Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2003 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 loop_ _publ_author_name 'Karl Coleman' 'Hamish T. Chamberlayne' 'Andrew R. Cowley' 'Malcolm L. H. Green' ; S.Turberville ; _publ_contact_author_name 'Dr Karl Coleman' _publ_contact_author_address ; Inorganic Chemistry Laboratory University of Oxford South Parks Road Oxford Oxon OX1 3QR UNITED KINGDOM ; _publ_contact_author_email KARL.COLEMAN@CHEM.OX.AC.UK _publ_section_title ; Silver (I) Complex of a New Imino-N-Heterocyclic Carbene and Ligand Transfer to Palladium (II) and Rhodium (I) ; data_COMPOUND_1 _database_code_CSD 209030 #========================================================================== # 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 _refine_special_details ; the most probable orientations of the methyl groups C20, C21, C22 were determined by examination of a difference Fourier map before hydrogens were included in the model. The methyl hydrogens were subsequently positioned geometrically in the appropriate locations. ; #============================================================= _cell_length_a 12.4006(4) _cell_angle_alpha 90 _cell_length_b 12.5704(3) _cell_angle_beta 96.5002(11) _cell_length_c 14.3606(5) _cell_angle_gamma 90 _cell_volume 2224.1 _symmetry_cell_setting 'Monoclinic ' _symmetry_space_group_name_H-M 'P 1 21/c 1 ' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x,y+1/2,-z+1/2 x,-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 '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 ' C21 H32 Br1 N3 ' _chemical_formula_moiety ' C21 H32 Br1 N3 ' _chemical_compound_source ; ? ; _chemical_formula_weight 406.41 _cell_measurement_reflns_used 16111 _cell_measurement_theta_min 5 _cell_measurement_theta_max 28 _cell_measurement_temperature 150 _cell_formula_units_Z 4 _exptl_crystal_description ' block ' _exptl_crystal_colour ' colourless ' _exptl_crystal_size_min 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_max 0.36 _exptl_crystal_density_diffrn 1.214 _exptl_crystal_density_meas 'not measured' _exptl_crystal_F_000 854.613 _exptl_absorpt_coefficient_mu 1.856 _diffrn_measurement_method \w _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; Denzo/Scalepack (Otwinowski & Minor, 1996) ; _exptl_absorpt_correction_T_min 0.51 _exptl_absorpt_correction_T_max 0.57 _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 16111 _reflns_number_total 5271 _diffrn_reflns_av_R_equivalents 0.031 _diffrn_measured_fraction_theta_max 0.996 _reflns_number_gt 3978 _diffrn_reflns_theta_min 5.14 _diffrn_reflns_theta_max 27.47 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _reflns_limit_h_min -16 _reflns_limit_h_max 15 _reflns_limit_k_min 0 _reflns_limit_k_max 16 _reflns_limit_l_min 0 _reflns_limit_l_max 18 _refine_diff_density_min -0.43 _refine_diff_density_max 0.31 _reflns_threshold_expression >3.00\s(I) _refine_ls_number_reflns 3978 _refine_ls_number_parameters 226 _refine_ls_R_factor_gt 0.0296 _refine_ls_wR_factor_ref 0.0392 _refine_ls_goodness_of_fit_ref 1.0043 _refine_ls_shift/su_max 0.001200 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Chebychev polynomial with 3 parameters (Carruthers & Watkin , 1979) 6.15 -2.00 5.33 ; _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 Br1 0.409816(14) 0.442021(14) 0.319282(11) 0.0290 1.0000 Uani N1 0.41851(11) 0.14942(11) 0.0853(1) 0.0226 1.0000 Uani N3 0.55717(12) 0.24905(12) 0.0697(1) 0.0245 1.0000 Uani N10 0.16732(12) 0.15662(12) 0.04658(12) 0.0306 1.0000 Uani C2 0.49925(13) 0.16683(13) 0.03395(12) 0.0235 1.0000 Uani C5 0.42600(15) 0.22246(15) 0.15742(13) 0.0284 1.0000 Uani C4 0.51216(15) 0.28516(15) 0.14739(13) 0.0289 