Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'M. Hosseini' _publ_contact_author_address ; Laboratoire de Chimie de Coordination Organique Universite Louis Pasteur 4 rue Blaise Pascal 67000 Strasbourg FRANCE ; _publ_contact_author_email HOSSEINI@CHIMIE.U-STRASBG.FR _publ_section_title ; A Stepwise Approach to the Formation of Heterometallic Discrete Complexes and Infinite Architectures ; loop_ _publ_author_name M.Hosseini S.Baudron M.Kurmoo N.Kyritsakas ###Material relevant to compound 1 at 173K ######## data_e273b _database_code_depnum_ccdc_archive 'CCDC 621039' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C18 H14 N4 S2), C H Cl3' _chemical_formula_sum 'C37 H29 Cl3 N8 S4' _chemical_formula_weight 820.27 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' 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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.4143(3) _cell_length_b 13.9395(4) _cell_length_c 14.7757(4) _cell_angle_alpha 98.334(2) _cell_angle_beta 104.786(2) _cell_angle_gamma 110.780(2) _cell_volume 1872.10(9) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 3502 _cell_measurement_theta_min 0.00 _cell_measurement_theta_max 0.00 _exptl_crystal_description rod _exptl_crystal_colour yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.455 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 844 _exptl_absorpt_coefficient_mu 0.509 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; The chloroform molecule shows positionnal disorder The two positions have been refined ; _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 23708 _diffrn_reflns_av_R_equivalents 0.0418 _diffrn_reflns_av_sigmaI/netI 0.0732 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.48 _diffrn_reflns_theta_max 30.11 _reflns_number_total 10851 _reflns_number_gt 6073 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _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^)+(0.1072P)^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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10851 _refine_ls_number_parameters 497 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1189 _refine_ls_R_factor_gt 0.0639 _refine_ls_wR_factor_ref 0.2006 _refine_ls_wR_factor_gt 0.1679 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.032 _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 0.66525(8) 0.49030(5) 0.24391(5) 0.03123(17) Uani 1 1 d . . . S2 S 0.46174(7) 0.60231(5) 0.21579(5) 0.02943(17) Uani 1 1 d . . . C1 C 0.5843(3) 0.56628(18) 0.29441(17) 0.0236(5) Uani 1 1 d . . . C2 C 0.6128(2) 0.59442(17) 0.39245(16) 0.0202(5) Uani 1 1 d . . . C3 C 0.7419(2) 0.60311(17) 0.47065(16) 0.0204(5) Uani 1 1 d . . . C4 C 0.8697(2) 0.59066(18) 0.47155(18) 0.0243(5) Uani 1 1 d . . . H4 H 0.8855 0.5695 0.4142 0.029 Uiso 1 1 calc R . . C5 C 0.9717(3) 0.61102(19) 0.56109(19) 0.0287(6) Uani 1 1 d . . . H5 H 1.0581 0.6039 0.5643 0.034 Uiso 1 1 calc R . . C6 C 0.9461(3) 0.64212(19) 0.64632(18) 0.0292(6) Uani 1 1 d . . . H6 H 1.0159 0.6532 0.7050 0.035 Uiso 1 1 calc R . . C7 C 0.7289(2) 0.63709(17) 0.56125(16) 0.0220(5) Uani 1 1 d . . . C8 C 0.5204(2) 0.62331(17) 0.44348(16) 0.0201(5) Uani 1 1 d . . . C9 C 0.3816(2) 0.62252(18) 0.41207(18) 0.0246(5) Uani 1 1 d . . . H9 H 0.3293 0.6055 0.3465 0.029 Uiso 1 1 calc R . . C10 C 0.3246(3) 0.64835(18) 0.48312(19) 0.0272(5) Uani 1 1 d . . . H10 H 0.2324 0.6485 0.4650 0.033 Uiso 1 1 calc R . . C11 C 0.4039(3) 0.67366(19) 0.58005(19) 0.0294(6) Uani 1 1 d . . . H11 H 0.3628 0.6919 0.6251 0.035 Uiso 1 1 calc R . . C12 C 0.5896(2) 0.64748(17) 0.54473(17) 0.0210(5) Uani 1 1 d . . . C13 C 0.7074(3) 0.5474(2) 0.14680(17) 0.0302(6) Uani 1 1 d . . . H13A H 0.7060 0.4930 0.0971 0.036 Uiso 1 1 calc R . . H13B H 0.6322 0.5702 0.1179 0.036 Uiso 1 1 calc R . . C14 C 0.8553(3) 0.6421(2) 0.18010(19) 0.0371(6) Uani 1 1 d . . . H14A H 0.8665 0.6735 0.1266 0.044 Uiso 1 1 calc R . . H14B H 0.8591 0.6956 0.2319 0.044 Uiso 1 1 calc R . . C15 C 0.9755(3) 0.6104(3) 0.2145(2) 0.0466(8) Uani 1 1 d . . . C16 C 0.3444(3) 0.4788(2) 0.12346(17) 0.0311(6) Uani 1 1 d . . . H16A H 0.2789 0.4923 0.0722 0.037 Uiso 1 1 calc R . . H16B H 0.4033 0.4518 0.0953 0.037 Uiso 1 1 calc R . . C17 C 0.2555(3) 0.3955(2) 0.1651(2) 0.0420(7) Uani 1 1 d . . . H17A H 0.3207 0.3822 0.2167 0.050 Uiso 1 1 calc R . . H17B H 0.1956 0.4219 0.1926 0.050 Uiso 1 1 calc R . . C18 C 0.1619(3) 0.2954(2) 0.0895(2) 0.0392(7) Uani 1 1 d . . . N1 N 0.8263(2) 0.65701(16) 0.64850(15) 0.0275(5) Uani 1 1 d . . . N2 N 0.5373(2) 0.67363(16) 0.61388(15) 0.0270(5) Uani 1 1 d . . . N3 N 1.0667(3) 0.5838(3) 0.2413(3) 0.0754(10) Uani 1 1 d . . . N4 N 0.0904(3) 0.2193(2) 0.0296(2) 0.0465(6) Uani 1 1 d . . . S3 S 0.14003(8) 0.97648(5) 0.23622(5) 0.03071(17) Uani 1 1 d . . . S4 S -0.06847(8) 1.08404(6) 0.20609(5) 0.03234(18) Uani 1 1 d . . . C19 C 0.0594(3) 1.05343(18) 0.28634(17) 0.0243(5) Uani 1 1 d . . . C20 C 0.0931(2) 1.08670(17) 0.38441(16) 0.0207(5) Uani 1 1 d . . . C21 C 0.2249(2) 1.09737(17) 0.46221(16) 0.0203(5) Uani 1 1 d . . . C22 C 0.3519(2) 1.08524(18) 0.46160(17) 0.0234(5) Uani 1 1 d . . . H22 H 0.3667 1.0642 0.4039 0.028 Uiso 1 1 calc R . . C23 C 0.4551(3) 1.10587(18) 0.55069(19) 0.0269(5) Uani 1 1 d . . . H23 H 0.5412 1.0984 0.5532 0.032 Uiso 1 1 calc R . . C24 C 0.4314(3) 1.13773(19) 0.63674(18) 0.0284(5) Uani 1 1 d . . . H24 H 0.5021 1.1493 0.6952 0.034 Uiso 1 1 calc R . . C25 C 0.2135(2) 1.13251(17) 0.55288(16) 0.0206(5) Uani 1 1 d . . . C26 C 0.0037(2) 1.11835(17) 0.43635(17) 0.0209(5) Uani 1 1 d . . . C27 C -0.1341(2) 1.11959(17) 0.40616(18) 0.0235(5) Uani 1 1 d . . . H27 H -0.1878 1.1018 0.3407 0.028 Uiso 1 1 calc R . . C28 C -0.1880(3) 1.14851(18) 0.47766(19) 0.0261(5) Uani 1 1 d . . . H28 H -0.2793 1.1503 0.4602 0.031 Uiso 1 1 calc R . . C29 C -0.1070(3) 1.17456(19) 0.57427(19) 0.0295(6) Uani 1 1 d . . . H29 H -0.1463 1.1943 0.6199 0.035 Uiso 1 1 calc R . . C30 C 0.0755(2) 1.14417(17) 0.53714(17) 0.0217(5) Uani 1 1 d . . . C31 C 0.1870(3) 1.0369(2) 0.14162(17) 0.0313(6) Uani 1 1 d . . . H31A H 0.1882 0.9839 0.0919 0.038 Uiso 1 1 calc R . . H31B H 0.1122 1.0597 0.1120 0.038 Uiso 1 1 calc R . . C32 C 0.3346(3) 1.1323(2) 0.1785(2) 0.0374(7) Uani 1 1 d . . . H32A H 0.3488 1.1653 0.1263 0.045 Uiso 1 1 calc R . . H32B H 0.3356 1.1844 0.2302 0.045 Uiso 1 1 calc R . . C33 C 0.4535(3) 1.1006(3) 0.2145(2) 0.0463(8) Uani 1 1 d . . . C34 C -0.1816(3) 0.9587(2) 0.11495(17) 0.0317(6) Uani 1 1 d . . . H34A H -0.2410 0.9715 0.0598 0.038 Uiso 1 1 calc R . . H34B H -0.1196 0.9299 0.0927 0.038 Uiso 1 1 calc R . . C35 C -0.2803(3) 0.8775(2) 0.1530(2) 0.0448(8) Uani 1 1 d . . . H35A H -0.2218 0.8643 0.2083 0.054 Uiso 1 1 calc R . . H35B H -0.3441 0.9051 0.1743 0.054 Uiso 1 1 calc R . . C36 C -0.3687(3) 0.7768(3) 0.0764(2) 0.0414(7) Uani 1 1 d . . . N5 N 0.3115(2) 1.15251(16) 0.63931(14) 0.0257(4) Uani 1 1 d . . . N6 N 0.0258(2) 1.17326(15) 0.60704(15) 0.0262(5) Uani 1 1 d . . . N7 N 0.5441(3) 1.0742(3) 0.2439(3) 0.0760(10) Uani 1 1 d . . . N8 N -0.4339(3) 0.7012(2) 0.0155(2) 0.0476(7) Uani 1 1 d . . . Cl1 Cl 0.1351(3) 0.6438(3) -0.0800(2) 0.149(2) Uani 0.614(3) 1 d P A 1 Cl2 Cl 0.2701(3) 0.7688(2) 0.11098(16) 0.0914(9) Uani 0.614(3) 1 d P A 1 Cl3 Cl 0.3592(4) 0.8651(3) -0.0308(3) 0.1530(19) Uani 0.614(3) 1 d P A 1 Cl4 Cl 0.1525(11) 0.6398(9) 0.0140(6) 0.308(7) Uani 0.386(3) 1 d P A 2 Cl5 Cl 0.2578(6) 0.7253(4) -0.1165(3) 0.146(2) Uani 0.386(3) 1 d P A 2 Cl6 Cl 0.3432(11) 0.8452(10) 0.0798(9) 0.471(14) Uani 0.386(3) 1 d P A 2 C37 C 0.2294(6) 0.7745(5) -0.0160(5) 0.136(3) Uani 1 1 d . . . H37 H 0.1536 0.8019 -0.0249 0.163 Uiso 1 1 calc R A 1 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 0.0494(4) 0.0381(4) 0.0217(3) 0.0091(3) 0.0171(3) 0.0311(3) S2 0.0411(4) 0.0352(4) 0.0213(3) 0.0085(3) 0.0105(3) 0.0255(3) C1 0.0313(12) 0.0262(12) 0.0206(11) 0.0075(9) 0.0123(10) 0.0168(10) C2 0.0264(11) 0.0174(10) 0.0223(11) 0.0060(9) 0.0108(9) 0.0127(9) C3 0.0277(12) 0.0160(10) 0.0211(11) 0.0052(9) 0.0110(9) 0.0107(9) C4 0.0306(12) 0.0213(11) 0.0263(12) 0.0065(10) 0.0137(10) 0.0134(10) C5 0.0267(12) 0.0283(13) 0.0349(14) 0.0111(11) 0.0113(10) 0.0138(10) C6 0.0287(13) 0.0307(13) 0.0258(13) 0.0077(10) 0.0054(10) 0.0119(11) C7 0.0286(12) 0.0184(11) 0.0208(11) 0.0054(9) 0.0119(9) 0.0087(9) C8 0.0256(11) 0.0150(10) 0.0224(11) 0.0052(9) 0.0118(9) 0.0087(9) C9 0.0252(12) 0.0237(12) 0.0270(12) 0.0051(10) 0.0105(10) 0.0118(10) C10 0.0283(12) 0.0221(12) 0.0388(15) 0.0082(11) 0.0190(11) 0.0134(10) C11 0.0371(14) 0.0255(12) 0.0348(14) 0.0073(11) 0.0250(12) 0.0142(11) C12 0.0286(12) 0.0158(10) 0.0221(11) 0.0052(9) 0.0130(9) 0.0097(9) C13 0.0376(14) 0.0430(15) 0.0183(12) 0.0073(11) 0.0118(10) 0.0244(12) C14 0.0428(16) 0.0426(16) 0.0260(14) 0.0070(12) 0.0091(12) 0.0201(13) C15 0.0383(16) 0.053(2) 0.0403(17) 0.0056(15) 0.0050(13) 0.0181(15) C16 0.0366(14) 0.0433(15) 0.0176(12) 0.0076(11) 0.0097(10) 0.0206(12) C17 0.0531(18) 0.0440(17) 0.0272(14) 0.0082(13) 0.0180(13) 0.0151(14) C18 0.0419(16) 0.0450(18) 0.0353(16) 0.0130(14) 0.0165(13) 0.0194(14) N1 0.0316(11) 0.0267(11) 0.0228(10) 0.0072(9) 0.0094(9) 0.0099(9) N2 0.0348(11) 0.0247(10) 0.0247(11) 0.0048(8) 0.0161(9) 0.0120(9) N3 0.0462(17) 0.089(2) 0.082(3) 0.013(2) 0.0006(16) 0.0355(17) N4 0.0465(15) 0.0468(16) 0.0481(16) 0.0108(13) 0.0185(13) 0.0199(13) S3 0.0456(4) 0.0370(4) 0.0218(3) 0.0068(3) 0.0145(3) 0.0286(3) S4 0.0451(4) 0.0392(4) 0.0223(3) 0.0075(3) 0.0094(3) 0.0294(3) C19 0.0308(12) 0.0247(12) 0.0235(12) 0.0057(10) 0.0103(10) 0.0174(10) C20 0.0268(11) 0.0181(11) 0.0217(11) 0.0053(9) 0.0109(9) 0.0121(9) C21 0.0257(11) 0.0161(10) 0.0200(11) 0.0057(9) 0.0092(9) 0.0082(9) C22 0.0278(12) 0.0226(12) 0.0240(12) 0.0045(9) 0.0125(10) 0.0127(10) C23 0.0258(12) 0.0218(12) 0.0352(14) 0.0083(10) 0.0105(10) 0.0116(10) C24 0.0295(13) 0.0261(13) 0.0268(13) 0.0067(10) 0.0061(10) 0.0108(10) C25 0.0261(11) 0.0164(11) 0.0211(11) 0.0064(9) 0.0109(9) 0.0077(9) C26 0.0266(12) 0.0169(11) 0.0239(12) 0.0057(9) 0.0129(9) 0.0110(9) C27 0.0265(12) 0.0210(11) 0.0267(12) 0.0065(9) 0.0121(10) 0.0116(10) C28 0.0279(12) 0.0208(12) 0.0364(14) 0.0081(10) 0.0171(11) 0.0130(10) C29 0.0354(14) 0.0254(13) 0.0373(15) 0.0088(11) 0.0243(12) 0.0144(11) C30 0.0280(12) 0.0161(11) 0.0222(12) 0.0045(9) 0.0129(9) 0.0074(9) C31 0.0360(14) 0.0449(15) 0.0189(12) 0.0056(11) 0.0106(10) 0.0230(12) C32 0.0415(15) 0.0445(17) 0.0253(14) 0.0057(12) 0.0076(11) 0.0203(13) C33 0.0370(16) 0.055(2) 0.0382(17) 0.0065(15) 0.0058(13) 0.0163(15) C34 0.0356(14) 0.0460(16) 0.0190(12) 0.0075(11) 0.0092(10) 0.0232(12) C35 0.063(2) 0.0464(17) 0.0294(15) 0.0100(13) 0.0217(14) 0.0230(15) C36 0.0509(18) 0.0493(19) 0.0363(16) 0.0187(15) 0.0229(14) 0.0256(15) N5 0.0286(11) 0.0245(10) 0.0218(10) 0.0043(8) 0.0075(8) 0.0097(9) N6 0.0345(11) 0.0219(10) 0.0260(11) 0.0044(8) 0.0173(9) 0.0113(9) N7 0.0420(17) 0.096(3) 0.082(3) 0.016(2) 0.0018(16) 0.0355(17) N8 0.0514(16) 0.0483(16) 0.0458(16) 0.0084(13) 0.0187(13) 0.0231(13) Cl1 0.143(2) 0.132(2) 0.121(2) -0.073(2) -0.059(2) 0.111(2) Cl2 0.0920(15) 0.1096(19) 0.0512(12) 0.0167(13) 0.0026(10) 0.0336(13) Cl3 0.134(3) 0.224(4) 0.245(4) 0.177(4) 0.122(3) 0.149(3) Cl4 0.508(15) 0.574(17) 0.211(8) 0.243(11) 0.216(10) 0.513(15) Cl5 0.139(4) 0.150(5) 0.093(3) 0.019(3) -0.041(3) 0.056(4) Cl6 0.298(11) 0.445(16) 0.423(16) -0.362(14) -0.265(11) 0.326(12) C37 0.097(4) 0.103(4) 0.158(6) -0.026(4) -0.044(4) 0.068(4) _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 1.764(2) . ? S1 C13 1.814(2) . ? S2 C1 1.761(2) . ? S2 C16 1.815(3) . ? C1 C2 1.369(3) . ? C2 C3 1.486(3) . ? C2 C8 1.488(3) . ? C3 C4 1.398(3) . ? C3 C7 1.410(3) . ? C4 C5 1.385(3) . ? C4 H4 0.9300 . ? C5 C6 1.393(4) . ? C5 H5 0.9300 . ? C6 N1 1.343(3) . ? C6 H6 0.9300 . ? C7 N1 1.340(3) . ? C7 C12 1.472(3) . ? C8 C9 1.396(3) . ? C8 C12 1.415(3) . ? C9 C10 1.394(3) . ? C9 H9 0.9300 . ? C10 C11 1.378(4) . ? C10 H10 0.9300 . ? C11 N2 1.352(3) . ? C11 H11 0.9300 . ? C12 N2 1.338(3) . ? C13 C14 1.529(4) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 C15 1.467(4) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 N3 1.139(4) . ? C16 C17 1.523(4) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 C18 1.474(4) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 N4 1.137(4) . ? S3 C19 1.770(2) . ? S3 C31 1.817(3) . ? S4 C19 1.762(2) . ? S4 C34 1.817(3) . ? C19 C20 1.367(3) . ? C20 C26 1.486(3) . ? C20 C21 1.493(3) . ? C21 C22 1.393(3) . ? C21 C25 1.407(3) . ? C22 C23 1.386(3) . ? C22 H22 0.9300 . ? C23 C24 1.396(3) . ? C23 H23 0.9300 . ? C24 N5 1.344(3) . ? C24 H24 0.9300 . ? C25 N5 1.334(3) . ? C25 C30 1.467(3) . ? C26 C27 1.397(3) . ? C26 C30 1.411(3) . ? C27 C28 1.390(3) . ? C27 H27 0.9300 . ? C28 C29 1.378(4) . ? C28 H28 0.9300 . ? C29 N6 1.351(3) . ? C29 H29 0.9300 . ? C30 N6 1.342(3) . ? C31 C32 1.530(4) . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C32 C33 1.460(4) . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C33 N7 1.140(4) . ? C34 C35 1.519(4) . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C35 C36 1.479(4) . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C36 N8 1.135(4) . ? Cl1 C37 1.713(6) . ? Cl2 C37 1.835(8) . ? Cl3 C37 1.578(7) . ? Cl4 C37 1.929(11) . ? Cl5 C37 1.684(9) . ? Cl6 C37 1.513(8) . ? C37 H37 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 S1 C13 104.14(12) . . ? C1 S2 C16 103.04(12) . . ? C2 C1 S2 120.40(18) . . ? C2 C1 S1 120.96(18) . . ? S2 C1 S1 118.62(13) . . ? C1 C2 C3 127.7(2) . . ? C1 C2 C8 127.1(2) . . ? C3 C2 C8 105.22(19) . . ? C4 C3 C7 117.1(2) . . ? C4 C3 C2 133.9(2) . . ? C7 C3 C2 108.9(2) . . ? C5 C4 C3 117.5(2) . . ? C5 C4 H4 121.3 . . ? C3 C4 H4 121.3 . . ? C4 C5 C6 120.6(2) . . ? C4 C5 H5 119.7 . . ? C6 C5 H5 119.7 . . ? N1 C6 C5 123.7(2) . . ? N1 C6 H6 118.1 . . ? C5 C6 H6 118.1 . . ? N1 C7 C3 126.3(2) . . ? N1 C7 C12 125.0(2) . . ? C3 C7 C12 108.7(2) . . ? C9 C8 C12 117.1(2) . . ? C9 C8 C2 133.6(2) . . ? C12 C8 C2 109.1(2) . . ? C10 C9 C8 117.3(2) . . ? C10 C9 H9 121.4 . . ? C8 C9 H9 121.4 . . ? C11 C10 C9 120.6(2) . . ? C11 C10 H10 119.7 . . ? C9 C10 H10 119.7 . . ? N2 C11 C10 124.3(2) . . ? N2 C11 H11 117.9 . . ? C10 C11 H11 117.9 . . ? N2 C12 C8 126.4(2) . . ? N2 C12 C7 125.6(2) . . ? C8 C12 C7 108.1(2) . . ? C14 C13 S1 113.52(17) . . ? C14 C13 H13A 108.9 . . ? S1 C13 H13A 108.9 . . ? C14 C13 H13B 108.9 . . ? S1 C13 H13B 108.9 . . ? H13A C13 H13B 107.7 . . ? C15 C14 C13 111.6(2) . . ? C15 C14 H14A 109.3 . . ? C13 C14 H14A 109.3 . . ? C15 C14 H14B 109.3 . . ? C13 C14 H14B 109.3 . . ? H14A C14 H14B 108.0 . . ? N3 C15 C14 178.5(4) . . ? C17 C16 S2 111.57(17) . . ? C17 C16 H16A 109.3 . . ? S2 C16 H16A 109.3 . . ? C17 C16 H16B 109.3 . . ? S2 C16 H16B 109.3 . . ? H16A C16 H16B 108.0 . . ? C18 C17 C16 110.9(2) . . ? C18 C17 H17A 109.5 . . ? C16 C17 H17A 109.5 . . ? C18 C17 H17B 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 108.0 . . ? N4 C18 C17 178.4(3) . . ? C7 N1 C6 114.8(2) . . ? C12 N2 C11 114.3(2) . . ? C19 S3 C31 103.35(12) . . ? C19 S4 C34 103.41(12) . . ? C20 C19 S4 120.81(19) . . ? C20 C19 S3 121.10(18) . . ? S4 C19 S3 118.08(14) . . ? C19 C20 C26 126.9(2) . . ? C19 C20 C21 127.9(2) . . ? C26 C20 C21 105.21(19) . . ? C22 C21 C25 117.6(2) . . ? C22 C21 C20 133.7(2) . . ? C25 C21 C20 108.7(2) . . ? C23 C22 C21 117.2(2) . . ? C23 C22 H22 121.4 . . ? C21 C22 H22 121.4 . . ? C22 C23 C24 120.7(2) . . ? C22 C23 H23 119.7 . . ? C24 C23 H23 119.7 . . ? N5 C24 C23 123.3(2) . . ? N5 C24 H24 118.3 . . ? C23 C24 H24 118.3 . . ? N5 C25 C21 126.1(2) . . ? N5 C25 C30 125.2(2) . . ? C21 C25 C30 108.8(2) . . ? C27 C26 C30 117.3(2) . . ? C27 C26 C20 133.7(2) . . ? C30 C26 C20 108.9(2) . . ? C28 C27 C26 117.5(2) . . ? C28 C27 H27 121.3 . . ? C26 C27 H27 121.3 . . ? C29 C28 C27 120.5(2) . . ? C29 C28 H28 119.8 . . ? C27 C28 H28 119.8 . . ? N6 C29 C28 124.3(2) . . ? N6 C29 H29 117.9 . . ? C28 C29 H29 117.9 . . ? N6 C30 C26 126.0(2) . . ? N6 C30 C25 125.6(2) . . ? C26 C30 C25 108.5(2) . . ? C32 C31 S3 113.39(17) . . ? C32 C31 H31A 108.9 . . ? S3 C31 H31A 108.9 . . ? C32 C31 H31B 108.9 . . ? S3 C31 H31B 108.9 . . ? H31A C31 H31B 107.7 . . ? C33 C32 C31 111.4(2) . . ? C33 C32 H32A 109.4 . . ? C31 C32 H32A 109.4 . . ? C33 C32 H32B 109.4 . . ? C31 C32 H32B 109.4 . . ? H32A C32 H32B 108.0 . . ? N7 C33 C32 178.1(4) . . ? C35 C34 S4 112.56(18) . . ? C35 C34 H34A 109.1 . . ? S4 C34 H34A 109.1 . . ? C35 C34 H34B 109.1 . . ? S4 C34 H34B 109.1 . . ? H34A C34 H34B 107.8 . . ? C36 C35 C34 110.3(2) . . ? C36 C35 H35A 109.6 . . ? C34 C35 H35A 109.6 . . ? C36 C35 H35B 109.6 . . ? C34 C35 H35B 109.6 . . ? H35A C35 H35B 108.1 . . ? N8 C36 C35 177.5(3) . . ? C25 N5 C24 115.2(2) . . ? C30 N6 C29 114.5(2) . . ? Cl6 C37 Cl3 68.3(8) . . ? Cl6 C37 Cl5 127.4(7) . . ? Cl3 C37 Cl5 71.7(5) . . ? Cl6 C37 Cl1 141.9(8) . . ? Cl3 C37 Cl1 129.5(5) . . ? Cl5 C37 Cl1 58.0(3) . . ? Cl6 C37 Cl2 44.2(8) . . ? Cl3 C37 Cl2 111.5(3) . . ? Cl5 C37 Cl2 138.2(4) . . ? Cl1 C37 Cl2 103.7(4) . . ? Cl6 C37 Cl4 102.4(9) . . ? Cl3 C37 Cl4 149.8(4) . . ? Cl5 C37 Cl4 95.3(4) . . ? Cl1 C37 Cl4 43.6(3) . . ? Cl2 C37 Cl4 60.3(4) . . ? Cl6 C37 H37 104.2 . . ? Cl3 C37 H37 103.0 . . ? Cl5 C37 H37 117.1 . . ? Cl1 C37 H37 103.0 . . ? Cl2 C37 H37 103.0 . . ? Cl4 C37 H37 107.2 . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 30.11 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 1.042 _refine_diff_density_min -0.498 _refine_diff_density_rms 0.093 ###Material relevant to compound 2 at 173K ######## data_e425a _database_code_depnum_ccdc_archive 'CCDC 621040' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C15 H11 N3 S2' _chemical_formula_sum 'C15 H11 N3 S2' _chemical_formula_weight 297.39 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' 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 8.1586(3) _cell_length_b 11.9152(4) _cell_length_c 14.0232(5) _cell_angle_alpha 96.836(2) _cell_angle_beta 93.1670(10) _cell_angle_gamma 96.5950(10) _cell_volume 1341.28(8) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 6060 _cell_measurement_theta_min 2.41 _cell_measurement_theta_max 27.44 _exptl_crystal_description platelet _exptl_crystal_colour purple _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.473 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 616 _exptl_absorpt_coefficient_mu 0.388 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; One of the proprionitrile chain shows disorder over two positions. Therefore, a disorder model has been introduced. As a consequence, hydrogen atoms have not been introduced on one carbon of this chain. However, these hydrogen atoms 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 17345 _diffrn_reflns_av_R_equivalents 0.0341 _diffrn_reflns_av_sigmaI/netI 0.0399 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.12 _diffrn_reflns_theta_max 27.48 _reflns_number_total 6147 _reflns_number_gt 4881 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _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^)+(0.0625P)^2^+1.0702P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6147 _refine_ls_number_parameters 388 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0648 _refine_ls_R_factor_gt 0.0510 _refine_ls_wR_factor_ref 0.1414 _refine_ls_wR_factor_gt 0.1330 _refine_ls_goodness_of_fit_ref 1.074 _refine_ls_restrained_S_all 1.232 _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 1.11926(9) 0.33690(6) 0.18726(5) 0.03556(19) Uani 1 1 d . . . S2 S 1.04598(8) 0.10688(5) 0.25224(5) 0.02974(17) Uani 1 1 d . . . N1 N 0.6591(3) -0.03556(18) -0.09297(15) 0.0283(4) Uani 1 1 d . . . H1 H 0.6188 -0.0326 -0.1505 0.034 Uiso 1 1 calc R . . N2 N 0.7736(3) 0.19004(19) -0.16727(16) 0.0362(5) Uani 1 1 d . . . C1 C 1.0241(3) 0.1924(2) 0.16628(18) 0.0254(5) Uani 1 1 d . . . C2 C 0.9337(3) 0.1615(2) 0.07670(17) 0.0262(5) Uani 1 1 d . . . C3 C 0.8316(3) 0.0531(2) 0.04763(17) 0.0255(5) Uani 1 1 d . . . C4 C 0.7853(3) -0.0434(2) 0.09330(19) 0.0315(6) Uani 1 1 d . . . H4 H 0.8254 -0.0472 0.1561 0.038 Uiso 1 1 calc R . . C5 C 0.6789(4) -0.1328(2) 0.0432(2) 0.0356(6) Uani 1 1 d . . . H5A H 0.6477 -0.1968 0.0731 0.043 Uiso 1 1 calc R . . C6 C 0.6182(3) -0.1287(2) -0.0500(2) 0.0333(6) Uani 1 1 d . . . H6 H 0.5492 -0.1904 -0.0830 0.040 Uiso 1 1 calc R . . C7 C 0.7620(3) 0.0532(2) -0.04731(17) 0.0261(5) Uani 1 1 d . . . C8 C 0.9200(3) 0.2263(2) -0.00535(18) 0.0287(5) Uani 1 1 d . . . C9 C 0.9864(4) 0.3338(2) -0.0257(2) 0.0405(7) Uani 1 1 d . . . H9 H 1.0594 0.3817 0.0187 0.049 Uiso 1 1 calc R . . C10 C 0.9407(5) 0.3672(2) -0.1137(2) 0.0493(8) Uani 1 1 d . . . H10 H 0.9808 0.4393 -0.1277 0.059 Uiso 1 1 calc R . . C11 C 0.8359(5) 0.2946(2) -0.1811(2) 0.0460(8) Uani 1 1 d . . . H11 H 0.8075 0.3204 -0.2392 0.055 Uiso 1 1 calc R . . C12 C 0.8156(3) 0.1592(2) -0.08069(18) 0.0288(5) Uani 1 1 d . . . C13 C 1.2358(3) 0.3480(2) 0.3012(2) 0.0366(6) Uani 1 1 d . . . H13A H 1.2771 0.2758 0.3070 0.044 Uiso 1 1 calc R . . H13B H 1.3308 0.4051 0.3018 0.044 Uiso 1 1 calc R . . C14 C 1.1395(4) 0.3790(2) 0.3889(2) 0.0379(6) Uani 1 1 d . . . H14A H 1.0487 0.3195 0.3914 0.045 Uiso 1 1 calc R . . H14B H 1.2118 0.3827 0.4468 0.045 Uiso 1 1 calc R . . C15 C 1.0736(4) 0.4883(2) 0.3871(2) 0.0372(6) Uani 1 1 d . . . S3A S 0.5305(6) 0.6174(3) 0.3717(3) 0.0721(12) Uani 0.40 1 d PD . . S4A S 0.7358(4) 0.7991(2) 0.29037(18) 0.0451(6) Uani 0.40 1 d PD . . S3B S 0.5244(2) 0.59075(14) 0.40540(12) 0.0336(3) Uani 0.60 1 d PD . . S4B