . . ? C7 C8 C9 C10 172.8(4) . . . . ? C5 C4 C9 C8 3.5(5) . . . . ? N1 C4 C9 C8 178.1(3) . . . . ? C5 C4 C9 C10 -171.5(3) . . . . ? N1 C4 C9 C10 3.0(5) . . . . ? C8 C9 C10 C11 34.2(5) . . . . ? C4 C9 C10 C11 -150.9(4) . . . . ? C8 C9 C10 C12 -90.7(4) . . . . ? C4 C9 C10 C12 84.2(4) . . . . ? C6 C5 C13 C15 71.1(4) . . . . ? C4 C5 C13 C15 -107.3(4) . . . . ? C6 C5 C13 C14 -50.9(5) . . . . ? C4 C5 C13 C14 130.8(4) . . . . ? C1 N2 C16 C17 80.0(4) . . . . ? C2 N2 C16 C17 -111.8(4) . . . . ? C1 N2 C16 C21 -100.3(4) . . . . ? C2 N2 C16 C21 67.8(4) . . . . ? C21 C16 C17 C18 1.4(5) . . . . ? N2 C16 C17 C18 -178.9(3) . . . . ? C21 C16 C17 C25 -176.7(4) . . . . ? N2 C16 C17 C25 2.9(5) . . . . ? C16 C17 C18 C19 -0.7(6) . . . . ? C25 C17 C18 C19 177.5(4) . . . . ? C17 C18 C19 C20 -0.2(6) . . . . ? C18 C19 C20 C21 0.5(6) . . . . ? C19 C20 C21 C16 0.1(5) . . . . ? C19 C20 C21 C22 -178.4(3) . . . . ? C17 C16 C21 C20 -1.2(5) . . . . ? N2 C16 C21 C20 179.2(3) . . . . ? C17 C16 C21 C22 177.3(3) . . . . ? N2 C16 C21 C22 -2.3(5) . . . . ? C20 C21 C22 C24 -56.9(4) . . . . ? C16 C21 C22 C24 124.6(4) . . . . ? C20 C21 C22 C23 65.7(4) . . . . ? C16 C21 C22 C23 -112.8(4) . . . . ? C18 C17 C25 C26 57.5(6) . . . . ? C16 C17 C25 C26 -124.4(4) . . . . ? C18 C17 C25 C27 -64.5(5) . . . . ? C16 C17 C25 C27 113.7(5) . . . . ? C32 Zn2 C28 C29 -148.9(3) . . . . ? C1 Zn2 C28 C29 33.0(4) . . . . ? C32 Zn2 C28 C30 91.1(4) . . . . ? C1 Zn2 C28 C30 -87.1(3) . . . . ? C32 Zn2 C28 C31 -26.7(5) . . . . ? C1 Zn2 C28 C31 155.2(4) . . . . ? C28 Zn2 C32 C34 -171.4(3) . . . . ? C1 Zn2 C32 C34 6.5(5) . . . . ? C28 Zn2 C32 C35 -49.4(5) . . . . ? C1 Zn2 C32 C35 128.5(4) . . . . ? C28 Zn2 C32 C33 69.0(4) . . . . ? C1 Zn2 C32 C33 -113.1(4) . . . . ? C2 Zn1 C36 C39 162.9(14) . . . . ? C40 Zn1 C36 C39 -17.8(19) . . . . ? C36A Zn1 C36 C39 -40(11) . . . . ? C2 Zn1 C36 C38 -78.0(15) . . . . ? C40 Zn1 C36 C38 101.3(14) . . . . ? C36A Zn1 C36 C38 79(11) . . . . ? C2 Zn1 C36 C37 41.9(17) . . . . ? C40 Zn1 C36 C37 -138.8(14) . . . . ? C36A Zn1 C36 C37 -161(12) . . . . ? C36 Zn1 C40 C41 154.6(10) . . . . ? C2 Zn1 C40 C41 -26.2(4) . . . . ? C36A Zn1 C40 C41 156.7(4) . . . . ? C36 Zn1 C40 C42 -85.6(10) . . . . ? C2 Zn1 C40 C42 93.6(4) . . . . ? C36A Zn1 C40 C42 -83.5(4) . . . . ? C36 Zn1 C40 C43 31.8(10) . . . . ? C2 Zn1 C40 C43 -149.0(3) . . . . ? C36A Zn1 C40 C43 33.9(5) . . . . ? C55 O3 C52 C53 -39.9(5) . . . . ? Na1 O3 C52 C53 130.8(4) . . . . ? O3 C52 C53 C54 21.2(5) . . . . ? C52 C53 C54 C55 3.7(5) . . . . ? C52 O3 C55 C54 42.1(5) . . . . ? Na1 O3 C55 C54 -130.0(3) . . . . ? C53 C54 C55 O3 -27.8(5) . . . . ? C67 O6 C64 C65 -7.4(5) . . . . ? Na1 O6 C64 C65 156.8(3) . . . . ? O6 C64 C65 C66 -11.9(6) . . . . ? C64 C65 C66 C67 25.5(6) . . . . ? C64 O6 C67 C66 23.6(6) . . . . ? Na1 O6 C67 C66 -138.3(4) . . . . ? C65 C66 C67 O6 -30.5(7) . . . . ? O6 Na1 O1 C47 -10.0(12) . . . . ? O5 Na1 O1 C47 169.3(12) . . . . ? O3 Na1 O1 C47 -104.7(19) . . . . ? O2 Na1 O1 C47 -99.4(12) . . . . ? O4 Na1 O1 C47 82.0(12) . . . . ? O6 Na1 O1 C44 -172.6(17) . . . . ? O5 Na1 O1 C44 6.7(17) . . . . ? O3 Na1 O1 C44 93(2) . . . . ? O2 Na1 O1 C44 98.0(17) . . . . ? O4 Na1 O1 C44 -80.6(17) . . . . ? O6 Na1 O1 C44A 172(3) . . . . ? O5 Na1 O1 C44A -9(3) . . . . ? O3 Na1 O1 C44A 77(4) . . . . ? O2 Na1 O1 C44A 83(3) . . . . ? O4 Na1 O1 C44A -96(3) . . . . ? O6 Na1 O1 C47A -2.8(18) . . . . ? O5 Na1 O1 C47A 176.5(18) . . . . ? O3 Na1 O1 C47A -97(2) . . . . ? O2 Na1 O1 C47A -92.1(18) . . . . ? O4 Na1 O1 C47A 89.2(18) . . . . ? O6 Na1 O2 C51 96(2) . . . . ? O5 Na1 O2 C51 -81(2) . . . . ? O1 Na1 O2 C51 -172(2) . . . . ? O3 Na1 O2 C51 8(2) . . . . ? O4 Na1 O2 C51 -156(3) . . . . ? O6 Na1 O2 C51A 81(4) . . . . ? O5 Na1 O2 C51A -97(4) . . . . ? O1 Na1 O2 C51A 173(4) . . . . ? O3 Na1 O2 C51A -8(4) . . . . ? O4 Na1 O2 C51A -172(4) . . . . ? O6 Na1 O2 C48A -113.5(9) . . . . ? O5 Na1 O2 C48A 69.4(9) . . . . ? O1 Na1 O2 C48A -21.5(9) . . . . ? O3 Na1 O2 C48A 158.1(9) . . . . ? O4 Na1 O2 C48A -5.9(18) . . . . ? O6 Na1 O2 C48 -84.3(6) . . . . ? O5 Na1 O2 C48 98.6(6) . . . . ? O1 Na1 O2 C48 7.8(6) . . . . ? O3 Na1 O2 C48 -172.6(6) . . . . ? O4 Na1 O2 C48 23.3(17) . . . . ? O6 Na1 O4 C59 98.7(7) . . . . ? O5 Na1 O4 C59 -84.2(7) . . . . ? O1 Na1 O4 C59 6.8(7) . . . . ? O3 Na1 O4 C59 -172.7(7) . . . . ? O2 Na1 O4 C59 -8.8(17) . . . . ? O6 Na1 O4 C56 -71.9(9) . . . . ? O5 Na1 O4 C56 105.1(9) . . . . ? O1 Na1 O4 C56 -163.9(9) . . . . ? O3 Na1 O4 C56 16.6(9) . . . . ? O2 Na1 O4 C56 -179(100) . . . . ? O6 Na1 O4 C56A -121.4(10) . . . . ? O5 Na1 O4 C56A 55.6(10) . . . . ? O1 Na1 O4 C56A 146.6(10) . . . . ? O3 Na1 O4 C56A -32.9(10) . . . . ? O2 Na1 O4 C56A 131.1(17) . . . . ? O6 Na1 O4 C59A 56.5(10) . . . . ? O5 Na1 O4 C59A -126.5(10) . . . . ? O1 Na1 O4 C59A -35.5(10) . . . . ? O3 Na1 O4 C59A 145.0(10) . . . . ? O2 Na1 O4 C59A -51.0(18) . . . . ? O6 Na1 O5 C63 -99(3) . . . . ? O1 Na1 O5 C63 94.4(12) . . . . ? O3 Na1 O5 C63 -81.1(12) . . . . ? O2 Na1 O5 C63 7.3(12) . . . . ? O4 Na1 O5 C63 -177.6(12) . . . . ? O6 Na1 O5 C60A 101(3) . . . . ? O1 Na1 O5 C60A -66.1(13) . . . . ? O3 Na1 O5 C60A 118.4(13) . . . . ? O2 Na1 O5 C60A -153.2(13) . . . . ? O4 Na1 O5 C60A 21.9(13) . . . . ? O6 Na1 O5 C63A -75(3) . . . . ? O1 Na1 O5 C63A 117.9(13) . . . . ? O3 Na1 O5 C63A -57.5(13) . . . . ? O2 Na1 O5 C63A 30.8(13) . . . . ? O4 Na1 O5 C63A -154.0(13) . . . . ? O6 Na1 O5 C60 68(3) . . . . ? O1 Na1 O5 C60 -98.5(7) . . . . ? O3 Na1 O5 C60 86.0(7) . . . . ? O2 Na1 O5 C60 174.4(7) . . . . ? O4 Na1 O5 C60 -10.5(7) . . . . ? C47 O1 C44 C45 13(3) . . . . ? C44A O1 C44 C45 -69(11) . . . . ? C47A O1 C44 C45 10(3) . . . . ? Na1 O1 C44 C45 179.7(13) . . . . ? O1 C44 C45 C46 10(3) . . . . ? C44 C45 C46 C47 -26(2) . . . . ? C44 O1 C47 C46 -31(2) . . . . ? C44A O1 C47 C46 -18(3) . . . . ? C47A O1 C47 C46 136(12) . . . . ? Na1 O1 C47 C46 163.3(7) . . . . ? C45 C46 C47 O1 36.3(17) . . . . ? C51 O2 C48 C49 7(2) . . . . ? C51A O2 C48 C49 20(4) . . . . ? C48A O2 C48 C49 -100(3) . . . . ? Na1 O2 C48 C49 -172.9(6) . . . . ? O2 C48 C49 C50 19.3(12) . . . . ? C48 C49 C50 C51 -34.4(17) . . . . ? C51A O2 C51 C50 -130(14) . . . . ? C48A O2 C51 C50 -4(3) . . . . ? C48 O2 C51 C50 -32(3) . . . . ? Na1 O2 C51 C50 147.9(13) . . . . ? C49 C50 C51 O2 41(3) . . . . ? C59 O4 C56 C57 12.2(13) . . . . ? C56A O4 C56 C57 -74.1(16) . . . . ? C59A O4 C56 C57 46.7(13) . . . . ? Na1 O4 C56 C57 -176.5(7) . . . . ? O4 C56 C57 C58 -11.8(15) . . . . ? C56 C57 C58 C59 6.8(16) . . . . ? C56 O4 C59 C58 -8.3(13) . . . . ? C56A O4 C59 C58 28.6(13) . . . . ? C59A O4 C59 C58 -77.6(16) . . . . ? Na1 O4 C59 C58 178.7(8) . . . . ? C57 C58 C59 O4 0.6(15) . . . . ? C63 O5 C60 C61 20.4(16) . . . . ? C60A O5 C60 C61 106(5) . . . . ? C63A O5 C60 C61 2.6(14) . . . . ? Na1 O5 C60 C61 -147.4(9) . . . . ? O5 C60 C61 C62 -32.6(13) . . . . ? C60 C61 C62 C63 32.2(15) . . . . ? C60A O5 C63 C62 -26(2) . . . . ? C63A O5 C63 C62 57(3) . . . . ? C60 O5 C63 C62 0(2) . . . . ? Na1 O5 C63 C62 169.1(9) . . . . ? C61 C62 C63 O5 -20.3(19) . . . . ? C71 O7 C68 C69 -14(2) . . . . ? O7 C68 C69 C70 -14(2) . . . . ? C68 C69 C70 C71 38(2) . . . . ? C69 C70 C71 O7 -52.0(16) . . . . ? C68 O7 C71 C70 42(2) . . . . ? C63A C62A C61A C60A -4(3) . . . . ? C51 O2 C48A C49A -8(3) . . . . ? C51A O2 C48A C49A 3(4) . . . . ? C48 O2 C48A C49A 73(3) . . . . ? Na1 O2 C48A C49A -164.2(10) . . . . ? O2 C48A C49A C50A -18.4(18) . . . . ? C59 O4 C56A C57A -13.2(15) . . . . ? C56 O4 C56A C57A 91(2) . . . . ? C59A O4 C56A C57A 25.0(17) . . . . ? Na1 O4 C56A C57A -156.9(10) . . . . ? C51 O2 C51A C50A 72(9) . . . . ? C48A O2 C51A C50A 13(6) . . . . ? C48 O2 C51A C50A -13(5) . . . . ? Na1 O2 C51A C50A 179.3(15) . . . . ? C48A C49A C50A C51A 28(4) . . . . ? O2 C51A C50A C49A -25(5) . . . . ? C63 O5 C63A C62A -141(4) . . . . ? C60A O5 C63A C62A -38.2(17) . . . . ? C60 O5 C63A C62A -13.6(15) . . . . ? Na1 O5 C63A C62A 138.6(8) . . . . ? C61A C62A C63A O5 26(3) . . . . ? C68A O7A C71A C70A -27(4) . . . . ? C71A O7A C68A C69A -3(7) . . . . ? C59 O4 C59A C58A 95.8(19) . . . . ? C56 O4 C59A C58A -21.6(15) . . . . ? C56A O4 C59A C58A 10.9(18) . . . . ? Na1 O4 C59A C58A -167.4(10) . . . . ? C57A C58A C59A O4 -39.4(18) . . . . ? C63 O5 C60A C61A 60(3) . . . . ? C63A O5 C60A C61A 39(3) . . . . ? C60 O5 C60A C61A -42(4) . . . . ? Na1 O5 C60A C61A -138(2) . . . . ? C62A C61A C60A O5 -21(3) . . . . ? O7A C68A C69A C70A 31(6) . . . . ? O4 C56A C57A C58A -47.2(17) . . . . ? C59A C58A C57A C56A 53.9(19) . . . . ? C68A C69A C70A C71A -39(4) . . . . ? O7A C71A C70A C69A 37(3) . . . . ? C47 O1 C47A C46A -21(8) . . . . ? C44 O1 C47A C46A -7(4) . . . . ? C44A O1 C47A C46A 7(4) . . . . ? Na1 O1 C47A C46A -177.5(17) . . . . ? C45A C46A C47A O1 -14(3) . . . . ? C47A C46A C45A C44A 17(4) . . . . ? C47 O1 C44A C45A 10(4) . . . . ? C44 O1 C44A C45A 111(15) . . . . ? C47A O1 C44A C45A 3(5) . . . . ? Na1 O1 C44A C45A -171.7(17) . . . . ? C46A C45A C44A O1 -12(5) . . . . ? C36 Zn1 C36A C39A -158(12) . . . . ? C2 Zn1 C36A C39A -134.5(5) . . . . ? C40 Zn1 C36A C39A 42.9(6) . . . . ? C36 Zn1 C36A C38A 84(11) . . . . ? C2 Zn1 C36A C38A 107.8(5) . . . . ? C40 Zn1 C36A C38A -74.8(5) . . . . ? C36 Zn1 C36A C37A -36(11) . . . . ? C2 Zn1 C36A C37A -12.3(7) . . . . ? C40 Zn1 C36A C37A 165.2(6) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.976 _refine_diff_density_min -0.603 _refine_diff_density_rms 0.075 _database_code_depnum_ccdc_archive 'CCDC 923039' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_seb446ark #TrackingRef 'hevia5.