1.0000 Uani C6 0.34269(13) 0.05964(12) 0.06788(12) 0.0233 1.0000 Uani C7 0.22749(13) 0.08620(14) 0.08875(12) 0.0247 1.0000 Uani C8 0.18233(14) 0.01604(15) 0.16171(13) 0.0292 1.0000 Uani C9A 0.25569(18) 0.02195(18) 0.25548(14) 0.0385 1.0000 Uani C9B 0.17797(17) -0.09893(16) 0.12522(16) 0.0366 1.0000 Uani C9C 0.06728(18) 0.05087(18) 0.17735(17) 0.0416 1.0000 Uani C11 0.20373(15) 0.22103(16) -0.02935(15) 0.0336 1.0000 Uani C12 0.1994(2) 0.33713(18) -0.00083(19) 0.0474 1.0000 Uani C13 0.1272(2) 0.1973(2) -0.11759(18) 0.0488 1.0000 Uani C14 0.64475(13) 0.29730(13) 0.02566(12) 0.0242 1.0000 Uani C15 0.61684(14) 0.35934(14) -0.05385(12) 0.0272 1.0000 Uani C16 0.70096(15) 0.40236(15) -0.09821(13) 0.0291 1.0000 Uani C17 0.80921(15) 0.38479(14) -0.06405(13) 0.0279 1.0000 Uani C18 0.83316(14) 0.32369(14) 0.01623(13) 0.0279 1.0000 Uani C19 0.75170(14) 0.27745(14) 0.06286(12) 0.0263 1.0000 Uani C20 0.50011(16) 0.37940(18) -0.09199(15) 0.0379 1.0000 Uani C21 0.89804(16) 0.42913(17) -0.11643(15) 0.0372 1.0000 Uani C22 0.77880(16) 0.20679(17) 0.14685(14) 0.0364 1.0000 Uani H21 0.5141 0.1249 -0.0224 0.0283 1.0000 Uiso H51 0.3767 0.2279 0.2077 0.0344 1.0000 Uiso H41 0.5384 0.3462 0.1885 0.0349 1.0000 Uiso H61 0.3703 -0.0013 0.1086 0.0282 1.0000 Uiso H62 0.3400 0.0385 0.0005 0.0282 1.0000 Uiso H9A1 0.2252 -0.0244 0.3027 0.0466 1.0000 Uiso H9A2 0.3303 -0.0030 0.2463 0.0466 1.0000 Uiso H9A3 0.2592 0.0971 0.2784 0.0466 1.0000 Uiso H9B1 0.1485 -0.1464 0.1721 0.0446 1.0000 Uiso H9B2 0.2527 -0.1228 0.1152 0.0446 1.0000 Uiso H9B3 0.1298 -0.1024 0.0645 0.0446 1.0000 Uiso H9C1 0.0393 0.0038 0.2254 0.0514 1.0000 Uiso H9C2 0.0688 0.1262 0.1998 0.0514 1.0000 Uiso H9C3 0.0186 0.0453 0.1171 0.0514 1.0000 Uiso H101 0.2797 0.2043 -0.0416 0.0399 1.0000 Uiso H121 0.2239 0.3828 -0.0514 0.0566 1.0000 Uiso H122 0.2483 0.3486 0.0586 0.0566 1.0000 Uiso H123 0.1233 0.3564 0.0091 0.0566 1.0000 Uiso H131 0.1496 0.2399 -0.1710 0.0572 1.0000 Uiso H132 0.0514 0.2167 -0.1070 0.0572 1.0000 Uiso H133 0.1306 0.1198 -0.1327 0.0572 1.0000 Uiso H161 0.6834 0.4467 -0.1557 0.0349 1.0000 Uiso H181 0.9108 0.3124 0.0414 0.0332 1.0000 Uiso H201 0.4976 0.4255 -0.1490 0.0448 1.0000 Uiso H202 0.4619 0.4159 -0.0432 0.0448 1.0000 Uiso H203 0.4635 0.3101 -0.1090 0.0448 1.0000 Uiso H211 0.9123 0.3789 -0.1676 0.0455 1.0000 Uiso H212 0.9657 0.4382 -0.0722 0.0455 1.0000 Uiso H213 0.8749 0.4996 -0.1442 0.0455 1.0000 Uiso H221 0.8594 0.2029 0.1623 0.0430 1.0000 Uiso H222 0.7457 0.2367 0.2015 0.0430 1.0000 Uiso H223 0.7494 0.1338 0.1325 0.0430 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 Br1 0.03415(11) 0.03146(11) 0.0213(1) 0.00088(7) 0.00317(6) 0.00148(7) N1 0.0213(6) 0.0247(7) 0.0221(6) -0.0020(5) 0.0042(5) 0.0001(5) N3 0.0234(6) 0.0285(7) 0.0220(7) -0.0033(5) 0.0037(5) -0.0021(5) N10 0.0227(7) 0.0293(8) 0.0401(9) 0.0020(6) 0.0048(6) 0.0009(6) C2 0.0214(7) 0.0245(7) 0.0247(8) -0.0022(6) 0.0039(6) -0.0006(6) C5 0.0287(8) 0.0323(8) 0.0251(8) -0.0060(7) 0.0073(6) -0.0007(7) C4 0.0308(8) 0.0335(9) 0.0230(8) -0.0086(7) 0.0060(6) -0.0037(7) C6 0.0226(7) 0.0217(7) 0.0261(8) -0.0025(6) 0.0049(6) -0.0021(6) C7 0.0221(7) 0.0264(8) 0.0262(8) -0.0053(6) 0.0055(6) -0.0018(6) C8 0.0275(8) 0.0306(9) 0.0313(9) -0.0011(7) 0.0111(7) -0.0027(7) C9A 0.0456(11) 0.043(1) 0.0282(9) 0.0012(8) 0.0078(8) -0.0057(9) C9B 0.039(1) 0.0286(9) 0.0436(11) -0.0004(8) 0.0121(8) -0.0069(8) C9C 0.0323(9) 0.0438(12) 0.0525(13) -0.0010(9) 0.0214(9) -0.0024(8) C11 0.0275(9) 0.0315(9) 0.041(1) 0.0076(8) -0.0013(7) -0.0000(7) C12 0.0502(12) 0.033(1) 0.0582(14) 0.007(1) 0.003(1) -0.0015(9) C13 0.0443(12) 0.0500(13) 0.0487(13) 0.011(1) -0.009(1) -0.009(1) C14 0.0218(7) 0.0259(8) 0.0248(8) -0.0037(6) 0.0023(6) -0.0042(6) C15 