# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full Adv.Synth.Catal. _journal_coden_cambridge 1366 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email gpyap@udel.edu _publ_contact_author_name 'Glenn P. A. Yap' loop_ _publ_author_name 'Yang-Ming Liu' 'Yi-Chun Lin' 'Glenn P. A. Yap' 'Shih-Sheng Sun' 'Tiow-Gan Ong' data_i11488 _database_code_depnum_ccdc_archive 'CCDC 818961' #TrackingRef '4821_web_deposit_cif_file_0_GlennYap_1301086809.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H38 Ag2 Cl2 N6' _chemical_formula_weight 841.36 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 '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 9.9245(4) _cell_length_b 16.8820(7) _cell_length_c 20.6772(9) _cell_angle_alpha 90.00 _cell_angle_beta 94.389(2) _cell_angle_gamma 90.00 _cell_volume 3454.2(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 6551 _cell_measurement_theta_min 2.31 _cell_measurement_theta_max 26.72 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.618 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1696 _exptl_absorpt_coefficient_mu 1.324 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6770 _exptl_absorpt_correction_T_max 0.7455 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2003)' _exptl_special_details ; Data collection is performed with four batch runs at \f = 0.00 \% (600 frames), at \f = 90.00 \% (600 frames), at \f = 180 \% (600 frames) and at \f = 270 \% (600 frames). Frame width = 0.30 \& in \w. Data is merged, corrected for decay, and treated with multi-scan absorption corrections. ; _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 'Bruker AXS APEX diffractometer' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 836.6 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 1 _diffrn_reflns_number 29460 _diffrn_reflns_av_R_equivalents 0.0480 _diffrn_reflns_av_sigmaI/netI 0.0479 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.56 _diffrn_reflns_theta_max 27.10 _reflns_number_total 7633 _reflns_number_gt 5699 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2002)' _computing_cell_refinement 'SAINT (Bruker, 2002)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2001)' _computing_publication_material 'SHELXTL (Sheldrick, 2001)' _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^)+(0.0561P)^2^] 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 7633 _refine_ls_number_parameters 421 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0595 _refine_ls_R_factor_gt 0.0416 _refine_ls_wR_factor_ref 0.1146 _refine_ls_wR_factor_gt 0.1038 _refine_ls_goodness_of_fit_ref 1.092 _refine_ls_restrained_S_all 1.092 _refine_ls_shift/su_max 0.011 _refine_ls_shift/su_mean 0.001 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 Ag1 Ag 0.61559(3) 0.080381(16) 0.008959(15) 0.02483(10) Uani 1 1 d . . . Ag2 Ag 0.04703(3) 0.414233(16) 0.045362(15) 0.02394(10) Uani 1 1 d . . . Cl1 Cl 0.60378(10) -0.01719(5) -0.07417(5) 0.0293(2) Uani 1 1 d . . . Cl2 Cl -0.14618(9) 0.49550(5) 0.05973(5) 0.0238(2) Uani 1 1 d . . . N1 N 0.7612(3) 0.16911(17) 0.12185(14) 0.0183(6) Uani 1 1 d . . . N2 N 0.6979(3) 0.25422(17) 0.04982(15) 0.0187(6) Uani 1 1 d . . . N3 N 0.9267(3) 0.2789(2) -0.15904(16) 0.0277(8) Uani 1 1 d . . . N4 N 0.2923(3) 0.34386(17) 0.11838(14) 0.0182(6) Uani 1 1 d . . . N5 N 0.2297(3) 0.25919(17) 0.04557(14) 0.0189(7) Uani 1 1 d . . . N6 N 0.4109(3) 0.2397(2) -0.17397(15) 0.0257(7) Uani 1 1 d . . . C1 C 0.8949(4) 0.0484(2) 0.13255(18) 0.0212(8) Uani 1 1 d . . . C2 C 0.9212(4) -0.0231(2) 0.16287(19) 0.0238(8) Uani 1 1 d . . . H2A H 0.9926 -0.0551 0.1494 0.029 Uiso 1 1 calc R . . C3 C 0.8467(4) -0.0496(2) 0.21226(19) 0.0234(8) Uani 1 1 d . . . C4 C 0.7426(4) -0.0018(2) 0.23202(18) 0.0230(8) Uani 1 1 d . . . H4A H 0.6915 -0.0194 0.2663 0.028 Uiso 1 1 calc R . . C5 C 0.7120(4) 0.0704(2) 0.20301(18) 0.0183(8) Uani 1 1 d . . . C6 C 0.7896(4) 0.0942(2) 0.15366(17) 0.0166(7) Uani 1 1 d . . . C7 C 0.9777(4) 0.0761(2) 0.0780(2) 0.0287(9) Uani 1 1 d . . . H7A H 1.0593 0.0436 0.0773 0.043 Uiso 1 1 calc R . . H7B H 1.0033 0.1317 0.0851 0.043 Uiso 1 1 calc R . . H7C H 0.9238 0.0709 0.0365 0.043 Uiso 1 1 calc R . . C8 C 0.8807(4) -0.1278(2) 0.2449(2) 0.0343(10) Uani 1 1 d . . . H8A H 0.9772 -0.1291 0.2590 0.051 Uiso 1 1 calc R . . H8B H 0.8594 -0.1711 0.2142 0.051 Uiso 1 1 calc R . . H8C H 0.8275 -0.1340 0.2826 0.051 Uiso 1 1 calc R . . C9 C 0.5946(4) 0.1189(2) 0.22230(19) 0.0255(9) Uani 1 1 d . . . H9A H 0.5521 0.0921 0.2575 0.038 Uiso 1 1 calc R . . H9B H 0.5285 0.1249 0.1849 0.038 Uiso 1 1 calc R . . H9C H 0.6267 0.1712 0.2370 0.038 Uiso 1 1 calc R . . C10 C 0.6929(3) 0.1761(2) 0.06294(17) 0.0184(8) Uani 1 1 d . . . C11 C 0.8082(4) 0.2417(2) 0.14523(19) 0.0234(8) Uani 1 1 d . . . H11A H 0.8580 0.2518 0.1854 0.028 Uiso 1 1 calc R . . C12 C 0.7682(4) 0.2951(2) 0.09889(19) 0.0229(8) Uani 1 1 d . . . H12A H 0.7855 0.3505 0.1001 0.028 Uiso 1 1 calc R . . C13 C 0.6423(4) 0.2894(2) -0.01143(18) 0.0230(8) Uani 1 1 d . . . H13A H 0.6179 0.3453 -0.0038 0.028 Uiso 1 1 calc R . . H13B H 0.5588 0.2607 -0.0268 0.028 Uiso 1 1 calc R . . C14 C 0.8506(4) 0.2172(2) -0.14533(19) 0.0269(9) Uani 1 1 d . . . H14A H 0.8607 0.1697 -0.1691 0.032 Uiso 1 1 calc R . . C15 C 0.7582(4) 0.2175(2) -0.09905(19) 0.0242(8) Uani 1 1 d . . . H15A H 0.7065 0.1715 -0.0916 0.029 Uiso 1 1 calc R . . C16 C 0.7415(3) 0.2860(2) -0.06326(18) 0.0195(8) Uani 1 1 d . . . C17 C 0.8192(4) 0.3508(2) -0.07685(18) 0.0233(8) Uani 1 1 d . . . H17A H 0.8109 0.3990 -0.0539 0.028 Uiso 1 1 calc R . . C18 C 0.9096(4) 0.3445(2) -0.12457(19) 0.0269(9) Uani 1 1 d . . . H18A H 0.9626 0.3896 -0.1332 0.032 Uiso 1 1 calc R . . C19 C 0.3790(3) 0.4767(2) 0.14439(18) 0.0208(8) Uani 1 1 d . . . C20 C 0.3793(4) 0.5420(2) 0.1846(2) 0.0245(9) Uani 1 1 d . . . H20A H 0.4359 0.5856 0.1762 0.029 Uiso 1 1 calc R . . C21 C 0.3002(4) 0.5463(2) 0.23685(19) 0.0237(8) Uani 1 1 d . . . C22 C 0.2181(4) 0.4827(2) 0.24883(18) 0.0220(8) Uani 1 1 d . . . H22A H 0.1637 0.4852 0.2846 0.026 Uiso 1 1 calc R . . C23 C 0.2125(4) 0.4159(2) 0.21062(18) 0.0200(8) Uani 1 1 d . . . C24 C 0.2955(4) 0.4133(2) 0.15878(18) 0.0172(7) Uani 1 1 d . . . C25 C 0.4646(4) 0.4732(3) 0.0868(2) 0.0335(10) Uani 1 1 d . . . H25A H 0.5187 0.5216 0.0853 0.050 Uiso 1 1 calc R . . H25B H 0.4058 0.4684 0.0468 0.050 Uiso 1 1 calc R . . H25C H 0.5248 0.4271 0.0912 0.050 Uiso 1 1 calc R . . C26 C 0.3016(5) 0.6193(2) 0.2795(2) 0.0358(11) Uani 1 1 d . . . H26A H 0.2737 0.6048 0.3224 0.054 Uiso 1 1 calc R . . H26B H 0.2391 0.6588 0.2597 0.054 Uiso 1 1 calc R . . H26C H 0.3932 0.6414 0.2841 0.054 Uiso 1 1 calc R . . C27 C 0.1184(4) 0.3492(2) 0.2227(2) 0.0317(10) Uani 1 1 d . . . H27A H 0.0943 0.3512 0.2677 0.048 Uiso 1 1 calc R . . H27B H 0.1628 0.2986 0.2148 0.048 Uiso 1 1 calc R . . H27C H 0.0364 0.3541 0.1933 0.048 Uiso 1 1 calc R . . C28 C 0.1991(3) 0.3318(2) 0.06837(18) 0.0189(8) Uani 1 1 d . . . C29 C 0.3801(4) 0.2805(2) 0.12663(19) 0.0254(9) Uani 1 1 d . . . H29A H 0.4536 0.2754 0.1586 0.031 Uiso 1 1 calc R . . C30 C 0.3409(4) 0.2275(2) 0.08055(19) 0.0241(9) Uani 1 1 d . . . H30A H 0.3819 0.1777 0.0734 0.029 Uiso 1 1 calc R . . C31 C 0.1636(4) 0.2222(2) -0.01236(18) 0.0224(8) Uani 1 1 d . . . H31A H 0.0760 0.2487 -0.0237 0.027 Uiso 1 1 calc R . . H31B H 0.1454 0.1658 -0.0033 0.027 Uiso 1 1 calc R . . C32 C 0.3427(4) 0.3017(2) -0.15382(19) 0.0231(8) Uani 1 1 d . . . H32A H 0.3489 0.3504 -0.1764 0.028 Uiso 1 1 calc R . . C33 C 0.2633(4) 0.2990(2) -0.10167(19) 0.0209(8) Uani 1 1 d . . . H33A H 0.2175 0.3450 -0.0885 0.025 Uiso 1 1 calc R . . C34 C 0.2518(3) 0.2281(2) -0.06924(17) 0.0172(7) Uani 1 1 d . . . C35 C 0.3228(4) 0.1638(2) -0.08896(18) 0.0209(8) Uani 1 1 d . . . H35A H 0.3183 0.1145 -0.0671 0.025 Uiso 1 1 calc R . . C36 C 0.4007(4) 0.1720(2) -0.14084(19) 0.0251(9) Uani 1 1 d . . . H36A H 0.4499 0.1272 -0.1539 0.030 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 Ag1 0.02957(17) 0.01576(16) 0.02813(18) -0.00201(12) -0.00448(13) -0.00139(11) Ag2 0.02246(16) 0.01941(16) 0.02966(18) -0.00152(12) 