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C39 H63 Li N2 Zn' _chemical_formula_weight 632.22 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Pbca 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' '-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 21.8628(13) _cell_length_b 22.1892(11) _cell_length_c 31.9347(14) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 15492.1(14) _cell_formula_units_Z 16 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 6860 _cell_measurement_theta_min 2.6876 _cell_measurement_theta_max 29.7102 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.084 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5504 _exptl_absorpt_coefficient_mu 0.660 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.28884 _exptl_absorpt_correction_T_max 1.00000 _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 ; Very weak diffraction, especially at high angles. Lots of non-indexed peaks. After multiple attemps, this was the best that could be found. ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford diffraction Gemini S' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 43518 _diffrn_reflns_av_R_equivalents 0.3604 _diffrn_reflns_av_sigmaI/netI 0.3924 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_theta_min 2.69 _diffrn_reflns_theta_max 25.00 _reflns_number_total 13585 _reflns_number_gt 5496 _reflns_threshold_expression I>2\s(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^ > 2\s(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^)+(0.0918P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13585 _refine_ls_number_parameters 809 _refine_ls_number_restraints 144 _refine_ls_R_factor_all 0.2203 _refine_ls_R_factor_gt 0.0897 _refine_ls_wR_factor_ref 0.2639 _refine_ls_wR_factor_gt 0.1845 _refine_ls_goodness_of_fit_ref 0.915 _refine_ls_restrained_S_all 0.911 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Li1 Li 0.0200(4) 0.4824(6) 0.2389(3) 0.025(3) Uani 1 1 d . . . Li2 Li 0.2515(5) 0.2791(6) 0.9868(4) 0.036(3) Uani 1 1 d . . . Zn1 Zn 0.10547(3) 0.46989(5) 0.19019(2) 0.0292(3) Uani 1 1 d . . . Zn2 Zn 0.27089(3) 0.37121(4) 0.94276(2) 0.0309(3) Uani 1 1 d . . . N1 N 0.2889(2) 0.1428(3) 1.01294(16) 0.0239(14) Uani 1 1 d U . . N2 N 0.2150(2) 0.1395(3) 0.97018(16) 0.0218(13) Uani 1 1 d U . . N3 N -0.1146(2) 0.5208(3) 0.27044(16) 0.0222(14) Uani 1 1 d . . . N4 N -0.1220(2) 0.4421(3) 0.23141(15) 0.0223(14) Uani 1 1 d . . . C1 C 0.2516(2) 0.1797(4) 0.99047(19) 0.0227(15) Uani 1 1 d U . . C2 C 0.2288(3) 0.0802(4) 0.9791(2) 0.0311(17) Uani 1 1 d U . . H2 H 0.2095 0.0452 0.9682 0.037 Uiso 1 1 calc R . . C3 C 0.2751(3) 0.0825(4) 1.0064(2) 0.0262(16) Uani 1 1 d U . . H3 H 0.2949 0.0490 1.0190 0.031 Uiso 1 1 calc R . . C4 C 0.1619(3) 0.1582(4) 0.9449(2) 0.0256(15) Uani 1 1 d U . . C5 C 0.1702(3) 0.1739(3) 0.90337(19) 0.0210(15) Uani 1 1 d U . . C6 C 0.1185(3) 0.1911(4) 0.8814(2) 0.0281(16) Uani 1 1 d U . . H6 H 0.1224 0.2029 0.8529 0.034 Uiso 1 1 calc R . . C7 C 0.0615(3) 0.1917(4) 0.8998(2) 0.0311(17) Uani 1 1 d U . . H7 H 0.0268 0.2045 0.8842 0.037 Uiso 1 1 calc R . . C8 C 0.0550(3) 0.1736(4) 0.9409(2) 0.0355(18) Uani 1 1 d U . . H8 H 0.0154 0.1728 0.9531 0.043 Uiso 1 1 calc R . . C9 C 0.1050(3) 0.1565(4) 0.96487(19) 0.0262(16) Uani 1 1 d U . . C10 C 0.2319(3) 0.1429(5) 0.8404(2) 0.051(3) Uani 1 1 d . . . H10A H 0.2111 0.1682 0.8197 0.077 Uiso 1 1 calc R . . H10B H 0.2103 0.1044 0.8431 0.077 Uiso 1 1 calc R . . H10C H 0.2741 0.1354 0.8313 0.077 Uiso 1 1 calc R . . C11 C 0.2325(3) 0.1755(4) 0.8834(2) 0.0254(17) Uani 1 1 d U . . H11 H 0.2614 0.1534 0.9022 0.030 Uiso 1 1 calc R . . C12 C 0.2557(4) 0.2383(5) 0.8786(3) 0.072(3) Uani 1 1 d . . . H12A H 0.2263 0.2619 0.8622 0.109 Uiso 1 1 calc R . . H12B H 0.2952 0.2376 0.8641 0.109 Uiso 1 1 calc R . . H12C H 0.2607 0.2566 0.9063 0.109 Uiso 1 1 calc R . . C13 C 0.0592(3) 0.0765(4) 1.0112(3) 0.055(3) Uani 1 1 d . . . H13A H 0.0193 0.0828 0.9980 0.083 Uiso 1 1 calc R . . H13B H 0.0533 0.0638 1.0404 0.083 Uiso 1 1 calc R . . H13C H 0.0817 0.0451 0.9960 0.083 Uiso 1 1 calc R . . C14 C 0.0961(3) 0.1360(4) 1.0102(2) 0.035(2) Uani 1 1 d . . . H14 H 0.1375 0.1276 1.0223 0.042 Uiso 1 1 calc R . . C15 C 0.0666(3) 0.1843(4) 1.0366(2) 0.046(2) Uani 1 1 d . . . H15A H 0.0920 0.2206 1.0361 0.069 Uiso 1 1 calc R . . H15B H 0.0625 0.1700 1.0655 0.069 Uiso 1 1 calc R . . H15C H 0.0260 0.1936 1.0253 0.069 Uiso 1 1 calc R . . C16 C 0.3320(3) 0.1625(4) 1.04485(19) 0.0252(18) Uani 1 1 d . . . C17 C 0.3089(3) 0.1831(4) 1.0827(2) 0.0262(18) Uani 1 1 d . . . C18 C 0.3508(3) 0.1996(4) 1.1134(2) 0.035(2) Uani 1 1 d . . . H18 H 0.3368 0.2136 1.1398 0.042 Uiso 1 1 calc R . . C19 C 0.4131(3) 0.1955(4) 1.1054(2) 0.035(2) Uani 1 1 d . . . H19 H 0.4414 0.2066 1.1266 0.042 Uiso 1 1 calc R . . C20 C 0.4344(3) 0.1759(4) 1.0678(2) 0.036(2) Uani 1 1 d . . . H20 H 0.4773 0.1751 1.0630 0.043 Uiso 1 1 calc R . . C21 C 0.3949(3) 0.1571(4) 1.0364(2) 0.0282(19) Uani 1 1 d . . . C22 C 0.2208(3) 0.2367(4) 1.1202(2) 0.051(3) Uani 1 1 d . . . H22A H 0.1767 0.2435 1.1172 0.077 Uiso 1 1 calc R . . H22B H 0.2430 0.2730 1.1117 0.077 Uiso 1 1 calc R . . H22C H 0.2303 0.2273 1.1495 0.077 Uiso 1 1 calc R . . C23 C 0.2400(3) 0.1843(4) 1.0926(2) 0.031(2) Uani 1 1 d . . . H23 H 0.2183 0.1895 1.0653 0.037 Uiso 1 1 calc R . . C24 C 0.2199(3) 0.1241(4) 1.1103(3) 0.053(3) Uani 1 1 d . . . H24A H 0.2370 0.1190 1.1384 0.079 Uiso 1 1 calc R . . H24B H 0.2347 0.0916 1.0921 0.079 Uiso 1 1 calc R . . H24C H 0.1752 0.1228 1.1117 0.079 Uiso 1 1 calc R . . C25 C 0.4709(3) 0.1695(4) 0.9771(2) 0.043(2) Uani 1 1 d . . . H25A H 0.4550 0.2098 0.9709 0.064 Uiso 1 1 calc R . . H25B H 0.4855 0.1506 0.9513 0.064 Uiso 1 1 calc R . . H25C H 0.5049 0.1728 0.9971 0.064 Uiso 1 1 calc R . . C26 C 0.4206(3) 0.1313(4) 0.9960(2) 0.033(2) Uani 1 1 d . . . H26 H 0.3865 0.1288 0.9752 0.040 Uiso 1 1 calc R . . C27 C 0.4446(3) 0.0670(4) 1.0038(2) 0.045(2) Uani 1 1 d . . . H27A H 0.4784 0.0684 1.0239 0.068 Uiso 1 1 calc R . . H27B H 0.4590 0.0497 0.9774 0.068 Uiso 1 1 calc R . . H27C H 0.4115 0.0420 1.0152 0.068 Uiso 1 1 calc R . . C28 C -0.0800(2) 0.4815(3) 0.24766(18) 0.0171(16) Uani 1 1 d . . . C29 C -0.1809(3) 0.4580(4) 0.2438(2) 0.033(2) Uani 1 1 d . . . H29 H -0.2176 0.4382 0.2358 0.040 Uiso 1 1 calc R . . C31 C -0.1767(3) 0.5052(4) 0.2684(2) 0.034(2) Uani 1 1 d . . . H31 H -0.2095 0.5250 0.2822 0.041 Uiso 1 1 calc R . . C32 C -0.0908(3) 0.5694(4) 0.2949(2) 0.0276(18) Uani 1 1 d . . . C33 C -0.0598(2) 0.5570(4) 0.3325(2) 0.028(2) Uani 1 1 d . . . C34 C -0.0361(3) 0.6054(4) 0.3537(2) 0.039(2) Uani 1 1 d . . . H34 H -0.0129 0.5983 0.3783 0.047 Uiso 1 1 calc R . . C35 C -0.0446(3) 0.6644(4) 0.3404(2) 0.039(2) Uani 1 1 d . . . H35 H -0.0289 0.6973 0.3561 0.046 Uiso 1 1 calc R . . C36 C -0.0769(3) 0.6739(4) 0.3034(2) 0.043(2) Uani 1 1 d . . . H36 H -0.0823 0.7140 0.2937 0.051 Uiso 1 1 calc R . . C37 C -0.1010(3) 0.6277(4) 0.2806(2) 0.031(2) Uani 1 1 d . . . C38 C -0.1109(3) 0.4757(4) 0.3732(2) 0.045(2) Uani 1 1 d . . . H38A H -0.1161 0.5034 0.3969 0.067 Uiso 1 1 calc R . . H38B H -0.1064 0.4344 0.3838 0.067 Uiso 1 1 calc R . . H38C H -0.1469 0.4779 0.3550 0.067 Uiso 1 1 calc R . . C39 C -0.0541(3) 0.4932(4) 0.34853(19) 0.032(2) Uani 1 1 d . . . H39 H -0.0519 0.4661 0.3236 0.038 Uiso 1 1 calc R . . C40 C 0.0042(3) 0.4826(4) 0.3744(2) 0.047(2) Uani 1 1 d . . . H40A H 0.0398 0.4970 0.3587 0.071 Uiso 1 1 calc R . . H40B H 0.0088 0.4395 0.3802 0.071 Uiso 1 1 calc R . . H40C H 0.0012 0.5047 0.4010 0.071 Uiso 1 1 calc R . . C41 C -0.1996(3) 0.6710(5) 0.2530(2) 0.054(3) Uani 1 1 d . . . H41A H -0.1922 0.7115 0.2642 0.081 Uiso 1 1 calc R . . H41B H -0.2196 0.6462 0.2744 0.081 Uiso 1 1 calc R . . H41C H -0.2260 0.6738 0.2283 0.081 Uiso 1 1 calc R . . C42 C -0.1376(3) 0.6418(4) 0.2406(2) 0.039(2) Uani 1 1 d . . . H42 H -0.1464 0.6029 0.2259 0.047 Uiso 1 1 calc R . . C43 C -0.1033(3) 0.6826(5) 0.2105(2) 0.052(3) Uani 1 1 d . . . H43A H -0.0959 0.7217 0.2239 0.078 Uiso 1 1 calc R . . H43B H -0.1278 0.6885 0.1851 0.078 Uiso 1 1 calc R . . H43C H -0.0641 0.6640 0.2031 0.078 Uiso 1 1 calc R . . C45 C -0.1082(3) 0.3902(4) 0.2072(2) 0.030(2) Uani 1 1 d . . . C46 C -0.1092(3) 0.3337(4) 0.2279(2) 0.0305(19) Uani 1 1 d . . . C47 C -0.0970(3) 0.2834(4) 0.2048(3) 0.046(2) Uani 1 1 d . . . H47 H -0.0973 0.2451 0.2180 0.055 Uiso 1 1 calc R . . C48 C -0.0842(3) 0.2871(4) 0.1622(3) 0.047(2) Uani 1 1 d . . . H48 H -0.0758 0.2518 0.1464 0.056 Uiso 1 1 calc R . . C49 C -0.0838(3) 0.3440(5) 0.1431(3) 0.049(3) Uani 1 1 d . . . H49 H -0.0746 0.3465 0.1141 0.059 Uiso 1 1 calc R . . C50 C -0.0963(3) 0.3965(4) 0.1647(2) 0.0274(18) Uani 1 1 d . . . C51 C -0.0348(3) 0.4708(5) 0.1247(2) 0.047(2) Uani 1 1 d . . . H51A H -0.0038 0.4682 0.1468 0.071 Uiso 1 1 calc R . . H51B H -0.0351 0.5117 0.1130 0.071 Uiso 1 1 calc R . . H51C H -0.0252 0.4418 0.1025 0.071 Uiso 1 1 calc R . . C52 C -0.0978(3) 0.4564(4) 0.14309(19) 0.032(2) Uani 1 1 d . . . H52 H -0.1087 0.4882 0.1640 0.038 Uiso 1 1 calc R . . C53 C -0.1454(3) 0.4566(4) 0.1083(2) 0.048(2) Uani 1 1 d . . . H53A H -0.1349 0.4258 0.0875 0.072 Uiso 1 1 calc R . . H53B H -0.1461 0.4963 0.0949 0.072 Uiso 1 1 calc R . . H53C H -0.1857 0.4478 0.1201 0.072 Uiso 1 1 calc R . . C54 C -0.0726(3) 0.2938(5) 0.2981(3) 0.067(3) Uani 1 1 d . . . H54A H -0.0718 0.2524 0.2874 0.100 Uiso 1 1 calc R . . H54B H -0.0815 0.2934 0.3281 0.100 Uiso 1 1 calc R . . H54C H -0.0327 0.3127 0.2933 0.100 Uiso 1 1 calc R . . C55 C -0.1228(3) 0.3301(5) 0.2749(2) 0.048(2) Uani 1 1 d . . . H55 H -0.1248 0.3718 0.2867 0.058 Uiso 1 1 calc R . . C56 C -0.1854(3) 0.2983(5) 0.2813(3) 0.073(4) Uani 1 1 d . . . H56A H -0.2142 0.3117 0.2597 0.110 Uiso 1 1 calc R . . H56B H -0.2016 0.3085 0.3091 0.110 Uiso 1 1 calc R . . H56C H -0.1799 0.2545 0.2793 0.110 Uiso 1 1 calc R . . C57 C 0.1471(3) 0.4555(5) 0.1340(2) 0.040(2) Uani 1 1 d . . . C58 C 0.1314(4) 0.3940(5) 0.1159(2) 0.057(3) Uani 1 1 d . . . H58A H 0.0869 0.3900 0.1136 0.086 Uiso 1 1 calc R . . H58B H 0.1474 0.3624 0.1343 0.086 Uiso 1 1 calc R . . H58C H 0.1499 0.3900 0.0881 0.086 Uiso 1 1 calc R . . C59 C 0.2172(3) 0.4598(5) 0.1390(2) 0.052(3) Uani 1 1 d . . . H59A H 0.2368 0.4517 0.1119 0.078 Uiso 1 1 calc R . . H59B H 0.2310 0.4300 0.1596 0.078 Uiso 1 1 calc R . . H59C H 0.2283 0.5003 0.1485 0.078 Uiso 1 1 calc R . . C60 C 0.1297(3) 0.5042(5) 0.1018(2) 0.049(3) Uani 1 1 d . . . H60A H 0.1508 0.4962 0.0753 0.073 Uiso 1 1 calc R . . H60B H 0.1417 0.5439 0.1124 0.073 Uiso 1 1 calc R . . H60C H 0.0854 0.5034 0.0972 0.073 Uiso 1 1 calc R . . C61 C 0.0866(3) 0.5571(4) 0.2139(2) 0.0308(19) Uani 1 1 d . . . C62 C 0.0410(3) 0.5932(4) 0.1883(3) 0.052(2) Uani 1 1 d . . . H62A H 0.0388 0.6344 0.1993 0.078 Uiso 1 1 calc R . . H62B H 0.0006 0.5743 0.1902 0.078 Uiso 1 1 calc R . . H62C H 0.0542 0.5943 0.1590 0.078 Uiso 1 1 calc R . . C63 C 0.1507(3) 0.5852(4) 0.2067(3) 0.051(2) Uani 1 1 d . . . H63A H 0.1629 0.5794 0.1774 0.077 Uiso 1 1 calc R . . H63B H 0.1805 0.5656 0.2251 0.077 Uiso 1 1 calc R . . H63C H 0.1492 0.6284 0.2130 0.077 Uiso 1 1 calc R . . C64 C 0.0743(3) 0.5675(5) 0.2606(2) 0.058(3) Uani 1 1 d . . . H64A H 0.0749 0.6109 0.2666 0.086 Uiso 1 1 calc R . . H64B H 0.1060 0.5474 0.2772 0.086 Uiso 1 1 calc R . . H64C H 0.0342 0.5510 0.2680 0.086 Uiso 1 1 calc R . . C65 C 0.0915(3) 0.3969(4) 0.2320(2) 0.0299(19) Uani 1 1 d . . . C66 C 0.0699(3) 0.4063(5) 0.2773(2) 0.047(2) Uani 1 1 d . . . H66A H 0.0254 0.4121 0.2776 0.070 Uiso 1 1 calc R . . H66B H 0.0899 0.4419 0.2891 0.070 Uiso 1 1 calc R . . H66C H 0.0804 0.3708 0.2941 0.070 Uiso 1 1 calc R . . C67 C 0.1588(3) 0.3777(5) 0.2353(3) 0.067(3) Uani 1 1 d . . . H67A H 0.1619 0.3410 0.2522 0.100 Uiso 1 1 calc R . . H67B H 0.1825 0.4100 0.2485 0.100 Uiso 1 1 calc R . . H67C H 0.1750 0.3699 0.2072 0.100 Uiso 1 1 calc R . . C68 C 0.0550(3) 0.3462(4) 0.2136(3) 0.049(2) Uani 1 1 d . . . H68A H 0.0681 0.3392 0.1847 0.074 Uiso 1 1 calc R . . H68B H 0.0115 0.3567 0.2140 0.074 Uiso 1 1 calc R . . H68C H 0.0617 0.3095 0.2301 0.074 Uiso 1 1 calc R . . C70 C 0.1789(3) 0.3640(4) 0.9598(2) 0.035(2) Uani 1 1 d . . . C71 C 0.1361(3) 0.3618(4) 0.9217(3) 0.052(3) Uani 1 1 d . . . H71A H 0.1327 0.3202 0.9117 0.078 Uiso 1 1 calc R . . H71B H 0.1527 0.3872 0.8993 0.078 Uiso 1 1 calc R . . H71C H 0.0955 0.3766 0.9298 0.078 Uiso 1 1 calc R . . C72 C 0.1726(3) 0.4267(4) 0.9806(2) 0.046(2) Uani 1 1 d . . . H72A H 0.1297 0.4337 0.9880 0.069 Uiso 1 1 calc R . . H72B H 0.1862 0.4579 0.9610 0.069 Uiso 1 1 calc R . . H72C H 0.1978 0.4281 1.0059 0.069 Uiso 1 1 calc R . . C73 C 0.1547(3) 0.3174(4) 0.9906(3) 0.053(3) Uani 1 1 d . . . H73A H 0.1130 0.3282 0.9990 0.079 Uiso 1 1 calc R . . H73B H 0.1811 0.3165 1.0154 0.079 Uiso 1 1 calc R . . H73C H 0.1545 0.2776 0.9773 0.079 Uiso 1 1 calc R . . C74 C 0.3311(3) 0.3503(4) 0.9932(2) 0.033(2) Uani 1 1 d . . . C75 C 0.3789(3) 0.3014(4) 0.9827(2) 0.044(2) Uani 1 1 d . . . H75A H 0.3971 0.3099 0.9553 0.066 Uiso 1 1 calc R . . H75B H 0.3589 0.2619 0.9821 0.066 Uiso 1 1 calc R . . H75C H 0.4109 0.3014 1.0042 0.066 Uiso 1 1 calc R . . C76 C 0.3647(4) 0.4104(5) 0.9973(3) 0.066(3) Uani 1 1 d . . . H76A H 0.3951 0.4076 1.0198 0.098 Uiso 1 1 calc R . . H76B H 0.3353 0.4423 1.0039 0.098 Uiso 1 1 calc R . . H76C H 0.3854 0.4198 0.9709 0.098 Uiso 1 1 calc R . . C77 C 0.3067(3) 0.3363(4) 1.0373(2) 0.043(2) Uani 1 1 d . . . H77A H 0.3410 0.3342 1.0570 0.065 Uiso 1 1 calc R . . H77B H 0.2852 0.2975 1.0369 0.065 Uiso 1 1 calc R . . H77C H 0.2784 0.3681 1.0460 0.065 Uiso 1 1 calc R . . C78 C 0.3054(3) 0.4090(4) 0.8900(2) 0.038(2) Uani 1 1 d . . . C79 C 0.2613(4) 0.4038(4) 0.8524(2) 0.050(2) Uani 1 1 d . . . H79A H 0.2235 0.4259 0.8585 0.075 Uiso 1 1 calc R . . H79B H 0.2517 0.3613 0.8474 0.075 Uiso 1 1 calc R . . H79C H 0.2807 0.4210 0.8274 0.075 Uiso 1 1 calc R . . C80 C 0.3195(3) 0.4754(4) 0.8952(2) 0.041(2) Uani 1 1 d . . . H80A H 0.3372 0.4911 0.8692 0.061 Uiso 1 1 calc R . . H80B H 0.3487 0.4808 0.9181 0.061 Uiso 1 1 calc R . . H80C H 0.2817 0.4973 0.9015 0.061 Uiso 1 1 calc R . . C81 C 0.3649(3) 0.3772(4) 0.8775(3) 0.054(3) Uani 1 1 d . . . H81A H 0.3830 0.3978 0.8534 0.082 Uiso 1 1 calc R . . H81B H 0.3561 0.3353 0.8702 0.082 Uiso 1 1 calc R . . H81C H 0.3935 0.3783 0.9011 0.082 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Li1 0.031(5) 0.027(9) 0.017(5) 0.013(6) 0.001(4) 0.010(6) Li2 0.028(6) 0.027(9) 0.053(7) -0.026(7) 0.001(5) -0.007(6) Zn1 0.0191(4) 0.0368(7) 0.0318(5) -0.0022(5) 0.0047(3) -0.0029(4) Zn2 0.0234(4) 0.0331(7) 0.0363(5) -0.0001(5) 0.0062(3) -0.0018(4) N1 0.017(2) 0.032(4) 0.023(3) -0.007(3) -0.002(2) 0.002(3) N2 0.014(2) 0.022(4) 0.029(3) 0.003(3) -0.003(2) 0.000(2) N3 0.014(2) 0.019(4) 0.033(3) 0.003(3) -0.001(2) -0.003(3) N4 0.018(2) 0.030(4) 0.019(3) 0.004(3) 0.002(2) -0.003(3) C1 0.015(3) 0.029(4) 0.024(3) -0.009(3) 0.005(3) 0.004(3) C2 0.030(3) 0.022(4) 0.041(4) -0.007(4) -0.010(3) 0.004(3) C3 0.027(3) 0.016(4) 0.035(4) 0.009(4) -0.007(3) 0.005(3) C4 0.019(2) 0.024(4) 0.033(3) -0.001(3) -0.006(2) 0.001(3) C5 0.027(2) 0.012(3) 0.025(3) -0.008(3) -0.002(2) 0.000(3) C6 0.030(3) 0.026(4) 0.028(3) -0.002(3) -0.006(2) 0.001(3) C7 0.027(3) 0.034(4) 0.033(3) -0.003(3) -0.008(2) 0.001(3) C8 0.019(2) 0.043(4) 0.044(3) 0.004(3) 0.000(2) 0.003(3) C9 0.023(2) 0.031(4) 0.025(3) 0.000(3) -0.002(2) 0.000(3) C10 0.040(4) 0.071(8) 0.042(5) -0.008(5) 0.003(4) 0.004(5) C11 0.024(3) 0.023(5) 0.029(4) 0.007(4) 0.001(3) 0.004(3) C12 0.048(5) 0.081(9) 0.088(7) 0.005(7) 0.046(5) -0.007(6) C13 0.050(5) 0.049(7) 0.066(5) 0.016(6) 0.010(4) 0.005(5) C14 0.026(3) 0.044(6) 0.035(4) 0.004(4) 0.003(3) 0.004(4) C15 0.060(5) 0.044(7) 0.035(4) 0.008(5) 0.019(4) 0.003(5) C16 0.018(3) 0.030(5) 0.028(4) 0.003(4) -0.001(3) 0.013(3) C17 0.018(3) 0.025(5) 0.035(4) 0.000(4) -0.001(3) 0.009(3) C18 0.030(4) 0.045(6) 0.030(4) -0.012(4) -0.012(3) 0.013(4) C19 0.025(3) 0.037(6) 0.043(4) -0.001(4) -0.010(3) 0.003(4) C20 0.014(3) 0.054(7) 0.040(4) -0.012(4) -0.002(3) 0.003(4) C21 0.019(3) 0.034(6) 0.032(4) -0.004(4) -0.007(3) 0.008(3) C22 0.028(4) 0.064(8) 0.062(5) -0.015(6) 0.013(4) 0.004(4) C23 0.016(3) 0.044(6) 0.032(4) -0.005(4) -0.001(3) 0.002(4) C24 0.023(3) 0.074(8) 0.061(5) -0.023(6) 0.012(4) -0.003(4) C25 0.026(3) 0.062(7) 0.041(4) -0.010(5) 0.007(3) -0.003(4) C26 0.018(3) 0.050(6) 0.031(4) -0.016(4) -0.006(3) 0.004(4) C27 0.046(4) 0.041(6) 0.049(5) -0.007(5) 0.004(4) 0.006(4) C28 0.017(3) 0.012(4) 0.022(3) -0.001(3) -0.006(3) 0.003(3) C29 0.015(3) 0.050(7) 0.034(4) 0.007(5) -0.001(3) -0.007(4) C31 0.015(3) 0.048(6) 0.038(4) 0.006(5) 0.005(3) -0.003(4) C32 0.018(3) 0.023(5) 0.042(4) -0.003(4) 0.006(3) 0.000(3) C33 0.008(3) 0.048(6) 0.028(4) 0.003(4) 0.003(3) 0.002(3) C34 0.018(3) 0.051(7) 0.048(5) -0.009(5) -0.002(3) -0.007(4) C35 0.034(4) 0.039(7) 0.043(5) -0.014(5) 0.003(4) -0.017(4) C36 0.040(4) 0.043(6) 0.045(5) -0.001(5) 0.006(4) -0.007(4) C37 0.027(3) 0.042(6) 0.023(4) -0.003(4) 0.004(3) -0.008(4) C38 0.040(4) 0.043(6) 0.051(5) 0.007(5) 0.005(4) -0.008(4) C39 0.027(3) 0.047(6) 0.020(3) -0.011(4) -0.003(3) 0.014(4) C40 0.042(4) 0.058(8) 0.043(4) -0.010(5) -0.004(4) 0.005(5) C41 0.038(4) 0.077(8) 0.048(5) -0.011(5) 0.000(4) 0.005(5) C42 0.043(4) 0.040(6) 0.034(4) -0.002(4) 0.002(3) 0.009(4) C43 0.047(4) 0.062(8) 0.048(5) 0.013(5) 0.007(4) 0.011(5) C45 0.018(3) 0.035(6) 0.036(4) 0.016(4) -0.005(3) -0.005(3) C46 0.026(3) 0.017(5) 0.049(5) -0.005(5) -0.004(3) -0.009(3) C47 0.032(4) 0.022(6) 0.082(6) -0.001(6) -0.018(4) 0.002(4) C48 0.037(4) 0.025(6) 0.077(6) -0.029(6) -0.018(4) 0.013(4) C49 0.029(4) 0.063(8) 0.056(5) -0.019(6) -0.011(4) 0.007(5) C50 0.024(3) 0.020(5) 0.038(4) -0.007(4) -0.003(3) -0.002(3) C51 0.041(4) 0.055(7) 0.046(4) 0.013(5) -0.004(4) -0.013(5) C52 0.031(3) 0.048(6) 0.017(3) -0.002(4) -0.001(3) 0.000(4) C53 0.044(4) 0.046(7) 0.054(5) 0.013(5) -0.013(4) -0.001(4) C54 0.041(4) 0.091(9) 0.068(6) 0.047(6) -0.009(4) -0.006(5) C55 0.043(4) 0.046(7) 0.057(5) 0.029(5) -0.006(4) -0.010(5) C56 0.032(4) 0.097(10) 0.091(7) 0.044(7) 0.006(4) 0.010(5) C57 0.020(3) 0.059(7) 0.041(4) 0.008(5) 0.007(3) -0.002(4) C58 0.051(5) 0.074(9) 0.047(5) -0.009(6) 0.014(4) 0.001(5) C59 0.031(4) 0.078(8) 0.047(5) -0.002(5) 0.021(4) 0.001(5) C60 0.034(4) 0.068(8) 0.045(4) 0.016(5) 0.015(3) -0.004(4) C61 0.032(3) 0.024(5) 0.037(4) -0.002(4) 0.019(3) -0.004(4) C62 0.043(4) 0.035(6) 0.079(6) -0.005(6) 0.002(4) -0.013(4) C63 0.040(4) 0.036(6) 0.078(6) -0.024(6) 0.020(4) -0.010(4) C64 0.049(4) 0.057(8) 0.066(6) -0.034(6) 0.027(4) -0.022(5) C65 0.025(3) 0.038(6) 0.028(4) 0.021(4) 0.002(3) -0.003(4) C66 0.037(4) 0.056(7) 0.047(5) 0.008(5) 0.003(4) 0.006(4) C67 0.025(4) 