data_publication_text _publ_contact_author_name 'Rosenani A. Haque' _publ_contact_author_address ;School of Chemical Sciences Universiti Sains Malaysia 11800 USM Penang Malaysia ; _publ_contact_author_email rosenani@usm.my _publ_contact_author_phone +604-6533578 loop_ _publ_author_name _publ_author_address 'Salman, Abbas Washeel' ;School of Chemical Sciences Universiti Sains Malaysia 11800 USM Penang Malaysia ; 'A. Haque, Rosenani' ;School of Chemical Sciences Universiti Sains Malaysia 11800 USM Penang Malaysia ; data_mo_ka1pdb_0m _audit_creation_method SHELXL-97 _chemical_name_systematic ; Dichlorobis(3-benzyl-1-methylimdazolium)palladium(II) ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C45 H50 Cl6 N8 Pd2' _chemical_formula_weight 1128.43 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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pd' 'Pd' -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'monoclinic' _symmetry_space_group_name_H-M 'P2(1)/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 15.3386(14) _cell_length_b 9.6356(8) _cell_length_c 34.681(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.256(2) _cell_angle_gamma 90.00 _cell_volume 5125.7(8) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.51 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.462 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2280 _exptl_absorpt_coefficient_mu 1.053 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.6147 _exptl_absorpt_correction_T_max 0.9385 _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 117035 _diffrn_reflns_av_R_equivalents 0.0586 _diffrn_reflns_av_sigmaI/netI 0.0422 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -51 _diffrn_reflns_limit_l_max 51 _diffrn_reflns_theta_min 1.77 _diffrn_reflns_theta_max 32.14 _reflns_number_total 17720 _reflns_number_gt 12507 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _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^)+(0.1866P)^2^+5.0143P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 17720 _refine_ls_number_parameters 577 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1082 _refine_ls_R_factor_gt 0.0733 _refine_ls_wR_factor_ref 0.2907 _refine_ls_wR_factor_gt 0.2431 _refine_ls_goodness_of_fit_ref 1.087 _refine_ls_restrained_S_all 1.087 _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 Pd1A Pd 0.445923(19) 0.36192(4) 0.389942(8) 0.03186(11) Uani 1 1 d . . . Cl1A Cl 0.32007(7) 0.37636(15) 0.35089(4) 0.0455(3) Uani 1 1 d . . . Cl2A Cl 0.42231(10) 0.58947(16) 0.41512(4) 0.0522(3) Uani 1 1 d . . . N1A N 0.4903(2) 0.1407(4) 0.33204(11) 0.0365(8) Uani 1 1 d . . . N2A N 0.4489(3) 0.0471(6) 0.38490(12) 0.0470(10) Uani 1 1 d . . . N3A N 0.6355(3) 0.3667(5) 0.41365(12) 0.0438(9) Uani 1 1 d . . . N4A N 0.5522(3) 0.3355(6) 0.46223(12) 0.0545(12) Uani 1 1 d . . . C1A C 0.5336(4) 0.1488(7) 0.23618(16) 0.0534(13) Uani 1 1 d . . . H1AA H 0.5891 0.1179 0.2427 0.064 Uiso 1 1 calc R . . C2A C 0.5010(6) 0.1290(8) 0.19812(18) 0.073(2) Uani 1 1 d . . . H2AA H 0.5351 0.0874 0.1792 0.088 Uiso 1 1 calc R . . C3A C 0.4156(6) 0.1742(8) 0.18990(19) 0.075(2) Uani 1 1 d . . . H3AA H 0.3934 0.1636 0.1651 0.090 Uiso 1 1 calc R . . C4A C 0.3656(5) 0.2321(8) 0.2170(2) 0.0676(19) Uani 1 1 d . . . H4AA H 0.3083 0.2562 0.2112 0.081 Uiso 1 1 calc R . . C5A C 0.3990(4) 0.2563(7) 