# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_publication _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _publ_contact_author_name 'Cross, Warren B.' _publ_contact_author_address 'Department of Chemistry, University of Leicester, Leicester, LE1 7RH, UK' _publ_contact_author_email wbc2@le.ac.uk loop_ _publ_author_name _publ_author_address W.B.Cross '' C.G.Daly '' R.L.Ackerman '' I.R.George '' K.Singh '' _publ_section_title 'N-heterocyclic carbene tethered amido complexes of palladium and platinum' data_09075n _database_code_depnum_ccdc_archive 'CCDC 791423' #TrackingRef '- Cross Dalton crystal structure data.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '[CNC-i-Pr]PdI (7a)' _chemical_melting_point ? _chemical_formula_moiety 'C24 H26 I N5 Pd,2(C6 H6)' _chemical_formula_sum 'C36 H38 I N5 Pd' _chemical_formula_weight 774.01 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' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M C222(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x, y, -z+1/2' 'x, -y, -z' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 10.8012(19) _cell_length_b 19.746(4) _cell_length_c 15.230(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3248.2(10) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 976 _cell_measurement_theta_min 3.379 _cell_measurement_theta_max 28.537 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.583 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1552 _exptl_absorpt_coefficient_mu 1.555 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.646 _exptl_absorpt_correction_T_max 0.831 _exptl_absorpt_process_details ; absorption correction based on 10643 reflections(SADABS);Rint 0.0932 before correction and 0.0291 after. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 Apex 2000 CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13040 _diffrn_reflns_av_R_equivalents 0.0341 _diffrn_reflns_av_sigmaI/netI 0.0252 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.06 _diffrn_reflns_theta_max 26.37 _reflns_number_total 3336 _reflns_number_gt 3149 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Disordered C6H6 was omitted using the SQUEEZE option of PLATON. The solvent accessible voids are 1128.7 A3 with an estimated 375e/cell to be added. Eight solvent C6H6 molecules/unit cell accounting for 336e were included in the formula, FWt, (000) and density calculations. PLATON Reference:Spek, A.L. (1990), Acta Cryst. A46, C-34. 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^)+(0.0362P)^2^+2.6372P] 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 0.04(3) _refine_ls_number_reflns 3336 _refine_ls_number_parameters 144 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0277 _refine_ls_R_factor_gt 0.0260 _refine_ls_wR_factor_ref 0.0667 _refine_ls_wR_factor_gt 0.0661 _refine_ls_goodness_of_fit_ref 1.064 _refine_ls_restrained_S_all 1.064 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.0000 0.664516(12) 0.7500 0.01718(8) Uani 1 2 d S . . I1 I 0.0000 0.795617(11) 0.7500 0.03443(9) Uani 1 2 d S . . N1 N 0.0000 0.56204(14) 0.7500 0.0194(6) Uani 1 2 d S . . N2 N 0.1165(2) 0.60700(13) 0.90727(17) 0.0219(5) Uani 1 1 d . . . N3 N -0.0034(4) 0.68626(12) 0.95424(15) 0.0247(4) Uani 1 1 d . . . C1 C 0.1008(3) 0.52836(15) 0.7837(2) 0.0242(7) Uani 1 1 d . . . C2 C 0.1682(3) 0.55467(16) 0.8555(2) 0.0227(6) Uani 1 1 d . . . C3 C 0.2827(3) 0.52693(18) 0.8782(2) 0.0297(7) Uani 1 1 d . . . H3 H 0.3308 0.5477 0.9229 0.036 Uiso 1 1 calc R . . C4 C 0.3273(3) 0.46995(18) 0.8367(3) 0.0342(8) Uani 1 1 d . . . H4 H 0.4048 0.4510 0.8531 0.041 Uiso 1 1 calc R . . C5 C 0.2569(3) 0.44072(18) 0.7707(2) 0.0369(10) Uani 1 1 d . . . H5 H 0.2859 0.4007 0.7428 0.044 Uiso 1 1 calc R . . C6 C 0.1468(3) 0.46822(14) 0.7450(4) 0.0312(7) Uani 1 1 d . . . H6 H 0.1001 0.4466 0.7002 0.037 Uiso 1 1 calc R . . C7 C 0.0371(3) 0.65612(15) 0.8798(2) 0.0208(6) Uani 1 1 d . . . C8 C 0.1261(3) 0.60808(18) 0.9985(2) 0.0271(7) Uani 1 1 d . . . H8 H 0.1758 0.5790 1.0335 0.033 Uiso 1 1 calc R . . C9 C 0.0530(3) 0.6574(2) 1.0276(2) 0.0327(8) Uani 1 1 d . . . H9 H 0.0414 0.6706 1.0870 0.039 Uiso 1 1 calc R . . C10 C -0.0991(3) 0.73945(17) 0.9613(2) 0.0275(7) Uani 1 1 d . . . H10 H -0.1319 0.7491 0.9012 0.033 Uiso 1 1 calc R . . C11 C -0.2046(4) 0.7140(2) 1.0177(3) 0.0421(10) Uani 1 1 d . . . H11A H -0.2500 0.6787 0.9859 0.063 Uiso 1 1 calc R . . H11B H -0.2607 0.7516 1.0312 0.063 Uiso 1 1 calc R . . H11C H -0.1715 0.6953 1.0724 0.063 Uiso 1 1 calc R . . C12 C -0.0437(4) 0.8040(2) 0.9980(3) 0.0409(10) Uani 1 1 d . . . H12A H -0.0080 0.7949 1.0560 0.061 Uiso 1 1 calc R . . H12B H -0.1085 0.8385 1.0034 0.061 Uiso 1 1 calc R . . H12C H 0.0212 0.8204 0.9584 0.061 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 0.01709(13) 0.01198(13) 0.02246(14) 0.000 -0.0001(2) 0.000 I1 0.03880(16) 0.01635(13) 0.04812(17) 0.000 -0.0013(3) 0.000 N1 0.0201(13) 0.0142(13) 0.0239(14) 0.000 0.005(3) 0.000 N2 0.0218(13) 0.0197(12) 0.0240(13) 0.0017(10) 0.0000(11) -0.0014(11) N3 0.0202(10) 0.0257(10) 0.0282(11) -0.0047(9) -0.0032(17) 0.001(2) C1 0.0288(16) 0.0143(14) 0.0295(14) 0.0030(12) 0.0049(13) -0.0027(13) C2 0.0204(14) 0.0170(14) 0.0307(17) 0.0035(12) -0.0011(12) -0.0011(12) C3 0.0284(16) 0.0256(17) 0.0350(19) 0.0045(14) -0.0014(15) 0.0020(14) C4 0.0305(17) 0.0269(18) 0.045(2) 0.0087(16) 0.0025(16) 0.0037(15) C5 0.044(2) 0.0219(14) 0.045(3) 0.0003(14) 0.0076(15) 0.0054(14) C6 0.0400(15) 0.0169(12) 0.0368(17) -0.002(2) 0.007(2) 0.0007(11) C7 0.0190(14) 0.0172(14) 0.0263(15) -0.0003(12) -0.0004(11) -0.0009(10) C8 0.0268(16) 0.0319(18) 0.0226(15) 0.0086(14) -0.0019(13) 0.0030(14) C9 0.0331(16) 0.044(2) 0.0213(15) -0.0038(15) 0.0002(14) 0.0007(16) C10 0.0199(15) 0.0322(18) 0.0304(17) -0.0108(14) -0.0003(13) 0.0022(14) C11 0.0253(18) 0.050(2) 0.051(2) -0.0120(19) 0.0025(17) 0.0013(17) C12 0.0371(19) 0.0323(19) 0.053(2) -0.0197(18) -0.0057(17) 0.0072(16) _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 N1 2.024(3) . ? Pd1 C7 2.024(3) . ? Pd1 C7 2.024(3) 3_556 ? Pd1 I1 2.5887(6) . ? N1 C1 1.375(3) 3_556 ? N1 C1 1.375(3) . ? N2 C7 1.361(4) . ? N2 C8 1.394(4) . ? N2 C2 1.414(4) . ? N3 C7 1.353(4) . ? N3 C9 1.393(5) . ? N3 C10 1.478(4) . ? C1 C2 1.413(4) . ? C1 C6 1.416(4) . ? C2 C3 1.397(4) . ? C3 C4 1.377(5) . ? C3 H3 0.9500 . ? C4 C5 1.386(5) . ? C4 H4 0.9500 . ? C5 C6 1.365(5) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C8 C9 1.330(5) . ? C8 H8 0.9500 . ? C9 H9 0.9500 . ? C10 C11 1.513(5) . ? C10 C12 1.516(5) . ? C10 H10 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Pd1 C7 85.30(9) . . ? N1 Pd1 C7 85.30(9) . 3_556 ? C7 Pd1 C7 170.61(17) . 3_556 ? N1 Pd1 I1 180.0 . . ? C7 Pd1 I1 94.70(9) . . ? C7 Pd1 I1 94.70(9) 3_556 . ? C1 N1 C1 122.2(3) 3_556 . ? C1 N1 Pd1 118.92(16) 3_556 . ? C1 N1 Pd1 118.92(16) . . ? C7 N2 C8 110.0(3) . . ? C7 N2 C2 126.7(3) . . ? C8 N2 C2 122.5(3) . . ? C7 N3 C9 110.5(3) . . ? C7 N3 C10 126.9(3) . . ? C9 N3 C10 122.5(3) . . ? N1 C1 C2 121.3(3) . . ? N1 C1 C6 121.9(3) . . ? C2 C1 C6 116.7(3) . . ? C3 C2 C1 120.2(3) . . ? C3 C2 N2 119.9(3) . . ? C1 C2 N2 119.8(3) . . ? C4 C3 C2 121.1(3) . . ? C4 C3 H3 119.4 . . ? C2 C3 H3 119.4 . . ? C3 C4 C5 118.8(3) . . ? C3 C4 H4 120.6 . . ? C5 C4 H4 120.6 . . ? C6 C5 C4 121.3(4) . . ? C6 C5 H5 119.3 . . ? C4 C5 H5 119.3 . . ? C5 C6 C1 121.4(4) . . ? C5 C6 H6 119.3 . . ? C1 C6 H6 119.3 . . ? N3 C7 N2 105.0(3) . . ? N3 C7 Pd1 135.9(2) . . ? N2 C7 Pd1 118.9(2) . . ? C9 C8 N2 107.3(3) . . ? C9 C8 H8 126.3 . . ? N2 C8 H8 126.3 . . ? C8 C9 N3 107.0(3) . . ? C8 C9 H9 126.5 . . ? N3 C9 H9 126.5 . . ? N3 C10 C11 109.4(3) . . ? N3 C10 C12 110.4(3) . . ? C11 C10 C12 111.5(3) . . ? N3 C10 H10 108.5 . . ? C11 C10 H10 108.5 . . ? C12 C10 H10 108.5 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? 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 C7 Pd1 N1 C1 126.68(17) . . . 3_556 ? C7 Pd1 N1 C1 -53.32(17) 3_556 . . 3_556 ? C7 Pd1 N1 C1 -53.32(17) . . . . ? C7 Pd1 N1 C1 126.68(17) 3_556 . . . ? C1 N1 C1 C2 -145.8(3) 3_556 . . . ? Pd1 N1 C1 C2 34.2(3) . . . . ? C1 N1 C1 C6 38.3(2) 3_556 . . . ? Pd1 N1 C1 C6 -141.7(2) . . . . ? N1 C1 C2 C3 -167.9(3) . . . . ? C6 C1 C2 C3 8.3(4) . . . . ? N1 C1 C2 N2 15.3(4) . . . . ? C6 C1 C2 N2 -168.6(3) . . . . ? C7 N2 C2 C3 152.4(3) . . . . ? C8 N2 C2 C3 -38.2(4) . . . . ? C7 N2 C2 C1 -30.7(4) . . . . ? C8 N2 C2 C1 138.6(3) . . . . ? C1 C2 C3 C4 -6.0(5) . . . . ? N2 C2 C3 C4 170.8(3) . . . . ? C2 C3 C4 C5 0.9(5) . . . . ? C3 C4 C5 C6 1.6(5) . . . . ? C4 C5 C6 C1 1.0(6) . . . . ? N1 C1 C6 C5 170.2(3) . . . . ? C2 C1 C6 C5 -5.9(5) . . . . ? C9 N3 C7 N2 1.7(4) . . . . ? C10 N3 C7 N2 -174.8(3) . . . . ? C9 N3 C7 Pd1 177.6(3) . . . . ? C10 N3 C7 Pd1 1.1(5) . . . . ? C8 N2 C7 N3 -1.1(3) . . . . ? C2 N2 C7 N3 169.3(3) . . . . ? C8 N2 C7 Pd1 -177.9(2) . . . . ? C2 N2 C7 Pd1 -7.4(4) . . . . ? N1 Pd1 C7 N3 -136.0(3) . . . . ? I1 Pd1 C7 N3 44.0(3) . . . . ? N1 Pd1 C7 N2 39.5(2) . . . . ? I1 Pd1 C7 N2 -140.5(2) . . . . ? C7 N2 C8 C9 0.1(4) . . . . ? C2 N2 C8 C9 -170.8(3) . . . . ? N2 C8 C9 N3 0.9(4) . . . . ? C7 N3 C9 C8 -1.6(4) . . . . ? C10 N3 C9 C8 175.0(3) . . . . ? C7 N3 C10 C11 119.7(4) . . . . ? C9 N3 C10 C11 -56.4(4) . . . . ? C7 N3 C10 C12 -117.2(4) . . . . ? C9 N3 C10 C12 66.7(4) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.692 _refine_diff_density_min -0.554 _refine_diff_density_rms 0.077 #===END data_09076 _database_code_depnum_ccdc_archive 'CCDC 791424' #TrackingRef '- Cross Dalton crystal structure data.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '[CNC-n-Bu]PdI (7b)' _chemical_melting_point ? _chemical_formula_moiety 'C26 H30 I N5 Pd, C6 H6 ' _chemical_formula_sum 'C32 H36 I N5 Pd' _chemical_formula_weight 723.96 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' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Aba2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z' 'x, y+1/2, z+1/2' '-x, -y+1/2, z+1/2' 'x+1/2, -y+1, z+1/2' '-x+1/2, y+1, z+1/2' _cell_length_a 29.370(5) _cell_length_b 20.178(3) _cell_length_c 10.3042(17) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6106.4(18) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 945 _cell_measurement_theta_min 2.325 _cell_measurement_theta_max 23.324 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.575 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2896 _exptl_absorpt_coefficient_mu 1.648 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.628 _exptl_absorpt_correction_T_max 0.802 _exptl_absorpt_process_details ; absorption correction based on 7763 reflections(SADABS);Rint 0.1132 before correction and 0.0489 after. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 Apex 2000 CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23246 _diffrn_reflns_av_R_equivalents 0.0843 _diffrn_reflns_av_sigmaI/netI 0.0818 _diffrn_reflns_limit_h_min -36 _diffrn_reflns_limit_h_max 36 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.02 _diffrn_reflns_theta_max 26.00 _reflns_number_total 5940 _reflns_number_gt 4827 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0206P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment 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 0.03(3) _refine_ls_number_reflns 5940 _refine_ls_number_parameters 354 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0594 _refine_ls_R_factor_gt 0.0457 _refine_ls_wR_factor_ref 0.0790 _refine_ls_wR_factor_gt 0.0751 _refine_ls_goodness_of_fit_ref 0.934 _refine_ls_restrained_S_all 0.934 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.885536(13) 0.178191(18) 0.74599(5) 0.01906(11) Uani 1 1 d . . . I1 I 0.891434(12) 0.306805(16) 0.73513(5) 0.02993(12) Uani 1 1 d . . . N1 N 0.88200(15) 0.0784(2) 0.7580(6) 0.0195(12) Uani 1 1 d . . . N2 N 0.96101(17) 0.1185(3) 0.8946(5) 0.0230(13) Uani 1 1 d . . . N3 N 0.99086(16) 0.1910(2) 0.7678(5) 0.0213(13) Uani 1 1 d . . . N4 N 0.80734(18) 0.1204(2) 0.6072(5) 0.0251(13) Uani 1 1 d . . . N5 N 0.78070(16) 0.2045(2) 0.7080(6) 0.0259(15) Uani 1 1 d . . . C1 C 0.8950(2) 0.0469(3) 0.8712(7) 0.0233(16) Uani 1 1 d . . . C2 C 0.9310(2) 0.0700(3) 0.9448(6) 0.0244(16) Uani 1 1 d . . . C3 C 0.9411(2) 0.0416(3) 1.0656(6) 0.0267(16) Uani 1 1 d . . . H3 H 0.9654 0.0586 1.1168 0.032 Uiso 1 1 calc R . . C4 C 0.9160(3) -0.0108(3) 1.1093(7) 0.0343(18) Uani 1 1 d . . . H4 H 0.9226 -0.0302 1.1912 0.041 Uiso 1 1 calc R . . C5 C 0.8811(3) -0.0355(5) 1.0349(8) 0.035(2) Uani 1 1 d . . . H5 H 0.8636 -0.0719 1.0654 0.042 Uiso 1 1 calc R . . C6 C 0.8715(3) -0.0076(3) 0.9165(8) 0.0323(19) Uani 1 1 d . . . H6 H 0.8481 -0.0263 0.8644 0.039 Uiso 1 1 calc R . . C7 C 0.9505(2) 0.1653(3) 0.8052(6) 0.0201(15) Uani 1 1 d . . . C8 C 1.0083(2) 0.1172(3) 0.9131(7) 0.0282(17) Uani 1 1 d . . . H8 H 1.0245 0.0896 0.9717 0.034 Uiso 1 1 calc R . . C9 C 1.0260(2) 0.1616(3) 0.8342(8) 0.0373(19) Uani 1 1 d . . . H9 H 1.0575 0.1715 0.8248 0.045 Uiso 1 1 calc R . . C10 C 0.8705(2) 0.0442(3) 0.6486(7) 0.0240(16) Uani 1 1 d . . . C11 C 0.8927(2) -0.0142(4) 0.6097(7) 0.0292(18) Uani 1 1 d . . . H11 H 0.9146 -0.0336 0.6659 0.035 Uiso 1 1 calc R . . C12 C 0.8835(2) -0.0440(4) 0.4929(8) 0.029(2) Uani 1 1 d . . . H12 H 0.8996 -0.0832 0.4696 0.035 Uiso 1 1 calc R . . C13 C 0.8516(3) -0.0185(4) 0.4085(8) 0.0369(19) Uani 1 1 d . . . H13 H 0.8464 -0.0388 0.3267 0.044 Uiso 1 1 calc R . . C14 C 0.8273(2) 0.0376(3) 0.4456(7) 0.0322(18) Uani 1 1 d . . . H14 H 0.8049 0.0557 0.3893 0.039 Uiso 1 1 calc R . . C15 C 0.8358(2) 0.0672(3) 0.5655(6) 0.0228(15) Uani 1 1 d . . . C16 C 0.8202(2) 0.1716(3) 0.6865(6) 0.0242(16) Uani 1 1 d . . . C17 C 0.7611(2) 0.1217(4) 0.5843(8) 0.040(2) Uani 1 1 d . . . H17 H 0.7442 0.0909 0.5339 0.048 Uiso 1 1 calc R . . C18 C 0.7448(2) 0.1746(3) 0.6469(8) 0.043(2) Uani 1 1 d . . . H18 H 0.7140 0.1889 0.6486 0.052 Uiso 1 1 calc R . . C19 C 0.9990(2) 0.2304(3) 0.6501(7) 0.0332(18) Uani 1 1 d . . . H19A H 1.0234 0.2632 0.6669 0.040 Uiso 1 1 calc R . . H19B H 0.9709 0.2550 0.6270 0.040 Uiso 1 1 calc R . . C20 C 1.0126(3) 0.1866(4) 0.5392(8) 0.051(2) Uani 1 1 d . . . H20A H 1.0203 0.2151 0.4640 0.062 Uiso 1 1 calc R . . H20B H 1.0405 0.1624 0.5641 0.062 Uiso 1 1 calc R . . C21 C 0.9781(3) 0.1382(5) 0.4980(9) 0.071(3) Uani 1 1 d . . . H21A H 0.9497 0.1627 0.4796 0.085 Uiso 1 1 calc R . . H21B H 0.9719 0.1085 0.5724 0.085 Uiso 1 1 calc R . . C22 C 0.9884(3) 0.0963(4) 0.3844(8) 0.058(2) Uani 1 1 d . . . H22A H 0.9958 0.1246 0.3099 0.087 Uiso 1 1 calc R . . H22B H 0.9618 0.0690 0.3636 0.087 Uiso 1 1 calc R . . H22C H 1.0144 0.0676 0.4041 0.087 Uiso 1 1 calc R . . C23 C 0.7743(2) 0.2641(3) 0.7894(6) 0.0339(19) Uani 1 1 d . . . H23A H 0.8023 0.2722 0.8401 0.041 Uiso 1 1 calc R . . H23B H 0.7491 0.2560 0.8515 0.041 Uiso 1 1 calc R . . C24 C 0.7634(2) 0.3249(3) 0.7099(7) 0.034(2) Uani 1 1 d . . . H24A H 0.7894 0.3346 0.6517 0.041 Uiso 1 1 calc R . . H24B H 0.7365 0.3157 0.6550 0.041 Uiso 1 1 calc R . . C25 C 0.7541(2) 0.3841(3) 0.7920(7) 0.039(2) Uani 1 1 d . . . H25A H 0.7804 0.3918 0.8500 0.047 Uiso 1 1 calc R . . H25B H 0.7272 0.3750 0.8472 0.047 Uiso 1 1 calc R . . C26 C 0.7453(2) 0.4463(3) 0.7133(11) 0.053(3) Uani 1 1 d . . . H26A H 0.7726 0.4573 0.6627 0.080 Uiso 1 1 calc R . . H26B H 0.7382 0.4831 0.7721 0.080 Uiso 1 1 calc R . . H26C H 0.7196 0.4388 0.6545 0.080 Uiso 1 1 calc R . . C27 C 0.8564(3) 0.2739(7) 0.3458(11) 0.044(3) Uani 1 1 d . . . H27 H 0.8485 0.2963 0.4237 0.053 Uiso 1 1 calc R . . C28 C 0.85666(19) 0.3079(3) 0.2275(14) 0.0331(19) Uani 1 1 d . . . H28 H 0.8500 0.3540 0.2259 0.040 Uiso 1 1 calc R . . C29 C 0.8661(3) 0.2769(6) 0.1183(12) 0.036(2) Uani 1 1 d . . . H29 H 0.8662 0.3005 0.0385 0.043 Uiso 1 1 calc R . . C30 C 0.8760(4) 0.2090(5) 0.1204(10) 0.038(2) Uani 1 1 d . . . H30 H 0.8820 0.1863 0.0415 0.046 Uiso 1 1 calc R . . C31 C 0.87690(19) 0.1755(3) 0.2346(14) 0.043(2) Uani 1 1 d . . . H31 H 0.8840 0.1296 0.2366 0.052 Uiso 1 1 calc R . . C32 C 0.8673(4) 0.2095(6) 0.3483(12) 0.049(3) Uani 1 1 d . . . H32 H 0.8686 0.1868 0.4290 0.059 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 0.01785(19) 0.01555(19) 0.0238(3) 0.0018(4) 0.0003(4) 0.00038(16) I1 0.0317(2) 0.01947(18) 0.0386(3) 0.0022(4) -0.0016(4) 0.00107(15) N1 0.023(2) 0.015(2) 0.021(3) -0.001(3) 0.001(3) -0.0016(19) N2 0.020(3) 0.027(3) 0.022(3) 0.000(3) -0.001(3) 0.005(2) N3 0.019(2) 0.025(3) 0.020(4) -0.002(3) 0.002(2) -0.004(2) N4 0.023(3) 0.022(3) 0.030(4) 0.002(2) -0.004(3) 0.000(2) N5 0.019(2) 0.027(3) 0.032(4) 0.004(3) 0.002(3) 0.003(2) C1 0.027(4) 0.022(4) 0.021(4) -0.001(3) 0.007(3) 0.007(3) C2 0.028(4) 0.019(4) 0.027(4) 0.005(3) 0.002(3) 0.009(3) C3 0.027(4) 0.031(4) 0.022(4) -0.006(3) 0.002(3) 0.013(3) C4 0.048(5) 0.034(4) 0.021(4) 0.006(3) 0.007(4) 0.017(4) C5 0.050(6) 0.030(5) 0.026(5) 0.002(4) 0.015(4) 0.008(4) C6 0.033(5) 0.022(4) 0.042(6) 0.000(4) 0.000(4) 0.009(4) C7 0.022(3) 0.016(3) 0.023(4) -0.003(3) -0.001(3) 0.000(3) C8 0.013(3) 0.036(4) 0.035(5) 0.008(3) -0.009(3) 0.007(3) C9 0.023(4) 0.035(4) 0.055(5) -0.006(4) -0.009(4) 0.000(3) C10 