# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _publ_contact_author_name 'Eduardo C. Escudero-Adan' _publ_contact_author_email eescudero@iciq.es loop_ _publ_author_name E.C.Escudero-Adan 'P.W.N.M.van Leeuwen' # Attachment '- 9Eprime-SP12401_0mX_ultima.cif' data_sp12401_0m _database_code_depnum_ccdc_archive 'CCDC 825586' #TrackingRef '- 9Eprime-SP12401_0mX_ultima.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C66 H70 N4 O10 P2 Zn2' _chemical_formula_weight 1271.94 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' P P 0.1023 0.0942 '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 P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 18.8474(12) _cell_length_b 7.8500(5) _cell_length_c 20.6464(13) _cell_angle_alpha 90.00 _cell_angle_beta 98.266(3) _cell_angle_gamma 90.00 _cell_volume 3022.9(3) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9957 _cell_measurement_theta_min 2.74 _cell_measurement_theta_max 33.87 _exptl_crystal_description neddle _exptl_crystal_colour translucent _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.397 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1328 _exptl_absorpt_coefficient_mu 0.909 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.85 _exptl_absorpt_correction_T_max 1.0 _exptl_absorpt_process_details ; SADABS Version 2008/1 Bruker-Nonius Blessing, Acta Cryst. (1995) A51 33-38 ; _exptl_special_details ; It should be noted that the esd's of the cell dimensions are probably too low; they should be multiplied by a factor of 2 to 10 ; _diffrn_ambient_temperature 100(2) _diffrn_measurement_specimen_suppport 'magnetic support whith 10 micron nylon fiber cryoloop' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'rotating anode X-ray tube' _diffrn_source_type 'Bruker-Nonius FR 591' _diffrn_source_power 50 _diffrn_source_current 70 _diffrn_source_size '3 mm x 0.3 mm fine focus' _diffrn_radiation_monochromator 'Multilayer Montel 200 mirrors' _diffrn_detector_type '4K CCD area detector APEX II' _diffrn_measurement_device_type 'Kappa 4-axis goniometer bruker-nonius' _diffrn_measurement_method ; Fullsphere data collection, phi and omega scans ; _diffrn_detector_area_resol_mean 512 _diffrn_reflns_number 53896 _diffrn_reflns_av_R_equivalents 0.0454 _diffrn_reflns_av_sigmaI/netI 0.0375 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 2.74 _diffrn_reflns_theta_max 33.96 _reflns_number_total 12184 _reflns_number_gt 9971 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2 v2009.1-0' _computing_cell_refinement 'Bruker APEX2 v2009.1-0' _computing_data_reduction 'Bruker SAINT V7.60A' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXS-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0579P)^2^+6.9388P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12184 _refine_ls_number_parameters 715 _refine_ls_number_restraints 561 _refine_ls_R_factor_all 0.0788 _refine_ls_R_factor_gt 0.0646 _refine_ls_wR_factor_ref 0.1767 _refine_ls_wR_factor_gt 0.1687 _refine_ls_goodness_of_fit_ref 1.156 _refine_ls_restrained_S_all 1.161 _refine_ls_shift/su_max 0.006 _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 0.49950(16) 0.7338(3) 1.07295(13) 0.0157(8) Uani 0.775(2) 1 d PDU A 1 C2 C 0.45406(19) 0.7269(4) 1.12227(14) 0.0192(6) Uani 0.775(2) 1 d PDU A 1 C3 C 0.4602(2) 0.5902(5) 1.16740(15) 0.0240(6) Uani 0.775(2) 1 d PDU A 1 H3 H 0.4303 0.5902 1.2008 0.029 Uiso 0.775(2) 1 calc PR A 1 C4 C 0.5071(2) 0.4580(4) 1.16524(17) 0.0261(7) Uani 0.775(2) 1 d PDU A 1 C5 C 0.5495(2) 0.4618(4) 1.1162(2) 0.0254(7) Uani 0.775(2) 1 d PDU A 1 H5 H 0.5812 0.3693 1.1127 0.031 Uiso 0.775(2) 1 calc PR A 1 C6 C 0.54807(18) 0.5970(4) 1.07085(19) 0.0207(8) Uani 0.775(2) 1 d PDU A 1 C7 C 0.40023(14) 0.8501(3) 1.13085(12) 0.0209(5) Uani 0.775(2) 1 d PDU A 1 H7 H 0.3758 0.8332 1.1675 0.025 Uiso 0.775(2) 1 calc PR A 1 C8 C 0.68294(14) 0.9270(3) 0.88866(12) 0.0355(8) Uani 0.775(2) 1 d PRDU . 1 H8A H 0.6961 0.9733 0.8474 0.043 Uiso 0.775(2) 1 d PR A 1 H8B H 0.7240 0.9455 0.9236 0.043 Uiso 0.775(2) 1 d PR A 1 C9 C 0.5146(3) 0.3138(5) 1.2147(2) 0.0366(9) Uani 0.775(2) 1 d PDU A 1 H9A H 0.5166 0.2048 1.1919 0.055 Uiso 0.775(2) 1 calc PR A 1 H9B H 0.4734 0.3142 1.2387 0.055 Uiso 0.775(2) 1 calc PR A 1 H9C H 0.5588 0.3292 1.2456 0.055 Uiso 0.775(2) 1 calc PR A 1 C10 C 0.59894(18) 0.5835(4) 1.0253(2) 0.0226(8) Uani 0.775(2) 1 d PDU A 1 H10 H 0.6216 0.4759 1.0235 0.027 Uiso 0.775(2) 1 calc PR A 1 C11 C 0.67378(18) 0.6463(4) 0.94802(19) 0.0273(7) Uani 0.775(2) 1 d PDU A 1 H11A H 0.6705 0.5217 0.9410 0.033 Uiso 0.775(2) 1 calc PR A 1 H11B H 0.7213 0.6711 0.9734 0.033 Uiso 0.775(2) 1 calc PR A 1 C12 C 0.6685(2) 0.7360(4) 0.88061(18) 0.0366(8) Uani 0.775(2) 1 d PDU A 1 H12A H 0.7037 0.6849 0.8551 0.044 Uiso 0.775(2) 1 calc PR A 1 H12B H 0.6200 0.7181 0.8560 0.044 Uiso 0.775(2) 1 calc PR A 1 C13 C 0.31016(15) 0.8638(4) 0.92803(16) 0.0143(5) Uani 0.775(2) 1 d PDU A 1 C14 C 0.25882(15) 0.8444(4) 0.86490(17) 0.0153(6) Uani 0.775(2) 1 d PDU A 1 C15 C 0.26594(16) 0.9433(4) 0.81124(18) 0.0185(6) Uani 0.775(2) 1 d PDU A 1 H15 H 0.3054 1.0190 0.8122 0.022 Uiso 0.775(2) 1 calc PR A 1 C16 C 0.21516(16) 0.9320(5) 0.75559(17) 0.0203(6) Uani 0.775(2) 1 d PDU A 1 H16 H 0.2195 1.0025 0.7190 0.024 Uiso 0.775(2) 1 calc PR A 1 C17 C 0.15830(18) 0.8192(5) 0.75289(19) 0.0202(7) Uani 0.775(2) 1 d PDU A 1 H17 H 0.1247 0.8099 0.7141 0.024 Uiso 0.775(2) 1 calc PR A 1 C18 C 0.15044(13) 0.7185(4) 0.80767(17) 0.0168(7) Uani 0.775(2) 1 d PDU A 1 C19 C 0.20166(17) 0.7315(5) 0.86312(18) 0.0169(7) Uani 0.775(2) 1 d PDU A 1 H19 H 0.1976 0.6626 0.9002 0.020 Uiso 0.775(2) 1 calc PR A 1 C20 C 0.00263(14) 0.7074(4) 0.8238(2) 0.0205(7) Uani 0.775(2) 1 d PDU A 1 C21 C 0.01354(17) 0.8656(5) 0.8545(2) 0.0263(9) Uani 0.775(2) 1 d PDU A 1 H21 H 0.0608 0.9089 0.8656 0.032 Uiso 0.775(2) 1 calc PR A 1 C22 C -0.04507(19) 0.9605(6) 0.8691(2) 0.0326(8) Uani 0.775(2) 1 d PDU A 1 H22 H -0.0381 1.0721 0.8867 0.039 Uiso 0.775(2) 1 calc PR A 1 C23 C -0.11373(19) 0.8905(6) 0.8577(3) 0.0354(9) Uani 0.775(2) 1 d PDU A 1 H23 H -0.1534 0.9537 0.8684 0.042 Uiso 0.775(2) 1 calc PR A 1 C24 C -0.12413(16) 0.7314(6) 0.8311(3) 0.0335(9) Uani 0.775(2) 1 d PDU A 1 H24 H -0.1708 0.6828 0.8248 0.040 Uiso 0.775(2) 1 calc PR A 1 C25 C -0.06655(15) 0.6402(5) 0.8133(2) 0.0272(8) Uani 0.775(2) 1 d PDU A 1 H25 H -0.0745 0.5310 0.7938 0.033 Uiso 0.775(2) 1 calc PR A 1 C26 C 0.09408(15) 0.4295(3) 0.86929(18) 0.0190(7) Uani 0.775(2) 1 d PDU A 1 C27 C 0.15304(19) 0.3212(5) 0.8702(2) 0.0260(8) Uani 0.775(2) 1 d PDU A 1 H27 H 0.1823 0.3298 0.8365 0.031 Uiso 0.775(2) 1 calc PR A 1 C28 C 0.1695(2) 0.2024(5) 0.9191(2) 0.0328(10) Uani 0.775(2) 1 d PDU A 1 H28 H 0.2105 0.1319 0.9194 0.039 Uiso 0.775(2) 1 calc PR A 1 C29 C 0.1268(2) 0.1851(5) 0.9680(2) 0.0314(10) Uani 0.775(2) 1 d PDU A 1 H29 H 0.1385 0.1040 1.0020 0.038 Uiso 0.775(2) 1 calc PR A 1 C30 C 0.0667(2) 0.2873(5) 0.9666(2) 0.0306(9) Uani 0.775(2) 1 d PDU A 1 H30 H 0.0364 0.2745 0.9993 0.037 Uiso 0.775(2) 1 calc PR A 1 C31 C 0.05046(19) 0.4084(5) 0.9178(2) 0.0251(7) Uani 0.775(2) 1 d PDU A 1 H31 H 0.0091 0.4777 0.9174 0.030 Uiso 0.775(2) 1 calc PR A 1 N1 N 0.38061(16) 0.9817(4) 1.09491(16) 0.0233(5) Uani 0.775(2) 1 d PDU . 1 N2 N 0.61766(13) 0.6991(3) 0.98670(12) 0.0196(5) Uani 0.775(2) 1 d PDU . 1 O1 O 0.49589(12) 0.8601(3) 1.03044(11) 0.0188(3) Uani 0.775(2) 1 d PDU . 1 O2 O 0.35830(12) 0.9773(3) 0.92804(13) 0.0199(5) Uani 0.775(2) 1 d PDU A 1 O3 O 0.30331(15) 0.7714(4) 0.97601(14) 0.0203(5) Uani 0.775(2) 1 d PDU A 1 P1 P 0.07336(6) 0.57397(16) 0.79859(7) 0.0198(3) Uani 0.775(2) 1 d PDU A 1 Zn1 Zn 0.41945(3) 1.04829(7) 1.00929(3) 0.01499(9) Uani 0.775(2) 1 d PDU . 1 C1' C 0.5054(5) 0.7249(9) 1.0726(4) 0.038(5) Uani 0.225(2) 1 d PDU A 2 C2' C 0.4638(5) 0.7056(10) 1.1245(5) 0.032(4) Uani 0.225(2) 1 d PDU A 2 C3' C 0.4741(6) 0.5615(11) 1.1659(5) 0.035(4) Uani 0.225(2) 1 d PDU A 2 H3'A H 0.4463 0.5522 1.2006 0.041 Uiso 0.225(2) 1 calc PR A 2 C4' C 0.5220(6) 0.4348(10) 1.1583(5) 0.028(3) Uani 0.225(2) 1 d PDU A 2 C5' C 0.5592(6) 0.4480(10) 1.1058(5) 0.027(3) Uani 0.225(2) 1 d PDU A 2 H5'A H 0.5906 0.3582 1.0979 0.032 Uiso 0.225(2) 1 calc PR A 2 C6' C 0.5524(5) 0.5896(9) 1.0631(5) 0.028(4) Uani 0.225(2) 1 d PDU A 2 C7' C 0.4134(6) 0.8272(11) 1.1420(5) 0.053(5) Uani 0.225(2) 1 d PDU A 2 H7'A H 0.3955 0.8067 1.1820 0.064 Uiso 0.225(2) 1 calc PR A 2 C8' C 0.6622(4) 0.9213(5) 0.86419(18) 0.038(3) Uani 0.225(2) 1 d PDU . 2 H8'B H 0.649(3) 0.808(5) 0.845(5) 0.046 Uiso 0.225(2) 1 d PD A 2 H8'C H 0.668(3) 0.993(8) 0.826(2) 0.046 Uiso 0.225(2) 1 d PD A 2 C9' C 0.5340(7) 0.2835(12) 1.2043(5) 0.033(3) Uani 0.225(2) 1 d PDU A 2 H9'A H 0.5032 0.2943 1.2385 0.049 Uiso 0.225(2) 1 calc PR A 2 H9'B H 0.5843 0.2803 1.2244 0.049 Uiso 0.225(2) 1 calc PR A 2 H9'C H 0.5221 0.1781 1.1797 0.049 Uiso 0.225(2) 1 calc PR A 2 C10' C 0.5963(5) 0.5805(9) 1.0117(5) 0.018(3) Uani 0.225(2) 1 d PDU A 2 H10A H 0.6179 0.4733 1.0058 0.022 Uiso 0.225(2) 1 calc PR A 2 C11' C 0.6673(5) 0.6559(8) 0.9338(5) 0.040(4) Uani 0.225(2) 1 d PDU A 2 H11C H 0.6461 0.5985 0.8929 0.048 Uiso 0.225(2) 1 calc PR A 2 H11D H 0.7010 0.5753 0.9590 0.048 Uiso 0.225(2) 1 calc PR A 2 C12' C 0.7090(3) 0.8161(10) 0.9167(4) 0.027(2) Uani 0.225(2) 1 d PDU A 2 H12C H 0.7223 0.8861 0.9564 0.033 Uiso 0.225(2) 1 calc PR A 2 H12E H 0.7537 0.7812 0.9002 0.033 Uiso 0.225(2) 1 calc PR A 2 C13' C 0.3080(4) 0.8637(12) 0.9416(3) 0.022(3) Uani 0.225(2) 1 d PDU A 2 C14' C 0.2588(4) 0.8401(13) 0.8774(3) 0.014(2) Uani 0.225(2) 1 d PDU A 2 C15' C 0.2675(6) 0.9366(17) 0.8235(4) 0.033(4) Uani 0.225(2) 1 d PDU A 2 H15A H 0.3058 1.0161 0.8257 0.040 Uiso 0.225(2) 1 calc PR A 2 C16' C 0.2201(6) 0.918(2) 0.7659(4) 0.050(5) Uani 0.225(2) 1 d PDU A 2 H16A H 0.2285 0.9771 0.7277 0.060 Uiso 0.225(2) 1 calc PR A 2 C17' C 0.1607(5) 0.8127(16) 0.7636(4) 0.025(4) Uani 0.225(2) 1 d PDU A 2 H17A H 0.1255 0.8106 0.7257 0.030 Uiso 0.225(2) 1 calc PR A 2 C18' C 0.1527(3) 0.7094(10) 0.8177(3) 0.028(4) Uani 0.225(2) 1 d PDU A 2 C19' C 0.2012(5) 0.7283(14) 0.8748(4) 0.014(3) Uani 0.225(2) 1 d PDU A 2 H19A H 0.1949 0.6640 0.9125 0.017 Uiso 0.225(2) 1 calc PR A 2 C20' C 0.0054(3) 0.7168(7) 0.8354(5) 0.026(3) Uani 0.225(2) 1 d PDU A 2 C21' C 0.0167(4) 0.8914(9) 0.8462(8) 0.024(3) Uani 0.225(2) 1 d PDU A 2 H21A H 0.0620 0.9402 0.8423 0.029 Uiso 0.225(2) 1 calc PR A 2 C22' C -0.0387(5) 0.9941(12) 0.8628(11) 0.047(5) Uani 0.225(2) 1 d PDU A 2 H22A H -0.0295 1.1091 0.8757 0.057 Uiso 0.225(2) 1 calc PR A 2 C23' C -0.1074(5) 0.9265(14) 0.8603(11) 0.041(4) Uani 0.225(2) 1 d PDU A 2 H23A H -0.1444 0.9918 0.8751 0.049 Uiso 0.225(2) 1 calc PR A 2 C24' C -0.1214(3) 0.7657(16) 0.8364(14) 0.053(5) Uani 0.225(2) 1 d PDU A 2 H24A H -0.1696 0.7272 0.8267 0.063 Uiso 0.225(2) 1 calc PR A 2 C25' C -0.0652(3) 0.6580(12) 0.8262(11) 0.046(5) Uani 0.225(2) 1 d PDU A 2 H25A H -0.0751 0.5436 0.8129 0.055 Uiso 0.225(2) 1 calc PR A 2 C26' C 0.0916(4) 0.4274(10) 0.8792(4) 0.037(5) Uani 0.225(2) 1 d PDU A 2 C27' C 0.1509(6) 0.3195(16) 0.8807(6) 0.043(5) Uani 0.225(2) 1 d PDU A 2 H27A H 0.1798 0.3261 0.8467 0.052 Uiso 0.225(2) 1 calc PR A 2 C28' C 0.1681(6) 0.2040(16) 0.9307(6) 0.034(4) Uani 0.225(2) 1 d PDU A 2 H28A H 0.2100 0.1360 0.9321 0.041 Uiso 0.225(2) 1 calc PR A 2 C29' C 0.1246(6) 0.1864(16) 0.9790(6) 0.034(4) Uani 0.225(2) 1 d PDU A 2 H29A H 0.1334 0.0985 1.0108 0.041 Uiso 0.225(2) 1 calc PR A 2 C30' C 0.0682(6) 0.2988(15) 0.9803(5) 0.027(3) Uani 0.225(2) 1 d PDU A 2 H30A H 0.0396 0.2917 1.0145 0.033 Uiso 0.225(2) 1 calc PR A 2 C31' C 0.0533(6) 0.4216(15) 0.9320(5) 0.031(4) Uani 0.225(2) 1 d PDU A 2 H31A H 0.0165 0.5027 0.9350 0.037 Uiso 0.225(2) 1 calc PR A 2 N1' N 0.3891(4) 0.9618(9) 1.1100(3) 0.037(4) Uani 0.225(2) 1 d PDU . 2 N2' N 0.6098(4) 0.7004(9) 0.9725(4) 0.0196(5) Uani 0.225(2) 1 d PDU . 2 O1' O 0.4986(3) 0.8602(7) 1.0342(3) 0.0188(3) Uani 0.225(2) 1 d PDU . 2 O2' O 0.3539(3) 0.9829(10) 0.9429(3) 0.027(3) Uani 0.225(2) 1 d PDU A 2 O3' O 0.2996(7) 0.7745(15) 0.9900(4) 0.032(3) Uani 0.225(2) 1 d PDU A 2 P1' P 0.0726(2) 0.5740(6) 0.8090(2) 0.0277(13) Uani 0.225(2) 1 d PDU A 2 Zn1' Zn 0.41933(12) 1.0446(3) 1.02274(11) 0.01499(9) Uani 0.225(2) 1 d PDU . 