Electronic Supplementary Material for CrystEngComm This Journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 _publ_contact_author_name 'Konarev, Dmitry V.' _publ_contact_author_address ; Institute of Problems of Chemical Physics, RAS, Chernogolovka, 142432, Russia ; _publ_contact_author_email konarev@icp.ac.ru loop_ _publ_author_name _publ_author_address D.V.Konarev ; Institute of Problems of Chemical Physics, RAS, Chernogolovka, 142432, Russia konarev@icp.ac.ru ; S.S.Khasanov ; Institute of Solid State Physics, RAS, Chernogolovka, 142432, Russia e-mail: khasanov@issp.ac.ru ; A.Yu.Kovalevsky ? L.S.Yu ; Institute of Organoelement Compounds RAS, 28 Vavilov St., 119991, Moscow, Russia. State University of New York at Buffalo, Buffalo, New York, 14260 USA ; A.Otsuka ; Division of chemistry, Graduate School of Science, Kyoto University, Sakyo-ku, Kyoto 606-8502, Japan ; ; G.Saito ; ; Division of chemistry, Graduate School of Science, Kyoto University, Sakyo-ku, Kyoto 606-8502, Japan ; R.N.Lyubovskaya ; Institute of Problems of Chemical Physics, RAS, Chernogolovka, 142432, Russia ; _publ_section_title ; Neutral and ionic complexes of C60 with ZnOEP2BPy dimers. ; data_ZnOEP_BPy_C60 _database_code_depnum_ccdc_archive 'CCDC 648658' _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common C60*(ZnOEP2.BPy)0.5*CHCl3 _chemical_melting_point ? _chemical_formula_moiety 'C60, C36H44N4Zn, (C10H8N2)0.5, CHCl3' _chemical_formula_sum 'C204 H98 Cl6 N10 Zn2' _chemical_formula_weight 3032.36 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.847(9) _cell_length_b 14.011(11) _cell_length_c 19.795(16) _cell_angle_alpha 78.50(3) _cell_angle_beta 76.35(3) _cell_angle_gamma 63.27(2) _cell_volume 3314(4) _cell_formula_units_Z 1 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 8834 _cell_measurement_theta_min 4 _cell_measurement_theta_max 28 _exptl_crystal_description prism _exptl_crystal_colour black _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.519 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1554 _exptl_absorpt_coefficient_mu 0.555 _exptl_absorpt_correction_type MULTISCAN _exptl_absorpt_correction_T_min 0.8512 _exptl_absorpt_correction_T_max 0.8971 _exptl_absorpt_process_details 'SADABS; Sheldrick, 1997' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(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 SMART' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26298 _diffrn_reflns_av_R_equivalents 0.1375 _diffrn_reflns_av_sigmaI/netI 0.1460 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.64 _diffrn_reflns_theta_max 30.04 _reflns_number_total 18271 _reflns_number_gt 10828 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Disordered fullerene molecules show relatively strong correlations for atomic parameters (coordinates, displacements). In general, it is needed to impose DFIX and SADI instructions of SHELXL to keep interatomic distances close to mean value. Further, it is essential to consider anisotropic thermal parameters for the fullerene carbon atoms to approximate fullerene molecular form factor correctly. These displacements are restrained by ISOR, DELU and SIMU instructions of SHELXL.Such approach resulted in large number of restraints. ; _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^)+(0.1444P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 18271 _refine_ls_number_parameters 1238 _refine_ls_number_restraints 8840 _refine_ls_R_factor_all 0.1366 _refine_ls_R_factor_gt 0.0917 _refine_ls_wR_factor_ref 0.2453 _refine_ls_wR_factor_gt 0.2181 _refine_ls_goodness_of_fit_ref 0.951 _refine_ls_restrained_S_all 0.848 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 1.30051(3) 0.32494(3) 1.365928(17) 0.01734(10) Uani 1 1 d . . . N1 N 1.4345(2) 0.17830(19) 1.35175(13) 0.0193(5) Uani 1 1 d . . . N2 N 1.2236(2) 0.24431(19) 1.44155(12) 0.0188(5) Uani 1 1 d . . . N3 N 1.14780(19) 0.45228(18) 1.35830(12) 0.0173(5) Uani 1 1 d . . . N4 N 1.3610(2) 0.38714(18) 1.26902(13) 0.0189(5) Uani 1 1 d . . . C1 C 1.5377(2) 0.2332(2) 1.24467(16) 0.0216(6) Uani 1 1 d . . . H1 H 1.6071 0.2110 1.2150 0.026 Uiso 1 1 calc R . . C2 C 1.5241(2) 0.1581(2) 1.29941(15) 0.0201(6) Uani 1 1 d . . . C3 C 1.5990(2) 0.0454(2) 1.30567(16) 0.0237(6) Uani 1 1 d . . . C4 C 1.5526(2) -0.0028(2) 1.36242(17) 0.0246(6) Uani 1 1 d . . . C5 C 1.4503(2) 0.0818(2) 1.39064(15) 0.0203(6) Uani 1 1 d . . . C6 C 1.3756(3) 0.0660(2) 1.44834(16) 0.0231(6) Uani 1 1 d . . . H6 H 1.3996 -0.0028 1.4746 0.028 Uiso 1 1 calc R . . C7 C 1.2697(2) 0.1411(2) 1.47092(15) 0.0212(6) Uani 1 1 d . . . C8 C 1.1912(3) 0.1172(2) 1.52619(15) 0.0222(6) Uani 1 1 d . . . C9 C 1.0958(3) 0.2074(2) 1.52762(15) 0.0212(6) Uani 1 1 d . . . C10 C 1.1154(3) 0.2862(2) 1.47389(15) 0.0224(6) Uani 1 1 d . . . C11 C 1.0361(3) 0.3877(2) 1.45465(16) 0.0235(6) Uani 1 1 d . . . H11 H 0.9648 0.4079 1.4819 0.028 Uiso 1 1 calc R . . C12 C 1.0498(2) 0.4623(2) 1.40005(16) 0.0222(6) Uani 1 1 d . . . C13 C 0.9604(3) 0.5611(2) 1.37689(17) 0.0258(6) Uani 1 1 d . . . C14 C 1.0070(3) 0.6099(2) 1.32099(18) 0.0260(6) Uani 1 1 d . . . C15 C 1.1242(3) 0.5399(2) 1.30974(16) 0.0234(6) Uani 1 1 d . . . C16 C 1.2000(3) 0.5571(2) 1.25370(16) 0.0228(6) Uani 1 1 d . . . H16 H 1.1755 0.6254 1.2269 0.027 Uiso 1 1 calc R . . C17 C 1.3072(3) 0.4845(2) 1.23330(16) 0.0219(6) Uani 1 1 d . . . C18 C 1.3764(3) 0.4967(2) 1.16649(16) 0.0242(6) Uani 1 1 d . . . C19 C 1.4709(3) 0.4052(2) 1.16399(17) 0.0239(6) Uani 1 1 d . . . C20 C 1.4603(2) 0.3373(2) 1.22877(16) 0.0210(6) Uani 1 1 d . . . C21 C 1.7042(3) -0.0049(3) 1.25581(19) 0.0347(8) Uani 1 1 d . . . H21A H 1.7537 -0.0725 1.2796 0.042 Uiso 1 1 calc R . . H21B H 1.7408 0.0443 1.2432 0.042 Uiso 1 1 calc R . . C22 C 1.6867(4) -0.0290(3) 1.1895(2) 0.0492(11) Uani 1 1 d . . . H22A H 1.7575 -0.0610 1.1590 0.074 Uiso 1 1 calc R . . H22B H 1.6388 0.0378 1.1652 0.074 Uiso 1 1 calc R . . H22C H 1.6524 -0.0794 1.2014 0.074 Uiso 1 1 calc R . . C23 C 1.5923(3) -0.1199(3) 1.38813(19) 0.0310(7) Uani 1 1 d . . . H23A H 1.5760 -0.1284 1.4399 0.037 Uiso 1 1 calc R . . H23B H 1.6728 -0.1559 1.3739 0.037 Uiso 1 1 calc R . . C24 C 1.5384(4) -0.1744(3) 1.3594(2) 0.0494(11) Uani 1 1 d . . . H24A H 1.5662 -0.2506 1.3775 0.074 Uiso 1 1 calc R . . H24B H 1.5559 -0.1678 1.3082 0.074 Uiso 1 1 calc R . . H24C H 1.4587 -0.1397 1.3739 0.074 Uiso 1 1 calc R . . C25 C 1.2143(3) 0.0101(3) 1.56893(17) 0.0285(7) Uani 1 1 d . . . H25A H 1.1619 0.0208 1.6135 0.034 Uiso 1 1 calc R . . H25B H 1.2891 -0.0202 1.5803 0.034 Uiso 1 1 calc R . . C26 C 1.2054(4) -0.0707(3) 1.5318(2) 0.0433(9) Uani 1 1 d . . . H26A H 1.2214 -0.1387 1.5620 0.065 Uiso 1 1 calc R . . H26B H 1.2582 -0.0831 1.4881 0.065 Uiso 1 1 calc R . . H26C H 1.1310 -0.0422 1.5214 0.065 Uiso 1 1 calc R . . C27 C 0.9856(3) 0.2242(3) 1.57237(17) 0.0288(7) Uani 1 1 d . . . H27A H 0.9477 0.2989 1.5849 0.035 Uiso 1 1 calc R . . H27B H 0.9972 0.1752 1.6162 0.035 Uiso 1 1 calc R . . C28 C 0.9120(3) 0.2037(3) 1.5351(2) 0.0387(8) Uani 1 1 d . . . H28A H 0.8419 0.2154 1.5660 0.058 Uiso 1 1 calc R . . H28B H 0.9485 0.1295 1.5233 0.058 Uiso 1 1 calc R . . H28C H 0.8988 0.2533 1.4922 0.058 Uiso 1 1 calc R . . C29 C 0.8412(3) 0.5944(3) 1.4079(2) 0.0326(8) Uani 1 1 d . . . H29A H 0.8014 0.6734 1.3987 0.039 Uiso 1 1 calc R . . H29B H 0.8343 0.5758 1.4593 0.039 Uiso 1 1 calc R . . C30 C 0.7876(3) 0.5405(4) 1.3783(2) 0.0462(10) Uani 1 1 d . . . H30A H 0.7104 0.5645 1.4003 0.069 Uiso 1 1 calc R . . H30B H 0.8258 0.4623 1.3880 0.069 Uiso 1 1 calc R . . H30C H 0.7922 0.5602 1.3277 0.069 Uiso 1 1 calc R . . C31 C 0.9512(3) 0.7122(3) 1.2762(2) 0.0376(8) Uani 1 1 d . . . H31A H 0.9979 0.7518 1.2633 0.045 Uiso 1 1 calc R . . H31B H 0.8810 0.7579 1.3035 0.045 Uiso 1 1 calc R . . C32 C 0.9288(4) 0.6926(3) 1.2098(2) 0.0555(12) Uani 1 1 d . . . H32A H 0.8929 0.7616 1.1825 0.083 Uiso 1 1 calc R . . H32B H 0.8809 0.6552 1.2221 0.083 Uiso 1 1 calc R . . H32C H 0.9982 0.6483 1.1820 0.083 Uiso 1 1 calc R . . C33 C 1.3415(3) 0.5918(3) 1.11194(19) 0.0310(7) Uani 1 1 d . . . H33A H 1.4076 0.5947 1.0805 0.037 Uiso 1 1 calc R . . H33B H 1.3027 0.6585 1.1353 0.037 Uiso 1 1 calc R . . C34 C 1.2662(3) 0.5870(3) 1.0681(2) 0.0382(8) Uani 1 1 d . . . H34A H 1.2464 0.6501 1.0332 0.057 Uiso 1 1 calc R . . H34B H 1.1996 0.5863 1.0987 0.057 Uiso 1 1 calc R . . H34C H 1.3045 0.5216 1.0443 0.057 Uiso 1 1 calc R . . C35 C 1.5669(3) 0.3720(3) 1.10488(18) 0.0297(7) Uani 1 1 d . . . H35A H 1.6358 0.3393 1.1243 0.036 Uiso 1 1 calc R . . H35B H 1.5654 0.4368 1.0732 0.036 Uiso 1 1 calc R . . C36 C 1.5664(3) 0.2919(3) 1.06262(19) 0.0363(8) Uani 1 1 d . . . H36A H 1.6302 0.2732 1.0251 0.054 Uiso 1 1 calc R . . H36B H 1.4991 0.3244 1.0423 0.054 Uiso 1 1 calc R . . H36C H 1.5695 0.2268 1.0934 0.054 Uiso 1 1 calc R . . N5 N 1.3679(2) 0.3878(2) 1.42569(14) 0.0245(5) Uani 1 1 d . . . C42 C 1.3267(3) 0.4919(3) 1.4309(3) 0.0605(15) Uani 1 1 d . . . H42 H 1.2605 0.5375 1.4134 0.073 Uiso 1 1 calc R . . C43 C 1.3742(4) 0.5381(3) 1.4601(3) 0.0704(19) Uani 1 1 d . . . H43 H 1.3392 0.6133 1.4633 0.085 Uiso 1 1 calc R . . C44 C 1.4722(3) 0.4763(2) 1.48498(18) 0.0260(7) Uani 1 1 d . . . C45 C 1.5117(3) 0.3672(3) 1.4826(2) 0.0370(9) Uani 1 1 d . . . H45 H 1.5755 0.3189 1.5018 0.044 Uiso 1 1 calc R . . C46 C 1.4581(3) 0.3276(3) 1.4521(2) 0.0382(9) Uani 1 1 d . . . H46 H 1.4888 0.2522 1.4501 0.046 Uiso 1 1 calc R . . C301 C 1.0986(3) 0.3722(3) 1.0309(2) 0.0516(13) Uani 0.488(3) 1 d PDU A 1 C302 C 1.0704(3) 0.4185(4) 1.09628(17) 0.0450(11) Uani 0.488(3) 1 d PDU A 1 C303 C 0.9630(3) 0.4241(4) 1.1304(2) 0.0427(9) Uani 0.488(3) 1 d PDU A 1 C304 C 0.9260(4) 0.3812(3) 1.08574(19) 0.0437(10) Uani 0.488(3) 1 d PDU A 1 C305 C 1.0088(3) 0.3499(3) 1.0238(3) 0.0468(10) Uani 0.488(3) 1 d PDU A 1 C306 C 1.2059(3) 0.3025(4) 1.0083(2) 0.0531(12) Uani 0.488(3) 1 d PDU A 1 C307 C 1.2282(3) 0.2074(2) 0.9772(3) 0.0496(12) Uani 0.488(3) 1 d PDU A 1 C308 C 1.3270(3) 0.1212(3) 0.9994(2) 0.0478(11) Uani 0.488(3) 1 d PDU A 1 C309 C 1.3636(4) 0.1644(3) 1.04422(19) 0.0452(11) Uani 0.488(3) 1 d PDU A 1 C310 C 1.2902(3) 0.2773(3) 1.04946(19) 0.0490(12) Uani 0.488(3) 1 d PDU A 1 C311 C 1.1502(3) 0.3932(4) 1.13593(18) 0.0481(11) Uani 0.488(3) 1 d PDU A 1 C312 C 1.2630(3) 0.3193(3) 1.1124(2) 0.0487(11) Uani 0.488(3) 1 d PDU A 1 C313 C 1.3112(4) 0.2521(3) 1.17250(17) 0.0478(11) Uani 0.488(3) 1 d PDU A 1 C314 C 1.2261(3) 0.2843(3) 1.2333(2) 0.0507(11) Uani 0.488(3) 1 d PDU A 1 C315 C 1.1274(3) 0.3717(4) 1.21152(19) 0.0510(12) Uani 0.488(3) 1 d