Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _journal_volume ? _journal_year ? _journal_page_first ? _publ_contact_author_name 'J. Zaleski' _publ_contact_author_address ; Department of Chemistry Indiana University 800 E. Kirkwood Avenue Bloomington IN 47405-4001 UNITED STATES OF AMERICA ; _publ_contact_author_email ZALESKI@INDIANA.EDU _publ_section_title ; A geometric switching approach toward thermal activation of metalloenediynes ; _publ_author_name J.Zaleski data_03193 _database_code_depnum_ccdc_archive 'CCDC 268256' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H18 Cu N2 S2, P F6, 0.75 C H2 Cl2' _chemical_formula_sum 'C26.75 H19.50 Cl1.50 Cu F6 N2 P S2' _chemical_formula_weight 694.75 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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' Cu Cu 0.3201 1.2651 '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 11.893(3) _cell_length_b 15.257(4) _cell_length_c 16.966(4) _cell_angle_alpha 83.414(6) _cell_angle_beta 75.378(6) _cell_angle_gamma 68.398(5) _cell_volume 2768.9(12) _cell_formula_units_Z 4 _cell_measurement_temperature 130(2) _cell_measurement_reflns_used 8548 _cell_measurement_theta_min 5.0 _cell_measurement_theta_max 26.4 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.667 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1398 _exptl_absorpt_coefficient_mu 1.205 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8123 _exptl_absorpt_correction_T_max 0.8890 _exptl_absorpt_process_details 'SADABS, R. Blessing (1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 130(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_details '0.30 degree frames measured for 50 seconds each' _diffrn_measurement_method \w-scans _diffrn_measurement_device 'three-circle goniometer with fixed chi' _diffrn_measurement_device_type 'Bruker Platform goniometer' _diffrn_detector 'CCD area detector' _diffrn_detector_type 'Bruker SMART 6000' _diffrn_standards_number 358 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 954 _diffrn_standards_decay_% 0.0 _diffrn_reflns_number 57258 _diffrn_reflns_av_R_equivalents 0.0432 _diffrn_reflns_av_sigmaI/netI 0.0317 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.88 _diffrn_reflns_theta_max 26.44 _reflns_number_total 11339 _reflns_number_gt 8910 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2002)' _computing_cell_refinement 'SAINT (Bruker, 2002)' _computing_data_reduction 'SAINT (Bruker, 2002)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XTEL (local library)' _computing_publication_material 'XCIF (Bruker, 2002), XTEL (local library)' _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. Pseudo-symmetry (translation of the cation), systematically weak reflections. ; _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^)+(0.0865P)^2^+7.9609P] 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 11339 _refine_ls_number_parameters 731 _refine_ls_number_restraints 103 _refine_ls_R_factor_all 0.0697 _refine_ls_R_factor_gt 0.0541 _refine_ls_wR_factor_ref 0.1671 _refine_ls_wR_factor_gt 0.1532 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.034 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.34787(4) 0.83982(3) -0.03507(3) 0.02224(13) Uani 1 1 d D . . S1A S 0.42419(8) 0.83187(6) 0.07863(5) 0.01893(19) Uani 1 1 d D . . S2A S 0.28477(8) 0.96815(6) -0.11720(5) 0.01921(19) Uani 1 1 d D . . N1A N 0.4764(3) 0.7098(2) -0.06231(18) 0.0213(6) Uani 1 1 d D . . N2A N 0.1769(3) 0.8306(2) -0.01909(18) 0.0206(6) Uani 1 1 d D . . C1A C 0.5438(4) 0.8856(3) 0.0535(2) 0.0245(8) Uani 1 1 d D . . H1A H 0.5032 0.9549 0.0577 0.029 Uiso 1 1 calc R . . H1B H 0.5963 0.8635 0.0939 0.029 Uiso 1 1 calc R . . C2A C 0.6228(3) 0.8635(3) -0.0279(2) 0.0225(8) Uani 1 1 d D . . C3A C 0.6884(3) 0.8412(3) -0.0937(2) 0.0240(8) Uani 1 1 d D . . C4A C 0.7696(4) 0.8147(3) -0.1718(2) 0.0279(8) Uani 1 1 d D . . H4A H 0.8566 0.7882 -0.1756 0.033 Uiso 1 1 calc R . . C5A C 0.7281(4) 0.8258(3) -0.2399(2) 0.0271(8) Uani 1 1 d D . . H5A H 0.7864 0.8073 -0.2902 0.033 Uiso 1 1 calc R . . C6A C 0.5986(4) 0.8647(3) -0.2393(2) 0.0241(8) Uani 1 1 d D . . C7A C 0.4894(4) 0.8965(3) -0.2355(2) 0.0233(8) Uani 1 1 d D . . C8A C 0.3549(3) 0.9334(3) -0.2247(2) 0.0233(8) Uani 1 1 d D . . H8A H 0.3263 0.8846 -0.2376 0.028 Uiso 1 1 calc R . . H8B H 0.3298 0.9887 -0.2616 0.028 Uiso 1 1 calc R . . C9A C 0.5215(3) 0.7109(3) 0.0687(2) 0.0212(7) Uani 1 1 d D . . C10A C 0.5798(4) 0.6640(3) 0.1295(3) 0.0324(9) Uani 1 1 d D . . H10A H 0.5668 0.6962 0.1776 0.039 Uiso 1 1 calc R . . C11A C 0.6580(5) 0.5697(3) 0.1217(3) 0.0470(13) Uani 1 1 d D . . H11A H 0.6986 0.5385 0.1639 0.056 Uiso 1 1 calc R . . C12A C 0.6761(5) 0.5224(3) 0.0537(3) 0.0467(13) Uani 1 1 d D . . H12A H 0.7288 0.4581 0.0493 0.056 Uiso 1 1 calc R . . C13A C 0.6176(4) 0.5677(3) -0.0105(3) 0.0327(9) Uani 1 1 d D . . C14A C 0.6332(5) 0.5211(3) -0.0824(3) 0.0422(11) Uani 1 1 d D . . H14A H 0.6868 0.4572 -0.0902 0.051 Uiso 1 1 calc R . . C15A C 0.5704(5) 0.5692(3) -0.1403(3) 0.0391(11) Uani 1 1 d D . . H15A H 0.5795 0.5391 -0.1887 0.047 Uiso 1 1 calc R . . C16A C 0.4922(4) 0.6634(3) -0.1276(2) 0.0291(9) Uani 1 1 d D . . H16A H 0.4483 0.6955 -0.1682 0.035 Uiso 1 1 calc R . . C17A C 0.5383(3) 0.6632(3) -0.0030(2) 0.0216(7) Uani 1 1 d D . . C18A C 0.1327(3) 0.9667(2) -0.1093(2) 0.0174(7) Uani 1 1 d D . . C19A C 0.0525(3) 1.0333(3) -0.1509(2) 0.0206(7) Uani 1 1 d D . . H19A H 0.0781 1.0804 -0.1837 0.025 Uiso 1 1 calc R . . C20A C -0.0669(3) 1.0320(3) -0.1450(2) 0.0225(8) Uani 1 1 d D . . H20A H -0.1213 1.0778 -0.1742 0.027 Uiso 1 1 calc R . . C21A C -0.1048(3) 0.9651(3) -0.0975(2) 0.0226(8) Uani 1 1 d D . . H21A H -0.1859 0.9650 -0.0936 0.027 Uiso 1 1 calc R . . C22A C -0.0246(3) 0.8955(3) -0.0539(2) 0.0199(7) Uani 1 1 d D . . C23A C -0.0597(4) 0.8250(3) -0.0039(2) 0.0254(8) Uani 1 1 d D . . H23A H -0.1400 0.8224 0.0018 0.031 Uiso 1 1 calc R . . C24A C 0.0230(4) 0.7603(3) 0.0362(2) 0.0271(8) Uani 1 1 d D . . H24A H 0.0006 0.7127 0.0703 0.033 Uiso 1 1 calc R . . C25A C 0.1405(4) 0.7654(3) 0.0263(2) 0.0250(8) Uani 1 1 d D . . H25A H 0.1975 0.7194 0.0538 0.030 Uiso 1 1 calc R . . C26A C 0.0956(3) 0.8962(2) -0.0599(2) 0.0174(7) Uani 1 1 d D . . Cu2 Cu 0.33365(4) 0.82387(3) 0.47122(3) 0.02089(13) Uani 1 1 d D . . S1B S 0.41361(8) 0.82256(6) 0.58213(5) 0.01826(19) Uani 1 1 d D . . S2B S 0.28240(8) 0.95277(6) 0.38607(5) 0.01820(19) Uani 1 1 d D . . N1B N 0.4645(3) 0.6945(2) 0.44614(18) 0.0211(6) Uani 1 1 d D . . N2B N 0.1584(3) 0.8250(2) 0.48591(17) 0.0189(6) Uani 1 1 d D . . C1B C 0.5222(4) 0.8862(3) 0.5520(2) 0.0250(8) Uani 1 1 d D . . H1C H 0.4744 0.9547 0.5508 0.030 Uiso 1 1 calc R . . H1D H 0.5720 0.8740 0.5935 0.030 Uiso 1 1 calc R . . C2B C 0.6062(3) 0.8597(3) 0.4724(2) 0.0216(7) Uani 1 1 d D . . C3B C 0.6769(4) 0.8327(3) 0.4098(2) 0.0246(8) Uani 1 1 d D . . C4B C 0.7622(4) 0.8014(3) 0.3336(2) 0.0281(8) Uani 1 1 d D . . H4B H 0.8487 0.7759 0.3317 0.034 Uiso 1 1 calc R . . C5B C 0.7239(4) 0.8068(3) 0.2647(2) 0.0293(9) Uani 1 1 d D . . H5B H 0.7837 0.7853 0.2155 0.035 Uiso 1 1 calc R . . C6B C 0.5949(4) 0.8442(3) 0.2637(2) 0.0246(8) Uani 1 1 d D . . C7B C 0.4855(3) 0.8759(3) 0.2686(2) 0.0235(8) Uani 1 1 d D . . C8B C 0.3508(3) 0.9132(3) 0.2798(2) 0.0232(8) Uani 1 1 d D . . H8C H 0.3213 0.8637 0.2694 0.028 Uiso 1 1 calc R . . H8D H 0.3259 0.9668 0.2413 0.028 Uiso 1 1 calc R . . C9B C 0.5219(3) 0.7048(3) 0.5706(2) 0.0196(7) Uani 1 1 d D . . C10B C 0.5909(4) 0.6636(3) 0.6275(2) 0.0274(8) Uani 1 1 d D . . H10B H 0.5795 0.6980 0.6738 0.033 Uiso 1 1 calc R . . C11B C 0.6779(4) 0.5715(3) 0.6186(3) 0.0348(10) Uani 1 1 d D . . H11B H 0.7255 0.5443 0.6583 0.042 Uiso 1 1 calc R . . C12B C 0.6941(4) 0.5212(3) 0.5529(3) 0.0353(10) Uani 1 1 d D . . H12B H 0.7526 0.4586 0.5473 0.042 Uiso 1 1 calc R . . C13B C 0.6244(4) 0.5608(3) 0.4926(2) 0.0266(8) Uani 1 1 d D . . C14B C 0.6378(4) 0.5109(3) 0.4237(3) 0.0346(10) Uani 1 1 d D . . H14B H 0.6964 0.4486 0.4154 0.042 Uiso 1 1 calc R . . C15B C 0.5659(4) 0.5528(3) 0.3689(3) 0.0344(10) Uani 1 1 d D . . H15B H 0.5742 0.5202 0.3221 0.041 Uiso 1 1 calc R . . C16B C 0.4796(4) 0.6448(3) 0.3828(2) 0.0272(8) Uani 1 1 d D . . H16B H 0.4293 0.6728 0.3446 0.033 Uiso 1 1 calc R . . C17B C 0.5363(3) 0.6538(2) 0.5016(2) 0.0196(7) Uani 1 1 d D . . C18B C 0.1268(3) 0.9598(2) 0.3934(2) 0.0177(7) Uani 1 1 d D . . C19B C 0.0513(3) 1.0291(2) 0.3505(2) 0.0199(7) Uani 1 1 d D . . H19B H 0.0818 1.0741 0.3179 0.024 Uiso 1 1 calc R . . C20B C -0.0703(3) 1.0337(3) 0.3546(2) 0.0211(7) Uani 1 1 d D . . H20B H -0.1213 1.0813 0.3245 0.025 Uiso 1 1 calc R . . C21B C -0.1148(3) 0.9697(3) 0.4018(2) 0.0215(7) Uani 1 1 d D . . H21B H -0.1971 0.9733 0.4043 0.026 Uiso 1 1 calc R . . C22B C -0.0402(3) 0.8976(3) 0.4473(2) 0.0191(7) Uani 1 1 d D . . C23B C -0.0819(4) 0.8300(3) 0.4960(2) 0.0237(8) Uani 1 1 d D . . H23B H -0.1636 0.8312 0.5001 0.028 Uiso 1 1 calc R . . C24B C -0.0047(4) 0.7623(3) 0.5378(2) 0.0257(8) Uani 1 1 d D . . H24B H -0.0319 0.7161 0.5709 0.031 Uiso 1 1 calc R . . C25B C 0.1152(4) 0.7624(3) 0.5306(2) 0.0227(8) Uani 1 1 d D . . H25B H 0.1684 0.7149 0.5595 0.027 Uiso 1 1 calc R . . C26B C 0.0823(3) 0.8930(2) 0.4432(2) 0.0166(7) Uani 1 1 d D . . P1 P 0.17884(10) 0.69650(7) 0.26054(6) 0.0233(2) Uani 1 1 d . . . F1 F 0.2480(3) 0.7385(2) 0.18082(17) 0.0495(8) Uani 1 1 d . . . F2 F 0.2187(3) 0.7517(2) 0.3156(2) 0.0580(9) Uani 1 1 d . . . F3 F 0.1082(3) 0.6564(2) 0.33963(17) 0.0583(9) Uani 1 1 d . . . F4 F 0.1423(4) 0.6414(3) 0.2039(2) 0.0869(14) Uani 1 1 d . . . F5 F 0.0549(3) 0.7830(3) 0.2601(2) 0.0713(11) Uani 1 1 d . . . F6 F 0.3070(3) 0.6112(2) 0.2609(2) 0.0668(10) Uani 1 1 d . . . P2 P 0.19520(10) 0.69199(7) 0.76085(6) 0.0231(2) Uani 1 1 d . . . F7 F 0.2629(2) 0.7017(2) 0.66813(14) 0.0385(6) Uani 1 1 d . . . F8 F 0.2228(3) 0.7805(2) 0.78150(18) 0.0519(8) Uani 1 1 d . . . F9 F 0.1297(4) 0.6817(3) 0.85281(17) 0.0769(13) Uani 1 1 d . . . F10 F 0.1724(3) 0.6016(2) 0.74044(19) 0.0468(7) Uani 1 1 d . . . F11 F 0.0673(3) 0.7593(2) 0.7416(2) 0.0610(9) Uani 1 1 d . . . F12 F 0.3278(3) 0.6238(2) 0.7770(2) 0.0539(8) Uani 1 1 d . . . Cl1 Cl 0.0408(2) 0.49831(16) 0.59496(14) 0.0921(6) Uani 1 1 d D . . Cl2 Cl -0.11133(19) 0.59012(17) 0.74429(16) 0.1025(8) Uani 1 1 