Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Pedro A Aguirre' _publ_contact_author_address ; Facultad de Ciencias Universidad de Chile Santiago 1 Casilla 233 CHILE ; _publ_contact_author_email PEDRO.AGUIRRE@UAB.ES _publ_section_title ; Methoxycarbonylation of olefins catalyzed by palladium complexes bearing P-, N-donor ligands ; loop_ _publ_author_name 'Pedro A. Aguirre' 'Joan Carles Bayon' 'Carolina Lagos' 'Sergio A. Moya' 'Gabriel Peris' 'Eduardo Sola' ; C.Vera-Oyarce ; 'Cesar Zuniga' data_str841m _database_code_depnum_ccdc_archive 'CCDC 629175' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C37 H30 Cl6 N2 P2 Pd' _chemical_formula_weight 883.67 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.6006(7) _cell_length_b 13.8728(10) _cell_length_c 15.8526(11) _cell_angle_alpha 94.061(2) _cell_angle_beta 95.855(2) _cell_angle_gamma 99.201(2) _cell_volume 2065.1(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.421 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 888 _exptl_absorpt_coefficient_mu 0.942 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8555 _exptl_absorpt_correction_T_max 0.9456 _exptl_absorpt_process_details ? _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_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11899 _diffrn_reflns_av_R_equivalents 0.0725 _diffrn_reflns_av_sigmaI/netI 0.1703 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.49 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7270 _reflns_number_gt 3717 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.1424P)^2^+5.2921P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7270 _refine_ls_number_parameters 451 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1774 _refine_ls_R_factor_gt 0.0858 _refine_ls_wR_factor_ref 0.2871 _refine_ls_wR_factor_gt 0.2292 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.031 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C31 C 0.8668(17) 0.8880(13) 0.9648(10) 0.072(5) Uani 1 1 d . . . H31 H 0.9376 0.8620 0.9956 0.086 Uiso 1 1 calc R . . Pd1 Pd 0.95107(10) 0.80983(7) 0.69077(6) 0.0322(3) Uani 1 1 d . . . P2 P 0.7936(3) 0.6953(2) 0.61016(18) 0.0308(7) Uani 1 1 d . . . P3 P 0.9070(3) 0.7647(2) 0.82275(18) 0.0338(8) Uani 1 1 d . . . N1 N 1.0041(10) 0.8511(7) 0.5711(6) 0.036(2) Uani 1 1 d . . . C24 C 1.1168(12) 0.9179(9) 0.5606(8) 0.040(3) Uani 1 1 d . . . H24 H 1.1757 0.9483 0.6085 0.049 Uiso 1 1 calc R . . C20 C 0.9215(12) 0.8078(9) 0.5022(7) 0.032(3) Uani 1 1 d . . . C1 C 0.8163(12) 0.5701(9) 0.5974(7) 0.033(3) Uani 1 1 d . . . C30 C 0.8311(14) 0.8593(9) 0.8776(8) 0.043(3) Uani 1 1 d . . . C2 C 0.7072(14) 0.4960(9) 0.5657(8) 