# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_publ_section_ _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _publ_contact_author_name 'Ingo-Peter Lorenz' _publ_contact_author_address ; Department Chemie Ludwig-Maximilians Universitaet Butenandtstrasse 5-13 (Haus D) D-81377 Muenchen Bundesrepublik Deutschland ; _publ_contact_author_email ipl@cup.uni-muenchen.de _publ_contact_author_phone 'Int+ 089-2180-77486' _publ_contact_author_fax 'Int+ 089-2180-77867' loop_ _publ_author_name _publ_author_address I.-P.Lorenz ; Department of Cosmetic Raw Materials Chemistry Faculty of Pharmacy Medical University of Lodz Muszynski Str. 1 90-151 Lodz, Poland ; S.Wirth ; Department Chemie Ludwig-Maximilians Universitaet Butenandtstrasse 5-13 (Haus D) D-81377 Muenchen Bundesrepublik Deutschland ; E.Budzisz ; Department Chemie Ludwig-Maximilians Universitaet Butenandtstrasse 5-13 (Haus D) D-81377 Muenchen Bundesrepublik Deutschland ; _publ_section_title ; Synthesis, structural characterization, and antimicrobial and cytotoxic effects of aziridine, 2-aminoethylaziridine and azirine complexes of copper(II) and palladium(II) ; _publ_section_abstract ? _publ_section_comment ? data_1a_CCDC-000000 _database_code_depnum_ccdc_archive 'CCDC 849020' #TrackingRef 'DTrans. aziridine.cif' # CCDC: 000000 # Messcode: lo087a _audit_author_name 'S. Wirth, S. Albrecht' _audit_block_code ? _audit_creation_method SHELXL-97 _audit_creation_date 21-Jun-07 _chemical_name_systematic ; Chlorido-(2,2-dimethylaziridine)-[2-{1-(dimethylaminoethyl} phenyl-C,N]-palladium(II) ; _chemical_name_common ? _chemical_formula_moiety 'C14 H23 Cl N2 Pd' _chemical_formula_sum 'C14 H23 Cl N2 Pd' _chemical_compound_source ? _exptl_crystal_recrystallization_method 'slow isothermic diffusion of n-pentane into a solution in dichloromethane' _exptl_crystal_description block _exptl_crystal_colour yellow _diffrn_ambient_temperature 200(2) _chemical_formula_weight 361.22 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 '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 'P 21' _symmetry_Int_Tables_number 4 _chemical_absolute_configuration ad _symmetry_space_group_name_Hall P2yb loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 10.7546(5) _cell_length_b 26.4634(11) _cell_length_c 11.0319(4) _cell_angle_alpha 90.00 _cell_angle_beta 92.912(3) _cell_angle_gamma 90.00 _cell_volume 3135.6(2) _cell_formula_units_Z 8 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 3.7635 _cell_measurement_theta_max 27.4996 _cell_special_details ? _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.53036 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1472 _exptl_absorpt_coefficient_mu 1.340 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ? loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist ? ? ? ? _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed X-ray tube' _diffrn_source_type 'Enhance (Mo) X-ray Source' _diffrn_source_power 2.00 _diffrn_source_voltage 50 _diffrn_source_current 40 _diffrn_radiation_monochromator graphite _diffrn_radiation_collimation '0.5 mm collimator' _diffrn_measurement_device 'Oxford Diffraction XCalibur' _diffrn_measurement_device_type 'Sapphire CCD detector' _diffrn_measurement_method omega-scan _diffrn_detector_area_resol_mean 15.9809 _kl_diffrn_measurement_scan_angle ? _kl_diffrn_measurement_scan_step_degree ? _kl_diffrn_measurement_scan_time_per_degree ? _kl_diffrn_measurement_detector_distance 50 _diffrn_special_details ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18229 _diffrn_reflns_av_R_equivalents 0.0295 _diffrn_reflns_av_sigmaI/netI 0.0340 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -34 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.78 _diffrn_reflns_theta_max 27.62 _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.62 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.483 _refine_diff_density_min -0.550 _refine_diff_density_rms 0.073 _reflns_number_total 10459 _reflns_number_gt 9832 _reflns_threshold_expression >2sigma(I) _reflns_special_details ? _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET) (compiled Oct 18 2006,16:28:17) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET) (compiled Oct 18 2006,16:28:17) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET) (compiled Oct 18 2006,16:28:17) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; Ortep-3 for Windows: L. J. Farrugia, J. Appl. Cryst. 1997, 30, 565 ; _computing_publication_material ? _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^)+(0.0291P)^2^+0.0000P] 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 -0.021(14) _refine_ls_number_reflns 10459 _refine_ls_number_parameters 649 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0247 _refine_ls_R_factor_gt 0.0221 _refine_ls_wR_factor_ref 0.0504 _refine_ls_wR_factor_gt 0.0494 _refine_ls_goodness_of_fit_ref 1.001 _refine_ls_restrained_S_all 1.001 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _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. ; 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 -0.02295(2) 0.018419(9) 0.213611(19) 0.01349(5) Uani 1 1 d . . . Pd2 Pd 0.53941(2) 0.197158(9) 0.77103(2) 0.01577(5) Uani 1 1 d . . . Pd3 Pd 0.52857(2) 0.274201(9) 0.07709(2) 0.01585(5) Uani 1 1 d . . . Pd4 Pd -0.02465(2) 0.464742(9) 0.458663(19) 0.01407(5) Uani 1 1 d . . . Cl1 Cl -0.24223(7) -0.00106(3) 0.23212(6) 0.01838(15) Uani 1 1 d . . . Cl2 Cl 0.47856(7) 0.27408(3) 0.66306(7) 0.02261(16) Uani 1 1 d . . . Cl3 Cl 0.75160(7) 0.25608(3) 0.09926(7) 0.02313(17) Uani 1 1 d . . . Cl4 Cl -0.08950(7) 0.55115(3) 0.40591(6) 0.01855(15) Uani 1 1 d . . . N1 N -0.0338(2) 0.07942(11) 0.3267(2) 0.0174(6) Uani 1 1 d . . . H1 H 0.0025 0.0732 0.4036 0.021 Uiso 1 1 calc R . . N2 N 0.0115(2) -0.03909(11) 0.0887(2) 0.0167(5) Uani 1 1 d . . . N3 N 0.7156(2) 0.22417(11) 0.8131(2) 0.0177(6) Uani 1 1 d . . . H3 H 0.7314 0.2267 0.8965 0.021 Uiso 1 1 calc R . . N4 N 