d D . . C1S C 0.0167(6) 0.4902(5) 0.7025(5) 0.080(2) Uani 1 1 d D . . H1SA H 0.0920 0.4879 0.7189 0.095 Uiso 1 1 calc R . . H1SB H -0.0002 0.4318 0.7231 0.095 Uiso 1 1 calc R . . Cl3 Cl -0.0203(16) 0.5089(10) 0.9518(8) 0.1116(18) Uiso 0.25 1 d PD A -1 Cl4 Cl 0.0379(12) 0.5133(9) 1.1038(8) 0.1116(18) Uiso 0.25 1 d PD A -1 C2S C 0.055(5) 0.4351(17) 1.027(2) 0.1116(18) Uiso 0.25 1 d PD A -1 H2SA H 0.1435 0.4011 1.0024 0.134 Uiso 0.25 1 calc PR A -1 H2SB H 0.0147 0.3883 1.0497 0.134 Uiso 0.25 1 calc PR A -1 Cl3D Cl 0.0093(17) 0.5190(10) 1.0628(9) 0.1116(18) Uiso 0.25 1 d PD B -2 Cl4D Cl 0.0367(12) 0.4505(8) 0.8976(8) 0.1116(18) Uiso 0.25 1 d PD B -2 C2D C -0.020(5) 0.5483(17) 0.9635(18) 0.1116(18) Uiso 0.25 1 d PD B -2 H2DA H 0.0195 0.5949 0.9378 0.134 Uiso 0.25 1 calc PR B -2 H2DB H -0.1102 0.5790 0.9687 0.134 Uiso 0.25 1 calc PR B -2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0174(2) 0.0277(3) 0.0183(2) -0.00476(18) -0.00759(18) -0.00047(19) S1A 0.0178(4) 0.0228(4) 0.0141(4) -0.0040(3) -0.0043(3) -0.0035(3) S2A 0.0176(4) 0.0236(4) 0.0167(4) -0.0051(3) -0.0046(3) -0.0057(3) N1A 0.0184(15) 0.0229(16) 0.0211(15) -0.0056(12) -0.0047(12) -0.0039(12) N2A 0.0206(15) 0.0234(16) 0.0151(14) -0.0049(12) -0.0046(12) -0.0031(13) C1A 0.031(2) 0.029(2) 0.0189(18) -0.0020(15) -0.0070(16) -0.0151(17) C2A 0.0233(18) 0.0253(19) 0.0224(19) -0.0007(15) -0.0080(15) -0.0109(15) C3A 0.0193(18) 0.029(2) 0.026(2) -0.0024(16) -0.0072(16) -0.0092(16) C4A 0.0178(18) 0.035(2) 0.028(2) -0.0060(17) -0.0012(15) -0.0076(16) C5A 0.0193(18) 0.034(2) 0.0230(19) -0.0071(16) 0.0035(15) -0.0070(16) C6A 0.027(2) 0.029(2) 0.0157(17) -0.0046(15) -0.0018(15) -0.0104(16) C7A 0.027(2) 0.0280(19) 0.0147(17) -0.0045(14) -0.0018(14) -0.0101(16) C8A 0.0232(19) 0.032(2) 0.0135(16) -0.0055(15) -0.0025(14) -0.0079(16) C9A 0.0218(18) 0.0213(18) 0.0185(17) 0.0009(14) -0.0044(14) -0.0058(15) C10A 0.042(2) 0.031(2) 0.023(2) 0.0017(17) -0.0118(18) -0.0084(19) C11A 0.063(3) 0.033(2) 0.038(3) 0.012(2) -0.026(2) -0.003(2) C12A 0.062(3) 0.022(2) 0.047(3) 0.005(2) -0.021(3) 0.000(2) C13A 0.040(2) 0.0204(19) 0.032(2) -0.0014(16) -0.0088(19) -0.0034(18) C14A 0.051(3) 0.021(2) 0.043(3) -0.0095(19) -0.007(2) 0.000(2) C15A 0.047(3) 0.033(2) 0.034(2) -0.0161(19) -0.005(2) -0.009(2) C16A 0.028(2) 0.033(2) 0.0232(19) -0.0104(17) -0.0066(16) -0.0048(17) C17A 0.0212(18) 0.0200(17) 0.0205(18) -0.0031(14) -0.0009(14) -0.0056(15) C18A 0.0170(16) 0.0186(17) 0.0157(16) -0.0060(13) -0.0054(13) -0.0025(14) C19A 0.0237(18) 0.0193(17) 0.0161(16) -0.0038(14) -0.0052(14) -0.0030(15) C20A 0.0221(18) 0.0207(18) 0.0220(18) -0.0063(14) -0.0098(15) 0.0006(15) C21A 0.0162(17) 0.0269(19) 0.0241(19) -0.0081(15) -0.0073(14) -0.0028(15) C22A 0.0180(17) 0.0227(18) 0.0181(17) -0.0074(14) -0.0027(14) -0.0050(14) C23A 0.026(2) 0.029(2) 0.0237(19) -0.0071(16) -0.0032(16) -0.0125(16) C24A 0.035(2) 0.0234(19) 0.0224(19) -0.0013(15) -0.0025(16) -0.0127(17) C25A 0.030(2) 0.0221(18) 0.0193(18) -0.0017(15) -0.0080(16) -0.0036(16) C26A 0.0190(17) 0.0173(16) 0.0135(16) -0.0073(13) -0.0044(13) -0.0013(13) Cu2 0.0163(2) 0.0252(2) 0.0168(2) -0.00270(17) -0.00669(17) 0.00027(18) S1B 0.0180(4) 0.0210(4) 0.0129(4) -0.0032(3) -0.0038(3) -0.0025(3) S2B 0.0161(4) 0.0231(4) 0.0140(4) -0.0034(3) -0.0032(3) -0.0046(3) N1B 0.0195(15) 0.0233(15) 0.0188(15) -0.0049(12) -0.0050(12) -0.0037(13) N2B 0.0190(15) 0.0202(15) 0.0145(14) -0.0044(12) -0.0045(12) -0.0019(12) C1B 0.030(2) 0.0270(19) 0.0199(18) -0.0035(15) -0.0037(16) -0.0121(17) C2B 0.0205(18) 0.0247(18) 0.0213(18) 0.0008(15) -0.0067(15) -0.0091(15) C3B 0.0218(18) 0.032(2) 0.0230(19) -0.0014(16) -0.0072(16) -0.0115(16) C4B 0.0166(18) 0.036(2) 0.028(2) -0.0057(17) -0.0016(15) -0.0061(16) C5B 0.0193(19) 0.040(2) 0.0220(19) -0.0091(17) 0.0036(15) -0.0059(17) C6B 0.025(2) 0.034(2) 0.0126(16) -0.0050(15) -0.0011(14) -0.0088(17) C7B 0.026(2) 0.030(2) 0.0133(16) -0.0046(14) -0.0003(14) -0.0095(16) C8B 0.0219(18) 0.031(2) 0.0142(17) -0.0047(15) -0.0029(14) -0.0063(16) C9B 0.0171(17) 0.0226(18) 0.0168(17) -0.0007(14) -0.0035(14) -0.0046(14) C10B 0.026(2) 0.032(2) 0.0232(19) 0.0028(16) -0.0095(16) -0.0075(17) C11B 0.031(2) 0.034(2) 0.034(2) 0.0099(19) -0.0157(19) -0.0023(19) C12B 0.032(2) 0.022(2) 0.041(2) 0.0039(18) -0.0098(19) 0.0024(17) C13B 0.0233(19) 0.0222(19) 0.028(2) -0.0018(15) -0.0022(16) -0.0024(16) C14B 0.033(2) 0.022(2) 0.039(2) -0.0083(17) -0.0040(19) 0.0019(17) C15B 0.038(2) 0.035(2) 0.029(2) -0.0162(18) -0.0043(18) -0.0089(19) C16B 0.029(2) 0.030(2) 0.0215(19) -0.0091(16) -0.0064(16) -0.0059(17) C17B 0.0168(17) 0.0197(17) 0.0201(17) -0.0007(14) -0.0028(14) -0.0048(14) C18B 0.0164(16) 0.0211(17) 0.0136(16) -0.0063(13) -0.0043(13) -0.0019(14) C19B 0.0233(18) 0.0185(17) 0.0148(16) -0.0029(13) -0.0054(14) -0.0026(14) C20B 0.0215(18) 0.0191(17) 0.0183(17) -0.0041(14) -0.0107(14) 0.0031(14) C21B 0.0186(17) 0.0246(18) 0.0210(18) -0.0067(14) -0.0086(14) -0.0029(15) C22B 0.0191(17) 0.0225(18) 0.0152(16) -0.0079(14) -0.0049(14) -0.0038(14) C23B 0.0231(19) 0.0270(19) 0.0238(19) -0.0032(15) -0.0080(15) -0.0096(16) C24B 0.033(2) 0.0223(19) 0.0221(19) 0.0022(15) -0.0083(16) -0.0104(16) C25B 0.029(2) 0.0206(18) 0.0178(17) 0.0005(14) -0.0103(15) -0.0048(15) C26B 0.0175(16) 0.0176(16) 0.0118(15) -0.0076(13) -0.0039(13) -0.0002(13) P1 0.0324(5) 0.0225(5) 0.0168(4) 0.0000(4) -0.0076(4) -0.0107(4) F1 0.0384(15) 0.074(2) 0.0375(15) 0.0207(14) -0.0080(12) -0.0282(15) F2 0.0533(18) 0.067(2) 0.062(2) -0.0359(17) -0.0072(16) -0.0248(16) F3 0.081(2) 0.073(2) 0.0283(14) 0.0171(14) -0.0078(15) -0.0444(19) F4 0.123(3) 0.134(4) 0.049(2) -0.030(2) -0.001(2) -0.101(3) F5 0.0274(15) 0.075(2) 0.086(3) 0.041(2) -0.0108(16) -0.0026(15) F6 0.071(2) 0.0323(16) 0.062(2) 0.0021(14) -0.0058(18) 0.0140(15) P2 0.0328(5) 0.0188(5) 0.0165(5) -0.0020(4) -0.0035(4) -0.0085(4) F7 0.0376(14) 0.0583(17) 0.0208(12) -0.0007(11) -0.0015(10) -0.0220(13) F8 0.080(2) 0.0342(15) 0.0483(17) -0.0126(13) -0.0066(16) -0.0302(15) F9 0.138(4) 0.062(2) 0.0225(14) -0.0037(14) 0.0215(18) -0.051(2) F10 0.0469(16) 0.0401(15) 0.0605(18) -0.0167(13) -0.0047(14) -0.0242(13) F11 0.0248(14) 0.0486(18) 0.092(3) 0.0146(17) -0.0051(15) -0.0026(13) F12 0.063(2) 0.0370(15) 0.072(2) 0.0128(14) -0.0481(17) -0.0123(14) Cl1 0.0837(13) 0.0981(15) 0.0933(14) -0.0014(11) 0.0091(11) -0.0504(12) Cl2 0.0694(12) 0.0999(15) 0.144(2) -0.0574(15) -0.0075(12) -0.0314(11) C1S 0.064(4) 0.062(4) 0.118(6) -0.025(4) 0.003(4) -0.037(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 Cu1 N1A 2.027(3) . ? Cu1 N2A 2.038(3) . ? Cu1 S2A 2.2713(11) . ? Cu1 S1A 2.3041(10) . ? S1A C9A 1.781(4) . ? S1A C1A 1.831(4) . ? S2A C18A 1.788(4) . ? S2A C8A 1.852(4) . ? N1A C16A 1.320(5) . ? N1A C17A 1.372(5) . ? N2A C25A 1.320(5) . ? N2A C26A 1.373(4) . ? C1A C2A 1.457(5) . ? C1A H1A 0.9900 . ? C1A H1B 0.9900 . ? C2A C3A 1.192(5) . ? C3A C4A 1.429(5) . ? C4A C5A 1.337(6) . ? C4A H4A 0.9500 . ? C5A C6A 1.430(5) . ? C5A H5A 0.9500 . ? C6A C7A 1.195(5) . ? C7A C8A 1.456(5) . ? C8A H8A 0.9900 . ? C8A H8B 0.9900 . ? C9A C10A 1.373(5) . ? C9A C17A 1.422(5) . ? C10A C11A 1.396(6) . ? C10A H10A 0.9500 . ? C11A C12A 1.359(7) . ? C11A H11A 0.9500 . ? C12A C13A 1.416(6) . ? C12A H12A 0.9500 . ? C13A C17A 1.415(5) . ? C13A C14A 1.419(6) . ? C14A C15A 1.365(7) . ? C14A H14A 0.9500 . ? C15A C16A 1.400(6) . ? C15A H15A 0.9500 . ? C16A H16A 0.9500 . ? C18A C19A 1.378(5) . ? C18A C26A 1.417(5) . ? C19A C20A 1.405(5) . ? C19A H19A 0.9500 . ? C20A C21A 1.365(5) . ? C20A H20A 0.9500 . ? C21A C22A 1.420(5) . ? C21A H21A 0.9500 . ? C22A C23A 1.411(5) . ? C22A C26A 1.411(5) . ? C23A C24A 1.369(6) . ? C23A H23A 0.9500 . ? C24A C25A 1.395(6) . ? C24A H24A 0.9500 . ? C25A H25A 0.9500 . ? Cu2 N1B 2.023(3) . ? Cu2 N2B 2.030(3) . ? Cu2 S2B 2.2883(11) . ? Cu2 S1B 2.3079(10) . ? S1B C9B 1.782(4) . ? S1B C1B 1.830(4) . ? S2B C18B 1.787(4) . ? S2B C8B 1.851(4) . ? N1B C16B 1.325(5) . ? N1B C17B 1.372(5) . ? N2B C25B 1.323(5) . ? N2B C26B 1.374(4) . ? C1B C2B 1.459(5) . ? C1B H1C 0.9900 . ? C1B H1D 0.9900 . ? C2B C3B 1.184(5) . ? C3B C4B 1.433(5) . ? C4B C5B 1.341(6) . ? C4B H4B 0.9500 . ? C5B C6B 1.430(5) . ? C5B H5B 0.9500 . ? C6B C7B 1.194(5) . ? C7B C8B 1.458(5) . ? C8B H8C 0.9900 . ? C8B H8D 0.9900 . ? C9B C10B 1.372(5) . ? C9B C17B 1.419(5) . ? C10B C11B 1.402(6) . ? C10B H10B 0.9500 . ? C11B C12B 1.359(6) . ? C11B H11B 0.9500 . ? C12B C13B 1.420(6) . ? C12B H12B 0.9500 . ? C13B C14B 1.412(6) . ? C13B C17B 1.417(5) . ? C14B C15B 1.366(6) . ? C14B H14B 0.9500 . ? C15B C16B 1.404(6) . ? C15B H15B 0.9500 . ? C16B H16B 0.9500 . ? C18B C19B 1.381(5) . ? C18B C26B 1.416(5) . ? C19B C20B 1.406(5) . ? C19B H19B 0.9500 . ? C20B C21B 1.365(5) . ? C20B H20B 0.9500 . ? C21B C22B 1.423(5) . ? C21B H21B 0.9500 . ? C22B C23B 1.404(5) . ? C22B C26B 1.417(5) . ? C23B C24B 1.369(5) . ? C23B H23B 0.9500 . ? C24B C25B 1.401(5) . ? C24B H24B 0.9500 . ? C25B H25B 0.9500 . ? P1 F4 1.576(3) . ? P1 F5 1.577(3) . ? P1 F3 1.582(3) . ? P1 F2 1.583(3) . ? P1 F1 1.595(3) . ? P1 F6 1.600(3) . ? P2 F9 1.577(3) . ? P2 F11 1.581(3) . ? P2 F10 1.590(3) . ? P2 F7 1.594(3) . ? P2 F8 1.596(3) . ? P2 F12 1.609(3) . ? Cl1 C1S 1.771(8) . ? Cl2 C1S 1.772(7) . ? C1S H1SA 0.9900 . ? C1S H1SB 0.9900 . ? Cl3 C2S 1.782(18) . ? Cl4 C2S 1.797(17) . ? C2S H2SA 0.9900 . ? C2S H2SB 0.9900 . ? Cl3D C2D 1.778(18) . ? Cl4D C2D 1.787(9) . ? C2D H2DA 0.9900 . ? C2D H2DB 0.9900 . ? 