# Electronic Supplementary Material (ESI) for Catalysis Science & Technology # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full Cat.Sci.Tech. _journal_coden_cambridge 1486 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email akleij@iciq.es _publ_contact_author_name 'Dr Arjan Kleij' _publ_section_title ; A highly active Zn(salphen) catalyst for production of organic carbonates in a green CO2 medium ; loop_ _publ_author_name A.Kleij M.Taherimehr P.Pescarmona W.Lueangchaichaweng ; S.Al-Amsyar ; A.Decortes C.Whiteoak E.Escudero # Attachment '- AWK644_0mX.cif' data_awk644_0m _database_code_depnum_ccdc_archive 'CCDC 855909' #TrackingRef '- AWK644_0mX.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H54 N2 O3 Zn' _chemical_formula_weight 676.22 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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.9698(5) _cell_length_b 12.9718(6) _cell_length_c 13.3427(7) _cell_angle_alpha 91.834(3) _cell_angle_beta 104.278(3) _cell_angle_gamma 92.660(3) _cell_volume 1836.16(15) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9247 _cell_measurement_theta_min 2.69 _cell_measurement_theta_max 37.03 _exptl_crystal_description Block _exptl_crystal_colour orange _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.223 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 724 _exptl_absorpt_coefficient_mu 0.707 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 1.0 _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 48868 _diffrn_reflns_av_R_equivalents 0.0579 _diffrn_reflns_av_sigmaI/netI 0.0477 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.92 _diffrn_reflns_theta_max 37.15 _reflns_number_total 17091 _reflns_number_gt 13539 _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^)+(0.0675P)^2^+0.4392P] 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 17091 _refine_ls_number_parameters 446 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0597 _refine_ls_R_factor_gt 0.0431 _refine_ls_wR_factor_ref 0.1279 _refine_ls_wR_factor_gt 0.1182 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.043 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.77575(10) 0.72138(8) 0.25052(9) 0.01645(17) Uani 1 1 d . . . C2 C 0.82463(10) 0.80630(7) 0.32398(9) 0.01609(17) Uani 1 1 d . . . C3 C 0.87149(10) 0.78513(8) 0.42653(9) 0.01705(18) Uani 1 1 d . . . H3 H 0.9084 0.8412 0.4734 0.020 Uiso 1 1 calc R . . C4 C 0.86840(10) 0.68527(8) 0.46707(9) 0.01625(17) Uani 1 1 d . . . C5 C 0.81507(10) 0.60564(8) 0.39767(9) 0.01685(18) Uani 1 1 d . . . H5 H 0.8077 0.5384 0.4225 0.020 Uiso 1 1 calc R . . C6 C 0.77059(10) 0.62014(8) 0.29015(9) 0.01643(17) Uani 1 1 d . . . C7 C 0.72631(11) 0.52794(8) 0.22671(9) 0.01744(18) Uani 1 1 d . . . H7 H 0.7186 0.4661 0.2615 0.021 Uiso 1 1 calc R . . C8 C 0.82277(11) 0.91740(8) 0.28671(9) 0.01917(19) Uani 1 1 d . . . C9 C 0.68611(12) 0.94396(9) 0.23953(11) 0.0249(2) Uani 1 1 d . . . H9A H 0.6376 0.9383 0.2919 0.037 Uiso 1 1 calc R . . H9B H 0.6486 0.8958 0.1807 0.037 Uiso 1 1 calc R . . H9C H 0.6849 1.0147 0.2158 0.037 Uiso 1 1 calc R . . C10 C 0.90015(14) 0.93136(10) 0.20604(12) 0.0276(3) Uani 1 1 d . . . H10A H 0.8979 1.0030 0.1848 0.041 Uiso 1 1 calc R . . H10B H 0.8644 0.8848 0.1455 0.041 Uiso 1 1 calc R . . H10C H 0.9876 0.9151 0.2363 0.041 Uiso 1 1 calc R . . C11 C 0.87807(15) 0.99644(9) 0.37602(11) 0.0303(3) Uani 1 1 d . . . H11A H 0.8712 1.0663 0.3501 0.046 Uiso 1 1 calc R . . H11B H 0.9669 0.9840 0.4055 0.046 Uiso 1 1 calc R . . H11C H 0.8315 0.9895 0.4296 0.046 Uiso 1 1 calc R . . C12 C 0.92540(11) 0.67174(8) 0.58223(9) 0.01871(19) Uani 1 1 d . . . C13 C 1.06924(12) 0.69131(10) 0.60494(11) 0.0254(2) Uani 1 1 d . . . H13A H 1.1041 0.6390 0.5670 0.038 Uiso 1 1 calc R . . H13B H 1.1062 0.6872 0.6794 0.038 Uiso 1 1 calc R . . H13C H 1.0889 0.7601 0.5829 0.038 Uiso 1 1 calc R . . C14 C 0.87312(13) 0.74935(11) 0.64831(11) 0.0263(2) Uani 1 1 d . . . H14A H 0.8922 0.8198 0.6300 0.040 Uiso 1 1 calc R . . H14B H 0.9122 0.7410 0.7218 0.040 Uiso 1 1 calc R . . H14C H 0.7817 0.7367 0.6352 0.040 Uiso 1 1 calc R . . C15 C 0.89769(15) 0.56273(10) 0.61483(11) 0.0296(3) Uani 1 1 d . . . H15A H 0.8064 0.5491 0.6020 0.044 Uiso 1 1 calc R . . H15B H 0.9369 0.5572 0.6887 0.044 Uiso 1 1 calc R . . H15C H 0.9320 0.5121 0.5746 0.044 Uiso 1 1 calc R . . C16 C 0.65680(10) 0.42711(8) 0.06846(9) 0.01720(18) Uani 1 1 d . . . C17 C 0.64399(12) 0.33125(8) 0.11134(10) 0.0205(2) Uani 1 1 d . . . H17 H 0.6616 0.3267 0.1844 0.025 Uiso 1 1 calc R . . C18 C 0.60566(12) 0.24286(8) 0.04774(11) 0.0238(2) Uani 1 1 d . . . H18 H 0.5971 0.1781 0.0774 0.029 Uiso 1 1 calc R . . C19 C 0.57982(13) 0.24898(9) -0.05923(11) 0.0268(3) Uani 1 1 d . . . H19 H 0.5537 0.1883 -0.1024 0.032 Uiso 1 1 calc R . . C20 C 0.59188(13) 0.34325(9) -0.10351(11) 0.0245(2) Uani 1 1 d . . . H20 H 0.5747 0.3466 -0.1766 0.029 Uiso 1 1 calc R . . C21 C 0.62936(11) 0.43345(8) -0.04042(9) 0.01868(19) Uani 1 1 d . . . C22 C 0.59807(11) 0.55270(8) -0.17447(9) 0.01851(19) Uani 1 1 d . . . H22 H 0.5587 0.4962 -0.2198 0.022 Uiso 1 1 calc R . . C23 C 0.60053(11) 0.65146(8) -0.21948(9) 0.01790(18) Uani 1 1 d . . . C24 C 0.53529(11) 0.65438(8) -0.32543(9) 0.01870(19) Uani 1 1 d . . . H24 H 0.4998 0.5916 -0.3619 0.022 Uiso 1 1 calc R . . C25 C 0.52179(11) 0.74467(9) -0.37699(9) 0.01834(18) Uani 1 1 d . . . C26 C 0.57766(11) 0.83598(8) -0.31909(9) 0.01874(19) Uani 1 1 d . . . H26 H 0.5688 0.8992 -0.3535 0.022 Uiso 1 1 calc R . . C27 C 0.64389(11) 0.83959(8) -0.21652(9) 0.01766(18) Uani 1 1 d . . . C28 C 0.65656(11) 0.74445(8) -0.16229(9) 0.01746(18) Uani 1 1 d . . . C29 C 0.45208(11) 0.75128(9) -0.49101(10) 0.0217(2) Uani 1 1 d . . . C30 C 0.34514(14) 0.82586(13) -0.50023(13) 0.0324(3) Uani 1 1 d . . . H30A H 0.2976 0.8270 -0.5727 0.049 Uiso 1 1 calc R . . H30B H 0.3810 0.8955 -0.4760 0.049 Uiso 1 1 calc R . . H30C H 0.2887 0.8026 -0.4578 0.049 Uiso 1 1 calc R . . C31 C 0.54287(14) 0.79206(13) -0.55368(11) 0.0307(3) Uani 1 1 d . . . H31A H 0.6104 0.7443 -0.5500 0.046 Uiso 1 1 calc R . . H31B H 0.5794 0.8603 -0.5250 0.046 Uiso 1 1 calc R . . H31C H 0.4968 0.7976 -0.6261 0.046 Uiso 1 1 calc R . . C32 C 0.39454(17) 0.64611(12) -0.53878(12) 0.0375(4) Uani 1 1 d . . . H32A H 0.4616 0.5980 -0.5354 0.056 Uiso 1 1 calc R . . H32B H 0.3499 0.6535 -0.6112 0.056 Uiso 1 1 calc R . . H32C H 0.3352 0.6194 -0.5004 0.056 Uiso 1 1 calc R . . C33 C 0.70428(11) 0.94089(8) -0.15879(9) 0.01948(19) Uani 1 1 d . . . C34 C 0.68732(14) 1.03213(9) -0.23088(11) 0.0273(3) Uani 1 1 d . . . H34A H 0.5973 1.0413 -0.2586 0.041 Uiso 1 1 calc R . . H34B H 0.7264 1.0180 -0.2881 0.041 Uiso 1 1 calc R . . H34C H 0.7275 1.0952 -0.1919 0.041 Uiso 1 1 calc R . . C35 C 0.84715(12) 0.93253(10) -0.11532(12) 0.0259(2) Uani 1 1 d . . . H35A H 0.8851 0.9995 -0.0839 0.039 Uiso 1 1 calc R . . H35B H 0.8854 0.9125 -0.1716 0.039 Uiso 1 1 calc R . . H35C H 0.8618 0.8803 -0.0629 0.039 Uiso 1 1 calc R . . C36 C 0.64307(13) 0.96669(9) -0.06952(10) 0.0236(2) Uani 1 1 d . . . H36A H 0.5538 0.9785 -0.0978 0.035 Uiso 1 1 calc R . . H36B H 0.6857 1.0291 -0.0308 0.035 Uiso 1 1 calc R . . H36C H 0.6508 0.9089 -0.0232 0.035 Uiso 1 1 calc R . . C37 C 1.0199(3) 0.6580(2) -0.07684(18) 0.0598(6) Uani 1 1 d . . . H37D H 1.0665 0.7127 -0.1033 0.090 Uiso 0.346(5) 1 calc PR A 2 H37E H 0.9380 0.6424 -0.1258 0.090 Uiso 0.346(5) 1 calc PR A 2 H37F H 1.0682 0.5957 -0.0685 0.090 Uiso 0.346(5) 1 calc PR A 2 H37A H 1.0350 0.6010 -0.1215 0.090 Uiso 0.654(5) 1 calc PR A 1 H37B H 1.0783 0.7170 -0.0786 0.090 Uiso 0.654(5) 1 calc PR A 1 H37C H 0.9330 0.6783 -0.1016 0.090 Uiso 0.654(5) 1 calc PR A 1 C38 C 1.04026(19) 0.62396(16) 0.03131(18) 0.0262(5) Uani 0.654(5) 1 d P A 1 H38B H 1.1026 0.5697 0.0510 0.031 Uiso 0.654(5) 1 calc PR A 1 C39 C 1.02486(18) 0.69251(14) 0.11771(16) 0.0201(4) Uani 0.654(5) 1 d P A 1 H39B H 1.0036 0.7649 0.0997 0.024 Uiso 0.654(5) 1 calc PR A 1 C40 C 1.0987(2) 0.67962(17) 0.22416(17) 0.0508(5) Uani 1 1 d . . . H40D H 1.1296 0.6263 0.2731 0.076 Uiso 0.346(5) 1 calc PR A 2 H40E H 1.0287 0.7126 0.2436 0.076 Uiso 0.346(5) 1 calc PR A 2 H40F H 1.1669 0.7317 0.2258 0.076 Uiso 0.346(5) 1 calc PR A 2 H40A H 1.0765 0.7314 0.2707 0.076 Uiso 0.654(5) 1 calc PR A 1 H40B H 1.1887 0.6885 0.2271 0.076 Uiso 0.654(5) 1 calc PR A 1 H40C H 1.0800 0.6103 0.2456 0.076 Uiso 0.654(5) 1 calc PR A 1 C38' C 1.0016(5) 0.6908(4) 0.0188(5) 0.0409(14) Uani 0.346(5) 1 d P A 2 H38A H 0.9874 0.7656 0.0291 0.049 Uiso 0.346(5) 1 calc PR A 2 C39' C 1.0532(7) 0.6304(8) 0.1155(6) 0.069(3) Uani 0.346(5) 1 d P A 2 H39A H 1.1058 0.5729 0.1024 0.082 Uiso 0.346(5) 1 calc PR A 2 N1 N 0.69575(9) 0.52120(7) 0.12589(8) 0.01727(16) Uani 1 1 d . . . N2 N 0.64417(10) 0.53243(7) -0.07794(8) 0.01948(17) Uani 1 1 d . . . O1 O 0.73920(9) 0.73943(6) 0.15312(7) 0.02166(16) Uani 1 1 d . . . O2 O 0.71638(9) 0.74668(6) -0.06543(7) 0.02246(17) Uani 1 1 d . . . O3 O 0.92825(10) 0.61142(9) 0.06919(11) 0.0372(3) Uani 1 1 d . . . Zn1 Zn 0.726199(13) 0.642141(9) 0.036597(10) 0.01820(4) Uani 1 1 d . A . 