0.3692(3) 0.15889(11) 0.7429(2) 0.0201(6) Uani 1 1 d . . . N5 N 0.5497(2) 0.31985(10) -0.0704(2) 0.0162(5) Uani 1 1 d . . . H5 H 0.5237 0.3045 -0.1433 0.019 Uiso 1 1 calc R . . N6 N 0.4798(3) 0.23495(12) 0.2333(2) 0.0237(6) Uani 1 1 d . . . N7 N 0.1564(2) 0.48761(11) 0.4876(2) 0.0175(6) Uani 1 1 d . . . H7 H 0.1796 0.4894 0.5699 0.021 Uiso 1 1 calc R . . N8 N -0.2015(2) 0.43121(11) 0.4279(2) 0.0179(6) Uani 1 1 d . . . C1 C -0.0224(3) 0.13349(13) 0.2897(3) 0.0193(7) Uani 1 1 d . . . C2 C -0.1421(3) 0.11395(14) 0.3297(3) 0.0230(7) Uani 1 1 d . . . H2A H -0.2106 0.1093 0.2673 0.028 Uiso 1 1 calc R . . H2B H -0.1690 0.1248 0.4102 0.028 Uiso 1 1 calc R . . C3 C 0.0572(3) 0.16660(14) 0.3755(3) 0.0245(7) Uani 1 1 d . . . H3A H 0.0351 0.2022 0.3618 0.037 Uiso 1 1 calc R . . H3B H 0.1453 0.1615 0.3603 0.037 Uiso 1 1 calc R . . H3C H 0.0424 0.1574 0.4596 0.037 Uiso 1 1 calc R . . C4 C -0.0063(4) 0.14325(15) 0.1570(3) 0.0270(8) Uani 1 1 d . . . H4A H -0.0594 0.1201 0.1082 0.041 Uiso 1 1 calc R . . H4B H 0.0809 0.1378 0.1387 0.041 Uiso 1 1 calc R . . H4C H -0.0300 0.1782 0.1375 0.041 Uiso 1 1 calc R . . C5 C 0.1583(3) 0.02931(13) 0.2005(3) 0.0180(7) Uani 1 1 d . . . C6 C 0.2423(3) 0.05253(13) 0.2844(3) 0.0193(7) Uani 1 1 d . . . H6 H 0.2130 0.0669 0.3566 0.023 Uiso 1 1 calc R . . C7 C 0.3697(3) 0.05467(14) 0.2620(3) 0.0221(7) Uani 1 1 d . . . H7B H 0.4264 0.0693 0.3209 0.026 Uiso 1 1 calc R . . C8 C 0.4137(3) 0.03573(15) 0.1550(3) 0.0271(8) Uani 1 1 d . . . H8 H 0.4991 0.0391 0.1381 0.033 Uiso 1 1 calc R . . C9 C 0.3303(3) 0.01163(15) 0.0724(3) 0.0255(8) Uani 1 1 d . . . H9 H 0.3596 -0.0025 -0.0001 0.031 Uiso 1 1 calc R . . C10 C 0.2045(3) 0.00819(13) 0.0958(3) 0.0194(7) Uani 1 1 d . . . C11 C 0.1106(3) -0.01768(13) 0.0099(3) 0.0203(7) Uani 1 1 d . . . H11 H 0.1523 -0.0461 -0.0319 0.024 Uiso 1 1 calc R . . C12 C 0.0579(3) 0.01952(16) -0.0849(3) 0.0271(8) Uani 1 1 d . . . H12A H 0.0124 0.0463 -0.0447 0.041 Uiso 1 1 calc R . . H12B H 0.0012 0.0017 -0.1427 0.041 Uiso 1 1 calc R . . H12C H 0.1262 0.0345 -0.1282 0.041 Uiso 1 1 calc R . . C13 C -0.0991(3) -0.05642(14) 0.0133(3) 0.0218(7) Uani 1 1 d . . . H13A H -0.0752 -0.0847 -0.0380 0.033 Uiso 1 1 calc R . . H13B H -0.1305 -0.0285 -0.0380 0.033 Uiso 1 1 calc R . . H13C H -0.1642 -0.0675 0.0664 0.033 Uiso 1 1 calc R . . C14 C 0.0626(3) -0.08361(13) 0.1552(3) 0.0200(7) Uani 1 1 d . . . H14A H 0.0033 -0.0949 0.2140 0.030 Uiso 1 1 calc R . . H14B H 0.1415 -0.0745 0.1980 0.030 Uiso 1 1 calc R . . H14C H 0.0770 -0.1109 0.0976 0.030 Uiso 1 1 calc R . . C15 C 0.8297(3) 0.20917(14) 0.7498(3) 0.0234(7) Uani 1 1 d . . . C16 C 0.7878(3) 0.26227(14) 0.7462(3) 0.0253(7) Uani 1 1 d . . . H16A H 0.7504 0.2753 0.6685 0.030 Uiso 1 1 calc R . . H16B H 0.8376 0.2872 0.7947 0.030 Uiso 1 1 calc R . . C17 C 0.9432(3) 0.19498(16) 0.8290(3) 0.0286(8) Uani 1 1 d . . . H17A H 1.0184 0.2008 0.7843 0.043 Uiso 1 1 calc R . . H17B H 0.9384 0.1592 0.8512 0.043 Uiso 1 1 calc R . . H17C H 0.9464 0.2157 0.9026 0.043 Uiso 1 1 calc R . . C18 C 0.8059(4) 0.17717(18) 0.6378(3) 0.0360(10) Uani 1 1 d . . . H18A H 0.7255 0.1865 0.5982 0.054 Uiso 1 1 calc R . . H18B H 0.8045 0.1414 0.6609 0.054 Uiso 1 1 calc R . . H18C H 0.8722 0.1828 0.5817 0.054 Uiso 1 1 calc R . . C19 C 0.5877(3) 0.13119(13) 0.8429(3) 0.0169(6) Uani 1 1 d . . . C20 C 0.6834(3) 0.12039(13) 0.9293(3) 0.0195(7) Uani 1 1 d . . . H20 H 0.7336 0.1469 0.9631 0.023 Uiso 1 1 calc R . . C21 C 0.7051(3) 0.07088(14) 0.9658(3) 0.0230(7) Uani 1 1 d . . . H21 H 0.7708 0.0638 1.0242 0.028 Uiso 1 1 calc R . . C22 C 0.6334(3) 0.03184(13) 0.9190(3) 0.0213(7) Uani 1 1 d . . . H22 H 0.6502 -0.0019 0.9445 0.026 Uiso 1 1 calc R . . C23 C 0.5359(3) 0.04168(13) 0.8340(3) 0.0185(6) Uani 1 1 d . . . H23 H 0.4864 0.0148 0.8011 0.022 Uiso 1 1 calc R . . C24 C 0.5119(3) 0.09081(13) 0.7982(3) 0.0168(6) Uani 1 1 d . . . C25 C 0.4054(3) 0.10548(13) 0.7101(3) 0.0194(7) Uani 1 1 d . . . H25 H 0.3333 0.0824 0.7214 0.023 Uiso 1 1 calc R . . C26 C 0.4449(3) 0.10152(16) 0.5785(3) 0.0276(8) Uani 1 1 d . . . H26A H 0.3725 0.1075 0.5227 0.041 Uiso 1 1 calc R . . H26B H 0.4783 0.0677 0.5644 0.041 Uiso 1 1 calc R . . H26C H 0.5090 0.1269 0.5644 0.041 Uiso 1 1 calc R . . C27 C 0.2799(3) 0.18054(15) 0.6505(3) 0.0280(8) Uani 1 1 d . . . H27A H 0.2123 0.1564 0.6328 0.042 Uiso 1 1 calc R . . H27B H 0.3228 0.1875 0.5760 0.042 Uiso 1 1 calc R . . H27C H 0.2454 0.2120 0.6813 0.042 Uiso 1 1 calc R . . C28 C 0.3040(3) 0.15658(15) 0.8586(3) 0.0249(8) Uani 1 1 d . . . H28A H 0.2834 0.1909 0.8843 0.037 Uiso 1 1 calc R . . H28B H 0.3583 0.1405 0.9214 0.037 Uiso 1 1 calc R . . H28C H 0.2273 0.1368 0.8464 0.037 Uiso 1 1 calc R . . C29 C 0.5273(3) 0.37539(13) -0.0703(3) 0.0205(7) Uani 1 1 d . . . C30 C 0.6552(3) 0.35500(14) -0.0834(3) 0.0214(7) Uani 1 1 d . . . H30A H 0.6911 0.3576 -0.1640 0.026 Uiso 1 1 calc R . . H30B H 0.7160 0.3586 -0.0135 0.026 Uiso 1 1 calc R . . C31 C 0.4937(4) 0.39662(16) 0.0505(3) 0.0324(9) Uani 1 1 d . . . H31A H 0.5406 0.3788 0.1159 0.049 Uiso 1 1 calc R . . H31B H 0.4043 0.3922 0.0603 0.049 Uiso 1 1 calc R . . H31C H 0.5144 0.4327 0.0540 0.049 Uiso 1 1 calc R . . C32 C 0.4586(4) 0.39717(15) -0.1801(3) 0.0309(8) Uani 1 1 d . . . H32A H 0.4874 0.4318 -0.1934 0.046 Uiso 1 1 calc R . . H32B H 0.3691 0.3975 -0.1672 0.046 Uiso 1 1 calc R . . H32C H 0.4744 0.3764 -0.2513 0.046 Uiso 1 1 calc R . . C33 C 0.3461(3) 0.28387(12) 0.0613(3) 0.0194(7) Uani 1 1 d . . . C34 C 0.2737(3) 0.29564(13) -0.0444(3) 0.0215(7) Uani 1 1 d . . . H34 H 0.3131 0.3007 -0.1185 0.026 Uiso 1 1 calc R . . C35 C 0.1446(3) 0.29990(15) -0.0417(4) 0.0281(8) Uani 1 1 d . . . H35 H 0.0967 0.3076 -0.1141 0.034 Uiso 1 1 calc R . . C36 C 0.0862(3) 0.29302(16) 0.0655(4) 0.0334(9) Uani 1 1 d . . . H36 H -0.0014 0.2971 0.0679 0.040 Uiso 1 1 calc R . . C37 C 0.1567(3) 0.28005(16) 0.1703(4) 0.0338(9) Uani 1 1 d . . . H37 H 0.1165 0.2740 0.2437 0.041 Uiso 1 1 calc R . . C38 C 0.2853(3) 0.27584(15) 0.1685(3) 0.0266(7) Uani 1 1 d . . . C39 C 