0.030(4) 0.013(4) 0.029(4) 0.009(3) 0.010(3) -0.005(3) C11 0.023(4) 0.028(4) 0.036(5) 0.003(4) 0.006(4) 0.003(3) C12 0.029(5) 0.017(4) 0.042(5) -0.001(4) 0.000(4) -0.003(3) C13 0.043(5) 0.037(5) 0.031(5) -0.008(4) -0.004(4) -0.013(4) C14 0.022(4) 0.036(4) 0.039(5) 0.005(3) -0.001(3) -0.009(3) C15 0.025(4) 0.015(3) 0.028(4) 0.007(3) 0.001(3) -0.006(3) C16 0.023(3) 0.019(3) 0.031(4) 0.003(3) 0.007(3) 0.009(3) C17 0.023(4) 0.034(4) 0.063(6) 0.001(4) -0.006(4) -0.001(3) C18 0.018(4) 0.044(5) 0.067(6) 0.000(4) -0.003(4) -0.001(3) C19 0.028(4) 0.029(4) 0.042(5) 0.006(4) 0.013(4) -0.005(3) C20 0.062(6) 0.049(5) 0.043(6) 0.005(4) 0.005(4) -0.012(4) C21 0.081(8) 0.085(8) 0.047(7) -0.008(6) 0.002(6) -0.016(6) C22 0.069(6) 0.061(6) 0.044(6) -0.008(5) 0.003(5) -0.005(5) C23 0.022(4) 0.038(4) 0.042(5) -0.002(3) 0.004(3) 0.005(3) C24 0.025(3) 0.034(4) 0.044(6) 0.004(4) 0.005(3) 0.005(3) C25 0.026(4) 0.028(4) 0.062(6) -0.002(3) -0.004(3) 0.006(3) C26 0.041(4) 0.032(4) 0.088(8) -0.001(5) -0.008(5) 0.008(3) C27 0.029(5) 0.064(8) 0.040(7) -0.027(6) 0.015(4) -0.009(5) C28 0.029(3) 0.028(3) 0.042(6) 0.006(5) -0.006(6) -0.001(3) C29 0.027(5) 0.047(6) 0.034(6) 0.002(5) 0.002(4) -0.013(4) C30 0.035(5) 0.045(6) 0.034(6) -0.006(5) 0.004(4) 0.007(4) C31 0.029(3) 0.034(3) 0.067(7) -0.009(8) -0.001(7) 0.005(3) C32 0.031(5) 0.070(9) 0.047(7) 0.037(6) 0.000(5) -0.006(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 N1 2.019(4) . ? Pd1 C16 2.020(6) . ? Pd1 C7 2.020(6) . ? Pd1 I1 2.6033(7) . ? N1 C10 1.365(9) . ? N1 C1 1.383(9) . ? N2 C7 1.354(7) . ? N2 C8 1.402(8) . ? N2 C2 1.415(8) . ? N3 C7 1.350(7) . ? N3 C9 1.372(8) . ? N3 C19 1.471(8) . ? N4 C16 1.368(7) . ? N4 C17 1.378(8) . ? N4 C15 1.426(8) . ? N5 C16 1.355(7) . ? N5 C18 1.368(8) . ? N5 C23 1.478(7) . ? C1 C6 1.379(10) . ? C1 C2 1.383(9) . ? C2 C3 1.403(9) . ? C3 C4 1.366(9) . ? C3 H3 0.9500 . ? C4 C5 1.372(11) . ? C4 H4 0.9500 . ? C5 C6 1.373(10) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C8 C9 1.316(9) . ? C8 H8 0.9500 . ? C9 H9 0.9500 . ? C10 C11 1.404(9) . ? C10 C15 1.411(9) . ? C11 C12 1.372(11) . ? C11 H11 0.9500 . ? C12 C13 1.378(10) . ? C12 H12 0.9500 . ? C13 C14 1.393(10) . ? C13 H13 0.9500 . ? C14 C15 1.394(9) . ? C14 H14 0.9500 . ? C17 C18 1.337(9) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 C20 1.499(10) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 C21 1.469(11) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 C22 1.475(11) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 C24 1.508(8) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 C25 1.489(8) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C26 1.517(9) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C32 1.339(18) . ? C27 C28 1.399(16) . ? C27 H27 0.9500 . ? C28 C29 1.317(16) . ? C28 H28 0.9500 . ? C29 C30 1.400(16) . ? C29 H29 0.9500 . ? C30 C31 1.358(15) . ? C30 H30 0.9500 . ? C31 C32 1.385(16) . ? C31 H31 0.9500 . ? C32 H32 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 N1 Pd1 C16 84.5(2) . . ? N1 Pd1 C7 84.3(2) . . ? C16 Pd1 C7 168.8(2) . . ? N1 Pd1 I1 178.65(17) . . ? C16 Pd1 I1 96.68(16) . . ? C7 Pd1 I1 94.52(16) . . ? C10 N1 C1 122.1(5) . . ? C10 N1 Pd1 117.8(4) . . ? C1 N1 Pd1 119.8(5) . . ? C7 N2 C8 109.3(5) . . ? C7 N2 C2 126.1(5) . . ? C8 N2 C2 123.7(5) . . ? C7 N3 C9 110.6(5) . . ? C7 N3 C19 125.9(5) . . ? C9 N3 C19 121.5(6) . . ? C16 N4 C17 111.1(6) . . ? C16 N4 C15 125.9(5) . . ? C17 N4 C15 122.6(6) . . ? C16 N5 C18 111.6(6) . . ? C16 N5 C23 127.0(5) . . ? C18 N5 C23 121.4(5) . . ? C6 C1 N1 121.0(7) . . ? C6 C1 C2 117.8(7) . . ? N1 C1 C2 121.2(6) . . ? C1 C2 C3 120.7(6) . . ? C1 C2 N2 120.6(6) . . ? C3 C2 N2 118.4(6) . . ? C4 C3 C2 119.6(7) . . ? C4 C3 H3 120.2 . . ? C2 C3 H3 120.2 . . ? C3 C4 C5 120.0(7) . . ? C3 C4 H4 120.0 . . ? C5 C4 H4 120.0 . . ? C4 C5 C6 120.1(8) . . ? C4 C5 H5 119.9 . . ? C6 C5 H5 119.9 . . ? C5 C6 C1 121.6(8) . . ? C5 C6 H6 119.2 . . ? C1 C6 H6 119.2 . . ? N3 C7 N2 105.2(5) . . ? N3 C7 Pd1 133.9(4) . . ? N2 C7 Pd1 120.7(4) . . ? C9 C8 N2 107.1(6) . . ? C9 C8 H8 126.4 . . ? N2 C8 H8 126.4 . . ? C8 C9 N3 107.7(6) . . ? C8 C9 H9 126.1 . . ? N3 C9 H9 126.1 . . ? N1 C10 C11 123.1(7) . . ? N1 C10 C15 120.9(6) . . ? C11 C10 C15 116.0(7) . . ? C12 C11 C10 121.9(7) . . ? C12 C11 H11 119.1 . . ? C10 C11 H11 119.1 . . ? C11 C12 C13 121.5(8) . . ? C11 C12 H12 119.3 . . ? C13 C12 H12 119.3 . . ? C12 C13 C14 118.7(8) . . ? C12 C13 H13 120.6 . . ? C14 C13 H13 120.6 . . ? C13 C14 C15 120.0(7) . . ? C13 C14 H14 120.0 . . ? C15 C14 H14 120.0 . . ? C14 C15 C10 121.7(6) . . ? C14 C15 N4 119.0(6) . . ? C10 C15 N4 119.2(6) . . ? N5 C16 N4 103.4(5) . . ? N5 C16 Pd1 137.0(5) . . ? N4 C16 Pd1 119.5(4) . . ? C18 C17 N4 106.6(6) . . ? C18 C17 H17 126.7 . . ? N4 C17 H17 126.7 . . ? C17 C18 N5 107.3(6) . . ? C17 C18 H18 126.3 . . ? N5 C18 H18 126.3 . . ? N3 C19 C20 110.7(5) . . ? N3 C19 H19A 109.5 . . ? C20 C19 H19A 109.5 . . ? N3 C19 H19B 109.5 . . ? C20 C19 H19B 109.5 . . ? H19A C19 H19B 108.1 . . ? C21 C20 C19 115.4(7) . . ? C21 C20 H20A 108.4 . . ? C19 C20 H20A 108.4 . . ? C21 C20 H20B 108.4 . . ? C19 C20 H20B 108.4 . . ? H20A C20 H20B 107.5 . . ? C20 C21 C22 118.1(8) . . ? C20 C21 H21A 107.8 . . ? C22 C21 H21A 107.8 . . ? C20 C21 H21B 107.8 . . ? C22 C21 H21B 107.8 . . ? H21A C21 H21B 107.1 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? N5 C23 C24 112.4(5) . . ? N5 C23 H23A 109.1 . . ? C24 C23 H23A 109.1 . . ? N5 C23 H23B 109.1 . . ? C24 C23 H23B 109.1 . . ? H23A C23 H23B 107.9 . . ? C25 C24 C23 112.5(6) . . ? C25 C24 H24A 109.1 . . ? C23 C24 H24A 109.1 . . ? C25 C24 H24B 109.1 . . ? C23 C24 H24B 109.1 . . ? H24A C24 H24B 107.8 . . ? C24 C25 C26 113.1(6) . . ? C24 C25 H25A 109.0 . . ? C26 C25 H25A 109.0 . . ? C24 C25 H25B 109.0 . . ? C26 C25 H25B 109.0 . . ? H25A C25 H25B 107.8 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C32 C27 C28 119.4(9) . . ? C32 C27 H27 120.3 . . ? C28 C27 H27 120.3 . . ? C29 C28 C27 120.8(6) . . ? C29 C28 H28 119.6 . . ? C27 C28 H28 119.6 . . ? C28 C29 C30 119.7(10) . . ? C28 C29 H29 120.1 . . ? C30 C29 H29 120.1 . . ? C31 C30 C29 120.3(9) . . ? C31 C30 H30 119.9 . . ? C29 C30 H30 119.9 . . ? C30 C31 C32 118.8(6) . . ? C30 C31 H31 120.6 . . ? C32 C31 H31 120.6 . . ? C27 C32 C31 120.8(10) . . ? C27 C32 H32 119.6 . . ? C31 C32 H32 119.6 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C16 Pd1 N1 C10 57.4(5) . . . . ? C7 Pd1 N1 C10 -121.8(5) . . . . ? I1 Pd1 N1 C10 -155(7) . . . . ? C16 Pd1 N1 C1 -128.3(5) . . . . ? C7 Pd1 N1 C1 52.5(5) . . . . ? I1 Pd1 N1 C1 20(7) . . . . ? C10 N1 C1 C6 -44.0(10) . . . . ? Pd1 N1 C1 C6 141.9(6) . . . . ? C10 N1 C1 C2 137.8(7) . . . . ? Pd1 N1 C1 C2 -36.3(8) . . . . ? C6 C1 C2 C3 -4.4(10) . . . . ? N1 C1 C2 C3 173.8(6) . . . . ? C6 C1 C2 N2 169.7(6) . . . . ? N1 C1 C2 N2 -12.1(9) . . . . ? C7 N2 C2 C1 28.3(9) . . . . ? C8 N2 C2 C1 -139.5(7) . . . . ? C7 N2 C2 C3 -157.4(6) . . . . ? C8 N2 C2 C3 34.7(9) . . . . ? C1 C2 C3 C4 2.0(10) . . . . ? N2 C2 C3 C4 -172.2(6) . . . . ? C2 C3 C4 C5 0.2(10) . . . . ? C3 C4 C5 C6 0.0(11) . . . . ? C4 C5 C6 C1 -2.6(12) . . . . ? N1 C1 C6 C5 -173.5(7) . . . . ? C2 C1 C6 C5 4.7(11) . . . . ? C9 N3 C7 N2 -1.0(7) . . . . ? C19 N3 C7 N2 163.0(5) . . . . ? C9 N3 C7 Pd1 -175.4(5) . . . . ? C19 N3 C7 Pd1 -11.4(9) . . . . ? C8 N2 C7 N3 1.4(7) . . . . ? C2 N2 C7 N3 -167.9(6) . . . . ? C8 N2 C7 Pd1 176.7(4) . . . . ? C2 N2 C7 Pd1 7.4(9) . . . . ? N1 Pd1 C7 N3 135.7(6) . . . . ? C16 Pd1 C7 N3 131.6(12) . . . . ? I1 Pd1 C7 N3 -45.0(6) . . . . ? N1 Pd1 C7 N2 -38.0(5) . . . . ? C16 Pd1 C7 N2 -42.1(15) . . . . ? I1 Pd1 C7 N2 141.3(5) . . . . ? C7 N2 C8 C9 -1.3(8) . . . . ? C2 N2 C8 C9 168.3(6) . . . . ? N2 C8 C9 N3 0.7(8) . . . . ? C7 N3 C9 C8 0.2(8) . . . . ? C19 N3 C9 C8 -164.6(6) . . . . ? C1 N1 C10 C11 -37.3(10) . . . . ? Pd1 N1 C10 C11 136.8(5) . . . . ? C1 N1 C10 C15 144.2(6) . . . . ? Pd1 N1 C10 C15 -41.6(8) . . . . ? N1 C10 C11 C12 -173.4(6) . . . . ? C15 C10 C11 C12 5.1(10) . . . . ? C10 C11 C12 C13 -0.9(12) . . . . ? C11 C12 C13 C14 -2.1(11) . . . . ? C12 C13 C14 C15 0.7(10) . . . . ? C13 C14 C15 C10 3.8(10) . . . . ? C13 C14 C15 N4 -173.7(6) . . . . ? N1 C10 C15 C14 172.0(6) . . . . ? C11 C10 C15 C14 -6.5(9) . . . . ? N1 C10 C15 N4 -10.5(9) . . . . ? C11 C10 C15 N4 171.0(6) . . . . ? C16 N4 C15 C14 -150.5(6) . . . . ? C17 N4 C15 C14 38.0(9) . . . . ? C16 N4 C15 C10 32.0(9) . . . . ? C17 N4 C15 C10 -139.5(6) . . . . ? C18 N5 C16 N4 1.0(7) . . . . ? C23 N5 C16 N4 179.1(5) . . . . ? C18 N5 C16 Pd1 -175.6(6) . . . . ? C23 N5 C16 Pd1 2.5(10) . . . . ? C17 N4 C16 N5 -1.5(7) . . . . ? C15 N4 C16 N5 -173.9(6) . . . . ? C17 N4 C16 Pd1 175.9(4) . . . . ? C15 N4 C16 Pd1 3.5(8) . . . . ? N1 Pd1 C16 N5 138.1(7) . . . . ? C7 Pd1 C16 N5 142.2(11) . . . . ? I1 Pd1 C16 N5 -41.2(7) . . . . ? N1 Pd1 C16 N4 -38.1(5) . . . . ? C7 Pd1 C16 N4 -34.0(15) . . . . ? I1 Pd1 C16 N4 142.6(4) . . . . ? C16 N4 C17 C18 1.4(8) . . . . ? C15 N4 C17 C18 174.1(6) . . . . ? N4 C17 C18 N5 -0.7(9) . . . . ? C16 N5 C18 C17 -0.2(9) . . . . ? C23 N5 C18 C17 -178.5(6) . . . . ? C7 N3 C19 C20 -91.5(8) . . . . ? C9 N3 C19 C20 71.0(8) . . . . ? N3 C19 C20 C21 62.9(9) . . . . ? C19 C20 C21 C22 176.4(8) . . . . ? C16 N5 C23 C24 110.7(7) . . . . ? C18 N5 C23 C24 -71.3(8) . . . . ? N5 C23 C24 C25 176.4(5) . . . . ? C23 C24 C25 C26 177.3(5) . . . . ? C32 C27 C28 C29 2.3(12) . . . . ? C27 C28 C29 C30 0.0(11) . . . . ? C28 C29 C30 C31 -1.5(14) . . . . ? C29 C30 C31 C32 0.9(11) . . . . ? C28 C27 C32 C31 -3.0(15) . . . . ? C30 C31 C32 C27 1.4(12) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.894 _refine_diff_density_min -1.009 _refine_diff_density_rms 0.105 #===END data_09083 _database_code_depnum_ccdc_archive 'CCDC 791425' #TrackingRef '- Cross Dalton crystal structure data.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '{[CNC-i-Pr]Pdpy}OTf (9a)' _chemical_melting_point ? _chemical_formula_moiety ' C29 H31 N6 Pd, C F3 O3 S,0.75 C H2 Cl2' _chemical_formula_sum 'C30.75 H32.50 Cl1.50 F3 N6 O3 Pd S' _chemical_formula_weight 782.76 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.372(4) _cell_length_b 11.933(5) _cell_length_c 26.284(11) _cell_angle_alpha 101.593(10) _cell_angle_beta 94.150(9) _cell_angle_gamma 95.257(10) _cell_volume 3159(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 958 _cell_measurement_theta_min 2.422 _cell_measurement_theta_max 23.439 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.646 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1590 _exptl_absorpt_coefficient_mu 0.842 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.338 _exptl_absorpt_correction_T_max 0.802 _exptl_absorpt_process_details ; absorption correction based on 3047 reflections(SADABS);Rint 0.2361 before correction and 0.0699 after. ; _exptl_special_details ; The crystal was weakly diffracting and hence the weak data. ; _diffrn_ambient_temperature 150(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 Apex 2000 CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25010 _diffrn_reflns_av_R_equivalents 0.2109 _diffrn_reflns_av_sigmaI/netI 0.3463 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 1.75 _diffrn_reflns_theta_max 26.00 _reflns_number_total 12296 _reflns_number_gt 4612 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Disordered CH2Cl2 was omitted using the SQUEEZE option of PLATON. The solvent accessible voids are 207.5 A3 with an estimated 124e/cell to be added. Three solvent CH2Cl2 molecules/unit cell accounting for 126e were included in the formula, FWt, (000) and density calculations. PLATON Reference: Spek, A.L. (1990), Acta Cryst. A46, C-34. The CF3 group of one of the anions was disordered and one of the F atoms has been split.Attempts to split other atoms failed. 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^)+(0.0472P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12296 _refine_ls_number_parameters 810 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.1872 _refine_ls_R_factor_gt 0.0910 _refine_ls_wR_factor_ref 0.1958 _refine_ls_wR_factor_gt 0.1639 _refine_ls_goodness_of_fit_ref 0.795 _refine_ls_restrained_S_all 0.795 _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 0.73594(7) 0.82805(6) 0.67917(3) 0.0249(2) Uani 1 1 d . . . N1 N 0.7893(8) 0.8109(7) 0.7525(3) 0.029(2) Uani 1 1 d . . . N2 N 0.9137(7) 0.6483(6) 0.6838(3) 0.026(2) Uani 1 1 d . . . N3 N 0.7664(7) 0.5822(6) 0.6195(3) 0.023(2) Uani 1 1 d . . . N4 N 0.6267(7) 0.9971(6) 0.7604(3) 0.025(2) Uani 1 1 d . . . N5 N 0.6730(8) 1.0880(6) 0.6994(4) 0.032(2) Uani 1 1 d . . . N6 N 0.6964(7) 0.8454(6) 0.6036(3) 0.021(2) Uani 1 1 d . . . C1 C 0.9123(9) 0.7866(8) 0.7656(5) 0.030(3) Uani 1 1 d . . . C2 C 0.9781(10) 0.7148(8) 0.7315(4) 0.027(3) Uani 1 1 d . . . C3 C 1.1092(9) 0.6995(8) 0.7436(5) 0.034(3) Uani 1 1 d . . . H3 H 1.1548 0.6538 0.7186 0.041 Uiso 1 1 calc R . . C4 C 1.1711(11) 0.7516(9) 0.7923(5) 0.040(3) Uani 1 1 d . . . H4 H 1.2583 0.7401 0.8018 0.048 Uiso 1 1 calc R . . C5 C 1.1038(10) 0.8187(9) 0.8255(4) 0.036(3) Uani 1 1 d . . . H5 H 1.1455 0.8553 0.8588 0.044 Uiso 1 1 calc R . . C6 C 0.9769(10) 0.8368(8) 0.8134(4) 0.033(3) Uani 1 1 d . . . H6 H 0.9335 0.8847 0.8384 0.039 Uiso 1 1 calc R . . C7 C 0.8050(9) 0.6759(8) 0.6578(4) 0.027(3) Uani 1 1 d . . . C8 C 0.9414(10) 0.5399(9) 0.6591(5) 0.037(3) Uani 1 1 d . . . H8 H 1.0129 0.5014 0.6685 0.044 Uiso 1 1 calc R . . C9 C 0.8494(10) 0.5000(8) 0.6200(4) 0.028(3) Uani 1 1 d . . . H9 H 0.8427 0.4273 0.5966 0.034 Uiso 1 1 calc R . . C10 C 0.6983(9) 0.8302(8) 0.7888(4) 0.024(3) Uani 1 1 d . . . C11 C 0.6864(10) 0.7577(7) 0.8267(4) 0.026(3) Uani 1 1 d . . . H11 H 0.7448 0.7013 0.8280 0.032 Uiso 1 1 calc R . . C12 C 0.5929(10) 0.7696(8) 0.8604(4) 0.033(3) Uani 1 1 d . . . H12 H 0.5894 0.7219 0.8853 0.039 Uiso 1 1 calc R . . C13 C 0.5028(10) 0.8474(8) 0.8602(4) 0.032(3) Uani 1 1 d . . . H13 H 0.4368 0.8517 0.8836 0.038 Uiso 1 1 calc R . . C14 C 0.5110(10) 0.9177(9) 0.8258(5) 0.038(3) Uani 1 1 d . . . H14 H 0.4495 0.9717 0.8248 0.046 Uiso 1 1 calc R . . C15 C 0.6088(10) 0.9120(7) 0.7916(4) 0.021(2) Uani 1 1 d . . . C16 C 0.6707(9) 0.9795(8) 0.7118(4) 0.026(3) Uani 1 1 d . . . C17 C 0.5958(9) 1.1071(8) 0.7759(4) 0.029(3) Uani 1 1 d . . . H17 H 0.5611 1.1379 0.8076 0.035 Uiso 1 1 calc R . . C18 C 0.6228(10) 1.1610(9) 0.7396(5) 0.040(3) Uani 1 1 d . . . H18 H 0.6103 1.2391 0.7402 0.048 Uiso 1 1 calc R . . C19 C 0.6456(8) 0.5636(8) 0.5860(4) 0.019(2) Uani 1 1 d . . . H19 H 0.5914 0.6253 0.6007 0.022 Uiso 1 1 calc R . . C20 C 0.5707(10) 0.4489(8) 0.5886(4) 0.037(3) Uani 1 1 d . . . H20A H 0.6150 0.3855 0.5704 0.055 Uiso 1 1 calc R . . H20B H 0.4822 0.4442 0.5718 0.055 Uiso 1 1 calc R . . H20C H 0.5667 0.4433 0.6251 0.055 Uiso 1 1 calc R . . C21 C 0.6628(10) 0.5743(8) 0.5312(4) 0.033(3) Uani 1 1 d . . . H21A H 0.7222 0.6433 0.5314 0.050 Uiso 1 1 calc R . . H21B H 0.5783 0.5806 0.5133 0.050 Uiso 1 1 calc R . . H21C H 0.6992 0.5062 0.5129 0.050 Uiso 1 1 calc R . . C22 C 0.7080(11) 1.1212(9) 0.6495(4) 0.038(3) Uani 1 1 d . . . H22 H 0.7334 1.0518 0.6258 0.045 Uiso 1 1 calc R . . C23 C 0.8225(11) 1.2122(9) 0.6610(5) 0.045(3) Uani 1 1 d . . . H23A H 0.7954 1.2846 0.6797 0.068 Uiso 1 1 calc R . . H23B H 0.8557 1.2235 0.6283 0.068 Uiso 1 1 calc R . . H23C H 0.8911 1.1878 0.6827 0.068 Uiso 1 1 calc R . . C24 C 0.5915(11) 1.1593(9) 0.6237(5) 0.047(4) Uani 1 1 d . . . H24A H 0.5185 1.0987 0.6188 0.071 Uiso 1 1 calc R . . H24B H 0.6115 1.1747 0.5897 0.071 Uiso 1 1 calc R . . H24C H 0.5680 1.2297 0.6457 0.071 Uiso 1 1 calc R . . C25 C 0.7968(10) 0.8704(8) 0.5781(5) 0.031(3) Uani 1 1 d . . . H25 H 0.8819 0.8712 0.5942 0.037 Uiso 1 1 calc R . . C26 C 0.7830(10) 0.8964(8) 0.5273(5) 0.033(3) Uani 1 1 d . . . H26 H 0.8576 0.9139 0.5102 0.040 Uiso 1 1 calc R . . C27 C 0.6598(10) 0.8956(9) 0.5036(5) 0.041(3) Uani 1 1 d . . . H27 H 0.6464 0.9144 0.4704 0.049 Uiso 1 1 calc R . . C28 C 0.5555(10) 0.8657(8) 0.5309(5) 0.037(3) Uani 1 1 d . . . H28 H 0.4689 0.8607 0.5154 0.044 Uiso 1 1 calc R . . C29 C 0.5778(10) 0.8433(8) 0.5806(4) 0.026(3) Uani 1 1 d . . . H29 H 0.5052 0.8259 0.5988 0.031 Uiso 1 1 calc R . . Pd1A Pd 0.30158(8) 0.34409(6) 0.78511(3) 0.0275(2) Uani 1 1 d . . . N1A N 0.4366(7) 0.4423(6) 0.7573(3) 0.030(2) Uani 1 1 d . . . N2A N 0.2621(7) 0.3227(7) 0.6705(3) 0.025(2) Uani 1 1 d . . . N3A N 0.2187(8) 0.1536(7) 0.6841(4) 0.037(3) Uani 1 1 d . . . N4A N 0.4988(8) 0.4707(6) 0.8680(4) 0.029(2) Uani 1 1 d . . . N5A N 0.3139(8) 0.4754(6) 0.9026(4) 0.027(2) Uani 1 1 d . . . N6A N 0.1644(7) 0.2438(6) 0.8149(4) 0.032(2) Uani 1 1 d . . . C1A C 0.3955(9) 0.4949(8) 0.7169(4) 0.026(3) Uani 1 1 d . . . C2A C 0.3086(9) 0.4433(8) 0.6765(4) 0.024(2) Uani 1 1 d . . . C3A C 0.2639(10) 0.4991(9) 0.6388(5) 0.044(3) Uani 1 1 d . . . H3A H 0.1968 0.4618 0.6128 0.052 Uiso 1 1 calc R . . C4A C 0.3174(10) 0.6104(9) 0.6388(5) 0.037(3) Uani 1 1 d . . . H4A H 0.2923 0.6477 0.6116 0.045 Uiso 1 1 calc R . . C5A C 0.4089(9) 0.6661(8) 0.6797(4) 0.032(3) Uani 1 1 d . . . H5A H 0.4468 0.7420 0.6805 0.038 