# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 ####################################################################### # # 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_c:1 _database_code_depnum_ccdc_archive 'CCDC 878060' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C102 H60 F12 N6 O6 Zn3' _chemical_formula_weight 1889.67 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/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 14.4768(8) _cell_length_b 27.4432(15) _cell_length_c 20.5602(11) _cell_angle_alpha 90.00 _cell_angle_beta 94.1160(10) _cell_angle_gamma 90.00 _cell_volume 8147.3(8) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 18717 _cell_measurement_theta_min 1.41 _cell_measurement_theta_max 27.61 _exptl_crystal_description Block _exptl_crystal_colour Red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.541 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3840 _exptl_absorpt_coefficient_mu 0.968 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8299 _exptl_absorpt_correction_T_max 0.8927 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Bruker APEX area-detector diffractometer' _diffrn_measurement_method '\f and \w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 54457 _diffrn_reflns_av_R_equivalents 0.0776 _diffrn_reflns_av_sigmaI/netI 0.0984 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 35 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.41 _diffrn_reflns_theta_max 27.61 _reflns_number_total 18717 _reflns_number_gt 9609 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1997)' _computing_cell_refinement 'SAINT (Bruker, 1999)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL-PLUS (Sheldrick, 1990)' _computing_publication_material SHELXL-97 _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The F atoms and phenyl C atoms suffer from disorder, SIMU restraints were used to give all the F and phenyl C atoms similar Ueq values so as to achieve reasonable model. ; _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^)+(0.0728P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 18717 _refine_ls_number_parameters 1270 _refine_ls_number_restraints 438 _refine_ls_R_factor_all 0.1315 _refine_ls_R_factor_gt 0.0518 _refine_ls_wR_factor_ref 0.1483 _refine_ls_wR_factor_gt 0.1133 _refine_ls_goodness_of_fit_ref 0.910 _refine_ls_restrained_S_all 0.908 _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 C1 C 0.2369(2) 0.33756(13) 0.73981(19) 0.0415(9) Uani 1 1 d . . . C1A C 0.4471(5) 0.6031(7) 0.7555(7) 0.071(2) Uani 0.50 1 d PGU . . C2A C 0.5022(6) 0.6248(5) 0.7111(6) 0.080(2) Uani 0.50 1 d PGU . . C3A C 0.5981(6) 0.6233(4) 0.7214(5) 0.087(3) Uani 0.50 1 d PGU . . H3AA H 0.6362 0.6383 0.6908 0.104 Uiso 0.50 1 d PR . . C4A C 0.6389(5) 0.5999(4) 0.7762(5) 0.085(3) Uani 0.50 1 d PGU . . H4AA H 0.7052 0.5989 0.7834 0.102 Uiso 0.50 1 d PR . . C5A C 0.5838(7) 0.5782(4) 0.8207(5) 0.086(3) Uani 0.50 1 d PGU . . H5AA H 0.6120 0.5621 0.8585 0.103 Uiso 0.50 1 d PR . . C6A C 0.4879(7) 0.5797(6) 0.8103(7) 0.080(2) Uani 0.50 1 d PGU . . C2 C 0.3298(3) 0.34134(15) 0.7299(2) 0.0548(11) Uani 1 1 d . . . H2 H 0.3617 0.3708 0.7410 0.066 Uiso 1 1 calc R . . C3 C 0.3775(3) 0.30299(18) 0.7042(3) 0.0685(14) Uani 1 1 d . . . H3 H 0.4416 0.3070 0.6983 0.082 Uiso 1 1 calc R . . C4 C 0.3368(3) 0.26005(17) 0.6870(2) 0.0660(13) Uani 1 1 d . . . H4 H 0.3721 0.2341 0.6709 0.079 Uiso 1 1 calc R . . C5 C 0.2409(3) 0.25463(15) 0.6933(2) 0.0547(11) Uani 1 1 d . . . C6 C 0.1906(2) 0.29338(14) 0.72009(19) 0.0431(9) Uani 1 1 d . . . C7 C 0.1896(3) 0.21258(17) 0.6747(3) 0.0733(15) Uani 1 1 d . . . H7 H 0.2200 0.1856 0.6568 0.088 Uiso 1 1 calc R . . C8 C 0.0966(3) 0.21016(16) 0.6821(2) 0.0675(14) Uani 1 1 d . . . H8 H 0.0625 0.1817 0.6697 0.081 Uiso 1 1 calc R . . C9 C 0.0520(3) 0.25082(14) 0.7086(2) 0.0492(10) Uani 1 1 d . . . C10 C -0.0467(3) 0.24956(14) 0.7189(2) 0.0542(11) Uani 1 1 d . . . H10 H -0.0672 0.2705 0.7517 0.065 Uiso 1 1 calc R . . C11 C -0.1105(3) 0.22249(15) 0.6874(2) 0.0570(11) Uani 1 1 d . . . H11 H -0.0912 0.2005 0.6553 0.068 Uiso 1 1 calc R . . C12 C -0.2084(3) 0.22404(14) 0.6986(2) 0.0523(11) Uani 1 1 d . . . C13 C -0.2760(4) 0.22025(18) 0.6477(3) 0.0727(14) Uani 1 1 d . . . C14 C -0.3693(4) 0.2233(2) 0.6556(4) 0.0927(19) Uani 1 1 d . . . H14 H -0.4130 0.2204 0.6191 0.111 Uiso 1 1 calc R . . C15 C -0.3984(4) 0.23062(19) 0.7160(4) 0.089(2) Uani 1 1 d . . . H15 H -0.4627 0.2338 0.7217 0.107 Uiso 1 1 calc R . . C16 C -0.3355(3) 0.23343(17) 0.7690(3) 0.0775(15) Uani 1 1 d . . . H16 H -0.3557 0.2377 0.8116 0.093 Uiso 1 1 calc R . . C17 C -0.2436(3) 0.23007(15) 0.7595(2) 0.0578(11) Uani 1 1 d . . . C18 C -0.1362(2) 0.35066(13) 0.8002(2) 0.0415(9) Uani 1 1 d . . . C19 C -0.2310(2) 0.35430(15) 0.8026(2) 0.0531(11) Uani 1 1 d . . . H19 H -0.2676 0.3647 0.7649 0.064 Uiso 1 1 calc R . . C20 C -0.2740(3) 0.34291(16) 0.8592(2) 0.0562(12) Uani 1 1 d . . . H20 H -0.3394 0.3461 0.8591 0.067 Uiso 1 1 calc R . . C21 C -0.2264(3) 0.32750(15) 0.9141(2) 0.0527(11) Uani 1 1 d . . . H21 H -0.2581 0.3190 0.9514 0.063 Uiso 1 1 calc R . . C22 C -0.1287(3) 0.32403(13) 0.9157(2) 0.0440(9) Uani 1 1 d . . . C23 C -0.0830(2) 0.33648(12) 0.85859(19) 0.0391(9) Uani 1 1 d . . . C24 C -0.0729(3) 0.30889(14) 0.9702(2) 0.0500(10) Uani 1 1 d . . . H24 H -0.1005 0.2999 1.0090 0.060 Uiso 1 1 calc R . . C25 C 0.0203(3) 0.30696(14) 0.9680(2) 0.0483(10) Uani 1 1 d . . . H25 H 0.0578 0.2968 1.0053 0.058 Uiso 1 1 calc R . . C26 C 0.0620(3) 0.32000(13) 0.9107(2) 0.0426(9) Uani 1 1 d . . . C27 C 0.1628(3) 0.31864(14) 0.9078(2) 0.0484(10) Uani 1 1 d . . . H27 H 0.1867 0.3207 0.8661 0.058 Uiso 1 1 calc R . . C28 C 0.2229(3) 0.31478(16) 0.9592(2) 0.0580(11) Uani 1 1 d . . . H28 H 0.1968 0.3115 1.0001 0.070 Uiso 1 1 calc R . . C29 C 0.3239(3) 0.31487(17) 0.9616(2) 0.0598(12) Uani 1 1 d . . . C30 C 0.3766(3) 0.3006(2) 0.9121(3) 0.0826(17) Uani 1 1 d . . . C31 C 0.4722(4) 0.3010(2) 0.9164(4) 0.109(2) Uani 1 1 d . . . H31 H 0.5055 0.2900 0.8811 0.131 Uiso 1 1 calc R . . C32 C 0.5175(4) 0.3173(3) 0.9722(5) 0.123(3) Uani 1 1 d . . . H32 H 0.5832 0.3191 0.9751 0.148 Uiso 1 1 calc R . . C33 C 0.4698(4) 0.3313(2) 1.0244(4) 0.105(2) Uani 1 1 d . . . H33 H 0.5013 0.3422 1.0639 0.126 Uiso 1 1 calc R . . C34 C 0.3746(3) 0.32902(19) 1.0174(3) 0.0727(14) Uani 1 1 d . . . C35 C -0.3064(3) 0.37527(15) 0.6287(2) 0.0522(11) Uani 1 1 d . . . C36 C -0.4015(3) 0.37169(17) 0.6352(2) 0.0638(13) Uani 1 1 d . . . H36 H -0.4277 0.3876 0.6705 0.077 Uiso 1 1 calc R . . C37 C -0.4585(3) 0.34521(19) 0.5907(3) 0.0756(16) Uani 1 1 d . . . H37 H -0.5230 0.3436 0.5964 0.091 Uiso 1 1 calc R . . C38 C -0.4241(3) 0.32126(19) 0.5390(3) 0.0780(15) Uani 1 1 d . . . H38 H -0.4644 0.3035 0.5091 0.094 Uiso 1 1 calc R . . C39 C -0.3293(3) 0.32333(17) 0.5310(3) 0.0649(13) Uani 1 1 d . . . C40 C -0.2701(3) 0.34913(14) 0.5766(2) 0.0498(10) Uani 1 1 d . . . C41 C -0.2870(4) 0.30122(18) 0.4789(3) 0.0798(16) Uani 1 1 d . . . H41 H -0.3237 0.2841 0.4463 0.096 Uiso 1 1 calc R . . C42 C -0.1945(3) 0.30425(18) 0.4751(3) 0.0727(14) Uani 1 1 d . . . H42 H -0.1669 0.2899 0.4392 0.087 Uiso 1 1 calc R . . C43 C -0.1379(3) 0.32865(15) 0.5241(2) 0.0543(11) Uani 1 1 d . . . C44 C -0.0372(3) 0.32954(14) 0.5231(2) 0.0540(11) Uani 1 1 d . . . H44 H -0.0024 0.3404 0.5612 0.065 Uiso 1 1 calc R . . C45 C 0.0094(3) 0.31614(15) 0.4724(2) 0.0550(11) Uani 1 1 d . . . H45 H -0.0272 0.3053 0.4350 0.066 Uiso 1 1 calc R . . C46 C 0.1094(3) 0.31599(15) 0.4669(2) 0.0553(11) Uani 1 1 d . . . C47 C 0.1468(4) 0.31332(19) 0.4070(3) 0.0784(15) Uani 1 1 d . . . C48 C 0.2387(5) 0.3145(2) 0.3982(4) 0.102(2) Uani 1 1 d . . . H48 H 0.2604 0.3129 0.3557 0.122 Uiso 1 1 calc R . . C49 C 0.2993(4) 0.3182(3) 0.4523(4) 0.112(2) Uani 1 1 d . . . H49 H 0.3639 0.3202 0.4473 0.134 Uiso 1 1 calc R . . C50 C 0.2683(4) 0.3191(2) 0.5129(3) 0.0959(19) Uani 1 1 d . . . H50 H 0.3105 0.3205 0.5504 0.115 Uiso 1 1 calc R . . C51 C 0.1753(4) 0.31795(18) 0.5190(3) 0.0708(14) Uani 1 1 d . . . C52 C 0.0635(2) 0.42530(14) 0.63408(17) 0.0397(9) Uani 1 1 d . . . C53 C 0.1586(3) 0.42602(15) 0.6300(2) 0.0497(10) Uani 1 1 d . . . H53 H 0.1942 0.3987 0.6450 0.060 Uiso 1 1 calc R . . C54 C 0.2035(3) 0.46626(17) 0.6042(2) 0.0582(12) Uani 1 1 d . . . H54 H 0.2688 0.4655 0.6021 0.070 Uiso 1 1 calc R . . C55 C 0.1556(3) 0.50608(16) 0.5823(2) 0.0565(11) Uani 1 1 d . . . H55 H 0.1874 0.5330 0.5654 0.068 Uiso 1 1 calc R . . C56 C 0.0593(3) 0.50749(14) 0.58438(19) 0.0464(10) Uani 1 1 d . . . C57 C 0.0119(2) 0.46707(14) 0.60966(18) 0.0408(9) Uani 1 1 d . . . C58 C 0.0031(3) 0.54674(15) 0.5620(2) 0.0568(11) Uani 1 1 d . . . H58 H 0.0307 0.5745 0.5439 0.068 Uiso 1 1 calc R . . C59 C -0.0894(3) 0.54543(15) 0.5661(2) 0.0565(11) Uani 1 1 d . . . H59 H -0.1260 0.5725 0.5515 0.068 Uiso 1 1 calc R . . C60 C -0.1323(3) 0.50419(14) 0.5917(2) 0.0476(10) Uani 1 1 d . . . C61 C -0.2324(3) 0.50195(15) 0.5991(2) 0.0532(11) Uani 1 1 d . . . H61 H -0.2553 0.4767 0.6251 0.064 Uiso 1 1 calc R . . C62 C -0.2925(3) 0.53372(15) 0.5709(2) 0.0545(11) Uani 1 1 d . . . H62 H -0.2676 0.5583 0.5448 0.065 Uiso 1 1 calc R . . C63 C -0.3932(3) 0.53472(14) 0.5761(2) 0.0524(11) Uani 1 1 d . . . C64 C -0.4495(3) 0.55817(15) 0.5289(3) 0.0628(13) Uani 1 1 d . . . C65 C -0.5437(3) 0.56144(16) 0.5307(3) 0.0694(14) Uani 1 1 d . . . H65 H -0.5793 0.5783 0.4973 0.083 Uiso 1 1 calc R . . C66 C -0.5858(3) 0.54062(17) 0.5804(3) 0.0746(15) Uani 1 1 d . . . H66 H -0.6513 0.5420 0.5812 0.089 Uiso 1 1 calc R . . C67 C -0.5330(3) 0.51711(17) 0.6305(3) 0.0731(14) Uani 1 1 d . . . H67 H -0.5618 0.5030 0.6661 0.088 Uiso 1 1 calc R . . C68 C -0.4399(3) 0.51480(16) 0.6272(2) 0.0593(12) Uani 1 1 d . . . C69 C 0.3881(3) 0.45097(14) 0.8093(3) 0.0593(12) Uani 1 1 d . . . C70 C 0.4834(3) 0.44808(17) 0.8012(3) 0.0795(16) Uani 1 1 d . . . H70 H 0.5045 0.4475 0.7585 0.095 Uiso 1 1 calc R . . C71 C 0.5485(4) 0.4460(2) 0.8558(4) 0.095(2) Uani 1 1 d . . . H71 H 0.6126 0.4437 0.8489 0.114 Uiso 1 1 calc R . . C72 C 0.5221(4) 0.4471(2) 0.9171(4) 0.0917(19) Uani 1 1 d . . . H72 H 0.5673 0.4470 0.9529 0.110 Uiso 1 1 calc R . . C73 C 0.4271(4) 0.44832(18) 0.9280(3) 0.0738(15) Uani 1 1 d . . . C74 C 0.3605(3) 0.44950(14) 0.8749(3) 0.0580(12) Uani 1 1 d . . . C75 C 0.3938(5) 0.44942(19) 0.9904(4) 0.097(2) Uani 1 1 d . . . H75 H 0.4361 0.4503 1.0278 0.116 Uiso 1 1 calc R . . C76 C 0.3008(4) 0.44917(19) 0.9974(3) 0.0818(16) Uani 1 1 d . . . H76 H 0.2785 0.4498 1.0397 0.098 Uiso 1 1 calc R . . C77 C 0.2365(3) 0.44803(15) 0.9410(2) 0.0571(11) Uani 1 1 d . . . C78 C 0.1372(3) 0.44452(15) 0.9474(2) 0.0591(12) Uani 1 1 d . . . H78 H 0.0974 0.4492 0.9091 0.071 Uiso 1 1 calc R . . C79 C 0.0977(4) 0.43522(15) 1.0029(2) 0.0675(13) Uani 1 1 d . . . H79A H 0.1411 0.4295 1.0397 0.081 Uiso 1 1 d R . . C80A C -0.0030(12) 0.4298(9) 1.0125(9) 0.069(2) Uani 0.50 1 d PU . . C81A C -0.0415(9) 0.4119(6) 1.0691(7) 0.076(2) Uani 0.50 1 d PU . . C82A C -0.1299(10) 0.4083(6) 1.0823(6) 0.078(3) Uani 0.50 1 d PU . . H82A H -0.1456 0.3943 1.1228 0.094 Uiso 0.50 1 d PR . . C83 C -0.1748(7) 0.4181(5) 1.0582(5) 0.078(2) Uani 0.50 1 d PGU . . H83A H -0.2362 0.4137 