# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Serrano, JoseLuis' _publ_contact_author_email jose.serrano@upct.es _publ_section_title ; New cyclometallated precursors of unsubstituted N-phenylpyrazol [{Pd(phpz)(\^I1/4-X)}2] (X = AcO or OH) and study of their reactivity towards selected ligands. ; loop_ _publ_author_name J.Serrano G.Sanchez J.Pirez J.Garcia E.Pirez L.Garcia ; J.M.Galiana ; 'I.da Silva' M.Martinez # Attachment '- crystaldata.cif' data_compound1 _database_code_depnum_ccdc_archive 'CCDC 783647' #TrackingRef '- crystaldata.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C22 H20 N4 O4 Pd2' _chemical_formula_sum 'C22 H20 N4 O4 Pd2' _chemical_formula_weight 617.22 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' _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M P3121 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z+1/3' 'y, x, -z' '-x+y, -x, z+2/3' '-x, -x+y, -z+1/3' 'x-y, -y, -z+2/3' _cell_length_a 11.7292(3) _cell_length_b 11.7292(3) _cell_length_c 27.8342(13) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 3316.2(2) _cell_formula_units_Z 6 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.854 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1824 _exptl_absorpt_coefficient_mu 1.663 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.7428 _exptl_absorpt_correction_T_max 0.8924 _exptl_absorpt_process_details ? _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 38625 _diffrn_reflns_av_R_equivalents 0.0415 _diffrn_reflns_av_sigmaI/netI 0.0281 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 2.00 _diffrn_reflns_theta_max 28.23 _reflns_number_total 5225 _reflns_number_gt 5153 _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^)+(0.0302P)^2^+2.0924P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.01(3) _refine_ls_number_reflns 5225 _refine_ls_number_parameters 289 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0267 _refine_ls_R_factor_gt 0.0260 _refine_ls_wR_factor_ref 0.0582 _refine_ls_wR_factor_gt 0.0578 _refine_ls_goodness_of_fit_ref 1.064 _refine_ls_restrained_S_all 1.064 _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 O1 O 0.9004(2) 0.1143(2) 0.06356(8) 0.0210(5) Uani 1 1 d . . . O4 O 0.7359(2) 0.0536(2) 0.18169(7) 0.0215(5) Uani 1 1 d . . . O2 O 0.7911(2) 0.2257(2) 0.13192(8) 0.0209(5) Uani 1 1 d . . . O3 O 0.8368(2) -0.0620(2) 0.11170(8) 0.0212(5) Uani 1 1 d . . . N3 N 0.5478(3) -0.2308(3) 0.08253(9) 0.0167(5) Uani 1 1 d . . . N2 N 0.4889(3) 0.0675(3) 0.02274(10) 0.0214(6) Uani 1 1 d . . . N4 N 0.4224(3) -0.2568(3) 0.07587(9) 0.0175(5) Uani 1 1 d . . . N1 N 0.5699(3) 0.1368(3) 0.05986(10) 0.0217(6) Uani 1 1 d . . . C21 C 0.7873(3) 0.1752(3) 0.17210(11) 0.0187(6) Uani 1 1 d . . . C10 C 0.9184(3) 0.0306(3) 0.08630(11) 0.0183(6) Uani 1 1 d . . . C6 C 0.5409(3) 0.0090(3) -0.00900(11) 0.0211(7) Uani 1 1 d . . . C22 C 0.8517(4) 0.2673(4) 0.21399(12) 0.0262(7) Uani 1 1 d . . . H22A H 0.8418 0.2159 0.2430 0.039 Uiso 1 1 calc R . . H22B H 0.8097 0.3205 0.2190 0.039 Uiso 1 1 calc R . . H22C H 0.9455 0.3253 0.2072 0.039 Uiso 1 1 calc R . . C12 C 0.4732(3) -0.1125(3) 0.14237(11) 0.0168(6) Uani 1 1 d . . . C1 C 0.6645(3) 0.0308(3) 0.00421(10) 0.0178(6) Uani 1 1 d . . . C11 C 1.0554(3) 0.0496(4) 0.08247(13) 0.0253(7) Uani 1 1 d . . . H11A H 1.1092 0.1249 0.0615 0.038 Uiso 1 1 calc R . . H11B H 1.0504 -0.0299 0.0689 0.038 Uiso 1 1 calc R . . H11C H 1.0954 0.0661 0.1145 0.038 Uiso 1 1 calc R . . C3 C 0.6616(4) -0.0870(3) -0.06783(12) 0.0297(8) Uani 1 1 d . . . H3 H 0.7035 -0.1196 -0.0883 0.036 Uiso 1 1 calc R . . C2 C 0.7249(4) -0.0174(3) -0.02610(11) 0.0231(7) Uani 1 1 d . . . H2 H 0.8100 -0.0031 -0.0184 0.028 Uiso 1 1 calc R . . C20 C 0.3694(4) -0.3331(4) 0.03650(12) 0.0261(8) Uani 1 1 d . . . H20 H 0.2833 -0.3639 0.0242 0.031 Uiso 1 1 calc R . . C5 C 0.4755(4) -0.0602(3) -0.05005(12) 0.0274(8) Uani 1 1 d . . . H5 H 0.3906 -0.0744 -0.0579 0.033 Uiso 1 1 calc R . . C18 C 0.5727(4) -0.2923(3) 0.04737(12) 0.0228(7) Uani 1 1 d . . . H18 H 0.6535 -0.2916 0.0432 0.027 Uiso 1 1 calc R . . C15 C 0.2172(4) -0.1505(4) 0.14107(13) 0.0263(8) Uani 1 1 d . . . H15 H 0.1307 -0.1629 0.1414 0.032 Uiso 1 1 calc R . . C17 C 0.3779(3) -0.1957(3) 0.10926(11) 0.0175(6) Uani 1 1 d . . . C4 C 0.5381(4) -0.1078(3) -0.07903(12) 0.0319(9) Uani 1 1 d . . . H4 H 0.4953 -0.1557 -0.1072 0.038 Uiso 1 1 calc R . . C14 C 0.3089(4) -0.0672(3) 0.17366(13) 0.0244(7) Uani 1 1 d . . . H14 H 0.2851 -0.0213 0.1959 0.029 Uiso 1 1 calc R . . C9 C 0.3786(4) 0.0771(4) 0.02276(15) 0.0331(9) Uani 1 1 d . . . H9 H 0.3077 0.0377 0.0006 0.040 Uiso 1 1 calc R . . C8 C 0.3896(4) 0.1554(5) 0.06139(15) 0.0366(10) Uani 1 1 d . . . H8 H 0.3278 0.1810 0.0709 0.044 Uiso 1 1 calc R . . C13 C 0.4358(3) -0.0483(3) 0.17488(12) 0.0219(7) Uani 1 1 d . . . H13 H 0.4969 0.0090 0.1981 0.026 Uiso 1 1 calc R . . C19 C 0.4633(4) -0.3577(4) 0.01753(13) 0.0275(8) Uani 1 1 d . . . H19 H 0.4552 -0.4087 -0.0101 0.033 Uiso 1 1 calc R . . C7 C 0.5091(4) 0.1900(4) 0.08381(14) 0.0292(8) Uani 1 1 d . . . H7 H 0.5421 0.2432 0.1118 0.035 Uiso 1 1 calc R . . C16 C 0.2508(3) -0.2164(4) 0.10773(12) 0.0223(7) Uani 1 1 d . . . H16 H 0.1890 -0.2737 0.0847 0.027 Uiso 1 1 calc R . . Pd1 Pd 0.73172(2) 0.12421(2) 0.065480(8) 0.01465(6) Uani 1 1 d . . . Pd2 Pd 0.64867(2) -0.08919(2) 0.130763(8) 0.01483(6) 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 O1 0.0167(11) 0.0253(13) 0.0209(11) 0.0027(10) 0.0003(9) 0.0103(10) O4 0.0227(12) 0.0230(12) 0.0170(10) -0.0031(9) -0.0047(9) 0.0100(10) O2 0.0234(12) 0.0193(11) 0.0184(11) -0.0020(9) -0.0017(9) 0.0095(10) O3 0.0161(11) 0.0195(12) 0.0281(12) -0.0009(10) -0.0023(9) 0.0090(10) N3 0.0157(13) 0.0172(13) 0.0121(12) 0.0020(10) -0.0015(10) 0.0044(11) N2 0.0144(13) 0.0229(15) 0.0211(14) 0.0102(12) 0.0009(11) 0.0048(11) N4 0.0126(13) 0.0157(13) 0.0190(13) 0.0015(10) -0.0015(10) 0.0032(11) N1 0.0165(14) 0.0277(16) 0.0204(14) 0.0053(12) 0.0017(11) 0.0105(12) C21 0.0118(14) 0.0225(16) 0.0217(15) -0.0064(12) -0.0018(12) 0.0085(13) C10 0.0146(14) 0.0175(16) 0.0206(15) -0.0072(13) -0.0036(12) 0.0064(13) C6 0.0207(16) 0.0156(16) 0.0197(15) 0.0087(12) 0.0024(13) 0.0037(12) C22 0.0223(17) 0.0328(19) 0.0238(17) -0.0106(15) -0.0074(14) 0.0140(16) C12 0.0153(15) 0.0173(15) 0.0146(14) 0.0072(12) 0.0010(12) 0.0058(13) C1 0.0147(14) 0.0127(15) 0.0185(14) 0.0032(12) 0.0002(11) 0.0013(12) C11 0.0156(16) 0.0280(18) 0.0366(19) -0.0056(15) -0.0053(14) 0.0142(15) C3 0.045(2) 0.0181(16) 0.0209(16) 0.0007(13) -0.0003(15) 0.0120(16) C2 0.0272(18) 0.0212(16) 0.0185(15) 0.0036(13) 0.0019(13) 0.0103(14) C20 0.0236(18) 0.0246(18) 0.0202(17) -0.0006(14) -0.0057(14) 0.0045(15) C5 0.0247(17) 0.0217(17) 0.0227(16) 0.0089(14) -0.0094(14) 0.0018(15) C18 0.0225(17) 0.0203(16) 0.0246(17) 0.0039(13) 0.0034(14) 0.0099(14) C15 0.0225(17) 0.0275(19) 0.0301(19) 0.0091(15) 0.0041(14) 0.0134(15) C17 0.0160(15) 0.0178(15) 0.0163(15) 0.0055(12) 0.0016(12) 0.0066(13) C4 0.043(2) 0.0191(16) 0.0193(16) -0.0009(13) -0.0064(16) 0.0048(17) C14 0.0246(18) 0.0214(17) 0.0282(18) 0.0020(14) 0.0096(14) 0.0123(15) C9 0.0119(16) 0.040(2) 0.040(2) 0.0180(18) 0.0039(15) 0.0082(16) C8 0.025(2) 0.054(3) 0.040(2) 0.014(2) 0.0125(17) 0.027(2) C13 0.0223(16) 0.0206(17) 0.0181(16) 0.0019(13) 0.0019(13) 0.0071(14) C19 0.033(2) 0.0244(19) 0.0188(17) -0.0079(14) 0.0007(15) 0.0093(16) C7 0.0268(19) 0.037(2) 0.0267(18) 0.0064(16) 0.0074(15) 0.0186(17) C16 0.0188(16) 0.0260(18) 0.0196(16) 0.0043(14) -0.0001(13) 0.0093(15) Pd1 0.01260(12) 0.01623(12) 0.01482(11) 0.00110(9) -0.00078(9) 0.00697(10) Pd2 0.01197(11) 0.01421(12) 0.01578(11) 0.00006(8) -0.00165(8) 0.00465(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1 C10 1.272(4) . ? O1 Pd1 2.040(2) . ? O4 C21 1.268(4) . ? O4 Pd2 2.037(2) . ? O2 C21 1.256(4) . ? O2 Pd1 2.120(2) . ? O3 C10 1.248(4) . ? O3 Pd2 2.132(2) . ? N3 C18 1.332(4) . ? N3 N4 1.357(4) . ? N3 Pd2 1.999(3) . ? N2 N1 1.363(4) . ? N2 C9 1.355(5) . ? N2 C6 1.429(4) . ? N4 C20 1.353(4) . ? N4 C17 1.423(4) . ? N1 C7 1.337(5) . ? N1 