0.00000(13) 0.00471(11) Cl1 0.0393(6) 0.0200(5) 0.0307(6) -0.0068(4) 0.0162(5) -0.0064(4) Cl2 0.0250(5) 0.0155(4) 0.0323(5) 0.0017(4) 0.0111(4) 0.0020(4) N1 0.0216(15) 0.0155(15) 0.0187(16) 0.0002(13) 0.0085(13) -0.0014(12) N2 0.0222(15) 0.0160(15) 0.0186(16) 0.0026(13) 0.0069(13) -0.0001(13) N3 0.0246(17) 0.036(2) 0.0228(18) 0.0040(15) 0.0057(15) 0.0016(15) N4 0.0227(15) 0.0153(15) 0.0174(16) -0.0012(13) 0.0069(13) 0.0024(12) N5 0.0216(15) 0.0203(16) 0.0160(16) -0.0044(13) 0.0086(13) 0.0008(13) N6 0.0224(16) 0.0355(19) 0.0202(17) -0.0017(15) 0.0069(14) 0.0003(15) C1 0.0178(18) 0.026(2) 0.021(2) 0.0005(16) 0.0038(15) -0.0028(15) C2 0.0216(19) 0.022(2) 0.027(2) -0.0018(17) -0.0006(16) 0.0021(16) C3 0.026(2) 0.0180(18) 0.025(2) 0.0017(16) -0.0073(17) 0.0000(16) C4 0.0264(19) 0.025(2) 0.0169(19) 0.0044(16) 0.0003(16) -0.0099(16) C5 0.0161(17) 0.0222(19) 0.0167(18) -0.0027(15) 0.0022(15) -0.0029(14) C6 0.0206(18) 0.0130(17) 0.0162(18) 0.0026(14) 0.0013(15) -0.0025(14) C7 0.025(2) 0.034(2) 0.028(2) 0.0038(18) 0.0101(18) 0.0056(17) C8 0.039(2) 0.026(2) 0.037(3) 0.0115(19) -0.007(2) -0.0026(19) C9 0.024(2) 0.028(2) 0.026(2) -0.0021(18) 0.0106(17) -0.0008(17) C10 0.0156(17) 0.0212(19) 0.0191(19) -0.0019(16) 0.0057(15) -0.0016(14) C11 0.029(2) 0.0177(19) 0.024(2) -0.0050(16) 0.0079(17) -0.0059(16) C12 0.026(2) 0.0182(19) 0.025(2) 0.0015(16) 0.0077(17) -0.0039(16) C13 0.0254(19) 0.0198(19) 0.024(2) 0.0052(16) 0.0055(17) 0.0053(16) C14 0.028(2) 0.028(2) 0.025(2) -0.0024(18) 0.0048(18) 0.0057(17) C15 0.027(2) 0.0181(19) 0.028(2) 0.0002(17) 0.0062(17) -0.0002(16) C16 0.0178(17) 0.0232(19) 0.0173(19) 0.0048(16) -0.0009(15) 0.0025(15) C17 0.026(2) 0.0223(19) 0.021(2) 0.0025(16) -0.0009(16) -0.0029(16) C18 0.025(2) 0.031(2) 0.025(2) 0.0065(18) 0.0021(17) -0.0070(17) C19 0.0155(17) 0.024(2) 0.023(2) 0.0012(16) 0.0007(15) -0.0010(15) C20 0.0189(18) 0.0198(19) 0.034(2) 0.0036(18) -0.0011(17) -0.0061(15) C21 0.0235(19) 0.023(2) 0.023(2) -0.0049(17) -0.0072(16) 0.0084(16) C22 0.027(2) 0.023(2) 0.0163(19) -0.0038(16) 0.0041(16) 0.0043(16) C23 0.0215(19) 0.0211(19) 0.0178(19) 0.0021(15) 0.0034(15) 0.0027(15) C24 0.0169(17) 0.0161(18) 0.0190(19) -0.0019(15) 0.0035(15) 0.0025(14) C25 0.032(2) 0.035(2) 0.035(3) 0.003(2) 0.017(2) -0.0056(19) C26 0.043(3) 0.025(2) 0.037(3) -0.012(2) -0.008(2) 0.0098(19) C27 0.037(2) 0.029(2) 0.030(2) -0.0020(19) 0.0116(19) -0.0070(19) C28 0.0201(18) 0.0186(18) 0.0189(19) 0.0019(15) 0.0075(15) 0.0001(15) C29 0.027(2) 0.022(2) 0.027(2) -0.0007(17) 0.0009(17) 0.0081(16) C30 0.029(2) 0.022(2) 0.022(2) -0.0013(16) 0.0051(17) 0.0089(16) C31 0.0223(19) 0.0222(19) 0.024(2) -0.0060(16) 0.0081(16) -0.0045(15) C32 0.0227(19) 0.0211(19) 0.025(2) 0.0036(16) 0.0024(16) -0.0039(16) C33 0.0180(18) 0.0193(19) 0.026(2) -0.0017(16) 0.0037(16) 0.0010(15) C34 0.0186(17) 0.0175(18) 0.0153(18) -0.0039(15) 0.0006(14) -0.0035(14) C35 0.0232(19) 0.0198(19) 0.0196(19) 0.0003(16) 0.0017(16) -0.0022(15) C36 0.026(2) 0.025(2) 0.025(2) -0.0049(17) 0.0062(17) 0.0028(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 C10 2.078(4) . ? Ag1 Cl1 2.3771(10) . ? Ag1 Cl1 2.8540(10) 3_655 ? Ag2 C28 2.081(4) . ? Ag2 Cl2 2.3947(9) . ? Ag2 Cl2 2.8879(10) 3_565 ? Cl1 Ag1 2.8540(10) 3_655 ? Cl2 Ag2 2.8879(10) 3_565 ? N1 C10 1.353(4) . ? N1 C11 1.384(4) . ? N1 C6 1.443(4) . ? N2 C10 1.347(4) . ? N2 C12 1.373(5) . ? N2 C13 1.467(5) . ? N3 C14 1.330(5) . ? N3 C18 1.334(5) . ? N4 C28 1.349(5) . ? N4 C29 1.382(4) . ? N4 C24 1.438(4) . ? N5 C28 1.356(4) . ? N5 C30 1.380(5) . ? N5 C31 1.461(4) . ? N6 C32 1.330(5) . ? N6 C36 1.341(5) . ? C1 C2 1.376(5) . ? C1 C6 1.396(5) . ? C1 C7 1.518(5) . ? C2 C3 1.380(5) . ? C3 C4 1.395(5) . ? C3 C8 1.510(5) . ? C4 C5 1.383(5) . ? C5 C6 1.384(5) . ? C5 C9 1.502(5) . ? C11 C12 1.353(5) . ? C13 C16 1.511(5) . ? C14 C15 1.375(5) . ? C15 C16 1.389(5) . ? C16 C17 1.380(5) . ? C17 C18 1.388(5) . ? C19 C20 1.381(5) . ? C19 C24 1.400(5) . ? C19 C25 1.516(5) . ? C20 C21 1.385(6) . ? C21 C22 1.382(5) . ? C21 C26 1.514(5) . ? C22 C23 1.376(5) . ? C23 C24 1.401(5) . ? C23 C27 1.496(5) . ? C29 C30 1.342(5) . ? C31 C34 1.522(5) . ? C32 C33 1.385(5) . ? C33 C34 1.381(5) . ? C34 C35 1.372(5) . ? C35 C36 1.376(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 C10 Ag1 Cl1 157.42(10) . . ? C10 Ag1 Cl1 107.51(10) . 3_655 ? Cl1 Ag1 Cl1 94.90(3) . 3_655 ? C28 Ag2 Cl2 158.17(10) . . ? C28 Ag2 Cl2 104.01(10) . 3_565 ? Cl2 Ag2 Cl2 96.50(3) . 3_565 ? Ag1 Cl1 Ag1 85.10(3) . 3_655 ? Ag2 Cl2 Ag2 83.50(3) . 3_565 ? C10 N1 C11 111.6(3) . . ? C10 N1 C6 123.6(3) . . ? C11 N1 C6 124.6(3) . . ? C10 N2 C12 111.6(3) . . ? C10 N2 C13 123.5(3) . . ? C12 N2 C13 124.8(3) . . ? C14 N3 C18 116.0(3) . . ? C28 N4 C29 111.5(3) . . ? C28 N4 C24 123.5(3) . . ? C29 N4 C24 125.0(3) . . ? C28 N5 C30 111.1(3) . . ? C28 N5 C31 124.9(3) . . ? C30 N5 C31 123.7(3) . . ? C32 N6 C36 116.8(3) . . ? C2 C1 C6 117.6(3) . . ? C2 C1 C7 120.9(3) . . ? C6 C1 C7 121.5(3) . . ? C1 C2 C3 121.9(4) . . ? C2 C3 C4 118.7(3) . . ? C2 C3 C8 120.0(4) . . ? C4 C3 C8 121.3(4) . . ? C5 C4 C3 121.7(3) . . ? C4 C5 C6 117.3(3) . . ? C4 C5 C9 121.0(3) . . ? C6 C5 C9 121.6(3) . . ? C5 C6 C1 122.8(3) . . ? C5 C6 N1 119.3(3) . . ? C1 C6 N1 117.8(3) . . ? N2 C10 N1 104.1(3) . . ? N2 C10 Ag1 132.1(3) . . ? N1 C10 Ag1 123.7(3) . . ? C12 C11 N1 105.7(3) . . ? C11 C12 N2 107.0(3) . . ? N2 C13 C16 112.0(3) . . ? N3 C14 C15 124.4(4) . . ? C14 C15 C16 119.1(4) . . ? C17 C16 C15 117.4(3) . . ? C17 C16 C13 121.3(3) . . ? C15 C16 C13 121.4(3) . . ? C16 C17 C18 119.1(4) . . ? N3 C18 C17 124.0(4) . . ? C20 C19 C24 117.2(3) . . ? C20 C19 C25 121.9(3) . . ? C24 C19 C25 120.9(3) . . ? C19 C20 C21 122.4(3) . . ? C22 C21 C20 118.4(3) . . ? C22 C21 C26 120.5(4) . . ? C20 C21 C26 121.1(4) . . ? C23 C22 C21 122.2(3) . . ? C22 C23 C24 117.7(3) . . ? C22 C23 C27 121.3(3) . . ? C24 C23 C27 121.0(3) . . ? C19 C24 C23 122.0(3) . . ? C19 C24 N4 119.2(3) . . ? C23 C24 N4 118.8(3) . . ? N4 C28 N5 104.1(3) . . ? N4 C28 Ag2 121.1(3) . . ? N5 C28 Ag2 134.7(3) . . ? C30 C29 N4 106.4(3) . . ? C29 C30 N5 106.9(3) . . ? N5 C31 C34 110.9(3) . . ? N6 C32 C33 123.5(3) . . ? C34 C33 C32 118.7(3) . . ? C35 C34 C33 118.5(3) . . ? C35 C34 C31 121.1(3) . . ? C33 C34 C31 120.4(3) . . ? C34 C35 C36 119.0(3) . . ? N6 C36 C35 123.5(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 C10 Ag1 Cl1 Ag1 172.9(3) . . . 3_655 ? Cl1 Ag1 Cl1 Ag1 0.0 3_655 . . 3_655 ? C28 Ag2 Cl2 Ag2 160.0(3) . . . 3_565 ? Cl2 Ag2 Cl2 Ag2 0.0 3_565 . . 3_565 ? C6 C1 C2 C3 0.2(6) . . . . ? C7 C1 C2 C3 -179.6(4) . . . . ? C1 C2 C3 C4 -0.5(6) . . . . ? C1 C2 C3 C8 -178.9(4) . . . . ? C2 C3 C4 C5 0.7(6) . . . . ? C8 C3 C4 C5 179.1(4) . . . . ? C3 C4 C5 C6 -0.5(5) . . . . ? C3 C4 C5 C9 176.5(4) . . . . ? C4 C5 C6 C1 0.3(5) . . . . ? C9 C5 C6 C1 -176.7(4) . . . . ? C4 C5 C6 N1 179.9(3) . . . . ? C9 C5 C6 N1 2.9(5) . . . . ? C2 C1 C6 C5 -0.1(6) . . . . ? C7 C1 C6 C5 179.7(4) . . . . ? C2 C1 C6 N1 -179.7(3) . . . . ? C7 C1 C6 N1 0.1(5) . . . . ? C10 N1 C6 C5 -101.8(4) . . . . ? C11 N1 C6 C5 83.0(4) . . . . ? C10 N1 C6 C1 77.8(4) . . . . ? C11 N1 C6 C1 -97.4(4) . . . . ? C12 N2 C10 N1 0.4(4) . . . . ? C13 N2 C10 N1 176.6(3) . . . . ? C12 N2 C10 Ag1 -175.6(3) . . . . ? C13 N2 C10 Ag1 0.6(5) . . . . ? C11 N1 C10 N2 0.0(4) . . . . ? C6 N1 C10 N2 -175.7(3) . . . . ? C11 N1 C10 Ag1 176.5(2) . . . . ? C6 N1 C10 Ag1 0.7(5) . . . . ? Cl1 Ag1 C10 N2 72.3(5) . . . . ? Cl1 Ag1 C10 N2 -115.1(3) 3_655 . . . ? Cl1 Ag1 C10 N1 -103.0(3) . . . . ? Cl1 Ag1 C10 N1 69.6(3) 3_655 . . . ? C10 N1 C11 C12 -0.5(4) . . . . ? C6 N1 C11 C12 175.2(3) . . . . ? N1 C11 C12 N2 0.7(4) . . . . ? C10 N2 C12 C11 -0.7(4) . . . . ? C13 N2 C12 C11 -176.9(3) . . . . ? C10 N2 C13 C16 -85.1(4) . . . . ? C12 N2 C13 C16 90.6(4) . . . . ? C18 N3 C14 C15 0.1(6) . . . . ? N3 C14 C15 C16 -0.3(6) . . . . ? C14 C15 C16 C17 0.5(6) . . . . ? C14 C15 C16 C13 -179.5(4) . . . . ? N2 C13 C16 C17 -99.0(4) . . . . ? N2 C13 C16 C15 81.0(4) . . . . ? C15 C16 C17 C18 -0.4(5) . . . . ? C13 C16 C17 C18 179.5(3) . . . . ? C14 N3 C18 C17 0.0(6) . . . . ? C16 C17 C18 