0.0249(8) 0.0297(8) 0.0265(8) -0.0018(6) 0.0008(6) -0.0003(6) C16 0.0313(9) 0.0308(8) 0.0251(8) 0.0026(7) 0.0025(7) -0.0014(7) C17 0.0288(8) 0.0267(8) 0.0290(9) -0.0030(7) 0.0069(7) -0.0033(7) C18 0.0233(8) 0.0288(8) 0.0309(9) -0.0033(7) 0.0006(6) -0.0010(7) C19 0.0255(8) 0.0274(8) 0.0256(8) -0.0027(6) 0.0007(6) -0.0005(7) C20 0.0266(9) 0.0457(11) 0.0396(11) 0.0086(9) -0.0039(7) 0.0032(8) C21 0.0328(9) 0.0409(11) 0.0400(11) 0.0017(8) 0.0132(8) -0.0048(8) C22 0.0317(9) 0.0443(11) 0.032(1) 0.0108(8) -0.0029(7) -0.0011(8) _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 N1 . C2 . 1.327(2) yes N1 . C5 . 1.380(2) yes N1 . C6 . 1.472(2) yes N3 . C2 . 1.328(2) yes N3 . C4 . 1.379(2) yes N3 . C14 . 1.450(2) yes N10 . C7 . 1.267(2) yes N10 . C11 . 1.470(2) yes C2 . H21 . 1.0000 no C5 . C4 . 1.349(3) yes C5 . H51 . 1.0000 no C4 . H41 . 1.0000 no C6 . C7 . 1.529(2) yes C6 . H61 . 1.0000 no C6 . H62 . 1.0000 no C7 . C8 . 1.524(2) yes C8 . C9A . 1.539(3) yes C8 . C9B . 1.536(3) yes C8 . C9C . 1.533(3) yes C9A . H9A1 . 1.000 no C9A . H9A2 . 1.000 no C9A . H9A3 . 1.000 no C9B . H9B1 . 1.000 no C9B . H9B2 . 1.000 no C9B . H9B3 . 1.000 no C9C . H9C1 . 1.000 no C9C . H9C2 . 1.000 no C9C . H9C3 . 1.000 no C11 . C12 . 1.518(3) yes C11 . C13 . 1.524(3) yes C11 . H101 . 1.0000 no C12 . H121 . 1.000 no C12 . H122 . 1.000 no C12 . H123 . 1.000 no C13 . H131 . 1.000 no C13 . H132 . 1.000 no C13 . H133 . 1.000 no C14 . C15 . 1.394(3) yes C14 . C19 . 1.395(2) yes C15 . C16 . 1.392(3) yes C15 . C20 . 1.510(2) yes C16 . C17 . 1.394(3) yes C16 . H161 . 1.0000 no C17 . C18 . 1.389(3) yes C17 . C21 . 1.509(2) yes C18 . C19 . 1.400(3) yes C18 . H181 . 1.0000 no C19 . C22 . 1.505(2) yes C20 . H201 . 1.000 no C20 . H202 . 1.000 no C20 . H203 . 1.000 no C21 . H211 . 1.000 no C21 . H212 . 1.000 no C21 . H213 . 1.000 no C22 . H221 . 1.000 no C22 . H222 . 1.000 no C22 . H223 . 1.000 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 C2 . N1 . C5 . 108.46(14) yes C2 . N1 . C6 . 122.67(14) yes C5 . N1 . C6 . 128.68(14) yes C2 . N3 . C4 . 108.55(14) yes C2 . N3 . C14 . 123.75(14) yes C4 . N3 . C14 . 127.35(14) yes C7 . N10 . C11 . 121.73(15) yes N1 . C2 . N3 . 108.81(14) yes N1 . C2 . H21 . 125.59 no N3 . C2 . H21 . 125.59 no N1 . C5 . C4 . 107.18(15) yes N1 . C5 . H51 . 126.41 no C4 . C5 . H51 . 126.41 no N3 . C4 . C5 . 106.99(15) yes N3 . C4 . H41 . 126.51 no C5 . C4 . H41 . 126.51 no N1 . C6 . C7 . 113.09(13) yes N1 . C6 . H61 . 108.56 no C7 . C6 . H61 . 108.56 no N1 . C6 . H62 . 108.56 no C7 . C6 . H62 . 108.56 no H61 . C6 . H62 . 109.47 no N10 . C7 . C6 . 124.86(16) yes N10 . C7 . C8 . 119.39(15) yes C6 . C7 . C8 . 115.63(15) yes C7 . C8 . C9A . 110.29(15) yes C7 . C8 . C9B . 108.14(15) yes C9A . C8 . C9B . 109.78(16) yes C7 . C8 . C9C . 110.85(16) yes C9A . C8 . C9C . 109.01(17) yes C9B . C8 . C9C . 108.74(16) yes C8 . C9A . H9A1 . 109.47 no C8 . C9A . H9A2 . 109.47 no H9A1 . C9A . H9A2 . 109.5 no C8 . C9A . H9A3 . 109.47 no H9A1 . C9A . H9A3 . 109.48 no H9A2 . C9A . H9A3 . 109.5 no C8 . C9B . H9B1 . 109.47 no C8 . C9B . H9B2 . 109.47 no H9B1 . C9B . H9B2 . 109.5 no C8 . C9B . H9B3 . 109.47 no H9B1 . C9B . H9B3 . 109.48 no H9B2 . C9B . H9B3 . 109.5 no C8 . C9C . H9C1 . 109.5 no C8 . C9C . H9C2 . 109.47 no H9C1 . C9C . H9C2 . 109.5 no C8 . C9C . H9C3 . 109.47 no H9C1 . C9C . H9C3 . 109.5 no H9C2 . C9C . H9C3 . 109.5 no N10 . C11 . C12 . 107.84(18) yes N10 . C11 . C13 . 107.15(16) yes C12 . C11 . C13 . 112.01(18) yes N10 . C11 . H101 . 112.93 no C12 . C11 . H101 . 108.15 no C13 . C11 . H101 . 108.8 no C11 . C12 . H121 . 109.5 no C11 . C12 . H122 . 109.47 no H121 . C12 . H122 . 109.5 no C11 . C12 . H123 . 109.5 no H121 . C12 . H123 . 