Uiso 1 1 calc R . . C6A C 0.4436(9) 0.6119(8) 0.7183(4) 0.032(3) Uani 1 1 d . . . H6A H 0.5015 0.6526 0.7471 0.038 Uiso 1 1 calc R . . C7A C 0.2554(9) 0.2635(9) 0.7096(4) 0.028(3) Uani 1 1 d . . . C8A C 0.2297(9) 0.2489(9) 0.6217(4) 0.032(3) Uani 1 1 d . . . H8A H 0.2263 0.2693 0.5885 0.038 Uiso 1 1 calc R . . C9A C 0.2041(9) 0.1417(9) 0.6317(4) 0.035(3) Uani 1 1 d . . . H9A H 0.1805 0.0720 0.6067 0.042 Uiso 1 1 calc R . . C10A C 0.5629(9) 0.4606(7) 0.7797(4) 0.023(3) Uani 1 1 d . . . C11A C 0.6670(9) 0.4684(8) 0.7489(5) 0.033(3) Uani 1 1 d . . . H11A H 0.6494 0.4692 0.7130 0.039 Uiso 1 1 calc R . . C12A C 0.7938(10) 0.4750(8) 0.7695(5) 0.034(3) Uani 1 1 d . . . H12A H 0.8623 0.4834 0.7480 0.041 Uiso 1 1 calc R . . C13A C 0.8228(10) 0.4694(8) 0.8210(5) 0.034(3) Uani 1 1 d . . . H13A H 0.9104 0.4721 0.8349 0.041 Uiso 1 1 calc R . . C14A C 0.7213(10) 0.4600(8) 0.8520(5) 0.033(3) Uani 1 1 d . . . H14A H 0.7392 0.4536 0.8872 0.040 Uiso 1 1 calc R . . C15A C 0.5975(9) 0.4597(8) 0.8324(5) 0.030(3) Uani 1 1 d . . . C16A C 0.3702(9) 0.4375(8) 0.8571(4) 0.027(3) Uani 1 1 d . . . C17A C 0.5219(11) 0.5266(8) 0.9219(4) 0.034(3) Uani 1 1 d . . . H17A H 0.6037 0.5567 0.9405 0.041 Uiso 1 1 calc R . . C18A C 0.4079(10) 0.5281(8) 0.9405(4) 0.034(3) Uani 1 1 d . . . H18A H 0.3935 0.5612 0.9754 0.041 Uiso 1 1 calc R . . C19A C 0.2122(10) 0.0527(8) 0.7103(5) 0.038(3) Uani 1 1 d . . . H19A H 0.2342 0.0819 0.7486 0.045 Uiso 1 1 calc R . . C20A C 0.3085(10) -0.0286(8) 0.6906(5) 0.038(3) Uani 1 1 d . . . H20D H 0.2862 -0.0605 0.6533 0.057 Uiso 1 1 calc R . . H20E H 0.3062 -0.0912 0.7097 0.057 Uiso 1 1 calc R . . H20F H 0.3960 0.0130 0.6960 0.057 Uiso 1 1 calc R . . C21A C 0.0731(11) -0.0062(9) 0.7014(6) 0.061(4) Uani 1 1 d . . . H21D H 0.0133 0.0497 0.7144 0.091 Uiso 1 1 calc R . . H21E H 0.0661 -0.0695 0.7200 0.091 Uiso 1 1 calc R . . H21F H 0.0504 -0.0365 0.6640 0.091 Uiso 1 1 calc R . . C22A C 0.1737(11) 0.4764(9) 0.9096(5) 0.039(3) Uani 1 1 d . . . H22A H 0.1244 0.4266 0.8777 0.047 Uiso 1 1 calc R . . C23A C 0.1371(11) 0.5993(9) 0.9129(5) 0.056(4) Uani 1 1 d . . . H23D H 0.1876 0.6511 0.9429 0.084 Uiso 1 1 calc R . . H23E H 0.0441 0.6005 0.9172 0.084 Uiso 1 1 calc R . . H23F H 0.1561 0.6249 0.8808 0.084 Uiso 1 1 calc R . . C24A C 0.1395(11) 0.4257(10) 0.9556(5) 0.049(3) Uani 1 1 d . . . H24D H 0.1866 0.3584 0.9563 0.073 Uiso 1 1 calc R . . H24E H 0.0457 0.4024 0.9525 0.073 Uiso 1 1 calc R . . H24F H 0.1640 0.4833 0.9879 0.073 Uiso 1 1 calc R . . C25A C 0.0388(10) 0.2422(9) 0.8013(5) 0.044(4) Uani 1 1 d . . . H25A H 0.0123 0.2784 0.7738 0.053 Uiso 1 1 calc R . . C26A C -0.0548(12) 0.1894(10) 0.8260(6) 0.054(4) Uani 1 1 d . . . H26A H -0.1445 0.1891 0.8156 0.065 Uiso 1 1 calc R . . C27A C -0.0160(14) 0.1366(10) 0.8664(6) 0.060(4) Uani 1 1 d . . . H27A H -0.0783 0.1033 0.8854 0.072 Uiso 1 1 calc R . . C28A C 0.1156(13) 0.1339(9) 0.8781(5) 0.051(4) Uani 1 1 d . . . H28A H 0.1445 0.0931 0.9036 0.062 Uiso 1 1 calc R . . C29A C 0.2028(11) 0.1886(8) 0.8536(5) 0.038(3) Uani 1 1 d . . . H29A H 0.2930 0.1891 0.8633 0.046 Uiso 1 1 calc R . . C30 C 0.0612(11) 0.6868(11) 0.5282(7) 0.061(5) Uani 1 1 d . . . F1 F 0.0103(7) 0.6968(6) 0.5725(3) 0.063(2) Uani 1 1 d . . . F2 F 0.1139(6) 0.5888(5) 0.5173(3) 0.073(3) Uani 1 1 d . . . F3 F -0.0422(6) 0.6768(5) 0.4906(3) 0.066(2) Uani 1 1 d . . . S1 S 0.1718(3) 0.8080(2) 0.52347(13) 0.0344(7) Uani 1 1 d . . . O1 O 0.0994(7) 0.9046(6) 0.5362(3) 0.044(2) Uani 1 1 d . . . O2 O 0.2081(8) 0.7811(7) 0.4714(3) 0.062(3) Uani 1 1 d . . . O3 O 0.2746(7) 0.8044(7) 0.5630(3) 0.061(3) Uani 1 1 d . . . C31 C 0.5294(18) 0.1634(12) 0.9749(7) 0.134(10) Uani 1 1 d D . . F4 F 0.4425(13) 0.2437(11) 0.9879(5) 0.163(6) Uani 1 1 d D A . F5 F 0.6060(16) 0.1612(9) 1.0154(4) 0.189(8) Uani 1 1 d D A . F6B F 0.502(5) 0.0475(16) 0.9626(11) 0.19(2) Uani 0.50 1 d PD A 1 F6C F 0.440(3) 0.0793(16) 0.9489(9) 0.086(8) Uani 0.50 1 d PD A 2 S2 S 0.6201(4) 0.2191(3) 0.92617(14) 0.0586(11) Uani 1 1 d . A . O4 O 0.7017(9) 0.1239(7) 0.9112(4) 0.097(4) Uani 1 1 d . . . O5 O 0.6894(8) 0.3257(6) 0.9549(3) 0.061(3) Uani 1 1 d . . . O6 O 0.5195(7) 0.2253(7) 0.8873(4) 0.064(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 Pd1 0.0288(5) 0.0156(4) 0.0284(5) 0.0038(4) -0.0043(4) 0.0002(4) N1 0.035(5) 0.027(5) 0.027(6) 0.014(4) -0.005(5) 0.007(4) N2 0.031(5) 0.017(5) 0.030(6) 0.006(4) -0.003(4) 0.002(4) N3 0.027(5) 0.021(5) 0.020(5) 0.003(4) 0.003(4) 0.008(4) N4 0.034(5) 0.011(4) 0.028(6) 0.002(4) -0.003(4) 0.006(4) N5 0.049(6) 0.005(4) 0.043(6) 0.004(4) 0.005(5) 0.007(4) N6 0.018(4) 0.016(4) 0.026(5) 0.003(4) -0.001(4) -0.003(4) C1 0.021(6) 0.017(6) 0.049(8) 0.006(5) -0.003(5) -0.007(5) C2 0.036(6) 0.025(6) 0.019(6) 0.008(5) -0.008(5) 0.006(5) C3 0.028(6) 0.024(6) 0.052(8) 0.013(6) -0.002(6) -0.003(5) C4 0.038(7) 0.034(7) 0.045(8) 0.011(6) -0.015(6) 0.002(6) C5 0.032(7) 0.042(7) 0.030(7) -0.002(6) -0.016(6) 0.008(6) C6 0.034(6) 0.023(6) 0.039(8) 0.004(5) -0.001(6) 0.002(5) C7 0.020(5) 0.035(6) 0.020(6) 0.005(5) -0.014(5) -0.013(5) C8 0.026(6) 0.036(7) 0.049(8) 0.007(6) 0.000(6) 0.017(5) C9 0.038(6) 0.013(5) 0.032(7) -0.004(5) 0.009(5) 0.002(5) C10 0.023(6) 0.021(6) 0.021(6) -0.003(5) -0.011(5) -0.006(5) C11 0.039(7) 0.006(5) 0.030(7) -0.002(5) -0.015(6) 0.008(5) C12 0.043(7) 0.023(6) 0.031(7) 0.004(5) 0.008(6) -0.003(5) C13 0.031(6) 0.027(6) 0.036(8) 0.003(5) 0.006(5) 0.001(5) C14 0.038(7) 0.022(6) 0.049(9) -0.006(6) 0.002(6) 0.006(5) C15 0.037(6) 0.010(5) 0.013(6) -0.003(4) -0.002(5) 0.003(5) C16 0.024(6) 0.021(6) 0.029(7) 0.004(5) -0.013(5) -0.001(4) C17 0.041(7) 0.011(5) 0.038(7) 0.007(5) -0.003(6) 0.016(5) C18 0.050(8) 0.017(6) 0.055(9) 0.009(6) -0.005(7) 0.019(5) C19 0.022(5) 0.024(5) 0.005(5) -0.005(4) -0.001(4) -0.006(4) C20 0.037(7) 0.031(6) 0.041(8) 0.011(6) -0.003(6) -0.008(5) C21 0.036(6) 0.022(6) 0.035(7) -0.002(5) -0.005(6) -0.008(5) C22 0.069(8) 0.034(7) 0.009(6) 0.001(5) -0.001(6) 0.008(6) C23 0.062(8) 0.029(7) 0.044(8) 0.008(6) -0.001(7) 0.000(6) C24 0.068(9) 0.034(7) 0.042(8) 0.020(6) -0.014(7) 0.004(6) C25 0.019(6) 0.014(5) 0.054(9) -0.002(5) -0.004(6) 0.004(5) C26 0.026(6) 0.026(6) 0.048(8) 0.008(6) 0.006(6) 0.006(5) C27 0.040(7) 0.035(7) 0.049(9) 0.013(6) -0.005(6) 0.009(6) C28 0.027(6) 0.026(6) 0.059(9) 0.013(6) 0.007(6) 0.002(5) C29 0.035(6) 0.026(6) 0.017(6) 0.004(5) 0.001(5) 0.008(5) Pd1A 0.0312(5) 0.0195(5) 0.0292(6) 0.0047(4) -0.0057(4) -0.0034(4) N1A 0.020(5) 0.019(5) 0.043(6) 0.002(4) -0.007(4) -0.011(4) N2A 0.028(5) 0.024(5) 0.021(5) 0.004(4) -0.013(4) 0.001(4) N3A 0.049(6) 0.018(5) 0.038(6) 0.002(4) -0.018(5) -0.006(4) N4A 0.035(5) 0.015(4) 0.037(6) 0.007(4) -0.010(5) 0.006(4) N5A 0.029(5) 0.012(4) 0.035(6) -0.004(4) 0.003(4) -0.001(4) N6A 0.022(5) 0.008(4) 0.056(7) -0.011(4) 0.002(5) -0.004(4) C1A 0.031(6) 0.016(5) 0.036(7) 0.018(5) -0.002(5) 0.009(5) C2A 0.031(6) 0.014(5) 0.028(7) 0.005(5) 0.003(5) 0.004(5) C3A 0.027(6) 0.035(7) 0.063(10) 0.008(6) -0.014(6) -0.004(5) C4A 0.046(7) 0.028(6) 0.045(8) 0.024(6) 0.001(6) 0.004(5) C5A 0.029(6) 0.023(6) 0.045(8) 0.011(5) 0.004(6) -0.001(5) C6A 0.038(6) 0.017(5) 0.039(8) 0.012(5) -0.014(6) -0.010(5) C7A 0.032(6) 0.031(6) 0.026(7) 0.018(5) -0.003(5) 0.002(5) C8A 0.027(6) 0.040(7) 0.028(7) 0.013(6) 0.000(5) -0.008(5) C9A 0.035(6) 0.029(6) 0.028(7) -0.013(5) -0.014(6) -0.010(5) C10A 0.017(5) 0.007(5) 0.042(7) 0.000(5) 0.003(5) -0.001(4) C11A 0.026(6) 0.016(6) 0.050(8) -0.008(5) 0.001(6) 0.000(5) C12A 0.031(6) 0.018(6) 0.047(8) -0.001(5) -0.007(6) -0.003(5) C13A 0.026(6) 0.026(6) 0.043(8) -0.006(6) -0.014(6) 0.009(5) C14A 0.033(7) 0.028(6) 0.037(8) 0.006(5) -0.009(6) 0.006(5) C15A 0.011(5) 0.024(6) 0.052(8) -0.002(6) 0.005(5) 0.003(4) C16A 0.023(6) 0.016(5) 0.039(8) 0.008(5) -0.011(5) -0.003(4) C17A 0.053(8) 0.029(6) 0.019(7) 0.012(5) -0.013(6) -0.008(6) C18A 0.038(7) 0.026(6) 0.030(7) -0.002(5) -0.010(6) -0.012(5) C19A 0.040(7) 0.024(6) 0.047(8) 0.010(6) -0.008(6) -0.004(5) C20A 0.040(7) 0.028(6) 0.045(8) 0.006(6) -0.001(6) 0.004(5) C21A 0.049(8) 0.032(7) 0.104(13) 0.027(8) 0.001(8) -0.006(6) C22A 0.046(8) 0.033(7) 0.028(7) -0.014(6) 0.000(6) 0.006(6) C23A 0.049(8) 0.047(8) 0.073(11) 0.015(7) -0.018(7) 0.020(6) C24A 0.042(8) 0.052(8) 0.048(9) -0.001(7) 0.015(7) -0.003(6) C25A 0.036(7) 0.028(7) 0.064(10) 0.007(6) -0.020(7) 0.000(6) C26A 0.038(8) 0.043(8) 0.075(12) 0.005(8) 0.010(7) -0.018(6) C27A 0.064(10) 0.038(8) 0.075(12) 0.003(8) 0.031(8) -0.014(7) C28A 0.063(9) 0.021(6) 0.070(11) 0.010(6) 0.012(8) -0.004(6) C29A 0.043(7) 0.025(6) 0.054(9) 0.024(6) 0.002(6) 0.006(5) C30 0.006(6) 0.053(9) 0.107(14) -0.017(9) -0.008(7) 0.004(6) F1 0.061(5) 0.049(5) 0.097(7) 0.037(5) 0.041(5) 0.017(4) F2 0.046(4) 0.022(4) 0.145(8) 0.000(4) 0.011(5) 0.008(3) F3 0.056(5) 0.043(4) 0.091(7) 0.005(4) -0.010(5) -0.006(4) S1 0.0318(16) 0.0282(16) 0.043(2) 0.0084(14) 0.0014(15) 0.0013(13) O1 0.042(5) 0.024(4) 0.065(6) 0.004(4) 0.008(4) 0.001(4) O2 0.092(7) 0.060(6) 0.036(6) 0.010(5) 0.020(5) 0.006(5) O3 0.042(5) 0.060(6) 0.073(7) 0.009(5) -0.017(5) 0.002(4) C31 0.22(3) 0.052(12) 0.11(2) 0.000(13) 0.052(19) -0.085(15) F4 0.188(12) 0.112(9) 0.145(12) -0.063(9) 0.068(10) -0.058(9) F5 0.38(2) 0.105(9) 0.054(7) 0.051(7) -0.063(10) -0.108(11) F6B 0.48(6) 0.038(13) 0.06(2) 0.033(12) 0.02(3) -0.05(2) F6C 0.161(19) 0.041(12) 0.040(14) 0.010(10) -0.005(12) -0.071(13) S2 0.083(3) 0.039(2) 0.049(2) 0.0117(18) -0.010(2) -0.0127(19) O4 0.078(7) 0.048(6) 0.137(11) -0.047(6) -0.023(7) 0.031(5) O5 0.071(6) 0.036(5) 0.066(7) 0.002(5) 0.000(5) -0.020(4) O6 0.053(6) 0.057(6) 0.076(7) -0.002(5) -0.016(5) 0.018(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 C7 2.003(11) . ? Pd1 N1 2.023(8) . ? Pd1 C16 2.036(10) . ? Pd1 N6 2.054(8) . ? N1 C1 1.369(11) . ? N1 C10 1.389(13) . ? N2 C7 1.375(11) . ? N2 C8 1.390(12) . ? N2 C2 1.426(11) . ? N3 C7 1.353(11) . ? N3 C9 1.364(11) . ? N3 C19 1.451(10) . ? N4 C17 1.369(11) . ? N4 C16 1.370(13) . ? N4 C15 1.436(12) . ? N5 C18 1.394(14) . ? N5 C16 1.396(11) . ? N5 C22 1.503(13) . ? N6 C25 1.322(12) . ? N6 C29 1.326(11) . ? C1 C6 1.373(14) . ? C1 C2 1.375(14) . ? C2 C3 1.411(12) . ? C3 C4 1.387(14) . ? C3 H3 0.9500 . ? C4 C5 1.342(15) . ? C4 H4 0.9500 . ? C5 C6 1.378(12) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C8 C9 1.331(13) . ? C8 H8 0.9500 . ? C9 H9 0.9500 . ? C10 C15 1.403(13) . ? C10 C11 1.449(13) . ? C11 C12 1.359(14) . ? C11 H11 0.9500 . ? C12 C13 1.377(13) . ? C12 H12 0.9500 . ? C13 C14 1.354(14) . ? C13 H13 0.9500 . ? C14 C15 1.400(14) . ? C14 H14 0.9500 . ? C17 C18 1.286(14) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 C21 1.493(13) . ? C19 C20 1.528(12) . ? C19 H19 1.0000 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 C24 1.494(13) . ? C22 C23 1.504(13) . ? C22 H22 1.0000 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C26 1.429(14) . ? C25 H25 0.9500 . ? C26 C27 1.379(13) . ? C26 H26 0.9500 . ? C27 C28 1.399(15) . ? C27 H27 0.9500 . ? C28 C29 1.394(14) . ? C28 H28 0.9500 . ? C29 H29 0.9500 . ? Pd1A N1A 2.016(8) . ? Pd1A C7A 2.027(11) . ? Pd1A C16A 2.034(10) . ? Pd1A N6A 2.072(9) . ? N1A C10A 1.377(11) . ? N1A C1A 1.397(11) . ? N2A C7A 1.361(12) . ? N2A C8A 1.400(12) . ? N2A C2A 1.449(11) . ? N3A C9A 1.350(13) . ? N3A C7A 1.354(11) . ? N3A C19A 1.501(12) . ? N4A C16A 1.350(11) . ? N4A C17A 1.431(13) . ? N4A C15A 1.433(13) . ? N5A C18A 1.354(11) . ? N5A C16A 1.382(13) . ? N5A C22A 1.480(13) . ? N6A C25A 1.323(11) . ? N6A C29A 1.375(12) . ? C1A C2A 1.347(13) . ? C1A C6A 1.432(12) . ? C2A C3A 1.379(14) . ? C3A C4A 1.391(13) . ? C3A H3A 0.9500 . ? C4A C5A 1.395(13) . ? C4A H4A 0.9500 . ? C5A C6A 1.351(13) . ? C5A H5A 0.9500 . ? C6A H6A 0.9500 . ? C8A C9A 1.365(13) . ? C8A H8A 0.9500 . ? C9A H9A 0.9500 . ? C10A C11A 1.403(14) . ? C10A C15A 1.409(14) . ? C11A C12A 1.374(12) . ? C11A H11A 0.9500 . ? C12A C13A 1.381(14) . ? C12A H12A 0.9500 . ? C13A C14A 1.388(15) . ? C13A H13A 0.9500 . ? C14A C15A 1.347(12) . ? C14A H14A 0.9500 . ? C17A C18A 1.312(14) . ? C17A H17A 0.9500 . ? C18A H18A 0.9500 . ? C19A C20A 1.502(14) . ? C19A C21A 1.527(13) . ? C19A H19A 1.0000 . ? C20A H20D 0.9800 . ? C20A H20E 0.9800 . ? C20A H20F 0.9800 . ? C21A H21D 0.9800 . ? C21A H21E 0.9800 . ? C21A H21F 0.9800 . ? C22A C24A 1.507(15) . ? C22A C23A 1.536(14) . ? C22A H22A 1.0000 . ? C23A H23D 0.9800 . ? C23A H23E 0.9800 . ? C23A H23F 0.9800 . ? C24A H24D 0.9800 . ? C24A H24E 0.9800 . ? C24A H24F 0.9800 . ? C25A C26A 1.380(16) . ? C25A H25A 0.9500 . ? C26A C27A 1.393(17) . ? C26A H26A 0.9500 . ? C27A C28A 1.382(15) . ? C27A H27A 0.9500 . ? C28A C29A 1.343(15) . ? C28A H28A 0.9500 . ? C29A H29A 0.9500 . ? C30 F1 1.303(16) . ? C30 F2 1.323(13) . ? C30 F3 1.384(13) . ? C30 S1 1.793(14) . ? S1 O2 1.426(9) . ? S1 O1 1.430(7) . ? S1 O3 1.444(7) . ? C31 F5 1.287(15) . ? C31 F6C 1.337(16) . ? C31 F6B 1.354(17) . ? C31 F4 1.386(16) . ? C31 S2 1.837(19) . ? S2 O6 1.424(8) . ? S2 O5 1.439(7) . ? S2 O4 1.485(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 C7 Pd1 N1 84.4(4) . . ? C7 Pd1 C16 171.6(4) . . ? N1 Pd1 C16 87.2(4) . . ? C7 Pd1 N6 93.5(4) . . ? N1 Pd1 N6 175.6(3) . . ? C16 Pd1 N6 94.9(4) . . ? C1 N1 C10 122.4(9) . . ? C1 N1 Pd1 120.4(8) . . ? C10 N1 Pd1 117.1(6) . . ? C7 N2 C8 109.0(8) . . ? C7 N2 C2 125.0(8) . . ? C8 N2 C2 125.6(8) . . ? C7 N3 C9 110.9(8) . . ? C7 N3 C19 125.5(8) . . ? C9 N3 C19 123.2(8) . . ? C17 N4 C16 111.6(9) . . ? C17 N4 C15 122.5(9) . . ? C16 N4 C15 125.8(8) . . ? C18 N5 C16 107.9(10) . . ? C18 N5 C22 124.1(8) . . ? C16 N5 C22 127.8(9) . . ? C25 N6 C29 118.2(9) . . ? C25 N6 Pd1 117.0(6) . . ? C29 N6 Pd1 124.5(7) . . ? N1 C1 C6 120.7(10) . . ? N1 C1 C2 122.1(10) . . ? C6 C1 C2 117.1(9) . . ? C1 C2 C3 121.5(9) . . ? C1 C2 N2 120.9(9) . . ? C3 C2 N2 117.6(10) . . ? C4 C3 C2 119.6(11) . . ? C4 C3 H3 120.2 . . ? C2 C3 H3 120.2 . . ? C5 C4 C3 117.8(10) . . ? C5 C4 H4 121.1 . . ? C3 C4 H4 121.1 . . ? C4 C5 C6 122.9(10) . . ? C4 C5 H5 118.6 . . ? C6 C5 H5 118.6 . . ? C1 C6 C5 121.0(11) . . ? C1 C6 H6 119.5 . . ? C5 C6 H6 119.5 . . ? N3 C7 N2 104.9(8) . . ? N3 C7 Pd1 133.3(6) . . ? N2 C7 Pd1 121.8(7) . . ? C9 C8 N2 107.4(9) . . ? C9 C8 H8 126.3 . . ? N2 C8 H8 126.3 . . ? C8 C9 N3 107.7(9) . . ? C8 C9 H9 126.1 . . ? N3 C9 H9 126.1 . . ? N1 C10 C15 126.3(10) . . ? N1 C10 C11 119.5(9) . . ? C15 C10 C11 114.1(10) . . ? C12 C11 C10 120.8(9) . . ? C12 C11 H11 119.6 . . ? C10 C11 H11 119.6 . . ? C11 C12 C13 123.1(11) . . ? C11 C12 H12 118.4 . . ? C13 C12 H12 118.4 . . ? C14 C13 C12 118.0(11) . . ? C14 C13 H13 121.0 . . ? C12 C13 H13 121.0 . . ? C13 C14 C15 121.0(10) . . ? C13 C14 H14 119.5 . . ? C15 C14 H14 119.5 . . ? C14 C15 C10 122.7(10) . . ? C14 C15 N4 120.1(9) . . ? C10 C15 N4 117.1(10) . . ? N4 C16 N5 103.2(9) . . ? N4 C16 Pd1 121.6(7) . . ? N5 C16 Pd1 134.6(9) . . ? C18 C17 N4 107.2(11) . . ? C18 C17 H17 126.4 . . ? N4 C17 H17 126.4 . . ? C17 C18 N5 110.0(9) . . ? C17 C18 H18 125.0 . . ? N5 C18 H18 125.0 . . ? N3 C19 C21 113.8(8) . . ? N3 C19 C20 110.1(8) . . ? C21 C19 C20 112.2(8) . . ? N3 C19 H19 106.8 . . ? C21 C19 H19 106.8 . . ? C20 C19 H19 106.8 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C24 C22 N5 109.1(10) . . ? C24 C22 C23 112.8(9) . . ? N5 C22 C23 109.4(8) . . ? C24 C22 H22 108.5 . . ? N5 C22 H22 108.5 . . ? C23 C22 H22 108.5 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N6 C25 C26 123.0(9) . . ? N6 C25 H25 118.5 . . ? C26 C25 H25 118.5 . . ? C27 C26 C25 118.9(11) . . ? C27 C26 H26 120.6 . . ? C25 C26 H26 120.6 . . ? C26 C27 C28 116.9(11) . . ? C26 C27 H27 121.6 . . ? C28 C27 H27 121.6 . . ? C29 C28 C27 120.3(10) . . ? C29 C28 H28 119.8 . . ? C27 C28 H28 119.8 . . ? N6 C29 C28 122.6(10) . . ? N6 C29 H29 118.7 . . ? C28 C29 H29 118.7 . . ? N1A Pd1A C7A 85.3(4) . . ? N1A Pd1A C16A 86.3(4) . . ? C7A Pd1A C16A 171.6(4) . . ? N1A Pd1A N6A 179.1(3) . . ? C7A Pd1A N6A 95.5(4) . . ? C16A Pd1A N6A 92.8(4) . . ? C10A N1A C1A 122.1(9) . . ? C10A N1A Pd1A 120.1(7) . . ? C1A N1A Pd1A 117.7(6) . . ? C7A N2A C8A 110.9(8) . . ? C7A N2A C2A 125.9(8) . . ? C8A N2A C2A 122.9(9) . . ? C9A N3A C7A 113.1(9) . . ? C9A N3A C19A 122.7(9) . . ? C7A N3A C19A 123.7(9) . . ? C16A N4A C17A 108.4(10) . . ? C16A N4A C15A 127.4(9) . . ? C17A N4A C15A 124.2(9) . . ? C18A N5A C16A 109.3(9) . . ? C18A N5A C22A 122.5(10) . . ? C16A N5A C22A 127.7(8) . . ? C25A N6A C29A 119.1(10) . . ? C25A N6A Pd1A 120.9(8) . . ? C29A N6A Pd1A 119.6(7) . . ? C2A C1A N1A 124.0(9) . . ? C2A C1A C6A 116.5(9) . . ? N1A C1A C6A 119.5(8) . . ? C1A C2A C3A 123.0(9) . . ? C1A C2A N2A 119.8(9) . . ? C3A C2A N2A 117.2(8) . . ? C2A C3A C4A 119.7(9) . . ? C2A C3A H3A 120.1 . . ? C4A C3A H3A 120.1 . . ? C3A C4A C5A 118.7(10) . . ? C3A C4A H4A 120.6 . . ? C5A C4A H4A 120.6 . . ? C6A C5A C4A 119.9(9) . . ? C6A C5A H5A 120.0 . . ? C4A C5A H5A 120.0 . . ? C5A C6A C1A 121.9(9) . . ? C5A C6A H6A 119.1 . . ? C1A C6A H6A 119.1 . . ? N3A C7A N2A 103.6(9) . . ? N3A C7A Pd1A 135.4(7) . . ? N2A C7A Pd1A 121.1(7) . . ? C9A C8A N2A 105.7(10) . . ? C9A C8A H8A 127.2 . . ? N2A C8A H8A 127.2 . . ? N3A C9A C8A 106.8(9) . . ? N3A C9A