# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Dr JoseLuis Serrano' _publ_contact_author_email jose.serrano@upct.es _publ_section_title ; Novel saccharinate-bridged palladium complexes for efficient C-O bond activation displaying promising luminescence properties. ; loop_ _publ_author_name J.Serrano J.Perez L.Garcia E.Perez M.D.Santana R.Garcia-Bueno ; G.Sanchez ; J.Garcia A.Kapdi G.Garcia S.Pednekar M.Naik # Attachment '- RevisedCrystalData.cif' data_compound_I1 _database_code_depnum_ccdc_archive 'CCDC 831012' #TrackingRef '- RevisedCrystalData.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H24 N4 O6 Pd2 S2, C H2 CL2' _chemical_formula_sum 'C37 H26 Cl2 N4 O6 Pd2 S2' _chemical_formula_weight 970.44 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 15.1661(10) _cell_length_b 17.9439(12) _cell_length_c 26.0050(18) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7077.0(8) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8681 _cell_measurement_theta_min 1.92 _cell_measurement_theta_max 28.62 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.822 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3856 _exptl_absorpt_coefficient_mu 1.340 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7570 _exptl_absorpt_correction_T_max 0.9360 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 81257 _diffrn_reflns_av_R_equivalents 0.0330 _diffrn_reflns_av_sigmaI/netI 0.0203 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 1.92 _diffrn_reflns_theta_max 28.62 _reflns_number_total 8681 _reflns_number_gt 8482 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _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^)+(0.0000P)^2^+33.8885P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8681 _refine_ls_number_parameters 478 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0510 _refine_ls_R_factor_gt 0.0488 _refine_ls_wR_factor_ref 0.0908 _refine_ls_wR_factor_gt 0.0897 _refine_ls_goodness_of_fit_ref 1.417 _refine_ls_restrained_S_all 1.417 _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 0.169787(19) 0.133735(16) 0.296986(11) 0.01238(7) Uani 1 1 d . . . N1 N 0.2351(2) 0.20432(17) 0.25044(12) 0.0128(6) Uani 1 1 d . . . C1 C 0.2680(2) 0.2705(2) 0.26507(15) 0.0154(8) Uani 1 1 d . . . H1 H 0.2636 0.2847 0.3002 0.019 Uiso 1 1 calc R . . C2 C 0.3077(3) 0.3185(2) 0.23101(16) 0.0164(8) Uani 1 1 d . . . H2 H 0.3282 0.3659 0.2421 0.020 Uiso 1 1 calc R . . C3 C 0.3175(3) 0.2963(2) 0.18009(16) 0.0172(8) Uani 1 1 d . . . H3 H 0.3465 0.3278 0.1561 0.021 Uiso 1 1 calc R . . C4 C 0.2846(2) 0.2281(2) 0.16474(15) 0.0147(7) Uani 1 1 d . . . H4 H 0.2917 0.2120 0.1302 0.018 Uiso 1 1 calc R . . C5 C 0.2409(2) 0.1830(2) 0.20026(14) 0.0133(7) Uani 1 1 d . . . C6 C 0.1948(2) 0.1132(2) 0.18978(15) 0.0135(7) Uani 1 1 d . . . C7 C 0.1852(3) 0.0825(2) 0.14046(16) 0.0184(8) Uani 1 1 d . . . H7 H 0.2128 0.1058 0.1119 0.022 Uiso 1 1 calc R . . C8 C 0.1359(3) 0.0185(2) 0.13326(17) 0.0224(9) Uani 1 1 d . . . H8 H 0.1300 -0.0024 0.0999 0.027 Uiso 1 1 calc R . . C9 C 0.0949(3) -0.0151(2) 0.17513(17) 0.0223(9) Uani 1 1 d . . . H9 H 0.0603 -0.0587 0.1701 0.027 Uiso 1 1 calc R . . C10 C 0.1040(3) 0.0146(2) 0.22433(17) 0.0184(8) Uani 1 1 d . . . H10 H 0.0765 -0.0094 0.2527 0.022 Uiso 1 1 calc R . . C11 C 0.1533(3) 0.0792(2) 0.23225(15) 0.0147(7) Uani 1 1 d . . . N2 N 0.0962(2) 0.06205(19) 0.34105(13) 0.0161(7) Uani 1 1 d . . . S1 S 0.14592(7) -0.00204(7) 0.37629(5) 0.0263(3) Uani 1 1 d . . . O3 O 0.2102(2) 0.0332(2) 0.40813(17) 0.0514(13) Uani 1 1 d . . . O4 O 0.1743(3) -0.0633(2) 0.34493(16) 0.0488(12) Uani 1 1 d . . . C12 C 0.0515(3) -0.0265(2) 0.41205(15) 0.0163(8) Uani 1 1 d . . . C13 C 0.0422(3) -0.0771(2) 0.45156(16) 0.0208(9) Uani 1 1 d . . . H13 H 0.0902 -0.1066 0.4633 0.025 Uiso 1 1 calc R . . C14 C -0.0410(3) -0.0829(2) 0.47328(16) 0.0235(9) Uani 1 1 d . . . H14 H -0.0500 -0.1169 0.5008 0.028 Uiso 1 1 calc R . . C15 C -0.1113(3) -0.0407(2) 0.45619(18) 0.0250(10) Uani 1 1 d . . . H15 H -0.1675 -0.0465 0.4718 0.030 Uiso 1 1 calc R . . C16 C -0.1008(3) 0.0105(2) 0.41626(17) 0.0210(9) Uani 1 1 d . . . H16 H -0.1488 0.0400 0.4046 0.025 Uiso 1 1 calc R . . C17 C -0.0178(3) 0.0167(2) 0.39428(15) 0.0161(8) Uani 1 1 d . . . C18 C 0.0103(3) 0.0694(2) 0.35301(14) 0.0138(7) Uani 1 1 d . . . O1 O -0.04114(18) 0.11554(15) 0.33371(10) 0.0154(6) Uani 1 1 d . . . Pd2 Pd 0.010088(19) 0.221375(16) 0.305926(11) 0.01136(7) Uani 1 1 d . . . N3 N -0.0285(2) 0.20560(18) 0.23248(12) 