data_global data_e2257a #TrackingRef 'web_deposit_cif_file_0_FERLAY_1361985472.2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C48 H36 N4 O4 S4, H2 O' _chemical_formula_sum 'C48 H38 N4 O5 S4' _chemical_formula_weight 879.06 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.7320(4) _cell_length_b 18.8313(7) _cell_length_c 22.5452(8) _cell_angle_alpha 70.428(2) _cell_angle_beta 83.211(2) _cell_angle_gamma 81.950(2) _cell_volume 4238.3(3) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 7882 _cell_measurement_theta_min 2.31 _cell_measurement_theta_max 23.43 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.378 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1832 _exptl_absorpt_coefficient_mu 0.278 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9621 _exptl_absorpt_correction_T_max 0.9727 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 83282 _diffrn_reflns_av_R_equivalents 0.0745 _diffrn_reflns_av_sigmaI/netI 0.1302 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.24 _diffrn_reflns_theta_max 29.07 _reflns_number_total 22584 _reflns_number_gt 10149 _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^)+(0.0576P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 22584 _refine_ls_number_parameters 1111 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.1725 _refine_ls_R_factor_gt 0.0597 _refine_ls_wR_factor_ref 0.1499 _refine_ls_wR_factor_gt 0.1157 _refine_ls_goodness_of_fit_ref 1.000 _refine_ls_restrained_S_all 1.001 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group S1 S 0.63902(7) 0.54469(4) 0.70486(4) 0.0371(2) Uani 1 1 d . . . C1 C 0.7073(3) 0.44956(16) 0.73529(13) 0.0280(7) Uani 1 1 d . . . C2 C 0.8206(3) 0.42321(15) 0.70921(13) 0.0258(7) Uani 1 1 d . . . C3 C 0.8682(3) 0.34701(15) 0.73264(13) 0.0277(7) Uani 1 1 d . . . C4 C 0.8021(3) 0.29779(17) 0.78325(14) 0.0339(7) Uani 1 1 d . . . H4 H 0.8350 0.2462 0.8002 0.041 Uiso 1 1 calc R . . C5 C 0.6898(3) 0.32394(17) 0.80851(14) 0.0365(8) Uani 1 1 d . . . H5 H 0.6446 0.2900 0.8426 0.044 Uiso 1 1 calc R . . C6 C 0.6418(3) 0.39879(17) 0.78502(14) 0.0328(7) Uani 1 1 d . . . H6 H 0.5635 0.4160 0.8028 0.039 Uiso 1 1 calc R . . O1 O 0.89002(17) 0.47302(10) 0.66227(8) 0.0295(5) Uani 1 1 d . . . C7 C 0.8577(3) 0.48605(17) 0.59898(13) 0.0406(8) Uani 1 1 d . . . H7A H 0.7649 0.4909 0.5977 0.049 Uiso 1 1 calc R . . H7B H 0.8953 0.4433 0.5842 0.049 Uiso 1 1 calc R . . C8 C 0.9092(3) 0.55826(16) 0.55781(14) 0.0339(7) Uani 1 1 d . . . C12 C 1.0188(3) 0.57929(19) 0.56786(18) 0.0563(10) Uani 1 1 d . . . H12 H 1.0667 0.5479 0.6017 0.068 Uiso 1 1 calc R . . C11 C 1.0598(4) 0.6468(2) 0.52831(19) 0.0683(12) Uani 1 1 d . . . H11 H 1.1361 0.6623 0.5349 0.082 Uiso 1 1 calc R . . C10 C 0.9908(4) 0.6902(2) 0.48036(17) 0.0583(11) Uani 1 1 d . . . H10 H 1.0166 0.7370 0.4526 0.070 Uiso 1 1 calc R . . C9 C 0.8833(4) 0.6649(2) 0.47320(16) 0.0635(12) Uani 1 1 d . . . H9 H 0.8348 0.6954 0.4392 0.076 Uiso 1 1 calc R . . N1 N 0.8400(3) 0.59954(15) 0.51073(12) 0.0514(8) Uani 1 1 d . . . S2 S 1.00493(7) 0.30950(4) 0.69648(4) 0.0371(2) Uani 1 1 d . . . C13 C 1.1267(3) 0.35821(15) 0.70674(14) 0.0293(7) Uani 1 1 d . . . C14 C 1.1558(3) 0.35210(15) 0.76757(13) 0.0272(7) Uani 1 1 d . . . C15 C 1.2541(3) 0.38899(15) 0.77446(13) 0.0293(7) Uani 1 1 d . . . C16 C 1.3266(3) 0.42820(17) 0.72154(14) 0.0374(8) Uani 1 1 d . . . H16 H 1.3939 0.4532 0.7262 0.045 Uiso 1 1 calc R . . C17 C 1.3016(3) 0.43101(17) 0.66226(14) 0.0391(8) Uani 1 1 d . . . H17 H 1.3542 0.4557 0.6264 0.047 Uiso 1 1 calc R . . C18 C 1.2001(3) 0.39793(16) 0.65486(14) 0.0361(8) Uani 1 1 d . . . H18 H 1.1806 0.4025 0.6136 0.043 Uiso 1 1 calc R . . O2 O 1.08585(17) 0.31104(10) 0.81998(9) 0.0303(5) Uani 1 1 d . . . C19 C 1.1372(3) 0.23245(16) 0.84327(14) 0.0382(8) Uani 1 1 d . . . H19A H 1.2275 0.2292 0.8503 0.046 Uiso 1 1 calc R . . H19B H 1.1309 0.2074 0.8117 0.046 Uiso 1 1 calc R . . C20 C 1.0658(3) 0.19309(17) 0.90390(14) 0.0336(7) Uani 1 1 d . . . N2 N 1.1204(3) 0.12380(14) 0.93365(12) 0.0464(7) Uani 1 1 d . . . C21 C 1.0627(4) 0.0844(2) 0.98794(17) 0.0593(11) Uani 1 1 d . . . H21 H 1.1006 0.0351 1.0095 0.071 Uiso 1 1 calc R . . C22 C 0.9530(4) 0.1103(2) 1.01450(18) 0.0622(11) Uani 1 1 d . . . H22 H 0.9160 0.0801 1.0536 0.075 Uiso 1 1 calc R . . C23 C 0.8973(3) 0.1812(2) 0.98307(17) 0.0555(10) Uani 1 1 d . . . H23 H 0.8200 0.2006 1.0000 0.067 Uiso 1 1 calc R . . C24 C 0.9544(3) 0.22404(18) 0.92674(14) 0.0394(8) Uani 1 1 d . . . H24 H 0.9179 0.2734 0.9044 0.047 Uiso 1 1 calc R . . S3 S 1.29671(7) 0.38179(5) 0.85035(4) 0.0358(2) Uani 1 1 d . . . C25 C 1.1538(3) 0.41156(16) 0.88808(13) 0.0303(7) Uani 1 1 d . . . C26 C 1.0929(3) 0.48456(16) 0.86428(13) 0.0281(7) Uani 1 1 d . . . C27 C 0.9852(3) 0.50751(16) 0.89774(14) 0.0316(7) Uani 1 1 d . . . C28 C 0.9417(3) 0.45720(18) 0.95455(15) 0.0386(8) Uani 1 1 d . . . H28 H 0.8681 0.4721 0.9772 0.046 Uiso 1 1 calc R . . C29 C 1.0045(3) 0.38566(19) 0.97841(15) 0.0413(8) Uani 1 1 d . . . H29 H 0.9749 0.3521 1.0178 0.050 Uiso 1 1 calc R . . C30 C 1.1091(3) 0.36269(18) 0.94570(14) 0.0366(8) Uani 1 1 d . . . H30 H 1.1514 0.3132 0.9624 0.044 Uiso 1 1 calc R . . O3 O 1.13773(17) 0.53330(10) 0.80770(9) 0.0315(5) Uani 1 1 d . . . C31 C 1.2254(3) 0.57901(17) 0.81607(14) 0.0376(8) Uani 1 1 d . . . H31A H 1.2923 0.5462 0.8424 0.045 Uiso 1 1 calc R . . H31B H 1.1814 0.6139 0.8382 0.045 Uiso 1 1 calc R . . C32 C 1.2838(3) 0.62394(16) 0.75324(14) 0.0321(7) Uani 1 1 d . . . N3 N 1.3723(2) 0.66512(14) 0.75777(12) 0.0383(6) Uani 1 1 d . . . C33 C 1.4298(3) 0.70653(17) 0.70331(18) 0.0467(9) Uani 1 1 d . . . H33 H 1.4931 0.7358 0.7057 0.056 Uiso 1 1 calc R . . C34 C 1.4033(3) 0.70918(19) 0.64545(18) 0.0517(10) Uani 1 1 d . . . H34 H 1.4469 0.7393 0.6084 0.062 Uiso 1 1 calc R . . C35 C 1.3119(3) 0.6672(2) 0.64174(16) 0.0555(10) Uani 1 1 d . . . H35 H 1.2910 0.6681 0.6017 0.067 Uiso 1 1 calc R . . C36 C 1.2500(3) 0.62350(18) 0.69639(15) 0.0414(8) Uani 1 1 d . . . H36 H 1.1862 0.5942 0.6947 0.050 Uiso 1 1 calc R . . S4 S 0.91151(8) 0.60248(5) 0.87412(4) 0.0401(2) Uani 1 1 d . . . C37 C 0.8723(3) 0.61945(16) 0.79598(14) 0.0319(7) Uani 1 1 d . . . C38 C 0.7830(3) 0.57917(15) 0.78415(14) 0.0288(7) Uani 1 1 d . . . C39 C 0.7507(3) 0.59494(15) 0.72199(14) 0.0305(7) Uani 1 1 d . . . C40 C 0.8036(3) 0.65239(16) 0.67344(15) 0.0390(8) Uani 1 1 d . . . H40 H 0.7817 0.6635 0.6314 0.047 Uiso 1 1 calc R . . C41 C 0.8887(3) 0.69387(17) 0.68609(17) 0.0439(9) Uani 1 1 d . . . H41 H 0.9225 0.7343 0.6529 0.053 Uiso 1 1 calc R . . C42 C 0.9240(3) 0.67652(17) 0.74654(17) 0.0417(8) Uani 1 1 d . . . H42 H 0.9844 0.7040 0.7545 0.050 Uiso 1 1 calc R . . O4 O 0.73107(17) 0.52287(10) 0.83297(9) 0.0310(5) Uani 1 1 d . . . C43 C 0.6133(3) 0.54900(16) 0.86034(14) 0.0350(8) Uani 1 1 d . . . H43A H 0.5532 0.5725 0.8273 0.042 Uiso 1 1 calc R . . H43B H 0.6269 0.5876 0.8791 0.042 Uiso 1 1 calc R . . C44 C 0.5607(3) 0.48338(17) 0.91003(13) 0.0322(7) Uani 1 1 d . . . N4 N 0.4410(2) 0.49889(14) 0.93158(11) 0.0360(6) Uani 1 1 d . . . C45 C 0.3873(3) 0.4421(2) 0.97482(15) 0.0424(8) Uani 1 1 d . . . H45 H 0.3028 0.4521 0.9904 0.051 Uiso 1 1 calc R . . C46 C 0.4455(3) 0.3704(2) 0.99829(15) 0.0479(9) Uani 1 1 d . . . H46 H 0.4021 0.3316 1.0286 0.058 Uiso 1 1 calc R . . C47 C 0.5688(3) 0.35544(19) 0.97709(15) 0.0479(9) Uani 1 1 d . . . H47 H 0.6126 0.3063 0.9933 0.058 Uiso 1 1 calc R . . C48 C 0.6281(3) 0.41272(17) 0.93192(14) 0.0372(8) Uani 1 1 d . . . H48 H 0.7130 0.4038 0.9163 0.045 Uiso 1 1 calc R . . S5 S 0.48723(7) 0.81066(4) 0.19872(4) 0.0360(2) Uani 1 1 d . . . C49 C 0.5900(2) 0.84655(15) 0.23486(13) 0.0260(7) Uani 1 1 d . . . C50 C 0.6168(2) 0.92200(15) 0.21063(13) 0.0255(7) Uani 1 1 d . . . C51 C 0.7070(3) 0.94641(15) 0.23707(13) 0.0273(7) Uani 1 1 d . . . C52 C 0.7703(3) 0.89517(17) 0.28745(13) 0.0313(7) Uani 1 1 d . . . H52 H 0.8319 0.9114 0.3056 0.038 Uiso 1 1 calc R . . C53 C 0.7432(3) 0.82053(17) 0.31102(14) 0.0343(8) Uani 1 1 d . . . H53 H 0.7869 0.7857 0.3451 0.041 Uiso 1 1 calc R . . C54 C 0.6540(3) 0.79663(16) 0.28552(14) 0.0327(7) Uani 1 1 d . . . H54 H 0.6354 0.7455 0.3025 0.039 Uiso 1 1 calc R . . O5 O 0.54849(17) 0.97248(10) 0.16345(9) 0.0298(5) Uani 1 1 d . . . C55 C 0.6073(3) 0.98525(17) 0.10074(13) 0.0388(8) Uani 1 1 d . . . H55A H 0.6020 0.9413 0.0867 0.047 Uiso 1 1 calc R . . H55B H 0.6974 0.9920 0.0998 0.047 Uiso 1 1 calc R . . C56 C 0.5389(3) 1.05557(16) 0.05804(13) 0.0317(7) Uani 1 1 d . . . N5 N 0.6100(3) 1.09666(15) 0.01021(12) 0.0453(7) Uani 1 1 d . . . C57 C 0.5517(4) 1.1601(2) -0.02818(16) 0.0571(11) Uani 1 1 d . . . H57 H 0.6016 1.1905 -0.0624 0.069 Uiso 1 1 calc R . . C58 C 0.4275(4) 1.1843(2) -0.02228(16) 0.0561(10) Uani 1 1 d . . . H58 H 0.3913 1.2294 -0.0517 0.067 Uiso 1 1 calc R . . C59 C 0.3564(4) 1.1414(2) 0.02749(18) 0.0597(11) Uani 1 1 d . . . H59 H 0.2688 1.1563 0.0336 0.072 Uiso 1 1 calc R . . C60 C 0.4125(3) 1.07649(18) 0.06864(16) 0.0484(9) Uani 1 1 d . . . H60 H 0.3646 1.0464 0.1040 0.058 Uiso 1 1 calc R . . S6 S 0.74896(7) 1.04045(4) 0.20595(4) 0.0369(2) Uani 1 1 d . . . C61 C 0.6062(3) 1.09414(15) 0.22052(14) 0.0301(7) Uani 1 1 d . . . C62 C 0.5473(3) 1.08056(15) 0.28140(14) 0.0291(7) Uani 1 1 d . . . C63 C 0.4346(3) 1.12350(15) 0.29117(14) 0.0297(7) Uani 1 1 d . . . C64 C 0.3835(3) 1.18132(16) 0.24047(16) 0.0395(8) Uani 1 1 d . . . H64 H 0.3064 1.2104 0.2469 0.047 Uiso 1 1 calc R . . C65 C 0.4448(3) 1.19640(17) 0.18096(16) 0.0433(9) Uani 1 1 d . . . H65 H 0.4117 1.2372 0.1468 0.052 Uiso 1 1 calc R . . C66 C 0.5545(3) 1.15221(17) 0.17092(15) 0.0383(8) Uani 1 1 d . . . H66 H 0.5946 1.1619 0.1295 0.046 Uiso 1 1 calc R . . O6 O 0.59830(17) 1.02429(10) 0.33210(9) 0.0301(5) Uani 1 1 d . . . C67 C 0.6915(3) 1.04786(16) 0.35982(14) 0.0356(7) Uani 1 1 d . . . H67A H 0.6526 1.0883 0.3772 0.043 Uiso 1 1 calc R . . H67B H 0.7592 1.0685 0.3273 0.043 Uiso 1 1 calc R . . C68 C 0.7462(3) 0.98146(16) 0.41157(13) 0.0305(7) Uani 1 1 d . . . N6 N 0.8475(2) 0.99449(14) 0.43456(12) 0.0366(6) Uani 1 1 d . . . C69 C 0.9001(3) 0.93756(19) 0.48068(15) 0.0428(8) Uani 1 1 d . . . H69 H 0.9722 0.9459 0.4972 0.051 Uiso 1 1 calc R . . C70 C 0.8568(3) 0.86720(19) 0.50601(16) 0.0488(9) Uani 1 1 d . . . H70 H 0.8983 0.8281 0.5386 0.059 Uiso 1 1 calc R . . C71 C 0.7510(4) 0.85538(18) 0.48251(15) 0.0483(9) Uani 1 1 d . . . H71 H 0.7173 0.8080 0.4995 0.058 Uiso 1 1 calc R . . C72 C 0.6946(3) 0.91302(17) 0.43420(14) 0.0371(8) Uani 1 1 d . . . H72 H 0.6225 0.9059 0.4170 0.045 Uiso 1 1 calc R . . S7 S 0.36233(8) 1.11198(4) 0.36844(4) 0.0389(2) Uani 1 1 d . . . C73 C 0.3231(3) 1.01697(16) 0.39531(14) 0.0313(7) Uani 1 1 d . . . C74 C 0.2419(3) 0.99272(16) 0.36391(13) 0.0290(7) Uani 1 1 d . . . C75 C 0.2041(2) 0.91958(16) 0.38947(13) 0.0278(7) Uani 1 1 d . . . C76 C 0.2453(3) 0.87259(17) 0.44707(14) 0.0353(8) Uani 1 1 d . . . H76 H 0.2186 0.8233 0.4653 0.042 Uiso 1 1 calc R . . C77 C 0.3249(3) 0.89715(19) 0.47801(14) 0.0400(8) Uani 1 1 d . . . H77 H 0.3525 0.8647 0.5176 0.048 Uiso 1 1 calc R . . C78 C 0.3647(3) 0.96782(18) 0.45237(14) 0.0372(8) Uani 1 1 d . . . H78 H 0.4213 0.9834 0.4738 0.045 Uiso 1 1 calc R . . O7 O 0.19878(16) 1.04025(10) 0.30718(9) 0.0299(5) Uani 1 1 d . . . C79 C 0.0839(3) 1.08621(17) 0.31639(14) 0.0361(8) Uani 1 1 d . . . H79A H 0.1010 1.1218 0.3376 0.043 Uiso 1 1 calc R . . H79B H 0.0211 1.0534 0.3438 0.043 Uiso 1 1 calc R . . C80 C 0.0319(3) 1.12991(15) 0.25417(14) 0.0303(7) Uani 1 1 d . . . N7 N -0.0836(2) 1.16663(13) 0.25987(12) 0.0327(6) Uani 1 1 d . . . C81 C -0.1378(3) 1.20548(16) 0.20676(16) 0.0385(8) Uani 1 1 d . . . H81 H -0.2193 1.2317 0.2101 0.046 Uiso 1 1 calc R . . C82 C -0.0837(3) 1.21028(17) 0.14741(16) 0.0446(9) Uani 1 1 d . . . H82 H -0.1266 1.2385 0.1108 0.053 Uiso 1 1 calc R . . C83 C 0.0346(3) 1.17281(19) 0.14276(16) 0.0502(9) Uani 1 1 d . . . H83 H 0.0755 1.1750 0.1025 0.060 Uiso 1 1 calc R . . C84 C 0.0934(3) 1.13188(18) 0.19709(15) 0.0408(8) Uani 1 1 d . . . H84 H 0.1752 1.1056 0.1948 0.049 Uiso 1 1 calc R . . S8 S 0.09199(7) 0.88901(4) 0.35390(4) 0.0353(2) Uani 1 1 d . . . C85 C 0.1661(3) 0.89456(16) 0.27813(13) 0.0293(7) Uani 1 1 d . . . C86 C 0.2840(3) 0.85609(15) 0.27059(13) 0.0275(7) Uani 1 1 d . . . C87 C 0.3387(3) 0.86124(15) 0.20975(14) 0.0304(7) Uani 1 1 d . . . C88 C 0.2710(3) 0.90121(16) 0.15769(14) 0.0349(7) Uani 1 1 d . . . H88 H 0.3070 0.9042 0.1165 0.042 Uiso 1 1 calc R . . C89 C 0.1506(3) 0.93690(17) 0.16565(15) 0.0408(8) Uani 1 1 d . . . H89 H 0.1034 0.9626 0.1301 0.049 Uiso 1 1 calc R . . C90 C 0.1000(3) 0.93497(17) 0.22529(15) 0.0381(8) Uani 1 1 d . . . H90 H 0.0194 0.9614 0.2304 0.046 Uiso 1 1 calc R . . O8 O 0.34790(17) 0.81355(10) 0.32287(9) 0.0297(5) Uani 1 1 d . . . C91 C 0.3186(3) 0.73591(16) 0.34607(14) 0.0375(8) Uani 1 1 d . . . H91A H 0.3483 0.7109 0.3139 0.045 Uiso 1 1 calc R . . H91B H 0.2260 0.7347 0.3542 0.045 Uiso 1 1 calc R . . C92 C 0.3813(3) 0.69444(16) 0.40565(13) 0.0325(7) Uani 1 1 d . . . N8 N 0.3455(3) 0.62498(14) 0.43380(13) 0.0460(7) Uani 1 1 d . . . C93 C 0.3968(4) 0.5835(2) 0.48721(17) 0.0578(10) Uani 1 1 d . . . H93 H 0.3711 0.5344 0.5082 0.069 Uiso 1 1 calc R . . C94 C 0.4846(4) 0.6073(2) 0.51391(17) 0.0592(11) Uani 1 1 d . . . H94 H 0.5196 0.5752 0.5518 0.071 Uiso 1 1 calc R . . C95 C 0.5206(3) 0.6789(2) 0.48438(16) 0.0524(10) Uani 1 1 d . . . H95 H 0.5810 0.6973 0.5015 0.063 Uiso 1 1 calc R . . C96 C 0.4673(3) 0.72344(18) 0.42935(15) 0.0387(8) Uani 1 1 d . . . H96 H 0.4897 0.7733 0.4082 0.046 Uiso 1 1 calc R . . O9 O 0.6499(3) 0.33156(16) 0.10759(14) 0.0834(9) Uani 1 1 d D . . O10 O 0.8775(3) 0.16699(14) 