0.3690(4) 0.26302(15) 0.2793(3) 0.0309(9) Uani 1 1 d . . . H39 H 0.3230 0.2403 0.3340 0.037 Uiso 1 1 calc R . . C40 C 0.4049(4) 0.31100(17) 0.3471(3) 0.0400(11) Uani 1 1 d . . . H40A H 0.4567 0.3025 0.4199 0.060 Uiso 1 1 calc R . . H40B H 0.3296 0.3285 0.3707 0.060 Uiso 1 1 calc R . . H40C H 0.4518 0.3330 0.2945 0.060 Uiso 1 1 calc R . . C41 C 0.5806(4) 0.23029(18) 0.3290(3) 0.0383(10) Uani 1 1 d . . . H41A H 0.5454 0.2191 0.4048 0.057 Uiso 1 1 calc R . . H41B H 0.6212 0.2632 0.3418 0.057 Uiso 1 1 calc R . . H41C H 0.6419 0.2055 0.3039 0.057 Uiso 1 1 calc R . . C42 C 0.4401(4) 0.18277(15) 0.1977(4) 0.0337(9) Uani 1 1 d . . . H42A H 0.5082 0.1656 0.1588 0.051 Uiso 1 1 calc R . . H42B H 0.3672 0.1845 0.1408 0.051 Uiso 1 1 calc R . . H42C H 0.4186 0.1639 0.2702 0.051 Uiso 1 1 calc R . . C43 C 0.2635(3) 0.47309(14) 0.4133(3) 0.0208(7) Uani 1 1 d . . . C44 C 0.2207(3) 0.52625(14) 0.4168(3) 0.0246(7) Uani 1 1 d . . . H44A H 0.2744 0.5509 0.4621 0.030 Uiso 1 1 calc R . . H44B H 0.1759 0.5399 0.3433 0.030 Uiso 1 1 calc R . . C45 C 0.3835(3) 0.45862(16) 0.4823(3) 0.0255(8) Uani 1 1 d . . . H45A H 0.4531 0.4617 0.4288 0.038 Uiso 1 1 calc R . . H45B H 0.3777 0.4236 0.5107 0.038 Uiso 1 1 calc R . . H45C H 0.3973 0.4812 0.5522 0.038 Uiso 1 1 calc R . . C46 C 0.2292(3) 0.44196(15) 0.3027(3) 0.0252(8) Uani 1 1 d . . . H46A H 0.1502 0.4542 0.2653 0.038 Uiso 1 1 calc R . . H46B H 0.2204 0.4065 0.3263 0.038 Uiso 1 1 calc R . . H46C H 0.2947 0.4449 0.2445 0.038 Uiso 1 1 calc R . . C47 C 0.0205(3) 0.39426(13) 0.5030(3) 0.0172(6) Uani 1 1 d . . . C48 C 0.1246(3) 0.37701(13) 0.5740(3) 0.0202(7) Uani 1 1 d . . . H48 H 0.1843 0.4005 0.6060 0.024 Uiso 1 1 calc R . . C49 C 0.1402(3) 0.32568(14) 0.5974(3) 0.0230(7) Uani 1 1 d . . . H49 H 0.2116 0.3144 0.6441 0.028 Uiso 1 1 calc R . . C50 C 0.0528(3) 0.29058(15) 0.5532(3) 0.0272(8) Uani 1 1 d . . . H50 H 0.0647 0.2556 0.5694 0.033 Uiso 1 1 calc R . . C51 C -0.0519(3) 0.30695(14) 0.4855(3) 0.0249(7) Uani 1 1 d . . . H51 H -0.1125 0.2832 0.4564 0.030 Uiso 1 1 calc R . . C52 C -0.0684(3) 0.35823(13) 0.4601(3) 0.0175(6) Uani 1 1 d . . . C53 C -0.1758(3) 0.37854(13) 0.3823(3) 0.0182(6) Uani 1 1 d . . . H53 H -0.2506 0.3568 0.3926 0.022 Uiso 1 1 calc R . . C54 C -0.1436(3) 0.37831(15) 0.2483(3) 0.0254(8) Uani 1 1 d . . . H54A H -0.0774 0.4029 0.2359 0.038 Uiso 1 1 calc R . . H54B H -0.2177 0.3873 0.1975 0.038 Uiso 1 1 calc R . . H54C H -0.1151 0.3445 0.2260 0.038 Uiso 1 1 calc R . . C55 C -0.2865(3) 0.45962(15) 0.3426(3) 0.0226(7) Uani 1 1 d . . . H55A H -0.3607 0.4392 0.3225 0.034 Uiso 1 1 calc R . . H55B H -0.2437 0.4671 0.2684 0.034 Uiso 1 1 calc R . . H55C H -0.3111 0.4913 0.3807 0.034 Uiso 1 1 calc R . . C56 C -0.2627(3) 0.42666(14) 0.5455(3) 0.0223(7) Uani 1 1 d . . . H56A H -0.2683 0.4601 0.5829 0.033 Uiso 1 1 calc R . . H56B H -0.2136 0.4042 0.5998 0.033 Uiso 1 1 calc R . . H56C H -0.3466 0.4127 0.5311 0.033 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 0.01303(10) 0.01552(12) 0.01192(10) -0.00120(9) 0.00051(8) 0.00015(10) Pd2 0.01469(11) 0.01628(12) 0.01604(11) 0.00018(9) -0.00213(8) 0.00033(10) Pd3 0.01580(11) 0.01580(12) 0.01604(11) 0.00046(10) 0.00172(8) 0.00064(10) Pd4 0.01253(11) 0.01588(12) 0.01368(10) -0.00076(9) -0.00065(8) 0.00135(9) Cl1 0.0144(3) 0.0235(4) 0.0171(3) 0.0009(3) -0.0003(3) -0.0021(3) Cl2 0.0278(4) 0.0210(4) 0.0186(3) 0.0020(3) -0.0030(3) 0.0033(4) Cl3 0.0178(4) 0.0260(5) 0.0252(4) -0.0032(3) -0.0029(3) 0.0023(3) Cl4 0.0205(4) 0.0175(4) 0.0174(3) -0.0003(3) -0.0021(3) 0.0027(3) N1 0.0156(13) 0.0186(15) 0.0178(12) -0.0028(11) 0.0006(10) -0.0010(11) N2 0.0156(12) 0.0205(15) 0.0139(11) 0.0021(11) -0.0023(9) -0.0044(12) N3 0.0164(12) 0.0178(15) 0.0190(12) 0.0006(11) 0.0029(10) -0.0011(11) N4 0.0194(14) 0.0178(15) 0.0225(13) -0.0018(11) -0.0033(11) 0.0010(12) N5 0.0170(13) 0.0144(14) 0.0173(12) 0.0006(10) 0.0014(10) -0.0022(11) N6 0.0288(16) 0.0218(16) 0.0210(14) 0.0063(12) 0.0068(12) 0.0016(13) N7 0.0154(13) 0.0200(15) 0.0170(12) -0.0041(11) 0.0005(10) 0.0011(11) N8 0.0150(13) 0.0205(15) 0.0178(13) -0.0017(11) -0.0029(10) 0.0004(11) C1 0.0211(16) 0.0170(17) 0.0198(15) -0.0024(13) 0.0013(12) 0.0004(14) C2 0.0173(16) 0.0239(19) 0.0281(17) -0.0077(14) 0.0036(13) 0.0029(14) C3 0.0303(18) 0.0197(18) 0.0237(17) -0.0043(14) 0.0026(14) -0.0031(15) C4 0.038(2) 0.0202(19) 0.0222(16) 0.0027(14) -0.0017(15) -0.0035(16) C5 0.0191(15) 0.0180(18) 0.0171(14) 0.0005(12) 0.0016(12) 0.0014(13) C6 0.0190(15) 0.0208(18) 0.0180(14) 0.0006(13) 0.0003(12) -0.0013(14) C7 0.0181(16) 0.0213(18) 0.0266(16) -0.0028(14) -0.0010(13) -0.0008(14) C8 0.0140(15) 0.032(2) 0.0360(19) -0.0038(16) 0.0077(14) -0.0029(15) C9 0.0240(17) 0.029(2) 0.0239(16) -0.0055(15) 0.0111(13) -0.0018(15) C10 0.0226(16) 0.0197(18) 0.0161(14) 0.0001(13) 0.0025(12) 0.0009(14) C11 0.0223(16) 0.0219(18) 0.0174(15) -0.0011(13) 0.0067(12) -0.0037(14) C12 0.0313(18) 0.030(2) 0.0204(15) -0.0009(16) 0.0002(13) -0.0036(18) C13 0.0234(16) 0.0215(18) 0.0200(15) -0.0054(13) -0.0034(13) -0.0010(14) C14 0.0227(16) 0.0170(17) 0.0202(15) -0.0015(13) 0.0012(13) -0.0001(14) C15 0.0185(15) 0.025(2) 0.0271(16) -0.0054(14) 0.0076(13) -0.0028(14) C16 0.0213(16) 0.023(2) 0.0324(18) 0.0013(15) 0.0062(14) -0.0052(15) C17 0.0165(15) 0.032(2) 0.0368(18) -0.0011(17) 0.0023(13) -0.0004(16) C18 0.033(2) 0.047(3) 0.0295(19) -0.0166(18) 0.0109(16) -0.0052(19) C19 0.0144(14) 0.0170(17) 0.0193(14) 0.0009(13) 0.0016(11) 0.0006(13) C20 0.0185(15) 0.0181(17) 0.0212(15) -0.0002(13) -0.0041(12) -0.0057(13) C21 0.0194(16) 0.027(2) 0.0225(16) 0.0056(14) -0.0040(13) 0.0013(15) C22 0.0176(15) 0.0187(18) 0.0277(16) 0.0059(13) 0.0020(13) 0.0012(13) C23 0.0176(15) 0.0171(17) 0.0208(15) -0.0017(13) 0.0015(12) -0.0020(13) C24 0.0133(14) 0.0205(17) 0.0169(14) 0.0002(13) 0.0025(11) -0.0019(13) C25 0.0179(15) 0.0157(17) 0.0241(16) -0.0004(13) -0.0042(12) 0.0010(13) C26 0.0261(18) 0.035(2) 0.0210(16) -0.0047(15) -0.0043(14) 0.0016(16) C27 0.0227(17) 0.025(2) 0.0345(19) 