# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Sandrine, Bouquillon' _publ_contact_author_email sandrine.bouquillon@univ-reims.fr _publ_section_title ; Synthesis of chiral \^I2-aminoalcohols palladium complexes exhibiting cytotoxic properties ; _publ_author_address ; 'Accadbled, Fabien' 'Institut de Chimie Mol\'eculaire de Reims' 'CNRS UMR 6229, Universit\'e de Reims Champagne-Ardenne' 'BP 1039, 51687 Reims Cedex, France' 'Tinant, Bernard ' 'CSTR 1, Place Louis Pasteur' '1348 Louvain-la-Neuve, Belgique' 'H\'enon, Eric' 'Institut de Chimie Mol\'eculaire de Reims' 'CNRS UMR 6229, Universit\'e de Reims Champagne-Ardenne' 'BP 1039, 51687 Reims Cedex, France.' 'Carrez, Dani\`ele' 'INSERM U759, B\^atiment 112' 'Centre Universitaire, 91405 Orsay, France' 'Centre de Recherche de l'Institut Curie, 91405 Orsay, France' 'Croisy, Alain' 'INSERM U759, B\^atiment 112' 'Centre Universitaire, 91405 Orsay, France' 'Centre de Recherche de l'Institut Curie, 91405 Orsay, France' 'Bouquillon, Sandrine' 'Institut de Chimie Mol\'eculaire de Reims' 'CNRS UMR 6229, Universit\'e de Reims Champagne-Ardenne' 'BP 1039, 51687 Reims Cedex, France.' ; _publ_contact_author_address "Institut de Chimie Mol\'eculaire de Reims" _publ_contact_author_phone 0326918196 loop_ _publ_author_name F.Accadbled B.Tinant E.Henon D.Carrez A.Croisy B.Sandrine # Attachment '- Compound 11.cif' data_fa3a _database_code_depnum_ccdc_archive 'CCDC 745867' #TrackingRef '- Compound 11.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H66 Cl6 N6 O6 Pd3' _chemical_formula_weight 1138.79 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' 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 Orthorhombic _symmetry_space_group_name_H-M P212121 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 9.5874(2) _cell_length_b 20.0334(3) _cell_length_c 23.3478(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4484.37(14) _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 Plaquet _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.687 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2304 _exptl_absorpt_coefficient_mu 1.592 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.5685 _exptl_absorpt_correction_T_max 0.8570 _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 34505 _diffrn_reflns_av_R_equivalents 0.0240 _diffrn_reflns_av_sigmaI/netI 0.0325 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 2.94 _diffrn_reflns_theta_max 27.91 _reflns_number_total 9622 _reflns_number_gt 5785 _reflns_threshold_expression >2sigma(I) _computing_data_collection mar _computing_cell_refinement mar _computing_data_reduction marhkl _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^)+(0.0292P)^2^+0.6240P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00(3) _chemical_absolute_configuration ad _refine_ls_number_reflns 9622 _refine_ls_number_parameters 471 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0697 _refine_ls_R_factor_gt 0.0321 _refine_ls_wR_factor_ref 0.0743 _refine_ls_wR_factor_gt 0.0655 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.042 _refine_ls_shift/su_max 0.002 _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 Pd1 Pd 0.27014(3) -0.168260(13) 0.392000(12) 0.03517(9) Uani 1 1 d . . . Pd2 Pd 0.26899(3) 0.166445(13) 0.393810(12) 0.03285(9) Uani 1 1 d . . . Pd3 Pd 0.27462(3) -0.500096(14) 0.390012(11) 0.03586(9) Uani 1 1 d . . . Cl1 Cl 0.13226(14) -0.25933(5) 0.37342(7) 0.0806(5) Uani 1 1 d . . . Cl2 Cl 0.40567(13) -0.07786(5) 0.41511(6) 0.0640(4) Uani 1 1 d . . . Cl3 Cl 0.12349(12) 0.07583(5) 0.40023(5) 0.0530(3) Uani 1 1 d . . . Cl4 Cl 0.41673(13) 0.25759(5) 0.39412(6) 0.0583(3) Uani 1 1 d . . . Cl5 Cl 0.12781(14) -0.59103(5) 0.38809(7) 0.0750(4) Uani 1 1 d . . . Cl6 Cl 0.42071(14) -0.40888(5) 0.39499(7) 0.0747(4) Uani 1 1 d . . . N1 N 0.4372(3) -0.23246(14) 0.39955(13) 0.0388(8) Uani 1 1 d . . . H1C H 0.4046 -0.2734 0.3893 0.047 Uiso 1 1 calc R . . N2 N 0.1057(4) -0.10327(16) 0.38414(15) 0.0434(9) Uani 1 1 d . . . H2C H 0.1438 -0.0617 0.3821 0.12(2) Uiso 1 1 calc R . . N3 N 0.4322(4) 0.10115(16) 0.38981(14) 0.0425(9) Uani 1 1 d . . . H3C H 0.3942 0.0596 0.3879 0.035(11) Uiso 1 1 calc R . . N4 N 0.1052(3) 0.23276(15) 0.39680(14) 0.0381(8) Uani 1 1 d . . . H4C H 0.1427 0.2741 0.3918 0.087(17) Uiso 1 1 calc R . . N5 N 0.4374(3) -0.56579(16) 0.39206(14) 0.0385(8) Uani 1 1 d . . . H5C H 0.4007 -0.6067 0.3843 0.042(12) Uiso 1 1 calc R . . N6 N 0.1103(3) -0.43484(15) 0.38768(13) 0.0382(8) Uani 1 1 d . . . H6C H 0.1482 -0.3932 0.3859 0.047(12) Uiso 1 1 calc R . . O1 O 0.6461(6) -0.2269(2) 0.26738(19) 0.156(2) Uani 1 1 d . . . H1D H 0.6300 -0.1921 0.2502 0.234 Uiso 1 1 calc R . . O2 O 0.1627(4) -0.03312(13) 0.28198(14) 0.0700(9) Uani 1 1 d . . . H2D H 0.1091 -0.0014 0.2795 0.105 Uiso 1 1 calc R . . O3 O 0.4423(5) 0.00894(19) 0.28932(18) 0.1140(14) Uani 1 1 d . . . H3D H 0.5131 -0.0080 0.3027 0.171 Uiso 1 1 calc R . . O4 O 0.1377(4) 0.19913(13) 0.27117(13) 0.0663(9) Uani 1 1 d . . . H4D H 0.2054 0.2183 0.2574 0.099 Uiso 1 1 calc R . . O5 O 0.4366(6) -0.5996(2) 0.2690(2) 0.1171(17) Uani 1 1 d . . . H5D H 0.4163 -0.5601 0.2656 0.176 Uiso 1 1 calc R . . O6 O -0.0016(4) -0.42236(14) 0.23659(12) 0.0706(10) Uani 1 1 d . . . H6D H -0.0603 -0.3926 0.2381 0.106 Uiso 1 1 calc R . . C1 C 0.4918(5) -0.2401(2) 0.45874(18) 0.0602(13) Uani 1 1 d . . . H1A H 0.4411 -0.2747 0.4790 0.072 Uiso 1 1 calc R . . H1B H 0.4827 -0.1986 0.4798 0.072 Uiso 1 1 calc R . . C2 C 0.6426(5) -0.2589(3) 0.4525(2) 0.102(2) Uani 1 1 d . . . H2A H 0.7009 -0.2286 0.4744 0.122 Uiso 1 1 calc R . . H2B H 0.6580 -0.3039 0.4665 0.122 Uiso 1 1 calc R . . C3 C 0.6760(6) -0.2547(3) 0.3923(3) 0.102(2) Uani 1 1 d . . . H3A H 0.6879 -0.2991 0.3766 0.123 Uiso 1 1 calc R . . H3B H 0.7626 -0.2304 0.3872 0.123 Uiso 1 1 calc R . . C4 C 0.5590(5) -0.2192(2) 0.3616(2) 0.0607(14) Uani 1 1 d . . . H4 H 0.5780 -0.1712 0.3603 0.073 Uiso 1 1 calc R . . C5 C 0.5271(7) -0.2442(3) 0.3026(2) 0.111(3) Uani 1 1 d . . . H5A H 0.5134 -0.2922 0.3030 0.133 Uiso 1 1 calc R . . H5B H 0.4432 -0.2233 0.2879 0.133 Uiso 1 1 calc R . . C6 C 0.0120(5) -0.1025(2) 0.4348(2) 0.0669(15) Uani 1 1 d . . . H6A H 0.0561 -0.0798 0.4666 0.080 Uiso 1 1 calc R . . H6B H -0.0110 -0.1477 0.4464 0.080 Uiso 1 1 calc R . . C7 C -0.1177(5) -0.0655(2) 0.4158(2) 0.0730(15) Uani 1 1 d . . . H7A H -0.2010 -0.0886 0.4287 0.088 Uiso 1 1 calc R . . H7B H -0.1185 -0.0205 0.4312 0.088 Uiso 1 1 calc R . . C8 C -0.1107(5) -0.0643(2) 0.3513(2) 0.0637(14) Uani 1 1 d . . . H8A H -0.0956 -0.0191 0.3377 0.076 Uiso 1 1 calc R . . H8B H -0.1970 -0.0809 0.3350 0.076 Uiso 1 1 calc R . . C9 C 0.0116(4) -0.10919(18) 0.33406(19) 0.0473(11) Uani 1 1 d . . . H9 H -0.0221 -0.1553 0.3320 0.057 Uiso 1 1 calc R . . C10 C 0.0858(5) -0.09350(18) 0.27969(19) 0.0560(13) Uani 1 1 d . . . H10A H 0.1490 -0.1298 0.2707 0.067 Uiso 1 1 calc R . . H10B H 0.0181 -0.0905 0.2489 0.067 Uiso 1 1 calc R . . C11 C 0.5257(6) 0.1012(2) 0.4405(2) 0.0777(17) Uani 1 1 d . . . H11A H 0.5356 0.1460 0.4556 0.093 Uiso 1 1 calc R . . H11B H 0.4884 0.0726 0.4703 0.093 Uiso 1 1 calc R . . C12 C 0.6618(7) 0.0756(4) 0.4203(4) 0.139(3) Uani 1 1 d . . . H12A H 0.7367 0.1036 0.4346 0.167 Uiso 1 1 calc R . . H12B H 0.6765 0.0305 0.4342 0.167 Uiso 1 1 calc R . . C13 C 0.6603(6) 0.0764(4) 0.3573(3) 0.116(3) Uani 1 1 d . . . H13A H 0.6671 0.0313 0.3426 0.140 Uiso 1 1 calc R . . H13B H 0.7388 0.1019 0.3429 0.140 Uiso 1 1 calc R . . C14 C 0.5232(5) 0.1084(2) 0.3380(2) 0.0672(15) Uani 1 1 d . . . H14 H 0.5394 0.1560 0.3310 0.081 Uiso 1 1 calc R . . C15 C 0.4598(6) 0.0782(3) 0.2857(2) 0.0784(16) Uani 1 1 d . . . H15A H 0.3696 0.0988 0.2790 0.094 Uiso 1 1 calc R . . H15B H 0.5187 0.0883 0.2530 0.094 Uiso 1 1 calc R . . C16 C 0.0305(5) 0.2345(2) 0.45236(19) 