H9A 126.6 . . ? C8A C9A H9A 126.6 . . ? N1A C10A C11A 120.4(10) . . ? N1A C10A C15A 123.7(10) . . ? C11A C10A C15A 115.5(9) . . ? C12A C11A C10A 121.6(11) . . ? C12A C11A H11A 119.2 . . ? C10A C11A H11A 119.2 . . ? C11A C12A C13A 120.8(12) . . ? C11A C12A H12A 119.6 . . ? C13A C12A H12A 119.6 . . ? C12A C13A C14A 118.7(9) . . ? C12A C13A H13A 120.7 . . ? C14A C13A H13A 120.7 . . ? C15A C14A C13A 120.3(11) . . ? C15A C14A H14A 119.9 . . ? C13A C14A H14A 119.9 . . ? C14A C15A C10A 123.0(11) . . ? C14A C15A N4A 118.1(11) . . ? C10A C15A N4A 118.5(8) . . ? N4A C16A N5A 106.0(9) . . ? N4A C16A Pd1A 119.7(8) . . ? N5A C16A Pd1A 134.3(7) . . ? C18A C17A N4A 106.6(9) . . ? C18A C17A H17A 126.7 . . ? N4A C17A H17A 126.7 . . ? C17A C18A N5A 109.8(11) . . ? C17A C18A H18A 125.1 . . ? N5A C18A H18A 125.1 . . ? N3A C19A C20A 111.0(10) . . ? N3A C19A C21A 108.6(8) . . ? C20A C19A C21A 112.0(9) . . ? N3A C19A H19A 108.4 . . ? C20A C19A H19A 108.4 . . ? C21A C19A H19A 108.4 . . ? C19A C20A H20D 109.5 . . ? C19A C20A H20E 109.5 . . ? H20D C20A H20E 109.5 . . ? C19A C20A H20F 109.5 . . ? H20D C20A H20F 109.5 . . ? H20E C20A H20F 109.5 . . ? C19A C21A H21D 109.5 . . ? C19A C21A H21E 109.5 . . ? H21D C21A H21E 109.5 . . ? C19A C21A H21F 109.5 . . ? H21D C21A H21F 109.5 . . ? H21E C21A H21F 109.5 . . ? N5A C22A C24A 111.1(9) . . ? N5A C22A C23A 109.0(9) . . ? C24A C22A C23A 113.7(10) . . ? N5A C22A H22A 107.6 . . ? C24A C22A H22A 107.6 . . ? C23A C22A H22A 107.6 . . ? C22A C23A H23D 109.5 . . ? C22A C23A H23E 109.5 . . ? H23D C23A H23E 109.5 . . ? C22A C23A H23F 109.5 . . ? H23D C23A H23F 109.5 . . ? H23E C23A H23F 109.5 . . ? C22A C24A H24D 109.5 . . ? C22A C24A H24E 109.5 . . ? H24D C24A H24E 109.5 . . ? C22A C24A H24F 109.5 . . ? H24D C24A H24F 109.5 . . ? H24E C24A H24F 109.5 . . ? N6A C25A C26A 121.8(12) . . ? N6A C25A H25A 119.1 . . ? C26A C25A H25A 119.1 . . ? C25A C26A C27A 119.1(12) . . ? C25A C26A H26A 120.5 . . ? C27A C26A H26A 120.5 . . ? C28A C27A C26A 118.1(13) . . ? C28A C27A H27A 120.9 . . ? C26A C27A H27A 120.9 . . ? C29A C28A C27A 120.3(13) . . ? C29A C28A H28A 119.9 . . ? C27A C28A H28A 119.9 . . ? C28A C29A N6A 121.4(11) . . ? C28A C29A H29A 119.3 . . ? N6A C29A H29A 119.3 . . ? F1 C30 F2 110.4(14) . . ? F1 C30 F3 105.7(10) . . ? F2 C30 F3 105.7(10) . . ? F1 C30 S1 114.2(9) . . ? F2 C30 S1 112.2(9) . . ? F3 C30 S1 108.1(11) . . ? O2 S1 O1 116.8(5) . . ? O2 S1 O3 114.1(6) . . ? O1 S1 O3 113.5(5) . . ? O2 S1 C30 104.2(6) . . ? O1 S1 C30 104.4(5) . . ? O3 S1 C30 101.5(6) . . ? F5 C31 F6C 127.3(17) . . ? F5 C31 F6B 93.2(19) . . ? F6C C31 F6B 38(2) . . ? F5 C31 F4 109.8(18) . . ? F6C C31 F4 95.8(18) . . ? F6B C31 F4 127(3) . . ? F5 C31 S2 110.4(13) . . ? F6C C31 S2 107.2(15) . . ? F6B C31 S2 113(2) . . ? F4 C31 S2 103.2(11) . . ? O6 S2 O5 117.6(5) . . ? O6 S2 O4 114.4(6) . . ? O5 S2 O4 115.2(5) . . ? O6 S2 C31 102.3(7) . . ? O5 S2 C31 104.1(6) . . ? O4 S2 C31 99.6(8) . . ? 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 C7 Pd1 N1 C1 51.4(7) . . . . ? C16 Pd1 N1 C1 -129.5(7) . . . . ? C7 Pd1 N1 C10 -131.6(7) . . . . ? C16 Pd1 N1 C10 47.6(7) . . . . ? C7 Pd1 N6 C25 -73.4(7) . . . . ? C16 Pd1 N6 C25 106.9(7) . . . . ? C7 Pd1 N6 C29 112.9(7) . . . . ? C16 Pd1 N6 C29 -66.9(8) . . . . ? C10 N1 C1 C6 -35.5(14) . . . . ? Pd1 N1 C1 C6 141.4(9) . . . . ? C10 N1 C1 C2 146.6(10) . . . . ? Pd1 N1 C1 C2 -36.5(12) . . . . ? N1 C1 C2 C3 173.7(9) . . . . ? C6 C1 C2 C3 -4.2(16) . . . . ? N1 C1 C2 N2 -9.8(16) . . . . ? C6 C1 C2 N2 172.3(9) . . . . ? C7 N2 C2 C1 25.1(16) . . . . ? C8 N2 C2 C1 -147.3(11) . . . . ? C7 N2 C2 C3 -158.2(9) . . . . ? C8 N2 C2 C3 29.3(15) . . . . ? C1 C2 C3 C4 4.4(16) . . . . ? N2 C2 C3 C4 -172.2(9) . . . . ? C2 C3 C4 C5 -2.4(16) . . . . ? C3 C4 C5 C6 0.5(18) . . . . ? N1 C1 C6 C5 -175.7(9) . . . . ? C2 C1 C6 C5 2.3(16) . . . . ? C4 C5 C6 C1 -0.5(18) . . . . ? C9 N3 C7 N2 -1.8(11) . . . . ? C19 N3 C7 N2 171.1(9) . . . . ? C9 N3 C7 Pd1 178.1(8) . . . . ? C19 N3 C7 Pd1 -8.9(16) . . . . ? C8 N2 C7 N3 2.3(12) . . . . ? C2 N2 C7 N3 -171.2(9) . . . . ? C8 N2 C7 Pd1 -177.6(7) . . . . ? C2 N2 C7 Pd1 8.8(14) . . . . ? N1 Pd1 C7 N3 142.8(11) . . . . ? N6 Pd1 C7 N3 -41.0(11) . . . . ? N1 Pd1 C7 N2 -37.2(8) . . . . ? N6 Pd1 C7 N2 138.9(8) . . . . ? C7 N2 C8 C9 -2.0(13) . . . . ? C2 N2 C8 C9 171.5(10) . . . . ? N2 C8 C9 N3 0.9(13) . . . . ? C7 N3 C9 C8 0.6(13) . . . . ? C19 N3 C9 C8 -172.5(9) . . . . ? C1 N1 C10 C15 141.2(9) . . . . ? Pd1 N1 C10 C15 -35.8(11) . . . . ? C1 N1 C10 C11 -41.9(12) . . . . ? Pd1 N1 C10 C11 141.1(7) . . . . ? N1 C10 C11 C12 -175.7(8) . . . . ? C15 C10 C11 C12 1.5(13) . . . . ? C10 C11 C12 C13 1.5(15) . . . . ? C11 C12 C13 C14 -2.1(15) . . . . ? C12 C13 C14 C15 -0.4(15) . . . . ? C13 C14 C15 C10 3.7(15) . . . . ? C13 C14 C15 N4 -171.6(9) . . . . ? N1 C10 C15 C14 173.0(9) . . . . ? C11 C10 C15 C14 -4.1(13) . . . . ? N1 C10 C15 N4 -11.6(13) . . . . ? C11 C10 C15 N4 171.4(7) . . . . ? C17 N4 C15 C14 28.6(13) . . . . ? C16 N4 C15 C14 -148.9(9) . . . . ? C17 N4 C15 C10 -147.0(9) . . . . ? C16 N4 C15 C10 35.5(13) . . . . ? C17 N4 C16 N5 3.5(10) . . . . ? C15 N4 C16 N5 -178.8(8) . . . . ? C17 N4 C16 Pd1 176.0(6) . . . . ? C15 N4 C16 Pd1 -6.2(12) . . . . ? C18 N5 C16 N4 -3.6(10) . . . . ? C22 N5 C16 N4 -177.2(9) . . . . ? C18 N5 C16 Pd1 -174.6(7) . . . . ? C22 N5 C16 Pd1 11.7(15) . . . . ? N1 Pd1 C16 N4 -29.1(7) . . . . ? N6 Pd1 C16 N4 154.7(7) . . . . ? N1 Pd1 C16 N5 140.6(9) . . . . ? N6 Pd1 C16 N5 -35.5(9) . . . . ? C16 N4 C17 C18 -2.0(12) . . . . ? C15 N4 C17 C18 -179.9(9) . . . . ? N4 C17 C18 N5 -0.4(12) . . . . ? C16 N5 C18 C17 2.6(12) . . . . ? C22 N5 C18 C17 176.6(9) . . . . ? C7 N3 C19 C21 107.8(11) . . . . ? C9 N3 C19 C21 -80.1(12) . . . . ? C7 N3 C19 C20 -125.3(10) . . . . ? C9 N3 C19 C20 46.8(13) . . . . ? C18 N5 C22 C24 -56.6(12) . . . . ? C16 N5 C22 C24 116.1(11) . . . . ? C18 N5 C22 C23 67.3(13) . . . . ? C16 N5 C22 C23 -120.0(10) . . . . ? C29 N6 C25 C26 0.7(14) . . . . ? Pd1 N6 C25 C26 -173.5(7) . . . . ? N6 C25 C26 C27 0.0(15) . . . . ? C25 C26 C27 C28 -1.8(14) . . . . ? C26 C27 C28 C29 2.8(15) . . . . ? C25 N6 C29 C28 0.4(14) . . . . ? Pd1 N6 C29 C28 174.1(7) . . . . ? C27 C28 C29 N6 -2.2(15) . . . . ? C7A Pd1A N1A C10A -131.4(8) . . . . ? C16A Pd1A N1A C10A 47.6(8) . . . . ? C7A Pd1A N1A C1A 52.1(7) . . . . ? C16A Pd1A N1A C1A -129.0(8) . . . . ? C7A Pd1A N6A C25A -61.6(8) . . . . ? C16A Pd1A N6A C25A 119.5(8) . . . . ? C7A Pd1A N6A C29A 125.9(8) . . . . ? C16A Pd1A N6A C29A -53.0(8) . . . . ? C10A N1A C1A C2A 143.0(11) . . . . ? Pd1A N1A C1A C2A -40.5(14) . . . . ? C10A N1A C1A C6A -39.1(15) . . . . ? Pd1A N1A C1A C6A 137.4(8) . . . . ? N1A C1A C2A C3A 176.2(10) . . . . ? C6A C1A C2A C3A -1.8(16) . . . . ? N1A C1A C2A N2A -6.3(16) . . . . ? C6A C1A C2A N2A 175.8(9) . . . . ? C7A N2A C2A C1A 26.8(15) . . . . ? C8A N2A C2A C1A -146.7(10) . . . . ? C7A N2A C2A C3A -155.5(10) . . . . ? C8A N2A C2A C3A 31.0(14) . . . . ? C1A C2A C3A C4A 5.8(18) . . . . ? N2A C2A C3A C4A -171.8(10) . . . . ? C2A C3A C4A C5A -4.7(17) . . . . ? C3A C4A C5A C6A -0.1(17) . . . . ? C4A C5A C6A C1A 4.2(17) . . . . ? C2A C1A C6A C5A -3.3(16) . . . . ? N1A C1A C6A C5A 178.7(10) . . . . ? C9A N3A C7A N2A 0.8(12) . . . . ? C19A N3A C7A N2A 173.0(9) . . . . ? C9A N3A C7A Pd1A -177.1(8) . . . . ? C19A N3A C7A Pd1A -5.0(16) . . . . ? C8A N2A C7A N3A -0.1(11) . . . . ? C2A N2A C7A N3A -174.2(8) . . . . ? C8A N2A C7A Pd1A 178.2(6) . . . . ? C2A N2A C7A Pd1A 4.1(13) . . . . ? N1A Pd1A C7A N3A 142.6(11) . . . . ? N6A Pd1A C7A N3A -37.1(11) . . . . ? N1A Pd1A C7A N2A -35.1(8) . . . . ? N6A Pd1A C7A N2A 145.2(8) . . . . ? C7A N2A C8A C9A -0.7(11) . . . . ? C2A N2A C8A C9A 173.7(8) . . . . ? C7A N3A C9A C8A -1.2(12) . . . . ? C19A N3A C9A C8A -173.5(9) . . . . ? N2A C8A C9A N3A 1.1(11) . . . . ? C1A N1A C10A C11A -39.4(13) . . . . ? Pd1A N1A C10A C11A 144.2(8) . . . . ? C1A N1A C10A C15A 148.1(10) . . . . ? Pd1A N1A C10A C15A -28.3(12) . . . . ? N1A C10A C11A C12A -173.3(8) . . . . ? C15A C10A C11A C12A -0.2(13) . . . . ? C10A C11A C12A C13A 2.6(15) . . . . ? C11A C12A C13A C14A -1.6(15) . . . . ? C12A C13A C14A C15A -2.0(15) . . . . ? C13A C14A C15A C10A 4.6(15) . . . . ? C13A C14A C15A N4A -168.9(9) . . . . ? N1A C10A C15A C14A 169.4(9) . . . . ? C11A C10A C15A C14A -3.5(14) . . . . ? N1A C10A C15A N4A -17.1(14) . . . . ? C11A C10A C15A N4A 170.0(8) . . . . ? C16A N4A C15A C14A -157.4(9) . . . . ? C17A N4A C15A C14A 26.4(14) . . . . ? C16A N4A C15A C10A 28.8(14) . . . . ? C17A N4A C15A C10A -147.4(9) . . . . ? C17A N4A C16A N5A 2.0(10) . . . . ? C15A N4A C16A N5A -174.6(8) . . . . ? C17A N4A C16A Pd1A -175.5(6) . . . . ? C15A N4A C16A Pd1A 7.8(13) . . . . ? C18A N5A C16A N4A -1.4(11) . . . . ? C22A N5A C16A N4A 170.2(9) . . . . ? C18A N5A C16A Pd1A 175.6(8) . . . . ? C22A N5A C16A Pd1A -12.8(15) . . . . ? N1A Pd1A C16A N4A -37.4(7) . . . . ? N6A Pd1A C16A N4A 142.3(7) . . . . ? N1A Pd1A C16A N5A 146.0(10) . . . . ? N6A Pd1A C16A N5A -34.3(10) . . . . ? C16A N4A C17A C18A -2.0(11) . . . . ? C15A N4A C17A C18A 174.8(9) . . . . ? N4A C17A C18A N5A 1.1(12) . . . . ? C16A N5A C18A C17A 0.2(12) . . . . ? C22A N5A C18A C17A -171.9(9) . . . . ? C9A N3A C19A C20A 55.6(13) . . . . ? C7A N3A C19A C20A -115.8(11) . . . . ? C9A N3A C19A C21A -67.9(14) . . . . ? C7A N3A C19A C21A 120.7(11) . . . . ? C18A N5A C22A C24A -57.8(12) . . . . ? C16A N5A C22A C24A 131.6(10) . . . . ? C18A N5A C22A C23A 68.4(13) . . . . ? C16A N5A C22A C23A -102.2(11) . . . . ? C29A N6A C25A C26A 1.9(16) . . . . ? Pd1A N6A C25A C26A -170.7(9) . . . . ? N6A C25A C26A C27A 0.2(19) . . . . ? C25A C26A C27A C28A -3.5(18) . . . . ? C26A C27A C28A C29A 5.0(19) . . . . ? C27A C28A C29A N6A -3.1(19) . . . . ? C25A N6A C29A C28A -0.4(16) . . . . ? Pd1A N6A C29A C28A 172.2(9) . . . . ? F1 C30 S1 O2 -176.6(9) . . . . ? F2 C30 S1 O2 56.9(12) . . . . ? F3 C30 S1 O2 -59.2(10) . . . . ? F1 C30 S1 O1 -53.6(11) . . . . ? F2 C30 S1 O1 179.9(10) . . . . ? F3 C30 S1 O1 63.8(11) . . . . ? F1 C30 S1 O3 64.7(10) . . . . ? F2 C30 S1 O3 -61.9(12) . . . . ? F3 C30 S1 O3 -178.0(9) . . . . ? F5 C31 S2 O6 -174.8(12) . . . . ? F6C C31 S2 O6 42.9(18) . . . . ? F6B C31 S2 O6 83(2) . . . . ? F4 C31 S2 O6 -57.5(11) . . . . ? F5 C31 S2 O5 -51.8(15) . . . . ? F6C C31 S2 O5 165.9(17) . . . . ? F6B C31 S2 O5 -154(2) . . . . ? F4 C31 S2 O5 65.5(11) . . . . ? F5 C31 S2 O4 67.4(14) . . . . ? F6C C31 S2 O4 -74.9(18) . . . . ? F6B C31 S2 O4 -35(2) . . . . ? F4 C31 S2 O4 -175.3(9) . . . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 1.347 _refine_diff_density_min -2.118 _refine_diff_density_rms 0.170 #===END data_10027 _database_code_depnum_ccdc_archive 'CCDC 791426' #TrackingRef '- Cross Dalton crystal structure data.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '[C,NH]PdI2py (10)' _chemical_melting_point ? _chemical_formula_moiety 'C29 H36 I2 N4 Pd,0.5(C H2 Cl2),1.5C H3.5' _chemical_formula_sum 'C31 H40.50 Cl I2 N4 Pd' _chemical_formula_weight 864.82 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' I I -0.4742 1.8119 '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 13.616(9) _cell_length_b 15.293(10) _cell_length_c 18.724(13) _cell_angle_alpha 73.804(12) _cell_angle_beta 73.014(12) _cell_angle_gamma 64.088(12) _cell_volume 3302(4) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 888 _cell_measurement_theta_min 2.668 _cell_measurement_theta_max 25.898 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.740 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1694 _exptl_absorpt_coefficient_mu 2.539 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.455 _exptl_absorpt_correction_T_max 0.831 _exptl_absorpt_process_details ; absorption correction based on 11369 reflections(SADABS);Rint 0.1949 before correction and 0.0702 after. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 Apex 2000 CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25832 _diffrn_reflns_av_R_equivalents 0.0875 _diffrn_reflns_av_sigmaI/netI 0.1003 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.70 _diffrn_reflns_theta_max 26.00 _reflns_number_total 12785 _reflns_number_gt 8932 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Disordered CH2Cl2 and C6H14 were omitted using the SQUEEZE option of PLATON. The solvent accessible voids are 325.1 A3 with an estimated 144e/cell to be added. Two solvent CH2Cl2 molecules and one C6H14 molecule/unit cell accounting for 134e were included in the formula, FWt, (000) and density calculations. PLATON Reference: Spek, A.L. (1990), Acta Cryst. A46, C-34. 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^)+(0.0660P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12785 _refine_ls_number_parameters 661 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0825 _refine_ls_R_factor_gt 0.0589 _refine_ls_wR_factor_ref 0.1428 _refine_ls_wR_factor_gt 0.1341 _refine_ls_goodness_of_fit_ref 0.952 _refine_ls_restrained_S_all 0.952 _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 0.40086(4) 0.78734(4) 0.05615(3) 0.03167(14) Uani 1 1 d . . . I1 I 0.44111(5) 0.76693(4) 0.18807(3) 0.04559(15) Uani 1 1 d . . . I2 I 0.34205(4) 0.79100(3) -0.06555(3) 0.04152(14) Uani 1 1 d . . . N1 N 0.7255(5) 0.5141(4) 0.1352(3) 0.0363(14) Uani 1 1 d . . . H1 H 0.6592 0.5151 0.1595 0.044 Uiso 1 1 calc R . . N2 N 0.5501(4) 0.5763(4) 0.0603(3) 0.0291(12) Uani 1 1 d . . . N3 N 0.3821(4) 0.5916(4) 0.1126(3) 0.0320(13) Uani 1 1 d . . . N4 N 0.3619(5) 0.9415(4) 0.0272(3) 0.0336(13) Uani 1 1 d . . . C1 C 0.4456(6) 0.6438(5) 0.0786(4) 0.0334(16) Uani 1 1 d . . . C2 C 0.5507(6) 0.4823(5) 0.0827(4) 0.0351(16) Uani 1 1 d . . . H2 H 0.6132 0.4224 0.0755 0.042 Uiso 1 1 calc R . . C3 C 0.4466(6) 0.4916(5) 0.1165(4) 0.0364(17) Uani 1 1 d . . . H3 H 0.4213 0.4393 0.1391 0.044 Uiso 1 1 calc R . . C4 C 0.6494(5) 0.5954(5) 0.0215(4) 0.0303(15) Uani 1 1 d . . . C5 C 0.6586(6) 0.6447(5) -0.0515(4) 0.0392(17) Uani 1 1 d . . . H5 H 0.5957 0.6737 -0.0750 0.047 Uiso 1 1 calc R . . C6 C 0.7575(6) 0.6534(5) -0.0920(4) 0.0383(17) Uani 1 1 d . . . H6 H 0.7638 0.6873 -0.1430 0.046 Uiso 1 1 calc R . . C7 C 0.8465(6) 0.6113(5) -0.0561(4) 0.0425(19) Uani 1 1 d . . . H7 H 0.9160 0.6141 -0.0838 0.051 Uiso 1 1 calc R . . C8 C 0.8381(6) 0.5654(5) 0.0183(4) 0.0385(17) Uani 1 1 d . . . H8 H 0.9008 0.5387 0.0418 0.046 Uiso 1 1 calc R . . C9 C 0.7388(6) 0.5576(5) 0.0595(4) 0.0321(16) Uani 1 1 d . . . C10 C 0.2637(6) 0.6341(6) 0.1441(5) 0.050(2) Uani 1 1 d . . . H10 H 0.2405 0.7072 0.1366 0.060 Uiso 1 1 calc R . . C11 C 0.1979(7) 0.6142(7) 0.1013(6) 0.068(3) Uani 1 1 d . . . H11A H 0.2246 0.6298 0.0466 0.102 Uiso 1 1 calc R . . H11B H 0.1187 0.6556 0.1144 0.102 Uiso 1 1 calc R . . H11C H 0.2083 0.5444 0.1154 0.102 Uiso 1 1 calc R . . C12 C 0.2395(9) 0.5962(9) 0.2284(6) 0.090(4) Uani 1 1 d . . . H12A H 0.2618 0.5244 0.2372 0.135 Uiso 1 1 calc R . . H12B H 0.1597 0.6275 0.2485 0.135 Uiso 1 1 calc R . . H12C H 0.2815 0.6120 0.2540 0.135 Uiso 1 1 calc R . . C13 C 0.8153(6) 0.4673(5) 0.1758(4) 0.0366(17) Uani 1 1 d . . . C14 C 0.8696(6) 0.3663(6) 0.1847(4) 0.0398(18) Uani 1 1 d . . . C15 C 0.9547(7) 0.3211(6) 0.2258(5) 0.051(2) Uani 1 1 d . . . H15 H 0.9940 0.2515 0.2317 0.061 Uiso 1 1 calc R . . C16 C 0.9826(8) 0.3751(7) 0.2577(5) 0.058(2) Uani 1 1 d . . . H16 H 1.0399 0.3430 0.2865 0.070 Uiso 1 1 calc R . . C17 C 0.9273(8) 0.4762(7) 0.2481(5) 0.056(2) Uani 1 1 d . . . H17 H 0.9480 0.5135 0.2697 0.067 Uiso 1 1 calc R . . C18 C 0.8426(7) 0.5243(6) 0.2079(5) 0.048(2) Uani 1 1 d . . . C19 C 0.7817(8) 0.6363(7) 0.1993(6) 0.069(3) Uani 1 1 d . . . H19 H 0.7267 0.6574 0.1661 0.083 Uiso 1 1 calc R . . C20 C 0.7170(10) 0.6678(9) 0.2765(7) 0.097(4) Uani 1 1 d . . . H20A H 0.6666 0.6331 0.3007 0.146 Uiso 1 1 calc R . . H20B H 0.6736 0.7392 0.2688 0.146 Uiso 1 1 calc R . . H20C H 0.7695 0.6512 0.3092 0.146 Uiso 1 1 calc R . . C21 C 0.8633(10) 0.6871(8) 0.1607(7) 0.090(4) Uani 1 1 d . . . H21A H 0.9145 0.6716 0.1940 0.135 Uiso 1 1 calc R . . H21B H 0.8219 0.7587 0.1503 0.135 Uiso 1 1 calc R . . H21C H 0.9058 0.6635 0.1129 0.135 Uiso 1 1 calc R . . C22 C 0.8422(6) 0.3025(6) 0.1508(5) 0.0444(19) Uani 1 1 d . . . H22 H 0.7828 0.3481 0.1213 0.053 Uiso 1 1 calc R . . C23 C 0.7920(7) 0.2378(6) 0.2146(5) 0.057(2) Uani 1 1 d . . . H23A H 0.8468 0.1937 0.2463 0.086 Uiso 1 1 calc R . . H23B H 0.7714 0.1983 0.1927 0.086 Uiso 1 1 calc R . . H23C H 0.7255 0.2797 0.2455 0.086 Uiso 1 1 calc R . . C24 C 0.9391(8) 0.2439(7) 0.0961(5) 0.067(3) Uani 1 1 d . . . H24A H 0.9638 0.2893 0.0540 0.101 Uiso 1 1 calc R . . H24B H 0.9158 0.2046 0.0763 0.101 Uiso 1 1 calc R . . H24C H 1.0006 0.2000 0.1224 0.101 Uiso 1 1 calc R . . C25 C 0.2910(6) 1.0031(5) 0.0746(4) 0.0387(17) Uani 1 1 d . . . H25 H 0.2559 0.9777 0.1225 0.046 Uiso 1 1 calc R . . C26 C 0.2672(6) 1.1050(6) 0.0549(5) 0.046(2) Uani 1 1 d . . . H26 H 0.2153 1.1483 0.0887 0.055 Uiso 1 1 calc R . . C27 C 0.3191(7) 1.1405(6) -0.0127(5) 0.047(2) Uani 1 1 d . . . H27 H 0.3065 1.2087 -0.0257 0.057 Uiso 1 1 calc R . . C28 C 