# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2006 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Qing-Yun Chen' _publ_contact_author_address ; Chinese Academy of Sciences Shanghai Institute of Organic Chemistry 354 Fenglin Lu Shanghai 200032 CHINA ; _publ_contact_author_email CHENQY@MAIL.SIOC.AC.CN _publ_section_title ; Unexpected bromination ring opening of tetraarylporphyrins ; loop_ _publ_author_name 'Qing-Yun Chen' 'Chao Liu' 'Dong-Mei Shen' # Attachment 'CCDC-286156.cif' data_cd24548 _database_code_depnum_ccdc_archive 'CCDC 286156' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C49 H34 Br9 N4 O3.50 Zn' _chemical_formula_weight 1519.36 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 28.0250(16) _cell_length_b 14.0764(8) _cell_length_c 26.7094(15) _cell_angle_alpha 90.00 _cell_angle_beta 102.3100(10) _cell_angle_gamma 90.00 _cell_volume 10294.4(10) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3753 _cell_measurement_theta_min 4.750 _cell_measurement_theta_max 46.330 _exptl_crystal_description ? _exptl_crystal_colour red _exptl_crystal_size_max 0.256 _exptl_crystal_size_mid 0.221 _exptl_crystal_size_min 0.203 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.961 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5832 _exptl_absorpt_coefficient_mu 7.510 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.75787 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26535 _diffrn_reflns_av_R_equivalents 0.1362 _diffrn_reflns_av_sigmaI/netI 0.1552 _diffrn_reflns_limit_h_min -33 _diffrn_reflns_limit_h_max 33 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 1.87 _diffrn_reflns_theta_max 25.50 _reflns_number_total 9547 _reflns_number_gt 4649 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0392P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9547 _refine_ls_number_parameters 590 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.1088 _refine_ls_R_factor_gt 0.0548 _refine_ls_wR_factor_ref 0.1287 _refine_ls_wR_factor_gt 0.1164 _refine_ls_goodness_of_fit_ref 0.831 _refine_ls_restrained_S_all 0.832 _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 Zn Zn 0.18691(3) 0.42338(6) 0.08696(3) 0.0366(2) Uani 1 1 d . . . Br1 Br 0.20916(3) 0.26405(6) 0.19936(4) 0.0629(3) Uani 1 1 d . . . Br2 Br 0.29893(4) 0.36438(8) 0.29844(4) 0.0901(4) Uani 1 1 d . . . Br3 Br 0.35037(3) 0.55911(7) 0.25113(3) 0.0650(3) Uani 1 1 d . . . Br4 Br 0.32377(4) 0.69343(7) 0.02275(4) 0.0829(4) Uani 1 1 d . . . Br5 Br 0.25515(4) 0.59146(7) -0.08627(4) 0.0752(3) Uani 1 1 d . . . Br6 Br 0.15608(4) 0.19872(7) -0.10624(4) 0.0775(3) Uani 1 1 d . . . Br7 Br 0.10793(4) 0.07090(7) -0.02147(4) 0.0739(3) Uani 1 1 d . . . Br8 Br 0.05061(3) 0.21747(7) 0.18427(4) 0.0622(3) Uani 1 1 d . . . Br9 Br 0.05687(3) 0.45220(7) 0.22677(4) 0.0669(3) Uani 1 1 d . . . O1 O 0.15711(17) 0.5722(3) 0.1127(2) 0.0440(13) Uani 1 1 d . . . O2 O 0.20869(18) 0.3910(4) -0.08221(19) 0.0489(14) Uani 1 1 d . . . O3 O 0.1343(2) 0.6073(4) 0.1903(2) 0.0595(16) Uani 1 1 d . . . O4 O 0.5000 0.469(2) 0.2500 0.202(18) Uiso 1 2 d SD . . N1 N 0.2436(2) 0.4159(4) 0.1485(2) 0.0376(15) Uani 1 1 d . . . N2 N 0.2310(2) 0.4812(4) 0.0460(2) 0.0370(15) Uani 1 1 d . . . N3 N 0.15868(19) 0.3325(4) 0.0297(2) 0.0364(15) Uani 1 1 d . . . N4 N 0.1250(2) 0.4029(4) 0.1105(2) 