# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Zhenming Yin' _publ_contact_author_address ; Chemistry Nankai University Tianjin 300387 CHINA ; _publ_contact_author_email HSXYYZM@MAIL.TJNU.EDU.CN _publ_section_title ; Hydrogen bonds assisting helical self-assembly and [n]catenane constructing ; loop_ _publ_author_name 'Zhenming Yin' 'Jin-Pei Cheng' 'Jiaqi He' 'Yanhua Zhang' data_51229c _database_code_depnum_ccdc_archive 'CCDC 640218' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C54 H58 Cl4 Hg2 N8 O9' _chemical_formula_weight 1506.06 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.7414(9) _cell_length_b 14.6499(11) _cell_length_c 16.8512(13) _cell_angle_alpha 71.0860(10) _cell_angle_beta 80.2820(10) _cell_angle_gamma 79.0090(10) _cell_volume 2901.6(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3855 _cell_measurement_theta_min 2.24 _cell_measurement_theta_max 22.17 _exptl_crystal_description BLOCK _exptl_crystal_colour COLORLESS _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas NONE _exptl_crystal_density_diffrn 1.723 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1474 _exptl_absorpt_coefficient_mu 5.529 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.627568 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details SADABS _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 15900 _diffrn_reflns_av_R_equivalents 0.0215 _diffrn_reflns_av_sigmaI/netI 0.0462 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.65 _diffrn_reflns_theta_max 25.03 _reflns_number_total 10118 _reflns_number_gt 7360 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART APEX II' _computing_cell_refinement 'Bruker SMART APEX II' _computing_data_reduction 'Bruker SAINT' _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^)+(0.0387P)^2^+15.7983P] 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 10118 _refine_ls_number_parameters 707 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0739 _refine_ls_R_factor_gt 0.0487 _refine_ls_wR_factor_ref 0.1168 _refine_ls_wR_factor_gt 0.1060 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.035 _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 Hg1 Hg 0.26155(3) -0.19759(3) 0.04796(2) 0.04984(11) Uani 1 1 d . . . Hg2 Hg 0.09268(4) 0.22780(3) 1.10076(2) 0.07524(15) Uani 1 1 d . . . Cl1 Cl 0.08370(17) -0.1912(2) 0.11242(16) 0.0695(7) Uani 1 1 d . . . Cl2 Cl 0.3926(2) -0.2012(2) -0.06565(15) 0.0777(7) Uani 1 1 d . . . Cl3 Cl 0.2419(3) 0.2993(2) 1.1003(3) 0.1239(14) Uani 1 1 d . . . Cl4 Cl -0.0473(3) 0.1397(3) 1.1742(2) 0.1153(12) Uani 1 1 d . . . O1 O 0.3030(4) 0.1280(4) 0.2860(3) 0.0484(14) Uani 1 1 d . . . O2 O 0.3835(4) 0.1060(4) 0.4014(3) 0.0434(12) Uani 1 1 d . . . O3 O 0.3709(4) 0.4130(4) 0.5099(3) 0.0461(13) Uani 1 1 d . . . O4 O 0.3697(4) 0.4131(4) 0.6433(3) 0.0441(13) Uani 1 1 d . . . O5 O 0.3034(4) 0.0881(4) 0.6148(3) 0.0432(12) Uani 1 1 d . . . O6 O 0.3686(4) 0.0828(4) 0.7315(3) 0.0491(14) Uani 1 1 d . . . O7 O 0.2132(4) 0.4131(4) 0.3789(3) 0.0441(12) Uani 1 1 d . . . O8 O 0.2176(4) 0.4426(4) 0.2392(3) 0.0491(14) Uani 1 1 d . . . N1 N 0.3121(5) -0.0862(5) 0.1120(4) 0.0466(16) Uani 1 1 d . . . N2 N 0.1781(4) 0.1806(4) 0.4750(3) 0.0306(13) Uani 1 1 d . . . H2 H 0.2235 0.1617 0.5116 0.037 Uiso 1 1 calc R . . N3 N 0.1785(4) 0.3242(4) 0.5634(4) 0.0324(13) Uani 1 1 d . . . H3 H 0.1952 0.3353 0.5099 0.039 Uiso 1 1 calc R . . N4 N 0.6470(5) 0.3224(5) 0.8388(4) 0.0525(17) Uani 1 1 d . . . N5 N 0.1782(6) 0.1426(5) 0.9982(4) 0.0540(18) Uani 1 1 d . . . N6 N 0.4874(4) 0.1682(4) 0.5178(3) 0.0330(13) Uani 1 1 d . . . H6 H 0.4512 0.1525 0.4867 0.040 Uiso 1 1 calc R . . N7 N 0.4359(4) 0.3336(4) 0.3646(3) 0.0325(13) Uani 1 1 d . . . H7 