Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Chen, Jwu-Ting' 'Lee, Gene-Hsiang' 'Liu, Shiuh-Tzung' 'Peng, Shie-ming' 'Reddy, K. Rajender' 'Surekha, K.' 'Tsai, Wei-wen' _publ_contact_author_name 'Prof Shiuh-Tzung Liu' _publ_contact_author_address ; Prof Shiuh-Tzung Liu Chemistry National Taiwan University 1, Sec. 4, Roosevelt Road Taipei 106 TAIWAN ; _publ_contact_author_email 'STLIU@CCMS.NTU.EDU.TW' _publ_section_title ; Ligand effects on palladium complexes catalyzed copolymerization of ethylene/carbon monoxide ; data_ic5413 _database_code_CSD 172819 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H25 Cl3 N O P Pd' _chemical_formula_weight 635.21 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' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pd' 'Pd' -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.5745(1) _cell_length_b 9.8728(1) _cell_length_c 15.3826(2) _cell_angle_alpha 79.672(1) _cell_angle_beta 83.546(1) _cell_angle_gamma 81.263(1) _cell_volume 1408.48(3) _cell_formula_units_Z 2 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 8192 _cell_measurement_theta_min 1.35 _cell_measurement_theta_max 27.50 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas not_measured _exptl_crystal_density_diffrn 1.498 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 640 _exptl_absorpt_coefficient_mu 1.021 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.4382 _exptl_absorpt_correction_T_max 0.4923 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 5 _diffrn_reflns_number 18402 _diffrn_reflns_av_R_equivalents 0.0335 _diffrn_reflns_av_sigmaI/netI 0.0403 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.35 _diffrn_reflns_theta_max 27.50 _reflns_number_total 6472 _reflns_number_gt 5314 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0333P)^2^+0.6865P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6472 _refine_ls_number_parameters 334 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0534 _refine_ls_R_factor_gt 0.0372 _refine_ls_wR_factor_ref 0.0849 _refine_ls_wR_factor_gt 0.0789 _refine_ls_goodness_of_fit_ref 1.071 _refine_ls_restrained_S_all 1.071 _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 Pd Pd 0.54524(2) 0.51562(2) 0.736623(13) 0.03688(7) Uani 1 1 d . . . Cl Cl 0.31842(8) 0.49067(9) 0.69730(5) 0.05405(19) Uani 1 1 d . . . P1 P 0.77180(7) 0.50146(7) 0.76720(5) 0.03724(16) Uani 1 1 d . . . O1 O 0.4608(3) 0.3882(3) 0.91090(17) 0.0816(8) Uani 1 1 d . . . N1 N 0.6590(2) 0.5421(2) 0.59717(14) 0.0383(5) Uani 1 1 d . . . C1 C 0.4578(3) 0.4961(4) 0.8606(2) 0.0540(8) Uani 1 1 d . . . C2 C 0.3767(5) 0.6300(5) 0.8836(3) 0.0886(13) Uani 1 1 d . . . H2A H 0.3367 0.6147 0.9441 0.133 Uiso 1 1 calc R . . H2B H 0.3019 0.6617 0.8452 0.133 Uiso 1 1 calc R . . H2C H 0.4397 0.6989 0.8763 0.133 Uiso 1 1 calc R . . C3 C 0.8619(3) 0.4238(3) 0.67305(18) 0.0381(6) Uani 1 1 d . . . C4 C 0.9918(3) 0.3370(3) 0.6761(2) 0.0475(7) Uani 1 1 d . . . H4A H 1.0406 0.3214 0.7267 0.057 Uiso 1 1 calc R . . C5 C 1.0478(3) 0.2743(3) 0.6039(2) 0.0542(8) Uani 1 1 d . . . H5A H 1.1343 0.2169 0.6060 0.065 Uiso 1 1 calc R . . C6 C 0.9752(3) 0.2967(3) 0.5288(2) 0.0550(8) Uani 1 1 d . . . H6A H 1.0127 0.2531 0.4809 0.066 Uiso 1 1 calc R . . C7 C 0.8467(3) 0.3839(3) 0.52398(19) 0.0478(7) Uani 1 1 d . . . H7A H 0.7989 0.3990 0.4730 0.057 Uiso 1 1 calc R . . C8 C 0.7901(3) 0.4482(3) 0.59593(18) 0.0377(6) Uani 1 1 d . . . C10 C 0.6247(3) 0.6181(3) 0.52388(18) 0.0421(6) Uani 1 1 d . . . H10A H 0.6801 0.5999 0.4725 0.050 Uiso 1 1 calc R . . C11 C 0.8389(3) 0.6660(3) 0.76192(19) 0.0425(6) Uani 1 1 d . . . C12 C 0.9668(4) 0.6936(4) 0.7184(3) 0.0750(11) Uani 1 1 d . . . H12A H 1.0236 0.6268 0.6898 0.090 Uiso 1 1 calc R . . C13 C 1.0120(6) 0.8217(6) 0.7168(4) 0.1057(17) Uani 1 1 d . . . H13A H 1.0992 0.8397 0.6874 0.127 Uiso 1 1 calc R . . C14 C 0.9302(6) 0.9208(5) 0.7578(3) 0.0947(16) Uani 1 1 d . . . H14A H 0.9609 1.0062 0.7562 0.114 Uiso 1 1 calc R . . C15 C 0.8054(5) 0.8944(4) 0.8004(4) 0.0939(15) Uani 1 1 d . . . H15A H 0.7494 0.9620 0.8287 0.113 Uiso 1 1 calc R . . C16 C 0.7585(4) 0.7681(4) 0.8030(3) 0.0733(11) Uani 1 1 d . . . H16A H 0.6712 0.7518 0.8330 0.088 Uiso 1 1 calc R . . C21 C 0.8461(3) 0.3866(3) 0.86232(18) 0.0443(7) Uani 1 1 d . . . C22 C 0.7878(4) 0.2644(3) 0.8934(2) 0.0580(8) Uani 1 1 d . . . H22A H 0.7107 0.2460 0.8677 0.070 Uiso 1 1 calc R . . C23 C 0.8447(5) 0.1702(4) 0.9623(3) 0.0775(12) Uani 1 1 d . . . H23A H 0.8060 0.0882 0.9826 0.093 Uiso 1 1 calc R . . C24 C 0.9568(6) 0.1965(5) 1.0007(3) 0.0865(14) Uani 1 1 d . . . H24A H 0.9937 0.1329 1.0475 0.104 Uiso 1 1 calc R . . C25 C 1.0156(5) 0.3164(5) 0.9706(3) 0.0870(14) Uani 1 1 d . . . H25A H 1.0926 0.3335 0.9969 0.104 Uiso 1 1 calc R . . C26 C 0.9602(4) 0.4132(4) 0.9006(2) 0.0650(9) Uani 1 1 d . . . H26A H 1.0001 0.4945 0.8801 0.078 Uiso 1 1 calc R . . C31 C 0.5061(3) 0.7309(3) 0.5138(2) 0.0441(6) Uani 1 1 d . . . C32 C 0.4597(4) 0.7765(4) 0.4293(2) 0.0609(9) Uani 1 1 d . . . H32A H 0.5000 0.7318 0.3824 0.073 Uiso 1 1 calc R . . C33 C 0.3533(4) 0.8884(4) 0.4152(3) 0.0830(13) Uani 1 1 d . . . H33A H 0.3214 0.9171 0.3591 0.100 Uiso 1 1 calc R . . C34 C 0.2953(4) 0.9563(4) 