# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_c:\Complex_1 _database_code_depnum_ccdc_archive 'CCDC 825045' #TrackingRef 'web_deposit_cif_file_0_Dr.RoderickC.Jones_1305088168.cif' #=============================================================================== # start Validation Reply Form _THETM01_ALERT_3_B ; PROBLEM: The value of sine(theta_max)/wavelength is less than 0.575 Calculated sin(theta_max)/wavelength = 0.5702 RESPONSE: The resolution limitation is due to the size of the detector at the Australian synchrotron ; # end Validation Reply Form #================================== _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C14 H26 P2 Pd' _chemical_formula_sum 'C14 H26 P2 Pd' _chemical_formula_weight 362.69 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.782(2) _cell_length_b 18.624(3) _cell_length_c 10.664(2) _cell_angle_alpha 90.00 _cell_angle_beta 107.991(16) _cell_angle_gamma 90.00 _cell_volume 1658.9(6) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 12390 _cell_measurement_theta_min 2.49 _cell_measurement_theta_max 26.22 _exptl_crystal_description rod _exptl_crystal_colour colourless _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.452 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 744 _exptl_absorpt_coefficient_mu 1.292 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.77488 _diffrn_radiation_type Synchrotron _diffrn_radiation_source 'synchrotron BM' _diffrn_radiation_monochromator Si<111> _diffrn_measurement_device_type '3-BM1 Australian Synchrotron' _diffrn_measurement_method Rotation _diffrn_detector_area_resol_mean 'ADSC Q210' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17001 _diffrn_reflns_av_R_equivalents 0.0926 _diffrn_reflns_av_sigmaI/netI 0.0558 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.49 _diffrn_reflns_theta_max 26.22 _reflns_number_total 2520 _reflns_number_gt 2152 _reflns_threshold_expression >2sigma(I) _computing_data_collection BLU-ICE _computing_cell_refinement XDS _computing_data_reduction XDS _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; 'X-SEED (Barbour, 2008) and ORTEPIII (Farrugia, 2008)' ; _computing_publication_material 'WinGX (Farrugia, 1999)' _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. The asymmetric unit contains one discrete molecule. All non-hydrogen atom positions were refined anisotropically. All hydrogens were included in calculated positons with a "riding" model. ; _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^)+(0.0595P)^2^+2.3621P] 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 2520 _refine_ls_number_parameters 160 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0523 _refine_ls_R_factor_gt 0.0449 _refine_ls_wR_factor_ref 0.1131 _refine_ls_wR_factor_gt 0.1106 _refine_ls_goodness_of_fit_ref 1.086 _refine_ls_restrained_S_all 1.086 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.86007(4) 0.19427(2) 0.80607(4) 0.01859(18) Uani 1 1 d . . . P1 P 0.64606(15) 0.26080(8) 0.82179(15) 0.0241(3) Uani 1 1 d . . . P2 P 0.70271(16) 0.09576(8) 0.80267(15) 0.0249(3) Uani 1 1 d . . . C1 C 1.0578(7) 0.1312(3) 0.8072(7) 0.0340(14) Uani 1 1 d . . . H1A H 1.1037 0.1490 0.7402 0.051 Uiso 1 1 calc R . . H1B H 1.0237 0.0813 0.7876 0.051 Uiso 1 1 calc R . . H1C H 1.1385 0.1339 0.8942 0.051 Uiso 1 1 calc R . . C2 C 1.0060(6) 0.2820(3) 0.8168(6) 0.0228(12) Uani 1 1 d . . . C3 C 0.9803(6) 0.3323(3) 0.7129(6) 0.0255(12) Uani 1 1 d . . . H3 H 0.8917 0.3257 0.6357 0.031 Uiso 1 1 calc R . . C4 C 1.0805(6) 0.3910(3) 0.7201(6) 0.0268(13) Uani 1 1 d . . . H4 H 1.0594 0.4228 0.6470 0.032 Uiso 1 1 calc R . . C5 C 1.2107(6) 0.4047(3) 0.8312(6) 0.0237(12) Uani 1 1 d . . . C6 C 1.2384(6) 0.3556(3) 0.9356(6) 0.0251(12) Uani 1 1 d . . . H6 H 1.3255 0.3631 1.0135 0.030 Uiso 1 1 calc R . . C7 C 1.1399(6) 0.2960(3) 0.9264(6) 0.0234(12) Uani 1 1 d . . . H7 H 1.1646 0.2631 0.9979 0.028 Uiso 1 1 calc R . . C8 C 1.3142(7) 0.4707(3) 0.8423(7) 0.0362(15) Uani 1 1 d . . . H8A H 1.2907 0.4935 0.7556 0.054 Uiso 1 1 calc R . . H8B H 1.4273 0.4568 0.8738 0.054 Uiso 1 1 calc R . . H8C H 1.2916 0.5045 0.9047 0.054 Uiso 1 1 calc R . . C9 C 0.5236(8) 0.3128(4) 0.6843(7) 0.0419(17) Uani 1 1 d . . . H9A H 0.4302 0.3314 0.7056 0.063 Uiso 1 1 calc R . . H9B H 0.4880 0.2822 0.6059 0.063 Uiso 1 1 calc R . . H9C H 0.5864 0.3529 0.6670 0.063 Uiso 1 1 calc R . . C10 C 0.6809(7) 0.3240(4) 0.9574(6) 0.0365(15) Uani 1 1 d . . . H10A H 0.7617 0.3592 0.9520 0.055 Uiso 1 1 calc R . . H10B H 0.7191 0.2980 1.0413 0.055 Uiso 1 1 calc R . . H10C H 0.5808 0.3489 0.9522 0.055 Uiso 1 1 calc R . . C11 C 0.6715(9) 0.0277(4) 0.6742(7) 0.0499(19) Uani 1 1 d . . . H11A H 0.7744 0.0058 0.6783 0.075 Uiso 1 1 calc R . . H11B H 0.6245 0.0501 0.5877 0.075 Uiso 1 1 calc R . . H11C H 0.5989 -0.0094 0.6876 0.075 Uiso 1 1 calc R . . C12 C 0.7647(7) 0.0411(4) 0.9503(7) 0.0383(15) Uani 1 1 d . . . H12A H 0.6874 0.0021 0.9431 0.057 Uiso 1 1 calc R . . H12B H 0.7696 0.0708 1.0272 0.057 Uiso 1 1 calc R . . H12C H 0.8707 0.0207 0.9603 0.057 Uiso 1 1 calc R . . C21 C 0.5054(8) 0.1962(4) 0.8600(9) 0.050(2) Uani 1 1 d . . . H21A H 0.5380 0.1883 0.9565 0.060 Uiso 1 1 calc R . . H21B H 0.3966 0.2173 0.8329 0.060 Uiso 1 1 calc R . . C22 C 0.5006(7) 0.1266(4) 0.7932(8) 0.0468(19) Uani 1 1 d . . . H22A H 0.4353 0.1312 0.6995 0.056 Uiso 1 1 calc R . . H22B H 0.4489 0.0904 0.8347 0.056 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 0.0108(2) 0.0188(3) 0.0273(3) -0.00205(17) 0.00758(17) -0.00057(14) P1 0.0118(6) 0.0275(8) 0.0322(8) -0.0050(6) 0.0059(6) 0.0013(5) P2 0.0172(7) 0.0245(8) 0.0325(8) 0.0015(6) 0.0071(6) -0.0039(5) C1 0.022(3) 0.030(3) 0.052(4) -0.008(3) 0.015(3) -0.005(2) C2 0.018(3) 0.022(3) 0.035(3) -0.002(2) 0.017(2) 0.006(2) C3 0.021(3) 0.028(3) 0.027(3) 0.003(3) 0.007(2) 0.000(2) C4 0.025(3) 0.024(3) 0.036(3) 0.003(3) 0.015(3) 0.004(2) C5 0.016(3) 0.026(3) 0.033(3) -0.003(3) 0.014(2) 0.000(2) C6 0.013(2) 0.036(3) 0.026(3) -0.003(3) 0.005(2) 0.000(2) C7 0.013(3) 0.029(3) 0.029(3) 0.005(2) 0.008(2) 0.000(2) C8 0.031(3) 0.026(3) 0.054(4) -0.003(3) 0.016(3) -0.004(3) C9 0.031(3) 0.056(4) 0.037(4) 0.003(3) 0.009(3) 0.024(3) C10 0.027(3) 0.046(4) 0.038(4) -0.012(3) 0.012(3) 0.007(3) C11 0.068(5) 0.038(4) 0.052(4) -0.017(3) 0.030(4) -0.033(3) C12 