S 0.6633(2) 0.77510(14) 0.29537(12) 0.0386(4) Uani 0.60 1 d PD . . N4 N 0.4895(3) 0.9077(2) 0.72124(16) 0.0340(5) Uani 1 1 d . . . N5 N 0.7396(3) 1.07656(18) 0.63690(15) 0.0282(5) Uani 1 1 d . . . H5 H 0.7222 1.0994 0.6956 0.034 Uiso 1 1 calc R . . N6 N 1.0224(4) 0.5732(2) 0.3847(2) 0.0511(7) Uani 1 1 d . . . N7 N 0.5970(5) 0.3880(3) 0.0659(3) 0.0729(10) Uani 1 1 d . . . C16 C 0.6024(4) 0.7402(3) 0.3939(2) 0.0645(12) Uani 1 1 d D . . C17 C 0.5952(3) 0.8198(2) 0.4762(2) 0.0346(6) Uani 1 1 d . . . C18 C 0.5065(3) 0.8013(2) 0.5611(2) 0.0330(6) Uani 1 1 d . . . C19 C 0.3885(4) 0.7142(3) 0.5841(2) 0.0461(8) Uani 1 1 d . . . H19 H 0.3549 0.6496 0.5404 0.055 Uiso 1 1 calc R . . C20 C 0.3246(4) 0.7276(3) 0.6727(3) 0.0537(9) Uani 1 1 d . . . H20 H 0.2453 0.6718 0.6890 0.064 Uiso 1 1 calc R . . C21 C 0.3769(4) 0.8235(3) 0.7383(2) 0.0454(7) Uani 1 1 d . . . H21 H 0.3308 0.8293 0.7976 0.054 Uiso 1 1 calc R . . C22 C 0.5487(3) 0.8957(2) 0.63291(18) 0.0282(5) Uani 1 1 d . . . C23 C 0.6886(3) 0.9329(2) 0.49782(18) 0.0289(5) Uani 1 1 d . . . C24 C 0.7937(3) 1.0032(3) 0.4478(2) 0.0358(6) Uani 1 1 d . . . H24 H 0.8121 0.9807 0.3839 0.043 Uiso 1 1 calc R . . C25 C 0.8693(4) 1.1061(3) 0.4946(2) 0.0378(6) Uani 1 1 d . . . H25 H 0.9395 1.1524 0.4615 0.045 Uiso 1 1 calc R . . C26 C 0.8431(3) 1.1420(2) 0.5894(2) 0.0345(6) Uani 1 1 d . . . H26 H 0.8970 1.2110 0.6200 0.041 Uiso 1 1 calc R . . C27 C 0.6627(3) 0.9759(2) 0.59423(17) 0.0256(5) Uani 1 1 d . . . C28A C 0.6218(12) 0.5427(8) 0.2685(8) 0.062(2) Uani 0.40 1 d P . . H28C H 0.7404 0.5646 0.2724 0.074 Uiso 0.40 1 calc PR . . H28D H 0.6014 0.4610 0.2694 0.074 Uiso 0.40 1 calc PR . . C28B C 0.6950(6) 0.6456(4) 0.2227(3) 0.0332(9) Uani 0.60 1 d P . . H28A H 0.7745 0.6641 0.1763 0.040 Uiso 0.60 1 calc PR . . H28B H 0.7433 0.5965 0.2639 0.040 Uiso 0.60 1 calc PR . . C29 C 0.5356(5) 0.5776(4) 0.1670(3) 0.0656(11) Uani 1 1 d . . . C30 C 0.5720(5) 0.4699(3) 0.1106(3) 0.0556(9) 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 S1 0.0476(4) 0.0252(3) 0.0313(4) 0.0035(3) -0.0039(3) -0.0029(3) S2 0.0365(3) 0.0280(3) 0.0248(3) 0.0057(2) -0.0022(2) 0.0038(2) N1 0.0339(11) 0.0285(11) 0.0220(10) 0.0010(8) 0.0000(8) 0.0050(9) N2 0.0593(15) 0.0280(11) 0.0231(11) 0.0039(9) -0.0004(10) 0.0139(10) C1 0.0282(12) 0.0230(11) 0.0254(12) 0.0023(9) 0.0059(9) 0.0037(9) C2 0.0357(13) 0.0210(11) 0.0227(12) 0.0032(9) 0.0045(10) 0.0055(9) C3 0.0313(12) 0.0237(12) 0.0218(12) 0.0012(9) 0.0028(9) 0.0064(9) C4 0.0409(14) 0.0287(13) 0.0242(12) 0.0051(10) 0.0001(10) 0.0013(11) C5 0.0456(15) 0.0280(13) 0.0325(14) 0.0084(11) 0.0010(12) -0.0025(11) C6 0.0361(13) 0.0298(13) 0.0321(14) 0.0012(11) 0.0009(11) -0.0003(11) C7 0.0334(12) 0.0242(12) 0.0221(12) 0.0015(9) 0.0046(9) 0.0089(10) C8 0.0422(14) 0.0229(12) 0.0226(12) 0.0022(9) 0.0064(10) 0.0100(10) C9 0.072(2) 0.0227(13) 0.0263(14) 0.0013(10) 0.0061(13) 0.0034(13) C10 0.098(3) 0.0205(13) 0.0300(15) 0.0052(11) 0.0074(16) 0.0069(15) C11 0.089(2) 0.0263(14) 0.0256(14) 0.0071(11) 0.0024(15) 0.0156(14) C12 0.0415(14) 0.0243(12) 0.0220(12) 0.0014(9) 0.0043(10) 0.0107(10) C13 0.0338(13) 0.0315(14) 0.0412(16) -0.0007(12) -0.0093(11) 0.0012(11) C14 0.0510(16) 0.0304(14) 0.0302(14) 0.0035(11) -0.0097(12) 0.0023(12) C15 0.0397(15) 0.0338(15) 0.0357(15) 0.0015(12) -0.0024(12) -0.0004(12) S3A 0.094(2) 0.060(2) 0.049(2) -0.0214(15) 0.0304(19) -0.0283(18) S4A 0.0678(18) 0.0380(14) 0.0255(10) -0.0014(9) 0.0013(12) -0.0036(12) S3B 0.0421(7) 0.0265(7) 0.0289(9) -0.0028(6) 0.0028(6) -0.0029(5) S4B 0.0570(10) 0.0305(8) 0.0237(6) -0.0009(5) 0.0036(7) -0.0100(7) N4 0.0297(11) 0.0418(13) 0.0308(12) 0.0073(10) -0.0012(9) 0.0041(9) N5 0.0359(11) 0.0250(10) 0.0240(10) 0.0029(8) -0.0037(9) 0.0072(9) N6 0.0573(17) 0.0391(15) 0.0575(18) 0.0048(13) 0.0040(14) 0.0100(13) N7 0.084(2) 0.0495(19) 0.080(3) -0.0024(18) 0.003(2) -0.0032(17) C16 0.061(2) 0.072(2) 0.053(2) -0.0344(18) -0.0341(17) 0.0392(19) C17 0.0381(14) 0.0325(14) 0.0311(14) -0.0046(11) -0.0138(11) 0.0118(11) C18 0.0332(13) 0.0279(13) 0.0365(14) 0.0027(11) -0.0133(11) 0.0072(10) C19 0.0447(16) 0.0338(15) 0.055(2) 0.0085(14) -0.0237(14) -0.0062(12) C20 0.0399(16) 0.062(2) 0.056(2) 0.0262(17) -0.0157(15) -0.0178(15) C21 0.0308(14) 0.064(2) 0.0414(17) 0.0167(15) -0.0019(12) -0.0031(13) C22 0.0274(12) 0.0286(13) 0.0288(13) 0.0043(10) -0.0058(10) 0.0072(10) C23 0.0330(13) 0.0324(13) 0.0225(12) 0.0029(10) -0.0062(10) 0.0131(10) C24 0.0399(14) 0.0458(16) 0.0245(13) 0.0078(11) -0.0008(11) 0.0152(12) C25 0.0374(14) 0.0438(16) 0.0360(15) 0.0189(13) 0.0024(12) 0.0063(12) C26 0.0386(14) 0.0270(13) 0.0380(15) 0.0088(11) -0.0067(11) 0.0041(11) C27 0.0303(12) 0.0245(12) 0.0227(12) 0.0027(9) -0.0048(9) 0.0092(9) C28A 0.054(5) 0.045(5) 0.087(7) 0.015(5) 0.001(5) 0.006(4) C28B 0.038(2) 0.033(2) 0.026(2) -0.0063(17) 0.0067(17) -0.0004(18) C29 0.059(2) 0.091(3) 0.0384(19) -0.0214(19) -0.0063(16) 0.009(2) C30 0.066(2) 0.055(2) 0.0418(18) 0.0047(16) 0.0078(16) -0.0107(17) _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 1.789(2) . ? S1 C13 1.797(3) . ? S2 C1 1.684(3) . ? N1 C6 1.342(3) . ? N1 C7 1.345(3) . ? N1 H1 0.8600 . ? N2 C11 1.331(4) . ? N2 C12 1.348(3) . ? C1 C2 1.408(4) . ? C2 C3 1.455(3) . ? C2 C8 1.466(3) . ? C3 C4 1.406(3) . ? C3 C7 1.418(3) . ? C4 C5 1.387(4) . ? C4 H4 0.9300 . ? C5 C6 1.381(4) . ? C5 H5A 0.9300 . ? C6 H6 0.9300 . ? C7 C12 1.429(3) . ? C8 C9 1.401(4) . ? C8 C12 1.422(4) . ? C9 C10 1.386(4) . ? C9 H9 0.9300 . ? C10 C11 1.385(5) . ? C10 H10 0.9300 . ? C11 H11 0.9300 . ? C13 C14 1.527(4) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 C15 1.468(4) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 N6 1.141(4) . ? S3A C16 1.502(5) . ? S3A C28A 1.845(11) . ? S4A C16 2.007(5) . ? S3B C16 1.850(4) . ? S4B C16 1.580(4) . ? S4B C28B 1.798(5) . ? N4 C21 1.333(4) . ? N4 C22 1.352(3) . ? N5 C26 1.341(3) . ? N5 C27 1.343(3) . ? N5 H5 0.8600 . ? N7 C30 1.140(5) . ? C16 C17 1.412(4) . ? C17 C18 1.453(4) . ? C17 C23 1.460(4) . ? C18 C19 1.411(4) . ? C18 C22 1.415(4) . ? C19 C20 1.372(5) . ? C19 H19 0.9300 . ? C20 C21 1.389(5) . ? C20 H20 0.9300 . ? C21 H21 0.9300 . ? C22 C27 1.431(4) . ? C23 C24 1.403(4) . ? C23 C27 1.424(3) . ? C24 C25 1.380(4) . ? C24 H24 0.9300 . ? C25 C26 1.384(4) . ? C25 H25 0.9300 . ? C26 H26 0.9300 . ? C28A C29 1.672(11) . ? C28A H28C 0.9700 . ? C28A H28D 0.9700 . ? C28B C29 1.566(6) . ? C28B H28A 0.9700 . ? C28B H28B 0.9700 . ? C29 C30 1.494(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 S1 C13 104.78(13) . . ? C6 N1 C7 120.9(2) . . ? C6 N1 H1 119.5 . . ? C7 N1 H1 119.5 . . ? C11 N2 C12 115.3(2) . . ? C2 C1 S2 125.80(19) . . ? C2 C1 S1 114.94(18) . . ? S2 C1 S1 119.25(14) . . ? C1 C2 C3 124.9(2) . . ? C1 C2 C8 129.5(2) . . ? C3 C2 C8 105.6(2) . . ? C4 C3 C7 117.0(2) . . ? C4 C3 C2 134.6(2) . . ? C7 C3 C2 108.4(2) . . ? C5 C4 C3 118.9(2) . . ? C5 C4 H4 120.5 . . ? C3 C4 H4 120.5 . . ? C6 C5 C4 121.4(2) . . ? C6 C5 H5A 119.3 . . ? C4 C5 H5A 119.3 . . ? N1 C6 C5 119.8(2) . . ? N1 C6 H6 120.1 . . ? C5 C6 H6 120.1 . . ? N1 C7 C3 121.9(2) . . ? N1 C7 C12 128.5(2) . . ? C3 C7 C12 109.5(2) . . ? C9 C8 C12 115.4(2) . . ? C9 C8 C2 135.3(3) . . ? C12 C8 C2 109.2(2) . . ? C10 C9 C8 118.4(3) . . ? C10 C9 H9 120.8 . . ? C8 C9 H9 120.8 . . ? C11 C10 C9 120.8(3) . . ? C11 C10 H10 119.6 . . ? C9 C10 H10 119.6 . . ? N2 C11 C10 123.5(3) . . ? N2 C11 H11 118.2 . . ? C10 C11 H11 118.2 . . ? N2 C12 C8 126.5(2) . . ? N2 C12 C7 126.2(2) . . ? C8 C12 C7 107.4(2) . . ? C14 C13 S1 114.9(2) . . ? C14 C13 H13A 108.5 . . ? S1 C13 H13A 108.5 . . ? C14 C13 H13B 108.5 . . ? S1 C13 H13B 108.5 . . ? H13A C13 H13B 107.5 . . ? C15 C14 C13 112.5(2) . . ? C15 C14 H14A 109.1 . . ? C13 C14 H14A 109.1 . . ? C15 C14 H14B 109.1 . . ? C13 C14 H14B 109.1 . . ? H14A C14 H14B 107.8 . . ? N6 C15 C14 179.2(3) . . ? C16 S3A C28A 112.6(4) . . ? C16 S4B C28B 106.7(2) . . ? C21 N4 C22 115.3(3) . . ? C26 N5 C27 121.0(2) . . ? C26 N5 H5 119.5 . . ? C27 N5 H5 119.5 . . ? C17 C16 S3A 130.8(3) . . ? C17 C16 S4B 123.1(3) . . ? S3A C16 S4B 105.1(2) . . ? C17 C16 S3B 115.9(3) . . ? S4B C16 S3B 120.9(2) . . ? C17 C16 S4A 114.9(3) . . ? S3A C16 S4A 114.2(2) . . ? S3B C16 S4A 127.97(19) . . ? C16 C17 C18 126.9(3) . . ? C16 C17 C23 127.0(3) . . ? C18 C17 C23 105.8(2) . . ? C19 C18 C22 116.2(3) . . ? C19 C18 C17 134.2(3) . . ? C22 C18 C17 109.6(2) . . ? C20 C19 C18 118.2(3) . . ? C20 C19 H19 120.9 . . ? C18 C19 H19 120.9 . . ? C19 C20 C21 120.7(3) . . ? C19 C20 H20 119.7 . . ? C21 C20 H20 119.7 . . ? N4 C21 C20 123.8(3) . . ? N4 C21 H21 118.1 . . ? C20 C21 H21 118.1 . . ? N4 C22 C18 125.8(2) . . ? N4 C22 C27 126.7(2) . . ? C18 C22 C27 107.5(2) . . ? C24 C23 C27 116.6(2) . . ? C24 C23 C17 135.5(3) . . ? C27 C23 C17 107.9(2) . . ? C25 C24 C23 119.2(3) . . ? C25 C24 H24 120.4 . . ? C23 C24 H24 120.4 . . ? C24 C25 C26 121.6(3) . . ? C24 C25 H25 119.2 . . ? C26 C25 H25 119.2 . . ? N5 C26 C25 119.5(3) . . ? N5 C26 H26 120.2 . . ? C25 C26 H26 120.2 . . ? N5 C27 C23 122.0(2) . . ? N5 C27 C22 128.8(2) . . ? C23 C27 C22 109.2(2) . . ? C29 C28A S3A 108.6(5) . . ? C29 C28A H28C 110.0 . . ? S3A C28A H28C 110.0 . . ? C29 C28A H28D 110.0 . . ? S3A C28A H28D 110.0 . . ? H28C C28A H28D 108.4 . . ? C29 C28B S4B 115.3(3) . . ? C29 C28B H28A 108.5 . . ? S4B C28B H28A 108.5 . . ? C29 C28B H28B 108.5 . . ? S4B C28B H28B 108.5 . . ? H28A C28B H28B 107.5 . . ? C30 C29 C28B 111.8(3) . . ? C30 C29 C28A 91.8(5) . . ? C28B C29 C28A 56.2(4) . . ? N7 C30 C29 178.4(4) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.392 _refine_diff_density_min -0.774 _refine_diff_density_rms 0.064 ###Material relevant to compound 3 at 173K ######## data_e319a _database_code_depnum_ccdc_archive 'CCDC 621041' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H12 N4 Ni S4, 2(C8 H20 N)' _chemical_formula_sum 'C40 H52 N6 Ni S4' _chemical_formula_weight 803.83 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 '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 -P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.9471(4) _cell_length_b 14.3923(5) _cell_length_c 14.6576(9) _cell_angle_alpha 108.838(2) _cell_angle_beta 103.726(2) _cell_angle_gamma 103.735(2) _cell_volume 1995.54(16) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 3588 _cell_measurement_theta_min 2.59 _cell_measurement_theta_max 26.81 _exptl_crystal_description rod _exptl_crystal_colour orange _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.338 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 852 _exptl_absorpt_coefficient_mu 0.732 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8268 _exptl_absorpt_correction_T_max 0.9574 _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 23465 _diffrn_reflns_av_R_equivalents 0.0566 _diffrn_reflns_av_sigmaI/netI 0.0871 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.56 _diffrn_reflns_theta_max 27.50 _reflns_number_total 9118 _reflns_number_gt 5910 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _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^)+(0.0645P)^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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9118 _refine_ls_number_parameters 463 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0918 _refine_ls_R_factor_gt 0.0458 _refine_ls_wR_factor_ref 0.1377 _refine_ls_wR_factor_gt 0.1015 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.040 _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 Ni1 Ni 0.5000 0.0000 0.5000 0.02623(16) Uani 1 2 d S . . S1 S 0.50150(8) -0.13694(6) 0.37674(6) 0.0270(2) Uani 1 1 d . . . S2 S 0.68683(9) -0.01725(6) 0.57444(7) 0.0327(2) Uani 1 1 d . . . N1 N 0.7034(3) -0.4753(2) 0.3607(2) 0.0298(6) Uani 1 1 d . . . N2 N 0.9041(3) -0.3350(2) 0.5747(2) 0.0279(6) Uani 1 1 d . . . C1 C 0.6401(3) -0.1337(2) 0.4676(3) 0.0253(7) Uani 1 1 d . . . C2 C 0.6955(3) -0.2107(2) 0.4618(2) 0.0226(7) Uani 1 1 d . . . C3 C 0.6489(3) -0.3156(2) 0.3812(2) 0.0228(7) Uani 1 1 d . . . C4 C 0.5512(3) -0.3652(2) 0.2828(2) 0.0267(7) Uani 1 1 d . . . H4 H 0.5006 -0.3302 0.2565 0.032 Uiso 1 1 calc R . . C5 C 0.5335(3) -0.4685(3) 0.2265(3) 0.0313(8) Uani 1 1 d . . . H5 H 0.4702 -0.5037 0.1609 0.038 Uiso 1 1 calc R . . C6 C 0.6087(4) -0.5200(3) 0.2667(3) 0.0331(8) Uani 1 1 d . . . H6 H 0.5931 -0.5894 0.2266 0.040 Uiso 1 1 calc R . . C7 C 0.7194(3) -0.3754(2) 0.4142(2) 0.0216(7) Uani 1 1 d . . . C8 C 0.8052(3) -0.2079(2) 0.5433(2) 0.0220(7) Uani 1 1 d . . . C9 C 0.8963(3) -0.1290(3) 0.6356(3) 0.0289(7) Uani 1 1 d . . . H9 H 0.8950 -0.0611 0.6559 0.035 Uiso 1 1 calc R . . C10 C 0.9883(3) -0.1548(3) 0.6958(3) 0.0318(8) Uani 1 1 d . . . H10 H 1.0507 -0.1037 0.7576 0.038 Uiso 1 1 calc R . . C11 C 0.9881(3) -0.2568(3) 0.6647(3) 0.0315(8) Uani 1 1 d . . . H11 H 1.0494 -0.2721 0.7082 0.038 Uiso 1 1 calc R . . C12 C 0.8174(3) -0.3080(2) 0.5168(2) 0.0231(7) Uani 1 1 d . . . Ni2 Ni 0.0000 0.5000 0.0000 0.02325(15) Uani 1 2 d S . . S3 S -0.09928(8) 0.58485(6) 0.09582(6) 0.0265(2) Uani 1 1 d . . . S4 S -0.13853(9) 0.53055(6) -0.11200(6) 0.0283(2) Uani 1 1 d . . . N3 N -0.3020(3) 0.92180(19) 0.1101(2) 0.0268(6) Uani 1 1 d . . . N4 N -0.3268(3) 0.8674(2) -0.1148(2) 0.0272(6) Uani 1 1 d . . . C13 C -0.1676(3) 0.6131(2) -0.0084(2) 0.0227(7) Uani 1 1 d . . . C14 C -0.2201(3) 0.6909(2) -0.0080(2) 0.0213(7) Uani 1 1 d . . . C15 C -0.2346(3) 0.7666(2) 0.0793(2) 0.0224(7) Uani 1 1 d . . . C16 C -0.2173(3) 0.7773(2) 0.1803(2) 0.0278(7) Uani 1 1 d . . . H16 H -0.1901 0.7304 0.2041 0.033 Uiso 1 1 calc R . . C17 C -0.2421(3) 0.8604(3) 0.2436(3) 0.0319(8) Uani 1 1 d . . . H17 H -0.2305 0.8703 0.3114 0.038 Uiso 1 1 calc R . . C18 C -0.2842(3) 0.9287(3) 0.2062(3) 0.0315(8) Uani 1 1 d . . . H18 H -0.3011 0.9829 0.2506 0.038 Uiso 1 1 calc R . . C19 C -0.2773(3) 0.8415(2) 0.0497(2) 0.0222(7) Uani 1 1 d . . . C20 C -0.2596(3) 0.7220(2) -0.0939(2) 0.0214(7) Uani 1 1 d . . . C21 C -0.2682(3) 0.6825(2) -0.1961(2) 0.0258(7) Uani 1 1 d . . . H21 H -0.2510 0.6211 -0.2244 0.031 Uiso 1 1 calc R . . C22 C -0.3030(3) 0.7370(3) -0.2547(3) 0.0300(8) Uani 1 1 d . . . H22 H -0.3085 0.7128 -0.3231 0.036 Uiso 1 1 calc R . . C23 C -0.3294(3) 0.8274(3) -0.2115(3) 0.0310(8) Uani 1 1 d . . . H23 H -0.3505 0.8628 -0.2526 0.037 Uiso 1 1 calc R . . C24 C -0.2922(3) 0.8140(2) -0.0584(2) 0.0229(7) Uani 1 1 d . . . N5 N 0.1991(3) 0.6574(2) 0.4435(2) 0.0259(6) Uani 1 1 d . . . C25 C 0.2579(3) 0.7187(3) 0.5596(2) 0.0309(8) Uani 1 1 d . . . H25A H 0.1886 0.7386 0.5833 0.037 Uiso 1 1 calc R . . H25B H 0.2828 0.6729 0.5908 0.037 Uiso 1 1 calc R . . C26 C 0.3782(4) 0.8159(3) 0.5974(3) 0.0455(10) Uani 1 1 d . . . H26A H 0.4078 0.8491 0.6709 0.068 Uiso 1 1 calc R . . H26B H 0.3545 0.8632 0.5688 0.068 Uiso 1 1 calc R . . H26C H 0.4489 0.7974 0.5766 0.068 Uiso 1 1 calc R . . C27 C 0.3029(3) 0.6203(3) 0.4023(3) 0.0285(7) Uani 1 1 d . . . H27A H 0.2606 0.5782 0.3292 0.034 Uiso 1 1 calc R . . H27B H 0.3739 0.6811 0.4112 0.034 Uiso 1 1 calc R . . C28 C 0.3652(4) 0.5573(3) 0.4517(3) 0.0366(9) Uani 1 1 d . . . H28A H 0.4285 0.5377 0.4209 0.055 Uiso 1 1 calc R . . H28B H 0.2966 0.4956 0.4417 0.055 Uiso 1 1 calc R . . H28C H 0.4102 0.5987 0.5238 0.055 Uiso 1 1 calc R . . C29 C 0.0782(3) 0.5662(2) 0.4242(3) 0.0293(8) Uani 1 1 d . . . H29A H 0.1091 0.5231 0.4567 0.035 Uiso 1 1 calc R . . H29B H 0.0205 0.5937 0.4578 0.035 Uiso 1 1 calc R . . C30 C -0.0048(4) 0.4969(3) 0.3130(3) 0.0391(9) Uani 1 1 d . . . H30A H -0.0779 0.4421 0.3095 0.059 Uiso 1 1 calc R . . H30B H 0.0501 0.4670 0.2788 0.059 Uiso 1 1 calc R . . H30C H -0.0391 0.5378 0.2801 0.059 Uiso 1 1 calc R . . C31 C 0.1608(3) 0.7258(3) 0.3890(3) 0.0284(8) Uani 1 1 d . . . H31A H 0.2408 0.7835 0.4053 0.034 Uiso 1 1 calc R . . H31B H 0.1290 0.6850 0.3156 0.034 Uiso 1 1 calc R . . C32 C 0.0552(4) 0.7701(3) 0.4153(3) 0.0428(10) Uani 1 1 d . . . H32A H 0.0379 0.8118 0.3775 0.064 Uiso 1 1 calc R . . H32B H 0.0865 0.8127 0.4875 0.064 Uiso 1 1 calc R . . H32C H -0.0257 0.7139 0.3977 0.064 Uiso 1 1 calc R . . N6 N 0.2534(3) 0.81241(19) 0.0135(2) 0.0267(6) Uani 1 1 d . . . C33 C 0.2583(3) 0.7023(2) -0.0144(3) 0.0343(8) Uani 1 1 d . . . H33A H 0.1919 0.6634 0.0055 0.041 Uiso 1 1 calc R . . H33B H 0.2327 0.6687 -0.0884 0.041 Uiso 1 1 calc R . . C34 C 0.3913(4) 0.6942(3) 0.0331(3) 0.0540(12) Uani 1 1 d . . . H34A H 0.3842 0.6221 0.0107 0.081 Uiso 1 1 calc R . . H34B H 0.4167 0.7249 0.1065 0.081 Uiso 1 1 calc R . . H34C H 0.4578 0.7307 0.0125 0.081 Uiso 1 1 calc R . . C35 C 0.2862(4) 0.8674(3) 0.1283(3) 0.0390(9) Uani 1 1 d . . . H35A H 0.3766 0.8731 0.1630 0.047 Uiso 1 1 calc R . . H35B H 0.2842 0.9377 0.1436 0.047 Uiso 1 1 calc R . . C36 C 0.1929(4) 0.8138(3) 0.1713(3) 0.0555(12) Uani 1 1 d . . . H36A H 0.2205 0.8529 0.2440 0.083 Uiso 1 1 calc R . . H36B H 0.1954 0.7446 0.1580 0.083 Uiso 1 1 calc R . . H36C H 0.1034 0.8098 0.1393 0.083 Uiso 1 1 calc R . . C37 C 0.1119(3) 0.7999(2) -0.0450(3) 0.0296(8) Uani 1 1 d . . . H37A H 0.0500 0.7519 -0.0295 0.036 Uiso 1 1 calc R . . H37B H 0.0968 0.7680 -0.1178 0.036 Uiso 1 1 calc R . . C38 C 0.0787(4) 0.8997(3) -0.0230(3) 0.0405(9) Uani 1 1 d . . . H38A H -0.0123 0.8838 -0.0636 0.061 Uiso 1 1 calc R . . H38B H 0.1374 0.9474 -0.0400 0.061 Uiso 1 1 calc R . . H38C H 0.0901 0.9311 0.0484 0.061 Uiso 1 1 calc R . . C39 C 0.3565(3) 0.8799(2) -0.0136(3) 0.0301(8) Uani 1 1 d . . . H39A H 0.3494 0.9490 0.0062 0.036 Uiso 1 1 calc R . . H39B H 0.4450 0.8872 0.0270 0.036 Uiso 1 1 calc R . . C40 C 0.3447(4) 0.8396(3) -0.1253(3) 0.0402(9) Uani 1 1 d . . . H40A H 0.4136 0.8871 -0.1348 0.060 Uiso 1 1 calc R . . H40B H 0.2587 0.8341 -0.1665 0.060 Uiso 1 1 calc R . . H40C H 0.3544 0.7721 -0.1456 0.060 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 Ni1 0.0277(3) 0.0198(3) 0.0335(4) 0.0113(3) 0.0100(3) 0.0116(3) S1 0.0277(5) 0.0252(4) 0.0306(5) 0.0123(4) 0.0085(4) 0.0129(4) S2 0.0323(5) 0.0211(4) 0.0361(5) 0.0041(4) 0.0042(4) 0.0117(4) N1 0.0321(17) 0.0250(15) 0.0334(17) 0.0097(13) 0.0125(14) 0.0129(13) N2 0.0281(16) 0.0320(15) 0.0285(16) 0.0145(13) 0.0099(13) 0.0148(13) C1 0.0249(18) 0.0201(16) 0.0309(19) 0.0111(14) 0.0106(15) 0.0055(14) C2 0.0229(17) 0.0175(15) 0.0244(17) 0.0069(13) 0.0078(14) 0.0039(14) C3 0.0218(17) 0.0252(17) 0.0249(18) 0.0120(14) 0.0116(14) 0.0075(14) C4 0.0272(18) 0.0269(17) 0.0278(19) 0.0126(15) 0.0096(15) 0.0099(15) C5 0.0295(19) 0.0326(19) 0.0264(19) 0.0087(16) 0.0069(15) 0.0082(16) C6 0.038(2) 0.0204(17) 0.033(2) 0.0012(15) 0.0116(17) 0.0103(16) C7 0.0217(17) 0.0208(16) 0.0256(17) 0.0110(14) 0.0103(14) 0.0088(14) C8 0.0206(17) 0.0221(16) 0.0246(17) 0.0105(14) 0.0085(14) 0.0071(14) C9 0.0273(19) 0.0258(17) 0.034(2) 0.0135(16) 0.0100(16) 0.0089(15) C10 0.0271(19) 0.0334(19) 0.0255(19) 0.0085(16) 0.0033(15) 0.0047(16) C11 0.0270(19) 0.039(2) 0.034(2) 0.0190(17) 0.0098(16) 0.0154(17) C12 0.0231(17) 0.0258(17) 0.0260(18) 0.0139(14) 0.0117(14) 0.0097(14) Ni2 0.0237(3) 0.0186(3) 0.0275(3) 0.0089(3) 0.0061(3) 0.0103(3) S3 0.0313(5) 0.0252(4) 0.0270(5) 0.0124(4) 0.0088(4) 0.0150(4) S4 0.0322(5) 0.0278(4) 0.0254(5) 0.0080(4) 0.0071(4) 0.0179(4) N3 0.0277(16) 0.0229(14) 0.0316(16) 0.0093(13) 0.0121(13) 0.0119(12) N4 0.0256(15) 0.0271(15) 0.0328(17) 0.0153(13) 0.0088(13) 0.0123(13) C13 0.0179(16) 0.0199(16) 0.0286(18) 0.0096(14) 0.0067(14) 0.0052(13) C14 0.0200(16) 0.0214(16) 0.0221(17) 0.0087(13) 0.0073(13) 0.0062(13) C15 0.0173(16) 0.0213(16) 0.0303(18) 0.0116(14) 0.0080(14) 0.0080(14) C16 0.0323(19) 0.0302(18) 0.0287(19) 0.0157(15) 0.0144(16) 0.0146(16) C17 0.037(2) 0.0331(19) 0.0285(19) 0.0119(16) 0.0163(17) 0.0125(17) C18 0.035(2) 0.0277(18) 0.034(2) 0.0088(16) 0.0178(17) 0.0149(16) C19 0.0163(16) 0.0205(16) 0.0292(18) 0.0094(14) 0.0086(14) 0.0053(13) C20 0.0143(15) 0.0198(15) 0.0293(18) 0.0099(14) 0.0070(13) 0.0049(13) C21 0.0242(18) 0.0241(16) 0.0286(18) 0.0105(14) 0.0073(15) 0.0097(14) C22 0.0295(19) 0.0355(19) 0.0240(18) 0.0136(16) 0.0073(15) 0.0089(16) C23 0.0286(19) 0.0345(19) 0.035(2) 0.0216(17) 0.0080(16) 0.0121(16) C24 0.0154(16) 0.0217(16) 0.0292(18) 0.0103(14) 0.0054(14) 0.0045(13) N5 0.0267(15) 0.0303(15) 0.0310(16) 0.0185(13) 0.0167(13) 0.0119(13) C25 0.036(2) 0.0358(19) 0.0242(19) 0.0131(16) 0.0131(16) 0.0140(17) C26 0.047(3) 0.047(2) 0.032(2) 0.0124(19) 0.0097(19) 0.006(2) C27 0.0289(19) 0.0333(19) 0.0302(19) 0.0161(16) 0.0165(16) 0.0112(16) C28 0.033(2) 0.040(2) 0.049(2) 0.0236(19) 0.0212(18) 0.0174(18) C29 0.0311(19) 0.0263(17) 0.040(2) 0.0190(16) 0.0195(17) 0.0104(15) C30 0.033(2) 0.035(2) 0.045(2) 0.0144(18) 0.0155(18) 0.0038(17) C31 0.0313(19) 0.0318(18) 0.0317(19) 0.0222(16) 0.0136(16) 0.0112(16) C32 0.039(2) 0.044(2) 0.060(3) 0.033(2) 0.020(2) 0.0193(19) N6 0.0201(14) 0.0216(14) 0.0284(16) 0.0087(12) -0.0008(12) 0.0008(12) C33 0.031(2) 0.0217(17) 0.042(2) 0.0118(16) 0.0049(17) 0.0042(16) C34 0.041(2) 0.031(2) 0.081(3) 0.025(2) 0.002(2) 0.0115(19) C35 0.039(2) 0.0280(19) 0.029(2) 0.0066(16) -0.0034(17) -0.0012(17) C36 0.070(3) 0.049(3) 0.027(2) 0.008(2) 0.013(2) -0.001(2) C37 0.0193(17) 0.0309(18) 0.0304(19) 0.0108(16) 0.0027(15) 0.0023(15) C38 0.027(2) 0.037(2) 0.052(2) 0.0157(19) 0.0068(18) 0.0105(17) C39 0.0203(17) 0.0222(17) 0.044(2) 0.0153(16) 0.0046(16) 0.0034(14) C40 0.031(2) 0.045(2) 0.047(2) 0.021(2) 0.0162(18) 0.0113(18) _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 Ni1 S2 2.1892(9) . ? Ni1 S2 2.1892(9) 2_656 ? Ni1 S1 2.2088(8) . ? Ni1 S1 2.2088(8) 2_656 ? S1 C1 1.745(3) . ? S2 C1 1.744(3) . ? N1 C7 1.341(4) . ? N1 C6 1.349(4) . ? N2 C12 1.333(4) . ? N2 C11 1.351(4) . ? C1 C2 1.373(4) . ? C2 C3 1.460(4) . ? C2 C8 1.461(4) . ? C3 C4 1.406(4) . ? C3 C7 1.406(4) . ? C4 C5 1.388(4) . ? C4 H4 0.9300 . ? C5 C6 1.384(5) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C7 C12 1.467(4) . ? C8 C9 1.394(4) . ? C8 C12 1.414(4) . ? C9 C10 1.379(4) . ? C9 H9 0.9300 . ? C10 C11 1.388(4) . ? C10 H10 0.9300 . ? C11 H11 0.9300 . ? Ni2 S4 2.1885(8) 2_565 ? Ni2 S4 2.1885(8) . ? Ni2 S3 2.2118(8) 2_565 ? Ni2 S3 2.2119(8) . ? S3 C13 1.749(3) . ? S4 C13 1.750(3) . ? N3 C19 1.339(4) . ? N3 C18 1.342(4) . ? N4 C23 1.337(4) . ? N4 C24 1.349(4) . ? C13 C14 1.374(4) . ? C14 C15 1.459(4) . ? C14 C20 1.473(4) . ? C15 C16 1.397(4) . ? C15 C19 1.419(4) . ? C16 C17 1.386(4) . ? C16 H16 0.9300 . ? C17 C18 1.387(4) . ? C17 H17 0.9300 . ? C18 H18 0.9300 . ? C19 C24 1.461(4) . ? C20 C21 1.391(4) . ? C20 C24 1.421(4) . ? C21 C22 1.385(4) . ? C21 H21 0.9300 . ? C22 C23 1.382(4) . ? C22 H22 0.9300 . ? C23 H23 0.9300 . ? N5 C29 1.520(4) . ? N5 C31 1.526(4) . ? N5 C25 1.527(4) . ? N5 C27 1.532(4) . ? C25 C26 1.509(5) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 C28 1.515(4) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 C30 1.514(5) . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C31 C32 1.515(5) . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? N6 C37 1.518(4) . ? N6 C35 1.518(4) . ? N6 C33 1.521(4) . ? N6 C39 1.522(4) . ? C33 C34 1.507(5) . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C35 C36 1.510(5) . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? C37 C38 1.518(4) . ? C37 H37A 0.9700 . ? C37 H37B 0.9700 . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? C39 C40 1.512(5) . ? C39 H39A 0.9700 . ? C39 H39B 0.9700 . ? C40 H40A 0.9600 . ? C40 H40B 0.9600 . ? C40 H40C 0.9600 . ? 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 S2 Ni1 S2 180.0 . 2_656 ? S2 Ni1 S1 78.89(3) . . ? S2 Ni1 S1 101.11(3) 2_656 . ? S2 Ni1 S1 101.11(3) . 2_656 ? S2 Ni1 S1 78.89(3) 2_656 2_656 ? S1 Ni1 S1 180.0 . 2_656 ? C1 S1 Ni1 86.37(11) . . ? C1 S2 Ni1 87.03(11) . . ? C7 N1 C6 114.6(3) . . ? C12 N2 C11 115.0(3) . . ? C2 C1 S2 125.7(3) . . ? C2 C1 S1 127.7(3) . . ? S2 C1 S1 106.43(16) . . ? C1 C2 C3 128.3(3) . . ? C1 C2 C8 125.8(3) . . ? C3 C2 C8 105.5(2) . . ? C4 C3 C7 117.1(3) . . ? C4 C3 C2 133.3(3) . . ? C7 C3 C2 109.6(3) . . ? C5 C4 C3 117.1(3) . . ? C5 C4 H4 121.4 . . ? C3 C4 H4 121.4 . . ? C6 C5 C4 120.9(3) . . ? C6 C5 H5 119.5 . . ? C4 C5 H5 119.5 . . ? N1 C6 C5 123.8(3) . . ? N1 C6 H6 118.1 . . ? C5 C6 H6 118.1 . . ? N1 C7 C3 126.5(3) . . ? N1 C7 C12 125.7(3) . . ? C3 C7 C12 107.8(3) . . ? C9 C8 C12 117.2(3) . . ? C9 C8 C2 133.5(3) . . ? C12 C8 C2 109.3(3) . . ? C10 C9 C8 117.9(3) . . ? C10 C9 H9 121.0 . . ? C8 C9 H9 121.0 . . ? C9 C10 C11 120.2(3) . . ? C9 C10 H10 119.9 . . ? C11 C10 H10 119.9 . . ? N2 C11 C10 123.8(3) . . ? N2 C11 H11 118.1 . . ? C10 C11 H11 118.1 . . ? N2 C12 C8 125.7(3) . . ? N2 C12 C7 126.6(3) . . ? C8 C12 C7 107.7(3) . . ? S4 Ni2 S4 180.0 2_565 . ? S4 Ni2 S3 78.53(3) 2_565 2_565 ? S4 Ni2 S3 101.47(3) . 2_565 ? S4 Ni2 S3 101.47(3) 2_565 . ? S4 Ni2 S3 78.53(3) . . ? S3 Ni2 S3 180.00(4) 2_565 . ? C13 S3 Ni2 86.43(10) . . ? C13 S4 Ni2 87.14(10) . . ? C19 N3 C18 114.9(3) . . ? C23 N4 C24 114.9(3) . . ? C14 C13 S3 127.9(2) . . ? C14 C13 S4 126.3(2) . . ? S3 C13 S4 105.46(15) . . ? C13 C14 C15 127.4(3) . . ? C13 C14 C20 126.5(3) . . ? C15 C14 C20 105.8(2) . . ? C16 C15 C19 117.1(3) . . ? C16 C15 C14 133.5(3) . . ? C19 C15 C14 109.4(3) . . ? C17 C16 C15 117.7(3) . . ? C17 C16 H16 121.2 . . ? C15 C16 H16 121.2 . . ? C16 C17 C18 120.2(3) . . ? C16 C17 H17 119.9 . . ? C18 C17 H17 119.9 . . ? N3 C18 C17 124.3(3) . . ? N3 C18 H18 117.9 . . ? C17 C18 H18 117.9 . . ? N3 C19 C15 125.7(3) . . ? N3 C19 C24 126.3(3) . . ? C15 C19 C24 107.9(3) . . ? C21 C20 C24 117.0(3) . . ? C21 C20 C14 134.1(3) . . ? C24 C20 C14 108.8(3) . . ? C22 C21 C20 118.1(3) . . ? C22 C21 H21 120.9 . . ? C20 C21 H21 120.9 . . ? C23 C22 C21 120.0(3) . . ? C23 C22 H22 120.0 . . ? C21 C22 H22 120.0 . . ? N4 C23 C22 124.6(3) . . ? N4 C23 H23 117.7 . . ? C22 C23 H23 117.7 . . ? N4 C24 C20 125.3(3) . . ? N4 C24 C19 126.6(3) . . ? C20 C24 C19 108.0(3) . . ? C29 N5 C31 111.8(2) . . ? C29 N5 C25 105.9(2) . . ? C31 N5 C25 111.3(2) . . ? C29 N5 C27 111.7(2) . . ? C31 N5 C27 105.6(2) . . ? C25 N5 C27 110.7(3) . . ? C26 C25 N5 115.5(3) . . ? C26 C25 H25A 108.4 . . ? N5 C25 H25A 108.4 . . ? C26 C25 H25B 108.4 . . ? N5 C25 H25B 108.4 . . ? H25A C25 H25B 107.5 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C28 C27 N5 115.6(3) . . ? C28 C27 H27A 108.4 . . ? N5 C27 H27A 108.4 . . ? C28 C27 H27B 108.4 . . ? N5 C27 H27B 108.4 . . ? H27A C27 H27B 107.4 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C30 C29 N5 116.3(3) . . ? C30 C29 H29A 108.2 . . ? N5 C29 H29A 108.2 . . ? C30 C29 H29B 108.2 . . ? N5 C29 H29B 108.2 . . ? H29A C29 H29B 107.4 . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C32 C31 N5 115.6(3) . . ? C32 C31 H31A 108.4 . . ? N5 C31 H31A 108.4 . . ? C32 C31 H31B 108.4 . . ? N5 C31 H31B 108.4 . . ? H31A C31 H31B 107.4 . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C37 N6 C35 111.1(3) . . ? C37 N6 C33 105.8(2) . . ? C35 N6 C33 110.8(3) . . ? C37 N6 C39 111.5(2) . . ? C35 N6 C39 105.9(2) . . ? C33 N6 C39 111.9(3) . . ? C34 C33 N6 115.8(3) . . ? C34 C33 H33A 108.3 . . ? N6 C33 H33A 108.3 . . ? C34 C33 H33B 108.3 . . ? N6 C33 H33B 108.3 . . ? H33A C33 H33B 107.4 . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C36 C35 N6 114.5(3) . . ? C36 C35 H35A 108.6 . . ? N6 C35 H35A 108.6 . . ? C36 C35 H35B 108.6 . . ? N6 C35 H35B 108.6 . . ? H35A C35 H35B 107.6 . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? N6 C37 C38 115.8(3) . . ? N6 C37 H37A 108.3 . . ? C38 C37 H37A 108.3 . . ? N6 C37 H37B 108.3 . . ? C38 C37 H37B 108.3 . . ? H37A C37 H37B 107.4 . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C40 C39 N6 115.6(3) . . ? C40 C39 H39A 108.4 . . ? N6 C39 H39A 108.4 . . ? C40 C39 H39B 108.4 . . ? N6 C39 H39B 108.4 . . ? H39A C39 H39B 107.4 . . ? C39 C40 H40A 109.5 . . ? C39 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C39 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.406 _refine_diff_density_min -0.465 _refine_diff_density_rms 0.115 ###Material relevant to compound 4 at 173K ######## data_e503b _database_code_depnum_ccdc_archive 'CCDC 621042' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H12 N4 Pd S4, 2(C8 H20 N)' _chemical_formula_sum 'C40 H52 N6 Pd S4' _chemical_formula_weight 851.52 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_h-m 'P2(1)/n ' _symmetry_space_group_name_hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.4747(6) _cell_length_b 17.9376(15) _cell_length_c 11.8826(9) _cell_angle_alpha 90.00 _cell_angle_beta 96.283(3) _cell_angle_gamma 90.00 _cell_volume 2007.4(3) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 1706 _cell_measurement_theta_min 2.85 _cell_measurement_theta_max 21.55 _exptl_crystal_description platelet _exptl_crystal_colour yellow _exptl_crystal_size_max 0.11 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.409 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 888 _exptl_absorpt_coefficient_mu 0.707 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9263 _exptl_absorpt_correction_T_max 0.9791 _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 16071 _diffrn_reflns_av_R_equivalents 0.0728 _diffrn_reflns_av_sigmaI/netI 0.0781 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.06 _diffrn_reflns_theta_max 27.44 _reflns_number_total 4419 _reflns_number_gt 3052 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _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^)+(0.0718P)^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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4419 _refine_ls_number_parameters 232 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0819 _refine_ls_R_factor_gt 0.0450 _refine_ls_wR_factor_ref 0.1338 _refine_ls_wR_factor_gt 0.1036 _refine_ls_goodness_of_fit_ref 1.006 _refine_ls_restrained_S_all 1.006 _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 C1 C -0.2122(4) 0.0313(2) -0.1859(3) 0.0206(8) Uani 1 1 d . . . C2 C -0.3134(4) 0.0456(2) -0.2750(3) 0.0183(8) Uani 1 1 d . . . C3 C -0.4634(4) 0.0629(2) -0.2681(3) 0.0198(8) Uani 1 1 d . . . C4 C -0.5483(4) 0.0632(2) -0.1795(3) 0.0248(9) Uani 1 1 d . . . H4 H -0.5128 0.0479 -0.1071 0.030 Uiso 1 1 calc R . . C5 C -0.6875(4) 0.0871(2) -0.2031(3) 0.0290(10) Uani 1 1 d . . . H5 H -0.7475 0.0878 -0.1462 0.035 Uiso 1 1 calc R . . C6 C -0.7371(4) 0.1098(3) -0.3118(3) 0.0308(10) Uani 1 1 d . . . H6 H -0.8306 0.1261 -0.3248 0.037 Uiso 1 1 calc R . . C7 C -0.5265(4) 0.0854(2) -0.3754(3) 0.0200(8) Uani 1 1 d . . . C8 C -0.2910(4) 0.0563(2) -0.3946(3) 0.0193(8) Uani 1 1 d . . . C9 C -0.1736(4) 0.0495(2) -0.4548(3) 0.0266(9) Uani 1 1 d . . . H9 H -0.0858 0.0345 -0.4194 0.032 Uiso 1 1 calc R . . C10 C -0.1925(5) 0.0658(2) -0.5691(4) 0.0317(10) Uani 1 1 d . . . H10 H -0.1162 0.0617 -0.6118 0.038 Uiso 1 1 calc R . . C11 C -0.3231(5) 0.0879(2) -0.6205(3) 0.0301(10) Uani 1 1 d . . . H11 H -0.3322 0.0974 -0.6978 0.036 Uiso 1 1 calc R . . C12 C -0.4192(4) 0.0801(2) -0.4549(3) 0.0206(8) Uani 1 1 d . . . N3 N 0.2247(4) 0.2143(2) 0.2541(3) 0.0378(10) Uani 1 1 d . . . C13 C 0.2985(6) 0.1589(3) 0.1853(4) 0.0504(14) Uani 1 1 d . . . H13A H 0.2337 0.1182 0.1637 0.060 Uiso 1 1 calc R . . H13B H 0.3794 0.1383 0.2323 0.060 Uiso 1 1 calc R . . C14 C 0.3499(9) 0.1921(4) 0.0782(5) 0.098(3) Uani 1 1 d . . . H14A H 0.3962 0.1541 0.0387 0.147 Uiso 1 1 calc R . . H14B H 0.4156 0.2318 0.0988 0.147 Uiso 1 1 calc R . . H14C H 0.2702 0.2112 0.0300 0.147 Uiso 1 1 calc R . . C15 C 0.3176(6) 0.2811(3) 0.2859(4) 0.0527(15) Uani 1 1 d . . . H15A H 0.2684 0.3132 0.3345 0.063 Uiso 1 1 calc R . . H15B H 0.3293 0.3089 0.2175 0.063 Uiso 1 1 calc R . . C16 C 0.4632(6) 0.2641(3) 0.3456(5) 0.0705(19) Uani 1 1 d . . . H16A H 0.5141 0.3098 0.3617 0.106 Uiso 1 1 calc R . . H16B H 0.5144 0.2333 0.2978 0.106 Uiso 1 1 calc R . . H16C H 0.4536 0.2383 0.4151 0.106 Uiso 1 1 calc R . . C17 C 0.0910(6) 0.2446(3) 0.1888(4) 0.0556(16) Uani 1 1 d . . . H17A H 0.0529 0.2832 0.2341 0.067 Uiso 1 1 calc R . . H17B H 0.1167 0.2681 0.1204 0.067 Uiso 1 1 calc R . . C18 C -0.0254(7) 0.1887(3) 0.1557(5) 0.073(2) Uani 1 1 d . . . H18A H -0.1047 0.2135 0.1144 0.110 Uiso 1 1 calc R . . H18B H -0.0551 0.1663 0.2226 0.110 Uiso 1 1 calc R . . H18C H 0.0095 0.1508 0.1089 0.110 Uiso 1 1 calc R . . C19 C 0.1896(5) 0.1716(3) 0.3569(4) 0.0416(12) Uani 1 1 d . . . H19A H 0.1364 0.1274 0.3314 0.050 Uiso 1 1 calc R . . H19B H 0.2777 0.1551 0.3987 0.050 Uiso 1 1 calc R . . C20 C 0.1058(6) 0.2138(4) 0.4363(4) 0.0686(19) Uani 1 1 d . . . H20A H 0.0886 0.1822 0.4987 0.103 Uiso 1 1 calc R . . H20B H 0.0167 0.2291 0.3968 0.103 Uiso 1 1 calc R . . H20C H 0.1584 0.2569 0.4643 0.103 Uiso 1 1 calc R . . N1 N -0.6595(3) 0.1100(2) -0.3991(3) 0.0254(8) Uani 1 1 d . . . N2 N -0.4382(4) 0.09649(19) -0.5647(3) 0.0252(8) Uani 1 1 d . . . S1 S -0.23967(11) 0.02676(6) -0.04296(8) 0.0248(2) Uani 1 1 d . . . S2 S -0.03210(11) 0.01640(6) -0.19520(8) 0.0252(3) Uani 1 1 d . . . Pd1 Pd 0.0000 0.0000 0.0000 0.02140(14) 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 C1 0.022(2) 0.0223(19) 0.018(2) 0.0014(15) 0.0040(16) -0.0020(16) C2 0.019(2) 0.023(2) 0.0134(18) 0.0011(14) 0.0020(15) 0.0011(15) C3 0.018(2) 0.023(2) 0.0187(19) 0.0002(15) 0.0015(15) -0.0005(16) C4 0.022(2) 0.038(2) 0.0148(19) 0.0037(16) 0.0020(16) -0.0033(18) C5 0.020(2) 0.045(3) 0.023(2) 0.0019(19) 0.0052(17) -0.0015(19) C6 0.011(2) 0.052(3) 0.030(2) 0.004(2) 0.0021(17) 0.0052(19) C7 0.020(2) 0.022(2) 0.0175(19) 0.0003(15) 0.0001(15) -0.0031(16) C8 0.024(2) 0.0190(19) 0.0144(18) -0.0007(14) 0.0006(15) -0.0006(16) C9 0.027(2) 0.031(2) 0.023(2) 0.0015(17) 0.0086(18) 0.0045(18) C10 0.031(2) 0.038(3) 0.029(2) 0.0007(19) 0.0147(19) 0.003(2) C11 0.040(3) 0.035(2) 0.015(2) 0.0028(17) 0.0053(19) 0.003(2) C12 0.024(2) 0.0209(19) 0.0172(19) -0.0033(15) 0.0016(15) -0.0027(16) N3 0.064(3) 0.024(2) 0.024(2) 0.0018(15) 0.0007(18) 0.0066(19) C13 0.079(4) 0.034(3) 0.043(3) -0.008(2) 0.026(3) -0.009(3) C14 0.158(8) 0.089(5) 0.060(4) -0.021(4) 0.069(5) -0.038(5) C15 0.093(5) 0.024(3) 0.038(3) -0.002(2) -0.009(3) 0.003(3) C16 0.083(5) 0.035(3) 0.088(5) 0.001(3) -0.016(4) -0.013(3) C17 0.089(4) 0.034(3) 0.038(3) 0.007(2) -0.021(3) 0.017(3) C18 0.089(5) 0.056(4) 0.065(4) 0.007(3) -0.034(4) 0.016(4) C19 0.047(3) 0.049(3) 0.029(3) 0.012(2) 0.005(2) 0.016(2) C20 0.064(4) 0.108(6) 0.035(3) -0.001(3) 0.006(3) 0.025(4) N1 0.0182(18) 0.036(2) 0.0215(18) 0.0027(15) 0.0002(14) 0.0012(15) N2 0.029(2) 0.0292(19) 0.0171(17) 0.0024(14) 0.0009(14) 0.0006(15) S1 0.0190(5) 0.0398(6) 0.0155(5) 0.0022(4) 0.0010(4) 0.0040(4) S2 0.0184(5) 0.0382(7) 0.0189(5) 0.0007(4) 0.0010(4) 0.0033(4) Pd1 0.0170(2) 0.0304(2) 0.0164(2) 0.00073(19) -0.00020(15) 0.0025(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.372(5) . ? C1 S2 1.743(4) . ? C1 S1 1.749(4) . ? C2 C3 1.465(5) . ? C2 C8 1.472(5) . ? C3 C4 1.393(5) . ? C3 C7 1.407(5) . ? C4 C5 1.386(6) . ? C4 H4 0.9300 . ? C5 C6 1.387(5) . ? C5 H5 0.9300 . ? C6 N1 1.335(5) . ? C6 H6 0.9300 . ? C7 N1 1.336(5) . ? C7 C12 1.466(5) . ? C8 C9 1.392(5) . ? C8 C12 1.407(5) . ? C9 C10 1.382(5) . ? C9 H9 0.9300 . ? C10 C11 1.377(6) . ? C10 H10 0.9300 . ? C11 N2 1.345(5) . ? C11 H11 0.9300 . ? C12 N2 1.330(5) . ? N3 C13 1.507(6) . ? N3 C19 1.509(5) . ? N3 C15 1.511(6) . ? N3 C17 1.513(6) . ? C13 C14 1.533(7) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 C16 1.511(8) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 C18 1.511(8) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 C20 1.503(7) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? S1 Pd1 2.3225(10) . ? S2 Pd1 2.3247(10) . ? Pd1 S1 2.3225(10) 3 ? Pd1 S2 2.3247(10) 3 ? 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 C2 C1 S2 125.9(3) . . ? C2 C1 S1 126.3(3) . . ? S2 C1 S1 107.8(2) . . ? C1 C2 C3 126.6(3) . . ? C1 C2 C8 127.3(4) . . ? C3 C2 C8 105.6(3) . . ? C4 C3 C7 117.4(3) . . ? C4 C3 C2 133.4(3) . . ? C7 C3 C2 109.2(3) . . ? C5 C4 C3 117.6(3) . . ? C5 C4 H4 121.2 . . ? C3 C4 H4 121.2 . . ? C4 C5 C6 119.8(4) . . ? C4 C5 H5 120.1 . . ? C6 C5 H5 120.1 . . ? N1 C6 C5 124.4(4) . . ? N1 C6 H6 117.8 . . ? C5 C6 H6 117.8 . . ? N1 C7 C3 125.7(4) . . ? N1 C7 C12 126.2(3) . . ? C3 C7 C12 108.0(3) . . ? C9 C8 C12 117.3(3) . . ? C9 C8 C2 133.8(3) . . ? C12 C8 C2 108.9(3) . . ? C10 C9 C8 117.5(4) . . ? C10 C9 H9 121.2 . . ? C8 C9 H9 121.2 . . ? C11 C10 C9 120.7(4) . . ? C11 C10 H10 119.7 . . ? C9 C10 H10 119.7 . . ? N2 C11 C10 123.5(4) . . ? N2 C11 H11 118.2 . . ? C10 C11 H11 118.2 . . ? N2 C12 C8 125.7(4) . . ? N2 C12 C7 126.1(3) . . ? C8 C12 C7 108.2(3) . . ? C13 N3 C19 105.1(4) . . ? C13 N3 C15 111.5(4) . . ? C19 N3 C15 112.0(4) . . ? C13 N3 C17 111.8(4) . . ? C19 N3 C17 110.6(4) . . ? C15 N3 C17 106.0(4) . . ? N3 C13 C14 113.7(5) . . ? N3 C13 H13A 108.8 . . ? C14 C13 H13A 108.8 . . ? N3 C13 H13B 108.8 . . ? C14 C13 H13B 108.8 . . ? H13A C13 H13B 107.7 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N3 C15 C16 115.7(4) . . ? N3 C15 H15A 108.3 . . ? C16 C15 H15A 108.3 . . ? N3 C15 H15B 108.3 . . ? C16 C15 H15B 108.3 . . ? H15A C15 H15B 107.4 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C18 C17 N3 116.2(4) . . ? C18 C17 H17A 108.2 . . ? N3 C17 H17A 108.2 . . ? C18 C17 H17B 108.2 . . ? N3 C17 H17B 108.2 . . ? H17A C17 H17B 107.4 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C20 C19 N3 115.6(4) . . ? C20 C19 H19A 108.4 . . ? N3 C19 H19A 108.4 . . ? C20 C19 H19B 108.4 . . ? N3 C19 H19B 108.4 . . ? H19A C19 H19B 107.5 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C6 N1 C7 115.0(3) . . ? C12 N2 C11 115.3(3) . . ? C1 S1 Pd1 88.71(13) . . ? C1 S2 Pd1 88.77(13) . . ? S1 Pd1 S1 180.00(5) . 3 ? S1 Pd1 S2 105.28(4) . 3 ? S1 Pd1 S2 74.72(4) 3 3 ? S1 Pd1 S2 74.72(4) . . ? S1 Pd1 S2 105.28(4) 3 . ? S2 Pd1 S2 180.00(5) 3 . ? _diffrn_measured_fraction_theta_max 0.96 _diffrn_reflns_theta_full 27.44 _diffrn_measured_fraction_theta_full 0.955 _refine_diff_density_max 0.593 _refine_diff_density_min -0.779 _refine_diff_density_rms 0.172 ###Material relevant to compound 5 at 173K ######## data_e509b _database_code_depnum_ccdc_archive 'CCDC 621043' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H12 N4 S4 Zn, 2(C8 H20 N)' _chemical_formula_sum 'C40 H52 N6 S4 Zn' _chemical_formula_weight 810.49 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'Pbca ' _symmetry_space_group_name_Hall '-P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 17.2827(7) _cell_length_b 18.2012(5) _cell_length_c 25.7071(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 8086.6(5) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 3625 _cell_measurement_theta_min 2.24 _cell_measurement_theta_max 19.72 _exptl_crystal_description rod _exptl_crystal_colour orange _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.331 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3424 _exptl_absorpt_coefficient_mu 0.851 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7844 _exptl_absorpt_correction_T_max 0.9507 _exptl_absorpt_process_details sadabs _exptl_special_details ; one of the tetraethylammonium cations is disordered over two positions. This disorder has been refined accordingly. Note however that the H atoms have not been introduced on the corresponding carbons although they are taken into account in the formula of the title compound ; _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 44220 _diffrn_reflns_av_R_equivalents 0.0886 _diffrn_reflns_av_sigmaI/netI 0.0903 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 1.58 _diffrn_reflns_theta_max 27.46 _reflns_number_total 9260 _reflns_number_gt 4758 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _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^)+(0.1385P)^2^+3.5659P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9260 _refine_ls_number_parameters 455 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1560 _refine_ls_R_factor_gt 0.0779 _refine_ls_wR_factor_ref 0.2609 _refine_ls_wR_factor_gt 0.2127 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.046 _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 C1 C 0.8093(3) 0.1389(3) 0.4913(2) 0.0408(12) Uani 1 1 d . . . C2 C 0.7703(3) 0.1023(3) 0.4516(2) 0.0417(13) Uani 1 1 d . . . C3 C 0.8049(3) 0.0665(3) 0.4066(2) 0.0439(13) Uani 1 1 d . . . C4 C 0.8782(4) 0.0650(4) 0.3850(2) 0.0571(16) Uani 1 1 d . . . H4 H 0.9183 0.0918 0.3999 0.069 Uiso 1 1 calc R . . C5 C 0.8912(4) 0.0228(4) 0.3407(3) 0.076(2) Uani 1 1 d . . . H5 H 0.9398 0.0221 0.3251 0.091 Uiso 1 1 calc R . . C6 C 0.8316(6) -0.0177(5) 0.3203(3) 0.087(3) Uani 1 1 d . . . H6 H 0.8424 -0.0462 0.2912 0.104 Uiso 1 1 calc R . . C7 C 0.7480(4) 0.0218(3) 0.3822(2) 0.0468(14) Uani 1 1 d . . . C8 C 0.6890(3) 0.0819(3) 0.4502(2) 0.0436(13) Uani 1 1 d . . . C9 C 0.6246(4) 0.1016(4) 0.4803(2) 0.0528(15) Uani 1 1 d . . . H9 H 0.6289 0.1351 0.5074 0.063 Uiso 1 1 calc R . . C10 C 0.5550(4) 0.0696(4) 0.4682(3) 0.067(2) Uani 1 1 d . . . H10 H 0.5113 0.0819 0.4874 0.081 Uiso 1 1 calc R . . C11 C 0.5487(5) 0.0200(5) 0.4285(3) 0.075(2) Uani 1 1 d . . . H11 H 0.5003 -0.0005 0.4221 0.090 Uiso 1 1 calc R . . C12 C 0.6756(4) 0.0317(3) 0.4091(2) 0.0496(15) Uani 1 1 d . . . C13 C 0.9789(3) 0.2323(3) 0.6682(2) 0.0398(12) Uani 1 1 d . . . C14 C 1.0144(3) 0.2536(3) 0.71350(19) 0.0364(12) Uani 1 1 d . . . C15 C 1.0326(3) 0.2086(3) 0.7592(2) 0.0399(12) Uani 1 1 d . . . C16 C 1.0253(3) 0.1338(3) 0.7709(2) 0.0487(14) Uani 1 1 d . . . H16 H 1.0046 0.1010 0.7469 0.058 Uiso 1 1 calc R . . C17 C 1.0496(4) 0.1104(4) 0.8191(3) 0.0598(18) Uani 1 1 d . . . H17 H 1.0459 0.0609 0.8276 0.072 Uiso 1 1 calc R . . C18 C 1.0795(4) 0.1592(4) 0.8551(2) 0.0638(19) Uani 1 1 d . . . H18 H 1.0954 0.1408 0.8871 0.077 Uiso 1 1 calc R . . C19 C 1.0632(3) 0.2542(3) 0.7987(2) 0.0421(13) Uani 1 1 d . . . C20 C 1.0399(3) 0.3287(3) 0.7272(2) 0.0367(12) Uani 1 1 d . . . C21 C 1.0460(3) 0.3943(3) 0.6996(2) 0.0457(13) Uani 1 1 d . . . H21 H 1.0280 0.3977 0.6656 0.055 Uiso 1 1 calc R . . C22 C 1.0790(3) 0.4538(3) 0.7238(2) 0.0493(14) Uani 1 1 d . . . H22 H 1.0853 0.4978 0.7058 0.059 Uiso 1 1 calc R . . C23 C 1.1029(4) 0.4483(3) 0.7750(2) 0.0559(16) Uani 1 1 d . . . H23 H 1.1227 0.4901 0.7909 0.067 Uiso 1 1 calc R . . C24 C 1.0685(3) 0.3289(3) 0.7784(2) 0.0398(12) Uani 1 1 d . . . C25 C 0.2584(4) 0.0780(4) 0.4927(3) 0.0741(16) Uani 1 1 d . . . H25A H 0.2805 0.0299 0.4857 0.089 Uiso 1 1 calc R . . H25B H 0.2353 0.0762 0.5270 0.089 Uiso 1 1 calc R . . C26 C 0.3234(4) 0.1333(5) 0.4938(3) 0.090(3) Uani 1 1 d . . . H26A H 0.3604 0.1195 0.5199 0.135 Uiso 1 1 calc R . . H26B H 0.3030 0.1810 0.5017 0.135 Uiso 1 1 calc R . . H26C H 0.3484 0.1346 0.4604 0.135 Uiso 1 1 calc R . . C27 C 0.2294(4) 0.0981(4) 0.3994(3) 0.0741(16) Uani 1 1 d . . . H27A H 0.1873 0.1056 0.3751 0.089 Uiso 1 1 calc R . . H27B H 0.2620 0.1414 0.3982 0.089 Uiso 1 1 calc R . . C28 C 0.2752(6) 0.0343(7) 0.3821(4) 0.135(4) Uani 1 1 d . . . H28A H 0.2936 0.0427 0.3474 0.203 Uiso 1 1 calc R . . H28B H 0.2433 -0.0089 0.3827 0.203 Uiso 1 1 calc R . . H28C H 0.3184 0.0275 0.4051 0.203 Uiso 1 1 calc R . . C29 C 0.1410(4) 0.0265(3) 