0.39762(12) 0.0586(7) Uani 1 1 d D . . H9A H 0.639(4) 0.3832(13) 0.0829(16) 0.120 Uiso 1 1 d D . . H9B H 0.639(5) 0.323(2) 0.1509(8) 0.120 Uiso 1 1 d D . . H10A H 0.876(3) 0.1828(17) 0.3561(8) 0.069 Uiso 1 1 d D . . H10B H 0.875(3) 0.1196(11) 0.4192(13) 0.069 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 S1 0.0303(4) 0.0385(5) 0.0437(5) -0.0138(4) -0.0147(4) 0.0031(3) C1 0.0254(16) 0.0314(16) 0.0304(17) -0.0108(14) -0.0093(14) -0.0064(13) C2 0.0250(16) 0.0274(16) 0.0255(16) -0.0055(13) -0.0062(13) -0.0083(13) C3 0.0293(16) 0.0267(16) 0.0303(17) -0.0101(13) -0.0087(14) -0.0064(13) C4 0.042(2) 0.0274(16) 0.0328(18) -0.0047(14) -0.0109(15) -0.0128(14) C5 0.040(2) 0.043(2) 0.0289(17) -0.0076(15) -0.0014(15) -0.0265(16) C6 0.0268(16) 0.0429(19) 0.0334(18) -0.0145(15) -0.0034(14) -0.0130(14) O1 0.0309(11) 0.0312(11) 0.0236(11) -0.0022(9) -0.0026(9) -0.0106(9) C7 0.052(2) 0.0408(19) 0.0274(18) -0.0040(15) -0.0063(16) -0.0144(16) C8 0.0398(19) 0.0325(17) 0.0276(17) -0.0078(14) -0.0012(15) -0.0031(14) C12 0.044(2) 0.043(2) 0.065(3) 0.0082(19) -0.0104(19) -0.0094(17) C11 0.063(3) 0.059(3) 0.070(3) 0.001(2) 0.004(2) -0.029(2) C10 0.094(3) 0.034(2) 0.039(2) -0.0037(18) 0.013(2) -0.020(2) C9 0.113(4) 0.040(2) 0.030(2) -0.0003(17) -0.015(2) -0.006(2) N1 0.076(2) 0.0409(17) 0.0331(16) -0.0021(14) -0.0205(15) -0.0041(15) S2 0.0375(5) 0.0354(4) 0.0441(5) -0.0203(4) -0.0068(4) -0.0011(4) C13 0.0271(16) 0.0244(15) 0.0350(18) -0.0103(14) -0.0027(14) 0.0041(13) C14 0.0247(16) 0.0228(15) 0.0284(17) -0.0033(13) 0.0006(14) 0.0016(12) C15 0.0251(16) 0.0288(16) 0.0304(17) -0.0048(13) -0.0058(14) 0.0005(13) C16 0.0288(17) 0.0396(19) 0.0359(19) -0.0012(15) -0.0029(15) -0.0049(14) C17 0.0363(19) 0.0427(19) 0.0286(18) 0.0005(15) 0.0037(15) -0.0082(15) C18 0.0406(19) 0.0335(18) 0.0282(17) -0.0037(14) -0.0039(15) 0.0016(15) O2 0.0279(11) 0.0262(11) 0.0314(11) -0.0051(9) 0.0001(9) 0.0018(9) C19 0.0425(19) 0.0293(17) 0.0379(19) -0.0083(14) -0.0003(16) 0.0029(14) C20 0.0389(19) 0.0343(18) 0.0287(17) -0.0088(14) -0.0025(15) -0.0111(15) N2 0.0574(18) 0.0338(16) 0.0379(17) 0.0017(13) -0.0011(15) -0.0073(14) C21 0.078(3) 0.046(2) 0.047(2) -0.0002(19) -0.008(2) -0.019(2) C22 0.070(3) 0.068(3) 0.042(2) -0.004(2) 0.012(2) -0.031(2) C23 0.044(2) 0.074(3) 0.050(2) -0.020(2) 0.0084(19) -0.019(2) C24 0.0356(19) 0.047(2) 0.0346(19) -0.0116(16) 0.0049(16) -0.0112(16) S3 0.0258(4) 0.0446(5) 0.0350(5) -0.0104(4) -0.0087(4) 0.0014(3) C25 0.0263(16) 0.0351(17) 0.0300(17) -0.0091(14) -0.0078(14) -0.0047(13) C26 0.0241(16) 0.0357(17) 0.0265(16) -0.0090(14) -0.0085(13) -0.0065(13) C27 0.0289(17) 0.0368(18) 0.0335(18) -0.0144(15) -0.0071(14) -0.0069(14) C28 0.0363(19) 0.050(2) 0.0362(19) -0.0212(17) -0.0005(16) -0.0092(16) C29 0.046(2) 0.049(2) 0.0306(18) -0.0119(16) 0.0011(16) -0.0177(17) C30 0.0397(19) 0.0399(19) 0.0314(18) -0.0111(15) -0.0051(16) -0.0073(15) O3 0.0307(11) 0.0329(11) 0.0299(12) -0.0050(9) -0.0053(9) -0.0103(9) C31 0.0346(18) 0.0406(19) 0.0390(19) -0.0103(15) -0.0091(15) -0.0098(15) C32 0.0276(17) 0.0276(16) 0.0396(19) -0.0099(14) -0.0021(15) -0.0008(13) N3 0.0372(15) 0.0314(14) 0.0480(17) -0.0141(13) -0.0014(14) -0.0072(12) C33 0.043(2) 0.0311(18) 0.062(3) -0.0114(18) 0.002(2) -0.0055(15) C34 0.052(2) 0.044(2) 0.047(2) -0.0005(18) 0.0036(19) -0.0060(18) C35 0.060(2) 0.063(2) 0.035(2) -0.0047(19) -0.0070(19) -0.004(2) C36 0.042(2) 0.045(2) 0.037(2) -0.0115(16) -0.0086(16) -0.0061(16) S4 0.0385(5) 0.0420(5) 0.0486(5) -0.0258(4) -0.0092(4) -0.0004(4) C37 0.0271(16) 0.0286(16) 0.0408(19) -0.0141(15) -0.0018(14) 0.0010(13) C38 0.0256(16) 0.0232(15) 0.0351(18) -0.0086(14) -0.0008(14) 0.0028(12) C39 0.0277(16) 0.0261(16) 0.0377(18) -0.0112(14) -0.0069(14) 0.0025(13) C40 0.0423(19) 0.0286(17) 0.0374(19) -0.0024(15) -0.0057(16) 0.0059(15) C41 0.046(2) 0.0271(17) 0.050(2) -0.0027(16) 0.0008(18) -0.0021(15) C42 0.0346(19) 0.0276(17) 0.062(2) -0.0135(17) -0.0040(17) -0.0037(14) O4 0.0283(11) 0.0300(11) 0.0333(12) -0.0093(9) 0.0004(9) -0.0035(9) C43 0.0294(17) 0.0357(18) 0.0362(18) -0.0102(15) 0.0013(15) 0.0012(14) C44 0.0335(18) 0.0402(19) 0.0269(17) -0.0147(14) -0.0060(14) -0.0049(14) N4 0.0304(15) 0.0475(17) 0.0305(15) -0.0130(13) 0.0001(12) -0.0062(12) C45 0.0384(19) 0.056(2) 0.038(2) -0.0224(18) 0.0038(16) -0.0102(17) C46 0.057(2) 0.054(2) 0.036(2) -0.0170(18) 0.0095(18) -0.0200(19) C47 0.063(3) 0.038(2) 0.039(2) -0.0116(17) -0.0029(19) 0.0003(17) C48 0.0422(19) 0.0354(18) 0.0349(18) -0.0133(15) -0.0017(16) -0.0036(15) S5 0.0352(4) 0.0354(4) 0.0420(5) -0.0194(4) 0.0015(4) -0.0055(4) C49 0.0230(15) 0.0278(16) 0.0265(16) -0.0107(13) 0.0039(13) -0.0001(12) C50 0.0213(15) 0.0265(16) 0.0239(16) -0.0059(13) 0.0057(13) 0.0013(12) C51 0.0218(15) 0.0274(16) 0.0298(17) -0.0084(13) 0.0059(13) -0.0022(12) C52 0.0214(15) 0.0422(19) 0.0306(17) -0.0138(15) 0.0014(14) -0.0019(14) C53 0.0314(17) 0.0390(19) 0.0254(16) -0.0055(14) -0.0030(14) 0.0081(14) C54 0.0354(18) 0.0234(16) 0.0341(18) -0.0066(14) 0.0040(15) 0.0011(13) O5 0.0277(11) 0.0287(11) 0.0268(11) -0.0022(9) -0.0013(9) -0.0003(9) C55 0.045(2) 0.0393(19) 0.0248(17) -0.0056(14) 0.0060(15) 0.0015(15) C56 0.0401(19) 0.0296(17) 0.0257(17) -0.0097(14) -0.0023(15) -0.0033(14) N5 0.0565(18) 0.0430(17) 0.0280(15) -0.0025(13) 0.0087(14) -0.0098(14) C57 0.092(3) 0.041(2) 0.031(2) -0.0047(17) 0.008(2) -0.008(2) C58 0.088(3) 0.038(2) 0.037(2) -0.0072(18) -0.017(2) 0.009(2) C59 0.053(2) 0.057(2) 0.061(3) -0.011(2) -0.014(2) 0.010(2) C60 0.043(2) 0.043(2) 0.044(2) 0.0058(17) -0.0026(17) -0.0050(17) S6 0.0297(4) 0.0347(4) 0.0450(5) -0.0122(4) 0.0103(4) -0.0120(3) C61 0.0308(17) 0.0230(15) 0.0355(18) -0.0067(14) 0.0013(15) -0.0103(13) C62 0.0318(17) 0.0228(15) 0.0328(18) -0.0060(13) -0.0034(14) -0.0095(13) C63 0.0284(16) 0.0259(16) 0.0364(18) -0.0125(14) 0.0016(14) -0.0060(13) C64 0.0374(19) 0.0281(17) 0.054(2) -0.0160(16) -0.0047(17) 0.0006(14) C65 0.050(2) 0.0307(18) 0.044(2) -0.0027(15) -0.0080(18) -0.0054(16) C66 0.047(2) 0.0330(18) 0.0325(18) -0.0069(15) 0.0043(16) -0.0120(15) O6 0.0304(11) 0.0266(11) 0.0328(12) -0.0068(9) -0.0028(9) -0.0082(9) C67 0.0337(17) 0.0346(18) 0.0404(19) -0.0112(15) -0.0068(15) -0.0093(14) C68 0.0282(17) 0.0354(18) 0.0267(16) -0.0113(14) 0.0030(14) -0.0004(14) N6 0.0298(14) 0.0458(16) 0.0330(15) -0.0122(13) -0.0010(12) -0.0026(12) C69 0.0390(19) 0.053(2) 0.0354(19) -0.0169(17) -0.0060(16) 0.0067(17) C70 0.058(2) 0.044(2) 0.036(2) -0.0081(17) -0.0075(18) 0.0119(18) C71 0.069(3) 0.0330(19) 0.039(2) -0.0076(16) -0.0004(19) -0.0054(18) C72 0.0398(19) 0.0352(18) 0.0351(18) -0.0104(15) -0.0006(15) -0.0042(15) S7 0.0387(5) 0.0395(5) 0.0448(5) -0.0233(4) 0.0064(4) -0.0085(4) C73 0.0261(16) 0.0373(17) 0.0314(17) -0.0160(15) 0.0074(14) -0.0025(13) C74 0.0239(16) 0.0356(18) 0.0261(16) -0.0107(14) 0.0041(13) -0.0019(13) C75 0.0223(15) 0.0338(17) 0.0265(16) -0.0107(14) 0.0039(13) -0.0032(13) C76 0.0389(19) 0.0342(18) 0.0298(18) -0.0099(15) 0.0062(15) -0.0022(14) C77 0.0401(19) 0.051(2) 0.0247(17) -0.0108(16) -0.0017(15) 0.0038(16) C78 0.0329(18) 0.049(2) 0.0333(18) -0.0190(16) -0.0013(15) -0.0034(15) O7 0.0243(11) 0.0329(11) 0.0288(11) -0.0069(9) 0.0006(9) -0.0003(9) C79 0.0284(17) 0.0396(18) 0.0367(19) -0.0110(15) 0.0016(15) 0.0019(14) C80 0.0288(17) 0.0223(15) 0.0376(19) -0.0062(13) 0.0012(15) -0.0069(13) N7 0.0292(14) 0.0253(13) 0.0419(16) -0.0084(12) -0.0045(12) -0.0017(11) C81 0.0354(18) 0.0215(16) 0.057(2) -0.0091(16) -0.0073(18) -0.0035(14) C82 0.046(2) 0.039(2) 0.043(2) -0.0023(16) -0.0102(18) -0.0059(16) C83 0.048(2) 0.059(2) 0.036(2) -0.0085(18) 0.0044(18) -0.0031(18) C84 0.0324(18) 0.043(2) 0.039(2) -0.0057(16) 0.0008(16) -0.0024(15) S8 0.0274(4) 0.0434(5) 0.0343(5) -0.0103(4) 0.0050(4) -0.0128(3) C85 0.0233(16) 0.0316(16) 0.0317(17) -0.0067(14) -0.0005(14) -0.0093(13) C86 0.0272(16) 0.0259(16) 0.0300(17) -0.0062(13) -0.0048(14) -0.0102(13) C87 0.0334(17) 0.0271(16) 0.0321(18) -0.0092(14) 0.0012(15) -0.0123(13) C88 0.0403(19) 0.0373(18) 0.0255(17) -0.0054(14) 0.0010(15) -0.0134(15) C89 0.040(2) 0.0412(19) 0.0324(19) 0.0042(15) -0.0107(16) -0.0077(16) C90 0.0283(17) 0.0405(19) 0.039(2) -0.0029(15) -0.0038(15) -0.0066(14) O8 0.0316(11) 0.0274(11) 0.0302(11) -0.0061(9) -0.0069(9) -0.0076(9) C91 0.048(2) 0.0266(17) 0.0391(19) -0.0072(14) -0.0113(16) -0.0096(14) C92 0.0350(18) 0.0325(18) 0.0274(17) -0.0073(14) -0.0012(14) -0.0017(14) N8 0.0563(18) 0.0324(16) 0.0407(17) -0.0001(13) -0.0055(14) -0.0047(13) C93 0.072(3) 0.043(2) 0.045(2) 0.0014(18) -0.007(2) -0.001(2) C94 0.066(3) 0.060(3) 0.039(2) -0.002(2) -0.018(2) 0.013(2) C95 0.049(2) 0.064(3) 0.043(2) -0.0151(19) -0.0185(18) 0.0041(19) C96 0.0355(18) 0.0417(19) 0.0402(19) -0.0138(16) -0.0055(16) -0.0047(15) O9 0.107(2) 0.0675(19) 0.077(2) -0.0230(17) -0.026(2) 0.0002(18) O10 0.0635(16) 0.0585(17) 0.0500(16) -0.0160(14) -0.0005(15) -0.0012(14) _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 S1 C1 1.773(3) . ? S1 C39 1.776(3) . ? C1 C2 1.389(4) . ? C1 C6 1.396(4) . ? C2 O1 1.378(3) . ? C2 C3 1.396(4) . ? C3 C4 1.396(4) . ? C3 S2 1.769(3) . ? C4 C5 1.371(4) . ? C4 H4 0.9500 . ? C5 C6 1.376(4) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? O1 C7 1.441(3) . ? C7 C8 1.503(4) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 N1 1.324(4) . ? C8 C12 1.358(5) . ? C12 C11 1.381(5) . ? C12 H12 0.9500 . ? C11 C10 1.347(5) . ? C11 H11 0.9500 . ? C10 C9 1.355(5) . ? C10 H10 0.9500 . ? C9 N1 1.347(4) . ? C9 H9 0.9500 . ? S2 C13 1.775(3) . ? C13 C18 1.382(4) . ? C13 C14 1.406(4) . ? C14 O2 1.378(3) . ? C14 C15 1.391(4) . ? C15 C16 1.388(4) . ? C15 S3 1.780(3) . ? C16 C17 1.376(4) . ? C16 H16 0.9500 . ? C17 C18 1.380(4) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? O2 C19 1.445(3) . ? C19 C20 1.496(4) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 N2 1.337(4) . ? C20 C24 1.376(4) . ? N2 C21 1.331(4) . ? C21 C22 1.360(5) . ? C21 H21 0.9500 . ? C22 C23 1.373(5) . ? C22 H22 0.9500 . ? C23 C24 1.381(4) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? S3 C25 1.778(3) . ? C25 C30 1.393(4) . ? C25 C26 1.393(4) . ? C26 O3 1.377(3) . ? C26 C27 1.402(4) . ? C27 C28 1.387(4) . ? C27 S4 1.781(3) . ? C28 C29 1.380(4) . ? C28 H28 0.9500 . ? C29 C30 1.369(4) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? O3 C31 1.428(3) . ? C31 C32 1.500(4) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 N3 1.340(4) . ? C32 C36 1.376(4) . ? N3 C33 1.346(4) . ? C33 C34 1.351(5) . ? C33 H33 0.9500 . ? C34 C35 1.369(5) . ? C34 H34 0.9500 . ? C35 C36 1.385(4) . ? C35 H35 0.9500 . ? C36 H36 0.9500 . ? S4 C37 1.773(3) . ? C37 C42 1.387(4) . ? C37 C38 1.401(4) . ? C38 O4 1.373(3) . ? C38 C39 1.407(4) . ? C39 C40 1.387(4) . ? C40 C41 1.391(5) . ? C40 H40 0.9500 . ? C41 C42 1.377(5) . ? C41 H41 0.9500 . ? C42 H42 0.9500 . ? O4 C43 1.437(3) . ? C43 C44 1.490(4) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 N4 1.347(4) . ? C44 C48 1.383(4) . ? N4 C45 1.330(4) . ? C45 C46 1.362(4) . ? C45 H45 0.9500 . ? C46 C47 1.376(5) . ? C46 H46 0.9500 . ? C47 C48 1.382(4) . ? C47 H47 0.9500 . ? C48 H48 0.9500 . ? S5 C49 1.769(3) . ? S5 C87 1.775(3) . ? C49 C54 1.395(4) . ? C49 C50 1.399(4) . ? C50 O5 1.373(3) . ? C50 C51 1.396(4) . ? C51 C52 1.395(4) . ? C51 S6 1.774(3) . ? C52 C53 1.386(4) . ? C52 H52 0.9500 . ? C53 C54 1.369(4) . ? C53 H53 0.9500 . ? C54 H54 0.9500 . ? O5 C55 1.435(3) . ? C55 C56 1.503(4) . ? C55 H55A 0.9900 . ? C55 H55B 0.9900 . ? C56 N5 1.325(4) . ? C56 C60 1.375(4) . ? N5 C57 1.339(4) . ? C57 C58 1.353(5) . ? C57 H57 0.9500 . ? C58 C59 1.363(5) . ? C58 H58 0.9500 . ? C59 C60 1.373(4) . ? C59 H59 0.9500 . ? C60 H60 0.9500 . ? S6 C61 1.774(3) . ? C61 C66 1.382(4) . ? C61 C62 1.398(4) . ? C62 O6 1.380(3) . ? C62 C63 1.395(4) . ? C63 C64 1.393(4) . ? C63 S7 1.777(3) . ? C64 C65 1.379(4) . ? C64 H64 0.9500 . ? C65 C66 1.385(4) . ? C65 H65 0.9500 . ? C66 H66 0.9500 . ? O6 C67 1.430(3) . ? C67 C68 1.500(4) . ? C67 H67A 0.9900 . ? C67 H67B 0.9900 . ? C68 N6 1.342(4) . ? C68 C72 1.386(4) . ? N6 C69 1.331(4) . ? C69 C70 1.379(5) . ? C69 H69 0.9500 . ? C70 C71 1.382(5) . ? C70 H70 0.9500 . ? C71 C72 1.382(4) . ? C71 H71 0.9500 . ? C72 H72 0.9500 . ? S7 C73 1.780(3) . ? C73 C78 1.390(4) . ? C73 C74 1.394(4) . ? C74 O7 1.381(3) . ? C74 C75 1.401(4) . ? C75 C76 1.386(4) . ? C75 S8 1.776(3) . ? C76 C77 1.378(4) . ? C76 H76 0.9500 . ? C77 C78 1.368(4) . ? C77 H77 0.9500 . ? C78 H78 0.9500 . ? O7 C79 1.440(3) . ? C79 C80 1.496(4) . ? C79 H79A 0.9900 . ? C79 H79B 0.9900 . ? C80 N7 1.347(3) . ? C80 C84 1.366(4) . ? N7 C81 1.329(4) . ? C81 C82 1.373(4) . ? C81 H81 0.9500 . ? C82 C83 1.374(4) . ? C82 H82 0.9500 . ? C83 C84 1.381(4) . ? C83 H83 0.9500 . ? C84 H84 0.9500 . ? S8 C85 1.773(3) . ? C85 C86 1.389(4) . ? C85 C90 1.394(4) . ? C86 O8 1.380(3) . ? C86 C87 1.404(4) . ? C87 C88 1.389(4) . ? C88 C89 1.391(4) . ? C88 H88 0.9500 . ? C89 C90 1.380(4) . ? C89 H89 0.9500 . ? C90 H90 0.9500 . ? O8 C91 1.445(3) . ? C91 C92 1.494(4) . ? C91 H91A 0.9900 . ? C91 H91B 0.9900 . ? C92 N8 1.337(4) . ? C92 C96 1.374(4) . ? N8 C93 1.330(4) . ? C93 C94 1.372(5) . ? C93 H93 0.9500 . ? C94 C95 1.376(5) . ? C94 H94 0.9500 . ? C95 C96 1.381(4) . ? C95 H95 0.9500 . ? C96 H96 0.9500 . ? O9 H9A 0.944(18) . ? O9 H9B 0.931(18) . ? O10 H10A 0.883(17) . ? O10 H10B 0.865(17) . ? 