2 O1N O 0.79429(16) 0.2244(4) 0.94100(14) 0.0549(7) Uani 1 1 d . . . H1N H 0.7750 0.2442 0.8987 0.020(8) Uiso 1 1 d RD . . C1N C 0.8539(2) 0.3253(6) 0.9668(2) 0.0554(10) Uani 1 1 d . . . H1N1 H 0.8371 0.4326 0.9835 0.083 Uiso 1 1 calc R . . H1N2 H 0.8831 0.3495 0.9322 0.083 Uiso 1 1 calc R . . H1N3 H 0.8829 0.2636 1.0025 0.083 Uiso 1 1 calc R . . O1M O 0.7441(2) 0.3734(7) 0.8261(2) 0.0844(12) Uani 1 1 d D . . H1M H 0.726(3) 0.434(7) 0.795(2) 0.127 Uiso 1 1 d D . . C1M C 0.7872(3) 0.2932(8) 0.7847(2) 0.0725(15) Uani 1 1 d . . . H1M1 H 0.7709 0.1756 0.7764 0.109 Uiso 1 1 calc R . . H1M2 H 0.8372 0.2931 0.8058 0.109 Uiso 1 1 calc R . . H1M3 H 0.7834 0.3552 0.7431 0.109 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0146(11) 0.0122(11) 0.0185(13) 0.0025(8) -0.0041(8) -0.0018(8) C2 0.0229(13) 0.0164(11) 0.0174(12) 0.0028(9) -0.0003(9) -0.0029(10) C3 0.0298(14) 0.0211(12) 0.0204(12) 0.0045(10) 0.0015(10) -0.0031(12) C4 0.0300(15) 0.0223(13) 0.0248(13) 0.0081(11) 0.0002(11) -0.0005(12) C5 0.0255(14) 0.0194(13) 0.0296(14) 0.0052(11) -0.0021(12) 0.0042(11) C6 0.0205(14) 0.0158(13) 0.0241(13) 0.0036(10) -0.0027(10) 0.0006(10) C7 0.0264(13) 0.0204(12) 0.0171(10) 0.0002(9) 0.0072(10) -0.0039(10) C8 0.0342(15) 0.0345(16) 0.0422(17) -0.0034(13) 0.0205(14) -0.0006(13) C9 0.0421(18) 0.0306(16) 0.0362(16) 0.0143(13) 0.0024(14) 0.0039(14) C10 0.0217(14) 0.0189(14) 0.0248(14) 0.0013(10) -0.0048(11) 0.0021(10) C11 0.0220(13) 0.0244(14) 0.0366(15) -0.0017(11) 0.0080(12) 0.0043(11) C12 0.0344(15) 0.0331(16) 0.0459(17) -0.0083(13) 0.0178(14) -0.0027(13) C13 0.0143(11) 0.0135(11) 0.0157(10) -0.0006(8) 0.0042(8) 0.0018(8) C14 0.0143(11) 0.0168(12) 0.0150(10) -0.0002(9) 0.0030(8) 0.0008(9) C15 0.0167(12) 0.0195(13) 0.0196(11) 0.0040(10) 0.0041(9) -0.0024(9) C16 0.0159(11) 0.0242(13) 0.0207(11) 0.0054(10) 0.0021(9) -0.0016(9) C17 0.0184(13) 0.0258(15) 0.0160(11) 0.0019(10) 0.0011(9) -0.0001(10) C18 0.0154(12) 0.0164(12) 0.0188(10) -0.0011(9) 0.0036(8) 0.0000(9) C19 0.0188(13) 0.0181(13) 0.0147(10) -0.0003(9) 0.0055(9) 0.0000(10) C20 0.0178(13) 0.0250(14) 0.0178(12) -0.0028(10) -0.0005(9) -0.0031(10) C21 0.0218(14) 0.0246(14) 0.0330(17) 0.0004(13) 0.0060(11) -0.0020(11) C22 0.0292(15) 0.0294(15) 0.0410(18) -0.0023(14) 0.0109(13) 0.0033(12) C23 0.0239(14) 0.0420(19) 0.0413(18) 0.0034(16) 0.0085(13) 0.0064(13) C24 0.0178(13) 0.0434(18) 0.0390(18) 0.0038(15) 0.0033(11) -0.0019(12) C25 0.0173(13) 0.0333(16) 0.0297(16) -0.0007(12) -0.0011(10) -0.0044(11) C26 0.0196(13) 0.0145(12) 0.0232(11) -0.0046(9) 0.0043(9) -0.0038(9) C27 0.0291(15) 0.0229(14) 0.0271(13) -0.0047(11) 0.0084(11) 0.0025(11) C28 0.0387(18) 0.0252(16) 0.0355(17) -0.0048(13) 0.0082(14) 0.0098(13) C29 0.0379(18) 0.0226(16) 0.0331(16) 0.0001(12) 0.0035(13) 0.0017(13) C30 0.0335(17) 0.0291(17) 0.0303(16) 0.0012(13) 0.0085(13) -0.0026(13) C31 0.0246(14) 0.0244(14) 0.0271(14) -0.0014(12) 0.0064(11) -0.0003(11) N1 0.0306(13) 0.0182(11) 0.0235(11) 0.0017(9) 0.0116(10) 0.0035(9) N2 0.0153(9) 0.0182(8) 0.0237(12) -0.0019(8) -0.0030(8) 0.0007(7) O1 0.0168(6) 0.0152(6) 0.0238(7) 0.0038(5) 0.0011(5) 0.0000(5) O2 0.0200(10) 0.0216(11) 0.0179(9) -0.0019(8) 0.0026(8) -0.0076(8) O3 0.0210(10) 0.0217(11) 0.0179(9) 0.0033(8) 0.0020(8) -0.0028(8) P1 0.0200(5) 0.0203(5) 0.0192(4) -0.0059(3) 0.0025(3) -0.0040(3) Zn1 0.01688(11) 0.01445(12) 0.0139(2) 0.00158(15) 0.00328(14) -0.00071(9) C1' 0.038(6) 0.037(6) 0.038(6) 0.001(3) 0.004(3) -0.003(3) C2' 0.031(4) 0.030(5) 0.034(5) -0.001(3) 0.000(3) 0.003(3) C3' 0.035(4) 0.034(4) 0.034(4) 0.003(3) 0.002(3) 0.000(3) C4' 0.028(4) 0.025(4) 0.030(4) 0.001(3) -0.001(2) 0.005(3) C5' 0.027(4) 0.024(4) 0.028(4) 0.000(3) 0.000(3) 0.001(3) C6' 0.029(5) 0.023(5) 0.029(5) 0.000(3) -0.004(3) 0.001(3) C7' 0.054(5) 0.051(5) 0.053(5) 0.002(3) 0.004(3) -0.001(3) C8' 0.039(4) 0.040(4) 0.035(4) -0.002(3) 0.002(3) 0.006(3) C9' 0.033(4) 0.031(4) 0.034(4) 0.003(3) 0.004(3) 0.002(3) C10' 0.017(3) 0.016(3) 0.018(3) -0.003(2) -0.007(2) 0.003(2) C11' 0.038(5) 0.039(5) 0.043(5) -0.001(3) 0.001(3) 0.001(3) C12' 0.025(3) 0.025(3) 0.033(3) -0.005(2) 0.006(2) 0.000(2) C13' 0.020(4) 0.022(4) 0.023(4) -0.004(2) 0.002(2) 0.001(2) C14' 0.016(3) 0.014(3) 0.014(3) 0.002(2) 0.003(2) 0.000(2) C15' 0.032(5) 0.034(5) 0.034(5) -0.002(3) 0.003(3) 0.000(3) C16' 0.050(6) 0.050(6) 0.050(6) 0.002(3) 0.009(3) 0.000(3) C17' 0.023(4) 0.027(4) 0.025(4) 0.000(3) 0.000(3) 0.002(3) C18' 0.029(4) 0.027(5) 0.031(5) 0.002(3) 0.008(3) 0.002(3) C19' 0.013(3) 0.015(3) 0.015(3) 0.000(2) 0.001(2) -0.003(2) C20' 0.025(4) 0.028(4) 0.024(4) 0.000(3) 0.002(2) -0.002(3) C21' 0.026(4) 0.022(4) 0.025(4) 0.000(3) 0.003(2) -0.001(2) C22' 0.047(5) 0.046(5) 0.049(5) 0.001(3) 0.008(3) -0.002(3) C23' 0.039(5) 0.040(5) 0.042(5) 0.000(3) 0.005(3) 0.002(3) C24' 0.049(6) 0.055(6) 0.054(6) 0.001(3) 0.007(3) 0.000(3) C25' 0.045(5) 0.045(6) 0.046(6) 0.000(3) 0.002(3) -0.004(3) C26' 0.036(5) 0.034(5) 0.039(5) -0.001(3) 0.002(3) -0.001(3) C27' 0.044(5) 0.044(6) 0.043(6) -0.002(3) 0.009(3) -0.001(3) C28' 0.036(5) 0.030(5) 0.035(5) 0.000(3) 0.004(3) 0.004(3) C29' 0.035(5) 0.032(5) 0.033(5) 0.001(3) 0.005(3) -0.001(3) C30' 0.028(4) 0.027(4) 0.027(4) -0.001(3) 0.006(3) 0.001(3) C31' 0.031(4) 0.031(4) 0.032(4) -0.004(3) 0.007(3) 0.001(3) N1' 0.039(4) 0.037(4) 0.037(4) 0.001(3) 0.007(3) 0.003(3) N2' 0.0153(9) 0.0182(8) 0.0237(12) -0.0019(8) -0.0030(8) 0.0007(7) O1' 0.0168(6) 0.0152(6) 0.0238(7) 0.0038(5) 0.0011(5) 0.0000(5) O2' 0.028(3) 0.027(3) 0.027(3) -0.002(2) 0.004(2) -0.002(2) O3' 0.032(4) 0.031(4) 0.032(4) 0.002(2) 0.006(2) -0.002(2) P1' 0.0264(19) 0.028(2) 0.027(2) -0.0023(14) -0.0011(13) -0.0083(14) Zn1' 0.01688(11) 0.01445(12) 0.0139(2) 0.00158(15) 0.00328(14) -0.00071(9) O1N 0.0572(16) 0.0617(18) 0.0507(15) -0.0132(13) 0.0241(12) -0.0204(14) C1N 0.0468(19) 0.063(3) 0.060(2) -0.0086(19) 0.0208(17) -0.0171(18) O1M 0.069(2) 0.115(4) 0.070(2) 0.006(2) 0.0100(18) 0.002(2) C1M 0.096(4) 0.086(4) 0.0363(18) -0.002(2) 0.014(2) -0.036(3) _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 1.320(3) . ? C1 C6 1.416(4) . ? C1 C2 1.423(4) . ? C2 C3 1.415(4) . ? C2 C7 1.431(4) . ? C3 C4 1.368(6) . ? C4 C5 1.379(6) . ? C4 C9 1.518(4) . ? C5 C6 1.412(4) . ? C6 C10 1.440(5) . ? C7 N1 1.295(4) . ? C8 N1 1.476(4) 3_677 ? C8 C12 1.529(4) . ? C10 N2 1.290(4) . ? C11 N2 1.473(4) . ? C11 C12 1.550(4) . ? C13 O3 1.249(4) . ? C13 O2 1.272(3) . ? C13 C14 1.515(4) . ? C14 C15 1.375(5) . ? C14 C19 1.391(3) . ? C15 C16 1.388(4) . ? C16 C17 1.385(4) . ? C17 C18 1.405(5) . ? C18 C19 1.391(4) . ? C18 P1 1.831(3) . ? C20 C25 1.394(4) . ? C20 C21 1.396(5) . ? C20 P1 1.829(3) . ? C21 C22 1.400(4) . ? C22 C23 1.395(6) . ? C23 C24 1.366(6) . ? C24 C25 1.393(5) . ? C26 C31 1.394(5) . ? C26 C27 1.397(4) . ? C26 P1 1.845(3) . ? C27 C28 1.377(5) . ? C28 C29 1.385(6) . ? C29 C30 1.385(5) . ? C30 C31 1.387(5) . ? N1 C8 1.476(4) 3_677 ? N1 Zn1 2.075(3) . ? N2 Zn1 2.108(3) 3_677 ? O1 Zn1 2.028(2) 3_677 ? O1 Zn1 2.0656(17) . ? O2 Zn1 1.974(2) . ? Zn1 O1 2.028(2) 3_677 ? Zn1 N2 2.108(3) 3_677 ? C1' O1' 1.321(3) . ? C1' C6' 1.414(5) . ? C1' C2' 1.423(4) . ? C2' C3' 1.414(5) . ? C2' C7' 1.430(5) . ? C3' C4' 1.367(6) . ? C4' C5' 1.378(6) . ? C4' C9' 1.517(5) . ? C5' C6' 1.413(4) . ? C6' C10' 1.438(6) . ? C7' N1' 1.294(5) . ? C8' N1' 1.486(8) 3_677 ? C8' C12' 1.537(4) . ? C10' N2' 1.289(5) . ? C11' N2' 1.479(4) . ? C11' C12' 1.550(4) . ? C13' O3' 1.249(5) . ? C13' O2' 1.271(4) . ? C13' C14' 1.516(5) . ? C14' C15' 1.375(5) . ? C14' C19' 1.392(4) . ? C15' C16' 1.388(5) . ? C16' C17' 1.386(4) . ? C17' C18' 1.406(5) . ? C18' C19' 1.391(5) . ? C18' P1' 1.834(3) . ? C20' C25' 1.396(4) . ? C20' C21' 1.400(5) . ? C20' P1' 1.831(4) . ? C21' C22' 1.400(5) . ? C22' C23' 1.395(6) . ? C23' C24' 1.367(7) . ? C24' C25' 1.394(6) . ? C26' C31' 1.393(5) . ? C26' C27' 1.398(5) . ? C26' P1' 1.845(4) . ? C27' C28' 1.377(6) . ? C28' C29' 1.386(6) . ? C29' C30' 1.385(5) . ? C30' C31' 1.387(5) . ? N1' C8' 1.486(8) 3_677 ? N1' Zn1' 2.070(4) . ? N2' Zn1' 2.082(7) 3_677 ? O1' Zn1' 2.070(3) . ? O1' Zn1' 2.204(6) 3_677 ? O2' Zn1' 1.972(3) . ? Zn1' N2' 2.082(7) 3_677 ? Zn1' O1' 2.204(6) 3_677 ? O1N C1N 1.415(5) . ? O1M C1M 1.408(7) . ? 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 C6 121.4(2) . . ? O1 C1 C2 121.7(3) . . ? C6 C1 C2 116.9(3) . . ? C3 C2 C1 120.0(3) . . ? C3 C2 C7 115.0(3) . . ? C1 C2 C7 125.0(3) . . ? C4 C3 C2 123.1(3) . . ? C3 C4 C5 116.9(3) . . ? C3 C4 C9 122.8(4) . . ? C5 C4 C9 120.2(4) . . ? C4 C5 C6 123.0(3) . . ? C5 C6 C1 120.0(3) . . ? C5 C6 C10 115.2(3) . . ? C1 C6 C10 124.8(2) . . ? N1 C7 C2 128.1(2) . . ? N1 C8 C12 111.3(2) 3_677 . ? N2 C10 C6 128.2(3) . . ? N2 C11 C12 113.6(3) . . ? C8 C12 C11 111.1(3) . . ? O3 C13 O2 124.2(3) . . ? O3 C13 C14 119.9(2) . . ? O2 C13 C14 116.0(3) . . ? C15 C14 C19 120.2(3) . . ? C15 C14 C13 120.8(2) . . ? C19 C14 C13 118.9(3) . . ? C14 C15 C16 119.7(2) . . ? C17 C16 C15 120.7(3) . . ? C16 C17 C18 119.9(3) . . ? C19 C18 C17 118.7(2) . . ? C19 C18 P1 125.2(3) . . ? C17 C18 P1 116.1(2) . . ? C18 C19 C14 120.8(3) . . ? C25 C20 C21 118.7(3) . . ? C25 C20 P1 116.3(3) . . ? C21 C20 P1 125.0(2) . . ? C20 C21 C22 120.1(3) . . ? C23 C22 C21 119.7(4) . . ? C24 C23 C22 120.3(3) . . ? C23 C24 C25 120.2(3) . . ? C24 C25 C20 120.7(4) . . ? C31 C26 C27 117.9(3) . . ? C31 C26 P1 124.2(2) . . ? C27 C26 P1 117.5(3) . . ? C28 C27 C26 121.2(4) . . ? C27 C28 C29 120.4(3) . . ? C30 C29 C28 119.2(4) . . ? C29 C30 C31 120.4(4) . . ? C30 C31 C26 120.8(3) . . ? C7 N1 C8 115.5(2) . 3_677 ? C7 N1 Zn1 125.64(19) . . ? C8 N1 Zn1 118.1(2) 3_677 . ? C10 N2 C11 114.7(2) . . ? C10 N2 Zn1 121.0(2) . 3_677 ? C11 N2 Zn1 123.6(2) . 3_677 ? C1 O1 Zn1 124.56(18) . 3_677 ? C1 O1 Zn1 130.22(18) . . ? Zn1 O1 Zn1 103.08(9) 3_677 . ? C13 O2 Zn1 121.8(2) . . ? C20 P1 C18 102.48(13) . . ? C20 P1 C26 101.92(16) . . ? C18 P1 C26 103.01(14) . . ? O2 Zn1 O1 98.83(11) . 3_677 ? O2 Zn1 O1 106.39(10) . . ? O1 Zn1 O1 76.92(9) 3_677 . ? O2 Zn1 N1 114.73(12) . . ? O1 Zn1 N1 145.93(12) 3_677 . ? O1 Zn1 N1 87.74(10) . . ? O2 Zn1 N2 98.18(10) . 3_677 ? O1 Zn1 N2 88.12(9) 3_677 3_677 ? O1 Zn1 N2 152.81(11) . 3_677 ? N1 Zn1 N2 92.51(10) . 3_677 ? O1' C1' C6' 122.0(4) . . ? O1' C1' C2' 121.4(4) . . ? C6' C1' C2' 116.6(3) . . ? C3' C2' C1' 119.8(4) . . ? C3' C2' C7' 114.8(4) . . ? C1' C2' C7' 125.3(4) . . ? C4' C3' C2' 123.2(4) . . ? C3' C4' C5' 117.0(4) . . ? C3' C4' C9' 122.6(5) . . ? C5' C4' C9' 120.3(5) . . ? C4' C5' C6' 122.7(5) . . ? C5' C6' C1' 120.4(4) . . ? C5' C6' C10' 114.3(4) . . ? C1' C6' C10' 125.3(4) . . ? N1' C7' C2' 127.9(4) . . ? N1' C8' C12' 114.6(5) 3_677 . ? N2' C10' C6' 127.8(5) . . ? N2' C11' C12' 111.6(4) . . ? C8' C12' C11' 109.7(4) . . ? O3' C13' O2' 124.1(5) . . ? O3' C13' C14' 119.9(4) . . ? O2' C13' C14' 115.9(4) . . ? C15' C14' C19' 120.0(4) . . ? C15' C14' C13' 120.7(4) . . ? C19' C14' C13' 119.1(4) . . ? C14' C15' C16' 119.8(4) . . ? C17' C16' C15' 120.7(5) . . ? C16' C17' C18' 119.6(4) . . ? C19' C18' C17' 118.6(4) . . ? C19' C18' P1' 125.2(4) . . ? C17' C18' P1' 115.9(3) . . ? C18' C19' C14' 120.9(4) . . ? C25' C20' C21' 117.7(4) . . ? C25' C20' P1' 116.4(4) . . ? C21' C20' P1' 123.4(4) . . ? C20' C21' C22' 120.1(5) . . ? C23' C22' C21' 119.6(5) . . ? C24' C23' C22' 119.7(5) . . ? C23' C24' C25' 120.2(5) . . ? C24' C25' C20' 120.6(5) . . ? C31' C26' C27' 117.7(4) . . ? C31' C26' P1' 124.8(4) . . ? C27' C26' P1' 117.4(4) . . ? C28' C27' C26' 121.1(5) . . ? C27' C28' C29' 120.3(4) . . ? C30' C29' C28' 119.0(5) . . ? C29' C30' C31' 120.4(5) . . ? C30' C31' C26' 120.8(4) . . ? C7' N1' C8' 121.4(4) . 3_677 ? C7' N1' Zn1' 125.4(3) . . ? C8' N1' Zn1' 113.1(3) 3_677 . ? C10' N2' C11' 113.2(4) . . ? C10' N2' Zn1' 126.5(4) . 3_677 ? C11' N2' Zn1' 118.1(4) . 3_677 ? C1' O1' Zn1' 129.6(3) . . ? C1' O1' Zn1' 125.3(3) . 3_677 ? Zn1' O1' Zn1' 104.6(2) . 3_677 ? C13' O2' Zn1' 122.6(4) . . ? C20' P1' C18' 102.2(3) . . ? C20' P1' C26' 102.3(3) . . ? C18' P1' C26' 102.7(3) . . ? O2' Zn1' O1' 106.2(2) . . ? O2' Zn1' N1' 115.7(3) . . ? O1' Zn1' N1' 88.00(18) . . ? O2' Zn1' N2' 98.0(4) . 3_677 ? O1' Zn1' N2' 149.1(4) . 3_677 ? N1' Zn1' N2' 98.8(3) . 3_677 ? O2' Zn1' O1' 92.3(3) . 3_677 ? O1' Zn1' O1' 75.4(2) . 3_677 ? N1' Zn1' O1' 150.8(3) . 3_677 ? N2' Zn1' O1' 84.8(2) 3_677 3_677 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 C1 C2 C3 -179.3(3) . . . . ? C6 C1 C2 C3 1.8(5) . . . . ? O1 C1 C2 C7 1.0(5) . . . . ? C6 C1 C2 C7 -178.0(3) . . . . ? C1 C2 C3 C4 -2.0(5) . . . . ? C7 C2 C3 C4 177.8(3) . . . . ? C2 C3 C4 C5 -0.1(6) . . . . ? C2 C3 C4 C9 178.6(4) . . . . ? C3 C4 C5 C6 2.3(6) . . . . ? C9 C4 C5 C6 -176.3(4) . . . . ? C4 C5 C6 C1 -2.5(6) . . . . ? C4 C5 C6 C10 176.7(4) . . . . ? O1 C1 C6 C5 -178.6(3) . . . . ? C2 C1 C6 C5 0.3(5) . . . . ? O1 C1 C6 C10 2.2(5) . . . . ? C2 C1 C6 C10 -178.8(3) . . . . ? C3 C2 C7 N1 -176.0(3) . . . . ? C1 C2 C7 N1 3.8(5) . . . . ? C5 C6 C10 N2 -167.3(4) . . . . ? C1 C6 C10 N2 11.9(7) . . . . ? N1 C8 C12 C11 -78.9(4) 3_677 . . . ? N2 C11 C12 C8 66.0(4) . . . . ? O3 C13 C14 C15 -179.2(4) . . . . ? O2 C13 C14 C15 1.1(5) . . . . ? O3 C13 C14 C19 4.5(5) . . . . ? O2 C13 C14 C19 -175.2(3) . . . . ? C19 C14 C15 C16 1.0(6) . . . . ? C13 C14 C15 C16 -175.3(3) . . . . ? C14 C15 C16 C17 -1.6(6) . . . . ? C15 C16 C17 C18 2.0(6) . . . . ? C16 C17 C18 C19 -1.8(6) . . . . ? C16 C17 C18 P1 180.0(3) . . . . ? C17 C18 C19 C14 1.3(5) . . . . ? P1 C18 C19 C14 179.3(3) . . . . ? C15 C14 C19 C18 -0.9(6) . . . . ? C13 C14 C19 C18 175.5(3) . . . . ? C25 C20 C21 C22 -5.5(7) . . . . ? P1 C20 C21 C22 177.1(4) . . . . ? C20 C21 C22 C23 5.2(8) . . . . ? C21 C22 C23 C24 -1.3(8) . . . . ? C22 C23 C24 C25 -2.1(8) . . . . ? C23 C24 C25 C20 1.8(8) . . . . ? C21 C20 C25 C24 2.0(7) . . . . ? P1 C20 C25 C24 179.7(4) . . . . ? C31 C26 C27 C28 -2.9(6) . . . . ? P1 C26 C27 C28 -176.0(3) . . . . ? C26 C27 C28 C29 1.5(7) . . . . ? C27 C28 C29 C30 0.8(7) . . . . ? C28 C29 C30 C31 -1.5(7) . . . . ? C29 C30 C31 C26 0.0(7) . . . . ? C27 C26 C31 C30 2.1(6) . . . . ? P1 C26 C31 C30 174.8(3) . . . . ? C2 C7 N1 C8 172.4(3) . . . 