0.0128(6) Uani 1 1 d . . . C19 C -0.0720(3) 0.1453(2) 0.21582(15) 0.0163(8) Uani 1 1 d . . . H19 H -0.0819 0.1050 0.2388 0.020 Uiso 1 1 calc R . . C20 C -0.1028(3) 0.1404(3) 0.16566(16) 0.0208(9) Uani 1 1 d . . . H20 H -0.1340 0.0976 0.1544 0.025 Uiso 1 1 calc R . . C21 C -0.0872(3) 0.1991(3) 0.13249(16) 0.0236(9) Uani 1 1 d . . . H21 H -0.1085 0.1971 0.0982 0.028 Uiso 1 1 calc R . . C22 C -0.0408(3) 0.2603(3) 0.14914(15) 0.0201(8) Uani 1 1 d . . . H22 H -0.0295 0.3006 0.1264 0.024 Uiso 1 1 calc R . . C23 C -0.0105(3) 0.2629(2) 0.20006(15) 0.0144(7) Uani 1 1 d . . . C24 C 0.0401(3) 0.3232(2) 0.22387(15) 0.0146(7) Uani 1 1 d . . . C25 C 0.0744(3) 0.3840(2) 0.19672(17) 0.0203(8) Uani 1 1 d . . . H25 H 0.0650 0.3882 0.1607 0.024 Uiso 1 1 calc R . . C26 C 0.1219(3) 0.4378(2) 0.22254(17) 0.0211(9) Uani 1 1 d . . . H26 H 0.1460 0.4788 0.2042 0.025 Uiso 1 1 calc R . . C27 C 0.1347(3) 0.4324(2) 0.27532(17) 0.0203(9) Uani 1 1 d . . . H27 H 0.1667 0.4700 0.2929 0.024 Uiso 1 1 calc R . . C28 C 0.1007(3) 0.3716(2) 0.30262(16) 0.0171(8) Uani 1 1 d . . . H28 H 0.1094 0.3686 0.3387 0.020 Uiso 1 1 calc R . . C29 C 0.0542(3) 0.3155(2) 0.27732(15) 0.0153(8) Uani 1 1 d . . . N4 N 0.0566(2) 0.23875(18) 0.37881(12) 0.0127(6) Uani 1 1 d . . . S2 S -0.00633(6) 0.27084(6) 0.42582(4) 0.01575(19) Uani 1 1 d . . . O5 O -0.0294(2) 0.34713(17) 0.41641(12) 0.0251(7) Uani 1 1 d . . . O6 O -0.07757(19) 0.22093(19) 0.43617(11) 0.0240(7) Uani 1 1 d . . . C30 C 0.0748(3) 0.2620(2) 0.47367(15) 0.0135(7) Uani 1 1 d . . . C31 C 0.0676(3) 0.2750(2) 0.52605(15) 0.0174(8) Uani 1 1 d . . . H31 H 0.0162 0.2968 0.5405 0.021 Uiso 1 1 calc R . . C32 C 0.1394(3) 0.2548(2) 0.55647(15) 0.0184(8) Uani 1 1 d . . . H32 H 0.1366 0.2623 0.5926 0.022 Uiso 1 1 calc R . . C33 C 0.2148(3) 0.2237(2) 0.53497(15) 0.0200(8) Uani 1 1 d . . . H33 H 0.2629 0.2102 0.5565 0.024 Uiso 1 1 calc R . . C34 C 0.2205(3) 0.2121(2) 0.48201(15) 0.0177(8) Uani 1 1 d . . . H34 H 0.2720 0.1911 0.4671 0.021 Uiso 1 1 calc R . . C35 C 0.1493(3) 0.2319(2) 0.45194(15) 0.0140(7) Uani 1 1 d . . . C36 C 0.1381(3) 0.2201(2) 0.39510(14) 0.0143(7) Uani 1 1 d . . . O2 O 0.19801(18) 0.19527(16) 0.36756(10) 0.0167(6) Uani 1 1 d . . . Cl1 Cl 0.70071(10) 0.07726(7) 0.50820(5) 0.0383(3) Uani 1 1 d . . . Cl2 Cl 0.59843(9) -0.05979(7) 0.51293(6) 0.0383(3) Uani 1 1 d . . . C37 C 0.6233(3) 0.0251(3) 0.54434(19) 0.0297(11) Uani 1 1 d . . . H37A H 0.6477 0.0146 0.5789 0.036 Uiso 1 1 calc R . . H37B H 0.5686 0.0546 0.5487 0.036 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.01238(13) 0.01455(13) 0.01020(13) 0.00219(11) 0.00246(10) 0.00108(11) N1 0.0111(15) 0.0154(15) 0.0119(14) 0.0018(13) 0.0008(12) 0.0020(12) C1 0.0126(18) 0.0200(19) 0.0137(18) -0.0004(15) -0.0027(14) 0.0019(15) C2 0.0144(18) 0.0136(18) 0.021(2) -0.0001(15) -0.0006(15) 0.0008(15) C3 0.0152(19) 0.0184(19) 0.0181(19) 0.0058(15) 0.0013(15) 0.0004(15) C4 0.0123(17) 0.0183(19) 0.0133(18) 0.0028(15) -0.0001(14) 0.0023(15) C5 0.0104(16) 0.0162(18) 0.0131(17) 0.0016(15) 0.0003(14) 0.0056(14) C6 0.0094(16) 0.0168(18) 0.0145(18) -0.0015(14) -0.0001(14) 0.0026(14) C7 0.021(2) 0.0199(19) 0.0144(19) -0.0009(15) 0.0029(15) 0.0012(16) C8 0.027(2) 0.022(2) 0.019(2) -0.0066(17) -0.0019(17) 0.0014(18) C9 0.022(2) 0.0159(19) 0.028(2) -0.0030(17) -0.0017(18) 0.0007(17) C10 0.0166(19) 0.0141(18) 0.025(2) 0.0008(16) 0.0050(16) 0.0035(15) C11 0.0115(18) 0.0160(18) 0.0167(18) 0.0001(15) 0.0020(14) 0.0042(14) N2 0.0144(16) 0.0175(16) 0.0165(16) 0.0067(13) 0.0019(13) 0.0007(13) S1 0.0154(5) 0.0295(6) 0.0341(6) 0.0200(5) 0.0043(4) 0.0053(4) O3 0.0242(18) 0.060(3) 0.070(3) 0.047(2) -0.0238(19) -0.0172(18) O4 0.050(2) 0.039(2) 0.058(3) 0.0279(19) 0.036(2) 0.0312(19) C12 0.0194(19) 0.0155(18) 0.0140(18) 0.0016(15) 0.0014(15) -0.0025(15) C13 0.028(2) 0.0140(19) 0.020(2) -0.0006(16) -0.0008(17) -0.0022(16) C14 0.040(3) 0.0154(19) 0.0152(19) 0.0002(16) 0.0053(18) -0.0075(18) C15 0.029(2) 0.021(2) 0.025(2) -0.0020(18) 0.0141(19) -0.0087(18) C16 0.022(2) 0.020(2) 0.021(2) -0.0041(17) 0.0023(17) -0.0014(17) C17 0.021(2) 0.0124(17) 0.0150(18) -0.0035(14) 0.0011(15) -0.0042(15) C18 0.0128(17) 0.0163(18) 0.0122(17) -0.0006(14) -0.0009(14) 0.0004(14) O1 0.0167(13) 0.0154(13) 0.0141(13) 0.0005(11) 0.0000(11) -0.0006(11) Pd2 0.01294(13) 0.01246(13) 0.00867(12) 0.00015(10) -0.00133(10) 0.00173(11) N3 0.0124(15) 0.0139(15) 0.0121(15) -0.0013(12) -0.0016(12) 0.0023(12) C19 0.0166(19) 0.0182(19) 0.0140(18) -0.0007(15) 0.0015(15) 