1.0721 0.094 Uiso 0.50 1 d PR . . C82 C -0.0980(8) 0.4076(5) 1.1003(5) 0.079(2) Uani 0.50 1 d PGU . . H82B H -0.1061 0.3958 1.1435 0.095 Uiso 0.50 1 d PR . . C81 C -0.0094(7) 0.4143(7) 1.0799(8) 0.0799(19) Uani 0.50 1 d PGU . . C80 C 0.0024(10) 0.4314(9) 1.0174(9) 0.0728(19) Uani 0.50 1 d PGU . . C85 C -0.0744(13) 0.4418(9) 0.9753(7) 0.0729(16) Uani 0.50 1 d PGU . . C84 C -0.1631(11) 0.4352(6) 0.9957(5) 0.074(2) Uani 0.50 1 d PGU . . H84A H -0.2162 0.4424 0.9666 0.089 Uiso 0.50 1 d PR . . C83A C -0.1966(10) 0.4238(6) 1.0352(6) 0.080(3) Uani 0.50 1 d PU . . H83B H -0.2607 0.4216 1.0441 0.096 Uiso 0.50 1 d PR . . C84A C -0.1697(12) 0.4428(6) 0.9773(7) 0.072(2) Uani 0.50 1 d PU . . H84B H -0.2132 0.4540 0.9432 0.087 Uiso 0.50 1 d PR . . C85A C -0.0755(14) 0.4442(9) 0.9713(8) 0.0698(18) Uani 0.50 1 d PU . . C86 C 0.0080(3) 0.47449(14) 0.77596(19) 0.0424(9) Uani 1 1 d U . . C87 C -0.0877(3) 0.47332(15) 0.7765(2) 0.0509(10) Uani 1 1 d . . . H87 H -0.1169 0.4443 0.7895 0.061 Uiso 1 1 d R . . C88 C -0.1408(3) 0.51401(17) 0.7588(2) 0.0605(12) Uani 1 1 d . . . H88 H -0.2062 0.5120 0.7603 0.073 Uiso 1 1 calc R . . C89 C -0.1037(3) 0.55609(17) 0.7395(2) 0.0664(13) Uani 1 1 d . . . H89 H -0.1423 0.5829 0.7268 0.080 Uiso 1 1 calc R . . C90 C -0.0064(3) 0.55992(14) 0.7383(2) 0.0542(11) Uani 1 1 d . . . C91 C 0.0496(3) 0.51961(14) 0.75836(19) 0.0439(9) Uani 1 1 d . . . C92 C 0.0396(4) 0.60196(16) 0.7199(3) 0.0722(14) Uani 1 1 d . . . H92 H 0.0049 0.6297 0.7050 0.087 Uiso 1 1 calc R . . C93 C 0.1334(3) 0.60347(16) 0.7232(2) 0.0686(13) Uani 1 1 d . . . H93 H 0.1639 0.6321 0.7101 0.082 Uiso 1 1 calc R . . C94 C 0.1866(3) 0.56264(14) 0.7458(2) 0.0521(11) Uani 1 1 d . . . C95 C 0.2860(3) 0.56490(14) 0.7559(2) 0.0589(12) Uani 1 1 d . . . H95 H 0.3159 0.5379 0.7774 0.071 Uiso 1 1 calc R . . C96 C 0.3400(3) 0.60092(16) 0.7382(2) 0.0699(14) Uani 1 1 d . . . H96A H 0.3074 0.6276 0.7169 0.084 Uiso 1 1 d R . . C97 C 0.4374(6) 0.6057(8) 0.7457(8) 0.076(2) Uani 0.50 1 d PGU . . C102 C 0.4776(7) 0.6319(6) 0.6972(7) 0.088(2) Uani 0.50 1 d PGU . . C101 C 0.5730(7) 0.6389(4) 0.7007(5) 0.090(2) Uani 0.50 1 d PGU . . H10A H 0.6008 0.6570 0.6672 0.108 Uiso 0.50 1 d PR . . C100 C 0.6280(6) 0.6198(4) 0.7527(5) 0.089(2) Uani 0.50 1 d PGU . . H10B H 0.6938 0.6246 0.7552 0.107 Uiso 0.50 1 d PR . . C99 C 0.5877(8) 0.5936(4) 0.8012(5) 0.087(2) Uani 0.50 1 d PGU . . H99A H 0.6258 0.5804 0.8371 0.104 Uiso 0.50 1 d PR . . C98 C 0.4924(8) 0.5866(6) 0.7977(7) 0.0803(18) Uani 0.50 1 d PGU . . F1 F -0.18223(19) 0.23133(10) 0.81230(14) 0.0779(8) Uani 1 1 d . . . F2 F -0.2483(2) 0.21297(14) 0.58706(16) 0.1111(11) Uani 1 1 d . . . F3 F 0.3281(2) 0.34349(12) 1.06880(16) 0.0950(10) Uani 1 1 d . . . F4 F 0.3325(2) 0.28251(13) 0.85648(17) 0.1045(11) Uani 1 1 d . . . F5 F 0.1454(2) 0.31702(13) 0.57959(15) 0.0969(10) Uani 1 1 d . . . F6 F 0.0847(2) 0.30821(14) 0.35366(16) 0.1121(12) Uani 1 1 d . . . F7 F -0.38890(17) 0.49305(11) 0.67656(14) 0.0827(8) Uani 1 1 d . . . F8 F -0.40846(17) 0.57814(11) 0.47786(15) 0.0835(9) Uani 1 1 d . . . F9 F 0.0259(7) 0.3922(4) 1.1134(6) 0.091(2) Uani 0.50 1 d PU . . F9A F 0.0610(7) 0.4048(4) 1.1227(5) 0.092(2) Uani 0.50 1 d PU . . F10 F -0.0600(10) 0.4530(3) 0.9117(7) 0.076(2) Uani 0.50 1 d PU . . F10A F -0.0572(10) 0.4702(3) 0.9174(7) 0.072(2) Uani 0.50 1 d PU . . F11 F 0.4388(10) 0.5722(4) 0.8546(8) 0.090(2) Uani 0.50 1 d PU . . F11A F 0.4511(9) 0.5566(4) 0.8471(8) 0.084(2) Uani 0.50 1 d PU . . F12 F 0.4272(6) 0.6521(5) 0.6457(7) 0.096(2) Uani 0.50 1 d PU . . F12A F 0.4639(6) 0.6462(5) 0.6602(7) 0.101(3) Uani 0.50 1 d PU . . N1 N 0.09824(19) 0.29060(11) 0.72733(15) 0.0404(7) Uani 1 1 d . . . N2 N 0.01091(19) 0.33427(10) 0.85696(16) 0.0392(7) Uani 1 1 d . . . N3 N -0.1755(2) 0.35079(11) 0.57256(16) 0.0467(8) Uani 1 1 d . . . N4 N -0.08155(19) 0.46556(11) 0.61301(15) 0.0392(7) Uani 1 1 d . . . N5 N 0.2672(2) 0.44896(11) 0.88250(18) 0.0506(8) Uani 1 1 d . . . N6 N 0.1439(2) 0.52103(11) 0.76114(15) 0.0448(8) Uani 1 1 d . . . O1 O 0.18689(15) 0.37227(8) 0.76641(13) 0.0422(6) Uani 1 1 d . . . O2 O -0.09089(15) 0.36028(9) 0.74730(13) 0.0432(6) Uani 1 1 d . . . O3 O -0.25117(17) 0.40145(10) 0.66795(14) 0.0523(7) Uani 1 1 d . . . O4 O 0.01854(15) 0.38844(9) 0.65952(12) 0.0411(6) Uani 1 1 d . . . O5 O 0.32608(18) 0.45413(10) 0.75988(15) 0.0562(7) Uani 1 1 d . . . O6 O 0.06304(16) 0.43682(8) 0.79145(13) 0.0416(6) Uani 1 1 d . . . Zn1 Zn 0.04818(3) 0.361418(15) 0.76025(2) 0.03880(12) Uani 1 1 d . . . Zn2 Zn 0.19919(3) 0.448176(16) 0.78753(2) 0.04392(13) Uani 1 1 d . . . Zn3 Zn -0.11919(3) 0.395626(16) 0.65397(2) 0.04299(13) 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 C1 0.034(2) 0.044(2) 0.047(2) 0.0037(18) 0.0103(17) 0.0063(16) C1A 0.072(4) 0.058(4) 0.089(5) -0.015(4) 0.045(4) -0.021(4) C2A 0.076(4) 0.073(5) 0.094(5) -0.003(4) 0.024(4) -0.020(4) C3A 0.073(5) 0.090(6) 0.101(6) 0.003(5) 0.023(5) -0.020(5) C4A 0.074(5) 0.077(6) 0.105(6) 0.001(5) 0.015(5) -0.029(4) C5A 0.079(4) 0.079(6) 0.101(6) -0.004(5) 0.013(5) -0.030(4) C6A 0.076(4) 0.073(5) 0.093(5) -0.012(4) 0.016(4) -0.019(4) C2 0.039(2) 0.051(3) 0.076(3) 0.003(2) 0.012(2) 0.0023(18) C3 0.049(3) 0.070(3) 0.090(4) 0.003(3) 0.029(2) 0.013(2) C4 0.047(3) 0.067(3) 0.087(4) -0.009(3) 0.023(2) 0.019(2) C5 0.051(3) 0.053(3) 0.062(3) -0.005(2) 0.016(2) 0.0107(19) C6 0.042(2) 0.046(2) 0.044(2) 0.0009(18) 0.0122(18) 0.0039(16) C7 0.074(3) 0.058(3) 0.091(4) -0.022(3) 0.028(3) 0.013(2) C8 0.060(3) 0.049(3) 0.096(4) -0.021(3) 0.018(3) 0.000(2) C9 0.049(2) 0.045(2) 0.055(3) -0.003(2) 0.013(2) 0.0003(18) C10 0.051(2) 0.038(2) 0.075(3) -0.010(2) 0.011(2) -0.0039(18) C11 0.062(3) 0.056(3) 0.053(3) -0.006(2) 0.006(2) -0.003(2) C12 0.050(3) 0.042(2) 0.063(3) 0.004(2) -0.003(2) -0.0083(18) C13 0.072(4) 0.068(3) 0.075(4) 0.004(3) -0.012(3) -0.003(2) C14 0.066(4) 0.080(4) 0.127(6) 0.011(4) -0.033(4) -0.001(3) C15 0.046(3) 0.062(3) 0.158(7) 0.010(4) -0.004(4) 0.004(2) C16 0.061(3) 0.063(3) 0.112(5) -0.001(3) 0.030(3) 0.001(2) C17 0.058(3) 0.049(3) 0.066(3) 0.001(2) 0.000(3) -0.008(2) C18 0.038(2) 0.037(2) 0.051(3) 0.0033(18) 0.0148(18) -0.0053(15) C19 0.034(2) 0.065(3) 0.062(3) 0.010(2) 0.008(2) 0.0012(18) C20 0.035(2) 0.067(3) 0.070(3) 0.009(2) 0.023(2) 0.0006(19) C21 0.047(2) 0.057(3) 0.057(3) 0.007(2) 0.021(2) 0.0005(19) C22 0.046(2) 0.039(2) 0.049(3) -0.0020(19) 0.0171(19) -0.0027(16) C23 0.038(2) 0.032(2) 0.049(3) 0.0011(17) 0.0109(18) -0.0011(15) C24 0.054(3) 0.050(2) 0.048(3) 0.005(2) 0.014(2) -0.0044(19) C25 0.054(2) 0.049(2) 0.042(2) 0.0084(19) 0.0062(19) -0.0035(18) C26 0.051(2) 0.033(2) 0.045(3) -0.0015(18) 0.011(2) -0.0024(16) C27 0.046(2) 0.047(2) 0.053(3) 0.007(2) 0.012(2) 0.0033(17) C28 0.049(3) 0.076(3) 0.049(3) 0.013(2) 0.006(2) 0.001(2) C29 0.048(3) 0.070(3) 0.061(3) 0.024(2) 0.003(2) 0.002(2) C30 0.058(3) 0.115(5) 0.076(4) 0.033(3) 0.014(3) 0.019(3) C31 0.059(4) 0.139(6) 0.135(7) 0.043(5) 0.036(4) 0.018(4) C32 0.046(4) 0.159(7) 0.164(8) 0.053(6) -0.001(4) 0.001(4) C33 0.061(4) 0.122(5) 0.126(6) 0.046(4) -0.032(4) -0.017(3) C34 0.060(3) 0.079(4) 0.078(4) 0.031(3) -0.009(3) -0.004(2) C35 0.035(2) 0.062(3) 0.060(3) 0.021(2) 0.000(2) -0.0031(18) C36 0.042(2) 0.075(3) 0.074(3) 0.027(3) 0.005(2) 0.000(2) C37 0.036(2) 0.089(4) 0.100(5) 0.032(3) -0.008(3) -0.010(2) C38 0.045(3) 0.087(4) 0.098(5) 0.013(3) -0.018(3) -0.013(2) C39 0.060(3) 0.060(3) 0.072(4) 0.010(3) -0.013(3) -0.001(2) C40 0.036(2) 0.051(2) 0.062(3) 0.008(2) -0.003(2) -0.0011(17) C41 0.074(4) 0.074(4) 0.086(4) -0.019(3) -0.027(3) -0.001(3) C42 0.069(3) 0.077(3) 0.070(4) -0.014(3) -0.012(3) 0.008(3) C43 0.059(3) 0.053(3) 0.050(3) 0.004(2) 0.000(2) 0.003(2) C44 0.061(3) 0.046(2) 0.055(3) -0.005(2) 0.005(2) 0.0039(19) C45 0.064(3) 0.054(3) 0.047(3) 0.001(2) 0.005(2) 0.006(2) C46 0.066(3) 0.047(3) 0.054(3) 0.005(2) 0.014(2) 0.008(2) C47 0.085(4) 0.089(4) 0.064(4) 0.018(3) 0.024(3) 0.020(3) C48 0.098(5) 0.106(5) 0.108(6) 0.023(4) 0.053(4) 0.009(4) C49 0.068(4) 0.133(6) 0.139(7) 0.010(5) 0.033(5) -0.006(4) C50 0.067(4) 0.115(5) 0.105(5) -0.013(4) 0.002(4) -0.003(3) C51 0.071(3) 0.073(3) 0.071(4) -0.008(3) 0.017(3) 0.005(2) C52 0.037(2) 0.052(2) 0.030(2) 0.0035(18) 0.0064(16) -0.0007(16) C53 0.039(2) 0.058(3) 0.054(3) 0.013(2) 0.0122(19) 0.0022(18) C54 0.034(2) 0.082(3) 0.060(3) 0.012(2) 0.011(2) -0.005(2) C55 0.044(2) 0.066(3) 0.060(3) 0.015(2) 0.008(2) -0.014(2) C56 0.047(2) 0.048(2) 0.044(2) 0.0031(19) 0.0047(19) -0.0070(18) C57 0.036(2) 0.049(2) 0.038(2) 0.0010(18) 0.0057(17) -0.0016(16) C58 0.059(3) 0.049(3) 0.064(3) 0.017(2) 0.009(2) -0.003(2) C59 0.055(3) 0.046(3) 0.068(3) 0.011(2) 0.001(2) 0.0020(19) C60 0.048(2) 0.050(2) 0.045(3) 0.005(2) 0.0067(19) 0.0059(18) C61 0.049(2) 0.047(2) 0.063(3) 0.004(2) 0.005(2) 0.0031(18) C62 0.048(2) 0.055(3) 0.061(3) 0.006(2) 0.008(2) 0.0045(19) C63 0.044(2) 0.044(2) 0.069(3) -0.001(2) 0.005(2) 0.0076(18) C64 0.053(3) 0.050(3) 0.086(4) 0.006(3) 0.004(3) 0.007(2) C65 0.041(3) 0.060(3) 0.106(4) 0.010(3) -0.005(3) 0.005(2) C66 0.042(3) 0.060(3) 0.120(5) -0.001(3) 0.001(3) 0.001(2) C67 0.064(3) 0.069(3) 0.088(4) 0.004(3) 0.021(3) 0.008(2) C68 0.045(2) 0.066(3) 0.066(3) -0.002(2) 0.005(2) 0.014(2) C69 0.050(3) 0.039(2) 0.089(4) 0.002(2) 0.008(3) -0.0041(18) C70 0.041(3) 0.073(3) 0.124(5) 0.011(3) 0.005(3) 0.000(2) C71 0.047(3) 0.082(4) 0.154(7) 0.005(4) -0.011(4) -0.001(3) C72 0.059(4) 0.080(4) 0.130(6) -0.002(4) -0.035(4) -0.004(3) C73 0.072(4) 0.062(3) 0.082(4) 0.000(3) -0.027(3) -0.001(2) C74 0.049(3) 0.040(2) 0.082(4) 0.003(2) -0.014(2) -0.0023(18) C75 0.105(5) 0.074(4) 0.102(5) -0.002(3) -0.052(4) 0.000(3) C76 0.097(4) 0.086(4) 0.060(4) -0.008(3) -0.016(3) -0.005(3) C77 0.074(3) 0.044(3) 0.052(3) -0.002(2) -0.008(2) 0.003(2) C78 0.083(3) 0.051(3) 0.043(3) -0.002(2) 0.001(2) 0.005(2) C79 0.102(4) 0.050(3) 0.051(3) -0.002(2) 0.007(3) 0.007(2) C80A 0.113(5) 0.049(4) 0.046(4) -0.005(4) 0.024(4) -0.006(4) C81A 0.112(5) 0.070(4) 0.049(4) 0.001(4) 0.023(4) -0.005(4) C82A 0.110(6) 0.078(4) 0.050(5) 0.001(4) 0.028(5) -0.003(5) C83 0.111(5) 0.073(4) 0.053(5) -0.002(4) 0.028(4) -0.009(4) C82 0.113(5) 0.074(3) 0.053(4) -0.001(4) 0.027(4) -0.011(4) C81 0.117(4) 0.072(3) 0.053(4) 0.003(3) 0.022(4) -0.011(3) C80 0.112(4) 0.058(3) 0.051(4) -0.004(3) 0.023(3) -0.008(3) C85 0.105(3) 0.061(3) 0.056(3) -0.007(3) 0.025(3) -0.010(3) C84 0.106(4) 0.065(4) 0.055(4) -0.005(4) 0.029(4) -0.010(3) C83A 0.110(5) 0.074(5) 0.058(6) -0.004(5) 0.022(5) -0.008(4) C84A 0.102(5) 0.063(5) 0.056(5) -0.004(4) 0.028(5) -0.005(4) C85A 0.100(4) 0.057(4) 0.056(4) -0.009(3) 0.031(3) -0.012(3) C86 0.042(2) 0.045(2) 0.040(2) -0.0055(17) 0.0055(17) 0.0034(16) C87 0.046(2) 0.055(3) 0.052(3) -0.010(2) 0.008(2) 0.0053(19) C88 0.044(2) 0.070(3) 0.068(3) -0.008(3) 0.005(2) 0.013(2) C89 0.061(3) 0.060(3) 0.077(4) -0.002(3) -0.003(2) 0.021(2) C90 0.067(3) 0.040(2) 0.056(3) -0.003(2) 0.002(2) 0.011(2) C91 0.049(2) 0.044(2) 0.039(2) 0.0000(18) 0.0061(18) 0.0023(17) C92 0.086(4) 0.047(3) 0.083(4) 0.012(3) 0.004(3) 0.017(2) C93 0.081(4) 0.042(3) 0.083(4) 0.009(2) 0.011(3) 0.000(2) C94 0.065(3) 0.041(2) 0.051(3) 0.001(2) 0.011(2) -0.0022(19) C95 0.068(3) 0.036(2) 0.073(3) 0.001(2) 