Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 182 loop_ _publ_author_name 'Frank Glorius' 'Gereon Altenhoff' 'Richard Goddard' 'Christian W. Lehmann' _publ_contact_author_name 'Dr Frank Glorius' _publ_contact_author_address ; Max-Planck-Institut fur Kohlenforschung Kaiser-Wilhelm-Platz 1 Mulheim/Ruhr 45470 GERMANY ; _publ_contact_author_email 'GLORIUS@MPI-MUELHEIM.MPG.DE' _publ_requested_journal 'Chemical Communications' _publ_section_title ; Oxazolines as chiral building blocks for imidazolium salts and N-heterocyclic carbene ligands ; data_2 _database_code_CSD 191920 _chemical_name_systematic ; (1-isopropylmethyl-methylene-oxy-5-yl)(2-isopropylmethyl- methylene-oxo-4-yl)imidazol-2-ylidium trifluoromethylsufonate ; _chemical_compound_source 'see paper' _chemical_formula_moiety 'C13 H21 N2 O2 1+, C F3 O3 S 1-' _chemical_formula_sum 'C14 H21 F3 N2 O5 S' _chemical_formula_weight 386.39 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' _symmetry_Int_Tables_number 19 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 9.6882(3) _cell_length_b 11.0578(3) _cell_length_c 16.3800(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1754.79(9) _cell_formula_units_Z 4 _cell_measurement_temperature 100 _cell_measurement_reflns_used 26186 _cell_measurement_theta_min 2.04 _cell_measurement_theta_max 26.37 _exptl_crystal_description prism _exptl_crystal_colour 'orange-yellow' _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.463 _exptl_crystal_density_method none _exptl_crystal_F_000 808 _exptl_absorpt_coefficient_mu 0.242 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details 'XPREP, Siemens (1995)' _exptl_absorpt_correction_T_min 0.93537 _exptl_absorpt_correction_T_max 0.98035 _diffrn_ambient_temperature 100 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source '0.3 mm focus rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method 'CCD \w-scan' _diffrn_standards_number 0 _diffrn_standards_decay_% 0.0 _diffrn_reflns_number 22778 _diffrn_reflns_av_R_equivalents 0.0806 _diffrn_reflns_av_sigmaI/netI 0.0460 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.22 _diffrn_reflns_theta_max 26.47 _reflns_number_total 3622 _reflns_number_gt 3086 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Collect software (Nonius, 1998)' _computing_cell_refinement 'Denzo / Scalepack (Otwinowski 1997)' _computing_data_reduction 'Denzo / Scalepack (Otwinowski 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP (Johnson, 1976)' _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^)+(0.0395P)^2^+0.3091P] 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_abs_structure_details 'Flack, H. D. (1983). Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.05(7) _refine_ls_number_reflns 3622 _refine_ls_number_parameters 310 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0491 _refine_ls_R_factor_gt 0.0365 _refine_ls_wR_factor_ref 0.0837 _refine_ls_wR_factor_gt 0.0788 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.024 _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 C1 C 0.1504(2) 0.59615(18) 0.63404(13) 0.0257(4) Uani 1 1 d . . . C2 C 0.3394(2) 0.7641(2) 0.62591(14) 0.0288(5) Uani 1 1 d . . . C3 C 0.4863(3) 0.7310(2) 0.59759(19) 0.0404(6) Uani 1 1 d . . . C4 C 0.3713(2) 0.5547(2) 0.60931(14) 0.0294(5) Uani 1 1 d . . . C5 C 0.3022(2) 0.4494(2) 0.60974(14) 0.0289(5) Uani 1 1 d . . . C6 C 0.1927(3) 0.2714(2) 0.62137(18) 0.0372(6) Uani 1 1 d . . . C7 C 0.0783(2) 0.3689(2) 0.62294(14) 0.0305(5) Uani 1 1 d . . . C8 C 0.3245(2) 0.8224(2) 0.71006(14) 0.0290(5) Uani 1 1 d . . . C9 C 0.3920(3) 0.7487(3) 0.77719(17) 0.0409(7) Uani 1 1 d . . . C10 C 0.3794(3) 0.9515(2) 0.70806(18) 0.0354(6) Uani 1 1 d . . . C11 C -0.0188(2) 0.3701(2) 0.54925(14) 0.0333(5) Uani 1 1 d . . . C12 C 0.0575(3) 0.3912(3) 0.46982(16) 0.0427(6) Uani 1 1 d . . . C13 C -0.1361(3) 0.4595(3) 0.56089(19) 0.0415(6) Uani 1 1 d . . . C14 C 0.0412(3) 0.4903(2) 0.87223(16) 0.0380(6) Uani 1 1 d . . . H1 H 0.072(2) 0.642(2) 0.6486(13) 0.027(6) Uiso 1 1 d . . . H2 H 0.298(2) 0.8125(18) 0.5841(13) 0.011(5) Uiso 1 1 d . . . H3A H 0.503(3) 0.755(2) 0.5414(19) 0.056(9) Uiso 1 1 d . . . H3B H 0.553(3) 0.760(2) 0.6341(17) 0.042(7) Uiso 1 1 d . . . H6A H 0.206(2) 0.2419(19) 0.6740(16) 0.024(6) Uiso 1 1 d . . . H6B H 0.173(2) 0.210(2) 0.5787(14) 0.028(6) Uiso 1 1 d . . . H7 H 0.029(3) 0.361(2) 0.6746(15) 0.036(6) Uiso 1 1 d . . . H8 H 0.229(2) 0.8270(19) 0.7211(13) 0.022(6) Uiso 1 1 d . . . H9A H 0.379(3) 0.786(3) 0.8273(19) 0.055(9) Uiso 1 1 d . . . H9B H 0.496(3) 0.744(2) 0.7696(18) 0.049(8) Uiso 1 1 d . . . H9C H 0.360(3) 0.669(3) 0.7821(16) 0.050(8) Uiso 1 1 d . . . H10A H 0.335(3) 0.996(2) 0.6664(17) 0.038(7) Uiso 1 1 d . . . H10B H 0.478(3) 0.953(2) 0.6986(16) 0.045(8) Uiso 1 1 d . . . H10C H 0.367(3) 0.988(2) 0.7594(16) 0.033(6) Uiso 1 1 d . . . H11 H -0.055(3) 0.293(2) 0.5501(14) 0.029(6) Uiso 1 1 d . . . H13A H -0.184(3) 0.445(3) 0.615(2) 0.055(8) Uiso 1 1 d . . . H13B H -0.203(4) 0.454(3) 0.519(2) 0.068(10) Uiso 1 1 d . . . H13C H -0.103(3) 0.540(2) 0.5592(15) 0.035(7) Uiso 1 1 d . . . H12A H 0.139(3) 0.327(3) 0.4613(17) 0.054(8) Uiso 1 1 d . . . H12B H 0.091(3) 0.469(3) 0.4640(18) 0.055(9) Uiso 1 1 d . . . H12C H -0.003(3) 0.380(3) 0.421(2) 