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 0.0223(4) 0.0117(4) 0.0148(5) -0.0010(3) 0.0041(4) -0.0020(3) C2 0.0206(4) 0.0114(4) 0.0153(5) -0.0017(3) 0.0036(3) -0.0023(3) C3 0.0205(4) 0.0136(4) 0.0160(5) -0.0026(3) 0.0035(4) -0.0019(3) C4 0.0194(4) 0.0149(4) 0.0141(4) -0.0005(3) 0.0040(3) -0.0005(3) C5 0.0214(4) 0.0131(4) 0.0156(5) 0.0003(3) 0.0041(4) -0.0010(3) C6 0.0218(4) 0.0115(4) 0.0152(5) -0.0007(3) 0.0039(4) -0.0021(3) C7 0.0231(5) 0.0115(4) 0.0165(5) 0.0002(3) 0.0032(4) -0.0017(3) C8 0.0261(5) 0.0116(4) 0.0179(5) -0.0011(3) 0.0029(4) -0.0033(3) C9 0.0292(6) 0.0168(4) 0.0268(6) 0.0019(4) 0.0030(5) 0.0015(4) C10 0.0342(6) 0.0196(5) 0.0310(7) 0.0039(4) 0.0124(5) -0.0057(4) C11 0.0467(8) 0.0137(4) 0.0242(6) -0.0035(4) -0.0018(5) -0.0049(4) C12 0.0229(5) 0.0173(4) 0.0146(5) -0.0008(3) 0.0026(4) 0.0000(3) C13 0.0226(5) 0.0232(5) 0.0272(6) -0.0026(4) 0.0005(4) 0.0028(4) C14 0.0319(6) 0.0302(6) 0.0172(5) -0.0031(4) 0.0066(5) 0.0055(5) C15 0.0448(7) 0.0231(5) 0.0176(6) 0.0035(4) 0.0028(5) -0.0072(5) C16 0.0220(4) 0.0104(3) 0.0180(5) -0.0015(3) 0.0036(4) -0.0025(3) C17 0.0274(5) 0.0119(4) 0.0213(5) 0.0003(3) 0.0051(4) -0.0029(3) C18 0.0310(6) 0.0116(4) 0.0263(6) -0.0006(4) 0.0037(5) -0.0041(4) C19 0.0368(6) 0.0116(4) 0.0269(6) -0.0036(4) -0.0001(5) -0.0037(4) C20 0.0364(6) 0.0130(4) 0.0194(5) -0.0034(4) -0.0010(4) -0.0030(4) C21 0.0249(5) 0.0112(4) 0.0176(5) -0.0013(3) 0.0016(4) -0.0019(3) C22 0.0249(5) 0.0134(4) 0.0158(5) -0.0024(3) 0.0033(4) -0.0020(3) C23 0.0249(5) 0.0136(4) 0.0145(5) -0.0008(3) 0.0043(4) -0.0023(3) C24 0.0233(5) 0.0171(4) 0.0148(5) -0.0011(3) 0.0041(4) -0.0030(3) C25 0.0207(4) 0.0194(4) 0.0150(5) 0.0017(3) 0.0049(4) -0.0014(3) C26 0.0226(5) 0.0175(4) 0.0169(5) 0.0024(3) 0.0066(4) -0.0007(3) C27 0.0233(5) 0.0143(4) 0.0163(5) 0.0005(3) 0.0074(4) -0.0027(3) C28 0.0235(5) 0.0139(4) 0.0148(5) -0.0003(3) 0.0052(4) -0.0023(3) C29 0.0228(5) 0.0237(5) 0.0172(5) 0.0032(4) 0.0024(4) -0.0018(4) C30 0.0257(6) 0.0407(7) 0.0295(7) 0.0073(6) 0.0031(5) 0.0058(5) C31 0.0286(6) 0.0463(8) 0.0183(6) 0.0075(5) 0.0074(5) 0.0009(5) C32 0.0513(9) 0.0294(6) 0.0218(7) 0.0015(5) -0.0083(6) -0.0079(6) C33 0.0271(5) 0.0132(4) 0.0180(5) 0.0012(3) 0.0065(4) -0.0046(3) C34 0.0399(7) 0.0167(4) 0.0244(6) 0.0048(4) 0.0071(5) -0.0063(4) C35 0.0261(5) 0.0215(5) 0.0287(7) 0.0002(4) 0.0058(5) -0.0067(4) C36 0.0342(6) 0.0156(4) 0.0225(6) -0.0024(4) 0.0110(5) -0.0027(4) C37 0.0861(17) 0.0647(14) 0.0363(11) 0.0118(10) 0.0248(11) 0.0246(12) C38 0.0249(9) 0.0281(9) 0.0267(11) 0.0040(7) 0.0071(7) 0.0068(7) C39 0.0217(8) 0.0152(7) 0.0220(9) 0.0001(6) 0.0028(6) 0.0004(5) C40 0.0559(11) 0.0520(11) 0.0384(11) 0.0082(8) 0.0002(8) -0.0001(9) C38' 0.035(2) 0.046(3) 0.050(3) 0.023(2) 0.022(2) 0.0088(18) C39' 0.042(3) 0.107(7) 0.054(5) 0.015(4) 0.005(3) 0.003(4) N1 0.0243(4) 0.0106(3) 0.0158(4) -0.0020(3) 0.0039(3) -0.0025(3) N2 0.0294(5) 0.0110(3) 0.0157(4) -0.0009(3) 0.0019(3) -0.0025(3) O1 0.0368(5) 0.0128(3) 0.0136(4) -0.0007(3) 0.0039(3) -0.0025(3) O2 0.0343(4) 0.0148(3) 0.0152(4) 0.0006(3) 0.0015(3) -0.0054(3) O3 0.0291(5) 0.0298(5) 0.0538(8) -0.0083(5) 0.0148(5) -0.0055(4) Zn1 0.02854(7) 0.01087(6) 0.01343(6) -0.00106(4) 0.00305(5) -0.00440(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 1.2945(14) . ? C1 C6 1.4353(14) . ? C1 C2 1.4417(15) . ? C2 C3 1.3792(16) . ? C2 C8 1.5389(15) . ? C3 C4 1.4218(15) . ? C4 C5 1.3719(15) . ? C4 C12 1.5285(16) . ? C5 C6 1.4185(16) . ? C6 C7 1.4356(15) . ? C7 N1 1.3027(15) . ? C8 C11 1.5319(17) . ? C8 C10 1.5364(18) . ? C8 C9 1.5358(18) . ? C12 C15 1.5317(17) . ? C12 C14 1.5382(17) . ? C12 C13 1.5389(17) . ? C16 C17 1.4008(15) . ? C16 N1 1.4106(14) . ? C16 C21 1.4149(17) . ? C17 C18 1.3887(16) . ? C18 C19 1.391(2) . ? C19 C20 1.3899(17) . ? C20 C21 1.4029(15) . ? C21 N2 1.4097(14) . ? C22 N2 1.3026(16) . ? C22 C23 1.4340(15) . ? C23 C24 1.4210(16) . ? C23 C28 1.4339(15) . ? C24 C25 1.3727(16) . ? C25 C26 1.4199(16) . ? C25 C29 1.5320(17) . ? C26 C27 1.3802(17) . ? C27 C28 1.4455(15) . ? C27 C33 1.5368(15) . ? C28 O2 1.2958(15) . ? C29 C32 1.5271(19) . ? C29 C31 1.5365(18) . ? C29 C30 1.5392(19) . ? C33 C34 1.5380(16) . ? C33 C36 1.5399(18) . ? C33 C35 1.5413(18) . ? C37 C38' 1.397(6) . ? C37 C38 1.489(3) . ? C38 O3 1.444(2) . ? C38 C39 1.481(3) . ? C39 C40 1.470(3) . ? C39 O3 1.471(2) . ? C40 C39' 1.521(9) . ? C38' C39' 1.532(10) . ? C38' O3 1.547(5) . ? C39' O3 1.365(7) . ? N1 Zn1 2.0638(9) . ? N2 Zn1 2.0577(10) . ? O1 Zn1 1.9438(9) . ? O2 Zn1 1.9399(9) . ? O3 Zn1 2.2086(11) . ? 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 123.30(9) . . ? O1 C1 C2 119.15(9) . . ? C6 C1 C2 117.55(10) . . ? C3 C2 C1 118.54(9) . . ? C3 C2 C8 121.82(9) . . ? C1 C2 C8 119.65(10) . . ? C2 C3 C4 124.59(10) . . ? C5 C4 C3 116.49(10) . . ? C5 C4 C12 123.98(9) . . ? C3 C4 C12 119.52(9) . . ? C4 C5 C6 122.34(9) . . ? C5 C6 C1 120.30(9) . . ? C5 C6 C7 115.60(9) . . ? C1 C6 C7 124.06(10) . . ? N1 C7 C6 126.04(10) . . ? C11 C8 C10 106.98(10) . . ? C11 C8 C9 107.37(11) . . ? C10 C8 C9 109.41(11) . . ? C11 C8 C2 111.78(10) . . ? C10 C8 C2 111.68(10) . . ? C9 C8 C2 109.48(9) . . ? C4 C12 C15 112.21(10) . . ? C4 C12 C14 110.47(10) . . ? C15 C12 C14 108.20(11) . . ? C4 C12 C13 108.79(10) . . ? C15 C12 C13 108.20(11) . . ? C14 C12 C13 108.89(10) . . ? C17 C16 N1 124.96(11) . . ? C17 C16 C21 119.47(10) . . ? N1 C16 C21 115.57(9) . . ? C18 C17 C16 120.42(12) . . ? C17 C18 C19 120.09(11) . . ? C18 C19 C20 120.51(11) . . ? C19 C20 C21 120.13(12) . . ? C20 C21 N2 124.33(11) . . ? C20 C21 C16 119.37(10) . . ? N2 C21 C16 116.28(9) . . ? N2 C22 C23 126.76(10) . . ? C24 C23 C22 115.67(10) . . ? C24 C23 C28 120.40(10) . . ? C22 C23 C28 123.79(11) . . ? C25 C24 C23 122.33(10) . . ? C24 C25 C26 116.48(11) . . ? C24 C25 C29 124.01(10) . . ? C26 C25 C29 119.51(10) . . ? C27 C26 C25 124.80(10) . . ? C26 C27 C28 118.47(10) . . ? C26 C27 C33 122.22(10) . . ? C28 C27 C33 119.31(10) . . ? O2 C28 C23 123.18(10) . . ? O2 C28 C27 119.31(9) . . ? C23 C28 C27 117.51(10) . . ? C32 C29 C25 111.77(10) . . ? C32 C29 C31 108.34(13) . . ? C25 C29 C31 110.25(10) . . ? C32 C29 C30 108.25(12) . . ? C25 C29 C30 109.58(11) . . ? C31 C29 C30 108.57(11) . . ? C34 C33 C27 111.59(10) . . ? C34 C33 C36 107.81(10) . . ? C27 C33 C36 110.21(9) . . ? C34 C33 C35 106.97(10) . . ? C27 C33 C35 110.67(10) . . ? C36 C33 C35 109.49(11) . . ? C38' C37 C38 39.7(2) . . ? O3 C38 C39 60.37(12) . . ? O3 C38 C37 115.56(18) . . ? C39 C38 C37 122.75(18) . . ? C40 C39 O3 118.31(16) . . ? C40 C39 C38 120.72(18) . . ? O3 C39 C38 58.57(12) . . ? C39 C40 C39' 34.1(4) . . ? C37 C38' C39' 120.3(5) . . ? C37 C38' O3 114.8(4) . . ? C39' C38' O3 52.6(3) . . ? O3 C39' C40 122.0(6) . . ? O3 C39' C38' 64.3(4) . . ? C40 C39' C38' 124.0(8) . . ? C7 N1 C16 122.98(9) . . ? C7 N1 Zn1 122.79(7) . . ? C16 N1 Zn1 113.59(8) . . ? C22 N2 C21 122.06(9) . . ? C22 N2 Zn1 124.14(7) . . ? C21 N2 Zn1 113.44(8) . . ? C1 O1 Zn1 127.17(7) . . ? C28 O2 Zn1 130.49(7) . . ? C39' O3 C38 45.9(4) . . ? C39' O3 C39 35.9(5) . . ? C38 O3 C39 61.06(13) . . ? C39' O3 C38' 63.1(4) . . ? C38 O3 C38' 38.2(2) . . ? C39 O3 C38' 50.1(3) . . ? C39' O3 Zn1 154.9(5) . . ? C38 O3 Zn1 144.02(12) . . ? C39 O3 Zn1 120.50(10) . . ? C38' O3 Zn1 111.42(19) . . ? O2 Zn1 O1 95.27(4) . . ? O2 Zn1 N2 90.60(4) . . ? O1 Zn1 N2 157.93(4) . . ? O2 Zn1 N1 166.98(4) . . ? O1 Zn1 N1 90.41(4) . . ? N2 Zn1 N1 79.95(4) . . ? O2 Zn1 O3 100.67(5) . . ? O1 Zn1 O3 96.70(4) . . ? N2 Zn1 O3 103.10(4) . . ? N1 Zn1 O3 90.25(4) . . ? 