N3 0.3(6) . . . . ? C24 C19 C20 C21 -0.7(6) . . . . ? C25 C19 C20 C21 179.2(4) . . . . ? C19 C20 C21 C22 0.0(6) . . . . ? C19 C20 C21 C26 -179.2(4) . . . . ? C20 C21 C22 C23 -0.2(6) . . . . ? C26 C21 C22 C23 179.1(3) . . . . ? C21 C22 C23 C24 1.1(6) . . . . ? C21 C22 C23 C27 -177.2(4) . . . . ? C20 C19 C24 C23 1.7(5) . . . . ? C25 C19 C24 C23 -178.2(4) . . . . ? C20 C19 C24 N4 -179.7(3) . . . . ? C25 C19 C24 N4 0.4(5) . . . . ? C22 C23 C24 C19 -1.8(6) . . . . ? C27 C23 C24 C19 176.5(4) . . . . ? C22 C23 C24 N4 179.5(3) . . . . ? C27 C23 C24 N4 -2.2(5) . . . . ? C28 N4 C24 C19 -95.2(4) . . . . ? C29 N4 C24 C19 86.9(4) . . . . ? C28 N4 C24 C23 83.5(4) . . . . ? C29 N4 C24 C23 -94.4(4) . . . . ? C29 N4 C28 N5 0.3(4) . . . . ? C24 N4 C28 N5 -177.8(3) . . . . ? C29 N4 C28 Ag2 177.5(2) . . . . ? C24 N4 C28 Ag2 -0.6(5) . . . . ? C30 N5 C28 N4 -0.6(4) . . . . ? C31 N5 C28 N4 -174.8(3) . . . . ? C30 N5 C28 Ag2 -177.3(3) . . . . ? C31 N5 C28 Ag2 8.6(5) . . . . ? Cl2 Ag2 C28 N4 -61.3(4) . . . . ? Cl2 Ag2 C28 N4 98.2(3) 3_565 . . . ? Cl2 Ag2 C28 N5 114.9(4) . . . . ? Cl2 Ag2 C28 N5 -85.6(3) 3_565 . . . ? C28 N4 C29 C30 0.1(4) . . . . ? C24 N4 C29 C30 178.2(3) . . . . ? N4 C29 C30 N5 -0.5(4) . . . . ? C28 N5 C30 C29 0.7(4) . . . . ? C31 N5 C30 C29 174.9(3) . . . . ? C28 N5 C31 C34 102.3(4) . . . . ? C30 N5 C31 C34 -71.1(4) . . . . ? C36 N6 C32 C33 -0.4(6) . . . . ? N6 C32 C33 C34 -1.1(6) . . . . ? C32 C33 C34 C35 1.8(5) . . . . ? C32 C33 C34 C31 -179.0(3) . . . . ? N5 C31 C34 C35 103.6(4) . . . . ? N5 C31 C34 C33 -75.5(4) . . . . ? C33 C34 C35 C36 -1.1(5) . . . . ? C31 C34 C35 C36 179.7(3) . . . . ? C32 N6 C36 C35 1.2(6) . . . . ? C34 C35 C36 N6 -0.4(6) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 2.128 _refine_diff_density_min -1.336 _refine_diff_density_rms 0.121 # Attachment 'web_deposit_cif_file_1_GlennYap_1301086809.cif' data_i11732 _database_code_depnum_ccdc_archive 'CCDC 818962' #TrackingRef 'web_deposit_cif_file_1_GlennYap_1301086809.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H15 Ag Cl N3' _chemical_formula_weight 344.59 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 '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 9.786(2) _cell_length_b 11.594(2) _cell_length_c 12.312(3) _cell_angle_alpha 90.00 _cell_angle_beta 109.01(3) _cell_angle_gamma 90.00 _cell_volume 1320.7(5) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.733 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 688 _exptl_absorpt_coefficient_mu 1.709 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details 'SADABS (Sheldrick, 2003)' _exptl_special_details ; Data collection is performed with four batch runs at \f = 0.00 \% (600 frames), at \f = 90.00 \% (600 frames), at \f = 180 \% (600 frames) and at \f = 270 \% (600 frames). Frame width = 0.30 \& in \w. Data is merged, corrected for decay, and treated with multi-scan absorption corrections. ; _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 'Bruker AXS APEX diffractometer' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 836.6 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 1 _diffrn_reflns_number 10945 _diffrn_reflns_av_R_equivalents 0.0335 _diffrn_reflns_av_sigmaI/netI 0.0348 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.32 _diffrn_reflns_theta_max 27.10 _reflns_number_total 2920 _reflns_number_gt 2471 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2002)' _computing_cell_refinement 'SAINT (Bruker, 2002)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2001)' _computing_publication_material 'SHELXTL (Sheldrick, 2001)' _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^)+(0.0256P)^2^+0.1421P] 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 2920 _refine_ls_number_parameters 156 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0327 _refine_ls_R_factor_gt 0.0249 _refine_ls_wR_factor_ref 0.0558 _refine_ls_wR_factor_gt 0.0525 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.025 _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 Ag Ag 0.05841(2) 0.852529(15) 0.598401(15) 0.01951(7) Uani 1 1 d . . . Cl Cl 0.14185(6) 0.93142(5) 0.45392(5) 0.02144(14) Uani 1 1 d . . . N1 N -0.0924(2) 0.75517(16) 0.76697(16) 0.0192(4) Uani 1 1 d . . . N2 N 0.1137(2) 0.67768(16) 0.79611(16) 0.0179(4) Uani 1 1 d . . . N3 N 0.2049(3) 0.37152(18) 0.53272(19) 0.0317(6) Uani 1 1 d . . . C1 C -0.2218(3) 0.8279(2) 0.7203(2) 0.0255(6) Uani 1 1 d . . . H1A H -0.2132 0.8690 0.6515 0.031 Uiso 1 1 calc R . . C2 C -0.3572(3) 0.7552(2) 0.6813(2) 0.0287(6) Uani 1 1 d . . . H2A H -0.4410 0.8049 0.6461 0.043 Uiso 1 1 calc R . . H2B H -0.3697 0.7151 0.7475 0.043 Uiso 1 1 calc R . . H2C H -0.3487 0.6984 0.6249 0.043 Uiso 1 1 calc R . . C3 C -0.2279(3) 0.9176(2) 0.8065(3) 0.0396(8) Uani 1 1 d . . . H3A H -0.1362 0.9599 0.8324 0.059 Uiso 1 1 calc R . . H3B H -0.2445 0.8801 0.8725 0.059 Uiso 1 1 calc R . . H3C H -0.3071 0.9715 0.7710 0.059 Uiso 1 1 calc R . . C4 C 0.0213(2) 0.75443(19) 0.72755(19) 0.0170(5) Uani 1 1 d . . . C5 C -0.0705(3) 0.6806(2) 0.8588(2) 0.0221(5) Uani 1 1 d . . . H5A H -0.1349 0.6668 0.9009 0.027 Uiso 1 1 calc R . . C6 C 0.0592(3) 0.6317(2) 0.8769(2) 0.0220(5) Uani 1 1 d . . . H6A H 0.1046 0.5762 0.9340 0.026 Uiso 1 1 calc R . . C7 C 0.2491(3) 0.6425(2) 0.7812(2) 0.0205(5) Uani 1 1 d . . . H7A H 0.3162 0.6159 0.8560 0.025 Uiso 1 1 calc R . . H7B H 0.2936 0.7100 0.7567 0.025 Uiso 1 1 calc R . . C8 C 0.3362(3) 0.5285(2) 0.6449(2) 0.0283(6) Uani 1 1 d . . . H8A H 0.4202 0.5756 0.6649 0.034 Uiso 1 1 calc R . . C9 C 0.3190(3) 0.4404(2) 0.5666(2) 0.0315(6) Uani 1 1 d . . . H9A H 0.3940 0.4282 0.5346 0.038 Uiso 1 1 calc R . . C10 C 0.1036(3) 0.3911(2) 0.5805(2) 0.0324(6) Uani 1 1 d . . . H10A H 0.0201 0.3435 0.5579 0.039 Uiso 1 1 calc R . . C11 C 0.1114(3) 0.4759(2) 0.6606(2) 0.0278(6) Uani 1 1 d . . . H11A H 0.0358 0.4849 0.6925 0.033 Uiso 1 1 calc R . . C12 C 0.2302(3) 0.5474(2) 0.6940(2) 0.0197(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 Ag 0.02129(11) 0.02023(11) 0.01857(11) 0.00003(7) 0.00864(8) -0.00426(8) Cl 0.0236(3) 0.0223(3) 0.0230(3) 0.0009(2) 0.0139(3) 0.0001(3) N1 0.0182(11) 0.0189(10) 0.0223(10) 0.0035(8) 0.0092(9) 0.0028(9) N2 0.0171(11) 0.0178(10) 0.0191(10) -0.0015(8) 0.0061(9) -0.0004(9) N3 0.0358(15) 0.0269(12) 0.0247(12) -0.0022(10) -0.0008(11) 0.0116(11) C1 0.0220(14) 0.0247(13) 0.0326(14) 0.0146(11) 0.0127(12) 0.0068(11) C2 0.0221(14) 0.0359(15) 0.0254(13) 0.0018(12) 0.0041(12) 0.0028(12) C3 0.0233(16) 0.0263(15) 0.069(2) -0.0100(15) 0.0150(15) 0.0010(13) C4 0.0160(12) 0.0162(12) 0.0172(11) -0.0019(10) 0.0034(10) -0.0017(10) C5 0.0264(14) 0.0224(12) 0.0200(12) 0.0049(11) 0.0110(11) -0.0011(11) C6 0.0238(14) 0.0214(13) 0.0196(12) 0.0033(10) 0.0056(11) 0.0000(11) C7 0.0145(13) 0.0204(13) 0.0253(13) -0.0033(10) 0.0047(11) -0.0004(10) C8 0.0253(15) 0.0275(14) 0.0336(15) -0.0004(12) 0.0119(13) -0.0002(12) C9 0.0338(17) 0.0340(15) 0.0279(14) -0.0019(12) 0.0119(13) 0.0078(14) C10 0.0266(15) 0.0238(14) 0.0390(16) -0.0045(13) -0.0002(13) -0.0023(13) C11 0.0250(14) 0.0233(13) 0.0365(15) -0.0068(12) 0.0121(13) -0.0001(12) C12 0.0182(13) 0.0165(12) 0.0219(12) 0.0034(10) 0.0031(11) 0.0036(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 Ag C4 2.081(2) . ? Ag Cl 2.3693(7) . ? N1 C4 1.351(3) . ? N1 C5 1.384(3) . ? N1 C1 1.474(3) . ? N2 C4 1.351(3) . ? N2 C6 1.380(3) . ? N2 C7 1.454(3) . ? N3 C10 1.326(4) . ? N3 C9 1.325(3) . ? C1 C3 1.501(4) . ? C1 C2 1.511(4) . ? C5 C6 1.342(3) . ? C7 C12 1.507(3) . ? C8 C9 1.376(4) . ? C8 C12 1.379(3) . ? C10 C11 1.377(4) . ? C11 C12 1.377(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C4 Ag Cl 166.72(6) . . ? C4 N1 C5 111.3(2) . . ? C4 N1 C1 124.59(19) . . ? C5 N1 C1 124.0(2) . . ? C4 N2 C6 111.6(2) . . ? C4 N2 C7 123.94(19) . . ? C6 N2 C7 124.4(2) . . ? C10 N3 C9 115.6(2) . . ? N1 C1 C3 110.4(2) . . ? N1 C1 C2 111.0(2) . . ? C3 C1 C2 112.3(2) . . ? N2 C4 N1 103.99(19) . . ? N2 C4 Ag 126.13(17) . . ? N1 C4 Ag 129.80(17) . . ? C6 C5 N1 106.6(2) . . ? C5 C6 N2 106.5(2) . . ? N2 C7 C12 112.9(2) . . ? C9 C8 C12 119.2(3) . . ? N3 C9 C8 124.5(3) . . ? N3 C10 C11 124.4(3) . . ? C10 C11 C12 119.3(2) . . ? C8 C12 C11 117.1(2) . . ? C8 C12 C7 119.6(2) . . ? C11 C12 C7 123.3(2) . . ? 