0.3907(6) 1.0771(5) -0.0628(4) 0.0407(18) Uani 1 1 d . . . H28 H 0.4249 1.1013 -0.1117 0.049 Uiso 1 1 calc R . . C29 C 0.4107(6) 0.9788(5) -0.0400(4) 0.0395(17) Uani 1 1 d . . . H29 H 0.4617 0.9347 -0.0735 0.047 Uiso 1 1 calc R . . Pd1A Pd 0.99870(4) 0.88700(4) 0.31408(3) 0.03408(15) Uani 1 1 d . . . I1A I 0.93294(5) 0.74171(4) 0.35879(3) 0.05415(17) Uani 1 1 d . . . I2A I 1.09045(4) 1.01600(4) 0.27261(3) 0.04252(14) Uani 1 1 d . . . N1A N 0.7615(5) 0.8526(4) 0.5755(3) 0.0390(14) Uani 1 1 d . . . H1A H 0.8312 0.8210 0.5812 0.047 Uiso 1 1 calc R . . N2A N 0.9324(5) 0.9068(4) 0.4764(3) 0.0336(13) Uani 1 1 d . . . N3A N 1.1079(5) 0.8228(5) 0.4467(3) 0.0380(14) Uani 1 1 d . . . N4A N 0.9721(5) 0.9079(4) 0.2053(3) 0.0356(14) Uani 1 1 d . . . C1A C 1.0163(6) 0.8683(5) 0.4193(4) 0.0367(17) Uani 1 1 d . . . C2A C 0.9760(6) 0.8812(6) 0.5407(4) 0.0383(17) Uani 1 1 d . . . H2A H 0.9359 0.8981 0.5890 0.046 Uiso 1 1 calc R . . C3A C 1.0837(7) 0.8290(6) 0.5226(4) 0.0446(19) Uani 1 1 d . . . H3A H 1.1352 0.8007 0.5557 0.054 Uiso 1 1 calc R . . C4A C 0.8190(6) 0.9658(5) 0.4710(4) 0.0339(16) Uani 1 1 d . . . C5A C 0.7954(7) 1.0492(6) 0.4155(4) 0.0429(19) Uani 1 1 d . . . H5A H 0.8547 1.0657 0.3822 0.051 Uiso 1 1 calc R . . C6A C 0.6854(6) 1.1098(6) 0.4077(5) 0.0461(19) Uani 1 1 d . . . H6A H 0.6687 1.1666 0.3691 0.055 Uiso 1 1 calc R . . C7A C 0.6015(7) 1.0830(6) 0.4589(5) 0.049(2) Uani 1 1 d . . . H7A H 0.5259 1.1238 0.4562 0.059 Uiso 1 1 calc R . . C8A C 0.6255(6) 0.9991(6) 0.5132(4) 0.0412(18) Uani 1 1 d . . . H8A H 0.5664 0.9825 0.5467 0.049 Uiso 1 1 calc R . . C9A C 0.7342(6) 0.9385(6) 0.5199(4) 0.0391(17) Uani 1 1 d . . . C10A C 1.2198(7) 0.7674(6) 0.4036(5) 0.053(2) Uani 1 1 d . . . H10A H 1.2152 0.7865 0.3487 0.064 Uiso 1 1 calc R . . C11A C 1.3049(7) 0.7989(8) 0.4123(5) 0.070(3) Uani 1 1 d . . . H11D H 1.2784 0.8711 0.4005 0.106 Uiso 1 1 calc R . . H11E H 1.3751 0.7704 0.3774 0.106 Uiso 1 1 calc R . . H11F H 1.3169 0.7759 0.4646 0.106 Uiso 1 1 calc R . . C12A C 1.2459(8) 0.6584(7) 0.4255(6) 0.078(3) Uani 1 1 d . . . H12D H 1.2532 0.6365 0.4788 0.117 Uiso 1 1 calc R . . H12E H 1.3159 0.6227 0.3934 0.117 Uiso 1 1 calc R . . H12F H 1.1855 0.6448 0.4186 0.117 Uiso 1 1 calc R . . C13A C 0.6793(6) 0.8142(5) 0.6237(4) 0.0403(18) Uani 1 1 d . . . C14A C 0.6036(6) 0.8614(6) 0.6826(4) 0.0435(19) Uani 1 1 d . . . C15A C 0.5289(7) 0.8207(6) 0.7290(5) 0.049(2) Uani 1 1 d . . . H15A H 0.4756 0.8535 0.7686 0.059 Uiso 1 1 calc R . . C16A C 0.5290(7) 0.7358(7) 0.7202(5) 0.058(2) Uani 1 1 d . . . H16A H 0.4758 0.7102 0.7523 0.070 Uiso 1 1 calc R . . C17A C 0.6089(8) 0.6863(6) 0.6629(5) 0.058(2) Uani 1 1 d . . . H17A H 0.6129 0.6244 0.6584 0.070 Uiso 1 1 calc R . . C18A C 0.6821(7) 0.7263(6) 0.6127(4) 0.047(2) Uani 1 1 d . . . C19A C 0.7690(9) 0.6731(7) 0.5491(5) 0.067(3) Uani 1 1 d . . . H19A H 0.7871 0.7244 0.5074 0.081 Uiso 1 1 calc R . . C20A C 0.8778(10) 0.6016(9) 0.5779(7) 0.113(5) Uani 1 1 d . . . H20D H 0.8614 0.5538 0.6218 0.169 Uiso 1 1 calc R . . H20E H 0.9089 0.6394 0.5927 0.169 Uiso 1 1 calc R . . H20F H 0.9318 0.5666 0.5374 0.169 Uiso 1 1 calc R . . C21A C 0.7260(13) 0.6204(10) 0.5162(7) 0.118(5) Uani 1 1 d . . . H21D H 0.6939 0.5790 0.5573 0.176 Uiso 1 1 calc R . . H21E H 0.7875 0.5790 0.4821 0.176 Uiso 1 1 calc R . . H21F H 0.6687 0.6691 0.4877 0.176 Uiso 1 1 calc R . . C22A C 0.6035(7) 0.9529(6) 0.7008(5) 0.050(2) Uani 1 1 d . . . H22A H 0.6547 0.9775 0.6581 0.059 Uiso 1 1 calc R . . C23A C 0.6489(8) 0.9247(7) 0.7723(5) 0.068(3) Uani 1 1 d . . . H23D H 0.5967 0.9060 0.8158 0.102 Uiso 1 1 calc R . . H23E H 0.6586 0.9810 0.7801 0.102 Uiso 1 1 calc R . . H23F H 0.7210 0.8688 0.7673 0.102 Uiso 1 1 calc R . . C24A C 0.4893(9) 1.0367(7) 0.7093(6) 0.082(3) Uani 1 1 d . . . H24D H 0.4360 1.0128 0.7478 0.123 Uiso 1 1 calc R . . H24E H 0.4646 1.0605 0.6607 0.123 Uiso 1 1 calc R . . H24F H 0.4936 1.0909 0.7248 0.123 Uiso 1 1 calc R . . C25A C 1.0563(6) 0.8862(5) 0.1459(4) 0.0399(18) Uani 1 1 d . . . H25A H 1.1299 0.8680 0.1522 0.048 Uiso 1 1 calc R . . C26A C 1.0399(8) 0.8893(6) 0.0760(5) 0.054(2) Uani 1 1 d . . . H26A H 1.1015 0.8709 0.0353 0.065 Uiso 1 1 calc R . . C27A C 0.9346(8) 0.9190(6) 0.0656(5) 0.055(2) Uani 1 1 d . . . H27A H 0.9216 0.9232 0.0174 0.066 Uiso 1 1 calc R . . C28A C 0.8461(8) 0.9431(6) 0.1265(5) 0.054(2) Uani 1 1 d . . . H28A H 0.7718 0.9637 0.1208 0.065 Uiso 1 1 calc R . . C29A C 0.8687(7) 0.9365(6) 0.1956(5) 0.050(2) Uani 1 1 d . . . H29A H 0.8086 0.9529 0.2375 0.060 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.0303(3) 0.0241(3) 0.0410(3) -0.0106(2) -0.0025(2) -0.0107(2) I1 0.0611(3) 0.0406(3) 0.0403(3) -0.0117(2) -0.0053(2) -0.0246(3) I2 0.0457(3) 0.0324(3) 0.0498(3) -0.0079(2) -0.0155(2) -0.0138(2) N1 0.029(3) 0.040(4) 0.045(4) -0.005(3) -0.008(3) -0.019(3) N2 0.029(3) 0.030(3) 0.035(3) -0.010(3) -0.004(2) -0.016(3) N3 0.026(3) 0.033(3) 0.039(3) -0.010(3) -0.003(3) -0.012(3) N4 0.032(3) 0.030(3) 0.036(3) -0.010(3) -0.001(3) -0.010(3) C1 0.032(4) 0.032(4) 0.042(4) -0.020(3) -0.001(3) -0.013(3) C2 0.041(4) 0.023(4) 0.045(4) -0.016(3) -0.009(3) -0.010(3) C3 0.037(4) 0.024(4) 0.053(5) -0.006(3) -0.010(4) -0.016(3) C4 0.030(4) 0.028(4) 0.036(4) -0.009(3) 0.000(3) -0.016(3) C5 0.039(4) 0.031(4) 0.046(5) -0.012(3) -0.012(4) -0.007(3) C6 0.044(4) 0.030(4) 0.040(4) -0.007(3) -0.004(4) -0.015(3) C7 0.041(4) 0.037(4) 0.048(5) -0.011(4) 0.004(4) -0.020(4) C8 0.033(4) 0.037(4) 0.049(5) -0.011(4) -0.010(3) -0.014(3) C9 0.037(4) 0.026(4) 0.039(4) -0.010(3) -0.009(3) -0.013(3) C10 0.028(4) 0.043(5) 0.079(6) -0.023(4) 0.008(4) -0.017(4) C11 0.033(5) 0.061(6) 0.110(8) -0.021(6) -0.005(5) -0.021(4) C12 0.069(7) 0.126(10) 0.056(7) -0.014(7) 0.012(5) -0.038(7) C13 0.035(4) 0.042(4) 0.034(4) -0.008(3) -0.002(3) -0.018(3) C14 0.040(4) 0.048(5) 0.039(4) -0.004(4) -0.014(3) -0.021(4) C15 0.064(6) 0.039(5) 0.053(5) 0.003(4) -0.024(4) -0.022(4) C16 0.066(6) 0.072(7) 0.053(5) -0.004(5) -0.026(5) -0.036(5) C17 0.067(6) 0.059(6) 0.062(6) -0.015(5) -0.029(5) -0.029(5) C18 0.056(5) 0.043(5) 0.050(5) -0.004(4) -0.016(4) -0.024(4) C19 0.067(6) 0.055(6) 0.103(8) -0.038(6) -0.036(6) -0.012(5) C20 0.093(9) 0.110(10) 0.106(9) -0.068(8) -0.016(7) -0.027(7) C21 0.101(9) 0.062(7) 0.129(10) 0.011(7) -0.053(8) -0.049(7) C22 0.046(5) 0.042(5) 0.055(5) -0.008(4) -0.026(4) -0.016(4) C23 0.062(6) 0.054(5) 0.060(6) -0.006(5) -0.013(5) -0.028(5) C24 0.061(6) 0.077(7) 0.064(6) -0.040(5) -0.002(5) -0.017(5) C25 0.039(4) 0.029(4) 0.050(5) -0.013(4) -0.004(3) -0.013(3) C26 0.043(4) 0.038(5) 0.059(5) -0.023(4) -0.003(4) -0.013(4) C27 0.062(5) 0.026(4) 0.059(5) -0.005(4) -0.026(4) -0.015(4) C28 0.047(5) 0.037(4) 0.040(4) 0.005(4) -0.011(4) -0.024(4) C29 0.038(4) 0.041(4) 0.044(4) -0.011(4) -0.001(3) -0.022(4) Pd1A 0.0352(3) 0.0391(3) 0.0300(3) -0.0108(2) -0.0028(2) -0.0157(3) I1A 0.0706(4) 0.0607(4) 0.0470(3) -0.0150(3) -0.0016(3) -0.0425(3) I2A 0.0472(3) 0.0463(3) 0.0375(3) -0.0112(2) 0.0010(2) -0.0247(2) N1A 0.035(3) 0.034(3) 0.043(4) -0.001(3) -0.003(3) -0.015(3) N2A 0.037(3) 0.035(3) 0.030(3) -0.013(3) 0.004(3) -0.017(3) N3A 0.036(3) 0.048(4) 0.033(3) -0.007(3) -0.004(3) -0.021(3) N4A 0.029(3) 0.035(3) 0.042(4) -0.009(3) -0.010(3) -0.009(3) C1A 0.044(4) 0.042(4) 0.034(4) -0.013(3) -0.005(3) -0.023(4) C2A 0.044(4) 0.051(5) 0.030(4) -0.009(3) -0.007(3) -0.027(4) C3A 0.049(5) 0.057(5) 0.034(4) -0.006(4) -0.016(4) -0.022(4) C4A 0.042(4) 0.032(4) 0.031(4) -0.010(3) 0.004(3) -0.021(3) C5A 0.049(5) 0.046(5) 0.042(4) -0.015(4) 0.001(4) -0.027(4) C6A 0.046(5) 0.049(5) 0.045(5) -0.001(4) -0.009(4) -0.024(4) C7A 0.042(5) 0.044(5) 0.060(5) -0.006(4) -0.011(4) -0.017(4) C8A 0.037(4) 0.046(5) 0.040(4) -0.003(4) -0.001(3) -0.022(4) C9A 0.040(4) 0.044(4) 0.041(4) -0.013(4) -0.002(3) -0.024(4) C10A 0.045(5) 0.052(5) 0.055(5) -0.015(4) -0.014(4) -0.006(4) C11A 0.046(5) 0.102(8) 0.059(6) -0.029(6) 0.009(4) -0.028(5) C12A 0.063(6) 0.075(7) 0.082(8) -0.027(6) -0.016(6) -0.005(6) C13A 0.044(4) 0.032(4) 0.046(4) -0.010(4) -0.001(4) -0.019(4) C14A 0.043(4) 0.040(4) 0.043(4) -0.007(4) 0.002(4) -0.019(4) C15A 0.055(5) 0.050(5) 0.045(5) -0.011(4) 0.003(4) -0.030(4) C16A 0.058(6) 0.068(6) 0.053(5) 0.006(5) -0.005(4) -0.042(5) C17A 0.075(6) 0.043(5) 0.067(6) -0.004(5) -0.016(5) -0.035(5) C18A 0.060(5) 0.043(5) 0.042(5) -0.001(4) -0.009(4) -0.029(4) C19A 0.096(8) 0.050(6) 0.052(6) -0.014(5) 0.007(5) -0.034(6) C20A 0.103(9) 0.096(9) 0.069(8) -0.020(7) 0.013(7) 0.010(8) C21A 0.186(15) 0.113(10) 0.098(10) -0.048(8) -0.009(9) -0.092(11) C22A 0.056(5) 0.051(5) 0.042(5) -0.013(4) 0.007(4) -0.028(4) C23A 0.075(7) 0.081(7) 0.062(6) -0.023(5) 0.000(5) -0.044(6) C24A 0.091(8) 0.063(7) 0.092(8) -0.040(6) -0.026(6) -0.009(6) C25A 0.038(4) 0.044(5) 0.037(4) -0.009(4) -0.005(3) -0.016(4) C26A 0.068(6) 0.055(5) 0.038(5) -0.013(4) -0.014(4) -0.018(5) C27A 0.082(7) 0.046(5) 0.034(5) 0.003(4) -0.023(5) -0.023(5) C28A 0.061(6) 0.043(5) 0.070(6) 0.003(4) -0.038(5) -0.022(4) C29A 0.050(5) 0.053(5) 0.053(5) -0.010(4) -0.009(4) -0.026(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 C1 1.957(7) . ? Pd1 N4 2.121(6) . ? Pd1 I1 2.5902(18) . ? Pd1 I2 2.6063(17) . ? N1 C9 1.385(9) . ? N1 C13 1.435(9) . ? N1 H1 0.8800 . ? N2 C1 1.355(8) . ? N2 C2 1.378(8) . ? N2 C4 1.447(8) . ? N3 C1 1.337(8) . ? N3 C3 1.385(9) . ? N3 C10 1.453(9) . ? N4 C25 1.334(8) . ? N4 C29 1.337(9) . ? C2 C3 1.335(10) . ? C2 H2 0.9500 . ? C3 H3 0.9500 . ? C4 C5 1.364(10) . ? C4 C9 1.408(9) . ? C5 C6 1.382(10) . ? C5 H5 0.9500 . ? C6 C7 1.373(10) . ? C6 H6 0.9500 . ? C7 C8 1.372(10) . ? C7 H7 0.9500 . ? C8 C9 1.385(10) . ? C8 H8 0.9500 . ? C10 C12 1.512(12) . ? C10 C11 1.527(11) . ? C10 H10 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.375(10) . ? C13 C18 1.401(10) . ? C14 C15 1.390(10) . ? C14 C22 1.516(9) . ? C15 C16 1.367(11) . ? C15 H15 0.9500 . ? C16 C17 1.377(12) . ? C16 H16 0.9500 . ? C17 C18 1.376(11) . ? C17 H17 0.9500 . ? C18 C19 1.526(12) . ? C19 C21 1.527(14) . ? C19 C20 1.540(14) . ? C19 H19 1.0000 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 C24 1.511(11) . ? C22 C23 1.526(11) . ? C22 H22 1.0000 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C26 1.406(10) . ? C25 H25 0.9500 . ? C26 C27 1.351(11) . ? C26 H26 0.9500 . ? C27 C28 1.386(11) . ? C27 H27 0.9500 . ? C28 C29 1.368(10) . ? C28 H28 0.9500 . ? C29 H29 0.9500 . ? Pd1A C1A 1.981(7) . ? Pd1A N4A 2.086(6) . ? Pd1A I1A 2.5889(16) . ? Pd1A I2A 2.6054(15) . ? N1A C9A 1.409(9) . ? N1A C13A 1.450(9) . ? N1A H1A 0.8800 . ? N2A C1A 1.358(9) . ? N2A C2A 1.381(9) . ? N2A C4A 1.426(9) . ? N3A C1A 1.310(9) . ? N3A C3A 1.384(9) . ? N3A C10A 1.491(10) . ? N4A C29A 1.331(9) . ? N4A C25A 1.338(9) . ? C2A C3A 1.319(10) . ? C2A H2A 0.9500 . ? C3A H3A 0.9500 . ? C4A C5A 1.380(10) . ? C4A C9A 1.392(9) . ? C5A C6A 1.402(11) . ? C5A H5A 0.9500 . ? C6A C7A 1.393(11) . ? C6A H6A 0.9500 . ? C7A C8A 1.373(11) . ? C7A H7A 0.9500 . ? C8A C9A 1.381(10) . ? C8A H8A 0.9500 . ? C10A C11A 1.498(12) . ? C10A C12A 1.504(12) . ? C10A H10A 1.0000 . ? C11A H11D 0.9800 . ? C11A H11E 0.9800 . ? C11A H11F 0.9800 . ? C12A H12D 0.9800 . ? C12A H12E 0.9800 . ? C12A H12F 0.9800 . ? C13A C14A 1.389(10) . ? C13A C18A 1.398(10) . ? C14A C15A 1.383(11) . ? C14A C22A 1.530(10) . ? C15A C16A 1.353(11) . ? C15A H15A 0.9500 . ? C16A C17A 1.399(12) . ? C16A H16A 0.9500 . ? C17A C18A 1.385(11) . ? C17A H17A 0.9500 . ? C18A C19A 1.535(12) . ? C19A C21A 1.507(13) . ? C19A C20A 1.550(15) . ? C19A H19A 1.0000 . ? C20A H20D 0.9800 . ? C20A H20E 0.9800 . ? C20A H20F 0.9800 . ? C21A H21D 0.9800 . ? C21A H21E 0.9800 . ? C21A H21F 0.9800 . ? C22A C23A 1.513(12) . ? C22A C24A 1.521(12) . ? C22A H22A 1.0000 . ? C23A H23D 0.9800 . ? C23A H23E 0.9800 . ? C23A H23F 0.9800 . ? C24A H24D 0.9800 . ? C24A H24E 0.9800 . ? C24A H24F 0.9800 . ? C25A C26A 1.376(11) . ? C25A H25A 0.9500 . ? C26A C27A 1.357(12) . ? C26A H26A 0.9500 . ? C27A C28A 1.390(12) . ? C27A H27A 0.9500 . ? C28A C29A 1.382(11) . ? C28A H28A 0.9500 . ? C29A H29A 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 C1 Pd1 N4 176.5(3) . . ? C1 Pd1 I1 85.4(2) . . ? N4 Pd1 I1 95.52(15) . . ? C1 Pd1 I2 88.7(2) . . ? N4 Pd1 I2 90.74(15) . . ? I1 Pd1 I2 170.99(3) . . ? C9 N1 C13 122.8(6) . . ? C9 N1 H1 118.6 . . ? C13 N1 H1 118.6 . . ? C1 N2 C2 110.2(5) . . ? C1 N2 C4 127.2(6) . . ? C2 N2 C4 122.5(6) . . ? C1 N3 C3 110.1(6) . . ? C1 N3 C10 124.6(6) . . ? C3 N3 C10 125.2(6) . . ? C25 N4 C29 118.4(6) . . ? C25 N4 Pd1 121.9(5) . . ? C29 N4 Pd1 119.6(5) . . ? N3 C1 N2 105.5(6) . . ? N3 C1 Pd1 128.6(5) . . ? N2 C1 Pd1 125.8(5) . . ? C3 C2 N2 106.8(6) . . ? C3 C2 H2 126.6 . . ? N2 C2 H2 126.6 . . ? C2 C3 N3 107.3(6) . . ? C2 C3 H3 126.4 . . ? N3 C3 H3 126.4 . . ? C5 C4 C9 120.5(6) . . ? C5 C4 N2 120.9(6) . . ? C9 C4 N2 118.5(6) . . ? C4 C5 C6 121.4(7) . . ? C4 C5 H5 119.3 . . ? C6 C5 H5 119.3 . . ? C7 C6 C5 117.8(7) . . ? C7 C6 H6 121.1 . . ? C5 C6 H6 121.1 . . ? C8 C7 C6 122.1(7) . . ? C8 C7 H7 119.0 . . ? C6 C7 H7 119.0 . . ? C7 C8 C9 120.3(7) . . ? C7 C8 H8 119.9 . . ? C9 C8 H8 119.9 . . ? C8 C9 N1 122.4(6) . . ? C8 C9 C4 117.7(7) . . ? N1 C9 C4 119.9(6) . . ? N3 C10 C12 111.1(7) . . ? N3 C10 C11 110.0(7) . . ? C12 C10 C11 111.9(8) . . ? N3 C10 H10 107.9 . . ? C12 C10 H10 107.9 . . ? C11 C10 H10 107.9 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C14 C13 C18 121.7(7) . . ? C14 C13 N1 118.5(6) . . ? C18 C13 N1 119.8(7) . . ? C13 C14 C15 118.3(7) . . ? C13 C14 C22 123.0(7) . . ? C15 C14 C22 118.6(7) . . ? C16 C15 C14 121.1(8) . . ? C16 C15 H15 119.5 . . ? C14 C15 H15 119.5 . . ? C15 C16 C17 119.7(8) . . ? C15 C16 H16 120.1 . . ? C17 C16 H16 120.1 . . ? C18 C17 C16 121.3(7) . . ? C18 C17 H17 119.3 . . ? C16 C17 H17 119.3 . . ? C17 C18 C13 117.9(7) . . ? C17 C18 C19 120.0(7) . . ? C13 C18 C19 122.0(7) . . ? C18 C19 C21 110.5(8) . . ? C18 C19 C20 111.2(9) . . ? C21 C19 C20 111.1(8) . . ? C18 C19 H19 108.0 . . ? C21 C19 H19 108.0 . . ? C20 C19 H19 108.0 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C24 C22 C14 113.7(7) . . ? C24 C22 C23 112.8(7) . . ? C14 C22 C23 109.3(7) . . ? C24 C22 H22 106.9 . . ? C14 C22 H22 106.9 . . ? C23 C22 H22 106.9 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N4 C25 C26 121.2(7) . . ? N4 C25 H25 119.4 . . ? C26 C25 H25 119.4 . . ? C27 C26 C25 119.2(7) . . ? C27 C26 H26 120.4 . . ? C25 C26 H26 120.4 . . ? C26 C27 C28 119.8(7) . . ? C26 C27 H27 120.1 . . ? C28 C27 H27 120.1 . . ? C29 C28 C27 118.0(7) . . ? C29 C28 H28 121.0 . . ? C27 C28 H28 121.0 . . ? N4 C29 C28 123.3(7) . . ? N4 C29 H29 118.3 . . ? C28 C29 H29 118.3 . . ? C1A Pd1A N4A 177.2(3) . . ? C1A Pd1A I1A 87.7(2) . . ? N4A Pd1A I1A 90.87(16) . . ? C1A Pd1A I2A 89.3(2) . . ? N4A Pd1A I2A 92.43(16) . . ? I1A Pd1A I2A 172.43(3) . . ? C9A N1A C13A 122.5(6) . . ? C9A N1A H1A 118.7 . . ? C13A N1A H1A 118.7 . . ? C1A N2A C2A 108.4(6) . . ? C1A N2A C4A 126.2(6) . . ? C2A N2A C4A 125.4(6) . . ? C1A N3A C3A 109.6(6) . . ? C1A N3A C10A 125.0(6) . . ? C3A N3A C10A 125.2(6) . . ? C29A N4A C25A 118.8(7) . . ? C29A N4A Pd1A 119.0(5) . . ? C25A N4A Pd1A 122.0(5) . . ? N3A C1A N2A 107.1(6) . . ? N3A C1A Pd1A 128.3(5) . . ? N2A C1A Pd1A 124.5(5) . . ? C3A C2A N2A 107.4(6) . . ? C3A C2A H2A 126.3 . . ? N2A C2A H2A 126.3 . . ? C2A C3A N3A 107.5(7) . . ? C2A C3A H3A 126.3 . . ? N3A C3A H3A 126.3 . . ? C5A C4A C9A 120.9(7) . . ? C5A C4A N2A 118.7(6) . . ? C9A C4A N2A 120.4(7) . . ? C4A C5A C6A 121.0(7) . . ? C4A C5A H5A 119.5 . . ? C6A C5A H5A 119.5 . . ? C7A C6A C5A 117.1(8) . . ? C7A C6A H6A 121.4 . . ? C5A C6A H6A 121.4 . . ? C8A C7A C6A 121.5(8) . . ? C8A C7A H7A 119.2 . . ? C6A C7A H7A 119.2 . . ? C7A C8A C9A 121.2(7) . . ? C7A C8A H8A 119.4 . . ? C9A C8A H8A 119.4 . . ? C8A C9A C4A 118.1(7) . . ? C8A C9A N1A 122.6(6) . . ? C4A C9A N1A 119.2(7) . . ? N3A C10A C11A 110.2(7) . . ? N3A C10A C12A 109.8(7) . . ? C11A C10A C12A 115.2(8) . . ? N3A C10A H10A 107.1 . . ? C11A C10A H10A 107.1 . . ? C12A C10A H10A 107.1 . . ? C10A C11A H11D 109.5 . . ? C10A C11A H11E 109.5 . . ? H11D C11A H11E 109.5 . . ? C10A C11A H11F 109.5 . . ? H11D C11A H11F 109.5 . . ? H11E C11A H11F 109.5 . . ? C10A C12A H12D 109.5 . . ? C10A C12A H12E 109.5 . . ? H12D C12A H12E 109.5 . . ? C10A C12A H12F 109.5 . . ? H12D C12A H12F 109.5 . . ? H12E C12A H12F 109.5 . . ? C14A C13A C18A 121.0(7) . . ? C14A C13A N1A 120.0(6) . . ? C18A C13A N1A 118.9(7) . . ? C15A C14A C13A 118.3(7) . . ? C15A C14A C22A 118.7(7) . . ? C13A C14A C22A 122.9(7) . . ? C16A C15A C14A 122.4(8) . . ? C16A C15A H15A 118.8 . . ? C14A C15A H15A 118.8 . . ? C15A C16A C17A 118.9(8) . . ? C15A C16A H16A 120.5 . . ? C17A C16A H16A 120.5 . . ? C18A C17A C16A 120.9(8) . . ? C18A C17A H17A 119.6 . . ? C16A C17A H17A 119.6 . . ? C17A C18A C13A 118.4(8) . . ? C17A C18A C19A 121.2(7) . . ? C13A C18A C19A 120.3(7) . . ? C21A C19A C18A 112.5(9) . . ? C21A C19A C20A 111.4(10) . . ? C18A C19A C20A 110.1(8) . . ? C21A C19A H19A 107.5 . . ? C18A C19A H19A 107.5 . . ? C20A C19A H19A 107.5 . . ? C19A C20A H20D 109.5 . . ? C19A C20A H20E 109.5 . . ? H20D C20A H20E 109.5 . . ? C19A C20A H20F 109.5 . . ? H20D C20A H20F 109.5 . . ? H20E C20A H20F 109.5 . . ? C19A C21A H21D 109.5 . . ? C19A C21A H21E 109.5 . . ? H21D C21A H21E 109.5 . . ? C19A C21A H21F 109.5 . . ? H21D C21A H21F 109.5 . . ? H21E C21A H21F 109.5 . . ? C23A C22A C24A 109.9(7) . . ? C23A C22A C14A 109.5(7) . . ? C24A C22A C14A 113.5(7) . . ? C23A C22A H22A 107.9 . . ? C24A C22A H22A 107.9 . . ? C14A C22A H22A 107.9 . . ? C22A C23A H23D 109.5 . . ? C22A C23A H23E 109.5 . . ? H23D C23A H23E 109.5 . . ? C22A C23A H23F 109.5 . . ? H23D C23A H23F 109.5 . . ? H23E C23A H23F 109.5 . . ? C22A C24A H24D 109.5 . . ? C22A C24A H24E 109.5 . . ? H24D C24A H24E 109.5 . . ? C22A C24A H24F 109.5 . . ? H24D C24A H24F 109.5 . . ? H24E C24A H24F 109.5 . . ? N4A C25A C26A 122.1(7) . . ? N4A C25A H25A 118.9 . . ? C26A C25A H25A 118.9 . . ? C27A C26A C25A 119.3(8) . . ? C27A C26A H26A 120.3 . . ? C25A C26A H26A 120.3 . . ? C26A C27A C28A 119.2(8) . . ? C26A C27A H27A 120.4 . . ? C28A C27A H27A 120.4 . . ? C29A C28A C27A 118.6(8) . . ? C29A C28A H28A 120.7 . . ? C27A C28A H28A 120.7 . . ? N4A C29A C28A 122.0(8) . . ? N4A C29A H29A 119.0 . . ? C28A C29A H29A 119.0 . . ? 