Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_B111487P _database_code_CSD 177302 _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Andersson, Carlaxel' 'Sjovall, Sven' 'Wendt, Ola F.' _publ_contact_author_name 'Prof Carlaxel Andersson' _publ_contact_author_address ; Inorganic Chemistry 1, Chemical Centre Lund University PO Box 124 S 221 00 Lund SWEDEN ; _publ_contact_author_email 'CARLAXEL.ANDERSSON@INORG.LU.SE' _publ_section_title ; Synthesis, characterisation and catalytic investigation of a new type of PC (sp3) P pincer Pd (II) complex ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H49 I P2 Pd' _chemical_formula_weight 632.87 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' 'I' 'I' -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.102(2) _cell_length_b 15.035(3) _cell_length_c 15.875(3) _cell_angle_alpha 90.00 _cell_angle_beta 100.27(3) _cell_angle_gamma 90.00 _cell_volume 2842.3(10) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5959 _cell_measurement_theta_min 4.363 _cell_measurement_theta_max 49.994 _exptl_crystal_description 'prism' _exptl_crystal_colour transparent _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.479 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1288 _exptl_absorpt_coefficient_mu 1.860 _exptl_absorpt_correction_type 'empirical' _exptl_absorpt_correction_T_min 0.6624 _exptl_absorpt_correction_T_max 0.7904 _exptl_absorpt_process_details 'absorption corrections using SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 512 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.0 _diffrn_reflns_number 29034 _diffrn_reflns_av_R_equivalents 0.0692 _diffrn_reflns_av_sigmaI/netI 0.0931 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.88 _diffrn_reflns_theta_max 32.00 _reflns_number_total 8936 _reflns_number_gt 4782 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond (Brandenburg)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^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 'riding model' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8936 _refine_ls_number_parameters 253 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1107 _refine_ls_R_factor_gt 0.0448 _refine_ls_wR_factor_ref 0.1566 _refine_ls_wR_factor_gt 0.1303 _refine_ls_goodness_of_fit_ref 0.824 _refine_ls_restrained_S_all 0.824 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd Pd 0.39713(3) 0.43565(2) 0.24972(2) 0.03258(11) Uani 1 1 d . . . I I 0.36700(3) 0.31025(2) 0.36750(2) 0.04734(12) Uani 1 1 d . . . P1 P 0.59282(10) 0.43624(9) 0.28165(9) 0.0393(3) Uani 1 1 d . . . P2 P 0.20821(10) 0.45388(8) 0.18870(8) 0.0356(3) Uani 1 1 d . . . C1 C 0.3234(4) 0.5862(3) 0.1225(3) 0.0418(12) Uani 1 1 d . . . H1 H 0.3199 0.6271 0.1700 0.050 Uiso 1 1 calc R . . C2 C 0.4212(4) 0.5233(3) 0.1509(3) 0.0415(11) Uani 1 1 d . . . H2 H 0.4254 0.4855 0.1013 0.050 Uiso 1 1 calc R . . C3 C 0.5330(5) 0.5738(4) 0.1694(3) 0.0455(12) Uani 1 1 d . . . H3 H 0.5301 0.6156 0.2163 0.055 