# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_1b/Hg(OTf)2 _database_code_depnum_ccdc_archive 'CCDC 910366' #TrackingRef '15353_web_deposit_cif_file_0_YoichiHabata_1352699762.All_complexes_1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H37 F6 Hg N3 O6 S2' _chemical_formula_weight 986.40 _chemical_absolute_configuration syn loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Hg Hg -2.3894 9.2266 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' _cell_length_a 25.096(2) _cell_length_b 10.4441(8) _cell_length_c 18.8981(13) _cell_angle_alpha 90.00 _cell_angle_beta 126.654(4) _cell_angle_gamma 90.00 _cell_volume 3973.8(5) _cell_formula_units_Z 4 _cell_measurement_temperature 223 _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.39 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.649 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1952 _exptl_absorpt_coefficient_mu 4.053 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.3037 _exptl_absorpt_correction_T_max 0.4367 _exptl_absorpt_process_details 'SADABS; Sheldrick, 1996' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223 _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 8.366 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13905 _diffrn_reflns_av_R_equivalents 0.0290 _diffrn_reflns_av_sigmaI/netI 0.0685 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.02 _diffrn_reflns_theta_max 27.48 _reflns_number_total 8778 _reflns_number_gt 7271 _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^+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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.007(9) _refine_ls_number_reflns 8778 _refine_ls_number_parameters 496 _refine_ls_number_restraints 220 _refine_ls_R_factor_all 0.0552 _refine_ls_R_factor_gt 0.0451 _refine_ls_wR_factor_ref 0.1108 _refine_ls_wR_factor_gt 0.1069 _refine_ls_goodness_of_fit_ref 0.983 _refine_ls_restrained_S_all 1.027 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.5331(4) 0.2080(9) 0.8111(6) 0.053(2) Uani 1 1 d . . . H1A H 0.5362 0.2307 0.8637 0.063 Uiso 1 1 calc R . . H1B H 0.5548 0.1247 0.8221 0.063 Uiso 1 1 calc R . . C2 C 0.4608(4) 0.1948(7) 0.7342(5) 0.0383(17) Uani 1 1 d . . . C3 C 0.4418(4) 0.1889(9) 0.6483(5) 0.050(2) Uani 1 1 d . . . H3 H 0.4739 0.1991 0.6380 0.060 Uiso 1 1 calc R . . C4 C 0.3777(4) 0.1687(8) 0.5798(5) 0.0470(19) Uani 1 1 d . . . H4 H 0.3661 0.1612 0.5226 0.056 Uiso 1 1 calc R . . C5 C 0.3474(4) 0.1653(8) 0.6752(5) 0.0460(19) Uani 1 1 d . . . H5 H 0.3149 0.1569 0.6847 0.055 Uiso 1 1 calc R . . C6 C 0.4119(4) 0.1836(8) 0.7442(5) 0.0456(19) Uani 1 1 d . . . H6 H 0.4231 0.1886 0.8013 0.055 Uiso 1 1 calc R . . C7 C 0.5590(4) 0.4308(8) 0.8173(6) 0.047(2) Uani 1 1 d . . . H7A H 0.5925 0.4880 0.8235 0.057 Uiso 1 1 calc R . . H7B H 0.5655 0.4297 0.8738 0.057 Uiso 1 1 calc R . . C8 C 0.4916(4) 0.4840(8) 0.7482(5) 0.0434(18) Uani 1 1 d . . . C9 C 0.4714(4) 0.5010(10) 0.6633(6) 0.055(2) Uani 1 1 d . . . H9 H 0.5012 0.4849 0.6498 0.066 Uiso 1 1 calc R . . C10 C 0.4081(4) 0.5410(8) 0.5982(5) 0.0456(19) Uani 1 1 d . . . H10 H 0.3952 0.5517 0.5405 0.055 Uiso 1 1 calc R . . C11 C 0.3820(4) 0.5509(9) 0.6963(6) 0.053(2) Uani 1 1 d . . . H11 H 0.3511 0.5653 0.7082 0.063 Uiso 1 1 calc R . . C12 C 0.4472(4) 0.5140(9) 0.7641(5) 0.054(2) Uani 1 1 d . . . H12 H 0.4604 0.5101 0.8222 0.065 Uiso 1 1 calc R . . C13 C 0.6410(4) 0.2676(9) 0.8448(6) 0.052(2) Uani 1 1 d . . . H13 H 0.6630 0.3435 0.8412 0.063 Uiso 1 1 calc R . . C14 C 0.6462(6) 0.1645(11) 0.7957(7) 0.071(3) Uani 1 1 d . . . H14A H 0.6216 0.0901 0.7925 0.106 Uiso 1 1 calc R . . H14B H 0.6925 0.1417 0.8259 0.106 Uiso 1 1 calc R . . H14C H 0.6278 0.1938 0.7365 0.106 Uiso 1 1 calc R . . C15 C 0.6770(4) 0.2405(9) 0.9426(6) 0.055(2) Uani 1 1 d . . . C16 C 0.6820(3) 0.1144(16) 0.9729(6) 0.061(2) Uani 1 1 d . . . H16 H 0.6648 0.0455 0.9331 0.074 Uiso 1 1 calc R . . C17 C 0.7123(4) 0.0927(14) 1.0612(7) 0.076(4) Uani 1 1 d . . . H17 H 0.7150 0.0088 1.0812 0.091 Uiso 1 1 calc R . . C18 C 0.7382(5) 0.1915(13) 1.1199(8) 0.081(3) Uani 1 1 d . . . H18 H 0.7590 0.1759 1.1800 0.098 Uiso 1 1 calc R . . C19 C 0.7339(5) 0.3138(12) 1.0907(7) 0.074(3) Uani 1 1 d . . . H19 H 0.7524 0.3819 1.1312 0.089 Uiso 1 1 calc R . . C20 C 0.7026(4) 0.3376(10) 1.0028(6) 0.057(2) Uani 1 1 d . . . H20 H 0.6988 0.4224 0.9837 0.069 Uiso 1 1 calc R . . C41 C 0.2097(9) 0.3617(16) 0.2480(8) 0.078(4) Uani 1 1 d . . . C42 C 0.2964(14) -0.107(2) 0.3337(18) 0.159(8) Uani 1 1 d U . . C1B C 0.4948(6) 0.8523(12) 0.8218(12) 0.114(5) Uani 1 1 d DU . . H1B1 H 0.4554 0.8815 0.8118 0.137 Uiso 1 1 calc R . . C2B C 0.5467(9) 0.8159(12) 0.9038(11) 0.239(14) Uani 1 1 d DU . . C3B C 0.6040(7) 0.7743(14) 0.9191(11) 0.178(9) Uani 1 1 d DU . . H3B H 0.6402 0.7487 0.9758 0.214 Uiso 1 1 calc R . . C4B C 0.6079(7) 0.7705(14) 0.8501(15) 0.137(6) Uani 1 1 d DU . . H4B H 0.6473 0.7417 0.8597 0.164 Uiso 1 1 calc R . . C5B C 0.5558(11) 0.808(2) 0.7673(13) 0.248(15) Uani 1 1 d DU . . H5B H 0.5592 0.8061 0.7204 0.298 Uiso 1 1 calc R . . C6B C 0.4994(9) 0.8468(17) 0.7542(10) 0.217(12) Uani 1 1 d DU . . H6B H 0.4628 0.8707 0.6973 0.260 Uiso 1 1 calc R . . C1A C 0.5000 0.567(3) 0.5000 0.135(9) Uani 1 2 d SDU . . C2A C 0.4429(8) 0.4812(14) 0.4510(8) 0.117(5) Uani 1 1 d DU . . H2A H 0.4013 0.5220 0.4153 0.140 Uiso 1 1 calc R . . C3A C 0.4408(9) 0.3422(15) 0.4493(9) 0.126(5) Uani 1 1 d DU . . H3A H 0.3990 0.3021 0.4136 0.152 Uiso 1 1 calc R . . C4A C 0.5000 0.261(3) 0.5000 0.133(8) Uani 1 2 d SDU . . F1 F 0.1748(6) 0.4679(11) 0.2081(5) 0.143(4) Uani 1 1 d . . . F2 F 0.1678(6) 0.2632(11) 0.1962(5) 0.149(4) Uani 1 1 d . . . F3 F 0.2589(7) 0.3555(12) 0.2439(7) 0.153(5) Uani 1 1 d . . . F4 F 0.3466(7) -0.1504(12) 0.3257(8) 0.167(4) Uani 1 1 d U . . F5 F 0.2973(10) 0.0207(16) 0.3133(10) 0.212(6) Uani 1 1 d U . . F6 F 0.2374(9) -0.151(2) 0.2742(11) 0.183(7) Uani 1 1 d U . . Hg1 Hg 0.232763(11) 0.11339(14) 0.488432(16) 0.04158(9) Uani 1 1 d . . . N1 N 0.5696(3) 0.3037(7) 0.7987(4) 0.0413(15) Uani 1 1 d . . . N2 N 0.3301(3) 0.1592(6) 0.5912(4) 0.0441(16) Uani 1 1 d . . . N3 N 0.3645(3) 0.5652(6) 0.6151(4) 0.0426(15) Uani 1 1 d . . . O1 O 0.2585(5) 0.2268(7) 0.3844(5) 0.077(2) Uani 1 1 d . . . O2 O 0.2742(3) 0.4528(7) 0.4013(5) 0.069(2) Uani 1 1 d . . . O3 O 0.1670(4) 0.3616(8) 0.3433(6) 0.090(3) Uani 1 1 d . . . O4 O 0.2682(5) -0.0728(8) 0.4360(6) 0.090(2) Uani 1 1 d U . . O5 O 0.3151(4) -0.2678(7) 0.4353(6) 0.077(2) Uani 1 1 d U . . O6 O 0.3862(9) -0.0693(14) 0.4907(11) 0.183(6) Uani 1 1 d U . . S1 S 0.23086(13) 0.3495(2) 0.35676(14) 0.0526(6) Uani 1 1 d . . . S2 S 0.31049(19) -0.1346(3) 0.4250(3) 0.0870(10) Uani 1 1 d U . . C7B C 0.5417(16) 0.822(3) 0.9753(16) 0.44(3) Uani 1 1 d DU . . C3C C 0.0590(5) 0.7895(12) 0.0383(6) 0.110(5) Uani 1 1 d DU . . H3C H 0.0988 0.7437 0.0641 0.132 Uiso 1 1 calc R . . C5C C 0.0000 0.5894(19) 0.0000 0.170(11) Uani 1 2 d SDU . . C2C C 0.0586(6) 0.9202(13) 0.0382(7) 0.150(7) Uani 1 1 d DU . . H2C H 0.0984 0.9661 0.0643 0.180 Uiso 1 1 calc R . . C4C C 0.0000 0.7270(17) 0.0000 0.120(7) Uani 1 2 d SDU . . C1C C 0.0000 0.984(3) 0.0000 0.203(15) Uani 1 2 d SDU . . C5A1 C 0.5000 0.122(3) 0.5000 0.18(3) Uani 0.40 2 d SPDU . . C5A2 C 0.5000 0.706(3) 0.5000 0.126(15) Uani 0.60 2 d SPDU . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.034(4) 0.061(6) 0.046(5) 0.009(4) 0.015(4) -0.010(4) C2 0.036(4) 0.034(4) 0.035(4) -0.003(3) 0.015(3) -0.008(3) C3 0.041(4) 0.064(6) 0.044(5) -0.001(4) 0.025(4) -0.010(4) C4 0.045(4) 0.058(5) 0.038(4) -0.001(4) 0.025(4) -0.011(4) C5 0.054(5) 0.048(4) 0.044(5) -0.006(3) 0.034(4) -0.007(4) C6 0.049(4) 0.051(5) 0.036(4) 0.001(4) 0.025(4) -0.005(4) C7 0.053(5) 0.036(4) 0.043(5) 0.007(3) 0.023(4) 0.018(4) C8 0.040(4) 0.032(4) 0.043(5) 0.000(3) 0.016(4) 0.006(3) C9 0.039(4) 0.064(6) 0.056(6) 0.013(5) 0.025(4) 0.009(4) C10 0.044(4) 0.057(5) 0.036(4) 0.008(4) 0.023(4) 0.007(4) C11 0.052(5) 0.063(5) 0.041(5) 0.003(4) 0.027(4) 0.013(4) C12 0.057(5) 0.059(6) 0.029(4) 0.006(4) 0.016(4) 0.016(4) C13 0.040(4) 0.054(5) 0.060(5) 0.008(4) 0.028(4) 0.004(4) C14 0.079(7) 0.068(7) 0.073(7) 0.007(5) 0.050(6) 0.018(5) C15 0.026(3) 0.054(5) 0.066(6) 0.017(5) 0.017(4) 0.004(3) C16 0.047(4) 0.050(4) 0.073(5) 0.018(8) 0.027(4) 0.012(7) C17 0.047(4) 0.076(10) 0.078(7) 0.028(7) 0.022(5) 0.017(6) C18 0.052(6) 0.086(9) 0.067(7) 0.019(7) 0.014(5) 0.003(6) C19 0.050(5) 0.080(8) 0.056(6) -0.001(5) 0.012(5) -0.013(5) C20 0.033(4) 0.057(6) 0.058(6) 0.003(5) 0.015(4) -0.003(4) C41 0.112(12) 0.084(8) 0.054(7) 0.021(7) 0.059(9) 0.028(8) C42 0.162(9) 0.148(10) 0.162(10) 0.000(6) 0.093(7) -0.002(6) C1B 0.093(7) 0.100(8) 0.145(9) -0.005(7) 0.069(7) -0.009(6) C2B 0.237(16) 0.224(17) 0.258(17) -0.005(10) 0.149(12) -0.010(10) C3B 0.167(12) 0.125(11) 0.202(13) 0.009(9) 0.087(9) -0.022(9) C4B 0.127(9) 0.099(9) 0.171(11) -0.014(8) 0.081(8) -0.023(7) C5B 0.239(17) 0.213(18) 0.269(18) -0.012(10) 0.139(12) -0.017(10) C6B 0.209(15) 0.169(15) 0.237(15) -0.006(10) 0.115(11) -0.017(10) C1A 0.155(12) 0.164(14) 0.123(11) 0.000 0.103(10) 0.000 C2A 0.132(9) 0.165(10) 0.093(8) 0.001(7) 0.088(7) 0.009(7) C3A 0.138(9) 0.164(11) 0.105(8) -0.016(7) 0.087(8) 0.005(8) C4A 0.149(12) 0.162(13) 0.126(11) 0.000 0.102(10) 0.000 F1 0.179(9) 0.161(9) 0.072(5) 0.059(6) 0.065(6) 0.078(8) F2 0.179(9) 0.173(10) 0.052(4) -0.046(5) 0.046(5) -0.039(8) F3 0.223(13) 0.175(10) 0.151(9) 0.034(8) 0.160(10) 0.065(10) F4 0.223(9) 0.203(9) 0.168(7) -0.013(6) 0.166(7) 0.007(7) F5 0.298(11) 0.222(11) 0.183(8) 0.019(7) 0.179(8) 0.010(8) F6 0.161(10) 0.205(11) 0.188(10) 0.012(8) 0.107(8) 0.009(8) Hg1 0.03633(13) 0.03746(14) 0.03906(14) -0.0045(2) 0.01610(10) -0.0074(2) N1 0.035(3) 0.042(4) 0.038(3) 0.008(3) 0.017(3) -0.001(3) N2 0.036(3) 0.050(4) 0.039(3) -0.010(3) 0.018(3) -0.014(3) N3 0.037(3) 0.040(3) 0.036(4) 0.004(3) 0.014(3) 0.002(3) O1 0.115(6) 0.052(4) 0.058(4) 0.008(3) 0.048(5) 0.013(4) O2 0.058(4) 0.050(4) 0.084(5) -0.027(4) 0.035(4) -0.018(3) O3 0.095(6) 0.089(6) 0.114(7) -0.033(5) 0.077(6) -0.026(5) O4 0.131(6) 0.074(5) 0.088(5) 0.000(4) 0.077(5) 0.012(4) O5 0.089(5) 0.051(4) 0.108(5) 0.022(4) 0.068(5) 0.010(4) O6 0.203(10) 0.126(8) 0.169(9) -0.007(7) 0.084(7) -0.041(7) S1 0.0748(15) 0.0367(11) 0.0382(11) -0.0010(9) 0.0293(12) -0.0048(10) S2 0.112(2) 0.0522(15) 0.147(3) 0.0223(17) 0.104(2) 0.0121(15) C7B 0.43(4) 0.42(4) 0.44(4) 0.012(11) 0.25(2) -0.011(11) C3C 0.121(8) 0.159(10) 0.072(7) 0.002(6) 0.070(7) -0.008(7) C5C 0.210(14) 0.164(15) 0.142(13) 0.000 0.109(10) 0.000 C2C 0.174(11) 0.190(13) 0.126(10) 0.008(8) 0.112(9) 0.002(8) C4C 0.151(12) 0.123(12) 0.092(10) 0.000 0.076(9) 0.000 C1C 0.225(18) 0.223(19) 0.185(18) 0.000 0.136(13) 0.000 C5A1 0.18(3) 0.19(3) 0.18(3) 0.000 0.110(18) 0.000 C5A2 0.133(17) 0.131(18) 0.128(17) 0.000 0.084(12) 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.467(10) . ? C1 C2 1.509(11) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C2 C6 1.352(11) . ? C2 C3 1.395(11) . ? C3 C4 1.351(12) . ? C3 H3 0.9400 . ? C4 N2 1.336(10) . ? C4 H4 0.9400 . ? C5 C6 1.354(12) . ? C5 N2 1.376(10) . ? C5 H5 0.9400 . ? C6 H6 0.9400 . ? C7 N1 1.437(10) . ? C7 C8 1.495(11) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C8 C12 1.353(12) . ? C8 C9 1.376(12) . ? C9 C10 1.369(12) . ? C9 H9 0.9400 . ? C10 N3 1.335(10) . ? C10 H10 0.9400 . ? C11 N3 1.330(11) . ? C11 C12 1.401(12) . ? C11 H11 0.9400 . ? C12 H12 0.9400 . ? C13 C14 1.476(14) . ? C13 N1 1.499(10) . ? C13 C15 1.523(13) . ? C13 H13 0.9900 . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C14 H14C 0.9700 . ? C15 C20 1.365(13) . ? C15 C16 1.412(17) . ? C16 C17 1.378(13) . ? C16 H16 0.9400 . ? C17 C18 1.363(17) . ? C17 H17 0.9400 . ? C18 C19 1.369(16) . ? C18 H18 0.9400 . ? C19 C20 1.371(14) . ? C19 H19 0.9400 . ? C20 H20 0.9400 . ? C41 F3 1.284(19) . ? C41 F1 1.333(16) . ? C41 F2 1.38(2) . ? C41 S1 1.795(10) . ? C42 F6 1.30(3) . ? C42 F5 1.40(3) . ? C42 F4 1.43(3) . ? C42 S2 1.57(3) . ? C1B C6B 1.351(9) . ? C1B C2B 1.354(9) . ? C1B H1B1 0.9400 . ? C2B C3B 1.359(9) . ? C2B C7B 1.430(11) . ? C3B C4B 1.364(9) . ? C3B H3B 0.9400 . ? C4B C5B 1.367(10) . ? C4B H4B 0.9400 . ? C5B C6B 1.344(10) . ? C5B H5B 0.9400 . ? C6B H6B 0.9400 . ? C1A C5A2 1.451(11) . ? C1A C2A 1.459(12) . ? C1A C2A 1.459(12) 2_656 ? C2A C3A 1.452(12) . ? C2A H2A 0.9400 . ? C3A C4A 1.466(12) . ? C3A H3A 0.9400 . ? C4A C5A1 1.454(11) . ? C4A C3A 1.466(12) 2_656 ? Hg1 N2 2.075(6) . ? Hg1 N3 2.082(6) 4_546 ? Hg1 O4 2.569(8) . ? N3 Hg1 2.082(6) 4_556 ? O1 S1 1.401(7) . ? O2 S1 1.401(7) . ? O3 S1 1.469(8) . ? O4 S2 1.361(9) . ? O5 S2 1.400(8) . ? O6 S2 1.674(17) . ? C3C C4C 1.364(7) . ? C3C C2C 1.366(7) . ? C3C H3C 0.9400 . ? C5C C4C 1.437(10) . ? C2C C1C 1.361(7) . ? C2C H2C 0.9400 . ? C4C C3C 1.364(7) 2 ? C1C C2C 1.361(7) 2 ? 