# Electronic Supplementary Material (ESI) for Chemical Science. # This journal is © The Royal Society of Chemistry 2020 ####################################################################### # # This file contains crystal structure data downloaded from the # Cambridge Structural Database (CSD) hosted by the Cambridge # Crystallographic Data Centre (CCDC). # # Full information about CCDC data access policies and citation # guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 # # Audit and citation data items may have been added by the CCDC. # Please retain this information to preserve the provenance of # this file and to allow appropriate attribution of the data. # ####################################################################### data_shelx _database_code_depnum_ccdc_archive 'CCDC 1965101' loop_ _audit_author_name _audit_author_address 'Prof. Jonathan M. White' ;The University of Melbourne Australia ; _audit_update_record ; 2019-11-12 deposited with the CCDC. 2020-01-22 downloaded from the CCDC. ; _audit_creation_method SHELXL-2016/6 _shelx_SHELXL_version_number 2016/6 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H20 Cl N3 O Pd' _chemical_formula_weight 436.22 _chemical_oxdiff_usercomment 'Tyra Horngren Pd complex' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.5074(4) _cell_length_b 11.2005(6) _cell_length_c 11.2581(5) _cell_angle_alpha 70.420(4) _cell_angle_beta 78.131(4) _cell_angle_gamma 84.462(4) _cell_volume 872.46(8) _cell_formula_units_Z 2 _cell_measurement_temperature 100.0(1) _cell_measurement_reflns_used 7049 _cell_measurement_theta_min 2.7640 _cell_measurement_theta_max 35.3450 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.661 _exptl_crystal_F_000 440 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.306 _exptl_crystal_size_mid 0.198 _exptl_crystal_size_min 0.016 _exptl_absorpt_coefficient_mu 1.226 _shelx_estimated_absorpt_T_min ? _shelx_estimated_absorpt_T_max ? _exptl_absorpt_correction_T_min 0.580 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018) Numerical absorption correction based on gaussian integration over a multifaceted crystal model Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _oxdiff_exptl_absorpt_empirical_full_min 0.725 _oxdiff_exptl_absorpt_empirical_full_max 2.086 _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; _diffrn_ambient_temperature 99.95(15) _diffrn_ambient_environment N~2~ _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'PhotonJet (Mo) X-ray Source' _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_monochromator mirror _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'XtaLAB