# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2011 data_global _journal_coden_Cambridge 182 _journal_volume ? _journal_page_first ? _journal_year ? loop_ _publ_author_name 'Grubel, Katarzyna' 'Laughlin, Brynna' 'Maltais, Thora' 'Smith, Rhett' 'Arif, Atta' 'Berreau, Lisa' _publ_contact_author_name 'Prof. Lisa Berreau' _publ_contact_author_email lisa.berreau@usu.edu _publ_section_title ; Photochemically-induced dioxygenase-type CO-release reactivity of Group 12 metal flavonolate complexes ; # Attachment '- CombinedCIF copy.txt' data_usu204 _database_code_depnum_ccdc_archive 'CCDC 832449' #TrackingRef '- CombinedCIF copy.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C45 H35 Cd N4 O3, Cl O4' _chemical_formula_sum 'C45 H35 Cd Cl N4 O7' _chemical_formula_weight 891.62 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' 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' Cl Cl 0.1484 0.1585 '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' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' 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 11.4616(2) _cell_length_b 16.3861(3) _cell_length_c 20.8770(4) _cell_angle_alpha 90.00 _cell_angle_beta 95.0205(11) _cell_angle_gamma 90.00 _cell_volume 3905.89(12) _cell_formula_units_Z 4 _cell_measurement_temperature 150(1) _cell_measurement_reflns_used 8311 _cell_measurement_theta_min 1.018 _cell_measurement_theta_max 27.485 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.516 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1816 _exptl_absorpt_coefficient_mu 0.686 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8310 _exptl_absorpt_correction_T_max 0.9161 _exptl_absorpt_process_details 'DENZO-SMN (Otwinowski & Minor, 1997)' _exptl_special_details ; The program Denzo-SMN (Otwinowski & Minor, 1997) uses a scaling algorithm (Fox & Holmes, 1966) which effectively corrects for absorption effects. High redundancy data were used in the scaling program hence the 'multi-scan' code word was used. No transmission coefficients are available from the program (only scale factors for each frame). The scale factors in the experimental table are calculated from the 'size' command in the SHELXL-97 input file. ; _diffrn_ambient_temperature 150(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD Diffractometer' _diffrn_measurement_method 'Phi and Omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15965 _diffrn_reflns_av_R_equivalents 0.0303 _diffrn_reflns_av_sigmaI/netI 0.0543 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.96 _diffrn_reflns_theta_max 27.48 _reflns_number_total 8943 _reflns_number_gt 6629 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius COLLECT' _computing_cell_refinement DENZO-SMN _computing_data_reduction ENZO-SMN _computing_structure_solution SIR97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'WinGX, Ortep3' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0375P)^2^+1.0726P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00153(15) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 8943 _refine_ls_number_parameters 552 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0631 _refine_ls_R_factor_gt 0.0364 _refine_ls_wR_factor_ref 0.0859 _refine_ls_wR_factor_gt 0.0765 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_restrained_S_all 1.021 _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 Cl1 Cl 1.12025(7) 0.36783(5) 0.72052(4) 0.0512(2) Uani 1 1 d . . . Cd1 Cd 0.738195(15) 0.142631(10) 0.605534(8) 0.02421(7) Uani 1 1 d . . . O1 O 0.62056(14) 0.21043(10) 0.53454(8) 0.0256(4) Uani 1 1 d . . . O2 O 0.85203(14) 0.24183(10) 0.56650(8) 0.0295(4) Uani 1 1 d . . . O3 O 0.68054(15) 0.36691(10) 0.41862(8) 0.0312(4) Uani 1 1 d . . . N1 N 0.91533(18) 0.10483(14) 0.66159(10) 0.0320(5) Uani 1 1 d . . . N2 N 0.70580(18) 0.02244(13) 0.66982(10) 0.0290(5) Uani 1 1 d . . . N3 N 0.61547(18) 0.18499(13) 0.69083(10) 0.0272(5) Uani 1 1 d . . . N4 N 0.70721(17) 0.02093(12) 0.54057(10) 0.0262(5) Uani 1 1 d . . . C1 C 1.0114(2) 0.15210(18) 0.66458(15) 0.0404(7) Uani 1 1 d . . . H1 H 1.0054 0.2054 0.6467 0.048 Uiso 1 1 calc R . . C2 C 1.1183(3) 0.1261(2) 0.69254(17) 0.0528(9) Uani 1 1 d . . . H2 H 1.1853 0.1602 0.6928 0.063 Uiso 1 1 calc R . . C3 C 1.1262(3) 0.0500(2) 0.72004(18) 0.0590(9) Uani 1 1 d . . . H3 H 1.1987 0.0309 0.7401 0.071 Uiso 1 1 calc R . . C4 C 1.0272(3) 0.0015(2) 0.71819(15) 0.0482(8) Uani 1 1 d . . . H4 H 1.0306 -0.0509 0.7377 0.058 Uiso 1 1 calc R . . C5 C 0.9229(2) 0.03012(17) 0.68762(13) 0.0355(6) Uani 1 1 d . . . C6 C 0.8166(2) -0.02411(17) 0.67823(14) 0.0377(7) Uani 1 1 d . . . H6A H 0.8232 -0.0588 0.6399 0.045 Uiso 1 1 calc R . . H6B H 0.8147 -0.0605 0.7160 0.045 Uiso 1 1 calc R . . C7 C 0.6710(2) 0.05009(17) 0.73241(13) 0.0347(6) Uani 1 1 d . . . H7A H 0.7415 0.0676 0.7597 0.042 Uiso 1 1 calc R . . H7B H 0.6351 0.0040 0.7542 0.042 Uiso 1 1 calc R . . C8 C 0.5851(2) 0.11988(16) 0.72536(12) 0.0299(6) Uani 1 1 d . . . C9 C 0.4830(2) 0.11719(18) 0.75601(13) 0.0377(7) Uani 1 1 d . . . H9 H 0.4636 0.0702 0.7795 0.045 Uiso 1 1 calc R . . C10 C 0.4097(2) 0.18428(18) 0.75175(13) 0.0374(7) Uani 1 1 d . . . H10 H 0.3385 0.1837 0.7718 0.045 Uiso 1 1 calc R . . C11 C 0.4409(2) 0.25170(17) 0.71825(13) 0.0351(6) Uani 1 1 d . . . H11 H 0.3916 0.2984 0.7155 0.042 Uiso 1 1 calc R . . C12 C 0.5452(2) 0.25182(16) 0.68810(12) 0.0286(6) Uani 1 1 d . . . C13 C 0.5838(2) 0.32660(16) 0.65589(13) 0.0329(6) Uani 1 1 d . . . C14 C 0.5014(3) 0.38070(18) 0.62655(15) 0.0447(7) Uani 1 1 d . . . H14 H 0.4203 0.3681 0.6252 0.054 Uiso 1 1 calc R . . C15 C 0.5372(3) 0.4527(2) 0.59940(17) 0.0587(9) Uani 1 1 d . . . H15 H 0.4804 0.4893 0.5799 0.070 Uiso 1 1 calc R . . C16 C 0.6546(4) 0.4714(2) 0.60056(17) 0.0595(10) Uani 1 1 d . . . H16 H 0.6788 0.5206 0.5816 0.071 Uiso 1 1 calc R . . C17 C 0.7366(3) 0.41857(19) 0.62930(15) 0.0478(8) Uani 1 1 d . . . H17 H 0.8175 0.4314 0.6301 0.057 Uiso 1 1 calc R . . C18 C 0.7017(3) 0.34642(17) 0.65729(13) 0.0355(6) Uani 1 1 d . . . H18 H 0.7588 0.3106 0.6774 0.043 Uiso 1 1 calc R . . C19 C 0.6137(2) -0.02555(16) 0.63460(13) 0.0331(6) Uani 1 1 d . . . H19A H 0.5370 0.0008 0.6387 0.040 Uiso 1 1 calc R . . H19B H 0.6115 -0.0807 0.6539 0.040 Uiso 1 1 calc R . . C20 C 0.6334(2) -0.03330(15) 0.56419(13) 0.0297(6) Uani 1 1 d . . . C21 C 0.5767(2) -0.09268(16) 0.52635(14) 0.0353(6) Uani 1 1 d . . . H21 H 0.5242 -0.1296 0.5441 0.042 Uiso 1 1 calc R . . C22 C 0.5974(2) -0.09763(17) 0.46245(15) 0.0396(7) Uani 1 1 d . . . H22 H 0.5589 -0.1379 0.4355 0.048 Uiso 1 1 calc R . . C23 C 0.6743(2) -0.04376(17) 0.43805(14) 0.0352(6) Uani 1 1 d . . . H23 H 0.6904 -0.0471 0.3943 0.042 Uiso 1 1 calc R . . C24 C 0.7279(2) 0.01539(15) 0.47801(12) 0.0283(6) Uani 1 1 d . . . C25 C 0.8145(2) 0.07303(16) 0.45461(13) 0.0323(6) Uani 1 1 d . . . C26 C 0.9214(2) 0.08614(17) 0.48988(15) 0.0381(7) Uani 1 1 d . . . H26 H 0.9381 0.0599 0.5302 0.046 Uiso 1 1 calc R . . C27 C 1.0039(3) 0.1376(2) 0.46617(18) 0.0552(9) Uani 1 1 d . . . H27 H 1.0774 0.1461 0.4900 0.066 Uiso 1 1 calc R . . C28 C 0.9785(4) 0.1763(2) 0.4078(2) 0.0649(12) Uani 1 1 d . . . H28 H 1.0349 0.2112 0.3913 0.078 Uiso 1 1 calc R . . C29 C 0.8716(4) 0.1646(2) 0.37367(17) 0.0649(11) Uani 1 1 d . . . H29 H 0.8540 0.1925 0.3341 0.078 Uiso 1 1 calc R . . C30 C 0.7900(3) 0.11278(19) 0.39613(14) 0.0460(8) Uani 1 1 d . . . H30 H 0.7171 0.1042 0.3718 0.055 Uiso 1 1 calc R . . C31 C 0.6748(2) 0.26641(14) 0.50308(11) 0.0230(5) Uani 1 1 d . . . C32 C 0.7987(2) 0.28128(15) 0.52143(12) 0.0249(5) Uani 1 1 d . . . C33 C 0.8579(2) 0.34145(15) 0.48495(12) 0.0268(6) Uani 1 1 d . . . C34 C 0.9782(2) 0.35928(15) 0.49855(14) 0.0326(6) Uani 1 1 d . . . H34 H 1.0229 0.3321 0.5326 0.039 Uiso 1 1 calc R . . C35 C 1.0301(2) 0.41662(18) 0.46176(14) 0.0401(7) Uani 1 1 d . . . H35 H 1.1113 0.4280 0.4699 0.048 Uiso 1 1 calc R . . C36 C 0.9643(3) 0.45781(18) 0.41299(14) 0.0422(7) Uani 1 1 d . . . H36 H 1.0011 0.4980 0.3888 0.051 Uiso 1 1 calc R . . C37 C 0.8478(3) 0.44195(17) 0.39887(14) 0.0387(7) Uani 1 1 d . . . H37 H 0.8033 0.4707 0.3656 0.046 Uiso 1 1 calc R . . C38 C 0.7959(2) 0.38197(16) 0.43506(12) 0.0288(6) Uani 1 1 d . . . C39 C 0.6215(2) 0.30990(15) 0.45219(12) 0.0261(5) Uani 1 1 d . . . C40 C 0.5006(2) 0.30148(15) 0.42368(13) 0.0296(6) Uani 1 1 d . . . C41 C 0.4070(2) 0.29474(17) 0.46163(15) 0.0370(7) Uani 1 1 d . . . H41 H 0.4212 0.2952 0.5071 0.044 Uiso 1 1 calc R . . C42 C 0.2939(3) 0.2874(2) 0.43372(17) 0.0485(8) Uani 1 1 d . . . H42 H 0.2307 0.2834 0.4601 0.058 Uiso 1 1 calc R . . C43 C 0.2718(3) 0.2858(2) 0.36713(18) 0.0563(9) Uani 1 1 d . . . H43 H 0.1938 0.2806 0.3480 0.068 Uiso 1 1 calc R . . C44 C 0.3640(3) 0.2916(2) 0.32913(17) 0.0528(9) Uani 1 1 d . . . H44 H 0.3499 0.2896 0.2836 0.063 Uiso 1 1 calc R . . C45 C 0.4771(2) 0.30053(18) 0.35737(14) 0.0398(7) Uani 1 1 d . . . H45 H 0.5398 0.3061 0.3308 0.048 Uiso 1 1 calc R . . O4 O 1.0290(11) 0.3577(6) 0.6757(6) 0.129(6) Uani 0.555(11) 1 d PD A 1 O5 O 1.0985(8) 0.4339(5) 0.7648(5) 0.102(4) Uani 0.555(11) 1 d PD A 1 O6 O 1.2276(5) 0.3989(4) 0.6959(4) 0.079(3) Uani 0.555(11) 1 d PD A 1 O4' O 0.9974(9) 0.3639(9) 0.7094(7) 0.113(5) Uani 0.445(11) 1 d PD A 2 O5' O 1.1490(15) 0.4409(6) 0.7423(8) 0.165(9) Uani 0.445(11) 1 d PD A 2 O6' O 1.1611(9) 0.3454(7) 0.6587(5) 0.108(5) Uani 0.445(11) 1 d PD A 2 O8 O 1.1544(2) 0.29961(14) 0.75972(13) 0.0651(7) 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 Cl1 0.0484(4) 0.0356(4) 0.0680(5) 0.0113(4) -0.0038(4) 0.0030(3) Cd1 0.02705(10) 0.02005(10) 0.02547(11) 0.00286(8) 0.00191(7) -0.00149(8) O1 0.0271(9) 0.0223(9) 0.0274(9) 0.0056(7) 0.0026(7) -0.0032(7) O2 0.0265(9) 0.0257(10) 0.0358(10) 0.0038(8) 0.0000(8) -0.0028(7) O3 0.0347(10) 0.0276(10) 0.0313(10) 0.0085(8) 0.0023(8) -0.0069(8) N1 0.0317(11) 0.0287(12) 0.0346(13) 0.0011(10) -0.0032(10) 0.0036(10) N2 0.0361(12) 0.0236(11) 0.0278(12) 0.0056(9) 0.0048(9) 0.0015(9) N3 0.0306(11) 0.0285(12) 0.0227(11) 0.0004(9) 0.0026(9) -0.0017(9) N4 0.0301(11) 0.0172(10) 0.0312(12) -0.0010(9) 0.0027(9) -0.0021(9) C1 0.0348(14) 0.0368(17) 0.0478(18) -0.0032(14) -0.0066(13) -0.0003(13) C2 0.0359(16) 0.056(2) 0.063(2) -0.0084(17) -0.0107(15) 0.0060(15) C3 0.0441(19) 0.064(2) 0.065(2) -0.0014(19) -0.0192(16) 0.0143(17) C4 0.0539(19) 0.0436(18) 0.0455(19) 0.0055(15) -0.0057(15) 0.0173(16) C5 0.0419(15) 0.0366(16) 0.0278(14) 0.0021(12) 0.0010(12) 0.0103(13) C6 0.0483(17) 0.0270(15) 0.0379(16) 0.0087(12) 0.0047(13) 0.0076(13) C7 0.0418(15) 0.0364(16) 0.0265(14) 0.0111(12) 0.0062(12) 0.0019(13) C8 0.0358(14) 0.0326(14) 0.0209(13) -0.0027(11) 0.0006(11) -0.0017(12) C9 0.0413(15) 0.0428(17) 0.0301(15) 0.0006(13) 0.0096(12) -0.0090(13) C10 0.0314(14) 0.0432(17) 0.0385(16) -0.0086(13) 0.0089(12) -0.0072(13) C11 0.0340(14) 0.0356(16) 0.0365(15) -0.0096(13) 0.0075(12) 0.0013(12) C12 0.0332(13) 0.0297(14) 0.0228(13) -0.0069(11) 0.0016(10) 0.0015(11) C13 0.0442(16) 0.0263(14) 0.0287(14) -0.0070(11) 0.0066(12) 0.0006(12) C14 0.0505(18) 0.0360(17) 0.0485(19) -0.0024(14) 0.0084(15) 0.0095(14) C15 0.081(3) 0.0345(18) 0.062(2) 0.0021(16) 0.0142(19) 0.0138(18) C16 0.096(3) 0.0272(17) 0.058(2) -0.0031(15) 0.021(2) -0.0063(18) C17 0.066(2) 0.0354(17) 0.0442(18) -0.0121(15) 0.0156(16) -0.0203(16) C18 0.0453(16) 0.0321(15) 0.0298(14) -0.0093(12) 0.0065(12) -0.0043(13) C19 0.0402(15) 0.0224(14) 0.0381(16) 0.0062(11) 0.0102(12) -0.0044(12) C20 0.0306(13) 0.0194(13) 0.0394(15) 0.0019(11) 0.0049(11) -0.0008(11) C21 0.0345(14) 0.0220(14) 0.0507(18) -0.0034(12) 0.0103(13) -0.0050(11) C22 0.0355(15) 0.0302(15) 0.0530(19) -0.0124(14) 0.0029(13) -0.0056(12) C23 0.0375(14) 0.0334(15) 0.0350(15) -0.0086(12) 0.0043(12) 0.0001(12) C24 0.0307(13) 0.0233(13) 0.0314(14) -0.0010(11) 0.0047(11) -0.0009(11) C25 0.0426(15) 0.0257(14) 0.0305(14) -0.0057(11) 0.0129(12) -0.0014(12) C26 0.0391(15) 0.0306(15) 0.0467(17) -0.0066(13) 0.0151(13) -0.0061(13) C27 0.0497(19) 0.046(2) 0.074(3) -0.0187(18) 0.0269(18) -0.0151(16) C28 0.089(3) 0.0411(19) 0.073(3) -0.0128(19) 0.054(2) -0.027(2) C29 0.112(3) 0.043(2) 0.045(2) 0.0029(16) 0.036(2) -0.015(2) C30 0.071(2) 0.0345(16) 0.0336(17) -0.0012(13) 0.0107(15) -0.0068(15) C31 0.0263(12) 0.0172(12) 0.0261(13) -0.0016(10) 0.0059(10) -0.0015(10) C32 0.0293(12) 0.0194(12) 0.0263(13) -0.0029(10) 0.0036(10) 0.0017(10) C33 0.0285(12) 0.0218(13) 0.0313(14) -0.0039(10) 0.0086(11) -0.0016(10) C34 0.0294(13) 0.0271(14) 0.0418(16) -0.0033(12) 0.0066(11) -0.0046(12) C35 0.0357(15) 0.0366(16) 0.0498(18) -0.0111(14) 0.0133(13) -0.0113(13) C36 0.0529(18) 0.0405(17) 0.0351(16) -0.0015(13) 0.0146(14) -0.0205(15) C37 0.0525(17) 0.0334(16) 0.0309(15) 0.0024(12) 0.0072(13) -0.0115(14) C38 0.0340(13) 0.0263(13) 0.0269(14) -0.0007(11) 0.0062(11) -0.0067(11) C39 0.0298(13) 0.0230(13) 0.0258(13) 0.0019(10) 0.0044(10) -0.0035(10) C40 0.0306(13) 0.0206(13) 0.0375(15) 0.0051(11) 0.0020(11) 0.0011(11) C41 0.0334(14) 0.0362(16) 0.0417(17) 0.0093(13) 0.0036(12) 0.0024(12) C42 0.0306(15) 0.0487(19) 0.067(2) 0.0185(17) 0.0079(15) 0.0017(14) C43 0.0369(16) 0.062(2) 0.067(2) 0.0255(19) -0.0126(16) -0.0104(16) C44 0.0491(18) 0.061(2) 0.0449(19) 0.0101(16) -0.0142(15) -0.0083(16) C45 0.0369(15) 0.0439(18) 0.0374(17) 0.0067(13) -0.0026(12) -0.0057(13) O4 0.157(11) 0.070(5) 0.137(9) 0.027(5) -0.116(8) -0.039(6) O5 