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 I1 Pd1 N4 C25 -48.9(5) . . . . ? I2 Pd1 N4 C25 124.6(5) . . . . ? I1 Pd1 N4 C29 130.1(5) . . . . ? I2 Pd1 N4 C29 -56.4(5) . . . . ? C3 N3 C1 N2 0.7(8) . . . . ? C10 N3 C1 N2 177.8(6) . . . . ? C3 N3 C1 Pd1 179.3(5) . . . . ? C10 N3 C1 Pd1 -3.6(10) . . . . ? C2 N2 C1 N3 0.4(8) . . . . ? C4 N2 C1 N3 179.1(6) . . . . ? C2 N2 C1 Pd1 -178.2(5) . . . . ? C4 N2 C1 Pd1 0.5(10) . . . . ? I1 Pd1 C1 N3 90.5(6) . . . . ? I2 Pd1 C1 N3 -82.6(6) . . . . ? I1 Pd1 C1 N2 -91.2(6) . . . . ? I2 Pd1 C1 N2 95.7(6) . . . . ? C1 N2 C2 C3 -1.4(8) . . . . ? C4 N2 C2 C3 179.9(6) . . . . ? N2 C2 C3 N3 1.7(8) . . . . ? C1 N3 C3 C2 -1.5(8) . . . . ? C10 N3 C3 C2 -178.6(7) . . . . ? C1 N2 C4 C5 -64.0(9) . . . . ? C2 N2 C4 C5 114.6(7) . . . . ? C1 N2 C4 C9 119.2(7) . . . . ? C2 N2 C4 C9 -62.2(8) . . . . ? C9 C4 C5 C6 4.4(10) . . . . ? N2 C4 C5 C6 -172.3(6) . . . . ? C4 C5 C6 C7 -0.5(10) . . . . ? C5 C6 C7 C8 -2.6(11) . . . . ? C6 C7 C8 C9 1.8(11) . . . . ? C7 C8 C9 N1 -178.4(6) . . . . ? C7 C8 C9 C4 2.0(10) . . . . ? C13 N1 C9 C8 -4.6(10) . . . . ? C13 N1 C9 C4 175.1(6) . . . . ? C5 C4 C9 C8 -5.0(10) . . . . ? N2 C4 C9 C8 171.8(6) . . . . ? C5 C4 C9 N1 175.3(6) . . . . ? N2 C4 C9 N1 -7.9(9) . . . . ? C1 N3 C10 C12 -119.3(9) . . . . ? C3 N3 C10 C12 57.4(10) . . . . ? C1 N3 C10 C11 116.2(8) . . . . ? C3 N3 C10 C11 -67.1(10) . . . . ? C9 N1 C13 C14 -98.2(8) . . . . ? C9 N1 C13 C18 84.4(9) . . . . ? C18 C13 C14 C15 -1.0(11) . . . . ? N1 C13 C14 C15 -178.4(7) . . . . ? C18 C13 C14 C22 180.0(7) . . . . ? N1 C13 C14 C22 2.6(11) . . . . ? C13 C14 C15 C16 1.2(12) . . . . ? C22 C14 C15 C16 -179.8(8) . . . . ? C14 C15 C16 C17 -1.2(14) . . . . ? C15 C16 C17 C18 1.2(14) . . . . ? C16 C17 C18 C13 -1.0(13) . . . . ? C16 C17 C18 C19 179.0(9) . . . . ? C14 C13 C18 C17 0.9(12) . . . . ? N1 C13 C18 C17 178.3(7) . . . . ? C14 C13 C18 C19 -179.1(8) . . . . ? N1 C13 C18 C19 -1.7(12) . . . . ? C17 C18 C19 C21 58.9(12) . . . . ? C13 C18 C19 C21 -121.1(9) . . . . ? C17 C18 C19 C20 -64.9(11) . . . . ? C13 C18 C19 C20 115.1(9) . . . . ? C13 C14 C22 C24 119.9(9) . . . . ? C15 C14 C22 C24 -59.1(10) . . . . ? C13 C14 C22 C23 -113.1(8) . . . . ? C15 C14 C22 C23 67.9(9) . . . . ? C29 N4 C25 C26 0.2(11) . . . . ? Pd1 N4 C25 C26 179.1(5) . . . . ? N4 C25 C26 C27 -1.4(12) . . . . ? C25 C26 C27 C28 3.0(12) . . . . ? C26 C27 C28 C29 -3.3(11) . . . . ? C25 N4 C29 C28 -0.6(11) . . . . ? Pd1 N4 C29 C28 -179.6(6) . . . . ? C27 C28 C29 N4 2.2(11) . . . . ? C1A Pd1A N4A C29A 6(5) . . . . ? I1A Pd1A N4A C29A 65.0(5) . . . . ? I2A Pd1A N4A C29A -121.8(5) . . . . ? I1A Pd1A N4A C25A -109.8(5) . . . . ? I2A Pd1A N4A C25A 63.4(5) . . . . ? C3A N3A C1A N2A 1.7(8) . . . . ? C10A N3A C1A N2A 178.1(6) . . . . ? C3A N3A C1A Pd1A 178.4(5) . . . . ? C10A N3A C1A Pd1A -5.2(11) . . . . ? C2A N2A C1A N3A -1.3(8) . . . . ? C4A N2A C1A N3A 177.3(6) . . . . ? C2A N2A C1A Pd1A -178.1(5) . . . . ? C4A N2A C1A Pd1A 0.5(9) . . . . ? I1A Pd1A C1A N3A 100.3(6) . . . . ? I2A Pd1A C1A N3A -72.8(6) . . . . ? I1A Pd1A C1A N2A -83.6(6) . . . . ? I2A Pd1A C1A N2A 103.4(6) . . . . ? C1A N2A C2A C3A 0.3(8) . . . . ? C4A N2A C2A C3A -178.3(6) . . . . ? N2A C2A C3A N3A 0.7(8) . . . . ? C1A N3A C3A C2A -1.6(9) . . . . ? C10A N3A C3A C2A -177.9(7) . . . . ? C1A N2A C4A C5A -53.7(9) . . . . ? C2A N2A C4A C5A 124.6(7) . . . . ? C1A N2A C4A C9A 125.2(7) . . . . ? C2A N2A C4A C9A -56.5(9) . . . . ? C9A C4A C5A C6A 1.1(11) . . . . ? N2A C4A C5A C6A 180.0(6) . . . . ? C4A C5A C6A C7A 1.1(11) . . . . ? C5A C6A C7A C8A -2.1(12) . . . . ? C6A C7A C8A C9A 0.9(12) . . . . ? C7A C8A C9A C4A 1.3(11) . . . . ? C7A C8A C9A N1A 179.2(7) . . . . ? C5A C4A C9A C8A -2.3(10) . . . . ? N2A C4A C9A C8A 178.8(6) . . . . ? C5A C4A C9A N1A 179.7(6) . . . . ? N2A C4A C9A N1A 0.8(10) . . . . ? C13A N1A C9A C8A 8.0(10) . . . . ? C13A N1A C9A C4A -174.0(6) . . . . ? C1A N3A C10A C11A 130.8(8) . . . . ? C3A N3A C10A C11A -53.4(10) . . . . ? C1A N3A C10A C12A -101.3(9) . . . . ? C3A N3A C10A C12A 74.5(10) . . . . ? C9A N1A C13A C14A -74.3(10) . . . . ? C9A N1A C13A C18A 109.6(8) . . . . ? C18A C13A C14A C15A -1.7(12) . . . . ? N1A C13A C14A C15A -177.8(7) . . . . ? C18A C13A C14A C22A 174.9(8) . . . . ? N1A C13A C14A C22A -1.1(12) . . . . ? C13A C14A C15A C16A 1.7(13) . . . . ? C22A C14A C15A C16A -175.1(8) . . . . ? C14A C15A C16A C17A 1.2(14) . . . . ? C15A C16A C17A C18A -4.2(14) . . . . ? C16A C17A C18A C13A 4.2(13) . . . . ? C16A C17A C18A C19A -179.2(9) . . . . ? C14A C13A C18A C17A -1.2(13) . . . . ? N1A C13A C18A C17A 174.9(7) . . . . ? C14A C13A C18A C19A -177.8(8) . . . . ? N1A C13A C18A C19A -1.7(12) . . . . ? C17A C18A C19A C21A 36.0(13) . . . . ? C13A C18A C19A C21A -147.4(9) . . . . ? C17A C18A C19A C20A -88.9(11) . . . . ? C13A C18A C19A C20A 87.7(11) . . . . ? C15A C14A C22A C23A 70.3(10) . . . . ? C13A C14A C22A C23A -106.4(9) . . . . ? C15A C14A C22A C24A -52.9(11) . . . . ? C13A C14A C22A C24A 130.5(9) . . . . ? C29A N4A C25A C26A -2.2(11) . . . . ? Pd1A N4A C25A C26A 172.6(6) . . . . ? N4A C25A C26A C27A 2.6(12) . . . . ? C25A C26A C27A C28A -1.6(13) . . . . ? C26A C27A C28A C29A 0.4(12) . . . . ? C25A N4A C29A C28A 0.9(11) . . . . ? Pd1A N4A C29A C28A -174.0(6) . . . . ? C27A C28A C29A N4A 0.0(12) . . . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 2.244 _refine_diff_density_min -0.858 _refine_diff_density_rms 0.186 #===END data_10070 _database_code_depnum_ccdc_archive 'CCDC 791427' #TrackingRef '- Cross Dalton crystal structure data.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '[C,NH]PtI2py (11)' _chemical_melting_point ? _chemical_formula_moiety 'C29 H36 I2 N4 Pt' _chemical_formula_sum 'C29 H36 I2 N4 Pt' _chemical_formula_weight 889.51 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' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 '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 13.412(3) _cell_length_b 15.242(3) _cell_length_c 18.357(4) _cell_angle_alpha 95.858(4) _cell_angle_beta 104.069(4) _cell_angle_gamma 114.812(4) _cell_volume 3214.0(12) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 1016 _cell_measurement_theta_min 2.484 _cell_measurement_theta_max 21.738 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.838 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1688 _exptl_absorpt_coefficient_mu 6.309 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.518 _exptl_absorpt_correction_T_max 0.831 _exptl_absorpt_process_details ; absorption correction based on 7100 reflections(SADABS);Rint 0.1156 before correction and 0.0454 after. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 Apex 2000 CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25327 _diffrn_reflns_av_R_equivalents 0.0920 _diffrn_reflns_av_sigmaI/netI 0.1514 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.69 _diffrn_reflns_theta_max 26.00 _reflns_number_total 12490 _reflns_number_gt 7475 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0264P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12490 _refine_ls_number_parameters 661 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1104 _refine_ls_R_factor_gt 0.0602 _refine_ls_wR_factor_ref 0.1130 _refine_ls_wR_factor_gt 0.1004 _refine_ls_goodness_of_fit_ref 0.897 _refine_ls_restrained_S_all 0.897 _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 Pt1 Pt 0.88150(4) 0.36141(4) 0.17011(3) 0.03228(14) Uani 1 1 d . . . I1 I 1.10146(7) 0.48520(6) 0.21462(5) 0.0442(2) Uani 1 1 d . . . I2 I 0.66902(7) 0.22294(7) 0.12460(5) 0.0477(3) Uani 1 1 d . . . N1 N 0.6067(7) 0.3358(7) -0.0816(5) 0.033(2) Uani 1 1 d . . . H1 H 0.6385 0.2975 -0.0905 0.039 Uiso 1 1 calc R . . N2 N 0.8313(7) 0.3800(7) 0.0070(5) 0.034(3) Uani 1 1 d . . . N3 N 0.9199(9) 0.2912(8) 0.0272(6) 0.044(3) Uani 1 1 d . . . N4 N 0.8758(8) 0.3872(6) 0.2829(5) 0.032(2) Uani 1 1 d . . . C1 C 0.8823(11) 0.3431(9) 0.0628(7) 0.039(3) Uani 1 1 d . . . C2 C 0.8980(10) 0.2913(10) -0.0496(7) 0.044(3) Uani 1 1 d . . . H2 H 0.9161 0.2576 -0.0868 0.053 Uiso 1 1 calc R . . C3 C 0.8446(11) 0.3501(9) -0.0616(7) 0.045(4) Uani 1 1 d . . . H3 H 0.8210 0.3671 -0.1088 0.055 Uiso 1 1 calc R . . C4 C 0.7849(9) 0.4469(8) 0.0210(6) 0.028(3) Uani 1 1 d . . . C5 C 0.8499(10) 0.5313(8) 0.0795(6) 0.037(3) Uani 1 1 d . . . H5 H 0.9263 0.5465 0.1091 0.045 Uiso 1 1 calc R . . C6 C 0.8040(10) 0.5930(9) 0.0948(6) 0.039(3) Uani 1 1 d . . . H6 H 0.8479 0.6511 0.1355 0.046 Uiso 1 1 calc R . . C7 C 0.6916(10) 0.5704(9) 0.0502(7) 0.040(3) Uani 1 1 d . . . H7 H 0.6600 0.6141 0.0596 0.049 Uiso 1 1 calc R . . C8 C 0.6290(10) 0.4870(9) -0.0056(6) 0.032(3) Uani 1 1 d . . . H8 H 0.5523 0.4720 -0.0342 0.039 Uiso 1 1 calc R . . C9 C 0.6709(9) 0.4221(8) -0.0233(6) 0.027(3) Uani 1 1 d . . . C10 C 0.9756(13) 0.2320(11) 0.0637(8) 0.059(4) Uani 1 1 d . . . H10 H 0.9879 0.2486 0.1203 0.071 Uiso 1 1 calc R . . C11 C 0.8959(15) 0.1215(11) 0.0346(11) 0.106(7) Uani 1 1 d . . . H11A H 0.8299 0.1035 0.0543 0.159 Uiso 1 1 calc R . . H11B H 0.9383 0.0849 0.0528 0.159 Uiso 1 1 calc R . . H11C H 0.8679 0.1047 -0.0219 0.159 Uiso 1 1 calc R . . C12 C 1.0928(12) 0.2625(12) 0.0543(9) 0.074(5) Uani 1 1 d . . . H12A H 1.0838 0.2343 0.0012 0.111 Uiso 1 1 calc R . . H12B H 1.1360 0.2380 0.0903 0.111 Uiso 1 1 calc R . . H12C H 1.1352 0.3352 0.0651 0.111 Uiso 1 1 calc R . . C13 C 0.4908(10) 0.3073(8) -0.1275(7) 0.031(3) Uani 1 1 d . . . C14 C 0.4712(9) 0.3589(8) -0.1848(6) 0.029(3) Uani 1 1 d . . . C15 C 0.3561(10) 0.3271(8) -0.2308(7) 0.036(3) Uani 1 1 d . . . H15 H 0.3408 0.3635 -0.2672 0.043 Uiso 1 1 calc R . . C16 C 0.2661(10) 0.2456(9) -0.2242(7) 0.042(3) Uani 1 1 d . . . H16 H 0.1896 0.2226 -0.2578 0.051 Uiso 1 1 calc R . . C17 C 0.2891(11) 0.1964(9) -0.1666(7) 0.047(4) Uani 1 1 d . . . H17 H 0.2261 0.1406 -0.1612 0.056 Uiso 1 1 calc R . . C18 C 0.3978(10) 0.2250(9) -0.1179(6) 0.038(3) Uani 1 1 d . . . C19 C 0.5640(10) 0.4467(9) -0.2001(7) 0.043(3) Uani 1 1 d . . . H19 H 0.6386 0.4637 -0.1597 0.052 Uiso 1 1 calc R . . C20 C 0.5466(12) 0.5407(10) -0.1937(9) 0.069(5) Uani 1 1 d . . . H20A H 0.6211 0.5995 -0.1837 0.103 Uiso 1 1 calc R . . H20B H 0.5157 0.5460 -0.1512 0.103 Uiso 1 1 calc R . . H20C H 0.4920 0.5363 -0.2421 0.103 Uiso 1 1 calc R . . C21 C 0.5779(10) 0.4194(10) -0.2765(7) 0.053(4) Uani 1 1 d . . . H21A H 0.5982 0.3647 -0.2767 0.079 Uiso 1 1 calc R . . H21B H 0.6394 0.4771 -0.2849 0.079 Uiso 1 1 calc R . . H21C H 0.5050 0.3985 -0.3177 0.079 Uiso 1 1 calc R . . C22 C 0.4196(12) 0.1758(9) -0.0527(8) 0.055(4) Uani 1 1 d . . . H22 H 0.4952 0.2237 -0.0132 0.066 Uiso 1 1 calc R . . C23 C 0.3282(14) 0.1486(13) -0.0142(10) 0.101(7) Uani 1 1 d . . . H23A H 0.3246 0.2086 0.0067 0.151 Uiso 1 1 calc R . . H23B H 0.3470 0.1177 0.0278 0.151 Uiso 1 1 calc R . . H23C H 0.2531 0.1017 -0.0520 0.151 Uiso 1 1 calc R . . C24 C 0.4297(15) 0.0845(11) -0.0823(8) 0.090(6) Uani 1 1 d . . . H24A H 0.4399 0.0510 -0.0404 0.136 Uiso 1 1 calc R . . H24B H 0.4966 0.1043 -0.1011 0.136 Uiso 1 1 calc R . . H24C H 0.3591 0.0391 -0.1246 0.136 Uiso 1 1 calc R . . C25 C 0.9449(10) 0.3730(8) 0.3406(6) 0.032(3) Uani 1 1 d . . . H25 H 1.0014 0.3553 0.3314 0.039 Uiso 1 1 calc R . . C26 C 0.9355(12) 0.3839(9) 0.4148(8) 0.050(4) Uani 1 1 d . . . H26 H 0.9841 0.3720 0.4553 0.060 Uiso 1 1 calc R . . C27 C 0.8566(13) 0.4115(9) 0.4288(8) 0.051(4) Uani 1 1 d . . . H27 H 0.8497 0.4191 0.4791 0.061 Uiso 1 1 calc R . . C28 C 0.7879(11) 0.4282(9) 0.3702(9) 0.051(4) Uani 1 1 d . . . H28 H 0.7335 0.4494 0.3786 0.061 Uiso 1 1 calc R . . C29 C 0.7994(11) 0.4135(9) 0.2992(9) 0.047(4) Uani 1 1 d . . . H29 H 0.7491 0.4228 0.2579 0.056 Uiso 1 1 calc R . . Pt1A Pt 0.18314(4) 0.28397(3) 0.44412(3) 0.02569(12) Uani 1 1 d . . . I1A I 0.12862(7) 0.29953(6) 0.57006(4) 0.0335(2) Uani 1 1 d . . . I2A I 0.21279(7) 0.25920(6) 0.31033(4) 0.0381(2) Uani 1 1 d . . . N1A N 0.2384(8) 0.0011(7) 0.3549(5) 0.034(2) Uani 1 1 d . . . H1A H 0.1732 0.0004 0.3294 0.041 Uiso 1 1 calc R . . N2A N 0.1226(7) 0.0726(6) 0.4350(5) 0.023(2) Uani 1 1 d . . . N3A N -0.0313(8) 0.0887(7) 0.3841(5) 0.032(2) Uani 1 1 d . . . N4A N 0.2989(7) 0.4367(6) 0.4756(5) 0.028(2) Uani 1 1 d . . . C1A C 0.0857(8) 0.1391(8) 0.4188(6) 0.026(3) Uani 1 1 d . . . C2A C -0.0668(10) -0.0127(8) 0.3779(6) 0.031(3) Uani 1 1 d . . . H2A H -0.1437 -0.0648 0.3559 0.037 Uiso 1 1 calc R . . C3A C 0.0295(10) -0.0228(7) 0.4092(6) 0.030(3) Uani 1 1 d . . . H3A H 0.0328 -0.0833 0.4129 0.036 Uiso 1 1 calc R . . C4A C 0.2374(9) 0.0906(7) 0.4727(6) 0.024(3) Uani 1 1 d . . . C5A C 0.2943(10) 0.1436(8) 0.5485(6) 0.028(3) Uani 1 1 d . . . H5A H 0.2577 0.1725 0.5739 0.034 Uiso 1 1 calc R . . C6A C 0.4009(10) 0.1559(8) 0.5879(7) 0.037(3) Uani 1 1 d . . . H6A H 0.4393 0.1933 0.6398 0.044 Uiso 1 1 calc R . . C7A C 0.4517(10) 0.1120(9) 0.5500(7) 0.036(3) Uani 1 1 d . . . H7A H 0.5237 0.1154 0.5772 0.043 Uiso 1 1 calc R . . C8A C 0.4005(10) 0.0644(8) 0.4749(7) 0.033(3) Uani 1 1 d . . . H8A H 0.4400 0.0388 0.4497 0.039 Uiso 1 1 calc R . . C9A C 0.2917(9) 0.0514(8) 0.4328(7) 0.029(3) Uani 1 1 d . . . C10A C -0.1075(10) 0.1324(8) 0.3592(7) 0.035(3) Uani 1 1 d . . . H10A H -0.0585 0.2059 0.3701 0.041 Uiso 1 1 calc R . . C11A C -0.1674(12) 0.0952(11) 0.2725(8) 0.082(6) Uani 1 1 d . . . H11D H -0.1094 0.1049 0.2462 0.122 Uiso 1 1 calc R . . H11E H -0.2095 0.1323 0.2548 0.122 Uiso 1 1 calc R . . H11F H -0.2219 0.0243 0.2606 0.122 Uiso 1 1 calc R . . C12A C -0.1955(12) 0.1134(11) 0.4019(10) 0.077(5) Uani 1 1 d . . . H12D H -0.2408 0.0417 0.3956 0.115 Uiso 1 1 calc R . . H12E H -0.2473 0.1411 0.3808 0.115 Uiso 1 1 calc R . . H12F H -0.1551 0.1452 0.4568 0.115 Uiso 1 1 calc R . . C13A C 0.2854(10) -0.0482(9) 0.3161(6) 0.031(3) Uani 1 1 d . . . C14A C 0.2485(10) -0.1496(9) 0.3106(6) 0.035(3) Uani 1 1 d . . . C15A C 0.2960(11) -0.1961(9) 0.2741(7) 0.042(3) Uani 1 1 d . . . H15A H 0.2711 -0.2651 0.2708 0.050 Uiso 1 1 calc R . . C16A C 0.3792(11) -0.1453(10) 0.2418(7) 0.042(3) Uani 1 1 d . . . H16A H 0.4120 -0.1789 0.2170 0.051 Uiso 1 1 calc R . . C17A C 0.4149(11) -0.0461(11) 0.2453(7) 0.049(4) Uani 1 1 d . . . H17A H 0.4707 -0.0121 0.2213 0.058 Uiso 1 1 calc R . . C18A C 0.3713(11) 0.0061(9) 0.2832(7) 0.040(3) Uani 1 1 d . . . C19A C 0.1559(9) -0.2062(8) 0.3445(6) 0.030(3) Uani 1 1 d . . . H19A H 0.1466 -0.1569 0.3790 0.036 Uiso 1 1 calc R . . C20A C 0.1800(11) -0.2756(10) 0.3913(7) 0.055(4) Uani 1 1 d . . . H20D H 0.2066 -0.3146 0.3627 0.083 Uiso 1 1 calc R . . H20E H 0.1089 -0.3205 0.4005 0.083 Uiso 1 1 calc R . . H20F H 0.2399 -0.2366 0.4408 0.083 Uiso 1 1 calc R . . C21A C 0.0404(10) -0.2680(9) 0.2796(7) 0.053(4) Uani 1 1 d . . . H21D H 0.0223 -0.2244 0.2489 0.079 Uiso 1 1 calc R . . H21E H -0.0212 -0.3001 0.3020 0.079 Uiso 1 1 calc R . . H21F H 0.0464 -0.3188 0.2463 0.079 Uiso 1 1 calc R . . C22A C 0.4102(10) 0.1147(10) 0.2855(7) 0.050(4) Uani 1 1 d . . . H22A H 0.3720 0.1377 0.3181 0.060 Uiso 1 1 calc R . . C23A C 0.5405(12) 0.1793(10) 0.3219(9) 0.073(5) Uani 1 1 d . . . H23D H 0.5669 0.1629 0.3709 0.109 Uiso 1 1 calc R . . H23E H 0.5581 0.2495 0.3315 0.109 Uiso 1 1 calc R . . H23F H 0.5802 0.1670 0.2868 0.109 Uiso 1 1 calc R . . C24A C 0.3734(14) 0.1347(12) 0.2059(9) 0.081(5) Uani 1 1 d . . . H24D H 0.3950 0.2055 0.2113 0.122 Uiso 1 1 calc R . . H24E H 0.2894 0.0954 0.1822 0.122 Uiso 1 1 calc R . . H24F H 0.4124 0.1160 0.1731 0.122 Uiso 1 1 calc R . . C25A C 0.3842(9) 0.4713(8) 0.5424(7) 0.035(3) Uani 1 1 d . . . H25A H 0.3893 0.4262 0.5733 0.042 Uiso 1 1 calc R . . C26A C 0.4668(9) 0.5713(8) 0.5689(7) 0.036(3) Uani 1 1 d . . . H26A H 0.5254 0.5947 0.6176 0.043 Uiso 1 1 calc R . . C27A C 0.4601(10) 0.6348(8) 0.5217(7) 0.036(3) Uani 1 1 d . . . H27A H 0.5168 0.7026 0.5365 0.043 Uiso 1 1 calc R . . C28A C 0.3708(11) 0.5997(9) 0.4530(7) 0.038(3) Uani 1 1 d . . . H28A H 0.3634 0.6437 0.4214 0.045 Uiso 1 1 calc R . . C29A C 0.2921(9) 