0.062(9) Uiso 1 1 d . . . N1 N 0.27583(18) 0.64321(16) 0.62383(11) 0.0262(4) Uani 1 1 d . . . N2 N 0.16625(19) 0.47784(15) 0.62552(11) 0.0266(4) Uani 1 1 d . . . O1 O 0.50075(15) 0.59822(15) 0.60088(10) 0.0365(4) Uani 1 1 d . . . O2 O 0.32239(16) 0.33021(13) 0.59732(10) 0.0359(4) Uani 1 1 d . . . O3 O 0.19120(18) 0.32473(17) 0.93686(11) 0.0449(5) Uani 1 1 d . . . O4 O 0.06181(19) 0.27789(15) 0.81424(11) 0.0420(4) Uani 1 1 d . . . O5 O 0.26095(16) 0.40690(15) 0.80563(11) 0.0369(4) Uani 1 1 d . . . F1 F -0.00773(17) 0.53433(14) 0.80243(10) 0.0549(4) Uani 1 1 d . . . F2 F 0.1066(2) 0.57785(15) 0.91080(13) 0.0783(6) Uani 1 1 d . . . F3 F -0.06858(16) 0.46193(17) 0.91771(10) 0.0588(5) Uani 1 1 d . . . S S 0.15232(6) 0.36030(5) 0.85605(3) 0.02818(14) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0236(11) 0.0273(10) 0.0261(11) -0.0047(9) -0.0008(10) -0.0001(10) C2 0.0261(12) 0.0299(11) 0.0303(12) 0.0015(9) -0.0027(11) -0.0058(10) C3 0.0323(14) 0.0474(15) 0.0413(16) -0.0100(12) 0.0033(12) -0.0104(12) C4 0.0222(12) 0.0382(13) 0.0277(12) -0.0011(10) -0.0022(9) 0.0047(10) C5 0.0242(11) 0.0351(12) 0.0274(12) -0.0010(10) -0.0007(9) 0.0070(10) C6 0.0456(16) 0.0282(12) 0.0378(15) 0.0020(11) 0.0004(12) 0.0019(11) C7 0.0357(13) 0.0253(11) 0.0305(12) 0.0018(10) 0.0033(10) -0.0036(10) C8 0.0250(13) 0.0327(12) 0.0294(12) 0.0006(9) -0.0030(10) -0.0023(10) C9 0.0530(19) 0.0387(16) 0.0311(15) -0.0024(12) -0.0089(12) -0.0019(13) C10 0.0313(15) 0.0346(13) 0.0405(16) -0.0033(12) -0.0037(12) -0.0043(11) C11 0.0354(13) 0.0294(12) 0.0352(13) -0.0001(10) -0.0043(10) -0.0097(11) C12 0.0476(17) 0.0486(17) 0.0319(14) -0.0039(12) -0.0058(13) -0.0055(14) C13 0.0326(15) 0.0443(16) 0.0477(17) -0.0007(12) -0.0091(13) -0.0064(13) C14 0.0337(13) 0.0418(14) 0.0385(15) -0.0047(11) 0.0005(12) 0.0064(11) N1 0.0227(9) 0.0282(9) 0.0278(10) -0.0025(8) -0.0018(7) -0.0008(8) N2 0.0247(10) 0.0291(9) 0.0260(10) -0.0016(7) -0.0009(8) 0.0001(8) O1 0.0190(8) 0.0459(10) 0.0446(10) 0.0003(8) 0.0007(7) -0.0025(7) O2 0.0353(10) 0.0305(8) 0.0420(10) -0.0030(7) 0.0017(8) 0.0074(7) O3 0.0426(11) 0.0596(11) 0.0324(10) 0.0051(8) 0.0022(8) 0.0198(9) O4 0.0431(10) 0.0397(10) 0.0431(10) -0.0034(8) 0.0036(9) -0.0132(8) O5 0.0248(8) 0.0423(9) 0.0435(10) 0.0068(8) 0.0045(7) -0.0013(7) F1 0.0515(10) 0.0630(10) 0.0501(10) 0.0168(8) 0.0052(8) 0.0246(8) F2 0.0724(13) 0.0492(10) 0.1135(17) -0.0407(11) -0.0193(11) 0.0122(9) F3 0.0406(9) 0.0921(13) 0.0439(9) 0.0046(8) 0.0107(8) 0.0254(9) S 0.0251(3) 0.0297(3) 0.0297(3) 0.0012(2) 0.0015(2) 0.0016(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 C1 N2 1.325(3) . y C1 N1 1.332(3) . y C1 H1 0.94(2) . y C2 N1 1.472(3) . y C2 C8 1.528(3) . y C2 C3 1.541(4) . y C2 H2 0.96(2) . y C3 O1 1.475(3) . y C3 H3A 0.97(3) . y C3 H3B 0.93(3) . y C4 C5 1.343(3) . y C4 O1 1.350(3) . y C4 N1 1.368(3) . y C5 O2 1.347(3) . y C5 N2 1.378(3) . y C6 O2 1.468(3) . y C6 C7 1.547(3) . y C6 H6A 0.93(3) . y C6 H6B 0.99(2) . y C7 N2 1.476(3) . y C7 C11 1.530(3) . y C7 H7 0.98(3) . y C8 C9 1.517(3) . y C8 C10 1.524(3) . y C8 H8 0.94(2) . y C9 H9A 0.92(3) . y C9 H9B 1.01(3) . y C9 H9C 0.94(3) . y C10 H10A 0.95(3) . y C10 H10B 0.97(3) . y C10 H10C 0.94(3) . y C11 C12 1.514(4) . y C11 C13 1.519(4) . y C11 H11 0.92(2) . y C12 H12A 1.07(3) . y C12 H12B 0.93(3) . y C12 H12C 0.99(3) . y C13 H13A 1.01(3) . y C13 H13B 0.95(3) . y C13 H13C 0.95(3) . y C14 F2 1.318(3) . y C14 F1 1.330(3) . y C14 F3 1.336(3) . y C14 S 1.815(2) . y O3 S 1.4313(19) . y O4 S 1.4381(18) . y O5 S 1.4336(17) . y 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 N2 C1 N1 105.5(2) . . y N2 C1 H1 130.3(14) . . y N1 C1 H1 124.0(14) . . y N1 C2 C8 111.38(18) . . y N1 C2 C3 99.38(18) . . y C8 C2 C3 117.3(2) . . y N1 C2 H2 108.4(12) . . y C8 C2 H2 111.7(12) . . y C3 C2 H2 107.8(12) . . y O1 C3 C2 108.3(2) . . y O1 C3 H3A 107.0(16) . . y C2 C3 H3A 112.1(18) . . y O1 C3 H3B 104.4(16) . . y C2 C3 H3B 111.4(16) . . y H3A C3 H3B 113(2) . . y C5 C4 O1 140.6(2) . . y C5 C4 N1 106.39(19) . . y O1 C4 N1 112.98(19) . . y C4 C5 O2 140.7(2) . . y C4 C5 N2 106.23(19) . . y O2 C5 N2 113.0(2) . . y O2 C6 C7 108.00(18) . . y O2 C6 H6A 106.5(14) . . y C7 C6 H6A 109.3(14) . . y O2 C6 H6B 106.1(14) . . y C7 C6 H6B 110.5(14) . . y H6A C6 H6B 116.0(19) . . y N2 C7 C11 111.78(18) . . y N2 C7 C6 98.94(18) . . y C11 C7 C6 115.7(2) . . y N2 C7 H7 109.6(15) . . y C11 C7 H7 112.4(14) . . y C6 C7 H7 107.7(14) . . y C9 C8 C10 111.6(2) . . y C9 C8 C2 112.7(2) . . y C10 C8 C2 110.1(2) . . y C9 C8 H8 108.2(14) . . y C10 C8 H8 107.2(13) . . y C2 C8 H8 106.7(14) . . y C8 C9 H9A 110.5(18) . . y C8 C9 H9B 111.5(17) . . y H9A C9 H9B 105(2) . . y C8 C9 H9C 115.1(17) . . y H9A C9 H9C 107(2) . . y H9B C9 H9C 107(2) . . y C8 C10 H10A 109.9(16) . . y C8 C10 H10B 111.1(16) . . y H10A C10 H10B 109(2) . . y C8 C10 H10C 109.6(15) . . y H10A C10 H10C 112(2) . . y H10B C10 H10C 105(2) . . y C12 C11 C13 111.9(2) . . y C12 C11 C7 112.3(2) . . y C13 C11 C7 111.5(2) . . y C12 C11 H11 110.0(15) . . y C13 C11 H11 108.4(15) . . y C7 C11 H11 102.4(15) . . y C11 C12 H12A 111.8(15) . . y C11 C12 H12B 113.8(19) . . y H12A C12 H12B 110(2) . . y C11 C12 H12C 112.3(17) . . y H12A C12 H12C 104(2) . . y H12B C12 H12C 104(2) . . y C11 C13 H13A 110.5(17) . . y