Pd1 1.983(3) . ? C21 C22 1.510(4) . ? C10 C11 1.511(4) . ? C6 C1 1.390(5) . ? C6 C5 1.389(5) . ? C12 C13 1.382(5) . ? C12 C17 1.400(4) . ? C12 Pd2 1.963(3) . ? C1 C2 1.391(5) . ? C1 Pd1 1.966(3) . ? C3 C4 1.378(6) . ? C3 C2 1.400(5) . ? C20 C19 1.376(5) . ? C5 C4 1.382(6) . ? C18 C19 1.393(5) . ? C15 C14 1.372(5) . ? C15 C16 1.385(5) . ? C17 C16 1.386(5) . ? C14 C13 1.392(5) . ? C9 C8 1.377(6) . ? C8 C7 1.396(5) . ? Pd1 Pd2 2.8421(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 O1 Pd1 124.8(2) . . ? C21 O4 Pd2 122.6(2) . . ? C21 O2 Pd1 126.0(2) . . ? C10 O3 Pd2 123.9(2) . . ? C18 N3 N4 106.5(3) . . ? C18 N3 Pd2 138.1(2) . . ? N4 N3 Pd2 113.8(2) . . ? N1 N2 C9 111.1(3) . . ? N1 N2 C6 114.7(3) . . ? C9 N2 C6 134.0(3) . . ? N3 N4 C20 110.3(3) . . ? N3 N4 C17 115.3(3) . . ? C20 N4 C17 134.3(3) . . ? C7 N1 N2 106.3(3) . . ? C7 N1 Pd1 138.6(3) . . ? N2 N1 Pd1 115.0(2) . . ? O2 C21 O4 127.1(3) . . ? O2 C21 C22 117.6(3) . . ? O4 C21 C22 115.4(3) . . ? O3 C10 O1 127.1(3) . . ? O3 C10 C11 117.7(3) . . ? O1 C10 C11 115.2(3) . . ? C1 C6 C5 123.0(3) . . ? C1 C6 N2 113.8(3) . . ? C5 C6 N2 123.1(3) . . ? C13 C12 C17 116.8(3) . . ? C13 C12 Pd2 128.9(3) . . ? C17 C12 Pd2 113.9(2) . . ? C6 C1 C2 117.5(3) . . ? C6 C1 Pd1 115.0(2) . . ? C2 C1 Pd1 127.5(3) . . ? C4 C3 C2 119.7(3) . . ? C1 C2 C3 120.7(3) . . ? N4 C20 C19 107.4(3) . . ? C4 C5 C6 117.8(3) . . ? N3 C18 C19 110.2(3) . . ? C14 C15 C16 120.0(3) . . ? C16 C17 C12 123.8(3) . . ? C16 C17 N4 121.7(3) . . ? C12 C17 N4 114.5(3) . . ? C3 C4 C5 121.3(3) . . ? C15 C14 C13 121.6(3) . . ? N2 C9 C8 106.3(3) . . ? C9 C8 C7 106.8(3) . . ? C12 C13 C14 120.2(3) . . ? C20 C19 C18 105.6(3) . . ? N1 C7 C8 109.5(4) . . ? C17 C16 C15 117.6(3) . . ? C1 Pd1 N1 80.86(13) . . ? C1 Pd1 O1 94.33(12) . . ? N1 Pd1 O1 173.91(10) . . ? C1 Pd1 O2 175.70(12) . . ? N1 Pd1 O2 94.86(11) . . ? O1 Pd1 O2 89.96(9) . . ? C1 Pd1 Pd2 101.45(9) . . ? N1 Pd1 Pd2 101.34(8) . . ? O1 Pd1 Pd2 83.21(7) . . ? O2 Pd1 Pd2 78.96(6) . . ? C12 Pd2 N3 81.44(12) . . ? C12 Pd2 O4 93.49(12) . . ? N3 Pd2 O4 174.92(10) . . ? C12 Pd2 O3 175.02(11) . . ? N3 Pd2 O3 95.46(10) . . ? O4 Pd2 O3 89.61(9) . . ? C12 Pd2 Pd1 95.84(9) . . ? N3 Pd2 Pd1 95.87(7) . . ? O4 Pd2 Pd1 84.87(6) . . ? O3 Pd2 Pd1 80.55(6) . . ? _diffrn_measured_fraction_theta_max 0.977 _diffrn_reflns_theta_full 0.50 _diffrn_measured_fraction_theta_full 0.000 _refine_diff_density_max 0.714 _refine_diff_density_min -0.396 _refine_diff_density_rms 0.100 #===END data_compound2 _database_code_depnum_ccdc_archive 'CCDC 783648' #TrackingRef '- crystaldata.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C16 H12 N2 O2 Pd' _chemical_formula_sum 'C16 H12 N2 O2 Pd' _chemical_formula_weight 370.68 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/a loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x-1/2, -y-1/2, z' _cell_length_a 14.4947(10) _cell_length_b 12.1565(9) _cell_length_c 15.8097(11) _cell_angle_alpha 90.00 _cell_angle_beta 99.4880(10) _cell_angle_gamma 90.00 _cell_volume 2747.6(3) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.792 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1472 _exptl_absorpt_coefficient_mu 1.356 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.7547 _exptl_absorpt_correction_T_max 0.9353 _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 32760 _diffrn_reflns_av_R_equivalents 0.0339 _diffrn_reflns_av_sigmaI/netI 0.0282 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.31 _diffrn_reflns_theta_max 28.68 _reflns_number_total 6649 _reflns_number_gt 6265 _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^)+(0.0612P)^2^+12.5404P] 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 6649 _refine_ls_number_parameters 379 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0627 _refine_ls_R_factor_gt 0.0590 _refine_ls_wR_factor_ref 0.1385 _refine_ls_wR_factor_gt 0.1362 _refine_ls_goodness_of_fit_ref 1.217 _refine_ls_restrained_S_all 1.217 _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 C17 C 0.1572(3) 0.4711(4) 0.5526(3) 0.0179(9) Uani 1 1 d . . . C27 C -0.0308(3) 0.8146(4) 0.5057(3) 0.0206(10) Uani 1 1 d . . . C21 C 0.2529(4) 0.3061(4) 0.5462(3) 0.0229(10) Uani 1 1 d . . . H21 H 0.2796 0.2533 0.5131 0.027 Uiso 1 1 calc R . . C20 C 0.2690(4) 0.3017(4) 0.6354(4) 0.0242(10) Uani 1 1 d . . . H20 H 0.3074 0.2453 0.6640 0.029 Uiso 1 1 calc R . . C22 C 0.1969(3) 0.3897(4) 0.5073(3) 0.0189(9) Uani 1 1 d . . . C28 C -0.0848(4) 0.9094(5) 0.5143(4) 0.0305(12) Uani 1 1 d . . . H28 H -0.1175 0.9437 0.4642 0.037 Uiso 1 1 calc R . . C15 C -0.0462(4) 0.6700(5) -0.0269(4) 0.0303(12) Uani 1 1 d . . . H16 H -0.0411 0.6710 -0.0860 0.036 Uiso 1 1 calc R . . C14 C -0.0971(4) 0.5881(5) 0.0032(5) 0.0363(14) Uani 1 1 d . . . H15 H -0.1273 0.5346 -0.0356 0.044 Uiso 1 1 calc R . . C26 C -0.0275(3) 0.7790(4) 0.4199(3) 0.0226(10) Uani 1 1 d . . . H26 H -0.0611 0.8235 0.3758 0.027 Uiso 1 1 calc R . . Pd2 Pd 0.08481(3) 0.58272(3) 0.48063(2) 0.01738(11) Uani 1 1 d . . . O4 O 0.0673(3) 0.6718(3) 0.5835(2) 0.0238(7) Uani 1 1 d . . . O3 O 0.0129(3) 0.6983(3) 0.3950(2) 0.0239(7) Uani 1 1 d . . . N3 N 0.1187(3) 0.4864(3) 0.3882(3) 0.0218(8) Uani 1 1 d . . . C25 C 0.1982(4) 0.3429(4) 0.3507(4) 0.0273(11) Uani 1 1 d . . . H23 H 0.2371 0.2796 0.3545 0.033 Uiso 1 1 calc R . . N4 N 0.1754(3) 0.4008(3) 0.4171(3) 0.0198(8) Uani 1 1 d . . . C18 C 0.1732(4) 0.4637(4) 0.6421(3) 0.0226(10) Uani 1 1 d . . . H18 H 0.1460 0.5161 0.6752 0.027 Uiso 1 1 calc R . . C32 C 0.0165(3) 0.7604(4) 0.5811(3) 0.0213(10) Uani 1 1 d . . . C19 C 0.2290(4) 0.3795(4) 0.6829(4) 0.0256(11) Uani 1 1 d . . . H19 H 0.2399 0.3752 0.7437 0.031 Uiso 1 1 calc R . . C23 C 0.1056(4) 0.4814(5) 0.3024(4) 0.0281(11) Uani 1 1 d . . . H25 H 0.0684 0.5311 0.2649 0.034 Uiso 1 1 calc R . . C29 C -0.0913(4) 0.9535(5) 0.5930(4) 0.0311(12) Uani 1 1 d . . . H29 H -0.1275 1.0178 0.5973 0.037 Uiso 1 1 calc R . . C24 C 0.1547(4) 0.3925(5) 0.2763(4) 0.0299(12) Uani 1 1 d . . . H24 H 0.1575 0.3706 0.2191 0.036 Uiso 1 1 calc R . . C31 C 0.0079(4) 0.8087(5) 0.6612(4) 0.0272(11) Uani 1 1 d . . . H31 H 0.0385 0.7754 0.7126 0.033 Uiso 1 1 calc R . . C30 C -0.0441(4) 0.9029(5) 0.6660(4) 0.0287(12) Uani 1 1 d . . . H30 H -0.0477 0.9338 0.7206 0.034 Uiso 1 1 calc R . . Pd1 Pd 0.11057(2) 0.95528(3) 0.05412(2) 0.01639(11) Uani 1 1 d . . . O2 O 0.0444(2) 0.8278(3) -0.0076(2) 0.0205(7) Uani 1 1 d . . . O1 O 0.0805(3) 0.9035(3) 0.1725(2) 0.0228(7) Uani 1 1 d . . . N1 N 0.1868(3) 1.0823(3) 0.1040(3) 0.0202(8) Uani 1 1 d . . . N2 N 0.2301(3) 1.1387(3) 0.0474(3) 0.0208(8) Uani 1 1 d . . . C1 C 0.1480(3) 1.0138(4) -0.0512(3) 0.0188(9) Uani 1 1 d . . . C16 C -0.0016(3) 0.7522(4) 0.0271(3) 0.0205(10) Uani 1 1 d . . . C6 C 0.2091(3) 1.1042(4) -0.0392(3) 0.0199(9) Uani 1 1 d . . . C10 C 0.0322(4) 0.8209(4) 0.1803(3) 0.0231(10) Uani 1 1 d . . . H10 H 0.0217 0.8056 0.2368 0.028 Uiso 1 1 calc R . . C2 C 0.1235(4) 0.9758(4) -0.1347(3) 0.0240(10) Uani 1 1 d . . . H2 H 0.0821 0.9150 -0.1461 0.029 Uiso 1 1 calc R . . C4 C 0.2196(4) 1.1147(5) -0.1868(4) 0.0303(12) Uani 1 1 d . . . H4 H 0.2436 1.1475 -0.2332 0.036 Uiso 1 1 calc R . . C9 C 0.2869(4) 1.2169(4) 0.0885(4) 0.0264(11) Uani 1 1 d . . . H7 H 0.3243 1.2672 0.0629 0.032 Uiso 1 1 calc R . . C5 C 0.2454(4) 1.1553(4) -0.1044(4) 0.0252(11) Uani 1 1 d . . . H5 H 0.2867 1.2162 -0.0932 0.030 Uiso 1 1 calc R . . C11 C -0.0092(3) 0.7465(4) 0.1165(3) 0.0217(10) Uani 1 1 d . . . C12 C -0.0623(4) 0.6587(4) 0.1451(4) 0.0279(11) Uani 1 1 d . . . H13 H -0.0673 0.6541 0.2041 0.033 Uiso 1 1 calc R . . C8 C 0.2807(4) 1.2100(5) 0.1735(4) 0.0300(12) Uani 1 1 d . . . H8 H 0.3131 1.2541 0.2185 0.036 Uiso 1 1 calc R . . C7 C 0.2178(4) 1.1263(4) 0.1816(3) 0.0248(10) Uani 1 1 d . . . H9 H 0.1994 1.1035 0.2338 0.030 Uiso 1 1 calc R . . C3 C 0.1586(4) 1.0256(4) -0.2015(3) 0.0255(11) Uani 1 1 d . . . H3 H 0.1407 0.9986 -0.2582 0.031 Uiso 1 1 calc R . . C13 C -0.1055(4) 0.5818(5) 0.0901(4) 0.0338(13) Uani 1 1 d . . . H14 H -0.1409 0.5246 0.1102 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 