PDU A 1 C316 C 0.9411(3) 0.4034(5) 1.2024(2) 0.0433(9) Uani 0.488(3) 1 d PDU A 1 C317 C 1.0252(3) 0.3772(4) 1.24403(19) 0.0475(10) Uani 0.488(3) 1 d PDU A 1 C318 C 1.0166(3) 0.2955(3) 1.3004(3) 0.0513(12) Uani 0.488(3) 1 d PDU A 1 C319 C 0.9265(3) 0.2728(3) 1.2942(3) 0.0503(12) Uani 0.488(3) 1 d PDU A 1 C320 C 0.8796(5) 0.3397(3) 1.23349(19) 0.0467(9) Uani 0.488(3) 1 d PDU A 1 C321 C 0.8670(4) 0.3210(4) 1.1152(2) 0.0456(10) Uani 0.488(3) 1 d PDU A 1 C322 C 0.8436(4) 0.2995(3) 1.1910(2) 0.0457(10) Uani 0.488(3) 1 d PDU A 1 C323 C 0.8516(4) 0.1904(3) 1.2076(2) 0.0432(10) Uani 0.488(3) 1 d PDU A 1 C324 C 0.8801(3) 0.1458(3) 1.14161(16) 0.0441(10) Uani 0.488(3) 1 d PDU A 1 C325 C 0.8886(3) 0.2261(3) 1.0845(2) 0.0451(10) Uani 0.488(3) 1 d PDU A 1 C326 C 1.0303(3) 0.2587(4) 0.9949(2) 0.0482(12) Uani 0.488(3) 1 d PDU A 1 C327 C 0.9682(4) 0.1955(3) 1.02572(19) 0.0523(11) Uani 0.488(3) 1 d PDU A 1 C328 C 1.0445(3) 0.0832(3) 1.0217(2) 0.0562(12) Uani 0.488(3) 1 d PDU A 1 C329 C 1.1522(3) 0.0760(3) 0.9872(2) 0.0530(12) Uani 0.488(3) 1 d PDU A 1 C330 C 1.1429(3) 0.1854(3) 0.9712(3) 0.0486(12) Uani 0.488(3) 1 d PDU A 1 C331 C 1.1624(3) -0.0825(4) 1.2791(2) 0.0516(13) Uani 0.488(3) 1 d PDU A 1 C332 C 1.1913(3) -0.1284(4) 1.21353(17) 0.0450(11) Uani 0.488(3) 1 d PDU A 1 C333 C 1.2997(3) -0.1360(4) 1.1793(2) 0.0427(9) Uani 0.488(3) 1 d PDU A 1 C334 C 1.3360(5) -0.0921(4) 1.22404(19) 0.0437(10) Uani 0.488(3) 1 d PDU A 1 C335 C 1.2525(3) -0.0599(3) 1.2856(3) 0.0468(10) Uani 0.488(3) 1 d PDU A 1 C336 C 1.0553(3) -0.0118(4) 1.3011(2) 0.0531(12) Uani 0.488(3) 1 d PDU A 1 C337 C 1.0334(3) 0.0827(2) 1.3327(3) 0.0496(12) Uani 0.488(3) 1 d PDU A 1 C338 C 0.9352(3) 0.1685(3) 1.3096(2) 0.0478(11) Uani 0.488(3) 1 d PDU A 1 C339 C 0.8972(4) 0.1265(3) 1.26497(18) 0.0452(11) Uani 0.488(3) 1 d PDU A 1 C340 C 0.9711(3) 0.0137(3) 1.25976(18) 0.0490(12) Uani 0.488(3) 1 d PDU A 1 C341 C 1.1115(3) -0.1034(4) 1.17393(18) 0.0481(11) Uani 0.488(3) 1 d PDU A 1 C342 C 0.9989(3) -0.0285(3) 1.1968(2) 0.0487(11) Uani 0.488(3) 1 d PDU A 1 C343 C 0.9505(4) 0.0383(3) 1.13671(16) 0.0478(11) Uani 0.488(3) 1 d PDU A 1 C344 C 1.0353(3) 0.0064(3) 1.0756(2) 0.0507(11) Uani 0.488(3) 1 d PDU A 1 C345 C 1.1336(3) -0.0806(4) 1.09843(19) 0.0510(12) Uani 0.488(3) 1 d PDU A 1 C346 C 1.3207(3) -0.1143(4) 1.1074(2) 0.0433(9) Uani 0.488(3) 1 d PDU A 1 C347 C 1.2362(3) -0.0870(4) 1.06591(19) 0.0475(10) Uani 0.488(3) 1 d PDU A 1 C348 C 1.2456(3) -0.0060(3) 1.0092(3) 0.0513(12) Uani 0.488(3) 1 d PDU A 1 C349 C 1.3355(3) 0.0172(3) 1.0150(3) 0.0503(12) Uani 0.488(3) 1 d PDU A 1 C350 C 1.3806(5) -0.0489(3) 1.0764(2) 0.0467(9) Uani 0.488(3) 1 d PDU A 1 C351 C 1.3944(4) -0.0312(4) 1.1944(2) 0.0456(10) Uani 0.488(3) 1 d PDU A 1 C352 C 1.4159(4) -0.0080(4) 1.1189(2) 0.0457(10) Uani 0.488(3) 1 d PDU A 1 C353 C 1.4095(4) 0.1004(3) 1.1015(2) 0.0432(10) Uani 0.488(3) 1 d PDU A 1 C354 C 1.3811(3) 0.1445(3) 1.16764(16) 0.0441(10) Uani 0.488(3) 1 d PDU A 1 C355 C 1.3720(3) 0.0643(3) 1.2248(2) 0.0451(10) Uani 0.488(3) 1 d PDU A 1 C356 C 1.2316(3) 0.0307(4) 1.3149(2) 0.0482(12) Uani 0.488(3) 1 d PDU A 1 C357 C 1.2923(4) 0.0951(3) 1.28338(19) 0.0523(11) Uani 0.488(3) 1 d PDU A 1 C358 C 1.2177(3) 0.2079(3) 1.2879(2) 0.0562(12) Uani 0.488(3) 1 d PDU A 1 C359 C 1.1102(3) 0.2136(3) 1.3220(2) 0.0530(12) Uani 0.488(3) 1 d PDU A 1 C360 C 1.1189(3) 0.1044(3) 1.3386(3) 0.0486(12) Uani 0.488(3) 1 d PDU A 1 C401 C 0.8863(4) 0.1684(3) 1.2669(3) 0.0447(11) Uani 0.512(3) 1 d PDU A 2 C402 C 0.8502(5) 0.2006(3) 1.1993(2) 0.0441(10) Uani 0.512(3) 1 d PDU A 2 C403 C 0.8443(5) 0.3079(4) 1.1748(2) 0.0469(10) Uani 0.512(3) 1 d PDU A 2 C404 C 0.8765(5) 0.3409(5) 1.2277(3) 0.0470(9) Uani 0.512(3) 1 d PDU A 2 C405 C 0.9020(4) 0.2554(3) 1.2850(3) 0.0422(10) Uani 0.512(3) 1 d PDU A 2 C406 C 0.9571(4) 0.0629(3) 1.2839(2) 0.0417(10) Uani 0.512(3) 1 d PDU A 2 C407 C 1.0463(3) 0.0399(3) 1.3202(3) 0.0453(11) Uani 0.512(3) 1 d PDU A 2 C408 C 1.1401(3) -0.0534(4) 1.2931(3) 0.0424(10) Uani 0.512(3) 1 d PDU A 2 C409 C 1.1074(3) -0.0859(4) 1.2401(2) 0.0448(10) Uani 0.512(3) 1 d PDU A 2 C410 C 0.9937(4) -0.0153(3) 1.2343(2) 0.0369(10) Uani 0.512(3) 1 d PDU A 2 C411 C 0.8860(5) 0.1265(3) 1.1519(2) 0.0474(11) Uani 0.512(3) 1 d PDU A 2 C412 C 0.9611(4) 0.0152(4) 1.1696(2) 0.0403(10) Uani 0.512(3) 1 d PDU A 2 C413 C 1.0397(3) -0.0261(4) 1.1076(2) 0.0418(10) Uani 0.512(3) 1 d PDU A 2 C414 C 1.0132(3) 0.0614(3) 1.0517(3) 0.0429(10) Uani 0.512(3) 1 d PDU A 2 C415 C 0.9187(4) 0.1549(3) 1.0782(2) 0.0466(10) Uani 0.512(3) 1 d PDU A 2 C416 C 0.8746(5) 0.3353(4) 1.1045(2) 0.0431(9) Uani 0.512(3) 1 d PDU A 2 C417 C 0.9117(4) 0.2573(3) 1.0547(2) 0.0474(11) Uani 0.512(3) 1 d PDU A 2 C418 C 1.0002(4) 0.2713(4) 1.0033(3) 0.0476(12) Uani 0.512(3) 1 d PDU A 2 C419 C 1.0163(4) 0.3585(4) 1.0207(3) 0.0445(9) Uani 0.512(3) 1 d PDU A 2 C420 C 0.9382(4) 0.3987(5) 1.0832(2) 0.0427(9) Uani 0.512(3) 1 d PDU A 2 C421 C 0.9367(5) 0.4016(5) 1.2076(2) 0.0450(9) Uani 0.512(3) 1 d PDU A 2 C422 C 0.9686(4) 0.4305(5) 1.1335(2) 0.0430(9) Uani 0.512(3) 1 d PDU A 2 C423 C 1.0787(3) 0.4248(4) 1.1233(2) 0.0431(10) Uani 0.512(3) 1 d PDU A 2 C424 C 1.1130(3) 0.3924(4) 1.1913(2) 0.0459(11) Uani 0.512(3) 1 d PDU A 2 C425 C 1.0259(3) 0.3787(4) 1.2436(3) 0.0478(10) Uani 0.512(3) 1 d PDU A 2 C426 C 0.9873(4) 0.2336(3) 1.3192(3) 0.0474(10) Uani 0.512(3) 1 d PDU A 2 C427 C 1.0508(3) 0.2969(4) 1.2979(3) 0.0480(11) Uani 0.512(3) 1 d PDU A 2 C428 C 1.1645(4) 0.2240(3) 1.3025(3) 0.0510(12) Uani 0.512(3) 1 d PDU A 2 C429 C 1.1719(4) 0.1163(3) 1.3270(3) 0.0484(11) Uani 0.512(3) 1 d PDU A 2 C430 C 1.0621(3) 0.1226(3) 1.3368(3) 0.0460(11) Uani 0.512(3) 1 d PDU A 2 C431 C 1.3756(5) 0.1317(3) 1.0368(3) 0.0447(11) Uani 0.512(3) 1 d PDU A 2 C432 C 1.4106(5) 0.0990(3) 1.1047(2) 0.0441(10) Uani 0.512(3) 1 d PDU A 2 C433 C 1.4201(5) -0.0098(4) 1.1291(2) 0.0469(10) Uani 0.512(3) 1 d PDU A 2 C434 C 1.3871(5) -0.0423(5) 1.0761(3) 0.0470(9) Uani 0.512(3) 1 d PDU A 2 C435 C 1.3596(4) 0.0440(3) 1.0195(3) 0.0422(10) Uani 0.512(3) 1 d PDU A 2 C436 C 1.3036(4) 0.2369(3) 1.0203(2) 0.0417(10) Uani 0.512(3) 1 d PDU A 2 C437 C 1.2149(3) 0.2598(3) 0.9834(3) 0.0453(11) Uani 0.512(3) 1 d PDU A 2 C438 C 1.1214(3) 0.3525(4) 1.0113(3) 0.0424(10) Uani 0.512(3) 1 d PDU A 2 C439 C 1.1530(3) 0.3863(4) 1.0640(2) 0.0448(10) Uani 0.512(3) 1 d PDU A 2 C440 C 1.2666(4) 0.3150(3) 1.0701(2) 0.0369(10) Uani 0.512(3) 1 d PDU A 2 C441 C 1.3755(5) 0.1731(3) 1.1520(2) 0.0474(11) Uani 0.512(3) 1 d PDU A 2 C442 C 1.2991(4) 0.2839(4) 1.1349(2) 0.0403(10) Uani 0.512(3) 1 d PDU A 2 C443 C 1.2215(3) 0.3250(4) 1.1970(2) 0.0418(10) Uani 0.512(3) 1 d PDU A 2 C444 C 1.2478(3) 0.2382(3) 1.2534(3) 0.0429(10) Uani 0.512(3) 1 d PDU A 2 C445 C 1.3424(4) 0.1453(3) 1.2257(2) 0.0466(10) Uani 0.512(3) 1 d PDU A 2 C446 C 1.3878(5) -0.0360(4) 1.1995(3) 0.0431(9) Uani 0.512(3) 1 d PDU A 2 C447 C 1.3495(4) 0.0429(3) 1.2489(3) 0.0474(11) Uani 0.512(3) 1 d PDU A 2 C448 C 1.2616(4) 0.0282(4) 1.3006(3) 0.0476(12) Uani 0.512(3) 1 d PDU A 2 C449 C 1.2449(4) -0.0589(4) 1.2832(3) 0.0445(9) Uani 0.512(3) 1 d PDU A 2 C450 C 1.3223(4) -0.0974(5) 1.2204(2) 0.0427(9) Uani 0.512(3) 1 d PDU A 2 C451 C 1.3251(5) -0.1015(5) 1.0964(2) 0.0450(9) Uani 0.512(3) 1 d PDU A 2 C452 C 1.2916(4) -0.1290(5) 1.1702(2) 0.0430(9) Uani 0.512(3) 1 d PDU A 2 C453 C 1.1822(3) -0.1252(4) 1.1811(2) 0.0431(10) Uani 0.512(3) 1 d PDU A 2 C454 C 1.1485(3) -0.0937(4) 1.1128(2) 0.0459(11) Uani 0.512(3) 1 d PDU A 2 C455 C 1.2356(4) -0.0787(4) 1.0608(3) 0.0478(10) Uani 0.512(3) 1 d PDU A 2 C456 C 1.2743(4) 0.0659(3) 0.9855(3) 0.0474(10) Uani 0.512(3) 1 d PDU A 2 C457 C 1.2099(4) 0.0034(4) 1.0066(3) 0.0480(11) Uani 0.512(3) 1 d PDU A 2 C458 C 1.0962(4) 0.0749(3) 1.0017(3) 0.0510(12) Uani 0.512(3) 1 d PDU A 2 C459 C 1.0895(4) 0.1826(3) 0.9773(3) 0.0484(11) Uani 0.512(3) 1 d PDU A 2 C460 C 1.1995(3) 0.1767(3) 0.9673(3) 0.0460(11) Uani 0.512(3) 1 d PDU A 2 C51 C 1.5333(9) 0.5566(8) 1.2560(4) 0.0580(13) Uani 0.660(5) 1 d PDU B 1 H51 H 1.4921 0.5317 1.2338 0.070 Uiso 0.660(5) 1 calc PR B 1 Cl1 Cl 1.4342(3) 0.66174(16) 1.30512(18) 0.1198(14) Uani 0.660(5) 1 d PDU B 1 Cl2 Cl 1.60881(16) 0.4494(2) 1.30766(13) 0.0684(9) Uani 0.660(5) 1 d PDU B 1 Cl3 Cl 1.6119(5) 0.6039(4) 1.1883(2) 0.162(2) Uani 0.660(5) 1 d PDU B 1 C51A C 1.5707(8) 0.6609(9) 1.1847(7) 0.047(2) Uani 0.236(3) 1 d PDU C 2 H51A H 1.5040 0.7309 1.1859 0.056 Uiso 0.236(3) 1 calc PR C 2 Cl1A Cl 1.5409(11) 0.5736(11) 1.2553(4) 0.116(4) Uani 0.236(3) 1 d PDU C 2 Cl2A Cl 1.5909(9) 0.6174(10) 1.1065(3) 0.134(4) Uani 0.236(3) 1 d PDU C 2 Cl3A Cl 1.6769(6) 0.6869(6) 1.1962(3) 0.090(2) Uani 0.236(3) 1 d PDU C 2 C51B C 1.5485(12) 0.5414(10) 1.2500(6) 0.082(5) Uiso 0.104(5) 1 d PDU D 3 H51B H 1.5300 0.4825 1.2441 0.099 Uiso 0.104(5) 1 calc PR D 3 Cl1B Cl 1.4226(8) 0.6536(11) 1.2695(8) 0.068(5) Uiso 0.104(5) 1 d PD D 3 Cl2B Cl 1.6204(8) 0.4957(12) 1.3169(5) 0.049(3) Uiso 0.104(5) 1 d PD D 3 Cl3B Cl 1.6226(11) 0.5683(13) 1.1705(5) 0.062(4) Uiso 0.104(5) 1 d PD D 3 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.01862(18) 0.01843(16) 0.02036(17) -0.00542(12) -0.00347(12) -0.01106(13) N1 0.0194(12) 0.0207(11) 0.0224(12) -0.0025(9) -0.0045(9) -0.0120(10) N2 0.0208(12) 0.0228(11) 0.0185(11) -0.0035(9) -0.0053(9) -0.0127(10) N3 0.0191(12) 0.0189(11) 0.0217(11) -0.0064(9) -0.0074(9) -0.0112(9) N4 0.0200(12) 0.0178(11) 0.0244(12) -0.0053(9) -0.0067(10) -0.0103(10) C1 0.0182(14) 0.0264(14) 0.0227(14) -0.0045(11) -0.0033(11) -0.0110(12) C2 0.0157(13) 0.0247(14) 0.0238(14) -0.0057(11) -0.0074(11) -0.0088(11) C3 0.0177(14) 0.0247(14) 0.0263(15) -0.0028(12) -0.0073(11) -0.0051(12) C4 0.0203(14) 0.0234(14) 0.0293(15) -0.0022(12) -0.0085(12) -0.0068(12) C5 0.0184(14) 0.0220(13) 0.0227(14) -0.0021(11) -0.0085(11) -0.0080(11) C6 0.0253(15) 0.0216(13) 0.0251(14) 0.0007(11) -0.0059(12) -0.0126(12) C7 0.0257(15) 0.0243(14) 0.0213(13) -0.0015(11) -0.0095(11) -0.0150(12) C8 0.0291(16) 0.0287(14) 0.0201(13) -0.0051(11) -0.0053(12) -0.0205(13) C9 0.0269(15) 0.0302(14) 0.0179(13) -0.0068(11) -0.0030(11) -0.0208(13) C10 0.0261(15) 0.0271(14) 0.0197(13) -0.0095(11) 0.0008(11) -0.0156(13) C11 0.0215(15) 0.0265(14) 0.0244(14) -0.0139(12) 0.0028(12) -0.0105(12) C12 0.0220(14) 0.0210(13) 0.0243(14) -0.0116(11) -0.0003(11) -0.0076(12) C13 0.0237(15) 0.0202(13) 0.0316(16) -0.0117(12) -0.0036(13) -0.0046(12) C14 0.0271(16) 0.0172(13) 0.0343(16) -0.0092(12) -0.0059(13) -0.0070(12) C15 0.0274(16) 0.0161(12) 0.0280(15) -0.0092(11) -0.0030(12) -0.0084(12) C16 0.0282(16) 0.0144(12) 