0.4830(4) 0.0860(14) Uani 1 1 d . . . H34A H 0.2239 1.0309 0.4730 0.103 Uiso 1 1 calc R . . C35 C 0.3423(4) 0.9147(4) 0.5665(3) 0.0771(12) Uani 1 1 d . . . H35A H 0.3039 0.9627 0.6124 0.093 Uiso 1 1 calc R . . C36 C 0.4462(4) 0.8017(3) 0.5822(2) 0.0578(8) Uani 1 1 d . . . H36A H 0.4761 0.7730 0.6388 0.069 Uiso 1 1 calc R . . C41 C 1.3453(7) 1.1470(6) 0.8404(4) 0.128(2) Uani 1 1 d . . . H41A H 1.3428 1.2382 0.8040 0.154 Uiso 0.50 1 calc PR A 1 H41B H 1.3252 1.1594 0.9020 0.154 Uiso 0.50 1 calc PR A 1 H41C H 1.2614 1.2019 0.8638 0.154 Uiso 0.50 1 d PR A 2 H41D H 1.4042 1.2102 0.8031 0.154 Uiso 0.50 1 d PR A 2 Cl2 Cl 1.2134(4) 1.0576(5) 0.8105(3) 0.1067(11) Uani 0.50 1 d P B 1 Cl3 Cl 1.4950(4) 1.0632(6) 0.8273(5) 0.228(3) Uani 0.50 1 d P B 1 Cl2' Cl 1.3003(9) 1.0460(8) 0.7831(5) 0.220(4) Uani 0.50 1 d P B 2 Cl3' Cl 1.4436(4) 1.0480(5) 0.9320(3) 0.1540(15) Uani 0.50 1 d P . 2 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 Pd 0.03169(11) 0.04582(13) 0.03471(12) -0.01137(8) -0.00396(8) -0.00383(8) Cl 0.0363(4) 0.0764(5) 0.0529(4) -0.0136(4) -0.0101(3) -0.0106(3) P1 0.0345(4) 0.0419(4) 0.0369(4) -0.0094(3) -0.0076(3) -0.0033(3) O1 0.087(2) 0.098(2) 0.0505(15) 0.0063(15) 0.0044(13) -0.0145(16) N1 0.0346(12) 0.0452(13) 0.0357(12) -0.0090(10) -0.0036(9) -0.0041(10) C1 0.0429(17) 0.079(2) 0.0414(17) -0.0158(17) 0.0002(13) -0.0089(16) C2 0.080(3) 0.113(4) 0.075(3) -0.051(3) 0.015(2) 0.004(2) C3 0.0332(14) 0.0411(15) 0.0404(14) -0.0100(12) -0.0033(11) -0.0026(11) C4 0.0402(16) 0.0527(17) 0.0487(17) -0.0083(14) -0.0097(13) 0.0011(13) C5 0.0433(17) 0.0534(18) 0.062(2) -0.0136(15) -0.0039(15) 0.0099(14) C6 0.0572(19) 0.0552(19) 0.0514(18) -0.0209(15) 0.0040(15) 0.0045(15) C7 0.0492(17) 0.0543(18) 0.0404(15) -0.0129(13) -0.0043(13) -0.0020(14) C8 0.0335(13) 0.0387(14) 0.0407(14) -0.0081(11) -0.0037(11) -0.0022(11) C10 0.0399(15) 0.0493(16) 0.0375(15) -0.0097(12) -0.0031(12) -0.0051(12) C11 0.0422(15) 0.0439(15) 0.0428(15) -0.0048(12) -0.0142(12) -0.0053(12) C12 0.069(2) 0.080(3) 0.084(3) -0.026(2) 0.014(2) -0.034(2) C13 0.107(4) 0.113(4) 0.110(4) -0.017(3) 0.012(3) -0.074(3) C14 0.130(4) 0.061(3) 0.107(4) 0.000(2) -0.049(3) -0.044(3) C15 0.096(3) 0.054(2) 0.144(4) -0.037(3) -0.041(3) -0.005(2) C16 0.057(2) 0.059(2) 0.112(3) -0.036(2) -0.007(2) -0.0068(17) C21 0.0533(17) 0.0428(16) 0.0368(14) -0.0108(12) -0.0091(13) 0.0021(13) C22 0.062(2) 0.0526(19) 0.0553(19) -0.0056(15) -0.0041(16) -0.0001(16) C23 0.100(3) 0.053(2) 0.067(2) 0.0061(18) -0.001(2) 0.006(2) C24 0.130(4) 0.067(3) 0.050(2) -0.0044(19) -0.024(2) 0.032(3) C25 0.114(4) 0.080(3) 0.075(3) -0.026(2) -0.057(3) 0.018(3) C26 0.080(2) 0.057(2) 0.063(2) -0.0092(17) -0.0358(19) -0.0033(18) C31 0.0393(15) 0.0398(15) 0.0518(17) -0.0036(13) -0.0019(13) -0.0075(12) C32 0.065(2) 0.055(2) 0.061(2) -0.0038(16) -0.0180(17) -0.0010(16) C33 0.075(3) 0.067(2) 0.101(3) 0.011(2) -0.040(2) 0.005(2) C34 0.058(2) 0.052(2) 0.136(4) 0.001(3) -0.007(3) 0.0114(18) C35 0.069(3) 0.048(2) 0.104(3) -0.011(2) 0.020(2) 0.0017(18) C36 0.061(2) 0.0481(18) 0.059(2) -0.0044(15) 0.0049(16) -0.0048(15) C41 0.154(6) 0.083(4) 0.146(5) 0.001(3) -0.031(4) -0.022(4) Cl2 0.115(2) 0.097(2) 0.109(3) 0.0103(18) -0.047(2) -0.0239(19) Cl3 0.090(3) 0.192(5) 0.416(10) -0.109(6) -0.044(4) 0.020(3) Cl2' 0.345(11) 0.162(5) 0.188(6) -0.020(4) -0.083(7) -0.107(7) Cl3' 0.126(3) 0.179(4) 0.156(3) 0.026(3) -0.037(2) -0.062(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 Pd C1 1.983(3) . ? Pd P1 2.2494(7) . ? Pd N1 2.284(2) . ? Pd Cl 2.3778(7) . ? P1 C11 1.821(3) . ? P1 C21 1.824(3) . ? P1 C3 1.829(3) . ? O1 C1 1.198(4) . ? N1 C10 1.283(3) . ? N1 C8 1.444(3) . ? C1 C2 1.508(5) . ? C3 C4 1.400(4) . ? C3 C8 1.403(4) . ? C4 C5 1.384(4) . ? C5 C6 1.382(4) . ? C6 C7 1.391(4) . ? C7 C8 1.391(4) . ? C10 C31 1.465(4) . ? C11 C12 1.369(5) . ? C11 C16 1.376(4) . ? C12 C13 1.393(6) . ? C13 C14 1.358(7) . ? C14 C15 1.335(7) . ? C15 C16 1.381(5) . ? C21 C26 1.378(4) . ? C21 C22 1.391(4) . ? C22 C23 1.381(5) . ? C23 C24 1.361(6) . ? C24 C25 1.371(6) . ? C25 C26 1.400(5) . ? C31 C36 1.389(4) . ? C31 C32 1.396(4) . ? C32 C33 1.388(5) . ? C33 C34 1.361(6) . ? C34 C35 1.381(6) . ? C35 C36 1.383(5) . ? C41 Cl3 1.554(7) . ? C41 Cl2' 1.578(9) . ? C41 Cl2 1.789(8) . ? C41 Cl3' 1.831(7) . ? Cl3' Cl3' 2.434(8) 2_877 ? 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 Pd P1 97.48(9) . . ? C1 Pd N1 176.16(11) . . ? P1 Pd N1 78.89(6) . . ? C1 Pd Cl 85.93(9) . . ? P1 Pd Cl 169.78(3) . . ? N1 Pd Cl 97.86(6) . . ? C11 P1 C21 105.67(13) . . ? C11 P1 C3 106.72(13) . . ? C21 P1 C3 102.96(12) . . ? C11 P1 Pd 116.12(9) . . ? C21 P1 Pd 123.47(11) . . ? C3 P1 Pd 99.67(9) . . ? C10 N1 C8 118.0(2) . . ? C10 N1 Pd 132.19(19) . . ? C8 N1 Pd 109.72(16) . . ? O1 C1 C2 122.7(3) . . ? O1 C1 Pd 124.2(3) . . ? C2 C1 Pd 113.0(3) . . ? C4 C3 C8 119.5(2) . . ? C4 C3 P1 123.8(2) . . ? C8 C3 P1 116.60(19) . . ? C5 C4 C3 120.1(3) . . ? C6 C5 C4 120.1(3) . . ? C5 C6 C7 120.8(3) . . ? C8 C7 C6 119.6(3) . . ? C7 C8 C3 120.0(2) . . ? C7 C8 N1 124.0(2) . . ? C3 C8 N1 116.1(2) . . ? N1 C10 C31 125.9(3) . . ? C12 C11 C16 117.9(3) . . ? C12 C11 P1 122.9(3) . . ? C16 C11 P1 119.2(2) . . ? C11 C12 C13 120.0(4) . . ? C14 C13 C12 120.8(4) . . ? C15 C14 C13 119.5(4) . . ? C14 C15 C16 120.8(4) . . ? C11 C16 C15 121.0(4) . . ? C26 C21 C22 119.8(3) . . ? C26 C21 P1 122.7(2) . . ? C22 C21 P1 117.5(2) . . ? C23 C22 C21 119.9(4) . . ? C24 C23 C22 120.5(4) . . ? C23 C24 C25 120.2(4) . . ? C24 C25 C26 120.3(4) . . ? C21 C26 C25 119.2(4) . . ? C36 C31 C32 118.6(3) . . ? C36 C31 C10 123.2(3) . . ? C32 C31 C10 117.9(3) . . ? C33 C32 C31 120.1(4) . . ? C34 C33 C32 120.5(4) . . ? C33 C34 C35 120.2(4) . . ? C34 C35 C36 120.1(4) . . ? C35 C36 C31 120.4(4) . . ? Cl3 C41 Cl2' 83.9(5) . . ? Cl3 C41 Cl2 110.3(4) . . ? Cl2' C41 Cl2 29.8(4) . . ? Cl3 C41 Cl3' 56.4(4) . . ? Cl2' C41 Cl3' 110.5(4) . . ? Cl2 C41 Cl3' 113.4(3) . . ? C41 Cl3' Cl3' 169.4(5) . 