0.113(6) 0.055(5) 0.142(6) -0.010(4) 0.038(5) 0.056(5) O6 0.068(4) 0.063(4) 0.112(6) 0.030(4) 0.035(4) 0.009(3) O4' 0.055(4) 0.143(9) 0.137(12) -0.036(8) -0.024(6) 0.031(5) O5' 0.228(17) 0.042(6) 0.193(15) 0.026(7) -0.155(13) -0.061(9) O6' 0.099(7) 0.134(10) 0.097(7) 0.050(6) 0.040(6) 0.031(7) O8 0.0800(17) 0.0377(13) 0.0768(18) 0.0190(12) 0.0024(14) 0.0012(12) _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 Cl1 O5' 1.312(9) . ? Cl1 O4 1.350(8) . ? Cl1 O4' 1.409(11) . ? Cl1 O8 1.420(2) . ? Cl1 O5 1.458(7) . ? Cl1 O6' 1.459(9) . ? Cl1 O6 1.466(5) . ? Cd1 O1 2.2134(17) . ? Cd1 O2 2.2792(16) . ? Cd1 N1 2.337(2) . ? Cd1 N4 2.420(2) . ? Cd1 N2 2.430(2) . ? Cd1 N3 2.4636(19) . ? O1 C31 1.316(3) . ? O2 C32 1.256(3) . ? O3 C38 1.359(3) . ? O3 C39 1.380(3) . ? N1 C5 1.339(3) . ? N1 C1 1.343(4) . ? N2 C19 1.462(3) . ? N2 C7 1.471(3) . ? N2 C6 1.479(3) . ? N3 C8 1.350(3) . ? N3 C12 1.357(3) . ? N4 C20 1.350(3) . ? N4 C24 1.351(3) . ? C1 C2 1.378(4) . ? C1 H1 0.9500 . ? C2 C3 1.372(5) . ? C2 H2 0.9500 . ? C3 C4 1.383(5) . ? C3 H3 0.9500 . ? C4 C5 1.386(4) . ? C4 H4 0.9500 . ? C5 C6 1.507(4) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.508(4) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.383(4) . ? C9 C10 1.381(4) . ? C9 H9 0.9500 . ? C10 C11 1.372(4) . ? C10 H10 0.9500 . ? C11 C12 1.399(3) . ? C11 H11 0.9500 . ? C12 C13 1.484(4) . ? C13 C18 1.387(4) . ? C13 C14 1.398(4) . ? C14 C15 1.386(4) . ? C14 H14 0.9500 . ? C15 C16 1.378(5) . ? C15 H15 0.9500 . ? C16 C17 1.376(5) . ? C16 H16 0.9500 . ? C17 C18 1.393(4) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 C20 1.512(4) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 C21 1.379(4) . ? C21 C22 1.378(4) . ? C21 H21 0.9500 . ? C22 C23 1.376(4) . ? C22 H22 0.9500 . ? C23 C24 1.387(4) . ? C23 H23 0.9500 . ? C24 C25 1.483(4) . ? C25 C26 1.390(4) . ? C25 C30 1.391(4) . ? C26 C27 1.390(4) . ? C26 H26 0.9500 . ? C27 C28 1.382(6) . ? C27 H27 0.9500 . ? C28 C29 1.376(6) . ? C28 H28 0.9500 . ? C29 C30 1.375(4) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? C31 C39 1.377(3) . ? C31 C32 1.458(3) . ? C32 C33 1.450(3) . ? C33 C38 1.379(4) . ? C33 C34 1.414(3) . ? C34 C35 1.380(4) . ? C34 H34 0.9500 . ? C35 C36 1.388(4) . ? C35 H35 0.9500 . ? C36 C37 1.367(4) . ? C36 H36 0.9500 . ? C37 C38 1.403(4) . ? C37 H37 0.9500 . ? C39 C40 1.466(3) . ? C40 C45 1.387(4) . ? C40 C41 1.392(4) . ? C41 C42 1.380(4) . ? C41 H41 0.9500 . ? C42 C43 1.391(5) . ? C42 H42 0.9500 . ? C43 C44 1.379(5) . ? C43 H43 0.9500 . ? C44 C45 1.384(4) . ? C44 H44 0.9500 . ? C45 H45 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O5' Cl1 O4 120.5(6) . . ? O5' Cl1 O4' 108.4(9) . . ? O4 Cl1 O4' 34.7(6) . . ? O5' Cl1 O8 118.0(5) . . ? O4 Cl1 O8 117.4(4) . . ? O4' Cl1 O8 106.3(7) . . ? O5' Cl1 O5 32.3(9) . . ? O4 Cl1 O5 111.4(7) . . ? O4' Cl1 O5 85.1(6) . . ? O8 Cl1 O5 105.8(4) . . ? O5' Cl1 O6' 116.5(8) . . ? O4 Cl1 O6' 69.2(6) . . ? O4' Cl1 O6' 103.7(6) . . ? O8 Cl1 O6' 102.6(3) . . ? O5 Cl1 O6' 146.5(5) . . ? O5' Cl1 O6 67.2(9) . . ? O4 Cl1 O6 115.0(6) . . ? O4' Cl1 O6 144.7(6) . . ? O8 Cl1 O6 106.1(2) . . ? O5 Cl1 O6 99.2(4) . . ? O6' Cl1 O6 55.4(4) . . ? O1 Cd1 O2 74.74(6) . . ? O1 Cd1 N1 156.95(7) . . ? O2 Cd1 N1 82.45(7) . . ? O1 Cd1 N4 89.28(7) . . ? O2 Cd1 N4 116.60(6) . . ? N1 Cd1 N4 98.09(7) . . ? O1 Cd1 N2 131.54(7) . . ? O2 Cd1 N2 153.56(7) . . ? N1 Cd1 N2 71.13(7) . . ? N4 Cd1 N2 67.65(7) . . ? O1 Cd1 N3 89.41(6) . . ? O2 Cd1 N3 116.00(7) . . ? N1 Cd1 N3 103.81(7) . . ? N4 Cd1 N3 124.90(7) . . ? N2 Cd1 N3 72.82(7) . . ? C31 O1 Cd1 113.41(14) . . ? C32 O2 Cd1 112.26(15) . . ? C38 O3 C39 120.3(2) . . ? C5 N1 C1 119.0(2) . . ? C5 N1 Cd1 117.93(18) . . ? C1 N1 Cd1 122.90(19) . . ? C19 N2 C7 111.9(2) . . ? C19 N2 C6 110.9(2) . . ? C7 N2 C6 110.5(2) . . ? C19 N2 Cd1 107.26(15) . . ? C7 N2 Cd1 107.90(15) . . ? C6 N2 Cd1 108.20(15) . . ? C8 N3 C12 118.7(2) . . ? C8 N3 Cd1 110.69(16) . . ? C12 N3 Cd1 124.82(16) . . ? C20 N4 C24 118.5(2) . . ? C20 N4 Cd1 113.81(16) . . ? C24 N4 Cd1 124.58(16) . . ? N1 C1 C2 122.4(3) . . ? N1 C1 H1 118.8 . . ? C2 C1 H1 118.8 . . ? C3 C2 C1 118.8(3) . . ? C3 C2 H2 120.6 . . ? C1 C2 H2 120.6 . . ? C2 C3 C4 119.1(3) . . ? C2 C3 H3 120.5 . . ? C4 C3 H3 120.5 . . ? C3 C4 C5 119.4(3) . . ? C3 C4 H4 120.3 . . ? C5 C4 H4 120.3 . . ? N1 C5 C4 121.2(3) . . ? N1 C5 C6 117.6(2) . . ? C4 C5 C6 121.0(3) . . ? N2 C6 C5 112.8(2) . . ? N2 C6 H6A 109.0 . . ? C5 C6 H6A 109.0 . . ? N2 C6 H6B 109.0 . . ? C5 C6 H6B 109.0 . . ? H6A C6 H6B 107.8 . . ? N2 C7 C8 111.9(2) . . ? N2 C7 H7A 109.2 . . ? C8 C7 H7A 109.2 . . ? N2 C7 H7B 109.2 . . ? C8 C7 H7B 109.2 . . ? H7A C7 H7B 107.9 . . ? N3 C8 C9 122.7(2) . . ? N3 C8 C7 117.1(2) . . ? C9 C8 C7 120.2(2) . . ? C10 C9 C8 118.6(3) . . ? C10 C9 H9 120.7 . . ? C8 C9 H9 120.7 . . ? C11 C10 C9 119.3(2) . . ? C11 C10 H10 120.3 . . ? C9 C10 H10 120.3 . . ? C10 C11 C12 120.1(3) . . ? C10 C11 H11 119.9 . . ? C12 C11 H11 119.9 . . ? N3 C12 C11 120.5(2) . . ? N3 C12 C13 119.1(2) . . ? C11 C12 C13 120.4(2) . . ? C18 C13 C14 118.7(3) . . ? C18 C13 C12 120.8(3) . . ? C14 C13 C12 120.4(3) . . ? C15 C14 C13 120.4(3) . . ? C15 C14 H14 119.8 . . ? C13 C14 H14 119.8 . . ? C16 C15 C14 120.4(3) . . ? C16 C15 H15 119.8 . . ? C14 C15 H15 119.8 . . ? C17 C16 C15 119.8(3) . . ? C17 C16 H16 120.1 . . ? C15 C16 H16 120.1 . . ? C16 C17 C18 120.4(3) . . ? C16 C17 H17 119.8 . . ? C18 C17 H17 119.8 . . ? C13 C18 C17 120.3(3) . . ? C13 C18 H18 119.8 . . ? C17 C18 H18 119.8 . . ? N2 C19 C20 111.8(2) . . ? N2 C19 H19A 109.2 . . ? C20 C19 H19A 109.2 . . ? N2 C19 H19B 109.2 . . ? C20 C19 H19B 109.2 . . ? H19A C19 H19B 107.9 . . ? N4 C20 C21 122.3(2) . . ? N4 C20 C19 116.8(2) . . ? C21 C20 C19 120.9(2) . . ? C22 C21 C20 118.9(3) . . ? C22 C21 H21 120.5 . . ? C20 C21 H21 120.5 . . ? C23 C22 C21 119.4(3) . . ? C23 C22 H22 120.3 . . ? C21 C22 H22 120.3 . . ? C22 C23 C24 119.4(3) . . ? C22 C23 H23 120.3 . . ? C24 C23 H23 120.3 . . ? N4 C24 C23 121.5(2) . . ? N4 C24 C25 117.1(2) . . ? C23 C24 C25 121.4(2) . . ? C26 C25 C30 119.6(3) . . ? C26 C25 C24 120.5(2) . . ? C30 C25 C24 119.9(3) . . ? C25 C26 C27 120.1(3) . . ? C25 C26 H26 120.0 . . ? C27 C26 H26 120.0 . . ? C28 C27 C26 119.7(3) . . ? C28 C27 H27 120.2 . . ? C26 C27 H27 120.2 . . ? C29 C28 C27 120.1(3) . . ? C29 C28 H28 119.9 . . ? C27 C28 H28 119.9 . . ? C30 C29 C28 120.7(4) . . ? C30 C29 H29 119.6 . . ? C28 C29 H29 119.6 . . ? C29 C30 C25 119.8(3) . . ? C29 C30 H30 120.1 . . ? C25 C30 H30 120.1 . . ? O1 C31 C39 123.3(2) . . ? O1 C31 C32 118.5(2) . . ? C39 C31 C32 118.2(2) . . ? O2 C32 C33 121.6(2) . . ? O2 C32 C31 120.6(2) . . ? C33 C32 C31 117.7(2) . . ? C38 C33 C34 118.8(2) . . ? C38 C33 C32 119.4(2) . . ? C34 C33 C32 121.9(2) . . ? C35 C34 C33 119.3(3) . . ? C35 C34 H34 120.4 . . ? C33 C34 H34 120.4 . . ? C34 C35 C36 120.4(3) . . ? C34 C35 H35 119.8 . . ? C36 C35 H35 119.8 . . ? C37 C36 C35 121.6(3) . . ? C37 C36 H36 119.2 . . ? C35 C36 H36 119.2 . . ? C36 C37 C38 118.0(3) . . ? C36 C37 H37 121.0 . . ? C38 C37 H37 121.0 . . ? O3 C38 C33 121.9(2) . . ? O3 C38 C37 116.1(2) . . ? C33 C38 C37 122.0(2) . . ? C31 C39 O3 122.5(2) . . ? C31 C39 C40 127.2(2) . . ? O3 C39 C40 110.2(2) . . ? C45 C40 C41 118.4(3) . . ? C45 C40 C39 120.0(2) . . ? C41 C40 C39 121.6(2) . . ? C42 C41 C40 120.6(3) . . ? C42 C41 H41 119.7 . . ? C40 C41 H41 119.7 . . ? C41 C42 C43 120.4(3) . . ? C41 C42 H42 119.8 . . ? C43 C42 H42 119.8 . . ? C44 C43 C42 119.5(3) . . ? C44 C43 H43 120.3 . . ? C42 C43 H43 120.3 . . ? C43 C44 C45 119.9(3) . . ? C43 C44 H44 120.0 . . ? C45 C44 H44 120.0 . . ? C44 C45 C40 121.3(3) . . ? C44 C45 H45 119.4 . . ? C40 C45 H45 119.4 . . ? 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 O2 Cd1 O1 C31 5.31(15) . . . . ? N1 Cd1 O1 C31 -3.3(3) . . . . ? N4 Cd1 O1 C31 -112.57(15) . . . . ? N2 Cd1 O1 C31 -171.29(14) . . . . ? N3 Cd1 O1 C31 122.52(15) . . . . ? O1 Cd1 O2 C32 -5.53(15) . . . . ? N1 Cd1 O2 C32 171.07(17) . . . . ? N4 Cd1 O2 C32 75.78(17) . . . . ? N2 Cd1 O2 C32 168.75(16) . . . . ? N3 Cd1 O2 C32 -87.20(17) . . . . ? O1 Cd1 N1 C5 -155.08(18) . . . . ? O2 Cd1 N1 C5 -163.5(2) . . . . ? N4 Cd1 N1 C5 -47.5(2) . . . . ? N2 Cd1 N1 C5 15.43(18) . . . . ? N3 Cd1 N1 C5 81.5(2) . . . . ? O1 Cd1 N1 C1 19.8(3) . . . . ? O2 Cd1 N1 C1 11.4(2) . . . . ? N4 Cd1 N1 C1 127.3(2) . . . . ? N2 Cd1 N1 C1 -169.7(2) . . . . ? N3 Cd1 N1 C1 -103.6(2) . . . . ? O1 Cd1 N2 C19 27.50(19) . . . . ? O2 Cd1 N2 C19 -145.12(16) . . . . ? N1 Cd1 N2 C19 -147.55(17) . . . . ? N4 Cd1 N2 C19 -40.02(15) . . . . ? N3 Cd1 N2 C19 100.75(16) . . . . ? O1 Cd1 N2 C7 -93.21(18) . . . . ? O2 Cd1 N2 C7 94.2(2) . . . . ? N1 Cd1 N2 C7 91.74(17) . . . . ? N4 Cd1 N2 C7 -160.73(18) . . . . ? N3 Cd1 N2 C7 -19.96(16) . . . . ? O1 Cd1 N2 C6 147.21(16) . . . . ? O2 Cd1 N2 C6 -25.4(3) . . . . ? N1 Cd1 N2 C6 -27.84(16) . . . . ? N4 Cd1 N2 C6 79.69(17) . . . . ? N3 Cd1 N2 C6 -139.54(18) . . . . ? O1 Cd1 N3 C8 128.91(17) . . . . ? O2 Cd1 N3 C8 -158.42(15) . . . . ? N1 Cd1 N3 C8 -70.17(17) . . . . ? N4 Cd1 N3 C8 40.20(19) . . . . ? N2 Cd1 N3 C8 -5.30(16) . . . . ? O1 Cd1 N3 C12 -23.7(2) . . . . ? O2 Cd1 N3 C12 48.9(2) . . . . ? N1 Cd1 N3 C12 137.18(19) . . . . ? N4 Cd1 N3 C12 -112.5(2) . . . . ? N2 Cd1 N3 C12 -158.0(2) . . . . ? O1 Cd1 N4 C20 -103.61(17) . . . . ? O2 Cd1 N4 C20 -176.12(16) . . . . ? N1 Cd1 N4 C20 98.31(18) . . . . ? N2 Cd1 N4 C20 32.62(17) . . . . ? N3 Cd1 N4 C20 -14.8(2) . . . . ? O1 Cd1 N4 C24 56.2(2) . . . . ? O2 Cd1 N4 C24 -16.3(2) . . . . ? N1 Cd1 N4 C24 -101.9(2) . . . . ? N2 Cd1 N4 C24 -167.6(2) . . . . ? N3 Cd1 N4 C24 144.96(18) . . . . ? C5 N1 C1 C2 1.1(4) . . . . ? Cd1 N1 C1 C2 -173.7(2) . . . . ? N1 C1 C2 C3 -2.0(5) . . . . ? C1 C2 C3 C4 0.7(5) . . . . ? C2 C3 C4 C5 1.2(5) . . . . ? C1 N1 C5 C4 1.0(4) . . . . ? Cd1 N1 C5 C4 176.0(2) . . . . ? C1 N1 C5 C6 -174.6(2) . . . . ? Cd1 N1 C5 C6 0.5(3) . . . . ? C3 C4 C5 N1 -2.1(5) . . . . ? C3 C4 C5 C6 173.3(3) . . . . ? C19 N2 C6 C5 155.6(2) . . . . ? C7 N2 C6 C5 -79.7(3) . . . . ? Cd1 N2 C6 C5 38.2(3) . . . . ? N1 C5 C6 N2 -27.6(3) . . . . ? C4 C5 C6 N2 156.8(3) . . . . ? C19 N2 C7 C8 -75.5(3) . . . . ? C6 N2 C7 C8 160.4(2) . . . . ? Cd1 N2 C7 C8 42.3(2) . . . . ? C12 N3 C8 C9 2.6(4) . . . . ? Cd1 N3 C8 C9 -151.9(2) . . . . ? C12 N3 C8 C7 -174.3(2) . . . . ? Cd1 N3 C8 C7 31.1(3) . . . . ? N2 C7 C8 N3 -52.5(3) . . . . ? N2 C7 C8 C9 130.4(3) . . . . ? N3 C8 C9 C10 -0.8(4) . . . . ? C7 C8 C9 C10 176.1(3) . . . . ? C8 C9 C10 C11 -0.9(4) . . . . ? C9 C10 C11 C12 0.8(4) . . . . ? C8 N3 C12 C11 -2.7(4) . . . . ? Cd1 N3 C12 C11 147.9(2) . . . . ? C8 N3 C12 C13 173.9(2) . . . . ? Cd1 N3 C12 C13 -35.5(3) . . . . ? C10 C11 C12 N3 1.0(4) . . . . ? C10 C11 C12 C13 -175.5(3) . . . . ? N3 C12 C13 C18 -32.4(4) . . . . ? C11 C12 C13 C18 144.2(3) . . . . ? N3 C12 C13 C14 151.1(3) . . . . ? C11 C12 C13 C14 -32.3(4) . . . . ? C18 C13 C14 C15 0.0(4) . . . . ? C12 C13 C14 C15 176.6(3) . . . . ? C13 C14 C15 C16 0.6(5) . . . . ? C14 C15 C16 C17 -0.5(5) . . . . ? C15 C16 C17 C18 -0.1(5) . . . . ? C14 C13 C18 C17 -0.7(4) . . . . ? C12 C13 C18 C17 -177.2(2) . . . . ? C16 C17 C18 C13 0.7(4) . . . . ? C7 N2 C19 C20 163.6(2) . . . . ? C6 N2 C19 C20 -72.6(3) . . . . ? Cd1 N2 C19 C20 45.4(2) . . . . ? C24 N4 C20 C21 -1.5(4) . . . . ? Cd1 N4 C20 C21 159.6(2) . . . . ? C24 N4 C20 C19 179.3(2) . . . . ? Cd1 N4 C20 C19 -19.6(3) . . . . ? N2 C19 C20 N4 -18.3(3) . . . . ? N2 C19 C20 C21 162.5(2) . . . . ? N4 C20 C21 C22 0.9(4) . . . . ? C19 C20 C21 C22 -179.9(3) . . . . ? C20 C21 C22 C23 0.4(4) . . . . ? C21 C22 C23 C24 -1.1(4) . . . . ? C20 N4 C24 C23 0.7(4) . . . . ? Cd1 N4 C24 C23 -158.21(19) . . . . ? C20 N4 C24 C25 -176.7(2) . . . . ? Cd1 N4 C24 C25 24.4(3) . . . . ? C22 C23 C24 N4 0.6(4) . . . . ? C22 C23 C24 C25 177.9(3) . . . . ? N4 C24 C25 C26 46.1(4) . . . . ? C23 C24 C25 C26 -131.4(3) . . . . ? N4 C24 C25 C30 -135.6(3) . . . . ? C23 C24 C25 C30 47.0(4) . . . . ? C30 C25 C26 C27 -1.1(4) . . . . ? C24 C25 C26 C27 177.2(3) . . . . ? C25 C26 C27 C28 0.8(4) . . . . ? C26 C27 C28 C29 0.6(5) . . . . ? C27 C28 C29 C30 -1.6(5) . . . . ? C28 C29 C30 C25 1.3(5) . . . . ? C26 C25 C30 C29 0.0(4) . . . . ? C24 C25 C30 C29 -178.3(3) . . . . ? Cd1 O1 C31 C39 173.04(19) . . . . ? Cd1 O1 C31 C32 -4.8(3) . . . . ? Cd1 O2 C32 C33 -173.40(17) . . . . ? Cd1 O2 C32 C31 5.1(3) . . . . ? O1 C31 C32 O2 -0.4(3) . . . . ? C39 C31 C32 O2 -178.3(2) . . . . ? O1 C31 C32 C33 178.2(2) . . . . ? C39 C31 C32 C33 0.3(3) . . . . ? O2 C32 C33 C38 178.7(2) . . . . ? C31 C32 C33 C38 0.1(3) . . . . ? O2 C32 C33 C34 -0.5(4) . . . . ? C31 C32 C33 C34 -179.1(2) . . . . ? C38 C33 C34 C35 0.1(4) . . . . ? C32 C33 C34 C35 179.4(2) . . . . ? C33 C34 C35 C36 1.6(4) . . . . ? C34 C35 C36 C37 -1.5(4) . . . . ? C35 C36 C37 C38 -0.4(4) . . . . ? C39 O3 C38 C33 0.2(4) . . . . ? C39 O3 C38 C37 -178.9(2) . . . . ? C34 C33 C38 O3 178.9(2) . . . . ? C32 C33 C38 O3 -0.4(4) . . . . ? C34 C33 C38 C37 -2.0(4) . . . . ? C32 C33 C38 C37 178.7(2) . . . . ? C36 C37 C38 O3 -178.7(2) . . . . ? C36 C37 C38 C33 2.2(4) . . . . ? O1 C31 C39 O3 -178.3(2) . . . . ? C32 C31 C39 O3 -0.5(4) . . . . ? O1 C31 C39 C40 -1.4(4) . . . . ? C32 C31 C39 C40 176.4(2) . . . . ? C38 O3 C39 C31 0.2(4) . . . . ? C38 O3 C39 C40 -177.1(2) . . . . ? C31 C39 C40 C45 -136.0(3) . . . . ? O3 C39 C40 C45 41.2(3) . . . . ? C31 C39 C40 C41 44.4(4) . . . . ? O3 C39 C40 C41 -138.4(2) . . . . ? C45 C40 C41 C42 -0.1(4) . . . . ? C39 C40 C41 C42 179.6(3) . . . . ? C40 C41 C42 C43 0.7(5) . . . . ? C41 C42 C43 C44 -0.1(5) . . . . ? C42 C43 C44 C45 -1.2(5) . . . . ? C43 C44 C45 C40 1.8(5) . . . . ? C41 C40 C45 C44 -1.2(4) . . . . ? C39 C40 C45 C44 179.2(3) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.840 _refine_diff_density_min -0.573 _refine_diff_density_rms 0.074 #===END data_usu212 _database_code_depnum_ccdc_archive 'CCDC 832450' #TrackingRef '- CombinedCIF copy.