0.0288(15) -0.0035(11) -0.0067(12) -0.0102(12) C17 0.0287(16) 0.0203(13) 0.0263(14) -0.0050(11) -0.0068(12) -0.0164(12) C18 0.0267(16) 0.0238(14) 0.0266(15) 0.0008(11) -0.0037(12) -0.0165(13) C19 0.0236(15) 0.0247(14) 0.0290(15) 0.0004(12) -0.0028(12) -0.0171(13) C20 0.0193(14) 0.0246(14) 0.0246(14) -0.0041(11) -0.0041(11) -0.0134(12) C21 0.0227(16) 0.0292(16) 0.0382(19) -0.0017(14) -0.0014(14) -0.0014(14) C22 0.043(2) 0.045(2) 0.036(2) -0.0147(17) 0.0043(17) 0.0006(19) C23 0.0247(16) 0.0252(15) 0.0365(18) 0.0015(13) -0.0114(14) -0.0039(13) C24 0.069(3) 0.0231(16) 0.058(3) 0.0025(17) -0.027(2) -0.0160(19) C25 0.0313(17) 0.0318(16) 0.0276(16) 0.0018(13) -0.0054(13) -0.0196(14) C26 0.051(2) 0.0309(18) 0.056(2) -0.0042(17) -0.011(2) -0.0242(18) C27 0.0283(17) 0.0348(17) 0.0260(15) -0.0051(13) 0.0027(13) -0.0184(14) C28 0.0274(18) 0.048(2) 0.049(2) -0.0114(17) -0.0034(16) -0.0221(17) C29 0.0227(16) 0.0270(16) 0.0428(19) -0.0133(14) -0.0023(14) -0.0035(13) C30 0.0240(18) 0.060(3) 0.056(2) -0.027(2) -0.0003(17) -0.0145(18) C31 0.0336(19) 0.0206(15) 0.045(2) -0.0048(14) -0.0065(16) 0.0005(14) C32 0.059(3) 0.038(2) 0.051(3) 0.0029(19) -0.028(2) 0.002(2) C33 0.0287(17) 0.0285(15) 0.0364(18) 0.0063(13) -0.0038(14) -0.0173(14) C34 0.036(2) 0.0425(19) 0.0366(19) 0.0113(16) -0.0097(16) -0.0215(17) C35 0.0274(17) 0.0310(16) 0.0308(17) -0.0003(13) 0.0011(13) -0.0165(14) C36 0.037(2) 0.0406(19) 0.0299(17) -0.0060(15) 0.0078(15) -0.0212(17) N5 0.0257(13) 0.0281(13) 0.0261(13) -0.0100(10) -0.0007(10) -0.0158(11) C42 0.034(2) 0.035(2) 0.126(5) -0.041(3) -0.038(3) -0.0007(17) C43 0.043(2) 0.035(2) 0.152(5) -0.048(3) -0.060(3) 0.0041(18) C44 0.0246(15) 0.0297(15) 0.0361(17) -0.0150(13) -0.0055(13) -0.0175(13) C45 0.049(2) 0.0267(15) 0.055(2) 0.0039(15) -0.0358(18) -0.0232(16) C46 0.052(2) 0.0229(15) 0.055(2) 0.0036(15) -0.0306(19) -0.0216(16) C301 0.059(2) 0.044(3) 0.049(3) 0.010(2) -0.008(2) -0.026(2) C302 0.054(2) 0.021(2) 0.060(3) 0.006(2) -0.0088(17) -0.020(2) C303 0.0402(18) 0.0169(18) 0.0642(17) -0.0005(16) -0.0161(16) -0.0042(16) C304 0.039(2) 0.031(2) 0.056(2) 0.0050(18) -0.0188(16) -0.0077(17) C305 0.0495(19) 0.0416(19) 0.0402(19) 0.0154(16) -0.0193(16) -0.0135(17) C306 0.057(2) 0.053(3) 0.042(3) 0.013(2) 0.002(2) -0.030(2) C307 0.055(3) 0.062(3) 0.020(3) 0.005(2) 0.009(2) -0.026(2) C308 0.039(2) 0.063(2) 0.031(2) -0.008(2) 0.0176(18) -0.022(2) C309 0.031(3) 0.053(2) 0.048(2) -0.0007(19) 0.0160(19) -0.028(2) C310 0.043(3) 0.046(2) 0.060(3) 0.009(2) 0.006(2) -0.033(2) C311 0.051(2) 0.026(2) 0.078(2) -0.006(2) -0.0099(19) -0.0266(19) C312 0.045(2) 0.037(2) 0.077(3) 0.001(2) -0.004(2) -0.0338(19) C313 0.043(2) 0.0523(19) 0.075(2) -0.0137(18) -0.0204(17) -0.0357(16) C314 0.059(2) 0.058(2) 0.065(2) -0.0247(16) -0.0290(17) -0.0341(17) C315 0.056(2) 0.043(3) 0.072(2) -0.031(2) -0.0138(19) -0.025(2) C316 0.0367(19) 0.0221(18) 0.0625(18) -0.0174(16) 0.0041(16) -0.0057(15) C317 0.0594(18) 0.0327(19) 0.055(2) -0.0284(17) -0.0019(15) -0.0171(17) C318 0.069(3) 0.046(3) 0.037(3) -0.0288(19) 0.000(2) -0.017(2) C319 0.049(3) 0.054(2) 0.036(2) -0.0232(19) 0.020(2) -0.017(2) C320 0.0311(19) 0.0365(19) 0.061(2) -0.0189(15) 0.0111(16) -0.0075(15) C321 0.026(2) 0.0384(18) 0.0670(19) 0.0049(16) -0.0196(18) -0.0073(15) C322 0.023(2) 0.0389(19) 0.068(2) -0.0074(18) -0.0008(19) -0.0087(18) C323 0.021(2) 0.0464(17) 0.0645(18) -0.0058(15) 0.0005(17) -0.0201(16) C324 0.028(2) 0.0560(18) 0.070(2) -0.0044(17) -0.0203(19) -0.0317(17) C325 0.031(2) 0.056(2) 0.062(2) 0.0014(18) -0.0315(18) -0.022(2) C326 0.050(2) 0.062(3) 0.030(3) 0.004(2) -0.022(2) -0.018(2) C327 0.050(3) 0.071(2) 0.050(3) -0.005(2) -0.0316(18) -0.027(2) C328 0.072(3) 0.073(2) 0.051(3) -0.026(2) -0.026(2) -0.039(2) C329 0.072(3) 0.064(2) 0.027(2) -0.026(2) -0.010(2) -0.023(2) C330 0.057(2) 0.063(2) 0.016(2) -0.002(2) -0.007(2) -0.017(2) C331 0.059(2) 0.044(3) 0.049(3) 0.010(2) -0.008(2) -0.026(2) C332 0.054(2) 0.021(2) 0.060(3) 0.006(2) -0.0088(17) -0.020(2) C333 0.0402(18) 0.0169(18) 0.0642(17) -0.0005(16) -0.0161(16) -0.0042(16) C334 0.039(2) 0.031(2) 0.056(2) 0.0050(18) -0.0188(16) -0.0077(17) C335 0.0495(19) 0.0416(19) 0.0402(19) 0.0154(16) -0.0193(16) -0.0135(17) C336 0.057(2) 0.053(3) 0.042(3) 0.013(2) 0.002(2) -0.030(2) C337 0.055(3) 0.062(3) 0.020(3) 0.005(2) 0.009(2) -0.026(2) C338 0.039(2) 0.063(2) 0.031(2) -0.008(2) 0.0176(18) -0.022(2) C339 0.031(3) 0.053(2) 0.048(2) -0.0007(19) 0.0160(19) -0.028(2) C340 0.043(3) 0.046(2) 0.060(3) 0.009(2) 0.006(2) -0.033(2) C341 0.051(2) 0.026(2) 0.078(2) -0.006(2) -0.0099(19) -0.0266(19) C342 0.045(2) 0.037(2) 0.077(3) 0.001(2) -0.004(2) -0.0338(19) C343 0.043(2) 0.0523(19) 0.075(2) -0.0137(18) -0.0204(17) -0.0357(16) C344 0.059(2) 0.058(2) 0.065(2) -0.0247(16) -0.0290(17) -0.0341(17) C345 0.056(2) 0.043(3) 0.072(2) -0.031(2) -0.0138(19) -0.025(2) C346 0.0367(19) 0.0221(18) 0.0625(18) -0.0174(16) 0.0041(16) -0.0057(15) C347 0.0594(18) 0.0327(19) 0.055(2) -0.0284(17) -0.0019(15) -0.0171(17) C348 0.069(3) 0.046(3) 0.037(3) -0.0288(19) 0.000(2) -0.017(2) C349 0.049(3) 0.054(2) 0.036(2) -0.0232(19) 0.020(2) -0.017(2) C350 0.0311(19) 0.0365(19) 0.061(2) -0.0189(15) 0.0111(16) -0.0075(15) C351 0.026(2) 0.0384(18) 0.0670(19) 0.0049(16) -0.0196(18) -0.0073(15) C352 0.023(2) 0.0389(19) 0.068(2) -0.0074(18) -0.0008(19) -0.0087(18) C353 0.021(2) 0.0464(17) 0.0645(18) -0.0058(15) 0.0005(17) -0.0201(16) C354 0.028(2) 0.0560(18) 0.070(2) -0.0044(17) -0.0203(19) -0.0317(17) C355 0.031(2) 0.056(2) 0.062(2) 0.0014(18) -0.0315(18) -0.022(2) C356 0.050(2) 0.062(3) 0.030(3) 0.004(2) -0.022(2) -0.018(2) C357 0.050(3) 0.071(2) 0.050(3) -0.005(2) -0.0316(18) -0.027(2) C358 0.072(3) 0.073(2) 0.051(3) -0.026(2) -0.026(2) -0.039(2) C359 0.072(3) 0.064(2) 0.027(2) -0.026(2) -0.010(2) -0.023(2) C360 0.057(2) 0.063(2) 0.016(2) -0.002(2) -0.007(2) -0.017(2) C401 0.034(3) 0.051(2) 0.050(2) -0.0087(19) 0.011(2) -0.0252(19) C402 0.0207(19) 0.0486(17) 0.0647(19) -0.0039(14) -0.0015(16) -0.0197(16) C403 0.021(2) 0.0430(19) 0.068(2) -0.0028(17) -0.0045(18) -0.0083(18) C404 0.0294(19) 0.0370(18) 0.061(2) -0.0166(15) 0.0110(16) -0.0066(15) C405 0.032(2) 0.042(2) 0.042(2) -0.0192(17) 0.0195(17) -0.013(2) C406 0.044(2) 0.050(2) 0.035(2) -0.0027(18) 0.0077(18) -0.0304(18) C407 0.057(2) 0.056(3) 0.022(2) 0.006(2) -0.0021(19) -0.0292(19) C408 0.050(2) 0.038(2) 0.037(2) 0.0220(18) -0.0124(19) -0.0252(19) C409 0.053(2) 0.027(2) 0.058(2) 0.0120(17) -0.0134(17) -0.0249(18) C410 0.042(2) 0.042(2) 0.041(2) -0.0018(18) 0.0031(19) -0.0369(18) C411 0.033(2) 0.059(2) 0.063(2) -0.0037(16) -0.0100(18) -0.0317(17) C412 0.044(3) 0.049(2) 0.051(2) -0.0054(18) -0.0087(17) -0.0400(18) C413 0.0532(19) 0.0434(19) 0.051(2) -0.0118(15) -0.0127(16) -0.0352(15) C414 0.056(2) 0.054(2) 0.044(2) -0.0092(16) -0.0227(15) -0.0365(16) C415 0.041(2) 0.057(2) 0.060(2) 0.0007(18) -0.0253(19) -0.0313(18) C416 0.0244(18) 0.0361(18) 0.0657(18) 0.0084(15) -0.0197(16) -0.0097(15) C417 0.038(3) 0.056(2) 0.058(3) 0.0052(19) -0.025(2) -0.025(2) C418 0.049(2) 0.066(3) 0.038(3) 0.011(2) -0.0256(19) -0.0299(19) C419 0.0469(18) 0.0413(18) 0.0409(18) 0.0186(16) -0.0184(15) -0.0187(16) C420 0.036(2) 0.028(2) 0.059(2) 0.0102(17) -0.0175(16) -0.0106(16) C421 0.0368(18) 0.0229(18) 0.0635(18) -0.0174(17) 0.0048(15) -0.0037(14) C422 0.0415(18) 0.0173(17) 0.0673(18) -0.0013(16) -0.0141(15) -0.0087(15) C423 0.046(2) 0.020(2) 0.068(2) -0.0010(19) -0.0125(17) -0.019(2) C424 0.055(2) 0.028(2) 0.070(2) -0.015(2) -0.0144(19) -0.0252(19) C425 0.0594(19) 0.0339(19) 0.0552(19) -0.0284(16) -0.0001(15) -0.0192(17) C426 0.056(2) 0.056(2) 0.030(2) -0.0234(19) 0.0108(18) -0.0241(19) C427 0.066(2) 0.056(3) 0.034(2) -0.0298(18) -0.003(2) -0.029(2) C428 0.068(2) 0.067(2) 0.033(3) -0.016(2) -0.009(2) -0.037(2) C429 0.068(2) 0.068(2) 0.021(2) -0.0003(19) -0.016(2) -0.0366(19) C430 0.057(2) 0.064(2) 0.016(2) -0.005(2) 0.000(2) -0.028(2) C431 0.034(3) 0.051(2) 0.050(2) -0.0087(19) 0.011(2) -0.0252(19) C432 0.0207(19) 0.0486(17) 0.0647(19) -0.0039(14) -0.0015(16) -0.0197(16) C433 0.021(2) 0.0430(19) 0.068(2) -0.0028(17) -0.0045(18) -0.0083(18) C434 0.0294(19) 0.0370(18) 0.061(2) -0.0166(15) 0.0110(16) -0.0066(15) C435 0.032(2) 0.042(2) 0.042(2) -0.0192(17) 0.0195(17) -0.013(2) C436 0.044(2) 0.050(2) 0.035(2) -0.0027(18) 0.0077(18) -0.0304(18) C437 0.057(2) 0.056(3) 0.022(2) 0.006(2) -0.0021(19) -0.0292(19) C438 0.050(2) 0.038(2) 0.037(2) 0.0220(18) -0.0124(19) -0.0252(19) C439 0.053(2) 0.027(2) 0.058(2) 0.0120(17) -0.0134(17) -0.0249(18) C440 0.042(2) 0.042(2) 0.041(2) -0.0018(18) 0.0031(19) -0.0369(18) C441 0.033(2) 0.059(2) 0.063(2) -0.0037(16) -0.0100(18) -0.0317(17) C442 0.044(3) 0.049(2) 0.051(2) -0.0054(18) -0.0087(17) -0.0400(18) C443 0.0532(19) 0.0434(19) 0.051(2) -0.0118(15) -0.0127(16) -0.0352(15) C444 0.056(2) 0.054(2) 0.044(2) -0.0092(16) -0.0227(15) -0.0365(16) C445 0.041(2) 0.057(2) 0.060(2) 0.0007(18) -0.0253(19) -0.0313(18) C446 0.0244(18) 0.0361(18) 0.0657(18) 0.0084(15) -0.0197(16) -0.0097(15) C447 0.038(3) 0.056(2) 0.058(3) 0.0052(19) -0.025(2) -0.025(2) C448 0.049(2) 0.066(3) 0.038(3) 0.011(2) -0.0256(19) -0.0299(19) C449 0.0469(18) 0.0413(18) 0.0409(18) 0.0186(16) -0.0184(15) -0.0187(16) C450 0.036(2) 0.028(2) 0.059(2) 0.0102(17) -0.0175(16) -0.0106(16) C451 0.0368(18) 0.0229(18) 0.0635(18) -0.0174(17) 0.0048(15) -0.0037(14) C452 0.0415(18) 0.0173(17) 0.0673(18) -0.0013(16) -0.0141(15) -0.0087(15) C453 0.046(2) 0.020(2) 0.068(2) -0.0010(19) -0.0125(17) -0.019(2) C454 0.055(2) 0.028(2) 0.070(2) -0.015(2) -0.0144(19) -0.0252(19) C455 0.0594(19) 0.0339(19) 0.0552(19) -0.0284(16) -0.0001(15) -0.0192(17) C456 0.056(2) 0.056(2) 0.030(2) -0.0234(19) 0.0108(18) -0.0241(19) C457 0.066(2) 0.056(3) 0.034(2) -0.0298(18) -0.003(2) -0.029(2) C458 0.068(2) 0.067(2) 0.033(3) -0.016(2) -0.009(2) -0.037(2) C459 0.068(2) 0.068(2) 0.021(2) -0.0003(19) -0.016(2) -0.0366(19) C460 0.057(2) 0.064(2) 0.016(2) -0.005(2) 0.000(2) -0.028(2) C51 0.090(4) 0.060(3) 0.046(3) -0.0080(16) -0.0298(18) -0.041(2) Cl1 0.191(3) 0.0325(10) 0.0797(19) 0.0022(10) -0.0224(18) -0.0023(13) Cl2 0.0395(10) 0.0612(13) 0.0786(14) 0.0049(10) 0.0023(9) -0.0096(9) Cl3 0.242(5) 0.131(4) 0.081(2) 0.025(2) 0.028(3) -0.093(3) C51A 0.016(6) 0.031(7) 0.070(5) -0.003(5) 0.000(6) 0.006(5) Cl1A 0.143(6) 0.130(7) 0.092(4) 0.014(5) 0.009(5) -0.097(5) Cl2A 0.208(9) 0.227(9) 0.077(4) -0.016(5) -0.021(5) -0.189(8) Cl3A 0.120(5) 0.132(6) 0.068(4) -0.014(4) -0.019(3) -0.094(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 