2_877 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.469 _refine_diff_density_min -0.520 _refine_diff_density_rms 0.068 data_ic5428 _database_code_CSD 172820 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H25 Cl N O P Pd' _chemical_formula_weight 540.29 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' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pd' 'Pd' -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.9142(2) _cell_length_b 10.3657(2) _cell_length_c 14.4963(3) _cell_angle_alpha 103.0520(10) _cell_angle_beta 101.3450(10) _cell_angle_gamma 92.2640(10) _cell_volume 1274.43(5) _cell_formula_units_Z 2 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 8960 _cell_measurement_theta_min 1.48 _cell_measurement_theta_max 27.50 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas not_measured _exptl_crystal_density_diffrn 1.408 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 548 _exptl_absorpt_coefficient_mu 0.913 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7261 _exptl_absorpt_correction_T_max 0.8620 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16566 _diffrn_reflns_av_R_equivalents 0.0472 _diffrn_reflns_av_sigmaI/netI 0.0588 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.48 _diffrn_reflns_theta_max 27.50 _reflns_number_total 5854 _reflns_number_gt 4528 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0532P)^2^+0.7492P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5854 _refine_ls_number_parameters 289 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0761 _refine_ls_R_factor_gt 0.0503 _refine_ls_wR_factor_ref 0.1233 _refine_ls_wR_factor_gt 0.1119 _refine_ls_goodness_of_fit_ref 1.137 _refine_ls_restrained_S_all 1.137 _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 Pd Pd 0.80527(4) 0.98873(3) 0.70750(2) 0.03229(11) Uani 1 1 d . . . Cl Cl 0.97524(17) 1.16609(13) 0.81391(9) 0.0617(4) Uani 1 1 d . . . P1 P 0.67083(12) 0.80819(10) 0.61351(8) 0.0321(2) Uani 1 1 d . . . N1 N 0.7687(4) 0.9031(3) 0.8262(2) 0.0377(8) Uani 1 1 d . . . C1 C 0.8320(6) 1.0691(4) 0.5950(3) 0.0458(11) Uani 1 1 d . . . H1A H 0.7715 1.0148 0.5356 0.069 Uiso 1 1 calc R . . H1B H 0.9382 1.0730 0.5911 0.069 Uiso 1 1 calc R . . H1C H 0.7987 1.1572 0.6053 0.069 Uiso 1 1 calc R . . C3 C 0.7693(4) 0.6715(4) 0.6528(3) 0.0361(9) Uani 1 1 d . . . C4 C 0.8012(5) 0.5638(4) 0.5860(4) 0.0446(10) Uani 1 1 d . . . H4A H 0.7710 0.5599 0.5202 0.054 Uiso 1 1 calc R . . C5 C 0.8781(6) 0.4609(5) 0.6159(4) 0.0574(13) Uani 1 1 d . . . H5A H 0.9005 0.3896 0.5704 0.069 Uiso 1 1 calc R . . C6 C 0.9206(6) 0.4656(5) 0.7137(5) 0.0635(15) Uani 1 1 d . . . H6A H 0.9728 0.3979 0.7344 0.076 Uiso 1 1 calc R . . C7 C 0.8859(6) 0.5698(5) 0.7796(4) 0.0579(13) Uani 1 1 d . . . H7A H 0.9108 0.5701 0.8451 0.069 Uiso 1 1 calc R . . C8 C 0.8138(5) 0.6764(4) 0.7517(3) 0.0416(10) Uani 1 1 d . . . C10 C 0.7822(5) 0.7820(5) 0.8298(3) 0.0456(11) Uani 1 1 d . . . H10A H 0.7710 0.7590 0.8866 0.055 Uiso 1 1 calc R . . C11 C 0.4793(4) 0.7872(4) 0.6361(3) 0.0327(8) Uani 1 1 d . . . C12 C 0.4194(5) 0.6670(5) 0.6467(3) 0.0472(11) Uani 1 1 d . . . H12A H 0.4782 0.5946 0.6427 0.057 Uiso 1 1 calc R . . C13 C 0.2719(6) 0.6547(5) 0.6631(4) 0.0579(13) Uani 1 1 d . . . H13A H 0.2322 0.5744 0.6709 0.070 Uiso 1 1 calc R . . C14 C 0.1852(5) 0.7610(6) 0.6679(3) 0.0572(14) Uani 1 1 d . . . H14A H 0.0858 0.7523 0.6780 0.069 Uiso 1 1 calc R . . C15 C 0.2440(5) 0.8813(5) 0.6579(3) 0.0508(12) Uani 1 1 d . . . H15A H 0.1848 0.9534 0.6617 0.061 Uiso 1 1 calc R . . C16 C 0.3904(5) 0.8935(5) 0.6424(3) 0.0415(10) Uani 1 1 d . . . H16A H 0.4301 0.9746 0.6361 0.050 Uiso 1 1 calc R . . C21 C 0.6449(5) 0.7673(4) 0.4822(3) 0.0356(9) Uani 1 1 d . . . C22 C 0.7732(5) 0.7781(5) 0.4413(3) 0.0457(11) Uani 1 1 d . . . H22A H 0.8699 0.8044 0.4810 0.055 Uiso 1 1 calc R . . C23 C 0.7558(6) 0.7495(5) 0.3417(4) 0.0556(13) Uani 1 1 d . . . H23A H 0.8412 0.7549 0.3143 0.067 Uiso 1 1 calc R . . C24 C 0.6120(7) 0.7131(6) 0.2830(4) 0.0629(15) Uani 1 1 d . . . H24A H 0.6005 0.6953 0.2161 0.075 Uiso 1 1 calc R . . C25 C 0.4869(7) 0.7029(6) 0.3223(4) 0.0632(14) Uani 1 1 d . . . H25A H 0.3903 0.6779 0.2821 0.076 Uiso 1 1 calc R . . C26 C 0.5023(5) 0.7295(5) 0.4220(3) 0.0456(11) Uani 1 1 d . . . H26A H 0.4162 0.7219 0.4483 0.055 Uiso 1 1 calc R . . C31 C 0.7336(6) 0.9918(5) 0.9086(3) 0.0458(11) Uani 1 1 d . . . C32 C 0.6251(7) 1.0792(6) 0.8924(4) 0.0687(16) Uani 1 1 d . . . H32A H 