0.0387(15) Uani 1 1 d . . . C1 C 0.2473(3) 0.3692(5) 0.1918(3) 0.0417(19) Uani 1 1 d . . . C2 C 0.2829(3) 0.4091(6) 0.2313(3) 0.047(2) Uani 1 1 d . . . C3 C 0.3022(3) 0.4838(5) 0.2105(3) 0.0395(19) Uani 1 1 d . . . C4 C 0.2784(2) 0.4899(5) 0.1580(3) 0.0318(17) Uani 1 1 d . . . C5 C 0.2883(2) 0.5500(5) 0.1196(3) 0.0332(17) Uani 1 1 d . . . C6 C 0.2674(2) 0.5455(5) 0.0664(3) 0.0360(18) Uani 1 1 d . . . C7 C 0.2792(3) 0.5957(5) 0.0240(3) 0.043(2) Uani 1 1 d . . . C8 C 0.2528(3) 0.5544(5) -0.0196(3) 0.043(2) Uani 1 1 d . . . C9 C 0.2234(2) 0.4843(5) -0.0050(3) 0.0366(18) Uani 1 1 d . . . C10 C 0.1873(3) 0.4194(5) -0.0413(3) 0.0403(19) Uani 1 1 d . . . C11 C 0.1694(2) 0.3315(5) -0.0165(3) 0.0371(18) Uani 1 1 d . . . C12 C 0.1527(3) 0.2454(6) -0.0414(3) 0.046(2) Uani 1 1 d . . . C13 C 0.1324(3) 0.1936(5) -0.0075(3) 0.048(2) Uani 1 1 d . . . C14 C 0.1335(2) 0.2512(5) 0.0376(3) 0.0358(18) Uani 1 1 d . . . C15 C 0.1097(2) 0.2409(5) 0.0781(3) 0.0346(18) Uani 1 1 d . . . C16 C 0.1052(2) 0.3114(5) 0.1139(3) 0.0374(18) Uani 1 1 d . . . C17 C 0.0802(2) 0.3148(5) 0.1536(3) 0.0375(19) Uani 1 1 d . . . C18 C 0.0842(3) 0.4062(6) 0.1736(3) 0.0413(19) Uani 1 1 d . . . C19 C 0.1108(2) 0.4579(5) 0.1448(3) 0.0389(19) Uani 1 1 d . . . C20 C 0.1206(3) 0.5625(5) 0.1422(3) 0.044(2) Uani 1 1 d . . . C21 C 0.3291(3) 0.6194(5) 0.1346(3) 0.042(2) Uani 1 1 d . . . C22 C 0.3202(3) 0.7073(6) 0.1522(3) 0.056(2) Uani 1 1 d . . . H22 H 0.2884 0.7252 0.1530 0.067 Uiso 1 1 calc R . . C23 C 0.3586(4) 0.7700(6) 0.1690(4) 0.077(3) Uani 1 1 d . . . H23 H 0.3527 0.8299 0.1810 0.092 Uiso 1 1 calc R . . C24 C 0.4043(4) 0.7435(8) 0.1676(4) 0.083(3) Uani 1 1 d . . . H24 H 0.4300 0.7853 0.1791 0.099 Uiso 1 1 calc R . . C25 C 0.4137(3) 0.6555(7) 0.1496(4) 0.071(3) Uani 1 1 d . . . H25 H 0.4454 0.6395 0.1474 0.085 Uiso 1 1 calc R . . C26 C 0.3773(3) 0.5924(6) 0.1353(3) 0.053(2) Uani 1 1 d . . . H26 H 0.3841 0.5311 0.1259 0.064 Uiso 1 1 calc R . . C27 C 0.1417(3) 0.4772(6) -0.0644(3) 0.043(2) Uani 1 1 d . . . C28 C 0.1243(3) 0.5497(6) -0.0391(4) 0.066(3) Uani 1 1 d . . . H28 H 0.1426 0.5678 -0.0073 0.079 Uiso 1 1 calc R . . C29 C 0.0815(4) 0.5971(8) -0.0580(5) 0.093(4) Uani 1 1 d . . . H29 H 0.0712 0.6466 -0.0397 0.111 Uiso 1 1 calc R . . C30 C 0.0553(4) 0.5707(9) -0.1027(5) 0.089(4) Uani 1 1 d . . . H30 H 0.0261 0.6021 -0.1157 0.107 Uiso 1 1 calc R . . C31 C 0.0698(4) 0.4971(9) -0.1313(4) 0.084(3) Uani 1 1 d . . . H31 H 0.0503 0.4795 -0.1627 0.100 Uiso 1 1 calc R . . C32 C 0.1127(3) 0.4517(7) -0.1127(4) 0.069(3) Uani 1 1 d . . . H32 H 0.1231 0.4036 -0.1317 0.083 Uiso 1 1 calc R . . C33 C 0.0824(3) 0.1502(5) 0.0812(3) 0.0401(19) Uani 1 1 d . . . C34 C 0.1067(3) 0.0717(7) 0.1037(4) 0.070(3) Uani 1 1 d . . . H34 H 0.1402 0.0742 0.1171 0.084 Uiso 1 1 calc R . . C35 C 0.0807(5) -0.0126(7) 0.1064(4) 0.092(4) Uani 1 1 d . . . H35 H 0.0966 -0.0663 0.1220 0.110 Uiso 1 1 calc R . . C36 C 0.0318(5) -0.0146(9) 0.0858(5) 0.115(5) Uani 1 1 d . . . H36 H 0.0141 -0.0698 0.0877 0.138 Uiso 1 1 calc R . . C37 C 0.0087(4) 0.0641(10) 0.0623(4) 0.095(4) Uani 1 1 d . . . H37 H -0.0244 0.0615 0.0472 0.114 Uiso 1 1 calc R . . C38 C 0.0339(3) 0.1458(6) 0.0609(3) 0.059(2) Uani 1 1 d . . . H38 H 0.0177 0.1996 0.0458 0.070 Uiso 1 1 calc R . . C39 C 0.0726(3) 0.6102(6) 0.1149(4) 0.049(2) Uani 1 1 d . . . C40 C 0.0516(3) 0.5814(6) 0.0655(4) 0.070(3) Uani 1 1 d . . . H40 H 0.0674 0.5347 0.0505 0.084 Uiso 1 1 calc R . . C41 C 0.0091(4) 0.6176(8) 0.0378(5) 0.095(4) Uani 1 1 d . . . H41 H -0.0035 0.5988 0.0042 0.114 Uiso 1 1 calc R . . C42 C -0.0148(4) 0.6850(11) 0.0627(7) 0.114(5) Uani 1 1 d . . . H42 H -0.0444 0.7107 0.0454 0.137 Uiso 1 1 calc R . . C43 C 0.0045(5) 0.7131(9) 0.1114(6) 0.114(5) Uani 1 1 d . . . H43 H -0.0120 0.7576 0.1272 0.137 Uiso 1 1 calc R . . C44 C 0.0487(4) 0.6761(7) 0.1380(4) 0.083(3) Uani 1 1 d . . . H44 H 0.0619 0.6961 0.1713 0.100 Uiso 1 1 calc R . . C45 C 0.2531(3) 0.3429(6) -0.0674(3) 0.062(2) Uani 1 1 d . . . H45A H 0.2783 0.3872 -0.0528 0.092 Uiso 1 1 calc R . . H45B H 0.2613 0.3130 -0.0967 0.092 Uiso 1 1 calc R . . H45C H 0.2503 0.2955 -0.0423 0.092 Uiso 1 1 calc R . . C46 C 0.1772(3) 0.5669(7) 0.2232(4) 0.075(3) Uani 1 1 d . . . H46A H 0.1710 0.5017 0.2303 0.112 Uiso 1 1 calc R . . H46B H 0.1849 0.6019 0.2548 0.112 Uiso 1 1 calc R . . H46C H 0.2043 0.5703 0.2065 0.112 Uiso 1 1 calc R . . C47 C 0.1702(3) 0.6674(6) 0.1021(4) 0.073(3) Uani 1 1 d . . . H47A H 0.1421 0.6998 0.0828 0.109 Uiso 1 1 calc R . . H47B H 0.1953 0.6658 0.0826 0.109 Uiso 1 1 calc R . . H47C H 0.1821 0.7003 0.1338 0.109 Uiso 1 1 calc R . . C48 C 0.4635(4) 0.4015(19) 0.2388(17) 0.23(2) Uiso 1 1 d D . . C49 C 0.4487(11) 0.3055(19) 0.2309(14) 0.182(18) Uiso 1 1 d 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 Zn 0.0397(5) 0.0400(5) 0.0307(5) -0.0024(4) 0.0085(4) -0.0091(4) Br1 0.0683(6) 0.0617(6) 0.0550(6) 0.0204(5) 0.0047(5) -0.0219(5) Br2 0.1111(9) 0.1114(9) 0.0370(6) 0.0259(6) -0.0081(6) -0.0338(7) Br3 0.0746(6) 0.0693(7) 0.0448(5) -0.0067(5) -0.0014(5) -0.0205(5) Br4 0.0973(8) 0.0837(8) 0.0643(7) 0.0212(6) 0.0094(6) -0.0467(6) Br5 0.0947(7) 0.0892(8) 0.0404(6) 0.0232(5) 0.0115(5) -0.0233(6) Br6 0.1112(8) 0.0724(7) 0.0536(6) -0.0269(5) 0.0279(6) -0.0149(6) Br7 0.0942(7) 0.0503(6) 0.0798(7) -0.0271(5) 0.0240(6) -0.0269(5) Br8 0.0628(6) 0.0682(7) 0.0587(6) 0.0131(5) 0.0197(5) -0.0178(5) Br9 0.0740(6) 0.0813(7) 0.0548(6) 0.0018(5) 0.0348(5) 0.0110(5) O1 0.053(3) 0.026(3) 0.056(4) 0.003(3) 0.019(3) -0.004(2) O2 0.045(3) 0.067(4) 0.034(3) 0.003(3) 0.009(3) 0.008(3) O3 0.074(4) 0.057(4) 0.049(4) -0.012(3) 0.018(3) 0.000(3) N1 0.034(3) 0.048(4) 0.032(4) -0.002(3) 0.007(3) -0.008(3) N2 0.036(4) 0.044(4) 0.031(4) 0.006(3) 0.006(3) -0.003(3) N3 0.038(4) 0.035(4) 0.037(4) -0.001(3) 0.010(3) -0.001(3) N4 0.043(4) 0.034(4) 0.042(4) -0.007(3) 0.015(3) -0.012(3) C1 0.045(5) 0.048(5) 0.031(5) 0.005(4) 0.006(4) 0.001(4) C2 0.052(5) 0.051(6) 0.040(5) 0.014(4) 0.011(4) -0.001(4) C3 0.041(5) 0.037(5) 0.038(5) -0.004(4) 0.003(4) -0.005(4) C4 0.030(4) 0.033(4) 0.032(4) -0.005(3) 0.006(3) -0.003(3) C5 0.031(4) 0.030(4) 0.037(5) 0.002(3) 0.004(4) 0.001(3) C6 0.026(4) 0.046(5) 0.035(5) 0.002(4) 0.004(3) -0.007(4) C7 0.036(4) 0.049(5) 0.043(5) 0.010(4) 0.005(4) -0.007(4) C8 0.049(5) 0.043(5) 0.036(5) 0.015(4) 0.009(4) -0.007(4) C9 0.032(4) 0.044(5) 0.031(5) 0.006(4) 0.000(3) 0.004(4) C10 0.051(5) 0.045(5) 0.025(4) 0.004(4) 0.008(4) -0.006(4) C11 0.037(4) 0.043(5) 0.028(4) 0.003(4) -0.001(4) 0.007(4) C12 0.064(5) 0.038(5) 0.038(5) -0.007(4) 0.015(4) 0.007(4) C13 0.035(5) 0.046(5) 0.057(6) -0.016(4) -0.002(4) -0.014(4) C14 0.033(4) 0.030(4) 