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C45 H35 Hg N4 O3, Cl O4' _chemical_formula_sum 'C45 H35 Cl Hg N4 O7' _chemical_formula_weight 979.81 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Hg Hg -2.3894 9.2266 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' 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 11.4117(2) _cell_length_b 16.3761(2) _cell_length_c 20.9794(3) _cell_angle_alpha 90.00 _cell_angle_beta 95.0070(9) _cell_angle_gamma 90.00 _cell_volume 3905.65(10) _cell_formula_units_Z 4 _cell_measurement_temperature 150(1) _cell_measurement_reflns_used 8852 _cell_measurement_theta_min 1.018 _cell_measurement_theta_max 27.485 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.666 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1944 _exptl_absorpt_coefficient_mu 4.068 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.4967 _exptl_absorpt_correction_T_max 0.6865 _exptl_absorpt_process_details 'DENZO-SMN (Otwinowski & Minor, 1997)' _exptl_special_details ; The program Denzo-SMN (Otwinowski & Minor, 1997) uses a scaling algorithm (Fox & Holmes, 1966) which effectively corrects for absorption effects. High redundancy data were used in the scaling program hence the 'multi-scan' code word was used. No transmission coefficients are available from the program (only scale factors for each frame). The scale factors in the experimental table are calculated from the 'size' command in the SHELXL-97 input file. ; _diffrn_ambient_temperature 150(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD Diffractometer' _diffrn_measurement_method 'Phi and Omega sacn' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16904 _diffrn_reflns_av_R_equivalents 0.0366 _diffrn_reflns_av_sigmaI/netI 0.0553 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.31 _diffrn_reflns_theta_max 27.49 _reflns_number_total 8946 _reflns_number_gt 6666 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius COLLECT' _computing_cell_refinement DENZO-SMN _computing_data_reduction DENZO-SMN _computing_structure_solution SIR97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'WinGX, Ortep3' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0266P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00090(7) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 8946 _refine_ls_number_parameters 552 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0565 _refine_ls_R_factor_gt 0.0324 _refine_ls_wR_factor_ref 0.0674 _refine_ls_wR_factor_gt 0.0608 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.040 _refine_ls_shift/su_max 0.003 _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 Hg1 Hg 0.240696(12) 0.143923(8) 0.603733(6) 0.02729(6) Uani 1 1 d . . . Cl1 Cl -0.38444(10) 0.36323(6) 0.71950(6) 0.0530(3) Uani 1 1 d . . . O1 O 0.1278(2) 0.21553(14) 0.53453(11) 0.0298(6) Uani 1 1 d . . . O2 O 0.3626(2) 0.24959(15) 0.56466(11) 0.0339(6) Uani 1 1 d . . . O3 O 0.1832(2) 0.37183(15) 0.41872(11) 0.0339(6) Uani 1 1 d . . . O4 O -0.3534(3) 0.29642(19) 0.76034(17) 0.0708(10) Uani 1 1 d . A . O5 O -0.5058(7) 0.3677(8) 0.7097(5) 0.101(4) Uani 0.545(11) 1 d PD A 1 O6 O -0.3443(8) 0.3405(5) 0.6581(4) 0.084(4) Uani 0.545(11) 1 d PD A 1 O7 O -0.3411(14) 0.4358(6) 0.7400(6) 0.136(8) Uani 0.545(11) 1 d PD A 1 O5A O -0.4684(19) 0.3546(8) 0.6722(9) 0.186(14) Uani 0.455(11) 1 d PD A 2 O6A O -0.2746(9) 0.3979(7) 0.7025(6) 0.091(5) Uani 0.455(11) 1 d PD A 2 O7A O -0.4116(15) 0.4293(8) 0.7641(7) 0.128(7) Uani 0.455(11) 1 d PD A 2 N1 N 0.4177(3) 0.10528(18) 0.65864(14) 0.0345(7) Uani 1 1 d . . . N2 N 0.2071(3) 0.02172(17) 0.66869(13) 0.0310(7) Uani 1 1 d . . . N3 N 0.1143(3) 0.18569(18) 0.69352(13) 0.0305(7) Uani 1 1 d . . . N4 N 0.2056(3) 0.01668(17) 0.53960(13) 0.0297(7) Uani 1 1 d . . . C1 C 0.5138(4) 0.1528(3) 0.6609(2) 0.0432(10) Uani 1 1 d . . . H1 H 0.5077 0.2059 0.6427 0.052 Uiso 1 1 calc R . . C2 C 0.6207(4) 0.1271(3) 0.6889(2) 0.0541(12) Uani 1 1 d . . . H2 H 0.6879 0.1614 0.6890 0.065 Uiso 1 1 calc R . . C3 C 0.6295(4) 0.0508(3) 0.7170(2) 0.0581(13) Uani 1 1 d . . . H3 H 0.7024 0.0318 0.7368 0.070 Uiso 1 1 calc R . . C4 C 0.5297(4) 0.0026(3) 0.7155(2) 0.0493(11) Uani 1 1 d . . . H4 H 0.5331 -0.0495 0.7354 0.059 Uiso 1 1 calc R . . C5 C 0.4253(4) 0.0303(2) 0.68503(17) 0.0361(9) Uani 1 1 d . . . C6 C 0.3181(4) -0.0240(2) 0.67632(19) 0.0384(9) Uani 1 1 d . . . H6A H 0.3241 -0.0587 0.6381 0.046 Uiso 1 1 calc R . . H6B H 0.3171 -0.0604 0.7139 0.046 Uiso 1 1 calc R . . C7 C 0.1729(4) 0.0501(2) 0.73172(16) 0.0378(9) Uani 1 1 d . . . H7A H 0.2442 0.0687 0.7580 0.045 Uiso 1 1 calc R . . H7B H 0.1393 0.0036 0.7542 0.045 Uiso 1 1 calc R . . C8 C 0.0847(3) 0.1186(2) 0.72607(16) 0.0318(8) Uani 1 1 d . . . C9 C -0.0170(4) 0.1127(2) 0.75596(17) 0.0375(9) Uani 1 1 d . . . H9 H -0.0356 0.0640 0.7775 0.045 Uiso 1 1 calc R . . C10 C -0.0920(4) 0.1794(3) 0.75397(18) 0.0399(10) Uani 1 1 d . . . H10 H -0.1627 0.1773 0.7747 0.048 Uiso 1 1 calc R . . C11 C -0.0629(3) 0.2491(2) 0.72153(16) 0.0366(9) Uani 1 1 d . . . H11 H -0.1136 0.2951 0.7196 0.044 Uiso 1 1 calc R . . C12 C 0.0420(3) 0.2512(2) 0.69154(16) 0.0305(8) Uani 1 1 d . . . C13 C 0.0776(4) 0.3264(2) 0.65956(17) 0.0335(9) Uani 1 1 d . . . C14 C -0.0063(4) 0.3809(2) 0.6323(2) 0.0456(10) Uani 1 1 d . . . H14 H -0.0876 0.3687 0.6330 0.055 Uiso 1 1 calc R . . C15 C 0.0278(5) 0.4525(3) 0.6045(2) 0.0583(13) Uani 1 1 d . . . H15 H -0.0301 0.4889 0.5857 0.070 Uiso 1 1 calc R . . C16 C 0.1452(5) 0.4714(3) 0.6037(2) 0.0583(13) Uani 1 1 d . . . H16 H 0.1681 0.5209 0.5847 0.070 Uiso 1 1 calc R . . C17 C 0.2295(4) 0.4184(2) 0.63050(19) 0.0472(11) Uani 1 1 d . . . H17 H 0.3105 0.4314 0.6297 0.057 Uiso 1 1 calc R . . C18 C 0.1965(4) 0.3460(2) 0.65879(17) 0.0371(9) Uani 1 1 d . . . H18 H 0.2549 0.3100 0.6776 0.044 Uiso 1 1 calc R . . C19 C 0.1137(4) -0.0267(2) 0.63441(17) 0.0358(9) Uani 1 1 d . . . H19A H 0.0369 0.0000 0.6385 0.043 Uiso 1 1 calc R . . H19B H 0.1114 -0.0815 0.6543 0.043 Uiso 1 1 calc R . . C20 C 0.1322(3) -0.0361(2) 0.56390(17) 0.0322(8) Uani 1 1 d . . . C21 C 0.0726(4) -0.0955(2) 0.52780(19) 0.0386(9) Uani 1 1 d . . . H21 H 0.0200 -0.1314 0.5465 0.046 Uiso 1 1 calc R . . C22 C 0.0910(4) -0.1017(2) 0.4636(2) 0.0397(9) Uani 1 1 d . . . H22 H 0.0512 -0.1423 0.4375 0.048 Uiso 1 1 calc R . . C23 C 0.1678(3) -0.0483(2) 0.43805(18) 0.0370(9) Uani 1 1 d . . . H23 H 0.1820 -0.0522 0.3942 0.044 Uiso 1 1 calc R . . C24 C 0.2244(3) 0.0111(2) 0.47660(17) 0.0312(8) Uani 1 1 d . . . C25 C 0.3092(4) 0.0691(2) 0.45225(17) 0.0352(9) Uani 1 1 d . . . C26 C 0.4154(4) 0.0845(2) 0.4868(2) 0.0414(10) Uani 1 1 d . . . H26 H 0.4335 0.0586 0.5270 0.050 Uiso 1 1 calc R . . C27 C 0.4961(4) 0.1379(3) 0.4633(3) 0.0605(14) Uani 1 1 d . . . H27 H 0.5702 0.1471 0.4864 0.073 Uiso 1 1 calc R . . C28 C 0.4671(5) 0.1777(3) 0.4053(3) 0.0678(16) Uani 1 1 d . . . H28 H 0.5216 0.2142 0.3887 0.081 Uiso 1 1 calc R . . C29 C 0.3598(5) 0.1640(3) 0.3723(2) 0.0638(15) Uani 1 1 d . . . H29 H 0.3395 0.1925 0.3334 0.077 Uiso 1 1 calc R . . C30 C 0.2812(4) 0.1096(3) 0.39470(18) 0.0475(11) Uani 1 1 d . . . H30 H 0.2079 0.0997 0.3709 0.057 Uiso 1 1 calc R . . C31 C 0.1826(3) 0.2715(2) 0.50319(15) 0.0258(7) Uani 1 1 d . . . C32 C 0.3064(3) 0.2872(2) 0.52015(16) 0.0276(8) Uani 1 1 d . . . C33 C 0.3639(3) 0.3475(2) 0.48286(16) 0.0280(8) Uani 1 1 d . . . C34 C 0.4842(3) 0.3658(2) 0.49412(19) 0.0368(9) Uani 1 1 d . . . H34 H 0.5308 0.3386 0.5274 0.044 Uiso 1 1 calc R . . C35 C 0.5346(4) 0.4227(2) 0.45734(19) 0.0421(10) Uani 1 1 d . . . H35 H 0.6164 0.4337 0.4644 0.051 Uiso 1 1 calc R . . C36 C 0.4662(4) 0.4646(2) 0.40953(18) 0.0450(11) Uani 1 1 d . . . H36 H 0.5018 0.5052 0.3853 0.054 Uiso 1 1 calc R . . C37 C 0.3488(4) 0.4482(2) 0.39692(18) 0.0414(10) Uani 1 1 d . . . H37 H 0.3027 0.4768 0.3643 0.050 Uiso 1 1 calc R . . C38 C 0.2987(3) 0.3881(2) 0.43349(17) 0.0314(8) Uani 1 1 d . . . C39 C 0.1264(3) 0.3141(2) 0.45247(16) 0.0288(8) Uani 1 1 d . . . C40 C 0.0050(3) 0.3044(2) 0.42547(17) 0.0314(8) Uani 1 1 d . . . C41 C -0.0887(4) 0.2988(2) 0.4648(2) 0.0418(10) Uani 1 1 d . . . H41 H -0.0736 0.3013 0.5100 0.050 Uiso 1 1 calc R . . C42 C -0.2028(4) 0.2896(3) 0.4373(2) 0.0553(13) Uani 1 1 d . . . H42 H -0.2658 0.2853 0.4639 0.066 Uiso 1 1 calc R . . C43 C -0.2257(4) 0.2864(3) 0.3710(2) 0.0599(13) Uani 1 1 d . . . H43 H -0.3043 0.2809 0.3524 0.072 Uiso 1 1 calc R . . C44 C -0.1349(4) 0.2914(3) 0.3326(2) 0.0565(13) Uani 1 1 d . . . H44 H -0.1503 0.2877 0.2874 0.068 Uiso 1 1 calc R . . C45 C -0.0210(4) 0.3018(3) 0.35941(18) 0.0425(10) Uani 1 1 d . . . H45 H 0.0410 0.3073 0.3322 0.051 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 Hg1 0.03265(9) 0.02100(8) 0.02826(8) 0.00423(6) 0.00286(5) -0.00119(6) Cl1 0.0502(7) 0.0334(6) 0.0738(8) 0.0114(5) -0.0033(6) 0.0000(5) O1 0.0330(15) 0.0231(13) 0.0333(13) 0.0085(10) 0.0036(11) -0.0028(11) O2 0.0303(15) 0.0302(14) 0.0408(14) 0.0073(12) 0.0000(11) -0.0033(11) O3 0.0367(16) 0.0304(14) 0.0349(14) 0.0083(11) 0.0038(11) -0.0050(11) O4 0.086(3) 0.0416(19) 0.084(2) 0.0229(18) 0.005(2) 0.0000(18) O5 0.043(5) 0.160(10) 0.096(8) -0.035(7) -0.016(5) 0.038(5) O6 0.076(6) 0.093(7) 0.085(6) 0.042(5) 0.028(5) 0.024(5) O7 0.201(17) 0.050(6) 0.135(12) 0.038(7) -0.111(11) -0.071(9) O5A 0.28(3) 0.080(9) 0.163(16) 0.043(10) -0.189(18) -0.080(13) O6A 0.074(7) 0.080(9) 0.124(11) 0.037(7) 0.031(7) 0.000(6) O7A 0.182(15) 0.074(10) 0.135(11) 0.002(8) 0.051(10) 0.080(10) N1 0.039(2) 0.0282(16) 0.0355(17) 0.0038(14) -0.0010(14) 0.0031(14) N2 0.0380(19) 0.0264(16) 0.0290(15) 0.0056(13) 0.0058(13) 0.0014(14) N3 0.0338(18) 0.0339(17) 0.0238(15) -0.0040(13) 0.0032(13) -0.0002(14) N4 0.0375(19) 0.0186(15) 0.0336(16) 0.0026(13) 0.0068(14) -0.0025(13) C1 0.036(2) 0.041(2) 0.050(2) -0.002(2) -0.0070(19) 0.0011(19) C2 0.040(3) 0.056(3) 0.063(3) -0.008(2) -0.009(2) 0.003(2) C3 0.047(3) 0.061(3) 0.063(3) 0.003(2) -0.012(2) 0.015(2) C4 0.055(3) 0.045(3) 0.047(2) 0.007(2) -0.002(2) 0.019(2) C5 0.045(3) 0.032(2) 0.0309(19) 0.0020(16) 0.0054(17) 0.0102(18) C6 0.047(3) 0.028(2) 0.041(2) 0.0111(17) 0.0059(18) 0.0086(18) C7 0.052(3) 0.037(2) 0.0256(18) 0.0080(16) 0.0088(17) 0.0065(19) C8 0.039(2) 0.035(2) 0.0223(17) -0.0022(15) 0.0047(15) -0.0016(17) C9 0.045(3) 0.037(2) 0.032(2) 0.0026(17) 0.0119(18) -0.0062(19) C10 0.031(2) 0.053(3) 0.038(2) -0.0085(19) 0.0139(17) -0.008(2) C11 0.039(2) 0.040(2) 0.0318(19) -0.0048(17) 0.0092(17) 0.0031(18) C12 0.033(2) 0.0297(19) 0.0286(18) -0.0075(16) 0.0023(15) -0.0024(16) C13 0.042(2) 0.0245(18) 0.035(2) -0.0084(16) 0.0053(17) -0.0014(17) C14 0.045(3) 0.035(2) 0.058(3) 0.001(2) 0.011(2) 0.0117(19) C15 0.075(4) 0.034(3) 0.067(3) 0.006(2) 0.016(3) 0.015(2) C16 0.088(4) 0.029(2) 0.060(3) -0.002(2) 0.018(3) -0.006(2) C17 0.062(3) 0.035(2) 0.046(2) -0.015(2) 0.016(2) -0.018(2) C18 0.045(2) 0.033(2) 0.034(2) -0.0088(17) 0.0064(17) -0.0078(18) C19 0.046(3) 0.0221(19) 0.041(2) 0.0066(16) 0.0103(18) -0.0049(17) C20 0.037(2) 0.0194(18) 0.040(2) 0.0033(15) 0.0042(17) 0.0032(16) C21 0.039(2) 0.023(2) 0.055(2) -0.0026(17) 0.0109(19) -0.0065(17) C22 0.038(2) 0.028(2) 0.053(2) -0.0110(19) 0.0053(19) -0.0048(17) C23 0.042(2) 0.033(2) 0.037(2) -0.0075(17) 0.0083(17) -0.0001(18) C24 0.035(2) 0.0241(19) 0.0350(19) 0.0012(16) 0.0048(16) 0.0042(16) C25 0.048(2) 0.0262(19) 0.0340(19) -0.0056(16) 0.0178(17) -0.0026(18) C26 0.043(3) 0.038(2) 0.046(2) -0.0060(19) 0.0166(19) -0.0039(19) C27 0.051(3) 0.060(3) 0.075(3) -0.024(3) 0.030(3) -0.017(2) C28 0.098(5) 0.043(3) 0.070(3) -0.014(3) 0.053(3) -0.026(3) C29 0.105(5) 0.046(3) 0.047(3) 0.002(2) 0.040(3) -0.013(3) C30 0.070(3) 0.039(2) 0.035(2) 0.0008(19) 0.013(2) -0.008(2) C31 0.031(2) 0.0184(17) 0.0291(18) -0.0017(14) 0.0085(15) 0.0014(14) C32 0.030(2) 0.0217(18) 0.0314(18) -0.0018(15) 0.0053(15) 0.0015(15) C33 0.031(2) 0.0225(18) 0.0314(18) -0.0016(15) 0.0104(15) -0.0032(15) C34 0.034(2) 0.029(2) 0.048(2) -0.0033(17) 0.0066(18) -0.0037(17) C35 0.034(2) 0.039(2) 0.055(2) -0.009(2) 0.0144(19) -0.0124(19) C36 0.059(3) 0.040(2) 0.039(2) -0.0014(19) 0.019(2) -0.021(2) C37 0.052(3) 0.039(2) 0.034(2) 0.0053(17) 0.0074(18) -0.015(2) C38 0.034(2) 0.0283(19) 0.0328(19) -0.0021(16) 0.0068(16) -0.0046(16) C39 0.033(2) 0.0230(18) 0.0307(18) 0.0007(15) 0.0067(16) -0.0003(15) C40 0.031(2) 0.0221(18) 0.042(2) 0.0060(16) 0.0039(17) 0.0015(15) C41 0.039(3) 0.032(2) 0.054(3) 0.0108(19) 0.006(2) 0.0020(18) C42 0.033(3) 0.049(3) 0.085(4) 0.024(3) 0.012(2) 0.003(2) C43 0.046(3) 0.054(3) 0.077(3) 0.025(3) -0.009(3) -0.004(2) C44 0.048(3) 0.061(3) 0.057(3) 0.011(2) -0.017(2) -0.009(2) C45 0.039(3) 0.046(3) 0.042(2) 0.0045(19) 0.0008(19) -0.0040(19) _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 Hg1 O1 2.194(2) . ? Hg1 N1 2.324(3) . ? Hg1 O2 2.408(2) . ? Hg1 N2 2.470(3) . ? Hg1 N4 2.494(3) . ? Hg1 