0.5796 1.0821 0.8295 0.082 Uiso 1 1 calc R . . C33 C 0.5837(9) 1.1634(7) 0.9713(5) 0.087(2) Uani 1 1 d . . . H33A H 0.5081 1.2210 0.9610 0.105 Uiso 1 1 calc R . . C34 C 0.6545(9) 1.1615(8) 1.0638(5) 0.093(2) Uani 1 1 d . . . H34A H 0.6270 1.2182 1.1162 0.112 Uiso 1 1 calc R . . C35 C 0.7651(8) 1.0768(7) 1.0795(4) 0.0777(18) Uani 1 1 d . . . H35A H 0.8144 1.0775 1.1424 0.093 Uiso 1 1 calc R . . C36 C 0.8040(6) 0.9899(6) 1.0020(4) 0.0588(13) Uani 1 1 d . . . H36A H 0.8771 0.9304 1.0128 0.071 Uiso 1 1 calc R . . O1 O 0.8768(17) 0.3885(11) 0.9819(8) 0.140(5) Uani 0.510(12) 1 d P A 1 H1 H 0.7967 0.3792 0.9266 0.210 Uiso 0.51 1 d P A 1 H1' H 0.9400 0.4602 0.9979 0.210 Uiso 0.51 1 d P A 1 O2 O 0.7527(15) 0.6253(13) 1.0309(10) 0.146(5) Uani 0.490(12) 1 d P A 2 H2 H 0.7481 0.5641 1.0605 0.219 Uiso 0.49 1 d P A 2 H2' H 0.8148 0.5911 1.0057 0.219 Uiso 0.49 1 d P A 2 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 Pd 0.03707(18) 0.03205(18) 0.02971(17) 0.01103(12) 0.00773(12) 0.00185(12) Cl 0.0837(9) 0.0506(7) 0.0434(7) 0.0132(6) -0.0008(6) -0.0224(7) P1 0.0310(5) 0.0330(5) 0.0346(6) 0.0105(4) 0.0098(4) 0.0031(4) N1 0.0416(19) 0.041(2) 0.0329(18) 0.0123(15) 0.0104(15) 0.0050(16) C1 0.056(3) 0.040(2) 0.044(3) 0.020(2) 0.006(2) -0.005(2) C3 0.032(2) 0.035(2) 0.043(2) 0.0117(18) 0.0094(18) 0.0015(17) C4 0.046(3) 0.035(2) 0.053(3) 0.009(2) 0.013(2) 0.0017(19) C5 0.057(3) 0.036(3) 0.085(4) 0.015(3) 0.027(3) 0.015(2) C6 0.063(3) 0.049(3) 0.088(4) 0.033(3) 0.016(3) 0.022(3) C7 0.070(3) 0.052(3) 0.061(3) 0.030(3) 0.016(3) 0.018(3) C8 0.040(2) 0.041(2) 0.054(3) 0.025(2) 0.015(2) 0.0060(19) C10 0.054(3) 0.052(3) 0.038(2) 0.023(2) 0.013(2) 0.008(2) C11 0.033(2) 0.037(2) 0.0273(19) 0.0054(16) 0.0090(16) 0.0002(17) C12 0.044(3) 0.045(3) 0.053(3) 0.008(2) 0.018(2) -0.002(2) C13 0.060(3) 0.055(3) 0.060(3) 0.009(3) 0.024(3) -0.014(3) C14 0.036(2) 0.090(4) 0.043(3) 0.006(3) 0.016(2) -0.003(3) C15 0.038(2) 0.073(4) 0.046(3) 0.017(2) 0.014(2) 0.016(2) C16 0.041(2) 0.048(3) 0.041(2) 0.018(2) 0.0120(19) 0.0084(19) C21 0.040(2) 0.036(2) 0.033(2) 0.0084(17) 0.0117(18) 0.0035(18) C22 0.043(2) 0.049(3) 0.049(3) 0.012(2) 0.017(2) 0.006(2) C23 0.066(3) 0.061(3) 0.051(3) 0.014(2) 0.033(3) 0.014(3) C24 0.089(4) 0.064(3) 0.038(3) 0.010(2) 0.020(3) 0.012(3) C25 0.062(3) 0.082(4) 0.041(3) 0.011(3) 0.006(2) -0.002(3) C26 0.049(3) 0.054(3) 0.034(2) 0.009(2) 0.011(2) 0.001(2) C31 0.057(3) 0.052(3) 0.033(2) 0.015(2) 0.016(2) 0.004(2) C32 0.084(4) 0.076(4) 0.045(3) 0.009(3) 0.011(3) 0.034(3) C33 0.109(5) 0.090(5) 0.073(4) 0.017(4) 0.038(4) 0.050(4) C34 0.126(6) 0.102(5) 0.053(4) -0.001(4) 0.040(4) 0.027(5) C35 0.102(5) 0.094(5) 0.037(3) 0.008(3) 0.021(3) 0.018(4) C36 0.067(3) 0.072(4) 0.042(3) 0.018(3) 0.015(2) 0.009(3) O1 0.231(14) 0.082(7) 0.093(8) -0.033(6) 0.067(9) -0.021(8) O2 0.133(10) 0.137(11) 0.136(11) -0.007(9) 0.002(8) -0.010(8) _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 Pd C1 2.040(4) . ? Pd N1 2.177(3) . ? Pd P1 2.1963(11) . ? Pd Cl 2.3737(12) . ? P1 C11 1.815(4) . ? P1 C21 1.820(4) . ? P1 C3 1.835(4) . ? N1 C10 1.277(5) . ? N1 C31 1.430(6) . ? C3 C4 1.382(6) . ? C3 C8 1.399(6) . ? C4 C5 1.395(6) . ? C5 C6 1.383(8) . ? C6 C7 1.361(7) . ? C7 C8 1.397(6) . ? C8 C10 1.466(6) . ? C11 C16 1.380(6) . ? C11 C12 1.388(6) . ? C12 C13 1.388(7) . ? C13 C14 1.368(8) . ? C14 C15 1.381(7) . ? C15 C16 1.373(6) . ? C21 C26 1.379(6) . ? C21 C22 1.399(6) . ? C22 C23 1.383(7) . ? C23 C24 1.377(8) . ? C24 C25 1.359(8) . ? C25 C26 1.386(6) . ? C31 C32 1.374(7) . ? C31 C36 1.381(7) . ? C32 C33 1.395(8) . ? C33 C34 1.371(9) . ? C34 C35 1.366(9) . ? C35 C36 1.383(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Pd N1 178.14(16) . . ? C1 Pd P1 94.07(13) . . ? N1 Pd P1 85.03(10) . . ? C1 Pd Cl 88.71(13) . . ? N1 Pd Cl 92.37(10) . . ? P1 Pd Cl 172.74(5) . . ? C11 P1 C21 105.00(19) . . ? C11 P1 C3 104.33(19) . . ? C21 P1 C3 105.35(19) . . ? C11 P1 Pd 113.07(13) . . ? C21 P1 Pd 123.07(14) . . ? C3 P1 Pd 104.30(14) . . ? C10 N1 C31 117.6(4) . . ? C10 N1 Pd 125.5(3) . . ? C31 N1 Pd 116.9(3) . . ? C4 C3 C8 119.3(4) . . ? C4 C3 P1 120.9(3) . . ? C8 C3 P1 119.7(3) . . ? C3 C4 C5 120.9(5) . . ? C6 C5 C4 119.5(5) . . ? C7 C6 C5 119.7(5) . . ? C6 C7 C8 121.8(5) . . ? C7 C8 C3 118.6(4) . . ? C7 C8 C10 116.4(4) . . ? C3 C8 C10 124.9(4) . . ? N1 C10 C8 125.4(4) . . ? C16 C11 C12 119.1(4) . . ? C16 C11 P1 119.0(3) . . ? C12 C11 P1 121.9(3) . . ? C13 C12 C11 120.1(5) . . ? C14 C13 C12 119.7(5) . . ? C13 C14 C15 120.6(4) . . ? C16 C15 C14 119.6(5) . . ? C15 C16 C11 120.9(4) . . ? C26 C21 C22 119.1(4) . . ? C26 C21 P1 122.0(3) . . ? C22 C21 P1 118.9(3) . . ? C23 C22 C21 119.9(5) . . ? C24 C23 C22 120.0(5) . . ? C25 C24 C23 120.4(5) . . ? C24 C25 C26 120.4(5) . . ? C21 C26 C25 120.2(4) . . ? C32 C31 C36 120.3(5) . . ? C32 C31 N1 117.9(4) . . ? C36 C31 N1 121.8(4) . . ? C31 C32 C33 119.3(5) . . ? C34 C33 C32 120.1(6) . . ? C35 C34 C33 120.3(6) . . ? C34 C35 C36 120.2(6) . . ? C31 C36 C35 119.7(5) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.830 _refine_diff_density_min -0.850 _refine_diff_density_rms 0.120 data_ic5520 _database_code_CSD 172821 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C19 