# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_coden_Cambridge 182 _journal_volume ? _journal_page_first ? _journal_year ? loop_ _publ_author_name 'Mir Wais Hosseini' 'Abdelaziz Jouaiti' 'Nathalie Kyritsakas' 'Mei-Jin Lin.' _publ_contact_author_name 'Mir Wais Hosseini' _publ_contact_author_email HOSSEINI@CHIMIE.U-STRASBG.FR _publ_section_title ; Molecular tectonics: from 1-D interwoven racemic chains to quadruple -stranded helices ; # Attachment '1-HgCl2.cif' data_e1512a _database_code_depnum_ccdc_archive 'CCDC 743764' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C66 H60 Cl2 Hg N4 O8' _chemical_formula_sum 'C66 H60 Cl2 Hg N4 O8' _chemical_formula_weight 1308.67 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' 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' 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' H H 0.0000 0.0000 '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 13.1808(12) _cell_length_b 14.0766(12) _cell_length_c 17.3666(15) _cell_angle_alpha 67.326(2) _cell_angle_beta 89.185(2) _cell_angle_gamma 76.700(3) _cell_volume 2883.5(4) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 4722 _cell_measurement_theta_min 2.59 _cell_measurement_theta_max 27.58 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.507 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1324 _exptl_absorpt_coefficient_mu 2.822 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7282 _exptl_absorpt_correction_T_max 0.8489 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 20466 _diffrn_reflns_av_R_equivalents 0.0379 _diffrn_reflns_av_sigmaI/netI 0.0883 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.59 _diffrn_reflns_theta_max 27.58 _reflns_number_total 12910 _reflns_number_gt 9823 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _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^)+(0.0588P)^2^+25.7501P] 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 12910 _refine_ls_number_parameters 732 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0888 _refine_ls_R_factor_gt 0.0622 _refine_ls_wR_factor_ref 0.1738 _refine_ls_wR_factor_gt 0.1613 _refine_ls_goodness_of_fit_ref 1.062 _refine_ls_restrained_S_all 1.062 _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 0.24319(3) 0.51870(3) 0.47260(2) 0.02888(10) Uani 1 1 d . . . Cl1 Cl 0.39120(17) 0.39300(16) 0.55500(14) 0.0367(5) Uani 1 1 d . . . Cl2 Cl 0.07581(17) 0.62209(18) 0.41327(17) 0.0438(6) Uani 1 1 d . . . N1 N 0.2865(5) 0.6673(5) 0.5095(4) 0.0288(15) Uani 1 1 d . . . C1 C 0.2178(7) 0.7542(7) 0.5073(6) 0.035(2) Uani 1 1 d . . . H1 H 0.1488 0.7688 0.4834 0.042 Uiso 1 1 calc R . . C2 C 0.2413(7) 0.8239(7) 0.5376(6) 0.035(2) Uani 1 1 d . . . H2 H 0.1890 0.8834 0.5368 0.042 Uiso 1 1 calc R . . C3 C 0.3433(6) 0.8054(6) 0.5697(5) 0.0243(16) Uani 1 1 d . . . C4 C 0.4159(6) 0.7167(6) 0.5720(5) 0.0260(16) Uani 1 1 d . . . H4 H 0.4862 0.7018 0.5936 0.031 Uiso 1 1 calc R . . C5 C 0.3835(7) 0.6497(7) 0.5419(6) 0.0321(19) Uani 1 1 d . . . H5 H 0.4332 0.5876 0.5444 0.039 Uiso 1 1 calc R . . C6 C 0.3700(7) 0.8829(6) 0.6004(5) 0.0299(18) Uani 1 1 d . . . O1 O 0.3096(5) 0.9546(6) 0.6071(6) 0.060(2) Uani 1 1 d . . . O2 O 0.4746(4) 0.8594(4) 0.6206(4) 0.0299(13) Uani 1 1 d . . . C7 C 0.5125(6) 0.9248(6) 0.6531(5) 0.0265(17) Uani 1 1 d . . . C8 C 0.5089(6) 1.0278(6) 0.6017(5) 0.0266(17) Uani 1 1 d . . . H8 H 0.4784 1.0571 0.5457 0.032 Uiso 1 1 calc R . . C9 C 0.5508(7) 1.0882(6) 0.6333(5) 0.0304(18) Uani 1 1 d . . . H9 H 0.5469 1.1607 0.5997 0.036 Uiso 1 1 calc R . . C10 C 0.5989(6) 1.0423(6) 0.7149(5) 0.0236(16) Uani 1 1 d . . . C11 C 0.6011(6) 0.9379(6) 0.7642(5) 0.0234(16) Uani 1 1 d . . . C12 C 0.5592(6) 0.8762(6) 0.7338(5) 0.0250(16) Uani 1 1 d . . . H12 H 0.5625 0.8037 0.7671 0.030 Uiso 1 1 calc R . . C13 C 0.6464(7) 1.0955(6) 0.7617(5) 0.0296(18) Uani 1 1 d . . . C14 C 0.7019(7) 0.9972(6) 0.8409(5) 0.0336(19) Uani 1 1 d . . . H14A H 0.6946 1.0148 0.8910 0.040 Uiso 1 1 calc R . . H14B H 0.7774 0.9763 0.8339 0.040 Uiso 1 1 calc R . . C15 C 0.6500(6) 0.9040(6) 0.8521(5) 0.0255(17) Uani 1 1 d . . . C16 C 0.7251(8) 1.1552(8) 0.7124(6) 0.040(2) Uani 1 1 d . . . H16A H 0.7778 1.1075 0.6950 0.060 Uiso 1 1 calc R . . H16B H 0.7594 1.1806 0.7478 0.060 Uiso 1 1 calc R . . H16C H 0.6885 1.2159 0.6627 0.060 Uiso 1 1 calc R . . C17 C 0.5599(8) 1.1703(7) 0.7842(6) 0.041(2) Uani 1 1 d . . . H17A H 0.5222 1.2268 0.7328 0.062 Uiso 1 1 calc R . . H17B H 0.5906 1.2017 0.8168 0.062 Uiso 1 1 calc R . . H17C H 0.5113 1.1307 0.8174 0.062 Uiso 1 1 calc R . . C18 C 0.5682(7) 0.8860(7) 0.9178(5) 0.0318(19) Uani 1 1 d . . . H18A H 0.5075 0.8707 0.8961 0.038 Uiso 1 1 calc R . . H18B H 0.5431 0.9506 0.9296 0.038 Uiso 1 1 calc R . . C19 C 0.6202(6) 0.7909(6) 0.9993(5) 0.0248(16) Uani 1 1 d . . . C20 C 0.7117(6) 0.7341(6) 0.9665(4) 0.0243(16) Uani 1 1 d . . . C21 C 0.7290(6) 0.7969(6) 0.8859(5) 0.0218(15) Uani 1 1 d . . . C22 C 0.5455(7) 0.7223(8) 1.0410(6) 0.040(2) Uani 1 1 d . . . H22A H 0.5223 0.6945 1.0023 0.059 Uiso 1 1 calc R . . H22B H 0.4846 0.7651 1.0556 0.059 Uiso 1 1 calc R . . H22C H 0.5812 0.6632 1.0919 0.059 Uiso 1 1 calc R . . C23 C 0.6646(9) 0.8291(8) 1.0608(6) 0.044(2) Uani 1 1 d . . . H23A H 0.6977 0.7676 1.1113 0.065 Uiso 1 1 calc R . . H23B H 0.6077 0.8754 1.0761 0.065 Uiso 1 1 calc R . . H23C H 0.7166 0.8686 1.0342 0.065 Uiso 1 1 calc R . . C24 C 0.7766(7) 0.6344(7) 1.0071(5) 0.0311(18) Uani 1 1 d . . . H24 H 0.7642 0.5910 1.0620 0.037 Uiso 1 1 calc R . . C25 C 0.8604(6) 0.5969(7) 0.9680(5) 0.033(2) Uani 1 1 d . . . H25 H 0.9050 0.5279 0.9951 0.039 Uiso 1 1 calc R . . C26 C 0.8762(6) 0.6629(7) 0.8889(5) 0.0292(18) Uani 1 1 d . . . C27 C 0.8124(6) 0.7621(6) 0.8460(5) 0.0265(17) Uani 1 1 d . . . H27 H 0.8251 0.8053 0.7911 0.032 Uiso 1 1 calc R . . O3 O 0.9675(4) 0.6320(5) 0.8506(4) 0.0358(14) Uani 1 1 d . . . O4 O 0.9037(5) 0.5094(6) 0.8291(5) 0.0489(18) Uani 1 1 d . . . C28 C 0.9704(6) 0.5552(7) 0.8222(5) 0.0292(18) Uani 1 1 d . . . C29 C 1.0694(6) 0.5354(6) 0.7803(5) 0.0280(17) Uani 1 1 d . . . C30 C 1.1425(7) 0.5935(7) 0.7714(5) 0.0336(19) Uani 1 1 d . . . H30 H 1.1337 0.6461 0.7941 0.040 Uiso 1 1 calc R . . C31 C 1.2285(7) 0.5746(8) 0.7290(6) 0.039(2) Uani 1 1 d . . . H31 H 1.2782 0.6159 0.7226 0.047 Uiso 1 1 calc R . . N2 N 1.2455(8) 0.5020(8) 0.6968(6) 0.061(3) Uani 1 1 d . . . C32 C 1.1742(10) 0.4462(9) 0.7068(8) 0.064(3) Uani 1 1 d . . . H32 H 1.1864 0.3924 0.6851 0.076 Uiso 1 1 calc R . . C33 C 1.0832(8) 0.4601(7) 0.7464(6) 0.044(2) Uani 1 1 d . . . H33 H 1.0331 0.4199 0.7499 0.052 Uiso 1 1 calc R . . N3 N 0.3219(5) 0.5412(6) 0.3305(4) 0.0317(16) Uani 1 1 d . . . C34 C 0.4199(6) 0.5463(6) 0.3165(5) 0.0286(17) Uani 1 1 d . . . H34 H 0.4532 0.5766 0.3462 0.034 Uiso 1 1 calc R . . C35 C 0.4775(6) 0.5101(6) 0.2607(5) 0.0283(17) Uani 1 1 d . . . H35 H 0.5473 0.5166 0.2515 0.034 Uiso 1 1 calc R . . C36 C 0.4280(6) 0.4643(6) 0.2194(5) 0.0266(17) Uani 1 1 d . . . C37 C 0.3253(7) 0.4603(7) 0.2314(5) 0.0311(18) Uani 1 1 d . . . H37 H 0.2901 0.4301 0.2028 0.037 Uiso 1 1 calc R . . C38 C 0.2750(7) 0.5012(8) 0.2861(5) 0.038(2) Uani 1 1 d . . . H38 H 0.2034 0.5011 0.2927 0.045 Uiso 1 1 calc R . . C39 C 0.4830(6) 0.4119(6) 0.1642(5) 0.0271(17) Uani 1 1 d . . . O5 O 0.4418(5) 0.3771(5) 0.1247(4) 0.0389(15) Uani 1 1 d . . . O6 O 0.5866(4) 0.4070(5) 0.1672(4) 0.0366(15) Uani 1 1 d . . . C40 C 0.6488(7) 0.3557(7) 0.1212(5) 0.0329(19) Uani 1 1 d . . . C41 C 0.6947(7) 0.2475(6) 0.1601(5) 0.0293(18) Uani 1 1 d . . . H41 H 0.6785 0.2067 0.2146 0.035 Uiso 1 1 calc R . . C42 C 0.7651(7) 0.2010(6) 0.1169(5) 0.0270(17) Uani 1 1 d . . . C43 C 0.7881(7) 0.2612(7) 0.0373(5) 0.0302(18) Uani 1 1 d . . . C44 C 0.7403(7) 0.3696(7) -0.0006(5) 0.036(2) Uani 1 1 d . . . H44 H 0.7559 0.4109 -0.0552 0.043 Uiso 1 1 calc R . . C45 C 0.6701(7) 0.4164(7) 0.0420(6) 0.038(2) Uani 1 1 d . . . H45 H 0.6368 0.4899 0.0167 0.046 Uiso 1 1 calc R . . C46 C 0.8668(7) 0.1955(7) 0.0027(5) 0.0345(19) Uani 1 1 d . . . C47 C 0.9053(9) 0.0918(8) 0.0790(6) 0.050(3) Uani 1 1 d . . . H47A H 0.9762 0.0877 0.1003 0.060 Uiso 1 1 calc R . . H47B H 0.9095 0.0308 0.0630 0.060 Uiso 1 1 calc R . . C48 C 0.8285(7) 0.0869(6) 0.1488(5) 0.0277(17) Uani 1 1 d . . . C49 C 0.9564(10) 0.2454(10) -0.0335(8) 0.067(2) Uani 1 1 d . . . H49A H 0.9299 0.3100 -0.0837 0.100 Uiso 1 1 calc R . . H49B H 1.0092 0.1950 -0.0483 0.100 Uiso 1 1 calc R . . H49C H 0.9881 0.2635 0.0081 0.100 Uiso 1 1 calc R . . C50 C 0.8130(11) 0.1766(11) -0.0652(8) 0.067(2) Uani 1 1 d . . . H50A H 0.7580 0.1399 -0.0416 0.100 Uiso 1 1 calc R . . H50B H 0.8644 0.1329 -0.0869 0.100 Uiso 1 1 calc R . . H50C H 0.7819 0.2449 -0.1108 0.100 Uiso 1 1 calc R . . C51 C 0.7607(7) 0.0057(6) 0.1660(5) 0.0322(19) Uani 1 1 d . . . H51A H 0.7537 -0.0108 0.1161 0.039 Uiso 1 1 calc R . . H51B H 0.6900 0.0352 0.1789 0.039 Uiso 1 1 calc R . . C52 C 0.8158(6) -0.0965(6) 0.2417(5) 0.0272(17) Uani 1 1 d . . . C53 C 0.8758(6) -0.0499(6) 0.2861(5) 0.0232(16) Uani 1 1 d . . . C54 C 0.8833(6) 0.0503(6) 0.2348(5) 0.0249(16) Uani 1 1 d . . . C55 C 0.8928(7) -0.1742(6) 0.2137(5) 0.034(2) Uani 