0.0653(14) Uani 1 1 d . . . H16A H 0.0822 0.2604 0.4803 0.078 Uiso 1 1 calc R . . H16B H 0.0171 0.1897 0.4672 0.078 Uiso 1 1 calc R . . C17 C -0.1095(5) 0.2673(3) 0.4392(2) 0.0833(17) Uani 1 1 d . . . H17A H -0.1850 0.2421 0.4565 0.100 Uiso 1 1 calc R . . H17B H -0.1117 0.3125 0.4542 0.100 Uiso 1 1 calc R . . C18 C -0.1240(5) 0.2681(2) 0.3756(2) 0.0664(13) Uani 1 1 d . . . H18A H -0.1175 0.3133 0.3610 0.080 Uiso 1 1 calc R . . H18B H -0.2132 0.2494 0.3642 0.080 Uiso 1 1 calc R . . C19 C -0.0044(4) 0.2255(2) 0.35304(17) 0.0468(11) Uani 1 1 d . . . H19 H -0.0342 0.1787 0.3515 0.056 Uiso 1 1 calc R . . C20 C 0.0450(5) 0.24665(19) 0.29447(19) 0.0579(13) Uani 1 1 d . . . H20A H -0.0347 0.2518 0.2692 0.069 Uiso 1 1 calc R . . H20B H 0.0916 0.2895 0.2972 0.069 Uiso 1 1 calc R . . C21 C 0.5003(5) -0.5706(3) 0.4498(2) 0.0738(16) Uani 1 1 d . . . H21A H 0.4463 -0.6002 0.4740 0.089 Uiso 1 1 calc R . . H21B H 0.5050 -0.5270 0.4678 0.089 Uiso 1 1 calc R . . C22 C 0.6435(6) -0.5980(3) 0.4400(3) 0.100(2) Uani 1 1 d . . . H22A H 0.7051 -0.5872 0.4716 0.121 Uiso 1 1 calc R . . H22B H 0.6411 -0.6461 0.4351 0.121 Uiso 1 1 calc R . . C23 C 0.6866(6) -0.5656(4) 0.3888(3) 0.124(3) Uani 1 1 d . . . H23A H 0.7553 -0.5926 0.3690 0.149 Uiso 1 1 calc R . . H23B H 0.7282 -0.5227 0.3977 0.149 Uiso 1 1 calc R . . C24 C 0.5546(5) -0.5559(2) 0.3504(2) 0.0627(14) Uani 1 1 d . . . H24 H 0.5523 -0.5105 0.3347 0.075 Uiso 1 1 calc R . . C25 C 0.5554(8) -0.6058(3) 0.3033(3) 0.123(3) Uani 1 1 d . . . H25A H 0.6381 -0.5994 0.2800 0.147 Uiso 1 1 calc R . . H25B H 0.5591 -0.6503 0.3194 0.147 Uiso 1 1 calc R . . C26 C 0.0187(5) -0.4353(2) 0.43885(19) 0.0592(13) Uani 1 1 d . . . H26A H 0.0651 -0.4145 0.4712 0.071 Uiso 1 1 calc R . . H26B H -0.0068 -0.4806 0.4491 0.071 Uiso 1 1 calc R . . C27 C -0.1094(5) -0.3954(2) 0.42133(19) 0.0629(13) Uani 1 1 d . . . H27A H -0.1933 -0.4150 0.4374 0.076 Uiso 1 1 calc R . . H27B H -0.1020 -0.3496 0.4344 0.076 Uiso 1 1 calc R . . C28 C -0.1123(5) -0.3984(2) 0.35680(17) 0.0554(12) Uani 1 1 d . . . H28A H -0.1067 -0.3539 0.3407 0.066 Uiso 1 1 calc R . . H28B H -0.1979 -0.4192 0.3437 0.066 Uiso 1 1 calc R . . C29 C 0.0142(4) -0.43998(17) 0.33870(17) 0.0382(10) Uani 1 1 d . . . H29 H -0.0148 -0.4866 0.3345 0.046 Uiso 1 1 calc R . . C30 C 0.0861(5) -0.4183(2) 0.28466(17) 0.0535(12) Uani 1 1 d . . . H30A H 0.1179 -0.3726 0.2891 0.064 Uiso 1 1 calc R . . H30B H 0.1674 -0.4462 0.2784 0.064 Uiso 1 1 calc R . . 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 0.0336(2) 0.02685(15) 0.04500(18) 0.00065(15) -0.00291(14) 0.00565(14) Pd2 0.0323(2) 0.02761(16) 0.03865(17) -0.00208(15) 0.00079(14) 0.00489(15) Pd3 0.0347(2) 0.02797(14) 0.04490(19) 0.00054(17) -0.00277(14) 0.00527(16) Cl1 0.0531(8) 0.0299(6) 0.1588(13) -0.0027(7) -0.0275(9) -0.0004(6) Cl2 0.0560(8) 0.0356(5) 0.1005(10) -0.0047(6) -0.0319(8) -0.0003(6) Cl3 0.0468(7) 0.0338(5) 0.0784(8) 0.0000(6) 0.0041(7) -0.0034(5) Cl4 0.0440(7) 0.0356(5) 0.0955(9) -0.0011(6) -0.0028(7) -0.0021(5) Cl5 0.0438(7) 0.0327(6) 0.1485(13) 0.0045(7) 0.0040(9) 0.0006(5) Cl6 0.0506(8) 0.0333(6) 0.1402(13) -0.0089(7) -0.0172(9) -0.0006(5) N1 0.039(2) 0.0332(17) 0.044(2) 0.0120(16) -0.0023(17) 0.0083(16) N2 0.038(2) 0.0334(18) 0.059(2) 0.0032(16) 0.004(2) 0.0081(17) N3 0.033(2) 0.043(2) 0.051(2) -0.0027(17) 0.006(2) 0.0122(17) N4 0.029(2) 0.0345(18) 0.051(2) -0.0003(16) 0.0037(18) 0.0066(15) N5 0.035(2) 0.0361(19) 0.044(2) 0.0104(16) 0.0066(18) 0.0076(16) N6 0.040(2) 0.0353(19) 0.039(2) 0.0009(15) -0.0014(18) 0.0060(17) O1 0.176(5) 0.187(5) 0.105(3) 0.062(3) 0.078(4) 0.106(4) O2 0.074(2) 0.0600(18) 0.076(2) 0.0080(19) 0.006(2) -0.0027(18) O3 0.143(4) 0.105(3) 0.094(3) -0.032(2) 0.024(3) -0.009(3) O4 0.080(3) 0.0560(17) 0.063(2) -0.0014(16) 0.0077(19) -0.0098(18) O5 0.138(5) 0.094(3) 0.119(4) 0.000(3) -0.013(4) -0.021(3) O6 0.101(3) 0.060(2) 0.051(2) -0.0040(17) -0.019(2) 0.0150(19) C1 0.064(4) 0.061(3) 0.055(3) 0.006(2) -0.011(3) 0.022(3) C2 0.047(4) 0.163(6) 0.096(4) 0.040(4) -0.015(4) 0.030(4) C3 0.043(3) 0.134(5) 0.129(6) 0.041(4) 0.024(4) 0.024(4) C4 0.049(3) 0.055(3) 0.079(4) 0.026(3) 0.019(3) 0.012(2) C5 0.159(7) 0.109(5) 0.065(4) 0.013(3) 0.055(4) 0.036(5) C6 0.068(4) 0.067(3) 0.066(3) 0.017(3) 0.030(3) 0.028(3) C7 0.045(3) 0.063(3) 0.110(5) 0.004(3) 0.024(3) 0.016(3) C8 0.030(3) 0.057(3) 0.104(4) 0.011(3) -0.004(3) 0.015(2) C9 0.040(3) 0.029(2) 0.073(3) 0.009(2) -0.017(3) 0.0068(19) C10 0.079(4) 0.038(2) 0.051(3) -0.002(2) -0.013(3) 0.000(2) C11 0.077(4) 0.061(3) 0.095(4) -0.010(3) -0.045(4) 0.020(3) C12 0.064(5) 0.160(6) 0.194(9) -0.039(6) -0.039(6) 0.052(5) C13 0.034(4) 0.145(6) 0.171(7) -0.081(6) 0.008(4) 0.006(4) C14 0.061(4) 0.044(3) 0.096(4) -0.015(3) 0.029(3) 0.004(2) C15 0.090(4) 0.073(3) 0.072(4) -0.004(3) 0.029(3) 0.012(3) C16 0.062(3) 0.073(3) 0.061(3) -0.006(3) 0.020(3) 0.030(3) C17 0.052(4) 0.096(4) 0.101(4) -0.022(3) 0.018(3) 0.022(3) C18 0.040(3) 0.062(3) 0.097(4) -0.012(3) -0.006(3) 0.013(2) C19 0.036(3) 0.040(2) 0.065(3) 0.001(2) -0.010(2) 0.000(2) C20 0.074(4) 0.037(2) 0.062(3) -0.001(2) -0.013(3) 0.009(2) C21 0.077(4) 0.083(3) 0.061(3) 0.001(3) -0.015(3) 0.042(3) C22 0.055(4) 0.130(5) 0.116(5) 0.011(4) -0.029(4) 0.025(4) C23 0.051(4) 0.157(6) 0.164(7) 0.063(6) 0.012(5) 0.019(4) C24 0.071(4) 0.037(3) 0.080(3) 0.010(2) 0.035(3) 0.008(2) C25 0.166(8) 0.053(3) 0.149(7) 0.016(4) 0.097(6) 0.008(4) C26 0.061(3) 0.062(3) 0.055(3) 0.001(2) 0.002(3) 0.024(3) C27 0.051(3) 0.069(3) 0.069(3) -0.001(3) 0.010(3) 0.016(3) C28 0.042(3) 0.065(3) 0.059(3) -0.001(2) -0.003(3) 0.007(2) C29 0.039(3) 0.028(2) 0.047(2) -0.0008(18) -0.006(2) 0.0010(18) C30 0.063(3) 0.052(2) 0.045(3) -0.001(2) -0.013(3) 0.014(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 Pd1 N2 2.053(3) . ? Pd1 N1 2.062(3) . ? Pd1 Cl2 2.2933(11) . ? Pd1 Cl1 2.2943(11) . ? Pd2 N3 2.042(3) . ? Pd2 N4 2.058(3) . ? Pd2 Cl3 2.2943(11) . ? Pd2 Cl4 2.3109(11) . ? Pd3 N5 2.042(3) . ? Pd3 N6 2.048(3) . ? Pd3 Cl5 2.3026(11) . ? Pd3 Cl6 2.3053(12) . ? N1 C1 1.486(5) . ? N1 C4 1.490(5) . ? N1 H1C 0.9100 . ? N2 C9 1.481(5) . ? N2 C6 1.484(5) . ? N2 H2C 0.9100 . ? N3 C11 1.484(5) . ? N3 C14 1.498(6) . ? N3 H3C 0.9100 . ? N4 C19 1.473(5) . ? N4 C16 1.482(5) . ? N4 H4C 0.9100 . ? N5 C21 1.480(5) . ? N5 C24 1.499(5) . ? N5 H5C 0.9100 . ? N6 C29 1.472(5) . ? N6 C26 1.483(5) . ? N6 H6C 0.9100 . ? O1 C5 1.448(6) . ? O1 H1D 0.8200 . ? O2 C10 1.418(4) . ? O2 H2D 0.8200 . ? O3 C15 1.401(5) . ? O3 H3D 0.8200 . ? O4 C20 1.412(5) . ? O4 H4D 0.8200 . ? O5 C25 1.399(8) . ? O5 H5D 0.8200 . ? O6 C30 1.405(5) . ? O6 H6D 0.8200 . ? C1 C2 1.501(6) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 C3 1.444(7) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C4 1.510(7) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 C5 1.496(7) . ? C4 H4 0.9800 . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 C7 1.514(6) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C8 1.509(6) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C9 1.532(5) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.489(6) . ? C9 H9 0.9800 . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C12 1.478(7) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 C13 1.472(9) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 C14 1.530(7) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 C15 1.493(7) . ? C14 H14 0.9800 . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 C17 1.526(6) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 C18 1.492(7) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 C19 1.523(6) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 C20 1.508(5) . ? C19 H19 0.9800 . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 C22 1.497(6) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 C23 1.422(8) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 C24 1.563(7) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 C25 1.485(7) . ? C24 H24 0.9800 . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 C27 1.521(6) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C27 C28 1.508(6) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 C29 1.531(5) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C29 C30 1.502(5) . ? C29 H29 0.9800 . ? C30 H30A 0.9700 . ? C30 H30B 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 N2 Pd1 N1 179.20(13) . . ? N2 Pd1 Cl2 87.45(10) . . ? N1 Pd1 Cl2 91.86(9) . . ? N2 Pd1 Cl1 92.57(10) . . ? N1 Pd1 Cl1 88.15(10) . . ? Cl2 Pd1 Cl1 177.28(6) . . ? N3 Pd2 N4 179.24(14) . . ? N3 Pd2 Cl3 87.83(11) . . ? N4 Pd2 Cl3 92.56(10) . . ? N3 Pd2 Cl4 92.10(11) . . ? N4 Pd2 Cl4 87.56(10) . . ? Cl3 Pd2 Cl4 176.07(6) . . ? N5 Pd3 N6 179.52(14) . . ? N5 Pd3 Cl5 87.58(10) . . ? N6 Pd3 Cl5 91.96(10) . . ? N5 Pd3 Cl6 92.59(10) . . ? N6 Pd3 Cl6 87.86(10) . . ? Cl5 Pd3 Cl6 178.22(7) . . ? C1 N1 C4 107.2(3) . . ? C1 N1 Pd1 114.7(2) . . ? C4 N1 Pd1 116.5(2) . . ? C1 N1 H1C 105.9 . . ? C4 N1 H1C 105.9 . . ? Pd1 N1 H1C 105.9 . . ? C9 N2 C6 105.1(3) . . ? C9 N2 Pd1 119.2(2) . . ? C6 N2 Pd1 113.6(3) . . ? C9 N2 H2C 106.0 . . ? C6 N2 H2C 106.0 . . ? Pd1 N2 H2C 106.0 . . ? C11 N3 C14 107.0(4) . . ? C11 N3 Pd2 115.2(3) . . ? C14 N3 Pd2 114.9(3) . . ? C11 N3 H3C 106.4 . . ? C14 N3 H3C 106.4 . . ? Pd2 N3 H3C 106.4 . . ? C19 N4 C16 105.3(3) . . ? C19 N4 Pd2 117.2(2) . . ? C16 N4 Pd2 114.4(2) . . ? C19 N4 H4C 106.4 . . ? C16 N4 H4C 106.4 . . ? Pd2 N4 H4C 106.4 . . ? C21 N5 C24 107.1(4) . . ? C21 N5 Pd3 112.0(3) . . ? C24 N5 Pd3 118.2(2) . . ? C21 N5 H5C 106.3 . . ? C24 N5 H5C 106.3 . . ? Pd3 N5 H5C 106.3 . . ? C29 N6 C26 104.8(3) . . ? C29 N6 Pd3 117.2(2) . . ? C26 N6 Pd3 115.5(2) . . ? C29 N6 H6C 106.2 . . ? C26 N6 H6C 106.2 . . ? Pd3 N6 H6C 106.2 . . ? C5 O1 H1D 109.5 . . ? C10 O2 H2D 109.5 . . ? C15 O3 H3D 109.5 . . ? C20 O4 H4D 109.5 . . ? C25 O5 H5D 109.5 . . ? C30 O6 H6D 109.5 . . ? N1 C1 C2 106.0(4) . . ? N1 C1 H1A 110.5 . . ? C2 C1 H1A 110.5 . . ? N1 C1 H1B 110.5 . . ? C2 C1 H1B 110.5 . . ? H1A C1 H1B 108.7 . . ? C3 C2 C1 107.0(4) . . ? C3 C2 H2A 110.3 . . ? C1 C2 H2A 110.3 . . ? C3 C2 H2B 110.3 . . ? C1 C2 H2B 110.3 . . ? H2A C2 H2B 108.6 . . ? C2 C3 C4 109.1(4) . . ? C2 C3 H3A 109.9 . . ? C4 C3 H3A 109.9 . . ? C2 C3 H3B 109.9 . . ? C4 C3 H3B 109.9 . . ? H3A C3 H3B 108.3 . . ? N1 C4 C5 109.1(4) . . ? N1 C4 C3 102.4(3) . . ? C5 C4 C3 115.6(5) . . ? N1 C4 H4 109.8 . . ? C5 C4 H4 109.8 . . ? C3 C4 H4 109.8 . . ? O1 C5 C4 106.4(5) . . ? O1 C5 H5A 110.5 . . ? C4 C5 H5A 110.5 . . ? O1 C5 H5B 110.5 . . ? C4 C5 H5B 110.5 . . ? H5A C5 H5B 108.6 . . ? N2 C6 C7 105.6(4) . . ? N2 C6 H6A 110.6 . . ? C7 C6 H6A 110.6 . . ? N2 C6 H6B 110.6 . . ? C7 C6 H6B 110.6 . . ? H6A C6 H6B 108.7 . . ? C8 C7 C6 105.2(4) . . ? C8 C7 H7A 110.7 . . ? C6 C7 H7A 110.7 . . ? C8 C7 H7B 110.7 . . ? C6 C7 H7B 110.7 . . ? H7A C7 H7B 108.8 . . ? C7 C8 C9 106.7(4) . . ? C7 C8 H8A 110.4 . . ? C9 C8 H8A 110.4 . . ? C7 C8 H8B 110.4 . . ? C9 C8 H8B 110.4 . . ? H8A C8 H8B 108.6 . . ? N2 C9 C10 111.4(4) . . ? N2 C9 C8 102.2(3) . . ? C10 C9 C8 117.8(4) . . ? N2 C9 H9 108.3 . . ? C10 C9 H9 108.3 . . ? C8 C9 H9 108.3 . . ? O2 C10 C9 113.4(3) . . ? O2 C10 H10A 108.9 . . ? C9 C10 H10A 108.9 . . ? O2 C10 H10B 108.9 . . ? C9 C10 H10B 108.9 . . ? H10A C10 H10B 107.7 . . ? C12 C11 N3 106.2(5) . . ? C12 C11 H11A 110.5 . . ? N3 C11 H11A 110.5 . . ? C12 C11 H11B 110.5 . . ? N3 C11 H11B 110.5 . . ? H11A C11 H11B 108.7 . . ? C13 C12 C11 107.8(6) . . ? C13 C12 H12A 110.1 . . ? C11 C12 H12A 110.1 . . ? C13 C12 H12B 110.1 . . ? C11 C12 H12B 110.1 . . ? H12A C12 H12B 108.5 . . ? C12 C13 C14 107.9(5) . . ? C12 C13 H13A 110.1 . . ? C14 C13 H13A 110.1 . . ? C12 C13 H13B 110.1 . . ? C14 C13 H13B 110.1 . . ? H13A C13 H13B 108.4 . . ? C15 C14 N3 112.6(4) . . ? C15 C14 C13 114.9(4) . . ? N3 C14 C13 102.8(4) . . ? C15 C14 H14 108.7 . . ? N3 C14 H14 108.7 . . ? C13 C14 H14 108.7 . . ? O3 C15 C14 113.6(4) . . ? O3 C15 H15A 108.9 . . ? C14 C15 H15A 108.9 . . ? O3 C15 H15B 108.9 . . ? C14 C15 H15B 108.9 . . ? H15A C15 H15B 107.7 . . ? N4 C16 C17 105.0(4) . . ? N4 C16 H16A 110.7 . . ? C17 C16 H16A 110.7 . . ? N4 C16 H16B 110.7 . . ? C17 C16 H16B 110.7 . . ? H16A C16 H16B 108.8 . . ? C18 C17 C16 106.7(4) . . ? C18 C17 H17A 110.4 . . ? C16 C17 H17A 110.4 . . ? C18 C17 H17B 110.4 . . ? C16 C17 H17B 110.4 . . ? H17A C17 H17B 108.6 . . ? C17 C18 C19 105.6(4) . . ? C17 C18 H18A 110.6 . . ? C19 C18 H18A 110.6 . . ? C17 C18 H18B 110.6 . . ? C19 C18 H18B 110.6 . . ? H18A C18 H18B 108.8 . . ? N4 C19 C20 112.2(3) . . ? N4 C19 C18 104.0(3) . . ? C20 C19 C18 113.1(4) . . ? N4 C19 H19 109.1 . . ? C20 C19 H19 109.1 . . ? C18 C19 H19 109.1 . . ? O4 C20 C19 111.0(3) . . ? O4 C20 H20A 109.4 . . ? C19 C20 H20A 109.4 . . ? O4 C20 H20B 109.4 . . ? C19 C20 H20B 109.4 . . ? H20A C20 H20B 108.0 . . ? N5 C21 C22 105.0(4) . . ? N5 C21 H21A 110.7 . . ? C22 C21 H21A 110.7 . . ? N5 C21 H21B 110.7 . . ? C22 C21 H21B 110.7 . . ? H21A C21 H21B 108.8 . . ? C23 C22 C21 103.1(5) . . ? C23 C22 H22A 111.1 . . ? C21 C22 H22A 111.1 . . ? C23 C22 H22B 111.1 . . ? C21 C22 H22B 111.1 . . ? H22A C22 H22B 109.1 . . ? C22 C23 C24 107.7(5) . . ? C22 C23 H23A 110.2 . . ? C24 C23 H23A 110.2 . . ? C22 C23 H23B 110.2 . . ? C24 C23 H23B 110.2 . . ? H23A C23 H23B 108.5 . . ? C25 C24 N5 113.3(4) . . ? C25 C24 C23 109.7(5) . . ? N5 C24 C23 102.6(4) . . ? C25 C24 H24 110.3 . . ? N5 C24 H24 110.3 . . ? C23 C24 H24 110.3 . . ? O5 C25 C24 111.2(5) . . ? O5 C25 H25A 109.4 . . ? C24 C25 H25A 109.4 . . ? O5 C25 H25B 109.4 . . ? C24 C25 H25B 109.4 . . ? H25A C25 H25B 108.0 . . ? N6 C26 C27 105.0(3) . . ? N6 C26 H26A 110.8 . . ? C27 C26 H26A 110.8 . . ? N6 C26 H26B 110.8 . . ? C27 C26 H26B 110.8 . . ? H26A C26 H26B 108.8 . . ? C28 C27 C26 105.2(4) . . ? C28 C27 H27A 110.7 . . ? C26 C27 H27A 110.7 . . ? C28 C27 H27B 110.7 . . ? C26 C27 H27B 110.7 . . ? H27A C27 H27B 108.8 . . ? C27 C28 C29 106.4(4) . . ? C27 C28 H28A 110.4 . . ? C29 C28 H28A 110.4 . . ? C27 C28 H28B 110.4 . . ? C29 C28 H28B 110.4 . . ? H28A C28 H28B 108.6 . . ? N6 C29 C30 110.2(3) . . ? N6 C29 C28 104.1(3) . . ? C30 C29 C28 116.0(3) . . ? N6 C29 H29 108.8 . . ? C30 C29 H29 108.8 . . ? C28 C29 H29 108.8 . . ? O6 C30 C29 112.3(4) . . ? O6 C30 H30A 109.1 . . ? C29 C30 H30A 109.1 . . ? O6 C30 H30B 109.1 . . ? C29 C30 H30B 109.1 . . ? H30A C30 H30B 107.9 . . ? 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 N2 Pd1 N1 C1 97(10) . . . . ? Cl2 Pd1 N1 C1 67.3(3) . . . . ? Cl1 Pd1 N1 C1 -110.0(3) . . . . ? N2 Pd1 N1 C4 -29(11) . . . . ? Cl2 Pd1 N1 C4 -59.1(3) . . . . ? Cl1 Pd1 N1 C4 123.6(3) . . . . ? N1 Pd1 N2 C9 105(10) . . . . ? Cl2 Pd1 N2 C9 134.9(3) . . . . ? Cl1 Pd1 N2 C9 -47.8(3) . . . . ? N1 Pd1 N2 C6 -131(10) . . . . ? Cl2 Pd1 N2 C6 -100.4(3) . . . . ? Cl1 Pd1 N2 C6 76.9(3) . . . . ? N4 Pd2 N3 C11 127(11) . . . . ? Cl3 Pd2 N3 C11 -111.5(3) . . . . ? Cl4 Pd2 N3 C11 64.6(3) . . . . ? N4 Pd2 N3 C14 2(11) . . . . ? Cl3 Pd2 N3 C14 123.4(3) . . . . ? Cl4 Pd2 N3 C14 -60.5(3) . . . . ? N3 Pd2 N4 C19 64(11) . . . . ? Cl3 Pd2 N4 C19 -56.8(3) . . . . ? Cl4 Pd2 N4 C19 127.2(3) . . . . ? N3 Pd2 N4 C16 -172(21) . . . . ? Cl3 Pd2 N4 C16 67.3(3) . . . . ? Cl4 Pd2 N4 C16 -108.8(3) . . . . ? N6 Pd3 N5 C21 -126(17) . . . . ? Cl5 Pd3 N5 C21 -104.4(3) . . . . ? Cl6 Pd3 N5 C21 73.8(3) . . . . ? N6 Pd3 N5 C24 109(17) . . . . ? Cl5 Pd3 N5 C24 130.3(3) . . . . ? Cl6 Pd3 N5 C24 -51.5(3) . . . . ? N5 Pd3 N6 C29 -37(17) . . . . ? Cl5 Pd3 N6 C29 -58.2(3) . . . . ? Cl6 Pd3 N6 C29 123.6(3) . . . . ? N5 Pd3 N6 C26 87(17) . . . . ? Cl5 Pd3 N6 C26 66.1(3) . . . . ? Cl6 Pd3 N6 C26 -112.1(3) . . . . ? C4 N1 C1 C2 -22.4(5) . . . . ? Pd1 N1 C1 C2 -153.5(3) . . . . ? N1 C1 C2 C3 6.1(6) . . . . ? C1 C2 C3 C4 12.3(7) . . . . ? C1 N1 C4 C5 151.9(4) . . . . ? Pd1 N1 C4 C5 -78.1(4) . . . . ? C1 N1 C4 C3 28.9(5) . . . . ? Pd1 N1 C4 C3 159.0(3) . . . . ? C2 C3 C4 N1 -25.5(6) . . . . ? C2 C3 C4 C5 -144.0(6) . . . . ? N1 C4 C5 O1 177.3(4) . . . . ? C3 C4 C5 O1 -68.0(6) . . . . ? C9 N2 C6 C7 -35.0(5) . . . . ? Pd1 N2 C6 C7 -167.0(3) . . . . ? N2 C6 C7 C8 16.0(5) . . . . ? C6 C7 C8 C9 8.0(5) . . . . ? C6 N2 C9 C10 165.6(3) . . . . ? Pd1 N2 C9 C10 -65.7(4) . . . . ? C6 N2 C9 C8 39.0(4) . . . . ? Pd1 N2 C9 C8 167.7(3) . . . . ? C7 C8 C9 N2 -28.8(4) . . . . ? C7 C8 C9 C10 -151.2(4) . . . . ? N2 C9 C10 O2 -49.1(5) . . . . ? C8 C9 C10 O2 68.5(5) . . . . ? C14 N3 C11 C12 -26.9(5) . . . . ? Pd2 N3 C11 C12 -156.0(4) . . . . ? N3 C11 C12 C13 13.6(7) . . . . ? C11 C12 C13 C14 4.4(8) . . . . ? C11 N3 C14 C15 152.9(4) . . . . ? Pd2 N3 C14 C15 -77.8(4) . . . . ? C11 N3 C14 C13 28.7(5) . . . . ? Pd2 N3 C14 C13 158.0(3) . . . . ? C12 C13 C14 C15 -143.0(6) . . . . ? C12 C13 C14 N3 -20.2(7) . . . . ? N3 C14 C15 O3 -64.1(6) . . . . ? C13 C14 C15 O3 53.2(7) . . . . ? C19 N4 C16 C17 -31.6(4) . . . . ? Pd2 N4 C16 C17 -161.8(3) . . . . ? N4 C16 C17 C18 13.4(5) . . . . ? C16 C17 C18 C19 9.1(5) . . . . ? C16 N4 C19 C20 160.0(3) . . . . ? Pd2 N4 C19 C20 -71.5(4) . . . . ? C16 N4 C19 C18 37.3(4) . . . . ? Pd2 N4 C19 C18 165.9(3) . . . . ? C17 C18 C19 N4 -28.5(5) . . . . ? C17 C18 C19 C20 -150.5(4) . . . . ? N4 C19 C20 O4 73.2(4) . . . . ? C18 C19 C20 O4 -169.5(4) . . . . ? C24 N5 C21 C22 -28.1(5) . . . . ? Pd3 N5 C21 C22 -159.2(4) . . . . ? N5 C21 C22 C23 38.5(7) . . . . ? C21 C22 C23 C24 -33.9(7) . . . . ? C21 N5 C24 C25 125.7(5) . . . . ? Pd3 N5 C24 C25 -106.7(5) . . . . ? C21 N5 C24 C23 7.5(5) . . . . ? Pd3 N5 C24 C23 135.1(4) . . . . ? C22 C23 C24 C25 -103.8(6) . . . . ? C22 C23 C24 N5 16.9(7) . . . . ? N5 C24 C25 O5 64.4(6) . . . . ? C23 C24 C25 O5 178.4(5) . . . . ? C29 N6 C26 C27 -37.3(4) . . . . ? Pd3 N6 C26 C27 -167.8(3) . . . . ? N6 C26 C27 C28 22.4(5) . . . . ? C26 C27 C28 C29 0.0(5) . . . . ? C26 N6 C29 C30 161.8(3) . . . . ? Pd3 N6 C29 C30 -68.6(3) . . . . ? C26 N6 C29 C28 36.8(4) . . . . ? Pd3 N6 C29 C28 166.3(2) . . . . ? C27 C28 C29 N6 -22.5(4) . . . . ? C27 C28 C29 C30 -143.7(4) . . . . ? N6 C29 C30 O6 180.0(3) . . . . ? C28 C29 C30 O6 -62.1(5) . . . . ? _diffrn_measured_fraction_theta_max 0.929 _diffrn_reflns_theta_full 27.91 _diffrn_measured_fraction_theta_full 0.929 _refine_diff_density_max 0.358 _refine_diff_density_min -0.397 _refine_diff_density_rms 0.059 # Attachment '- Compound 13.cif' data_facc _database_code_depnum_ccdc_archive 'CCDC 745868' #TrackingRef '- Compound 13.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C17 H37 Cl4 N3 O4.50 Pd1.50' _chemical_formula_weight 656.90 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' Pd Pd -0.9988 1.0072 '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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M ' C2221 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, -z' '-x, -y, z+1/2' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, -z' '-x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, -z+1/2' _cell_length_a 15.444(5) _cell_length_b 16.302(5) _cell_length_c 20.352(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5124(3) _cell_formula_units_Z 8 _cell_measurement_temperature 120(2) #_cell_measurement_reflns_used 'all' _cell_measurement_theta_min 3.5 _cell_measurement_theta_max 26. _exptl_crystal_description bloc _exptl_crystal_colour yellow _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.5 _exptl_crystal_size_min 0.45 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.703 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2664 _exptl_absorpt_coefficient_mu 1.511 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'RU200 rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'mar345 image plate' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean 6.66 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 89627 _diffrn_reflns_av_R_equivalents 0.051 _diffrn_reflns_av_sigmaI/netI 0.0163 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 3.20 _diffrn_reflns_theta_max 26.40 _reflns_number_total 5207 _reflns_number_gt 5207 _reflns_threshold_expression >2sigma(I) _computing_data_collection mar _computing_cell_refinement mar _computing_data_reduction marhkl _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; H atoms of the solvent molecules were not localized 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^)+(0.0321P)^2^+32.3454P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _chemical_absolute_configuration ad _refine_ls_abs_structure_Flack 0.01(3) _refine_ls_number_reflns 5207 _refine_ls_number_parameters 292 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0288 _refine_ls_R_factor_gt 0.0288 _refine_ls_wR_factor_ref 0.0812 _refine_ls_wR_factor_gt 0.0812 _refine_ls_goodness_of_fit_ref 1.159 _refine_ls_restrained_S_all 1.159 _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 Pd1 Pd 0.603471(19) 0.603542(18) 0.687278(14) 0.01420(8) Uani 1 1 d . . . N1 N 0.7002(2) 0.5232(2) 0.71219(17) 0.0159(7) Uani 1 1 d . . . C2 C 0.7570(3) 0.5694(3) 0.7592(2) 0.0188(9) Uani 1 1 d . . . H2 H 0.7925 0.5299 0.7855 0.028(3) Uiso 1 1 calc R . . C3 C 0.8162(3) 0.6195(3) 0.7134(2) 0.0247(10) Uani 1 1 d . . . H3A H 0.8773 0.6152 0.7279 0.028(3) Uiso 1 1 calc R . . H3B H 0.7992 0.6780 0.7139 0.028(3) Uiso 1 1 calc R . . C4 C 0.8057(3) 0.5835(3) 0.6436(2) 0.0238(10) Uani 1 1 d . . . H4A H 0.7711 0.6205 0.6153 0.028(3) Uiso 1 1 calc R . . H4B H 0.8626 0.5738 0.6227 0.028(3) Uiso 1 1 calc R . . C5 C 0.7581(3) 0.5028(3) 0.6561(2) 0.0190(9) Uani 1 1 d . . . H5A H 0.7243 0.4858 0.6171 0.028(3) Uiso 1 1 calc R . . H5B H 0.7990 0.4585 0.6679 0.028(3) Uiso 1 1 calc R . . C6 C 0.7010(3) 0.6198(3) 0.8044(2) 0.0224(9) Uani 1 1 d . . . H6A H 0.6675 0.5832 0.8338 0.028(3) Uiso 1 1 calc R . . H6B H 0.7377 0.6557 0.8320 0.028(3) Uiso 1 1 calc R . . O7 O 0.64304(19) 0.66867(19) 0.76601(14) 0.0175(6) Uani 1 1 d . . . N11 N 0.5098(3) 0.6857(2) 0.66030(17) 0.0159(7) Uani 1 1 d . . . C12 C 0.4926(3) 0.6702(3) 0.58930(19) 0.0184(8) Uani 1 1 d . . . H12 H 0.4351 0.6935 0.5766 0.028(3) Uiso 1 1 calc R . . C13 C 0.5663(3) 0.7181(3) 0.5545(2) 0.0236(10) Uani 1 1 d . . . H13A H 0.6144 0.6809 0.5423 0.028(3) Uiso 1 1 calc R . . H13B H 0.5446 0.7456 0.5144 0.028(3) Uiso 1 1 calc R . . C14 C 0.5967(3) 0.7820(3) 0.6059(2) 0.0245(9) Uani 1 1 d . . . H14A H 0.6571 0.7709 0.6197 0.028(3) Uiso 1 1 calc R . . H14B H 0.5935 0.8382 0.5876 0.028(3) Uiso 1 1 calc R . . C15 C 0.5360(3) 0.7727(3) 0.6629(2) 0.0211(9) Uani 1 1 d . . . H15A H 0.5655 0.7854 0.7049 0.028(3) Uiso 1 1 calc R . . H15B H 0.4852 0.8093 0.6581 0.028(3) Uiso 1 1 calc R . . C16 C 0.4937(3) 0.5786(2) 0.5774(2) 0.0185(8) Uani 1 1 d . . . H16A H 0.4415 0.5535 0.5973 0.028(3) Uiso 1 1 calc R . . H16B H 0.4922 0.5677 0.5295 0.028(3) Uiso 1 1 calc R . . O17 O 0.5694(2) 0.54220(19) 0.60506(14) 0.0171(6) Uani 1 1 d . . . Pd2 Pd 0.5000 0.38382(3) 0.7500 0.01430(10) Uani 1 2 d S . . N21 N 0.5232(2) 0.3835(2) 0.65079(16) 0.0154(7) Uani 1 1 d . . . C22 C 0.4426(3) 0.3501(3) 0.6201(2) 0.0191(9) Uani 1 1 d . . . H22 H 0.4407 0.3649 0.5724 0.028(3) Uiso 1 1 calc R . . C23 C 0.4556(3) 0.2569(3) 0.6281(3) 0.0263(10) Uani 1 1 d . . . H23A H 0.4249 0.2367 0.6676 0.028(3) Uiso 1 1 calc R . . H23B H 0.4333 0.2272 0.5892 0.028(3) Uiso 1 1 calc R . . C24 C 0.5536(4) 0.2443(3) 0.6351(3) 0.0276(11) Uani 1 1 d . . . H24A H 0.5676 0.2198 0.6783 0.028(3) Uiso 1 1 calc R . . H24B H 0.5755 0.2077 0.6000 0.028(3) Uiso 1 1 calc R . . C25 C 0.5937(3) 0.3292(3) 0.6290(2) 0.0184(8) Uani 1 1 d . . . H25A H 0.6452 0.3347 0.6576 0.028(3) Uiso 