# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'LeGrande Slaughter' _publ_contact_author_email LMS@CHEM.OKSTATE.EDU _publ_section_title ; Direct observation of a carbonylation reaction relevant to CO/alkene copolymerization in a methylpalladium carbonyl complex containing a bis(N-heterocyclic carbene) ligand ; loop_ _publ_author_name 'LeGrande Slaughter' 'Sri S Subramanium' # Attachment 'Slaughter_Cmplx5.cif' data_cmplx5_lms173 _database_code_depnum_ccdc_archive 'CCDC 729935' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common '(Pd(DIMESMe)(CH3)(NCCH3))+ BF4-' _chemical_melting_point ? _chemical_formula_moiety 'C28 H34 N5 Pd, C2 H3 N, B F4' _chemical_formula_sum 'C30 H37 B F4 N6 Pd' _chemical_formula_weight 674.87 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' B B 0.0013 0.0007 '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' F F 0.0171 0.0103 '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 'P 21/n' _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 11.5389(1) _cell_length_b 19.0724(2) _cell_length_c 15.1677(2) _cell_angle_alpha 90.00 _cell_angle_beta 108.068(1) _cell_angle_gamma 90.00 _cell_volume 3173.42(6) _cell_formula_units_Z 4 _cell_measurement_temperature 115(2) _cell_measurement_reflns_used 9740 _cell_measurement_theta_min 2.56 _cell_measurement_theta_max 30.83 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.43 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.413 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1384 _exptl_absorpt_coefficient_mu 0.638 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7711 _exptl_absorpt_correction_T_max 0.8831 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 115(2) _diffrn_radiation_probe ? _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX II CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 0.75 _diffrn_standards_number 0 _diffrn_standards_interval_count N/A _diffrn_standards_interval_time N/A _diffrn_standards_decay_% N/A _diffrn_reflns_number 54834 _diffrn_reflns_av_R_equivalents 0.0325 _diffrn_reflns_av_sigmaI/netI 0.0240 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.77 _diffrn_reflns_theta_max 30.86 _reflns_number_total 9914 _reflns_number_gt 8388 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL (XS)' _computing_structure_refinement 'Bruker SHELXTL (XL)' _computing_molecular_graphics 'Bruker SHELXTL (XP)' _computing_publication_material 'Bruker SHELXTL (XCIF)' _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^)+(0.0347P)^2^+1.5356P] 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 9914 _refine_ls_number_parameters 388 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0364 _refine_ls_R_factor_gt 0.0278 _refine_ls_wR_factor_ref 0.0726 _refine_ls_wR_factor_gt 0.0682 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.216805(10) 0.048920(5) 0.554978(7) 0.01591(4) Uani 1 1 d . . . C1 C 0.13816(13) 0.12313(7) 0.60627(10) 0.0170(3) Uani 1 1 d . . . C2 C 0.17460(13) -0.02026(8) 0.64814(10) 0.0186(3) Uani 1 1 d . . . N1 N 0.16805(12) 0.19106(6) 0.62931(9) 0.0194(2) Uani 1 1 d . . . C3 C 0.09290(15) 0.21956(8) 0.67615(12) 0.0258(3) Uani 1 1 d . . . H3 H 0.0962 0.2661 0.6991 0.031 Uiso 1 1 calc R . . C4 C 0.01494(15) 0.16917(8) 0.68285(12) 0.0247(3) Uani 1 1 d . . . H4 H -0.0471 0.1728 0.7117 0.030 Uiso 1 1 calc R . . N2 N 0.04336(11) 0.11083(6) 0.63912(9) 0.0188(2) Uani 1 1 d . . . N3 N 0.22326(12) -0.07952(7) 0.69428(10) 0.0216(3) Uani 1 1 d . . . C5 C 0.14967(16) -0.10693(9) 0.74319(13) 0.0287(3) Uani 1 1 d . . . H5 H 0.1649 -0.1480 0.7804 0.034 Uiso 1 1 calc R . . C6 C 0.05301(15) -0.06416(9) 0.72771(13) 0.0271(3) Uani 1 1 d . . . H6 H -0.0138 -0.0691 0.7513 0.032 Uiso 1 1 calc R . . N4 N 0.07053(12) -0.01152(7) 0.67042(9) 0.0204(2) Uani 1 1 d . . . C7 C -0.01703(13) 0.04334(7) 0.62948(11) 0.0197(3) Uani 1 1 d . . . H7A H -0.0569 0.0331 0.5630 0.024 Uiso 1 1 calc R . . H7B H -0.0808 0.0446 0.6606 0.024 Uiso 1 1 calc R . . C8 C 0.22860(16) 0.11665(8) 0.45202(11) 0.0251(3) Uani 1 1 d . . . H8A H 0.1518 0.1425 0.4279 0.038 Uiso 1 1 calc R . . H8B H 0.2441 0.0898 0.4017 0.038 Uiso 1 1 calc R . . H8C H 0.2955 0.1498 0.4776 0.038 Uiso 1 1 calc R . . N5 N 0.31169(12) -0.02196(7) 0.50219(10) 0.0239(3) Uani 1 1 d . . . C9 C 0.36821(16) -0.05584(9) 0.46955(13) 0.0294(3) Uani 1 1 d . . . C10 C 0.4415(2) -0.09938(12) 0.42849(18) 0.0486(6) Uani 1 1 d . . . H10A H 0.5242 -0.1036 0.4719 0.073 Uiso 1 1 calc R . . H10B H 0.4450 -0.0778 0.3707 0.073 Uiso 1 1 calc R . . H10C H 0.4046 -0.1460 0.4152 0.073 Uiso 1 1 calc R . . C11 C 0.26856(14) 0.22942(7) 0.61539(11) 0.0194(3) Uani 1 1 d . . . C12 C 0.24378(15) 0.28163(8) 0.54753(11) 0.0243(3) Uani 1 1 d . . . C13 C 0.34269(17) 0.31824(8) 0.53604(12) 0.0281(3) Uani 1 1 d . . . H13 H 0.3283 0.3536 0.4897 0.034 Uiso 1 1 calc R . . C14 C 0.46154(16) 0.30456(9) 0.59032(13) 0.0280(3) Uani 1 1 d . . . C15 C 0.48162(15) 0.25294(9) 0.65810(12) 0.0250(3) Uani 1 1 d . . . H15 H 0.5627 0.2437 0.6960 0.030 Uiso 1 1 calc R . . C16 C 0.38649(14) 0.21432(8) 0.67207(11) 0.0204(3) Uani 1 1 d . . . C17 C 0.11613(18) 0.29798(10) 0.48759(15) 0.0368(4) Uani 1 1 d . . . H17A H 0.1182 0.3361 0.4448 0.055 Uiso 1 1 calc R . . H17B H 0.0670 0.3123 0.5268 0.055 Uiso 1 1 calc R . . H17C H 0.0800 0.2562 0.4520 0.055 Uiso 1 1 calc R . . C18 C 0.5662(2) 0.34534(11) 0.57553(16) 0.0417(5) Uani 1 1 d . . . H18A H 0.5893 0.3835 0.6209 0.062 Uiso 1 1 calc R . . H18B H 0.5412 0.3650 0.5127 0.062 Uiso 1 1 calc R . . H18C H 0.6360 0.3140 0.5833 0.062 Uiso 1 1 calc R . . C19 C 0.41094(16) 0.15843(9) 0.74505(12) 0.0284(3) Uani 1 1 d . . . H19A H 0.4988 0.1557 0.7771 0.043 Uiso 1 1 calc R . . H19B H 0.3818 0.1132 0.7159 0.043 Uiso 1 1 calc R . . H19C H 0.3682 0.1699 0.7898 0.043 Uiso 1 1 calc R . . C21 C 0.33485(14) -0.11227(8) 0.69250(11) 0.0215(3) Uani 1 1 d . . . C22 C 0.32853(16) -0.16629(8) 0.62900(12) 0.0279(3) Uani 1 1 d . . . C23 C 0.43654(18) -0.19962(9) 0.63142(13) 0.0316(4) Uani 1 1 d . . . H23 H 0.4341 -0.2368 0.5892 0.038 Uiso 1 1 calc R . . C24 C 0.54776(17) -0.18032(9) 0.69361(13) 0.0303(4) Uani 1 1 d . . . C25 C 0.55039(15) -0.12547(9) 0.75419(13) 0.0283(3) Uani 1 1 d . . . H25 H 0.6265 -0.1110 0.7958 0.034 Uiso 1 1 calc R . . C26 C 0.44434(15) -0.09085(8) 0.75594(12) 0.0236(3) Uani 1 1 d . . . C27 C 0.2091(2) -0.18856(11) 0.56082(16) 0.0439(5) Uani 1 1 d . . . H27A H 0.1592 -0.2118 0.5940 0.066 Uiso 1 1 calc R . . H27B H 0.2245 -0.2212 0.5157 0.066 Uiso 1 1 calc