0.041(5) -0.002(4) 0.001(4) -0.006(3) C15 0.028(4) 0.031(4) 0.042(5) 0.004(4) 0.002(4) -0.010(3) C16 0.036(4) 0.041(5) 0.033(5) 0.000(4) 0.004(4) -0.008(4) C17 0.023(4) 0.047(5) 0.042(5) 0.008(4) 0.005(4) -0.006(3) C18 0.037(4) 0.051(5) 0.038(5) -0.001(4) 0.011(4) 0.005(4) C19 0.038(5) 0.042(5) 0.037(5) -0.006(4) 0.010(4) -0.007(4) C20 0.055(5) 0.038(5) 0.040(5) -0.006(4) 0.010(4) -0.001(4) C21 0.052(5) 0.033(5) 0.035(5) -0.001(4) 0.001(4) -0.008(4) C22 0.052(5) 0.043(6) 0.067(6) 0.006(5) 0.000(5) 0.007(4) C23 0.088(8) 0.036(6) 0.092(8) -0.003(5) -0.011(7) -0.012(6) C24 0.075(8) 0.082(9) 0.082(8) 0.006(6) -0.005(6) -0.045(7) C25 0.055(6) 0.079(8) 0.080(7) -0.018(6) 0.016(5) -0.027(6) C26 0.045(5) 0.061(6) 0.055(6) -0.015(4) 0.017(4) -0.017(5) C27 0.041(5) 0.042(5) 0.048(5) 0.012(4) 0.011(4) -0.001(4) C28 0.072(7) 0.064(7) 0.059(6) 0.004(5) 0.007(5) 0.007(5) C29 0.078(8) 0.099(9) 0.094(10) 0.021(7) 0.002(7) 0.044(7) C30 0.058(7) 0.092(9) 0.115(11) 0.064(8) 0.010(7) 0.030(6) C31 0.071(7) 0.105(9) 0.062(7) 0.039(7) -0.017(6) 0.014(7) C32 0.082(7) 0.069(7) 0.051(6) 0.009(5) 0.004(5) 0.002(6) C33 0.041(5) 0.036(5) 0.040(5) 0.002(4) 0.001(4) -0.007(4) C34 0.070(6) 0.069(7) 0.068(7) 0.001(6) 0.008(5) -0.024(6) C35 0.141(11) 0.054(7) 0.074(8) 0.009(6) 0.009(8) -0.030(7) C36 0.146(12) 0.088(10) 0.106(11) -0.017(8) 0.015(9) -0.099(9) C37 0.086(8) 0.123(11) 0.067(8) -0.005(7) -0.002(6) -0.056(8) C38 0.045(6) 0.059(6) 0.068(6) 0.000(5) 0.005(5) -0.029(5) C39 0.049(5) 0.037(5) 0.064(6) 0.000(4) 0.020(5) 0.003(4) C40 0.050(6) 0.067(7) 0.084(8) -0.002(6) -0.005(5) 0.014(5) C41 0.080(8) 0.101(9) 0.099(10) 0.006(8) 0.007(7) 0.024(7) C42 0.071(8) 0.132(13) 0.140(13) 0.078(11) 0.023(9) 0.013(8) C43 0.120(11) 0.102(10) 0.130(12) 0.019(9) 0.051(10) 0.072(9) C44 0.092(8) 0.067(7) 0.096(9) 0.003(6) 0.031(7) 0.026(6) C45 0.043(5) 0.072(6) 0.075(7) -0.002(5) 0.024(5) 0.009(5) C46 0.084(7) 0.086(8) 0.049(6) -0.017(5) 0.005(5) -0.002(6) C47 0.095(7) 0.039(6) 0.093(8) 0.003(5) 0.041(6) -0.010(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn N4 1.988(6) . ? Zn N2 1.990(6) . ? Zn N3 2.021(6) . ? Zn N1 2.031(6) . ? Zn O1 2.409(5) . ? Br1 C1 1.862(8) . ? Br2 C2 1.863(8) . ? Br3 C3 1.870(7) . ? Br4 C7 1.863(7) . ? Br5 C8 1.870(7) . ? Br6 C12 1.872(8) . ? Br7 C13 1.866(7) . ? Br8 C17 1.876(7) . ? Br9 C18 1.867(7) . ? O1 C20 1.426(9) . ? O1 C47 1.434(8) . ? O2 C45 1.399(8) . ? O2 C10 1.411(8) . ? O3 C20 1.409(9) . ? O3 C46 1.446(9) . ? O4 C48 1.380(18) . ? O4 C48 1.380(18) 2_655 ? N1 C1 1.316(8) . ? N1 C4 1.412(8) . ? N2 C9 1.334(9) . ? N2 C6 1.386(8) . ? N3 C11 1.329(8) . ? N3 C14 1.384(8) . ? N4 C19 1.325(9) . ? N4 C16 1.413(8) . ? C1 C2 1.404(10) . ? C2 C3 1.357(10) . ? C3 C4 1.421(9) . ? C4 C5 1.402(9) . ? C5 C6 1.419(9) . ? C5 C21 1.494(9) . ? C6 C7 1.431(10) . ? C7 C8 1.370(10) . ? C8 C9 1.394(9) . ? C9 C10 1.543(10) . ? C10 C27 1.530(10) . ? C10 C11 1.538(10) . ? C11 C12 1.413(10) . ? C12 C13 1.379(10) . ? C13 C14 1.446(10) . ? C14 C15 1.395(10) . ? C15 C16 1.401(10) . ? C15 C33 1.501(9) . ? C16 C17 1.392(10) . ? C17 C18 1.389(10) . ? C18 C19 1.386(10) . ? C19 C20 1.502(10) . ? C20 C39 1.541(10) . ? C21 C22 1.365(10) . ? C21 C26 1.399(10) . ? C22 C23 1.390(11) . ? C22 H22 0.9300 . ? C23 C24 1.341(13) . ? C23 H23 0.9300 . ? C24 C25 1.375(13) . ? C24 