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 C4 N1 C1 C3 -111.9(3) . . . . ? C5 N1 C1 C3 66.5(3) . . . . ? C4 N1 C1 C2 122.9(2) . . . . ? C5 N1 C1 C2 -58.6(3) . . . . ? C6 N2 C4 N1 -0.2(3) . . . . ? C7 N2 C4 N1 175.9(2) . . . . ? C6 N2 C4 Ag 176.83(16) . . . . ? C7 N2 C4 Ag -7.1(3) . . . . ? C5 N1 C4 N2 0.3(3) . . . . ? C1 N1 C4 N2 178.9(2) . . . . ? C5 N1 C4 Ag -176.51(17) . . . . ? C1 N1 C4 Ag 2.1(3) . . . . ? Cl Ag C4 N2 19.5(4) . . . . ? Cl Ag C4 N1 -164.24(17) . . . . ? C4 N1 C5 C6 -0.4(3) . . . . ? C1 N1 C5 C6 -179.0(2) . . . . ? N1 C5 C6 N2 0.2(3) . . . . ? C4 N2 C6 C5 -0.1(3) . . . . ? C7 N2 C6 C5 -176.1(2) . . . . ? C4 N2 C7 C12 -83.8(3) . . . . ? C6 N2 C7 C12 91.8(3) . . . . ? C10 N3 C9 C8 -0.6(4) . . . . ? C12 C8 C9 N3 0.8(4) . . . . ? C9 N3 C10 C11 -0.3(4) . . . . ? N3 C10 C11 C12 0.9(4) . . . . ? C9 C8 C12 C11 -0.2(4) . . . . ? C9 C8 C12 C7 179.1(2) . . . . ? C10 C11 C12 C8 -0.6(4) . . . . ? C10 C11 C12 C7 -179.9(2) . . . . ? N2 C7 C12 C8 160.5(2) . . . . ? N2 C7 C12 C11 -20.3(3) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.458 _refine_diff_density_min -0.414 _refine_diff_density_rms 0.088 # Attachment '4822_web_deposit_cif_file_2_GlennYap_1301086809.cif' data_i12139 _database_code_depnum_ccdc_archive 'CCDC 818963' #TrackingRef '4822_web_deposit_cif_file_2_GlennYap_1301086809.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H38 Cl2 N6 Pd' _chemical_formula_weight 732.02 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbcn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' '-x, y, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' 'x, -y, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 15.7750(9) _cell_length_b 12.1317(8) _cell_length_c 17.5570(12) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3360.0(4) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 6525 _cell_measurement_theta_min 2.12 _cell_measurement_theta_max 27.01 _exptl_crystal_description PRISM _exptl_crystal_colour yellow _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.447 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1504 _exptl_absorpt_coefficient_mu 0.747 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details 'SADABS (Sheldrick, 2003)' _exptl_special_details ; Data collection is performed with four batch runs at \f = 0.00 \% (600 frames), at \f = 90.00 \% (600 frames), at \f = 180 \% (600 frames) and at \f = 270 \% (600 frames). Frame width = 0.30 \& in \w. Data is merged, corrected for decay, and treated with multi-scan absorption corrections. ; _diffrn_ambient_temperature 296(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 'Bruker AXS APEX diffractometer' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 836.6 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 1 _diffrn_reflns_number 27361 _diffrn_reflns_av_R_equivalents 0.0661 _diffrn_reflns_av_sigmaI/netI 0.0484 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.12 _diffrn_reflns_theta_max 27.03 _reflns_number_total 3688 _reflns_number_gt 2642 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2002)' _computing_cell_refinement 'SAINT (Bruker, 2002)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2001)' _computing_publication_material 'SHELXTL (Sheldrick, 2001)' _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^)+(0.0256P)^2^] 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 3688 _refine_ls_number_parameters 207 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0478 _refine_ls_R_factor_gt 0.0292 _refine_ls_wR_factor_ref 0.0670 _refine_ls_wR_factor_gt 0.0623 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.051 _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 Pd Pd 0.0000 0.58909(2) 0.2500 0.01582(8) Uani 1 2 d S . . Cl Cl 0.06048(4) 0.45308(5) 0.17042(4) 0.02693(15) Uani 1 1 d . . . N1 N -0.00329(11) 0.77643(15) 0.13590(10) 0.0170(4) Uani 1 1 d . . . N2 N 0.12397(11) 0.72810(16) 0.16486(10) 0.0183(4) Uani 1 1 d . . . N3 N 0.40554(13) 0.60918(18) 0.04989(13) 0.0315(6) Uani 1 1 d . . . C1 C -0.13403(14) 0.6947(2) 0.08605(13) 0.0209(5) Uani 1 1 d . . . C2 C -0.22212(14) 0.6985(2) 0.07885(14) 0.0264(6) Uani 1 1 d . . . H2A H -0.2494 0.6421 0.0527 0.032 Uiso 1 1 calc R . . C3 C -0.27062(14) 0.7837(2) 0.10952(14) 0.0267(6) Uani 1 1 d . . . C4 C -0.22914(15) 0.8682(2) 0.14833(14) 0.0270(6) Uani 1 1 d . . . H4A H -0.2608 0.9260 0.1683 0.032 Uiso 1 1 calc R . . C5 C -0.14067(14) 0.8680(2) 0.15802(13) 0.0209(5) Uani 1 1 d . . . C6 C -0.09518(13) 0.7789(2) 0.12781(13) 0.0180(5) Uani 1 1 d . . . C7 C -0.08399(15) 0.6055(2) 0.04625(14) 0.0284(6) Uani 1 1 d . . . H7A H -0.0568 0.5597 0.0835 0.043 Uiso 1 1 calc R . . H7B H -0.0418 0.6387 0.0142 0.043 Uiso 1 1 calc R . . H7C H -0.1215 0.5616 0.0158 0.043 Uiso 1 1 calc R . . C8 C -0.36596(14) 0.7846(2) 0.09914(16) 0.0395(7) Uani 1 1 d . . . H8A H -0.3869 0.7103 0.0999 0.059 Uiso 1 1 calc R . . H8B H -0.3798 0.8181 0.0512 0.059 Uiso 1 1 calc R . . H8C H -0.3916 0.8258 0.1397 0.059 Uiso 1 1 calc R . . C9 C -0.09911(15) 0.9614(2) 0.20075(15) 0.0297(6) Uani 1 1 d . . . H9A H -0.0507 0.9869 0.1727 0.045 Uiso 1 1 calc R . . H9B H -0.0814 0.9360 0.2500 0.045 Uiso 1 1 calc R . . H9C H -0.1388 1.0207 0.2067 0.045 Uiso 1 1 calc R . . C10 C 0.04196(13) 0.70526(19) 0.18037(12) 0.0160(5) Uani 1 1 d . . . C11 C 0.05103(14) 0.8424(2) 0.09310(14) 0.0232(6) Uani 1 1 d . . . H11A H 0.0355 0.8965 0.0582 0.028 Uiso 1 1 calc R . . C12 C 0.13038(14) 0.8126(2) 0.11213(13) 0.0229(6) Uani 1 1 d . . . H12A H 0.1803 0.8430 0.0933 0.028 Uiso 1 1 calc R . . C13 C 0.19593(13) 0.6732(2) 0.20257(13) 0.0214(6) Uani 1 1 d . . . H13A H 0.1769 0.6040 0.2242 0.026 Uiso 1 1 calc R . . H13B H 0.2161 0.7193 0.2439 0.026 Uiso 1 1 calc R . . C14 C 0.32888(16) 0.5666(2) 0.03789(15) 0.0300(6) Uani 1 1 d . . . H14A H 0.3215 0.5220 -0.0047 0.036 Uiso 1 1 calc R . . C15 C 0.25888(14) 0.5841(2) 0.08478(14) 0.0259(6) Uani 1 1 d . . . H15A H 0.2070 0.5515 0.0738 0.031 Uiso 1 1 calc R . . C16 C 0.26821(14) 0.65118(19) 0.14794(13) 0.0196(5) Uani 1 1 d . . . C17 C 0.34696(14) 0.6980(2) 0.16052(15) 0.0278(6) Uani 1 1 d . . . H17A H 0.3559 0.7443 0.2020 0.033 Uiso 1 1 calc R . . C18 C 0.41253(15) 0.6744(2) 0.10991(17) 0.0340(7) Uani 1 1 d . . . H18A H 0.4650 0.7069 0.1190 0.041 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 Pd 0.01657(12) 0.01553(13) 0.01535(13) 0.000 0.00145(11) 0.000 Cl 0.0311(3) 0.0219(3) 0.0277(3) -0.0055(3) 0.0042(3) 0.0049(3) N1 0.0146(9) 0.0191(10) 0.0174(10) 0.0020(8) 0.0003(9) 0.0016(9) N2 0.0141(9) 0.0234(11) 0.0174(11) 0.0029(9) 0.0003(8) 0.0016(9) N3 0.0265(12) 0.0257(14) 0.0422(15) 0.0107(11) 0.0138(10) 0.0059(10) C1 0.0195(12) 0.0248(14) 0.0184(13) 0.0041(11) -0.0011(10) 0.0022(11) C2 0.0237(13) 0.0291(15) 0.0264(15) 0.0015(12) -0.0065(11) -0.0058(12) C3 0.0159(12) 0.0369(17) 0.0273(15) 0.0062(12) -0.0025(10) 0.0019(12) C4 0.0205(13) 0.0301(15) 0.0305(15) 0.0031(12) -0.0001(11) 0.0059(12) C5 0.0193(12) 0.0232(13) 0.0203(13) 0.0013(11) -0.0009(10) 0.0013(11) C6 0.0144(11) 0.0236(14) 0.0160(12) 0.0044(10) 0.0005(9) -0.0002(10) C7 0.0304(14) 0.0296(16) 0.0254(14) -0.0075(12) -0.0066(11) 0.0033(12) C8 0.0184(13) 0.049(2) 0.051(2) 0.0026(16) -0.0065(13) -0.0011(13) C9 0.0277(13) 0.0251(15) 0.0364(17) -0.0048(12) -0.0022(12) 0.0063(12) C10 0.0150(11) 0.0183(13) 0.0147(12) -0.0017(10) 0.0016(9) 0.0028(10) C11 0.0227(13) 0.0235(14) 0.0233(14) 0.0092(11) 0.0008(11) -0.0003(11) C12 0.0178(12) 0.0266(15) 0.0244(14) 0.0084(11) 0.0047(10) -0.0017(11) C13 0.0171(12) 0.0267(14) 0.0202(13) 0.0044(11) 0.0008(10) 0.0045(11) C14 0.0395(15) 0.0257(15) 0.0248(15) 0.0006(12) 0.0065(12) 0.0057(13) C15 0.0190(12) 0.0296(15) 0.0290(14) 0.0020(12) -0.0006(11) -0.0013(11) C16 0.0162(12) 0.0197(14) 0.0228(13) 0.0080(11) 0.0002(10) 0.0029(10) C17 0.0220(13) 0.0250(15) 0.0364(16) -0.0010(12) 0.0019(12) -0.0029(11) C18 0.0159(13) 0.0294(16) 0.057(2) 0.0061(15) 0.0070(12) -0.0029(12) _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 Pd C10 1.980(2) . ? Pd C10 1.980(2) 3 ? Pd Cl 2.3633(6) 3 ? Pd Cl 2.3633(6) . ? N1 C10 1.365(3) . ? N1 C11 1.393(3) . ? N1 C6 1.457(3) . ? N2 C10 1.351(3) . ? N2 C12 1.385(3) . ? N2 C13 1.473(3) . ? N3 C18 1.322(3) . ? N3 C14 1.332(3) . ? C1 C2 1.396(3) . ? C1 C6 1.399(3) . ? C1 C7 1.511(3) . ? C2 C3 1.395(3) . ? C3 C4 1.394(3) . ? C3 C8 1.515(3) . ? C4 C5 1.406(3) . ? C5 C6 1.401(3) . ? C5 C9 1.509(3) . ? C11 C12 1.345(3) . ? C13 C16 1.514(3) . ? C14 C15 1.394(3) . ? C15 C16 1.383(3) . ? C16 C17 1.384(3) . ? C17 C18 1.393(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C10 Pd C10 89.22(13) . 