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 N1A Cu1 N2A 107.77(12) . . ? N1A Cu1 S2A 130.26(9) . . ? N2A Cu1 S2A 87.62(9) . . ? N1A Cu1 S1A 87.40(9) . . ? N2A Cu1 S1A 118.29(9) . . ? S2A Cu1 S1A 127.02(4) . . ? C9A S1A C1A 99.23(18) . . ? C9A S1A Cu1 95.57(12) . . ? C1A S1A Cu1 108.85(12) . . ? C18A S2A C8A 99.35(16) . . ? C18A S2A Cu1 96.72(12) . . ? C8A S2A Cu1 108.74(13) . . ? C16A N1A C17A 118.5(3) . . ? C16A N1A Cu1 124.3(3) . . ? C17A N1A Cu1 116.5(2) . . ? C25A N2A C26A 118.4(3) . . ? C25A N2A Cu1 124.6(3) . . ? C26A N2A Cu1 117.0(2) . . ? C2A C1A S1A 113.0(3) . . ? C2A C1A H1A 109.0 . . ? S1A C1A H1A 109.0 . . ? C2A C1A H1B 109.0 . . ? S1A C1A H1B 109.0 . . ? H1A C1A H1B 107.8 . . ? C3A C2A C1A 177.1(4) . . ? C2A C3A C4A 178.6(4) . . ? C5A C4A C3A 122.6(4) . . ? C5A C4A H4A 118.7 . . ? C3A C4A H4A 118.7 . . ? C4A C5A C6A 122.1(4) . . ? C4A C5A H5A 118.9 . . ? C6A C5A H5A 118.9 . . ? C7A C6A C5A 177.3(4) . . ? C6A C7A C8A 175.9(4) . . ? C7A C8A S2A 108.1(3) . . ? C7A C8A H8A 110.1 . . ? S2A C8A H8A 110.1 . . ? C7A C8A H8B 110.1 . . ? S2A C8A H8B 110.1 . . ? H8A C8A H8B 108.4 . . ? C10A C9A C17A 120.2(3) . . ? C10A C9A S1A 120.5(3) . . ? C17A C9A S1A 119.4(3) . . ? C9A C10A C11A 120.9(4) . . ? C9A C10A H10A 119.6 . . ? C11A C10A H10A 119.6 . . ? C12A C11A C10A 120.2(4) . . ? C12A C11A H11A 119.9 . . ? C10A C11A H11A 119.9 . . ? C11A C12A C13A 120.9(4) . . ? C11A C12A H12A 119.5 . . ? C13A C12A H12A 119.5 . . ? C17A C13A C12A 119.1(4) . . ? C17A C13A C14A 117.9(4) . . ? C12A C13A C14A 123.0(4) . . ? C15A C14A C13A 119.2(4) . . ? C15A C14A H14A 120.4 . . ? C13A C14A H14A 120.4 . . ? C14A C15A C16A 119.4(4) . . ? C14A C15A H15A 120.3 . . ? C16A C15A H15A 120.3 . . ? N1A C16A C15A 123.4(4) . . ? N1A C16A H16A 118.3 . . ? C15A C16A H16A 118.3 . . ? N1A C17A C13A 121.6(3) . . ? N1A C17A C9A 119.8(3) . . ? C13A C17A C9A 118.6(3) . . ? C19A C18A C26A 120.4(3) . . ? C19A C18A S2A 120.4(3) . . ? C26A C18A S2A 119.2(3) . . ? C18A C19A C20A 120.5(3) . . ? C18A C19A H19A 119.8 . . ? C20A C19A H19A 119.8 . . ? C21A C20A C19A 120.2(3) . . ? C21A C20A H20A 119.9 . . ? C19A C20A H20A 119.9 . . ? C20A C21A C22A 120.8(3) . . ? C20A C21A H21A 119.6 . . ? C22A C21A H21A 119.6 . . ? C23A C22A C26A 117.9(3) . . ? C23A C22A C21A 122.9(3) . . ? C26A C22A C21A 119.1(3) . . ? C24A C23A C22A 119.4(4) . . ? C24A C23A H23A 120.3 . . ? C22A C23A H23A 120.3 . . ? C23A C24A C25A 119.1(4) . . ? C23A C24A H24A 120.4 . . ? C25A C24A H24A 120.4 . . ? N2A C25A C24A 123.5(4) . . ? N2A C25A H25A 118.2 . . ? C24A C25A H25A 118.2 . . ? N2A C26A C22A 121.6(3) . . ? N2A C26A C18A 119.5(3) . . ? C22A C26A C18A 119.0(3) . . ? N1B Cu2 N2B 112.86(12) . . ? N1B Cu2 S2B 129.04(9) . . ? N2B Cu2 S2B 87.45(9) . . ? N1B Cu2 S1B 87.20(9) . . ? N2B Cu2 S1B 121.10(9) . . ? S2B Cu2 S1B 122.70(4) . . ? C9B S1B C1B 99.20(18) . . ? C9B S1B Cu2 96.01(12) . . ? C1B S1B Cu2 107.61(13) . . ? C18B S2B C8B 98.94(16) . . ? C18B S2B Cu2 96.49(12) . . ? C8B S2B Cu2 108.16(13) . . ? C16B N1B C17B 118.3(3) . . ? C16B N1B Cu2 124.2(3) . . ? C17B N1B Cu2 117.3(2) . . ? C25B N2B C26B 118.4(3) . . ? C25B N2B Cu2 124.4(2) . . ? C26B N2B Cu2 117.2(2) . . ? C2B C1B S1B 113.3(3) . . ? C2B C1B H1C 108.9 . . ? S1B C1B H1C 108.9 . . ? C2B C1B H1D 108.9 . . ? S1B C1B H1D 108.9 . . ? H1C C1B H1D 107.7 . . ? C3B C2B C1B 176.0(4) . . ? C2B C3B C4B 179.2(4) . . ? C5B C4B C3B 122.1(4) . . ? C5B C4B H4B 118.9 . . ? C3B C4B H4B 118.9 . . ? C4B C5B C6B 121.5(3) . . ? C4B C5B H5B 119.3 . . ? C6B C5B H5B 119.3 . . ? C7B C6B C5B 175.5(4) . . ? C6B C7B C8B 176.5(4) . . ? C7B C8B S2B 107.8(3) . . ? C7B C8B H8C 110.1 . . ? S2B C8B H8C 110.1 . . ? C7B C8B H8D 110.1 . . ? S2B C8B H8D 110.1 . . ? H8C C8B H8D 108.5 . . ? C10B C9B C17B 120.1(3) . . ? C10B C9B S1B 120.6(3) . . ? C17B C9B S1B 119.3(3) . . ? C9B C10B C11B 121.3(4) . . ? C9B C10B H10B 119.4 . . ? C11B C10B H10B 119.4 . . ? C12B C11B C10B 119.8(4) . . ? C12B C11B H11B 120.1 . . ? C10B C11B H11B 120.1 . . ? C11B C12B C13B 120.8(4) . . ? C11B C12B H12B 119.6 . . ? C13B C12B H12B 119.6 . . ? C14B C13B C17B 117.9(4) . . ? C14B C13B C12B 122.7(4) . . ? C17B C13B C12B 119.4(4) . . ? C15B C14B C13B 119.6(4) . . ? C15B C14B H14B 120.2 . . ? C13B C14B H14B 120.2 . . ? C14B C15B C16B 119.0(4) . . ? C14B C15B H15B 120.5 . . ? C16B C15B H15B 120.5 . . ? N1B C16B C15B 123.5(4) . . ? N1B C16B H16B 118.2 . . ? C15B C16B H16B 118.2 . . ? N1B C17B C13B 121.7(3) . . ? N1B C17B C9B 119.8(3) . . ? C13B C17B C9B 118.5(3) . . ? C19B C18B C26B 120.5(3) . . ? C19B C18B S2B 120.3(3) . . ? C26B C18B S2B 119.1(3) . . ? C18B C19B C20B 120.6(3) . . ? C18B C19B H19B 119.7 . . ? C20B C19B H19B 119.7 . . ? C21B C20B C19B 119.9(3) . . ? C21B C20B H20B 120.1 . . ? C19B C20B H20B 120.1 . . ? C20B C21B C22B 121.2(3) . . ? C20B C21B H21B 119.4 . . ? C22B C21B H21B 119.4 . . ? C23B C22B C26B 118.1(3) . . ? C23B C22B C21B 123.0(3) . . ? C26B C22B C21B 118.9(3) . . ? C24B C23B C22B 119.8(4) . . ? C24B C23B H23B 120.1 . . ? C22B C23B H23B 120.1 . . ? C23B C24B C25B 118.7(4) . . ? C23B C24B H24B 120.6 . . ? C25B C24B H24B 120.6 . . ? N2B C25B C24B 123.6(3) . . ? N2B C25B H25B 118.2 . . ? C24B C25B H25B 118.2 . . ? N2B C26B C18B 119.8(3) . . ? N2B C26B C22B 121.4(3) . . ? C18B C26B C22B 118.9(3) . . ? F4 P1 F5 90.1(3) . . ? F4 P1 F3 91.31(19) . . ? F5 P1 F3 88.86(19) . . ? F4 P1 F2 178.5(2) . . ? F5 P1 F2 90.7(2) . . ? F3 P1 F2 89.99(18) . . ? F4 P1 F1 88.76(18) . . ? F5 P1 F1 90.17(17) . . ? F3 P1 F1 179.0(2) . . ? F2 P1 F1 89.95(18) . . ? F4 P1 F6 91.5(2) . . ? F5 P1 F6 178.0(2) . . ? F3 P1 F6 92.30(19) . . ? F2 P1 F6 87.8(2) . . ? F1 P1 F6 88.66(18) . . ? F9 P2 F11 90.9(2) . . ? F9 P2 F10 89.55(18) . . ? F11 P2 F10 91.24(18) . . ? F9 P2 F7 179.4(2) . . ? F11 P2 F7 89.75(17) . . ? F10 P2 F7 90.50(16) . . ? F9 P2 F8 90.72(18) . . ? F11 P2 F8 90.67(19) . . ? F10 P2 F8 178.06(19) . . ? F7 P2 F8 89.21(15) . . ? F9 P2 F12 91.3(2) . . ? F11 P2 F12 177.87(19) . . ? F10 P2 F12 88.71(16) . . ? F7 P2 F12 88.12(17) . . ? F8 P2 F12 89.36(17) . . ? Cl1 C1S Cl2 108.7(4) . . ? Cl1 C1S H1SA 110.0 . . ? Cl2 C1S H1SA 110.0 . . ? Cl1 C1S H1SB 110.0 . . ? Cl2 C1S H1SB 110.0 . . ? H1SA C1S H1SB 108.3 . . ? Cl3 C2S Cl4 105.4(14) . . ? Cl3 C2S H2SA 110.7 . . ? Cl4 C2S H2SA 110.7 . . ? Cl3 C2S H2SB 110.7 . . ? Cl4 C2S H2SB 110.7 . . ? H2SA C2S H2SB 108.8 . . ? Cl3D C2D Cl4D 114.7(15) . . ? Cl3D C2D H2DA 108.6 . . ? Cl4D C2D H2DA 108.6 . . ? Cl3D C2D H2DB 108.6 . . ? Cl4D C2D H2DB 108.6 . . ? H2DA C2D H2DB 107.6 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1A Cu1 S1A C9A -9.07(15) . . . . ? N2A Cu1 S1A C9A 99.74(16) . . . . ? S2A Cu1 S1A C9A -149.97(12) . . . . ? N1A Cu1 S1A C1A 92.68(17) . . . . ? N2A Cu1 S1A C1A -158.51(17) . . . . ? S2A Cu1 S1A C1A -48.22(15) . . . . ? N1A Cu1 S2A C18A 110.62(16) . . . . ? N2A Cu1 S2A C18A -0.79(14) . . . . ? S1A Cu1 S2A C18A -125.03(11) . . . . ? N1A Cu1 S2A C8A 8.34(18) . . . . ? N2A Cu1 S2A C8A -103.06(15) . . . . ? S1A Cu1 S2A C8A 132.69(13) . . . . ? N2A Cu1 N1A C16A 62.5(3) . . . . ? S2A Cu1 N1A C16A -39.9(4) . . . . ? S1A Cu1 N1A C16A -178.6(3) . . . . ? N2A Cu1 N1A C17A -108.5(3) . . . . ? S2A Cu1 N1A C17A 149.2(2) . . . . ? S1A Cu1 N1A C17A 10.5(3) . . . . ? N1A Cu1 N2A C25A 48.1(3) . . . . ? S2A Cu1 N2A C25A 179.8(3) . . . . ? S1A Cu1 N2A C25A -48.7(3) . . . . ? N1A Cu1 N2A C26A -130.7(2) . . . . ? S2A Cu1 N2A C26A 1.0(2) . . . . ? S1A Cu1 N2A C26A 132.5(2) . . . . ? C9A S1A C1A C2A 60.0(3) . . . . ? Cu1 S1A C1A C2A -39.2(3) . . . . ? S1A C1A C2A C3A -54(8) . . . . ? C1A C2A C3A C4A -99(20) . . . . ? C2A C3A C4A C5A -154(19) . . . . ? C3A C4A C5A C6A -0.3(7) . . . . ? C4A C5A C6A C7A -18(9) . . . . ? C5A C6A C7A C8A -2(14) . . . . ? C6A C7A C8A S2A 26(6) . . . . ? C18A S2A C8A C7A -159.1(3) . . . . ? Cu1 S2A C8A C7A -58.7(3) . . . . ? C1A S1A C9A C10A 78.5(4) . . . . ? Cu1 S1A C9A C10A -171.4(3) . . . . ? C1A S1A C9A C17A -101.5(3) . . . . ? Cu1 S1A C9A C17A 8.7(3) . . . . ? C17A C9A C10A C11A 1.1(7) . . . . ? S1A C9A C10A C11A -178.8(4) . . . . ? C9A C10A C11A C12A -0.9(8) . . . . ? C10A C11A C12A C13A 0.7(9) . . . . ? C11A C12A C13A C17A -0.6(8) . . . . ? C11A C12A C13A C14A -179.7(5) . . . . ? C17A C13A C14A C15A -1.1(7) . . . . ? C12A C13A C14A C15A 178.0(5) . . . . ? C13A C14A C15A C16A 0.2(8) . . . . ? C17A N1A C16A C15A -0.9(6) . . . . ? Cu1 N1A C16A C15A -171.6(3) . . . . ? C14A C15A C16A N1A 0.9(7) . . . . ? C16A N1A C17A C13A -0.1(6) . . . . ? Cu1 N1A C17A C13A 171.3(3) . . . . ? C16A N1A C17A C9A -178.9(4) . . . . ? Cu1 N1A C17A C9A -7.5(4) . . . . ? C12A C13A C17A N1A -178.1(4) . . . . ? C14A C13A C17A N1A 1.1(6) . . . . ? C12A C13A C17A C9A 0.7(6) . . . . ? C14A C13A C17A C9A 179.9(4) . . . . ? C10A C9A C17A N1A 177.8(4) . . . . ? S1A C9A C17A N1A -2.2(5) . . . . ? C10A C9A C17A C13A -1.0(6) . . . . ? S1A C9A C17A C13A 178.9(3) . . . . ? C8A S2A C18A C19A -69.0(3) . . . . ? Cu1 S2A C18A C19A -179.3(3) . . . . ? C8A S2A C18A C26A 111.0(3) . . . . ? Cu1 S2A C18A C26A 0.7(3) . . . . ? C26A C18A C19A C20A -0.2(5) . . . . ? S2A C18A C19A C20A 179.7(3) . . . . ? C18A C19A C20A C21A 0.5(5) . . . . ? C19A C20A C21A C22A -0.5(5) . . . . ? C20A C21A C22A C23A 179.9(3) . . . . ? C20A C21A C22A C26A 0.2(5) . . . . ? C26A C22A C23A C24A -0.3(5) . . . . ? C21A C22A C23A C24A -180.0(3) . . . . ? C22A C23A C24A C25A -0.4(6) . . . . ? C26A N2A C25A C24A -1.0(5) . . . . ? Cu1 N2A C25A C24A -179.8(3) . . . . ? C23A C24A C25A N2A 1.1(6) . . . . ? C25A N2A C26A C22A 0.3(5) . . . . ? Cu1 N2A C26A C22A 179.2(2) . . . . ? C25A N2A C26A C18A -179.8(3) . . . . ? Cu1 N2A C26A C18A -0.9(4) . . . . ? C23A C22A C26A N2A 0.3(5) . . . . ? C21A C22A C26A N2A -180.0(3) . . . . ? C23A C22A C26A C18A -179.6(3) . . . . ? C21A C22A C26A C18A 0.1(5) . . . . ? C19A C18A C26A N2A 180.0(3) . . . . ? S2A C18A C26A N2A 0.0(4) . . . . ? C19A C18A C26A C22A -0.1(5) . . . . ? S2A C18A C26A C22A 180.0(3) . . . . ? N1B Cu2 S1B C9B -5.19(15) . . . . ? N2B Cu2 S1B C9B 109.94(15) . . . . ? S2B Cu2 S1B C9B -141.07(12) . . . . ? N1B Cu2 S1B C1B 96.47(16) . . . . ? N2B Cu2 S1B C1B -148.40(17) . . . . ? S2B Cu2 S1B C1B -39.41(14) . . . . ? N1B Cu2 S2B C18B 117.02(16) . . . . ? N2B Cu2 S2B C18B -0.66(13) . . . . ? S1B Cu2 S2B C18B -126.52(11) . . . . ? N1B Cu2 S2B C8B 15.37(18) . . . . ? N2B Cu2 S2B C8B -102.31(15) . . . . ? S1B Cu2 S2B C8B 131.84(13) . . . . ? N2B Cu2 N1B C16B 58.5(3) . . . . ? S2B Cu2 N1B C16B -47.7(4) . . . . ? S1B Cu2 N1B C16B -178.8(3) . . . . ? N2B Cu2 N1B C17B -117.0(3) . . . . ? S2B Cu2 N1B C17B 136.7(2) . . . . ? S1B Cu2 N1B C17B 5.7(3) . . . . ? N1B Cu2 N2B C25B 46.4(3) . . . . ? S2B Cu2 N2B C25B 178.1(3) . . . . ? S1B Cu2 N2B C25B -54.7(3) . . . . ? N1B Cu2 N2B C26B -130.4(2) . . . . ? S2B Cu2 N2B C26B 1.3(2) . . . . ? S1B Cu2 N2B C26B 128.5(2) . . . . ? C9B S1B C1B C2B 53.9(3) . . . . ? Cu2 S1B C1B C2B -45.5(3) . . . . ? S1B C1B C2B C3B -61(6) . . . . ? C1B C2B C3B C4B -167(100) . . . . ? C2B C3B C4B C5B -74(31) . . . . ? C3B C4B C5B C6B -0.2(7) . . . . ? C4B C5B C6B C7B -5(6) . . . . ? C5B C6B C7B C8B -16(12) . . . . ? C6B C7B C8B S2B 27(7) . . . . ? C18B S2B C8B