H24 0.9300 . ? C25 C26 1.344(10) . ? C25 H25 0.9300 . ? C26 H26 0.9300 . ? C27 C28 1.370(11) . ? C27 C32 1.416(11) . ? C28 C29 1.371(12) . ? C28 H28 0.9300 . ? C29 C30 1.314(15) . ? C29 H29 0.9300 . ? C30 C31 1.398(15) . ? C30 H30 0.9300 . ? C31 C32 1.359(12) . ? C31 H31 0.9300 . ? C32 H32 0.9300 . ? C33 C38 1.352(9) . ? C33 C34 1.369(11) . ? C34 C35 1.402(12) . ? C34 H34 0.9300 . ? C35 C36 1.365(15) . ? C35 H35 0.9300 . ? C36 C37 1.365(15) . ? C36 H36 0.9300 . ? C37 C38 1.355(12) . ? C37 H37 0.9300 . ? C38 H38 0.9300 . ? C39 C44 1.366(11) . ? C39 C40 1.384(12) . ? C40 C41 1.360(12) . ? C40 H40 0.9300 . ? C41 C42 1.407(17) . ? C41 H41 0.9300 . ? C42 C43 1.358(17) . ? C42 H42 0.9300 . ? C43 C44 1.391(15) . ? C43 H43 0.9300 . ? C44 H44 0.9300 . ? C45 H45A 0.9600 . ? C45 H45B 0.9600 . ? C45 H45C 0.9600 . ? C46 H46A 0.9600 . ? C46 H46B 0.9600 . ? C46 H46C 0.9600 . ? C47 H47A 0.9600 . ? C47 H47B 0.9600 . ? C47 H47C 0.9600 . ? C48 C49 1.416(18) . ? 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 N4 Zn N2 156.8(2) . . ? N4 Zn N3 85.5(2) . . ? N2 Zn N3 91.8(2) . . ? N4 Zn N1 108.7(2) . . ? N2 Zn N1 89.7(2) . . ? N3 Zn N1 133.8(2) . . ? N4 Zn O1 70.0(2) . . ? N2 Zn O1 95.4(2) . . ? N3 Zn O1 131.49(19) . . ? N1 Zn O1 94.2(2) . . ? C20 O1 C47 116.3(6) . . ? C20 O1 Zn 114.1(4) . . ? C47 O1 Zn 129.6(5) . . ? C45 O2 C10 114.7(6) . . ? C20 O3 C46 114.2(6) . . ? C48 O4 C48 93.2(19) . 2_655 ? C1 N1 C4 106.8(6) . . ? C1 N1 Zn 129.7(5) . . ? C4 N1 Zn 119.9(5) . . ? C9 N2 C6 108.9(6) . . ? C9 N2 Zn 126.2(5) . . ? C6 N2 Zn 122.9(5) . . ? C11 N3 C14 110.8(6) . . ? C11 N3 Zn 125.4(5) . . ? C14 N3 Zn 122.5(5) . . ? C19 N4 C16 108.0(6) . . ? C19 N4 Zn 123.1(5) . . ? C16 N4 Zn 122.3(5) . . ? N1 C1 C2 111.8(7) . . ? N1 C1 Br1 123.6(6) . . ? C2 C1 Br1 124.6(6) . . ? C3 C2 C1 106.5(7) . . ? C3 C2 Br2 128.4(6) . . ? C1 C2 Br2 125.1(6) . . ? C2 C3 C4 107.8(6) . . ? C2 C3 Br3 120.2(6) . . ? C4 C3 Br3 131.9(6) . . ? C5 C4 N1 123.4(6) . . ? C5 C4 C3 129.2(6) . . ? N1 C4 C3 107.1(6) . . ? C4 C5 C6 127.1(6) . . ? C4 C5 C21 117.3(6) . . ? C6 C5 C21 115.2(6) . . ? N2 C6 C5 122.2(6) . . ? N2 C6 C7 106.7(6) . . ? C5 C6 C7 130.9(7) . . ? C8 C7 C6 106.8(6) . . ? C8 C7 Br4 122.8(6) . . ? C6 C7 Br4 130.4(6) . . ? C7 C8 C9 107.9(7) . . ? C7 C8 Br5 124.7(6) . . ? C9 C8 Br5 127.4(6) . . ? N2 C9 C8 109.5(6) . . ? N2 C9 C10 124.3(7) . . ? C8 C9 C10 126.2(7) . . ? O2 C10 C27 107.2(6) . . ? O2 C10 C11 109.8(6) . . ? C27 C10 C11 106.3(6) . . ? O2 C10 C9 109.0(6) . . ? C27 C10 C9 108.5(6) . . ? C11 C10 C9 115.8(6) . . ? N3 C11 C12 109.3(7) . . ? N3 C11 C10 123.4(6) . . ? C12 C11 C10 126.2(7) . . ? C13 C12 C11 106.5(7) . . ? C13 C12 Br6 122.1(6) . . ? C11 C12 Br6 131.4(6) . . ? C12 C13 C14 108.2(7) . . ? C12 C13 Br7 122.9(6) . . ? C14 C13 Br7 128.9(6) . . ? N3 C14 C15 123.3(7) . . ? N3 C14 C13 104.9(6) . . ? C15 C14 C13 131.2(7) . . ? C14 C15 C16 125.6(6) . . ? C14 C15 C33 117.7(7) . . ? C16 C15 C33 116.4(6) . . ? C17 C16 C15 132.6(7) . . ? C17 C16 N4 106.6(6) . . ? C15 C16 N4 120.5(6) . . ? C18 C17 C16 108.2(6) . . ? C18 C17 Br8 121.1(6) . . ? C16 C17 Br8 130.4(6) . . ? C19 C18 C17 106.4(7) . . ? C19 C18 Br9 126.6(6) . . ? C17 C18 Br9 126.9(6) . . ? N4 C19 C18 110.7(7) . . ? N4 C19 C20 117.2(7) . . ? C18 C19 C20 131.7(7) . . ? O3 C20 O1 111.8(6) . . ? O3 C20 C19 