0.0020(15) -0.0131(15) 0.0020(15) C28 0.0150(15) 0.027(2) 0.0329(18) -0.0053(15) 0.0030(13) 0.0026(14) C29 0.0211(16) 0.0142(17) 0.0267(17) 0.0021(13) 0.0065(13) -0.0015(14) C30 0.0216(16) 0.0201(18) 0.0229(16) -0.0012(14) 0.0043(13) -0.0053(14) C31 0.039(2) 0.022(2) 0.037(2) -0.0049(16) 0.0125(17) -0.0005(17) C32 0.034(2) 0.0210(19) 0.037(2) 0.0073(16) -0.0008(16) 0.0029(16) C33 0.0199(15) 0.0111(17) 0.0274(16) 0.0019(13) 0.0036(12) 0.0004(13) C34 0.0194(16) 0.0183(18) 0.0268(16) -0.0027(14) 0.0014(13) -0.0018(14) C35 0.0190(16) 0.022(2) 0.043(2) -0.0010(16) -0.0018(15) -0.0018(15) C36 0.0183(17) 0.031(2) 0.052(2) -0.0007(18) 0.0106(16) -0.0004(16) C37 0.0285(18) 0.030(2) 0.045(2) 0.0093(18) 0.0188(16) 0.0020(17) C38 0.0274(17) 0.0217(18) 0.0314(17) 0.0043(16) 0.0095(14) 0.0020(16) C39 0.038(2) 0.029(2) 0.0262(18) 0.0095(15) 0.0136(15) 0.0035(17) C40 0.060(3) 0.040(3) 0.0195(17) 0.0013(17) 0.0058(18) 0.018(2) C41 0.047(2) 0.043(3) 0.0251(18) 0.0105(18) 0.0011(17) 0.008(2) C42 0.040(2) 0.019(2) 0.042(2) 0.0062(16) 0.0072(18) 0.0031(17) C43 0.0156(14) 0.029(2) 0.0188(14) 0.0007(14) 0.0077(12) -0.0002(14) C44 0.0176(15) 0.026(2) 0.0307(17) 0.0021(15) 0.0048(13) -0.0033(15) C45 0.0146(15) 0.036(2) 0.0263(16) 0.0034(16) 0.0039(12) 0.0040(16) C46 0.0267(17) 0.030(2) 0.0197(15) -0.0035(14) 0.0068(13) 0.0019(16) C47 0.0168(15) 0.0183(17) 0.0166(14) -0.0023(12) 0.0026(12) -0.0017(13) C48 0.0193(16) 0.0221(19) 0.0189(15) -0.0003(13) -0.0024(12) 0.0023(14) C49 0.0235(17) 0.0232(19) 0.0221(16) 0.0016(14) -0.0002(13) 0.0057(15) C50 0.0302(18) 0.0211(19) 0.0299(18) 0.0015(15) -0.0017(14) 0.0038(15) C51 0.0283(18) 0.0218(19) 0.0242(16) 0.0004(14) -0.0014(14) -0.0023(15) C52 0.0177(15) 0.0187(17) 0.0161(14) -0.0011(12) 0.0021(12) -0.0010(13) C53 0.0171(15) 0.0163(17) 0.0208(15) -0.0036(13) -0.0021(12) -0.0008(13) C54 0.0287(18) 0.031(2) 0.0163(15) -0.0045(14) -0.0034(13) 0.0028(16) C55 0.0156(14) 0.0271(19) 0.0245(16) 0.0030(15) -0.0044(12) 0.0029(15) C56 0.0163(15) 0.029(2) 0.0221(16) -0.0027(14) 0.0020(13) -0.0013(14) 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 C5 1.983(3) . ? Pd1 N1 2.047(3) . ? Pd1 N2 2.099(3) . ? Pd1 Cl1 2.4326(8) . ? Pd2 C19 1.976(3) . ? Pd2 N3 2.056(3) . ? Pd2 N4 2.101(3) . ? Pd2 Cl2 2.4314(9) . ? Pd3 C33 1.978(3) . ? Pd3 N5 2.049(3) . ? Pd3 N6 2.101(3) . ? Pd3 Cl3 2.4460(8) . ? Pd4 C47 1.982(3) . ? Pd4 N7 2.049(3) . ? Pd4 N8 2.111(3) . ? Pd4 Cl4 2.4522(8) . ? N1 C2 1.483(4) . ? N1 C1 1.495(4) . ? N1 H1 0.9300 . ? N2 C14 1.479(4) . ? N2 C13 1.488(4) . ? N2 C11 1.518(4) . ? N3 C16 1.491(4) . ? N3 C15 1.495(4) . ? N3 H3 0.9300 . ? N4 C27 1.480(4) . ? N4 C28 1.489(4) . ? N4 C25 1.515(4) . ? N5 C30 1.480(4) . ? N5 C29 1.490(4) . ? N5 H5 0.9300 . ? N6 C41 1.480(5) . ? N6 C42 1.492(5) . ? N6 C39 1.514(5) . ? N7 C44 1.479(4) . ? N7 C43 1.497(4) . ? N7 H7 0.9300 . ? N8 C55 1.482(4) . ? N8 C56 1.489(4) . ? N8 C53 1.512(4) . ? C1 C2 1.476(5) . ? C1 C4 1.506(4) . ? C1 C3 1.521(5) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 C10 1.397(4) . ? C5 C6 1.402(4) . ? C6 C7 1.406(4) . ? C6 H6 0.9500 . ? C7 C8 1.388(5) . ? C7 H7B 0.9500 . ? C8 C9 1.400(5) . ? C8 H8 0.9500 . ? C9 C10 1.393(4) . ? C9 H9 0.9500 . ? C10 C11 1.514(4) . ? C11 C12 1.525(5) . ? C11 H11 1.0000 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C16 1.475(5) . ? C15 C18 1.509(5) . ? C15 C17 1.512(5) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C20 1.397(4) . ? C19 C24 1.417(5) . ? C20 C21 1.387(5) . ? C20 H20 0.9500 . ? C21 C22 1.374(5) . ? C21 H21 0.9500 . ? C22 C23 1.395(4) . ? C22 H22 0.9500 . ? C23 C24 1.380(5) . ? C23 H23 0.9500 . ? C24 C25 1.515(4) . ? C25 C26 1.536(5) . ? C25 H25 1.0000 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 C30 1.491(5) . ? C29 C32 1.502(5) . ? C29 C31 1.507(5) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 C38 1.396(4) . ? C33 C34 1.404(5) . ? C34 C35 1.395(5) . ? C34 H34 0.9500 . ? C35 C36 1.379(5) . ? C35 H35 0.9500 . ? C36 C37 1.393(6) . ? C36 H36 0.9500 . ? C37 C38 1.389(5) . ? C37 H37 0.9500 . ? C38 C39 1.519(5) . ? C39 C40 1.514(6) . ? C39 H39 1.0000 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 C44 1.481(5) . ? C43 C46 1.502(5) . ? C43 C45 1.514(4) . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 C48 1.409(4) . ? C47 C52 1.414(4) . ? C48 C49 1.391(5) . ? C48 H48 0.9500 . ? C49 C50 1.392(5) . ? C49 H49 0.9500 . ? C50 C51 1.388(5) . ? C50 H50 0.9500 . ? C51 C52 1.395(5) . ? C51 H51 0.9500 . ? C52 C53 1.503(4) . ? C53 C54 1.535(4) . ? C53 H53 1.0000 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 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 C5 Pd1 N1 90.94(12) . . ? C5 Pd1 N2 81.41(12) . . ? N1 Pd1 N2 171.67(10) . . ? C5 Pd1 Cl1 176.06(10) . . ? N1 Pd1 Cl1 91.75(8) . . ? N2 Pd1 Cl1 96.06(7) . . ? C19 Pd2 N3 89.79(12) . . ? C19 Pd2 N4 80.93(12) . . ? N3 Pd2 N4 170.70(11) . . ? C19 Pd2 Cl2 174.26(9) . . ? N3 Pd2 Cl2 92.38(8) . . ? N4 Pd2 Cl2 96.92(8) . . ? C33 Pd3 N5 90.21(12) . . ? C33 Pd3 N6 81.26(12) . . ? N5 Pd3 N6 170.18(11) . . ? C33 Pd3 Cl3 176.05(10) . . ? N5 Pd3 Cl3 92.70(8) . . ? N6 Pd3 Cl3 96.06(8) . . ? C47 Pd4 N7 91.18(12) . . ? C47 Pd4 N8 81.46(12) . . ? N7 Pd4 N8 172.28(11) . . ? C47 Pd4 Cl4 177.58(9) . . ? N7 Pd4 Cl4 91.05(8) . . ? N8 Pd4 Cl4 96.35(8) . . ? C2 N1 C1 59.4(2) . . ? C2 N1 Pd1 124.7(2) . . ? C1 N1 Pd1 125.5(2) . . ? C2 N1 H1 112.5 . . ? C1 N1 H1 112.5 . . ? Pd1 N1 H1 112.5 . . ? C14 N2 C13 107.4(3) . . ? C14 N2 C11 109.1(2) . . ? C13 N2 C11 111.1(2) . . ? C14 N2 Pd1 108.98(18) . . ? C13 N2 Pd1 115.3(2) . . ? C11 N2 Pd1 104.9(2) . . ? C16 N3 C15 59.2(2) . . ? C16 N3 Pd2 128.4(2) . . ? C15 N3 Pd2 124.8(2) . . ? C16 N3 H3 111.6 . . ? C15 N3 H3 111.6 . . ? Pd2 N3 H3 111.6 . . ? C27 N4 C28 106.8(3) . . ? C27 N4 C25 111.2(3) . . ? C28 N4 C25 107.7(3) . . ? C27 N4 Pd2 116.4(2) . . ? C28 N4 Pd2 109.7(2) . . ? C25 N4 Pd2 104.65(19) . . ? C30 N5 C29 60.3(2) . . ? C30 N5 Pd3 124.3(2) . . ? C29 N5 Pd3 123.8(2) . . ? C30 N5 H5 112.9 . . ? C29 N5 H5 112.9 . . ? Pd3 N5 H5 112.9 . . ? C41 N6 C42 107.5(3) . . ? C41 N6 C39 111.2(3) . . ? C42 N6 C39 108.8(3) . . ? C41 N6 Pd3 115.0(2) . . ? C42 N6 Pd3 108.8(2) . . ? C39 N6 Pd3 105.4(2) . . ? C44 N7 C43 59.7(2) . . ? C44 N7 Pd4 126.0(2) . . ? C43 N7 Pd4 126.2(2) . . ? C44 N7 H7 111.8 . . ? C43 N7 H7 111.8 . . ? Pd4 N7 H7 111.8 . . ? C55 N8 C56 108.0(2) . . ? C55 N8 C53 112.0(2) . . ? C56 N8 C53 108.2(3) . . ? C55 N8 Pd4 114.2(2) . . ? C56 N8 Pd4 109.17(19) . . ? C53 N8 Pd4 105.19(18) . . ? C2 C1 N1 59.9(2) . . ? C2 C1 C4 119.8(3) . . ? N1 C1 C4 116.4(3) . . ? C2 C1 C3 119.2(3) . . ? N1 C1 C3 115.7(3) . . ? C4 C1 C3 114.7(3) . . ? C1 C2 N1 60.7(2) . . ? C1 C2 H2A 117.7 . . ? N1 C2 H2A 117.7 . . ? C1 C2 H2B 117.7 . . ? N1 C2 H2B 117.7 . . ? H2A C2 H2B 114.8 . . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C1 C4 H4A 109.5 . . ? C1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C10 C5 C6 118.5(3) . . ? C10 C5 Pd1 113.2(2) . . ? C6 C5 Pd1 128.2(2) . . ? C5 C6 C7 120.1(3) . . ? C5 C6 H6 119.9 . . ? C7 C6 H6 119.9 . . ? C8 C7 C6 120.9(3) . . ? C8 C7 H7B 119.6 . . ? C6 C7 H7B 119.6 . . ? C7 C8 C9 118.9(3) . . ? C7 C8 H8 120.5 . . ? C9 C8 H8 120.5 . . ? C10 C9 C8 120.3(3) . . ? C10 C9 H9 119.8 . . ? C8 C9 H9 119.8 . . ? C9 C10 C5 121.1(3) . . ? C9 C10 C11 122.5(3) . . ? C5 C10 C11 116.4(3) . . ? C10 C11 N2 106.0(2) . . ? C10 C11 C12 110.5(3) . . ? N2 C11 C12 112.7(3) . . ? C10 C11 H11 109.2 . . ? N2 C11 H11 109.2 . . ? C12 C11 H11 109.2 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N2 C13 H13A 109.5 . . ? N2 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? N2 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N2 C14 H14A 109.5 . . ? N2 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? N2 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C16 C15 N3 60.2(2) . . ? C16 C15 C18 118.3(3) . . ? N3 C15 C18 115.0(3) . . ? C16 C15 C17 119.3(3) . . ? N3 C15 C17 117.0(3) . . ? C18 C15 C17 115.6(3) . . ? C15 C16 N3 60.6(2) . . ? C15 C16 H16A 117.7 . . ? N3 C16 H16A 117.7 . . ? C15 C16 H16B 117.7 . . ? N3 C16 H16B 117.7 . . ? H16A C16 H16B 114.8 . . ? 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 . . ? C15 C18 H18A 109.5 . . ? C15 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C15 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C20 C19 C24 118.3(3) . . ? C20 C19 Pd2 128.6(3) . . ? C24 C19 Pd2 113.1(2) . . ? C21 C20 C19 119.9(3) . . ? C21 C20 H20 120.0 . . ? C19 C20 H20 120.0 . . ? C22 C21 C20 121.2(3) . . ? C22 C21 H21 119.4 . . ? C20 C21 H21 119.4 . . ? C21 C22 C23 120.1(3) . . ? C21 C22 H22 120.0 . . ? C23 C22 H22 120.0 . . ? C24 C23 C22 119.4(3) . . ? C24 C23 H23 120.3 . . ? C22 C23 H23 120.3 . . ? C23 C24 C19 121.0(3) . . ? C23 C24 C25 123.3(3) . . ? C19 C24 C25 115.6(3) . . ? N4 C25 C24 106.3(3) . . ? N4 C25 C26 112.1(3) . . ? C24 C25 C26 110.6(3) . . ? N4 C25 H25 109.2 . . ? C24 C25 H25 109.2 . . ? C26 C25 H25 109.2 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? N4 C27 H27A 109.5 . . ? N4 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? N4 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? N4 C28 H28A 109.5 . . ? N4 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? N4 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? N5 C29 C30 59.5(2) . . ? N5 C29 C32 116.8(3) . . ? C30 C29 C32 118.7(3) . . ? N5 C29 C31 114.5(3) . . ? C30 C29 C31 119.0(3) . . ? C32 C29 C31 116.1(3) . . ? N5 C30 C29 60.2(2) . . ? N5 C30 H30A 117.8 . . ? C29 C30 H30A 117.8 . . ? N5 C30 H30B 117.8 . . ? C29 C30 H30B 117.8 . . ? H30A C30 H30B 114.9 . . ? C29 C31 H31A 109.5 . . ? C29 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C29 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C29 C32 H32A 109.5 . . ? C29 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C29 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C38 C33 C34 118.3(3) . . ? C38 C33 Pd3 114.2(2) . . ? C34 C33 Pd3 127.4(2) . . ? C35 C34 C33 120.8(3) . . ? C35 C34 H34 119.6 . . ? C33 C34 H34 119.6 . . ? C36 C35 C34 120.3(4) . . ? C36 C35 H35 119.9 . . ? C34 C35 H35 119.9 . . ? C35 C36 C37 119.5(3) . . ? C35 C36 H36 120.3 . . ? C37 C36 H36 120.3 . . ? C38 C37 C36 120.6(3) . . ? C38 C37 H37 119.7 . . ? C36 C37 H37 119.7 . . ? C37 C38 C33 120.6(3) . . ? C37 C38 C39 123.8(3) . . ? C33 C38 C39 115.6(3) . . ? C40 C39 N6 113.1(3) . . ? C40 C39 C38 109.6(3) . . ? N6 C39 C38 106.5(3) . . ? C40 C39 H39 109.2 . . ? N6 C39 H39 109.2 . . ? C38 C39 H39 109.2 . . ? C39 C40 H40A 109.5 . . ? C39 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C39 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? N6 C41 H41A 109.5 . . ? N6 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? N6 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? N6 C42 H42A 109.5 . . ? N6 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? N6 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C44 C43 N7 59.6(2) . . ? C44 C43 C46 118.6(3) . . ? N7 C43 C46 114.9(3) . . ? C44 C43 C45 119.0(3) . . ? N7 C43 C45 116.7(2) . . ? C46 C43 C45 115.9(3) . . ? N7 C44 C43 60.8(2) . . ? N7 C44 H44A 117.7 . . ? C43 C44 H44A 117.7 . . ? N7 C44 H44B 117.7 . . ? C43 C44 H44B 117.7 . . ? H44A C44 H44B 114.8 . . ? C43 C45 H45A 109.5 . . ? C43 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C43 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C43 C46 H46A 109.5 . . ? C43 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C43 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C48 C47 C52 118.1(3) . . ? C48 C47 Pd4 128.3(3) . . ? C52 C47 Pd4 113.5(2) . . ? C49 C48 C47 120.3(3) . . ? C49 C48 H48 119.8 . . ? C47 C48 H48 119.8 . . ? C48 C49 C50 120.9(3) . . ? C48 C49 H49 119.6 . . ? C50 C49 H49 119.6 . . ? C51 C50 C49 119.7(4) . . ? C51 C50 H50 120.2 . . ? C49 C50 H50 120.2 . . ? C50 C51 C52 120.2(3) . . ? C50 C51 H51 119.9 . . ? C52 C51 H51 119.9 . . ? C51 C52 C47 120.8(3) . . ? C51 C52 C53 123.3(3) . . ? C47 C52 C53 115.9(3) . . ? C52 C53 N8 106.8(2) . . ? C52 