0.012(2) -0.0055(19) C96 0.086(4) 0.042(3) 0.084(4) 0.006(2) 0.024(3) -0.007(2) C97 0.073(3) 0.068(4) 0.091(4) -0.012(4) 0.028(3) -0.019(3) C102 0.082(4) 0.084(4) 0.099(5) -0.003(3) 0.026(4) -0.017(4) C101 0.081(4) 0.091(5) 0.101(5) -0.001(4) 0.024(4) -0.020(4) C100 0.077(4) 0.091(5) 0.100(5) 0.000(4) 0.019(4) -0.026(4) C99 0.081(3) 0.082(5) 0.098(5) -0.005(4) 0.016(4) -0.026(4) C98 0.077(3) 0.073(4) 0.093(4) -0.007(3) 0.021(3) -0.022(3) F1 0.0774(19) 0.094(2) 0.0633(19) -0.0081(15) 0.0090(15) -0.0113(15) F2 0.117(3) 0.148(3) 0.064(2) -0.010(2) -0.016(2) -0.006(2) F3 0.086(2) 0.125(3) 0.072(2) 0.0109(19) -0.0118(18) -0.0166(18) F4 0.086(2) 0.154(3) 0.076(2) 0.013(2) 0.0259(19) 0.036(2) F5 0.080(2) 0.147(3) 0.063(2) -0.0099(19) 0.0026(16) 0.0240(18) F6 0.121(3) 0.159(3) 0.057(2) 0.012(2) 0.015(2) 0.045(2) F7 0.0606(17) 0.118(2) 0.071(2) 0.0253(17) 0.0171(14) 0.0213(15) F8 0.0592(17) 0.092(2) 0.099(2) 0.0398(18) 0.0050(16) 0.0088(14) F9 0.127(5) 0.087(4) 0.062(4) 0.012(4) 0.014(4) -0.015(4) F9A 0.136(6) 0.091(5) 0.051(4) 0.009(4) 0.011(4) -0.036(4) F10 0.103(3) 0.067(4) 0.060(3) -0.005(4) 0.015(3) -0.009(4) F10A 0.101(4) 0.057(5) 0.061(4) -0.009(4) 0.016(3) -0.007(4) F11 0.089(4) 0.086(5) 0.097(4) -0.008(4) 0.013(3) -0.014(4) F11A 0.087(4) 0.065(5) 0.101(5) -0.010(4) 0.007(4) -0.005(4) F12 0.085(5) 0.101(4) 0.103(5) 0.014(4) 0.025(4) -0.013(5) F12A 0.092(6) 0.106(5) 0.106(6) 0.029(4) 0.029(5) -0.024(5) N1 0.0352(17) 0.0402(18) 0.047(2) 0.0003(15) 0.0089(14) 0.0013(13) N2 0.0351(17) 0.0350(17) 0.048(2) -0.0008(15) 0.0098(15) -0.0008(12) N3 0.0453(19) 0.0450(19) 0.049(2) 0.0074(16) 0.0019(16) 0.0022(14) N4 0.0350(17) 0.0439(18) 0.0391(19) 0.0044(15) 0.0053(14) 0.0008(13) N5 0.062(2) 0.0384(19) 0.050(2) -0.0013(16) -0.0066(18) 0.0008(15) N6 0.052(2) 0.0387(19) 0.045(2) -0.0024(15) 0.0109(16) -0.0002(14) O1 0.0351(13) 0.0390(14) 0.0532(17) 0.0013(12) 0.0086(12) 0.0026(10) O2 0.0319(13) 0.0501(16) 0.0484(17) 0.0066(13) 0.0085(12) 0.0005(11) O3 0.0334(14) 0.0684(19) 0.0555(19) 0.0050(15) 0.0066(13) 0.0004(12) O4 0.0362(14) 0.0455(15) 0.0421(16) 0.0060(12) 0.0075(11) -0.0009(11) O5 0.0418(16) 0.0563(18) 0.070(2) 0.0092(15) 0.0038(15) -0.0057(12) O6 0.0372(14) 0.0391(15) 0.0491(17) -0.0002(12) 0.0064(12) 0.0000(11) Zn1 0.0301(2) 0.0398(2) 0.0474(3) 0.0012(2) 0.00836(18) 0.00021(17) Zn2 0.0380(2) 0.0426(3) 0.0513(3) 0.0034(2) 0.0043(2) -0.00305(18) Zn3 0.0329(2) 0.0488(3) 0.0475(3) 0.0026(2) 0.00405(19) -0.00063(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O1 1.337(4) . ? C1 C2 1.380(5) . ? C1 C6 1.429(5) . ? C1A C98 1.14(2) . ? C1A C2A 1.3900 . ? C1A C6A 1.3900 . ? C1A C102 1.53(2) . ? C1A C96 1.567(9) . ? C2A C101 1.129(19) . ? C2A F12A 1.290(12) . ? C2A C97 1.33(2) . ? C2A C3A 1.3900 . ? C2A F12 1.827(15) . ? C2A C100 1.961(14) . ? C3A C101 0.690(12) . ? C3A C100 0.755(15) . ? C3A C4A 1.3900 . ? C3A C102 1.795(15) . ? C3A C99 1.847(12) . ? C3A H3AA 0.9601 . ? C3A H10A 1.4509 . ? C3A H10B 1.5045 . ? C4A C100 0.737(11) . ? C4A C99 0.947(17) . ? C4A C5A 1.3900 . ? C4A H4AA 0.9601 . ? C4A H10B 1.1522 . ? C4A H99A 1.3876 . ? C5A C99 0.588(12) . ? C5A C6A 1.3900 . ? C5A C98 1.39(2) . ? C5A C100 1.947(11) . ? C5A H5AA 0.9599 . ? C5A H99A 0.6764 . ? C6A F11A 1.147(16) . ? C6A F11 1.213(16) . ? C6A C99 1.519(17) . ? C6A C97 1.63(3) . ? C2 C3 1.385(6) . ? C2 H2 0.9500 . ? C3 C4 1.353(6) . ? C3 H3 0.9500 . ? C4 C5 1.411(5) . ? C4 H4 0.9500 . ? C5 C7 1.411(6) . ? C5 C6 1.422(5) . ? C6 N1 1.358(4) . ? C7 C8 1.366(6) . ? C7 H7 0.9500 . ? C8 C9 1.417(5) . ? C8 H8 0.9500 . ? C9 N1 1.323(5) . ? C9 C10 1.461(5) . ? C10 C11 1.318(5) . ? C10 H10 0.9500 . ? C11 C12 1.452(5) . ? C11 H11 0.9500 . ? C12 C13 1.385(6) . ? C12 C17 1.394(6) . ? C13 F2 1.353(6) . ? C13 C14 1.375(7) . ? C14 C15 1.354(8) . ? C14 H14 0.9500 . ? C15 C16 1.370(8) . ? C15 H15 0.9500 . ? C16 C17 1.362(6) . ? C16 H16 0.9500 . ? C17 F1 1.353(5) . ? C18 O2 1.336(4) . ? C18 C19 1.381(5) . ? C18 C23 1.433(5) . ? C19 C20 1.395(5) . ? C19 H19 0.9500 . ? C20 C21 1.347(6) . ? C20 H20 0.9500 . ? C21 C22 1.415(5) . ? C21 H21 0.9500 . ? C22 C24 1.397(5) . ? C22 C23 1.430(5) . ? C23 N2 1.364(4) . ? C24 C25 1.355(5) . ? C24 H24 0.9500 . ? C25 C26 1.408(5) . ? C25 H25 0.9500 . ? C26 N2 1.343(5) . ? C26 C27 1.464(5) . ? C27 C28 1.324(6) . ? C27 H27 0.9500 . ? C28 C29 1.459(5) . ? C28 H28 0.9500 . ? C29 C34 1.372(7) . ? C29 C30 1.373(7) . ? C30 F4 1.362(7) . ? C30 C31 1.380(7) . ? C31 C32 1.356(10) . ? C31 H31 0.9500 . ? C32 C33 1.372(10) . ? C32 H32 0.9500 . ? C33 C34 1.377(7) . ? C33 H33 0.9500 . ? C34 F3 1.353(6) . ? C35 O3 1.309(5) . ? C35 C36 1.396(5) . ? C35 C40 1.422(6) . ? C36 C37 1.391(7) . ? C36 H36 0.9500 . ? C37 C38 1.374(7) . ? C37 H37 0.9500 . ? C38 C39 1.395(6) . ? C38 H38 0.9500 . ? C39 C41 1.408(7) . ? C39 C40 1.414(6) . ? C40 N3 1.379(5) . ? C41 C42 1.350(6) . ? C41 H41 0.9500 . ? C42 C43 1.420(6) . ? C42 H42 0.9500 . ? C43 N3 1.318(5) . ? C43 C44 1.460(5) . ? C44 C45 1.332(5) . ? C44 H44 0.9500 . ? C45 C46 1.461(6) . ? C45 H45 0.9500 . ? C46 C47 1.382(6) . ? C46 C51 1.384(7) . ? C47 C48 1.356(7) . ? C47 F6 1.374(6) . ? C48 C49 1.371(9) . ? C48 H48 0.9500 . ? C49 C50 1.354(8) . ? C49 H49 0.9500 . ? C50 C51 1.361(7) . ? C50 H50 0.9500 . ? C51 F5 1.347(5) . ? C52 O4 1.331(4) . ? C52 C53 1.384(5) . ? C52 C57 1.439(5) . ? C53 C54 1.405(5) . ? C53 H53 0.9500 . ? C54 C55 1.354(6) . ? C54 H54 0.9500 . ? C55 C56 1.398(5) . ? C55 H55 0.9500 . ? C56 C58 1.407(5) . ? C56 C57 1.423(5) . ? C57 N4 1.359(4) . ? C58 C59 1.348(5) . ? C58 H58 0.9500 . ? C59 C60 1.412(5) . ? C59 H59 0.9500 . ? C60 N4 1.345(5) . ? C60 C61 1.468(5) . ? C61 C62 1.335(5) . ? C61 H61 0.9500 . ? C62 C63 1.468(5) . ? C62 H62 0.9500 . ? C63 C64 1.381(6) . ? C63 C68 1.401(6) . ? C64 F8 1.357(5) . ? C64 C65 1.370(6) . ? C65 C66 1.353(7) . ? C65 H65 0.9500 . ? C66 C67 1.395(7) . ? C66 H66 0.9500 . ? C67 C68 1.357(6) . ? C67 H67 0.9500 . ? C68 F7 1.350(5) . ? C69 O5 1.310(5) . ? C69 C70 1.404(6) . ? C69 C74 1.435(7) . ? C70 C71 1.414(8) . ? C70 H70 0.9500 . ? C71 C72 1.344(8) . ? C71 H71 0.9500 . ? C72 C73 1.410(7) . ? C72 H72 0.9500 . ? C73 C75 1.402(8) . ? C73 C74 1.404(6) . ? C74 N5 1.370(5) . ? C75 C76 1.365(8) . ? C75 H75 0.9500 . ? C76 C77 1.433(7) . ? C76 H76 0.9500 . ? C77 N5 1.312(5) . ? C77 C78 1.456(6) . ? C78 C79 1.338(6) . ? C78 H78 0.9500 . ? C79 C80 1.436(13) . ? C79 C80A 1.492(16) . ? C79 H79A 0.9601 . ? C80A C85 1.28(4) . ? C80A C85A 1.360(14) . ? C80A C81A 1.415(13) . ? C80A C81 1.46(3) . ? C81A C81 0.50(2) . ? C81A C82 1.08(2) . ? C81A C82A 1.331(15) . ? C81A C80 1.38(3) . ? C81A F9 1.395(16) . ? C81A F9A 1.795(18) . ? C81A C83 1.935(19) . ? C82A C82 0.571(16) . ? C82A C83 0.834(16) . ? C82A C83A 1.384(16) . ? C82A C81 1.76(2) . ? C82A C84 1.956(17) . ? C82A H82A 0.9601 . ? C82A H83A 1.5450 . ? C82A H82B 1.3249 . ? C83 C83A 0.571(16) . ? C83 C82 1.3900 . ? C83 C84 1.3900 . ? C83 C84A 1.802(19) . ? C83 H82A 1.5141 . ? C83 H83A 0.9601 . ? C83 H83B 1.2587 . ? C82 C81 1.3900 . ? C82 F9 1.844(17) . ? C82 C83A 1.937(18) . ? C82 H82A 0.9327 . ? C82 H82B 0.9600 . ? C81 F9 1.024(19) . ? C81 F9A 1.323(14) . ? C81 C80 1.3900 . ? C80 C85 1.3900 . ? C80 C85A 1.46(4) . ? C85 F10 1.373(18) . ? C85 C84A 1.38(3) . ? C85 C84 1.3900 . ? C85 F10A 1.459(18) . ? C84 C83A 1.02(2) . ? C84 C85A 1.42(3) . ? C84 H84A 0.9601 . ? C84 H84B 1.3591 . ? C83A C84A 1.381(15) . ? C83A H83A 1.0216 . ? C83A H84A 1.5081 . ? C83A H83B 0.9601 . ? C84A C85A 1.378(14) . ? C84A H84A 0.6929 . ? C84A H84B 0.9599 . ? C85A F10 1.284(19) . ? C85A F10A 1.359(18) . ? C86 O6 1.329(4) . ? C86 C87 1.388(5) . ? C86 C91 1.434(5) . ? C87 C88 1.390(6) . ? C87 H87 0.9500 . ? C88 C89 1.346(6) . ? C88 H88 0.9500 . ? C89 C90 1.414(6) . ? C89 H89 0.9500 . ? C90 C92 1.398(6) . ? C90 C91 1.415(5) . ? C91 N6 1.363(4) . ? C92 C93 1.355(6) . ? C92 H92 0.9500 . ? C93 C94 1.419(6) . ? C93 H93 0.9500 . ? C94 N6 1.347(5) . ? C94 C95 1.441(6) . ? C95 C96 1.327(5) . ? C95 H95 0.9500 . ? C96 C97 1.413(9) . ? C96 H96A 0.9598 . ? C97 C102 1.3900 . ? C97 C98 1.3900 . ? C102 F12A 0.867(18) . ? C102 F12 1.360(13) . ? C102 C101 1.3900 . ? C101 C100 1.3900 . ? C101 F12A 1.743(14) . ? C101 H3AA 0.9527 . ? C101 H10A 0.9600 . ? C100 C99 1.3900 . ? C100 H3AA 1.3849 . ? C100 H4AA 1.3686 . ? C100 H10B 0.9600 . ? C99 C98 1.3900 . ? C99 H5AA 1.4833 . ? C99 H99A 0.9599 . ? C98 F11A 1.467(19) . ? C98 F11 1.50(2) . ? F9 F9A 0.633(12) . ? F12 F12A 0.612(14) . ? N1 Zn1 2.198(3) . ? N2 Zn1 2.226(3) . ? N3 Zn3 2.187(3) . ? N4 Zn3 2.181(3) . ? N5 Zn2 2.123(3) . ? N6 Zn2 2.207(3) . ? O1 Zn1 2.025(2) . ? O1 Zn2 2.133(2) . ? O2 Zn1 2.012(2) . ? O2 Zn3 2.163(3) . ? O3 Zn3 1.959(2) . ? O4 Zn3 1.999(2) . ? O4 Zn1 2.213(2) . ? O5 Zn2 1.968(3) . ? O6 Zn2 2.003(2) . ? O6 Zn1 2.173(2) . ? 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 O1 C1 C2 124.7(3) . . ? O1 C1 C6 117.7(3) . . ? C2 C1 C6 117.7(3) . . ? C98 C1A C2A 110.1(7) . . ? C98 C1A C6A 10.0(7) . . ? C2A C1A C6A 120.0 . . ? C98 C1A C102 128.2(11) . . ? C2A C1A C102 18.2(6) . . ? C6A C1A C102 138.1(6) . . ? C98 C1A C96 131.4(11) . . ? C2A C1A C96 118.2(7) . . ? C6A C1A C96 121.5(8) . . ? C102 C1A C96 100.3(8) . . ? C101 C2A F12A 92.0(9) . . ? C101 C2A C97 157.4(16) . . ? F12A C2A C97 109.6(10) . . ? C101 C2A C1A 147.4(7) . . ? F12A C2A C1A 119.7(8) . . ? C97 C2A C1A 10.2(10) . . ? C101 C2A C3A 29.5(6) . . ? F12A C2A C3A 120.3(8) . . ? C97 C2A C3A 130.0(10) . . ? C1A C2A C3A 120.0 . . ? C101 C2A F12 102.8(10) . . ? F12A C2A F12 11.0(8) . . ? C97 C2A F12 98.6(8) . . ? C1A C2A F12 108.7(8) . . ? C3A C2A F12 131.3(8) . . ? C101 C2A C100 44.0(5) . . ? F12A C2A C100 135.9(9) . . ? C97 C2A C100 114.1(10) . . ? C1A C2A C100 104.0(4) . . ? C3A C2A C100 17.2(5) . . ? F12 C2A C100 146.6(9) . . ? C101 C3A C100 148(3) . . ? C101 C3A C4A 164(2) . . ? C100 C3A C4A 21.1(12) . . ? C101 C3A C2A 53.7(16) . . ? C100 C3A C2A 129.7(12) . . ? C4A C3A C2A 120.0 . . ? C101 C3A C102 44.5(10) . . ? C100 C3A C102 137.7(17) . . ? C4A C3A C102 129.3(8) . . ? C2A C3A C102 9.4(8) . . ? C101 C3A C99 138.5(18) . . ? C100 C3A C99 42.7(8) . . ? C4A C3A C99 30.0(6) . . ? C2A C3A C99 90.3(6) . . ? C102 C3A C99 99.5(7) . . ? C101 C3A H3AA 68.3 . . ? C100 C3A H3AA 107.1 . . ? C4A C3A H3AA 120.0 . . ? C2A C3A H3AA 120.0 . . ? C102 C3A H3AA 110.7 . . ? C99 C3A H3AA 149.3 . . ? C101 C3A H10A 34.0 . . ? C100 C3A H10A 133.7 . . ? C4A C3A H10A 152.0 . . ? C2A C3A H10A 86.8 . . ? C102 C3A H10A 77.4 . . ? C99 C3A H10A 166.3 . . ? H3AA C3A H10A 34.3 . . ? C101 C3A H10B 134.2 . . ? C100 C3A H10B 32.7 . . ? C4A C3A H10B 46.7 . . ? C2A C3A H10B 161.2 . . ? C102 C3A H10B 165.7 . . ? C99 C3A H10B 74.5 . . ? H3AA C3A H10B 74.9 . . ? H10A C3A H10B 105.3 . . ? C100 C4A C99 110.6(19) . . ? C100 C4A C3A 21.6(14) . . ? C99 C4A C3A 102.7(10) . . ? C100 C4A C5A 129.9(12) . . ? C99 C4A C5A 19.4(10) . . ? C3A C4A C5A 120.0 . . ? C100 C4A H4AA 106.8 . . ? C99 C4A H4AA 136.3 . . ? C3A C4A H4AA 120.0 . . ? C5A C4A H4AA 120.0 . . ? C100 C4A H10B 56.0 . . ? C99 C4A H10B 154.1 . . ? C3A C4A H10B 71.9 . . ? C5A C4A H10B 160.7 . . ? H4AA C4A H10B 50.8 . . ? C100 C4A H99A 147.2 . . ? C99 C4A H99A 43.7 . . ? C3A C4A H99A 146.3 . . ? C5A