C7B -163.2(3) . . . . ? Cu2 S2B C8B C7B -63.3(3) . . . . ? C1B S1B C9B C10B 76.3(3) . . . . ? Cu2 S1B C9B C10B -174.8(3) . . . . ? C1B S1B C9B C17B -103.7(3) . . . . ? Cu2 S1B C9B C17B 5.3(3) . . . . ? C17B C9B C10B C11B 1.0(6) . . . . ? S1B C9B C10B C11B -179.0(3) . . . . ? C9B C10B C11B C12B -0.7(7) . . . . ? C10B C11B C12B C13B 0.5(7) . . . . ? C11B C12B C13B C14B -179.7(4) . . . . ? C11B C12B C13B C17B -0.6(7) . . . . ? C17B C13B C14B C15B -0.5(6) . . . . ? C12B C13B C14B C15B 178.6(4) . . . . ? C13B C14B C15B C16B -0.3(7) . . . . ? C17B N1B C16B C15B -0.5(6) . . . . ? Cu2 N1B C16B C15B -176.0(3) . . . . ? C14B C15B C16B N1B 0.8(7) . . . . ? C16B N1B C17B C13B -0.3(5) . . . . ? Cu2 N1B C17B C13B 175.5(3) . . . . ? C16B N1B C17B C9B -179.5(3) . . . . ? Cu2 N1B C17B C9B -3.7(4) . . . . ? C14B C13B C17B N1B 0.8(6) . . . . ? C12B C13B C17B N1B -178.3(4) . . . . ? C14B C13B C17B C9B -180.0(4) . . . . ? C12B C13B C17B C9B 0.8(6) . . . . ? C10B C9B C17B N1B 178.1(3) . . . . ? S1B C9B C17B N1B -1.9(5) . . . . ? C10B C9B C17B C13B -1.1(5) . . . . ? S1B C9B C17B C13B 178.9(3) . . . . ? C8B S2B C18B C19B -69.8(3) . . . . ? Cu2 S2B C18B C19B -179.4(3) . . . . ? C8B S2B C18B C26B 109.7(3) . . . . ? Cu2 S2B C18B C26B 0.1(3) . . . . ? C26B C18B C19B C20B -0.9(5) . . . . ? S2B C18B C19B C20B 178.5(3) . . . . ? C18B C19B C20B C21B 0.5(5) . . . . ? C19B C20B C21B C22B -0.1(5) . . . . ? C20B C21B C22B C23B -179.5(3) . . . . ? C20B C21B C22B C26B 0.1(5) . . . . ? C26B C22B C23B C24B 0.0(5) . . . . ? C21B C22B C23B C24B 179.6(3) . . . . ? C22B C23B C24B C25B 0.0(6) . . . . ? C26B N2B C25B C24B -0.9(5) . . . . ? Cu2 N2B C25B C24B -177.6(3) . . . . ? C23B C24B C25B N2B 0.4(6) . . . . ? C25B N2B C26B C18B -178.7(3) . . . . ? Cu2 N2B C26B C18B -1.7(4) . . . . ? C25B N2B C26B C22B 0.9(5) . . . . ? Cu2 N2B C26B C22B 177.9(2) . . . . ? C19B C18B C26B N2B -179.5(3) . . . . ? S2B C18B C26B N2B 1.0(4) . . . . ? C19B C18B C26B C22B 1.0(5) . . . . ? S2B C18B C26B C22B -178.5(2) . . . . ? C23B C22B C26B N2B -0.4(5) . . . . ? C21B C22B C26B N2B 179.9(3) . . . . ? C23B C22B C26B C18B 179.1(3) . . . . ? C21B C22B C26B C18B -0.5(5) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 26.44 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.409 _refine_diff_density_min -1.286 _refine_diff_density_rms 0.122 data_03263 _database_code_depnum_ccdc_archive 'CCDC 268257' _exptl_crystal_id MSC03263 _audit_creation_date 12/31/2003 _chemical_formula_structural '[Pd(C26H18N2S2)]+2, 2[BF4]-, MecN' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H21 B2 F8 N3 Pd S2' _chemical_formula_weight 743.62 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' F F 0.0171 0.0103 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P2(1)/n ' 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 13.2183(14) _cell_length_b 11.6622(13) _cell_length_c 18.790(2) _cell_angle_alpha 90.00 _cell_angle_beta 93.675(3) _cell_angle_gamma 90.00 _cell_volume 2890.5(5) _cell_formula_units_Z 4 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used 996 _cell_measurement_theta_min 2.53 _cell_measurement_theta_max 27.17 _exptl_crystal_description irregular _exptl_crystal_colour yellow _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.709 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1480 _exptl_absorpt_coefficient_mu 0.864 _exptl_absorpt_correction_type none _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_details ' 0.30 degree frames measured for 10.17 seconds each' _diffrn_measurement_method '\w scans' _diffrn_measurement_device 'three-circle goniometer with fixed chi' _diffrn_measurement_device_type 'Bruker Platform goniometer' _diffrn_detector 'CCD area detector' _diffrn_detector_type 'Bruker SMART 6000' _diffrn_detector_area_resol_mean 44.52 _diffrn_standards_decay_% 0.0 _diffrn_reflns_number 63145 _diffrn_reflns_av_R_equivalents 0.0949 _diffrn_reflns_av_sigmaI/netI 0.0572 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.94 _diffrn_reflns_theta_max 27.54 _reflns_number_total 6654 _reflns_number_gt 4412 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1999)' _computing_cell_refinement 'SAINT (Bruker, 1999)' _computing_data_reduction 'SAINT (Bruker, 1999), XTEL (local program)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0356P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6654 _refine_ls_number_parameters 498 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0571 _refine_ls_R_factor_gt 0.0314 _refine_ls_wR_factor_ref 0.0740 _refine_ls_wR_factor_gt 0.0681 _refine_ls_goodness_of_fit_ref 0.859 _refine_ls_restrained_S_all 0.859 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.719222(15) 0.137117(18) 0.918548(11) 0.01613(6) Uani 1 1 d . . . S12 S 0.78005(5) 0.13735(7) 0.80607(3) 0.01852(14) Uani 1 1 d . . . S21 S 0.65869(5) 0.12613(6) 1.03025(3) 0.01712(15) Uani 1 1 d . . . F35 F 0.72140(13) -0.14158(18) 0.98796(9) 0.0385(5) Uani 1 1 d . . . F37 F 0.65095(13) 0.34048(18) 1.21683(9) 0.0388(5) Uani 1 1 d . . . N3 N 0.57927(16) 0.12925(19) 0.86638(11) 0.0165(5) Uani 1 1 d . . . N30 N 0.85973(16) 0.1394(2) 0.97094(11) 0.0170(5) Uani 1 1 d . . . C22 C 0.7756(2) 0.1200(2) 1.08072(15) 0.0172(5) Uani 1 1 d . . . F34 F 0.56864(13) -0.11418(16) 0.93053(10) 0.0371(5) Uani 1 1 d . . . C29 C 0.9459(2) 0.1485(3) 0.93909(16) 0.0212(6) Uani 1 1 d . . . C31 C 0.8660(2) 0.1294(2) 1.04486(14) 0.0172(6) Uani 1 1 d . . . C5 C 0.3973(2) 0.1247(3) 0.86249(15) 0.0215(6) Uani 1 1 d . . . C28 C 1.0419(2) 0.1492(3) 0.97547(15) 0.0232(6) Uani 1 1 d . . . C4 C 0.4928(2) 0.1289(2) 0.89862(15) 0.0190(6) Uani 1 1 d . . . C27 C 1.0491(2) 0.1386(3) 1.04781(16) 0.0236(6) Uani 1 1 d . . . C6 C 0.3901(2) 0.1155(3) 0.79020(17) 0.0238(7) Uani 1 1 d . . . C8 C 0.4786(2) 0.0996(3) 0.67817(16) 0.0260(7) Uani 1 1 d . . . C41A C 0.6601(2) 0.1117(3) 0.68287(16) 0.0247(7) Uani 1 1 d . . . C2 C 0.5736(2) 0.1209(2) 0.79246(14) 0.0179(6) Uani 1 1 d . . . C26 C 0.9598(2) 0.1277(2) 1.08455(15) 0.0208(6) Uani 1 1 d . . . C23 C 0.7791(2) 0.1094(2) 1.15375(15) 0.0213(6) Uani 1 1 d . . . C11 C 0.6632(2) 0.1224(2) 0.75571(15) 0.0201(6) Uani 1 1 d . . . F36 F 0.65533(16) -0.27716(16) 0.91082(12) 0.0464(5) Uani 1 1 d . . . C7 C 0.4795(2) 0.1107(2) 0.75314(15) 0.0206(6) Uani 1 1 d . . . C14 C 0.7211(2) 0.3619(3) 0.80185(15) 0.0247(6) Uani 1 1 d . . . C18 C 0.5458(2) 0.3966(3) 0.94606(16) 0.0261(7) Uani 1 1 d . . . C24 C 0.8730(2) 0.1067(3) 1.19322(16) 0.0262(7) Uani 1 1 d . . . C20 C 0.6165(2) 0.2723(3) 1.05527(16) 0.0236(7) Uani 1 1 d . . . C9 C 0.5667(2) 0.0997(3) 0.64415(16) 0.0274(7) Uani 1 1 d . . . C19 C 0.5763(2) 0.3394(3) 0.99497(16) 0.0243(7) Uani 1 1 d . . . C13 C 0.8071(2) 0.2898(3) 0.78816(18) 0.0275(7) Uani 1 1 d . . . C16 C 0.5591(2) 0.4791(3) 0.82784(17) 0.0270(7) Uani 1 1 d . . . C15 C 0.6473(2) 0.4147(3) 0.81373(16) 0.0264(7) Uani 1 1 d . . . C17 C 0.5118(3) 0.4688(3) 0.88842(17) 0.0307(8) Uani 1 1 d . . . N42 N 0.8523(3) 0.4109(3) 1.0038(2) 0.0621(10) Uani 1 1 d . . . B32 B 0.6645(2) -0.1622(3) 0.92434(18) 0.0245(8) Uani 1 1 d . . . C44 C 0.7619(4) 0.5887(4) 1.0483(3) 0.0719(14) Uani 1 1 d . . . H63 H 0.6912 0.5883 1.0291 0.108 Uiso 1 1 calc R . . H64 H 0.7954 0.6585 1.0328 0.108 Uiso 1 1 calc R . . H65 H 0.7639 0.5868 1.1005 0.108 Uiso 1 1 calc R . . C43 C 0.8136(3) 0.4895(3) 1.0226(2) 0.0427(9) Uani 1 1 d . . . F33 F 0.71239(13) -0.10902(15) 0.86909(9) 0.0306(4) Uani 1 1 d . . . F39 F 0.5139(7) 0.3146(10) 1.2837(7) 0.049(3) Uani 0.62(3) 1 d P . . F40 F 0.6699(5) 0.3158(9) 1.3370(3) 0.0414(19) Uani 0.62(3) 1 d P . . C25 C 0.9606(2) 0.1162(3) 1.15948(16) 0.0255(7) Uani 1 1 d . . . B37 B 0.6120(3) 0.2787(3) 1.2726(2) 0.0320(9) Uani 1 1 d . . . H62 H 0.939(2) 0.154(2) 0.8914(16) 0.014(7) Uiso 1 1 d . . . H45 H 0.4980(18) 0.128(2) 0.9460(14) 0.001(6) Uiso 1 1 d . . . H61 H 1.097(3) 0.158(3) 0.9498(17) 0.034(9) Uiso 1 1 d . . . H46 H 0.340(2) 0.130(2) 0.8880(16) 0.020(8) Uiso 1 1 d . . . H59 H 1.026(2) 0.112(2) 1.1851(14) 0.011(7) Uiso 1 1 d . . . H47 H 0.335(2) 0.112(2) 0.7654(16) 0.022(8) Uiso 1 1 d . . . H58 H 0.873(2) 0.108(3) 1.2440(18) 0.030(9) Uiso 1 1 d . . . H48 H 0.413(2) 0.087(3) 0.6541(16) 0.029(9) Uiso 1 1 d . . . H50 H 0.724(2) 0.111(2) 0.6601(16) 0.023(8) Uiso 1 1 d . . . H49 H 0.562(2) 0.085(3) 0.5973(17) 0.022(8) Uiso 1 1 d . . . H60 H 1.109(2) 0.136(3) 1.0730(17) 0.032(9) Uiso 1 1 d . . . H54 H 0.459(2) 0.511(3) 0.8936(16) 0.028(9) Uiso 1 1 d . . . H51 H 0.821(3) 0.286(3) 0.7424(19) 0.041(10) Uiso 1 1 d . . . H55 H 0.678(2) 0.310(2) 1.0785(15) 0.019(8) Uiso 1 1 d . . . H53 H 0.535(2) 0.528(3) 0.7941(16) 0.023(8) Uiso 1 1 d . . . H52 H 0.868(2) 0.308(3) 0.8206(16) 0.026(8) Uiso 1 1 d . . . H57 H 0.720(2) 0.105(2) 1.1737(16) 0.024(8) Uiso 1 1 d . . . H56 H 0.573(3) 0.259(3) 1.0867(17) 0.032(9) Uiso 1 1 d . . . F38 F 0.6216(8) 0.1624(4) 1.2713(7) 0.058(3) Uani 0.62(3) 1 d P . . F38A F 0.5785(13) 0.1787(11) 1.2306(13) 0.065(6) Uani 0.38(3) 1 d P . . F40A F 0.6769(9) 0.256(3) 1.3196(12) 0.086(7) Uani 0.38(3) 1 d P . . F39A F 0.5216(12) 0.3228(12) 1.2873(10) 0.040(4) Uani 0.38(3) 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 Pd1 0.01129(10) 0.02460(11) 0.01258(10) -0.00018(10) 0.00124(7) 0.00044(10) S12 0.0136(3) 0.0286(4) 0.0135(3) 0.0011(3) 0.0021(3) 0.0016(3) S21 0.0129(3) 0.0254(4) 0.0132(3) -0.0005(3) 0.0016(3) 0.0006(3) F35 0.0259(9) 0.0677(14) 0.0220(9) -0.0018(9) 0.0016(8) 0.0002(10) F37 0.0241(9) 0.0730(15) 0.0197(9) 0.0001(9) 0.0055(8) -0.0039(10) N3 0.0149(11) 0.0206(12) 0.0142(11) 0.0002(10) 0.0023(9) -0.0002(10) N30 0.0128(10) 0.0227(12) 0.0154(11) -0.0003(10) 0.0013(9) 0.0013(10) C22 0.0128(12) 0.0200(14) 0.0186(13) -0.0001(12) -0.0004(10) 0.0006(12) F34 0.0185(9) 0.0521(13) 0.0414(11) -0.0002(9) 0.0075(8) 0.0053(8) C29 0.0185(14) 0.0294(17) 0.0157(14) -0.0018(13) 0.0018(11) 0.0025(13) C31 0.0169(13) 0.0205(14) 0.0142(13) -0.0010(11) 0.0012(10) 0.0020(12) C5 0.0136(13) 0.0300(17) 0.0211(15) 0.0006(13) 0.0029(11) -0.0012(12) C28 0.0133(13) 0.0341(18) 0.0228(15) -0.0002(13) 0.0042(12) 0.0009(13) C4 0.0168(13) 0.0252(16) 0.0150(14) -0.0011(12) 0.0009(11) -0.0001(12) C27 0.0138(13) 0.0310(16) 0.0254(16) 0.0000(14) -0.0027(12) 0.0005(14) C6 0.0155(14) 0.0321(18) 0.0233(16) 0.0006(13) -0.0019(12) -0.0023(13) C8 