1 1 d . . . H55A H 0.9436 -0.1384 0.1801 0.051 Uiso 1 1 calc R . . H55B H 0.8545 -0.1987 0.1801 0.051 Uiso 1 1 calc R . . H55C H 0.9297 -0.2351 0.2631 0.051 Uiso 1 1 calc R . . C56 C 0.7385(8) -0.1524(8) 0.2955(6) 0.042(2) Uani 1 1 d . . . H56A H 0.7764 -0.2131 0.3445 0.063 Uiso 1 1 calc R . . H56B H 0.6993 -0.1775 0.2627 0.063 Uiso 1 1 calc R . . H56C H 0.6897 -0.1029 0.3138 0.063 Uiso 1 1 calc R . . C57 C 0.9344(6) 0.1077(7) 0.2631(5) 0.0303(18) Uani 1 1 d . . . H57 H 0.9413 0.1761 0.2269 0.036 Uiso 1 1 calc R . . C58 C 0.9747(6) 0.0632(7) 0.3447(6) 0.0311(19) Uani 1 1 d . . . C59 C 0.9702(7) -0.0379(7) 0.3982(5) 0.036(2) Uani 1 1 d . . . H59 H 1.0001 -0.0672 0.4543 0.043 Uiso 1 1 calc R . . C60 C 0.9208(7) -0.0963(7) 0.3684(5) 0.0338(19) Uani 1 1 d . . . H60 H 0.9178 -0.1665 0.4036 0.041 Uiso 1 1 calc R . . O7 O 1.0134(5) 0.1272(5) 0.3776(5) 0.0431(17) Uani 1 1 d . . . C61 C 1.1179(7) 0.1160(7) 0.3831(5) 0.0298(18) Uani 1 1 d . . . O8 O 1.1797(5) 0.0512(6) 0.3690(5) 0.0510(19) Uani 1 1 d . . . C62 C 1.1423(6) 0.1971(6) 0.4098(5) 0.0261(16) Uani 1 1 d . . . C63 C 1.2454(7) 0.1887(7) 0.4333(6) 0.038(2) Uani 1 1 d . . . H63 H 1.3003 0.1321 0.4322 0.045 Uiso 1 1 calc R . . C64 C 1.2657(7) 0.2650(7) 0.4582(7) 0.039(2) Uani 1 1 d . . . H64 H 1.3358 0.2576 0.4763 0.047 Uiso 1 1 calc R . . N4 N 1.1934(6) 0.3486(6) 0.4585(5) 0.0354(17) Uani 1 1 d . . . C65 C 1.0962(7) 0.3556(7) 0.4353(5) 0.0319(19) Uani 1 1 d . . . H65 H 1.0438 0.4149 0.4346 0.038 Uiso 1 1 calc R . . C66 C 1.0653(6) 0.2824(6) 0.4117(5) 0.0277(17) Uani 1 1 d . . . H66 H 0.9938 0.2902 0.3972 0.033 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 0.03178(16) 0.02501(16) 0.03324(18) -0.01782(13) 0.00316(12) -0.00204(11) Cl1 0.0406(11) 0.0248(10) 0.0454(12) -0.0201(9) -0.0092(9) 0.0029(9) Cl2 0.0344(11) 0.0288(11) 0.0671(16) -0.0261(11) -0.0061(10) 0.0080(9) N1 0.035(4) 0.028(4) 0.026(4) -0.014(3) 0.000(3) -0.006(3) C1 0.031(4) 0.027(4) 0.044(5) -0.014(4) -0.002(4) -0.001(4) C2 0.035(4) 0.024(4) 0.044(5) -0.017(4) 0.000(4) 0.002(4) C3 0.033(4) 0.025(4) 0.016(4) -0.009(3) 0.004(3) -0.006(3) C4 0.033(4) 0.021(4) 0.023(4) -0.009(3) 0.004(3) -0.006(3) C5 0.034(4) 0.021(4) 0.042(5) -0.015(4) -0.001(4) -0.004(3) C6 0.036(4) 0.021(4) 0.032(4) -0.013(3) 0.010(3) 0.000(3) O1 0.041(4) 0.061(5) 0.109(7) -0.066(5) 0.018(4) -0.011(4) O2 0.032(3) 0.025(3) 0.033(3) -0.015(2) -0.003(2) 0.000(2) C7 0.037(4) 0.022(4) 0.024(4) -0.016(3) 0.003(3) -0.001(3) C8 0.042(4) 0.016(4) 0.019(4) -0.009(3) 0.002(3) 0.003(3) C9 0.051(5) 0.015(4) 0.022(4) -0.005(3) 0.007(4) -0.006(3) C10 0.037(4) 0.017(4) 0.024(4) -0.016(3) 0.012(3) -0.005(3) C11 0.030(4) 0.023(4) 0.018(4) -0.010(3) 0.005(3) -0.005(3) C12 0.033(4) 0.024(4) 0.017(4) -0.007(3) 0.006(3) -0.007(3) C13 0.045(5) 0.020(4) 0.030(4) -0.015(3) 0.007(4) -0.011(4) C14 0.045(5) 0.023(4) 0.033(5) -0.014(4) 0.001(4) -0.004(4) C15 0.037(4) 0.022(4) 0.021(4) -0.014(3) 0.007(3) -0.006(3) C16 0.055(6) 0.035(5) 0.039(5) -0.019(4) 0.014(4) -0.021(4) C17 0.064(6) 0.030(5) 0.036(5) -0.022(4) 0.013(4) -0.008(4) C18 0.039(5) 0.025(4) 0.028(4) -0.012(3) 0.004(4) 0.001(4) C19 0.031(4) 0.031(4) 0.017(4) -0.014(3) 0.005(3) -0.009(3) C20 0.035(4) 0.026(4) 0.014(4) -0.013(3) 0.001(3) -0.005(3) C21 0.027(4) 0.019(4) 0.022(4) -0.012(3) 0.000(3) -0.004(3) C22 0.047(5) 0.038(5) 0.034(5) -0.013(4) 0.014(4) -0.013(4) C23 0.069(7) 0.055(6) 0.025(5) -0.029(4) 0.009(4) -0.026(5) C24 0.037(4) 0.032(5) 0.020(4) -0.005(3) 0.000(3) -0.009(4) C25 0.025(4) 0.023(4) 0.038(5) -0.005(4) -0.005(3) 0.005(3) C26 0.021(4) 0.036(5) 0.039(5) -0.021(4) 0.009(3) -0.012(3) C27 0.035(4) 0.022(4) 0.025(4) -0.012(3) 0.006(3) -0.008(3) O3 0.031(3) 0.035(3) 0.051(4) -0.026(3) 0.012(3) -0.011(3) O4 0.039(4) 0.057(5) 0.071(5) -0.041(4) 0.013(3) -0.023(3) C28 0.033(4) 0.025(4) 0.028(4) -0.009(3) -0.003(3) -0.006(3) C29 0.030(4) 0.023(4) 0.024(4) -0.005(3) -0.004(3) -0.001(3) C30 0.037(4) 0.029(4) 0.036(5) -0.016(4) 0.005(4) -0.008(4) C31 0.035(5) 0.036(5) 0.047(5) -0.016(4) 0.011(4) -0.010(4) N2 0.066(6) 0.050(6) 0.071(7) -0.024(5) 0.032(5) -0.022(5) C32 0.084(9) 0.035(6) 0.084(9) -0.038(6) 0.039(7) -0.013(6) C33 0.056(6) 0.023(4) 0.058(6) -0.020(4) 0.018(5) -0.016(4) N3 0.035(4) 0.040(4) 0.023(3) -0.017(3) 0.010(3) -0.008(3) C34 0.036(4) 0.020(4) 0.030(4) -0.012(3) 0.000(3) -0.005(3) C35 0.023(4) 0.021(4) 0.036(5) -0.006(3) 0.001(3) -0.006(3) C36 0.035(4) 0.021(4) 0.022(4) -0.005(3) -0.003(3) -0.009(3) C37 0.037(4) 0.037(5) 0.024(4) -0.015(4) 0.000(3) -0.013(4) C38 0.039(5) 0.053(6) 