C11 C13 H13B 112(2) . . y H13A C13 H13B 108(3) . . y C11 C13 H13C 111.0(15) . . y H13A C13 H13C 109(2) . . y H13B C13 H13C 106(2) . . y F2 C14 F1 108.3(2) . . y F2 C14 F3 106.7(2) . . y F1 C14 F3 106.3(2) . . y F2 C14 S 111.52(18) . . y F1 C14 S 112.09(17) . . y F3 C14 S 111.59(17) . . y C1 N1 C4 111.04(18) . . y C1 N1 C2 137.14(19) . . y C4 N1 C2 111.80(18) . . y C1 N2 C5 110.84(19) . . y C1 N2 C7 137.9(2) . . y C5 N2 C7 111.09(18) . . y C4 O1 C3 105.68(18) . . y C5 O2 C6 105.54(17) . . y O3 S O5 116.00(11) . . y O3 S O4 115.26(11) . . y O5 S O4 113.64(11) . . y O3 S C14 103.81(11) . . y O5 S C14 103.58(11) . . y O4 S C14 102.10(11) . . y _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.47 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.220 _refine_diff_density_min -0.226 _refine_diff_density_rms 0.041 #===END data_4226 _database_code_CSD 191921 _chemical_name_systematic ; Bis[(1-isopropylmethyl-methylene-oxy-5-yl)(2-isopropylmethyl- methylene-oxo-4-yl)imidazol-2-ylidene]palladium diiodide chloroform solvate ; _chemical_melting_point ? _chemical_compound_source 'see paper' _chemical_formula_moiety 'C26 H40 I2 N4 O4 Pd, 2(C H Cl3)' _chemical_formula_sum 'C28 H42 Cl6 I2 N4 O4 Pd' _chemical_formula_weight 1071.56 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' 'Cl' 'Cl' 0.1484 0.1585 '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' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pd' 'Pd' -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 2' _symmetry_Int_Tables_number 18 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' _cell_length_a 12.257(3) _cell_length_b 13.001(3) _cell_length_c 12.305(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1960.9(7) _cell_formula_units_Z 2 _cell_measurement_temperature 200 _cell_measurement_reflns_used 33760 _cell_measurement_theta_min 2.04 _cell_measurement_theta_max 33.14 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.815 _exptl_crystal_density_method none _exptl_crystal_F_000 1048 _exptl_absorpt_coefficient_mu 2.493 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details 'XPREP, Siemens (1995)' _exptl_absorpt_correction_T_min 0.79669 _exptl_absorpt_correction_T_max 0.80937 _diffrn_ambient_temperature 200 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source '0.3 mm focus rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method 'CCD \w-scan' _diffrn_standards_number 0 _diffrn_standards_decay_% 0.0 _diffrn_reflns_number 68069 _diffrn_reflns_av_R_equivalents 0.0873 _diffrn_reflns_av_sigmaI/netI 0.0422 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 6.65 _diffrn_reflns_theta_max 33.10 _reflns_number_total 6714 _reflns_number_gt 4958 _reflns_threshold_expression I>2\s(I) _diffrn_reflns_number 68069 _computing_data_collection 'Collect software (Nonius, 1998)' _computing_cell_refinement 'Denzo / Scalepack (Otwinowski 1997)' _computing_data_reduction 'Denzo / Scalepack (Otwinowski 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP (Johnson, 1976)' _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. The crystal contains per Pd complex two molecules of chloroform solvate (CHCl~3~), which are rotationally disordered. C and Cl atoms of the disordered solvate were refined with isotropic atomic displacement parameters and half occupancy for the C atoms and 0.2 occupancy for the Cl atoms. H atoms of the solvate were not included in the model. Otherwise, H atoms were calculated and refined using a riding model. Highest peak 0.76 at 0.8394 0.0773 0.2211 [ 0.78 A from I ] Deepest hole -0.80 at 0.8279 0.1589 0.2170 [ 0.61 A from I ] ; _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^)+(0.0165P)^2^+3.6019P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_abs_structure_details 'Flack, H. D. (1983). Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.02(3) _refine_ls_number_reflns 6714 _refine_ls_number_parameters 236 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0745 _refine_ls_R_factor_gt 0.0431 _refine_ls_wR_factor_ref 0.0848 _refine_ls_wR_factor_gt 0.0741 _refine_ls_goodness_of_fit_ref 1.084 _refine_ls_restrained_S_all 1.084 _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 C1 C 0.8938(3) 0.8796(3) 0.2529(5) 0.0319(7) Uani 1 1 d . . . C2 C 0.9222(4) 0.7837(4) 0.4400(4) 0.0429(11) Uani 1 1 d . . . H2 H 0.9979 0.7614 0.4304 0.051 Uiso 1 1 calc R . . C3 C 0.8538(7) 0.6908(5) 0.4694(6) 0.074(2) Uani 1 1 d . . . H3A H 0.9011 0.6325 0.4839 0.089 Uiso 1 1 calc R . . H3B H 0.8122 0.7051 0.5348 0.089 Uiso 1 1 calc R . . C4 C 0.7976(4) 0.7385(4) 0.3055(5) 0.0451(12) Uani 1 1 d . . . C5 C 0.7627(4) 0.7641(4) 0.2074(5) 0.0428(12) Uani 1 1 d . . . C6 C 0.7041(5) 0.8051(5) 0.0405(6) 0.0700(19) Uani 1 1 d . . . H6A H 0.6342 0.8351 0.0212 0.084 Uiso 1 1 calc R . . H6B H 0.7315 0.7679 -0.0222 0.084 Uiso 1 1 calc R . . C7 C 0.7846(4) 0.8907(4) 0.0717(4) 0.0390(10) Uani 1 1 d . . . H7 H 0.7429 0.9538 0.0849 0.047 Uiso 1 1 calc R . . C8 C 0.9206(7) 0.8728(5) 0.5208(5) 0.067(2) Uani 1 1 d . . . H8 H 0.9649 0.9281 0.4895 0.080 Uiso 1 1 calc R . . C9 C 0.8111(10) 0.9146(8) 0.5378(8) 0.131(4) Uani 1 1 d . . . H9A H 0.8164 0.9816 0.5702 0.197 Uiso 1 1 calc R . . H9B H 0.7708 0.8698 0.5852 0.197 Uiso 1 1 calc R . . H9C