Synergy, Dualflex, HyPix' _diffrn_detector 'CCD plate' _diffrn_detector_type HyPix _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 19203 _diffrn_reflns_av_unetI/netI 0.0668 _diffrn_reflns_av_R_equivalents 0.0455 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.774 _diffrn_reflns_theta_max 37.213 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.891 _diffrn_measured_fraction_theta_full 0.997 _diffrn_reflns_Laue_measured_fraction_max 0.891 _diffrn_reflns_Laue_measured_fraction_full 0.997 _diffrn_reflns_point_group_measured_fraction_max 0.891 _diffrn_reflns_point_group_measured_fraction_full 0.997 _reflns_number_total 8018 _reflns_number_gt 6236 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)' _computing_cell_refinement 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)' _computing_data_reduction 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)' _computing_structure_solution ? _computing_structure_refinement 'SHELXL-2016/6 (Sheldrick, 2016)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ? _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0503P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 8018 _refine_ls_number_parameters 220 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0686 _refine_ls_R_factor_gt 0.0500 _refine_ls_wR_factor_ref 0.1152 _refine_ls_wR_factor_gt 0.1073 _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_restrained_S_all 1.060 _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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.8244(4) 0.4777(2) 0.4072(3) 0.0250(5) Uani 1 1 d . . . . . H1 H 0.773237 0.398586 0.448714 0.030 Uiso 1 1 calc R U . . . C2 C 0.9285(4) 0.5007(2) 0.2841(3) 0.0286(5) Uani 1 1 d . . . . . H2 H 0.946588 0.437832 0.245540 0.034 Uiso 1 1 calc R U . . . C3 C 1.0031(4) 0.6159(2) 0.2213(3) 0.0263(5) Uani 1 1 d . . . . . H3 H 1.072410 0.632227 0.139262 0.032 Uiso 1 1 calc R U . . . C4 C 0.9752(3) 0.7120(2) 0.2810(2) 0.0233(5) Uani 1 1 d . . . . . C5 C 1.0449(3) 0.8344(2) 0.2251(2) 0.0238(5) Uani 1 1 d . . . . . C6 C 1.0179(4) 0.9199(2) 0.2918(3) 0.0254(5) Uani 1 1 d . . . . . H6 H 1.067504 0.999830 0.253737 0.031 Uiso 1 1 calc R U . . . C7 C 0.9156(4) 0.8867(2) 0.4172(2) 0.0245(5) Uani 1 1 d . . . . . H7 H 0.899755 0.945210 0.461018 0.029 Uiso 1 1 calc R U . . . C8 C 0.8379(3) 0.7693(2) 0.4771(2) 0.0208(4) Uani 1 1 d . . . . . C9 C 0.8705(3) 0.6800(2) 0.4070(2) 0.0204(4) Uani 1 1 d . . . . . C10 C 0.6708(4) 0.7984(2) 0.6768(2) 0.0229(5) Uani 1 1 d . . . . . C11 C 0.5349(4) 0.7302(2) 0.7968(2) 0.0236(5) Uani 1 1 d . . . . . C12 C 0.5253(4) 0.5880(2) 0.8140(3) 