0.026(3) 0.043(4) 0.046(4) 0.010(3) 0.010(3) -0.004(3) C21 0.021(3) 0.058(5) 0.079(6) -0.006(4) 0.027(4) -0.001(3) C22 0.023(3) 0.035(4) 0.082(6) 0.018(4) 0.015(3) 0.000(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 C2 2.058(5) . ? Pd1 C1 2.093(6) . ? Pd1 P2 2.2903(14) . ? Pd1 P1 2.3000(14) . ? P1 C9 1.808(6) . ? P1 C10 1.816(6) . ? P1 C21 1.857(7) . ? P2 C12 1.812(6) . ? P2 C11 1.824(7) . ? P2 C22 1.839(6) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C7 1.403(8) . ? C2 C3 1.414(8) . ? C3 C4 1.391(8) . ? C3 H3 0.9500 . ? C4 C5 1.392(8) . ? C4 H4 0.9500 . ? C5 C6 1.402(8) . ? C5 C8 1.512(8) . ? C6 C7 1.392(8) . ? C6 H6 0.9500 . ? C7 H7 0.9500 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C21 C22 1.475(10) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 Pd1 C1 86.8(2) . . ? C2 Pd1 P2 177.77(17) . . ? C1 Pd1 P2 92.64(16) . . ? C2 Pd1 P1 94.41(14) . . ? C1 Pd1 P1 175.49(19) . . ? P2 Pd1 P1 85.99(5) . . ? C9 P1 C10 102.1(3) . . ? C9 P1 C21 104.8(4) . . ? C10 P1 C21 101.8(3) . . ? C9 P1 Pd1 121.6(2) . . ? C10 P1 Pd1 117.8(2) . . ? C21 P1 Pd1 106.3(2) . . ? C12 P2 C11 101.3(3) . . ? C12 P2 C22 104.4(3) . . ? C11 P2 C22 104.9(4) . . ? C12 P2 Pd1 114.8(2) . . ? C11 P2 Pd1 121.2(2) . . ? C22 P2 Pd1 108.6(2) . . ? Pd1 C1 H1A 109.5 . . ? Pd1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? Pd1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C7 C2 C3 114.8(5) . . ? C7 C2 Pd1 122.7(4) . . ? C3 C2 Pd1 122.4(4) . . ? C4 C3 C2 122.2(5) . . ? C4 C3 H3 118.9 . . ? C2 C3 H3 118.9 . . ? C5 C4 C3 121.9(5) . . ? C5 C4 H4 119.0 . . ? C3 C4 H4 119.0 . . ? C4 C5 C6 116.9(5) . . ? C4 C5 C8 122.1(5) . . ? C6 C5 C8 121.0(5) . . ? C7 C6 C5 120.8(5) . . ? C7 C6 H6 119.6 . . ? C5 C6 H6 119.6 . . ? C6 C7 C2 123.3(5) . . ? C6 C7 H7 118.3 . . ? C2 C7 H7 118.3 . . ? C5 C8 H8A 109.5 . . ? C5 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C5 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? P1 C9 H9A 109.5 . . ? P1 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? P1 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? P1 C10 H10A 109.5 . . ? P1 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? P1 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? P2 C11 H11A 109.5 . . ? P2 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? P2 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? P2 C12 H12A 109.5 . . ? P2 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? P2 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C22 C21 P1 112.7(5) . . ? C22 C21 H21A 109.1 . . ? P1 C21 H21A 109.1 . . ? C22 C21 H21B 109.1 . . ? P1 C21 H21B 109.1 . . ? H21A C21 H21B 107.8 . . ? C21 C22 P2 111.4(4) . . ? C21 C22 H22A 109.4 . . ? P2 C22 H22A 109.4 . . ? C21 C22 H22B 109.4 . . ? P2 C22 H22B 109.4 . . ? H22A C22 H22B 108.0 . . ? 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 C2 Pd1 P1 C9 75.2(3) . . . . ? C1 Pd1 P1 C9 -179(100) . . . . ? P2 Pd1 P1 C9 -107.0(3) . . . . ? C2 Pd1 P1 C10 -51.9(3) . . . . ? C1 Pd1 P1 C10 53(2) . . . . ? P2 Pd1 P1 C10 125.9(3) . . . . ? C2 Pd1 P1 C21 -165.2(3) . . . . ? C1 Pd1 P1 C21 -60(2) . . . . ? P2 Pd1 P1 C21 12.6(3) . . . . ? C2 Pd1 P2 C12 -9(4) . . . . ? C1 Pd1 P2 C12 66.2(3) . . . . ? P1 Pd1 P2 C12 -109.5(2) . . . . ? C2 Pd1 P2 C11 -131(4) . . . . ? C1 Pd1 P2 C11 -56.0(4) . . . . ? P1 Pd1 P2 C11 128.3(3) . . . . ? C2 Pd1 P2 C22 107(4) . . . . ? C1 Pd1 P2 C22 -177.4(3) . . . . ? P1 Pd1 P2 C22 6.9(3) . . . . ? C1 Pd1 C2 C7 -65.3(5) . . . . ? P2 Pd1 C2 C7 10(4) . . . . ? P1 Pd1 C2 C7 110.3(4) . . . . ? C1 Pd1 C2 C3 113.6(5) . . . . ? P2 Pd1 C2 C3 -171(3) . . . . ? P1 Pd1 C2 C3 -70.8(4) . . . . ? C7 C2 C3 C4 -0.3(8) . . . . ? Pd1 C2 C3 C4 -179.2(4) . . . . ? C2 C3 C4 C5 -1.2(9) . . . . ? C3 C4 C5 C6 1.1(8) . . . . ? C3 C4 C5 C8 -176.5(5) . . . . ? C4 C5 C6 C7 0.5(8) . . . . ? C8 C5 C6 C7 178.1(5) . . . . ? C5 C6 C7 C2 -2.0(8) . . . . ? C3 C2 C7 C6 1.9(8) . . . . ? Pd1 C2 C7 C6 -179.2(4) . . . . ? C9 P1 C21 C22 93.8(6) . . . . ? C10 P1 C21 C22 -160.0(6) . . . . ? Pd1 P1 C21 C22 -36.1(6) . . . . ? P1 C21 C22 P2 43.5(7) . . . . ? C12 P2 C22 C21 91.8(6) . . . . ? C11 P2 C22 C21 -162.0(6) . . . . ? Pd1 P2 C22 C21 -31.1(6) . . . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 26.22 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.846 _refine_diff_density_min -1.330 _refine_diff_density_rms 0.128 data_c:\Complex_2 _database_code_depnum_ccdc_archive 'CCDC 825046' #TrackingRef 'web_deposit_cif_file_1_Dr.RoderickC.Jones_1305088168.cif' #=============================================================================== # start Validation Reply Form _THETM01_ALERT_3_B ; PROBLEM: The value of sine(theta_max)/wavelength is less than 0.575 Calculated sin(theta_max)/wavelength = 0.5704 RESPONSE: The resolution limitation is due to the size of the detector at the Australian synchrotron ; # end Validation Reply Form #================================== _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C18 H18 N2 Pd' _chemical_formula_sum 'C18 H18 N2 Pd' _chemical_formula_weight 368.74 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' Pd Pd -0.9988 1.0072 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c _symmetry_space_group_name_Hall '-C 2yc' _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 47.366(2) _cell_length_b 8.4950(9) _cell_length_c 25.0650(15) _cell_angle_alpha 90.00 _cell_angle_beta 115.3600(10) _cell_angle_gamma 90.00 _cell_volume 9113.6(12) _cell_formula_units_Z 24 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 39584 _cell_measurement_theta_min 1.96 _cell_measurement_theta_max 26.23 _exptl_crystal_description rod _exptl_crystal_colour yellow _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.612 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4464 _exptl_absorpt_coefficient_mu 1.216 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.77487 _diffrn_radiation_type Synchrotron _diffrn_radiation_source 'synchrotron BM' _diffrn_radiation_monochromator Si<111> _diffrn_measurement_device_type '3-BM1 Australian Synchrotron' _diffrn_measurement_method Rotation _diffrn_detector_area_resol_mean 'ADSC Q210' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 46306 _diffrn_reflns_av_R_equivalents 0.0324 _diffrn_reflns_av_sigmaI/netI 