3 ? C10 Pd Cl 175.68(6) . 3 ? C10 Pd Cl 89.83(6) 3 3 ? C10 Pd Cl 89.83(6) . . ? C10 Pd Cl 175.68(6) 3 . ? Cl Pd Cl 91.43(3) 3 . ? C10 N1 C11 110.51(17) . . ? C10 N1 C6 126.10(18) . . ? C11 N1 C6 123.20(18) . . ? C10 N2 C12 110.89(19) . . ? C10 N2 C13 123.70(19) . . ? C12 N2 C13 125.35(19) . . ? C18 N3 C14 115.7(2) . . ? C2 C1 C6 117.4(2) . . ? C2 C1 C7 120.1(2) . . ? C6 C1 C7 122.5(2) . . ? C3 C2 C1 122.4(2) . . ? C4 C3 C2 118.4(2) . . ? C4 C3 C8 121.3(2) . . ? C2 C3 C8 120.2(2) . . ? C3 C4 C5 121.6(2) . . ? C6 C5 C4 117.6(2) . . ? C6 C5 C9 122.99(19) . . ? C4 C5 C9 119.4(2) . . ? C1 C6 C5 122.5(2) . . ? C1 C6 N1 118.1(2) . . ? C5 C6 N1 119.3(2) . . ? N2 C10 N1 104.81(19) . . ? N2 C10 Pd 126.21(16) . . ? N1 C10 Pd 128.94(15) . . ? C12 C11 N1 106.5(2) . . ? C11 C12 N2 107.3(2) . . ? N2 C13 C16 112.06(18) . . ? N3 C14 C15 124.5(3) . . ? C16 C15 C14 118.6(2) . . ? C15 C16 C17 117.7(2) . . ? C15 C16 C13 122.1(2) . . ? C17 C16 C13 120.2(2) . . ? C16 C17 C18 118.7(2) . . ? N3 C18 C17 124.7(2) . . ? 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 C6 C1 C2 C3 2.0(4) . . . . ? C7 C1 C2 C3 -175.0(2) . . . . ? C1 C2 C3 C4 0.3(4) . . . . ? C1 C2 C3 C8 179.2(2) . . . . ? C2 C3 C4 C5 -1.0(4) . . . . ? C8 C3 C4 C5 -179.9(2) . . . . ? C3 C4 C5 C6 -0.6(4) . . . . ? C3 C4 C5 C9 -179.8(2) . . . . ? C2 C1 C6 C5 -3.7(3) . . . . ? C7 C1 C6 C5 173.1(2) . . . . ? C2 C1 C6 N1 -180.0(2) . . . . ? C7 C1 C6 N1 -3.1(3) . . . . ? C4 C5 C6 C1 3.1(3) . . . . ? C9 C5 C6 C1 -177.8(2) . . . . ? C4 C5 C6 N1 179.3(2) . . . . ? C9 C5 C6 N1 -1.5(3) . . . . ? C10 N1 C6 C1 -72.8(3) . . . . ? C11 N1 C6 C1 101.6(3) . . . . ? C10 N1 C6 C5 110.8(3) . . . . ? C11 N1 C6 C5 -74.8(3) . . . . ? C12 N2 C10 N1 0.5(2) . . . . ? C13 N2 C10 N1 177.63(19) . . . . ? C12 N2 C10 Pd 178.41(16) . . . . ? C13 N2 C10 Pd -4.4(3) . . . . ? C11 N1 C10 N2 0.2(2) . . . . ? C6 N1 C10 N2 175.2(2) . . . . ? C11 N1 C10 Pd -177.67(17) . . . . ? C6 N1 C10 Pd -2.7(3) . . . . ? C10 Pd C10 N2 112.4(2) 3 . . . ? Cl Pd C10 N2 -170.4(7) 3 . . . ? Cl Pd C10 N2 -63.44(19) . . . . ? C10 Pd C10 N1 -70.21(18) 3 . . . ? Cl Pd C10 N1 7.0(10) 3 . . . ? Cl Pd C10 N1 114.00(19) . . . . ? C10 N1 C11 C12 -0.8(3) . . . . ? C6 N1 C11 C12 -175.9(2) . . . . ? N1 C11 C12 N2 1.0(3) . . . . ? C10 N2 C12 C11 -1.0(3) . . . . ? C13 N2 C12 C11 -178.1(2) . . . . ? C10 N2 C13 C16 141.6(2) . . . . ? C12 N2 C13 C16 -41.6(3) . . . . ? C18 N3 C14 C15 -1.8(4) . . . . ? N3 C14 C15 C16 0.7(4) . . . . ? C14 C15 C16 C17 0.6(3) . . . . ? C14 C15 C16 C13 -179.0(2) . . . . ? N2 C13 C16 C15 -61.3(3) . . . . ? N2 C13 C16 C17 119.1(2) . . . . ? C15 C16 C17 C18 -0.7(4) . . . . ? C13 C16 C17 C18 178.9(2) . . . . ? C14 N3 C18 C17 1.6(4) . . . . ? C16 C17 C18 N3 -0.4(4) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.505 _refine_diff_density_min -0.575 _refine_diff_density_rms 0.083 # Attachment '4823_web_deposit_cif_file_3_GlennYap_1301086809.cif' data_i11686 _database_code_depnum_ccdc_archive 'CCDC 818964' #TrackingRef '4823_web_deposit_cif_file_3_GlennYap_1301086809.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H42 Cl2 N6 O3 Pd' _chemical_formula_weight 808.08 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 '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' _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 12.7736(4) _cell_length_b 19.7296(7) _cell_length_c 14.8140(5) _cell_angle_alpha 90.00 _cell_angle_beta 102.0670(10) _cell_angle_gamma 90.00 _cell_volume 3650.9(2) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9917 _cell_measurement_theta_min 2.37 _cell_measurement_theta_max 27.05 _exptl_crystal_description PRISM _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.470 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1664 _exptl_absorpt_coefficient_mu 0.701 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details 'SADABS (Sheldrick, 2003)' _exptl_special_details ; Data collection is performed with four batch runs at \f = 0.00 \% (600 frames), at \f = 90.00 \% (600 frames), at \f = 180 \% (600 frames) and at \f = 270 \% (600 frames). Frame width = 0.30 \& in \w. Data is merged, corrected for decay, and treated with multi-scan absorption corrections. ; _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 'Bruker AXS APEX diffractometer' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 836.6 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 1 _diffrn_reflns_number 30770 _diffrn_reflns_av_R_equivalents 0.0353 _diffrn_reflns_av_sigmaI/netI 0.0377 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.92 _diffrn_reflns_theta_max 27.09 _reflns_number_total 8034 _reflns_number_gt 6711 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2002)' _computing_cell_refinement 'SAINT (Bruker, 2002)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2001)' _computing_publication_material 'SHELXTL (Sheldrick, 2001)' _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^)+(0.0457P)^2^+3.1731P] 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 8034 _refine_ls_number_parameters 457 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0430 _refine_ls_R_factor_gt 0.0333 _refine_ls_wR_factor_ref 0.0910 _refine_ls_wR_factor_gt 0.0851 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.024 _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 Pd Pd 0.756243(14) 0.208671(9) 0.673798(12) 0.01331(7) Uani 1 1 d . . . N1 N 0.60030(16) 0.09557(10) 0.60655(13) 0.0169(4) Uani 1 1 d . . . N2 N 0.61634(16) 0.11354(10) 0.75128(13) 0.0165(4) Uani 1 1 d . . . N3 N 0.85300(18) 0.00530(11) 1.03059(15) 0.0231(5) Uani 1 1 d . . . H3A H 0.8939 -0.0227 1.0687 0.028 Uiso 1 1 calc R . . N4 N 0.56745(16) 0.30446(10) 0.63595(14) 0.0160(4) Uani 1 1 d . . . N5 N 0.63696(16) 0.29264(10) 0.51717(14) 0.0151(4) Uani 1 1 d . . . N6 N 0.91291(17) 0.43950(12) 0.40560(15) 0.0241(5) Uani 1 1 d . . . H6A H 0.9565 0.4714 0.3941 0.029 Uiso 1 1 calc R . . O1 O 0.89549(13) 0.26313(9) 0.68825(11) 0.0182(4) Uani 1 1 d . . . O2 O 0.88984(13) 0.15966(9) 0.74298(12) 0.0196(4) Uani 1 1 d . . . O3 O 1.04920(14) 0.21226(9) 0.75943(13) 0.0239(4) Uani 1 1 d . . . C1 C 0.5314(2) 0.13216(12) 0.44742(16) 0.0177(5) Uani 1 1 d . . . C2 C 0.5447(2) 0.13686(12) 0.35681(17) 0.0206(5) Uani 1 1 d . . . H2A H 0.4894 0.1565 0.3114 0.025 Uiso 1 1 calc R . . C3 C 0.6370(2) 0.11357(13) 0.33107(18) 0.0242(6) Uani 1 1 d . . . C4 C 0.7164(2) 0.08380(14) 0.39741(18) 0.0251(6) Uani 1 1 d . . . H4A H 0.7797 0.0681 0.3801 0.030 Uiso 1 1 calc R . . C5 C 0.7062(2) 0.07612(13) 0.48889(17) 0.0216(5) Uani 1 1 d . . . C6 C 0.6132(2) 0.10137(12) 0.51164(16) 0.0181(5) Uani 1 1 d . . . C7 C 0.4347(2) 0.16184(14) 0.47523(18) 0.0248(6) Uani 1 1 d . . . H7A H 0.4575 0.1941 0.5259 0.037 Uiso 1 1 calc R . . H7B H 0.3928 0.1255 0.4956 0.037 Uiso 1 1 calc R . . H7C H 0.3907 0.1853 0.4224 0.037 Uiso 1 1 calc R . . C8 C 0.6493(3) 0.12106(16) 0.23206(19) 0.0344(7) Uani 1 1 d . . . H8A H 0.7249 0.1280 0.2309 0.052 Uiso 1 1 calc R . . H8B H 0.6075 0.1601 0.2038 0.052 Uiso 1 1 calc R . . H8C H 0.6234 0.0799 0.1975 0.052 Uiso 1 1 calc R . . C9 C 0.7938(2) 0.04289(15) 0.55954(19) 0.0291(6) Uani 1 1 d . . . H9A H 0.7631 0.0063 0.5906 0.044 Uiso 1 1 calc R . . H9B H 0.8269 0.0766 0.6052 0.044 Uiso 1 1 calc R . . H9C H 0.8481 0.0242 0.5286 0.044 Uiso 1 1 calc R . . C10 C 0.64812(19) 0.13758(12) 0.67592(16) 