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 C1 S1 C39 101.71(13) . . ? C2 C1 C6 119.1(3) . . ? C2 C1 S1 122.1(2) . . ? C6 C1 S1 118.8(2) . . ? O1 C2 C1 120.0(2) . . ? O1 C2 C3 119.6(2) . . ? C1 C2 C3 120.3(2) . . ? C4 C3 C2 119.5(3) . . ? C4 C3 S2 118.7(2) . . ? C2 C3 S2 121.6(2) . . ? C5 C4 C3 120.0(3) . . ? C5 C4 H4 120.0 . . ? C3 C4 H4 120.0 . . ? C4 C5 C6 120.7(3) . . ? C4 C5 H5 119.7 . . ? C6 C5 H5 119.7 . . ? C5 C6 C1 120.5(3) . . ? C5 C6 H6 119.8 . . ? C1 C6 H6 119.8 . . ? C2 O1 C7 115.2(2) . . ? O1 C7 C8 107.1(2) . . ? O1 C7 H7A 110.3 . . ? C8 C7 H7A 110.3 . . ? O1 C7 H7B 110.3 . . ? C8 C7 H7B 110.3 . . ? H7A C7 H7B 108.5 . . ? N1 C8 C12 122.6(3) . . ? N1 C8 C7 114.9(3) . . ? C12 C8 C7 122.6(3) . . ? C8 C12 C11 119.3(3) . . ? C8 C12 H12 120.3 . . ? C11 C12 H12 120.3 . . ? C10 C11 C12 119.4(4) . . ? C10 C11 H11 120.3 . . ? C12 C11 H11 120.3 . . ? C11 C10 C9 117.6(3) . . ? C11 C10 H10 121.2 . . ? C9 C10 H10 121.2 . . ? N1 C9 C10 124.8(4) . . ? N1 C9 H9 117.6 . . ? C10 C9 H9 117.6 . . ? C8 N1 C9 116.3(3) . . ? C3 S2 C13 103.80(13) . . ? C18 C13 C14 119.3(3) . . ? C18 C13 S2 119.9(2) . . ? C14 C13 S2 120.6(2) . . ? O2 C14 C15 120.2(3) . . ? O2 C14 C13 120.2(3) . . ? C15 C14 C13 119.6(3) . . ? C16 C15 C14 119.8(3) . . ? C16 C15 S3 118.6(2) . . ? C14 C15 S3 121.4(2) . . ? C17 C16 C15 120.4(3) . . ? C17 C16 H16 119.8 . . ? C15 C16 H16 119.8 . . ? C16 C17 C18 120.1(3) . . ? C16 C17 H17 120.0 . . ? C18 C17 H17 120.0 . . ? C17 C18 C13 120.7(3) . . ? C17 C18 H18 119.6 . . ? C13 C18 H18 119.6 . . ? C14 O2 C19 112.28(19) . . ? O2 C19 C20 109.7(2) . . ? O2 C19 H19A 109.7 . . ? C20 C19 H19A 109.7 . . ? O2 C19 H19B 109.7 . . ? C20 C19 H19B 109.7 . . ? H19A C19 H19B 108.2 . . ? N2 C20 C24 123.0(3) . . ? N2 C20 C19 113.1(3) . . ? C24 C20 C19 123.9(3) . . ? C21 N2 C20 117.1(3) . . ? N2 C21 C22 124.2(3) . . ? N2 C21 H21 117.9 . . ? C22 C21 H21 117.9 . . ? C21 C22 C23 118.0(3) . . ? C21 C22 H22 121.0 . . ? C23 C22 H22 121.0 . . ? C22 C23 C24 119.6(3) . . ? C22 C23 H23 120.2 . . ? C24 C23 H23 120.2 . . ? C20 C24 C23 118.0(3) . . ? C20 C24 H24 121.0 . . ? C23 C24 H24 121.0 . . ? C25 S3 C15 103.92(13) . . ? C30 C25 C26 119.8(3) . . ? C30 C25 S3 118.5(2) . . ? C26 C25 S3 121.4(2) . . ? O3 C26 C25 119.9(2) . . ? O3 C26 C27 120.4(2) . . ? C25 C26 C27 119.7(3) . . ? C28 C27 C26 119.3(3) . . ? C28 C27 S4 118.4(2) . . ? C26 C27 S4 122.0(2) . . ? C29 C28 C27 120.6(3) . . ? C29 C28 H28 119.7 . . ? C27 C28 H28 119.7 . . ? C30 C29 C28 120.5(3) . . ? C30 C29 H29 119.8 . . ? C28 C29 H29 119.8 . . ? C29 C30 C25 120.3(3) . . ? C29 C30 H30 119.9 . . ? C25 C30 H30 119.9 . . ? C26 O3 C31 112.1(2) . . ? O3 C31 C32 110.2(3) . . ? O3 C31 H31A 109.6 . . ? C32 C31 H31A 109.6 . . ? O3 C31 H31B 109.6 . . ? C32 C31 H31B 109.6 . . ? H31A C31 H31B 108.1 . . ? N3 C32 C36 123.0(3) . . ? N3 C32 C31 113.3(3) . . ? C36 C32 C31 123.7(3) . . ? C32 N3 C33 116.8(3) . . ? N3 C33 C34 124.3(3) . . ? N3 C33 H33 117.9 . . ? C34 C33 H33 117.9 . . ? C33 C34 C35 118.1(3) . . ? C33 C34 H34 121.0 . . ? C35 C34 H34 121.0 . . ? C34 C35 C36 120.0(4) . . ? C34 C35 H35 120.0 . . ? C36 C35 H35 120.0 . . ? C32 C36 C35 117.9(3) . . ? C32 C36 H36 121.1 . . ? C35 C36 H36 121.1 . . ? C37 S4 C27 104.31(14) . . ? C42 C37 C38 119.5(3) . . ? C42 C37 S4 119.8(3) . . ? C38 C37 S4 120.6(2) . . ? O4 C38 C37 119.7(3) . . ? O4 C38 C39 120.5(3) . . ? C37 C38 C39 119.7(3) . . ? C40 C39 C38 119.6(3) . . ? C40 C39 S1 119.2(2) . . ? C38 C39 S1 121.1(2) . . ? C39 C40 C41 120.2(3) . . ? C39 C40 H40 119.9 . . ? C41 C40 H40 119.9 . . ? C42 C41 C40 120.2(3) . . ? C42 C41 H41 119.9 . . ? C40 C41 H41 119.9 . . ? C41 C42 C37 120.7(3) . . ? C41 C42 H42 119.6 . . ? C37 C42 H42 119.6 . . ? C38 O4 C43 112.9(2) . . ? O4 C43 C44 109.0(2) . . ? O4 C43 H43A 109.9 . . ? C44 C43 H43A 109.9 . . ? O4 C43 H43B 109.9 . . ? C44 C43 H43B 109.9 . . ? H43A C43 H43B 108.3 . . ? N4 C44 C48 122.9(3) . . ? N4 C44 C43 114.0(3) . . ? C48 C44 C43 123.1(3) . . ? C45 N4 C44 116.9(3) . . ? N4 C45 C46 124.3(3) . . ? N4 C45 H45 117.8 . . ? C46 C45 H45 117.8 . . ? C45 C46 C47 118.4(3) . . ? C45 C46 H46 120.8 . . ? C47 C46 H46 120.8 . . ? C46 C47 C48 119.2(3) . . ? C46 C47 H47 120.4 . . ? C48 C47 H47 120.4 . . ? C47 C48 C44 118.2(3) . . ? C47 C48 H48 120.9 . . ? C44 C48 H48 120.9 . . ? C49 S5 C87 103.28(13) . . ? C54 C49 C50 119.3(3) . . ? C54 C49 S5 118.8(2) . . ? C50 C49 S5 121.7(2) . . ? O5 C50 C51 120.5(2) . . ? O5 C50 C49 119.4(3) . . ? C51 C50 C49 119.9(3) . . ? C52 C51 C50 119.7(3) . . ? C52 C51 S6 118.7(2) . . ? C50 C51 S6 121.6(2) . . ? C53 C52 C51 120.0(3) . . ? C53 C52 H52 120.0 . . ? C51 C52 H52 120.0 . . ? C54 C53 C52 120.5(3) . . ? C54 C53 H53 119.8 . . ? C52 C53 H53 119.8 . . ? C53 C54 C49 120.7(3) . . ? C53 C54 H54 119.6 . . ? C49 C54 H54 119.6 . . ? C50 O5 C55 115.1(2) . . ? O5 C55 C56 107.7(2) . . ? O5 C55 H55A 110.2 . . ? C56 C55 H55A 110.2 . . ? O5 C55 H55B 110.2 . . ? C56 C55 H55B 110.2 . . ? H55A C55 H55B 108.5 . . ? N5 C56 C60 122.5(3) . . ? N5 C56 C55 115.0(3) . . ? C60 C56 C55 122.4(3) . . ? C56 N5 C57 116.3(3) . . ? N5 C57 C58 125.4(3) . . ? N5 C57 H57 117.3 . . ? C58 C57 H57 117.3 . . ? C57 C58 C59 117.3(3) . . ? C57 C58 H58 121.3 . . ? C59 C58 H58 121.3 . . ? C58 C59 C60 119.3(3) . . ? C58 C59 H59 120.3 . . ? C60 C59 H59 120.3 . . ? C59 C60 C56 119.1(3) . . ? C59 C60 H60 120.4 . . ? C56 C60 H60 120.4 . . ? C51 S6 C61 102.03(12) . . ? C66 C61 C62 119.4(3) . . ? C66 C61 S6 119.2(2) . . ? C62 C61 S6 121.3(2) . . ? O6 C62 C63 119.3(2) . . ? O6 C62 C61 120.8(2) . . ? C63 C62 C61 119.9(3) . . ? C64 C63 C62 119.8(3) . . ? C64 C63 S7 118.8(2) . . ? C62 C63 S7 121.1(2) . . ? C65 C64 C63 120.0(3) . . ? C65 C64 H64 120.0 . . ? C63 C64 H64 120.0 . . ? C64 C65 C66 120.2(3) . . ? C64 C65 H65 119.9 . . ? C66 C65 H65 119.9 . . ? C61 C66 C65 120.7(3) . . ? C61 C66 H66 119.7 . . ? C65 C66 H66 119.7 . . ? C62 O6 C67 113.9(2) . . ? O6 C67 C68 109.5(2) . . ? O6 C67 H67A 109.8 . . ? C68 C67 H67A 109.8 . . ? O6 C67 H67B 109.8 . . ? C68 C67 H67B 109.8 . . ? H67A C67 H67B 108.2 . . ? N6 C68 C72 123.2(3) . . ? N6 C68 C67 114.4(3) . . ? C72 C68 C67 122.4(3) . . ? C69 N6 C68 117.1(3) . . ? N6 C69 C70 124.2(3) . . ? N6 C69 H69 117.9 . . ? C70 C69 H69 117.9 . . ? C69 C70 C71 117.9(3) . . ? C69 C70 H70 121.1 . . ? C71 C70 H70 121.1 . . ? C72 C71 C70 119.5(3) . . ? C72 C71 H71 120.2 . . ? C70 C71 H71 120.2 . . ? C71 C72 C68 118.1(3) . . ? C71 C72 H72 120.9 . . ? C68 C72 H72 120.9 . . ? C63 S7 C73 103.66(13) . . ? C78 C73 C74 119.0(3) . . ? C78 C73 S7 119.0(2) . . ? C74 C73 S7 121.7(2) . . ? O7 C74 C73 120.4(3) . . ? O7 C74 C75 119.5(3) . . ? C73 C74 C75 120.2(3) . . ? C76 C75 C74 119.3(3) . . ? C76 C75 S8 118.9(2) . . ? C74 C75 S8 121.5(2) . . ? C77 C76 C75 120.1(3) . . ? C77 C76 H76 119.9 . . ? C75 C76 H76 119.9 . . ? C78 C77 C76 120.7(3) . . ? C78 C77 H77 119.7 . . ? C76 C77 H77 119.7 . . ? C77 C78 C73 120.7(3) . . ? C77 C78 H78 119.7 . . ? C73 C78 H78 119.7 . . ? C74 O7 C79 111.7(2) . . ? O7 C79 C80 110.1(2) . . ? O7 C79 H79A 109.6 . . ? C80 C79 H79A 109.6 . . ? O7 C79 H79B 109.6 . . ? C80 C79 H79B 109.6 . . ? H79A C79 H79B 108.2 . . ? N7 C80 C84 122.8(3) . . ? N7 C80 C79 113.1(3) . . ? C84 C80 C79 124.0(3) . . ? C81 N7 C80 116.9(3) . . ? N7 C81 C82 124.3(3) . . ? N7 C81 H81 117.8 . . ? C82 C81 H81 117.8 . . ? C81 C82 C83 117.7(3) . . ? C81 C82 H82 121.2 . . ? C83 C82 H82 121.2 . . ? C82 C83 C84 119.4(3) . . ? C82 C83 H83 120.3 . . ? C84 C83 H83 120.3 . . ? C80 C84 C83 118.8(3) . . ? C80 C84 H84 120.6 . . ? C83 C84 H84 120.6 . . ? C85 S8 C75 103.58(13) . . ? C86 C85 C90 119.7(3) . . ? C86 C85 S8 121.7(2) . . ? C90 C85 S8 118.5(2) . . ? O8 C86 C85 120.0(2) . . ? O8 C86 C87 120.1(2) . . ? C85 C86 C87 119.9(3) . . ? C88 C87 C86 119.6(3) . . ? C88 C87 S5 119.3(2) . . ? C86 C87 S5 120.9(2) . . ? C87 C88 C89 120.3(3) . . ? C87 C88 H88 119.9 . . ? C89 C88 H88 119.9 . . ? C90 C89 C88 119.9(3) . . ? C90 C89 H89 120.0 . . ? C88 C89 H89 120.0 . . ? C89 C90 C85 120.5(3) . . ? C89 C90 H90 119.8 . . ? C85 C90 H90 119.8 . . ? C86 O8 C91 112.0(2) . . ? O8 C91 C92 109.7(2) . . ? O8 C91 H91A 109.7 . . ? C92 C91 H91A 109.7 . . ? O8 C91 H91B 109.7 . . ? C92 C91 H91B 109.7 . . ? H91A C91 H91B 108.2 . . ? N8 C92 C96 123.0(3) . . ? N8 C92 C91 112.7(3) . . ? C96 C92 C91 124.3(3) . . ? C93 N8 C92 117.0(3) . . ? N8 C93 C94 124.1(3) . . ? N8 C93 H93 118.0 . . ? C94 C93 H93 118.0 . . ? C93 C94 C95 118.3(3) . . ? C93 C94 H94 120.9 . . ? C95 C94 H94 120.9 . . ? C94 C95 C96 118.8(4) . . ? C94 C95 H95 120.6 . . ? C96 C95 H95 120.6 . . ? C92 C96 C95 118.9(3) . . ? C92 C96 H96 120.6 . . ? C95 C96 H96 120.6 . . ? H9A O9 H9B 114(3) . . ? H10A O10 H10B 121(3) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 29.07 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.311 _refine_diff_density_min -0.510 _refine_diff_density_rms 0.068 data_global # Attachment 'web_deposit_cif_file_1_FERLAY_1361985472.3.cif' data_e2265a #TrackingRef 'web_deposit_cif_file_1_FERLAY_1361985472.3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C48 H36 N4 O4 S4' _chemical_formula_sum 'C48 H36 N4 O4 S4' _chemical_formula_weight 861.05 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 11.1018(6) _cell_length_b 16.7176(6) _cell_length_c 22.8556(11) _cell_angle_alpha 90.00 _cell_angle_beta 94.190(2) _cell_angle_gamma 90.00 _cell_volume 4230.6(3) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 3784 _cell_measurement_theta_min 2.33 _cell_measurement_theta_max 26.03 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.352 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1792 _exptl_absorpt_coefficient_mu 0.275 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9730 _exptl_absorpt_correction_T_max 0.9864 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20682 _diffrn_reflns_av_R_equivalents 0.0425 _diffrn_reflns_av_sigmaI/netI 0.0441 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 2.21 _diffrn_reflns_theta_max 28.28 _reflns_number_total 5255 _reflns_number_gt 3541 _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^)+(0.0473P)^2^+2.4822P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5255 _refine_ls_number_parameters 272 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0738 _refine_ls_R_factor_gt 0.0424 _refine_ls_wR_factor_ref 0.1132 _refine_ls_wR_factor_gt 0.0983 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.024 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group S1 S 1.0000 0.14921(4) 0.2500 0.02922(16) Uani 1 2 d S . . C1 C 0.88212(17) 0.21350(10) 0.26928(7) 0.0252(4) Uani 1 1 d . . . C2 C 0.82856(16) 0.26770(11) 0.22868(7) 0.0242(4) Uani 1 1 d . . . C3 C 0.73007(17) 0.31316(11) 0.24378(8) 0.0285(4) Uani 1 1 d . . . C4 C 0.68300(19) 0.30199(12) 0.29800(9) 0.0351(5) Uani 1 1 d . . . H4 H 0.6149 0.3321 0.3080 0.042 Uiso 1 1 calc R . . C5 C 0.73543(19) 0.24692(12) 0.33754(9) 0.0359(5) Uani 1 1 d . . . H5 H 0.7026 0.2391 0.3744 0.043 Uiso 1 1 calc R . . C6 C 0.83507(19) 0.20341(12) 0.32356(8) 0.0325(4) Uani 1 1 d . . . H6 H 0.8716 0.1665 0.3511 0.039 Uiso 1 1 calc R . . O1 O 0.87524(11) 0.27641(7) 0.17470(5) 0.0267(3) Uani 1 1 d . . . C7 C 0.8123(2) 0.22854(13) 0.13016(8) 0.0385(5) Uani 1 1 d . . . H7A H 0.7283 0.2480 0.1231 0.046 Uiso 1 1 calc R . . H7B H 0.8094 0.1723 0.1435 0.046 Uiso 1 1 calc R . . C8 C 0.87462(18) 0.23282(11) 0.07456(8) 0.0286(4) Uani 1 1 d . . . C9 C 0.84396(19) 0.17706(12) 0.03086(8) 0.0337(5) Uani 1 1 d . . . H9 H 0.7862 0.1373 0.0388 0.040 Uiso 1 1 calc R . . N1 N 0.89011(17) 0.17546(11) -0.02153(7) 0.0417(4) Uani 1 1 d . . . C10 C 0.9710(2) 0.23157(15) -0.03126(9) 0.0461(6) Uani 1 1 d . . . H10 H 1.0048 0.2320 -0.0683 0.055 Uiso 1 1 calc R . . C11 C 1.0090(2) 0.28921(14) 0.00918(9) 0.0459(6) Uani 1 1 d . . . H11 H 1.0679 0.3277 0.0002 0.055 Uiso 1 1 calc R . . C12 C 0.9596(2) 0.28993(13) 0.06309(8) 0.0379(5) Uani 1 1 d . . . H12 H 0.9838 0.3291 0.0917 0.046 Uiso 1 1 calc R . . S2 S 0.65562(5) 0.37989(3) 0.19277(2) 0.03943(15) Uani 1 1 d . . . C13 C 0.77061(17) 0.44679(11) 0.17348(8) 0.0288(4) Uani 1 1 d . . . C14 C 0.84028(17) 0.49047(11) 0.21586(7) 0.0271(4) Uani 1 1 d . . . C15 C 0.92071(19) 0.54840(11) 0.19882(8) 0.0307(4) Uani 1 1 d . . . C16 C 0.9299(2) 0.56318(12) 0.13932(8) 0.0366(5) Uani 1 1 d . . . H16 H 0.9841 0.6030 0.1274 0.044 Uiso 1 1 calc R . . C17 C 0.8605(2) 0.52011(13) 0.09731(8) 0.0377(5) Uani 1 1 d . . . H17 H 0.8671 0.5308 0.0568 0.045 Uiso 1 1 calc R . . C18 C 0.78194(19) 0.46173(12) 0.11408(8) 0.0343(5) Uani 1 1 d . . . H18 H 0.7356 0.4318 0.0852 0.041 Uiso 1 1 calc R . . O2 O 0.82903(12) 0.47514(7) 0.27471(5) 0.0301(3) Uani 1 1 d . . . C19 C 0.7355(3) 0.52295(15) 0.29703(9) 0.0539(7) Uani 1 1 d . . . H19A H 0.6614 0.5194 0.2703 0.065 Uiso 1 1 calc R . . H19B H 0.7612 0.5796 0.2993 0.065 Uiso 1 1 calc R . . C20 C 0.7096(2) 0.49357(12) 0.35704(8) 0.0335(5) Uani 1 1 d . . . C21 C 0.7996(2) 0.46350(14) 0.39659(9) 0.0431(5) Uani 1 1 d . . . H21 H 0.8797 0.4614 0.3846 0.052 Uiso 1 1 calc R . . N2 N 0.78035(18) 0.43730(12) 0.45047(7) 0.0458(5) Uani 1 1 d . . . C22 C 0.6668(2) 0.43935(14) 0.46539(9) 0.0445(6) Uani 1 1 d . . . H22 H 0.6507 0.4203 0.5032 0.053 Uiso 1 1 calc R . . C23 C 0.5713(2) 0.46738(14) 0.42941(10) 0.0452(6) Uani 1 1 d . . . H23 H 0.4917 0.4674 0.4421 0.054 Uiso 1 1 calc R . . C24 C 0.5938(2) 0.49545(12) 0.37462(8) 0.0372(5) Uani 1 1 d . . . H24 H 0.5298 0.5160 0.3491 0.045 Uiso 1 1 calc R . . S3 S 1.0000 0.61312(4) 0.2500 0.0428(2) Uani 1 2 d S . . 