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 -175.47(10) . . . . ? C6 C1 C2 C3 4.39(16) . . . . ? O1 C1 C2 C8 4.84(16) . . . . ? C6 C1 C2 C8 -175.31(10) . . . . ? C1 C2 C3 C4 -4.02(17) . . . . ? C8 C2 C3 C4 175.67(11) . . . . ? C2 C3 C4 C5 0.29(17) . . . . ? C2 C3 C4 C12 179.10(10) . . . . ? C3 C4 C5 C6 3.01(16) . . . . ? C12 C4 C5 C6 -175.75(10) . . . . ? C4 C5 C6 C1 -2.46(17) . . . . ? C4 C5 C6 C7 175.34(11) . . . . ? O1 C1 C6 C5 178.49(11) . . . . ? C2 C1 C6 C5 -1.36(16) . . . . ? O1 C1 C6 C7 0.88(18) . . . . ? C2 C1 C6 C7 -178.97(11) . . . . ? C5 C6 C7 N1 -171.24(11) . . . . ? C1 C6 C7 N1 6.46(19) . . . . ? C3 C2 C8 C11 0.08(16) . . . . ? C1 C2 C8 C11 179.77(11) . . . . ? C3 C2 C8 C10 119.91(12) . . . . ? C1 C2 C8 C10 -60.41(14) . . . . ? C3 C2 C8 C9 -118.76(12) . . . . ? C1 C2 C8 C9 60.93(14) . . . . ? C5 C4 C12 C15 -9.14(16) . . . . ? C3 C4 C12 C15 172.14(11) . . . . ? C5 C4 C12 C14 -129.97(12) . . . . ? C3 C4 C12 C14 51.31(14) . . . . ? C5 C4 C12 C13 110.55(12) . . . . ? C3 C4 C12 C13 -68.17(13) . . . . ? N1 C16 C17 C18 -179.57(11) . . . . ? C21 C16 C17 C18 0.52(18) . . . . ? C16 C17 C18 C19 0.1(2) . . . . ? C17 C18 C19 C20 -0.1(2) . . . . ? C18 C19 C20 C21 -0.5(2) . . . . ? C19 C20 C21 N2 -179.97(12) . . . . ? C19 C20 C21 C16 1.1(2) . . . . ? C17 C16 C21 C20 -1.10(18) . . . . ? N1 C16 C21 C20 178.98(11) . . . . ? C17 C16 C21 N2 179.89(11) . . . . ? N1 C16 C21 N2 -0.03(15) . . . . ? N2 C22 C23 C24 -175.52(12) . . . . ? N2 C22 C23 C28 0.3(2) . . . . ? C22 C23 C24 C25 175.28(11) . . . . ? C28 C23 C24 C25 -0.68(18) . . . . ? C23 C24 C25 C26 0.54(17) . . . . ? C23 C24 C25 C29 -179.89(11) . . . . ? C24 C25 C26 C27 0.35(18) . . . . ? C29 C25 C26 C27 -179.23(11) . . . . ? C25 C26 C27 C28 -1.06(18) . . . . ? C25 C26 C27 C33 178.82(11) . . . . ? C24 C23 C28 O2 179.51(11) . . . . ? C22 C23 C28 O2 3.89(19) . . . . ? C24 C23 C28 C27 -0.05(16) . . . . ? C22 C23 C28 C27 -175.66(11) . . . . ? C26 C27 C28 O2 -178.71(11) . . . . ? C33 C27 C28 O2 1.41(16) . . . . ? C26 C27 C28 C23 0.87(16) . . . . ? C33 C27 C28 C23 -179.02(10) . . . . ? C24 C25 C29 C32 2.56(18) . . . . ? C26 C25 C29 C32 -177.88(12) . . . . ? C24 C25 C29 C31 -118.00(13) . . . . ? C26 C25 C29 C31 61.56(15) . . . . ? C24 C25 C29 C30 122.56(13) . . . . ? C26 C25 C29 C30 -57.88(14) . . . . ? C26 C27 C33 C34 -3.23(16) . . . . ? C28 C27 C33 C34 176.65(11) . . . . ? C26 C27 C33 C36 116.51(12) . . . . ? C28 C27 C33 C36 -63.61(14) . . . . ? C26 C27 C33 C35 -122.23(12) . . . . ? C28 C27 C33 C35 57.65(14) . . . . ? C38' C37 C38 O3 59.6(4) . . . . ? C38' C37 C38 C39 -10.2(4) . . . . ? O3 C38 C39 C40 106.47(19) . . . . ? C37 C38 C39 C40 -150.6(2) . . . . ? C37 C38 C39 O3 103.0(2) . . . . ? O3 C39 C40 C39' 51.7(5) . . . . ? C38 C39 C40 C39' -16.6(5) . . . . ? C38 C37 C38' C39' 6.6(4) . . . . ? C38 C37 C38' O3 -53.1(3) . . . . ? C39 C40 C39' O3 -61.4(7) . . . . ? C39 C40 C39' C38' 17.3(3) . . . . ? C37 C38' C39' O3 -99.5(5) . . . . ? C37 C38' C39' C40 147.9(5) . . . . ? O3 C38' C39' C40 -112.6(7) . . . . ? C6 C7 N1 C16 177.83(11) . . . . ? C6 C7 N1 Zn1 7.61(17) . . . . ? C17 C16 N1 C7 1.20(18) . . . . ? C21 C16 N1 C7 -178.88(11) . . . . ? C17 C16 N1 Zn1 172.24(9) . . . . ? C21 C16 N1 Zn1 -7.85(13) . . . . ? C23 C22 N2 C21 175.79(11) . . . . ? C23 C22 N2 Zn1 3.04(18) . . . . ? C20 C21 N2 C22 15.49(19) . . . . ? C16 C21 N2 C22 -165.56(11) . . . . ? C20 C21 N2 Zn1 -171.05(10) . . . . ? C16 C21 N2 Zn1 7.90(13) . . . . ? C6 C1 O1 Zn1 -23.05(16) . . . . ? C2 C1 O1 Zn1 156.80(8) . . . . ? C23 C28 O2 Zn1 -11.91(18) . . . . ? C27 C28 O2 Zn1 167.64(8) . . . . ? C40 C39' O3 C38 158.2(12) . . . . ? C38' C39' O3 C38 42.7(4) . . . . ? C40 C39' O3 C39 57.2(7) . . . . ? C38' C39' O3 C39 -58.3(5) . . . . ? C40 C39' O3 C38' 115.5(9) . . . . ? C40 C39' O3 Zn1 32.2(14) . . . . ? C38' C39' O3 Zn1 -83.3(8) . . . . ? C39 C38 O3 C39' -41.1(6) . . . . ? C37 C38 O3 C39' -155.8(7) . . . . ? C37 C38 O3 C39 -114.7(2) . . . . ? C39 C38 O3 C38' 61.2(4) . . . . ? C37 C38 O3 C38' -53.5(4) . . . . ? C39 C38 O3 Zn1 103.04(19) . . . . ? C37 C38 O3 Zn1 -11.7(3) . . . . ? C40 C39 O3 C39' -56.9(6) . . . . ? C38 C39 O3 C39' 53.7(6) . . . . ? C40 C39 O3 C38 -110.5(2) . . . . ? C40 C39 O3 C38' -155.5(3) . . . . ? C38 C39 O3 C38' -44.9(3) . . . . ? C40 C39 O3 Zn1 111.09(18) . . . . ? C38 C39 O3 Zn1 -138.37(14) . . . . ? C37 C38' O3 C39' 110.3(6) . . . . ? C37 C38' O3 C38 58.4(4) . . . . ? C39' C38' O3 C38 -51.9(6) . . . . ? C37 C38' O3 C39 150.9(5) . . . . ? C39' C38' O3 C39 40.5(5) . . . . ? C37 C38' O3 Zn1 -96.6(3) . . . . ? C39' C38' O3 Zn1 153.0(5) . . . . ? C28 O2 Zn1 O1 -146.99(11) . . . . ? C28 O2 Zn1 N2 11.71(11) . . . . ? C28 O2 Zn1 N1 -31.4(2) . . . . ? C28 O2 Zn1 O3 115.16(11) . . . . ? C1 O1 Zn1 O2 -163.88(10) . . . . ? C1 O1 Zn1 N2 91.32(14) . . . . ? C1 O1 Zn1 N1 27.85(10) . . . . ? C1 O1 Zn1 O3 -62.46(10) . . . . ? C22 N2 Zn1 O2 -6.94(11) . . . . ? C21 N2 Zn1 O2 179.76(9) . . . . ? C22 N2 Zn1 O1 98.75(13) . . . . ? C21 N2 Zn1 O1 -74.56(13) . . . . ? C22 N2 Zn1 N1 164.06(11) . . . . ? C21 N2 Zn1 N1 -9.24(8) . . . . ? C22 N2 Zn1 O3 -108.04(10) . . . . ? C21 N2 Zn1 O3 78.66(9) . . . . ? C7 N1 Zn1 O2 -135.70(16) . . . . ? C16 N1 Zn1 O2 53.2(2) . . . . ? C7 N1 Zn1 O1 -19.64(10) . . . . ? C16 N1 Zn1 O1 169.30(8) . . . . ? C7 N1 Zn1 N2 -179.68(10) . . . . ? C16 N1 Zn1 N2 9.26(8) . . . . ? C7 N1 Zn1 O3 77.06(10) . . . . ? C16 N1 Zn1 O3 -94.00(8) . . . . ? C39' O3 Zn1 O2 81.5(9) . . . . ? C38 O3 Zn1 O2 -16.9(2) . . . . ? C39 O3 Zn1 O2 64.81(13) . . . . ? C38' O3 Zn1 O2 9.5(3) . . . . ? C39' O3 Zn1 O1 -15.2(9) . . . . ? C38 O3 Zn1 O1 -113.56(19) . . . . ? C39 O3 Zn1 O1 -31.87(13) . . . . ? C38' O3 Zn1 O1 -87.2(3) . . . . ? C39' O3 Zn1 N2 174.7(9) . . . . ? C38 O3 Zn1 N2 76.25(19) . . . . ? C39 O3 Zn1 N2 157.94(12) . . . . ? C38' O3 Zn1 N2 102.6(3) . . . . ? C39' O3 Zn1 N1 -105.6(9) . . . . ? C38 O3 Zn1 N1 155.99(19) . . . . ? C39 O3 Zn1 N1 -122.32(13) . . . . ? C38' O3 Zn1 N1 -177.7(3) . . . . ? _diffrn_measured_fraction_theta_max 0.905 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.971 _refine_diff_density_max 1.746 _refine_diff_density_min -0.653 _refine_diff_density_rms 0.077 # Attachment '- AWK656_0mX.cif' data_awk656_0m _database_code_depnum_ccdc_archive 'CCDC 867372' #TrackingRef '- AWK656_0mX.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C68.50 H85 N4 O9 Zn2' _chemical_formula_weight 1239.15 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' 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 C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 42.190 _cell_length_b 9.719 _cell_length_c 31.932 _cell_angle_alpha 90.00 _cell_angle_beta 110.08 _cell_angle_gamma 90.00 _cell_volume 12297.7 _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9864 _cell_measurement_theta_min 2.31 _cell_measurement_theta_max 34.12 _exptl_crystal_description Needle _exptl_crystal_colour orange _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.339 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5248 _exptl_absorpt_coefficient_mu 0.841 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8002 _exptl_absorpt_correction_T_max 0.9811 _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 110625 _diffrn_reflns_av_R_equivalents 0.0437 _diffrn_reflns_av_sigmaI/netI 0.0420 _diffrn_reflns_limit_h_min -68 _diffrn_reflns_limit_h_max 67 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -51 _diffrn_reflns_limit_l_max 50 _diffrn_reflns_theta_min 1.03 _diffrn_reflns_theta_max 35.06 _reflns_number_total 26810 _reflns_number_gt 19976 _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 asymmetric unit is made up of two Zn-salphen with a coordinated oxetane, one of them disordered in two position with occupations ratio 52:48 and a free oxetane disordered in two positions over a special position with half occupancy. ; _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^)+(0.0569P)^2^+7.2723P] 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 26810 _refine_ls_number_parameters 840 _refine_ls_number_restraints 28 _refine_ls_R_factor_all 0.0630 _refine_ls_R_factor_gt 0.0393 _refine_ls_wR_factor_ref 0.1120 _refine_ls_wR_factor_gt 0.0984 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.024 _refine_ls_shift/su_max 0.016 _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 C1A C 0.32636(3) 0.54546(10) 0.09010(3) 0.0216(2) Uani 1 1 d . . . C2A C 0.33546(3) 0.66944(10) 0.11657(3) 0.0279(2) Uani 1 1 d . . . C3A C 0.33695(3) 0.79189(11) 0.09517(4) 0.0297(3) Uani 1 1 d . . . H3AA H 0.3422 0.8719 0.1121 0.036 Uiso 1 1 calc R . . C4A C 0.33093(3) 0.80165(10) 0.04919(4) 0.0255(2) Uani 1 1 d . . . H4AA H 0.3323 0.8862 0.0363 0.031 Uiso 1 1 calc R . . C5A C 0.32303(2) 0.68530(10) 0.02378(3) 0.02048(19) Uani 1 1 d . . . H5AA H 0.3194 0.6906 -0.0066 0.025 Uiso 1 1 calc R . . C6A C 0.32034(2) 0.55624(9) 0.04310(3) 0.01788(18) Uani 1 1 d . . . C7A C 0.31006(2) 0.44402(9) 0.01225(3) 0.01677(17) Uani 1 1 d . . . H7AA H 0.3076 0.4629 -0.0172 0.020 Uiso 1 1 calc R . . C8A C 0.34356(4) 0.66440(11) 0.16725(4) 0.0446(4) Uani 1 1 d U . . C9A C 0.31302(5) 0.61053(15) 0.17862(4) 0.0575(4) Uani 1 1 d U . . H9AA H 0.3071 0.5203 0.1662 0.086 Uiso 1 1 calc R . . H9AB H 0.2942 0.6716 0.1663 0.086 Uiso 1 1 calc R . . H9AC H 0.3188 0.6062 0.2104 0.086 Uiso 1 1 calc R . . C10A C 0.37412(5) 0.57237(14) 0.18887(5) 0.0640(5) Uani 1 1 d U . . H10A H 0.3930 0.6061 0.1817 0.096 Uiso 1 1 calc R . . H10B H 0.3690 0.4801 0.1779 