0.0158(5) Uani 1 1 d . . . C11 C 0.5413(2) 0.04558(13) 0.63937(17) 0.0218(5) Uani 1 1 d . . . H11A H 0.5011 0.0104 0.6044 0.026 Uiso 1 1 calc R . . C12 C 0.5522(2) 0.05694(13) 0.73046(17) 0.0197(5) Uani 1 1 d . . . H12A H 0.5216 0.0310 0.7724 0.024 Uiso 1 1 calc R . . C13 C 0.6502(2) 0.14128(13) 0.84425(16) 0.0197(5) Uani 1 1 d . . . H13A H 0.5860 0.1516 0.8695 0.024 Uiso 1 1 calc R . . H13B H 0.6891 0.1843 0.8410 0.024 Uiso 1 1 calc R . . C14 C 0.8001(2) 0.05464(13) 0.88069(17) 0.0222(5) Uani 1 1 d . . . H14A H 0.8104 0.0576 0.8191 0.027 Uiso 1 1 calc R . . C15 C 0.8626(2) 0.01227(13) 0.94324(18) 0.0244(6) Uani 1 1 d . . . H15A H 0.9161 -0.0136 0.9230 0.029 Uiso 1 1 calc R . . C16 C 0.7785(2) 0.04276(14) 1.05743(18) 0.0233(6) Uani 1 1 d . . . H16A H 0.7708 0.0390 1.1196 0.028 Uiso 1 1 calc R . . C17 C 0.7118(2) 0.08682(13) 1.00005(17) 0.0201(5) Uani 1 1 d . . . H17A H 0.6598 0.1125 1.0227 0.024 Uiso 1 1 calc R . . C18 C 0.7215(2) 0.09315(12) 0.90874(16) 0.0175(5) Uani 1 1 d . . . C19 C 0.4649(2) 0.27451(13) 0.75326(18) 0.0212(5) Uani 1 1 d . . . C20 C 0.4574(2) 0.27504(14) 0.84523(19) 0.0282(6) Uani 1 1 d . . . H20A H 0.3951 0.2568 0.8616 0.034 Uiso 1 1 calc R . . C21 C 0.5373(3) 0.30111(14) 0.91401(19) 0.0282(6) Uani 1 1 d . . . C22 C 0.6258(2) 0.33111(14) 0.88910(18) 0.0243(6) Uani 1 1 d . . . H22A H 0.6805 0.3499 0.9358 0.029 Uiso 1 1 calc R . . C23 C 0.6360(2) 0.33425(13) 0.79712(17) 0.0203(5) Uani 1 1 d . . . C24 C 0.5560(2) 0.30342(12) 0.73083(17) 0.0179(5) Uani 1 1 d . . . C25 C 0.3765(2) 0.24271(15) 0.68205(18) 0.0272(6) Uani 1 1 d . . . H25A H 0.3661 0.2688 0.6246 0.041 Uiso 1 1 calc R . . H25B H 0.3099 0.2427 0.7051 0.041 Uiso 1 1 calc R . . H25C H 0.3961 0.1960 0.6703 0.041 Uiso 1 1 calc R . . C26 C 0.5276(3) 0.29718(18) 1.0140(2) 0.0473(9) Uani 1 1 d . . . H26A H 0.5018 0.2521 1.0266 0.071 Uiso 1 1 calc R . . H26B H 0.4768 0.3316 1.0259 0.071 Uiso 1 1 calc R . . H26C H 0.5978 0.3053 1.0541 0.071 Uiso 1 1 calc R . . C27 C 0.7267(2) 0.37291(13) 0.76992(18) 0.0227(6) Uani 1 1 d . . . H27A H 0.7600 0.4028 0.8207 0.034 Uiso 1 1 calc R . . H27B H 0.6988 0.4001 0.7148 0.034 Uiso 1 1 calc R . . H27C H 0.7801 0.3409 0.7566 0.034 Uiso 1 1 calc R . . C28 C 0.64707(19) 0.27146(12) 0.60508(16) 0.0153(5) Uani 1 1 d . . . C29 C 0.50935(19) 0.34510(13) 0.56646(17) 0.0193(5) Uani 1 1 d . . . H29A H 0.4502 0.3732 0.5710 0.023 Uiso 1 1 calc R . . C30 C 0.5520(2) 0.33739(13) 0.49247(18) 0.0195(5) Uani 1 1 d . . . H30A H 0.5287 0.3585 0.4340 0.023 Uiso 1 1 calc R . . C31 C 0.7108(2) 0.27481(12) 0.45711(16) 0.0170(5) Uani 1 1 d . . . H31A H 0.6692 0.2587 0.3969 0.020 Uiso 1 1 calc R . . H31B H 0.7579 0.2374 0.4856 0.020 Uiso 1 1 calc R . . C32 C 0.8526(2) 0.36543(13) 0.51268(17) 0.0204(5) Uani 1 1 d . . . H32A H 0.8590 0.3509 0.5747 0.025 Uiso 1 1 calc R . . C33 C 0.9162(2) 0.41735(13) 0.49123(18) 0.0222(5) Uani 1 1 d . . . H33A H 0.9650 0.4384 0.5404 0.027 Uiso 1 1 calc R . . C34 C 0.8407(2) 0.41119(14) 0.33837(18) 0.0238(6) Uani 1 1 d . . . H34A H 0.8357 0.4272 0.2771 0.029 Uiso 1 1 calc R . . C35 C 0.7720(2) 0.35922(13) 0.35304(17) 0.0185(5) Uani 1 1 d . . . H35A H 0.7211 0.3409 0.3029 0.022 Uiso 1 1 calc R . . C36 C 0.77903(19) 0.33487(12) 0.44151(16) 0.0167(5) Uani 1 1 d . . . C37 C 0.9515(2) 0.21190(12) 0.73215(16) 0.0178(5) Uani 1 1 d . . . C38 C 0.0613(2) 0.04576(14) 0.7419(2) 0.0292(6) Uani 1 1 d . . . H38A H 0.1127 0.0513 0.8015 0.035 Uiso 1 1 calc R . . H38B H 0.0029 0.0791 0.7396 0.035 Uiso 1 1 calc R . . Cl1 Cl 0.12714(7) 0.06112(4) 0.64979(5) 0.0415(2) Uani 1 1 d . . . Cl2 Cl 0.00822(7) -0.03695(4) 0.73404(6) 0.04070(19) 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 Pd 0.01449(10) 0.01267(10) 0.01232(10) 0.00042(7) 0.00177(7) 0.00116(7) N1 0.0206(11) 0.0153(10) 0.0143(10) -0.0007(8) 0.0025(8) -0.0034(8) N2 0.0203(11) 0.0152(10) 0.0140(10) 0.0017(8) 0.0036(8) 0.0014(8) N3 0.0253(12) 0.0201(11) 0.0214(11) 0.0041(9) -0.0007(9) 0.0018(9) N4 0.0162(10) 0.0161(10) 0.0161(10) 0.0022(8) 0.0047(8) 0.0025(8) N5 0.0158(10) 0.0149(10) 0.0145(10) 0.0023(8) 0.0025(8) 0.0002(8) N6 0.0178(11) 0.0254(12) 0.0309(13) 0.0006(10) 0.0091(9) -0.0049(9) O1 0.0166(9) 0.0172(9) 0.0195(9) 0.0005(7) 0.0008(7) 0.0008(7) O2 0.0192(9) 0.0182(9) 0.0197(9) 0.0031(7) 0.0001(7) 0.0031(7) O3 0.0156(9) 0.0259(10) 0.0270(10) -0.0013(8) -0.0027(7) 0.0044(7) C1 0.0220(13) 0.0121(12) 0.0181(12) -0.0031(9) 0.0021(10) -0.0032(10) C2 0.0263(14) 0.0158(12) 0.0173(12) -0.0013(10) -0.0010(10) 0.0007(10) C3 0.0361(16) 0.0178(13) 0.0202(13) -0.0035(10) 0.0093(11) -0.0021(11) C4 0.0291(15) 0.0254(14) 0.0223(13) -0.0015(11) 0.0089(11) 0.0063(12) C5 0.0268(14) 0.0178(13) 0.0194(13) -0.0010(10) 0.0032(11) 0.0041(11) C6 0.0248(13) 0.0152(12) 0.0134(12) -0.0029(10) 0.0021(10) -0.0035(10) C7 0.0227(14) 0.0283(15) 0.0221(13) -0.0026(11) 0.0015(11) 0.0029(11) C8 0.0516(19) 0.0360(17) 0.0183(14) 0.0014(12) 0.0134(13) 0.0079(15) C9 0.0342(16) 0.0284(15) 0.0245(14) -0.0001(12) 0.0059(12) 0.0113(13) C10 0.0182(12) 0.0147(12) 0.0137(11) 0.0017(9) 0.0012(9) 0.0053(10) C11 0.0247(14) 0.0191(13) 0.0215(13) -0.0019(10) 0.0044(10) -0.0047(11) C12 0.0194(13) 0.0180(13) 0.0219(13) 0.0018(10) 0.0045(10) -0.0013(10) C13 0.0251(14) 0.0183(13) 0.0160(12) -0.0012(10) 0.0054(10) 0.0021(10) C14 0.0275(14) 0.0234(14) 0.0158(12) -0.0013(10) 0.0048(10) 0.0025(11) C15 0.0309(15) 0.0201(14) 0.0207(13) -0.0027(11) 0.0021(11) 0.0046(11) C16 0.0245(14) 0.0276(14) 0.0176(12) 0.0038(11) 0.0040(10) -0.0060(11) C17 0.0182(13) 0.0236(14) 0.0192(12) 0.0008(10) 0.0053(10) -0.0011(10) C18 0.0205(13) 0.0155(12) 0.0151(12) 0.0002(10) 0.0006(9) -0.0017(10) C19 0.0268(14) 0.0145(12) 0.0255(14) -0.0028(10) 0.0125(11) -0.0010(10) C20 0.0358(16) 0.0250(14) 0.0298(15) -0.0032(12) 0.0209(13) -0.0073(12) C21 0.0452(18) 0.0226(14) 0.0211(14) -0.0040(11) 0.0166(13) -0.0034(12) C22 0.0291(14) 0.0242(14) 0.0200(13) -0.0034(11) 0.0061(11) -0.0014(12) C23 0.0235(13) 0.0159(12) 0.0225(13) 0.0011(10) 0.0071(10) 0.0027(10) C24 0.0238(13) 0.0126(12) 0.0191(12) 0.0004(9) 0.0086(10) 0.0055(10) C25 0.0296(15) 0.0299(15) 0.0256(14) -0.0008(12) 0.0135(12) -0.0067(12) C26 0.068(2) 0.054(2) 0.0267(17) -0.0114(15) 0.0233(17) -0.0241(18) C27 0.0216(13) 0.0222(13) 0.0244(14) -0.0018(11) 0.0053(11) -0.0031(11) C28 0.0159(12) 0.0147(11) 0.0153(12) -0.0010(9) 0.0035(9) -0.0019(9) C29 0.0151(12) 0.0168(12) 0.0255(13) 0.0053(10) 0.0033(10) 0.0031(10) C30 0.0173(12) 0.0185(13) 0.0221(13) 0.0057(10) 0.0026(10) 0.0014(10) C31 0.0189(12) 0.0178(12) 0.0150(12) -0.0005(10) 0.0051(10) 0.0017(10) C32 0.0201(13) 0.0228(13) 0.0183(12) 0.0007(10) 0.0039(10) 0.0030(10) C33 0.0162(13) 0.0253(14) 0.0239(13) -0.0012(11) 0.0010(10) -0.0002(11) C34 0.0231(14) 0.0283(15) 0.0216(13) 0.0021(11) 0.0081(11) -0.0009(11) C35 0.0196(13) 0.0194(13) 0.0165(12) -0.0018(10) 0.0034(10) 0.0001(10) C36 0.0161(12) 0.0171(12) 0.0186(12) -0.0016(10) 0.0073(10) 0.0037(10) C37 0.0221(13) 0.0176(13) 0.0126(11) -0.0021(9) 0.0015(10) 0.0032(10) C38 0.0330(16) 0.0202(14) 0.0323(15) -0.0033(12) 0.0022(12) 0.0023(12) Cl1 0.0608(5) 0.0319(4) 0.0335(4) -0.0006(3) 0.0136(4) 0.0019(4) Cl2 0.0456(5) 0.0266(4) 0.0442(5) -0.0011(3) -0.0035(4) -0.0065(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd C10 1.973(2) . ? Pd C28 1.980(2) . ? Pd O2 2.0412(17) . ? Pd O1 2.0506(17) . ? Pd C37 2.463(3) . ? N1 C10 1.362(3) . ? N1 C11 1.390(3) . ? N1 C6 1.454(3) . ? N2 C10 1.351(3) . ? N2 C12 1.381(3) . ? N2 C13 1.461(3) . ? N3 C16 1.330(3) . ? N3 C15 1.332(3) . ? N4 C28 1.364(3) . ? N4 C29 1.391(3) . ? N4 C24 1.443(3) . ? N5 C28 1.348(3) . ? N5 C30 1.388(3) . ? N5 C31 1.469(3) . ? N6 C34 1.330(3) . ? N6 C33 1.334(3) . ? O1 C37 1.327(3) . ? O2 C37 1.327(3) . ? O3 C37 1.229(3) . ? C1 C2 1.391(3) . ? C1 C6 1.396(3) . ? C1 C7 1.501(3) . ? C2 C3 1.390(4) . ? C3 C4 1.387(4) . ? C3 C8 1.515(3) . ? C4 C5 1.396(3) . ? C5 C6 1.394(4) . ? C5 C9 1.512(4) . ? C11 C12 1.346(3) . ? C13 C18 1.510(3) . ? C14 C15 1.373(4) . ? C14 C18 1.390(4) . ? C16 C17 1.379(4) . ? C17 C18 1.390(3) . ? C19 C20 1.386(4) . ? C19 C24 