0.047(3) Uani 1 1 d . . . H2 H 0.6166 0.5102 0.5520 0.057 Uiso 1 1 calc R . . C21 C 0.9467(13) 0.8316(9) 0.4198(7) 0.037(3) Uani 1 1 d . . . H21 H 0.8855 0.8024 0.3724 0.044 Uiso 1 1 calc R . . C4 C 0.863(2) 0.3779(13) 0.5714(11) 0.081(5) Uani 1 1 d . . . H4 H 0.8788 0.3137 0.5631 0.097 Uiso 1 1 calc R . . C11 C 0.5662(15) 0.7901(11) 0.6082(10) 0.063(4) Uani 1 1 d . . . H11 H 0.6258 0.8380 0.5847 0.076 Uiso 1 1 calc R . . C22 C 1.0617(15) 0.8978(10) 0.4115(8) 0.048(4) Uani 1 1 d . . . H22 H 1.0826 0.9129 0.3575 0.058 Uiso 1 1 calc R . . C15 C 0.5217(12) 0.6349(10) 0.6623(8) 0.041(3) Uani 1 1 d . . . H15 H 0.5511 0.5766 0.6758 0.049 Uiso 1 1 calc R . . C10 C 0.6128(12) 0.7024(9) 0.6264(7) 0.034(3) Uani 1 1 d . . . C6 C 0.9508(14) 0.5490(11) 0.6160(8) 0.050(4) Uani 1 1 d . . . H6 H 1.0253 0.5988 0.6377 0.060 Uiso 1 1 calc R . . C40 C 1.0652(13) 0.7446(10) 0.8858(7) 0.041(3) Uani 1 1 d . . . C23 C 1.1484(14) 0.9432(10) 0.4815(8) 0.043(3) Uani 1 1 d . . . H23 H 1.2270 0.9901 0.4758 0.052 Uiso 1 1 calc R . . C14 C 0.3899(15) 0.6498(12) 0.6792(9) 0.061(4) Uani 1 1 d . . . H14 H 0.3307 0.6019 0.7030 0.074 Uiso 1 1 calc R . . C3 C 0.7311(19) 0.3982(11) 0.5534(10) 0.068(4) Uani 1 1 d . . . H3 H 0.6561 0.3482 0.5331 0.081 Uiso 1 1 calc R . . C50 C 0.7865(13) 0.6519(9) 0.8291(7) 0.039(3) Uani 1 1 d . . . C55 C 0.6547(13) 0.6496(11) 0.8624(8) 0.050(4) Uani 1 1 d . . . H55 H 0.6252 0.7075 0.8806 0.061 Uiso 1 1 calc R . . C51 C 0.8244(15) 0.5647(9) 0.8026(8) 0.047(3) Uani 1 1 d . . . H51 H 0.9117 0.5654 0.7819 0.056 Uiso 1 1 calc R . . C52 C 0.7392(17) 0.4772(11) 0.8055(9) 0.060(4) Uani 1 1 d . . . H52 H 0.7675 0.4194 0.7858 0.071 Uiso 1 1 calc R . . C35 C 0.726(2) 0.8965(13) 0.8327(12) 0.085(6) Uani 1 1 d . . . H35 H 0.6986 0.8775 0.7752 0.101 Uiso 1 1 calc R . . C5 C 0.9756(19) 0.4523(13) 0.6022(10) 0.068(5) Uani 1 1 d . . . H5 H 1.0667 0.4382 0.6137 0.082 Uiso 1 1 calc R . . C13 C 0.3448(17) 0.7362(14) 0.6608(11) 0.073(5) Uani 1 1 d . . . H13 H 0.2554 0.7470 0.6728 0.088 Uiso 1 1 calc R . . C12 C 0.4321(17) 0.8066(12) 0.6247(11) 0.072(5) Uani 1 1 d . . . H12 H 0.4016 0.8647 0.6116 0.087 Uiso 1 1 calc R . . C53 C 0.6111(18) 0.4743(13) 0.8376(10) 0.069(5) Uani 1 1 d . . . H53 H 0.5517 0.4147 0.8389 0.083 Uiso 1 1 calc R . . C33 C 0.690(2) 0.9914(15) 0.9592(16) 0.097(7) Uani 1 1 d . . . H33 H 0.6402 1.0341 0.9869 0.117 Uiso 1 1 calc R . . C41 C 1.2004(15) 0.7759(12) 0.8676(9) 0.060(4) Uani 1 1 d . . . H41 H 1.2123 0.8104 0.8199 0.072 Uiso 1 1 calc R . . C45 C 1.0551(17) 0.6953(14) 0.9593(8) 0.075(5) Uani 1 1 d . . . H45 H 0.9656 0.6720 0.9744 0.090 Uiso 1 1 calc R . . C44 C 1.1716(18) 0.6802(16) 1.0094(10) 0.087(6) Uani 