H 0.4167 0.3417 0.4135 0.039 Uiso 1 1 calc R . . N8 N -0.0075(7) 0.6389(6) 0.0093(5) 0.067(2) Uani 1 1 d . . . C1 C 0.4374(6) 0.0009(6) 0.1343(5) 0.048(2) Uani 1 1 d . . . H1 H 0.5053 0.0203 0.1198 0.058 Uiso 1 1 calc R . . C2 C 0.4078(6) -0.0564(6) 0.0939(5) 0.050(2) Uani 1 1 d . . . H2A H 0.4567 -0.0749 0.0522 0.060 Uiso 1 1 calc R . . C3 C 0.2431(7) -0.0577(7) 0.1700(6) 0.058(2) Uani 1 1 d . . . H3A H 0.1750 -0.0763 0.1817 0.070 Uiso 1 1 calc R . . C4 C 0.2678(7) -0.0013(6) 0.2141(5) 0.052(2) Uani 1 1 d . . . H4 H 0.2175 0.0157 0.2558 0.063 Uiso 1 1 calc R . . C5 C 0.3671(6) 0.0297(5) 0.1961(4) 0.0378(17) Uani 1 1 d . . . C6 C 0.3979(6) 0.0891(6) 0.2427(5) 0.047(2) Uani 1 1 d . . . H6A H 0.4471 0.0488 0.2828 0.056 Uiso 1 1 calc R . . H6B H 0.4337 0.1417 0.2035 0.056 Uiso 1 1 calc R . . C7 C 0.3052(6) 0.1328(5) 0.3628(4) 0.0339(16) Uani 1 1 d . . . C8 C 0.1990(6) 0.1728(5) 0.3949(4) 0.0341(16) Uani 1 1 d . . . C9 C 0.1072(6) 0.2117(5) 0.3562(5) 0.0409(18) Uani 1 1 d . . . H9 H 0.0984 0.2164 0.3013 0.049 Uiso 1 1 calc R . . C10 C 0.0294(6) 0.2431(5) 0.4146(5) 0.0405(18) Uani 1 1 d . . . H10 H -0.0407 0.2726 0.4054 0.049 Uiso 1 1 calc R . . C11 C 0.0748(5) 0.2225(5) 0.4880(4) 0.0316(15) Uani 1 1 d . . . C12 C 0.0255(5) 0.2317(5) 0.5735(4) 0.0352(16) Uani 1 1 d . . . C13 C -0.0860(5) 0.2943(6) 0.5678(5) 0.0451(19) Uani 1 1 d . . . H13A H -0.1290 0.2676 0.5408 0.054 Uiso 1 1 calc R . . H13B H -0.1208 0.2884 0.6247 0.054 Uiso 1 1 calc R . . C14 C -0.0869(7) 0.4017(6) 0.5202(6) 0.064(3) Uani 1 1 d . . . H14A H -0.0508 0.4308 0.5494 0.096 Uiso 1 1 calc R . . H14B H -0.1599 0.4335 0.5169 0.096 Uiso 1 1 calc R . . H14C H -0.0505 0.4088 0.4643 0.096 Uiso 1 1 calc R . . C15 C 0.0144(6) 0.1271(5) 0.6352(5) 0.0395(17) Uani 1 1 d . . . H15A H 0.0860 0.0913 0.6436 0.047 Uiso 1 1 calc R . . H15B H -0.0204 0.1332 0.6895 0.047 Uiso 1 1 calc R . . C16 C -0.0482(7) 0.0680(6) 0.6066(6) 0.061(2) Uani 1 1 d . . . H16A H -0.1212 0.0997 0.6028 0.091 Uiso 1 1 calc R . . H16B H -0.0473 0.0040 0.6466 0.091 Uiso 1 1 calc R . . H16C H -0.0159 0.0627 0.5522 0.091 Uiso 1 1 calc R . . C17 C 0.0968(5) 0.2762(5) 0.6098(4) 0.0359(16) Uani 1 1 d . . . C18 C 0.0971(7) 0.2746(7) 0.6920(5) 0.054(2) Uani 1 1 d . . . H18 H 0.0498 0.2463 0.7379 0.064 Uiso 1 1 calc R . . C19 C 0.1800(6) 0.3226(6) 0.6944(5) 0.048(2) Uani 1 1 d . . . H19 H 0.1978 0.3324 0.7421 0.057 Uiso 1 1 calc R . . C20 C 0.2306(5) 0.3525(5) 0.6147(4) 0.0346(16) Uani 1 1 d . . . C21 C 0.3282(6) 0.3945(5) 0.5823(5) 0.0353(16) Uani 1 1 d . . . C22 C 0.4762(6) 0.4408(6) 0.6218(5) 0.0424(18) Uani 1 1 d . . . H22A H 0.4713 0.5113 0.6014 0.051 Uiso 1 1 calc R . . H22B H 0.5155 0.4145 0.5776 0.051 Uiso 1 1 calc R . . C23 C 0.5334(6) 0.4012(5) 0.6993(5) 0.0408(18) Uani 1 1 d . . . C24 C 0.4809(7) 0.3754(7) 0.7792(5) 0.058(2) Uani 1 1 d . . . H24 H 0.4061 0.3836 0.7877 0.069 Uiso 1 1 calc R . . C25 C 0.5399(7) 0.3371(8) 0.8474(6) 0.066(3) Uani 1 1 d . . . H25 H 0.5032 0.3209 0.9016 0.080 Uiso 1 1 calc R . . C26 C 0.6974(6) 0.3496(6) 0.7613(5) 0.052(2) Uani 1 1 d . . . H26 H 0.7722 0.3414 0.7544 0.063 Uiso 1 1 calc R . . C27 C 0.6443(6) 0.3894(6) 0.6905(5) 0.0456(19) Uani 1 1 d . . . H27 H 0.6829 0.4083 0.6373 0.055 Uiso 1 1 calc R . . C28 C 0.1647(6) 0.0398(6) 0.9169(5) 0.047(2) Uani 1 1 d . . . H28 H 0.1304 -0.0077 0.9108 0.057 Uiso 1 1 calc R . . C29 C 0.1326(7) 0.0760(7) 0.9845(5) 0.058(2) Uani 1 1 d . . . H29 H 0.0753 0.0522 1.0229 0.070 Uiso 1 1 calc R . . C30 C 0.2619(8) 0.1729(7) 0.9434(6) 0.062(2) Uani 1 1 d . . . H30 H 0.2983 0.2169 0.9532 0.074 Uiso 1 1 calc R . . C31 C 0.2972(7) 0.1428(7) 0.8733(5) 0.056(2) Uani 1 1 d . . . H31 H 0.3544 0.1681 0.8358 0.067 Uiso 1 1 