0.0234(16) 0.0343(18) 0.0197(16) -0.0013(13) -0.0037(13) 0.0011(14) C41A 0.0230(15) 0.0336(19) 0.0178(15) 0.0007(12) 0.0046(12) 0.0050(13) C2 0.0184(13) 0.0211(16) 0.0140(13) 0.0003(11) 0.0007(11) 0.0022(11) C26 0.0172(13) 0.0255(16) 0.0198(14) -0.0004(12) 0.0009(11) 0.0006(12) C23 0.0194(14) 0.0276(17) 0.0169(14) 0.0009(12) 0.0015(12) 0.0003(12) C11 0.0174(13) 0.0252(16) 0.0179(13) 0.0023(12) 0.0013(11) 0.0031(12) F36 0.0475(13) 0.0331(11) 0.0610(14) -0.0076(10) 0.0217(11) -0.0025(10) C7 0.0174(14) 0.0245(16) 0.0194(15) 0.0010(12) -0.0015(12) 0.0004(12) C14 0.0252(15) 0.0266(15) 0.0219(15) 0.0061(13) -0.0029(12) -0.0068(14) C18 0.0279(16) 0.0295(17) 0.0208(16) -0.0072(13) 0.0003(13) 0.0065(13) C24 0.0274(16) 0.0370(19) 0.0141(15) -0.0003(13) -0.0001(13) 0.0017(14) C20 0.0249(16) 0.0287(17) 0.0174(16) -0.0040(13) 0.0041(13) 0.0048(13) C9 0.0309(17) 0.0383(19) 0.0126(15) -0.0012(13) -0.0020(13) 0.0053(14) C19 0.0226(15) 0.0283(17) 0.0221(15) -0.0045(13) 0.0025(12) 0.0054(13) C13 0.0202(15) 0.0366(19) 0.0257(18) 0.0093(14) 0.0018(14) -0.0031(14) C16 0.0326(17) 0.0228(16) 0.0243(17) -0.0016(13) -0.0097(14) 0.0029(14) C15 0.0301(17) 0.0287(17) 0.0196(15) 0.0040(13) -0.0055(13) -0.0061(14) C17 0.0351(19) 0.0319(18) 0.0244(17) -0.0043(14) -0.0035(14) 0.0126(15) N42 0.070(3) 0.053(2) 0.062(2) -0.001(2) -0.006(2) -0.003(2) B32 0.0180(16) 0.033(2) 0.0227(17) -0.0042(14) 0.0036(14) -0.0006(14) C44 0.074(3) 0.055(3) 0.086(4) -0.003(3) -0.004(3) 0.003(3) C43 0.049(2) 0.039(2) 0.038(2) 0.0114(18) -0.0124(18) -0.0093(19) F33 0.0253(9) 0.0446(12) 0.0226(9) -0.0013(8) 0.0066(7) -0.0038(8) F39 0.010(3) 0.107(7) 0.030(5) 0.005(4) 0.002(3) 0.003(3) F40 0.020(2) 0.084(5) 0.019(2) 0.000(2) 0.0001(14) -0.009(3) C25 0.0189(15) 0.0368(19) 0.0198(15) 0.0026(13) -0.0054(12) -0.0011(13) B37 0.0195(17) 0.039(2) 0.039(2) 0.0012(18) 0.0069(17) 0.0038(17) F38 0.076(5) 0.046(3) 0.055(5) -0.004(2) 0.038(5) 0.004(2) F38A 0.070(7) 0.056(5) 0.076(11) -0.026(6) 0.045(8) -0.023(5) F40A 0.037(5) 0.137(18) 0.082(11) 0.070(11) -0.018(6) -0.011(7) F39A 0.055(9) 0.034(5) 0.035(8) 0.015(4) 0.030(6) 0.024(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 N3 2.039(2) . ? Pd1 N30 2.046(2) . ? Pd1 S21 2.2971(7) . ? Pd1 S12 2.3089(7) . ? S12 C11 1.767(3) . ? S12 C13 1.849(3) . ? S21 C22 1.762(3) . ? S21 C20 1.863(3) . ? F35 B32 1.392(4) . ? F37 B37 1.396(4) . ? N3 C4 1.328(3) . ? N3 C2 1.389(3) . ? N30 C29 1.324(3) . ? N30 C31 1.391(3) . ? C22 C23 1.376(4) . ? C22 C31 1.412(4) . ? F34 B32 1.397(4) . ? C29 C28 1.402(4) . ? C29 H62 0.90(3) . ? C31 C26 1.406(4) . ? C5 C6 1.360(4) . ? C5 C4 1.395(4) . ? C5 H46 0.92(3) . ? C28 C27 1.362(4) . ? C28 H61 0.91(3) . ? C4 H45 0.89(2) . ? C27 C26 1.411(4) . ? C27 H60 0.89(3) . ? C6 C7 1.411(4) . ? C6 H47 0.84(3) . ? C8 C9 1.364(4) . ? C8 C7 1.414(4) . ? C8 H48 0.96(3) . ? C41A C11 1.372(4) . ? C41A C9 1.400(4) . ? C41A H50 0.97(3) . ? C2 C11 1.409(4) . ? C2 C7 1.410(4) . ? C26 C25 1.414(4) . ? C23 C24 1.405(4) . ? C23 H57 0.89(3) . ? F36 B32 1.368(4) . ? C14 C15 1.187(4) . ? C14 C13 1.450(4) . ? C18 C19 1.185(4) . ? C18 C17 1.422(4) . ? C24 C25 1.359(4) . ? C24 H58 0.95(3) . ? C20 C19 1.449(4) . ? C20 H55 1.00(3) . ? C20 H56 0.87(3) . ? C9 H49 0.90(3) . ? C13 H51 0.89(3) . ? C13 H52 1.00(3) . ? C16 C17 1.338(4) . ? C16 C15 1.427(4) . ? C16 H53 0.89(3) . ? C17 H54 0.87(3) . ? N42 C43 1.119(5) . ? B32 F33 1.396(4) . ? C44 C43 1.442(6) . ? C44 H63 0.9800 . ? C44 H64 0.9800 . ? C44 H65 0.9800 . ? F39 B37 1.392(10) . ? F40 B37 1.456(7) . ? C25 H59 0.97(3) . ? B37 F40A 1.220(13) . ? B37 F39A 1.347(15) . ? B37 F38 1.362(6) . ? B37 F38A 1.460(12) . ? 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 Pd1 N30 178.18(9) . . ? N3 Pd1 S21 94.49(6) . . ? N30 Pd1 S21 85.40(6) . . ? N3 Pd1 S12 85.32(6) . . ? N30 Pd1 S12 94.69(6) . . ? S21 Pd1 S12 176.87(3) . . ? C11 S12 C13 99.79(14) . . ? C11 S12 Pd1 98.41(10) . . ? C13 S12 Pd1 104.51(11) . . ? C22 S21 C20 99.67(13) . . ? C22 S21 Pd1 98.58(10) . . ? C20 S21 Pd1 107.88(10) . . ? C4 N3 C2 117.6(2) . . ? C4 N3 Pd1 124.20(18) . . ? C2 N3 Pd1 118.22(17) . . ? C29 N30 C31 117.4(2) . . ? C29 N30 Pd1 124.35(19) . . ? C31 N30 Pd1 118.24(17) . . ? C23 C22 C31 120.5(3) . . ? C23 C22 S21 120.8(2) . . ? C31 C22 S21 118.6(2) . . ? N30 C29 C28 123.9(3) . . ? N30 C29 H62 114.6(18) . . ? C28 C29 H62 121.5(18) . . ? N30 C31 C26 121.6(2) . . ? N30 C31 C22 119.0(2) . . ? C26 C31 C22 119.3(2) . . ? C6 C5 C4 119.5(3) . . ? C6 C5 H46 121.3(18) . . ? C4 C5 H46 119.2(18) . . ? C27 C28 C29 119.3(3) . . ? C27 C28 H61 122(2) . . ? C29 C28 H61 118(2) . . ? N3 C4 C5 123.8(3) . . ? N3 C4 H45 116.3(16) . . ? C5 C4 H45 119.9(16) . . ? C28 C27 C26 119.3(3) . . ? C28 C27 H60 122(2) . . ? C26 C27 H60 118(2) . . ? C5 C6 C7 119.3(3) . . ? C5 C6 H47 124(2) . . ? C7 C6 H47 116(2) . . ? C9 C8 C7 120.9(3) . . ? C9 C8 H48 123.4(19) . . ? C7 C8 H48 115.6(19) . . ? C11 C41A C9 119.8(3) . . ? C11 C41A H50 118.1(18) . . ? C9 C41A H50 122.1(18) . . ? N3 C2 C11 119.7(2) . . ? N3 C2 C7 121.3(2) . . ? C11 C2 C7 119.0(2) . . ? C31 C26 C27 118.4(3) . . ? C31 C26 C25 118.7(3) . . ? C27 C26 C25 122.9(3) . . ? C22 C23 C24 120.0(3) . . ? C22 C23 H57 117(2) . . ? C24 C23 H57 123(2) . . ? C41A C11 C2 121.0(3) . . ? C41A C11 S12 120.8(2) . . ? C2 C11 S12 118.2(2) . . ? C2 C7 C6 118.4(3) . . ? C2 C7 C8 118.7(3) . . ? C6 C7 C8 122.8(3) . . ? C15 C14 C13 175.8(3) . . ? C19 C18 C17 177.6(4) . . ? C25 C24 C23 120.1(3) . . ? C25 C24 H58 121.2(19) . . ? C23 C24 H58 118.2(19) . . ? C19 C20 S21 113.4(2) . . ? C19 C20 H55 110.3(17) . . ? S21 C20 H55 105.7(16) . . ? C19 C20 H56 114(2) . . ? S21 C20 H56 104(2) . . ? H55 C20 H56 110(3) . . ? C8 C9 C41A 120.5(3) . . ? C8 C9 H49 117(2) . . ? C41A C9 H49 122.0(19) . . ? C18 C19 C20 178.1(3) . . ? C14 C13 S12 111.2(2) . . ? C14 C13 H51 114(2) . . ? S12 C13 H51 101(2) . . ? C14 C13 H52 111.9(18) . . ? S12 C13 H52 104.7(18) . . ? H51 C13 H52 113(3) . . ? C17 C16 C15 122.9(3) . . ? C17 C16 H53 120(2) . . ? C15 C16 H53 118(2) . . ? C14 C15 C16 179.5(4) . . ? C16 C17 C18 124.0(3) . . ? C16 C17 H54 118(2) . . ? C18 C17 H54 118(2) . . ? F36 B32 F35 111.4(3) . . ? F36 B32 F33 109.7(3) . . ? F35 B32 F33 108.4(2) . . ? F36 B32 F34 109.8(3) . . ? F35 B32 F34 107.6(2) . . ? F33 B32 F34 109.9(3) . . ? C43 C44 H63 109.5 . . ? C43 C44 H64 109.5 . . ? H63 C44 H64 109.5 . . ? C43 C44 H65 109.5 . . ? H63 C44 H65 109.5 . . ? H64 C44 H65 109.5 . . ? N42 C43 C44 178.3(5) . . ? C24 C25 C26 121.3(3) . . ? C24 C25 H59 121.9(16) . . ? C26 C25 H59 116.7(16) . . ? F40A B37 F39A 121.7(15) . . ? F40A B37 F38 74.8(10) . . ? F39A B37 F38 117.9(8) . . ? F40A B37 F39 125.0(13) . . ? F39A B37 F39 6.1(12) . . ? F38 B37 F39 113.0(6) . . ? F40A B37 F37 112.3(6) . . ? F39A B37 F37 109.4(7) . . ? F38 B37 F37 117.5(4) . . ? F39 B37 F37 110.5(6) . . ? F40A B37 F40 32.2(14) . . ? F39A B37 F40 98.2(9) . . ? F38 B37 F40 105.4(5) . . ? F39 B37 F40 103.3(6) . . ? F37 B37 F40 105.8(4) . . ? F40A B37 F38A 113.3(9) . . ? F39A B37 F38A 99.9(9) . . ? F38 B37 F38A 38.8(6) . . ? F39 B37 F38A 93.9(8) . . ? F37 B37 F38A 96.9(8) . . ? F40 B37 F38A 144.2(9) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N3 Pd1 S12 C11 -3.14(12) . . . . ? N30 Pd1 S12 C11 175.03(11) . . . . ? S21 Pd1 S12 C11 83.6(5) . . . . ? N3 Pd1 S12 C13 99.32(12) . . . . ? N30 Pd1 S12 C13 -82.50(13) . . . . ? S21 Pd1 S12 C13 -174.0(5) . . . . ? N3 Pd1 S21 C22 175.27(11) . . . . ? N30 Pd1 S21 C22 -2.90(11) . . . . ? S12 Pd1 S21 C22 88.8(5) . . . . ? N3 Pd1 S21 C20 -81.60(13) . . . . ? N30 Pd1 S21 C20 100.22(13) . . . . ? S12 Pd1 S21 C20 -168.1(5) . . . . ? N30 Pd1 N3 C4 91(3) . . . . ? S21 Pd1 N3 C4 4.9(2) . . . . ? S12 Pd1 N3 C4 -178.2(2) . . . . ? N30 Pd1 N3 C2 -87(3) . . . . ? S21 Pd1 N3 C2 -173.42(18) . . . . ? S12 Pd1 N3 C2 3.45(18) . . . . ? N3 Pd1 N30 C29 95(3) . . . . ? S21 Pd1 N30 C29 -178.3(2) . . . . ? S12 Pd1 N30 C29 4.9(2) . . . . ? N3 Pd1 N30 C31 -84(3) . . . . ? S21 Pd1 N30 C31 2.63(19) . . . . ? S12 Pd1 N30 C31 -174.24(19) . . . . ? C20 S21 C22 C23 71.8(2) . . . . ? Pd1 S21 C22 C23 -178.3(2) . . . . ? C20 S21 C22 C31 -106.4(2) . . . . ? Pd1 S21 C22 C31 3.5(2) . . . . ? C31 N30 C29 C28 -0.4(4) . . . . ? Pd1 N30 C29 C28 -179.6(2) . . . . ? C29 N30 C31 C26 -0.6(4) . . . . ? Pd1 N30 C31 C26 178.5(2) . . . . ? C29 N30 C31 C22 179.8(3) . . . . ? Pd1 N30 C31 C22 -1.0(3) . . . . ? C23 C22 C31 N30 179.7(3) . . . . ? S21 C22 C31 N30 -2.1(4) . . . . ? C23 C22 C31 C26 0.1(4) . . . . ? S21 C22 C31 C26 178.4(2) . . . . ? N30 C29 C28 C27 0.9(5) . . . . ? C2 N3 C4 C5 -2.4(4) . . . . ? Pd1 N3 C4 C5 179.3(2) . . . . ? C6 C5 C4 N3 3.0(5) . . . . ? C29 C28 C27 C26 -0.3(5) . . . . ? C4 C5 C6 C7 -0.2(4) . . . . ? C4 N3 C2 C11 179.2(3) . . . . ? Pd1 N3 C2 C11 -2.3(3) . . . . ? C4 N3 C2 C7 -0.9(4) . . . . ? Pd1 N3 C2 C7 177.5(2) . . . . ? N30 C31 C26 C27 1.2(4) . . . . ? C22 C31 C26 C27 -179.2(3) . . . . ? N30 C31 C26 C25 -179.4(3) . . . . ? C22 C31 C26 C25 0.2(4) . . . . ? C28 C27 C26 C31 -0.7(5) . . . . ? C28 C27 C26 C25 180.0(3) . . . . ? C31 C22 C23 C24 -0.7(4) . . . . ? S21 C22 C23 C24 -178.9(2) . . . . ? C9 C41A C11 C2 0.3(4) . . . . ? C9 C41A C11 S12 179.8(2) . . . . ? N3 C2 C11 C41A 178.5(3) . . . . ? C7 C2 C11 C41A -1.3(4) . . . . ? N3 C2 C11 S12 -1.0(4) . . . . ? C7 C2 C11 S12 179.1(2) . . . . ? C13 S12 C11 C41A 77.2(3) . . . . ? Pd1 S12 C11 C41A -176.4(2) . . . . ? C13 S12 C11 C2 -103.3(2) . . . . ? Pd1 S12 C11 C2 3.2(2) . . . . ? N3 C2 C7 C6 3.5(4) . . . . ? C11 C2 C7 C6 -176.6(3) . . . . ? N3 C2 C7 C8 -178.4(3) . . . . ? C11 C2 C7 C8 1.5(4) . . . . ? C5 C6 C7 C2 -2.9(4) . . . . ? C5 C6 C7 C8 179.1(3) . . . . ? C9 C8 C7 C2 -0.6(5) . . . . ? C9 C8 C7 C6 177.4(3) . . . . ? C22 C23 C24 C25 1.0(5) . . . . ? C22 S21 C20 C19 135.1(2) . . . . ? Pd1 S21 C20 C19 32.7(3) . . . . ? C7 C8 C9 C41A -0.5(5) . . . . ? C11 C41A C9 C8 0.6(5) . . . . ? C17 C18 C19 C20 -13(16) . . . . ? S21 C20 C19 C18 -117(10) . . . . ? C15 C14 C13 S12 -7(5) . . . . ? C11 S12 C13 C14 51.1(3) . . . . ? Pd1 S12 C13 C14 -50.4(2) . . . . ? C13 C14 C15 C16 -173(100) . . . . ? C17 C16 C15 C14 -130(39) . . . . ? C15 C16 C17 C18 2.3(5) . . . . ? C19 C18 C17 C16 85(8) . . . . ? C23 C24 C25 C26 -0.7(5) . . . . ? C31 C26 C25 C24 0.1(5) . . . . ? C27 C26 C25 C24 179.5(3) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.54 