0.0043(15) C20 0.018(2) 0.028(2) 0.016(2) -0.0087(17) -0.0009(16) -0.0011(17) C21 0.019(2) 0.041(3) 0.0108(18) -0.0033(18) -0.0028(15) 0.0029(19) C22 0.019(2) 0.029(2) 0.0115(18) 0.0033(16) 0.0000(15) -0.0002(17) C23 0.0156(18) 0.0152(18) 0.0125(17) 0.0048(14) -0.0010(14) 0.0056(14) C24 0.0118(17) 0.0153(18) 0.0168(18) 0.0033(15) -0.0020(14) 0.0017(14) C25 0.021(2) 0.022(2) 0.018(2) 0.0056(16) 0.0005(16) 0.0009(17) C26 0.020(2) 0.0167(19) 0.026(2) 0.0067(17) 0.0005(17) 0.0000(16) C27 0.019(2) 0.0117(18) 0.030(2) 0.0006(16) -0.0016(17) -0.0001(15) C28 0.0171(19) 0.0160(18) 0.0181(19) -0.0008(16) 0.0002(15) 0.0036(15) C29 0.0155(18) 0.0144(18) 0.0160(19) 0.0023(15) -0.0004(15) 0.0018(15) N4 0.0145(15) 0.0164(16) 0.0073(14) -0.0025(12) 0.0001(12) 0.0004(12) S2 0.0147(4) 0.0206(5) 0.0120(4) -0.0032(4) -0.0020(3) 0.0042(4) O5 0.0330(18) 0.0252(16) 0.0171(15) -0.0042(12) -0.0084(13) 0.0144(14) O6 0.0161(14) 0.0374(18) 0.0184(15) -0.0047(14) -0.0010(12) -0.0003(13) C30 0.0148(18) 0.0127(18) 0.0130(18) 0.0001(14) -0.0021(14) -0.0045(14) C31 0.0183(19) 0.0194(19) 0.0147(18) -0.0020(16) 0.0012(15) -0.0001(16) C32 0.023(2) 0.023(2) 0.0089(17) -0.0022(15) -0.0007(15) -0.0011(17) C33 0.020(2) 0.028(2) 0.0121(18) 0.0015(16) -0.0053(15) -0.0049(17) C34 0.0144(18) 0.023(2) 0.0163(19) 0.0013(16) -0.0001(15) -0.0014(16) C35 0.0149(18) 0.0152(18) 0.0119(17) -0.0014(14) -0.0017(14) -0.0023(14) C36 0.0152(18) 0.0152(18) 0.0124(17) 0.0014(14) 0.0001(14) -0.0020(15) O2 0.0154(13) 0.0237(15) 0.0110(13) -0.0014(11) 0.0022(10) 0.0004(11) Cl1 0.0492(8) 0.0251(6) 0.0406(7) 0.0088(5) -0.0090(6) 0.0066(5) Cl2 0.0396(7) 0.0254(6) 0.0498(8) -0.0036(5) -0.0151(6) 0.0052(5) C37 0.028(2) 0.030(2) 0.032(3) -0.007(2) -0.008(2) 0.009(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 C11 1.963(4) . ? Pd1 N1 2.012(3) . ? Pd1 N2 2.053(3) . ? Pd1 O2 2.184(3) . ? Pd1 Pd2 2.8971(4) . ? N1 C1 1.344(5) . ? N1 C5 1.363(5) . ? C1 C2 1.374(5) . ? C2 C3 1.391(6) . ? C3 C4 1.380(6) . ? C4 C5 1.396(5) . ? C5 C6 1.460(5) . ? C6 C7 1.403(5) . ? C6 C11 1.410(5) . ? C7 C8 1.384(6) . ? C8 C9 1.391(6) . ? C9 C10 1.393(6) . ? C10 C11 1.395(6) . ? N2 C18 1.346(5) . ? N2 S1 1.653(3) . ? S1 O3 1.427(4) . ? S1 O4 1.435(4) . ? S1 C12 1.763(4) . ? C12 C13 1.379(6) . ? C12 C17 1.385(6) . ? C13 C14 1.386(6) . ? C14 C15 1.381(7) . ? C15 C16 1.395(6) . ? C16 C17 1.388(6) . ? C17 C18 1.492(5) . ? C18 O1 1.243(5) . ? O1 Pd2 2.175(3) . ? Pd2 C29 1.962(4) . ? Pd2 N3 2.018(3) . ? Pd2 N4 2.046(3) . ? N3 C19 1.339(5) . ? N3 C23 1.357(5) . ? C19 C20 1.388(6) . ? C20 C21 1.381(6) . ? C21 C22 1.374(6) . ? C22 C23 1.403(5) . ? C23 C24 1.464(5) . ? C24 C25 1.400(6) . ? C24 C29 1.413(5) . ? C25 C26 1.380(6) . ? C26 C27 1.390(6) . ? C27 C28 1.400(6) . ? C28 C29 1.395(6) . ? N4 C36 1.349(5) . ? N4 S2 1.654(3) . ? S2 O6 1.429(3) . ? S2 O5 1.434(3) . ? S2 C30 1.757(4) . ? C30 C35 1.373(5) . ? C30 C31 1.386(5) . ? C31 C32 1.393(6) . ? C32 C33 1.391(6) . ? C33 C34 1.395(5) . ? C34 C35 1.380(5) . ? C35 C36 1.503(5) . ? C36 O2 1.240(5) . ? Cl1 C37 1.771(6) . ? Cl2 C37 1.769(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C11 Pd1 N1 81.99(15) . . ? C11 Pd1 N2 95.56(15) . . ? N1 Pd1 N2 176.11(13) . . ? C11 Pd1 O2 175.93(13) . . ? N1 Pd1 O2 95.21(12) . . ? N2 Pd1 O2 87.39(12) . . ? C11 Pd1 Pd2 103.46(11) . . ? N1 Pd1 Pd2 96.77(9) . . ? N2 Pd1 Pd2 80.83(9) . . ? O2 Pd1 Pd2 79.75(7) . . ? C1 N1 C5 119.7(3) . . ? C1 N1 Pd1 124.7(3) . . ? C5 N1 Pd1 115.6(3) . . ? N1 C1 C2 122.3(4) . . ? C1 C2 C3 118.8(4) . . ? C4 C3 C2 119.4(4) . . ? C3 C4 C5 119.6(4) . . ? N1 C5 C4 120.1(4) . . ? N1 C5 C6 112.9(3) . . ? C4 C5 C6 127.0(4) . . ? C7 C6 C11 120.0(4) . . ? C7 C6 C5 123.8(4) . . ? C11 C6 C5 116.0(3) . . ? C8 C7 C6 120.4(4) . . ? C7 C8 C9 119.7(4) . . ? C8 C9 C10 120.6(4) . . ? C9 C10 C11 120.5(4) . . ? C10 C11 C6 118.9(4) . . ? C10 C11 Pd1 127.5(3) . . ? C6 C11 Pd1 113.5(3) . . ? C18 N2 S1 112.5(3) . . ? C18 N2 Pd1 126.4(3) . . ? S1 N2 Pd1 119.81(19) . . ? O3 S1 O4 117.7(3) . . ? O3 S1 N2 109.0(2) . . ? O4 S1 N2 110.8(2) . . ? O3 S1 C12 111.0(2) . . ? O4 S1 C12 110.7(2) . . ? N2 S1 C12 95.43(18) . . ? C13 C12 C17 122.7(4) . . ? C13 C12 S1 129.8(3) . . ? C17 C12 S1 107.5(3) . . ? C12 C13 C14 116.5(4) . . ? C15 C14 C13 122.0(4) . . ? C14 C15 C16 120.9(4) . . ? C17 C16 C15 117.6(4) . . ? C12 C17 C16 120.4(4) . . ? C12 C17 C18 112.3(3) . . ? C16 C17 C18 127.3(4) . . ? O1 C18 N2 125.4(4) . . ? O1 C18 C17 122.3(4) . . ? N2 C18 C17 112.3(3) . . ? C18 O1 Pd2 