calc R . . C32 C 0.2480(6) 0.0749(6) 0.8585(5) 0.0428(18) Uani 1 1 d . . . C33 C 0.2773(7) 0.0404(7) 0.7825(5) 0.054(2) Uani 1 1 d . . . H33A H 0.2944 -0.0302 0.7998 0.064 Uiso 1 1 calc R . . H33B H 0.2167 0.0588 0.7497 0.064 Uiso 1 1 calc R . . C34 C 0.3719(6) 0.1043(5) 0.6471(4) 0.0369(17) Uani 1 1 d . . . C35 C 0.4649(5) 0.1498(5) 0.6035(4) 0.0359(16) Uani 1 1 d . . . C36 C 0.5394(6) 0.1854(6) 0.6302(5) 0.0447(19) Uani 1 1 d . . . H36 H 0.5440 0.1823 0.6855 0.054 Uiso 1 1 calc R . . C37 C 0.6076(6) 0.2275(6) 0.5584(5) 0.0452(19) Uani 1 1 d . . . H37 H 0.6651 0.2585 0.5577 0.054 Uiso 1 1 calc R . . C38 C 0.5751(5) 0.2150(5) 0.4890(4) 0.0338(16) Uani 1 1 d . . . C39 C 0.6213(5) 0.2429(5) 0.3975(4) 0.0349(16) Uani 1 1 d . . . C40 C 0.6811(6) 0.1480(6) 0.3770(5) 0.0439(19) Uani 1 1 d . . . H40A H 0.6290 0.1044 0.3852 0.053 Uiso 1 1 calc R . . H40B H 0.7102 0.1653 0.3179 0.053 Uiso 1 1 calc R . . C41 C 0.7723(7) 0.0935(6) 0.4302(7) 0.068(3) Uani 1 1 d . . . H41A H 0.8261 0.1349 0.4207 0.102 Uiso 1 1 calc R . . H41B H 0.8039 0.0360 0.4145 0.102 Uiso 1 1 calc R . . H41C H 0.7444 0.0753 0.4889 0.102 Uiso 1 1 calc R . . C42 C 0.7007(6) 0.3160(6) 0.3840(5) 0.0470(19) Uani 1 1 d . . . H42A H 0.6616 0.3718 0.4006 0.056 Uiso 1 1 calc R . . H42B H 0.7555 0.2852 0.4218 0.056 Uiso 1 1 calc R . . C43 C 0.7565(8) 0.3530(9) 0.2952(7) 0.087(4) Uani 1 1 d . . . H43A H 0.7923 0.2985 0.2763 0.131 Uiso 1 1 calc R . . H43B H 0.8084 0.3927 0.2951 0.131 Uiso 1 1 calc R . . H43C H 0.7042 0.3910 0.2580 0.131 Uiso 1 1 calc R . . C44 C 0.5334(5) 0.2866(5) 0.3398(4) 0.0334(16) Uani 1 1 d . . . C45 C 0.5317(6) 0.2895(6) 0.2586(5) 0.049(2) Uani 1 1 d . . . H45 H 0.5877 0.2632 0.2257 0.059 Uiso 1 1 calc R . . C46 C 0.4317(6) 0.3388(6) 0.2326(5) 0.048(2) Uani 1 1 d . . . H46 H 0.4093 0.3509 0.1799 0.058 Uiso 1 1 calc R . . C47 C 0.3737(6) 0.3656(5) 0.2995(4) 0.0381(17) Uani 1 1 d . . . C48 C 0.2622(6) 0.4076(5) 0.3119(5) 0.0384(17) Uani 1 1 d . . . C49 C 0.1056(6) 0.4749(7) 0.2465(5) 0.060(2) Uani 1 1 d . . . H49A H 0.0886 0.5187 0.2809 0.072 Uiso 1 1 calc R . . H49B H 0.0675 0.4194 0.2742 0.072 Uiso 1 1 calc R . . C50 C 0.0702(6) 0.5262(6) 0.1613(5) 0.0471(19) Uani 1 1 d . . . C51 C 0.1372(7) 0.5674(7) 0.0919(5) 0.063(2) Uani 1 1 d . . . H51 H 0.2110 0.5576 0.0945 0.075 Uiso 1 1 calc R . . C52 C 0.0957(8) 0.6237(7) 0.0179(6) 0.066(3) Uani 1 1 d . . . H52 H 0.1429 0.6523 -0.0280 0.079 Uiso 1 1 calc R . . C53 C -0.0722(9) 0.5945(8) 0.0745(8) 0.088(4) Uani 1 1 d . . . H53 H -0.1446 0.6005 0.0685 0.106 Uiso 1 1 calc R . . C54 C -0.0365(8) 0.5392(8) 0.1514(6) 0.077(3) Uani 1 1 d . . . H54 H -0.0852 0.5109 0.1963 0.092 Uiso 1 1 calc R . . O9 O 0.3242(15) 0.448(2) 0.9374(12) 0.149(9) Uani 0.50 1 d P A 1 O9' O 0.385(2) 0.513(2) 0.9481(19) 0.188(12) Uani 0.50 1 d P B 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 Hg1 0.04852(19) 0.0612(2) 0.03929(19) -0.01478(15) -0.00368(14) -0.00882(15) Hg2 0.1040(3) 0.0694(3) 0.0431(2) -0.01639(19) -0.0205(2) 0.0191(2) Cl1 0.0449(12) 0.0907(18) 0.0706(16) -0.0230(13) -0.0010(11) -0.0117(12) Cl2 0.0897(18) 0.0917(19) 0.0473(14) -0.0274(13) 0.0165(12) -0.0128(15) Cl3 0.173(3) 0.086(2) 0.137(3) -0.030(2) -0.108(3) -0.001(2) Cl4 0.122(3) 0.131(3) 0.070(2) -0.0161(19) 0.0148(18) -0.012(2) O1 0.041(3) 0.070(4) 0.037(3) -0.030(3) -0.010(2) 0.015(3) O2 0.035(3) 0.062(3) 0.037(3) -0.024(3) -0.006(2) 0.000(2) O3 0.045(3) 0.063(4) 0.034(3) -0.015(3) -0.004(2) -0.019(3) O4 0.040(3) 0.063(4) 0.039(3) -0.023(3) -0.004(2) -0.017(3) O5 0.043(3) 0.056(3) 0.032(3) -0.010(2) -0.008(2) -0.012(2) O6 0.043(3) 0.077(4) 0.025(3) -0.011(3) -0.005(2) -0.009(3) O7 0.043(3) 0.054(3) 0.031(3) -0.009(2) -0.008(2) 0.000(2) O8 