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.358 _refine_diff_density_min -0.667 _refine_diff_density_rms 0.088 data_04170 _database_code_depnum_ccdc_archive 'CCDC 268258' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H20 B2 F8 N2 Pd S2' _chemical_formula_weight 704.58 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 '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 7.9642(5) _cell_length_b 9.4857(6) _cell_length_c 17.9043(11) _cell_angle_alpha 85.756(2) _cell_angle_beta 88.366(2) _cell_angle_gamma 71.6800(10) _cell_volume 1280.50(14) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 4735 _cell_measurement_theta_min 2.5 _cell_measurement_theta_max 25.0 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.827 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 700 _exptl_absorpt_coefficient_mu 0.968 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8225 _exptl_absorpt_correction_T_max 0.9094 _exptl_absorpt_process_details 'SADABS, R. Blessing (1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_details '0.30 degree frames measured for 10 seconds each' _diffrn_measurement_method \w-scans _diffrn_measurement_device 'three-circle goniometer with fixed chi' _diffrn_measurement_device_type 'Bruker Platform goniometer' _diffrn_detector 'CCD area detector' _diffrn_detector_type 'Bruker SMART 6000' _diffrn_detector_area_resol_mean 44.52 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7999 _diffrn_reflns_av_R_equivalents 0.0194 _diffrn_reflns_av_sigmaI/netI 0.0304 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.27 _diffrn_reflns_theta_max 25.04 _reflns_number_total 4504 _reflns_number_gt 4127 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, current version)' _computing_cell_refinement 'SAINT (Bruker, current version)' _computing_data_reduction 'SAINT (Bruker, current version)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XTEL (local library)' _computing_publication_material 'XCIF (Bruker, 1999), XTEL (local library)' _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^)+(0.0539P)^2^+3.0580P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4504 _refine_ls_number_parameters 409 _refine_ls_number_restraints 42 _refine_ls_R_factor_all 0.0408 _refine_ls_R_factor_gt 0.0373 _refine_ls_wR_factor_ref 0.0986 _refine_ls_wR_factor_gt 0.0952 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.054 _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 Pd1 Pd 0.17217(3) -0.00464(3) 0.279027(13) 0.01667(11) Uani 1 1 d . . . S1 S 0.45936(11) -0.05841(9) 0.24412(5) 0.01788(19) Uani 1 1 d . . . S2 S 0.10470(11) 0.20859(9) 0.20301(5) 0.01901(19) Uani 1 1 d . . . N1 N 0.2517(4) -0.2163(3) 0.33606(16) 0.0177(6) Uani 1 1 d . . . N2 N -0.0912(4) 0.0751(3) 0.31358(16) 0.0179(6) Uani 1 1 d . . . C1 C 0.4793(5) -0.1057(4) 0.14517(19) 0.0228(8) Uani 1 1 d . . . H1A H 0.5904 -0.1872 0.1372 0.027 Uiso 1 1 calc R . . H1B H 0.3785 -0.1383 0.1313 0.027 Uiso 1 1 calc R . . C2 C 0.4796(5) 0.0323(4) 0.09862(19) 0.0214(7) Uani 1 1 d . . . C3 C 0.6417(5) 0.0464(5) 0.0739(2) 0.0260(8) Uani 1 1 d . . . H3 H 0.7480 -0.0310 0.0865 0.031 Uiso 1 1 calc R . . C4 C 0.6494(5) 0.1719(5) 0.0312(2) 0.0277(8) Uani 1 1 d . . . H4 H 0.7605 0.1793 0.0142 0.033 Uiso 1 1 calc R . . C5 C 0.4955(6) 0.2871(4) 0.0132(2) 0.0275(8) Uani 1 1 d . . . H5 H 0.5010 0.3729 -0.0164 0.033 Uiso 1 1 calc R . . C6 C 0.3345(5) 0.2760(4) 0.0386(2) 0.0268(8) Uani 1 1 d . . . H6 H 0.2296 0.3558 0.0271 0.032 Uiso 1 1 calc R . . C7 C 0.3236(5) 0.1487(4) 0.08095(19) 0.0225(8) Uani 1 1 d . . . C8 C 0.1444(5) 0.1437(4) 0.10696(19) 0.0234(8) Uani 1 1 d . . . H8A H 0.1394 0.0408 0.1069 0.028 Uiso 1 1 calc R . . H8B H 0.0522 0.2086 0.0727 0.028 Uiso 1 1 calc R . . C9 C 0.1446(5) -0.2842(4) 0.36966(19) 0.0203(7) Uani 1 1 d . . . H9 H 0.0206 -0.2381 0.3646 0.024 Uiso 1 1 calc R . . C10 C 0.2049(5) -0.4204(4) 0.41230(19) 0.0218(7) Uani 1 1 d . . . H10 H 0.1227 -0.4636 0.4360 0.026 Uiso 1 1 calc R . . C11 C 0.3816(5) -0.4903(4) 0.41953(19) 0.0201(7) Uani 1 1 d . . . H11 H 0.4242 -0.5799 0.4504 0.024 Uiso 1 1 calc R . . C12 C 0.5010(5) -0.4279(4) 0.38041(19) 0.0192(7) Uani 1 1 d . . . C13 C 0.6857(5) -0.5005(4) 0.3789(2) 0.0219(8) Uani 1 1 d . . . H13 H 0.7345 -0.5911 0.4083 0.026 Uiso 1 1 calc R . . C14 C 0.7954(5) -0.4412(4) 0.3351(2) 0.0241(8) Uani 1 1 d . . . H14 H 0.9186 -0.4927 0.3334 0.029 Uiso 1 1 calc R . . C15 C 0.7258(5) -0.3053(4) 0.2933(2) 0.0225(8) Uani 1 1 d . . . H15 H 0.8018 -0.2642 0.2634 0.027 Uiso 1 1 calc R . . C16 C 0.5484(5) -0.2324(4) 0.29546(19) 0.0192(7) Uani 1 1 d . . . C17 C 0.4312(5) -0.2905(4) 0.33834(18) 0.0174(7) Uani 1 1 d . . . C18 C -0.1575(5) 0.0318(4) 0.37648(19) 0.0205(7) Uani 1 1 d . . . H18 H -0.0789 -0.0358 0.4113 0.025 Uiso 1 1 calc R . . C19 C -0.3382(5) 0.0809(4) 0.3940(2) 0.0220(7) Uani 1 1 d . . . H19 H -0.3806 0.0444 0.4391 0.026 Uiso 1 1 calc R . . C20 C -0.4531(5) 0.1814(4) 0.3460(2) 0.0210(7) Uani 1 1 d . . . H20 H -0.5769 0.2101 0.3553 0.025 Uiso 1 1 calc R . . C21 C -0.3853(5) 0.2424(4) 0.28208(19) 0.0201(7) Uani 1 1 d . . . C22 C -0.4929(5) 0.3597(4) 0.2342(2) 0.0247(8) Uani 1 1 d . . . H22 H -0.6175 0.3921 0.2412 0.030 Uiso 1 1 calc R . . C23 C -0.4184(5) 0.4271(4) 0.1777(2) 0.0281(9) Uani 1 1 d . . . H23 H -0.4919 0.5054 0.1458 0.034 Uiso 1 1 calc R . . C24 C -0.2343(5) 0.3805(4) 0.1668(2) 0.0257(8) Uani 1 1 d . . . H24 H -0.1826 0.4309 0.1296 0.031 Uiso 1 1 calc R . . C25 C -0.1289(5) 0.2614(4) 0.2104(2) 0.0212(7) Uani 1 1 d . . . C26 C -0.2015(5) 0.1893(4) 0.26810(19) 0.0181(7) Uani 1 1 d . . . B1 B 0.0661(15) -0.3081(13) 0.1496(7) 0.0288(16) Uani 0.50 1 d PDU A 1 F1 F 0.2224(10) -0.3137(10) 0.1160(7) 0.088(4) Uani 0.50 1 d PDU A 1 F2 F -0.0162(10) -0.1678(7) 0.1747(4) 0.0480(16) Uani 0.50 1 d PDU A 1 F3 F 0.1069(14) -0.4091(11) 0.2125(5) 0.0391(18) Uani 0.50 1 d PDU A 1 F4 F -0.0522(17) -0.3338(18) 0.1035(8) 0.115(5) Uani 0.50 1 d PDU A 1 B1D B 0.0664(15) -0.3146(13) 0.1324(7) 0.0288(16) Uani 0.50 1 d PDU B 2 F1D F 0.1971(13) -0.3787(9) 0.0844(6) 0.083(3) Uani 0.50 1 d PDU B 2 F2D F 0.0568(10) -0.1699(8) 0.1420(6) 0.068(2) Uani 0.50 1 d PDU B 2 F3D F 0.109(2) -0.4039(19) 0.1980(8) 0.102(5) Uani 0.50 1 d PDU B 2 F4D F -0.0916(12) -0.3259(11) 0.1153(6) 0.0452(19) Uani 0.50 1 d PDU B 2 B2 B 0.1429(5) 0.1941(5) 0.4478(2) 0.0208(8) Uani 1 1 d . . . F5 F 0.1187(3) 0.2790(2) 0.37923(12) 0.0255(5) Uani 1 1 d . . . F6 F -0.0203(3) 0.1927(3) 0.47641(12) 0.0304(5) Uani 1 1 d . . . F7 F 0.2254(3) 0.2549(3) 0.49820(13) 0.0345(5) Uani 1 1 d . . . F8 F 0.2474(3) 0.0491(2) 0.43585(12) 0.0297(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.01767(16) 0.01397(16) 0.01557(16) 0.00254(10) -0.00112(10) -0.00165(11) S1 0.0199(4) 0.0154(4) 0.0167(4) 0.0020(3) -0.0011(3) -0.0037(3) S2 0.0200(4) 0.0164(4) 0.0181(4) 0.0026(3) -0.0007(3) -0.0029(3) N1 0.0196(15) 0.0155(14) 0.0166(14) 0.0002(11) -0.0020(11) -0.0039(12) N2 0.0205(15) 0.0149(14) 0.0155(14) 0.0005(11) -0.0014(11) -0.0019(12) C1 0.0279(19) 0.0225(19) 0.0145(16) 0.0011(14) 0.0021(14) -0.0036(16) C2 0.0270(19) 0.0216(18) 0.0139(16) 0.0010(14) 0.0003(14) -0.0057(15) C3 0.026(2) 0.031(2) 0.0182(17) 0.0018(15) -0.0014(15) -0.0056(17) C4 0.032(2) 0.037(2) 0.0178(17) 0.0008(16) 0.0041(15) -0.0166(18) C5 0.041(2) 0.026(2) 0.0175(17) 0.0028(15) 0.0018(16) -0.0150(18) C6 0.034(2) 0.0234(19) 0.0189(18) 0.0041(15) -0.0012(16) -0.0045(17) C7 0.0279(19) 0.0221(18) 0.0157(16) -0.0001(14) -0.0016(14) -0.0055(16) C8 0.027(2) 0.0248(19) 0.0148(16) 0.0009(14) -0.0009(14) -0.0035(16) C9 0.0219(18) 0.0176(17) 0.0205(17) 0.0003(14) -0.0011(14) -0.0054(15) C10 0.030(2) 0.0179(17) 0.0185(17) -0.0015(14) 0.0031(15) -0.0093(16) C11 0.0294(19) 0.0119(16) 0.0168(16) -0.0003(13) -0.0017(14) -0.0035(15) C12 0.0241(18) 0.0151(16) 0.0151(16) -0.0020(13) -0.0031(14) -0.0010(14) C13 0.0250(19) 0.0164(17) 0.0193(17) 0.0003(14) -0.0060(14) 0.0010(15) C14 0.0202(18) 0.0220(19) 0.0249(19) 0.0002(15) -0.0039(15) 0.0006(15) C15 0.0204(18) 0.0238(19) 0.0217(18) 0.0021(15) -0.0012(14) -0.0054(15) C16 0.0242(18) 0.0163(17) 0.0151(16) 0.0023(13) -0.0034(14) -0.0041(15) C17 0.0208(18) 0.0137(16) 0.0144(16) -0.0022(13) -0.0014(13) -0.0002(14) C18 0.0249(19) 0.0153(17) 0.0189(17) 0.0011(14) -0.0001(14) -0.0031(15) C19 0.0260(19) 0.0199(18) 0.0202(17) -0.0015(14) 0.0042(14) -0.0075(15) C20 0.0204(18) 0.0180(17) 0.0234(18) -0.0051(14) 0.0022(14) -0.0037(15) C21 0.0211(18) 0.0188(18) 0.0196(17) -0.0028(14) -0.0029(14) -0.0047(15) C22 0.0199(18) 0.0235(19) 0.0254(19) -0.0020(15) -0.0040(15) 0.0009(15) C23 0.028(2) 0.025(2) 0.0221(18) 0.0046(16) -0.0060(16) 0.0048(16) C24 0.030(2) 0.0210(19) 0.0209(18) 0.0020(15) 0.0000(15) -0.0006(16) C25 0.0233(19) 0.0176(17) 0.0201(17) 0.0011(14) -0.0004(14) -0.0032(15) C26 0.0198(17) 0.0143(16) 0.0183(16) -0.0039(13) -0.0015(13) -0.0019(14) B1 0.022(2) 0.031(2) 0.031(5) 0.004(3) -0.001(2) -0.0057(19) F1 0.040(3) 0.054(5) 0.139(9) 0.054(5) 0.043(4) 0.010(4) F2 0.043(4) 0.031(3) 0.060(4) 0.004(3) -0.010(3) 0.001(3) F3 0.033(4) 0.040(4) 0.032(3) 0.007(3) 0.010(3) 0.003(3) F4 0.097(8) 0.098(8) 0.142(11) -0.034(7) -0.092(8) -0.003(7) B1D 0.022(2) 0.031(2) 0.031(5) 0.004(3) -0.001(2) -0.0057(19) F1D 0.072(5) 0.042(5) 0.113(7) 0.014(4) 0.064(5) 0.003(4) F2D 0.041(4) 0.033(3) 0.133(8) -0.010(4) -0.015(4) -0.012(3) F3D 0.095(9) 0.093(7) 0.071(6) 0.049(6) -0.003(5) 0.028(7) F4D 0.039(3) 0.036(4) 0.067(4) 0.010(3) 0.001(3) -0.025(3) B2 0.020(2) 0.018(2) 0.0219(19) 0.0031(16) -0.0015(16) -0.0036(17) F5 0.0258(11) 0.0213(11) 0.0251(11) 0.0075(9) -0.0011(9) -0.0032(9) F6 0.0300(12) 0.0326(12) 0.0282(11) 0.0001(10) 0.0075(9) -0.0102(10) F7 0.0454(14) 0.0318(13) 0.0308(12) 0.0008(10) -0.0100(11) -0.0181(11) F8 0.0360(13) 0.0190(11) 0.0257(11) 0.0037(9) -0.0012(9) 0.0021(10) _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 Pd1 N2 2.086(3) . ? Pd1 N1 2.100(3) . ? Pd1 S1 2.2615(9) . ? Pd1 S2 2.2766(9) . ? S1 C16 1.774(3) . ? S1 C1 1.850(3) . ? S2 C25 1.772(4) . ? S2 C8 1.855(4) . ? N1 C9 1.328(5) . ? N1 C17 1.381(5) . ? N2 C18 1.323(5) . ? N2 C26 1.386(4) . ? C1 C2 1.499(5) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C3 1.396(5) . ? C2 C7 1.404(5) . ? C3 C4 1.383(6) . ? C3 H3 0.9500 . ? C4 C5 1.389(6) . ? C4 H4 0.9500 . ? C5 C6 1.380(6) . ? C5 H5 0.9500 . ? C6 C7 1.403(5) . ? C6 H6 0.9500 . ? C7 C8 1.502(5) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.403(5) . ? C9 H9 0.9500 . ? C10 C11 1.359(5) . ? C10 H10 0.9500 . ? C11 C12 1.415(5) . ? C11 H11 0.9500 . ? C12 C17 1.414(5) . ? C12 C13 1.415(5) . ? C13 C14 1.377(5) . ? C13 H13 0.9500 . ? C14 C15 1.401(5) . ? C14 H14 0.9500 . ? C15 C16 1.365(5) . ? C15 H15 0.9500 . ? C16 C17 1.409(5) . ? C18 C19 1.401(5) . ? C18 H18 0.9500 . ? C19 C20 1.364(5) . ? C19 H19 0.9500 . ? C20 C21 1.414(5) . ? C20 H20 0.9500 . ? C21 C26 1.412(5) . ? C21 C22 1.417(5) . ? C22 C23 1.376(6) . ? C22 H22 0.9500 . ? C23 C24 1.404(6) . ? C23 H23 0.9500 . ? C24 C25 1.379(5) . ? C24 H24 0.9500 . ? C25 C26 1.407(5) . ? B1 F1 1.354(11) . ? B1 F4 1.359(11) . ? B1 F2 1.388(11) . ? B1 F3 1.399(11) . ? B1D F4D 1.341(11) . ? B1D F1D 1.349(11) . ? B1D F2D 1.374(11) . ? B1D F3D 1.380(11) . ? B2 F6 1.387(5) . ? B2 F7 1.388(5) . ? B2 F8 1.394(5) . ? B2 F5 1.401(4) . ? 