0.096 Uiso 1 1 calc R . . H10C H 0.3796 0.5729 0.2206 0.096 Uiso 1 1 calc R . . C11A C 0.35235(5) 0.80790(13) 0.18833(4) 0.0591(5) Uani 1 1 d U . . H11A H 0.3714 0.8441 0.1820 0.089 Uiso 1 1 calc R . . H11B H 0.3578 0.8011 0.2200 0.089 Uiso 1 1 calc R . . H11C H 0.3334 0.8681 0.1761 0.089 Uiso 1 1 calc R . . C12A C 0.29172(2) 0.21955(9) -0.01289(3) 0.01468(16) Uani 1 1 d . . . C13A C 0.29221(2) 0.23388(10) -0.05637(3) 0.01868(18) Uani 1 1 d . . . H13A H 0.3018 0.3118 -0.0640 0.022 Uiso 1 1 calc R . . C14A C 0.27851(2) 0.13304(10) -0.08807(3) 0.02040(19) Uani 1 1 d . . . H14A H 0.2785 0.1444 -0.1170 0.024 Uiso 1 1 calc R . . C15A C 0.26480(2) 0.01470(11) -0.07662(3) 0.0229(2) Uani 1 1 d . . . H15A H 0.2556 -0.0529 -0.0980 0.027 Uiso 1 1 calc R . . C16A C 0.26474(2) -0.00285(11) -0.03359(3) 0.02181(19) Uani 1 1 d . . . H16A H 0.2558 -0.0829 -0.0261 0.026 Uiso 1 1 calc R . . C17A C 0.27795(2) 0.09894(9) -0.00126(3) 0.01495(16) Uani 1 1 d . . . C18A C 0.26392(2) -0.00551(10) 0.05721(3) 0.01688(17) Uani 1 1 d . . . H18A H 0.2541 -0.0748 0.0368 0.020 Uiso 1 1 calc R . . C19A C 0.26150(2) -0.01942(10) 0.10076(3) 0.01769(17) Uani 1 1 d . . . C20A C 0.24205(2) -0.13290(11) 0.10575(3) 0.0230(2) Uani 1 1 d . . . H20A H 0.2323 -0.1913 0.0817 0.028 Uiso 1 1 calc R . . C21A C 0.23738(3) -0.15812(12) 0.14543(3) 0.0273(2) Uani 1 1 d . . . H21A H 0.2242 -0.2318 0.1483 0.033 Uiso 1 1 calc R . . C22A C 0.25283(2) -0.07066(12) 0.18169(3) 0.0246(2) Uani 1 1 d . . . H22A H 0.2499 -0.0898 0.2087 0.030 Uiso 1 1 calc R . . C23A C 0.27211(2) 0.04240(11) 0.17948(3) 0.01984(18) Uani 1 1 d . . . C24A C 0.27669(2) 0.07247(10) 0.13746(3) 0.01787(17) Uani 1 1 d . . . C25A C 0.28812(2) 0.13497(11) 0.22022(3) 0.02134(19) Uani 1 1 d . . . C26A C 0.32681(2) 0.13862(12) 0.23259(3) 0.0257(2) Uani 1 1 d . . . H26A H 0.3356 0.0469 0.2387 0.039 Uiso 1 1 calc R . . H26B H 0.3365 0.1948 0.2586 0.039 Uiso 1 1 calc R . . H26C H 0.3324 0.1764 0.2082 0.039 Uiso 1 1 calc R . . C27A C 0.27401(2) 0.28233(12) 0.21052(3) 0.0258(2) Uani 1 1 d . . . H27A H 0.2499 0.2802 0.2029 0.039 Uiso 1 1 calc R . . H27B H 0.2795 0.3200 0.1861 0.039 Uiso 1 1 calc R . . H27C H 0.2838 0.3385 0.2365 0.039 Uiso 1 1 calc R . . C28A C 0.28093(3) 0.08311(14) 0.26159(3) 0.0308(2) Uani 1 1 d . . . H28A H 0.2895 -0.0087 0.2686 0.046 Uiso 1 1 calc R . . H28B H 0.2570 0.0830 0.2556 0.046 Uiso 1 1 calc R . . H28C H 0.2917 0.1426 0.2864 0.046 Uiso 1 1 calc R . . C29A C 0.37857(2) 0.17258(10) 0.14646(3) 0.01975(18) Uani 1 1 d . . . H29E H 0.3774 0.1031 0.1677 0.024 Uiso 0.5182(11) 1 calc PR A 2 H29F H 0.3789 0.2644 0.1585 0.024 Uiso 0.5182(11) 1 calc PR A 2 H29C H 0.3724 0.2431 0.1633 0.024 Uiso 0.4818(11) 1 d PR A 1 H29D H 0.3838 0.0886 0.1633 0.024 Uiso 0.4818(11) 1 d PR A 1 C30A C 0.40652(4) 0.2203(2) 0.12843(6) 0.0166(4) Uani 0.4818(11) 1 d P A 1 C31A C 0.37814(4) 0.2420(2) 0.08311(6) 0.0194(4) Uani 0.4818(11) 1 d P A 1 H31A H 0.3825 0.1993 0.0582 0.023 Uiso 0.4818(11) 1 calc PR A 1 H31B H 0.3714 0.3373 0.0767 0.023 Uiso 0.4818(11) 1 calc PR A 1 C32A C 0.42762(6) 0.0957(3) 0.12687(7) 0.0307(5) Uani 0.4818(11) 1 d P A 1 H32A H 0.4133 0.0278 0.1069 0.037 Uiso 0.4818(11) 1 calc PR A 1 H32B H 0.4449 0.1228 0.1148 0.037 Uiso 0.4818(11) 1 calc PR A 1 C33A C 0.42741(5) 0.3473(2) 0.14765(7) 0.0234(4) Uani 0.4818(11) 1 d P A 1 H33A H 0.4443 0.3247 0.1757 0.035 Uiso 0.4818(11) 1 calc PR A 1 H33B H 0.4130 0.4182 0.1520 0.035 Uiso 0.4818(11) 1 calc PR A 1 H33C H 0.4381 0.3792 0.1274 0.035 Uiso 0.4818(11) 1 calc PR A 1 O4A O 0.44324(5) 0.0351(2) 0.16934(6) 0.0417(5) Uani 0.4818(11) 1 d PD A 1 H4AB H 0.4544 -0.0317 0.1671 0.063 Uiso 0.2409(6) 1 d PR A 1 H4A' H 0.4527(5) 0.0999(9) 0.1872(4) 0.063 Uiso 0.2409(6) 1 d PD A 1 C30' C 0.40701(4) 0.1465(2) 0.12628(6) 0.0187(4) Uani 0.5182(11) 1 d P A 2 C31' C 0.37743(4) 0.1613(3) 0.08179(6) 0.0252(4) Uani 0.5182(11) 1 d P A 2 H31C H 0.3774 0.2487 0.0671 0.030 Uiso 0.5182(11) 1 calc PR A 2 H31D H 0.3760 0.0857 0.0614 0.030 Uiso 0.5182(11) 1 calc PR A 2 C32' C 0.42001(5) -0.0006(2) 0.13140(6) 0.0244(4) Uani 0.5182(11) 1 d P A 2 H32C H 0.4012 -0.0642 0.1222 0.029 Uiso 0.5182(11) 1 calc PR A 2 H32D H 0.4335 -0.0154 0.1126 0.029 Uiso 0.5182(11) 1 calc PR A 2 C33' C 0.43418(6) 0.2556(3) 0.13532(8) 0.0370(6) Uani 0.5182(11) 1 d P A 2 H33D H 0.4503 0.2291 0.1217 0.056 Uiso 0.5182(11) 1 calc PR A 2 H33E H 0.4453 0.2650 0.1669 0.056 Uiso 0.5182(11) 1 calc PR A 2 H33F H 0.4241 0.3418 0.1231 0.056 Uiso 0.5182(11) 1 calc PR A 2 O4' O 0.43994(4) -0.02494(17) 0.17681(5) 0.0325(4) Uani 0.5182(11) 1 d PD A 2 H4'A H 0.4470 -0.1043 0.1799 0.049 Uiso 0.2591(6) 1 d PR A 2 H4'' H 0.4479(6) 0.0447(8) 0.1932(5) 0.049 Uiso 0.2591(6) 1 d PD A 2 C1B C 0.45346(2) 0.16763(9) 0.47962(3) 0.01556(16) Uani 1 1 d . . . C2B C 0.43067(2) 0.07130(9) 0.48896(3) 0.01731(16) Uani 1 1 d . . . C3B C 0.44293(2) -0.00925(10) 0.52690(3) 0.02047(18) Uani 1 1 d . . . H3BA H 0.4283 -0.0711 0.5330 0.025 Uiso 1 1 calc R . . C4B C 0.47639(2) -0.00244(10) 0.55664(3) 0.02191(19) Uani 1 1 d . . . H4BA H 0.4836 -0.0587 0.5817 0.026 Uiso 1 1 calc R . . C5B C 0.49818(2) 0.08826(10) 0.54804(3) 0.01946(18) Uani 1 1 d . . . H5BA H 0.5204 0.0924 0.5673 0.023 Uiso 1 1 calc R . . C6B C 0.48754(2) 0.17594(9) 0.51040(3) 0.01593(16) Uani 1 1 d . . . C7B C 0.51305(2) 0.26422(9) 0.50495(3) 0.01620(16) Uani 1 1 d . . . H7BA H 0.5345 0.2577 0.5264 0.019 Uiso 1 1 calc R . . C8B C 0.39425(2) 0.05654(10) 0.45609(3) 0.01925(17) Uani 1 1 d . . . C9B C 0.37326(3) -0.04089(12) 0.47377(4) 0.0297(2) Uani 1 1 d . . . H9BA H 0.3839 -0.1295 0.4796 0.045 Uiso 1 1 calc R . . H9BB H 0.3511 -0.0500 0.4520 0.045 Uiso 1 1 calc R . . H9BC H 0.3716 -0.0043 0.5009 0.045 Uiso 1 1 calc R . . C10B C 0.37567(3) 0.19596(11) 0.44776(4) 0.0288(2) Uani 1 1 d . . . H10D H 0.3531 0.1836 0.4271 0.043 Uiso 1 1 calc R . . H10E H 0.3875 0.2599 0.4356 0.043 Uiso 1 1 calc R . . H10F H 0.3747 0.2312 0.4754 0.043 Uiso 1 1 calc R . . C11B C 0.39485(2) -0.00314(11) 0.41193(3) 0.0252(2) Uani 1 1 d . . . H11D H 0.4065 -0.0898 0.4174 0.038 Uiso 1 1 calc R . . H11E H 0.4063 0.0595 0.3987 0.038 Uiso 1 1 calc R . . H11F H 0.3721 -0.0165 0.3920 0.038 Uiso 1 1 calc R . . C12B C 0.53636(2) 0.42825(9) 0.46803(3) 0.01607(16) Uani 1 1 d . . . C13B C 0.57057(2) 0.40366(10) 0.49203(3) 0.02095(19) Uani 1 1 d . . . H13B H 0.5766 0.3369 0.5142 0.025 Uiso 1 1 calc R . . C14B C 0.59533(2) 0.47846(11) 0.48278(3) 0.0248(2) Uani 1 1 d . . . H14B H 0.6179 0.4616 0.4989 0.030 Uiso 1 1 calc R . . C15B C 0.58676(2) 0.57834(12) 0.44964(4) 0.0272(2) Uani 1 1 d . . . H15B H 0.6036 0.6274 0.4435 0.033 Uiso 1 1 calc R . . C16B C 0.55309(2) 0.60469(11) 0.42580(4) 0.0242(2) Uani 1 1 d . . . H16B H 0.5474 0.6718 0.4037 0.029 Uiso 1 1 calc R . . C17B C 0.52763(2) 0.53108(9) 0.43474(3) 0.01651(17) Uani 1 1 d . . . C18B C 0.48064(2) 0.65357(9) 0.38620(3) 0.01607(16) Uani 1 1 d . . . H18B H 0.4962 0.7163 0.3828 0.019 Uiso 1 1 calc R . . C19B C 0.44556(2) 0.68226(9) 0.36268(3) 0.01547(16) Uani 1 1 d . . . C20B C 0.43909(2) 0.80142(10) 0.33565(3) 0.01880(18) Uani 1 1 d . . . H20B H 0.4571 0.8517 0.3331 0.023 Uiso 1 1 calc R . . C21B C 0.40679(2) 0.84420(10) 0.31313(3) 0.0220(2) Uani 1 1 d . . . H21B H 0.4028 0.9212 0.2948 0.026 Uiso 1 1 calc R . . C22B C 0.37984(2) 0.77003(10) 0.31820(3) 0.02045(19) Uani 1 1 d . . . H22B H 0.3580 0.8008 0.3032 0.025 Uiso 1 1 calc R . . C23B C 0.38411(2) 0.65337(9) 0.34442(3) 0.01643(17) Uani 1 1 d . . . C24B C 0.41799(2) 0.60311(9) 0.36675(3) 0.01547(16) Uani 1 1 d . . . C25B C 0.35368(2) 0.57841(10) 0.34979(3) 0.01854(18) Uani 1 1 d . . . C26B C 0.35755(2) 0.56950(11) 0.39951(3) 0.0238(2) Uani 1 1 d . . . H26D H 0.3595 0.6605 0.4118 0.036 Uiso 1 1 calc R . . H26E H 0.3774 0.5176 0.4153 0.036 Uiso 1 1 calc R . . H26F H 0.3381 0.5248 0.4024 0.036 Uiso 1 1 calc R . . C27B C 0.35059(2) 0.43281(11) 0.32979(4) 0.0243(2) Uani 1 1 d . . . H27D H 0.3482 0.4390 0.2989 0.037 Uiso 1 1 calc R . . H27E H 0.3312 0.3878 0.3326 0.037 Uiso 1 1 calc R . . H27F H 0.3705 0.3808 0.3455 0.037 Uiso 1 1 calc R . . C28B C 0.32043(2) 0.65438(12) 0.32593(4) 0.0287(2) Uani 1 1 d . . . H28D H 0.3171 0.6618 0.2947 0.043 Uiso 1 1 calc R . . H28E H 0.3214 0.7448 0.3384 0.043 Uiso 1 1 calc R . . H28F H 0.3020 0.6041 0.3297 0.043 Uiso 1 1 calc R . . C29B C 0.46907(2) 0.33349(11) 0.32694(3) 0.0234(2) Uani 1 1 d . . . H29A H 0.4907 0.3299 0.3225 0.028 Uiso 1 1 calc R . . H29B H 0.4601 0.4263 0.3226 0.028 Uiso 1 1 calc R . . C30B C 0.44394(2) 0.22539(9) 0.29993(3) 0.01613(16) Uani 1 1 d . . . C31B C 0.44138(2) 0.18253(10) 0.34507(3) 0.01915(17) Uani 1 1 d . . . H31E H 0.4203 0.2094 0.3486 0.023 Uiso 1 1 calc R . . H31F H 