0.0166 _diffrn_reflns_limit_h_min -53 _diffrn_reflns_limit_h_max 54 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.96 _diffrn_reflns_theta_max 26.23 _reflns_number_total 6953 _reflns_number_gt 6758 _reflns_threshold_expression >2sigma(I) _computing_data_collection BLU-ICE _computing_cell_refinement XDS _computing_data_reduction XDS _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; 'X-SEED (Barbour, 2008) and ORTEPIII (Farrugia, 2008)' ; _computing_publication_material 'WinGX (Farrugia, 1999)' _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.The asymmetric unit contains three discrete molecule. All non-hydrogen atom positions were refined anisotropically. All hydrogens were included in calculated positons with a "riding" model. ; _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^)+(0.0350P)^2^+178.5525P] 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 6953 _refine_ls_number_parameters 553 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0466 _refine_ls_R_factor_gt 0.0458 _refine_ls_wR_factor_ref 0.1075 _refine_ls_wR_factor_gt 0.1070 _refine_ls_goodness_of_fit_ref 1.081 _refine_ls_restrained_S_all 1.081 _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 Pd11 Pd 0.188340(9) -0.05294(5) 0.545840(17) 0.01278(12) Uani 1 1 d . . . Pd12 Pd 0.038188(9) 0.52178(5) 0.379951(17) 0.01315(12) Uani 1 1 d . . . Pd13 Pd 0.138805(9) 0.02675(5) 0.302983(17) 0.01291(12) Uani 1 1 d . . . N11 N 0.18368(10) 0.1703(5) 0.58045(18) 0.0140(9) Uani 1 1 d . . . N12 N 0.03194(11) 0.2955(5) 0.4108(2) 0.0194(10) Uani 1 1 d . . . N13 N 0.14397(10) 0.2526(5) 0.27039(19) 0.0176(10) Uani 1 1 d . . . N21 N 0.22857(9) 0.0700(5) 0.55186(19) 0.0136(9) Uani 1 1 d . . . N22 N 0.08118(11) 0.4052(5) 0.39670(19) 0.0169(10) Uani 1 1 d . . . N23 N 0.09568(10) 0.1406(5) 0.28717(19) 0.0159(10) Uani 1 1 d . . . C11 C 0.19499(12) -0.2566(7) 0.5088(2) 0.0193(12) Uani 1 1 d . . . H11A H 0.1824 -0.3412 0.5144 0.029 Uiso 1 1 calc R . . H11B H 0.2171 -0.2859 0.5278 0.029 Uiso 1 1 calc R . . H11C H 0.1886 -0.2403 0.4665 0.029 Uiso 1 1 calc R . . C12 C 0.04895(13) 0.7262(7) 0.3498(2) 0.0218(12) Uani 1 1 d . . . H12A H 0.0321 0.8027 0.3414 0.033 Uiso 1 1 calc R . . H12B H 0.0514 0.7050 0.3136 0.033 Uiso 1 1 calc R . . H12C H 0.0685 0.7690 0.3799 0.033 Uiso 1 1 calc R . . C13 C 0.13021(12) -0.1744(7) 0.3379(2) 0.0211(12) Uani 1 1 d . . . H13A H 0.1470 -0.2505 0.3448 0.032 Uiso 1 1 calc R . . H13B H 0.1102 -0.2193 0.3103 0.032 Uiso 1 1 calc R . . H13C H 0.1293 -0.1500 0.3754 0.032 Uiso 1 1 calc R . . C21 C 0.15212(12) -0.1582(6) 0.5516(2) 0.0147(11) Uani 1 1 d . . . C22 C -0.00106(12) 0.6277(6) 0.3737(2) 0.0164(11) Uani 1 1 d . . . C23 C 0.17706(12) -0.0769(6) 0.3041(2) 0.0164(11) Uani 1 1 d . . . C31 C 0.15037(12) -0.1458(6) 0.6063(2) 0.0165(11) Uani 1 1 d . . . H31 H 0.1668 -0.0944 0.6382 0.020 Uiso 1 1 calc R . . C32 C -0.00840(12) 0.6225(7) 0.4222(2) 0.0197(12) Uani 1 1 d . . . H32 H 0.0051 0.5670 0.4566 0.024 Uiso 1 1 calc R . . C33 C 0.18086(12) -0.0676(7) 0.2520(2) 0.0187(12) Uani 1 1 d . . . H33 H 0.1655 -0.0137 0.2192 0.022 Uiso 1 1 calc R . . C41 C 0.12545(12) -0.2062(6) 0.6149(2) 0.0165(11) Uani 1 1 d . . . H41 H 0.1253 -0.1962 0.6525 0.020 Uiso 1 1 calc R . . C42 C -0.03465(13) 0.6955(7) 0.4217(3) 0.0233(13) Uani 1 1 d . . . H42 H -0.0386 0.6898 0.4558 0.028 Uiso 1 1 calc R . . C43 C 0.20628(12) -0.1343(7) 0.2464(3) 0.0203(12) Uani 1 1 d . . . H43 H 0.2078 -0.1254 0.2099 0.024 Uiso 1 1 calc R . . C51 C 0.10083(12) -0.2807(6) 0.5697(2) 0.0169(11) Uani 1 1 d . . . C52 C -0.05534(13) 0.7768(7) 0.3724(3) 0.0258(14) Uani 1 1 d . . . C53 C 0.22950(12) -0.2139(7) 0.2933(3) 0.0208(12) Uani 1 1 d . . . C61 C 0.10224(13) -0.2966(6) 0.5157(2) 0.0199(12) Uani 1 1 d . . . H61 H 0.0858 -0.3491 0.4841 0.024 Uiso 1 1 calc R . . C62 C -0.04850(13) 0.7819(7) 0.3237(3) 0.0257(13) Uani 1 1 d . . . H62 H -0.0623 0.8357 0.2890 0.031 Uiso 1 1 calc R . . C63 C 0.22581(13) -0.2232(7) 0.3453(3) 0.0230(13) Uani 1 1 d . . . H63 H 0.2411 -0.2769 0.3783 0.028 Uiso 1 1 calc R . . C71 C 0.12725(13) -0.2368(6) 0.5074(2) 0.0182(12) Uani 1 1 d . . . H71 H 0.1275 -0.2500 0.4700 0.022 Uiso 1 1 calc R . . C72 C -0.02182(12) 0.7095(7) 0.3245(3) 0.0217(12) Uani 1 1 d . . . H72 H -0.0178 0.7164 0.2906 0.026 Uiso 1 1 calc R . . C73 C 0.20037(12) -0.1559(7) 0.3502(2) 0.0191(12) Uani 1 1 d . . . H73 H 0.1989 -0.1644 0.3867 0.023 Uiso 1 1 calc R . . C81 C 0.07346(14) -0.3435(8) 0.5790(3) 0.0319(15) Uani 1 1 d . . . H81A H 0.0786 -0.4478 0.5974 0.048 Uiso 1 1 calc R . . H81B H 0.0552 -0.3516 0.5408 0.048 Uiso 1 1 calc R . . H81C H 0.0688 -0.2718 0.6048 0.048 Uiso 1 1 calc R . . C82 C -0.08403(15) 0.8565(8) 0.3713(3) 0.0393(17) Uani 1 1 d . . . H82A H -0.0973 0.7783 0.3780 0.059 Uiso 1 1 calc R . . H82B H -0.0956 0.9063 0.3327 0.059 Uiso 1 1 calc R . . H82C H -0.0778 0.9369 0.4023 0.059 Uiso 1 1 calc R . . C83 C 0.25690(5) -0.2892(3) 0.28710(9) 0.0342(16) Uani 1 1 d . . . H83A H 0.2722 -0.3252 0.3259 0.051 Uiso 1 1 calc R . . H83B H 0.2667 -0.2119 0.2713 0.051 Uiso 1 1 calc R . . H83C H 0.2496 -0.3792 0.2602 0.051 Uiso 1 1 calc R . . C211 C 0.20799(5) 0.2695(3) 0.59357(8) 0.0176(12) Uani 1 1 d R . . C212 C 0.05722(5) 0.2000(3) 0.42946(11) 0.0196(12) Uani 1 1 d R . . C213 C 0.11859(6) 0.3468(3) 0.25356(10) 0.0181(12) Uani 1 1 d R . . C221 C 0.23431(5) 0.2084(3) 0.58186(8) 0.0175(12) Uani 1 1 d R . . C222 C 0.08507(5) 0.2632(3) 0.42372(9) 0.0183(12) Uani 1 1 d R . . C223 C 0.09099(6) 0.2783(4) 0.25784(9) 0.0177(12) Uani 1 1 d R . . C311 C 0.20761(5) 0.4203(3) 0.61362(9) 0.0265(13) Uani 1 1 d R . . H311 H 0.2252 0.4870 0.6234 0.032 Uiso 1 1 calc R . . C312 C 0.05662(16) 0.0504(7) 0.4509(3) 0.0285(14) Uani 1 1 d . . . H312 H 0.0749 -0.0132 0.4652 0.034 Uiso 1 1 calc R . . C313 C 0.11956(16) 0.5014(7) 0.2360(3) 0.0283(14) Uani 1 1 d . . . H313 H 0.1015 0.5662 0.2239 0.034 Uiso 1 1 calc R . . C321 C 0.26223(13) 0.2896(7) 0.5989(2) 0.0229(13) Uani 1 1 d . . . H321 H 0.2658 0.3841 0.6211 0.027 Uiso 1 1 calc R . . C322 C 0.11313(14) 0.1830(7) 0.4427(2) 0.0238(13) Uani 1 1 d . . . H322 H 0.1156 0.0841 0.4618 0.029 Uiso 1 1 calc R . . C323 C 0.06196(14) 0.3528(7) 0.2342(2) 0.0235(13) Uani 1 1 d . . . H323 H 0.0589 0.4477 0.2124 0.028 Uiso 1 1 calc R . . C411 C 0.18144(16) 0.4741(7) 