3_677 ? C2 C7 N1 Zn1 3.1(5) . . . . ? C6 C10 N2 C11 177.5(4) . . . . ? C6 C10 N2 Zn1 6.0(5) . . . 3_677 ? C12 C11 N2 C10 149.7(3) . . . . ? C12 C11 N2 Zn1 -39.1(4) . . . 3_677 ? C6 C1 O1 Zn1 -33.0(4) . . . 3_677 ? C2 C1 O1 Zn1 148.0(2) . . . 3_677 ? C6 C1 O1 Zn1 166.5(3) . . . . ? C2 C1 O1 Zn1 -12.4(4) . . . . ? O3 C13 O2 Zn1 -10.2(5) . . . . ? C14 C13 O2 Zn1 169.5(2) . . . . ? C25 C20 P1 C18 171.0(3) . . . . ? C21 C20 P1 C18 -11.5(4) . . . . ? C25 C20 P1 C26 -82.5(3) . . . . ? C21 C20 P1 C26 94.9(4) . . . . ? C19 C18 P1 C20 93.4(3) . . . . ? C17 C18 P1 C20 -88.5(3) . . . . ? C19 C18 P1 C26 -12.2(3) . . . . ? C17 C18 P1 C26 165.9(3) . . . . ? C31 C26 P1 C20 15.0(3) . . . . ? C27 C26 P1 C20 -172.4(3) . . . . ? C31 C26 P1 C18 121.0(3) . . . . ? C27 C26 P1 C18 -66.4(3) . . . . ? C13 O2 Zn1 O1 156.5(3) . . . 3_677 ? C13 O2 Zn1 O1 77.7(3) . . . . ? C13 O2 Zn1 N1 -17.5(3) . . . . ? C13 O2 Zn1 N2 -114.1(3) . . . 3_677 ? C1 O1 Zn1 O2 -100.9(3) . . . . ? Zn1 O1 Zn1 O2 95.51(13) 3_677 . . . ? C1 O1 Zn1 O1 163.6(4) . . . 3_677 ? Zn1 O1 Zn1 O1 -0.001(1) 3_677 . . 3_677 ? C1 O1 Zn1 N1 14.2(3) . . . . ? Zn1 O1 Zn1 N1 -149.35(13) 3_677 . . . ? C1 O1 Zn1 N2 105.3(3) . . . 3_677 ? Zn1 O1 Zn1 N2 -58.3(2) 3_677 . . 3_677 ? C7 N1 Zn1 O2 97.9(3) . . . . ? C8 N1 Zn1 O2 -71.2(2) 3_677 . . . ? C7 N1 Zn1 O1 -71.5(3) . . . 3_677 ? C8 N1 Zn1 O1 119.4(2) 3_677 . . 3_677 ? C7 N1 Zn1 O1 -9.1(3) . . . . ? C8 N1 Zn1 O1 -178.2(2) 3_677 . . . ? C7 N1 Zn1 N2 -161.9(3) . . . 3_677 ? C8 N1 Zn1 N2 29.0(2) 3_677 . . 3_677 ? O1' C1' C2' C3' -178.1(12) . . . . ? C6' C1' C2' C3' 3.9(19) . . . . ? O1' C1' C2' C7' -2(2) . . . . ? C6' C1' C2' C7' -179.9(13) . . . . ? C1' C2' C3' C4' -1(2) . . . . ? C7' C2' C3' C4' -177.6(14) . . . . ? C2' C3' C4' C5' -3(2) . . . . ? C2' C3' C4' C9' 178.1(13) . . . . ? C3' C4' C5' C6' 4(2) . . . . ? C9' C4' C5' C6' -177.2(13) . . . . ? C4' C5' C6' C1' -1(2) . . . . ? C4' C5' C6' C10' 179.3(13) . . . . ? O1' C1' C6' C5' 179.0(12) . . . . ? C2' C1' C6' C5' -3.0(19) . . . . ? O1' C1' C6' C10' -1(2) . . . . ? C2' C1' C6' C10' 176.8(12) . . . . ? C3' C2' C7' N1' -173.4(14) . . . . ? C1' C2' C7' N1' 10(2) . . . . ? C5' C6' C10' N2' -168.1(13) . . . . ? C1' C6' C10' N2' 12(2) . . . . ? N1' C8' C12' C11' 83.4(7) 3_677 . . . ? N2' C11' C12' C8' -72.6(9) . . . . ? O3' C13' C14' C15' -179.7(15) . . . . ? O2' C13' C14' C15' 3.8(18) . . . . ? O3' C13' C14' C19' 5.1(19) . . . . ? O2' C13' C14' C19' -171.3(12) . . . . ? C19' C14' C15' C16' -2(2) . . . . ? C13' C14' C15' C16' -177.5(14) . . . . ? C14' C15' C16' C17' 5(3) . . . . ? C15' C16' C17' C18' -7(3) . . . . ? C16' C17' C18' C19' 6(2) . . . . ? C16' C17' C18' P1' -179.3(13) . . . . ? C17' C18' C19' C14' -3.6(19) . . . . ? P1' C18' C19' C14' -177.2(9) . . . . ? C15' C14' C19' C18' 2(2) . . . . ? C13' C14' C19' C18' 176.7(11) . . . . ? C25' C20' C21' C22' 15(2) . . . . ? P1' C20' C21' C22' 176.4(13) . . . . ? C20' C21' C22' C23' -8(3) . . . . ? C21' C22' C23' C24' -6(3) . . . . ? C22' C23' C24' C25' 12(4) . . . . ? C23' C24' C25' C20' -5(4) . . . . ? C21' C20' C25' C24' -9(3) . . . . ? P1' C20' C25' C24' -171.3(18) . . . . ? C31' C26' C27' C28' 4(2) . . . . ? P1' C26' C27' C28' -178.8(13) . . . . ? C26' C27' C28' C29' 3(3) . . . . ? C27' C28' C29' C30' -7(3) . . . . ? C28' C29' C30' C31' 3(3) . . . . ? C29' C30' C31' C26' 4(2) . . . . ? C27' C26' C31' C30' -8(2) . . . . ? P1' C26' C31' C30' 175.4(11) . . . . ? C2' C7' N1' C8' -178.4(12) . . . 3_677 ? C2' C7' N1' Zn1' -2(2) . . . . ? C6' C10' N2' C11' 169.4(12) . . . . ? C6' C10' N2' Zn1' 6.8(19) . . . 3_677 ? C12' C11' N2' C10' -150.3(10) . . . . ? C12' C11' N2' Zn1' 13.9(10) . . . 3_677 ? C6' C1' O1' Zn1' 163.9(9) . . . . ? C2' C1' O1' Zn1' -14.0(17) . . . . ? C6' C1' O1' Zn1' -25.1(16) . . . 3_677 ? C2' C1' O1' Zn1' 157.0(9) . . . 3_677 ? O3' C13' O2' Zn1' 0.0(19) . . . . ? C14' C13' O2' Zn1' 176.3(8) . . . . ? C25' C20' P1' C18' 171.8(11) . . . . ? C21' C20' P1' C18' 10.1(11) . . . . ? C25' C20' P1' C26' -82.1(12) . . . . ? C21' C20' P1' C26' 116.2(11) . . . . ? C19' C18' P1' C20' 87.1(10) . . . . ? C17' C18' P1' C20' -86.6(10) . . . . ? C19' C18' P1' C26' -18.7(10) . . . . ? C17' C18' P1' C26' 167.5(9) . . . . ? C31' C26' P1' C20' 8.6(11) . . . . ? C27' C26' P1' C20' -168.4(10) . . . . ? C31' C26' P1' C18' 114.3(11) . . . . ? C27' C26' P1' C18' -62.8(11) . . . . ? C13' O2' Zn1' O1' 76.8(10) . . . . ? C13' O2' Zn1' N1' -18.9(10) . . . . ? C13' O2' Zn1' N2' -122.7(9) . . . 3_677 ? C13' O2' Zn1' O1' 152.2(9) . . . 3_677 ? C1' O1' Zn1' O2' -99.5(9) . . . . ? Zn1' O1' Zn1' O2' 88.1(4) 3_677 . . . ? C1' O1' Zn1' N1' 16.7(10) . . . . ? Zn1' O1' Zn1' N1' -155.7(4) 3_677 . . . ? C1' O1' Zn1' N2' 120.6(9) . . . 3_677 ? Zn1' O1' Zn1' N2' -51.8(6) 3_677 . . 3_677 ? C1' O1' Zn1' O1' 172.4(12) . . . 3_677 ? Zn1' O1' Zn1' O1' 0.002(1) 3_677 . . 3_677 ? C7' N1' Zn1' O2' 98.4(11) . . . . ? C8' N1' Zn1' O2' -84.5(7) 3_677 . . . ? C7' N1' Zn1' O1' -8.5(11) . . . . ? C8' N1' Zn1' O1' 168.5(7) 3_677 . . . ? C7' N1' Zn1' N2' -158.2(11) . . . 3_677 ? C8' N1' Zn1' N2' 18.8(7) 3_677 . . 3_677 ? C7' N1' Zn1' O1' -63.1(14) . . . 3_677 ? C8' N1' Zn1' O1' 113.9(6) 3_677 . . 3_677 ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 33.96 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 2.782 _refine_diff_density_min -0.777 _refine_diff_density_rms 0.113 # Attachment '- 9Dprime-sp125p21cX.cif' data_sp125p21c _database_code_depnum_ccdc_archive 'CCDC 825587' #TrackingRef '- 9Dprime-sp125p21cX.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C60 H54 N4 O6 P2 Zn2' _chemical_formula_weight 1119.75 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' P P 0.1023 0.0942 '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 P2(1)/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 8.4567(3) _cell_length_b 34.8441(9) _cell_length_c 8.4433(2) _cell_angle_alpha 90.00 _cell_angle_beta 97.9190(10) _cell_angle_gamma 90.00 _cell_volume 2464.23(12) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 7765 _cell_measurement_theta_min 2.70 _cell_measurement_theta_max 39.46 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.509 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1160 _exptl_absorpt_coefficient_mu 1.099 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.95 _exptl_absorpt_correction_T_max 1.0 _exptl_absorpt_process_details ; SADABS Version 2008/1 Bruker-Nonius Blessing, Acta Cryst. (1995) A51 33-38 ; _exptl_special_details ; It should be noted that the esd's of the cell dimensions are probably too low; they should be multiplied by a factor of 2 to 10 ; _diffrn_ambient_temperature 100(2) _diffrn_measurement_specimen_suppport 'magnetic support whith 10 micron nylon fiber cryoloop' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'rotating anode X-ray tube' _diffrn_source_type 'Bruker-Nonius FR 591' _diffrn_source_power 50 _diffrn_source_current 70 _diffrn_source_size '3 mm x 0.3 mm fine focus' _diffrn_radiation_monochromator 'Multilayer Montel 200 mirrors' _diffrn_detector_type '4K CCD area detector APEX II' _diffrn_measurement_device_type 'Kappa 4-axis goniometer bruker-nonius' _diffrn_measurement_method ; Fullsphere data collection, phi and omega scans ; _diffrn_detector_area_resol_mean 512 _diffrn_reflns_number 60636 _diffrn_reflns_av_R_equivalents 0.0321 _diffrn_reflns_av_sigmaI/netI 0.0259 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -61 _diffrn_reflns_limit_k_max 63 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.00 _diffrn_reflns_theta_max 40.02 _reflns_number_total 14185 _reflns_number_gt 12913 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2 v2009.1-0' _computing_cell_refinement 'Bruker APEX2 v2009.1-0' _computing_data_reduction 'Bruker SAINT V7.60A' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXS-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0381P)^2^+1.4061P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 14185 _refine_ls_number_parameters 335 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0413 _refine_ls_R_factor_gt 0.0371 _refine_ls_wR_factor_ref 0.0967 _refine_ls_wR_factor_gt 0.0947 _refine_ls_goodness_of_fit_ref 1.115 _refine_ls_restrained_S_all 1.115 _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 0.20427(15) 0.09087(3) 0.71949(13) 0.02093(18) Uani 1 1 d . . . H19A H 0.2728 0.1036 0.6491 0.025 Uiso 1 1 calc R . . H19B H 0.1304 0.1104 0.7527 0.025 Uiso 1 1 calc R . . C2 C 0.10780(14) 0.05948(3) 0.62614(13) 0.02000(17) Uani 1 1 d . . . H20A H 0.0224 0.0715 0.5501 0.024 Uiso 1 1 calc R . . H20B H 0.0560 0.0435 0.7013 0.024 Uiso 1 1 calc R . . C3 C 0.20789(14) 0.03376(3) 0.53394(12) 0.01859(17) Uani 1 1 d . . . H21A H 0.1359 0.0181 0.4570 0.022 Uiso 1 1 calc R . . H21B H 0.2734 0.0500 0.4720 0.022 Uiso 1 1 calc R . . C4 C 0.32619(13) -0.02605(3) 0.58240(11) 0.01532(14) Uani 1 1 d . . . H22 H 0.2645 -0.0311 0.4817 0.018 Uiso 1 1 calc R . . C5 C 0.42207(12) -0.05780(3) 0.65347(11) 0.01383(13) Uani 1 1 d . . . C6 C 0.42393(13) -0.09003(3) 0.55403(11) 0.01571(15) Uani 1 1 d . . . H24 H 0.3624 -0.0894 0.4511 0.019 Uiso 1 1 calc R . . C7 C 0.51168(13) -0.12282(3) 0.59945(12) 0.01596(15) Uani 1 1 d . . . C8 C 0.59918(13) -0.12257(3) 0.75174(12) 0.01546(14) Uani 1 1 d . . . H26 H 0.6631 -0.1443 0.7853 0.019 Uiso 1 1 calc R . . C9 C 0.59702(12) -0.09165(3) 0.85775(11) 0.01345(13) Uani 1 1 d . . . C10 C 0.69014(12) -0.09743(3) 1.01336(11) 0.01522(14) Uani 1 1 d . . . H30 H 0.7555 -0.1197 1.0247 0.018 Uiso 1 1 calc R . . C11 C 0.51153(16) -0.15712(3) 0.49057(14) 0.02223(19) Uani 1 1 d . . . H29A H 0.6218 -0.1649 0.4838 0.033 Uiso 1 1 calc R . . H29B H 0.4582 -0.1504 0.3837 0.033 Uiso 1 1 calc R . . H29C H 0.4546 -0.1784 0.5335 0.033 Uiso 1 1 calc R . . C12 C 0.50860(11) -0.05780(2) 0.81040(10) 0.01221(13) Uani 1 1 d . . . C13 C 0.75533(12) 0.06139(3) 0.89874(11) 0.01332(13) Uani 1 1 d . . . C14 C 0.78184(12) 0.10111(3) 0.91796(11) 0.01407(13) Uani 1 1 d . . . H2 H 0.7234 0.1184 0.8451 0.017 Uiso 1 1 calc R . . C15 C 0.89207(12) 0.11560(3) 1.04173(11) 0.01400(13) Uani 1 1 d . . . C16 C 0.98153(13) 0.09054(3) 1.14840(12) 0.01665(15) Uani 1 1 d . . . H4 H 1.0560 0.1002 1.2336 0.020 Uiso 1 1 calc R . . C17 C 0.95949(14) 0.05117(3) 1.12753(13) 0.01879(16) Uani 1 1 d . . . H5 H 1.0214 0.0339 1.1979 0.023 Uiso 1 1 calc R . . C18 C 0.84881(13) 0.03666(3) 1.00586(12) 0.01669(15) Uani 1 1 d . . . H6 H 0.8358 0.0097 0.9945 0.020 Uiso 1 1 calc R . . C19 C 0.75463(12) 0.19069(3) 0.96941(11) 0.01446(14) Uani 1 1 d . . . C20 C 0.76869(14) 0.22210(3) 0.87001(14) 0.02028(17) Uani 1 1 d . . . H14 H 0.8709 0.2300 0.8480 0.024 Uiso 1 1 calc R . . C21 C 0.63236(17) 0.24188(4) 0.80302(16) 0.0261(2) Uani 1 1 d . . . H15 H 0.6416 0.2632 0.7349 0.031 Uiso 1 1 calc R . . C22 C 0.48318(16) 0.23040(4) 0.83582(15) 0.0242(2) Uani 1 1 d . . . H16 H 0.3906 0.2439 0.7894 0.029 Uiso 1 1 calc R . . C23 C 0.46787(14) 0.19933(3) 0.93615(15) 0.02117(18) Uani 1 1 d . . . H17 H 0.3655 0.1917 0.9588 0.025 Uiso 1 1 calc R . . C24 C 0.60376(13) 0.17958(3) 1.00294(13) 0.01777(16) Uani 1 1 d . . . H18 H 0.5941 0.1584 1.0718 0.021 Uiso 1 1 calc R . . C25 C 0.97329(12) 0.17813(3) 1.26218(11) 0.01530(14) Uani 1 1 d . . . C26 C 0.89249(15) 0.16116(4) 1.37772(13) 0.02155(18) Uani 1 1 d . . . H8 H 0.8103 0.1430 1.3469 0.026 Uiso 1 1 calc R . . C27 C 0.93268(17) 0.17099(4) 1.53854(14) 0.0249(2) Uani 1 1 d . . . H9 H 0.8787 0.1592 1.6172 0.030 Uiso 1 1 calc R . . C28 C 1.05104(16) 0.19787(4) 1.58395(14) 0.0243(2) Uani 1 1 d . . . H10 H 1.0791 0.2042 1.6937 0.029 Uiso 1 1 calc R . . C29 C 1.12875(16) 0.21558(4) 1.46878(14) 0.0238(2) Uani 1 1 d . . . H11 H 1.2076 0.2346 1.4995 0.029 Uiso 1 1 calc R . . C30 C 1.09121(14) 0.20550(3) 1.30862(13) 0.01884(16) Uani 1 1 d . . . H12 H 1.1460 0.2173 