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 N1 C1 C2 114.6(7) . . ? N1 C1 H1A 108.6 . . ? C2 C1 H1A 108.6 . . ? N1 C1 H1B 108.6 . . ? C2 C1 H1B 108.6 . . ? H1A C1 H1B 107.6 . . ? C6 C2 C3 116.8(7) . . ? C6 C2 C1 123.0(7) . . ? C3 C2 C1 120.2(7) . . ? C4 C3 C2 120.3(8) . . ? C4 C3 H3 119.8 . . ? C2 C3 H3 119.8 . . ? N2 C4 C3 121.7(8) . . ? N2 C4 H4 119.1 . . ? C3 C4 H4 119.1 . . ? C6 C5 N2 119.3(7) . . ? C6 C5 H5 120.3 . . ? N2 C5 H5 120.3 . . ? C2 C6 C5 122.7(7) . . ? C2 C6 H6 118.7 . . ? C5 C6 H6 118.7 . . ? N1 C7 C8 114.1(7) . . ? N1 C7 H7A 108.7 . . ? C8 C7 H7A 108.7 . . ? N1 C7 H7B 108.7 . . ? C8 C7 H7B 108.7 . . ? H7A C7 H7B 107.6 . . ? C12 C8 C9 116.7(7) . . ? C12 C8 C7 123.1(8) . . ? C9 C8 C7 120.2(8) . . ? C10 C9 C8 120.7(8) . . ? C10 C9 H9 119.7 . . ? C8 C9 H9 119.7 . . ? N3 C10 C9 121.3(8) . . ? N3 C10 H10 119.3 . . ? C9 C10 H10 119.3 . . ? N3 C11 C12 119.2(8) . . ? N3 C11 H11 120.4 . . ? C12 C11 H11 120.4 . . ? C8 C12 C11 121.9(8) . . ? C8 C12 H12 119.1 . . ? C11 C12 H12 119.1 . . ? C14 C13 N1 109.9(8) . . ? C14 C13 C15 114.5(8) . . ? N1 C13 C15 112.9(7) . . ? C14 C13 H13 106.3 . . ? N1 C13 H13 106.3 . . ? C15 C13 H13 106.3 . . ? 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 . . ? C20 C15 C16 118.1(9) . . ? C20 C15 C13 121.1(8) . . ? C16 C15 C13 120.7(9) . . ? C17 C16 C15 119.8(14) . . ? C17 C16 H16 120.1 . . ? C15 C16 H16 120.1 . . ? C18 C17 C16 120.7(14) . . ? C18 C17 H17 119.7 . . ? C16 C17 H17 119.7 . . ? C17 C18 C19 119.6(12) . . ? C17 C18 H18 120.2 . . ? C19 C18 H18 120.2 . . ? C18 C19 C20 120.5(11) . . ? C18 C19 H19 119.8 . . ? C20 C19 H19 119.8 . . ? C15 C20 C19 121.3(10) . . ? C15 C20 H20 119.3 . . ? C19 C20 H20 119.3 . . ? F3 C41 F1 109.8(12) . . ? F3 C41 F2 105.8(12) . . ? F1 C41 F2 104.8(13) . . ? F3 C41 S1 115.2(12) . . ? F1 C41 S1 110.6(9) . . ? F2 C41 S1 109.9(10) . . ? F6 C42 F5 107(2) . . ? F6 C42 F4 115(2) . . ? F5 C42 F4 96(2) . . ? F6 C42 S2 106(2) . . ? F5 C42 S2 116.6(18) . . ? F4 C42 S2 115.2(19) . . ? C6B C1B C2B 120.3(5) . . ? C6B C1B H1B1 119.8 . . ? C2B C1B H1B1 119.8 . . ? C1B C2B C3B 120.3(5) . . ? C1B C2B C7B 120.2(7) . . ? C3B C2B C7B 119.5(7) . . ? C2B C3B C4B 118.5(6) . . ? C2B C3B H3B 120.7 . . ? C4B C3B H3B 120.7 . . ? C3B C4B C5B 121.3(5) . . ? C3B C4B H4B 119.3 . . ? C5B C4B H4B 119.3 . . ? C6B C5B C4B 118.7(5) . . ? C6B C5B H5B 120.6 . . ? C4B C5B H5B 120.6 . . ? C5B C6B C1B 120.8(6) . . ? C5B C6B H6B 119.6 . . ? C1B C6B H6B 119.6 . . ? C5A2 C1A C2A 127.8(10) . . ? C5A2 C1A C2A 127.8(10) . 2_656 ? C2A C1A C2A 104(2) . 2_656 ? C3A C2A C1A 129.5(19) . . ? C3A C2A H2A 115.3 . . ? C1A C2A H2A 115.3 . . ? C2A C3A C4A 124(2) . . ? C2A C3A H3A 118.1 . . ? C4A C3A H3A 118.1 . . ? C5A1 C4A C3A 125.4(11) . 2_656 ? C5A1 C4A C3A 125.4(11) . . ? C3A C4A C3A 109(2) 2_656 . ? N2 Hg1 N3 179.2(3) . 4_546 ? N2 Hg1 O4 92.9(3) . . ? N3 Hg1 O4 86.3(3) 4_546 . ? C7 N1 C1 111.4(7) . . ? C7 N1 C13 114.9(7) . . ? C1 N1 C13 112.3(7) . . ? C4 N2 C5 119.1(7) . . ? C4 N2 Hg1 122.2(5) . . ? C5 N2 Hg1 118.4(5) . . ? C11 N3 C10 120.1(7) . . ? C11 N3 Hg1 120.4(6) . 4_556 ? C10 N3 Hg1 119.4(5) . 4_556 ? S2 O4 Hg1 154.0(6) . . ? O2 S1 O1 116.6(5) . . ? O2 S1 O3 114.4(5) . . ? O1 S1 O3 112.8(5) . . ? O2 S1 C41 103.1(7) . . ? O1 S1 C41 103.6(6) . . ? O3 S1 C41 104.4(7) . . ? O4 S2 O5 117.2(6) . . ? O4 S2 C42 113.5(11) . . ? O5 S2 C42 106.2(10) . . ? O4 S2 O6 109.7(7) . . ? O5 S2 O6 109.8(7) . . ? C42 S2 O6 98.8(11) . . ? C4C C3C C2C 118.2(10) . . ? C4C C3C H3C 120.9 . . ? C2C C3C H3C 120.9 . . ? C1C C2C C3C 119.5(11) . . ? C1C C2C H2C 120.3 . . ? C3C C2C H2C 120.3 . . ? C3C C4C C3C 122.9(17) . 2 ? C3C C4C C5C 118.6(9) . . ? C3C C4C C5C 118.6(9) 2 . ? C2C C1C C2C 121.8(18) . 2 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.585 _refine_diff_density_min -0.651 _refine_diff_density_rms 0.128 data_2a/HgCl2 _database_code_depnum_ccdc_archive 'CCDC 910367' #TrackingRef '15353_web_deposit_cif_file_0_YoichiHabata_1352699762.All_complexes_1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H46 Cl4 Hg2 N6' _chemical_formula_weight 1249.89 _chemical_absolute_configuration syn 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Hg Hg -2.3894 9.2266 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 11.269(2) _cell_length_b 14.216(3) _cell_length_c 14.794(3) _cell_angle_alpha 90.00 _cell_angle_beta 106.79(3) _cell_angle_gamma 90.00 _cell_volume 2269.1(8) _cell_formula_units_Z 2 _cell_measurement_temperature 153 _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.829 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1208 _exptl_absorpt_coefficient_mu 7.035 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.3641 _exptl_absorpt_correction_T_max 0.7661 _exptl_absorpt_process_details 'SADABS; Sheldrick, 1996' _exptl_special_details ; ? ; _diffrn_ambient_temperature 153 _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 P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ?8.333 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14516 _diffrn_reflns_av_R_equivalents 0.0215 _diffrn_reflns_av_sigmaI/netI 0.0509 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.44 _diffrn_reflns_theta_max 27.48 _reflns_number_total 9560 _reflns_number_gt 8707 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _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^)+(0.0324P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.001(5) _refine_ls_number_reflns 9560 _refine_ls_number_parameters 543 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0291 _refine_ls_R_factor_gt 0.0249 _refine_ls_wR_factor_ref 0.0526 _refine_ls_wR_factor_gt 0.0509 _refine_ls_goodness_of_fit_ref 0.739 _refine_ls_restrained_S_all 0.739 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C14 C 1.2782(4) 0.9111(4) 0.5980(3) 0.0241(11) Uani 1 1 d . . . H14A H 1.2143 0.9295 0.6276 0.036 Uiso 1 1 calc R . . H14B H 1.2586 0.9379 0.5344 0.036 Uiso 1 1 calc R . . H14C H 1.3590 0.9346 0.6361 0.036 Uiso 1 1 calc R . . C41 C -0.0557(6) 0.5723(5) -0.0507(4) 0.0331(16) Uani 1 1 d . . . H41 H -0.1282 0.5344 -0.0678 0.040 Uiso 1 1 calc R . . C5 C 1.5702(5) 0.5603(5) 0.8571(4) 0.0238(13) Uani 1 1 d . . . H5 H 1.5778 0.4971 0.8386 0.029 Uiso 1 1 calc R . . Hg2 Hg -0.286475(16) 0.713665(12) 0.137817(12) 0.02037(6) Uani 1 1 d . . . Hg1 Hg 0.708319(16) 0.638701(12) 0.647072(12) 0.02119(6) Uani 1 1 d . . . Cl4 Cl -0.36673(13) 0.86730(12) 0.14831(10) 0.0283(3) Uani 1 1 d . . . Cl3 Cl -0.27040(12) 0.55562(11) 0.19812(9) 0.0231(3) Uani 1 1 d . . . Cl2 Cl 0.72635(12) 0.79577(12) 0.70967(9) 0.0269(3) Uani 1 1 d . . . Cl1 Cl 0.63490(13) 0.48108(11) 0.64615(9) 0.0270(3) Uani 1 1 d . . . N1 N 1.3126(4) 0.7560(3) 0.6854(3) 0.0156(10) Uani 1 1 d . . . N4 N 0.3205(4) 0.6006(4) 0.1928(3) 0.0171(10) Uani 1 1 d . . . C24 C 1.1663(4) 0.6654(4) 0.4936(3) 0.0137(12) Uani 1 1 d . . . N3 N 0.9183(4) 0.6125(3) 0.6593(3) 0.0188(11) Uani 1 1 d . . . C15 C 1.1648(5) 0.7612(4) 0.5256(3) 0.0149(12) Uani 1 1 d . . . N5 N 0.6086(4) 0.6793(3) 0.4885(3) 0.0207(11) Uani 1 1 d . . . C30 C 0.5153(5) 0.7265(5) 0.2996(4) 0.0210(13) Uani 1 1 d . . . H30 H 0.4846 0.7422 0.2346 0.025 Uiso 1 1 calc R . . C32 C 0.1343(5) 0.6870(4) 0.2091(3) 0.0136(11) Uani 1 1 d . . . C9 C 0.9996(4) 0.6848(4) 0.6800(3) 0.0163(12) Uani 1 1 d . . . H9 H 0.9676 0.7468 0.6780 0.020 Uiso 1 1 calc R . . C25 C 0.4335(5) 0.5597(4) 0.2602(3) 0.0202(12) Uani 1 1 d . . . H25A H 0.4903 0.5359 0.2254 0.024 Uiso 1 1 calc R . . H25B H 0.4103 0.5065 0.2948 0.024 Uiso 1 1 calc R . . C10 C 0.9628(5) 0.5261(5) 0.6611(3) 0.0230(13) Uani 1 1 d . . . H10 H 0.9063 0.4750 0.6450 0.028 Uiso 1 1 calc R . . C33 C 0.0069(5) 0.6727(4) 0.1826(3) 0.0195(12) Uani 1 1 d . . . H33 H -0.0233 0.6103 0.1826 0.023 Uiso 1 1 calc R . . C35 C 0.0913(5) 0.8520(4) 0.1836(3) 0.0218(12) Uani 1 1 d . . . H35 H 0.1191 0.9150 0.1834 0.026 Uiso 1 1 calc R . . C34 C -0.0338(5) 0.8317(4) 0.1570(4) 0.0219(12) Uani 1 1 d . . . H34 H -0.0918 0.8816 0.1382 0.026 Uiso 1 1 calc R . . C31 C 0.2229(5) 0.6058(4) 0.2409(3) 0.0186(12) Uani 1 1 d . . . H31A H 0.2626 0.6114 0.3098 0.022 Uiso 1 1 calc R . . H31B H 0.1751 0.5464 0.2297 0.022 Uiso 1 1 calc R . . C19 C 1.0548(5) 0.6243(5) 0.4365(3) 0.0182(12) Uani 1 1 d . . . C7 C 1.2131(5) 0.7562(4) 0.7307(3) 0.0179(12) Uani 1 1 d . . . H7A H 1.1646 0.8149 0.7134 0.022 Uiso 1 1 calc R . . H7B H 1.2504 0.7563 0.8000 0.022 Uiso 1 1 calc R . . C36 C 0.1751(5) 0.7794(4) 0.2104(3) 0.0200(12) Uani 1 1 d . . . H36 H 0.2615 0.7926 0.2298 0.024 Uiso 1 1 calc R . . C11 C 1.0887(5) 0.5075(5) 0.6855(4) 0.0256(13) Uani 1 1 d . . . H11 H 1.1180 0.4447 0.6867 0.031 Uiso 1 1 calc R . . N6 N -0.0756(4) 0.7432(3) 0.1570(3) 0.0194(11) Uani 1 1 d . . . C12 C 1.1707(5) 0.5816(5) 0.7079(4) 0.0222(13) Uani 1 1 d . . . H12 H 1.2574 0.5701 0.7261 0.027 Uiso 1 1 calc R . . C26 C 0.4980(4) 0.6365(6) 0.3300(3) 0.0183(11) Uani 1 1 d . . . C13 C 1.2826(5) 0.8050(4) 0.5921(3) 0.0169(11) Uani 1 1 d . . . H13 H 1.3515 0.7899 0.5645 0.020 Uiso 1 1 calc R . . C17 C 0.9461(5) 0.7703(5) 0.4407(3) 0.0204(13) Uani 1 1 d . . . H17 H 0.8721 0.8065 0.4230 0.025 Uiso 1 1 calc R . . C27 C 0.5468(4) 0.6154(4) 0.4253(3) 0.0185(12) Uani 1 1 d . . . H27 H 0.5361 0.5538 0.4464 0.022 Uiso 1 1 calc R . . C8 C 1.1263(5) 0.6734(4) 0.7039(4) 0.0186(12) Uani 1 1 d . . . C18 C 0.9448(5) 0.6803(4) 0.4112(3) 0.0199(13) Uani 1 1 d . . . H18 H 0.8696 0.6538 0.3730 0.024 Uiso 1 1 calc R . . C16 C 1.0568(5) 0.8107(4) 0.4976(3) 0.0188(12) Uani 1 1 d . . . H16 H 1.0561 0.8744 0.5170 0.023 Uiso 1 1 calc R . . C29 C 0.5774(5) 0.7932(5) 0.3642(4) 0.0242(13) Uani 1 1 d . . . H29 H 0.5891 0.8555 0.3450 0.029 Uiso 1 1 calc R . . C28 C 0.6219(5) 0.7658(4) 0.4582(4) 0.0226(13) Uani 1 1 d . . . H28 H 0.6641 0.8112 0.5032 0.027 Uiso 1 1 calc R . . C46 C 0.2631(5) 0.8284(4) -0.0130(3) 0.0240(14) Uani 1 1 d . . . H46 H 0.3350 0.8669 0.0013 0.029 Uiso 1 1 calc R . . C45 C 0.1495(6) 0.8643(5) -0.0730(4) 0.0318(15) Uani 1 1 d . . . H45 H 0.1468 0.9263 -0.0975 0.038 Uiso 1 1 calc R . . C44 C 0.0457(6) 0.8114(5) -0.0957(4) 0.0330(16) Uani 1 1 d . . . H44 H -0.0298 0.8363 -0.1351 0.040 Uiso 1 1 calc R . . C43 C 0.0499(5) 0.7179(6) -0.0601(3) 0.0227(12) Uani 1 1 d . . . C47 C 0.2707(6) 0.7418(5) 0.0239(4) 0.0259(16) Uani 1 1 d . . . H47 H 0.3470 0.7203 0.0652 0.031 Uiso 1 1 calc R . . C39 C 0.1638(5) 0.5881(5) 0.0369(4) 0.0228(14) Uani 1 1 d . . . C48 C 0.1626(6) 0.6802(4) 0.0010(4) 0.0242(14) Uani 1 1 d . . . C40 C 0.0560(5) 0.5353(5) 0.0094(4) 0.0255(14) Uani 1 1 d . . . H40 H 0.0570 0.4725 0.0316 0.031 Uiso 1 1 calc R . . C42 C -0.0598(6) 0.6614(5) -0.0838(4) 0.0325(18) Uani 1 1 d . . . H42 H -0.1356 0.6864 -0.1228 0.039 Uiso 1 1 calc R . . C2 C 1.4934(4) 0.7186(6) 0.8199(3) 0.0175(11) Uani 1 1 d . . . C6 C 1.5057(4) 0.6259(5) 0.7923(3) 0.0197(13) Uani 1 1 d . . . H6 H 1.4694 0.6078 0.7285 0.024 Uiso 1 1 calc R . . N2 N 1.6139(4) 0.6770(4) 0.9780(3) 0.0203(11) Uani 1 1 d . . . C37 C 0.2783(5) 0.5447(5) 0.1042(4) 0.0235(13) Uani 1 1 d . . . H37 H 0.2525 0.4819 0.1224 0.028 Uiso 1 1 calc R . . C1 C 1.4305(5) 0.7913(4) 0.7498(3) 0.0196(12) Uani 1 1 d . . . H1A H 1.4135 0.8475 0.7836 0.024 Uiso 1 1 calc R . . H1B H 1.4864 0.8106 0.7123 0.024 Uiso 1 1 calc R . . C4 C 1.6233(5) 0.5885(5) 0.9491(4) 0.0236(14) Uani 1 1 d . . . H4 H 1.6683 0.5438 0.9936 0.028 Uiso 1 1 calc R . . C3 C 1.5503(4) 0.7400(4) 0.9149(3) 0.0189(12) Uani 1 1 d . . . H3 H 1.5435 0.8024 0.9358 0.023 Uiso 1 1 calc R . . C21 C 1.1619(5) 0.4773(4) 0.4302(4) 0.0259(13) Uani 1 1 d . . . H21 H 1.1602 0.4141 0.4089 0.031 