H 0.7741 0.9198 0.4692 0.197 Uiso 1 1 calc R . . C10 C 0.9743(9) 0.8417(7) 0.6261(6) 0.100(3) Uani 1 1 d . . . H10A H 1.0520 0.8400 0.6165 0.150 Uiso 1 1 calc R . . H10B H 0.9490 0.7747 0.6471 0.150 Uiso 1 1 calc R . . H10C H 0.9561 0.8905 0.6817 0.150 Uiso 1 1 calc R . . C11 C 0.8731(5) 0.9148(6) -0.0083(4) 0.0540(15) Uani 1 1 d . . . H11 H 0.9192 0.9679 0.0247 0.065 Uiso 1 1 calc R . . C12 C 0.8265(7) 0.9600(6) -0.1116(5) 0.080(2) Uani 1 1 d . . . H12A H 0.8272 1.0337 -0.1068 0.120 Uiso 1 1 calc R . . H12B H 0.7529 0.9365 -0.1211 0.120 Uiso 1 1 calc R . . H12C H 0.8699 0.9385 -0.1725 0.120 Uiso 1 1 calc R . . C13 C 0.9430(7) 0.8259(9) -0.0291(7) 0.102(3) Uani 1 1 d . . . H13A H 0.9676 0.7979 0.0388 0.153 Uiso 1 1 calc R . . H13B H 1.0047 0.8469 -0.0716 0.153 Uiso 1 1 calc R . . H13C H 0.9024 0.7746 -0.0680 0.153 Uiso 1 1 calc R . . C14 C 0.5423(10) 1.0181(10) 0.2806(10) 0.069(4) Uiso 0.50 1 d P . . C15 C 0.5501(10) 1.0175(10) -0.2268(11) 0.070(4) Uiso 0.50 1 d P . . Cl1A Cl 0.5000 1.0000 0.1427(15) 0.101(5) Uiso 0.20 2 d SP . . Cl1B Cl 0.4800(9) 0.9409(10) 0.1597(9) 0.082(3) Uiso 0.20 1 d P . . Cl1C Cl 0.5072(9) 0.8941(8) 0.1971(9) 0.071(2) Uiso 0.20 1 d P . . Cl2A Cl 0.5393(13) 0.8921(11) 0.2704(18) 0.115(5) Uiso 0.20 1 d P . . Cl2B Cl 0.5685(11) 0.9065(10) 0.3234(12) 0.071(3) Uiso 0.20 1 d P . . Cl2C Cl 0.5873(11) 0.9335(11) 0.3483(14) 0.067(3) Uiso 0.20 1 d P . . Cl2D Cl 0.5806(11) 0.9356(10) 0.3862(11) 0.069(3) Uiso 0.20 1 d P . . Cl2E Cl 0.535(2) 0.9705(19) 0.4098(19) 0.178(10) Uiso 0.20 1 d P . . Cl3A Cl 0.5000 1.0000 -0.0740(14) 0.103(5) Uiso 0.20 2 d SP . . Cl3B Cl 0.4499(9) 0.9497(9) -0.0830(9) 0.071(3) Uiso 0.20 1 d P . . Cl3C Cl 0.4655(11) 0.9217(11) -0.1175(13) 0.099(4) Uiso 0.20 1 d P . . Cl4A Cl 0.5323(14) 0.8849(14) -0.2070(15) 0.112(8) Uiso 0.20 1 d P . . Cl4B Cl 0.5523(12) 0.8842(9) -0.2345(11) 0.041(2) Uiso 0.20 1 d P . . Cl4C Cl 0.5706(9) 0.8861(10) -0.2543(11) 0.057(4) Uiso 0.20 1 d P . . Cl4D Cl 0.5594(10) 0.9282(12) -0.2886(12) 0.068(3) Uiso 0.20 1 d P . . Cl4E Cl 0.5678(8) 0.9509(8) -0.3167(9) 0.061(3) Uiso 0.20 1 d P . . I I 0.83577(2) 1.128247(19) 0.25408(4) 0.04051(8) Uani 1 1 d . . . N1 N 0.8769(3) 0.8093(3) 0.3327(3) 0.0363(8) Uani 1 1 d . . . N2 N 0.8225(3) 0.8511(3) 0.1769(3) 0.0357(8) Uani 1 1 d . . . O1 O 0.7809(3) 0.6662(3) 0.3823(4) 0.0661(12) Uani 1 1 d . . . O2 O 0.6905(3) 0.7361(3) 0.1296(4) 0.0616(11) Uani 1 1 d . . . Pd Pd 1.0000 1.0000 0.25436(4) 0.02507(8) Uani 1 2 d S . . 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 C1 0.0256(15) 0.0294(16) 0.0406(18) -0.005(3) 0.007(2) -0.0046(13) C2 0.051(3) 0.041(3) 0.038(2) 0.0064(19) 0.011(2) 0.003(2) C3 0.099(6) 0.056(4) 0.068(4) 0.020(3) 0.013(4) -0.027(4) C4 0.033(3) 0.031(2) 0.071(3) 0.011(2) 0.009(2) -0.009(2) C5 0.027(2) 0.031(2) 0.070(3) -0.005(2) 0.002(2) -0.0087(19) C6 0.057(4) 0.071(4) 0.082(5) -0.004(3) -0.024(3) -0.026(3) C7 0.033(2) 0.036(2) 0.048(3) -0.0079(19) -0.0077(18) -0.0014(19) C8 0.112(6) 0.044(3) 0.044(3) 0.001(2) 0.008(3) 0.001(4) C9 0.183(11) 0.123(8) 0.087(6) 0.006(5) 0.020(7) 0.103(9) C10 0.152(9) 0.104(6) 0.044(4) 0.006(3) -0.006(4) -0.012(6) C11 0.038(3) 0.082(4) 0.042(3) -0.002(3) -0.005(2) 0.002(3) C12 0.100(5) 0.089(5) 0.050(4) 0.008(3) -0.015(4) -0.009(5) C13 0.094(6) 0.149(9) 0.064(5) 0.003(5) 0.003(4) 0.062(7) I 0.03359(12) 0.03646(12) 0.05147(16 -0.00530(18) 0.0013(2) 0.00280(10) N1 0.0325(19) 0.035(2) 0.041(2) 0.0020(16) 0.0084(15) -0.0079(16) N2 0.0290(18) 0.0330(18) 0.045(2) -0.0016(15) -0.0006(16) -0.0097(16) O1 0.059(3) 0.049(2) 0.090(3) 0.026(2) 0.010(2) -0.022(2) O2 0.043(2) 0.047(2) 0.095(3) 0.001(2) -0.0173(19) -0.0221(18) Pd 0.02454(15) 0.02589(15) 0.02479(16) 0.000 0.000 -0.00590(13) _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 C1 N2 1.333(6) . y C1 N1 1.358(6) . y C1 Pd 2.035(3) . y C2 N1 1.470(6) . y C2 C3 1.515(8) . y C2 C8 1.527(8) . y C3 O1 1.432(8) . y C4 C5 1.323(7) . y C4 O1 1.348(6) . y C4 N1 1.380(6) . y C5 O2 1.355(6) . y C5 N2 1.398(6) . y C6 O2 1.427(8) . y C6 C7 1.537(7) . y C7 N2 1.469(6) . y C7 C11 1.498(8) . y C8 C9 1.463(12) . y C8 C10 1.509(10) . y C11 C13 1.460(10) . y C11 C12 1.512(8) . y C14 C14 1.14(2) 2_675 y C14 Cl2C 1.486(18) . y C14 Cl2A 1.542(19) 2_675 y C14 Cl2B 1.577(18) . y C14 Cl1B 1.604(17) 2_675 y C14 Cl2A 1.644(19) . y C14 Cl1C 1.651(16) 2_675 y C14 Cl2E 1.71(3) . y C14 Cl2D 1.749(18) . y C14 Cl2B 1.755(18) 2_675 y C14 Cl1A 1.79(2) . y C14 Cl2E 1.85(3) 2_675 y C15 C15 1.31(2) 2_675 y C15 Cl4D 1.393(17) . y C15 Cl4E 1.421(17) . y C15 Cl3C 1.572(19) 2_675 y C15 Cl4A 1.64(2) 2_675 y C15 Cl4D 1.697(17) 2_675 y C15 Cl4B 1.735(17) . y C15 Cl4A 1.76(2) . y C15 Cl4C 1.760(18) . y C15 Cl4B 1.793(18) 2_675 y C15 Cl3B 1.821(18) 2_675 y C15 Cl4E 1.866(17) 2_675 y Cl1A Cl1B 0.834(12) . y Cl1A Cl1B 0.834(12) 2_675 y Cl1A Cl1C 1.533(14) 2_675 y Cl1A Cl1C 1.533(14) . y Cl1A C14 1.79(2) 2_675 y Cl1A Cl2A 2.16(2) 2_675 y Cl1A Cl2A 2.16(2) . y Cl1B Cl1C 0.832(12) . y Cl1B C14 1.604(17) 2_675 y Cl1B Cl1B 1.61(2) 2_675 y Cl1B Cl2A 1.67(2) . y Cl1B Cl1C 2.200(18) 2_675 y Cl1B Cl2B 2.331(18) . y Cl1C Cl2A 0.98(2) . y Cl1C C14 1.651(16) 2_675 y Cl1C Cl2B 1.734(17) . y Cl1C Cl2C 2.166(19) . y Cl1C Cl1B 2.200(18) 2_675 y Cl2A Cl2B 0.767(17) . y Cl2A Cl2C 