0.028(4) -0.020(4) 0.001(4) -0.017(4) C39 0.036(4) 0.017(4) 0.022(4) 0.000(3) -0.002(3) -0.008(3) O5 0.050(4) 0.041(4) 0.034(3) -0.022(3) 0.002(3) -0.016(3) O6 0.030(3) 0.039(4) 0.050(4) -0.032(3) -0.001(3) 0.001(3) C40 0.036(4) 0.033(5) 0.034(5) -0.022(4) -0.003(4) 0.000(4) C41 0.042(5) 0.024(4) 0.022(4) -0.009(3) 0.000(3) -0.008(3) C42 0.040(4) 0.022(4) 0.020(4) -0.011(3) -0.001(3) -0.004(3) C43 0.044(5) 0.035(5) 0.020(4) -0.018(4) 0.001(3) -0.015(4) C44 0.052(5) 0.025(4) 0.022(4) -0.002(3) -0.004(4) -0.005(4) C45 0.052(5) 0.020(4) 0.035(5) -0.010(4) -0.009(4) 0.005(4) C46 0.048(5) 0.029(5) 0.028(4) -0.013(4) 0.007(4) -0.009(4) C47 0.069(7) 0.044(6) 0.031(5) -0.014(4) 0.021(5) -0.002(5) C48 0.042(4) 0.019(4) 0.020(4) -0.010(3) 0.001(3) 0.000(3) C49 0.083(6) 0.067(6) 0.061(5) -0.041(5) 0.014(5) -0.008(5) C50 0.083(6) 0.067(6) 0.061(5) -0.041(5) 0.014(5) -0.008(5) C51 0.039(4) 0.022(4) 0.040(5) -0.021(4) -0.012(4) 0.003(3) C52 0.037(4) 0.023(4) 0.026(4) -0.015(3) 0.000(3) -0.006(3) C53 0.031(4) 0.017(4) 0.026(4) -0.015(3) 0.000(3) 0.001(3) C54 0.029(4) 0.017(4) 0.026(4) -0.009(3) 0.004(3) 0.000(3) C55 0.050(5) 0.013(4) 0.035(5) -0.015(3) 0.004(4) 0.005(4) C56 0.052(6) 0.039(5) 0.051(6) -0.028(5) 0.010(5) -0.020(4) C57 0.033(4) 0.028(4) 0.037(5) -0.018(4) 0.010(4) -0.012(3) C58 0.029(4) 0.026(4) 0.046(5) -0.028(4) -0.007(4) 0.002(3) C59 0.037(4) 0.039(5) 0.030(4) -0.021(4) -0.010(4) 0.005(4) C60 0.044(5) 0.034(5) 0.025(4) -0.012(4) 0.002(4) -0.011(4) O7 0.030(3) 0.043(4) 0.070(5) -0.040(4) -0.006(3) -0.002(3) C61 0.037(4) 0.025(4) 0.026(4) -0.008(3) 0.007(3) -0.009(4) O8 0.035(3) 0.050(4) 0.087(6) -0.048(4) 0.022(4) -0.011(3) C62 0.030(4) 0.022(4) 0.027(4) -0.009(3) 0.009(3) -0.009(3) C63 0.031(4) 0.027(5) 0.058(6) -0.022(4) 0.009(4) -0.005(4) C64 0.029(4) 0.020(4) 0.071(7) -0.026(4) -0.006(4) 0.004(3) N4 0.036(4) 0.032(4) 0.047(5) -0.023(4) 0.004(3) -0.013(3) C65 0.034(4) 0.021(4) 0.041(5) -0.016(4) 0.001(4) 0.001(3) C66 0.031(4) 0.024(4) 0.030(4) -0.014(3) 0.004(3) -0.006(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Hg1 Cl2 2.341(2) . ? Hg1 Cl1 2.350(2) . ? Hg1 N1 2.589(7) . ? Hg1 N3 2.597(7) . ? N1 C1 1.332(10) . ? N1 C5 1.334(10) . ? C1 C2 1.370(12) . ? C1 H1 0.9500 . ? C2 C3 1.391(11) . ? C2 H2 0.9500 . ? C3 C4 1.375(10) . ? C3 C6 1.493(11) . ? C4 C5 1.385(11) . ? C4 H4 0.9500 . ? C5 H5 0.9500 . ? C6 O1 1.175(10) . ? C6 O2 1.360(10) . ? O2 C7 1.427(10) . ? C7 C8 1.369(11) . ? C7 C12 1.379(11) . ? C8 C9 1.383(12) . ? C8 H8 0.9500 . ? C9 C10 1.399(11) . ? C9 H9 0.9500 . ? C10 C11 1.380(11) . ? C10 C13 1.521(11) . ? C11 C12 1.385(11) . ? C11 C15 1.517(10) . ? C12 H12 0.9500 . ? C13 C17 1.521(12) . ? C13 C16 1.529(12) . ? C13 C14 1.561(11) . ? C14 C15 1.562(12) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C21 1.521(10) . ? C15 C18 1.548(11) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C19 1.551(11) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C22 1.518(12) . ? C19 C20 1.519(10) . ? C19 C23 1.543(11) . ? C20 C24 1.378(11) . ? C20 C21 1.387(11) . ? C21 C27 1.386(11) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 C25 1.395(12) . ? C24 H24 0.9500 . ? C25 C26 1.375(12) . ? C25 H25 0.9500 . ? C26 C27 1.374(11) . ? C26 O3 1.428(9) . ? C27 H27 0.9500 . ? O3 C28 1.343(10) . ? O4 C28 1.184(10) . ? C28 C29 1.508(12) . ? C29 C30 1.371(12) . ? C29 C33 1.376(12) . ? C30 C31 1.373(12) . ? C30 H30 0.9500 . ? C31 N2 1.319(13) . ? C31 H31 0.9500 . ? N2 C32 1.327(15) . ? C32 C33 1.386(15) . ? C32 H32 0.9500 . ? C33 H33 0.9500 . ? N3 C34 1.324(11) . ? N3 C38 1.343(11) . ? C34 C35 1.399(12) . ? C34 H34 0.9500 . ? C35 C36 1.386(11) . ? C35 H35 0.9500 . ? C36 C37 1.378(11) . ? C36 C39 1.504(12) . ? C37 C38 1.379(12) . ? C37 H37 0.9500 . ? C38 H38 0.9500 . ? C39 O5 1.183(10) . ? C39 O6 1.352(10) . ? O6 C40 1.409(10) . ? C40 C45 1.377(13) . ? C40 C41 1.392(11) . ? C41 C42 1.390(11) . ? C41 H41 0.9500 . ? C42 C43 1.387(11) . ? C42 C48 1.516(10) . ? C43 C44 1.398(12) . ? C43 C46 1.503(12) . ? C44 C45 1.382(13) . ? C44 H44 0.9500 . ? C45 H45 0.9500 . ? C46 C49 1.519(16) . ? C46 C50 1.522(15) . ? C46 C47 1.527(13) . ? C47 C48 1.559(12) . ? C47 H47A 0.9900 . ? C47 H47B 0.9900 . ? C48 C54 1.511(11) . ? C48 C51 1.547(12) . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C49 H49C 0.9800 . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? C51 C52 1.554(11) . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? C52 C53 1.515(11) . ? C52 C56 1.519(13) . ? C52 C55 1.533(11) . ? C53 C54 1.373(11) . ? C53 C60 1.395(11) . ? C54 C57 1.384(11) . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? C57 C58 1.367(12) . ? C57 H57 0.9500 . ? C58 C59 1.382(13) . ? C58 O7 1.419(10) . ? C59 C60 1.397(12) . ? C59 H59 0.9500 . ? C60 H60 0.9500 . ? O7 C61 1.349(10) . ? C61 O8 1.174(10) . ? C61 C62 1.485(12) . ? C62 C63 1.390(12) . ? C62 C66 1.394(11) . ? C63 C64 1.381(12) . ? C63 H63 0.9500 . ? C64 N4 1.334(10) . ? C64 H64 0.9500 . ? N4 C65 1.318(11) . ? C65 C66 1.384(12) . ? C65 H65 0.9500 . ? C66 H66 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 Cl2 Hg1 Cl1 167.49(9) . . ? Cl2 Hg1 N1 92.31(16) . . ? Cl1 Hg1 N1 92.06(16) . . ? Cl2 Hg1 N3 95.17(17) . . ? Cl1 Hg1 N3 95.04(17) . . ? N1 Hg1 N3 104.7(2) . . ? C1 N1 C5 117.1(7) . . ? C1 N1 Hg1 125.6(6) . . ? C5 N1 Hg1 116.9(5) . . ? N1 C1 C2 123.6(8) . . ? N1 C1 H1 118.2 . . ? C2 C1 H1 118.2 . . ? C1 C2 C3 118.5(8) . . ? C1 C2 H2 120.8 . . ? C3 C2 H2 120.8 . . ? C4 C3 C2 119.0(8) . . ? C4 C3 C6 122.3(7) . . ? C2 C3 C6 118.7(7) . . ? C3 C4 C5 117.9(8) . . ? C3 C4 H4 121.0 . . ? C5 C4 H4 121.0 . . ? N1 C5 C4 123.8(8) . . ? N1 C5 H5 118.1 . . ? C4 C5 H5 118.1 . . ? O1 C6 O2 123.9(8) . . ? O1 C6 C3 125.3(8) . . ? O2 C6 C3 110.8(6) . . ? C6 O2 C7 117.7(6) . . ? C8 C7 C12 123.8(8) . . ? C8 C7 O2 119.3(7) . . ? C12 C7 O2 116.7(7) . . ? C7 C8 C9 118.3(7) . . ? C7 C8 H8 120.9 . . ? C9 C8 H8 120.9 . . ? C8 C9 C10 119.9(7) . . ? C8 C9 H9 120.0 . . ? C10 C9 H9 120.0 . . ? C11 C10 C9 119.6(7) . . ? C11 C10 C13 112.4(7) . . ? C9 C10 C13 127.9(7) . . ? C10 C11 C12 121.4(7) . . ? C10 C11 C15 112.2(7) . . ? C12 C11 C15 126.4(7) . . ? C7 C12 C11 116.9(7) . . ? C7 C12 H12 121.5 . . ? C11 C12 H12 121.5 . . ? C17 C13 C10 109.7(7) . . ? C17 C13 C16 110.2(7) . . ? C10 C13 C16 112.8(7) . . ? C17 C13 C14 111.9(7) . . ? C10 C13 C14 100.9(6) . . ? C16 C13 C14 111.0(8) . . ? C13 C14 C15 108.4(7) . . ? C13 C14 H14A 110.0 . . ? C15 C14 H14A 110.0 . . ? C13 C14 H14B 110.0 . . ? C15 C14 H14B 110.0 . . ? H14A C14 H14B 108.4 . . ? C11 C15 C21 115.1(6) . . ? C11 C15 C18 112.0(7) . . ? C21 C15 C18 101.5(6) . . ? C11 C15 C14 101.2(6) . . ? C21 C15 C14 112.0(7) . . ? C18 C15 C14 115.7(7) . . ? C13 C16 H16A 109.5 . . ? C13 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C13 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C13 C17 H17A 109.5 . . ? C13 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C13 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C15 C18 C19 108.7(6) . . ? C15 C18 H18A 110.0 . . ? C19 C18 H18A 110.0 . . ? C15 C18 H18B 110.0 . . ? C19 C18 H18B 110.0 . . ? H18A C18 H18B 108.3 . . ? C22 C19 C20 113.1(7) . . ? C22 C19 C23 110.7(7) . . ? C20 C19 C23 108.0(7) . . ? C22 C19 C18 111.9(7) . . ? C20 C19 C18 101.5(6) . . ? C23 C19 C18 111.1(7) . . ? C24 C20 C21 119.8(7) . . ? C24 C20 C19 128.5(7) . . ? C21 C20 C19 111.7(7) . . ? C27 C21 C20 120.9(7) . . ? C27 C21 C15 127.0(7) . . ? C20 C21 C15 112.0(7) . . ? C19 C22 H22A 109.5 . . ? C19 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C19 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C19 C23 H23A 109.5 . . ? C19 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C19 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C20 C24 C25 120.4(8) . . ? C20 C24 H24 119.8 . . ? C25 C24 H24 119.8 . . ? C26 C25 C24 117.8(7) . . ? C26 C25 H25 121.1 . . ? C24 C25 H25 121.1 . . ? C27 C26 C25 123.4(7) . . ? C27 C26 O3 117.0(7) . . ? C25 C26 O3 119.4(7) . . ? C26 C27 C21 117.6(7) . . ? C26 C27 H27 121.2 . . ? C21 C27 H27 121.2 . . ? C28 O3 C26 117.7(7) . . ? O4 C28 O3 124.3(8) . . ? O4 C28 C29 124.5(8) . . ? O3 C28 C29 111.1(7) . . ? C30 C29 C33 119.6(8) . . ? C30 C29 C28 122.1(8) . . ? C33 C29 C28 118.2(8) . . ? C29 C30 C31 119.1(9) . . ? C29 C30 H30 120.5 . . ? C31 C30 H30 120.5 . . ? N2 C31 C30 123.2(9) . . ? N2 C31 H31 118.4 . . ? C30 C31 H31 118.4 . . ? C31 N2 C32 116.6(9) . . ? N2 C32 C33 125.2(10) . . ? N2 C32 H32 117.4 . . ? C33 C32 H32 117.4 . . ? C29 C33 C32 116.2(10) . . ? C29 C33 H33 121.9 . . ? C32 C33 H33 121.9 . . ? C34 N3 C38 117.1(7) . . ? C34 N3 Hg1 124.1(5) . . ? C38 N3 Hg1 112.9(6) . . ? N3 C34 C35 124.2(8) . . ? N3 C34 H34 117.9 . . ? C35 C34 H34 117.9 . . ? C36 C35 C34 116.8(7) . . ? C36 C35 H35 121.6 . . ? C34 C35 H35 121.6 . . ? C37 C36 C35 120.0(8) . . ? C37 C36 C39 116.9(7) . . ? C35 C36 C39 123.0(7) . . ? C36 C37 C38 118.2(8) . . ? C36 C37 H37 120.9 . . ? C38 C37 H37 120.9 . . ? N3 C38 C37 123.5(8) . . ? N3 C38 H38 118.3 . . ? C37 C38 H38 118.3 . . ? O5 C39 O6 123.9(8) . . ? O5 C39 C36 124.7(8) . . ? O6 C39 C36 111.4(7) . . ? C39 