0.043(3) 0.060(4) 0.038(3) -0.006(3) -0.019(2) 0.005(3) N1 0.048(4) 0.054(4) 0.040(4) -0.019(3) 0.004(3) -0.010(3) N2 0.025(3) 0.038(3) 0.030(3) -0.011(3) -0.005(2) -0.004(2) N3 0.032(3) 0.036(3) 0.028(3) -0.011(3) -0.001(2) -0.004(3) N4 0.049(4) 0.064(5) 0.041(4) -0.008(3) -0.012(3) -0.006(3) N5 0.059(4) 0.058(5) 0.045(4) -0.019(4) -0.008(4) 0.000(4) N6 0.031(3) 0.039(3) 0.032(3) -0.012(3) -0.009(2) -0.007(3) N7 0.033(3) 0.039(3) 0.026(3) -0.009(3) -0.005(2) -0.006(3) N8 0.076(6) 0.067(5) 0.050(5) -0.011(4) -0.024(4) 0.008(4) C1 0.038(4) 0.061(5) 0.052(5) -0.029(4) 0.004(4) -0.008(4) C2 0.045(5) 0.071(6) 0.040(5) -0.032(4) 0.010(4) -0.009(4) C3 0.046(5) 0.072(6) 0.058(6) -0.028(5) 0.013(4) -0.017(4) C4 0.050(5) 0.071(6) 0.039(5) -0.026(4) 0.008(4) -0.009(4) C5 0.046(4) 0.039(4) 0.027(4) -0.011(3) -0.005(3) 0.000(3) C6 0.040(4) 0.066(6) 0.038(4) -0.026(4) -0.001(3) -0.001(4) C7 0.038(4) 0.032(4) 0.035(4) -0.012(3) -0.005(3) -0.008(3) C8 0.042(4) 0.036(4) 0.027(4) -0.012(3) -0.005(3) -0.010(3) C9 0.042(4) 0.051(5) 0.032(4) -0.012(3) -0.011(3) -0.007(4) C10 0.033(4) 0.048(5) 0.041(4) -0.016(4) -0.008(3) -0.001(3) C11 0.028(4) 0.035(4) 0.032(4) -0.009(3) 0.000(3) -0.007(3) C12 0.025(3) 0.044(4) 0.035(4) -0.013(3) 0.001(3) -0.005(3) C13 0.029(4) 0.055(5) 0.048(5) -0.017(4) 0.003(3) -0.001(3) C14 0.052(5) 0.051(5) 0.080(7) -0.017(5) -0.008(5) 0.012(4) C15 0.034(4) 0.045(4) 0.035(4) -0.008(3) 0.004(3) -0.010(3) C16 0.057(5) 0.054(5) 0.071(6) -0.010(5) -0.003(5) -0.025(4) C17 0.032(4) 0.042(4) 0.032(4) -0.010(3) 0.002(3) -0.007(3) C18 0.059(5) 0.074(6) 0.031(4) -0.018(4) 0.009(4) -0.025(5) C19 0.054(5) 0.062(5) 0.033(4) -0.020(4) -0.004(4) -0.014(4) C20 0.034(4) 0.039(4) 0.033(4) -0.014(3) -0.007(3) -0.004(3) C21 0.040(4) 0.031(4) 0.034(4) -0.010(3) -0.007(3) 0.000(3) C22 0.040(4) 0.051(5) 0.041(4) -0.011(4) -0.012(3) -0.016(4) C23 0.054(5) 0.038(4) 0.036(4) -0.015(3) -0.008(4) -0.010(4) C24 0.040(5) 0.089(7) 0.046(5) -0.025(5) -0.011(4) 0.000(4) C25 0.051(5) 0.100(8) 0.039(5) -0.015(5) -0.003(4) -0.004(5) C26 0.040(4) 0.057(5) 0.056(6) -0.008(4) -0.012(4) -0.010(4) C27 0.044(5) 0.058(5) 0.038(4) -0.011(4) -0.005(3) -0.021(4) C28 0.043(4) 0.062(5) 0.040(5) -0.017(4) -0.004(4) -0.014(4) C29 0.048(5) 0.074(6) 0.042(5) -0.011(5) 0.002(4) 0.001(5) C30 0.070(6) 0.065(6) 0.060(6) -0.025(5) -0.018(5) -0.012(5) C31 0.059(5) 0.066(6) 0.043(5) -0.015(4) -0.003(4) -0.016(5) C32 0.036(4) 0.055(5) 0.031(4) -0.007(4) -0.007(3) 0.000(4) C33 0.055(5) 0.076(6) 0.034(4) -0.018(4) 0.003(4) -0.023(5) C34 0.036(4) 0.039(4) 0.033(4) -0.009(3) -0.009(3) 0.004(3) C35 0.035(4) 0.042(4) 0.027(4) -0.010(3) -0.008(3) 0.006(3) C36 0.048(5) 0.057(5) 0.035(4) -0.017(4) -0.016(4) -0.005(4) C37 0.040(4) 0.054(5) 0.047(5) -0.014(4) -0.012(4) -0.013(4) C38 0.030(4) 0.037(4) 0.035(4) -0.011(3) -0.009(3) 0.000(3) C39 0.027(3) 0.039(4) 0.041(4) -0.015(3) -0.005(3) -0.003(3) C40 0.036(4) 0.046(5) 0.053(5) -0.021(4) -0.002(4) -0.005(3) C41 0.055(5) 0.050(6) 0.106(8) -0.035(5) -0.026(5) 0.011(4) C42 0.037(4) 0.044(5) 0.060(5) -0.013(4) -0.009(4) -0.008(3) C43 0.072(7) 0.112(9) 0.075(7) -0.007(6) 0.005(6) -0.057(7) C44 0.032(4) 0.037(4) 0.029(4) -0.006(3) -0.001(3) -0.009(3) C45 0.044(5) 0.064(6) 0.041(5) -0.023(4) 0.002(4) -0.006(4) C46 0.046(5) 0.067(6) 0.031(4) -0.015(4) -0.004(3) -0.010(4) C47 0.041(4) 0.042(4) 0.029(4) -0.001(3) -0.011(3) -0.013(3) C48 0.042(4) 0.034(4) 0.037(4) -0.001(3) -0.013(4) -0.008(3) C49 0.041(5) 0.071(6) 0.049(5) 0.007(4) -0.016(4) 0.000(4) C50 0.051(5) 0.045(5) 0.043(5) -0.007(4) -0.017(4) -0.002(4) C51 0.054(5) 0.080(7) 0.048(5) -0.013(5) -0.017(4) 0.003(5) C52 0.062(6) 0.085(7) 0.043(5) -0.011(5) -0.016(4) 0.002(5) C53 