119.4(3) . . ? C29 Pd2 N3 81.99(15) . . ? C29 Pd2 N4 95.89(15) . . ? N3 Pd2 N4 176.60(13) . . ? C29 Pd2 O1 177.06(14) . . ? N3 Pd2 O1 95.07(12) . . ? N4 Pd2 O1 87.04(12) . . ? C29 Pd2 Pd1 98.74(12) . . ? N3 Pd2 Pd1 95.19(9) . . ? N4 Pd2 Pd1 82.48(9) . . ? O1 Pd2 Pd1 81.45(7) . . ? C19 N3 C23 120.7(3) . . ? C19 N3 Pd2 124.2(3) . . ? C23 N3 Pd2 115.0(3) . . ? N3 C19 C20 121.4(4) . . ? C21 C20 C19 118.8(4) . . ? C22 C21 C20 120.0(4) . . ? C21 C22 C23 119.4(4) . . ? N3 C23 C22 119.7(4) . . ? N3 C23 C24 113.8(3) . . ? C22 C23 C24 126.6(4) . . ? C25 C24 C29 121.1(4) . . ? C25 C24 C23 123.9(4) . . ? C29 C24 C23 115.0(3) . . ? C26 C25 C24 119.6(4) . . ? C25 C26 C27 120.3(4) . . ? C26 C27 C28 120.3(4) . . ? C29 C28 C27 120.7(4) . . ? C28 C29 C24 118.0(4) . . ? C28 C29 Pd2 127.9(3) . . ? C24 C29 Pd2 114.0(3) . . ? C36 N4 S2 112.5(3) . . ? C36 N4 Pd2 124.7(3) . . ? S2 N4 Pd2 122.62(18) . . ? O6 S2 O5 116.5(2) . . ? O6 S2 N4 110.91(18) . . ? O5 S2 N4 110.30(18) . . ? O6 S2 C30 109.85(18) . . ? O5 S2 C30 112.19(18) . . ? N4 S2 C30 95.06(18) . . ? C35 C30 C31 122.4(4) . . ? C35 C30 S2 108.7(3) . . ? C31 C30 S2 128.7(3) . . ? C30 C31 C32 116.9(4) . . ? C33 C32 C31 121.3(4) . . ? C32 C33 C34 120.5(4) . . ? C35 C34 C33 118.2(4) . . ? C30 C35 C34 120.8(4) . . ? C30 C35 C36 111.6(3) . . ? C34 C35 C36 127.5(4) . . ? O2 C36 N4 125.4(4) . . ? O2 C36 C35 122.4(4) . . ? N4 C36 C35 112.2(3) . . ? C36 O2 Pd1 121.6(3) . . ? Cl2 C37 Cl1 110.6(3) . . ? _diffrn_measured_fraction_theta_max 0.956 _diffrn_reflns_theta_full 0.50 _diffrn_measured_fraction_theta_full 0.000 _refine_diff_density_max 0.765 _refine_diff_density_min -0.618 _refine_diff_density_rms 0.124 #===END data_compound_I2 _database_code_depnum_ccdc_archive 'CCDC 831013' #TrackingRef '- RevisedCrystalData.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C23 H17 N3 O3 Pd S' _chemical_formula_sum 'C23 H17 N3 O3 Pd S' _chemical_formula_weight 521.86 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 30.576(3) _cell_length_b 8.0645(8) _cell_length_c 16.6896(17) _cell_angle_alpha 90.00 _cell_angle_beta 97.634(2) _cell_angle_gamma 90.00 _cell_volume 4078.9(7) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 4885 _cell_measurement_theta_min 1.34 _cell_measurement_theta_max 28.51 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.700 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2096 _exptl_absorpt_coefficient_mu 1.044 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8105 _exptl_absorpt_correction_T_max 0.9496 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23618 _diffrn_reflns_av_R_equivalents 0.1257 _diffrn_reflns_av_sigmaI/netI 0.0696 _diffrn_reflns_limit_h_min -39 _diffrn_reflns_limit_h_max 40 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.34 _diffrn_reflns_theta_max 28.51 _reflns_number_total 4885 _reflns_number_gt 4650 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _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^)+(0.0407P)^2^+62.7436P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4885 _refine_ls_number_parameters 270 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0811 _refine_ls_R_factor_gt 0.0745 _refine_ls_wR_factor_ref 0.1836 _refine_ls_wR_factor_gt 0.1704 _refine_ls_goodness_of_fit_ref 1.370 _refine_ls_restrained_S_all 1.370 _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 C8 C 0.2923(2) -0.0245(7) 0.0097(4) 0.0153(12) Uani 1 1 d . . . H8 H 0.3225 -0.0217 0.0321 0.018 Uiso 1 1 calc R . . C10 C 0.2348(2) -0.1128(8) -0.0932(4) 0.0182(13) Uani 1 1 d . . . H10 H 0.2252 -0.1702 -0.1420 0.022 Uiso 1 1 calc R . . C9 C 0.2792(2) -0.1103(8) -0.0618(4) 0.0179(12) Uani 1 1 d . . . H9 H 0.3003 -0.1665 -0.0888 0.022 Uiso 1 1 calc R . . N2 N 0.11652(17) 0.0795(8) 0.0155(3) 0.0218(12) Uani 1 1 d . . . Pd1 Pd 0.175677(15) 0.16681(6) 0.08499(3) 0.01253(15) Uani 1 1 d . A . C6 C 0.2696(2) 0.1543(7) 0.1222(4) 0.0143(11) Uani 1 1 d . A . N3 N 0.13885(17) 0.2823(7) 0.1629(3) 0.0158(10) Uani 1 1 d . . . N1 N 0.21754(17) 0.0519(6) 0.0173(3) 0.0133(10) Uani 1 1 d . . . C1 C 0.2326(2) 0.2277(7) 0.1496(4) 0.0143(12) Uani 1 1 d . . . C3 C 0.2817(2) 0.3477(8) 0.2612(4) 0.0200(13) Uani 1 1 d . . . H3 H 0.2858 0.4134 0.3089 0.024 Uiso 1 1 calc R A . C2 C 0.2394(2) 0.3255(8) 0.2195(4) 0.0178(12) Uani 1 1 d . A . H2 H 0.2149 0.3773 0.2387 0.021 Uiso 1 1 calc R . . C5 C 0.3122(2) 0.1796(8) 0.1635(4) 0.0193(13) Uani 1 1 d . . . H5 H 0.3371 0.1321 0.1435 0.023 Uiso 1 1 calc R A . C4 C 0.3179(2) 