C17 0.017(2) 0.012(2) 0.025(2) -0.0020(17) 0.0048(18) -0.0026(16) C27 0.020(2) 0.013(2) 0.029(3) 0.0010(18) 0.0041(19) -0.0005(18) C21 0.022(2) 0.015(2) 0.032(3) -0.0008(19) 0.004(2) -0.0026(18) C20 0.021(2) 0.017(2) 0.034(3) 0.008(2) 0.005(2) -0.0008(19) C22 0.020(2) 0.016(2) 0.022(2) 0.0011(18) 0.0054(18) -0.0044(18) C28 0.026(3) 0.024(3) 0.041(3) -0.003(2) 0.006(2) 0.004(2) C15 0.027(3) 0.030(3) 0.034(3) -0.004(2) 0.002(2) -0.003(2) C14 0.027(3) 0.028(3) 0.053(4) -0.003(3) 0.006(3) -0.008(2) C26 0.020(2) 0.020(2) 0.026(3) 0.003(2) 0.0014(19) 0.0003(19) Pd2 0.01822(19) 0.01411(18) 0.01996(19) -0.00151(13) 0.00361(14) -0.00029(13) O4 0.0284(19) 0.0201(17) 0.0224(17) -0.0029(14) 0.0027(14) 0.0061(15) O3 0.0266(18) 0.0222(18) 0.0228(18) 0.0000(14) 0.0038(14) 0.0001(15) N3 0.024(2) 0.0173(19) 0.024(2) -0.0030(16) 0.0043(17) 0.0000(16) C25 0.031(3) 0.022(3) 0.028(3) -0.006(2) 0.005(2) 0.002(2) N4 0.024(2) 0.0144(19) 0.021(2) -0.0028(15) 0.0049(16) 0.0016(16) C18 0.020(2) 0.021(2) 0.028(3) -0.001(2) 0.008(2) -0.0012(19) C32 0.017(2) 0.017(2) 0.029(3) -0.0041(19) 0.0034(19) -0.0018(18) C19 0.024(3) 0.025(3) 0.028(3) 0.005(2) 0.006(2) -0.001(2) C23 0.033(3) 0.027(3) 0.025(3) -0.001(2) 0.005(2) 0.002(2) C29 0.020(2) 0.026(3) 0.048(4) -0.008(2) 0.008(2) 0.006(2) C24 0.037(3) 0.028(3) 0.024(3) -0.007(2) 0.005(2) 0.001(2) C31 0.023(2) 0.031(3) 0.028(3) -0.009(2) 0.003(2) 0.003(2) C30 0.020(2) 0.031(3) 0.036(3) -0.015(2) 0.008(2) 0.001(2) Pd1 0.01595(18) 0.01215(18) 0.02154(19) 0.00104(13) 0.00442(13) -0.00011(12) O2 0.0228(17) 0.0176(16) 0.0214(17) -0.0004(13) 0.0044(14) -0.0033(14) O1 0.0246(18) 0.0216(18) 0.0232(18) -0.0019(14) 0.0065(14) -0.0044(14) N1 0.019(2) 0.0145(19) 0.028(2) 0.0015(16) 0.0068(17) 0.0022(15) N2 0.022(2) 0.0119(18) 0.029(2) 0.0012(16) 0.0065(17) -0.0005(15) C1 0.021(2) 0.010(2) 0.025(2) 0.0019(18) 0.0034(19) 0.0037(17) C16 0.018(2) 0.015(2) 0.029(3) 0.0027(19) 0.0042(19) 0.0044(18) C6 0.018(2) 0.013(2) 0.029(3) 0.0013(18) 0.0030(19) 0.0027(17) C10 0.022(2) 0.025(2) 0.023(2) 0.006(2) 0.0054(19) 0.003(2) C2 0.027(3) 0.017(2) 0.027(3) 0.0026(19) 0.002(2) 0.0016(19) C4 0.034(3) 0.029(3) 0.030(3) 0.010(2) 0.014(2) 0.005(2) C9 0.022(2) 0.017(2) 0.040(3) -0.002(2) 0.006(2) -0.0036(19) C5 0.025(2) 0.018(2) 0.034(3) 0.009(2) 0.010(2) 0.003(2) C11 0.017(2) 0.017(2) 0.031(3) 0.003(2) 0.0046(19) 0.0004(18) C12 0.022(2) 0.022(3) 0.041(3) 0.008(2) 0.009(2) 0.003(2) C8 0.028(3) 0.025(3) 0.037(3) -0.008(2) 0.004(2) -0.004(2) C7 0.027(3) 0.022(2) 0.026(3) -0.003(2) 0.008(2) 0.001(2) C3 0.033(3) 0.022(2) 0.021(2) 0.001(2) 0.003(2) 0.004(2) C13 0.027(3) 0.019(3) 0.057(4) 0.007(2) 0.011(3) -0.010(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 C17 C18 1.398(7) . ? C17 C22 1.400(7) . ? C17 Pd2 1.961(5) . ? C27 C28 1.412(7) . ? C27 C26 1.433(7) . ? C27 C32 1.434(7) . ? C21 C22 1.381(7) . ? C21 C20 1.392(8) . ? C20 C19 1.392(8) . ? C22 N4 1.415(6) . ? C28 C29 1.371(8) . ? C15 C14 1.369(8) . ? C15 C16 1.402(7) . ? C14 C13 1.401(10) . ? C26 O3 1.239(6) . ? Pd2 N3 1.996(4) . ? Pd2 O4 2.005(4) . ? Pd2 O3 2.105(4) . ? O4 C32 1.301(6) . ? N3 C23 1.340(7) . ? N3 N4 1.358(6) . ? C25 N4 1.349(7) . ? C25 C24 1.378(8) . ? C18 C19 1.395(7) . ? C32 C31 1.421(7) . ? C23 C24 1.392(8) . ? C29 C30 1.385(9) . ? C31 C30 1.380(7) . ? Pd1 C1 1.967(5) . ? Pd1 N1 1.984(4) . ? Pd1 O2 1.992(3) . ? Pd1 O1 2.088(4) . ? O2 C16 1.308(6) . ? O1 C10 1.241(6) . ? N1 C7 1.346(7) . ? N1 N2 1.360(6) . ? N2 C9 1.352(7) . ? N2 C6 1.416(7) . ? C1 C2 1.388(7) . ? C1 C6 1.405(7) . ? C16 C11 1.437(7) . ? C6 C5 1.380(7) . ? C10 C11 1.412(7) . ? C2 C3 1.385(7) . ? C4 C5 1.386(8) . ? C4 C3 1.394(8) . ? C9 C8 1.365(8) . ? C11 C12 1.432(7) . ? C12 C13 1.357(9) . ? C8 C7 1.387(8) . ? 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 C18 C17 C22 117.3(4) . . ? C18 C17 Pd2 128.0(4) . . ? C22 C17 Pd2 114.7(4) . . ? C28 C27 C26 116.4(5) . . ? C28 C27 C32 119.5(5) . . ? C26 C27 C32 124.2(4) . . ? C22 C21 C20 117.8(5) . . ? C21 C20 C19 120.4(5) . . ? C21 C22 C17 123.6(5) . . ? C21 C22 N4 122.3(5) . . ? C17 C22 N4 114.1(4) . . ? C29 C28 C27 121.9(6) . . ? C14 C15 C16 121.9(6) . . ? C15 C14 C13 121.2(6) . . ? O3 C26 C27 129.2(5) . . ? C17 Pd2 N3 81.16(19) . . ? C17 Pd2 O4 91.72(17) . . ? N3 Pd2 O4 171.98(16) . . ? C17 Pd2 O3 175.23(17) . . ? N3 Pd2 O3 94.37(16) . . ? O4 Pd2 O3 92.63(14) . . ? C32 O4 Pd2 124.7(3) . . ? C26 O3 Pd2 122.3(3) . . ? C23 N3 N4 106.4(4) . . ? C23 N3 Pd2 139.2(4) . . ? N4 N3 Pd2 114.3(3) . . ? N4 C25 C24 107.4(5) . . ? C25 N4 N3 110.5(4) . . ? C25 N4 C22 133.9(4) . . ? N3 N4 C22 115.6(4) . . ? C19 C18 C17 120.1(5) . . ? O4 C32 C31 116.6(5) . . ? O4 C32 C27 126.6(5) . . ? C31 C32 C27 116.8(5) . . ? C20 C19 C18 120.7(5) . . ? N3 C23 C24 110.0(5) . . ? C28 C29 C30 118.9(5) . . ? C25 C24 C23 105.7(5) . . ? C30 C31 C32 121.4(5) . . ? C31 C30 C29 121.5(5) . . ? C1 Pd1 N1 80.91(19) . . ? C1 Pd1 O2 92.52(17) . . ? N1 Pd1 O2 172.61(16) . . ? C1 Pd1 O1 174.43(17) . . ? N1 Pd1 O1 93.63(16) . . ? O2 Pd1 O1 92.86(14) . . ? C16 O2 Pd1 125.3(3) . . ? C10 O1 Pd1 122.5(3) . . ? C7 N1 N2 106.2(4) . . ? C7 N1 Pd1 138.7(4) . . ? N2 N1 Pd1 114.7(3) . . ? C9 N2 N1 110.4(4) . . ? C9 N2 C6 133.6(5) . . ? N1 N2 C6 116.0(4) . . ? C2 C1 C6 116.4(5) . . ? C2 C1 Pd1 128.4(4) . . ? C6 C1 Pd1 115.1(4) . . ? O2 C16 C15 117.5(5) . . ? O2 C16 C11 125.0(5) . . ? C15 C16 C11 117.5(5) . . ? C5 C6 C1 124.1(5) . . ? C5 C6 N2 122.8(5) . . ? C1 C6 N2 113.1(4) . . ? O1 C10 C11 128.9(5) . . ? C3 C2 C1 120.7(5) . . ? C5 C4 C3 119.9(5) . . ? N2 C9 C8 107.2(5) . . ? C6 C5 C4 117.7(5) . . ? C10 C11 C12 116.1(5) . . ? C10 C11 C16 125.3(5) . . ? C12 C11 C16 118.6(5) . . ? C13 C12 C11 121.8(6) . . ? C9 C8 C7 106.7(5) . . ? N1 C7 C8 109.5(5) . . ? C2 C3 C4 121.1(5) . . ? C12 C13 C14 119.0(5) . . ? _diffrn_measured_fraction_theta_max 0.938 _diffrn_reflns_theta_full 0.50 _diffrn_measured_fraction_theta_full 0.000 _refine_diff_density_max 6.025 _refine_diff_density_min -0.864 _refine_diff_density_rms 0.183 #===END data_compound3 _database_code_depnum_ccdc_archive 'CCDC 783649' #TrackingRef '- crystaldata.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C14 H17 N3 Pd S2' _chemical_formula_sum 'C14 H17 N3 Pd S2' _chemical_formula_weight 397.83 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 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 8.8527(7) _cell_length_b 12.4569(10) _cell_length_c 13.7577(11) _cell_angle_alpha 90.00 _cell_angle_beta 95.1880(10) _cell_angle_gamma 90.00 _cell_volume 1510.9(2) _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 0.33 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.749 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 800 _exptl_absorpt_coefficient_mu 1.497 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.6379 _exptl_absorpt_correction_T_max 0.8526 _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 18234 _diffrn_reflns_av_R_equivalents 0.0206 _diffrn_reflns_av_sigmaI/netI 0.0158 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.21 _diffrn_reflns_theta_max 28.61 _reflns_number_total 3674 _reflns_number_gt 3650 _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^)+(0.0352P)^2^+4.8446P] 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 3674 _refine_ls_number_parameters 181 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0338 _refine_ls_R_factor_gt 0.0336 _refine_ls_wR_factor_ref 0.0816 _refine_ls_wR_factor_gt 0.0814 _refine_ls_goodness_of_fit_ref 1.118 _refine_ls_restrained_S_all 1.118 _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 C14 C 0.1994(4) 1.0819(3) 0.4710(2) 0.0238(6) Uani 1 1 d . . . H14A H 0.1277 1.1113 0.5144 0.036 Uiso 1 1 calc R . . H14B H 0.3033 1.0995 0.4969 0.036 Uiso 1 1 calc R . . H14C H 0.1877 1.0038 0.4671 0.036 Uiso 1 1 calc R . . C13 C 0.1678(3) 1.1302(2) 0.3700(2) 0.0186(6) Uani 1 1 d . . . H13A H 0.0621 1.1135 0.3449 0.022 Uiso 1 1 calc R . . H13B H 0.1775 1.2093 0.3747 0.022 Uiso 1 1 calc R . . Pd1 Pd 0.10830(2) 0.902971(16) 0.067490(14) 