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 N2 Pd1 N1 100.88(11) . . ? N2 Pd1 S1 171.85(8) . . ? N1 Pd1 S1 85.17(8) . . ? N2 Pd1 S2 84.65(8) . . ? N1 Pd1 S2 172.04(8) . . ? S1 Pd1 S2 89.90(3) . . ? C16 S1 C1 104.18(16) . . ? C16 S1 Pd1 99.73(12) . . ? C1 S1 Pd1 108.41(13) . . ? C25 S2 C8 102.15(17) . . ? C25 S2 Pd1 98.62(12) . . ? C8 S2 Pd1 104.39(12) . . ? C9 N1 C17 117.7(3) . . ? C9 N1 Pd1 125.6(2) . . ? C17 N1 Pd1 116.7(2) . . ? C18 N2 C26 118.2(3) . . ? C18 N2 Pd1 125.6(2) . . ? C26 N2 Pd1 116.1(2) . . ? C2 C1 S1 106.9(2) . . ? C2 C1 H1A 110.3 . . ? S1 C1 H1A 110.3 . . ? C2 C1 H1B 110.3 . . ? S1 C1 H1B 110.3 . . ? H1A C1 H1B 108.6 . . ? C3 C2 C7 119.2(3) . . ? C3 C2 C1 118.5(3) . . ? C7 C2 C1 122.3(3) . . ? C4 C3 C2 120.8(4) . . ? C4 C3 H3 119.6 . . ? C2 C3 H3 119.6 . . ? C3 C4 C5 120.4(4) . . ? C3 C4 H4 119.8 . . ? C5 C4 H4 119.8 . . ? C6 C5 C4 119.5(3) . . ? C6 C5 H5 120.2 . . ? C4 C5 H5 120.2 . . ? C5 C6 C7 121.0(4) . . ? C5 C6 H6 119.5 . . ? C7 C6 H6 119.5 . . ? C6 C7 C2 119.2(3) . . ? C6 C7 C8 118.4(3) . . ? C2 C7 C8 122.5(3) . . ? C7 C8 S2 108.7(2) . . ? C7 C8 H8A 109.9 . . ? S2 C8 H8A 109.9 . . ? C7 C8 H8B 109.9 . . ? S2 C8 H8B 109.9 . . ? H8A C8 H8B 108.3 . . ? N1 C9 C10 123.5(3) . . ? N1 C9 H9 118.3 . . ? C10 C9 H9 118.3 . . ? C11 C10 C9 119.6(3) . . ? C11 C10 H10 120.2 . . ? C9 C10 H10 120.2 . . ? C10 C11 C12 119.1(3) . . ? C10 C11 H11 120.5 . . ? C12 C11 H11 120.5 . . ? C17 C12 C11 118.3(3) . . ? C17 C12 C13 118.9(3) . . ? C11 C12 C13 122.8(3) . . ? C14 C13 C12 120.7(3) . . ? C14 C13 H13 119.6 . . ? C12 C13 H13 119.6 . . ? C13 C14 C15 120.2(3) . . ? C13 C14 H14 119.9 . . ? C15 C14 H14 119.9 . . ? C16 C15 C14 119.7(3) . . ? C16 C15 H15 120.2 . . ? C14 C15 H15 120.2 . . ? C15 C16 C17 121.9(3) . . ? C15 C16 S1 120.1(3) . . ? C17 C16 S1 118.0(3) . . ? N1 C17 C16 119.8(3) . . ? N1 C17 C12 121.6(3) . . ? C16 C17 C12 118.5(3) . . ? N2 C18 C19 123.0(3) . . ? N2 C18 H18 118.5 . . ? C19 C18 H18 118.5 . . ? C20 C19 C18 119.7(3) . . ? C20 C19 H19 120.2 . . ? C18 C19 H19 120.2 . . ? C19 C20 C21 119.0(3) . . ? C19 C20 H20 120.5 . . ? C21 C20 H20 120.5 . . ? C26 C21 C20 118.3(3) . . ? C26 C21 C22 119.0(3) . . ? C20 C21 C22 122.6(3) . . ? C23 C22 C21 120.6(4) . . ? C23 C22 H22 119.7 . . ? C21 C22 H22 119.7 . . ? C22 C23 C24 120.3(3) . . ? C22 C23 H23 119.8 . . ? C24 C23 H23 119.8 . . ? C25 C24 C23 119.7(4) . . ? C25 C24 H24 120.2 . . ? C23 C24 H24 120.2 . . ? C24 C25 C26 121.2(3) . . ? C24 C25 S2 120.8(3) . . ? C26 C25 S2 117.6(3) . . ? N2 C26 C25 119.8(3) . . ? N2 C26 C21 121.0(3) . . ? C25 C26 C21 119.0(3) . . ? F1 B1 F4 113.8(12) . . ? F1 B1 F2 110.5(10) . . ? F4 B1 F2 105.6(11) . . ? F1 B1 F3 106.2(9) . . ? F4 B1 F3 113.0(11) . . ? F2 B1 F3 107.6(9) . . ? F4D B1D F1D 113.9(10) . . ? F4D B1D F2D 111.7(10) . . ? F1D B1D F2D 111.7(10) . . ? F4D B1D F3D 102.6(12) . . ? F1D B1D F3D 104.2(10) . . ? F2D B1D F3D 112.1(12) . . ? F6 B2 F7 109.4(3) . . ? F6 B2 F8 109.5(3) . . ? F7 B2 F8 109.8(3) . . ? F6 B2 F5 109.3(3) . . ? F7 B2 F5 110.0(3) . . ? F8 B2 F5 108.7(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Pd1 S1 C16 133.9(6) . . . . ? N1 Pd1 S1 C16 -4.44(13) . . . . ? S2 Pd1 S1 C16 -178.18(12) . . . . ? N2 Pd1 S1 C1 -117.5(6) . . . . ? N1 Pd1 S1 C1 104.17(15) . . . . ? S2 Pd1 S1 C1 -69.58(13) . . . . ? N2 Pd1 S2 C25 -14.17(14) . . . . ? N1 Pd1 S2 C25 120.3(6) . . . . ? S1 Pd1 S2 C25 171.91(12) . . . . ? N2 Pd1 S2 C8 -119.16(15) . . . . ? N1 Pd1 S2 C8 15.3(6) . . . . ? S1 Pd1 S2 C8 66.91(13) . . . . ? N2 Pd1 N1 C9 13.0(3) . . . . ? S1 Pd1 N1 C9 -172.5(3) . . . . ? S2 Pd1 N1 C9 -120.6(5) . . . . ? N2 Pd1 N1 C17 -167.1(2) . . . . ? S1 Pd1 N1 C17 7.4(2) . . . . ? S2 Pd1 N1 C17 59.3(7) . . . . ? N1 Pd1 N2 C18 25.4(3) . . . . ? S1 Pd1 N2 C18 -112.1(5) . . . . ? S2 Pd1 N2 C18 -160.4(3) . . . . ? N1 Pd1 N2 C26 -158.6(2) . . . . ? S1 Pd1 N2 C26 63.9(7) . . . . ? S2 Pd1 N2 C26 15.6(2) . . . . ? C16 S1 C1 C2 -156.9(3) . . . . ? Pd1 S1 C1 C2 97.5(2) . . . . ? S1 C1 C2 C3 98.7(3) . . . . ? S1 C1 C2 C7 -79.6(4) . . . . ? C7 C2 C3 C4 -1.2(5) . . . . ? C1 C2 C3 C4 -179.5(3) . . . . ? C2 C3 C4 C5 0.9(6) . . . . ? C3 C4 C5 C6 0.4(6) . . . . ? C4 C5 C6 C7 -1.4(6) . . . . ? C5 C6 C7 C2 1.0(5) . . . . ? C5 C6 C7 C8 179.9(3) . . . . ? C3 C2 C7 C6 0.3(5) . . . . ? C1 C2 C7 C6 178.5(3) . . . . ? C3 C2 C7 C8 -178.5(3) . . . . ? C1 C2 C7 C8 -0.3(5) . . . . ? C6 C7 C8 S2 -94.4(3) . . . . ? C2 C7 C8 S2 84.4(4) . . . . ? C25 S2 C8 C7 159.1(3) . . . . ? Pd1 S2 C8 C7 -98.5(2) . . . . ? C17 N1 C9 C10 5.6(5) . . . . ? Pd1 N1 C9 C10 -174.6(3) . . . . ? N1 C9 C10 C11 -1.1(5) . . . . ? C9 C10 C11 C12 -3.4(5) . . . . ? C10 C11 C12 C17 3.3(5) . . . . ? C10 C11 C12 C13 -173.6(3) . . . . ? C17 C12 C13 C14 -2.2(5) . . . . ? C11 C12 C13 C14 174.7(3) . . . . ? C12 C13 C14 C15 2.0(6) . . . . ? C13 C14 C15 C16 -0.5(6) . . . . ? C14 C15 C16 C17 -0.7(5) . . . . ? C14 C15 C16 S1 178.8(3) . . . . ? C1 S1 C16 C15 70.6(3) . . . . ? Pd1 S1 C16 C15 -177.4(3) . . . . ? C1 S1 C16 C17 -109.9(3) . . . . ? Pd1 S1 C16 C17 2.0(3) . . . . ? C9 N1 C17 C16 171.7(3) . . . . ? Pd1 N1 C17 C16 -8.2(4) . . . . ? C9 N1 C17 C12 -5.6(5) . . . . ? Pd1 N1 C17 C12 174.6(2) . . . . ? C15 C16 C17 N1 -176.9(3) . . . . ? S1 C16 C17 N1 3.7(4) . . . . ? C15 C16 C17 C12 0.4(5) . . . . ? S1 C16 C17 C12 -179.0(2) . . . . ? C11 C12 C17 N1 1.2(5) . . . . ? C13 C12 C17 N1 178.3(3) . . . . ? C11 C12 C17 C16 -176.0(3) . . . . ? C13 C12 C17 C16 1.0(5) . . . . ? C26 N2 C18 C19 9.1(5) . . . . ? Pd1 N2 C18 C19 -174.9(3) . . . . ? N2 C18 C19 C20 -2.0(5) . . . . ? C18 C19 C20 C21 -4.7(5) . . . . ? C19 C20 C21 C26 4.0(5) . . . . ? C19 C20 C21 C22 -172.5(3) . . . . ? C26 C21 C22 C23 -3.9(5) . . . . ? C20 C21 C22 C23 172.6(4) . . . . ? C21 C22 C23 C24 -0.2(6) . . . . ? C22 C23 C24 C25 3.6(6) . . . . ? C23 C24 C25 C26 -2.9(6) . . . . ? C23 C24 C25 S2 -175.2(3) . . . . ? C8 S2 C25 C24 -66.5(3) . . . . ? Pd1 S2 C25 C24 -173.3(3) . . . . ? C8 S2 C25 C26 121.0(3) . . . . ? Pd1 S2 C25 C26 14.1(3) . . . . ? C18 N2 C26 C25 165.6(3) . . . . ? Pd1 N2 C26 C25 -10.7(4) . . . . ? C18 N2 C26 C21 -9.6(5) . . . . ? Pd1 N2 C26 C21 174.0(2) . . . . ? C24 C25 C26 N2 -176.5(3) . . . . ? S2 C25 C26 N2 -4.0(4) . . . . ? C24 C25 C26 C21 -1.1(5) . . . . ? S2 C25 C26 C21 171.4(3) . . . . ? C20 C21 C26 N2 3.2(5) . . . . ? C22 C21 C26 N2 179.8(3) . . . . ? C20 C21 C26 C25 -172.1(3) . . . . ? C22 C21 C26 C25 4.5(5) . . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.04 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 3.543 _refine_diff_density_min -0.529 _refine_diff_density_rms 0.105 data_03203 _database_code_depnum_ccdc_archive 'CCDC 268259' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H18 N2 S2' _chemical_formula_weight 422.54 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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.8181(6) _cell_length_b 11.2558(9) _cell_length_c 11.7943(9) _cell_angle_alpha 86.300(2) _cell_angle_beta 81.141(2) _cell_angle_gamma 88.620(2) _cell_volume 1023.26(14) _cell_formula_units_Z 2 _cell_measurement_temperature 130(2) _cell_measurement_reflns_used 6162 _cell_measurement_theta_min 2.4 _cell_measurement_theta_max 26.4 _exptl_crystal_description 'irregular block' _exptl_crystal_colour colorless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.371 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 440 _exptl_absorpt_coefficient_mu 0.276 _exptl_absorpt_correction_type multi-scans _exptl_absorpt_correction_T_min 0.9520 _exptl_absorpt_correction_T_max 0.9729 _exptl_absorpt_process_details 'SADABS, R. Blessing (1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 130(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_details '0.30 degree frames measured for 40 seconds each' _diffrn_measurement_method \w-scans _diffrn_measurement_device 'three-circle goniometer with fixed chi' _diffrn_measurement_device_type 'Bruker Platform goniometer' _diffrn_detector 'CCD area detector' _diffrn_detector_type 'Bruker SMART 6000' _diffrn_detector_area_resol_mean 44.52 _diffrn_standards_number 118 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 793 _diffrn_standards_decay_% 0.0 _diffrn_reflns_number 17797 _diffrn_reflns_av_R_equivalents 0.0341 _diffrn_reflns_av_sigmaI/netI 0.0277 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.44 _diffrn_reflns_theta_max 26.42 _reflns_number_total 4166 _reflns_number_gt 3576 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2002)' _computing_cell_refinement 'SAINT (Bruker, 2002)' _computing_data_reduction 'SAINT (Bruker, 2002)' _computing_structure_solution 'SHELXD (Sheldrick, 2002)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XTEL (local library)' _computing_publication_material 'XCIF (Bruker, 2002), XTEL (local library)' _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^)+(0.0520P)^2^+0.4032P] 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 4166 _refine_ls_number_parameters 271 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0422 _refine_ls_R_factor_gt 0.0349 _refine_ls_wR_factor_ref 0.0984 _refine_ls_wR_factor_gt 0.0924 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.054 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group S1 S 0.19034(5) 0.76664(3) 0.01745(3) 0.02430(12) Uani 