1.25(2) . y Cl2A C14 1.542(19) 2_675 y Cl2A Cl2D 1.61(2) . y Cl2A Cl2E 2.00(3) . y Cl2B Cl2C 0.521(17) . y Cl2B Cl2D 0.873(19) . y Cl2B Cl2E 1.41(2) . y Cl2B C14 1.755(18) 2_675 y Cl2B Cl2E 2.30(3) 2_675 y Cl2C Cl2E 1.10(2) . y Cl2C C14 1.901(19) 2_675 y Cl2C Cl2E 2.09(3) 2_675 y Cl2D Cl2E 0.78(2) . y Cl2D Cl2E 1.89(3) 2_675 y Cl2D C14 2.078(18) 2_675 y Cl2E Cl2E 1.14(5) 2_675 y Cl2E C14 1.85(2) 2_675 y Cl2E Cl2D 1.89(3) 2_675 y Cl2E Cl2C 2.09(3) 2_675 y Cl2E Cl2B 2.30(3) 2_675 y Cl3A Cl3B 0.904(11) 2_675 y Cl3A Cl3B 0.904(11) . y Cl3A Cl3C 1.225(16) 2_675 y Cl3A Cl3C 1.225(16) . y Cl3A C15 1.99(2) 2_675 y Cl3A Cl4A 2.25(2) 2_675 y Cl3A Cl4A 2.25(2) . y Cl3B Cl3C 0.591(15) . y Cl3B Cl3B 1.79(2) 2_675 y Cl3B C15 1.821(18) 2_675 y Cl3B Cl3C 2.012(15) 2_675 y Cl3B Cl4A 2.01(2) . y Cl3B Cl4B 2.40(2) . y Cl3C Cl4A 1.45(2) . y Cl3C C15 1.572(19) 2_675 y Cl3C Cl4B 1.86(2) . y Cl3C Cl3B 2.012(15) 2_675 y Cl3C Cl4C 2.170(19) . y Cl3C Cl3C 2.20(3) 2_675 y Cl3C Cl4D 2.401(19) . y Cl4A Cl4C 0.75(2) . y Cl4A Cl4D 1.198(19) . y Cl4A C15 1.64(2) 2_675 y Cl4A Cl4E 1.659(19) . y Cl4B Cl4D 0.882(18) . y Cl4B Cl4E 1.346(17) . y Cl4B C15 1.793(18) 2_675 y Cl4C Cl4D 0.704(16) . y Cl4C Cl4E 1.141(17) . y Cl4C C15 1.968(18) 2_675 y Cl4D C15 1.697(17) 2_675 y Cl4D Cl4E 2.241(14) 2_675 y Cl4D Cl4D 2.37(3) 2_675 y Cl4E C15 1.866(17) 2_675 y Cl4E Cl4E 2.10(2) 2_675 y Cl4E Cl4D 2.241(14) 2_675 y I Pd 2.6138(5) . y Pd C1 2.035(3) 2_775 y Pd I 2.6139(5) 2_775 y 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 N2 C1 N1 102.7(3) . . y N2 C1 Pd 129.8(4) . . y N1 C1 Pd 127.5(4) . . y N1 C2 C3 100.7(5) . . y N1 C2 C8 114.1(4) . . y C3 C2 C8 116.2(5) . . y O1 C3 C2 110.1(5) . . y C5 C4 O1 140.0(6) . . y C5 C4 N1 106.3(4) . . y O1 C4 N1 113.7(5) . . y C4 C5 O2 142.1(5) . . y C4 C5 N2 106.2(5) . . y O2 C5 N2 111.7(5) . . y O2 C6 C7 109.8(5) . . y N2 C7 C11 115.1(4) . . y N2 C7 C6 99.7(4) . . y C11 C7 C6 116.9(5) . . y C9 C8 C10 112.2(6) . . y C9 C8 C2 112.7(7) . . y C10 C8 C2 110.5(6) . . y C13 C11 C7 112.0(6) . . y C13 C11 C12 112.5(6) . . y C7 C11 C12 111.1(5) . . y C14 C14 Cl2C 91.8(13) 2_675 . y C14 C14 Cl2A 73.9(14) 2_675 2_675 y Cl2C C14 Cl2A 147.8(14) . 2_675 y C14 C14 Cl2B 78.7(14) 2_675 . y Cl2C C14 Cl2B 19.3(7) . . y Cl2A C14 Cl2B 148.9(12) 2_675 . y C14 C14 Cl1B 89.0(8) 2_675 2_675 y Cl2C C14 Cl1B 146.0(12) . 2_675 y Cl2A C14 Cl1B 64.0(10) 2_675 2_675 y Cl2B C14 Cl1B 130.5(11) . 2_675 y C14 C14 Cl2A 64.3(13) 2_675 . y Cl2C C14 Cl2A 46.7(9) . . y Cl2A C14 Cl2A 137.2(9) 2_675 . y Cl2B C14 Cl2A 27.5(7) . . y Cl1B C14 Cl2A 104.8(12) 2_675 . y C14 C14 Cl1C 87.3(12) 2_675 2_675 y Cl2C C14 Cl1C 175.5(12) . 2_675 y Cl2A C14 Cl1C 35.7(8) 2_675 2_675 y Cl2B C14 Cl1C 156.7(11) . 2_675 y Cl1B C14 Cl1C 29.6(5) 2_675 2_675 y Cl2A C14 Cl1C 129.3(12) . 2_675 y C14 C14 Cl2E 78.4(10) 2_675 . y Cl2C C14 Cl2E 39.7(9) . . y Cl2A C14 Cl2E 108.3(15) 2_675 . y Cl2B C14 Cl2E 50.7(10) . . y Cl1B C14 Cl2E 166.9(13) 2_675 . y Cl2A C14 Cl2E 73.1(11) . . y Cl1C C14 Cl2E 144.0(13) 2_675 . y C14 C14 Cl2D 89.4(11) 2_675 . y Cl2C C14 Cl2D 14.0(7) . . y Cl2A C14 Cl2D 134.4(13) 2_675 . y Cl2B C14 Cl2D 29.9(7) . . y Cl1B C14 Cl2D 159.8(11) 2_675 . y Cl2A C14 Cl2D 56.7(9) . . y Cl1C C14 Cl2D 170.0(11) 2_675 . y Cl2E C14 Cl2D 26.0(7) . . y C14 C14 Cl2B 61.8(13) 2_675 2_675 y Cl2C C14 Cl2B 122.1(11) . 2_675 y Cl2A C14 Cl2B 25.9(7) 2_675 2_675 y Cl2B C14 Cl2B 124.8(11) . 2_675 y Cl1B C14 Cl2B 87.8(9) 2_675 2_675 y Cl2A C14 Cl2B 124.2(10) . 2_675 y Cl1C C14 Cl2B 61.1(7) 2_675 2_675 y Cl2E C14 Cl2B 83.1(12) . 2_675 y Cl2D C14 Cl2B 109.1(11) . 2_675 y C14 C14 Cl1A 71.5(4) 2_675 . y Cl2C C14 Cl1A 122.8(11) . . y Cl2A C14 Cl1A 80.5(9) 2_675 . y Cl2B C14 Cl1A 104.7(9) . . y Cl1B C14 Cl1A 27.7(5) 2_675 . y Cl2A C14 Cl1A 77.8(9) . . y Cl1C C14 Cl1A 52.7(5) 2_675 . y Cl2E C14 Cl1A 144.9(11) . . y Cl2D C14 Cl1A 134.5(9) . . y Cl2B C14 Cl1A 97.7(8) 2_675 . y C14 C14 Cl2E 64.5(9) 2_675 2_675 y Cl2C C14 Cl2E 76.5(12) . 2_675 y Cl2A C14 Cl2E 71.4(11) 2_675 2_675 y Cl2B C14 Cl2E 83.7(11) . 2_675 y Cl1B C14 Cl2E 133.0(12) 2_675 2_675 y Cl2A C14 Cl2E 97.7(12) . 2_675 y Cl1C C14 Cl2E 107.0(11) 2_675 2_675 y Cl2E C14 Cl2E 37.2(16) . 2_675 y Cl2D C14 Cl2E 63.2(12) . 2_675 y Cl2B C14 Cl2E 46.0(8) 2_675 2_675 y Cl1A C14 Cl2E 132.5(11) . 2_675 y C15 C15 Cl4D 77.7(11) 2_675 . y C15 C15 Cl4E 86.1(9) 2_675 . y Cl4D C15 Cl4E 19.1(7) . . y C15 C15 Cl3C 93.5(9) 2_675 2_675 y Cl4D C15 Cl3C 153.7(13) . 2_675 y Cl4E C15 Cl3C 172.2(12) . 2_675 y C15 C15 Cl4A 72.0(12) 2_675 2_675 y Cl4D C15 Cl4A 141.0(13) . 2_675 y Cl4E C15 Cl4A 132.9(12) . 2_675 y Cl3C C15 Cl4A 53.8(9) 2_675 2_675 y C15 C15 Cl4D 53.3(9) 2_675 2_675 y Cl4D C15 Cl4D 99.6(14) . 2_675 y Cl4E C15 Cl4D 91.5(10) . 2_675 y Cl3C C15 Cl4D 94.5(11) 2_675 2_675 y Cl4A C15 Cl4D 42.0(7) 2_675 2_675 y C15 C15 Cl4B 70.6(11) 2_675 . y Cl4D C15 Cl4B 30.3(7) . . y Cl4E C15 Cl4B 49.3(8) . . y Cl3C C15 Cl4B 123.4(11) 2_675 . y Cl4A C15 Cl4B 142.2(12) 2_675 . y Cl4D C15 Cl4B 113.8(9) 2_675 . y C15 C15 Cl4A 62.8(11) 2_675 . y Cl4D C15 Cl4A 42.8(7) . . y Cl4E C15 Cl4A 61.9(9) . . y Cl3C C15 Cl4A 111.1(11) 2_675 . y Cl4A C15 Cl4A 131.5(10) 2_675 . y Cl4D C15 Cl4A 111.9(11) 2_675 . y Cl4B C15 Cl4A 13.7(7) . . y C15 C15 Cl4C 78.2(12) 2_675 . y Cl4D C15 Cl4C 22.1(7) . . y Cl4E C15 Cl4C 40.3(7) . . y Cl3C C15 Cl4C 132.1(11) 2_675 . y Cl4A C15 Cl4C 150.2(10) 2_675 . y Cl4D C15 Cl4C 115.5(11) 2_675 . y Cl4B C15 Cl4C 10.9(7) . . y Cl4A C15 Cl4C 24.6(7) . . y C15 C15 Cl4B 65.9(11) 2_675 2_675 y Cl4D C15 Cl4B 128.5(12) . 