109.5 no H122 . C12 . H123 . 109.5 no C11 . C13 . H131 . 109.5 no C11 . C13 . H132 . 109.5 no H131 . C13 . H132 . 109.5 no C11 . C13 . H133 . 109.5 no H131 . C13 . H133 . 109.5 no H132 . C13 . H133 . 109.5 no N3 . C14 . C15 . 117.56(15) yes N3 . C14 . C19 . 118.98(16) yes C15 . C14 . C19 . 123.44(16) yes C14 . C15 . C16 . 117.58(16) yes C14 . C15 . C20 . 121.98(16) yes C16 . C15 . C20 . 120.44(17) yes C15 . C16 . C17 . 121.28(17) yes C15 . C16 . H161 . 119.36 no C17 . C16 . H161 . 119.36 no C16 . C17 . C18 . 119.13(16) yes C16 . C17 . C21 . 119.62(17) yes C18 . C17 . C21 . 121.22(17) yes C17 . C18 . C19 . 121.90(16) yes C17 . C18 . H181 . 119.05 no C19 . C18 . H181 . 119.05 no C14 . C19 . C18 . 116.66(16) yes C14 . C19 . C22 . 121.93(16) yes C18 . C19 . C22 . 121.38(16) yes C15 . C20 . H201 . 109.47 no C15 . C20 . H202 . 109.47 no H201 . C20 . H202 . 109.5 no C15 . C20 . H203 . 109.47 no H201 . C20 . H203 . 109.5 no H202 . C20 . H203 . 109.48 no C17 . C21 . H211 . 109.47 no C17 . C21 . H212 . 109.47 no H211 . C21 . H212 . 109.48 no C17 . C21 . H213 . 109.47 no H211 . C21 . H213 . 109.5 no H212 . C21 . H213 . 109.48 no C19 . C22 . H221 . 109.47 no C19 . C22 . H222 . 109.47 no H221 . C22 . H222 . 109.48 no C19 . C22 . H223 . 109.47 no H221 . C22 . H223 . 109.5 no H222 . C22 . H223 . 109.48 no # #===END # # # # data_COMPOUND_3 _database_code_CSD 209031 #========================================================================== # 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_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment ; mixed the most probable orientations of the methyl groups C20, C21, C22 were determined by examination of a difference Fourier map before hydrogens were included in the model. The methyl hydrogens were subsequently positioned geometrically in the appropriate locations. ; #============================================================= _cell_length_a 11.2224(2) _cell_angle_alpha 90 _cell_length_b 19.2162(3) _cell_angle_beta 93.4326(7) _cell_length_c 15.4168(2) _cell_angle_gamma 90 _cell_volume 3318.7 _symmetry_cell_setting 'Monoclinic ' _symmetry_space_group_name_H-M 'P 1 21/c 1 ' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x,y+1/2,-z+1/2 x,-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 '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 '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 ' C23.07 H35.14 Cl6.14 N3 Pd1 ' _chemical_formula_moiety ' C23.07 H35.14 Cl6.14 N3 Pd1 ' _chemical_compound_source ; synthesis as described ; _chemical_formula_weight 678.69 _cell_measurement_reflns_used 41359 _cell_measurement_theta_min 5 _cell_measurement_theta_max 28 _cell_measurement_temperature 150 _cell_formula_units_Z 4 _exptl_crystal_description ' block ' _exptl_crystal_colour ' yellow ' _exptl_crystal_size_min 0.10 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_max 0.25 _exptl_crystal_density_diffrn 1.358 _exptl_crystal_density_meas 'not measured' _exptl_crystal_F_000 1378.561 _exptl_absorpt_coefficient_mu 1.069 _diffrn_measurement_method \w _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; Denzo/Scalepack (Otwinowski & Minor, 1996) ; _exptl_absorpt_correction_T_min 0.77 _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 150 _diffrn_reflns_number 41359 _reflns_number_total 7741 _diffrn_reflns_av_R_equivalents 0.045 _diffrn_measured_fraction_theta_max 0.999 _reflns_number_gt 5616 _diffrn_reflns_theta_min 5.09 _diffrn_reflns_theta_max 27.45 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _reflns_limit_h_min -14 _reflns_limit_h_max 14 _reflns_limit_k_min 0 _reflns_limit_k_max 24 _reflns_limit_l_min 0 _reflns_limit_l_max 19 _refine_diff_density_min -0.86 _refine_diff_density_max 1.17 _reflns_threshold_expression >3.00\s(I) _refine_ls_number_reflns 5616 _refine_ls_number_parameters 344 _refine_ls_R_factor_gt 0.0464 _refine_ls_wR_factor_ref 0.0504 _refine_ls_goodness_of_fit_ref 1.0273 _refine_ls_shift/su_max 0.038279 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Chebychev polynomial with 3 parameters (Carruthers & Watkin , 1979) 2.55 -.0671 1.51 ; _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 0.29467(2) 0.256713(12) 0.371806(15) 0.0253 1.0000 Uani Cl1 0.1873(1) 0.18927(6) 0.26667(6) 0.0451 1.0000 Uani Cl2 0.45782(8) 0.26818(5) 0.28853(5) 0.0335 1.0000 Uani N1 0.3465(3) 0.29965(15) 0.55130(17) 0.0291 1.0000 Uani N3 0.4217(3) 0.37702(15) 0.46971(18) 0.0290 1.0000 Uani N10 0.1569(3) 0.23782(16) 0.4535(2) 0.0312 1.0000 Uani C2 0.3650(3) 0.31478(17) 0.4666(2) 0.0263 1.0000 Uani C4 0.4407(4) 0.3992(2) 0.5553(2) 0.0359 1.0000 Uani C5 0.3951(4) 0.35052(19) 0.6066(2) 0.0334 1.0000 Uani C6 0.2925(3) 0.23772(18) 0.5792(2) 0.0310 1.0000 Uani C7 0.2075(3) 0.20459(19) 0.5321(2) 0.0309 1.0000 Uani C8 0.1696(4) 0.1302(2) 0.5512(2) 0.0386 1.0000 Uani C9A 0.2203(5) 0.1070(2) 0.6394(3) 0.0561 1.0000 Uani C9B 0.0323(5) 0.1222(3) 0.5483(4) 0.0645 1.0000 Uani C9C 0.2177(6) 0.0834(2) 0.4809(3) 0.0645 1.0000 Uani C11 0.0799(4) 0.3017(2) 0.4664(3) 0.0389 1.0000 Uani C12 0.0177(4) 0.3199(3) 0.3793(3) 0.0542 1.0000 Uani C13 -0.0094(4) 0.2920(3) 0.5352(3) 0.0551 1.0000 Uani C14 0.4589(3) 0.41692(18) 0.3964(2) 0.0305 1.0000 Uani C15 0.5779(4) 0.4133(2) 0.3760(3) 0.0376 1.0000 Uani C16 0.6117(4) 0.4528(2) 0.3057(3) 0.0444 1.0000 Uani C17 0.5313(4) 0.4937(2) 0.2572(3) 0.0463 1.0000 Uani C18 0.4143(4) 0.4963(2) 0.2803(3) 0.0432 1.0000 Uani C19 0.3756(4) 0.45842(19) 0.3510(2) 0.0354 1.0000 Uani C20 0.6666(4) 0.3679(3) 0.4267(3) 0.0522 1.0000 Uani C21 0.5707(6) 0.5356(3) 0.1808(3) 0.0650 1.0000 Uani C22 0.2486(4) 0.4635(2) 0.3753(3) 0.0494 1.0000 Uani C23 0.9303(9) 0.5458(4) 0.3101(6) 0.1103 1.0000 Uani Cl3 0.9240(2) 0.51756(11) 0.41303(15) 0.1090 1.0000 Uani Cl4 0.94306(17) 0.48159(11) 0.23391(11) 0.0882 1.0000 Uani C24 0.2526(17) 0.6882(6) 0.2229(6) 0.1224 0.520(6) Uani Cl5 0.2647(4) 0.66611(19) 0.3288(2) 0.0933 0.520(6) Uani Cl6 0.1752(4) 0.6308(2) 0.1571(3) 0.1048 0.520(6) Uani C25 0.3970(9) 0.8389(16) 0.3964(5) 0.0885 0.438(5) Uani Cl7 0.2514(3) 0.8604(3) 0.3764(3) 0.0978 0.438(5) Uani Cl8 0.4431(4) 0.8298(3) 0.5029(2) 0.0965 0.438(5) Uani C26 0.325(6) 0.773(3) 0.400(2) 0.107(7) 0.112(7) Uiso Cl9 0.2435(18) 0.760(1) 0.3051(14) 0.107(7) 0.112(7) Uiso Cl10 0.417(2) 0.8426(16) 0.4022(15) 0.107(7) 0.112(7) Uiso H1 0.113(7) 0.212(4) 0.423(5) 0.11(3) 1.0000 Uiso H41 0.4809 0.4434 0.5752 0.0431 1.0000 Uiso H51 0.3961 0.3509 0.6715 0.0401 1.0000 Uiso H61 0.3196 0.2180 0.6370 0.0375 1.0000 Uiso H9A1 0.1943 0.0582 0.6505 0.0670 1.0000 Uiso H9A2 0.1907 0.1384 0.6851 0.0670 1.0000 Uiso H9A3 0.3094 0.1090 0.6410 0.0670 1.0000 Uiso H9B1 0.0114 0.0728 0.5612 0.0774 1.0000 Uiso H9B2 -0.0010 0.1535 0.5927 0.0774 1.0000 Uiso H9B3 -0.0022 0.1351 0.4892 0.0774 1.0000 Uiso H9C1 0.1944 0.0340 0.4916 0.0784 1.0000 Uiso H9C2 0.3067 0.0870 0.4827 0.0784 1.0000 Uiso H9C3 0.1835 0.0985 0.4225 0.0784 1.0000 Uiso H111 0.1327 0.3406 0.4884 0.0470 1.0000 Uiso H121 -0.0338 0.3618 0.3859 0.0648 1.0000 Uiso H122 0.0788 0.3300 0.3364 0.0648 1.0000 Uiso H123 -0.0330 0.2798 0.3582 0.0648 1.0000 Uiso H131 -0.0569 0.3357 0.5405 0.0670 1.0000 Uiso H132 0.0340 0.2814 0.5922 0.0670 1.0000 Uiso H133 -0.0642 0.2526 0.5184 0.0670 1.0000 Uiso H161 0.6968 0.4515 0.2899 0.0537 1.0000 Uiso H181 0.3557 0.5260 0.2456 0.0513 1.0000 Uiso H201 0.7466 0.3724 0.4021 0.0627 1.0000 Uiso H202 0.6721 0.3828 0.4889 0.0627 1.0000 Uiso H203 0.6398 