H19 Cl N P Pd' _chemical_formula_weight 434.17 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' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pd' 'Pd' -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.6838(3) _cell_length_b 9.8823(3) _cell_length_c 10.5044(3) _cell_angle_alpha 81.180(1) _cell_angle_beta 89.079(1) _cell_angle_gamma 65.848(1) _cell_volume 905.20(5) _cell_formula_units_Z 2 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 6151 _cell_measurement_theta_min 1.96 _cell_measurement_theta_max 27.50 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas not_measured _exptl_crystal_density_diffrn 1.593 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 436 _exptl_absorpt_coefficient_mu 1.259 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6740 _exptl_absorpt_correction_T_max 0.8017 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9868 _diffrn_reflns_av_R_equivalents 0.0270 _diffrn_reflns_av_sigmaI/netI 0.0343 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.96 _diffrn_reflns_theta_max 27.50 _reflns_number_total 4121 _reflns_number_gt 3586 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0246P)^2^+0.2566P] 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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0025(6) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 4121 _refine_ls_number_parameters 210 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0349 _refine_ls_R_factor_gt 0.0263 _refine_ls_wR_factor_ref 0.0621 _refine_ls_wR_factor_gt 0.0589 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.051 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd Pd 1.218506(18) 0.058192(19) 1.154995(17) 0.03299(7) Uani 1 1 d . . . Cl Cl 1.26073(8) -0.11729(8) 1.01156(7) 0.05375(17) Uani 1 1 d . . . N1 N 1.0183(2) 0.2209(2) 1.04063(18) 0.0384(4) Uani 1 1 d . . . H1D H 1.0463 0.2454 0.9614 0.046 Uiso 1 1 calc R . . H1E H 0.9546 0.1770 1.0317 0.046 Uiso 1 1 calc R . . C1 C 1.4066(3) -0.0866(3) 1.2665(3) 0.0578(7) Uani 1 1 d . . . H1A H 1.4144 -0.1873 1.2718 0.087 Uiso 1 1 calc R . . H1B H 1.3990 -0.0605 1.3515 0.087 Uiso 1 1 calc R . . H1C H 1.4950 -0.0801 1.2287 0.087 Uiso 1 1 calc R . . P1 P 1.16798(6) 0.22723(7) 1.28151(6) 0.03229(13) Uani 1 1 d . . . C3 C 0.9966(2) 0.3811(3) 1.2034(2) 0.0343(5) Uani 1 1 d . . . C4 C 0.9201(3) 0.5149(3) 1.2521(3) 0.0464(6) Uani 1 1 d . . . H4A H 0.9613 0.5329 1.3237 0.056 Uiso 1 1 calc R . . C5 C 0.7841(3) 0.6203(3) 1.1946(3) 0.0521(7) Uani 1 1 d . . . H5A H 0.7334 0.7088 1.2279 0.062 Uiso 1 1 calc R . . C6 C 0.7228(3) 0.5951(3) 1.0876(3) 0.0515(7) Uani 1 1 d . . . H6A H 0.6298 0.6656 1.0502 0.062 Uiso 1 1 calc R . . C7 C 0.7991(3) 0.4656(3) 1.0360(2) 0.0438(6) Uani 1 1 d . . . H7A H 0.7587 0.4499 0.9628 0.053 Uiso 1 1 calc R . . C8 C 0.9364(2) 0.3586(3) 1.0936(2) 0.0341(5) Uani 1 1 d . . . C11 C 1.1152(2) 0.1837(3) 1.4445(2) 0.0359(5) Uani 1 1 d . . . C12 C 0.9672(3) 0.2046(3) 1.4697(3) 0.0473(6) Uani 1 1 d . . . H12A H 0.8919 0.2479 1.4037 0.057 Uiso 1 1 calc R . . C13 C 0.9320(3) 0.1611(3) 1.5930(3) 0.0599(8) Uani 1 1 d . . . H13A H 0.8326 0.1760 1.6095 0.072 Uiso 1 1 calc R . . C14 C 1.0417(4) 0.0965(3) 1.6907(3) 0.0575(7) Uani 1 1 d . . . H14A H 1.0165 0.0688 1.7735 0.069 Uiso 1 1 calc R . . C15 C 1.1876(4) 0.0727(3) 1.6669(3) 0.0593(8) Uani 1 1 d . . . H15A H 1.2626 0.0267 1.7330 0.071 Uiso 1 1 calc R . . C16 C 1.2248(3) 0.1170(3) 1.5443(2) 0.0508(6) Uani 1 1 d . . . H16A H 1.3246 0.1017 1.5290 0.061 Uiso 1 1 calc R . . C21 C 1.3048(2) 0.3062(3) 1.3005(2) 0.0350(5) Uani 1 1 d . . . C22 C 1.2823(3) 0.4115(3) 1.3815(3) 0.0538(7) Uani 1 1 d . . . H22A H 1.1998 0.4369 1.4336 0.065 Uiso 1 1 calc R . . C23 C 1.3818(3) 0.4782(4) 1.3848(4) 0.0682(9) Uani 1 1 d . . . H23A H 1.3662 0.5488 1.4390 0.082 Uiso 1 1 calc R . . C24 C 1.5047(3) 0.4409(4) 1.3082(3) 0.0645(8) Uani 1 1 d . . . H24A H 1.5702 0.4883 1.3091 0.077 Uiso 1 1 calc R . . C25 C 1.5305(3) 0.3346(3) 1.2310(3) 0.0531(7) Uani 1 1 d . . . H25A H 1.6150 0.3078 1.1812 0.064 Uiso 1 1 calc R . . C26 C 1.4312(3) 0.2667(3) 1.2268(2) 0.0405(5) Uani 1 1 d . . . H26A H 1.4495 0.1941 1.1742 0.049 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 Pd 0.02744(10) 0.03364(11) 0.03960(11) -0.01464(7) 0.00480(6) -0.01138(7) Cl 0.0496(4) 0.0550(4) 0.0617(4) -0.0344(3) 0.0077(3) -0.0181(3) N1 0.0398(10) 0.0422(11) 0.0367(10) -0.0115(9) 0.0016(8) -0.0186(9) C1 0.0404(14) 0.0461(16) 0.0758(19) -0.0199(14) -0.0095(13) -0.0027(12) P1 0.0259(3) 0.0347(3) 0.0365(3) -0.0128(2) 0.0023(2) -0.0104(2) C3 0.0289(10) 0.0330(12) 0.0408(12) -0.0085(9) 0.0044(9) -0.0118(9) C4 0.0451(14) 0.0402(14) 0.0508(15) -0.0159(11) 0.0008(11) -0.0115(11) C5 0.0469(15) 0.0343(13) 0.0633(17) -0.0104(12) 0.0051(13) -0.0041(12) C6 0.0393(13) 0.0405(14) 0.0584(16) 0.0020(12) -0.0015(12) -0.0034(11) C7 0.0390(13) 0.0456(14) 0.0430(13) 0.0004(11) -0.0048(10) -0.0162(11) C8 0.0320(11) 0.0340(12) 0.0383(12) -0.0047(9) 0.0051(9) -0.0162(10) C11 0.0342(11) 0.0340(12) 0.0396(12) -0.0125(10) 0.0052(9) -0.0120(10) C12 0.0369(13) 0.0461(15) 0.0569(16) -0.0058(12) 0.0060(11) -0.0160(11) C13 0.0550(17) 0.0541(17) 0.074(2) -0.0104(15) 0.0264(15) -0.0268(14) C14 0.082(2) 