N3 2.563(3) . ? Cl1 O5A 1.325(10) . ? Cl1 O7 1.343(8) . ? Cl1 O5 1.384(8) . ? Cl1 O4 1.416(3) . ? Cl1 O6A 1.449(10) . ? Cl1 O6 1.453(8) . ? Cl1 O7A 1.481(11) . ? O1 C31 1.317(4) . ? O2 C32 1.248(4) . ? O3 C38 1.354(4) . ? O3 C39 1.377(4) . ? N1 C1 1.343(5) . ? N1 C5 1.346(5) . ? N2 C19 1.466(5) . ? N2 C6 1.469(5) . ? N2 C7 1.485(4) . ? N3 C12 1.351(5) . ? N3 C8 1.352(5) . ? N4 C20 1.335(5) . ? N4 C24 1.361(4) . ? C1 C2 1.373(6) . ? C1 H1 0.9500 . ? C2 C3 1.382(6) . ? C2 H2 0.9500 . ? C3 C4 1.383(6) . ? C3 H3 0.9500 . ? C4 C5 1.378(5) . ? C4 H4 0.9500 . ? C5 C6 1.510(6) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.506(5) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.369(5) . ? C9 C10 1.387(6) . ? C9 H9 0.9500 . ? C10 C11 1.384(5) . ? C10 H10 0.9500 . ? C11 C12 1.400(5) . ? C11 H11 0.9500 . ? C12 C13 1.476(5) . ? C13 C14 1.395(5) . ? C13 C18 1.395(5) . ? C14 C15 1.381(6) . ? C14 H14 0.9500 . ? C15 C16 1.376(7) . ? C15 H15 0.9500 . ? C16 C17 1.378(6) . ? C16 H16 0.9500 . ? C17 C18 1.393(5) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 C20 1.520(5) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 C21 1.375(5) . ? C21 C22 1.384(5) . ? C21 H21 0.9500 . ? C22 C23 1.380(5) . ? C22 H22 0.9500 . ? C23 C24 1.388(5) . ? C23 H23 0.9500 . ? C24 C25 1.478(5) . ? C25 C26 1.381(5) . ? C25 C30 1.390(5) . ? C26 C27 1.391(6) . ? C26 H26 0.9500 . ? C27 C28 1.394(7) . ? C27 H27 0.9500 . ? C28 C29 1.372(7) . ? C28 H28 0.9500 . ? C29 C30 1.377(6) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? C31 C39 1.383(5) . ? C31 C32 1.449(5) . ? C32 C33 1.451(5) . ? C33 C38 1.391(5) . ? C33 C34 1.405(5) . ? C34 C35 1.368(5) . ? C34 H34 0.9500 . ? C35 C36 1.396(6) . ? C35 H35 0.9500 . ? C36 C37 1.369(6) . ? C36 H36 0.9500 . ? C37 C38 1.400(5) . ? C37 H37 0.9500 . ? C39 C40 1.459(5) . ? C40 C45 1.392(5) . ? C40 C41 1.409(5) . ? C41 C42 1.385(6) . ? C41 H41 0.9500 . ? C42 C43 1.395(6) . ? C42 H42 0.9500 . ? C43 C44 1.369(7) . ? C43 H43 0.9500 . ? C44 C45 1.382(5) . ? C44 H44 0.9500 . ? C45 H45 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Hg1 N1 155.23(10) . . ? O1 Hg1 O2 73.37(8) . . ? N1 Hg1 O2 82.05(10) . . ? O1 Hg1 N2 133.43(9) . . ? N1 Hg1 N2 71.10(11) . . ? O2 Hg1 N2 153.15(9) . . ? O1 Hg1 N4 91.84(9) . . ? N1 Hg1 N4 97.57(10) . . ? O2 Hg1 N4 119.16(9) . . ? N2 Hg1 N4 66.12(9) . . ? O1 Hg1 N3 90.47(9) . . ? N1 Hg1 N3 103.23(10) . . ? O2 Hg1 N3 115.92(9) . . ? N2 Hg1 N3 71.72(10) . . ? N4 Hg1 N3 123.03(10) . . ? O5A Cl1 O7 123.7(7) . . ? O5A Cl1 O5 41.0(11) . . ? O7 Cl1 O5 109.6(9) . . ? O5A Cl1 O4 119.8(5) . . ? O7 Cl1 O4 115.1(4) . . ? O5 Cl1 O4 109.0(6) . . ? O5A Cl1 O6A 116.2(10) . . ? O7 Cl1 O6A 55.3(7) . . ? O5 Cl1 O6A 144.9(7) . . ? O4 Cl1 O6A 106.0(5) . . ? O5A Cl1 O6 64.7(11) . . ? O7 Cl1 O6 112.0(8) . . ? O5 Cl1 O6 105.7(5) . . ? O4 Cl1 O6 104.9(3) . . ? O6A Cl1 O6 62.3(6) . . ? O5A Cl1 O7A 111.9(11) . . ? O7 Cl1 O7A 40.8(8) . . ? O5 Cl1 O7A 78.1(8) . . ? O4 Cl1 O7A 103.7(6) . . ? O6A Cl1 O7A 95.9(7) . . ? O6 Cl1 O7A 147.9(7) . . ? C31 O1 Hg1 115.2(2) . . ? C32 O2 Hg1 109.6(2) . . ? C38 O3 C39 120.7(3) . . ? C1 N1 C5 119.4(3) . . ? C1 N1 Hg1 122.1(3) . . ? C5 N1 Hg1 118.3(3) . . ? C19 N2 C6 111.2(3) . . ? C19 N2 C7 111.7(3) . . ? C6 N2 C7 110.7(3) . . ? C19 N2 Hg1 108.0(2) . . ? C6 N2 Hg1 107.4(2) . . ? C7 N2 Hg1 107.7(2) . . ? C12 N3 C8 118.8(3) . . ? C12 N3 Hg1 124.8(2) . . ? C8 N3 Hg1 109.6(2) . . ? C20 N4 C24 119.0(3) . . ? C20 N4 Hg1 114.3(2) . . ? C24 N4 Hg1 123.3(2) . . ? N1 C1 C2 122.0(4) . . ? N1 C1 H1 119.0 . . ? C2 C1 H1 119.0 . . ? C1 C2 C3 119.2(5) . . ? C1 C2 H2 120.4 . . ? C3 C2 H2 120.4 . . ? C2 C3 C4 118.5(4) . . ? C2 C3 H3 120.7 . . ? C4 C3 H3 120.7 . . ? C5 C4 C3 120.0(4) . . ? C5 C4 H4 120.0 . . ? C3 C4 H4 120.0 . . ? N1 C5 C4 120.9(4) . . ? N1 C5 C6 117.7(3) . . ? C4 C5 C6 121.4(4) . . ? N2 C6 C5 113.3(3) . . ? N2 C6 H6A 108.9 . . ? C5 C6 H6A 108.9 . . ? N2 C6 H6B 108.9 . . ? C5 C6 H6B 108.9 . . ? H6A C6 H6B 107.7 . . ? N2 C7 C8 112.9(3) . . ? N2 C7 H7A 109.0 . . ? C8 C7 H7A 109.0 . . ? N2 C7 H7B 109.0 . . ? C8 C7 H7B 109.0 . . ? H7A C7 H7B 107.8 . . ? N3 C8 C9 123.2(4) . . ? N3 C8 C7 116.8(3) . . ? C9 C8 C7 119.9(3) . . ? C8 C9 C10 118.4(4) . . ? C8 C9 H9 120.8 . . ? C10 C9 H9 120.8 . . ? C11 C10 C9 119.4(4) . . ? C11 C10 H10 120.3 . . ? C9 C10 H10 120.3 . . ? C10 C11 C12 119.5(4) . . ? C10 C11 H11 120.2 . . ? C12 C11 H11 120.2 . . ? N3 C12 C11 120.7(3) . . ? N3 C12 C13 119.0(3) . . ? C11 C12 C13 120.3(3) . . ? C14 C13 C18 118.7(4) . . ? C14 C13 C12 120.9(4) . . ? C18 C13 C12 120.3(3) . . ? C15 C14 C13 120.5(4) . . ? C15 C14 H14 119.7 . . ? C13 C14 H14 119.7 . . ? C16 C15 C14 120.4(4) . . ? C16 C15 H15 119.8 . . ? C14 C15 H15 119.8 . . ? C15 C16 C17 120.0(4) . . ? C15 C16 H16 120.0 . . ? C17 C16 H16 120.0 . . ? C16 C17 C18 120.2(4) . . ? C16 C17 H17 119.9 . . ? C18 C17 H17 119.9 . . ? C17 C18 C13 120.1(4) . . ? C17 C18 H18 120.0 . . ? C13 C18 H18 120.0 . . ? N2 C19 C20 112.0(3) . . ? N2 C19 H19A 109.2 . . ? C20 C19 H19A 109.2 . . ? N2 C19 H19B 109.2 . . ? C20 C19 H19B 109.2 . . ? H19A C19 H19B 107.9 . . ? N4 C20 C21 122.9(3) . . ? N4 C20 C19 116.8(3) . . ? C21 C20 C19 120.2(3) . . ? C20 C21 C22 118.6(4) . . ? C20 C21 H21 120.7 . . ? C22 C21 H21 120.7 . . ? C23 C22 C21 119.1(4) . . ? C23 C22 H22 120.4 . . ? C21 C22 H22 120.4 . . ? C22 C23 C24 119.8(3) . . ? C22 C23 H23 120.1 . . ? C24 C23 H23 120.1 . . ? N4 C24 C23 120.5(3) . . ? N4 C24 C25 117.2(3) . . ? C23 C24 C25 122.3(3) . . ? C26 C25 C30 119.6(4) . . ? C26 C25 C24 120.5(3) . . ? C30 C25 C24 119.9(4) . . ? C25 C26 C27 120.4(4) . . ? C25 C26 H26 119.8 . . ? C27 C26 H26 119.8 . . ? C26 C27 C28 119.3(5) . . ? C26 C27 H27 120.3 . . ? C28 C27 H27 120.3 . . ? C29 C28 C27 119.8(5) . . ? C29 C28 H28 120.1 . . ? C27 C28 H28 120.1 . . ? C28 C29 C30 120.9(5) . . ? C28 C29 H29 119.6 . . ? C30 C29 H29 119.6 . . ? C29 C30 C25 119.9(4) . . ? C29 C30 H30 120.0 . . ? C25 C30 H30 120.0 . . ? O1 C31 C39 121.8(3) . . ? O1 C31 C32 119.8(3) . . ? C39 C31 C32 118.4(3) . . ? O2 C32 C31 121.5(3) . . ? O2 C32 C33 120.8(3) . . ? C31 C32 C33 117.8(3) . . ? C38 C33 C34 118.3(3) . . ? C38 C33 C32 119.3(3) . . ? C34 C33 C32 122.4(3) . . ? C35 C34 C33 120.2(4) . . ? C35 C34 H34 119.9 . . ? C33 C34 H34 119.9 . . ? C34 C35 C36 120.3(4) . . ? C34 C35 H35 119.9 . . ? C36 C35 H35 119.9 . . ? C37 C36 C35 121.2(4) . . ? C37 C36 H36 119.4 . . ? C35 C36 H36 119.4 . . ? C36 C37 C38 118.1(4) . . ? C36 C37 H37 120.9 . . ? C38 C37 H37 120.9 . . ? O3 C38 C33 121.5(3) . . ? O3 C38 C37 116.7(3) . . ? C33 C38 C37 121.8(4) . . ? O3 C39 C31 122.3(3) . . ? O3 C39 C40 110.4(3) . . ? C31 C39 C40 127.2(3) . . ? C45 C40 C41 118.3(4) . . ? C45 C40 C39 120.1(3) . . ? C41 C40 C39 121.6(3) . . ? C42 C41 C40 119.8(4) . . ? C42 C41 H41 120.1 . . ? C40 C41 H41 120.1 . . ? C41 C42 C43 120.4(5) . . ? C41 C42 H42 119.8 . . ? C43 C42 H42 119.8 . . ? C44 C43 C42 120.0(4) . . ? C44 C43 H43 120.0 . . ? C42 C43 H43 120.0 . . ? C43 C44 C45 120.1(4) . . ? C43 C44 H44 120.0 . . ? C45 C44 H44 120.0 . . ? C44 C45 C40 121.3(4) . . ? C44 C45 H45 119.3 . . ? C40 C45 H45 119.3 . . ? 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 Hg1 O1 C31 -0.8(4) . . . . ? O2 Hg1 O1 C31 6.6(2) . . . . ? N2 Hg1 O1 C31 -171.6(2) . . . . ? N4 Hg1 O1 C31 -113.4(2) . . . . ? N3 Hg1 O1 C31 123.5(2) . . . . ? O1 Hg1 O2 C32 -6.9(2) . . . . ? N1 Hg1 O2 C32 170.0(2) . . . . ? N2 Hg1 O2 C32 170.1(2) . . . . ? N4 Hg1 O2 C32 75.8(2) . . . . ? N3 Hg1 O2 C32 -89.1(2) . . . . ? O1 Hg1 N1 C1 17.4(5) . . . . ? O2 Hg1 N1 C1 10.3(3) . . . . ? N2 Hg1 N1 C1 -169.7(3) . . . . ? N4 Hg1 N1 C1 128.8(3) . . . . ? N3 Hg1 N1 C1 -104.6(3) . . . . ? O1 Hg1 N1 C5 -157.9(2) . . . . ? O2 Hg1 N1 C5 -165.0(3) . . . . ? N2 Hg1 N1 C5 15.0(3) . . . . ? N4 Hg1 N1 C5 -46.5(3) . . . . ? N3 Hg1 N1 C5 80.1(3) . . . . ? O1 Hg1 N2 C19 28.4(3) . . . . ? N1 Hg1 N2 C19 -147.5(2) . . . . ? O2 Hg1 N2 C19 -147.6(2) . . . . ? N4 Hg1 N2 C19 -39.9(2) . . . . ? N3 Hg1 N2 C19 100.9(2) . . . . ? O1 Hg1 N2 C6 148.4(2) . . . . ? N1 Hg1 N2 C6 -27.5(2) . . . . ? O2 Hg1 N2 C6 -27.6(3) . . . . ? N4 Hg1 N2 C6 80.1(2) . . . . ? N3 Hg1 N2 C6 -139.1(2) . . . . ? O1 Hg1 N2 C7 -92.4(2) . . . . ? N1 Hg1 N2 C7 91.7(2) . . . . ? O2 Hg1 N2 C7 91.6(3) . . . . ? N4 Hg1 N2 C7 -160.6(3) . . . . ? N3 Hg1 N2 C7 -19.9(2) . . . . ? O1 Hg1 N3 C12 -20.3(3) . . . . ? N1 Hg1 N3 C12 138.9(3) . . . . ? O2 Hg1 N3 C12 51.4(3) . . . . ? N2 Hg1 N3 C12 -156.5(3) . . . . ? N4 Hg1 N3 C12 -112.8(3) . . . . ? O1 Hg1 N3 C8 130.2(2) . . . . ? N1 Hg1 N3 C8 -70.7(2) . . . . ? O2 Hg1 N3 C8 -158.2(2) . . . . ? N2 Hg1 N3 C8 -6.0(2) . . . . ? N4 Hg1 N3 C8 37.7(3) . . . . ? O1 Hg1 N4 C20 -104.9(2) . . . . ? N1 Hg1 N4 C20 98.1(3) . . . . ? O2 Hg1 N4 C20 -176.8(2) . . . . ? N2 Hg1 N4 C20 32.7(2) . . . . ? N3 Hg1 N4 C20 -13.1(3) . . . . ? O1 Hg1 N4 C24 54.0(3) . . . . ? N1 Hg1 N4 C24 -103.0(3) . . . . ? O2 Hg1 N4 C24 -17.9(3) . . . . ? N2 Hg1 N4 C24 -168.4(3) . . . . ? N3 Hg1 N4 C24 145.8(3) . . . . ? C5 N1 C1 C2 0.7(6) . . . . ? Hg1 N1 C1 C2 -174.6(3) . . . . ? N1 C1 C2 C3 -1.6(7) . . . . ? C1 C2 C3 C4 0.4(7) . . . . ? C2 C3 C4 C5 1.6(7) . . . . ? C1 N1 C5 C4 1.4(6) . . . . ? Hg1 N1 C5 C4 176.8(3) . . . . ? C1 N1 C5 C6 -174.7(3) . . . . ? Hg1 N1 C5 C6 0.7(4) . . . . ? C3 C4 C5 N1 -2.5(6) . . . . ? C3 C4 C5 C6 173.4(4) . . . . ? C19 N2 C6 C5 155.9(3) . . . . ? C7 N2 C6 C5 -79.3(4) . . . . ? Hg1 N2 C6 C5 37.9(4) . . . . ? N1 C5 C6 N2 -28.2(5) . . . . ? C4 C5 C6 N2 155.8(4) . . . . ? C19 N2 C7 C8 -74.3(4) . . . . ? C6 N2 C7 C8 161.2(3) . . . . ? Hg1 N2 C7 C8 44.1(4) . . . . ? C12 N3 C8 C9 1.8(5) . . . . ? Hg1 N3 C8 C9 -150.7(3) . . . . ? C12 N3 C8 C7 -174.9(3) . . . . ? Hg1 N3 C8 C7 32.7(3) . . . . ? N2 C7 C8 N3 -55.4(4) . . . . ? N2 C7 C8 C9 127.9(4) . . . . ? N3 C8 C9 C10 -1.5(6) . . . . ? C7 C8 C9 C10 175.0(3) . . . . ? C8 C9 C10 C11 0.7(6) . . . . ? C9 C10 C11 C12 -0.3(5) . . . . ? C8 N3 C12 C11 -1.3(5) . . . . ? Hg1 N3 C12 C11 146.7(3) . . . . ? C8 N3 C12 C13 176.2(3) . . . . ? Hg1 N3 C12 C13 -35.8(4) . . . . ? C10 C11 C12 N3 0.6(5) . . . . ? C10 C11 C12 C13 -176.8(3) . . . . ? N3 C12 C13 C14 152.8(4) . . . . ? C11 C12 C13 C14 -29.8(5) . . . . ? N3 C12 C13 C18 -30.4(5) . . . . ? C11 C12 C13 C18 147.1(4) . . . . ? C18 C13 C14 C15 0.8(6) . . . . ? C12 C13 C14 C15 177.7(4) . . . . ? C13 C14 C15 C16 -0.6(7) . . . . ? C14 C15 C16 C17 0.4(7) . . . . ? C15 C16 C17 C18 -0.5(6) . . . . ? C16 C17 C18 C13 0.7(6) . . . . ? C14 C13 C18 C17 -0.8(5) . . . . ? C12 C13 C18 C17 -177.8(3) . . . . ? C6 N2 C19 C20 -71.6(4) . . . . ? C7 N2 C19 C20 164.2(3) . . . . ? Hg1 N2 C19 C20 46.0(3) . . . . ? C24 N4 C20 C21 -1.1(5) . . . . ? Hg1 N4 C20 C21 158.7(3) . . . . ? C24 N4 C20 C19 -179.6(3) . . . . ? Hg1 N4 C20 C19 -19.7(4) . . . . ? N2 C19 C20 N4 -18.2(5) . . . . ? N2 C19 C20 C21 163.3(3) . . . . ? N4 C20 C21 C22 1.1(6) . . . . ? C19 C20 C21 C22 179.5(4) . . . . ? C20 C21 C22 C23 -0.2(6) . . . . ? C21 C22 C23 C24 -0.7(6) . . . . ? C20 N4 C24 C23 0.2(5) . . . . ? Hg1 N4 C24 C23 -157.7(3) . . . . ? C20 N4 C24 C25 -178.1(3) . . . . ? Hg1 N4 C24 C25 24.0(4) . . . . ? C22 C23 C24 N4 0.6(6) . . . . ? C22 C23 C24 C25 178.9(4) . . . . ? N4 C24 C25 C26 44.3(5) . . . . ? C23 C24 C25 C26 -134.0(4) . . . . ? N4 C24 C25 C30 -134.5(4) . . . . ? C23 C24 C25 C30 47.2(5) . . . . ? C30 C25 C26 C27 -2.5(6) . . . . ? C24 C25 C26 C27 178.7(4) . . . . ? C25 C26 C27 C28 2.1(6) . . . . ? C26 C27 C28 C29 0.1(7) . . . . ? C27 C28 C29 C30 -1.9(7) . . . . ? C28 C29 C30 C25 1.5(7) . . . . ? C26 C25 C30 C29 0.7(6) . . . . ? C24 C25 C30 C29 179.5(4) . . . . ? Hg1 O1 C31 C39 171.6(3) . . . . ? Hg1 O1 C31 C32 -6.0(4) . . . . ? Hg1 O2 C32 C31 6.5(4) . . . . ? Hg1 O2 C32 C33 -172.4(2) . . . . ? O1 C31 C32 O2 -1.0(5) . . . . ? C39 C31 C32 O2 -178.6(3) . . . . ? O1 C31 C32 C33 178.0(3) . . . . ? C39 C31 C32 C33 0.3(5) . . . . ? O2 C32 C33 C38 179.9(3) . . . . ? C31 C32 C33 C38 0.9(5) . . . . ? O2 C32 C33 C34 0.7(5) . . . . ? C31 C32 C33 C34 -178.2(3) . . . . ? C38 C33 C34 C35 0.4(5) . . . . ? C32 C33 C34 C35 179.5(3) . . . . ? C33 C34 C35 C36 1.8(6) . . . . ? C34 C35 C36 C37 -2.1(6) . . . . ? C35 C36 C37 C38 0.2(6) . . . . ? C39 O3 C38 C33 0.1(5) . . . . ? C39 O3 C38 C37 -179.5(3) . . . . ? C34 C33 C38 O3 178.0(3) . . . . ? C32 C33 C38 O3 -1.1(5) . . . . ? C34 C33 C38 C37 -2.4(5) . . . . ? C32 C33 C38 C37 178.5(3) . . . . ? C36 C37 C38 O3 -178.3(3) . . . . ? C36 C37 C38 C33 2.1(6) . . . . ? C38 O3 C39 C31 1.2(5) . . . . ? C38 O3 C39 C40 -176.9(3) . . . . ? O1 C31 C39 O3 -179.0(3) . . . . ? C32 C31 C39 O3 -1.4(5) . . . . ? O1 C31 C39 C40 -1.2(6) . . . . ? C32 C31 C39 C40 176.4(3) . . . . ? O3 C39 C40 C45 42.5(5) . . . . ? C31 C39 C40 C45 -135.5(4) . . . . ? O3 C39 C40 C41 -136.5(3) . . . . ? C31 C39 C40 C41 45.6(5) . . . . ? C45 C40 C41 C42 1.0(6) . . . . ? C39 C40 C41 C42 -180.0(4) . . . . ? C40 C41 C42 C43 -0.5(6) . . . . ? C41 C42 C43 C44 0.9(7) . . . . ? C42 C43 C44 C45 -1.9(7) . . . . ? C43 C44 C45 C40 2.4(7) . . . . ? C41 C40 C45 C44 -2.0(6) . . . . ? C39 C40 C45 C44 179.0(4) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.486 _refine_diff_density_min -0.784 _refine_diff_density_rms 0.107 #===END data_usu197 _database_code_depnum_ccdc_archive 'CCDC 832451' #TrackingRef '- CombinedCIF copy.