R . . H27C H 0.1659 -0.1472 0.5283 0.066 Uiso 1 1 calc R . . C28 C 0.66382(19) -0.21901(12) 0.69827(16) 0.0427(5) Uani 1 1 d . . . H28A H 0.6900 -0.2470 0.7552 0.064 Uiso 1 1 calc R . . H28B H 0.7277 -0.1851 0.6983 0.064 Uiso 1 1 calc R . . H28C H 0.6491 -0.2500 0.6443 0.064 Uiso 1 1 calc R . . C29 C 0.45042(18) -0.03382(9) 0.82590(14) 0.0332(4) Uani 1 1 d . . . H29A H 0.3846 -0.0001 0.8002 0.050 Uiso 1 1 calc R . . H29B H 0.5292 -0.0098 0.8405 0.050 Uiso 1 1 calc R . . H29C H 0.4414 -0.0545 0.8826 0.050 Uiso 1 1 calc R . . B1 B 0.8009(2) 0.05833(13) 0.80043(17) 0.0357(5) Uani 1 1 d . . . F1 F 0.90956(16) 0.06884(17) 0.86677(15) 0.1186(9) Uani 1 1 d . . . F2 F 0.79122(15) 0.10626(8) 0.72940(13) 0.0656(4) Uani 1 1 d . . . F3 F 0.70589(13) 0.06817(9) 0.83603(11) 0.0596(4) Uani 1 1 d . . . F4 F 0.79687(17) -0.00674(8) 0.76264(14) 0.0743(5) Uani 1 1 d . . . N100 N 0.8132(4) 0.37254(16) 0.4522(3) 0.1154(14) Uani 1 1 d . . . C100 C 0.7603(3) 0.42146(13) 0.4534(2) 0.0557(7) Uani 1 1 d . . . C101 C 0.6952(3) 0.48511(13) 0.4586(2) 0.0572(6) Uani 1 1 d . . . H11A H 0.7073 0.4968 0.5237 0.086 Uiso 1 1 calc R . . H11B H 0.6081 0.4783 0.4265 0.086 Uiso 1 1 calc R . . H11C H 0.7261 0.5234 0.4290 0.086 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 0.01662(6) 0.01424(5) 0.01761(6) -0.00157(4) 0.00638(4) -0.00014(4) C1 0.0168(6) 0.0163(6) 0.0171(6) -0.0009(5) 0.0040(5) -0.0005(5) C2 0.0173(6) 0.0166(6) 0.0220(7) -0.0007(5) 0.0063(5) -0.0001(5) N1 0.0192(6) 0.0161(5) 0.0237(6) -0.0024(5) 0.0078(5) 0.0003(4) C3 0.0249(7) 0.0207(7) 0.0346(9) -0.0083(6) 0.0133(7) 0.0005(6) C4 0.0228(7) 0.0221(7) 0.0326(8) -0.0072(6) 0.0136(7) 0.0010(6) N2 0.0172(6) 0.0168(5) 0.0234(6) -0.0021(5) 0.0074(5) 0.0003(4) N3 0.0194(6) 0.0184(6) 0.0277(7) 0.0043(5) 0.0085(5) 0.0005(5) C5 0.0270(8) 0.0250(8) 0.0370(9) 0.0110(7) 0.0140(7) -0.0004(6) C6 0.0228(7) 0.0263(8) 0.0345(9) 0.0073(6) 0.0124(7) -0.0017(6) N4 0.0183(6) 0.0191(6) 0.0246(6) 0.0024(5) 0.0077(5) -0.0007(5) C7 0.0155(6) 0.0173(6) 0.0265(7) -0.0014(5) 0.0067(6) -0.0008(5) C8 0.0335(8) 0.0227(7) 0.0220(7) 0.0011(6) 0.0130(7) -0.0001(6) N5 0.0228(6) 0.0213(6) 0.0294(7) -0.0027(5) 0.0106(6) 0.0004(5) C9 0.0250(8) 0.0282(8) 0.0366(9) -0.0073(7) 0.0120(7) -0.0010(6) C10 0.0375(11) 0.0488(12) 0.0668(15) -0.0228(11) 0.0268(11) 0.0049(9) C11 0.0208(7) 0.0153(6) 0.0228(7) -0.0043(5) 0.0079(6) -0.0020(5) C12 0.0280(8) 0.0188(7) 0.0243(7) -0.0014(6) 0.0057(6) -0.0010(6) C13 0.0404(9) 0.0190(7) 0.0280(8) -0.0012(6) 0.0152(7) -0.0049(6) C14 0.0320(8) 0.0242(8) 0.0335(9) -0.0081(6) 0.0185(7) -0.0079(6) C15 0.0210(7) 0.0256(7) 0.0293(8) -0.0075(6) 0.0094(6) -0.0019(6) C16 0.0226(7) 0.0186(6) 0.0208(7) -0.0044(5) 0.0077(6) 0.0000(5) C17 0.0337(9) 0.0278(9) 0.0406(10) 0.0080(7) -0.0006(8) 0.0023(7) C18 0.0423(11) 0.0404(11) 0.0512(12) -0.0058(9) 0.0275(10) -0.0155(9) C19 0.0271(8) 0.0285(8) 0.0262(8) 0.0024(6) 0.0032(7) -0.0001(6) C21 0.0201(7) 0.0181(6) 0.0264(7) 0.0057(5) 0.0074(6) 0.0022(5) C22 0.0326(9) 0.0204(7) 0.0277(8) 0.0021(6) 0.0050(7) 0.0042(6) C23 0.0435(10) 0.0249(8) 0.0284(8) 0.0038(6) 0.0140(8) 0.0114(7) C24 0.0309(8) 0.0308(8) 0.0351(9) 0.0149(7) 0.0187(7) 0.0108(7) C25 0.0207(7) 0.0296(8) 0.0352(9) 0.0092(7) 0.0093(7) 0.0014(6) C26 0.0237(7) 0.0198(7) 0.0272(8) 0.0048(6) 0.0078(6) 0.0004(6) C27 0.0430(11) 0.0288(9) 0.0465(12) -0.0084(8) -0.0059(9) 0.0027(8) C28 0.0402(11) 0.0443(11) 0.0544(13) 0.0200(10) 0.0303(10) 0.0192(9) C29 0.0318(9) 0.0276(8) 0.0352(9) -0.0032(7) 0.0034(8) -0.0003(7) B1 0.0278(10) 0.0463(12) 0.0380(11) -0.0093(9) 0.0174(9) -0.0036(9) F1 0.0379(9) 0.236(3) 0.0695(13) -0.0450(16) -0.0007(9) -0.0096(13) F2 0.0628(9) 0.0530(8) 0.0984(12) 0.0193(8) 0.0503(9) 0.0005(7) F3 0.0466(8) 0.0815(10) 0.0658(9) -0.0055(8) 0.0396(7) 0.0023(7) F4 0.0914(12) 0.0385(7) 0.1190(15) -0.0152(8) 0.0707(12) -0.0068(8) N100 0.137(3) 0.0534(16) 0.201(4) -0.013(2) 0.119(3) 0.0034(18) C100 0.0704(17) 0.0401(12) 0.0736(17) -0.0060(11) 0.0471(15) -0.0110(11) C101 0.0607(16) 0.0453(13) 0.0710(17) 0.0159(12) 0.0284(14) 0.0092(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 C1 1.9672(14) . ? Pd1 N5 2.0521(13) . ? Pd1 C8 2.0635(15) . ? Pd1 C2 2.0980(15) . ? C1 N2 1.3558(18) . ? C1 N1 1.3582(18) . ? C2 N4 1.3549(18) . ? C2 N3 1.3559(19) . ? N1 C3 1.3908(19) . ? N1 C11 1.4411(19) . ? C3 C4 1.342(2) . ? C3 H3 0.9500 . ? C4 N2 1.3858(19) . ? C4 H4 0.9500 . ? N2 C7 1.4494(18) . ? N3 C5 1.391(2) . ? N3 C21 1.4390(19) . ? C5 C6 1.342(2) . ? C5 H5 0.9500 . ? C6 N4 1.383(2) . ? C6 H6 0.9500 . ? N4 C7 1.4533(19) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? N5 C9 1.135(2) . ? C9 C10 1.456(2) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C16 1.396(2) . ? C11 C12 1.396(2) . ? C12 C13 1.394(2) . ? C12 C17 1.504(2) . ? C13 C14 1.388(3) . ? C13 H13 0.9500 . ? C14 C15 1.390(2) . ? C14 C18 1.511(2) . ? C15 C16 1.392(2) . ? C15 H15 0.9500 . ? C16 C19 1.499(2) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C21 C26 1.391(2) . ? C21 C22 1.397(2) . ? C22 C23 1.389(2) . ? C22 C27 1.505(3) . ? C23 C24 1.386(3) . ? C23 H23 0.9500 . ? C24 C25 1.386(3) . ? C24 C28 1.511(2) . ? C25 C26 1.398(2) . ? C25 H25 0.9500 . ? C26 C29 1.506(2) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? B1 F1 1.357(3) . ? B1 F4 1.362(3) . ? B1 F3 1.377(2) . ? B1 F2 1.391(3) . ? N100 C100 1.118(4) . ? C100 C101 1.442(4) . ? C101 H11A 0.9800 . ? C101 H11B 0.9800 . ? C101 H11C 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 N5 174.65(6) . . ? C1 Pd1 C8 89.75(6) . . ? N5 Pd1 C8 87.06(6) . . ? C1 Pd1 C2 87.38(6) . . ? N5 Pd1 C2 96.43(6) . . ? C8 Pd1 C2 170.76(6) . . ? N2 C1 N1 103.89(12) . . ? N2 C1 Pd1 122.99(10) . . ? N1 C1 Pd1 132.58(11) . . ? N4 C2 N3 103.36(12) . . ? N4 C2 Pd1 119.96(10) . . ? N3 C2 Pd1 136.58(11) . . ? C1 N1 C3 110.82(13) . . ? C1 N1 C11 126.74(12) . . ? C3 N1 C11 122.28(12) . . ? C4 C3 N1 107.32(13) . . ? C4 C3 H3 126.3 . . ? N1 C3 H3 126.3 . . ? C3 C4 N2 105.98(13) . . ? C3 C4 H4 127.0 . . ? N2 C4 H4 127.0 . . ? C1 N2 C4 111.99(12) . . ? C1 N2 C7 122.29(12) . . ? C4 N2 C7 125.71(13) . . ? C2 N3 C5 111.41(13) . . ? C2 N3 C21 125.58(12) . . ? C5 N3 C21 122.99(13) . . ? C6 C5 N3 106.84(14) . . ? C6 C5 H5 126.6 . . ? N3 C5 H5 126.6 . . ? C5 C6 N4 106.00(14) . . ? C5 C6 H6 127.0 . . ? N4 C6 H6 127.0 . . ? C2 N4 C6 112.39(13) . . ? C2 N4 C7 122.31(13) . . ? C6 N4 C7 124.98(13) . . ? N2 C7 N4 110.34(12) . . ? N2 C7 H7A 109.6 . . ? N4 C7 H7A 109.6 . . ? N2 C7 H7B 109.6 . . ? N4 C7 H7B 109.6 . . ? H7A C7 H7B 108.1 . . ? Pd1 C8 H8A 109.5 . . ? Pd1 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? Pd1 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C9 N5 Pd1 173.48(14) . . ? N5 C9 C10 179.5(2) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C16 C11 C12 122.60(14) . . ? C16 C11 N1 118.70(13) . . ? C12 C11 N1 118.67(14) . . ? C13 C12 C11 117.44(15) . . ? C13 C12 C17 120.44(16) . . ? C11 C12 C17 122.12(15) . . ? C14 C13 C12 121.88(16) . . ? C14 C13 H13 119.1 . . ? C12 C13 H13 119.1 . . ? C13 C14 C15 118.64(15) . . ? C13 C14 C18 120.23(17) . . ? C15 C14 C18 121.13(18) . . ? C14 C15 C16 121.95(16) . . ? C14 C15 H15 119.0 . . ? C16 C15 H15 119.0 . . ? C15 C16 C11 117.47(14) . . ? C15 C16 C19 120.81(15) . . ? C11 C16 C19 121.72(14) . . ? C12 C17 H17A 109.5 . . ? C12 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C12 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C14 C18 H18A 109.5 . . ? C14 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C14 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C16 C19 H19A 109.5 . . ? C16 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C16 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C26 C21 C22 122.39(15) . . ? C26 C21 N3 119.05(14) . . ? C22 C21 N3 118.52(14) . . ? C23 C22 C21 117.69(16) . . ? C23 C22 C27 120.78(17) . . ? C21 C22 C27 121.53(16) . . ? C24 C23 C22 122.01(17) . . ? C24 C23 H23 119.0 . . ? C22 C23 H23 119.0 . . ? C23 C24 C25 118.47(16) . . ? C23 C24 C28 121.47(18) . . ? C25 C24 C28 120.03(19) . . ? C24 C25 C26 121.98(17) . . ? C24 C25 H25 119.0 . . ? C26 C25 H25 119.0 . . ? C21 C26 C25 117.43(15) . . ? C21 C26 C29 122.24(15) . . ? C25 C26 C29 120.32(16) . . ? C22 C27 H27A 109.5 . . ? C22 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C22 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C24 C28 H28A 109.5 . . ? C24 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C24 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C26 C29 H29A 109.5 . . ? C26 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C26 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? F1 B1 F4 110.5(2) . . ? F1 B1 F3 110.72(19) . . ? F4 B1 F3 111.21(18) . . ? F1 B1 F2 108.1(2) . . ? F4 B1 F2 106.80(19) . . ? F3 B1 F2 109.37(19) . . ? N100 C100 C101 177.7(4) . . ? C100 C101 H11A 109.5 . . ? C100 C101 H11B 109.5 . . ? H11A C101 H11B 109.5 . . ? C100 C101 H11C 109.5 . . ? H11A C101 H11C 109.5 . . ? H11B C101 H11C 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 C8 Pd1 C1 N2 139.63(13) . . . . ? C2 Pd1 C1 N2 -31.58(12) . . . . ? C8 Pd1 C1 N1 -50.28(15) . . . . ? C2 Pd1 C1 N1 138.51(15) . . . . ? C1 Pd1 C2 N4 33.99(12) . . . . ? N5 Pd1 C2 N4 -149.78(12) . . . . ? C1 Pd1 C2 N3 -150.36(17) . . . . ? N5 Pd1 C2 N3 25.87(17) . . . . ? N2 C1 N1 C3 0.40(17) . . . . ? Pd1 C1 N1 C3 -171.04(12) . . . . ? N2 C1 N1 C11 175.87(14) . . . . ? Pd1 C1 N1 C11 4.4(2) . . . . ? C1 N1 C3 C4 0.06(19) . . . . ? C11 N1 C3 C4 -175.64(14) . . . . ? N1 C3 C4 N2 -0.50(19) . . . . ? N1 C1 N2 C4 -0.73(17) . . . . ? Pd1 C1 N2 C4 171.76(11) . . . . ? N1 C1 N2 C7 -179.73(13) . . . . ? Pd1 C1 N2 C7 -7.23(19) . . . . ? C3 C4 N2 C1 0.79(19) . . . . ? C3 C4 N2 C7 179.74(15) . . . . ? N4 C2 N3 C5 0.58(18) . . . . ? Pd1 C2 N3 C5 -175.54(13) . . . . ? N4 C2 N3 C21 179.07(14) . . . . ? Pd1 C2 N3 C21 2.9(3) . . . . ? C2 N3 C5 C6 -0.1(2) . . . . ? C21 N3 C5 C6 -178.61(16) . . . . ? N3 C5 C6 N4 -0.5(2) . . . . ? N3 C2 N4 C6 -0.89(18) . . . . ? Pd1 C2 N4 C6 176.04(11) . . . . ? N3 C2 N4 C7 -174.77(13) . . . . ? Pd1 C2 N4 C7 2.16(19) . . . . ? C5 C6 N4 C2 0.9(2) . . . . ? C5 C6 N4 C7 174.56(15) . . . . ? C1 N2 C7 N4 56.52(19) . . . . ? C4 N2 C7 N4 -122.32(16) . . . . ? C2 N4 C7 N2 -52.09(19) . . . . ? C6 N4 C7 N2 134.82(16) . . . . ? C1 N1 C11 C16 -73.1(2) . . . . ? C3 N1 C11 C16 101.89(17) . . . . ? C1 N1 C11 C12 108.74(17) . . . . ? C3 N1 C11 C12 -76.3(2) . . . . ? C16 C11 C12 C13 1.5(2) . . . . ? N1 C11 C12 C13 179.55(14) . . . . ? C16 C11 C12 C17 -179.29(16) . . . . ? N1 C11 C12 C17 -1.2(2) . . . . ? C11 C12 C13 C14 -0.9(2) . . . . ? C17 C12 C13 C14 179.86(17) . . . . ? C12 C13 C14 C15 -0.2(2) . . . . ? C12 C13 C14 C18 179.90(16) . . . . ? C13 C14 C15 C16 0.8(2) . . . . ? C18 C14 C15 C16 -179.31(16) . . . . ? C14 C15 C16 C11 -0.3(2) . . . . ? C14 C15 C16 C19 179.36(15) . . . . ? C12 C11 C16 C15 -0.9(2) . . . . ? N1 C11 C16 C15 -178.99(13) . . . . ? C12 C11 C16 C19 179.48(15) . . . . ? N1 C11 C16 C19 1.4(2) . . . . ? C2 N3 C21 C26 87.7(2) . . . . ? C5 N3 C21 C26 -93.97(19) . . . . ? C2 N3 C21 C22 -94.52(19) . . . . ? C5 N3 C21 C22 83.8(2) . . . . ? C26 C21 C22 C23 0.8(2) . . . . ? N3 C21 C22 C23 -176.86(14) . . . . ? C26 C21 C22 C27 -179.89(17) . . . . ? N3 C21 C22 C27 2.4(2) . . . . ? C21 C22 C23 C24 -0.6(3) . . . . ? C27 C22 C23 C24 -179.84(18) . . . . ? C22 C23 C24 C25 -0.8(3) . . . . ? C22 C23 C24 C28 177.37(16) . . . . ? C23 C24 C25 C26 1.9(2) . . . . ? C28 C24 C25 C26 -176.28(16) . . . . ? C22 C21 C26 C25 0.2(2) . . . . ? N3 C21 C26 C25 177.90(14) . . . . ? C22 C21 C26 C29 -178.42(16) . . . . ? N3 C21 C26 C29 -0.7(2) . . . . ? C24 C25 C26 C21 -1.6(2) . . . . ? C24 C25 C26 C29 177.06(16) . . . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 30.86 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.603 _refine_diff_density_min -0.568 _refine_diff_density_rms 0.070 _exptl_crystal_recrystallization_method 'slow diff of diethyl ether into acetonitrile soln' # Attachment 'Slaughter_Cmplx6_form21.cif' data_cmplx6_form2_lms194 _database_code_depnum_ccdc_archive 'CCDC 730056' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common (Pd(DIMesMe)(CH3)(CO))(BF4) _chemical_melting_point ? _chemical_formula_moiety 'C27 H31 N4 O Pd, B F4' _chemical_formula_sum 'C27 H31 B F4 N4 O Pd' _chemical_formula_weight 620.77 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' B B 0.0013 0.0007 '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' 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' _symmetry_int_tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.7458(3) _cell_length_b 12.1565(4) _cell_length_c 12.6369(4) _cell_angle_alpha 68.230(2) _cell_angle_beta 73.986(2) _cell_angle_gamma 67.495(2) _cell_volume 1398.94(8) _cell_formula_units_Z 2 _cell_measurement_temperature 115(2) _cell_measurement_reflns_used 6231 _cell_measurement_theta_min 2.17 _cell_measurement_theta_max 23.5 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.474 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 