0.2738(8) 0.2331(4) 0.0188(13) Uani 1 1 d . A . H4 H 0.3466 0.2882 0.2619 0.023 Uiso 1 1 calc R . . C22 C 0.0949(2) 0.5089(9) 0.1976(5) 0.0237(14) Uani 1 1 d . . . H22 H 0.0811 0.6121 0.1830 0.028 Uiso 1 1 calc R A . C11 C 0.2048(2) -0.0305(8) -0.0524(4) 0.0166(12) Uani 1 1 d . A . H11 H 0.1745 -0.0320 -0.0739 0.020 Uiso 1 1 calc R . . C7 C 0.2606(2) 0.0576(8) 0.0486(4) 0.0146(12) Uani 1 1 d . A . C21 C 0.0909(2) 0.4372(10) 0.2714(5) 0.0259(15) Uani 1 1 d . A . H21 H 0.0751 0.4919 0.3089 0.031 Uiso 1 1 calc R . . C19 C 0.1342(2) 0.2105(10) 0.2338(4) 0.0247(15) Uani 1 1 d . A . H19 H 0.1475 0.1056 0.2462 0.030 Uiso 1 1 calc R . . C20 C 0.1104(3) 0.2846(10) 0.2901(5) 0.0298(16) Uani 1 1 d . . . H20 H 0.1076 0.2316 0.3400 0.036 Uiso 1 1 calc R A . C23 C 0.1193(2) 0.4281(8) 0.1449(4) 0.0191(13) Uani 1 1 d . A . H23 H 0.1221 0.4782 0.0943 0.023 Uiso 1 1 calc R . . S1A S 0.08135(13) 0.1511(5) -0.0566(3) 0.0192(10) Uiso 0.471(6) 1 d P A 1 O1A O 0.1021(4) 0.1732(15) -0.1284(7) 0.033(3) Uiso 0.471(6) 1 d P A 1 O2A O 0.0616(4) 0.2978(14) -0.0284(7) 0.028(3) Uiso 0.471(6) 1 d P A 1 O3A O 0.1223(4) -0.1864(14) 0.0825(7) 0.027(2) Uiso 0.471(6) 1 d P A 1 C12A C 0.0439(4) -0.016(2) -0.0720(9) 0.014(3) Uiso 0.471(6) 1 d P A 1 C13A C 0.0065(4) -0.0308(18) -0.1275(8) 0.019(3) Uiso 0.471(6) 1 d P A 1 H13A H -0.0051 0.0578 -0.1615 0.022 Uiso 0.471(6) 1 calc PR A 1 C14A C -0.0132(6) -0.190(2) -0.1293(10) 0.023(4) Uiso 0.471(6) 1 d P A 1 H14A H -0.0394 -0.2077 -0.1656 0.028 Uiso 0.471(6) 1 calc PR A 1 C15A C 0.0030(5) -0.3172(19) -0.0828(9) 0.022(3) Uiso 0.471(6) 1 d P A 1 H15A H -0.0116 -0.4214 -0.0881 0.026 Uiso 0.471(6) 1 calc PR A 1 C16A C 0.0407(5) -0.2997(19) -0.0274(9) 0.022(3) Uiso 0.471(6) 1 d P A 1 H16A H 0.0523 -0.3889 0.0061 0.026 Uiso 0.471(6) 1 calc PR A 1 C17A C 0.0610(4) -0.1411(17) -0.0233(7) 0.010(2) Uiso 0.471(6) 1 d P A 1 C18A C 0.0944(6) -0.081(2) 0.0241(11) 0.004(5) Uiso 0.471(6) 1 d P A 1 S1B S 0.10016(17) -0.0979(7) 0.0305(3) 0.0186(15) Uiso 0.529(6) 1 d P A 2 O1B O 0.1258(3) -0.2207(13) 0.0024(6) 0.026(2) Uiso 0.529(6) 1 d P A 2 O2B O 0.0875(3) -0.1133(13) 0.1095(6) 0.027(2) Uiso 0.529(6) 1 d P A 2 O3B O 0.0956(3) 0.3290(12) -0.0548(6) 0.025(2) Uiso 0.529(6) 1 d P A 2 C12B C 0.0499(4) -0.0687(19) -0.0433(9) 0.018(2) Uiso 0.529(6) 1 d P A 2 C13B C 0.0174(5) -0.186(2) -0.0682(9) 0.030(3) Uiso 0.529(6) 1 d P A 2 H13B H 0.0181 -0.2948 -0.0465 0.036 Uiso 0.529(6) 1 calc PR A 2 C14B C -0.0162(6) -0.131(3) -0.1273(11) 0.033(4) Uiso 0.529(6) 1 d P A 2 H14B H -0.0392 -0.2057 -0.1466 0.040 Uiso 0.529(6) 1 calc PR A 2 C15B C -0.0169(5) 0.025(2) -0.1580(9) 0.032(3) Uiso 0.529(6) 1 d P A 2 H15B H -0.0407 0.0578 -0.1974 0.039 Uiso 0.529(6) 1 calc PR A 2 C16B C 0.0163(5) 0.138(2) -0.1328(9) 0.030(3) Uiso 0.529(6) 1 d P A 2 H16B H 0.0159 0.2465 -0.1546 0.036 Uiso 0.529(6) 1 calc PR A 2 C17B C 0.0501(4) 0.0861(18) -0.0751(8) 0.020(3) Uiso 0.529(6) 1 d P A 2 C18B C 0.0888(5) 0.1845(19) -0.0365(9) 0.016(3) Uiso 0.529(6) 1 d P A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C8 0.025(3) 0.002(3) 0.020(3) 0.003(2) 0.005(2) 0.001(2) C10 0.034(4) 0.009(3) 0.013(3) -0.006(2) 0.009(3) -0.003(2) C9 0.027(3) 0.013(3) 0.015(3) 0.001(2) 0.010(2) 0.001(2) N2 0.015(2) 0.029(3) 0.022(3) 0.000(2) 0.002(2) 0.004(2) Pd1 0.0154(2) 0.0102(2) 0.0124(2) 0.00117(17) 0.00324(16) -0.00047(17) C6 0.025(3) 0.005(3) 0.013(3) 0.001(2) 0.004(2) 0.000(2) N3 0.018(2) 0.014(3) 0.016(2) 0.000(2) 0.001(2) 0.0000(19) N1 0.023(3) 0.005(2) 0.013(2) -0.0008(18) 0.007(2) -0.0016(19) C1 0.019(3) 0.008(3) 0.017(3) 0.003(2) 0.003(2) -0.003(2) C3 0.029(3) 0.013(3) 0.018(3) 0.004(2) 0.002(3) -0.002(3) C2 0.020(3) 0.016(3) 0.019(3) 0.001(2) 0.008(2) 0.004(2) C5 0.026(3) 0.012(3) 0.019(3) 0.000(2) 0.002(2) 0.004(2) C4 0.023(3) 0.015(3) 0.017(3) 0.000(2) -0.003(2) -0.001(2) C22 0.018(3) 0.015(3) 0.037(4) -0.002(3) 0.002(3) 0.004(3) C11 0.023(3) 0.011(3) 0.015(3) 0.001(2) 0.002(2) -0.008(2) C7 0.022(3) 0.010(3) 0.013(3) 0.002(2) 0.004(2) 0.001(2) C21 0.022(3) 0.029(4) 0.029(4) -0.007(3) 0.007(3) -0.001(3) C19 0.027(3) 0.028(4) 0.020(3) 0.008(3) 0.007(3) 0.006(3) C20 0.033(4) 0.034(4) 0.026(4) 0.008(3) 0.013(3) 0.005(3) C23 0.017(3) 0.018(3) 0.022(3) 0.001(3) 0.003(2) -0.005(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C8 C9 1.393(9) . ? C8 C7 1.401(8) . ? C10 C11 1.383(9) . ? C10 C9 1.387(10) . ? N2 C18B 1.412(15) . ? N2 C18A 1.474(19) . ? N2 S1B 1.547(8) . ? N2 S1A 1.612(7) . ? N2 Pd1 2.134(6) . ? Pd1 C1 