2_675 y Cl4E C15 Cl4B 120.0(10) . 2_675 y Cl3C C15 Cl4B 66.5(9) 2_675 2_675 y Cl4A C15 Cl4B 13.0(7) 2_675 2_675 y Cl4D C15 Cl4B 29.1(6) 2_675 2_675 y Cl4B C15 Cl4B 136.0(8) . 2_675 y Cl4A C15 Cl4B 128.3(10) . 2_675 y Cl4C C15 Cl4B 141.4(10) . 2_675 y C15 C15 Cl3B 94.7(6) 2_675 2_675 y Cl4D C15 Cl3B 136.5(12) . 2_675 y Cl4E C15 Cl3B 154.0(11) . 2_675 y Cl3C C15 Cl3B 18.2(6) 2_675 2_675 y Cl4A C15 Cl3B 71.0(9) 2_675 2_675 y Cl4D C15 Cl3B 109.8(10) 2_675 2_675 y Cl4B C15 Cl3B 106.6(9) . 2_675 y Cl4A C15 Cl3B 95.4(10) . 2_675 y Cl4C C15 Cl3B 114.5(9) . 2_675 y Cl4B C15 Cl3B 83.4(9) 2_675 2_675 y C15 C15 Cl4E 49.5(7) 2_675 2_675 y Cl4D C15 Cl4E 85.6(10) . 2_675 y Cl4E C15 Cl4E 77.9(9) . 2_675 y Cl3C C15 Cl4E 107.6(10) 2_675 2_675 y Cl4A C15 Cl4E 56.0(8) 2_675 2_675 y Cl4D C15 Cl4E 14.0(6) 2_675 2_675 y Cl4B C15 Cl4E 101.5(8) . 2_675 y Cl4A C15 Cl4E 101.7(9) . 2_675 y Cl4C C15 Cl4E 102.1(8) . 2_675 y Cl4B C15 Cl4E 43.1(6) 2_675 2_675 y Cl3B C15 Cl4E 121.7(9) 2_675 2_675 y Cl1B Cl1A Cl1B 151(3) . 2_675 y Cl1B Cl1A Cl1C 135(2) . 2_675 y Cl1B Cl1A Cl1C 23.0(10) 2_675 2_675 y Cl1B Cl1A Cl1C 23.0(10) . . y Cl1B Cl1A Cl1C 135(2) 2_675 . y Cl1C Cl1A Cl1C 128.2(14) 2_675 . y Cl1B Cl1A C14 88.2(18) . . y Cl1B Cl1A C14 63.6(15) 2_675 . y Cl1C Cl1A C14 59.0(8) 2_675 . y Cl1C Cl1A C14 71.8(9) . . y Cl1B Cl1A C14 63.6(15) . 2_675 y Cl1B Cl1A C14 88.2(18) 2_675 2_675 y Cl1C Cl1A C14 71.8(9) 2_675 2_675 y Cl1C Cl1A C14 59.0(8) . 2_675 y C14 Cl1A C14 37.1(9) . 2_675 y Cl1B Cl1A Cl2A 110.5(18) . 2_675 y Cl1B Cl1A Cl2A 44.3(13) 2_675 2_675 y Cl1C Cl1A Cl2A 24.0(6) 2_675 2_675 y Cl1C Cl1A Cl2A 106.2(11) . 2_675 y C14 Cl1A Cl2A 44.7(7) . 2_675 y C14 Cl1A Cl2A 48.1(8) 2_675 2_675 y Cl1B Cl1A Cl2A 44.3(13) . . y Cl1B Cl1A Cl2A 110.5(18) 2_675 . y Cl1C Cl1A Cl2A 106.2(11) 2_675 . y Cl1C Cl1A Cl2A 24.0(6) . . y C14 Cl1A Cl2A 48.1(8) . . y C14 Cl1A Cl2A 44.7(7) 2_675 . y Cl2A Cl1A Cl2A 86.7(11) 2_675 . y Cl1C Cl1B Cl1A 134(2) . . y Cl1C Cl1B C14 78.3(13) . 2_675 y Cl1A Cl1B C14 88.6(17) . 2_675 y Cl1C Cl1B Cl1B 125.1(14) . 2_675 y Cl1A Cl1B Cl1B 14.5(16) . 2_675 y C14 Cl1B Cl1B 74.6(7) 2_675 2_675 y Cl1C Cl1B Cl2A 25.4(11) . . y Cl1A Cl1B Cl2A 115.3(17) . . y C14 Cl1B Cl2A 56.2(8) 2_675 . y Cl1B Cl1B Cl2A 103.3(8) 2_675 . y Cl1C Cl1B C14 78.3(12) . . y Cl1A Cl1B C14 66.5(17) . . y C14 Cl1B C14 35.7(8) 2_675 . y Cl1B Cl1B C14 52.4(5) 2_675 . y Cl2A Cl1B C14 53.3(7) . . y Cl1C Cl1B Cl1C 124.6(14) . 2_675 y Cl1A Cl1B Cl1C 29.8(14) . 2_675 y C14 Cl1B Cl1C 59.6(7) 2_675 2_675 y Cl1B Cl1B Cl1C 18.0(5) 2_675 2_675 y Cl2A Cl1B Cl1C 99.7(9) . 2_675 y C14 Cl1B Cl1C 46.4(6) . 2_675 y Cl1C Cl1B Cl2B 36.4(10) . . y Cl1A Cl1B Cl2B 104.9(16) . . y C14 Cl1B Cl2B 48.8(7) 2_675 . y Cl1B Cl1B Cl2B 92.4(6) 2_675 . y Cl2A Cl1B Cl2B 11.3(6) . . y C14 Cl1B Cl2B 42.1(6) . . y Cl1C Cl1B Cl2B 88.4(7) 2_675 . y Cl1B Cl1C Cl2A 133.4(19) . . y Cl1B Cl1C Cl1A 23.0(10) . . y Cl2A Cl1C Cl1A 116.6(14) . . y Cl1B Cl1C C14 72.1(13) . 2_675 y Cl2A Cl1C C14 66.1(12) . 2_675 y Cl1A Cl1C C14 68.3(8) . 2_675 y Cl1B Cl1C Cl2B 127.0(14) . . y Cl2A Cl1C Cl2B 7.2(11) . . y Cl1A Cl1C Cl2B 109.5(9) . . y C14 Cl1C Cl2B 62.4(7) 2_675 . y Cl1B Cl1C C14 77.1(12) . . y Cl2A Cl1C C14 56.9(11) . . y Cl1A Cl1C C14 60.2(8) . . y C14 Cl1C C14 35.5(8) 2_675 . y Cl2B Cl1C C14 50.1(6) . . y Cl1B Cl1C Cl2C 119.0(13) . . y Cl2A Cl1C Cl2C 15.8(10) . . y Cl1A Cl1C Cl2C 100.9(8) . . y C14 Cl1C Cl2C 57.9(6) 2_675 . y Cl2B Cl1C Cl2C 8.6(6) . . y C14 Cl1C Cl2C 41.9(5) . . y Cl1B Cl1C Cl1B 36.9(11) . 2_675 y Cl2A Cl1C Cl1B 100.9(13) . 2_675 y Cl1A Cl1C Cl1B 15.7(6) . 2_675 y C14 Cl1C Cl1B 58.8(7) 2_675 2_675 y Cl2B Cl1C Cl1B 93.8(7) . 2_675 y C14 Cl1C Cl1B 44.9(6) . 2_675 y Cl2C Cl1C Cl1B 85.2(6) . 2_675 y Cl2B Cl2A Cl1C 164(3) . . y Cl2B Cl2A Cl2C 11.8(15) . . y Cl1C Cl2A Cl2C 151.8(18) . . y Cl2B Cl2A C14 92.8(17) . 2_675 y Cl1C Cl2A C14 78.2(13) . 2_675 y Cl2C Cl2A C14 85.2(11) . 2_675 y Cl2B Cl2A Cl2D 10.9(12) . . y Cl1C Cl2A Cl2D 157.6(16) . . y Cl2C Cl2A Cl2D 12.1(9) . . y C14 Cl2A Cl2D 82.3(10) 2_675 . y Cl2B Cl2A C14 71.4(16) . . y Cl1C Cl2A C14 93.0(14) . . y Cl2C Cl2A C14 60.0(9) . . y C14 Cl2A C14 41.7(9) 2_675 . y Cl2D Cl2A C14 64.9(9) . . y Cl2B Cl2A Cl1B 143.5(19) . . y Cl1C Cl2A Cl1B 21.2(9) . . y Cl2C Cl2A Cl1B 131.9(12) . . y C14 Cl2A Cl1B 59.8(8) 2_675 . y Cl2D Cl2A Cl1B 136.3(11) . . y C14 Cl2A Cl1B 72.1(8) . . y Cl2B Cl2A Cl2E 32.7(15) . . y Cl1C Cl2A Cl2E 139.6(16) . . y Cl2C Cl2A Cl2E 29.8(10) . . y C14 Cl2A Cl2E 61.6(9) 2_675 . y Cl2D Cl2A Cl2E 21.8(8) . . y C14 Cl2A Cl2E 55.0(9) . . y Cl1B Cl2A Cl2E 119.6(10) . . y Cl2B Cl2A Cl1A 124.3(18) . . y Cl1C Cl2A Cl1A 39.4(10) . . y Cl2C Cl2A Cl1A 112.6(10) . . y C14 Cl2A Cl1A 54.8(8) 2_675 . y Cl2D Cl2A Cl1A 118.9(9) . . y C14 Cl2A Cl1A 54.1(7) . . y Cl1B Cl2A Cl1A 20.4(5) . . y Cl2E Cl2A Cl1A 106.7(10) . . y Cl2C Cl2B Cl2A 151(4) . . y Cl2C Cl2B Cl2D 27(2) . . y Cl2A Cl2B Cl2D 160(2) . . y Cl2C Cl2B Cl2E 45(2) . . y Cl2A Cl2B Cl2E 130(2) . . y Cl2D Cl2B Cl2E 29.4(12) . . y Cl2C Cl2B C14 70(2) . . y Cl2A Cl2B C14 81.1(16) . . y Cl2D Cl2B C14 86.0(13) . . y Cl2E Cl2B C14 69.4(11) . . y Cl2C Cl2B Cl1C 142(3) . . y Cl2A Cl2B Cl1C 9.3(14) . . y Cl2D Cl2B Cl1C 155.1(13) . . y Cl2E Cl2B Cl1C 127.0(13) . . y C14 Cl2B Cl1C 72.4(8) . . y Cl2C Cl2B C14 98(2) . 