Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 186 loop_ _publ_author_name _publ_author_address 'Coleman, Karl S.' ; Inorganic Chemistry Laboratory South Parks Road Oxford OX1 3QR UK ; 'Green, Malcolm L. H.' ; Inorganic Chemistry Laboratory South Parks Road Oxford OX1 3QR UK ; 'Pascu, Sofia I.' ; Inorganic Chemistry Laboratory South Parks Road Oxford OX1 3QR UK ; 'Rees, Nick H.' ; Inorganic Chemistry Laboratory South Parks Road Oxford OX1 3QR UK' ; 'Rees, Leigh H.' ; 'Inorganic Chemistry Laboratory' South Parks Road Oxford OX1 3QR UK' ; # Local code str45 _audit_creation_method shelxl #**************************************************************************** # 1. SUBMISSION DETAILS _publ_contact_letter ; Please consider this CIF submission for publication as part of a paper for "J. Chem. Soc., Dalton Trans." The remainder of the manuscript and figures have been sent by mail. ; _publ_contact_author_name 'Prof Malcolm L.H. Green' _publ_contact_author_address ; Inorganic Chemistry Laboratory University of Oxford South Parks Road Oxford OX1 3QR UNITED KINGDOM ; _publ_contact_author_phone ' 01865 272 649 ' _publ_contact_author_fax ' 01865 272 690 ' _publ_contact_author_email ' malcolm.green@chem.ox.ac.uk' _publ_requested_journal 'J. Chem. Soc., Dalton Trans.' _publ_requested_category FA _publ_requested_coeditor_name ' Graham McCann ' _publ_section_title ; Palladium(II) complexes with the bidentate iminophosphine ligand [Ph2PCH2C(Ph)=N(2,6-Me2C6H3)] and some catalysts properties ; _publ_section_references # Add your own references - in alphabetic order ; # SIR92 # Altomare, A., Cascarano, G., Giacovazzo G., Guagliardi A., Burla M.C., Polidori, G. & Camalli, M. (1994) SIR92 - a program for automatic solution of crystal structures by direct methods. J. Appl. Cryst. (27), 435-435 # Denzo # Otwinowski, Z. & Minor, W. (1996), Processing of X-ray Diffraction Data Collected in Oscillation Mode. Methods Enzymol. 276, 1997, 307-326. Ed Carter, C.W. & Sweet, R.M., Academic Press. # Extinction correction # Larson, A.C. (1970), Crystallographic Computing, Ed Ahmed, F.R., Munksgaard, Copenhagen, 291-294 # Azimutal absorption correction # North, A.C.T., Phillips, D.C. and Mathews, F.S., (1968), Acta Cryst, A24, 351-359 # SHELXS 86 # Sheldrick, G.M. (1986). SHELXS86. Program for the solution of crystal structures. Univ. of Gottingen, Federal Republic of Germany. # DIFABS # Walker, N., and Stuart, D. Acta Cryst, (1983) A39, 158-166 # CRYSTALS # Watkin, D.J., Prout, C.K. Carruthers, J.R. & Betteridge, P.W. (1996) CRYSTALS Issue 10. Chemical Crystallography Laboratory, OXFORD, UK. #CAMERON # Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996) CAMERON, Chemical Crystallography Laboratory, OXFORD, UK. # RC93 # Watkin, D.J., Prout, C.K., Lilley, P.M.deQ. (1994), RC93, Chemical Crystallography Laboratory, Oxford, UK. ; #========================================================================== # Diffractometer details #========================================================================== _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ' Enraf-nonius DIP2000 ' _computing_data_collection 'DIP2000 software ,Xpress, MAC Science, 1989' _computing_data_reduction 'DIP2000 software DENZO, Otwinowski & Minor, 1996' _computing_cell_refinement 'DIP2000 software DENZO, Otwinowski & Minor, 1996' # end_choice #========================================================================== data_compound1 _database_code_CSD 171176 _chemical_name_systematic # IUPAC name, in full ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C28 H26 N P' _chemical_formula_structural 'C28 H26 N P' _chemical_formula_analytical ? _chemical_formula_sum 'C28 H26 N P' _chemical_formula_weight 407.47 _chemical_melting_point ? _chemical_compound_source 'synthesis as described' 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_h-m 'P 21/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 13.402(5) _cell_length_b 9.595(5) _cell_length_c 17.249(5) _cell_angle_alpha 90.000 _cell_angle_beta 92.423(5) _cell_angle_gamma 90.000 _cell_volume 2216.1(16) _cell_formula_units_z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 147 _cell_measurement_theta_min 2 _cell_measurement_theta_max 25 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.3 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.221 _exptl_crystal_density_method none _exptl_crystal_f_000 864 _exptl_absorpt_coefficient_mu 0.139 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_t_min 0.9052 _exptl_absorpt_correction_t_max 1.1141 _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type mok\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_measurement_device ? _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27212 _diffrn_reflns_av_r_equivalents 0.027 _diffrn_reflns_av_sigmai/neti 0.0264 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.89 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3906 _reflns_number_observed 3662 _reflns_observed_criterion >2sigma(i) _computing_structure_refinement 'shelxl-93 (sheldrick, 1993)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1998)' _refine_special_details ; refinement on f^2^ for all reflections except for 2 with very negative f^2^ or flagged by the user for potential systematic errors. weighted r-factors wr and all goodnesses 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 observed criterion of f^2^ > 2sigma(f^2^) is used only for calculating _r_factor_obs 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 w=1/[\s^2^(fo^2^)+(0.0279p)^2^+1.7349p] 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 0 _refine_ls_number_reflns 3904 _refine_ls_number_parameters 273 _refine_ls_number_restraints 0 _refine_ls_r_factor_all 0.0521 _refine_ls_r_factor_obs 0.0476 _refine_ls_wr_factor_all 0.1186 _refine_ls_wr_factor_obs 0.1049 _refine_ls_goodness_of_fit_all 1.189 _refine_ls_goodness_of_fit_obs 1.212 _refine_ls_restrained_s_all 1.325 _refine_ls_restrained_s_obs 1.212 _refine_ls_shift/esd_max 0.001 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group n1 n 0.53949(11) 0.2697(2) 0.07207(9) 0.0226(4) uani 1 d . . p1 p 0.72902(4) 0.18673(5) 0.21947(3) 0.02068(14) uani 1 d . . c1 c 0.62773(13) 0.3044(2) 0.09448(10) 0.0197(4) uani 1 d . . c2 c 0.66038(13) 0.3390(2) 0.17672(10) 0.0201(4) uani 1 d . . h2a h 0.60140(13) 0.3601(2) 0.20735(10) 0.024 uiso 1 calc r . h2b h 0.70431(13) 0.4220(2) 0.17762(10) 0.024 uiso 1 calc r . c11 c 0.46161(13) 0.2643(2) 0.12479(10) 0.0240(4) uani 1 d . . c12 c 0.43099(14) 0.1325(2) 0.14910(11) 0.0261(4) uani 1 d . . c13 c 0.4852(2) 0.0049(2) 0.12454(12) 0.0327(5) uani 1 d . . h13a h 0.4520(7) -0.0780(2) 0.1443(7) 0.049 uiso 1 calc r . h13b h 0.5543(3) 0.0082(8) 0.1454(7) 0.049 uiso 1 calc r . h13c h 0.4848(10) 0.0010(8) 0.06776(12) 0.049 uiso 1 calc r . c14 c 0.3497(2) 0.1239(3) 0.19588(12) 0.0345(5) uani 1 d . . h14 h 0.3283(2) 0.0354(3) 0.21342(12) 0.041 uiso 1 calc r . c15 c 0.2995(2) 0.2424(3) 0.21727(13) 0.0409(6) uani 1 d . . h15 h 0.2440(2) 0.2354(3) 0.24958(13) 0.049 uiso 1 calc r . c16 c 0.3298(2) 0.3703(3) 0.19175(13) 0.0393(6) uani 1 d . . h16 h 0.2943(2) 0.4512(3) 0.20635(13) 0.047 uiso 1 calc r . c17 c 0.41099(15) 0.3844(2) 0.14516(12) 0.0308(5) uani 1 d . . c18 c 0.4425(2) 0.5254(3) 0.1178(2) 0.0451(6) uani 1 d . . h18a h 0.4527(13) 0.5221(5) 0.0619(2) 0.068 uiso 1 calc r . h18b h 0.5049(7) 0.5526(8) 0.1453(7) 0.068 uiso 1 calc r . h18c h 0.3904(6) 0.5937(4) 0.1282(9) 0.068 uiso 1 calc r . c21 c 0.70577(13) 0.2998(2) 0.03607(10) 0.0205(4) uani 1 d . . c22 c 0.71025(15) 0.1861(2) -0.01309(11) 0.0283(4) uani 1 d . . h22 h 0.66364(15) 0.1122(2) -0.00898(11) 0.034 uiso 1 calc r . c23 c 0.7819(2) 0.1796(3) -0.06795(12) 0.0363(5) uani 1 d . . h23 h 0.7851(2) 0.1008(3) -0.10105(12) 0.044 uiso 1 calc r . c24 c 0.8488(2) 0.2869(3) -0.07486(12) 0.0377(5) uani 1 d . . h24 h 0.8975(2) 0.2830(3) -0.11325(12) 0.045 uiso 1 calc r . c25 c 0.8452(2) 0.3998(3) -0.02620(12) 0.0362(5) uani 1 d . . h25 h 0.8915(2) 0.4740(3) -0.03106(12) 0.043 uiso 1 calc r . c26 c 0.77467(15) 0.4063(2) 0.02976(11) 0.0281(4) uani 1 d . . h26 h 0.77342(15) 0.4839(2) 0.06395(11) 0.034 uiso 1 calc r . c31 c 0.85565(14) 0.2206(2) 0.19058(10) 0.0221(4) uani 1 d . . c32 c 0.9048(2) 0.1134(3) 0.15479(13) 0.0380(5) uani 1 d . . h32 h 0.8732(2) 0.0255(3) 0.14729(13) 0.046 uiso 1 calc r . c33 c 1.0007(2) 0.1347(3) 0.1299(2) 0.0575(8) uani 1 d . . h33 h 1.0347(2) 0.0609(3) 0.1054(2) 0.069 uiso 1 calc r . c34 c 1.0470(2) 0.2609(4) 0.14027(14) 0.0533(8) uani 1 d . . h34 h 1.1127(2) 0.2744(4) 0.12312(14) 0.064 uiso 1 calc r . c35 c 0.9985(2) 0.3676(3) 0.17533(12) 0.0415(6) uani 1 d . . h35 h 1.0304(2) 0.4554(3) 0.18236(12) 0.050 uiso 1 calc r . c36 c 0.90355(15) 0.3479(2) 0.20040(11) 0.0285(5) uani 1 d . . h36 h 0.87030(15) 0.4224(2) 0.22477(11) 0.034 uiso 1 calc r . c41 c 0.73257(14) 0.2335(2) 0.32234(10) 0.0209(4) uani 1 d . . c42 c 0.82047(15) 0.2506(2) 0.36653(11) 0.0264(4) uani 1 d . . h42 h 0.88262(15) 0.2448(2) 0.34220(11) 0.032 uiso 1 calc r . c43 c 0.8194(2) 0.2760(2) 0.44541(12) 0.0334(5) uani 1 d . . h43 h 0.8804(2) 0.2871(2) 0.47476(12) 0.040 uiso 1 calc r . c44 c 0.7300(2) 0.2851(2) 0.48138(12) 0.0350(5) uani 1 d . . h44 h 0.7291(2) 0.3041(2) 0.53540(12) 0.042 uiso 1 calc r . c45 c 0.6415(2) 0.2666(2) 0.43853(12) 0.0316(5) uani 1 d . . h45 h 0.5796(2) 0.2725(2) 0.46318(12) 0.038 uiso 1 calc r . c46 c 0.64294(15) 0.2394(2) 0.36002(11) 0.0264(4) uani 1 d . . h46 h 0.58181(15) 0.2246(2) 0.33130(11) 0.032 uiso 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 n1 0.0179(8) 0.0328(9) 0.0170(8) 0.0045(7) 0.0008(6) 0.0004(7) p1 0.0213(3) 0.0227(3) 0.0179(2) 0.0012(2) -0.0010(2) -0.0009(2) c1 0.0187(9) 0.0221(9) 0.0183(9) 0.0041(7) 0.0001(7) 0.0025(7) c2 0.0171(9) 0.0245(10) 0.0186(9) 0.0014(7) 0.0016(7) 0.0013(7) c11 0.0153(9) 0.0409(12) 0.0155(9) 0.0037(8) -0.0030(7) -0.0006(8) c12 0.0188(9) 0.0417(12) 0.0174(9) 0.0033(8) -0.0027(7) -0.0031(9) c13 0.0316(11) 0.0364(12) 0.0299(11) 0.0001(9) -0.0004(9) -0.0071(9) c14 0.0240(11) 0.0544(14) 0.0249(10) 0.0094(10) -0.0001(8) -0.0070(10) c15 0.0218(11) 0.073(2) 0.0282(11) 0.0066(12) 0.0083(9) 0.0005(11) c16 0.0257(11) 0.060(2) 0.0328(12) -0.0011(11) 0.0055(9) 0.0143(11) c17 0.0218(10) 0.0440(13) 0.0263(10) 0.0050(9) -0.0007(8) 0.0071(9) c18 0.0383(13) 0.0424(14) 0.055(2) 0.0127(12) 0.0070(11) 0.0132(11) c21 0.0178(9) 0.0285(10) 0.0152(9) 0.0036(8) -0.0009(7) 0.0017(8) c22 0.0236(10) 0.0364(12) 0.0250(10) -0.0034(9) 0.0011(8) -0.0037(9) c23 0.0314(11) 0.0499(14) 0.0279(11) -0.0128(10) 0.0043(9) 0.0012(10) c24 0.0260(11) 0.063(2) 0.0248(10) -0.0020(11) 0.0087(9) -0.0011(11) c25 0.0306(11) 0.0476(14) 0.0311(11) 0.0048(10) 0.0084(9) -0.0107(10) c26 0.0287(11) 0.0322(11) 0.0235(10) 0.0009(9) 0.0034(8) -0.0033(9) c31 0.0206(9) 0.0306(11) 0.0151(9) 0.0005(8) -0.0020(7) 0.0046(8) c32 0.0402(13) 0.0388(13) 0.0353(12) -0.0049(10) 0.0056(10) 0.0132(10) c33 0.046(2) 0.079(2) 0.049(2) -0.0098(15) 0.0163(12) 0.031(2) c34 0.0229(12) 0.102(2) 0.0355(13) -0.0037(15) 0.0067(10) 0.0018(14) c35 0.0275(11) 0.072(2) 0.0255(11) -0.0012(11) 0.0016(9) -0.0130(12) c36 0.0229(10) 0.0399(12) 0.0228(10) -0.0032(9) 0.0011(8) -0.0024(9) c41 0.0241(10) 0.0191(9) 0.0196(9) 0.0031(7) 0.0000(7) -0.0022(7) c42 0.0253(10) 0.0315(11) 0.0222(10) 0.0058(8) 0.0002(8) -0.0050(8) c43 0.0367(12) 0.0411(13) 0.0219(10) 0.0066(9) -0.0055(9) -0.0135(10) c44 0.0525(14) 0.0343(12) 0.0184(10) 0.0011(9) 0.0035(9) -0.0092(10) c45 0.0368(12) 0.0343(12) 0.0246(10) 0.0039(9) 0.0104(9) 0.0008(9) c46 0.0241(10) 0.0304(11) 0.0246(10) 0.0047(8) 0.0004(8) 0.0004(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 n1 c1 1.273(2) . ? n1 c11 1.414(2) . ? p1 c31 1.818(2) . ? p1 c41 1.829(2) . ? p1 c2 1.862(2) . ? c1 c21 1.483(2) . ? c1 c2 1.504(2) . ? c11 c17 1.390(3) . ? c11 c12 1.399(3) . ? c12 c14 1.386(3) . ? c12 c13 1.494(3) . ? c14 c15 1.379(3) . ? c15 c16 1.372(4) . ? c16 c17 1.387(3) . ? c17 c18 1.499(3) . ? c21 c26 1.384(3) . ? c21 c22 1.385(3) . ? c22 c23 1.378(3) . ? c23 c24 1.374(3) . ? c24 c25 1.373(3) . ? c25 c26 1.381(3) . ? c31 c32 1.382(3) . ? c31 c36 1.387(3) . ? c32 c33 1.387(4) . ? c33 c34 1.369(4) . ? c34 c35 1.368(4) . ? c35 c36 1.374(3) . ? c41 c42 1.386(3) . ? c41 c46 1.391(3) . ? c42 c43 1.383(3) . ? c43 c44 1.375(3) . ? c44 c45 1.382(3) . ? c45 c46 1.380(3) . ? 