114.5(7) . . ? O1 C20 C19 106.2(6) . . ? O3 C20 C39 106.2(6) . . ? O1 C20 C39 110.7(6) . . ? C19 C20 C39 107.4(6) . . ? C22 C21 C26 119.2(7) . . ? C22 C21 C5 119.9(7) . . ? C26 C21 C5 120.6(7) . . ? C21 C22 C23 120.1(8) . . ? C21 C22 H22 120.0 . . ? C23 C22 H22 120.0 . . ? C24 C23 C22 119.5(9) . . ? C24 C23 H23 120.3 . . ? C22 C23 H23 120.3 . . ? C23 C24 C25 121.0(9) . . ? C23 C24 H24 119.5 . . ? C25 C24 H24 119.5 . . ? C26 C25 C24 120.3(9) . . ? C26 C25 H25 119.8 . . ? C24 C25 H25 119.8 . . ? C25 C26 C21 119.7(8) . . ? C25 C26 H26 120.1 . . ? C21 C26 H26 120.1 . . ? C28 C27 C32 116.3(8) . . ? C28 C27 C10 123.5(8) . . ? C32 C27 C10 119.9(8) . . ? C27 C28 C29 123.8(10) . . ? C27 C28 H28 118.1 . . ? C29 C28 H28 118.1 . . ? C30 C29 C28 118.0(11) . . ? C30 C29 H29 121.0 . . ? C28 C29 H29 121.0 . . ? C29 C30 C31 122.5(10) . . ? C29 C30 H30 118.8 . . ? C31 C30 H30 118.8 . . ? C32 C31 C30 119.0(10) . . ? C32 C31 H31 120.5 . . ? C30 C31 H31 120.5 . . ? C31 C32 C27 120.3(10) . . ? C31 C32 H32 119.8 . . ? C27 C32 H32 119.8 . . ? C38 C33 C34 120.2(8) . . ? C38 C33 C15 119.9(7) . . ? C34 C33 C15 119.8(7) . . ? C33 C34 C35 119.3(9) . . ? C33 C34 H34 120.4 . . ? C35 C34 H34 120.4 . . ? C36 C35 C34 119.1(10) . . ? C36 C35 H35 120.5 . . ? C34 C35 H35 120.5 . . ? C35 C36 C37 120.4(10) . . ? C35 C36 H36 119.8 . . ? C37 C36 H36 119.8 . . ? C38 C37 C36 120.1(10) . . ? C38 C37 H37 120.0 . . ? C36 C37 H37 120.0 . . ? C33 C38 C37 120.9(9) . . ? C33 C38 H38 119.6 . . ? C37 C38 H38 119.6 . . ? C44 C39 C40 118.7(9) . . ? C44 C39 C20 122.9(9) . . ? C40 C39 C20 118.3(8) . . ? C41 C40 C39 123.6(10) . . ? C41 C40 H40 118.2 . . ? C39 C40 H40 118.2 . . ? C40 C41 C42 116.5(11) . . ? C40 C41 H41 121.7 . . ? C42 C41 H41 121.7 . . ? C43 C42 C41 121.0(12) . . ? C43 C42 H42 119.5 . . ? C41 C42 H42 119.5 . . ? C42 C43 C44 120.7(12) . . ? C42 C43 H43 119.7 . . ? C44 C43 H43 119.7 . . ? C39 C44 C43 119.4(11) . . ? C39 C44 H44 120.3 . . ? C43 C44 H44 120.3 . . ? O2 C45 H45A 109.5 . . ? O2 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? O2 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? O3 C46 H46A 109.5 . . ? O3 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? O3 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? O1 C47 H47A 109.5 . . ? O1 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? O1 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? O4 C48 C49 150(2) . . ? O4 C48 C48 43.4(10) . 2_655 ? C49 C48 C48 107.1(14) . 2_655 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N4 Zn O1 C20 15.4(5) . . . . ? N2 Zn O1 C20 176.9(5) . . . . ? N3 Zn O1 C20 79.6(5) . . . . ? N1 Zn O1 C20 -93.0(5) . . . . ? N4 Zn O1 C47 -163.7(7) . . . . ? N2 Zn O1 C47 -2.2(6) . . . . ? N3 Zn O1 C47 -99.5(6) . . . . ? N1 Zn O1 C47 87.9(6) . . . . ? N4 Zn N1 C1 27.5(7) . . . . ? N2 Zn N1 C1 -166.8(7) . . . . ? N3 Zn N1 C1 -74.6(7) . . . . ? O1 Zn N1 C1 97.7(7) . . . . ? N4 Zn N1 C4 -128.0(5) . . . . ? N2 Zn N1 C4 37.7(5) . . . . ? N3 Zn N1 C4 129.9(5) . . . . ? O1 Zn N1 C4 -57.7(5) . . . . ? N4 Zn N2 C9 -56.3(10) . . . . ? N3 Zn N2 C9 26.3(6) . . . . ? N1 Zn N2 C9 160.2(6) . . . . ? O1 Zn N2 C9 -105.6(6) . . . . ? N4 Zn N2 C6 105.8(7) . . . . ? N3 Zn N2 C6 -171.5(5) . . . . ? N1 Zn N2 C6 -37.7(5) . . . . ? O1 Zn N2 C6 56.5(5) . . . . ? N4 Zn N3 C11 