1.984(6) . ? Pd1 N1 2.039(5) . ? Pd1 N3 2.053(5) . ? C6 C1 1.404(9) . ? C6 C5 1.407(9) . ? C6 C7 1.451(8) . ? N3 C23 1.336(9) . ? N3 C19 1.343(8) . ? N1 C11 1.351(8) . ? N1 C7 1.352(8) . ? C1 C2 1.400(9) . ? C3 C4 1.392(10) . ? C3 C2 1.399(9) . ? C5 C4 1.379(9) . ? C22 C21 1.380(11) . ? C22 C23 1.389(10) . ? C21 C20 1.384(11) . ? C19 C20 1.396(10) . ? S1A O2A 1.435(12) . ? S1A O1A 1.440(13) . ? S1A C12A 1.765(15) . ? S1A C18A 2.308(19) . ? O3A C18A 1.48(2) . ? C12A C17A 1.356(18) . ? C12A C13A 1.378(19) . ? C13A C14A 1.42(2) . ? C14A C15A 1.34(2) . ? C15A C16A 1.38(2) . ? C16A C17A 1.419(19) . ? C17A C18A 1.30(2) . ? S1B O1B 1.382(11) . ? S1B O2B 1.426(11) . ? S1B C12B 1.853(16) . ? O3B C18B 1.229(17) . ? C12B C17B 1.36(2) . ? C12B C13B 1.392(19) . ? C13B C14B 1.40(2) . ? C14B C15B 1.36(3) . ? C15B C16B 1.39(2) . ? C16B C17B 1.378(19) . ? C17B C18B 1.50(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C9 C8 C7 119.5(6) . . ? C11 C10 C9 119.1(6) . . ? C10 C9 C8 119.1(6) . . ? C18B N2 C18A 109.9(11) . . ? C18B N2 S1B 118.3(8) . . ? C18A N2 S1B 8.7(8) . . ? C18B N2 S1A 16.0(6) . . ? C18A N2 S1A 96.7(8) . . ? S1B N2 S1A 104.8(4) . . ? C18B N2 Pd1 122.1(8) . . ? C18A N2 Pd1 127.1(8) . . ? S1B N2 Pd1 119.1(4) . . ? S1A N2 Pd1 136.1(4) . . ? C1 Pd1 N1 81.0(2) . . ? C1 Pd1 N3 93.4(2) . . ? N1 Pd1 N3 174.0(2) . . ? C1 Pd1 N2 174.9(2) . . ? N1 Pd1 N2 95.6(2) . . ? N3 Pd1 N2 89.8(2) . . ? C1 C6 C5 120.9(6) . . ? C1 C6 C7 115.7(6) . . ? C5 C6 C7 123.4(6) . . ? C23 N3 C19 118.8(6) . . ? C23 N3 Pd1 121.6(4) . . ? C19 N3 Pd1 119.6(5) . . ? C11 N1 C7 120.2(5) . . ? C11 N1 Pd1 124.8(4) . . ? C7 N1 Pd1 115.0(4) . . ? C2 C1 C6 118.2(6) . . ? C2 C1 Pd1 127.8(5) . . ? C6 C1 Pd1 113.9(4) . . ? C4 C3 C2 120.1(6) . . ? C3 C2 C1 120.8(6) . . ? C4 C5 C6 119.8(6) . . ? C5 C4 C3 120.3(6) . . ? C21 C22 C23 119.1(7) . . ? N1 C11 C10 121.7(6) . . ? N1 C7 C8 120.2(6) . . ? N1 C7 C6 114.2(5) . . ? C8 C7 C6 125.6(6) . . ? C22 C21 C20 119.2(7) . . ? N3 C19 C20 122.3(7) . . ? C21 C20 C19 118.4(7) . . ? N3 C23 C22 122.2(6) . . ? O2A S1A O1A 115.0(7) . . ? O2A S1A N2 108.5(6) . . ? O1A S1A N2 110.0(6) . . ? O2A S1A C12A 112.6(7) . . ? O1A S1A C12A 108.8(7) . . ? N2 S1A C12A 101.0(6) . . ? O2A S1A C18A 121.5(7) . . ? O1A S1A C18A 121.7(7) . . ? N2 S1A C18A 39.4(5) . . ? C12A S1A C18A 61.6(7) . . ? C17A C12A C13A 123.9(13) . . ? C17A C12A S1A 106.9(10) . . ? C13A C12A S1A 128.9(13) . . ? C12A C13A C14A 113.8(14) . . ? C15A C14A C13A 123.9(15) . . ? C14A C15A C16A 121.3(15) . . ? C15A C16A C17A 116.3(14) . . ? C18A C17A C12A 107.1(14) . . ? C18A C17A C16A 132.0(15) . . ? C12A C17A C16A 120.8(12) . . ? C17A C18A N2 127.1(16) . . ? C17A C18A O3A 121.6(15) . . ? N2 C18A O3A 109.6(13) . . ? C17A C18A S1A 83.5(11) . . ? N2 C18A S1A 43.9(6) . . ? O3A C18A S1A 153.0(12) . . ? O1B S1B O2B 119.1(7) . . ? O1B S1B N2 113.4(6) . . ? O2B S1B N2 111.3(6) . . ? O1B S1B C12B 108.8(6) . . ? O2B S1B C12B 108.9(6) . . ? N2 S1B C12B 91.8(6) . . ? C17B C12B C13B 123.1(15) . . ? C17B C12B S1B 109.3(10) . . ? C13B C12B S1B 127.4(13) . . ? C14B C13B C12B 115.2(16) . . ? C15B C14B C13B 122.1(17) . . ? C14B C15B C16B 121.2(15) . . ? C17B C16B C15B 117.8(14) . . ? C12B C17B C16B 120.6(14) . . ? C12B C17B C18B 111.3(11) . . ? C16B C17B C18B 128.0(13) . . ? O3B C18B N2 128.0(14) . . ? O3B C18B C17B 123.0(13) . . ? N2 C18B C17B 108.8(11) . . ? _diffrn_measured_fraction_theta_max 0.944 _diffrn_reflns_theta_full 0.50 _diffrn_measured_fraction_theta_full 0.000 _refine_diff_density_max 1.254 _refine_diff_density_min -2.837 _refine_diff_density_rms 0.272 #===END data_compound_II2 _database_code_depnum_ccdc_archive 'CCDC 831014' #TrackingRef '- RevisedCrystalData.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C25 H17 N3 O3 Pd S, C H2 CL2' _chemical_formula_sum 'C26 H19 Cl2 N3 O3 Pd S' _chemical_formula_weight 630.80 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/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 8.474(3) _cell_length_b 19.208(7) _cell_length_c 14.671(5) _cell_angle_alpha 90.00 _cell_angle_beta 94.607(6) _cell_angle_gamma 90.00 _cell_volume 2380.5(15) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5676 _cell_measurement_theta_min 1.34 _cell_measurement_theta_max 28.57 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.760 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1264 _exptl_absorpt_coefficient_mu 1.128 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8490 _exptl_absorpt_correction_T_max 