1 1 d . . . H44 H 1.1613 0.6496 1.0592 0.104 Uiso 1 1 calc R . . C42 C 1.3192(16) 0.7592(14) 0.9161(11) 0.076(5) Uani 1 1 d . . . H42 H 1.4097 0.7808 0.9017 0.091 Uiso 1 1 calc R . . C34 C 0.659(2) 0.9662(16) 0.8782(16) 0.108(7) Uani 1 1 d . . . H34 H 0.5900 0.9946 0.8482 0.130 Uiso 1 1 calc R . . C43 C 1.2994(19) 0.7092(15) 0.9872(12) 0.086(6) Uani 1 1 d . . . H43 H 1.3782 0.6955 1.0205 0.103 Uiso 1 1 calc R . . C32 C 0.799(2) 0.9528(15) 1.0041(13) 0.094(6) Uani 1 1 d . . . H32 H 0.8247 0.9723 1.0617 0.113 Uiso 1 1 calc R . . N2 N 0.8078(10) 0.7387(7) 0.5148(5) 0.037(2) Uani 1 1 d . . . H70 H 0.7429 0.7175 0.4732 0.045 Uiso 1 1 calc R . . Cl2 Cl 1.0837(4) 0.9540(3) 0.7617(2) 0.0611(11) Uani 1 1 d . . . C54 C 0.5708(16) 0.5601(13) 0.8676(10) 0.069(5) Uani 1 1 d . . . H54 H 0.4861 0.5576 0.8917 0.083 Uiso 1 1 calc R . . Cl1 Cl 0.6416(4) 0.6263(3) 0.3510(2) 0.0508(9) Uani 1 1 d . . . C61 C 0.8078(18) 0.6541(15) 0.1722(11) 0.088(6) Uani 1 1 d . . . Cl20 Cl 0.8458(9) 0.5410(6) 0.1387(7) 0.119(3) Uani 0.67 1 d P . . Cl21 Cl 0.7030(6) 0.6897(7) 0.0899(4) 0.107(3) Uani 0.67 1 d P . . Cl22 Cl 0.9614(7) 0.7387(8) 0.1968(4) 0.125(4) Uani 0.67 1 d P . . C60 C 0.4890(16) 0.8235(13) 0.3073(11) 0.074(5) Uani 1 1 d . . . Cl12 Cl 0.4675(10) 0.8847(7) 0.4059(5) 0.119(3) Uani 0.67 1 d P . . Cl10 Cl 0.6220(6) 0.8950(5) 0.2661(4) 0.0747(18) Uani 0.67 1 d P . . Cl11 Cl 0.3292(7) 0.8047(5) 0.2454(6) 0.109(3) Uani 0.67 1 d P . . 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 C31 0.062(10) 0.087(13) 0.063(10) -0.011(9) 0.003(8) 0.017(10) Pd1 0.0336(5) 0.0357(6) 0.0253(5) 0.0037(4) 0.0003(4) 0.0010(4) P2 0.0299(16) 0.0332(18) 0.0281(16) 0.0031(13) 0.0006(13) 0.0031(14) P3 0.0336(17) 0.043(2) 0.0242(15) 0.0050(14) 0.0006(13) 0.0046(15) N1 0.030(5) 0.042(6) 0.036(6) 0.006(5) 0.003(5) 0.002(5) C24 0.034(7) 0.039(8) 0.047(8) 0.002(6) -0.001(6) 0.007(6) C20 0.033(7) 0.040(7) 0.028(6) 0.009(5) 0.005(5) 0.018(6) C1 0.029(6) 0.036(7) 0.032(6) 0.010(5) -0.001(5) 0.000(5) C30 0.049(8) 0.038(8) 0.039(7) -0.002(6) 0.014(6) -0.005(6) C2 0.051(8) 0.039(8) 0.051(8) -0.002(6) -0.005(7) 0.018(7) C21 0.047(8) 0.037(7) 0.028(6) 0.008(5) 0.002(5) 0.012(6) C4 0.112(16) 0.058(11) 0.084(13) 0.005(9) 0.016(12) 0.044(12) C11 0.050(9) 0.042(9) 0.097(12) 0.017(8) 0.007(8) 0.005(7) C22 0.066(9) 0.059(9) 0.032(7) 0.019(7) 0.032(7) 0.027(8) C15 0.030(7) 0.049(8) 0.046(7) 0.008(6) 0.005(6) 0.007(6) C10 0.031(6) 0.042(8) 0.028(6) 0.004(5) -0.002(5) 0.004(6) C6 0.041(8) 0.062(10) 0.048(8) 0.017(7) 0.005(6) 0.007(7) C40 0.033(7) 0.059(9) 0.029(6) -0.002(6) -0.002(5) 0.010(6) C23 0.046(8) 0.048(8) 0.040(8) 0.013(6) 0.021(6) 0.006(7) C14 0.048(9) 