0.0286(5) Uani 1 1 d . . . . . H12A H 0.398999 0.563714 0.837259 0.034 Uiso 1 1 calc R U . . . H12B H 0.587245 0.537785 0.882941 0.034 Uiso 1 1 calc R U . . . C13 C 0.3466(4) 0.7980(2) 0.7799(3) 0.0259(5) Uani 1 1 d . . . . . H13A H 0.255679 0.754304 0.852525 0.031 Uiso 1 1 calc R U . . . H13B H 0.351557 0.883816 0.781040 0.031 Uiso 1 1 calc R U . . . C14 C 0.2860(4) 0.8037(3) 0.6571(3) 0.0308(6) Uani 1 1 d . . . . . H14A H 0.359657 0.862036 0.584910 0.046 Uiso 1 1 calc R U . . . H14B H 0.160649 0.831684 0.660970 0.046 Uiso 1 1 calc R U . . . H14C H 0.299610 0.720965 0.647863 0.046 Uiso 1 1 calc R U . . . C15 C 0.5890(4) 0.7497(3) 0.9140(2) 0.0275(5) Uani 1 1 d . . . . . H15A H 0.578929 0.839525 0.903598 0.033 Uiso 1 1 calc R U . . . H15B H 0.502716 0.706872 0.990191 0.033 Uiso 1 1 calc R U . . . C16 C 0.7816(4) 0.7014(3) 0.9358(3) 0.0381(7) Uani 1 1 d . . . . . H16A H 0.793101 0.612323 0.947311 0.057 Uiso 1 1 calc R U . . . H16B H 0.803428 0.715776 1.010911 0.057 Uiso 1 1 calc R U . . . H16C H 0.868907 0.745957 0.862672 0.057 Uiso 1 1 calc R U . . . C17 C 0.5181(4) 0.2706(2) 0.7304(3) 0.0246(5) Uani 1 1 d . . . . . C18 C 0.4708(4) 0.1388(2) 0.7605(3) 0.0330(6) Uani 1 1 d . . . . . H18A H 0.361794 0.136433 0.729365 0.049 Uiso 1 1 calc R U . . . H18B H 0.451116 0.097927 0.851671 0.049 Uiso 1 1 calc R U . . . H18C H 0.568536 0.095567 0.720062 0.049 Uiso 1 1 calc R U . . . N1 N 0.7947(3) 0.56301(19) 0.4681(2) 0.0229(4) Uani 1 1 d . . . . . N2 N 0.7277(3) 0.72605(18) 0.5977(2) 0.0217(4) Uani 1 1 d . . . . . N3 N 0.5549(3) 0.37356(19) 0.7070(2) 0.0239(4) Uani 1 1 d . . . . . O1 O 0.7166(3) 0.90774(17) 0.65443(18) 0.0291(4) Uani 1 1 d . . . . . Pd1 Pd 0.64184(3) 0.55255(2) 0.65109(2) 0.02072(6) Uani 1 1 d . . . . . Cl1 Cl 1.16943(10) 0.87882(6) 0.06879(6) 0.03078(14) 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 C1 0.0265(12) 0.0208(11) 0.0345(13) -0.0149(9) -0.0130(10) 0.0047(9) C2 0.0330(14) 0.0281(12) 0.0335(13) -0.0206(10) -0.0125(11) 0.0091(10) C3 0.0252(12) 0.0319(13) 0.0293(12) -0.0191(10) -0.0107(10) 0.0093(10) C4 0.0203(11) 0.0254(11) 0.0296(12) -0.0141(9) -0.0113(9) 0.0066(8) C5 0.0189(11) 0.0299(12) 0.0251(11) -0.0120(9) -0.0057(9) 0.0024(9) C6 0.0246(12) 0.0253(11) 0.0292(12) -0.0117(9) -0.0071(10) 0.0005(9) C7 0.0264(12) 0.0222(11) 0.0283(11) -0.0122(9) -0.0068(10) 0.0018(9) C8 0.0226(11) 0.0187(10) 0.0259(11) -0.0126(8) -0.0086(9) 0.0046(8) C9 0.0202(11) 0.0208(10) 0.0251(10) -0.0120(8) -0.0100(9) 0.0056(8) C10 0.0250(12) 0.0222(11) 0.0257(11) -0.0125(9) -0.0076(9) 0.0034(8) C11 0.0267(12) 0.0213(11) 0.0255(11) -0.0114(9) -0.0057(9) 0.0023(8) C12 0.0338(14) 