0.6195(3) 0.0309(15) Uani 1 1 d . . . H411 H 0.1808 0.5779 0.6330 0.037 Uiso 1 1 calc R . . C412 C 0.02939(17) -0.0061(7) 0.4514(3) 0.0347(16) Uani 1 1 d . . . H412 H 0.0286 -0.1091 0.4655 0.042 Uiso 1 1 calc R . . C413 C 0.14672(16) 0.5601(7) 0.2364(3) 0.0325(15) Uani 1 1 d . . . H413 H 0.1478 0.6664 0.2255 0.039 Uiso 1 1 calc R . . C421 C 0.28482(14) 0.2305(8) 0.5829(3) 0.0262(14) Uani 1 1 d . . . H421 H 0.3041 0.2841 0.5940 0.031 Uiso 1 1 calc R . . C422 C 0.13761(14) 0.2467(8) 0.4337(3) 0.0258(13) Uani 1 1 d . . . H422 H 0.1569 0.1925 0.4464 0.031 Uiso 1 1 calc R . . C423 C 0.03776(14) 0.2863(8) 0.2431(3) 0.0280(14) Uani 1 1 d . . . H423 H 0.0178 0.3348 0.2274 0.034 Uiso 1 1 calc R . . C511 C 0.15644(14) 0.3743(7) 0.6053(3) 0.0243(13) Uani 1 1 d . . . H511 H 0.1381 0.4084 0.6082 0.029 Uiso 1 1 calc R . . C512 C 0.00350(15) 0.0895(7) 0.4311(3) 0.0300(15) Uani 1 1 d . . . H512 H -0.0156 0.0529 0.4302 0.036 Uiso 1 1 calc R . . C513 C 0.17237(16) 0.4630(7) 0.2527(3) 0.0302(15) Uani 1 1 d . . . H513 H 0.1912 0.5003 0.2525 0.036 Uiso 1 1 calc R . . C521 C 0.27896(13) 0.0929(8) 0.5507(3) 0.0250(13) Uani 1 1 d . . . H521 H 0.2939 0.0515 0.5386 0.030 Uiso 1 1 calc R . . C522 C 0.13333(13) 0.3917(7) 0.4056(2) 0.0226(13) Uani 1 1 d . . . H522 H 0.1497 0.4379 0.3985 0.027 Uiso 1 1 calc R . . C523 C 0.04294(13) 0.1489(7) 0.2751(3) 0.0241(13) Uani 1 1 d . . . H523 H 0.0268 0.1033 0.2828 0.029 Uiso 1 1 calc R . . C611 C 0.15850(13) 0.2242(7) 0.5868(2) 0.0201(12) Uani 1 1 d . . . H611 H 0.1413 0.1549 0.5780 0.024 Uiso 1 1 calc R . . C612 C 0.00568(14) 0.2401(7) 0.4118(2) 0.0247(13) Uani 1 1 d . . . H612 H -0.0121 0.3066 0.3988 0.030 Uiso 1 1 calc R . . C613 C 0.17014(13) 0.3108(7) 0.2693(2) 0.0214(12) Uani 1 1 d . . . H613 H 0.1878 0.2440 0.2804 0.026 Uiso 1 1 calc R . . C621 C 0.25086(12) 0.0164(7) 0.5363(2) 0.0192(12) Uani 1 1 d . . . H621 H 0.2470 -0.0787 0.5144 0.023 Uiso 1 1 calc R . . C622 C 0.10505(13) 0.4671(7) 0.3882(2) 0.0193(12) Uani 1 1 d . . . H622 H 0.1023 0.5669 0.3695 0.023 Uiso 1 1 calc R . . C623 C 0.07208(13) 0.0779(7) 0.2958(2) 0.0203(12) Uani 1 1 d . . . H623 H 0.0754 -0.0185 0.3169 0.024 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 Pd11 0.0125(2) 0.0129(2) 0.0139(2) -0.00293(16) 0.00659(16) 0.00189(16) Pd12 0.0119(2) 0.0113(2) 0.0142(2) 0.00245(16) 0.00372(16) -0.00328(16) Pd13 0.0122(2) 0.0119(2) 0.0147(2) 0.00417(16) 0.00580(16) -0.00144(16) N11 0.013(2) 0.013(2) 0.016(2) 0.0008(18) 0.0073(18) 0.0033(19) N12 0.020(2) 0.018(2) 0.019(2) -0.0070(19) 0.007(2) -0.010(2) N13 0.019(2) 0.017(2) 0.015(2) -0.0011(19) 0.0056(19) -0.003(2) N21 0.005(2) 0.018(2) 0.019(2) 0.0034(19) 0.0061(18) -0.0014(18) N22 0.025(2) 0.012(2) 0.014(2) -0.0018(18) 0.0091(19) 0.000(2) N23 0.016(2) 0.015(2) 0.016(2) 0.0000(19) 0.0062(18) 0.0023(19) C11 0.012(3) 0.025(3) 0.022(3) -0.004(2) 0.010(2) -0.004(2) C12 0.018(3) 0.025(3) 0.022(3) -0.001(2) 0.009(2) -0.004(2) C13 0.013(3) 0.027(3) 0.026(3) -0.001(3) 0.012(2) -0.002(2) C21 0.018(3) 0.010(3) 0.016(3) 0.003(2) 0.006(2) 0.008(2) C22 0.010(2) 0.017(3) 0.019(3) -0.001(2) 0.004(2) -0.005(2) C23 0.012(3) 0.014(3) 0.019(3) 0.002(2) 0.004(2) -0.005(2) C31 0.015(3) 0.014(3) 0.016(3) -0.007(2) 0.002(2) 0.001(2) C32 0.014(3) 0.016(3) 0.023(3) 0.004(2) 0.002(2) -0.005(2) C33 0.009(3) 0.021(3) 0.020(3) 0.009(2) 0.001(2) -0.001(2) C41 0.012(3) 0.020(3) 0.016(3) -0.001(2) 0.005(2) 0.000(2) C42 0.016(3) 0.021(3) 0.031(3) -0.002(3) 0.009(2) -0.011(2) C43 0.016(3) 0.022(3) 0.024(3) -0.001(2) 0.010(2) -0.005(2) C51 0.013(3) 0.012(3) 0.022(3) 0.002(2) 0.004(2) 0.001(2) C52 0.009(3) 0.018(3) 0.045(4) -0.004(3) 0.006(3) -0.006(2) C53 0.009(3) 0.015(3) 0.036(3) 0.000(2) 0.007(2) -0.005(2) C61 0.017(3) 0.014(3) 0.022(3) 0.001(2) 0.002(2) -0.004(2) C62 0.019(3) 0.019(3) 0.029(3) 0.005(3) 0.001(3) -0.004(2) C63 0.013(3) 0.019(3) 0.030(3) 0.009(3) 0.003(2) 0.001(2) C71 0.022(3) 0.016(3) 0.017(3) 0.002(2) 0.008(2) 0.007(2) C72 0.016(3) 0.022(3) 0.025(3) 0.004(2) 0.007(2) -0.003(2) C73 0.017(3) 0.017(3) 0.024(3) 0.000(2) 0.009(2) -0.010(2) C81 0.019(3) 0.038(4) 0.037(4) 0.006(3) 0.010(3) -0.009(3) C82 0.022(3) 0.031(4) 0.064(5) -0.002(3) 0.017(3) 0.003(3) C83 0.019(3) 0.030(4) 0.054(4) -0.004(3) 0.016(3) 0.007(3) C211 0.022(3) 0.017(3) 0.015(3) 0.006(2) 0.009(2) 0.002(2) C212 0.027(3) 0.012(3) 0.017(3) -0.004(2) 0.007(2) -0.001(2) C213 0.025(3) 0.016(3) 0.013(3) -0.002(2) 0.008(2) -0.002(2) C221 0.021(3) 0.014(3) 0.016(3) 0.001(2) 0.007(2) -0.001(2) C222 0.024(3) 0.016(3) 0.015(3) -0.005(2) 0.008(2) -0.006(2) C223 0.025(3) 0.013(3) 0.016(3) -0.002(2) 0.010(2) 0.003(2) C311 0.034(3) 0.014(3) 0.036(3) -0.002(3) 0.020(3) -0.002(3) C312 0.038(4) 0.013(3) 0.036(4) 0.004(3) 0.018(3) 0.000(3) C313 0.047(4) 0.012(3) 0.027(3) 0.001(2) 0.016(3) 0.003(3) C321 0.027(3) 0.020(3) 0.020(3) 0.003(2) 0.009(2) 0.003(3) C322 0.029(3) 0.022(3) 0.016(3) 0.001(2) 0.006(2) 0.006(3) C323 0.028(3) 0.023(3) 0.019(3) 0.003(2) 0.010(2) 0.009(3) C411 0.048(4) 0.013(3) 0.039(4) -0.002(3) 0.025(3) 0.005(3) C412 0.052(4) 0.013(3) 0.044(4) 0.002(3) 0.026(3) -0.008(3) C413 0.051(4) 0.012(3) 0.032(3) 0.001(3) 0.015(3) -0.009(3) C421 0.018(3) 0.035(4) 0.025(3) 0.005(3) 0.009(2) -0.003(3) C422 0.022(3) 0.033(4) 0.023(3) -0.001(3) 0.010(2) 0.008(3) C423 0.019(3) 0.039(4) 0.023(3) 0.003(3) 0.006(2) 0.013(3) C511 0.025(3) 0.021(3) 0.030(3) 0.002(3) 0.015(3) 0.012(3) C512 0.036(4) 0.021(3) 0.034(3) -0.002(3) 0.015(3) -0.017(3) C513 0.035(4) 0.025(3) 0.029(3) -0.001(3) 0.012(3) -0.017(3) C521 0.020(3) 0.033(4) 0.024(3) 0.004(3) 0.012(2) 0.004(3) C522 0.016(3) 0.028(3) 0.023(3) -0.004(3) 0.008(2) -0.004(3) C523 0.017(3) 0.033(3) 0.024(3) -0.001(3) 0.011(2) 0.001(3) C611 0.019(3) 0.022(3) 0.021(3) 0.003(2) 0.010(2) 0.005(2) C612 0.021(3) 0.026(3) 0.022(3) -0.002(3) 0.004(2) -0.009(3) C613 0.020(3) 0.018(3) 0.021(3) 0.002(2) 0.004(2) -0.008(2) C621 0.016(3) 0.021(3) 0.022(3) 0.004(2) 0.010(2) 0.004(2) C622 0.021(3) 0.019(3) 0.019(3) -0.002(2) 0.010(2) -0.003(2) C623 0.019(3) 0.024(3) 0.021(3) 0.000(2) 0.011(2) -0.002(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd11 C21 1.994(5) . ? Pd11 C11 2.051(6) . ? Pd11 N21 2.121(4) . ? Pd11 N11 2.135(4) . ? Pd12 C22 2.010(5) . ? Pd12 C12 2.044(6) . ? Pd12 N22 2.138(5) . ? Pd12 N12 2.139(5) . ? Pd13 C23 2.003(5) . ? Pd13 C13 2.039(6) . ? Pd13 N23 2.138(4) . ? Pd13 N13 2.140(5) . ? N11 C611 1.349(7) . ? N11 C211 1.349(5) . ? N12 C612 1.341(7) . ? N12 C212 1.354(5) . ? N13 C613 1.346(7) . ? N13 C213 1.352(5) . ? N21 C621 1.351(7) . ? N21 C221 1.359(5) . ? N22 C622 1.344(7) . ? N22 C222 1.357(5) . ? N23 C623 1.337(7) . ? N23 C223 1.349(5) . ? 