Uiso 1 1 calc R . . C22 C 1.2732(5) 0.5173(4) 0.4877(4) 0.0209(12) Uani 1 1 d . . . H22 H 1.3466 0.4805 0.5057 0.025 Uiso 1 1 calc R . . C20 C 1.0570(5) 0.5311(4) 0.4057(4) 0.0217(13) Uani 1 1 d . . . H20 H 0.9826 0.5044 0.3664 0.026 Uiso 1 1 calc R . . C23 C 1.2758(5) 0.6095(4) 0.5177(4) 0.0192(13) Uani 1 1 d . . . H23 H 1.3516 0.6360 0.5549 0.023 Uiso 1 1 calc R . . C38 C 0.3801(4) 0.5258(4) 0.0566(3) 0.0281(12) Uani 1 1 d . . . H38A H 0.4297 0.5829 0.0589 0.042 Uiso 1 1 calc R . . H38B H 0.3421 0.5077 -0.0094 0.042 Uiso 1 1 calc R . . H38C H 0.4336 0.4748 0.0898 0.042 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 C14 0.024(3) 0.022(3) 0.022(2) 0.000(2) -0.0006(19) -0.008(2) C41 0.040(4) 0.031(4) 0.030(3) -0.009(3) 0.012(3) -0.012(3) C5 0.023(3) 0.018(4) 0.030(3) -0.009(2) 0.008(2) -0.004(3) Hg2 0.01655(11) 0.02154(14) 0.01986(9) 0.00033(9) 0.00026(8) 0.00222(10) Hg1 0.01627(11) 0.02270(14) 0.02266(10) 0.00096(9) 0.00253(8) -0.00314(10) Cl4 0.0308(8) 0.0232(9) 0.0331(7) 0.0035(6) 0.0129(6) 0.0063(7) Cl3 0.0197(7) 0.0235(9) 0.0235(6) 0.0046(5) 0.0023(5) 0.0010(6) Cl2 0.0248(7) 0.0262(9) 0.0311(7) -0.0057(6) 0.0102(6) -0.0046(6) Cl1 0.0278(8) 0.0225(9) 0.0310(7) 0.0016(6) 0.0090(6) -0.0057(7) N1 0.014(2) 0.016(3) 0.016(2) -0.0004(17) 0.0030(16) -0.0035(18) N4 0.012(2) 0.023(3) 0.015(2) -0.0005(18) 0.0012(16) -0.0006(19) C24 0.014(2) 0.018(3) 0.009(2) 0.0019(18) 0.0032(18) -0.002(2) N3 0.017(2) 0.022(3) 0.016(2) 0.0033(17) 0.0030(17) 0.002(2) C15 0.017(3) 0.016(3) 0.010(2) 0.000(2) 0.0027(19) -0.003(2) N5 0.020(2) 0.019(3) 0.020(2) -0.0030(18) 0.0006(18) -0.0026(19) C30 0.022(3) 0.020(4) 0.022(2) 0.005(2) 0.007(2) -0.001(3) C32 0.015(2) 0.014(3) 0.013(2) -0.0003(18) 0.0044(18) -0.0008(19) C9 0.010(2) 0.017(3) 0.020(2) -0.0021(19) 0.0023(19) -0.003(2) C25 0.017(3) 0.019(3) 0.023(3) 0.005(2) 0.002(2) 0.006(2) C10 0.023(3) 0.024(4) 0.022(3) -0.001(2) 0.005(2) -0.004(3) C33 0.025(3) 0.020(3) 0.014(2) -0.003(2) 0.006(2) -0.002(2) C35 0.024(3) 0.018(3) 0.024(3) -0.003(2) 0.008(2) 0.002(2) C34 0.024(3) 0.020(3) 0.022(3) 0.001(2) 0.006(2) 0.003(2) C31 0.018(3) 0.022(3) 0.017(2) 0.003(2) 0.006(2) -0.001(2) C19 0.018(3) 0.021(4) 0.014(2) 0.000(2) 0.0024(18) -0.003(3) C7 0.014(3) 0.023(3) 0.015(2) -0.003(2) 0.0015(19) -0.001(2) C36 0.020(3) 0.018(3) 0.023(3) -0.005(2) 0.007(2) -0.012(2) C11 0.031(3) 0.018(3) 0.030(3) 0.005(2) 0.013(3) 0.005(3) N6 0.019(2) 0.023(3) 0.016(2) 0.0017(17) 0.0050(17) 0.004(2) C12 0.015(3) 0.032(4) 0.019(3) 0.005(2) 0.003(2) -0.003(3) C26 0.009(2) 0.020(3) 0.025(2) -0.005(3) 0.0018(18) 0.000(3) C13 0.021(3) 0.013(3) 0.017(2) 0.001(2) 0.005(2) -0.002(2) C17 0.008(2) 0.027(4) 0.023(3) 0.002(2) -0.001(2) 0.002(2) C27 0.016(3) 0.013(3) 0.027(3) 0.004(2) 0.006(2) 0.003(2) C8 0.018(3) 0.019(3) 0.020(2) 0.000(2) 0.008(2) 0.000(2) C18 0.016(3) 0.024(4) 0.015(2) -0.002(2) -0.002(2) -0.008(2) C16 0.023(3) 0.013(3) 0.018(2) 0.002(2) 0.003(2) 0.004(2) C29 0.025(3) 0.019(4) 0.027(3) -0.001(2) 0.006(2) -0.006(3) C28 0.024(3) 0.017(3) 0.025(3) -0.001(2) 0.005(2) -0.001(2) C46 0.024(3) 0.032(4) 0.019(3) -0.008(2) 0.010(2) -0.009(3) C45 0.040(4) 0.032(4) 0.028(3) 0.003(3) 0.016(3) 0.006(3) C44 0.036(4) 0.038(5) 0.025(3) -0.003(3) 0.009(3) 0.005(3) C43 0.027(3) 0.028(4) 0.013(2) -0.007(3) 0.0059(19) 0.003(3) C47 0.026(3) 0.033(5) 0.020(3) -0.006(2) 0.010(2) -0.012(3) C39 0.023(3) 0.024(4) 0.022(3) -0.004(2) 0.006(2) -0.003(3) C48 0.035(3) 0.022(4) 0.017(3) -0.001(2) 0.011(2) 0.001(3) C40 0.024(3) 0.024(4) 0.028(3) -0.003(2) 0.006(2) -0.003(3) C42 0.025(3) 0.048(5) 0.023(3) -0.007(3) 0.005(2) -0.002(3) C2 0.011(2) 0.022(3) 0.019(2) -0.002(3) 0.0044(18) -0.005(3) C6 0.012(2) 0.028(4) 0.016(2) 0.000(2) 0.0006(17) -0.002(3) N2 0.018(2) 0.021(3) 0.020(2) 0.0001(18) 0.0013(18) 0.0000(19) C37 0.023(3) 0.022(4) 0.022(3) -0.001(2) -0.001(2) -0.003(3) C1 0.014(3) 0.022(4) 0.020(2) 0.001(2) -0.0003(19) -0.001(2) C4 0.018(3) 0.033(4) 0.019(3) 0.006(2) 0.003(2) 0.001(3) C3 0.015(3) 0.020(4) 0.019(2) 0.002(2) 0.001(2) -0.002(2) C21 0.042(4) 0.013(3) 0.026(3) 0.001(2) 0.015(2) 0.001(3) C22 0.023(3) 0.014(3) 0.025(3) -0.001(2) 0.006(2) 0.002(2) C20 0.024(3) 0.020(4) 0.019(3) -0.006(2) 0.002(2) -0.011(2) C23 0.023(3) 0.014(4) 0.018(2) -0.001(2) 0.002(2) -0.008(2) C38 0.024(3) 0.029(3) 0.028(3) -0.007(2) 0.004(2) 0.005(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 C14 C13 1.512(7) . ? C41 C42 1.354(10) . ? C41 C40 1.416(8) . ? C5 C4 1.379(7) . ? C5 C6 1.383(8) . ? Hg2 N6 2.348(4) . ? Hg2 N2 2.364(4) 1_354 ? Hg2 Cl4 2.3860(17) . ? Hg2 Cl3 2.4049(16) . ? Hg1 N3 2.350(4) . ? Hg1 N5 2.362(4) . ? Hg1 Cl1 2.3873(16) . ? Hg1 Cl2 2.4033(17) . ? N1 C1 1.481(6) . ? N1 C7 1.464(6) . ? N1 C13 1.495(6) . ? N4 C37 1.489(7) . ? N4 C31 1.474(6) . ? N4 C25 1.490(6) . ? C24 C23 1.423(7) . ? C24 C19 1.422(7) . ? C24 C15 1.444(7) . ? N3 C10 1.324(7) . ? N3 C9 1.352(7) . ? C15 C16 1.362(7) . ? C15 C13 1.537(7) . ? N5 C28 1.333(7) . ? N5 C27 1.345(7) . ? C30 C29 1.385(8) . ? C30 C26 1.388(10) . ? C32 C33 1.390(7) . ? C32 C36 1.390(8) . ? C32 C31 1.510(7) . ? C9 C8 1.378(7) . ? C25 C26 1.533(9) . ? C10 C11 1.385(8) . ? C33 N6 1.345(7) . ? C35 C34 1.380(7) . ? C35 C36 1.378(8) . ? C34 N6 1.345(7) . ? C19 C20 1.404(8) . ? C19 C18 1.428(8) . ? C7 C8 1.508(8) . ? C11 C12 1.377(9) . ? C12 C8 1.393(8) . ? C26 C27 1.390(7) . ? C17 C18 1.350(8) . ? C17 C16 1.411(7) . ? C29 C28 1.390(7) . ? C46 C47 1.340(9) . ? C46 C45 1.425(8) . ? C45 C44 1.349(9) . ? C44 C43 1.425(10) . ? C43 C48 1.433(8) . ? C43 C42 1.431(9) . ? C47 C48 1.458(8) . ? C39 C40 1.386(8) . ? C39 C48 1.411(8) . ? C39 C37 1.515(8) . ? C2 C6 1.399(10) . ? C2 C3 1.399(6) . ? C2 C1 1.491(8) . ? N2 C4 1.342(7) . ? N2 C3 1.342(7) . ? N2 Hg2 2.364(4) 1_756 ? C37 C38 1.534(7) . ? C21 C20 1.366(8) . ? C21 C22 1.415(7) . ? C22 C23 1.382(8) . ? 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 C42 C41 C40 120.4(6) . . ? C4 C5 C6 118.6(6) . . ? N6 Hg2 N2 109.40(14) . 1_354 ? N6 Hg2 Cl4 102.59(12) . . ? N2 Hg2 Cl4 100.81(12) 1_354 . ? N6 Hg2 Cl3 99.02(12) . . ? N2 Hg2 Cl3 97.36(12) 1_354 . ? Cl4 Hg2 Cl3 145.12(4) . . ? N3 Hg1 N5 107.13(14) . . ? N3 Hg1 Cl1 101.03(12) . . ? N5 Hg1 Cl1 99.15(12) . . ? N3 Hg1 Cl2 98.42(12) . . ? N5 Hg1 Cl2 96.82(12) . . ? Cl1 Hg1 Cl2 149.86(4) . . ? C1 N1 C7 111.6(4) . . ? C1 N1 C13 111.0(4) . . ? C7 N1 C13 115.0(4) . . ? C37 N4 C31 111.0(4) . . ? C37 N4 C25 112.0(4) . . ? C31 N4 C25 108.0(4) . . ? C23 C24 C19 118.3(5) . . ? C23 C24 C15 122.4(5) . . ? C19 C24 C15 119.3(5) . . ? C10 N3 C9 118.1(5) . . ? C10 N3 Hg1 121.1(4) . . ? C9 N3 Hg1 119.9(3) . . ? C16 C15 C24 118.8(5) . . ? C16 C15 C13 121.0(5) . . ? C24 C15 C13 120.1(5) . . ? C28 N5 C27 118.4(5) . . ? C28 N5 Hg1 119.5(4) . . ? C27 N5 Hg1 121.9(4) . . ? C29 C30 C26 119.9(5) . . ? C33 C32 C36 117.0(5) . . ? C33 C32 C31 120.8(5) . . ? C36 C32 C31 122.1(5) . . ? N3 C9 C8 123.6(5) . . ? N4 C25 C26 108.6(5) . . ? N3 C10 C11 122.5(6) . . ? N6 C33 C32 122.9(5) . . ? C34 C35 C36 119.0(6) . . ? N6 C34 C35 121.6(6) . . ? N4 C31 C32 114.0(4) . . ? C20 C19 C24 119.0(5) . . ? C20 C19 C18 122.4(5) . . ? C24 C19 C18 118.6(6) . . ? N1 C7 C8 113.8(4) . . ? C35 C36 C32 120.4(5) . . ? C12 C11 C10 118.9(6) . . ? C33 N6 C34 118.9(5) . . ? C33 N6 Hg2 119.6(4) . . ? C34 N6 Hg2 120.7(4) . . ? C11 C12 C8 119.9(5) . . ? C27 C26 C30 118.4(6) . . ? C27 C26 C25 120.0(6) . . ? C30 C26 C25 121.4(5) . . ? N1 C13 C14 114.4(4) . . ? N1 C13 C15 109.0(4) . . ? C14 C13 C15 113.9(4) . . ? C18 C17 C16 120.2(5) . . ? N5 C27 C26 122.2(6) . . ? C9 C8 C12 117.0(5) . . ? C9 C8 C7 121.4(5) . . ? C12 C8 C7 121.5(5) . . ? C17 C18 C19 121.0(5) . . ? C15 C16 C17 122.0(6) . . ? C30 C29 C28 117.6(6) . . ? N5 C28 C29 123.5(6) . . ? C47 C46 C45 121.5(6) . . ? C44 C45 C46 120.9(7) . . ? C45 C44 C43 119.6(6) . . ? C48 C43 C44 120.7(6) . . ? C48 C43 C42 119.4(7) . . ? C44 C43 C42 119.9(6) . . ? C46 C47 C48 120.4(6) . . ? C40 C39 C48 118.7(6) . . ? C40 C39 C37 118.7(6) . . ? C48 C39 C37 122.6(6) . . ? C39 C48 C43 119.6(6) . . ? C39 C48 C47 123.6(6) . . ? C43 C48 C47 116.8(6) . . ? C39 C40 C41 121.8(6) . . ? C41 C42 C43 119.9(6) . . ? C6 C2 C3 116.3(6) . . ? C6 C2 C1 121.2(5) . . ? C3 C2 C1 122.4(6) . . ? C2 C6 C5 120.6(5) . . ? C4 N2 C3 118.6(5) . . ? C4 N2 Hg2 117.9(4) . 1_756 ? C3 N2 Hg2 123.6(4) . 1_756 ? N4 C37 C39 110.9(5) . . ? N4 C37 C38 114.0(4) . . ? C39 C37 C38 112.2(4) . . ? N1 C1 C2 111.7(5) . . ? N2 C4 C5 122.4(6) . . ? N2 C3 C2 123.5(6) . . ? C20 C21 C22 118.9(6) . . ? C23 C22 C21 120.5(5) . . ? C21 C20 C19 122.5(5) . . ? C22 C23 C24 120.8(5) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.819 _refine_diff_density_min -0.844 _refine_diff_density_rms 0.092 data_2a/Hg(OTf)2 _database_code_depnum_ccdc_archive 'CCDC 910368' #TrackingRef '15353_web_deposit_cif_file_0_YoichiHabata_1352699762.All_complexes_1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C51 H50 F6 Hg N6 O7 S2' _chemical_formula_weight 1237.68 _chemical_absolute_configuration syn loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Hg Hg -2.3894 9.2266 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 10.8176(6) _cell_length_b 18.1757(11) _cell_length_c 25.9297(15) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5098.2(5) _cell_formula_units_Z 4 _cell_measurement_temperature 100 _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.612 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2480 _exptl_absorpt_coefficient_mu 3.180 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.4284 _exptl_absorpt_correction_T_max 0.5387 _exptl_absorpt_process_details 'SADABS; Sheldrick, 1996' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100 _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 8.366 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 35592 _diffrn_reflns_av_R_equivalents 0.0345 _diffrn_reflns_av_sigmaI/netI 0.0513 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 1.37 _diffrn_reflns_theta_max 27.48 _reflns_number_total 11673 _reflns_number_gt 10957 _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^)+(0.0431P)^2^+11.4719P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.023(6) _refine_ls_number_reflns 11673 _refine_ls_number_parameters 661 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0476 _refine_ls_R_factor_gt 0.0436 _refine_ls_wR_factor_ref 0.1047 _refine_ls_wR_factor_gt 0.1015 _refine_ls_goodness_of_fit_ref 1.138 _refine_ls_restrained_S_all 1.140 _refine_ls_shift/su_max 0.010 _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 C7 C 0.9160(6) 0.6236(4) 0.7819(3) 0.0283(14) Uani 1 1 d . . . H7A H 0.9551 0.5907 0.7562 0.034 Uiso 1 1 calc R . . H7B H 0.8437 0.5975 0.7966 0.034 Uiso 1 1 calc R . . C31 C -0.1383(6) 0.4855(4) 0.9568(3) 0.0304(15) Uani 1 1 d . . . H31A H -0.0682 0.5142 0.9427 0.037 Uiso 1 1 calc R . . H31B H -0.1852 0.5179 0.9804 0.037 Uiso 1 1 calc R . . C35 C -0.2620(8) 0.3931(5) 0.8351(3) 0.049(2) Uani 1 1 d . . . H35 H -0.2388 0.3570 0.8104 0.059 Uiso 1 1 calc R . . C12 C 0.9817(6) 0.6909(4) 0.8623(3) 0.0340(15) Uani 1 1 d . . . H12 H 0.9048 0.7160 0.8621 0.041 Uiso 1 1 calc R . . C34 C -0.3721(8) 0.4295(4) 0.8314(3) 0.0358(17) Uani 1 1 d . . . H34 H -0.4234 0.4195 0.8025 0.043 Uiso 1 1 calc R . . Hg1 Hg 0.391538(19) 0.546688(12) 0.865300(9) 0.02159(6) Uani 1 1 d . . . S1 S 0.33918(16) 0.46171(11) 0.73616(6) 0.0333(4) Uani 1 1 d . . . N5 N 0.2730(4) 0.4546(3) 0.89414(19) 0.0240(10) Uani 1 1 d . . . C27 C 0.1999(6) 0.4686(3) 0.9355(2) 0.0242(13) Uani 1 1 d . . . H27 H 0.2022 0.5163 0.9504 0.029 Uiso 1 1 calc R . . C30 C 0.1220(6) 0.3468(3) 0.9345(2) 0.0275(13) Uani 1 1 d . . . H30 H 0.0702 0.3091 0.9478 0.033 Uiso 1 1 calc R . . C5 C 0.5983(6) 0.7589(3) 0.8673(3) 0.0318(13) Uani 1 1 d . . . H5 H 0.6018 0.8001 0.8898 0.038 Uiso 1 1 calc R . . N2 N 0.5148(5) 0.6423(3) 0.8476(2) 0.0249(11) Uani 1 1 d . . . C46 C -0.1917(8) 0.1980(5) 0.9367(3) 0.0393(18) Uani 1 1 d . . . H46 H -0.2353 0.1983 0.9049 0.047 Uiso 1 1 calc R . . C48 C -0.1258(6) 0.2610(4) 1.0143(3) 0.0289(14) Uani 1 1 d . . . C4 C 0.5208(6) 0.7005(4) 0.8777(3) 0.0305(15) Uani 1 1 d . . . H4 H 0.4701 0.7024 0.9076 0.037 Uiso 1 1 calc R . . C2 C 0.6648(6) 