0.0232(11) 0.0274(12) -0.0085(9) -0.0042(11) 0.0037(10) C13 0.0266(13) 0.0234(11) 0.0291(12) -0.0112(9) -0.0045(10) 0.0008(9) C14 0.0311(14) 0.0300(13) 0.0357(14) -0.0137(11) -0.0116(12) 0.0017(10) C15 0.0300(14) 0.0312(13) 0.0240(11) -0.0121(10) -0.0061(10) 0.0008(10) C16 0.0354(16) 0.0468(18) 0.0361(15) -0.0157(13) -0.0138(13) 0.0036(13) C17 0.0235(12) 0.0212(11) 0.0314(12) -0.0102(9) -0.0104(10) 0.0052(8) C18 0.0307(14) 0.0202(11) 0.0517(17) -0.0128(11) -0.0154(13) 0.0030(9) N1 0.0240(10) 0.0193(9) 0.0305(10) -0.0127(8) -0.0110(8) 0.0050(7) N2 0.0247(10) 0.0172(9) 0.0247(9) -0.0095(7) -0.0043(8) 0.0019(7) N3 0.0239(10) 0.0204(9) 0.0304(10) -0.0109(8) -0.0097(9) 0.0054(7) O1 0.0384(11) 0.0222(8) 0.0313(9) -0.0163(7) -0.0021(8) -0.0038(7) Pd1 0.02246(9) 0.01617(8) 0.02652(10) -0.00997(6) -0.00771(7) 0.00331(6) Cl1 0.0294(3) 0.0360(3) 0.0261(3) -0.0113(2) -0.0036(2) 0.0044(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 C1 N1 1.330(3) . ? C1 C2 1.398(4) . ? C1 H1 0.9300 . ? C2 C3 1.357(4) . ? C2 H2 0.9300 . ? C3 C4 1.428(3) . ? C3 H3 0.9300 . ? C4 C5 1.404(4) . ? C4 C9 1.419(4) . ? C5 C6 1.381(3) . ? C5 Cl1 1.745(3) . ? C6 C7 1.406(4) . ? C6 H6 0.9300 . ? C7 C8 1.384(3) . ? C7 H7 0.9300 . ? C8 N2 1.391(3) . ? C8 C9 1.445(3) . ? C9 N1 1.376(3) . ? C10 O1 1.233(3) . ? C10 N2 1.377(3) . ? C10 C11 1.530(4) . ? C11 C15 1.545(3) . ? C11 C12 1.546(3) . ? C11 C13 1.555(4) . ? C12 Pd1 2.012(3) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 C14 1.522(4) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 C16 1.532(4) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 N3 1.141(3) . ? C17 C18 1.462(3) . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? N1 Pd1 2.113(2) . ? N2 Pd1 1.963(2) . ? N3 Pd1 2.020(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 123.4(2) . . ? N1 C1 H1 118.3 . . ? C2 C1 H1 118.3 . . ? C3 C2 C1 119.3(2) . . ? C3 C2 H2 120.4 . . ? C1 C2 H2 120.4 . . ? C2 C3 C4 120.1(3) . . ? C2 C3 H3 119.9 . . ? C4 C3 H3 119.9 . . ? C5 C4 C9 118.0(2) . . ? C5 C4 C3 125.0(2) . . ? C9 C4 C3 117.0(2) . . ? C6 C5 C4 121.3(2) . . ? C6 C5 Cl1 119.3(2) . . ? C4 C5 Cl1 119.42(19) . . ? C5 C6 C7 120.2(2) . . ? C5 C6 H6 119.9 . . ? C7 C6 H6 119.9 . . ? C8 C7 C6 121.8(2) . . ? C8 C7 H7 119.1 . . ? C6 C7 H7 119.1 . . ? C7 C8 N2 127.9(2) . . ? C7 C8 C9 117.2(2) . . ? N2 C8 C9 114.9(2) . . ? N1 C9 C4 121.8(2) . . ? N1 C9 C8 116.8(2) . . ? C4 C9 C8 121.4(2) . . ? O1 C10 N2 125.3(2) . . ? O1 C10 C11 122.2(2) . . ? N2 C10 C11 112.5(2) . . ? C10 C11 C15 108.4(2) . . ? C10 C11 C12 111.9(2) . . ? C15 C11 C12 111.6(2) . . ? C10 C11 C13 106.48(19) . . ? C15 C11 C13 