0.4459 0.0856 0.3518 0.023 Uiso 1 1 calc R . . C32B C 0.46043(3) 0.11454(12) 0.28104(3) 0.0305(2) Uani 1 1 d . . . H32E H 0.4811 0.0840 0.3038 0.037 Uiso 1 1 calc R . . H32F H 0.4454 0.0362 0.2719 0.037 Uiso 1 1 calc R . . C33B C 0.41214(3) 0.27936(15) 0.26533(4) 0.0349(3) Uani 1 1 d . . . H33G H 0.4167 0.3029 0.2387 0.052 Uiso 1 1 calc R . . H33H H 0.4046 0.3597 0.2767 0.052 Uiso 1 1 calc R . . H33I H 0.3949 0.2099 0.2586 0.052 Uiso 1 1 calc R . . N1A N 0.303770(18) 0.31862(8) 0.02123(2) 0.01662(15) Uani 1 1 d . A . N2A N 0.278394(17) 0.09352(8) 0.04330(2) 0.01506(14) Uani 1 1 d . A . N1B N 0.509164(17) 0.35256(8) 0.47298(2) 0.01531(14) Uani 1 1 d . . . N2B N 0.492587(17) 0.54839(8) 0.41175(2) 0.01549(14) Uani 1 1 d . . . O1A O 0.32403(2) 0.42971(7) 0.10911(2) 0.02493(16) Uani 1 1 d . A . O2A O 0.294406(16) 0.17869(7) 0.13437(2) 0.02019(14) Uani 1 1 d . A . O3A O 0.353581(16) 0.15427(8) 0.10167(2) 0.02501(16) Uani 1 1 d . A . O1B O 0.442585(16) 0.24134(7) 0.44359(2) 0.01918(14) Uani 1 1 d . . . O2B O 0.422564(15) 0.48998(7) 0.38971(2) 0.01959(14) Uani 1 1 d . . . O3B O 0.469750(16) 0.27184(7) 0.36906(2) 0.01774(13) Uani 1 1 d . . . O4B O 0.46784(2) 0.16708(12) 0.24373(3) 0.0439(2) Uani 1 1 d D . . H4BB H 0.4580(5) 0.1232(11) 0.2196(3) 0.059(11) Uiso 0.50 1 d PD B -1 H4'B H 0.48936(9) 0.164(3) 0.2528(10) 0.043(9) Uiso 0.50 1 d PD C 2 Zn1A Zn 0.305521(2) 0.250276(10) 0.083990(3) 0.01390(2) Uani 1 1 d . . . Zn1B Zn 0.463962(2) 0.389584(10) 0.422738(3) 0.01396(2) Uani 1 1 d . . . O1C O 0.45064(4) 0.70287(17) 0.19599(5) 0.0293(4) Uani 0.50 1 d P . . O2C O 0.51871(4) 0.79777(18) 0.31447(5) 0.0340(4) Uani 0.50 1 d P . . H2CA H 0.5278 0.8735 0.3257 0.051 Uiso 0.50 1 d PR . . C1C C 0.48432(5) 0.6691(2) 0.19727(7) 0.0256(4) Uani 0.50 1 d P . . H1CA H 0.4943 0.7406 0.1852 0.031 Uiso 0.50 1 d PR . . H1CB H 0.4852 0.5830 0.1830 0.031 Uiso 0.50 1 d PR . . C2C C 0.5000 0.65972(15) 0.2500 0.0251(3) Uani 1 2 d S . . C3C C 0.45978(5) 0.6649(3) 0.24315(7) 0.0277(5) Uani 0.50 1 d P . . H3CA H 0.4509 0.5773 0.2475 0.033 Uiso 0.50 1 d PR . . H3CB H 0.4542 0.7344 0.2608 0.033 Uiso 0.50 1 d PR . . C4C C 0.51585(6) 0.7913(2) 0.26892(7) 0.0280(5) Uani 0.50 1 d P . . H4CA H 0.5378 0.7983 0.2664 0.034 Uiso 0.50 1 d PR . . H4CB H 0.5023 0.8663 0.2528 0.034 Uiso 0.50 1 d PR . . C5C C 0.51712(7) 0.5319(2) 0.26906(9) 0.0376(6) Uani 0.50 1 d P . . H5CA H 0.5405 0.5371 0.2720 0.056 Uiso 0.50 1 d PR . . H5CB H 0.5153 0.5182 0.2979 0.056 Uiso 0.50 1 d PR . . H5CC H 0.5067 0.4564 0.2500 0.056 Uiso 0.50 1 d PR . . 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 C1A 0.0275(4) 0.0130(4) 0.0180(4) 0.0000(3) -0.0004(3) 0.0018(3) C2A 0.0419(5) 0.0133(4) 0.0186(4) -0.0017(3) -0.0025(4) 0.0030(4) C3A 0.0392(5) 0.0129(4) 0.0267(5) -0.0007(4) -0.0019(4) 0.0015(4) C4A 0.0282(4) 0.0150(4) 0.0281(5) 0.0040(3) 0.0030(4) 0.0004(3) C5A 0.0194(3) 0.0182(4) 0.0213(4) 0.0037(3) 0.0038(3) -0.0002(3) C6A 0.0184(3) 0.0150(4) 0.0169(3) 0.0003(3) 0.0018(3) 0.0000(3) C7A 0.0159(3) 0.0183(4) 0.0144(3) 0.0014(3) 0.0030(3) 0.0006(3) C8A 0.0866(9) 0.0129(4) 0.0167(4) -0.0029(4) -0.0048(5) 0.0053(5) C9A 0.1160(11) 0.0335(7) 0.0226(5) -0.0049(5) 0.0232(6) -0.0013(7) C10A 0.1022(11) 0.0230(5) 0.0288(6) -0.0049(5) -0.0264(7) 0.0152(7) C11A 0.1136(13) 0.0174(5) 0.0225(5) -0.0065(4) -0.0072(7) 0.0066(7) C12A 0.0134(3) 0.0164(3) 0.0129(3) -0.0009(3) 0.0028(2) 0.0022(3) C13A 0.0216(3) 0.0200(4) 0.0146(3) 0.0007(3) 0.0064(3) 0.0029(3) C14A 0.0228(3) 0.0246(4) 0.0129(3) -0.0005(3) 0.0050(3) 0.0045(3) C15A 0.0256(4) 0.0259(4) 0.0149(3) -0.0067(3) 0.0040(3) -0.0030(3) C16A 0.0251(4) 0.0233(4) 0.0160(3) -0.0054(3) 0.0057(3) -0.0066(3) C17A 0.0134(3) 0.0179(4) 0.0126(3) -0.0018(3) 0.0031(2) 0.0006(3) C18A 0.0146(3) 0.0194(4) 0.0148(3) -0.0018(3) 0.0027(3) -0.0017(3) C19A 0.0154(3) 0.0225(4) 0.0146(3) -0.0008(3) 0.0044(3) -0.0041(3) C20A 0.0219(4) 0.0268(4) 0.0186(4) -0.0013(3) 0.0048(3) -0.0085(3) C21A 0.0276(4) 0.0324(5) 0.0229(4) -0.0003(4) 0.0100(3) -0.0135(4) C22A 0.0235(4) 0.0344(5) 0.0178(3) 0.0005(3) 0.0093(3) -0.0072(4) C23A 0.0158(3) 0.0292(4) 0.0152(3) -0.0018(3) 0.0063(3) -0.0038(3) C24A 0.0134(3) 0.0253(4) 0.0146(3) -0.0013(3) 0.0044(2) -0.0034(3) C25A 0.0183(3) 0.0332(5) 0.0144(3) -0.0040(3) 0.0080(3) -0.0041(3) C26A 0.0182(3) 0.0393(5) 0.0182(4) -0.0079(4) 0.0045(3) -0.0030(4) C27A 0.0225(4) 0.0341(5) 0.0216(4) -0.0053(4) 0.0087(3) -0.0013(4) C28A 0.0339(4) 0.0442(6) 0.0172(4) -0.0039(4) 0.0125(3) -0.0083(4) C29A 0.0207(3) 0.0239(4) 0.0143(3) -0.0029(3) 0.0055(3) -0.0007(3) C30A 0.0140(6) 0.0241(8) 0.0122(6) 0.0007(6) 0.0051(5) 0.0053(6) C31A 0.0142(6) 0.0302(10) 0.0146(7) 0.0017(7) 0.0062(5) 0.0025(7) C32A 0.0286(9) 0.0415(12) 0.0180(8) -0.0047(8) 0.0031(7) 0.0177(9) C33A 0.0189(7) 0.0283(10) 0.0215(8) 0.0045(7) 0.0049(6) -0.0051(7) O4A 0.0523(10) 0.0338(9) 0.0285(8) -0.0007(7) 0.0004(8) 0.0270(8) C30' 0.0160(6) 0.0237(8) 0.0150(6) 0.0034(6) 0.0034(5) 0.0023(6) C31' 0.0185(7) 0.0420(11) 0.0146(7) 0.0024(7) 0.0050(6) 0.0047(8) C32' 0.0210(7) 0.0297(9) 0.0215(7) -0.0018(7) 0.0059(6) 0.0063(7) C33' 0.0250(9) 0.0418(12) 0.0353(11) 0.0150(9) -0.0011(8) -0.0112(9) O4' 0.0361(8) 0.0257(8) 0.0252(7) -0.0016(6) -0.0030(6) 0.0075(7) C1B 0.0190(3) 0.0150(3) 0.0134(3) -0.0010(3) 0.0066(2) -0.0005(3) C2B 0.0219(3) 0.0167(4) 0.0161(3) -0.0009(3) 0.0101(3) -0.0009(3) C3B 0.0289(4) 0.0187(4) 0.0180(3) 0.0013(3) 0.0135(3) 0.0003(3) C4B 0.0312(4) 0.0210(4) 0.0158(3) 0.0036(3) 0.0110(3) 0.0046(3) C5B 0.0236(3) 0.0211(4) 0.0137(3) 0.0004(3) 0.0065(3) 0.0045(3) C6B 0.0189(3) 0.0163(3) 0.0128(3) -0.0008(3) 0.0057(3) 0.0016(3) C7B 0.0164(3) 0.0185(4) 0.0124(3) -0.0020(3) 0.0034(2) 0.0013(3) C8B 0.0201(3) 0.0187(4) 0.0216(3) 0.0008(3) 0.0105(3) -0.0031(3) C9B 0.0271(4) 0.0304(5) 0.0374(5) 0.0048(4) 0.0185(3) -0.0054(4) C10B 0.0223(4) 0.0244(5) 0.0404(5) 0.0017(4) 0.0116(4) 0.0003(4) C11B 0.0252(4) 0.0296(5) 0.0207(4) -0.0048(3) 0.0078(3) -0.0090(4) C12B 0.0134(3) 0.0173(4) 0.0162(3) -0.0028(3) 0.0034(3) -0.0008(3) C13B 0.0150(3) 0.0246(4) 0.0206(4) 0.0005(3) 0.0027(3) 0.0003(3) C14B 0.0135(3) 0.0306(5) 0.0272(4) 0.0001(4) 0.0032(3) 0.0002(3) C15B 0.0155(3) 0.0294(5) 0.0365(5) 0.0047(4) 0.0087(3) -0.0019(3) C16B 0.0159(3) 0.0243(4) 0.0315(4) 0.0069(4) 0.0071(3) -0.0013(3) C17B 0.0131(3) 0.0162(3) 0.0192(3) -0.0015(3) 0.0043(3) -0.0007(3) C18B 0.0159(3) 0.0147(3) 0.0183(3) -0.0011(3) 0.0067(3) -0.0010(3) C19B 0.0164(3) 0.0148(3) 0.0147(3) -0.0004(3) 0.0047(3) 0.0000(3) C20B 0.0209(3) 0.0166(4) 0.0180(3) 0.0013(3) 0.0056(3) -0.0003(3) C21B 0.0241(4) 0.0187(4) 0.0199(4) 0.0041(3) 0.0032(3) 0.0009(3) C22B 0.0182(3) 0.0193(4) 0.0190(4) 0.0005(3) 0.0003(3) 0.0023(3) C23B 0.0154(3) 0.0164(3) 0.0153(3) -0.0021(3) 0.0024(3) 0.0003(3) C24B 0.0157(3) 0.0150(3) 0.0147(3) -0.0010(3) 0.0039(3) -0.0002(3) C25B 0.0143(3) 0.0184(4) 0.0214(4) -0.0018(3) 0.0043(3) 0.0005(3) C26B 0.0218(3) 0.0279(5) 0.0232(4) -0.0025(3) 0.0097(3) -0.0006(3) C27B 0.0190(3) 0.0231(4) 0.0297(4) -0.0075(4) 0.0067(3) -0.0048(3) C28B 0.0162(3) 0.0312(5) 0.0355(5) 0.0026(4) 0.0047(4) 0.0030(4) C29B 0.0295(4) 0.0257(4) 0.0159(3) -0.0013(3) 0.0091(3) -0.0116(3) C30B 0.0160(3) 0.0188(4) 0.0137(3) -0.0017(3) 0.0052(2) -0.0010(3) C31B 0.0225(3) 0.0198(4) 0.0160(3) -0.0029(3) 0.0078(3) -0.0075(3) C32B 0.0455(5) 0.0291(5) 0.0210(4) 0.0000(4) 0.0166(4) 0.0098(4) C33B 0.0213(4) 0.0588(8) 0.0224(4) 0.0058(5) 0.0045(4) 0.0086(5) N1A 0.0185(3) 0.0157(3) 0.0145(3) -0.0003(2) 0.0042(2) 0.0004(2) N2A 0.0135(2) 0.0188(3) 0.0122(3) -0.0020(2) 0.0033(2) -0.0013(2) N1B 0.0149(3) 0.0152(3) 0.0144(3) -0.0013(2) 0.0032(2) -0.0009(2) N2B 0.0138(3) 0.0147(3) 0.0169(3) -0.0003(2) 0.0039(2) -0.0013(2) O1A 0.0408(4) 0.0138(3) 0.0146(3) -0.0004(2) 0.0023(3) -0.0009(3) O2A 0.0198(2) 0.0269(3) 0.0146(2) -0.0040(2) 0.0068(2) -0.0094(2) O3A 0.0155(3) 0.0346(4) 0.0212(3) -0.0111(3) 0.0014(2) 0.0039(3) O1B 0.0182(2) 0.0206(3) 0.0159(3) 0.0046(2) 0.0023(2) -0.0044(2) O2B 0.0150(2) 0.0180(3) 0.0235(3) 0.0060(2) 0.0037(2) -0.0001(2) O3B 0.0197(2) 0.0191(3) 0.0131(2) -0.0010(2) 0.0040(2) -0.0036(2) O4B 0.0480(4) 0.0673(6) 0.0230(3) 0.0065(4) 0.0207(3) 0.0222(4) Zn1A 0.01455(4) 0.01447(4) 0.01200(4) -0.00083(3) 0.00368(3) -0.00027(3) Zn1B 0.01355(4) 0.01362(4) 0.01306(4) 0.00038(3) 0.00243(3) -0.00185(3) O1C 0.0309(7) 0.0291(7) 0.0262(7) 0.0004(6) 0.0076(6) 0.0027(6) O2C 0.0472(8) 0.0299(8) 0.0235(7) -0.0033(6) 0.0102(6) -0.0180(7) C1C 0.0303(8) 0.0261(9) 0.0225(8) -0.0020(7) 0.0119(6) 0.0001(7) C2C 0.0337(6) 0.0190(6) 0.0261(6) 0.000 0.0149(5) 0.000 C3C 0.0247(8) 0.0363(11) 0.0230(8) -0.0013(8) 0.0091(7) -0.0052(8) C4C 0.0329(9) 0.0245(9) 0.0268(9) -0.0004(7) 0.0103(7) -0.0088(8) C5C 