0.6952(4) 0.7912(3) 0.0262(14) Uani 1 1 d . . . C26 C 0.1220(6) 0.4165(3) 0.9569(2) 0.0229(12) Uani 1 1 d . . . C45 C -0.1273(8) 0.1340(5) 0.9519(3) 0.047(2) Uani 1 1 d . . . H45 H -0.1289 0.0913 0.9308 0.056 Uiso 1 1 calc R . . C44 C -0.0651(7) 0.1339(4) 0.9955(3) 0.044(2) Uani 1 1 d . . . H44 H -0.0201 0.0910 1.0049 0.053 Uiso 1 1 calc R . . C6 C 0.6707(6) 0.7562(4) 0.8234(3) 0.0291(14) Uani 1 1 d . . . H6 H 0.7244 0.7960 0.8153 0.035 Uiso 1 1 calc R . . C28 C 0.2710(6) 0.3887(4) 0.8734(3) 0.0272(14) Uani 1 1 d . . . H28 H 0.3214 0.3790 0.8442 0.033 Uiso 1 1 calc R . . C47 C -0.1922(6) 0.2596(4) 0.9669(3) 0.0297(15) Uani 1 1 d . . . H47 H -0.2373 0.3018 0.9562 0.036 Uiso 1 1 calc R . . C3 C 0.5858(5) 0.6397(4) 0.8046(2) 0.0250(13) Uani 1 1 d . . . H3 H 0.5805 0.5977 0.7830 0.030 Uiso 1 1 calc R . . C40 C -0.0663(6) 0.3175(4) 1.0940(3) 0.0346(16) Uani 1 1 d . . . H40 H -0.0674 0.3581 1.1170 0.041 Uiso 1 1 calc R . . C39 C -0.1243(6) 0.3240(4) 1.0476(2) 0.0260(13) Uani 1 1 d . . . C43 C -0.0629(6) 0.1955(4) 1.0289(3) 0.0337(16) Uani 1 1 d . . . C29 C 0.1971(6) 0.3329(4) 0.8930(3) 0.0275(14) Uani 1 1 d . . . H29 H 0.1986 0.2853 0.8778 0.033 Uiso 1 1 calc R . . S2 S 0.46399(17) 0.60567(13) 1.00911(7) 0.0397(5) Uani 1 1 d . . . N6 N -0.4115(4) 0.4783(3) 0.8660(2) 0.0254(10) Uani 1 1 d . . . O1 O 0.3750(5) 0.5196(3) 0.77086(17) 0.0341(11) Uani 1 1 d . . . N3 N 1.2038(5) 0.6177(3) 0.8635(2) 0.0286(11) Uani 1 1 d . . . C9 C 1.1203(6) 0.6043(3) 0.8268(2) 0.0260(13) Uani 1 1 d . . . H9 H 1.1393 0.5689 0.8010 0.031 Uiso 1 1 calc R . . C25 C 0.0384(6) 0.4350(4) 1.0021(2) 0.0244(14) Uani 1 1 d . . . H25A H 0.0586 0.4032 1.0320 0.029 Uiso 1 1 calc R . . H25B H 0.0502 0.4869 1.0125 0.029 Uiso 1 1 calc R . . O4 O 0.4141(5) 0.5755(3) 0.96357(19) 0.0478(15) Uani 1 1 d . . . C32 C -0.2225(6) 0.4622(4) 0.9124(2) 0.0270(13) Uani 1 1 d . . . C33 C -0.3369(6) 0.4945(3) 0.9055(3) 0.0271(14) Uani 1 1 d . . . H33 H -0.3638 0.5299 0.9299 0.033 Uiso 1 1 calc R . . O3 O 0.3919(9) 0.3915(3) 0.7495(2) 0.0639(19) Uani 1 1 d . . . O2 O 0.2153(6) 0.4616(6) 0.7209(3) 0.096(3) Uani 1 1 d . . . C10 C 1.1782(7) 0.6674(4) 0.8992(3) 0.0332(15) Uani 1 1 d . . . H10 H 1.2379 0.6774 0.9252 0.040 Uiso 1 1 calc R . . C37 C -0.1726(6) 0.3975(4) 1.0285(2) 0.0259(14) Uani 1 1 d . . . H37 H -0.2549 0.3875 1.0123 0.031 Uiso 1 1 calc R . . C36 C -0.1856(7) 0.4104(5) 0.8757(3) 0.045(2) Uani 1 1 d . . . H36 H -0.1075 0.3870 0.8789 0.053 Uiso 1 1 calc R . . N1 N 0.8739(5) 0.6905(3) 0.7562(2) 0.0248(11) Uani 1 1 d . . . C8 C 1.0077(6) 0.6396(4) 0.8247(3) 0.0265(13) Uani 1 1 d . . . C13 C 0.9523(6) 0.7137(4) 0.7113(2) 0.0250(14) Uani 1 1 d . . . H13 H 0.9203 0.7627 0.7000 0.030 Uiso 1 1 calc R . . C1 C 0.7426(6) 0.6908(4) 0.7436(3) 0.0260(14) Uani 1 1 d . . . H1A H 0.7218 0.6455 0.7243 0.031 Uiso 1 1 calc R . . H1B H 0.7242 0.7335 0.7211 0.031 Uiso 1 1 calc R . . C11 C 1.0666(7) 0.7054(4) 0.9000(3) 0.0390(18) Uani 1 1 d . . . H11 H 1.0498 0.7407 0.9261 0.047 Uiso 1 1 calc R . . C20 C 1.2594(7) 0.8534(5) 0.8160(3) 0.046(2) Uani 1 1 d . . . H20 H 1.3413 0.8594 0.8286 0.055 Uiso 1 1 calc R . . N4 N -0.0896(5) 0.4228(3) 0.9861(2) 0.0256(11) Uani 1 1 d . . . C24 C 1.1098(7) 0.7868(3) 0.7631(2) 0.0246(12) Uani 1 1 d . . . C38 C -0.1944(6) 0.4547(5) 1.0699(3) 0.0363(15) Uani 1 1 d . . . H38A H -0.1148 0.4716 1.0835 0.054 Uiso 1 1 calc R . . H38B H -0.2432 0.4330 1.0979 0.054 Uiso 1 1 calc R . . H38C H -0.2394 0.4965 1.0552 0.054 Uiso 1 1 calc R . . C23 C 1.0195(6) 0.8391(4) 0.7788(3) 0.0287(14) Uani 1 1 d . . . H23 H 0.9370 0.8346 0.7666 0.034 Uiso 1 1 calc R . . C18 C 1.3272(6) 0.7474(4) 0.7640(3) 0.0319(15) Uani 1 1 d . . . H18 H 1.4098 0.7541 0.7755 0.038 Uiso 1 1 calc R . . C42 C -0.0003(7) 0.1941(4) 1.0762(3) 0.0407(19) Uani 1 1 d . . . H42 H 0.0460 0.1519 1.0858 0.049 Uiso 1 1 calc R . . C19 C 1.2341(6) 0.7956(4) 0.7817(3) 0.0293(14) Uani 1 1 d . . . C22 C 1.0495(7) 0.8952(4) 0.8108(3) 0.0417(19) Uani 1 1 d . . . H22 H 0.9887 0.9310 0.8192 0.050 Uiso 1 1 calc R . . C21 C 1.1695(9) 0.9016(5) 0.8320(4) 0.052(2) Uani 1 1 d . . . H21 H 1.1875 0.9386 0.8568 0.063 Uiso 1 1 calc R . . C41 C -0.0056(7) 0.2535(5) 1.1087(3) 0.0420(19) Uani 1 1 d . . . H41 H 0.0326 0.2509 1.1416 0.050 Uiso 1 1 calc R . . C15 C 1.0845(6) 0.7262(4) 0.7289(3) 0.0270(14) Uani 1 1 d . . . C16 C 1.1797(6) 0.6802(4) 0.7135(3) 0.0268(14) Uani 1 1 d . . . H16 H 1.1636 0.6402 0.6910 0.032 Uiso 1 1 calc R . . C17 C 1.3023(6) 0.6934(4) 0.7318(3) 0.0281(14) Uani 1 1 d . . . H17 H 1.3675 0.6624 0.7204 0.034 Uiso 1 1 calc R . . C14 C 0.9398(7) 0.6618(4) 0.6642(3) 0.0355(16) Uani 1 1 d . . . H14A H 0.9693 0.6126 0.6735 0.053 Uiso 1 1 calc R . . H14B H 0.9892 0.6809 0.6355 0.053 Uiso 1 1 calc R . . H14C H 0.8528 0.6590 0.6538 0.053 Uiso 1 1 calc R . . F3 F 0.3770(5) 0.5475(3) 0.65678(15) 0.0537(12) Uani 1 1 d . . . F1 F 0.4185(7) 0.4353(2) 0.64214(17) 0.074(2) Uani 1 1 d . . . F2 F 0.5398(5) 0.5021(4) 0.6878(2) 0.0741(18) Uani 1 1 d . . . C49 C 0.4229(8) 0.4873(4) 0.6775(3) 0.0370(18) Uani 1 1 d . . . F4 F 0.3603(5) 0.6408(3) 1.09704(17) 0.0603(15) Uani 1 1 d . . . F6 F 0.2807(7) 0.5455(5) 1.0597(3) 0.093(2) Uani 1 1 d . . . O5 O 0.5436(8) 0.5546(8) 1.0349(3) 0.124(4) Uani 1 1 d . . . F5 F 0.2435(6) 0.6502(6) 1.0295(3) 0.120(4) Uani 1 1 d . . . O6 O 0.5096(12) 0.6764(5) 1.0061(3) 0.126(5) Uani 1 1 d . . . C50 C 0.3319(10) 0.6090(6) 1.0515(3) 0.052(2) Uani 1 1 d . . . O7 O 0.303(3) 0.8339(14) 0.9874(10) 0.289(11) Uani 1 1 d U . . C51 C 0.431(2) 0.8323(12) 0.9688(8) 0.152(8) Uani 1 1 d U . . H51A H 0.4506 0.8790 0.9517 0.227 Uiso 1 1 calc R . . H51B H 0.4411 0.7918 0.9441 0.227 Uiso 1 1 calc R . . H51C H 0.4874 0.8249 0.9980 0.227 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 C7 0.020(3) 0.023(3) 0.042(4) 0.001(3) 0.003(3) -0.001(2) C31 0.026(4) 0.029(3) 0.037(4) 0.008(3) -0.005(3) 0.002(3) C35 0.054(5) 0.065(6) 0.027(4) -0.012(4) -0.004(4) 0.026(5) C12 0.030(3) 0.038(4) 0.034(4) 0.003(3) 0.007(3) 0.013(3) C34 0.049(5) 0.036(4) 0.022(3) 0.001(3) -0.016(3) 0.009(3) Hg1 0.01455(9) 0.02168(10) 0.02853(10) 0.00831(10) -0.00007(10) -0.00232(9) S1 0.0342(8) 0.0377(10) 0.0282(8) 0.0042(7) -0.0067(7) -0.0151(8) N5 0.021(2) 0.021(2) 0.030(3) 0.008(2) 0.001(2) 0.004(2) C27 0.025(3) 0.022(3) 0.026(3) 0.005(2) -0.007(2) 0.000(2) C30 0.022(3) 0.022(3) 0.039(3) 0.008(2) -0.004(3) -0.003(3) C5 0.027(3) 0.023(3) 0.045(4) -0.002(3) 0.000(4) 0.001(3) N2 0.023(3) 0.020(3) 0.032(3) 0.007(2) 0.004(2) 0.003(2) C46 0.045(5) 0.039(4) 0.034(4) -0.001(3) 0.010(3) -0.009(4) C48 0.017(3) 0.029(3) 0.040(4) 0.003(3) 0.000(3) -0.005(3) C4 0.023(3) 0.033(4) 0.035(4) 0.006(3) 0.002(3) -0.001(3) C2 0.015(3) 0.032(4) 0.032(3) 0.006(3) -0.004(3) 0.005(3) C26 0.017(3) 0.029(3) 0.022(3) 0.007(2) -0.004(2) 0.002(3) C45 0.055(5) 0.035(4) 0.051(5) -0.006(3) 0.026(4) -0.016(4) C44 0.040(4) 0.033(4) 0.060(5) 0.009(4) 0.022(4) -0.002(3) C6 0.020(3) 0.020(3) 0.047(4) 0.011(3) 0.000(3) 0.003(3) C28 0.029(3) 0.028(3) 0.025(3) 0.003(3) -0.004(3) 0.008(3) C47 0.023(3) 0.040(4) 0.026(3) 0.004(3) 0.004(3) 0.003(3) C3 0.021(3) 0.026(3) 0.028(3) 0.006(3) 0.001(2) 0.002(2) C40 0.034(4) 0.040(4) 0.030(4) 0.010(3) -0.002(3) -0.013(3) C39 0.016(3) 0.034(3) 0.028(3) 0.007(3) 0.004(3) -0.006(3) C43 0.026(3) 0.030(4) 0.045(4) 0.014(3) 0.012(3) -0.003(3) C29 0.025(3) 0.026(3) 0.031(3) 0.009(3) -0.006(3) -0.002(3) S2 0.0287(9) 0.0617(13) 0.0288(9) -0.0137(9) -0.0022(7) -0.0048(9) N6 0.026(3) 0.021(2) 0.029(2) 0.009(2) -0.008(3) -0.0042(19) O1 0.044(3) 0.032(2) 0.026(2) 0.0004(18) 0.005(2) 0.000(2) N3 0.026(3) 0.027(3) 0.033(3) 0.011(3) 0.003(3) 0.002(2) C9 0.024(3) 0.024(3) 0.030(3) 0.002(2) 0.003(3) -0.002(3) C25 0.020(3) 0.030(4) 0.024(3) 0.008(2) -0.001(2) -0.004(2) O4 0.037(3) 0.076(4) 0.030(3) -0.026(3) 0.005(2) -0.012(3) C32 0.032(3) 0.023(3) 0.025(3) 0.007(3) -0.002(2) -0.001(3) C33 0.031(3) 0.018(3) 0.032(3) 0.009(3) 0.003(3) 0.000(3) O3 0.128(6) 0.031(3) 0.033(3) -0.002(2) -0.021(4) -0.004(4) O2 0.038(4) 0.171(9) 0.080(5) 0.040(6) -0.021(3) -0.051(5) C10 0.032(4) 0.032(4) 0.035(4) 0.008(3) 0.001(3) -0.001(3) C37 0.015(3) 0.035(4) 0.027(3) 0.007(3) 0.000(2) -0.006(3) C36 0.033(4) 0.069(6) 0.032(4) 0.008(4) -0.003(3) 0.023(4) N1 0.019(3) 0.028(3) 0.028(3) 0.006(2) 0.002(2) 0.001(2) C8 0.027(3) 0.021(3) 0.031(3) 0.006(3) 0.001(3) 0.004(3) C13 0.024(3) 0.028(4) 0.023(3) -0.005(3) 0.001(3) -0.006(3) C1 0.022(3) 0.027(3) 0.029(3) 0.010(3) 0.000(3) -0.008(3) C11 0.043(4) 0.042(4) 0.032(4) -0.004(3) -0.004(3) 0.011(3) C20 0.031(4) 0.043(5) 0.063(5) -0.003(4) -0.017(4) 0.001(3) N4 0.018(3) 0.031(3) 0.027(3) 0.006(2) -0.002(2) -0.002(2) C24 0.023(3) 0.021(3) 0.029(3) 0.000(2) 0.004(3) 0.000(3) C38 0.033(3) 0.036(4) 0.040(4) 0.001(4) 0.006(3) -0.002(4) C23 0.023(3) 0.028(4) 0.035(4) 0.000(3) -0.004(3) 0.001(3) C18 0.017(3) 0.034(4) 0.045(4) 0.015(3) -0.002(3) 0.005(3) C42 0.032(4) 0.030(4) 0.060(5) 0.019(4) 0.003(4) -0.003(3) C19 0.023(3) 0.031(4) 0.033(4) 0.008(3) -0.002(3) 0.003(3) C22 0.027(4) 0.033(4) 0.065(6) -0.014(4) -0.007(4) 0.003(3) C21 0.051(5) 0.040(5) 0.066(6) -0.019(4) -0.019(5) 0.000(4) C41 0.033(4) 0.048(5) 0.044(4) 0.025(4) -0.009(3) -0.005(3) C15 0.023(3) 0.028(3) 0.030(3) 0.009(3) 0.003(3) -0.003(3) C16 0.026(3) 0.026(3) 0.029(3) 0.002(3) 0.007(3) -0.004(3) C17 0.024(3) 0.025(3) 0.036(4) 0.007(3) 0.008(3) 0.003(3) C14 0.033(4) 0.037(4) 0.036(4) -0.006(3) 0.002(3) -0.005(3) F3 0.092(4) 0.036(2) 0.032(2) 0.0103(19) 0.007(2) 0.004(3) F1 0.164(6) 0.030(3) 0.030(2) -0.0061(18) 0.003(3) -0.001(3) F2 0.046(3) 0.107(5) 0.070(4) -0.006(3) 0.023(3) 0.000(3) C49 0.054(5) 0.031(4) 0.026(3) -0.002(3) 0.002(3) 0.000(3) F4 0.080(4) 0.068(3) 0.033(2) -0.019(2) 0.011(2) -0.005(3) F6 0.092(5) 0.100(5) 0.089(4) -0.026(4) 0.048(4) -0.040(5) O5 0.063(5) 0.229(13) 0.082(6) -0.008(7) -0.020(4) 0.077(7) F5 0.065(4) 0.229(11) 0.065(4) -0.010(5) -0.006(3) 0.087(6) O6 0.204(12) 0.112(7) 0.062(5) -0.045(5) 0.057(6) -0.104(8) C50 0.062(6) 0.059(6) 0.035(4) -0.017(4) 0.010(4) 0.005(5) O7 0.266(14) 0.269(14) 0.332(14) -0.003(9) -0.028(10) -0.005(9) C51 0.181(12) 0.137(11) 0.137(10) -0.001(8) 0.000(9) 0.000(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C7 N1 1.460(8) . ? C7 C8 1.516(9) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C31 N4 1.468(8) . ? C31 C32 1.528(9) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C35 C34 1.366(11) . ? C35 C36 1.376(11) . ? C35 H35 0.9500 . ? C12 C11 1.366(11) . ? C12 C8 1.378(10) . ? C12 H12 0.9500 . ? C34 N6 1.333(9) . ? C34 H34 0.9500 . ? Hg1 N5 2.237(5) . ? Hg1 N2 2.238(5) . ? Hg1 N3 2.406(5) 1_455 ? Hg1 N6 2.467(5) 1_655 ? Hg1 O1 2.504(4) . ? Hg1 O4 2.613(5) . ? S1 O2 1.397(6) . ? S1 O1 1.438(5) . ? S1 O3 1.441(6) . ? S1 C49 1.832(8) . ? N5 C28 1.312(9) . ? N5 C27 1.357(8) . ? C27 C26 1.384(9) . ? C27 H27 0.9500 . ? C30 C29 1.371(9) . ? C30 C26 1.395(9) . ? C30 H30 0.9500 . ? C5 C4 1.379(9) . ? C5 C6 1.382(10) . ? C5 H5 0.9500 . ? N2 C4 1.316(9) . ? N2 C3 1.355(8) . ? C46 C47 1.366(11) . ? C46 C45 1.412(12) . ? C46 H46 0.9500 . ? C48 C43 1.423(10) . ? C48 C47 1.423(10) . ? C48 C39 1.435(10) . ? C4 H4 0.9500 . ? C2 C3 1.366(9) . ? C2 C6 1.391(10) . ? C2 C1 1.496(9) . ? C26 C25 1.518(9) . ? C45 C44 1.315(12) . ? C45 H45 0.9500 . ? C44 C43 1.416(12) . ? C44 H44 0.9500 . ? C6 H6 0.9500 . ? C28 C29 1.388(9) . ? C28 H28 0.9500 . ? C47 H47 0.9500 . ? C3 H3 0.9500 . ? C40 C39 1.361(9) . ? C40 C41 1.389(11) . ? C40 H40 0.9500 . ? C39 C37 1.519(9) . ? C43 C42 1.401(11) . ? C29 H29 0.9500 . ? S2 O6 1.380(8) . ? S2 O4 1.410(5) . ? S2 O5 1.431(10) . ? S2 C50 1.803(9) . ? N6 C33 1.335(8) . ? N6 Hg1 2.467(5) 1_455 ? N3 C10 1.322(9) . ? N3 C9 1.336(9) . ? N3 Hg1 2.406(5) 1_655 ? C9 C8 1.378(9) . ? C9 H9 0.9500 . ? C25 N4 1.462(8) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C32 C33 1.382(9) . ? C32 C36 1.395(10) . ? C33 H33 0.9500 . ? C10 C11 1.392(10) . ? C10 H10 0.9500 . ? C37 N4 1.490(8) . ? C37 C38 1.514(10) . ? C37 H37 1.0000 . ? C36 H36 0.9500 . ? N1 C1 1.457(8) . ? N1 C13 1.500(8) . ? C13 C15 1.518(9) . ? C13 C14 1.549(9) . ? C13 H13 1.0000 . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C11 H11 0.9500 . ? C20 C21 1.374(12) . ? C20 C19 1.404(11) . ? C20 H20 0.9500 . ? C24 C23 1.423(9) . ? C24 C19 1.437(10) . ? C24 C15 1.440(9) . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C23 C22 1.354(10) . ? C23 H23 0.9500 . ? C18 C17 1.317(10) . ? C18 C19 1.411(10) . ? C18 H18 0.9500 . ? C42 C41 1.370(12) . ? C42 H42 0.9500 . ? C22 C21 1.414(11) . ? C22 H22 0.9500 . ? C21 H21 0.9500 . ? C41 H41 0.9500 . ? C15 C16 1.385(9) . ? C16 C17 1.428(10) . ? C16 H16 0.9500 . ? C17 H17 0.9500 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? F3 C49 1.316(9) . ? F1 C49 1.317(8) . ? F2 C49 1.320(10) . ? F4 C50 1.352(9) . ? F6 C50 1.298(12) . ? F5 C50 1.342(12) . ? O7 C51 1.47(3) . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C7 C8 112.2(5) . . ? N1 C7 H7A 109.2 . . ? C8 C7 H7A 109.2 . . ? N1 C7 H7B 109.2 . . ? C8 C7 H7B 109.2 . . ? H7A C7 H7B 107.9 . . ? N4 C31 C32 113.0(6) . . ? N4 C31 H31A 109.0 . . ? C32 C31 H31A 109.0 . . ? N4 C31 H31B 109.0 . . ? C32 C31 H31B 109.0 . . ? H31A C31 H31B 107.8 . . ? C34 C35 C36 117.8(7) . . ? C34 C35 H35 121.1 . . ? C36 C35 H35 121.1 . . ? C11 C12 C8 120.0(6) . . ? C11 C12 H12 120.0 . . ? C8 C12 H12 120.0 . . ? N6 C34 C35 123.7(7) . . ? N6 C34 H34 118.2 . . ? C35 C34 H34 118.2 . . ? N5 Hg1 N2 172.28(19) . . ? N5 Hg1 N3 85.63(18) . 1_455 ? N2 Hg1 N3 94.73(18) . 1_455 ? N5 Hg1 N6 96.60(17) . 1_655 ? N2 Hg1 N6 83.04(17) . 1_655 ? N3 Hg1 N6 177.77(17) 1_455 1_655 ? N5 Hg1 O1 97.98(18) . . ? N2 Hg1 O1 89.72(18) . . ? N3 Hg1 O1 91.5(2) 1_455 . ? N6 Hg1 O1 88.31(18) 1_655 . ? N5 Hg1 O4 82.96(19) . . ? N2 Hg1 O4 89.34(19) . . ? N3 Hg1 O4 89.4(2) 1_455 . ? N6 Hg1 O4 90.74(19) 1_655 . ? O1 Hg1 O4 178.73(18) . . ? O2 S1 O1 115.9(5) . . ? O2 S1 O3 116.5(6) . . ? O1 S1 O3 113.1(3) . . ? O2 S1 C49 103.9(4) . . ? O1 S1 C49 101.6(3) . . ? O3 S1 C49 103.3(4) . . ? C28 N5 C27 119.0(6) . . ? C28 N5 Hg1 123.8(4) . . ? C27 N5 Hg1 117.2(4) . . ? N5 C27 C26 122.9(6) . . ? N5 C27 H27 118.5 . . ? C26 C27 H27 118.5 . . ? C29 C30 C26 119.7(6) . . ? C29 C30 H30 120.2 . . ? C26 C30 H30 120.2 . . ? C4 C5 C6 118.6(6) . . ? C4 C5 H5 120.7 . . ? C6 C5 H5 120.7 . . ? C4 N2 C3 119.2(6) . . ? C4 N2 Hg1 122.2(4) . . ? C3 N2 Hg1 118.6(4) . . ? C47 C46 C45 121.1(8) . . ? C47 C46 H46 119.4 . . ? C45 C46 H46 119.4 . . ? C43 C48 C47 117.2(6) . . ? C43 C48 C39 120.1(6) . . ? C47 C48 C39 122.6(6) . . ? N2 C4 C5 122.2(6) . . ? N2 C4 H4 118.9 . . ? C5 C4 H4 118.9 . . ? C3 C2 C6 117.6(6) . . ? C3 C2 C1 121.6(6) . . ? C6 C2 C1 120.8(6) . . ? C27 C26 C30 117.0(6) . . ? C27 C26 C25 121.4(6) . . ? C30 C26 C25 121.6(6) . . ? C44 C45 C46 119.6(8) . . ? C44 C45 H45 120.2 . . ? C46 C45 H45 120.2 . . ? C45 C44 C43 122.2(8) . . ? C45 C44 H44 118.9 . . ? C43 C44 H44 118.9 . . ? C5 C6 C2 119.8(6) . . ? C5 C6 H6 120.1 . . ? C2 C6 H6 120.1 . . ? N5 C28 C29 121.8(6) . . ? N5 C28 H28 119.1 . . ? C29 C28 H28 119.1 . . ? C46 C47 C48 120.4(7) . . ? C46 C47 H47 119.8 . . ? C48 C47 H47 119.8 . . ? N2 C3 C2 122.6(6) . . ? N2 C3 H3 118.7 . . ? C2 C3 H3 118.7 . . ? C39 C40 C41 122.2(7) . . ? C39 C40 H40 118.9 . . ? C41 C40 H40 118.9 . . ? C40 C39 C48 117.9(6) . . ? C40 C39 C37 121.6(6) . . ? C48 C39 C37 120.1(6) . . ? C42 C43 C44 122.0(7) . . ? C42 C43 C48 118.7(7) . . ? C44 C43 C48 119.3(7) . . ? C30 C29 C28 119.5(6) . . ? C30 C29 H29 120.2 . . ? C28 C29 H29 120.2 . . ? O6 S2 O4 116.9(5) . . ? O6 S2 O5 114.6(8) . . ? O4 S2 O5 111.7(6) . . ? O6 S2 C50 106.7(5) . . ? O4 S2 C50 102.7(4) . . ? O5 S2 C50 102.3(5) . . ? C34 N6 C33 118.0(6) . . ? C34 N6 Hg1 127.4(4) . 1_455 ? C33 N6 Hg1 114.6(4) . 1_455 ? S1 O1 Hg1 140.8(3) . . ? C10 N3 C9 118.8(6) . . ? C10 N3 Hg1 122.0(5) . 1_655 ? C9 N3 Hg1 119.1(4) . 1_655 ? N3 C9 C8 122.8(6) . . ? N3 C9 H9 118.6 . . ? C8 C9 H9 118.6 . . ? N4 C25 C26 108.2(5) . . ? N4 C25 H25A 110.1 . . ? C26 C25 H25A 110.1 . . ? N4 C25 H25B 110.1 . . ? C26 C25 H25B 110.1 . . ? H25A C25 H25B 108.4 . . ? S2 O4 Hg1 158.5(4) . . ? C33 C32 C36 117.0(6) . . ? C33 C32 C31 120.9(6) . . ? C36 C32 C31 122.0(6) . . ? N6 C33 C32 123.1(6) . . ? N6 C33 H33 118.4 . . ? C32 C33 H33 118.4 . . ? N3 C10 C11 122.1(7) . . ? N3 C10 H10 119.0 . . ? C11 C10 H10 119.0 . . ? N4 C37 C38 113.9(6) . . ? N4 C37 C39 107.7(5) . . ? C38 C37 C39 115.2(6) . . ? N4 C37 H37 106.5 . . ? C38 C37 H37 106.5 . . ? C39 C37 H37 106.5 . . ? C35 C36 C32 120.3(7) . . ? C35 C36 H36 119.8 . . ? C32 C36 H36 119.8 . . ? C1 N1 C7 114.2(5) . . ? C1 N1 C13 112.1(5) . . ? C7 N1 C13 114.4(5) . . ? C12 C8 C9 117.9(6) . . ? C12 C8 C7 121.0(6) . . ? C9 C8 C7 121.2(6) . . ? N1 C13 C15 110.0(5) . . ? N1 C13 C14 112.9(5) . . ? C15 C13 C14 114.2(6) . . ? N1 C13 H13 106.4 . . ? C15 C13 H13 106.4 . . ? C14 C13 H13 106.4 . . ? N1 C1 C2 111.4(5) . . ? N1 C1 H1A 109.4 . . ? C2 C1 H1A 109.4 . . ? N1 C1 H1B 109.4 . . ? C2 C1 H1B 109.4 . . ? H1A C1 H1B 108.0 . . ? C12 C11 C10 118.4(7) . . ? C12 C11 H11 120.8 . . ? C10 C11 H11 120.8 . . ? C21 C20 C19 122.1(7) . . ? C21 C20 H20 119.0 . . ? C19 C20 H20 119.0 . . ? C25 N4 C31 111.7(5) . . ? C25 N4 C37 114.1(5) . . ? C31 N4 C37 113.9(5) . . ? C23 C24 C19 118.1(6) . . ? C23 C24 C15 123.8(6) . . ? C19 C24 C15 118.0(6) . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C22 C23 C24 121.0(7) . . ? C22 C23 H23 119.5 . . ? C24 C23 H23 119.5 . . ? C17 C18 C19 121.5(7) . . ? C17 C18 H18 119.3 . . ? C19 C18 H18 119.3 . . ? C41 C42 C43 120.3(7) . . ? C41 C42 H42 119.9 . . ? C43 C42 H42 119.9 . . ? C20 C19 C18 122.1(7) . . ? C20 C19 C24 118.6(6) . . ? C18 C19 C24 119.3(6) . . ? C23 C22 C21 121.3(7) . . ? C23 C22 H22 119.3 . . ? C21 C22 H22 119.3 . . ? C20 C21 C22 118.7(7) . . ? C20 C21 H21 120.6 . . ? C22 C21 H21 120.6 . . ? C42 C41 C40 120.7(7) . . ? C42 C41 H41 119.7 . . ? C40 C41 H41 119.7 . . ? C16 C15 C24 119.8(6) . . ? C16 C15 C13 121.6(6) . . ? C24 C15 C13 118.6(6) . . ? C15 C16 C17 119.6(6) . . ? C15 C16 H16 120.2 . . ? C17 C16 H16 120.2 . . ? C18 C17 C16 121.7(6) . . ? C18 C17 H17 119.1 . . ? C16 C17 H17 119.1 . . ? 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 . . ? F3 C49 F1 107.5(6) . . ? F3 C49 F2 106.0(7) . . ? F1 C49 F2 108.8(7) . . ? F3 C49 S1 111.3(5) . . ? F1 C49 S1 112.2(5) . . ? F2 C49 S1 110.9(5) . . ? F6 C50 F5 105.2(10) . . ? F6 C50 F4 109.5(8) . . ? F5 C50 F4 107.0(8) . . ? F6 C50 S2 114.2(6) . . ? F5 C50 S2 109.0(7) . . ? F4 C50 S2 111.5(7) . . ? O7 C51 H51A 109.5 . . ? O7 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? O7 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 3.126 _refine_diff_density_min -1.965 _refine_diff_density_rms 0.134 data_2b/HgCl2 _database_code_depnum_ccdc_archive 'CCDC 910369' #TrackingRef '15353_web_deposit_cif_file_0_YoichiHabata_1352699762.All_complexes_1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H21 Cl2 Hg N3' _chemical_formula_weight 574.89 _chemical_absolute_configuration syn 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Hg Hg -2.3894 9.2266 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' _cell_length_a 25.6810(15) _cell_length_b 12.3916(7) _cell_length_c 17.8922(10) _cell_angle_alpha 90.00 _cell_angle_beta 133.4980(10) _cell_angle_gamma 90.00 _cell_volume 4130.3(4) _cell_formula_units_Z 8 _cell_measurement_temperature 90 _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.37 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.849 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2208 _exptl_absorpt_coefficient_mu 7.720 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.1604 _exptl_absorpt_correction_T_max 0.2556 _exptl_absorpt_process_details 'SADABS; Sheldrick, 1996' _exptl_special_details ; ? ; _diffrn_ambient_temperature 90 _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 8.366 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15282 _diffrn_reflns_av_R_equivalents 0.0199 _diffrn_reflns_av_sigmaI/netI 0.0491 _diffrn_reflns_limit_h_min -34 _diffrn_reflns_limit_h_max 34 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.57 _diffrn_reflns_theta_max 28.32 _reflns_number_total 9158 _reflns_number_gt 8745 _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^)+(0.0000P)^2^+1.3643P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.005(4) _refine_ls_number_reflns 9158 _refine_ls_number_parameters 471 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0230 _refine_ls_R_factor_gt 0.0215 _refine_ls_wR_factor_ref 0.0538 _refine_ls_wR_factor_gt 0.0498 _refine_ls_goodness_of_fit_ref 0.994 _refine_ls_restrained_S_all 0.994 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.6013(2) -0.0179(3) 0.1452(3) 0.0193(8) Uani 1 1 d . . . H1A H 0.5534 -0.0495 0.0882 0.023 Uiso 1 1 calc R . . H1B H 0.6354 -0.0496 0.1427 0.023 Uiso 1 1 calc R . . C2 C 0.5978(2) 0.1021(3) 0.1298(3) 0.0163(7) Uani 1 1 d . . . C3 C 0.5909(2) 0.1728(3) 0.1832(3) 0.0193(8) Uani 1 1 d . . . H3 H 0.5904 0.1437 0.2319 0.023 Uiso 1 1 calc R . . C4 C 0.5855(2) 0.3217(4) 0.1006(3) 0.0238(9) Uani 1 1 d . . . H4 H 0.5815 0.3977 0.0907 0.029 Uiso 1 1 calc R . . C5 C 0.5918(2) 0.2580(4) 0.0443(3) 0.0266(10) Uani 1 1 d . . . H5 H 0.5918 0.2896 -0.0041 0.032 Uiso 1 1 calc R . . C6 C 0.5981(2) 0.1469(4) 0.0585(3) 0.0222(8) Uani 1 1 d . . . H6 H 0.6025 0.1019 0.0202 0.027 Uiso 1 1 calc R . . C7 C 0.7026(2) -0.0412(3) 0.3271(3) 0.0198(8) Uani 1 1 d . . . H7A H 0.7202 0.0211 0.3150 0.024 Uiso 1 1 calc R . . H7B H 0.7233 -0.1075 0.3254 0.024 Uiso 1 1 calc R . . C8 C 0.7289(2) -0.0303(3) 0.4327(3) 0.0169(8) Uani 1 1 d . . . C9 C 0.7937(2) -0.0788(3) 0.5169(3) 0.0195(8) Uani 1 1 d . . . H9 H 0.8165 -0.1262 0.5051 0.023 Uiso 1 1 calc R . . C10 C 0.7931(2) 0.0045(4) 0.6314(3) 0.0226(9) Uani 1 1 d . . . H10 H 0.8160 0.0179 0.7005 0.027 Uiso 1 1 calc R . . C11 C 0.7278(2) 0.0538(4) 0.5526(3) 0.0242(9) Uani 1 1 d . . . H11 H 0.7056 0.0983 0.5672 0.029 Uiso 1 1 calc R . . C12 C 0.6955(2) 0.0365(4) 0.4517(3) 0.0226(9) Uani 1 1 d . . . H12 H 0.6511 0.0701 0.3962 0.027 Uiso 1 1 calc R . . C13 C 0.5923(2) -0.1483(3) 0.2398(3) 0.0212(9) Uani 1 1 d . . . H13 H 0.6119 -0.1597 0.3106 0.025 Uiso 1 1 calc R . . C14 C 0.6124(3) -0.2467(4) 0.2154(4) 0.0370(12) Uani 1 1 d . . . H14A H 0.5949 -0.2390 0.1467 0.055 Uiso 1 1 calc R . . H14B H 0.5907 -0.3107 0.2168 0.055 Uiso 1 1 calc R . . H14C H 0.6648 -0.2545 0.2666 0.055 Uiso 1 1 calc R . . C15 C 0.5111(2) -0.1290(4) 0.1690(3) 0.0225(8) Uani 1 1 d . . . C16 C 0.4602(3) -0.1926(4) 0.0828(3) 0.0331(11) Uani 1 1 d . . . H16 H 0.4749 -0.2513 0.0667 0.040 Uiso 1 1 calc R . . C17 C 0.3875(3) -0.1696(6) 0.0201(4) 0.0487(18) Uani 1 1 d . . . H17 H 0.3532 -0.2118 -0.0401 0.058 Uiso 1 1 calc R . . C18 C 0.3642(3) -0.0886(6) 0.0423(4) 0.0501(18) Uani 1 1 d . . . H18 H 0.3144 -0.0757 -0.0005 0.060 Uiso 1 1 calc R . . C19 C 0.4155(3) -0.0238(5) 0.1300(4) 0.0418(14) Uani 1 1 d . . . H19 H 0.4004 0.0337 0.1464 0.050 Uiso 1 1 calc R . . C20 C 0.4879(3) -0.0447(4) 0.1918(4) 0.0288(10) Uani 1 1 d . . . H20 H 0.5223 -0.0009 0.2507 0.035 Uiso 1 1 calc R . . C21 C 0.8630(2) 0.1860(4) 0.1764(3) 0.0252(9) Uani 1 1 d . . . H21A H 0.8752 0.1107 0.1748 0.030 Uiso 1 1 calc R . . H21B H 0.8993 0.2335 0.1887 0.030 Uiso 1 1 calc R . . C22 C 0.7899(2) 0.2130(4) 0.0715(3) 0.0211(8) Uani 1 1 d . . . C23 C 0.7697(2) 0.1688(3) -0.0163(3) 0.0209(8) Uani 1 1 d . . . H23 H 0.7987 0.1132 -0.0083 0.025 Uiso 1 1 calc R . . C24 C 0.6691(2) 0.2761(4) -0.1245(3) 0.0218(9) Uani 1 1 d . . . H24 H 0.6281 0.2994 -0.1921 0.026 Uiso 1 1 calc R . . C25 C 0.6837(2) 0.3217(4) -0.0410(3) 0.0210(8) Uani 1 1 d . . . H25 H 0.6520 0.3738 -0.0515 0.025 Uiso 1 1 calc R . . C26 C 0.7448(2) 0.2905(4) 0.0580(3) 0.0220(9) Uani 1 1 d . . . H26 H 0.7559 0.3217 0.1160 0.026 Uiso 1 1 calc R . . C27 C 0.9418(2) 0.2323(4) 0.3552(3) 0.0221(9) Uani 1 1 d . . . H27A H 0.9762 0.1962 0.3552 0.027 Uiso 1 1 calc R . . H27B H 0.9527 0.2082 0.4175 0.027 Uiso 1 1 calc R . . C28 C 0.9532(2) 0.3527(3) 0.3618(3) 0.0203(9) Uani 1 1 d . . . C29 C 0.8967(2) 0.4232(4) 0.3175(3) 0.0225(9) Uani 1 1 d . . . H29 H 0.8500 0.3940 0.2785 0.027 Uiso 1 1 calc R . . C30 C 0.9703(2) 0.5718(4) 0.3825(3) 0.0278(10) Uani 1 1 d . . . H30 H 0.9768 0.6478 0.3908 0.033 Uiso 1 1 calc R . . C31 C 1.0278(3) 0.5072(5) 0.4273(3) 0.0324(11) Uani 1 1 d . . . H31 H 1.0740 0.5379 0.4658 