1.2305 0.023 Uiso 1 1 calc R . . N1 N 0.30525(11) 0.07596(2) 0.86220(10) 0.01585(13) Uani 1 1 d . . . N2 N 0.31411(11) 0.00794(2) 0.63827(10) 0.01470(13) Uani 1 1 d . . . O1 O 0.50819(10) -0.028298(19) 0.90602(8) 0.01369(11) Uani 1 1 d . . . O2 O 0.64744(10) 0.04809(2) 0.78384(8) 0.01540(12) Uani 1 1 d . . . O3 O 1.07614(9) 0.17820(2) 0.96790(9) 0.01669(12) Uani 1 1 d . . . P1 P 0.93552(3) 0.166129(7) 1.05221(3) 0.01295(4) Uani 1 1 d . . . Zn1 Zn 0.449510(14) 0.027960(3) 0.844736(13) 0.01198(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0274(5) 0.0174(4) 0.0159(4) 0.0012(3) -0.0043(3) 0.0072(3) C2 0.0169(4) 0.0235(4) 0.0180(4) 0.0025(3) -0.0034(3) 0.0039(3) C3 0.0235(5) 0.0169(4) 0.0132(3) 0.0014(3) -0.0051(3) 0.0030(3) C4 0.0181(4) 0.0153(3) 0.0116(3) -0.0012(2) -0.0016(3) -0.0005(3) C5 0.0167(4) 0.0125(3) 0.0119(3) -0.0010(2) 0.0003(3) -0.0006(3) C6 0.0194(4) 0.0145(3) 0.0127(3) -0.0024(2) 0.0005(3) -0.0009(3) C7 0.0191(4) 0.0138(3) 0.0150(3) -0.0027(3) 0.0024(3) -0.0009(3) C8 0.0169(4) 0.0139(3) 0.0157(3) -0.0015(3) 0.0026(3) 0.0007(3) C9 0.0147(3) 0.0126(3) 0.0129(3) -0.0002(2) 0.0012(3) 0.0005(3) C10 0.0164(4) 0.0143(3) 0.0146(3) 0.0003(3) 0.0009(3) 0.0026(3) C11 0.0284(5) 0.0171(4) 0.0206(4) -0.0064(3) 0.0014(4) 0.0018(4) C12 0.0141(3) 0.0112(3) 0.0112(3) -0.0003(2) 0.0011(3) -0.0009(2) C13 0.0144(3) 0.0132(3) 0.0122(3) -0.0002(2) 0.0013(3) -0.0010(3) C14 0.0157(4) 0.0125(3) 0.0132(3) 0.0006(2) -0.0009(3) -0.0002(3) C15 0.0147(3) 0.0128(3) 0.0138(3) 0.0005(2) -0.0004(3) -0.0013(3) C16 0.0163(4) 0.0156(3) 0.0166(4) 0.0020(3) -0.0031(3) -0.0012(3) C17 0.0195(4) 0.0151(3) 0.0197(4) 0.0034(3) -0.0043(3) 0.0008(3) C18 0.0188(4) 0.0121(3) 0.0181(4) 0.0012(3) -0.0014(3) 0.0007(3) C19 0.0155(4) 0.0123(3) 0.0152(3) 0.0003(2) 0.0006(3) -0.0007(3) C20 0.0208(4) 0.0177(4) 0.0222(4) 0.0058(3) 0.0023(3) 0.0000(3) C21 0.0276(6) 0.0218(5) 0.0285(5) 0.0100(4) 0.0019(4) 0.0044(4) C22 0.0233(5) 0.0227(4) 0.0254(5) 0.0019(4) -0.0014(4) 0.0068(4) C23 0.0168(4) 0.0200(4) 0.0262(5) -0.0025(3) 0.0012(4) 0.0015(3) C24 0.0160(4) 0.0152(3) 0.0221(4) 0.0009(3) 0.0025(3) -0.0002(3) C25 0.0158(4) 0.0156(3) 0.0142(3) -0.0009(3) 0.0007(3) -0.0012(3) C26 0.0225(5) 0.0262(5) 0.0165(4) -0.0014(3) 0.0047(3) -0.0056(4) C27 0.0271(6) 0.0313(5) 0.0170(4) -0.0008(4) 0.0054(4) -0.0013(4) C28 0.0250(5) 0.0305(5) 0.0167(4) -0.0047(4) 0.0005(4) 0.0019(4) C29 0.0239(5) 0.0269(5) 0.0194(4) -0.0065(4) -0.0011(4) -0.0042(4) C30 0.0198(4) 0.0185(4) 0.0175(4) -0.0024(3) 0.0000(3) -0.0041(3) N1 0.0179(3) 0.0156(3) 0.0131(3) 0.0005(2) -0.0012(3) 0.0032(3) N2 0.0173(3) 0.0134(3) 0.0121(3) 0.0004(2) -0.0025(2) 0.0001(2) O1 0.0186(3) 0.0110(2) 0.0107(2) -0.00103(18) -0.0006(2) 0.0003(2) O2 0.0175(3) 0.0163(3) 0.0118(2) -0.0009(2) -0.0001(2) -0.0037(2) O3 0.0126(3) 0.0196(3) 0.0177(3) -0.0026(2) 0.0013(2) 0.0019(2) P1 0.01356(10) 0.01210(9) 0.01283(9) 0.00025(7) 0.00055(7) -0.00180(7) Zn1 0.01399(5) 0.01098(4) 0.01010(4) 0.00046(3) -0.00141(3) 0.00003(3) _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 N1 1.4722(13) . ? C1 C2 1.5185(17) . ? C2 C3 1.5189(16) . ? C3 N2 1.4745(13) . ? C4 N2 1.2840(12) . ? C4 C5 1.4515(14) . ? C5 C6 1.4036(13) . ? C5 C12 1.4227(13) . ? C6 C7 1.3873(14) . ? C7 C8 1.3925(14) . ? C7 C11 1.5078(14) . ? C8 C9 1.4025(13) . ? C9 C12 1.4238(13) . ? C9 C10 1.4498(13) . ? C10 N1 1.2859(13) 3_657 ? C12 O1 1.3075(11) . ? C13 O2 1.3208(12) . ? C13 C14 1.4076(13) . ? C13 C18 1.4101(14) . ? C14 C15 1.3956(13) . ? C15 C16 1.3992(14) . ? C15 P1 1.7984(9) . ? C16 C17 1.3924(14) . ? C17 C18 1.3864(15) . ? C19 C20 1.3941(14) . ? C19 C24 1.3990(15) . ? C19 P1 1.8074(10) . ? C20 C21 1.3944(17) . ? C21 C22 1.387(2) . ? C22 C23 1.3917(18) . ? C23 C24 1.3905(16) . ? C25 C30 1.3963(14) . ? C25 C26 1.3971(15) . ? C25 P1 1.8066(10) . ? C26 C27 1.3962(16) . ? C27 C28 1.3859(19) . ? C28 C29 1.3907(19) . ? C29 C30 1.3909(15) . ? N1 C10 1.2859(13) 3_657 ? N1 Zn1 2.0875(9) . ? N2 Zn1 2.0705(8) . ? O1 Zn1 2.0703(7) . ? O1 Zn1 2.0855(7) 3_657 ? O2 Zn1 1.9481(8) . ? O3 P1 1.5267(8) . ? Zn1 O1 2.0855(7) 3_657 ? 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 C1 C2 112.36(9) . . ? C1 C2 C3 113.17(10) . . ? N2 C3 C2 112.98(8) . . ? N2 C4 C5 128.25(9) . . ? C6 C5 C12 120.68(9) . . ? C6 C5 C4 114.47(8) . . ? C12 C5 C4 124.85(8) . . ? C7 C6 C5 122.91(9) . . ? C6 C7 C8 116.49(8) . . ? C6 C7 C11 121.93(9) . . ? C8 C7 C11 121.58(9) . . ? C7 C8 C9 122.83(9) . . ? C8 C9 C12 120.64(8) . . ? C8 C9 C10 114.73(8) . . ? C12 C9 C10 124.63(8) . . ? N1 C10 C9 127.68(9) 3_657 . ? O1 C12 C5 122.02(8) . . ? O1 C12 C9 121.59(8) . . ? C5 C12 C9 116.39(8) . . ? O2 C13 C14 120.83(8) . . ? O2 C13 C18 121.75(8) . . ? C14 C13 C18 117.42(9) . . ? C15 C14 C13 121.42(8) . . ? C14 C15 C16 120.16(8) . . ? C14 C15 P1 120.13(7) . . ? C16 C15 P1 119.37(7) . . ? C17 C16 C15 118.83(9) . . ? C18 C17 C16 121.20(9) . . ? C17 C18 C13 120.94(9) . . ? C20 C19 C24 119.66(10) . . ? C20 C19 P1 117.82(8) . . ? C24 C19 P1 122.52(7) . . ? C19 C20 C21 119.85(11) . . ? C22 C21 C20 120.03(11) . . ? C21 C22 C23 120.61(11) . . ? C24 C23 C22 119.40(11) . . ? C23 C24 C19 120.45(10) . . ? C30 C25 C26 119.47(9) . . ? C30 C25 P1 117.16(8) . . ? C26 C25 P1 123.36(8) . . ? C27 C26 C25 119.89(11) . . ? C28 C27 C26 120.30(11) . . ? C27 C28 C29 119.96(11) . . ? C28 C29 C30 120.07(11) . . ? C29 C30 C25 120.27(10) . . ? C10 N1 C1 114.37(8) 3_657 . ? C10 N1 Zn1 124.85(7) 3_657 . ? C1 N1 Zn1 120.24(7) . . ? C4 N2 C3 114.58(8) . . ? C4 N2 Zn1 123.87(7) . . ? C3 N2 Zn1 121.20(6) . . ? C12 O1 Zn1 127.67(6) . . ? C12 O1 Zn1 127.80(6) . 3_657 ? Zn1 O1 Zn1 104.41(3) . 3_657 ? C13 O2 Zn1 117.65(6) . . ? O3 P1 C15 114.45(5) . . ? O3 P1 C25 110.49(5) . . ? C15 P1 C25 106.39(4) . . ? O3 P1 C19 111.18(4) . . ? C15 P1 C19 106.75(5) . . ? C25 P1 C19 107.20(5) . . ? O2 Zn1 O1 102.81(3) . . ? O2 Zn1 N2 107.14(3) . . ? O1 Zn1 N2 88.69(3) . . ? O2 Zn1 O1 103.31(3) . 3_657 ? O1 Zn1 O1 75.60(3) . 3_657 ? N2 Zn1 O1 148.16(3) . 3_657 ? O2 Zn1 N1 105.18(3) . . ? O1 Zn1 N1 149.70(3) . . ? N2 Zn1 N1 93.94(3) . . ? O1 Zn1 N1 86.84(3) 3_657 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 C3 -73.63(12) . . . . ? C1 C2 C3 N2 71.84(12) . . . . ? N2 C4 C5 C6 -172.93(11) . . . . ? N2 C4 C5 C12 7.35(17) . . . . ? C12 C5 C6 C7 -1.80(16) . . . . ? C4 C5 C6 C7 178.47(10) . . . . ? C5 C6 C7 C8 0.41(16) . . . . ? C5 C6 C7 C11 179.89(10) . . . . ? C6 C7 C8 C9 1.87(15) . . . . ? C11 C7 C8 C9 -177.62(10) . . . . ? C7 C8 C9 C12 -2.75(15) . . . . ? C7 C8 C9 C10 177.35(10) . . . . ? C8 C9 C10 N1 -171.51(10) . . . 3_657 ? C12 C9 C10 N1 8.60(17) . . . 3_657 ? C6 C5 C12 O1 -179.54(9) . . . . ? C4 C5 C12 O1 0.16(15) . . . . ? C6 C5 C12 C9 0.91(14) . . . . ? C4 C5 C12 C9 -179.39(9) . . . . ? C8 C9 C12 O1 -178.30(9) . . . . ? C10 C9 C12 O1 1.59(15) . . . . ? C8 C9 C12 C5 1.26(14) . . . . ? C10 C9 C12 C5 -178.85(9) . . . . ? O2 C13 C14 C15 178.07(9) . . . . ? C18 C13 C14 C15 -2.32(14) . . . . ? C13 C14 C15 C16 1.25(15) . . . . ? C13 C14 C15 P1 174.53(7) . . . . ? C14 C15 C16 C17 0.63(16) . . . . ? P1 C15 C16 C17 -172.69(8) . . . . ? C15 C16 C17 C18 -1.39(17) . . . . ? C16 C17 C18 C13 0.27(17) . . . . ? O2 C13 C18 C17 -178.84(10) . . . . ? C14 C13 C18 C17 1.56(15) . . . . ? C24 C19 C20 C21 -0.88(17) . . . . ? P1 C19 C20 C21 179.82(10) . . . . ? C19 C20 C21 C22 0.28(19) . . . . ? C20 C21 C22 C23 0.4(2) . . . . ? C21 C22 C23 C24 -0.39(18) . . . . ? C22 C23 C24 C19 -0.22(17) . . . . ? C20 C19 C24 C23 0.86(16) . . . . ? P1 C19 C24 C23 -179.87(8) . . . . ? C30 C25 C26 C27 -1.50(18) . . . . ? P1 C25 C26 C27 177.67(10) . . . . ? C25 C26 C27 C28 0.8(2) . . . . ? C26 C27 C28 C29 0.9(2) . . . . ? C27 C28 C29 C30 -1.9(2) . . . . ? C28 C29 C30 C25 1.25(19) . . . . ? C26 C25 C30 C29 0.47(17) . . . . ? P1 C25 C30 C29 -178.75(9) . . . . ? C2 C1 N1 C10 -139.41(10) . . . 3_657 ? C2 C1 N1 Zn1 48.64(13) . . . . ? C5 C4 N2 C3 178.88(10) . . . . ? C5 C4 N2 Zn1 5.51(16) . . . . ? C2 C3 N2 C4 140.74(10) . . . . ? C2 C3 N2 Zn1 -45.70(12) . . . . ? C5 C12 O1 Zn1 -19.72(13) . . . . ? C9 C12 O1 Zn1 159.82(7) . . . . ? C5 C12 O1 Zn1 155.48(7) . . . 3_657 ? C9 C12 O1 Zn1 -24.98(13) . . . 3_657 ? C14 C13 O2 Zn1 -106.39(9) . . . . ? C18 C13 O2 Zn1 74.02(11) . . . . ? C14 C15 P1 O3 -91.87(9) . . . . ? C16 C15 P1 O3 81.46(9) . . . . ? C14 C15 P1 C25 145.83(8) . . . . ? C16 C15 P1 C25 -40.85(10) . . . . ? C14 C15 P1 C19 31.59(9) . . . . ? C16 C15 P1 C19 -155.08(8) . . . . ? C30 C25 P1 O3 18.80(10) . . . . ? C26 C25 P1 O3 -160.38(9) . . . . ? C30 C25 P1 C15 143.58(9) . . . . ? C26 C25 P1 C15 -35.61(11) . . . . ? C30 C25 P1 C19 -102.49(9) . . . . ? C26 C25 P1 C19 78.32(10) . . . . ? C20 C19 P1 O3 -13.44(10) . . . . ? C24 C19 P1 O3 167.28(8) . . . . ? C20 C19 P1 C15 -138.91(8) . . . . ? C24 C19 P1 C15 41.81(9) . . . . ? C20 C19 P1 C25 107.41(9) . . . . ? C24 C19 P1 C25 -71.87(9) . . . . ? C13 O2 Zn1 O1 -85.23(7) . . . . ? C13 O2 Zn1 N2 -177.84(7) . . . . ? C13 O2 Zn1 O1 -7.26(7) . . . 3_657 ? C13 O2 Zn1 N1 83.06(7) . . . . ? C12 O1 Zn1 O2 -83.24(8) . . . . ? Zn1 O1 Zn1 O2 100.68(4) 3_657 . . . ? C12 O1 Zn1 N2 24.05(8) . . . . ? Zn1 O1 Zn1 N2 -152.04(4) 3_657 . . . ? C12 O1 Zn1 O1 176.09(10) . . . 3_657 ? Zn1 O1 Zn1 O1 0.0 3_657 . . 3_657 ? C12 O1 Zn1 N1 119.61(9) . . . . ? Zn1 O1 Zn1 N1 -56.47(7) 3_657 . . . ? C4 N2 Zn1 O2 86.83(9) . . . . ? C3 N2 Zn1 O2 -86.12(8) . . . . ? C4 N2 Zn1 O1 -16.18(9) . . . . ? C3 N2 Zn1 O1 170.87(8) . . . . ? C4 N2 Zn1 O1 -75.61(11) . . . 3_657 ? C3 N2 Zn1 O1 111.44(9) . . . 3_657 ? C4 N2 Zn1 N1 -165.96(9) . . . . ? C3 N2 Zn1 N1 21.09(9) . . . . ? C10 N1 Zn1 O2 -84.65(9) 3_657 . . . ? C1 N1 Zn1 O2 86.40(9) . . . . ? C10 N1 Zn1 O1 72.25(12) 3_657 . . . ? C1 N1 Zn1 O1 -116.69(9) . . . . ? C10 N1 Zn1 N2 166.40(9) 3_657 . . . ? C1 N1 Zn1 N2 -22.55(9) . . . . ? C10 N1 Zn1 O1 18.29(9) 3_657 . . 3_657 ? C1 N1 Zn1 O1 -170.66(9) . . . 3_657 ? _diffrn_measured_fraction_theta_max 0.928 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 1.266 _refine_diff_density_min -0.400 _refine_diff_density_rms 0.087 # Attachment '- 8Eprime-SP132_0mX.cif' data_sp132_0m _database_code_depnum_ccdc_archive 'CCDC 825588' #TrackingRef '- 8Eprime-SP132_0mX.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C60 H50 N4 O8 P2 Zn2' _chemical_formula_weight 1147.72 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' P P 0.1023 0.0942 '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 P2(1)/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 18.819(5) _cell_length_b 6.9218(16) _cell_length_c 19.998(5) _cell_angle_alpha 90.00 _cell_angle_beta 100.119(13) _cell_angle_gamma 90.00 _cell_volume 2564.5(11) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 2430 _cell_measurement_theta_min 3.14 _cell_measurement_theta_max 22.73 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.486 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1184 _exptl_absorpt_coefficient_mu 1.061 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.94 _exptl_absorpt_correction_T_max 1.0 _exptl_absorpt_process_details ; SADABS Version 2008/1 Bruker-Nonius Blessing, Acta Cryst. (1995) A51 33-38 ; _exptl_special_details ; It should be noted that the esd's of the cell dimensions are probably too low; they should be multiplied by a factor of 2 to 10 ; _diffrn_ambient_temperature 120(2) _diffrn_measurement_specimen_suppport 'magnetic support whith 10 micron nylon fiber cryoloop' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'rotating anode X-ray tube' _diffrn_source_type 'Bruker-Nonius FR 591' _diffrn_source_power 50 _diffrn_source_current 70 _diffrn_source_size '3 mm x 0.3 mm fine focus' _diffrn_radiation_monochromator 'Multilayer Montel 200 mirrors' _diffrn_detector_type '4K CCD area detector APEX II' _diffrn_measurement_device_type 'Kappa 4-axis goniometer bruker-nonius' _diffrn_measurement_method ; Fullsphere data collection, phi and omega scans ; _diffrn_detector_area_resol_mean 512 _diffrn_reflns_number 19563 _diffrn_reflns_av_R_equivalents 0.0743 _diffrn_reflns_av_sigmaI/netI 0.1128 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 3.12 _diffrn_reflns_theta_max 31.32 _reflns_number_total 7959 _reflns_number_gt 3735 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2 v2009.1-0' _computing_cell_refinement 'Bruker APEX2 v2009.1-0' _computing_data_reduction 'Bruker SAINT V7.60A' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXS-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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 phosphine is diordered in three positions with occupations ratio 45:35:20. C10 is also disordered in two positions with occupations ratio 69:31. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0918P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7959 _refine_ls_number_parameters 711 _refine_ls_number_restraints 2273 _refine_ls_R_factor_all 0.1543 _refine_ls_R_factor_gt 0.0608 _refine_ls_wR_factor_ref 0.1865 _refine_ls_wR_factor_gt 0.1452 _refine_ls_goodness_of_fit_ref 0.975 _refine_ls_restrained_S_all 0.890 _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 C1 C -0.03395(19) 0.7295(5) 0.08672(15) 0.0390(7) Uani 1 1 d . A . C2 C 0.0067(2) 0.8998(5) 0.10259(15) 0.0410(8) Uani 1 1 d . . . C3 C -0.0125(2) 1.0253(5) 0.15188(18) 0.0506(9) Uani 1 1 d . . . H3 H 0.0130 1.1433 0.1614 0.061 Uiso 1 1 calc R . . C4 C -0.0670(3) 0.9819(6) 0.18640(19) 0.0569(10) Uani 1 1 d . . . C5 C -0.1061(2) 0.8152(5) 0.17021(17) 0.0515(9) Uani 1 1 d . . . H5 H -0.1438 0.7848 0.1944 0.062 Uiso 1 1 calc R . . C6 C -0.0924(2) 0.6897(5) 0.11975(15) 0.0424(8) Uani 1 1 d . . . C7 C -0.0854(3) 1.1181(8) 0.2414(3) 0.0880(16) Uani 1 1 d . . . H7A H -0.1377 1.1385 0.2344 0.132 Uiso 1 1 calc R . . H7B H -0.0611 1.2423 0.2387 0.132 Uiso 1 1 calc R . . H7C H -0.0692 1.0605 0.2863 0.132 Uiso 1 1 calc R . . C8 C 0.0645(2) 0.9575(5) 0.06774(16) 0.0430(8) Uani 1 1 d . . . H8 H 0.0779 1.0900 0.0695 0.052 Uiso 1 1 calc R . . C9 C 0.1560(2) 0.9118(5) 0.0008(2) 0.0548(10) Uani 1 1 d D . . H9A H 0.2012 0.9201 0.0344 0.066 Uiso 0.316(17) 1 calc PR A 1 H9B H 0.1439 1.0439 -0.0166 0.066 Uiso 0.316(17) 1 calc PR A 1 H9C H 0.1936 0.9754 0.0345 0.066 Uiso 0.684(17) 1 calc PR A 2 H9D H 0.1360 1.0099 -0.0334 0.066 Uiso 0.684(17) 1 calc PR A 2 C10 C 0.1689(12) 0.7874(13) -0.0568(7) 0.0554(17) Uani 0.316(17) 1 d PDU A 1 H10A H 0.1458 0.8469 -0.1002 0.066 Uiso 0.316(17) 1 calc PR A 1 H10B H 0.2215 0.7794 -0.0568 0.066 Uiso 0.316(17) 1 calc PR A 1 C10' C 0.1902(4) 0.7537(9) -0.0337(5) 0.0554(17) Uani 0.684(17) 1 d PDU A 2 H10C H 0.2049 0.8051 -0.0754 0.066 Uiso 0.684(17) 1 calc PR A 2 H10D H 0.2340 0.7074 -0.0032 0.066 Uiso 0.684(17) 1 calc PR A 2 C11 C -0.1375(2) 0.5184(5) 0.10394(17) 0.0500(9) Uani 1 1 d . . . H11 H -0.1680 0.4840 0.1352 0.060 Uiso 1 1 calc R . . N1 N 0.09844(16) 0.8438(4) 0.03515(13) 0.0410(7) Uani 1 1 d . A . N2 N 0.13955(18) 0.5891(4) -0.05187(15) 0.0492(8) Uani 1 1 d D . . O1 O -0.01717(14) 0.6123(4) 0.04105(12) 0.0508(6) Uani 1 1 d . . . Zn1 Zn 0.08354(2) 0.55357(5) 0.025549(17) 0.04031(15) Uani 1 1 d D . . P1 P 0.3728(2) 0.4144(7) 0.36523(16) 0.0512(10) Uani 0.45 1 d PDU B 1 O4 O 0.3573(6) 0.6155(12) 0.3681(4) 0.117(4) Uani 0.45 1 d PDU B 1 C19 C 0.4619(3) 0.3693(10) 0.3490(3) 0.060(2) Uani 0.45 1 d PGDU B 1 C20 C 0.4796(3) 0.2006(11) 0.3179(4) 0.074(3) Uani 0.45 1 d PGDU B 1 H20 H 0.4435 0.1063 0.3034 0.089 Uiso 0.45 1 calc PR B 1 C21 C 0.5500(4) 0.1701(14) 0.3080(4) 0.087(3) Uani 0.45 1 d PGDU B 1 H21 H 0.5620 0.0549 0.2867 0.105 Uiso 0.45 1 calc PR B 1 C22 C 0.6028(3) 0.3082(16) 0.3292(5) 0.101(4) Uani 0.45 1 d PGDU B 1 H22 H 0.6509 0.2873 0.3224 0.121 Uiso 0.45 1 calc PR B 1 C23 C 0.5851(3) 0.4768(14) 0.3603(5) 0.102(4) Uani 0.45 1 d PGDU B 1 H23 H 0.6212 0.5712 0.3748 0.122 Uiso 0.45 1 calc PR B 1 C24 C 0.5147(4) 0.5074(10) 0.3702(4) 0.095(3) Uani 0.45 1 d PGDU B 1 H24 H 0.5027 0.6226 0.3915 0.114 Uiso 0.45 1 calc PR B 1 C25 C 0.3663(3) 0.2788(8) 0.43906(18) 0.060(3) Uani 0.45 1 d PGDU B 1 C26 C 0.4159(3) 0.1401(9) 0.4677(2) 0.092(4) Uani 0.45 1 d PGDU B 1 H26 H 0.4584 0.1183 0.4492 0.111 Uiso 0.45 1 calc PR B 1 C27 C 0.4033(4) 0.0334(9) 0.5233(2) 0.094(4) Uani 0.45 1 d PGDU B 1 H27 H 0.4372 -0.0613 0.5429 0.112 Uiso 0.45 1 calc PR B 1 C28 C 0.3412(4) 0.0654(12) 0.5504(2) 0.079(4) Uani 0.45 1 d PGDU B 1 H28 H 0.3326 -0.0076 0.5884 0.095 Uiso 0.45 1 calc PR B 1 C29 C 0.2916(4) 0.2040(13) 0.5218(2) 0.076(3) Uani 0.45 1 d PGDU B 1 H29 H 0.2491 0.2258 0.5402 0.091 Uiso 0.45 1 calc PR B 1 C30 C 0.3041(3) 0.3107(10) 0.4661(2) 0.062(3) Uani 0.45 1 d PGDU B 1 H30 H 0.2702 0.4054 0.4466 0.075 Uiso 0.45 1 calc PR B 1 C12 C 0.1878(4) 0.4608(8) 0.1379(3) 0.035(3) Uani 0.45 1 d PGDU B 1 C13 C 0.2263(3) 0.3297(7) 0.1931(2) 0.036(3) Uani 0.45 1 d PGDU B 1 C14 C 0.2151(4) 0.1326(7) 0.1919(3) 0.037(3) Uani 0.45 1 d PGDU B 1 H14 H 0.1829 0.0765 0.1551 0.044 Uiso 0.45 1 calc PR B 1 C15 C 0.2497(5) 0.0164(6) 0.2431(3) 0.046(4) Uani 0.45 1 d PGDU B 1 H15 H 0.2409 -0.1188 0.2419 0.055 Uiso 0.45 1 calc PR B 1 C16 C 0.2977(3) 0.0973(6) 0.2965(2) 0.052(3) Uani 0.45 1 d PGDU B 1 H16 H 0.3220 0.0164 0.3316 0.063 Uiso 0.45 1 calc PR B 1 C17 C 0.3106(2) 0.2973(7) 0.29920(18) 0.044(2) Uani 0.45 1 d PGDU B 1 C18 C 0.2749(3) 0.4107(6) 0.2459(2) 0.045(3) Uani 0.45 1 d PGDU B 1 H18 H 0.2840 0.5457 0.2459 0.054 Uiso 0.45 1 calc PR B 1 O2 O 0.1352(5) 0.3885(9) 0.0983(3) 0.042(4) Uani 0.45 1 d PGDU B 1 O3 O 0.2090(5) 0.6283(8) 0.1350(3) 0.040(3) Uani 0.45 1 d PGDU B 1 P1Y P 0.3699(4) 0.3630(10) 0.3659(3) 0.106(3) Uani 0.35 1 d PDU C 2 O4Y O 0.3518(7) 0.5609(14) 0.3732(5) 0.164(7) Uani 0.35 1 d PDU C 2 C19Y C 0.4613(4) 0.3319(15) 0.3537(4) 0.096(4) Uani 0.35 1 d PDU C 2 C20Y C 0.4780(5) 0.248(2) 0.2951(6) 0.106(5) Uani 0.35 1 d PDU C 2 H20Y H 0.4405 0.1987 0.2613 0.128 Uiso 0.35 1 calc PR C 2 C21Y C 0.5494(5) 0.237(2) 0.2861(7) 0.111(5) Uani 0.35 1 d PDU C 2 H21Y H 0.5615 0.1667 0.2488 0.133 Uiso 0.35 1 calc PR C 2 C22Y C 0.6032(4) 0.328(3) 0.3318(8) 0.107(5) Uani 0.35 1 d PDU C 2 H22Y H 0.6512 0.3329 0.3230 0.128 Uiso 0.35 1 calc PR C 2 C23Y C 0.5866(4) 0.412(3) 0.3903(7) 0.124(5) Uani 0.35 1 d PDU C 2 H23Y H 0.6240 0.4608 0.4242 0.149 Uiso 0.35 1 calc PR C 2 C24Y C 0.5151(5) 0.425(2) 0.3990(6) 0.114(5) Uani 0.35 1 d PDU C 2 H24Y H 0.5029 0.4963 0.4359 0.137 Uiso 0.35 1 calc PR C 2 C25Y C 0.3604(5) 0.2095(11) 0.4347(3) 0.089(4) Uani 0.35 1 d PDU C 2 C26Y C 0.3928(7) 0.0294(13) 0.4467(6) 0.093(4) Uani 0.35 1 d PDU C 2 H26Y H 0.4246 -0.0164 0.4182 0.112 Uiso 0.35 1 calc PR C 2 C27Y C 0.3787(8) -0.0837(14) 0.5002(6) 0.096(4) Uani 0.35 1 d PDU C 2 H27Y H 0.4015 -0.2057 0.5090 0.115 Uiso 0.35 1 calc PR C 2 C28Y C 0.3310(9) -0.0181(18) 0.5410(7) 0.110(5) Uani 0.35 1 d PDU C 2 H28Y H 0.3178 -0.0999 0.5750 0.132 Uiso 0.35 1 calc PR C 2 C29Y C 0.3028(10) 0.168(2) 0.5320(8) 0.113(5) Uani 0.35 1 d PDU C 2 H29Y H 0.2763 0.2204 0.5640 0.136 Uiso 0.35 1 calc PR C 2 C30Y C 0.3133(9) 0.2757(18) 0.4760(8) 0.098(4) Uani 0.35 1 d PDU C 2 H30Y H 0.2885 0.3946 0.4660 0.117 Uiso 0.35 1 calc PR C 2 C12Y C 0.1931(8) 0.4458(14) 0.1350(6) 0.056(4) Uani 0.35 1 d PDU C 2 C13Y C 0.2286(8) 0.3063(10) 0.1889(6) 0.055(4) Uani 0.35 1 d PDU C 2 C14Y C 0.2169(11) 0.1097(11) 0.1833(7) 0.057(4) Uani 0.35 1 d PDU C 2 H14Y H 0.1862 0.0594 0.1443 0.069 Uiso 0.35 1 calc PR C 2 C15Y C 0.2491(11) -0.0144(10) 0.2331(8) 0.063(4) Uani 0.35 1 d PDU C 2 H15Y H 0.2384 -0.1486 0.2299 0.075 Uiso 0.35 1 calc PR C 2 C16Y C 0.2973(11) 0.0569(9) 0.2882(7) 0.065(4) Uani 0.35 1 d PDU C 2 H16Y H 0.3203 -0.0295 0.3222 0.078 Uiso 0.35 1 calc PR C 2 C17Y C 0.3125(5) 0.2557(9) 0.2942(4) 0.063(3) Uani 0.35 1 d PDU C 2 C18Y C 0.2754(9) 0.3786(10) 0.2447(6) 0.059(4) Uani 0.35 1 d PDU C 2 H18Y H 0.2823 0.5142 0.2493 0.071 Uiso 0.35 1 calc PR C 2 O2Y O 0.1334(10) 0.394(2) 0.1010(10) 0.055(5) Uani 0.35 1 d PDU C 2 O3Y O 0.2221(9) 0.6030(18) 0.1294(9) 0.082(6) Uani 0.35 1 d PDU C 2 P1X P 0.3558(5) 0.4616(14) 0.3666(5) 0.088(3) Uani 0.20 1 d PDU D 3 O4X O 0.3216(8) 0.644(2) 0.3714(8) 0.144(8) Uani 0.20 1 d PDU D 3 C19X C 0.4470(6) 0.4860(17) 0.3533(7) 0.104(5) Uani 0.20 1 d PDU D 3 C20X C 0.4810(8) 0.344(3) 0.3212(16) 0.110(5) Uani 0.20 1 d PDU D 3 H20X H 0.4559 0.2289 0.3058 0.132 Uiso 0.20 1 calc PR D 3 C21X C 0.5517(8) 0.371(3) 0.3115(15) 0.125(5) Uani 0.20 1 d PDU D 3 H21X H 0.5755 0.2726 0.2907 0.150 Uiso 0.20 1 calc PR D 3 C22X C 0.5877(8) 0.542(3) 0.3325(14) 0.127(6) Uani 0.20 1 d PDU D 3 H22X H 0.6340 0.5664 0.3216 0.153 Uiso 0.20 1 calc PR D 3 C23X C 0.5557(8) 0.677(3) 0.3693(15) 0.135(7) Uani 0.20 1 d PDU D 3 H23X H 0.5818 0.7883 0.3871 0.162 Uiso 0.20 1 calc PR D 3 C24X C 0.4854(9) 0.648(3) 0.3800(14) 0.127(6) Uani 0.20 1 d PDU D 3 H24X H 0.4636 0.7398 0.4055 0.152 Uiso 0.20 1 calc PR D 3 C25X C 0.3603(5) 0.307(2) 0.4378(5) 0.085(5) Uani 0.20 1 d PDU D 3 C26X C 0.4239(6) 0.250(3) 0.4796(8) 0.089(5) Uani 0.20 1 d PDU D 3 H26X H 0.4692 0.2783 0.4669 0.107 Uiso 0.20 1 calc PR D 3 C27X C 0.4213(8) 0.153(4) 0.5400(9) 0.106(6) Uani 0.20 1 d PDU D 3 H27X H 0.4646 0.1090 0.5675 0.127 Uiso 0.20 1 calc PR D 3 C28X C 0.3552(9) 0.121(4) 0.5600(8) 0.100(6) Uani 0.20 1 d PDU D 3 H28X H 0.3535 0.0720 0.6040 0.120 Uiso 0.20 1 calc PR D 3 C29X C 0.2916(8) 0.161(4) 0.5152(10) 0.090(5) Uani 0.20 1 d PDU D 3 H29X H 0.2465 0.1202 0.5256 0.108 Uiso 0.20 1 calc PR D 3 C30X C 0.2941(6) 0.260(4) 0.4553(9) 0.077(5) Uani 0.20 1 d PDU D 3 H30X H 0.2506 0.2961 0.4263 0.092 Uiso 0.20 1 calc PR D 3 C12X C 0.1782(13) 0.4572(14) 0.1370(10) 0.051(5) Uani 0.20 1 d PDU D 3 C13X C 0.2214(10) 0.3338(15) 0.1920(8) 0.050(5) Uani 0.20 1 d PDU D 3 C14X C 0.2057(14) 0.1410(16) 0.1995(11) 0.044(5) Uani 0.20 1 d PDU D 3 H14X H 0.1682 0.0819 0.1683 0.052 Uiso 0.20 1 calc PR D 3 C15X C 0.2436(14) 0.0335(15) 0.2516(11) 0.049(4) Uani 0.20 1 d PDU D 3 H15X H 0.2356 -0.1017 0.2537 0.058 Uiso 0.20 1 calc PR D 3 C16X C 0.2939(12) 0.1233(13) 0.3011(9) 0.050(4) Uani 0.20 1 d PDU D 3 H16X H 0.3188 0.0497 0.3380 0.060 Uiso 0.20 1 calc PR D 3 C17X C 0.3081(6) 0.3220(15) 0.2972(5) 0.072(5) Uani 0.20 1 d PDU D 3 C18X C 0.2747(12) 0.421(2) 0.2392(8) 0.056(5) Uani 0.20 1 d PDU D 3 H18X H 0.2887 0.5501 0.2319 0.068 Uiso 0.20 1 calc PR D 3 O2X O 0.1348(19) 0.3696(19) 0.0922(14) 0.047(6) Uani 0.20 1 d PDU D 3 O3X O 0.1899(14) 0.6322(15) 0.1371(12) 0.070(7) Uani 0.20 1 d PDU 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 C1 0.041(2) 0.0440(17) 0.0309(14) -0.0002(12) 0.0027(13) -0.0032(15) C2 0.043(2) 0.0402(17) 0.0370(16) 0.0012(12) -0.0008(14) -0.0016(15) C3 0.052(2) 0.0452(19) 0.052(2) -0.0091(15) 0.0019(18) -0.0065(18) C4 0.066(3) 0.057(2) 0.050(2) -0.0112(16) 0.0180(19) 0.001(2) C5 0.057(3) 0.060(2) 0.0410(17) 0.0000(15) 0.0171(16) -0.0064(19) C6 0.048(2) 0.0454(17) 0.0347(15) 0.0017(13) 0.0086(14) -0.0043(16) C7 0.086(4) 0.092(3) 0.091(3) -0.043(3) 0.030(3) -0.013(3) C8 0.045(2) 0.0374(16) 0.0435(17) 0.0040(14) -0.0003(15) -0.0091(16) C9 0.047(2) 0.050(2) 0.070(2) 0.0058(17) 0.0155(19) -0.0122(18) C10 0.055(3) 0.059(2) 0.052(3) 0.002(2) 0.011(2) -0.013(2) C10' 0.055(3) 0.059(2) 0.052(3) 0.002(2) 0.011(2) -0.013(2) C11 0.056(3) 0.055(2) 0.0431(18) 0.0046(15) 0.0181(16) -0.0101(18) N1 0.0361(18) 0.0450(15) 0.0404(14) 0.0037(11) 0.0028(12) -0.0082(13) N2 0.051(2) 0.0510(17) 0.0474(16) -0.0016(12) 0.0130(14) -0.0165(15) O1 0.0431(16) 0.0597(14) 0.0521(14) -0.0189(11) 0.0155(11) -0.0185(12) Zn1 0.0411(3) 0.0428(2) 0.0368(2) -0.00183(15) 0.00628(15) -0.01096(19) P1 0.0438(18) 0.073(3) 0.0318(14) 0.0049(14) -0.0070(12) 0.0150(16) O4 0.139(9) 0.088(5) 0.108(7) -0.018(5) -0.018(7) 0.022(6) C19 0.054(4) 0.086(6) 0.037(5) 0.009(4) 0.001(4) -0.002(4) C20 0.050(5) 0.114(7) 0.057(5) -0.009(5) 0.005(4) 0.005(5) C21 0.063(6) 0.137(8) 0.063(6) -0.008(6) 0.016(5) 0.006(5) C22 0.065(7) 0.133(8) 0.106(8) 0.027(7) 0.018(7) -0.007(6) C23 0.075(6) 0.125(7) 0.100(8) 0.022(6) 0.001(6) -0.025(6) C24 0.065(5) 0.107(7) 0.103(7) 0.001(6) -0.017(6) -0.008(5) C25 0.052(5) 0.091(6) 0.037(4) 0.002(4) 0.006(4) 0.027(5) C26 0.086(7) 0.112(8) 0.086(7) 0.035(6) 0.036(6) 0.051(6) C27 0.084(7) 0.112(8) 0.088(7) 0.042(6) 0.026(6) 0.033(6) C28 0.077(7) 0.094(8) 0.067(6) 0.022(5) 0.017(5) 0.019(6) C29 0.077(7) 0.102(7) 0.054(5) 0.022(5) 0.025(5) 0.031(5) C30 0.061(6) 0.076(6) 0.050(5) 0.001(4) 0.010(4) 0.029(5) C12 0.039(6) 0.033(4) 0.033(5) 0.000(4) 0.007(4) -0.001(4) C13 0.038(6) 0.039(4) 0.031(5) -0.001(4) 0.004(4) 0.005(5) C14 0.047(6) 0.040(4) 0.029(4) -0.006(3) 0.021(4) 0.008(4) C15 0.058(7) 0.037(4) 0.047(6) -0.001(4) 0.021(6) 0.018(5) C16 0.056(7) 0.054(4) 0.046(6) 0.007(5) 0.008(5) 0.025(5) C17 0.040(5) 0.053(4) 0.038(4) 0.000(3) 0.004(4) 0.020(4) C18 0.052(7) 0.048(5) 0.032(4) 0.000(4) -0.003(4) 0.007(5) O2 0.051(7) 0.038(7) 0.032(6) -0.001(5) -0.002(5) -0.008(6) O3 0.021(5) 0.047(4) 0.048(5) 0.008(3) -0.005(4) -0.002(3) P1Y 0.106(5) 0.112(5) 0.090(4) -0.024(3) -0.014(3) 0.016(4) O4Y 0.199(14) 0.101(7) 0.178(14) -0.036(7) -0.003(12) 0.016(9) C19Y 0.097(6) 0.117(9) 0.066(8) 0.005(7) -0.004(6) -0.019(7) C20Y 0.084(7) 0.113(9) 0.116(9) -0.023(8) 0.001(7) -0.004(8) C21Y 0.095(8) 0.123(10) 0.114(9) -0.007(8) 0.013(7) 0.000(8) C22Y 0.081(8) 0.131(10) 0.106(9) 0.021(8) 0.009(7) -0.011(8) C23Y 0.100(7) 0.142(10) 0.128(9) -0.013(8) 0.015(8) -0.022(9) C24Y 0.100(6) 0.124(10) 0.116(9) -0.017(7) 0.010(7) -0.026(8) C25Y 0.066(8) 0.122(8) 0.072(6) -0.015(5) -0.007(5) 