0.063(7) 0.086(8) 0.104(9) 0.000(7) -0.048(7) -0.001(6) C54 0.059(6) 0.086(7) 0.065(6) 0.016(5) -0.025(5) -0.014(5) O9 0.082(12) 0.27(3) 0.087(14) -0.044(16) 0.008(10) -0.026(16) O9' 0.16(2) 0.19(3) 0.19(3) -0.04(2) 0.06(2) -0.07(2) _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 Cl2 2.326(2) . ? Hg1 Cl1 2.341(2) . ? Hg1 N1 2.452(6) . ? Hg1 N4 2.454(6) 2_656 ? Hg2 Cl3 2.336(4) . ? Hg2 Cl4 2.340(4) . ? Hg2 N8 2.440(7) 2_566 ? Hg2 N5 2.445(7) . ? O1 C7 1.324(8) . ? O1 C6 1.424(8) . ? O2 C7 1.215(8) . ? O3 C21 1.215(8) . ? O4 C21 1.353(8) . ? O4 C22 1.444(8) . ? O5 C34 1.200(8) . ? O6 C34 1.347(8) . ? O6 C33 1.438(9) . ? O7 C48 1.214(9) . ? O8 C48 1.343(8) . ? O8 C49 1.413(9) . ? N1 C3 1.318(10) . ? N1 C2 1.328(10) . ? N2 C11 1.357(8) . ? N2 C8 1.370(8) . ? N2 H2 0.8600 . ? N3 C17 1.355(8) . ? N3 C20 1.376(9) . ? N3 H3 0.8600 . ? N4 C26 1.324(10) . ? N4 C25 1.330(10) . ? N4 Hg1 2.454(6) 2_656 ? N5 C29 1.322(11) . ? N5 C30 1.331(11) . ? N6 C38 1.359(8) . ? N6 C35 1.371(9) . ? N6 H6 0.8600 . ? N7 C47 1.367(8) . ? N7 C44 1.369(9) . ? N7 H7 0.8600 . ? N8 C52 1.315(11) . ? N8 C53 1.321(13) . ? N8 Hg2 2.440(7) 2_566 ? C1 C2 1.375(11) . ? C1 C5 1.375(10) . ? C1 H1 0.9300 . ? C2 H2A 0.9300 . ? C3 C4 1.382(12) . ? C3 H3A 0.9300 . ? C4 C5 1.378(11) . ? C4 H4 0.9300 . ? C5 C6 1.484(10) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C8 1.457(10) . ? C8 C9 1.371(10) . ? C9 C10 1.398(10) . ? C9 H9 0.9300 . ? C10 C11 1.374(10) . ? C10 H10 0.9300 . ? C11 C12 1.508(9) . ? C12 C17 1.515(10) . ? C12 C13 1.537(9) . ? C12 C15 1.565(10) . ? C13 C14 1.515(11) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 C16 1.511(11) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 C18 1.378(10) . ? C18 C19 1.389(11) . ? C18 H18 0.9300 . ? C19 C20 1.358(10) . ? C19 H19 0.9300 . ? C20 C21 1.437(10) . ? C22 C23 1.498(10) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 C24 1.366(11) . ? C23 C27 1.380(10) . ? C24 C25 1.384(11) . ? C24 H24 0.9300 . ? C25 H25 0.9300 . ? C26 C27 1.374(11) . ? C26 H26 0.9300 . ? C27 H27 0.9300 . ? C28 C32 1.373(10) . ? C28 C29 1.378(12) . ? C28 H28 0.9300 . ? C29 H29 0.9300 . ? C30 C31 1.369(12) . ? C30 H30 0.9300 . ? C31 C32 1.377(11) . ? C31 H31 0.9300 . ? C32 C33 1.491(11) . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C34 C35 1.441(10) . ? C35 C36 1.364(10) . ? C36 C37 1.401(11) . ? C36 H36 0.9300 . ? C37 C38 1.381(10) . ? C37 H37 0.9300 . ? C38 C39 1.505(10) . ? C39 C44 1.517(9) . ? C39 C42 1.549(10) . ? C39 C40 1.565(10) . ? C40 C41 1.525(11) . ? C40 H40A 0.9700 . ? C40 H40B 0.9700 . ? C41 H41A 0.9600 . ? C41 H41B 0.9600 . ? C41 H41C 0.9600 . ? C42 C43 1.517(12) . ? C42 H42A 0.9700 . ? C42 H42B 0.9700 . ? C43 H43A 0.9600 . ? C43 H43B 0.9600 . ? C43 H43C 0.9600 . ? C44 C45 1.359(10) . ? C45 C46 1.404(11) . ? C45 H45 0.9300 . ? C46 C47 1.366(11) . ? C46 H46 0.9300 . ? C47 C48 1.446(10) . ? C49 C50 1.491(10) . ? C49 H49A 0.9700 . ? C49 H49B 0.9700 . ? C50 C51 1.365(12) . ? C50 C54 1.367(11) . ? C51 C52 1.380(11) . ? C51 H51 0.9300 . ? C52 H52 0.9300 . ? C53 C54 1.385(13) . ? C53 H53 0.9300 . ? C54 H54 0.9300 . ? 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 Cl2 Hg1 Cl1 153.09(10) . . ? Cl2 Hg1 N1 105.23(16) . . ? Cl1 Hg1 N1 95.16(16) . . ? Cl2 Hg1 N4 99.50(18) . 2_656 ? Cl1 Hg1 N4 100.33(17) . 2_656 ? N1 Hg1 N4 82.8(2) . 2_656 ? Cl3 Hg2 Cl4 150.38(14) . . ? Cl3 Hg2 N8 97.5(2) . 2_566 ? Cl4 Hg2 N8 104.0(2) . 2_566 ? Cl3 Hg2 N5 96.0(2) . . ? Cl4 Hg2 N5 103.6(2) . . ? N8 Hg2 N5 91.2(2) 2_566 . ? C7 O1 C6 119.7(6) . . ? C21 O4 C22 116.5(6) . . ? C34 O6 C33 117.1(6) . . ? C48 O8 C49 115.8(6) . . ? C3 N1 C2 117.9(7) . . ? C3 N1 Hg1 118.9(5) . . ? C2 N1 Hg1 123.2(5) . . ? C11 N2 C8 109.6(6) . . ? C11 N2 H2 125.2 . . ? C8 N2 H2 125.2 . . ? C17 N3 C20 109.9(6) . . ? C17 N3 H3 125.0 . . ? C20 N3 H3 125.0 . . ? C26 N4 C25 117.5(7) . . ? C26 N4 Hg1 120.3(5) . 