C4A H99A 28.2 . . ? H4AA C4A H99A 92.8 . . ? H10B C4A H99A 135.2 . . ? C99 C5A C4A 32(2) . . ? C99 C5A C6A 91.0(18) . . ? C4A C5A C6A 120.0 . . ? C99 C5A C98 78(2) . . ? C4A C5A C98 106.4(7) . . ? C6A C5A C98 13.6(7) . . ? C99 C5A C100 15.6(18) . . ? C4A C5A C100 16.9(5) . . ? C6A C5A C100 104.4(4) . . ? C98 C5A C100 90.7(7) . . ? C99 C5A H5AA 145.8 . . ? C4A C5A H5AA 120.0 . . ? C6A C5A H5AA 120.0 . . ? C98 C5A H5AA 133.6 . . ? C100 C5A H5AA 135.2 . . ? C99 C5A H99A 98.6 . . ? C4A C5A H99A 75.7 . . ? C6A C5A H99A 157.7 . . ? C98 C5A H99A 162.3 . . ? C100 C5A H99A 88.7 . . ? H5AA C5A H99A 47.3 . . ? F11A C6A F11 23.8(8) . . ? F11A C6A C5A 112.8(11) . . ? F11 C6A C5A 120.8(12) . . ? F11A C6A C1A 126.8(11) . . ? F11 C6A C1A 116.7(12) . . ? C5A C6A C1A 120.0 . . ? F11A C6A C99 135.3(14) . . ? F11 C6A C99 138.6(15) . . ? C5A C6A C99 22.8(5) . . ? C1A C6A C99 97.9(5) . . ? F11A C6A C97 125.1(11) . . ? F11 C6A C97 115.6(14) . . ? C5A C6A C97 121.5(6) . . ? C1A C6A C97 1.9(10) . . ? C99 C6A C97 99.5(9) . . ? C1 C2 C3 121.2(4) . . ? C1 C2 H2 119.4 . . ? C3 C2 H2 119.4 . . ? C4 C3 C2 122.8(4) . . ? C4 C3 H3 118.6 . . ? C2 C3 H3 118.6 . . ? C3 C4 C5 118.7(4) . . ? C3 C4 H4 120.6 . . ? C5 C4 H4 120.6 . . ? C7 C5 C4 124.3(4) . . ? C7 C5 C6 116.2(4) . . ? C4 C5 C6 119.5(4) . . ? N1 C6 C5 122.4(3) . . ? N1 C6 C1 117.5(3) . . ? C5 C6 C1 120.1(3) . . ? C8 C7 C5 120.9(4) . . ? C8 C7 H7 119.5 . . ? C5 C7 H7 119.5 . . ? C7 C8 C9 118.9(4) . . ? C7 C8 H8 120.5 . . ? C9 C8 H8 120.5 . . ? N1 C9 C8 121.8(4) . . ? N1 C9 C10 117.2(3) . . ? C8 C9 C10 121.0(4) . . ? C11 C10 C9 126.9(4) . . ? C11 C10 H10 116.5 . . ? C9 C10 H10 116.5 . . ? C10 C11 C12 124.2(4) . . ? C10 C11 H11 117.9 . . ? C12 C11 H11 117.9 . . ? C13 C12 C17 113.7(4) . . ? C13 C12 C11 121.5(5) . . ? C17 C12 C11 124.8(4) . . ? F2 C13 C14 118.5(5) . . ? F2 C13 C12 117.9(5) . . ? C14 C13 C12 123.6(6) . . ? C15 C14 C13 119.3(6) . . ? C15 C14 H14 120.3 . . ? C13 C14 H14 120.3 . . ? C14 C15 C16 120.3(5) . . ? C14 C15 H15 119.8 . . ? C16 C15 H15 119.8 . . ? C17 C16 C15 118.8(5) . . ? C17 C16 H16 120.6 . . ? C15 C16 H16 120.6 . . ? F1 C17 C16 118.3(5) . . ? F1 C17 C12 117.5(4) . . ? C16 C17 C12 124.2(5) . . ? O2 C18 C19 124.2(4) . . ? O2 C18 C23 118.1(3) . . ? C19 C18 C23 117.7(3) . . ? C18 C19 C20 121.2(4) . . ? C18 C19 H19 119.4 . . ? C20 C19 H19 119.4 . . ? C21 C20 C19 122.5(4) . . ? C21 C20 H20 118.7 . . ? C19 C20 H20 118.7 . . ? C20 C21 C22 119.4(4) . . ? C20 C21 H21 120.3 . . ? C22 C21 H21 120.3 . . ? C24 C22 C21 123.9(4) . . ? C24 C22 C23 117.0(3) . . ? C21 C22 C23 119.0(4) . . ? N2 C23 C22 122.0(4) . . ? N2 C23 C18 117.9(3) . . ? C22 C23 C18 120.1(3) . . ? C25 C24 C22 120.3(4) . . ? C25 C24 H24 119.8 . . ? C22 C24 H24 119.8 . . ? C24 C25 C26 120.4(4) . . ? C24 C25 H25 119.8 . . ? C26 C25 H25 119.8 . . ? N2 C26 C25 121.2(3) . . ? N2 C26 C27 117.8(3) . . ? C25 C26 C27 121.0(4) . . ? C28 C27 C26 124.8(4) . . ? C28 C27 H27 117.6 . . ? C26 C27 H27 117.6 . . ? C27 C28 C29 128.8(4) . . ? C27 C28 H28 115.6 . . ? C29 C28 H28 115.6 . . ? C34 C29 C30 114.1(5) . . ? C34 C29 C28 120.2(5) . . ? C30 C29 C28 125.7(5) . . ? F4 C30 C29 118.3(5) . . ? F4 C30 C31 117.6(6) . . ? C29 C30 C31 123.9(6) . . ? C32 C31 C30 118.6(7) . . ? C32 C31 H31 120.7 . . ? C30 C31 H31 120.7 . . ? C31 C32 C33 121.0(6) . . ? C31 C32 H32 119.5 . . ? C33 C32 H32 119.5 . . ? C32 C33 C34 117.4(7) . . ? C32 C33 H33 121.3 . . ? C34 C33 H33 121.3 . . ? F3 C34 C29 118.0(4) . . ? F3 C34 C33 117.0(6) . . ? C29 C34 C33 124.9(6) . . ? O3 C35 C36 122.9(4) . . ? O3 C35 C40 120.0(3) . . ? C36 C35 C40 117.1(4) . . ? C37 C36 C35 121.2(5) . . ? C37 C36 H36 119.4 . . ? C35 C36 H36 119.4 . . ? C38 C37 C36 121.8(4) . . ? C38 C37 H37 119.1 . . ? C36 C37 H37 119.1 . . ? C37 C38 C39 119.1(5) . . ? C37 C38 H38 120.4 . . ? C39 C38 H38 120.4 . . ? C38 C39 C41 123.9(5) . . ? C38 C39 C40 119.8(5) . . ? C41 C39 C40 116.3(4) . . ? N3 C40 C39 122.3(4) . . ? N3 C40 C35 116.8(4) . . ? C39 C40 C35 120.9(4) . . ? C42 C41 C39 120.4(5) . . ? C42 C41 H41 119.8 . . ? C39 C41 H41 119.8 . . ? C41 C42 C43 120.8(5) . . ? C41 C42 H42 119.6 . . ? C43 C42 H42 119.6 . . ? N3 C43 C42 120.3(4) . . ? N3 C43 C44 118.0(4) . . ? C42 C43 C44 121.6(4) . . ? C45 C44 C43 124.6(4) . . ? C45 C44 H44 117.7 . . ? C43 C44 H44 117.7 . . ? C44 C45 C46 128.4(4) . . ? C44 C45 H45 115.8 . . ? C46 C45 H45 115.8 . . ? C47 C46 C51 113.6(5) . . ? C47 C46 C45 121.5(5) . . ? C51 C46 C45 124.9(4) . . ? C48 C47 F6 119.2(5) . . ? C48 C47 C46 124.6(6) . . ? F6 C47 C46 116.2(5) . . ? C47 C48 C49 118.1(6) . . ? C47 C48 H48 121.0 . . ? C49 C48 H48 121.0 . . ? C50 C49 C48 120.8(6) . . ? C50 C49 H49 119.6 . . ? C48 C49 H49 119.6 . . ? C49 C50 C51 118.7(6) . . ? C49 C50 H50 120.6 . . ? C51 C50 H50 120.6 . . ? F5 C51 C50 118.1(5) . . ? F5 C51 C46 117.8(4) . . ? C50 C51 C46 124.1(5) . . ? O4 C52 C53 123.5(3) . . ? O4 C52 C57 119.1(3) . . ? C53 C52 C57 117.5(3) . . ? C52 C53 C54 121.5(4) . . ? C52 C53 H53 119.2 . . ? C54 C53 H53 119.2 . . ? C55 C54 C53 121.3(4) . . ? C55 C54 H54 119.3 . . ? C53 C54 H54 119.3 . . ? C54 C55 C56 120.0(4) . . ? C54 C55 H55 120.0 . . ? C56 C55 H55 120.0 . . ? C55 C56 C58 124.4(4) . . ? C55 C56 C57 119.9(4) . . ? C58 C56 C57 115.6(3) . . ? N4 C57 C56 123.4(3) . . ? N4 C57 C52 116.9(3) . . ? C56 C57 C52 119.7(3) . . ? C59 C58 C56 120.9(4) . . ? C59 C58 H58 119.5 . . ? C56 C58 H58 119.5 . . ? C58 C59 C60 120.7(4) . . ? C58 C59 H59 119.6 . . ? C60 C59 H59 119.6 . . ? N4 C60 C59 120.5(3) . . ? N4 C60 C61 117.0(3) . . ? C59 C60 C61 122.4(4) . . ? C62 C61 C60 123.1(4) . . ? C62 C61 H61 118.5 . . ? C60 C61 H61 118.5 . . ? C61 C62 C63 126.9(4) . . ? C61 C62 H62 116.5 . . ? C63 C62 H62 116.5 . . ? C64 C63 C68 114.6(4) . . ? C64 C63 C62 119.8(4) . . ? C68 C63 C62 125.6(4) . . ? F8 C64 C65 119.1(4) . . ? F8 C64 C63 117.6(4) . . ? C65 C64 C63 123.3(5) . . ? C66 C65 C64 119.8(5) . . ? C66 C65 H65 120.1 . . ? C64 C65 H65 120.1 . . ? C65 C66 C67 120.0(4) . . ? C65 C66 H66 120.0 . . ? C67 C66 H66 120.0 . . ? C68 C67 C66 118.6(5) . . ? C68 C67 H67 120.7 . . ? C66 C67 H67 120.7 . . ? F7 C68 C67 118.4(4) . . ? F7 C68 C63 118.0(4) . . ? C67 C68 C63 123.6(4) . . ? O5 C69 C70 122.4(5) . . ? O5 C69 C74 120.6(4) . . ? C70 C69 C74 117.0(5) . . ? C69 C70 C71 120.8(6) . . ? C69 C70 H70 119.6 . . ? C71 C70 H70 119.6 . . ? C72 C71 C70 121.7(6) . . ? C72 C71 H71 119.1 . . ? C70 C71 H71 119.1 . . ? C71 C72 C73 119.8(6) . . ? C71 C72 H72 120.1 . . ? C73 C72 H72 120.1 . . ? C75 C73 C74 116.6(5) . . ? C75 C73 C72 123.3(6) . . ? C74 C73 C72 120.0(6) . . ? N5 C74 C73 122.6(5) . . ? N5 C74 C69 116.8(4) . . ? C73 C74 C69 120.6(5) . . ? C76 C75 C73 120.2(5) . . ? C76 C75 H75 119.9 . . ? C73 C75 H75 119.9 . . ? C75 C76 C77 120.2(5) . . ? C75 C76 H76 119.9 . . ? C77 C76 H76 119.9 . . ? N5 C77 C76 119.9(5) . . ? N5 C77 C78 119.1(4) . . ? C76 C77 C78 121.1(5) . . ? C79 C78 C77 125.1(5) . . ? C79 C78 H78 117.5 . . ? C77 C78 H78 117.5 . . ? C78 C79 C80 131.8(9) . . ? C78 C79 C80A 127.8(9) . . ? C80 C79 C80A 4.6(16) . . ? C78 C79 H79A 114.0 . . ? C80 C79 H79A 114.1 . . ? C80A C79 H79A 118.1 . . ? C85 C80A C85A 3.2(13) . . ? C85 C80A C81A 103.3(14) . . ? C85A C80A C81A 106.3(11) . . ? C85 C80A C81 122.4(17) . . ? C85A C80A C81 125.3(12) . . ? C81A C80A C81 20.1(8) . . ? C85 C80A C79 130.5(14) . . ? C85A C80A C79 127.4(13) . . ? C81A C80A C79 126.1(15) . . ? C81 C80A C79 106.4(15) . . ? C81 C81A C82 118(4) . . ? C81 C81A C82A 142(4) . . ? C82 C81A C82A 24.7(8) . . ? C81 C81A C80 80(3) . . ? C82 C81A C80 155(2) . . ? C82A C81A C80 133.3(16) . . ? C81 C81A F9 35(3) . . ? C82 C81A F9 95.4(13) . . ? C82A C81A F9 118.4(11) . . ? C80 C81A F9 108.2(12) . . ? C81 C81A C80A 85(4) . . ? C82 C81A C80A 152.3(15) . . ? C82A C81A C80A 129.4(12) . . ? C80 C81A C80A 5.2(17) . . ? F9 C81A C80A 112.0(13) . . ? C81 C81A F9A 18(3) . . ? C82 C81A F9A 104.5(13) . . ? C82A C81A F9A 129.1(11) . . ? C80 C81A F9A 96.2(11) . . ? F9 C81A F9A 17.9(6) . . ? C80A C81A F9A 100.7(13) . . ? C81 C81A C83 157(4) . . ? C82 C81A C83 44.6(7) . . ? C82A C81A C83 20.6(7) . . ? C80 C81A C83 112.7(14) . . ? F9 C81A C83 139.0(11) . . ? C80A C81A C83 108.8(11) . . ? F9A C81A C83 148.7(11) . . ? C82 C82A C83 163(4) . . ? C82 C82A C81A 52(2) . . ? C83 C82A C81A 125.1(18) . . ? C82 C82A C83A 163(3) . . ? C83 C82A C83A 8.0(14) . . ? C81A C82A C83A 117.9(11) . . ? C82 C82A C81 42.5(17) . . ? C83 C82A C81 133(2) . . ? C81A C82A C81 10.2(10) . . ? C83A C82A C81 126.6(13) . . ? C82 C82A C84 137(3) . . ? C83 C82A C84 37.5(10) . . ? C81A C82A C84 87.9(11) . . ? C83A C82A C84 30.0(9) . . ? C81 C82A C84 96.8(10) . . ? C82 C82A H82A 69.8 . . ? C83 C82A H82A 115.0 . . ? C81A C82A H82A 119.9 . . ? C83A C82A H82A 122.2 . . ? C81 C82A H82A 111.0 . . ? C84 C82A H82A 152.1 . . ? C82 C82A H83A 147.4 . . ? C83 C82A H83A 33.0 . . ? C81A C82A H83A 158.2 . . ? C83A C82A H83A 40.4 . . ? C81 C82A H83A 165.7 . . ? C84 C82A H83A 70.3 . . ? H82A C82A H83A 82.0 . . ? C82 C82A H82B 40.0 . . ? C83 C82A H82B 141.9 . . ? C81A C82A H82B 91.4 . . ? C83A C82A H82B 149.8 . . ? C81 C82A H82B 81.9 . . ? C84 C82A H82B 172.8 . . ? H82A C82A H82B 30.0 . . ? H83A C82A H82B 110.0 . . ? C83A C83 C82A 160(3) . . ? C83A C83 C82 160(2) . . ? C82A C83 C82 6.9(18) . . ? C83A C83 C84 40(2) . . ? C82A C83 C84 121.1(15) . . ? C82 C83 C84 120.0 . . ? C83A C83 C84A 35.9(18) . . ? C82A C83 C84A 126(2) . . ? C82 C83 C84A 124.6(10) . . ? C84 C83 C84A 5.2(11) . . ? C83A C83 C81A 127(2) . . ? C82A C83 C81A 34.2(12) . . ? C82 C83 C81A 33.1(8) . . ? C84 C83 C81A 87.1(8) . . ? C84A C83 C81A 91.9(9) . . ? C83A C83 H82A 161.4 . . ? C82A C83 H82A 35.1 . . ? C82 C83 H82A 37.2 . . ? C84 C83 H82A 155.8 . . ? C84A C83 H82A 160.9 . . ? C81A C83 H82A 69.3 . . ? C83A C83 H83A 79.3 . . ? C82A C83 H83A 118.8 . . ? C82 C83 H83A 120.3 . . ? C84 C83 H83A 119.7 . . ? C84A C83 H83A 115.0 . . ? C81A C83 H83A 153.0 . . ? H82A C83 H83A 83.7 . . ? C83A C83 H83B 46.5 . . ? C82A C83 H83B 151.2 . . ? C82 C83 H83B 153.0 . . ? C84 C83 H83B 86.9 . . ? C84A C83 H83B 82.3 . . ? C81A C83 H83B 173.4 . . ? H82A C83 H83B 116.3 . . ? H83A C83 H83B 32.8 . . ? C82A C82 C81A 103(3) . . ? C82A C82 C81 121(2) . . ? C81A C82 C81 18.8(12) . . ? C82A C82 C83 10(3) . . ? C81A C82 C83 102.3(12) . . ? C81 C82 C83 120.0 . . ? C82A C82 F9 147(3) . . ? C81A C82 F9 48.9(10) . . ? C81 C82 F9 33.3(8) . . ? C83 C82 F9 149.9(8) . . ? C82A C82 C83A 12(2) . . ? C81A C82 C83A 96.7(12) . . ? C81 C82 C83A 114.3(6) . . ? C83 C82 C83A 5.7(6) . . ? F9 C82 C83A 144.5(10) . . ? C82A C82 H82A 75.1 . . ? C81A C82 H82A 162.7 . . ? C81 C82 H82A 158.8 . . ? C83 C82 H82A 78.7 . . ? F9 C82 H82A 125.7 . . ? C83A C82 H82A 84.2 . . ? C82A C82 H82B 117.6 . . ? C81A C82 H82B 137.1 . . ? C81 C82 H82B 120.0 . . ? C83 C82 H82B 120.0 . . ? F9 C82 H82B 88.3 . . ? C83A C82 H82B 125.7 . . ? H82A C82 H82B 42.6 . . ? C81A C81 F9 128(4) . . ? C81A C81 F9A 155(4) . . ? F9 C81 F9A 27.7(7) . . ? C81A C81 C82 44(3) . . ? F9 C81 C82 98.4(13) . . ? F9A C81 C82 117.2(10) . . ? C81A C81 C80 79(3) . . ? F9 C81 C80 137.1(14) . . ? F9A C81 C80 122.8(10) . . ? C82 C81 C80 120.0 . . ? C81A C81 C80A 75(3) . . ? F9 C81 C80A 138(2) . . ? F9A C81 