1 1 calc R . . H25B H 0.6105 0.3410 0.5830 0.028(3) Uiso 1 1 calc R . . C26 C 0.3648(3) 0.3860(3) 0.6555(2) 0.0222(9) Uani 1 1 d . . . H26A H 0.3588 0.4447 0.6439 0.028(3) Uiso 1 1 calc R . . H26B H 0.3116 0.3572 0.6409 0.028(3) Uiso 1 1 calc R . . O27 O 0.37333(19) 0.3782(2) 0.72486(14) 0.0193(6) Uani 1 1 d . . . H1 H 0.677(4) 0.482(4) 0.732(3) 0.023 Uiso 1 1 d . . . H11 H 0.469(4) 0.674(4) 0.679(3) 0.023 Uiso 1 1 d . . . H21 H 0.544(4) 0.428(4) 0.637(3) 0.023 Uiso 1 1 d . . . Cl1 Cl 0.90234(9) 0.38310(8) 0.53223(6) 0.0342(3) Uani 1 1 d . . . Cl2 Cl 0.78091(9) 0.24727(9) 0.51161(7) 0.0357(3) Uani 1 1 d . . . C100 C 0.7976(4) 0.3442(3) 0.5494(3) 0.0300(11) Uani 1 1 d . . . H101 H 0.755(4) 0.387(5) 0.529(3) 0.045 Uiso 1 1 d . . . H102 H 0.794(5) 0.337(4) 0.601(3) 0.045 Uiso 1 1 d . . . C200 C 1.0000 0.4478(5) 0.7500 0.0385(17) Uani 1 2 d S . . Cl3 Cl 1.02167(8) 0.50742(9) 0.67955(7) 0.0369(3) Uani 1 1 d . . . H201 H 0.955(4) 0.415(4) 0.743(4) 0.055 Uiso 1 1 d . . . C300 C 0.6945(12) 1.0167(12) 0.5451(9) 0.069(4) Uiso 0.50 1 d P . . Cl4 Cl 0.5967(2) 1.0000 0.5000 0.1044(16) Uani 1 2 d S . . Cl5 Cl 0.7840(2) 1.0000 0.5000 0.0844(11) Uani 1 2 d S . . O400 O 0.1727(3) 1.0000 0.5000 0.0279(11) Uani 1 2 d S . . O500 O 0.2055(2) 0.3273(2) 0.77326(19) 0.0325(8) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.01562(14) 0.01505(14) 0.01192(13) -0.00013(11) 0.00030(11) -0.00028(12) N1 0.0149(17) 0.0173(17) 0.0155(16) 0.0010(14) -0.0006(14) -0.0018(15) C2 0.019(2) 0.022(2) 0.016(2) 0.0015(16) -0.0020(16) 0.0023(16) C3 0.020(2) 0.024(2) 0.031(2) -0.0001(19) 0.0054(18) 0.0004(19) C4 0.026(2) 0.026(2) 0.020(2) 0.0039(17) 0.0058(18) -0.0020(18) C5 0.0167(19) 0.024(2) 0.017(2) -0.0009(17) 0.0002(16) 0.0037(18) C6 0.0202(19) 0.029(2) 0.018(2) 0.0034(19) -0.0009(16) -0.0015(19) O7 0.0187(14) 0.0192(15) 0.0147(15) -0.0023(11) -0.0013(11) -0.0006(12) N11 0.0169(17) 0.0177(16) 0.0130(15) -0.0003(13) 0.0032(14) 0.0018(15) C12 0.024(2) 0.019(2) 0.0123(18) 0.0011(15) -0.0047(17) 0.0030(19) C13 0.031(2) 0.024(2) 0.015(2) -0.0001(18) 0.0074(18) -0.0037(19) C14 0.029(2) 0.024(2) 0.021(2) -0.0011(17) 0.000(2) -0.004(2) C15 0.028(2) 0.013(2) 0.022(2) 0.0011(16) 0.0009(18) 0.0055(17) C16 0.022(2) 0.0203(19) 0.0136(18) 0.0003(15) -0.0072(17) 0.0008(18) O17 0.0202(15) 0.0173(14) 0.0139(14) -0.0025(11) -0.0027(11) 0.0013(12) Pd2 0.01595(19) 0.0155(2) 0.01144(18) 0.000 0.00008(15) 0.000 N21 0.0189(17) 0.0174(17) 0.0100(14) 0.0031(13) 0.0014(12) -0.0028(14) C22 0.021(2) 0.023(2) 0.0126(19) 0.0008(16) 0.0011(16) -0.0047(18) C23 0.031(3) 0.023(2) 0.025(2) -0.0076(19) 0.004(2) -0.008(2) C24 0.037(3) 0.019(2) 0.028(3) 0.0024(19) 0.002(2) 0.002(2) C25 0.020(2) 0.021(2) 0.0138(18) -0.0026(15) 0.0021(17) 0.0033(18) C26 0.025(2) 0.025(2) 0.0161(19) 0.0016(19) -0.0027(16) -0.002(2) O27 0.0194(14) 0.0243(16) 0.0141(13) -0.0014(12) -0.0012(11) -0.0012(13) Cl1 0.0315(6) 0.0350(6) 0.0362(6) 0.0004(5) -0.0031(5) 0.0006(6) Cl2 0.0294(6) 0.0351(7) 0.0425(8) -0.0087(6) -0.0096(5) 0.0041(5) C100 0.028(2) 0.036(3) 0.026(2) -0.004(2) 0.000(2) 0.006(2) C200 0.040(4) 0.024(3) 0.052(5) 0.000 -0.002(4) 0.000 Cl3 0.0352(7) 0.0425(7) 0.0331(7) 0.0000(6) -0.0038(5) 0.0016(5) Cl4 0.0437(14) 0.155(4) 0.114(3) 0.088(3) 0.000 0.000 Cl5 0.0493(15) 0.143(3) 0.0607(18) 0.015(2) 0.000 0.000 O400 0.025(2) 0.037(3) 0.021(2) -0.006(2) 0.000 0.000 O500 0.0289(18) 0.0267(18) 0.042(2) -0.0102(15) 0.0084(16) -0.0048(16) _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 Pd1 O7 2.017(3) . ? Pd1 O17 2.019(3) . ? Pd1 N11 2.046(4) . ? Pd1 N1 2.050(4) . ? N1 C5 1.488(5) . ? N1 C2 1.501(6) . ? N1 H1 0.86(6) . ? C2 C6 1.507(6) . ? C2 C3 1.541(6) . ? C2 H2 1.0000 . ? C3 C4 1.546(7) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.528(6) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 O7 1.431(5) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? N11 C15 1.476(6) . ? N11 C12 1.491(5) . ? N11 H11 0.75(6) . ? C12 C16 1.513(6) . ? C12 C13 1.552(6) . ? C12 H12 1.0000 . ? C13 C14 1.549(6) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.499(7) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 O17 1.426(5) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? Pd2 O27 2.024(3) . ? Pd2 O27 2.024(3) 4_656 ? Pd2 N21 2.051(3) 4_656 ? Pd2 N21 2.051(3) . ? N21 C25 1.473(5) . ? N21 C22 1.495(5) . ? N21 H21 0.84(6) . ? C22 C26 1.519(6) . ? C22 C23 1.542(7) . ? C22 H22 1.0000 . ? C23 C24 1.535(7) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 C25 1.520(6) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 O27 1.424(5) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? Cl1 C100 1.772(6) . ? Cl2 C100 1.776(6) . ? C100 H101 1.04(7) . ? C100 H102 1.05(7) . ? C200 Cl3 1.764(4) 4_756 ? C200 Cl3 1.764(4) . ? C200 H201 0.90(7) . ? C300 Cl5 1.682(19) . ? C300 Cl4 1.789(19) . ? C300 C300 1.92(4) 2_576 ? Cl4 C300 1.789(19) 2_576 ? Cl5 C300 1.682(19) 2_576 ? 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 O7 Pd1 O17 176.42(13) . . ? O7 Pd1 N11 94.75(13) . . ? O17 Pd1 N11 85.26(13) . . ? O7 Pd1 N1 85.34(13) . . ? O17 Pd1 N1 94.52(13) . . ? N11 Pd1 N1 178.04(16) . . ? C5 N1 C2 104.5(3) . . ? C5 N1 Pd1 113.0(3) . . ? C2 N1 Pd1 105.3(3) . . ? C5 N1 H1 116(4) . . ? C2 N1 H1 109(4) . . ? Pd1 N1 H1 108(4) . . ? N1 C2 C6 109.1(4) . . ? N1 C2 C3 103.1(4) . . ? C6 C2 C3 114.9(4) . . ? N1 C2 H2 109.8 . . ? C6 C2 H2 109.8 . . ? C3 C2 H2 109.8 . . ? C2 C3 C4 107.0(4) . . ? C2 C3 H3A 110.3 . . ? C4 C3 H3A 110.3 . . ? C2 C3 H3B 110.3 . . ? C4 C3 H3B 110.3 . . ? H3A C3 H3B 108.6 . . ? C5 C4 C3 103.0(4) . . ? C5 C4 H4A 111.2 . . ? C3 C4 H4A 111.2 . . ? C5 C4 H4B 111.2 . . ? C3 C4 H4B 111.2 . . ? H4A C4 H4B 109.1 . . ? N1 C5 C4 102.9(4) . . ? N1 C5 H5A 111.2 . . ? C4 C5 H5A 111.2 . . ? N1 C5 H5B 111.2 . . ? C4 C5 H5B 111.2 . . ? H5A C5 H5B 109.1 . . ? O7 C6 C2 109.2(3) . . ? O7 C6 H6A 109.8 . . ? C2 C6 H6A 109.8 . . ? O7 C6 H6B 109.8 . . ? C2 C6 H6B 109.8 . . ? H6A C6 H6B 108.3 . . ? C6 O7 Pd1 109.3(3) . . ? C15 N11 C12 104.3(3) . . ? C15 N11 Pd1 115.2(3) . . ? C12 N11 Pd1 106.0(3) . . ? C15 N11 H11 117(5) . . ? C12 N11 H11 107(5) . . ? Pd1 N11 H11 107(4) . . ? N11 C12 C16 108.7(3) . . ? N11 C12 C13 103.1(4) . . ? C16 C12 C13 114.6(4) . . ? N11 C12 H12 110.1 . . ? C16 C12 H12 110.1 . . ? C13 C12 H12 110.1 . . ? C14 C13 C12 104.6(3) . . ? C14 C13 H13A 110.8 . . ? C12 C13 H13A 110.8 . . ? C14 C13 H13B 110.8 . . ? C12 C13 H13B 110.8 . . ? H13A C13 H13B 108.9 . . ? C15 C14 C13 105.4(4) . . ? C15 C14 H14A 110.7 . . ? C13 C14 H14A 110.7 . . ? C15 C14 H14B 110.7 . . ? C13 C14 H14B 110.7 . . ? H14A C14 H14B 108.8 . . ? N11 C15 C14 103.9(4) . . ? N11 C15 H15A 111.0 . . ? C14 C15 H15A 111.0 . . ? N11 C15 H15B 111.0 . . ? C14 C15 H15B 111.0 . . ? H15A C15 H15B 109.0 . . ? O17 C16 C12 110.9(4) . . ? O17 C16 H16A 109.5 . . ? C12 C16 H16A 109.5 . . ? O17 C16 H16B 109.5 . . ? C12 C16 H16B 109.5 . . ? H16A C16 H16B 108.1 . . ? C16 O17 Pd1 109.6(2) . . ? O27 Pd2 O27 174.83(19) . 4_656 ? O27 Pd2 N21 94.60(13) . 4_656 ? O27 Pd2 N21 85.39(13) 4_656 4_656 ? O27 Pd2 N21 85.39(13) . . ? O27 Pd2 N21 94.60(13) 4_656 . ? N21 Pd2 N21 179.7(2) 4_656 . ? C25 N21 C22 105.7(3) . . ? C25 N21 Pd2 115.3(3) . . ? C22 N21 Pd2 105.5(2) . . ? C25 N21 H21 97(4) . . ? C22 N21 H21 120(4) . . ? Pd2 N21 H21 113(4) . . ? N21 C22 C26 108.7(4) . . ? N21 C22 C23 101.9(4) . . ? C26 C22 C23 115.6(4) . . ? N21 C22 H22 110.1 . . ? C26 C22 H22 110.1 . . ? C23 C22 H22 110.1 . . ? C24 C23 C22 105.6(4) . . ? C24 C23 H23A 110.6 . . ? C22 C23 H23A 110.6 . . ? C24 C23 H23B 110.6 . . ? C22 C23 H23B 110.6 . . ? H23A C23 H23B 108.7 . . ? C25 C24 C23 105.8(4) . . ? C25 C24 H24A 110.6 . . ? C23 C24 H24A 110.6 . . ? C25 C24 H24B 110.6 . . ? C23 C24 H24B 110.6 . . ? H24A C24 H24B 108.7 . . ? N21 C25 C24 102.8(4) . . ? N21 C25 H25A 111.2 . . ? C24 C25 H25A 111.2 . . ? N21 C25 H25B 111.2 . . ? C24 C25 H25B 111.2 . . ? H25A C25 H25B 109.1 . . ? O27 C26 C22 111.3(4) . . ? O27 C26 H26A 109.4 . . ? C22 C26 H26A 109.4 . . ? O27 C26 H26B 109.4 . . ? C22 C26 H26B 109.4 . . ? H26A C26 H26B 108.0 . . ? C26 O27 Pd2 109.7(3) . . ? Cl1 C100 Cl2 111.5(3) . . ? Cl1 C100 H101 105(4) . . ? Cl2 C100 H101 110(4) . . ? Cl1 C100 H102 106(4) . . ? Cl2 C100 H102 109(4) . . ? H101 C100 H102 115(5) . . ? Cl3 C200 Cl3 113.1(4) 4_756 . ? Cl3 C200 H201 108(5) 4_756 . ? Cl3 C200 H201 111(5) . . ? Cl5 C300 Cl4 112.9(10) . . ? Cl5 C300 C300 55.3(6) . 