0.0517(17) 0.0476(15) -0.0127(13) 0.0199(15) -0.0348(16) C15 0.074(2) 0.0642(19) 0.0425(15) -0.0030(13) -0.0038(14) -0.0329(17) C16 0.0437(14) 0.0623(18) 0.0460(14) -0.0083(13) 0.0016(11) -0.0215(13) C21 0.0300(11) 0.0389(12) 0.0381(12) -0.0121(10) 0.0038(9) -0.0144(10) C22 0.0417(14) 0.0681(19) 0.0660(17) -0.0408(15) 0.0175(13) -0.0273(14) C23 0.0575(18) 0.072(2) 0.099(2) -0.0533(19) 0.0175(17) -0.0374(17) C24 0.0535(17) 0.070(2) 0.093(2) -0.0296(18) 0.0168(16) -0.0432(16) C25 0.0441(14) 0.0654(18) 0.0612(17) -0.0220(14) 0.0191(13) -0.0303(14) C26 0.0372(12) 0.0438(14) 0.0418(13) -0.0137(11) 0.0065(10) -0.0158(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 Pd C1 2.039(3) . ? Pd N1 2.1724(19) . ? Pd P1 2.1880(6) . ? Pd Cl 2.3761(6) . ? N1 C8 1.458(3) . ? P1 C11 1.818(2) . ? P1 C21 1.818(2) . ? P1 C3 1.826(2) . ? C3 C8 1.387(3) . ? C3 C4 1.398(3) . ? C4 C5 1.376(4) . ? C5 C6 1.381(4) . ? C6 C7 1.379(4) . ? C7 C8 1.390(3) . ? C11 C16 1.383(3) . ? C11 C12 1.388(3) . ? C12 C13 1.383(4) . ? C13 C14 1.367(4) . ? C14 C15 1.360(4) . ? C15 C16 1.386(4) . ? C21 C26 1.387(3) . ? C21 C22 1.391(3) . ? C22 C23 1.376(4) . ? C23 C24 1.379(4) . ? C24 C25 1.365(4) . ? C25 C26 1.384(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Pd N1 177.31(9) . . ? C1 Pd P1 92.00(8) . . ? N1 Pd P1 85.43(5) . . ? C1 Pd Cl 91.03(8) . . ? N1 Pd Cl 91.54(5) . . ? P1 Pd Cl 176.94(2) . . ? C8 N1 Pd 115.04(14) . . ? C11 P1 C21 104.76(11) . . ? C11 P1 C3 104.36(10) . . ? C21 P1 C3 106.72(11) . . ? C11 P1 Pd 118.05(8) . . ? C21 P1 Pd 118.63(7) . . ? C3 P1 Pd 102.91(8) . . ? C8 C3 C4 119.1(2) . . ? C8 C3 P1 117.30(17) . . ? C4 C3 P1 123.53(19) . . ? C5 C4 C3 120.3(3) . . ? C4 C5 C6 120.2(2) . . ? C7 C6 C5 120.2(2) . . ? C6 C7 C8 119.9(2) . . ? C3 C8 C7 120.2(2) . . ? C3 C8 N1 119.11(19) . . ? C7 C8 N1 120.7(2) . . ? C16 C11 C12 118.5(2) . . ? C16 C11 P1 120.24(18) . . ? C12 C11 P1 121.01(19) . . ? C13 C12 C11 119.9(3) . . ? C14 C13 C12 120.7(3) . . ? C15 C14 C13 120.0(3) . . ? C14 C15 C16 120.1(3) . . ? C11 C16 C15 120.7(3) . . ? C26 C21 C22 118.9(2) . . ? C26 C21 P1 119.08(18) . . ? C22 C21 P1 121.97(18) . . ? C23 C22 C21 120.2(2) . . ? C22 C23 C24 120.3(3) . . ? C25 C24 C23 120.1(3) . . ? C24 C25 C26 120.2(2) . . ? C25 C26 C21 120.3(2) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.369 _refine_diff_density_min -0.485 _refine_diff_density_rms 0.082 data_ic5595 _database_code_CSD 172822 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C37 H34 B F4 N P2 Pd' _chemical_formula_weight 747.80 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' '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 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 16.6481(2) _cell_length_b 10.6638(1) _cell_length_c 19.8024(2) _cell_angle_alpha 90.00 _cell_angle_beta 101.990(1) _cell_angle_gamma 90.00 _cell_volume 3438.86(6) _cell_formula_units_Z 4 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 7578 _cell_measurement_theta_min 1.46 _cell_measurement_theta_max 27.50 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas not_measured _exptl_crystal_density_diffrn 1.444 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1520 _exptl_absorpt_coefficient_mu 0.681 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5516 _exptl_absorpt_correction_T_max 0.6948 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23327 _diffrn_reflns_av_R_equivalents 0.0262 _diffrn_reflns_av_sigmaI/netI 0.0295 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.46 _diffrn_reflns_theta_max 27.50 _reflns_number_total 7866 _reflns_number_gt 6253 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0340P)^2^+2.0124P] 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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00087(13) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 7866 _refine_ls_number_parameters 417 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0478 _refine_ls_R_factor_gt 0.0333 _refine_ls_wR_factor_ref 0.0860 _refine_ls_wR_factor_gt 0.0783 _refine_ls_goodness_of_fit_ref 1.062 _refine_ls_restrained_S_all 1.062 _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 Pd Pd -0.071848(10) 0.163142(17) 0.165268(8) 0.03504(7) Uani 1 1 d . . . P1 P -0.15092(4) 0.16777(6) 0.05674(3) 0.03682(13) Uani 1 1 d . . . P2 P 0.01489(3) 0.16297(6) 0.27345(3) 0.03574(13) Uani 1 1 d . . . N1 N -0.17807(12) 0.2489(2) 0.19348(10) 0.0467(5) Uani 1 1 d . . . H1D H -0.1928 0.2018 0.2266 0.056 Uiso 1 1 calc R . . H1E H -0.1632 0.3247 0.2120 0.056 Uiso 1 1 calc R . . C1 C 0.02353(16) 0.0899(3) 0.12683(14) 0.0600(8) Uani 1 1 d . . . H1A H 0.0646 0.0576 0.1641 0.090 Uiso 1 1 calc R . . H1B H 0.0471 0.1544 0.1032 0.090 Uiso 1 1 calc R . . H1C H 0.0035 0.0233 0.0951 0.090 Uiso 1 1 calc R . . C3 C -0.24712(14) 0.2312(2) 0.07060(12) 0.0420(5) Uani 1 1 d . . . C4 C -0.31693(16) 0.2436(3) 0.01839(14) 0.0595(8) Uani 1 1 d . . . H4A H -0.3156 0.2185 -0.0264 0.071 Uiso 1 1 calc R . . C5 C -0.38785(17) 0.2927(4) 0.03287(16) 0.0662(9) Uani 1 1 d . . . H5A H -0.4345 0.3007 -0.0020 0.079 Uiso 1 1 calc R . . C6 C -0.38955(17) 0.3298(3) 0.09909(17) 0.0660(9) Uani 1 1 d . . . H6A H -0.4372 0.3650 0.1084 0.079 Uiso 1 