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 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C21 C71 1.394(8) . ? C21 C31 1.412(7) . ? C22 C72 1.389(8) . ? C22 C32 1.402(8) . ? C23 C73 1.382(8) . ? C23 C33 1.395(8) . ? C31 C41 1.386(8) . ? C31 H31 0.9500 . ? C32 C42 1.384(8) . ? C32 H32 0.9500 . ? C33 C43 1.392(8) . ? C33 H33 0.9500 . ? C41 C51 1.383(8) . ? C41 H41 0.9500 . ? C42 C52 1.388(9) . ? C42 H42 0.9500 . ? C43 C53 1.394(8) . ? C43 H43 0.9500 . ? C51 C61 1.391(8) . ? C51 C81 1.509(8) . ? C52 C62 1.393(9) . ? C52 C82 1.507(8) . ? C53 C63 1.389(8) . ? C53 C83 1.513(6) . ? C61 C71 1.383(8) . ? C61 H61 0.9500 . ? C62 C72 1.397(8) . ? C62 H62 0.9500 . ? C63 C73 1.386(8) . ? C63 H63 0.9500 . ? C71 H71 0.9500 . ? C72 H72 0.9500 . ? C73 H73 0.9500 . ? C81 H81A 0.9800 . ? C81 H81B 0.9800 . ? C81 H81C 0.9800 . ? C82 H82A 0.9800 . ? C82 H82B 0.9800 . ? C82 H82C 0.9800 . ? C83 H83A 0.9800 . ? C83 H83B 0.9800 . ? C83 H83C 0.9800 . ? C211 C311 1.3790 . ? C211 C221 1.4909 . ? C212 C312 1.384(6) . ? C212 C222 1.4873 . ? C213 C313 1.391(7) . ? C213 C223 1.4761 . ? C221 C321 1.387(6) . ? C222 C322 1.384(6) . ? C223 C323 1.394(6) . ? C311 C411 1.387(7) . ? C311 H311 0.9500 . ? C312 C412 1.382(9) . ? C312 H312 0.9500 . ? C313 C413 1.376(9) . ? C313 H313 0.9500 . ? C321 C421 1.387(8) . ? C321 H321 0.9500 . ? C322 C422 1.383(9) . ? C322 H322 0.9500 . ? C323 C423 1.379(9) . ? C323 H323 0.9500 . ? C411 C511 1.373(9) . ? C411 H411 0.9500 . ? C412 C512 1.374(10) . ? C412 H412 0.9500 . ? C413 C513 1.378(10) . ? C413 H413 0.9500 . ? C421 C521 1.379(9) . ? C421 H421 0.9500 . ? C422 C522 1.389(9) . ? C422 H422 0.9500 . ? C423 C523 1.377(9) . ? C423 H423 0.9500 . ? C511 C611 1.375(8) . ? C511 H511 0.9500 . ? C512 C612 1.387(9) . ? C512 H512 0.9500 . ? C513 C613 1.375(8) . ? C513 H513 0.9500 . ? C521 C621 1.383(8) . ? C521 H521 0.9500 . ? C522 C622 1.377(8) . ? C522 H522 0.9500 . ? C523 C623 1.387(8) . ? C523 H523 0.9500 . ? C611 H611 0.9500 . ? C612 H612 0.9500 . ? C613 H613 0.9500 . ? C621 H621 0.9500 . ? C622 H622 0.9500 . ? C623 H623 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 C21 Pd11 C11 87.6(2) . . ? C21 Pd11 N21 172.03(19) . . ? C11 Pd11 N21 98.07(19) . . ? C21 Pd11 N11 97.30(19) . . ? C11 Pd11 N11 174.68(19) . . ? N21 Pd11 N11 77.28(17) . . ? C22 Pd12 C12 87.7(2) . . ? C22 Pd12 N22 173.66(19) . . ? C12 Pd12 N22 95.7(2) . . ? C22 Pd12 N12 99.4(2) . . ? C12 Pd12 N12 172.8(2) . . ? N22 Pd12 N12 77.32(17) . . ? C23 Pd13 C13 88.4(2) . . ? C23 Pd13 N23 171.01(19) . . ? C13 Pd13 N23 96.2(2) . . ? C23 Pd13 N13 98.56(19) . . ? C13 Pd13 N13 172.6(2) . . ? N23 Pd13 N13 77.30(17) . . ? C611 N11 C211 117.7(4) . . ? C611 N11 Pd11 126.8(4) . . ? C211 N11 Pd11 115.3(3) . . ? C612 N12 C212 118.2(5) . . ? C612 N12 Pd12 126.6(4) . . ? C212 N12 Pd12 115.2(3) . . ? C613 N13 C213 118.6(4) . . ? C613 N13 Pd13 126.5(4) . . ? C213 N13 Pd13 114.7(3) . . ? C621 N21 C221 117.1(4) . . ? C621 N21 Pd11 127.1(4) . . ? C221 N21 Pd11 115.2(3) . . ? C622 N22 C222 118.9(4) . . ? C622 N22 Pd12 125.6(4) . . ? C222 N22 Pd12 115.1(3) . . ? C623 N23 C223 118.7(4) . . ? C623 N23 Pd13 126.1(4) . . ? C223 N23 Pd13 114.5(3) . . ? Pd11 C11 H11A 109.5 . . ? Pd11 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? Pd11 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? Pd12 C12 H12A 109.5 . . ? Pd12 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? Pd12 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? Pd13 C13 H13A 109.5 . . ? Pd13 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? Pd13 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C71 C21 C31 115.2(5) . . ? C71 C21 Pd11 128.2(4) . . ? C31 C21 Pd11 116.5(4) . . ? C72 C22 C32 116.2(5) . . ? C72 C22 Pd12 124.9(4) . . ? C32 C22 Pd12 118.9(4) . . ? C73 C23 C33 115.6(5) . . ? C73 C23 Pd13 128.3(4) . . ? C33 C23 Pd13 116.1(4) . . ? C41 C31 C21 122.1(5) . . ? C41 C31 H31 118.9 . . ? C21 C31 H31 118.9 . . ? C42 C32 C22 122.3(5) . . ? C42 C32 H32 118.9 . . ? C22 C32 H32 118.9 . . ? C43 C33 C23 122.4(5) . . ? C43 C33 H33 118.8 . . ? C23 C33 H33 118.8 . . ? C51 C41 C31 121.1(5) . . ? C51 C41 H41 119.4 . . ? C31 C41 H41 119.4 . . ? C32 C42 C52 121.3(6) . . ? C32 C42 H42 119.3 . . ? C52 C42 H42 119.3 . . ? C33 C43 C53 121.0(5) . . ? C33 C43 H43 119.5 . . ? C53 C43 H43 119.5 . . ? C41 C51 C61 117.8(5) . . ? C41 C51 C81 120.9(5) . . ? C61 C51 C81 121.2(5) . . ? C42 C52 C62 117.1(5) . . ? C42 C52 C82 121.9(6) . . ? C62 C52 C82 121.0(6) . . ? C63 C53 C43 116.7(5) . . ? C63 C53 C83 122.0(5) . . ? C43 C53 C83 121.3(5) . . ? C71 C61 C51 120.7(5) . . ? C71 C61 H61 119.6 . . ? C51 C61 H61 119.6 . . ? C52 C62 C72 121.4(5) . . ? C52 C62 H62 119.3 . . ? C72 C62 H62 119.3 . . ? C73 C63 C53 121.5(5) . . ? C73 C63 H63 119.2 . . ? C53 C63 H63 119.2 . . ? C61 C71 C21 123.0(5) . . ? C61 C71 H71 118.5 . . ? C21 C71 H71 118.5 . . ? C22 C72 C62 121.7(5) . . ? C22 C72 H72 119.1 . . ? C62 C72 H72 119.1 . . ? C23 C73 C63 122.7(5) . . ? C23 C73 H73 118.6 . . ? C63 C73 H73 118.6 . . ? C51 C81 H81A 109.5 . . ? C51 C81 H81B 109.5 . . ? H81A C81 H81B 109.5 . . ? C51 C81 H81C 109.5 . . ? H81A C81 H81C 109.5 . . ? H81B C81 H81C 109.5 . . ? C52 C82 H82A 109.5 . . ? C52 C82 H82B 109.5 . . ? H82A C82 H82B 109.5 . . ? C52 C82 H82C 109.5 . . ? H82A C82 H82C 109.5 . . ? H82B C82 H82C 109.5 . . ? C53 C83 H83A 109.5 . . ? C53 C83 H83B 109.5 . . ? H83A C83 H83B 109.5 . . ? C53 C83 H83C 109.5 . . ? H83A C83 H83C 109.5 . . ? H83B C83 H83C 109.5 . . ? N11 C211 C311 121.8(2) . . ? N11 C211 C221 115.7(2) . . ? C311 C211 C221 122.5 . . ? N12 C212 C312 121.5(4) . . ? N12 C212 C222 116.1(2) . . ? C312 C212 C222 122.4(3) . . ? N13 C213 C313 120.8(4) . . ? N13 C213 C223 116.1(2) . . ? C313 C213 C223 123.0(3) . . ? N21 C221 C321 122.6(3) . . ? N21 C221 C211 115.08(19) . . ? C321 C221 C211 122.3(3) . . ? N22 C222 C322 120.9(4) . . ? N22 C222 C212 115.7(2) . . ? C322 C222 C212 