0.01191(8) Uani 1 1 d . . . S2 S 0.34029(8) 0.97452(6) 0.14450(5) 0.01449(14) Uani 1 1 d . . . S1 S 0.04390(8) 0.96974(6) 0.21328(5) 0.01488(14) Uani 1 1 d . . . N1 N 0.1645(3) 0.83989(19) -0.06167(17) 0.0135(4) Uani 1 1 d . . . N3 N 0.2717(3) 1.08981(19) 0.30058(17) 0.0142(5) Uani 1 1 d . . . C1 C -0.0923(3) 0.8386(2) 0.0198(2) 0.0142(5) Uani 1 1 d . . . N2 N 0.0511(3) 0.78067(19) -0.10917(17) 0.0139(4) Uani 1 1 d . . . C10 C 0.2253(3) 1.0203(2) 0.23085(19) 0.0130(5) Uani 1 1 d . . . C12 C 0.5429(3) 1.0639(3) 0.3647(2) 0.0225(6) Uani 1 1 d . . . H12A H 0.6431 1.0976 0.3662 0.034 Uiso 1 1 calc R . . H12B H 0.5461 0.9933 0.3335 0.034 Uiso 1 1 calc R . . H12C H 0.5146 1.0554 0.4315 0.034 Uiso 1 1 calc R . . C9 C 0.0970(3) 0.7385(2) -0.1926(2) 0.0157(5) Uani 1 1 d . . . H9 H 0.0386 0.6946 -0.2383 0.019 Uiso 1 1 calc R . . C2 C -0.2298(3) 0.8416(2) 0.0616(2) 0.0169(5) Uani 1 1 d . . . H2 H -0.2370 0.8818 0.1197 0.020 Uiso 1 1 calc R . . C5 C -0.2139(3) 0.7242(2) -0.1102(2) 0.0163(5) Uani 1 1 d . . . H5 H -0.2076 0.6848 -0.1688 0.020 Uiso 1 1 calc R . . C11 C 0.4263(3) 1.1343(2) 0.3069(2) 0.0173(5) Uani 1 1 d . . . H11A H 0.4257 1.2060 0.3380 0.021 Uiso 1 1 calc R . . H11B H 0.4571 1.1440 0.2400 0.021 Uiso 1 1 calc R . . C3 C -0.3575(3) 0.7865(2) 0.0198(2) 0.0181(5) Uani 1 1 d . . . H3 H -0.4501 0.7890 0.0498 0.022 Uiso 1 1 calc R . . C8 C 0.2439(3) 0.7714(2) -0.1984(2) 0.0191(6) Uani 1 1 d . . . H8 H 0.3076 0.7543 -0.2482 0.023 Uiso 1 1 calc R . . C4 C -0.3484(3) 0.7286(2) -0.0652(2) 0.0182(6) Uani 1 1 d . . . H4 H -0.4352 0.6912 -0.0933 0.022 Uiso 1 1 calc R . . C6 C -0.0891(3) 0.7794(2) -0.06654(19) 0.0147(5) Uani 1 1 d . . . C7 C 0.2809(3) 0.8353(2) -0.1157(2) 0.0178(5) Uani 1 1 d . . . H7 H 0.3756 0.8702 -0.1007 0.021 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 C14 0.0309(17) 0.0248(15) 0.0162(14) -0.0004(12) 0.0043(12) 0.0076(13) C13 0.0214(14) 0.0181(13) 0.0161(13) -0.0053(11) 0.0005(11) 0.0059(11) Pd1 0.01368(11) 0.01060(12) 0.01088(11) -0.00013(7) -0.00202(7) -0.00077(7) S2 0.0158(3) 0.0154(3) 0.0120(3) -0.0021(2) -0.0002(2) -0.0002(2) S1 0.0144(3) 0.0157(3) 0.0142(3) -0.0004(2) -0.0003(2) -0.0014(2) N1 0.0134(10) 0.0140(11) 0.0124(10) -0.0010(8) -0.0026(8) -0.0011(9) N3 0.0159(11) 0.0140(11) 0.0122(11) -0.0024(8) -0.0016(9) 0.0021(9) C1 0.0171(12) 0.0120(12) 0.0125(12) 0.0031(10) -0.0036(10) -0.0012(10) N2 0.0141(11) 0.0131(11) 0.0137(10) -0.0015(9) -0.0034(8) -0.0010(9) C10 0.0164(12) 0.0111(12) 0.0109(12) 0.0022(9) -0.0013(9) -0.0005(10) C12 0.0177(14) 0.0236(15) 0.0251(15) 0.0043(12) -0.0047(11) -0.0005(12) C9 0.0172(13) 0.0161(13) 0.0134(12) -0.0006(10) -0.0013(10) -0.0001(10) C2 0.0213(14) 0.0162(13) 0.0127(12) 0.0034(10) -0.0007(10) 0.0003(11) C5 0.0179(13) 0.0141(13) 0.0159(12) 0.0001(10) -0.0028(10) -0.0020(10) C11 0.0182(13) 0.0139(13) 0.0188(13) -0.0011(10) -0.0027(10) -0.0026(11) C3 0.0168(13) 0.0198(14) 0.0177(13) 0.0046(11) 0.0017(10) -0.0012(11) C8 0.0194(14) 0.0196(14) 0.0182(13) -0.0038(11) 0.0013(11) -0.0002(11) C4 0.0155(13) 0.0183(14) 0.0204(14) 0.0053(11) -0.0013(10) -0.0029(11) C6 0.0167(12) 0.0133(13) 0.0134(12) 0.0031(10) -0.0015(10) 0.0013(10) C7 0.0161(13) 0.0188(14) 0.0179(13) -0.0019(11) -0.0010(10) -0.0013(11) _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 C14 C13 1.517(4) . ? C13 N3 1.473(4) . ? Pd1 C1 2.004(3) . ? Pd1 N1 2.045(2) . ? Pd1 S1 2.2906(7) . ? Pd1 S2 2.3961(7) . ? S2 C10 1.730(3) . ? S1 C10 1.722(3) . ? N1 C7 1.326(4) . ? N1 N2 1.364(3) . ? N3 C10 1.329(3) . ? N3 C11 1.472(4) . ? C1 C2 1.393(4) . ? C1 C6 1.401(4) . ? N2 C9 1.358(4) . ? N2 C6 1.420(4) . ? C12 C11 1.523(4) . ? C9 C8 1.373(4) . ? C2 C3 1.401(4) . ? C5 C6 1.391(4) . ? C5 C4 1.392(4) . ? C3 C4 1.383(4) . ? C8 C7 1.402(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 C13 C14 112.6(2) . . ? C1 Pd1 N1 80.77(10) . . ? C1 Pd1 S1 98.55(8) . . ? N1 Pd1 S1 178.68(7) . . ? C1 Pd1 S2 172.88(8) . . ? N1 Pd1 S2 105.14(7) . . ? S1 Pd1 S2 75.46(2) . . ? C10 S2 Pd1 83.82(9) . . ? C10 S1 Pd1 87.30(9) . . ? C7 N1 N2 106.5(2) . . ? C7 N1 Pd1 140.0(2) . . ? N2 N1 Pd1 113.46(17) . . ? C10 N3 C11 120.8(2) . . ? C10 N3 C13 121.4(2) . . ? C11 N3 C13 117.7(2) . . ? C2 C1 C6 116.8(3) . . ? C2 C1 Pd1 129.4(2) . . ? C6 C1 Pd1 113.8(2) . . ? C9 N2 N1 110.6(2) . . ? C9 N2 C6 133.2(2) . . ? N1 N2 C6 116.2(2) . . ? N3 C10 S1 124.2(2) . . ? N3 C10 S2 123.2(2) . . ? S1 C10 S2 112.46(15) . . ? N2 C9 C8 106.9(2) . . ? C1 C2 C3 121.3(3) . . ? C6 C5 C4 117.8(3) . . ? N3 C11 C12 113.4(2) . . ? C4 C3 C2 119.7(3) . . ? C9 C8 C7 106.0(3) . . ? C3 C4 C5 121.0(3) . . ? C5 C6 C1 123.4(3) . . ? C5 C6 N2 121.1(3) . . ? C1 C6 N2 115.4(2) . . ? N1 C7 C8 110.1(3) . . ? _diffrn_measured_fraction_theta_max 0.949 _diffrn_reflns_theta_full 0.50 _diffrn_measured_fraction_theta_full 0.000 _refine_diff_density_max 3.651 _refine_diff_density_min -0.957 _refine_diff_density_rms 0.135 #===END data_compound4 _database_code_depnum_ccdc_archive 'CCDC 783650' #TrackingRef '- crystaldata.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H24 N8 PD2 S2' _chemical_formula_sum 'C26 H24 N8 Pd2 S2' _chemical_formula_weight 725.45 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' 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 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 11.1797(5) _cell_length_b 17.5215(7) _cell_length_c 26.8062(11) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5250.9(4) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour pale-yellow _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.835 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2880 _exptl_absorpt_coefficient_mu 1.562 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.7556 _exptl_absorpt_correction_T_max 0.9121 _exptl_absorpt_process_details ? _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 57537 _diffrn_reflns_av_R_equivalents 0.0385 _diffrn_reflns_av_sigmaI/netI 0.0226 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 2.29 _diffrn_reflns_theta_max 28.17 _reflns_number_total 6240 _reflns_number_gt 5927 _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^)+(0.0357P)^2^+15.2285P] 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 6240 _refine_ls_number_parameters 343 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0451 _refine_ls_R_factor_gt 0.0419 _refine_ls_wR_factor_ref 0.0915 _refine_ls_wR_factor_gt 0.0901 _refine_ls_goodness_of_fit_ref 1.209 _refine_ls_restrained_S_all 1.209 _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 N8 N 0.9204(3) 0.25112(17) 0.44575(11) 0.0178(6) Uani 1 1 d . . . C25 C 1.0246(3) 0.2372(2) 0.41952(15) 0.0242(8) Uani 1 1 d . . . H25 H 1.0987 0.2632 0.4227 0.029 Uiso 1 1 calc R . . C15 C 0.4586(3) 0.2346(2) 0.38751(14) 0.0221(8) Uani 1 1 d . . . H15 H 0.5129 0.2674 0.4043 0.027 Uiso 1 1 calc R . . C24 C 0.9989(3) 0.1784(2) 0.38813(14) 0.0227(8) Uani 1 1 d . . . H24 H 1.0539 0.1560 0.3654 0.027 Uiso 1 1 calc R . . C18 C 0.3012(3) 0.1426(2) 0.33603(14) 0.0238(8) Uani 1 1 d . . . H18 H 0.2478 0.1106 0.3181 0.029 Uiso 1 1 calc R . . C17 C 0.2839(4) 0.2208(3) 0.33713(16) 0.0301(9) Uani 1 1 d . . . H17 H 0.2184 0.2429 0.3198 0.036 Uiso 1 1 calc R . . C16 C 0.3613(4) 0.2660(2) 0.36315(15) 0.0272(9) Uani 1 1 d . . . H16 H 0.3482 0.3195 0.3646 0.033 Uiso 1 1 calc R . . C13 C 0.9753(3) -0.1037(2) 0.48526(14) 0.0211(8) Uani 1 1 d . . . H13A H 0.9915 -0.1228 0.5190 0.032 Uiso 1 1 calc R . . H13B H 1.0445 -0.0747 0.4733 0.032 Uiso 1 1 calc R . . H13C H 0.9604 -0.1469 0.4628 0.032 Uiso 1 1 calc R . . C26 C 0.9018(4) 0.3082(2) 0.48437(15) 0.0255(8) Uani 1 1 d . . . H26A H 0.9756 0.3375 0.4892 0.038 Uiso 1 1 calc R . . H26B H 0.8801 0.2829 0.5157 0.038 Uiso 1 1 calc R . . H26C H 0.8373 0.3428 0.4743 0.038 Uiso 1 1 calc R . . Pd1 Pd 0.79598(2) 0.077179(14) 0.346284(9) 0.01238(8) Uani 1 1 d . . . Pd2 Pd 0.60610(2) 0.094481(15) 0.422511(10) 0.01403(8) Uani 1 1 d . . . S1 S 0.87758(8) -0.02582(5) 0.38704(3) 0.01922(19) Uani 1 1 d . . . S2 S 0.69383(8) 0.20168(5) 0.45515(4) 0.0219(2) Uani 