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C44 H35 N4 O4 Zn, C F3 S O3' _chemical_formula_sum 'C45 H35 F3 N4 O7 S Zn' _chemical_formula_weight 898.20 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c _symmetry_space_group_name_Hall '-P 2ybc' 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 10.1785(2) _cell_length_b 16.3337(5) _cell_length_c 24.1620(5) _cell_angle_alpha 90.00 _cell_angle_beta 91.0370(14) _cell_angle_gamma 90.00 _cell_volume 4016.34(17) _cell_formula_units_Z 4 _cell_measurement_temperature 150(1) _cell_measurement_reflns_used 8374 _cell_measurement_theta_min 1.018 _cell_measurement_theta_max 27.485 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.485 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1848 _exptl_absorpt_coefficient_mu 0.736 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8374 _exptl_absorpt_correction_T_max 0.9104 _exptl_absorpt_process_details 'DENZO-SMN (Otwinowski & Minor, 1997)' _exptl_special_details ; The program Denzo-SMN (Otwinowski & Minor, 1997) uses a scaling algorithm (Fox & Holmes, 1966) which effectively corrects for absorption effects. High redundancy data were used in the scaling program hence the 'multi-scan' code word was used. No transmission coefficients are available from the program (only scale factors for each frame). The scale factors in the experimental table are calculated from the 'size' command in the SHELXL-97 input file. ; _diffrn_ambient_temperature 150(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD Diffractometer' _diffrn_measurement_method 'Phi and Omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15119 _diffrn_reflns_av_R_equivalents 0.0342 _diffrn_reflns_av_sigmaI/netI 0.0668 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 2.00 _diffrn_reflns_theta_max 27.46 _reflns_number_total 9139 _reflns_number_gt 6218 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius COLLECT' _computing_cell_refinement DENZO-SMN _computing_data_reduction DENZO-SMN _computing_structure_solution SIR97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'WinGX, Ortep3' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0429P)^2^+0.9142P] 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 refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9139 _refine_ls_number_parameters 690 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0829 _refine_ls_R_factor_gt 0.0432 _refine_ls_wR_factor_ref 0.1034 _refine_ls_wR_factor_gt 0.0883 _refine_ls_goodness_of_fit_ref 1.016 _refine_ls_restrained_S_all 1.016 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.30765(2) 0.152538(18) 0.306785(10) 0.02407(9) Uani 1 1 d . . . F1 F 0.5992(3) 0.44648(14) 0.46946(8) 0.0988(9) Uani 1 1 d . . . F2 F 0.7971(3) 0.44170(18) 0.50042(11) 0.1168(10) Uani 1 1 d . . . F3 F 0.6373(2) 0.44078(12) 0.55734(7) 0.0695(6) Uani 1 1 d . . . S1 S 0.67409(7) 0.30275(5) 0.50450(3) 0.04009(18) Uani 1 1 d . . . O1 O 0.15704(15) 0.11021(11) 0.26570(7) 0.0302(4) Uani 1 1 d . . . O2 O 0.10100(16) 0.03002(12) 0.33625(7) 0.0365(4) Uani 1 1 d . . . O3 O -0.15889(17) -0.02471(11) 0.33141(7) 0.0348(4) Uani 1 1 d . . . O4 O -0.15856(17) 0.10830(12) 0.35585(8) 0.0391(5) Uani 1 1 d . . . O5 O 0.71438(18) 0.28612(13) 0.44895(7) 0.0404(5) Uani 1 1 d . . . O6 O 0.7614(3) 0.27882(18) 0.54763(9) 0.0799(9) Uani 1 1 d . . . O7 O 0.5378(2) 0.28456(17) 0.51441(9) 0.0662(7) Uani 1 1 d . . . N1 N 0.21097(19) 0.23490(13) 0.35997(8) 0.0301(5) Uani 1 1 d . . . N2 N 0.47025(18) 0.20329(12) 0.35658(8) 0.0255(4) Uani 1 1 d . . . N3 N 0.41182(18) 0.04690(13) 0.33810(8) 0.0264(5) Uani 1 1 d . . . N4 N 0.42926(19) 0.20261(12) 0.24432(8) 0.0258(4) Uani 1 1 d . . . C1 C 0.0822(3) 0.23349(18) 0.37114(11) 0.0350(6) Uani 1 1 d . . . C2 C 0.0276(3) 0.2842(2) 0.41047(12) 0.0424(7) Uani 1 1 d . . . C3 C 0.1079(3) 0.3376(2) 0.43932(12) 0.0468(8) Uani 1 1 d . . . C4 C 0.2409(3) 0.33907(18) 0.42805(11) 0.0401(7) Uani 1 1 d . . . C5 C 0.2890(2) 0.28748(16) 0.38803(10) 0.0307(6) Uani 1 1 d . . . C6 C 0.4312(3) 0.28733(17) 0.37184(11) 0.0318(6) Uani 1 1 d . . . C7 C 0.4847(3) 0.14959(17) 0.40494(10) 0.0292(6) Uani 1 1 d . . . C8 C 0.4698(2) 0.06127(16) 0.38799(10) 0.0272(5) Uani 1 1 d . . . C9 C 0.5110(2) -0.00171(18) 0.42256(11) 0.0344(6) Uani 1 1 d . . . C10 C 0.4885(3) -0.0812(2) 0.40671(13) 0.0429(7) Uani 1 1 d . . . C11 C 0.4308(3) -0.09652(18) 0.35565(13) 0.0409(7) Uani 1 1 d . . . C12 C 0.3957(2) -0.03151(16) 0.32152(10) 0.0300(6) Uani 1 1 d . . . C13 C 0.3448(2) -0.04670(16) 0.26443(10) 0.0306(6) Uani 1 1 d . . . C14 C 0.3960(3) -0.00507(17) 0.21965(11) 0.0348(6) Uani 1 1 d . . . C15 C 0.3495(3) -0.02127(19) 0.16632(12) 0.0406(7) Uani 1 1 d . . . C16 C 0.2517(3) -0.07846(19) 0.15757(13) 0.0432(7) Uani 1 1 d . . . C17 C 0.2009(3) -0.1198(2) 0.20162(13) 0.0421(7) Uani 1 1 d . . . C18 C 0.2474(3) -0.10510(18) 0.25500(12) 0.0362(6) Uani 1 1 d . . . C19 C 0.5877(2) 0.20150(19) 0.32195(11) 0.0316(6) Uani 1 1 d . . . C20 C 0.5566(2) 0.19781(15) 0.26091(10) 0.0276(5) Uani 1 1 d . . . C21 C 0.6573(3) 0.18864(17) 0.22371(11) 0.0335(6) Uani 1 1 d . . . C22 C 0.6272(3) 0.18449(17) 0.16803(12) 0.0370(6) Uani 1 1 d . . . C23 C 0.4975(3) 0.19364(16) 0.15039(11) 0.0334(6) Uani 1 1 d . . . C24 C 0.3995(2) 0.20350(15) 0.18884(9) 0.0273(5) Uani 1 1 d . . . C25 C 0.2620(2) 0.22010(15) 0.17196(10) 0.0286(6) Uani 1 1 d . . . C26 C 0.1836(3) 0.27105(17) 0.20366(10) 0.0328(6) Uani 1 1 d . . . C27 C 0.0562(3) 0.2900(2) 0.18690(12) 0.0402(7) Uani 1 1 d . . . C28 C 0.0051(3) 0.2582(2) 0.13828(12) 0.0452(8) Uani 1 1 d . . . C29 C 0.0802(3) 0.2079(2) 0.10635(12) 0.0477(8) Uani 1 1 d . . . C30 C 0.2087(3) 0.18902(19) 0.12251(11) 0.0400(7) Uani 1 1 d . . . C31 C 0.0824(2) 0.05822(16) 0.28961(9) 0.0282(6) Uani 1 1 d . . . C32 C -0.0356(2) 0.03211(15) 0.25437(10) 0.0269(5) Uani 1 1 d . . . C33 C -0.0332(3) 0.04529(17) 0.19746(11) 0.0321(6) Uani 1 1 d . . . C34 C -0.1362(3) 0.02087(18) 0.16301(11) 0.0361(6) Uani 1 1 d . . . C35 C -0.2453(3) -0.01525(17) 0.18520(11) 0.0364(6) Uani 1 1 d . . . C36 C -0.2511(3) -0.02836(17) 0.24129(12) 0.0350(6) Uani 1 1 d . . . C37 C -0.1465(2) -0.00490(16) 0.27539(10) 0.0292(6) Uani 1 1 d . . . C38 C -0.1577(2) 0.03710(18) 0.36909(11) 0.0332(6) Uani 1 1 d . . . C39 C -0.1636(2) 0.00591(19) 0.42652(11) 0.0364(6) Uani 1 1 d . . . C40 C -0.1702(3) -0.0778(2) 0.43802(12) 0.0413(7) Uani 1 1 d . . . C41 C -0.1779(3) -0.1036(3) 0.49284(13) 0.0506(8) Uani 1 1 d . . . C42 C -0.1770(3) -0.0472(3) 0.53490(13) 0.0564(10) Uani 1 1 d . . . C43 C -0.1708(3) 0.0353(3) 0.52403(13) 0.0546(9) Uani 1 1 d . . . C44 C -0.1638(3) 0.0628(2) 0.46943(12) 0.0453(8) Uani 1 1 d . . . C45 C 0.6751(4) 0.4126(2) 0.50795(12) 0.0569(9) Uani 1 1 d . . . H1 H 0.028(3) 0.1926(17) 0.3516(10) 0.034(7) Uiso 1 1 d . . . H2 H -0.055(3) 0.2810(19) 0.4154(12) 0.049(9) Uiso 1 1 d . . . H3 H 0.068(3) 0.3710(19) 0.4665(12) 0.050(9) Uiso 1 1 d . . . H4 H 0.298(3) 0.3743(17) 0.4464(11) 0.036(7) Uiso 1 1 d . . . H6A H 0.443(3) 0.3216(17) 0.3365(11) 0.035(7) Uiso 1 1 d . . . H6B H 0.487(3) 0.3088(17) 0.3999(11) 0.037(7) Uiso 1 1 d . . . H7A H 0.422(3) 0.1629(16) 0.4308(10) 0.029(7) Uiso 1 1 d . . . H7B H 0.565(3) 0.1558(16) 0.4247(11) 0.036(7) Uiso 1 1 d . . . H9 H 0.550(3) 0.0110(17) 0.4538(11) 0.036(8) Uiso 1 1 d . . . H10 H 0.507(3) -0.1205(18) 0.4291(11) 0.034(8) Uiso 1 1 d . . . H11 H 0.419(3) -0.153(2) 0.3417(12) 0.051(9) Uiso 1 1 d . . . H14 H 0.463(3) 0.0323(17) 0.2255(10) 0.032(7) Uiso 1 1 d . . . H15 H 0.386(3) 0.0051(17) 0.1375(11) 0.032(7) Uiso 1 1 d . . . H16 H 0.223(3) -0.0908(18) 0.1227(11) 0.041(8) Uiso 1 1 d . . . H17 H 0.140(3) -0.1603(19) 0.1968(12) 0.053(9) Uiso 1 1 d . . . H18 H 0.213(3) -0.1332(16) 0.2832(10) 0.028(7) Uiso 1 1 d . . . H19A H 0.647(3) 0.2501(19) 0.3300(11) 0.046(8) Uiso 1 1 d . . . H19B H 0.636(2) 0.1562(16) 0.3309(10) 0.026(7) Uiso 1 1 d . . . H21 H 0.743(3) 0.1845(16) 0.2376(10) 0.033(7) Uiso 1 1 d . . . H22 H 0.695(3) 0.1765(17) 0.1392(11) 0.038(7) Uiso 1 1 d . . . H23 H 0.474(3) 0.1978(18) 0.1120(12) 0.045(8) Uiso 1 1 d . . . H26 H 0.216(2) 0.2935(15) 0.2365(10) 0.025(6) Uiso 1 1 d . . . H27 H 0.010(3) 0.3261(18) 0.2085(12) 0.041(8) Uiso 1 1 d . . . H28 H -0.080(3) 0.274(2) 0.1252(12) 0.057(9) Uiso 1 1 d . . . H29 H 0.054(3) 0.1808(18) 0.0723(12) 0.048(8) Uiso 1 1 d . . . H30 H 0.259(3) 0.1519(17) 0.1031(11) 0.035(8) Uiso 1 1 d . . . H33 H 0.040(3) 0.0689(17) 0.1825(11) 0.037(8) Uiso 1 1 d . . . H34 H -0.130(2) 0.0299(16) 0.1254(11) 0.031(7) Uiso 1 1 d . . . H35 H -0.320(3) -0.0303(18) 0.1631(12) 0.050(8) Uiso 1 1 d . . . H36 H -0.324(3) -0.0496(18) 0.2571(11) 0.046(8) Uiso 1 1 d . . . H40 H -0.177(3) -0.121(2) 0.4062(13) 0.059(9) Uiso 1 1 d . . . H41 H -0.182(3) -0.159(2) 0.4995(13) 0.054(10) Uiso 1 1 d . . . H42 H -0.178(3) -0.0679(19) 0.5748(13) 0.058(9) Uiso 1 1 d . . . H43 H -0.172(3) 0.0777(17) 0.5528(11) 0.037(7) Uiso 1 1 d . . . H44 H -0.161(3) 0.120(2) 0.4578(11) 0.043(8) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.01950(13) 0.02859(17) 0.02407(14) -0.00114(12) -0.00114(10) -0.00114(12) F1 0.180(3) 0.0737(16) 0.0426(11) 0.0030(10) 0.0025(14) 0.0607(17) F2 0.134(2) 0.104(2) 0.113(2) -0.0383(16) 0.0362(18) -0.0684(19) F3 0.1076(17) 0.0611(13) 0.0397(10) -0.0189(9) -0.0024(10) 0.0149(12) S1 0.0421(4) 0.0518(5) 0.0263(3) -0.0062(3) -0.0025(3) 0.0066(3) O1 0.0241(9) 0.0340(10) 0.0322(9) 0.0014(8) -0.0035(7) -0.0051(8) O2 0.0269(9) 0.0536(13) 0.0289(9) 0.0050(9) -0.0022(7) 0.0030(9) O3 0.0357(10) 0.0362(11) 0.0326(9) 0.0005(8) 0.0020(8) -0.0041(8) O4 0.0312(10) 0.0363(12) 0.0499(11) -0.0018(9) 0.0012(8) 0.0055(9) O5 0.0338(10) 0.0562(13) 0.0313(9) -0.0097(9) 0.0048(8) 0.0013(9) O6 0.0958(19) 0.097(2) 0.0460(13) -0.0126(13) -0.0289(13) 0.0511(17) O7 0.0552(14) 0.100(2) 0.0441(12) -0.0182(13) 0.0209(10) -0.0244(14) N1 0.0279(11) 0.0326(13) 0.0296(10) -0.0002(9) -0.0005(9) 0.0032(9) N2 0.0223(10) 0.0270(12) 0.0271(10) -0.0004(9) -0.0039(8) -0.0022(9) N3 0.0188(9) 0.0281(12) 0.0323(10) 0.0008(9) -0.0022(8) -0.0006(8) N4 0.0239(10) 0.0244(12) 0.0293(10) -0.0016(9) 0.0019(8) -0.0032(9) C1 0.0275(13) 0.0378(17) 0.0399(14) 0.0024(13) 0.0021(12) 0.0051(12) C2 0.0369(16) 0.0467(19) 0.0438(16) 0.0075(14) 0.0109(13) 0.0108(15) C3 0.059(2) 0.045(2) 0.0369(15) 0.0005(14) 0.0153(14) 0.0169(16) C4 0.0535(18) 0.0321(16) 0.0347(14) -0.0076(13) -0.0034(13) 0.0057(14) C5 0.0340(13) 0.0305(15) 0.0274(12) 0.0023(11) -0.0043(11) 0.0036(11) C6 0.0307(13) 0.0307(15) 0.0337(14) -0.0043(12) -0.0046(11) -0.0026(11) C7 0.0264(12) 0.0317(15) 0.0293(12) 0.0004(12) -0.0061(11) -0.0007(12) C8 0.0168(11) 0.0333(15) 0.0315(12) 0.0007(11) 0.0020(10) -0.0009(10) C9 0.0264(13) 0.0412(17) 0.0353(14) 0.0071(13) -0.0033(11) -0.0006(12) C10 0.0376(15) 0.0382(18) 0.0526(18) 0.0171(15) -0.0082(14) 0.0019(14) C11 0.0380(15) 0.0254(16) 0.0589(18) 0.0024(14) -0.0091(14) 0.0004(12) C12 0.0206(12) 0.0270(14) 0.0424(14) -0.0005(12) -0.0028(10) 0.0005(10) C13 0.0252(12) 0.0269(14) 0.0395(14) -0.0066(11) -0.0024(11) 0.0045(11) C14 0.0293(14) 0.0301(15) 0.0451(16) -0.0094(13) 0.0017(12) 0.0003(12) C15 0.0444(17) 0.0380(18) 0.0397(16) -0.0071(14) 0.0095(13) 0.0028(14) C16 0.0429(16) 0.0450(19) 0.0416(16) -0.0160(14) -0.0034(13) 0.0036(14) C17 0.0342(15) 0.0379(17) 0.0539(18) -0.0162(15) -0.0057(13) -0.0023(14) C18 0.0293(14) 0.0317(17) 0.0476(16) -0.0060(13) -0.0002(13) 0.0001(12) C19 0.0206(12) 0.0356(17) 0.0385(14) 0.0007(13) -0.0015(11) -0.0028(12) C20 0.0249(12) 0.0208(13) 0.0372(13) -0.0005(11) 0.0039(10) -0.0022(10) C21 0.0269(13) 0.0272(15) 0.0466(16) -0.0005(12) 0.0067(12) 0.0006(11) C22 0.0403(15) 0.0289(15) 0.0424(15) -0.0013(12) 0.0168(13) 0.0009(13) C23 0.0413(15) 0.0253(15) 0.0337(14) 0.0006(11) 0.0075(12) -0.0013(12) C24 0.0339(13) 0.0220(13) 0.0263(12) -0.0006(10) 0.0043(10) -0.0042(11) C25 0.0334(13) 0.0259(14) 0.0266(12) 0.0023(10) 0.0005(10) -0.0045(11) C26 0.0345(14) 0.0346(16) 0.0291(13) 0.0019(11) -0.0043(11) -0.0019(12) C27 0.0345(15) 0.0441(19) 0.0419(16) 0.0044(14) -0.0022(13) 0.0033(14) C28 0.0384(16) 0.052(2) 0.0451(16) 0.0145(15) -0.0133(14) -0.0076(15) C29 0.0560(19) 0.053(2) 0.0335(15) 0.0043(14) -0.0166(14) -0.0122(16) C30 0.0525(18) 0.0395(17) 0.0278(13) -0.0019(12) -0.0011(13) -0.0005(15) C31 0.0224(12) 0.0365(16) 0.0258(12) -0.0034(11) 0.0006(10) 0.0051(11) C32 0.0233(12) 0.0249(14) 0.0323(12) 0.0007(11) -0.0025(10) 0.0011(10) C33 0.0296(14) 0.0348(16) 0.0319(13) -0.0014(12) -0.0001(11) -0.0006(12) C34 0.0362(15) 0.0420(17) 0.0299(14) -0.0061(12) -0.0070(12) -0.0018(13) C35 0.0314(14) 0.0364(17) 0.0412(15) -0.0065(13) -0.0080(12) -0.0011(12) C36 0.0265(13) 0.0299(16) 0.0484(16) 0.0005(13) -0.0016(12) -0.0064(12) C37 0.0295(13) 0.0292(14) 0.0289(12) 0.0028(11) 0.0013(10) -0.0004(11) C38 0.0181(12) 0.0383(17) 0.0431(15) -0.0033(13) 0.0007(11) 0.0019(11) C39 0.0206(12) 0.0537(19) 0.0352(14) -0.0029(13) 0.0038(10) -0.0015(12) C40 0.0316(14) 0.054(2) 0.0386(15) 0.0057(14) 0.0026(12) 0.0033(14) C41 0.0416(17) 0.068(3) 0.0423(17) 0.0165(17) 0.0029(13) 0.0018(17) C42 0.0363(17) 0.100(3) 0.0325(16) 0.0066(18) 0.0027(13) -0.0059(18) C43 0.0340(16) 0.091(3) 0.0389(17) -0.0156(19) 0.0051(13) -0.0091(17) C44 0.0286(14) 0.063(2) 0.0441(17) -0.0071(16) 0.0046(12) -0.0037(14) C45 0.077(2) 0.058(2) 0.0363(16) -0.0103(15) 0.0057(16) -0.0013(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O1 1.9387(15) . ? Zn1 N1 2.115(2) . ? Zn1 N4 