0.9152 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26100 _diffrn_reflns_av_R_equivalents 0.0370 _diffrn_reflns_av_sigmaI/netI 0.0320 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.75 _diffrn_reflns_theta_max 28.57 _reflns_number_total 5676 _reflns_number_gt 5464 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _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^)+(0.0565P)^2^+30.9065P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5676 _refine_ls_number_parameters 302 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0802 _refine_ls_R_factor_gt 0.0770 _refine_ls_wR_factor_ref 0.1780 _refine_ls_wR_factor_gt 0.1753 _refine_ls_goodness_of_fit_ref 1.122 _refine_ls_restrained_S_all 1.122 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.34280(5) 0.10306(2) 0.14154(3) 0.01589(14) Uani 1 1 d . . . N1 N 0.2530(6) 0.0200(3) 0.0676(3) 0.0181(10) Uani 1 1 d . . . C1 C 0.1658(7) -0.0322(3) 0.0956(4) 0.0198(11) Uani 1 1 d . . . H1 H 0.1454 -0.0347 0.1583 0.024 Uiso 1 1 calc R . . C2 C 0.1034(8) -0.0834(3) 0.0356(4) 0.0239(13) Uani 1 1 d . . . H2 H 0.0421 -0.1202 0.0578 0.029 Uiso 1 1 calc R . . C3 C 0.1300(8) -0.0807(3) -0.0551(4) 0.0243(13) Uani 1 1 d . . . H3 H 0.0864 -0.1152 -0.0962 0.029 Uiso 1 1 calc R . . C4 C 0.2223(7) -0.0266(3) -0.0870(4) 0.0218(12) Uani 1 1 d . . . C5 C 0.2597(8) -0.0166(4) -0.1802(4) 0.0272(14) Uani 1 1 d . . . H5 H 0.2182 -0.0481 -0.2260 0.033 Uiso 1 1 calc R . . C6 C 0.3525(8) 0.0366(4) -0.2042(4) 0.0251(13) Uani 1 1 d . . . H6 H 0.3773 0.0407 -0.2659 0.030 Uiso 1 1 calc R . . C7 C 0.4146(7) 0.0871(4) -0.1383(4) 0.0232(13) Uani 1 1 d . . . C8 C 0.5088(8) 0.1447(4) -0.1605(5) 0.0278(14) Uani 1 1 d . . . H8 H 0.5379 0.1509 -0.2212 0.033 Uiso 1 1 calc R . . C9 C 0.5577(8) 0.1919(4) -0.0928(5) 0.0281(14) Uani 1 1 d . . . H9 H 0.6198 0.2308 -0.1079 0.034 Uiso 1 1 calc R . . C10 C 0.5179(8) 0.1837(4) -0.0019(4) 0.0245(13) Uani 1 1 d . . . H10 H 0.5532 0.2171 0.0428 0.029 Uiso 1 1 calc R . . C11 C 0.4285(7) 0.1278(3) 0.0230(4) 0.0188(11) Uani 1 1 d . . . C12 C 0.3774(7) 0.0796(3) -0.0467(4) 0.0198(12) Uani 1 1 d . . . C13 C 0.2833(7) 0.0232(3) -0.0223(4) 0.0196(11) Uani 1 1 d . . . N2 N 0.2341(6) 0.0777(3) 0.2649(3) 0.0175(9) Uani 1 1 d . . . C14 C 0.1083(7) 0.1137(3) 0.2936(4) 0.0177(11) Uani 1 1 d . . . O1 O 0.0229(5) 0.1534(2) 0.2460(3) 0.0219(9) Uani 1 1 d . . . C15 C 0.0872(7) 0.1006(3) 0.3928(4) 0.0174(11) Uani 1 1 d . . . C16 C -0.0268(7) 0.1287(3) 0.4451(4) 0.0194(11) Uani 1 1 d . . . H16 H -0.1059 0.1593 0.4189 0.023 Uiso 1 1 calc R . . C17 C -0.0214(7) 0.1106(3) 0.5369(4) 0.0221(12) Uani 1 1 d . . . H17 H -0.0980 0.1291 0.5741 0.027 Uiso 1 1 calc R . . C18 C 0.0944(7) 0.0657(3) 0.5753(4) 0.0226(12) Uani 1 1 d . . . H18 H 0.0950 0.0541 0.6382 0.027 Uiso 1 1 calc R . . C19 C 0.2093(7) 0.0375(3) 0.5238(4) 0.0214(12) Uani 1 1 d . . . H19 H 0.2883 0.0067 0.5498 0.026 Uiso 1 1 calc R . . C20 C 0.2026(7) 0.0566(3) 0.4327(4) 0.0195(11) Uani 1 1 d . . . S1 S 0.32489(17) 0.03171(8) 0.34668(10) 0.0182(3) Uani 1 1 d . . . O2 O 0.3096(6) -0.0420(2) 0.3273(3) 0.0288(10) Uani 1 1 d . . . O3 O 0.4847(5) 0.0563(2) 0.3679(3) 0.0229(9) Uani 1 1 d . . . N3 N 0.4382(6) 0.1900(3) 0.2031(3) 0.0190(10) Uani 1 1 d . . . C21 C 0.3471(7) 0.2439(3) 0.2207(4) 0.0192(11) Uani 1 1 d . . . H21 H 0.2358 0.2399 0.2077 0.023 Uiso 1 1 calc R . . C22 C 0.4083(8) 0.3059(3) 0.2575(4) 0.0254(13) Uani 1 1 d . . . H22 H 0.3406 0.3439 0.2686 0.030 Uiso 1 1 calc R . . C23 C 0.5715(8) 0.3108(4) 0.2777(5) 0.0298(14) Uani 1 1 d . . . H23 H 0.6174 0.3526 0.3021 0.036 Uiso 1 1 calc R . . C24 C 0.6648(8) 0.2546(4) 0.2619(5) 0.0300(14) Uani 1 1 d . . . H24 H 0.7760 0.2569 0.2764 0.036 Uiso 1 1 calc R . . C25 C 0.59694(17) 0.19419(7) 0.22493(10) 0.0265(13) Uani 1 1 d . . . H25 H 0.6622 0.1552 0.2146 0.032 Uiso 1 1 calc R . . Cl1 Cl 1.15888(17) 0.25253(7) 0.00401(10) 0.0325(4) Uiso 1 1 d R . . Cl2 Cl 0.86828(17) 0.29243(7) 0.08371(10) 0.0546(6) Uiso 1 1 d R . . C26 C 1.01838(17) 0.32223(7) 0.01401(10) 0.058(2) Uiso 1 1 d R . . H26A H 1.0723 0.3635 0.0423 0.069 Uiso 1 1 calc R . . H26B H 0.9704 0.3355 -0.0473 0.069 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.0154(2) 0.0168(2) 0.0156(2) -0.00168(15) 0.00227(15) 0.00021(16) N1 0.017(2) 0.017(2) 0.020(2) -0.0028(18) -0.0004(18) 0.0046(18) C1 0.018(3) 0.019(3) 0.022(3) 0.002(2) -0.001(2) 0.004(2) C2 0.028(3) 0.014(3) 0.028(3) -0.001(2) -0.009(2) 0.001(2) C3 0.029(3) 0.019(3) 0.024(3) -0.004(2) -0.005(2) 