0.25349(15) 0.0517(13) Uani 1 1 d . . . H5AA H 0.3651 0.3017 0.2717 0.062 Uiso 1 1 calc R . . C6A C 0.4829(3) 0.2133(5) 0.26309(12) 0.0373(9) Uani 1 1 d . . . C7A C 0.5191(3) 0.2420(6) 0.30267(13) 0.0460(11) Uani 1 1 d . . . H7AA H 0.5823 0.2410 0.3015 0.055 Uiso 1 1 calc R . . H7AB H 0.5013 0.3343 0.3106 0.055 Uiso 1 1 calc R . . C8A C 0.4645(3) 0.1733(5) 0.36797(12) 0.0336(8) Uani 1 1 d . . . C9A C 0.4911(4) 0.0005(6) 0.32642(15) 0.0476(11) Uani 1 1 d . . . H9AA H 0.5061 -0.0455 0.3038 0.057 Uiso 1 1 calc R . . C10A C 0.4661(4) -0.0585(6) 0.35972(16) 0.0528(13) Uani 1 1 d . . . H10A H 0.4614 -0.1530 0.3647 0.063 Uiso 1 1 calc R . . C11A C 0.4119(6) 0.0299(9) 0.4232(2) 0.079(2) Uani 1 1 d . . . H11A H 0.4074 -0.0672 0.4291 0.119 Uiso 1 1 calc R . . H11B H 0.3550 0.0713 0.4239 0.119 Uiso 1 1 calc R . . H11C H 0.4489 0.0743 0.4419 0.119 Uiso 1 1 calc R . . C12A C 0.7556(4) 0.2865(8) 0.32222(19) 0.0591(15) Uani 1 1 d . . . H12A H 0.7667 0.3764 0.3138 0.071 Uiso 1 1 calc R . . C13A C 0.7876(5) 0.1762(10) 0.3016(3) 0.080(2) Uani 1 1 d . . . H13A H 0.8198 0.1905 0.2793 0.096 Uiso 1 1 calc R . . C14A C 0.7707(5) 0.0432(9) 0.3147(2) 0.077(2) Uani 1 1 d . . . H14A H 0.7924 -0.0319 0.3009 0.092 Uiso 1 1 calc R . . C15A C 0.7236(4) 0.0190(8) 0.3470(2) 0.0720(19) Uani 1 1 d . . . H15A H 0.7126 -0.0712 0.3551 0.086 Uiso 1 1 calc R . . C16A C 0.6917(4) 0.1328(7) 0.36779(18) 0.0560(14) Uani 1 1 d . . . H16A H 0.6600 0.1178 0.3902 0.067 Uiso 1 1 calc R . . C17A C 0.7069(3) 0.2664(6) 0.35546(16) 0.0431(10) Uani 1 1 d . . . C18A C 0.6671(3) 0.3912(6) 0.37469(15) 0.0468(11) Uani 1 1 d . . . H18A H 0.7104 0.4646 0.3756 0.056 Uiso 1 1 calc R . . H18B H 0.6189 0.4239 0.3589 0.056 Uiso 1 1 calc R . . C19A C 0.5517(3) 0.3484(6) 0.42361(12) 0.0390(10) Uani 1 1 d . . . C20A C 0.6891(4) 0.3667(8) 0.44592(18) 0.0640(18) Uani 1 1 d . . . H20A H 0.7494 0.3762 0.4464 0.077 Uiso 1 1 calc R . . C21A C 0.6368(5) 0.3503(9) 0.47607(18) 0.070(2) Uani 1 1 d . . . H21A H 0.6538 0.3490 0.5018 0.083 Uiso 1 1 calc R . . C22A C 0.4766(4) 0.3165(9) 0.48630(16) 0.0648(18) Uani 1 1 d . . . H22A H 0.4255 0.3084 0.4704 0.097 Uiso 1 1 calc R . . H22B H 0.4705 0.3947 0.5032 0.097 Uiso 1 1 calc R . . H22C H 0.4834 0.2335 0.5013 0.097 Uiso 1 1 calc R . . Pd1B Pd 0.04568(2) 0.18050(5) 0.109170(9) 0.03920(12) Uani 1 1 d . . . Cl1B Cl 0.17380(8) 0.16329(18) 0.14660(4) 0.0534(3) Uani 1 1 d . . . Cl2B Cl 0.06350(14) -0.0460(2) 0.08270(5) 0.0744(5) Uani 1 1 d . . . N1B N -0.1461(3) 0.1987(7) 0.08797(13) 0.0577(13) Uani 1 1 d . . . N2B N -0.0645(4) 0.2282(8) 0.03862(14) 0.0738(19) Uani 1 1 d . . . N3B N 0.0043(3) 0.3993(5) 0.16834(11) 0.0408(8) Uani 1 1 d . . . N4B N 0.0426(3) 0.4956(6) 0.11538(13) 0.0540(12) Uani 1 1 d . . . C1B C -0.2560(4) 0.2481(9) 0.18380(19) 0.0624(16) Uani 1 1 d . . . H1BA H -0.2656 0.1561 0.1908 0.075 Uiso 1 1 calc R . . C2B C -0.2836(5) 0.3566(10) 0.2071(2) 0.079(2) Uani 1 1 d . . . H2BA H -0.3109 0.3365 0.2303 0.095 Uiso 1 1 calc R . . C3B C -0.2713(5) 0.4980(11) 0.1964(3) 0.093(3) Uani 1 1 d . . . H3BA H -0.2910 0.5692 0.2121 0.112 Uiso 1 1 calc R . . C4B C -0.2312(5) 0.5262(8) 0.1635(3) 0.079(2) Uani 1 1 d . . . H4BA H -0.2223 0.6182 0.1564 0.094 Uiso 1 1 calc R . . C5B C -0.2016(4) 0.4179(8) 0.1390(2) 0.0626(16) Uani 1 1 d . . . H5BA H -0.1743 0.4393 0.1159 0.075 Uiso 1 1 calc R . . C6B C -0.2132(3) 0.2820(6) 0.14950(16) 0.0468(11) Uani 1 1 d . . . C7B C -0.1762(4) 0.1610(7) 0.12641(16) 0.0536(13) Uani 1 1 d . . . H7BA H -0.1277 0.1211 0.1407 0.064 Uiso 1 1 calc R . . H7BB H -0.2207 0.0901 0.1240 0.064 Uiso 1 1 calc R . . C8B C -0.0624(4) 0.2042(8) 0.07710(14) 0.0530(14) Uani 1 1 d . . . C9B C -0.2016(5) 0.2242(12) 0.0574(2) 0.087(3) Uani 1 1 d . . . H9BA H -0.2621 0.2288 0.0580 0.104 Uiso 1 1 calc R . . C10B C -0.1506(5) 0.2412(13) 0.0265(2) 0.101(4) Uani 1 1 d . . . H10B H -0.1694 0.2585 0.0015 0.121 Uiso 1 1 calc R . . C11B C 0.0110(5) 0.2274(12) 0.01342(18) 0.090(3) Uani 1 1 d . . . H11D H 0.0630 0.2152 0.0286 0.135 Uiso 1 1 calc R . . H11E H 0.0142 0.3139 -0.0002 0.135 Uiso 1 1 calc R . . H11F H 0.0058 0.1525 -0.0047 0.135 Uiso 1 1 calc R . . C12B C 0.1021(3) 0.2914(7) 0.24542(16) 0.0506(12) Uani 1 1 d . . . H12B H 0.1363 0.2475 0.2270 0.061 Uiso 1 1 calc R . . C13B C 0.1369(5) 0.3215(9) 0.2813(2) 0.0675(18) Uani 1 1 d . . . H13B H 0.1956 0.3050 0.2863 0.081 Uiso 1 1 calc R . . C14B C 0.0849(6) 0.3755(8) 0.3092(2) 0.074(2) Uani 1 1 d . . . H14B H 0.1076 0.3900 0.3338 0.089 Uiso 1 1 calc R . . C15B C -0.0016(6) 0.4091(8) 0.30151(18) 0.072(2) Uani 1 1 d . . . H15B H -0.0366 0.4464 0.3207 0.087 Uiso 1 1 calc R . . C16B C -0.0353(4) 0.3864(7) 0.26457(16) 0.0520(13) Uani 1 1 d . . . H16B H -0.0924 0.4118 0.2588 0.062 Uiso 1 1 calc R . . C17B C 0.0161(3) 0.3262(6) 0.23664(13) 0.0393(9) Uani 1 1 d . . . C18B C -0.0204(4) 0.2935(6) 0.19732(14) 0.0461(11) Uani 1 1 d . . . H18C H 0.0008 0.2034 0.1891 0.055 Uiso 1 1 calc R . . H18D H -0.0835 0.2884 0.1988 0.055 Uiso 1 1 calc R . . C19B C 0.0291(3) 0.3682(5) 0.13208(13) 0.0382(9) Uani 1 1 d . . . C20B C 0.0009(4) 0.5400(6) 0.17381(16) 0.0486(11) Uani 1 1 d . . . H20B H -0.0148 0.5853 0.1964 0.058 Uiso 1 1 calc R . . C21B C 0.0242(4) 0.5996(7) 0.14099(17) 0.0551(13) Uani 1 1 d . . . H21B H 0.0274 0.6944 0.1362 0.066 Uiso 1 1 calc R . . C22B C 0.0757(6) 0.5146(11) 0.0766(2) 0.085(3) Uani 1 1 d . . . H22D H 0.0804 0.6120 0.0711 0.127 Uiso 1 1 calc R . . H22E H 0.0365 0.4722 0.0584 0.127 Uiso 1 1 calc R . . H22F H 0.1322 0.4723 0.0746 0.127 Uiso 1 1 calc R . . Cl3B Cl 0.2983(4) 0.4626(6) 0.03175(12) 0.1093(19) Uani 0.50 1 d P . . Cl4B Cl 0.37856(19) 0.2437(4) 0.07635(8) 0.0600(7) Uani 0.50 1 d P . . C23B C 0.2781(9) 0.311(2) 0.0597(4) 0.074(4) Uani 0.50 1 d P . . H23A H 0.2413 0.3342 0.0815 0.089 Uiso 0.50 1 calc PR . . H23B H 0.2481 0.2423 0.0442 0.089 Uiso 0.50 1 calc PR . . Cl3A Cl 0.1570(3) 0.1403(6) 0.44116(15) 0.1077(19) Uani 0.50 1 d P . . Cl4A Cl 0.2159(4) 0.3974(6) 0.47281(17) 0.1138(18) Uani 0.50 1 d P . . C23A C 0.1554(16) 0.3172(17) 0.4293(4) 0.136(11) Uani 0.50 1 d P . . H23C H 0.0963 0.3520 0.4272 0.163 Uiso 0.50 1 calc PR . . H23D H 0.1860 0.3350 0.4054 0.163 Uiso 0.50 1 calc PR . . 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 Pd1A 0.03302(17) 0.0337(2) 0.02890(17) -0.00317(11) 0.00129(11) -0.00091(11) Cl1A 0.0362(5) 0.0523(8) 0.0479(6) -0.0098(5) -0.0072(4) 0.0057(4) Cl2A 0.0643(7) 0.0414(7) 0.0508(6) -0.0129(5) -0.0038(5) 0.0051(6) N1A 0.0386(17) 0.035(2) 0.0360(17) -0.0030(14) -0.0023(13) 0.0027(14) N2A 0.061(3) 0.044(3) 0.0367(19) -0.0041(17) 0.0015(17) -0.0066(19) N3A 0.0342(17) 0.057(3) 0.0401(19) -0.0021(18) -0.0034(14) -0.0016(16) N4A 0.050(2) 0.080(4) 0.0339(19) -0.006(2) -0.0047(17) -0.001(2) C1A 