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 n1 c11 121.1(2) . . ? c31 p1 c41 103.64(8) . . ? c31 p1 c2 101.67(9) . . ? c41 p1 c2 100.60(8) . . ? n1 c1 c21 117.3(2) . . ? n1 c1 c2 125.0(2) . . ? c21 c1 c2 117.5(2) . . ? c1 c2 p1 108.62(13) . . ? c17 c11 c12 121.4(2) . . ? c17 c11 n1 120.9(2) . . ? c12 c11 n1 117.4(2) . . ? c14 c12 c11 118.5(2) . . ? c14 c12 c13 121.3(2) . . ? c11 c12 c13 120.2(2) . . ? c15 c14 c12 120.7(2) . . ? c16 c15 c14 119.8(2) . . ? c15 c16 c17 121.6(2) . . ? c16 c17 c11 118.0(2) . . ? c16 c17 c18 120.6(2) . . ? c11 c17 c18 121.4(2) . . ? c26 c21 c22 119.1(2) . . ? c26 c21 c1 121.6(2) . . ? c22 c21 c1 119.3(2) . . ? c23 c22 c21 120.4(2) . . ? c24 c23 c22 120.1(2) . . ? c25 c24 c23 119.9(2) . . ? c24 c25 c26 120.4(2) . . ? c25 c26 c21 120.0(2) . . ? c32 c31 c36 118.9(2) . . ? c32 c31 p1 117.2(2) . . ? c36 c31 p1 123.83(15) . . ? c31 c32 c33 119.6(2) . . ? c34 c33 c32 120.7(2) . . ? c35 c34 c33 120.0(2) . . ? c34 c35 c36 120.0(2) . . ? c35 c36 c31 120.9(2) . . ? c42 c41 c46 118.0(2) . . ? c42 c41 p1 123.33(15) . . ? c46 c41 p1 118.42(14) . . ? c43 c42 c41 121.2(2) . . ? c44 c43 c42 120.1(2) . . ? c43 c44 c45 119.6(2) . . ? c46 c45 c44 120.2(2) . . ? c45 c46 c41 120.9(2) . . ? _refine_diff_density_max 0.668 _refine_diff_density_min -0.266 _refine_diff_density_rms 0.045 #=end data_compound_2 _database_code_CSD 171177 # Local code str12 _audit_creation_method SHELXL #========================================================================== # Diffractometer details #========================================================================== _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ' Enraf-nonius DIP2000 ' _computing_data_collection 'DIP2000 software ,Xpress, MAC Science, 1989' _computing_data_reduction 'DIP2000 software DENZO, Otwinowski & Minor, 1996' _computing_cell_refinement 'DIP2000 software DENZO, Otwinowski & Minor, 1996' #========================================================================== _chemical_name_systematic # IUPAC name, in full ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C28 H26 Cl2 N1 P1 Pd1' _chemical_formula_structural 'C28 H26 P1 PD1 CL2 N1' _chemical_formula_analytical ? _chemical_formula_sum 'C28 H26 Cl2 N P Pd' _chemical_formula_weight 584.77 _chemical_melting_point ? _chemical_compound_source 'synthesis as described' 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 monoclinic _symmetry_space_group_name_H-M 'P 21/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 11.182(1) _cell_length_b 22.663(1) _cell_length_c 11.314(1) _cell_angle_alpha 90.00 _cell_angle_beta 117.47(2) _cell_angle_gamma 90.00 _cell_volume 2544.0 _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 2 _cell_measurement_theta_max 25 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.3 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.527 _exptl_crystal_density_method none _exptl_crystal_F_000 1184 _exptl_absorpt_coefficient_mu 1.019 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.7095 _exptl_absorpt_correction_T_max 0.794 _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_measurement_device ? _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29609 _diffrn_reflns_av_R_equivalents 0.048 _diffrn_reflns_av_sigmaI/netI 0.0340 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.80 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4207 _reflns_number_observed 4205 _reflns_observed_criterion >2sigma(I) _computing_structure_solution SIR92 _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'CAMERON (Watkin & Pearce, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1998)' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 2 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+3.8068P] 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 0 _refine_ls_number_reflns 4205 _refine_ls_number_parameters 300 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0572 _refine_ls_R_factor_obs 0.0563 _refine_ls_wR_factor_all 0.1133 _refine_ls_wR_factor_obs 0.0915 _refine_ls_goodness_of_fit_all 1.675 _refine_ls_goodness_of_fit_obs 1.675 _refine_ls_restrained_S_all 2.072 _refine_ls_restrained_S_obs 1.675 _refine_ls_shift/esd_max 0.001 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Pd1 Pd 0.03578(3) 0.152284(15) 0.93137(3) 0.01796(11) Uani 1 d . . Cl1 Cl 0.01595(12) 0.13837(5) 1.12747(11) 0.0296(3) Uani 1 d . . Cl2 Cl 0.26476(11) 0.16352(5) 1.04420(12) 0.0294(3) Uani 1 d . . N1 N -0.1637(4) 0.13659(15) 0.8056(4) 0.0175(8) Uani 1 d . . C1 C -0.2183(4) 0.1553(2) 0.6845(4) 0.0197(9) Uani 1 d . . C2 C -0.1350(4) 0.1892(2) 0.6366(5) 0.0253(10) Uani 1 d . . H2A H -0.1535(4) 0.2311(2) 0.6361(5) 0.030 Uiso 1 calc R . H2B H -0.1573(4) 0.1774(2) 0.5464(5) 0.030 Uiso 1 calc R . P1 P 0.04380(12) 0.17490(5) 0.74747(12) 0.0217(3) Uani 1 d . . C11 C -0.2416(5) 0.0989(2) 0.8472(4) 0.0220(10) Uani 1 d . . C12 C -0.2145(5) 0.0386(2) 0.8506(5) 0.0296(11) Uani 1 d . . C13 C -0.1092(6) 0.0150(2) 0.8169(6) 0.0400(14) Uani 1 d . . H13A H -0.1134(25) -0.0273(2) 0.8140(37) 0.060 Uiso 1 calc R . H13B H -0.0217(7) 0.0274(14) 0.8834(21) 0.060 Uiso 1 calc R . H13C H -0.1247(23) 0.0299(13) 0.7315(18) 0.060 Uiso 1 calc R . C14 C -0.2897(6) 0.0010(2) 0.8865(5) 0.0426(15) Uani 1 d . . H14 H -0.2756(6) -0.0395(2) 0.8885(5) 0.051 Uiso 1 calc R . C15 C -0.3841(7) 0.0228(3) 0.9190(6) 0.052(2) Uani 1 d . . H15 H -0.4346(7) -0.0033(3) 0.9413(6) 0.063 Uiso 1 calc R . C16 C -0.4068(6) 0.0819(3) 0.9197(6) 0.046(2) Uani 1 d . . H16 H -0.4711(6) 0.0956(3) 0.9435(6) 0.055 Uiso 1 calc R . C17 C -0.3334(5) 0.1221(2) 0.8846(5) 0.0322(12) Uani 1 d . . C18 C -0.3518(6) 0.1867(3) 0.8911(6) 0.0432(14) Uani 1 d . . H18A H -0.4163(30) 0.1940(3) 0.9233(37) 0.065 Uiso 1 calc R . H18B H -0.3839(38) 0.2035(4) 0.8038(9) 0.065 Uiso 1 calc R . H18C H -0.2672(10) 0.2045(4) 0.9504(30) 0.065 Uiso 1 calc R . C21 C -0.3618(4) 0.1450(2) 0.5861(4) 0.0218(10) Uani 1 d . . C22 C -0.4487(5) 0.1923(2) 0.5423(5) 0.0328(12) Uani 1 d . . H22 H -0.4186(5) 0.2299(2) 0.5757(5) 0.039 Uiso 1 calc R . C23 C -0.5815(5) 0.1835(3) 0.4478(6) 0.047(2) Uani 1 d . . H23 H -0.6412(5) 0.2151(3) 0.4202(6) 0.057 Uiso 1 calc R . C24 C -0.6257(6) 0.1287(3) 0.3949(6) 0.052(2) Uani 1 d . . H24 H -0.7144(6) 0.1231(3) 0.3303(6) 0.063 Uiso 1 calc R . C25 C -0.5384(6) 0.0822(3) 0.4376(6) 0.050(2) Uani 1 d . . H25 H -0.5680(6) 0.0450(3) 0.4015(6) 0.060 Uiso 1 calc R . C26 C -0.4069(5) 0.0898(2) 0.5334(5) 0.0358(13) Uani 1 d . . H26 H -0.3487(5) 0.0577(2) 0.5626(5) 0.043 Uiso 1 calc R . C31 C 0.0970(5) 0.1161(2) 0.6753(5) 0.0285(11) Uani 1 d . . C32 C 0.1625(5) 0.0680(2) 0.7510(6) 0.0363(13) Uani 1 d . . H32 H 0.1797(5) 0.0659(2) 0.8395(6) 0.044 Uiso 1 calc R . C33 C 0.2031(7) 0.0224(3) 0.6957(7) 0.054(2) Uani 1 d . . H33 H 0.2471(7) -0.0104(3) 0.7466(7) 0.064 Uiso 1 calc R . C34 C 0.1775(7) 0.0263(3) 0.5650(7) 0.063(2) Uani 1 d . . H34 H 0.2039(7) -0.0043(3) 0.5276(7) 0.076 Uiso 1 calc R . C35 C 0.1137(7) 0.0745(3) 0.4886(7) 0.058(2) Uani 1 d . . H35 H 0.0981(7) 0.0767(3) 0.4006(7) 0.070 Uiso 1 calc R . C36 C 0.0730(6) 0.1195(3) 0.5436(5) 0.0419(14) Uani 1 d . . H36 H 0.0294(6) 0.1523(3) 0.4924(5) 0.050 Uiso 1 calc R . C41 C 0.1363(5) 0.2393(2) 0.7450(5) 0.0252(11) Uani 1 d . . C42 C 0.0863(5) 0.2946(2) 0.7486(5) 0.0267(11) Uani 1 d . . H42 H 0.0051(5) 0.2984(2) 0.7519(5) 0.032 Uiso 1 calc R . C43 C 0.1572(5) 0.3441(2) 0.7475(5) 0.0311(11) Uani 1 d . . H43 H 0.1233(5) 0.3814(2) 0.7489(5) 0.037 Uiso 1 calc R . C44 C 0.2784(5) 0.3385(2) 0.7442(5) 0.0328(12) Uani 1 d . . H44 H 0.3252(5) 0.3720(2) 0.7418(5) 0.039 Uiso 1 calc R . C45 C 0.3299(5) 0.2839(2) 0.7446(6) 0.0374(13) Uani 1 d . . H45 H 0.4127(5) 0.2802(2) 0.7446(6) 0.045 Uiso 1 calc R . C46 C 0.2594(5) 0.2342(2) 0.7448(5) 0.0341(12) Uani 1 d . . H46 H 0.2947(5) 0.1970(2) 0.7450(5) 0.041 Uiso 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 0.0156(2) 0.0180(2) 0.0165(2) 0.00074(14) 0.00420(13) 0.00079(15) Cl1 0.0287(7) 0.0386(7) 0.0198(5) 0.0015(5) 0.0097(5) 0.0082(5) Cl2 0.0176(6) 0.0288(7) 0.0305(6) 0.0014(5) 0.0015(5) -0.0027(5) N1 0.016(2) 0.016(2) 0.020(2) -0.0007(15) 0.008(2) -0.0009(14) C1 0.018(2) 0.015(2) 0.023(2) 0.000(2) 0.007(2) 0.001(2) C2 0.017(2) 0.030(3) 0.025(2) 0.009(2) 0.007(2) 0.000(2) P1 0.0158(6) 0.0261(6) 0.0204(6) 0.0050(5) 0.0058(5) -0.0012(5) C11 0.018(2) 0.030(3) 0.015(2) 0.002(2) 0.005(2) -0.007(2) C12 0.038(3) 0.026(3) 0.018(2) 0.000(2) 0.007(2) -0.009(2) C13 0.060(4) 0.022(3) 0.037(3) 0.003(2) 0.021(3) 0.007(3) C14 0.060(4) 0.033(3) 0.030(3) 0.003(2) 0.017(3) -0.017(3) C15 0.058(4) 0.065(5) 0.038(3) 0.000(3) 0.026(3) -0.032(3) C16 0.037(3) 0.072(5) 0.038(3) -0.002(3) 0.025(3) -0.011(3) C17 0.025(3) 0.048(3) 0.022(3) 0.003(2) 0.009(2) -0.001(2) C18 0.039(3) 0.059(4) 0.039(3) 0.006(3) 0.024(3) 0.018(3) C21 0.017(2) 0.030(3) 0.017(2) 0.005(2) 0.007(2) -0.003(2) C22 0.030(3) 0.035(3) 0.031(3) 0.011(2) 0.012(2) 0.004(2) C23 0.018(3) 0.070(4) 0.043(3) 0.030(3) 0.005(3) 0.012(3) C24 0.024(3) 0.086(5) 0.029(3) 0.018(3) -0.003(3) -0.021(3) C25 0.044(4) 0.054(4) 0.032(3) 0.001(3) 0.001(3) -0.023(3) C26 0.034(3) 0.033(3) 0.031(3) 0.001(2) 0.008(3) -0.005(2) C31 0.022(3) 0.036(3) 0.027(3) -0.005(2) 0.011(2) -0.007(2) C32 0.034(3) 0.040(3) 0.035(3) -0.003(2) 0.016(3) 0.003(2) C33 0.053(4) 0.049(4) 0.057(4) -0.008(3) 0.024(3) 0.014(3) C34 0.063(5) 0.072(5) 0.065(5) -0.029(4) 0.038(4) 0.002(4) C35 0.062(5) 0.082(5) 0.042(4) -0.018(4) 0.034(4) -0.005(4) C36 0.042(3) 0.056(4) 0.030(3) 0.001(3) 0.018(3) -0.004(3) C41 0.016(2) 0.032(3) 0.023(2) 0.008(2) 0.005(2) -0.002(2) C42 0.019(3) 0.033(3) 0.026(3) 0.003(2) 0.009(2) -0.001(2) C43 0.034(3) 0.027(3) 0.029(3) 0.003(2) 0.011(2) -0.002(2) C44 0.032(3) 0.032(3) 0.035(3) 0.007(2) 0.017(2) -0.009(2) C45 0.025(3) 0.040(3) 0.051(3) 0.010(3) 0.021(3) -0.004(2) C46 0.026(3) 0.031(3) 0.045(3) 0.012(2) 0.016(3) 0.004(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 N1 2.049(4) . ? Pd1 P1 2.1845(12) . ? Pd1 Cl2 2.2881(12) . ? Pd1 Cl1 2.3505(12) . ? N1 C1 1.288(5) . ? N1 C11 1.445(6) . ? C1 C2 1.489(6) . ? C1 C21 1.490(6) . ? C2 P1 1.834(5) . ? P1 C41 1.796(5) . ? P1 C31 1.801(5) . ? C11 C17 1.382(7) . ? C11 C12 1.397(7) . ? C12 C14 1.383(7) . ? C12 C13 1.494(7) . ? C14 C15 1.361(9) . ? C15 C16 1.365(9) . ? C16 C17 1.400(8) . ? C17 C18 1.486(8) . ? C21 C22 1.377(7) . ? C21 C26 1.378(7) . ? C22 C23 1.387(8) . ? C23 C24 1.368(9) . ? C24 C25 1.364(9) . ? C25 C26 1.377(8) . ? C31 C32 1.371(7) . ? C31 C36 1.388(7) . ? C32 C33 1.388(8) . ? C33 C34 1.373(9) . ? C34 C35 1.371(10) . ? C35 C36 1.378(9) . ? C41 C42 1.380(7) . ? C41 C46 1.382(7) . ? C42 C43 1.378(7) . ? C43 C44 1.378(7) . ? C44 C45 1.365(7) . ? C45 C46 1.376(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 N1 Pd1 P1 83.63(10) . . ? N1 Pd1 Cl2 170.53(10) . . ? P1 Pd1 Cl2 88.76(5) . . ? N1 Pd1 Cl1 94.92(10) . . ? P1 Pd1 Cl1 173.57(5) . . ? Cl2 Pd1 Cl1 93.26(4) . . ? C1 N1 C11 118.7(4) . . ? C1 N1 Pd1 120.8(3) . . ? C11 N1 Pd1 120.2(3) . . ? N1 C1 C2 119.2(4) . . ? N1 C1 C21 124.2(4) . . ? C2 C1 C21 116.6(4) . . ? C1 C2 P1 109.1(3) . . ? C41 P1 C31 106.3(2) . . ? C41 P1 C2 107.4(2) . . ? C31 P1 C2 107.8(2) . . ? C41 P1 Pd1 118.9(2) . . ? C31 P1 Pd1 115.2(2) . . ? C2 P1 Pd1 100.5(2) . . ? C17 C11 C12 123.1(5) . . ? C17 C11 N1 121.3(4) . . ? C12 C11 N1 115.6(4) . . ? C14 C12 C11 117.3(5) . . ? C14 C12 C13 120.8(5) . . ? C11 C12 C13 121.9(4) . . ? C15 C14 C12 120.5(6) . . ? C14 C15 C16 121.9(5) . . ? C15 C16 C17 120.1(6) . . ? C11 C17 C16 117.0(5) . . ? C11 C17 C18 122.0(5) . . ? C16 C17 C18 121.0(5) . . ? C22 C21 C26 119.7(5) . . ? C22 C21 C1 119.0(4) . . ? C26 C21 C1 121.3(4) . . ? C21 C22 C23 119.4(5) . . ? C24 C23 C22 120.7(6) . . ? C25 C24 C23 119.4(5) . . ? C24 C25 C26 120.8(6) . . ? C21 C26 C25 119.9(5) . . ? C32 C31 C36 119.9(5) . . ? C32 C31 P1 119.8(4) . . ? C36 C31 P1 120.3(4) . . ? C31 C32 C33 120.1(5) . . ? C34 C33 C32 119.2(6) . . ? C35 C34 C33 121.3(6) . . ? C34 C35 C36 119.3(6) . . ? C35 C36 C31 120.2(6) . . ? C42 C41 C46 119.6(4) . . ? C42 C41 P1 119.5(4) . . ? C46 C41 P1 120.8(4) . . ? C43 C42 C41 119.8(5) . . ? C42 C43 C44 120.1(5) . . ? C45 C44 C43 120.2(5) . . ? C44 C45 C46 120.1(5) . . ? C45 C46 C41 120.2(5) . . ? _refine_diff_density_max 0.419 _refine_diff_density_min -0.597 _refine_diff_density_rms 0.086 #=end data_compound_3 _database_code_CSD 171178 #Local code str8 _audit_creation_method SHELXL #========================================================================== # Diffractometer details #========================================================================== _diffrn_measurement_device_type 'Enraf-nonius DIP2000' _diffrn_radiation_monochromator graphite _computing_data_collection 'DIP2000 software 'Xpress' (MAC Science, 1989)' _computing_data_reduction 'DIP2000 software 'DENZO' (Otwinowski & Minor, 1996)' _computing_cell_refinement 'DIP2000 software 'DENZO' (Otwinowski & Minor, 1996)' #========================================================================== _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C30 H36 N1 P1 Pd1' _chemical_formula_structural 'C30 H36 N1 P1 PD1' _chemical_formula_analytical ? _chemical_formula_sum 'C28 H26 Br2 N P Pd' _chemical_formula_weight 673.69 _chemical_melting_point ? _chemical_compound_source 'synthesis as described' 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' 'Pd' 'Pd' -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Br' 'Br' -0.2901 2.4595 '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' 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 9.037(2) _cell_length_b 13.944(3) _cell_length_c 20.419(4) _cell_angle_alpha 90.00 _cell_angle_beta 97.06(3) _cell_angle_gamma 90.00 _cell_volume 2553.5(9) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 0 _cell_measurement_theta_max 0 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.752 _exptl_crystal_density_method none _exptl_crystal_F_000 1328 _exptl_absorpt_coefficient_mu 3.936 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 1 _exptl_absorpt_correction_T_max 1 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_measurement_device ? _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5084 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0427 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.77 _diffrn_reflns_theta_max 26.48 _reflns_number_total 5084 _reflns_number_observed 4442 _reflns_observed_criterion >2sigma(I) _computing_structure_solution SIR92 _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'CAMERON (Pearce & Watkin, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1998)' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0338P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5084 _refine_ls_number_parameters 300 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0299 _refine_ls_R_factor_obs 0.0246 _refine_ls_wR_factor_all 0.0659 _refine_ls_wR_factor_obs 0.0642 _refine_ls_goodness_of_fit_all 1.006 _refine_ls_goodness_of_fit_obs 1.053 _refine_ls_restrained_S_all 1.006 _refine_ls_restrained_S_obs 1.053 _refine_ls_shift/esd_max -0.004 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Pd1 Pd 0.93636(2) 0.094557(14) 0.223181(9) 0.01695(6) Uani 1 d . . Br1 Br 1.08254(3) -0.02356(2) 0.166060(13) 0.02517(7) Uani 1 d . . Br2 Br 0.94474(3) -0.00096(2) 0.322338(13) 0.02559(7) Uani 1 d . . N1 N 0.9239(2) 0.1959(2) 0.14792(10) 0.0181(4) Uani 1 d . . C1 C 0.8130(3) 0.2550(2) 0.13978(11) 0.0182(5) Uani 1 d . . C2 C 0.6995(3) 0.2508(2) 0.18762(12) 0.0225(5) Uani 1 d . . H2A H 0.6132(3) 0.2146(2) 0.16850(12) 0.027 Uiso 1 calc R . H2B H 0.6670(3) 0.3152(2) 0.19687(12) 0.027 Uiso 1 calc R . P1 P 0.78164(7) 0.19348(5) 0.26424(3) 0.01756(14) Uani 1 d . . C11 C 1.0388(3) 0.2018(2) 0.10433(12) 0.0187(5) Uani 1 d . . C12 C 1.0151(3) 0.1568(2) 0.04287(12) 0.0208(5) Uani 1 d . . C13 C 0.8763(3) 0.1007(2) 0.02149(13) 0.0251(6) Uani 1 d . . H13A H 0.7913(4) 0.1423(4) 0.0196(9) 0.038 Uiso 1 calc R . H13B H 0.8664(12) 0.0501(9) 0.0526(5) 0.038 Uiso 1 calc R . H13C H 0.8820(10) 0.0736(12) -0.0213(4) 0.038 Uiso 1 calc R . C14 C 1.1274(3) 0.1639(2) 0.00260(13) 0.0265(6) Uani 1 d . . H14 H 1.1152(3) 0.1348(2) -0.03870(13) 0.032 Uiso 1 calc R . C15 C 1.2574(3) 0.2135(2) 0.02284(15) 0.0335(7) Uani 1 d . . H15 H 1.3309(3) 0.2184(2) -0.00508(15) 0.040 Uiso 1 calc R . C16 C 1.2782(3) 0.2558(2) 0.08437(14) 0.0283(6) Uani 1 d . . H16 H 1.3661(3) 0.2890(2) 0.09745(14) 0.034 Uiso 1 calc R . C17 C 1.1701(3) 0.2497(2) 0.12726(12) 0.0229(5) Uani 1 d . . C18 C 1.1980(3) 0.2916(2) 0.19531(13) 0.0309(6) Uani 1 d . . H18A H 1.2865(14) 0.3303(13) 0.1989(4) 0.046 Uiso 1 calc R . H18B H 1.2108(24) 0.2408(2) 0.22721(15) 0.046 Uiso 1 calc R . H18C H 1.1145(11) 0.3306(12) 0.2034(4) 0.046 Uiso 1 calc R . C21 C 0.7846(3) 0.3270(2) 0.08581(12) 0.0200(5) Uani 1 d . . C22 C 0.8730(3) 0.4065(2) 0.08177(13) 0.0271(6) Uani 1 d . . H22 H 0.9599(3) 0.4139(2) 0.11089(13) 0.032 Uiso 1 calc R . C23 C 0.8322(4) 0.4761(2) 0.03399(14) 0.0330(7) Uani 1 d . . H23 H 0.8923(4) 0.5298(2) 0.03122(14) 0.040 Uiso 1 calc R . C24 C 0.7038(3) 0.4659(2) -0.00911(14) 0.0319(7) Uani 1 d . . H24 H 0.6763(3) 0.5131(2) -0.04045(14) 0.038 Uiso 1 calc R . C25 C 0.6153(3) 0.3852(2) -0.00581(14) 0.0304(7) Uani 1 d . . H25 H 0.5302(3) 0.3771(2) -0.03581(14) 0.036 Uiso 1 calc R . C26 C 0.6546(3) 0.3169(2) 0.04244(13) 0.0243(6) Uani 1 d . . H26 H 0.5935(3) 0.2639(2) 0.04582(13) 0.029 Uiso 1 calc R . C31 C 0.6199(3) 0.1525(2) 0.30032(12) 0.0203(5) Uani 1 d . . C32 C 0.5269(3) 0.0868(2) 0.26422(14) 0.0309(7) Uani 1 d . . H32 H 0.5533(3) 0.0613(2) 0.22520(14) 0.037 Uiso 1 calc R . C33 C 0.3945(3) 0.0596(2) 0.2868(2) 0.0361(7) Uani 1 d . . H33 H 0.3314(3) 0.0163(2) 0.2626(2) 0.043 Uiso 1 calc R . C34 C 0.3561(3) 0.0963(2) 0.3449(2) 0.0343(7) Uani 1 d . . H34 H 0.2669(3) 0.0782(2) 0.3597(2) 0.041 Uiso 1 calc R . C35 C 0.4496(3) 0.1599(2) 0.3814(2) 0.0351(7) Uani 1 d . . H35 H 0.4237(3) 0.1841(2) 0.4209(2) 0.042 Uiso 1 calc R . C36 C 0.5821(3) 0.1879(2) 0.35938(14) 0.0287(6) Uani 1 d . . H36 H 0.6455(3) 0.2304(2) 0.38423(14) 0.034 Uiso 1 calc R . C41 C 0.8726(3) 0.2851(2) 0.31681(12) 0.0209(5) Uani 1 d . . C42 C 0.7998(3) 0.3694(2) 0.33092(13) 0.0255(6) Uani 1 d . . H42 H 0.7011(3) 0.3794(2) 0.31336(13) 0.031 Uiso 1 calc R . C43 C 0.8745(4) 0.4380(2) 0.37098(14) 0.0311(6) Uani 1 d . . H43 H 0.8252(4) 0.4937(2) 0.38105(14) 0.037 Uiso 1 calc R . C44 C 1.0222(4) 0.4247(2) 0.39627(15) 0.0355(7) Uani 1 d . . H44 H 1.0721(4) 0.4713(2) 0.42305(15) 0.043 Uiso 1 calc R . C45 C 1.0954(3) 0.3420(2) 0.38169(14) 0.0328(7) Uani 1 d . . H45 H 1.1953(3) 0.3336(2) 0.39780(14) 0.039 Uiso 1 calc R . C46 C 1.0202(3) 0.2718(2) 0.34318(13) 0.0260(6) Uani 1 d . . H46 H 1.0689(3) 0.2151(2) 0.33483(13) 0.031 Uiso 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 0.01665(10) 0.01660(11) 0.01770(10) -0.00082(7) 0.00248(7) 0.00083(7) Br1 0.02553(14) 0.0250(2) 0.02501(14) -0.00384(10) 0.00335(10) 0.00717(11) Br2 0.0309(2) 0.02245(15) 0.02312(14) 0.00457(10) 0.00227(10) -0.00180(11) N1 0.0169(10) 0.0194(11) 0.0182(10) -0.0009(8) 0.0028(8) -0.0012(9) C1 0.0165(12) 0.0212(13) 0.0170(11) -0.0011(9) 0.0022(9) -0.0013(10) C2 0.0202(13) 0.0274(15) 0.0204(12) 0.0020(10) 0.0043(10) 0.0048(11) P1 0.0163(3) 0.0190(3) 0.0176(3) -0.0001(2) 0.0030(2) 0.0006(3) C11 0.0185(12) 0.0194(13) 0.0189(12) 0.0030(9) 0.0046(9) 0.0036(10) C12 0.0218(13) 0.0202(14) 0.0205(12) 0.0013(10) 0.0033(10) 0.0033(11) C13 0.0251(14) 0.027(2) 0.0229(13) -0.0043(10) 0.0021(10) 0.0015(11) C14 0.031(2) 0.029(2) 0.0209(13) -0.0002(11) 0.0082(11) 0.0036(12) C15 0.029(2) 0.040(2) 0.034(2) 0.0044(13) 0.0163(12) 0.0018(13) C16 0.0187(13) 0.034(2) 0.0329(15) 0.0018(12) 0.0044(11) -0.0040(12) C17 0.0227(13) 0.0222(14) 0.0238(13) 0.0003(10) 0.0029(10) 0.0013(11) C18 0.0270(15) 0.036(2) 0.0290(14) -0.0068(12) 0.0013(11) -0.0032(13) C21 0.0194(13) 0.0211(14) 0.0199(12) -0.0016(10) 0.0045(10) 0.0026(10) C22 0.0295(15) 0.027(2) 0.0245(14) 0.0002(11) 0.0042(11) -0.0038(12) C23 0.044(2) 0.024(2) 0.033(2) 0.0025(12) 0.0125(13) -0.0023(13) C24 0.040(2) 0.030(2) 0.0266(14) 0.0087(12) 0.0121(12) 0.0132(14) C25 0.029(2) 0.038(2) 0.0234(13) 0.0032(12) 0.0013(11) 0.0095(13) C26 0.0220(14) 0.0245(15) 0.0264(13) 0.0006(11) 0.0035(10) -0.0005(11) C31 0.0165(12) 0.0212(14) 0.0234(12) 0.0005(10) 0.0038(10) 0.0001(10) C32 0.032(2) 0.034(2) 0.0274(14) -0.0038(12) 0.0039(11) -0.0094(13) C33 0.027(2) 0.036(2) 0.043(2) 0.0045(14) -0.0048(13) -0.0120(14) C34 0.0184(14) 0.041(2) 0.045(2) 0.0166(14) 0.0093(12) 0.0007(13) C35 0.035(2) 0.036(2) 0.038(2) -0.0011(13) 0.0186(13) -0.0013(14) C36 0.0282(15) 0.031(2) 0.0281(14) -0.0041(12) 0.0082(11) -0.0054(12) C41 0.0208(13) 0.0218(14) 0.0203(12) 0.0023(10) 0.0040(10) -0.0033(11) C42 0.0272(14) 0.0218(15) 0.0281(14) 0.0012(11) 0.0052(11) 0.0026(12) C43 0.045(2) 0.0198(14) 0.0302(15) -0.0021(11) 0.0120(13) 0.0018(13) C44 0.043(2) 0.029(2) 0.034(2) -0.0061(12) 0.0002(13) -0.0132(14) C45 0.028(2) 0.037(2) 0.031(2) -0.0046(12) -0.0046(12) -0.0041(13) C46 0.0249(14) 0.027(2) 0.0265(13) -0.0024(11) 0.0033(11) 0.0025(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 N1 2.081(2) . ? Pd1 P1 2.2020(8) . ? Pd1 Br2 2.4169(5) . ? Pd1 Br1 2.4894(5) . ? N1 C1 1.292(3) . ? N1 C11 1.451(3) . ? C1 C21 1.490(3) . ? C1 C2 1.502(3) . ? C2 P1 1.831(3) . ? P1 C41 1.800(3) . ? P1 C31 1.809(3) . ? C11 C12 1.396(3) . ? C11 C17 1.391(4) . ? C12 C14 1.386(3) . ? C12 C13 1.497(4) . ? C14 C15 1.381(4) . ? C15 C16 1.380(4) . ? C16 C17 1.392(3) . ? C17 C18 1.500(4) . ? C21 C22 1.375(4) . ? C21 C26 1.389(4) . ? C22 C23 1.393(4) . ? C23 C24 1.375(4) . ? C24 C25 1.387(4) . ? C25 C26 1.385(4) . ? C31 C36 1.384(4) . ? C31 C32 1.392(4) . ? C32 C33 1.387(4) . ? C33 C34 1.375(4) . ? C34 C35 1.378(5) . ? C35 C36 1.386(4) . ? C41 C46 1.388(4) . ? C41 C42 1.396(4) . ? C42 C43 1.380(4) . ? C43 C44 1.383(4) . ? C44 C45 1.379(4) . ? C45 C46 1.381(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 N1 Pd1 P1 82.91(6) . . ? N1 Pd1 Br2 170.51(6) . . ? P1 Pd1 Br2 88.98(3) . . ? N1 Pd1 Br1 94.99(6) . . ? P1 Pd1 Br1 172.40(2) . . ? Br2 Pd1 Br1 93.68(2) . . ? C1 N1 C11 119.2(2) . . ? C1 N1 Pd1 119.9(2) . . ? C11 N1 Pd1 120.9(2) . . ? N1 C1 C21 125.8(2) . . ? N1 C1 C2 118.2(2) . . ? C21 C1 C2 116.0(2) . . ? C1 C2 P1 109.6(2) . . ? C41 P1 C31 108.28(12) . . ? C41 P1 C2 107.90(13) . . ? C31 P1 C2 102.88(12) . . ? C41 P1 Pd1 113.99(9) . . ? C31 P1 Pd1 122.70(9) . . ? C2 P1 Pd1 99.07(8) . . ? C12 C11 C17 123.3(2) . . ? C12 C11 N1 118.9(2) . . ? C17 C11 N1 117.7(2) . . ? C14 C12 C11 117.3(2) . . ? C14 C12 C13 120.9(2) . . ? C11 C12 C13 121.8(2) . . ? C12 C14 C15 121.1(2) . . ? C16 C15 C14 120.1(2) . . ? C15 C16 C17 121.2(3) . . ? C16 C17 C11 116.9(2) . . ? C16 C17 C18 120.5(2) . . ? C11 C17 C18 122.5(2) . . ? C22 C21 C26 119.7(3) . . ? C22 C21 C1 122.7(2) . . ? C26 C21 C1 117.3(2) . . ? C21 C22 C23 119.9(3) . . ? C24 C23 C22 120.4(3) . . ? C23 C24 C25 119.9(3) . . ? C24 C25 C26 119.6(3) . . ? C25 C26 C21 120.4(3) . . ? C36 C31 C32 119.9(3) . . ? C36 C31 P1 122.7(2) . . ? C32 C31 P1 117.2(2) . . ? C33 C32 C31 119.5(3) . . ? C34 C33 C32 120.3(3) . . ? C33 C34 C35 120.2(3) . . ? C34 C35 C36 120.2(3) . . ? C31 C36 C35 119.8(3) . . ? C46 C41 C42 119.2(3) . . ? C46 C41 P1 118.9(2) . . ? C42 C41 P1 121.9(2) . . ? C43 C42 C41 119.9(3) . . ? C44 C43 C42 120.5(3) . . ? C43 C44 C45 119.9(3) . . ? C44 C45 C46 120.0(3) . . ? C45 C46 C41 120.5(3) . . ? _refine_diff_density_max 0.593 _refine_diff_density_min -0.780 _refine_diff_density_rms 0.090 #=end data_conpound_4 _database_code_CSD 171179 # Local code str70 _audit_creation_method CRYSTALS_ver_12_03_99 #========================================================================== # Diffractometer details #========================================================================== _diffrn_measurement_device_type 'Enraf-nonius DIP2000' _diffrn_radiation_monochromator graphite _computing_data_collection 'DIP2000 software 'Xpress' (MAC Science, 1989)' _computing_data_reduction 'DIP2000 software 'DENZO' (Otwinowski & Minor, 1996)' _computing_cell_refinement 'DIP2000 software 'DENZO' (Otwinowski & Minor, 1996)' #========================================================================== # General computing #========================================================================== _computing_structure_refinement ; CRYSTALS Issue 10 (Watkin, Prout, Carruthers & Betteridge, 1996) ; _computing_publication_material ; CRYSTALS Issue 10 (Watkin, Prout, Carruthers & Betteridge, 1996) ; _computing_molecular_graphics ; CAMERON (Watkin, Prout & Pearce, 1996) ; # choose one of the following two lines _computing_structure_solution 'SIR97 (Giacovazzo et al, 1997)' #========================================================================== _chemical_name_systematic # IUPAC name, in full ; ? ; _chemical_melting_point 'not measured' _refine_ls_matrix_type full _atom_sites_solution_primary direct _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment noref #**************************************************************************** _cell_length_a 20.307(6) _cell_angle_alpha 90 _cell_length_b 10.905(5) _cell_angle_beta 130.49(2) _cell_length_c 15.256(7) _cell_angle_gamma 90 _cell_volume 2569.3(6) _symmetry_cell_setting 'Monoclinic ' _symmetry_space_group_name_H-M 'C 1 c 1 ' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' 'x+1/2,y+1/2,z' 'x,-y,z+1/2' 'x+1/2,-y+1/2,z+1/2' loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source 'C ' 0.0020 0.0020 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International_Tables_Vol_IV_Table_2.2B' 'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7997 0.0030 'International_Tables_Vol_IV_Table_2.2B' 'N ' 0.0040 0.0030 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International_Tables_Vol_IV_Table_2.2B' 'P ' 0.0900 0.0950 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645 1.1149 'International_Tables_Vol_IV_Table_2.2B' 'Pd ' -1.1770 1.0070 19.3319 0.6987 15.5017 7.9893 5.2954 25.2052 0.6058 76.8986 5.2659 'International_Tables_Vol_IV_Table_2.2B' 'Cl ' 0.1320 0.1590 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784 -9.5574 'International_Tables_Vol_IV_Table_2.2B' _chemical_formula_sum 'C29 H29 Cl N P Pd' _chemical_formula_moiety 'C29 H29 Cl N P Pd' _chemical_compound_source ; ? ; _chemical_formula_weight 564.38 _cell_measurement_reflns_used 13025 _cell_measurement_theta_min 0 _cell_measurement_theta_max 27 _cell_measurement_temperature 150 _cell_formula_units_Z 4 _exptl_crystal_description ' fragment ' _exptl_crystal_colour ' golden ' _exptl_crystal_size_min 0.40 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_max 0.40 _exptl_crystal_density_diffrn 1.46 _exptl_crystal_density_meas 'not measured' _exptl_crystal_F_000 1152.0 _exptl_absorpt_coefficient_mu 0.91 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; Denzo/Scalepack (Otwinowski & Minor, 1996) ; _exptl_absorpt_correction_T_min 0.70 _exptl_absorpt_correction_T_max 0.70 # Sheldrick geometric definitions 0.70 0.70 _diffrn_standards_interval_time 0 _diffrn_standards_interval_count 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0.00 _diffrn_ambient_temperature 150 _diffrn_reflns_number 13025 _reflns_number_total 2594 _diffrn_reflns_av_R_equivalents 0.03 # Number of reflections with Friedels Law is 2594 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 2683 _diffrn_measured_fraction_theta_max 0.967 _reflns_number_gt 2589 _diffrn_reflns_theta_min 0.00 _diffrn_reflns_theta_max 26.57 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 14 _reflns_limit_h_min -24 _reflns_limit_h_max 19 _reflns_limit_k_min 0 _reflns_limit_k_max 13 _reflns_limit_l_min 0 _reflns_limit_l_max 19 _refine_diff_density_min -1.40 _refine_diff_density_max 1.01 _reflns_threshold_expression >3.00\s(I) _refine_ls_number_reflns 2589 _refine_ls_number_parameters 298 _refine_ls_R_factor_gt 0.0308 _refine_ls_wR_factor_ref 0.0161 _refine_ls_goodness_of_fit_ref 0.9959 _refine_ls_shift/su_max 0.000413 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Chebychev