C53 C54 110.1(3) . . ? N8 C53 C54 112.2(3) . . ? C52 C53 H53 109.2 . . ? N8 C53 H53 109.2 . . ? C54 C53 H53 109.2 . . ? C53 C54 H54A 109.5 . . ? C53 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C53 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? N8 C55 H55A 109.5 . . ? N8 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? N8 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? N8 C56 H56A 109.5 . . ? N8 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? N8 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 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 C5 Pd1 N1 C2 145.7(3) . . . . ? N2 Pd1 N1 C2 122.4(7) . . . . ? Cl1 Pd1 N1 C2 -37.2(3) . . . . ? C5 Pd1 N1 C1 71.2(3) . . . . ? N2 Pd1 N1 C1 47.9(8) . . . . ? Cl1 Pd1 N1 C1 -111.7(2) . . . . ? C5 Pd1 N2 C14 81.3(2) . . . . ? N1 Pd1 N2 C14 104.8(7) . . . . ? Cl1 Pd1 N2 C14 -95.68(19) . . . . ? C5 Pd1 N2 C13 -157.9(2) . . . . ? N1 Pd1 N2 C13 -134.4(7) . . . . ? Cl1 Pd1 N2 C13 25.1(2) . . . . ? C5 Pd1 N2 C11 -35.42(19) . . . . ? N1 Pd1 N2 C11 -11.9(8) . . . . ? Cl1 Pd1 N2 C11 147.62(17) . . . . ? C19 Pd2 N3 C16 148.1(3) . . . . ? N4 Pd2 N3 C16 152.2(6) . . . . ? Cl2 Pd2 N3 C16 -26.6(3) . . . . ? C19 Pd2 N3 C15 72.3(3) . . . . ? N4 Pd2 N3 C15 76.4(7) . . . . ? Cl2 Pd2 N3 C15 -102.4(2) . . . . ? C19 Pd2 N4 C27 -161.1(3) . . . . ? N3 Pd2 N4 C27 -165.3(6) . . . . ? Cl2 Pd2 N4 C27 13.5(2) . . . . ? C19 Pd2 N4 C28 77.5(2) . . . . ? N3 Pd2 N4 C28 73.3(7) . . . . ? Cl2 Pd2 N4 C28 -107.9(2) . . . . ? C19 Pd2 N4 C25 -37.86(19) . . . . ? N3 Pd2 N4 C25 -42.0(7) . . . . ? Cl2 Pd2 N4 C25 136.76(18) . . . . ? C33 Pd3 N5 C30 144.3(3) . . . . ? N6 Pd3 N5 C30 114.7(7) . . . . ? Cl3 Pd3 N5 C30 -38.4(2) . . . . ? C33 Pd3 N5 C29 69.6(3) . . . . ? N6 Pd3 N5 C29 40.0(8) . . . . ? Cl3 Pd3 N5 C29 -113.1(2) . . . . ? C33 Pd3 N6 C41 -157.1(3) . . . . ? N5 Pd3 N6 C41 -127.1(6) . . . . ? Cl3 Pd3 N6 C41 25.8(3) . . . . ? C33 Pd3 N6 C42 82.4(2) . . . . ? N5 Pd3 N6 C42 112.3(7) . . . . ? Cl3 Pd3 N6 C42 -94.7(2) . . . . ? C33 Pd3 N6 C39 -34.2(2) . . . . ? N5 Pd3 N6 C39 -4.2(8) . . . . ? Cl3 Pd3 N6 C39 148.7(2) . . . . ? C47 Pd4 N7 C44 143.9(3) . . . . ? N8 Pd4 N7 C44 126.6(7) . . . . ? Cl4 Pd4 N7 C44 -37.0(3) . . . . ? C47 Pd4 N7 C43 67.9(3) . . . . ? N8 Pd4 N7 C43 50.6(9) . . . . ? Cl4 Pd4 N7 C43 -113.0(3) . . . . ? C47 Pd4 N8 C55 -157.0(2) . . . . ? N7 Pd4 N8 C55 -139.4(7) . . . . ? Cl4 Pd4 N8 C55 24.1(2) . . . . ? C47 Pd4 N8 C56 82.1(2) . . . . ? N7 Pd4 N8 C56 99.6(8) . . . . ? Cl4 Pd4 N8 C56 -96.9(2) . . . . ? C47 Pd4 N8 C53 -33.82(19) . . . . ? N7 Pd4 N8 C53 -16.3(9) . . . . ? Cl4 Pd4 N8 C53 147.21(17) . . . . ? Pd1 N1 C1 C2 113.0(3) . . . . ? C2 N1 C1 C4 -110.6(3) . . . . ? Pd1 N1 C1 C4 2.3(4) . . . . ? C2 N1 C1 C3 110.3(3) . . . . ? Pd1 N1 C1 C3 -136.7(2) . . . . ? C4 C1 C2 N1 105.1(3) . . . . ? C3 C1 C2 N1 -104.4(3) . . . . ? Pd1 N1 C2 C1 -114.3(3) . . . . ? N1 Pd1 C5 C10 -157.1(3) . . . . ? N2 Pd1 C5 C10 19.5(2) . . . . ? Cl1 Pd1 C5 C10 69.8(14) . . . . ? N1 Pd1 C5 C6 26.5(3) . . . . ? N2 Pd1 C5 C6 -156.9(3) . . . . ? Cl1 Pd1 C5 C6 -106.6(13) . . . . ? C10 C5 C6 C7 0.6(5) . . . . ? Pd1 C5 C6 C7 176.8(3) . . . . ? C5 C6 C7 C8 2.5(5) . . . . ? C6 C7 C8 C9 -3.8(6) . . . . ? C7 C8 C9 C10 2.0(6) . . . . ? C8 C9 C10 C5 1.2(6) . . . . ? C8 C9 C10 C11 -179.7(3) . . . . ? C6 C5 C10 C9 -2.4(5) . . . . ? Pd1 C5 C10 C9 -179.2(3) . . . . ? C6 C5 C10 C11 178.4(3) . . . . ? Pd1 C5 C10 C11 1.6(4) . . . . ? C9 C10 C11 N2 149.5(3) . . . . ? C5 C10 C11 N2 -31.3(4) . . . . ? C9 C10 C11 C12 -88.0(4) . . . . ? C5 C10 C11 C12 91.2(3) . . . . ? C14 N2 C11 C10 -73.3(3) . . . . ? C13 N2 C11 C10 168.5(3) . . . . ? Pd1 N2 C11 C10 43.3(3) . . . . ? C14 N2 C11 C12 165.6(3) . . . . ? C13 N2 C11 C12 47.5(4) . . . . ? Pd1 N2 C11 C12 -77.8(3) . . . . ? Pd2 N3 C15 C16 117.8(3) . . . . ? C16 N3 C15 C18 -109.6(4) . . . . ? Pd2 N3 C15 C18 8.2(4) . . . . ? C16 N3 C15 C17 109.9(4) . . . . ? Pd2 N3 C15 C17 -132.3(3) . . . . ? C18 C15 C16 N3 104.2(3) . . . . ? C17 C15 C16 N3 -106.2(3) . . . . ? Pd2 N3 C16 C15 -112.1(3) . . . . ? N3 Pd2 C19 C20 22.9(3) . . . . ? N4 Pd2 C19 C20 -156.4(3) . . . . ? Cl2 Pd2 C19 C20 135.2(8) . . . . ? N3 Pd2 C19 C24 -157.4(2) . . . . ? N4 Pd2 C19 C24 23.3(2) . . . . ? Cl2 Pd2 C19 C24 -45.1(10) . . . . ? C24 C19 C20 C21 2.4(5) . . . . ? Pd2 C19 C20 C21 -177.9(2) . . . . ? C19 C20 C21 C22 -0.4(5) . . . . ? C20 C21 C22 C23 -0.6(5) . . . . ? C21 C22 C23 C24 -0.4(5) . . . . ? C22 C23 C24 C19 2.4(5) . . . . ? C22 C23 C24 C25 -177.7(3) . . . . ? C20 C19 C24 C23 -3.4(4) . . . . ? Pd2 C19 C24 C23 176.9(2) . . . . ? C20 C19 C24 C25 176.7(3) . . . . ? Pd2 C19 C24 C25 -3.0(3) . . . . ? C27 N4 C25 C24 170.6(3) . . . . ? C28 N4 C25 C24 -72.7(3) . . . . ? Pd2 N4 C25 C24 44.1(3) . . . . ? C27 N4 C25 C26 49.6(4) . . . . ? C28 N4 C25 C26 166.3(3) . . . . ? Pd2 N4 C25 C26 -76.9(3) . . . . ? C23 C24 C25 N4 151.3(3) . . . . ? C19 C24 C25 N4 -28.8(4) . . . . ? C23 C24 C25 C26 -86.8(4) . . . . ? C19 C24 C25 C26 93.1(3) . . . . ? Pd3 N5 C29 C30 113.5(3) . . . . ? C30 N5 C29 C32 109.0(3) . . . . ? Pd3 N5 C29 C32 -137.4(3) . . . . ? C30 N5 C29 C31 -110.4(3) . . . . ? Pd3 N5 C29 C31 3.1(4) . . . . ? Pd3 N5 C30 C29 -112.7(3) . . . . ? C32 C29 C30 N5 -105.9(3) . . . . ? C31 C29 C30 N5 103.0(3) . . . . ? N5 Pd3 C33 C38 -156.6(3) . . . . ? N6 Pd3 C33 C38 18.5(3) . . . . ? Cl3 Pd3 C33 C38 65.9(15) . . . . ? N5 Pd3 C33 C34 26.0(3) . . . . ? N6 Pd3 C33 C34 -158.8(3) . . . . ? Cl3 Pd3 C33 C34 -111.4(13) . . . . ? C38 C33 C34 C35 0.9(5) . . . . ? Pd3 C33 C34 C35 178.2(3) . . . . ? C33 C34 C35 C36 0.6(6) . . . . ? C34 C35 C36 C37 -2.2(6) . . . . ? C35 C36 C37 C38 2.4(6) . . . . ? C36 C37 C38 C33 -0.9(6) . . . . ? C36 C37 C38 C39 178.6(4) . . . . ? C34 C33 C38 C37 -0.8(6) . . . . ? Pd3 C33 C38 C37 -178.4(3) . . . . ? C34 C33 C38 C39 179.7(3) . . . . ? Pd3 C33 C38 C39 2.1(4) . . . . ? C41 N6 C39 C40 47.1(4) . . . . ? C42 N6 C39 C40 165.3(3) . . . . ? Pd3 N6 C39 C40 -78.1(3) . . . . ? C41 N6 C39 C38 