0.011(7) C26Y 0.075(9) 0.118(8) 0.084(8) -0.013(6) 0.008(6) 0.010(7) C27Y 0.090(10) 0.109(9) 0.085(8) -0.008(6) 0.006(7) 0.003(8) C28Y 0.108(10) 0.128(9) 0.097(9) 0.007(7) 0.027(7) 0.013(8) C29Y 0.102(10) 0.136(9) 0.107(9) 0.003(8) 0.032(7) 0.027(8) C30Y 0.092(9) 0.109(8) 0.085(8) -0.009(7) -0.004(6) 0.033(7) C12Y 0.056(8) 0.058(6) 0.057(7) 0.004(6) 0.019(6) -0.009(6) C13Y 0.052(8) 0.064(6) 0.049(6) 0.001(5) 0.012(5) -0.001(6) C14Y 0.061(8) 0.059(5) 0.051(7) -0.008(5) 0.011(6) 0.001(6) C15Y 0.073(9) 0.055(6) 0.062(7) -0.009(5) 0.018(6) 0.013(6) C16Y 0.069(8) 0.064(6) 0.062(7) -0.002(5) 0.013(6) 0.018(6) C17Y 0.070(7) 0.067(6) 0.052(6) 0.004(5) 0.012(5) 0.004(6) C18Y 0.055(8) 0.056(6) 0.067(7) 0.003(5) 0.013(6) -0.005(6) O2Y 0.052(8) 0.052(9) 0.061(9) 0.017(8) 0.009(7) -0.005(7) O3Y 0.058(9) 0.077(7) 0.110(11) 0.021(7) 0.009(7) -0.020(6) P1X 0.100(7) 0.072(6) 0.088(5) 0.002(4) 0.006(5) 0.013(5) O4X 0.173(14) 0.111(10) 0.148(15) -0.013(8) 0.026(13) 0.048(11) C19X 0.100(7) 0.119(10) 0.091(10) 0.007(8) 0.008(7) -0.012(7) C20X 0.090(8) 0.130(10) 0.106(11) -0.004(9) 0.004(9) -0.003(8) C21X 0.101(8) 0.145(10) 0.128(10) 0.002(9) 0.016(9) -0.006(9) C22X 0.108(10) 0.149(11) 0.124(12) 0.013(10) 0.018(9) -0.017(8) C23X 0.109(10) 0.145(12) 0.146(13) -0.003(10) 0.006(11) -0.019(10) C24X 0.110(10) 0.138(11) 0.128(13) -0.011(10) 0.006(10) -0.017(9) C25X 0.076(8) 0.110(10) 0.070(7) -0.009(7) 0.014(7) 0.013(9) C26X 0.074(8) 0.114(12) 0.080(9) 0.002(8) 0.015(7) 0.013(10) C27X 0.086(8) 0.130(12) 0.100(10) 0.018(9) 0.010(9) 0.008(11) C28X 0.087(9) 0.122(11) 0.091(10) 0.019(9) 0.015(7) 0.011(10) C29X 0.082(8) 0.109(10) 0.080(9) 0.000(8) 0.019(8) 0.022(9) C30X 0.071(8) 0.084(10) 0.073(8) -0.018(7) 0.004(7) 0.007(8) C12X 0.055(9) 0.053(7) 0.048(9) -0.003(7) 0.018(7) -0.001(8) C13X 0.047(9) 0.056(7) 0.052(8) -0.003(7) 0.020(7) 0.004(8) C14X 0.034(8) 0.055(7) 0.047(8) -0.004(6) 0.023(6) 0.007(6) C15X 0.048(8) 0.059(8) 0.049(8) 0.000(6) 0.035(6) 0.016(7) C16X 0.053(9) 0.070(7) 0.034(8) 0.015(7) 0.023(6) 0.018(8) C17X 0.068(9) 0.078(8) 0.068(8) 0.017(7) 0.012(8) 0.003(8) C18X 0.055(10) 0.055(8) 0.062(8) 0.012(7) 0.018(7) -0.001(8) O2X 0.058(10) 0.041(9) 0.046(8) -0.007(7) 0.016(7) -0.004(7) O3X 0.072(15) 0.064(7) 0.068(11) -0.003(8) -0.003(9) -0.013(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 C1 O1 1.301(4) . ? C1 C6 1.406(5) . ? C1 C2 1.411(5) . ? C2 C3 1.408(5) . ? C2 C8 1.448(5) . ? C3 C4 1.366(6) . ? C4 C5 1.377(5) . ? C4 C7 1.534(6) . ? C5 C6 1.390(5) . ? C6 C11 1.461(5) . ? C8 N1 1.264(4) . ? C9 N1 1.458(5) . ? C9 C10 1.493(7) . ? C9 C10' 1.498(6) . ? C10 N2 1.489(6) . ? C10' N2 1.488(5) . ? C11 N2 1.275(4) 3_565 ? N1 Zn1 2.033(3) . ? N2 C11 1.275(4) 3_565 ? N2 Zn1 2.035(3) . ? O1 Zn1 2.015(3) . ? O1 Zn1 2.017(2) 3_565 ? Zn1 O2 1.967(3) . ? Zn1 O2X 1.969(4) . ? Zn1 O2Y 1.969(4) . ? Zn1 O1 2.017(2) 3_565 ? P1 O4 1.425(7) . ? P1 C25 1.772(4) . ? P1 C19 1.792(5) . ? P1 C17 1.796(3) . ? C19 C20 1.3900 . ? C19 C24 1.3900 . ? C20 C21 1.3900 . ? C21 C22 1.3900 . ? C22 C23 1.3900 . ? C23 C24 1.3900 . ? C25 C26 1.3900 . ? C25 C30 1.3900 . ? C26 C27 1.3900 . ? C27 C28 1.3900 . ? C28 C29 1.3900 . ? C29 C30 1.3900 . ? C12 O3 1.2310 . ? C12 O2 1.2578 . ? C12 C13 1.5119 . ? C13 C14 1.3798 . ? C13 C18 1.3885 . ? C14 C15 1.3728 . ? C15 C16 1.3899 . ? C16 C17 1.4056 . ? C17 C18 1.3965 . ? P1Y O4Y 1.425(7) . ? P1Y C25Y 1.772(4) . ? P1Y C19Y 1.792(5) . ? P1Y C17Y 1.796(3) . ? C19Y C20Y 1.3909(9) . ? C19Y C24Y 1.3912(10) . ? C20Y C21Y 1.3902(10) . ? C21Y C22Y 1.3903(10) . ? C22Y C23Y 1.3904(10) . ? C23Y C24Y 1.3902(10) . ? C25Y C26Y 1.3899(9) . ? C25Y C30Y 1.3904(9) . ? C26Y C27Y 1.3901(9) . ? C27Y C28Y 1.3903(9) . ? C28Y C29Y 1.3906(10) . ? C29Y C30Y 1.3904(9) . ? C12Y O3Y 1.2313(9) . ? C12Y O2Y 1.2580(9) . ? C12Y C13Y 1.5120(9) . ? C13Y C14Y 1.3799(9) . ? C13Y C18Y 1.3886(9) . ? C14Y C15Y 1.3728(9) . ? C15Y C16Y 1.3899(9) . ? C16Y C17Y 1.4059(9) . ? C17Y C18Y 1.3969(9) . ? P1X O4X 1.426(7) . ? P1X C25X 1.772(4) . ? P1X C19X 1.791(5) . ? P1X C17X 1.796(3) . ? C19X C20X 1.3902(9) . ? C19X C24X 1.3904(9) . ? C20X C21X 1.3903(10) . ? C21X C22X 1.3902(10) . ? C22X C23X 1.3902(9) . ? C23X C24X 1.3902(10) . ? C25X C26X 1.3903(9) . ? C25X C30X 1.3904(9) . ? C26X C27X 1.3902(10) . ? C27X C28X 1.3905(10) . ? C28X C29X 1.3906(10) . ? C29X C30X 1.3901(10) . ? C12X O3X 1.2313(10) . ? C12X O2X 1.2580(9) . ? C12X C13X 1.5120(9) . ? C13X C14X 1.3801(9) . ? C13X C18X 1.3889(9) . ? C14X C15X 1.3729(10) . ? C15X C16X 1.3900(9) . ? C16X C17X 1.4063(9) . ? C17X C18X 1.3974(9) . ? 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 C6 120.9(3) . . ? O1 C1 C2 119.3(3) . . ? C6 C1 C2 119.8(3) . . ? C3 C2 C1 118.4(3) . . ? C3 C2 C8 118.3(3) . . ? C1 C2 C8 123.1(3) . . ? C4 C3 C2 121.8(3) . . ? C3 C4 C5 118.9(3) . . ? C3 C4 C7 120.8(4) . . ? C5 C4 C7 120.3(4) . . ? C4 C5 C6 122.3(4) . . ? C5 C6 C1 118.6(3) . . ? C5 C6 C11 119.3(3) . . ? C1 C6 C11 122.0(3) . . ? N1 C8 C2 124.5(3) . . ? N1 C9 C10 114.4(5) . . ? N1 C9 C10' 113.3(3) . . ? C10 C9 C10' 23.2(7) . . ? N2 C10 C9 111.5(4) . . ? N2 C10' C9 111.3(4) . . ? N2 C11 C6 125.7(3) 3_565 . ? C8 N1 C9 121.7(3) . . ? C8 N1 Zn1 126.2(2) . . ? C9 N1 Zn1 112.1(2) . . ? C11 N2 C10' 124.9(4) 3_565 . ? C11 N2 C10 116.2(4) 3_565 . ? C10' N2 C10 23.3(7) . . ? C11 N2 Zn1 127.3(3) 3_565 . ? C10' N2 Zn1 107.6(3) . . ? C10 N2 Zn1 114.2(3) . . ? C1 O1 Zn1 125.8(2) . . ? C1 O1 Zn1 128.3(2) . 3_565 ? Zn1 O1 Zn1 105.88(11) . 3_565 ? O2 Zn1 O2X 5.2(9) . . ? O2 Zn1 O2Y 2.3(10) . . ? O2X Zn1 O2Y 7.3(17) . . ? O2 Zn1 O1 111.1(3) . . ? O2X Zn1 O1 112.9(14) . . ? O2Y Zn1 O1 109.2(8) . . ? O2 Zn1 O1 109.0(2) . 3_565 ? O2X Zn1 O1 104.6(4) . 3_565 ? O2Y Zn1 O1 110.1(4) . 3_565 ? O1 Zn1 O1 74.12(11) . 3_565 ? O2 Zn1 N1 117.5(2) . . ? O2X Zn1 N1 122.2(4) . . ? O2Y Zn1 N1 116.2(5) . . ? O1 Zn1 N1 84.49(11) . . ? O1 Zn1 N1 133.17(11) 3_565 . ? O2 Zn1 N2 112.2(3) . . ? O2X Zn1 N2 109.6(14) . . ? O2Y Zn1 N2 114.2(8) . . ? O1 Zn1 N2 136.02(12) . . ? O1 Zn1 N2 84.83(11) 3_565 . ? N1 Zn1 N2 82.59(11) . . ? O4 P1 C25 116.1(4) . . ? O4 P1 C19 112.5(5) . . ? C25 P1 C19 105.2(3) . . ? O4 P1 C17 111.0(3) . . ? C25 P1 C17 104.0(2) . . ? C19 P1 C17 107.3(2) . . ? C20 C19 C24 120.0 . . ? C20 C19 P1 122.2(3) . . ? C24 C19 P1 117.8(3) . . ? C19 C20 C21 120.0 . . ? C22 C21 C20 120.0 . . ? C21 C22 C23 120.0 . . ? C24 C23 C22 120.0 . . ? C23 C24 C19 120.0 . . ? C26 C25 C30 120.0 . . ? C26 C25 P1 124.7(2) . . ? C30 C25 P1 115.2(2) . . ? C27 C26 C25 120.0 . . ? C26 C27 C28 120.0 . . ? C29 C28 C27 120.0 . . ? C30 C29 C28 120.0 . . ? C29 C30 C25 120.0 . . ? O3 C12 O2 124.8 . . ? O3 C12 C13 118.8 . . ? O2 C12 C13 116.4 . . ? C14 C13 C18 119.4 . . ? C14 C13 C12 121.9 . . ? C18 C13 C12 118.7 . . ? C15 C14 C13 121.0 . . ? C14 C15 C16 119.8 . . ? C15 C16 C17 120.7 . . ? C18 C17 C16 117.9 . . ? C18 C17 P1 118.12(16) . . ? C16 C17 P1 123.98(17) . . ? C13 C18 C17 121.2 . . ? C12 O2 Zn1 117.8(3) . . ? O4Y P1Y C25Y 116.0(4) . . ? O4Y P1Y C19Y 112.4(5) . . ? C25Y P1Y C19Y 105.3(3) . . ? O4Y P1Y C17Y 111.0(3) . . ? C25Y P1Y C17Y 104.1(2) . . ? C19Y P1Y C17Y 107.3(3) . . ? C20Y C19Y C24Y 119.66(14) . . ? C20Y C19Y P1Y 121.9(3) . . ? C24Y C19Y P1Y 117.5(3) . . ? C21Y C20Y C19Y 119.94(14) . . ? C20Y C21Y C22Y 119.93(15) . . ? C21Y C22Y C23Y 119.78(15) . . ? C24Y C23Y C22Y 119.88(15) . . ? C23Y C24Y C19Y 119.93(14) . . ? C26Y C25Y C30Y 119.95(11) . . ? C26Y C25Y P1Y 124.8(2) . . ? C30Y C25Y P1Y 115.2(2) . . ? C25Y C26Y C27Y 120.03(12) . . ? C26Y C27Y C28Y 119.91(13) . . ? C27Y C28Y C29Y 119.82(15) . . ? C30Y C29Y C28Y 119.77(16) . . ? C25Y C30Y C29Y 119.83(14) . . ? O3Y C12Y O2Y 124.71(16) . . ? O3Y C12Y C13Y 118.77(15) . . ? O2Y C12Y C13Y 116.43(15) . . ? C14Y C13Y C18Y 119.34(11) . . ? C14Y C13Y C12Y 121.88(13) . . ? C18Y C13Y C12Y 118.76(13) . . ? C15Y C14Y C13Y 120.98(13) . . ? C14Y C15Y C16Y 119.76(13) . . ? C15Y C16Y C17Y 120.71(12) . . ? C18Y C17Y C16Y 117.78(12) . . ? C18Y C17Y P1Y 118.0(2) . . ? C16Y C17Y P1Y 123.9(2) . . ? C13Y C18Y C17Y 121.24(12) . . ? C12Y O2Y Zn1 121.0(5) . . ? O4X P1X C25X 116.0(4) . . ? O4X P1X C19X 112.5(5) . . ? C25X P1X C19X 105.3(3) . . ? O4X P1X C17X 110.9(4) . . ? C25X P1X C17X 104.0(2) . . ? C19X P1X C17X 107.4(3) . . ? C20X C19X C24X 119.92(14) . . ? C20X C19X P1X 122.2(3) . . ? C24X C19X P1X 117.8(3) . . ? C19X C20X C21X 119.92(13) . . ? C22X C21X C20X 119.93(14) . . ? C23X C22X C21X 119.88(16) . . ? C22X C23X C24X 119.92(14) . . ? C23X C24X C19X 119.93(13) . . ? C26X C25X C30X 119.93(11) . . ? C26X C25X P1X 124.6(2) . . ? C30X C25X P1X 115.1(2) . . ? C27X C26X C25X 120.00(13) . . ? C26X C27X C28X 119.82(15) . . ? C27X C28X C29X 119.74(17) . . ? C30X C29X C28X 119.80(16) . . ? C29X C30X C25X 119.96(14) . . ? O3X C12X O2X 124.72(18) . . ? O3X C12X C13X 118.77(16) . . ? O2X C12X C13X 116.43(15) . . ? C14X C13X C18X 119.25(12) . . ? C14X C13X C12X 121.86(16) . . ? C18X C13X C12X 118.71(14) . . ? C15X C14X C13X 120.93(15) . . ? C14X C15X C16X 119.72(15) . . ? C15X C16X C17X 120.64(13) . . ? C18X C17X C16X 117.62(11) . . ? C18X C17X P1X 117.9(2) . . ? C16X C17X P1X 123.8(2) . . ? C13X C18X C17X 121.11(15) . . ? C12X O2X Zn1 110.5(6) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 C1 C2 C3 179.6(3) . . . . ? C6 C1 C2 C3 0.4(5) . . . . ? O1 C1 C2 C8 3.5(5) . . . . ? C6 C1 C2 C8 -175.8(3) . . . . ? C1 C2 C3 C4 3.0(5) . . . . ? C8 C2 C3 C4 179.3(4) . . . . ? C2 C3 C4 C5 -3.0(6) . . . . ? C2 C3 C4 C7 178.1(4) . . . . ? C3 C4 C5 C6 -0.3(6) . . . . ? C7 C4 C5 C6 178.6(4) . . . . ? C4 C5 C6 C1 3.5(6) . . . . ? C4 C5 C6 C11 -178.2(4) . . . . ? O1 C1 C6 C5 177.2(3) . . . . ? C2 C1 C6 C5 -3.5(5) . . . . ? O1 C1 C6 C11 -1.0(5) . . . . ? C2 C1 C6 C11 178.3(3) . . . . ? C3 C2 C8 N1 162.5(3) . . . . ? C1 C2 C8 N1 -21.4(5) . . . . ? N1 C9 C10 N2 -20.1(19) . . . . ? C10' C9 C10 N2 72.5(7) . . . . ? N1 C9 C10' N2 25.6(9) . . . . ? C10 C9 C10' N2 -72.3(7) . . . . ? C5 C6 C11 N2 166.9(4) . . . 3_565 ? C1 C6 C11 N2 -14.9(6) . . . 3_565 ? C2 C8 N1 C9 179.6(3) . . . . ? C2 C8 N1 Zn1 -2.1(5) . . . . ? C10 C9 N1 C8 -155.7(10) . . . . ? C10' C9 N1 C8 178.9(5) . . . . ? C10 C9 N1 Zn1 25.8(11) . . . . ? C10' C9 N1 Zn1 0.4(6) . . . . ? C9 C10' N2 C11 147.0(5) . . . 3_565 ? C9 C10' N2 C10 72.0(7) . . . . ? C9 C10' N2 Zn1 -38.7(8) . . . . ? C9 C10 N2 C11 169.2(10) . . . 3_565 ? C9 C10 N2 C10' -72.9(7) . . . . ? C9 C10 N2 Zn1 5.1(19) . . . . ? C6 C1 O1 Zn1 -144.5(3) . . . . ? C2 C1 O1 Zn1 36.2(4) . . . . ? C6 C1 O1 Zn1 33.0(4) . . . 3_565 ? C2 C1 O1 Zn1 -146.3(3) . . . 3_565 ? C1 O1 Zn1 O2 73.3(3) . . . . ? Zn1 O1 Zn1 O2 -104.7(2) 3_565 . . . ? C1 O1 Zn1 O2X 78.5(6) . . . . ? Zn1 O1 Zn1 O2X -99.4(6) 3_565 . . . ? C1 O1 Zn1 O2Y 71.8(6) . . . . ? Zn1 O1 Zn1 O2Y -106.2(5) 3_565 . . . ? C1 O1 Zn1 O1 178.0(3) . . . 3_565 ? Zn1 O1 Zn1 O1 0.0 3_565 . . 3_565 ? C1 O1 Zn1 N1 -44.1(3) . . . . ? Zn1 O1 Zn1 N1 137.91(13) 3_565 . . . ? C1 O1 Zn1 N2 -117.5(3) . . . . ? Zn1 O1 Zn1 N2 64.55(18) 3_565 . . . ? C8 N1 Zn1 O2 -84.9(5) . . . . ? C9 N1 Zn1 O2 93.5(4) . . . . ? C8 N1 Zn1 O2X -87.6(17) . . . . ? C9 N1 Zn1 O2X 90.8(17) . . . . ? C8 N1 Zn1 O2Y -82.7(10) . . . . ? C9 N1 Zn1 O2Y 95.7(9) . . . . ? C8 N1 Zn1 O1 26.0(3) . . . . ? C9 N1 Zn1 O1 -155.5(2) . . . . ? C8 N1 Zn1 O1 88.1(3) . . . 3_565 ? C9 N1 Zn1 O1 -93.4(3) . . . 3_565 ? C8 N1 Zn1 N2 163.9(3) . . . . ? C9 N1 Zn1 N2 -17.7(2) . . . . ? C11 N2 Zn1 O2 88.1(4) 3_565 . . . ? C10' N2 Zn1 O2 -86.0(5) . . . . ? C10 N2 Zn1 O2 -110.0(11) . . . . ? C11 N2 Zn1 O2X 83.3(6) 3_565 . . . ? C10' N2 Zn1 O2X -90.8(6) . . . . ? C10 N2 Zn1 O2X -114.8(11) . . . . ? C11 N2 Zn1 O2Y 89.4(6) 3_565 . . . ? C10' N2 Zn1 O2Y -84.7(6) . . . . ? C10 N2 Zn1 O2Y -108.7(12) . . . . ? C11 N2 Zn1 O1 -81.0(4) 3_565 . . . ? C10' N2 Zn1 O1 104.9(4) . . . . ? C10 N2 Zn1 O1 80.9(11) . . . . ? C11 N2 Zn1 O1 -20.3(4) 3_565 . . 3_565 ? C10' N2 Zn1 O1 165.6(4) . . . 3_565 ? C10 N2 Zn1 O1 141.6(11) . . . 