0.070(4) 0.049(3) 0.041(3) -0.004(2) 0.014(2) 0.003(3) C2A 0.130(7) 0.046(4) 0.042(3) -0.013(2) 0.015(3) -0.015(4) C3A 0.118(6) 0.064(5) 0.042(3) 0.002(3) -0.023(4) -0.032(4) C4A 0.068(4) 0.067(5) 0.067(4) 0.017(3) -0.025(3) -0.016(3) C5A 0.048(3) 0.063(4) 0.045(3) 0.005(2) 0.002(2) -0.005(2) C6A 0.042(2) 0.037(2) 0.0330(19) -0.0007(16) 0.0028(15) -0.0055(17) C7A 0.045(2) 0.056(3) 0.037(2) -0.004(2) 0.0002(17) -0.012(2) C8A 0.0330(17) 0.037(2) 0.0308(18) 0.0019(15) -0.0017(14) 0.0029(15) C9A 0.058(3) 0.038(3) 0.047(3) -0.010(2) -0.004(2) 0.005(2) C10A 0.072(3) 0.037(3) 0.049(3) 0.000(2) -0.008(2) 0.003(2) C11A 0.127(7) 0.057(5) 0.054(3) 0.009(3) 0.014(4) -0.022(4) C12A 0.047(3) 0.061(4) 0.069(4) -0.002(3) 0.018(2) -0.005(3) C13A 0.060(4) 0.092(7) 0.089(5) -0.026(5) 0.032(4) -0.008(4) C14A 0.068(4) 0.071(5) 0.091(5) -0.027(4) 0.023(4) 0.008(4) C15A 0.060(4) 0.052(4) 0.104(6) 0.003(4) 0.006(3) 0.006(3) C16A 0.062(3) 0.048(4) 0.059(3) 0.005(2) 0.007(3) 0.003(3) C17A 0.0334(19) 0.040(3) 0.056(3) -0.001(2) -0.0004(17) -0.0023(17) C18A 0.041(2) 0.053(3) 0.047(3) 0.002(2) 0.0056(18) -0.003(2) C19A 0.045(2) 0.045(3) 0.0269(18) -0.0041(16) -0.0009(15) 0.0043(19) C20A 0.047(3) 0.089(5) 0.056(3) -0.008(3) -0.020(2) 0.000(3) C21A 0.066(4) 0.099(6) 0.044(3) -0.007(3) -0.020(3) 0.000(4) C22A 0.070(4) 0.091(6) 0.034(2) -0.005(3) 0.001(2) -0.006(3) Pd1B 0.04092(19) 0.0438(3) 0.03295(18) -0.00176(13) 0.00435(13) -0.00475(13) Cl1B 0.0409(6) 0.0564(9) 0.0629(8) -0.0062(6) -0.0036(5) 0.0085(5) Cl2B 0.0974(12) 0.0611(11) 0.0648(9) -0.0210(8) 0.0070(8) -0.0051(9) N1B 0.044(2) 0.086(4) 0.043(2) -0.003(2) -0.0030(17) -0.019(2) N2B 0.057(3) 0.129(6) 0.036(2) 0.002(3) -0.0051(19) -0.026(3) N3B 0.0403(18) 0.043(2) 0.0393(19) 0.0004(16) -0.0024(14) -0.0009(16) N4B 0.055(2) 0.065(4) 0.042(2) 0.003(2) -0.0075(18) 0.006(2) C1B 0.049(3) 0.073(5) 0.066(4) -0.006(3) 0.014(3) -0.011(3) C2B 0.056(4) 0.104(7) 0.078(5) -0.026(4) 0.019(3) -0.005(4) C3B 0.065(4) 0.081(7) 0.134(8) -0.043(6) 0.013(5) -0.003(4) C4B 0.081(5) 0.033(3) 0.122(7) -0.007(4) -0.009(4) 0.012(3) C5B 0.061(3) 0.051(4) 0.075(4) 0.015(3) -0.008(3) -0.001(3) C6B 0.035(2) 0.048(3) 0.057(3) 0.004(2) -0.0033(19) -0.0067(19) C7B 0.052(3) 0.056(4) 0.053(3) 0.002(2) 0.009(2) -0.015(2) C8B 0.056(3) 0.074(4) 0.029(2) -0.003(2) 0.0045(19) -0.012(3) C9B 0.051(3) 0.149(9) 0.060(4) -0.010(5) -0.012(3) -0.025(4) C10B 0.074(5) 0.175(11) 0.054(4) 0.011(5) -0.027(3) -0.032(6) C11B 0.083(5) 0.147(9) 0.040(3) 0.002(4) 0.009(3) -0.030(5) C12B 0.044(2) 0.053(3) 0.055(3) 0.011(2) -0.003(2) -0.003(2) C13B 0.061(3) 0.073(5) 0.068(4) 0.016(3) -0.023(3) -0.011(3) C14B 0.116(6) 0.050(4) 0.056(4) 0.005(3) -0.033(4) -0.025(4) C15B 0.118(6) 0.052(4) 0.046(3) -0.012(3) 0.011(3) -0.006(4) C16B 0.057(3) 0.051(4) 0.048(3) 0.000(2) 0.009(2) 0.002(2) C17B 0.041(2) 0.042(3) 0.035(2) 0.0004(17) 0.0014(16) -0.0055(18) C18B 0.051(3) 0.050(3) 0.037(2) -0.001(2) -0.0018(18) -0.013(2) C19B 0.0374(19) 0.043(3) 0.0340(19) 0.0041(17) -0.0016(15) -0.0004(17) C20B 0.053(3) 0.040(3) 0.053(3) -0.006(2) -0.008(2) 0.004(2) C21B 0.068(3) 0.041(3) 0.056(3) 0.004(2) -0.012(3) 0.004(3) C22B 0.099(6) 0.100(7) 0.055(4) 0.029(4) 0.010(3) -0.013(5) Cl3B 0.152(4) 0.112(4) 0.064(2) 0.019(2) 0.011(2) 0.065(4) Cl4B 0.0550(14) 0.076(2) 0.0485(13) 0.0064(13) 0.0065(11) 