2_576 ? Cl4 C300 C300 57.6(6) . 2_576 ? C300 Cl4 C300 64.8(12) . 2_576 ? C300 Cl5 C300 69.5(13) 2_576 . ? 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 O7 Pd1 N1 C5 -129.0(3) . . . . ? O17 Pd1 N1 C5 47.4(3) . . . . ? N11 Pd1 N1 C5 -36(5) . . . . ? O7 Pd1 N1 C2 -15.5(3) . . . . ? O17 Pd1 N1 C2 160.9(3) . . . . ? N11 Pd1 N1 C2 77(4) . . . . ? C5 N1 C2 C6 158.9(3) . . . . ? Pd1 N1 C2 C6 39.6(4) . . . . ? C5 N1 C2 C3 36.4(4) . . . . ? Pd1 N1 C2 C3 -82.9(3) . . . . ? N1 C2 C3 C4 -13.8(4) . . . . ? C6 C2 C3 C4 -132.3(4) . . . . ? C2 C3 C4 C5 -12.9(5) . . . . ? C2 N1 C5 C4 -45.4(4) . . . . ? Pd1 N1 C5 C4 68.6(4) . . . . ? C3 C4 C5 N1 35.1(4) . . . . ? N1 C2 C6 O7 -52.5(5) . . . . ? C3 C2 C6 O7 62.7(5) . . . . ? C2 C6 O7 Pd1 37.5(4) . . . . ? O17 Pd1 O7 C6 -100(2) . . . . ? N11 Pd1 O7 C6 169.8(3) . . . . ? N1 Pd1 O7 C6 -12.1(3) . . . . ? O7 Pd1 N11 C15 43.6(3) . . . . ? O17 Pd1 N11 C15 -132.8(3) . . . . ? N1 Pd1 N11 C15 -49(5) . . . . ? O7 Pd1 N11 C12 158.3(3) . . . . ? O17 Pd1 N11 C12 -18.1(3) . . . . ? N1 Pd1 N11 C12 66(4) . . . . ? C15 N11 C12 C16 161.9(4) . . . . ? Pd1 N11 C12 C16 39.9(4) . . . . ? C15 N11 C12 C13 39.9(4) . . . . ? Pd1 N11 C12 C13 -82.1(3) . . . . ? N11 C12 C13 C14 -21.0(5) . . . . ? C16 C12 C13 C14 -139.0(4) . . . . ? C12 C13 C14 C15 -4.7(5) . . . . ? C12 N11 C15 C14 -43.7(4) . . . . ? Pd1 N11 C15 C14 72.0(4) . . . . ? C13 C14 C15 N11 29.2(5) . . . . ? N11 C12 C16 O17 -49.7(5) . . . . ? C13 C12 C16 O17 65.0(5) . . . . ? C12 C16 O17 Pd1 33.0(4) . . . . ? O7 Pd1 O17 C16 -99(2) . . . . ? N11 Pd1 O17 C16 -8.1(3) . . . . ? N1 Pd1 O17 C16 173.8(3) . . . . ? O27 Pd2 N21 C25 -135.8(3) . . . . ? O27 Pd2 N21 C25 39.0(3) 4_656 . . . ? N21 Pd2 N21 C25 -48.4(4) 4_656 . . . ? O27 Pd2 N21 C22 -19.6(3) . . . . ? O27 Pd2 N21 C22 155.2(3) 4_656 . . . ? N21 Pd2 N21 C22 67.8(3) 4_656 . . . ? C25 N21 C22 C26 163.3(3) . . . . ? Pd2 N21 C22 C26 40.7(4) . . . . ? C25 N21 C22 C23 40.8(4) . . . . ? Pd2 N21 C22 C23 -81.8(3) . . . . ? N21 C22 C23 C24 -23.1(5) . . . . ? C26 C22 C23 C24 -140.7(4) . . . . ? C22 C23 C24 C25 -1.6(5) . . . . ? C22 N21 C25 C24 -42.2(4) . . . . ? Pd2 N21 C25 C24 73.9(4) . . . . ? C23 C24 C25 N21 26.1(5) . . . . ? N21 C22 C26 O27 -49.3(5) . . . . ? C23 C22 C26 O27 64.5(5) . . . . ? C22 C26 O27 Pd2 31.3(5) . . . . ? O27 Pd2 O27 C26 -96.4(3) 4_656 . . . ? N21 Pd2 O27 C26 174.0(3) 4_656 . . . ? N21 Pd2 O27 C26 -6.3(3) . . . . ? Cl5 C300 Cl4 C300 0.000(2) . . . 2_576 ? Cl4 C300 Cl5 C300 0.000(2) . . . 2_576 ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 26.40 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.532 _refine_diff_density_min -1.005 _refine_diff_density_rms 0.129 # Attachment '- Compound 6.cif' data_ha28 _database_code_depnum_ccdc_archive 'CCDC 745869' #TrackingRef '- Compound 6.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H32 N2 O6 Pd' _chemical_formula_weight 430.82 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' 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 ' P21 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 7.873(3) _cell_length_b 10.736(4) _cell_length_c 11.073(4) _cell_angle_alpha 90.00 _cell_angle_beta 95.92(2) _cell_angle_gamma 90.00 _cell_volume 930.9(6) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) #_cell_measurement_reflns_used 'all' _cell_measurement_theta_min 3. _cell_measurement_theta_max 24.7 _exptl_crystal_description plate _exptl_crystal_colour ' colourless ' _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.537 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 448 _exptl_absorpt_coefficient_mu 1.026 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'RU200 rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'MAR345 image plate' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean 6.66 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13971 _diffrn_reflns_av_R_equivalents 0.010 _diffrn_reflns_av_sigmaI/netI 0.0333 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 3.03 _diffrn_reflns_theta_max 24.71 _reflns_number_total 3163 _reflns_number_gt 3078 _reflns_threshold_expression >2sigma(I) _computing_data_collection mar _computing_cell_refinement mar _computing_data_reduction marhkl _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Constrains were applied on the N-H bond lengths for which the H atoms were localized by Fourier difference to keep values in the range 0.92-0.98 \%A 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^)+(0.1352P)^2^+0.0695P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.01(6) _chemical_absolute_configuration ad _refine_ls_number_reflns 3163 _refine_ls_number_parameters 220 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.0646 _refine_ls_R_factor_gt 0.0638 _refine_ls_wR_factor_ref 0.1690 _refine_ls_wR_factor_gt 0.1667 _refine_ls_goodness_of_fit_ref 1.203 _refine_ls_restrained_S_all 1.202 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.26100(5) 0.51160(16) 0.00299(3) 0.0161(2) Uani 1 1 d . . . N1 N 0.5099(8) 0.5426(6) 0.0806(5) 0.0222(15) Uani 1 1 d D . . C2 C 0.6078(9) 0.4441(6) 0.1528(6) 0.0226(14) Uani 1 1 d . . . H2 H 0.7255 0.4766 0.1766 0.027 Uiso 1 1 calc R . . C3 C 0.6228(10) 0.3311(6) 0.0694(6) 0.0254(15) Uani 1 1 d . . . H3A H 0.6946 0.2656 0.1118 0.030 Uiso 1 1 calc R . . H3B H 0.5086 0.2957 0.0437 0.030 Uiso 1 1 calc R . . O4 O 0.7002(7) 0.3771(5) -0.0332(5) 0.0258(10) Uani 1 1 d . . . H4 H 0.7106 0.3186 -0.0822 0.031 Uiso 1 1 calc R . . C5 C 0.5286(9) 0.4124(7) 0.2680(6) 0.0251(14) Uani 1 1 d . . . H5 H 0.4073 0.3872 0.2450 0.030 Uiso 1 1 calc R . . C6 C 0.5291(10) 0.5245(9) 0.3534(6) 0.0347(16) Uani 1 1 d . . . H6A H 0.4750 0.5014 0.4260 0.042 Uiso 1 1 calc R . . H6B H 0.4656 0.5933 0.3117 0.042 Uiso 1 1 calc R . . H6C H 0.6471 0.5507 0.3771 0.042 Uiso 1 1 calc R . . C7 C 0.6208(11) 0.3037(7) 0.3365(6) 0.0348(17) Uani 1 1 d . . . H7A H 0.5643 0.2847 0.4092 0.042 Uiso 1 1 calc R . . H7B H 0.7400 0.3267 0.3604 0.042 Uiso 1 1 calc R . . H7C H 0.6169 0.2303 0.2837 0.042 Uiso 1 1 calc R . . N11 N 0.0248(7) 0.4955(6) -0.0928(5) 0.0215(12) Uani 1 1 d D . . C12 C -0.0142(10) 0.6081(7) -0.1720(6) 0.0229(14) Uani 1 1 d . . . H12 H 0.0935 0.6328 -0.2063 0.027 Uiso 1 1 calc R . . C13 C -0.0609(9) 0.7121(7) -0.0891(5) 0.0239(14) Uani 1 1 d . . . H13A H 0.0330 0.7258 -0.0238 0.029 Uiso 1 1 calc R . . H13B H -0.0796 0.7905 -0.1358 0.029 Uiso 1 1 calc R . . O14 O -0.2132(7) 0.6776(5) -0.0378(5) 0.0284(11) Uani 1 1 d . . . H14 H -0.2405 0.7344 0.0086 0.034 Uiso 1 1 calc R . . C15 C -0.1484(9) 0.5780(7) -0.2796(6) 0.0270(15) Uani 1 1 d . . . H15 H -0.2584 0.5550 -0.2476 0.032 Uiso 1 1 calc R . . C16 C -0.1769(12) 0.6924(8) -0.3607(7) 0.046(2) Uani 1 1 d . . . H16A H -0.2625 0.6733 -0.4289 0.056 Uiso 1 1 calc R . . H16B H -0.0693 0.7158 -0.3919 0.056 Uiso 1 1 calc R . . H16C H -0.2174 0.7616 -0.3136 0.056 Uiso 1 1 calc R . . C17 C -0.0921(12) 0.4713(7) -0.3570(7) 0.0371(19) Uani 1 1 d . . . H17A H -0.1809 0.4549 -0.4238 0.044 Uiso 1 1 calc R . . H17B H -0.0735 0.3964 -0.3068 0.044 Uiso 1 1 calc R . . H17C H 0.0144 0.4940 -0.3901 0.044 Uiso 1 1 calc R . . O20 O 0.3591(6) 0.5040(16) -0.1577(5) 0.0218(16) Uani 