polynomial with 3 parameters, Carruthers & Watkin , 1979, 1.36 -1.45 0.870 ; _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w # Uequiv = arithmetic mean of Ui # i.e. Ueqiv = (U1+U2+U3)/3 loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_adp_type Pd1 0.73073(3) 0.13338(2) 0.33805(5) 0.0191 1.0000 Uani Cl1 0.79263(7) 0.02723(8) 0.27052(9) 0.0284 1.0000 Uani P1 0.67664(6) 0.22207(8) 0.40807(8) 0.0212 1.0000 Uani C31 0.7392(2) 0.3219(3) 0.5332(3) 0.0237 1.0000 Uani C32 0.7906(2) 0.2746(3) 0.6439(3) 0.0338 1.0000 Uani C33 0.8414(3) 0.3504(4) 0.7385(3) 0.0396 1.0000 Uani C34 0.8412(2) 0.4764(3) 0.7248(3) 0.0354 1.0000 Uani C35 0.7896(3) 0.5238(3) 0.6150(3) 0.0407 1.0000 Uani C36 0.7389(2) 0.4479(3) 0.5194(3) 0.0366 1.0000 Uani C41 0.5758(2) 0.3043(3) 0.3030(3) 0.0235 1.0000 Uani C42 0.5330(2) 0.3603(4) 0.3353(3) 0.0334 1.0000 Uani C43 0.4553(2) 0.4208(3) 0.2525(3) 0.0392 1.0000 Uani C44 0.4221(2) 0.4283(4) 0.1411(3) 0.0397 1.0000 Uani C45 0.4640(2) 0.3733(4) 0.1076(3) 0.0426 1.0000 Uani C46 0.5416(2) 0.3107(3) 0.1897(3) 0.0318 1.0000 Uani C3 0.6466(2) 0.0906(3) 0.4506(3) 0.0273 1.0000 Uani C2 0.6338(2) -0.0228(3) 0.3843(3) 0.0224 1.0000 Uani N1 0.66065(18) -0.0244(2) 0.3271(2) 0.0233 1.0000 Uani C11 0.64567(19) -0.1350(3) 0.2643(3) 0.0257 1.0000 Uani C17 0.7040(2) -0.2324(3) 0.3213(3) 0.0312 1.0000 Uani C16 0.6832(3) -0.3411(3) 0.2591(4) 0.0423 1.0000 Uani C15 0.6090(3) -0.3503(4) 0.1458(4) 0.0508 1.0000 Uani C14 0.5549(3) -0.2509(4) 0.0897(3) 0.0451 1.0000 Uani C12 0.5730(2) -0.1401(4) 0.1471(3) 0.0334 1.0000 Uani C13 0.5152(3) -0.0294(4) 0.0838(3) 0.0425 1.0000 Uani C18 0.7870(3) -0.2185(3) 0.4433(4) 0.0409 1.0000 Uani C21 0.59129(19) -0.1301(3) 0.3926(3) 0.0245 1.0000 Uani C26 0.6358(2) -0.1858(3) 0.4993(3) 0.0300 1.0000 Uani C25 0.5988(3) -0.2862(3) 0.5100(3) 0.0363 1.0000 Uani C24 0.5171(3) -0.3241(3) 0.4173(4) 0.0387 1.0000 Uani C23 0.4716(2) -0.2660(3) 0.3119(4) 0.0388 1.0000 Uani C22 0.5087(2) -0.1700(3) 0.2994(3) 0.0322 1.0000 Uani C1 0.7896(3) 0.2950(3) 0.3519(4) 0.0315 1.0000 Uani H11 0.8318 0.2783 0.3410 0.0600 1.0000 Uiso H12 0.8200 0.3311 0.4291 0.0600 1.0000 Uiso H13 0.7452 0.3532 0.2920 0.0600 1.0000 Uiso H321 0.7909 0.1851 0.6551 0.0600 1.0000 Uiso H331 0.8784 0.3149 0.8170 0.0600 1.0000 Uiso H341 0.8775 0.5310 0.7927 0.0600 1.0000 Uiso H351 0.7886 0.6135 0.6040 0.0600 1.0000 Uiso H361 0.7024 0.4835 0.4410 0.0600 1.0000 Uiso H421 0.5576 0.3573 0.4165 0.0600 1.0000 Uiso H431 0.4237 0.4589 0.2746 0.0600 1.0000 Uiso H441 0.3675 0.4736 0.0838 0.0600 1.0000 Uiso H451 0.4395 0.3783 0.0265 0.0600 1.0000 Uiso H461 0.5721 0.2706 0.1667 0.0600 1.0000 Uiso H31 0.6933 0.0752 0.5341 0.0600 1.0000 Uiso H32 0.5921 0.1095 0.4349 0.0600 1.0000 Uiso H161 0.7227 -0.4124 0.2974 0.0600 1.0000 Uiso H151 0.5943 -0.4289 0.1043 0.0600 1.0000 Uiso H141 0.5024 -0.2582 0.0075 0.0600 1.0000 Uiso H131 0.4675 -0.0510 0.0021 0.0600 1.0000 Uiso H132 0.5495 0.0385 0.0882 0.0600 1.0000 Uiso H133 0.4908 -0.0035 0.1198 0.0600 1.0000 Uiso H181 0.8200 -0.2964 0.4694 0.0600 1.0000 Uiso H182 0.8221 -0.1520 0.4473 0.0600 1.0000 Uiso H183 0.7739 -0.1981 0.4938 0.0600 1.0000 Uiso H261 0.6933 -0.1547 0.5673 0.0600 1.0000 Uiso H251 0.6316 -0.3300 0.5845 0.0600 1.0000 Uiso H241 0.4904 -0.3938 0.4259 0.0600 1.0000 Uiso H231 0.4123 -0.2935 0.2455 0.0600 1.0000 Uiso H221 0.4765 -0.1292 0.2236 0.0600 1.0000 Uiso 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 0.0220(1) 0.01717(9) 0.0218(1) 0.00028(17) 0.01587(8) 0.00135(17) Cl1 0.0315(5) 0.0278(5) 0.0364(5) -0.0031(4) 0.0267(4) 0.0014(4) P1 0.0266(5) 0.0181(4) 0.0238(4) -0.0004(3) 0.0186(4) 0.0004(3) C31 0.0251(16) 0.0212(14) 0.0267(17) 0.0014(12) 0.0178(14) 0.0052(12) C32 0.039(2) 0.0227(17) 0.0322(19) -0.0016(15) 0.0197(17) 0.0003(15) C33 0.040(2) 0.036(2) 0.0286(18) -0.0018(17) 0.0158(16) 0.0016(18) C34 0.0345(19) 0.035(2) 0.0336(19) -0.0102(16) 0.0208(17) -0.0049(16) C35 0.049(2) 0.0237(19) 0.037(2) -0.0069(16) 0.023(2) -0.0053(16) C36 0.045(2) 0.0245(17) 0.0304(19) 0.0009(15) 0.0199(18) -0.0074(16) C41 0.0260(16) 0.0203(15) 0.0308(18) -0.0043(13) 0.0214(15) -0.0038(13) C42 0.0346(17) 0.0364(17) 0.0354(17) -0.0013(19) 0.0255(15) 0.0031(19) C43 0.0283(19) 0.0361(19) 0.049(2) -0.0096(18) 0.0229(19) 0.0011(16) C44 0.0248(18) 0.041(2) 0.040(2) 0.0064(17) 0.0151(17) 0.0036(15) C45 0.0314(17) 0.058(2) 0.0342(18) 0.008(2) 0.0195(16) 0.004(2) C46 0.0307(18) 0.0394(18) 0.0296(18) 0.0001(15) 0.0214(16) -0.0003(14) C3 0.043(2) 0.0206(15) 0.0315(18) -0.0053(13) 0.0298(17) -0.0054(14) C2 0.0259(17) 0.0176(16) 0.0256(17) 0.0010(13) 0.0176(15) 0.0007(14) N1 0.0262(15) 0.0225(14) 0.0239(15) -0.0011(11) 0.0174(13) -0.0017(11) C11 0.0340(16) 0.0204(13) 0.0333(16) -0.0071(16) 0.0266(14) -0.0064(16) C17 0.041(2) 0.0248(16) 0.042(2) -0.0016(15) 0.033(2) -0.0003(13) C16 0.067(3) 0.0215(19) 0.064(3) -0.0039(16) 0.054(2) 0.0003(16) C15 0.085(3) 0.030(2) 0.060(3) -0.019(2) 0.057(3) -0.016(2) C14 0.056(3) 0.043(2) 0.039(2) -0.0144(18) 0.032(2) -0.014(2) C12 0.0408(17) 0.0329(16) 0.0360(17) -0.0063(18) 0.0292(16) -0.0064(19) C13 0.038(2) 0.052(2) 0.0267(19) -0.0031(17) 0.0160(17) -0.0015(18) C18 0.042(2) 0.0324(19) 0.046(2) 0.0072(17) 0.028(2) 0.0097(16) C21 0.0316(16) 0.0196(13) 0.0296(15) -0.0029(16) 0.0231(14) -0.0028(16) C26 0.040(2) 0.0298(17) 0.0271(18) -0.0028(14) 0.0245(17) -0.0038(15) C25 0.055(2) 0.0305(18) 0.039(2) 0.0038(15) 0.037(2) -0.0012(17) C24 0.059(3) 0.0287(17) 0.052(2) -0.0076(16) 0.046(2) -0.0110(16) C23 0.036(2) 0.035(2) 0.050(2) -0.0054(18) 0.0304(19) -0.0106(16) C22 0.0306(17) 0.0319(17) 0.0348(18) 0.0005(13) 0.0216(16) -0.0025(13) C1 0.044(2) 0.0228(17) 0.045(2) -0.0020(16) 0.0361(19) -0.0037(15) _refine_ls_extinction_method 'None' loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Pd1 . Cl1 . 2.3798(9) yes Pd1 . P1 . 2.1925(9) yes Pd1 . N1 . 2.169(3) yes Pd1 . C1 . 2.062(4) yes P1 . C31 . 1.815(3) yes P1 . C41 . 1.818(3) yes P1 . C3 . 1.834(3) yes C31 . C32 . 1.385(5) yes C31 . C36 . 1.389(5) yes C32 . C33 . 1.378(5) yes C32 . H321 . 0.990(3) no C33 . C34 . 1.389(6) yes C33 . H331 . 0.990(4) no C34 . C35 . 1.375(6) yes C34 . H341 . 0.990(3) no C35 . C36 . 1.387(5) yes C35 . H351 . 0.990(4) no C36 . H361 . 0.990(4) no C41 . C42 . 1.388(4) yes C41 . C46 . 1.384(5) yes C42 . C43 . 1.390(5) yes C42 . H421 . 0.990(3) no C43 . C44 . 1.363(6) yes C43 . H431 . 0.990(4) no C44 . C45 . 1.383(6) yes C44 . H441 . 0.990(4) no C45 . C46 . 1.398(5) yes C45 . H451 . 0.990(3) no C46 . H461 . 0.990(3) no C3 . C2 . 1.509(5) yes C3 . H31 . 0.990(4) no C3 . H32 . 0.990(4) no C2 . N1 . 1.297(4) yes C2 . C21 . 1.506(5) yes N1 . C11 . 1.444(4) yes C11 . C17 . 1.396(5) yes C11 . C12 . 1.397(5) yes C17 . C16 . 1.401(5) yes C17 . C18 . 1.502(6) yes C16 . C15 . 1.373(6) yes C16 . H161 . 0.990(4) no C15 . C14 . 1.375(6) yes C15 . H151 . 0.990(4) no C14 . C12 . 1.395(5) yes C14 . H141 . 0.990(4) no C12 . C13 . 1.514(6) yes C13 . H131 . 0.990(4) no C13 . H132 . 0.990(4) no C13 . H133 . 0.990(4) no C18 . H181 . 0.991(4) no C18 . H182 . 0.990(4) no C18 . H183 . 0.990(4) no C21 . C26 . 1.388(5) yes C21 . C22 . 1.388(5) yes C26 . C25 . 1.396(5) yes C26 . H261 . 0.991(4) no C25 . C24 . 1.370(6) yes C25 . H251 . 0.990(4) no C24 . C23 . 1.382(6) yes C24 . H241 . 0.991(3) no C23 . C22 . 1.375(5) yes C23 . H231 . 0.991(4) no C22 . H221 . 0.990(4) no C1 . H11 . 0.990(4) no C1 . H12 . 0.989(4) no C1 . H13 . 0.991(4) no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag Cl1 . Pd1 . P1 . 176.46(4) yes Cl1 . Pd1 . N1 . 94.88(8) yes P1 . Pd1 . N1 . 82.91(8) yes Cl1 . Pd1 . C1 . 91.5(1) yes P1 . Pd1 . C1 . 90.8(1) yes N1 . Pd1 . C1 . 173.54(14) yes Pd1 . P1 . C31 . 123.14(11) yes Pd1 . P1 . C41 . 114.96(11) yes C31 . P1 . C41 . 104.47(15) yes Pd1 . P1 . C3 . 102.39(11) yes C31 . P1 . C3 . 105.29(15) yes C41 . P1 . C3 . 104.76(16) yes P1 . C31 . C32 . 121.2(2) yes P1 . C31 . C36 . 120.2(3) yes C32 . C31 . C36 . 118.6(3) yes C31 . C32 . C33 . 120.9(3) yes C31 . C32 . H321 . 119.5(3) no C33 . C32 . H321 . 119.6(4) no C32 . C33 . C34 . 120.5(4) yes C32 . C33 . H331 . 119.8(4) no C34 . C33 . H331 . 119.7(4) no C33 . C34 . C35 . 118.8(3) yes C33 . C34 . H341 . 120.6(4) no C35 . C34 . H341 . 120.6(4) no C34 . C35 . C36 . 121.0(3) yes C34 . C35 . H351 . 119.5(4) no C36 . C35 . H351 . 119.5(4) no C31 . C36 . C35 . 120.3(3) yes C31 . C36 . H361 . 119.9(4) no C35 . C36 . H361 . 119.9(3) no P1 . C41 . C42 . 120.7(2) yes P1 . C41 . C46 . 119.4(2) yes C42 . C41 . C46 . 120.0(3) yes C41 . C42 . C43 . 119.2(3) yes C41 . C42 . H421 . 120.4(3) no C43 . C42 . H421 . 120.4(3) no C42 . C43 . C44 . 120.8(3) yes C42 . C43 . H431 . 119.6(4) no C44 . C43 . H431 . 119.6(4) no C43 . C44 . C45 . 120.7(3) yes C43 . C44 . H441 . 119.7(4) no C45 . C44 . H441 . 119.7(4) no C44 . C45 . C46 . 119.0(3) yes C44 . C45 . H451 . 120.5(4) no C46 . C45 . H451 . 120.5(4) no C41 . C46 . C45 . 120.3(3) yes C41 . C46 . H461 . 119.9(3) no C45 . C46 . H461 . 119.9(3) no P1 . C3 . C2 . 110.8(2) yes P1 . C3 . H31 . 109.1(3) no C2 . C3 . H31 . 109.1(3) no P1 . C3 . H32 . 109.2(3) no C2 . C3 . H32 . 109.2(3) no H31 . C3 . H32 . 109.5(3) no C3 . C2 . N1 . 119.8(3) yes C3 . C2 . C21 . 116.1(3) yes N1 . C2 . C21 . 124.1(3) yes Pd1 . N1 . C2 . 118.6(2) yes Pd1 . N1 . C11 . 124.0(2) yes C2 . N1 . C11 . 117.3(3) yes N1 . C11 . C17 . 119.6(3) yes N1 . C11 . C12 . 118.3(3) yes C17 . C11 . C12 . 122.1(3) yes C11 . C17 . C16 . 117.4(4) yes C11 . C17 . C18 . 120.7(3) yes C16 . C17 . C18 . 121.8(3) yes C17 . C16 . C15 . 121.1(4) yes C17 . C16 . H161 . 119.4(4) no C15 . C16 . H161 . 119.5(4) no C16 . C15 . C14 . 120.4(3) yes C16 . C15 . H151 . 119.8(4) no C14 . C15 . H151 . 119.8(4) no C15 . C14 . C12 . 120.9(4) yes C15 . C14 . H141 . 119.6(4) no C12 . C14 . H141 . 119.5(4) no C11 . C12 . C14 . 117.8(4) yes C11 . C12 . C13 . 121.4(3) yes C14 . C12 . C13 . 120.8(3) yes C12 . C13 . H131 . 109.4(4) no C12 . C13 . H132 . 109.5(3) no H131 . C13 . H132 . 109.5(4) no C12 . C13 . H133 . 109.5(3) no H131 . C13 . H133 . 109.5(4) no H132 . C13 . H133 . 109.5(4) no C17 . C18 . H181 . 109.5(3) no C17 . C18 . H182 . 109.5(4) no H181 . C18 . H182 . 109.4(4) no C17 . C18 . H183 . 109.5(3) no H181 . C18 . H183 . 109.4(4) no H182 . C18 . H183 . 109.5(4) no C2 . C21 . C26 . 117.8(3) yes C2 . C21 . C22 . 122.3(3) yes C26 . C21 . C22 . 119.9(3) yes C21 . C26 . C25 . 119.4(3) yes C21 . C26 . H261 . 120.3(3) no C25 . C26 . H261 . 120.3(3) no C26 . C25 . C24 . 119.9(3) yes C26 . C25 . H251 . 120.1(4) no C24 . C25 . H251 . 120.0(3) no C25 . C24 . C23 . 120.6(3) yes C25 . C24 . H241 . 119.7(4) no C23 . C24 . H241 . 119.7(4) no C24 . C23 . C22 . 119.9(4) yes C24 . C23 . H231 . 120.1(3) no C22 . C23 . H231 . 120.0(4) no C21 . C22 . C23 . 120.2(3) yes C21 . C22 . H221 . 119.9(3) no C23 . C22 . H221 . 119.9(4) no Pd1 . C1 . H11 . 109.5(3) no Pd1 . C1 . H12 . 109.5(3) no H11 . C1 . H12 . 109.5(4) no Pd1 . C1 . H13 . 109.4(3) no H11 . C1 . H13 . 109.4(3) no H12 . C1 . H13 . 109.5(3) no #=end data_compound_6 _database_code_CSD 171180 #Local code sip9 _audit_creation_date 00-05-08 _audit_creation_method CRYSTALS_ver_12-03-99 #========================================================================== # Diffractometer details #========================================================================== _diffrn_measurement_device_type ; Enraf-nonius DIP2000 ; _diffrn_radiation_monochromator graphite _computing_data_collection ; DIP2000 software 'Xpress' (MAC Science, 1989) ; _computing_data_reduction ; DIP2000 software 'DENZO' (Otwinowski & Minor, 1996) ; _computing_cell_refinement ; DIP2000 software 'DENZO' (Otwinowski & Minor, 1996) ; #========================================================================== # General computing #========================================================================== _computing_structure_refinement ; CRYSTALS Issue 10 (Watkin, Prout, Carruthers & Betteridge, 1996) ; _computing_publication_material ; CRYSTALS Issue 10 (Watkin, Prout, Carruthers & Betteridge, 1996) ; _computing_molecular_graphics ; CAMERON (Watkin, Prout & Pearce, 1996) ; # choose one of the following two lines # _computing_structure_solution 'SHELXS86 (Sheldrick, 1986)' _computing_structure_solution 'SIR92 (Giacovazzo et al, 1992)' #========================================================================== _chemical_name_systematic # IUPAC name, in full ; ? ; _chemical_melting_point 'not measured' # choose from 'full, fullcycle, atomblock, userblock, diagonal, sparse' _refine_ls_matrix_type full # choose from 'heavy, direct, difmap, geom' _atom_sites_solution_primary direct # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom # choose from 'none, undef, noref, refall, refxyz, refU, constr, mixed' _refine_ls_hydrogen_treatment noref #**************************************************************************** _cell_length_a 7.8590(7) _cell_angle_alpha 89.044(6) _cell_length_b 9.2000(13) _cell_angle_beta 84.199(8) _cell_length_c 18.778(3) _cell_angle_gamma 70.296(7) _cell_volume 1271.4 _symmetry_cell_setting 'Triclinic ' _symmetry_space_group_name_H-M 'P -1 ' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' '-x,-y,-z' loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source 'C ' 0.0020 0.0020 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International_Tables_Vol_IV_Table_2.2B' 'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7997 0.0030 'International_Tables_Vol_IV_Table_2.2B' 'Pd ' -1.1770 1.0070 19.3319 0.6987 15.5017 7.9893 5.2954 25.2052 0.6058 76.8986 5.2659 'International_Tables_Vol_IV_Table_2.2B' 'P ' 0.0900 0.0950 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645 1.1149 'International_Tables_Vol_IV_Table_2.2B' 'N ' 0.0040 0.0030 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International_Tables_Vol_IV_Table_2.2B' _chemical_formula_sum ' C30 H32 N1 P1 Pd1 ' _chemical_formula_moiety ' C30 H32 N1 P1 Pd1 ' _chemical_compound_source ; ? ; _chemical_formula_weight 543.97 _cell_measurement_reflns_used 11841 _cell_measurement_theta_min 0 _cell_measurement_theta_max 27 _cell_measurement_temperature 150 _cell_formula_units_Z 2 _exptl_crystal_description ' fragment ' _exptl_crystal_colour ' yellow ' _exptl_crystal_size_min 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_max 0.10 _exptl_crystal_density_diffrn 1.42 _exptl_crystal_density_meas 'not measured' _exptl_crystal_F_000 559.90 _exptl_absorpt_coefficient_mu 0.81 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; Denzo/Scalepack (Otwinowski & Minor, 1996) ; _exptl_absorpt_correction_T_min 0.92 _exptl_absorpt_correction_T_max 0.92 # Sheldrick geometric definitions 0.92 0.92 _diffrn_standards_interval_time 0 _diffrn_standards_interval_count 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0.00 _diffrn_ambient_temperature 150 _diffrn_reflns_number 11841 _reflns_number_total 4630 _diffrn_reflns_av_R_equivalents 0.08 # Number of reflections with Friedels Law is 4630 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 5311 _diffrn_measured_fraction_theta_max 0.872 _reflns_number_gt 3085 _diffrn_reflns_theta_min 0.00 _diffrn_reflns_theta_max 26.57 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _reflns_limit_h_min -8 _reflns_limit_h_max 9 _reflns_limit_k_min -11 _reflns_limit_k_max 11 _reflns_limit_l_min 0 _reflns_limit_l_max 23 _refine_diff_density_min -1.47 _refine_diff_density_max 2.02 _reflns_threshold_expression >4.00\s(I) _refine_ls_number_reflns 3085 _refine_ls_number_parameters 298 _refine_ls_R_factor_gt 0.0868 _refine_ls_wR_factor_ref 0.0704 _refine_ls_goodness_of_fit_ref 1.1147 _refine_ls_shift/su_max 0.000186 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Chebychev polynomial with 3 parameters, Carruthers & Watkin , 1979, 1.70 -1.44 0.855 ; _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71069 _diffrn_measurement_method \w # Uequiv = arithmetic mean of Ui # i.e. Ueqiv = (U1+U2+U3)/3 loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_adp_type Pd1 0.46984(12) 0.40596(9) 0.75508(5) 0.0220 1.0000 Uani P2 0.6330(4) 0.1962(3) 0.81459(14) 0.0245 1.0000 Uani C3 0.5463(13) 0.045(1) 0.8459(5) 0.0271 1.0000 Uani C4 0.4264(15) 0.0118(11) 0.8049(5) 0.0339 1.0000 Uani C5 0.3588(15) -0.1069(12) 0.8244(6) 0.0382 1.0000 Uani C6 0.4088(16) -0.1903(11) 0.8854(6) 0.0413 1.0000 Uani C7 0.5238(17) -0.1590(12) 0.9261(6) 0.0432 1.0000 Uani C8 0.5967(15) -0.0421(12) 0.9080(5) 0.0352 1.0000 Uani C9 0.7656(14) 0.2304(11) 0.8837(5) 0.0274 1.0000 Uani C10 0.6966(14) 0.3706(11) 0.9194(5) 0.0331 1.0000 Uani C11 0.7889(17) 0.4074(11) 0.9715(6) 0.0432 1.0000 Uani C12 0.9539(15) 0.3020(12) 0.9883(6) 0.0394 1.0000 Uani C13 1.0263(16) 0.1624(13) 0.9501(7) 0.0459 1.0000 Uani C14 0.9304(15) 0.1251(12) 0.8983(6) 0.0402 1.0000 Uani C15 0.8032(14) 0.097(1) 0.7410(5) 0.0292 1.0000 Uani C16 0.8579(13) 0.213(1) 0.6946(4) 0.0247 1.0000 Uani N17 0.7300(12) 0.3447(9) 0.6889(4) 0.0251 1.0000 Uani C18 0.7614(13) 0.4605(9) 0.6410(5) 0.0248 1.0000 Uani C19 0.7617(13) 0.447(1) 0.5678(5) 0.0280 1.0000 Uani C20 0.7417(15) 0.3068(13) 0.5338(5) 0.0385 1.0000 Uani C21 0.7811(14) 0.5653(11) 0.5248(5) 0.0334 1.0000 Uani C22 0.7999(15) 0.6949(11) 0.5535(7) 0.0416 1.0000 Uani C23 0.7986(14) 0.7083(11) 0.6261(6) 0.0352 1.0000 Uani C24 0.7800(13) 0.593(1) 0.6732(6) 0.0311 1.0000 Uani C25 0.7757(15) 0.6070(11) 0.7524(6) 0.0374 1.0000 Uani C26 1.0468(12) 0.1634(9) 0.6594(4) 0.0211 1.0000 Uani C27 1.1309(15) 0.011(1) 0.6320(5) 0.0312 1.0000 Uani C28 1.3072(16) -0.0370(12) 0.6022(6) 0.0348 1.0000 Uani C29 1.4097(13) 0.0616(11) 0.5988(5) 0.0280 1.0000 Uani C30 1.3275(13) 0.209(1) 0.6286(5) 0.0272 1.0000 Uani C31 1.1500(13) 0.2609(9) 0.6586(5) 0.0232 1.0000 Uani C32 0.3319(16) 0.5864(12) 0.6909(6) 0.0374 1.0000 Uani C33 0.2367(15) 0.4598(13) 0.8234(6) 0.0391 1.0000 Uani H41 0.3876 0.0729 0.7612 0.0414 1.0000 Uiso H51 0.2743 -0.1328 0.7944 0.0466 1.0000 Uiso H61 0.3587 -0.2744 0.8998 0.0467 1.0000 Uiso H71 0.5595 -0.2190 0.9702 0.0512 1.0000 Uiso H81 0.6838 -0.0217 0.9382 0.0438 1.0000 Uiso H101 0.5791 0.4457 0.9078 0.0398 1.0000 Uiso H111 0.7388 0.5099 0.9965 0.0507 1.0000 Uiso H121 1.0196 0.3263 1.0266 0.0507 1.0000 Uiso H131 1.1480 0.0885 0.9595 0.0533 1.0000 Uiso H141 0.9789 0.0229 0.8727 0.0461 1.0000 Uiso H151 0.9123 0.0245 0.7611 0.0354 1.0000 Uiso H152 0.7496 0.0371 0.7111 0.0354 1.0000 Uiso H201 0.7456 0.3187 0.4805 0.0517 1.0000 Uiso H202 0.8442 0.2126 0.5451 0.0517 1.0000 Uiso H203 0.6238 0.2957 0.5527 0.0517 1.0000 Uiso H211 0.7810 0.5569 0.4717 0.0396 1.0000 Uiso H221 0.8133 0.7789 0.5211 0.0470 1.0000 Uiso H231 0.8113 0.8035 0.6466 0.0439 1.0000 Uiso H271 1.0629 -0.0634 0.6345 0.0395 1.0000 Uiso H281 1.3623 -0.1430 0.5811 0.0418 1.0000 Uiso H291 1.5384 0.0256 0.5765 0.0349 1.0000 Uiso H301 1.4001 0.2797 0.6286 0.0349 1.0000 Uiso H311 1.0947 0.3677 0.6786 0.0283 1.0000 Uiso H251 0.7909 0.7062 0.7660 0.0431 1.0000 Uiso H252 0.8733 0.5183 0.7707 0.0431 1.0000 Uiso H253 0.6538 0.6060 0.7756 0.0431 1.0000 Uiso # methyl hydrogens could not be located 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 0.0259(4) 0.0150(3) 0.0234(4) 0.0013(2) -0.0055(3) -0.0036(3) P2 0.0271(15) 0.0186(12) 0.0255(14) 0.001(1) 0.0010(11) -0.006(1) C3 0.032(6) 0.023(5) 0.021(5) 0.002(4) 0.007(4) -0.006(4) C4 0.040(7) 0.035(5) 0.027(5) -0.001(4) 0.004(4) -0.015(5) C5 0.033(6) 0.029(5) 0.048(7) -0.010(5) 0.003(5) -0.006(5) C6 0.040(7) 0.026(5) 0.051(7) -0.002(5) 0.016(5) -0.008(5) C7 0.050(8) 0.025(5) 0.047(7) 0.002(5) 0.004(6) -0.006(5) C8 0.038(7) 0.034(6) 0.033(6) 0.003(4) -0.005(5) -0.012(5) C9 0.030(6) 0.033(5) 0.025(5) 0.008(4) -0.008(4) -0.017(4) C10 0.037(6) 0.024(5) 0.033(5) -0.005(4) -0.009(5) -0.002(4) C11 0.058(8) 0.025(5) 0.042(6) -0.003(5) -0.002(6) -0.009(5) C12 0.040(7) 0.045(6) 0.038(6) 0.010(5) -0.014(5) -0.018(5) C13 0.039(7) 0.036(6) 0.056(7) 0.002(5) -0.007(6) -0.003(5) C14 0.038(7) 0.028(5) 0.045(6) -0.002(5) -0.011(5) 0.004(5) C15 0.033(6) 0.019(4) 0.031(5) -0.000(4) 0.004(4) -0.006(4) C16 0.040(6) 0.020(4) 0.014(4) 0.004(3) -0.006(4) -0.009(4) N17 0.034(5) 0.021(4) 0.021(4) -0.004(3) -0.001(4) -0.009(4) C18 0.025(5) 0.013(4) 0.034(5) 0.009(4) -0.005(4) -0.004(4) C19 0.023(5) 0.020(4) 0.041(6) 0.006(4) -0.004(4) -0.006(4) C20 0.042(7) 0.052(7) 0.029(5) 0.005(5) -0.003(5) -0.027(5) C21 0.032(6) 0.030(5) 0.033(6) 0.007(4) -0.004(4) -0.005(4) C22 0.034(7) 0.015(5) 0.070(8) 0.010(5) 0.006(6) -0.003(4) C23 0.032(6) 0.021(5) 0.049(7) -0.001(4) 0.003(5) -0.007(4) C24 0.028(6) 0.020(5) 0.044(6) 0.003(4) -0.009(5) -0.004(4) C25 0.042(7) 0.020(5) 0.046(6) -0.007(4) -0.012(5) -0.001(4) C26 0.029(5) 0.017(4) 0.013(4) 0.001(3) 0.002(4) -0.003(4) C27 0.045(7) 0.020(5) 0.031(5) 0.005(4) -0.005(5) -0.013(4) C28 0.041(7) 0.025(5) 0.033(6) -0.003(4) 0.006(5) -0.007(5) C29 0.031(6) 0.026(5) 0.026(5) -0.002(4) 0.003(4) -0.010(4) C30 0.029(6) 0.024(5) 0.031(5) 0.007(4) -0.012(4) -0.010(4) C31 0.028(5) 0.019(4) 0.021(4) 0.005(3) -0.004(4) -0.006(4) C32 0.052(7) 0.028(5) 0.029(6) 0.011(5) -0.017(5) -0.007(5) C33 0.031(6) 0.041(6) 0.038(6) 0.002(5) 0.013(5) -0.007(5) _refine_ls_extinction_method 'None' loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Pd1 . P2 . 2.273(3) yes Pd1 . N17 . 2.185(8) yes Pd1 . C32 . 2.09(1) yes Pd1 . C33 . 2.045(11) yes P2 . C3 . 1.81(1) yes P2 . C9 . 1.84(1) yes P2 . C15 . 1.84(1) yes C3 . C4 . 1.385(14) yes C3 . C8 . 1.416(13) yes C4 . C5 . 1.395(15) yes C4 . H41 . 1.00(1) no C5 . C6 . 1.382(15) yes C5 . H51 . 1.001(11) no C6 . C7 . 1.344(16) yes C6 . H61 . 1.002(11) no C7 . C8 . 1.402(15) yes C7 . H71 . 0.998(11) no C8 . H81 . 1.00(1) no C9 . C10 . 1.375(13) yes C9 . C14 . 1.381(14) yes C10 . C11 . 1.384(15) yes C10 . H101 . 0.991(9) no C11 . C12 . 1.395(15) yes C11 . H111 . 1.00(1) no C12 . C13 . 1.394(15) yes C12 . H121 . 1.00(1) no C13 . C14 . 1.401(15) yes C13 . H131 . 1.000(11) no C14 . H141 . 1.00(1) no C15 . C16 . 1.510(12) yes C15 . H151 . 0.997(9) no C15 . H152 . 1.00(1) no C16 . N17 . 1.300(11) yes C16 . C26 . 1.485(13) yes N17 . C18 . 1.451(11) yes C18 . C19 . 1.381(13) yes C18 . C24 . 1.428(13) yes C19 . C20 . 1.514(14) yes C19 . C21 . 1.382(13) yes C20 . H201 . 1.00(1) no C20 . H202 . 1.001(11) no C20 . H203 . 0.996(11) no C21 . C22 . 1.374(15) yes C21 . H211 . 1.00(1) no C22 . C23 . 1.370(16) yes C22 . H221 . 1.00(1) no C23 . C24 . 1.406(14) yes C23 . H231 . 1.00(1) no C24 . C25 . 1.491(14) yes C25 . H251 . 1.00(1) no C25 . H252 . 1.00(1) no C25 . H253 . 1.014(12) no C26 . C27 . 1.416(12) yes C26 . C31 . 1.397(13) yes C27 . C28 . 1.366(15) yes C27 . H271 . 1.00(1) no C28 . C29 . 1.399(15) yes C28 . H281 . 1.00(1) no C29 . C30 . 1.391(13) yes C29 . H291 . 1.00(1) no C30 . C31 . 1.376(13) yes C30 . H301 . 0.999(9) no C31 . H311 . 0.993(8) no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag P2 . Pd1 . N17 . 80.2(2) yes P2 . Pd1 . C32 . 174.3(3) yes N17 . Pd1 . C32 . 95.5(4) yes P2 . Pd1 . C33 . 96.6(3) yes N17 . Pd1 . C33 . 175.8(4) yes C32 . Pd1 . C33 . 87.8(5) yes Pd1 . P2 . C3 . 123.4(3) yes Pd1 . P2 . C9 . 116.9(3) yes C3 . P2 . C9 . 107.5(4) yes Pd1 . P2 . C15 . 99.2(3) yes C3 . P2 . C15 . 101.6(4) yes C9 . P2 . C15 . 104.8(5) yes P2 . C3 . C4 . 116.9(7) yes P2 . C3 . C8 . 124.0(8) yes C4 . C3 . C8 . 119.1(9) yes C3 . C4 . C5 . 120.1(9) yes C3 . C4 . H41 . 120.3(10) no C5 . C4 . H41 . 119.6(10) no C4 . C5 . C6 . 120.2(10) yes C4 . C5 . H51 . 120.4(11) no C6 . C5 . H51 . 119.4(11) no C5 . C6 . C7 . 120.6(10) yes C5 . C6 . H61 . 120.2(12) no C7 . C6 . H61 . 119.3(11) no C6 . C7 . C8 . 121.1(10) yes C6 . C7 . H71 . 120.5(12) no C8 . C7 . H71 . 118.4(12) no C3 . C8 . C7 . 119.0(10) yes C3 . C8 . H81 . 120.8(10) no C7 . C8 . H81 . 120.2(10) no P2 . C9 . C10 . 116.7(7) yes P2 . C9 . C14 . 122.9(8) yes C10 . C9 . C14 . 120.4(9) yes C9 . C10 . C11 . 120.7(9) yes C9 . C10 . H101 . 119.5(9) no C11 . C10 . H101 . 119.8(9) no C10 . C11 . C12 . 120.1(9) yes C10 . C11 . H111 . 120.2(11) no C12 . C11 . H111 . 119.8(11) no C11 . C12 . C13 . 118.9(10) yes C11 . C12 . H121 . 120.7(11) no C13 . C12 . H121 . 120.4(10) no C12 . C13 . C14 . 120.5(10) yes C12 . C13 . H131 . 119.7(11) no C14 . C13 . H131 . 119.8(10) no C9 . C14 . C13 . 119.4(9) yes C9 . C14 . H141 . 120.0(10) no C13 . C14 . H141 . 120.6(10) no P2 . C15 . C16 . 110.4(6) yes P2 . C15 . H151 . 109.5(7) no C16 . C15 . H151 . 109.5(9) no P2 . C15 . H152 . 108.9(7) no C16 . C15 . H152 . 109.3(8) no H151 . C15 . H152 . 109.3(8) no C15 . C16 . N17 . 115.1(8) yes C15 . C16 . C26 . 117.4(7) yes N17 . C16 . C26 . 127.4(8) yes Pd1 . N17 . C16 . 121.8(6) yes Pd1 . N17 . C18 . 117.8(6) yes C16 . N17 . C18 . 120.2(8) yes N17 . C18 . C19 . 121.4(8) yes N17 . C18 . C24 . 117.0(8) yes C19 . C18 . C24 . 121.6(8) yes C18 . C19 . C20 . 121.5(8) yes C18 . C19 . C21 . 119.2(9) yes C20 . C19 . C21 . 119.4(9) yes C19 . C20 . H201 . 109.5(9) no C19 . C20 . H202 . 109.4(9) no H201 . C20 . H202 . 109.0(10) no C19 . C20 . H203 . 109.7(10) no H201 . C20 . H203 . 109.5(10) no H202 . C20 . H203 . 109.7(10) no C19 . C21 . C22 . 121.2(10) yes C19 . C21 . H211 . 119.7(10) no C22 . C21 . H211 . 119.1(10) no C21 . C22 . C23 . 119.6(9) yes C21 . C22 . H221 . 119.7(12) no C23 . C22 . H221 . 120.7(11) no C22 . C23 . C24 . 122.4(9) yes C22 . C23 . H231 . 119.1(10) no C24 . C23 . H231 . 118.5(11) no C18 . C24 . C23 . 116.0(9) yes C18 . C24 . C25 . 121.0(9) yes C23 . C24 . C25 . 123.0(9) yes C24 . C25 . H251 . 110.7(10) no C24 . C25 . H252 . 110.4(9) no H251 . C25 . H252 . 109.7(10) no C24 . C25 . H253 . 109.0(9) no H251 . C25 . H253 . 108.4(9) no H252 . C25 . H253 . 108.6(10) no C16 . C26 . C27 . 120.1(8) yes C16 . C26 . C31 . 120.9(8) yes C27 . C26 . C31 . 118.7(8) yes C26 . C27 . C28 . 120.2(9) yes C26 . C27 . H271 . 120.5(10) no C28 . C27 . H271 . 119.3(9) no C27 . C28 . C29 . 121.5(9) yes C27 . C28 . H281 . 119.1(11) no C29 . C28 . H281 . 119.4(11) no C28 . C29 . C30 . 117.6(9) yes C28 . C29 . H291 . 120.7(9) no C30 . C29 . H291 . 121.7(9) no C29 . C30 . C31 . 122.3(9) yes C29 . C30 . H301 . 118.9(10) no C31 . C30 . H301 . 118.8(9) no C26 . C31 . C30 . 119.5(8) yes C26 . C31 . H311 . 120.2(9) no C30 . C31 . H311 . 