632 _exptl_absorpt_coefficient_mu 0.717 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9126 _exptl_absorpt_correction_T_max 0.9788 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; All crystals obtained were small and relatively weakly diffracting. As a result, data at the higher end of the usual 2Theta range of 0 - 50 were not observed or too weak to use. ; _diffrn_ambient_temperature 115(2) _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX II CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 0.75 _diffrn_standards_number 0 _diffrn_standards_interval_count N/A _diffrn_standards_interval_time N/A _diffrn_standards_decay_% N/A _diffrn_reflns_number 15017 _diffrn_reflns_av_R_equivalents 0.0468 _diffrn_reflns_av_sigmaI/netI 0.0585 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.76 _diffrn_reflns_theta_max 23.54 _reflns_number_total 4140 _reflns_number_gt 3346 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL (XS)' _computing_structure_refinement 'Bruker SHELXTL (XL)' _computing_molecular_graphics 'Bruker SHELXTL (XP)' _computing_publication_material 'Bruker SHELXTL (XCIF)' _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^)+(0.0700P)^2^+0.6478P] 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 4140 _refine_ls_number_parameters 350 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0637 _refine_ls_R_factor_gt 0.0467 _refine_ls_wR_factor_ref 0.1209 _refine_ls_wR_factor_gt 0.1121 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.038 _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 0.89095(4) 0.72784(4) 0.84028(3) 0.02762(17) Uani 1 1 d . . . C1 C 1.0925(5) 0.6583(4) 0.7812(4) 0.0271(12) Uani 1 1 d . . . C2 C 0.8622(5) 0.7671(5) 0.6723(4) 0.0268(12) Uani 1 1 d . . . N1 N 1.2055(4) 0.6685(4) 0.7992(3) 0.0272(10) Uani 1 1 d . . . N2 N 1.1381(4) 0.6016(4) 0.6976(3) 0.0291(10) Uani 1 1 d . . . N3 N 0.7735(4) 0.8578(4) 0.6035(3) 0.0293(10) Uani 1 1 d . . . N4 N 0.9409(4) 0.6913(4) 0.6072(3) 0.0287(10) Uani 1 1 d . . . C3 C 1.3178(5) 0.6194(5) 0.7259(4) 0.0324(13) Uani 1 1 d . . . H3 H 1.4089 0.6160 0.7215 0.039 Uiso 1 1 calc R . . C4 C 1.2759(5) 0.5780(5) 0.6627(4) 0.0330(13) Uani 1 1 d . . . H4 H 1.3305 0.5397 0.6048 0.040 Uiso 1 1 calc R . . C5 C 0.7971(5) 0.8378(5) 0.4976(4) 0.0338(13) Uani 1 1 d . . . H5 H 0.7482 0.8886 0.4350 0.041 Uiso 1 1 calc R . . C6 C 0.9020(6) 0.7330(5) 0.5009(4) 0.0360(13) Uani 1 1 d . . . H6 H 0.9421 0.6947 0.4410 0.043 Uiso 1 1 calc R . . C7 C 1.0461(5) 0.5757(5) 0.6512(4) 0.0307(12) Uani 1 1 d . . . H7A H 1.0976 0.5381 0.5883 0.037 Uiso 1 1 calc R . . H7B H 1.0037 0.5157 0.7124 0.037 Uiso 1 1 calc R . . C8 C 0.9316(5) 0.6698(5) 1.0094(5) 0.0416(14) Uani 1 1 d . . . H8A H 0.9437 0.7384 1.0243 0.062 Uiso 1 1 calc R . . H8B H 1.0150 0.5982 1.0185 0.062 Uiso 1 1 calc R . . H8C H 0.8551 0.6458 1.0642 0.062 Uiso 1 1 calc R . . C9 C 0.7048(6) 0.7948(6) 0.9051(5) 0.0393(14) Uani 1 1 d . . . O1 O 0.5996(5) 0.8298(5) 0.9512(4) 0.0700(14) Uani 1 1 d . . . C11 C 1.2111(5) 0.7264(5) 0.8784(4) 0.0285(12) Uani 1 1 d . . . C12 C 1.2736(5) 0.6504(5) 0.9744(4) 0.0310(12) Uani 1 1 d . . . C13 C 1.2837(5) 0.7089(6) 1.0463(5) 0.0374(14) Uani 1 1 d . . . H13 H 1.3273 0.6593 1.1122 0.045 Uiso 1 1 calc R . . C14 C 1.2322(5) 0.8374(6) 1.0249(5) 0.0380(14) Uani 1 1 d . . . C15 C 1.1660(5) 0.9083(5) 0.9313(4) 0.0323(13) Uani 1 1 d . . . H15 H 1.1260 0.9957 0.9185 0.039 Uiso 1 1 calc R . . C16 C 1.1560(5) 0.8549(5) 0.8541(4) 0.0302(13) Uani 1 1 d . . . C17 C 1.3265(6) 0.5108(5) 1.0011(5) 0.0413(14) Uani 1 1 d . . . H17A H 1.2542 0.4804 1.0012 0.062 Uiso 1 1 calc R . . H17B H 1.3556 0.4733 1.0772 0.062 Uiso 1 1 calc R . . H17C H 1.4043 0.4877 0.9425 0.062 Uiso 1 1 calc R . . C18 C 1.2493(6) 0.8974(6) 1.1042(5) 0.0548(17) Uani 1 1 d . . . H18A H 1.3457 0.8898 1.0946 0.082 Uiso 1 1 calc R . . H18B H 1.2185 0.8552 1.1844 0.082 Uiso 1 1 calc R . . H18C H 1.1949 0.9858 1.0845 0.082 Uiso 1 1 calc R . . C19 C 1.0906(6) 0.9354(5) 0.7485(5) 0.0401(14) Uani 1 1 d . . . H19A H 1.1535 0.9171 0.6800 0.060 Uiso 1 1 calc R . . H19B H 1.0692 1.0235 0.7417 0.060 Uiso 1 1 calc R . . H19C H 1.0064 0.9182 0.7549 0.060 Uiso 1 1 calc R . . C21 C 0.6631(5) 0.9582(5) 0.6361(4) 0.0275(12) Uani 1 1 d . . . C22 C 0.5365(5) 0.9396(5) 0.6820(4) 0.0349(13) Uani 1 1 d . . . C23 C 0.4306(5) 1.0327(5) 0.7173(4) 0.0366(14) Uani 1 1 d . . . H23 H 0.3448 1.0198 0.7514 0.044 Uiso 1 1 calc R . . C24 C 0.4466(5) 1.1459(5) 0.7043(4) 0.0338(13) Uani 1 1 d . . . C25 C 0.5719(5) 1.1630(5) 0.6551(4) 0.0313(13) Uani 1 1 d . . . H25 H 0.5831 1.2404 0.6447 0.038 Uiso 1 1 calc R . . C26 C 0.6829(5) 1.0697(5) 0.6203(4) 0.0264(12) Uani 1 1 d . . . C27 C 0.5162(6) 0.8185(6) 0.6953(6) 0.0537(17) Uani 1 1 d . . . H27A H 0.5194 0.8131 0.6191 0.081 Uiso 1 1 calc R . . H27B H 0.4275 0.8157 0.7422 0.081 Uiso 1 1 calc R . . H27C H 0.5887 0.7482 0.7334 0.081 Uiso 1 1 calc R . . C28 C 0.3282(6) 1.2477(6) 0.7424(5) 0.0516(17) Uani 1 1 d . . . H28A H 0.2836 1.3068 0.6760 0.077 Uiso 1 1 calc R . . H28B H 0.3615 1.2915 0.7743 0.077 Uiso 1 1 calc R . . H28C H 0.2625 1.2107 0.8015 0.077 Uiso 1 1 calc R . . C29 C 0.8177(5) 1.0938(5) 0.5668(4) 0.0353(13) Uani 1 1 d . . . H29A H 0.8911 1.0140 0.5734 0.053 Uiso 1 1 calc R . . H29B H 0.8336 1.1411 0.6070 0.053 Uiso 1 1 calc R . . H29C H 0.8158 1.1417 0.4852 0.053 Uiso 1 1 calc R . . B1 B 0.2781(7) 0.5197(6) 0.3726(6) 0.0352(16) Uani 1 1 d . . . F1 F 0.1429(4) 0.5335(5) 0.3795(5) 0.1121(18) Uani 1 1 d . . . F2 F 0.2778(6) 0.6323(4) 0.3580(5) 0.122(2) Uani 1 1 d . . . F3 F 0.3132(5) 0.4383(4) 0.4749(3) 0.0959(15) Uani 1 1 d . . . F4 F 0.3485(4) 0.4732(4) 0.2846(3) 0.0878(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 Pd1 0.0304(3) 0.0259(3) 0.0290(3) -0.00868(18) -0.00525(17) -0.01050(19) C1 0.036(3) 0.015(3) 0.032(3) -0.006(2) -0.008(2) -0.007(2) C2 0.032(3) 0.020(3) 0.032(3) -0.004(2) -0.008(2) -0.014(2) N1 0.030(2) 0.023(3) 0.032(2) -0.012(2) -0.0057(19) -0.008(2) N2 0.036(3) 0.019(3) 0.033(2) -0.011(2) -0.0087(19) -0.005(2) N3 0.033(2) 0.021(3) 0.035(3) -0.007(2) -0.009(2) -0.009(2) N4 0.038(3) 0.024(3) 0.029(2) -0.012(2) -0.007(2) -0.010(2) C3 0.037(3) 0.022(3) 0.039(3) -0.010(3) -0.007(3) -0.007(3) C4 0.034(3) 0.023(3) 0.038(3) -0.015(3) -0.003(2) -0.001(3) C5 0.044(3) 0.038(4) 0.029(3) -0.008(3) -0.015(2) -0.019(3) C6 0.049(4) 0.039(4) 0.031(3) -0.015(3) -0.009(3) -0.017(3) C7 0.042(3) 0.020(3) 0.035(3) -0.012(2) -0.010(2) -0.007(3) C8 0.032(3) 