123.4(3) . . ? N23 C223 C323 121.8(4) . . ? N23 C223 C213 115.9(2) . . ? C323 C223 C213 122.2(3) . . ? C211 C311 C411 119.8(3) . . ? C211 C311 H311 120.1 . . ? C411 C311 H311 120.1 . . ? C412 C312 C212 119.8(6) . . ? C412 C312 H312 120.1 . . ? C212 C312 H312 120.1 . . ? C413 C313 C213 119.8(6) . . ? C413 C313 H313 120.1 . . ? C213 C313 H313 120.1 . . ? C221 C321 C421 118.9(5) . . ? C221 C321 H321 120.6 . . ? C421 C321 H321 120.6 . . ? C422 C322 C222 120.0(5) . . ? C422 C322 H322 120.0 . . ? C222 C322 H322 120.0 . . ? C423 C323 C223 118.9(5) . . ? C423 C323 H323 120.6 . . ? C223 C323 H323 120.6 . . ? C511 C411 C311 118.6(5) . . ? C511 C411 H411 120.7 . . ? C311 C411 H411 120.7 . . ? C512 C412 C312 118.7(6) . . ? C512 C412 H412 120.7 . . ? C312 C412 H412 120.7 . . ? C313 C413 C513 119.2(6) . . ? C313 C413 H413 120.4 . . ? C513 C413 H413 120.4 . . ? C521 C421 C321 119.3(6) . . ? C521 C421 H421 120.4 . . ? C321 C421 H421 120.4 . . ? C322 C422 C522 118.6(5) . . ? C322 C422 H422 120.7 . . ? C522 C422 H422 120.7 . . ? C523 C423 C323 119.2(5) . . ? C523 C423 H423 120.4 . . ? C323 C423 H423 120.4 . . ? C411 C511 C611 118.9(5) . . ? C411 C511 H511 120.6 . . ? C611 C511 H511 120.6 . . ? C412 C512 C612 119.1(6) . . ? C412 C512 H512 120.4 . . ? C612 C512 H512 120.4 . . ? C613 C513 C413 118.7(6) . . ? C613 C513 H513 120.6 . . ? C413 C513 H513 120.6 . . ? C421 C521 C621 118.7(5) . . ? C421 C521 H521 120.6 . . ? C621 C521 H521 120.6 . . ? C622 C522 C422 118.9(5) . . ? C622 C522 H522 120.5 . . ? C422 C522 H522 120.5 . . ? C423 C523 C623 119.2(5) . . ? C423 C523 H523 120.4 . . ? C623 C523 H523 120.4 . . ? N11 C611 C511 123.3(5) . . ? N11 C611 H611 118.4 . . ? C511 C611 H611 118.4 . . ? N12 C612 C512 122.6(6) . . ? N12 C612 H612 118.7 . . ? C512 C612 H612 118.7 . . ? N13 C613 C513 122.8(6) . . ? N13 C613 H613 118.6 . . ? C513 C613 H613 118.6 . . ? N21 C621 C521 123.4(5) . . ? N21 C621 H621 118.3 . . ? C521 C621 H621 118.3 . . ? N22 C622 C522 122.6(5) . . ? N22 C622 H622 118.7 . . ? C522 C622 H622 118.7 . . ? N23 C623 C523 122.2(5) . . ? N23 C623 H623 118.9 . . ? C523 C623 H623 118.9 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C21 Pd11 N11 C611 -15.8(5) . . . . ? C11 Pd11 N11 C611 141(2) . . . . ? N21 Pd11 N11 C611 170.2(5) . . . . ? C21 Pd11 N11 C211 168.7(3) . . . . ? C11 Pd11 N11 C211 -35(2) . . . . ? N21 Pd11 N11 C211 -5.4(3) . . . . ? C22 Pd12 N12 C612 12.5(5) . . . . ? C12 Pd12 N12 C612 -161.5(15) . . . . ? N22 Pd12 N12 C612 -173.1(5) . . . . ? C22 Pd12 N12 C212 -169.3(3) . . . . ? C12 Pd12 N12 C212 16.7(17) . . . . ? N22 Pd12 N12 C212 5.1(3) . . . . ? C23 Pd13 N13 C613 -16.6(5) . . . . ? C13 Pd13 N13 C613 143.3(15) . . . . ? N23 Pd13 N13 C613 171.5(5) . . . . ? C23 Pd13 N13 C213 168.3(3) . . . . ? C13 Pd13 N13 C213 -31.7(17) . . . . ? N23 Pd13 N13 C213 -3.5(3) . . . . ? C21 Pd11 N21 C621 133.2(13) . . . . ? C11 Pd11 N21 C621 -1.8(5) . . . . ? N11 Pd11 N21 C621 -179.2(5) . . . . ? C21 Pd11 N21 C221 -37.3(15) . . . . ? C11 Pd11 N21 C221 -172.3(3) . . . . ? N11 Pd11 N21 C221 10.3(3) . . . . ? C22 Pd12 N22 C622 -120.8(17) . . . . ? C12 Pd12 N22 C622 0.9(5) . . . . ? N12 Pd12 N22 C622 179.5(5) . . . . ? C22 Pd12 N22 C222 52.2(19) . . . . ? C12 Pd12 N22 C222 173.9(3) . . . . ? N12 Pd12 N22 C222 -7.5(3) . . . . ? C23 Pd13 N23 C623 115.8(12) . . . . ? C13 Pd13 N23 C623 -4.3(5) . . . . ? N13 Pd13 N23 C623 179.2(5) . . . . ? C23 Pd13 N23 C223 -54.0(13) . . . . ? C13 Pd13 N23 C223 -174.0(3) . . . . ? N13 Pd13 N23 C223 9.4(3) . . . . ? C11 Pd11 C21 C71 -50.8(5) . . . . ? N21 Pd11 C21 C71 173.7(11) . . . . ? N11 Pd11 C21 C71 127.1(5) . . . . ? C11 Pd11 C21 C31 132.6(4) . . . . ? N21 Pd11 C21 C31 -2.9(16) . . . . ? N11 Pd11 C21 C31 -49.5(4) . . . . ? C12 Pd12 C22 C72 49.1(5) . . . . ? N22 Pd12 C22 C72 171.2(15) . . . . ? N12 Pd12 C22 C72 -130.1(5) . . . . ? C12 Pd12 C22 C32 -129.9(4) . . . . ? N22 Pd12 C22 C32 -8(2) . . . . ? N12 Pd12 C22 C32 50.9(4) . . . . ? C13 Pd13 C23 C73 -49.2(5) . . . . ? N23 Pd13 C23 C73 -169.8(10) . . . . ? N13 Pd13 C23 C73 128.3(5) . . . . ? C13 Pd13 C23 C33 131.2(4) . . . . ? N23 Pd13 C23 C33 10.6(15) . . . . ? N13 Pd13 C23 C33 -51.3(4) . . . . ? C71 C21 C31 C41 -0.7(8) . . . . ? Pd11 C21 C31 C41 176.3(4) . . . . ? C72 C22 C32 C42 -0.5(8) . . . . ? Pd12 C22 C32 C42 178.6(4) . . . . ? C73 C23 C33 C43 0.5(8) . . . . ? Pd13 C23 C33 C43 -179.9(4) . . . . ? C21 C31 C41 C51 -0.6(8) . . . . ? C22 C32 C42 C52 0.7(9) . . . . ? C23 C33 C43 C53 -0.3(9) . . . . ? C31 C41 C51 C61 1.6(8) . . . . ? C31 C41 C51 C81 -178.8(5) . . . . ? C32 C42 C52 C62 -0.1(8) . . . . ? C32 C42 C52 C82 179.9(6) . . . . ? C33 C43 C53 C63 0.2(8) . . . . ? C33 C43 C53 C83 178.9(5) . . . . ? C41 C51 C61 C71 -1.2(8) . . . . ? C81 C51 C61 C71 179.2(5) . . . . ? C42 C52 C62 C72 -0.6(8) . . . . ? C82 C52 C62 C72 179.4(6) . . . . ? C43 C53 C63 C73 -0.3(8) . . . . ? C83 C53 C63 C73 -179.0(5) . . . . ? C51 C61 C71 C21 -0.2(8) . . . . ? C31 C21 C71 C61 1.1(8) . . . . ? Pd11 C21 C71 C61 -175.6(4) . . . . ? C32 C22 C72 C62 -0.2(8) . . . . ? Pd12 C22 C72 C62 -179.2(4) . . . . ? C52 C62 C72 C22 0.7(9) . . . . ? C33 C23 C73 C63 -0.6(8) . . . . ? Pd13 C23 C73 C63 179.9(4) . . . . ? C53 C63 C73 C23 0.5(9) . . . . ? C611 N11 C211 C311 0.9(5) . . . . ? Pd11 N11 C211 C311 176.88(10) . . . . ? C611 N11 C211 C221 -175.9(3) . . . . ? Pd11 N11 C211 C221 0.1(3) . . . . ? C612 N12 C212 C312 -2.0(6) . . . . ? Pd12 N12 C212 C312 179.7(4) . . . . ? C612 N12 C212 C222 176.1(4) . . . . ? Pd12 N12 C212 C222 -2.3(3) . . . . ? C613 N13 C213 C313 -0.7(6) . . . . ? Pd13 N13 C213 C313 174.7(3) . . . . ? C613 N13 C213 C223 -177.8(3) . . . . ? Pd13 N13 C213 C223 -2.4(3) . . . . ? C621 N21 C221 C321 -3.1(6) . . . . ? Pd11 N21 C221 C321 168.4(3) . . . . ? C621 N21 C221 C211 175.1(3) . . . . ? Pd11 N21 C221 C211 -13.4(3) . . . . ? N11 C211 C221 N21 8.9(3) . . . . ? C311 C211 C221 N21 -167.9(2) . . . . ? N11 C211 C221 C321 -172.9(4) . . . . ? C311 C211 C221 C321 10.3(3) . . . . ? C622 N22 C222 C322 0.3(6) . . . . ? Pd12 N22 C222 C322 -173.2(3) . . . . ? C622 N22 C222 C212 -177.8(3) . . . . ? Pd12 N22 C222 C212 8.7(3) . . . . ? N12 C212 C222 N22 -4.3(3) . . . . ? C312 C212 C222 N22 173.7(4) . . . . ? N12 C212 C222 C322 177.6(4) . . . . ? C312 C212 C222 C322 -4.3(4) . . . . ? C623 N23 