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 S1 0.0296(4) 0.0211(3) 0.0366(3) 0.000 -0.0006(3) 0.000 C1 0.0245(10) 0.0229(9) 0.0278(9) -0.0015(7) -0.0003(7) -0.0038(8) C2 0.0235(10) 0.0254(9) 0.0235(8) -0.0002(7) 0.0002(7) -0.0053(8) C3 0.0236(10) 0.0266(10) 0.0347(10) 0.0007(7) -0.0007(8) -0.0034(8) C4 0.0289(11) 0.0356(11) 0.0417(11) -0.0039(9) 0.0098(9) -0.0023(9) C5 0.0397(12) 0.0359(11) 0.0336(10) -0.0001(8) 0.0124(9) -0.0061(10) C6 0.0390(12) 0.0299(10) 0.0286(9) 0.0045(8) 0.0018(8) -0.0056(9) O1 0.0285(7) 0.0289(7) 0.0227(6) 0.0004(5) 0.0003(5) -0.0042(6) C7 0.0445(13) 0.0453(12) 0.0256(9) -0.0033(8) 0.0011(9) -0.0165(11) C8 0.0317(11) 0.0275(10) 0.0259(9) 0.0024(7) -0.0025(8) 0.0014(8) C9 0.0365(12) 0.0315(11) 0.0325(10) -0.0028(8) -0.0014(8) 0.0009(9) N1 0.0430(11) 0.0468(11) 0.0356(9) -0.0085(8) 0.0038(8) 0.0022(9) C10 0.0455(14) 0.0646(16) 0.0291(10) -0.0033(10) 0.0085(10) 0.0020(12) C11 0.0471(14) 0.0527(14) 0.0387(11) 0.0041(10) 0.0096(10) -0.0119(12) C12 0.0441(13) 0.0373(12) 0.0324(10) -0.0037(8) 0.0026(9) -0.0063(10) S2 0.0259(3) 0.0414(3) 0.0500(3) 0.0099(2) -0.0044(2) 0.0047(2) C13 0.0277(10) 0.0274(10) 0.0307(9) 0.0022(7) -0.0013(8) 0.0083(8) C14 0.0356(11) 0.0237(9) 0.0217(8) 0.0017(7) 0.0002(7) 0.0110(8) C15 0.0429(12) 0.0236(9) 0.0246(9) 0.0001(7) -0.0041(8) 0.0049(9) C16 0.0457(13) 0.0331(11) 0.0304(10) 0.0079(8) -0.0013(9) 0.0006(10) C17 0.0469(13) 0.0438(12) 0.0218(9) 0.0038(8) -0.0018(9) 0.0067(10) C18 0.0382(12) 0.0372(11) 0.0260(9) -0.0020(8) -0.0081(8) 0.0072(10) O2 0.0410(8) 0.0276(7) 0.0218(6) 0.0031(5) 0.0033(5) 0.0127(6) C19 0.0804(19) 0.0497(14) 0.0341(11) 0.0103(10) 0.0226(12) 0.0390(14) C20 0.0459(13) 0.0281(10) 0.0271(9) -0.0024(8) 0.0065(8) 0.0077(9) C21 0.0404(13) 0.0530(14) 0.0367(11) 0.0077(10) 0.0082(9) 0.0081(11) N2 0.0448(12) 0.0628(13) 0.0292(9) 0.0076(8) -0.0010(8) 0.0013(10) C22 0.0480(14) 0.0574(15) 0.0281(10) 0.0072(10) 0.0031(9) -0.0071(12) C23 0.0356(13) 0.0543(14) 0.0461(12) 0.0080(10) 0.0061(10) -0.0076(11) C24 0.0416(13) 0.0328(11) 0.0356(10) -0.0019(8) -0.0077(9) -0.0015(10) S3 0.0702(6) 0.0220(4) 0.0337(4) 0.000 -0.0138(4) 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 S1 C1 1.7737(19) 2_755 ? S1 C1 1.7737(19) . ? C1 C6 1.391(2) . ? C1 C2 1.398(2) . ? C2 O1 1.380(2) . ? C2 C3 1.395(3) . ? C3 C4 1.392(3) . ? C3 S2 1.7737(19) . ? C4 C5 1.388(3) . ? C4 H4 0.9500 . ? C5 C6 1.381(3) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? O1 C7 1.436(2) . ? C7 C8 1.492(3) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C12 1.381(3) . ? C8 C9 1.390(3) . ? C9 N1 1.337(2) . ? C9 H9 0.9500 . ? N1 C10 1.329(3) . ? C10 C11 1.380(3) . ? C10 H10 0.9500 . ? C11 C12 1.385(3) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? S2 C13 1.777(2) . ? C13 C18 1.395(2) . ? C13 C14 1.400(3) . ? C14 O2 1.384(2) . ? C14 C15 1.392(3) . ? C15 C16 1.393(2) . ? C15 S3 1.7786(19) . ? C16 C17 1.388(3) . ? C16 H16 0.9500 . ? C17 C18 1.382(3) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? O2 C19 1.434(2) . ? C19 C20 1.504(3) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 C24 1.374(3) . ? C20 C21 1.391(3) . ? C21 N2 1.339(3) . ? C21 H21 0.9500 . ? N2 C22 1.330(3) . ? C22 C23 1.376(3) . ? C22 H22 0.9500 . ? C23 C24 1.377(3) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? S3 C15 1.7787(19) 2_755 ? 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 C1 S1 C1 105.41(12) 2_755 . ? C6 C1 C2 120.08(17) . . ? C6 C1 S1 118.68(14) . . ? C2 C1 S1 120.91(13) . . ? O1 C2 C3 121.04(16) . . ? O1 C2 C1 119.48(16) . . ? C3 C2 C1 119.46(16) . . ? C4 C3 C2 119.92(17) . . ? C4 C3 S2 118.83(15) . . ? C2 C3 S2 121.06(14) . . ? C5 C4 C3 120.11(19) . . ? C5 C4 H4 119.9 . . ? C3 C4 H4 119.9 . . ? C6 C5 C4 120.25(18) . . ? C6 C5 H5 119.9 . . ? C4 C5 H5 119.9 . . ? C5 C6 C1 120.12(18) . . ? C5 C6 H6 119.9 . . ? C1 C6 H6 119.9 . . ? C2 O1 C7 112.33(14) . . ? O1 C7 C8 110.19(16) . . ? O1 C7 H7A 109.6 . . ? C8 C7 H7A 109.6 . . ? O1 C7 H7B 109.6 . . ? C8 C7 H7B 109.6 . . ? H7A C7 H7B 108.1 . . ? C12 C8 C9 117.52(18) . . ? C12 C8 C7 124.10(17) . . ? C9 C8 C7 118.37(18) . . ? N1 C9 C8 124.6(2) . . ? N1 C9 H9 117.7 . . ? C8 C9 H9 117.7 . . ? C10 N1 C9 116.35(18) . . ? N1 C10 C11 123.9(2) . . ? N1 C10 H10 118.0 . . ? C11 C10 H10 118.0 . . ? C10 C11 C12 118.7(2) . . ? C10 C11 H11 120.6 . . ? C12 C11 H11 120.6 . . ? C8 C12 C11 118.91(19) . . ? C8 C12 H12 120.5 . . ? C11 C12 H12 120.5 . . ? C3 S2 C13 104.49(9) . . ? C18 C13 C14 119.70(18) . . ? C18 C13 S2 118.14(15) . . ? C14 C13 S2 121.81(14) . . ? O2 C14 C15 120.41(16) . . ? O2 C14 C13 119.44(17) . . ? C15 C14 C13 120.16(16) . . ? C14 C15 C16 119.40(17) . . ? C14 C15 S3 122.40(13) . . ? C16 C15 S3 117.77(15) . . ? C17 C16 C15 120.44(19) . . ? C17 C16 H16 119.8 . . ? C15 C16 H16 119.8 . . ? C18 C17 C16 120.30(18) . . ? C18 C17 H17 119.8 . . ? C16 C17 H17 119.8 . . ? C17 C18 C13 119.99(18) . . ? C17 C18 H18 120.0 . . ? C13 C18 H18 120.0 . . ? C14 O2 C19 111.21(14) . . ? O2 C19 C20 109.52(16) . . ? O2 C19 H19A 109.8 . . ? C20 C19 H19A 109.8 . . ? O2 C19 H19B 109.8 . . ? C20 C19 H19B 109.8 . . ? H19A C19 H19B 108.2 . . ? C24 C20 C21 117.42(18) . . ? C24 C20 C19 120.27(19) . . ? C21 C20 C19 122.3(2) . . ? N2 C21 C20 124.1(2) . . ? N2 C21 H21 117.9 . . ? C20 C21 H21 117.9 . . ? C22 N2 C21 116.42(19) . . ? N2 C22 C23 123.99(19) . . ? N2 C22 H22 118.0 . . ? C23 C22 H22 118.0 . . ? C22 C23 C24 118.4(2) . . ? C22 C23 H23 120.8 . . ? C24 C23 H23 120.8 . . ? C20 C24 C23 119.59(19) . . ? C20 C24 H24 120.2 . . ? C23 C24 H24 120.2 . . ? C15 S3 C15 105.07(12) . 2_755 ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.262 _refine_diff_density_min -0.333 _refine_diff_density_rms 0.050 data_global # Attachment 'web_deposit_cif_file_2_FERLAY_1361985472.4.cif' data_e2262a #TrackingRef 'web_deposit_cif_file_2_FERLAY_1361985472.4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C48 H36 N4 O4 S4' _chemical_formula_sum 'C48 H36 N4 O4 S4' _chemical_formula_weight 861.05 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 23.3704(5) _cell_length_b 12.3507(3) _cell_length_c 16.9803(7) _cell_angle_alpha 90.00 _cell_angle_beta 120.7310(10) _cell_angle_gamma 90.00 _cell_volume 4213.0(2) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9963 _cell_measurement_theta_min 2.67 _cell_measurement_theta_max 29.21 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.358 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1792 _exptl_absorpt_coefficient_mu 0.276 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9676 _exptl_absorpt_correction_T_max 0.9782 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 53835 _diffrn_reflns_av_R_equivalents 0.0388 _diffrn_reflns_av_sigmaI/netI 0.0317 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.94 _diffrn_reflns_theta_max 30.09 _reflns_number_total 5886 _reflns_number_gt 4259 _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^)+(0.0486P)^2^+3.6359P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5886 _refine_ls_number_parameters 271 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0674 _refine_ls_R_factor_gt 0.0411 _refine_ls_wR_factor_ref 0.1084 _refine_ls_wR_factor_gt 0.0962 _refine_ls_goodness_of_fit_ref 1.012 _refine_ls_restrained_S_all 1.012 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group S1 S 0.194925(19) 0.23554(3) 0.39125(3) 0.02661(11) Uani 1 1 d . . . C1 C 0.13765(7) 0.30163(12) 0.41455(10) 0.0238(3) Uani 1 1 d . . . C2 C 0.09485(7) 0.24227(12) 0.43223(10) 0.0220(3) Uani 1 1 d . . . C3 C 0.05040(8) 0.29582(12) 0.45066(10) 0.0244(3) Uani 1 1 d . . . C4 C 0.05127(9) 0.40841(13) 0.45442(11) 0.0303(4) Uani 1 1 d . . . H4 H 0.0208 0.4453 0.4664 0.036 Uiso 1 1 calc R . . C5 C 0.09578(9) 0.46720(13) 0.44092(11) 0.0334(4) Uani 1 1 d . . . H5 H 0.0970 0.5439 0.4459 0.040 Uiso 1 1 calc R . . C6 C 0.13849(8) 0.41416(13) 0.42013(11) 0.0289(4) Uani 1 1 d . . . H6 H 0.1685 0.4546 0.4096 0.035 Uiso 1 1 calc R . . O1 O 0.09481(5) 0.13074(8) 0.42915(7) 0.0248(2) Uani 1 1 d . . . C7 C 0.14384(8) 0.08356(13) 0.51477(11) 0.0288(3) Uani 1 1 d . . . H7A H 0.1320 0.0978 0.5621 0.035 Uiso 1 1 calc R . . H7B H 0.1880 0.1162 0.5353 0.035 Uiso 1 1 calc R . . C8 C 0.14655(8) -0.03634(13) 0.50219(11) 0.0282(3) Uani 1 1 d . . . C9 C 0.20073(10) -0.09549(15) 0.56679(14) 0.0406(4) Uani 1 1 d . . . H9 H 0.2363 -0.0606 0.6186 0.049 Uiso 1 1 calc R . . C10 C 0.20236(11) -0.20635(16) 0.55477(17) 0.0520(5) Uani 1 1 d . . . H10 H 0.2403 -0.2454 0.5990 0.062 Uiso 1 1 calc R . . N1 N 0.15422(10) -0.26110(13) 0.48539(14) 0.0502(5) Uani 1 1 d . . . C11 C 0.10287(11) -0.20307(15) 0.42460(15) 0.0439(5) Uani 1 1 d . . . H11 H 0.0677 -0.2405 0.3742 0.053 Uiso 1 1 calc R . . C12 C 0.09639(9) -0.09154(14) 0.42887(13) 0.0341(4) Uani 1 1 d . . . H12 H 0.0584 -0.0545 0.3825 0.041 Uiso 1 1 calc R . . S2 S -0.00320(2) 0.22296(4) 0.47706(3) 0.02915(11) Uani 1 1 d . . . C13 C -0.05781(7) 0.15742(12) 0.37148(10) 0.0237(3) Uani 1 1 d . . . C14 C -0.09869(7) 0.21644(12) 0.29209(10) 0.0212(3) Uani 1 1 d . . . C15 C 0.14144(7) 0.16265(12) 0.28951(10) 0.0224(3) Uani 1 1 d . . . C16 C 0.14562(8) 0.05014(13) 0.29025(11) 0.0272(3) Uani 1 1 d . . . H16 H 0.1750 0.0133 0.3457 0.033 Uiso 1 1 calc R . . C17 C -0.06298(8) 0.04545(13) 0.36897(11) 0.0287(3) Uani 1 1 d . . . H17 H -0.0356 0.0048 0.4230 0.034 Uiso 1 1 calc R . . C18 C -0.10733(9) -0.00810(13) 0.28915(12) 0.0310(4) Uani 1 1 d . . . H18 H -0.1114 -0.0846 0.2890 0.037 Uiso 1 1 calc R . . O2 O -0.09626(5) 0.32800(8) 0.29310(7) 0.0244(2) Uani 1 1 d . . . C19 C -0.14136(9) 0.37484(13) 0.31697(12) 0.0303(4) Uani 1 1 d . . . H19A H -0.1280 0.3544 0.3805 0.036 Uiso 1 1 calc R . . H19B H -0.1869 0.3471 0.2755 0.036 Uiso 1 1 calc R . . C20 C -0.14059(8) 0.49550(12) 0.30924(10) 0.0260(3) Uani 1 1 d . . . C21 C -0.09767(9) 0.54983(14) 0.29030(12) 0.0345(4) Uani 1 1 d . . . H21 H -0.0666 0.5113 0.2806 0.041 Uiso 1 1 calc R . . C22 C -0.10061(11) 0.66211(15) 0.28558(14) 0.0451(5) Uani 1 1 d . . . H22 H -0.0705 0.6987 0.2727 0.054 Uiso 1 1 calc R . . N2 N -0.14266(9) 0.72167(12) 0.29787(12) 0.0469(4) Uani 1 1 d . . . C23 C -0.18355(10) 0.66819(15) 0.31637(14) 0.0431(5) Uani 1 1 d . . . H23 H -0.2140 0.7089 0.3259 0.052 Uiso 1 1 calc R . . C24 C -0.18456(9) 0.55697(14) 0.32256(12) 0.0350(4) Uani 1 1 d . . . H24 H -0.2151 0.5228 0.3358 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 S1 0.0205(2) 0.0328(2) 0.02429(19) -0.00628(15) 0.00979(15) -0.00377(15) C1 0.0232(8) 0.0252(7) 0.0200(7) -0.0043(6) 0.0088(6) -0.0024(6) C2 0.0243(8) 0.0201(7) 0.0181(6) -0.0033(5) 0.0083(6) -0.0023(6) C3 0.0248(8) 0.0272(8) 0.0203(7) -0.0016(6) 0.0110(6) -0.0009(6) C4 0.0353(9) 0.0275(8) 0.0280(8) -0.0046(6) 0.0160(7) 0.0054(7) C5 0.0446(10) 0.0193(7) 0.0331(9) -0.0044(6) 0.0176(8) -0.0007(7) C6 0.0338(9) 0.0241(8) 0.0272(8) -0.0027(6) 0.0145(7) -0.0072(6) O1 0.0260(6) 0.0192(5) 0.0253(5) -0.0021(4) 0.0102(5) -0.0022(4) C7 0.0310(9) 0.0246(8) 0.0271(8) 0.0018(6) 0.0123(7) -0.0014(6) C8 0.0328(9) 0.0241(8) 0.0351(9) 0.0027(6) 0.0228(7) -0.0016(6) C9 0.0393(10) 0.0328(9) 0.0461(11) 0.0081(8) 0.0191(9) 0.0004(8) C10 0.0508(13) 0.0352(11) 0.0709(15) 0.0155(10) 0.0317(12) 0.0102(9) N1 0.0615(12) 0.0261(8) 0.0770(13) 0.0043(8) 0.0456(11) 0.0033(8) C11 0.0543(13) 0.0297(9) 0.0565(12) -0.0087(8) 0.0348(11) -0.0089(9) C12 0.0358(10) 0.0283(9) 0.0411(10) -0.0027(7) 0.0217(8) -0.0022(7) S2 0.0270(2) 0.0402(2) 0.02166(19) 0.00046(16) 0.01350(16) -0.00161(17) C13 0.0218(8) 0.0284(8) 0.0231(7) 0.0034(6) 0.0131(6) -0.0003(6) C14 0.0209(7) 0.0209(7) 0.0252(7) 0.0029(6) 0.0144(6) 0.0002(6) C15 0.0201(7) 0.0246(7) 0.0245(7) -0.0043(6) 0.0130(6) -0.0012(6) C16 0.0271(8) 0.0253(8) 0.0313(8) 0.0022(6) 0.0164(7) 0.0034(6) C17 0.0306(9) 0.0267(8) 0.0302(8) 0.0102(6) 0.0165(7) 0.0047(6) C18 0.0371(10) 0.0213(7) 0.0404(9) 0.0041(7) 0.0240(8) 0.0005(7) O2 0.0273(6) 0.0195(5) 0.0309(6) 0.0018(4) 0.0182(5) 0.0007(4) C19 0.0344(9) 0.0226(8) 0.0433(10) -0.0003(7) 0.0267(8) 0.0010(6) C20 0.0264(8) 0.0237(8) 0.0235(7) -0.0007(6) 0.0097(6) 0.0007(6) C21 0.0403(10) 0.0273(9) 0.0419(10) 0.0013(7) 0.0254(8) 0.0007(7) C22 0.0585(13) 0.0293(9) 0.0560(12) 0.0030(8) 0.0355(11) -0.0043(9) N2 0.0609(11) 0.0239(8) 0.0567(11) 0.0011(7) 0.0306(9) 0.0054(7) C23 0.0458(11) 0.0321(10) 0.0504(11) -0.0017(8) 0.0238(10) 0.0090(8) C24 0.0320(9) 0.0327(9) 0.0398(10) -0.0007(7) 0.0179(8) 0.0038(7) _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 S1 C15 1.7749(15) . ? S1 C1 1.7764(16) . ? C1 C2 1.391(2) . ? C1 C6 1.393(2) . ? C2 O1 1.3785(17) . ? C2 C3 1.395(2) . ? C3 C4 1.392(2) . ? C3 S2 1.7760(16) . ? C4 C5 1.380(2) . ? C4 H4 0.9500 . ? C5 C6 1.382(2) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? O1 C7 1.4366(18) . ? C7 C8 1.502(2) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C12 1.377(2) . ? C8 C9 1.386(2) . ? C9 C10 1.388(3) . ? C9 H9 0.9500 . ? C10 N1 1.325(3) . ? C10 H10 0.9500 . ? N1 C11 1.324(3) . ? C11 C12 1.392(3) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? S2 C13 1.7776(16) . ? C13 C17 1.387(2) . ? C13 C14 1.395(2) . ? C14 O2 1.3788(17) . ? C14 C15 1.395(2) 2 ? C15 C16 1.393(2) . ? C15 C14 1.395(2) 2 ? C16 C18 1.379(2) 2 ? C16 H16 0.9500 . ? C17 C18 1.383(2) . ? C17 H17 0.9500 . ? C18 C16 1.379(2) 2 ? C18 H18 0.9500 . ? O2 C19 1.4306(19) . ? C19 C20 1.497(2) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 C21 1.375(2) . ? C20 C24 1.386(2) . ? C21 C22 1.389(2) . ? C21 H21 0.9500 . ? C22 N2 1.327(3) . ? C22 H22 0.9500 . ? N2 C23 1.325(3) . ? C23 C24 1.379(3) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C15 S1 C1 102.35(7) . . ? C2 C1 C6 119.86(15) . . ? C2 C1 S1 120.84(12) . . ? C6 C1 S1 119.20(12) . . ? O1 C2 C1 120.35(13) . . ? O1 C2 C3 119.73(13) . . ? C1 C2 C3 119.90(14) . . ? C4 C3 C2 119.26(15) . . ? C4 C3 S2 119.36(12) . . ? C2 C3 S2 121.23(12) . . ? C5 C4 C3 120.83(15) . . ? C5 C4 H4 119.6 . . ? C3 C4 H4 119.6 . . ? C4 C5 C6 119.80(15) . . ? C4 C5 H5 120.1 . . ? C6 C5 H5 120.1 . . ? C5 C6 C1 120.24(15) . . ? C5 C6 H6 119.9 . . ? C1 C6 H6 119.9 . . ? C2 O1 C7 112.47(11) . . ? O1 C7 C8 109.01(13) . . ? O1 C7 H7A 109.9 . . ? C8 C7 H7A 109.9 . . ? O1 C7 H7B 109.9 . . ? C8 C7 H7B 109.9 . . ? H7A C7 H7B 108.3 . . ? C12 C8 C9 117.76(16) . . ? C12 C8 C7 122.57(15) . . ? C9 C8 C7 119.66(16) . . ? C8 C9 C10 119.10(19) . . ? C8 C9 H9 120.5 . . ? C10 C9 H9 120.5 . . ? N1 C10 C9 124.0(2) . . ? N1 C10 H10 118.0 . . ? C9 C10 H10 118.0 . . ? C11 N1 C10 115.87(17) . . ? N1 C11 C12 125.06(19) . . ? N1 C11 H11 117.5 . . ? C12 C11 H11 117.5 . . ? C8 C12 C11 118.17(17) . . ? C8 C12 H12 120.9 . . ? C11 C12 H12 120.9 . . ? C3 S2 C13 102.22(7) . . ? C17 C13 C14 119.05(14) . . ? C17 C13 S2 119.43(12) . . ? C14 C13 S2 121.40(12) . . ? O2 C14 C15 119.51(13) . 