0.4572(3) 0.0734(16) Uani 1 1 d . . . H29A H 0.1691 -0.0172 0.4468 0.088 Uiso 1 1 calc R . . H29B H 0.1260 0.0201 0.4933 0.088 Uiso 1 1 calc R . . C30 C 0.0683(5) 0.0313(5) 0.4248(3) 0.092(2) Uani 1 1 d . . . H30A H 0.0382 -0.0125 0.4296 0.138 Uiso 1 1 calc R . . H30B H 0.0819 0.0362 0.3888 0.138 Uiso 1 1 calc R . . H30C H 0.0385 0.0732 0.4355 0.138 Uiso 1 1 calc R . . C31 C 0.1524(4) 0.1618(4) 0.4661(3) 0.0734(16) Uani 1 1 d . . . H31A H 0.1139 0.1699 0.4393 0.088 Uiso 1 1 calc R . . H31B H 0.1886 0.2026 0.4648 0.088 Uiso 1 1 calc R . . C32 C 0.1125(5) 0.1619(5) 0.5188(4) 0.092(2) Uani 1 1 d . . . H32A H 0.0868 0.2081 0.5240 0.138 Uiso 1 1 calc R . . H32B H 0.1503 0.1548 0.5458 0.138 Uiso 1 1 calc R . . H32C H 0.0752 0.1228 0.5201 0.138 Uiso 1 1 calc R . . C33A C 0.8490(6) 0.2536(5) 0.8440(4) 0.061(3) Uani 0.678(6) 1 d P A 1 C35A C 0.7671(6) 0.3213(6) 0.7769(4) 0.066(3) Uani 0.678(6) 1 d P A 1 C37A C 0.8093(6) 0.1883(6) 0.7621(4) 0.071(3) Uani 0.678(6) 1 d P A 1 C39A C 0.7074(5) 0.2191(6) 0.8268(4) 0.057(2) Uani 0.678(6) 1 d P A 1 C33B C 0.8339(11) 0.1778(10) 0.8260(8) 0.053(5) Uani 0.322(6) 1 d P A 2 C35B C 0.8408(12) 0.2745(13) 0.7603(8) 0.066(3) Uani 0.322(6) 1 d P A 2 C37B C 0.7268(11) 0.1854(13) 0.7589(9) 0.066(6) Uani 0.322(6) 1 d P A 2 C39B C 0.7311(11) 0.2829(12) 0.8288(8) 0.057(2) Uani 0.322(6) 1 d P A 2 C34 C 0.8695(7) 0.1959(6) 0.8736(4) 0.113(2) Uani 1 1 d . . . C36 C 0.8292(7) 0.3493(6) 0.7431(4) 0.113(2) Uani 1 1 d . . . C38 C 0.7583(5) 0.1732(6) 0.7164(3) 0.098(2) Uani 1 1 d . . . C40 C 0.6798(5) 0.2610(6) 0.8710(3) 0.098(2) Uani 1 1 d . . . N1 N 0.7589(4) -0.0196(3) 0.3389(2) 0.0750(17) Uani 1 1 d . . . N2 N 0.6076(4) -0.0010(3) 0.3984(2) 0.0672(16) Uani 1 1 d . . . N3 N 1.0871(3) 0.2324(3) 0.8463(2) 0.0556(13) Uani 1 1 d . . . N4 N 1.0993(3) 0.3866(3) 0.80317(19) 0.0515(12) Uani 1 1 d . . . N5 N 0.1956(3) 0.0915(2) 0.4541(2) 0.0508(13) Uani 1 1 d . . . N6 N 0.7836(3) 0.2419(3) 0.7992(2) 0.0585(14) Uani 1 1 d . . . S1 S 0.76584(10) 0.16446(9) 0.55048(6) 0.0537(4) Uani 1 1 d . . . S2 S 0.90816(9) 0.15802(9) 0.49027(6) 0.0507(4) Uani 1 1 d . . . S3 S 0.95635(9) 0.14080(8) 0.65294(6) 0.0509(4) Uani 1 1 d . . . S4 S 0.94881(10) 0.29381(9) 0.61972(6) 0.0559(4) Uani 1 1 d . . . Zn1 Zn 0.89577(4) 0.19115(4) 0.57768(3) 0.0447(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.045(3) 0.042(3) 0.036(3) 0.006(2) -0.002(3) 0.005(2) C2 0.039(3) 0.048(3) 0.038(3) 0.003(2) -0.009(3) 0.009(3) C3 0.050(3) 0.050(3) 0.031(3) -0.001(2) -0.009(3) 0.014(3) C4 0.044(3) 0.082(4) 0.045(4) -0.011(3) -0.007(3) 0.013(3) C5 0.059(4) 0.103(6) 0.065(5) -0.029(4) -0.006(4) 0.021(4) C6 0.111(7) 0.094(6) 0.056(5) -0.026(4) -0.003(5) 0.027(6) C7 0.059(4) 0.046(3) 0.035(3) 0.003(3) -0.016(3) 0.008(3) C8 0.050(3) 0.045(3) 0.036(3) 0.015(2) -0.008(3) 0.003(3) C9 0.048(4) 0.066(4) 0.044(4) 0.016(3) -0.002(3) -0.002(3) C10 0.048(4) 0.094(5) 0.061(5) 0.031(4) -0.005(3) -0.013(4) C11 0.063(5) 0.100(6) 0.062(5) 0.037(4) -0.023(4) -0.036(4) C12 0.051(4) 0.058(3) 0.040(3) 0.015(3) -0.018(3) -0.004(3) C13 0.031(3) 0.052(3) 0.036(3) -0.003(2) -0.003(2) 0.007(2) C14 0.028(2) 0.046(3) 0.036(3) 0.001(2) -0.006(2) 0.003(2) C15 0.028(3) 0.058(3) 0.033(3) 0.003(2) -0.006(2) 0.001(2) C16 0.041(3) 0.055(3) 0.050(4) 0.005(3) -0.006(3) 0.001(3) C17 0.054(4) 0.061(4) 0.064(4) 0.023(3) -0.018(3) -0.015(3) C18 0.068(4) 0.079(5) 0.045(4) 0.020(3) -0.019(3) -0.006(4) C19 0.031(3) 0.060(3) 0.036(3) 0.007(3) -0.005(2) 0.002(3) C20 0.028(3) 0.048(3) 0.034(3) -0.002(2) 0.000(2) 0.003(2) C21 0.046(3) 0.055(3) 0.037(3) 0.000(3) -0.001(3) 0.009(3) C22 0.055(4) 0.045(3) 0.048(4) -0.003(3) 0.000(3) 0.002(3) C23 0.065(4) 0.048(3) 0.055(4) -0.010(3) -0.008(3) -0.004(3) C24 0.034(3) 0.052(3) 0.034(3) -0.006(2) -0.001(2) 0.003(2) C25 0.062(3) 0.103(4) 0.057(3) 0.039(3) -0.020(3) -0.018(3) C26 0.058(4) 0.125(7) 0.086(6) 0.043(5) -0.042(4) -0.020(5) C27 0.062(3) 0.103(4) 0.057(3) 0.039(3) -0.020(3) -0.018(3) C28 0.122(9) 0.211(12) 0.073(6) -0.005(7) 0.044(6) -0.036(9) C29 0.059(3) 0.054(3) 0.108(5) 0.010(3) -0.029(3) -0.005(2) C30 0.068(4) 0.094(4) 0.114(5) -0.039(4) -0.024(4) 0.003(3) C31 0.059(3) 0.054(3) 0.108(5) 0.010(3) -0.029(3) -0.005(2) C32 0.068(4) 0.094(4) 0.114(5) -0.039(4) -0.024(4) 0.003(3) C33A 0.055(6) 0.058(6) 0.068(7) -0.015(5) 0.007(5) -0.001(5) C35A 0.054(5) 0.081(6) 0.064(6) 0.015(5) 0.017(5) 0.015(5) C37A 0.063(7) 0.088(7) 0.060(7) -0.026(6) -0.006(5) 0.019(6) C39A 0.037(5) 0.073(5) 0.061(5) -0.008(5) 0.000(4) 0.003(4) C33B 0.044(11) 0.064(12) 0.051(12) 0.010(9) -0.012(9) 0.018(9) C35B 0.054(5) 0.081(6) 0.064(6) 0.015(5) 0.017(5) 0.015(5) C37B 0.031(10) 0.103(17) 0.063(14) -0.022(12) 0.007(10) 0.008(10) C39B 0.037(5) 0.073(5) 0.061(5) -0.008(5) 0.000(4) 0.003(4) C34 0.120(6) 0.129(6) 0.091(5) -0.006(4) 0.006(5) 0.039(5) C36 0.120(6) 0.129(6) 0.091(5) -0.006(4) 0.006(5) 0.039(5) C38 0.066(4) 0.174(6) 0.053(3) -0.025(4) 0.001(3) -0.018(4) C40 0.066(4) 0.174(6) 0.053(3) -0.025(4) 0.001(3) -0.018(4) N1 0.107(5) 0.068(4) 0.050(3) -0.014(3) -0.013(4) 0.006(4) N2 0.076(4) 0.076(4) 0.049(3) 0.024(3) -0.023(3) -0.030(3) N3 0.050(3) 0.073(4) 0.043(3) 0.010(3) -0.014(3) -0.008(3) N4 0.058(3) 0.057(3) 0.039(3) -0.007(2) -0.011(2) -0.003(3) N5 0.041(3) 0.053(3) 0.058(3) 0.019(2) -0.016(2) -0.003(2) N6 0.039(3) 0.081(4) 0.055(3) 0.009(3) 0.003(3) 0.009(3) S1 0.0591(10) 0.0586(9) 0.0433(9) -0.0055(7) 0.0032(8) 0.0053(8) S2 0.0457(9) 0.0667(9) 0.0397(9) -0.0070(7) -0.0063(7) -0.0025(7) S3 0.0520(9) 0.0535(8) 0.0471(9) -0.0069(7) -0.0094(7) -0.0022(7) S4 0.0682(11) 0.0593(9) 0.0401(9) 0.0003(7) -0.0205(8) 0.0069(8) Zn1 0.0435(4) 0.0544(4) 0.0363(4) -0.0048(3) -0.0079(3) 0.0019(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.393(7) . ? C1 S2 1.743(6) . ? C1 S1 1.761(6) . ? C2 C8 1.454(8) . ? C2 C3 1.456(8) . ? C3 C4 1.383(8) . ? C3 C7 1.422(8) . ? C4 C5 1.391(9) . ? C4 H4 0.9300 . ? C5 C6 1.370(11) . ? C5 H5 0.9300 . ? C6 N1 1.345(10) . ? C6 H6 0.9300 . ? C7 N1 1.357(8) . ? C7 C12 1.440(9) . ? C8 C9 1.403(8) . ? C8 C12 1.417(8) . ? C9 C10 1.371(9) . ? C9 H9 0.9300 . ? C10 C11 1.368(10) . ? C10 H10 0.9300 . ? C11 N2 1.334(10) . ? C11 H11 0.9300 . ? C12 N2 1.346(8) . ? C13 C14 1.372(7) . ? C13 S4 1.754(5) . ? C13 S3 1.754(6) . ? C14 C15 1.466(7) . ? C14 C20 1.479(7) . ? C15 C16 1.399(8) . ? C15 C19 1.417(8) . ? C16 C17 1.375(8) . ? C16 H16 0.9300 . ? C17 C18 1.383(9) . ? C17 H17 0.9300 . ? C18 N3 1.358(9) . ? C18 H18 0.9300 . ? C19 N3 1.350(7) . ? C19 C24 1.459(8) . ? C20 C21 1.393(7) . ? C20 C24 1.405(7) . ? C21 C22 1.375(8) . ? C21 H21 0.9300 . ? C22 C23 1.383(8) . ? C22 H22 0.9300 . ? C23 N4 1.336(8) . ? C23 H23 0.9300 . ? C24 N4 1.340(7) . ? C25 N5 1.490(7) . ? C25 C26 1.510(9) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 C28 1.475(13) . ? C27 N5 1.525(9) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 C30 1.510(10) . ? C29 N5 1.515(8) . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C31 N5 1.515(8) . ? C31 C32 1.522(11) . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? C33A C34 1.343(13) . ? C33A N6 1.628(11) . ? C35A C36 1.472(14) . ? C35A N6 1.581(11) . ? C37A N6 1.436(11) . ? C37A C38 1.493(12) . ? C39A C40 1.449(12) . ? C39A N6 1.552(10) . ? C33B C34 1.41(2) . ? C33B N6 1.609(18) . ? C35B C36 1.44(2) . ? C35B N6 1.53(2) . ? C37B C38 1.24(2) . ? C37B N6 1.76(2) . ? C39B N6 1.40(2) . ? C39B C40 1.46(2) . ? S1 Zn1 2.4014(18) . ? S2 Zn1 2.3364(17) . ? S3 Zn1 2.3830(17) . ? S4 Zn1 2.3451(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 C2 C1 S2 124.0(4) . . ? C2 C1 S1 123.6(4) . . ? S2 C1 S1 112.2(3) . . ? C1 C2 C8 127.4(5) . . ? C1 C2 C3 126.7(5) . . ? C8 C2 C3 105.3(5) . . ? C4 C3 C7 116.5(5) . . ? C4 C3 C2 134.7(6) . . ? C7 C3 C2 108.8(5) . . ? C3 C4 C5 119.2(6) . . ? C3 C4 H4 120.4 . . ? C5 C4 H4 120.4 . . ? C6 C5 C4 119.2(7) . . ? C6 C5 H5 120.4 . . ? C4 C5 H5 120.4 . . ? N1 C6 C5 125.4(7) . . ? N1 C6 H6 117.3 . . ? C5 C6 H6 117.3 . . ? N1 C7 C3 125.6(6) . . ? N1 C7 C12 125.7(6) . . ? C3 C7 C12 108.6(5) . . ? C9 C8 C12 116.5(6) . . ? C9 C8 C2 133.6(6) . . ? C12 C8 C2 109.9(5) . . ? C10 C9 C8 117.6(6) . . ? C10 C9 H9 121.2 . . ? C8 C9 H9 121.2 . . ? C11 C10 C9 121.3(7) . . ? C11 C10 H10 119.4 . . ? C9 C10 H10 119.4 . . ? N2 C11 C10 124.1(7) . . ? N2 C11 H11 117.9 . . ? C10 C11 H11 117.9 . . ? N2 C12 C8 125.4(6) . . ? N2 C12 C7 127.3(6) . . ? C8 C12 C7 107.2(5) . . ? C14 C13 S4 123.7(4) . . ? C14 C13 S3 123.9(4) . . ? S4 C13 S3 112.4(3) . . ? C13 C14 C15 128.1(5) . . ? C13 C14 C20 126.6(5) . . ? C15 C14 C20 105.2(4) . . ? C16 C15 C19 116.7(5) . . ? C16 C15 C14 134.2(5) . . ? C19 C15 C14 109.1(5) . . ? C17 C16 C15 117.9(6) . . ? C17 C16 H16 121.0 . . ? C15 C16 H16 121.0 . . ? C16 C17 C18 121.2(6) . . ? C16 C17 H17 119.4 . . ? C18 C17 H17 119.4 . . ? N3 C18 C17 123.7(6) . . ? N3 C18 H18 118.2 . . ? C17 C18 H18 118.2 . . ? N3 C19 C15 126.3(5) . . ? N3 C19 C24 125.5(5) . . ? C15 C19 C24 108.2(5) . . ? C21 C20 C24 116.6(5) . . ? C21 C20 C14 133.9(5) . . ? C24 C20 C14 109.3(5) . . ? C22 C21 C20 118.5(5) . . ? C22 C21 H21 120.8 . . ? C20 C21 H21 120.8 . . ? C21 C22 C23 119.8(6) . . ? C21 C22 H22 120.1 . . ? C23 C22 H22 120.1 . . ? N4 C23 C22 124.3(6) . . ? N4 C23 H23 117.9 . . ? C22 C23 H23 117.9 . . ? N4 C24 C20 126.0(5) . . ? N4 C24 C19 125.8(5) . . ? C20 C24 C19 108.2(5) . . ? N5 C25 C26 116.4(5) . . ? N5 C25 H25A 108.2 . . ? C26 C25 H25A 108.2 . . ? N5 C25 H25B 108.2 . . ? C26 C25 H25B 108.2 . . ? H25A C25 H25B 107.3 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C28 C27 N5 114.8(6) . . ? C28 C27 H27A 108.6 . . ? N5 C27 H27A 108.6 . . ? C28 C27 H27B 108.6 . . ? N5 C27 H27B 108.6 . . ? H27A C27 H27B 107.5 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C30 C29 N5 116.4(6) . . ? C30 C29 H29A 108.2 . . ? N5 C29 H29A 108.2 . . ? C30 C29 H29B 108.2 . . ? N5 C29 H29B 108.2 . . ? H29A C29 H29B 107.3 . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? N5 C31 C32 113.9(6) . . ? N5 C31 H31A 108.8 . . ? C32 C31 H31A 108.8 . . ? N5 C31 H31B 108.8 . . ? C32 C31 H31B 108.8 . . ? H31A C31 H31B 107.7 . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C34 C33A N6 118.8(8) . . ? C36 C35A N6 113.5(8) . . ? N6 C37A C38 117.7(8) . . ? C40 C39A N6 119.8(8) . . ? C34 C33B N6 116.0(14) . . ? C36 C35B N6 118.5(14) . . ? C38 C37B N6 112.3(14) . . ? N6 C39B C40 130.8(17) . . ? C33A C34 C33B 64.9(10) . . ? C35B C36 C35A 66.0(10) . . ? C37B C38 C37A 62.2(11) . . ? C39A C40 C39B 50.2(9) . . ? C6 N1 C7 114.1(6) . . ? C11 N2 C12 115.0(6) . . ? C19 N3 C18 114.3(5) . . ? C23 N4 C24 114.8(5) . . ? C25 N5 C29 106.8(5) . . ? C25 N5 C31 111.2(6) . . ? C29 N5 C31 110.0(5) . . ? C25 N5 C27 110.3(5) . . ? C29 N5 C27 110.5(6) . . ? C31 N5 C27 108.0(5) . . ? C39B N6 C37A 157.6(10) . . ? C39B N6 C35B 124.7(13) . . ? C37A N6 C35B 68.2(10) . . ? C39B N6 C39A 49.0(9) . . ? C37A N6 C39A 112.6(7) . . ? C35B N6 C39A 162.3(9) . . ? C39B N6 C35A 66.0(10) . . ? C37A N6 C35A 115.8(7) . . ? C35B N6 C35A 61.5(9) . . ? C39A N6 C35A 104.9(6) . . ? C39B N6 C33B 120.3(12) . . ? C37A N6 C33B 68.0(9) . . ? C35B N6 C33B 102.3(11) . . ? C39A N6 C33B 94.0(9) . . ? C35A N6 C33B 156.3(9) . . ? C39B N6 C33A 89.8(9) . . ? C37A N6 C33A 110.2(6) . . ? C35B N6 C33A 87.9(10) . . ? C39A N6 C33A 107.5(6) . . ? C35A N6 C33A 105.3(6) . . ? C33B N6 C33A 54.3(8) . . ? C39B N6 C37B 105.6(11) . . ? C37A N6 C37B 51.9(8) . . ? C35B N6 C37B 101.6(12) . . ? C39A N6 C37B 68.9(8) . . ? C35A N6 C37B 102.7(9) . . ? C33B N6 C37B 97.5(11) . . ? C33A N6 C37B 151.7(9) . . ? C1 S1 Zn1 84.6(2) . . ? C1 S2 Zn1 87.00(19) . . ? C13 S3 Zn1 85.07(18) . . ? C13 S4 Zn1 86.25(19) . . ? S2 Zn1 S4 127.81(7) . . ? S2 Zn1 S3 129.88(6) . . ? S4 Zn1 S3 76.14(5) . . ? S2 Zn1 S1 75.73(6) . . ? S4 Zn1 S1 131.37(6) . . ? S3 Zn1 S1 124.71(6) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.142 _refine_diff_density_min -0.889 _refine_diff_density_rms 0.108 ###Material relevant to compound 6 at 173K ######## data_e483b _database_code_depnum_ccdc_archive 'CCDC 621044' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H12 Hg N4 S4, 2(C8 H20 N), C2 H3 N' _chemical_formula_sum 'C42 H55 Hg N7 S4' _chemical_formula_weight 986.76 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Hg Hg -2.3894 9.2266 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 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 11.9427(4) _cell_length_b 13.0629(5) _cell_length_c 14.7549(6) _cell_angle_alpha 77.514(2) _cell_angle_beta 71.562(2) _cell_angle_gamma 81.054(2) _cell_volume 2122.60(14) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 8165 _cell_measurement_theta_min 0.00 _cell_measurement_theta_max 0.00 _exptl_crystal_description rod _exptl_crystal_colour orange _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.544 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1000 _exptl_absorpt_coefficient_mu 3.862 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2754 _exptl_absorpt_correction_T_max 0.5597 _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 38002 _diffrn_reflns_av_R_equivalents 0.0337 _diffrn_reflns_av_sigmaI/netI 0.0354 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.48 _diffrn_reflns_theta_max 30.05 _reflns_number_total 12377 _reflns_number_gt 10784 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _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^)+(0.0493P)^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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12377 _refine_ls_number_parameters 496 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0351 _refine_ls_R_factor_gt 0.0268 _refine_ls_wR_factor_ref 0.0848 _refine_ls_wR_factor_gt 0.0704 _refine_ls_goodness_of_fit_ref 1.121 _refine_ls_restrained_S_all 1.121 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.2433(2) 1.11052(18) 0.26208(17) 0.0191(4) Uani 1 1 d . . . C2 C 0.1505(2) 1.16120(19) 0.22676(17) 0.0187(4) Uani 1 1 d . . . C3 C 0.1551(2) 1.19687(18) 0.12420(17) 0.0193(4) Uani 1 1 d . . . C4 C 0.2467(2) 1.2047(2) 0.03693(18) 0.0245(5) Uani 1 1 d . . . H4 H 0.3255 1.1894 0.0367 0.029 Uiso 1 1 calc R . . C5 C 0.2170(3) 1.2360(2) -0.04972(19) 0.0282(5) Uani 1 1 d . . . H5 H 0.2762 1.2413 -0.1089 0.034 Uiso 1 1 calc R . . C6 C 0.0990(3) 1.2591(2) -0.0475(2) 0.0296(6) Uani 1 1 d . . . H6 H 0.0816 1.2780 -0.1064 0.036 Uiso 1 1 calc R . . C7 C 0.0382(2) 1.22551(19) 0.11738(18) 0.0203(4) Uani 1 1 d . . . C8 C 0.0247(2) 1.17592(18) 0.28156(17) 0.0182(4) Uani 1 1 d . . . C9 C -0.0388(2) 1.1586(2) 0.38030(18) 0.0222(5) Uani 1 1 d . . . H9 H 0.0001 1.1354 0.4276 0.027 Uiso 1 1 calc R . . C10 C -0.1615(2) 1.1770(2) 0.4055(2) 0.0264(5) Uani 1 1 d . . . H10 H -0.2058 1.1659 0.4706 0.032 Uiso 1 1 calc R . . C11 C -0.2186(2) 1.2122(2) 0.3337(2) 0.0291(6) Uani 1 1 d . . . H11 H -0.3010 1.2228 0.3530 0.035 Uiso 1 1 calc R . . C12 C -0.0432(2) 1.21288(18) 0.21546(18) 0.0198(4) Uani 1 1 d . . . C13 C 0.6506(2) 0.83805(19) 0.34325(17) 0.0200(4) Uani 1 1 d . . . C14 C 0.7598(2) 0.77834(18) 0.33026(16) 0.0190(4) Uani 1 1 d . . . C15 C 0.8695(2) 0.80446(19) 0.34166(16) 0.0189(4) Uani 1 1 d . . . C16 C 0.9010(2) 0.8913(2) 0.36733(17) 0.0216(5) Uani 1 1 d . . . H16 H 0.8467 0.9495 0.3803 0.026 Uiso 1 1 calc R . . C17 C 1.0158(2) 0.8875(2) 0.37273(18) 0.0233(5) Uani 1 1 d . . . H17 H 1.0385 0.9431 0.3910 0.028 Uiso 1 1 calc R . . C18 C 1.0971(2) 0.8009(2) 0.35100(19) 0.0261(5) Uani 1 1 d . . . H18 H 1.1734 0.8016 0.3543 0.031 Uiso 1 1 calc R . . C19 C 0.9596(2) 0.72039(19) 0.32231(17) 0.0210(4) Uani 1 1 d . . . C20 C 0.7886(2) 0.67239(19) 0.30532(17) 0.0206(4) Uani 1 1 d . . . C21 C 0.7227(3) 0.6008(2) 0.2896(2) 0.0269(5) Uani 1 1 d . . . H21 H 0.6436 0.6184 0.2916 0.032 Uiso 1 1 calc R . . C22 C 0.7798(3) 0.5032(2) 0.2710(2) 0.0332(6) Uani 1 1 d . . . H22 H 0.7381 0.4537 0.2620 0.040 Uiso 1 1 calc R . . C23 C 0.8992(3) 0.4791(2) 0.2657(3) 0.0405(7) Uani 1 1 d . . . H23 H 0.9352 0.4138 0.2512 0.049 Uiso 1 1 calc R . . C24 C 0.9088(2) 0.63797(19) 0.30023(18) 0.0222(5) Uani 1 1 d . . . C25 C 0.3353(2) 0.3420(3) 0.4398(2) 0.0332(6) Uani 1 1 d . . . H25A H 0.3111 0.3650 0.5020 0.040 Uiso 1 1 calc R . . H25B H 0.2986 0.2779 0.4489 0.040 Uiso 1 1 calc R . . C26 C 0.4680(3) 0.3167(4) 0.4104(3) 0.0610(12) Uani 1 1 d . . . H26A H 0.4920 0.2834 0.3543 0.091 Uiso 1 1 calc R . . H26B H 0.4906 0.2700 0.4628 0.091 Uiso 1 1 calc R . . H26C H 0.5058 0.3805 0.3952 0.091 Uiso 1 1 calc R . . C27 C 0.3403(3) 0.5292(3) 0.3498(2) 0.0435(8) Uani 1 1 d . . . H27A H 0.3023 0.5809 0.3081 0.052 Uiso 1 1 calc R . . H27B H 0.4238 0.5195 0.3146 0.052 Uiso 1 1 calc R . . C28 C 0.3289(4) 0.5736(4) 0.4401(3) 0.0658(12) Uani 1 1 d . . . H28A H 0.2466 0.5873 0.4739 0.099 Uiso 1 1 calc R . . H28B H 0.3664 0.6380 0.4213 0.099 Uiso 1 1 calc R . . H28C H 0.3667 0.5235 0.4819 0.099 Uiso 1 1 calc R . . C29 C 0.3185(3) 0.3849(3) 0.2742(2) 0.0398(7) Uani 1 1 d . . . H29A H 0.2898 0.3161 0.2881 0.048 Uiso 1 1 calc R . . H29B H 0.4041 0.3759 0.2483 0.048 Uiso 1 1 calc R . . C30 C 0.2687(3) 0.4547(3) 0.1966(2) 0.0507(9) Uani 1 1 d . . . H30A H 0.1847 0.4700 0.2232 0.076 Uiso 1 1 calc R . . H30B H 0.2839 0.4191 0.1429 0.076 Uiso 1 1 calc R . . H30C H 0.3059 0.5193 0.1748 0.076 Uiso 1 1 calc R . . C31 C 0.1547(2) 0.4452(2) 0.41262(19) 0.0245(5) Uani 1 1 d . . . H31A H 0.1258 0.5067 0.3733 0.029 Uiso 1 1 calc R . . H31B H 0.1395 0.4614 0.4768 0.029 Uiso 1 1 calc R . . C32 C 0.0843(2) 0.3547(2) 0.4214(2) 0.0304(6) Uani 1 1 d . . . H32A H 0.0940 0.3409 0.3579 0.046 Uiso 1 1 calc R . . H32B H 0.0019 0.3729 0.4521 0.046 Uiso 1 1 calc R . . H32C H 0.1123 0.2929 0.4597 0.046 Uiso 1 1 calc R . . C33 C 0.7098(2) 0.2425(2) 0.0473(2) 0.0295(6) Uani 1 1 d . . . H33A H 0.7792 0.2403 0.0686 0.035 Uiso 1 1 calc R . . H33B H 0.7098 0.3046 -0.0026 0.035 Uiso 1 1 calc R . . C34 C 0.6006(3) 0.2541(3) 0.1322(3) 0.0528(10) Uani 1 1 d . . . H34A H 0.5310 0.2555 0.1124 0.079 Uiso 1 1 calc R . . H34B H 0.5990 0.3185 0.1541 0.079 Uiso 1 1 calc R . . H34C H 0.6022 0.1956 0.1841 0.079 Uiso 1 1 calc R . . C35 C 0.6196(2) 0.1466(2) -0.0403(2) 0.0298(6) Uani 1 1 d . . . H35A H 0.6318 0.0837 -0.0684 0.036 Uiso 1 1 calc R . . H35B H 0.5462 0.1431 0.0123 0.036 Uiso 1 1 calc R . . C36 C 0.6054(3) 0.2418(3) -0.1174(3) 0.0459(8) Uani 1 1 d . . . H36A H 0.5846 0.3042 -0.0889 0.069 Uiso 1 1 calc R . . H36B H 0.5439 0.2330 -0.1433 0.069 Uiso 1 1 calc R . . H36C H 0.6786 0.2484 -0.1686 0.069 Uiso 1 1 calc R . . C37 C 0.7164(2) 0.0452(2) 0.07790(18) 0.0253(5) Uani 1 1 d . . . H37A H 0.6423 0.0497 0.1293 0.030 Uiso 1 1 calc R . . H37B H 0.7164 -0.0139 0.0478 0.030 Uiso 1 1 calc R . . C38 C 0.8174(3) 0.0229(2) 0.1228(2) 0.0347(6) Uani 1 1 d . . . H38A H 0.8912 0.0142 0.0733 0.052 Uiso 1 1 calc R . . H38B H 0.8066 -0.0403 0.1708 0.052 Uiso 1 1 calc R . . H38C H 0.8184 0.0808 0.1530 0.052 Uiso 1 1 calc R . . C39 C 0.8401(2) 0.1466(2) -0.07624(18) 0.0232(5) Uani 1 1 d . . . H39A H 0.8377 0.2087 -0.1257 0.028 Uiso 1 1 calc R . . H39B H 0.9011 0.1524 -0.0476 0.028 Uiso 1 1 calc R . . C40 C 0.8745(2) 0.0508(2) -0.1243(2) 0.0299(6) Uani 1 1 d . . . H40A H 0.8841 -0.0106 -0.0772 0.045 Uiso 1 1 calc R . . H40B H 0.9478 0.0594 -0.1753 0.045 Uiso 1 1 calc R . . H40C H 0.8136 0.0428 -0.1511 0.045 Uiso 1 1 calc R . . N1 N 0.0083(2) 1.25574(18) 0.03451(16) 0.0257(4) Uani 1 1 d . . . N2 N -0.16166(19) 1.23154(18) 0.23846(17) 0.0259(4) Uani 1 1 d . . . N3 N 1.0715(2) 0.71634(18) 0.32558(16) 0.0247(4) Uani 1 1 d . . . N4 N 0.9650(2) 0.5446(2) 0.2803(2) 0.0340(5) Uani 1 1 d . . . N5 N 0.28741(19) 0.42581(18) 0.36883(15) 0.0254(4) Uani 1 1 d . . . N6 N 0.72105(18) 0.14560(16) 0.00217(15) 0.0213(4) Uani 1 1 d . . . S2 S 0.22724(5) 1.07730(5) 0.38766(4) 0.02359(12) Uani 1 1 d . . . S3 S 0.62612(6) 0.95860(5) 0.38465(5) 0.02744(13) Uani 1 1 d . . . S1 S 0.38116(5) 1.07175(6) 0.18793(5) 0.02999(14) Uani 1 1 d . . . S4 S 0.52914(6) 0.80068(6) 0.32147(6) 0.03207(15) Uani 1 1 d . . . Hg1 Hg 0.428493(8) 0.992933(8) 0.362059(7) 0.02925(4) Uani 1 1 d . . . C41 C 0.8330(4) 0.4939(3) 0.0218(3) 0.0532(9) Uani 1 1 d . . . H41A H 0.8728 0.5453 0.0344 0.080 Uiso 1 1 calc R . . H41B H 0.8514 0.4979 -0.0470 0.080 Uiso 1 1 calc R . . H41C H 0.8589 0.4248 0.0506 0.080 Uiso 1 1 calc R . . C42 C 0.7048(4) 0.5145(3) 0.0636(3) 0.0490(9) Uani 1 1 d . . . N7 N 0.6065(4) 0.5289(3) 0.0969(3) 0.0682(10) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0186(10) 0.0184(11) 0.0205(11) -0.0035(8) -0.0054(8) -0.0026(8) C2 0.0184(10) 0.0185(11) 0.0197(11) -0.0038(8) -0.0062(8) -0.0007(8) C3 0.0204(10) 0.0164(10) 0.0219(11) -0.0020(8) -0.0086(9) -0.0012(8) C4 0.0224(11) 0.0263(13) 0.0232(12) -0.0013(9) -0.0072(9) -0.0013(9) C5 0.0314(13) 0.0304(14) 0.0197(12) 0.0003(10) -0.0060(10) -0.0040(11) C6 0.0350(14) 0.0333(15) 0.0225(12) 0.0018(10) -0.0149(11) -0.0050(11) C7 0.0215(11) 0.0167(11) 0.0241(11) -0.0039(8) -0.0095(9) 0.0006(8) C8 0.0184(10) 0.0152(10) 0.0220(11) -0.0069(8) -0.0061(8) 0.0009(8) C9 0.0214(11) 0.0202(12) 0.0242(12) -0.0067(9) -0.0059(9) 0.0024(9) C10 0.0212(11) 0.0269(13) 0.0287(13) -0.0085(10) -0.0035(10) 0.0015(10) C11 0.0180(11) 0.0317(14) 0.0368(15) -0.0114(11) -0.0058(10) 0.0030(10) C12 0.0207(11) 0.0151(10) 0.0258(12) -0.0069(8) -0.0091(9) 0.0010(8) C13 0.0227(11) 0.0197(11) 0.0161(10) -0.0015(8) -0.0049(9) -0.0014(9) C14 0.0225(11) 0.0187(11) 0.0145(10) -0.0005(8) -0.0054(8) -0.0012(8) C15 0.0220(11) 0.0190(11) 