2.132(2) . ? Zn1 N3 2.155(2) . ? Zn1 N2 2.1913(18) . ? F1 C45 1.320(4) . ? F2 C45 1.345(4) . ? F3 C45 1.342(3) . ? S1 O6 1.413(2) . ? S1 O5 1.4366(18) . ? S1 O7 1.442(2) . ? S1 C45 1.797(4) . ? O1 C31 1.284(3) . ? O2 C31 1.229(3) . ? O3 C38 1.359(3) . ? O3 C37 1.400(3) . ? O4 C38 1.206(3) . ? N1 C1 1.343(3) . ? N1 C5 1.345(3) . ? N2 C7 1.466(3) . ? N2 C19 1.472(3) . ? N2 C6 1.478(3) . ? N3 C12 1.351(3) . ? N3 C8 1.353(3) . ? N4 C20 1.352(3) . ? N4 C24 1.369(3) . ? C1 C2 1.384(4) . ? C1 H1 0.98(3) . ? C2 C3 1.376(5) . ? C2 H2 0.86(3) . ? C3 C4 1.386(4) . ? C3 H3 0.95(3) . ? C4 C5 1.379(4) . ? C4 H4 0.92(3) . ? C5 C6 1.506(4) . ? C6 H6A 1.03(3) . ? C6 H6B 0.94(3) . ? C7 C8 1.506(4) . ? C7 H7A 0.93(3) . ? C7 H7B 0.95(3) . ? C8 C9 1.385(4) . ? C9 C10 1.371(4) . ? C9 H9 0.87(3) . ? C10 C11 1.380(4) . ? C10 H10 0.86(3) . ? C11 C12 1.387(4) . ? C11 H11 0.99(3) . ? C12 C13 1.485(3) . ? C13 C14 1.387(4) . ? C13 C18 1.392(4) . ? C14 C15 1.390(4) . ? C14 H14 0.93(3) . ? C15 C16 1.379(4) . ? C15 H15 0.90(3) . ? C16 C17 1.369(4) . ? C16 H16 0.91(3) . ? C17 C18 1.387(4) . ? C17 H17 0.91(3) . ? C18 H18 0.90(3) . ? C19 C20 1.504(3) . ? C19 H19A 1.01(3) . ? C19 H19B 0.91(3) . ? C20 C21 1.383(4) . ? C21 C22 1.376(4) . ? C21 H21 0.94(3) . ? C22 C23 1.388(4) . ? C22 H22 0.99(3) . ? C23 C24 1.385(4) . ? C23 H23 0.96(3) . ? C24 C25 1.476(3) . ? C25 C26 1.392(4) . ? C25 C30 1.399(3) . ? C26 C27 1.387(4) . ? C26 H26 0.93(2) . ? C27 C28 1.377(4) . ? C27 H27 0.92(3) . ? C28 C29 1.369(5) . ? C28 H28 0.95(3) . ? C29 C30 1.393(4) . ? C29 H29 0.97(3) . ? C30 H30 0.93(3) . ? C31 C32 1.520(3) . ? C32 C37 1.385(3) . ? C32 C33 1.393(3) . ? C33 C34 1.385(3) . ? C33 H33 0.92(3) . ? C34 C35 1.375(4) . ? C34 H34 0.92(2) . ? C35 C36 1.375(4) . ? C35 H35 0.95(3) . ? C36 C37 1.388(3) . ? C36 H36 0.91(3) . ? C38 C39 1.480(4) . ? C39 C44 1.392(4) . ? C39 C40 1.397(4) . ? C40 C41 1.393(4) . ? C40 H40 1.04(3) . ? C41 C42 1.371(5) . ? C41 H41 0.93(3) . ? C42 C43 1.375(5) . ? C42 H42 1.02(3) . ? C43 C44 1.396(5) . ? C43 H43 0.98(3) . ? C44 H44 0.98(3) . ? 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 Zn1 N1 99.53(7) . . ? O1 Zn1 N4 103.78(7) . . ? N1 Zn1 N4 117.93(8) . . ? O1 Zn1 N3 105.88(7) . . ? N1 Zn1 N3 121.81(8) . . ? N4 Zn1 N3 105.51(8) . . ? O1 Zn1 N2 176.79(8) . . ? N1 Zn1 N2 77.34(7) . . ? N4 Zn1 N2 78.53(7) . . ? N3 Zn1 N2 75.42(7) . . ? O6 S1 O5 116.77(14) . . ? O6 S1 O7 114.51(17) . . ? O5 S1 O7 114.05(12) . . ? O6 S1 C45 103.83(16) . . ? O5 S1 C45 103.35(14) . . ? O7 S1 C45 101.71(17) . . ? C31 O1 Zn1 118.34(14) . . ? C38 O3 C37 118.4(2) . . ? C1 N1 C5 118.6(2) . . ? C1 N1 Zn1 125.27(19) . . ? C5 N1 Zn1 115.81(17) . . ? C7 N2 C19 111.8(2) . . ? C7 N2 C6 112.4(2) . . ? C19 N2 C6 112.6(2) . . ? C7 N2 Zn1 105.95(14) . . ? C19 N2 Zn1 107.06(14) . . ? C6 N2 Zn1 106.54(14) . . ? C12 N3 C8 118.5(2) . . ? C12 N3 Zn1 126.75(15) . . ? C8 N3 Zn1 112.20(16) . . ? C20 N4 C24 119.0(2) . . ? C20 N4 Zn1 109.49(15) . . ? C24 N4 Zn1 125.18(15) . . ? N1 C1 C2 122.2(3) . . ? N1 C1 H1 117.3(16) . . ? C2 C1 H1 120.5(16) . . ? C3 C2 C1 119.0(3) . . ? C3 C2 H2 123(2) . . ? C1 C2 H2 118(2) . . ? C2 C3 C4 119.0(3) . . ? C2 C3 H3 117.4(18) . . ? C4 C3 H3 123.7(19) . . ? C5 C4 C3 119.2(3) . . ? C5 C4 H4 119.4(17) . . ? C3 C4 H4 121.4(17) . . ? N1 C5 C4 122.0(3) . . ? N1 C5 C6 115.4(2) . . ? C4 C5 C6 122.6(2) . . ? N2 C6 C5 109.3(2) . . ? N2 C6 H6A 105.3(15) . . ? C5 C6 H6A 109.7(15) . . ? N2 C6 H6B 111.4(17) . . ? C5 C6 H6B 112.2(17) . . ? H6A C6 H6B 109(2) . . ? N2 C7 C8 110.38(19) . . ? N2 C7 H7A 109.7(16) . . ? C8 C7 H7A 110.0(16) . . ? N2 C7 H7B 114.2(16) . . ? C8 C7 H7B 108.8(16) . . ? H7A C7 H7B 104(2) . . ? N3 C8 C9 122.1(2) . . ? N3 C8 C7 116.6(2) . . ? C9 C8 C7 121.3(2) . . ? C10 C9 C8 119.2(2) . . ? C10 C9 H9 122.5(19) . . ? C8 C9 H9 118.3(19) . . ? C9 C10 C11 119.2(3) . . ? C9 C10 H10 119.9(18) . . ? C11 C10 H10 120.9(18) . . ? C10 C11 C12 119.6(3) . . ? C10 C11 H11 121.4(17) . . ? C12 C11 H11 118.9(17) . . ? N3 C12 C11 121.4(2) . . ? N3 C12 C13 118.2(2) . . ? C11 C12 C13 120.4(2) . . ? C14 C13 C18 119.0(2) . . ? C14 C13 C12 120.8(2) . . ? C18 C13 C12 120.1(2) . . ? C13 C14 C15 120.2(3) . . ? C13 C14 H14 119.4(16) . . ? C15 C14 H14 120.3(16) . . ? C16 C15 C14 120.2(3) . . ? C16 C15 H15 120.6(17) . . ? C14 C15 H15 119.1(17) . . ? C17 C16 C15 119.8(3) . . ? C17 C16 H16 119.5(18) . . ? C15 C16 H16 120.7(18) . . ? C16 C17 C18 120.7(3) . . ? C16 C17 H17 121.5(19) . . ? C18 C17 H17 117.6(19) . . ? C17 C18 C13 120.1(3) . . ? C17 C18 H18 119.0(16) . . ? C13 C18 H18 121.0(16) . . ? N2 C19 C20 113.58(19) . . ? N2 C19 H19A 111.1(17) . . ? C20 C19 H19A 109.5(16) . . ? N2 C19 H19B 108.8(16) . . ? C20 C19 H19B 107.7(15) . . ? H19A C19 H19B 106(2) . . ? N4 C20 C21 122.1(2) . . ? N4 C20 C19 118.1(2) . . ? C21 C20 C19 119.8(2) . . ? C22 C21 C20 119.1(2) . . ? C22 C21 H21 122.5(16) . . ? C20 C21 H21 118.4(16) . . ? C21 C22 C23 119.2(3) . . ? C21 C22 H22 123.2(15) . . ? C23 C22 H22 117.6(15) . . ? C24 C23 C22 120.0(2) . . ? C24 C23 H23 118.1(17) . . ? C22 C23 H23 121.7(17) . . ? N4 C24 C23 120.4(2) . . ? N4 C24 C25 117.7(2) . . ? C23 C24 C25 121.8(2) . . ? C26 C25 C30 118.0(2) . . ? C26 C25 C24 120.5(2) . . ? C30 C25 C24 121.4(2) . . ? C27 C26 C25 121.0(2) . . ? C27 C26 H26 118.5(15) . . ? C25 C26 H26 120.5(15) . . ? C28 C27 C26 120.1(3) . . ? C28 C27 H27 122.4(17) . . ? C26 C27 H27 117.5(17) . . ? C29 C28 C27 120.0(3) . . ? C29 C28 H28 119.4(19) . . ? C27 C28 H28 120.4(19) . . ? C28 C29 C30 120.4(3) . . ? C28 C29 H29 127.0(18) . . ? C30 C29 H29 112.6(18) . . ? C29 C30 C25 120.4(3) . . ? C29 C30 H30 121.8(16) . . ? C25 C30 H30 117.5(16) . . ? O2 C31 O1 125.3(2) . . ? O2 C31 C32 121.0(2) . . ? O1 C31 C32 113.7(2) . . ? C37 C32 C33 117.3(2) . . ? C37 C32 C31 123.9(2) . . ? C33 C32 C31 118.8(2) . . ? C34 C33 C32 121.5(3) . . ? C34 C33 H33 119.7(16) . . ? C32 C33 H33 118.8(16) . . ? C35 C34 C33 119.8(3) . . ? C35 C34 H34 121.5(16) . . ? C33 C34 H34 118.7(16) . . ? C34 C35 C36 120.1(2) . . ? C34 C35 H35 122.1(18) . . ? C36 C35 H35 117.8(18) . . ? C35 C36 C37 119.7(3) . . ? C35 C36 H36 121.6(17) . . ? C37 C36 H36 118.6(18) . . ? C32 C37 C36 121.6(2) . . ? C32 C37 O3 122.9(2) . . ? C36 C37 O3 115.4(2) . . ? O4 C38 O3 122.6(2) . . ? O4 C38 C39 125.5(3) . . ? O3 C38 C39 111.8(2) . . ? C44 C39 C40 120.3(3) . . ? C44 C39 C38 118.0(3) . . ? C40 C39 C38 121.7(3) . . ? C41 C40 C39 119.3(3) . . ? C41 C40 H40 119.6(18) . . ? C39 C40 H40 121.0(18) . . ? C42 C41 C40 120.1(4) . . ? C42 C41 H41 122(2) . . ? C40 C41 H41 118(2) . . ? C41 C42 C43 121.1(3) . . ? C41 C42 H42 118.5(18) . . ? C43 C42 H42 120.4(18) . . ? C42 C43 C44 119.9(3) . . ? C42 C43 H43 123.6(16) . . ? C44 C43 H43 116.5(17) . . ? C39 C44 C43 119.4(4) . . ? C39 C44 H44 115.2(17) . . ? C43 C44 H44 125.4(17) . . ? F1 C45 F3 108.0(3) . . ? F1 C45 F2 106.7(3) . . ? F3 C45 F2 106.2(3) . . ? F1 C45 S1 112.5(2) . . ? F3 C45 S1 112.5(2) . . ? F2 C45 S1 110.6(3) . . ? 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 Zn1 O1 C31 -75.53(18) . . . . ? N4 Zn1 O1 C31 162.46(17) . . . . ? N3 Zn1 O1 C31 51.60(19) . . . . ? N2 Zn1 O1 C31 -61.8(14) . . . . ? O1 Zn1 N1 C1 18.3(2) . . . . ? N4 Zn1 N1 C1 129.6(2) . . . . ? N3 Zn1 N1 C1 -97.2(2) . . . . ? N2 Zn1 N1 C1 -160.9(2) . . . . ? O1 Zn1 N1 C5 -167.91(17) . . . . ? N4 Zn1 N1 C5 -56.66(19) . . . . ? N3 Zn1 N1 C5 76.57(19) . . . . ? N2 Zn1 N1 C5 12.87(17) . . . . ? O1 Zn1 N2 C7 76.0(14) . . . . ? N1 Zn1 N2 C7 89.85(16) . . . . ? N4 Zn1 N2 C7 -147.78(17) . . . . ? N3 Zn1 N2 C7 -38.22(15) . . . . ? O1 Zn1 N2 C19 -164.6(13) . . . . ? N1 Zn1 N2 C19 -150.74(17) . . . . ? N4 Zn1 N2 C19 -28.37(16) . . . . ? N3 Zn1 N2 C19 81.18(17) . . . . ? O1 Zn1 N2 C6 -43.8(14) . . . . ? N1 Zn1 N2 C6 -30.00(16) . . . . ? N4 Zn1 N2 C6 92.37(16) . . . . ? N3 Zn1 N2 C6 -158.07(17) . . . . ? O1 Zn1 N3 C12 15.0(2) . . . . ? N1 Zn1 N3 C12 127.3(2) . . . . ? N4 Zn1 N3 C12 -94.7(2) . . . . ? N2 Zn1 N3 C12 -168.1(2) . . . . ? O1 Zn1 N3 C8 -146.52(16) . . . . ? N1 Zn1 N3 C8 -34.24(19) . . . . ? N4 Zn1 N3 C8 103.85(16) . . . . ? N2 Zn1 N3 C8 30.43(16) . . . . ? O1 Zn1 N4 C20 -150.46(16) . . . . ? N1 Zn1 N4 C20 100.69(17) . . . . ? N3 Zn1 N4 C20 -39.33(17) . . . . ? N2 Zn1 N4 C20 31.83(16) . . . . ? O1 Zn1 N4 C24 1.0(2) . . . . ? N1 Zn1 N4 C24 -107.8(2) . . . . ? N3 Zn1 N4 C24 112.15(19) . . . . ? N2 Zn1 N4 C24 -176.7(2) . . . . ? C5 N1 C1 C2 -0.1(4) . . . . ? Zn1 N1 C1 C2 173.6(2) . . . . ? N1 C1 C2 C3 -0.3(4) . . . . ? C1 C2 C3 C4 0.1(4) . . . . ? C2 C3 C4 C5 0.5(4) . . . . ? C1 N1 C5 C4 0.6(4) . . . . ? Zn1 N1 C5 C4 -173.6(2) . . . . ? C1 N1 C5 C6 -178.1(2) . . . . ? Zn1 N1 C5 C6 7.7(3) . . . . ? C3 C4 C5 N1 -0.8(4) . . . . ? C3 C4 C5 C6 177.8(3) . . . . ? C7 N2 C6 C5 -73.4(2) . . . . ? C19 N2 C6 C5 159.27(19) . . . . ? Zn1 N2 C6 C5 42.2(2) . . . . ? N1 C5 C6 N2 -34.6(3) . . . . ? C4 C5 C6 N2 146.8(2) . . . . ? C19 N2 C7 C8 -75.1(2) . . . . ? C6 N2 C7 C8 157.2(2) . . . . ? Zn1 N2 C7 C8 41.2(2) . . . . ? C12 N3 C8 C9 -0.9(3) . . . . ? Zn1 N3 C8 C9 162.2(2) . . . . ? C12 N3 C8 C7 -179.5(2) . . . . ? Zn1 N3 C8 C7 -16.3(3) . . . . ? N2 C7 C8 N3 -17.8(3) . . . . ? N2 C7 C8 C9 163.7(2) . . . . ? N3 C8 C9 C10 -2.2(4) . . . . ? C7 C8 C9 C10 176.2(3) . . . . ? C8 C9 C10 C11 2.9(4) . . . . ? C9 C10 C11 C12 -0.5(5) . . . . ? C8 N3 C12 C11 3.4(4) . . . . ? Zn1 N3 C12 C11 -157.0(2) . . . . ? C8 N3 C12 C13 -173.7(2) . . . . ? Zn1 N3 C12 C13 25.8(3) . . . . ? C10 C11 C12 N3 -2.8(4) . . . . ? C10 C11 C12 C13 174.4(3) . . . . ? N3 C12 C13 C14 46.5(3) . . . . ? C11 C12 C13 C14 -130.7(3) . . . . ? N3 C12 C13 C18 -135.5(3) . . . . ? C11 C12 C13 C18 47.3(4) . . . . ? C18 C13 C14 C15 0.5(4) . . . . ? C12 C13 C14 C15 178.5(2) . . . . ? C13 C14 C15 C16 0.4(4) . . . . ? C14 C15 C16 C17 -0.5(4) . . . . ? C15 C16 C17 C18 -0.4(5) . . . . ? C16 C17 C18 C13 1.3(4) . . . . ? C14 C13 C18 C17 -1.3(4) . . . . ? C12 C13 C18 C17 -179.4(2) . . . . ? C7 N2 C19 C20 137.3(2) . . . . ? C6 N2 C19 C20 -95.1(3) . . . . ? Zn1 N2 C19 C20 21.7(3) . . . . ? C24 N4 C20 C21 -4.1(4) . . . . ? Zn1 N4 C20 C21 149.4(2) . . . . ? C24 N4 C20 C19 176.8(2) . . . . ? Zn1 N4 C20 C19 -29.7(3) . . . . ? N2 C19 C20 N4 4.8(3) . . . . ? N2 C19 C20 C21 -174.4(2) . . . . ? N4 C20 C21 C22 0.2(4) . . . . ? C19 C20 C21 C22 179.3(3) . . . . ? C20 C21 C22 C23 3.1(4) . . . . ? C21 C22 C23 C24 -2.6(4) . . . . ? C20 N4 C24 C23 4.6(4) . . . . ? Zn1 N4 C24 C23 -144.4(2) . . . . ? C20 N4 C24 C25 -171.8(2) . . . . ? Zn1 N4 C24 C25 39.2(3) . . . . ? C22 C23 C24 N4 -1.3(4) . . . . ? C22 C23 C24 C25 175.0(2) . . . . ? N4 C24 C25 C26 31.6(3) . . . . ? C23 C24 C25 C26 -144.8(3) . . . . ? N4 C24 C25 C30 -151.8(2) . . . . ? C23 C24 C25 C30 31.8(4) . . . . ? C30 C25 C26 C27 0.4(4) . . . . ? C24 C25 C26 C27 177.1(3) . . . . ? C25 C26 C27 C28 0.1(4) . . . . ? C26 C27 C28 C29 -0.1(5) . . . . ? C27 C28 C29 C30 -0.4(5) . . . . ? C28 C29 C30 C25 1.0(5) . . . . ? C26 C25 C30 C29 -0.9(4) . . . . ? C24 C25 C30 C29 -177.6(3) . . . . ? Zn1 O1 C31 O2 -3.0(3) . . . . ? Zn1 O1 C31 C32 177.53(15) . . . . ? O2 C31 C32 C37 18.6(4) . . . . ? O1 C31 C32 C37 -162.0(2) . . . . ? O2 C31 C32 C33 -161.0(2) . . . . ? O1 C31 C32 C33 18.5(3) . . . . ? C37 C32 C33 C34 -1.3(4) . . . . ? C31 C32 C33 C34 178.3(2) . . . . ? C32 C33 C34 C35 1.8(4) . . . . ? C33 C34 C35 C36 -1.1(4) . . . . ? C34 C35 C36 C37 0.1(4) . . . . ? C33 C32 C37 C36 0.3(4) . . . . ? C31 C32 C37 C36 -179.3(2) . . . . ? C33 C32 C37 O3 177.2(2) . . . . ? C31 C32 C37 O3 -2.4(4) . . . . ? C35 C36 C37 C32 0.4(4) . . . . ? C35 C36 C37 O3 -176.8(2) . . . . ? C38 O3 C37 C32 63.0(3) . . . . ? C38 O3 C37 C36 -119.9(3) . . . . ? C37 O3 C38 O4 6.9(3) . . . . ? C37 O3 C38 C39 -176.6(2) . . . . ? O4 C38 C39 C44 -3.3(4) . . . . ? O3 C38 C39 C44 -179.7(2) . . . . ? O4 C38 C39 C40 176.1(3) . . . . ? O3 C38 C39 C40 -0.3(3) . . . . ? C44 C39 C40 C41 0.5(4) . . . . ? C38 C39 C40 C41 -178.9(2) . . . . ? C39 C40 C41 C42 -1.0(4) . . . . ? C40 C41 C42 C43 1.1(5) . . . . ? C41 C42 C43 C44 -0.7(5) . . . . ? C40 C39 C44 C43 -0.1(4) . . . . ? C38 C39 C44 C43 179.3(2) . . . . ? C42 C43 C44 C39 0.2(4) . . . . ? O6 S1 C45 F1 179.0(3) . . . . ? O5 S1 C45 F1 56.6(3) . . . . ? O7 S1 C45 F1 -61.8(3) . . . . ? O6 S1 C45 F3 -58.7(3) . . . . ? O5 S1 C45 F3 178.9(2) . . . . ? O7 S1 C45 F3 60.5(3) . . . . ? O6 S1 C45 F2 59.8(3) . . . . ? O5 S1 C45 F2 -62.5(3) . . . . ? O7 S1 C45 F2 179.0(2) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.332 _refine_diff_density_min -0.482 _refine_diff_density_rms 0.065 #===END data_usu205 _database_code_depnum_ccdc_archive 'CCDC 832452' #TrackingRef '- CombinedCIF copy.