2_675 y Cl2A Cl2B C14 61.3(15) . 2_675 y Cl2D Cl2B C14 98.9(12) . 2_675 y Cl2E Cl2B C14 70.7(11) . 2_675 y C14 Cl2B C14 39.5(8) . 2_675 y Cl1C Cl2B C14 56.5(7) . 2_675 y Cl2C Cl2B Cl2E 60(2) . 2_675 y Cl2A Cl2B Cl2E 107.8(17) . 2_675 y Cl2D Cl2B Cl2E 51.9(13) . 2_675 y Cl2E Cl2B Cl2E 23.1(12) . 2_675 y C14 Cl2B Cl2E 53.3(9) . 2_675 y Cl1C Cl2B Cl2E 103.9(8) . 2_675 y C14 Cl2B Cl2E 47.6(8) 2_675 2_675 y Cl2C Cl2B Cl1B 126(3) . . y Cl2A Cl2B Cl1B 25.2(14) . . y Cl2D Cl2B Cl1B 139.5(12) . . y Cl2E Cl2B Cl1B 113.6(12) . . y C14 Cl2B Cl1B 56.0(7) . . y Cl1C Cl2B Cl1B 16.6(4) . . y C14 Cl2B Cl1B 43.4(6) 2_675 . y Cl2E Cl2B Cl1B 90.6(8) 2_675 . y Cl2B Cl2C Cl2E 116(3) . . y Cl2B Cl2C Cl2A 17(2) . . y Cl2E Cl2C Cl2A 116.0(17) . . y Cl2B Cl2C C14 90(3) . . y Cl2E Cl2C C14 81.1(15) . . y Cl2A Cl2C C14 73.4(11) . . y Cl2B Cl2C C14 66(2) . 2_675 y Cl2E Cl2C C14 70.6(14) . 2_675 y Cl2A Cl2C C14 54.0(9) . 2_675 y C14 Cl2C C14 36.8(8) . 2_675 y Cl2B Cl2C Cl2E 108(3) . 2_675 y Cl2E Cl2C Cl2E 22.1(13) . 2_675 y Cl2A Cl2C Cl2E 101.5(12) . 2_675 y C14 Cl2C Cl2E 59.7(10) . 2_675 y C14 Cl2C Cl2E 50.5(8) 2_675 2_675 y Cl2B Cl2C Cl1C 30(2) . . y Cl2E Cl2C Cl1C 115.2(16) . . y Cl2A Cl2C Cl1C 12.4(8) . . y C14 Cl2C Cl1C 61.6(8) . . y C14 Cl2C Cl1C 47.3(6) 2_675 . y Cl2E Cl2C Cl1C 97.4(9) 2_675 . y Cl2E Cl2D Cl2B 117(3) . . y Cl2E Cl2D Cl2A 108(2) . . y Cl2B Cl2D Cl2A 9.5(10) . . y Cl2E Cl2D C14 74(2) . . y Cl2B Cl2D C14 64.1(11) . . y Cl2A Cl2D C14 58.4(8) . . y Cl2E Cl2D Cl2E 13.2(14) . 2_675 y Cl2B Cl2D Cl2E 106.8(15) . 2_675 y Cl2A Cl2D Cl2E 97.3(12) . 2_675 y C14 Cl2D Cl2E 61.1(10) . 2_675 y Cl2E Cl2D C14 63(2) . 2_675 y Cl2B Cl2D C14 56.6(10) . 2_675 y Cl2A Cl2D C14 47.3(7) . 2_675 y C14 Cl2D C14 33.2(7) . 2_675 y Cl2E Cl2D C14 50.8(9) 2_675 2_675 y Cl2D Cl2E Cl2C 21.4(15) . . y Cl2D Cl2E Cl2E 158(2) . 2_675 y Cl2C Cl2E Cl2E 136.5(16) . 2_675 y Cl2D Cl2E Cl2B 33.3(16) . . y Cl2C Cl2E Cl2B 19.3(10) . . y Cl2E Cl2E Cl2B 127.8(15) 2_675 . y Cl2D Cl2E C14 80(2) . . y Cl2C Cl2E C14 59.2(13) . . y Cl2E Cl2E C14 78.3(12) 2_675 . y Cl2B Cl2E C14 59.8(11) . . y Cl2D Cl2E C14 95(2) . 2_675 y Cl2C Cl2E C14 75.2(15) . 2_675 y Cl2E Cl2E C14 64.5(11) 2_675 2_675 y Cl2B Cl2E C14 63.3(11) . 2_675 y C14 Cl2E C14 37.0(9) . 2_675 y Cl2D Cl2E Cl2D 149(3) . 2_675 y Cl2C Cl2E Cl2D 128(2) . 2_675 y Cl2E Cl2E Cl2D 8.9(9) 2_675 2_675 y Cl2B Cl2E Cl2D 119.0(17) . 2_675 y C14 Cl2E Cl2D 70.4(11) . 2_675 y C14 Cl2E Cl2D 55.7(10) 2_675 2_675 y Cl2D Cl2E Cl2A 50.4(19) . . y Cl2C Cl2E Cl2A 34.2(11) . . y Cl2E Cl2E Cl2A 111.3(14) 2_675 . y Cl2B Cl2E Cl2A 17.1(8) . . y C14 Cl2E Cl2A 52.0(8) . . y C14 Cl2E Cl2A 47.0(8) 2_675 . y Cl2D Cl2E Cl2A 102.7(13) 2_675 . y Cl2D Cl2E Cl2C 137(3) . 2_675 y Cl2C Cl2E Cl2C 116(2) . 2_675 y Cl2E Cl2E Cl2C 21.3(7) 2_675 2_675 y Cl2B Cl2E Cl2C 106.9(14) . 2_675 y C14 Cl2E Cl2C 59.1(10) . 2_675 y C14 Cl2E Cl2C 43.8(8) 2_675 2_675 y Cl2D Cl2E Cl2C 12.4(5) 2_675 2_675 y Cl2A Cl2E Cl2C 90.8(11) . 2_675 y Cl2D Cl2E Cl2B 129(2) . 2_675 y Cl2C Cl2E Cl2B 107.9(17) . 2_675 y Cl2E Cl2E Cl2B 29.0(9) 2_675 2_675 y Cl2B Cl2E Cl2B 102.9(14) . 2_675 y C14 Cl2E Cl2B 49.3(9) . 2_675 y C14 Cl2E Cl2B 43.0(7) 2_675 2_675 y Cl2D Cl2E Cl2B 21.3(6) 2_675 2_675 y Cl2A Cl2E Cl2B 88.5(10) . 2_675 y Cl2C Cl2E Cl2B 12.5(5) 2_675 2_675 y Cl3B Cl3A Cl3B 166(3) 2_675 . y Cl3B Cl3A Cl3C 27.3(10) 2_675 2_675 y Cl3B Cl3A Cl3C 141(2) . 2_675 y Cl3B Cl3A Cl3C 141(2) 2_675 . y Cl3B Cl3A Cl3C 27.3(10) . . y Cl3C Cl3A Cl3C 128(2) 2_675 . y Cl3B Cl3A C15 100.2(16) 2_675 2_675 y Cl3B Cl3A C15 65.9(13) . 2_675 y Cl3C Cl3A C15 77.8(12) 2_675 2_675 y Cl3C Cl3A C15 52.1(10) . 2_675 y Cl3B Cl3A C15 65.9(13) 2_675 . y Cl3B Cl3A C15 100.2(16) . . y Cl3C Cl3A C15 52.1(10) 2_675 . y Cl3C Cl3A C15 77.8(12) . . y C15 Cl3A C15 38.4(8) 2_675 . y Cl3B Cl3A Cl4A 63.3(12) 2_675 2_675 y Cl3B Cl3A Cl4A 105.8(14) . 2_675 y Cl3C Cl3A Cl4A 36.1(9) 2_675 2_675 y Cl3C Cl3A Cl4A 100.0(13) . 2_675 y C15 Cl3A Cl4A 48.4(7) 2_675 2_675 y C15 Cl3A Cl4A 45.0(6) . 2_675 y Cl3B Cl3A Cl4A 105.8(14) 2_675 . y Cl3B Cl3A Cl4A 63.3(12) . . y Cl3C Cl3A Cl4A 100.0(13) 2_675 . y Cl3C Cl3A Cl4A 36.1(9) . . y C15 Cl3A Cl4A 45.0(6) 2_675 . y C15 Cl3A Cl4A 48.4(7) . . y Cl4A Cl3A Cl4A 86.8(11) 2_675 . y Cl3C Cl3B Cl3A 108(2) . . y Cl3C Cl3B Cl3B 103(2) . 2_675 y Cl3A Cl3B Cl3B 7.0(14) . 2_675 y Cl3C Cl3B C15 56(2) . 2_675 y Cl3A Cl3B C15 87.1(15) . 2_675 y Cl3B Cl3B C15 80.2(5) 2_675 2_675 y Cl3C Cl3B Cl3C 101(2) . 2_675 y Cl3A Cl3B Cl3C 22.3(12) . 2_675 y Cl3B Cl3B Cl3C 16.6(5) 2_675 2_675 y C15 Cl3B Cl3C 66.5(7) 2_675 2_675 y Cl3C Cl3B Cl4A 15.5(19) . . y Cl3A Cl3B Cl4A 93.1(14) . . y Cl3B Cl3B Cl4A 87.8(7) 2_675 . y C15 Cl3B Cl4A 50.3(7) 2_675 . y Cl3C Cl3B Cl4A 86.0(8) 2_675 . y Cl3C Cl3B Cl4B 19.2(19) . . y Cl3A Cl3B Cl4B 89.8(13) . . y Cl3B Cl3B Cl4B 84.3(6) 2_675 . y C15 Cl3B Cl4B 47.8(6) 2_675 . y Cl3C Cl3B Cl4B 82.0(7) 2_675 . y Cl4A Cl3B Cl4B 4.0(7) . . y Cl3B Cl3C Cl3A 44.4(18) . . y Cl3B Cl3C Cl4A 158(3) . . y Cl3A Cl3C Cl4A 114.2(14) . . y Cl3B Cl3C C15 105(2) . 