C223 C323 -2.9(6) . . . . ? Pd13 N23 C223 C323 167.7(3) . . . . ? C623 N23 C223 C213 175.7(4) . . . . ? Pd13 N23 C223 C213 -13.7(3) . . . . ? N13 C213 C223 N23 10.8(3) . . . . ? C313 C213 C223 N23 -166.2(4) . . . . ? N13 C213 C223 C323 -170.6(4) . . . . ? C313 C213 C223 C323 12.4(4) . . . . ? N11 C211 C311 C411 -1.4(4) . . . . ? C221 C211 C311 C411 175.2(3) . . . . ? N12 C212 C312 C412 2.4(8) . . . . ? C222 C212 C312 C412 -175.5(4) . . . . ? N13 C213 C313 C413 -0.7(7) . . . . ? C223 C213 C313 C413 176.2(4) . . . . ? N21 C221 C321 C421 2.4(7) . . . . ? C211 C221 C321 C421 -175.7(4) . . . . ? N22 C222 C322 C422 -0.6(7) . . . . ? C212 C222 C322 C422 177.4(4) . . . . ? N23 C223 C323 C423 2.5(7) . . . . ? C213 C223 C323 C423 -176.1(4) . . . . ? C211 C311 C411 C511 0.4(7) . . . . ? C212 C312 C412 C512 -0.8(9) . . . . ? C213 C313 C413 C513 1.7(9) . . . . ? C221 C321 C421 C521 -0.1(8) . . . . ? C222 C322 C422 C522 0.1(8) . . . . ? C223 C323 C423 C523 0.1(8) . . . . ? C311 C411 C511 C611 1.1(9) . . . . ? C312 C412 C512 C612 -1.2(10) . . . . ? C313 C413 C513 C613 -1.3(9) . . . . ? C321 C421 C521 C621 -1.3(8) . . . . ? C322 C422 C522 C622 0.6(8) . . . . ? C323 C423 C523 C623 -2.2(9) . . . . ? C211 N11 C611 C511 0.6(7) . . . . ? Pd11 N11 C611 C511 -174.8(4) . . . . ? C411 C511 C611 N11 -1.6(9) . . . . ? C212 N12 C612 C512 -0.1(8) . . . . ? Pd12 N12 C612 C512 178.1(4) . . . . ? C412 C512 C612 N12 1.7(9) . . . . ? C213 N13 C613 C513 1.1(8) . . . . ? Pd13 N13 C613 C513 -173.7(4) . . . . ? C413 C513 C613 N13 -0.1(9) . . . . ? C221 N21 C621 C521 1.7(7) . . . . ? Pd11 N21 C621 C521 -168.7(4) . . . . ? C421 C521 C621 N21 0.5(9) . . . . ? C222 N22 C622 C522 0.4(7) . . . . ? Pd12 N22 C622 C522 173.1(4) . . . . ? C422 C522 C622 N22 -0.8(8) . . . . ? C223 N23 C623 C523 0.7(8) . . . . ? Pd13 N23 C623 C523 -168.7(4) . . . . ? C423 C523 C623 N23 1.8(9) . . . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 26.23 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 1.668 _refine_diff_density_min -1.376 _refine_diff_density_rms 0.129 data_c:\Complex_11 _database_code_depnum_ccdc_archive 'CCDC 825047' #TrackingRef 'web_deposit_cif_file_2_Dr.RoderickC.Jones_1305088168.cif' #=============================================================================== # start Validation Reply Form _vrf_THETM01_Compound2 ; PROBLEM: The value of sine(theta_max)/wavelength is less than 0.575 Calculated sin(theta_max)/wavelength = 0.5704 RESPONSE: The resolution limitation is due to the size of the detector at the Australian synchrotron ; _PLAT029_ALERT_3_A ; PROBLEM: diffrn measured fraction theta full Low ....... 0.88 RESPONSE: This is due to the limitations of the instrument available at the Australian Synchrotron operating under rotation data collection with a fixed detector and affects some high angle data ; # end Validation Reply Form #================================== _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C14 H16 N2 O Pd' _chemical_formula_sum 'C14 H16 N2 O Pd' _chemical_formula_weight 334.69 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 triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.6740(7) _cell_length_b 9.1480(7) _cell_length_c 9.4860(6) _cell_angle_alpha 84.0070(10) _cell_angle_beta 80.678(5) _cell_angle_gamma 79.390(4) _cell_volume 643.99(9) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 6461 _cell_measurement_theta_min 2.98 _cell_measurement_theta_max 26.23 _exptl_crystal_description rod _exptl_crystal_colour 'pale orange' _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.726 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 336 _exptl_absorpt_coefficient_mu 1.429 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.77487 _diffrn_radiation_type Synchrotron _diffrn_radiation_source 'synchrotron BM' _diffrn_radiation_monochromator Si<111> _diffrn_measurement_device_type '3-BM1 Australian Synchrotron' _diffrn_measurement_method Rotation _diffrn_detector_area_resol_mean 'ADSC Q210' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6554 _diffrn_reflns_av_R_equivalents 0.0786 _diffrn_reflns_av_sigmaI/netI 0.0690 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.98 _diffrn_reflns_theta_max 26.23 _reflns_number_total 1750 _reflns_number_gt 1694 _reflns_threshold_expression >2sigma(I) _computing_data_collection BLU-ICE _computing_cell_refinement XDS _computing_data_reduction XDS _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; 'X-SEED (Barbour, 2008) and ORTEPIII (Farrugia, 2008)' ; _computing_publication_material 'WinGX (Farrugia, 1999)' _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. The asymmetric unit contains one discrete molecule. All non-hydrogen atom positions were refined anisotropically. All hydrogens were included in calculated positons with a "riding" model. ; _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^)+(0.0497P)^2^+1.0630P] 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 SHELXL _refine_ls_extinction_coef 0.082(8) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 1750 _refine_ls_number_parameters 166 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0390 _refine_ls_R_factor_gt 0.0385 _refine_ls_wR_factor_ref 0.0982 _refine_ls_wR_factor_gt 0.0978 _refine_ls_goodness_of_fit_ref 1.070 _refine_ls_restrained_S_all 1.070 _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 0.25954(3) 0.67434(3) 0.69982(3) 0.0102(3) Uani 1 1 d . . . O1 O -0.1590(4) 0.8996(3) 0.6711(3) 0.0198(7) Uani 1 1 d . . . N1 N 0.1878(5) 0.6380(4) 0.4994(4) 0.0118(8) Uani 1 1 d . . . N2 N 0.3621(5) 0.4455(4) 0.6813(4) 0.0114(8) Uani 1 1 d . . . C1 C 0.3508(7) 0.6859(6) 0.8876(5) 0.0214(11) Uani 1 1 d . . . H1A H 0.3120 0.7868 0.9195 0.032 Uiso 1 1 calc R . . H1B H 0.4820 0.6625 0.8733 0.032 Uiso 1 1 calc R . . H1C H 0.3023 0.6140 0.9605 0.032 Uiso 1 1 calc R . . C2 C 0.1411(7) 0.8976(5) 0.7093(5) 0.0150(10) Uani 1 1 d . . . H2A H 0.1880 0.9461 0.7803 0.018 Uiso 1 1 calc R . . H2B H 0.1593 0.9537 0.6146 0.018 Uiso 1 1 calc R . . C3 C -0.0474(6) 0.8851(4) 0.7544(5) 0.0153(9) Uani 1 1 d . . . C4 C -0.1126(7) 0.8568(6) 0.9132(5) 0.0278(11) Uani 1 1 d . . . H4A H -0.1652 0.9519 0.9541 0.042 Uiso 1 1 calc R . . H4B H -0.0113 0.8084 0.9620 0.042 Uiso 1 1 calc R . . H4C H -0.2032 0.7919 