Uiso 1 1 calc R . . C4 C 0.5489(5) 0.6274(4) 0.0899(4) 0.0594(16) Uani 1 1 d . . . H4A H 0.6185 0.6608 0.1027 0.071 Uiso 1 1 calc R . . H4B H 0.5546 0.5868 0.0434 0.071 Uiso 1 1 calc R . . C5 C 0.4530(7) 0.6906(4) 0.0621(4) 0.072(2) Uani 1 1 d . . . H5A H 0.4641 0.7211 0.0104 0.086 Uiso 1 1 calc R . . H5B H 0.4521 0.7350 0.1064 0.086 Uiso 1 1 calc R . . C6 C 0.3414(5) 0.6425(4) 0.0454(3) 0.0523(14) Uani 1 1 d . . . H6A H 0.3384 0.6042 -0.0042 0.063 Uiso 1 1 calc R . . H6B H 0.2813 0.6857 0.0325 0.063 Uiso 1 1 calc R . . C7 C 0.6288(5) 0.5100(4) 0.1973(4) 0.0515(14) Uani 1 1 d . . . H7A H 0.6968 0.5429 0.2193 0.062 Uiso 1 1 calc R . . H7B H 0.6420 0.4748 0.1489 0.062 Uiso 1 1 calc R . . C8 C 0.2126(4) 0.5366(4) 0.1038(3) 0.0461(12) Uani 1 1 d . . . H8A H 0.2050 0.5071 0.0488 0.055 Uiso 1 1 calc R . . H8B H 0.1509 0.5782 0.1016 0.055 Uiso 1 1 calc R . . C9 C 0.6619(5) 0.4888(4) 0.3859(3) 0.0506(14) Uani 1 1 d . . . C10 C 0.6629(5) 0.3265(4) 0.2625(4) 0.0558(15) Uani 1 1 d . . . C11 C 0.1410(5) 0.3535(4) 0.1283(3) 0.0509(14) Uani 1 1 d . . . C12 C 0.1151(4) 0.5063(3) 0.2582(3) 0.0437(12) Uani 1 1 d . . . C13 C 0.7919(5) 0.4954(6) 0.3971(5) 0.091(3) Uani 1 1 d . . . C14 C 0.6125(7) 0.5841(4) 0.3850(5) 0.082(2) Uani 1 1 d . . . C15 C 0.6288(6) 0.4417(4) 0.4635(4) 0.0653(17) Uani 1 1 d . . . C16 C 0.7786(5) 0.3396(5) 0.2375(5) 0.079(2) Uani 1 1 d . . . C17 C 0.5813(6) 0.2828(4) 0.1850(5) 0.0709(19) Uani 1 1 d . . . C18 C 0.6730(5) 0.2634(5) 0.3404(5) 0.0689(18) Uani 1 1 d . . . C19 C 0.0381(6) 0.3783(5) 0.0566(4) 0.079(2) Uani 1 1 d . . . C20 C 0.2357(6) 0.3100(4) 0.0881(5) 0.074(2) Uani 1 1 d . . . C21 C 0.1006(6) 0.2854(4) 0.1881(5) 0.073(2) Uani 1 1 d . . . C22 C -0.0005(5) 0.5356(5) 0.2089(5) 0.0691(18) Uani 1 1 d . . . C23 C 0.1814(6) 0.5909(4) 0.2974(4) 0.0642(17) Uani 1 1 d . . . C24 C 0.0995(5) 0.4459(4) 0.3337(4) 0.0650(18) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.02988(19) 0.0329(2) 0.03349(19) 0.00267(15) 0.00178(13) -0.00175(15) I1 0.0447(2) 0.0466(2) 0.0484(2) 0.01413(15) 0.00216(15) -0.00278(15) P1 0.0303(6) 0.0459(8) 0.0410(7) -0.0020(6) 0.0046(5) -0.0029(6) P2 0.0317(6) 0.0328(6) 0.0391(6) 0.0020(5) -0.0026(5) -0.0007(5) C1 0.049(3) 0.038(3) 0.038(3) 0.002(2) 0.007(2) -0.003(2) C2 0.051(3) 0.036(3) 0.038(3) 0.002(2) 0.010(2) -0.002(2) C3 0.051(3) 0.046(3) 0.040(3) 0.000(2) 0.010(2) -0.014(2) C4 0.069(4) 0.055(4) 0.057(4) -0.001(3) 0.020(3) -0.024(3) C5 0.112(6) 0.055(4) 0.051(4) 0.014(3) 0.021(4) -0.019(4) C6 0.072(4) 0.046(3) 0.039(3) 0.005(2) 0.011(3) 0.006(3) C7 0.042(3) 0.064(4) 0.049(3) -0.002(3) 0.012(2) -0.017(3) C8 0.050(3) 0.043(3) 0.042(3) 0.006(2) 0.001(2) 0.005(2) C9 0.046(3) 0.060(4) 0.042(3) -0.005(3) -0.004(2) -0.013(3) C10 0.042(3) 0.059(4) 0.069(4) -0.012(3) 0.015(3) 0.004(3) C11 0.052(3) 0.042(3) 0.049(3) -0.004(2) -0.016(3) -0.005(2) C12 0.039(3) 0.038(3) 0.054(3) 0.006(2) 0.007(2) 0.005(2) C13 0.035(3) 0.154(8) 0.078(5) -0.027(5) -0.006(3) -0.025(4) C14 0.127(7) 