0.109(10) 0.067(6) 0.037(6) 0.003(4) 0.020(5) C68 0.054(5) 0.026(6) 0.067(6) 0.002(5) -0.007(4) 0.004(4) C70 0.025(3) 0.049(7) 0.031(4) 0.007(4) 0.008(3) -0.003(4) C71 0.025(4) 0.048(7) 0.082(6) -0.022(6) 0.006(4) 0.002(4) C72 0.053(4) 0.044(7) 0.041(4) -0.005(5) 0.006(4) 0.018(5) C73 0.022(3) 0.046(7) 0.090(6) 0.012(6) 0.012(4) 0.005(4) C74 0.029(3) 0.037(6) 0.033(4) -0.002(4) 0.000(3) -0.002(4) C75 0.035(4) 0.032(6) 0.065(5) 0.014(5) -0.012(4) -0.001(4) C76 0.062(5) 0.080(9) 0.055(5) 0.011(6) -0.020(4) -0.033(6) C77 0.058(5) 0.022(5) 0.048(5) -0.006(5) -0.020(4) -0.005(4) C78 0.029(3) 0.057(7) 0.029(4) -0.016(4) 0.005(3) -0.003(4) C79 0.071(5) 0.022(6) 0.056(5) 0.020(5) 0.012(4) -0.017(5) C80 0.038(4) 0.044(7) 0.040(4) -0.015(5) 0.012(3) -0.001(4) C81 0.056(5) 0.038(7) 0.069(6) -0.024(5) 0.037(4) -0.017(5) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Li1 C28 2.205(11) . ? Li1 C61 2.347(14) . ? Li1 Zn1 2.447(10) . ? Li1 C65 2.467(14) . ? Li2 C1 2.209(16) . ? Li2 C74 2.360(14) . ? Li2 Zn2 2.517(14) . ? Li2 C70 2.611(16) . ? Zn1 C57 2.036(7) . ? Zn1 C61 2.119(8) . ? Zn1 C65 2.122(7) . ? Zn2 C78 2.028(7) . ? Zn2 C70 2.089(6) . ? Zn2 C74 2.131(7) . ? N1 C1 1.360(8) . ? N1 C3 1.387(10) . ? N1 C16 1.455(8) . ? N2 C1 1.362(8) . ? N2 C2 1.380(10) . ? N2 C4 1.473(7) . ? N3 C28 1.366(8) . ? N3 C31 1.403(7) . ? N3 C32 1.429(9) . ? N4 C28 1.369(8) . ? N4 C29 1.391(8) . ? N4 C45 1.421(10) . ? C2 C3 1.337(8) . ? C2 H2 0.9500 . ? C3 H3 0.9500 . ? C4 C5 1.383(9) . ? C4 C9 1.399(8) . ? C5 C6 1.384(8) . ? C5 C11 1.504(8) . ? C6 C7 1.378(8) . ? C6 H6 0.9500 . ? C7 C8 1.381(9) . ? C7 H7 0.9500 . ? C8 C9 1.387(8) . ? C8 H8 0.9500 . ? C9 C14 1.531(9) . ? C10 C11 1.552(10) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.491(12) . ? C11 H11 1.0000 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.548(11) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 C15 1.508(10) . ? C14 H14 1.0000 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.387(9) . ? C16 C21 1.407(8) . ? C17 C18 1.389(9) . ? C17 C23 1.540(8) . ? C18 C19 1.389(9) . ? C18 H18 0.9500 . ? C19 C20 1.357(9) . ? C19 H19 0.9500 . ? C20 C21 1.388(9) . ? C20 H20 0.9500 . ? C21 C26 1.520(9) . ? C22 C23 1.517(11) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 C24 1.515(12) . ? C23 H23 1.0000 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C26 1.514(10) . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 C27 1.541(11) . ? C26 H26 1.0000 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C29 C31 1.311(11) . ? C29 H29 0.9500 . ? C31 H31 0.9500 . ? C32 C37 1.390(11) . ? C32 C33 1.407(9) . ? C33 C34 1.371(11) . ? C33 C39 1.510(11) . ? C34 C35 1.388(12) . ? C34 H34 0.9500 . ? C35 C36 1.394(10) . ? C35 H35 0.9500 . ? C36 C37 1.363(11) . ? C36 H36 0.9500 . ? C37 C42 1.540(9) . ? C38 C39 1.523(9) . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 C40 1.537(9) . ? C39 H39 1.0000 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 C42 1.554(10) . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 C43 1.518(11) . ? C42 H42 1.0000 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C45 C50 1.388(9) . ? C45 C46 1.417(11) . ? C46 C47 1.365(11) . ? C46 C55 1.530(10) . ? C47 C48 1.389(11) . ? C47 H47 0.9500 . ? C48 C49 1.402(13) . ? C48 H48 0.9500 . ? C49 C50 1.380(12) . ? C49 H49 0.9500 . ? C50 C52 1.499(11) . ? C51 C52 1.531(9) . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C52 C53 1.522(9) . ? C52 H52 1.0000 . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C54 C55 1.549(11) . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C55 C56 1.555(10) . ? C55 H55 1.0000 . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? C57 C58 1.522(13) . ? C57 C60 1.539(11) . ? C57 C59 1.544(9) . ? C58 H58A 0.9800 . ? C58 H58B 0.9800 . ? C58 H58C 0.9800 . ? C59 H59A 0.9800 . ? C59 H59B 0.9800 . ? C59 H59C 0.9800 . ? C60 H60A 0.9800 . ? C60 H60B 0.9800 . ? C60 H60C 0.9800 . ? C61 C62 1.516(10) . ? C61 C64 1.535(9) . ? C61 C63 1.551(9) . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C62 H62C 0.9800 . ? C63 H63A 0.9800 . ? C63 H63B 0.9800 . ? C63 H63C 0.9800 . ? C64 H64A 0.9800 . ? C64 H64B 0.9800 . ? C64 H64C 0.9800 . ? C65 C68 1.499(11) . ? C65 C67 1.535(8) . ? C65 C66 1.535(9) . ? C66 H66A 0.9800 . ? C66 H66B 0.9800 . ? C66 H66C 0.9800 . ? C67 H67A 0.9800 . ? C67 H67B 0.9800 . ? C67 H67C 0.9800 . ? C68 H68A 0.9800 . ? C68 H68B 0.9800 . ? C68 H68C 0.9800 . ? C70 C73 1.522(11) . ? C70 C71 1.536(10) . ? C70 C72 1.546(12) . ? C71 H71A 0.9800 . ? C71 H71B 0.9800 . ? C71 H71C 0.9800 . ? C72 H72A 0.9800 . ? C72 H72B 0.9800 . ? C72 H72C 0.9800 . ? C73 H73A 0.9800 . ? C73 H73B 0.9800 . ? C73 H73C 0.9800 . ? C74 C76 1.528(12) . ? C74 C77 1.537(10) . ? C74 C75 1.543(10) . ? C75 H75A 0.9800 . ? C75 H75B 0.9800 . ? C75 H75C 0.9800 . ? C76 H76A 0.9800 . ? C76 H76B 0.9800 . ? C76 H76C 0.9800 . ? C77 H77A 0.9800 . ? C77 H77B 0.9800 . ? C77 H77C 0.9800 . ? C78 C80 1.515(12) . ? C78 C81 1.531(10) . ? C78 C79 1.543(10) . ? C79 H79A 0.9800 . ? C79 H79B 0.9800 . ? C79 H79C 0.9800 . ? C80 H80A 0.9800 . ? C80 H80B 0.9800 . ? C80 H80C 0.9800 . ? C81 H81A 0.9800 . ? C81 H81B 0.9800 . ? C81 H81C 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 C28 Li1 C61 131.7(6) . . ? C28 Li1 Zn1 146.8(5) . . ? C61 Li1 Zn1 52.4(3) . . ? C28 Li1 C65 129.2(6) . . ? C61 Li1 C65 96.9(4) . . ? Zn1 Li1 C65 51.2(3) . . ? C1 Li2 C74 131.6(6) . . ? C1 Li2 Zn2 147.2(6) . . ? C74 Li2 Zn2 51.7(3) . . ? C1 Li2 C70 137.7(5) . . ? C74 Li2 C70 89.6(5) . . ? Zn2 Li2 C70 48.0(3) . . ? C57 Zn1 C61 123.0(3) . . ? C57 Zn1 C65 120.0(3) . . ? C61 Zn1 C65 116.4(3) . . ? C57 Zn1 Li1 156.8(3) . . ? C61 Zn1 Li1 61.4(4) . . ? C65 Zn1 Li1 64.9(3) . . ? C78 Zn2 C70 127.3(3) . . ? C78 Zn2 C74 119.2(3) . . ? C70 Zn2 C74 112.4(3) . . ? C78 Zn2 Li2 149.6(4) . . ? C70 Zn2 Li2 68.3(3) . . ? C74 Zn2 Li2 60.3(3) . . ? C1 N1 C3 111.8(5) . . ? C1 N1 C16 125.2(6) . . ? C3 N1 C16 122.5(6) . . ? C1 N2 C2 113.4(5) . . ? C1 N2 C4 122.7(6) . . ? C2 N2 C4 123.6(6) . . ? C28 N3 C31 110.7(6) . . ? C28 N3 C32 124.8(5) . . ? C31 N3 C32 124.4(6) . . ? C28 N4 C29 110.6(6) . . ? C28 N4 C45 125.5(5) . . ? C29 N4 C45 123.8(6) . . ? N1 C1 N2 102.1(6) . . ? N1 C1 Li2 129.0(6) . . ? N2 C1 Li2 128.9(6) . . ? C3 C2 N2 105.3(7) . . ? C3 C2 H2 127.4 . . ? N2 C2 H2 127.4 . . ? C2 C3 N1 107.5(7) . . ? C2 C3 H3 126.3 . . ? N1 C3 H3 126.3 . . ? C5 C4 C9 124.0(6) . . ? C5 C4 N2 119.6(5) . . ? C9 C4 N2 116.4(6) . . ? C4 C5 C6 116.7(6) . . ? C4 C5 C11 122.0(6) . . ? C6 C5 C11 121.2(6) . . ? C7 C6 C5 121.7(6) . . ? C7 C6 H6 119.2 . . ? C5 C6 H6 119.2 . . ? C6 C7 C8 119.7(6) . . ? C6 C7 H7 120.1 . . ? C8 C7 H7 120.1 . . ? C7 C8 C9 121.5(6) . . ? C7 C8 H8 119.3 . . ? C9 C8 H8 119.3 . . ? C8 C9 C4 116.3(6) . . ? C8 C9 C14 120.2(5) . . ? C4 C9 C14 123.5(6) . . ? C11 C10 H10A 109.5 . . ? C11 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C11 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C12 C11 C5 111.9(6) . . ? C12 C11 C10 110.3(6) . . ? C5 C11 C10 110.9(6) . . ? C12 C11 H11 107.9 . . ? C5 C11 H11 107.9 . . ? C10 C11 H11 107.9 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C14 C13 H13A 109.5 . . ? C14 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C14 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C15 C14 C9 111.7(7) . . ? C15 C14 C13 111.8(6) . . ? C9 C14 C13 109.9(6) . . ? C15 C14 H14 107.8 . . ? C9 C14 H14 107.8 . . ? C13 C14 H14 107.8 . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C17 C16 C21 123.4(6) . . ? C17 C16 N1 118.3(5) . . ? C21 C16 N1 118.3(5) . . ? C16 C17 C18 117.5(5) . . ? C16 C17 C23 122.7(6) . . ? C18 C17 C23 119.7(6) . . ? C19 C18 C17 119.9(6) . . ? C19 C18 H18 120.0 . . ? C17 C18 H18 120.0 . . ? C20 C19 C18 121.4(6) . . ? C20 C19 H19 119.3 . . ? C18 C19 H19 119.3 . . ? C19 C20 C21 121.4(6) . . ? C19 C20 H20 119.3 . . ? C21 C20 H20 119.3 . . ? C20 C21 C16 116.4(6) . . ? C20 C21 C26 119.8(5) . . ? C16 C21 C26 123.8(6) . . ? C23 C22 H22A 109.5 . . ? C23 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C23 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C24 C23 C22 112.3(6) . . ? C24 C23 C17 110.1(6) . . ? C22 C23 C17 113.8(6) . . ? C24 C23 H23 106.7 . . ? C22 C23 H23 106.7 . . ? C17 C23 H23 106.7 . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C26 C25 H25A 109.5 . . ? C26 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C26 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C25 C26 C21 113.3(7) . . ? C25 C26 C27 109.6(6) . . ? C21 C26 C27 109.7(6) . . ? C25 C26 H26 108.0 . . ? C21 C26 H26 108.0 . . ? C27 C26 H26 108.0 . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? N3 C28 N4 103.7(5) . . ? N3 C28 Li1 127.7(6) . . ? N4 C28 Li1 128.6(6) . . ? C31 C29 N4 107.9(6) . . ? C31 C29 H29 126.0 . . ? N4 C29 H29 126.0 . . ? C29 C31 N3 107.1(6) . . ? C29 C31 H31 126.5 . . ? N3 C31 H31 126.5 . . ? C37 C32 C33 122.7(7) . . ? C37 C32 N3 117.7(6) . . ? C33 C32 N3 119.6(7) . . ? C34 C33 C32 116.7(8) . . ? C34 C33 C39 122.4(6) . . ? C32 C33 C39 120.9(7) . . ? C33 C34 C35 122.6(7) . . ? C33 C34 H34 118.7 . . ? C35 C34 H34 118.7 . . ? C34 C35 C36 117.9(8) . . ? C34 C35 H35 121.0 . . ? C36 C35 H35 121.0 . . ? C37 C36 C35 122.4(9) . . ? C37 C36 H36 118.8 . . ? C35 C36 H36 118.8 . . ? C36 C37 C32 117.5(7) . . ? C36 C37 C42 119.5(8) . . ? C32 C37 C42 123.0(7) . . ? C39 C38 H38A 109.5 . . ? C39 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C39 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C33 C39 C38 110.3(6) . . ? C33 C39 C40 113.2(7) . . ? C38 C39 C40 111.0(6) . . ? C33 C39 H39 107.3 . . ? C38 C39 H39 107.3 . . ? C40 C39 H39 107.3 . . ? C39 C40 H40A 109.5 . . ? C39 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C39 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C42 C41 H41A 109.5 . . ? C42 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C42 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C43 C42 C37 112.9(6) . . ? C43 C42 C41 110.0(7) . . ? C37 C42 C41 109.0(6) . . ? C43 C42 H42 108.3 . . ? C37 C42 H42 108.3 . . ? C41 C42 H42 108.3 . . ? C42 C43 H43A 109.5 . . ? C42 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C42 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C50 C45 C46 123.3(8) . . ? C50 C45 N4 119.3(7) . . ? C46 C45 N4 117.3(6) . . ? C47 C46 C45 117.8(8) . . ? C47 C46 C55 121.7(8) . . ? C45 C46 C55 120.5(8) . . ? C46 C47 C48 121.4(9) . . ? C46 C47 H47 119.3 . . ? C48 C47 H47 119.3 . . ? C47 C48 C49 118.6(9) . . ? C47 C48 H48 120.7 . . ? C49 C48 H48 120.7 . . ? C50 C49 C48 122.7(8) . . ? C50 C49 H49 118.6 . . ? C48 C49 H49 118.6 . . ? C49 C50 C45 116.1(8) . . ? C49 C50 C52 121.5(7) . . ? C45 C50 C52 122.4(7) . . ? C52 C51 H51A 109.5 . . ? C52 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C52 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C50 C52 C53 110.7(7) . . ? C50 C52 C51 110.1(6) . . ? C53 C52 C51 109.5(6) . . ? C50 C52 H52 108.8 . . ? C53 C52 H52 108.8 . . ? C51 C52 H52 108.8 . . ? C52 C53 H53A 109.5 . . ? C52 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C52 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C55 C54 H54A 109.5 . . ? C55 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C55 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C46 C55 C54 111.0(7) . . ? C46 C55 C56 108.9(7) . . ? C54 C55 C56 108.9(7) . . ? C46 C55 H55 109.3 . . ? C54 C55 H55 109.3 . . ? C56 C55 H55 109.3 . . ? C55 C56 H56A 109.5 . . ? C55 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C55 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? C58 C57 C60 108.6(7) . . ? C58 C57 C59 108.5(7) . . ? C60 C57 C59 105.7(6) . . ? C58 C57 Zn1 112.0(5) . . ? C60 C57 Zn1 111.7(5) . . ? C59 C57 Zn1 110.1(5) . . ? C57 C58 H58A 109.5 . . ? C57 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? C57 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? C57 C59 H59A 109.5 . . ? C57 C59 H59B 109.5 . . ? H59A C59 H59B 109.5 . . ? C57 C59 H59C 109.5 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? C57 C60 H60A 109.5 . . ? C57 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? C57 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? C62 C61 C64 109.2(7) . . ? C62 C61 C63 107.5(6) . . ? C64 C61 C63 104.0(6) . . ? C62 C61 Zn1 114.7(5) . . ? C64 C61 Zn1 121.3(6) . . ? C63 C61 Zn1 98.0(5) . . ? C62 C61 Li1 98.6(5) . . ? C64 C61 Li1 70.5(5) . . ? C63 C61 Li1 153.5(6) . . ? Zn1 C61 Li1 66.2(4) . . ? C61 C62 H62A 109.5 . . ? C61 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C61 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? C61 C63 H63A 109.5 . . ? C61 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? C61 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? C61 C64 H64A 109.5 . . ? C61 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? C61 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? C68 C65 C67 109.2(7) . . ? C68 C65 C66 107.9(6) . . ? C67 C65 C66 105.6(5) . . ? C68 C65 Zn1 113.7(5) . . ? C67 C65 Zn1 96.7(5) . . ? C66 C65 Zn1 122.3(6) . . ? C68 C65 Li1 106.0(5) . . ? C67 C65 Li1 144.5(7) . . ? C66 C65 Li1 67.5(5) . . ? Zn1 C65 Li1 63.9(3) . . ? C65 C66 H66A 109.5 . . ? C65 C66 H66B 109.5 . . ? H66A C66 H66B 109.5 . . ? C65 C66 H66C 109.5 . . ? H66A C66 H66C 109.5 . . ? H66B C66 H66C 109.5 . . ? C65 C67 H67A 109.5 . . ? C65 C67 H67B 109.5 . . ? H67A C67 H67B 109.5 . . ? C65 C67 H67C 109.5 . . ? H67A C67 H67C 109.5 . . ? H67B C67 H67C 109.5 . . ? C65 C68 H68A 109.5 . . ? C65 C68 H68B 109.5 . . ? H68A C68 H68B 109.5 . . ? C65 C68 H68C 109.5 . . ? H68A C68 H68C 109.5 . . ? H68B C68 H68C 109.5 . . ? C73 C70 C71 106.1(6) . . ? C73 C70 C72 107.6(6) . . ? C71 C70 C72 108.3(7) . . ? C73 C70 Zn2 123.7(5) . . ? C71 C70 Zn2 112.5(4) . . ? C72 C70 Zn2 97.5(5) . . ? C73 C70 Li2 60.5(4) . . ? C71 C70 Li2 127.5(6) . . ? C72 C70 Li2 124.2(5) . . ? Zn2 C70 Li2 63.7(3) . . ? C70 C71 H71A 109.5 . . ? C70 C71 H71B 109.5 . . ? H71A C71 H71B 109.5 . . ? C70 C71 H71C 109.5 . . ? H71A C71 H71C 109.5 . . ? H71B C71 H71C 109.5 . . ? C70 C72 H72A 109.5 . . ? C70 C72 H72B 109.5 . . ? H72A C72 H72B 109.5 . . ? C70 C72 H72C 109.5 . . ? H72A C72 H72C 109.5 . . ? H72B C72 H72C 109.5 . . ? C70 C73 H73A 109.5 . . ? C70 C73 H73B 109.5 . . ? H73A C73 H73B 109.5 . . ? C70 C73 H73C 109.5 . . ? H73A C73 H73C 109.5 . . ? H73B C73 H73C 109.5 . . ? C76 C74 C77 105.4(6) . . ? C76 C74 C75 107.8(6) . . ? C77 C74 C75 106.9(7) . . ? C76 C74 Zn2 99.9(5) . . ? C77 C74 Zn2 121.5(4) . . ? C75 C74 Zn2 114.1(5) . . ? C76 C74 Li2 161.2(7) . . ? C77 C74 Li2 71.8(5) . . ? C75 C74 Li2 90.5(6) . . ? Zn2 C74 Li2 68.0(4) . . ? C74 C75 H75A 109.5 . . ? C74 C75 H75B 109.5 . . ? H75A C75 H75B 109.5 . . ? C74 C75 H75C 109.5 . . ? H75A C75 H75C 109.5 . . ? H75B C75 H75C 109.5 . . ? C74 C76 H76A 109.5 . . ? C74 C76 H76B 109.5 . . ? H76A C76 H76B 109.5 . . ? C74 C76 H76C 109.5 . . ? H76A C76 H76C 109.5 . . ? H76B C76 H76C 109.5 . . ? C74 C77 H77A 109.5 . . ? C74 C77 H77B 109.5 . . ? H77A C77 H77B 109.5 . . ? C74 C77 H77C 109.5 . . ? H77A C77 H77C 109.5 . . ? H77B C77 H77C 109.5 . . ? C80 C78 C81 107.6(6) . . ? C80 C78 C79 106.5(7) . . ? C81 C78 C79 107.1(6) . . ? C80 C78 Zn2 112.8(5) . . ? C81 C78 Zn2 109.9(6) . . ? C79 C78 Zn2 112.6(5) . . ? C78 C79 H79A 109.5 . . ? C78 C79 H79B 109.5 . . ? H79A C79 H79B 109.5 . . ? C78 C79 H79C 109.5 . . ? H79A C79 H79C 109.5 . . ? H79B C79 H79C 109.5 . . ? C78 C80 H80A 109.5 . . ? C78 C80 H80B 109.5 . . ? H80A C80 H80B 109.5 . . ? C78 C80 H80C 109.5 . . ? H80A C80 H80C 109.5 . . ? H80B C80 H80C 109.5 . . ? C78 C81 H81A 109.5 . . ? C78 C81 H81B 109.5 . . ? H81A C81 H81B 109.5 . . ? C78 C81 H81C 109.5 . . ? H81A C81 H81C 109.5 . . ? H81B C81 H81C 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 C28 Li1 Zn1 C57 3.4(19) . . . . ? C61 Li1 Zn1 C57 -107.5(10) . . . . ? C65 Li1 Zn1 C57 108.0(10) . . . . ? C28 Li1 Zn1 C61 110.8(12) . . . . ? C65 Li1 Zn1 C61 -144.6(4) . . . . ? C28 Li1 Zn1 C65 -104.6(12) . . . . ? C61 Li1 Zn1 C65 144.6(4) . . . . ? C1 Li2 Zn2 C78 -11.5(14) . . . . ? C74 Li2 Zn2 C78 98.1(6) . . . . ? C70 Li2 Zn2 C78 -127.7(6) . . . . ? C1 Li2 Zn2 C70 116.1(10) . . . . ? C74 Li2 Zn2 C70 -134.3(4) . . . . ? C1 Li2 Zn2 C74 -109.6(10) . . . . ? C70 Li2 Zn2 C74 134.3(4) . . . . ? C3 N1 C1 N2 -0.1(6) . . . . ? C16 N1 C1 N2 -171.3(5) . . . . ? C3 N1 C1 Li2 -179.1(6) . . . . ? C16 N1 C1 Li2 9.7(9) . . . . ? C2 N2 C1 N1 -0.5(7) . . . . ? C4 N2 C1 N1 173.3(5) . . . . ? C2 N2 C1 Li2 178.5(6) . . . . ? C4 N2 C1 Li2 -7.8(9) . . . . ? C74 Li2 C1 N1 30.2(11) . . . . ? Zn2 Li2 C1 N1 111.4(10) . . . . ? C70 Li2 C1 N1 -166.0(6) . . . . ? C74 Li2 C1 N2 -148.5(7) . . . . ? Zn2 Li2 C1 N2 -67.3(12) . . . . ? C70 Li2 C1 N2 15.3(12) . . . . ? C1 N2 C2 C3 0.9(7) . . . . ? C4 N2 C2 C3 -172.8(5) . . . . ? N2 C2 C3 N1 -0.9(7) . . . . ? C1 N1 C3 C2 0.6(7) . . . . ? C16 N1 C3 C2 172.1(5) . . . . ? C1 N2 C4 C5 85.9(9) . . . . ? C2 N2 C4 C5 -100.9(8) . . . . ? C1 N2 C4 C9 -96.3(8) . . . . ? C2 N2 C4 C9 76.8(9) . . . . ? C9 C4 C5 C6 2.6(12) . . . . ? N2 C4 C5 C6 -179.9(7) . . . . ? C9 C4 C5 C11 179.5(7) . . . . ? N2 C4 C5 C11 -3.0(11) . . . . ? C4 C5 C6 C7 -1.0(12) . . . . ? C11 C5 C6 C7 -177.9(7) . . . . ? C5 C6 C7 C8 -1.3(12) . . . . ? C6 C7 C8 C9 2.1(13) . . . . ? C7 C8 C9 C4 -0.6(12) . . . . ? C7 C8 C9 C14 -179.3(8) . . . . ? C5 C4 C9 C8 -1.8(12) . . . . ? N2 C4 C9 C8 -179.4(7) . . . . ? C5 C4 C9 C14 176.8(8) . . . . ? N2 C4 C9 C14 -0.8(12) . . . . ? C4 C5 C11 C12 -103.4(9) . . . . ? C6 C5 C11 C12 73.4(9) . . . . ? C4 C5 C11 C10 133.0(8) . . . . ? C6 C5 C11 C10 -50.2(10) . . . . ? C8 C9 C14 C15 -59.2(10) . . . . ? C4 C9 C14 C15 122.2(8) . . . . ? C8 C9 C14 C13 65.5(10) . . . . ? C4 C9 C14 C13 -113.1(8) . . . . ? C1 N1 C16 C17 71.5(9) . . . . ? C3 N1 C16 C17 -98.8(8) . . . . ? C1 N1 C16 C21 -111.5(8) . . . . ? C3 N1 C16 C21 78.2(9) . . . . ? C21 C16 C17 C18 0.8(12) . . . . ? N1 C16 C17 C18 177.6(7) . . . . ? C21 C16 C17 C23 -175.4(8) . . . . ? N1 C16 C17 C23 1.5(11) . . . . ? C16 C17 C18 C19 0.4(12) . . . . ? C23 C17 C18 C19 176.6(8) . . . . ? C17 C18 C19 C20 0.4(13) . . . . ? C18 C19 C20 C21 -2.3(14) . . . . ? C19 C20 C21 C16 3.3(13) . . . . ? C19 C20 C21 C26 -175.6(8) . . . . ? C17 C16 C21 C20 -2.5(12) . . . . ? N1 C16 C21 C20 -179.4(7) . . . . ? C17 C16 C21 C26 176.3(8) . . . . ? N1 C16 C21 C26 -0.5(12) . . . . ? C16 C17 C23 C24 86.7(9) . . . . ? C18 C17 C23 C24 -89.3(9) . . . . ? C16 C17 C23 C22 -146.3(7) . . . . ? C18 C17 C23 C22 37.7(11) . . . . ? C20 C21 C26 C25 -48.3(10) . . . . ? C16 C21 C26 C25 132.9(8) . . . . ? C20 C21 C26 C27 74.5(9) . . . . ? C16 C21 C26 C27 -104.3(8) . . . . ? C31 N3 C28 N4 0.6(7) . . . . ? C32 N3 C28 N4 177.6(6) . . . . ? C31 N3 C28 Li1 -180.0(6) . . . . ? C32 N3 C28 Li1 -3.1(10) . . . . ? C29 N4 C28 N3 0.7(7) . . . . ? C45 N4 C28 N3 -176.0(6) . . . . ? C29 N4 