0.080(12) 0.058(9) 0.016(8) 0.001(7) 0.017(8) C3 0.087(12) 0.048(10) 0.068(10) -0.006(8) -0.008(9) 0.028(9) C50 0.043(7) 0.040(8) 0.035(7) 0.013(6) 0.000(6) 0.005(6) C55 0.040(8) 0.056(9) 0.052(8) 0.005(7) 0.007(7) -0.001(7) C51 0.056(9) 0.037(8) 0.049(8) 0.007(6) 0.015(7) 0.005(7) C52 0.065(10) 0.051(10) 0.062(9) 0.008(7) 0.001(8) 0.009(8) C35 0.104(14) 0.088(14) 0.078(12) 0.015(10) 0.016(11) 0.056(12) C5 0.073(11) 0.079(13) 0.068(11) 0.024(9) 0.019(9) 0.042(10) C13 0.046(9) 0.097(14) 0.082(12) 0.006(10) 0.009(8) 0.028(10) C12 0.061(10) 0.062(11) 0.105(14) 0.007(10) 0.015(10) 0.038(9) C53 0.070(12) 0.066(12) 0.064(10) 0.007(9) -0.002(9) -0.004(9) C33 0.089(15) 0.084(15) 0.122(19) -0.019(14) 0.045(14) 0.017(12) C41 0.055(10) 0.084(12) 0.047(8) 0.013(8) 0.004(7) 0.029(9) C45 0.064(10) 0.140(17) 0.028(7) 0.025(9) 0.005(7) 0.028(11) C44 0.062(11) 0.156(19) 0.051(10) 0.040(11) -0.005(9) 0.041(12) C42 0.044(9) 0.101(14) 0.084(13) -0.009(11) 0.013(9) 0.023(9) C34 0.132(19) 0.107(18) 0.111(18) 0.028(14) 0.031(15) 0.078(16) C43 0.059(12) 0.129(18) 0.069(12) 0.007(12) -0.005(9) 0.028(11) C32 0.102(15) 0.095(15) 0.080(13) -0.041(12) 0.011(12) 0.018(13) N2 0.045(6) 0.042(6) 0.020(5) 0.009(4) -0.002(4) -0.005(5) Cl2 0.080(3) 0.052(2) 0.0401(19) 0.0003(16) 0.0013(18) -0.019(2) C54 0.041(9) 0.089(14) 0.076(11) 0.014(10) 0.021(8) -0.010(9) Cl1 0.051(2) 0.056(2) 0.0402(18) -0.0016(16) -0.0012(15) -0.0007(17) C61 0.065(11) 0.124(17) 0.072(12) 0.006(11) 0.029(9) -0.004(11) Cl20 0.099(6) 0.093(6) 0.181(9) 0.003(6) 0.060(6) 0.038(5) Cl21 0.047(4) 0.204(9) 0.075(4) 0.082(5) 0.000(3) 0.004(4) Cl22 0.063(4) 0.211(10) 0.064(4) -0.068(5) 0.026(3) -0.063(5) C60 0.050(9) 0.080(12) 0.091(12) 0.015(10) 0.013(9) 0.006(9) Cl12 0.145(8) 0.149(8) 0.079(5) -0.007(5) 0.040(5) 0.059(7) Cl10 0.049(3) 0.083(5) 0.099(5) 0.038(4) 0.029(3) 0.005(3) Cl11 0.058(4) 0.066(4) 0.178(8) 0.026(5) -0.067(5) -0.018(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 C31 C32 1.35(2) . ? C31 C30 1.403(19) . ? Pd1 N1 2.107(9) . ? Pd1 P2 2.234(3) . ? Pd1 P3 2.287(3) . ? Pd1 Cl2 2.337(3) . ? P2 N2 1.676(9) . ? P2 C1 1.786(12) . ? P2 C10 1.797(12) . ? P3 C40 1.803(12) . ? P3 C50 1.806(13) . ? P3 C30 1.812(13) . ? N1 C20 1.327(14) . ? N1 C24 1.340(14) . ? C24 C23 1.377(16) . ? C20 N2 1.374(14) . ? C20 C21 1.405(15) . ? C1 C2 1.372(16) . ? C1 C6 1.376(17) . ? C30 C35 1.37(2) . ? C2 C3 1.415(19) . ? C21 C22 1.342(17) . ? C4 C3 1.35(2) . ? C4 C5 1.39(2) . ? C11 C12 1.39(2) . ? C11 C10 1.400(18) . ? C22 C23 1.365(18) . ? C15 C14 1.364(18) . ? C15 C10 1.372(16) . ? C6 C5 1.41(2) . ? C40 C41 1.368(18) . ? C40 C45 1.396(18) . ? C14 C13 1.38(2) . ? C50 C51 