0.007(2) C4 0.021(3) 0.021(3) 0.022(3) -0.006(2) -0.005(2) 0.007(2) C5 0.027(3) 0.033(3) 0.020(3) -0.006(3) -0.004(2) 0.016(3) C6 0.026(3) 0.033(3) 0.016(3) 0.000(2) 0.001(2) 0.014(3) C7 0.018(3) 0.031(3) 0.021(3) 0.003(2) 0.003(2) 0.013(2) C8 0.021(3) 0.040(4) 0.024(3) 0.011(3) 0.010(2) 0.013(3) C9 0.023(3) 0.031(3) 0.032(3) 0.010(3) 0.009(3) 0.004(3) C10 0.023(3) 0.027(3) 0.024(3) 0.000(2) 0.007(2) 0.001(2) C11 0.017(3) 0.022(3) 0.018(3) 0.003(2) 0.005(2) 0.006(2) C12 0.014(3) 0.026(3) 0.020(3) 0.001(2) 0.002(2) 0.012(2) C13 0.015(3) 0.021(3) 0.022(3) -0.002(2) -0.003(2) 0.007(2) N2 0.017(2) 0.021(2) 0.015(2) -0.0012(18) 0.0022(18) -0.0002(19) C14 0.018(3) 0.017(3) 0.018(3) 0.000(2) 0.003(2) -0.003(2) O1 0.021(2) 0.024(2) 0.020(2) 0.0022(17) 0.0005(16) -0.0015(17) C15 0.020(3) 0.016(3) 0.017(3) -0.001(2) 0.004(2) -0.003(2) C16 0.018(3) 0.017(3) 0.024(3) 0.000(2) 0.003(2) 0.001(2) C17 0.023(3) 0.027(3) 0.017(3) 0.001(2) 0.010(2) 0.001(2) C18 0.026(3) 0.025(3) 0.017(3) 0.001(2) 0.002(2) -0.003(2) C19 0.020(3) 0.023(3) 0.021(3) 0.002(2) 0.001(2) 0.003(2) C20 0.018(3) 0.016(3) 0.025(3) -0.005(2) 0.002(2) 0.000(2) S1 0.0177(6) 0.0185(7) 0.0188(6) -0.0025(5) 0.0036(5) 0.0015(5) O2 0.033(3) 0.020(2) 0.034(3) -0.0076(19) 0.008(2) 0.0014(19) O3 0.017(2) 0.029(2) 0.024(2) -0.0023(18) 0.0023(16) 0.0040(17) N3 0.017(2) 0.020(2) 0.020(2) -0.0009(19) 0.0006(18) -0.0042(19) C21 0.017(3) 0.025(3) 0.016(3) 0.000(2) 0.002(2) -0.003(2) C22 0.029(3) 0.023(3) 0.026(3) -0.006(2) 0.008(2) -0.002(3) C23 0.028(3) 0.033(4) 0.028(3) -0.002(3) 0.002(3) -0.014(3) C24 0.021(3) 0.033(4) 0.035(4) 0.003(3) -0.002(3) -0.008(3) C25 0.021(3) 0.028(3) 0.031(3) 0.001(3) -0.002(2) 0.001(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 C11 1.995(6) . ? Pd1 N3 2.035(5) . ? Pd1 N1 2.041(5) . ? Pd1 N2 2.152(5) . ? N1 C1 1.330(8) . ? N1 C13 1.365(8) . ? C1 C2 1.396(8) . ? C2 C3 1.368(9) . ? C3 C4 1.403(9) . ? C4 C13 1.415(8) . ? C4 C5 1.442(9) . ? C5 C6 1.352(10) . ? C6 C7 1.439(9) . ? C7 C12 1.412(8) . ? C7 C8 1.419(10) . ? C8 C9 1.383(10) . ? C9 C10 1.410(9) . ? C10 C11 1.380(9) . ? C11 C12 1.421(9) . ? C12 C13 1.409(9) . ? N2 C14 1.364(7) . ? N2 S1 1.632(5) . ? C14 O1 1.230(7) . ? C14 C15 1.501(8) . ? C15 C20 1.387(8) . ? C15 C16 1.390(8) . ? C16 C17 1.388(8) . ? C17 C18 1.391(9) . ? C18 C19 1.390(9) . ? C19 C20 1.383(8) . ? C20 S1 1.762(6) . ? S1 O3 1.444(5) . ? S1 O2 1.449(5) . ? N3 C21 1.329(8) . ? N3 C25 1.360(5) . ? C21 C22 1.390(9) . ? C22 C23 1.395(9) . ? C23 C24 1.369(11) . ? C24 C25 1.386(7) . ? Cl1 C26 1.8055 . ? Cl2 C26 1.7890 . ? 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 C11 Pd1 N3 91.8(2) . . ? C11 Pd1 N1 82.5(2) . . ? N3 Pd1 N1 174.2(2) . . ? C11 Pd1 N2 176.0(2) . . ? N3 Pd1 N2 89.63(19) . . ? N1 Pd1 N2 96.0(2) . . ? C1 N1 C13 118.9(5) . . ? C1 N1 Pd1 128.1(4) . . ? C13 N1 Pd1 112.8(4) . . ? N1 C1 C2 121.9(6) . . ? C3 C2 C1 120.2(6) . . ? C2 C3 C4 119.5(6) . . ? C3 C4 C13 117.4(6) . . ? C3 C4 C5 125.8(6) . . ? C13 C4 C5 116.7(6) . . ? C6 C5 C4 121.6(6) . . ? C5 C6 C7 121.6(6) . . ? C12 C7 C8 118.1(6) . . ? C12 C7 C6 118.2(6) . . ? C8 C7 C6 123.7(6) . . ? C9 C8 C7 119.2(6) . . ? C8 C9 C10 121.7(6) . . ? C11 C10 C9 121.1(6) . . ? C10 C11 C12 117.3(6) . . ? C10 C11 Pd1 131.5(5) . . ? C12 C11 Pd1 111.1(4) . . ? C13 C12 C7 119.6(6) . . ? C13 C12 C11 117.7(5) . . ? C7 C12 C11 122.7(6) . . ? N1 C13 C12 115.7(5) . . ? N1 C13 C4 122.1(6) . . ? C12 C13 C4 122.2(6) . . ? C14 N2 S1 112.4(4) . . ? C14 N2 Pd1 122.9(4) . . ? S1 N2 Pd1 122.2(3) . . ? O1 C14 N2 125.3(5) . . ? O1 C14 C15 122.9(5) . . ? N2 C14 C15 111.8(5) . . ? C20 C15 C16 120.1(5) . . ? C20 C15 C14 112.1(5) . . ? C16 C15 C14 127.9(5) . . ? C17 C16 C15 118.0(6) . . ? C16 C17 C18 121.0(6) . . ? C19 C18 C17 121.6(6) . . ? C20 C19 C18 116.5(6) . . ? C19 C20 C15 122.9(6) . . ? C19 C20 S1 129.8(5) . . ? C15 C20 S1 107.4(4) . . ? O3 S1 O2 115.4(3) . . ? O3 S1 N2 111.1(3) . . ? O2 S1 N2 110.9(3) . . ? O3 S1 C20 110.6(3) . . ? O2 S1 C20 110.9(3) . . ? N2 S1 C20 96.3(3) . . ? C21 N3 C25 119.2(4) . . ? C21 N3 Pd1 120.6(4) . . ? C25 N3 Pd1 120.2(3) . . ? N3 C21 C22 122.5(6) . . ? C21 C22 C23 118.3(6) . . ? C24 C23 C22 119.1(6) . . ? C23 C24 C25 120.0(6) . . ? N3 C25 C24 120.9(4) . . ? Cl2 C26 Cl1 108.2 . . ? _diffrn_measured_fraction_theta_max 0.935 _diffrn_reflns_theta_full 0.50 _diffrn_measured_fraction_theta_full 0.000 _refine_diff_density_max 4.248 _refine_diff_density_min -3.038 _refine_diff_density_rms 0.189 #===END