0.5000(8) 0.4305(6) 0.029(3) Uani 1 1 d . . . H29A H 0.2320 0.4755 0.3824 0.035 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 Pt1 0.0256(3) 0.0333(3) 0.0337(3) 0.0151(2) 0.0050(2) 0.0106(2) I1 0.0279(5) 0.0431(5) 0.0479(5) 0.0211(4) 0.0025(4) 0.0066(4) I2 0.0276(5) 0.0518(6) 0.0447(5) 0.0195(5) 0.0052(4) 0.0028(4) N1 0.027(6) 0.047(7) 0.021(5) -0.006(5) 0.004(4) 0.019(5) N2 0.020(5) 0.044(7) 0.031(6) 0.017(5) 0.007(5) 0.008(5) N3 0.049(7) 0.057(8) 0.044(7) 0.024(6) 0.029(6) 0.030(6) N4 0.025(6) 0.021(5) 0.040(6) 0.009(5) 0.005(5) 0.003(5) C1 0.039(8) 0.030(7) 0.053(9) 0.020(7) 0.024(7) 0.013(6) C2 0.035(8) 0.051(9) 0.042(8) 0.005(7) 0.013(6) 0.016(7) C3 0.045(9) 0.048(9) 0.035(8) 0.018(7) 0.011(7) 0.012(7) C4 0.017(6) 0.032(7) 0.034(7) 0.016(6) 0.008(5) 0.007(6) C5 0.032(7) 0.030(7) 0.025(7) -0.001(6) -0.005(6) 0.000(6) C6 0.034(8) 0.031(7) 0.026(7) -0.010(6) -0.005(6) 0.004(6) C7 0.029(7) 0.036(8) 0.040(8) 0.007(6) 0.002(6) 0.005(6) C8 0.021(7) 0.041(8) 0.020(6) 0.002(6) -0.004(5) 0.008(6) C9 0.018(6) 0.031(7) 0.024(6) 0.012(5) 0.004(5) 0.005(5) C10 0.083(12) 0.080(12) 0.056(10) 0.036(9) 0.029(9) 0.066(10) C11 0.115(16) 0.046(11) 0.158(19) 0.055(12) 0.033(14) 0.036(11) C12 0.048(10) 0.108(14) 0.092(12) 0.045(11) 0.028(9) 0.051(10) C13 0.032(7) 0.027(7) 0.037(7) 0.009(6) 0.009(6) 0.016(6) C14 0.023(7) 0.032(7) 0.019(6) -0.001(5) -0.002(5) 0.005(6) C15 0.031(7) 0.033(7) 0.040(8) 0.010(6) 0.004(6) 0.015(6) C16 0.024(7) 0.057(9) 0.024(7) -0.011(7) -0.005(6) 0.011(7) C17 0.037(8) 0.035(8) 0.048(9) -0.006(7) 0.006(7) 0.005(7) C18 0.043(8) 0.031(7) 0.020(6) -0.001(6) -0.004(6) 0.007(6) C19 0.031(8) 0.048(9) 0.036(8) 0.018(7) 0.002(6) 0.007(7) C20 0.065(11) 0.051(10) 0.079(12) 0.014(9) 0.030(9) 0.013(8) C21 0.032(8) 0.066(10) 0.031(8) 0.008(7) -0.002(6) 0.004(7) C22 0.071(11) 0.032(8) 0.042(9) 0.021(7) 0.004(7) 0.010(7) C23 0.087(14) 0.123(16) 0.104(15) 0.083(13) 0.050(12) 0.035(12) C24 0.133(16) 0.052(11) 0.056(11) 0.016(9) -0.003(10) 0.033(11) C25 0.044(8) 0.025(7) 0.023(7) 0.002(5) 0.002(6) 0.017(6) C26 0.061(10) 0.039(8) 0.047(9) 0.010(7) 0.006(7) 0.028(8) C27 0.076(11) 0.036(8) 0.037(8) 0.011(7) 0.024(8) 0.018(8) C28 0.041(9) 0.040(9) 0.066(11) 0.003(8) 0.022(8) 0.014(7) C29 0.036(8) 0.035(8) 0.072(11) 0.006(8) 0.018(8) 0.019(7) Pt1A 0.0209(2) 0.0214(2) 0.0272(3) 0.0070(2) 0.00223(19) 0.0055(2) I1A 0.0332(5) 0.0286(4) 0.0346(5) 0.0090(4) 0.0108(4) 0.0101(4) I2A 0.0369(5) 0.0350(5) 0.0301(5) 0.0071(4) 0.0078(4) 0.0069(4) N1A 0.028(6) 0.051(7) 0.026(6) 0.005(5) 0.006(5) 0.024(5) N2A 0.014(5) 0.016(5) 0.033(6) 0.003(4) 0.005(4) 0.003(4) N3A 0.024(6) 0.025(6) 0.042(6) 0.005(5) 0.002(5) 0.013(5) N4A 0.014(5) 0.025(5) 0.023(5) 0.000(4) -0.004(4) -0.004(4) C1A 0.011(6) 0.029(7) 0.020(6) -0.004(5) 0.001(5) -0.001(5) C2A 0.030(7) 0.022(7) 0.036(7) 0.005(6) 0.009(6) 0.010(6) C3A 0.043(8) 0.011(6) 0.036(7) 0.006(5) 0.015(6) 0.012(6) C4A 0.028(7) 0.010(6) 0.033(7) 0.007(5) 0.011(5) 0.007(5) C5A 0.037(7) 0.027(7) 0.026(7) 0.009(5) 0.017(6) 0.016(6) C6A 0.039(8) 0.021(7) 0.027(7) 0.010(6) -0.006(6) 0.001(6) C7A 0.025(7) 0.044(8) 0.040(8) 0.010(7) 0.005(6) 0.020(6) C8A 0.033(7) 0.026(7) 0.038(7) 0.008(6) 0.008(6) 0.014(6) C9A 0.022(6) 0.022(6) 0.035(7) 0.012(6) 0.008(6) 0.004(5) C10A 0.027(7) 0.024(7) 0.053(8) 0.013(6) 0.010(6) 0.013(6) C11A 0.065(11) 0.093(13) 0.064(11) 0.024(10) -0.025(9) 0.039(10) C12A 0.050(10) 0.086(12) 0.131(15) 0.058(11) 0.044(10) 0.049(9) C13A 0.026(7) 0.043(8) 0.020(6) -0.001(6) -0.002(5) 0.019(6) C14A 0.027(7) 0.040(8) 0.024(7) -0.007(6) -0.002(5) 0.013(6) C15A 0.040(8) 0.028(7) 0.039(8) -0.001(6) -0.001(6) 0.009(6) C16A 0.035(8) 0.058(10) 0.031(7) -0.006(7) 0.002(6) 0.026(7) C17A 0.042(9) 0.059(10) 0.040(8) 0.001(8) 0.019(7) 0.018(8) C18A 0.044(8) 0.043(8) 0.027(7) 0.000(6) 0.008(6) 0.019(7) C19A 0.028(7) 0.027(7) 0.026(7) 0.002(5) 0.000(5) 0.010(6) C20A 0.041(9) 0.067(10) 0.060(10) 0.024(8) 0.012(7) 0.027(8) C21A 0.030(8) 0.061(10) 0.043(8) 0.004(7) 0.005(6) 0.004(7) C22A 0.032(8) 0.053(9) 0.046(9) 0.009(7) 0.010(7) 0.006(7) C23A 0.058(11) 0.045(9) 0.104(14) 0.002(9) 0.040(10) 0.009(8) C24A 0.094(14) 0.086(13) 0.094(13) 0.055(11) 0.052(11) 0.051(11) C25A 0.025(7) 0.030(7) 0.041(8) 0.015(6) 0.008(6) 0.005(6) C26A 0.024(7) 0.035(7) 0.026(7) -0.007(6) 0.004(5) -0.002(6) C27A 0.027(7) 0.019(7) 0.060(9) 0.007(6) 0.017(7) 0.006(6) C28A 0.053(9) 0.030(7) 0.044(8) 0.015(6) 0.031(7) 0.022(7) C29A 0.029(7) 0.022(6) 0.034(7) 0.011(6) 0.010(5) 0.009(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 Pt1 C1 1.965(13) . ? Pt1 N4 2.094(10) . ? Pt1 I2 2.5901(10) . ? Pt1 I1 2.6024(10) . ? N1 C9 1.389(12) . ? N1 C13 1.426(13) . ? N1 H1 0.8800 . ? N2 C3 1.374(14) . ? N2 C1 1.391(14) . ? N2 C4 1.430(14) . ? N3 C1 1.301(14) . ? N3 C2 1.370(14) . ? N3 C10 1.505(14) . ? N4 C25 1.328(13) . ? N4 C29 1.330(14) . ? C2 C3 1.365(16) . ? C2 H2 0.9500 . ? C3 H3 0.9500 . ? C4 C5 1.375(14) . ? C4 C9 1.411(14) . ? C5 C6 1.363(15) . ? C5 H5 0.9500 . ? C6 C7 1.402(15) . ? C6 H6 0.9500 . ? C7 C8 1.338(14) . ? C7 H7 0.9500 . ? C8 C9 1.375(15) . ? C8 H8 0.9500 . ? C10 C12 1.501(17) . ? C10 C11 1.514(19) . ? C10 H10 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.415(14) . ? C13 C18 1.415(15) . ? C14 C15 1.409(14) . ? C14 C19 1.507(15) . ? C15 C16 1.363(15) . ? C15 H15 0.9500 . ? C16 C17 1.405(16) . ? C16 H16 0.9500 . ? C17 C18 1.366(15) . ? C17 H17 0.9500 . ? C18 C22 1.509(15) . ? C19 C21 1.497(16) . ? C19 C20 1.543(17) . ? C19 H19 1.0000 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 C23 1.492(18) . ? C22 C24 1.513(18) . ? C22 H22 1.0000 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C26 1.396(16) . ? C25 H25 0.9500 . ? C26 C27 1.359(17) . ? C26 H26 0.9500 . ? C27 C28 1.358(17) . ? C27 H27 0.9500 . ? C28 C29 1.357(17) . ? C28 H28 0.9500 . ? C29 H29 0.9500 . ? Pt1A C1A 1.968(11) . ? Pt1A N4A 2.102(8) . ? Pt1A I2A 2.5969(11) . ? Pt1A I1A 2.6060(10) . ? N1A C9A 1.401(13) . ? N1A C13A 1.406(13) . ? N1A H1A 0.8800 . ? N2A C1A 1.331(13) . ? N2A C3A 1.394(12) . ? N2A C4A 1.419(13) . ? N3A C1A 1.365(12) . ? N3A C2A 1.396(13) . ? N3A C10A 1.451(13) . ? N4A C25A 1.331(13) . ? N4A C29A 1.350(12) . ? C2A C3A 1.359(14) . ? C2A H2A 0.9500 . ? C3A H3A 0.9500 . ? C4A C5A 1.382(14) . ? C4A C9A 1.400(15) . ? C5A C6A 1.360(14) . ? C5A H5A 0.9500 . ? C6A C7A 1.383(15) . ? C6A H6A 0.9500 . ? C7A C8A 1.348(15) . ? C7A H7A 0.9500 . ? C8A C9A 1.393(14) . ? C8A H8A 0.9500 . ? C10A C12A 1.516(16) . ? C10A C11A 1.519(16) . ? C10A H10A 1.0000 . ? C11A H11D 0.9800 . ? C11A H11E 0.9800 . ? C11A H11F 0.9800 . ? C12A H12D 0.9800 . ? C12A H12E 0.9800 . ? C12A H12F 0.9800 . ? C13A C14A 1.396(15) . ? C13A C18A 1.419(16) . ? C14A C15A 1.359(15) . ? C14A C19A 1.502(15) . ? C15A C16A 1.374(16) . ? C15A H15A 0.9500 . ? C16A C17A 1.370(17) . ? C16A H16A 0.9500 . ? C17A C18A 1.391(16) . ? C17A H17A 0.9500 . ? C18A C22A 1.505(17) . ? C19A C20A 1.516(15) . ? C19A C21A 1.535(14) . ? C19A H19A 1.0000 . ? C20A H20D 0.9800 . ? C20A H20E 0.9800 . ? C20A H20F 0.9800 . ? C21A H21D 0.9800 . ? C21A H21E 0.9800 . ? C21A H21F 0.9800 . ? C22A C23A 1.524(16) . ? C22A C24A 1.529(17) . ? C22A H22A 1.0000 . ? C23A H23D 0.9800 . ? C23A H23E 0.9800 . ? C23A H23F 0.9800 . ? C24A H24D 0.9800 . ? C24A H24E 0.9800 . ? C24A H24F 0.9800 . ? C25A C26A 1.399(14) . ? C25A H25A 0.9500 . ? C26A C27A 1.378(15) . ? C26A H26A 0.9500 . ? C27A C28A 1.379(15) . ? C27A H27A 0.9500 . ? C28A C29A 1.382(14) . ? C28A H28A 0.9500 . ? C29A H29A 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 C1 Pt1 N4 176.3(5) . . ? C1 Pt1 I2 89.2(3) . . ? N4 Pt1 I2 90.4(2) . . ? C1 Pt1 I1 89.5(3) . . ? N4 Pt1 I1 91.3(2) . . ? I2 Pt1 I1 173.79(4) . . ? C9 N1 C13 122.2(9) . . ? C9 N1 H1 118.9 . . ? C13 N1 H1 118.9 . . ? C3 N2 C1 108.1(10) . . ? C3 N2 C4 126.0(10) . . ? C1 N2 C4 125.5(10) . . ? C1 N3 C2 112.7(11) . . ? C1 N3 C10 125.0(11) . . ? C2 N3 C10 122.3(11) . . ? C25 N4 C29 117.2(11) . . ? C25 N4 Pt1 121.1(8) . . ? C29 N4 Pt1 121.6(9) . . ? N3 C1 N2 105.9(11) . . ? N3 C1 Pt1 129.9(10) . . ? N2 C1 Pt1 124.0(9) . . ? C3 C2 N3 105.5(12) . . ? C3 C2 H2 127.3 . . ? N3 C2 H2 127.3 . . ? C2 C3 N2 107.7(11) . . ? C2 C3 H3 126.1 . . ? N2 C3 H3 126.1 . . ? C5 C4 C9 121.3(11) . . ? C5 C4 N2 119.6(10) . . ? C9 C4 N2 119.0(10) . . ? C6 C5 C4 119.6(11) . . ? C6 C5 H5 120.2 . . ? C4 C5 H5 120.2 . . ? C5 C6 C7 119.7(11) . . ? C5 C6 H6 120.1 . . ? C7 C6 H6 120.1 . . ? C8 C7 C6 119.8(12) . . ? C8 C7 H7 120.1 . . ? C6 C7 H7 120.1 . . ? C7 C8 C9 122.9(11) . . ? C7 C8 H8 118.6 . . ? C9 C8 H8 118.6 . . ? C8 C9 N1 123.1(10) . . ? C8 C9 C4 116.6(11) . . ? N1 C9 C4 120.2(11) . . ? C12 C10 N3 111.3(11) . . ? C12 C10 C11 113.2(13) . . ? N3 C10 C11 111.2(12) . . ? C12 C10 H10 106.9 . . ? N3 C10 H10 106.9 . . ? C11 C10 H10 106.9 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C14 C13 C18 120.9(10) . . ? C14 C13 N1 119.3(10) . . ? C18 C13 N1 119.7(10) . . ? C15 C14 C13 118.0(10) . . ? C15 C14 C19 116.9(10) . . ? C13 C14 C19 125.0(10) . . ? C16 C15 C14 121.7(11) . . ? C16 C15 H15 119.1 . . ? C14 C15 H15 119.1 . . ? C15 C16 C17 118.4(11) . . ? C15 C16 H16 120.8 . . ? C17 C16 H16 120.8 . . ? C18 C17 C16 123.2(12) . . ? C18 C17 H17 118.4 . . ? C16 C17 H17 118.4 . . ? C17 C18 C13 117.6(11) . . ? C17 C18 C22 122.3(12) . . ? C13 C18 C22 119.9(11) . . ? C21 C19 C14 110.7(10) . . ? C21 C19 C20 111.1(11) . . ? C14 C19 C20 114.1(11) . . ? C21 C19 H19 106.8 . . ? C14 C19 H19 106.8 . . ? C20 C19 H19 106.8 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C23 C22 C18 112.8(12) . . ? C23 C22 C24 110.0(13) . . ? C18 C22 C24 109.8(11) . . ? C23 C22 H22 108.0 . . ? C18 C22 H22 108.0 . . ? C24 C22 H22 108.0 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N4 C25 C26 120.9(12) . . ? N4 C25 H25 119.6 . . ? C26 C25 H25 119.6 . . ? C27 C26 C25 119.9(12) . . ? C27 C26 H26 120.1 . . ? C25 C26 H26 120.1 . . ? C28 C27 C26 119.2(13) . . ? C28 C27 H27 120.4 . . ? C26 C27 H27 120.4 . . ? C29 C28 C27 117.8(14) . . ? C29 C28 H28 121.1 . . ? C27 C28 H28 121.1 . . ? N4 C29 C28 125.0(13) . . ? N4 C29 H29 117.5 . . ? C28 C29 H29 117.5 . . ? C1A Pt1A N4A 175.2(4) . . ? C1A Pt1A I2A 86.5(3) . . ? N4A Pt1A I2A 93.6(2) . . ? C1A Pt1A I1A 90.1(3) . . ? N4A Pt1A I1A 90.2(2) . . ? I2A Pt1A I1A 173.58(3) . . ? C9A N1A C13A 122.2(9) . . ? C9A N1A H1A 118.9 . . ? C13A N1A H1A 118.9 . . ? C1A N2A C3A 109.8(9) . . ? C1A N2A C4A 127.7(9) . . ? C3A N2A C4A 122.4(9) . . ? C1A N3A C2A 108.7(9) . . ? C1A N3A C10A 126.2(9) . . ? C2A N3A C10A 125.2(9) . . ? C25A N4A C29A 119.0(9) . . ? C25A N4A Pt1A 117.8(7) . . ? C29A N4A Pt1A 123.2(7) . . ? N2A C1A N3A 107.5(9) . . ? N2A C1A Pt1A 125.6(7) . . ? N3A C1A Pt1A 126.8(8) . . ? C3A C2A N3A 107.0(10) . . ? C3A C2A H2A 126.5 . . ? N3A C2A H2A 126.5 . . ? C2A C3A N2A 107.0(9) . . ? C2A C3A H3A 126.5 . . ? N2A C3A H3A 126.5 . . ? C5A C4A C9A 120.0(10) . . ? C5A C4A N2A 120.8(10) . . ? C9A C4A N2A 119.2(10) . . ? C6A C5A C4A 122.1(11) . . ? C6A C5A H5A 118.9 . . ? C4A C5A H5A 118.9 . . ? C5A C6A C7A 117.9(11) . . ? C5A C6A H6A 121.1 . . ? C7A C6A H6A 121.1 . . ? C8A C7A C6A 120.9(11) . . ? C8A C7A H7A 119.6 . . ? C6A C7A H7A 119.6 . . ? C7A C8A C9A 122.4(12) . . ? C7A C8A H8A 118.8 . . ? C9A C8A H8A 118.8 . . ? C8A C9A C4A 116.4(11) . . ? C8A C9A N1A 122.2(11) . . ? C4A C9A N1A 121.3(10) . . ? N3A C10A C12A 112.9(10) . . ? N3A C10A C11A 109.9(10) . . ? C12A C10A C11A 110.8(11) . . ? N3A C10A H10A 107.7 . . ? C12A C10A H10A 107.7 . . ? C11A C10A H10A 107.7 . . ? C10A C11A H11D 109.5 . . ? C10A C11A H11E 109.5 . . ? H11D C11A H11E 109.5 . . ? C10A C11A H11F 109.5 . . ? H11D C11A H11F 109.5 . . ? H11E C11A H11F 109.5 . . ? C10A C12A H12D 109.5 . . ? C10A C12A H12E 109.5 . . ? H12D C12A H12E 109.5 . . ? C10A C12A H12F 109.5 . . ? H12D C12A H12F 109.5 . . ? H12E C12A H12F 109.5 . . ? C14A C13A N1A 120.1(11) . . ? C14A C13A C18A 120.3(11) . . ? N1A C13A C18A 119.6(11) . . ? C15A C14A C13A 119.5(12) . . ? C15A C14A C19A 120.9(11) . . ? C13A C14A C19A 119.6(11) . . ? C14A C15A C16A 121.2(12) . . ? C14A C15A H15A 119.4 . . ? C16A C15A H15A 119.4 . . ? C17A C16A C15A 120.0(13) . . ? C17A C16A H16A 120.0 . . ? C15A C16A H16A 120.0 . . ? C16A C17A C18A 121.4(13) . . ? C16A C17A H17A 119.3 . . ? C18A C17A H17A 119.3 . . ? C17A C18A C13A 117.4(12) . . ? C17A C18A C22A 120.7(12) . . ? C13A C18A C22A 121.8(12) . . ? C14A C19A C20A 115.1(10) . . ? C14A C19A C21A 109.6(9) . . ? C20A C19A C21A 107.9(10) . . ? C14A C19A H19A 108.0 . . ? C20A C19A H19A 108.0 . . ? C21A C19A H19A 108.0 . . ? C19A C20A H20D 109.5 . . ? C19A C20A H20E 109.5 . . ? H20D C20A H20E 109.5 . . ? C19A C20A H20F 109.5 . . ? H20D C20A H20F 109.5 . . ? H20E C20A H20F 109.5 . . ? C19A C21A H21D 109.5 . . ? C19A C21A H21E 109.5 . . ? H21D C21A H21E 109.5 . . ? C19A C21A H21F 109.5 . . ? H21D C21A H21F 109.5 . . ? H21E C21A H21F 109.5 . . ? C18A C22A C23A 113.6(11) . . ? C18A C22A C24A 113.0(11) . . ? C23A C22A C24A 108.3(12) . . ? C18A C22A H22A 107.2 . . ? C23A C22A H22A 107.2 . . ? C24A C22A H22A 107.2 . . ? C22A C23A H23D 109.5 . . ? C22A C23A H23E 109.5 . . ? H23D C23A H23E 109.5 . . ? C22A C23A H23F 109.5 . . ? H23D C23A H23F 109.5 . . ? H23E C23A H23F 109.5 . . ? C22A C24A H24D 109.5 . . ? C22A C24A H24E 109.5 . . ? H24D C24A H24E 109.5 . . ? C22A C24A H24F 109.5 . . ? H24D C24A H24F 109.5 . . ? H24E C24A H24F 109.5 . . ? N4A C25A C26A 122.8(11) . . ? N4A C25A H25A 118.6 . . ? C26A C25A H25A 118.6 . . ? C27A C26A C25A 117.5(10) . . ? C27A C26A H26A 121.2 . . ? C25A C26A H26A 121.2 . . ? C26A C27A C28A 119.9(11) . . ? C26A C27A H27A 120.1 . . ? C28A C27A H27A 120.1 . . ? C27A C28A C29A 119.4(11) . . ? C27A C28A H28A 120.3 . . ? C29A C28A H28A 120.3 . . ? N4A C29A C28A 121.3(10) . . ? N4A C29A H29A 119.3 . . ? C28A C29A H29A 119.3 . . ? 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 C1 Pt1 N4 C25 -158(6) . . . . ? I2 Pt1 N4 C25 117.6(8) . . . . ? I1 Pt1 N4 C25 -56.5(8) . . . . ? C1 Pt1 N4 C29 25(7) . . . . ? I2 Pt1 N4 C29 -59.1(9) . . . . ? I1 Pt1 N4 C29 126.9(9) . . . . ? C2 N3 C1 N2 0.4(14) . . . . ? C10 N3 C1 N2 -176.3(11) . . . . ? C2 N3 C1 Pt1 175.7(9) . . . . ? C10 N3 C1 Pt1 -1.0(19) . . . . ? C3 N2 C1 N3 -2.1(13) . . . . ? C4 N2 C1 N3 -175.6(10) . . . . ? C3 N2 C1 Pt1 -177.7(8) . . . . ? C4 N2 C1 Pt1 8.7(15) . . . . ? N4 Pt1 C1 N3 179(59) . . . . ? I2 Pt1 C1 N3 -96.8(12) . . . . ? I1 Pt1 C1 N3 77.1(12) . . . . ? N4 Pt1 C1 N2 -7(7) . . . . ? I2 Pt1 C1 N2 77.7(9) . . . . ? I1 Pt1 C1 N2 -108.4(9) . . . . ? C1 N3 C2 C3 1.3(15) . . . . ? C10 N3 C2 C3 178.2(11) . . . . ? N3 C2 C3 N2 -2.6(14) . . . . ? C1 N2 C3 C2 2.9(13) . . . . ? C4 N2 C3 C2 176.4(10) . . . . ? C3 N2 C4 C5 -123.3(12) . . . . ? C1 N2 C4 C5 49.1(15) . . . . ? C3 N2 C4 C9 59.7(15) . . . . ? C1 N2 C4 C9 -127.9(11) . . . . ? C9 C4 C5 C6 -0.5(17) . . . . ? N2 C4 C5 C6 -177.5(10) . . . . ? C4 C5 C6 C7 -0.8(18) . . . . ? C5 C6 C7 C8 1.9(18) . . . . ? C6 C7 C8 C9 -1.8(18) . . . . ? C7 C8 C9 N1 -179.5(11) . . . . ? C7 C8 C9 C4 0.5(17) . . . . ? C13 N1 C9 C8 -0.6(16) . . . . ? C13 N1 C9 C4 179.5(10) . . . . ? C5 C4 C9 C8 0.7(16) . . . . ? N2 C4 C9 C8 177.6(9) . . . . ? C5 C4 C9 N1 -179.4(10) . . . . ? N2 C4 C9 N1 -2.4(15) . . . . ? C1 N3 C10 C12 -124.4(14) . . . . ? C2 N3 C10 C12 59.1(17) . . . . ? C1 N3 C10 C11 108.4(15) . . . . ? C2 N3 C10 C11 -68.1(17) . . . . ? C9 N1 C13 C14 74.1(14) . . . . ? C9 N1 C13 C18 -109.2(13) . . . . ? C18 C13 C14 C15 1.4(17) . . . . ? N1 C13 C14 C15 178.2(10) . . . . ? C18 C13 C14 C19 -179.5(11) . . . . ? N1 C13 C14 C19 -2.8(17) . . . . ? C13 C14 C15 C16 -4.0(17) . . . . ? C19 C14 C15 C16 176.8(11) . . . . ? C14 C15 C16 C17 4.1(18) . . . . ? C15 C16 C17 C18 -1.6(19) . . . . ? C16 C17 C18 C13 -0.9(19) . . . . ? C16 C17 C18 C22 175.5(12) . . . . ? C14 C13 C18 C17 0.9(18) . . . . ? N1 C13 C18 C17 -175.8(11) . . . . ? C14 C13 C18 C22 -175.5(11) . . . . ? N1 C13 C18 C22 7.7(17) . . . . ? C15 C14 C19 C21 -69.7(14) . . . . ? C13 C14 C19 C21 111.2(13) . . . . ? C15 C14 C19 C20 56.5(15) . . . . ? C13 C14 C19 C20 -122.6(13) . . . . ? C17 C18 C22 C23 -37.6(18) . . . . ? C13 C18 C22 C23 138.7(13) . . . . ? C17 C18 C22 C24 85.5(16) . . . . ? C13 C18 C22 C24 -98.1(14) . . . . ? C29 N4 C25 C26 1.1(16) . . . . ? Pt1 N4 C25 C26 -175.7(8) . . . . ? N4 C25 C26 C27 -1.6(19) . . . . ? C25 C26 C27 C28 0(2) . . . . ? C26 C27 C28 C29 2(2) . . . . ? C25 N4 C29 C28 0.8(18) . . . . ? Pt1 N4 C29 C28 177.6(10) . . . . ? C27 C28 C29 N4 -2(2) . . . . ? C1A Pt1A N4A C25A -35(5) . . . . ? I2A Pt1A N4A C25A -126.5(8) . . . . ? I1A Pt1A N4A C25A 58.6(8) . . . . ? C1A Pt1A N4A C29A 144(4) . . . . ? I2A Pt1A N4A C29A 51.8(9) . . . . ? I1A Pt1A N4A C29A -123.0(8) . . . . ? C3A N2A C1A N3A 1.2(12) . . . . ? C4A N2A C1A N3A -178.5(10) . . . . ? C3A N2A C1A Pt1A 179.4(7) . . . . ? C4A N2A C1A Pt1A -0.3(16) . . . . ? C2A N3A C1A N2A -0.9(12) . . . . ? C10A N3A C1A N2A 177.9(10) . . . . ? C2A N3A C1A Pt1A -179.0(8) . . . . ? C10A N3A C1A Pt1A -0.3(16) . . . . ? N4A Pt1A C1A N2A -2(5) . . . . ? I2A Pt1A C1A N2A 89.9(9) . . . . ? I1A Pt1A C1A N2A -95.5(9) . . . . ? N4A Pt1A C1A N3A 176(4) . . . . ? I2A Pt1A C1A N3A -92.2(9) . . . . ? I1A Pt1A C1A N3A 82.3(9) . . . . ? C1A N3A C2A C3A 0.2(12) . . . . ? C10A N3A C2A C3A -178.6(10) . . . . ? N3A C2A C3A N2A 0.5(12) . . . . ? C1A N2A C3A C2A -1.1(13) . . . . ? C4A N2A C3A C2A 178.6(9) . . . . ? C1A N2A C4A C5A 63.7(15) . . . . ? C3A N2A C4A C5A -116.0(11) . . . . ? C1A N2A C4A C9A -118.1(12) . . . . ? C3A N2A C4A C9A 62.2(14) . . . . ? C9A C4A C5A C6A -3.1(16) . . . . ? N2A C4A C5A C6A 175.1(10) . . . . ? C4A C5A C6A C7A -0.8(16) . . . . ? C5A C6A C7A C8A 4.4(17) . . . . ? C6A C7A C8A C9A -4.0(18) . . . . ? C7A C8A C9A C4A 0.0(16) . . . . ? C7A C8A C9A N1A -179.5(11) . . . . ? C5A C4A C9A C8A 3.5(15) . . . . ? N2A C4A C9A C8A -174.8(9) . . . . ? C5A C4A C9A N1A -177.1(10) . . . . ? N2A C4A C9A N1A 4.7(15) . . . . ? C13A N1A C9A C8A 6.6(16) . . . . ? C13A N1A C9A C4A -172.9(10) . . . . ? C1A N3A C10A C12A -116.6(13) . . . . ? C2A N3A C10A C12A 62.0(15) . . . . ? C1A N3A C10A C11A 119.2(12) . . . . ? C2A N3A C10A C11A -62.2(15) . . . . ? C9A N1A C13A C14A 94.5(13) . . . . ? C9A N1A C13A C18A -84.8(14) . . . . ? N1A C13A C14A C15A -178.9(10) . . . . ? C18A C13A C14A C15A 0.4(17) . . . . ? N1A C13A C14A C19A 1.7(16) . . . . ? C18A C13A C14A C19A -178.9(10) . . . . ? C13A C14A C15A C16A -0.5(18) . . . . ? C19A C14A C15A C16A 178.9(10) . . . . ? C14A C15A C16A C17A -0.7(19) . . . . ? C15A C16A C17A C18A 2.0(19) . . . . ? C16A C17A C18A C13A -2.0(18) . . . . ? C16A C17A C18A C22A -179.1(11) . . . . ? C14A C13A C18A C17A 0.8(17) . . . . ? N1A C13A C18A C17A -179.9(10) . . . . ? C14A C13A C18A C22A 177.8(10) . . . . ? N1A C13A C18A C22A -2.9(17) . . . . ? C15A C14A C19A C20A 45.9(15) . . . . ? C13A C14A C19A C20A -134.8(11) . . . . ? C15A C14A C19A C21A -75.9(14) . . . . ? C13A C14A C19A C21A 103.4(12) . . . . ? C17A C18A C22A C23A -58.4(17) . . . . ? C13A C18A C22A C23A 124.7(13) . . . . ? C17A C18A C22A C24A 65.5(16) . . . . ? C13A C18A C22A C24A -111.5(14) . . . . ? C29A N4A C25A C26A 1.1(17) . . . . ? Pt1A N4A C25A C26A 179.5(9) . . . . ? N4A C25A C26A C27A -2.2(18) . . . . ? C25A C26A C27A C28A 3.1(17) . . . . ? C26A C27A C28A C29A -3.1(18) . . . . ? C25A N4A C29A C28A -0.9(17) . . . . ? Pt1A N4A C29A C28A -179.3(8) . . . . ? C27A C28A C29A N4A 2.0(18) . . . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 3.255 _refine_diff_density_min -1.506 _refine_diff_density_rms 0.220 #===END data_10072 _database_code_depnum_ccdc_archive 'CCDC 791428' #TrackingRef '- Cross Dalton crystal structure data.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '{[C,N]Pd(mu-OH)}2 (12)' _chemical_melting_point ? _chemical_formula_moiety 'C48 H62 N6 O2 Pd2,C5 H12' _chemical_formula_sum 'C53 H74 N6 O2 Pd2' _chemical_formula_weight 1039.98 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M I4(1)/a loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-y+3/4, x+1/4, z+1/4' 'y+3/4, -x+3/4, z+3/4' 'x+1/2, y+1/2, z+1/2' '-x+1, -y+1/2, z+1' '-y+5/4, x+3/4, z+3/4' 'y+5/4, -x+5/4, z+5/4' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'y-3/4, -x-1/4, -z-1/4' '-y-3/4, x-3/4, -z-3/4' '-x+1/2, -y+1/2, -z+1/2' 'x, y+1/2, -z' 'y-1/4, -x+1/4, -z+1/4' '-y-1/4, x-1/4, -z-1/4' _cell_length_a 19.443(2) _cell_length_b 19.443(2) _cell_length_c 25.426(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 9612(2) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 982 _cell_measurement_theta_min 2.964 _cell_measurement_theta_max 26.583 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.437 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4336 _exptl_absorpt_coefficient_mu 0.796 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.634 _exptl_absorpt_correction_T_max 0.802 _exptl_absorpt_process_details ; absorption correction based on 16031 reflections(SADABS);Rint 0.1710 before correction and 0.0484 after. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 Apex 2000 CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 37121 _diffrn_reflns_av_R_equivalents 0.0767 _diffrn_reflns_av_sigmaI/netI 0.0436 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 2.09 _diffrn_reflns_theta_max 26.00 _reflns_number_total 4713 _reflns_number_gt 3961 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Disordered pentane (C5H12) was omitted using the SQUEEZE option of PLATON. The solvent accessible voids are 1135.0 A3 with an estimated 332e/cell to be added. Eight solvent C5H12 molecules/unit cell accounting for 336e were included in the formula, FWt, (000) and density calculations. PLATON Reference: Spek, A.L. (1990), Acta Cryst. A46, C-34. 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^)+(0.0527P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4713 _refine_ls_number_parameters 268 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0497 _refine_ls_R_factor_gt 0.0378 _refine_ls_wR_factor_ref 0.0960 _refine_ls_wR_factor_gt 0.0914 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.029 _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 0.581190(11) 0.268119(11) 0.162672(9) 0.02291(10) Uani 1 1 d . . . O1 O 0.51551(10) 0.18560(11) 0.15943(8) 0.0286(5) Uani 1 1 d . . . H1 H 0.5298 0.1554 0.1858 0.034 Uiso 1 1 d R . . N1 N 0.63460(13) 0.35481(13) 0.17323(9) 0.0259(6) Uani 1 1 d . . . N2 N 0.73152(12) 0.24386(13) 0.16801(9) 0.0252(6) Uani 1 1 d . . . N3 N 0.68096(13) 0.16207(13) 0.12564(10) 0.0293(6) Uani 1 1 d . . . C1 C 0.66837(15) 0.22094(15) 0.15251(11) 0.0243(6) Uani 1 1 d . . . C2 C 0.78174(16) 0.19834(17) 0.15094(12) 0.0302(7) Uani 1 1 d . . . H2 H 0.8298 0.2023 0.1569 0.036 Uiso 1 1 calc R . . C3 C 0.75046(16) 0.14832(18) 0.12485(13) 0.0345(8) Uani 1 1 d . . . H3 H 0.7720 0.1100 0.1086 0.041 Uiso 1 1 calc R . . C4 C 0.74680(15) 0.30657(15) 0.19418(11) 0.0240(6) Uani 1 1 d . . . C5 C 0.81031(15) 0.31408(16) 0.21881(12) 0.0279(7) Uani 1 1 d . . . H5 H 0.8404 0.2757 0.2208 0.033 Uiso 1 1 calc R . . C6 C 0.83046(16) 0.37564(18) 0.24027(12) 0.0320(7) Uani 1 1 d . . . H6 H 0.8735 0.3797 0.2576 0.038 Uiso 1 1 calc R . . C7 C 0.78732(16) 0.43134(17) 0.23621(13) 0.0330(8) Uani 1 1 d . . . H7 H 0.8016 0.4748 0.2494 0.040 Uiso 1 1 calc R . . C8 C 0.72332(16) 0.42468(17) 0.21302(12) 0.0309(7) Uani 1 1 d . . . H8 H 0.6945 0.4640 0.2107 0.037 Uiso 1 1 calc R . . C9 C 0.69942(15) 0.36176(15) 0.19269(11) 0.0253(7) Uani 1 1 d . . . C10 C 0.63035(17) 0.12278(17) 0.09432(13) 0.0346(8) Uani 1 1 d . . . H10 H 0.5835 0.1326 0.1086 0.042 Uiso 1 1 calc R . . C11 C 0.6326(2) 0.1473(2) 0.03775(14) 0.0471(9) Uani 1 1 d . . . H11A H 0.6241 0.1969 0.0366 0.071 Uiso 1 1 calc R . . H11B H 0.5972 0.1233 0.0173 0.071 Uiso 1 1 calc R . . H11C H 0.6780 0.1374 0.0228 0.071 Uiso 1 1 calc R . . C12 C 0.6437(2) 0.04658(19) 0.09958(16) 0.0492(10) Uani 1 1 d . . . H12A H 0.6895 0.0358 0.0857 0.074 Uiso 1 1 calc R . . H12B H 0.6089 0.0210 0.0797 0.074 Uiso 1 1 calc R . . H12C H 0.6414 0.0334 0.1367 0.074 Uiso 1 1 calc R . . C13 C 0.58953(16) 0.41320(15) 0.17731(13) 0.0281(7) Uani 1 1 d . . . C14 C 0.55914(16) 0.42965(16) 0.22585(13) 0.0322(7) Uani 1 1 d . . . C15 C 0.51249(19) 0.48379(19) 0.22677(16) 0.0461(9) Uani 1 1 d . . . H15 H 0.4907 0.4954 0.2590 0.055 Uiso 1 1 calc R . . C16 C 0.4971(2) 0.52098(19) 0.18230(17) 0.0528(10) Uani 1 1 d . . . H16 H 0.4645 0.5573 0.1839 0.063 Uiso 1 1 calc R . . C17 C 0.5289(2) 0.50546(19) 0.13571(16) 0.0493(10) Uani 1 1 d . . . H17 H 0.5189 0.5322 0.1054 0.059 Uiso 1 1 calc R . . C18 C 0.57560(17) 0.45122(17) 0.13187(14) 0.0361(8) Uani 1 1 d . . . C19 C 0.6100(2) 0.4336(2) 0.07992(14) 0.0463(10) Uani 1 1 d . . . H19 H 0.6460 0.3983 0.0878 0.056 Uiso 1 1 calc R . . C20 C 0.5611(3) 0.4013(4) 0.0420(2) 0.110(2) Uani 1 1 d . . . H20A H 0.5294 0.4363 0.0286 0.165 Uiso 1 1 calc R . . H20B H 0.5349 0.3651 0.0599 0.165 Uiso 1 1 calc R . . H20C H 0.5869 0.3811 0.0127 0.165 Uiso 1 1 calc R . . C21 C 0.6464(3) 0.4941(3) 0.0557(2) 0.0969(19) Uani 1 1 d . . . H21A H 0.6637 0.4813 0.0208 0.145 Uiso 1 1 calc R . . H21B H 0.6851 0.5077 0.0781 0.145 Uiso 1 1 calc R . . H21C H 0.6143 0.5327 0.0523 0.145 Uiso 1 1 calc R . . C22 C 0.57620(17) 0.39186(17) 0.27599(12) 0.0336(8) Uani 1 1 d . . . H22 H 0.6146 0.3592 0.2681 0.040 Uiso 1 1 calc R . . C23 C 0.60120(19) 0.4413(2) 0.31880(15) 0.0468(10) Uani 1 1 d . . . H23A H 0.6435 0.4640 0.3071 0.070 Uiso 1 1 calc R . . H23B H 0.6104 0.4155 0.3512 0.070 Uiso 1 1 calc R . . H23C H 0.5657 0.4760 0.3256 0.070 Uiso 1 1 calc R . . C24 C 0.51567(19) 0.34985(19) 0.29659(14) 0.0442(9) Uani 1 1 d . . . H24A H 0.4771 0.3806 0.3044 0.066 Uiso 1 1 calc R . . H24B H 0.5294 0.3256 0.3287 0.066 Uiso 1 1 calc R . . H24C H 0.5016 0.3164 0.2699 0.066 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 0.01989(14) 0.02554(15) 0.02330(15) 0.00039(9) 0.00086(9) 0.00292(9) O1 0.0214(11) 0.0277(11) 0.0367(13) 0.0021(9) -0.0012(9) 0.0040(9) N1 0.0239(13) 0.0253(14) 0.0285(14) 0.0019(11) -0.0009(11) 0.0021(11) N2 0.0228(13) 0.0314(14) 0.0213(13) 0.0012(11) 0.0038(10) 0.0025(11) N3 0.0245(13) 0.0345(15) 0.0289(15) -0.0047(12) 0.0014(12) 0.0059(11) C1 0.0252(16) 0.0287(16) 0.0190(15) 0.0014(12) 0.0020(12) 0.0036(13) C2 0.0218(16) 0.0385(19) 0.0303(18) 0.0004(14) 0.0041(13) 0.0088(14) C3 0.0301(18) 0.040(2) 0.0332(19) -0.0041(15) 0.0040(15) 0.0117(15) C4 0.0227(15) 0.0316(17) 0.0176(15) 0.0031(12) 0.0040(12) 0.0001(13) C5 0.0251(16) 0.0348(18) 0.0236(16) 0.0043(14) 0.0038(13) 0.0026(14) C6 0.0227(16) 0.048(2) 0.0254(17) 0.0077(15) -0.0002(13) -0.0062(15) C7 0.0321(18) 0.0350(18) 0.0321(19) 0.0012(15) 0.0038(15) -0.0121(15) C8 0.0285(17) 0.0308(17) 0.0335(18) 0.0057(14) 0.0043(14) -0.0009(14) C9 0.0251(16) 0.0329(17) 0.0179(15) 0.0046(13) 0.0031(12) -0.0033(13) C10 0.0285(17) 0.0363(19) 0.039(2) -0.0123(15) 0.0025(15) 0.0003(15) C11 0.046(2) 0.055(2) 0.040(2) -0.0062(18) -0.0047(18) -0.0040(19) C12 0.048(2) 0.042(2) 0.058(3) -0.0126(19) 0.0062(19) -0.0054(18) C13 0.0242(16) 0.0229(16) 0.0373(19) 0.0028(14) -0.0014(13) -0.0027(13) C14 0.0295(17) 0.0261(17) 0.041(2) -0.0039(14) -0.0055(15) 0.0032(14) C15 0.048(2) 0.041(2) 0.049(2) -0.0083(18) -0.0004(19) 0.0144(18) C16 0.057(3) 0.036(2) 0.066(3) 0.000(2) -0.002(2) 0.0207(19) C17 0.051(2) 0.041(2) 0.056(3) 0.0225(19) -0.011(2) 0.0073(18) C18 0.0309(18) 0.0327(18) 0.045(2) 0.0085(16) -0.0034(15) -0.0024(14) C19 0.042(2) 0.054(2) 0.042(2) 0.0192(18) 0.0034(17) 0.0032(19) C20 0.081(4) 0.191(7) 0.059(3) -0.034(4) 0.024(3) -0.041(4) C21 0.098(4) 0.099(4) 0.094(4) 0.030(4) 0.040(4) -0.023(3) C22 0.0313(18) 0.0410(19) 0.0284(18) -0.0046(15) 0.0012(14) 0.0104(15) C23 0.035(2) 0.062(3) 0.043(2) -0.0126(19) 0.0008(17) 0.0029(18) C24 0.048(2) 0.050(2) 0.035(2) 0.0001(17) 0.0009(17) 0.0011(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 C1 1.945(3) . ? Pd1 N1 1.998(3) . ? Pd1 O1 2.052(2) . ? Pd1 O1 2.086(2) 6_554 ? Pd1 Pd1 3.2348(6) 6_554 ? O1 Pd1 2.086(2) 6_554 ? O1 H1 0.9342 . ? N1 C9 1.361(4) . ? N1 C13 1.438(4) . ? N2 C1 1.364(4) . ? N2 C2 1.387(4) . ? N2 C4 1.420(4) . ? N3 C1 1.355(4) . ? N3 C3 1.378(4) . ? N3 C10 1.478(4) . ? C2 C3 1.325(4) . ? C2 H2 0.9500 . ? C3 H3 0.9500 . ? C4 C5 1.392(4) . ? C4 C9 1.415(4) . ? C5 C6 1.373(4) . ? C5 H5 0.9500 . ? C6 C7 1.374(5) . ? C6 H6 0.9500 . ? C7 C8 1.383(4) . ? C7 H7 0.9500 . ? C8 C9 1.407(4) . ? C8 H8 0.9500 . ? C10 C12 1.510(5) . ? C10 C11 1.516(5) . ? C10 H10 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C18 1.398(4) . ? C13 C14 1.405(4) . ? C14 C15 1.390(4) . ? C14 C22 1.508(5) . ? C15 C16 1.375(5) . ? C15 H15 0.9500 . ? C16 C17 1.370(5) . ? C16 H16 0.9500 . ? C17 C18 1.396(5) . ? C17 H17 0.9500 . ? C18 C19 1.520(5) . ? C19 C20 1.493(6) . ? C19 C21 1.506(6) . ? C19 H19 1.0000 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 C24 1.525(5) . ? C22 C23 1.531(5) . ? C22 H22 1.0000 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Pd1 N1 87.87(11) . . ? C1 Pd1 O1 99.69(10) . . ? N1 Pd1 O1 171.26(9) . . ? C1 Pd1 O1 169.70(10) . 6_554 ? N1 Pd1 O1 96.31(9) . 6_554 ? O1 Pd1 O1 76.99(9) . 6_554 ? C1 Pd1 Pd1 138.42(9) . 6_554 ? N1 Pd1 Pd1 133.72(7) . 6_554 ? O1 Pd1 Pd1 38.96(6) . 6_554 ? O1 Pd1 Pd1 38.22(6) 6_554 6_554 ? Pd1 O1 Pd1 102.82(9) . 6_554 ? Pd1 O1 H1 106.1 . . ? Pd1 O1 H1 120.8 6_554 . ? C9 N1 C13 117.4(3) . . ? C9 N1 Pd1 127.9(2) . . ? C13 N1 Pd1 111.04(19) . . ? C1 N2 C2 109.5(3) . . ? C1 N2 C4 127.2(2) . . ? C2 N2 C4 123.2(3) . . ? C1 N3 C3 110.4(3) . . ? C1 N3 C10 126.0(3) . . ? C3 N3 C10 123.0(3) . . ? N3 C1 N2 105.0(2) . . ? N3 C1 Pd1 128.5(2) . . ? N2 C1 Pd1 126.3(2) . . ? C3 C2 N2 107.6(3) . . ? C3 C2 H2 126.2 . . ? N2 C2 H2 126.2 . . ? C2 C3 N3 107.5(3) . . ? C2 C3 H3 126.3 . . ? N3 C3 H3 126.3 . . ? C5 C4 C9 120.7(3) . . ? C5 C4 N2 119.1(3) . . ? C9 C4 N2 120.2(3) . . ? C6 C5 C4 121.6(3) . . ? C6 C5 H5 119.2 . . ? C4 C5 H5 119.2 . . ? C5 C6 C7 118.9(3) . . ? C5 C6 H6 120.6 . . ? C7 C6 H6 120.6 . . ? C6 C7 C8 120.5(3) . . ? C6 C7 H7 119.7 . . ? C8 C7 H7 119.7 . . ? C7 C8 C9 122.3(3) . . ? C7 C8 H8 118.8 . . ? C9 C8 H8 118.8 . . ? N1 C9 C8 121.7(3) . . ? N1 C9 C4 122.5(3) . . ? C8 C9 C4 115.8(3) . . ? N3 C10 C12 110.2(3) . . ? N3 C10 C11 109.2(3) . . ? C12 C10 C11 112.8(3) . . ? N3 C10 H10 108.2 . . ? C12 C10 H10 108.2 . . ? C11 C10 H10 108.2 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C18 C13 C14 121.6(3) . . ? C18 C13 N1 118.4(3) . . ? C14 C13 N1 120.0(3) . . ? C15 C14 C13 117.5(3) . . ? C15 C14 C22 119.9(3) . . ? C13 C14 C22 122.6(3) . . ? C16 C15 C14 121.8(4) . . ? C16 C15 H15 119.1 . . ? C14 C15 H15 119.1 . . ? C17 C16 C15 119.8(3) . . ? C17 C16 H16 120.1 . . ? C15 C16 H16 120.1 . . ? C16 C17 C18 121.4(3) . . ? C16 C17 H17 119.3 . . ? C18 C17 H17 119.3 . . ? C17 C18 C13 117.9(3) . . ? C17 C18 C19 121.2(3) . . ? C13 C18 C19 120.9(3) . . ? C20 C19 C21 111.4(4) . . ? C20 C19 C18 112.1(3) . . ? C21 C19 C18 112.7(4) . . ? C20 C19 H19 106.7 . . ? C21 C19 H19 106.7 . . ? C18 C19 H19 106.7 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C14 C22 C24 112.4(3) . . ? C14 C22 C23 111.4(3) . . ? C24 C22 C23 109.7(3) . . ? C14 C22 H22 107.7 . . ? C24 C22 H22 107.7 . . ? C23 C22 H22 107.7 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? 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 C1 Pd1 O1 Pd1 -174.70(10) . . . 6_554 ? N1 Pd1 O1 Pd1 35.8(6) . . . 6_554 ? O1 Pd1 O1 Pd1 -4.64(12) 6_554 . . 6_554 ? C1 Pd1 N1 C9 -29.1(3) . . . . ? O1 Pd1 N1 C9 120.9(6) . . . . ? O1 Pd1 N1 C9 160.4(2) 6_554 . . . ? Pd1 Pd1 N1 C9 151.5(2) 6_554 . . . ? C1 Pd1 N1 C13 173.5(2) . . . . ? O1 Pd1 N1 C13 -36.5(7) . . . . ? O1 Pd1 N1 C13 2.9(2) 6_554 . . . ? Pd1 Pd1 N1 C13 -6.0(2) 6_554 . . . ? C3 N3 C1 N2 0.5(3) . . . . ? C10 N3 C1 N2 -170.6(3) . . . . ? C3 N3 C1 Pd1 175.9(2) . . . . ? C10 N3 C1 Pd1 4.7(5) . . . . ? C2 N2 C1 N3 -0.7(3) . . . . ? C4 N2 C1 N3 175.0(3) . . . . ? C2 N2 C1 Pd1 -176.2(2) . . . . ? C4 N2 C1 Pd1 -0.5(4) . . . . ? N1 Pd1 C1 N3 -155.2(3) . . . . ? O1 Pd1 C1 N3 29.2(3) . . . . ? O1 Pd1 C1 N3 -41.0(8) 6_554 . . . ? Pd1 Pd1 C1 N3 24.2(3) 6_554 . . . ? N1 Pd1 C1 N2 19.3(3) . . . . ? O1 Pd1 C1 N2 -156.3(2) . . . . ? O1 Pd1 C1 N2 133.5(5) 6_554 . . . ? Pd1 Pd1 C1 N2 -161.30(18) 6_554 . . . ? C1 N2 C2 C3 0.6(4) . . . . ? C4 N2 C2 C3 -175.3(3) . . . . ? N2 C2 C3 N3 -0.2(4) . . . . ? C1 N3 C3 C2 -0.2(4) . . . . ? C10 N3 C3 C2 171.3(3) . . . . ? C1 N2 C4 C5 163.8(3) . . . . ? C2 N2 C4 C5 -21.1(4) . . . . ? C1 N2 C4 C9 -19.6(4) . . . . ? C2 N2 C4 C9 155.5(3) . . . . ? C9 C4 C5 C6 -3.0(4) . . . . ? N2 C4 C5 C6 173.6(3) . . . . ? C4 C5 C6 C7 -1.4(5) . . . . ? C5 C6 C7 C8 2.9(5) . . . . ? C6 C7 C8 C9 0.0(5) . . . . ? C13 N1 C9 C8 -4.0(4) . . . . ? Pd1 N1 C9 C8 -160.2(2) . . . . ? C13 N1 C9 C4 175.6(3) . . . . ? Pd1 N1 C9 C4 19.4(4) . . . . ? C7 C8 C9 N1 175.4(3) . . . . ? C7 C8 C9 C4 -4.2(4) . . . . ? C5 C4 C9 N1 -174.0(3) . . . . ? N2 C4 C9 N1 9.4(4) . . . . ? C5 C4 C9 C8 5.6(4) . . . . ? N2 C4 C9 C8 -171.0(3) . . . . ? C1 N3 C10 C12 -143.7(3) . . . . ? C3 N3 C10 C12 46.1(4) . . . . ? C1 N3 C10 C11 91.9(4) . . . . ? C3 N3 C10 C11 -78.3(4) . . . . ? C9 N1 C13 C18 105.5(3) . . . . ? Pd1 N1 C13 C18 -94.4(3) . . . . ? C9 N1 C13 C14 -76.3(4) . . . . ? Pd1 N1 C13 C14 83.8(3) . . . . ? C18 C13 C14 C15 2.3(5) . . . . ? N1 C13 C14 C15 -175.8(3) . . . . ? C18 C13 C14 C22 -176.7(3) . . . . ? N1 C13 C14 C22 5.2(5) . . . . ? C13 C14 C15 C16 -1.0(5) . . . . ? C22 C14 C15 C16 178.0(3) . . . . ? C14 C15 C16 C17 -0.9(6) . . . . ? C15 C16 C17 C18 1.7(6) . . . . ? C16 C17 C18 C13 -0.4(5) . . . . ? C16 C17 C18 C19 179.2(4) . . . . ? C14 C13 C18 C17 -1.6(5) . . . . ? N1 C13 C18 C17 176.5(3) . . . . ? C14 C13 C18 C19 178.8(3) . . . . ? N1 C13 C18 C19 -3.1(5) . . . . ? C17 C18 C19 C20 -71.9(5) . . . . ? C13 C18 C19 C20 107.7(5) . . . . ? C17 C18 C19 C21 54.7(5) . . . . ? C13 C18 C19 C21 -125.7(4) . . . . ? C15 C14 C22 C24 68.5(4) . . . . ? C13 C14 C22 C24 -112.6(4) . . . . ? C15 C14 C22 C23 -55.1(4) . . . . ? C13 C14 C22 C23 123.9(3) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.690 _refine_diff_density_min -0.388 _refine_diff_density_rms 0.098