0.0142(10) -0.0008(8) -0.0060(8) 0.0006(8) C16 0.0246(11) 0.0196(11) 0.0201(11) -0.0028(9) -0.0074(9) 0.0001(9) C17 0.0260(12) 0.0234(12) 0.0221(12) -0.0028(9) -0.0090(9) -0.0043(9) C18 0.0224(11) 0.0298(13) 0.0281(13) -0.0034(10) -0.0120(10) -0.0009(10) C19 0.0232(11) 0.0201(11) 0.0196(11) -0.0016(8) -0.0089(9) 0.0014(9) C20 0.0258(11) 0.0186(11) 0.0166(10) 0.0000(8) -0.0085(9) 0.0005(9) C21 0.0315(13) 0.0231(13) 0.0288(13) -0.0020(10) -0.0139(11) -0.0037(10) C22 0.0423(16) 0.0222(13) 0.0425(16) -0.0076(11) -0.0217(13) -0.0022(11) C23 0.0520(19) 0.0246(14) 0.058(2) -0.0187(13) -0.0342(17) 0.0118(13) C24 0.0272(12) 0.0192(11) 0.0221(11) -0.0038(9) -0.0126(10) 0.0038(9) C25 0.0263(13) 0.0420(16) 0.0249(13) 0.0031(11) -0.0076(11) 0.0033(11) C26 0.0285(16) 0.099(3) 0.0411(19) 0.005(2) -0.0116(14) 0.0136(18) C27 0.0381(16) 0.0483(19) 0.0403(17) 0.0111(14) -0.0103(14) -0.0221(15) C28 0.080(3) 0.060(3) 0.068(3) -0.009(2) -0.024(2) -0.040(2) C29 0.0309(14) 0.060(2) 0.0239(14) -0.0128(13) -0.0051(11) 0.0111(14) C30 0.050(2) 0.076(3) 0.0239(15) -0.0030(15) -0.0151(14) 0.0026(18) C31 0.0199(11) 0.0236(12) 0.0274(12) -0.0061(9) -0.0040(9) 0.0016(9) C32 0.0276(13) 0.0287(14) 0.0340(14) -0.0032(11) -0.0096(11) -0.0029(11) C33 0.0286(13) 0.0240(13) 0.0362(15) -0.0120(11) -0.0046(11) -0.0047(10) C34 0.0402(18) 0.051(2) 0.065(2) -0.0416(19) 0.0112(16) -0.0121(16) C35 0.0230(12) 0.0350(15) 0.0329(14) -0.0074(11) -0.0094(11) -0.0033(11) C36 0.0415(18) 0.049(2) 0.049(2) -0.0013(15) -0.0253(16) 0.0036(15) C37 0.0279(12) 0.0225(12) 0.0226(12) -0.0022(9) -0.0027(10) -0.0060(10) C38 0.0407(16) 0.0346(15) 0.0262(13) 0.0018(11) -0.0115(12) -0.0028(12) C39 0.0198(11) 0.0250(12) 0.0217(11) -0.0028(9) -0.0022(9) -0.0037(9) C40 0.0268(13) 0.0346(15) 0.0253(13) -0.0097(11) -0.0016(10) -0.0003(11) N1 0.0279(11) 0.0258(11) 0.0252(11) -0.0012(8) -0.0128(9) -0.0020(9) N2 0.0201(10) 0.0275(11) 0.0325(12) -0.0092(9) -0.0110(9) 0.0029(8) N3 0.0246(10) 0.0256(11) 0.0251(11) -0.0061(8) -0.0112(9) 0.0049(8) N4 0.0390(13) 0.0259(12) 0.0458(15) -0.0152(10) -0.0253(12) 0.0103(10) N5 0.0210(10) 0.0319(12) 0.0190(10) -0.0007(8) -0.0032(8) -0.0009(8) N6 0.0204(9) 0.0198(10) 0.0223(10) -0.0045(8) -0.0031(8) -0.0034(8) S2 0.0206(3) 0.0303(3) 0.0188(3) -0.0055(2) -0.0070(2) 0.0049(2) S3 0.0228(3) 0.0286(3) 0.0359(3) -0.0148(3) -0.0140(3) 0.0070(2) S1 0.0159(3) 0.0466(4) 0.0215(3) -0.0013(3) -0.0033(2) 0.0032(3) S4 0.0242(3) 0.0269(3) 0.0500(4) -0.0086(3) -0.0175(3) -0.0005(2) Hg1 0.01945(5) 0.03175(6) 0.03284(7) 0.00055(4) -0.00976(4) 0.00414(4) C41 0.057(2) 0.046(2) 0.066(3) -0.0165(18) -0.031(2) 0.0039(17) C42 0.060(2) 0.0302(17) 0.067(2) -0.0079(15) -0.036(2) -0.0002(15) N7 0.057(2) 0.052(2) 0.101(3) -0.014(2) -0.031(2) 0.0000(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.388(3) . ? C1 S1 1.733(2) . ? C1 S2 1.764(2) . ? C2 C8 1.469(3) . ? C2 C3 1.470(3) . ? C3 C4 1.397(3) . ? C3 C7 1.418(3) . ? C4 C5 1.395(4) . ? C4 H4 0.9300 . ? C5 C6 1.386(4) . ? C5 H5 0.9300 . ? C6 N1 1.343(4) . ? C6 H6 0.9300 . ? C7 N1 1.342(3) . ? C7 C12 1.457(3) . ? C8 C9 1.400(3) . ? C8 C12 1.420(3) . ? C9 C10 1.388(3) . ? C9 H9 0.9300 . ? C10 C11 1.397(4) . ? C10 H10 0.9300 . ? C11 N2 1.340(4) . ? C11 H11 0.9300 . ? C12 N2 1.342(3) . ? C13 C14 1.392(3) . ? C13 S4 1.740(2) . ? C13 S3 1.760(3) . ? C14 C20 1.470(3) . ? C14 C15 1.471(3) . ? C15 C16 1.407(3) . ? C15 C19 1.421(3) . ? C16 C17 1.391(3) . ? C16 H16 0.9300 . ? C17 C18 1.394(4) . ? C17 H17 0.9300 . ? C18 N3 1.346(4) . ? C18 H18 0.9300 . ? C19 N3 1.345(3) . ? C19 C24 1.453(3) . ? C20 C21 1.409(4) . ? C20 C24 1.420(3) . ? C21 C22 1.388(4) . ? C21 H21 0.9300 . ? C22 C23 1.392(4) . ? C22 H22 0.9300 . ? C23 N4 1.338(4) . ? C23 H23 0.9300 . ? C24 N4 1.342(3) . ? C25 C26 1.508(4) . ? C25 N5 1.520(3) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 N5 1.514(4) . ? C27 C28 1.524(5) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 N5 1.518(4) . ? C29 C30 1.519(4) . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C31 N5 1.513(3) . ? C31 C32 1.515(4) . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? C33 C34 1.510(4) . ? C33 N6 1.522(3) . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C35 C36 1.521(4) . ? C35 N6 1.527(3) . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? C37 C38 1.514(4) . ? C37 N6 1.524(3) . ? C37 H37A 0.9700 . ? C37 H37B 0.9700 . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? C39 C40 1.509(4) . ? C39 N6 1.522(3) . ? C39 H39A 0.9700 . ? C39 H39B 0.9700 . ? C40 H40A 0.9600 . ? C40 H40B 0.9600 . ? C40 H40C 0.9600 . ? S2 Hg1 2.4323(6) . ? S3 Hg1 2.4467(6) . ? S1 Hg1 2.7522(7) . ? S4 Hg1 2.7142(7) . ? C41 C42 1.464(6) . ? C41 H41A 0.9600 . ? C41 H41B 0.9600 . ? C41 H41C 0.9600 . ? C42 N7 1.123(5) . ? 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 C2 C1 S1 123.28(18) . . ? C2 C1 S2 121.77(18) . . ? S1 C1 S2 114.93(13) . . ? C1 C2 C8 127.5(2) . . ? C1 C2 C3 126.5(2) . . ? C8 C2 C3 105.32(19) . . ? C4 C3 C7 116.8(2) . . ? C4 C3 C2 134.0(2) . . ? C7 C3 C2 109.2(2) . . ? C5 C4 C3 118.3(2) . . ? C5 C4 H4 120.9 . . ? C3 C4 H4 120.9 . . ? C6 C5 C4 119.9(2) . . ? C6 C5 H5 120.1 . . ? C4 C5 H5 120.1 . . ? N1 C6 C5 124.0(2) . . ? N1 C6 H6 118.0 . . ? C5 C6 H6 118.0 . . ? N1 C7 C3 125.6(2) . . ? N1 C7 C12 126.3(2) . . ? C3 C7 C12 108.1(2) . . ? C9 C8 C12 116.4(2) . . ? C9 C8 C2 134.4(2) . . ? C12 C8 C2 109.2(2) . . ? C10 C9 C8 118.1(2) . . ? C10 C9 H9 121.0 . . ? C8 C9 H9 121.0 . . ? C9 C10 C11 120.3(2) . . ? C9 C10 H10 119.8 . . ? C11 C10 H10 119.8 . . ? N2 C11 C10 123.8(2) . . ? N2 C11 H11 118.1 . . ? C10 C11 H11 118.1 . . ? N2 C12 C8 126.4(2) . . ? N2 C12 C7 125.6(2) . . ? C8 C12 C7 108.0(2) . . ? C14 C13 S4 123.67(19) . . ? C14 C13 S3 121.25(18) . . ? S4 C13 S3 115.08(14) . . ? C13 C14 C20 126.7(2) . . ? C13 C14 C15 128.3(2) . . ? C20 C14 C15 105.0(2) . . ? C16 C15 C19 116.4(2) . . ? C16 C15 C14 134.1(2) . . ? C19 C15 C14 109.5(2) . . ? C17 C16 C15 118.0(2) . . ? C17 C16 H16 121.0 . . ? C15 C16 H16 121.0 . . ? C16 C17 C18 120.4(2) . . ? C16 C17 H17 119.8 . . ? C18 C17 H17 119.8 . . ? N3 C18 C17 123.8(2) . . ? N3 C18 H18 118.1 . . ? C17 C18 H18 118.1 . . ? N3 C19 C15 126.3(2) . . ? N3 C19 C24 125.8(2) . . ? C15 C19 C24 107.9(2) . . ? C21 C20 C24 116.6(2) . . ? C21 C20 C14 134.0(2) . . ? C24 C20 C14 109.4(2) . . ? C22 C21 C20 117.8(3) . . ? C22 C21 H21 121.1 . . ? C20 C21 H21 121.1 . . ? C21 C22 C23 120.5(3) . . ? C21 C22 H22 119.8 . . ? C23 C22 H22 119.8 . . ? N4 C23 C22 123.7(3) . . ? N4 C23 H23 118.2 . . ? C22 C23 H23 118.2 . . ? N4 C24 C20 125.8(2) . . ? N4 C24 C19 126.0(2) . . ? C20 C24 C19 108.2(2) . . ? C26 C25 N5 115.6(2) . . ? C26 C25 H25A 108.4 . . ? N5 C25 H25A 108.4 . . ? C26 C25 H25B 108.4 . . ? N5 C25 H25B 108.4 . . ? H25A C25 H25B 107.5 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? N5 C27 C28 115.2(3) . . ? N5 C27 H27A 108.5 . . ? C28 C27 H27A 108.5 . . ? N5 C27 H27B 108.5 . . ? C28 C27 H27B 108.5 . . ? H27A C27 H27B 107.5 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? N5 C29 C30 115.1(3) . . ? N5 C29 H29A 108.5 . . ? C30 C29 H29A 108.5 . . ? N5 C29 H29B 108.5 . . ? C30 C29 H29B 108.5 . . ? H29A C29 H29B 107.5 . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? N5 C31 C32 115.3(2) . . ? N5 C31 H31A 108.4 . . ? C32 C31 H31A 108.4 . . ? N5 C31 H31B 108.4 . . ? C32 C31 H31B 108.4 . . ? H31A C31 H31B 107.5 . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C34 C33 N6 115.2(2) . . ? C34 C33 H33A 108.5 . . ? N6 C33 H33A 108.5 . . ? C34 C33 H33B 108.5 . . ? N6 C33 H33B 108.5 . . ? H33A C33 H33B 107.5 . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C36 C35 N6 115.5(2) . . ? C36 C35 H35A 108.4 . . ? N6 C35 H35A 108.4 . . ? C36 C35 H35B 108.4 . . ? N6 C35 H35B 108.4 . . ? H35A C35 H35B 107.5 . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C38 C37 N6 114.8(2) . . ? C38 C37 H37A 108.6 . . ? N6 C37 H37A 108.6 . . ? C38 C37 H37B 108.6 . . ? N6 C37 H37B 108.6 . . ? H37A C37 H37B 107.5 . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C40 C39 N6 114.6(2) . . ? C40 C39 H39A 108.6 . . ? N6 C39 H39A 108.6 . . ? C40 C39 H39B 108.6 . . ? N6 C39 H39B 108.6 . . ? H39A C39 H39B 107.6 . . ? C39 C40 H40A 109.5 . . ? C39 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C39 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C7 N1 C6 115.5(2) . . ? C11 N2 C12 115.1(2) . . ? C19 N3 C18 115.0(2) . . ? C23 N4 C24 115.7(2) . . ? C31 N5 C27 107.9(2) . . ? C31 N5 C29 111.8(2) . . ? C27 N5 C29 109.2(2) . . ? C31 N5 C25 108.17(19) . . ? C27 N5 C25 112.1(2) . . ? C29 N5 C25 107.6(2) . . ? C33 N6 C39 105.84(19) . . ? C33 N6 C37 111.1(2) . . ? C39 N6 C37 110.80(19) . . ? C33 N6 C35 112.1(2) . . ? C39 N6 C35 111.16(19) . . ? C37 N6 C35 105.98(19) . . ? C1 S2 Hg1 92.84(8) . . ? C13 S3 Hg1 91.53(8) . . ? C1 S1 Hg1 83.22(8) . . ? C13 S4 Hg1 83.43(8) . . ? S2 Hg1 S3 155.09(2) . . ? S2 Hg1 S4 132.82(2) . . ? S3 Hg1 S4 69.60(2) . . ? S2 Hg1 S1 69.00(2) . . ? S3 Hg1 S1 125.28(2) . . ? S4 Hg1 S1 97.08(2) . . ? C42 C41 H41A 109.5 . . ? C42 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C42 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? N7 C42 C41 178.8(5) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 30.05 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.552 _refine_diff_density_min -1.563 _refine_diff_density_rms 0.185 ###Material relevant to compound 7 at 173K ######## data_e541a _database_code_depnum_ccdc_archive 'CCDC 621045' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C40 H52 N12 Ni2 Pd S4, 6(C3 H7 N O), 2(B F4)' _chemical_formula_sum 'C58 H94 B2 F8 N18 Ni2 O6 Pd S4' _chemical_formula_weight 1665.19 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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 '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' Pd Pd -0.9988 1.0072 '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 8.4793(6) _cell_length_b 8.6656(7) _cell_length_c 25.7473(18) _cell_angle_alpha 84.402(4) _cell_angle_beta 88.143(4) _cell_angle_gamma 80.473(4) _cell_volume 1856.6(2) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 4939 _cell_measurement_theta_min 2.44 _cell_measurement_theta_max 27.11 _exptl_crystal_description platelet _exptl_crystal_colour orange _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.489 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 864 _exptl_absorpt_coefficient_mu 0.933 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7867 _exptl_absorpt_correction_T_max 0.9291 _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 26190 _diffrn_reflns_av_R_equivalents 0.0796 _diffrn_reflns_av_sigmaI/netI 0.1018 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 0.79 _diffrn_reflns_theta_max 27.19 _reflns_number_total 8082 _reflns_number_gt 5026 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _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^)+(0.1007P)^2^+0.9684P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8082 _refine_ls_number_parameters 454 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1166 _refine_ls_R_factor_gt 0.0665 _refine_ls_wR_factor_ref 0.1884 _refine_ls_wR_factor_gt 0.1683 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.032 _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 Ni1 Ni 0.18885(8) 0.14428(8) -0.35605(2) 0.01952(19) Uani 1 1 d . . . Pd1 Pd 0.0000 0.0000 0.0000 0.02733(19) Uani 1 2 d S . . S2 S 0.15292(19) -0.10918(18) -0.06795(5) 0.0332(4) Uani 1 1 d . . . S1 S -0.09923(19) 0.14861(19) -0.07551(5) 0.0331(4) Uani 1 1 d . . . N1 N 0.0121(5) 0.2366(5) -0.29689(15) 0.0217(10) Uani 1 1 d . . . N2 N 0.2852(5) -0.0134(5) -0.28763(15) 0.0230(10) Uani 1 1 d . . . N3 N 0.0714(5) 0.3145(5) -0.41104(15) 0.0258(10) Uani 1 1 d . . . H3 H -0.0097 0.3708 -0.3934 0.031 Uiso 1 1 calc R . . N4 N 0.0453(5) -0.0006(5) -0.38758(16) 0.0243(10) Uani 1 1 d . . . H4A H -0.0085 -0.0474 -0.3610 0.029 Uiso 1 1 calc R . . N5 N 0.3668(5) 0.0219(5) -0.40157(15) 0.0251(10) Uani 1 1 d . . . H5A H 0.4234 -0.0538 -0.3794 0.030 Uiso 1 1 calc R . . N6 N 0.3516(5) 0.3049(5) -0.35695(17) 0.0242(10) Uani 1 1 d . . . H6A H 0.3682 0.3235 -0.3236 0.029 Uiso 1 1 calc R . . C1 C 0.0461(6) 0.0337(6) -0.11023(19) 0.0244(12) Uani 1 1 d . . . C2 C 0.0740(6) 0.0569(6) -0.16398(18) 0.0205(11) Uani 1 1 d . . . C3 C -0.0157(6) 0.1738(6) -0.20162(18) 0.0203(11) Uani 1 1 d . . . C4 C -0.1549(6) 0.2868(6) -0.20067(19) 0.0241(12) Uani 1 1 d . . . H4 H -0.2105 0.3060 -0.1696 0.029 Uiso 1 1 calc R . . C5 C -0.2061(7) 0.3679(7) -0.2472(2) 0.0290(13) Uani 1 1 d . . . H5 H -0.2993 0.4415 -0.2476 0.035 Uiso 1 1 calc R . . C6 C -0.1225(7) 0.3431(6) -0.2940(2) 0.0271(13) Uani 1 1 d . . . H6 H -0.1610 0.4023 -0.3244 0.033 Uiso 1 1 calc R . . C7 C 0.0570(6) 0.1580(6) -0.25171(18) 0.0209(11) Uani 1 1 d . . . C8 C 0.2031(6) -0.0310(6) -0.19381(18) 0.0195(11) Uani 1 1 d . . . C9 C 0.3259(7) -0.1555(6) -0.18323(19) 0.0279(13) Uani 1 1 d . . . H9 H 0.3419 -0.2039 -0.1495 0.034 Uiso 1 1 calc R . . C10 C 0.4252(7) -0.2064(7) -0.2246(2) 0.0281(13) Uani 1 1 d . . . H10 H 0.5088 -0.2896 -0.2182 0.034 Uiso 1 1 calc R . . C11 C 0.4015(7) -0.1348(7) -0.2752(2) 0.0289(13) Uani 1 1 d . . . H11 H 0.4699 -0.1732 -0.3016 0.035 Uiso 1 1 calc R . . C12 C 0.1905(6) 0.0337(6) -0.24653(17) 0.0163(10) Uani 1 1 d . . . C13 C -0.0048(7) 0.2410(7) -0.4505(2) 0.0320(13) Uani 1 1 d . . . H13A H 0.0729 0.2056 -0.4771 0.038 Uiso 1 1 calc R . . H13B H -0.0902 0.3160 -0.4672 0.038 Uiso 1 1 calc R . . C14 C -0.0723(7) 0.1009(7) -0.4225(2) 0.0335(14) Uani 1 1 d . . . H14A H -0.1664 0.1397 -0.4022 0.040 Uiso 1 1 calc R . . H14B H -0.1051 0.0388 -0.4484 0.040 Uiso 1 1 calc R . . C15 C 0.1529(7) -0.1237(7) -0.4132(2) 0.0327(14) Uani 1 1 d . . . H15A H 0.0938 -0.1640 -0.4390 0.039 Uiso 1 1 calc R . . H15B H 0.1905 -0.2099 -0.3873 0.039 Uiso 1 1 calc R . . C16 C 0.2963(7) -0.0612(7) -0.4396(2) 0.0310(13) Uani 1 1 d . . . H16A H 0.3742 -0.1473 -0.4506 0.037 Uiso 1 1 calc R . . H16B H 0.2624 0.0099 -0.4701 0.037 Uiso 1 1 calc R . . C17 C 0.4805(7) 0.1265(7) -0.4222(2) 0.0324(14) Uani 1 1 d . . . H17A H 0.4378 0.1904 -0.4532 0.039 Uiso 1 1 calc R . . H17B H 0.5816 0.0643 -0.4315 0.039 Uiso 1 1 calc R . . C18 C 0.5053(6) 0.2309(7) -0.3800(2) 0.0287(13) Uani 1 1 d . . . H18A H 0.5698 0.1685 -0.3526 0.034 Uiso 1 1 calc R . . H18B H 0.5635 0.3126 -0.3948 0.034 Uiso 1 1 calc R . . C19 C 0.2769(8) 0.4545(7) -0.3863(2) 0.0356(14) Uani 1 1 d . . . H19A H 0.3603 0.5125 -0.3998 0.043 Uiso 1 1 calc R . . H19B H 0.2096 0.5183 -0.3627 0.043 Uiso 1 1 calc R . . C20 C 0.1782(8) 0.4268(7) -0.4308(2) 0.0345(14) Uani 1 1 d . . . H20A H 0.1153 0.5251 -0.4447 0.041 Uiso 1 1 calc R . . H20B H 0.2472 0.3841 -0.4585 0.041 Uiso 1 1 calc R . . B1 B 0.7191(9) 0.6696(9) 0.5864(2) 0.0355(17) Uani 1 1 d . . . F1 F 0.8707(5) 0.6488(6) 0.60886(18) 0.0766(14) Uani 1 1 d . . . F2 F 0.7096(7) 0.5303(5) 0.5680(2) 0.0929(18) Uani 1 1 d . . . F3 F 0.7101(5) 0.7885(5) 0.54780(15) 0.0647(13) Uani 1 1 d . . . F4 F 0.5996(5) 0.7030(5) 0.62378(15) 0.0605(12) Uani 1 1 d . . . O1 O 0.3516(6) 0.3866(6) 0.74868(17) 0.0504(12) Uani 1 1 d . . . N7 N 0.3736(6) 0.2939(6) 0.8348(2) 0.0408(13) Uani 1 1 d . . . C21 C 0.4110(8) 0.2914(8) 0.7839(3) 0.0411(16) Uani 1 1 d . . . H21 H 0.4892 0.2100 0.7745 0.049 Uiso 1 1 calc R . . C22 C 0.4562(9) 0.1783(9) 0.8733(3) 0.064(2) Uani 1 1 d . . . H22A H 0.5324 0.1047 0.8560 0.096 Uiso 1 1 calc R . . H22B H 0.3802 0.1235 0.8925 0.096 Uiso 1 1 calc R . . H22C H 0.5109 0.2300 0.8968 0.096 Uiso 1 1 calc R . . C23 C 0.2539(10) 0.4124(9) 0.8527(3) 0.056(2) Uani 1 1 d . . . H23A H 0.2031 0.4758 0.8233 0.084 Uiso 1 1 calc R . . H23B H 0.3020 0.4774 0.8736 0.084 Uiso 1 1 calc R . . H23C H 0.1756 0.3643 0.8733 0.084 Uiso 1 1 calc R . . O2 O 0.8015(5) 0.9588(6) 0.69501(18) 0.0493(12) Uani 1 1 d . . . N8 N 0.8963(6) 0.7846(6) 0.7631(2) 0.0392(13) Uani 1 1 d . . . C24 C 0.8007(8) 0.9086(8) 0.7411(3) 0.0403(16) Uani 1 1 d . . . H24 H 0.7257 0.9626 0.7627 0.048 Uiso 1 1 calc R . . C25 C 0.8850(10) 0.7378(9) 0.8194(3) 0.056(2) Uani 1 1 d . . . H25A H 0.8029 0.8097 0.8350 0.083 Uiso 1 1 calc R . . H25B H 0.9856 0.7395 0.8352 0.083 Uiso 1 1 calc R . . H25C H 0.8592 0.6335 0.8247 0.083 Uiso 1 1 calc R . . C26 C 1.0149(8) 0.6932(7) 0.7317(3) 0.0451(17) Uani 1 1 d . . . H26A H 0.9820 0.7070 0.6960 0.068 Uiso 1 1 calc R . . H26B H 1.0253 0.5841 0.7443 0.068 Uiso 1 1 calc R . . H26C H 1.1160 0.7280 0.7340 0.068 Uiso 1 1 calc R . . O3 O 0.5797(8) 0.5688(8) 0.8858(3) 0.088(2) Uani 1 1 d . . . N9 N 0.6805(8) 0.6438(8) 0.9576(2) 0.0590(17) Uani 1 1 d . . . C27 C 0.6544(13) 0.5445(12) 0.9246(4) 0.086(3) Uani 1 1 d . . . H27 H 0.7012 0.4406 0.9329 0.103 Uiso 1 1 calc R . . C28 C 0.787(2) 0.5965(16) 1.0011(6) 0.175(7) Uani 1 1 d . . . H28A H 0.7260 0.5959 1.0331 0.262 Uiso 1 1 calc R . . H28B H 0.8610 0.6693 1.0015 0.262 Uiso 1 1 calc R . . H28C H 0.8452 0.4931 0.9975 0.262 Uiso 1 1 calc R . . C29 C 0.6160(14) 0.8044(11) 0.9529(5) 0.116(4) Uani 1 1 d . . . H29A H 0.6339 0.8486 0.9179 0.174 Uiso 1 1 calc R . . H29B H 0.6669 0.8571 0.9771 0.174 Uiso 1 1 calc R . . H29C H 0.5032 0.8172 0.9603 0.174 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 Ni1 0.0186(4) 0.0219(4) 0.0183(3) 0.0014(2) 0.0035(3) -0.0067(3) Pd1 0.0294(4) 0.0365(4) 0.0151(3) 0.0009(2) 0.0049(2) -0.0055(3) S2 0.0361(9) 0.0401(9) 0.0189(6) 0.0022(6) 0.0051(6) 0.0035(8) S1 0.0346(9) 0.0413(9) 0.0189(6) -0.0005(6) 0.0053(6) 0.0049(8) N1 0.019(3) 0.021(2) 0.024(2) -0.0001(17) -0.0007(17) -0.004(2) N2 0.021(3) 0.021(2) 0.025(2) -0.0026(18) 0.0055(18) -0.001(2) N3 0.028(3) 0.028(3) 0.020(2) 0.0033(18) 0.0057(18) -0.003(2) N4 0.021(3) 0.027(2) 0.027(2) -0.0005(18) 0.0053(18) -0.012(2) N5 0.031(3) 0.026(2) 0.0179(19) 0.0037(17) 0.0035(18) -0.009(2) N6 0.019(2) 0.024(2) 0.030(2) -0.0017(18) 0.0004(18) -0.006(2) C1 0.021(3) 0.026(3) 0.026(3) -0.001(2) 0.005(2) -0.006(3) C2 0.017(3) 0.026(3) 0.018(2) -0.002(2) 0.0051(19) -0.004(2) C3 0.023(3) 0.019(3) 0.020(2) 0.0007(19) 0.003(2) -0.008(3) C4 0.023(3) 0.025(3) 0.024(2) -0.002(2) 0.009(2) -0.004(3) C5 0.022(3) 0.027(3) 0.035(3) 0.001(2) 0.008(2) 0.001(3) C6 0.029(3) 0.023(3) 0.027(3) 0.006(2) 0.003(2) -0.003(3) C7 0.019(3) 0.022(3) 0.024(2) -0.003(2) 0.004(2) -0.009(3) C8 0.017(3) 0.020(3) 0.021(2) 0.000(2) 0.000(2) -0.003(2) C9 0.029(3) 0.031(3) 0.021(2) 0.006(2) 0.005(2) -0.005(3) C10 0.026(3) 0.027(3) 0.028(3) 0.002(2) 0.003(2) 0.001(3) C11 0.024(3) 0.030(3) 0.031(3) -0.005(2) 0.011(2) 0.002(3) C12 0.013(3) 0.021(3) 0.016(2) 0.0003(18) 0.0004(18) -0.006(2) C13 0.027(3) 0.038(3) 0.028(3) 0.002(2) -0.004(2) 0.002(3) C14 0.026(3) 0.046(4) 0.031(3) -0.004(3) -0.001(2) -0.015(3) C15 0.035(4) 0.026(3) 0.040(3) -0.007(2) 0.007(3) -0.013(3) C16 0.028(3) 0.034(3) 0.032(3) -0.009(2) 0.004(2) -0.008(3) C17 0.021(3) 0.034(3) 0.040(3) 0.001(3) 0.014(2) -0.003(3) C18 0.014(3) 0.036(3) 0.035(3) 0.003(2) 0.005(2) -0.008(3) C19 0.039(4) 0.024(3) 0.044(3) 0.006(2) 0.007(3) -0.011(3) C20 0.041(4) 0.025(3) 0.035(3) 0.007(2) 0.010(3) -0.003(3) B1 0.037(4) 0.045(4) 0.026(3) 0.000(3) 0.007(3) -0.015(4) F1 0.047(3) 0.101(4) 0.071(3) 0.004(3) -0.003(2) 0.010(3) F2 0.108(4) 0.063(3) 0.120(4) -0.043(3) 0.059(3) -0.045(3) F3 0.067(3) 0.058(3) 0.055(2) 0.023(2) 0.019(2) 0.010(2) F4 0.056(3) 0.070(3) 0.053(2) -0.009(2) 0.030(2) -0.006(2) O1 0.060(3) 0.055(3) 0.041(3) -0.006(2) -0.002(2) -0.021(3) N7 0.039(3) 0.039(3) 0.047(3) -0.001(2) -0.007(3) -0.014(3) C21 0.032(4) 0.041(4) 0.055(4) -0.010(3) -0.001(3) -0.016(3) C22 0.063(5) 0.062(5) 0.070(5) 0.015(4) -0.018(4) -0.026(5) C23 0.074(6) 0.057(5) 0.039(4) -0.007(3) -0.002(4) -0.015(4) O2 0.039(3) 0.058(3) 0.053(3) 0.002(2) 0.004(2) -0.020(2) N8 0.037(3) 0.041(3) 0.043(3) -0.003(2) 0.006(2) -0.017(3) C24 0.026(4) 0.047(4) 0.054(4) -0.006(3) 0.012(3) -0.025(3) C25 0.075(6) 0.053(5) 0.043(4) -0.003(3) 0.006(4) -0.026(4) C26 0.051(4) 0.038(4) 0.051(4) -0.007(3) 0.008(3) -0.020(3) O3 0.098(5) 0.089(5) 0.080(4) -0.001(4) -0.034(4) -0.026(4) N9 0.076(5) 0.050(4) 0.049(3) -0.002(3) -0.014(3) -0.005(4) C27 0.111(9) 0.074(7) 0.078(6) -0.005(5) -0.018(6) -0.029(6) C28 0.236(18) 0.118(11) 0.155(13) -0.003(10) -0.109(13) 0.030(12) C29 0.105(9) 0.063(7) 0.180(12) -0.032(8) -0.040(9) 0.002(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 Ni1 N3 2.091(4) . ? Ni1 N5 2.091(4) . ? Ni1 N6 2.114(4) . ? Ni1 N4 2.118(4) . ? Ni1 N2 2.211(4) . ? Ni1 N1 2.213(4) . ? Pd1 S1 2.3249(14) 2 ? Pd1 S1 2.3249(14) . ? Pd1 S2 2.3253(14) 2 ? Pd1 S2 2.3253(14) . ? S2 C1 1.723(6) . ? S1 C1 1.734(5) . ? N1 C7 1.323(6) . ? N1 C6 1.349(7) . ? N2 C11 1.339(7) . ? N2 C12 1.361(6) . ? N3 C13 1.470(7) . ? N3 C20 1.480(7) . ? N3 H3 0.9100 . ? N4 C15 1.476(7) . ? N4 C14 1.481(7) . ? N4 H4A 0.9100 . ? N5 C16 1.468(7) . ? N5 C17 1.482(7) . ? N5 H5A 0.9100 . ? N6 C18 1.486(7) . ? N6 C19 1.491(7) . ? N6 H6A 0.9100 . ? C1 C2 1.397(7) . ? C2 C3 1.465(7) . ? C2 C8 1.467(7) . ? C3 C4 1.404(8) . ? C3 C7 1.420(6) . ? C4 C5 1.374(7) . ? C4 H4 0.9300 . ? C5 C6 1.394(7) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C7 C12 1.428(7) . ? C8 C9 1.383(7) . ? C8 C12 1.417(6) . ? C9 C10 1.395(7) . ? C9 H9 0.9300 . ? C10 C11 1.393(7) . ? C10 H10 0.9300 . ? C11 H11 0.9300 . ? C13 C14 1.533(8) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 C16 1.526(8) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 C18 1.523(8) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 C20 1.501(8) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? B1 F3 1.354(8) . ? B1 F2 1.355(8) . ? B1 F4 1.390(7) . ? B1 F1 1.404(9) . ? O1 C21 1.226(8) . ? N7 C21 1.339(8) . ? N7 C23 1.420(9) . ? N7 C22 1.447(8) . ? C21 H21 0.9300 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? O2 C24 1.223(7) . ? N8 C24 1.325(8) . ? N8 C26 1.449(8) . ? N8 C25 1.472(8) . ? C24 H24 0.9300 . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? O3 C27 1.182(10) . ? N9 C27 1.315(11) . ? N9 C29 1.403(10) . ? N9 C28 1.446(13) . ? C27 H27 0.9300 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? 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 N3 Ni1 N5 102.12(16) . . ? N3 Ni1 N6 82.70(17) . . ? N5 Ni1 N6 83.12(17) . . ? N3 Ni1 N4 82.77(17) . . ? N5 Ni1 N4 82.47(17) . . ? N6 Ni1 N4 156.88(16) . . ? N3 Ni1 N2 169.81(16) . . ? N5 Ni1 N2 88.01(16) . . ? N6 Ni1 N2 97.61(16) . . ? N4 Ni1 N2 99.86(16) . . ? N3 Ni1 N1 88.19(16) . . ? N5 Ni1 N1 169.41(16) . . ? N6 Ni1 N1 100.83(16) . . ? N4 Ni1 N1 96.58(16) . . ? N2 Ni1 N1 81.75(15) . . ? S1 Pd1 S1 180.00(8) 2 . ? S1 Pd1 S2 74.71(5) 2 2 ? S1 Pd1 S2 105.29(5) . 2 ? S1 Pd1 S2 105.29(5) 2 . ? S1 Pd1 S2 74.71(5) . . ? S2 Pd1 S2 180.00(8) 2 . ? C1 S2 Pd1 88.02(18) . . ? C1 S1 Pd1 87.77(18) . . ? C7 N1 C6 114.2(4) . . ? C7 N1 Ni1 106.5(3) . . ? C6 N1 Ni1 139.3(3) . . ? C11 N2 C12 114.1(4) . . ? C11 N2 Ni1 140.4(3) . . ? C12 N2 Ni1 105.4(3) . . ? C13 N3 C20 116.5(4) . . ? C13 N3 Ni1 110.8(3) . . ? C20 N3 Ni1 110.5(3) . . ? C13 N3 H3 106.1 . . ? C20 N3 H3 106.1 . . ? Ni1 N3 H3 106.1 . . ? C15 N4 C14 114.7(4) . . ? C15 N4 Ni1 107.8(3) . . ? C14 N4 Ni1 108.1(3) . . ? C15 N4 H4A 108.7 . . ? C14 N4 H4A 108.7 . . ? Ni1 N4 H4A 108.7 . . ? C16 N5 C17 116.8(4) . . ? C16 N5 Ni1 110.9(3) . . ? C17 N5 Ni1 110.1(3) . . ? C16 N5 H5A 106.1 . . ? C17 N5 H5A 106.1 . . ? Ni1 N5 H5A 106.1 . . ? C18 N6 C19 114.2(4) . . ? C18 N6 Ni1 108.0(3) . . ? C19 N6 Ni1 107.7(3) . . ? C18 N6 H6A 108.9 . . ? C19 N6 H6A 108.9 . . ? Ni1 N6 H6A 108.9 . . ? C2 C1 S2 125.7(4) . . ? C2 C1 S1 124.9(4) . . ? S2 C1 S1 109.4(3) . . ? C1 C2 C3 127.7(5) . . ? C1 C2 C8 126.1(5) . . ? C3 C2 C8 106.2(4) . . ? C4 C3 C7 114.9(4) . . ? C4 C3 C2 136.5(4) . . ? C7 C3 C2 108.5(4) . . ? C5 C4 C3 117.6(4) . . ? C5 C4 H4 121.2 . . ? C3 C4 H4 121.2 . . ? C4 C5 C6 122.0(5) . . ? C4 C5 H5 119.0 . . ? C6 C5 H5 119.0 . . ? N1 C6 C5 122.5(5) . . ? N1 C6 H6 118.7 . . ? C5 C6 H6 118.7 . . ? N1 C7 C3 128.7(5) . . ? N1 C7 C12 123.3(4) . . ? C3 C7 C12 108.0(4) . . ? C9 C8 C12 116.0(4) . . ? C9 C8 C2 136.4(4) . . ? C12 C8 C2 107.5(4) . . ? C8 C9 C10 118.1(5) . . ? C8 C9 H9 121.0 . . ? C10 C9 H9 121.0 . . ? C11 C10 C9 121.2(5) . . ? C11 C10 H10 119.4 . . ? C9 C10 H10 119.4 . . ? N2 C11 C10 123.3(5) . . ? N2 C11 H11 118.4 . . ? C10 C11 H11 118.4 . . ? N2 C12 C8 127.3(5) . . ? N2 C12 C7 123.0(4) . . ? C8 C12 C7 109.7(4) . . ? N3 C13 C14 107.6(4) . . ? N3 C13 H13A 110.2 . . ? C14 C13 H13A 110.2 . . ? N3 C13 H13B 110.2 . . ? C14 C13 H13B 110.2 . . ? H13A C13 H13B 108.5 . . ? N4 C14 C13 112.4(5) . . ? N4 C14 H14A 109.1 . . ? C13 C14 H14A 109.1 . . ? N4 C14 H14B 109.1 . . ? C13 C14 H14B 109.1 . . ? H14A C14 H14B 107.8 . . ? N4 C15 C16 111.8(4) . . ? N4 C15 H15A 109.2 . . ? C16 C15 H15A 109.2 . . ? N4 C15 H15B 109.2 . . ? C16 C15 H15B 109.2 . . ? H15A C15 H15B 107.9 . . ? N5 C16 C15 107.6(4) . . ? N5 C16 H16A 110.2 . . ? C15 C16 H16A 110.2 . . ? N5 C16 H16B 110.2 . . ? C15 C16 H16B 110.2 . . ? H16A C16 H16B 108.5 . . ? N5 C17 C18 108.0(4) . . ? N5 C17 H17A 110.1 . . ? C18 C17 H17A 110.1 . . ? N5 C17 H17B 110.1 . . ? C18 C17 H17B 110.1 . . ? H17A C17 H17B 108.4 . . ? N6 C18 C17 112.2(4) . . ? N6 C18 H18A 109.2 . . ? C17 C18 H18A 109.2 . . ? N6 C18 H18B 109.2 . . ? C17 C18 H18B 109.2 . . ? H18A C18 H18B 107.9 . . ? N6 C19 C20 112.2(5) . . ? N6 C19 H19A 109.2 . . ? C20 C19 H19A 109.2 . . ? N6 C19 H19B 109.2 . . ? C20 C19 H19B 109.2 . . ? H19A C19 H19B 107.9 . . ? N3 C20 C19 108.3(4) . . ? N3 C20 H20A 110.0 . . ? C19 C20 H20A 110.0 . . ? N3 C20 H20B 110.0 . . ? C19 C20 H20B 110.0 . . ? H20A C20 H20B 108.4 . . ? F3 B1 F2 112.1(6) . . ? F3 B1 F4 110.5(6) . . ? F2 B1 F4 109.8(5) . . ? F3 B1 F1 108.6(6) . . ? F2 B1 F1 105.1(6) . . ? F4 B1 F1 110.6(5) . . ? C21 N7 C23 120.8(6) . . ? C21 N7 C22 121.1(6) . . ? C23 N7 C22 118.0(6) . . ? O1 C21 N7 126.0(7) . . ? O1 C21 H21 117.0 . . ? N7 C21 H21 117.0 . . ? N7 C22 H22A 109.5 . . ? N7 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? N7 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? N7 C23 H23A 109.5 . . ? N7 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? N7 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C24 N8 C26 120.0(5) . . ? C24 N8 C25 121.0(6) . . ? C26 N8 C25 119.0(6) . . ? O2 C24 N8 126.3(6) . . ? O2 C24 H24 116.8 . . ? N8 C24 H24 116.8 . . ? N8 C25 H25A 109.5 . . ? N8 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? N8 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? N8 C26 H26A 109.5 . . ? N8 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? N8 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C27 N9 C29 124.1(8) . . ? C27 N9 C28 121.9(9) . . ? C29 N9 C28 113.9(9) . . ? O3 C27 N9 129.1(10) . . ? O3 C27 H27 115.4 . . ? N9 C27 H27 115.4 . . ? N9 C28 H28A 109.5 . . ? N9 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? N9 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? N9 C29 H29A 109.5 . . ? N9 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? N9 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.98 _diffrn_reflns_theta_full 27.19 _diffrn_measured_fraction_theta_full 0.98 _refine_diff_density_max 1.903 _refine_diff_density_min -1.094 _refine_diff_density_rms 0.139 ###Material relevant to compound 8 at 173K ######## data_e484a _database_code_depnum_ccdc_archive 'CCDC 621046' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C34 H42 N4 Na2 Ni O5 S9' _chemical_formula_sum 'C34 H42 N4 Na2 Ni O5 S9' _chemical_formula_weight 979.95 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' Na Na 0.0362 0.0249 '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' Ni Ni 0.3393 1.1124 '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 15.4567(4) _cell_length_b 13.0732(4) _cell_length_c 22.4156(6) _cell_angle_alpha 90.00 _cell_angle_beta 106.5800(10) _cell_angle_gamma 90.00 _cell_volume 4341.2(2) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 8360 _cell_measurement_theta_min 2.75 _cell_measurement_theta_max 27.42 _exptl_crystal_description rod _exptl_crystal_colour purple _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.499 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2032 _exptl_absorpt_coefficient_mu 0.944 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8264 _exptl_absorpt_correction_T_max 0.9368 _exptl_absorpt_process_details sadabs _exptl_special_details ; The large C Ueqmax/min results from the high thermal agitation of the carbon atoms of the DMSO molecules. As a consequence, a high H Ueq max/min is observed. Note that the hydrogen atoms on C17 have been introduced owing to the fact that it is shared between S5 and its symmetry equivalent. However the corresponding H atoms have been taken into account in the final 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 24593 _diffrn_reflns_av_R_equivalents 0.0379 _diffrn_reflns_av_sigmaI/netI 0.0324 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 2.08 _diffrn_reflns_theta_max 27.50 _reflns_number_total 4972 _reflns_number_gt 4008 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _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^)+(0.0900P)^2^+19.7943P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4972 _refine_ls_number_parameters 253 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0686 _refine_ls_R_factor_gt 0.0538 _refine_ls_wR_factor_ref 0.1704 _refine_ls_wR_factor_gt 0.1550 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.049 _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 Ni1 Ni 0.0000 0.0000 0.0000 0.02306(18) Uani 1 2 d S . . Na1 Na -0.43494(9) -0.08935(11) 0.20655(7) 0.0300(3) Uani 1 1 d . . . S1 S -0.10533(6) 0.08654(7) 0.02589(4) 0.0300(2) Uani 1 1 d . . . S2 S -0.01690(6) -0.09172(7) 0.07869(4) 0.0264(2) Uani 1 1 d . . . N1 N -0.36284(18) 0.0484(2) 0.16357(13) 0.0243(6) Uani 1 1 d . . . N2 N -0.26936(19) -0.1467(2) 0.22075(13) 0.0263(6) Uani 1 1 d . . . C1 C -0.1047(2) -0.0092(2) 0.08002(15) 0.0214(6) Uani 1 1 d . . . C2 C -0.1639(2) -0.0183(2) 0.11548(15) 0.0213(6) Uani 1 1 d . . . C3 C -0.2401(2) 0.0491(3) 0.11440(15) 0.0213(6) Uani 1 1 d . . . C4 C -0.2748(2) 0.1376(3) 0.08187(17) 0.0277(7) Uani 1 1 d . . . H4 H -0.2465 0.1682 0.0550 0.033 Uiso 1 1 calc R . . C5 C -0.3531(3) 0.1789(3) 0.09063(17) 0.0309(8) Uani 1 1 d . . . H5 H -0.3780 0.2379 0.0694 0.037 Uiso 1 1 calc R . . C6 C -0.3944(2) 0.1323(3) 0.13103(16) 0.0282(7) Uani 1 1 d . . . H6 H -0.4470 0.1614 0.1356 0.034 Uiso 1 1 calc R . . C7 C -0.2875(2) 0.0089(2) 0.15457(15) 0.0210(6) Uani 1 1 d . . . C8 C -0.1671(2) -0.1006(3) 0.15890(15) 0.0212(6) Uani 1 1 d . . . C9 C -0.1145(2) -0.1878(3) 0.17994(16) 0.0262(7) Uani 1 1 d . . . H9 H -0.0640 -0.2022 0.1668 0.031 Uiso 1 1 calc R . . C10 C -0.1407(2) -0.2520(3) 0.22119(17) 0.0324(8) Uani 1 1 d . . . H10 H -0.1065 -0.3097 0.2367 0.039 Uiso 1 1 calc R . . C11 C -0.2177(2) -0.2304(3) 0.23937(17) 0.0316(8) Uani 1 1 d . . . H11 H -0.2343 -0.2762 0.2658 0.038 Uiso 1 1 calc R . . C12 C -0.2425(2) -0.0848(3) 0.18208(14) 0.0212(6) Uani 1 1 d . . . S3 S -0.45181(8) -0.20084(10) 0.04352(6) 0.0505(3) Uani 1 1 d . . . O1 O -0.4591(3) -0.1518(4) 0.10138(19) 0.0801(13) Uani 1 1 d . . . C13 C -0.3984(6) -0.1143(7) 0.0058(3) 0.1019(18) Uani 1 1 d . . . H13A H -0.4348 -0.0538 -0.0052 0.153 Uiso 1 1 calc R . . H13B H -0.3910 -0.1454 -0.0313 0.153 Uiso 1 1 calc R . . H13C H -0.3404 -0.0963 0.0330 0.153 Uiso 1 1 calc R . . C14 C -0.3604(5) -0.2852(7) 0.0685(4) 0.1019(18) Uani 1 1 d . . . H14A H -0.3091 -0.2489 0.0940 0.153 Uiso 1 1 calc R . . H14B H -0.3460 -0.3134 0.0330 0.153 Uiso 1 1 calc R . . H14C H -0.3762 -0.3395 0.0923 0.153 Uiso 1 1 calc R . . S4 S -0.34661(8) -0.00776(9) 0.36840(5) 0.0454(3) Uani 1 1 d . . . O2 O -0.42062(18) -0.0136(2) 0.30783(13) 0.0364(6) Uani 1 1 d . . . C15 C -0.2440(3) 0.0010(5) 0.3497(3) 0.0638(16) Uani 1 1 d . . . H15A H -0.2410 -0.0522 0.3209 0.096 Uiso 1 1 calc R . . H15B H -0.1947 -0.0063 0.3869 0.096 Uiso 1 1 calc R . . H15C H -0.2402 0.0664 0.3311 0.096 Uiso 1 1 calc R . . C16 C -0.3299(4) -0.1335(6) 0.3968(4) 0.097(3) Uani 1 1 d . . . H16A H -0.3820 -0.1557 0.4084 0.146 Uiso 1 1 calc R . . H16B H -0.2778 -0.1358 0.4325 0.146 Uiso 1 1 calc R . . H16C H -0.3206 -0.1778 0.3650 0.146 Uiso 1 1 calc R . . S5 S -0.46639(12) -0.32613(14) 0.27865(9) 0.0323(4) Uani 0.50 1 d P . . O3 O -0.5000 -0.2260(3) 0.2500 0.0403(9) Uani 1 2 d S . . C17 C -0.4391(3) -0.3981(4) 0.2171(3) 0.0572(13) 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 Ni1 0.0210(3) 0.0277(3) 0.0264(3) 0.0015(2) 0.0163(2) 0.0009(2) Na1 0.0232(7) 0.0349(8) 0.0379(8) 0.0027(6) 0.0185(6) -0.0003(6) S1 0.0313(4) 0.0305(5) 0.0373(5) 0.0101(4) 0.0246(4) 0.0074(3) S2 0.0249(4) 0.0297(5) 0.0311(4) 0.0047(3) 0.0187(3) 0.0064(3) N1 0.0200(13) 0.0298(15) 0.0264(14) -0.0023(12) 0.0121(11) 0.0017(11) N2 0.0247(13) 0.0328(16) 0.0252(14) 0.0049(12) 0.0134(11) 0.0015(12) C1 0.0202(14) 0.0230(16) 0.0245(15) 0.0001(12) 0.0119(12) -0.0001(12) C2 0.0194(14) 0.0228(16) 0.0253(15) 0.0007(12) 0.0119(12) 0.0005(12) C3 0.0205(14) 0.0234(16) 0.0229(15) -0.0028(12) 0.0107(12) 0.0004(12) C4 0.0305(17) 0.0266(18) 0.0320(18) 0.0046(14) 0.0183(14) 0.0033(14) C5 0.0325(18) 0.0296(19) 0.0335(19) 0.0038(15) 0.0139(15) 0.0103(15) C6 0.0225(15) 0.0343(19) 0.0311(18) -0.0027(15) 0.0126(13) 0.0068(14) C7 0.0187(14) 0.0252(17) 0.0214(15) -0.0013(12) 0.0093(12) -0.0008(12) C8 0.0188(14) 0.0264(17) 0.0217(15) -0.0003(12) 0.0113(12) -0.0012(12) C9 0.0231(15) 0.0301(18) 0.0291(17) 0.0039(14) 0.0136(13) 0.0040(13) C10 0.0313(18) 0.034(2) 0.0336(19) 0.0110(15) 0.0121(15) 0.0090(15) C11 0.0318(18) 0.035(2) 0.0328(18) 0.0128(15) 0.0172(15) 0.0033(15) C12 0.0175(14) 0.0271(17) 0.0213(15) -0.0011(12) 0.0093(11) -0.0003(12) S3 0.0525(7) 0.0557(7) 0.0408(6) -0.0047(5) 0.0094(5) -0.0140(5) O1 0.067(2) 0.110(4) 0.065(2) -0.042(2) 0.021(2) -0.022(2) C13 0.096(4) 0.116(5) 0.080(3) -0.017(3) 0.004(3) -0.029(3) C14 0.096(4) 0.116(5) 0.080(3) -0.017(3) 0.004(3) -0.029(3) S4 0.0374(6) 0.0559(7) 0.0407(6) -0.0084(5) 0.0078(4) 0.0016(5) O2 0.0261(13) 0.0502(17) 0.0339(14) 0.0003(12) 0.0099(11) -0.0047(11) C15 0.033(2) 0.100(5) 0.057(3) -0.001(3) 0.012(2) -0.017(3) C16 0.056(3) 0.092(5) 0.114(6) 0.050(4) -0.023(4) -0.018(3) S5 0.0299(9) 0.0294(9) 0.0364(10) -0.0008(7) 0.0076(7) -0.0029(7) O3 0.049(2) 0.030(2) 0.054(2) 0.000 0.034(2) 0.000 C17 0.051(3) 0.052(3) 0.070(3) -0.018(2) 0.020(2) 0.016(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 S1 2.1924(8) . ? Ni1 S1 2.1924(8) 5 ? Ni1 S2 2.2091(8) . ? Ni1 S2 2.2091(8) 5 ? Na1 O2 2.379(3) 2_455 ? Na1 O3 2.390(3) . ? Na1 O1 2.421(4) . ? Na1 O2 2.428(3) . ? Na1 N1 2.455(3) . ? Na1 N2 2.598(3) . ? Na1 C7 3.117(3) . ? Na1 Na1 3.174(3) 2_455 ? S1 C1 1.742(3) . ? S2 C1 1.741(3) . ? N1 C6 1.330(5) . ? N1 C7 1.341(4) . ? N2 C12 1.335(4) . ? N2 C11 1.348(5) . ? C1 C2 1.377(4) . ? C2 C8 1.462(4) . ? C2 C3 1.466(4) . ? C3 C4 1.391(5) . ? C3 C7 1.414(4) . ? C4 C5 1.389(5) . ? C4 H4 0.9300 . ? C5 C6 1.388(5) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C7 C12 1.456(5) . ? C8 C9 1.401(5) . ? C8 C12 1.420(4) . ? C9 C10 1.391(5) . ? C9 H9 0.9300 . ? C10 C11 1.392(5) . ? C10 H10 0.9300 . ? C11 H11 0.9300 . ? S3 O1 1.480(4) . ? S3 C14 1.753(9) . ? S3 C13 1.754(8) . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? S4 O2 1.507(3) . ? S4 C16 1.755(7) . ? S4 C15 1.756(5) . ? O2 Na1 2.379(3) 2_455 ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? S5 S5 1.403(4) 2_455 ? S5 O3 1.485(4) . ? S5 C17 1.763(5) 2_455 ? S5 C17 1.816(5) . ? O3 S5 1.485(4) 2_455 ? O3 Na1 2.390(3) 2_455 ? C17 S5 1.763(5) 2_455 ? 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 S1 Ni1 S1 180.00(6) . 5 ? S1 Ni1 S2 78.63(3) . . ? S1 Ni1 S2 101.37(3) 5 . ? S1 Ni1 S2 101.37(3) . 5 ? S1 Ni1 S2 78.63(3) 5 5 ? S2 Ni1 S2 180.00(6) . 5 ? O2 Na1 O3 83.01(9) 2_455 . ? O2 Na1 O1 97.48(14) 2_455 . ? O3 Na1 O1 100.30(14) . . ? O2 Na1 O2 77.80(12) 2_455 . ? O3 Na1 O2 81.97(9) . . ? O1 Na1 O2 174.54(16) . . ? O2 Na1 N1 98.93(11) 2_455 . ? O3 Na1 N1 177.99(10) . . ? O1 Na1 N1 80.01(14) . . ? O2 Na1 N1 97.90(11) . . ? O2 Na1 N2 172.12(12) 2_455 . ? O3 Na1 N2 104.39(9) . . ? O1 Na1 N2 83.97(13) . . ? O2 Na1 N2 100.33(10) . . ? N1 Na1 N2 73.64(10) . . ? O2 Na1 C7 122.41(11) 2_455 . ? O3 Na1 C7 153.89(10) . . ? O1 Na1 C7 72.61(12) . . ? O2 Na1 C7 107.47(10) . . ? N1 Na1 C7 24.34(9) . . ? N2 Na1 C7 50.58(9) . . ? O2 Na1 Na1 49.35(8) 2_455 2_455 ? O3 Na1 Na1 48.38(7) . 2_455 ? O1 Na1 Na1 130.45(12) . 2_455 ? O2 Na1 Na1 48.00(7) . 2_455 ? N1 Na1 Na1 132.76(7) . 2_455 ? N2 Na1 Na1 134.38(9) . 2_455 ? C7 Na1 Na1 152.66(7) . 2_455 ? C1 S1 Ni1 87.52(11) . . ? C1 S2 Ni1 87.01(11) . . ? C6 N1 C7 115.7(3) . . ? C6 N1 Na1 133.1(2) . . ? C7 N1 Na1 106.7(2) . . ? C12 N2 C11 115.2(3) . . ? C12 N2 Na1 102.9(2) . . ? C11 N2 Na1 138.4(2) . . ? C2 C1 S2 127.3(3) . . ? C2 C1 S1 126.3(3) . . ? S2 C1 S1 106.42(17) . . ? C1 C2 C8 127.1(3) . . ? C1 C2 C3 127.0(3) . . ? C8 C2 C3 105.9(3) . . ? C4 C3 C7 116.8(3) . . ? C4 C3 C2 134.2(3) . . ? C7 C3 C2 109.0(3) . . ? C5 C4 C3 118.1(3) . . ? C5 C4 H4 121.0 . . ? C3 C4 H4 121.0 . . ? C6 C5 C4 120.1(3) . . ? C6 C5 H5 119.9 . . ? C4 C5 H5 119.9 . . ? N1 C6 C5 123.7(3) . . ? N1 C6 H6 118.1 . . ? C5 C6 H6 118.1 . . ? N1 C7 C3 125.6(3) . . ? N1 C7 C12 126.2(3) . . ? C3 C7 C12 108.1(3) . . ? N1 C7 Na1 48.98(17) . . ? C3 C7 Na1 163.3(2) . . ? C12 C7 Na1 78.84(18) . . ? C9 C8 C12 116.9(3) . . ? C9 C8 C2 134.1(3) . . ? C12 C8 C2 108.9(3) . . ? C10 C9 C8 117.6(3) . . ? C10 C9 H9 121.2 . . ? C8 C9 H9 121.2 . . ? C9 C10 C11 120.4(3) . . ? C9 C10 H10 119.8 . . ? C11 C10 H10 119.8 . . ? N2 C11 C10 123.7(3) . . ? N2 C11 H11 118.2 . . ? C10 C11 H11 118.2 . . ? N2 C12 C8 126.1(3) . . ? N2 C12 C7 125.9(3) . . ? C8 C12 C7 108.0(3) . . ? O1 S3 C14 104.4(3) . . ? O1 S3 C13 107.9(3) . . ? C14 S3 C13 96.5(4) . . ? S3 O1 Na1 166.0(3) . . ? S3 C13 H13A 109.5 . . ? S3 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? S3 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? S3 C14 H14A 109.5 . . ? S3 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? S3 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? O2 S4 C16 105.9(3) . . ? O2 S4 C15 107.0(2) . . ? C16 S4 C15 95.6(3) . . ? S4 O2 Na1 125.81(17) . 2_455 ? S4 O2 Na1 134.94(17) . . ? Na1 O2 Na1 82.65(10) 2_455 . ? S4 C15 H15A 109.5 . . ? S4 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? S4 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? S4 C16 H16A 109.5 . . ? S4 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? S4 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? S5 S5 O3 61.82(10) 2_455 . ? S5 S5 C17 68.9(2) 2_455 2_455 ? O3 S5 C17 107.5(2) . 2_455 ? S5 S5 C17 64.9(2) 2_455 . ? O3 S5 C17 104.9(2) . . ? C17 S5 C17 98.0(4) 2_455 . ? S5 O3 S5 56.4(2) 2_455 . ? S5 O3 Na1 128.22(8) 2_455 . ? S5 O3 Na1 134.36(8) . . ? S5 O3 Na1 134.36(8) 2_455 2_455 ? S5 O3 Na1 128.22(8) . 2_455 ? Na1 O3 Na1 83.24(14) . 2_455 ? S5 C17 S5 46.13(16) 2_455 . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.845 _refine_diff_density_min -0.886 _refine_diff_density_rms 0.116 ###Material relevant to compound 9 at 173K ######## data_e494a _database_code_depnum_ccdc_archive 'CCDC 621047' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C34 H42 N4 Na2 O5 Pd S9' _chemical_formula_sum 'C34 H42 N4 Na2 O5 Pd S9' _chemical_formula_weight 1027.64 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' Na Na 0.0362 0.0249 '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' Pd Pd -0.9988 1.0072 '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 15.3267(5) _cell_length_b 12.8644(5) _cell_length_c 22.9486(10) _cell_angle_alpha 90.00 _cell_angle_beta 107.9490(10) _cell_angle_gamma 90.00 _cell_volume 4304.5(3) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 6863 _cell_measurement_theta_min 2.48 _cell_measurement_theta_max 29.90 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.586 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2104 _exptl_absorpt_coefficient_mu 0.933 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8141 _exptl_absorpt_correction_T_max 0.8727 _exptl_absorpt_process_details sadabs _exptl_special_details ; The large C Ueqmax/min results from the high thermal agitation of the carbon atoms of the DMSO molecules. As a consequence, a high H Ueq max/min is observed. ; _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 22627 _diffrn_reflns_av_R_equivalents 0.0307 _diffrn_reflns_av_sigmaI/netI 0.0318 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 1.87 _diffrn_reflns_theta_max 30.08 _reflns_number_total 6318 _reflns_number_gt 4945 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _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^)+(0.1226P)^2^+19.7744P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6318 _refine_ls_number_parameters 265 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0770 _refine_ls_R_factor_gt 0.0603 _refine_ls_wR_factor_ref 0.2041 _refine_ls_wR_factor_gt 0.1840 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.059 _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 C1 C -0.1096(3) -0.0048(3) 0.08111(18) 0.0262(7) Uani 1 1 d . . . C2 C -0.1680(3) -0.0110(3) 0.11607(18) 0.0263(7) Uani 1 1 d . . . C3 C -0.2442(3) 0.0588(3) 0.11401(17) 0.0275(7) Uani 1 1 d . . . C4 C -0.2806(3) 0.1483(3) 0.0803(2) 0.0400(10) Uani 1 1 d . . . H4 H -0.2538 0.1771 0.0528 0.048 Uiso 1 1 calc R . . C5 C -0.3580(3) 0.1924(3) 0.0895(2) 0.0405(10) Uani 1 1 d . . . H5 H -0.3823 0.2531 0.0689 0.049 Uiso 1 1 calc R . . C6 C -0.3994(3) 0.1472(3) 0.12888(19) 0.0342(8) Uani 1 1 d . . . H6 H -0.4527 0.1771 0.1324 0.041 Uiso 1 1 calc R . . C7 C -0.2913(3) 0.0212(3) 0.15353(16) 0.0247(6) Uani 1 1 d . . . C8 C -0.1701(2) -0.0919(3) 0.16007(16) 0.0250(6) Uani 1 1 d . . . C9 C -0.1167(3) -0.1793(3) 0.18272(18) 0.0309(8) Uani 1 1 d . . . H9 H -0.0661 -0.1954 0.1702 0.037 Uiso 1 1 calc R . . C10 C -0.1411(3) -0.2418(3) 0.2245(2) 0.0380(9) Uani 1 1 d . . . H10 H -0.1063 -0.3002 0.2407 0.046 Uiso 1 1 calc R . . C11 C -0.2178(3) -0.2167(3) 0.2419(2) 0.0385(9) Uani 1 1 d . . . H11 H -0.2335 -0.2610 0.2691 0.046 Uiso 1 1 calc R . . C12 C -0.2446(2) -0.0730(3) 0.18258(16) 0.0250(6) Uani 1 1 d . . . C13 C -0.3645(8) -0.2736(7) 0.0711(4) 0.1078(8) Uani 1 1 d . . . H13A H -0.3143 -0.2376 0.0994 0.162 Uiso 1 1 calc R . . H13B H -0.3469 -0.2957 0.0363 0.162 Uiso 1 1 calc R . . H13C H -0.3804 -0.3333 0.0909 0.162 Uiso 1 1 calc R . . C14 C -0.4038(8) -0.1066(8) 0.0074(4) 0.1078(8) Uani 1 1 d . . . H14A H -0.4009 -0.1398 -0.0295 0.162 Uiso 1 1 calc R . . H14B H -0.3428 -0.0912 0.0331 0.162 Uiso 1 1 calc R . . H14C H -0.4382 -0.0433 -0.0028 0.162 Uiso 1 1 calc R . . C15 C -0.2380(5) 0.0130(8) 0.3533(5) 0.091(2) Uani 0.90 1 d PD . . C16 C -0.3259(7) -0.1262(10) 0.3927(6) 0.091(2) Uani 0.70 1 d PD . . C16A C -0.3439(15) 0.034(2) 0.4173(9) 0.071(6) Uani 0.30 1 d PD . . C16B C -0.299(2) -0.121(3) 0.3706(15) 0.022(6) Uiso 0.10 1 d P . . C17 C -0.4422(5) -0.3890(5) 0.2164(3) 0.0646(16) Uani 1 1 d . . . N1 N -0.3664(2) 0.0624(3) 0.16217(14) 0.0279(6) Uani 1 1 d . . . N2 N -0.2705(2) -0.1332(3) 0.22204(15) 0.0324(7) Uani 1 1 d . . . O1 O -0.4647(5) -0.1478(5) 0.1052(3) 0.1078(8) Uani 1 1 d . . . O2 O -0.4175(3) 0.0006(3) 0.30798(18) 0.0467(9) Uani 1 1 d . . . O3 O -0.5000 -0.2145(4) 0.2500 0.0523(13) Uani 1 2 d S . . Na1 Na -0.43564(11) -0.07471(14) 0.20844(9) 0.0391(4) Uani 1 1 d . . . S1 S -0.11039(8) 0.09244(8) 0.02809(5) 0.0349(2) Uani 1 1 d . . . S2 S -0.02324(7) -0.09261(7) 0.08108(5) 0.0311(2) Uani 1 1 d . . . S3 S -0.4583(2) -0.1912(2) 0.04698(12) 0.1078(8) Uani 1 1 d . . . S4 S -0.53526(16) -0.31601(17) 0.22338(11) 0.0396(5) Uani 0.50 1 d P . . S5 S -0.34401(15) 0.00654(19) 0.36958(12) 0.0460(4) Uani 0.70 1 d PD . . S6 S -0.3325(4) -0.0539(7) 0.3606(4) 0.0499(15) Uani 0.20 1 d PD . . S7 S -0.3252(9) 0.0120(12) 0.3442(6) 0.042(3) Uani 0.10 1 d P . . Pd1 Pd 0.0000 0.0000 0.0000 0.02590(14) 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 C1 0.0285(17) 0.0266(16) 0.0292(17) 0.0023(12) 0.0172(14) 0.0038(13) C2 0.0287(17) 0.0259(16) 0.0305(17) 0.0034(12) 0.0180(14) 0.0041(13) C3 0.0307(17) 0.0278(16) 0.0307(17) 0.0019(13) 0.0192(14) 0.0047(14) C4 0.052(3) 0.036(2) 0.046(2) 0.0136(17) 0.035(2) 0.0159(19) C5 0.046(2) 0.038(2) 0.046(2) 0.0133(18) 0.027(2) 0.0207(18) C6 0.0331(19) 0.0352(19) 0.040(2) 0.0003(16) 0.0192(16) 0.0093(16) C7 0.0250(16) 0.0281(15) 0.0241(15) 0.0003(12) 0.0120(13) 0.0003(13) C8 0.0261(16) 0.0281(15) 0.0252(15) 0.0014(12) 0.0143(13) 0.0014(13) C9 0.0280(17) 0.0349(18) 0.0352(19) 0.0056(15) 0.0179(15) 0.0085(15) C10 0.038(2) 0.041(2) 0.041(2) 0.0158(17) 0.0203(17) 0.0123(17) C11 0.041(2) 0.041(2) 0.041(2) 0.0166(17) 0.0235(18) 0.0073(18) C12 0.0217(15) 0.0302(16) 0.0268(16) 0.0024(12) 0.0132(13) 0.0024(13) C13 0.1320(19) 0.0950(14) 0.0831(13) -0.0099(10) 0.0136(12) -0.0421(13) C14 0.1320(19) 0.0950(14) 0.0831(13) -0.0099(10) 0.0136(12) -0.0421(13) C15 0.042(3) 0.125(6) 0.093(5) 0.029(4) 0.003(3) -0.009(3) C16 0.042(3) 0.125(6) 0.093(5) 0.029(4) 0.003(3) -0.009(3) C16A 0.050(11) 0.120(18) 0.039(9) -0.023(11) 0.008(8) 0.016(12) C17 0.067(4) 0.053(3) 0.081(4) -0.016(3) 0.032(3) 0.017(3) N1 0.0270(15) 0.0329(15) 0.0285(14) -0.0006(12) 0.0154(12) 0.0033(12) N2 0.0275(15) 0.0411(17) 0.0349(17) 0.0100(13) 0.0191(13) 0.0058(13) O1 0.1320(19) 0.0950(14) 0.0831(13) -0.0099(10) 0.0136(12) -0.0421(13) O2 0.0329(17) 0.063(2) 0.0461(19) -0.0003(14) 0.0146(14) -0.0064(14) O3 0.061(3) 0.036(2) 0.078(4) 0.000 0.047(3) 0.000 Na1 0.0287(8) 0.0386(9) 0.0566(11) 0.0068(7) 0.0231(8) 0.0009(7) S1 0.0416(5) 0.0335(5) 0.0418(5) 0.0123(4) 0.0309(4) 0.0112(4) S2 0.0346(5) 0.0319(4) 0.0361(5) 0.0071(3) 0.0247(4) 0.0102(4) S3 0.1320(19) 0.0950(14) 0.0831(13) -0.0099(10) 0.0136(12) -0.0421(13) S4 0.0364(10) 0.0361(10) 0.0453(12) 0.0011(8) 0.0110(9) 0.0048(8) S5 0.0392(10) 0.0524(13) 0.0446(11) -0.0078(8) 0.0102(9) -0.0016(8) S6 0.029(3) 0.057(4) 0.059(4) 0.018(4) 0.007(3) 0.001(3) S7 0.039(6) 0.065(10) 0.029(5) -0.010(5) 0.021(5) -0.004(5) Pd1 0.0270(2) 0.0288(2) 0.0290(2) 0.00214(13) 0.01912(16) 0.00241(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 C1 C2 1.376(5) . ? C1 S2 1.741(4) . ? C1 S1 1.742(4) . ? C2 C8 1.458(5) . ? C2 C3 1.462(5) . ? C3 C4 1.403(5) . ? C3 C7 1.407(5) . ? C4 C5 1.388(6) . ? C4 H4 0.9300 . ? C5 C6 1.381(6) . ? C5 H5 0.9300 . ? C6 N1 1.338(5) . ? C6 H6 0.9300 . ? C7 N1 1.336(5) . ? C7 C12 1.459(5) . ? C7 Na1 3.118(4) . ? C8 C9 1.393(5) . ? C8 C12 1.413(5) . ? C9 C10 1.386(5) . ? C9 H9 0.9300 . ? C10 C11 1.392(6) . ? C10 H10 0.9300 . ? C11 N2 1.337(5) . ? C11 H11 0.9300 . ? C12 N2 1.341(5) . ? C13 S3 1.734(11) . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 S3 1.783(10) . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 S7 1.288(16) . ? C15 S6 1.737(10) . ? C15 S5 1.778(9) . ? C16 S6 1.170(13) . ? C16 S5 1.784(12) . ? C16 S7 2.099(19) . ? C16A S5 1.148(16) . ? C16A S6 1.769(15) . ? C16A S7 1.81(2) . ? C16B S6 1.00(3) . ? C16B S5 1.78(3) . ? C16B S7 1.82(4) . ? C17 S4 1.756(6) . ? C17 S4 1.791(6) 2_455 ? N1 Na1 2.462(4) . ? N2 Na1 2.566(4) . ? O1 S3 1.479(7) . ? O1 Na1 2.459(6) . ? O2 S7 1.410(14) . ? O2 S5 1.514(4) . ? O2 S6 1.637(8) . ? O2 Na1 2.372(4) 2_455 ? O2 Na1 2.417(4) . ? O3 S4 1.472(5) . ? O3 S4 1.472(5) 2_455 ? O3 Na1 2.386(4) 2_455 ? O3 Na1 2.386(4) . ? Na1 O2 2.372(4) 2_455 ? Na1 Na1 3.139(3) 2_455 ? Na1 S7 3.250(13) . ? Na1 S6 3.372(8) . ? S1 Pd1 2.3162(9) . ? S2 Pd1 2.3275(9) . ? S4 S4 1.359(5) 2_455 ? S4 C17 1.791(6) 2_455 ? S5 S7 0.729(14) . ? S6 S7 0.949(16) . ? Pd1 S1 2.3162(9) 5 ? Pd1 S2 2.3275(9) 5 ? 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 C2 C1 S2 126.4(3) . . ? C2 C1 S1 125.7(3) . . ? S2 C1 S1 107.9(2) . . ? C1 C2 C8 127.1(3) . . ? C1 C2 C3 127.0(3) . . ? C8 C2 C3 105.8(3) . . ? C4 C3 C7 116.2(3) . . ? C4 C3 C2 134.4(3) . . ? C7 C3 C2 109.4(3) . . ? C5 C4 C3 117.7(4) . . ? C5 C4 H4 121.2 . . ? C3 C4 H4 121.2 . . ? C6 C5 C4 120.9(4) . . ? C6 C5 H5 119.6 . . ? C4 C5 H5 119.6 . . ? N1 C6 C5 123.2(4) . . ? N1 C6 H6 118.4 . . ? C5 C6 H6 118.4 . . ? N1 C7 C3 126.5(3) . . ? N1 C7 C12 125.8(3) . . ? C3 C7 C12 107.7(3) . . ? N1 C7 Na1 49.17(19) . . ? C3 C7 Na1 164.8(3) . . ? C12 C7 Na1 78.21(19) . . ? C9 C8 C12 116.8(3) . . ? C9 C8 C2 134.4(3) . . ? C12 C8 C2 108.8(3) . . ? C10 C9 C8 118.3(3) . . ? C10 C9 H9 120.9 . . ? C8 C9 H9 120.9 . . ? C9 C10 C11 119.7(4) . . ? C9 C10 H10 120.2 . . ? C11 C10 H10 120.2 . . ? N2 C11 C10 124.3(4) . . ? N2 C11 H11 117.8 . . ? C10 C11 H11 117.8 . . ? N2 C12 C8 126.0(3) . . ? N2 C12 C7 125.7(3) . . ? C8 C12 C7 108.3(3) . . ? S3 C13 H13A 109.5 . . ? S3 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? S3 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? S3 C14 H14A 109.5 . . ? S3 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? S3 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? S7 C15 S6 32.5(7) . . ? S7 C15 S5 20.6(6) . . ? S6 C15 S5 27.5(3) . . ? S6 C16 S5 22.7(6) . . ? S6 C16 S7 7.1(6) . . ? S5 C16 S7 19.6(4) . . ? S5 C16A S6 22.7(6) . . ? S5 C16A S7 12.3(7) . . ? S6 C16A S7 30.7(6) . . ? S6 C16B S5 12.7(10) . . ? S6 C16B S7 20.1(12) . . ? S5 C16B S7 23.3(6) . . ? S4 C17 S4 45.05(19) . 2_455 ? C7 N1 C6 115.5(3) . . ? C7 N1 Na1 106.6(2) . . ? C6 N1 Na1 133.9(3) . . ? C11 N2 C12 114.9(3) . . ? C11 N2 Na1 138.3(3) . . ? C12 N2 Na1 103.6(2) . . ? S3 O1 Na1 166.4(5) . . ? S7 O2 S5 28.6(6) . . ? S7 O2 S6 35.3(6) . . ? S5 O2 S6 30.5(3) . . ? S7 O2 Na1 150.1(7) . 2_455 ? S5 O2 Na1 124.4(2) . 2_455 ? S6 O2 Na1 116.3(3) . 2_455 ? S7 O2 Na1 113.6(6) . . ? S5 O2 Na1 137.6(2) . . ? S6 O2 Na1 111.1(4) . . ? Na1 O2 Na1 81.89(13) 2_455 . ? S4 O3 S4 55.0(2) . 2_455 ? S4 O3 Na1 133.63(10) . 2_455 ? S4 O3 Na1 130.29(11) 2_455 2_455 ? S4 O3 Na1 130.29(11) . . ? S4 O3 Na1 133.63(10) 2_455 . ? Na1 O3 Na1 82.24(17) 2_455 . ? O2 Na1 O3 83.24(12) 2_455 . ? O2 Na1 O2 79.24(16) 2_455 . ? O3 Na1 O2 82.28(11) . . ? O2 Na1 O1 97.0(2) 2_455 . ? O3 Na1 O1 97.05(17) . . ? O2 Na1 O1 176.2(2) . . ? O2 Na1 N1 98.80(13) 2_455 . ? O3 Na1 N1 176.85(13) . . ? O2 Na1 N1 100.42(13) . . ? O1 Na1 N1 80.35(17) . . ? O2 Na1 N2 172.52(14) 2_455 . ? O3 Na1 N2 104.15(11) . . ? O2 Na1 N2 100.41(14) . . ? O1 Na1 N2 83.4(2) . . ? N1 Na1 N2 73.87(11) . . ? O2 Na1 C7 122.07(13) 2_455 . ? O3 Na1 C7 153.09(12) . . ? O2 Na1 C7 109.50(12) . . ? O1 Na1 C7 72.68(17) . . ? N1 Na1 C7 24.25(10) . . ? N2 Na1 C7 50.87(10) . . ? O2 Na1 Na1 49.68(10) 2_455 2_455 ? O3 Na1 Na1 48.88(9) . 2_455 ? O2 Na1 Na1 48.43(10) . 2_455 ? O1 Na1 Na1 128.64(19) . 2_455 ? N1 Na1 Na1 134.23(8) . 2_455 ? N2 Na1 Na1 135.02(12) . 2_455 ? C7 Na1 Na1 154.53(8) . 2_455 ? O2 Na1 S7 101.6(3) 2_455 . ? O3 Na1 S7 91.9(3) . . ? O2 Na1 S7 23.4(3) . . ? O1 Na1 S7 160.2(3) . . ? N1 Na1 S7 90.1(3) . . ? N2 Na1 S7 77.4(3) . . ? C7 Na1 S7 91.5(3) . . ? Na1 Na1 S7 69.9(3) 2_455 . ? O2 Na1 S6 104.55(18) 2_455 . ? O3 Na1 S6 76.43(14) . . ? O2 Na1 S6 26.94(18) . . ? O1 Na1 S6 156.4(2) . . ? N1 Na1 S6 105.25(15) . . ? N2 Na1 S6 76.54(16) . . ? C7 Na1 S6 102.86(14) . . ? Na1 Na1 S6 63.40(13) 2_455 . ? S7 Na1 S6 16.3(3) . . ? C1 S1 Pd1 88.70(12) . . ? C1 S2 Pd1 88.38(12) . . ? O1 S3 C13 102.8(4) . . ? O1 S3 C14 113.7(4) . . ? C13 S3 C14 93.6(5) . . ? S4 S4 O3 62.52(12) 2_455 . ? S4 S4 C17 68.8(3) 2_455 . ? O3 S4 C17 107.9(3) . . ? S4 S4 C17 66.1(3) 2_455 2_455 ? O3 S4 C17 106.2(3) . 2_455 ? C17 S4 C17 98.4(4) . 2_455 ? S7 S5 C16A 148.0(18) . . ? S7 S5 O2 67.8(11) . . ? C16A S5 O2 133.5(10) . . ? S7 S5 C15 38.3(11) . . ? C16A S5 C15 116.9(12) . . ? O2 S5 C15 105.7(4) . . ? S7 S5 C16 105.5(13) . . ? C16A S5 C16 93.0(15) . . ? O2 S5 C16 103.4(4) . . ? C15 S5 C16 92.2(5) . . ? S7 S5 C16B 81.4(17) . . ? C16A S5 C16B 112.4(17) . . ? O2 S5 C16B 98.1(11) . . ? C15 S5 C16B 70.6(12) . . ? C16 S5 C16B 24.4(11) . . ? S7 S6 C16B 139(2) . . ? S7 S6 C16 164.2(13) . . ? C16B S6 C16 40(2) . . ? S7 S6 O2 59.2(9) . . ? C16B S6 O2 141(2) . . ? C16 S6 O2 134.3(7) . . ? S7 S6 C15 46.8(9) . . ? C16B S6 C15 94(2) . . ? C16 S6 C15 122.8(7) . . ? O2 S6 C15 102.4(5) . . ? S7 S6 C16A 76.9(15) . . ? C16B S6 C16A 123(2) . . ? C16 S6 C16A 93.0(13) . . ? O2 S6 C16A 91.9(8) . . ? C15 S6 C16A 91.7(11) . . ? S7 S6 Na1 74.5(10) . . ? C16B S6 Na1 102(2) . . ? C16 S6 Na1 120.7(8) . . ? O2 S6 Na1 42.0(3) . . ? C15 S6 Na1 94.5(5) . . ? C16A S6 Na1 133.7(8) . . ? S5 S7 S6 58.1(12) . . ? S5 S7 C15 121.1(16) . . ? S6 S7 C15 100.8(14) . . ? S5 S7 O2 83.6(12) . . ? S6 S7 O2 85.5(10) . . ? C15 S7 O2 154.1(13) . . ? S5 S7 C16A 19.7(11) . . ? S6 S7 C16A 72.3(14) . . ? C15 S7 C16A 107.5(12) . . ? O2 S7 C16A 98.4(11) . . ? S5 S7 C16B 75.3(17) . . ? S6 S7 C16B 21.3(14) . . ? C15 S7 C16B 80.8(14) . . ? O2 S7 C16B 100.3(14) . . ? C16A S7 C16B 85.3(15) . . ? S5 S7 C16 55.0(11) . . ? S6 S7 C16 8.7(7) . . ? C15 S7 C16 95.5(9) . . ? O2 S7 C16 93.2(8) . . ? C16A S7 C16 67.0(11) . . ? C16B S7 C16 20.6(11) . . ? S5 S7 Na1 121.1(12) . . ? S6 S7 Na1 89.1(10) . . ? C15 S7 Na1 111.5(10) . . ? O2 S7 Na1 43.0(5) . . ? C16A S7 Na1 139.2(10) . . ? C16B S7 Na1 89.6(11) . . ? C16 S7 Na1 97.5(6) . . ? S1 Pd1 S1 180.00(6) . 5 ? S1 Pd1 S2 105.34(3) . 5 ? S1 Pd1 S2 74.66(3) 5 5 ? S1 Pd1 S2 74.66(3) . . ? S1 Pd1 S2 105.34(3) 5 . ? S2 Pd1 S2 180.00(6) 5 . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 30.08 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.497 _refine_diff_density_min -2.061 _refine_diff_density_rms 0.163 ###Material relevant to compound 10 at 173K ######## data_e487a _database_code_depnum_ccdc_archive 'CCDC 621048' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H18 Hg N4 Na O S5), C8 H20 N, 0.2(O)' _chemical_formula_sum 'C34 H38 Hg N5 Na O1.2 S5' _chemical_formula_weight 919.77 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' Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Hg Hg -2.3894 9.2266 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P2(1)/c ' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 15.9344(4) _cell_length_b 12.7430(3) _cell_length_c 37.3352(8) _cell_angle_alpha 90.00 _cell_angle_beta 99.3850(10) _cell_angle_gamma 90.00 _cell_volume 7479.5(3) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 6235 _cell_measurement_theta_min 3.04 _cell_measurement_theta_max 27.45 _exptl_crystal_description platelet _exptl_crystal_colour orange _exptl_crystal_size_max 0.41 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.635 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3664 _exptl_absorpt_coefficient_mu 4.442 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2632 _exptl_absorpt_correction_T_max 0.8084 _exptl_absorpt_process_details sadabs _exptl_special_details ; One DMSO molecule shows positional disorder of its sulfur atom. This disorder has been modeled and the hydrogen atoms not been introduced on this molecule. ; _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 58023 _diffrn_reflns_av_R_equivalents 0.0598 _diffrn_reflns_av_sigmaI/netI 0.0649 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -47 _diffrn_reflns_limit_l_max 48 _diffrn_reflns_theta_min 1.11 _diffrn_reflns_theta_max 27.64 _reflns_number_total 17316 _reflns_number_gt 11798 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _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^)+(0.0967P)^2^+16.2085P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 17316 _refine_ls_number_parameters 801 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0951 _refine_ls_R_factor_gt 0.0553 _refine_ls_wR_factor_ref 0.1778 _refine_ls_wR_factor_gt 0.1488 _refine_ls_goodness_of_fit_ref 1.066 _refine_ls_restrained_S_all 1.066 _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 0.21634(2) 0.59781(3) 0.222680(7) 0.04578(12) Uani 1 1 d . . . S1 S 0.28743(12) 0.71553(15) 0.17694(4) 0.0311(4) Uani 1 1 d . . . S2 S 0.12832(12) 0.59254(14) 0.16156(4) 0.0279(4) Uani 1 1 d . . . S3 S 0.12640(14) 0.72440(16) 0.26725(4) 0.0372(5) Uani 1 1 d . . . S4 S 0.25755(15) 0.56049(18) 0.28608(5) 0.0419(5) Uani 1 1 d . . . N1 N 0.2334(4) 0.8665(5) 0.03303(15) 0.0336(15) Uani 1 1 d . . . N2 N 0.0833(4) 0.7225(4) 0.01543(14) 0.0258(12) Uani 1 1 d . . . N3 N 0.2500(4) 0.6104(5) 0.43444(15) 0.0333(14) Uani 1 1 d . . . N4 N 0.1081(4) 0.7669(5) 0.41723(14) 0.0272(13) Uani 1 1 d . . . C1 C 0.1983(4) 0.6818(5) 0.14619(16) 0.0223(13) Uani 1 1 d . . . C2 C 0.1817(4) 0.7205(5) 0.11055(16) 0.0210(13) Uani 1 1 d . . . C3 C 0.2330(4) 0.7977(5) 0.09451(16) 0.0231(14) Uani 1 1 d . . . C4 C 0.3021(5) 0.8620(6) 0.10766(18) 0.0295(16) Uani 1 1 d . . . H4 H 0.3254 0.8617 0.1322 0.035 Uiso 1 1 calc R . . C5 C 0.3353(5) 0.9260(7) 0.0836(2) 0.0386(19) Uani 1 1 d . . . H5 H 0.3810 0.9697 0.0919 0.046 Uiso 1 1 calc R . . C6 C 0.3005(5) 0.9254(7) 0.0468(2) 0.043(2) Uani 1 1 d . . . H6 H 0.3251 0.9680 0.0311 0.051 Uiso 1 1 calc R . . C7 C 0.2011(4) 0.8044(6) 0.05704(17) 0.0259(14) Uani 1 1 d . . . C8 C 0.1145(4) 0.6867(5) 0.08105(16) 0.0218(13) Uani 1 1 d . . . C9 C 0.0471(5) 0.6169(6) 0.07801(18) 0.0308(16) Uani 1 1 d . . . H9 H 0.0341 0.5817 0.0982 0.037 Uiso 1 1 calc R . . C10 C -0.0004(5) 0.6013(6) 0.04401(19) 0.0328(16) Uani 1 1 d . . . H10 H -0.0464 0.5554 0.0413 0.039 Uiso 1 1 calc R . . C11 C 0.0198(5) 0.6537(6) 0.01377(18) 0.0302(16) Uani 1 1 d . . . H11 H -0.0126 0.6398 -0.0088 0.036 Uiso 1 1 calc R . . C12 C 0.1290(4) 0.7367(5) 0.04818(16) 0.0225(14) Uani 1 1 d . . . C13 C 0.1896(4) 0.6540(6) 0.30013(17) 0.0267(15) Uani 1 1 d . . . C14 C 0.1894(4) 0.6660(5) 0.33766(16) 0.0247(14) Uani 1 1 d . . . C15 C 0.1344(4) 0.7361(5) 0.35462(16) 0.0237(14) Uani 1 1 d . . . C16 C 0.0720(5) 0.8099(6) 0.34116(18) 0.0296(16) Uani 1 1 d . . . H16 H 0.0598 0.8252 0.3165 0.035 Uiso 1 1 calc R . . C17 C 0.0289(5) 0.8595(6) 0.3660(2) 0.0345(17) Uani 1 1 d . . . H17 H -0.0133 0.9084 0.3580 0.041 Uiso 1 1 calc R . . C18 C 0.0488(5) 0.8361(6) 0.40320(19) 0.0333(17) Uani 1 1 d . . . H18 H 0.0189 0.8709 0.4190 0.040 Uiso 1 1 calc R . . C19 C 0.2167(4) 0.6432(6) 0.40093(17) 0.0252(14) Uani 1 1 d . . . C20 C 0.2407(4) 0.6085(6) 0.36787(17) 0.0255(14) Uani 1 1 d . . . C21 C 0.3029(5) 0.5314(6) 0.37082(18) 0.0373(19) Uani 1 1 d . . . H21 H 0.3202 0.5031 0.3502 0.045 Uiso 1 1 calc R . . C22 C 0.3390(6) 0.4970(7) 0.4056(2) 0.043(2) Uani 1 1 d . . . H22 H 0.3819 0.4467 0.4083 0.052 Uiso 1 1 calc R . . C23 C 0.3112(5) 0.5377(7) 0.43582(19) 0.040(2) Uani 1 1 d . . . H23 H 0.3365 0.5132 0.4585 0.048 Uiso 1 1 calc R . . C24 C 0.1502(4) 0.7191(5) 0.39281(17) 0.0229(14) Uani 1 1 d . . . Hg2 Hg 0.21000(2) 0.35525(3) 0.152257(7) 0.04019(11) Uani 1 1 d . . . S5 S 0.18719(13) 0.40092(18) 0.08866(5) 0.0384(5) Uani 1 1 d . . . S6 S 0.30770(15) 0.22835(17) 0.11023(5) 0.0411(5) Uani 1 1 d . . . S7 S 0.32091(12) 0.38521(16) 0.21114(4) 0.0314(4) Uani 1 1 d . . . S8 S 0.14977(12) 0.29553(16) 0.20698(4) 0.0317(4) Uani 1 1 d . . . N5 N 0.2819(4) 0.4220(5) -0.04943(13) 0.0258(13) Uani 1 1 d . . . N6 N 0.3981(4) 0.2372(5) -0.03079(15) 0.0291(13) Uani 1 1 d . . . N8 N 0.4015(4) 0.2689(5) 0.35880(15) 0.0299(13) Uani 1 1 d . . . N7 N 0.2301(4) 0.1703(5) 0.35472(15) 0.0352(15) Uani 1 1 d . . . C25 C 0.2646(5) 0.3153(6) 0.07723(17) 0.0258(14) Uani 1 1 d . . . C26 C 0.2885(4) 0.3213(5) 0.04233(16) 0.0228(14) Uani 1 1 d . . . C27 C 0.2571(4) 0.3958(5) 0.01316(16) 0.0204(13) Uani 1 1 d . . . C28 C 0.2038(4) 0.4839(5) 0.01004(16) 0.0217(13) Uani 1 1 d . . . H28 H 0.1766 0.5046 0.0291 0.026 Uiso 1 1 calc R . . C29 C 0.1929(4) 0.5392(6) -0.02230(17) 0.0261(15) Uani 1 1 d . . . H29 H 0.1594 0.5994 -0.0247 0.031 Uiso 1 1 calc R . . C30 C 0.2316(4) 0.5060(6) -0.05133(17) 0.0270(15) Uani 1 1 d . . . H30 H 0.2219 0.5440 -0.0729 0.032 Uiso 1 1 calc R . . C31 C 0.2945(4) 0.3708(5) -0.01745(16) 0.0225(13) Uani 1 1 d . . . C32 C 0.3490(4) 0.2551(5) 0.02820(17) 0.0232(14) Uani 1 1 d . . . C33 C 0.4040(5) 0.1740(6) 0.0419(2) 0.0338(17) Uani 1 1 d . . . H33 H 0.4065 0.1516 0.0657 0.041 Uiso 1 1 calc R . . C34 C 0.4549(5) 0.1273(6) 0.0197(2) 0.0347(17) Uani 1 1 d . . . H34 H 0.4922 0.0737 0.0286 0.042 Uiso 1 1 calc R . . C35 C 0.4498(5) 0.1610(6) -0.0161(2) 0.0338(17) Uani 1 1 d . . . H35 H 0.4844 0.1285 -0.0305 0.041 Uiso 1 1 calc R . . C36 C 0.3506(4) 0.2828(5) -0.00856(17) 0.0226(14) Uani 1 1 d . . . C37 C 0.2496(4) 0.3202(5) 0.23367(16) 0.0218(13) Uani 1 1 d . . . C38 C 0.2671(4) 0.2912(5) 0.26990(16) 0.0214(13) Uani 1 1 d . . . C39 C 0.3472(4) 0.3107(6) 0.29480(17) 0.0259(14) Uani 1 1 d . . . C40 C 0.4238(5) 0.3612(6) 0.29218(19) 0.0338(17) Uani 1 1 d . . . H40 H 0.4325 0.3937 0.2708 0.041 Uiso 1 1 calc R . . C41 C 0.4866(5) 0.3610(7) 0.3228(2) 0.044(2) Uani 1 1 d . . . H41 H 0.5385 0.3928 0.3216 0.053 Uiso 1 1 calc R . . C42 C 0.4747(5) 0.3161(7) 0.3544(2) 0.0364(18) Uani 1 1 d . . . H42 H 0.5191 0.3178 0.3740 0.044 Uiso 1 1 calc R . . C43 C 0.3411(4) 0.2667(5) 0.32924(16) 0.0229(14) Uani 1 1 d . . . C44 C 0.2119(4) 0.2361(5) 0.29141(16) 0.0235(14) Uani 1 1 d . . . C45 C 0.1292(5) 0.1967(6) 0.28524(18) 0.0333(17) Uani 1 1 d . . . H45 H 0.0953 0.2045 0.2626 0.040 Uiso 1 1 calc R . . C46 C 0.0981(5) 0.1463(7) 0.3130(2) 0.041(2) Uani 1 1 d . . . H46 H 0.0428 0.1206 0.3093 0.049 Uiso 1 1 calc R . . C47 C 0.1508(5) 0.1337(7) 0.3472(2) 0.042(2) Uani 1 1 d . . . H47 H 0.1289 0.0979 0.3653 0.051 Uiso 1 1 calc R . . C48 C 0.2578(5) 0.2202(6) 0.32733(17) 0.0277(15) Uani 1 1 d . . . O1 O 0.0758(5) 0.5084(5) 0.4613(2) 0.0631(19) Uani 1 1 d . . . S9A S 0.06941(19) 0.3948(2) 0.47002(9) 0.0502(10) Uani 0.765(7) 1 d P A 1 S9B S 0.1559(6) 0.4224(8) 0.4804(3) 0.050(3) Uani 0.235(7) 1 d P . 2 C49 C 0.1552(10) 0.3317(11) 0.4561(4) 0.090(3) Uani 1 1 d . . . C50 C 0.1045(10) 0.3824(10) 0.5180(4) 0.090(3) Uani 1 1 d . . . S10 S 0.55755(16) 0.3544(2) -0.06372(9) 0.0656(8) Uani 1 1 d . . . O2 O 0.4808(4) 0.4178(6) -0.0799(3) 0.078(3) Uani 1 1 d . . . C51 C 0.6447(7) 0.4105(12) -0.0798(4) 0.092(3) Uani 1 1 d . . . H51A H 0.6414 0.3945 -0.1052 0.138 Uiso 1 1 calc R . . H51B H 0.6965 0.3824 -0.0666 0.138 Uiso 1 1 calc R . . H51C H 0.6438 0.4852 -0.0766 0.138 Uiso 1 1 calc R . . C52 C 0.5830(7) 0.3976(12) -0.0172(3) 0.092(3) Uani 1 1 d . . . H52A H 0.5404 0.3724 -0.0038 0.138 Uiso 1 1 calc R . . H52B H 0.5844 0.4728 -0.0164 0.138 Uiso 1 1 calc R . . H52C H 0.6375 0.3703 -0.0066 0.138 Uiso 1 1 calc R . . N9 N 0.0582(6) 0.9756(7) 0.1736(3) 0.077(2) Uani 1 1 d . . . C53 C 0.1451(8) 0.9287(11) 0.1880(4) 0.091(3) Uani 1 1 d . . . H53A H 0.1651 0.8910 0.1684 0.110 Uiso 1 1 calc R . . H53B H 0.1389 0.8784 0.2068 0.110 Uiso 1 1 calc R . . C54 C 0.2128(8) 1.0099(11) 0.2035(4) 0.090(3) Uani 1 1 d . . . H54A H 0.2656 0.9747 0.2119 0.134 Uiso 1 1 calc R . . H54B H 0.1945 1.0464 0.2233 0.134 Uiso 1 1 calc R . . H54C H 0.2206 1.0592 0.1848 0.134 Uiso 1 1 calc R . . C55 C 0.0642(8) 1.0602(11) 0.1448(3) 0.079(2) Uani 1 1 d . . . H55A H 0.0075 1.0864 0.1360 0.095 Uiso 1 1 calc R . . H55B H 0.0976 1.1182 0.1564 0.095 Uiso 1 1 calc R . . C56 C 0.1021(8) 1.0254(11) 0.1135(4) 0.090(3) Uani 1 1 d . . . H56A H 0.1036 1.0831 0.0971 0.134 Uiso 1 1 calc R . . H56B H 0.0686 0.9696 0.1013 0.134 Uiso 1 1 calc R . . H56C H 0.1590 1.0009 0.1217 0.134 Uiso 1 1 calc R . . C57 C 0.0207(8) 1.0320(10) 0.2033(3) 0.079(2) Uani 1 1 d . . . H57A H -0.0315 1.0666 0.1924 0.095 Uiso 1 1 calc R . . H57B H 0.0603 1.0861 0.2136 0.095 Uiso 1 1 calc R . . C58 C 0.0013(10) 0.9605(11) 0.2342(4) 0.106(3) Uani 1 1 d . . . H58A H -0.0224 1.0017 0.2516 0.159 Uiso 1 1 calc R . . H58B H 0.0530 0.9279 0.2458 0.159 Uiso 1 1 calc R . . H58C H -0.0386 0.9074 0.2244 0.159 Uiso 1 1 calc R . . C59 C 0.0040(8) 0.8847(9) 0.1575(4) 0.081(3) Uani 1 1 d . . . H59A H 0.0050 0.8309 0.1759 0.097 Uiso 1 1 calc R . . H59B H 0.0292 0.8552 0.1378 0.097 Uiso 1 1 calc R . . C60 C -0.0892(7) 0.9132(9) 0.1430(3) 0.067(3) Uani 1 1 d . . . H60A H -0.1193 0.8515 0.1334 0.101 Uiso 1 1 calc R . . H60B H -0.0911 0.9648 0.1241 0.101 Uiso 1 1 calc R . . H60C H -0.1153 0.9412 0.1623 0.101 Uiso 1 1 calc R . . N10 N 0.4248(6) 0.6420(7) 0.8465(3) 0.077(2) Uani 1 1 d . . . C61 C 0.4909(9) 0.5932(10) 0.8311(4) 0.091(3) Uani 1 1 d . . . H61A H 0.5435 0.6256 0.8426 0.110 Uiso 1 1 calc R . . H61B H 0.4827 0.6150 0.8058 0.110 Uiso 1 1 calc R . . C62 C 0.5079(13) 0.4762(14) 0.8311(6) 0.151(6) Uani 1 1 d . . . H62A H 0.5507 0.4617 0.8164 0.227 Uiso 1 1 calc R . . H62B H 0.4565 0.4398 0.8213 0.227 Uiso 1 1 calc R . . H62C H 0.5274 0.4530 0.8555 0.227 Uiso 1 1 calc R . . C63 C 0.3440(8) 0.5736(10) 0.8396(4) 0.081(3) Uani 1 1 d . . . H63A H 0.3612 0.5032 0.8476 0.097 Uiso 1 1 calc R . . H63B H 0.3069 0.5989 0.8559 0.097 Uiso 1 1 calc R . . C64 C 0.2925(13) 0.5630(14) 0.8048(6) 0.151(6) Uani 1 1 d . . . H64A H 0.2455 0.5173 0.8066 0.227 Uiso 1 1 calc R . . H64B H 0.3259 0.5338 0.7881 0.227 Uiso 1 1 calc R . . H64C H 0.2715 0.6306 0.7963 0.227 Uiso 1 1 calc R . . C65 C 0.4582(8) 0.6517(11) 0.8897(3) 0.079(2) Uani 1 1 d . . . H65A H 0.4715 0.5816 0.8991 0.095 Uiso 1 1 calc R . . H65B H 0.5109 0.6912 0.8931 0.095 Uiso 1 1 calc R . . C66 C 0.4046(12) 0.6976(17) 0.9103(7) 0.177(10) Uani 1 1 d . . . H66A H 0.4320 0.7007 0.9351 0.265 Uiso 1 1 calc R . . H66B H 0.3534 0.6569 0.9086 0.265 Uiso 1 1 calc R . . H66C H 0.3908 0.7674 0.9015 0.265 Uiso 1 1 calc R . . C67 C 0.4001(8) 0.7477(9) 0.8361(4) 0.079(2) Uani 1 1 d . . . H67A H 0.3542 0.7679 0.8489 0.095 Uiso 1 1 calc R . . H67B H 0.3776 0.7481 0.8104 0.095 Uiso 1 1 calc R . . C68 C 0.4711(11) 0.8329(11) 0.8435(4) 0.106(3) Uani 1 1 d . . . H68A H 0.4506 0.8974 0.8320 0.159 Uiso 1 1 calc R . . H68B H 0.5203 0.8099 0.8339 0.159 Uiso 1 1 calc R . . H68C H 0.4860 0.8440 0.8692 0.159 Uiso 1 1 calc R . . Na1 Na 0.14677(19) 0.6622(2) 0.47309(7) 0.0310(6) Uani 1 1 d . . . Na2 Na 0.35487(18) 0.3277(2) -0.09179(7) 0.0316(6) Uani 1 1 d . . . O3 O 0.4124(11) 0.4357(15) 0.7404(5) 0.062(4) Uiso 0.40 1 d P . . 