O6 C40 117.6(7) . . ? C45 C40 C41 122.2(8) . . ? C45 C40 O6 118.6(8) . . ? C41 C40 O6 119.0(8) . . ? C42 C41 C40 117.9(8) . . ? C42 C41 H41 121.0 . . ? C40 C41 H41 121.0 . . ? C43 C42 C41 120.6(8) . . ? C43 C42 C48 112.4(7) . . ? C41 C42 C48 126.9(7) . . ? C42 C43 C44 120.2(8) . . ? C42 C43 C46 111.7(7) . . ? C44 C43 C46 128.1(8) . . ? C45 C44 C43 119.5(8) . . ? C45 C44 H44 120.2 . . ? C43 C44 H44 120.2 . . ? C40 C45 C44 119.5(8) . . ? C40 C45 H45 120.2 . . ? C44 C45 H45 120.2 . . ? C43 C46 C49 113.5(8) . . ? C43 C46 C50 109.8(8) . . ? C49 C46 C50 108.6(9) . . ? C43 C46 C47 102.7(7) . . ? C49 C46 C47 111.3(9) . . ? C50 C46 C47 110.7(9) . . ? C46 C47 C48 109.6(8) . . ? C46 C47 H47A 109.8 . . ? C48 C47 H47A 109.8 . . ? C46 C47 H47B 109.8 . . ? C48 C47 H47B 109.8 . . ? H47A C47 H47B 108.2 . . ? C54 C48 C42 112.7(6) . . ? C54 C48 C51 100.6(6) . . ? C42 C48 C51 113.4(7) . . ? C54 C48 C47 113.3(7) . . ? C42 C48 C47 101.2(7) . . ? C51 C48 C47 116.2(7) . . ? C46 C49 H49A 109.5 . . ? C46 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C46 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? C46 C50 H50A 109.5 . . ? C46 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C46 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C48 C51 C52 107.8(6) . . ? C48 C51 H51A 110.2 . . ? C52 C51 H51A 110.2 . . ? C48 C51 H51B 110.2 . . ? C52 C51 H51B 110.2 . . ? H51A C51 H51B 108.5 . . ? C53 C52 C56 113.0(7) . . ? C53 C52 C55 109.5(7) . . ? C56 C52 C55 109.6(7) . . ? C53 C52 C51 100.3(6) . . ? C56 C52 C51 112.4(7) . . ? C55 C52 C51 111.7(7) . . ? C54 C53 C60 120.2(7) . . ? C54 C53 C52 111.8(7) . . ? C60 C53 C52 128.1(7) . . ? C53 C54 C57 121.3(7) . . ? C53 C54 C48 112.1(7) . . ? C57 C54 C48 126.6(7) . . ? C52 C55 H55A 109.5 . . ? C52 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? C52 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? C52 C56 H56A 109.5 . . ? C52 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C52 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? C58 C57 C54 118.1(8) . . ? C58 C57 H57 120.9 . . ? C54 C57 H57 120.9 . . ? C57 C58 C59 122.4(8) . . ? C57 C58 O7 118.4(8) . . ? C59 C58 O7 118.9(8) . . ? C58 C59 C60 119.0(8) . . ? C58 C59 H59 120.5 . . ? C60 C59 H59 120.5 . . ? C53 C60 C59 118.9(8) . . ? C53 C60 H60 120.5 . . ? C59 C60 H60 120.5 . . ? C61 O7 C58 117.7(6) . . ? O8 C61 O7 124.7(8) . . ? O8 C61 C62 125.5(8) . . ? O7 C61 C62 109.8(7) . . ? C63 C62 C66 118.4(8) . . ? C63 C62 C61 119.3(7) . . ? C66 C62 C61 122.3(7) . . ? C64 C63 C62 117.9(8) . . ? C64 C63 H63 121.0 . . ? C62 C63 H63 121.0 . . ? N4 C64 C63 124.4(8) . . ? N4 C64 H64 117.8 . . ? C63 C64 H64 117.8 . . ? C65 N4 C64 116.6(7) . . ? N4 C65 C66 124.5(8) . . ? N4 C65 H65 117.7 . . ? C66 C65 H65 117.7 . . ? C65 C66 C62 118.0(8) . . ? C65 C66 H66 121.0 . . ? C62 C66 H66 121.0 . . ? _diffrn_measured_fraction_theta_max 0.967 _diffrn_reflns_theta_full 27.58 _diffrn_measured_fraction_theta_full 0.967 _refine_diff_density_max 1.543 _refine_diff_density_min -0.920 _refine_diff_density_rms 0.174 # Attachment '2-HgCl2.cif' data_e1570a _database_code_depnum_ccdc_archive 'CCDC 743765' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '6(C33 H30 Cl2 Hg N2 O4), 2(C H Cl3), 2(H2 O)' _chemical_formula_sum 'C200 H186 Cl18 Hg6 N12 O24' _chemical_formula_weight 4983.25 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' 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' 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' _symmetry_cell_setting Hexagonal _symmetry_space_group_name_H-M R-3c _symmetry_space_group_name_Hall '-R 3 2"c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'y, x, -z+1/2' 'x-y, -y, -z+1/2' '-x, -x+y, -z+1/2' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'y+2/3, x+1/3, -z+5/6' 'x-y+2/3, -y+1/3, -z+5/6' '-x+2/3, -x+y+1/3, -z+5/6' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' 'y+1/3, x+2/3, -z+7/6' 'x-y+1/3, -y+2/3, -z+7/6' '-x+1/3, -x+y+2/3, -z+7/6' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-y, -x, z-1/2' '-x+y, y, z-1/2' 'x, x-y, z-1/2' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-y+2/3, -x+1/3, z-1/6' '-x+y+2/3, y+1/3, z-1/6' 'x+2/3, x-y+1/3, z-1/6' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' '-y+1/3, -x+2/3, z+1/6' '-x+y+1/3, y+2/3, z+1/6' 'x+1/3, x-y+2/3, z+1/6' _cell_length_a 39.9988(10) _cell_length_b 39.9988(10) _cell_length_c 10.8667(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 15056.4(7) _cell_formula_units_Z 3 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9590 _cell_measurement_theta_min 2.44 _cell_measurement_theta_max 27.51 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.649 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 7344 _exptl_absorpt_coefficient_mu 4.878 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6412 _exptl_absorpt_correction_T_max 0.7925 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 120760 _diffrn_reflns_av_R_equivalents 0.0305 _diffrn_reflns_av_sigmaI/netI 0.0095 _diffrn_reflns_limit_h_min -50 _diffrn_reflns_limit_h_max 52 _diffrn_reflns_limit_k_min -51 _diffrn_reflns_limit_k_max 51 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.04 _diffrn_reflns_theta_max 27.54 _reflns_number_total 3864 _reflns_number_gt 3073 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _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^)+(0.0396P)^2^+8.2845P] 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 3864 _refine_ls_number_parameters 207 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0414 _refine_ls_R_factor_gt 0.0285 _refine_ls_wR_factor_ref 0.0881 _refine_ls_wR_factor_gt 0.0750 _refine_ls_goodness_of_fit_ref 1.088 _refine_ls_restrained_S_all 1.088 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Hg1 Hg 0.167302(5) 0.3333 1.0833 0.03548(9) Uani 1 2 d S . . Cl1 Cl 0.21283(3) 0.39857(3) 1.05556(10) 0.0495(2) Uani 1 1 d . . . N1 N 0.12129(9) 0.32834(8) 0.9246(3) 0.0364(6) Uani 1 1 d . . . C1 C 0.08981(11) 0.29384(10) 0.9058(3) 0.0399(8) Uani 1 1 d . . . H1 H 0.0882 0.2720 0.9464 0.048 Uiso 1 1 calc R . . C2 C 0.05974(11) 0.28827(11) 0.8311(4) 0.0447(9) Uani 1 1 d . . . H2 H 0.0379 0.2633 0.8208 0.054 Uiso 1 1 calc R . . C3 C 0.06189(11) 0.31980(11) 0.7712(4) 0.0438(9) Uani 1 1 d . . . H3 H 0.0415 0.3169 0.7192 0.053 Uiso 1 1 calc R . . C4 C 0.09450(10) 0.35586(10) 0.7886(3) 0.0342(7) Uani 1 1 d . . . C5 C 0.12347(10) 0.35888(10) 0.8657(3) 0.0328(7) Uani 1 1 d . . . H5 H 0.1457 0.3835 0.8773 0.039 Uiso 1 1 calc R . . C6 C 0.09660(10) 0.38942(10) 0.7225(3) 0.0362(7) Uani 1 1 d . . . O1 O 0.07450(9) 0.38709(8) 0.6436(3) 0.0620(9) Uani 1 1 d . . . O2 O 0.12629(7) 0.42308(6) 0.7607(2) 0.0325(5) Uani 1 1 d . . . C7 C 0.13375(9) 0.45724(9) 0.6993(3) 0.0271(6) Uani 1 1 d . . . C8 C 0.15007(9) 0.46506(9) 0.5831(3) 0.0246(6) Uani 1 1 d . . . H8 H 0.1529 0.4462 0.5385 0.029 Uiso 1 1 calc R . . C9 C 0.16212(8) 0.50141(8) 0.5341(2) 0.0213(5) Uani 1 1 d . . . C10 C 0.15776(9) 0.52871(9) 0.6005(3) 0.0247(6) Uani 1 1 d . . . C11 C 0.13960(10) 0.51935(10) 0.7148(3) 0.0312(7) Uani 1 1 d . . . H11 H 0.1356 0.5376 0.7582 0.037 Uiso 1 1 calc R . . C12 C 0.12748(10) 0.48327(10) 0.7646(3) 0.0313(7) Uani 1 1 d . . . H12 H 0.1150 0.4765 0.8425 0.038 Uiso 1 1 calc R . . C13 C 0.18498(10) 0.51832(10) 0.4167 0.0223(8) Uani 1 2 d S . . C14 C 0.18654(10) 0.55808(9) 0.4098(3) 0.0281(6) Uani 1 1 d . . . H14A H 0.2124 0.5784 0.3821 0.034 Uiso 1 1 calc R . . H14B H 0.1672 0.5567 0.3501 0.034 Uiso 1 1 calc R . . C15 C 0.17792(10) 0.56802(9) 0.5392(3) 0.0299(7) Uani 1 1 d . . . C16 C 0.21575(12) 0.59418(11) 0.6093(3) 0.0446(9) Uani 1 1 d . . . H16A H 0.2098 0.5967 0.6951 0.067 Uiso 1 1 calc R . . H16B H 0.2291 0.6197 0.5706 0.067 Uiso 1 1 calc R . . H16C H 0.2324 0.5827 0.6066 0.067 Uiso 1 1 calc R . . C17 C 0.15294(14) 0.58689(13) 0.5335(4) 0.0463(10) Uani 1 1 d . . . H17A H 0.1291 0.5700 0.4885 0.069 Uiso 1 1 calc R . . H17B H 0.1671 0.6118 0.4911 0.069 Uiso 1 1 calc R . . H17C H 0.1466 0.5910 0.6172 0.069 Uiso 1 1 calc R . . C18 C 0.6667 0.3333 0.0833 0.186(16) Uani 1 6 d S . . Cl2 Cl 0.69458(19) 0.37695(18) 0.0405(13) 0.232(5) Uani 0.50 1 d P . . O3 O 0.6667 0.3333 0.273(2) 0.135(8) Uani 0.50 3 d SP . . 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 0.03551(11) 0.02759(11) 0.04071(14) 0.00621(7) 0.00310(3) 0.01380(6) Cl1 0.0346(5) 0.0326(5) 0.0690(7) 0.0057(4) 0.0098(4) 0.0075(4) N1 0.0399(16) 0.0297(14) 0.0362(15) 0.0081(12) 0.0006(12) 0.0149(13) C1 0.046(2) 0.0280(17) 0.040(2) 0.0114(14) 0.0071(16) 0.0140(15) C2 0.040(2) 0.0292(18) 0.049(2) 0.0043(16) 0.0005(17) 0.0062(16) C3 0.0362(19) 0.040(2) 0.047(2) 0.0047(16) -0.0046(16) 0.0123(16) C4 0.0347(17) 0.0320(17) 0.0319(17) 0.0064(13) 0.0021(13) 0.0137(14) C5 0.0345(17) 0.0260(15) 0.0314(16) 0.0056(13) 0.0015(13) 0.0104(13) C6 0.0348(18) 0.0353(18) 0.0351(18) 0.0032(14) -0.0035(14) 0.0150(15) O1 0.0590(19) 0.0424(16) 0.072(2) 0.0077(14) -0.0311(16) 0.0157(14) O2 0.0369(12) 0.0296(11) 0.0270(11) 0.0089(9) -0.0016(9) 0.0136(10) C7 0.0294(16) 0.0299(16) 0.0232(14) 0.0051(12) -0.0029(12) 