0.3183 0.4227 0.0627 1.0000 Uiso H211 0.6575 0.5274 0.1737 0.0785 1.0000 Uiso H212 0.5569 0.5862 0.1915 0.0785 1.0000 Uiso H213 0.5236 0.5209 0.1267 0.0785 1.0000 Uiso H221 0.2038 0.4960 0.3346 0.0593 1.0000 Uiso H222 0.2465 0.4814 0.4361 0.0593 1.0000 Uiso H223 0.2108 0.4163 0.3715 0.0593 1.0000 Uiso H231 1.0010 0.5773 0.3076 0.1312 1.0000 Uiso H232 0.8557 0.5727 0.2946 0.1312 1.0000 Uiso H241 0.2116 0.7343 0.2177 0.1443 0.5201 Uiso H242 0.3350 0.6923 0.2020 0.1443 0.5201 Uiso H251 0.4466 0.8761 0.3711 0.1066 0.4383 Uiso H252 0.4112 0.7937 0.3666 0.1066 0.4383 Uiso H261 0.2683 0.7784 0.4467 0.1283 0.1125 Uiso H262 0.3751 0.7303 0.4116 0.1283 0.1125 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 0.03196(14) 0.02720(13) 0.01711(12) -0.00077(9) 0.00372(8) -0.00296(11) Cl1 0.0591(6) 0.0523(6) 0.0242(4) -0.0073(4) 0.0039(4) -0.0207(5) Cl2 0.0367(4) 0.0436(5) 0.0212(4) -0.0056(3) 0.0105(3) -0.0053(4) N1 0.0365(16) 0.0317(14) 0.0194(13) 0.0003(11) 0.0047(12) -0.0040(12) N3 0.0335(15) 0.0316(14) 0.0220(13) -0.0002(11) 0.0033(12) -0.0055(12) N10 0.0344(16) 0.0327(15) 0.0269(14) 0.0013(12) 0.0040(12) -0.0031(13) C2 0.0287(16) 0.0288(16) 0.0218(15) -0.0021(12) 0.0061(13) -0.0008(13) C4 0.044(2) 0.0391(19) 0.0247(17) -0.0045(14) 0.0024(15) -0.0091(16) C5 0.044(2) 0.0339(18) 0.0223(16) -0.0043(13) 0.0033(15) -0.0079(15) C6 0.0398(19) 0.0321(17) 0.0219(15) 0.0027(13) 0.0085(13) -0.0023(14) C7 0.040(2) 0.0334(17) 0.0204(15) 0.0014(13) 0.0098(14) -0.0021(14) C8 0.049(2) 0.0329(18) 0.0342(19) 0.0055(15) 0.0079(17) -0.0076(16) C9A 0.081(4) 0.045(2) 0.042(2) 0.0126(19) -0.001(2) -0.017(2) C9B 0.063(3) 0.055(3) 0.076(4) 0.015(3) 0.004(3) -0.023(2) C9C 0.106(5) 0.034(2) 0.056(3) -0.0041(19) 0.027(3) -0.010(2) C11 0.036(2) 0.038(2) 0.044(2) -0.0002(16) 0.0089(17) 0.0023(15) C12 0.043(2) 0.057(3) 0.062(3) 0.011(2) -0.000(2) 0.008(2) C13 0.043(2) 0.061(3) 0.063(3) -0.002(2) 0.021(2) 0.007(2) C14 0.0361(19) 0.0330(17) 0.0227(15) -0.0015(13) 0.0041(14) -0.0076(14) C15 0.036(2) 0.042(2) 0.0346(19) -0.0019(15) 0.0070(16) -0.0083(16) C16 0.043(2) 0.055(2) 0.036(2) -0.0016(18) 0.0117(18) -0.0150(19) C17 0.066(3) 0.044(2) 0.0295(19) -0.0041(16) 0.013(2) -0.024(2) C18 0.061(3) 0.037(2) 0.0304(19) 0.0020(15) -0.0067(18) -0.0107(18) C19 0.042(2) 0.0333(18) 0.0309(18) -0.0006(14) 0.0004(16) -0.0086(15) C20 0.038(2) 0.060(3) 0.059(3) 0.006(2) 0.004(2) 0.002(2) C21 0.089(4) 0.066(3) 0.040(2) 0.009(2) 0.014(3) -0.027(3) C22 0.043(2) 0.045(2) 0.060(3) 0.010(2) 0.002(2) 0.0011(19) C23 0.137(7) 0.060(4) 0.131(7) 0.005(4) -0.015(6) 0.027(4) Cl3 0.1355(18) 0.0909(13) 0.1053(15) -0.0292(11) 0.0460(13) -0.0152(12) Cl4 0.0875(11) 0.1067(13) 0.072(1) 0.0045(9) 0.0156(8) 0.024(1) C24 0.139(14) 0.111(11) 0.110(5) 0.051(8) -0.05(1) -0.05(1) Cl5 0.115(3) 0.088(2) 0.080(2) -0.0056(17) 0.0191(19) 0.0057(19) Cl6 0.084(3) 0.135(4) 0.092(3) 0.005(2) -0.0254(19) -0.001(2) C25 0.050(5) 0.151(18) 0.066(4) 0.012(9) 0.011(6) 0.011(9) Cl7 0.053(2) 0.123(4) 0.119(4) 0.050(3) 0.0180(19) 0.015(2) Cl8 0.082(3) 0.147(4) 0.060(2) -0.017(2) 0.0064(18) 0.017(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 . Cl1 . 2.3506(9) yes Pd1 . Cl2 . 2.3089(8) yes Pd1 . N10 . 2.083(3) yes Pd1 . C2 . 1.966(3) yes N1 . C2 . 1.366(4) yes N1 . C5 . 1.388(4) yes N1 . C6 . 1.414(4) yes N3 . C2 . 1.355(4) yes N3 . C4 . 1.392(4) yes N3 . C14 . 1.448(4) yes N10 . C7 . 1.455(5) yes N10 . C11 . 1.521(5) yes N10 . H1 . 0.81(8) yes C4 . C5 . 1.346(5) yes C4 . H41 . 1.000 no C5 . H51 . 1.000 no C6 . C7 . 1.326(5) yes C6 . H61 . 1.000 no C7 . C8 . 1.526(5) yes C8 . C9A . 1.509(6) yes C8 . C9B . 1.546(7) yes C8 . C9C . 1.532(6) yes C9A . H9A1 . 1.000 no C9A . H9A2 . 1.000 no C9A . H9A3 . 