107.9(2) . . ? C12 C11 C13 110.3(2) . . ? C11 C12 Pd1 110.67(18) . . ? C11 C12 H12A 109.5 . . ? Pd1 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? Pd1 C12 H12B 109.5 . . ? H12A C12 H12B 108.1 . . ? C14 C13 C11 114.4(2) . . ? C14 C13 H13A 108.7 . . ? C11 C13 H13A 108.7 . . ? C14 C13 H13B 108.7 . . ? C11 C13 H13B 108.7 . . ? H13A C13 H13B 107.6 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C16 C15 C11 114.8(2) . . ? C16 C15 H15A 108.6 . . ? C11 C15 H15A 108.6 . . ? C16 C15 H15B 108.6 . . ? C11 C15 H15B 108.6 . . ? H15A C15 H15B 107.5 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N3 C17 C18 179.9(4) . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C1 N1 C9 118.4(2) . . ? C1 N1 Pd1 130.61(19) . . ? C9 N1 Pd1 110.98(15) . . ? C10 N2 C8 124.3(2) . . ? C10 N2 Pd1 119.30(17) . . ? C8 N2 Pd1 116.36(15) . . ? C17 N3 Pd1 173.9(2) . . ? N2 Pd1 C12 83.74(10) . . ? N2 Pd1 N3 179.56(8) . . ? C12 Pd1 N3 96.12(10) . . ? N2 Pd1 N1 81.00(8) . . ? C12 Pd1 N1 164.65(10) . . ? N3 Pd1 N1 99.13(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 N1 C1 C2 C3 -0.6(4) . . . . ? C1 C2 C3 C4 0.1(4) . . . . ? C2 C3 C4 C5 -179.7(2) . . . . ? C2 C3 C4 C9 1.0(3) . . . . ? C9 C4 C5 C6 2.1(3) . . . . ? C3 C4 C5 C6 -177.2(2) . . . . ? C9 C4 C5 Cl1 -178.37(17) . . . . ? C3 C4 C5 Cl1 2.4(3) . . . . ? C4 C5 C6 C7 -1.4(4) . . . . ? Cl1 C5 C6 C7 179.02(19) . . . . ? C5 C6 C7 C8 -0.6(4) . . . . ? C6 C7 C8 N2 -177.0(2) . . . . ? C6 C7 C8 C9 1.8(4) . . . . ? C5 C4 C9 N1 179.0(2) . . . . ? C3 C4 C9 N1 -1.7(3) . . . . ? C5 C4 C9 C8 -0.8(3) . . . . ? C3 C4 C9 C8 178.5(2) . . . . ? C7 C8 C9 N1 179.1(2) . . . . ? N2 C8 C9 N1 -1.9(3) . . . . ? C7 C8 C9 C4 -1.1(3) . . . . ? N2 C8 C9 C4 177.9(2) . . . . ? O1 C10 C11 C15 -46.9(3) . . . . ? N2 C10 C11 C15 135.4(2) . . . . ? O1 C10 C11 C12 -170.4(2) . . . . ? N2 C10 C11 C12 11.9(3) . . . . ? O1 C10 C11 C13 69.0(3) . . . . ? N2 C10 C11 C13 -108.7(2) . . . . ? C10 C11 C12 Pd1 -15.1(3) . . . . ? C15 C11 C12 Pd1 -136.78(19) . . . . ? C13 C11 C12 Pd1 103.3(2) . . . . ? C10 C11 C13 C14 55.5(3) . . . . ? C15 C11 C13 C14 171.8(2) . . . . ? C12 C11 C13 C14 -66.1(3) . . . . ? C10 C11 C15 C16 -58.6(3) . . . . ? C12 C11 C15 C16 65.1(3) . . . . ? C13 C11 C15 C16 -173.5(2) . . . . ? C2 C1 N1 C9 -0.1(4) . . . . ? C2 C1 N1 Pd1 179.16(18) . . . . ? C4 C9 N1 C1 1.3(3) . . . . ? C8 C9 N1 C1 -178.9(2) . . . . ? C4 C9 N1 Pd1 -178.10(17) . . . . ? C8 C9 N1 Pd1 1.7(2) . . . . ? O1 C10 N2 C8 -3.7(4) . . . . ? C11 C10 N2 C8 173.9(2) . . . . ? O1 C10 N2 Pd1 179.3(2) . . . . ? C11 C10 N2 Pd1 -3.1(3) . . . . ? C7 C8 N2 C10 2.9(4) . . . . ? C9 C8 N2 C10 -175.9(2) . . . . ? C7 