0.039 Uiso 1 1 calc R . . C32 C 1.0191(2) 0.3962(4) 0.4167(3) 0.0266(10) Uani 1 1 d . . . H32 H 1.0593 0.3507 0.4479 0.032 Uiso 1 1 calc R . . C33 C 0.8514(2) 0.0977(4) 0.2883(3) 0.0213(8) Uani 1 1 d . . . H33 H 0.8916 0.0453 0.3213 0.026 Uiso 1 1 calc R . . C34 C 0.7824(2) 0.0452(3) 0.1936(3) 0.0259(9) Uani 1 1 d . . . H34A H 0.7426 0.0963 0.1596 0.039 Uiso 1 1 calc R . . H34B H 0.7727 -0.0192 0.2142 0.039 Uiso 1 1 calc R . . H34C H 0.7873 0.0245 0.1459 0.039 Uiso 1 1 calc R . . C35 C 0.8468(2) 0.1281(3) 0.3664(3) 0.0227(9) Uani 1 1 d . . . C36 C 0.8004(3) 0.2084(4) 0.3438(4) 0.0333(11) Uani 1 1 d . . . H36 H 0.7713 0.2451 0.2796 0.040 Uiso 1 1 calc R . . C37 C 0.7964(4) 0.2357(5) 0.4151(5) 0.0499(17) Uani 1 1 d . . . H37 H 0.7636 0.2893 0.3992 0.060 Uiso 1 1 calc R . . C38 C 0.8405(4) 0.1840(6) 0.5092(5) 0.064(2) Uani 1 1 d . . . H38 H 0.8384 0.2038 0.5583 0.077 Uiso 1 1 calc R . . C39 C 0.8880(3) 0.1037(5) 0.5338(4) 0.0500(17) Uani 1 1 d . . . H39 H 0.9184 0.0692 0.5991 0.060 Uiso 1 1 calc R . . C40 C 0.8902(3) 0.0752(4) 0.4611(3) 0.0317(11) Uani 1 1 d . . . H40 H 0.9215 0.0192 0.4759 0.038 Uiso 1 1 calc R . . Cl1 Cl 0.47669(7) 0.51785(10) 0.13648(10) 0.0385(3) Uani 1 1 d . . . Cl2 Cl 0.54914(7) 0.23825(10) 0.33440(10) 0.0350(3) Uani 1 1 d . . . Cl3 Cl 0.65184(8) 0.28358(12) -0.36749(10) 0.0480(3) Uani 1 1 d . . . Cl4 Cl 0.78982(7) 0.00739(11) -0.16503(9) 0.0328(3) Uani 1 1 d . . . Hg1 Hg 0.556823(9) 0.378233(11) 0.249199(12) 0.02372(4) Uani 1 1 d . . . Hg2 Hg 0.696145(10) 0.138640(12) -0.251580(12) 0.02533(5) Uani 1 1 d . . . N1 N 0.62402(18) -0.0462(3) 0.2438(2) 0.0182(7) Uani 1 1 d . . . N2 N 0.58487(19) 0.2801(3) 0.1691(3) 0.0212(7) Uani 1 1 d . . . N3 N 0.82491(18) -0.0603(3) 0.6144(2) 0.0207(7) Uani 1 1 d . . . N4 N 0.86844(18) 0.1973(3) 0.2632(2) 0.0189(7) Uani 1 1 d . . . N5 N 0.71148(19) 0.2002(3) -0.1120(3) 0.0214(7) Uani 1 1 d . . . N6 N 0.9046(2) 0.5306(3) 0.3270(3) 0.0242(8) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.018(2) 0.024(2) 0.0132(18) -0.0031(14) 0.0095(17) -0.0035(16) C2 0.0105(18) 0.0238(19) 0.0085(16) -0.0003(14) 0.0042(15) -0.0019(15) C3 0.016(2) 0.024(2) 0.0139(18) 0.0011(14) 0.0086(17) -0.0013(15) C4 0.018(2) 0.023(2) 0.021(2) 0.0066(16) 0.0097(18) -0.0012(17) C5 0.016(2) 0.041(3) 0.023(2) 0.0146(18) 0.0136(19) 0.0060(19) C6 0.016(2) 0.035(2) 0.0138(17) 0.0018(17) 0.0097(17) 0.0011(19) C7 0.017(2) 0.024(2) 0.0167(19) -0.0008(15) 0.0111(17) -0.0004(16) C8 0.0146(19) 0.021(2) 0.0118(17) -0.0025(14) 0.0076(16) -0.0038(15) C9 0.015(2) 0.0194(18) 0.021(2) -0.0022(15) 0.0108(18) -0.0024(16) C10 0.022(2) 0.027(2) 0.0137(18) -0.0015(16) 0.0102(18) -0.0034(18) C11 0.019(2) 0.033(2) 0.020(2) -0.0050(17) 0.0134(19) -0.0023(19) C12 0.015(2) 0.029(2) 0.0167(19) 0.0008(16) 0.0082(18) 0.0002(17) C13 0.021(2) 0.021(2) 0.0176(19) 0.0018(14) 0.0115(18) -0.0012(16) C14 0.032(3) 0.020(2) 0.042(3) -0.004(2) 0.019(2) -0.003(2) C15 0.0169(19) 0.026(2) 0.0169(18) 0.0058(17) 0.0087(16) -0.0032(19) C16 0.033(3) 0.040(3) 0.023(2) 0.0020(19) 0.018(2) -0.012(2) C17 0.023(3) 0.080(4) 0.019(2) 0.010(2) 0.005(2) -0.028(3) C18 0.018(3) 0.085(5) 0.039(3) 0.039(3) 0.017(3) 0.008(3) C19 0.036(3) 0.050(3) 0.052(3) 0.027(3) 0.035(3) 0.016(3) C20 0.027(2) 0.035(3) 0.029(2) 0.0120(19) 0.021(2) 0.002(2) C21 0.019(2) 0.039(3) 0.019(2) 0.0009(17) 0.0136(19) 0.0033(19) C22 0.015(2) 0.033(2) 0.0142(18) 0.0060(16) 0.0093(17) 0.0034(17) C23 0.022(2) 0.023(2) 0.023(2) 0.0054(15) 0.0175(19) 0.0040(16) C24 0.017(2) 0.030(2) 0.018(2) 0.0028(16) 0.0117(18) 0.0008(18) C25 0.019(2) 0.026(2) 0.020(2) 0.0017(16) 0.0140(19) 0.0015(17) C26 0.022(2) 0.028(2) 0.019(2) 0.0006(16) 0.0154(19) 0.0026(18) C27 0.0088(19) 0.034(2) 0.0151(19) 0.0061(16) 0.0048(17) 0.0017(17) C28 0.017(2) 0.032(2) 0.0135(18) 0.0037(15) 0.0109(17) 0.0003(16) C29 0.016(2) 0.031(2) 0.0159(19) -0.0025(16) 0.0094(17) -0.0064(17) C30 0.025(2) 0.039(3) 0.019(2) -0.0043(18) 0.015(2) -0.013(2) C31 0.023(2) 0.051(3) 0.024(2) -0.003(2) 0.016(2) -0.012(2) C32 0.023(2) 0.040(3) 0.019(2) 0.0021(17) 0.0147(19) -0.0051(19) C33 0.021(2) 0.026(2) 0.0190(19) -0.0018(16) 0.0148(19) -0.0018(18) C34 0.029(2) 0.022(2) 0.019(2) -0.0036(16) 0.014(2) -0.0025(18) C35 0.027(2) 0.023(2) 0.0229(19) -0.0064(16) 0.0188(19) -0.0104(18) C36 0.044(3) 0.027(2) 0.044(3) -0.010(2) 0.037(3) -0.010(2) C37 0.069(4) 0.039(3) 0.081(5) -0.032(3) 0.067(4) -0.032(3) C38 0.097(6) 0.075(5) 0.056(4) -0.046(3) 0.067(4) -0.065(4) C39 0.059(4) 0.063(4) 0.031(3) -0.015(3) 0.032(3) -0.041(3) C40 0.028(3) 0.040(3) 0.020(2) -0.0034(19) 0.014(2) -0.017(2) Cl1 0.0265(6) 0.0243(5) 0.0418(7) 0.0102(5) 0.0147(6) 0.0058(5) Cl2 0.0448(7) 0.0305(6) 0.0385(6) 0.0055(5) 0.0320(6) 0.0006(5) Cl3 0.0545(9) 0.0437(7) 0.0360(7) 0.0154(6) 0.0274(7) -0.0007(7) Cl4 0.0277(6) 0.0445(7) 0.0311(6) 0.0066(5) 0.0222(5) 0.0106(5) Hg1 0.02066(8) 0.02021(7) 0.01780(7) -0.00021(6) 0.00846(6) 0.00092(7) Hg2 0.02752(9) 0.03051(9) 0.01710(7) 0.00076(6) 0.01502(7) 0.00294(7) N1 0.0169(17) 0.0182(16) 0.0144(16) 0.0012(12) 0.0088(14) -0.0024(14) N2 0.0160(18) 0.0246(18) 0.0149(17) 0.0030(14) 0.0076(15) -0.0008(15) N3 0.0155(17) 0.0241(18) 0.0160(16) 0.0013(13) 0.0083(15) -0.0041(14) N4 0.0107(16) 0.0278(19) 0.0116(15) 0.0008(13) 0.0051(14) 0.0000(14) N5 0.0203(18) 0.0280(19) 0.0193(17) 0.0005(14) 0.0149(16) 0.0009(15) N6 0.022(2) 0.035(2) 0.0157(17) 0.0004(14) 0.0132(16) -0.0044(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.469(5) . ? C1 C2 1.503(6) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C6 1.395(5) . ? C2 C3 1.396(5) . ? C3 N2 1.342(5) . ? C3 H3 0.9500 . ? C4 N2 1.340(5) . ? C4 C5 1.375(6) . ? C4 H4 0.9500 . ? C5 C6 1.389(7) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 N1 1.469(5) . ? C7 C8 1.512(5) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C12 1.391(6) . ? C8 C9 1.397(5) . ? C9 N3 1.346(5) . ? C9 H9 0.9500 . ? C10 N3 1.321(6) . ? C10 C11 1.385(6) . ? C10 H10 0.9500 . ? C11 C12 1.389(5) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 N1 1.480(5) . ? C13 C14 1.503(6) . ? C13 C15 1.540(6) . ? C13 H13 1.0000 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C16 1.391(6) . ? C15 C20 1.396(7) . ? C16 C17 1.393(8) . ? C16 H16 0.9500 . ? C17 C18 1.361(9) . ? C17 H17 0.9500 . ? C18 C19 1.412(9) . ? C18 H18 0.9500 . ? C19 C20 1.384(7) . ? C19 H19 0.9500 . ? C20 H20 0.9500 . ? C21 N4 1.469(5) . ? C21 C22 1.519(6) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C23 1.384(5) . ? C22 C26 1.391(6) . ? C23 N5 1.340(5) . ? C23 H23 0.9500 . ? C24 N5 1.335(6) . ? C24 C25 1.386(5) . ? C24 H24 0.9500 . ? C25 C26 1.387(6) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C27 N4 1.475(5) . ? C27 C28 1.509(6) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 C32 1.352(6) . ? C28 C29 1.384(6) . ? C29 N6 1.340(6) . ? C29 H29 0.9500 . ? C30 N6 1.336(6) . ? C30 C31 1.355(7) . ? C30 H30 0.9500 . ? C31 C32 1.385(7) . ? C31 H31 0.9500 . ? C32 H32 0.9500 . ? C33 N4 1.479(5) . ? C33 C34 1.517(6) . ? C33 C35 1.527(5) . ? C33 H33 1.0000 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 C36 1.383(7) . ? C35 C40 1.394(6) . ? C36 C37 1.391(7) . ? C36 H36 0.9500 . ? C37 C38 1.378(10) . ? C37 H37 0.9500 . ? C38 C39 1.391(10) . ? C38 H38 0.9500 . ? C39 C40 1.385(7) . ? C39 H39 0.9500 . ? C40 H40 0.9500 . ? Cl1 Hg1 2.3626(12) . ? Cl2 Hg1 2.4054(12) . ? Cl3 Hg2 2.3607(12) . ? Cl4 Hg2 2.3879(12) . ? Hg1 N2 2.340(4) . ? Hg1 N3 2.358(3) 4_656 ? Hg2 N6 2.346(4) 4_645 ? Hg2 N5 2.371(3) . ? N3 Hg1 2.358(3) 4_646 ? N6 Hg2 2.346(4) 4_655 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 112.4(3) . . ? N1 C1 H1A 109.1 . . ? C2 C1 H1A 109.1 . . ? N1 C1 H1B 109.1 . . ? C2 C1 H1B 109.1 . . ? H1A C1 H1B 107.9 . . ? C6 C2 C3 117.3(4) . . ? C6 C2 C1 121.6(4) . . ? C3 C2 C1 121.0(3) . . ? N2 C3 C2 123.0(4) . . ? N2 C3 H3 118.5 . . ? C2 C3 H3 118.5 . . ? N2 C4 C5 122.0(4) . . ? N2 C4 H4 119.0 . . ? C5 C4 H4 119.0 . . ? C4 C5 C6 119.5(4) . . ? C4 C5 H5 120.2 . . ? C6 C5 H5 120.2 . . ? C5 C6 C2 119.3(4) . . ? C5 C6 H6 120.3 . . ? C2 C6 H6 120.3 . . ? N1 C7 C8 113.0(3) . . ? N1 C7 H7A 109.0 . . ? C8 C7 H7A 109.0 . . ? N1 C7 H7B 109.0 . . ? C8 C7 H7B 109.0 . . ? H7A C7 H7B 107.8 . . ? C12 C8 C9 118.0(3) . . ? C12 C8 C7 122.6(4) . . ? C9 C8 C7 119.0(4) . . ? N3 C9 C8 121.9(4) . . ? N3 C9 H9 119.1 . . ? C8 C9 H9 119.1 . . ? N3 C10 C11 122.7(4) . . ? N3 C10 H10 118.6 . . ? C11 C10 H10 118.6 . . ? C10 C11 C12 118.4(4) . . ? C10 C11 H11 120.8 . . ? C12 C11 H11 120.8 . . ? C11 C12 C8 119.5(4) . . ? C11 C12 H12 120.3 . . ? C8 C12 H12 120.3 . . ? N1 C13 C14 114.7(4) . . ? N1 C13 C15 107.3(3) . . ? C14 C13 C15 115.4(4) . . ? N1 C13 H13 106.3 . . ? C14 C13 H13 106.3 . . ? C15 C13 H13 106.3 . . ? 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 C20 119.0(4) . . ? C16 C15 C13 122.1(4) . . ? C20 C15 C13 118.9(4) . . ? C15 C16 C17 119.5(5) . . ? C15 C16 H16 120.3 . . ? C17 C16 H16 120.3 . . ? C18 C17 C16 122.0(5) . . ? C18 C17 H17 119.0 . . ? C16 C17 H17 119.0 . . ? C17 C18 C19 118.9(5) . . ? C17 C18 H18 120.6 . . ? C19 C18 H18 120.6 . . ? C20 C19 C18 119.6(5) . . ? C20 C19 H19 120.2 . . ? C18 C19 H19 120.2 . . ? C19 C20 C15 121.0(5) . . ? C19 C20 H20 119.5 . . ? C15 C20 H20 119.5 . . ? N4 C21 C22 115.0(3) . . ? N4 C21 H21A 108.5 . . ? C22 C21 H21A 108.5 . . ? N4 C21 H21B 108.5 . . ? C22 C21 H21B 108.5 . . ? H21A C21 H21B 107.5 . . ? C23 C22 C26 117.3(4) . . ? C23 C22 C21 119.6(4) . . ? C26 C22 C21 122.7(4) . . ? N5 C23 C22 123.5(4) . . ? N5 C23 H23 118.2 . . ? C22 C23 H23 118.2 . . ? N5 C24 C25 121.5(4) . . ? N5 C24 H24 119.3 . . ? C25 C24 H24 119.3 . . ? C24 C25 C26 119.4(4) . . ? C24 C25 H25 120.3 . . ? C26 C25 H25 120.3 . . ? C25 C26 C22 119.4(4) . . ? C25 C26 H26 120.3 . . ? C22 C26 H26 120.3 . . ? N4 C27 C28 114.1(3) . . ? N4 C27 H27A 108.7 . . ? C28 C27 H27A 108.7 . . ? N4 C27 H27B 108.7 . . ? C28 C27 H27B 108.7 . . ? H27A C27 H27B 107.6 . . ? C32 C28 C29 117.3(4) . . ? C32 C28 C27 122.0(4) . . ? C29 C28 C27 120.5(4) . . ? N6 C29 C28 123.1(4) . . ? N6 C29 H29 118.4 . . ? C28 C29 H29 118.4 . . ? N6 C30 C31 121.2(5) . . ? N6 C30 H30 119.4 . . ? C31 C30 H30 119.4 . . ? C30 C31 C32 119.8(5) . . ? C30 C31 H31 120.1 . . ? C32 C31 H31 120.1 . . ? C28 C32 C31 120.0(5) . . ? C28 C32 H32 120.0 . . ? C31 C32 H32 120.0 . . ? N4 C33 C34 112.4(3) . . ? N4 C33 C35 107.3(3) . . ? C34 C33 C35 111.2(4) . . ? N4 C33 H33 108.6 . . ? C34 C33 H33 108.6 . . ? C35 C33 H33 108.6 . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C36 C35 C40 120.1(4) . . ? C36 C35 C33 120.2(4) . . ? C40 C35 C33 119.8(4) . . ? C35 C36 C37 120.0(5) . . ? C35 C36 H36 120.0 . . ? C37 C36 H36 120.0 . . ? C38 C37 C36 119.3(6) . . ? C38 C37 H37 120.3 . . ? C36 C37 H37 120.3 . . ? C37 C38 C39 121.6(5) . . ? C37 C38 H38 119.2 . . ? C39 C38 H38 119.2 . . ? C40 C39 C38 118.6(5) . . ? C40 C39 H39 120.7 . . ? C38 C39 H39 120.7 . . ? C39 C40 C35 120.4(5) . . ? C39 C40 H40 119.8 . . ? C35 C40 H40 119.8 . . ? N2 Hg1 N3 94.70(12) . 4_656 ? N2 Hg1 Cl1 108.20(9) . . ? N3 Hg1 Cl1 113.05(9) 4_656 . ? N2 Hg1 Cl2 101.97(10) . . ? N3 Hg1 Cl2 100.73(9) 4_656 . ? Cl1 Hg1 Cl2 131.75(5) . . ? N6 Hg2 Cl3 104.78(10) 4_645 . ? N6 Hg2 N5 96.15(12) 4_645 . ? Cl3 Hg2 N5 108.10(10) . . ? N6 Hg2 Cl4 101.80(10) 4_645 . ? Cl3 Hg2 Cl4 138.51(5) . . ? N5 Hg2 Cl4 99.99(9) . . ? C1 N1 C7 110.0(3) . . ? C1 N1 C13 113.4(3) . . ? C7 N1 C13 114.3(3) . . ? C4 N2 C3 118.8(4) . . ? C4 N2 Hg1 124.2(3) . . ? C3 N2 Hg1 116.3(3) . . ? C10 N3 C9 119.4(4) . . ? C10 N3 Hg1 121.2(3) . 4_646 ? C9 N3 Hg1 118.7(3) . 4_646 ? C21 N4 C27 109.1(3) . . ? C21 N4 C33 114.1(3) . . ? C27 N4 C33 108.9(3) . . ? C24 N5 C23 118.9(3) . . ? C24 N5 Hg2 121.6(3) . . ? C23 N5 Hg2 118.9(3) . . ? C30 N6 C29 118.6(4) . . ? C30 N6 Hg2 122.5(3) . 4_655 ? C29 N6 Hg2 118.9(3) . 