0.9261 0.042 Uiso 1 1 calc R . . C21 C 0.2355(5) 0.4957(5) 0.4628(5) 0.0112(9) Uani 1 1 d . . . C22 C 0.3284(5) 0.3886(5) 0.5661(5) 0.0131(9) Uani 1 1 d . . . C31 C 0.1935(6) 0.4532(5) 0.3375(5) 0.0139(9) Uani 1 1 d . . . H31 H 0.2266 0.3526 0.3136 0.017 Uiso 1 1 calc R . . C32 C 0.3808(6) 0.2365(5) 0.5442(5) 0.0171(10) Uani 1 1 d . . . H32 H 0.3574 0.1981 0.4612 0.021 Uiso 1 1 calc R . . C41 C 0.1023(6) 0.5600(5) 0.2477(5) 0.0169(10) Uani 1 1 d . . . H41 H 0.0715 0.5334 0.1618 0.020 Uiso 1 1 calc R . . C42 C 0.4664(6) 0.1439(5) 0.6449(5) 0.0185(10) Uani 1 1 d . . . H42 H 0.5025 0.0405 0.6321 0.022 Uiso 1 1 calc R . . C51 C 0.0574(6) 0.7052(5) 0.2857(5) 0.0151(9) Uani 1 1 d . . . H51 H -0.0033 0.7803 0.2254 0.018 Uiso 1 1 calc R . . C52 C 0.4998(6) 0.2016(5) 0.7645(5) 0.0194(10) Uani 1 1 d . . . H52 H 0.5587 0.1393 0.8352 0.023 Uiso 1 1 calc R . . C61 C 0.1012(6) 0.7404(5) 0.4116(5) 0.0142(9) Uani 1 1 d . . . H61 H 0.0690 0.8406 0.4372 0.017 Uiso 1 1 calc R . . C62 C 0.4451(6) 0.3525(5) 0.7786(5) 0.0155(9) Uani 1 1 d . . . H62 H 0.4672 0.3926 0.8611 0.019 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 0.0104(3) 0.0106(3) 0.0104(3) -0.00193(16) -0.00464(17) -0.00067(16) O1 0.0210(17) 0.0157(16) 0.0238(18) -0.0040(13) -0.0102(14) 0.0018(13) N1 0.0091(18) 0.0123(19) 0.014(2) -0.0011(15) -0.0016(15) -0.0011(15) N2 0.0087(18) 0.0156(19) 0.011(2) -0.0022(15) -0.0025(15) -0.0044(15) C1 0.024(3) 0.027(3) 0.012(2) -0.003(2) -0.007(2) 0.003(2) C2 0.020(2) 0.012(2) 0.015(2) -0.0037(19) -0.0069(19) -0.005(2) C3 0.023(2) 0.007(2) 0.016(2) -0.0056(17) -0.0054(19) 0.0008(18) C4 0.028(3) 0.032(3) 0.021(3) -0.003(2) -0.005(2) 0.002(2) C21 0.008(2) 0.013(2) 0.014(2) 0.0002(17) -0.0044(17) -0.0030(17) C22 0.005(2) 0.014(2) 0.017(2) 0.0010(18) 0.0040(17) -0.0009(17) C31 0.011(2) 0.021(2) 0.011(2) -0.0025(18) 0.0025(16) -0.0078(18) C32 0.017(2) 0.014(2) 0.021(2) -0.0036(18) -0.0043(19) -0.0020(19) C41 0.018(2) 0.024(2) 0.011(2) -0.0019(18) -0.0049(18) -0.0070(19) C42 0.017(2) 0.010(2) 0.028(3) -0.0045(19) -0.005(2) 0.0010(18) C51 0.013(2) 0.019(2) 0.012(2) 0.0032(18) -0.0016(17) -0.0014(18) C52 0.014(2) 0.020(2) 0.022(3) 0.0035(19) -0.0055(19) 0.0000(19) C61 0.014(2) 0.011(2) 0.018(2) -0.0035(17) -0.0027(18) -0.0017(17) C62 0.010(2) 0.019(2) 0.018(2) -0.0003(18) -0.0067(17) 0.0015(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 2.036(5) . ? Pd1 C2 2.082(5) . ? Pd1 N2 2.111(4) . ? Pd1 N1 2.137(4) . ? O1 C3 1.237(5) . ? N1 C61 1.342(6) . ? N1 C21 1.351(6) . ? N2 C22 1.339(6) . ? N2 C62 1.345(6) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C3 1.462(7) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.520(7) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C21 C31 1.390(6) . ? C21 C22 1.483(6) . ? C22 C32 1.402(6) . ? C31 C41 1.393(6) . ? C31 H31 0.9500 . ? C32 C42 1.376(7) . ? C32 H32 0.9500 . ? C41 C51 1.380(6) . ? C41 H41 0.9500 . ? C42 C52 1.379(7) . ? C42 H42 0.9500 . ? C51 C61 1.375(7) . ? C51 H51 0.9500 . ? C52 C62 1.381(7) . ? C52 H52 0.9500 . ? C61 H61 0.9500 . ? C62 H62 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 C2 88.5(2) . . ? C1 Pd1 N2 95.63(18) . . ? C2 Pd1 N2 175.22(14) . . ? C1 Pd1 N1 172.98(15) . . ? C2 Pd1 N1 98.24(17) . . ? N2 Pd1 N1 77.77(14) . . ? C61 N1 C21 119.2(4) . . ? C61 N1 Pd1 126.5(3) . . ? C21 N1 Pd1 114.3(3) . . ? C22 N2 C62 118.3(4) . . ? C22 N2 Pd1 115.6(3) . . ? C62 N2 Pd1 125.9(3) . . ? Pd1 C1 H1A 109.5 . . ? Pd1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? Pd1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C3 C2 Pd1 101.4(3) . . ? C3 C2 H2A 111.5 . . ? Pd1 C2 H2A 111.5 . . ? C3 C2 H2B 111.5 . . ? Pd1 C2 H2B 111.5 . . ? H2A C2 H2B 109.3 . . ? O1 C3 C2 123.9(4) . . ? O1 C3 C4 117.6(4) . . ? C2 C3 C4 118.5(4) . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N1 C21 C31 121.3(4) . . ? N1 C21 C22 116.0(4) . . ? C31 C21 C22 122.7(4) . . ? N2 C22 C32 121.6(4) . . ? N2 C22 C21 116.2(4) . . ? C32 C22 C21 122.3(4) . . ? C21 C31 C41 119.2(4) . . ? C21 C31 H31 120.4 . . ? C41 C31 H31 120.4 . . ? C42 C32 C22 118.9(4) . . ? C42 C32 H32 120.5 . . ? C22 C32 H32 120.5 . . ? C51 C41 C31 118.7(4) . . ? C51 C41 H41 120.7 . . ? C31 C41 H41 120.7 . . ? C32 C42 C52 119.8(4) . . ? C32 C42 H42 120.1 . . ? C52 C42 H42 120.1 . . ? C61 C51 C41 119.5(4) . . ? C61 C51 H51 120.2 . . ? C41 C51 H51 120.2 . . ? C42 C52 C62 118.1(4) . . ? C42 C52 H52 120.9 . . ? C62 C52 H52 120.9 . . ? N1 C61 C51 122.2(4) . . ? N1 C61 H61 118.9 . . ? C51 C61 H61 118.9 . . ? N2 C62 C52 123.3(4) . . ? N2 C62 H62 118.4 . . ? C52 C62 H62 118.4 . . ? 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 N1 C61 -158.9(13) . . . . ? C2 Pd1 N1 C61 3.4(4) . . . . ? N2 Pd1 N1 C61 -179.3(4) . . . . ? C1 Pd1 N1 C21 21.9(14) . . . . ? C2 Pd1 N1 C21 -175.8(3) . . . . ? N2 Pd1 N1 C21 1.5(3) . . . . ? C1 Pd1 N2 C22 179.4(3) . . . . ? C2 Pd1 N2 C22 30.6(18) . . . . ? N1 Pd1 N2 C22 -3.1(3) . . . . ? C1 Pd1 N2 C62 4.3(4) . . . . ? C2 Pd1 N2 C62 -144.4(17) . . . . ? N1 Pd1 N2 C62 -178.1(4) . . . . ? C1 Pd1 C2 C3 -104.0(3) . . . . ? N2 Pd1 C2 C3 44.8(18) . . . . ? N1 Pd1 C2 C3 78.1(3) . . . . ? Pd1 C2 C3 O1 -97.8(4) . . . . ? Pd1 C2 C3 C4 83.9(4) . . . . ? C61 N1 C21 C31 -1.2(6) . . . . ? Pd1 N1 C21 C31 178.1(3) . . . . ? C61 N1 C21 C22 -179.2(4) . . . . ? Pd1 N1 C21 C22 0.1(5) . . . . ? C62 N2 C22 C32 -1.3(6) . . . . ? Pd1 N2 C22 C32 -176.7(3) . . . . ? C62 N2 C22 C21 179.6(4) . . . . ? Pd1 N2 C22 C21 4.1(5) . . . . ? N1 C21 C22 N2 -2.8(6) . . . . ? C31 C21 C22 N2 179.3(4) . . . . ? N1 C21 C22 C32 178.0(4) . . . . ? C31 C21 C22 C32 0.1(7) . . . . ? N1 C21 C31 C41 0.7(7) . . . . ? C22 C21 C31 C41 178.5(4) . . . . ? N2 C22 C32 C42 0.9(7) . . . . ? C21 C22 C32 C42 -180.0(4) . . . . ? C21 C31 C41 C51 0.4(6) . . . . ? C22 C32 C42 C52 -0.2(7) . . . . ? C31 C41 C51 C61 -0.9(6) . . . . ? C32 C42 C52 C62 -0.1(7) . . . . ? C21 N1 C61 C51 0.6(7) . . . . ? Pd1 N1 C61 C51 -178.5(3) . . . . ? C41 C51 C61 N1 0.4(7) . . . . ? C22 N2 C62 C52 1.0(7) . . . . ? Pd1 N2 C62 C52 175.9(3) . . . . ? C42 C52 C62 N2 -0.4(7) . . . . ? _diffrn_measured_fraction_theta_max 0.878 _diffrn_reflns_theta_full 26.23 _diffrn_measured_fraction_theta_full 0.878 _refine_diff_density_max 0.555 _refine_diff_density_min -0.913 _refine_diff_density_rms 0.148