0.0373(11) 0.0237(10) 0.0430(13) 0.0037(9) 0.0026(10) 0.0031(9) _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 C1A O1A 1.2982(12) . ? C1A C6A 1.4371(13) . ? C1A C2A 1.4460(14) . ? C2A C3A 1.3844(15) . ? C2A C8A 1.5359(16) . ? C3A C4A 1.4046(16) . ? C4A C5A 1.3648(14) . ? C5A C6A 1.4195(13) . ? C6A C7A 1.4335(13) . ? C7A N1A 1.3001(12) . ? C8A C10A 1.526(2) . ? C8A C11A 1.5375(17) . ? C8A C9A 1.545(3) . ? C12A C13A 1.4025(13) . ? C12A N1A 1.4115(11) . ? C12A C17A 1.4133(13) . ? C13A C14A 1.3849(13) . ? C14A C15A 1.3916(15) . ? C15A C16A 1.3854(14) . ? C16A C17A 1.4000(12) . ? C17A N2A 1.4177(11) . ? C18A N2A 1.2972(12) . ? C18A C19A 1.4351(13) . ? C19A C20A 1.4162(14) . ? C19A C24A 1.4373(12) . ? C20A C21A 1.3695(15) . ? C21A C22A 1.4035(15) . ? C22A C23A 1.3833(14) . ? C23A C24A 1.4496(13) . ? C23A C25A 1.5344(13) . ? C24A O2A 1.2979(12) . ? C25A C28A 1.5384(14) . ? C25A C27A 1.5411(15) . ? C25A C26A 1.5422(13) . ? C29A O3A 1.4676(10) . ? C29A C30A 1.550(2) . ? C29A C30' 1.565(2) . ? C30A C32A 1.514(3) . ? C30A C33A 1.518(3) . ? C30A C31A 1.543(2) . ? C31A O3A 1.604(2) . ? C32A O4A 1.416(3) . ? C30' C33' 1.514(3) . ? C30' C32' 1.520(3) . ? C30' C31' 1.542(2) . ? C31' O3A 1.363(2) . ? C32' O4' 1.424(2) . ? C1B O1B 1.2980(10) . ? C1B C6B 1.4388(11) . ? C1B C2B 1.4446(13) . ? C2B C3B 1.3849(12) . ? C2B C8B 1.5414(12) . ? C3B C4B 1.4067(13) . ? C4B C5B 1.3678(14) . ? C5B C6B 1.4149(12) . ? C6B C7B 1.4328(13) . ? C7B N1B 1.3007(12) . ? C8B C9B 1.5306(14) . ? C8B C11B 1.5329(14) . ? C8B C10B 1.5421(14) . ? C12B C13B 1.4030(12) . ? C12B C17B 1.4128(13) . ? C12B N1B 1.4166(12) . ? C13B C14B 1.3853(15) . ? C14B C15B 1.3895(15) . ? C15B C16B 1.3857(13) . ? C16B C17B 1.3993(13) . ? C17B N2B 1.4168(10) . ? C18B N2B 1.2970(11) . ? C18B C19B 1.4385(11) . ? C19B C20B 1.4138(13) . ? C19B C24B 1.4370(12) . ? C20B C21B 1.3689(13) . ? C21B C22B 1.4018(14) . ? C22B C23B 1.3840(13) . ? C23B C24B 1.4456(11) . ? C23B C25B 1.5361(13) . ? C24B O2B 1.2988(11) . ? C25B C28B 1.5361(13) . ? C25B C27B 1.5395(14) . ? C25B C26B 1.5419(14) . ? C29B O3B 1.4637(12) . ? C29B C30B 1.5311(13) . ? C30B C33B 1.5093(13) . ? C30B C32B 1.5153(14) . ? C30B C31B 1.5394(13) . ? C31B O3B 1.4640(11) . ? C32B O4B 1.4261(15) . ? N1A Zn1A 2.0884(8) . ? N2A Zn1A 2.0732(7) . ? N1B Zn1B 2.0589(7) . ? N2B Zn1B 2.0628(8) . ? O1A Zn1A 1.9658(7) . ? O2A Zn1A 1.9520(7) . ? O3A Zn1A 2.1248(7) . ? O1B Zn1B 1.9352(7) . ? O2B Zn1B 1.9622(6) . ? O3B Zn1B 2.1434(7) . ? O1C C1C 1.445(3) . ? O1C C3C 1.467(3) . ? O1C C4C 1.704(3) 2_655 ? O1C O2C 1.712(3) 2_655 ? O2C C1C 1.299(3) 2_655 ? O2C C4C 1.419(3) . ? O2C O1C 1.712(3) 2_655 ? C1C O2C 1.299(3) 2_655 ? C1C C2C 1.586(2) . ? C1C C4C 1.606(3) 2_655 ? C1C C5C 1.727(3) 2_655 ? C2C C5C 1.460(3) . ? C2C C5C 1.460(3) 2_655 ? C2C C4C 1.473(2) 2_655 ? C2C C4C 1.473(3) . ? C2C C1C 1.586(2) 2_655 ? C2C C3C 1.635(2) . ? C2C C3C 1.636(2) 2_655 ? C3C C4C 1.728(3) 2_655 ? C3C C5C 1.741(4) 2_655 ? C4C C4C 1.462(4) 2_655 ? C4C C1C 1.606(3) 2_655 ? C4C O1C 1.704(3) 2_655 ? C4C C3C 1.728(3) 2_655 ? C5C C5C 1.537(5) 2_655 ? C5C C1C 1.727(3) 2_655 ? C5C C3C 1.741(4) 2_655 ? 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 O1A C1A C6A 122.47(8) . . ? O1A C1A C2A 119.75(9) . . ? C6A C1A C2A 117.77(9) . . ? C3A C2A C1A 118.41(10) . . ? C3A C2A C8A 121.07(9) . . ? C1A C2A C8A 120.52(9) . . ? C2A C3A C4A 123.46(10) . . ? C5A C4A C3A 119.02(10) . . ? C4A C5A C6A 120.89(9) . . ? C5A C6A C7A 115.09(8) . . ? C5A C6A C1A 120.42(8) . . ? C7A C6A C1A 124.44(8) . . ? N1A C7A C6A 126.73(8) . . ? C10A C8A C2A 110.08(13) . . ? C10A C8A C11A 107.13(12) . . ? C2A C8A C11A 111.43(10) . . ? C10A C8A C9A 109.78(12) . . ? C2A C8A C9A 110.88(11) . . ? C11A C8A C9A 107.44(14) . . ? C13A C12A N1A 124.92(8) . . ? C13A C12A C17A 119.31(8) . . ? N1A C12A C17A 115.76(8) . . ? C14A C13A C12A 120.59(9) . . ? C13A C14A C15A 119.98(9) . . ? C16A C15A C14A 120.32(9) . . ? C15A C16A C17A 120.56(9) . . ? C16A C17A C12A 119.21(8) . . ? C16A C17A N2A 125.35(8) . . ? C12A C17A N2A 115.44(7) . . ? N2A C18A C19A 126.88(8) . . ? C20A C19A C18A 114.78(8) . . ? C20A C19A C24A 120.37(8) . . ? C18A C19A C24A 124.84(8) . . ? C21A C20A C19A 121.10(9) . . ? C20A C21A C22A 118.77(10) . . ? C23A C22A C21A 123.63(9) . . ? C22A C23A C24A 118.35(8) . . ? C22A C23A C25A 121.20(8) . . ? C24A C23A C25A 120.44(8) . . ? O2A C24A C19A 122.65(8) . . ? O2A C24A C23A 119.60(8) . . ? C19A C24A C23A 117.75(8) . . ? C23A C25A C28A 112.13(9) . . ? C23A C25A C27A 110.32(7) . . ? C28A C25A C27A 107.49(9) . . ? C23A C25A C26A 110.48(8) . . ? C28A C25A C26A 106.91(8) . . ? C27A C25A C26A 109.39(9) . . ? O3A C29A C30A 93.32(9) . . ? O3A C29A C30' 88.56(8) . . ? C30A C29A C30' 26.76(10) . . ? C32A C30A C33A 113.40(16) . . ? C32A C30A C31A 110.73(16) . . ? C33A C30A C31A 115.08(17) . . ? C32A C30A C29A 107.69(17) . . ? C33A C30A C29A 120.20(15) . . ? C31A C30A C29A 86.84(12) . . ? C30A C31A O3A 88.44(13) . . ? O4A C32A C30A 112.74(18) . . ? C33' C30' C32' 114.62(16) . . ? C33' C30' C31' 115.51(17) . . ? C32' C30' C31' 109.54(16) . . ? C33' C30' C29A 116.43(17) . . ? C32' C30' C29A 114.02(15) . . ? C31' C30' C29A 82.64(12) . . ? O3A C31' C30' 93.43(13) . . ? O4' C32' C30' 109.31(16) . . ? O1B C1B C6B 122.73(8) . . ? O1B C1B C2B 118.88(7) . . ? C6B C1B C2B 118.38(8) . . ? C3B C2B C1B 118.16(8) . . ? C3B C2B C8B 121.92(8) . . ? C1B C2B C8B 119.88(7) . . ? C2B C3B C4B 123.42(9) . . ? C5B C4B C3B 118.87(8) . . ? C4B C5B C6B 121.30(8) . . ? C5B C6B C7B 115.55(7) . . ? C5B C6B C1B 119.85(8) . . ? C7B C6B C1B 124.54(8) . . ? N1B C7B C6B 126.37(7) . . ? C9B C8B C11B 107.43(8) . . ? C9B C8B C2B 111.97(8) . . ? C11B C8B C2B 109.52(8) . . ? C9B C8B C10B 106.44(8) . . ? C11B C8B C10B 109.99(8) . . ? C2B C8B C10B 111.38(8) . . ? C13B C12B C17B 119.02(8) . . ? C13B C12B N1B 124.85(8) . . ? C17B C12B N1B 116.06(7) . . ? C14B C13B C12B 120.26(9) . . ? C13B C14B C15B 120.72(8) . . ? C16B C15B C14B 119.82(10) . . ? C15B C16B C17B 120.49(9) . . ? C16B C17B C12B 119.67(8) . . ? C16B C17B N2B 124.83(8) . . ? C12B C17B N2B 115.47(8) . . ? N2B C18B C19B 126.09(8) . . ? C20B C19B C24B 120.07(7) . . ? C20B C19B C18B 115.20(8) . . ? C24B C19B C18B 124.66(8) . . ? C21B C20B C19B 121.21(9) . . ? C20B C21B C22B 118.93(9) . . ? C23B C22B C21B 123.28(8) . . ? C22B C23B C24B 118.46(8) . . ? C22B C23B C25B 121.05(8) . . ? C24B C23B C25B 120.50(8) . . ? O2B C24B C19B 122.42(7) . . ? O2B C24B C23B 119.64(8) . . ? C19B C24B C23B 117.93(8) . . ? C28B C25B C23B 111.88(8) . . ? C28B C25B C27B 107.65(8) . . ? C23B C25B C27B 110.16(8) . . ? C28B C25B C26B 107.07(8) . . ? C23B C25B C26B 110.15(7) . . ? C27B C25B C26B 109.85(8) . . ? O3B C29B C30B 91.61(7) . . ? C33B C30B C32B 111.71(8) . . ? C33B C30B C29B 116.33(9) . . ? C32B C30B C29B 112.86(8) . . ? C33B C30B C31B 116.67(8) . . ? C32B C30B C31B 111.70(8) . . ? C29B C30B C31B 85.16(6) . . ? O3B C31B C30B 91.27(7) . . ? O4B C32B C30B 109.89(9) . . ? C7A N1A C12A 121.06(8) . . ? C7A N1A Zn1A 124.56(6) . . ? C12A N1A Zn1A 114.11(6) . . ? C18A N2A C17A 121.73(7) . . ? C18A N2A Zn1A 123.64(6) . . ? C17A N2A Zn1A 114.58(6) . . ? C7B N1B C12B 122.79(7) . . ? C7B N1B Zn1B 124.09(6) . . ? C12B N1B Zn1B 113.04(5) . . ? C18B N2B C17B 122.04(8) . . ? C18B N2B Zn1B 124.96(6) . . ? C17B N2B Zn1B 112.99(6) . . ? C1A O1A Zn1A 131.39(6) . . ? C24A O2A Zn1A 130.82(6) . . ? C31' O3A C29A 92.84(9) . . ? C31' O3A C31A 29.28(12) . . ? C29A O3A C31A 87.50(8) . . ? C31' O3A Zn1A 130.09(10) . . ? C29A O3A Zn1A 120.42(6) . . ? C31A O3A Zn1A 110.31(8) . . ? C1B O1B Zn1B 130.64(6) . . ? C24B O2B Zn1B 131.05(6) . . ? C29B O3B C31B 90.41(6) . . ? C29B O3B Zn1B 122.99(6) . . ? C31B O3B Zn1B 115.97(6) . . ? O2A Zn1A O1A 98.86(3) . . ? O2A Zn1A N2A 91.00(3) . . ? O1A Zn1A N2A 164.61(3) . . ? O2A Zn1A N1A 164.78(3) . . ? O1A Zn1A N1A 89.29(3) . . ? N2A Zn1A N1A 78.60(3) . . ? O2A Zn1A O3A 95.85(3) . . ? O1A Zn1A O3A 94.13(3) . . ? N2A Zn1A O3A 96.60(3) . . ? N1A Zn1A O3A 96.36(3) . . ? O1B Zn1B O2B 96.96(3) . . ? O1B Zn1B N1B 91.04(3) . . ? O2B Zn1B N1B 157.09(3) . . ? O1B Zn1B N2B 170.02(3) . . ? O2B Zn1B N2B 90.09(3) . . ? N1B Zn1B N2B 79.84(3) . . ? O1B Zn1B O3B 94.14(3) . . ? O2B Zn1B O3B 99.24(3) . . ? N1B Zn1B O3B 101.56(3) . . ? N2B Zn1B O3B 91.68(3) . . ? C1C O1C C3C 90.26(14) . . ? C1C O1C C4C 60.66(13) . 2_655 ? C3C O1C C4C 65.53(13) . 2_655 ? C1C O1C O2C 47.67(12) . 2_655 ? C3C O1C O2C 112.69(13) . 2_655 ? C4C O1C O2C 49.08(11) 2_655 2_655 ? C1C O2C C4C 72.30(15) 2_655 . ? C1C O2C O1C 55.32(13) 2_655 2_655 ? C4C O2C O1C 65.17(13) . 2_655 ? O2C C1C O1C 77.01(15) 2_655 . ? O2C C1C C2C 109.01(16) 2_655 . ? O1C C1C C2C 95.21(14) . . ? O2C C1C C4C 57.32(14) 2_655 2_655 ? O1C C1C C4C 67.68(14) . 