C80A 126.2(12) . . ? C82 C81 C80A 116.6(12) . . ? C80 C81 C80A 4.4(15) . . ? C81A C81 C82A 28(3) . . ? F9 C81 C82A 112.0(16) . . ? F9A C81 C82A 133.0(13) . . ? C82 C81 C82A 16.1(6) . . ? C80 C81 C82A 104.2(6) . . ? C80A C81 C82A 100.6(14) . . ? C81A C80 C81 21.0(8) . . ? C81A C80 C85 99.6(8) . . ? C81 C80 C85 120.0 . . ? C81A C80 C79 133.5(18) . . ? C81 C80 C79 113.6(11) . . ? C85 C80 C79 126.4(12) . . ? C81A C80 C85A 102.5(14) . . ? C81 C80 C85A 122.7(9) . . ? C85 C80 C85A 3.0(12) . . ? C79 C80 C85A 123.7(12) . . ? C80A C85 F10 116.9(16) . . ? C80A C85 C84A 138.6(15) . . ? F10 C85 C84A 104.2(15) . . ? C80A C85 C84 120.6(10) . . ? F10 C85 C84 121.5(13) . . ? C84A C85 C84 18.1(8) . . ? C80A C85 C80 3(2) . . ? F10 C85 C80 118.0(13) . . ? C84A C85 C80 137.8(8) . . ? C84 C85 C80 120.0 . . ? C80A C85 F10A 116.4(15) . . ? F10 C85 F10A 19.5(6) . . ? C84A C85 F10A 104.1(15) . . ? C84 C85 F10A 122.1(13) . . ? C80 C85 F10A 116.3(13) . . ? C83A C84 C85 141.2(11) . . ? C83A C84 C83 21.2(11) . . ? C85 C84 C83 120.0 . . ? C83A C84 C85A 145(2) . . ? C85 C84 C85A 4.2(15) . . ? C83 C84 C85A 123.9(13) . . ? C83A C84 C82A 42.4(10) . . ? C85 C84 C82A 98.8(6) . . ? C83 C84 C82A 21.4(6) . . ? C85A C84 C82A 102.8(14) . . ? C83A C84 H84A 98.8 . . ? C85 C84 H84A 120.0 . . ? C83 C84 H84A 120.0 . . ? C85A C84 H84A 116.1 . . ? C82A C84 H84A 141.1 . . ? C83A C84 H84B 119.3 . . ? C85 C84 H84B 99.4 . . ? C83 C84 H84B 140.3 . . ? C85A C84 H84B 95.3 . . ? C82A C84 H84B 161.7 . . ? H84A C84 H84B 21.3 . . ? C83 C83A C84 118(3) . . ? C83 C83A C84A 130(2) . . ? C84 C83A C84A 12.1(14) . . ? C83 C83A C82A 12(2) . . ? C84 C83A C82A 107.6(17) . . ? C84A C83A C82A 119.5(12) . . ? C83 C83A C82 13.9(17) . . ? C84 C83A C82 104.5(15) . . ? C84A C83A C82 116.3(11) . . ? C82A C83A C82 5.0(9) . . ? C83 C83A H83A 67.4 . . ? C84 C83A H83A 174.1 . . ? C84A C83A H83A 161.9 . . ? C82A C83A H83A 78.3 . . ? C82 C83A H83A 81.3 . . ? C83 C83A H84A 157.3 . . ? C84 C83A H84A 39.0 . . ? C84A C83A H84A 27.3 . . ? C82A C83A H84A 146.4 . . ? C82 C83A H84A 143.5 . . ? H83A C83A H84A 135.2 . . ? C83 C83A H83B 107.9 . . ? C84 C83A H83B 133.6 . . ? C84A C83A H83B 121.7 . . ? C82A C83A H83B 118.8 . . ? C82 C83A H83B 121.8 . . ? H83A C83A H83B 40.5 . . ? H84A C83A H83B 94.7 . . ? C85A C84A C83A 115.5(12) . . ? C85A C84A C85 4.4(13) . . ? C83A C84A C85 111.2(14) . . ? C85A C84A C83 101.6(10) . . ? C83A C84A C83 14.0(8) . . ? C85 C84A C83 97.3(13) . . ? C85A C84A H84A 156.3 . . ? C83A C84A H84A 86.6 . . ? C85 C84A H84A 159.7 . . ? C83 C84A H84A 100.6 . . ? C85A C84A H84B 121.8 . . ? C83A C84A H84B 122.7 . . ? C85 C84A H84B 126.0 . . ? C83 C84A H84B 136.6 . . ? H84A C84A H84B 36.9 . . ? F10 C85A F10A 21.0(6) . . ? F10 C85A C80A 117.9(16) . . ? F10A C85A C80A 118.2(15) . . ? F10 C85A C84A 109.5(17) . . ? F10A C85A C84A 109.9(16) . . ? C80A C85A C84A 131.4(11) . . ? F10 C85A C84 126(2) . . ? F10A C85A C84 128(2) . . ? C80A C85A C84 113.5(12) . . ? C84A C85A C84 17.9(8) . . ? F10 C85A C80 118.9(17) . . ? F10A C85A C80 117.9(16) . . ? C80A C85A C80 3(2) . . ? C84A C85A C80 131.0(13) . . ? C84 C85A C80 113.3(15) . . ? O6 C86 C87 124.2(3) . . ? O6 C86 C91 118.5(3) . . ? C87 C86 C91 117.3(3) . . ? C86 C87 C88 120.9(4) . . ? C86 C87 H87 119.1 . . ? C88 C87 H87 120.0 . . ? C89 C88 C87 122.8(4) . . ? C89 C88 H88 118.6 . . ? C87 C88 H88 118.6 . . ? C88 C89 C90 119.2(4) . . ? C88 C89 H89 120.4 . . ? C90 C89 H89 120.4 . . ? C92 C90 C89 124.1(4) . . ? C92 C90 C91 116.7(4) . . ? C89 C90 C91 119.2(4) . . ? N6 C91 C90 122.8(3) . . ? N6 C91 C86 116.8(3) . . ? C90 C91 C86 120.4(4) . . ? C93 C92 C90 120.5(4) . . ? C93 C92 H92 119.8 . . ? C90 C92 H92 119.8 . . ? C92 C93 C94 120.7(4) . . ? C92 C93 H93 119.7 . . ? C94 C93 H93 119.7 . . ? N6 C94 C93 119.9(4) . . ? N6 C94 C95 118.3(4) . . ? C93 C94 C95 121.7(4) . . ? C96 C95 C94 126.5(4) . . ? C96 C95 H95 116.8 . . ? C94 C95 H95 116.8 . . ? C95 C96 C97 130.0(8) . . ? C95 C96 C1A 124.0(7) . . ? C97 C96 C1A 7.5(10) . . ? C95 C96 H96A 114.4 . . ? C97 C96 H96A 115.6 . . ? C1A C96 H96A 121.4 . . ? C2A C97 C102 20.2(6) . . ? C2A C97 C98 100.0(6) . . ? C102 C97 C98 120.0 . . ? C2A C97 C96 135.9(14) . . ? C102 C97 C96 115.9(9) . . ? C98 C97 C96 124.1(9) . . ? C2A C97 C6A 108.4(10) . . ? C102 C97 C6A 128.5(5) . . ? C98 C97 C6A 8.5(5) . . ? C96 C97 C6A 115.6(9) . . ? F12A C102 F12 19.2(11) . . ? F12A C102 C97 141.5(14) . . ? F12 C102 C97 122.6(8) . . ? F12A C102 C101 98.4(14) . . ? F12 C102 C101 117.4(8) . . ? C97 C102 C101 120.0 . . ? F12A C102 C1A 149.6(15) . . ? F12 C102 C1A 130.7(9) . . ? C97 C102 C1A 8.2(7) . . ? C101 C102 C1A 111.9(7) . . ? F12A C102 C3A 117.4(16) . . ? F12 C102 C3A 136.6(10) . . ? C97 C102 C3A 100.5(4) . . ? C101 C102 C3A 20.4(4) . . ? C1A C102 C3A 92.5(8) . . ? C3A C101 C2A 96.7(17) . . ? C3A C101 C100 16.6(18) . . ? C2A C101 C100 101.7(8) . . ? C3A C101 C102 115.1(13) . . ? C2A C101 C102 18.5(8) . . ? C100 C101 C102 120.0 . . ? C3A C101 F12A 141.9(19) . . ? C2A C101 F12A 47.7(7) . . ? C100 C101 F12A 149.4(8) . . ? C102 C101 F12A 29.5(8) . . ? C3A C101 H3AA 69.4 . . ? C2A C101 H3AA 159.0 . . ? C100 C101 H3AA 69.6 . . ? C102 C101 H3AA 162.2 . . ? F12A C101 H3AA 138.6 . . ? C3A C101 H10A 122.3 . . ? C2A C101 H10A 138.1 . . ? C100 C101 H10A 120.0 . . ? C102 C101 H10A 120.0 . . ? F12A C101 H10A 90.5 . . ? H3AA C101 H10A 52.8 . . ? C4A C100 C3A 137(2) . . ? C4A C100 C99 39.6(14) . . ? C3A C100 C99 115.6(11) . . ? C4A C100 C101 150.2(14) . . ? C3A C100 C101 15.2(15) . . ? C99 C100 C101 120.0 . . ? C4A C100 C5A 33.2(8) . . ? C3A C100 C5A 119.2(13) . . ? C99 C100 C5A 6.5(8) . . ? C101 C100 C5A 125.0(6) . . ? C4A C100 C2A 119.2(13) . . ? C3A C100 C2A 33.0(8) . . ? C99 C100 C2A 85.7(6) . . ? C101 C100 C2A 34.3(6) . . ? C5A C100 C2A 90.7(6) . . ? C4A C100 H3AA 147.8 . . ? C3A C100 H3AA 41.5 . . ? C99 C100 H3AA 156.6 . . ? C101 C100 H3AA 40.2 . . ? C5A C100 H3AA 158.4 . . ? C2A C100 H3AA 73.2 . . ? C4A C100 H4AA 42.2 . . ? C3A C100 H4AA 147.6 . . ? C99 C100 H4AA 79.8 . . ? C101 C100 H4AA 156.5 . . ? C5A C100 H4AA 73.9 . . ? C2A C100 H4AA 158.8 . . ? H3AA C100 H4AA 117.2 . . ? C4A C100 H10B 84.4 . . ? C3A C100 H10B 122.2 . . ? C99 C100 H10B 120.0 . . ? C101 C100 H10B 120.0 . . ? C5A C100 H10B 114.8 . . ? C2A C100 H10B 154.2 . . ? H3AA C100 H10B 81.2 . . ? H4AA C100 H10B 42.3 . . ? C5A C99 C4A 128(3) . . ? C5A C99 C100 158(3) . . ? C4A C99 C100 29.8(8) . . ? C5A C99 C98 78(2) . . ? C4A C99 C98 144.0(9) . . ? C100 C99 C98 120.0 . . ? C5A C99 C6A 66.2(15) . . ? C4A C99 C6A 154.3(17) . . ? C100 C99 C6A 132.0(9) . . ? C98 C99 C6A 12.0(9) . . ? C5A C99 C3A 160(3) . . ? C4A C99 C3A 47.2(6) . . ? C100 C99 C3A 21.6(5) . . ? C98 C99 C3A 99.1(5) . . ? C6A C99 C3A 111.0(10) . . ? C5A C99 H5AA 21.3 . . ? C4A C99 H5AA 112.8 . . ? C100 C99 H5AA 141.6 . . ? C98 C99 H5AA 97.9 . . ? C6A C99 H5AA 85.9 . . ? C3A C99 H5AA 158.9 . . ? C5A C99 H99A 44.2 . . ? C4A C99 H99A 93.4 . . ? C100 C99 H99A 120.0 . . ? C98 C99 H99A 120.0 . . ? C6A C99 H99A 108.0 . . ? C3A C99 H99A 140.4 . . ? H5AA C99 H99A 22.9 . . ? C1A C98 C99 119.9(9) . . ? C1A C98 C97 1(2) . . ? C99 C98 C97 120.0 . . ? C1A C98 C5A 143.4(12) . . ? C99 C98 C5A 24.4(5) . . ? C97 C98 C5A 143.4(5) . . ? C1A C98 F11A 120.5(12) . . ? C99 C98 F11A 119.6(10) . . ? C97 C98 F11A 120.3(10) . . ? C5A C98 F11A 95.6(11) . . ? C1A C98 F11 113.2(12) . . ? C99 C98 F11 124.2(10) . . ? C97 C98 F11 113.5(10) . . ? C5A C98 F11 102.9(11) . . ? F11A C98 F11 19.0(6) . . ? F9A F9 C81 103(2) . . ? F9A F9 C81A 120(2) . . ? C81 F9 C81A 16.5(13) . . ? F9A F9 C82 132(2) . . ? C81 F9 C82 48.2(7) . . ? C81A F9 C82 35.8(8) . . ? F9 F9A C81 48.8(19) . . ? F9 F9A C81A 42.5(19) . . ? C81 F9A C81A 6.7(11) . . ? C85A F10 C85 2(2) . . ? C85A F10A C85 1.5(17) . . ? C6A F11 C98 6.7(14) . . ? C6A F11A C98 3.7(11) . . ? F12A F12 C102 28(2) . . ? F12A F12 C2A 24(2) . . ? C102 F12 C2A 4.3(9) . . ? F12 F12A C102 133(3) . . ? F12 F12A C2A 145(3) . . ? C102 F12A C2A 12.4(12) . . ? F12 F12A C101 171(3) . . ? C102 F12A C101 52.1(8) . . ? C2A F12A C101 40.3(7) . . ? C9 N1 C6 119.7(3) . . ? C9 N1 Zn1 130.4(2) . . ? C6 N1 Zn1 109.5(2) . . ? C26 N2 C23 119.0(3) . . ? C26 N2 Zn1 132.7(2) . . ? C23 N2 Zn1 108.2(2) . . ? C43 N3 C40 119.7(4) . . ? C43 N3 Zn3 133.4(3) . . ? C40 N3 Zn3 106.9(3) . . ? C60 N4 C57 118.8(3) . . ? C60 N4 Zn3 132.3(2) . . ? C57 N4 Zn3 108.9(2) . . ? C77 N5 C74 120.4(4) . . ? C77 N5 Zn2 132.6(3) . . ? C74 N5 Zn2 106.9(3) . . ? C94 N6 C91 119.3(3) . . ? C94 N6 Zn2 131.4(3) . . ? C91 N6 Zn2 109.2(2) . . ? C1 O1 Zn1 115.7(2) . . ? C1 O1 Zn2 137.7(2) . . ? Zn1 O1 Zn2 102.96(10) . . ? C18 O2 Zn1 116.1(2) . . ? C18 O2 Zn3 137.6(2) . . ? Zn1 O2 Zn3 103.56(10) . . ? C35 O3 Zn3 115.1(3) . . ? C52 O4 Zn3 114.7(2) . . ? C52 O4 Zn1 123.7(2) . . ? Zn3 O4 Zn1 102.25(10) . . ? C69 O5 Zn2 111.9(3) . . ? C86 O6 Zn2 116.3(2) . . ? C86 O6 Zn1 128.7(2) . . ? Zn2 O6 Zn1 102.31(10) . . ? O2 Zn1 O1 171.47(10) . . ? O2 Zn1 O6 97.52(9) . . ? O1 Zn1 O6 76.40(9) . . ? O2 Zn1 N1 107.12(11) . . ? O1 Zn1 N1 78.57(10) . . ? O6 Zn1 N1 154.86(10) . . ? O2 Zn1 O4 75.90(9) . . ? O1 Zn1 O4 97.70(9) . . ? O6 Zn1 O4 88.02(9) . . ? N1 Zn1 O4 93.10(10) . . ? O2 Zn1 N2 78.97(10) . . ? O1 Zn1 N2 107.23(11) . . ? O6 Zn1 N2 94.61(10) . . ? N1 Zn1 N2 94.91(11) . . ? O4 Zn1 N2 154.86(10) . . ? O5 Zn2 O6 165.04(12) . . ? O5 Zn2 N5 83.32(13) . . ? O6 Zn2 N5 110.95(12) . . ? O5 Zn2 O1 95.07(10) . . ? O6 Zn2 O1 77.78(9) . . ? N5 Zn2 O1 102.92(11) . . ? O5 Zn2 N6 100.58(11) . . ? O6 Zn2 N6 79.04(10) . . ? N5 Zn2 N6 110.68(12) . . ? O1 Zn2 N6 144.22(11) . . ? O3 Zn3 O4 168.28(11) . . ? O3 Zn3 O2 91.78(10) . . ? O4 Zn3 O2 77.31(9) . . ? O3 Zn3 N4 104.97(11) . . ? O4 Zn3 N4 80.38(10) . . ? O2 Zn3 N4 134.48(11) . . ? O3 Zn3 N3 81.05(12) . . ? O4 Zn3 N3 107.67(11) . . ? O2 Zn3 N3 117.58(11) . . ? N4 Zn3 N3 106.81(12) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 27.61 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.447 _refine_diff_density_min -0.295 _refine_diff_density_rms 0.063 data_2 _database_code_depnum_ccdc_archive 'CCDC 878061' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C102 H60 N18 O30 Zn3' _chemical_formula_weight 2213.79 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' 'N' 'N' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Zn' 'Zn' -1.5491 0.6778 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 31.0821(5) _cell_length_b 21.4890(4) _cell_length_c 16.0173(2) _cell_angle_alpha 90.00 _cell_angle_beta 118.5090(10) _cell_angle_gamma 90.00 _cell_volume 9401.1(3) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 8142 _cell_measurement_theta_min 2.62 _cell_measurement_theta_max 67.82 _exptl_crystal_description Block _exptl_crystal_colour Red _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.564 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4512 _exptl_absorpt_coefficient_mu 1.715 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.6937 _exptl_absorpt_correction_T_max 0.8206 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX area-detector diffractometer' _diffrn_measurement_method '\f and \w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27252 _diffrn_reflns_av_R_equivalents 