1 1 d . . . N1 N 0.7110(3) 0.16002(17) 0.30611(11) 0.0161(6) Uani 1 1 d . . . C6 C 0.6318(3) 0.0518(2) 0.26623(13) 0.0154(7) Uani 1 1 d . . . N7 N 0.8823(3) 0.15613(18) 0.39407(11) 0.0183(6) Uani 1 1 d . . . C14 C 0.4793(3) 0.1561(2) 0.38816(13) 0.0164(7) Uani 1 1 d . . . N5 N 0.5129(3) 0.00797(17) 0.39039(11) 0.0175(6) Uani 1 1 d . . . N4 N 0.8700(3) -0.05413(17) 0.48629(11) 0.0169(6) Uani 1 1 d . . . C19 C 0.3976(3) 0.1116(2) 0.36149(13) 0.0179(7) Uani 1 1 d . . . C1 C 0.7132(3) 0.0113(2) 0.29613(13) 0.0152(7) Uani 1 1 d . . . C12 C 0.8018(4) -0.0382(2) 0.52798(14) 0.0235(8) Uani 1 1 d . . . H12 H 0.8144 -0.0569 0.5608 0.028 Uiso 1 1 calc R . . C3 C 0.6553(3) -0.1018(2) 0.24921(14) 0.0202(7) Uani 1 1 d . . . H3 H 0.6643 -0.1549 0.2432 0.024 Uiso 1 1 calc R . . C4 C 0.5748(3) -0.0593(2) 0.22060(14) 0.0222(8) Uani 1 1 d . . . H4 H 0.5289 -0.0835 0.1954 0.027 Uiso 1 1 calc R . . C5 C 0.5622(3) 0.0183(2) 0.22905(13) 0.0195(7) Uani 1 1 d . . . H5 H 0.5075 0.0478 0.2100 0.023 Uiso 1 1 calc R . . N3 N 0.7251(3) 0.02218(17) 0.46202(11) 0.0163(6) Uani 1 1 d . . . C20 C 0.5226(4) -0.0669(2) 0.38310(15) 0.0241(8) Uani 1 1 d . . . H20 H 0.5813 -0.0988 0.3980 0.029 Uiso 1 1 calc R . . N2 N 0.6271(3) 0.13138(17) 0.27434(11) 0.0157(6) Uani 1 1 d . . . C23 C 0.8362(3) 0.2009(2) 0.42982(13) 0.0166(7) Uani 1 1 d . . . C11 C 0.7138(3) 0.0092(2) 0.51291(14) 0.0234(8) Uani 1 1 d . . . H11 H 0.6537 0.0304 0.5338 0.028 Uiso 1 1 calc R . . N6 N 0.4189(3) 0.03196(19) 0.36190(11) 0.0197(6) Uani 1 1 d . . . C2 C 0.7222(3) -0.0668(2) 0.28656(13) 0.0178(7) Uani 1 1 d . . . H2 H 0.7754 -0.0968 0.3060 0.021 Uiso 1 1 calc R . . C9 C 0.5583(3) 0.1885(2) 0.25605(14) 0.0215(8) Uani 1 1 d . . . H9 H 0.4934 0.1831 0.2334 0.026 Uiso 1 1 calc R . . C8 C 0.5995(3) 0.2557(2) 0.27624(14) 0.0222(8) Uani 1 1 d . . . H8 H 0.5698 0.3057 0.2703 0.027 Uiso 1 1 calc R . . C10 C 0.8204(3) -0.0174(2) 0.44697(13) 0.0155(7) Uani 1 1 d . . . C22 C 0.3690(4) -0.0270(2) 0.33701(15) 0.0281(9) Uani 1 1 d . . . H22 H 0.3028 -0.0246 0.3148 0.034 Uiso 1 1 calc R . . C21 C 0.4329(4) -0.0917(2) 0.35008(17) 0.0315(10) Uani 1 1 d . . . H21 H 0.4190 -0.1424 0.3390 0.038 Uiso 1 1 calc R . . C7 C 0.6941(3) 0.2350(2) 0.30733(14) 0.0192(7) Uani 1 1 d . . . H7 H 0.7401 0.2697 0.3267 0.023 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 N8 0.0206(14) 0.0160(14) 0.0167(14) -0.0013(11) -0.0051(12) -0.0027(12) C25 0.0187(18) 0.027(2) 0.0266(19) 0.0041(16) -0.0015(15) -0.0029(15) C15 0.0218(18) 0.0235(19) 0.0211(18) 0.0019(15) 0.0023(15) 0.0008(15) C24 0.0217(18) 0.026(2) 0.0207(18) 0.0000(15) 0.0006(15) 0.0002(15) C18 0.0170(18) 0.036(2) 0.0186(18) 0.0032(16) -0.0033(14) -0.0020(16) C17 0.023(2) 0.039(2) 0.028(2) 0.0098(18) -0.0005(17) 0.0037(18) C16 0.028(2) 0.028(2) 0.026(2) 0.0081(16) 0.0043(17) 0.0088(17) C13 0.0211(18) 0.0185(18) 0.0236(18) 0.0031(14) -0.0067(15) 0.0049(14) C26 0.033(2) 0.0210(19) 0.0224(19) -0.0077(15) -0.0040(16) -0.0028(16) Pd1 0.01232(13) 0.01298(13) 0.01184(13) -0.00047(9) -0.00089(9) 0.00062(9) Pd2 0.01254(13) 0.01590(14) 0.01364(13) -0.00160(9) -0.00042(10) 0.00170(9) S1 0.0231(4) 0.0212(4) 0.0134(4) 0.0010(3) 0.0004(3) 0.0089(3) S2 0.0159(4) 0.0234(5) 0.0263(5) -0.0093(4) -0.0015(4) 0.0016(3) N1 0.0157(14) 0.0170(14) 0.0154(14) 0.0007(11) -0.0009(11) -0.0006(11) C6 0.0145(16) 0.0171(17) 0.0146(16) 0.0004(13) 0.0040(13) -0.0024(13) N7 0.0199(15) 0.0184(15) 0.0166(14) 0.0000(12) -0.0060(12) -0.0001(12) C14 0.0122(15) 0.0237(18) 0.0132(15) 0.0022(13) 0.0024(13) 0.0033(13) N5 0.0158(14) 0.0204(15) 0.0161(14) 0.0003(12) 0.0028(12) -0.0017(12) N4 0.0187(15) 0.0144(14) 0.0176(14) 0.0006(11) -0.0027(12) 0.0020(11) C19 0.0149(16) 0.0242(18) 0.0147(16) 0.0021(14) 0.0030(13) 0.0012(14) C1 0.0139(15) 0.0177(17) 0.0140(15) -0.0001(13) 0.0016(13) -0.0012(13) C12 0.032(2) 0.0231(19) 0.0154(17) 0.0040(14) 0.0020(15) 0.0014(16) C3 0.0249(19) 0.0143(16) 0.0214(18) -0.0009(14) 0.0011(15) -0.0028(14) C4 0.0219(18) 0.0250(19) 0.0197(18) -0.0005(15) -0.0017(15) -0.0076(15) C5 0.0171(16) 0.0246(19) 0.0168(17) 0.0028(14) -0.0021(14) -0.0026(14) N3 0.0159(14) 0.0195(15) 0.0135(13) 0.0005(11) 0.0005(11) 0.0024(11) C20 0.030(2) 0.0186(18) 0.0240(19) 0.0023(15) 0.0034(16) -0.0031(15) N2 0.0168(14) 0.0163(14) 0.0139(14) 0.0006(11) -0.0011(11) 0.0010(11) C23 0.0163(16) 0.0151(16) 0.0184(17) 0.0006(13) -0.0056(14) 0.0002(13) C11 0.0228(19) 0.026(2) 0.0219(19) 0.0005(15) 0.0051(15) 0.0022(15) N6 0.0152(14) 0.0274(17) 0.0167(14) 0.0006(13) 0.0003(12) -0.0033(12) C2 0.0170(17) 0.0181(17) 0.0182(17) 0.0014(13) 0.0015(14) 0.0012(13) C9 0.0211(18) 0.0266(19) 0.0167(17) 0.0019(15) 0.0013(14) 0.0072(15) C8 0.0277(19) 0.0173(17) 0.0216(18) 0.0027(14) 0.0023(15) 0.0065(15) C10 0.0145(15) 0.0160(16) 0.0160(16) -0.0004(13) -0.0049(13) -0.0012(13) C22 0.026(2) 0.033(2) 0.025(2) -0.0037(17) -0.0021(16) -0.0095(17) C21 0.035(2) 0.024(2) 0.035(2) -0.0038(17) 0.0045(19) -0.0080(18) C7 0.0219(18) 0.0150(17) 0.0206(18) 0.0029(13) 0.0025(15) -0.0009(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N8 C23 1.357(4) . ? N8 C25 1.383(5) . ? N8 C26 1.455(5) . ? C25 C24 1.361(6) . ? C15 C16 1.383(5) . ? C15 C14 1.395(5) . ? C24 N7 1.370(5) . ? C18 C17 1.385(6) . ? C18 C19 1.386(5) . ? C17 C16 1.364(6) . ? C13 N4 1.464(4) . ? Pd1 C1 1.999(3) . ? Pd1 N1 2.042(3) . ? Pd1 N7 2.118(3) . ? Pd1 S1 2.2985(9) . ? Pd1 Pd2 2.9621(4) . ? Pd2 C14 2.006(3) . ? Pd2 N5 2.031(3) . ? Pd2 N3 2.121(3) . ? Pd2 S2 2.2925(10) . ? S1 C10 1.735(4) . ? S2 C23 1.731(4) . ? N1 C7 1.328(5) . ? N1 N2 1.363(4) . ? C6 C5 1.395(5) . ? C6 C1 1.405(5) . ? C6 N2 1.413(5) . ? N7 C23 1.341(5) . ? C14 C19 1.397(5) . ? N5 C20 1.330(5) . ? N5 N6 1.366(4) . ? N4 C10 1.354(4) . ? N4 C12 1.381(5) . ? C19 N6 1.415(5) . ? C1 C2 1.395(5) . ? C12 C11 1.349(5) . ? C3 C2 1.393(5) . ? C3 C4 1.397(5) . ? C4 C5 1.385(5) . ? N3 C10 1.334(4) . ? N3 C11 1.389(5) . ? C20 C21 1.406(6) . ? N2 C9 1.354(5) . ? N6 C22 1.350(5) . ? C9 C8 1.376(6) . ? C8 C7 1.395(5) . ? C22 C21 1.384(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C23 N8 C25 108.0(3) . . ? C23 N8 C26 124.8(3) . . ? C25 N8 C26 127.1(3) . . ? C24 C25 N8 105.7(3) . . ? C16 C15 C14 121.9(4) . . ? C25 C24 N7 110.1(3) . . ? C17 C18 C19 119.1(4) . . ? C16 C17 C18 119.8(4) . . ? C17 C16 C15 120.6(4) . . ? C1 Pd1 N1 80.84(13) . . ? C1 Pd1 N7 174.18(13) . . ? N1 Pd1 N7 93.82(12) . . ? C1 Pd1 S1 92.85(10) . . ? N1 Pd1 S1 173.49(9) . . ? N7 Pd1 S1 92.55(8) . . ? C1 Pd1 Pd2 101.04(10) . . ? N1 Pd1 Pd2 87.57(8) . . ? N7 Pd1 Pd2 80.93(9) . . ? S1 Pd1 Pd2 92.11(2) . . ? C14 Pd2 N5 81.03(14) . . ? C14 Pd2 N3 173.86(13) . . ? N5 Pd2 N3 95.05(12) . . ? C14 Pd2 S2 92.11(11) . . ? N5 Pd2 S2 173.12(9) . . ? N3 Pd2 S2 91.74(9) . . ? C14 Pd2 Pd1 104.19(10) . . ? N5 Pd2 Pd1 89.94(8) . . ? N3 Pd2 Pd1 80.43(8) . . ? S2 Pd2 Pd1 92.32(3) . . ? C10 S1 Pd1 103.12(12) . . ? C23 S2 Pd2 103.74(12) . . ? C7 N1 N2 106.4(3) . . ? C7 N1 Pd1 139.2(3) . . ? N2 N1 Pd1 112.8(2) . . ? C5 C6 C1 123.8(3) . . ? C5 C6 N2 120.3(3) . . ? C1 C6 N2 115.8(3) . . ? C23 N7 C24 106.4(3) . . ? C23 N7 Pd1 129.7(2) . . ? C24 N7 Pd1 123.3(3) . . ? C15 C14 C19 115.8(3) . . ? C15 C14 Pd2 130.8(3) . . ? C19 C14 Pd2 113.4(3) . . ? C20 N5 N6 106.5(3) . . ? C20 N5 Pd2 139.1(3) . . ? N6 N5 Pd2 113.7(2) . . ? C10 N4 C12 107.9(3) . . ? C10 N4 C13 126.6(3) . . ? C12 N4 C13 125.4(3) . . ? C18 C19 C14 122.8(4) . . ? C18 C19 N6 121.4(3) . . ? C14 C19 N6 115.9(3) . . ? C2 C1 C6 115.9(3) . . ? C2 C1 Pd1 131.0(3) . . ? C6 C1 Pd1 113.0(3) . . ? C11 C12 N4 106.5(3) . . ? C2 C3 C4 120.4(3) . . ? C5 C4 C3 119.9(3) . . ? C4 C5 C6 118.2(3) . . ? C10 N3 C11 106.6(3) . . ? C10 N3 Pd2 131.3(2) . . ? C11 N3 Pd2 122.1(2) . . ? N5 C20 C21 109.8(4) . . ? C9 N2 N1 110.2(3) . . ? C9 N2 C6 134.0(3) . . ? N1 N2 C6 115.7(3) . . ? N7 C23 N8 109.8(3) . . ? N7 C23 S2 129.6(3) . . ? N8 C23 S2 120.6(3) . . ? C12 C11 N3 109.2(3) . . ? C22 N6 N5 111.0(3) . . ? C22 N6 C19 132.9(3) . . ? N5 N6 C19 115.9(3) . . ? C3 C2 C1 121.7(3) . . ? N2 C9 C8 107.4(3) . . ? C9 C8 C7 105.5(3) . . ? N3 C10 N4 109.8(3) . . ? N3 C10 S1 128.2(3) . . ? N4 C10 S1 122.0(3) . . ? N6 C22 C21 106.7(4) . . ? C22 C21 C20 105.9(4) . . ? N1 C7 C8 110.5(3) . . ? _diffrn_measured_fraction_theta_max 0.967 _diffrn_reflns_theta_full 0.50 _diffrn_measured_fraction_theta_full 0.000 _refine_diff_density_max 1.325 _refine_diff_density_min -0.597 _refine_diff_density_rms 0.121 #===END data_compound5 _database_code_depnum_ccdc_archive 'CCDC 783651' #TrackingRef '- crystaldata.