2_655 ? C2C C1C C4C 54.94(11) . 2_655 ? O2C C1C C5C 154.4(2) 2_655 2_655 ? O1C C1C C5C 87.05(16) . 2_655 ? C2C C1C C5C 52.10(12) . 2_655 ? C4C C1C C5C 98.22(17) 2_655 2_655 ? C5C C2C C5C 63.5(2) . 2_655 ? C5C C2C C4C 177.55(15) . 2_655 ? C5C C2C C4C 118.51(13) 2_655 2_655 ? C5C C2C C4C 118.50(13) . . ? C5C C2C C4C 177.56(15) 2_655 . ? C4C C2C C4C 59.54(18) 2_655 . ? C5C C2C C1C 117.25(16) . . ? C5C C2C C1C 68.91(14) 2_655 . ? C4C C2C C1C 63.21(12) 2_655 . ? C4C C2C C1C 110.52(14) . . ? C5C C2C C1C 68.91(14) . 2_655 ? C5C C2C C1C 117.26(16) 2_655 2_655 ? C4C C2C C1C 110.52(14) 2_655 2_655 ? C4C C2C C1C 63.21(12) . 2_655 ? C1C C2C C1C 173.39(19) . 2_655 ? C5C C2C C3C 115.08(16) . . ? C5C C2C C3C 68.19(14) 2_655 . ? C4C C2C C3C 67.32(13) 2_655 . ? C4C C2C C3C 109.41(14) . . ? C1C C2C C3C 79.67(11) . . ? C1C C2C C3C 100.13(11) 2_655 . ? C5C C2C C3C 68.19(14) . 2_655 ? C5C C2C C3C 115.08(16) 2_655 2_655 ? C4C C2C C3C 109.40(14) 2_655 2_655 ? C4C C2C C3C 67.32(13) . 2_655 ? C1C C2C C3C 100.12(11) . 2_655 ? C1C C2C C3C 79.67(11) 2_655 2_655 ? C3C C2C C3C 176.5(2) . 2_655 ? O1C C3C C2C 92.30(14) . . ? O1C C3C C4C 63.85(13) . 2_655 ? C2C C3C C4C 51.84(11) . 2_655 ? O1C C3C C5C 85.81(16) . 2_655 ? C2C C3C C5C 51.13(11) . 2_655 ? C4C C3C C5C 93.20(16) 2_655 2_655 ? O2C C4C C4C 125.4(3) . 2_655 ? O2C C4C C2C 109.03(16) . . ? C4C C4C C2C 60.23(9) 2_655 . ? O2C C4C C1C 50.39(13) . 2_655 ? C4C C4C C1C 109.98(17) 2_655 2_655 ? C2C C4C C1C 61.85(11) . 2_655 ? O2C C4C O1C 65.74(13) . 2_655 ? C4C C4C O1C 149.32(10) 2_655 2_655 ? C2C C4C O1C 89.40(13) . 2_655 ? C1C C4C O1C 51.65(11) 2_655 2_655 ? O2C C4C C3C 114.37(17) . 2_655 ? C4C C4C C3C 105.13(17) 2_655 2_655 ? C2C C4C C3C 60.84(11) . 2_655 ? C1C C4C C3C 76.41(15) 2_655 2_655 ? O1C C4C C3C 50.62(11) 2_655 2_655 ? C2C C5C C5C 58.25(10) . 2_655 ? C2C C5C C1C 59.00(12) . 2_655 ? C5C C5C C1C 105.60(19) 2_655 2_655 ? C2C C5C C3C 60.69(12) . 2_655 ? C5C C5C C3C 105.6(2) 2_655 2_655 ? C1C C5C C3C 73.05(14) 2_655 2_655 ? 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 O1A C1A C2A C3A -178.47(11) . . . . ? C6A C1A C2A C3A 1.75(16) . . . . ? O1A C1A C2A C8A 2.12(17) . . . . ? C6A C1A C2A C8A -177.67(11) . . . . ? C1A C2A C3A C4A -1.67(19) . . . . ? C8A C2A C3A C4A 177.74(13) . . . . ? C2A C3A C4A C5A 0.26(18) . . . . ? C3A C4A C5A C6A 1.03(15) . . . . ? C4A C5A C6A C7A 176.66(9) . . . . ? C4A C5A C6A C1A -0.86(14) . . . . ? O1A C1A C6A C5A 179.67(9) . . . . ? C2A C1A C6A C5A -0.55(14) . . . . ? O1A C1A C6A C7A 2.39(16) . . . . ? C2A C1A C6A C7A -177.83(9) . . . . ? C5A C6A C7A N1A -175.39(9) . . . . ? C1A C6A C7A N1A 2.02(15) . . . . ? C3A C2A C8A C10A -117.82(14) . . . . ? C1A C2A C8A C10A 61.58(17) . . . . ? C3A C2A C8A C11A 0.9(2) . . . . ? C1A C2A C8A C11A -179.72(13) . . . . ? C3A C2A C8A C9A 120.51(13) . . . . ? C1A C2A C8A C9A -60.09(15) . . . . ? N1A C12A C13A C14A -177.35(8) . . . . ? C17A C12A C13A C14A 1.87(13) . . . . ? C12A C13A C14A C15A -1.53(14) . . . . ? C13A C14A C15A C16A 0.08(15) . . . . ? C14A C15A C16A C17A 1.01(15) . . . . ? C15A C16A C17A C12A -0.65(14) . . . . ? C15A C16A C17A N2A 178.26(9) . . . . ? C13A C12A C17A C16A -0.78(12) . . . . ? N1A C12A C17A C16A 178.51(8) . . . . ? C13A C12A C17A N2A -179.79(7) . . . . ? N1A C12A C17A N2A -0.50(11) . . . . ? N2A C18A C19A C20A 175.49(9) . . . . ? N2A C18A C19A C24A -3.67(15) . . . . ? C18A C19A C20A C21A -179.50(9) . . . . ? C24A C19A C20A C21A -0.30(15) . . . . ? C19A C20A C21A C22A -1.22(16) . . . . ? C20A C21A C22A C23A 1.43(16) . . . . ? C21A C22A C23A C24A -0.05(15) . . . . ? C21A C22A C23A C25A 179.47(10) . . . . ? C20A C19A C24A O2A -179.19(9) . . . . ? C18A C19A C24A O2A -0.07(14) . . . . ? C20A C19A C24A C23A 1.64(13) . . . . ? C18A C19A C24A C23A -179.24(8) . . . . ? C22A C23A C24A O2A 179.35(9) . . . . ? C25A C23A C24A O2A -0.18(13) . . . . ? C22A C23A C24A C19A -1.45(13) . . . . ? C25A C23A C24A C19A 179.02(8) . . . . ? C22A C23A C25A C28A 1.89(13) . . . . ? C24A C23A C25A C28A -178.60(9) . . . . ? C22A C23A C25A C27A -117.88(10) . . . . ? C24A C23A C25A C27A 61.63(11) . . . . ? C22A C23A C25A C26A 121.04(10) . . . . ? C24A C23A C25A C26A -59.45(12) . . . . ? O3A C29A C30A C32A -95.26(13) . . . . ? C30' C29A C30A C32A -15.10(16) . . . . ? O3A C29A C30A C33A 132.83(15) . . . . ? C30' C29A C30A C33A -147.0(3) . . . . ? O3A C29A C30A C31A 15.51(12) . . . . ? C30' C29A C30A C31A 95.7(2) . . . . ? C32A C30A C31A O3A 93.59(17) . . . . ? C33A C30A C31A O3A -136.17(16) . . . . ? C29A C30A C31A O3A -14.14(11) . . . . ? C33A C30A C32A O4A 75.1(2) . . . . ? C31A C30A C32A O4A -153.77(19) . . . . ? C29A C30A C32A O4A -60.4(2) . . . . ? O3A C29A C30' C33' 125.94(15) . . . . ? C30A C29A C30' C33' 25.66(18) . . . . ? O3A C29A C30' C32' -97.10(13) . . . . ? C30A C29A C30' C32' 162.6(3) . . . . ? O3A C29A C30' C31' 11.06(12) . . . . ? C30A C29A C30' C31' -89.2(2) . . . . ? C33' C30' C31' O3A -127.76(19) . . . . ? C32' C30' C31' O3A 101.00(17) . . . . ? C29A C30' C31' O3A -11.94(13) . . . . ? C33' C30' C32' O4' 65.2(2) . . . . ? C31' C30' C32' O4' -163.07(17) . . . . ? C29A C30' C32' O4' -72.53(19) . . . . ? O1B C1B C2B C3B 178.26(9) . . . . ? C6B C1B C2B C3B -0.64(13) . . . . ? O1B C1B C2B C8B 0.62(13) . . . . ? C6B C1B C2B C8B -178.28(8) . . . . ? C1B C2B C3B C4B -0.26(14) . . . . ? C8B C2B C3B C4B 177.32(9) . . . . ? C2B C3B C4B C5B 0.14(15) . . . . ? C3B C4B C5B C6B 0.93(15) . . . . ? C4B C5B C6B C7B -179.00(9) . . . . ? C4B C5B C6B C1B -1.85(14) . . . . ? O1B C1B C6B C5B -177.19(9) . . . . ? C2B C1B C6B C5B 1.67(13) . . . . ? O1B C1B C6B C7B -0.30(14) . . . . ? C2B C1B C6B C7B 178.56(8) . . . . ? C5B C6B C7B N1B 179.80(9) . . . . ? C1B C6B C7B N1B 2.79(15) . . . . ? C3B C2B C8B C9B 7.42(13) . . . . ? C1B C2B C8B C9B -175.03(9) . . . . ? C3B C2B C8B C11B -111.64(10) . . . . ? C1B C2B C8B C11B 65.91(11) . . . . ? C3B C2B C8B C10B 126.47(10) . . . . ? C1B C2B C8B C10B -55.98(12) . . . . ? C17B C12B C13B C14B -0.61(14) . . . . ? N1B C12B C13B C14B 176.16(9) . . . . ? C12B C13B C14B C15B -0.22(16) . . . . ? C13B C14B C15B C16B 0.65(17) . . . . ? C14B C15B C16B C17B -0.23(17) . . . . ? C15B C16B C17B C12B -0.61(15) . . . . ? C15B C16B C17B N2B -178.76(10) . . . . ? C13B C12B C17B C16B 1.02(14) . . . . ? N1B C12B C17B C16B -176.03(9) . . . . ? C13B C12B C17B N2B 179.34(8) . . . . ? N1B C12B C17B N2B 2.29(12) . . . . ? N2B C18B C19B C20B -177.86(9) . . . . ? N2B C18B C19B C24B 5.09(15) . . . . ? C24B C19B C20B C21B 0.32(14) . . . . ? C18B C19B C20B C21B -176.88(9) . . . . ? C19B C20B C21B C22B 1.85(15) . . . . ? C20B C21B C22B C23B -1.12(15) . . . . ? C21B C22B C23B C24B -1.77(14) . . . . ? C21B C22B C23B C25B 178.30(9) . . . . ? C20B C19B C24B O2B 177.21(9) . . . . ? C18B C19B C24B O2B -5.87(14) . . . . ? C20B C19B C24B C23B -3.16(13) . . . . ? C18B C19B C24B C23B 173.76(8) . . . . ? C22B C23B C24B O2B -176.54(9) . . . . ? C25B C23B C24B O2B 3.39(13) . . . . ? C22B C23B C24B C19B 3.82(13) . . . . ? C25B C23B C24B C19B -176.25(8) . . . . ? C22B C23B C25B C28B -3.95(13) . . . . ? C24B C23B C25B C28B 176.12(9) . . . . ? C22B C23B C25B C27B 115.75(10) . . . . ? C24B C23B C25B C27B -64.18(11) . . . . ? C22B C23B C25B C26B -122.92(9) . . . . ? C24B C23B C25B C26B 57.15(11) . . . . ? O3B C29B C30B C33B 126.62(9) . . . . ? O3B C29B C30B C32B -102.34(8) . . . . ? O3B C29B C30B C31B 9.19(7) . . . . ? C33B C30B C31B O3B -126.28(9) . . . . ? C32B C30B C31B O3B 103.52(8) . . . . ? C29B C30B C31B O3B -9.18(7) . . . . ? C33B C30B C32B O4B 57.69(12) . . . . ? C29B C30B C32B O4B -75.62(10) . . . . ? C31B C30B C32B O4B -169.59(8) . . . . ? C6A C7A N1A C12A 175.89(8) . . . . ? C6A C7A N1A Zn1A 2.32(13) . . . . ? C13A C12A N1A C7A 14.40(13) . . . . ? C17A C12A N1A C7A -164.85(8) . . . . ? C13A C12A N1A Zn1A -171.40(7) . . . . ? C17A C12A N1A Zn1A 9.35(9) . . . . ? C19A C18A N2A C17A -177.35(8) . . . . ? C19A C18A N2A Zn1A 5.42(13) . . . . ? C16A C17A N2A C18A -5.10(13) . . . . ? C12A C17A N2A C18A 173.85(8) . . . . ? C16A C17A N2A Zn1A 172.36(7) . . . . ? C12A C17A N2A Zn1A -8.69(9) . . . . ? C6B C7B N1B C12B -174.79(9) . . . . ? C6B C7B N1B Zn1B 1.76(13) . . . . ? C13B C12B N1B C7B 9.94(14) . . . . ? C17B C12B N1B C7B -173.20(8) . . . . ? C13B C12B N1B Zn1B -166.96(8) . . . . ? C17B C12B N1B Zn1B 9.90(10) . . . . ? C19B C18B N2B C17B -177.93(8) . . . . ? C19B C18B N2B Zn1B 3.09(13) . . . . ? C16B C17B N2B C18B -14.21(14) . . . . ? C12B C17B N2B C18B 167.58(8) . . . . ? C16B C17B N2B Zn1B 164.89(8) . . . . ? C12B C17B N2B Zn1B -13.33(10) . . . . ? C6A C1A O1A Zn1A -11.76(16) . . . . ? C2A C1A O1A Zn1A 