N1 2.073(3) . ? Zn1 N2 2.075(3) . ? Zn1 N3 2.080(3) . ? Zn1 N4 2.091(3) . ? Zn1 N5 2.174(3) . ? N1 C5 1.366(4) . ? N1 C2 1.374(4) . ? N2 C7 1.359(4) . ? N2 C10 1.381(4) . ? N3 C15 1.362(4) . ? N3 C12 1.375(4) . ? N4 C20 1.362(4) . ? N4 C17 1.366(4) . ? C1 C2 1.394(4) . ? C1 C20 1.395(4) . ? C1 H1 0.9500 . ? C2 C3 1.447(4) . ? C3 C4 1.371(5) . ? C3 C21 1.506(5) . ? C4 C5 1.450(4) . ? C4 C23 1.497(4) . ? C5 C6 1.404(4) . ? C6 C7 1.396(4) . ? C6 H6 0.9500 . ? C7 C8 1.452(4) . ? C8 C9 1.356(4) . ? C8 C25 1.503(4) . ? C9 C10 1.445(4) . ? C9 C27 1.514(4) . ? C10 C11 1.396(4) . ? C11 C12 1.389(5) . ? C11 H11 0.9500 . ? C12 C13 1.460(4) . ? C13 C14 1.367(5) . ? C13 C29 1.504(5) . ? C14 C15 1.459(4) . ? C14 C31 1.502(5) . ? C15 C16 1.401(5) . ? C16 C17 1.387(4) . ? C16 H16 0.9500 . ? C17 C18 1.468(4) . ? C18 C19 1.358(4) . ? C18 C33 1.506(4) . ? C19 C20 1.456(4) . ? C19 C35 1.510(5) . ? C21 C22 1.517(6) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 C24 1.533(6) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C26 1.529(5) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C28 1.538(5) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 C30 1.534(5) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 C32 1.520(6) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 C34 1.537(5) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 C36 1.531(5) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? N5 C46 1.315(5) . ? N5 C42 1.322(5) . ? C42 C43 1.377(5) . ? C42 H42 0.9500 . ? C43 C44 1.387(5) . ? C43 H43 0.9500 . ? C44 C45 1.380(4) . ? C44 C44 1.490(6) 2_868 ? C45 C46 1.391(5) . ? C45 H45 0.9500 . ? C46 H46 0.9500 . ? C301 C306 1.384(3) . ? C301 C302 1.454(3) . ? C301 C305 1.454(3) . ? C302 C311 1.383(3) . ? C302 C303 1.455(3) . ? C303 C316 1.384(3) . ? C303 C304 1.452(3) . ? C304 C321 1.386(3) . ? C304 C305 1.453(3) . ? C305 C326 1.385(3) . ? C306 C307 1.454(3) . ? C306 C310 1.455(3) . ? C307 C330 1.383(3) . ? C307 C308 1.452(3) . ? C308 C349 1.385(3) . ? C308 C309 1.454(3) . ? C309 C353 1.385(3) . ? C309 C310 1.454(3) . ? C310 C312 1.383(3) . ? C311 C315 1.453(3) . ? C311 C312 1.456(3) . ? C312 C313 1.452(3) . ? C313 C354 1.386(3) . ? C313 C314 1.452(3) . ? C314 C358 1.385(3) . ? C314 C315 1.455(3) . ? C315 C317 1.384(3) . ? C316 C317 1.454(3) . ? C316 C320 1.456(3) . ? C317 C318 1.455(3) . ? C318 C359 1.382(3) . ? C318 C319 1.454(3) . ? C319 C338 1.387(3) . ? C319 C320 1.454(3) . ? C320 C322 1.383(3) . ? C321 C325 1.452(3) . ? C321 C322 1.457(3) . ? C322 C323 1.457(3) . ? C323 C339 1.384(3) . ? C323 C324 1.453(3) . ? C324 C343 1.387(3) . ? C324 C325 1.451(3) . ? C325 C327 1.385(3) . ? C326 C330 1.453(3) . ? C326 C327 1.454(3) . ? C327 C328 1.454(3) . ? C328 C344 1.383(3) . ? C328 C329 1.454(3) . ? C329 C348 1.383(3) . ? C329 C330 1.454(3) . ? C331 C336 1.384(3) . ? C331 C332 1.455(3) . ? C331 C335 1.457(3) . ? C332 C341 1.382(3) . ? C332 C333 1.459(3) . ? C333 C346 1.385(3) . ? C333 C334 1.455(3) . ? C334 C351 1.386(3) . ? C334 C335 1.454(3) . ? C335 C356 1.384(3) . ? C336 C337 1.454(3) . ? C336 C340 1.455(3) . ? C337 C360 1.382(3) . ? C337 C338 1.452(3) . ? C338 C339 1.452(3) . ? C339 C340 1.455(3) . ? C340 C342 1.383(3) . ? C341 C345 1.453(3) . ? C341 C342 1.457(3) . ? C342 C343 1.452(3) . ? C343 C344 1.454(3) . ? C344 C345 1.456(3) . ? C345 C347 1.384(3) . ? C346 C347 1.455(3) . ? C346 C350 1.456(3) . ? C347 C348 1.456(3) . ? C348 C349 1.455(3) . ? C349 C350 1.453(3) . ? C350 C352 1.383(3) . ? C351 C355 1.452(3) . ? C351 C352 1.454(3) . ? C352 C353 1.455(3) . ? C353 C354 1.453(3) . ? C354 C355 1.453(3) . ? C355 C357 1.385(3) . ? C356 C357 1.455(3) . ? C356 C360 1.457(3) . ? C357 C358 1.455(3) . ? C358 C359 1.456(3) . ? C359 C360 1.455(3) . ? C401 C406 1.383(4) . ? C401 C405 1.453(4) . ? C401 C402 1.455(4) . ? C402 C411 1.382(4) . ? C402 C403 1.456(4) . ? C403 C416 1.384(4) . ? C403 C404 1.451(4) . ? C404 C421 1.387(4) . ? C404 C405 1.452(4) . ? C405 C426 1.385(4) . ? C406 C410 1.453(4) . ? C406 C407 1.454(4) . ? C407 C430 1.382(4) . ? C407 C408 1.452(4) . ? C408 C449 1.385(4) . ? C408 C409 1.454(4) . ? C409 C453 1.384(4) . ? C409 C410 1.453(4) . ? C410 C412 1.382(4) . ? C411 C415 1.452(4) . ? C411 C412 1.459(4) . ? C412 C413 1.452(4) . ? C413 C454 1.388(4) . ? C413 C414 1.452(4) . ? C414 C458 1.386(4) . ? C414 C415 1.453(4) . ? C415 C417 1.384(4) . ? C416 C417 1.455(4) . ? C416 C420 1.456(4) . ? C417 C418 1.456(4) . ? C418 C459 1.382(4) . ? C418 C419 1.454(4) . ? C419 C438 1.389(4) . ? C419 C420 1.454(4) . ? C420 C422 1.383(4) . ? C421 C425 1.450(4) . ? C421 C422 1.458(4) . ? C422 C423 1.457(4) . ? C423 C439 1.382(4) . ? C423 C424 1.451(4) . ? C424 C443 1.387(4) . ? C424 C425 1.451(4) . ? C425 C427 1.386(4) . ? C426 C427 1.454(4) . ? C426 C430 1.455(4) . ? C427 C428 1.453(4) . ? C428 C444 1.383(4) . ? C428 C429 1.455(4) . ? C429 C448 1.382(4) . ? C429 C430 1.452(4) . ? C431 C436 1.383(4) . ? C431 C432 1.454(4) . ? C431 C435 1.458(4) . ? C432 C441 1.381(4) . ? C432 C433 1.460(4) . ? C433 C446 1.387(4) . ? C433 C434 1.457(4) . ? C434 C451 1.390(4) . ? C434 C435 1.454(4) . ? C435 C456 1.382(4) . ? C436 C440 1.455(4) . ? C436 C437 1.456(4) . ? C437 C460 1.381(4) . ? C437 C438 1.450(4) . ? C438 C439 1.451(4) . ? C439 C440 1.455(4) . ? C440 C442 1.382(4) . ? C441 C445 1.452(4) . ? C441 C442 1.458(4) . ? C442 C443 1.450(4) . ? C443 C444 1.453(4) . ? C444 C445 1.457(4) . ? C445 C447 1.383(4) . ? C446 C450 1.455(4) . ? C446 C447 1.456(4) . ? C447 C448 1.457(4) . ? C448 C449 1.457(4) . ? C449 C450 1.451(4) . ? C450 C452 1.383(4) . ? C451 C455 1.450(4) . ? C451 C452 1.453(4) . ? C452 C453 1.456(4) . ? C453 C454 1.454(4) . ? C454 C455 1.455(4) . ? C455 C457 1.386(4) . ? C456 C457 1.455(4) . ? C456 C460 1.456(4) . ? C457 C458 1.452(4) . ? C458 C459 1.458(4) . ? C459 C460 1.455(4) . ? C51 Cl2 1.695(10) . ? C51 Cl3 1.739(9) . ? C51 Cl1 1.767(11) . ? C51 H51 1.0000 . ? C51A Cl2A 1.693(10) . ? C51A Cl3A 1.738(9) . ? C51A Cl1A 1.765(11) . ? C51A H51A 1.0000 . ? C51B Cl2B 1.694(10) . ? C51B Cl3B 1.738(9) . ? C51B Cl1B 1.766(11) . ? C51B H51B 1.0000 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Zn1 N2 88.09(11) . . ? N1 Zn1 N3 160.61(9) . . ? N2 Zn1 N3 88.85(11) . . ? N1 Zn1 N4 88.72(11) . . ? N2 Zn1 N4 161.74(9) . . ? N3 Zn1 N4 88.21(11) . . ? N1 Zn1 N5 97.86(11) . . ? N2 Zn1 N5 103.93(11) . . ? N3 Zn1 N5 101.46(11) . . ? N4 Zn1 N5 94.32(11) . . ? C5 N1 C2 106.0(2) . . ? C5 N1 Zn1 127.4(2) . . ? C2 N1 Zn1 126.6(2) . . ? C7 N2 C10 105.9(3) . . ? C7 N2 Zn1 127.4(2) . . ? C10 N2 Zn1 126.7(2) . . ? C15 N3 C12 106.4(2) . . ? C15 N3 Zn1 127.1(2) . . ? C12 N3 Zn1 126.4(2) . . ? C20 N4 C17 107.0(3) . . ? C20 N4 Zn1 126.6(2) . . ? C17 N4 Zn1 126.4(2) . . ? C2 C1 C20 126.9(3) . . ? C2 C1 H1 116.5 . . ? C20 C1 H1 116.5 . . ? N1 C2 C1 125.1(3) . . ? N1 C2 C3 110.5(3) . . ? C1 C2 C3 124.2(3) . . ? C4 C3 C2 106.6(3) . . ? C4 C3 C21 128.9(3) . . ? C2 C3 C21 124.4(3) . . ? C3 C4 C5 106.2(3) . . ? C3 C4 C23 128.1(3) . . ? C5 C4 C23 125.5(3) . . ? N1 C5 C6 124.6(3) . . ? N1 C5 C4 110.7(3) . . ? C6 C5 C4 124.6(3) . . ? C7 C6 C5 126.5(3) . . ? C7 C6 H6 116.7 . . ? C5 C6 H6 116.7 . . ? N2 C7 C6 124.8(3) . . ? N2 C7 C8 110.8(3) . . ? C6 C7 C8 124.3(3) . . ? C9 C8 C7 106.2(3) . . ? C9 C8 C25 128.8(3) . . ? C7 C8 C25 124.9(3) . . ? C8 C9 C10 107.1(3) . . ? C8 C9 C27 128.2(3) . . ? C10 C9 C27 124.5(3) . . ? N2 C10 C11 124.6(3) . . ? N2 C10 C9 109.9(3) . . ? C11 C10 C9 125.4(3) . . ? C12 C11 C10 127.2(3) . . ? C12 C11 H11 116.4 . . ? C10 C11 H11 116.4 . . ? N3 C12 C11 125.4(3) . . ? N3 C12 C13 110.2(3) . . ? C11 C12 C13 124.4(3) . . ? C14 C13 C12 106.4(3) . . ? C14 C13 C29 128.9(3) . . ? C12 C13 C29 124.6(3) . . ? C13 C14 C15 106.4(3) . . ? C13 C14 C31 128.3(3) . . ? C15 C14 C31 125.2(3) . . ? N3 C15 C16 124.9(3) . . ? N3 C15 C14 110.6(3) . . ? C16 C15 C14 124.3(3) . . ? C17 C16 C15 126.6(3) . . ? C17 C16 H16 116.7 . . ? C15 C16 H16 116.7 . . ? N4 C17 C16 125.4(3) . . ? N4 C17 C18 109.7(3) . . ? C16 C17 C18 124.7(3) . . ? C19 C18 C17 106.4(3) . . ? C19 C18 C33 129.1(3) . . ? C17 C18 C33 124.4(3) . . ? C18 C19 C20 106.7(3) . . ? C18 C19 C35 128.6(3) . . ? C20 C19 C35 124.5(3) . . ? N4 C20 C1 125.1(3) . . ? N4 C20 C19 110.2(3) . . ? C1 C20 C19 124.6(3) . . ? C3 C21 C22 113.0(3) . . ? C3 C21 H21A 109.0 . . ? C22 C21 H21A 109.0 . . ? C3 C21 H21B 109.0 . . ? C22 C21 H21B 109.0 . . ? H21A C21 H21B 107.8 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C4 C23 C24 112.0(3) . . ? C4 C23 H23A 109.2 . . ? C24 C23 H23A 109.2 . . ? C4 C23 H23B 109.2 . . ? C24 C23 H23B 109.2 . . ? H23A C23 H23B 107.9 . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C8 C25 C26 113.3(3) . . ? C8 C25 H25A 108.9 . . ? C26 C25 H25A 108.9 . . ? C8 C25 H25B 108.9 . . ? C26 C25 H25B 108.9 . . ? H25A C25 H25B 107.7 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C9 C27 C28 112.5(3) . . ? C9 C27 H27A 109.1 . . ? C28 C27 H27A 109.1 . . ? C9 C27 H27B 109.1 . . ? C28 C27 H27B 109.1 . . ? H27A C27 H27B 107.8 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C13 C29 C30 112.7(3) . . ? C13 C29 H29A 109.1 . . ? C30 C29 H29A 109.1 . . ? C13 C29 H29B 109.1 . . ? C30 C29 H29B 109.1 . . ? H29A C29 H29B 107.8 . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C14 C31 C32 112.8(3) . . ? C14 C31 H31A 109.0 . . ? C32 C31 H31A 109.0 . . ? C14 C31 H31B 109.0 . . ? C32 C31 H31B 109.0 . . ? H31A C31 H31B 107.8 . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C18 C33 C34 112.6(3) . . ? C18 C33 H33A 109.1 . . ? C34 C33 H33A 109.1 . . ? C18 C33 H33B 109.1 . . ? C34 C33 H33B 109.1 . . ? H33A C33 H33B 107.8 . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C19 C35 C36 112.9(3) . . ? C19 C35 H35A 109.0 . . ? C36 C35 H35A 109.0 . . ? C19 C35 H35B 109.0 . . ? C36 C35 H35B 109.0 . . ? H35A C35 H35B 107.8 . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C46 N5 C42 115.9(3) . . ? C46 N5 Zn1 122.5(2) . . ? C42 N5 Zn1 121.1(3) . . ? N5 C42 C43 123.8(4) . . ? N5 C42 H42 118.1 . . ? C43 C42 H42 118.1 . . ? C42 C43 C44 120.9(3) . . ? C42 C43 H43 119.5 . . ? C44 C43 H43 119.5 . . ? C45 C44 C43 114.8(3) . . ? C45 C44 C44 122.7(4) . 2_868 ? C43 C44 C44 122.5(4) . 