167.6(3) . . . . ? C42 N6 C39 C38 -74.3(4) . . . . ? Pd3 N6 C39 C38 42.3(3) . . . . ? C37 C38 C39 C40 -87.7(5) . . . . ? C33 C38 C39 C40 91.8(4) . . . . ? C37 C38 C39 N6 149.7(4) . . . . ? C33 C38 C39 N6 -30.8(4) . . . . ? Pd4 N7 C43 C44 114.5(3) . . . . ? C44 N7 C43 C46 -109.8(3) . . . . ? Pd4 N7 C43 C46 4.8(4) . . . . ? C44 N7 C43 C45 109.6(4) . . . . ? Pd4 N7 C43 C45 -135.9(3) . . . . ? Pd4 N7 C44 C43 -114.9(3) . . . . ? C46 C43 C44 N7 103.7(3) . . . . ? C45 C43 C44 N7 -105.6(3) . . . . ? N7 Pd4 C47 C48 22.3(3) . . . . ? N8 Pd4 C47 C48 -160.0(3) . . . . ? Cl4 Pd4 C47 C48 -135(2) . . . . ? N7 Pd4 C47 C52 -160.4(2) . . . . ? N8 Pd4 C47 C52 17.3(2) . . . . ? Cl4 Pd4 C47 C52 43(2) . . . . ? C52 C47 C48 C49 1.9(5) . . . . ? Pd4 C47 C48 C49 179.0(2) . . . . ? C47 C48 C49 C50 -1.1(5) . . . . ? C48 C49 C50 C51 -0.4(5) . . . . ? C49 C50 C51 C52 1.1(5) . . . . ? C50 C51 C52 C47 -0.3(5) . . . . ? C50 C51 C52 C53 176.9(3) . . . . ? C48 C47 C52 C51 -1.1(5) . . . . ? Pd4 C47 C52 C51 -178.7(2) . . . . ? C48 C47 C52 C53 -178.5(3) . . . . ? Pd4 C47 C52 C53 3.9(3) . . . . ? C51 C52 C53 N8 150.2(3) . . . . ? C47 C52 C53 N8 -32.5(4) . . . . ? C51 C52 C53 C54 -87.7(4) . . . . ? C47 C52 C53 C54 89.6(3) . . . . ? C55 N8 C53 C52 167.4(3) . . . . ? C56 N8 C53 C52 -73.7(3) . . . . ? Pd4 N8 C53 C52 42.9(3) . . . . ? C55 N8 C53 C54 46.7(3) . . . . ? C56 N8 C53 C54 165.6(3) . . . . ? Pd4 N8 C53 C54 -77.8(3) . . . . ? loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag ? ? ? ? ? ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1 Cl4 0.93 2.33 3.259(3) 175.6 2_546 N3 H3 Cl3 0.93 2.37 3.272(3) 164.2 1_556 N5 H5 Cl2 0.93 2.31 3.235(3) 171.9 1_554 N7 H7 Cl1 0.93 2.27 3.195(3) 176.0 2_556 _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. ; data_2b_CCDC-849021 _database_code_depnum_ccdc_archive 'CCDC 849021' #TrackingRef 'Revision - CCDC-849021.cif' # CCDC: 849021 # Messcode: kn291 _audit_author_name 'S. Wirth, P. Mayer' _audit_block_code ? _audit_creation_method SHELXL-97 _audit_creation_date 30-Jun-06 _chemical_name_systematic '[Bis(N-(2-aminoethyl)aziridine-N,N)palladium(II)]bis(trifluormethansulfonate)' _chemical_name_common ;(Bis(N-(2-aminoethyl)aziridine- N,N)palladium(ii))bis(trifluormethansulfonate) ; _chemical_formula_moiety 'C8 H20 N4 Pd, 2(C F3 O3 S)' _chemical_formula_sum 'C10 H20 F6 N4 O6 Pd S2' _chemical_compound_source ? _exptl_crystal_recrystallization_method 'slow isothermic diffusion of n-pentane into a solution in methanol' _chemical_melting_point ? _exptl_crystal_description platelet _exptl_crystal_colour colourless _diffrn_ambient_temperature 200(2) _chemical_formula_weight 576.83 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 'P 21/c' _symmetry_Int_Tables_number 14 _chemical_absolute_configuration ? _symmetry_space_group_name_Hall -P2ybc 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 11.6261(3) _cell_length_b 9.8324(2) _cell_length_c 9.8676(2) _cell_angle_alpha 90.00 _cell_angle_beta 111.6582(13) _cell_angle_gamma 90.00 _cell_volume 1048.36(4) _cell_formula_units_Z 2 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 12644 _cell_measurement_theta_min 3.134 _cell_measurement_theta_max 27.485 _cell_special_details ? _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.82736 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 576 _exptl_absorpt_coefficient_mu 1.170 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ? loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0 0 1 0.020000 0 0 -1 0.020000 3 2 0 0.050000 -3 -2 0 0.050000 -3 1 0 0.050000 3 -1 0 0.050000 _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'rotating anode X-ray tube' _diffrn_source_type ? _diffrn_source_power 3.025 _diffrn_source_voltage 55.00 _diffrn_source_current 55.00 _diffrn_radiation_monochromator graphite _diffrn_radiation_collimation 0.25 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD; rotation images; thick slices' _diffrn_detector_area_resol_mean 9 _kl_diffrn_measurement_scan_angle phi/omega-scan _kl_diffrn_measurement_scan_step_degree 2.0 _kl_diffrn_measurement_scan_time_per_degree 8 _kl_diffrn_measurement_detector_distance 30 _diffrn_special_details ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4640 _diffrn_reflns_av_R_equivalents 0.0142 _diffrn_reflns_av_sigmaI/netI 0.0223 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 3.99 _diffrn_reflns_theta_max 27.52 _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.52 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.605 _refine_diff_density_min -0.552 _refine_diff_density_rms 0.060 _reflns_number_total 2400 _reflns_number_gt 2123 _reflns_threshold_expression >2sigma(I) _reflns_special_details ? _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; Ortep-3 for Windows: L. J. Farrugia, J. Appl. Cryst. 1997, 30, 565 ; _computing_publication_material ? _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^)+(0.0242P)^2^+0.3783P] 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 ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 2400 _refine_ls_number_parameters 169 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0278 _refine_ls_R_factor_gt 0.0228 _refine_ls_wR_factor_ref 0.0546 _refine_ls_wR_factor_gt 0.0523 _refine_ls_goodness_of_fit_ref 1.104 _refine_ls_restrained_S_all 1.104 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _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. ; 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 0.5000 0.0000 0.0000 0.02540(7) Uani 1 2 d S . . N1 N 0.63830(13) 0.07778(15) 0.17642(16) 0.0302(3) Uani 1 1 d . . . N2 N 0.40204(15) 0.15812(17) 0.03886(19) 0.0323(3) Uani 1 1 d . . . H2C H 0.351(2) 0.123(2) 0.074(3) 0.046(6) Uiso 1 1 d . . . H2D H 0.362(2) 0.202(2) -0.037(3) 0.047(7) Uiso 1 1 d . . . C1 C 0.75443(17) 0.1280(2) 0.1630(2) 0.0375(4) Uani 1 1 d . . . H1A H 0.7687 0.1060 0.0726 0.045 Uiso 1 1 calc R . . H1B H 0.7864 0.2177 0.2062 0.045 Uiso 1 1 calc R . . C2 C 0.75859(19) 0.0152(2) 