C28 Li1 -178.7(6) . . . . ? C45 N4 C28 Li1 4.6(10) . . . . ? C61 Li1 C28 N3 -55.7(9) . . . . ? Zn1 Li1 C28 N3 -138.2(10) . . . . ? C65 Li1 C28 N3 145.2(6) . . . . ? C61 Li1 C28 N4 123.5(8) . . . . ? Zn1 Li1 C28 N4 41.1(14) . . . . ? C65 Li1 C28 N4 -35.5(9) . . . . ? C28 N4 C29 C31 -1.8(8) . . . . ? C45 N4 C29 C31 174.9(6) . . . . ? N4 C29 C31 N3 2.1(8) . . . . ? C28 N3 C31 C29 -1.8(8) . . . . ? C32 N3 C31 C29 -178.7(7) . . . . ? C28 N3 C32 C37 109.6(7) . . . . ? C31 N3 C32 C37 -73.9(9) . . . . ? C28 N3 C32 C33 -72.1(8) . . . . ? C31 N3 C32 C33 104.4(7) . . . . ? C37 C32 C33 C34 -4.2(9) . . . . ? N3 C32 C33 C34 177.6(5) . . . . ? C37 C32 C33 C39 175.2(6) . . . . ? N3 C32 C33 C39 -3.0(8) . . . . ? C32 C33 C34 C35 3.6(10) . . . . ? C39 C33 C34 C35 -175.8(6) . . . . ? C33 C34 C35 C36 -2.2(11) . . . . ? C34 C35 C36 C37 1.3(10) . . . . ? C35 C36 C37 C32 -1.8(10) . . . . ? C35 C36 C37 C42 178.4(6) . . . . ? C33 C32 C37 C36 3.4(10) . . . . ? N3 C32 C37 C36 -178.4(6) . . . . ? C33 C32 C37 C42 -176.9(5) . . . . ? N3 C32 C37 C42 1.4(9) . . . . ? C34 C33 C39 C38 94.9(7) . . . . ? C32 C33 C39 C38 -84.4(7) . . . . ? C34 C33 C39 C40 -30.2(9) . . . . ? C32 C33 C39 C40 150.5(6) . . . . ? C36 C37 C42 C43 52.1(9) . . . . ? C32 C37 C42 C43 -127.7(8) . . . . ? C36 C37 C42 C41 -70.5(9) . . . . ? C32 C37 C42 C41 109.7(8) . . . . ? C28 N4 C45 C50 -81.6(8) . . . . ? C29 N4 C45 C50 102.2(7) . . . . ? C28 N4 C45 C46 100.3(7) . . . . ? C29 N4 C45 C46 -75.9(8) . . . . ? C50 C45 C46 C47 0.9(10) . . . . ? N4 C45 C46 C47 178.9(5) . . . . ? C50 C45 C46 C55 -179.9(6) . . . . ? N4 C45 C46 C55 -1.9(9) . . . . ? C45 C46 C47 C48 -0.2(10) . . . . ? C55 C46 C47 C48 -179.4(6) . . . . ? C46 C47 C48 C49 0.1(11) . . . . ? C47 C48 C49 C50 -0.7(11) . . . . ? C48 C49 C50 C45 1.3(10) . . . . ? C48 C49 C50 C52 -177.8(6) . . . . ? C46 C45 C50 C49 -1.5(9) . . . . ? N4 C45 C50 C49 -179.4(5) . . . . ? C46 C45 C50 C52 177.7(6) . . . . ? N4 C45 C50 C52 -0.3(9) . . . . ? C49 C50 C52 C53 58.9(8) . . . . ? C45 C50 C52 C53 -120.1(7) . . . . ? C49 C50 C52 C51 -62.3(8) . . . . ? C45 C50 C52 C51 118.7(7) . . . . ? C47 C46 C55 C54 51.7(9) . . . . ? C45 C46 C55 C54 -127.5(8) . . . . ? C47 C46 C55 C56 -68.2(9) . . . . ? C45 C46 C55 C56 112.6(8) . . . . ? C61 Zn1 C57 C58 -155.5(5) . . . . ? C65 Zn1 C57 C58 34.1(6) . . . . ? Li1 Zn1 C57 C58 -61.8(13) . . . . ? C61 Zn1 C57 C60 -33.4(6) . . . . ? C65 Zn1 C57 C60 156.2(5) . . . . ? Li1 Zn1 C57 C60 60.2(13) . . . . ? C61 Zn1 C57 C59 83.7(7) . . . . ? C65 Zn1 C57 C59 -86.7(7) . . . . ? Li1 Zn1 C57 C59 177.4(9) . . . . ? C57 Zn1 C61 C62 64.7(6) . . . . ? C65 Zn1 C61 C62 -124.5(5) . . . . ? Li1 Zn1 C61 C62 -88.7(5) . . . . ? C57 Zn1 C61 C64 -160.6(5) . . . . ? C65 Zn1 C61 C64 10.2(6) . . . . ? Li1 Zn1 C61 C64 46.0(5) . . . . ? C57 Zn1 C61 C63 -48.8(6) . . . . ? C65 Zn1 C61 C63 121.9(5) . . . . ? Li1 Zn1 C61 C63 157.8(6) . . . . ? C57 Zn1 C61 Li1 153.4(3) . . . . ? C65 Zn1 C61 Li1 -35.9(4) . . . . ? C28 Li1 C61 C62 -23.4(9) . . . . ? Zn1 Li1 C61 C62 113.3(5) . . . . ? C65 Li1 C61 C62 140.4(5) . . . . ? C28 Li1 C61 C64 84.0(8) . . . . ? Zn1 Li1 C61 C64 -139.2(6) . . . . ? C65 Li1 C61 C64 -112.2(6) . . . . ? C28 Li1 C61 C63 166.3(11) . . . . ? Zn1 Li1 C61 C63 -57.0(12) . . . . ? C65 Li1 C61 C63 -29.9(14) . . . . ? C28 Li1 C61 Zn1 -136.8(7) . . . . ? C65 Li1 C61 Zn1 27.1(3) . . . . ? C57 Zn1 C65 C68 -57.5(6) . . . . ? C61 Zn1 C65 C68 131.5(5) . . . . ? Li1 Zn1 C65 C68 96.9(6) . . . . ? C57 Zn1 C65 C67 56.9(6) . . . . ? C61 Zn1 C65 C67 -114.1(5) . . . . ? Li1 Zn1 C65 C67 -148.8(6) . . . . ? C57 Zn1 C65 C66 170.1(5) . . . . ? C61 Zn1 C65 C66 -0.9(6) . . . . ? Li1 Zn1 C65 C66 -35.6(5) . . . . ? C57 Zn1 C65 Li1 -154.3(4) . . . . ? C61 Zn1 C65 Li1 34.6(4) . . . . ? C28 Li1 C65 C68 27.8(8) . . . . ? C61 Li1 C65 C68 -136.6(5) . . . . ? Zn1 Li1 C65 C68 -109.0(5) . . . . ? C28 Li1 C65 C67 -160.8(8) . . . . ? C61 Li1 C65 C67 34.8(10) . . . . ? Zn1 Li1 C65 C67 62.4(8) . . . . ? C28 Li1 C65 C66 -75.3(7) . . . . ? C61 Li1 C65 C66 120.3(6) . . . . ? Zn1 Li1 C65 C66 147.8(6) . . . . ? C28 Li1 C65 Zn1 136.8(6) . . . . ? C61 Li1 C65 Zn1 -27.6(3) . . . . ? C78 Zn2 C70 C73 157.4(6) . . . . ? C74 Zn2 C70 C73 -34.6(8) . . . . ? Li2 Zn2 C70 C73 7.7(7) . . . . ? C78 Zn2 C70 C71 27.8(8) . . . . ? C74 Zn2 C70 C71 -164.3(6) . . . . ? Li2 Zn2 C70 C71 -122.0(7) . . . . ? C78 Zn2 C70 C72 -85.6(6) . . . . ? C74 Zn2 C70 C72 82.3(5) . . . . ? Li2 Zn2 C70 C72 124.6(5) . . . . ? C78 Zn2 C70 Li2 149.8(4) . . . . ? C74 Zn2 C70 Li2 -42.3(4) . . . . ? C1 Li2 C70 C73 53.6(9) . . . . ? C74 Li2 C70 C73 -138.5(6) . . . . ? Zn2 Li2 C70 C73 -172.7(6) . . . . ? C1 Li2 C70 C71 -34.6(12) . . . . ? C74 Li2 C70 C71 133.3(6) . . . . ? Zn2 Li2 C70 C71 99.1(6) . . . . ? C1 Li2 C70 C72 145.6(8) . . . . ? C74 Li2 C70 C72 -46.5(7) . . . . ? Zn2 Li2 C70 C72 -80.7(6) . . . . ? C1 Li2 C70 Zn2 -133.7(9) . . . . ? C74 Li2 C70 Zn2 34.2(3) . . . . ? C78 Zn2 C74 C76 50.0(6) . . . . ? C70 Zn2 C74 C76 -119.0(5) . . . . ? Li2 Zn2 C74 C76 -165.0(6) . . . . ? C78 Zn2 C74 C77 165.0(6) . . . . ? C70 Zn2 C74 C77 -4.0(8) . . . . ? Li2 Zn2 C74 C77 -50.0(7) . . . . ? C78 Zn2 C74 C75 -64.8(7) . . . . ? C70 Zn2 C74 C75 126.2(5) . . . . ? Li2 Zn2 C74 C75 80.2(6) . . . . ? C78 Zn2 C74 Li2 -145.0(4) . . . . ? C70 Zn2 C74 Li2 46.0(5) . . . . ? C1 Li2 C74 C76 -170.7(15) . . . . ? Zn2 Li2 C74 C76 52.3(18) . . . . ? C70 Li2 C74 C76 20(2) . . . . ? C1 Li2 C74 C77 -86.5(9) . . . . ? Zn2 Li2 C74 C77 136.5(5) . . . . ? C70 Li2 C74 C77 104.4(5) . . . . ? C1 Li2 C74 C75 21.1(9) . . . . ? Zn2 Li2 C74 C75 -115.9(5) . . . . ? C70 Li2 C74 C75 -148.0(5) . . . . ? C1 Li2 C74 Zn2 137.0(8) . . . . ? C70 Li2 C74 Zn2 -32.2(3) . . . . ? C70 Zn2 C78 C80 90.6(6) . . . . ? C74 Zn2 C78 C80 -76.7(6) . . . . ? Li2 Zn2 C78 C80 -157.1(6) . . . . ? C70 Zn2 C78 C81 -149.3(5) . . . . ? C74 Zn2 C78 C81 43.5(7) . . . . ? Li2 Zn2 C78 C81 -36.9(9) . . . . ? C70 Zn2 C78 C79 -30.0(8) . . . . ? C74 Zn2 C78 C79 162.8(6) . . . . ? Li2 Zn2 C78 C79 82.4(8) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.060 _refine_diff_density_min -1.824 _refine_diff_density_rms 0.138 _database_code_depnum_ccdc_archive 'CCDC 923040' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_jg_au #TrackingRef 'hevia5.cif' _audit_creation_method ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C45 H50 Au2 Cl N2 P' _chemical_formula_sum 'C45 H50 Au2 Cl N2 P' _chemical_formula_weight 1079.22 _chemical_compound_source synthesis loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Au Au -4.4197 7.2980 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 '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' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.2833(3) _cell_length_b 14.4759(3) _cell_length_c 16.9188(4) _cell_angle_alpha 68.109(2) _cell_angle_beta 81.380(2) _cell_angle_gamma 86.270(2) _cell_volume 2085.74(9) _cell_formula_units_Z 2 _cell_measurement_temperature 150.0(1) _cell_measurement_reflns_used 24916 _cell_measurement_theta_min 2.8387 _cell_measurement_theta_max 74.4603 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.1540 _exptl_crystal_size_mid 0.0832 _exptl_crystal_size_min 0.0195 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.718 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1048 _exptl_absorpt_coefficient_mu 14.225 _exptl_absorpt_correction_T_min 0.41541 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150.0(1) _diffrn_radiation_wavelength 1.5418 _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_source 'Nova (Cu) X-ray Source' _diffrn_radiation_monochromator mirror _diffrn_measurement_device_type 'Xcalibur, Onyx, Nova' _diffrn_measurement_device ; 165 mm Onyx CCD detector in \k-geometry diffractometer ; _diffrn_detector_area_resol_mean 8.2640 _diffrn_measurement_method '\w scans' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 46765 _diffrn_reflns_av_R_equivalents 0.0487 _diffrn_reflns_av_sigmaI/netI 0.0290 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.84 _diffrn_reflns_theta_max 74.63 _reflns_number_total 8371 _reflns_number_gt 7267 _reflns_threshold_expression I>2\s(I) _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_structure_solution 'DIRDIF-99 (Beurskens, 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 2007)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^ > 2\s(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^)+(0.0317P)^2^+8.8668P] 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 8371 _refine_ls_number_parameters 468 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0382 _refine_ls_R_factor_gt 0.0311 _refine_ls_wR_factor_ref 0.0804 _refine_ls_wR_factor_gt 0.0764 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.051 _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 C11 C 0.7433(10) 0.1024(5) 0.0077(5) 0.065(2) Uani 1 1 d . . . H11A H 0.8032 0.0639 -0.0202 0.098 Uiso 1 1 calc R . . H11B H 0.6562 0.0663 0.0382 0.098 Uiso 1 1 calc R . . H11C H 0.7959 0.1146 0.0475 0.098 Uiso 1 1 calc R . . C1 C 0.3047(6) 0.1954(4) -0.1859(3) 0.0273(10) Uani 1 1 d . . . C5 C 0.5946(6) 0.2591(4) -0.0178(3) 0.0318(11) Uani 1 1 d . . . C34 C 0.2070(6) -0.0706(4) -0.3137(4) 0.0348(12) Uani 1 1 d . . . C20 C 0.4886(6) 0.3426(4) -0.4707(3) 0.0365(12) Uani 1 1 d . . . H20 H 0.5589 0.3221 -0.5061 0.044 Uiso 1 1 calc R . . C43 C 0.0456(7) 0.2389(4) -0.5756(4) 0.0404(13) Uani 1 1 d . . . H43 H 0.0397 0.2804 -0.6322 0.048 Uiso 1 1 calc R . . C21 C 0.4854(6) 0.2982(4) -0.3823(3) 0.0292(11) Uani 1 1 d . . . C45 C 0.1522(7) 0.1969(5) -0.4462(4) 0.0423(14) Uani 1 1 d . . . H45 H 0.2163 0.2119 -0.4155 0.051 Uiso 1 1 calc R . . C32 C -0.2863(7) -0.1318(4) -0.2340(4) 0.0424(14) Uani 1 1 d . . . H32 H -0.3250 -0.1808 -0.2476 0.051 Uiso 1 1 calc R . . C42 C -0.0416(7) 0.1571(4) -0.5375(4) 0.0372(12) Uani 1 1 d . . . H42 H -0.1087 0.1445 -0.5678 0.045 Uiso 1 1 calc R . . C10 C 0.7031(6) 0.2015(5) -0.0595(4) 0.0386(13) Uani 1 1 d . . . H10 H 0.6557 0.1869 -0.1015 0.046 Uiso 1 1 calc R . . C17 C 0.2740(6) 0.4036(4) -0.3659(3) 0.0308(11) Uani 1 1 d . . . C35 C 0.1904(8) -0.1682(4) -0.2562(4) 0.0433(14) Uani 1 1 d . . . H35 H 0.1173 -0.1836 -0.2094 0.052 Uiso 1 1 calc R . . C22 C 0.1553(6) 0.4372(4) -0.3104(4) 0.0380(13) Uani 1 1 d . . . H22 H 0.1586 0.3931 -0.2505 0.046 Uiso 1 1 calc R . . C25 C 0.5985(6) 0.2207(4) -0.3439(4) 0.0344(12) Uani 1 1 d . . . H25 H 0.5715 0.1943 -0.2813 0.041 Uiso 1 1 calc R . . C40 C 0.0682(6) 0.1127(4) -0.4080(3) 0.0296(11) Uani 1 1 d . . . C8 C 0.3961(7) 0.3635(4) 0.0612(3) 0.0366(12) Uani 1 1 d . . . H8 H 0.3313 0.3979 0.0881 0.044 Uiso 1 1 calc R . . C44 C 0.1415(8) 0.2597(5) -0.5305(4) 0.0500(16) Uani 1 1 d . . . H44 H 0.1996 0.3159 -0.5563 0.060 Uiso 1 1 calc R . . C19 C 0.3916(7) 0.4156(4) -0.5072(4) 0.0388(13) Uani 1 1 d . . . H19 H 0.3983 0.4454 -0.5667 0.047 Uiso 1 1 calc R . . C2 C 0.3327(6) 0.1834(4) -0.1059(3) 0.0310(11) Uani 1 1 d . . . H2 H 0.3022 0.1301 -0.0556 0.037 Uiso 1 1 calc R . . C9 C 0.3520(6) 0.3351(4) -0.0018(3) 0.0314(11) Uani 1 1 d . . . C14 C 0.0857(7) 0.3147(5) 0.0529(4) 0.0481(15) Uani 1 1 d . . . H14A H 0.0954 0.2435 0.0746 0.072 Uiso 1 1 calc R . . H14B H -0.0098 0.3333 0.0366 0.072 Uiso 1 1 calc R . . H14C H 0.0995 0.3392 0.0967 0.072 Uiso 1 1 calc R . . C6 C 0.6319(6) 0.2892(5) 0.0459(4) 0.0379(13) Uani 1 1 d . . . H6 H 0.7239 0.2738 0.0630 0.045 Uiso 1 1 calc R . . C33 C -0.1470(7) -0.0973(4) -0.2690(4) 0.0383(13) Uani 1 1 d . . . H33 H -0.0923 -0.1230 -0.3069 0.046 Uiso 1 1 calc R . . C16 C 0.3776(6) 0.3313(4) -0.3316(3) 0.0271(10) Uani 1 1 d . . . C41 C -0.0306(6) 0.0929(4) -0.4542(3) 0.0334(12) Uani 1 1 d . . . H41 H -0.0889 0.0367 -0.4290 0.040 Uiso 1 1 calc R . . C13 C 0.2005(6) 0.3597(4) -0.0257(4) 0.0354(12) Uani 1 1 d . . . H13 H 0.1887 0.3297 -0.0675 0.042 Uiso 1 1 calc R . . C7 C 0.5342(7) 0.3415(5) 0.0839(4) 0.0442(14) Uani 1 1 d . . . H7 H 0.5620 0.3621 0.1253 0.053 Uiso 1 1 calc R . . C30 C -0.3096(8) -0.0205(5) -0.1561(4) 0.0524(17) Uani 1 1 d . . . H30 H -0.3644 0.0050 -0.1180 0.063 Uiso 1 1 calc R . . C18 C 0.2828(7) 0.4452(4) -0.4551(4) 0.0380(13) Uani 1 1 d . . . H18 H 0.2151 0.4934 -0.4803 0.046 Uiso 1 1 calc R . . C4 C 0.4556(6) 0.2844(4) -0.0409(3) 0.0283(11) Uani 1 1 d . . . C15 C 0.1784(8) 0.4721(5) -0.0684(5) 0.0514(16) Uani 1 1 d . . . H15A H 0.1831 0.5030 -0.0275 0.077 Uiso 1 1 calc R . . H15B H 0.0848 0.4854 -0.0882 0.077 Uiso 1 1 calc R . . H15C H 0.2533 0.4986 -0.1163 0.077 Uiso 1 1 calc R . . C12 C 0.8371(8) 0.2628(6) -0.1071(5) 0.0595(19) Uani 1 1 d . . . H12A H 0.8083 0.3247 -0.1484 0.089 Uiso 1 1 calc R . . H12B H 0.9002 0.2267 -0.1361 0.089 Uiso 1 1 calc R . . H12C H 0.8878 0.2758 -0.0669 0.089 Uiso 1 1 calc R . . C39 C 0.3188(7) -0.0488(5) -0.3814(4) 0.0447(14) Uani 1 1 d . . . H39 H 0.3308 0.0161 -0.4210 0.054 Uiso 1 1 calc R . . C36 C 0.2808(9) -0.2423(5) -0.2678(5) 0.0551(18) Uani 1 1 d . . . H36 H 0.2653 -0.3078 -0.2304 0.066 Uiso 1 1 calc R . . C29 C -0.1693(7) 0.0128(5) -0.1912(4) 0.0450(15) Uani 1 1 d . . . H29 H -0.1300 0.0605 -0.1762 0.054 Uiso 1 1 calc R . . C23 C 0.1836(9) 0.5424(5) -0.3177(5) 0.0575(18) Uani 1 1 d . . . H23A H 0.2766 0.5446 -0.3001 0.086 Uiso 1 1 calc R . . H23B H 0.1086 0.5622 -0.2814 0.086 Uiso 1 1 calc R . . H23C H 0.1835 0.5871 -0.3763 0.086 Uiso 1 1 calc R . . C3 C 0.4409(5) 0.3275(4) -0.1934(3) 0.0258(10) Uani 1 1 d . . . C27 C 0.7486(7) 0.2676(5) -0.3634(5) 0.0519(17) Uani 1 1 d . . . H27A H 0.7779 0.2939 -0.4245 0.078 Uiso 1 1 calc R . . H27B H 0.8179 0.2180 -0.3364 0.078 Uiso 1 1 calc R . . H27C H 0.7444 0.3204 -0.3417 0.078 Uiso 1 1 calc R . . C26 C 0.6003(7) 0.1336(5) -0.3749(5) 0.0478(15) Uani 1 1 d . . . H26A H 0.5050 0.1050 -0.3607 0.072 Uiso 1 1 calc R . . H26B H 0.6691 0.0839 -0.3473 0.072 Uiso 1 1 calc R . . H26C H 0.6280 0.1572 -0.4361 0.072 Uiso 1 1 calc R . . C31 C -0.3678(8) -0.0920(5) -0.1779(4) 0.0530(17) Uani 1 1 d . . . H31 H -0.4625 -0.1137 -0.1549 0.064 Uiso 1 1 calc R . . C28 C -0.0866(6) -0.0241(4) -0.2486(3) 0.0332(11) Uani 1 1 d . . . C37 C 0.3938(9) -0.2206(5) -0.3342(5) 0.059(2) Uani 1 1 d . . . H37 H 0.4564 -0.2707 -0.3411 0.071 Uiso 1 1 calc R . . C38 C 0.4129(8) -0.1233(6) -0.3903(5) 0.0570(18) Uani 1 1 d . . . H38 H 0.4902 -0.1077 -0.4348 0.068 Uiso 1 1 calc R . . C24 C 0.0047(8) 0.4284(7) -0.3324(6) 0.067(2) Uani 1 1 d . . . H24A H 0.0012 0.4665 -0.3922 0.101 Uiso 1 1 calc R . . H24B H -0.0675 0.4533 -0.2982 0.101 Uiso 1 1 calc R . . H24C H -0.0144 0.3598 -0.3206 0.101 Uiso 1 1 calc R . . Au1 Au 0.19867(3) 0.114786(16) -0.233917(14) 0.03270(7) Uani 1 1 d . . . Au2 Au 0.55261(2) 0.451513(14) -0.230448(12) 0.02633(6) Uani 1 1 d . . . N1 N 0.4140(5) 0.2632(3) -0.1111(3) 0.0274(9) Uani 1 1 d . . . N2 N 0.3743(4) 0.2867(3) -0.2388(3) 0.0246(8) Uani 1 1 d . . . P1 P 0.09081(15) 0.02998(10) -0.29920(8) 0.0300(3) Uani 1 1 d . . . Cl1 Cl 0.68488(16) 0.59201(10) -0.26418(9) 0.0392(3) Uani 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 C11 0.082(6) 0.053(4) 0.053(4) -0.015(3) -0.003(4) 0.023(4) C1 0.026(3) 0.029(2) 0.030(2) -0.013(2) -0.007(2) 0.000(2) C5 0.030(3) 0.034(3) 0.029(3) -0.009(2) -0.001(2) -0.004(2) C34 0.034(3) 0.037(3) 0.041(3) -0.021(2) -0.015(2) 0.005(2) C20 0.035(3) 0.043(3) 0.033(3) -0.017(2) 0.003(2) -0.006(3) C43 0.051(4) 0.034(3) 0.032(3) -0.005(2) -0.010(3) 0.003(3) C21 0.023(3) 0.032(3) 0.031(3) -0.011(2) -0.001(2) -0.003(2) C45 0.043(4) 0.044(3) 0.039(3) -0.011(3) -0.012(3) -0.009(3) C32 0.040(4) 0.039(3) 0.043(3) -0.009(3) -0.003(3) -0.014(3) C42 0.035(3) 0.046(3) 0.035(3) -0.019(2) -0.009(2) 0.003(3) C10 0.030(3) 0.049(3) 0.040(3) -0.021(3) -0.005(2) 0.005(3) C17 0.027(3) 0.025(2) 0.038(3) -0.008(2) -0.008(2) -0.002(2) C35 0.050(4) 0.039(3) 0.039(3) -0.011(2) -0.015(3) 0.007(3) C22 0.030(3) 0.038(3) 0.042(3) -0.011(2) -0.008(2) 0.011(2) C25 0.029(3) 0.036(3) 0.039(3) -0.017(2) -0.002(2) 0.005(2) C40 0.029(3) 0.028(2) 0.031(3) -0.011(2) -0.002(2) 0.003(2) C8 0.042(3) 0.039(3) 0.032(3) -0.018(2) -0.003(2) -0.001(2) C44 0.063(5) 0.043(3) 0.039(3) -0.005(3) -0.008(3) -0.018(3) C19 0.045(4) 0.039(3) 0.028(3) -0.007(2) -0.005(2) -0.010(3) C2 0.029(3) 0.032(3) 0.030(3) -0.009(2) -0.002(2) 0.001(2) C9 0.031(3) 0.034(3) 0.028(3) -0.010(2) -0.004(2) -0.002(2) C14 0.035(4) 0.053(4) 0.050(4) -0.012(3) -0.002(3) -0.004(3) C6 0.028(3) 0.052(3) 0.035(3) -0.016(3) -0.008(2) -0.004(3) C33 0.043(4) 0.036(3) 0.033(3) -0.010(2) -0.004(2) -0.003(3) C16 0.027(3) 0.028(2) 0.025(2) -0.0089(19) -0.006(2) 0.001(2) C41 0.031(3) 0.036(3) 0.036(3) -0.017(2) -0.004(2) 0.004(2) C13 0.033(3) 0.038(3) 0.038(3) -0.018(2) -0.007(2) 0.006(2) C7 0.048(4) 0.055(4) 0.036(3) -0.024(3) -0.006(3) -0.007(3) C30 0.055(4) 0.056(4) 0.042(3) -0.019(3) 0.012(3) -0.008(3) C18 0.034(3) 0.034(3) 0.039(3) -0.004(2) -0.012(2) -0.002(2) C4 0.032(3) 0.026(2) 0.026(2) -0.0086(19) -0.004(2) -0.003(2) C15 0.046(4) 0.042(3) 0.060(4) -0.012(3) -0.007(3) 0.009(3) C12 0.038(4) 0.070(5) 0.062(4) -0.023(4) 0.014(3) 0.001(3) C39 0.033(3) 0.046(3) 0.058(4) -0.023(3) -0.004(3) 0.000(3) C36 0.069(5) 0.042(3) 0.057(4) -0.015(3) -0.032(4) 0.016(3) C29 0.049(4) 0.048(3) 0.040(3) -0.021(3) 0.004(3) -0.009(3) C23 0.058(5) 0.051(4) 0.066(4) -0.027(3) -0.008(4) 0.015(3) C3 0.018(2) 0.029(2) 0.031(2) -0.013(2) -0.0013(19) 0.0016(19) C27 0.031(4) 0.055(4) 0.078(5) -0.033(4) -0.014(3) 0.008(3) C26 0.037(4) 0.044(3) 0.066(4) -0.026(3) -0.006(3) 0.009(3) C31 0.043(4) 0.055(4) 0.048(4) -0.009(3) 0.011(3) -0.015(3) C28 0.033(3) 0.033(3) 0.031(3) -0.009(2) -0.004(2) -0.004(2) C37 0.054(5) 0.055(4) 0.085(5) -0.038(4) -0.038(4) 0.031(4) C38 0.040(4) 0.069(5) 0.073(5) -0.040(4) -0.006(3) 0.009(3) C24 0.034(4) 0.083(6) 0.083(6) -0.031(5) -0.003(4) 0.006(4) Au1 0.03433(14) 0.03168(12) 0.03276(12) -0.01192(9) -0.00616(9) -0.00100(9) Au2 0.02515(12) 0.02683(11) 0.02645(11) -0.00974(8) -0.00231(8) 0.00044(8) N1 0.029(2) 0.029(2) 0.025(2) -0.0106(17) -0.0054(17) -0.0004(18) N2 0.024(2) 0.0237(19) 0.028(2) -0.0115(16) -0.0043(16) 0.0029(16) P1 0.0302(7) 0.0294(6) 0.0295(6) -0.0098(5) -0.0045(5) 0.0000(5) Cl1 0.0421(8) 0.0340(6) 0.0403(7) -0.0140(5) 0.0031(6) -0.0094(6) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 C11 C10 1.527(9) . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C1 C2 1.362(7) . ? C1 N2 1.421(6) . ? C1 Au1 2.022(5) . ? C5 C4 1.392(8) . ? C5 C6 1.398(8) . ? C5 C10 1.524(8) . ? C34 C39 1.381(9) . ? C34 C35 1.387(8) . ? C34 P1 1.823(6) . ? C20 C19 1.365(9) . ? C20 C21 1.386(7) . ? C20 H20 0.9300 . ? C43 C42 1.368(8) . ? C43 C44 1.369(9) . ? C43 H43 0.9300 . ? C21 C16 1.398(7) . ? C21 C25 1.514(8) . ? C45 C40 1.378(8) . ? C45 C44 1.391(8) . ? C45 H45 0.9300 . ? C32 C33 1.381(8) . ? C32 C31 1.393(9) . ? C32 H32 0.9300 . ? C42 C41 1.384(8) . ? C42 H42 0.9300 . ? C10 C12 1.515(9) . ? C10 H10 0.9800 . ? C17 C18 1.393(8) . ? C17 C16 1.393(7) . ? C17 C22 1.515(8) . ? C35 C36 1.373(9) . ? C35 H35 0.9300 . ? C22 C23 1.519(9) . ? C22 C24 1.524(10) . ? C22 H22 0.9800 . ? C25 C27 1.526(8) . ? C25 C26 1.534(8) . ? C25 H25 0.9800 . ? C40 C41 1.396(8) . ? C40 P1 1.818(5) . ? C8 C7 1.377(9) . ? C8 C9 1.397(7) . ? C8 H8 0.9300 . ? C44 H44 0.9300 . ? C19 C18 1.392(9) . ? C19 H19 0.9300 . ? C2 N1 1.389(7) . ? C2 H2 0.9300 . ? C9 C4 1.408(7) . ? C9 C13 1.505(8) . ? C14 C13 1.532(8) . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C6 C7 1.380(9) . ? C6 H6 0.9300 . ? C33 C28 1.402(8) . ? C33 H33 0.9300 . ? C16 N2 1.455(6) . ? C41 H41 0.9300 . ? C13 C15 1.528(8) . ? C13 H13 0.9800 . ? C7 H7 0.9300 . ? C30 C31 1.385(10) . ? C30 C29 1.385(9) . ? C30 H30 0.9300 . ? C18 H18 0.9300 . ? C4 N1 1.442(6) . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C39 C38 1.381(9) . ? C39 H39 0.9300 . ? C36 C37 1.373(11) . ? C36 H36 0.9300 . ? C29 C28 1.388(8) . ? C29 H29 0.9300 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C3 N1 1.351(6) . ? C3 N2 1.359(6) . ? C3 Au2 1.975(5) . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C31 H31 0.9300 . ? C28 P1 1.817(6) . ? C37 C38 1.379(11) . ? C37 H37 0.9300 . ? C38 H38 0.9300 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? Au1 P1 2.2874(13) . ? Au2 Cl1 2.2846(13) . ? 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 C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C2 C1 N2 103.0(4) . . ? C2 C1 Au1 134.5(4) . . ? N2 C1 Au1 122.5(3) . . ? C4 C5 C6 116.9(5) . . ? C4 C5 C10 122.3(5) . . ? C6 C5 C10 120.8(5) . . ? C39 C34 C35 118.8(6) . . ? C39 C34 P1 119.4(5) . . ? C35 C34 P1 121.8(5) . . ? C19 C20 C21 122.0(5) . . ? C19 C20 H20 119.0 . . ? C21 C20 H20 119.0 . . ? C42 C43 C44 120.2(5) . . ? C42 C43 H43 119.9 . . ? C44 C43 H43 119.9 . . ? C20 C21 C16 117.0(5) . . ? C20 C21 C25 120.7(5) . . ? C16 C21 C25 122.3(5) . . ? C40 C45 C44 120.3(6) . . ? C40 C45 H45 119.9 . . ? C44 C45 H45 119.9 . . ? C33 C32 C31 118.9(6) . . ? C33 C32 H32 120.6 . . ? C31 C32 H32 120.6 . . ? C43 C42 C41 120.5(5) . . ? C43 C42 H42 119.8 . . ? C41 C42 H42 119.8 . . ? C12 C10 C5 111.2(5) . . ? C12 C10 C11 111.4(6) . . ? C5 C10 C11 110.4(5) . . ? C12 C10 H10 107.9 . . ? C5 C10 H10 107.9 . . ? C11 C10 H10 107.9 . . ? C18 C17 C16 117.2(5) . . ? C18 C17 C22 120.1(5) . . ? C16 C17 C22 122.7(5) . . ? C36 C35 C34 120.6(6) . . ? C36 C35 H35 119.7 . . ? C34 C35 H35 119.7 . . ? C17 C22 C23 110.4(5) . . ? C17 C22 C24 111.5(5) . . ? C23 C22 C24 111.6(6) . . ? C17 C22 H22 107.7 . . ? C23 C22 H22 107.7 . . ? C24 C22 H22 107.7 . . ? C21 C25 C27 110.7(5) . . ? C21 C25 C26 111.1(5) . . ? C27 C25 C26 111.6(5) . . ? C21 C25 H25 107.7 . . ? C27 C25 H25 107.7 . . ? C26 C25 H25 107.7 . . ? C45 C40 C41 119.1(5) . . ? C45 C40 P1 118.9(4) . . ? C41 C40 P1 122.0(4) . . ? C7 C8 C9 120.9(5) . . ? C7 C8 H8 119.5 . . ? C9 C8 H8 119.5 . . ? C43 C44 C45 120.1(6) . . ? C43 C44 H44 120.0 . . ? C45 C44 H44 120.0 . . ? C20 C19 C18 119.8(5) . . ? C20 C19 H19 120.1 . . ? C18 C19 H19 120.1 . . ? C1 C2 N1 109.3(4) . . ? C1 C2 H2 125.4 . . ? N1 C2 H2 125.4 . . ? C8 C9 C4 116.8(5) . . ? C8 C9 C13 120.2(5) . . ? C4 C9 C13 123.0(5) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C7 C6 C5 121.1(6) . . ? C7 C6 H6 119.5 . . ? C5 C6 H6 119.5 . . ? C32 C33 C28 121.2(6) . . ? C32 C33 H33 119.4 . . ? C28 C33 H33 119.4 . . ? C17 C16 C21 123.0(5) . . ? C17 C16 N2 119.3(4) . . ? C21 C16 N2 117.7(4) . . ? C42 C41 C40 119.8(5) . . ? C42 C41 H41 120.1 . . ? C40 C41 H41 120.1 . . ? C9 C13 C15 111.2(5) . . ? C9 C13 C14 110.9(5) . . ? C15 C13 C14 111.3(5) . . ? C9 C13 H13 107.8 . . ? C15 C13 H13 107.8 . . ? C14 C13 H13 107.8 . . ? C8 C7 C6 120.7(5) . . ? C8 C7 H7 119.6 . . ? C6 C7 H7 119.6 . . ? C31 C30 C29 119.7(6) . . ? C31 C30 H30 120.2 . . ? C29 C30 H30 120.2 . . ? C19 C18 C17 120.9(5) . . ? C19 C18 H18 119.5 . . ? C17 C18 H18 119.5 . . ? C5 C4 C9 123.4(5) . . ? C5 C4 N1 120.0(5) . . ? C9 C4 N1 116.6(5) . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C34 C39 C38 120.0(6) . . ? C34 C39 H39 120.0 . . ? C38 C39 H39 120.0 . . ? C35 C36 C37 120.7(7) . . ? C35 C36 H36 119.7 . . ? C37 C36 H36 119.7 . . ? C30 C29 C28 120.8(6) . . ? C30 C29 H29 119.6 . . ? C28 C29 H29 119.6 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? N1 C3 N2 104.4(4) . . ? N1 C3 Au2 124.3(4) . . ? N2 C3 Au2 131.3(4) . . ? 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 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 . . ? C30 C31 C32 120.8(6) . . ? C30 C31 H31 119.6 . . ? C32 C31 H31 119.6 . . ? C29 C28 C33 118.6(5) . . ? C29 C28 P1 118.6(4) . . ? C33 C28 P1 122.6(4) . . ? C36 C37 C38 118.9(6) . . ? C36 C37 H37 120.6 . . ? C38 C37 H37 120.6 . . ? C37 C38 C39 120.9(7) . . ? C37 C38 H38 119.5 . . ? C39 C38 H38 119.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C1 Au1 P1 175.13(15) . . ? C3 Au2 Cl1 176.23(15) . . ? C3 N1 C2 110.6(4) . . ? C3 N1 C4 121.8(4) . . ? C2 N1 C4 127.3(4) . . ? C3 N2 C1 112.7(4) . . ? C3 N2 C16 123.1(4) . . ? C1 N2 C16 124.2(4) . . ? C28 P1 C40 106.5(3) . . ? C28 P1 C34 106.5(3) . . ? C40 P1 C34 104.2(2) . . ? C28 P1 Au1 117.50(18) . . ? C40 P1 Au1 109.28(17) . . ? C34 P1 Au1 111.90(18) . . ? 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 C19 C20 C21 C16 0.2(8) . . . . ? C19 C20 C21 C25 -177.3(5) . . . . ? C44 C43 C42 C41 -2.1(9) . . . . ? C4 C5 C10 C12 117.2(6) . . . . ? C6 C5 C10 C12 -62.6(7) . . . . ? C4 C5 C10 C11 -118.6(6) . . . . ? C6 C5 C10 C11 61.7(8) . . . . ? C39 C34 C35 C36 -1.9(9) . . . . ? P1 C34 C35 C36 -179.0(5) . . . . ? C18 C17 C22 C23 -70.6(7) . . . . ? C16 C17 C22 C23 109.4(6) . . . . ? C18 C17 C22 C24 54.0(7) . . . . ? C16 C17 C22 C24 -126.0(6) . . . . ? C20 C21 C25 C27 67.8(7) . . . . ? C16 C21 C25 C27 -109.5(6) . . . . ? C20 C21 C25 C26 -56.7(7) . . . . ? C16 C21 C25 C26 125.9(6) . . . . ? C44 C45 C40 C41 -1.9(9) . . . . ? C44 C45 C40 P1 177.5(5) . . . . ? C42 C43 C44 C45 0.9(11) . . . . ? C40 C45 C44 C43 1.1(11) . . . . ? C21 C20 C19 C18 -2.0(9) . . . . ? N2 C1 C2 N1 0.1(6) . . . . ? Au1 C1 C2 N1 179.0(4) . . . . ? C7 C8 C9 C4 -0.7(8) . . . . ? C7 C8 C9 C13 179.9(5) . . . . ? C4 C5 C6 C7 0.2(8) . . . . ? C10 C5 C6 C7 179.9(5) . . . . ? C31 C32 C33 C28 0.6(9) . . . . ? C18 C17 C16 C21 -1.5(8) . . . . ? C22 C17 C16 C21 178.4(5) . . . . ? C18 C17 C16 N2 179.1(5) . . . . ? C22 C17 C16 N2 -0.9(8) . . . . ? C20 C21 C16 C17 1.6(8) . . . . ? C25 C21 C16 C17 179.1(5) . . . . ? C20 C21 C16 N2 -179.0(4) . . . . ? C25 C21 C16 N2 -1.5(7) . . . . ? C43 C42 C41 C40 1.2(9) . . . . ? C45 C40 C41 C42 0.7(8) . . . . ? P1 C40 C41 C42 -178.6(4) . . . . ? C8 C9 C13 C15 66.0(7) . . . . ? C4 C9 C13 C15 -113.3(6) . . . . ? C8 C9 C13 C14 -58.4(7) . . . . ? C4 C9 C13 C14 122.3(6) . . . . ? C9 C8 C7 C6 -1.1(9) . . . . ? C5 C6 C7 C8 1.4(9) . . . . ? C20 C19 C18 C17 2.1(9) . . . . ? C16 C17 C18 C19 -0.3(8) . . . . ? C22 C17 C18 C19 179.7(5) . . . . ? C6 C5 C4 C9 -2.1(8) . . . . ? C10 C5 C4 C9 178.2(5) . . . . ? C6 C5 C4 N1 174.8(5) . . . . ? C10 C5 C4 N1 -5.0(7) . . . . ? C8 C9 C4 C5 2.3(8) . . . . ? C13 C9 C4 C5 -178.3(5) . . . . ? C8 C9 C4 N1 -174.6(4) . . . . ? C13 C9 C4 N1 4.8(7) . . . . ? C35 C34 C39 C38 -0.9(9) . . . . ? P1 C34 C39 C38 176.3(5) . . . . ? C34 C35 C36 C37 3.1(10) . . . . ? C31 C30 C29 C28 0.4(11) . . . . ? C29 C30 C31 C32 0.8(11) . . . . ? C33 C32 C31 C30 -1.4(10) . . . . ? C30 C29 C28 C33 -1.2(9) . . . . ? C30 C29 C28 P1 175.0(5) . . . . ? C32 C33 C28 C29 0.6(9) . . . . ? C32 C33 C28 P1 -175.3(5) . . . . ? C35 C36 C37 C38 -1.6(11) . . . . ? C36 C37 C38 C39 -1.2(11) . . . . ? C34 C39 C38 C37 2.4(11) . . . . ? C2 C1 Au1 P1 -154.8(14) . . . . ? N2 C1 Au1 P1 24(2) . . . . ? N1 C3 Au2 Cl1 4(3) . . . . ? N2 C3 Au2 Cl1 -176.1(18) . . . . ? N2 C3 N1 C2 0.4(5) . . . . ? Au2 C3 N1 C2 179.9(4) . . . . ? N2 C3 N1 C4 -174.2(4) . . . . ? Au2 C3 N1 C4 5.3(7) . . . . ? C1 C2 N1 C3 -0.3(6) . . . . ? C1 C2 N1 C4 173.9(5) . . . . ? C5 C4 N1 C3 -87.0(6) . . . . ? C9 C4 N1 C3 90.1(6) . . . . ? C5 C4 N1 C2 99.4(6) . . . . ? C9 C4 N1 C2 -83.6(6) . . . . ? N1 C3 N2 C1 -0.3(5) . . . . ? Au2 C3 N2 C1 -179.8(4) . . . . ? N1 C3 N2 C16 -179.0(4) . . . . ? Au2 C3 N2 C16 1.5(7) . . . . ? C2 C1 N2 C3 0.1(6) . . . . ? Au1 C1 N2 C3 -179.0(3) . . . . ? C2 C1 N2 C16 178.8(4) . . . . ? Au1 C1 N2 C16 -0.3(7) . . . . ? C17 C16 N2 C3 -86.0(6) . . . . ? C21 C16 N2 C3 94.6(6) . . . . ? C17 C16 N2 C1 95.4(6) . . . . ? C21 C16 N2 C1 -84.0(6) . . . . ? C29 C28 P1 C40 -102.5(5) . . . . ? C33 C28 P1 C40 73.4(5) . . . . ? C29 C28 P1 C34 146.7(5) . . . . ? C33 C28 P1 C34 -37.4(5) . . . . ? C29 C28 P1 Au1 20.3(6) . . . . ? C33 C28 P1 Au1 -163.7(4) . . . . ? C45 C40 P1 C28 147.9(5) . . . . ? C41 C40 P1 C28 -32.7(5) . . . . ? C45 C40 P1 C34 -99.7(5) . . . . ? C41 C40 P1 C34 79.7(5) . . . . ? C45 C40 P1 Au1 20.1(5) . . . . ? C41 C40 P1 Au1 -160.6(4) . . . . ? C39 C34 P1 C28 150.4(5) . . . . ? C35 C34 P1 C28 -32.5(5) . . . . ? C39 C34 P1 C40 38.1(5) . . . . ? C35 C34 P1 C40 -144.8(5) . . . . ? C39 C34 P1 Au1 -79.9(5) . . . . ? C35 C34 P1 Au1 97.2(5) . . . . ? C1 Au1 P1 C28 -160.3(18) . . . . ? C1 Au1 P1 C40 -38.9(18) . . . . ? C1 Au1 P1 C34 76.0(18) . . . . ? _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 74.63 _diffrn_measured_fraction_theta_full 0.978 _refine_diff_density_max 1.418 _refine_diff_density_min -1.759 _refine_diff_density_rms 0.126 #===END _database_code_depnum_ccdc_archive 'CCDC 923041'