0.042(4) 0.049(4) -0.015(3) -0.002(3) -0.011(3) C9 0.034(3) 0.045(4) 0.036(3) -0.012(3) -0.004(3) -0.011(3) O1 0.054(3) 0.081(4) 0.063(3) -0.021(3) -0.006(3) -0.012(3) C11 0.026(3) 0.029(3) 0.033(3) -0.013(3) -0.001(2) -0.010(2) C12 0.030(3) 0.029(3) 0.035(3) -0.010(3) -0.005(2) -0.010(2) C13 0.035(3) 0.047(4) 0.036(3) -0.016(3) -0.011(2) -0.012(3) C14 0.039(3) 0.045(4) 0.040(3) -0.023(3) -0.002(3) -0.017(3) C15 0.032(3) 0.030(3) 0.039(3) -0.017(3) 0.004(2) -0.014(3) C16 0.029(3) 0.032(4) 0.031(3) -0.012(3) 0.001(2) -0.012(3) C17 0.041(3) 0.031(4) 0.057(4) -0.013(3) -0.020(3) -0.009(3) C18 0.057(4) 0.064(5) 0.064(4) -0.040(4) -0.015(3) -0.016(4) C19 0.051(4) 0.030(4) 0.038(3) -0.008(3) -0.005(3) -0.015(3) C21 0.032(3) 0.027(3) 0.025(3) -0.005(2) -0.011(2) -0.008(3) C22 0.034(3) 0.029(3) 0.041(3) -0.003(3) -0.014(3) -0.011(3) C23 0.031(3) 0.034(4) 0.038(3) -0.001(3) -0.009(2) -0.009(3) C24 0.031(3) 0.034(4) 0.027(3) -0.004(2) -0.008(2) -0.004(3) C25 0.043(3) 0.023(3) 0.029(3) -0.006(2) -0.010(2) -0.011(3) C26 0.030(3) 0.027(3) 0.022(3) -0.004(2) -0.008(2) -0.008(3) C27 0.044(4) 0.042(4) 0.079(5) -0.016(3) -0.005(3) -0.023(3) C28 0.045(4) 0.046(4) 0.053(4) -0.016(3) 0.002(3) -0.007(3) C29 0.043(3) 0.038(4) 0.034(3) -0.010(3) -0.003(2) -0.024(3) B1 0.043(4) 0.028(4) 0.042(4) -0.016(3) -0.009(3) -0.014(3) F1 0.066(3) 0.144(5) 0.159(5) -0.087(4) 0.005(3) -0.042(3) F2 0.208(6) 0.076(4) 0.124(4) -0.024(3) -0.028(4) -0.093(4) F3 0.163(5) 0.057(3) 0.057(3) -0.022(2) -0.045(3) 0.002(3) F4 0.089(3) 0.081(3) 0.049(2) -0.027(2) -0.011(2) 0.029(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 Pd1 C9 1.918(6) . ? Pd1 C1 2.034(5) . ? Pd1 C2 2.081(5) . ? Pd1 C8 2.101(5) . ? C1 N2 1.351(6) . ? C1 N1 1.352(6) . ? C2 N4 1.349(6) . ? C2 N3 1.350(6) . ? N1 C3 1.383(6) . ? N1 C11 1.445(6) . ? N2 C4 1.370(6) . ? N2 C7 1.455(6) . ? N3 C5 1.386(6) . ? N3 C21 1.436(6) . ? N4 C6 1.371(6) . ? N4 C7 1.454(6) . ? C3 C4 1.329(7) . ? C3 H3 0.9500 . ? C4 H4 0.9500 . ? C5 C6 1.335(7) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 O1 1.118(6) . ? C11 C12 1.386(7) . ? C11 C16 1.387(7) . ? C12 C13 1.391(7) . ? C12 C17 1.503(7) . ? C13 C14 1.388(8) . ? C13 H13 0.9500 . ? C14 C15 1.374(7) . ? C14 C18 1.522(7) . ? C15 C16 1.401(7) . ? C15 H15 0.9500 . ? C16 C19 1.501(7) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C21 C26 1.386(7) . ? C21 C22 1.393(7) . ? C22 C23 1.373(7) . ? C22 C27 1.510(7) . ? C23 C24 1.396(7) . ? C23 H23 0.9500 . ? C24 C25 1.378(7) . ? C24 C28 1.510(8) . ? C25 C26 1.396(7) . ? C25 H25 0.9500 . ? C26 C29 1.509(6) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? B1 F2 1.311(7) . ? B1 F4 1.342(7) . ? B1 F3 1.352(7) . ? B1 F1 1.379(7) . ? 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 C9 Pd1 C1 175.8(2) . . ? C9 Pd1 C2 98.5(2) . . ? C1 Pd1 C2 85.42(19) . . ? C9 Pd1 C8 85.3(2) . . ? C1 Pd1 C8 90.9(2) . . ? C2 Pd1 C8 174.2(2) . . ? N2 C1 N1 104.5(4) . . ? N2 C1 Pd1 122.9(3) . . ? N1 C1 Pd1 132.1(4) . . ? N4 C2 N3 104.0(4) . . ? N4 C2 Pd1 121.4(4) . . ? N3 C2 Pd1 134.6(4) . . ? C1 N1 C3 109.8(4) . . ? C1 N1 C11 126.5(4) . . ? C3 N1 C11 123.7(4) . . ? C1 N2 C4 111.5(4) . . ? C1 N2 C7 121.8(4) . . ? C4 N2 C7 126.7(4) . . ? C2 N3 C5 111.0(4) . . ? C2 N3 C21 125.4(4) . . ? C5 N3 C21 123.5(4) . . ? C2 N4 C6 111.7(4) . . ? C2 N4 C7 122.4(4) . . ? C6 N4 C7 125.8(4) . . ? C4 C3 N1 107.9(5) . . ? C4 C3 H3 126.0 . . ? N1 C3 H3 126.0 . . ? C3 C4 N2 106.3(5) . . ? C3 C4 H4 126.9 . . ? N2 C4 H4 126.9 . . ? C6 C5 N3 106.6(5) . . ? C6 C5 H5 126.7 . . ? N3 C5 H5 126.7 . . ? C5 C6 N4 106.8(5) . . ? C5 C6 H6 126.6 . . ? N4 C6 H6 126.6 . . ? N4 C7 N2 109.3(4) . . ? N4 C7 H7A 109.8 . . ? N2 C7 H7A 109.8 . . ? N4 C7 H7B 109.8 . . ? N2 C7 H7B 109.8 . . ? H7A C7 H7B 108.3 . . ? Pd1 C8 H8A 109.5 . . ? Pd1 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? Pd1 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? O1 C9 Pd1 174.5(5) . . ? C12 C11 C16 123.1(5) . . ? C12 C11 N1 118.1(5) . . ? C16 C11 N1 118.8(4) . . ? C11 C12 C13 117.0(5) . . ? C11 C12 C17 121.7(5) . . ? C13 C12 C17 121.3(5) . . ? C14 C13 C12 122.1(5) . . ? C14 C13 H13 118.9 . . ? C12 C13 H13 118.9 . . ? C15 C14 C13 118.6(5) . . ? C15 C14 C18 121.2(6) . . ? C13 C14 C18 120.2(5) . . ? C14 C15 C16 121.7(5) . . ? C14 C15 H15 119.1 . . ? C16 C15 H15 119.1 . . ? C11 C16 C15 117.3(5) . . ? C11 C16 C19 122.1(5) . . ? C15 C16 C19 120.6(5) . . ? C12 C17 H17A 109.5 . . ? C12 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C12 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C14 C18 H18A 109.5 . . ? C14 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C14 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C16 C19 H19A 109.5 . . ? C16 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C16 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C26 C21 C22 121.9(5) . . ? C26 C21 N3 120.5(4) . . ? C22 C21 N3 117.6(5) . . ? C23 C22 C21 118.6(5) . . ? C23 C22 C27 120.4(5) . . ? C21 C22 C27 121.0(5) . . ? C22 C23 C24 121.3(5) . . ? C22 C23 H23 119.4 . . ? C24 C23 H23 119.4 . . ? C25 C24 C23 118.7(5) . . ? C25 C24 C28 121.0(5) . . ? C23 C24 C28 120.4(5) . . ? C24 C25 C26 121.8(5) . . ? C24 C25 H25 119.1 . . ? C26 C25 H25 119.1 . . ? C21 C26 C25 117.7(4) . . ? C21 C26 C29 122.8(5) . . ? C25 C26 C29 119.5(5) . . ? C22 C27 H27A 109.5 . . ? C22 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C22 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C24 C28 H28A 109.5 . . ? C24 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C24 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C26 C29 H29A 109.5 . . ? C26 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C26 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? F2 B1 F4 114.8(6) . . ? F2 B1 F3 112.9(6) . . ? F4 B1 F3 111.7(5) . . ? F2 B1 F1 104.0(6) . . ? F4 B1 F1 107.4(5) . . ? F3 B1 F1 105.2(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 C2 Pd1 C1 N2 -33.1(4) . . . . ? C8 Pd1 C1 N2 142.4(4) . . . . ? C2 Pd1 C1 N1 137.3(5) . . . . ? C8 Pd1 C1 N1 -47.1(5) . . . . ? C9 Pd1 C2 N4 -146.9(4) . . . . ? C1 Pd1 C2 N4 34.7(4) . . . . ? C9 Pd1 C2 N3 31.4(5) . . . . ? C1 Pd1 C2 N3 -147.0(5) . . . . ? N2 C1 N1 C3 0.7(5) . . . . ? Pd1 C1 N1 C3 -171.1(4) . . . . ? N2 C1 N1 C11 178.0(4) . . . . ? Pd1 C1 N1 C11 6.2(7) . . . . ? N1 C1 N2 C4 -0.7(5) . . . . ? Pd1 C1 N2 C4 172.0(3) . . . . ? N1 C1 N2 C7 -178.6(4) . . . . ? Pd1 C1 N2 C7 -5.9(6) . . . . ? N4 C2 N3 C5 0.2(5) . . . . ? Pd1 C2 N3 C5 -178.3(3) . . . . ? N4 