120.3(9) no #=end data_compound_7 _database_code_CSD 171181 _audit_creation_date 01-14-08 _audit_creation_method CRYSTALS_ver_12-03-99 # Local code sip39a #========================================================================== # Diffractometer details #========================================================================== _diffrn_measurement_device_type ; Nonius KappaCCD ; _diffrn_radiation_monochromator graphite _computing_data_collection ; KappaCCD software 'Collect' (Nonius, 2000) ; _computing_data_reduction ; KappaCCD software 'DENZO' (Otwinowski & Minor, 1996) ; _computing_cell_refinement ; KappaCCD software 'DENZO' (Otwinowski & Minor, 1996) ; #========================================================================== # General computing #========================================================================== _computing_structure_refinement ; CRYSTALS (Watkin et al, 2001) ; _computing_publication_material ; CRYSTALS (Watkin et al, 2001) ; _computing_structure_solution 'SIR92 (Giacovazzo et al, 1992)' _chemical_name_systematic # IUPAC name, in full ; ? ; _chemical_melting_point 'not measured' _refine_ls_matrix_type full _atom_sites_solution_primary direct _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment noref #************************************************************************** _cell_length_a 28.0025(4) _cell_angle_alpha 90 _cell_length_b 11.6282(2) _cell_angle_beta 121.2300(6) _cell_length_c 19.8002(4) _cell_angle_gamma 90 _cell_volume 5513.1 _symmetry_cell_setting 'Monoclinic ' _symmetry_space_group_name_H-M 'C 1 2/c 1 ' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' '-x,-y,-z' 'x+1/2,y+1/2,z' '-x+1/2,-y+1/2,-z' '-x,y,-z+1/2' 'x,-y,z+1/2' '-x+1/2,y+1/2,-z+1/2' 'x+1/2,-y+1/2,z+1/2' loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source 'C ' 0.0020 0.0020 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International_Tables_Vol_IV_Table_2.2B' 'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7997 0.0030 'International_Tables_Vol_IV_Table_2.2B' 'Br ' -0.3740 2.4560 17.1789 2.1723 5.2358 16.5796 5.6377 0.2609 3.9851 41.4328 2.9557 'International_Tables_Vol_IV_Table_2.2B' 'Cl ' 0.1320 0.1590 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784 -9.5574 'International_Tables_Vol_IV_Table_2.2B' 'N ' 0.0040 0.0030 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International_Tables_Vol_IV_Table_2.2B' 'P ' 0.0900 0.0950 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645 1.1149 'International_Tables_Vol_IV_Table_2.2B' 'Pd ' -1.1770 1.0070 19.3319 0.6987 15.5017 7.9893 5.2954 25.2052 0.6058 76.8986 5.2659 'International_Tables_Vol_IV_Table_2.2B' _chemical_formula_sum ' C29 H27 Br1 Cl2 N1 P1 Pd1 ' _chemical_formula_moiety ' C29 H27 Br1 Cl2 N1 P1 Pd1 ' _chemical_compound_source ; ? ; _chemical_formula_weight 677.72 _cell_measurement_reflns_used 42409 _cell_measurement_theta_min 5 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 150 _cell_formula_units_Z 8 _exptl_crystal_description ' fragment ' _exptl_crystal_colour ' green ' _exptl_crystal_size_min 0.10 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_max 0.20 _exptl_crystal_density_diffrn 1.633 _exptl_crystal_density_meas 'not measured' _exptl_crystal_F_000 2694.818 _exptl_absorpt_coefficient_mu 2.394 _diffrn_measurement_method \w _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; Denzo/Scalepack (Otwinowski & Minor, 1996) ; _exptl_absorpt_correction_T_min 0.62 _exptl_absorpt_correction_T_max 0.79 _diffrn_standards_interval_time 0 _diffrn_standards_interval_count 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0.00 _diffrn_ambient_temperature 150 _diffrn_reflns_number 42409 _reflns_number_total 5914 _diffrn_reflns_av_R_equivalents 0.052 _diffrn_measured_fraction_theta_max 0.998 _reflns_number_gt 4694 _diffrn_reflns_theta_min 5.09 _diffrn_reflns_theta_max 27.45 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 21 _reflns_limit_h_min -29 _reflns_limit_h_max 29 _reflns_limit_k_min -14 _reflns_limit_k_max 14 _reflns_limit_l_min -25 _reflns_limit_l_max 25 _refine_diff_density_min -1.57 _refine_diff_density_max 1.10 _reflns_threshold_expression >3.00\s(I) _refine_ls_number_reflns 4694 _refine_ls_number_parameters 314 _refine_ls_R_factor_gt 0.0354 _refine_ls_wR_factor_ref 0.0415 _refine_ls_goodness_of_fit_ref 1.0485 _refine_ls_shift/su_max 0.005918 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Chebychev polynomial with 3 parameters, Carruthers & Watkin , 1979, 1.94 -.180 1.21 ; _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 # Uequiv = arithmetic mean of Ui # i.e. Ueqiv = (U1+U2+U3)/3 loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_adp_type Pd1 0.43072(1) 0.12529(2) 0.717648(13) 0.0172 1.0000 Uani Br1 0.481670(13) 0.06121(3) 0.653718(19) 0.0231 1.0000 Uani P1 0.35437(4) 0.17059(8) 0.60464(5) 0.0209 1.0000 Uani N1 0.38903(12) 0.1978(2) 0.76616(15) 0.0205 1.0000 Uani C1 0.31661(15) 0.2485(3) 0.63637(19) 0.0257 1.0000 Uani C2 0.34138(14) 0.2553(3) 0.71729(18) 0.0202 1.0000 Uani C3 0.42019(14) 0.2179(3) 0.84908(18) 0.0199 1.0000 Uani C4 0.42425(15) 0.1286(3) 0.8999(2) 0.0273 1.0000 Uani C5 0.45674(18) 0.1480(5) 0.9816(2) 0.0433 1.0000 Uani C6 0.4834(2) 0.2517(5) 1.0112(2) 0.0508 1.0000 Uani C7 0.47983(18) 0.3373(4) 0.9608(3) 0.0434 1.0000 Uani C8 0.44919(16) 0.3218(3) 0.8792(2) 0.0297 1.0000 Uani C9 0.39656(18) 0.0153(4) 0.8691(3) 0.0394 1.0000 Uani C10 0.44936(19) 0.4118(4) 0.8250(3) 0.0429 1.0000 Uani C11 0.31314(14) 0.3294(3) 0.74831(19) 0.0206 1.0000 Uani C12 0.30392(15) 0.2947(3) 0.8079(2) 0.0229 1.0000 Uani C13 0.27436(16) 0.3647(3) 0.8307(2) 0.0288 1.0000 Uani C14 0.25435(16) 0.4710(4) 0.7954(2) 0.0319 1.0000 Uani C15 0.26458(17) 0.5071(3) 0.7375(2) 0.0328 1.0000 Uani C16 0.29335(16) 0.4377(3) 0.7137(2) 0.0277 1.0000 Uani C17 0.36405(15) 0.2590(3) 0.5368(2) 0.0254 1.0000 Uani C18 0.38913(17) 0.3663(3) 0.5642(2) 0.0312 1.0000 Uani C19 0.39457(18) 0.4414(4) 0.5133(3) 0.0380 1.0000 Uani C20 0.37464(19) 0.4089(4) 0.4356(3) 0.0404 1.0000 Uani C21 0.35029(19) 0.3025(4) 0.4087(2) 0.0397 1.0000 Uani C22 0.34510(17) 0.2270(4) 0.4593(2) 0.0314 1.0000 Uani C23 0.31483(15) 0.0469(3) 0.54674(18) 0.0224 1.0000 Uani C24 0.25939(15) 0.0338(3) 0.5257(2) 0.0267 1.0000 Uani C25 0.22790(16) -0.0583(4) 0.4785(2) 0.0315 1.0000 Uani C26 0.25226(17) -0.1379(3) 0.4531(2) 0.0295 1.0000 Uani C27 0.30791(17) -0.1276(3) 0.4756(2) 0.0308 1.0000 Uani C28 0.33916(16) -0.0350(3) 0.5223(2) 0.0288 1.0000 Uani C29 0.4131(4) -0.1979(6) 0.7059(5) 0.055(2) 0.738(6) Uiso Cl1 0.3819(1) -0.2820(2) 0.74670(13) 0.0649(7) 0.738(6) Uiso Cl2 0.4284(1) -0.2783(3) 0.64480(15) 0.0659(7) 0.738(6) Uiso C30 0.4271(6) -0.2148(14) 0.7208(12) 0.041(5) 0.262(6) Uiso Cl3 0.3653(4) -0.2218(9) 0.7248(5) 0.090(3) 0.262(6) Uiso Cl4 0.4311(3) -0.3265(8) 0.6634(5) 0.075(2) 0.262(6) Uiso H11 0.2799 0.2853 0.5990 0.0302 1.0000 Uiso H51 0.4606 0.0857 1.0190 0.0536 1.0000 Uiso H61 0.5054 0.2648 1.0695 0.0597 1.0000 Uiso H71 0.4996 0.4119 0.9832 0.0503 1.0000 Uiso H91 0.4045 -0.0359 0.9143 0.0492 1.0000 Uiso H92 0.4113 -0.0211 0.8377 0.0492 1.0000 Uiso H93 0.3553 0.0268 0.8345 0.0492 1.0000 Uiso H101 0.4720 0.4793 0.8567 0.0506 1.0000 Uiso H102 0.4660 0.3790 0.7951 0.0506 1.0000 Uiso H103 0.4102 0.4370 0.7870 0.0506 1.0000 Uiso H121 0.3186 0.2188 0.8346 0.0286 1.0000 Uiso H131 0.2675 0.3382 0.8729 0.0372 1.0000 Uiso H141 0.2328 0.5208 0.8115 0.0384 1.0000 Uiso H151 0.2510 0.5843 0.7125 0.0385 1.0000 Uiso H161 0.3001 0.4649 0.6715 0.0340 1.0000 Uiso H181 0.4032 0.3895 0.6201 0.0383 1.0000 Uiso H191 0.4127 0.5181 0.5328 0.0469 1.0000 Uiso H201 0.3780 0.4630 0.3989 0.0502 1.0000 Uiso H211 0.3363 0.2794 0.3529 0.0485 1.0000 Uiso H221 0.3277 0.1497 0.4397 0.0390 1.0000 Uiso H241 0.2333 0.0777 0.5364 0.0319 1.0000 Uiso H251 0.1879 -0.0670 0.4629 0.0382 1.0000 Uiso H261 0.2295 -0.2031 0.4183 0.0337 1.0000 Uiso H271 0.3256 -0.1863 0.4584 0.0368 1.0000 Uiso H281 0.3793 -0.0272 0.5385 0.0346 1.0000 Uiso H291 0.4486 -0.1644 0.7499 0.0658 0.7377 Uiso H292 0.3869 -0.1345 0.6741 0.0658 0.7377 Uiso H301 0.4601 -0.2205 0.7757 0.0497 0.2623 Uiso H302 0.4279 -0.1394 0.6972 0.0497 0.2623 Uiso 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 0.01590(13) 0.02114(12) 0.01461(12) -0.00026(9) 0.00797(9) 0.00174(9) Br1 0.01657(17) 0.03485(19) 0.01880(16) -0.00713(13) 0.00986(13) -0.00226(13) P1 0.0191(4) 0.0279(4) 0.0143(4) -0.0009(3) 0.0077(3) 0.0036(3) N1 0.0199(14) 0.0253(14) 0.0157(12) 0.0012(11) 0.0088(11) 0.0044(11) C1 0.0228(17) 0.0365(19) 0.0162(15) 0.0019(13) 0.0091(13) 0.0097(14) C2 0.0231(17) 0.0209(15) 0.0173(15) 0.0005(12) 0.0111(13) 0.0026(12) C3 0.0203(16) 0.0271(17) 0.0140(14) -0.0001(12) 0.0101(12) 0.0021(13) C4 0.0211(17) 0.039(2) 0.0252(17) 0.0081(15) 0.0142(14) 0.0049(15) C5 0.031(2) 0.078(3) 0.0248(19) 0.017(2) 0.0174(17) 0.011(2) C6 0.032(2) 0.093(4) 0.0242(19) -0.014(2) 0.0122(17) 0.001(2) C7 0.031(2) 0.055(3) 0.040(2) -0.022(2) 0.0152(18) -0.0038(19) C8 0.0234(18) 0.0324(19) 0.0326(18) -0.0086(15) 0.0141(15) 0.0013(15) C9 0.033(2) 0.035(2) 0.054(3) 0.0198(19) 0.026(2) 0.0044(17) C10 0.039(2) 0.0264(19) 0.061(3) 0.0019(19) 0.024(2) -0.0061(17) C11 0.0206(16) 0.0229(16) 0.0189(14) -0.0013(12) 0.0106(13) 0.0024(12) C12 0.0230(17) 0.0242(16) 0.0245(16) -0.0012(13) 0.0143(14) -0.0004(13) C13 0.0282(19) 0.038(2) 0.0265(17) -0.0029(15) 0.0187(15) 0.0004(16) C14 0.0284(19) 0.039(2) 0.0282(18) -0.0057(16) 0.0149(15) 0.0101(16) C15 0.037(2) 0.0303(19) 0.0294(18) 0.0048(15) 0.0155(16) 0.0131(16) C16 0.033(2) 0.0298(18) 0.0219(16) 0.0051(14) 0.0156(15) 0.0091(15) C17 0.0197(17) 0.0349(19) 0.0223(16) 0.0030(14) 0.0115(13) 0.0082(14) C18 0.033(2) 0.0326(19) 0.0303(19) -0.0024(15) 0.0178(16) -0.0008(16) C19 0.033(2) 0.038(2) 0.046(2) 0.0054(18) 0.0228(19) 0.0002(17) C20 0.037(2) 0.048(2) 0.040(2) 0.0174(19) 0.0230(19) 0.0102(19) C21 0.044(2) 0.049(2) 0.0272(19) 0.0086(18) 0.0201(18) 0.008(2) C22 0.033(2) 0.038(2) 0.0255(17) 0.0008(15) 0.0175(15) 0.0050(16) C23 0.0225(17) 0.0291(17) 0.0141(14) 0.0026(12) 0.0084(13) 0.0031(13) C24 0.0227(18) 0.0336(19) 0.0235(16) 0.0041(14) 0.0117(14) 0.0035(14) C25 0.0253(19) 0.037(2) 0.0330(19) 0.0025(16) 0.0157(16) -0.0036(16) C26 0.032(2) 0.0273(18) 0.0253(17) -0.0005(14) 0.0118(15) -0.0057(15) C27 0.035(2) 0.0319(19) 0.0250(17) -0.0041(15) 0.0154(16) 0.0008(16) C28 0.0237(18) 0.035(2) 0.0281(18) -0.0064(15) 0.0135(15) 0.0016(15) _refine_ls_extinction_method 'None' loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Pd1 . Br1 . 2.4629(4) yes Pd1 . Br1 5_656 2.5655(4) yes Pd1 . P1 . 2.2123(8) yes Pd1 . N1 . 2.039(3) yes P1 . C1 . 1.738(4) yes P1 . C17 . 1.820(4) yes P1 . C23 . 1.814(4) yes N1 . C2 . 1.351(4) yes N1 . C3 . 1.424(4) yes C1 . C2 . 1.379(4) yes C1 . H11 . 1.000 no C2 . C11 . 1.499(4) yes C3 . C4 . 1.409(5) yes C3 . C8 . 1.404(5) yes C4 . C5 . 1.405(5) yes C4 . C9 . 1.489(6) yes C5 . C6 . 1.378(8) yes C5 . H51 . 1.000 no C6 . C7 . 1.375(8) yes C6 . H61 . 1.000 no C7 . C8 . 1.394(6) yes C7 . H71 . 1.000 no C8 . C10 . 1.501(6) yes C9 . H91 . 1.000 no C9 . H92 . 1.000 no C9 . H93 . 1.000 no C10 . H101 . 1.000 no C10 . H102 . 1.000 no C10 . H103 . 1.000 no C11 . C12 . 1.392(5) yes C11 . C16 . 1.403(5) yes C12 . C13 . 1.393(5) yes C12 . H121 . 1.000 no C13 . C14 . 1.387(6) yes C13 . H131 . 1.000 no C14 . C15 . 1.383(6) yes C14 . H141 . 1.000 no C15 . C16 . 1.383(5) yes C15 . H151 . 1.000 no C16 . H161 . 1.000 no C17 . C18 . 1.396(5) yes C17 . C22 . 1.390(5) yes C18 . C19 . 1.400(6) yes C18 . H181 . 1.000 no C19 . C20 . 1.390(6) yes C19 . H191 . 1.000 no C20 . C21 . 1.380(7) yes C20 . H201 . 1.000 no C21 . C22 . 1.394(6) yes C21 . H211 . 1.000 no C22 . H221 . 1.000 no C23 . C24 . 1.392(5) yes C23 . C28 . 1.395(5) yes C24 . C25 . 1.394(5) yes C24 . H241 . 1.000 no C25 . C26 . 1.390(6) yes C25 . H251 . 1.000 no C26 . C27 . 1.386(6) yes C26 . H261 . 1.000 no C27 . C28 . 1.394(5) yes C27 . H271 . 1.000 no C28 . H281 . 1.000 no C29 . Cl1 . 1.761(6) yes C29 . Cl2 . 1.749(6) yes C29 . C30 . 0.40(2) yes C29 . Cl3 . 1.591(11) yes C29 . Cl4 . 1.91(1) yes C29 . H291 . 1.000 no C29 . H292 . 1.00 no C29 . H302 . 0.861 no Cl1 . C30 . 1.774(13) yes Cl1 . Cl3 . 0.829(9) yes Cl2 . C30 . 1.693(12) yes Cl2 . Cl4 . 0.653(9) yes C30 . Cl3 . 1.776(9) yes C30 . Cl4 . 1.767(9) yes C30 . H291 . 0.824 no C30 . H301 . 1.00 no C30 . H302 . 1.00 no H291 . H301 . 0.788 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag Br1 . Pd1 . Br1 5_656 84.937(14) yes Br1 . Pd1 . P1 . 93.77(2) yes Br1 5_656 Pd1 . P1 . 176.87(3) yes Br1 . Pd1 . N1 . 173.09(8) yes Br1 5_656 Pd1 . N1 . 97.98(7) yes P1 . Pd1 . N1 . 83.62(8) yes Pd1 . Br1 . Pd1 5_656 84.981(13) yes Pd1 . P1 . C1 . 102.03(11) yes Pd1 . P1 . C17 . 116.45(12) yes C1 . P1 . C17 . 108.88(17) yes Pd1 . P1 . C23 . 113.80(11) yes C1 . P1 . C23 . 110.79(18) yes C17 . P1 . C23 . 104.90(16) yes Pd1 . N1 . C2 . 117.5(2) yes Pd1 . N1 . C3 . 116.9(2) yes C2 . N1 . C3 . 122.1(3) yes P1 . C1 . C2 . 114.6(3) yes P1 . C1 . H11 . 122.7 no C2 . C1 . H11 . 122.7 no N1 . C2 . C1 . 121.2(3) yes N1 . C2 . C11 . 121.7(3) yes C1 . C2 . C11 . 117.0(3) yes N1 . C3 . C4 . 118.4(3) yes N1 . C3 . C8 . 120.3(3) yes C4 . C3 . C8 . 121.1(3) yes C3 . C4 . C5 . 117.9(4) yes C3 . C4 . C9 . 121.9(3) yes C5 . C4 . C9 . 120.2(4) yes C4 . C5 . C6 . 121.0(4) yes C4 . C5 . H51 . 119.5 no C6 . C5 . H51 . 119.5 no C5 . C6 . C7 . 120.4(4) yes C5 . C6 . H61 . 119.8 no C7 . C6 . H61 . 119.8 no C6 . C7 . C8 . 121.1(4) yes C6 . C7 . H71 . 119.4 no C8 . C7 . H71 . 119.4 no C3 . C8 . C7 . 118.5(4) yes C3 . C8 . C10 . 120.7(3) yes C7 . C8 . C10 . 120.7(4) yes C4 . C9 . H91 . 109.5 no C4 . C9 . H92 . 109.5 no H91 . C9 . H92 . 109.5 no C4 . C9 . H93 . 109.5 no H91 . C9 . H93 . 109.5 no H92 . C9 . H93 . 109.5 no C8 . C10 . H101 . 109.5 no C8 . C10 . H102 . 109.5 no H101 . C10 . H102 . 109.5 no C8 . C10 . H103 . 109.5 no H101 . C10 . H103 . 109.5 no H102 . C10 . H103 . 109.5 no C2 . C11 . C12 . 123.4(3) yes C2 . C11 . C16 . 118.3(3) yes C12 . C11 . C16 . 118.3(3) yes C11 . C12 . C13 . 120.5(3) yes C11 . C12 . H121 . 119.8 no C13 . C12 . H121 . 119.8 no C12 . C13 . C14 . 120.7(3) yes C12 . C13 . H131 . 119.6 no C14 . C13 . H131 . 119.6 no C13 . C14 . C15 . 119.0(3) yes C13 . C14 . H141 . 120.5 no C15 . C14 . H141 . 