2_868 ? C44 C45 C46 120.2(3) . . ? C44 C45 H45 119.9 . . ? C46 C45 H45 119.9 . . ? N5 C46 C45 124.2(3) . . ? N5 C46 H46 117.9 . . ? C45 C46 H46 117.9 . . ? C306 C301 C302 119.89(19) . . ? C306 C301 C305 119.89(19) . . ? C302 C301 C305 108.6(4) . . ? C311 C302 C301 120.29(19) . . ? C311 C302 C303 119.8(2) . . ? C301 C302 C303 107.9(4) . . ? C316 C303 C304 120.24(19) . . ? C316 C303 C302 120.04(19) . . ? C304 C303 C302 107.4(4) . . ? C321 C304 C303 119.89(19) . . ? C321 C304 C305 120.02(19) . . ? C303 C304 C305 109.0(4) . . ? C326 C305 C304 120.06(19) . . ? C326 C305 C301 120.20(19) . . ? C304 C305 C301 107.1(4) . . ? C301 C306 C307 119.84(19) . . ? C301 C306 C310 119.81(19) . . ? C307 C306 C310 109.4(4) . . ? C330 C307 C308 119.90(19) . . ? C330 C307 C306 120.29(19) . . ? C308 C307 C306 107.6(4) . . ? C349 C308 C307 120.10(19) . . ? C349 C308 C309 120.02(19) . . ? C307 C308 C309 107.3(4) . . ? C353 C309 C308 119.80(19) . . ? C353 C309 C310 119.88(19) . . ? C308 C309 C310 109.6(4) . . ? C312 C310 C309 119.94(19) . . ? C312 C310 C306 120.29(19) . . ? C309 C310 C306 106.1(4) . . ? C302 C311 C315 120.20(19) . . ? C302 C311 C312 119.85(19) . . ? C315 C311 C312 107.5(4) . . ? C310 C312 C313 120.15(19) . . ? C310 C312 C311 119.81(19) . . ? C313 C312 C311 109.3(4) . . ? C354 C313 C314 120.06(19) . . ? C354 C313 C312 119.96(19) . . ? C314 C313 C312 106.4(4) . . ? C358 C314 C313 120.03(19) . . ? C358 C314 C315 119.95(19) . . ? C313 C314 C315 109.5(3) . . ? C317 C315 C311 119.98(19) . . ? C317 C315 C314 120.14(19) . . ? C311 C315 C314 107.3(4) . . ? C303 C316 C317 120.03(19) . . ? C303 C316 C320 119.93(18) . . ? C317 C316 C320 108.5(4) . . ? C315 C317 C316 119.9(2) . . ? C315 C317 C318 119.84(19) . . ? C316 C317 C318 107.5(4) . . ? C359 C318 C319 120.17(19) . . ? C359 C318 C317 120.04(19) . . ? C319 C318 C317 108.4(4) . . ? C338 C319 C318 119.83(19) . . ? C338 C319 C320 120.00(19) . . ? C318 C319 C320 108.0(4) . . ? C322 C320 C319 120.1(2) . . ? C322 C320 C316 119.89(19) . . ? C319 C320 C316 107.7(4) . . ? C304 C321 C325 119.9(2) . . ? C304 C321 C322 119.92(18) . . ? C325 C321 C322 108.4(4) . . ? C320 C322 C321 120.13(19) . . ? C320 C322 C323 119.83(19) . . ? C321 C322 C323 108.2(4) . . ? C339 C323 C324 120.1(2) . . ? C339 C323 C322 119.98(19) . . ? C324 C323 C322 107.0(4) . . ? C343 C324 C325 119.80(19) . . ? C343 C324 C323 119.94(19) . . ? C325 C324 C323 109.2(4) . . ? C327 C325 C324 120.11(19) . . ? C327 C325 C321 120.17(19) . . ? C324 C325 C321 107.2(4) . . ? C305 C326 C330 119.91(19) . . ? C305 C326 C327 119.96(19) . . ? C330 C326 C327 108.3(4) . . ? C325 C327 C328 119.99(19) . . ? C325 C327 C326 119.89(19) . . ? C328 C327 C326 107.0(4) . . ? C344 C328 C329 120.00(19) . . ? C344 C328 C327 119.98(19) . . ? C329 C328 C327 109.4(4) . . ? C348 C329 C328 120.16(19) . . ? C348 C329 C330 120.20(19) . . ? C328 C329 C330 106.8(4) . . ? C307 C330 C326 119.86(19) . . ? C307 C330 C329 120.01(19) . . ? C326 C330 C329 108.6(4) . . ? C336 C331 C332 119.98(19) . . ? C336 C331 C335 119.7(2) . . ? C332 C331 C335 107.7(4) . . ? C341 C332 C331 120.07(19) . . ? C341 C332 C333 120.01(19) . . ? C331 C332 C333 108.9(4) . . ? C346 C333 C334 119.99(19) . . ? C346 C333 C332 119.63(19) . . ? C334 C333 C332 106.7(4) . . ? C351 C334 C335 119.6(2) . . ? C351 C334 C333 119.91(19) . . ? C335 C334 C333 109.1(4) . . ? C356 C335 C334 120.29(19) . . ? C356 C335 C331 120.4(2) . . ? C334 C335 C331 107.6(4) . . ? C331 C336 C337 119.96(19) . . ? C331 C336 C340 119.91(19) . . ? C337 C336 C340 109.7(4) . . ? C360 C337 C338 120.17(19) . . ? C360 C337 C336 120.3(2) . . ? C338 C337 C336 106.7(4) . . ? C319 C338 C339 119.83(19) . . ? C319 C338 C337 119.92(19) . . ? C339 C338 C337 108.5(4) . . ? C323 C339 C338 120.21(19) . . ? C323 C339 C340 119.88(19) . . ? C338 C339 C340 108.7(4) . . ? C342 C340 C336 120.10(19) . . ? C342 C340 C339 119.97(19) . . ? C336 C340 C339 106.4(4) . . ? C332 C341 C345 120.27(19) . . ? C332 C341 C342 119.99(19) . . ? C345 C341 C342 106.4(4) . . ? C340 C342 C343 120.14(19) . . ? C340 C342 C341 119.84(19) . . ? C343 C342 C341 109.8(3) . . ? C324 C343 C342 119.88(19) . . ? C324 C343 C344 120.11(19) . . ? C342 C343 C344 106.6(4) . . ? C328 C344 C343 119.96(19) . . ? C328 C344 C345 119.87(19) . . ? C343 C344 C345 108.5(4) . . ? C347 C345 C341 119.78(19) . . ? C347 C345 C344 120.16(19) . . ? C341 C345 C344 108.6(4) . . ? C333 C346 C347 120.19(19) . . ? C333 C346 C350 120.01(18) . . ? C347 C346 C350 107.7(4) . . ? C345 C347 C346 120.1(2) . . ? C345 C347 C348 119.83(19) . . ? C346 C347 C348 107.6(4) . . ? C329 C348 C349 119.75(19) . . ? C329 C348 C347 119.96(19) . . ? C349 C348 C347 108.8(4) . . ? C308 C349 C350 120.14(19) . . ? C308 C349 C348 120.03(19) . . ? C350 C349 C348 107.1(4) . . ? C352 C350 C349 119.9(2) . . ? C352 C350 C346 119.99(19) . . ? C349 C350 C346 108.8(4) . . ? C334 C351 C355 120.1(2) . . ? C334 C351 C352 120.02(18) . . ? C355 C351 C352 107.3(4) . . ? C350 C352 C351 120.04(19) . . ? C350 C352 C353 120.00(19) . . ? C351 C352 C353 109.5(4) . . ? C309 C353 C354 120.2(2) . . ? C309 C353 C352 120.10(19) . . ? C354 C353 C352 106.1(4) . . ? C313 C354 C355 119.88(19) . . ? C313 C354 C353 119.80(19) . . ? C355 C354 C353 109.4(4) . . ? C357 C355 C351 120.27(19) . . ? C357 C355 C354 120.03(19) . . ? C351 C355 C354 107.6(4) . . ? C335 C356 C357 120.0(2) . . ? C335 C356 C360 119.7(2) . . ? C357 C356 C360 107.5(4) . . ? C355 C357 C358 120.04(19) . . ? C355 C357 C356 119.68(19) . . ? C358 C357 C356 108.5(4) . . ? C314 C358 C357 119.90(19) . . ? C314 C358 C359 119.86(19) . . ? C357 C358 C359 107.8(4) . . ? C318 C359 C360 119.96(19) . . ? C318 C359 C358 120.14(19) . . ? C360 C359 C358 107.9(4) . . ? C337 C360 C359 119.95(19) . . ? C337 C360 C356 119.85(19) . . ? C359 C360 C356 108.3(4) . . ? C406 C401 C405 119.9(3) . . ? C406 C401 C402 119.8(3) . . ? C405 C401 C402 108.4(4) . . ? C411 C402 C401 120.5(3) . . ? C411 C402 C403 119.6(3) . . ? C401 C402 C403 108.0(4) . . ? C416 C403 C404 120.5(3) . . ? C416 C403 C402 120.1(3) . . ? C404 C403 C402 107.4(4) . . ? C421 C404 C403 119.6(3) . . ? C421 C404 C405 120.2(3) . . ? C403 C404 C405 109.0(4) . . ? C426 C405 C404 120.1(3) . . ? C426 C405 C401 120.5(3) . . ? C404 C405 C401 107.2(4) . . ? C401 C406 C410 119.7(3) . . ? C401 C406 C407 119.7(3) . . ? C410 C406 C407 109.5(4) . . ? C430 C407 C408 119.7(3) . . ? C430 C407 C406 120.6(3) . . ? C408 C407 C406 107.5(4) . . ? C449 C408 C407 120.1(3) . . ? C449 C408 C409 119.9(3) . . ? C407 C408 C409 107.3(4) . . ? C453 C409 C410 119.9(3) . . ? C453 C409 C408 119.7(3) . . ? C410 C409 C408 109.6(4) . . ? C412 C410 C409 119.9(3) . . ? C412 C410 C406 120.7(3) . . ? C409 C410 C406 106.1(4) . . ? C402 C411 C415 120.3(3) . . ? C402 C411 C412 119.8(3) . . ? C415 C411 C412 107.3(4) . . ? C410 C412 C413 120.1(3) . . ? C410 C412 C411 119.4(3) . . ? C413 C412 C411 109.3(4) . . ? C454 C413 C414 120.0(3) . . ? C454 C413 C412 120.2(3) . . ? C414 C413 C412 106.3(4) . . ? C458 C414 C413 120.1(3) . . ? C458 C414 C415 119.8(3) . . ? C413 C414 C415 109.5(4) . . ? C417 C415 C411 120.2(3) . . ? C417 C415 C414 120.5(3) . . ? C411 C415 C414 107.5(4) . . ? C403 C416 C417 120.2(3) . . ? C403 C416 C420 120.0(3) . . ? C417 C416 C420 108.4(4) . . ? C415 C417 C416 119.6(3) . . ? C415 C417 C418 119.7(3) . . ? C416 C417 C418 107.5(4) . . ? C459 C418 C419 119.9(3) . . ? C459 C418 C417 120.0(3) . . ? C419 C418 C417 108.3(4) . . ? C438 C419 C420 120.2(3) . . ? C438 C419 C418 119.9(3) . . ? C420 C419 C418 108.0(4) . . ? C422 C420 C419 120.1(3) . . ? C422 C420 C416 119.6(3) . . ? C419 C420 C416 107.8(4) . . ? C404 C421 C425 119.7(3) . . ? C404 C421 C422 119.9(3) . . ? C425 C421 C422 108.4(4) . . ? C420 C422 C423 119.8(3) . . ? C420 C422 C421 120.4(3) . . ? C423 C422 C421 108.1(4) . . ? C439 C423 C424 120.4(3) . . ? C439 C423 C422 120.1(3) . . ? C424 C423 C422 107.0(4) . . ? C443 C424 C425 119.7(3) . . ? C443 C424 C423 120.2(3) . . ? C425 C424 C423 109.4(4) . . ? C427 C425 C421 120.3(3) . . ? C427 C425 C424 120.2(3) . . ? C421 C425 C424 107.1(4) . . ? C405 C426 C427 119.8(3) . . ? C405 C426 C430 119.7(3) . . ? C427 C426 C430 108.1(4) . . ? C425 C427 C428 120.0(3) . . ? C425 C427 C426 120.0(3) . . ? C428 C427 C426 107.3(4) . . ? C444 C428 C427 119.9(3) . . ? C444 C428 C429 120.0(3) . . ? C427 C428 C429 109.0(4) . . ? C448 C429 C430 120.5(3) . . ? C448 C429 C428 120.0(3) . . ? C430 C429 C428 107.1(4) . . ? C407 C430 C429 120.1(3) . . ? C407 C430 C426 119.7(3) . . ? C429 C430 C426 108.5(4) . . ? C436 C431 C432 119.8(3) . . ? C436 C431 C435 119.6(4) . . ? C432 C431 C435 107.5(4) . . ? C441 C432 C431 120.5(3) . . ? C441 C432 C433 120.1(3) . . ? C431 C432 C433 109.1(4) . . ? C446 C433 C434 120.0(3) . . ? C446 C433 C432 119.4(3) . . ? C434 C433 C432 106.5(4) . . ? C451 C434 C435 119.0(3) . . ? C451 C434 C433 119.7(3) . . ? C435 C434 C433 109.1(4) . . ? C456 C435 C434 120.6(3) . . ? C456 C435 C431 120.2(3) . . ? C434 C435 C431 107.7(4) . . ? C431 C436 C440 119.6(3) . . ? C431 C436 C437 120.1(3) . . ? C440 C436 C437 109.6(4) . . ? C460 C437 C438 120.0(3) . . ? C460 C437 C436 120.2(3) . . ? C438 C437 C436 106.7(4) . . ? C419 C438 C437 120.1(3) . . ? C419 C438 C439 119.6(3) . . ? C437 C438 C439 108.5(4) . . ? C423 C439 C438 120.3(3) . . ? C423 C439 C440 119.4(3) . . ? C438 C439 C440 108.8(4) . . ? C442 C440 C439 120.1(3) . . ? C442 C440 C436 120.6(3) . . ? C439 C440 C436 106.3(4) . . ? C432 C441 C445 120.4(3) . . ? C432 C441 C442 119.8(3) . . ? C445 C441 C442 106.4(4) . . ? C440 C442 C443 120.5(3) . . ? C440 C442 C441 119.6(3) . . ? C443 C442 C441 109.7(4) . . ? C424 C443 C442 119.3(3) . . ? C424 C443 C444 120.2(3) . . ? C442 C443 C444 107.0(4) . . ? C428 C444 C443 120.0(3) . . ? C428 C444 C445 120.1(3) . . ? C443 C444 C445 108.1(4) . . ? C447 C445 C441 119.7(3) . . ? C447 C445 C444 120.0(3) . . ? C441 C445 C444 108.8(4) . . ? C433 C446 C450 120.0(3) . . ? C433 C446 C447 120.3(3) . . ? C450 C446 C447 107.8(4) . . ? C445 C447 C446 120.1(3) . . ? C445 C447 C448 119.8(3) . . ? C446 C447 C448 107.6(4) . . ? C429 C448 C449 119.3(3) . . ? C429 C448 C447 120.2(3) . . ? C449 C448 C447 108.6(4) . . ? C408 C449 C450 120.4(3) . . ? C408 C449 C448 120.2(3) . . ? C450 C449 C448 107.2(4) . . ? C452 C450 C449 119.9(3) . . ? C452 C450 C446 120.0(3) . . ? C449 C450 C446 108.7(4) . . ? C434 C451 C455 120.5(3) . . ? C434 C451 C452 120.2(3) . . ? C455 C451 C452 107.4(4) . . ? C450 C452 C451 120.1(3) . . ? C450 C452 C453 119.8(3) . . ? C451 C452 C453 109.4(4) . . ? C409 C453 C454 120.4(3) . . ? C409 C453 C452 120.3(3) . . ? C454 C453 C452 106.2(4) . . ? C413 C454 C453 119.4(3) . . ? C413 C454 C455 119.8(3) . . ? C453 C454 C455 109.3(4) . . ? C457 C455 C451 120.3(3) . . ? C457 C455 C454 119.9(3) . . ? C451 C455 C454 107.7(4) . . ? C435 C456 C457 