0.0377 _diffrn_reflns_av_sigmaI/netI 0.0357 _diffrn_reflns_limit_h_min -36 _diffrn_reflns_limit_h_max 37 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.62 _diffrn_reflns_theta_max 67.82 _reflns_number_total 8142 _reflns_number_gt 6505 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1997)' _computing_cell_refinement 'SAINT (Bruker, 1999)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL-PLUS (Sheldrick, 1990)' _computing_publication_material SHELXL-97 _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The terminal NO2 groups suffer from disorder, DFIX restraints were applied to fix the terminal group and SIMU restraints were used to give all the N and O atoms similar Ueq values so as to achieve reasonable model DFIX 1.47 N6A C32 DFIX 1.25 O9A N6A DFIX 1.25 O4A N1 DFIX 1.25 O3 N1 SIMU 0.01 0.08 1.7 O9A N6A O10A SIMU 0.01 0.08 1.7 O4A O4 N1 O3A O3 ; _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^)+(0.0713P)^2^+5.6820P] 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 8142 _refine_ls_number_parameters 855 _refine_ls_number_restraints 53 _refine_ls_R_factor_all 0.0549 _refine_ls_R_factor_gt 0.0420 _refine_ls_wR_factor_ref 0.1214 _refine_ls_wR_factor_gt 0.1111 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.027 _refine_ls_shift/su_max 0.008 _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 C1 C -0.06510(18) 0.3840(2) -0.1597(3) 0.0859(13) Uani 1 1 d . . . H1 H -0.040(2) 0.364(3) -0.165(4) 0.136(19) Uiso 1 1 d . . . C2 C -0.10391(15) 0.41269(16) -0.2341(2) 0.0701(9) Uani 1 1 d . . . C3 C -0.14046(13) 0.44137(15) -0.2238(2) 0.0610(8) Uani 1 1 d . . . H3 H -0.1685(13) 0.4622(16) -0.274(2) 0.069(10) Uiso 1 1 d . . . C4 C -0.13762(11) 0.43999(14) -0.1352(2) 0.0549(7) Uani 1 1 d . . . C5 C -0.09928(12) 0.41114(15) -0.0561(2) 0.0580(7) Uani 1 1 d . . . C6 C -0.06306(16) 0.3838(2) -0.0719(3) 0.0794(12) Uani 1 1 d . . . H6 H -0.0346(17) 0.365(2) -0.023(3) 0.108(15) Uiso 1 1 d . . . C7 C -0.09593(13) 0.41094(16) 0.0383(2) 0.0608(8) Uani 1 1 d . . . H7 H -0.1097(12) 0.4458(17) 0.054(2) 0.068(10) Uiso 1 1 d . . . C8 C -0.07434(11) 0.36697(15) 0.10324(19) 0.0518(7) Uani 1 1 d . . . H8 H -0.0627(11) 0.3311(16) 0.088(2) 0.057(9) Uiso 1 1 d . . . C9 C -0.07364(10) 0.36546(13) 0.19519(19) 0.0488(6) Uani 1 1 d . . . C10 C -0.10065(14) 0.40885(17) 0.2178(2) 0.0670(9) Uani 1 1 d . . . H10 H -0.1166(13) 0.4402(18) 0.176(3) 0.074(10) Uiso 1 1 d . . . C11 C -0.10139(14) 0.40476(17) 0.3015(2) 0.0675(9) Uani 1 1 d . . . H11 H -0.1220(14) 0.4288(18) 0.310(3) 0.080(11) Uiso 1 1 d . . . C12 C -0.07528(11) 0.35782(14) 0.36703(19) 0.0516(7) Uani 1 1 d . . . C13 C -0.07569(12) 0.34902(16) 0.4538(2) 0.0584(8) Uani 1 1 d . . . H13 H -0.0965(12) 0.3771(16) 0.465(2) 0.067(9) Uiso 1 1 d . . . C14 C -0.05094(11) 0.30035(16) 0.5102(2) 0.0551(7) Uani 1 1 d . . . H14 H -0.0509(13) 0.2916(16) 0.564(3) 0.071(10) Uiso 1 1 d . . . C15 C -0.02307(11) 0.25966(15) 0.48691(18) 0.0504(7) Uani 1 1 d . . . H15 H -0.0076(10) 0.2249(14) 0.523(2) 0.044(7) Uiso 1 1 d . . . C16 C -0.01901(9) 0.26856(13) 0.40546(17) 0.0424(6) Uani 1 1 d . . . C17 C -0.04796(10) 0.31631(13) 0.34139(17) 0.0432(6) Uani 1 1 d . . . C18 C 0.08106(11) 0.18876(14) 0.62922(17) 0.0497(6) Uani 1 1 d . . . C19 C 0.07482(14) 0.19416(17) 0.7098(2) 0.0623(8) Uani 1 1 d . . . H19 H 0.0484(12) 0.1741(15) 0.710(2) 0.056(9) Uiso 1 1 d . . . C20 C 0.10647(16) 0.22996(19) 0.7875(2) 0.0738(10) Uani 1 1 d . . . H20 H 0.0986(14) 0.2323(18) 0.842(3) 0.087(12) Uiso 1 1 d . . . C21 C 0.14504(16) 0.26146(18) 0.7904(2) 0.0695(10) Uani 1 1 d . . . H21 H 0.1683(16) 0.286(2) 0.841(3) 0.101(14) Uiso 1 1 d . . . C22 C 0.15289(12) 0.25998(14) 0.71035(18) 0.0554(7) Uani 1 1 d . . . C23 C 0.12041(10) 0.22479(13) 0.62993(16) 0.0484(6) Uani 1 1 d . . . C24 C 0.19062(13) 0.29198(16) 0.7033(2) 0.0641(8) Uani 1 1 d . . . H24 H 0.2121(15) 0.316(2) 0.761(3) 0.092(12) Uiso 1 1 d . . . C25 C 0.19440(13) 0.28970(16) 0.6225(2) 0.0593(8) Uani 1 1 d . . . H25 H 0.2188(12) 0.3116(15) 0.619(2) 0.055(9) Uiso 1 1 d . . . C26 C 0.16014(11) 0.25403(14) 0.54389(17) 0.0499(6) Uani 1 1 d . . . C27 C 0.16025(11) 0.25066(16) 0.4529(2) 0.0549(7) Uani 1 1 d . . . H27 H 0.1377(13) 0.2198(16) 0.410(3) 0.070(10) Uiso 1 1 d . . . C28 C 0.18663(12) 0.28463(17) 0.4256(2) 0.0593(8) Uani 1 1 d . . . H28 H 0.2075(17) 0.317(2) 0.467(3) 0.108(15) Uiso 1 1 d . . . C29 C 0.18284(11) 0.27977(16) 0.33123(19) 0.0575(7) Uani 1 1 d . . . C30 C 0.20810(12) 0.31887(18) 0.2997(2) 0.0661(9) Uani 1 1 d . . . C31 C 0.20656(14) 0.3112(3) 0.2121(3) 0.0832(12) Uani 1 1 d . . . H31 H 0.2238(16) 0.340(2) 0.199(3) 0.093(14) Uiso 1 1 d . . . C32 C 0.17817(14) 0.2648(2) 0.1546(2) 0.0796(12) Uani 1 1 d D . . C33 C 0.15151(14) 0.2256(2) 0.1800(2) 0.0701(9) Uani 1 1 d . . . H33 H 0.1308(14) 0.1933(19) 0.140(3) 0.082(12) Uiso 1 1 d . . . C34 C 0.15417(13) 0.23312(17) 0.2675(2) 0.0627(8) Uani 1 1 d . . . H34 H 0.1328(15) 0.207(2) 0.283(3) 0.091(13) Uiso 1 1 d . . . C35 C 0.05693(9) 0.11644(13) 0.27725(16) 0.0419(6) Uani 1 1 d . . . C36 C 0.04393(10) 0.10631(15) 0.18271(18) 0.0499(7) Uani 1 1 d . . . H36 H 0.0385(11) 0.1407(15) 0.146(2) 0.050(8) Uiso 1 1 d . . . C37 C 0.04263(11) 0.04579(16) 0.14883(19) 0.0571(8) Uani 1 1 d . . . H37 H 0.0320(14) 0.0434(18) 0.085(3) 0.084(11) Uiso 1 1 d . . . C38 C 0.05486(12) -0.00478(17) 0.2059(2) 0.0582(7) Uani 1 1 d . . . H38 H 0.0545(15) -0.044(2) 0.184(3) 0.098(13) Uiso 1 1 d . . . C39 C 0.07148(10) 0.00317(14) 0.30424(18) 0.0496(6) Uani 1 1 d . . . C40 C 0.07216(9) 0.06395(13) 0.33937(16) 0.0416(6) Uani 1 1 d . . . C41 C 0.08859(13) -0.04511(16) 0.3713(2) 0.0614(8) Uani 1 1 d . . . H41 H 0.0900(15) -0.083(2) 0.348(3) 0.095(13) Uiso 1 1 d . . . C42 C 0.10658(12) -0.03239(16) 0.4652(2) 0.0580(7) Uani 1 1 d . . . H42 H 0.1187(14) -0.0622(19) 0.503(3) 0.080(12) Uiso 1 1 d . . . C43 C 0.10720(10) 0.02890(13) 0.49636(18) 0.0464(6) Uani 1 1 d . . . C44 C 0.12889(11) 0.04545(15) 0.59670(19) 0.0515(7) Uani 1 1 d . . . H44 H 0.1206(12) 0.0823(17) 0.606(2) 0.061(9) Uiso 1 1 d . . . C45 C 0.15824(12) 0.01101(16) 0.6692(2) 0.0570(7) Uani 1 1 d . . . H45 H 0.1661(17) -0.028(2) 0.657(3) 0.108(15) Uiso 1 1 d . . . C46 C 0.18002(10) 0.03045(14) 0.76894(18) 0.0504(6) Uani 1 1 d . . . C47 C 0.18438(12) 0.09345(16) 0.7927(2) 0.0597(8) Uani 1 1 d . . . H47 H 0.1735(13) 0.1240(18) 0.742(3) 0.081(11) Uiso 1 1 d . . . C48 C 0.20368(12) 0.11435(18) 0.8850(2) 0.0632(8) Uani 1 1 d . . . H48 H 0.2095(13) 0.1563(18) 0.894(3) 0.075(11) Uiso 1 1 d . . . C49 C 0.21837(11) 0.07091(17) 0.95641(19) 0.0591(8) Uani 1 1 d . . . C50 C 0.21486(11) 0.00891(17) 0.9390(2) 0.0589(8) Uani 1 1 d . . . H50 H 0.2257(12) -0.0163(16) 0.987(2) 0.061(9) Uiso 1 1 d . . . C51 C 0.19691(11) -0.01063(15) 0.84651(19) 0.0550(7) Uani 1 1 d . . . N1 N -0.10680(19) 0.41344(19) -0.3290(3) 0.0964(11) Uani 1 1 d DU . . N2 N -0.17760(10) 0.46975(14) -0.12663(19) 0.0637(7) Uani 1 1 d . . . N3 N -0.04822(8) 0.32029(10) 0.25522(14) 0.0426(5) Uani 1 1 d . . . N4 N 0.12494(8) 0.22237(11) 0.54924(13) 0.0458(5) Uani 1 1 d . . . N5 N 0.23732(12) 0.37127(19) 0.3593(2) 0.0822(10) Uani 1 1 d . . . N6 N 0.1749(9) 0.2515(10) 0.0607(10) 0.097(4) Uani 0.60 1 d P . . N6A N 0.1757(17) 0.2652(19) 0.0617(18) 0.134(9) Uani 0.40 1 d PDU . . N7 N 0.08834(7) 0.07554(10) 0.43394(13) 0.0421(5) Uani 1 1 d . . . N8 N 0.19676(13) -0.07829(15) 0.8337(2) 0.0804(9) Uani 1 1 d . . . N9 N 0.23829(11) 0.09225(18) 1.05483(19) 0.0734(8) Uani 1 1 d . . . O1 O -0.19259(11) 0.44508(15) -0.0771(2) 0.0924(8) Uani 1 1 d . . . O2 O -0.19405(10) 0.51774(14) -0.1699(2) 0.0913(8) Uani 1 1 d . . . O3A O -0.1377(9) 0.4445(13) -0.3874(15) 0.108(5) Uani 0.60 1 d PU . . O4 O -0.0660(6) 0.4020(6) -0.3266(11) 0.109(3) Uani 0.40 1 d PU . . O4A O -0.0805(4) 0.3787(4) -0.3442(7) 0.114(3) Uani 0.60 1 d PDU . . O5 O 0.01066(6) 0.23607(9) 0.38365(11) 0.0435(4) Uani 1 1 d . . . O6 O 0.05359(7) 0.15387(9) 0.55647(12) 0.0510(5) Uani 1 1 d . . . O7 O 0.21894(13) 0.40497(17) 0.3941(2) 0.1086(11) Uani 1 1 d . . . O8 O 0.27844(12) 0.3771(2) 0.3703(3) 0.1321(14) Uani 1 1 d . . . O9 O 0.2003(5) 0.2838(7) 0.0392(10) 0.126(4) Uani 0.60 1 d P . . O9A O 0.1879(8) 0.3109(12) 0.0319(14) 0.138(8) Uani 0.40 1 d PDU . . O10 O 0.1525(9) 0.2057(11) 0.0177(14) 0.121(5) Uani 0.60 1 d P . . O10A O 0.1517(13) 0.2225(18) 0.008(2) 0.135(9) Uani 0.40 1 d PDU . . O11 O 0.05703(6) 0.17242(8) 0.31377(11) 0.0424(4) Uani 1 1 d . . . O12 O 0.20525(16) -0.09827(14) 0.7710(2) 0.1201(12) Uani 1 1 d . . . O13 O 0.19547(16) -0.11148(14) 0.8922(2) 0.1247(13) Uani 1 1 d . . . O14 O 0.24446(12) 0.05427(17) 1.11586(17) 0.1042(10) Uani 1 1 d . . . O15 O 0.24828(14) 0.14667(19) 1.0717(2) 0.1154(11) Uani 1 1 d . . . Zn1 Zn 0.067574(12) 0.168010(17) 0.44910(2) 0.04324(12) Uani 1 1 d . . . Zn2 Zn 0.0000 0.24381(2) 0.2500 0.04150(14) Uani 1 2 d S . . O3 O -0.1436(12) 0.435(2) -0.399(2) 0.111(9) Uani 0.40 1 d PDU . . 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 C1 0.117(3) 0.095(3) 0.069(2) 0.023(2) 0.062(2) 0.040(3) C2 0.113(3) 0.063(2) 0.0489(16) 0.0043(15) 0.0499(18) 0.0060(19) C3 0.080(2) 0.0538(18) 0.0448(15) 0.0059(14) 0.0260(15) -0.0029(16) C4 0.0649(18) 0.0517(17) 0.0519(15) 0.0073(13) 0.0310(14) 0.0024(13) C5 0.076(2) 0.0555(17) 0.0486(15) 0.0131(13) 0.0347(14) 0.0138(15) C6 0.102(3) 0.092(3) 0.0595(19) 0.0287(19) 0.051(2) 0.045(2) C7 0.080(2) 0.0607(19) 0.0525(16) 0.0109(14) 0.0403(16) 0.0190(16) C8 0.0604(17) 0.0556(18) 0.0436(14) 0.0057(13) 0.0283(13) 0.0086(13) C9 0.0586(17) 0.0487(16) 0.0444(14) 0.0029(12) 0.0289(13) 0.0047(12) C10 0.090(2) 0.062(2) 0.0633(19) 0.0169(17) 0.0487(18) 0.0236(18) C11 0.091(2) 0.062(2) 0.069(2) 0.0070(16) 0.0547(19) 0.0242(18) C12 0.0616(17) 0.0559(17) 0.0458(14) -0.0026(13) 0.0326(13) 0.0033(13) C13 0.070(2) 0.070(2) 0.0492(16) -0.0081(15) 0.0400(15) 0.0021(16) C14 0.0614(18) 0.077(2) 0.0379(13) -0.0020(14) 0.0327(13) -0.0013(15) C15 0.0545(16) 0.0663(19) 0.0328(12) 0.0017(13) 0.0229(12) -0.0001(13) C16 0.0469(14) 0.0508(15) 0.0317(11) -0.0061(10) 0.0205(11) -0.0029(11) C17 0.0506(15) 0.0496(15) 0.0359(12) -0.0034(11) 0.0260(11) -0.0030(11) C18 0.0623(17) 0.0563(17) 0.0311(12) 0.0077(12) 0.0228(12) 0.0121(13) C19 0.080(2) 0.077(2) 0.0385(14) 0.0082(14) 0.0350(15) 0.0119(18) C20 0.103(3) 0.090(3) 0.0329(14) 0.0022(15) 0.0365(17) 0.018(2) C21 0.095(3) 0.077(2) 0.0286(13) -0.0067(14) 0.0229(16) 0.0084(19) C22 0.072(2) 0.0566(17) 0.0293(12) -0.0041(12) 0.0172(13) 0.0058(14) C23 0.0612(17) 0.0543(16) 0.0255(11) 0.0016(11) 0.0173(11) 0.0132(13) C24 0.074(2) 0.066(2) 0.0340(14) -0.0121(13) 0.0107(13) -0.0037(16) C25 0.065(2) 0.063(2) 0.0405(14) -0.0071(13) 0.0176(14) -0.0080(15) C26 0.0555(17) 0.0570(17) 0.0307(12) -0.0069(11) 0.0153(12) -0.0029(13) C27 0.0564(18) 0.0687(19) 0.0373(13) -0.0063(13) 0.0206(13) -0.0083(14) C28 0.0621(19) 0.072(2) 0.0399(14) -0.0082(14) 0.0211(13) -0.0108(15) C29 0.0590(18) 0.074(2) 0.0386(13) 0.0006(14) 0.0227(13) -0.0014(15) C30 0.0565(19) 0.097(3) 0.0443(15) 0.0019(16) 0.0233(14) -0.0072(16) C31 0.063(2) 0.141(4) 0.0505(18) 0.011(2) 0.0307(17) -0.005(2) C32 0.067(2) 0.135(4) 0.0360(15) 0.0044(19) 0.0233(16) 0.021(2) C33 