1.000 no C9B . H9B1 . 1.000 no C9B . H9B2 . 1.000 no C9B . H9B3 . 1.000 no C9C . H9C1 . 1.000 no C9C . H9C2 . 1.000 no C9C . H9C3 . 1.000 no C11 . C12 . 1.517(6) yes C11 . C13 . 1.513(6) yes C11 . H111 . 1.000 no C12 . H121 . 1.000 no C12 . H122 . 1.000 no C12 . H123 . 1.000 no C13 . H131 . 1.000 no C13 . H132 . 1.000 no C13 . H133 . 1.000 no C14 . C15 . 1.392(5) yes C14 . C19 . 1.386(5) yes C15 . C16 . 1.394(6) yes C15 . C20 . 1.506(6) yes C16 . C17 . 1.383(7) yes C16 . H161 . 1.000 no C17 . C18 . 1.382(7) yes C17 . C21 . 1.515(6) yes C18 . C19 . 1.402(5) yes C18 . H181 . 1.000 no C19 . C22 . 1.498(6) yes C20 . H201 . 1.000 no C20 . H202 . 1.000 no C20 . H203 . 1.000 no C21 . H211 . 1.000 no C21 . H212 . 1.000 no C21 . H213 . 1.000 no C22 . H221 . 1.000 no C22 . H222 . 1.000 no C22 . H223 . 1.000 no C23 . Cl3 . 1.68(1) yes C23 . Cl4 . 1.716(9) yes C23 . H231 . 1.00 no C23 . H232 . 1.000 no C24 . Cl5 . 1.685(8) yes C24 . Cl6 . 1.700(8) yes C24 . Cl9 . 1.87(3) yes C24 . H241 . 1.000 no C24 . H242 . 1.000 no Cl5 . Cl9 . 1.85(2) yes C25 . Cl7 . 1.696(8) yes C25 . Cl8 . 1.700(8) yes C25 . C26 . 1.51(5) yes C25 . Cl10 . 0.25(3) yes C25 . H251 . 1.00 no C25 . H252 . 1.00 no Cl7 . C26 . 1.90(7) yes Cl7 . Cl9 . 2.23(2) yes Cl7 . Cl10 . 1.91(2) yes Cl8 . Cl10 . 1.58(2) yes C26 . Cl9 . 1.69(1) yes C26 . Cl10 . 1.69(1) yes C26 . H252 . 1.19 no C26 . H261 . 1.00 no C26 . H262 . 1.00 no Cl9 . H241 . 1.46 no Cl10 . H251 . 0.88 no Cl10 . H252 . 1.09 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 . Cl2 . 93.44(3) yes Cl1 . Pd1 . N10 . 87.27(9) yes Cl2 . Pd1 . N10 . 174.03(9) yes Cl1 . Pd1 . C2 . 172.7(1) yes Cl2 . Pd1 . C2 . 93.6(1) yes N10 . Pd1 . C2 . 85.93(13) yes C2 . N1 . C5 . 111.2(3) yes C2 . N1 . C6 . 124.2(3) yes C5 . N1 . C6 . 124.5(3) yes C2 . N3 . C4 . 110.5(3) yes C2 . N3 . C14 . 126.6(3) yes C4 . N3 . C14 . 122.9(3) yes Pd1 . N10 . C7 . 108.3(2) yes Pd1 . N10 . C11 . 112.8(2) yes C7 . N10 . C11 . 116.2(3) yes Pd1 . N10 . H1 . 101.8(57) yes C7 . N10 . H1 . 113.7(58) yes C11 . N10 . H1 . 103.3(58) yes Pd1 . C2 . N1 . 120.9(2) yes Pd1 . C2 . N3 . 134.0(2) yes N1 . C2 . N3 . 104.6(3) yes N3 . C4 . C5 . 107.6(3) yes N3 . C4 . H41 . 126.2 no C5 . C4 . H41 . 126.2 no N1 . C5 . C4 . 106.1(3) yes N1 . C5 . H51 . 126.9 no C4 . C5 . H51 . 126.9 no N1 . C6 . C7 . 123.0(3) yes N1 . C6 . H61 . 118.5 no C7 . C6 . H61 . 118.5 no N10 . C7 . C6 . 118.5(3) yes N10 . C7 . C8 . 118.3(3) yes C6 . C7 . C8 . 122.9(3) yes C7 . C8 . C9A . 110.9(3) yes C7 . C8 . C9B . 112.1(4) yes C9A . C8 . C9B . 108.6(4) yes C7 . C8 . C9C . 107.4(3) yes C9A . C8 . C9C . 109.5(4) yes C9B . C8 . C9C . 108.3(4) yes C8 . C9A . H9A1 . 109.5 no C8 . C9A . H9A2 . 109.5 no H9A1 . C9A . H9A2 . 109.5 no C8 . C9A . H9A3 . 109.5 no H9A1 . C9A . H9A3 . 109.5 no H9A2 . C9A . H9A3 . 109.5 no C8 . C9B . H9B1 . 109.5 no C8 . C9B . H9B2 . 109.5 no H9B1 . C9B . H9B2 . 109.5 no C8 . C9B . H9B3 . 109.5 no H9B1 . C9B . H9B3 . 109.5 no H9B2 . C9B . H9B3 . 109.5 no C8 . C9C . H9C1 . 109.5 no C8 . C9C . H9C2 . 109.5 no H9C1 . C9C . H9C2 . 109.5 no C8 . C9C . H9C3 . 109.5 no H9C1 . C9C . H9C3 . 109.5 no H9C2 . C9C . H9C3 . 109.5 no N10 . C11 . C12 . 107.7(3) yes N10 . C11 . C13 . 113.5(3) yes C12 . C11 . C13 . 111.1(4) yes N10 . C11 . H111 . 108.5 no C12 . C11 . H111 . 111.0 no C13 . C11 . H111 . 105.0 no C11 . C12 . H121 . 109.5 no C11 . C12 . H122 . 109.5 no H121 . C12 . H122 . 109.5 no C11 . C12 . H123 . 109.5 no H121 . C12 . H123 . 109.5 no H122 . C12 . H123 . 109.5 no C11 . C13 . H131 . 109.5 no C11 . C13 . H132 . 109.5 no H131 . C13 . H132 . 109.5 no C11 . C13 . H133 . 109.5 no H131 . C13 . H133 . 109.5 no H132 . C13 . H133 . 109.5 no N3 . C14 . C15 . 118.3(3) yes N3 . C14 . C19 . 