120.3(3) . . ? C435 C456 C460 120.1(3) . . ? C457 C456 C460 107.5(4) . . ? C455 C457 C458 120.3(3) . . ? C455 C457 C456 119.3(3) . . ? C458 C457 C456 108.5(4) . . ? C414 C458 C457 119.8(3) . . ? C414 C458 C459 119.8(3) . . ? C457 C458 C459 107.9(4) . . ? C418 C459 C460 120.0(3) . . ? C418 C459 C458 120.2(3) . . ? C460 C459 C458 107.7(4) . . ? C437 C460 C459 120.1(3) . . ? C437 C460 C456 119.7(3) . . ? C459 C460 C456 108.5(4) . . ? Cl2 C51 Cl3 113.7(6) . . ? Cl2 C51 Cl1 111.9(4) . . ? Cl3 C51 Cl1 110.8(5) . . ? Cl2 C51 H51 106.7 . . ? Cl3 C51 H51 106.7 . . ? Cl1 C51 H51 106.7 . . ? Cl2A C51A Cl3A 113.7(6) . . ? Cl2A C51A Cl1A 112.1(5) . . ? Cl3A C51A Cl1A 111.1(6) . . ? Cl2A C51A H51A 106.5 . . ? Cl3A C51A H51A 106.5 . . ? Cl1A C51A H51A 106.5 . . ? Cl2B C51B Cl3B 113.6(6) . . ? Cl2B C51B Cl1B 111.8(5) . . ? Cl3B C51B Cl1B 110.9(6) . . ? Cl2B C51B H51B 106.7 . . ? Cl3B C51B H51B 106.7 . . ? Cl1B C51B H51B 106.7 . . ? _diffrn_measured_fraction_theta_max 0.942 _diffrn_reflns_theta_full 30.04 _diffrn_measured_fraction_theta_full 0.942 _refine_diff_density_max 3.014 _refine_diff_density_min -1.559 _refine_diff_density_rms 0.147 # Attachment 'ZnOEP_BPy_C60_TDAE.cif' data_ZnOEP_BPy_C60_TDAE _database_code_depnum_ccdc_archive 'CCDC 648659' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 2(C60-)*(ZnOEP2.BPy)*2(TDAE+)*(C6H4Cl2)0.25*(C6H6)0.75 _chemical_melting_point ? _chemical_formula_moiety ; 2(C36 H44 N4 ZN1), (C10 H8 N2), 2(C60), 2(C10 H24 N4), 0.25(C6 H4 CL2), 0.75(C6 H6) ; _chemical_formula_sum 'C228 H149.5 Cl0.5 N18 Zn2' _chemical_formula_weight 3289.6 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'I 2 2 2' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x, -y, -z' '-x, y, -z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-x+1/2, y+1/2, -z+1/2' _cell_length_a 14.8555(4) _cell_length_b 21.2150(7) _cell_length_c 24.2022(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7627.6(4) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9984 _cell_measurement_theta_min 4 _cell_measurement_theta_max 30 _exptl_crystal_description prism _exptl_crystal_colour black _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.436 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3424 _exptl_absorpt_coefficient_mu 0.397 _exptl_absorpt_correction_type multiscan _exptl_absorpt_correction_T_min 0.8574 _exptl_absorpt_correction_T_max 0.9614 _exptl_absorpt_process_details 'SADABS; Sheldrick, 1997' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 124312 _diffrn_reflns_av_R_equivalents 0.0604 _diffrn_reflns_av_sigmaI/netI 0.0270 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -38 _diffrn_reflns_limit_l_max 38 _diffrn_reflns_theta_min 1.61 _diffrn_reflns_theta_max 34.50 _reflns_number_total 15596 _reflns_number_gt 13620 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Disordered fullerene molecules show relatively strong correlations for atomic parameters (coordinates, displacements). Additionally, it is essential to consider anisotropic thermal parameters for the fullerene carbon atoms to approximate fullerene molecular form factor correctly. These displacements are restrained by ISOR, DELU and SIMU instructions of SHELXL.Such approach resulted in large number of restraints. ; _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^)+(0.0967P)^2^+3.8253P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.501(12) _refine_ls_number_reflns 15596 _refine_ls_number_parameters 934 _refine_ls_number_restraints 1930 _refine_ls_R_factor_all 0.0571 _refine_ls_R_factor_gt 0.0496 _refine_ls_wR_factor_ref 0.1466 _refine_ls_wR_factor_gt 0.1401 _refine_ls_goodness_of_fit_ref 1.077 _refine_ls_restrained_S_all 1.112 _refine_ls_shift/su_max 0.034 _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 Zn Zn 0.0000 0.0000 0.267625(6) 0.01134(5) Uani 1 2 d S . . N101 N -0.0005(2) -0.09672(4) 0.25550(4) 0.01352(15) Uani 1 1 d . . . N102 N -0.13789(6) 0.00034(13) 0.25583(4) 0.01334(15) Uani 1 1 d . . . C101 C -0.04582(19) -0.19958(12) 0.24109(13) 0.0205(6) Uani 1 1 d . . . C102 C -0.07354(19) -0.13467(12) 0.24985(11) 0.0150(5) Uani 1 1 d . . . C103 C -0.19180(18) -0.05174(12) 0.25120(11) 0.0146(4) Uani 1 1 d . . . C104 C -0.28494(18) -0.03261(13) 0.24299(12) 0.0188(6) Uani 1 1 d . . . C105 C -0.28556(17) 0.03171(13) 0.24308(11) 0.0170(5) Uani 1 1 d . . . C106 C -0.19317(18) 0.05143(13) 0.25072(10) 0.0144(4) Uani 1 1 d . . . C107 C 0.07393(19) -0.13495(12) 0.25039(11) 0.0159(5) Uani 1 1 d . . . C108 C 0.04621(19) -0.19973(12) 0.24142(13) 0.0197(6) Uani 1 1 d . . . C109 C -0.1629(2) -0.11391(13) 0.25024(11) 0.0166(5) Uani 1 1 d . . . H109 H -0.2082 -0.1455 0.2498 0.020 Uiso 1 1 calc R . . C110 C -0.16281(19) 0.11401(12) 0.25027(11) 0.0157(5) Uani 1 1 d . . . H110 H -0.2080 0.1457 0.2498 0.019 Uiso 1 1 calc R . . C111 C -0.1087(2) -0.25390(12) 0.2309(2) 0.0282(6) Uani 1 1 d . . . H11C H -0.1590 -0.2516 0.2577 0.034 Uiso 1 1 calc R . . H11D H -0.0760 -0.2938 0.2377 0.034 Uiso 1 1 calc R . . C112 C -0.36244(19) -0.07613(12) 0.23329(19) 0.0251(5) Uani 1 1 d . . . H11M H -0.4195 -0.0535 0.2407 0.030 Uiso 1 1 calc R . . H11N H -0.3585 -0.1121 0.2592 0.030 Uiso 1 1 calc R . . C113 C -0.36269(19) 0.07558(13) 0.23269(19) 0.0257(5) Uani 1 1 d . . . H11A H -0.3587 0.1114 0.2588 0.031 Uiso 1 1 calc R . . H11B H -0.4197 0.0530 0.2403 0.031 Uiso 1 1 calc R . . C114 C 0.1080(2) -0.25403(13) 0.2309(2) 0.0273(6) Uani 1 1 d . . . H11E H 0.0755 -0.2939 0.2385 0.033 Uiso 1 1 calc R . . H11F H 0.1596 -0.2515 0.2566 0.033 Uiso 1 1 calc R . . C115 C -0.1474(3) -0.25521(18) 0.17246(17) 0.0368(8) Uani 1 1 d . . . H11J H -0.1858 -0.2924 0.1681 0.055 Uiso 1 1 calc R . . H11K H -0.0981 -0.2570 0.1456 0.055 Uiso 1 1 calc R . . H11L H -0.1832 -0.2171 0.1662 0.055 Uiso 1 1 calc R . . C116 C -0.3630(3) -0.1013(2) 0.17269(18) 0.0406(9) Uani 1 1 d . . . H11G H -0.4150 -0.1291 0.1674 0.061 Uiso 1 1 calc R . . H11H H -0.3075 -0.1248 0.1656 0.061 Uiso 1 1 calc R . . H11I H -0.3671 -0.0657 0.1470 0.061 Uiso 1 1 calc R . . C117 C -0.3653(3) 0.10101(19) 0.17447(17) 0.0350(8) Uani 1 1 d . . . H11R H -0.4166 0.1297 0.1705 0.053 Uiso 1 1 calc R . . H11S H -0.3717 0.0660 0.1484 0.053 Uiso 1 1 calc R . . H11T H -0.3094 0.1238 0.1667 0.053 Uiso 1 1 calc R . . C118 C 0.1433(3) -0.25536(17) 0.17171(16) 0.0353(8) Uani 1 1 d . . . H11O H 0.1845 -0.2911 0.1672 0.053 Uiso 1 1 calc R . . H11P H 0.1754 -0.2160 0.1639 0.053 Uiso 1 1 calc R . . H11Q H 0.0927 -0.2598 0.1460 0.053 Uiso 1 1 calc R . . N1 N 0.0000 0.0000 0.35486(5) 0.0187(2) Uani 1 2 d S . . C1 C 0.0000 0.0000 0.46949(7) 0.0257(4) Uani 1 2 d S . . C2 C 0.0756(5) 0.0137(3) 0.4402(3) 0.0215(16) Uiso 0.26 1 d P A 1 H2 H 0.1303 0.0212 0.4594 0.026 Uiso 0.26 1 calc PR A 1 C3 C 0.0748(5) 0.0170(3) 0.3829(3) 0.0147(13) Uiso 0.26 1 d P A 1 H3 H 0.1266 0.0311 0.3635 0.018 Uiso 0.26 1 calc PR A 1 C4 C -0.0739(5) 0.0266(4) 0.4400(3) 0.0181(12) Uiso 0.30 1 d P A 2 H4 H -0.1243 0.0446 0.4583 0.022 Uiso 0.30 1 calc PR A 2 C5 C -0.0674(6) 0.0245(5) 0.3825(4) 0.0258(18) Uiso 0.30 1 d P A 2 H5 H -0.1155 0.0421 0.3618 0.031 Uiso 0.30 1 calc PR A 2 C6 C 0.0559(7) 0.0401(5) 0.4392(4) 0.0224(15) Uiso 0.22 1 d P A 3 H6 H 0.0943 0.0689 0.4578 0.027 Uiso 0.22 1 calc PR A 3 C7 C 0.0555(6) 0.0380(4) 0.3824(3) 0.0188(14) Uiso 0.22 1 d P A 3 H7 H 0.0956 0.0643 0.3624 0.023 Uiso 0.22 1 calc PR A 3 C8 C 0.0212(5) 0.0540(4) 0.4407(3) 0.0197(13) Uiso 0.22 1 d P A 4 H8 H 0.0363 0.0918 0.4596 0.024 Uiso 0.22 1 calc PR A 4 C9 C 0.0201(4) 0.0520(3) 0.3835(3) 0.0181(12) Uiso 0.22 1 d P A 4 H9 H 0.0343 0.0894 0.3637 0.022 Uiso 0.22 1 calc PR A 4 C301 C -0.0131(5) 0.1141(4) 0.1067(2) 0.0404(9) Uani 0.50 1 d PU . . C302 C 0.0121(6) 0.1563(5) 0.0504(5) 0.0431(13) Uani 0.50 1 d PU . . C303 C 0.0916(7) 0.1515(4) 0.0295(3) 0.0373(11) Uani 0.50 1 d PU . . C304 C 0.1641(12) 0.1157(9) 0.0505(9) 0.0497(15) Uani 0.50 1 d PU . . C305 C 0.1031(6) 0.0919(4) 0.1046(3) 0.0451(11) Uani 0.50 1 d PU . . C306 C -0.0485(6) 0.0798(4) 0.1238(3) 0.0436(10) Uani 0.50 1 d PU . . C311 C 0.0132(5) 0.1254(3) 0.0945(3) 0.0425(10) Uani 0.50 1 d PU . . C312 C 0.0471(7) 0.0786(4) 0.1257(3) 0.0477(11) Uani 0.50 1 d PU . . C313 C -0.0112(6) 0.0304(3) 0.1429(2) 0.0467(10) Uani 0.50 1 d PU . . C314 C -0.1136(6) 0.0364(5) 0.1249(3) 0.0438(12) Uani 0.50 1 d PU . . C315 C -0.1075(5) 0.1005(4) 0.0960(3) 0.0412(11) Uani 0.50 1 d PU . . C316 C -0.0084(7) 0.1536(6) 0.0574(4) 0.0383(12) Uani 0.50 1 d PU . . C307 C -0.1583(3) 0.1091(2) 0.0537(2) 0.0198(7) Uani 0.50 1 d PU . . C308 C 0.2168(9) -0.0050(5) 0.0585(4) 0.0323(14) Uani 0.50 1 d PU . . C309 C 0.1618(4) -0.0024(6) 0.1082(2) 0.0367(10) Uani 0.50 1 d PU . . C310 C 0.2189(4) -0.0592(3) 0.0301(2) 0.0210(9) Uani 0.50 1 d PU . . C317 C -0.0900(6) 0.1514(3) 0.0311(2) 0.0313(10) Uani 0.50 1 d PU . . C318 C 0.2157(4) 0.0630(4) 0.0311(2) 0.0304(9) Uani 0.50 1 d PU . . C319 C 0.1097(6) 0.0348(5) 0.1246(3) 0.0470(12) Uani 0.50 1 d PU . . C320 C -0.1333(7) 0.0764(4) 0.1011(3) 0.0446(12) Uani 0.50 1 d PU . . C321 C 0.1204(5) 0.1416(3) -0.0104(3) 0.0564(14) Uani 0.50 1 d PU . . C322 C -0.0461(5) 0.1621(3) -0.0066(4) 0.0652(17) Uani 0.50 1 d PU . . C323 C 0.2301(6) 0.0341(4) -0.0099(3) 0.0675(17) Uani 0.50 1 d PU . . C324 C 0.0383(5) 0.0133(3) 0.14166(19) 0.0467(10) Uani 0.50 1 d PU . . C325 C 0.2049(5) 0.0799(4) -0.0142(3) 0.0586(14) Uani 0.50 1 d PU . . C326 C 0.1614(11) 0.0997(6) 0.0548(7) 0.0479(13) Uani 0.50 1 d PU . . C327 C 0.1305(7) 0.0699(5) 0.1048(4) 0.0440(11) Uani 0.50 1 d PU . . C328 C 0.1778(5) 0.0106(3) 0.0965(3) 0.0412(12) Uani 0.50 1 d PU . . C329 C 0.2241(9) 0.0068(5) 0.0514(5) 0.0400(13) Uani 0.50 1 d PU . . C330 C 0.1469(11) 0.1131(9) 0.0532(9) 0.0488(15) Uani 0.50 1 d PU . . C401 C 0.5476(9) 0.0831(5) 0.3782(4) 0.0693(14) Uani 0.50 1 d PU . . C402 C 0.4673(11) 0.1601(5) 0.4684(5) 0.073(2) Uani 0.50 1 d PU . . C403 C 0.5546(9) 0.0125(6) 0.3599(4) 0.0646(16) Uani 0.50 1 d PU . . C404 C 0.6242(9) 0.1264(6) 0.5569(5) 0.080(3) Uani 0.50 1 d PU . . C405 C 0.6011(9) 0.0571(6) 0.3777(4) 0.0744(15) Uani 0.50 1 d PU . . C406 C 0.6994(10) 0.0286(6) 0.4244(5) 0.081(2) Uani 0.50 1 d PU . . C407 C 0.4664(9) 0.1045(5) 0.3904(5) 0.0639(14) Uani 0.50 1 d PU . . C408 C 0.4357(8) 0.0657(5) 0.3719(3) 0.0646(14) Uani 0.50 1 d PU . . C409 C 0.6998(9) 0.0767(6) 0.4596(5) 0.084(2) Uani 0.50 1 d PU . . C410 C 0.5566(9) 0.1444(5) 0.4356(5) 0.0728(14) Uani 0.50 1 d PU . . C411 C 0.3170(10) 0.0750(9) 0.4255(7) 0.102(4) Uani 0.50 1 d PU . . C412 C 0.6172(6) -0.0196(4) 0.3730(3) 0.0683(14) Uani 0.50 1 d PU . . C413 C 0.6446(10) 0.1061(5) 0.4322(5) 0.0772(14) Uani 0.50 1 d PU . . C414 C 0.6664(8) 0.0414(6) 0.4043(5) 0.0770(17) Uani 0.50 1 d PU . . C415 C 0.6906(6) -0.0070(6) 0.4108(4) 0.0695(15) Uani 0.50 1 d PU . . C416 C 0.4127(9) 0.0864(4) 0.3879(4) 0.0607(13) Uani 0.50 1 d PU . . C417 C 0.4696(7) 0.1470(3) 0.4349(3) 0.0662(13) Uani 0.50 1 d PU . . C418 C 0.6431(10) 0.1323(6) 0.4651(7) 0.0808(19) Uani 0.50 1 d PU . . C419 C 0.3590(8) 0.0787(5) 0.4063(4) 0.0696(18) Uani 0.50 1 d PU . . C420 C 0.5114(12) 0.1637(3) 0.4724(4) 0.0644(16) Uani 0.50 1 d PU . . C421 C 0.6132(9) 0.1009(6) 0.4054(5) 0.0781(14) Uani 0.50 1 d PU . . C422 C 0.5040(13) 0.1065(5) 0.3859(3) 0.0631(12) Uani 0.50 1 d PU . . C423 C 0.7166(8) 0.0737(5) 0.5144(4) 0.0777(19) Uani 0.50 1 d PU . . C424 C 0.4642(8) 0.0133(5) 0.3563(4) 0.0626(16) Uani 0.50 1 d PU . . C425 C 0.6593(6) 0.1247(3) 0.5038(7) 0.0779(15) Uani 0.50 1 d PU . . C426 C 0.7333(9) 0.0226(5) 0.4750(4) 0.083(2) Uani 0.50 1 d PU . . C427 C 0.7048(9) -0.0508(6) 0.4424(6) 0.083(3) Uani 0.50 1 d PU . . C428 C 0.7283(6) 0.0401(4) 0.5029(6) 0.0707(15) Uani 0.50 1 d PU . . C429 C 0.3989(13) 0.1427(8) 0.4686(6) 0.077(2) Uani 0.50 1 d PU . . C430 C 0.6088(14) 0.1448(7) 0.4675(8) 0.080(2) Uani 0.50 1 d PU . . C501 C 0.49082(17) 0.7228(3) 0.02832(11) 0.0847(19) Uani 0.709(6) 1 d PDU . 