C8 N2 Pd1 180.0(2) . . . . ? C9 C8 N2 Pd1 1.2(3) . . . . ? _refine_diff_density_max 1.720 _refine_diff_density_min -2.367 _refine_diff_density_rms 0.145 _shelx_res_file ; TITL shelxt_a.res in P-1 shelx.res created by SHELXL-2016/6 at 11:20:25 on 17-Nov-2018 CELL 0.71073 7.5074 11.2005 11.2581 70.420 78.131 84.462 ZERR 2.00 0.0004 0.0006 0.0005 0.004 0.004 0.004 LATT 1 SFAC C H N O PD CL UNIT 36 40 6 2 2 2 MERG 2 FMAP 2 PLAN 20 ACTA BOND $H CONF L.S. 10 WGHT 0.050300 FVAR 1.79229 C1 1 0.824408 0.477668 0.407222 11.00000 0.02646 0.02081 = 0.03454 -0.01489 -0.01299 0.00466 AFIX 43 H1 2 0.773237 0.398586 0.448714 11.00000 -1.20000 AFIX 0 C2 1 0.928550 0.500726 0.284065 11.00000 0.03298 0.02811 = 0.03352 -0.02055 -0.01250 0.00911 AFIX 43 H2 2 0.946588 0.437832 0.245540 11.00000 -1.20000 AFIX 0 C3 1 1.003070 0.615899 0.221303 11.00000 0.02524 0.03191 = 0.02928 -0.01907 -0.01074 0.00933 AFIX 43 H3 2 1.072410 0.632227 0.139262 11.00000 -1.20000 AFIX 0 C4 1 0.975210 0.712033 0.280992 11.00000 0.02028 0.02539 = 0.02959 -0.01411 -0.01126 0.00664 C5 1 1.044923 0.834359 0.225116 11.00000 0.01891 0.02991 = 0.02505 -0.01204 -0.00570 0.00243 C6 1 1.017889 0.919932 0.291836 11.00000 0.02461 0.02528 = 0.02925 -0.01165 -0.00710 0.00055 AFIX 43 H6 2 1.067504 0.999830 0.253737 11.00000 -1.20000 AFIX 0 C7 1 0.915615 0.886700 0.417172 11.00000 0.02642 0.02220 = 0.02831 -0.01218 -0.00682 0.00177 AFIX 43 H7 2 0.899755 0.945210 0.461018 11.00000 -1.20000 AFIX 0 C8 1 0.837855 0.769297 0.477139 11.00000 0.02261 0.01871 = 0.02589 -0.01257 -0.00863 0.00462 C9 1 0.870519 0.679999 0.406983 11.00000 0.02022 0.02080 = 0.02512 -0.01204 -0.00999 0.00556 C10 1 0.670797 0.798421 0.676843 11.00000 0.02502 0.02222 = 0.02568 -0.01248 -0.00757 0.00342 C11 1 0.534883 0.730250 0.796803 11.00000 0.02671 0.02129 = 0.02555 -0.01142 -0.00572 0.00227 C12 1 0.525258 0.587993 0.813990 11.00000 0.03379 0.02323 = 0.02742 -0.00847 -0.00421 0.00372 AFIX 23 H12A 2 0.398999 0.563714 0.837259 11.00000 -1.20000 H12B 2 0.587245 0.537785 0.882941 11.00000 -1.20000 AFIX 0 C13 1 0.346602 0.798001 0.779881 11.00000 0.02664 0.02342 = 0.02913 -0.01120 -0.00451 0.00078 AFIX 23 H13A 2 0.255679 0.754304 0.852525 11.00000 -1.20000 H13B 2 0.351557 0.883816 0.781040 11.00000 -1.20000 AFIX 0 C14 1 0.286039 0.803697 0.657070 11.00000 0.03112 0.03001 = 0.03566 -0.01371 -0.01165 0.00171 AFIX 137 H14A 2 0.359657 0.862036 0.584910 11.00000 -1.50000 H14B 2 0.160649 0.831684 0.660970 11.00000 -1.50000 H14C 2 0.299610 0.720965 0.647863 11.00000 -1.50000 AFIX 0 C15 1 0.589034 0.749723 0.914047 11.00000 0.03001 0.03120 = 0.02395 -0.01210 -0.00606 