3_565 ? C11 N2 Zn1 N1 -155.1(4) 3_565 . . . ? C10' N2 Zn1 N1 30.8(4) . . . . ? C10 N2 Zn1 N1 6.8(11) . . . . ? O4 P1 C19 C20 -153.7(5) . . . . ? C25 P1 C19 C20 79.1(5) . . . . ? C17 P1 C19 C20 -31.3(5) . . . . ? O4 P1 C19 C24 28.0(5) . . . . ? C25 P1 C19 C24 -99.3(4) . . . . ? C17 P1 C19 C24 150.4(4) . . . . ? C24 C19 C20 C21 0.0 . . . . ? P1 C19 C20 C21 -178.3(5) . . . . ? C19 C20 C21 C22 0.0 . . . . ? C20 C21 C22 C23 0.0 . . . . ? C21 C22 C23 C24 0.0 . . . . ? C22 C23 C24 C19 0.0 . . . . ? C20 C19 C24 C23 0.0 . . . . ? P1 C19 C24 C23 178.4(5) . . . . ? O4 P1 C25 C26 -136.4(4) . . . . ? C19 P1 C25 C26 -11.4(3) . . . . ? C17 P1 C25 C26 101.4(2) . . . . ? O4 P1 C25 C30 47.4(5) . . . . ? C19 P1 C25 C30 172.4(3) . . . . ? C17 P1 C25 C30 -74.9(3) . . . . ? C30 C25 C26 C27 0.0 . . . . ? P1 C25 C26 C27 -176.04(16) . . . . ? C25 C26 C27 C28 0.0 . . . . ? C26 C27 C28 C29 0.0 . . . . ? C27 C28 C29 C30 0.0 . . . . ? C28 C29 C30 C25 0.0 . . . . ? C26 C25 C30 C29 0.0 . . . . ? P1 C25 C30 C29 176.40(15) . . . . ? O3 C12 C13 C14 -167.3 . . . . ? O2 C12 C13 C14 13.3 . . . . ? O3 C12 C13 C18 12.0 . . . . ? O2 C12 C13 C18 -167.3 . . . . ? C18 C13 C14 C15 1.7 . . . . ? C12 C13 C14 C15 -178.9 . . . . ? C13 C14 C15 C16 -0.9 . . . . ? C14 C15 C16 C17 0.7 . . . . ? C15 C16 C17 C18 -1.3 . . . . ? C15 C16 C17 P1 -178.8(2) . . . . ? O4 P1 C17 C18 22.3(5) . . . . ? C25 P1 C17 C18 147.84(19) . . . . ? C19 P1 C17 C18 -101.0(3) . . . . ? O4 P1 C17 C16 -160.1(5) . . . . ? C25 P1 C17 C16 -34.6(4) . . . . ? C19 P1 C17 C16 76.6(3) . . . . ? C14 C13 C18 C17 -2.3 . . . . ? C12 C13 C18 C17 178.3 . . . . ? C16 C17 C18 C13 2.1 . . . . ? P1 C17 C18 C13 179.8(2) . . . . ? O3 C12 O2 Zn1 0.9(4) . . . . ? C13 C12 O2 Zn1 -179.9(4) . . . . ? O2X Zn1 O2 C12 136(15) . . . . ? O2Y Zn1 O2 C12 -74(13) . . . . ? O1 Zn1 O2 C12 -112.3(3) . . . . ? O1 Zn1 O2 C12 168.0(2) 3_565 . . . ? N1 Zn1 O2 C12 -17.4(5) . . . . ? N2 Zn1 O2 C12 75.8(4) . . . . ? O4Y P1Y C19Y C20Y -118.8(10) . . . . ? C25Y P1Y C19Y C20Y 114.0(10) . . . . ? C17Y P1Y C19Y C20Y 3.5(10) . . . . ? O4Y P1Y C19Y C24Y 50.1(10) . . . . ? C25Y P1Y C19Y C24Y -77.1(9) . . . . ? C17Y P1Y C19Y C24Y 172.4(9) . . . . ? C24Y C19Y C20Y C21Y 8(2) . . . . ? P1Y C19Y C20Y C21Y 176.4(12) . . . . ? C19Y C20Y C21Y C22Y -7(2) . . . . ? C20Y C21Y C22Y C23Y 7(2) . . . . ? C21Y C22Y C23Y C24Y -8(2) . . . . ? C22Y C23Y C24Y C19Y 8(2) . . . . ? C20Y C19Y C24Y C23Y -8.2(19) . . . . ? P1Y C19Y C24Y C23Y -177.3(12) . . . . ? O4Y P1Y C25Y C26Y -161.5(10) . . . . ? C19Y P1Y C25Y C26Y -36.5(10) . . . . ? C17Y P1Y C25Y C26Y 76.3(10) . . . . ? O4Y P1Y C25Y C30Y 22.3(13) . . . . ? C19Y P1Y C25Y C30Y 147.3(12) . . . . ? C17Y P1Y C25Y C30Y -99.9(12) . . . . ? C30Y C25Y C26Y C27Y -1(2) . . . . ? P1Y C25Y C26Y C27Y -176.6(11) . . . . ? C25Y C26Y C27Y C28Y 1(2) . . . . ? C26Y C27Y C28Y C29Y -6(2) . . . . ? C27Y C28Y C29Y C30Y 10(2) . . . . ? C26Y C25Y C30Y C29Y 5(2) . . . . ? P1Y C25Y C30Y C29Y -179.1(12) . . . . ? C28Y C29Y C30Y C25Y -9(2) . . . . ? O3Y C12Y C13Y C14Y -155(2) . . . . ? O2Y C12Y C13Y C14Y 28(2) . . . . ? O3Y C12Y C13Y C18Y 23(2) . . . . ? O2Y C12Y C13Y C18Y -153.5(19) . . . . ? C18Y C13Y C14Y C15Y 2(3) . . . . ? C12Y C13Y C14Y C15Y -179.2(18) . . . . ? C13Y C14Y C15Y C16Y -4(3) . . . . ? C14Y C15Y C16Y C17Y 1(3) . . . . ? C15Y C16Y C17Y C18Y 3(2) . . . . ? C15Y C16Y C17Y P1Y 176.2(16) . . . . ? O4Y P1Y C17Y C18Y 18.9(12) . . . . ? C25Y P1Y C17Y C18Y 144.3(11) . . . . ? C19Y P1Y C17Y C18Y -104.3(11) . . . . ? O4Y P1Y C17Y C16Y -154.7(14) . . . . ? C25Y P1Y C17Y C16Y -29.3(14) . . . . ? C19Y P1Y C17Y C16Y 82.0(14) . . . . ? C14Y C13Y C18Y C17Y 2(3) . . . . ? C12Y C13Y C18Y C17Y -176.7(13) . . . . ? C16Y C17Y C18Y C13Y -4(2) . . . . ? P1Y C17Y C18Y C13Y -178.2(13) . . . . ? O3Y C12Y O2Y Zn1 7(3) . . . . ? C13Y C12Y O2Y Zn1 -176.3(14) . . . . ? O2 Zn1 O2Y C12Y 93(13) . . . . ? O2X Zn1 O2Y C12Y 114(14) . . . . ? O1 Zn1 O2Y C12Y -125.0(18) . . . . ? O1 Zn1 O2Y C12Y 155.4(17) 3_565 . . . ? N1 Zn1 O2Y C12Y -32(2) . . . . ? N2 Zn1 O2Y C12Y 62(2) . . . . ? O4X P1X C19X C20X -153.8(18) . . . . ? C25X P1X C19X C20X 78.9(18) . . . . ? C17X P1X C19X C20X -31.5(18) . . . . ? O4X P1X C19X C24X 29.9(18) . . . . ? C25X P1X C19X C24X -97.3(17) . . . . ? C17X P1X C19X C24X 152.2(17) . . . . ? C24X C19X C20X C21X -4(4) . . . . ? P1X C19X C20X C21X 179(2) . . . . ? C19X C20X C21X C22X -2(4) . . . . ? C20X C21X C22X C23X 7(3) . . . . ? C21X C22X C23X C24X -6(4) . . . . ? C22X C23X C24X C19X -1(4) . . . . ? C20X C19X C24X C23X 6(3) . . . . ? P1X C19X C24X C23X -178(2) . . . . ? O4X P1X C25X C26X -114.8(14) . . . . ? C19X P1X C25X C26X 10.3(13) . . . . ? C17X P1X C25X C26X 123.1(13) . . . . ? O4X P1X C25X C30X 57.9(14) . . . . ? C19X P1X C25X C30X -177.0(13) . . . . ? C17X P1X C25X C30X -64.2(13) . . . . ? C30X C25X C26X C27X -2(2) . . . . ? P1X C25X C26X C27X 170.1(18) . . . . ? C25X C26X C27X C28X -3(3) . . . . ? C26X C27X C28X C29X 9(3) . . . . ? C27X C28X C29X C30X -10(3) . . . . ? C28X C29X C30X C25X 5(3) . . . . ? C26X C25X C30X C29X 1(3) . . . . ? P1X C25X C30X C29X -172(2) . . . . ? O3X C12X C13X C14X 173(3) . . . . ? O2X C12X C13X C14X -11(3) . . . . ? O3X C12X C13X C18X -3(3) . . . . ? O2X C12X C13X C18X 174(3) . . . . ? C18X C13X C14X C15X -2(3) . . . . ? C12X C13X C14X C15X -177(3) . . . . ? C13X C14X C15X C16X 6(4) . . . . ? C14X C15X C16X C17X -2(4) . . . . ? C15X C16X C17X C18X -5(2) . . . . ? C15X C16X C17X P1X 166(2) . . . . ? O4X P1X C17X C18X 33.7(13) . . . . ? C25X P1X C17X C18X 159.1(12) . . . . ? C19X P1X C17X C18X -89.6(12) . . . . ? O4X P1X C17X C16X -137.2(15) . . . . ? C25X P1X C17X C16X -11.8(14) . . . . ? C19X P1X C17X C16X 99.5(15) . . . . ? C14X C13X C18X C17X -6(3) . . . . ? C12X C13X C18X C17X 170(2) . . . . ? C16X C17X C18X C13X 9.3(16) . . . . ? P1X C17X C18X C13X -162.1(16) . . . . ? O3X C12X O2X Zn1 -4(4) . . . . ? C13X C12X O2X Zn1 180(2) . . . . ? O2 Zn1 O2X C12X -31(13) . . . . ? O2Y Zn1 O2X C12X -40(10) . . . . ? O1 Zn1 O2X C12X -101(3) . . . . ? O1 Zn1 O2X C12X -180(2) 3_565 . . . ? N1 Zn1 O2X C12X -3(4) . . . . ? N2 Zn1 O2X C12X 90(3) . . . . ? _diffrn_measured_fraction_theta_max 0.948 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 0.747 _refine_diff_density_min -0.557 _refine_diff_density_rms 0.083 data_sp218_0m _database_code_depnum_ccdc_archive 'CCDC 825589' #TrackingRef '- 7C-SP218_0mX.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C70 H76 Cl8 N6 O10 P2 Zn2' _chemical_formula_weight 1637.65 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' P P 0.1023 0.0942 '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 Monoclinic _symmetry_space_group_name_H-M P2(1)/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 8.8886(14) _cell_length_b 21.225(4) _cell_length_c 19.390(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.878(8) _cell_angle_gamma 90.00 _cell_volume 3657.7(10) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 684 _cell_measurement_theta_min 2.99 _cell_measurement_theta_max 18.66 _exptl_crystal_description Needle _exptl_crystal_colour white _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.487 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1688 _exptl_absorpt_coefficient_mu 1.053 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.95 _exptl_absorpt_correction_T_max 1.0 _exptl_absorpt_process_details ; SADABS Version 2008/1 Bruker-Nonius Blessing, Acta Cryst. (1995) A51 33-38 ; _exptl_special_details ; It should be noted that the esd's of the cell dimensions are probably too low; they should be multiplied by a factor of 2 to 10 ; _diffrn_ambient_temperature 100(2) _diffrn_measurement_specimen_suppport 'magnetic support whith 10 micron nylon fiber cryoloop' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'rotating anode X-ray tube' _diffrn_source_type 'Bruker-Nonius FR 591' _diffrn_source_power 50 _diffrn_source_current 70 _diffrn_source_size '3 mm x 0.3 mm fine focus' _diffrn_radiation_monochromator 'Multilayer Montel 200 mirrors' _diffrn_detector_type '4K CCD area detector APEX II' _diffrn_measurement_device_type 'Kappa 4-axis goniometer bruker-nonius' _diffrn_measurement_method ; Fullsphere data collection, phi and omega scans ; _diffrn_detector_area_resol_mean 512 _diffrn_reflns_number 21869 _diffrn_reflns_av_R_equivalents 0.2768 _diffrn_reflns_av_sigmaI/netI 0.3525 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.48 _diffrn_reflns_theta_max 25.64 _reflns_number_total 6814 _reflns_number_gt 2641 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2 v2009.1-0' _computing_cell_refinement 'Bruker APEX2 v2009.1-0' _computing_data_reduction 'Bruker SAINT V7.60A' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXS-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.1015P)^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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6814 _refine_ls_number_parameters 482 _refine_ls_number_restraints 54 _refine_ls_R_factor_all 0.2536 _refine_ls_R_factor_gt 0.0915 _refine_ls_wR_factor_ref 0.2497 _refine_ls_wR_factor_gt 0.1844 _refine_ls_goodness_of_fit_ref 0.933 _refine_ls_restrained_S_all 0.931 _refine_ls_shift/su_max 0.015 _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 0.3700(7) 0.4193(4) 0.5800(4) 0.024(2) Uani 1 1 d . . . C2 C 0.3209(8) 0.4384(4) 0.6455(4) 0.029(2) Uani 1 1 d . . . C3 C 0.2517(8) 0.3947(4) 0.6896(5) 0.035(2) Uani 1 1 d . . . H3 H 0.2235 0.4085 0.7342 0.042 Uiso 1 1 calc R . . C4 C 0.2229(8) 0.3334(4) 0.6714(4) 0.028(2) Uani 1 1 d . . . C5 C 0.2647(8) 0.3165(4) 0.6046(5) 0.035(2) Uani 1 1 d . . . H5 H 0.2414 0.2751 0.5892 0.042 Uiso 1 1 calc R . . C6 C 0.3390(7) 0.3569(3) 0.5589(4) 0.023(2) Uani 1 1 d . . . C7 C 0.1615(9) 0.2845(4) 0.7209(5) 0.038(2) Uani 1 1 d . . . C8 C 0.0166(9) 0.2553(5) 0.6909(5) 0.053(3) Uani 1 1 d . . . H8A H -0.0161 0.2207 0.7206 0.079 Uiso 1 1 calc R . . H8B H 0.0357 0.2390 0.6445 0.079 Uiso 1 1 calc R . . H8C H -0.0624 0.2874 0.6883 0.079 Uiso 1 1 calc R . . C9 C 0.2789(10) 0.2291(5) 0.7288(6) 0.057(3) Uani 1 1 d . . . H9A H 0.3743 0.2458 0.7470 0.086 Uiso 1 1 calc R . . H9B H 0.2953 0.2098 0.6836 0.086 Uiso 1 1 calc R . . H9C H 0.2399 0.1974 0.7606 0.086 Uiso 1 1 calc R . . C10 C 0.1358(11) 0.3094(4) 0.7918(5) 0.052(3) Uani 1 1 d . . . H10A H 0.2311 0.3249 0.8115 0.079 Uiso 1 1 calc R . . H10B H 0.0965 0.2757 0.8210 0.079 Uiso 1 1 calc R . . H10C H 0.0629 0.3441 0.7895 0.079 Uiso 1 1 calc R . . C11 C 0.3481(8) 0.5003(4) 0.6757(4) 0.031(2) Uani 1 1 d . . . H11 H 0.3217 0.5052 0.7227 0.037 Uiso 1 1 calc R . . C12 C 0.2756(7) 0.7914(4) 0.4686(5) 0.034(2) Uani 1 1 d . . . C13 C 0.3477(8) 0.7562(4) 0.4173(5) 0.034(2) Uani 1 1 d . . . H13 H 0.4214 0.7759 0.3898 0.041 Uiso 1 1 calc R . . C14 C 0.3136(8) 0.6938(4) 0.4063(4) 0.033(2) Uani 1 1 d . . . H14 H 0.3625 0.6711 0.3708 0.039 Uiso 1 1 calc R . . C15 C 0.2076(8) 0.6639(4) 0.4470(4) 0.031(2) Uani 1 1 d . . . C16 C 0.1271(8) 0.6995(4) 0.4937(5) 0.034(2) Uani 1 1 d . . . H16 H 0.0457 0.6809 0.5175 0.041 Uiso 1 1 calc R . . C17 C 0.1635(8) 0.7613(4) 0.5060(4) 0.035(2) Uani 1 1 d . . . H17 H 0.1116 0.7840 0.5405 0.042 Uiso 1 1 calc R . . C18 C 0.2236(8) 0.9181(4) 0.4225(5) 0.034(2) Uani 1 1 d . . . C19 C 0.1858(8) 0.8967(4) 0.3590(5) 0.045(3) Uani 1 1 d . . . H19 H 0.2153 0.8553 0.3467 0.054 Uiso 1 1 calc R . . C20 C 0.1074(9) 0.9316(4) 0.3116(5) 0.046(3) Uani 1 1 d . . . H20 H 0.0830 0.9142 0.2678 0.055 Uiso 1 1 calc R . . C21 C 0.0640(9) 0.9915(5) 0.3271(5) 0.049(3) Uani 1 1 d . . . H21 H 0.0090 1.0160 0.2944 0.059 Uiso 1 1 calc R . . C22 C 0.1004(9) 1.0153(5) 0.3896(6) 0.053(3) Uani 1 1 d . . . H22 H 0.0716 1.0573 0.4002 0.063 Uiso 1 1 calc R . . C23 C 0.1803(9) 0.9798(4) 0.4399(5) 0.046(3) Uani 1 1 d . . . H23 H 0.2040 0.9971 0.4839 0.055 Uiso 1 1 calc R . . C24 C 0.5173(8) 0.8772(4) 0.4680(4) 0.030(2) Uani 1 1 d . . . C25 C 0.6183(8) 0.8493(4) 0.5130(5) 0.035(2) Uani 1 1 d . . . H25 H 0.5824 0.8298 0.5536 0.042 Uiso 1 1 calc R . . C26 C 0.7713(9) 0.8490(4) 0.5002(5) 0.048(3) Uani 1 1 d . . . H26 H 0.8393 0.8292 0.5316 0.058 Uiso 1 1 calc R . . C27 C 0.8239(9) 0.8774(4) 0.4421(6) 0.051(3) Uani 1 1 d . . . H27 H 0.9287 0.8774 0.4333 0.061 Uiso 1 1 calc R . . C28 C 0.7256(9) 0.9063(4) 0.3958(5) 0.046(3) Uani 1 1 d . . . H28 H 0.7625 0.9258 0.3553 0.056 Uiso 1 1 calc R . . C29 C 0.5703(8) 0.9063(4) 0.4093(4) 0.034(2) Uani 1 1 d . . . H29 H 0.5021 0.9264 0.3782 0.041 Uiso 1 1 calc R . . C31 C 0.4332(10) 0.6036(4) 0.6916(5) 0.039(2) Uani 1 1 d . . . H31A H 0.5422 0.6061 0.7024 0.047 Uiso 1 1 calc R . . H31B H 0.3793 0.5979 0.7355 0.047 Uiso 1 1 calc R . . C32 C 0.3821(9) 0.6637(4) 0.6575(5) 0.039(2) Uani 1 1 d . . . H32A H 0.3641 0.6955 0.6938 0.046 Uiso 1 1 calc R . . H32B H 0.2848 0.6558 0.6335 0.046 Uiso 1 1 calc R . . C33 C 0.4901(8) 0.6910(4) 0.6064(4) 0.032(2) Uani 1 1 d . . . H33A H 0.4479 0.7307 0.5877 0.039 Uiso 1 1 calc R . . H33B H 0.5861 0.7012 0.6305 0.039 Uiso 1 1 calc R . . C34 C 0.1750(8) 0.5944(4) 0.4346(5) 0.035(2) Uani 1 1 d . . . H34A H 0.0672 0.5887 0.4225 0.041 Uiso 1 1 calc R . . H34B H 0.2353 0.5790 0.3955 0.041 Uiso 1 1 calc R . . C35 C 0.3868(8) 0.3298(4) 0.4951(4) 0.029(2) Uani 1 1 d . . . H35 H 0.3445 0.2899 0.4838 0.035 Uiso 1 1 calc R . . C1A C 0.6387(10) 0.4154(4) 0.8205(5) 0.048(3) Uani 1 1 d . . . H1AS H 0.7115 0.4220 0.8596 0.057 Uiso 1 1 calc R . . Cl1A Cl 0.6966(2) 0.46109(12) 0.75125(13) 0.0539(7) Uani 1 1 d . . . Cl2A Cl 0.4591(2) 