1 1 d . . . C21 C 0.3600(9) 0.3919(7) -0.2082(6) 0.0253(14) Uani 1 1 d . . . O22 O 0.3053(7) 0.2950(5) -0.1682(4) 0.0289(11) Uani 1 1 d . . . C23 C 0.4364(10) 0.3918(7) -0.3281(6) 0.0305(16) Uani 1 1 d . . . H23A H 0.4753 0.4760 -0.3456 0.037 Uiso 1 1 calc R . . H23B H 0.3499 0.3651 -0.3929 0.037 Uiso 1 1 calc R . . H23C H 0.5335 0.3343 -0.3235 0.037 Uiso 1 1 calc R . . O30 O 0.1499(6) 0.5192(15) 0.1599(4) 0.0187(14) Uani 1 1 d . . . C31 C 0.1377(9) 0.6161(7) 0.2202(6) 0.0260(15) Uani 1 1 d . . . O32 O 0.1998(8) 0.7183(5) 0.1947(5) 0.0420(14) Uani 1 1 d . . . C33 C 0.0450(11) 0.6041(7) 0.3309(7) 0.0342(18) Uani 1 1 d . . . H33A H 0.0036 0.5184 0.3372 0.041 Uiso 1 1 calc R . . H33B H -0.0521 0.6616 0.3249 0.041 Uiso 1 1 calc R . . H33C H 0.1228 0.6242 0.4032 0.041 Uiso 1 1 calc R . . H1A H 0.577(11) 0.553(8) 0.018(6) 0.051 Uiso 1 1 d D . . H1B H 0.507(14) 0.611(7) 0.135(8) 0.051 Uiso 1 1 d D . . H11A H -0.063(9) 0.487(9) -0.041(7) 0.051 Uiso 1 1 d D . . H11B H 0.010(12) 0.417(5) -0.130(8) 0.051 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.0148(3) 0.0150(3) 0.0190(3) -0.0004(2) 0.0045(2) 0.0005(4) N1 0.022(3) 0.021(4) 0.025(3) -0.007(2) 0.010(2) 0.000(2) C2 0.022(4) 0.021(3) 0.025(3) -0.006(2) 0.001(3) -0.004(3) C3 0.022(4) 0.022(3) 0.031(3) 0.003(2) 0.000(3) 0.007(2) O4 0.020(3) 0.027(3) 0.032(2) 0.000(2) 0.007(2) 0.002(2) C5 0.023(4) 0.030(3) 0.024(3) 0.003(3) 0.005(3) 0.004(3) C6 0.037(4) 0.036(5) 0.031(3) 0.000(4) 0.005(3) 0.003(4) C7 0.038(5) 0.035(4) 0.033(4) 0.005(3) 0.009(3) 0.007(3) N11 0.018(3) 0.017(3) 0.030(3) 0.005(2) 0.004(2) 0.003(3) C12 0.022(4) 0.028(3) 0.020(3) 0.002(3) 0.007(3) -0.002(3) C13 0.019(4) 0.027(3) 0.025(3) 0.005(2) -0.001(3) 0.008(3) O14 0.018(2) 0.026(2) 0.042(3) -0.013(2) 0.007(2) -0.007(2) C15 0.019(3) 0.035(4) 0.027(4) -0.009(3) 0.000(3) -0.003(3) C16 0.054(6) 0.045(4) 0.036(4) -0.005(4) -0.010(4) 0.026(4) C17 0.047(5) 0.033(4) 0.031(4) 0.001(3) -0.002(3) 0.003(3) O20 0.020(2) 0.024(5) 0.023(2) -0.012(4) 0.0045(18) -0.008(3) C21 0.018(4) 0.035(4) 0.022(3) 0.005(3) 0.000(3) -0.003(3) O22 0.033(3) 0.025(2) 0.030(2) -0.0021(19) 0.006(2) -0.006(2) C23 0.036(4) 0.030(3) 0.026(4) -0.001(3) 0.012(3) -0.001(3) O30 0.023(2) 0.013(4) 0.020(2) 0.007(3) 0.0052(18) 0.005(3) C31 0.025(4) 0.025(3) 0.028(3) 0.003(3) 0.004(3) -0.003(3) O32 0.065(4) 0.025(3) 0.038(3) -0.003(2) 0.017(3) -0.012(3) C33 0.045(5) 0.023(3) 0.039(4) -0.010(3) 0.026(4) -0.007(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 O20 2.013(5) . ? Pd1 O30 2.025(5) . ? Pd1 N11 2.051(6) . ? Pd1 N1 2.084(6) . ? N1 C2 1.492(9) . ? N1 H1A 0.93(3) . ? N1 H1B 0.95(3) . ? C2 C5 1.515(9) . ? C2 C3 1.536(8) . ? C2 H2 1.0000 . ? C3 O4 1.431(8) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? O4 H4 0.8400 . ? C5 C6 1.531(10) . ? C5 C7 1.533(9) . ? C5 H5 1.0000 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? N11 C12 1.507(8) . ? N11 H11A 0.95(3) . ? N11 H11B 0.94(3) . ? C12 C13 1.514(9) . ? C12 C15 1.542(10) . ? C12 H12 1.0000 . ? C13 O14 1.428(8) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? O14 H14 0.8400 . ? C15 C17 1.523(10) . ? C15 C16 1.525(10) . ? C15 H15 1.0000 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? O20 C21 1.328(19) . ? C21 O22 1.226(8) . ? C21 C23 1.513(8) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? O30 C31 1.245(18) . ? C31 O32 1.245(8) . ? C31 C33 1.495(8) . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? 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 O20 Pd1 O30 177.01(16) . . ? O20 Pd1 N11 87.1(2) . . ? O30 Pd1 N11 89.9(2) . . ? O20 Pd1 N1 86.6(2) . . ? O30 Pd1 N1 96.3(2) . . ? N11 Pd1 N1 172.2(2) . . ? C2 N1 Pd1 121.3(4) . . ? C2 N1 H1A 101(6) . . ? Pd1 N1 H1A 107(6) . . ? C2 N1 H1B 105(7) . . ? Pd1 N1 H1B 107(7) . . ? H1A N1 H1B 116(9) . . ? N1 C2 C5 112.1(5) . . ? N1 C2 C3 107.8(5) . . ? C5 C2 C3 113.1(5) . . ? N1 C2 H2 107.9 . . ? C5 C2 H2 107.9 . . ? C3 C2 H2 107.9 . . ? O4 C3 C2 105.7(5) . . ? O4 C3 H3A 110.6 . . ? C2 C3 H3A 110.6 . . ? O4 C3 H3B 110.6 . . ? C2 C3 H3B 110.6 . . ? H3A C3 H3B 108.7 . . ? C3 O4 H4 109.5 . . ? C2 C5 C6 111.6(5) . . ? C2 C5 C7 111.9(5) . . ? C6 C5 C7 108.8(6) . . ? C2 C5 H5 108.1 . . ? C6 C5 H5 108.1 . . ? C7 C5 H5 108.1 . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C5 C7 H7A 109.5 . . ? C5 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C5 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C12 N11 Pd1 110.7(4) . . ? C12 N11 H11A 108(6) . . ? Pd1 N11 H11A 112(6) . . ? C12 N11 H11B 117(6) . . ? Pd1 N11 H11B 112(6) . . ? H11A N11 H11B 96(8) . . ? N11 C12 C13 106.6(5) . . ? N11 C12 C15 111.3(5) . . ? C13 C12 C15 115.7(6) . . ? N11 C12 H12 107.6 . . ? C13 C12 H12 107.6 . . ? C15 C12 H12 107.6 . . ? O14 C13 C12 108.4(5) . . ? O14 C13 H13A 110.0 . . ? C12 C13 H13A 110.0 . . ? O14 C13 H13B 110.0 . . ? C12 C13 H13B 110.0 . . ? H13A C13 H13B 108.4 . . ? C13 O14 H14 109.5 . . ? C17 C15 C16 107.9(6) . . ? C17 C15 C12 112.1(6) . . ? C16 C15 C12 109.5(6) . . ? C17 C15 H15 109.1 . . ? C16 C15 H15 109.1 . . ? C12 C15 H15 109.1 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C21 O20 Pd1 115.4(9) . . ? O22 C21 O20 126.8(7) . . ? O22 C21 C23 120.2(6) . . ? O20 C21 C23 112.9(6) . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C31 O30 Pd1 123.9(9) . . ? O30 C31 O32 124.1(7) . . ? O30 C31 C33 116.0(7) . . ? O32 C31 C33 119.9(6) . . ? C31 C33 H33A 109.5 . . ? C31 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C31 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? 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 O20 Pd1 N1 C2 -107.1(7) . . . . ? O30 Pd1 N1 C2 73.3(6) . . . . ? N11 Pd1 N1 C2 -143.6(19) . . . . ? Pd1 N1 C2 C5 -65.0(6) . . . . ? Pd1 N1 C2 C3 60.1(6) . . . . ? N1 C2 C3 O4 55.9(7) . . . . ? C5 C2 C3 O4 -179.6(5) . . . . ? N1 C2 C5 C6 -62.6(8) . . . . ? C3 C2 C5 C6 175.3(6) . . . . ? N1 C2 C5 C7 175.3(6) . . . . ? C3 C2 C5 C7 53.2(8) . . . . ? O20 Pd1 N11 C12 -65.3(6) . . . . ? O30 Pd1 N11 C12 114.5(6) . . . . ? N1 Pd1 N11 C12 -29(2) . . . . ? Pd1 N11 C12 C13 -76.3(6) . . . . ? Pd1 N11 C12 C15 156.7(4) . . . . ? N11 C12 C13 O14 -63.8(6) . . . . ? C15 C12 C13 O14 60.5(7) . . . . ? N11 C12 C15 C17 -57.3(7) . . . . ? C13 C12 C15 C17 -179.2(6) . . . . ? N11 C12 C15 C16 -177.1(5) . . . . ? C13 C12 C15 C16 61.0(7) . . . . ? O30 Pd1 O20 C21 -80(19) . . . . ? N11 Pd1 O20 C21 -75.3(5) . . . . ? N1 Pd1 O20 C21 109.3(6) . . . . ? Pd1 O20 C21 O22 1.3(10) . . . . ? Pd1 O20 C21 C23 -179.5(5) . . . . ? O20 Pd1 O30 C31 -102(18) . . . . ? N11 Pd1 O30 C31 -106.3(6) . . . . ? N1 Pd1 O30 C31 69.0(6) . . . . ? Pd1 O30 C31 O32 -3.8(11) . . . . ? Pd1 O30 C31 C33 177.6(5) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 24.71 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 3.412 _refine_diff_density_min -1.130 _refine_diff_density_rms 0.264 # Attachment '- Compound3 .cif' data_975_0m _database_code_depnum_ccdc_archive 'CCDC 767180' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H26 Cl2 N2 O2 Pd' _chemical_melting_point ? _exptl_crystal_description ? _exptl_crystal_colour ? _diffrn_ambient_temperature 100(2) _chemical_formula_weight 479.71 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0031 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 0.0109 0.0061 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1495 0.1591 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9739 1.0091 '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 _chemical_absolute_configuration ad loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 6.3630(2) _cell_length_b 9.0651(2) _cell_length_c 34.8315(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2009.12(9) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9926 _cell_measurement_theta_min 2.34 _cell_measurement_theta_max 37.02 _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.586 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 976 _exptl_absorpt_coefficient_mu 1.203 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.624 _exptl_absorpt_correction_T_max 0.887 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_source_type 'KAPPA APEX II ICMMO' _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 57870 _diffrn_reflns_av_R_equivalents 0.0227 _diffrn_reflns_av_sigmaI/netI 0.0178 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -58 _diffrn_reflns_limit_l_max 58 _diffrn_reflns_theta_min 2.32 _diffrn_reflns_theta_max 37.02 _reflns_number_total 9723 _reflns_number_gt 9637 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _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^)+(0.0324P)^2^+2.2078P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.03(2) _refine_ls_number_reflns 9723 _refine_ls_number_parameters 230 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0320 _refine_ls_R_factor_gt 0.0317 _refine_ls_wR_factor_ref 0.0825 _refine_ls_wR_factor_gt 0.0824 _refine_ls_goodness_of_fit_ref 1.310 _refine_ls_restrained_S_all 1.310 _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 Pd1 Pd 0.27387(2) 0.825392(15) 0.228971(4) 0.00947(3) Uani 1 1 d . . . Cl1 Cl 0.54210(8) 0.71137(5) 0.196844(14) 0.01417(8) Uani 1 1 d . . . Cl2 Cl 0.01319(8) 0.95309(5) 0.261225(14) 0.01382(8) Uani 1 1 d . . . N1 N 0.4864(3) 0.87119(18) 0.27138(5) 0.0128(2) Uani 1 1 d . . . H10 H 0.6141 0.8423 0.2632 0.015 Uiso 1 1 calc R . . H11 H 0.4911 0.9697 0.2745 0.015 Uiso 1 1 calc R . . C1 C 0.4485(3) 0.8031(2) 0.30971(5) 0.0120(3) Uani 1 1 d . . . H12 H 0.3203 0.8464 0.3205 0.014 Uiso 1 1 calc R . . C2 C 0.4143(4) 0.6377(2) 0.30531(6) 0.0169(4) Uani 1 1 d . . . H1A H 0.2911 0.6204 0.2901 0.025 Uiso 1 1 calc R . . H1B H 0.3960 0.5939 0.3302 0.025 Uiso 1 1 calc R . . H1C H 0.5341 0.5945 0.2929 0.025 Uiso 1 1 calc R . . C3 C 0.6334(3) 0.8414(2) 0.33649(6) 0.0134(3) Uani 1 1 d . . . H13 H 0.6664 0.9460 0.3328 0.016 Uiso 1 1 calc R . . O1 O 0.8170(3) 0.7583(2) 0.32649(5) 0.0175(3) Uani 1 1 d . . . H14 H 0.8822 0.8019 0.3097 0.026 Uiso 1 1 calc R . . C4 C 0.5907(4) 0.8182(3) 0.37880(6) 0.0161(3) Uani 1 1 d . . . C5 C 0.7568(5) 0.8430(3) 0.40413(6) 0.0263(5) Uani 1 1 d . . . H5 H 0.8879 0.8700 0.3946 0.032 Uiso 1 1 calc R . . C6 C 0.7274(6) 0.8276(4) 0.44357(7) 0.0355(6) Uani 1 1 d . . . H6 H 0.8388 0.8450 0.4602 0.043 Uiso 1 1 calc R . . C7 C 0.5347(7) 0.7867(4) 0.45807(7) 0.0355(7) Uani 1 1 d . . . H7 H 0.5162 0.7760 0.4844 0.043 Uiso 1 1 calc R . . C8 C 0.3697(7) 0.7619(4) 0.43340(8) 0.0374(8) Uani 1 1 d . . . H8 H 0.2398 0.7334 0.4432 0.045 Uiso 1 1 calc R . . C9 C 0.3955(5) 0.7791(4) 0.39367(7) 0.0271(5) Uani 1 1 d . . . H9 H 0.2822 0.7644 0.3772 0.033 Uiso 1 1 calc R . . N2 N 0.0567(3) 0.7729(2) 0.18782(5) 0.0130(3) Uani 1 1 d . . . H20 H -0.0002 0.6860 0.1947 0.016 Uiso 1 1 calc R . . H21 H -0.0464 0.8406 0.1895 0.016 Uiso 1 1 calc R . . C21 C 0.1124(4) 0.7604(2) 0.14625(6) 0.0132(3) Uani 1 1 d . . . H22 H 0.2379 0.6985 0.1438 0.016 Uiso 1 1 calc R . . C22 C -0.0691(4) 0.6869(3) 0.12467(6) 0.0186(4) Uani 1 1 d . . . H22A H -0.1038 0.5952 0.1369 0.028 Uiso 1 1 calc R . . H22B H -0.0278 0.6687 0.0986 0.028 Uiso 1 1 calc R . . H22C H -0.1894 0.7508 0.1250 0.028 Uiso 1 1 calc R . . C23 C 0.1646(3) 0.9162(2) 0.13204(6) 0.0127(3) Uani 1 1 d . . . H23 H 0.2868 0.9524 0.1463 0.015 Uiso 1 1 calc R . . O2 O -0.0094(3) 1.00872(18) 0.14047(5) 0.0174(3) Uani 1 1 d . . . H24 H 0.0327 1.0919 0.1456 0.026 Uiso 1 1 calc R . . C24 C 0.2185(4) 0.9159(2) 0.08965(6) 0.0156(3) Uani 1 1 d . . . C25 C 0.0648(5) 0.9414(3) 0.06198(7) 0.0217(4) Uani 1 1 d . . . H25 H -0.0716 0.9645 0.0695 0.026 Uiso 1 1 calc R . . C26 C 0.1148(6) 0.9324(3) 0.02315(7) 0.0288(6) Uani 1 1 d . . . H26 H 0.0112 0.9484 0.0048 0.035 Uiso 1 1 calc R . . C27 C 0.3180(6) 0.8997(4) 0.01171(8) 0.0336(7) Uani 1 1 d . . . H27 H 0.3508 0.8933 -0.0143 0.040 Uiso 1 1 calc R . . C28 C 0.4716(6) 0.8768(4) 0.03901(8) 0.0342(7) Uani 1 1 d . . . H28 H 0.6086 0.8558 0.0315 0.041 Uiso 1 1 calc R . . C29 C 0.4212(4) 0.8851(3) 0.07794(7) 0.0245(5) Uani 1 1 d . . . H29 H 0.5254 0.8697 0.0962 0.029 Uiso 1 1 calc R . . 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 0.00914(5) 0.01087(5) 0.00840(4) 0.00077(4) -0.00022(4) 0.00009(4) Cl1 0.01163(19) 0.01557(18) 0.01530(18) -0.00228(14) 0.00098(14) 0.00164(14) Cl2 0.01198(19) 0.01687(18) 0.01261(16) -0.00149(13) 0.00105(13) 0.00190(15) N1 0.0135(7) 0.0135(6) 0.0114(6) 0.0014(5) -0.0005(6) -0.0005(5) C1 0.0129(7) 0.0135(8) 0.0096(6) 0.0007(5) -0.0006(5) -0.0001(6) C2 0.0230(10) 0.0145(8) 0.0133(8) 0.0015(6) -0.0024(7) -0.0026(7) C3 0.0144(8) 0.0141(8) 0.0116(6) 0.0018(6) -0.0014(5) -0.0003(6) O1 0.0137(7) 0.0229(7) 0.0161(6) 0.0063(5) 0.0013(5) 0.0032(5) C4 0.0231(9) 0.0149(7) 0.0104(6) 0.0005(6) -0.0014(6) -0.0010(8) C5 0.0310(13) 0.0333(12) 0.0147(8) 0.0011(8) -0.0072(8) -0.0001(11) C6 0.0520(18) 0.0411(14) 0.0135(8) 0.0010(9) -0.0102(10) 0.0045(18) C7 0.065(2) 0.0305(13) 0.0105(8) 0.0011(8) 0.0047(11) 0.0017(14) C8 0.055(2) 0.0408(17) 0.0170(10) -0.0003(11) 0.0147(12) -0.0100(15) C9 0.0321(14) 0.0360(13) 0.0132(9) -0.0029(9) 0.0049(8) -0.0073(11) N2 0.0122(7) 0.0157(7) 0.0111(6) 0.0003(5) 0.0005(5) -0.0007(5) C21 0.0146(8) 0.0144(8) 0.0106(7) -0.0008(6) 0.0006(6) 0.0006(6) C22 0.0215(10) 0.0184(9) 0.0160(8) -0.0028(7) -0.0025(7) -0.0056(8) C23 0.0134(8) 0.0138(7) 0.0110(7) -0.0005(6) -0.0003(6) 0.0006(6) O2 0.0177(7) 0.0151(6) 0.0195(7) -0.0030(5) 0.0015(6) 0.0025(5) C24 0.0173(9) 0.0176(8) 0.0118(7) 0.0001(6) -0.0005(7) -0.0003(7) C25 0.0273(12) 0.0246(10) 0.0133(8) 0.0015(7) -0.0059(8) 0.0014(9) C26 0.0433(17) 0.0309(13) 0.0121(9) 0.0011(9) -0.0061(9) -0.0023(12) C27 0.049(2) 0.0390(15) 0.0130(9) -0.0016(9) 0.0054(10) -0.0105(13) C28 0.0306(15) 0.0521(18) 0.0200(11) -0.0075(11) 0.0103(10) -0.0038(13) C29 0.0197(11) 0.0370(13) 0.0168(9) -0.0024(9) 0.0024(8) 0.0016(9) _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 Pd1 N1 2.0455(18) . ? Pd1 N2 2.0469(18) . ? Pd1 Cl1 2.2877(5) . ? Pd1 Cl2 2.3138(5) . ? N1 C1 1.490(3) . ? C1 C2 1.523(3) . ? C1 C3 1.541(3) . ? C3 O1 1.433(3) . ? C3 C4 1.513(3) . ? C4 C9 1.392(4) . ? C4 C5 1.395(3) . ? C5 C6 1.393(3) . ? C6 C7 1.377(6) . ? C7 C8 1.375(6) . ? C8 C9 1.402(4) . ? N2 C21 1.495(3) . ? C21 C22 1.530(3) . ? C21 C23 1.533(3) . ? C23 O2 1.420(3) . ? C23 C24 1.516(3) . ? C24 C29 1.381(4) . ? C24 C25 1.392(3) . ? C25 C26 1.392(4) . ? C26 C27 1.385(5) . ? C27 C28 1.379(5) . ? C28 C29 1.395(4) . ? 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 N1 Pd1 N2 177.75(7) . . ? N1 Pd1 Cl1 87.23(5) . . ? N2 Pd1 Cl1 93.22(5) . . ? N1 Pd1 Cl2 91.25(5) . . ? N2 Pd1 Cl2 88.41(5) . . ? Cl1 Pd1 Cl2 176.75(2) . . ? C1 N1 Pd1 117.12(12) . . ? N1 C1 C2 109.90(16) . . ? N1 C1 C3 109.00(16) . . ? C2 C1 C3 113.08(17) . . ? O1 C3 C4 108.04(17) . . ? O1 C3 C1 110.89(17) . . ? C4 C3 C1 114.93(17) . . ? C9 C4 C5 118.8(2) . . ? C9 C4 C3 123.9(2) . . ? C5 C4 C3 117.2(2) . . ? C6 C5 C4 120.3(3) . . ? C7 C6 C5 120.6(3) . . ? C8 C7 C6 119.7(2) . . ? C7 C8 C9 120.6(3) . . ? C4 C9 C8 120.0(3) . . ? C21 N2 Pd1 122.40(14) . . ? N2 C21 C22 109.27(17) . . ? N2 C21 C23 107.12(16) . . ? C22 C21 C23 113.95(18) . . ? O2 C23 C24 112.27(17) . . ? O2 C23 C21 107.95(17) . . ? C24 C23 C21 111.23(16) . . ? C29 C24 C25 119.0(2) . . ? C29 C24 C23 120.0(2) . . ? C25 C24 C23 121.0(2) . . ? C26 C25 C24 120.2(3) . . ? C27 C26 C25 120.3(3) . . ? C28 C27 C26 119.7(2) . . ? C27 C28 C29 119.9(3) . . ? C24 C29 C28 120.8(3) . . ? _diffrn_measured_fraction_theta_max 0.956 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.916 _refine_diff_density_min -2.717 _refine_diff_density_rms 0.143