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 0.0800(3) 0.0412(2) 0.01713(14) 0.00524(11) 0.01101(14) 0.01446(17) S1 0.0347(10) 0.0350(11) 0.0211(7) 0.0055(7) -0.0030(7) -0.0046(8) S2 0.0344(10) 0.0302(10) 0.0198(7) 0.0023(6) 0.0066(7) -0.0044(8) S3 0.0565(13) 0.0362(11) 0.0176(7) 0.0039(7) 0.0023(8) 0.0173(9) S4 0.0634(14) 0.0438(12) 0.0195(8) 0.0014(8) 0.0100(8) 0.0259(11) N1 0.038(4) 0.038(4) 0.024(3) 0.008(3) 0.005(3) -0.009(3) N2 0.033(3) 0.024(3) 0.019(2) -0.002(2) 0.001(2) -0.001(3) N3 0.038(4) 0.041(4) 0.019(3) 0.004(2) -0.002(2) 0.013(3) N4 0.026(3) 0.034(4) 0.021(3) -0.007(2) 0.001(2) 0.003(3) C1 0.029(4) 0.019(3) 0.018(3) -0.001(2) 0.002(3) 0.001(3) C2 0.022(3) 0.019(3) 0.021(3) 0.000(2) 0.002(2) 0.002(3) C3 0.024(4) 0.024(4) 0.021(3) -0.002(3) 0.004(3) -0.001(3) C4 0.032(4) 0.030(4) 0.023(3) 0.005(3) -0.005(3) -0.002(3) C5 0.038(4) 0.037(5) 0.039(4) 0.009(3) -0.001(3) -0.020(4) C6 0.045(5) 0.043(5) 0.037(4) 0.014(4) -0.002(4) -0.016(4) C7 0.028(4) 0.026(4) 0.024(3) 0.006(3) 0.003(3) 0.002(3) C8 0.021(3) 0.022(3) 0.022(3) 0.000(3) 0.002(2) 0.003(3) C9 0.029(4) 0.037(4) 0.025(3) 0.006(3) 0.002(3) -0.007(3) C10 0.025(4) 0.039(5) 0.032(3) -0.003(3) -0.002(3) -0.007(3) C11 0.039(4) 0.028(4) 0.022(3) -0.007(3) -0.001(3) -0.002(3) C12 0.025(3) 0.021(3) 0.020(3) -0.001(2) 0.000(2) 0.002(3) C13 0.031(4) 0.029(4) 0.020(3) 0.005(3) 0.004(3) 0.005(3) C14 0.032(4) 0.023(4) 0.016(3) 0.003(2) -0.002(3) 0.005(3) C15 0.028(4) 0.024(4) 0.017(3) -0.005(2) 0.000(3) -0.001(3) C16 0.034(4) 0.029(4) 0.023(3) 0.000(3) -0.002(3) 0.006(3) C17 0.035(4) 0.033(4) 0.034(4) -0.004(3) 0.002(3) 0.013(3) C18 0.038(4) 0.035(4) 0.026(3) -0.009(3) 0.003(3) 0.013(4) C19 0.026(3) 0.027(4) 0.021(3) 0.001(3) -0.002(3) 0.001(3) C20 0.027(4) 0.030(4) 0.018(3) 0.000(3) 0.000(3) 0.006(3) C21 0.053(5) 0.038(5) 0.021(3) 0.002(3) 0.008(3) 0.019(4) C22 0.058(6) 0.037(5) 0.035(4) 0.006(3) 0.010(4) 0.032(4) C23 0.039(5) 0.054(6) 0.025(3) 0.012(3) 0.000(3) 0.019(4) C24 0.023(3) 0.020(3) 0.024(3) -0.004(3) 0.002(3) -0.004(3) Hg2 0.0598(2) 0.0436(2) 0.01894(13) 0.00600(12) 0.01176(12) 0.00726(16) S5 0.0419(11) 0.0535(13) 0.0222(8) 0.0105(8) 0.0123(8) 0.0191(10) S6 0.0637(14) 0.0345(11) 0.0276(8) 0.0118(8) 0.0147(9) 0.0186(10) S7 0.0325(10) 0.0394(11) 0.0234(8) 0.0073(7) 0.0075(7) -0.0036(8) S8 0.0372(10) 0.0392(11) 0.0181(7) 0.0046(7) 0.0030(7) -0.0107(8) N5 0.027(3) 0.034(3) 0.015(2) -0.003(2) 0.001(2) 0.001(3) N6 0.031(3) 0.032(3) 0.025(3) -0.009(2) 0.005(2) 0.000(3) N8 0.030(3) 0.036(4) 0.025(3) 0.003(2) 0.007(2) 0.003(3) N7 0.034(4) 0.050(4) 0.022(3) 0.009(3) 0.004(2) -0.013(3) C25 0.035(4) 0.023(4) 0.019(3) 0.001(3) 0.004(3) 0.000(3) C26 0.029(4) 0.021(3) 0.019(3) -0.003(2) 0.004(3) -0.001(3) C27 0.022(3) 0.019(3) 0.019(3) -0.004(2) 0.000(2) -0.003(3) C28 0.020(3) 0.027(4) 0.017(3) -0.004(2) 0.001(2) -0.005(3) C29 0.023(4) 0.031(4) 0.022(3) 0.002(3) -0.001(3) 0.002(3) C30 0.028(4) 0.033(4) 0.019(3) 0.002(3) -0.001(3) 0.002(3) C31 0.023(3) 0.024(4) 0.020(3) -0.002(2) 0.000(2) -0.001(3) C32 0.026(4) 0.018(3) 0.025(3) -0.003(3) 0.002(3) 0.001(3) C33 0.044(5) 0.025(4) 0.032(4) -0.001(3) 0.007(3) 0.000(3) C34 0.034(4) 0.026(4) 0.042(4) -0.005(3) 0.001(3) 0.006(3) C35 0.033(4) 0.032(4) 0.036(4) -0.006(3) 0.005(3) 0.003(3) C36 0.024(3) 0.019(3) 0.024(3) -0.009(3) 0.003(3) -0.006(3) C37 0.027(4) 0.018(3) 0.021(3) 0.005(2) 0.006(3) 0.003(3) C38 0.026(3) 0.021(3) 0.018(3) 0.002(2) 0.006(2) 0.000(3) C39 0.030(4) 0.025(4) 0.023(3) 0.003(3) 0.006(3) 0.003(3) C40 0.028(4) 0.047(5) 0.026(3) 0.014(3) 0.002(3) 0.002(3) C41 0.018(4) 0.061(6) 0.051(5) 0.015(4) 0.001(3) -0.006(4) C42 0.025(4) 0.050(5) 0.032(4) 0.009(3) -0.004(3) 0.001(4) C43 0.025(3) 0.024(4) 0.021(3) 0.005(3) 0.006(3) 0.003(3) C44 0.028(4) 0.027(4) 0.018(3) 0.001(3) 0.010(3) -0.003(3) C45 0.037(4) 0.042(5) 0.018(3) -0.001(3) -0.001(3) -0.008(4) C46 0.036(4) 0.055(6) 0.033(4) 0.001(4) 0.010(3) -0.017(4) C47 0.045(5) 0.053(5) 0.029(4) 0.015(4) 0.007(3) -0.012(4) C48 0.032(4) 0.032(4) 0.020(3) 0.002(3) 0.007(3) 0.001(3) O1 0.069(5) 0.029(3) 0.088(5) 0.010(3) 0.005(4) 0.000(3) S9A 0.0401(18) 0.0316(16) 0.075(2) 0.0079(14) -0.0015(14) -0.0019(13) S9B 0.040(6) 0.040(6) 0.068(7) 0.014(5) 0.003(5) -0.003(4) C49 0.122(8) 0.070(6) 0.082(6) 0.024(5) 0.034(6) 0.035(6) C50 0.122(8) 0.070(6) 0.082(6) 0.024(5) 0.034(6) 0.035(6) S10 0.0426(14) 0.0617(17) 0.091(2) -0.0388(15) 0.0066(13) -0.0127(12) O2 0.033(4) 0.056(5) 0.147(8) -0.018(5) 0.018(4) -0.011(3) C51 0.052(5) 0.127(9) 0.099(7) -0.062(6) 0.022(5) -0.030(5) C52 0.052(5) 0.127(9) 0.099(7) -0.062(6) 0.022(5) -0.030(5) N9 0.056(4) 0.052(4) 0.119(6) 0.005(4) 0.003(4) 0.012(3) C53 0.072(6) 0.069(6) 0.130(9) -0.006(6) 0.006(6) 0.013(5) C54 0.070(6) 0.089(7) 0.100(7) -0.023(5) -0.011(5) 0.021(5) C55 0.074(6) 0.079(6) 0.081(6) -0.014(5) 0.001(5) 0.002(5) C56 0.070(6) 0.089(7) 0.100(7) -0.023(5) -0.011(5) 0.021(5) C57 0.086(6) 0.058(5) 0.090(6) -0.005(5) 0.003(5) 0.009(5) C58 0.134(10) 0.070(7) 0.106(8) 0.009(6) 0.000(7) 0.006(6) C59 0.068(6) 0.055(5) 0.114(8) 0.002(5) 0.000(5) -0.004(4) C60 0.068(7) 0.051(7) 0.074(7) -0.014(5) -0.013(6) 0.001(5) N10 0.056(4) 0.052(4) 0.119(6) 0.005(4) 0.003(4) 0.012(3) C61 0.072(6) 0.069(6) 0.130(9) -0.006(6) 0.006(6) 0.013(5) C62 0.148(12) 0.107(10) 0.203(15) 0.080(10) 0.040(11) 0.042(9) C63 0.068(6) 0.055(5) 0.114(8) 0.002(5) 0.000(5) -0.004(4) C64 0.148(12) 0.107(10) 0.203(15) 0.080(10) 0.040(11) 0.042(9) C65 0.074(6) 0.079(6) 0.081(6) -0.014(5) 0.001(5) 0.002(5) C66 0.107(15) 0.121(17) 0.30(3) -0.024(19) 0.028(18) 0.022(13) C67 0.086(6) 0.058(5) 0.090(6) -0.005(5) 0.003(5) 0.009(5) C68 0.134(10) 0.070(7) 0.106(8) 0.009(6) 0.000(7) 0.006(6) Na1 0.0394(16) 0.0328(17) 0.0202(12) -0.0039(11) 0.0034(11) 0.0058(13) Na2 0.0344(16) 0.0408(18) 0.0209(12) -0.0083(11) 0.0080(11) -0.0022(13) _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 S4 2.3984(17) . ? Hg1 S2 2.4769(17) . ? Hg1 S1 2.6609(18) . ? Hg1 S3 2.8640(19) . ? S1 C1 1.729(7) . ? S2 C1 1.753(7) . ? S3 C13 1.710(7) . ? S4 C13 1.747(7) . ? N1 C6 1.339(10) . ? N1 C7 1.358(8) . ? N1 Na1 2.458(6) 4_575 ? N2 C12 1.330(8) . ? N2 C11 1.332(9) . ? N2 Na1 2.491(6) 4_575 ? N3 C23 1.341(10) . ? N3 C19 1.344(8) . ? N3 Na1 2.449(7) . ? N4 C18 1.335(9) . ? N4 C24 1.362(8) . ? N4 Na1 2.468(6) . ? C1 C2 1.403(8) . ? C2 C3 1.468(9) . ? C2 C8 1.469(9) . ? C3 C4 1.396(10) . ? C3 C7 1.411(9) . ? C4 C5 1.381(10) . ? C4 H4 0.9300 . ? C5 C6 1.393(11) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C7 C12 1.432(10) . ? C8 C9 1.385(10) . ? C8 C12 1.434(9) . ? C9 C10 1.382(10) . ? C9 H9 0.9300 . ? C10 C11 1.394(10) . ? C10 H10 0.9300 . ? C11 H11 0.9300 . ? C13 C14 1.410(8) . ? C14 C15 1.465(9) . ? C14 C20 1.475(9) . ? C15 C16 1.401(10) . ? C15 C24 1.424(8) . ? C16 C17 1.393(10) . ? C16 H16 0.9300 . ? C17 C18 1.405(10) . ? C17 H17 0.9300 . ? C18 H18 0.9300 . ? C19 C20 1.421(9) . ? C19 C24 1.430(10) . ? C19 Na1 3.089(7) . ? C20 C21 1.387(10) . ? C21 C22 1.402(10) . ? C21 H21 0.9300 . ? C22 C23 1.379(10) . ? C22 H22 0.9300 . ? C23 H23 0.9300 . ? C24 Na1 3.093(7) . ? Hg2 S5 2.4139(17) . ? Hg2 S8 2.5128(16) . ? Hg2 S7 2.6144(18) . ? Hg2 S6 2.881(2) . ? S5 C25 1.751(7) . ? S6 C25 1.715(7) . ? S7 C37 1.731(6) . ? S8 C37 1.762(7) . ? N5 C30 1.331(9) . ? N5 C31 1.347(8) . ? N5 Na2 2.429(6) . ? N6 C35 1.332(10) . ? N6 C36 1.343(8) . ? N6 Na2 2.546(6) . ? N8 C43 1.341(9) . ? N8 C42 1.345(10) . ? N8 Na2 2.433(6) 4_566 ? N7 C47 1.333(10) . ? N7 C48 1.339(8) . ? N7 Na2 2.578(7) 4_566 ? C25 C26 1.417(8) . ? C26 C32 1.444(9) . ? C26 C27 1.470(9) . ? C27 C28 1.401(9) . ? C27 C31 1.409(9) . ? C28 C29 1.384(9) . ? C28 H28 0.9300 . ? C29 C30 1.397(9) . ? C29 H29 0.9300 . ? C30 H30 0.9300 . ? C31 C36 1.439(10) . ? C32 C33 1.397(10) . ? C32 C36 1.422(9) . ? C33 C34 1.385(10) . ? C33 H33 0.9300 . ? C34 C35 1.392(11) . ? C34 H34 0.9300 . ? C35 H35 0.9300 . ? C37 C38 1.386(8) . ? C38 C44 1.464(8) . ? C38 C39 1.472(9) . ? C39 C40 1.398(10) . ? C39 C43 1.420(8) . ? C40 C41 1.392(10) . ? C40 H40 0.9300 . ? C41 C42 1.351(11) . ? C41 H41 0.9300 . ? C42 H42 0.9300 . ? C43 C48 1.444(10) . ? C44 C45 1.394(10) . ? C44 C48 1.433(9) . ? C45 C46 1.378(10) . ? C45 H45 0.9300 . ? C46 C47 1.418(11) . ? C46 H46 0.9300 . ? C47 H47 0.9300 . ? O1 S9A 1.492(7) . ? O1 S9B 1.745(12) . ? O1 Na1 2.270(7) . ? S9A C49 1.737(14) . ? S9A C50 1.794(14) . ? S9B C49 1.468(18) . ? S9B C50 1.811(17) . ? S9B Na1 3.069(11) . ? S10 O2 1.507(8) . ? S10 C51 1.753(12) . ? S10 C52 1.803(11) . ? S10 Na2 3.247(4) . ? O2 Na2 2.292(7) . ? C51 H51A 0.9600 . ? C51 H51B 0.9600 . ? C51 H51C 0.9600 . ? C52 H52A 0.9600 . ? C52 H52B 0.9600 . ? C52 H52C 0.9600 . ? N9 C59 1.509(15) . ? N9 C57 1.523(15) . ? N9 C53 1.523(15) . ? N9 C55 1.536(16) . ? C53 C54 1.538(18) . ? C53 H53A 0.9700 . ? C53 H53B 0.9700 . ? C54 H54A 0.9600 . ? C54 H54B 0.9600 . ? C54 H54C 0.9600 . ? C55 C56 1.468(17) . ? C55 H55A 0.9700 . ? C55 H55B 0.9700 . ? C56 H56A 0.9600 . ? C56 H56B 0.9600 . ? C56 H56C 0.9600 . ? C57 C58 1.540(18) . ? C57 H57A 0.9700 . ? C57 H57B 0.9700 . ? C58 H58A 0.9600 . ? C58 H58B 0.9600 . ? C58 H58C 0.9600 . ? C59 C60 1.539(15) . ? C59 H59A 0.9700 . ? C59 H59B 0.9700 . ? C60 H60A 0.9600 . ? C60 H60B 0.9600 . ? C60 H60C 0.9600 . ? N10 C61 1.423(16) . ? N10 C67 1.438(14) . ? N10 C63 1.542(15) . ? N10 C65 1.618(16) . ? C61 C62 1.52(2) . ? C61 H61A 0.9700 . ? C61 H61B 0.9700 . ? C62 H62A 0.9600 . ? C62 H62B 0.9600 . ? C62 H62C 0.9600 . ? C63 C64 1.42(2) . ? C63 H63A 0.9700 . ? C63 H63B 0.9700 . ? C64 H64A 0.9600 . ? C64 H64B 0.9600 . ? C64 H64C 0.9600 . ? C65 C66 1.37(2) . ? C65 H65A 0.9700 . ? C65 H65B 0.9700 . ? C66 H66A 0.9600 . ? C66 H66B 0.9600 . ? C66 H66C 0.9600 . ? C67 C68 1.560(18) . ? C67 H67A 0.9700 . ? C67 H67B 0.9700 . ? C68 H68A 0.9600 . ? C68 H68B 0.9600 . ? C68 H68C 0.9600 . ? Na1 N1 2.458(6) 4_576 ? Na1 N2 2.491(6) 4_576 ? Na2 N8 2.433(6) 4_565 ? Na2 N7 2.578(7) 4_565 ? 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 S4 Hg1 S2 157.90(8) . . ? S4 Hg1 S1 131.94(7) . . ? S2 Hg1 S1 70.15(5) . . ? S4 Hg1 S3 67.71(6) . . ? S2 Hg1 S3 106.78(6) . . ? S1 Hg1 S3 111.17(6) . . ? C1 S1 Hg1 84.0(2) . . ? C1 S2 Hg1 89.4(2) . . ? C13 S3 Hg1 80.2(2) . . ? C13 S4 Hg1 94.5(2) . . ? C6 N1 C7 116.0(6) . . ? C6 N1 Na1 136.7(5) . 4_575 ? C7 N1 Na1 107.3(5) . 4_575 ? C12 N2 C11 115.5(6) . . ? C12 N2 Na1 106.6(4) . 4_575 ? C11 N2 Na1 138.0(4) . 4_575 ? C23 N3 C19 115.1(6) . . ? C23 N3 Na1 135.9(5) . . ? C19 N3 Na1 105.3(4) . . ? C18 N4 C24 115.3(6) . . ? C18 N4 Na1 138.8(5) . . ? C24 N4 Na1 104.0(4) . . ? C2 C1 S1 123.4(5) . . ? C2 C1 S2 120.4(5) . . ? S1 C1 S2 116.2(3) . . ? C1 C2 C3 126.2(6) . . ? C1 C2 C8 127.6(6) . . ? C3 C2 C8 106.1(5) . . ? C4 C3 C7 116.7(6) . . ? C4 C3 C2 135.2(6) . . ? C7 C3 C2 108.1(6) . . ? C5 C4 C3 118.8(6) . . ? C5 C4 H4 120.6 . . ? C3 C4 H4 120.6 . . ? C4 C5 C6 120.4(7) . . ? C4 C5 H5 119.8 . . ? C6 C5 H5 119.8 . . ? N1 C6 C5 123.1(7) . . ? N1 C6 H6 118.5 . . ? C5 C6 H6 118.5 . . ? N1 C7 C3 125.1(7) . . ? N1 C7 C12 125.1(6) . . ? C3 C7 C12 109.8(6) . . ? C9 C8 C12 116.5(6) . . ? C9 C8 C2 135.2(6) . . ? C12 C8 C2 108.2(6) . . ? C10 C9 C8 118.0(6) . . ? C10 C9 H9 121.0 . . ? C8 C9 H9 121.0 . . ? C9 C10 C11 120.7(7) . . ? C9 C10 H10 119.7 . . ? C11 C10 H10 119.7 . . ? N2 C11 C10 123.5(6) . . ? N2 C11 H11 118.3 . . ? C10 C11 H11 118.3 . . ? N2 C12 C7 126.4(6) . . ? N2 C12 C8 125.9(6) . . ? C7 C12 C8 107.8(5) . . ? C14 C13 S3 124.1(5) . . ? C14 C13 S4 118.3(5) . . ? S3 C13 S4 117.6(4) . . ? C13 C14 C15 126.4(6) . . ? C13 C14 C20 128.0(6) . . ? C15 C14 C20 105.6(5) . . ? C16 C15 C24 117.4(6) . . ? C16 C15 C14 133.9(6) . . ? C24 C15 C14 108.6(6) . . ? C17 C16 C15 117.7(6) . . ? C17 C16 H16 121.2 . . ? C15 C16 H16 121.2 . . ? C16 C17 C18 120.3(7) . . ? C16 C17 H17 119.8 . . ? C18 C17 H17 119.8 . . ? N4 C18 C17 124.0(6) . . ? N4 C18 H18 118.0 . . ? C17 C18 H18 118.0 . . ? N3 C19 C20 126.2(6) . . ? N3 C19 C24 125.0(6) . . ? C20 C19 C24 108.8(6) . . ? N3 C19 Na1 49.9(4) . . ? C20 C19 Na1 165.6(5) . . ? C24 C19 Na1 76.8(4) . . ? C21 C20 C19 116.2(6) . . ? C21 C20 C14 135.4(6) . . ? C19 C20 C14 108.4(6) . . ? C20 C21 C22 118.4(6) . . ? C20 C21 H21 120.8 . . ? C22 C21 H21 120.8 . . ? C23 C22 C21 120.1(7) . . ? C23 C22 H22 119.9 . . ? C21 C22 H22 119.9 . . ? N3 C23 C22 123.9(7) . . ? N3 C23 H23 118.1 . . ? C22 C23 H23 118.1 . . ? N4 C24 C15 125.2(6) . . ? N4 C24 C19 126.2(6) . . ? C15 C24 C19 108.6(6) . . ? N4 C24 Na1 50.7(3) . . ? C15 C24 Na1 168.0(5) . . ? C19 C24 Na1 76.5(4) . . ? S5 Hg2 S8 148.93(7) . . ? S5 Hg2 S7 139.88(7) . . ? S8 Hg2 S7 69.88(6) . . ? S5 Hg2 S6 66.89(6) . . ? S8 Hg2 S6 125.80(6) . . ? S7 Hg2 S6 100.88(6) . . ? C25 S5 Hg2 95.2(2) . . ? C25 S6 Hg2 80.8(2) . . ? C37 S7 Hg2 86.1(2) . . ? C37 S8 Hg2 88.7(2) . . ? C30 N5 C31 116.0(5) . . ? C30 N5 Na2 135.3(4) . . ? C31 N5 Na2 108.6(4) . . ? C35 N6 C36 115.7(6) . . ? C35 N6 Na2 139.3(5) . . ? C36 N6 Na2 105.0(4) . . ? C43 N8 C42 115.4(6) . . ? C43 N8 Na2 110.3(4) . 4_566 ? C42 N8 Na2 134.1(5) . 4_566 ? C47 N7 C48 115.1(6) . . ? C47 N7 Na2 138.7(5) . 4_566 ? C48 N7 Na2 106.1(5) . 4_566 ? C26 C25 S6 124.0(5) . . ? C26 C25 S5 119.7(5) . . ? S6 C25 S5 116.3(4) . . ? C25 C26 C32 126.8(6) . . ? C25 C26 C27 127.4(6) . . ? C32 C26 C27 105.8(5) . . ? C28 C27 C31 116.4(6) . . ? C28 C27 C26 135.0(6) . . ? C31 C27 C26 108.5(6) . . ? C29 C28 C27 117.9(6) . . ? C29 C28 H28 121.0 . . ? C27 C28 H28 121.0 . . ? C28 C29 C30 120.9(7) . . ? C28 C29 H29 119.6 . . ? C30 C29 H29 119.6 . . ? N5 C30 C29 122.7(6) . . ? N5 C30 H30 118.6 . . ? C29 C30 H30 118.6 . . ? N5 C31 C27 126.0(6) . . ? N5 C31 C36 125.4(6) . . ? C27 C31 C36 108.6(5) . . ? C33 C32 C36 115.3(6) . . ? C33 C32 C26 135.7(6) . . ? C36 C32 C26 109.0(6) . . ? C34 C33 C32 119.6(7) . . ? C34 C33 H33 120.2 . . ? C32 C33 H33 120.2 . . ? C33 C34 C35 119.5(7) . . ? C33 C34 H34 120.3 . . ? C35 C34 H34 120.3 . . ? N6 C35 C34 123.8(7) . . ? N6 C35 H35 118.1 . . ? C34 C35 H35 118.1 . . ? N6 C36 C32 126.2(6) . . ? N6 C36 C31 125.9(6) . . ? C32 C36 C31 107.9(5) . . ? C38 C37 S7 123.9(5) . . ? C38 C37 S8 121.6(5) . . ? S7 C37 S8 114.5(3) . . ? C37 C38 C44 128.3(6) . . ? C37 C38 C39 126.0(6) . . ? C44 C38 C39 105.7(5) . . ? C40 C39 C43 115.8(6) . . ? C40 C39 C38 135.3(6) . . ? C43 C39 C38 109.0(6) . . ? C41 C40 C39 117.4(6) . . ? C41 C40 H40 121.3 . . ? C39 C40 H40 121.3 . . ? C42 C41 C40 122.3(7) . . ? C42 C41 H41 118.8 . . ? C40 C41 H41 118.8 . . ? N8 C42 C41 122.9(7) . . ? N8 C42 H42 118.6 . . ? C41 C42 H42 118.6 . . ? N8 C43 C39 126.2(6) . . ? N8 C43 C48 125.4(6) . . ? C39 C43 C48 108.3(6) . . ? C45 C44 C48 115.4(6) . . ? C45 C44 C38 136.0(6) . . ? C48 C44 C38 108.6(6) . . ? C46 C45 C44 119.3(6) . . ? C46 C45 H45 120.4 . . ? C44 C45 H45 120.4 . . ? C45 C46 C47 119.8(7) . . ? C45 C46 H46 120.1 . . ? C47 C46 H46 120.1 . . ? N7 C47 C46 123.5(7) . . ? N7 C47 H47 118.2 . . ? C46 C47 H47 118.2 . . ? N7 C48 C44 126.8(7) . . ? N7 C48 C43 124.9(6) . . ? C44 C48 C43 108.3(6) . . ? S9A O1 S9B 51.1(4) . . ? S9A O1 Na1 147.7(5) . . ? S9B O1 Na1 98.9(5) . . ? O1 S9A C49 107.4(6) . . ? O1 S9A C50 106.4(6) . . ? C49 S9A C50 97.2(6) . . ? C49 S9B O1 108.1(9) . . ? C49 S9B C50 107.3(9) . . ? O1 S9B C50 95.8(7) . . ? C49 S9B Na1 137.2(7) . . ? O1 S9B Na1 46.9(3) . . ? C50 S9B Na1 109.2(6) . . ? S9B C49 S9A 51.5(6) . . ? S9A C50 S9B 46.2(5) . . ? O2 S10 C51 106.2(6) . . ? O2 S10 C52 105.3(6) . . ? C51 S10 C52 98.1(5) . . ? O2 S10 Na2 39.4(3) . . ? C51 S10 Na2 137.2(5) . . ? C52 S10 Na2 113.5(4) . . ? S10 O2 Na2 115.9(4) . . ? S10 C51 H51A 109.5 . . ? S10 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? S10 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? S10 C52 H52A 109.5 . . ? S10 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? S10 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C59 N9 C57 112.7(10) . . ? C59 N9 C53 105.5(9) . . ? C57 N9 C53 111.7(10) . . ? C59 N9 C55 110.9(10) . . ? C57 N9 C55 104.8(9) . . ? C53 N9 C55 111.3(10) . . ? N9 C53 C54 114.3(11) . . ? N9 C53 H53A 108.7 . . ? C54 C53 H53A 108.7 . . ? N9 C53 H53B 108.7 . . ? C54 C53 H53B 108.7 . . ? H53A C53 H53B 107.6 . . ? C53 C54 H54A 109.5 . . ? C53 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C53 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C56 C55 N9 115.2(11) . . ? C56 C55 H55A 108.5 . . ? N9 C55 H55A 108.5 . . ? C56 C55 H55B 108.5 . . ? N9 C55 H55B 108.5 . . ? H55A C55 H55B 107.5 . . ? C55 C56 H56A 109.5 . . ? C55 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C55 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? N9 C57 C58 114.6(10) . . ? N9 C57 H57A 108.6 . . ? C58 C57 H57A 108.6 . . ? N9 C57 H57B 108.6 . . ? C58 C57 H57B 108.6 . . ? H57A C57 H57B 107.6 . . ? C57 C58 H58A 109.5 . . ? C57 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? C57 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? N9 C59 C60 114.6(9) . . ? N9 C59 H59A 108.6 . . ? C60 C59 H59A 108.6 . . ? N9 C59 H59B 108.6 . . ? C60 C59 H59B 108.6 . . ? H59A C59 H59B 107.6 . . ? C59 C60 H60A 109.5 . . ? C59 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? C59 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? C61 N10 C67 119.3(11) . . ? C61 N10 C63 109.8(10) . . ? C67 N10 C63 107.5(9) . . ? C61 N10 C65 106.9(10) . . ? C67 N10 C65 103.2(9) . . ? C63 N10 C65 109.8(10) . . ? N10 C61 C62 125.0(14) . . ? N10 C61 H61A 106.1 . . ? C62 C61 H61A 106.1 . . ? N10 C61 H61B 106.1 . . ? C62 C61 H61B 106.1 . . ? H61A C61 H61B 106.3 . . ? C61 C62 H62A 109.5 . . ? C61 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C61 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? C64 C63 N10 123.1(13) . . ? C64 C63 H63A 106.5 . . ? N10 C63 H63A 106.5 . . ? C64 C63 H63B 106.5 . . ? N10 C63 H63B 106.5 . . ? H63A C63 H63B 106.5 . . ? C63 C64 H64A 109.5 . . ? C63 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? C63 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? C66 C65 N10 117.3(14) . . ? C66 C65 H65A 108.0 . . ? N10 C65 H65A 108.0 . . ? C66 C65 H65B 108.0 . . ? N10 C65 H65B 108.0 . . ? H65A C65 H65B 107.2 . . ? C65 C66 H66A 109.5 . . ? C65 C66 H66B 109.5 . . ? H66A C66 H66B 109.5 . . ? C65 C66 H66C 109.5 . . ? H66A C66 H66C 109.5 . . ? H66B C66 H66C 109.5 . . ? N10 C67 C68 116.5(11) . . ? N10 C67 H67A 108.2 . . ? C68 C67 H67A 108.2 . . ? N10 C67 H67B 108.2 . . ? C68 C67 H67B 108.2 . . ? H67A C67 H67B 107.3 . . ? C67 C68 H68A 109.5 . . ? C67 C68 H68B 109.5 . . ? H68A C68 H68B 109.5 . . ? C67 C68 H68C 109.5 . . ? H68A C68 H68C 109.5 . . ? H68B C68 H68C 109.5 . . ? O1 Na1 N3 90.8(3) . . ? O1 Na1 N1 103.7(3) . 4_576 ? N3 Na1 N1 99.5(2) . 4_576 ? O1 Na1 N4 104.7(2) . . ? N3 Na1 N4 75.4(2) . . ? N1 Na1 N4 151.1(2) 4_576 . ? O1 Na1 N2 113.0(3) . 4_576 ? N3 Na1 N2 156.1(3) . 4_576 ? N1 Na1 N2 74.7(2) 4_576 4_576 ? N4 Na1 N2 98.4(2) . 4_576 ? O1 Na1 S9B 34.2(3) . . ? N3 Na1 S9B 75.9(3) . . ? N1 Na1 S9B 76.1(3) 4_576 . ? N4 Na1 S9B 127.9(3) . . ? N2 Na1 S9B 123.3(3) 4_576 . ? O1 Na1 C19 90.1(2) . . ? N3 Na1 C19 24.81(18) . . ? N1 Na1 C19 123.6(2) 4_576 . ? N4 Na1 C19 51.78(18) . . ? N2 Na1 C19 147.3(2) 4_576 . ? S9B Na1 C19 88.9(3) . . ? O1 Na1 C24 95.8(2) . . ? N3 Na1 C24 51.13(19) . . ? N1 Na1 C24 145.2(2) 4_576 . ? N4 Na1 C24 25.30(18) . . ? N2 Na1 C24 123.4(2) 4_576 . ? S9B Na1 C24 108.1(3) . . ? C19 Na1 C24 26.76(18) . . ? O2 Na2 N5 97.1(3) . . ? O2 Na2 N8 91.9(3) . 4_565 ? N5 Na2 N8 169.2(2) . 4_565 ? O2 Na2 N6 87.4(3) . . ? N5 Na2 N6 74.3(2) . . ? N8 Na2 N6 112.2(2) 4_565 . ? O2 Na2 N7 133.2(3) . 4_565 ? N5 Na2 N7 96.3(2) . 4_565 ? N8 Na2 N7 73.1(2) 4_565 4_565 ? N6 Na2 N7 139.4(2) . 4_565 ? O2 Na2 S10 24.7(2) . . ? N5 Na2 S10 107.13(16) . . ? N8 Na2 S10 83.52(17) 4_565 . ? N6 Na2 S10 69.46(16) . . ? N7 Na2 S10 148.20(18) 4_565 . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.64 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 2.100 _refine_diff_density_min -1.916 _refine_diff_density_rms 0.222