4_655 ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 28.32 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.437 _refine_diff_density_min -0.935 _refine_diff_density_rms 0.094 data_2b_HgOTf2 _database_code_depnum_ccdc_archive 'CCDC 910370' #TrackingRef '15353_web_deposit_cif_file_0_YoichiHabata_1352699762.All_complexes_1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C46 H50 F12 Hg2 N6 O14 S4' _chemical_formula_weight 1668.38 _chemical_absolute_configuration syn 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' F F 0.0171 0.0103 '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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' _cell_length_a 10.983(2) _cell_length_b 11.610(2) _cell_length_c 12.528(3) _cell_angle_alpha 102.42(3) _cell_angle_beta 95.40(3) _cell_angle_gamma 109.96(3) _cell_volume 1441.8(5) _cell_formula_units_Z 1 _cell_measurement_temperature 100 _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.922 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 812 _exptl_absorpt_coefficient_mu 5.568 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.3366 _exptl_absorpt_correction_T_max 0.4192 _exptl_absorpt_process_details 'SADABS; Sheldrick, 1996' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100 _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 P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 8.366 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9104 _diffrn_reflns_av_R_equivalents 0.0143 _diffrn_reflns_av_sigmaI/netI 0.0504 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.69 _diffrn_reflns_theta_max 27.48 _reflns_number_total 7466 _reflns_number_gt 6971 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _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^)+(0.0178P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.005(6) _refine_ls_number_reflns 7466 _refine_ls_number_parameters 761 _refine_ls_number_restraints 39 _refine_ls_R_factor_all 0.0269 _refine_ls_R_factor_gt 0.0247 _refine_ls_wR_factor_ref 0.0571 _refine_ls_wR_factor_gt 0.0565 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.027 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.6995(7) 0.5596(6) 0.3487(6) 0.0182(14) Uani 1 1 d . . . H1A H 0.6612 0.6208 0.3838 0.022 Uiso 1 1 calc R . . H1B H 0.6390 0.5049 0.2785 0.022 Uiso 1 1 calc R . . C2 C 0.8319(8) 0.6316(7) 0.3230(7) 0.0175(16) Uani 1 1 d . . . C3 C 0.9168(8) 0.5714(7) 0.2941(6) 0.0156(17) Uani 1 1 d . . . H3A H 0.8940 0.4853 0.2958 0.019 Uiso 1 1 calc R . . C4 C 1.0661(11) 0.7524(8) 0.2583(9) 0.022(2) Uani 1 1 d . . . H4 H 1.1466 0.7927 0.2357 0.026 Uiso 1 1 calc R . . C5 C 0.9840(12) 0.8174(10) 0.2862(10) 0.025(3) Uani 1 1 d . . . H5A H 1.0087 0.9037 0.2845 0.030 Uiso 1 1 calc R . . C6 C 0.8672(13) 0.7567(10) 0.3161(10) 0.025(3) Uani 1 1 d . . . H6A H 0.8094 0.8004 0.3325 0.029 Uiso 1 1 calc R . . C7 C 0.5803(7) 0.3969(6) 0.4320(6) 0.0214(15) Uani 1 1 d . . . H7A H 0.5254 0.4484 0.4484 0.026 Uiso 1 1 calc R . . H7B H 0.5890 0.3601 0.4953 0.026 Uiso 1 1 calc R . . C8 C 0.5094(9) 0.2887(7) 0.3274(7) 0.0199(18) Uani 1 1 d . . . C9 C 0.5773(10) 0.2289(8) 0.2629(7) 0.0144(18) Uani 1 1 d . . . H9 H 0.6709 0.2617 0.2788 0.017 Uiso 1 1 calc R . . C10 C 0.3819(12) 0.0760(10) 0.1576(9) 0.019(2) Uani 1 1 d . . . H10 H 0.3375 0.0005 0.0995 0.023 Uiso 1 1 calc R . . C11 C 0.3093(12) 0.1310(11) 0.2179(10) 0.023(3) Uani 1 1 d . . . H11 H 0.2158 0.0950 0.2006 0.027 Uiso 1 1 calc R . . C12 C 0.3722(10) 0.2380(9) 0.3031(8) 0.022(2) Uani 1 1 d . . . H12 H 0.3229 0.2775 0.3453 0.026 Uiso 1 1 calc R . . C13 C 0.7930(7) 0.5570(6) 0.5364(6) 0.0215(15) Uani 1 1 d . . . H13 H 0.8652 0.6305 0.5238 0.026 Uiso 1 1 calc R . . C14 C 0.8596(12) 0.4783(9) 0.5835(9) 0.042(3) Uani 1 1 d . . . H14A H 0.7931 0.3957 0.5815 0.062 Uiso 1 1 calc R . . H14B H 0.9037 0.5232 0.6605 0.062 Uiso 1 1 calc R . . H14C H 0.9247 0.4653 0.5388 0.062 Uiso 1 1 calc R . . C15 C 0.7170(7) 0.6138(6) 0.6150(6) 0.0203(14) Uani 1 1 d . . . C16 C 0.7071(7) 0.7290(6) 0.6118(6) 0.0213(15) Uani 1 1 d . . . H16 H 0.7495 0.7732 0.5618 0.026 Uiso 1 1 calc R . . C17 C 0.6368(7) 0.7808(6) 0.6799(6) 0.0240(15) Uani 1 1 d . . . H17 H 0.6312 0.8599 0.6766 0.029 Uiso 1 1 calc R . . C18 C 0.5736(7) 0.7166(7) 0.7540(6) 0.0257(16) Uani 1 1 d . . . H18 H 0.5251 0.7515 0.8012 0.031 Uiso 1 1 calc R . . C19 C 0.5830(13) 0.6027(9) 0.7571(10) 0.028(3) Uani 1 1 d . . . H19 H 0.5400 0.5578 0.8064 0.034 Uiso 1 1 calc R . . C20 C 0.6550(14) 0.5525(10) 0.6887(9) 0.025(2) Uani 1 1 d . . . H20 H 0.6616 0.4740 0.6929 0.030 Uiso 1 1 calc R . . C21 C 1.1795(7) 0.1000(6) -0.0667(6) 0.0179(14) Uani 1 1 d . . . H21A H 1.2357 0.0731 -0.1159 0.021 Uiso 1 1 calc R . . H21B H 1.1639 0.0467 -0.0136 0.021 Uiso 1 1 calc R . . C22 C 1.2539(8) 0.2385(8) -0.0016(7) 0.0173(17) Uani 1 1 d . . . C23 C 1.1872(10) 0.3068(8) 0.0552(7) 0.0133(18) Uani 1 1 d . . . H23 H 1.0948 0.2672 0.0500 0.016 Uiso 1 1 calc R . . C24 C 1.3813(11) 0.4857(9) 0.1237(10) 0.021(3) Uani 1 1 d . . . H24 H 1.4246 0.5715 0.1661 0.025 Uiso 1 1 calc R . . C25 C 1.4538(13) 0.4212(10) 0.0689(10) 0.022(3) Uani 1 1 d U . . H25 H 1.5463 0.4614 0.0754 0.026 Uiso 1 1 calc R . . C26 C 1.3873(11) 0.2968(9) 0.0046(8) 0.017(2) Uani 1 1 d U . . H26 H 1.4343 0.2521 -0.0352 0.021 Uiso 1 1 calc R . . C27 C 0.9750(7) -0.0588(6) -0.1689(6) 0.0198(14) Uani 1 1 d . . . H27A H 1.0334 -0.1072 -0.1815 0.024 Uiso 1 1 calc R . . H27B H 0.9154 -0.0780 -0.2402 0.024 Uiso 1 1 calc R . . C28 C 0.8939(8) -0.1008(6) -0.0831(7) 0.0172(16) Uani 1 1 d . . . C29 C 0.8152(8) -0.0366(7) -0.0456(7) 0.0137(16) Uani 1 1 d . . . H29 H 0.8205 0.0375 -0.0686 0.016 Uiso 1 1 calc R . . C30 C 0.7254(11) -0.1798(8) 0.0571(9) 0.022(2) Uani 1 1 d . . . H30 H 0.6665 -0.2081 0.1051 0.026 Uiso 1 1 calc R . . C31 C 0.8029(13) -0.2459(9) 0.0244(9) 0.025(3) Uani 1 1 d . . . H31 H 0.7988 -0.3178 0.0506 0.030 Uiso 1 1 calc R . . C32 C 0.8884(12) -0.2068(9) -0.0478(10) 0.021(2) Uani 1 1 d . . . H32 H 0.9420 -0.2527 -0.0724 0.026 Uiso 1 1 calc R . . C33 C 1.0695(7) 0.1471(6) -0.2214(6) 0.0198(14) Uani 1 1 d . . . H33 H 1.1110 0.2395 -0.1814 0.024 Uiso 1 1 calc R . . C34 C 0.9332(9) 0.1270(8) -0.2819(8) 0.028(2) Uani 1 1 d . . . H34A H 0.8934 0.0408 -0.3314 0.042 Uiso 1 1 calc R . . H34B H 0.9418 0.1889 -0.3257 0.042 Uiso 1 1 calc R . . H34C H 0.8770 0.1383 -0.2274 0.042 Uiso 1 1 calc R . . C35 C 1.1578(7) 0.1220(7) -0.3024(6) 0.0216(15) Uani 1 1 d . . . C36 C 1.2702(8) 0.2217(8) -0.3072(7) 0.0343(19) Uani 1 1 d . . . H36 H 1.2936 0.3027 -0.2562 0.041 Uiso 1 1 calc R . . C37 C 1.3490(10) 0.2049(9) -0.3854(8) 0.044(2) Uani 1 1 d . . . H37 H 1.4239 0.2747 -0.3890 0.053 Uiso 1 1 calc R . . C38 C 1.3188(10) 0.0884(10) -0.4568(8) 0.046(3) Uani 1 1 d . . . H38 H 1.3736 0.0764 -0.5091 0.055 Uiso 1 1 calc R . . C39 C 1.2091(14) -0.0117(11) -0.4531(10) 0.042(4) Uani 1 1 d . . . H39 H 1.1874 -0.0926 -0.5036 0.051 Uiso 1 1 calc R . . C40 C 1.1289(15) 0.0047(12) -0.3754(10) 0.035(3) Uani 1 1 d . . . H40 H 1.0539 -0.0655 -0.3727 0.042 Uiso 1 1 calc R . . C1A C 0.9878(15) 0.1765(12) 0.3986(12) 0.032(3) Uani 1 1 d . . . C2A C 0.7625(12) 0.3818(10) -0.1091(10) 0.023(2) Uani 1 1 d . . . C3A C 1.2152(12) 0.5852(9) -0.1400(9) 0.033(3) Uani 1 1 d . . . C4A C 0.5930(12) -0.0242(10) 0.4627(9) 0.034(3) Uani 1 1 d . . . C1S C 0.4655(10) 0.0066(8) -0.2031(8) 0.030(2) Uani 1 1 d . . . H1S1 H 0.5588 0.0517 -0.2038 0.046 Uiso 1 1 calc R . . H1S2 H 0.4139 0.0541 -0.2261 0.046 Uiso 1 1 calc R . . H1S3 H 0.4346 -0.0783 -0.2546 0.046 Uiso 1 1 calc R . . C2S C 1.2743(13) 0.5841(11) 0.4900(9) 0.061(4) Uani 1 1 d . . . H2S1 H 1.2673 0.6673 0.5143 0.092 Uiso 1 1 calc R . . H2S2 H 1.3433 0.5787 0.5420 0.092 Uiso 1 1 calc R . . H2S3 H 1.1899 0.5171 0.4881 0.092 Uiso 1 1 calc R . . F1 F 0.9192(9) 0.0568(6) 0.3916(7) 0.056(2) Uani 1 1 d . . . F2 F 1.1109(10) 0.2032(10) 0.4363(8) 0.079(3) Uani 1 1 d . . . F3 F 0.9444(8) 0.2470(6) 0.4729(6) 0.047(2) Uani 1 1 d . . . F4 F 0.8270(8) 0.5052(6) -0.0948(6) 0.0415(18) Uani 1 1 d . . . F5 F 0.6343(7) 0.3597(6) -0.1375(6) 0.0363(15) Uani 1 1 d . . . F6 F 0.7970(7) 0.3195(6) -0.1964(5) 0.0362(17) Uani 1 1 d . . . F7 F 1.2567(7) 0.4954(4) -0.1200(4) 0.0519(15) Uani 1 1 d . . . F8 F 1.2601(8) 0.6151(6) -0.2286(6) 0.0416(18) Uani 1 1 d . . . F9 F 1.0846(6) 0.5321(5) -0.1696(5) 0.0516(15) Uani 1 1 d . . . F10 F 0.6157(6) 0.0961(4) 0.4644(5) 0.0520(15) Uani 1 1 d . . . F11 F 0.5192(9) -0.0543(8) 0.5386(6) 0.052(2) Uani 1 1 d . . . F12 F 0.7097(5) -0.0318(6) 0.4959(5) 0.0510(15) Uani 1 1 d . . . Hg1 Hg 0.619994(18) 0.029163(16) 0.088941(16) 0.01453(9) Uani 1 1 d U . . Hg2 Hg 1.142466(18) 0.523835(16) 0.200003(16) 0.01547(9) Uani 1 1 d U . . N1 N 0.7109(11) 0.4803(9) 0.4236(9) 0.022(2) Uani 1 1 d . . . N2 N 1.0295(10) 0.6293(9) 0.2639(8) 0.017(2) Uani 1 1 d . . . N3 N 0.5126(10) 0.1250(8) 0.1778(8) 0.016(2) Uani 1 1 d . . . N4 N 1.0547(9) 0.0768(8) -0.1334(8) 0.015(2) Uani 1 1 d . . . N5 N 1.2487(11) 0.4265(8) 0.1168(8) 0.014(2) Uani 1 1 d U . . N6 N 0.7291(10) -0.0759(8) 0.0240(8) 0.014(2) Uani 1 1 d U . . O1 O 1.0515(10) 0.3423(8) 0.2889(8) 0.049(3) Uani 1 1 d . . . O2 O 0.8302(10) 0.1860(8) 0.2379(8) 0.036(2) Uani 1 1 d . . . O3 O 1.0100(9) 0.1227(8) 0.1932(7) 0.037(2) Uani 1 1 d . . . O4 O 0.7258(8) 0.1970(7) -0.0191(7) 0.0275(17) Uani 1 1 d . . . O5 O 0.9363(9) 0.3742(8) 0.0402(8) 0.0259(18) Uani 1 1 d . . . O6 O 0.7367(9) 0.3990(8) 0.0941(7) 0.0313(18) Uani 1 1 d . . . O7 O 1.2236(8) 0.8105(7) -0.0612(8) 0.0284(18) Uani 1 1 d . . . O8 O 1.1967(9) 0.6726(6) 0.0598(6) 0.039(2) Uani 1 1 d . . . O9 O 1.4073(5) 0.7579(5) 0.0045(5) 0.0330(13) Uani 1 1 d . . . O11 O 0.5143(9) -0.2506(7) 0.3422(8) 0.036(2) Uani 1 1 d . . . O12 O 0.6058(8) -0.0817(6) 0.2559(6) 0.0322(17) Uani 1 1 d . . . O10 O 0.3900(6) -0.1176(6) 0.3083(5) 0.0421(15) Uani 1 1 d . . . O1S O 0.4500(8) -0.0045(7) -0.0931(7) 0.0255(17) Uani 1 1 d . . . O2S O 1.3070(10) 0.5683(8) 0.3810(7) 0.043(2) Uani 1 1 d . . . S1 S 0.9670(3) 0.2094(3) 0.2640(3) 0.0193(7) Uani 1 1 d . . . S2 S 0.7942(3) 0.3330(3) 0.0159(3) 0.0168(6) Uani 1 1 d . . . S3 S 1.2668(3) 0.7214(2) -0.0206(2) 0.0207(5) Uani 1 1 d . . . S4 S 0.5156(3) -0.1298(2) 0.3268(2) 0.0196(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.016(4) 0.029(3) 0.014(3) 0.007(3) 0.002(3) 0.013(3) C2 0.017(4) 0.028(4) 0.006(4) 0.002(3) 0.000(3) 0.009(3) C3 0.023(5) 0.020(3) 0.004(4) 0.006(3) 0.000(3) 0.008(3) C4 0.017(5) 0.016(4) 0.027(5) 0.001(3) 0.005(4) 0.003(3) C5 0.025(6) 0.019(4) 0.036(6) 0.005(4) 0.011(5) 0.012(4) C6 0.024(6) 0.028(5) 0.024(6) 0.003(4) 0.006(4) 0.014(4) C7 0.021(4) 0.028(4) 0.013(4) 0.002(3) 0.008(3) 0.009(3) C8 0.026(4) 0.020(4) 0.017(5) 0.006(3) 0.009(4) 0.011(3) C9 0.016(4) 0.021(4) 0.009(4) 0.005(3) 0.004(3) 0.009(3) C10 0.024(6) 0.025(5) 0.007(5) 0.002(3) 0.000(4) 0.011(4) C11 0.009(4) 0.034(5) 0.026(5) 0.011(3) 0.004(3) 0.007(3) C12 0.015(4) 0.028(4) 0.026(5) 0.011(4) 0.012(4) 0.009(3) C13 0.017(4) 0.026(3) 0.021(4) 0.005(3) 0.004(3) 0.009(3) C14 0.049(7) 0.052(6) 0.036(6) 0.010(5) 0.006(5) 0.035(6) C15 0.015(4) 0.026(3) 0.018(4) 0.004(3) 0.000(3) 0.009(3) C16 0.016(4) 0.030(4) 0.017(4) 0.007(3) 0.004(3) 0.008(3) C17 0.021(4) 0.027(4) 0.022(4) 0.000(3) 0.003(3) 0.011(3) C18 0.018(4) 0.037(4) 0.015(4) -0.003(3) 0.000(3) 0.008(3) C19 0.031(6) 0.033(5) 0.020(5) 0.009(4) 0.010(4) 0.009(4) C20 0.036(6) 0.025(5) 0.017(5) 0.006(3) 0.002(4) 0.014(4) C21 0.016(4) 0.021(3) 0.020(4) 0.007(3) 0.005(3) 0.010(3) C22 0.012(4) 0.025(4) 0.020(5) 0.012(3) 0.004(3) 0.010(3) C23 0.012(4) 0.023(4) 0.009(4) 0.009(3) 0.003(3) 0.008(3) C24 0.006(5) 0.017(4) 0.037(6) 0.005(4) 0.009(4) 0.000(3) C25 0.021(3) 0.022(3) 0.022(3) 0.0054(12) 0.0041(11) 0.0078(14) C26 0.017(2) 0.017(2) 0.017(2) 0.0041(11) 0.0033(11) 0.0072(12) C27 0.019(4) 0.022(3) 0.019(4) 0.003(3) 0.008(3) 0.008(3) C28 0.017(4) 0.019(3) 0.010(4) -0.003(3) 0.001(3) 0.004(3) C29 0.017(4) 0.019(3) 0.008(4) 0.007(3) 0.001(3) 0.009(3) C30 0.024(6) 0.023(4) 0.022(5) 0.007(4) 0.009(4) 0.010(4) C31 0.034(6) 0.023(4) 0.025(5) 0.010(4) 0.009(4) 0.015(4) C32 0.023(5) 0.021(4) 0.020(5) 0.002(3) 0.003(4) 0.010(4) C33 0.022(4) 0.024(3) 0.016(4) 0.006(3) 0.006(3) 0.010(3) C34 0.021(5) 0.048(5) 0.020(5) 0.009(4) 0.001(4) 0.021(4) C35 0.021(4) 0.037(4) 0.014(4) 0.010(3) 0.005(3) 0.017(3) C36 0.032(5) 0.047(5) 0.032(5) 0.023(4) 0.010(4) 0.016(4) C37 0.033(5) 0.071(6) 0.045(6) 0.035(5) 0.021(5) 0.024(5) C38 0.054(6) 0.087(7) 0.039(6) 0.042(5) 0.033(5) 0.057(6) C39 0.067(10) 0.058(8) 0.027(6) 0.017(6) 0.016(6) 0.047(7) C40 