2 ? O2 C14 C13 120.45(13) . . ? C15 C14 C13 120.03(13) 2 . ? C16 C15 C14 119.71(14) . 2 ? C16 C15 S1 119.08(12) . . ? C14 C15 S1 121.07(11) 2 . ? C18 C16 C15 120.27(15) 2 . ? C18 C16 H16 119.9 2 . ? C15 C16 H16 119.9 . . ? C18 C17 C13 121.11(14) . . ? C18 C17 H17 119.4 . . ? C13 C17 H17 119.4 . . ? C16 C18 C17 119.70(15) 2 . ? C16 C18 H18 120.2 2 . ? C17 C18 H18 120.2 . . ? C14 O2 C19 112.07(11) . . ? O2 C19 C20 109.52(13) . . ? O2 C19 H19A 109.8 . . ? C20 C19 H19A 109.8 . . ? O2 C19 H19B 109.8 . . ? C20 C19 H19B 109.8 . . ? H19A C19 H19B 108.2 . . ? C21 C20 C24 117.47(15) . . ? C21 C20 C19 123.33(15) . . ? C24 C20 C19 119.20(15) . . ? C20 C21 C22 118.71(17) . . ? C20 C21 H21 120.6 . . ? C22 C21 H21 120.6 . . ? N2 C22 C21 124.29(18) . . ? N2 C22 H22 117.9 . . ? C21 C22 H22 117.9 . . ? C23 N2 C22 116.29(16) . . ? N2 C23 C24 123.88(18) . . ? N2 C23 H23 118.1 . . ? C24 C23 H23 118.1 . . ? C23 C24 C20 119.35(18) . . ? C23 C24 H24 120.3 . . ? C20 C24 H24 120.3 . . ? _diffrn_measured_fraction_theta_max 0.950 _diffrn_reflns_theta_full 30.09 _diffrn_measured_fraction_theta_full 0.950 _refine_diff_density_max 0.375 _refine_diff_density_min -0.282 _refine_diff_density_rms 0.052 data_global # Attachment 'web_deposit_cif_file_3_FERLAY_1361985472.2-HgCl2.cif' data_e2308a #TrackingRef 'web_deposit_cif_file_3_FERLAY_1361985472.2-HgCl2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H18 Cl2 Hg N2 O2 S2' _chemical_formula_sum 'C24 H18 Cl2 Hg N2 O2 S2' _chemical_formula_weight 702.01 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' S S 0.1246 0.1234 '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 Orthorhombic _symmetry_space_group_name_H-M Ccca _symmetry_space_group_name_Hall '-C 2b 2bc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z' '-x, y, -z+1/2' 'x+1/2, -y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1, -y+1/2, z' '-x+1/2, y+1/2, -z+1/2' 'x+1, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z' 'x, -y, z-1/2' '-x-1/2, y, z-1/2' '-x+1/2, -y+1/2, -z' 'x, y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' '-x, y+1/2, z-1/2' _cell_length_a 14.3514(3) _cell_length_b 21.4182(3) _cell_length_c 15.7934(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4854.59(15) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9977 _cell_measurement_theta_min 2.58 _cell_measurement_theta_max 30.06 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.921 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2704 _exptl_absorpt_coefficient_mu 6.758 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6139 _exptl_absorpt_correction_T_max 0.7738 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29956 _diffrn_reflns_av_R_equivalents 0.0253 _diffrn_reflns_av_sigmaI/netI 0.0128 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.14 _diffrn_reflns_theta_max 30.08 _reflns_number_total 3579 _reflns_number_gt 3004 _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^)+(0.0204P)^2^+7.4274P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3579 _refine_ls_number_parameters 151 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0224 _refine_ls_R_factor_gt 0.0163 _refine_ls_wR_factor_ref 0.0439 _refine_ls_wR_factor_gt 0.0412 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.032 _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 Hg1 Hg 0.2500 1.0000 1.027925(6) 0.02517(4) Uani 1 2 d S . . Cl1 Cl 0.39146(4) 1.03035(2) 1.09556(4) 0.03699(12) Uani 1 1 d . . . S1 S 0.0000 0.93481(3) 0.7500 0.02500(13) Uani 1 2 d S . . C1 C -0.05898(13) 0.88221(8) 0.81852(11) 0.0209(3) Uani 1 1 d . . . C2 C -0.01030(12) 0.84062(8) 0.87010(10) 0.0203(3) Uani 1 1 d . . . C3 C -0.05899(13) 0.80104(8) 0.92542(11) 0.0231(3) Uani 1 1 d . . . C4 C -0.15580(14) 0.80486(9) 0.92932(12) 0.0285(4) Uani 1 1 d . . . H4 H -0.1892 0.7781 0.9664 0.034 Uiso 1 1 calc R . . C5 C -0.20347(13) 0.84715(10) 0.87987(13) 0.0298(4) Uani 1 1 d . . . H5 H -0.2694 0.8498 0.8837 0.036 Uiso 1 1 calc R . . C6 C -0.15576(13) 0.88572(9) 0.82475(12) 0.0266(4) Uani 1 1 d . . . H6 H -0.1891 0.9148 0.7909 0.032 Uiso 1 1 calc R . . S2 S 0.0000 0.7500 0.99573(4) 0.02930(14) Uani 1 2 d S . . O1 O 0.08500(9) 0.83584(6) 0.86450(8) 0.0219(3) Uani 1 1 d . . . C7 C 0.13385(13) 0.88123(9) 0.91435(12) 0.0263(4) Uani 1 1 d . . . H7A H 0.1240 0.8729 0.9754 0.032 Uiso 1 1 calc R . . H7B H 0.1103 0.9236 0.9015 0.032 Uiso 1 1 calc R . . C8 C 0.23563(12) 0.87710(9) 0.89347(12) 0.0225(3) Uani 1 1 d . . . N1 N 0.29100(11) 0.92138(7) 0.92738(10) 0.0236(3) Uani 1 1 d . . . C9 C 0.38266(14) 0.91971(10) 0.91083(14) 0.0319(4) Uani 1 1 d . . . H9 H 0.4216 0.9506 0.9355 0.038 Uiso 1 1 calc R . . C10 C 0.42283(16) 0.87520(11) 0.85974(16) 0.0408(5) Uani 1 1 d . . . H10 H 0.4878 0.8758 0.8481 0.049 Uiso 1 1 calc R . . C11 C 0.36566(16) 0.82935(11) 0.82575(16) 0.0395(5) Uani 1 1 d . . . H11 H 0.3913 0.7976 0.7908 0.047 Uiso 1 1 calc R . . C12 C 0.27162(14) 0.83019(10) 0.84291(14) 0.0296(4) Uani 1 1 d . . . H12 H 0.2319 0.7989 0.8203 0.036 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Hg1 0.01772(5) 0.02494(6) 0.03286(6) 0.000 0.000 -0.00335(4) Cl1 0.0264(2) 0.0347(3) 0.0499(3) 0.0128(2) -0.0153(2) -0.0109(2) S1 0.0274(3) 0.0185(3) 0.0291(3) 0.000 0.0030(3) 0.000 C1 0.0200(8) 0.0192(8) 0.0235(8) -0.0041(6) 0.0019(6) -0.0024(6) C2 0.0199(8) 0.0204(8) 0.0206(7) -0.0060(6) 0.0012(6) -0.0037(6) C3 0.0267(9) 0.0224(8) 0.0201(8) -0.0041(6) 0.0023(7) -0.0029(7) C4 0.0262(10) 0.0309(9) 0.0282(9) -0.0050(7) 0.0082(7) -0.0080(8) C5 0.0163(9) 0.0357(10) 0.0373(11) -0.0128(8) 0.0053(7) -0.0027(8) C6 0.0233(9) 0.0268(9) 0.0296(9) -0.0076(7) 0.0002(7) 0.0027(7) S2 0.0398(4) 0.0287(3) 0.0193(3) 0.000 0.000 -0.0017(3) O1 0.0163(6) 0.0218(6) 0.0276(6) -0.0059(5) -0.0008(5) -0.0026(5) C7 0.0203(9) 0.0290(9) 0.0296(9) -0.0080(7) -0.0016(7) -0.0038(7) C8 0.0205(9) 0.0223(8) 0.0246(8) 0.0018(7) -0.0024(6) -0.0016(6) N1 0.0196(7) 0.0219(7) 0.0293(8) -0.0019(6) -0.0004(6) -0.0032(6) C9 0.0202(9) 0.0324(10) 0.0432(11) -0.0063(9) 0.0023(8) -0.0058(8) C10 0.0217(10) 0.0437(13) 0.0570(14) -0.0156(11) 0.0078(9) -0.0028(9) C11 0.0268(11) 0.0408(12) 0.0507(13) -0.0185(10) 0.0049(9) 0.0005(9) C12 0.0263(10) 0.0276(9) 0.0350(10) -0.0083(8) -0.0014(8) -0.0018(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Hg1 Cl1 2.3843(5) 2_575 ? Hg1 Cl1 2.3844(5) . ? Hg1 N1 2.3881(15) 2_575 ? Hg1 N1 2.3882(15) . ? S1 C1 1.7768(18) . ? S1 C1 1.7769(18) 3_556 ? C1 C6 1.394(3) . ? C1 C2 1.395(3) . ? C2 O1 1.374(2) . ? C2 C3 1.404(2) . ? C3 C4 1.393(3) . ? C3 S2 1.7733(19) . ? C4 C5 1.378(3) . ? C4 H4 0.9500 . ? C5 C6 1.382(3) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? S2 C3 1.7734(19) 6_465 ? O1 C7 1.434(2) . ? C7 C8 1.500(3) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 N1 1.348(2) . ? C8 C12 1.383(3) . ? N1 C9 1.342(2) . ? C9 C10 1.376(3) . ? C9 H9 0.9500 . ? C10 C11 1.388(3) . ? C10 H10 0.9500 . ? C11 C12 1.377(3) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl1 Hg1 Cl1 126.77(3) 2_575 . ? Cl1 Hg1 N1 106.28(4) 2_575 2_575 ? Cl1 Hg1 N1 108.39(4) . 2_575 ? Cl1 Hg1 N1 108.39(4) 2_575 . ? Cl1 Hg1 N1 106.28(4) . . ? N1 Hg1 N1 96.65(8) 2_575 . ? C1 S1 C1 101.29(11) . 3_556 ? C6 C1 C2 119.49(17) . . ? C6 C1 S1 118.90(15) . . ? C2 C1 S1 121.47(14) . . ? O1 C2 C1 120.56(16) . . ? O1 C2 C3 119.38(16) . . ? C1 C2 C3 119.99(17) . . ? C4 C3 C2 119.24(18) . . ? C4 C3 S2 118.99(15) . . ? C2 C3 S2 121.63(14) . . ? C5 C4 C3 120.58(18) . . ? C5 C4 H4 119.7 . . ? C3 C4 H4 119.7 . . ? C4 C5 C6 120.28(18) . . ? C4 C5 H5 119.9 . . ? C6 C5 H5 119.9 . . ? C5 C6 C1 120.38(19) . . ? C5 C6 H6 119.8 . . ? C1 C6 H6 119.8 . . ? C3 S2 C3 102.46(12) . 6_465 ? C2 O1 C7 113.62(13) . . ? O1 C7 C8 108.39(15) . . ? O1 C7 H7A 110.0 . . ? C8 C7 H7A 110.0 . . ? O1 C7 H7B 110.0 . . ? C8 C7 H7B 110.0 . . ? H7A C7 H7B 108.4 . . ? N1 C8 C12 121.34(17) . . ? N1 C8 C7 116.43(17) . . ? C12 C8 C7 122.23(17) . . ? C9 N1 C8 118.79(17) . . ? C9 N1 Hg1 112.95(12) . . ? C8 N1 Hg1 127.95(13) . . ? N1 C9 C10 122.94(19) . . ? N1 C9 H9 118.5 . . ? C10 C9 H9 118.5 . . ? C9 C10 C11 118.0(2) . . ? C9 C10 H10 121.0 . . ? C11 C10 H10 121.0 . . ? C12 C11 C10 119.6(2) . . ? C12 C11 H11 120.2 . . ? C10 C11 H11 120.2 . . ? C11 C12 C8 119.29(19) . . ? C11 C12 H12 120.4 . . ? C8 C12 H12 120.4 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 30.08 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.034 _refine_diff_density_min -0.502 _refine_diff_density_rms 0.070 data_global # Attachment 'web_deposit_cif_file_4_FERLAY_1361985472.3-HgCl2.cif' data_e2310a #TrackingRef 'web_deposit_cif_file_4_FERLAY_1361985472.3-HgCl2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C96 H72 Cl8 Hg4 N8 O8 S8, 2(CH4O),2(CHCl3),H2O' _chemical_formula_sum 'C100 H84 Cl14 Hg4 N8 O11 S8' _chemical_formula_weight 3128.89 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Hg Hg -2.3894 9.2266 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.0664(2) _cell_length_b 10.3405(2) _cell_length_c 28.7661(6) _cell_angle_alpha 88.8900(10) _cell_angle_beta 81.2840(10) _cell_angle_gamma 67.8680(10) _cell_volume 2739.33(10) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9426 _cell_measurement_theta_min 2.42 _cell_measurement_theta_max 30.08 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.897 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1514 _exptl_absorpt_coefficient_mu 6.143 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6393 _exptl_absorpt_correction_T_max 0.7487 _exptl_absorpt_process_details sadabs _exptl_special_details ; The hydrogen atoms on the water molecule were not found but are taken into account in the compound formula. ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 53387 _diffrn_reflns_av_R_equivalents 0.0310 _diffrn_reflns_av_sigmaI/netI 0.0301 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -40 _diffrn_reflns_limit_l_max 40 _diffrn_reflns_theta_min 2.13 _diffrn_reflns_theta_max 29.02 _reflns_number_total 14201 _reflns_number_gt 11677 _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^)+(0.0416P)^2^+5.3803P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 14201 _refine_ls_number_parameters 655 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0473 _refine_ls_R_factor_gt 0.0346 _refine_ls_wR_factor_ref 0.0893 _refine_ls_wR_factor_gt 0.0837 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.045 _refine_ls_shift/su_max 0.010 _refine_ls_shift/su_mean 0.016 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Hg1 Hg 0.187107(18) 0.823859(17) 0.977222(5) 0.03121(5) Uani 1 1 d . . . Cl1 Cl 0.24426(13) 0.64392(11) 1.03164(4) 0.0375(2) Uani 1 1 d . . . Cl2 Cl 0.13802(12) 1.06541(11) 0.96550(4) 0.0348(2) Uani 1 1 d . . . Hg2 Hg -0.35448(2) 1.36667(2) 0.540781(6) 0.03846(6) Uani 1 1 d . . . Cl3 Cl -0.48450(15) 1.27899(15) 0.60007(4) 0.0511(3) Uani 1 1 d . . . Cl4 Cl -0.39615(13) 1.60790(11) 0.51949(4) 0.0370(2) Uani 1 1 d . . . S1 S 0.48481(12) 0.56405(11) 0.71420(4) 0.0339(2) Uani 1 1 d . . . C1 C 0.4393(4) 0.7319(4) 0.69008(14) 0.0290(8) Uani 1 1 d . . . C2 C 0.3868(4) 0.8536(4) 0.71879(13) 0.0245(8) Uani 1 1 d . . . C3 C 0.3606(4) 0.9827(4) 0.69816(15) 0.0293(9) Uani 1 1 d . . . C4 C 0.3900(5) 0.9866(5) 0.64916(16) 0.0388(11) Uani 1 1 d . . . H4 H 0.3710 1.0739 0.6348 0.047 Uiso 1 1 calc R . . C5 C 0.4459(5) 0.8653(6) 0.62169(15) 0.0403(11) Uani 1 1 d . . . H5 H 0.4678 0.8695 0.5885 0.048 Uiso 1 1 calc R . . C6 C 0.4705(5) 0.7375(5) 0.64169(15) 0.0367(10) Uani 1 1 d . . . H6 H 0.5086 0.6541 0.6224 0.044 Uiso 1 1 calc R . . O1 O 0.3624(3) 0.8435(3) 0.76703(9) 0.0254(6) Uani 1 1 d . . . C7 C 0.4862(5) 0.8301(5) 0.78861(14) 0.0325(9) Uani 1 1 d . . . H7A H 0.4822 0.9238 0.7973 0.039 Uiso 1 1 calc R . . H7B H 0.5765 0.7829 0.7662 0.039 Uiso 1 1 calc R . . C8 C 0.4859(4) 0.7462(4) 0.83181(14) 0.0282(8) Uani 1 1 d . . . C9 C 0.3908(5) 0.8042(5) 0.87271(14) 0.0313(9) Uani 1 1 d . . . H9 H 0.3256 0.8987 0.8729 0.038 Uiso 1 1 calc R . . N1 N 0.3861(4) 0.7341(4) 0.91199(12) 0.0325(8) Uani 1 1 d . . . C10 C 0.4784(5) 0.6018(4) 0.91208(15) 0.0331(9) Uani 1 1 d . . . H10 H 0.4761 0.5514 0.9400 0.040 Uiso 1 1 calc R . . C11 C 0.5767(5) 0.5361(5) 0.87302(16) 0.0375(10) Uani 1 1 d . . . H11 H 0.6416 0.4419 0.8740 0.045 Uiso 1 1 calc R . . C12 C 0.5801(5) 0.6083(5) 0.83257(15) 0.0336(9) Uani 1 1 d . . . H12 H 0.6467 0.5639 0.8052 0.040 Uiso 1 1 calc R . . S2 S 0.31378(13) 1.13996(12) 0.73161(4) 0.0372(3) Uani 1 1 d . . . C13 C 0.1613(5) 1.1500(4) 0.77310(14) 0.0307(9) Uani 1 1 d . . . C14 C 0.0286(5) 1.1666(4) 0.75980(13) 0.0268(8) Uani 1 1 d . . . C15 C -0.0912(5) 1.1848(4) 0.79445(15) 0.0309(9) Uani 1 1 d . . . C16 C -0.0783(6) 1.1947(4) 0.84198(15) 0.0401(11) Uani 1 1 d . . . H16 H -0.1599 1.2087 0.8656 0.048 Uiso 1 1 calc R . . C17 C 0.0513(6) 1.1843(5) 0.85465(16) 0.0443(13) Uani 1 1 d . . . H17 H 0.0581 1.1949 0.8868 0.053 Uiso 1 1 calc R . . C18 C 