1 N501 N 0.4055(3) 0.7345(3) 0.0492(2) 0.171(5) Uani 0.709(6) 1 d PDU . 1 N502 N 0.5584(4) 0.7111(3) 0.06694(15) 0.152(4) Uani 0.709(6) 1 d PDU . 1 C502 C 0.3456(6) 0.7785(7) 0.0272(5) 0.226(8) Uani 0.709(6) 1 d PDU . 1 H50A H 0.2898 0.7783 0.0488 0.339 Uiso 0.709(6) 1 calc PR . 1 H50B H 0.3323 0.7675 -0.0113 0.339 Uiso 0.709(6) 1 calc PR . 1 H50C H 0.3728 0.8205 0.0286 0.339 Uiso 0.709(6) 1 calc PR . 1 C503 C 0.3696(5) 0.7036(5) 0.0954(3) 0.135(4) Uani 0.709(6) 1 d PDU . 1 H50D H 0.3095 0.7205 0.1033 0.203 Uiso 0.709(6) 1 calc PR . 1 H50E H 0.4088 0.7105 0.1273 0.203 Uiso 0.709(6) 1 calc PR . 1 H50F H 0.3652 0.6584 0.0877 0.203 Uiso 0.709(6) 1 calc PR . 1 C504 C 0.6217(8) 0.6631(6) 0.0615(4) 0.202(7) Uani 0.709(6) 1 d PDU . 1 H50G H 0.6623 0.6637 0.0934 0.302 Uiso 0.709(6) 1 calc PR . 1 H50H H 0.6565 0.6696 0.0276 0.302 Uiso 0.709(6) 1 calc PR . 1 H50I H 0.5908 0.6224 0.0598 0.302 Uiso 0.709(6) 1 calc PR . 1 C505 C 0.5701(9) 0.7463(6) 0.1149(3) 0.234(8) Uani 0.709(6) 1 d PDU . 1 H50J H 0.6207 0.7292 0.1361 0.351 Uiso 0.709(6) 1 calc PR . 1 H50K H 0.5152 0.7443 0.1373 0.351 Uiso 0.709(6) 1 calc PR . 1 H50L H 0.5826 0.7903 0.1052 0.351 Uiso 0.709(6) 1 calc PR . 1 C511 C 0.51132(14) 0.7224(2) 0.02803(11) 0.0270(16) Uani 0.291(6) 1 d PDU . 2 N511 N 0.4505(3) 0.7049(3) 0.06876(12) 0.0384(19) Uani 0.291(6) 1 d PDU . 2 N512 N 0.5972(2) 0.7395(3) 0.04559(19) 0.042(2) Uani 0.291(6) 1 d PDU . 2 C512 C 0.3824(4) 0.6605(5) 0.0611(3) 0.052(3) Uani 0.291(6) 1 d PDU . 2 H51A H 0.3485 0.6554 0.0955 0.078 Uiso 0.291(6) 1 calc PR . 2 H51B H 0.4091 0.6200 0.0506 0.078 Uiso 0.291(6) 1 calc PR . 2 H51C H 0.3418 0.6748 0.0317 0.078 Uiso 0.291(6) 1 calc PR . 2 C513 C 0.4505(7) 0.7299(6) 0.1221(2) 0.079(4) Uani 0.291(6) 1 d PDU . 2 H51D H 0.4025 0.7101 0.1438 0.119 Uiso 0.291(6) 1 calc PR . 2 H51E H 0.4403 0.7754 0.1203 0.119 Uiso 0.291(6) 1 calc PR . 2 H51F H 0.5088 0.7216 0.1396 0.119 Uiso 0.291(6) 1 calc PR . 2 C514 C 0.6468(5) 0.7881(6) 0.0218(4) 0.077(4) Uani 0.291(6) 1 d PDU . 2 H51G H 0.7044 0.7924 0.0412 0.116 Uiso 0.291(6) 1 calc PR . 2 H51H H 0.6130 0.8276 0.0248 0.116 Uiso 0.291(6) 1 calc PR . 2 H51I H 0.6578 0.7786 -0.0172 0.116 Uiso 0.291(6) 1 calc PR . 2 C515 C 0.6428(6) 0.7098(5) 0.0887(4) 0.061(3) Uani 0.291(6) 1 d PDU . 2 H51J H 0.7018 0.7297 0.0936 0.091 Uiso 0.291(6) 1 calc PR . 2 H51K H 0.6508 0.6651 0.0799 0.091 Uiso 0.291(6) 1 calc PR . 2 H51L H 0.6078 0.7139 0.1228 0.091 Uiso 0.291(6) 1 calc PR . 2 Cl1 Cl 0.4876(2) -0.1128(5) 0.0648(7) 0.119(4) Uiso 0.062 1 d PD B 1 Cl2 Cl 0.4803(5) -0.1143(5) -0.0620(7) 0.119(4) Uiso 0.062 1 d PD B 1 C2S C 0.49326(18) -0.0447(2) 0.0293(4) 0.0630(10) Uiso 0.062 1 d PD B 1 C3S C 0.5013(3) 0.0122(4) 0.0573(3) 0.0630(10) Uiso 0.062 1 d PD B 1 H3S H 0.5035 0.0126 0.0966 0.076 Uiso 0.062 1 calc PR B 1 C4S C 0.5059(4) 0.0684(2) 0.0280(5) 0.0630(10) Uiso 0.062 1 d PD B 1 H4S H 0.5114 0.1073 0.0472 0.076 Uiso 0.062 1 calc PR B 1 C5S C 0.5026(4) 0.0677(3) -0.0294(5) 0.0630(10) Uiso 0.062 1 d PD B 1 H5S H 0.5058 0.1061 -0.0495 0.076 Uiso 0.062 1 calc PR B 1 C6S C 0.4946(5) 0.0108(4) -0.0574(3) 0.0630(10) Uiso 0.062 1 d PD B 1 H6S H 0.4924 0.0103 -0.0967 0.076 Uiso 0.062 1 calc PR B 1 C7S C 0.4899(3) -0.0454(3) -0.0281(4) 0.0630(10) Uiso 0.062 1 d PD B 1 C12S C 0.4767(5) -0.0426(3) 0.0296(4) 0.0630(10) Uiso 0.188 1 d PD C 2 H12S H 0.4622 -0.0796 0.0499 0.076 Uiso 0.188 1 calc PR C 2 C13S C 0.5013(3) 0.0122(4) 0.0573(3) 0.0630(10) Uiso 0.188 1 d PD C 2 H13S H 0.5035 0.0126 0.0966 0.076 Uiso 0.188 1 calc PR C 2 C14S C 0.5225(4) 0.0663(3) 0.0277(5) 0.0630(10) Uiso 0.188 1 d PD C 2 H14S H 0.5392 0.1037 0.0466 0.076 Uiso 0.188 1 calc PR C 2 C15S C 0.5191(5) 0.0656(3) -0.0297(5) 0.0630(10) Uiso 0.188 1 d PD C 2 H15S H 0.5336 0.1025 -0.0500 0.076 Uiso 0.188 1 calc PR C 2 C16S C 0.4946(5) 0.0108(4) -0.0574(3) 0.0630(10) Uiso 0.188 1 d PD C 2 H16S H 0.4924 0.0103 -0.0967 0.076 Uiso 0.188 1 calc PR C 2 C17S C 0.4734(5) -0.0433(3) -0.0278(4) 0.0630(10) Uiso 0.188 1 d PD C 2 H17S H 0.4567 -0.0807 -0.0467 0.076 Uiso 0.188 1 calc PR C 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn 0.01523(8) 0.00873(8) 0.01007(8) 0.000 0.000 0.00056(16) N101 0.0154(3) 0.0092(3) 0.0160(4) 0.0004(3) 0.0005(9) 0.0019(10) N102 0.0154(4) 0.0099(3) 0.0147(3) -0.0013(9) 0.0011(3) -0.0042(9) C101 0.0215(12) 0.0086(9) 0.0313(17) 0.0013(10) 0.0008(11) -0.0047(8) C102 0.0171(11) 0.0098(10) 0.0183(10) 0.0003(8) 0.0025(8) -0.0026(8) C103 0.0160(11) 0.0113(10) 0.0166(10) 0.0011(8) 0.0022(9) -0.0015(8) C104 0.0149(11) 0.0151(10) 0.0264(16) -0.0007(10) 0.0039(9) -0.0014(9) C105 0.0136(11) 0.0160(10) 0.0212(14) -0.0004(9) 0.0015(8) 0.0008(8) C106 0.0148(11) 0.0128(10) 0.0157(10) 0.0007(8) 0.0017(8) 0.0005(8) C107 0.0196(12) 0.0090(10) 0.0190(10) 0.0010(8) 0.0012(8) 0.0002(9) C108 0.0217(12) 0.0087(9) 0.0287(16) -0.0004(9) 0.0002(10) -0.0017(8) C109 0.0186(12) 0.0118(10) 0.0194(11) -0.0010(8) 0.0021(9) -0.0037(9) C110 0.0158(11) 0.0110(10) 0.0201(11) -0.0019(8) 0.0017(8) 0.0008(8) C111 0.0256(13) 0.0084(10) 0.0507(17) 0.0001(15) 0.0044(17) -0.0032(8) C112 0.0159(12) 0.0187(11) 0.0405(14) -0.0078(14) 0.0020(15) -0.0044(9) C113 0.0145(11) 0.0238(12) 0.0388(14) -0.0052(15) 0.0018(15) 0.0046(9) C114 0.0264(13) 0.0126(11) 0.0427(16) -0.0019(15) 0.0032(16) 0.0045(9) C115 0.0369(19) 0.0272(16) 0.046(2) -0.0088(14) -0.0018(14) -0.0106(14) C116 0.035(2) 0.043(2) 0.044(2) -0.0107(16) -0.0107(15) -0.0130(16) C117 0.0279(17) 0.0358(19) 0.0413(19) 0.0038(14) -0.0085(13) 0.0085(13) C118 0.0362(18) 0.0228(14) 0.047(2) -0.0181(14) 0.0008(14) 0.0062(12) N1 0.0243(6) 0.0214(6) 0.0105(5) 0.000 0.000 -0.0047(17) C1 0.0277(8) 0.0371(10) 0.0124(6) 0.000 0.000 -0.011(2) C301 0.055(2) 0.047(2) 0.0196(18) -0.0170(13) 0.0068(16) 0.0045(17) C302 0.054(3) 0.024(2) 0.052(4) -0.014(2) 0.005(2) -0.016(2) C303 0.059(2) 0.027(3) 0.025(2) -0.0082(18) -0.0023(19) -0.027(2) C304 0.042(3) 0.040(3) 0.067(3) -0.007(2) -0.006(2) -0.022(3) C305 0.046(2) 0.051(3) 0.038(2) -0.022(2) -0.0132(19) -0.0033(19) C306 0.0702(19) 0.045(3) 0.015(2) -0.0084(18) 0.0174(19) 0.0122(19) C311 0.049(3) 0.044(2) 0.035(3) -0.0246(15) -0.0004(17) 0.0001(17) C312 0.067(2) 0.057(3) 0.020(2) -0.016(2) 0.002(2) 0.000(2) C313 0.062(3) 0.065(3) 0.0135(14) -0.0085(15) -0.0024(19) 0.000(2) C314 0.044(2) 0.073(3) 0.015(2) -0.007(2) 0.012(2) 0.015(2) C315 0.0395(19) 0.049(3) 0.035(2) -0.0231(19) 0.0160(17) -0.0035(18) C316 0.052(3) 0.033(3) 0.0299(18) -0.0100(14) 0.016(2) -0.014(3) C307 0.0167(15) 0.0192(16) 0.0237(16) -0.0120(14) 0.0096(12) 0.0068(13) C308 0.023(3) 0.047(3) 0.0269(18) 0.011(2) -0.0077(14) -0.009(3) C309 0.0266(18) 0.069(3) 0.0149(17) 0.010(3) -0.0071(11) -0.006(3) C310 0.0130(18) 0.042(2) 0.0076(14) 0.0048(14) -0.0053(13) -0.0007(16) C317 0.063(3) 0.023(3) 0.0076(16) -0.0062(14) -0.0027(17) 0.014(2) C318 0.020(2) 0.052(2) 0.019(2) 0.0053(17) -0.0086(15) -0.0273(16) C319 0.049(2) 0.071(4) 0.021(3) -0.008(2) -0.013(2) -0.006(2) C320 0.056(2) 0.034(3) 0.043(3) -0.008(2) 0.034(2) 0.004(2) C321 0.066(3) 0.039(2) 0.064(3) 0.006(3) 0.028(3) -0.0144(19) C322 0.079(3) 0.057(3) 0.059(3) 0.029(4) 0.027(3) 0.021(3) C323 0.068(4) 0.086(3) 0.048(3) -0.013(2) 0.023(3) -0.018(3) C324 0.061(2) 0.069(3) 0.0098(13) -0.0063(16) -0.0042(15) -0.0012(19) C325 0.034(2) 0.085(4) 0.056(3) 0.034(3) 0.003(2) -0.012(2) C326 0.042(3) 0.039(3) 0.063(3) -0.011(2) -0.004(2) -0.020(2) C327 0.047(2) 0.051(3) 0.034(2) -0.016(2) -0.020(2) -0.0004(19) C328 0.042(3) 0.052(3) 0.029(3) 0.0050(17) -0.0178(16) -0.002(2) C329 0.020(2) 0.051(3) 0.049(4) -0.001(2) -0.009(2) -0.011(3) C330 0.046(4) 0.038(3) 0.062(3) -0.008(2) -0.008(3) -0.020(3) C401 0.112(3) 0.062(4) 0.034(3) 0.016(2) 0.020(2) 0.000(2) C402 0.132(4) 0.045(5) 0.042(3) 0.015(3) 0.012(5) 0.021(5) C403 0.103(4) 0.064(4) 0.026(4) 0.007(2) 0.027(3) 0.001(3) C404 0.104(7) 0.075(7) 0.062(4) -0.034(5) -0.004(5) -0.042(5) C405 0.098(4) 0.090(4) 0.036(3) 0.009(2) 0.026(2) -0.004(3) C406 0.109(6) 0.077(4) 0.057(4) -0.001(3) 0.007(3) -0.008(3) C407 0.110(3) 0.042(3) 0.040(3) 0.0258(19) 0.010(3) 0.000(3) C408 0.103(3) 0.071(4) 0.020(2) 0.009(2) -0.005(3) 0.023(3) C409 0.106(5) 0.075(4) 0.072(4) -0.009(3) 0.001(3) -0.014(3) C410 0.120(3) 0.044(3) 0.055(3) 0.015(2) 0.024(2) -0.022(2) C411 0.076(5) 0.123(9) 0.107(9) 0.025(7) 0.012(5) 0.027(5) C412 0.074(3) 0.082(3) 0.049(3) -0.014(3) 0.027(2) -0.008(2) C413 0.108(4) 0.058(3) 0.065(3) 0.018(2) 0.018(2) -0.024(2) C414 0.083(4) 0.085(4) 0.063(4) -0.002(3) 0.015(3) -0.014(3) C415 0.063(3) 0.083(4) 0.063(3) -0.018(3) 0.020(2) -0.009(4) C416 0.107(3) 0.038(3) 0.037(3) 0.018(2) 0.007(3) 0.008(3) C417 0.131(4) 0.024(2) 0.043(2) 0.0183(15) 0.004(3) 0.012(2) C418 0.113(5) 0.045(4) 0.084(4) 0.007(3) 0.008(4) -0.031(3) C419 0.089(4) 0.062(4) 0.058(4) 0.032(3) 0.003(3) 0.021(3) C420 0.137(4) 0.0084(17) 0.048(3) 0.0058(17) 0.008(3) -0.007(3) C421 0.109(3) 0.068(3) 0.058(3) 0.016(2) 0.020(2) -0.017(2) C422 0.115(3) 0.048(2) 0.0260(18) 0.0248(15) 0.025(3) 0.001(2) C423 0.103(6) 0.067(4) 0.063(3) 0.000(3) 0.012(3) -0.017(3) C424 0.112(4) 0.063(3) 0.013(2) 0.004(2) -0.002(3) 0.011(3) C425 0.099(4) 0.055(3) 0.080(3) -0.007(3) 