0.43950(13) 0.84759(13) 0.0537(7) Uani 1 1 d . . . Cl3A Cl 0.6375(4) 0.33502(13) 0.79976(18) 0.0911(11) Uani 1 1 d . . . N1 N 0.4036(7) 0.5490(3) 0.6462(3) 0.0320(18) Uani 1 1 d . . . N2 N 0.5204(6) 0.6477(3) 0.5490(3) 0.0285(18) Uani 1 1 d . . . N3 N 0.2131(6) 0.5573(3) 0.4979(4) 0.0343(19) Uani 1 1 d . . . H3A H 0.1912 0.5159 0.4882 0.041 Uiso 1 1 calc R . . H3B H 0.1476 0.5699 0.5315 0.041 Uiso 1 1 calc R . . O1 O 0.4409(5) 0.4599(2) 0.5390(3) 0.0280(14) Uani 1 1 d . . . Cl1S Cl 0.8907(2) 0.58625(11) 0.61760(13) 0.0452(6) Uani 1 1 d . . . O1S O 0.8780(11) 0.5689(5) 0.5486(4) 0.031(3) Uani 0.415(8) 1 d PDU A 1 O2S O 0.7984(11) 0.5624(6) 0.6645(6) 0.082(4) Uani 0.415(8) 1 d PDU A 1 O3S O 1.0474(8) 0.5802(5) 0.6408(5) 0.023(3) Uani 0.415(8) 1 d PDU A 1 O4S O 0.8611(12) 0.6595(4) 0.6164(6) 0.034(3) Uani 0.415(8) 1 d PDU A 1 O1S' O 0.8927(10) 0.5818(5) 0.5418(4) 0.039(3) Uani 0.585(8) 1 d PDU A 2 O2S' O 0.7601(8) 0.5488(4) 0.6401(5) 0.036(2) Uani 0.585(8) 1 d PDU A 2 O3S' O 1.0186(10) 0.5486(6) 0.6420(6) 0.072(3) Uani 0.585(8) 1 d PDU A 2 O4S' O 0.8823(12) 0.6462(4) 0.6395(6) 0.063(3) Uani 0.585(8) 1 d PDU A 2 P1 P 0.3176(2) 0.87349(11) 0.49012(14) 0.0374(6) Uani 1 1 d . . . Zn1 Zn 0.42765(9) 0.55917(4) 0.54171(5) 0.0269(2) 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 0.025(3) 0.027(4) 0.021(5) 0.010(4) -0.003(3) 0.007(3) C2 0.031(4) 0.026(4) 0.029(5) 0.008(4) 0.007(3) -0.008(4) C3 0.030(4) 0.035(5) 0.040(6) -0.002(5) 0.005(4) 0.001(4) C4 0.028(4) 0.025(4) 0.032(5) -0.001(4) -0.002(4) -0.002(3) C5 0.023(4) 0.022(4) 0.059(7) 0.004(5) -0.003(4) 0.002(3) C6 0.015(3) 0.024(4) 0.031(5) 0.000(4) 0.002(3) 0.004(3) C7 0.042(4) 0.022(4) 0.049(6) 0.004(5) 0.001(4) -0.010(4) C8 0.047(5) 0.053(6) 0.059(7) 0.014(6) -0.001(5) -0.021(5) C9 0.058(6) 0.046(6) 0.068(8) 0.025(6) 0.007(5) -0.003(5) C10 0.080(6) 0.041(6) 0.036(6) 0.001(5) 0.013(5) -0.012(5) C11 0.034(4) 0.031(4) 0.026(5) -0.013(4) 0.010(4) -0.009(4) C12 0.018(3) 0.035(5) 0.051(6) 0.011(5) 0.003(4) 0.001(3) C13 0.020(3) 0.040(5) 0.044(6) 0.009(5) 0.007(4) 0.005(3) C14 0.030(4) 0.034(5) 0.034(6) 0.011(4) 0.007(4) 0.005(4) C15 0.036(4) 0.021(4) 0.035(6) 0.015(4) -0.007(4) 0.009(4) C16 0.025(4) 0.033(5) 0.046(6) 0.005(5) 0.005(4) -0.004(4) C17 0.033(4) 0.042(5) 0.030(5) -0.004(5) 0.006(4) 0.002(4) C18 0.024(4) 0.036(5) 0.040(6) -0.007(5) 0.007(4) -0.010(4) C19 0.025(4) 0.041(5) 0.071(7) 0.013(6) 0.013(4) -0.004(4) C20 0.035(4) 0.044(6) 0.059(7) 0.006(5) 0.003(4) -0.017(4) C21 0.034(4) 0.060(7) 0.054(7) 0.017(6) -0.001(4) -0.010(5) C22 0.040(5) 0.033(5) 0.085(9) 0.021(6) -0.005(5) 0.004(4) C23 0.045(5) 0.029(5) 0.062(7) 0.005(5) 0.009(5) 0.003(4) C24 0.028(4) 0.023(4) 0.039(6) 0.002(4) -0.002(4) 0.000(3) C25 0.036(4) 0.032(5) 0.036(6) 0.000(5) 0.000(4) -0.005(4) C26 0.030(4) 0.042(6) 0.072(8) 0.000(6) -0.006(5) 0.008(4) C27 0.028(4) 0.038(5) 0.086(8) -0.014(6) 0.004(5) 0.006(4) C28 0.037(4) 0.040(5) 0.063(7) -0.018(5) 0.024(4) -0.012(4) C29 0.032(4) 0.037(5) 0.034(5) 0.000(5) 0.004(4) 0.009(4) C31 0.059(5) 0.025(4) 0.033(6) 0.008(5) 0.010(4) 0.002(4) C32 0.052(5) 0.033(5) 0.031(6) 0.001(5) 0.007(4) -0.001(4) C33 0.030(4) 0.025(4) 0.041(6) -0.007(4) 0.002(4) -0.007(3) C34 0.031(4) 0.024(4) 0.049(6) -0.003(5) -0.006(4) 0.000(4) C35 0.033(4) 0.026(4) 0.028(5) 0.007(4) -0.009(4) 0.008(4) C1A 0.055(5) 0.050(6) 0.039(6) 0.010(5) 0.004(5) 0.003(5) Cl1A 0.0470(12) 0.0646(16) 0.0504(16) 0.0102(14) 0.0080(11) -0.0163(11) Cl2A 0.0475(12) 0.0595(15) 0.0542(16) 0.0102(15) 0.0089(11) -0.0074(12) Cl3A 0.131(2) 0.0433(15) 0.101(3) -0.0023(17) 0.052(2) -0.0063(17) N1 0.039(3) 0.027(4) 0.030(4) -0.013(4) 0.010(3) -0.009(3) N2 0.023(3) 0.027(4) 0.035(4) 0.002(4) 0.004(3) -0.006(3) N3 0.023(3) 0.019(3) 0.061(5) -0.008(4) 0.010(3) 0.004(3) O1 0.021(2) 0.023(3) 0.040(3) -0.005(3) 0.013(2) -0.003(2) Cl1S 0.0274(10) 0.0549(14) 0.0535(16) 0.0018(13) 0.0101(10) 0.0029(10) O1S 0.032(4) 0.030(5) 0.030(5) 0.002(4) 0.001(3) -0.004(3) O2S 0.082(5) 0.083(6) 0.082(6) 0.003(4) 0.005(4) -0.005(4) O3S 0.019(4) 0.026(4) 0.023(4) 0.002(4) -0.004(3) 0.006(3) O4S 0.036(4) 0.030(5) 0.036(5) -0.002(4) 0.003(4) 0.001(3) O1S' 0.035(4) 0.040(4) 0.041(4) 0.005(3) 0.008(3) -0.009(3) O2S' 0.034(3) 0.038(4) 0.036(4) 0.008(3) 0.006(3) -0.009(3) O3S' 0.067(4) 0.075(5) 0.073(5) -0.002(4) -0.003(4) 0.005(4) O4S' 0.067(4) 0.061(5) 0.061(5) -0.003(4) 0.002(4) -0.001(4) P1 0.0261(10) 0.0305(12) 0.0558(17) 0.0044(13) 0.0103(10) 0.0010(9) Zn1 0.0220(4) 0.0218(4) 0.0372(6) -0.0015(5) 0.0074(4) -0.0003(4) _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(8) . ? C1 C2 1.409(11) . ? C1 C6 1.413(10) . ? C2 C3 1.408(11) . ? C2 C11 1.457(11) . ? C3 C4 1.371(11) . ? C4 C5 1.400(11) . ? C4 C7 1.521(11) . ? C5 C6 1.405(10) . ? C6 C35 1.435(11) . ? C7 C10 1.494(12) . ? C7 C8 1.536(12) . ? C7 C9 1.578(12) . ? C11 N1 1.283(10) . ? C12 C17 1.395(10) . ? C12 C13 1.406(11) . ? C12 P1 1.829(9) . ? C13 C14 1.374(11) . ? C14 C15 1.392(10) . ? C15 C16 1.388(11) . ? C15 C34 1.523(11) . ? C16 C17 1.370(12) . ? C18 C19 1.350(13) . ? C18 C23 1.408(12) . ? C18 P1 1.811(9) . ? C19 C20 1.362(13) . ? C20 C21 1.363(13) . ? C21 C22 1.348(14) . ? C22 C23 1.414(13) . ? C24 C25 1.376(11) . ? C24 C29 1.384(11) . ? C24 P1 1.834(7) . ? C25 C26 1.387(11) . ? C26 C27 1.366(13) . ? C27 C28 1.386(13) . ? C28 C29 1.409(10) . ? C31 N1 1.477(10) . ? C31 C32 1.505(12) . ? C32 C33 1.506(11) . ? C33 N2 1.472(10) . ? C34 N3 1.491(11) . ? C35 N2 1.288(9) 3_666 ? C1A Cl1A 1.740(9) . ? C1A Cl3A 1.753(10) . ? C1A Cl2A 1.764(9) . ? N1 Zn1 2.052(7) . ? N2 C35 1.288(9) 3_666 ? N2 Zn1 2.056(6) . ? N3 Zn1 2.077(6) . ? O1 Zn1 2.008(5) 3_666 ? O1 Zn1 2.110(5) . ? Cl1S O2S 1.334(9) . ? Cl1S O4S' 1.343(9) . ? Cl1S O1S 1.391(8) . ? Cl1S O3S 1.463(8) . ? Cl1S O3S' 1.463(9) . ? Cl1S O1S' 1.474(8) . ? Cl1S O2S' 1.479(7) . ? Cl1S O4S 1.577(9) . ? Zn1 O1 2.008(5) 3_666 ? 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 120.5(7) . . ? O1 C1 C6 121.6(7) . . ? C2 C1 C6 117.9(7) . . ? C3 C2 C1 120.2(7) . . ? C3 C2 C11 114.9(7) . . ? C1 C2 C11 124.6(7) . . ? C4 C3 C2 123.3(8) . . ? C3 C4 C5 115.5(7) . . ? C3 C4 C7 123.6(8) . . ? C5 C4 C7 120.7(7) . . ? C4 C5 C6 124.1(7) . . ? C5 C6 C1 118.8(7) . . ? C5 C6 C35 116.6(7) . . ? C1 C6 C35 124.5(7) . . ? C10 C7 C4 113.6(7) . . ? C10 C7 C8 110.7(7) . . ? C4 C7 C8 110.1(7) . . ? C10 C7 C9 106.6(8) . . ? C4 C7 C9 109.1(6) . . ? C8 C7 C9 106.6(7) . . ? N1 C11 C2 127.6(7) . . ? C17 C12 C13 117.4(8) . . ? C17 C12 P1 117.6(6) . . ? C13 C12 P1 125.0(6) . . ? C14 C13 C12 121.4(7) . . ? C13 C14 C15 120.0(7) . . ? C16 C15 C14 118.9(7) . . ? C16 C15 C34 122.2(7) . . ? C14 C15 C34 118.8(7) . . ? C17 C16 C15 120.8(7) . . ? C16 C17 C12 121.1(8) . . ? C19 C18 C23 117.8(9) . . ? C19 C18 P1 126.2(7) . . ? C23 C18 P1 116.0(7) . . ? C18 C19 C20 123.3(9) . . ? C19 C20 C21 120.1(10) . . ? C22 C21 C20 118.9(10) . . ? C21 C22 C23 122.0(9) . . ? C18 C23 C22 117.9(10) . . ? C25 C24 C29 119.1(7) . . ? C25 C24 P1 117.2(6) . . ? C29 C24 P1 123.7(6) . . ? C24 C25 C26 121.4(8) . . ? C27 C26 C25 119.6(9) . . ? C26 C27 C28 120.6(8) . . ? C27 C28 C29 119.3(8) . . ? C24 C29 C28 120.0(8) . . ? N1 C31 C32 110.7(7) . . ? C31 C32 C33 115.1(7) . . ? N2 C33 C32 112.6(6) . . ? N3 C34 C15 109.9(7) . . ? N2 C35 C6 128.6(7) 3_666 . ? Cl1A C1A Cl3A 111.5(5) . . ? Cl1A C1A Cl2A 110.4(5) . . ? Cl3A C1A Cl2A 110.4(5) . . ? C11 N1 C31 115.6(7) . . ? C11 N1 Zn1 124.9(6) . . ? C31 N1 Zn1 119.1(5) . . ? C35 N2 C33 113.4(6) 3_666 . ? C35 N2 Zn1 123.6(5) 3_666 . ? C33 N2 Zn1 123.0(5) . . ? C34 N3 Zn1 121.5(4) . . ? C1 O1 Zn1 128.2(4) . 3_666 ? C1 O1 Zn1 127.0(4) . . ? Zn1 O1 Zn1 104.7(2) 3_666 . ? O2S Cl1S O4S' 96.1(8) . . ? O2S Cl1S O1S 120.9(7) . . ? O4S' Cl1S O1S 123.4(7) . . ? O2S Cl1S O3S 110.5(6) . . ? O4S' Cl1S O3S 92.5(7) . . ? O1S Cl1S O3S 109.6(5) . . ? O2S Cl1S O3S' 93.2(7) . . ? O4S' Cl1S O3S' 117.5(7) . . ? O1S Cl1S O3S' 102.6(7) . . ? O3S Cl1S O3S' 28.4(5) . . ? O2S Cl1S O1S' 132.3(7) . . ? O4S' Cl1S O1S' 112.2(6) . . ? O1S Cl1S O1S' 12.9(6) . . ? O3S Cl1S O1S' 105.9(6) . . ? O3S' Cl1S O1S' 105.4(5) . . ? O2S Cl1S O2S' 26.0(6) . . ? O4S' Cl1S O2S' 111.6(5) . . ? O1S Cl1S O2S' 95.1(6) . . ? O3S Cl1S O2S' 127.6(6) . . ? O3S' Cl1S O2S' 102.7(6) . . ? O1S' Cl1S O2S' 106.4(5) . . ? O2S Cl1S O4S 106.2(6) . . ? O4S' Cl1S O4S 20.1(6) . . ? O1S Cl1S O4S 103.7(6) . . ? O3S Cl1S O4S 104.4(6) . . ? O3S' Cl1S O4S 132.2(7) . . ? O1S' Cl1S O4S 93.1(7) . . ? O2S' Cl1S O4S 113.8(5) . . ? C18 P1 C12 104.0(4) . . ? C18 P1 C24 104.2(4) . . ? C12 P1 C24 100.5(3) . . ? O1 Zn1 N1 144.9(2) 3_666 . ? O1 Zn1 N2 90.0(2) 3_666 . ? N1 Zn1 N2 94.4(3) . . ? O1 Zn1 N3 102.6(2) 3_666 . ? N1 Zn1 N3 107.1(3) . . ? N2 Zn1 N3 114.2(3) . . ? O1 Zn1 O1 75.3(2) 3_666 . ? N1 Zn1 O1 85.8(2) . . ? N2 Zn1 O1 153.1(2) . . ? N3 Zn1 O1 91.3(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 C1 C2 C3 -177.5(7) . . . . ? C6 C1 C2 C3 3.9(10) . . . . ? O1 C1 C2 C11 -3.4(11) . . . . ? C6 C1 C2 C11 177.9(7) . . . . ? C1 C2 C3 C4 -2.6(12) . . . . ? C11 C2 C3 C4 -177.2(7) . . . . ? C2 C3 C4 C5 -1.1(11) . . . . ? C2 C3 C4 C7 174.2(7) . . . . ? C3 C4 C5 C6 3.5(11) . . . . ? C7 C4 C5 C6 -171.9(7) . . . . ? C4 C5 C6 C1 -2.1(11) . . . . ? C4 C5 C6 C35 173.9(7) . . . . ? O1 C1 C6 C5 179.7(6) . . . . ? C2 C1 C6 C5 -1.7(10) . . . . ? O1 C1 C6 C35 4.1(11) . . . . ? C2 C1 C6 C35 -177.4(7) . . . . ? C3 C4 C7 C10 -0.3(11) . . . . ? C5 C4 C7 C10 174.7(7) . . . . ? C3 C4 C7 C8 124.5(8) . . . . ? C5 C4 C7 C8 -60.5(10) . . . . ? C3 C4 C7 C9 -118.9(9) . . . . ? C5 C4 C7 C9 56.1(10) . . . . ? C3 C2 C11 N1 -177.0(8) . . . . ? C1 C2 C11 N1 8.7(13) . . . . ? C17 C12 C13 C14 -2.6(12) . . . . ? P1 C12 C13 C14 177.3(7) . . . . ? C12 C13 C14 C15 -1.1(13) . . . . ? C13 C14 C15 C16 6.4(12) . . . . ? C13 C14 C15 C34 -178.6(8) . . . . ? C14 C15 C16 C17 -8.1(13) . . . . ? C34 C15 C16 C17 177.1(8) . . . . ? C15 C16 C17 C12 4.4(13) . . . . ? C13 C12 C17 C16 1.0(13) . . . . ? P1 C12 C17 C16 -179.0(7) . . . . ? C23 C18 C19 C20 -0.5(11) . . . . ? P1 C18 C19 C20 176.2(6) . . . . ? C18 C19 C20 C21 0.5(12) . . . . ? C19 C20 C21 C22 0.3(12) . . . . ? C20 C21 C22 C23 -0.9(13) . . . . ? C19 C18 C23 C22 -0.1(11) . . . . ? P1 C18 C23 C22 -177.2(6) . . . . ? C21 C22 C23 C18 0.9(12) . . . . ? C29 C24 C25 C26 -1.0(13) . . . . ? P1 C24 C25 C26 179.2(7) . . . . ? C24 C25 C26 C27 0.6(14) . . . . ? C25 C26 C27 C28 -0.2(14) . . . . ? C26 C27 C28 C29 0.3(14) . . . . ? C25 C24 C29 C28 1.1(12) . . . . ? P1 C24 C29 C28 -179.2(6) . . . . ? C27 C28 C29 C24 -0.7(13) . . . . ? N1 C31 C32 C33 -81.0(9) . . . . ? C31 C32 C33 N2 60.0(10) . . . . ? C16 C15 C34 N3 -66.4(9) . . . . ? C14 C15 C34 N3 118.7(8) . . . . ? C5 C6 C35 N2 -165.7(8) . . . 3_666 ? C1 C6 C35 N2 10.1(13) . . . 3_666 ? C2 C11 N1 C31 -173.8(7) . . . . ? C2 C11 N1 Zn1 14.1(11) . . . . ? C32 C31 N1 C11 -136.4(7) . . . . ? C32 C31 N1 Zn1 36.1(8) . . . . ? C32 C33 N2 C35 -179.7(7) . . . 3_666 ? C32 C33 N2 Zn1 -1.3(9) . . . . ? C15 C34 N3 Zn1 -57.4(7) . . . . ? C2 C1 O1 Zn1 160.6(5) . . . 3_666 ? C6 C1 O1 Zn1 -20.9(9) . . . 3_666 ? C2 C1 O1 Zn1 -23.4(9) . . . . ? C6 C1 O1 Zn1 155.2(5) . . . . ? C19 C18 P1 C12 -23.4(7) . . . . ? C23 C18 P1 C12 153.3(6) . . . . ? C19 C18 P1 C24 81.5(7) . . . . ? C23 C18 P1 C24 -101.8(6) . . . . ? C17 C12 P1 C18 -101.9(7) . . . . ? C13 C12 P1 C18 78.1(8) . . . . ? C17 C12 P1 C24 150.4(7) . . . . ? C13 C12 P1 C24 -29.5(8) . . . . ? C25 C24 P1 C18 177.0(7) . . . . ? C29 C24 P1 C18 -2.8(8) . . . . ? C25 C24 P1 C12 -75.5(7) . . . . ? C29 C24 P1 C12 104.8(8) . . . . ? C11 N1 Zn1 O1 -83.8(7) . . . 3_666 ? C31 N1 Zn1 O1 104.4(6) . . . 3_666 ? C11 N1 Zn1 N2 179.9(6) . . . . ? C31 N1 Zn1 N2 8.1(6) . . . . ? C11 N1 Zn1 N3 62.9(7) . . . . ? C31 N1 Zn1 N3 -108.9(6) . . . . ? C11 N1 Zn1 O1 -27.1(6) . . . . ? C31 N1 Zn1 O1 161.1(6) . . . . ? C35 N2 Zn1 O1 6.2(6) 3_666 . . 3_666 ? C33 N2 Zn1 O1 -172.0(6) . . . 3_666 ? C35 N2 Zn1 N1 151.4(6) 3_666 . . . ? C33 N2 Zn1 N1 -26.9(6) . . . . ? C35 N2 Zn1 N3 -97.7(6) 3_666 . . . ? C33 N2 Zn1 N3 84.1(6) . . . . ? C35 N2 Zn1 O1 62.0(9) 3_666 . . . ? C33 N2 Zn1 O1 -116.2(6) . . . . ? C34 N3 Zn1 O1 -51.2(6) . . . 3_666 ? C34 N3 Zn1 N1 147.6(5) . . . . ? C34 N3 Zn1 N2 44.6(6) . . . . ? C34 N3 Zn1 O1 -126.4(6) . . . . ? C1 O1 Zn1 O1 -176.8(7) . . . 3_666 ? Zn1 O1 Zn1 O1 0.0 3_666 . . 3_666 ? C1 O1 Zn1 N1 33.0(6) . . . . ? Zn1 O1 Zn1 N1 -150.2(3) 3_666 . . . ? C1 O1 Zn1 N2 124.4(6) . . . . ? Zn1 O1 Zn1 N2 -58.8(6) 3_666 . . . ? C1 O1 Zn1 N3 -74.0(6) . . . . ? Zn1 O1 Zn1 N3 102.8(3) 3_666 . . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 25.64 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 1.537 _refine_diff_density_min -0.907 _refine_diff_density_rms 0.133