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H22 N6 O4 PD2, C H2 CL2' _chemical_formula_sum 'C27 H24 Cl2 N6 O4 Pd2' _chemical_formula_weight 780.22 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.9145(4) _cell_length_b 10.8879(4) _cell_length_c 15.3871(8) _cell_angle_alpha 103.0790(10) _cell_angle_beta 90.5410(10) _cell_angle_gamma 107.2350(10) _cell_volume 1384.71(11) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.871 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 772 _exptl_absorpt_coefficient_mu 1.538 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.7383 _exptl_absorpt_correction_T_max 0.8369 _exptl_absorpt_process_details ? _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 15980 _diffrn_reflns_av_R_equivalents 0.0178 _diffrn_reflns_av_sigmaI/netI 0.0227 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.36 _diffrn_reflns_theta_max 28.23 _reflns_number_total 6209 _reflns_number_gt 5829 _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^)+(0.0458P)^2^+5.8219P] 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 6209 _refine_ls_number_parameters 370 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0368 _refine_ls_R_factor_gt 0.0343 _refine_ls_wR_factor_ref 0.0876 _refine_ls_wR_factor_gt 0.0856 _refine_ls_goodness_of_fit_ref 0.911 _refine_ls_restrained_S_all 0.911 _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 0.52728(3) 0.68651(2) 0.367743(16) 0.01821(7) Uani 1 1 d . . . Pd2 Pd 0.46555(3) 0.68256(2) 0.180884(17) 0.02068(8) Uani 1 1 d . . . O2 O 0.7179(3) 0.8543(2) 0.35037(18) 0.0269(5) Uani 1 1 d . . . N4 N 0.3095(3) 0.5019(3) 0.14883(19) 0.0233(6) Uani 1 1 d . . . O1 O 0.2962(3) 0.7752(2) 0.23954(17) 0.0268(5) Uani 1 1 d . . . O3 O 0.4059(3) 0.8629(3) 0.54139(18) 0.0302(6) Uani 1 1 d . . . N3 N 0.3773(3) 0.7979(3) 0.38680(19) 0.0213(5) Uani 1 1 d . . . N1 N 0.6596(3) 0.5634(3) 0.34838(18) 0.0186(5) Uani 1 1 d . . . N2 N 0.5886(3) 0.4432(3) 0.36460(18) 0.0180(5) Uani 1 1 d . . . N6 N 0.6364(4) 0.8600(3) 0.2098(2) 0.0248(6) Uani 1 1 d . . . C6 C 0.4323(4) 0.4224(3) 0.3908(2) 0.0174(6) Uani 1 1 d . . . C14 C 0.6062(4) 0.5837(3) 0.1248(2) 0.0212(6) Uani 1 1 d . . . N5 N 0.3683(3) 0.4052(3) 0.10580(19) 0.0234(6) Uani 1 1 d . . . C7 C 0.7986(4) 0.5596(3) 0.3193(2) 0.0222(6) Uani 1 1 d . . . H7 H 0.8738 0.6304 0.3021 0.027 Uiso 1 1 calc R . . C8 C 0.8181(4) 0.4363(3) 0.3176(2) 0.0232(7) Uani 1 1 d . . . H8 H 0.9065 0.4079 0.2998 0.028 Uiso 1 1 calc R . . C1 C 0.3734(4) 0.5298(3) 0.3942(2) 0.0185(6) Uani 1 1 d . . . C10 C 0.2934(4) 0.8187(3) 0.3210(2) 0.0239(7) Uani 1 1 d . . . C2 C 0.2191(4) 0.5116(3) 0.4183(2) 0.0217(6) Uani 1 1 d . . . H2 H 0.1732 0.5805 0.4205 0.026 Uiso 1 1 calc R . . C13 C 0.3446(4) 0.8627(3) 0.4701(2) 0.0253(7) Uani 1 1 d . . . O4 O 0.6300(4) 0.9238(3) 0.0780(2) 0.0431(7) Uani 1 1 d . . . C5 C 0.3484(4) 0.3058(3) 0.4120(2) 0.0210(6) Uani 1 1 d . . . H5 H 0.3938 0.2366 0.4100 0.025 Uiso 1 1 calc R . . C15 C 0.7658(4) 0.6289(4) 0.1143(2) 0.0254(7) Uani 1 1 d . . . H15 H 0.8206 0.7209 0.1332 0.030 Uiso 1 1 calc R . . C18 C 0.6100(5) 0.3575(4) 0.0573(2) 0.0291(7) Uani 1 1 d . . . H18 H 0.5557 0.2654 0.0380 0.035 Uiso 1 1 calc R . . C9 C 0.6820(4) 0.3645(3) 0.3472(2) 0.0220(6) Uani 1 1 d . . . H9 H 0.6584 0.2764 0.3540 0.026 Uiso 1 1 calc R . . C11 C 0.1923(4) 0.9052(4) 0.3579(3) 0.0270(7) Uani 1 1 d . . . H11A H 0.2247 0.9893 0.3385 0.032 Uiso 1 1 calc R . . H11B H 0.0796 0.8590 0.3384 0.032 Uiso 1 1 calc R . . C4 C 0.1961(4) 0.2927(3) 0.4362(2) 0.0231(7) Uani 1 1 d . . . H4 H 0.1355 0.2134 0.4509 0.028 Uiso 1 1 calc R . . C19 C 0.5319(4) 0.4470(3) 0.0948(2) 0.0224(6) Uani 1 1 d . . . C17 C 0.7714(5) 0.4074(4) 0.0490(3) 0.0320(8) Uani 1 1 d . . . H17 H 0.8289 0.3488 0.0243 0.038 Uiso 1 1 calc R . . C3 C 0.1316(4) 0.3950(3) 0.4390(2) 0.0230(7) Uani 1 1 d . . . H3 H 0.0269 0.3850 0.4553 0.028 Uiso 1 1 calc R . . C24 C 0.8410(4) 1.0455(3) 0.2930(3) 0.0298(8) Uani 1 1 d . . . H24A H 0.8192 1.1135 0.3415 0.036 Uiso 1 1 calc R . . H24B H 0.9507 1.0454 0.3035 0.036 Uiso 1 1 calc R . . C20 C 0.1570(4) 0.4439(4) 0.1533(3) 0.0290(7) Uani 1 1 d . . . H20 H 0.0855 0.4876 0.1805 0.035 Uiso 1 1 calc R . . C22 C 0.2533(5) 0.2877(4) 0.0822(3) 0.0307(8) Uani 1 1 d . . . H22 H 0.2645 0.2055 0.0508 0.037 Uiso 1 1 calc R . . C23 C 0.7247(4) 0.9095(3) 0.2879(3) 0.0265(7) Uani 1 1 d . . . C16 C 0.8472(4) 0.5415(4) 0.0766(3) 0.0304(8) Uani 1 1 d . . . H16 H 0.9566 0.5748 0.0697 0.036 Uiso 1 1 calc R . . C21 C 0.1178(5) 0.3099(4) 0.1121(3) 0.0351(9) Uani 1 1 d . . . H21 H 0.0166 0.2462 0.1059 0.042 Uiso 1 1 calc R . . C12 C 0.2220(5) 0.9302(4) 0.4584(3) 0.0316(8) Uani 1 1 d . . . H12A H 0.1242 0.8914 0.4854 0.038 Uiso 1 1 calc R . . H12B H 0.2624 1.0264 0.4863 0.038 Uiso 1 1 calc R . . C25 C 0.8140(5) 1.0703(4) 0.2031(3) 0.0407(10) Uani 1 1 d . . . H25A H 0.9111 1.0822 0.1710 0.049 Uiso 1 1 calc R . . H25B H 0.7791 1.1498 0.2090 0.049 Uiso 1 1 calc R . . C26 C 0.6855(5) 0.9461(4) 0.1551(3) 0.0347(8) Uani 1 1 d . . . Cl1 Cl 0.40085(15) 1.09763(11) 0.19351(7) 0.0461(3) Uani 1 1 d . . . Cl2 Cl 0.10776(15) 0.92766(13) 0.09176(10) 0.0572(3) Uani 1 1 d . . . C27 C 0.3111(5) 0.9585(4) 0.1035(3) 0.0383(9) Uani 1 1 d . . . H27A H 0.3565 0.9752 0.0472 0.046 Uiso 1 1 calc R . . H27B H 0.3341 0.8795 0.1145 0.046 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 0.01781(13) 0.01497(12) 0.02496(13) 0.00808(9) 0.00596(9) 0.00704(9) Pd2 0.02219(13) 0.01878(13) 0.02415(14) 0.00819(10) 0.00642(9) 0.00844(10) O2 0.0247(12) 0.0196(11) 0.0382(14) 0.0116(10) 0.0080(10) 0.0060(9) N4 0.0229(14) 0.0249(14) 0.0246(14) 0.0093(11) 0.0054(11) 0.0086(11) O1 0.0297(13) 0.0262(12) 0.0309(13) 0.0095(10) 0.0065(10) 0.0158(10) O3 0.0385(14) 0.0284(13) 0.0319(14) 0.0138(11) 0.0094(11) 0.0174(11) N3 0.0225(13) 0.0165(12) 0.0286(14) 0.0094(11) 0.0091(11) 0.0082(10) N1 0.0200(13) 0.0161(12) 0.0216(13) 0.0078(10) 0.0040(10) 0.0059(10) N2 0.0174(12) 0.0174(12) 0.0218(13) 0.0079(10) 0.0048(10) 0.0066(10) N6 0.0295(15) 0.0169(13) 0.0303(15) 0.0091(11) 0.0118(12) 0.0077(11) C6 0.0168(14) 0.0193(14) 0.0179(14) 0.0054(11) 0.0031(11) 0.0078(11) C14 0.0251(16) 0.0222(16) 0.0200(15) 0.0085(12) 0.0062(12) 0.0100(13) N5 0.0250(14) 0.0231(14) 0.0246(14) 0.0082(11) 0.0050(11) 0.0092(11) C7 0.0172(15) 0.0240(16) 0.0277(17) 0.0105(13) 0.0052(12) 0.0065(12) C8 0.0207(16) 0.0276(17) 0.0252(16) 0.0075(13) 0.0061(12) 0.0122(13) C1 0.0198(15) 0.0174(14) 0.0198(15) 0.0057(12) 0.0025(11) 0.0066(12) C10 0.0215(16) 0.0195(15) 0.0350(19) 0.0121(14) 0.0080(13) 0.0086(13) C2 0.0217(16) 0.0216(15) 0.0252(16) 0.0071(13) 0.0037(12) 0.0105(13) C13 0.0272(17) 0.0199(15) 0.0351(19) 0.0145(14) 0.0122(14) 0.0105(13) O4 0.062(2) 0.0374(16) 0.0340(16) 0.0135(13) 0.0122(14) 0.0177(15) C5 0.0236(16) 0.0185(15) 0.0244(16) 0.0082(12) 0.0039(12) 0.0091(12) C15 0.0258(17) 0.0272(17) 0.0258(17) 0.0098(14) 0.0060(13) 0.0093(14) C18 0.035(2) 0.0254(17) 0.0295(18) 0.0070(14) 0.0065(15) 0.0133(15) C9 0.0232(16) 0.0219(15) 0.0260(16) 0.0074(13) 0.0051(13) 0.0130(13) C11 0.0265(17) 0.0244(17) 0.0365(19) 0.0107(15) 0.0082(14) 0.0145(14) C4 0.0232(16) 0.0198(15) 0.0269(17) 0.0098(13) 0.0043(13) 0.0043(12) C19 0.0245(16) 0.0231(16) 0.0219(15) 0.0095(13) 0.0060(12) 0.0072(13) C17 0.034(2) 0.038(2) 0.0325(19) 0.0106(16) 0.0111(15) 0.0207(17) C3 0.0171(15) 0.0266(17) 0.0277(17) 0.0091(13) 0.0053(12) 0.0082(13) C24 0.0273(18) 0.0181(16) 0.045(2) 0.0118(15) 0.0090(15) 0.0057(13) C20 0.0209(16) 0.0350(19) 0.0339(19) 0.0159(16) 0.0082(14) 0.0070(14) C22 0.0332(19) 0.0218(17) 0.036(2) 