0.0158(13) C8 0.0262(15) 0.0287(15) 0.0226(14) -0.0004(11) -0.0018(11) 0.0165(13) C9 0.0245(14) 0.0267(14) 0.0163(12) 0.0002(10) -0.0020(10) 0.0154(12) C10 0.0326(15) 0.0301(15) 0.0177(13) -0.0002(11) -0.0011(11) 0.0204(13) C11 0.0429(18) 0.0428(18) 0.0202(14) -0.0002(13) 0.0026(13) 0.0308(16) C12 0.0369(17) 0.0463(19) 0.0181(14) 0.0057(13) 0.0052(12) 0.0264(16) C13 0.0258(15) 0.0258(15) 0.0173(18) 0.0000(7) 0.0000(7) 0.0143(17) C14 0.0402(18) 0.0236(14) 0.0211(14) 0.0017(11) 0.0013(12) 0.0165(13) C15 0.0467(19) 0.0291(15) 0.0213(14) -0.0008(12) 0.0018(13) 0.0245(15) C16 0.059(2) 0.0346(19) 0.0334(18) -0.0112(15) -0.0063(17) 0.0179(18) C17 0.079(3) 0.049(2) 0.0354(19) 0.0038(16) 0.0047(19) 0.050(2) C18 0.17(2) 0.17(2) 0.22(4) 0.000 0.000 0.084(11) Cl2 0.175(5) 0.089(3) 0.432(17) -0.012(6) 0.034(8) 0.066(4) O3 0.152(12) 0.152(12) 0.103(14) 0.000 0.000 0.076(6) _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 Cl1 2.3376(9) . ? Hg1 Cl1 2.3377(9) 17_556 ? Hg1 N1 2.457(3) 17_556 ? Hg1 N1 2.457(3) . ? N1 C1 1.339(5) . ? N1 C5 1.343(4) . ? C1 C2 1.374(6) . ? C1 H1 0.9500 . ? C2 C3 1.383(5) . ? C2 H2 0.9500 . ? C3 C4 1.392(5) . ? C3 H3 0.9500 . ? C4 C5 1.385(5) . ? C4 C6 1.487(5) . ? C5 H5 0.9500 . ? C6 O1 1.201(4) . ? C6 O2 1.340(4) . ? O2 C7 1.412(4) . ? C7 C12 1.382(5) . ? C7 C8 1.383(4) . ? C8 C9 1.389(4) . ? C8 H8 0.9500 . ? C9 C10 1.391(4) . ? C9 C13 1.517(3) . ? C10 C11 1.392(4) . ? C10 C15 1.516(4) . ? C11 C12 1.382(5) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C9 1.517(3) 10_455 ? C13 C14 1.562(4) 10_455 ? C13 C14 1.562(4) . ? C14 C15 1.546(4) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C17 1.525(5) . ? C15 C16 1.543(5) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 Cl2 1.600(7) 18_654 ? C18 Cl2 1.600(7) . ? C18 Cl2 1.600(7) 3_665 ? C18 Cl2 1.600(7) 16_544 ? C18 Cl2 1.600(7) 2_655 ? C18 Cl2 1.600(7) 17_554 ? Cl2 Cl2 2.146(17) 18_654 ? 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 Cl1 Hg1 Cl1 154.47(5) . 17_556 ? Cl1 Hg1 N1 100.32(7) . 17_556 ? Cl1 Hg1 N1 97.70(7) 17_556 17_556 ? Cl1 Hg1 N1 97.70(7) . . ? Cl1 Hg1 N1 100.32(7) 17_556 . ? N1 Hg1 N1 89.79(14) 17_556 . ? C1 N1 C5 117.7(3) . . ? C1 N1 Hg1 118.1(2) . . ? C5 N1 Hg1 123.7(2) . . ? N1 C1 C2 123.6(3) . . ? N1 C1 H1 118.2 . . ? C2 C1 H1 118.2 . . ? C1 C2 C3 118.7(3) . . ? C1 C2 H2 120.7 . . ? C3 C2 H2 120.7 . . ? C2 C3 C4 118.7(4) . . ? C2 C3 H3 120.7 . . ? C4 C3 H3 120.7 . . ? C5 C4 C3 118.8(3) . . ? C5 C4 C6 123.1(3) . . ? C3 C4 C6 118.1(3) . . ? N1 C5 C4 122.5(3) . . ? N1 C5 H5 118.7 . . ? C4 C5 H5 118.7 . . ? O1 C6 O2 123.2(3) . . ? O1 C6 C4 124.6(3) . . ? O2 C6 C4 112.3(3) . . ? C6 O2 C7 118.6(2) . . ? C12 C7 C8 122.7(3) . . ? C12 C7 O2 117.1(3) . . ? C8 C7 O2 119.9(3) . . ? C7 C8 C9 117.7(3) . . ? C7 C8 H8 121.2 . . ? C9 C8 H8 121.2 . . ? C8 C9 C10 120.5(3) . . ? C8 C9 C13 127.3(2) . . ? C10 C9 C13 111.8(2) . . ? C9 C10 C11 120.4(3) . . ? C9 C10 C15 112.1(2) . . ? C11 C10 C15 127.3(3) . . ? C12 C11 C10 119.6(3) . . ? C12 C11 H11 120.2 . . ? C10 C11 H11 120.2 . . ? C11 C12 C7 119.0(3) . . ? C11 C12 H12 120.5 . . ? C7 C12 H12 120.5 . . ? C9 C13 C9 116.8(3) 10_455 . ? C9 C13 C14 101.69(15) 10_455 10_455 ? C9 C13 C14 110.62(15) . 10_455 ? C9 C13 C14 110.61(15) 10_455 . ? C9 C13 C14 101.68(15) . . ? C14 C13 C14 116.1(4) 10_455 . ? C15 C14 C13 108.5(2) . . ? C15 C14 H14A 110.0 . . ? C13 C14 H14A 110.0 . . ? C15 C14 H14B 110.0 . . ? C13 C14 H14B 110.0 . . ? H14A C14 H14B 108.4 . . ? C10 C15 C17 113.0(3) . . ? C10 C15 C16 108.6(3) . . ? C17 C15 C16 110.3(3) . . ? C10 C15 C14 101.8(2) . . ? C17 C15 C14 112.1(3) . . ? C16 C15 C14 110.7(3) . . ? 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 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? Cl2 C18 Cl2 84.3(5) 18_654 . ? Cl2 C18 Cl2 162.4(4) 18_654 3_665 ? Cl2 C18 Cl2 111.9(4) . 3_665 ? Cl2 C18 Cl2 111.9(4) 18_654 16_544 ? Cl2 C18 Cl2 53.2(7) . 16_544 ? Cl2 C18 Cl2 84.2(5) 3_665 16_544 ? Cl2 C18 Cl2 53.2(7) 18_654 2_655 ? Cl2 C18 Cl2 111.9(4) . 2_655 ? Cl2 C18 Cl2 111.9(4) 3_665 2_655 ? Cl2 C18 Cl2 162.5(4) 16_544 2_655 ? Cl2 C18 Cl2 111.9(4) 18_654 17_554 ? Cl2 C18 Cl2 162.4(4) . 17_554 ? Cl2 C18 Cl2 53.2(7) 3_665 17_554 ? Cl2 C18 Cl2 111.9(4) 16_544 17_554 ? Cl2 C18 Cl2 84.3(5) 2_655 17_554 ? Cl2 Cl2 C18 63.4(3) 16_544 . ? Cl2 Cl2 Cl2 93.5(10) 16_544 18_654 ? C18 Cl2 Cl2 47.9(3) . 18_654 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.54 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 2.182 _refine_diff_density_min -0.931 _refine_diff_density_rms 0.096