2_656 ? C25 N4 Hg1 118.3(6) . 2_656 ? C29 N5 C30 116.3(8) . . ? C29 N5 Hg2 121.4(6) . . ? C30 N5 Hg2 121.2(6) . . ? C38 N6 C35 110.2(6) . . ? C38 N6 H6 124.9 . . ? C35 N6 H6 124.9 . . ? C47 N7 C44 109.6(6) . . ? C47 N7 H7 125.2 . . ? C44 N7 H7 125.2 . . ? C52 N8 C53 117.2(8) . . ? C52 N8 Hg2 124.3(7) . 2_566 ? C53 N8 Hg2 116.6(6) . 2_566 ? C2 C1 C5 120.2(7) . . ? C2 C1 H1 119.9 . . ? C5 C1 H1 119.9 . . ? N1 C2 C1 122.5(7) . . ? N1 C2 H2A 118.8 . . ? C1 C2 H2A 118.8 . . ? N1 C3 C4 122.9(8) . . ? N1 C3 H3A 118.6 . . ? C4 C3 H3A 118.6 . . ? C5 C4 C3 119.7(7) . . ? C5 C4 H4 120.2 . . ? C3 C4 H4 120.2 . . ? C1 C5 C4 116.8(7) . . ? C1 C5 C6 121.5(7) . . ? C4 C5 C6 121.7(7) . . ? O1 C6 C5 108.7(6) . . ? O1 C6 H6A 110.0 . . ? C5 C6 H6A 110.0 . . ? O1 C6 H6B 110.0 . . ? C5 C6 H6B 110.0 . . ? H6A C6 H6B 108.3 . . ? O2 C7 O1 125.1(6) . . ? O2 C7 C8 125.2(6) . . ? O1 C7 C8 109.8(6) . . ? N2 C8 C9 107.7(6) . . ? N2 C8 C7 121.5(6) . . ? C9 C8 C7 130.8(7) . . ? C8 C9 C10 107.3(6) . . ? C8 C9 H9 126.4 . . ? C10 C9 H9 126.4 . . ? C11 C10 C9 107.9(6) . . ? C11 C10 H10 126.0 . . ? C9 C10 H10 126.0 . . ? N2 C11 C10 107.5(6) . . ? N2 C11 C12 121.5(6) . . ? C10 C11 C12 130.7(6) . . ? C11 C12 C17 111.3(5) . . ? C11 C12 C13 110.7(6) . . ? C17 C12 C13 109.3(6) . . ? C11 C12 C15 108.4(6) . . ? C17 C12 C15 107.5(6) . . ? C13 C12 C15 109.5(6) . . ? C14 C13 C12 115.8(6) . . ? C14 C13 H13A 108.3 . . ? C12 C13 H13A 108.3 . . ? C14 C13 H13B 108.3 . . ? C12 C13 H13B 108.3 . . ? H13A C13 H13B 107.4 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C16 C15 C12 115.4(6) . . ? C16 C15 H15A 108.4 . . ? C12 C15 H15A 108.4 . . ? C16 C15 H15B 108.4 . . ? C12 C15 H15B 108.4 . . ? H15A C15 H15B 107.5 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N3 C17 C18 106.6(6) . . ? N3 C17 C12 123.7(6) . . ? C18 C17 C12 129.6(6) . . ? C17 C18 C19 108.4(7) . . ? C17 C18 H18 125.8 . . ? C19 C18 H18 125.8 . . ? C20 C19 C18 107.7(7) . . ? C20 C19 H19 126.1 . . ? C18 C19 H19 126.1 . . ? C19 C20 N3 107.4(6) . . ? C19 C20 C21 131.7(7) . . ? N3 C20 C21 120.5(6) . . ? O3 C21 O4 121.9(6) . . ? O3 C21 C20 126.6(7) . . ? O4 C21 C20 111.5(6) . . ? O4 C22 C23 108.3(6) . . ? O4 C22 H22A 110.0 . . ? C23 C22 H22A 110.0 . . ? O4 C22 H22B 110.0 . . ? C23 C22 H22B 110.0 . . ? H22A C22 H22B 108.4 . . ? C24 C23 C27 117.8(7) . . ? C24 C23 C22 123.1(7) . . ? C27 C23 C22 119.1(7) . . ? C23 C24 C25 119.5(8) . . ? C23 C24 H24 120.3 . . ? C25 C24 H24 120.3 . . ? N4 C25 C24 122.7(8) . . ? N4 C25 H25 118.6 . . ? C24 C25 H25 118.6 . . ? N4 C26 C27 123.1(7) . . ? N4 C26 H26 118.4 . . ? C27 C26 H26 118.4 . . ? C26 C27 C23 119.4(7) . . ? C26 C27 H27 120.3 . . ? C23 C27 H27 120.3 . . ? C32 C28 C29 119.2(8) . . ? C32 C28 H28 120.4 . . ? C29 C28 H28 120.4 . . ? N5 C29 C28 124.1(8) . . ? N5 C29 H29 118.0 . . ? C28 C29 H29 118.0 . . ? N5 C30 C31 123.3(9) . . ? N5 C30 H30 118.3 . . ? C31 C30 H30 118.3 . . ? C30 C31 C32 120.0(8) . . ? C30 C31 H31 120.0 . . ? C32 C31 H31 120.0 . . ? C28 C32 C31 117.0(8) . . ? C28 C32 C33 118.8(7) . . ? C31 C32 C33 124.1(7) . . ? O6 C33 C32 109.9(7) . . ? O6 C33 H33A 109.7 . . ? C32 C33 H33A 109.7 . . ? O6 C33 H33B 109.7 . . ? C32 C33 H33B 109.7 . . ? H33A C33 H33B 108.2 . . ? O5 C34 O6 122.5(7) . . ? O5 C34 C35 126.1(7) . . ? O6 C34 C35 111.5(6) . . ? C36 C35 N6 107.9(6) . . ? C36 C35 C34 132.4(7) . . ? N6 C35 C34 119.7(6) . . ? C35 C36 C37 107.0(7) . . ? C35 C36 H36 126.5 . . ? C37 C36 H36 126.5 . . ? C38 C37 C36 108.5(6) . . ? C38 C37 H37 125.7 . . ? C36 C37 H37 125.7 . . ? N6 C38 C37 106.4(6) . . ? N6 C38 C39 122.7(6) . . ? C37 C38 C39 130.9(6) . . ? C38 C39 C44 111.3(5) . . ? C38 C39 C42 108.3(6) . . ? C44 C39 C42 110.9(6) . . ? C38 C39 C40 108.1(6) . . ? C44 C39 C40 107.4(6) . . ? C42 C39 C40 110.7(6) . . ? C41 C40 C39 114.6(7) . . ? C41 C40 H40A 108.6 . . ? C39 C40 H40A 108.6 . . ? C41 C40 H40B 108.6 . . ? C39 C40 H40B 108.6 . . ? H40A C40 H40B 107.6 . . ? C40 C41 H41A 109.5 . . ? C40 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C40 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C43 C42 C39 116.5(7) . . ? C43 C42 H42A 108.2 . . ? C39 C42 H42A 108.2 . . ? C43 C42 H42B 108.2 . . ? C39 C42 H42B 108.2 . . ? H42A C42 H42B 107.3 . . ? C42 C43 H43A 109.5 . . ? C42 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C42 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C45 C44 N7 106.9(6) . . ? C45 C44 C39 130.3(7) . . ? N7 C44 C39 122.8(6) . . ? C44 C45 C46 108.8(7) . . ? C44 C45 H45 125.6 . . ? C46 C45 H45 125.6 . . ? C47 C46 C45 106.8(7) . . ? C47 C46 H46 126.6 . . ? C45 C46 H46 126.6 . . ? C46 C47 N7 107.9(7) . . ? C46 C47 C48 130.8(7) . . ? N7 C47 C48 120.8(6) . . ? O7 C48 O8 122.7(7) . . ? O7 C48 C47 125.4(6) . . ? O8 C48 C47 111.9(6) . . ? O8 C49 C50 110.1(7) . . ? O8 C49 H49A 109.6 . . ? C50 C49 H49A 109.6 . . ? O8 C49 H49B 109.6 . . ? C50 C49 H49B 109.6 . . ? H49A C49 H49B 108.2 . . ? C51 C50 C54 116.7(8) . . ? C51 C50 C49 123.9(7) . . ? C54 C50 C49 119.3(8) . . ? C50 C51 C52 120.1(8) . . ? C50 C51 H51 119.9 . . ? C52 C51 H51 119.9 . . ? N8 C52 C51 123.1(9) . . ? N8 C52 H52 118.4 . . ? C51 C52 H52 118.4 . . ? N8 C53 C54 122.7(9) . . ? N8 C53 H53 118.6 . . ? C54 C53 H53 118.6 . . ? C50 C54 C53 120.0(9) . . ? C50 C54 H54 120.0 . . ? C53 C54 H54 120.0 . . ? 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 Cl2 Hg1 N1 C3 169.4(6) . . . . ? Cl1 Hg1 N1 C3 7.1(6) . . . . ? N4 Hg1 N1 C3 -92.6(7) 2_656 . . . ? Cl2 Hg1 N1 C2 -13.7(7) . . . . ? Cl1 Hg1 N1 C2 -176.0(6) . . . . ? N4 Hg1 N1 C2 84.2(6) 2_656 . . . ? Cl3 Hg2 N5 C29 169.0(6) . . . . ? Cl4 Hg2 N5 C29 11.4(7) . . . . ? N8 Hg2 N5 C29 -93.4(7) 2_566 . . . ? Cl3 Hg2 N5 C30 -23.2(7) . . . . ? Cl4 Hg2 N5 C30 179.2(6) . . . . ? N8 Hg2 N5 C30 74.4(7) 2_566 . . . ? C3 N1 C2 C1 1.3(13) . . . . ? Hg1 N1 C2 C1 -175.6(6) . . . . ? C5 C1 C2 N1 0.0(13) . . . . ? C2 N1 C3 C4 -2.2(13) . . . . ? Hg1 N1 C3 C4 174.8(7) . . . . ? N1 C3 C4 C5 1.9(14) . . . . ? C2 C1 C5 C4 -0.3(12) . . . . ? C2 C1 C5 C6 178.1(8) . . . . ? C3 C4 C5 C1 -0.6(12) . . . . ? C3 C4 C5 C6 -179.0(8) . . . . ? C7 O1 C6 C5 141.1(7) . . . . ? C1 C5 C6 O1 165.5(7) . . . . ? C4 C5 C6 O1 -16.2(10) . . . . ? C6 O1 C7 O2 -0.2(11) . . . . ? C6 O1 C7 C8 -178.7(6) . . . . ? C11 N2 C8 C9 0.7(8) . . . . ? C11 N2 C8 C7 178.1(6) . . . . ? O2 C7 C8 N2 -2.1(11) . . . . ? O1 C7 C8 N2 176.5(6) . . . . ? O2 C7 C8 C9 174.7(8) . . . . ? O1 C7 C8 C9 -6.8(11) . . . . ? N2 C8 C9 C10 -0.3(8) . . . . ? C7 C8 C9 C10 -177.4(7) . . . . ? C8 C9 C10 C11 -0.2(9) . . . . ? C8 N2 C11 C10 -0.8(8) . . . . ? C8 N2 C11 C12 174.0(6) . . . . ? C9 C10 C11 N2 0.6(8) . . . . ? C9 C10 C11 C12 -173.5(7) . . . . ? N2 C11 C12 C17 50.3(9) . . . . ? C10 C11 C12 C17 -136.3(8) . . . . ? N2 C11 C12 C13 172.0(6) . . . . ? C10 C11 C12 C13 -14.5(11) . . . . ? N2 C11 C12 C15 -67.8(8) . . . . ? C10 C11 C12 C15 105.6(8) . . . . ? C11 C12 C13 C14 -68.9(9) . . . . ? C17 C12 C13 C14 54.1(9) . . . . ? C15 C12 C13 C14 171.6(7) . . . . ? C11 C12 C15 C16 -55.6(8) . . . . ? C17 C12 C15 C16 -176.0(6) . . . . ? C13 C12 C15 C16 65.3(8) . . . . ? C20 N3 C17 C18 0.3(8) . . . . ? C20 N3 C17 C12 -177.6(6) . . . . ? C11 C12 C17 N3 15.9(9) . . . . ? C13 C12 C17 N3 -106.7(7) . . . . ? C15 C12 C17 N3 