120.5 no C14 . C15 . C16 . 120.8(3) yes C14 . C15 . H151 . 119.6 no C16 . C15 . H151 . 119.6 no C11 . C16 . C15 . 120.7(3) yes C11 . C16 . H161 . 119.7 no C15 . C16 . H161 . 119.7 no P1 . C17 . C18 . 117.1(3) yes P1 . C17 . C22 . 123.1(3) yes C18 . C17 . C22 . 119.7(4) yes C17 . C18 . C19 . 119.9(4) yes C17 . C18 . H181 . 120.0 no C19 . C18 . H181 . 120.0 no C18 . C19 . C20 . 119.8(4) yes C18 . C19 . H191 . 120.1 no C20 . C19 . H191 . 120.1 no C19 . C20 . C21 . 120.3(4) yes C19 . C20 . H201 . 119.9 no C21 . C20 . H201 . 119.9 no C20 . C21 . C22 . 120.2(4) yes C20 . C21 . H211 . 119.9 no C22 . C21 . H211 . 119.9 no C17 . C22 . C21 . 120.1(4) yes C17 . C22 . H221 . 119.9 no C21 . C22 . H221 . 119.9 no P1 . C23 . C24 . 119.7(3) yes P1 . C23 . C28 . 120.8(3) yes C24 . C23 . C28 . 119.4(3) yes C23 . C24 . C25 . 120.3(3) yes C23 . C24 . H241 . 134.9 no C25 . C24 . H241 . 104.8 no C24 . C25 . C26 . 119.8(3) yes C24 . C25 . H251 . 120.1 no C26 . C25 . H251 . 120.1 no C25 . C26 . C27 . 120.4(3) yes C25 . C26 . H261 . 119.8 no C27 . C26 . H261 . 119.8 no C26 . C27 . C28 . 119.6(4) yes C26 . C27 . H271 . 120.2 no C28 . C27 . H271 . 120.2 no C23 . C28 . C27 . 120.4(3) yes C23 . C28 . H281 . 119.8 no C27 . C28 . H281 . 119.8 no Cl1 . C29 . Cl2 . 112.2(4) yes Cl1 . C29 . C30 . 85.4(26) yes Cl2 . C29 . C30 . 75.4(22) yes Cl1 . C29 . Cl3 . 28.0(4) yes Cl2 . C29 . Cl3 . 127.5(5) yes C30 . C29 . Cl3 . 111.4(26) yes Cl1 . C29 . Cl4 . 94.3(4) yes Cl2 . C29 . Cl4 . 20.0(3) yes C30 . C29 . Cl4 . 63.6(20) yes Cl3 . C29 . Cl4 . 114.5(5) yes Cl1 . C29 . H291 . 108.8 no Cl2 . C29 . H291 . 108.8 no C30 . C29 . H291 . 53.0 no Cl3 . C29 . H291 . 116.1 no Cl4 . C29 . H291 . 108.7 no Cl1 . C29 . H292 . 108.8 no Cl2 . C29 . H292 . 108.8 no C30 . C29 . H292 . 161.3 no Cl3 . C29 . H292 . 81.0 no Cl4 . C29 . H292 . 125.2 no Cl1 . C29 . H302 . 159.5 no Cl2 . C29 . H302 . 88.1 no C30 . C29 . H302 . 98.4 no Cl3 . C29 . H302 . 137.6 no Cl4 . C29 . H302 . 105.4 no H291 . C29 . H292 . 109.5 no H291 . C29 . H302 . 60.0 no H292 . C29 . H302 . 64.1 no C29 . Cl1 . C30 . 13.0(7) yes C29 . Cl1 . Cl3 . 64.5(6) yes C30 . Cl1 . Cl3 . 76.6(8) yes C29 . Cl2 . C30 . 13.2(7) yes C29 . Cl2 . Cl4 . 93.9(7) yes C30 . Cl2 . Cl4 . 85.6(9) yes C29 . C30 . Cl1 . 81.7(22) yes C29 . C30 . Cl2 . 91.4(26) yes Cl1 . C30 . Cl2 . 114.4(6) yes C29 . C30 . Cl3 . 56.5(21) yes Cl1 . C30 . Cl3 . 27.0(3) yes Cl2 . C30 . Cl3 . 119.4(8) yes C29 . C30 . Cl4 . 104.7(24) yes Cl1 . C30 . Cl4 . 98.9(6) yes Cl2 . C30 . Cl4 . 21.6(3) yes Cl3 . C30 . Cl4 . 112.6(6) yes C29 . C30 . H291 . 104.3 no Cl1 . C30 . H291 . 118.8 no Cl2 . C30 . H291 . 126.0 no Cl3 . C30 . H291 . 112.0 no Cl4 . C30 . H291 . 135.0 no C29 . C30 . H301 . 146.6 no Cl1 . C30 . H301 . 92.9 no Cl2 . C30 . H301 . 120.3 no Cl3 . C30 . H301 . 108.7 no Cl4 . C30 . H301 . 108.7 no C29 . C30 . H302 . 58.4 no Cl1 . C30 . H302 . 135.6 no Cl2 . C30 . H302 . 87.2 no Cl3 . C30 . H302 . 108.7 no Cl4 . C30 . H302 . 108.7 no H291 . C30 . H301 . 50.1 no H291 . C30 . H302 . 61.0 no H301 . C30 . H302 . 109.5 no C29 . Cl3 . Cl1 . 87.5(7) yes C29 . Cl3 . C30 . 12.1(8) yes Cl1 . Cl3 . C30 . 76.4(9) yes C29 . Cl4 . Cl2 . 66.1(7) yes C29 . Cl4 . C30 . 11.7(7) yes Cl2 . Cl4 . C30 . 72.7(9) yes C29 . H291 . C30 . 22.8 no C29 . H291 . H301 . 97.5 no C30 . H291 . H301 . 76.6 no C30 . H301 . H291 . 53.3 no C29 . H302 . C30 . 23.3 no #=end data_compound_8 _database_code_CSD 171182 _audit_creation_date 01-14-08 _audit_creation_method CRYSTALS_ver_12-03-99 # THIS IS THE DEFAULT SETTING FOR THE TITLE, PROVIDED WHEN NO # Check this file using the IUCr facility at: # http://www/iucr.ac.uk/iucr-top/journals/acta/c/services/checkcif.html #========================================================================== # Diffractometer details #========================================================================== _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ' Enraf-nonius DIP2000 ' _computing_data_collection 'DIP2000 software ,Xpress, MAC Science, 1989' _computing_data_reduction ; 'DIP2000 software DENZO, Otwinowski & Minor, 1996' ; _computing_cell_refinement ; 'DIP2000 software DENZO, Otwinowski & Minor, 1996' ; # end_choice #========================================================================== # General computing #========================================================================== _computing_structure_refinement ; CRYSTALS Issue 10 (Watkin, Prout, Carruthers & Betteridge, 1996) ; _computing_publication_material ; CRYSTALS Issue 10 (Watkin, Prout, Carruthers & Betteridge, 1996) ; _computing_molecular_graphics ; CAMERON (Watkin, Prout & Pearce, 1996) ; # choose one of the following two lines # _computing_structure_solution 'SHELXS86 (Sheldrick, 1986)' _computing_structure_solution 'SIR92 (Giacovazzo et al, 1992)' #========================================================================== _chemical_name_systematic # IUPAC name, in full ; ? ; _chemical_melting_point 'not measured' _refine_ls_matrix_type full _atom_sites_solution_primary direct # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap # choose from 'none, undef, noref, refall, refxyz, refU, constr, mixed' _refine_ls_hydrogen_treatment mixed _cell_length_a 11.0320(9) _cell_angle_alpha 99.511(5) _cell_length_b 12.1030(7) _cell_angle_beta 106.438(4) _cell_length_c 17.4530(14) _cell_angle_gamma 90.095(5) _cell_volume 2201.5 _symmetry_cell_setting 'Triclinic ' _symmetry_space_group_name_H-M 'P -1 ' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' '-x,-y,-z' loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source 'C ' 0.0020 0.0020 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International_Tables_Vol_IV_Table_2.2B' 'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7997 0.0030 'International_Tables_Vol_IV_Table_2.2B' 'Pd ' -1.1770 1.0070 19.3319 0.6987 15.5017 7.9893 5.2954 25.2052 0.6058 76.8986 5.2659 'International_Tables_Vol_IV_Table_2.2B' 'P ' 0.0900 0.0950 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645 1.1149 'International_Tables_Vol_IV_Table_2.2B' 'N ' 0.0040 0.0030 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International_Tables_Vol_IV_Table_2.2B' _chemical_formula_sum ' C54 H51 N1 P2 Pd1 ' _chemical_formula_moiety ' C54 H51 N1 P2 Pd1 ' _chemical_compound_source ; ? ; _chemical_formula_weight 882.35 _cell_measurement_reflns_used 20284 _cell_measurement_theta_min 0 _cell_measurement_theta_max 27 _cell_measurement_temperature 190 _cell_formula_units_Z 2 _exptl_crystal_description ' block ' _exptl_crystal_colour ' orange ' _exptl_crystal_size_min 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_max 0.20 _exptl_crystal_density_diffrn 1.331 _exptl_crystal_density_meas 'not measured' _exptl_crystal_F_000 914.130 _exptl_absorpt_coefficient_mu 0.532 # Sheldrick geometric definitions 0.90 0.90 _diffrn_measurement_method \w _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; Denzo/Scalepack (Otwinowski & Minor, 1996) ; _exptl_absorpt_correction_T_min 0.90 _exptl_absorpt_correction_T_max 0.90 _diffrn_standards_interval_time 0 _diffrn_standards_interval_count 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0.00 _diffrn_ambient_temperature 190 _diffrn_reflns_number 20284 _reflns_number_total 6812 _diffrn_reflns_av_R_equivalents 0.0264 # Number of reflections with Friedels Law is 6812 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 9111 _diffrn_measured_fraction_theta_max 0.748 _reflns_number_gt 6067 _diffrn_reflns_theta_min 1.93 _diffrn_reflns_theta_max 26.48 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _reflns_limit_h_min -13 _reflns_limit_h_max 13 _reflns_limit_k_min -14 _reflns_limit_k_max 13 _reflns_limit_l_min 0 _reflns_limit_l_max 21 _refine_diff_density_min -1.12 _refine_diff_density_max 0.75 _reflns_threshold_expression >3.00\s(I) _refine_ls_number_reflns 6067 _refine_ls_number_parameters 532 _refine_ls_R_factor_gt 0.0564 _refine_ls_wR_factor_ref 0.0264 _refine_ls_goodness_of_fit_ref 1.1317 _refine_ls_shift/su_max 0.008003 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Chebychev polynomial with 3 parameters, Carruthers & Watkin , 1979, 1.94 -1.82 1.38 ; _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71069 # Uequiv = arithmetic mean of Ui # i.e. Ueqiv = (U1+U2+U3)/3 loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_adp_type Pd1 0.18646(2) 0.25750(2) 0.767959(12) 0.0149 1.0000 Uani P2 0.37077(6) 0.35435(6) 0.85290(4) 0.0177 1.0000 Uani P32 0.13559(6) 0.35282(6) 0.66445(4) 0.0183 1.0000 Uani N11 0.2173(2) 0.1623(2) 0.86114(12) 0.0203 1.0000 Uani C3 0.5232(2) 0.3608(2) 0.83218(15) 0.0228 1.0000 Uani C4 0.6104(3) 0.4527(3) 0.86251(16) 0.0290 1.0000 Uani C5 0.7262(3) 0.4497(3) 0.84624(19) 0.0391 1.0000 Uani C6 0.7587(3) 0.3560(4) 0.8018(2) 0.0440 1.0000 Uani C7 0.6744(4) 0.2633(4) 0.7726(2) 0.0451 1.0000 Uani C8 0.5572(3) 0.2661(3) 0.78777(18) 0.0351 1.0000 Uani C9 0.3952(2) 0.2872(2) 0.93744(14) 0.0209 1.0000 Uani C10 0.3143(2) 0.1986(2) 0.93089(14) 0.0204 1.0000 Uani C12 0.1293(2) 0.0766(2) 0.85914(14) 0.0164 1.0000 Uani C13 0.1305(2) -0.0276(2) 0.81067(14) 0.0214 1.0000 Uani C14 0.0422(3) -0.1128(3) 0.80669(15) 0.0266 1.0000 Uani C15 -0.0473(3) -0.0942(3) 0.84840(17) 0.0325 1.0000 Uani C16 -0.0505(3) 0.0091(3) 0.89488(17) 0.0298 1.0000 Uani C17 0.0375(2) 0.0975(3) 0.90064(15) 0.0227 1.0000 Uani C18 0.0289(3) 0.2102(3) 0.94829(18) 0.0351 1.0000 Uani C19 0.2262(3) -0.0483(3) 0.76392(15) 0.0260 1.0000 Uani C20 0.3378(2) 0.1373(3) 1.00165(14) 0.0203 1.0000 Uani C21 0.3495(2) 0.0221(2) 0.99368(14) 0.0206 1.0000 Uani C22 0.3813(3) -0.0300(3) 1.06120(17) 0.0265 1.0000 Uani C23 0.4004(3) 0.0335(3) 1.13809(17) 0.0313 1.0000 Uani C24 0.3895(3) 0.1475(3) 1.14726(15) 0.0342 1.0000 Uani C25 0.3577(3) 0.2008(3) 1.07947(16) 0.0271 1.0000 Uani C26 0.3322(2) 0.4988(2) 0.88237(14) 0.0215 1.0000 Uani C27 0.3565(3) 0.5885(3) 0.84649(16) 0.0269 1.0000 Uani C28 0.3102(3) 0.6928(3) 0.86562(17) 0.0327 1.0000 Uani C29 0.2390(3) 0.7095(3) 0.91973(17) 0.0386 1.0000 Uani C30 0.2141(3) 0.6207(3) 0.95536(17) 0.0378 1.0000 Uani C31 0.2608(3) 0.5164(3) 0.93677(16) 0.0287 1.0000 Uani C33 0.0004(2) 0.4384(2) 0.66815(15) 0.0218 1.0000 Uani C34 0.0117(3) 0.5133(3) 0.74007(15) 0.0258 1.0000 Uani C35 -0.0855(3) 0.5820(3) 0.74809(18) 0.0324 1.0000 Uani C36 -0.1964(3) 0.5756(3) 0.6851(2) 0.0369 1.0000 Uani C37 -0.2100(3) 0.5000(3) 0.6143(2) 0.0377 1.0000 Uani C38 -0.1116(3) 0.4319(3) 0.60548(16) 0.0288 1.0000 Uani C39 0.2521(2) 0.4531(3) 0.65342(14) 0.0224 1.0000 Uani C40 0.3678(3) 0.4120(3) 0.64820(18) 0.0313 1.0000 Uani C41 0.4583(3) 0.4814(4) 0.6356(2) 0.0433 1.0000 Uani C42 0.4331(3) 0.5911(4) 0.6274(2) 0.0477 1.0000 Uani C43 0.3187(3) 0.6329(3) 0.63208(19) 0.0402 1.0000 Uani C44 0.2288(3) 0.5632(3) 0.64588(17) 0.0300 1.0000 Uani C45 0.0980(2) 0.2679(2) 0.56273(15) 0.0225 1.0000 Uani C46 0.1116(3) 0.1538(3) 0.55276(16) 0.0289 1.0000 Uani C47 0.0920(3) 0.0894(3) 0.47600(17) 0.0339 1.0000 Uani C48 0.0557(3) 0.1418(3) 0.40782(16) 0.0317 1.0000 Uani C49 0.0442(3) 0.2562(3) 0.41793(16) 0.0313 1.0000 Uani C50 0.0663(3) 0.3208(3) 0.49456(16) 0.0291 1.0000 Uani C51 0.0011(2) 0.1790(3) 0.71247(15) 0.0179 1.0000 Uani C52 0.3217(5) -0.1640(5) 0.4824(3) 0.0796 1.0000 Uani C53 0.3259(4) -0.1046(4) 0.5585(3) 0.0631 1.0000 Uani C54 0.4412(4) -0.0733(4) 0.6145(2) 0.0529 1.0000 Uani C55 0.5523(4) -0.0999(4) 0.5980(2) 0.0532 1.0000 Uani C56 0.6773(4) -0.0684(5) 0.6583(3) 0.0734 1.0000 Uani C57 0.4361(6) -0.1898(5) 0.4667(3) 0.0851 1.0000 Uani C58 0.5466(5) -0.1610(5) 0.5221(2) 0.0684 1.0000 Uani H511 0.017(4) 0.116(4) 0.702(2) 0.0500 1.0000 Uiso H512 -0.054(3) 0.216(3) 0.661(2) 0.0500 1.0000 Uiso H513 -0.036(3) 0.190(3) 0.755(2) 0.0500 1.0000 Uiso H41 0.5890 0.5225 0.8956 0.0600 1.0000 Uiso H51 0.7879 0.5179 0.8668 0.0471 1.0000 Uiso H61 0.8433 0.3548 0.7898 0.0570 1.0000 Uiso H71 0.6980 0.1932 0.7412 0.0564 1.0000 Uiso H81 0.4954 0.1984 0.7656 0.0600 1.0000 Uiso H91 0.4653 0.3140 0.9886 0.0600 1.0000 Uiso H141 0.0431 -0.1891 0.7723 0.0600 1.0000 Uiso H151 -0.1116 -0.1504 0.8445 0.0600 1.0000 Uiso H161 -0.1162 0.0229 0.9255 0.0600 1.0000 Uiso H181 -0.0420 0.2092 0.9741 0.0452 1.0000 Uiso H182 0.1099 0.2343 0.9922 0.0452 1.0000 Uiso H183 0.0111 0.2685 0.9116 0.0452 1.0000 Uiso H191 0.2131 -0.1275 0.7328 0.0600 1.0000 Uiso H192 0.3139 -0.0382 0.8020 0.0600 1.0000 Uiso H193 0.2163 0.0049 0.7246 0.0600 1.0000 Uiso H211 0.3370 -0.0245 0.9381 0.0600 1.0000 Uiso H221 0.3897 -0.1147 1.0536 0.0600 1.0000 Uiso H231 0.4207 -0.0045 1.1872 0.0600 1.0000 Uiso H241 0.4068 0.1918 1.2039 0.0600 1.0000 Uiso H251 0.3482 0.2856 1.0862 0.0600 1.0000 Uiso H271 0.4081 0.5769 0.8069 0.0600 1.0000 Uiso H281 0.3284 0.7571 0.8395 0.0600 1.0000 Uiso H291 0.2077 0.7866 0.9345 0.0600 1.0000 Uiso H301 0.1617 0.6313 0.9950 0.0600 1.0000 Uiso H311 0.2415 0.4518 0.9624 0.0600 1.0000 Uiso H341 0.0901 0.5156 0.7872 0.0600 1.0000 Uiso H351 -0.0750 0.6376 0.7997 0.0600 1.0000 Uiso H361 -0.2666 0.6276 0.6920 0.0600 1.0000 Uiso H371 -0.2921 0.4936 0.5694 0.0600 1.0000 Uiso H381 -0.1214 0.3787 0.5524 0.0600 1.0000 Uiso H401 0.3847 0.3300 0.6530 0.0600 1.0000 Uiso H411 0.5432 0.4505 0.6318 0.0509 1.0000 Uiso H421 0.4982 0.6402 0.6174 0.0551 1.0000 Uiso H431 0.2996 0.7151 0.6271 0.0501 1.0000 Uiso H441 0.1451 0.5929 0.6508 0.0600 1.0000 Uiso H461 0.1365 0.1171 0.6023 0.0600 1.0000 Uiso H471 0.1027 0.0045 0.4691 0.0600 1.0000 Uiso H481 0.0388 0.0968 0.3518 0.0600 1.0000 Uiso H491 0.0173 0.2929 0.3680 0.0600 