0.074(2) 0.090(3) 0.0403(15) -0.0048(17) 0.0224(15) 0.0128(19) C34 0.068(2) 0.075(2) 0.0402(14) -0.0055(14) 0.0223(14) 0.0006(16) C35 0.0413(13) 0.0557(16) 0.0307(11) -0.0058(11) 0.0188(10) 0.0000(11) C36 0.0548(16) 0.0648(19) 0.0316(12) -0.0009(13) 0.0218(12) 0.0080(13) C37 0.0625(18) 0.076(2) 0.0333(13) -0.0119(14) 0.0230(13) 0.0075(15) C38 0.0655(19) 0.062(2) 0.0467(15) -0.0158(15) 0.0268(14) 0.0028(15) C39 0.0518(16) 0.0564(17) 0.0416(13) -0.0076(12) 0.0231(12) -0.0003(12) C40 0.0382(13) 0.0543(16) 0.0318(11) -0.0073(11) 0.0163(10) -0.0029(10) C41 0.075(2) 0.0491(18) 0.0587(18) -0.0096(14) 0.0306(16) 0.0003(15) C42 0.068(2) 0.0531(18) 0.0466(15) 0.0019(14) 0.0221(14) 0.0035(14) C43 0.0477(15) 0.0510(16) 0.0383(13) 0.0008(11) 0.0189(11) -0.0021(11) C44 0.0599(17) 0.0519(17) 0.0385(13) 0.0010(12) 0.0201(12) 0.0029(13) C45 0.0660(19) 0.0571(18) 0.0398(14) 0.0047(13) 0.0188(13) 0.0060(15) C46 0.0468(15) 0.0611(18) 0.0366(13) 0.0036(12) 0.0146(11) 0.0020(12) C47 0.0647(19) 0.063(2) 0.0412(14) 0.0074(14) 0.0169(13) 0.0077(14) C48 0.064(2) 0.066(2) 0.0464(16) -0.0052(15) 0.0162(14) 0.0024(16) C49 0.0507(17) 0.083(2) 0.0363(13) -0.0003(14) 0.0151(12) 0.0024(14) C50 0.0593(18) 0.074(2) 0.0367(14) 0.0126(15) 0.0170(13) 0.0079(15) C51 0.0581(17) 0.0577(18) 0.0439(14) 0.0091(13) 0.0200(13) 0.0058(13) N1 0.167(4) 0.084(2) 0.0600(19) 0.0055(19) 0.071(2) 0.011(2) N2 0.0622(16) 0.0691(18) 0.0588(15) 0.0127(13) 0.0281(13) 0.0056(13) N3 0.0497(12) 0.0488(13) 0.0330(10) -0.0009(9) 0.0228(9) -0.0006(9) N4 0.0541(13) 0.0543(13) 0.0256(9) -0.0035(9) 0.0163(9) 0.0008(10) N5 0.070(2) 0.119(3) 0.0541(16) 0.0050(17) 0.0270(15) -0.0316(18) N6 0.084(6) 0.167(10) 0.039(5) 0.000(5) 0.028(4) 0.008(6) N6A 0.115(10) 0.25(3) 0.044(7) 0.006(9) 0.044(7) 0.039(11) N7 0.0434(12) 0.0503(13) 0.0309(9) -0.0018(9) 0.0163(9) -0.0026(9) N8 0.112(2) 0.0631(18) 0.0491(15) 0.0076(14) 0.0252(15) 0.0005(16) N9 0.0679(18) 0.102(3) 0.0398(14) -0.0090(16) 0.0173(12) -0.0020(16) O1 0.0938(19) 0.109(2) 0.0983(19) 0.0228(17) 0.0655(17) 0.0123(16) O2 0.0883(18) 0.0871(19) 0.104(2) 0.0332(17) 0.0504(16) 0.0299(15) O3A 0.187(12) 0.089(5) 0.043(6) 0.008(8) 0.049(6) 0.005(8) O4 0.171(7) 0.113(7) 0.078(5) -0.012(5) 0.090(5) 0.006(6) O4A 0.194(7) 0.101(5) 0.082(4) -0.007(4) 0.094(4) 0.021(4) O5 0.0500(10) 0.0568(11) 0.0258(8) 0.0028(7) 0.0197(7) 0.0064(8) O6 0.0641(12) 0.0588(12) 0.0330(9) 0.0028(8) 0.0254(8) 0.0036(9) O7 0.110(2) 0.121(3) 0.093(2) -0.0382(19) 0.0478(19) -0.047(2) O8 0.090(2) 0.189(4) 0.121(3) -0.009(3) 0.054(2) -0.059(2) O9 0.157(10) 0.179(10) 0.080(5) 0.004(6) 0.087(7) -0.002(7) O9A 0.126(9) 0.25(2) 0.053(5) 0.016(9) 0.057(5) 0.028(10) O10 0.135(9) 0.173(10) 0.050(7) -0.029(8) 0.040(6) -0.014(8) O10A 0.118(10) 0.25(3) 0.038(6) -0.003(10) 0.040(6) 0.040(12) O11 0.0515(10) 0.0487(10) 0.0259(7) -0.0008(7) 0.0176(7) 0.0031(8) O12 0.201(4) 0.0718(19) 0.084(2) 0.0047(15) 0.065(2) 0.022(2) O13 0.214(4) 0.0733(19) 0.0668(17) 0.0159(15) 0.051(2) -0.025(2) O14 0.120(2) 0.140(3) 0.0409(12) 0.0002(16) 0.0288(14) -0.008(2) O15 0.149(3) 0.117(3) 0.0606(16) -0.0315(17) 0.0342(18) -0.019(2) Zn1 0.0530(2) 0.0509(2) 0.02427(17) -0.00168(13) 0.01722(15) -0.00023(15) Zn2 0.0498(3) 0.0517(3) 0.0241(2) 0.000 0.01857(19) 0.000 O3 0.150(13) 0.14(2) 0.040(7) -0.011(8) 0.043(7) -0.003(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.372(5) . ? C1 C6 1.378(5) . ? C1 H1 0.92(6) . ? C2 C3 1.370(5) . ? C2 N1 1.479(4) . ? C3 C4 1.379(4) . ? C3 H3 0.97(4) . ? C4 C5 1.403(4) . ? C4 N2 1.461(4) . ? C5 C6 1.395(5) . ? C5 C7 1.465(4) . ? C6 H6 0.94(5) . ? C7 C8 1.326(4) . ? C7 H7 0.95(4) . ? C8 C9 1.463(4) . ? C8 H8 0.93(3) . ? C9 N3 1.329(4) . ? C9 C10 1.413(4) . ? C10 C11 1.356(4) . ? C10 H10 0.91(4) . ? C11 C12 1.402(4) . ? C11 H11 0.89(4) . ? C12 C13 1.409(4) . ? C12 C17 1.421(4) . ? C13 C14 1.356(5) . ? C13 H13 0.96(4) . ? C14 C15 1.401(4) . ? C14 H14 0.88(3) . ? C15 C16 1.383(3) . ? C15 H15 0.93(3) . ? C16 O5 1.330(3) . ? C16 C17 1.426(4) . ? C17 N3 1.379(3) . ? C18 O6 1.303(3) . ? C18 C19 1.398(4) . ? C18 C23 1.443(4) . ? C19 C20 1.393(5) . ? C19 H19 0.93(3) . ? C20 C21 1.358(6) . ? C20 H20 1.01(4) . ? C21 C22 1.416(4) . ? C21 H21 0.94(5) . ? C22 C24 1.410(5) . ? C22 C23 1.417(4) . ? C23 N4 1.366(3) . ? C24 C25 1.355(4) . ? C24 H24 0.99(4) . ? C25 C26 1.424(4) . ? C25 H25 0.92(3) . ? C26 N4 1.326(4) . ? C26 C27 1.461(4) . ? C27 C28 1.318(4) . ? C27 H27 0.97(4) . ? C28 C29 1.464(4) . ? C28 H28 0.97(5) . ? C29 C30 1.398(4) . ? C29 C34 1.404(5) . ? C30 C31 1.391(5) . ? C30 N5 1.475(5) . ? C31 C32 1.360(6) . ? C31 H31 0.91(4) . ? C32 C33 1.373(6) . ? C32 N6A 1.453(18) . ? C32 N6 1.486(14) . ? C33 C34 1.374(4) . ? C33 H33 0.95(4) . ? C34 H34 0.98(4) . ? C35 O11 1.337(3) . ? C35 C36 1.386(3) . ? C35 C40 1.427(4) . ? C36 C37 1.402(4) . ? C36 H36 0.91(3) . ? C37 C38 1.353(5) . ? C37 H37 0.91(4) . ? C38 C39 1.414(4) . ? C38 H38 0.92(4) . ? C39 C41 1.403(4) . ? C39 C40 1.418(4) . ? C40 N7 1.372(3) . ? C41 C42 1.359(4) . ? C41 H41 0.91(4) . ? C42 C43 1.405(4) . ? C42 H42 0.84(4) . ? C43 N7 1.337(3) . ? C43 C44 1.459(4) . ? C44 C45 1.310(4) . ? C44 H44 0.87(4) . ? C45 C46 1.467(4) . ? C45 H45 0.91(5) . ? C46 C47 1.395(4) . ? C46 C51 1.406(4) . ? C47 C48 1.380(4) . ? C47 H47 0.97(4) . ? C48 C49 1.374(5) . ? C48 H48 0.92(4) . ? C49 C50 1.355(5) . ? C49 N9 1.465(4) . ? C50 C51 1.376(4) . ? C50 H50 0.86(3) . ? C51 N8 1.468(4) . ? N1 O3A 1.178(15) . ? N1 O4A 1.214(10) . ? N1 O3 1.252(19) . ? N1 O4 1.274(17) . ? N2 O2 1.211(4) . ? N2 O1 1.216(3) . ? N3 Zn2 2.253(2) . ? N4 Zn1 2.094(2) . ? N5 O8 1.210(4) . ? N5 O7 1.211(5) . ? N6 O10A 1.02(4) . ? N6 O10 1.211(13) . ? N6 O9 1.216(17) . ? N6 O9A 1.48(4) . ? N6A O9 1.06(4) . ? N6A O10A 1.23(2) . ? N6A O9A 1.227(19) . ? N6A O10 1.47(5) . ? N7 Zn1 2.139(2) . ? N8 O13 1.194(4) . ? N8 O12 1.230(4) . ? N9 O15 1.207(4) . ? N9 O14 1.216(4) . ? O4 O4A 0.642(16) . ? O5 Zn2 2.0107(15) . ? O5 Zn1 2.1440(18) . ? O6 Zn1 1.9880(17) . ? O9 O9A 0.68(3) . ? O9 O10A 1.88(4) . ? O10 O10A 0.39(6) . ? O11 Zn1 2.0340(15) . ? O11 Zn2 2.1933(18) . ? Zn2 O5 2.0107(15) 2 ? Zn2 O11 2.1933(18) 2 ? Zn2 N3 2.253(2) 2 ? 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 C2 C1 C6 118.7(3) . . ? C2 C1 H1 124(3) . . ? C6 C1 H1 117(3) . . ? C3 C2 C1 122.2(3) . . ? C3 C2 N1 118.2(3) . . ? C1 C2 N1 119.6(3) . . ? C2 C3 C4 117.7(3) . . ? C2 C3 H3 126(2) . . ? C4 C3 H3 117(2) . . ? C3 C4 C5 123.2(3) . . ? C3 C4 N2 116.6(3) . . ? C5 C4 N2 120.2(3) . . ? C6 C5 C4 115.7(3) . . ? C6 C5 C7 121.3(3) . . ? C4 C5 C7 123.0(3) . . ? C1 C6 C5 122.4(3) . . ? C1 C6 H6 115(3) . . ? C5 C6 H6 123(3) . . ? C8 C7 C5 124.9(3) . . ? C8 C7 H7 119(2) . . ? C5 C7 H7 117(2) . . ? C7 C8 C9 124.4(3) . . ? C7 C8 H8 120(2) . . ? C9 C8 H8 115(2) . . ? N3 C9 C10 121.2(2) . . ? N3 C9 C8 117.6(2) . . ? C10 C9 C8 121.2(3) . . ? C11 C10 C9 120.2(3) . . ? C11 C10 H10 121(2) . . ? C9 C10 H10 119(2) . . ? C10 C11 C12 120.7(3) . . ? C10 C11 H11 118(2) . . ? C12 C11 H11 120(2) . . ? C11 C12 C13 124.1(3) . . ? C11 C12 C17 116.6(2) . . ? C13 C12 C17 119.3(3) . . ? C14 C13 C12 119.4(3) . . ? C14 C13 H13 126(2) . . ? C12 C13 H13 115(2) . . ? C13 C14 C15 122.0(3) . . ? C13 C14 H14 123(2) . . ? C15 C14 H14 114(2) . . ? C16 C15 C14 120.8(3) . . ? C16 C15 H15 116.9(17) . . ? C14 C15 H15 122.3(17) . . ? O5 C16 C15 124.2(2) . . ? O5 C16 C17 117.9(2) . . ? C15 C16 C17 117.9(2) . . ? N3 C17 C12 122.1(2) . . ? N3 C17 C16 117.7(2) . . ? C12 C17 C16 120.2(2) . . ? O6 C18 C19 123.5(3) . . ? O6 C18 C23 120.4(2) . . ? C19 C18 C23 116.0(3) . . ? C20 C19 C18 121.3(3) . . ? C20 C19 H19 120(2) . . ? C18 C19 H19 119(2) . . ? C21 C20 C19 122.8(3) . . ? C21 C20 H20 121(2) . . ? C19 C20 H20 116(2) . . ? C20 C21 C22 119.2(3) . . ? C20 C21 H21 128(3) . . ? C22 C21 H21 113(3) . . ? C24 C22 C21 124.9(3) . . ? C24 C22 C23 116.5(3) . . ? C21 C22 C23 118.6(3) . . ? N4 C23 C22 122.0(3) . . ? N4 C23 C18 116.2(2) . . ? C22 C23 C18 121.8(2) . . ? C25 C24 C22 120.9(3) . . ? C25 C24 H24 126(2) . . ? C22 C24 H24 113(2) . . ? C24 C25 C26 119.7(3) . . ? C24 C25 H25 120(2) . . ? C26 C25 H25 120(2) . . ? N4 C26 C25 120.7(3) . . ? N4 C26 C27 115.7(2) . . ? C25 C26 C27 123.5(3) . . ? C28 C27 C26 126.9(3) . . ? C28 C27 H27 120(2) . . ? C26 C27 H27 114(2) . . ? C27 C28 C29 123.1(3) . . ? C27 C28 H28 120(3) . . ? C29 C28 H28 117(3) . . ? C30 C29 C34 116.0(3) . . ? C30 C29 C28 123.2(3) . . ? C34 C29 C28 120.8(3) . . ? C31 C30 C29 122.6(3) . . ? C31 C30 N5 117.2(3) . . ? C29 C30 N5 120.3(3) . . ? C32 C31 C30 118.0(4) . . ? C32 C31 H31 128(3) . . ? C30 C31 H31 114(3) . . ? C31 C32 C33 122.5(3) . . ? C31 C32 N6A 112.9(13) . . ? C33 C32 N6A 124.3(13) . . ? C31 C32 N6 122.4(7) . . ? C33 C32 N6 115.0(7) . . ? N6A C32 N6 12(2) . . ? C32 C33 C34 118.6(4) . . ? C32 C33 H33 124(2) . . ? C34 C33 H33 117(2) . . ? C33 C34 C29 122.3(4) . . ? C33 C34 H34 118(2) . . ? C29 C34 H34 119(2) . . ? O11 C35 C36 123.9(2) . . ? O11 C35 C40 118.4(2) . . ? C36 C35 C40 117.7(2) . . ? C35 C36 C37 120.5(3) . . ? C35 C36 H36 116.8(19) . . ? C37 C36 H36 122.5(19) . . ? C38 C37 C36 122.5(3) . . ? C38 C37 H37 123(2) . . ? C36 C37 H37 114(2) . . ? C37 C38 C39 119.4(3) . . ? C37 C38 H38 123(3) . . ? C39 C38 H38 118(3) . . ? C41 C39 C38 124.6(3) . . ? C41 C39 C40 116.7(2) . . ? C38 C39 C40 118.8(3) . . ? N7 C40 C39 122.2(2) . . ? N7 C40 C35 116.8(2) . . ? C39 C40 C35 120.9(2) . . ? C42 C41 C39 120.3(3) . . ? C42 C41 H41 124(3) . . ? C39 C41 H41 115(3) . . ? C41 C42 C43 120.6(3) . . ? C41 C42 H42 117(3) . . ? C43 C42 H42 122(3) . . ? N7 C43 C42 120.7(2) . . ? N7 C43 C44 116.6(2) . . ? C42 C43 C44 122.7(3) . . ? C45 C44 C43 126.8(3) . . ? C45 C44 H44 120(2) . . ? C43 C44 H44 113(2) . . ? C44 C45 C46 124.6(3) . . ? C44 C45 H45 118(3) . . ? C46 C45 H45 117(3) . . ? C47 C46 C51 115.0(3) . . ? C47 C46 C45 120.5(3) . . ? C51 C46 C45 124.6(3) . . ? C48 C47 C46 123.0(3) . . ? C48 C47 H47 118(2) . . ? C46 C47 H47 119(2) . . ? C49 C48 C47 118.2(3) . . ? C49 C48 H48 125(2) . . ? C47 C48 H48 116(2) . . ? C50 C49 C48 122.3(3) . . ? C50 C49 N9 118.7(3) . . ? C48 C49 N9 119.0(3) . . ? C49 C50 C51 118.3(3) . . ? C49 C50 H50 118(2) . . ? C51 C50 H50 123(2) . . ? C50 C51 C46 123.3(3) . . ? C50 C51 N8 115.2(3) . . ? C46 C51 N8 121.5(3) . . ? O3A N1 O4A 124.2(16) . . ? O3A N1 O3 13(4) . . ? O4A N1 O3 118(2) . . ? O3A N1 O4 123.8(16) . . ? O4A N1 O4 29.8(7) . . ? O3 N1 O4 125(2) . . ? O3A N1 C2 116.6(15) . . ? O4A N1 C2 118.9(6) . . ? O3 N1 C2 121(2) . . ? O4 N1 C2 113.3(8) . . ? O2 N2 O1 123.8(3) . . ? O2 N2 C4 117.7(3) . . ? O1 N2 C4 118.6(3) . . ? C9 N3 C17 119.1(2) . . ? C9 N3 Zn2 133.03(16) . . ? C17 N3 Zn2 107.80(16) . . ? C26 N4 C23 120.2(2) . . ? C26 N4 Zn1 131.61(16) . . ? C23 N4 Zn1 108.14(18) . . ? O8 N5 O7 124.6(4) . . ? O8 N5 C30 117.1(4) . . ? O7 N5 C30 118.3(3) . . ? O10A N6 O10 17(4) . . ? O10A N6 O9 114(2) . . ? O10 N6 O9 125.2(17) . . ? O10A N6 C32 129(3) . . ? O10 N6 C32 118.3(13) . . ? O9 N6 C32 115.8(12) . . ? O10A N6 O9A 117(3) . . ? O10 N6 O9A 133.8(18) . . ? O9 N6 O9A 27.0(10) . . ? C32 N6 O9A 104.6(15) . . ? O9 N6A O10A 110(3) . . ? O9 N6A O9A 33.5(15) . . ? O10A N6A O9A 121(2) . . ? O9 N6A C32 131(3) . . ? O10A N6A C32 115(2) . . ? O9A N6A C32 122(2) . . ? O9 N6A O10 116(3) . . ? O10A N6A O10 13(3) . . ? O9A N6A O10 133(2) . . ? C32 N6A O10 105(2) . . ? C43 N7 C40 119.2(2) . . ? C43 N7 Zn1 131.29(17) . . ? C40 N7 Zn1 108.82(17) . . ? O13 N8 O12 122.2(4) . . ? O13 N8 C51 118.7(3) . . ? O12 N8 C51 118.2(3) . . ? O15 N9 O14 123.0(3) . . ? O15 N9 C49 118.4(3) . . ? O14 N9 C49 118.6(3) . . ? O4A O4 N1 70(2) . . ? O4 O4A N1 80(2) . . ? C16 O5 Zn2 116.99(15) . . ? C16 O5 Zn1 138.04(14) . . ? Zn2 O5 Zn1 104.79(7) . . ? C18 O6 Zn1 111.42(17) . . ? O9A O9 N6A 87(3) . . ? O9A O9 N6 99(4) . . ? N6A O9 N6 13(4) . . ? O9A O9 O10A 104(4) . . ? N6A O9 O10A 38.1(18) . . ? N6 O9 O10A 29.5(12) . . ? O9 O9A N6A 60(3) . . ? O9 O9A N6 54(4) . . ? N6A O9A N6 7(2) . . ? O10A O10 N6 52(6) . . ? O10A O10 N6A 46(6) . . ? N6 O10 N6A 6(3) . . ? O10 O10A N6 111(9) . . ? O10 O10A N6A 121(8) . . ? N6 O10A N6A 10(4) . . ? O10 O10A O9 131(9) . . ? N6 O10A O9 36.1(18) . . ? N6A O10A O9 32.2(15) . . ? C35 O11 Zn1 112.94(14) . . ? C35 O11 Zn2 126.36(14) . . ? Zn1 O11 Zn2 102.25(7) . . ? O6 Zn1 O11 159.81(8) . . ? O6 Zn1 N4 83.13(8) . . ? O11 Zn1 N4 115.81(8) . . ? O6 Zn1 N7 99.13(8) . . ? O11 Zn1 N7 79.99(7) . . ? N4 Zn1 N7 114.36(8) . . ? O6 Zn1 O5 93.29(7) . . ? O11 Zn1 O5 76.79(6) . . ? N4 Zn1 O5 101.31(8) . . ? N7 Zn1 O5 143.28(7) . . ? O5 Zn2 O5 170.51(11) 2 . ? O5 Zn2 O11 76.14(6) 2 2 ? O5 Zn2 O11 97.11(7) . 