0.009(3) -0.029(2) C426 0.120(7) 0.078(4) 0.051(3) 0.008(2) 0.009(3) -0.007(3) C427 0.101(7) 0.076(4) 0.073(5) -0.025(3) 0.019(4) 0.028(4) C428 0.089(4) 0.056(3) 0.067(4) -0.016(3) 0.005(4) -0.013(3) C429 0.108(4) 0.056(6) 0.066(5) 0.018(4) -0.001(4) 0.045(5) C430 0.119(5) 0.044(4) 0.077(4) 0.009(3) 0.012(4) -0.026(3) C501 0.075(3) 0.107(5) 0.072(3) 0.000(4) 0.007(3) 0.007(4) N501 0.136(6) 0.151(8) 0.226(10) 0.083(7) 0.106(6) 0.059(6) N502 0.183(8) 0.132(8) 0.141(7) -0.066(6) -0.091(6) 0.056(6) C502 0.182(11) 0.266(15) 0.229(15) 0.007(10) 0.023(10) 0.146(11) C503 0.109(7) 0.231(11) 0.066(5) -0.036(5) 0.035(4) -0.055(7) C504 0.141(10) 0.221(13) 0.243(14) 0.065(10) 0.006(10) 0.097(9) C505 0.333(17) 0.285(15) 0.083(7) -0.071(8) -0.040(8) -0.078(11) C511 0.030(3) 0.045(3) 0.0057(18) -0.009(2) -0.0001(17) -0.016(3) N511 0.032(3) 0.070(5) 0.014(2) 0.006(2) 0.012(2) 0.002(3) N512 0.030(3) 0.054(5) 0.042(4) -0.003(3) -0.026(3) -0.016(3) C512 0.017(3) 0.099(8) 0.039(4) 0.024(4) 0.006(3) -0.014(3) C513 0.055(6) 0.153(13) 0.029(4) -0.023(5) 0.016(4) -0.009(7) C514 0.029(4) 0.104(9) 0.099(9) 0.006(7) 0.003(5) -0.039(5) C515 0.051(6) 0.064(6) 0.067(7) -0.019(4) -0.038(5) 0.012(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn N102 2.0683(9) . ? Zn N102 2.0683(9) 2 ? Zn N101 2.0728(9) . ? Zn N101 2.0728(9) 2 ? Zn N1 2.1113(13) . ? N101 C102 1.358(4) . ? N101 C107 1.377(4) . ? N102 C106 1.365(4) . ? N102 C103 1.369(3) . ? C101 C108 1.3671(18) . ? C101 C102 1.453(4) . ? C101 C111 1.504(4) . ? C102 C109 1.398(4) . ? C103 C109 1.388(4) . ? C103 C104 1.456(4) . ? C104 C105 1.3645(16) . ? C104 C112 1.494(4) . ? C105 C106 1.447(4) . ? C105 C113 1.498(4) . ? C106 C110 1.402(4) . ? C107 C110 1.393(4) 2 ? C107 C108 1.451(4) . ? C108 C114 1.495(4) . ? C109 H109 0.9500 . ? C110 C107 1.393(4) 2 ? C110 H110 0.9500 . ? C111 C115 1.527(6) . ? C111 H11C 0.9900 . ? C111 H11D 0.9900 . ? C112 C116 1.561(6) . ? C112 H11M 0.9900 . ? C112 H11N 0.9900 . ? C113 C117 1.509(6) . ? C113 H11A 0.9900 . ? C113 H11B 0.9900 . ? C114 C118 1.525(6) . ? C114 H11E 0.9900 . ? C114 H11F 0.9900 . ? C115 H11J 0.9800 . ? C115 H11K 0.9800 . ? C115 H11L 0.9800 . ? C116 H11G 0.9800 . ? C116 H11H 0.9800 . ? C116 H11I 0.9800 . ? C117 H11R 0.9800 . ? C117 H11S 0.9800 . ? C117 H11T 0.9800 . ? C118 H11O 0.9800 . ? C118 H11P 0.9800 . ? C118 H11Q 0.9800 . ? N1 C5 1.311(9) 2 ? N1 C5 1.311(9) . ? N1 C7 1.332(8) . ? N1 C7 1.332(8) 2 ? N1 C9 1.338(7) . ? N1 C9 1.338(7) 2 ? N1 C3 1.351(7) 2 ? N1 C3 1.351(7) . ? C1 C2 1.359(7) . ? C1 C2 1.359(7) 2 ? C1 C8 1.378(7) 2 ? C1 C8 1.378(7) . ? C1 C6 1.396(9) . ? C1 C6 1.396(9) 2 ? C1 C4 1.426(7) 2 ? C1 C4 1.426(7) . ? C1 C1 1.477(3) 3_556 ? C2 C3 1.390(10) . ? C2 H2 0.9500 . ? C3 H3 0.9500 . ? C4 C5 1.395(11) . ? C4 H4 0.9500 . ? C5 H5 0.9500 . ? C6 C7 1.375(12) . ? C6 H6 0.9500 . ? C7 H7 0.9500 . ? C8 C9 1.383(10) . ? C8 H8 0.9500 . ? C9 H9 0.9500 . ? C501 N501 1.388(2) . ? C501 N502 1.394(2) . ? C501 C501 1.398(5) 4_655 ? N501 C502 1.394(3) . ? N501 C503 1.400(3) . ? N502 C504 1.392(3) . ? N502 C505 1.392(3) . ? C502 H50A 0.9800 . ? C502 H50B 0.9800 . ? C502 H50C 0.9800 . ? C503 H50D 0.9800 . ? C503 H50E 0.9800 . ? C503 H50F 0.9800 . ? C504 H50G 0.9800 . ? C504 H50H 0.9800 . ? C504 H50I 0.9800 . ? C505 H50J 0.9800 . ? C505 H50K 0.9800 . ? C505 H50L 0.9800 . ? C511 N511 1.387(2) . ? C511 N512 1.393(2) . ? C511 C511 1.398(5) 4_655 ? N511 C513 1.395(3) . ? N511 C512 1.396(3) . ? N512 C514 1.392(3) . ? N512 C515 1.393(3) . ? C512 H51A 0.9800 . ? C512 H51B 0.9800 . ? C512 H51C 0.9800 . ? C513 H51D 0.9800 . ? C513 H51E 0.9800 . ? C513 H51F 0.9800 . ? C514 H51G 0.9800 . ? C514 H51H 0.9800 . ? C514 H51I 0.9800 . ? C515 H51J 0.9800 . ? C515 H51K 0.9800 . ? C515 H51L 0.9800 . ? Cl1 C2S 1.683(7) . ? Cl2 C7S 1.683(7) . ? C2S C3S 1.3898(9) . ? C2S C7S 1.3901(9) . ? C3S C4S 1.3899(9) . ? C3S H3S 0.9500 . ? C4S C5S 1.3900(9) . ? C4S H4S 0.9500 . ? C5S C6S 1.3899(9) . ? C5S H5S 0.9500 . ? C6S C7S 1.3897(9) . ? C6S H6S 0.9500 . ? C12S C17S 1.3903(9) . ? C12S H12S 0.9500 . ? C14S C15S 1.3902(9) . ? C14S H14S 0.9500 . ? C15S H15S 0.9500 . ? C17S H17S 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N102 Zn N102 164.13(5) . 2 ? N102 Zn N101 88.88(11) . . ? N102 Zn N101 88.88(11) 2 . ? N102 Zn N101 88.88(11) . 2 ? N102 Zn N101 88.88(11) 2 2 ? N101 Zn N101 163.72(5) . 2 ? N102 Zn N1 97.93(3) . . ? N102 Zn N1 97.93(3) 2 . ? N101 Zn N1 98.14(3) . . ? N101 Zn N1 98.14(3) 2 . ? C102 N101 C107 106.46(9) . . ? C102 N101 Zn 127.15(19) . . ? C107 N101 Zn 126.38(19) . . ? C106 N102 C103 106.34(9) . . ? C106 N102 Zn 127.65(18) . . ? C103 N102 Zn 126.00(19) . . ? C108 C101 C102 106.5(3) . . ? C108 C101 C111 128.4(3) . . ? C102 C101 C111 125.0(3) . . ? N101 C102 C109 124.8(2) . . ? N101 C102 C101 110.5(2) . . ? C109 C102 C101 124.6(2) . . ? N102 C103 C109 126.0(3) . . ? N102 C103 C104 110.0(2) . . ? C109 C103 C104 123.9(3) . . ? C105 C104 C103 106.6(3) . . ? C105 C104 C112 127.8(3) . . ? C103 C104 C112 125.6(2) . . ? C104 C105 C106 106.4(3) . . ? C104 C105 C113 128.8(3) . . ? C106 C105 C113 124.6(2) . . ? N102 C106 C110 124.0(2) . . ? N102 C106 C105 110.6(2) . . ? C110 C106 C105 125.3(3) . . ? N101 C107 C110 125.0(2) . 2 ? N101 C107 C108 110.1(2) . . ? C110 C107 C108 124.8(2) 2 . ? C101 C108 C107 106.4(3) . . ? C101 C108 C114 127.9(3) . . ? C107 C108 C114 125.5(3) . . ? C103 C109 C102 126.4(2) . . ? C103 C109 H109 116.8 . . ? C102 C109 H109 116.8 . . ? C107 C110 C106 127.3(3) 2 . ? C107 C110 H110 116.3 2 . ? C106 C110 H110 116.3 . . ? C101 C111 C115 113.6(3) . . ? C101 C111 H11C 108.9 . . ? C115 C111 H11C 108.9 . . ? C101 C111 H11D 108.9 . . ? C115 C111 H11D 108.9 . . ? H11C C111 H11D 107.7 . . ? C104 C112 C116 111.3(3) . . ? C104 C112 H11M 109.4 . . ? C116 C112 H11M 109.4 . . ? C104 C112 H11N 109.4 . . ? C116 C112 H11N 109.4 . . ? H11M C112 H11N 108.0 . . ? C105 C113 C117 113.5(3) . . ? C105 C113 H11A 108.9 . . ? C117 C113 H11A 108.9 . . ? C105 C113 H11B 108.9 . . ? C117 C113 H11B 108.9 . . ? H11A C113 H11B 107.7 . . ? C108 C114 C118 112.7(3) . . ? C108 C114 H11E 109.1 . . ? C118 C114 H11E 109.1 . . ? C108 C114 H11F 109.1 . . ? C118 C114 H11F 109.1 . . ? H11E C114 H11F 107.8 . . ? C111 C115 H11J 109.5 . . ? C111 C115 H11K 109.5 . . ? H11J C115 H11K 109.5 . . ? C111 C115 H11L 109.5 . . ? H11J C115 H11L 109.5 . . ? H11K C115 H11L 109.5 . . ? C112 C116 H11G 109.5 . . ? C112 C116 H11H 109.5 . . ? H11G C116 H11H 109.5 . . ? C112 C116 H11I 109.5 . . ? H11G C116 H11I 109.5 . . ? H11H C116 H11I 109.5 . . ? C113 C117 H11R 109.5 . . ? C113 C117 H11S 109.5 . . ? H11R C117 H11S 109.5 . . ? C113 C117 H11T 109.5 . . ? H11R C117 H11T 109.5 . . ? H11S C117 H11T 109.5 . . ? C114 C118 H11O 109.5 . . ? C114 C118 H11P 109.5 . . ? H11O C118 H11P 109.5 . . ? C114 C118 H11Q 109.5 . . ? H11O C118 H11Q 109.5 . . ? H11P C118 H11Q 109.5 . . ? C5 N1 C5 118.6(8) 2 . ? C7 N1 C7 120.0(7) . 2 ? C9 N1 C9 117.5(6) . 2 ? C3 N1 C3 119.8(6) 2 . ? C5 N1 Zn 120.7(4) 2 . ? C5 N1 Zn 120.7(4) . . ? C7 N1 Zn 120.0(4) . . ? C7 N1 Zn 120.0(4) 2 . ? C9 N1 Zn 121.2(3) . . ? C9 N1 Zn 121.2(3) 2 . ? C3 N1 Zn 120.1(3) 2 . ? C3 N1 Zn 120.1(3) . . ? C2 C1 C2 117.1(6) . 2 ? C8 C1 C8 119.1(6) 2 . ? C6 C1 C6 116.6(7) . 2 ? C4 C1 C4 119.9(5) 2 . ? C2 C1 C1 121.4(3) . 3_556 ? C2 C1 C1 121.4(3) 2 3_556 ? C1 C2 C3 121.7(6) . . ? C1 C2 H2 119.2 . . ? C3 C2 H2 119.2 . . ? N1 C3 C2 119.6(6) . . ? N1 C3 H3 120.2 . . ? C2 C3 H3 120.2 . . ? C5 C4 C1 115.7(6) . . ? C5 C4 H4 122.2 . . ? C1 C4 H4 122.2 . . ? N1 C5 C4 125.1(8) . . ? N1 C5 H5 117.5 . . ? C4 C5 H5 117.5 . . ? C7 C6 C1 120.2(7) . . ? C7 C6 H6 119.9 . . ? C1 C6 H6 119.9 . . ? N1 C7 C6 121.5(7) . . ? N1 C7 H7 119.3 . . ? C6 C7 H7 119.3 . . ? C1 C8 C9 118.6(6) . . ? C1 C8 H8 120.7 . . ? C9 C8 H8 120.7 . . ? N1 C9 C8 123.1(6) . . ? N1 C9 H9 118.5 . . ? C8 C9 H9 118.5 . . ? N501 C501 N502 116.5(3) . . ? N501 C501 C501 122.41(19) . 4_655 ? N502 C501 C501 121.1(2) . 4_655 ? C501 N501 C502 124.3(3) . . ? C501 N501 C503 123.7(3) . . ? C502 N501 C503 112.0(4) . . ? C504 N502 C505 112.8(5) . . ? C504 N502 C501 123.6(3) . . ? C505 N502 C501 123.6(3) . . ? N501 C502 H50A 109.5 . . ? N501 C502 H50B 109.5 . . ? H50A C502 H50B 109.5 . . ? N501 C502 H50C 109.5 . . ? H50A C502 H50C 109.5 . . ? H50B C502 H50C 109.5 . . ? N501 C503 H50D 109.5 . . ? N501 C503 H50E 109.5 . . ? H50D C503 H50E 109.5 . . ? N501 C503 H50F 109.5 . . ? H50D C503 H50F 109.5 . . ? H50E C503 H50F 109.5 . . ? N502 C504 H50G 109.5 . . ? N502 C504 H50H 109.5 . . ? H50G C504 H50H 109.5 . . ? N502 C504 H50I 109.5 . . ? H50G C504 H50I 109.5 . . ? H50H C504 H50I 109.5 . . ? N502 C505 H50J 109.5 . . ? N502 C505 H50K 109.5 . . ? H50J C505 H50K 109.5 . . ? N502 C505 H50L 109.5 . . ? H50J C505 H50L 109.5 . . ? H50K C505 H50L 109.5 . . ? N511 C511 N512 116.7(3) . . ? N511 C511 C511 122.20(19) . 4_655 ? N512 C511 C511 121.11(18) . 4_655 ? C511 N511 C513 123.8(3) . . ? C511 N511 C512 123.9(3) . . ? C513 N511 C512 112.3(4) . . ? C514 N512 C511 123.4(3) . . ? C514 N512 C515 112.7(4) . . ? C511 N512 C515 123.8(3) . . ? N511 C512 H51A 109.5 . . ? N511 C512 H51B 109.5 . . ? H51A C512 H51B 109.5 . . ? N511 C512 H51C 109.5 . . ? H51A C512 H51C 109.5 . . ? H51B C512 H51C 109.5 . . ? N511 C513 H51D 109.5 . . ? N511 C513 H51E 109.5 . . ? H51D C513 H51E 109.5 . . ? N511 C513 H51F 109.5 . . ? H51D C513 H51F 109.5 . . ? H51E C513 H51F 109.5 . . ? N512 C514 H51G 109.5 . . ? N512 C514 H51H 109.5 . . ? H51G C514 H51H 109.5 . . ? N512 C514 H51I 109.5 . . ? H51G C514 H51I 109.5 . . ? H51H C514 H51I 109.5 . . ? N512 C515 H51J 109.5 . . ? N512 C515 H51K 109.5 . . ? H51J C515 H51K 109.5 . . ? N512 C515 H51L 109.5 . . ? H51J C515 H51L 109.5 . . ? H51K C515 H51L 109.5 . . ? C3S C2S C7S 119.99(6) . . ? C3S C2S Cl1 120.03(10) . . ? C7S C2S Cl1 119.98(10) . . ? C2S C3S C4S 120.01(6) . . ? C2S C3S H3S 120.0 . . ? C4S C3S H3S 120.0 . . ? C3S C4S C5S 119.99(6) . . ? C3S C4S H4S 120.0 . . ? C5S C4S H4S 120.0 . . ? C6S C5S C4S 119.99(6) . . ? C6S C5S H5S 120.0 . . ? C4S C5S H5S 120.0 . . ? C7S C6S C5S 120.01(6) . . ? C7S C6S H6S 120.0 . . ? C5S C6S H6S 120.0 . . ? C6S C7S C2S 120.00(6) . . ? C6S C7S Cl2 120.03(10) . . ? C2S C7S Cl2 119.98(10) . . ? C17S C12S H12S 120.0 . . ? C15S C14S H14S 120.0 . . ? C14S C15S H15S 120.0 . . ? C12S C17S H17S 120.0 . . ? _diffrn_measured_fraction_theta_max 0.975 _diffrn_reflns_theta_full 34.50 _diffrn_measured_fraction_theta_full 0.975 _refine_diff_density_max 1.148 _refine_diff_density_min -0.595 _refine_diff_density_rms 0.103