0.049(4) 0.061(4) -0.015(3) -0.004(4) 0.008(4) C15 0.071(4) 0.077(5) 0.044(3) 0.008(3) 0.002(3) -0.010(3) C16 0.044(4) 0.091(5) 0.109(6) -0.010(5) 0.031(4) 0.011(4) C17 0.068(4) 0.063(4) 0.080(5) -0.029(4) 0.009(4) -0.006(3) C18 0.056(4) 0.064(4) 0.083(5) 0.010(4) 0.002(3) 0.021(3) C19 0.075(5) 0.063(4) 0.078(5) -0.009(3) -0.040(4) 0.003(3) C20 0.076(5) 0.057(4) 0.085(5) -0.027(4) 0.002(4) -0.001(3) C21 0.072(4) 0.050(4) 0.090(5) 0.005(4) -0.008(4) -0.026(3) C22 0.036(3) 0.087(5) 0.081(4) 0.005(4) 0.000(3) 0.021(3) C23 0.074(4) 0.054(4) 0.067(4) -0.019(3) 0.019(3) -0.011(3) C24 0.057(4) 0.067(4) 0.077(4) 0.030(3) 0.027(3) 0.009(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd C2 2.108(5) . ? Pd P1 2.3318(14) . ? Pd P2 2.3348(14) . ? Pd I 2.7252(6) . ? P1 C7 1.849(6) . ? P1 C9 1.889(5) . ? P1 C10 1.905(6) . ? P2 C8 1.842(5) . ? P2 C12 1.884(5) . ? P2 C11 1.892(5) . ? C1 C8 1.516(7) . ? C1 C2 1.520(7) . ? C1 C6 1.535(7) . ? C7 C3 1.509(8) . ? C2 C3 1.533(7) . ? C3 C4 1.538(7) . ? C4 C5 1.503(9) . ? C5 C6 1.513(9) . ? C12 C22 1.540(7) . ? C12 C24 1.542(8) . ? C12 C23 1.573(8) . ? C10 C16 1.534(8) . ? C10 C18 1.546(9) . ? C10 C17 1.577(9) . ? C11 C21 1.535(9) . ? C11 C20 1.551(9) . ? C11 C19 1.575(7) . ? C9 C15 1.535(8) . ? C9 C14 1.551(9) . ? C9 C13 1.555(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 Pd P1 83.66(14) . . ? C2 Pd P2 82.70(14) . . ? P1 Pd P2 166.22(5) . . ? C2 Pd I 174.88(14) . . ? P1 Pd I 96.22(4) . . ? P2 Pd I 97.18(4) . . ? C7 P1 C9 105.0(3) . . ? C7 P1 C10 103.6(3) . . ? C9 P1 C10 111.2(3) . . ? C7 P1 Pd 101.89(18) . . ? C9 P1 Pd 117.76(19) . . ? C10 P1 Pd 115.22(19) . . ? C8 P2 C12 104.1(2) . . ? C8 P2 C11 103.5(2) . . ? C12 P2 C11 112.5(3) . . ? C8 P2 Pd 103.22(18) . . ? C12 P2 Pd 116.73(17) . . ? C11 P2 Pd 114.65(18) . . ? C8 C1 C2 111.5(4) . . ? C8 C1 C6 111.2(4) . . ? C2 C1 C6 111.5(4) . . ? C3 C7 P1 109.0(4) . . ? C1 C2 C3 111.2(4) . . ? C1 C2 Pd 114.0(3) . . ? C3 C2 Pd 113.7(3) . . ? C7 C3 C2 110.3(4) . . ? C7 C3 C4 111.9(5) . . ? C2 C3 C4 109.8(4) . . ? C1 C8 P2 109.2(3) . . ? C5 C4 C3 111.6(5) . . ? C4 C5 C6 111.6(5) . . ? C5 C6 C1 111.9(5) . . ? C22 C12 C24 109.7(5) . . ? C22 C12 C23 108.8(5) . . ? C24 C12 C23 107.0(5) . . ? C22 C12 P2 114.0(4) . . ? C24 C12 P2 112.2(4) . . ? C23 C12 P2 104.7(4) . . ? C16 C10 C18 109.9(5) . . ? C16 C10 C17 109.0(5) . . ? C18 C10 C17 108.4(6) . . ? C16 C10 P1 112.5(5) . . ? C18 C10 P1 112.2(4) . . ? C17 C10 P1 104.5(4) . . ? C21 C11 C20 108.3(5) . . ? C21 C11 C19 107.9(5) . . ? C20 C11 C19 110.5(5) . . ? C21 C11 P2 111.9(4) . . ? C20 C11 P2 105.2(4) . . ? C19 C11 P2 113.0(4) . . ? C15 C9 C14 106.1(5) . . ? C15 C9 C13 109.9(5) . . ? C14 C9 C13 108.8(6) . . ? C15 C9 P1 111.9(4) . . ? C14 C9 P1 105.6(4) . . ? C13 C9 P1 114.1(4) . . ? _diffrn_measured_fraction_theta_max 0.905 _diffrn_reflns_theta_full 32.00 _diffrn_measured_fraction_theta_full 0.905 _refine_diff_density_max 0.669 _refine_diff_density_min -0.682 _refine_diff_density_rms 0.131