2 ? O5 Zn2 O11 97.11(7) 2 . ? O5 Zn2 O11 76.14(6) . . ? O11 Zn2 O11 91.24(9) 2 . ? O5 Zn2 N3 78.19(7) 2 2 ? O5 Zn2 N3 108.99(7) . 2 ? O11 Zn2 N3 153.79(6) 2 2 ? O11 Zn2 N3 97.09(7) . 2 ? O5 Zn2 N3 108.99(7) 2 . ? O5 Zn2 N3 78.19(7) . . ? O11 Zn2 N3 97.09(7) 2 . ? O11 Zn2 N3 153.79(6) . . ? N3 Zn2 N3 86.29(11) 2 . ? _diffrn_measured_fraction_theta_max 0.953 _diffrn_reflns_theta_full 67.82 _diffrn_measured_fraction_theta_full 0.952 _refine_diff_density_max 0.717 _refine_diff_density_min -0.379 _refine_diff_density_rms 0.057 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.500 -0.011 160 18 ' ' 2 0.500 0.000 0.020 160 18 ' ' 3 0.458 0.354 0.075 19 1 ' ' 4 0.958 0.854 0.075 19 1 ' ' 5 0.500 0.224 0.250 17 1 ' ' 6 1.000 0.724 0.250 17 1 ' ' 7 0.042 0.854 0.424 19 1 ' ' 8 0.542 0.354 0.424 19 1 ' ' 9 0.458 0.646 0.575 19 1 ' ' 10 0.958 0.146 0.575 19 1 ' ' 11 0.500 0.776 0.750 18 1 ' ' 12 1.000 0.276 0.750 18 1 ' ' 13 0.042 0.146 0.924 19 1 ' ' 14 0.542 0.646 0.924 19 1 ' ' _platon_squeeze_details ; ; data_hl2 _database_code_depnum_ccdc_archive 'CCDC 894164' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C17 H11 N3 O5' _chemical_formula_weight 337.29 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 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' 'N' 'N' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 22.1420(15) _cell_length_b 8.6629(6) _cell_length_c 15.6854(9) _cell_angle_alpha 90.00 _cell_angle_beta 91.506(4) _cell_angle_gamma 90.00 _cell_volume 3007.6(3) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 2668 _cell_measurement_theta_min 3.99 _cell_measurement_theta_max 68.17 _exptl_crystal_description Block _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.490 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1392 _exptl_absorpt_coefficient_mu 0.951 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7901 _exptl_absorpt_correction_T_max 0.8944 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX area-detector diffractometer' _diffrn_measurement_method '\f and \w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6469 _diffrn_reflns_av_R_equivalents 0.0281 _diffrn_reflns_av_sigmaI/netI 0.0384 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.99 _diffrn_reflns_theta_max 68.17 _reflns_number_total 2668 _reflns_number_gt 2343 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1997)' _computing_cell_refinement 'SAINT (Bruker, 1999)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL-PLUS (Sheldrick, 1990)' _computing_publication_material SHELXL-97 _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0690P)^2^+0.9513P] 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 2668 _refine_ls_number_parameters 270 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0536 _refine_ls_R_factor_gt 0.0395 _refine_ls_wR_factor_ref 0.1217 _refine_ls_wR_factor_gt 0.1175 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.055 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group N1 N 0.45649(5) 0.15995(13) 0.02281(7) 0.0427(3) Uani 1 1 d . . . C1 C 0.49270(7) 0.21897(15) -0.03467(8) 0.0429(3) Uani 1 1 d . . . C5 C 0.40952(6) 0.07153(15) -0.00507(9) 0.0443(3) Uani 1 1 d . . . C11 C 0.55393(7) 0.35812(16) 0.07416(8) 0.0434(3) Uani 1 1 d . . . C15 C 0.69857(7) 0.65150(16) 0.15710(9) 0.0479(3) Uani 1 1 d . . . N3 N 0.74782(7) 0.75361(16) 0.18531(9) 0.0606(4) Uani 1 1 d . . . N2 N 0.58522(6) 0.40719(16) 0.25708(7) 0.0533(3) Uani 1 1 d . . . O1 O 0.38460(7) 0.03673(17) 0.14164(7) 0.0691(4) Uani 1 1 d . . . O2 O 0.57049(6) 0.27328(14) 0.24877(7) 0.0685(4) Uani 1 1 d . . . C16 C 0.66429(7) 0.58102(16) 0.21720(9) 0.0467(3) Uani 1 1 d . . . C17 C 0.61872(6) 0.48342(16) 0.18945(8) 0.0420(3) Uani 1 1 d . . . C12 C 0.60435(6) 0.45563(15) 0.10299(8) 0.0410(3) Uani 1 1 d . . . C10 C 0.54355(7) 0.31504(17) -0.00577(9) 0.0454(3) Uani 1 1 d . . . C2 C 0.48354(8) 0.19104(18) -0.12354(9) 0.0532(4) Uani 1 1 d . . . C6 C 0.37167(7) 0.00849(19) 0.05800(10) 0.0536(4) Uani 1 1 d . . . C3 C 0.43648(8) 0.10268(19) -0.15128(9) 0.0560(4) Uani 1 1 d . . . O5 O 0.78045(7) 0.80927(17) 0.13186(9) 0.0805(4) Uani 1 1 d . . . C13 C 0.64010(7) 0.53571(19) 0.04514(9) 0.0512(4) Uani 1 1 d . . . C4 C 0.39672(7) 0.03904(16) -0.09241(9) 0.0489(4) Uani 1 1 d . . . C14 C 0.68681(8) 0.63005(19) 0.07076(10) 0.0544(4) Uani 1 1 d . . . O4 O 0.75407(8) 0.77831(19) 0.26169(9) 0.0906(5) Uani 1 1 d . . . C9 C 0.34566(8) -0.0522(2) -0.11482(11) 0.0615(4) Uani 1 1 d . . . O3 O 0.57517(9) 0.4823(2) 0.32066(9) 0.1009(6) Uani 1 1 d . . . C7 C 0.32266(8) -0.0792(2) 0.03451(13) 0.0678(5) Uani 1 1 d . . . C8 C 0.30996(9) -0.1081(2) -0.05272(14) 0.0701(5) Uani 1 1 d . . . H16 H 0.6735(8) 0.593(2) 0.2733(12) 0.064(5) Uiso 1 1 d . . . H11 H 0.5275(8) 0.324(2) 0.1173(11) 0.060(5) Uiso 1 1 d . . . H3 H 0.4300(9) 0.086(2) -0.2122(12) 0.068(5) Uiso 1 1 d . . . H9 H 0.3374(9) -0.068(2) -0.1787(13) 0.072(6) Uiso 1 1 d . . . H10 H 0.5679(9) 0.343(2) -0.0492(12) 0.067(5) Uiso 1 1 d . . . H13 H 0.6314(9) 0.527(2) -0.0157(12) 0.068(5) Uiso 1 1 d . . . H14 H 0.7096(9) 0.682(2) 0.0314(13) 0.069(5) Uiso 1 1 d . . . H2 H 0.5106(9) 0.234(2) -0.1597(12) 0.060(5) Uiso 1 1 d . . . H7 H 0.2972(10) -0.120(3) 0.0783(14) 0.078(6) Uiso 1 1 d . . . H8 H 0.2760(11) -0.165(3) -0.0683(13) 0.081(6) Uiso 1 1 d . . . H1 H 0.4141(12) 0.100(3) 0.1451(15) 0.094(8) 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 N1 0.0482(7) 0.0412(6) 0.0387(6) -0.0020(4) -0.0030(5) 0.0024(5) C1 0.0531(8) 0.0392(7) 0.0363(6) 0.0008(5) -0.0025(5) 0.0039(6) C5 0.0469(8) 0.0395(7) 0.0463(7) -0.0046(5) -0.0044(6) 0.0052(6) C11 0.0465(8) 0.0461(7) 0.0377(6) 0.0013(5) 0.0025(5) -0.0003(6) C15 0.0473(8) 0.0427(7) 0.0534(8) 0.0028(6) -0.0080(6) -0.0002(6) N3 0.0586(8) 0.0554(8) 0.0669(8) 0.0067(6) -0.0148(7) -0.0077(6) N2 0.0635(8) 0.0607(8) 0.0360(6) 0.0000(5) 0.0043(5) -0.0036(6) O1 0.0762(9) 0.0825(9) 0.0491(6) -0.0036(6) 0.0088(5) -0.0209(7) O2 0.0946(10) 0.0595(7) 0.0515(6) 0.0111(5) 0.0035(6) -0.0166(6) C16 0.0543(8) 0.0456(7) 0.0400(7) -0.0003(5) -0.0072(6) 0.0042(6) C17 0.0469(8) 0.0428(7) 0.0363(6) 0.0016(5) 0.0020(5) 0.0048(5) C12 0.0452(7) 0.0409(6) 0.0369(6) 0.0007(5) 0.0016(5) 0.0049(5) C10 0.0528(8) 0.0463(7) 0.0373(6) 0.0034(5) 0.0024(6) -0.0022(6) C2 0.0687(10) 0.0550(8) 0.0358(7) 0.0008(6) -0.0006(6) -0.0036(7) C6 0.0539(9) 0.0545(8) 0.0526(8) -0.0056(6) 0.0024(6) -0.0009(7) C3 0.0726(11) 0.0565(9) 0.0383(7) -0.0059(6) -0.0097(7) 0.0027(8) O5 0.0704(9) 0.0840(9) 0.0868(9) 0.0070(7) -0.0022(7) -0.0286(7) C13 0.0577(9) 0.0594(9) 0.0365(7) 0.0023(6) 0.0005(6) -0.0075(7) C4 0.0543(8) 0.0438(7) 0.0481(7) -0.0064(6) -0.0097(6) 0.0073(6) C14 0.0586(10) 0.0571(9) 0.0476(8) 0.0074(6) 0.0037(7) -0.0103(7) O4 0.1038(11) 0.0987(11) 0.0676(8) 0.0012(7) -0.0285(8) -0.0404(9) C9 0.0600(10) 0.0587(9) 0.0647(10) -0.0140(7) -0.0168(8) 0.0027(7) O3 0.1420(15) 0.1030(11) 0.0599(7) -0.0269(7) 0.0467(9) -0.0308(10) C7 0.0593(11) 0.0690(11) 0.0755(11) -0.0079(9) 0.0077(9) -0.0121(8) C8 0.0531(10) 0.0687(11) 0.0880(13) -0.0181(9) -0.0081(9) -0.0094(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N1 C1 1.3248(18) . ? N1 C5 1.3550(18) . ? C1 C2 1.4241(18) . ? C1 C10 1.462(2) . ? C5 C4 1.4198(19) . ? C5 C6 1.422(2) . ? C11 C10 1.3225(19) . ? C11 C12 1.462(2) . ? C11 H11 0.954(19) . ? C15 C16 1.369(2) . ? C15 C14 1.385(2) . ? C15 N3 1.4635(19) . ? N3 O5 1.2203(19) . ? N3 O4 1.2213(19) . ? N2 O2 1.2112(18) . ? N2 O3 1.2163(18) . ? N2 C17 1.4673(18) . ? O1 C6 1.3576(19) . ? O1 H1 0.85(3) . ? C16 C17 1.378(2) . ? C16 H16 0.903(19) . ? C17 C12 1.4056(18) . ? C12 C13 1.403(2) . ? C10 H10 0.91(2) . ? C2 C3 1.356(2) . ? C2 H2 0.914(19) . ? C6 C7 1.367(2) . ? C3 C4 1.405(2) . ? C3 H3 0.973(19) . ? C13 C14 1.370(2) . ? C13 H13 0.972(19) . ? C4 C9 1.416(2) . ? C14 H14 0.92(2) . ? C9 C8 1.360(3) . ? C9 H9 1.02(2) . ? C7 C8 1.412(3) . ? C7 H7 0.97(2) . ? C8 H8 0.92(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 N1 C5 118.14(11) . . ? N1 C1 C2 121.83(13) . . ? N1 C1 C10 118.91(11) . . ? C2 C1 C10 119.26(13) . . ? N1 C5 C4 123.75(13) . . ? N1 C5 C6 116.99(12) . . ? C4 C5 C6 119.26(13) . . ? C10 C11 C12 124.65(13) . . ? C10 C11 H11 119.4(11) . . ? C12 C11 H11 115.9(11) . . ? C16 C15 C14 121.33(14) . . ? C16 C15 N3 118.91(13) . . ? C14 C15 N3 119.75(14) . . ? O5 N3 O4 123.43(14) . . ? O5 N3 C15 118.75(14) . . ? O4 N3 C15 117.82(14) . . ? O2 N2 O3 123.11(14) . . ? O2 N2 C17 119.55(12) . . ? O3 N2 C17 117.31(14) . . ? C6 O1 H1 108.6(17) . . ? C15 C16 C17 118.07(13) . . ? C15 C16 H16 120.2(12) . . ? C17 C16 H16 121.5(12) . . ? C16 C17 C12 123.72(13) . . ? C16 C17 N2 115.32(11) . . ? C12 C17 N2 120.96(12) . . ? C13 C12 C17 114.96(13) . . ? C13 C12 C11 121.65(12) . . ? C17 C12 C11 123.30(12) . . ? C11 C10 C1 124.59(13) . . ? C11 C10 H10 122.8(12) . . ? C1 C10 H10 112.6(12) . . ? C3 C2 C1 119.91(15) . . ? C3 C2 H2 122.7(11) . . ? C1 C2 H2 117.4(12) . . ? O1 C6 C7 120.42(15) . . ? O1 C6 C5 119.34(14) . . ? C7 C6 C5 120.25(15) . . ? C2 C3 C4 120.02(13) . . ? C2 C3 H3 119.3(11) . . ? C4 C3 H3 120.7(11) . . ? C14 C13 C12 122.65(13) . . ? C14 C13 H13 117.6(12) . . ? C12 C13 H13 119.8(12) . . ? C3 C4 C9 124.45(14) . . ? C3 C4 C5 116.34(13) . . ? C9 C4 C5 119.20(15) . . ? C13 C14 C15 119.20(14) . . ? C13 C14 H14 121.0(13) . . ? C15 C14 H14 119.8(13) . . ? C8 C9 C4 119.76(15) . . ? C8 C9 H9 124.3(11) . . ? C4 C9 H9 115.9(11) . . ? C6 C7 C8 119.75(17) . . ? C6 C7 H7 119.0(13) . . ? C8 C7 H7 121.3(13) . . ? C9 C8 C7 121.75(16) . . ? C9 C8 H8 118.9(13) . . ? C7 C8 H8 119.3(13) . . ? _diffrn_measured_fraction_theta_max 0.967 _diffrn_reflns_theta_full 68.17 _diffrn_measured_fraction_theta_full 0.967 _refine_diff_density_max 0.252 _refine_diff_density_min -0.172 _refine_diff_density_rms 0.035