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C44 H35 Cd N4 O4, Cl O4, C2 H3 N' _chemical_formula_sum 'C46 H38 Cd Cl N5 O8' _chemical_formula_weight 936.66 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.2066(2) _cell_length_b 13.24300(10) _cell_length_c 14.3060(2) _cell_angle_alpha 102.5400(9) _cell_angle_beta 116.8087(6) _cell_angle_gamma 99.7178(9) _cell_volume 2075.18(5) _cell_formula_units_Z 2 _cell_measurement_temperature 150(1) _cell_measurement_reflns_used 9137 _cell_measurement_theta_min 1.018 _cell_measurement_theta_max 27.485 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.499 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 956 _exptl_absorpt_coefficient_mu 0.652 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8644 _exptl_absorpt_correction_T_max 0.9200 _exptl_absorpt_process_details 'DENZO-SMN (Otwinowski & Minor, 1997)' _exptl_special_details ; The program Denzo-SMN (Otwinowski & Minor, 1997) uses a scaling algorithm (Fox & Holmes, 1966) which effectively corrects for absorption effects. High redundancy data were used in the scaling program hence the 'multi-scan' code word was used. No transmission coefficients are available from the program (only scale factors for each frame). The scale factors in the experimental table are calculated from the 'size' command in the SHELXL-97 input file. ; _diffrn_ambient_temperature 150(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD Diffractometer' _diffrn_measurement_method 'Phi and Omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17877 _diffrn_reflns_av_R_equivalents 0.0202 _diffrn_reflns_av_sigmaI/netI 0.0355 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.41 _diffrn_reflns_theta_max 27.47 _reflns_number_total 9483 _reflns_number_gt 8015 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius COLLECT' _computing_cell_refinement DENZO-SMN _computing_data_reduction DENZO-SMN _computing_structure_solution SIR97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'WinGX, Ortep3' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0314P)^2^+1.6605P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0045(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 9483 _refine_ls_number_parameters 571 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0469 _refine_ls_R_factor_gt 0.0348 _refine_ls_wR_factor_ref 0.0803 _refine_ls_wR_factor_gt 0.0749 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.037 _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 Cd1 Cd 0.250333(14) 0.219526(13) 0.824474(13) 0.02710(7) Uani 1 1 d . . . Cl1 Cl 0.08992(6) 0.39491(7) 0.24998(6) 0.0528(2) Uani 1 1 d . . . O1 O 0.36304(14) 0.15922(12) 0.74267(13) 0.0314(4) Uani 1 1 d . . . O2 O 0.34803(14) 0.09859(13) 0.86903(13) 0.0328(4) Uani 1 1 d . . . O3 O 0.47979(15) 0.07149(14) 0.64887(14) 0.0354(4) Uani 1 1 d . . . O4 O 0.67534(16) 0.16674(15) 0.74501(15) 0.0448(4) Uani 1 1 d . . . N1 N 0.21487(17) 0.32723(15) 0.71084(15) 0.0298(4) Uani 1 1 d . . . N2 N 0.12092(16) 0.31304(15) 0.84909(15) 0.0288(4) Uani 1 1 d . . . N3 N 0.05195(16) 0.08401(15) 0.72429(15) 0.0301(4) Uani 1 1 d . . . N4 N 0.35278(16) 0.34620(14) 1.01191(14) 0.0254(4) Uani 1 1 d . . . N5 N 0.8483(5) 0.8937(3) -0.0077(4) 0.193(3) Uani 1 1 d . . . C1 C 0.2325(2) 0.31226(19) 0.62402(19) 0.0345(5) Uani 1 1 d . . . H1 H 0.2727 0.2616 0.6134 0.041 Uiso 1 1 calc R . . C2 C 0.1943(2) 0.3679(2) 0.5496(2) 0.0392(6) Uani 1 1 d . . . H2 H 0.2079 0.3559 0.4889 0.047 Uiso 1 1 calc R . . C3 C 0.1360(2) 0.4412(2) 0.5653(2) 0.0408(6) Uani 1 1 d . . . H3 H 0.1088 0.4804 0.5153 0.049 Uiso 1 1 calc R . . C4 C 0.1175(2) 0.4571(2) 0.65430(19) 0.0372(6) Uani 1 1 d . . . H4 H 0.0773 0.5072 0.6662 0.045 Uiso 1 1 calc R . . C5 C 0.1584(2) 0.39887(18) 0.72628(18) 0.0297(5) Uani 1 1 d . . . C6 C 0.1468(2) 0.41588(18) 0.82799(18) 0.0306(5) Uani 1 1 d . . . H6A H 0.2219 0.4675 0.8931 0.037 Uiso 1 1 calc R . . H6B H 0.0820 0.4484 0.8182 0.037 Uiso 1 1 calc R . . C7 C -0.0037(2) 0.24507(19) 0.7692(2) 0.0351(5) Uani 1 1 d . . . H7A H -0.0285 0.2558 0.6965 0.042 Uiso 1 1 calc R . . H7B H -0.0560 0.2687 0.7959 0.042 Uiso 1 1 calc R . . C8 C -0.0195(2) 0.1261(2) 0.75399(19) 0.0335(5) Uani 1 1 d . . . C9 C -0.1068(2) 0.0635(2) 0.7644(2) 0.0428(6) Uani 1 1 d . . . H9 H -0.1558 0.0953 0.7856 0.051 Uiso 1 1 calc R . . C10 C -0.1206(2) -0.0465(2) 0.7432(2) 0.0474(7) Uani 1 1 d . . . H10 H -0.1767 -0.0906 0.7537 0.057 Uiso 1 1 calc R . . C11 C -0.0527(2) -0.0916(2) 0.7069(2) 0.0416(6) Uani 1 1 d . . . H11 H -0.0640 -0.1676 0.6889 0.050 Uiso 1 1 calc R . . C12 C 0.0328(2) -0.02470(18) 0.69680(19) 0.0322(5) Uani 1 1 d . . . C13 C 0.0993(2) -0.07208(18) 0.64755(19) 0.0320(5) Uani 1 1 d . . . C14 C 0.1240(2) -0.1689(2) 0.6592(2) 0.0429(6) Uani 1 1 d . . . H14 H 0.1029 -0.2022 0.7031 0.051 Uiso 1 1 calc R . . C15 C 0.1790(3) -0.2162(2) 0.6071(3) 0.0509(7) Uani 1 1 d . . . H15 H 0.1954 -0.2818 0.6154 0.061 Uiso 1 1 calc R . . C16 C 0.2102(2) -0.1687(2) 0.5432(2) 0.0502(7) Uani 1 1 d . . . H16 H 0.2479 -0.2016 0.5076 0.060 Uiso 1 1 calc R . . C17 C 0.1866(2) -0.0732(2) 0.5313(2) 0.0424(6) Uani 1 1 d . . . H17 H 0.2080 -0.0403 0.4874 0.051 Uiso 1 1 calc R . . C18 C 0.1315(2) -0.0252(2) 0.58332(18) 0.0335(5) Uani 1 1 d . . . H18 H 0.1158 0.0406 0.5748 0.040 Uiso 1 1 calc R . . C19 C 0.1474(2) 0.33438(19) 0.96442(19) 0.0324(5) Uani 1 1 d . . . H19A H 0.1104 0.2669 0.9713 0.039 Uiso 1 1 calc R . . H19B H 0.1115 0.3900 0.9823 0.039 Uiso 1 1 calc R . . C20 C 0.2791(2) 0.37312(18) 1.04684(18) 0.0285(5) Uani 1 1 d . . . C21 C 0.3197(2) 0.4327(2) 1.15700(19) 0.0370(6) Uani 1 1 d . . . H21 H 0.2656 0.4514 1.1792 0.044 Uiso 1 1 calc R . . C22 C 0.4401(2) 0.4637(2) 1.23292(19) 0.0394(6) Uani 1 1 d . . . H22 H 0.4701 0.5037 1.3086 0.047 Uiso 1 1 calc R . . C23 C 0.5165(2) 0.43627(19) 1.19788(18) 0.0342(5) Uani 1 1 d . . . H23 H 0.5995 0.4568 1.2494 0.041 Uiso 1 1 calc R . . C24 C 0.4712(2) 0.37819(17) 1.08643(18) 0.0268(5) Uani 1 1 d . . . C25 C 0.5527(2) 0.35343(17) 1.04667(18) 0.0280(5) Uani 1 1 d . . . C26 C 0.5366(2) 0.36312(17) 0.94630(18) 0.0285(5) Uani 1 1 d . . . H26 H 0.4716 0.3853 0.9017 0.034 Uiso 1 1 calc R . . C27 C 0.6152(2) 0.34059(18) 0.9110(2) 0.0357(5) Uani 1 1 d . . . H27 H 0.6028 0.3460 0.8418 0.043 Uiso 1 1 calc R . . C28 C 0.7109(2) 0.3104(2) 0.9764(2) 0.0424(6) Uani 1 1 d . . . H28 H 0.7646 0.2954 0.9522 0.051 Uiso 1 1 calc R . . C29 C 0.7288(2) 0.3020(2) 1.0768(2) 0.0440(6) Uani 1 1 d . . . H29 H 0.7954 0.2820 1.1221 0.053 Uiso 1 1 calc R . . C30 C 0.6503(2) 0.32245(19) 1.1116(2) 0.0372(6) Uani 1 1 d . . . H30 H 0.6625 0.3155 1.1803 0.045 Uiso 1 1 calc R . . C31 C 0.38427(18) 0.09934(17) 0.80141(18) 0.0265(5) Uani 1 1 d . . . C32 C 0.45328(19) 0.02111(17) 0.79138(17) 0.0270(5) Uani 1 1 d . . . C33 C 0.4696(2) -0.04710(18) 0.85523(19) 0.0314(5) Uani 1 1 d . . . H33 H 0.4393 -0.0416 0.9045 0.038 Uiso 1 1 calc R . . C34 C 0.5291(2) -0.1229(2) 0.8484(2) 0.0378(6) Uani 1 1 d . . . H34 H 0.5419 -0.1667 0.8947 0.045 Uiso 1 1 calc R . . C35 C 0.5696(2) -0.1345(2) 0.7745(2) 0.0419(6) Uani 1 1 d . . . H35 H 0.6080 -0.1879 0.7680 0.050 Uiso 1 1 calc R . . C36 C 0.5542(2) -0.0685(2) 0.7098(2) 0.0396(6) Uani 1 1 d . . . H36 H 0.5822 -0.0763 0.6588 0.048 Uiso 1 1 calc R . . C37 C 0.4978(2) 0.00910(19) 0.71944(18) 0.0312(5) Uani 1 1 d . . . C38 C 0.5747(2) 0.15188(19) 0.67300(19) 0.0325(5) Uani 1 1 d . . . C39 C 0.5386(2) 0.21914(18) 0.59974(19) 0.0313(5) Uani 1 1 d . . . C40 C 0.4197(2) 0.2042(2) 0.52692(19) 0.0342(5) Uani 1 1 d . . . H40 H 0.3590 0.1494 0.5219 0.041 Uiso 1 1 calc R . . C41 C 0.3899(2) 0.2698(2) 0.4613(2) 0.0394(6) Uani 1 1 d . . . H41 H 0.3085 0.2597 0.4109 0.047 Uiso 1 1 calc R . . C42 C 0.4778(3) 0.3493(2) 0.4689(2) 0.0444(6) Uani 1 1 d . . . H42 H 0.4567 0.3942 0.4240 0.053 Uiso 1 1 calc R . . C43 C 0.5962(3) 0.3646(2) 0.5410(2) 0.0479(7) Uani 1 1 d . . . H43 H 0.6564 0.4191 0.5451 0.058 Uiso 1 1 calc R . . C44 C 0.6273(2) 0.2999(2) 0.6078(2) 0.0400(6) Uani 1 1 d . . . H44 H 0.7087 0.3110 0.6587 0.048 Uiso 1 1 calc R . . C45 C 0.8347(3) 0.9735(3) 0.0054(3) 0.0709(10) Uani 1 1 d . . . C46 C 0.8182(5) 1.0748(3) 0.0165(4) 0.122(2) Uani 1 1 d . . . H46A H 0.8934 1.1296 0.0423 0.183 Uiso 1 1 calc R . . H46B H 0.7919 1.0916 0.0705 0.183 Uiso 1 1 calc R . . H46C H 0.7575 1.0749 -0.0555 0.183 Uiso 1 1 calc R . . O5 O 0.01056(18) 0.35544(18) 0.28295(18) 0.0564(5) Uani 1 1 d . A . O6 O 0.19907(17) 0.3717(2) 0.30509(18) 0.0579(6) Uani 1 1 d . A . O7 O 0.1101(4) 0.4928(5) 0.2460(9) 0.077(3) Uani 0.573(16) 1 d P A 1 O8 O 0.0269(5) 0.3159(8) 0.1298(4) 0.079(3) Uani 0.573(16) 1 d P A 1 O7' O 0.1213(6) 0.5228(6) 0.3300(13) 0.078(4) Uani 0.427(16) 1 d P A 2 O8' O 0.0556(10) 0.4115(17) 0.1546(9) 0.110(8) Uani 0.427(16) 1 d P A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.02484(9) 0.02627(9) 0.02655(10) 0.00531(6) 0.01063(7) 0.01090(6) Cl1 0.0285(3) 0.0900(6) 0.0599(4) 0.0539(4) 0.0232(3) 0.0247(3) O1 0.0328(9) 0.0268(8) 0.0324(9) 0.0102(7) 0.0127(7) 0.0144(7) O2 0.0338(9) 0.0333(9) 0.0317(9) 0.0095(7) 0.0158(7) 0.0149(7) O3 0.0348(9) 0.0435(10) 0.0331(9) 0.0205(7) 0.0157(8) 0.0187(8) O4 0.0355(10) 0.0474(11) 0.0409(10) 0.0138(8) 0.0097(9) 0.0176(8) N1 0.0315(10) 0.0308(10) 0.0236(9) 0.0069(8) 0.0108(8) 0.0136(8) N2 0.0274(10) 0.0292(10) 0.0257(9) 0.0051(8) 0.0112(8) 0.0113(8) N3 0.0243(10) 0.0316(10) 0.0277(10) 0.0048(8) 0.0104(8) 0.0077(8) N4 0.0297(10) 0.0228(9) 0.0226(9) 0.0087(7) 0.0114(8) 0.0095(7) N5 0.150(4) 0.053(2) 0.161(4) 0.003(2) -0.080(3) 0.039(3) C1 0.0388(14) 0.0347(13) 0.0275(12) 0.0065(10) 0.0151(11) 0.0158(10) C2 0.0447(15) 0.0469(15) 0.0244(12) 0.0104(10) 0.0159(11) 0.0172(12) C3 0.0452(15) 0.0467(15) 0.0234(12) 0.0139(11) 0.0088(11) 0.0201(12) C4 0.0386(14) 0.0400(13) 0.0268(12) 0.0093(10) 0.0089(11) 0.0223(11) C5 0.0296(12) 0.0294(11) 0.0237(11) 0.0052(9) 0.0088(9) 0.0126(9) C6 0.0363(13) 0.0285(11) 0.0256(11) 0.0068(9) 0.0127(10) 0.0181(10) C7 0.0245(12) 0.0389(13) 0.0341(13) 0.0041(10) 0.0109(10) 0.0137(10) C8 0.0211(11) 0.0393(13) 0.0287(12) 0.0022(10) 0.0080(10) 0.0080(9) C9 0.0267(13) 0.0508(16) 0.0397(14) 0.0005(12) 0.0161(11) 0.0067(11) C10 0.0357(14) 0.0466(16) 0.0473(16) 0.0025(12) 0.0225(13) -0.0043(12) C11 0.0366(14) 0.0340(13) 0.0427(15) 0.0033(11) 0.0185(12) 0.0012(11) C12 0.0262(12) 0.0310(12) 0.0277(12) 0.0025(9) 0.0093(10) 0.0038(9) C13 0.0244(11) 0.0280(11) 0.0288(12) -0.0005(9) 0.0077(10) 0.0037(9) C14 0.0418(15) 0.0312(13) 0.0434(15) 0.0045(11) 0.0166(12) 0.0074(11) C15 0.0452(16) 0.0335(14) 0.0538(18) -0.0022(12) 0.0155(14) 0.0147(12) C16 0.0350(14) 0.0522(17) 0.0396(15) -0.0104(13) 0.0113(12) 0.0139(12) C17 0.0285(13) 0.0553(16) 0.0257(12) -0.0011(11) 0.0086(10) 0.0060(11) C18 0.0240(11) 0.0365(13) 0.0238(11) 0.0002(9) 0.0050(9) 0.0050(9) C19 0.0333(13) 0.0345(12) 0.0308(12) 0.0067(10) 0.0189(11) 0.0116(10) C20 0.0361(12) 0.0274(11) 0.0246(11) 0.0113(9) 0.0160(10) 0.0105(9) C21 0.0477(15) 0.0399(13) 0.0285(12) 0.0116(10) 0.0243(12) 0.0105(11) C22 0.0518(16) 0.0393(14) 0.0207(11) 0.0087(10) 0.0161(11) 0.0078(12) C23 0.0373(13) 0.0340(12) 0.0220(11) 0.0116(9) 0.0079(10) 0.0070(10) C24 0.0306(12) 0.0221(10) 0.0240(11) 0.0119(8) 0.0092(9) 0.0076(9) C25 0.0272(11) 0.0199(10) 0.0277(11) 0.0073(8) 0.0076(9) 0.0053(8) C26 0.0285(12) 0.0223(10) 0.0272(11) 0.0067(9) 0.0093(9) 0.0066(9) C27 0.0372(13) 0.0281(12) 0.0370(13) 0.0045(10) 0.0193(11) 0.0057(10) C28 0.0352(14) 0.0335(13) 0.0506(16) 0.0017(11) 0.0208(12) 0.0110(11) C29 0.0324(14) 0.0363(14) 0.0478(16) 0.0079(11) 0.0090(12) 0.0157(11) C30 0.0335(13) 0.0340(13) 0.0339(13) 0.0123(10) 0.0082(11) 0.0113(10) C31 0.0189(10) 0.0218(10) 0.0250(11) 0.0008(8) 0.0038(9) 0.0044(8) C32 0.0253(11) 0.0237(10) 0.0227(11) 0.0039(8) 0.0061(9) 0.0087(8) C33 0.0339(12) 0.0295(12) 0.0277(12) 0.0095(9) 0.0125(10) 0.0120(10) C34 0.0427(14) 0.0326(13) 0.0370(13) 0.0170(10) 0.0142(12) 0.0197(11) C35 0.0492(16) 0.0371(14) 0.0395(14) 0.0117(11) 0.0181(12) 0.0278(12) C36 0.0465(15) 0.0479(15) 0.0317(13) 0.0141(11) 0.0205(12) 0.0284(12) C37 0.0323(12) 0.0343(12) 0.0244(11) 0.0117(9) 0.0098(10) 0.0154(10) C38 0.0345(13) 0.0355(12) 0.0290(12) 0.0076(10) 0.0164(11) 0.0174(10) C39 0.0369(13) 0.0329(12) 0.0292(12) 0.0088(9) 0.0192(10) 0.0172(10) C40 0.0383(13) 0.0371(13) 0.0311(12) 0.0128(10) 0.0183(11) 0.0170(11) C41 0.0468(15) 0.0401(14) 0.0310(13) 0.0123(11) 0.0170(12) 0.0204(12) C42 0.0676(19) 0.0361(14) 0.0365(14) 0.0155(11) 0.0280(14) 0.0230(13) C43 0.0603(19) 0.0408(15) 0.0512(17) 0.0167(13) 0.0350(15) 0.0137(13) C44 0.0396(14) 0.0413(14) 0.0399(14) 0.0098(11) 0.0217(12) 0.0142(11) C45 0.065(2) 0.0474(19) 0.063(2) 0.0116(16) 0.0036(17) 0.0215(16) C46 0.162(5) 0.051(2) 0.077(3) 0.003(2) 0.003(3) 0.047(3) O5 0.0430(11) 0.0741(14) 0.0696(14) 0.0358(12) 0.0361(11) 0.0214(10) O6 0.0362(11) 0.0953(16) 0.0654(14) 0.0510(13) 0.0281(10) 0.0362(11) O7 0.042(2) 0.054(3) 0.131(9) 0.050(4) 0.031(4) 0.015(2) O8 0.059(3) 0.124(6) 0.035(2) 0.005(3) 0.022(2) 0.015(3) O7' 0.042(3) 0.051(4) 0.129(10) 0.028(5) 0.036(4) 0.012(3) O8' 0.091(8) 0.25(2) 0.065(7) 0.106(12) 0.056(7) 0.117(13) _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 Cd1 O2 2.2439(16) . ? Cd1 N1 2.3328(19) . ? Cd1 N2 2.3762(18) . ? Cd1 O1 2.4062(16) . ? Cd1 N4 2.4172(17) . ? Cd1 N3 2.4592(18) . ? Cd1 C31 2.649(2) . ? Cl1 O7 1.298(4) . ? Cl1 O8' 1.312(6) . ? Cl1 O5 1.401(2) . ? Cl1 O6 1.4228(19) . ? Cl1 O8 1.542(5) . ? Cl1 O7' 1.687(11) . ? O1 C31 1.251(3) . ? O2 C31 1.259(3) . ? O3 C38 1.351(3) . ? O3 C37 1.404(3) . ? O4 C38 1.206(3) . ? N1 C5 1.342(3) . ? N1 C1 1.344(3) . ? N2 C19 1.472(3) . ? N2 C6 1.476(3) . ? N2 C7 1.477(3) . ? N3 C8 1.349(3) . ? N3 C12 1.354(3) . ? N4 C20 1.342(3) . ? N4 C24 1.356(3) . ? N5 C45 1.092(5) . ? C1 C2 1.383(3) . ? C1 H1 0.9500 . ? C2 C3 1.378(4) . ? C2 H2 0.9500 . ? C3 C4 1.381(4) . ? C3 H3 0.9500 . ? C4 C5 1.389(3) . ? C4 H4 0.9500 . ? C5 C6 1.503(3) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.508(3) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.387(4) . ? C9 C10 1.384(4) . ? C9 H9 0.9500 . ? C10 C11 1.378(4) . ? C10 H10 0.9500 . ? C11 C12 1.395(3) . ? C11 H11 0.9500 . ? C12 C13 1.488(3) . ? C13 C18 1.386(3) . ? C13 C14 1.400(4) . ? C14 C15 1.385(4) . ? C14 H14 0.9500 . ? C15 C16 1.379(5) . ? C15 H15 0.9500 . ? C16 C17 1.380(4) . ? C16 H16 0.9500 . ? C17 C18 1.388(3) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 C20 1.505(3) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 C21 1.396(3) . ? C21 C22 1.380(4) . ? C21 H21 0.9500 . ? C22 C23 1.379(4) . ? C22 H22 0.9500 . ? C23 C24 1.394(3) . ? C23 H23 0.9500 . ? C24 C25 1.476(3) . ? C25 C26 1.392(3) . ? C25 C30 1.398(3) . ? C26 C27 1.389(3) . ? C26 H26 0.9500 . ? C27 C28 1.378(4) . ? C27 H27 0.9500 . ? C28 C29 1.381(4) . ? C28 H28 0.9500 . ? C29 C30 1.378(4) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? C31 C32 1.515(3) . ? C32 C37 1.392(3) . ? C32 C33 1.394(3) . ? C33 C34 1.389(3) . ? C33 H33 0.9500 . ? C34 C35 1.376(4) . ? C34 H34 0.9500 . ? C35 C36 1.379(4) . ? C35 H35 0.9500 . ? C36 C37 1.385(3) . ? C36 H36 0.9500 . ? C38 C39 1.489(3) . ? C39 C40 1.386(3) . ? C39 C44 1.390(4) . ? C40 C41 1.389(3) . ? C40 H40 0.9500 . ? C41 C42 1.376(4) . ? C41 H41 0.9500 . ? C42 C43 1.377(4) . ? C42 H42 0.9500 . ? C43 C44 1.391(4) . ? C43 H43 0.9500 . ? C44 H44 0.9500 . ? C45 C46 1.381(5) . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Cd1 N1 140.59(6) . . ? O2 Cd1 N2 146.73(6) . . ? N1 Cd1 N2 72.65(7) . . ? O2 Cd1 O1 56.42(6) . . ? N1 Cd1 O1 84.18(6) . . ? N2 Cd1 O1 156.65(6) . . ? O2 Cd1 N4 95.08(6) . . ? N1 Cd1 N4 105.14(6) . . ? N2 Cd1 N4 70.54(6) . . ? O1 Cd1 N4 119.88(6) . . ? O2 Cd1 N3 94.16(6) . . ? N1 Cd1 N3 99.30(7) . . ? N2 Cd1 N3 73.96(6) . . ? O1 Cd1 N3 107.88(6) . . ? N4 Cd1 N3 127.72(6) . . ? O2 Cd1 C31 28.29(6) . . ? N1 Cd1 C31 112.31(7) . . ? N2 Cd1 C31 174.24(7) . . ? O1 Cd1 C31 28.13(6) . . ? N4 Cd1 C31 110.00(6) . . ? N3 Cd1 C31 101.90(6) . . ? O7 Cl1 O8' 59.3(6) . . ? O7 Cl1 O5 121.6(4) . . ? O8' Cl1 O5 123.3(5) . . ? O7 Cl1 O6 110.5(2) . . ? O8' Cl1 O6 120.8(3) . . ? O5 Cl1 O6 111.12(13) . . ? O7 Cl1 O8 107.3(4) . . ? O8' Cl1 O8 48.0(6) . . ? O5 Cl1 O8 100.0(3) . . ? O6 Cl1 O8 104.4(4) . . ? O7 Cl1 O7' 41.2(3) . . ? O8' Cl1 O7' 98.5(7) . . ? O5 Cl1 O7' 90.8(4) . . ? O6 Cl1 O7' 102.5(3) . . ? O8 Cl1 O7' 145.0(4) . . ? C31 O1 Cd1 86.80(13) . . ? C31 O2 Cd1 94.05(13) . . ? C38 O3 C37 117.64(18) . . ? C5 N1 C1 119.0(2) . . ? C5 N1 Cd1 115.83(15) . . ? C1 N1 Cd1 124.56(15) . . ? C19 N2 C6 110.66(17) . . ? C19 N2 C7 111.21(18) . . ? C6 N2 C7 111.03(18) . . ? C19 N2 Cd1 108.18(13) . . ? C6 N2 Cd1 106.69(13) . . ? C7 N2 Cd1 108.91(13) . . ? C8 N3 C12 118.6(2) . . ? C8 N3 Cd1 108.56(14) . . ? C12 N3 Cd1 124.13(15) . . ? C20 N4 C24 118.77(19) . . ? C20 N4 Cd1 113.58(14) . . ? C24 N4 Cd1 126.91(14) . . ? N1 C1 C2 122.4(2) . . ? N1 C1 H1 118.8 . . ? C2 C1 H1 118.8 . . ? C3 C2 C1 118.6(2) . . ? C3 C2 H2 120.7 . . ? C1 C2 H2 120.7 . . ? C2 C3 C4 119.4(2) . . ? C2 C3 H3 120.3 . . ? C4 C3 H3 120.3 . . ? C3 C4 C5 119.2(2) . . ? C3 C4 H4 120.4 . . ? C5 C4 H4 120.4 . . ? N1 C5 C4 121.4(2) . . ? N1 C5 C6 116.35(19) . . ? C4 C5 C6 122.2(2) . . ? N2 C6 C5 111.78(17) . . ? N2 C6 H6A 109.3 . . ? C5 C6 H6A 109.3 . . ? N2 C6 H6B 109.3 . . ? C5 C6 H6B 109.3 . . ? H6A C6 H6B 107.9 . . ? N2 C7 C8 112.10(19) . . ? N2 C7 H7A 109.2 . . ? C8 C7 H7A 109.2 . . ? N2 C7 H7B 109.2 . . ? C8 C7 H7B 109.2 . . ? H7A C7 H7B 107.9 . . ? N3 C8 C9 122.6(2) . . ? N3 C8 C7 115.8(2) . . ? C9 C8 C7 121.5(2) . . ? C10 C9 C8 118.4(2) . . ? C10 C9 H9 120.8 . . ? C8 C9 H9 120.8 . . ? C11 C10 C9 119.6(3) . . ? C11 C10 H10 120.2 . . ? C9 C10 H10 120.2 . . ? C10 C11 C12 119.4(2) . . ? C10 C11 H11 120.3 . . ? C12 C11 H11 120.3 . . ? N3 C12 C11 121.2(2) . . ? N3 C12 C13 118.0(2) . . ? C11 C12 C13 120.6(2) . . ? C18 C13 C14 118.6(2) . . ? C18 C13 C12 120.7(2) . . ? C14 C13 C12 120.6(2) . . ? C15 C14 C13 120.2(3) . . ? C15 C14 H14 119.9 . . ? C13 C14 H14 119.9 . . ? C16 C15 C14 120.6(3) . . ? C16 C15 H15 119.7 . . ? C14 C15 H15 119.7 . . ? C15 C16 C17 119.7(3) . . ? C15 C16 H16 120.1 . . ? C17 C16 H16 120.1 . . ? C16 C17 C18 120.1(3) . . ? C16 C17 H17 119.9 . . ? C18 C17 H17 119.9 . . ? C13 C18 C17 120.8(2) . . ? C13 C18 H18 119.6 . . ? C17 C18 H18 119.6 . . ? N2 C19 C20 112.55(18) . . ? N2 C19 H19A 109.1 . . ? C20 C19 H19A 109.1 . . ? N2 C19 H19B 109.1 . . ? C20 C19 H19B 109.1 . . ? H19A C19 H19B 107.8 . . ? N4 C20 C21 122.5(2) . . ? N4 C20 C19 118.44(19) . . ? C21 C20 C19 119.0(2) . . ? C22 C21 C20 118.5(2) . . ? C22 C21 H21 120.7 . . ? C20 C21 H21 120.7 . . ? C23 C22 C21 119.4(2) . . ? C23 C22 H22 120.3 . . ? C21 C22 H22 120.3 . . ? C22 C23 C24 119.7(2) . . ? C22 C23 H23 120.2 . . ? C24 C23 H23 120.2 . . ? N4 C24 C23 121.1(2) . . ? N4 C24 C25 118.65(19) . . ? C23 C24 C25 120.2(2) . . ? C26 C25 C30 118.6(2) . . ? C26 C25 C24 121.3(2) . . ? C30 C25 C24 120.1(2) . . ? C27 C26 C25 120.4(2) . . ? C27 C26 H26 119.8 . . ? C25 C26 H26 119.8 . . ? C28 C27 C26 120.1(2) . . ? C28 C27 H27 120.0 . . ? C26 C27 H27 120.0 . . ? C27 C28 C29 120.2(2) . . ? C27 C28 H28 119.9 . . ? C29 C28 H28 119.9 . . ? C30 C29 C28 120.1(2) . . ? C30 C29 H29 120.0 . . ? C28 C29 H29 120.0 . . ? C29 C30 C25 120.7(2) . . ? C29 C30 H30 119.7 . . ? C25 C30 H30 119.7 . . ? O1 C31 O2 122.7(2) . . ? O1 C31 C32 120.6(2) . . ? O2 C31 C32 116.7(2) . . ? O1 C31 Cd1 65.06(11) . . ? O2 C31 Cd1 57.65(11) . . ? C32 C31 Cd1 173.43(16) . . ? C37 C32 C33 117.2(2) . . ? C37 C32 C31 124.7(2) . . ? C33 C32 C31 118.0(2) . . ? C34 C33 C32 121.4(2) . . ? C34 C33 H33 119.3 . . ? C32 C33 H33 119.3 . . ? C35 C34 C33 119.9(2) . . ? C35 C34 H34 120.0 . . ? C33 C34 H34 120.0 . . ? C34 C35 C36 120.0(2) . . ? C34 C35 H35 120.0 . . ? C36 C35 H35 120.0 . . ? C35 C36 C37 119.8(2) . . ? C35 C36 H36 120.1 . . ? C37 C36 H36 120.1 . . ? C36 C37 C32 121.7(2) . . ? C36 C37 O3 117.9(2) . . ? C32 C37 O3 120.3(2) . . ? O4 C38 O3 123.9(2) . . ? O4 C38 C39 124.9(2) . . ? O3 C38 C39 111.2(2) . . ? C40 C39 C44 120.2(2) . . ? C40 C39 C38 121.4(2) . . ? C44 C39 C38 118.4(2) . . ? C39 C40 C41 119.5(2) . . ? C39 C40 H40 120.2 . . ? C41 C40 H40 120.2 . . ? C42 C41 C40 120.2(3) . . ? C42 C41 H41 119.9 . . ? C40 C41 H41 119.9 . . ? C41 C42 C43 120.6(2) . . ? C41 C42 H42 119.7 . . ? C43 C42 H42 119.7 . . ? C42 C43 C44 119.8(3) . . ? C42 C43 H43 120.1 . . ? C44 C43 H43 120.1 . . ? C39 C44 C43 119.7(3) . . ? C39 C44 H44 120.2 . . ? C43 C44 H44 120.2 . . ? N5 C45 C46 176.4(7) . . ? C45 C46 H46A 109.5 . . ? C45 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C45 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 Cd1 O1 C31 1.22(11) . . . . ? N1 Cd1 O1 C31 -179.65(13) . . . . ? N2 Cd1 O1 C31 -172.58(15) . . . . ? N4 Cd1 O1 C31 76.22(13) . . . . ? N3 Cd1 O1 C31 -81.73(13) . . . . ? N1 Cd1 O2 C31 -2.57(17) . . . . ? N2 Cd1 O2 C31 174.31(12) . . . . ? O1 Cd1 O2 C31 -1.21(11) . . . . ? N4 Cd1 O2 C31 -123.99(13) . . . . ? N3 Cd1 O2 C31 107.52(13) . . . . ? O2 Cd1 N1 C5 -171.89(14) . . . . ? N2 Cd1 N1 C5 9.90(15) . . . . ? O1 Cd1 N1 C5 -173.03(16) . . . . ? N4 Cd1 N1 C5 -53.60(17) . . . . ? N3 Cd1 N1 C5 79.76(16) . . . . ? C31 Cd1 N1 C5 -173.21(15) . . . . ? O2 Cd1 N1 C1 17.3(2) . . . . ? N2 Cd1 N1 C1 -161.0(2) . . . . ? O1 Cd1 N1 C1 16.12(18) . . . . ? N4 Cd1 N1 C1 135.54(18) . . . . ? N3 Cd1 N1 C1 -91.10(19) . . . . ? C31 Cd1 N1 C1 15.9(2) . . . . ? O2 Cd1 N2 C19 34.4(2) . . . . ? N1 Cd1 N2 C19 -147.63(15) . . . . ? O1 Cd1 N2 C19 -155.00(14) . . . . ? N4 Cd1 N2 C19 -34.01(13) . . . . ? N3 Cd1 N2 C19 106.95(15) . . . . ? C31 Cd1 N2 C19 62.4(7) . . . . ? O2 Cd1 N2 C6 153.53(13) . . . . ? N1 Cd1 N2 C6 -28.54(13) . . . . ? O1 Cd1 N2 C6 -35.9(2) . . . . ? N4 Cd1 N2 C6 85.07(13) . . . . ? N3 Cd1 N2 C6 -133.97(14) . . . . ? C31 Cd1 N2 C6 -178.5(6) . . . . ? O2 Cd1 N2 C7 -86.56(18) . . . . ? N1 Cd1 N2 C7 91.37(15) . . . . ? O1 Cd1 N2 C7 84.0(2) . . . . ? N4 Cd1 N2 C7 -155.02(16) . . . . ? N3 Cd1 N2 C7 -14.05(15) . . . . ? C31 Cd1 N2 C7 -58.6(7) . . . . ? O2 Cd1 N3 C8 135.80(16) . . . . ? N1 Cd1 N3 C8 -81.37(16) . . . . ? N2 Cd1 N3 C8 -12.56(15) . . . . ? O1 Cd1 N3 C8 -168.20(15) . . . . ? N4 Cd1 N3 C8 36.10(18) . . . . ? C31 Cd1 N3 C8 163.31(16) . . . . ? O2 Cd1 N3 C12 -11.10(18) . . . . ? N1 Cd1 N3 C12 131.73(18) . . . . ? N2 Cd1 N3 C12 -159.46(19) . . . . ? O1 Cd1 N3 C12 44.89(19) . . . . ? N4 Cd1 N3 C12 -110.80(18) . . . . ? C31 Cd1 N3 C12 16.41(19) . . . . ? O2 Cd1 N4 C20 -126.31(14) . . . . ? N1 Cd1 N4 C20 87.84(15) . . . . ? N2 Cd1 N4 C20 22.88(14) . . . . ? O1 Cd1 N4 C20 179.80(13) . . . . ? N3 Cd1 N4 C20 -27.06(17) . . . . ? C31 Cd1 N4 C20 -151.03(14) . . . . ? O2 Cd1 N4 C24 43.63(17) . . . . ? N1 Cd1 N4 C24 -102.22(17) . . . . ? N2 Cd1 N4 C24 -167.18(18) . . . . ? O1 Cd1 N4 C24 -10.26(19) . . . . ? N3 Cd1 N4 C24 142.89(16) . . . . ? C31 Cd1 N4 C24 18.91(18) . . . . ? C5 N1 C1 C2 -0.2(4) . . . . ? Cd1 N1 C1 C2 170.43(19) . . . . ? N1 C1 C2 C3 0.0(4) . . . . ? C1 C2 C3 C4 0.1(4) . . . . ? C2 C3 C4 C5 0.1(4) . . . . ? C1 N1 C5 C4 0.3(3) . . . . ? Cd1 N1 C5 C4 -171.06(18) . . . . ? C1 N1 C5 C6 -177.1(2) . . . . ? Cd1 N1 C5 C6 11.5(3) . . . . ? C3 C4 C5 N1 -0.3(4) . . . . ? C3 C4 C5 C6 176.9(2) . . . . ? C19 N2 C6 C5 161.96(19) . . . . ? C7 N2 C6 C5 -74.0(2) . . . . ? Cd1 N2 C6 C5 44.5(2) . . . . ? N1 C5 C6 N2 -39.4(3) . . . . ? C4 C5 C6 N2 143.3(2) . . . . ? C19 N2 C7 C8 -81.1(2) . . . . ? C6 N2 C7 C8 155.19(19) . . . . ? Cd1 N2 C7 C8 38.0(2) . . . . ? C12 N3 C8 C9 4.3(3) . . . . ? Cd1 N3 C8 C9 -144.7(2) . . . . ? C12 N3 C8 C7 -172.4(2) . . . . ? Cd1 N3 C8 C7 38.6(2) . . . . ? N2 C7 C8 N3 -54.9(3) . . . . ? N2 C7 C8 C9 128.4(2) . . . . ? N3 C8 C9 C10 -0.1(4) . . . . ? C7 C8 C9 C10 176.4(2) . . . . ? C8 C9 C10 C11 -3.5(4) . . . . ? C9 C10 C11 C12 2.8(4) . . . . ? C8 N3 C12 C11 -4.9(3) . . . . ? Cd1 N3 C12 C11 138.9(2) . . . . ? C8 N3 C12 C13 170.7(2) . . . . ? Cd1 N3 C12 C13 -45.5(3) . . . . ? C10 C11 C12 N3 1.4(4) . . . . ? C10 C11 C12 C13 -174.1(2) . . . . ? N3 C12 C13 C18 -30.8(3) . . . . ? C11 C12 C13 C18 144.9(2) . . . . ? N3 C12 C13 C14 153.3(2) . . . . ? C11 C12 C13 C14 -31.0(3) . . . . ? C18 C13 C14 C15 -0.2(4) . . . . ? C12 C13 C14 C15 175.8(2) . . . . ? C13 C14 C15 C16 0.0(4) . . . . ? C14 C15 C16 C17 0.1(4) . . . . ? C15 C16 C17 C18 0.0(4) . . . . ? C14 C13 C18 C17 0.3(3) . . . . ? C12 C13 C18 C17 -175.7(2) . . . . ? C16 C17 C18 C13 -0.1(4) . . . . ? C6 N2 C19 C20 -73.4(2) . . . . ? C7 N2 C19 C20 162.71(19) . . . . ? Cd1 N2 C19 C20 43.2(2) . . . . ? C24 N4 C20 C21 -0.1(3) . . . . ? Cd1 N4 C20 C21 170.74(18) . . . . ? C24 N4 C20 C19 -178.14(19) . . . . ? Cd1 N4 C20 C19 -7.3(2) . . . . ? N2 C19 C20 N4 -24.7(3) . . . . ? N2 C19 C20 C21 157.1(2) . . . . ? N4 C20 C21 C22 -0.8(4) . . . . ? C19 C20 C21 C22 177.2(2) . . . . ? C20 C21 C22 C23 0.7(4) . . . . ? C21 C22 C23 C24 0.4(4) . . . . ? C20 N4 C24 C23 1.2(3) . . . . ? Cd1 N4 C24 C23 -168.32(16) . . . . ? C20 N4 C24 C25 -176.87(19) . . . . ? Cd1 N4 C24 C25 13.7(3) . . . . ? C22 C23 C24 N4 -1.3(3) . . . . ? C22 C23 C24 C25 176.7(2) . . . . ? N4 C24 C25 C26 40.3(3) . . . . ? C23 C24 C25 C26 -137.7(2) . . . . ? N4 C24 C25 C30 -141.5(2) . . . . ? C23 C24 C25 C30 40.4(3) . . . . ? C30 C25 C26 C27 1.1(3) . . . . ? C24 C25 C26 C27 179.3(2) . . . . ? C25 C26 C27 C28 -1.2(3) . . . . ? C26 C27 C28 C29 0.3(4) . . . . ? C27 C28 C29 C30 0.8(4) . . . . ? C28 C29 C30 C25 -0.9(4) . . . . ? C26 C25 C30 C29 0.0(3) . . . . ? C24 C25 C30 C29 -178.2(2) . . . . ? Cd1 O1 C31 O2 -2.2(2) . . . . ? Cd1 O1 C31 C32 176.18(17) . . . . ? Cd1 O2 C31 O1 2.3(2) . . . . ? Cd1 O2 C31 C32 -176.08(15) . . . . ? O2 Cd1 C31 O1 -177.9(2) . . . . ? N1 Cd1 C31 O1 0.38(14) . . . . ? N2 Cd1 C31 O1 149.3(6) . . . . ? N4 Cd1 C31 O1 -116.35(12) . . . . ? N3 Cd1 C31 O1 105.74(12) . . . . ? N1 Cd1 C31 O2 178.23(12) . . . . ? N2 Cd1 C31 O2 -32.8(7) . . . . ? O1 Cd1 C31 O2 177.9(2) . . . . ? N4 Cd1 C31 O2 61.51(13) . . . . ? N3 Cd1 C31 O2 -76.40(13) . . . . ? O2 Cd1 C31 C32 32.2(13) . . . . ? N1 Cd1 C31 C32 -149.5(13) . . . . ? N2 Cd1 C31 C32 -0.6(17) . . . . ? O1 Cd1 C31 C32 -149.9(14) . . . . ? N4 Cd1 C31 C32 93.8(13) . . . . ? N3 Cd1 C31 C32 -44.2(13) . . . . ? O1 C31 C32 C37 0.2(3) . . . . ? O2 C31 C32 C37 178.6(2) . . . . ? Cd1 C31 C32 C37 148.3(12) . . . . ? O1 C31 C32 C33 -177.1(2) . . . . ? O2 C31 C32 C33 1.3(3) . . . . ? Cd1 C31 C32 C33 -29.0(14) . . . . ? C37 C32 C33 C34 0.8(3) . . . . ? C31 C32 C33 C34 178.3(2) . . . . ? C32 C33 C34 C35 -2.4(4) . . . . ? C33 C34 C35 C36 2.0(4) . . . . ? C34 C35 C36 C37 -0.1(4) . . . . ? C35 C36 C37 C32 -1.5(4) . . . . ? C35 C36 C37 O3 -177.5(2) . . . . ? C33 C32 C37 C36 1.1(3) . . . . ? C31 C32 C37 C36 -176.2(2) . . . . ? C33 C32 C37 O3 177.0(2) . . . . ? C31 C32 C37 O3 -0.3(3) . . . . ? C38 O3 C37 C36 -76.1(3) . . . . ? C38 O3 C37 C32 107.9(2) . . . . ? C37 O3 C38 O4 6.9(3) . . . . ? C37 O3 C38 C39 -172.83(18) . . . . ? O4 C38 C39 C40 -173.0(2) . . . . ? O3 C38 C39 C40 6.8(3) . . . . ? O4 C38 C39 C44 5.4(3) . . . . ? O3 C38 C39 C44 -174.8(2) . . . . ? C44 C39 C40 C41 0.6(3) . . . . ? C38 C39 C40 C41 179.0(2) . . . . ? C39 C40 C41 C42 -0.3(4) . . . . ? C40 C41 C42 C43 0.3(4) . . . . ? C41 C42 C43 C44 -0.8(4) . . . . ? C40 C39 C44 C43 -1.1(4) . . . . ? C38 C39 C44 C43 -179.5(2) . . . . ? C42 C43 C44 C39 1.2(4) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.907 _refine_diff_density_min -1.184 _refine_diff_density_rms 0.066 #===END