C2 N3 C21 176.5(4) . . . . ? Pd1 C2 N3 C21 -2.0(7) . . . . ? N3 C2 N4 C6 -0.3(5) . . . . ? Pd1 C2 N4 C6 178.4(3) . . . . ? N3 C2 N4 C7 -176.1(4) . . . . ? Pd1 C2 N4 C7 2.6(6) . . . . ? C1 N1 C3 C4 -0.4(6) . . . . ? C11 N1 C3 C4 -177.8(4) . . . . ? N1 C3 C4 N2 -0.1(6) . . . . ? C1 N2 C4 C3 0.5(6) . . . . ? C7 N2 C4 C3 178.3(5) . . . . ? C2 N3 C5 C6 0.0(6) . . . . ? C21 N3 C5 C6 -176.3(4) . . . . ? N3 C5 C6 N4 -0.2(5) . . . . ? C2 N4 C6 C5 0.4(6) . . . . ? C7 N4 C6 C5 176.0(4) . . . . ? C2 N4 C7 N2 -54.2(6) . . . . ? C6 N4 C7 N2 130.7(5) . . . . ? C1 N2 C7 N4 56.5(6) . . . . ? C4 N2 C7 N4 -121.1(5) . . . . ? C1 N1 C11 C12 111.2(5) . . . . ? C3 N1 C11 C12 -71.8(6) . . . . ? C1 N1 C11 C16 -69.8(6) . . . . ? C3 N1 C11 C16 107.2(5) . . . . ? C16 C11 C12 C13 -2.1(7) . . . . ? N1 C11 C12 C13 176.9(4) . . . . ? C16 C11 C12 C17 177.1(4) . . . . ? N1 C11 C12 C17 -4.0(7) . . . . ? C11 C12 C13 C14 0.9(7) . . . . ? C17 C12 C13 C14 -178.2(5) . . . . ? C12 C13 C14 C15 1.8(8) . . . . ? C12 C13 C14 C18 -178.3(5) . . . . ? C13 C14 C15 C16 -3.5(7) . . . . ? C18 C14 C15 C16 176.5(5) . . . . ? C12 C11 C16 C15 0.4(7) . . . . ? N1 C11 C16 C15 -178.5(4) . . . . ? C12 C11 C16 C19 179.1(5) . . . . ? N1 C11 C16 C19 0.1(7) . . . . ? C14 C15 C16 C11 2.4(7) . . . . ? C14 C15 C16 C19 -176.2(5) . . . . ? C2 N3 C21 C26 89.7(6) . . . . ? C5 N3 C21 C26 -94.4(6) . . . . ? C2 N3 C21 C22 -91.3(6) . . . . ? C5 N3 C21 C22 84.5(6) . . . . ? C26 C21 C22 C23 -3.2(7) . . . . ? N3 C21 C22 C23 177.9(4) . . . . ? C26 C21 C22 C27 178.3(5) . . . . ? N3 C21 C22 C27 -0.7(7) . . . . ? C21 C22 C23 C24 2.3(8) . . . . ? C27 C22 C23 C24 -179.1(5) . . . . ? C22 C23 C24 C25 -0.2(8) . . . . ? C22 C23 C24 C28 179.1(5) . . . . ? C23 C24 C25 C26 -1.2(7) . . . . ? C28 C24 C25 C26 179.5(5) . . . . ? C22 C21 C26 C25 1.9(7) . . . . ? N3 C21 C26 C25 -179.2(4) . . . . ? C22 C21 C26 C29 -177.7(5) . . . . ? N3 C21 C26 C29 1.2(7) . . . . ? C24 C25 C26 C21 0.4(7) . . . . ? C24 C25 C26 C29 179.9(4) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 23.54 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.063 _refine_diff_density_min -0.506 _refine_diff_density_rms 0.095 _exptl_crystal_recrystallization_method 'slow diff of n-hexane into ether/dichloromethane soln' # Attachment 'Slaughter_Cmplx6_form11.cif' data_cmplx6_form1_lms195 _database_code_depnum_ccdc_archive 'CCDC 736964' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common (Pd(DIMesMe)(CO)(CH3))(BF4) _chemical_formula_moiety 'C27 H31 N4 O Pd, C H2 Cl2, B F4' _chemical_formula_sum 'C28 H33 B Cl2 F4 N4 O Pd' _chemical_compound_source ? _exptl_crystal_recrystallization_method 'slow diff of hexane into diethyl ether/dichloromethane soln' _chemical_melting_point ? _exptl_crystal_description block _exptl_crystal_colour yellow _diffrn_ambient_temperature 115(2) _chemical_formula_weight 705.69 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' B B 0.0013 0.0007 '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' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_int_tables_number 2 _chemical_absolute_configuration ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.3442(5) _cell_length_b 14.0019(9) _cell_length_c 15.7474(10) _cell_angle_alpha 101.273(4) _cell_angle_beta 101.577(4) _cell_angle_gamma 96.190(4) _cell_volume 1537.46(17) _cell_formula_units_Z 2 _cell_measurement_temperature 115(2) _cell_measurement_reflns_used 9849 _cell_measurement_theta_min 2.71 _cell_measurement_theta_max 26.30 _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.524 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 716 _exptl_absorpt_coefficient_mu 0.830 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8069 _exptl_absorpt_correction_T_max 0.9216 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; ? ; _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX II CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 0.75 _diffrn_standards_number 0 _diffrn_standards_interval_count N/A _diffrn_standards_interval_time N/A _diffrn_standards_decay_% N/A _diffrn_reflns_number 21988 _diffrn_reflns_av_R_equivalents 0.0251 _diffrn_reflns_av_sigmaI/netI 0.0227 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.35 _diffrn_reflns_theta_max 25.68 _reflns_number_total 5799 _reflns_number_gt 5179 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL (XS)' _computing_structure_refinement 'Bruker SHELXTL (XL)' _computing_molecular_graphics 'Bruker SHELXTL (XP)' _computing_publication_material 'Bruker SHELXTL (XCIF)' _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^)+(0.0586P)^2^+2.8491P] 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 5799 _refine_ls_number_parameters 377 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0435 _refine_ls_R_factor_gt 0.0375 _refine_ls_wR_factor_ref 0.1066 _refine_ls_wR_factor_gt 0.1012 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.037 _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 -0.00434(3) 0.255107(17) 0.217061(16) 0.02541(10) Uani 1 1 d . . . C1 C 0.1782(5) 0.1684(2) 0.1710(2) 0.0273(7) Uani 1 1 d . . . C2 C 0.1305(5) 0.3661(2) 0.1727(2) 0.0286(7) Uani 1 1 d . . . N1 N 0.2596(4) 0.0938(2) 0.19774(18) 0.0286(6) Uani 1 1 d . . . C3 C 0.3761(5) 0.0601(3) 0.1430(2) 0.0345(8) Uani 1 1 d . . . H3 H 0.4473 0.0079 0.1478 0.041 Uiso 1 1 calc R . . C4 C 0.3694(5) 0.1148(3) 0.0822(2) 0.0350(8) Uani 1 1 d . . . H4 H 0.4349 0.1094 0.0356 0.042 Uiso 1 1 calc R . . N2 N 0.2485(4) 0.1806(2) 0.10044(17) 0.0280(6) Uani 1 1 d . . . N3 N 0.1654(4) 0.4654(2) 0.20022(18) 0.0286(6) Uani 1 1 d . . . N4 N 0.2120(4) 0.3483(2) 0.10244(17) 0.0292(6) Uani 1 1 d . . . C5 C 0.2650(6) 0.5082(3) 0.1476(2) 0.0355(8) Uani 1 1 d . . . H5 H 0.3052 0.5766 0.1540 0.043 Uiso 1 1 calc R . . C6 C 0.2935(5) 0.4343(3) 0.0860(2) 0.0345(8) Uani 1 1 d . . . H6 H 0.3573 0.4399 0.0399 0.041 Uiso 1 1 calc R . . C7 C 0.1914(5) 0.2507(2) 0.0464(2) 0.0307(7) Uani 1 1 d . . . H7A H 0.2701 0.2522 0.0023 0.037 Uiso 1 1 calc R . . H7B H 0.0587 0.2295 0.0137 0.037 Uiso 1 1 calc R . . C8 C -0.1411(6) 0.1420(3) 0.2588(3) 0.0470(10) Uani 1 1 d . . . H8A H -0.0811 0.1436 0.3207 0.071 Uiso 1 1 calc R . . H8B H -0.1336 0.0786 0.2211 0.071 Uiso 1 1 calc R . . H8C H -0.2733 0.1500 0.2544 0.071 Uiso 1 1 calc R . . C9 C -0.1941(6) 0.3286(3) 0.2538(3) 0.0407(9) Uani 1 1 d . . . O1 O -0.3063(6) 0.3614(3) 0.2740(3) 0.0843(13) Uani 1 1 d . . . C11 C 0.2319(5) 0.0503(2) 0.2710(2) 0.0279(7) Uani 1 1 d . . . C12 C 0.1263(5) -0.0439(3) 