168.47(8) . . . . ? C19A C24A O2A Zn1A 1.24(13) . . . . ? C23A C24A O2A Zn1A -179.60(6) . . . . ? C30' C31' O3A C29A 12.65(14) . . . . ? C30' C31' O3A C31A 92.4(2) . . . . ? C30' C31' O3A Zn1A 147.44(10) . . . . ? C30A C29A O3A C31' 13.90(14) . . . . ? C30' C29A O3A C31' -12.45(14) . . . . ? C30A C29A O3A C31A -14.90(12) . . . . ? C30' C29A O3A C31A -41.25(11) . . . . ? C30A C29A O3A Zn1A -127.07(9) . . . . ? C30' C29A O3A Zn1A -153.42(9) . . . . ? C30A C31A O3A C31' -85.4(2) . . . . ? C30A C31A O3A C29A 14.94(12) . . . . ? C30A C31A O3A Zn1A 136.57(10) . . . . ? C6B C1B O1B Zn1B -7.13(13) . . . . ? C2B C1B O1B Zn1B 174.02(6) . . . . ? C19B C24B O2B Zn1B -2.03(13) . . . . ? C23B C24B O2B Zn1B 178.35(6) . . . . ? C30B C29B O3B C31B -9.63(7) . . . . ? C30B C29B O3B Zn1B -131.42(6) . . . . ? C30B C31B O3B C29B 9.58(7) . . . . ? C30B C31B O3B Zn1B 137.11(5) . . . . ? C24A O2A Zn1A O1A 168.34(8) . . . . ? C24A O2A Zn1A N2A 0.20(8) . . . . ? C24A O2A Zn1A N1A 46.64(16) . . . . ? C24A O2A Zn1A O3A -96.54(8) . . . . ? C1A O1A Zn1A O2A -154.84(10) . . . . ? C1A O1A Zn1A N2A -25.57(19) . . . . ? C1A O1A Zn1A N1A 12.26(10) . . . . ? C1A O1A Zn1A O3A 108.58(10) . . . . ? C18A N2A Zn1A O2A -3.37(7) . . . . ? C17A N2A Zn1A O2A 179.22(6) . . . . ? C18A N2A Zn1A O1A -133.46(12) . . . . ? C17A N2A Zn1A O1A 49.14(15) . . . . ? C18A N2A Zn1A N1A -172.18(7) . . . . ? C17A N2A Zn1A N1A 10.42(6) . . . . ? C18A N2A Zn1A O3A 92.63(7) . . . . ? C17A N2A Zn1A O3A -84.77(6) . . . . ? C7A N1A Zn1A O2A 115.66(12) . . . . ? C12A N1A Zn1A O2A -58.31(14) . . . . ? C7A N1A Zn1A O1A -7.12(7) . . . . ? C12A N1A Zn1A O1A 178.91(6) . . . . ? C7A N1A Zn1A N2A 163.32(8) . . . . ? C12A N1A Zn1A N2A -10.65(6) . . . . ? C7A N1A Zn1A O3A -101.20(7) . . . . ? C12A N1A Zn1A O3A 84.83(6) . . . . ? C31' O3A Zn1A O2A -177.72(14) . . . . ? C29A O3A Zn1A O2A -53.01(7) . . . . ? C31A O3A Zn1A O2A -152.42(8) . . . . ? C31' O3A Zn1A O1A -78.36(14) . . . . ? C29A O3A Zn1A O1A 46.35(7) . . . . ? C31A O3A Zn1A O1A -53.06(8) . . . . ? C31' O3A Zn1A N2A 90.59(14) . . . . ? C29A O3A Zn1A N2A -144.70(7) . . . . ? C31A O3A Zn1A N2A 115.89(8) . . . . ? C31' O3A Zn1A N1A 11.39(14) . . . . ? C29A O3A Zn1A N1A 136.10(7) . . . . ? C31A O3A Zn1A N1A 36.69(8) . . . . ? C1B O1B Zn1B O2B -149.70(8) . . . . ? C1B O1B Zn1B N1B 8.78(8) . . . . ? C1B O1B Zn1B N2B -15.1(2) . . . . ? C1B O1B Zn1B O3B 110.45(8) . . . . ? C24B O2B Zn1B O1B 179.98(8) . . . . ? C24B O2B Zn1B N1B 70.35(12) . . . . ? C24B O2B Zn1B N2B 7.06(8) . . . . ? C24B O2B Zn1B O3B -84.66(8) . . . . ? C7B N1B Zn1B O1B -5.84(8) . . . . ? C12B N1B Zn1B O1B 171.02(6) . . . . ? C7B N1B Zn1B O2B 104.92(10) . . . . ? C12B N1B Zn1B O2B -78.23(10) . . . . ? C7B N1B Zn1B N2B 170.08(8) . . . . ? C12B N1B Zn1B N2B -13.06(6) . . . . ? C7B N1B Zn1B O3B -100.27(8) . . . . ? C12B N1B Zn1B O3B 76.58(6) . . . . ? C18B N2B Zn1B O1B -142.41(16) . . . . ? C17B N2B Zn1B O1B 38.5(2) . . . . ? C18B N2B Zn1B O2B -7.33(8) . . . . ? C17B N2B Zn1B O2B 173.60(6) . . . . ? C18B N2B Zn1B N1B -166.65(8) . . . . ? C17B N2B Zn1B N1B 14.29(6) . . . . ? C18B N2B Zn1B O3B 91.91(8) . . . . ? C17B N2B Zn1B O3B -87.16(6) . . . . ? C29B O3B Zn1B O1B 149.03(6) . . . . ? C31B O3B Zn1B O1B 40.01(6) . . . . ? C29B O3B Zn1B O2B 51.28(7) . . . . ? C31B O3B Zn1B O2B -57.74(6) . . . . ? C29B O3B Zn1B N1B -119.06(6) . . . . ? C31B O3B Zn1B N1B 131.93(6) . . . . ? C29B O3B Zn1B N2B -39.09(6) . . . . ? C31B O3B Zn1B N2B -148.10(6) . . . . ? C3C O1C C1C O2C -121.17(16) . . . 2_655 ? C4C O1C C1C O2C -59.71(13) 2_655 . . 2_655 ? C3C O1C C1C C2C -12.84(16) . . . . ? C4C O1C C1C C2C 48.63(12) 2_655 . . . ? O2C O1C C1C C2C 108.34(16) 2_655 . . . ? C3C O1C C1C C4C -61.46(15) . . . 2_655 ? O2C O1C C1C C4C 59.71(13) 2_655 . . 2_655 ? C3C O1C C1C C5C 38.67(16) . . . 2_655 ? C4C O1C C1C C5C 100.13(15) 2_655 . . 2_655 ? O2C O1C C1C C5C 159.84(18) 2_655 . . 2_655 ? O2C C1C C2C C5C -157.27(18) 2_655 . . . ? O1C C1C C2C C5C 124.70(17) . . . . ? C4C C1C C2C C5C -177.30(17) 2_655 . . . ? C5C C1C C2C C5C 42.5(3) 2_655 . . . ? O2C C1C C2C C5C 160.2(2) 2_655 . . 2_655 ? O1C C1C C2C C5C 82.15(17) . . . 2_655 ? C4C C1C C2C C5C 140.15(17) 2_655 . . 2_655 ? O2C C1C C2C C4C 20.04(16) 2_655 . . 2_655 ? O1C C1C C2C C4C -58.00(15) . . . 2_655 ? C5C C1C C2C C4C -140.15(17) 2_655 . . 2_655 ? O2C C1C C2C C4C -17.3(2) 2_655 . . . ? O1C C1C C2C C4C -95.31(16) . . . . ? C4C C1C C2C C4C -37.3(2) 2_655 . . . ? C5C C1C C2C C4C -177.46(16) 2_655 . . . ? O2C C1C C2C C1C 0.91(15) 2_655 . . 2_655 ? O1C C1C C2C C1C -77.13(11) . . . 2_655 ? C4C C1C C2C C1C -19.13(11) 2_655 . . 2_655 ? C5C C1C C2C C1C -159.28(13) 2_655 . . 2_655 ? O2C C1C C2C C3C 89.73(18) 2_655 . . . ? O1C C1C C2C C3C 11.69(15) . . . . ? C4C C1C C2C C3C 69.69(14) 2_655 . . . ? C5C C1C C2C C3C -70.46(15) 2_655 . . . ? O2C C1C C2C C3C -86.70(19) 2_655 . . 2_655 ? O1C C1C C2C C3C -164.73(15) . . . 2_655 ? C4C C1C C2C C3C -106.73(16) 2_655 . . 2_655 ? C5C C1C C2C C3C 113.12(17) 2_655 . . 2_655 ? C1C O1C C3C C2C 12.40(15) . . . . ? C4C O1C C3C C2C -44.89(12) 2_655 . . . ? O2C O1C C3C C2C -30.87(18) 2_655 . . . ? C1C O1C C3C C4C 57.29(14) . . . 2_655 ? O2C O1C C3C C4C 14.02(14) 2_655 . . 2_655 ? C1C O1C C3C C5C -38.35(15) . . . 2_655 ? C4C O1C C3C C5C -95.64(14) 2_655 . . 2_655 ? O2C O1C C3C C5C -81.62(16) 2_655 . . 2_655 ? C5C C2C C3C O1C -126.85(16) . . . . ? C5C C2C C3C O1C -82.75(17) 2_655 . . . ? C4C C2C C3C O1C 53.67(14) 2_655 . . . ? C4C C2C C3C O1C 96.80(15) . . . . ? C1C C2C C3C O1C -11.47(14) . . . . ? C1C C2C C3C O1C 161.81(15) 2_655 . . . ? C3C C2C C3C O1C 75.44(12) 2_655 . . . ? C5C C2C C3C C4C 179.48(16) . . . 2_655 ? C5C C2C C3C C4C -136.42(16) 2_655 . . 2_655 ? C4C C2C C3C C4C 43.1(2) . . . 2_655 ? C1C C2C C3C C4C -65.14(13) . . . 2_655 ? C1C C2C C3C C4C 108.14(15) 2_655 . . 2_655 ? C3C C2C C3C C4C 21.77(10) 2_655 . . 2_655 ? C5C C2C C3C C5C -44.1(3) . . . 2_655 ? C4C C2C C3C C5C 136.42(16) 2_655 . . 2_655 ? C4C C2C C3C C5C 179.55(16) . . . 2_655 ? C1C C2C C3C C5C 71.28(15) . . . 2_655 ? C1C C2C C3C C5C -115.44(17) 2_655 . . 2_655 ? C3C C2C C3C C5C 158.19(13) 2_655 . . 2_655 ? C1C O2C C4C C4C 87.51(15) 2_655 . . 2_655 ? O1C O2C C4C C4C 146.82(12) 2_655 . . 2_655 ? C1C O2C C4C C2C 21.04(16) 2_655 . . . ? O1C O2C C4C C2C 80.35(15) 2_655 . . . ? O1C O2C C4C C1C 59.31(13) 2_655 . . 2_655 ? C1C O2C C4C O1C -59.31(13) 2_655 . . 2_655 ? C1C O2C C4C C3C -44.78(18) 2_655 . . 2_655 ? O1C O2C C4C C3C 14.53(14) 2_655 . . 2_655 ? C5C C2C C4C O2C -61.2(2) . . . . ? C5C C2C C4C O2C 83(4) 2_655 . . . ? C4C C2C C4C O2C 120.5(3) 2_655 . . . ? C1C C2C C4C O2C 159.41(15) . . . . ? C1C C2C C4C O2C -18.28(15) 2_655 . . . ? C3C C2C C4C O2C 73.49(18) . . . . ? C3C C2C C4C O2C -107.90(18) 2_655 . . . ? C5C C2C C4C C4C 178.31(18) . . . 2_655 ? C5C C2C C4C C4C -37(4) 2_655 . . 2_655 ? C1C C2C C4C C4C 38.9(2) . . . 2_655 ? C1C C2C C4C C4C -138.8(2) 2_655 . . 2_655 ? C3C C2C C4C C4C -47.0(2) . . . 2_655 ? C3C C2C C4C C4C 131.6(2) 2_655 . . 2_655 ? C5C C2C C4C C1C -42.88(19) . . . 2_655 ? C5C C2C C4C C1C 102(4) 2_655 . . 2_655 ? C4C C2C C4C C1C 138.8(2) 2_655 . . 2_655 ? C1C C2C C4C C1C 177.69(7) . . . 2_655 ? C3C C2C C4C C1C 91.77(13) . . . 2_655 ? C3C C2C C4C C1C -89.62(13) 2_655 . . 2_655 ? C5C C2C C4C O1C 2.8(2) . . . 2_655 ? C5C C2C C4C O1C 147(4) 2_655 . . 2_655 ? C4C C2C C4C O1C -175.5(3) 2_655 . . 2_655 ? C1C C2C C4C O1C -136.58(12) . . . 2_655 ? C1C C2C C4C O1C 45.72(12) 2_655 . . 2_655 ? C3C C2C C4C O1C 137.50(12) . . . 2_655 ? C3C C2C C4C O1C -43.89(12) 2_655 . . 2_655 ? C5C C2C C4C C3C 46.74(18) . . . 2_655 ? C5C C2C C4C C3C -169(4) 2_655 . . 2_655 ? C4C C2C C4C C3C -131.6(2) 2_655 . . 2_655 ? C1C C2C C4C C3C -92.69(13) . . . 2_655 ? C1C C2C C4C C3C 89.62(13) 2_655 . . 2_655 ? C3C C2C C4C C3C -178.61(8) . . . 2_655 ? C4C C2C C5C C5C -145(3) 2_655 . . 2_655 ? C4C C2C C5C C5C 178.41(17) . . . 2_655 ? C1C C2C C5C C5C -44.8(3) . . . 2_655 ? C1C C2C C5C C5C 137.8(3) 2_655 . . 2_655 ? C3C C2C C5C C5C 46.2(3) . . . 2_655 ? C3C C2C C5C C5C -135.2(3) 2_655 . . 2_655 ? C5C C2C C5C C1C -137.8(3) 2_655 . . 2_655 ? C4C C2C C5C C1C 77(4) 2_655 . . 2_655 ? C4C C2C C5C C1C 40.61(17) . . . 2_655 ? C1C C2C C5C C1C 177.37(8) . . . 2_655 ? C3C C2C C5C C1C -91.58(13) . . . 2_655 ? C3C C2C C5C C1C 86.98(13) 2_655 . . 2_655 ? C5C C2C C5C C3C 135.2(3) 2_655 . . 2_655 ? C4C C2C C5C C3C -10(4) 2_655 . . 2_655 ? C4C C2C C5C C3C -46.37(17) . . . 2_655 ? C1C C2C C5C C3C 90.39(14) . . . 2_655 ? C1C C2C C5C C3C -86.98(13) 2_655 . . 2_655 ? C3C C2C C5C C3C -178.56(8) . . . 2_655 ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.833 _refine_diff_density_min -0.714 _refine_diff_density_rms 0.093