1 calc R . . C7 C -0.32160(16) 0.3156(3) 0.15185(15) 0.0582(7) Uani 1 1 d . . . H7A H -0.3237 0.3394 0.1966 0.070 Uiso 1 1 calc R . . C8 C -0.25027(14) 0.2654(2) 0.13751(12) 0.0419(5) Uani 1 1 d . . . C11 C -0.17596(14) 0.0219(2) 0.00989(12) 0.0406(5) Uani 1 1 d . . . C12 C -0.16507(16) -0.0904(3) 0.04576(14) 0.0500(6) Uani 1 1 d . . . H12A H -0.1449 -0.0906 0.0932 0.060 Uiso 1 1 calc R . . C13 C -0.18449(18) -0.2029(3) 0.01049(17) 0.0590(7) Uani 1 1 d . . . H13A H -0.1775 -0.2785 0.0344 0.071 Uiso 1 1 calc R . . C14 C -0.21391(17) -0.2022(3) -0.05946(17) 0.0588(7) Uani 1 1 d . . . H14A H -0.2257 -0.2778 -0.0829 0.071 Uiso 1 1 calc R . . C15 C -0.22615(17) -0.0921(3) -0.09520(15) 0.0582(7) Uani 1 1 d . . . H15A H -0.2472 -0.0927 -0.1425 0.070 Uiso 1 1 calc R . . C16 C -0.20714(16) 0.0204(3) -0.06086(13) 0.0508(6) Uani 1 1 d . . . H16A H -0.2153 0.0955 -0.0853 0.061 Uiso 1 1 calc R . . C21 C -0.11486(14) 0.2708(2) -0.00366(11) 0.0387(5) Uani 1 1 d . . . C22 C -0.05876(16) 0.2254(3) -0.04080(13) 0.0484(6) Uani 1 1 d . . . H22A H -0.0440 0.1411 -0.0373 0.058 Uiso 1 1 calc R . . C23 C -0.02469(17) 0.3036(3) -0.08276(15) 0.0568(7) Uani 1 1 d . . . H23A H 0.0124 0.2718 -0.1076 0.068 Uiso 1 1 calc R . . C24 C -0.04535(19) 0.4277(3) -0.08783(16) 0.0643(8) Uani 1 1 d . . . H24A H -0.0224 0.4805 -0.1161 0.077 Uiso 1 1 calc R . . C25 C -0.1001(2) 0.4741(3) -0.05116(17) 0.0686(8) Uani 1 1 d . . . H25A H -0.1138 0.5588 -0.0546 0.082 Uiso 1 1 calc R . . C26 C -0.13529(18) 0.3970(3) -0.00904(14) 0.0536(7) Uani 1 1 d . . . H26A H -0.1725 0.4297 0.0155 0.064 Uiso 1 1 calc R . . C31 C 0.11286(14) 0.2376(2) 0.27105(12) 0.0404(5) Uani 1 1 d . . . C32 C 0.10986(19) 0.3487(3) 0.23450(17) 0.0671(9) Uani 1 1 d . . . H32A H 0.0593 0.3829 0.2141 0.081 Uiso 1 1 calc R . . C33 C 0.1814(2) 0.4094(4) 0.22787(18) 0.0765(10) Uani 1 1 d . . . H33A H 0.1785 0.4843 0.2034 0.092 Uiso 1 1 calc R . . C34 C 0.25641(19) 0.3597(3) 0.25715(17) 0.0641(8) Uani 1 1 d . . . H34A H 0.3044 0.4001 0.2522 0.077 Uiso 1 1 calc R . . C35 C 0.26016(16) 0.2513(3) 0.29337(17) 0.0623(8) Uani 1 1 d . . . H35A H 0.3110 0.2178 0.3137 0.075 Uiso 1 1 calc R . . C36 C 0.18874(15) 0.1892(3) 0.30055(15) 0.0501(6) Uani 1 1 d . . . H36A H 0.1923 0.1147 0.3254 0.060 Uiso 1 1 calc R . . C41 C -0.02543(14) 0.2482(3) 0.33897(12) 0.0428(5) Uani 1 1 d . . . C42 C -0.09260(17) 0.1974(3) 0.36076(14) 0.0572(7) Uani 1 1 d . . . H42A H -0.1116 0.1181 0.3457 0.069 Uiso 1 1 calc R . . C43 C -0.1317(2) 0.2645(4) 0.40509(17) 0.0763(10) Uani 1 1 d . . . H43A H -0.1764 0.2297 0.4196 0.092 Uiso 1 1 calc R . . C44 C -0.1045(3) 0.3808(5) 0.4273(2) 0.0923(13) Uani 1 1 d . . . H44A H -0.1313 0.4259 0.4562 0.111 Uiso 1 1 calc R . . C45 C -0.0381(3) 0.4311(4) 0.4071(2) 0.0931(12) Uani 1 1 d . . . H45A H -0.0192 0.5099 0.4231 0.112 Uiso 1 1 calc R . . C46 C 0.0017(2) 0.3656(3) 0.36283(17) 0.0680(8) Uani 1 1 d . . . H46A H 0.0468 0.4011 0.3492 0.082 Uiso 1 1 calc R . . C51 C 0.04060(13) 0.0084(2) 0.31049(13) 0.0420(5) Uani 1 1 d . . . C52 C 0.01607(16) -0.0984(3) 0.27126(15) 0.0531(7) Uani 1 1 d . . . H52A H -0.0147 -0.0908 0.2265 0.064 Uiso 1 1 calc R . . C53 C 0.0375(2) -0.2168(3) 0.2989(2) 0.0718(9) Uani 1 1 d . . . H53A H 0.0208 -0.2881 0.2728 0.086 Uiso 1 1 calc R . . C54 C 0.08266(19) -0.2279(4) 0.3640(2) 0.0777(11) Uani 1 1 d . . . H54A H 0.0979 -0.3072 0.3817 0.093 Uiso 1 1 calc R . . C55 C 0.10625(18) -0.1239(4) 0.40431(19) 0.0706(9) Uani 1 1 d . . . H55A H 0.1365 -0.1330 0.4491 0.085 Uiso 1 1 calc R . . C56 C 0.08478(15) -0.0054(3) 0.37780(14) 0.0543(7) Uani 1 1 d . . . H56A H 0.1000 0.0651 0.4051 0.065 Uiso 1 1 calc R . . B B -0.3392(3) 0.0930(4) 0.3146(2) 0.0679(10) Uani 1 1 d . . . F1 F -0.36724(16) 0.2126(2) 0.31570(13) 0.1050(7) Uani 1 1 d . . . F2 F -0.30269(19) 0.0577(2) 0.38111(12) 0.1181(9) Uani 1 1 d . . . F3 F -0.28083(17) 0.0864(3) 0.27609(13) 0.1248(10) Uani 1 1 d . . . F4 F -0.40092(19) 0.0151(3) 0.29037(19) 0.1499(12) 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 Pd 0.03067(10) 0.04349(11) 0.03071(10) -0.00197(8) 0.00580(6) 0.00509(7) P1 0.0345(3) 0.0457(3) 0.0303(3) -0.0021(3) 0.0070(2) 0.0064(3) P2 0.0305(3) 0.0420(3) 0.0335(3) 0.0018(3) 0.0041(2) 0.0010(2) N1 0.0436(11) 0.0605(14) 0.0365(10) -0.0038(10) 0.0094(9) 0.0113(10) C1 0.0428(14) 0.088(2) 0.0502(15) -0.0118(15) 0.0131(12) 0.0149(15) C3 0.0341(11) 0.0527(15) 0.0406(12) -0.0004(11) 0.0111(9) 0.0063(11) C4 0.0456(14) 0.089(2) 0.0416(14) 0.0029(15) 0.0050(11) 0.0119(15) C5 0.0367(14) 0.099(3) 0.0606(18) 0.0107(17) 0.0062(12) 0.0136(15) C6 0.0390(14) 0.092(2) 0.0707(19) 0.0069(18) 0.0203(13) 0.0165(15) C7 0.0452(14) 0.082(2) 0.0517(15) 0.0000(15) 0.0193(12) 0.0124(14) C8 0.0357(12) 0.0501(15) 0.0406(12) 0.0027(11) 0.0094(10) 0.0059(10) C11 0.0358(11) 0.0468(14) 0.0400(12) -0.0026(10) 0.0094(9) 0.0006(10) C12 0.0474(14) 0.0509(16) 0.0524(15) 0.0053(13) 0.0123(12) 0.0041(12) C13 0.0528(16) 0.0453(15) 0.081(2) 0.0041(15) 0.0173(15) -0.0026(13) C14 0.0441(15) 0.0556(17) 0.077(2) -0.0184(15) 0.0138(14) -0.0086(13) C15 0.0548(16) 0.0658(19) 0.0513(16) -0.0143(14) 0.0048(13) -0.0085(14) C16 0.0580(16) 0.0531(16) 0.0403(13) -0.0016(12) 0.0080(11) -0.0038(13) C21 