0.00085 AFIX 23 H15A 2 0.578929 0.839525 0.903598 11.00000 -1.20000 H15B 2 0.502716 0.706872 0.990191 11.00000 -1.20000 AFIX 0 C16 1 0.781598 0.701436 0.935763 11.00000 0.03541 0.04676 = 0.03606 -0.01571 -0.01382 0.00363 AFIX 137 H16A 2 0.793101 0.612323 0.947311 11.00000 -1.50000 H16B 2 0.803428 0.715776 1.010911 11.00000 -1.50000 H16C 2 0.868907 0.745957 0.862672 11.00000 -1.50000 AFIX 0 C17 1 0.518061 0.270649 0.730407 11.00000 0.02351 0.02123 = 0.03140 -0.01018 -0.01036 0.00521 C18 1 0.470822 0.138831 0.760455 11.00000 0.03071 0.02017 = 0.05174 -0.01275 -0.01544 0.00296 AFIX 137 H18A 2 0.361794 0.136433 0.729365 11.00000 -1.50000 H18B 2 0.451116 0.097927 0.851671 11.00000 -1.50000 H18C 2 0.568536 0.095567 0.720062 11.00000 -1.50000 AFIX 0 N1 3 0.794728 0.563011 0.468124 11.00000 0.02399 0.01927 = 0.03050 -0.01266 -0.01101 0.00503 N2 3 0.727677 0.726054 0.597657 11.00000 0.02475 0.01721 = 0.02469 -0.00948 -0.00434 0.00191 N3 3 0.554876 0.373563 0.707035 11.00000 0.02395 0.02040 = 0.03042 -0.01094 -0.00971 0.00542 O1 4 0.716561 0.907744 0.654428 11.00000 0.03842 0.02218 = 0.03129 -0.01634 -0.00214 -0.00380 PD1 5 0.641844 0.552547 0.651094 11.00000 0.02246 0.01617 = 0.02652 -0.00997 -0.00771 0.00331 CL1 6 1.169432 0.878817 0.068788 11.00000 0.02936 0.03604 = 0.02608 -0.01134 -0.00356 0.00444 HKLF 4 REM shelxt_a.res in P-1 REM R1 = 0.0500 for 6236 Fo > 4sig(Fo) and 0.0686 for all 8018 data REM 220 parameters refined using 0 restraints END WGHT 0.0503 0.0000 REM Highest difference peak 1.720, deepest hole -2.367, 1-sigma level 0.145 Q1 1 0.6828 0.5570 0.7000 11.00000 0.05 1.72 Q2 1 0.7041 0.5769 0.6029 11.00000 0.05 1.68 Q3 1 0.5823 0.5671 0.5869 11.00000 0.05 1.14 Q4 1 0.7079 0.4887 0.6412 11.00000 0.05 1.10 Q5 1 0.5978 0.6024 0.6715 11.00000 0.05 1.09 Q6 1 1.0079 0.8844 0.2504 11.00000 0.05 0.76 Q7 1 0.9846 0.6726 0.2523 11.00000 0.05 0.75 Q8 1 0.5669 0.4700 0.7038 11.00000 0.05 0.75 Q9 1 0.5957 0.5399 0.7778 11.00000 0.05 0.73 Q10 1 0.6998 0.6464 0.6212 11.00000 0.05 0.71 Q11 1 0.8597 0.7197 0.4552 11.00000 0.05 0.70 Q12 1 0.3634 0.5480 0.8716 11.00000 0.05 0.68 Q13 1 0.7197 0.5481 0.5389 11.00000 0.05 0.67 Q14 1 1.1311 0.9203 0.0078 11.00000 0.05 0.66 Q15 1 1.0872 0.8519 0.2680 11.00000 0.05 0.65 Q16 1 0.7804 0.5311 0.4264 11.00000 0.05 0.64 Q17 1 0.7919 0.7483 0.5580 11.00000 0.05 0.63 Q18 1 1.1208 0.9405 0.0823 11.00000 0.05 0.58 Q19 1 0.9057 0.6467 0.9620 11.00000 0.05 0.58 Q20 1 0.6538 0.4141 0.6870 11.00000 0.05 0.56 ; _shelx_res_checksum 63556 _exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: chloroform, hexane' _exptl_crystal_preparation Luminescent