0.1714(6) 1.1586(4) 0.82077(16) 0.0391(11) Uani 1 1 d . . . H18 H 0.2621 1.1465 0.8299 0.047 Uiso 1 1 calc R . . O2 O 0.0155(3) 1.1680(3) 0.71249(9) 0.0258(6) Uani 1 1 d . . . C19 C -0.0361(6) 1.3108(4) 0.69807(15) 0.0358(10) Uani 1 1 d . . . H19A H 0.0225 1.3595 0.7088 0.043 Uiso 1 1 calc R . . H19B H -0.1385 1.3603 0.7127 0.043 Uiso 1 1 calc R . . C20 C -0.0246(5) 1.3137(4) 0.64529(14) 0.0311(9) Uani 1 1 d . . . C21 C -0.1416(5) 1.3221(4) 0.62322(14) 0.0316(9) Uani 1 1 d . . . H21 H -0.2279 1.3224 0.6420 0.038 Uiso 1 1 calc R . . N2 N -0.1368(4) 1.3298(4) 0.57654(12) 0.0345(8) Uani 1 1 d . . . C22 C -0.0157(6) 1.3309(5) 0.55045(16) 0.0429(11) Uani 1 1 d . . . H22 H -0.0129 1.3385 0.5174 0.052 Uiso 1 1 calc R . . C23 C 0.1049(6) 1.3218(6) 0.56927(18) 0.0456(12) Uani 1 1 d . . . H23 H 0.1899 1.3213 0.5496 0.055 Uiso 1 1 calc R . . C24 C 0.0997(5) 1.3132(5) 0.61783(17) 0.0379(10) Uani 1 1 d . . . H24 H 0.1814 1.3071 0.6318 0.046 Uiso 1 1 calc R . . S3 S -0.26423(13) 1.21124(12) 0.78064(5) 0.0412(3) Uani 1 1 d . . . C25 C -0.2349(4) 1.0663(4) 0.74368(16) 0.0310(9) Uani 1 1 d . . . C26 C -0.1664(4) 0.9261(4) 0.75613(14) 0.0252(8) Uani 1 1 d . . . C27 C -0.1581(4) 0.8184(4) 0.72605(14) 0.0281(8) Uani 1 1 d . . . C28 C -0.2167(5) 0.8483(5) 0.68419(15) 0.0360(10) Uani 1 1 d . . . H28 H -0.2094 0.7744 0.6636 0.043 Uiso 1 1 calc R . . C29 C -0.2854(5) 0.9855(6) 0.67286(17) 0.0436(12) Uani 1 1 d . . . H29 H -0.3266 1.0056 0.6447 0.052 Uiso 1 1 calc R . . C30 C -0.2944(5) 1.0927(5) 0.70205(18) 0.0401(11) Uani 1 1 d . . . H30 H -0.3418 1.1866 0.6938 0.048 Uiso 1 1 calc R . . O3 O -0.1041(3) 0.8928(3) 0.79624(9) 0.0291(6) Uani 1 1 d . . . C31 C -0.2025(5) 0.9107(5) 0.83954(15) 0.0390(10) Uani 1 1 d . . . H31A H -0.2870 0.8896 0.8340 0.047 Uiso 1 1 calc R . . H31B H -0.2383 1.0087 0.8517 0.047 Uiso 1 1 calc R . . C32 C -0.1249(5) 0.8143(5) 0.87480(14) 0.0336(9) Uani 1 1 d . . . C33 C -0.0217(5) 0.8403(4) 0.89608(15) 0.0330(9) Uani 1 1 d . . . H33 H 0.0022 0.9185 0.8867 0.040 Uiso 1 1 calc R . . N3 N 0.0453(4) 0.7603(4) 0.92902(12) 0.0322(8) Uani 1 1 d . . . C34 C 0.0124(6) 0.6491(5) 0.94173(16) 0.0429(11) Uani 1 1 d . . . H34 H 0.0601 0.5913 0.9650 0.051 Uiso 1 1 calc R . . C35 C -0.0872(7) 0.6160(6) 0.92236(18) 0.0498(13) Uani 1 1 d . . . H35 H -0.1075 0.5359 0.9317 0.060 Uiso 1 1 calc R . . C36 C -0.1573(6) 0.7005(6) 0.88915(18) 0.0466(12) Uani 1 1 d . . . H36 H -0.2287 0.6802 0.8760 0.056 Uiso 1 1 calc R . . S4 S -0.10163(12) 0.64286(11) 0.74237(4) 0.0315(2) Uani 1 1 d . . . C37 C 0.0708(5) 0.5943(4) 0.76051(14) 0.0270(8) Uani 1 1 d . . . C38 C 0.1870(4) 0.6175(4) 0.73415(13) 0.0252(8) Uani 1 1 d . . . C39 C 0.3236(5) 0.5623(4) 0.74820(15) 0.0284(8) Uani 1 1 d . . . C40 C 0.3412(5) 0.4858(4) 0.78876(16) 0.0358(10) Uani 1 1 d . . . H40 H 0.4335 0.4494 0.7988 0.043 Uiso 1 1 calc R . . C41 C 0.2260(6) 0.4625(5) 0.81445(17) 0.0407(11) Uani 1 1 d . . . H41 H 0.2395 0.4095 0.8419 0.049 Uiso 1 1 calc R . . C42 C 0.0907(5) 0.5159(4) 0.80055(16) 0.0362(10) Uani 1 1 d . . . H42 H 0.0116 0.4991 0.8183 0.043 Uiso 1 1 calc R . . O4 O 0.1657(3) 0.6987(3) 0.69540(9) 0.0247(6) Uani 1 1 d . . . C43 C 0.1834(5) 0.6213(4) 0.65250(14) 0.0322(9) Uani 1 1 d . . . H43A H 0.1079 0.5811 0.6543 0.039 Uiso 1 1 calc R . . H43B H 0.2798 0.5438 0.6474 0.039 Uiso 1 1 calc R . . C44 C 0.1706(4) 0.7188(4) 0.61264(14) 0.0267(8) Uani 1 1 d . . . C45 C 0.2291(5) 0.6642(4) 0.56784(14) 0.0291(8) Uani 1 1 d . . . H45 H 0.2771 0.5657 0.5634 0.035 Uiso 1 1 calc R . . N4 N 0.2220(4) 0.7427(4) 0.52988(12) 0.0333(8) Uani 1 1 d . . . C46 C 0.1544(5) 0.8811(5) 0.53635(17) 0.0406(11) Uani 1 1 d . . . H46 H 0.1485 0.9377 0.5097 0.049 Uiso 1 1 calc R . . C47 C 0.0927(6) 0.9447(5) 0.58030(17) 0.0417(11) Uani 1 1 d . . . H47 H 0.0451 1.0435 0.5838 0.050 Uiso 1 1 calc R . . C48 C 0.1010(5) 0.8633(4) 0.61924(15) 0.0323(9) Uani 1 1 d . . . H48 H 0.0600 0.9050 0.6499 0.039 Uiso 1 1 calc R . . C49 C 0.851(3) 0.685(2) 0.5648(9) 0.308(11) Uani 1 1 d D . . H49A H 0.9566 0.6411 0.5637 0.462 Uiso 1 1 calc R . . H49B H 0.8199 0.6318 0.5440 0.462 Uiso 1 1 calc R . . H49C H 0.8028 0.6860 0.5971 0.462 Uiso 1 1 calc R . . O5 O 0.8105(18) 0.8364(19) 0.5484(7) 0.308(11) Uani 1 1 d D . . H5A H 0.7217 0.8820 0.5576 0.462 Uiso 1 1 calc R . . O6 O 0.5579(14) 0.9775(19) 0.5000(9) 0.215(11) Uani 0.50 1 d P . . C51 C 0.4423(6) 0.1601(5) 0.94448(19) 0.0458(12) Uani 1 1 d . . . H51 H 0.3736 0.1105 0.9512 0.055 Uiso 1 1 calc R . . Cl5 Cl 0.3744(2) 0.31484(18) 0.97919(7) 0.0727(5) Uani 1 1 d . . . Cl6 Cl 0.61239(16) 0.05078(16) 0.95677(5) 0.0581(4) Uani 1 1 d . . . Cl7 Cl 0.45712(19) 0.1991(2) 0.88465(6) 0.0737(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 Hg1 0.03368(10) 0.03364(9) 0.02466(8) 0.00793(6) -0.00641(7) -0.01050(8) Cl1 0.0437(7) 0.0350(5) 0.0311(5) 0.0134(4) -0.0093(5) -0.0110(5) Cl2 0.0340(6) 0.0327(5) 0.0352(5) 0.0091(4) -0.0041(5) -0.0107(5) Hg2 0.03856(11) 0.04864(11) 0.02457(8) 0.01030(7) -0.00442(8) -0.01302(9) Cl3 0.0522(8) 0.0659(8) 0.0401(6) 0.0262(6) -0.0112(6) -0.0277(7) Cl4 0.0431(7) 0.0366(5) 0.0263(5) 0.0035(4) -0.0025(5) -0.0107(5) S1 0.0253(6) 0.0297(5) 0.0390(6) -0.0016(5) 0.0001(5) -0.0034(5) C1 0.023(2) 0.035(2) 0.0273(19) 0.0018(17) -0.0017(18) -0.0097(19) C2 0.019(2) 0.034(2) 0.0216(17) 0.0031(16) -0.0018(16) -0.0112(17) C3 0.026(2) 0.035(2) 0.031(2) 0.0084(17) -0.0070(18) -0.0157(19) C4 0.038(3) 0.054(3) 0.032(2) 0.018(2) -0.012(2) -0.024(2) C5 0.042(3) 0.064(3) 0.0195(19) 0.006(2) -0.002(2) -0.026(3) C6 0.034(3) 0.052(3) 0.0217(19) -0.0048(19) 0.0037(19) -0.016(2) O1 0.0222(15) 0.0333(14) 0.0195(12) 0.0034(11) -0.0024(11) -0.0095(12) C7 0.030(2) 0.048(2) 0.0256(19) 0.0085(18) -0.0092(18) -0.020(2) C8 0.025(2) 0.039(2) 0.0237(18) 0.0064(17) -0.0068(17) -0.0146(19) C9 0.027(2) 0.033(2) 0.027(2) 0.0080(17) -0.0028(18) -0.0050(19) N1 0.032(2) 0.0347(18) 0.0240(16) 0.0068(15) 0.0005(16) -0.0068(17) C10 0.035(3) 0.031(2) 0.028(2) 0.0082(17) -0.006(2) -0.007(2) C11 0.040(3) 0.031(2) 0.036(2) 0.0028(19) -0.010(2) -0.006(2) C12 0.029(2) 0.037(2) 0.028(2) -0.0028(18) -0.0007(19) -0.006(2) S2 0.0388(6) 0.0332(5) 0.0469(6) 0.0060(5) -0.0118(5) -0.0202(5) C13 0.044(3) 0.0215(17) 0.029(2) 0.0026(16) -0.0111(19) -0.0127(19) C14 0.039(2) 0.0189(16) 0.0217(17) 0.0015(14) -0.0045(18) -0.0098(18) C15 0.038(3) 0.0171(17) 0.031(2) -0.0014(16) -0.0004(19) -0.0040(18) C16 0.059(3) 0.0233(19) 0.025(2) -0.0010(17) 0.008(2) -0.007(2) C17 0.073(4) 0.030(2) 0.028(2) 0.0005(18) -0.019(3) -0.013(2) C18 0.057(3) 0.029(2) 0.034(2) 0.0032(18) -0.020(2) -0.014(2) O2 0.0325(16) 0.0217(12) 0.0218(13) 0.0010(10) -0.0061(12) -0.0080(12) C19 0.052(3) 0.0239(19) 0.027(2) 0.0033(16) -0.013(2) -0.007(2) C20 0.042(3) 0.0218(18) 0.0271(19) 0.0047(16) -0.0087(19) -0.0077(19) C21 0.034(2) 0.033(2) 0.0250(19) 0.0052(17) -0.0043(18) -0.0091(19) N2 0.035(2) 0.042(2) 0.0244(17) 0.0095(15) -0.0062(16) -0.0127(18) C22 0.046(3) 0.053(3) 0.030(2) 0.015(2) -0.006(2) -0.019(3) C23 0.036(3) 0.054(3) 0.046(3) 0.012(2) -0.001(2) -0.019(3) C24 0.041(3) 0.036(2) 0.043(3) 0.011(2) -0.014(2) -0.019(2) S3 0.0298(6) 0.0262(5) 0.0563(8) 0.0011(5) 0.0013(6) -0.0009(5) C25 0.021(2) 0.029(2) 0.040(2) 0.0093(18) -0.0035(19) -0.0066(18) C26 0.018(2) 0.0267(18) 0.0284(19) 0.0054(16) -0.0024(17) -0.0066(17) C27 0.024(2) 0.034(2) 0.0274(19) 0.0075(17) -0.0038(17) -0.0123(18) C28 0.036(3) 0.052(3) 0.027(2) 0.0045(19) -0.0080(19) -0.023(2) C29 0.035(3) 0.066(3) 0.036(2) 0.023(2) -0.017(2) -0.022(2) C30 0.026(2) 0.043(2) 0.053(3) 0.023(2) -0.014(2) -0.013(2) O3 0.0314(16) 0.0303(14) 0.0218(13) 0.0013(11) -0.0033(12) -0.0080(13) C31 0.034(3) 0.051(3) 0.026(2) 0.006(2) -0.003(2) -0.011(2) C32 0.039(3) 0.038(2) 0.0229(19) 0.0025(17) -0.0069(19) -0.013(2) C33 0.043(3) 0.029(2) 0.030(2) 0.0068(17) -0.013(2) -0.015(2) N3 0.040(2) 0.0298(17) 0.0269(17) 0.0061(14) -0.0080(16) -0.0122(17) C34 0.064(3) 0.041(2) 0.030(2) 0.0112(19) -0.013(2) -0.025(3) C35 0.074(4) 0.051(3) 0.041(3) 0.010(2) -0.012(3) -0.041(3) C36 0.057(3) 0.053(3) 0.043(3) 0.004(2) -0.016(2) -0.032(3) S4 0.0286(6) 0.0284(5) 0.0392(6) 0.0027(4) -0.0033(5) -0.0134(5) C37 0.030(2) 0.0209(17) 0.0279(19) 0.0020(15) -0.0023(18) -0.0084(17) C38 0.030(2) 0.0193(16) 0.0233(18) 0.0013(14) -0.0023(17) -0.0065(17) C39 0.028(2) 0.0216(17) 0.031(2) 0.0006(16) -0.0016(18) -0.0064(17) C40 0.040(3) 0.0257(19) 0.040(2) 0.0062(18) -0.015(2) -0.0069(19) C41 0.049(3) 0.032(2) 0.038(2) 0.016(2) -0.008(2) -0.013(2) C42 0.041(3) 0.030(2) 0.035(2) 0.0091(18) -0.001(2) -0.013(2) O4 0.0301(16) 0.0214(12) 0.0202(12) 0.0018(10) -0.0030(12) -0.0075(12) C43 0.044(3) 0.0279(19) 0.0216(18) -0.0032(16) 0.0013(19) -0.013(2) C44 0.026(2) 0.0288(19) 0.0247(18) 0.0031(16) -0.0060(17) -0.0096(18) C45 0.030(2) 0.0295(19) 0.0239(18) 0.0032(16) -0.0032(18) -0.0080(18) N4 0.033(2) 0.0333(18) 0.0256(17) 0.0025(15) -0.0043(16) -0.0042(17) C46 0.041(3) 0.038(2) 0.035(2) 0.012(2) -0.008(2) -0.005(2) C47 0.048(3) 0.030(2) 0.038(2) 0.0050(19) -0.005(2) -0.006(2) C48 0.035(3) 0.029(2) 0.027(2) -0.0031(17) -0.0009(19) -0.0072(19) C49 0.193(12) 0.44(3) 0.318(17) -0.19(2) 0.052(11) -0.17(2) O5 0.193(12) 0.44(3) 0.318(17) -0.19(2) 0.052(11) -0.17(2) O6 0.097(11) 0.165(15) 0.28(2) 0.169(15) 0.081(17) 0.013(12) C51 0.045(3) 0.050(3) 0.052(3) 0.011(2) -0.017(3) -0.025(3) Cl5 0.0709(11) 0.0630(9) 0.0768(11) -0.0159(8) 0.0083(9) -0.0234(9) Cl6 0.0517(8) 0.0626(8) 0.0554(8) 0.0172(7) -0.0191(7) -0.0130(7) Cl7 0.0691(11) 0.0901(12) 0.0484(8) 0.0161(8) -0.0241(8) -0.0100(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 Hg1 Cl1 2.3658(9) . ? Hg1 Cl2 2.3843(10) . ? Hg1 N3 2.395(3) . ? Hg1 N1 2.434(4) . ? Hg2 N4 2.307(4) 2_576 ? Hg2 Cl3 2.3668(12) . ? Hg2 Cl4 2.4502(11) . ? Hg2 N2 2.458(4) . ? S1 C39 1.769(4) . ? S1 C1 1.776(4) . ? C1 C6 1.385(6) . ? C1 C2 1.397(6) . ? C2 O1 1.381(4) . ? C2 C3 1.398(5) . ? C3 C4 1.399(6) . ? C3 S2 1.771(4) . ? C4 C5 1.373(7) . ? C4 H4 0.9500 . ? C5 C6 1.381(7) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? O1 C7 1.435(4) . ? C7 C8 1.502(5) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.383(6) . ? C8 C12 1.385(6) . ? C9 N1 1.335(5) . ? C9 H9 0.9500 . ? N1 C10 1.333(5) . ? C10 C11 1.374(7) . ? C10 H10 0.9500 . ? C11 C12 1.373(6) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? S2 C13 1.767(5) . ? C13 C14 1.392(6) . ? C13 C18 1.397(6) . ? C14 O2 1.386(4) . ? C14 C15 1.398(6) . ? C15 C16 1.402(6) . ? C15 S3 1.764(5) . ? C16 C17 1.372(8) . ? C16 H16 0.9500 . ? C17 C18 1.376(8) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? O2 C19 1.445(5) . ? C19 C20 1.505(6) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 C24 1.373(7) . ? C20 C21 1.395(6) . ? C21 N2 1.338(5) . ? C21 H21 0.9500 . ? N2 C22 1.335(6) . ? C22 C23 1.373(7) . ? C22 H22 0.9500 . ? C23 C24 1.392(7) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? S3 C25 1.760(5) . ? C25 C30 1.396(6) . ? C25 C26 1.417(5) . ? C26 O3 1.373(4) . ? C26 C27 1.393(6) . ? C27 C28 1.399(5) . ? C27 S4 1.764(4) . ? C28 C29 1.381(7) . ? C28 H28 0.9500 . ? C29 C30 1.372(7) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? O3 C31 1.436(5) . ? C31 C32 1.499(6) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 C36 1.375(6) . ? C32 C33 1.392(6) . ? C33 N3 1.334(5) . ? C33 H33 0.9500 . ? N3 C34 1.341(5) . ? C34 C35 1.367(7) . ? C34 H34 0.9500 . ? C35 C36 1.372(7) . ? C35 H35 0.9500 . ? C36 H36 0.9500 . ? S4 C37 1.773(4) . ? C37 C42 1.391(5) . ? C37 C38 1.391(6) . ? C38 O4 1.376(4) . ? C38 C39 1.396(6) . ? C39 C40 1.392(6) . ? C40 C41 1.376(7) . ? C40 H40 0.9500 . ? C41 C42 1.382(7) . ? C41 H41 0.9500 . ? C42 H42 0.9500 . ? O4 C43 1.435(5) . ? C43 C44 1.499(5) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 C45 1.369(6) . ? C44 C48 1.394(6) . ? C45 N4 1.342(5) . ? C45 H45 0.9500 . ? N4 C46 1.336(6) . ? N4 Hg2 2.306(4) 2_576 ? C46 C47 1.380(7) . ? C46 H46 0.9500 . ? C47 C48 1.382(6) . ? C47 H47 0.9500 . ? C48 H48 0.9500 . ? C49 O5 1.545(18) . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C49 H49C 0.9800 . ? O6 O6 1.08(3) 2_676 ? C51 Cl6 1.745(5) . ? C51 Cl5 1.748(6) . ? C51 Cl7 1.757(5) . ? C51 H51 1.0000 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl1 Hg1 Cl2 145.18(4) . . ? Cl1 Hg1 N3 103.67(8) . . ? Cl2 Hg1 N3 106.03(8) . . ? Cl1 Hg1 N1 103.17(8) . . ? Cl2 Hg1 N1 96.57(9) . . ? N3 Hg1 N1 86.18(13) . . ? N4 Hg2 Cl3 127.70(10) 2_576 . ? N4 Hg2 Cl4 97.96(9) 2_576 . ? Cl3 Hg2 Cl4 130.13(5) . . ? N4 Hg2 N2 93.42(13) 2_576 . ? Cl3 Hg2 N2 99.86(9) . . ? Cl4 Hg2 N2 95.67(9) . . ? C39 S1 C1 106.42(19) . . ? C6 C1 C2 120.7(4) . . ? C6 C1 S1 117.5(4) . . ? C2 C1 S1 121.6(3) . . ? O1 C2 C1 119.1(3) . . ? O1 C2 C3 121.5(4) . . ? C1 C2 C3 119.4(4) . . ? C2 C3 C4 119.1(4) . . ? C2 C3 S2 122.6(3) . . ? C4 C3 S2 117.8(3) . . ? C5 C4 C3 120.6(4) . . ? C5 C4 H4 119.7 . . ? C3 C4 H4 119.7 . . ? C4 C5 C6 120.8(4) . . ? C4 C5 H5 119.6 . . ? C6 C5 H5 119.6 . . ? C5 C6 C1 119.4(4) . . ? C5 C6 H6 120.3 . . ? C1 C6 H6 120.3 . . ? C2 O1 C7 112.7(3) . . ? O1 C7 C8 109.0(3) . . ? O1 C7 H7A 109.9 . . ? C8 C7 H7A 109.9 . . ? O1 C7 H7B 109.9 . . ? C8 C7 H7B 109.9 . . ? H7A C7 H7B 108.3 . . ? C9 C8 C12 117.2(4) . . ? C9 C8 C7 121.0(4) . . ? C12 C8 C7 121.8(4) . . ? N1 C9 C8 123.3(4) . . ? N1 C9 H9 118.3 . . ? C8 C9 H9 118.3 . . ? C10 N1 C9 118.5(4) . . ? C10 N1 Hg1 118.6(3) . . ? C9 N1 Hg1 121.8(3) . . ? N1 C10 C11 121.9(4) . . ? N1 C10 H10 119.0 . . ? C11 C10 H10 119.0 . . ? C12 C11 C10 119.3(4) . . ? C12 C11 H11 120.4 . . ? C10 C11 H11 120.4 . . ? C11 C12 C8 119.8(4) . . ? C11 C12 H12 120.1 . . ? C8 C12 H12 120.1 . . ? C13 S2 C3 105.05(18) . . ? C14 C13 C18 119.7(4) . . ? C14 C13 S2 122.2(3) . . ? C18 C13 S2 117.7(4) . . ? O2 C14 C13 119.9(4) . . ? O2 C14 C15 120.6(4) . . ? C13 C14 C15 119.5(4) . . ? C14 C15 C16 119.5(4) . . ? C14 C15 S3 122.4(3) . . ? C16 C15 S3 117.9(4) . . ? C17 C16 C15 120.5(5) . . ? C17 C16 H16 119.7 . . ? C15 C16 H16 119.7 . . ? C16 C17 C18 120.0(4) . . ? C16 C17 H17 120.0 . . ? C18 C17 H17 120.0 . . ? C17 C18 C13 120.6(4) . . ? C17 C18 H18 119.7 . . ? C13 C18 H18 119.7 . . ? C14 O2 C19 109.1(3) . . ? O2 C19 C20 109.9(3) . . ? O2 C19 H19A 109.7 . . ? C20 C19 H19A 109.7 . . ? O2 C19 H19B 109.7 . . ? C20 C19 H19B 109.7 . . ? H19A C19 H19B 108.2 . . ? C24 C20 C21 118.4(4) . . ? C24 C20 C19 120.7(4) . . ? C21 C20 C19 120.9(4) . . ? N2 C21 C20 122.4(4) . . ? N2 C21 H21 118.8 . . ? C20 C21 H21 118.8 . . ? C22 N2 C21 118.4(4) . . ? C22 N2 Hg2 120.7(3) . . ? C21 N2 Hg2 120.6(3) . . ? N2 C22 C23 123.0(4) . . ? N2 C22 H22 118.5 . . ? C23 C22 H22 118.5 . . ? C22 C23 C24 118.5(5) . . ? C22 C23 H23 120.8 . . ? C24 C23 H23 120.8 . . ? C20 C24 C23 119.4(4) . . ? C20 C24 H24 120.3 . . ? C23 C24 H24 120.3 . . ? C25 S3 C15 104.6(2) . . ? C30 C25 C26 119.1(4) . . ? C30 C25 S3 117.3(3) . . ? C26 C25 S3 123.3(3) . . ? O3 C26 C27 118.9(3) . . ? O3 C26 C25 122.0(4) . . ? C27 C26 C25 119.0(4) . . ? C26 C27 C28 120.5(4) . . ? C26 C27 S4 122.5(3) . . ? C28 C27 S4 116.3(3) . . ? C29 C28 C27 119.9(4) . . ? C29 C28 H28 120.0 . . ? C27 C28 H28 120.0 . . ? C30 C29 C28 120.3(4) . . ? C30 C29 H29 119.8 . . ? C28 C29 H29 119.8 . . ? C29 C30 C25 121.1(4) . . ? C29 C30 H30 119.5 . . ? C25 C30 H30 119.5 . . ? C26 O3 C31 116.0(3) . . ? O3 C31 C32 109.2(4) . . ? O3 C31 H31A 109.8 . . ? C32 C31 H31A 109.8 . . ? O3 C31 H31B 109.8 . . ? C32 C31 H31B 109.8 . . ? H31A C31 H31B 108.3 . . ? C36 C32 C33 117.1(4) . . ? C36 C32 C31 121.7(4) . . ? C33 C32 C31 121.1(4) . . ? N3 C33 C32 122.9(4) . . ? N3 C33 H33 118.5 . . ? C32 C33 H33 118.5 . . ? C33 N3 C34 118.3(4) . . ? C33 N3 Hg1 124.1(3) . . ? C34 N3 Hg1 116.6(3) . . ? N3 C34 C35 122.3(4) . . ? N3 C34 H34 118.8 . . ? C35 C34 H34 118.8 . . ? C34 C35 C36 118.8(4) . . ? C34 C35 H35 120.6 . . ? C36 C35 H35 120.6 . . ? C35 C36 C32 120.4(4) . . ? C35 C36 H36 119.8 . . ? C32 C36 H36 119.8 . . ? C27 S4 C37 108.51(18) . . ? C42 C37 C38 120.2(4) . . ? C42 C37 S4 116.2(3) . . ? C38 C37 S4 123.2(3) . . ? O4 C38 C37 120.0(3) . . ? O4 C38 C39 120.3(4) . . ? C37 C38 C39 119.7(3) . . ? C40 C39 C38 119.3(4) . . ? C40 C39 S1 115.9(3) . . ? C38 C39 S1 124.3(3) . . ? C41 C40 C39 120.6(4) . . ? C41 C40 H40 119.7 . . ? C39 C40 H40 119.7 . . ? C40 C41 C42 120.3(4) . . ? C40 C41 H41 119.8 . . ? C42 C41 H41 119.8 . . ? C41 C42 C37 119.8(4) . . ? C41 C42 H42 120.1 . . ? C37 C42 H42 120.1 . . ? C38 O4 C43 113.7(3) . . ? O4 C43 C44 108.4(3) . . ? O4 C43 H43A 110.0 . . ? C44 C43 H43A 110.0 . . ? O4 C43 H43B 110.0 . . ? C44 C43 H43B 110.0 . . ? H43A C43 H43B 108.4 . . ? C45 C44 C48 118.3(4) . . ? C45 C44 C43 119.0(4) . . ? C48 C44 C43 122.7(4) . . ? N4 C45 C44 123.4(4) . . ? N4 C45 H45 118.3 . . ? C44 C45 H45 118.3 . . ? C46 N4 C45 118.1(4) . . ? C46 N4 Hg2 123.7(3) . 2_576 ? C45 N4 Hg2 117.7(3) . 2_576 ? N4 C46 C47 122.3(4) . . ? N4 C46 H46 118.8 . . ? C47 C46 H46 118.8 . . ? C46 C47 C48 119.3(4) . . ? C46 C47 H47 120.4 . . ? C48 C47 H47 120.4 . . ? C47 C48 C44 118.6(4) . . ? C47 C48 H48 120.7 . . ? C44 C48 H48 120.7 . . ? Cl6 C51 Cl5 111.0(3) . . ? Cl6 C51 Cl7 109.2(3) . . ? Cl5 C51 Cl7 109.7(3) . . ? Cl6 C51 H51 109.0 . . ? Cl5 C51 H51 109.0 . . ? Cl7 C51 H51 109.0 . . ? _diffrn_measured_fraction_theta_max 0.972 _diffrn_reflns_theta_full 29.02 _diffrn_measured_fraction_theta_full 0.972 _refine_diff_density_max 1.665 _refine_diff_density_min -1.007 _refine_diff_density_rms 0.115 data_global # Attachment 'web_deposit_cif_file_5_FERLAY_1361985472.4-HgCl2.cif' data_e2318a #TrackingRef 'web_deposit_cif_file_5_FERLAY_1361985472.4-HgCl2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(C48 H36 Cl6 Hg3 N4 O4 S4), 0.27(C2 H2 Cl6), C H Cl3' _chemical_formula_sum 'C49.54 H37.54 Cl10.61 Hg3 N4 O4 S4' _chemical_formula_weight 1859.15 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Hg Hg -2.3894 9.2266 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.4949(3) _cell_length_b 13.5043(4) _cell_length_c 18.1231(5) _cell_angle_alpha 70.1100(10) _cell_angle_beta 83.5310(10) _cell_angle_gamma 72.9180(10) _cell_volume 2968.42(14) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9876 _cell_measurement_theta_min 2.39 _cell_measurement_theta_max 27.83 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.07 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 2.080 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1758.1 _exptl_absorpt_coefficient_mu 8.404 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5909 _exptl_absorpt_correction_T_max 0.6327 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 55007 _diffrn_reflns_av_R_equivalents 0.0377 _diffrn_reflns_av_sigmaI/netI 0.0515 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.67 _diffrn_reflns_theta_max 29.17 _reflns_number_total 15847 _reflns_number_gt 11233 _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^)+(0.0446P)^2^+4.1832P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 15847 _refine_ls_number_parameters 731 _refine_ls_number_restraints 15 _refine_ls_R_factor_all 0.0681 _refine_ls_R_factor_gt 0.0384 _refine_ls_wR_factor_ref 0.0968 _refine_ls_wR_factor_gt 0.0864 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.034 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Hg1 Hg 0.763516(18) 0.074746(18) 0.758845(14) 0.03622(7) Uani 1 1 d . . . Cl1 Cl 0.77672(17) 0.05743(19) 0.89353(10) 0.0703(6) Uani 1 1 d . . . Cl2 Cl 0.78471(14) -0.06193(14) 0.70054(11) 0.0547(4) Uani 1 1 d . . . Hg2 Hg 0.952405(18) 0.215354(18) 0.826382(13) 0.03734(7) Uani 1 1 d . . . Cl3 Cl 0.87883(10) 0.21141(10) 0.69428(8) 0.0307(3) Uani 1 1 d . . . Cl4 Cl 0.82757(15) 0.34555(13) 0.86860(10) 0.0599(5) Uani 1 1 d . . . Hg3 Hg 0.009669(16) 1.382769(16) 0.603247(12) 0.02895(6) Uani 1 1 d . . . Cl5 Cl 0.10987(11) 1.28588(12) 0.75023(8) 0.0352(3) Uani 1 1 d . . . Cl6 Cl 0.11647(10) 1.52082(11) 0.53013(8) 0.0306(3) Uani 1 1 d . . . S1 S 0.27548(12) 0.70162(12) 0.51164(8) 0.0360(3) Uani 1 1 d . . . C1 C 0.2036(4) 0.7059(4) 0.5988(3) 0.0326(13) Uani 1 1 d . . . C2 C 0.2356(4) 0.6265(4) 0.6716(3) 0.0284(12) Uani 1 1 d . . . C3 C 0.1736(4) 0.6276(5) 0.7388(3) 0.0347(13) Uani 1 1 d . . . C4 C 0.0799(5) 0.7057(6) 0.7329(4) 0.0452(16) Uani 1 1 d . . . H4 H 0.0380 0.7071 0.7785 0.054 Uiso 1 1 calc R . . C5 C 0.0464(5) 0.7819(6) 0.6615(5) 0.0524(19) Uani 1 1 d . . . H5 H -0.0194 0.8341 0.6578 0.063 Uiso 1 1 calc R . . C6 C 0.1083(5) 0.7827(5) 0.5947(4) 0.0448(16) Uani 1 1 d . . . H6 H 0.0851 0.8365 0.5458 0.054 Uiso 1 1 calc R . . O1 O 0.3285(3) 0.5490(3) 0.6764(2) 0.0276(8) Uani 1 1 d . . . C7 C 0.3186(4) 0.4493(4) 0.6704(4) 0.0338(13) Uani 1 1 d . . . H7A H 0.2948 0.4622 0.6174 0.041 Uiso 1 1 calc R . . H7B H 0.2669 0.4223 0.7094 0.041 Uiso 1 1 calc R . . C8 C 0.4222(4) 0.3663(4) 0.6854(3) 0.0275(11) Uani 1 1 d . . . C9 C 0.5120(4) 0.3938(5) 0.6896(3) 0.0355(13) Uani 1 1 d . . . H9 H 0.5099 0.4676 0.6819 0.043 Uiso 1 1 calc R . . C10 C 0.6033(5) 0.3138(5) 0.7048(4) 0.0377(14) Uani 1 1 d . . . H10 H 0.6641 0.3335 0.7084 0.045 Uiso 1 1 calc R . . N1 N 0.6117(4) 0.2089(4) 0.7149(3) 0.0334(11) Uani 1 1 d . . . C11 C 0.5242(5) 0.1829(5) 0.7100(4) 0.0425(15) Uani 1 1 d . . . H11 H 0.5287 0.1087 0.7170 0.051 Uiso 1 1 calc R . . C12 C 0.4302(4) 0.2571(5) 0.6953(4) 0.0374(14) Uani 1 1 d . . . H12 H 0.3706 0.2352 0.6919 0.045 Uiso 1 1 calc R . . S2 S 0.20398(14) 0.52277(15) 0.83144(10) 0.0493(4) Uani 1 1 d . . . C13 C 0.3334(5) 0.5122(5) 0.8506(3) 0.0353(13) Uani 1 1 d . . . C14 C 0.3598(4) 0.5971(4) 0.8638(3) 0.0290(12) Uani 1 1 d . . . C15 C 0.4610(4) 0.5836(4) 0.8843(3) 0.0310(12) Uani 1 1 d . . . C16 C 0.5339(5) 0.4847(5) 0.8934(3) 0.0453(16) Uani 1 1 d . . . H16 H 0.6030 0.4753 0.9067 0.054 Uiso 1 1 calc R . . C17 C 0.5070(6) 0.3990(5) 0.8833(3) 0.0503(18) Uani 1 1 d . . . H17 H 0.5573 0.3303 0.8912 0.060 Uiso 1 1 calc R . . C18 C 0.4090(6) 0.4118(5) 0.8620(3) 0.0441(16) Uani 1 1 d . . . H18 H 0.3918 0.3522 0.8550 0.053 Uiso 1 1 calc R . . O2 O 0.2858(3) 0.6965(3) 0.85151(19) 0.0277(8) Uani 1 1 d . . . C19 C 0.2335(4) 0.7111(4) 0.9228(3) 0.0336(13) Uani 1 1 d . . . H19A H 0.2846 0.6969 0.9628 0.040 Uiso 1 1 calc R . . H19B H 0.1897 0.6601 0.9443 0.040 Uiso 1 1 calc R . . C20 C 0.1680(4) 0.8273(4) 0.9012(3) 0.0295(12) Uani 1 1 d . . . C21 C 0.1563(4) 0.8875(4) 0.9513(3) 0.0309(12) Uani 1 1 d . . . H21 H 0.1891 0.8550 1.0009 0.037 Uiso 1 1 calc R . . C22 C 0.0968(4) 0.9948(5) 0.9293(3) 0.0317(12) Uani 1 1 d . . . H22 H 0.0915 1.0360 0.9636 0.038 Uiso 1 1 calc R . . N2 N 0.0464(3) 1.0427(3) 0.8615(3) 0.0284(10) Uani 1 1 d . . . C23 C 0.0566(5) 0.9848(5) 0.8127(3) 0.0359(13) Uani 1 1 d . . . H23 H 0.0213 1.0186 0.7642 0.043 Uiso 1 1 calc R . . C24 C 0.1167(5) 0.8776(5) 0.8305(3) 0.0370(13) Uani 1 1 d . . . H24 H 0.1227 0.8388 0.7945 0.044 Uiso 1 1 calc R . . S3 S 0.49498(12) 0.68586(13) 0.90881(8) 0.0382(3) Uani 1 1 d . . . C25 C 0.4556(4) 0.8050(4) 0.8260(3) 0.0287(12) Uani 1 1 d . . . C26 C 0.4951(4) 0.8078(4) 0.7505(3) 0.0227(10) Uani 1 1 d . . . C27 C 0.4618(4) 0.9036(4) 0.6876(3) 0.0271(11) Uani 1 1 d . . . C28 C 0.3925(4) 0.9961(5) 0.7006(4) 0.0368(13) Uani 1 1 d . . . H28 H 0.3693 1.0608 0.6574 0.044 Uiso 1 1 calc R . . C29 C 0.3577(5) 0.9943(5) 0.7753(4) 0.0429(15) Uani 1 1 d . . . H29 H 0.3124 1.0580 0.7841 0.051 Uiso 1 1 calc R . . C30 C 0.3898(4) 0.8981(5) 0.8377(3) 0.0371(14) Uani 1 1 d . . . H30 H 0.3658 0.8966 0.8893 0.045 Uiso 1 1 calc R . . O3 O 0.5659(3) 0.7182(3) 0.73741(19) 0.0240(7) Uani 1 1 d . . . C31 C 0.6694(4) 0.7056(5) 0.7591(4) 0.0356(13) Uani 1 1 d . . . H31A H 0.6746 0.6788 0.8170 0.043 Uiso 1 1 calc R . . H31B H 0.6850 0.7775 0.7392 0.043 Uiso 1 1 calc R . . C32 C 0.7464(4) 0.6263(4) 0.7257(3) 0.0252(11) Uani 1 1 d . . . C33 C 0.7173(4) 0.5657(4) 0.6890(3) 0.0262(11) Uani 1 1 d . . . H33 H 0.6460 0.5710 0.6859 0.031 Uiso 1 1 calc R . . C34 C 0.7921(4) 0.4968(4) 0.6566(3) 0.0261(11) Uani 1 1 d . . . H34 H 0.7711 0.4566 0.6302 0.031 Uiso 1 1 calc R . . N3 N 0.8928(3) 0.4853(3) 0.6616(2) 0.0258(9) Uani 1 1 d . . . C35 C 0.9217(4) 0.5424(4) 0.6992(3) 0.0271(11) Uani 1 1 d . . . H35 H 0.9936 0.5328 0.7039 0.032 Uiso 1 1 calc R . . C36 C 0.8519(4) 0.6138(4) 0.7308(3) 0.0297(12) Uani 1 1 d . . . H36 H 0.8749 0.6542 0.7560 0.036 Uiso 1 1 calc R . . S4 S 0.51542(12) 0.92088(12) 0.59184(8) 0.0333(3) Uani 1 1 d . . . C37 C 0.5008(4) 0.8131(4) 0.5628(3) 0.0244(11) Uani 1 1 d . . . C38 C 0.4034(4) 0.8016(4) 0.5551(3) 0.0208(10) Uani 1 1 d . . . C39 C 0.3960(4) 0.7191(4) 0.5277(3) 0.0269(11) Uani 1 1 d . . . C40 C 0.4860(5) 0.6515(4) 0.5066(3) 0.0355(13) Uani 1 1 d . . . H40 H 0.4816 0.5942 0.4890 0.043 Uiso 1 1 calc R . . C41 C 0.5821(5) 0.6670(5) 0.5110(3) 0.0384(14) Uani 1 1 d . . . H41 H 0.6430 0.6228 0.4943 0.046 Uiso 1 1 calc R . . C42 C 0.5884(4) 0.7462(5) 0.5396(3) 0.0323(12) Uani 1 1 d . . . H42 H 0.6544 0.7556 0.5436 0.039 Uiso 1 1 calc R . . O4 O 0.3166(3) 0.8739(3) 0.57278(19) 0.0249(8) Uani 1 1 d . . . C43 C 0.2672(4) 0.9597(4) 0.5041(3) 0.0265(11) Uani 1 1 d . . . H43A H 0.2226 0.9328 0.4800 0.032 Uiso 1 1 calc R . . H43B H 0.3204 0.9824 0.4649 0.032 Uiso 1 1 calc R . . C44 C 0.2031(4) 1.0550(4) 0.5282(3) 0.0224(10) Uani 1 1 d . . . C45 C 0.1820(4) 1.0485(4) 0.6055(3) 0.0324(13) Uani 1 1 d . . . H45 H 0.2048 0.9805 0.6459 0.039 Uiso 1 1 calc R . . C46 C 0.1280(4) 1.1403(4) 0.6241(3) 0.0339(13) Uani 1 1 d . . . H46 H 0.1153 1.1348 0.6778 0.041 Uiso 1 1 calc R . . N4 N 0.0922(3) 1.2383(3) 0.5686(2) 0.0249(9) Uani 1 1 d . . . C47 C 0.1101(4) 1.2444(4) 0.4937(3) 0.0296(12) Uani 1 1 d . . . H47 H 0.0838 1.3128 0.4545 0.035 Uiso 1 1 calc R . . C48 C 0.1650(4) 1.1566(4) 0.4705(3) 0.0292(12) Uani 1 1 d . . . H48 H 0.1770 1.1644 0.4164 0.035 Uiso 1 1 calc R . . C49 C 0.3709(11) 0.1100(14) -0.0311(9) 0.110(7) Uani 0.538(3) 1 d PD A 1 H49 H 0.3652 0.0340 -0.0031 0.132 Uiso 0.538(3) 1 calc PR A 1 Cl7 Cl 0.2688(4) 0.1822(4) -0.0962(2) 0.0820(14) Uani 0.538(3) 1 d PD A 1 Cl9 Cl 0.4827(4) 0.1051(4) -0.0819(3) 0.1063(19) Uani 0.538(3) 1 d PD A 1 Cl8 Cl 0.3681(6) 0.1771(7) 0.0378(3) 0.153(3) Uani 0.538(3) 1 d PD A 1 C51 C 0.1040(14) 0.3602(13) 0.0149(9) 0.120(8) Uani 0.538(3) 1 d PD A 1 H51 H 0.1702 0.3369 -0.0134 0.145 Uiso 0.538(3) 1 calc PR A 1 Cl14 Cl 0.1067(6) 0.4609(5) 0.0532(3) 0.120(2) Uani 0.538(3) 1 d PD . 1 Cl13 Cl 0.0006(7) 0.3975(12) -0.0417(5) 0.120(2) Uani 0.538(3) 1 d PD . 