0.0366(11) 0.0441(14) 0.0337(11) -0.0027(10) 0.0035(9) 0.0019(10) C22 0.0516(15) 0.0479(15) 0.0494(14) 0.0022(12) 0.0187(12) 0.0098(12) C23 0.0494(15) 0.073(2) 0.0514(15) 0.0068(14) 0.0179(12) 0.0033(14) C24 0.0641(18) 0.072(2) 0.0550(17) 0.0163(16) 0.0081(14) -0.0102(16) C25 0.088(2) 0.0451(17) 0.072(2) 0.0101(15) 0.0143(18) 0.0074(16) C26 0.0653(17) 0.0464(15) 0.0502(15) -0.0030(12) 0.0147(13) 0.0115(13) C31 0.0357(12) 0.0486(14) 0.0369(12) 0.0000(10) 0.0071(9) -0.0044(10) C32 0.0498(16) 0.075(2) 0.0696(19) 0.0297(17) -0.0039(14) -0.0092(15) C33 0.064(2) 0.081(2) 0.080(2) 0.0309(19) 0.0032(17) -0.0240(18) C34 0.0510(16) 0.074(2) 0.0683(19) -0.0038(16) 0.0157(14) -0.0245(15) C35 0.0347(13) 0.0643(19) 0.087(2) -0.0104(17) 0.0109(14) -0.0030(13) C36 0.0395(13) 0.0462(15) 0.0642(16) -0.0009(12) 0.0101(12) 0.0005(11) C41 0.0391(12) 0.0534(15) 0.0346(11) 0.0011(11) 0.0048(9) 0.0048(11) C42 0.0528(16) 0.0715(19) 0.0498(15) -0.0021(14) 0.0162(12) 0.0013(14) C43 0.0619(19) 0.113(3) 0.0606(19) -0.003(2) 0.0286(16) 0.011(2) C44 0.097(3) 0.111(3) 0.074(2) -0.028(2) 0.032(2) 0.020(3) C45 0.112(3) 0.083(3) 0.090(3) -0.034(2) 0.034(2) -0.003(2) C46 0.074(2) 0.066(2) 0.0654(19) -0.0147(16) 0.0181(16) -0.0068(16) C51 0.0296(11) 0.0464(14) 0.0497(13) 0.0069(11) 0.0080(10) 0.0029(10) C52 0.0467(14) 0.0511(17) 0.0626(17) 0.0042(13) 0.0140(12) -0.0007(12) C53 0.0626(19) 0.0477(18) 0.108(3) 0.0065(18) 0.0239(19) -0.0008(15) C54 0.0496(17) 0.064(2) 0.122(3) 0.036(2) 0.0219(19) 0.0114(16) C55 0.0443(16) 0.086(2) 0.078(2) 0.033(2) 0.0049(15) 0.0118(16) C56 0.0419(14) 0.0645(18) 0.0537(15) 0.0131(14) 0.0034(11) 0.0024(13) B 0.087(3) 0.056(2) 0.066(2) 0.0008(18) 0.030(2) 0.003(2) F1 0.135(2) 0.0726(14) 0.1042(17) 0.0027(13) 0.0184(15) 0.0254(14) F2 0.189(3) 0.0899(17) 0.0823(15) 0.0235(13) 0.0453(16) 0.0352(17) F3 0.121(2) 0.169(3) 0.0997(17) 0.0241(18) 0.0590(15) 0.0307(19) F4 0.132(2) 0.113(2) 0.200(3) -0.032(2) 0.024(2) -0.0469(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd C1 2.053(2) . ? Pd N1 2.1649(19) . ? Pd P1 2.2756(6) . ? Pd P2 2.3214(6) . ? P1 C3 1.811(2) . ? P1 C11 1.815(3) . ? P1 C21 1.816(2) . ? P2 C51 1.819(3) . ? P2 C41 1.823(2) . ? P2 C31 1.824(2) . ? N1 C8 1.466(3) . ? C3 C8 1.386(3) . ? C3 C4 1.392(3) . ? C4 C5 1.375(4) . ? C5 C6 1.376(4) . ? C6 C7 1.380(4) . ? C7 C8 1.385(3) . ? C11 C12 1.385(4) . ? C11 C16 1.389(3) . ? C12 C13 1.392(4) . ? C13 C14 1.370(4) . ? C14 C15 1.364(4) . ? C15 C16 1.383(4) . ? C21 C26 1.386(4) . ? C21 C22 1.390(3) . ? C22 C23 1.380(4) . ? C23 C24 1.365(4) . ? C24 C25 1.370(4) . ? C25 C26 1.385(4) . ? C31 C36 1.377(3) . ? C31 C32 1.383(4) . ? C32 C33 1.386(4) . ? C33 C34 1.369(5) . ? C34 C35 1.356(5) . ? C35 C36 1.394(4) . ? C41 C46 1.381(4) . ? C41 C42 1.389(4) . ? C42 C43 1.394(4) . ? C43 C44 1.361(6) . ? C44 C45 1.360(6) . ? C45 C46 1.392(5) . ? C51 C56 1.390(4) . ? C51 C52 1.392(4) . ? C52 C53 1.392(4) . ? C53 C54 1.356(5) . ? C54 C55 1.375(5) . ? C55 C56 1.387(4) . ? B F4 1.331(5) . ? B F3 1.357(4) . ? B F1 1.359(4) . ? B F2 1.383(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Pd N1 173.14(10) . . ? C1 Pd P1 89.90(8) . . ? N1 Pd P1 83.76(5) . . ? C1 Pd P2 87.77(8) . . ? N1 Pd P2 98.46(5) . . ? P1 Pd P2 176.76(2) . . ? C3 P1 C11 106.34(11) . . ? C3 P1 C21 107.30(11) . . ? C11 P1 C21 104.73(11) . . ? C3 P1 Pd 102.78(8) . . ? C11 P1 Pd 119.38(8) . . ? C21 P1 Pd 115.45(8) . . ? C51 P2 C41 104.79(12) . . ? C51 P2 C31 105.61(11) . . ? C41 P2 C31 105.34(12) . . ? C51 P2 Pd 114.97(8) . . ? C41 P2 Pd 113.96(8) . . ? C31 P2 Pd 111.33(8) . . ? C8 N1 Pd 116.15(14) . . ? C8 C3 C4 119.6(2) . . ? C8 C3 P1 116.96(17) . . ? C4 C3 P1 123.42(19) . . ? C5 C4 C3 120.1(3) . . ? C4 C5 C6 119.8(3) . . ? C5 C6 C7 120.9(3) . . ? C6 C7 C8 119.4(3) . . ? C7 C8 C3 120.1(2) . . ? C7 C8 N1 119.6(2) . . ? C3 C8 N1 120.2(2) . . ? C12 C11 C16 119.3(2) . . ? C12 C11 P1 119.15(19) . . ? C16 C11 P1 121.6(2) . . ? C11 C12 C13 119.7(3) . . ? C14 C13 C12 120.0(3) . . ? C15 C14 C13 120.8(3) . . ? C14 C15 C16 119.8(3) . . ? C15 C16 C11 120.3(3) . . ? C26 C21 C22 118.6(2) . . ? C26 C21 P1 121.90(19) . . ? C22 C21 P1 119.18(19) . . ? C23 C22 C21 120.8(3) . . ? C24 C23 C22 120.1(3) . . ? C23 C24 C25 119.8(3) . . ? C24 C25 C26 121.1(3) . . ? C25 C26 C21 119.6(3) . . ? C36 C31 C32 118.2(2) . . ? C36 C31 P2 124.9(2) . . ? C32 C31 P2 116.86(19) . . ? C31 C32 C33 120.7(3) . . ? C34 C33 C32 120.4(3) . . ? C35 C34 C33 119.5(3) . . ? C34 C35 C36 120.8(3) . . ? C31 C36 C35 120.4(3) . . ? C46 C41 C42 118.3(3) . . ? C46 C41 P2 123.6(2) . . ? C42 C41 P2 117.8(2) . . ? C41 C42 C43 120.4(3) . . ? C44 C43 C42 120.2(3) . . ? C45 C44 C43 120.0(3) . . ? C44 C45 C46 120.6(4) . . ? C41 C46 C45 120.4(3) . . ? C56 C51 C52 119.0(2) . . ? C56 C51 P2 121.1(2) . . ? C52 C51 P2 119.99(19) . . ? C51 C52 C53 120.1(3) . . ? C54 C53 C52 120.0(3) . . ? C53 C54 C55 121.1(3) . . ? C54 C55 C56 119.7(3) . . ? C55 C56 C51 120.2(3) . . ? F4 B F3 110.7(4) . . ? F4 B F1 110.5(4) . . ? F3 B F1 110.2(3) . . ? F4 B F2 109.1(3) . . ? F3 B F2 107.2(3) . . ? F1 B F2 109.0(3) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.494 _refine_diff_density_min -0.337 _refine_diff_density_rms 0.055