0.2508(2) 0.0330(7) Uani 1 1 d . . . C13 C 0.1114(5) -0.0879(3) 0.3209(3) 0.0359(8) Uani 1 1 d . . . H13 H 0.0426 -0.1524 0.3087 0.043 Uiso 1 1 calc R . . C14 C 0.1936(5) -0.0410(3) 0.4082(2) 0.0326(7) Uani 1 1 d . . . C15 C 0.2937(5) 0.0526(2) 0.4256(2) 0.0292(7) Uani 1 1 d . . . H15 H 0.3485 0.0855 0.4855 0.035 Uiso 1 1 calc R . . C16 C 0.3170(4) 0.1004(2) 0.3579(2) 0.0263(7) Uani 1 1 d . . . C17 C 0.0293(6) -0.0957(3) 0.1568(3) 0.0458(10) Uani 1 1 d . . . H17A H 0.1233 -0.1171 0.1240 0.069 Uiso 1 1 calc R . . H17B H -0.0401 -0.0505 0.1277 0.069 Uiso 1 1 calc R . . H17C H -0.0584 -0.1533 0.1576 0.069 Uiso 1 1 calc R . . C18 C 0.1715(6) -0.0922(3) 0.4825(3) 0.0418(9) Uani 1 1 d . . . H18A H 0.0439 -0.0914 0.4922 0.063 Uiso 1 1 calc R . . H18B H 0.2631 -0.0578 0.5371 0.063 Uiso 1 1 calc R . . H18C H 0.1932 -0.1605 0.4663 0.063 Uiso 1 1 calc R . . C19 C 0.4270(5) 0.2022(3) 0.3789(2) 0.0341(8) Uani 1 1 d . . . H19A H 0.5255 0.2026 0.3451 0.051 Uiso 1 1 calc R . . H19B H 0.4849 0.2219 0.4427 0.051 Uiso 1 1 calc R . . H19C H 0.3425 0.2485 0.3626 0.051 Uiso 1 1 calc R . . C21 C 0.1089(5) 0.5198(2) 0.2757(2) 0.0282(7) Uani 1 1 d . . . C22 C -0.0478(5) 0.5672(3) 0.2604(3) 0.0360(8) Uani 1 1 d . . . C23 C -0.1018(6) 0.6167(3) 0.3349(3) 0.0411(9) Uani 1 1 d . . . H23 H -0.2087 0.6494 0.3266 0.049 Uiso 1 1 calc R . . C24 C -0.0045(6) 0.6198(3) 0.4206(3) 0.0396(9) Uani 1 1 d . . . C25 C 0.1531(6) 0.5735(3) 0.4325(2) 0.0375(8) Uani 1 1 d . . . H25 H 0.2212 0.5759 0.4911 0.045 Uiso 1 1 calc R . . C26 C 0.2141(5) 0.5235(2) 0.3606(2) 0.0321(7) Uani 1 1 d . . . C27 C -0.1551(6) 0.5636(4) 0.1669(3) 0.0506(10) Uani 1 1 d . . . H27A H -0.0803 0.6050 0.1389 0.076 Uiso 1 1 calc R . . H27B H -0.2746 0.5880 0.1691 0.076 Uiso 1 1 calc R . . H27C H -0.1798 0.4955 0.1322 0.076 Uiso 1 1 calc R . . C28 C -0.0702(8) 0.6716(3) 0.5006(3) 0.0552(12) Uani 1 1 d . . . H28A H -0.1635 0.7127 0.4814 0.083 Uiso 1 1 calc R . . H28B H 0.0375 0.7132 0.5440 0.083 Uiso 1 1 calc R . . H28C H -0.1270 0.6224 0.5279 0.083 Uiso 1 1 calc R . . C29 C 0.3897(6) 0.4774(3) 0.3737(3) 0.0446(9) Uani 1 1 d . . . H29A H 0.4469 0.4893 0.4374 0.067 Uiso 1 1 calc R . . H29B H 0.4787 0.5065 0.3435 0.067 Uiso 1 1 calc R . . H29C H 0.3585 0.4063 0.3487 0.067 Uiso 1 1 calc R . . B1 B 0.6360(7) 0.2785(3) 0.9665(3) 0.0412(10) Uani 1 1 d . . . F1 F 0.8004(4) 0.2999(2) 0.9410(2) 0.0705(9) Uani 1 1 d . . . F2 F 0.6552(5) 0.2997(2) 1.05743(17) 0.0661(8) Uani 1 1 d . . . F3 F 0.5633(4) 0.17883(18) 0.93184(17) 0.0615(7) Uani 1 1 d . . . F4 F 0.5054(3) 0.33307(19) 0.93063(16) 0.0507(6) Uani 1 1 d . . . C100 C 0.4865(6) 0.7957(3) 0.2623(3) 0.0479(10) Uani 1 1 d . . . H101 H 0.5457 0.7512 0.2228 0.057 Uiso 1 1 calc R . . H100 H 0.3648 0.8048 0.2268 0.057 Uiso 1 1 calc R . . Cl1 Cl 0.63230(18) 0.90999(9) 0.30142(9) 0.0626(3) Uani 1 1 d . . . Cl2 Cl 0.44514(16) 0.74055(8) 0.34881(7) 0.0491(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 0.03019(15) 0.02396(14) 0.02353(14) 0.00525(9) 0.00760(10) 0.00773(10) C1 0.0329(17) 0.0266(16) 0.0217(15) 0.0044(12) 0.0047(13) 0.0065(13) C2 0.0385(18) 0.0303(17) 0.0170(15) 0.0050(12) 0.0046(13) 0.0085(14) N1 0.0374(16) 0.0273(14) 0.0241(14) 0.0050(11) 0.0110(12) 0.0118(12) C3 0.046(2) 0.0322(18) 0.0306(18) 0.0060(14) 0.0162(16) 0.0170(15) C4 0.048(2) 0.0323(18) 0.0292(18) 0.0045(14) 0.0169(16) 0.0140(16) N2 0.0372(15) 0.0285(14) 0.0204(13) 0.0040(11) 0.0093(11) 0.0110(12) N3 0.0409(16) 0.0249(14) 0.0213(13) 0.0063(11) 0.0080(12) 0.0066(12) N4 0.0435(16) 0.0256(14) 0.0193(13) 0.0040(11) 0.0081(12) 0.0090(12) C5 0.051(2) 0.0283(17) 0.0300(18) 0.0098(14) 0.0129(16) 0.0073(15) C6 0.048(2) 0.0348(18) 0.0261(17) 0.0133(14) 0.0132(15) 0.0080(16) C7 0.044(2) 0.0292(17) 0.0190(15) 0.0043(13) 0.0068(14) 0.0099(14) C8 0.037(2) 0.053(2) 0.065(3) 0.024(2) 0.023(2) 0.0210(18) C9 0.044(2) 0.039(2) 0.046(2) 0.0124(17) 0.0221(18) 0.0087(17) O1 0.093(3) 0.064(2) 0.124(4) 0.036(2) 0.063(3) 0.030(2) C11 0.0316(17) 0.0284(16) 0.0267(16) 0.0071(13) 0.0095(13) 0.0107(13) C12 0.0399(19) 0.0297(17) 0.0293(18) 0.0022(14) 0.0103(15) 0.0086(15) C13 0.040(2) 0.0258(17) 0.042(2) 0.0058(15) 0.0128(16) 0.0033(14) C14 0.0381(19) 0.0295(17) 0.0345(18) 0.0092(14) 0.0138(15) 0.0099(14) C15 0.0335(18) 0.0298(17) 0.0251(16) 0.0042(13) 0.0089(14) 0.0080(13) C16 0.0281(16) 0.0255(16) 0.0270(16) 0.0048(13) 0.0085(13) 0.0093(13) C17 0.058(3) 0.038(2) 0.033(2) -0.0041(16) 0.0054(18) 0.0010(18) C18 0.054(2) 0.036(2) 0.042(2) 0.0162(17) 0.0187(18) 0.0099(17) C19 0.042(2) 0.0300(18) 0.0298(18) 0.0061(14) 0.0089(15) 0.0017(15) C21 0.0370(18) 0.0224(15) 0.0263(16) 0.0047(13) 0.0103(14) 0.0047(13) C22 0.040(2) 0.0312(18) 0.038(2) 0.0103(15) 0.0095(16) 0.0084(15) C23 0.044(2) 0.0316(19) 0.056(2) 0.0127(17) 0.0216(19) 0.0128(16) C24 0.059(2) 0.0248(17) 0.042(2) 0.0072(15) 0.0275(19) 0.0072(16) C25 0.055(2) 0.0319(18) 0.0269(18) 0.0057(14) 0.0131(16) 0.0069(16) C26 0.043(2) 0.0283(17) 0.0266(17) 0.0068(13) 0.0101(15) 0.0088(14) C27 0.047(2) 0.061(3) 0.045(2) 0.017(2) 0.0003(19) 0.020(2) C28 0.087(3) 0.036(2) 0.058(3) 0.0090(19) 0.050(3) 0.016(2) C29 0.056(2) 0.051(2) 0.0279(19) 0.0081(17) 0.0045(17) 0.0218(19) B1 0.046(3) 0.041(2) 0.042(2) 0.0195(19) 0.010(2) 0.0116(19) F1 0.0459(15) 0.0645(18) 0.121(3) 0.0487(18) 0.0308(16) 0.0225(13) F2 0.090(2) 0.0595(17) 0.0414(14) 0.0117(12) -0.0041(14) 0.0135(15) F3 0.099(2) 0.0420(13) 0.0510(15) 0.0088(11) 0.0384(15) 0.0062(13) F4 0.0524(14) 0.0670(16) 0.0457(13) 0.0249(12) 0.0188(11) 0.0290(12) C100 0.053(2) 0.050(2) 0.040(2) 0.0077(18) 0.0091(19) 0.0084(19) Cl1 0.0583(7) 0.0570(7) 0.0683(8) 0.0123(6) 0.0127(6) -0.0027(5) Cl2 0.0633(6) 0.0418(5) 0.0466(6) 0.0105(4) 0.0194(5) 0.0127(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 C9 1.933(4) . ? Pd1 C1 2.047(3) . ? Pd1 C2 2.062(3) . ? Pd1 C8 2.069(4) . ? C1 N2 1.349(4) . ? C1 N1 1.354(4) . ? C2 N3 1.353(4) . ? C2 N4 1.355(4) . ? N1 C3 1.386(4) . ? N1 C11 1.443(4) . ? C3 C4 1.335(5) . ? C3 H3 0.9500 . ? C4 N2 1.377(4) . ? C4 H4 0.9500 . ? N2 C7 1.461(4) . ? N3 C5 1.387(4) . ? N3 C21 1.441(4) . ? N4 C6 1.379(5) . ? N4 C7 1.449(4) . ? C5 C6 1.339(5) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 O1 1.059(5) . ? C11 C16 1.394(5) . ? C11 C12 1.399(5) . ? C12 C13 1.382(5) . ? C12 C17 1.507(5) . ? C13 C14 1.384(5) . ? C13 H13 0.9500 . ? C14 C15 1.380(5) . ? C14 C18 1.512(5) . ? C15 C16 1.393(5) . ? C15 H15 0.9500 . ? C16 C19 1.502(5) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C21 C26 