1.398(4) . ? C19 C25 1.511(4) . ? C20 C21 1.382(4) . ? C21 C22 1.392(4) . ? C21 C26 1.514(4) . ? C22 C23 1.397(3) . ? C23 C24 1.400(4) . ? C23 C27 1.510(3) . ? C29 C30 1.331(3) . ? C31 C36 1.517(3) . ? C32 C33 1.385(4) . ? C32 C36 1.394(4) . ? C34 C35 1.396(4) . ? C35 C36 1.381(3) . ? C38 Cl2 1.762(3) . ? C38 Cl1 1.772(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C10 Pd C28 91.88(10) . . ? C10 Pd O2 99.77(8) . . ? C28 Pd O2 168.35(8) . . ? C10 Pd O1 164.91(8) . . ? C28 Pd O1 103.19(8) . . ? O2 Pd O1 65.16(7) . . ? C10 Pd C37 132.32(9) . . ? C28 Pd C37 135.77(9) . . ? O2 Pd C37 32.58(7) . . ? O1 Pd C37 32.59(7) . . ? C10 N1 C11 111.0(2) . . ? C10 N1 C6 123.9(2) . . ? C11 N1 C6 125.0(2) . . ? C10 N2 C12 111.5(2) . . ? C10 N2 C13 124.5(2) . . ? C12 N2 C13 123.9(2) . . ? C16 N3 C15 116.8(2) . . ? C28 N4 C29 110.3(2) . . ? C28 N4 C24 123.6(2) . . ? C29 N4 C24 125.6(2) . . ? C28 N5 C30 111.3(2) . . ? C28 N5 C31 124.6(2) . . ? C30 N5 C31 124.0(2) . . ? C34 N6 C33 117.0(2) . . ? C37 O1 Pd 91.07(14) . . ? C37 O2 Pd 91.49(14) . . ? C2 C1 C6 117.5(2) . . ? C2 C1 C7 120.8(2) . . ? C6 C1 C7 121.6(2) . . ? C1 C2 C3 121.6(2) . . ? C4 C3 C2 118.8(2) . . ? C4 C3 C8 121.3(2) . . ? C2 C3 C8 119.9(3) . . ? C3 C4 C5 122.1(2) . . ? C4 C5 C6 116.9(2) . . ? C4 C5 C9 120.9(2) . . ? C6 C5 C9 122.2(2) . . ? C1 C6 C5 123.0(2) . . ? C1 C6 N1 118.3(2) . . ? C5 C6 N1 118.7(2) . . ? N2 C10 N1 104.2(2) . . ? N2 C10 Pd 126.51(18) . . ? N1 C10 Pd 128.74(17) . . ? C12 C11 N1 106.4(2) . . ? C11 C12 N2 106.9(2) . . ? N2 C13 C18 112.4(2) . . ? C15 C14 C18 119.1(2) . . ? N3 C15 C14 124.0(2) . . ? N3 C16 C17 123.7(2) . . ? C16 C17 C18 119.2(2) . . ? C17 C18 C14 117.3(2) . . ? C17 C18 C13 120.5(2) . . ? C14 C18 C13 122.2(2) . . ? C20 C19 C24 117.6(3) . . ? C20 C19 C25 119.6(2) . . ? C24 C19 C25 122.8(2) . . ? C21 C20 C19 122.4(3) . . ? C20 C21 C22 118.6(2) . . ? C20 C21 C26 120.2(3) . . ? C22 C21 C26 121.2(3) . . ? C23 C22 C21 121.6(3) . . ? C22 C23 C24 117.5(2) . . ? C22 C23 C27 121.1(2) . . ? C24 C23 C27 121.4(2) . . ? C23 C24 C19 122.2(2) . . ? C23 C24 N4 118.0(2) . . ? C19 C24 N4 119.8(2) . . ? N5 C28 N4 104.4(2) . . ? N5 C28 Pd 127.26(17) . . ? N4 C28 Pd 128.34(17) . . ? C30 C29 N4 107.3(2) . . ? C29 C30 N5 106.7(2) . . ? N5 C31 C36 111.56(19) . . ? C33 C32 C36 118.8(2) . . ? N6 C33 C32 123.9(2) . . ? N6 C34 C35 123.5(2) . . ? C36 C35 C34 119.0(2) . . ? C35 C36 C32 117.8(2) . . ? C35 C36 C31 119.4(2) . . ? C32 C36 C31 122.7(2) . . ? O3 C37 O2 123.5(2) . . ? O3 C37 O1 124.2(2) . . ? O2 C37 O1 112.2(2) . . ? O3 C37 Pd 178.25(19) . . ? O2 C37 Pd 55.93(12) . . ? O1 C37 Pd 56.34(12) . . ? Cl2 C38 Cl1 110.22(15) . . ? 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 C10 Pd O1 C37 -2.5(4) . . . . ? C28 Pd O1 C37 -179.01(13) . . . . ? O2 Pd O1 C37 1.08(12) . . . . ? C10 Pd O2 C37 177.96(14) . . . . ? C28 Pd O2 C37 -1.6(5) . . . . ? O1 Pd O2 C37 -1.08(12) . . . . ? C6 C1 C2 C3 -1.7(4) . . . . ? C7 C1 C2 C3 175.8(2) . . . . ? C1 C2 C3 C4 1.3(4) . . . . ? C1 C2 C3 C8 -178.6(2) . . . . ? C2 C3 C4 C5 0.4(4) . . . . ? C8 C3 C4 C5 -179.6(3) . . . . ? C3 C4 C5 C6 -1.6(4) . . . . ? C3 C4 C5 C9 179.5(3) . . . . ? C2 C1 C6 C5 0.5(4) . . . . ? C7 C1 C6 C5 -177.0(2) . . . . ? C2 C1 C6 N1 -179.6(2) . . . . ? C7 C1 C6 N1 3.0(3) . . . . ? C4 C5 C6 C1 1.1(4) . . . . ? C9 C5 C6 C1 -180.0(2) . . . . ? C4 C5 C6 N1 -178.9(2) . . . . ? C9 C5 C6 N1 0.1(4) . . . . ? C10 N1 C6 C1 -100.9(3) . . . . ? C11 N1 C6 C1 81.4(3) . . . . ? C10 N1 C6 C5 79.0(3) . . . . ? C11 N1 C6 C5 -98.6(3) . . . . ? C12 N2 C10 N1 1.3(3) . . . . ? C13 N2 C10 N1 178.1(2) . . . . ? C12 N2 C10 Pd -170.53(17) . . . . ? C13 N2 C10 Pd 6.2(3) . . . . ? C11 N1 C10 N2 -1.0(3) . . . . ? C6 N1 C10 N2 -178.9(2) . . . . ? C11 N1 C10 Pd 170.64(18) . . . . ? C6 N1 C10 Pd -7.3(3) . . . . ? C28 Pd C10 N2 -113.8(2) . . . . ? O2 Pd C10 N2 66.3(2) . . . . ? O1 Pd C10 N2 69.6(4) . . . . ? C37 Pd C10 N2 67.8(2) . . . . ? C28 Pd C10 N1 76.3(2) . . . . ? O2 Pd C10 N1 -103.6(2) . . . . ? O1 Pd C10 N1 -100.2(3) . . . . ? C37 Pd C10 N1 -102.1(2) . . . . ? C10 N1 C11 C12 0.3(3) . . . . ? C6 N1 C11 C12 178.2(2) . . . . ? N1 C11 C12 N2 0.5(3) . . . . ? C10 N2 C12 C11 -1.2(3) . . . . ? C13 N2 C12 C11 -178.0(2) . . . . ? C10 N2 C13 C18 -111.7(3) . . . . ? C12 N2 C13 C18 64.6(3) . . . . ? C16 N3 C15 C14 -0.8(4) . . . . ? C18 C14 C15 N3 0.1(4) . . . . ? C15 N3 C16 C17 0.7(4) . . . . ? N3 C16 C17 C18 0.1(4) . . . . ? C16 C17 C18 C14 -0.8(4) . . . . ? C16 C17 C18 C13 -179.6(2) . . . . ? C15 C14 C18 C17 0.7(4) . . . . ? C15 C14 C18 C13 179.5(2) . . . . ? N2 C13 C18 C17 -141.3(2) . . . . ? N2 C13 C18 C14 40.0(3) . . . . ? C24 C19 C20 C21 -1.8(4) . . . . ? C25 C19 C20 C21 177.6(3) . . . . ? C19 C20 C21 C22 3.5(4) . . . . ? C19 C20 C21 C26 -176.9(3) . . . . ? C20 C21 C22 C23 -1.1(4) . . . . ? C26 C21 C22 C23 179.2(3) . . . . ? C21 C22 C23 C24 -2.7(4) . . . . ? C21 C22 C23 C27 173.9(3) . . . . ? C22 C23 C24 C19 4.5(4) . . . . ? C27 C23 C24 C19 -172.1(2) . . . . ? C22 C23 C24 N4 -178.1(2) . . . . ? C27 C23 C24 N4 5.3(3) . . . . ? C20 C19 C24 C23 -2.3(4) . . . . ? C25 C19 C24 C23 178.3(2) . . . . ? C20 C19 C24 N4 -179.7(2) . . . . ? C25 C19 C24 N4 0.9(4) . . . . ? C28 N4 C24 C23 65.6(3) . . . . ? C29 N4 C24 C23 -105.7(3) . . . . ? C28 N4 C24 C19 -116.8(3) . . . . ? C29 N4 C24 C19 71.9(3) . . . . ? C30 N5 C28 N4 -0.8(3) . . . . ? C31 N5 C28 N4 175.0(2) . . . . ? C30 N5 C28 Pd -179.12(17) . . . . ? C31 N5 C28 Pd -3.3(3) . . . . ? C29 N4 C28 N5 0.3(3) . . . . ? C24 N4 C28 N5 -172.1(2) . . . . ? C29 N4 C28 Pd 178.64(18) . . . . ? C24 N4 C28 Pd 6.2(3) . . . . ? C10 Pd C28 N5 -111.4(2) . . . . ? O2 Pd C28 N5 68.2(5) . . . . ? O1 Pd C28 N5 67.7(2) . . . . ? C37 Pd C28 N5 67.0(3) . . . . ? C10 Pd C28 N4 70.6(2) . . . . ? O2 Pd C28 N4 -109.8(4) . . . . ? O1 Pd C28 N4 -110.3(2) . . . . ? C37 Pd C28 N4 -111.0(2) . . . . ? C28 N4 C29 C30 0.3(3) . . . . ? C24 N4 C29 C30 172.5(2) . . . . ? N4 C29 C30 N5 -0.7(3) . . . . ? C28 N5 C30 C29 0.9(3) . . . . ? C31 N5 C30 C29 -174.9(2) . . . . ? C28 N5 C31 C36 -108.2(3) . . . . ? C30 N5 C31 C36 67.1(3) . . . . ? C34 N6 C33 C32 2.8(4) . . . . ? C36 C32 C33 N6 -1.3(4) . . . . ? C33 N6 C34 C35 -1.8(4) . . . . ? N6 C34 C35 C36 -0.7(4) . . . . ? C34 C35 C36 C32 2.3(3) . . . . ? C34 C35 C36 C31 -175.3(2) . . . . ? C33 C32 C36 C35 -1.3(3) . . . . ? C33 C32 C36 C31 176.1(2) . . . . ? N5 C31 C36 C35 -118.7(2) . . . . ? N5 C31 C36 C32 64.0(3) . . . . ? Pd O2 C37 O3 -178.0(2) . . . . ? Pd O2 C37 O1 1.64(19) . . . . ? Pd O1 C37 O3 178.0(2) . . . . ? Pd O1 C37 O2 -1.63(19) . . . . ? C10 Pd C37 O3 70(7) . . . . ? C28 Pd C37 O3 -108(7) . . . . ? O2 Pd C37 O3 72(7) . . . . ? O1 Pd C37 O3 -110(7) . . . . ? C10 Pd C37 O2 -2.71(18) . . . . ? C28 Pd C37 O2 179.55(13) . . . . ? O1 Pd C37 O2 178.2(2) . . . . ? C10 Pd C37 O1 179.11(13) . . . . ? C28 Pd C37 O1 1.38(19) . . . . ? O2 Pd C37 O1 -178.2(2) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.728 _refine_diff_density_min -0.751 _refine_diff_density_rms 0.083 # Attachment '4824_web_deposit_cif_file_4_GlennYap_1301086809.cif' data_i12290 _database_code_depnum_ccdc_archive 'CCDC 818965' #TrackingRef '4824_web_deposit_cif_file_4_GlennYap_1301086809.