1.368(17) . ? C50 C55 1.417(17) . ? C55 C54 1.381(19) . ? C51 C52 1.357(18) . ? C52 C53 1.37(2) . ? C35 C34 1.44(2) . ? C13 C12 1.38(2) . ? C53 C54 1.38(2) . ? C33 C34 1.30(3) . ? C33 C32 1.41(3) . ? C41 C42 1.37(2) . ? C45 C44 1.36(2) . ? C44 C43 1.32(2) . ? C42 C43 1.38(2) . ? C61 Cl21 1.71(2) . ? C61 Cl22 1.722(19) . ? C61 Cl20 1.73(2) . ? C60 Cl10 1.702(16) . ? C60 Cl11 1.707(17) . ? C60 Cl12 1.772(19) . ? 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 C32 C31 C30 120.3(17) . . ? N1 Pd1 P2 82.4(3) . . ? N1 Pd1 P3 176.7(3) . . ? P2 Pd1 P3 99.59(11) . . ? N1 Pd1 Cl2 92.4(3) . . ? P2 Pd1 Cl2 166.89(13) . . ? P3 Pd1 Cl2 86.19(12) . . ? N2 P2 C1 106.2(5) . . ? N2 P2 C10 102.9(5) . . ? C1 P2 C10 110.0(6) . . ? N2 P2 Pd1 99.5(4) . . ? C1 P2 Pd1 122.4(4) . . ? C10 P2 Pd1 113.1(4) . . ? C40 P3 C50 102.0(6) . . ? C40 P3 C30 109.5(6) . . ? C50 P3 C30 105.4(6) . . ? C40 P3 Pd1 112.2(4) . . ? C50 P3 Pd1 118.1(4) . . ? C30 P3 Pd1 109.1(4) . . ? C20 N1 C24 118.1(10) . . ? C20 N1 Pd1 118.0(8) . . ? C24 N1 Pd1 123.8(8) . . ? N1 C24 C23 122.4(12) . . ? N1 C20 N2 116.9(10) . . ? N1 C20 C21 122.2(11) . . ? N2 C20 C21 120.9(10) . . ? C2 C1 C6 119.5(12) . . ? C2 C1 P2 122.5(9) . . ? C6 C1 P2 117.9(10) . . ? C35 C30 C31 119.8(14) . . ? C35 C30 P3 117.4(11) . . ? C31 C30 P3 122.5(12) . . ? C1 C2 C3 120.7(13) . . ? C22 C21 C20 118.0(11) . . ? C3 C4 C5 120.4(16) . . ? C12 C11 C10 121.0(14) . . ? C21 C22 C23 120.8(11) . . ? C14 C15 C10 122.8(13) . . ? C15 C10 C11 117.1(12) . . ? C15 C10 P2 126.4(10) . . ? C11 C10 P2 116.1(9) . . ? C1 C6 C5 120.1(14) . . ? C41 C40 C45 115.3(12) . . ? C41 C40 P3 124.3(10) . . ? C45 C40 P3 120.3(10) . . ? C22 C23 C24 118.4(12) . . ? C15 C14 C13 119.7(15) . . ? C4 C3 C2 119.7(16) . . ? C51 C50 C55 118.2(12) . . ? C51 C50 P3 119.2(10) . . ? C55 C50 P3 122.6(10) . . ? C54 C55 C50 119.0(14) . . ? C52 C51 C50 122.4(13) . . ? C51 C52 C53 119.8(15) . . ? C30 C35 C34 117.1(18) . . ? C4 C5 C6 119.6(14) . . ? C12 C13 C14 120.0(15) . . ? C13 C12 C11 119.4(15) . . ? C52 C53 C54 119.8(16) . . ? C34 C33 C32 118.7(19) . . ? C40 C41 C42 123.3(15) . . ? C44 C45 C40 122.2(15) . . ? C43 C44 C45 119.9(16) . . ? C41 C42 C43 117.5(16) . . ? C33 C34 C35 123(2) . . ? C44 C43 C42 121.7(17) . . ? C31 C32 C33 120.8(18) . . ? C20 N2 P2 121.0(8) . . ? C53 C54 C55 120.8(14) . . ? Cl21 C61 Cl22 110.0(11) . . ? Cl21 C61 Cl20 107.0(11) . . ? Cl22 C61 Cl20 110.8(11) . . ? Cl10 C60 Cl11 114.4(11) . . ? Cl10 C60 Cl12 106.8(10) . . ? Cl11 C60 Cl12 107.8(10) . . ? _diffrn_measured_fraction_theta_max 1.49 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.468 _refine_diff_density_min -0.903 _refine_diff_density_rms 0.161