1 1 d . . . S2 S 0.06429(5) 0.83391(3) 0.49817(3) 0.02332(11) Uani 1 1 d . . . N1 N -0.10015(17) 0.64407(11) -0.02279(11) 0.0228(3) Uani 1 1 d . . . N2 N -0.17542(17) 0.64644(12) 0.54605(11) 0.0243(3) Uani 1 1 d . . . C1 C 0.3473(2) 0.88466(14) 0.00560(13) 0.0234(3) Uani 1 1 d . . . H1A H 0.4063 0.8960 -0.0748 0.028 Uiso 1 1 calc R . . H1B H 0.2884 0.9604 0.0279 0.028 Uiso 1 1 calc R . . C2 C 0.4732(2) 0.85117(14) 0.08170(13) 0.0244(3) Uani 1 1 d . . . C3 C 0.5776(2) 0.82430(14) 0.14310(13) 0.0237(3) Uani 1 1 d . . . C4 C 0.7090(2) 0.79204(14) 0.21090(13) 0.0239(3) Uani 1 1 d . . . H4 H 0.8164 0.7631 0.1727 0.029 Uiso 1 1 calc R . . C5 C 0.6913(2) 0.79973(14) 0.32525(13) 0.0235(3) Uani 1 1 d . . . H5 H 0.7857 0.7750 0.3635 0.028 Uiso 1 1 calc R . . C6 C 0.5380(2) 0.84309(13) 0.39191(13) 0.0231(3) Uani 1 1 d . . . C7 C 0.4102(2) 0.88129(14) 0.44812(13) 0.0247(3) Uani 1 1 d . . . C8 C 0.2481(2) 0.92464(14) 0.51102(14) 0.0255(3) Uani 1 1 d . . . H8A H 0.2261 1.0072 0.4820 0.031 Uiso 1 1 calc R . . H8B H 0.2597 0.9266 0.5933 0.031 Uiso 1 1 calc R . . C9 C 0.0500(2) 0.82482(13) -0.07640(12) 0.0211(3) Uani 1 1 d . . . C10 C 0.0669(2) 0.93304(14) -0.13888(13) 0.0240(3) Uani 1 1 d . . . H10 H 0.1609 0.9832 -0.1333 0.029 Uiso 1 1 calc R . . C11 C -0.0557(2) 0.96929(14) -0.21121(13) 0.0270(3) Uani 1 1 d . . . H11 H -0.0434 1.0442 -0.2534 0.032 Uiso 1 1 calc R . . C12 C -0.1909(2) 0.89903(15) -0.22145(13) 0.0264(3) Uani 1 1 d . . . H12 H -0.2721 0.9252 -0.2703 0.032 Uiso 1 1 calc R . . C13 C -0.2110(2) 0.78709(14) -0.15954(12) 0.0230(3) Uani 1 1 d . . . C14 C -0.3467(2) 0.70851(15) -0.16572(13) 0.0262(3) Uani 1 1 d . . . H14 H -0.4317 0.7295 -0.2133 0.031 Uiso 1 1 calc R . . C15 C -0.3548(2) 0.60220(15) -0.10295(13) 0.0273(3) Uani 1 1 d . . . H15 H -0.4447 0.5480 -0.1068 0.033 Uiso 1 1 calc R . . C16 C -0.2281(2) 0.57399(14) -0.03233(13) 0.0262(3) Uani 1 1 d . . . H16 H -0.2357 0.4997 0.0110 0.031 Uiso 1 1 calc R . . C17 C -0.09013(19) 0.75030(13) -0.08618(12) 0.0205(3) Uani 1 1 d . . . C18 C 0.09389(19) 0.70943(13) 0.59155(12) 0.0207(3) Uani 1 1 d . . . C19 C 0.2321(2) 0.68997(14) 0.64953(13) 0.0243(3) Uani 1 1 d . . . H19 H 0.3234 0.7457 0.6393 0.029 Uiso 1 1 calc R . . C20 C 0.2393(2) 0.58716(15) 0.72463(13) 0.0279(4) Uani 1 1 d . . . H20 H 0.3348 0.5754 0.7653 0.034 Uiso 1 1 calc R . . C21 C 0.1121(2) 0.50520(15) 0.73948(13) 0.0281(4) Uani 1 1 d . . . H21 H 0.1184 0.4375 0.7912 0.034 Uiso 1 1 calc R . . C22 C -0.0295(2) 0.51990(14) 0.67858(13) 0.0239(3) Uani 1 1 d . . . C23 C -0.1639(2) 0.43693(15) 0.68659(14) 0.0286(4) Uani 1 1 d . . . H23 H -0.1614 0.3656 0.7340 0.034 Uiso 1 1 calc R . . C24 C -0.2971(2) 0.45943(15) 0.62618(14) 0.0305(4) Uani 1 1 d . . . H24 H -0.3879 0.4040 0.6302 0.037 Uiso 1 1 calc R . . C25 C -0.2977(2) 0.56646(16) 0.55766(14) 0.0285(4) Uani 1 1 d . . . H25 H -0.3927 0.5819 0.5171 0.034 Uiso 1 1 calc R . . C26 C -0.04045(19) 0.62390(13) 0.60498(12) 0.0209(3) 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 0.0270(2) 0.0217(2) 0.0249(2) 0.00550(15) -0.00875(15) -0.00345(15) S2 0.0248(2) 0.0233(2) 0.0214(2) 0.00502(14) -0.00516(14) 0.00049(15) N1 0.0265(7) 0.0212(6) 0.0200(6) 0.0013(5) -0.0025(5) -0.0018(5) N2 0.0236(6) 0.0297(7) 0.0200(6) -0.0003(5) -0.0051(5) 0.0000(5) C1 0.0264(8) 0.0227(8) 0.0209(7) 0.0019(6) -0.0042(6) -0.0037(6) C2 0.0279(8) 0.0221(8) 0.0229(7) -0.0005(6) -0.0022(6) -0.0046(6) C3 0.0282(8) 0.0212(7) 0.0211(7) -0.0002(6) -0.0017(6) -0.0028(6) C4 0.0241(8) 0.0215(7) 0.0255(8) 0.0019(6) -0.0035(6) 0.0004(6) C5 0.0225(7) 0.0221(7) 0.0261(8) 0.0017(6) -0.0054(6) -0.0011(6) C6 0.0277(8) 0.0215(7) 0.0207(7) 0.0027(6) -0.0067(6) -0.0035(6) C7 0.0290(8) 0.0220(8) 0.0231(7) 0.0024(6) -0.0055(6) -0.0034(6) C8 0.0282(8) 0.0219(8) 0.0251(8) 0.0014(6) -0.0013(6) -0.0017(6) C9 0.0255(7) 0.0203(7) 0.0169(7) 0.0006(5) -0.0020(6) 0.0005(6) C10 0.0302(8) 0.0217(8) 0.0198(7) 0.0017(6) -0.0038(6) -0.0014(6) C11 0.0368(9) 0.0239(8) 0.0192(7) 0.0041(6) -0.0036(6) 0.0031(7) C12 0.0325(8) 0.0292(8) 0.0176(7) 0.0018(6) -0.0066(6) 0.0049(7) C13 0.0262(8) 0.0264(8) 0.0161(7) -0.0028(6) -0.0017(6) 0.0027(6) C14 0.0263(8) 0.0346(9) 0.0185(7) -0.0031(6) -0.0051(6) 0.0017(7) C15 0.0270(8) 0.0316(9) 0.0232(8) -0.0033(6) -0.0019(6) -0.0071(7) C16 0.0314(8) 0.0237(8) 0.0225(8) 0.0010(6) -0.0021(6) -0.0030(6) C17 0.0250(7) 0.0211(7) 0.0142(6) -0.0005(5) -0.0001(5) 0.0012(6) C18 0.0238(7) 0.0223(7) 0.0153(7) -0.0001(5) -0.0019(5) 0.0028(6) C19 0.0254(8) 0.0270(8) 0.0205(7) 0.0011(6) -0.0048(6) -0.0005(6) C20 0.0296(8) 0.0319(9) 0.0229(8) 0.0033(6) -0.0090(6) 0.0049(7) C21 0.0373(9) 0.0250(8) 0.0214(7) 0.0039(6) -0.0054(7) 0.0056(7) C22 0.0307(8) 0.0230(8) 0.0172(7) -0.0011(6) -0.0015(6) 0.0024(6) C23 0.0381(9) 0.0229(8) 0.0229(8) -0.0002(6) 0.0008(7) -0.0019(7) C24 0.0334(9) 0.0306(9) 0.0276(8) -0.0054(7) -0.0024(7) -0.0088(7) C25 0.0263(8) 0.0362(9) 0.0240(8) -0.0026(7) -0.0065(6) -0.0029(7) C26 0.0233(7) 0.0243(8) 0.0148(7) -0.0013(6) -0.0020(6) 0.0025(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag S1 C9 1.7616(16) . ? S1 C1 1.8141(16) . ? S2 C18 1.7587(15) . ? S2 C8 1.8138(17) . ? N1 C16 1.311(2) . ? N1 C17 1.3659(19) . ? N2 C25 1.315(2) . ? N2 C26 1.3606(19) . ? C1 C2 1.459(2) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C3 1.193(2) . ? C3 C4 1.423(2) . ? C4 C5 1.343(2) . ? C4 H4 0.9500 . ? C5 C6 1.423(2) . ? C5 H5 0.9500 . ? C6 C7 1.197(2) . ? C7 C8 1.457(2) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.381(2) . ? C9 C17 1.419(2) . ? C10 C11 1.415(2) . ? C10 H10 0.9500 . ? C11 C12 1.360(2) . ? C11 H11 0.9500 . ? C12 C13 1.414(2) . ? C12 H12 0.9500 . ? C13 C14 1.411(2) . ? C13 C17 1.414(2) . ? C14 C15 1.363(2) . ? C14 H14 0.9500 . ? C15 C16 1.407(2) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C18 C19 1.371(2) . ? C18 C26 1.426(2) . ? C19 C20 1.417(2) . ? C19 H19 0.9500 . ? C20 C21 1.357(2) . ? C20 H20 0.9500 . ? C21 C22 1.410(2) . ? C21 H21 0.9500 . ? C22 C23 1.411(2) . ? C22 C26 1.421(2) . ? C23 C24 1.360(3) . ? C23 H23 0.9500 . ? C24 C25 1.407(2) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C9 S1 C1 101.24(7) . . ? C18 S2 C8 102.05(7) . . ? C16 N1 C17 117.41(13) . . ? C25 N2 C26 117.46(14) . . ? C2 C1 S1 108.30(11) . . ? C2 C1 H1A 110.0 . . ? S1 C1 H1A 110.0 . . ? C2 C1 H1B 110.0 . . ? S1 C1 H1B 110.0 . . ? H1A C1 H1B 108.4 . . ? C3 C2 C1 179.32(17) . . ? C2 C3 C4 176.88(16) . . ? C5 C4 C3 124.34(14) . . ? C5 C4 H4 117.8 . . ? C3 C4 H4 117.8 . . ? C4 C5 C6 123.18(14) . . ? C4 C5 H5 118.4 . . ? C6 C5 H5 118.4 . . ? C7 C6 C5 178.93(17) . . ? C6 C7 C8 176.16(17) . . ? C7 C8 S2 113.10(11) . . ? C7 C8 H8A 109.0 . . ? S2 C8 H8A 109.0 . . ? C7 C8 H8B 109.0 . . ? S2 C8 H8B 109.0 . . ? H8A C8 H8B 107.8 . . ? C10 C9 C17 119.45(14) . . ? C10 C9 S1 125.80(12) . . ? C17 C9 S1 114.75(11) . . ? C9 C10 C11 120.03(15) . . ? C9 C10 H10 120.0 . . ? C11 C10 H10 120.0 . . ? C12 C11 C10 121.27(14) . . ? C12 C11 H11 119.4 . . ? C10 C11 H11 119.4 . . ? C11 C12 C13 120.13(15) . . ? C11 C12 H12 119.9 . . ? C13 C12 H12 119.9 . . ? C14 C13 C17 117.08(14) . . ? C14 C13 C12 123.78(14) . . ? C17 C13 C12 119.15(14) . . ? C15 C14 C13 119.49(15) . . ? C15 C14 H14 120.3 . . ? C13 C14 H14 120.3 . . ? C14 C15 C16 119.02(15) . . ? C14 C15 H15 120.5 . . ? C16 C15 H15 120.5 . . ? N1 C16 C15 123.96(15) . . ? N1 C16 H16 118.0 . . ? C15 C16 H16 118.0 . . ? N1 C17 C13 123.05(14) . . ? N1 C17 C9 116.98(13) . . ? C13 C17 C9 119.97(13) . . ? C19 C18 C26 119.55(14) . . ? C19 C18 S2 125.57(12) . . ? C26 C18 S2 114.88(11) . . ? C18 C19 C20 120.28(15) . . ? C18 C19 H19 119.9 . . ? C20 C19 H19 119.9 . . ? C21 C20 C19 121.12(15) . . ? C21 C20 H20 119.4 . . ? C19 C20 H20 119.4 . . ? C20 C21 C22 120.39(14) . . ? C20 C21 H21 119.8 . . ? C22 C21 H21 119.8 . . ? C21 C22 C23 123.76(15) . . ? C21 C22 C26 119.09(15) . . ? C23 C22 C26 117.14(14) . . ? C24 C23 C22 119.76(15) . . ? C24 C23 H23 120.1 . . ? C22 C23 H23 120.1 . . ? C23 C24 C25 118.64(16) . . ? C23 C24 H24 120.7 . . ? C25 C24 H24 120.7 . . ? N2 C25 C24 124.28(15) . . ? N2 C25 H25 117.9 . . ? C24 C25 H25 117.9 . . ? N2 C26 C22 122.68(14) . . ? N2 C26 C18 117.79(13) . . ? C22 C26 C18 119.52(14) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C9 S1 C1 C2 178.68(11) . . . . ? S1 C1 C2 C3 143(15) . . . . ? C1 C2 C3 C4 -27(17) . . . . ? C2 C3 C4 C5 166(3) . . . . ? C3 C4 C5 C6 -0.9(2) . . . . ? C4 C5 C6 C7 -103(9) . . . . ? C5 C6 C7 C8 134(8) . . . . ? C6 C7 C8 S2 30(3) . . . . ? C18 S2 C8 C7 76.32(12) . . . . ? C1 S1 C9 C10 0.11(15) . . . . ? C1 S1 C9 C17 179.76(11) . . . . ? C17 C9 C10 C11 0.5(2) . . . . ? S1 C9 C10 C11 -179.86(12) . . . . ? C9 C10 C11 C12 -0.4(2) . . . . ? C10 C11 C12 C13 -0.2(2) . . . . ? C11 C12 C13 C14 -179.61(14) . . . . ? C11 C12 C13 C17 0.8(2) . . . . ? C17 C13 C14 C15 -0.6(2) . . . . ? C12 C13 C14 C15 179.81(15) . . . . ? C13 C14 C15 C16 0.7(2) . . . . ? C17 N1 C16 C15 -0.4(2) . . . . ? C14 C15 C16 N1 -0.2(2) . . . . ? C16 N1 C17 C13 0.5(2) . . . . ? C16 N1 C17 C9 -179.21(13) . . . . ? C14 C13 C17 N1 0.0(2) . . . . ? C12 C13 C17 N1 179.63(14) . . . . ? C14 C13 C17 C9 179.68(13) . . . . ? C12 C13 C17 C9 -0.7(2) . . . . ? C10 C9 C17 N1 179.75(13) . . . . ? S1 C9 C17 N1 0.08(17) . . . . ? C10 C9 C17 C13 0.1(2) . . . . ? S1 C9 C17 C13 -179.62(11) . . . . ? C8 S2 C18 C19 -3.98(15) . . . . ? C8 S2 C18 C26 176.21(11) . . . . ? C26 C18 C19 C20 -1.6(2) . . . . ? S2 C18 C19 C20 178.55(12) . . . . ? C18 C19 C20 C21 1.1(2) . . . . ? C19 C20 C21 C22 1.0(2) . . . . ? C20 C21 C22 C23 177.95(15) . . . . ? C20 C21 C22 C26 -2.4(2) . . . . ? C21 C22 C23 C24 178.86(15) . . . . ? C26 C22 C23 C24 -0.8(2) . . . . ? C22 C23 C24 C25 -0.6(2) . . . . ? C26 N2 C25 C24 -0.4(2) . . . . ? C23 C24 C25 N2 1.3(3) . . . . ? C25 N2 C26 C22 -1.1(2) . . . . ? C25 N2 C26 C18 179.13(13) . . . . ? C21 C22 C26 N2 -177.94(14) . . . . ? C23 C22 C26 N2 1.7(2) . . . . ? C21 C22 C26 C18 1.8(2) . . . . ? C23 C22 C26 C18 -178.55(13) . . . . ? C19 C18 C26 N2 179.98(13) . . . . ? S2 C18 C26 N2 -0.20(18) . . . . ? C19 C18 C26 C22 0.2(2) . . . . ? S2 C18 C26 C22 -179.96(11) . . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 26.42 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.317 _refine_diff_density_min -0.401 _refine_diff_density_rms 0.052