1.0000 Uiso H501 0.0604 0.4052 0.5011 0.0600 1.0000 Uiso H521 0.2360 -0.1837 0.4410 0.0854 1.0000 Uiso H531 0.2451 -0.0870 0.5732 0.0718 1.0000 Uiso H541 0.4426 -0.0268 0.6691 0.0638 1.0000 Uiso H561 0.7481 -0.0939 0.6359 0.0793 1.0000 Uiso H562 0.6846 -0.0987 0.7093 0.0793 1.0000 Uiso H563 0.6882 0.0179 0.6742 0.0793 1.0000 Uiso H571 0.4342 -0.2333 0.4099 0.0938 1.0000 Uiso H581 0.6289 -0.1835 0.5095 0.0824 1.0000 Uiso 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 0.0174(1) 0.01323(13) 0.01238(9) 0.00448(7) 0.00054(7) -0.00062(7) P2 0.0215(3) 0.0148(4) 0.0153(3) 0.0043(3) 0.0017(2) -0.0009(3) P32 0.0218(3) 0.0168(5) 0.0147(3) 0.0062(3) 0.0007(3) -0.0009(3) N11 0.0248(12) 0.0185(16) 0.017(1) 0.0073(9) 0.0020(9) -0.0014(9) C3 0.0252(14) 0.0222(19) 0.0220(12) 0.0089(11) 0.005(1) 0.0033(11) C4 0.0277(15) 0.029(2) 0.0300(14) 0.0088(12) 0.0051(11) -0.0012(12) C5 0.0312(16) 0.047(3) 0.0418(17) 0.0150(15) 0.0102(13) -0.0013(14) C6 0.0371(18) 0.058(3) 0.0481(19) 0.0242(17) 0.0222(15) 0.0097(17) C7 0.052(2) 0.039(3) 0.0548(19) 0.0121(16) 0.0288(16) 0.0181(16) C8 0.0409(18) 0.028(2) 0.0370(16) 0.0033(13) 0.0130(13) 0.0061(14) C9 0.0245(13) 0.0183(18) 0.0162(11) 0.006(1) -0.001(1) -0.0028(11) C10 0.0225(13) 0.0210(18) 0.0155(11) 0.004(1) 0.001(1) 0.0034(11) C12 0.0167(12) 0.0201(17) 0.0139(11) 0.010(1) 0.0031(9) -0.001(1) C13 0.0248(14) 0.0220(19) 0.0144(11) 0.008(1) -0.002(1) 0.0003(11) C14 0.0313(15) 0.0193(19) 0.0237(12) 0.0077(11) -0.0030(11) -0.0079(12) C15 0.0288(15) 0.035(2) 0.0319(14) 0.0129(13) 0.0023(12) -0.0102(13) C16 0.0179(13) 0.047(2) 0.0278(13) 0.0149(13) 0.0077(11) -0.0007(12) C17 0.0194(13) 0.028(2) 0.0203(12) 0.0073(11) 0.003(1) 0.0029(11) C18 0.0363(17) 0.038(2) 0.0334(15) 0.0036(13) 0.0148(13) 0.0114(14) C19 0.0308(15) 0.026(2) 0.0207(12) 0.0036(11) 0.0068(11) 0.0055(12) C20 0.0167(12) 0.026(2) 0.0170(11) 0.007(1) 0.0010(9) -0.001(1) C21 0.0191(13) 0.0219(19) 0.0207(12) 0.0081(11) 0.003(1) 0.003(1) C22 0.0208(14) 0.028(2) 0.0317(14) 0.0135(12) 0.0047(11) 0.0030(11) C23 0.0299(16) 0.038(2) 0.0271(14) 0.0160(13) 0.0033(12) -0.0021(13) C24 0.0360(16) 0.047(3) 0.0168(12) 0.0072(12) 0.0014(11) -0.0052(14) C25 0.0325(15) 0.026(2) 0.0201(12) 0.0044(11) 0.0036(11) -0.0026(12) C26 0.0212(13) 0.0215(18) 0.0176(11) 0.005(1) -0.002(1) 0.000(1) C27 0.0240(14) 0.023(2) 0.0282(13) 0.0069(11) -0.0018(11) -0.0019(11) C28 0.0355(16) 0.021(2) 0.0314(14) 0.0065(12) -0.0084(12) -0.0034(13) C29 0.053(2) 0.020(2) 0.0294(15) -0.0017(12) -0.0061(14) 0.0117(14) C30 0.0468(19) 0.038(3) 0.0264(14) 0.0033(13) 0.0077(13) 0.0160(15) C31 0.0405(17) 0.022(2) 0.0217(12) 0.0024(11) 0.0060(11) 0.0081(12) C33 0.0219(13) 0.0191(18) 0.0250(12) 0.0099(11) 0.004(1) -0.002(1) C34 0.0264(14) 0.026(2) 0.0263(13) 0.0090(11) 0.0067(11) 0.0006(11) C35 0.0371(17) 0.024(2) 0.0421(16) 0.0094(13) 0.0190(13) 0.0033(13) C36 0.0256(15) 0.039(3) 0.0535(19) 0.0207(16) 0.0161(14) 0.0086(13) C37 0.0222(15) 0.046(3) 0.0447(17) 0.0196(16) 0.0025(13) 0.0022(14) C38 0.0220(14) 0.036(2) 0.0284(13) 0.0134(12) 0.0030(11) 0.0010(12) C39 0.0252(14) 0.029(2) 0.0128(11) 0.0093(11) 0.001(1) -0.0048(11) C40 0.0266(15) 0.035(2) 0.0341(15) 0.0125(13) 0.0079(12) 0.0006(13) C41 0.0286(17) 0.053(3) 0.052(2) 0.0147(17) 0.0145(15) -0.0012(16) C42 0.041(2) 0.053(3) 0.052(2) 0.0271(18) 0.0089(16) -0.0134(17) C43 0.0447(19) 0.032(2) 0.0439(17) 0.0190(15) 0.0054(14) -0.0071(15) C44 0.0361(16) 0.023(2) 0.0308(14) 0.0141(12) 0.0041(12) -0.0012(12) C45 0.0267(14) 0.017(2) 0.0218(12) 0.0062(11) 0.003(1) -0.0009(11) C46 0.0394(17) 0.026(2) 0.0208(12) 0.0085(11) 0.0046(11) 0.0014(12) C47 0.0496(19) 0.026(2) 0.0249(14) 0.0058(12) 0.0080(13) -0.0022(14) C48 0.0360(16) 0.035(2) 0.0199(13) 0.0002(12) 0.0034(11) 0.0011(13) C49 0.0424(17) 0.030(2) 0.0196(12) 0.0094(12) 0.0036(12) 0.0047(13) C50 0.0379(16) 0.028(2) 0.0190(12) 0.0081(12) 0.0020(11) 0.0030(13) C51 0.0206(13) 0.0197(18) 0.0162(11) 0.0100(11) 0.006(1) 0.0022(11) C52 0.085(4) 0.058(4) 0.074(3) 0.029(3) -0.022(3) -0.011(3) C53 0.057(2) 0.062(4) 0.071(3) 0.035(2) 0.006(2) 0.004(2) C54 0.064(3) 0.051(3) 0.048(2) 0.0160(17) 0.0173(18) 0.0066(19) C55 0.067(3) 0.047(3) 0.052(2) 0.0131(17) 0.0262(19) -0.0003(19) C56 0.068(3) 0.104(5) 0.053(2) 0.010(2) 0.027(2) -0.011(3) C57 0.110(5) 0.065(4) 0.063(3) 0.002(2) 0.003(3) -0.000(3) C58 0.089(3) 0.070(4) 0.049(2) 0.009(2) 0.024(2) 0.019(3) _refine_ls_extinction_method 'None' loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Pd1 . P2 . 2.3276(7) yes Pd1 . P32 . 2.2420(7) yes Pd1 . N11 . 2.097(2) yes Pd1 . C51 . 2.143(3) yes P2 . C3 . 1.821(3) yes P2 . C9 . 1.756(2) yes P2 . C26 . 1.825(3) yes P32 . C33 . 1.827(3) yes P32 . C39 . 1.836(3) yes P32 . C45 . 1.833(3) yes N11 . C10 . 1.380(3) yes N11 . C12 . 1.410(3) yes C3 . C4 . 1.399(4) yes C3 . C8 . 1.389(4) yes C4 . C5 . 1.385(4) yes C4 . H41 . 1.010(3) no C5 . C6 . 1.373(5) yes C5 . H51 . 1.018(4) no C6 . C7 . 1.386(6) yes C6 . H61 . 1.012(3) no C7 . C8 . 1.391(5) yes C7 . H71 . 1.008(4) no C8 . H81 . 1.014(3) no C9 . C10 . 1.363(4) yes C9 . H91 . 1.006(2) no C10 . C20 . 1.505(3) yes C12 . C13 . 1.399(4) yes C12 . C17 . 1.403(4) yes C13 . C14 . 1.397(4) yes C13 . C19 . 1.505(4) yes C14 . C15 . 1.382(4) yes C14 . H141 . 1.016(3) no C15 . C16 . 1.380(5) yes C15 . H151 . 0.962(3) no C16 . C17 . 1.415(4) yes C16 . H161 . 1.015(3) no C17 . C18 . 1.494(5) yes C18 . H181 . 1.008(3) no C18 . H182 . 1.005(3) no C18 . H183 . 1.012(3) no C19 . H191 . 1.008(3) no C19 . H192 . 1.001(3) no C19 . H193 . 1.000(3) no C20 . C21 . 1.388(4) yes C20 . C25 . 1.403(4) yes C21 . C22 . 1.386(4) yes C21 . H211 . 1.010(3) no C22 . C23 . 1.391(4) yes C22 . H221 . 1.020(3) no C23 . C24 . 1.372(5) yes C23 . H231 . 1.009(3) no C24 . C25 . 1.399(4) yes C24 . H241 . 1.009(3) no C25 . H251 . 1.023(3) no C26 . C27 . 1.401(4) yes C26 . C31 . 1.387(4) yes C27 . C28 . 1.388(5) yes C27 . H271 . 1.006(3) no C28 . C29 . 1.381(5) yes C28 . H281 . 1.011(3) no C29 . C30 . 1.391(5) yes C29 . H291 . 1.014(3) no C30 . C31 . 1.388(5) yes C30 . H301 . 1.013(3) no C31 . H311 . 1.013(3) no C33 . C34 . 1.396(4) yes C33 . C38 . 1.392(4) yes C34 . C35 . 1.382(4) yes C34 . H341 . 1.008(3) no C35 . C36 . 1.386(4) yes C35 . H351 . 1.008(3) no C36 . C37 . 1.382(5) yes C36 . H361 . 1.019(3) no C37 . C38 . 1.391(5) yes C37 . H371 . 1.010(3) no C38 . H381 . 1.015(3) no C39 . C40 . 1.392(4) yes C39 . C44 . 1.378(4) yes C40 . C41 . 1.391(5) yes C40 . H401 . 1.024(3) no C41 . C42 . 1.379(6) yes C41 . H411 . 1.024(4) no C42 . C43 . 1.379(5) yes C42 . H421 . 1.001(3) no C43 . C44 . 1.398(4) yes C43 . H431 . 1.030(4) no C44 . H441 . 1.012(3) no C45 . C46 . 1.377(5) yes C45 . C50 . 1.402(4) yes C46 . C47 . 1.393(4) yes C46 . H461 . 1.006(3) no C47 . C48 . 1.400(4) yes C47 . H471 . 1.025(4) no C48 . C49 . 1.376(5) yes C48 . H481 . 1.005(3) no C49 . C50 . 1.389(4) yes C49 . H491 . 1.014(3) no C50 . H501 . 1.013(3) no C51 . H511 . 0.79(4) no C51 . H512 . 1.09(4) no C51 . H513 . 0.93(4) no C52 . C53 . 1.391(8) yes C52 . C57 . 1.391(8) yes C52 . H521 . 1.014(5) no C53 . C54 . 1.374(6) yes C53 . H531 . 1.009(5) no C54 . C55 . 1.363(6) yes C54 . H541 . 1.021(4) no C55 . C56 . 1.482(6) yes C55 . C58 . 1.391(6) yes C56 . H561 . 0.996(5) no C56 . H562 . 1.000(4) no C56 . H563 . 1.033(6) no C57 . C58 . 1.328(7) yes C57 . H571 . 1.037(5) no C58 . H581 . 1.021(5) no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag P2 . Pd1 . P32 . 102.48(3) yes P2 . Pd1 . N11 . 82.42(6) yes P32 . Pd1 . N11 . 174.86(7) yes P2 . Pd1 . C51 . 167.27(7) yes P32 . Pd1 . C51 . 83.95(7) yes N11 . Pd1 . C51 . 90.95(9) yes Pd1 . P2 . C3 . 126.55(9) yes Pd1 . P2 . C9 . 100.37(9) yes C3 . P2 . C9 . 106.04(12) yes Pd1 . P2 . C26 . 107.75(8) yes C3 . P2 . C26 . 106.80(13) yes C9 . P2 . C26 . 108.12(13) yes Pd1 . P32 . C33 . 110.95(8) yes Pd1 . P32 . C39 . 119.87(8) yes C33 . P32 . C39 . 103.01(13) yes Pd1 . P32 . C45 . 115.8(1) yes C33 . P32 . C45 . 107.18(12) yes C39 . P32 . C45 . 98.36(12) yes Pd1 . N11 . C10 . 117.66(18) yes Pd1 . N11 . C12 . 121.18(15) yes C10 . N11 . C12 . 120.2(2) yes P2 . C3 . C4 . 123.8(2) yes P2 . C3 . C8 . 117.6(2) yes C4 . C3 . C8 . 118.5(3) yes C3 . C4 . C5 . 120.3(3) yes C3 . C4 . H41 . 120.4(3) no C5 . C4 . H41 . 119.3(3) no C4 . C5 . C6 . 120.8(3) yes C4 . C5 . H51 . 119.8(4) no C6 . C5 . H51 . 119.3(3) no C5 . C6 . C7 . 119.6(3) yes C5 . C6 . H61 . 120.2(4) no C7 . C6 . H61 . 120.2(4) no C6 . C7 . C8 . 120.0(4) yes C6 . C7 . H71 . 120.5(4) no C8 . C7 . H71 . 119.5(4) no C3 . C8 . C7 . 120.8(3) yes C3 . C8 . H81 . 119.6(3) no C7 . C8 . H81 . 119.6(3) no P2 . C9 . C10 . 117.06(18) yes P2 . C9 . H91 . 121.1(2) no C10 . C9 . H91 . 121.9(2) no N11 . C10 . C9 . 122.0(2) yes N11 . C10 . C20 . 120.5(2) yes C9 . C10 . C20 . 117.5(2) yes N11 . C12 . C13 . 118.4(2) yes N11 . C12 . C17 . 120.6(3) yes C13 . C12 . C17 . 120.9(2) yes C12 . C13 . C14 . 119.1(3) yes C12 . C13 . C19 . 120.7(2) yes C14 . C13 . C19 . 120.2(3) yes C13 . C14 . C15 . 120.7(3) yes C13 . C14 . H141 . 119.7(3) no C15 . C14 . H141 . 119.5(3) no C14 . C15 . C16 . 120.3(3) yes C14 . C15 . H151 . 122.2(3) no C16 . C15 . H151 . 117.4(3) no C15 . C16 . C17 . 120.7(3) yes C15 . C16 . H161 . 120.4(3) no C17 . C16 . H161 . 118.9(3) no C12 . C17 . C16 . 118.2(3) yes C12 . C17 . C18 . 121.9(3) yes C16 . C17 . C18 . 119.9(3) yes C17 . C18 . H181 . 110.6(3) no C17 . C18 . H182 . 111.3(3) no H181 . C18 . H182 . 108.5(3) no C17 . C18 . H183 . 110.3(2) no H181 . C18 . H183 . 107.9(3) no H182 . C18 . H183 . 108.2(3) no C13 . C19 . H191 . 109.6(3) no C13 . C19 . H192 . 110.1(2) no H191 . C19 . H192 . 108.8(3) no C13 . C19 . H193 . 110.2(2) no H191 . C19 . H193 . 108.8(2) no H192 . C19 . H193 . 109.4(3) no C10 . C20 . C21 . 122.7(2) yes C10 . C20 . C25 . 118.2(3) yes C21 . C20 . C25 . 118.9(2) yes C20 . C21 . C22 . 121.0(3) yes C20 . C21 . H211 . 119.8(2) no C22 . C21 . H211 . 119.2(3) no C21 . C22 . C23 . 119.7(3) yes C21 . C22 . H221 . 119.3(3) no C23 . C22 . H221 . 121.0(3) no C22 . C23 . C24 . 120.2(3) yes C22 . C23 . H231 . 119.9(3) no C24 . C23 . H231 . 119.9(3) no C23 . C24 . C25 . 120.4(3) yes C23 . C24 . H241 . 118.5(3) no C25 . C24 . H241 . 121.0(3) no C20 . C25 . C24 . 119.7(3) yes C20 . C25 . H251 . 119.8(3) no C24 . C25 . H251 . 120.5(3) no P2 . C26 . C27 . 124.2(2) yes P2 . C26 . C31 . 116.7(2) yes C27 . C26 . C31 . 118.7(3) yes C26 . C27 . C28 . 120.3(3) yes C26 . C27 . H271 . 119.5(3) no C28 . C27 . H271 . 120.2(3) no C27 . C28 . C29 . 120.6(3) yes C27 . C28 . H281 . 119.7(3) no C29 . C28 . H281 . 119.7(3) no C28 . C29 . C30 . 119.4(3) yes C28 . C29 . H291 . 120.0(3) no C30 . C29 . H291 . 120.6(3) no C29 . C30 . C31 . 120.2(3) yes C29 . C30 . H301 . 120.6(3) no C31 . C30 . H301 . 119.3(3) no C26 . C31 . C30 . 120.8(3) yes C26 . C31 . H311 . 119.3(3) no C30 . C31 . H311 . 119.9(3) no P32 . C33 . C34 . 116.53(19) yes P32 . C33 . C38 . 124.5(2) yes C34 . C33 . C38 . 118.9(3) yes C33 . C34 . C35 . 120.5(3) yes C33 . C34 . H341 . 119.8(3) no C35 . C34 . H341 . 119.6(3) no C34 . C35 . C36 . 120.2(3) yes C34 . C35 . H351 . 119.8(3) no C36 . C35 . H351 . 120.0(3) no C35 . C36 . C37 . 119.9(3) yes C35 . C36 . H361 . 119.0(3) no C37 . C36 . H361 . 121.1(3) no C36 . C37 . C38 . 120.1(3) yes C36 . C37 . H371 . 119.6(3) no C38 . C37 . H371 . 120.3(4) no C33 . C38 . C37 . 120.3(3) yes C33 . C38 . H381 . 120.2(3) no C37 . C38 . H381 . 119.4(3) no P32 . C39 . C40 . 117.0(2) yes P32 . C39 . C44 . 123.9(2) yes C40 . C39 . C44 . 119.0(3) yes C39 . C40 . C41 . 120.3(3) yes C39 . C40 . H401 . 119.1(3) no C41 . C40 . H401 . 120.6(3) no C40 . C41 . C42 . 120.0(3) yes C40 . C41 . H411 . 119.8(4) no C42 . C41 . H411 . 120.2(3) no C41 . C42 . C43 . 120.4(3) yes C41 . C42 . H421 . 119.5(4) no C43 . C42 . H421 . 120.1(4) no C42 . C43 . C44 . 119.3(3) yes C42 . C43 . H431 . 121.0(3) no C44 . C43 . H431 . 119.6(3) no C39 . C44 . C43 . 120.9(3) yes C39 . C44 . H441 . 118.6(3) no C43 . C44 . H441 . 120.5(3) no P32 . C45 . C46 . 120.63(19) yes P32 . C45 . C50 . 119.6(2) yes C46 . C45 . C50 . 119.5(3) yes C45 . C46 . C47 . 121.3(3) yes C45 . C46 . H461 . 118.7(3) no C47 . C46 . H461 . 120.0(3) no C46 . C47 . C48 . 119.1(3) yes C46 . C47 . H471 . 120.8(3) no C48 . C47 . H471 . 120.1(3) no C47 . C48 . C49 . 119.6(3) yes C47 . C48 . H481 . 120.5(3) no C49 . C48 . H481 . 119.9(3) no C48 . C49 . C50 . 121.3(3) yes C48 . C49 . H491 . 118.7(3) no C50 . C49 . H491 . 119.9(3) no C45 . C50 . C49 . 119.2(3) yes C45 . C50 . H501 . 120.4(3) no C49 . C50 . H501 . 120.4(3) no Pd1 . C51 . H511 . 101.1(28) no Pd1 . C51 . H512 . 113.2(20) no H511 . C51 . H512 . 115.4(34) no Pd1 . C51 . H513 . 102.7(22) no H511 . C51 . H513 . 111.8(37) no H512 . C51 . H513 . 111.5(31) no C53 . C52 . C57 . 117.7(4) yes C53 . C52 . H521 . 118.4(6) no C57 . C52 . H521 . 123.8(6) no C52 . C53 . C54 . 119.4(5) yes C52 . C53 . H531 . 120.3(5) no C54 . C53 . H531 . 120.3(5) no C53 . C54 . C55 . 122.0(4) yes C53 . C54 . H541 . 118.3(4) no C55 . C54 . H541 . 119.7(4) no C54 . C55 . C56 . 122.5(4) yes C54 . C55 . C58 . 118.0(4) yes C56 . C55 . C58 . 119.4(4) yes C55 . C56 . H561 . 111.7(4) no C55 . C56 . H562 . 111.6(4) no H561 . C56 . H562 . 109.8(5) no C55 . C56 . H563 . 109.5(5) no H561 . C56 . H563 . 107.2(4) no H562 . C56 . H563 . 106.9(4) no C52 . C57 . C58 . 122.1(5) yes C52 . C57 . H571 . 118.5(5) no C58 . C57 . H571 . 119.4(6) no C55 . C58 . C57 . 120.8(5) yes C55 . C58 . H581 . 119.0(4) no C57 . C58 . H581 . 120.2(5) no