0.0113(15) 0.0034(15) 0.0040(14) C23 0.0232(16) 0.0178(15) 0.042(2) 0.0107(14) 0.0140(15) 0.0080(13) C16 0.0257(18) 0.040(2) 0.0330(19) 0.0180(16) 0.0115(15) 0.0148(16) C21 0.0272(19) 0.034(2) 0.041(2) 0.0168(17) 0.0050(16) -0.0001(15) C12 0.034(2) 0.034(2) 0.038(2) 0.0147(16) 0.0135(16) 0.0213(16) C25 0.044(2) 0.029(2) 0.052(3) 0.0154(18) 0.018(2) 0.0114(18) C26 0.043(2) 0.032(2) 0.036(2) 0.0128(16) 0.0137(17) 0.0178(17) Cl1 0.0622(7) 0.0376(5) 0.0386(5) 0.0089(4) -0.0013(5) 0.0159(5) Cl2 0.0431(6) 0.0456(6) 0.0756(9) 0.0091(6) 0.0036(6) 0.0070(5) C27 0.050(2) 0.036(2) 0.034(2) 0.0117(17) 0.0079(18) 0.0186(19) _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 C1 1.974(3) . ? Pd1 N1 2.010(3) . ? Pd1 N3 2.037(3) . ? Pd1 O2 2.165(2) . ? Pd1 Pd2 2.9106(4) . ? Pd2 C14 1.968(3) . ? Pd2 N4 1.994(3) . ? Pd2 N6 2.026(3) . ? Pd2 O1 2.151(2) . ? O2 C23 1.237(4) . ? N4 C20 1.328(4) . ? N4 N5 1.356(4) . ? O1 C10 1.238(4) . ? O3 C13 1.221(5) . ? N3 C10 1.352(5) . ? N3 C13 1.395(4) . ? N1 C7 1.331(4) . ? N1 N2 1.355(4) . ? N2 C9 1.350(4) . ? N2 C6 1.421(4) . ? N6 C23 1.338(5) . ? N6 C26 1.380(5) . ? C6 C5 1.380(4) . ? C6 C1 1.408(4) . ? C14 C15 1.385(5) . ? C14 C19 1.402(5) . ? N5 C22 1.351(5) . ? N5 C19 1.418(4) . ? C7 C8 1.398(5) . ? C8 C9 1.378(5) . ? C1 C2 1.396(4) . ? C10 C11 1.515(4) . ? C2 C3 1.387(5) . ? C13 C12 1.516(5) . ? O4 C26 1.223(5) . ? C5 C4 1.387(5) . ? C15 C16 1.391(5) . ? C18 C19 1.387(5) . ? C18 C17 1.397(5) . ? C11 C12 1.514(5) . ? C4 C3 1.390(5) . ? C17 C16 1.378(6) . ? C24 C25 1.498(6) . ? C24 C23 1.520(5) . ? C20 C21 1.388(6) . ? C22 C21 1.364(6) . ? C25 C26 1.517(6) . ? Cl1 C27 1.779(4) . ? Cl2 C27 1.743(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 C1 Pd1 N1 81.31(12) . . ? C1 Pd1 N3 94.10(12) . . ? N1 Pd1 N3 175.24(11) . . ? C1 Pd1 O2 172.49(11) . . ? N1 Pd1 O2 93.67(10) . . ? N3 Pd1 O2 91.02(10) . . ? C1 Pd1 Pd2 108.06(9) . . ? N1 Pd1 Pd2 97.69(8) . . ? N3 Pd1 Pd2 82.46(8) . . ? O2 Pd1 Pd2 78.05(7) . . ? C14 Pd2 N4 81.56(13) . . ? C14 Pd2 N6 94.21(13) . . ? N4 Pd2 N6 175.77(11) . . ? C14 Pd2 O1 175.23(12) . . ? N4 Pd2 O1 93.67(11) . . ? N6 Pd2 O1 90.56(11) . . ? C14 Pd2 Pd1 100.03(9) . . ? N4 Pd2 Pd1 95.98(8) . . ? N6 Pd2 Pd1 84.52(9) . . ? O1 Pd2 Pd1 80.50(7) . . ? C23 O2 Pd1 125.9(2) . . ? C20 N4 N5 106.3(3) . . ? C20 N4 Pd2 139.1(3) . . ? N5 N4 Pd2 114.5(2) . . ? C10 O1 Pd2 124.3(2) . . ? C10 N3 C13 109.9(3) . . ? C10 N3 Pd1 125.2(2) . . ? C13 N3 Pd1 124.9(2) . . ? C7 N1 N2 106.3(3) . . ? C7 N1 Pd1 139.3(2) . . ? N2 N1 Pd1 114.35(19) . . ? C9 N2 N1 111.0(3) . . ? C9 N2 C6 133.2(3) . . ? N1 N2 C6 115.7(2) . . ? C23 N6 C26 109.0(3) . . ? C23 N6 Pd2 123.1(2) . . ? C26 N6 Pd2 127.8(3) . . ? C5 C6 C1 123.9(3) . . ? C5 C6 N2 121.5(3) . . ? C1 C6 N2 114.6(3) . . ? C15 C14 C19 116.7(3) . . ? C15 C14 Pd2 129.6(3) . . ? C19 C14 Pd2 113.7(2) . . ? C22 N5 N4 110.7(3) . . ? C22 N5 C19 134.1(3) . . ? N4 N5 C19 115.2(3) . . ? N1 C7 C8 110.2(3) . . ? C9 C8 C7 105.6(3) . . ? C2 C1 C6 116.0(3) . . ? C2 C1 Pd1 130.0(2) . . ? C6 C1 Pd1 114.0(2) . . ? O1 C10 N3 126.0(3) . . ? O1 C10 C11 122.1(3) . . ? N3 C10 C11 111.9(3) . . ? C3 C2 C1 121.4(3) . . ? O3 C13 N3 124.1(3) . . ? O3 C13 C12 125.8(3) . . ? N3 C13 C12 110.1(3) . . ? C6 C5 C4 118.1(3) . . ? C14 C15 C16 121.0(3) . . ? C19 C18 C17 117.7(3) . . ? N2 C9 C8 107.0(3) . . ? C12 C11 C10 103.7(3) . . ? C5 C4 C3 120.3(3) . . ? C18 C19 C14 123.6(3) . . ? C18 C19 N5 121.5(3) . . ? C14 C19 N5 114.9(3) . . ? C16 C17 C18 120.1(3) . . ? C2 C3 C4 120.4(3) . . ? C25 C24 C23 103.6(3) . . ? N4 C20 C21 109.8(3) . . ? N5 C22 C21 106.7(3) . . ? O2 C23 N6 126.0(3) . . ? O2 C23 C24 121.6(3) . . ? N6 C23 C24 112.4(3) . . ? C17 C16 C15 120.9(3) . . ? C22 C21 C20 106.5(3) . . ? C11 C12 C13 104.3(3) . . ? C24 C25 C26 103.6(3) . . ? O4 C26 N6 123.4(4) . . ? O4 C26 C25 125.3(4) . . ? N6 C26 C25 111.3(4) . . ? Cl2 C27 Cl1 111.3(2) . . ? _diffrn_measured_fraction_theta_max 0.906 _diffrn_reflns_theta_full 0.50 _diffrn_measured_fraction_theta_full 0.000 _refine_diff_density_max 3.154 _refine_diff_density_min -0.620 _refine_diff_density_rms 0.113 #===END ############################################################################## ### FullProf-generated CIF output file (version: February 2008) ### ### Template of CIF submission form for structure report ### ############################################################################## # This file has been generated using FullProf.2k taking one example of # structure report provided by Acta Cryst. It is given as a 'template' with # filled structural items. Many other items are left unfilled and it is the # responsibility of the user to properly fill or suppress them. In principle # all question marks '?' should be replaced by the appropriate text or # numerical value depending on the kind of CIF item. # See the document: cif_core.dic (URL: http://www.iucr.org) for details. # Please notify any error or suggestion to: # Juan Rodriguez-Carvajal (jrc@ill.eu) # Improvements will be progressively added as needed. #============================================================================= data_compound6 _database_code_depnum_ccdc_archive 'CCDC 783652' #TrackingRef '- crystaldata.cif' #============================================================================= # 5. CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_iupac ? _chemical_formula_sum 'C24 H20 N8 Pd2' _chemical_formula_weight 633.20 _chemical_melting_point ? _chemical_compound_source ? # for minerals and # natural products loop_ _atom_type_symbol _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source c 2.31000 20.84390 1.02000 10.20750 1.58860 0.56870 0.86500 51.65120 0.21560 0.00200 0.00200 International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5 h 0.49300 10.51090 0.32291 26.12570 0.14019 3.14236 0.04081 57.79970 0.00304 0.00000 0.00000 International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5 pd 19.33190 0.69866 15.50170 7.98929 5.29537 25.20520 0.60584 76.89860 5.26593 -1.17700 1.00700 International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5 n 12.21260 0.00570 3.13220 9.89330 2.01250 28.99750 1.16630 0.58260 -11.52900 0.00400 0.00300 International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5 #============================================================================= # 6. POWDER SPECIMEN AND CRYSTAL DATA _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 1 21/A 1' _symmetry_space_group_name_Hall '-P 2yab' loop_ _symmetry_equiv_pos_as_xyz #<--must include 'x,y,z' x,y,z -x+1/2,y+1/2,-z -x,-y,-z x+1/2,-y+1/2,z _cell_length_a 23.3603(5) _cell_length_b 8.95252(17) _cell_length_c 11.5684(2) _cell_angle_alpha 90.00000 _cell_angle_beta 104.0736(14) _cell_angle_gamma 90.00000 _cell_volume 2346.74(8) _cell_formula_units_Z ? _cell_measurement_temperature ? _cell_special_details ; ? ; # The next three fields give the specimen dimensions in mm. The equatorial # plane contains the incident and diffracted beam. _pd_spec_size_axial ? # perpendicular to # equatorial plane _pd_spec_size_equat ? # parallel to # scattering vector # in transmission _pd_spec_size_thick ? # parallel to # scattering vector # in reflection # The next five fields are character fields that describe the specimen. _pd_spec_mounting # This field should be # used to give details of the # container. ; ? ; _pd_spec_mount_mode ? # options are 'reflection' # or 'transmission' _pd_spec_shape ? # options are 'cylinder' # 'flat_sheet' or 'irregular' _pd_char_particle_morphology ? _pd_char_colour ? # use ICDD colour descriptions # The following three fields describe the preparation of the specimen. # The cooling rate is in K/min. The pressure at which the sample was # prepared is in kPa. The temperature of preparation is in K. _pd_prep_cool_rate ? _pd_prep_pressure ? _pd_prep_temperature ? # The next four fields are normally only needed for transmission experiments. _exptl_absorpt_coefficient_mu ? _exptl_absorpt_correction_type ? _exptl_absorpt_process_details ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? #============================================================================= # 7. EXPERIMENTAL DATA _exptl_special_details ; ? ; # The following item is used to identify the equipment used to record # the powder pattern when the diffractogram was measured at a laboratory # other than the authors' home institution, e.g. when neutron or synchrotron # radiation is used. _pd_instr_location ; ? ; _pd_calibration_special_details # description of the method used # to calibrate the instrument ; ? ; _diffrn_ambient_temperature ? _diffrn_source Synchrotron _diffrn_radiation_type ? _diffrn_radiation_wavelength 0.82400 _diffrn_radiation_monochromator ? _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? # Not in version 2.0.1 _diffrn_detector ? _diffrn_detector_type ? # make or model of detector _pd_meas_scan_method ? # options are 'step', 'cont', # 'tof', 'fixed' or # 'disp' (= dispersive) _pd_meas_special_details ; ? ; # The following four items give details of the measured (not processed) # powder pattern. Angles are in degrees. _pd_meas_number_of_points 3134 _pd_meas_2theta_range_min 2.99891 _pd_meas_2theta_range_max 49.98451 _pd_meas_2theta_range_inc 0.014997 #============================================================================= # 8. REFINEMENT DATA _refine_special_details ; ? ; # Use the next field to give any special details about the fitting of the # powder pattern. _pd_proc_ls_special_details ; ? ; # The next three items are given as text. _pd_proc_ls_profile_function ? _pd_proc_ls_background_function ? _pd_proc_ls_pref_orient_corr ; ? ; # The following profile R-factors are NOT CORRECTED for background # The sum is extended to all non-excluded points. # These are the current CIF standard _pd_proc_ls_prof_R_factor 8.0971 _pd_proc_ls_prof_wR_factor 10.3922 _pd_proc_ls_prof_wR_expected 2.1707 # The following profile R-factors are CORRECTED for background # The sum is extended to all non-excluded points. # These items are not in the current CIF standard, but are defined above #_pd_proc_ls_prof_cR_factor 13.5021 #_pd_proc_ls_prof_cwR_factor 15.4601 #_pd_proc_ls_prof_cwR_expected 3.2292 # The following items are not in the CIF standard, but are defined above #_pd_proc_ls_prof_chi2 22.9204 #_pd_proc_ls_prof_echi2 23.1263 # Items related to LS refinement _refine_ls_R_I_factor 8.0273 _refine_ls_number_reflns 2993 _refine_ls_number_parameters 69 _refine_ls_number_restraints 8 # The following four items apply to angular dispersive measurements. # 2theta minimum, maximum and increment (in degrees) are for the # intensities used in the refinement. _pd_proc_2theta_range_min 2.9886 _pd_proc_2theta_range_max 49.9742 _pd_proc_2theta_range_inc 0.014997 _pd_proc_wavelength 0.824000 _pd_block_diffractogram_id ? # The id used for the block containing # the powder pattern profile (section 11) # Give appropriate details in the next two text fields. _pd_proc_info_excluded_regions ? _pd_proc_info_data_reduction ? # The following items are used to identify the programs used. _computing_data_collection ? _computing_structure_solution ? _computing_structure_refinement FULLPROF _computing_molecular_graphics ? _computing_publication_material ? #============================================================================= # 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_adp_type # Not in version 2.0.1 _atom_site_type_symbol C8 -0.0294(2) 0.6875(7) -0.1713(6) 0.088(6) 1.00000 Uiso C H2 -0.0513(2) 0.6005(7) -0.1914(6) 0.088(6) 1.00000 Uiso H C9 0.0214(2) 0.6851(7) -0.0825(6) 0.088(6) 1.00000 Uiso C H1 0.0329(2) 0.5951(7) -0.0432(6) 0.088(6) 1.00000 Uiso H Pd1 0.12140(14) 0.9091(4) 0.0371(4) 0.049(2) 1.00000 Uiso Pd C1 0.0873(2) 1.0905(7) -0.0633(6) 0.088(6) 1.00000 Uiso C C2 0.1124(2) 1.2310(7) -0.0709(6) 0.088(6) 1.00000 Uiso C C4 0.0313(2) 1.3145(7) -0.2280(6) 0.088(6) 1.00000 Uiso C H5 0.0130(2) 1.3889(7) -0.2805(6) 0.088(6) 1.00000 Uiso H C5 0.0036(2) 1.1795(7) -0.2224(6) 0.088(6) 1.00000 Uiso C H4 -0.0338(2) 1.1623(7) -0.2715(6) 0.088(6) 1.00000 Uiso H C6 0.0311(2) 1.0699(7) -0.1441(6) 0.088(6) 1.00000 Uiso C N2 0.0070(2) 0.9153(7) -0.1501(6) 0.088(6) 1.00000 Uiso N H7 0.1432(2) 1.2565(7) -0.0153(6) 0.088(6) 1.00000 Uiso H C22 0.2383(3) 1.1025(11) 0.0772(7) 0.101(8) 1.00000 Uiso C N7 0.1973(3) 1.0207(11) 0.1118(7) 0.101(8) 1.00000 Uiso N N8 0.2130(3) 1.0155(11) 0.2324(7) 0.101(8) 1.00000 Uiso N C24 0.2625(3) 1.0923(11) 0.2771(7) 0.101(8) 1.00000 Uiso C H20 0.2820(3) 1.1057(11) 0.3568(7) 0.101(8) 1.00000 Uiso H C23 0.2782(3) 1.1477(11) 0.1752(7) 0.101(8) 1.00000 Uiso C H19 0.3111(3) 1.2064(11) 0.1756(7) 0.101(8) 1.00000 Uiso H N5 0.1548(5) 0.7104(7) 0.1233(7) 0.101(8) 1.00000 Uiso N N6 0.1768(5) 0.7231(7) 0.2426(7) 0.101(8) 1.00000 Uiso N C21 0.1967(5) 0.5889(7) 0.2847(7) 0.101(8) 1.00000 Uiso C H17 0.2137(5) 0.5681(7) 0.3646(7) 0.101(8) 1.00000 Uiso H C20 0.1888(5) 0.4859(7) 0.1940(7) 0.101(8) 1.00000 Uiso C H16 0.1990(5) 0.3852(7) 0.1992(7) 0.101(8) 1.00000 Uiso H C19 0.1617(5) 0.5685(7) 0.0919(7) 0.101(8) 1.00000 Uiso C H15 0.1504(5) 0.5308(7) 0.0146(7) 0.101(8) 1.00000 Uiso H Pd2 0.17155(19) 0.8960(4) 0.3507(4) 0.042(2) 1.00000 Uiso Pd N3 0.1630(3) 1.0765(8) 0.4596(6) 0.088(6) 1.00000 Uiso N C18 0.1822(3) 1.2198(8) 0.4604(6) 0.088(6) 1.00000 Uiso C C17 0.1671(3) 1.2880(8) 0.5546(6) 0.088(6) 1.00000 Uiso C H9 0.1744(3) 1.3879(8) 0.5760(6) 0.088(6) 1.00000 Uiso H C16 0.1400(3) 1.1880(8) 0.6124(6) 0.088(6) 1.00000 Uiso C H10 0.1258(3) 1.2054(8) 0.6797(6) 0.088(6) 1.00000 Uiso H N4 0.1380(3) 1.0538(8) 0.5493(6) 0.088(6) 1.00000 Uiso N C15 0.1198(3) 0.8959(8) 0.5574(6) 0.088(6) 1.00000 Uiso C C14 0.0912(3) 0.8476(8) 0.6421(6) 0.088(6) 1.00000 Uiso C H11 0.0809(3) 0.9160(8) 0.6944(6) 0.088(6) 1.00000 Uiso H C13 0.0778(3) 0.6982(8) 0.6495(6) 0.088(6) 1.00000 Uiso C H12 0.0591(3) 0.6648(8) 0.7070(6) 0.088(6) 1.00000 Uiso H C12 0.0927(3) 0.5985(8) 0.5697(6) 0.088(6) 1.00000 Uiso C H13 0.0842(3) 0.4976(8) 0.5740(6) 0.088(6) 1.00000 Uiso H C11 0.1203(3) 0.6487(8) 0.4840(6) 0.088(6) 1.00000 Uiso C H14 0.1295(3) 0.5792(8) 0.4313(6) 0.088(6) 1.00000 Uiso H C10 0.1349(3) 0.7985(8) 0.4719(6) 0.088(6) 1.00000 Uiso C H8 0.1940(3) 1.2608(8) 0.4021(6) 0.088(6) 1.00000 Uiso H H18 0.2406(3) 1.1275(11) 0.0004(7) 0.101(8) 1.00000 Uiso H C7 -0.0400(2) 0.8290(7) -0.2149(6) 0.088(6) 1.00000 Uiso C N1 0.0426(2) 0.8270(7) -0.0729(6) 0.088(6) 1.00000 Uiso N H3 -0.0718(2) 0.8613(7) -0.2750(6) 0.088(6) 1.00000 Uiso H C3 0.0870(2) 1.3380(7) -0.1540(6) 0.088(6) 1.00000 Uiso C H6 0.1030(2) 1.4337(7) -0.1492(6) 0.088(6) 1.00000 Uiso H # Note: if the displacement parameters were refined anisotropically # the U matrices should be given as for single-crystal studies. #============================================================================= # 10. DISTANCES AND ANGLES / MOLECULAR GEOMETRY _geom_special_details ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag ? ? ? ? ? ? loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag ? ? ? ? ? ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag ? ? ? ? ? ? ? ? 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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag ? ? ? ? ? ? ? ? ? ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_D _geom_hbond_site_symmetry_H _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag ? ? ? ? ? ? ? ? ? ? ? #============================================================================= #============================================================================= # Additional structures (last six sections and associated data_? identifiers) # may be added at this point. #============================================================================= # The following lines are used to test the character set of files sent by # network email or other means. They are not part of the CIF data set. # abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789 # !@#$%^&*()_+{}:"~<>?|\-=[];'`,./