1 Cl15 Cl 0.0859(15) 0.2606(12) 0.0918(8) 0.120(2) Uani 0.538(3) 1 d PD A 1 C50 C 0.1887(13) 0.2189(15) 0.0319(8) 0.107(9) Uani 0.462(3) 1 d PD A 2 H50 H 0.2293 0.1407 0.0548 0.128 Uiso 0.462(3) 1 calc PR A 2 Cl10 Cl 0.1616(6) 0.2475(5) -0.0611(3) 0.111(3) Uani 0.462(3) 1 d PD A 2 Cl11 Cl 0.2534(6) 0.3039(8) 0.0396(3) 0.111(3) Uani 0.462(3) 1 d PD A 2 Cl12 Cl 0.0788(7) 0.2433(7) 0.0763(6) 0.111(3) Uani 0.462(3) 1 d PD A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Hg1 0.03300(14) 0.03179(12) 0.04753(14) -0.01917(10) -0.00638(10) -0.00460(10) Cl1 0.0959(16) 0.0935(15) 0.0386(9) -0.0186(9) -0.0059(9) -0.0527(13) Cl2 0.0674(12) 0.0489(10) 0.0611(10) -0.0363(8) 0.0088(9) -0.0173(9) Hg2 0.03766(15) 0.03072(12) 0.04113(13) -0.01707(10) -0.00113(10) 0.00097(10) Cl3 0.0262(7) 0.0267(6) 0.0366(7) -0.0064(5) -0.0036(5) -0.0068(6) Cl4 0.0760(13) 0.0311(8) 0.0469(9) -0.0075(7) 0.0225(8) 0.0085(8) Hg3 0.02528(12) 0.02293(10) 0.03648(11) -0.01282(8) -0.00060(8) 0.00047(9) Cl5 0.0325(8) 0.0372(7) 0.0351(7) -0.0085(6) -0.0071(6) -0.0097(6) Cl6 0.0255(7) 0.0329(7) 0.0349(7) -0.0079(5) -0.0073(5) -0.0114(6) S1 0.0453(9) 0.0332(7) 0.0350(7) -0.0111(6) -0.0123(6) -0.0146(7) C1 0.028(3) 0.028(3) 0.048(3) -0.016(2) -0.007(2) -0.010(3) C2 0.023(3) 0.029(3) 0.042(3) -0.018(2) -0.001(2) -0.012(2) C3 0.032(3) 0.039(3) 0.045(3) -0.020(3) 0.002(3) -0.019(3) C4 0.024(4) 0.059(4) 0.072(5) -0.041(4) 0.004(3) -0.016(3) C5 0.020(3) 0.048(4) 0.106(6) -0.047(4) -0.004(4) -0.006(3) C6 0.028(4) 0.030(3) 0.076(5) -0.013(3) -0.019(3) -0.006(3) O1 0.022(2) 0.0249(19) 0.036(2) -0.0106(15) -0.0039(15) -0.0048(16) C7 0.026(3) 0.032(3) 0.049(3) -0.020(3) -0.009(2) -0.005(3) C8 0.023(3) 0.033(3) 0.027(3) -0.010(2) -0.004(2) -0.007(2) C9 0.031(3) 0.026(3) 0.050(3) -0.010(2) -0.004(3) -0.009(3) C10 0.027(3) 0.034(3) 0.055(4) -0.018(3) 0.001(3) -0.010(3) N1 0.028(3) 0.032(3) 0.042(3) -0.012(2) -0.006(2) -0.009(2) C11 0.041(4) 0.026(3) 0.064(4) -0.017(3) -0.009(3) -0.007(3) C12 0.026(3) 0.035(3) 0.055(4) -0.014(3) -0.010(3) -0.011(3) S2 0.0597(11) 0.0573(11) 0.0447(9) -0.0172(8) 0.0130(8) -0.0405(9) C13 0.051(4) 0.030(3) 0.023(3) -0.003(2) 0.003(2) -0.016(3) C14 0.040(4) 0.025(3) 0.018(2) -0.005(2) 0.005(2) -0.007(2) C15 0.034(3) 0.032(3) 0.019(2) -0.002(2) 0.001(2) -0.003(3) C16 0.039(4) 0.047(4) 0.030(3) -0.005(3) -0.004(3) 0.011(3) C17 0.059(5) 0.040(4) 0.029(3) -0.008(3) -0.003(3) 0.017(3) C18 0.076(5) 0.023(3) 0.031(3) -0.009(2) 0.006(3) -0.011(3) O2 0.032(2) 0.0227(18) 0.0253(18) -0.0071(14) 0.0026(15) -0.0042(16) C19 0.035(3) 0.024(3) 0.030(3) -0.006(2) 0.005(2) 0.003(2) C20 0.032(3) 0.024(3) 0.027(3) -0.004(2) 0.002(2) -0.006(2) C21 0.031(3) 0.029(3) 0.025(3) -0.006(2) 0.000(2) -0.001(2) C22 0.035(3) 0.034(3) 0.027(3) -0.014(2) 0.002(2) -0.009(3) N2 0.027(3) 0.022(2) 0.033(2) -0.0083(18) -0.0007(19) -0.0028(19) C23 0.040(4) 0.028(3) 0.034(3) -0.006(2) -0.012(2) -0.001(3) C24 0.046(4) 0.028(3) 0.037(3) -0.014(2) -0.005(3) -0.004(3) S3 0.0411(9) 0.0519(9) 0.0228(6) -0.0086(6) -0.0020(6) -0.0180(7) C25 0.030(3) 0.035(3) 0.027(3) -0.013(2) 0.002(2) -0.014(3) C26 0.017(3) 0.024(2) 0.030(3) -0.012(2) 0.002(2) -0.006(2) C27 0.030(3) 0.032(3) 0.026(3) -0.013(2) 0.003(2) -0.017(2) C28 0.038(4) 0.025(3) 0.052(4) -0.014(3) 0.000(3) -0.012(3) C29 0.039(4) 0.035(3) 0.065(4) -0.028(3) 0.015(3) -0.016(3) C30 0.032(3) 0.047(4) 0.042(3) -0.026(3) 0.015(3) -0.018(3) O3 0.023(2) 0.0239(18) 0.0278(18) -0.0131(14) 0.0018(14) -0.0050(15) C31 0.024(3) 0.045(3) 0.049(3) -0.032(3) -0.001(2) -0.007(3) C32 0.025(3) 0.024(3) 0.026(2) -0.007(2) -0.003(2) -0.007(2) C33 0.020(3) 0.025(3) 0.033(3) -0.009(2) 0.000(2) -0.006(2) C34 0.025(3) 0.018(2) 0.034(3) -0.007(2) -0.004(2) -0.002(2) N3 0.025(3) 0.020(2) 0.030(2) -0.0076(17) -0.0037(18) -0.0013(18) C35 0.017(3) 0.028(3) 0.035(3) -0.009(2) -0.006(2) -0.003(2) C36 0.028(3) 0.028(3) 0.036(3) -0.013(2) -0.004(2) -0.008(2) S4 0.0466(9) 0.0343(7) 0.0256(6) -0.0076(5) 0.0031(6) -0.0244(7) C37 0.030(3) 0.021(2) 0.022(2) -0.0061(19) 0.000(2) -0.007(2) C38 0.025(3) 0.013(2) 0.018(2) -0.0007(17) -0.0044(19) -0.001(2) C39 0.035(3) 0.023(3) 0.023(2) -0.007(2) -0.005(2) -0.007(2) C40 0.050(4) 0.024(3) 0.029(3) -0.013(2) -0.006(3) 0.002(3) C41 0.032(4) 0.042(3) 0.031(3) -0.015(3) 0.002(2) 0.007(3) C42 0.023(3) 0.040(3) 0.026(3) -0.007(2) -0.001(2) -0.002(3) O4 0.027(2) 0.0190(17) 0.0244(17) -0.0062(14) -0.0020(14) -0.0002(15) C43 0.029(3) 0.022(3) 0.024(2) -0.004(2) -0.002(2) -0.003(2) C44 0.018(3) 0.019(2) 0.029(3) -0.0058(19) -0.0001(19) -0.004(2) C45 0.031(3) 0.019(3) 0.035(3) -0.002(2) 0.004(2) 0.003(2) C46 0.031(3) 0.030(3) 0.028(3) -0.005(2) 0.003(2) 0.004(2) N4 0.021(2) 0.017(2) 0.032(2) -0.0070(17) -0.0021(17) 0.0012(18) C47 0.030(3) 0.023(3) 0.026(3) -0.002(2) -0.003(2) 0.001(2) C48 0.034(3) 0.020(3) 0.028(3) -0.008(2) -0.004(2) 0.002(2) C49 0.151(19) 0.101(15) 0.117(16) -0.051(13) 0.027(14) -0.083(15) Cl7 0.102(3) 0.100(3) 0.073(3) -0.043(2) 0.006(2) -0.057(3) Cl9 0.096(4) 0.082(3) 0.112(4) -0.013(3) 0.029(3) -0.015(3) Cl8 0.185(7) 0.270(9) 0.101(4) -0.106(5) 0.026(4) -0.164(7) C51 0.14(2) 0.112(17) 0.141(19) -0.041(15) 0.040(16) -0.103(16) Cl14 0.199(7) 0.110(4) 0.071(3) -0.032(3) 0.008(3) -0.071(4) Cl13 0.199(7) 0.110(4) 0.071(3) -0.032(3) 0.008(3) -0.071(4) Cl15 0.199(7) 0.110(4) 0.071(3) -0.032(3) 0.008(3) -0.071(4) C50 0.126(19) 0.105(18) 0.095(16) 0.018(13) -0.020(13) -0.093(16) Cl10 0.190(7) 0.103(4) 0.063(3) 0.001(3) -0.039(4) -0.093(5) Cl11 0.190(7) 0.103(4) 0.063(3) 0.001(3) -0.039(4) -0.093(5) Cl12 0.190(7) 0.103(4) 0.063(3) 0.001(3) -0.039(4) -0.093(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Hg1 N1 2.307(5) . ? Hg1 Cl2 2.3567(16) . ? Hg1 Cl1 2.3937(17) . ? Hg1 Cl3 2.6466(13) . ? Hg2 N2 2.211(4) 1_645 ? Hg2 Cl4 2.3237(15) . ? Hg2 Cl5 2.6383(14) 1_645 ? Hg2 Cl3 2.7154(13) . ? Hg3 N4 2.201(4) . ? Hg3 N3 2.205(4) 1_465 ? Hg3 Cl6 2.6030(13) . ? Hg3 Cl6 2.8140(13) 2_586 ? Hg3 Cl5 2.8349(13) . ? Cl5 Hg2 2.6383(14) 1_465 ? Cl6 Hg3 2.8140(13) 2_586 ? S1 C1 1.767(6) . ? S1 C39 1.779(5) . ? C1 C6 1.386(8) . ? C1 C2 1.404(8) . ? C2 O1 1.366(6) . ? C2 C3 1.401(8) . ? C3 C4 1.376(9) . ? C3 S2 1.785(6) . ? C4 C5 1.374(10) . ? C4 H4 0.9500 . ? C5 C6 1.390(10) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? O1 C7 1.432(6) . ? C7 C8 1.497(8) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.384(7) . ? C8 C12 1.396(8) . ? C9 C10 1.361(8) . ? C9 H9 0.9500 . ? C10 N1 1.336(7) . ? C10 H10 0.9500 . ? N1 C11 1.347(7) . ? C11 C12 1.353(8) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? S2 C13 1.775(6) . ? C13 C14 1.394(8) . ? C13 C18 1.402(8) . ? C14 O2 1.381(6) . ? C14 C15 1.400(8) . ? C15 C16 1.377(8) . ? C15 S3 1.775(6) . ? C16 C17 1.383(10) . ? C16 H16 0.9500 . ? C17 C18 1.364(10) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? O2 C19 1.446(6) . ? C19 C20 1.497(7) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 C21 1.380(8) . ? C20 C24 1.384(8) . ? C21 C22 1.378(8) . ? C21 H21 0.9500 . ? C22 N2 1.334(7) . ? C22 H22 0.9500 . ? N2 C23 1.339(7) . ? N2 Hg2 2.211(4) 1_465 ? C23 C24 1.381(8) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? S3 C25 1.777(5) . ? C25 C30 1.377(8) . ? C25 C26 1.405(7) . ? C26 O3 1.377(6) . ? C26 C27 1.394(7) . ? C27 C28 1.398(8) . ? C27 S4 1.769(5) . ? C28 C29 1.377(8) . ? C28 H28 0.9500 . ? C29 C30 1.391(9) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? O3 C31 1.440(6) . ? C31 C32 1.497(7) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 C33 1.372(7) . ? C32 C36 1.394(7) . ? C33 C34 1.385(7) . ? C33 H33 0.9500 . ? C34 N3 1.331(7) . ? C34 H34 0.9500 . ? N3 C35 1.343(7) . ? N3 Hg3 2.205(4) 1_645 ? C35 C36 1.366(7) . ? C35 H35 0.9500 . ? C36 H36 0.9500 . ? S4 C37 1.775(5) . ? C37 C42 1.382(7) . ? C37 C38 1.396(7) . ? C38 O4 1.372(6) . ? C38 C39 1.396(7) . ? C39 C40 1.391(8) . ? C40 C41 1.389(9) . ? C40 H40 0.9500 . ? C41 C42 1.364(8) . ? C41 H41 0.9500 . ? C42 H42 0.9500 . ? O4 C43 1.445(6) . ? C43 C44 1.495(7) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 C45 1.375(7) . ? C44 C48 1.403(7) . ? C45 C46 1.371(8) . ? C45 H45 0.9500 . ? C46 N4 1.351(6) . ? C46 H46 0.9500 . ? N4 C47 1.329(6) . ? C47 C48 1.373(7) . ? C47 H47 0.9500 . ? C48 H48 0.9500 . ? C49 Cl9 1.672(14) . ? C49 Cl7 1.743(15) . ? C49 Cl8 1.766(14) . ? C49 H49 1.0000 . ? C51 Cl15 1.628(15) . ? C51 Cl13 1.676(16) . ? C51 Cl14 1.735(15) . ? C51 H51 1.0000 . ? Cl14 Cl13 1.993(14) 2_565 ? Cl13 Cl14 1.993(14) 2_565 ? C50 Cl12 1.606(16) . ? C50 Cl10 1.654(14) . ? C50 Cl11 1.681(14) . ? C50 H50 1.0000 . ? 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 Hg1 Cl2 108.89(13) . . ? N1 Hg1 Cl1 105.84(13) . . ? Cl2 Hg1 Cl1 129.71(7) . . ? N1 Hg1 Cl3 92.69(12) . . ? Cl2 Hg1 Cl3 114.29(5) . . ? Cl1 Hg1 Cl3 99.00(6) . . ? N2 Hg2 Cl4 144.44(12) 1_645 . ? N2 Hg2 Cl5 92.43(11) 1_645 1_645 ? Cl4 Hg2 Cl5 113.73(6) . 1_645 ? N2 Hg2 Cl3 95.03(12) 1_645 . ? Cl4 Hg2 Cl3 106.73(6) . . ? Cl5 Hg2 Cl3 92.70(4) 1_645 . ? Hg1 Cl3 Hg2 99.41(4) . . ? N4 Hg3 N3 158.67(15) . 1_465 ? N4 Hg3 Cl6 102.13(11) . . ? N3 Hg3 Cl6 99.20(11) 1_465 . ? N4 Hg3 Cl6 93.43(11) . 2_586 ? N3 Hg3 Cl6 88.23(11) 1_465 2_586 ? Cl6 Hg3 Cl6 85.79(4) . 2_586 ? N4 Hg3 Cl5 90.64(11) . . ? N3 Hg3 Cl5 85.40(11) 1_465 . ? Cl6 Hg3 Cl5 100.33(4) . . ? Cl6 Hg3 Cl5 171.79(4) 2_586 . ? Hg2 Cl5 Hg3 94.47(4) 1_465 . ? Hg3 Cl6 Hg3 94.21(4) . 2_586 ? C1 S1 C39 103.9(2) . . ? C6 C1 C2 118.6(6) . . ? C6 C1 S1 119.6(5) . . ? C2 C1 S1 121.5(4) . . ? O1 C2 C3 120.3(5) . . ? O1 C2 C1 119.4(5) . . ? C3 C2 C1 120.3(5) . . ? C4 C3 C2 119.6(6) . . ? C4 C3 S2 117.4(5) . . ? C2 C3 S2 122.7(5) . . ? C5 C4 C3 120.6(6) . . ? C5 C4 H4 119.7 . . ? C3 C4 H4 119.7 . . ? C4 C5 C6 120.2(6) . . ? C4 C5 H5 119.9 . . ? C6 C5 H5 119.9 . . ? C1 C6 C5 120.7(6) . . ? C1 C6 H6 119.7 . . ? C5 C6 H6 119.7 . . ? C2 O1 C7 112.9(4) . . ? O1 C7 C8 108.4(4) . . ? O1 C7 H7A 110.0 . . ? C8 C7 H7A 110.0 . . ? O1 C7 H7B 110.0 . . ? C8 C7 H7B 110.0 . . ? H7A C7 H7B 108.4 . . ? C9 C8 C12 117.9(5) . . ? C9 C8 C7 122.3(5) . . ? C12 C8 C7 119.8(5) . . ? C10 C9 C8 119.1(5) . . ? C10 C9 H9 120.4 . . ? C8 C9 H9 120.4 . . ? N1 C10 C9 123.4(5) . . ? N1 C10 H10 118.3 . . ? C9 C10 H10 118.3 . . ? C10 N1 C11 117.2(5) . . ? C10 N1 Hg1 121.0(4) . . ? C11 N1 Hg1 121.1(4) . . ? N1 C11 C12 123.4(5) . . ? N1 C11 H11 118.3 . . ? C12 C11 H11 118.3 . . ? C11 C12 C8 119.0(5) . . ? C11 C12 H12 120.5 . . ? C8 C12 H12 120.5 . . ? C13 S2 C3 105.7(2) . . ? C14 C13 C18 118.6(6) . . ? C14 C13 S2 121.6(5) . . ? C18 C13 S2 119.3(5) . . ? O2 C14 C13 118.6(5) . . ? O2 C14 C15 120.8(5) . . ? C13 C14 C15 120.4(5) . . ? C16 C15 C14 119.5(6) . . ? C16 C15 S3 118.5(5) . . ? C14 C15 S3 121.7(4) . . ? C15 C16 C17 120.2(6) . . ? C15 C16 H16 119.9 . . ? C17 C16 H16 119.9 . . ? C18 C17 C16 120.8(6) . . ? C18 C17 H17 119.6 . . ? C16 C17 H17 119.6 . . ? C17 C18 C13 120.4(6) . . ? C17 C18 H18 119.8 . . ? C13 C18 H18 119.8 . . ? C14 O2 C19 113.4(4) . . ? O2 C19 C20 106.6(4) . . ? O2 C19 H19A 110.4 . . ? C20 C19 H19A 110.4 . . ? O2 C19 H19B 110.4 . . ? C20 C19 H19B 110.4 . . ? H19A C19 H19B 108.6 . . ? C21 C20 C24 117.8(5) . . ? C21 C20 C19 121.1(5) . . ? C24 C20 C19 121.0(5) . . ? C22 C21 C20 119.8(5) . . ? C22 C21 H21 120.1 . . ? C20 C21 H21 120.1 . . ? N2 C22 C21 122.2(5) . . ? N2 C22 H22 118.9 . . ? C21 C22 H22 118.9 . . ? C22 N2 C23 118.5(5) . . ? C22 N2 Hg2 121.8(4) . 1_465 ? C23 N2 Hg2 119.6(3) . 1_465 ? N2 C23 C24 122.3(5) . . ? N2 C23 H23 118.9 . . ? C24 C23 H23 118.9 . . ? C23 C24 C20 119.4(5) . . ? C23 C24 H24 120.3 . . ? C20 C24 H24 120.3 . . ? C15 S3 C25 103.7(2) . . ? C30 C25 C26 119.9(5) . . ? C30 C25 S3 118.6(4) . . ? C26 C25 S3 121.4(4) . . ? O3 C26 C27 119.6(4) . . ? O3 C26 C25 121.4(4) . . ? C27 C26 C25 119.0(5) . . ? C26 C27 C28 120.1(5) . . ? C26 C27 S4 122.9(4) . . ? C28 C27 S4 116.6(4) . . ? C29 C28 C27 120.6(5) . . ? C29 C28 H28 119.7 . . ? C27 C28 H28 119.7 . . ? C28 C29 C30 119.2(6) . . ? C28 C29 H29 120.4 . . ? C30 C29 H29 120.4 . . ? C25 C30 C29 121.1(5) . . ? C25 C30 H30 119.4 . . ? C29 C30 H30 119.4 . . ? C26 O3 C31 112.6(4) . . ? O3 C31 C32 110.3(4) . . ? O3 C31 H31A 109.6 . . ? C32 C31 H31A 109.6 . . ? O3 C31 H31B 109.6 . . ? C32 C31 H31B 109.6 . . ? H31A C31 H31B 108.1 . . ? C33 C32 C36 118.2(5) . . ? C33 C32 C31 122.6(5) . . ? C36 C32 C31 119.2(5) . . ? C32 C33 C34 119.8(5) . . ? C32 C33 H33 120.1 . . ? C34 C33 H33 120.1 . . ? N3 C34 C33 121.7(5) . . ? N3 C34 H34 119.2 . . ? C33 C34 H34 119.2 . . ? C34 N3 C35 118.7(4) . . ? C34 N3 Hg3 120.8(3) . 1_645 ? C35 N3 Hg3 120.4(3) . 1_645 ? N3 C35 C36 122.7(5) . . ? N3 C35 H35 118.7 . . ? C36 C35 H35 118.7 . . ? C35 C36 C32 118.9(5) . . ? C35 C36 H36 120.6 . . ? C32 C36 H36 120.6 . . ? C27 S4 C37 107.1(2) . . ? C42 C37 C38 119.6(5) . . ? C42 C37 S4 118.2(4) . . ? C38 C37 S4 121.9(4) . . ? O4 C38 C37 118.9(4) . . ? O4 C38 C39 121.5(4) . . ? C37 C38 C39 119.6(5) . . ? C40 C39 C38 119.4(5) . . ? C40 C39 S1 117.5(4) . . ? C38 C39 S1 122.9(4) . . ? C41 C40 C39 120.6(5) . . ? C41 C40 H40 119.7 . . ? C39 C40 H40 119.7 . . ? C42 C41 C40 119.4(5) . . ? C42 C41 H41 120.3 . . ? C40 C41 H41 120.3 . . ? C41 C42 C37 121.4(5) . . ? C41 C42 H42 119.3 . . ? C37 C42 H42 119.3 . . ? C38 O4 C43 113.1(4) . . ? O4 C43 C44 108.8(4) . . ? O4 C43 H43A 109.9 . . ? C44 C43 H43A 109.9 . . ? O4 C43 H43B 109.9 . . ? C44 C43 H43B 109.9 . . ? H43A C43 H43B 108.3 . . ? C45 C44 C48 117.9(5) . . ? C45 C44 C43 122.6(4) . . ? C48 C44 C43 119.5(4) . . ? C46 C45 C44 119.9(5) . . ? C46 C45 H45 120.0 . . ? C44 C45 H45 120.0 . . ? N4 C46 C45 122.1(5) . . ? N4 C46 H46 118.9 . . ? C45 C46 H46 118.9 . . ? C47 N4 C46 118.1(4) . . ? C47 N4 Hg3 121.9(3) . . ? C46 N4 Hg3 120.0(4) . . ? N4 C47 C48 123.1(5) . . ? N4 C47 H47 118.4 . . ? C48 C47 H47 118.4 . . ? C47 C48 C44 118.8(5) . . ? C47 C48 H48 120.6 . . ? C44 C48 H48 120.6 . . ? Cl9 C49 Cl7 108.7(9) . . ? Cl9 C49 Cl8 109.0(8) . . ? Cl7 C49 Cl8 110.0(9) . . ? Cl9 C49 H49 109.7 . . ? Cl7 C49 H49 109.7 . . ? Cl8 C49 H49 109.7 . . ? Cl15 C51 Cl13 105.6(11) . . ? Cl15 C51 Cl14 103.7(11) . . ? Cl13 C51 Cl14 112.2(11) . . ? Cl15 C51 H51 111.6 . . ? Cl13 C51 H51 111.6 . . ? Cl14 C51 H51 111.6 . . ? C51 Cl14 Cl13 127.1(7) . 2_565 ? C51 Cl13 Cl14 120.5(8) . 2_565 ? Cl12 C50 Cl10 105.8(10) . . ? Cl12 C50 Cl11 108.0(11) . . ? Cl10 C50 Cl11 109.9(8) . . ? Cl12 C50 H50 111.0 . . ? Cl10 C50 H50 111.0 . . ? Cl11 C50 H50 111.0 . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 29.17 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 1.774 _refine_diff_density_min -1.435 _refine_diff_density_rms 0.158