118.8(3) yes C15 . C14 . C19 . 122.9(3) yes C14 . C15 . C16 . 117.2(4) yes C14 . C15 . C20 . 121.7(4) yes C16 . C15 . C20 . 121.1(4) yes C15 . C16 . C17 . 122.1(4) yes C15 . C16 . H161 . 119.0 no C17 . C16 . H161 . 119.0 no C16 . C17 . C18 . 118.7(4) yes C16 . C17 . C21 . 120.8(5) yes C18 . C17 . C21 . 120.4(5) yes C17 . C18 . C19 . 121.6(4) yes C17 . C18 . H181 . 119.2 no C19 . C18 . H181 . 119.2 no C14 . C19 . C18 . 117.4(4) yes C14 . C19 . C22 . 122.3(3) yes C18 . C19 . C22 . 120.3(4) yes C15 . C20 . H201 . 109.5 no C15 . C20 . H202 . 109.5 no H201 . C20 . H202 . 109.5 no C15 . C20 . H203 . 109.5 no H201 . C20 . H203 . 109.5 no H202 . C20 . H203 . 109.5 no C17 . C21 . H211 . 109.5 no C17 . C21 . H212 . 109.5 no H211 . C21 . H212 . 109.5 no C17 . C21 . H213 . 109.5 no H211 . C21 . H213 . 109.5 no H212 . C21 . H213 . 109.5 no C19 . C22 . H221 . 109.5 no C19 . C22 . H222 . 109.5 no H221 . C22 . H222 . 109.5 no C19 . C22 . H223 . 109.5 no H221 . C22 . H223 . 109.5 no H222 . C22 . H223 . 109.5 no Cl3 . C23 . Cl4 . 115.0(4) yes Cl3 . C23 . H231 . 108.1 no Cl4 . C23 . H231 . 108.1 no Cl3 . C23 . H232 . 108.1 no Cl4 . C23 . H232 . 108.1 no H231 . C23 . H232 . 109.5 no Cl5 . C24 . Cl6 . 115.1(4) yes Cl5 . C24 . Cl9 . 62.2(8) yes Cl6 . C24 . Cl9 . 146.1(14) yes Cl5 . C24 . H241 . 108.1 no Cl6 . C24 . H241 . 108.1 no Cl9 . C24 . H241 . 50.3 no Cl5 . C24 . H242 . 108.1 no Cl6 . C24 . H242 . 108.1 no Cl9 . C24 . H242 . 104.3 no H241 . C24 . H242 . 109.5 no C24 . Cl5 . Cl9 . 64.0(9) yes Cl7 . C25 . Cl8 . 115.8(4) yes Cl7 . C25 . C26 . 72.5(29) yes Cl8 . C25 . C26 . 90.8(12) yes Cl7 . C25 . Cl10 . 147.0(123) yes Cl8 . C25 . Cl10 . 57.7(78) yes C26 . C25 . Cl10 . 135.3(128) yes Cl7 . C25 . H251 . 107.9 no Cl8 . C25 . H251 . 107.9 no C26 . C25 . H251 . 157.9 no Cl10 . C25 . H251 . 54.4(106) no Cl7 . C25 . H252 . 107.9 no Cl8 . C25 . H252 . 107.9 no C26 . C25 . H252 . 51.9 no Cl10 . C25 . H252 . 104.6(103) no H251 . C25 . H252 . 109.5 no C25 . Cl7 . C26 . 49.2(19) yes C25 . Cl7 . Cl9 . 83.5(12) yes C26 . Cl7 . Cl9 . 47.6(7) yes C25 . Cl7 . Cl10 . 4.0(17) yes C26 . Cl7 . Cl10 . 52.8(11) yes Cl9 . Cl7 . Cl10 . 87.5(8) yes C25 . Cl8 . Cl10 . 7.5(13) yes C25 . C26 . Cl7 . 58.2(20) yes C25 . C26 . Cl9 . 111.1(11) yes Cl7 . C26 . Cl9 . 76.3(20) yes C25 . C26 . Cl10 . 5.8(11) yes Cl7 . C26 . Cl10 . 63.7(17) yes Cl9 . C26 . Cl10 . 115.7(5) yes C25 . C26 . H252 . 41.4 no Cl7 . C26 . H252 . 88.4 no Cl9 . C26 . H252 . 95.3 no Cl10 . C26 . H252 . 39.7 no C25 . C26 . H261 . 107.1 no Cl7 . C26 . H261 . 75.5 no Cl9 . C26 . H261 . 107.9 no Cl10 . C26 . H261 . 107.9 no H252 . C26 . H261 . 147.3 no C25 . C26 . H262 . 113.3 no Cl7 . C26 . H262 . 171.5 no Cl9 . C26 . H262 . 107.9 no Cl10 . C26 . H262 . 107.9 no H252 . C26 . H262 . 83.8 no H261 . C26 . H262 . 109.4 no C24 . Cl9 . Cl5 . 53.9(6) yes C24 . Cl9 . Cl7 . 165.6(12) yes Cl5 . Cl9 . Cl7 . 138.4(11) yes C24 . Cl9 . C26 . 130.0(30) yes Cl5 . Cl9 . C26 . 85.2(20) yes Cl7 . Cl9 . C26 . 56.1(23) yes C24 . Cl9 . H241 . 31.9 no Cl5 . Cl9 . H241 . 83.1 no Cl7 . Cl9 . H241 . 138.4 no C26 . Cl9 . H241 . 159.5 no C25 . Cl10 . Cl7 . 29.0(107) yes C25 . Cl10 . Cl8 . 114.8(88) yes Cl7 . Cl10 . Cl8 . 110.7(14) yes C25 . Cl10 . C26 . 38.9(119) yes Cl7 . Cl10 . C26 . 63.5(26) yes Cl8 . Cl10 . C26 . 88.7(16) yes C25 . Cl10 . H251 . 112.5(111) no Cl7 . Cl10 . H251 . 98.7 no Cl8 . Cl10 . H251 . 126.4 no C26 . Cl10 . H251 . 144.9 no C25 . Cl10 . H252 . 62.8(102) no Cl7 . Cl10 . H252 . 91.4 no Cl8 . Cl10 . H252 . 111.2 no C26 . Cl10 . H252 . 44.4 no H251 . Cl10 . H252 . 111.7 no C24 . H241 . Cl9 . 97.8 no C25 . H251 . Cl10 . 13.1 no C25 . H252 . C26 . 86.7 no C25 . H252 . Cl10 . 12.6 no C26 . H252 . Cl10 . 95.9 no