0.042(7) 0.041(6) 0.028(6) 0.008(4) 0.014(5) 0.022(5) C1A 0.041(7) 0.037(6) 0.043(7) 0.027(5) 0.024(5) 0.030(5) C2A 0.021(5) 0.025(5) 0.024(5) 0.011(4) 0.004(4) 0.007(4) C3A 0.042(7) 0.023(4) 0.037(7) 0.015(4) 0.018(5) 0.008(4) C4A 0.038(7) 0.036(5) 0.028(6) 0.003(4) 0.001(5) 0.020(5) C1S 0.034(5) 0.034(5) 0.022(5) 0.004(3) 0.009(4) 0.012(4) C2S 0.051(9) 0.075(9) 0.029(6) 0.007(6) 0.004(6) -0.009(6) F1 0.096(6) 0.032(3) 0.063(5) 0.031(3) 0.050(4) 0.033(3) F2 0.056(6) 0.161(8) 0.052(5) 0.054(5) 0.005(4) 0.065(5) F3 0.083(5) 0.047(3) 0.026(3) 0.016(3) 0.019(3) 0.038(3) F4 0.057(4) 0.021(3) 0.055(4) 0.019(3) 0.015(3) 0.018(3) F5 0.024(3) 0.058(3) 0.039(4) 0.035(3) 0.003(3) 0.016(3) F6 0.064(4) 0.040(3) 0.023(3) 0.018(2) 0.020(3) 0.034(3) F7 0.087(5) 0.033(3) 0.040(3) 0.003(2) 0.008(3) 0.033(3) F8 0.042(4) 0.055(4) 0.023(3) 0.011(3) 0.016(3) 0.009(3) F9 0.029(3) 0.054(3) 0.045(4) -0.004(3) -0.005(3) -0.005(3) F10 0.061(4) 0.026(2) 0.060(4) -0.003(2) 0.011(3) 0.013(2) F11 0.079(6) 0.083(5) 0.020(3) 0.019(3) 0.023(4) 0.056(4) F12 0.030(3) 0.079(4) 0.038(4) 0.008(3) -0.011(3) 0.023(3) Hg1 0.0133(2) 0.01794(17) 0.0154(2) 0.00519(14) 0.00531(17) 0.00835(15) Hg2 0.0139(2) 0.01768(17) 0.0169(2) 0.00466(14) 0.00610(18) 0.00746(15) N1 0.025(6) 0.024(4) 0.018(5) 0.002(4) 0.010(5) 0.013(4) N2 0.011(4) 0.029(4) 0.010(3) -0.001(2) 0.001(3) 0.009(3) N3 0.012(4) 0.020(3) 0.020(4) 0.008(2) 0.008(3) 0.008(2) N4 0.007(5) 0.020(4) 0.014(5) 0.005(3) -0.002(4) 0.002(3) N5 0.014(2) 0.014(2) 0.014(2) 0.0038(11) 0.0020(11) 0.0053(12) N6 0.014(2) 0.013(2) 0.014(2) 0.0032(11) 0.0025(11) 0.0053(12) O1 0.056(6) 0.037(4) 0.033(5) 0.021(3) -0.005(4) -0.012(4) O2 0.023(5) 0.043(4) 0.039(5) -0.003(4) 0.000(4) 0.016(4) O3 0.038(5) 0.063(5) 0.024(4) 0.011(3) 0.014(4) 0.034(4) O4 0.027(4) 0.022(3) 0.033(4) 0.017(3) 0.007(3) 0.004(3) O5 0.013(4) 0.034(3) 0.028(4) 0.004(3) 0.002(3) 0.010(3) O6 0.028(4) 0.049(4) 0.028(4) 0.010(3) 0.011(3) 0.027(3) O7 0.023(4) 0.024(3) 0.041(4) 0.012(3) 0.007(3) 0.010(3) O8 0.062(6) 0.027(3) 0.031(4) 0.015(3) 0.028(4) 0.012(3) O9 0.024(3) 0.032(3) 0.041(4) 0.007(3) -0.004(3) 0.012(3) O11 0.040(5) 0.023(3) 0.047(5) 0.012(3) 0.016(4) 0.010(3) O12 0.044(5) 0.039(4) 0.028(4) 0.021(3) 0.016(3) 0.023(3) O10 0.028(4) 0.063(4) 0.039(4) 0.011(3) 0.003(3) 0.025(3) O1S 0.020(4) 0.033(3) 0.021(4) 0.015(3) 0.002(3) 0.003(3) O2S 0.042(6) 0.048(5) 0.019(4) 0.009(3) -0.009(4) -0.003(4) S1 0.0122(15) 0.0249(14) 0.0214(16) 0.0110(11) 0.0017(12) 0.0050(11) S2 0.0147(15) 0.0205(13) 0.0178(15) 0.0055(10) 0.0034(11) 0.0093(11) S3 0.0222(12) 0.0194(11) 0.0204(12) 0.0060(9) 0.0060(9) 0.0066(9) S4 0.0184(11) 0.0232(11) 0.0196(11) 0.0072(9) 0.0044(9) 0.0094(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.474(12) . ? C1 C2 1.513(10) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C3 1.375(11) . ? C2 C6 1.394(13) . ? C3 N2 1.325(13) . ? C3 H3A 0.9500 . ? C4 N2 1.365(13) . ? C4 C5 1.384(15) . ? C4 H4 0.9500 . ? C5 C6 1.368(16) . ? C5 H5A 0.9500 . ? C6 H6A 0.9500 . ? C7 N1 1.459(12) . ? C7 C8 1.527(11) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.385(12) . ? C8 C12 1.393(14) . ? C9 N3 1.347(13) . ? C9 H9 0.9500 . ? C10 N3 1.326(16) . ? C10 C11 1.367(16) . ? C10 H10 0.9500 . ? C11 C12 1.366(15) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 N1 1.508(13) . ? C13 C14 1.525(12) . ? C13 C15 1.534(9) . ? C13 H13 1.0000 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C20 1.376(13) . ? C15 C16 1.388(9) . ? C16 C17 1.381(9) . ? C16 H16 0.9500 . ? C17 C18 1.401(10) . ? C17 H17 0.9500 . ? C18 C19 1.369(13) . ? C18 H18 0.9500 . ? C19 C20 1.388(16) . ? C19 H19 0.9500 . ? C20 H20 0.9500 . ? C21 N4 1.445(11) . ? C21 C22 1.527(10) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C26 1.375(13) . ? C22 C23 1.387(12) . ? C23 N5 1.336(12) . ? C23 H23 0.9500 . ? C24 N5 1.367(15) . ? C24 C25 1.398(16) . ? C24 H24 0.9500 . ? C25 C26 1.392(14) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C27 N4 1.459(10) . ? C27 C28 1.515(10) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 C29 1.374(11) . ? C28 C32 1.379(13) . ? C29 N6 1.377(12) . ? C29 H29 0.9500 . ? C30 N6 1.346(13) . ? C30 C31 1.362(16) . ? C30 H30 0.9500 . ? C31 C32 1.397(16) . ? C31 H31 0.9500 . ? C32 H32 0.9500 . ? C33 N4 1.496(11) . ? C33 C35 1.520(9) . ? C33 C34 1.530(11) . ? C33 H33 1.0000 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 C40 1.381(14) . ? C35 C36 1.391(11) . ? C36 C37 1.393(11) . ? C36 H36 0.9500 . ? C37 C38 1.363(13) . ? C37 H37 0.9500 . ? C38 C39 1.372(16) . ? C38 H38 0.9500 . ? C39 C40 1.398(17) . ? C39 H39 0.9500 . ? C40 H40 0.9500 . ? C1A F2 1.295(17) . ? C1A F1 1.314(14) . ? C1A F3 1.337(14) . ? C1A S1 1.819(14) . ? C2A F4 1.326(12) . ? C2A F6 1.337(13) . ? C2A F5 1.339(14) . ? C2A S2 1.819(12) . ? C3A F8 1.322(12) . ? C3A F7 1.331(11) . ? C3A F9 1.331(12) . ? C3A S3 1.808(11) . ? C4A F10 1.328(11) . ? C4A F11 1.333(14) . ? C4A F12 1.347(12) . ? C4A S4 1.801(11) . ? C1S O1S 1.432(12) . ? C1S H1S1 0.9800 . ? C1S H1S2 0.9800 . ? C1S H1S3 0.9800 . ? C2S O2S 1.434(14) . ? C2S H2S1 0.9800 . ? C2S H2S2 0.9800 . ? C2S H2S3 0.9800 . ? Hg1 N6 2.083(10) . ? Hg1 N3 2.117(10) . ? Hg1 O4 2.619(7) . ? Hg1 O2 2.643(9) . ? Hg1 O12 2.671(7) . ? Hg1 O1S 2.676(9) . ? Hg2 N5 2.085(10) . ? Hg2 N2 2.117(10) . ? Hg2 O1 2.542(8) . ? Hg2 O2S 2.601(9) . ? Hg2 O5 2.668(9) . ? Hg2 O8 2.688(7) . ? O1 S1 1.449(9) . ? O2 S1 1.425(10) . ? O3 S1 1.428(9) . ? O4 S2 1.442(8) . ? O5 S2 1.447(10) . ? O6 S2 1.439(9) . ? O7 S3 1.439(8) . ? O8 S3 1.422(7) . ? O9 S3 1.436(6) . ? O11 S4 1.451(8) . ? O12 S4 1.444(7) . ? O10 S4 1.437(6) . ? 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 N1 C1 C2 111.7(7) . . ? N1 C1 H1A 109.3 . . ? C2 C1 H1A 109.3 . . ? N1 C1 H1B 109.3 . . ? C2 C1 H1B 109.3 . . ? H1A C1 H1B 107.9 . . ? C3 C2 C6 117.0(8) . . ? C3 C2 C1 120.8(7) . . ? C6 C2 C1 121.9(8) . . ? N2 C3 C2 122.3(8) . . ? N2 C3 H3A 118.8 . . ? C2 C3 H3A 118.8 . . ? N2 C4 C5 118.9(10) . . ? N2 C4 H4 120.6 . . ? C5 C4 H4 120.6 . . ? C6 C5 C4 119.6(10) . . ? C6 C5 H5A 120.2 . . ? C4 C5 H5A 120.2 . . ? C5 C6 C2 120.9(11) . . ? C5 C6 H6A 119.5 . . ? C2 C6 H6A 119.5 . . ? N1 C7 C8 114.1(7) . . ? N1 C7 H7A 108.7 . . ? C8 C7 H7A 108.7 . . ? N1 C7 H7B 108.7 . . ? C8 C7 H7B 108.7 . . ? H7A C7 H7B 107.6 . . ? C9 C8 C12 118.4(8) . . ? C9 C8 C7 121.4(8) . . ? C12 C8 C7 119.7(7) . . ? N3 C9 C8 120.9(10) . . ? N3 C9 H9 119.5 . . ? C8 C9 H9 119.5 . . ? N3 C10 C11 121.9(10) . . ? N3 C10 H10 119.0 . . ? C11 C10 H10 119.0 . . ? C12 C11 C10 119.5(11) . . ? C12 C11 H11 120.3 . . ? C10 C11 H11 120.3 . . ? C11 C12 C8 119.3(9) . . ? C11 C12 H12 120.3 . . ? C8 C12 H12 120.3 . . ? N1 C13 C14 109.2(7) . . ? N1 C13 C15 113.3(7) . . ? C14 C13 C15 114.4(7) . . ? N1 C13 H13 106.5 . . ? C14 C13 H13 106.5 . . ? C15 C13 H13 106.5 . . ? 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 . . ? C20 C15 C16 117.9(7) . . ? C20 C15 C13 121.9(7) . . ? C16 C15 C13 120.1(6) . . ? C17 C16 C15 121.3(6) . . ? C17 C16 H16 119.3 . . ? C15 C16 H16 119.3 . . ? C16 C17 C18 119.9(7) . . ? C16 C17 H17 120.0 . . ? C18 C17 H17 120.0 . . ? C19 C18 C17 118.9(7) . . ? C19 C18 H18 120.6 . . ? C17 C18 H18 120.6 . . ? C18 C19 C20 120.5(10) . . ? C18 C19 H19 119.8 . . ? C20 C19 H19 119.8 . . ? C15 C20 C19 121.5(9) . . ? C15 C20 H20 119.3 . . ? C19 C20 H20 119.3 . . ? N4 C21 C22 114.1(6) . . ? N4 C21 H21A 108.7 . . ? C22 C21 H21A 108.7 . . ? N4 C21 H21B 108.7 . . ? C22 C21 H21B 108.7 . . ? H21A C21 H21B 107.6 . . ? C26 C22 C23 118.8(8) . . ? C26 C22 C21 121.3(7) . . ? C23 C22 C21 119.9(7) . . ? N5 C23 C22 122.1(10) . . ? N5 C23 H23 118.9 . . ? C22 C23 H23 118.9 . . ? N5 C24 C25 120.6(10) . . ? N5 C24 H24 119.7 . . ? C25 C24 H24 119.7 . . ? C26 C25 C24 118.6(12) . . ? C26 C25 H25 120.7 . . ? C24 C25 H25 120.7 . . ? C22 C26 C25 120.1(10) . . ? C22 C26 H26 119.9 . . ? C25 C26 H26 119.9 . . ? N4 C27 C28 111.6(6) . . ? N4 C27 H27A 109.3 . . ? C28 C27 H27A 109.3 . . ? N4 C27 H27B 109.3 . . ? C28 C27 H27B 109.3 . . ? H27A C27 H27B 108.0 . . ? C29 C28 C32 118.8(8) . . ? C29 C28 C27 118.6(6) . . ? C32 C28 C27 122.4(8) . . ? C28 C29 N6 122.3(7) . . ? C28 C29 H29 118.8 . . ? N6 C29 H29 118.8 . . ? N6 C30 C31 122.6(10) . . ? N6 C30 H30 118.7 . . ? C31 C30 H30 118.7 . . ? C30 C31 C32 119.4(10) . . ? C30 C31 H31 120.3 . . ? C32 C31 H31 120.3 . . ? C28 C32 C31 119.1(11) . . ? C28 C32 H32 120.4 . . ? C31 C32 H32 120.4 . . ? N4 C33 C35 116.4(6) . . ? N4 C33 C34 109.5(7) . . ? C35 C33 C34 111.7(6) . . ? N4 C33 H33 106.2 . . ? C35 C33 H33 106.2 . . ? C34 C33 H33 106.2 . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C40 C35 C36 118.0(8) . . ? C40 C35 C33 122.8(8) . . ? C36 C35 C33 119.2(7) . . ? C35 C36 C37 121.1(8) . . ? C35 C36 H36 119.5 . . ? C37 C36 H36 119.5 . . ? C38 C37 C36 120.0(9) . . ? C38 C37 H37 120.0 . . ? C36 C37 H37 120.0 . . ? C37 C38 C39 119.9(9) . . ? C37 C38 H38 120.1 . . ? C39 C38 H38 120.1 . . ? C38 C39 C40 120.4(11) . . ? C38 C39 H39 119.8 . . ? C40 C39 H39 119.8 . . ? C35 C40 C39 120.6(11) . . ? C35 C40 H40 119.7 . . ? C39 C40 H40 119.7 . . ? F2 C1A F1 109.9(11) . . ? F2 C1A F3 107.5(13) . . ? F1 C1A F3 107.2(10) . . ? F2 C1A S1 110.9(10) . . ? F1 C1A S1 110.5(10) . . ? F3 C1A S1 110.7(8) . . ? F4 C2A F6 107.9(9) . . ? F4 C2A F5 106.7(9) . . ? F6 C2A F5 106.9(9) . . ? F4 C2A S2 111.6(8) . . ? F6 C2A S2 112.3(8) . . ? F5 C2A S2 111.2(8) . . ? F8 C3A F7 107.4(9) . . ? F8 C3A F9 106.1(9) . . ? F7 C3A F9 107.0(7) . . ? F8 C3A S3 112.4(7) . . ? F7 C3A S3 111.6(8) . . ? F9 C3A S3 112.0(7) . . ? F10 C4A F11 108.4(9) . . ? F10 C4A F12 107.4(9) . . ? F11 C4A F12 106.7(9) . . ? F10 C4A S4 111.9(7) . . ? F11 C4A S4 111.3(9) . . ? F12 C4A S4 110.8(7) . . ? O1S C1S H1S1 109.5 . . ? O1S C1S H1S2 109.5 . . ? H1S1 C1S H1S2 109.5 . . ? O1S C1S H1S3 109.5 . . ? H1S1 C1S H1S3 109.5 . . ? H1S2 C1S H1S3 109.5 . . ? O2S C2S H2S1 109.5 . . ? O2S C2S H2S2 109.5 . . ? H2S1 C2S H2S2 109.5 . . ? O2S C2S H2S3 109.5 . . ? H2S1 C2S H2S3 109.5 . . ? H2S2 C2S H2S3 109.5 . . ? N6 Hg1 N3 170.7(4) . . ? N6 Hg1 O4 89.7(3) . . ? N3 Hg1 O4 98.1(3) . . ? N6 Hg1 O2 89.8(3) . . ? N3 Hg1 O2 86.7(3) . . ? O4 Hg1 O2 79.3(3) . . ? N6 Hg1 O12 87.7(3) . . ? N3 Hg1 O12 83.1(3) . . ? O4 Hg1 O12 156.2(2) . . ? O2 Hg1 O12 77.0(3) . . ? N6 Hg1 O1S 101.1(3) . . ? N3 Hg1 O1S 86.3(3) . . ? O4 Hg1 O1S 69.9(2) . . ? O2 Hg1 O1S 147.1(3) . . ? O12 Hg1 O1S 133.7(2) . . ? N5 Hg2 N2 172.1(4) . . ? N5 Hg2 O1 89.1(3) . . ? N2 Hg2 O1 96.9(4) . . ? N5 Hg2 O2S 87.4(4) . . ? N2 Hg2 O2S 99.3(3) . . ? O1 Hg2 O2S 72.1(3) . . ? N5 Hg2 O5 86.4(3) . . ? N2 Hg2 O5 89.4(3) . . ? O1 Hg2 O5 81.3(3) . . ? O2S Hg2 O5 152.7(3) . . ? N5 Hg2 O8 86.7(3) . . ? N2 Hg2 O8 86.3(3) . . ? O1 Hg2 O8 165.4(3) . . ? O2S Hg2 O8 121.6(3) . . ? O5 Hg2 O8 84.6(3) . . ? C7 N1 C1 110.2(8) . . ? C7 N1 C13 111.9(8) . . ? C1 N1 C13 113.0(7) . . ? C3 N2 C4 121.2(10) . . ? C3 N2 Hg2 120.0(7) . . ? C4 N2 Hg2 118.2(8) . . ? C10 N3 C9 119.9(10) . . ? C10 N3 Hg1 120.2(7) . . ? C9 N3 Hg1 119.5(8) . . ? C21 N4 C27 110.6(7) . . ? C21 N4 C33 112.6(7) . . ? C27 N4 C33 116.8(7) . . ? C23 N5 C24 119.7(10) . . ? C23 N5 Hg2 120.2(8) . . ? C24 N5 Hg2 120.1(7) . . ? C30 N6 C29 117.7(9) . . ? C30 N6 Hg1 120.2(8) . . ? C29 N6 Hg1 121.9(6) . . ? S1 O1 Hg2 142.7(6) . . ? S1 O2 Hg1 139.3(5) . . ? S2 O4 Hg1 132.6(5) . . ? S2 O5 Hg2 141.0(5) . . ? S3 O8 Hg2 153.1(6) . . ? S4 O12 Hg1 140.4(5) . . ? C1S O1S Hg1 133.2(6) . . ? C2S O2S Hg2 124.2(8) . . ? O2 S1 O3 114.8(6) . . ? O2 S1 O1 114.0(6) . . ? O3 S1 O1 115.7(6) . . ? O2 S1 C1A 104.4(7) . . ? O3 S1 C1A 103.9(6) . . ? O1 S1 C1A 101.8(6) . . ? O6 S2 O4 114.5(5) . . ? O6 S2 O5 115.7(5) . . ? O4 S2 O5 114.4(5) . . ? O6 S2 C2A 103.0(6) . . ? O4 S2 C2A 103.1(5) . . ? O5 S2 C2A 103.9(6) . . ? O8 S3 O9 115.5(5) . . ? O8 S3 O7 114.0(5) . . ? O9 S3 O7 114.7(4) . . ? O8 S3 C3A 103.4(4) . . ? O9 S3 C3A 103.9(5) . . ? O7 S3 C3A 103.3(5) . . ? O10 S4 O12 115.9(4) . . ? O10 S4 O11 116.6(5) . . ? O12 S4 O11 112.6(5) . . ? O10 S4 C4A 103.6(5) . . ? O12 S4 C4A 103.8(5) . . ? O11 S4 C4A 101.9(5) . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 2.182 _refine_diff_density_min -1.415 _refine_diff_density_rms 0.173 # END