2_675 y Cl3A Cl3C C15 89.9(12) . 2_675 y Cl4A Cl3C C15 65.5(10) . 2_675 y Cl3B Cl3C Cl4B 155(2) . . y Cl3A Cl3C Cl4B 111.0(12) . . y Cl4A Cl3C Cl4B 4.0(9) . . y C15 Cl3C Cl4B 62.5(8) 2_675 . y Cl3B Cl3C Cl3B 60(2) . 2_675 y Cl3A Cl3C Cl3B 16.3(8) . 2_675 y Cl4A Cl3C Cl3B 98.2(10) . 2_675 y C15 Cl3C Cl3B 80.0(8) 2_675 2_675 y Cl4B Cl3C Cl3B 94.9(7) . 2_675 y Cl3B Cl3C C15 105(2) . . y Cl3A Cl3C C15 67.5(11) . . y Cl4A Cl3C C15 55.5(9) . . y C15 Cl3C C15 38.4(8) 2_675 . y Cl4B Cl3C C15 51.5(6) . . y Cl3B Cl3C C15 52.4(6) 2_675 . y Cl3B Cl3C Cl4C 152(2) . . y Cl3A Cl3C Cl4C 108.1(11) . . y Cl4A Cl3C Cl4C 7.0(7) . . y C15 Cl3C Cl4C 61.0(7) 2_675 . y Cl4B Cl3C Cl4C 3.0(6) . . y Cl3B Cl3C Cl4C 92.0(7) 2_675 . y C15 Cl3C Cl4C 48.6(6) . . y Cl3B Cl3C Cl3C 64(2) . 2_675 y Cl3A Cl3C Cl3C 25.9(10) . 2_675 y Cl4A Cl3C Cl3C 95.0(10) . 2_675 y C15 Cl3C Cl3C 65.3(7) 2_675 2_675 y Cl4B Cl3C Cl3C 91.3(7) . 2_675 y Cl3B Cl3C Cl3C 15.2(5) 2_675 2_675 y C15 Cl3C Cl3C 42.7(5) . 2_675 y Cl4C Cl3C Cl3C 88.2(7) . 2_675 y Cl3B Cl3C Cl4D 140(2) . . y Cl3A Cl3C Cl4D 100.9(11) . . y Cl4A Cl3C Cl4D 22.6(8) . . y C15 Cl3C Cl4D 44.8(7) 2_675 . y Cl4B Cl3C Cl4D 18.9(5) . . y Cl3B Cl3C Cl4D 84.8(7) 2_675 . y C15 Cl3C Cl4D 35.2(5) . . y Cl4C Cl3C Cl4D 16.7(4) . . y Cl3C Cl3C Cl4D 77.5(5) 2_675 . y Cl4C Cl4A Cl4D 33.2(11) . . y Cl4C Cl4A Cl3C 159(2) . . y Cl4D Cl4A Cl3C 129.5(17) . . y Cl4C Cl4A C15 104.7(17) . 2_675 y Cl4D Cl4A C15 71.5(12) . 2_675 y Cl3C Cl4A C15 60.7(10) . 2_675 y Cl4C Cl4A Cl4E 35.9(12) . . y Cl4D Cl4A Cl4E 3.2(9) . . y Cl3C Cl4A Cl4E 126.5(13) . . y C15 Cl4A Cl4E 68.9(9) 2_675 . y Cl4C Cl4A C15 78.0(15) . . y Cl4D Cl4A C15 52.2(10) . . y Cl3C Cl4A C15 81.5(11) . . y C15 Cl4A C15 45.2(9) 2_675 . y Cl4E Cl4A C15 49.1(7) . . y Cl4C Cl4A Cl3B 153.5(19) . . y Cl4D Cl4A Cl3B 125.2(15) . . y Cl3C Cl4A Cl3B 6.2(7) . . y C15 Cl4A Cl3B 58.7(8) 2_675 . y Cl4E Cl4A Cl3B 122.1(10) . . y C15 Cl4A Cl3B 75.9(9) . . y Cl4C Cl4A Cl3A 131.4(18) . . y Cl4D Cl4A Cl3A 110.2(13) . . y Cl3C Cl4A Cl3A 29.7(7) . . y C15 Cl4A Cl3A 59.1(8) 2_675 . y Cl4E Cl4A Cl3A 107.1(9) . . y C15 Cl4A Cl3A 58.0(7) . . y Cl3B Cl4A Cl3A 23.6(4) . . y Cl4D Cl4B Cl4E 2.4(12) . . y Cl4D Cl4B C15 52.8(10) . . y Cl4E Cl4B C15 53.1(8) . . y Cl4D Cl4B C15 69.4(12) . 2_675 y Cl4E Cl4B C15 71.3(7) . 2_675 y C15 Cl4B C15 43.5(8) . 2_675 y Cl4D Cl4B Cl3C 118.2(15) . . y Cl4E Cl4B Cl3C 119.7(10) . . y C15 Cl4B Cl3C 71.8(8) . . y C15 Cl4B Cl3C 51.0(8) 2_675 . y Cl4D Cl4B Cl3B 114.1(14) . . y Cl4E Cl4B Cl3B 115.4(9) . . y C15 Cl4B Cl3B 66.2(7) . . y C15 Cl4B Cl3B 48.8(7) 2_675 . y Cl3C Cl4B Cl3B 6.0(6) . . y Cl4D Cl4C Cl4A 111(2) . . y Cl4D Cl4C Cl4E 10.6(15) . . y Cl4A Cl4C Cl4E 121.5(18) . . y Cl4D Cl4C C15 48.2(15) . . y Cl4A Cl4C C15 77.4(16) . . y Cl4E Cl4C C15 53.7(8) . . y Cl4D Cl4C C15 57.5(15) . 2_675 y Cl4A Cl4C C15 53.8(14) . 2_675 y Cl4E Cl4C C15 67.9(9) . 2_675 y C15 Cl4C C15 40.7(8) . 2_675 y Cl4D Cl4C Cl3C 100.6(17) . . y Cl4A Cl4C Cl3C 13.6(14) . . y Cl4E Cl4C Cl3C 110.3(10) . . y C15 Cl4C Cl3C 63.8(7) . . y C15 Cl4C Cl3C 44.3(6) 2_675 . y Cl4C Cl4D Cl4B 20.5(17) . . y Cl4C Cl4D Cl4A 35.6(16) . . y Cl4B Cl4D Cl4A 15.2(14) . . y Cl4C Cl4D C15 109.7(19) . . y Cl4B Cl4D C15 96.9(13) . . y Cl4A Cl4D C15 84.9(12) . . y Cl4C Cl4D C15 102.0(19) . 2_675 y Cl4B Cl4D C15 81.5(13) . 2_675 y Cl4A Cl4D C15 66.5(11) . 2_675 y C15 Cl4D C15 49.0(9) . 2_675 y Cl4C Cl4D Cl4E 140.6(18) . 2_675 y Cl4B Cl4D Cl4E 120.1(14) . 2_675 y Cl4A Cl4D Cl4E 105.4(12) . 2_675 y C15 Cl4D Cl4E 56.1(8) . 2_675 y C15 Cl4D Cl4E 39.3(7) 2_675 2_675 y Cl4C Cl4D Cl4D 137.0(17) . 2_675 y Cl4B Cl4D Cl4D 116.7(14) . 2_675 y Cl4A Cl4D Cl4D 101.5(12) . 2_675 y C15 Cl4D Cl4D 44.9(9) . 2_675 y C15 Cl4D Cl4D 35.4(7) 2_675 2_675 y Cl4E Cl4D Cl4D 11.2(4) 2_675 2_675 y Cl4C Cl4D Cl3C 62.6(16) . . y Cl4B Cl4D Cl3C 42.9(12) . . y Cl4A Cl4D Cl3C 27.8(10) . . y C15 Cl4D Cl3C 60.8(8) . . y C15 Cl4D Cl3C 40.8(7) 2_675 . y Cl4E Cl4D Cl3C 80.0(6) 2_675 . y Cl4D Cl4D Cl3C 74.5(5) 2_675 . y Cl4C Cl4E Cl4B 12.1(10) . . y Cl4C Cl4E C15 86.0(10) . . y Cl4B Cl4E C15 77.6(9) . . y Cl4C Cl4E Cl4A 22.6(8) . . y Cl4B Cl4E Cl4A 10.6(9) . . y C15 Cl4E Cl4A 69.0(10) . . y Cl4C Cl4E C15 77.6(9) . 2_675 y Cl4B Cl4E C15 65.6(8) . 2_675 y C15 Cl4E C15 44.5(9) . 2_675 y Cl4A Cl4E C15 55.1(8) . 2_675 y Cl4C Cl4E Cl4E 118.2(9) . 2_675 y Cl4B Cl4E Cl4E 106.3(8) . 2_675 y C15 Cl4E Cl4E 60.5(7) . 2_675 y Cl4A Cl4E Cl4E 96.2(7) . 2_675 y C15 Cl4E Cl4E 41.5(5) 2_675 2_675 y Cl4C Cl4E Cl4D 115.8(9) . 2_675 y Cl4B Cl4E Cl4D 103.7(9) . 2_675 y C15 Cl4E Cl4D 49.2(7) . 2_675 y Cl4A Cl4E Cl4D 93.1(8) . 2_675 y C15 Cl4E Cl4D 38.3(6) 2_675 2_675 y Cl4E Cl4E Cl4D 11.8(4) 2_675 2_675 y C1 N1 C4 112.4(4) . . y C1 N1 C2 138.1(4) . . y C4 N1 C2 109.5(4) . . y C1 N2 C5 112.4(4) . . y C1 N2 C7 136.7(4) . . y C5 N2 C7 110.8(4) . . y C4 O1 C3 106.0(4) . . y C5 O2 C6 107.3(4) . . y C1 Pd C1 179.0(3) 2_775 . y C1 Pd I 90.11(10) 2_775 . y C1 Pd I 89.89(10) . . y C1 Pd I 89.89(10) 2_775 2_775 y C1 Pd I 90.11(10) . 2_775 y I Pd I 179.85(3) . 2_775 y _diffrn_measured_fraction_theta_max 0.891 _diffrn_reflns_theta_full 33.10 _diffrn_measured_fraction_theta_full 0.891 _refine_diff_density_max 0.762 _refine_diff_density_min -0.797 _refine_diff_density_rms 0.103