0.0114(14) C23B 0.057(7) 0.111(14) 0.054(7) 0.008(7) -0.003(5) 0.005(7) Cl3A 0.091(3) 0.126(5) 0.105(3) -0.070(3) 0.030(2) -0.012(3) Cl4A 0.134(4) 0.069(3) 0.138(4) 0.001(3) 0.002(3) -0.047(3) C23A 0.25(2) 0.071(11) 0.084(10) 0.051(9) 0.132(14) 0.069(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 Pd1A C8A 1.992(5) . ? Pd1A C19A 1.999(5) . ? Pd1A Cl1A 2.3572(11) . ? Pd1A Cl2A 2.3882(14) . ? N1A C8A 1.346(6) . ? N1A C9A 1.365(7) . ? N1A C7A 1.480(7) . ? N2A C10A 1.367(7) . ? N2A C8A 1.372(7) . ? N2A C11A 1.457(8) . ? N3A C19A 1.343(6) . ? N3A C20A 1.386(7) . ? N3A C18A 1.457(6) . ? N4A C19A 1.345(6) . ? N4A C21A 1.388(8) . ? N4A C22A 1.445(8) . ? C1A C6A 1.367(7) . ? C1A C2A 1.422(9) . ? C1A H1AA 0.9300 . ? C2A C3A 1.409(13) . ? C2A H2AA 0.9300 . ? C3A C4A 1.336(12) . ? C3A H3AA 0.9300 . ? C4A C5A 1.384(8) . ? C4A H4AA 0.9300 . ? C5A C6A 1.391(7) . ? C5A H5AA 0.9300 . ? C6A C7A 1.504(6) . ? C7A H7AA 0.9700 . ? C7A H7AB 0.9700 . ? C9A C10A 1.345(8) . ? C9A H9AA 0.9300 . ? C10A H10A 0.9300 . ? C11A H11A 0.9600 . ? C11A H11B 0.9600 . ? C11A H11C 0.9600 . ? C12A C13A 1.373(10) . ? C12A C17A 1.390(8) . ? C12A H12A 0.9300 . ? C13A C14A 1.385(13) . ? C13A H13A 0.9300 . ? C14A C15A 1.355(11) . ? C14A H14A 0.9300 . ? C15A C16A 1.402(10) . ? C15A H15A 0.9300 . ? C16A C17A 1.377(8) . ? C16A H16A 0.9300 . ? C17A C18A 1.505(8) . ? C18A H18A 0.9700 . ? C18A H18B 0.9700 . ? C20A C21A 1.330(10) . ? C20A H20A 0.9300 . ? C21A H21A 0.9300 . ? C22A H22A 0.9600 . ? C22A H22B 0.9600 . ? C22A H22C 0.9600 . ? Pd1B C19B 1.992(5) . ? Pd1B C8B 2.005(6) . ? Pd1B Cl1B 2.3562(14) . ? Pd1B Cl2B 2.3839(19) . ? N1B C8B 1.341(7) . ? N1B C9B 1.380(8) . ? N1B C7B 1.459(7) . ? N2B C8B 1.355(7) . ? N2B C10B 1.389(9) . ? N2B C11B 1.455(9) . ? N3B C19B 1.350(6) . ? N3B C20B 1.369(7) . ? N3B C18B 1.482(7) . ? N4B C21B 1.369(8) . ? N4B C19B 1.374(8) . ? N4B C22B 1.453(8) . ? C1B C2B 1.389(11) . ? C1B C6B 1.400(8) . ? C1B H1BA 0.9300 . ? C2B C3B 1.425(14) . ? C2B H2BA 0.9300 . ? C3B C4B 1.325(13) . ? C3B H3BA 0.9300 . ? C4B C5B 1.421(11) . ? C4B H4BA 0.9300 . ? C5B C6B 1.372(9) . ? C5B H5BA 0.9300 . ? C6B C7B 1.525(9) . ? C7B H7BA 0.9700 . ? C7B H7BB 0.9700 . ? C9B C10B 1.338(11) . ? C9B H9BA 0.9300 . ? C10B H10B 0.9300 . ? C11B H11D 0.9600 . ? C11B H11E 0.9600 . ? C11B H11F 0.9600 . ? C12B C13B 1.382(9) . ? C12B C17B 1.393(7) . ? C12B H12B 0.9300 . ? C13B C14B 1.360(12) . ? C13B H13B 0.9300 . ? C14B C15B 1.392(12) . ? C14B H14B 0.9300 . ? C15B C16B 1.397(9) . ? C15B H15B 0.9300 . ? C16B C17B 1.380(7) . ? C16B H16B 0.9300 . ? C17B C18B 1.505(6) . ? C18B H18C 0.9700 . ? C18B H18D 0.9700 . ? C20B C21B 1.325(8) . ? C20B H20B 0.9300 . ? C21B H21B 0.9300 . ? C22B H22D 0.9600 . ? C22B H22E 0.9600 . ? C22B H22F 0.9600 . ? Cl3B C23B 1.781(18) . ? Cl4B C23B 1.767(14) . ? C23B H23A 0.9700 . ? C23B H23B 0.9700 . ? Cl3A C23A 1.753(16) . ? Cl4A C23A 1.93(3) . ? C23A H23C 0.9700 . ? C23A H23D 0.9700 . ? 