152.8(6) . . . . ? N2 Zn N3 C11 -4.1(6) . . . . ? N1 Zn N3 C11 -95.5(6) . . . . ? O1 Zn N3 C11 94.8(6) . . . . ? N4 Zn N3 C14 -41.1(5) . . . . ? N2 Zn N3 C14 162.0(5) . . . . ? N1 Zn N3 C14 70.6(6) . . . . ? O1 Zn N3 C14 -99.1(5) . . . . ? N2 Zn N4 C19 -81.7(9) . . . . ? N3 Zn N4 C19 -165.7(6) . . . . ? N1 Zn N4 C19 59.4(6) . . . . ? O1 Zn N4 C19 -28.3(6) . . . . ? N2 Zn N4 C16 130.2(6) . . . . ? N3 Zn N4 C16 46.3(5) . . . . ? N1 Zn N4 C16 -88.7(6) . . . . ? O1 Zn N4 C16 -176.3(6) . . . . ? C4 N1 C1 C2 0.9(9) . . . . ? Zn N1 C1 C2 -157.0(5) . . . . ? C4 N1 C1 Br1 -179.7(5) . . . . ? Zn N1 C1 Br1 22.4(10) . . . . ? N1 C1 C2 C3 -0.7(9) . . . . ? Br1 C1 C2 C3 180.0(6) . . . . ? N1 C1 C2 Br2 179.7(5) . . . . ? Br1 C1 C2 Br2 0.3(10) . . . . ? C1 C2 C3 C4 0.1(9) . . . . ? Br2 C2 C3 C4 179.8(6) . . . . ? C1 C2 C3 Br3 178.4(5) . . . . ? Br2 C2 C3 Br3 -2.0(10) . . . . ? C1 N1 C4 C5 174.2(7) . . . . ? Zn N1 C4 C5 -25.3(9) . . . . ? C1 N1 C4 C3 -0.8(8) . . . . ? Zn N1 C4 C3 159.7(5) . . . . ? C2 C3 C4 C5 -174.2(7) . . . . ? Br3 C3 C4 C5 7.8(12) . . . . ? C2 C3 C4 N1 0.4(8) . . . . ? Br3 C3 C4 N1 -177.6(5) . . . . ? N1 C4 C5 C6 -2.4(11) . . . . ? C3 C4 C5 C6 171.5(7) . . . . ? N1 C4 C5 C21 -174.6(6) . . . . ? C3 C4 C5 C21 -0.8(11) . . . . ? C9 N2 C6 C5 -171.6(6) . . . . ? Zn N2 C6 C5 23.5(9) . . . . ? C9 N2 C6 C7 4.9(8) . . . . ? Zn N2 C6 C7 -159.9(5) . . . . ? C4 C5 C6 N2 4.1(11) . . . . ? C21 C5 C6 N2 176.4(6) . . . . ? C4 C5 C6 C7 -171.5(8) . . . . ? C21 C5 C6 C7 0.8(12) . . . . ? N2 C6 C7 C8 -5.0(8) . . . . ? C5 C6 C7 C8 171.2(7) . . . . ? N2 C6 C7 Br4 178.7(5) . . . . ? C5 C6 C7 Br4 -5.2(13) . . . . ? C6 C7 C8 C9 3.2(9) . . . . ? Br4 C7 C8 C9 179.9(5) . . . . ? C6 C7 C8 Br5 -179.0(5) . . . . ? Br4 C7 C8 Br5 -2.3(10) . . . . ? C6 N2 C9 C8 -3.1(8) . . . . ? Zn N2 C9 C8 161.2(5) . . . . ? C6 N2 C9 C10 176.9(6) . . . . ? Zn N2 C9 C10 -18.9(10) . . . . ? C7 C8 C9 N2 -0.2(9) . . . . ? Br5 C8 C9 N2 -177.9(5) . . . . ? C7 C8 C9 C10 179.9(7) . . . . ? Br5 C8 C9 C10 2.2(11) . . . . ? C45 O2 C10 C27 175.5(6) . . . . ? C45 O2 C10 C11 -69.4(7) . . . . ? C45 O2 C10 C9 58.3(8) . . . . ? N2 C9 C10 O2 -139.7(7) . . . . ? C8 C9 C10 O2 40.2(10) . . . . ? N2 C9 C10 C27 103.9(8) . . . . ? C8 C9 C10 C27 -76.1(9) . . . . ? N2 C9 C10 C11 -15.4(10) . . . . ? C8 C9 C10 C11 164.5(7) . . . . ? C14 N3 C11 C12 -2.0(8) . . . . ? Zn N3 C11 C12 165.5(5) . . . . ? C14 N3 C11 C10 166.6(6) . . . . ? Zn N3 C11 C10 -25.9(9) . . . . ? O2 C10 C11 N3 163.1(6) . . . . ? C27 C10 C11 N3 -81.3(8) . . . . ? C9 C10 C11 N3 39.3(9) . . . . ? O2 C10 C11 C12 -30.3(9) . . . . ? C27 C10 C11 C12 85.3(9) . . . . ? C9 C10 C11 C12 -154.1(7) . . . . ? N3 C11 C12 C13 -1.3(8) . . . . ? C10 C11 C12 C13 -169.5(7) . . . . ? N3 C11 C12 Br6 -179.8(6) . . . . ? C10 C11 C12 Br6 12.0(12) . . . . ? C11 C12 C13 C14 3.9(8) . . . . ? Br6 C12 C13 C14 -177.4(5) . . . . ? C11 C12 C13 Br7 -176.7(5) . . . . ? Br6 C12 C13 Br7 2.0(10) . . . . ? C11 N3 C14 C15 -167.6(6) . . . . ? Zn N3 C14 C15 24.4(9) . . . . ? C11 N3 C14 C13 4.3(7) . . . . ? Zn N3 C14 C13 -163.6(5) . . . . ? C12 C13 C14 N3 -5.0(8) . . . . ? Br7 C13 C14 N3 175.6(5) . . . . ? C12 C13 C14 C15 166.0(7) . . . . ? Br7 C13 C14 C15 -13.4(12) . . . . ? N3 C14 C15 C16 4.5(11) . . . . ? C13 C14 C15 C16 -165.1(7) . . . . ? N3 C14 C15 C33 178.0(6) . . . . ? C13 