134.5(7) . . . . ? C11 C12 C17 C18 -161.5(8) . . . . ? C13 C12 C17 C18 76.0(10) . . . . ? C15 C12 C17 C18 -42.9(10) . . . . ? N3 C17 C18 C19 0.1(9) . . . . ? C12 C17 C18 C19 177.8(7) . . . . ? C17 C18 C19 C20 -0.5(10) . . . . ? C18 C19 C20 N3 0.7(9) . . . . ? C18 C19 C20 C21 -171.5(8) . . . . ? C17 N3 C20 C19 -0.6(8) . . . . ? C17 N3 C20 C21 172.6(6) . . . . ? C22 O4 C21 O3 -9.9(10) . . . . ? C22 O4 C21 C20 170.5(6) . . . . ? C19 C20 C21 O3 174.6(8) . . . . ? N3 C20 C21 O3 3.4(11) . . . . ? C19 C20 C21 O4 -5.8(11) . . . . ? N3 C20 C21 O4 -177.0(6) . . . . ? C21 O4 C22 C23 -146.2(6) . . . . ? O4 C22 C23 C24 -20.8(11) . . . . ? O4 C22 C23 C27 159.0(7) . . . . ? C27 C23 C24 C25 -1.4(13) . . . . ? C22 C23 C24 C25 178.4(8) . . . . ? C26 N4 C25 C24 2.6(15) . . . . ? Hg1 N4 C25 C24 -155.0(8) 2_656 . . . ? C23 C24 C25 N4 -1.1(15) . . . . ? C25 N4 C26 C27 -1.7(13) . . . . ? Hg1 N4 C26 C27 155.5(7) 2_656 . . . ? N4 C26 C27 C23 -0.8(13) . . . . ? C24 C23 C27 C26 2.3(12) . . . . ? C22 C23 C27 C26 -177.5(7) . . . . ? C30 N5 C29 C28 -1.9(13) . . . . ? Hg2 N5 C29 C28 166.4(6) . . . . ? C32 C28 C29 N5 -1.0(13) . . . . ? C29 N5 C30 C31 3.7(13) . . . . ? Hg2 N5 C30 C31 -164.7(7) . . . . ? N5 C30 C31 C32 -2.6(14) . . . . ? C29 C28 C32 C31 2.2(12) . . . . ? C29 C28 C32 C33 -175.8(8) . . . . ? C30 C31 C32 C28 -0.5(12) . . . . ? C30 C31 C32 C33 177.3(8) . . . . ? C34 O6 C33 C32 -145.6(7) . . . . ? C28 C32 C33 O6 -177.8(7) . . . . ? C31 C32 C33 O6 4.4(11) . . . . ? C33 O6 C34 O5 -1.2(11) . . . . ? C33 O6 C34 C35 177.6(7) . . . . ? C38 N6 C35 C36 0.1(8) . . . . ? C38 N6 C35 C34 177.3(6) . . . . ? O5 C34 C35 C36 168.9(8) . . . . ? O6 C34 C35 C36 -9.9(11) . . . . ? O5 C34 C35 N6 -7.6(11) . . . . ? O6 C34 C35 N6 173.7(6) . . . . ? N6 C35 C36 C37 0.8(8) . . . . ? C34 C35 C36 C37 -176.0(7) . . . . ? C35 C36 C37 C38 -1.3(9) . . . . ? C35 N6 C38 C37 -0.9(8) . . . . ? C35 N6 C38 C39 178.5(6) . . . . ? C36 C37 C38 N6 1.4(8) . . . . ? C36 C37 C38 C39 -177.9(7) . . . . ? N6 C38 C39 C44 43.9(9) . . . . ? C37 C38 C39 C44 -136.9(8) . . . . ? N6 C38 C39 C42 166.0(6) . . . . ? C37 C38 C39 C42 -14.8(10) . . . . ? N6 C38 C39 C40 -73.9(8) . . . . ? C37 C38 C39 C40 105.3(9) . . . . ? C38 C39 C40 C41 -59.2(8) . . . . ? C44 C39 C40 C41 -179.5(7) . . . . ? C42 C39 C40 C41 59.3(9) . . . . ? C38 C39 C42 C43 179.8(7) . . . . ? C44 C39 C42 C43 -57.8(9) . . . . ? C40 C39 C42 C43 61.4(9) . . . . ? C47 N7 C44 C45 0.0(8) . . . . ? C47 N7 C44 C39 179.6(6) . . . . ? C38 C39 C44 C45 -153.7(8) . . . . ? C42 C39 C44 C45 85.6(10) . . . . ? C40 C39 C44 C45 -35.5(10) . . . . ? C38 C39 C44 N7 26.8(9) . . . . ? C42 C39 C44 N7 -93.9(8) . . . . ? C40 C39 C44 N7 145.0(6) . . . . ? N7 C44 C45 C46 -0.1(9) . . . . ? C39 C44 C45 C46 -179.7(7) . . . . ? C44 C45 C46 C47 0.2(9) . . . . ? C45 C46 C47 N7 -0.1(9) . . . . ? C45 C46 C47 C48 -171.8(8) . . . . ? C44 N7 C47 C46 0.1(8) . . . . ? C44 N7 C47 C48 172.7(6) . . . . ? C49 O8 C48 O7 -8.2(11) . . . . ? C49 O8 C48 C47 173.0(7) . . . . ? C46 C47 C48 O7 166.3(8) . . . . ? N7 C47 C48 O7 -4.5(11) . . . . ? C46 C47 C48 O8 -15.0(11) . . . . ? N7 C47 C48 O8 174.3(6) . . . . ? C48 O8 C49 C50 170.8(7) . . . . ? O8 C49 C50 C51 -22.4(13) . . . . ? O8 C49 C50 C54 161.9(9) . . . . ? C54 C50 C51 C52 3.7(15) . . . . ? C49 C50 C51 C52 -172.1(9) . . . . ? C53 N8 C52 C51 -2.5(16) . . . . ? Hg2 N8 C52 C51 160.9(8) 2_566 . . . ? C50 C51 C52 N8 -1.5(16) . . . . ? C52 N8 C53 C54 4.4(17) . . . . ? Hg2 N8 C53 C54 -160.4(10) 2_566 . . . ? C51 C50 C54 C53 -1.9(16) . . . . ? C49 C50 C54 C53 174.1(10) . . . . ? N8 C53 C54 C50 -2.2(19) . . . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 4.705 _refine_diff_density_min -3.786 _refine_diff_density_rms 0.119