1.391(5) . ? C21 C22 1.393(5) . ? C22 C23 1.392(5) . ? C22 C27 1.512(5) . ? C23 C24 1.386(6) . ? C23 H23 0.9500 . ? C24 C25 1.384(6) . ? C24 C28 1.519(5) . ? C25 C26 1.391(5) . ? C25 H25 0.9500 . ? C26 C29 1.499(5) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? B1 F1 1.369(5) . ? B1 F2 1.379(5) . ? B1 F4 1.390(5) . ? B1 F3 1.399(5) . ? C100 Cl1 1.751(4) . ? C100 Cl2 1.752(4) . ? C100 H101 0.9900 . ? C100 H100 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 C9 Pd1 C1 175.04(15) . . ? C9 Pd1 C2 95.86(15) . . ? C1 Pd1 C2 86.77(13) . . ? C9 Pd1 C8 84.69(16) . . ? C1 Pd1 C8 92.60(14) . . ? C2 Pd1 C8 178.78(16) . . ? N2 C1 N1 104.0(3) . . ? N2 C1 Pd1 122.1(2) . . ? N1 C1 Pd1 133.9(2) . . ? N3 C2 N4 103.5(3) . . ? N3 C2 Pd1 133.7(2) . . ? N4 C2 Pd1 122.7(2) . . ? C1 N1 C3 110.7(3) . . ? C1 N1 C11 127.1(3) . . ? C3 N1 C11 122.2(3) . . ? C4 C3 N1 107.2(3) . . ? C4 C3 H3 126.4 . . ? N1 C3 H3 126.4 . . ? C3 C4 N2 106.2(3) . . ? C3 C4 H4 126.9 . . ? N2 C4 H4 126.9 . . ? C1 N2 C4 111.9(3) . . ? C1 N2 C7 123.5(3) . . ? C4 N2 C7 124.5(3) . . ? C2 N3 C5 111.6(3) . . ? C2 N3 C21 124.2(3) . . ? C5 N3 C21 124.2(3) . . ? C2 N4 C6 111.9(3) . . ? C2 N4 C7 122.2(3) . . ? C6 N4 C7 125.5(3) . . ? C6 C5 N3 106.5(3) . . ? C6 C5 H5 126.7 . . ? N3 C5 H5 126.7 . . ? C5 C6 N4 106.6(3) . . ? C5 C6 H6 126.7 . . ? N4 C6 H6 126.7 . . ? N4 C7 N2 110.2(3) . . ? N4 C7 H7A 109.6 . . ? N2 C7 H7A 109.6 . . ? N4 C7 H7B 109.6 . . ? N2 C7 H7B 109.6 . . ? H7A C7 H7B 108.1 . . ? Pd1 C8 H8A 109.5 . . ? Pd1 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? Pd1 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? O1 C9 Pd1 173.8(4) . . ? C16 C11 C12 122.5(3) . . ? C16 C11 N1 119.7(3) . . ? C12 C11 N1 117.7(3) . . ? C13 C12 C11 117.4(3) . . ? C13 C12 C17 120.6(3) . . ? C11 C12 C17 122.0(3) . . ? C12 C13 C14 122.1(3) . . ? C12 C13 H13 119.0 . . ? C14 C13 H13 119.0 . . ? C15 C14 C13 118.7(3) . . ? C15 C14 C18 121.3(3) . . ? C13 C14 C18 119.9(3) . . ? C14 C15 C16 122.0(3) . . ? C14 C15 H15 119.0 . . ? C16 C15 H15 119.0 . . ? C15 C16 C11 117.2(3) . . ? C15 C16 C19 120.8(3) . . ? C11 C16 C19 122.0(3) . . ? C12 C17 H17A 109.5 . . ? C12 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C12 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C14 C18 H18A 109.5 . . ? C14 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C14 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C16 C19 H19A 109.5 . . ? C16 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C16 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C26 C21 C22 122.8(3) . . ? C26 C21 N3 118.7(3) . . ? C22 C21 N3 118.5(3) . . ? C23 C22 C21 117.0(3) . . ? C23 C22 C27 121.9(4) . . ? C21 C22 C27 121.1(3) . . ? C24 C23 C22 122.1(4) . . ? C24 C23 H23 119.0 . . ? C22 C23 H23 119.0 . . ? C25 C24 C23 118.8(3) . . ? C25 C24 C28 120.3(4) . . ? C23 C24 C28 120.9(4) . . ? C24 C25 C26 121.6(4) . . ? C24 C25 H25 119.2 . . ? C26 C25 H25 119.2 . . ? C25 C26 C21 117.7(3) . . ? C25 C26 C29 121.3(3) . . ? C21 C26 C29 121.0(3) . . ? C22 C27 H27A 109.5 . . ? C22 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C22 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C24 C28 H28A 109.5 . . ? C24 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C24 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C26 C29 H29A 109.5 . . ? C26 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C26 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? F1 B1 F2 113.6(4) . . ? F1 B1 F4 109.0(3) . . ? F2 B1 F4 107.9(4) . . ? F1 B1 F3 109.3(4) . . ? F2 B1 F3 109.5(3) . . ? F4 B1 F3 107.5(4) . . ? Cl1 C100 Cl2 112.4(2) . . ? Cl1 C100 H101 109.1 . . ? Cl2 C100 H101 109.1 . . ? Cl1 C100 H100 109.1 . . ? Cl2 C100 H100 109.1 . . ? H101 C100 H100 107.9 . . ? 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 C2 Pd1 C1 N2 -30.8(3) . . . . ? C8 Pd1 C1 N2 148.2(3) . . . . ? C2 Pd1 C1 N1 147.4(3) . . . . ? C8 Pd1 C1 N1 -33.7(4) . . . . ? C9 Pd1 C2 N3 35.2(4) . . . . ? C1 Pd1 C2 N3 -149.1(3) . . . . ? C9 Pd1 C2 N4 -146.0(3) . . . . ? C1 Pd1 C2 N4 29.7(3) . . . . ? N2 C1 N1 C3 -0.9(4) . . . . ? Pd1 C1 N1 C3 -179.3(3) . . . . ? N2 C1 N1 C11 -179.5(3) . . . . ? Pd1 C1 N1 C11 2.1(5) . . . . ? C1 N1 C3 C4 0.8(4) . . . . ? C11 N1 C3 C4 179.5(3) . . . . ? N1 C3 C4 N2 -0.3(4) . . . . ? N1 C1 N2 C4 0.7(4) . . . . ? Pd1 C1 N2 C4 179.4(2) . . . . ? N1 C1 N2 C7 176.5(3) . . . . ? Pd1 C1 N2 C7 -4.8(4) . . . . ? C3 C4 N2 C1 -0.3(4) . . . . ? C3 C4 N2 C7 -176.0(3) . . . . ? N4 C2 N3 C5 0.5(4) . . . . ? Pd1 C2 N3 C5 179.4(3) . . . . ? N4 C2 N3 C21 -178.5(3) . . . . ? Pd1 C2 N3 C21 0.4(5) . . . . ? N3 C2 N4 C6 -0.7(4) . . . . ? Pd1 C2 N4 C6 -179.8(2) . . . . ? N3 C2 N4 C7 -173.4(3) . . . . ? Pd1 C2 N4 C7 7.5(4) . . . . ? C2 N3 C5 C6 -0.1(4) . . . . ? C21 N3 C5 C6 178.9(3) . . . . ? N3 C5 C6 N4 -0.3(4) . . . . ? C2 N4 C6 C5 0.6(4) . . . . ? C7 N4 C6 C5 173.0(3) . . . . ? C2 N4 C7 N2 -54.4(4) . . . . ? C6 N4 C7 N2 133.9(3) . . . . ? C1 N2 C7 N4 53.5(4) . . . . ? C4 N2 C7 N4 -131.3(3) . . . . ? C1 N1 C11 C16 -75.9(4) . . . . ? C3 N1 C11 C16 105.6(4) . . . . ? C1 N1 C11 C12 107.1(4) . . . . ? C3 N1 C11 C12 -71.4(4) . . . . ? C16 C11 C12 C13 -1.3(5) . . . . ? N1 C11 C12 C13 175.6(3) . . . . ? C16 C11 C12 C17 177.8(3) . . . . ? N1 C11 C12 C17 -5.3(5) . . . . ? C11 C12 C13 C14 1.3(5) . . . . ? C17 C12 C13 C14 -177.8(4) . . . . ? C12 C13 C14 C15 -0.1(6) . . . . ? C12 C13 C14 C18 179.5(3) . . . . ? C13 C14 C15 C16 -1.1(5) . . . . ? C18 C14 C15 C16 179.3(3) . . . . ? C14 C15 C16 C11 1.0(5) . . . . ? C14 C15 C16 C19 -179.9(3) . . . . ? C12 C11 C16 C15 0.2(5) . . . . ? N1 C11 C16 C15 -176.6(3) . . . . ? C12 C11 C16 C19 -178.8(3) . . . . ? N1 C11 C16 C19 4.3(5) . . . . ? C2 N3 C21 C26 78.2(4) . . . . ? C5 N3 C21 C26 -100.7(4) . . . . ? C2 N3 C21 C22 -102.4(4) . . . . ? C5 N3 C21 C22 78.7(4) . . . . ? C26 C21 C22 C23 -2.5(5) . . . . ? N3 C21 C22 C23 178.2(3) . . . . ? C26 C21 C22 C27 178.3(4) . . . . ? N3 C21 C22 C27 -1.0(5) . . . . ? C21 C22 C23 C24 0.4(6) . . . . ? C27 C22 C23 C24 179.7(4) . . . . ? C22 C23 C24 C25 1.1(6) . . . . ? C22 C23 C24 C28 -178.1(4) . . . . ? C23 C24 C25 C26 -0.7(6) . . . . ? C28 C24 C25 C26 178.5(4) . . . . ? C24 C25 C26 C21 -1.2(5) . . . . ? C24 C25 C26 C29 177.2(4) . . . . ? C22 C21 C26 C25 2.8(5) . . . . ? N3 C21 C26 C25 -177.8(3) . . . . ? C22 C21 C26 C29 -175.6(4) . . . . ? N3 C21 C26 C29 3.8(5) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 2.374 _refine_diff_density_min -1.000 _refine_diff_density_rms 0.087