C14 C15 C33 8.4(11) . . . . ? C14 C15 C16 C17 174.7(7) . . . . ? C33 C15 C16 C17 1.1(12) . . . . ? C14 C15 C16 N4 0.6(11) . . . . ? C33 C15 C16 N4 -173.0(6) . . . . ? C19 N4 C16 C17 -2.6(8) . . . . ? Zn N4 C16 C17 149.6(5) . . . . ? C19 N4 C16 C15 172.8(6) . . . . ? Zn N4 C16 C15 -34.9(9) . . . . ? C15 C16 C17 C18 -174.0(7) . . . . ? N4 C16 C17 C18 0.7(8) . . . . ? C15 C16 C17 Br8 12.6(12) . . . . ? N4 C16 C17 Br8 -172.7(5) . . . . ? C16 C17 C18 C19 1.4(8) . . . . ? Br8 C17 C18 C19 175.5(5) . . . . ? C16 C17 C18 Br9 178.8(5) . . . . ? Br8 C17 C18 Br9 -7.1(9) . . . . ? C16 N4 C19 C18 3.6(8) . . . . ? Zn N4 C19 C18 -148.4(5) . . . . ? C16 N4 C19 C20 -170.0(6) . . . . ? Zn N4 C19 C20 38.0(9) . . . . ? C17 C18 C19 N4 -3.2(8) . . . . ? Br9 C18 C19 N4 179.5(5) . . . . ? C17 C18 C19 C20 169.3(7) . . . . ? Br9 C18 C19 C20 -8.1(12) . . . . ? C46 O3 C20 O1 -63.4(8) . . . . ? C46 O3 C20 C19 57.5(9) . . . . ? C46 O3 C20 C39 175.8(6) . . . . ? C47 O1 C20 O3 -58.4(8) . . . . ? Zn O1 C20 O3 122.3(5) . . . . ? C47 O1 C20 C19 176.0(6) . . . . ? Zn O1 C20 C19 -3.2(7) . . . . ? C47 O1 C20 C39 59.8(8) . . . . ? Zn O1 C20 C39 -119.5(5) . . . . ? N4 C19 C20 O3 -142.0(7) . . . . ? C18 C19 C20 O3 46.0(11) . . . . ? N4 C19 C20 O1 -18.1(9) . . . . ? C18 C19 C20 O1 169.9(7) . . . . ? N4 C19 C20 C39 100.4(8) . . . . ? C18 C19 C20 C39 -71.6(10) . . . . ? C4 C5 C21 C22 -89.0(9) . . . . ? C6 C5 C21 C22 97.8(9) . . . . ? C4 C5 C21 C26 85.0(9) . . . . ? C6 C5 C21 C26 -88.1(9) . . . . ? C26 C21 C22 C23 2.1(12) . . . . ? C5 C21 C22 C23 176.3(8) . . . . ? C21 C22 C23 C24 0.1(15) . . . . ? C22 C23 C24 C25 0.4(16) . . . . ? C23 C24 C25 C26 -3.2(16) . . . . ? C24 C25 C26 C21 5.4(14) . . . . ? C22 C21 C26 C25 -4.9(13) . . . . ? C5 C21 C26 C25 -179.0(8) . . . . ? O2 C10 C27 C28 -149.2(7) . . . . ? C11 C10 C27 C28 93.4(9) . . . . ? C9 C10 C27 C28 -31.7(10) . . . . ? O2 C10 C27 C32 36.2(9) . . . . ? C11 C10 C27 C32 -81.2(9) . . . . ? C9 C10 C27 C32 153.7(7) . . . . ? C32 C27 C28 C29 -0.1(13) . . . . ? C10 C27 C28 C29 -174.9(8) . . . . ? C27 C28 C29 C30 0.9(16) . . . . ? C28 C29 C30 C31 -0.4(17) . . . . ? C29 C30 C31 C32 -0.7(17) . . . . ? C30 C31 C32 C27 1.5(14) . . . . ? C28 C27 C32 C31 -1.1(12) . . . . ? C10 C27 C32 C31 173.9(8) . . . . ? C14 C15 C33 C38 -95.0(9) . . . . ? C16 C15 C33 C38 79.1(9) . . . . ? C14 C15 C33 C34 83.9(9) . . . . ? C16 C15 C33 C34 -102.0(9) . . . . ? C38 C33 C34 C35 -1.2(14) . . . . ? C15 C33 C34 C35 179.9(8) . . . . ? C33 C34 C35 C36 0.9(16) . . . . ? C34 C35 C36 C37 0.8(19) . . . . ? C35 C36 C37 C38 -2(2) . . . . ? C34 C33 C38 C37 -0.3(13) . . . . ? C15 C33 C38 C37 178.6(9) . . . . ? C36 C37 C38 C33 2.1(17) . . . . ? O3 C20 C39 C44 -5.3(11) . . . . ? O1 C20 C39 C44 -126.9(8) . . . . ? C19 C20 C39 C44 117.6(9) . . . . ? O3 C20 C39 C40 177.9(7) . . . . ? O1 C20 C39 C40 56.3(9) . . . . ? C19 C20 C39 C40 -59.2(10) . . . . ? C44 C39 C40 C41 2.5(15) . . . . ? C20 C39 C40 C41 179.4(9) . . . . ? C39 C40 C41 C42 -2.7(16) . . . . ? C40 C41 C42 C43 1.4(18) . . . . ? C41 C42 C43 C44 0(2) . . . . ? C40 C39 C44 C43 -0.7(14) . . . . ? C20 C39 C44 C43 -177.4(9) . . . . ? C42 C43 C44 C39 -0.6(19) . . . . ? C48 O4 C48 C49 -7(7) 2_655 . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.854 _refine_diff_density_min -0.912 _refine_diff_density_rms 0.137