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 C8A Pd1A C19A 92.68(19) . . ? C8A Pd1A Cl1A 87.27(12) . . ? C19A Pd1A Cl1A 179.23(15) . . ? C8A Pd1A Cl2A 178.87(12) . . ? C19A Pd1A Cl2A 88.30(15) . . ? Cl1A Pd1A Cl2A 91.76(5) . . ? C8A N1A C9A 111.5(4) . . ? C8A N1A C7A 125.0(4) . . ? C9A N1A C7A 123.5(4) . . ? C10A N2A C8A 110.6(4) . . ? C10A N2A C11A 125.1(6) . . ? C8A N2A C11A 124.1(5) . . ? C19A N3A C20A 110.9(5) . . ? C19A N3A C18A 125.7(4) . . ? C20A N3A C18A 123.3(5) . . ? C19A N4A C21A 109.6(5) . . ? C19A N4A C22A 125.9(5) . . ? C21A N4A C22A 124.4(5) . . ? C6A C1A C2A 119.8(6) . . ? C6A C1A H1AA 120.1 . . ? C2A C1A H1AA 120.1 . . ? C3A C2A C1A 117.9(6) . . ? C3A C2A H2AA 121.0 . . ? C1A C2A H2AA 121.0 . . ? C4A C3A C2A 121.5(6) . . ? C4A C3A H3AA 119.2 . . ? C2A C3A H3AA 119.2 . . ? C3A C4A C5A 120.1(7) . . ? C3A C4A H4AA 119.9 . . ? C5A C4A H4AA 119.9 . . ? C4A C5A C6A 120.5(6) . . ? C4A C5A H5AA 119.8 . . ? C6A C5A H5AA 119.8 . . ? C1A C6A C5A 120.0(5) . . ? C1A C6A C7A 119.9(5) . . ? C5A C6A C7A 120.1(5) . . ? N1A C7A C6A 113.4(4) . . ? N1A C7A H7AA 108.9 . . ? C6A C7A H7AA 108.9 . . ? N1A C7A H7AB 108.9 . . ? C6A C7A H7AB 108.9 . . ? H7AA C7A H7AB 107.7 . . ? N1A C8A N2A 104.0(4) . . ? N1A C8A Pd1A 127.6(3) . . ? N2A C8A Pd1A 128.3(3) . . ? C10A C9A N1A 107.1(5) . . ? C10A C9A H9AA 126.5 . . ? N1A C9A H9AA 126.5 . . ? C9A C10A N2A 106.9(5) . . ? C9A C10A H10A 126.6 . . ? N2A C10A H10A 126.6 . . ? N2A C11A H11A 109.5 . . ? N2A C11A H11B 109.5 . . ? H11A C11A H11B 109.5 . . ? N2A C11A H11C 109.5 . . ? H11A C11A H11C 109.5 . . ? H11B C11A H11C 109.5 . . ? C13A C12A C17A 121.3(7) . . ? C13A C12A H12A 119.4 . . ? C17A C12A H12A 119.4 . . ? C12A C13A C14A 118.5(7) . . ? C12A C13A H13A 120.8 . . ? C14A C13A H13A 120.8 . . ? C15A C14A C13A 122.2(7) . . ? C15A C14A H14A 118.9 . . ? C13A C14A H14A 118.9 . . ? C14A C15A C16A 118.6(7) . . ? C14A C15A H15A 120.7 . . ? C16A C15A H15A 120.7 . . ? C17A C16A C15A 120.8(6) . . ? C17A C16A H16A 119.6 . . ? C15A C16A H16A 119.6 . . ? C16A C17A C12A 118.7(6) . . ? C16A C17A C18A 122.7(5) . . ? C12A C17A C18A 118.5(5) . . ? N3A C18A C17A 114.7(5) . . ? N3A C18A H18A 108.6 . . ? C17A C18A H18A 108.6 . . ? N3A C18A H18B 108.6 . . ? C17A C18A H18B 108.6 . . ? H18A C18A H18B 107.6 . . ? N3A C19A N4A 105.5(4) . . ? N3A C19A Pd1A 128.0(3) . . ? N4A C19A Pd1A 126.1(4) . . ? C21A C20A N3A 106.1(5) . . ? C21A C20A H20A 127.0 . . ? N3A C20A H20A 127.0 . . ? C20A C21A N4A 107.8(5) . . ? C20A C21A H21A 126.1 . . ? N4A C21A H21A 126.1 . . ? N4A C22A H22A 109.5 . . ? N4A C22A H22B 109.5 . . ? H22A C22A H22B 109.5 . . ? N4A C22A H22C 109.5 . . ? H22A C22A H22C 109.5 . . ? H22B C22A H22C 109.5 . . ? C19B Pd1B C8B 90.7(2) . . ? C19B Pd1B Cl1B 87.23(13) . . ? C8B Pd1B Cl1B 177.5(2) . . ? C19B Pd1B Cl2B 178.83(15) . . ? C8B Pd1B Cl2B 89.2(2) . . ? Cl1B Pd1B Cl2B 92.92(6) . . ? C8B N1B C9B 111.4(5) . . ? C8B N1B C7B 125.0(5) . . ? C9B N1B C7B 123.4(5) . . ? C8B N2B C10B 109.4(6) . . ? C8B N2B C11B 125.1(6) . . ? C10B N2B C11B 125.3(6) . . ? C19B N3B C20B 111.1(5) . . ? C19B N3B C18B 123.6(5) . . ? C20B N3B C18B 125.3(5) . . ? C21B N4B C19B 110.4(5) . . ? C21B N4B C22B 125.7(7) . . ? C19B N4B C22B 123.8(6) . . ? C2B C1B C6B 117.6(7) . . ? C2B C1B H1BA 121.2 . . ? C6B C1B H1BA 121.2 . . ? C1B C2B C3B 121.8(8) . . ? C1B C2B H2BA 119.1 . . ? C3B C2B H2BA 119.1 . . ? C4B C3B C2B 118.9(8) . . ? C4B C3B H3BA 120.5 . . ? C2B C3B H3BA 120.5 . . ? C3B C4B C5B 120.9(8) . . ? C3B C4B H4BA 119.6 . . ? C5B C4B H4BA 119.6 . . ? C6B C5B C4B 120.1(7) . . ? C6B C5B H5BA 120.0 . . ? C4B C5B H5BA 120.0 . . ? C5B C6B C1B 120.7(6) . . ? C5B C6B C7B 122.8(6) . . ? C1B C6B C7B 116.4(6) . . ? N1B C7B C6B 114.2(5) . . ? N1B C7B H7BA 108.7 . . ? C6B C7B H7BA 108.7 . . ? N1B C7B H7BB 108.7 . . ? C6B C7B H7BB 108.7 . . ? H7BA C7B H7BB 107.6 . . ? N1B C8B N2B 105.3(5) . . ? N1B C8B Pd1B 129.0(4) . . ? N2B C8B Pd1B 125.6(4) . . ? C10B C9B N1B 106.0(6) . . ? C10B C9B H9BA 127.0 . . ? N1B C9B H9BA 127.0 . . ? C9B C10B N2B 107.8(6) . . ? C9B C10B H10B 126.1 . . ? N2B C10B H10B 126.1 . . ? N2B C11B H11D 109.5 . . ? N2B C11B H11E 109.5 . . ? H11D C11B H11E 109.5 . . ? N2B C11B H11F 109.5 . . ? H11D C11B H11F 109.5 . . ? H11E C11B H11F 109.5 . . ? C13B C12B C17B 120.5(6) . . ? C13B C12B H12B 119.8 . . ? C17B C12B H12B 119.8 . . ? C14B C13B C12B 119.7(6) . . ? C14B C13B H13B 120.1 . . ? C12B C13B H13B 120.1 . . ? C13B C14B C15B 120.9(6) . . ? C13B C14B H14B 119.5 . . ? C15B C14B H14B 119.5 . . ? C14B C15B C16B 119.2(7) . . ? C14B C15B H15B 120.4 . . ? C16B C15B H15B 120.4 . . ? C17B C16B C15B 120.0(6) . . ? C17B C16B H16B 120.0 . . ? C15B C16B H16B 120.0 . . ? C16B C17B C12B 119.4(5) . . ? C16B C17B C18B 120.8(5) . . ? C12B C17B C18B 119.7(5) . . ? N3B C18B C17B 112.0(4) . . ? N3B C18B H18C 109.2 . . ? C17B C18B H18C 109.2 . . ? N3B C18B H18D 109.2 . . ? C17B C18B H18D 109.2 . . ? H18C C18B H18D 107.9 . . ? N3B C19B N4B 103.7(5) . . ? N3B C19B Pd1B 127.6(4) . . ? N4B C19B Pd1B 128.6(4) . . ? C21B C20B N3B 107.4(5) . . ? C21B C20B H20B 126.3 . . ? N3B C20B H20B 126.3 . . ? C20B C21B N4B 107.3(6) . . ? C20B C21B H21B 126.4 . . ? N4B C21B H21B 126.4 . . ? N4B C22B H22D 109.5 . . ? N4B C22B H22E 109.5 . . ? H22D C22B H22E 109.5 . . ? N4B C22B H22F 109.5 . . ? H22D C22B H22F 109.5 . . ? H22E C22B H22F 109.5 . . ? Cl4B C23B Cl3B 109.0(8) . . ? Cl4B C23B H23A 109.9 . . ? Cl3B C23B H23A 109.9 . . ? Cl4B C23B H23B 109.9 . . ? Cl3B C23B H23B 109.9 . . ? H23A C23B H23B 108.3 . . ? Cl3A C23A Cl4A 101.6(9) . . ? Cl3A C23A H23C 111.5 . . ? Cl4A C23A H23C 111.5 . . ? Cl3A C23A H23D 111.5 . . ? Cl4A C23A H23D 111.5 . . ? H23C C23A H23D 109.3 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6A C1A C2A C3A -1.7(10) . . . . ? C1A C2A C3A C4A -1.0(11) . . . . ? C2A C3A C4A C5A 3.8(11) . . . . ? C3A C4A C5A C6A -3.8(10) . . . . ? C2A C1A C6A C5A 1.6(9) . . . . ? C2A C1A C6A C7A -176.4(6) . . . . ? C4A C5A C6A C1A 1.1(9) . . . . ? C4A C5A C6A C7A 179.1(6) . . . . ? C8A N1A C7A C6A -137.2(5) . . . . ? C9A N1A C7A C6A 46.4(7) . . . . ? C1A C6A C7A N1A -100.5(6) . . . . ? C5A C6A C7A N1A 81.6(6) . . . . ? C9A N1A C8A N2A 0.0(5) . . . . ? C7A N1A C8A N2A -176.8(4) . . . . ? C9A N1A C8A Pd1A -176.4(3) . . . . ? C7A N1A C8A Pd1A 6.8(6) . . . . ? C10A N2A C8A N1A 0.7(5) . . . . ? C11A N2A C8A N1A -174.3(6) . . . . ? C10A N2A C8A Pd1A 177.0(4) . . . . ? C11A N2A C8A Pd1A 2.0(8) . . . . ? C19A Pd1A C8A N1A -108.9(4) . . . . ? Cl1A Pd1A C8A N1A 71.9(4) . . . . ? Cl2A Pd1A C8A N1A 41(7) . . . . ? C19A Pd1A C8A N2A 75.7(4) . . . . ? Cl1A Pd1A C8A N2A -103.6(4) . . . . ? Cl2A Pd1A C8A N2A -135(7) . . . . ? C8A N1A C9A C10A -0.7(6) . . . . ? C7A N1A C9A C10A 176.2(4) . . . . ? N1A C9A C10A N2A 1.1(6) . . . . ? C8A N2A C10A C9A -1.1(6) . . . . ? C11A N2A C10A C9A 173.8(6) . . . . ? C17A C12A C13A C14A -0.4(12) . . . . ? C12A C13A C14A C15A 0.3(13) . . . . ? C13A C14A C15A C16A -0.6(12) . . . . ? C14A C15A C16A C17A 0.9(11) . . . . ? C15A C16A C17A C12A -0.9(9) . . . . ? C15A C16A C17A C18A 174.2(6) . . . . ? C13A C12A C17A C16A 0.7(9) . . . . ? C13A C12A C17A C18A -174.6(6) . . . . ? C19A N3A C18A C17A -102.1(6) . . . . ? C20A N3A C18A C17A 81.5(7) . . . . ? C16A C17A C18A N3A 18.9(7) . . . . ? C12A C17A C18A N3A -166.0(5) . . . . ? C20A N3A C19A N4A -0.5(7) . . . . ? C18A N3A C19A N4A -177.3(5) . . . . ? C20A N3A C19A Pd1A 172.1(5) . . . . ? C18A N3A C19A Pd1A -4.6(8) . . . . ? C21A N4A C19A N3A 1.8(7) . . . . ? C22A N4A C19A N3A 178.9(7) . . . . ? C21A N4A C19A Pd1A -171.0(5) . . . . ? C22A N4A C19A Pd1A 6.0(10) . . . . ? C8A Pd1A C19A N3A 79.3(5) . . . . ? Cl1A Pd1A C19A N3A 165(12) . . . . ? Cl2A Pd1A C19A N3A -100.2(5) . . . . ? C8A Pd1A C19A N4A -109.5(5) . . . . ? Cl1A Pd1A C19A N4A -23(12) . . . . ? Cl2A Pd1A C19A N4A 71.1(5) . . . . ? C19A N3A C20A C21A -1.0(8) . . . . ? C18A N3A C20A C21A 175.9(6) . . . . ? N3A C20A C21A N4A 2.1(9) . . . . ? C19A N4A C21A C20A -2.5(9) . . . . ? C22A N4A C21A C20A -179.6(7) . . . . ? C6B C1B C2B C3B 1.5(11) . . . . ? C1B C2B C3B C4B -1.0(13) . . . . ? C2B C3B C4B C5B 0.7(13) . . . . ? C3B C4B C5B C6B -1.0(11) . . . . ? C4B C5B C6B C1B 1.6(9) . . . . ? C4B C5B C6B C7B -174.5(6) . . . . ? C2B C1B C6B C5B -1.8(9) . . . . ? C2B C1B C6B C7B 174.5(6) . . . . ? C8B N1B C7B C6B 108.9(7) . . . . ? C9B N1B C7B C6B -75.7(9) . . . . ? C5B C6B C7B N1B -14.0(8) . . . . ? C1B C6B C7B N1B 169.8(5) . . . . ? C9B N1B C8B N2B -2.4(9) . . . . ? C7B N1B C8B N2B 173.5(7) . . . . ? C9B N1B C8B Pd1B 178.3(6) . . . . ? C7B N1B C8B Pd1B -5.8(11) . . . . ? C10B N2B C8B N1B 1.7(10) . . . . ? C11B N2B C8B N1B -172.9(8) . . . . ? C10B N2B C8B Pd1B -179.0(7) . . . . ? C11B N2B C8B Pd1B 6.4(12) . . . . ? C19B Pd1B C8B N1B -74.5(7) . . . . ? Cl1B Pd1B C8B N1B -108(3) . . . . ? Cl2B Pd1B C8B N1B 104.3(7) . . . . ? C19B Pd1B C8B N2B 106.3(7) . . . . ? Cl1B Pd1B C8B N2B 73(4) . . . . ? Cl2B Pd1B C8B N2B -74.8(7) . . . . ? C8B N1B C9B C10B 2.1(11) . . . . ? C7B N1B C9B C10B -173.8(8) . . . . ? N1B C9B C10B N2B -1.0(12) . . . . ? C8B N2B C10B C9B -0.4(12) . . . . ? C11B N2B C10B C9B 174.2(10) . . . . ? C17B C12B C13B C14B 5.2(10) . . . . ? C12B C13B C14B C15B -4.1(11) . . . . ? C13B C14B C15B C16B 0.3(11) . . . . ? C14B C15B C16B C17B 2.5(10) . . . . ? C15B C16B C17B C12B -1.4(9) . . . . ? C15B C16B C17B C18B 176.6(6) . . . . ? C13B C12B C17B C16B -2.5(9) . . . . ? C13B C12B C17B C18B 179.6(6) . . . . ? C19B N3B C18B C17B 138.4(5) . . . . ? C20B N3B C18B C17B -45.0(7) . . . . ? C16B C17B C18B N3B 100.4(6) . . . . ? C12B C17B C18B N3B -81.7(7) . . . . ? C20B N3B C19B N4B 1.0(5) . . . . ? C18B N3B C19B N4B 178.0(4) . . . . ? C20B N3B C19B Pd1B 179.3(4) . . . . ? C18B N3B C19B Pd1B -3.8(7) . . . . ? C21B N4B C19B N3B -1.3(5) . . . . ? C22B N4B C19B N3B 175.9(6) . . . . ? C21B N4B C19B Pd1B -179.6(4) . . . . ? C22B N4B C19B Pd1B -2.3(8) . . . . ? C8B Pd1B C19B N3B 108.3(4) . . . . ? Cl1B Pd1B C19B N3B -73.1(4) . . . . ? Cl2B Pd1B C19B N3B 24(8) . . . . ? C8B Pd1B C19B N4B -73.8(4) . . . . ? Cl1B Pd1B C19B N4B 104.8(4) . . . . ? Cl2B Pd1B C19B N4B -158(7) . . . . ? C19B N3B C20B C21B -0.3(6) . . . . ? C18B N3B C20B C21B -177.2(5) . . . . ? N3B C20B C21B N4B -0.5(6) . . . . ? C19B N4B C21B C20B 1.2(6) . . . . ? C22B N4B C21B C20B -176.0(6) . . . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 32.14 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 2.412 _refine_diff_density_min -1.653 _refine_diff_density_rms 0.253