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Department of Chemistry University of Anywhere Sometown Somewhere, UK ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H32 Cl2 N4 Pd' _chemical_formula_sum 'C24 H30 Cl2 N6 Pd' _chemical_formula_weight 579.84 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Pd Pd -0.9988 1.0072 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _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 7.2059(4) _cell_length_b 8.5398(4) _cell_length_c 10.6540(5) _cell_angle_alpha 80.801(3) _cell_angle_beta 76.925(2) _cell_angle_gamma 87.557(2) _cell_volume 630.39(5) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9982 _cell_measurement_theta_min 2.42 _cell_measurement_theta_max 33.61 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.527 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 296 _exptl_absorpt_coefficient_mu 0.972 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8293 _exptl_absorpt_correction_T_max 0.8445 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2003)' _exptl_special_details ; Data collection is performed with four batch runs at \f = 0.00 \% (600 frames), at \f = 90.00 \% (600 frames), at \f = 180 \% (600 frames) and at \f = 270 \% (600 frames). Frame width = 0.30 \& in \w. Data is merged, corrected for decay, and treated with multi-scan absorption corrections. ; _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 'Bruker AXS APEX diffractometer' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 836.6 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 1 _diffrn_reflns_number 10135 _diffrn_reflns_av_R_equivalents 0.0197 _diffrn_reflns_av_sigmaI/netI 0.0167 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.99 _diffrn_reflns_theta_max 27.10 _reflns_number_total 2772 _reflns_number_gt 2721 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2002)' _computing_cell_refinement 'SAINT (Bruker, 2002)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2001)' _computing_publication_material 'SHELXTL (Sheldrick, 2001)' _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^)+(0.0329P)^2^+0.4282P] 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 2772 _refine_ls_number_parameters 153 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0195 _refine_ls_R_factor_gt 0.0190 _refine_ls_wR_factor_ref 0.0539 _refine_ls_wR_factor_gt 0.0534 _refine_ls_goodness_of_fit_ref 1.002 _refine_ls_restrained_S_all 1.002 _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 Pd Pd 0.5000 0.0000 0.5000 0.01342(6) Uani 1 2 d S . . Cl Cl 0.53396(5) 0.10766(5) 0.67928(4) 0.01900(9) Uani 1 1 d . . . N1 N 0.26941(19) 0.26885(16) 0.38808(13) 0.0180(3) Uani 1 1 d . . . N2 N 0.09895(18) 0.14456(15) 0.56414(12) 0.0153(3) Uani 1 1 d . . . C1 C 0.4381(3) 0.3192(2) 0.28265(17) 0.0251(4) Uani 1 1 d . . . H1A H 0.5113 0.2211 0.2613 0.030 Uiso 1 1 calc R . . C2 C 0.3780(4) 0.3977(4) 0.1612(2) 0.0585(8) Uani 1 1 d . . . H2A H 0.2861 0.3302 0.1402 0.088 Uiso 1 1 calc R . . H2B H 0.4899 0.4133 0.0885 0.088 Uiso 1 1 calc R . . H2C H 0.3188 0.5006 0.1755 0.088 Uiso 1 1 calc R . . C3 C 0.5675(3) 0.4209(3) 0.3318(2) 0.0433(5) Uani 1 1 d . . . H3A H 0.5949 0.3649 0.4134 0.065 Uiso 1 1 calc R . . H3B H 0.5036 0.5219 0.3473 0.065 Uiso 1 1 calc R . . H3C H 0.6869 0.4413 0.2663 0.065 Uiso 1 1 calc R . . C4 C 0.2746(2) 0.14643(18) 0.48467(15) 0.0157(3) Uani 1 1 d . . . C5 C 0.0925(2) 0.3429(2) 0.40679(16) 0.0214(3) Uani 1 1 d . . . H5A H 0.0545 0.4319 0.3524 0.026 Uiso 1 1 calc R . . C6 C -0.0148(2) 0.26425(19) 0.51698(16) 0.0204(3) Uani 1 1 d . . . H6A H -0.1437 0.2864 0.5551 0.025 Uiso 1 1 calc R . . C7 C 0.0349(2) 0.03424(18) 0.68514(15) 0.0173(3) Uani 1 1 d . . . H7A H 0.1389 -0.0420 0.6980 0.021 Uiso 1 1 calc R . . H7B H -0.0749 -0.0267 0.6776 0.021 Uiso 1 1 calc R . . C8 C -0.2200(3) 0.1411(2) 1.01260(17) 0.0260(4) Uani 1 1 d . . . H8A H -0.3234 0.1013 1.0814 0.031 Uiso 1 1 calc R . . C9 C -0.1750(2) 0.0651(2) 0.90348(16) 0.0208(3) Uani 1 1 d . . . H9A H -0.2477 -0.0228 0.8981 0.025 Uiso 1 1 calc R . . C10 C -0.0229(2) 0.11893(19) 0.80243(15) 0.0172(3) Uani 1 1 d . . . C11 C 0.0764(2) 0.2496(2) 0.81574(17) 0.0212(3) Uani 1 1 d . . . H11A H 0.1817 0.2908 0.7491 0.025 Uiso 1 1 calc R . . C12 C 0.0196(3) 0.3182(2) 0.92712(18) 0.0242(3) Uani 1 1 d . . . H12A H 0.0884 0.4078 0.9339 0.029 Uiso 1 1 calc R . . N3 N -0.1260(2) 0.2675(2) 1.02652(15) 0.0279(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 Pd 0.01309(9) 0.01364(9) 0.01174(9) -0.00158(6) 0.00045(6) 0.00122(6) Cl 0.01808(18) 0.02240(19) 0.01676(18) -0.00656(14) -0.00225(14) 0.00177(14) N1 0.0196(7) 0.0164(6) 0.0151(6) -0.0007(5) 0.0007(5) 0.0021(5) N2 0.0162(6) 0.0159(6) 0.0128(6) -0.0036(5) -0.0003(5) 0.0014(5) C1 0.0258(9) 0.0212(8) 0.0199(8) 0.0027(6) 0.0074(7) 0.0038(7) C2 0.0519(15) 0.0773(19) 0.0252(11) 0.0232(11) 0.0090(10) 0.0257(13) C3 0.0363(11) 0.0357(11) 0.0494(13) -0.0099(10) 0.0133(10) -0.0157(9) C4 0.0172(7) 0.0153(7) 0.0135(7) -0.0036(5) -0.0004(6) -0.0003(5) C5 0.0228(8) 0.0185(8) 0.0213(8) -0.0024(6) -0.0031(6) 0.0058(6) C6 0.0187(7) 0.0192(8) 0.0221(8) -0.0048(6) -0.0018(6) 0.0047(6) C7 0.0179(7) 0.0170(7) 0.0147(7) -0.0024(6) 0.0010(6) -0.0010(6) C8 0.0236(8) 0.0355(10) 0.0156(8) -0.0039(7) 0.0012(6) 0.0054(7) C9 0.0189(8) 0.0244(8) 0.0175(8) -0.0021(6) -0.0016(6) 0.0004(6) C10 0.0168(7) 0.0187(7) 0.0152(7) -0.0024(6) -0.0023(6) 0.0034(6) C11 0.0200(8) 0.0208(8) 0.0211(8) -0.0048(6) 0.0000(6) 0.0007(6) C12 0.0258(8) 0.0218(8) 0.0263(9) -0.0098(7) -0.0045(7) 0.0024(6) N3 0.0294(8) 0.0333(8) 0.0211(7) -0.0112(6) -0.0025(6) 0.0069(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 Pd C4 2.0275(15) 2_656 ? Pd C4 2.0275(15) . ? Pd Cl 2.3121(4) . ? Pd Cl 2.3121(4) 2_656 ? N1 C4 1.350(2) . ? N1 C5 1.386(2) . ? N1 C1 1.482(2) . ? N2 C4 1.353(2) . ? N2 C6 1.386(2) . ? N2 C7 1.464(2) . ? C1 C2 1.505(3) . ? C1 C3 1.528(3) . ? C1 H1A 1.0000 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C5 C6 1.345(2) . ? C5 H5A 0.9500 . ? C6 H6A 0.9500 . ? C7 C10 1.512(2) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 N3 1.344(3) . ? C8 C9 1.389(2) . ? C8 H8A 0.9500 . ? C9 C10 1.387(2) . ? C9 H9A 0.9500 . ? C10 C11 1.394(2) . ? C11 C12 1.379(2) . ? C11 H11A 0.9500 . ? C12 N3 1.341(2) . ? C12 H12A 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 C4 Pd C4 180.0 2_656 . ? C4 Pd Cl 90.45(4) 2_656 . ? C4 Pd Cl 89.55(4) . . ? C4 Pd Cl 89.55(4) 2_656 2_656 ? C4 Pd Cl 90.45(4) . 2_656 ? Cl Pd Cl 180.0 . 2_656 ? C4 N1 C5 110.98(13) . . ? C4 N1 C1 122.72(13) . . ? C5 N1 C1 126.19(14) . . ? C4 N2 C6 110.86(13) . . ? C4 N2 C7 125.62(13) . . ? C6 N2 C7 123.51(13) . . ? N1 C1 C2 110.68(16) . . ? N1 C1 C3 109.82(15) . . ? C2 C1 C3 114.0(2) . . ? N1 C1 H1A 107.3 . . ? C2 C1 H1A 107.3 . . ? C3 C1 H1A 107.3 . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? N1 C4 N2 104.76(13) . . ? N1 C4 Pd 125.97(11) . . ? N2 C4 Pd 129.27(11) . . ? C6 C5 N1 106.66(14) . . ? C6 C5 H5A 126.7 . . ? N1 C5 H5A 126.7 . . ? C5 C6 N2 106.73(14) . . ? C5 C6 H6A 126.6 . . ? N2 C6 H6A 126.6 . . ? N2 C7 C10 112.12(12) . . ? N2 C7 H7A 109.2 . . ? C10 C7 H7A 109.2 . . ? N2 C7 H7B 109.2 . . ? C10 C7 H7B 109.2 . . ? H7A C7 H7B 107.9 . . ? N3 C8 C9 123.85(16) . . ? N3 C8 H8A 118.1 . . ? C9 C8 H8A 118.1 . . ? C10 C9 C8 119.34(16) . . ? C10 C9 H9A 120.3 . . ? C8 C9 H9A 120.3 . . ? C9 C10 C11 117.43(15) . . ? C9 C10 C7 120.53(15) . . ? C11 C10 C7 122.01(14) . . ? C12 C11 C10 118.99(16) . . ? C12 C11 H11A 120.5 . . ? C10 C11 H11A 120.5 . . ? N3 C12 C11 124.64(17) . . ? N3 C12 H12A 117.7 . . ? C11 C12 H12A 117.7 . . ? C12 N3 C8 115.74(15) . . ? 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 C4 N1 C1 C2 153.08(19) . . . . ? C5 N1 C1 C2 -31.0(3) . . . . ? C4 N1 C1 C3 -80.1(2) . . . . ? C5 N1 C1 C3 95.7(2) . . . . ? C5 N1 C4 N2 0.01(18) . . . . ? C1 N1 C4 N2 176.45(14) . . . . ? C5 N1 C4 Pd 179.23(11) . . . . ? C1 N1 C4 Pd -4.3(2) . . . . ? C6 N2 C4 N1 0.33(17) . . . . ? C7 N2 C4 N1 -178.72(13) . . . . ? C6 N2 C4 Pd -178.86(11) . . . . ? C7 N2 C4 Pd 2.1(2) . . . . ? C4 Pd C4 N1 -86(4) 2_656 . . . ? Cl Pd C4 N1 111.44(13) . . . . ? Cl Pd C4 N1 -68.56(13) 2_656 . . . ? C4 Pd C4 N2 93(4) 2_656 . . . ? Cl Pd C4 N2 -69.53(14) . . . . ? Cl Pd C4 N2 110.47(14) 2_656 . . . ? C4 N1 C5 C6 -0.35(19) . . . . ? C1 N1 C5 C6 -176.63(16) . . . . ? N1 C5 C6 N2 0.53(18) . . . . ? C4 N2 C6 C5 -0.56(18) . . . . ? C7 N2 C6 C5 178.52(14) . . . . ? C4 N2 C7 C10 118.83(16) . . . . ? C6 N2 C7 C10 -60.11(19) . . . . ? N3 C8 C9 C10 1.0(3) . . . . ? C8 C9 C10 C11 -0.7(2) . . . . ? C8 C9 C10 C7 177.29(15) . . . . ? N2 C7 C10 C9 143.56(15) . . . . ? N2 C7 C10 C11 -38.5(2) . . . . ? C9 C10 C11 C12 0.0(2) . . . . ? C7 C10 C11 C12 -178.01(15) . . . . ? C10 C11 C12 N3 0.6(3) . . . . ? C11 C12 N3 C8 -0.3(3) . . . . ? C9 C8 N3 C12 -0.5(3) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.535 _refine_diff_density_min -0.224 _refine_diff_density_rms 0.062