0.2636(2) 0.0371(4) Uani 1 1 d . . . H2A H 0.7934 0.0344 0.3696 0.044 Uiso 1 1 calc R . . H2B H 0.7757 -0.0773 0.2360 0.044 Uiso 1 1 calc R . . C3 C 0.58398(18) 0.1685(2) 0.2575(2) 0.0353(4) Uani 1 1 d . . . H3A H 0.6487 0.2273 0.3257 0.042 Uiso 1 1 calc R . . H3B H 0.5456 0.1141 0.3141 0.042 Uiso 1 1 calc R . . C4 C 0.48820(18) 0.25312(19) 0.1453(2) 0.0358(4) Uani 1 1 d . . . H4A H 0.4428 0.3096 0.1921 0.043 Uiso 1 1 calc R . . H4B H 0.5279 0.3140 0.0956 0.043 Uiso 1 1 calc R . . C5 C 0.0847(2) 0.0603(3) 0.2520(4) 0.0665(7) Uani 1 1 d . . . F1A F 0.0614(11) 0.117(2) 0.3590(12) 0.072(3) Uani 0.42(5) 1 d P A 1 F2A F 0.0210(17) -0.0561(19) 0.221(3) 0.105(5) Uani 0.42(5) 1 d P A 1 F3A F 0.043(2) 0.136(3) 0.1244(19) 0.134(6) Uani 0.42(5) 1 d P A 1 F1B F 0.0740(13) 0.149(2) 0.3497(14) 0.113(4) Uani 0.58(5) 1 d P A 2 F2B F 0.0429(17) -0.0601(14) 0.271(4) 0.126(5) Uani 0.58(5) 1 d P A 2 F3B F 0.0178(10) 0.1122(13) 0.1284(8) 0.080(2) Uani 0.58(5) 1 d P A 2 S1 S 0.24825(4) 0.04180(5) 0.28705(5) 0.03268(11) Uani 1 1 d . A . O1 O 0.25325(16) -0.04039(17) 0.16995(18) 0.0506(4) Uani 1 1 d . . . O2 O 0.2967(2) -0.01933(18) 0.4272(2) 0.0609(5) Uani 1 1 d . . . O3 O 0.28786(15) 0.17946(15) 0.28075(17) 0.0501(4) 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 0.02417(11) 0.02515(11) 0.02695(11) 0.00165(7) 0.00950(8) -0.00041(7) N1 0.0284(7) 0.0307(8) 0.0310(8) 0.0005(6) 0.0104(6) -0.0018(6) N2 0.0310(8) 0.0326(9) 0.0338(9) 0.0031(7) 0.0126(7) 0.0031(7) C1 0.0289(9) 0.0406(11) 0.0428(11) -0.0016(9) 0.0128(8) -0.0057(8) C2 0.0282(9) 0.0409(11) 0.0352(10) 0.0015(8) 0.0036(8) 0.0028(8) C3 0.0372(10) 0.0372(10) 0.0325(10) -0.0050(8) 0.0140(8) -0.0028(8) C4 0.0388(10) 0.0302(10) 0.0401(10) -0.0035(8) 0.0165(8) -0.0001(8) C5 0.0438(14) 0.0652(19) 0.092(2) -0.0034(17) 0.0276(15) 0.0027(14) F1A 0.053(4) 0.098(8) 0.079(7) -0.011(4) 0.041(4) 0.009(4) F2A 0.050(5) 0.092(7) 0.168(11) -0.046(9) 0.036(6) -0.030(4) F3A 0.046(7) 0.123(8) 0.184(13) 0.039(7) -0.017(5) 0.023(6) F1B 0.108(6) 0.089(6) 0.187(9) -0.007(4) 0.108(6) 0.026(4) F2B 0.060(5) 0.104(5) 0.223(15) 0.017(7) 0.063(8) -0.034(3) F3B 0.032(3) 0.116(4) 0.075(5) -0.004(3) -0.0012(19) 0.009(2) S1 0.0328(2) 0.0331(2) 0.0337(2) -0.0013(2) 0.01408(18) 0.0009(2) O1 0.0662(10) 0.0445(8) 0.0464(9) -0.0112(7) 0.0272(8) 0.0034(8) O2 0.0726(13) 0.0717(12) 0.0425(10) 0.0192(8) 0.0259(9) 0.0216(9) O3 0.0589(9) 0.0383(8) 0.0552(9) -0.0073(7) 0.0237(8) -0.0142(7) 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 2.0333(15) . ? Pd1 N1 2.0334(15) 3_655 ? Pd1 N2 2.0454(16) 3_655 ? Pd1 N2 2.0454(16) . ? N1 C2 1.479(2) . ? N1 C3 1.486(2) . ? N1 C1 1.489(2) . ? N2 C4 1.484(2) . ? N2 H2C 0.87(3) . ? N2 H2D 0.84(3) . ? C1 C2 1.478(3) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.499(3) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 F3B 1.286(9) . ? C5 F1A 1.307(13) . ? C5 F2B 1.320(13) . ? C5 F2A 1.336(16) . ? C5 F1B 1.341(13) . ? C5 F3A 1.38(2) . ? C5 S1 1.812(3) . ? S1 O2 1.4202(18) . ? S1 O1 1.4287(16) . ? S1 O3 1.4384(15) . ? 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 N1 180.0 . 3_655 ? N1 Pd1 N2 97.31(6) . 3_655 ? N1 Pd1 N2 82.69(6) 3_655 3_655 ? N1 Pd1 N2 82.69(6) . . ? N1 Pd1 N2 97.31(6) 3_655 . ? N2 Pd1 N2 180.0 3_655 . ? C2 N1 C3 115.80(15) . . ? C2 N1 C1 59.73(12) . . ? C3 N1 C1 115.35(15) . . ? C2 N1 Pd1 128.37(12) . . ? C3 N1 Pd1 109.14(11) . . ? C1 N1 Pd1 120.36(12) . . ? C4 N2 Pd1 109.52(12) . . ? C4 N2 H2C 110.4(16) . . ? Pd1 N2 H2C 106.7(15) . . ? C4 N2 H2D 108.3(16) . . ? Pd1 N2 H2D 112.5(16) . . ? H2C N2 H2D 109(2) . . ? C2 C1 N1 59.81(12) . . ? C2 C1 H1A 117.8 . . ? N1 C1 H1A 117.8 . . ? C2 C1 H1B 117.8 . . ? N1 C1 H1B 117.8 . . ? H1A C1 H1B 114.9 . . ? C1 C2 N1 60.46(12) . . ? C1 C2 H2A 117.7 . . ? N1 C2 H2A 117.7 . . ? C1 C2 H2B 117.7 . . ? N1 C2 H2B 117.7 . . ? H2A C2 H2B 114.8 . . ? N1 C3 C4 106.45(15) . . ? N1 C3 H3A 110.4 . . ? C4 C3 H3A 110.4 . . ? N1 C3 H3B 110.4 . . ? C4 C3 H3B 110.4 . . ? H3A C3 H3B 108.6 . . ? N2 C4 C3 107.26(15) . . ? N2 C4 H4A 110.3 . . ? C3 C4 H4A 110.3 . . ? N2 C4 H4B 110.3 . . ? C3 C4 H4B 110.3 . . ? H4A C4 H4B 108.5 . . ? F3B C5 F1A 111.4(8) . . ? F3B C5 F2B 111.5(12) . . ? F1A C5 F2B 94.0(11) . . ? F3B C5 F2A 92.0(12) . . ? F1A C5 F2A 106.6(12) . . ? F2B C5 F2A 20.2(17) . . ? F3B C5 F1B 103.9(8) . . ? F1A C5 F1B 16.2(13) . . ? F2B C5 F1B 110.2(9) . . ? F2A C5 F1B 122.2(11) . . ? F3B C5 F3A 16.2(13) . . ? F1A C5 F3A 113.6(12) . . ? F2B C5 F3A 126.0(10) . . ? F2A C5 F3A 105.9(13) . . ? F1B C5 F3A 102.2(10) . . ? F3B C5 S1 116.4(5) . . ? F1A C5 S1 113.8(6) . . ? F2B C5 S1 107.3(8) . . ? F2A C5 S1 114.3(8) . . ? F1B C5 S1 107.3(7) . . ? F3A C5 S1 102.4(12) . . ? O2 S1 O1 115.36(11) . . ? O2 S1 O3 114.96(11) . . ? O1 S1 O3 112.83(10) . . ? O2 S1 C5 103.88(14) . . ? O1 S1 C5 104.81(13) . . ? O3 S1 C5 103.14(12) . . ? 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 N1 Pd1 N1 C2 39(11) 3_655 . . . ? N2 Pd1 N1 C2 -12.64(16) 3_655 . . . ? N2 Pd1 N1 C2 167.36(16) . . . . ? N1 Pd1 N1 C3 -111(11) 3_655 . . . ? N2 Pd1 N1 C3 -162.22(12) 3_655 . . . ? N2 Pd1 N1 C3 17.78(12) . . . . ? N1 Pd1 N1 C1 113(11) 3_655 . . . ? N2 Pd1 N1 C1 61.02(14) 3_655 . . . ? N2 Pd1 N1 C1 -118.98(14) . . . . ? N1 Pd1 N2 C4 12.11(13) . . . . ? N1 Pd1 N2 C4 -167.89(13) 3_655 . . . ? N2 Pd1 N2 C4 -68(8) 3_655 . . . ? C3 N1 C1 C2 106.33(17) . . . . ? Pd1 N1 C1 C2 -119.41(15) . . . . ? C3 N1 C2 C1 -105.57(17) . . . . ? Pd1 N1 C2 C1 106.52(16) . . . . ? C2 N1 C3 C4 162.31(15) . . . . ? C1 N1 C3 C4 95.29(18) . . . . ? Pd1 N1 C3 C4 -43.86(16) . . . . ? Pd1 N2 C4 C3 -39.37(18) . . . . ? N1 C3 C4 N2 54.40(19) . . . . ? F3B C5 S1 O2 -178.9(6) . . . . ? F1A C5 S1 O2 49.5(11) . . . . ? F2B C5 S1 O2 -53.1(14) . . . . ? F2A C5 S1 O2 -73.4(13) . . . . ? F1B C5 S1 O2 65.3(10) . . . . ? F3A C5 S1 O2 172.5(9) . . . . ? F3B C5 S1 O1 -57.4(6) . . . . ? F1A C5 S1 O1 170.9(11) . . . . ? F2B C5 S1 O1 68.4(14) . . . . ? F2A C5 S1 O1 48.0(13) . . . . ? F1B C5 S1 O1 -173.2(10) . . . . ? F3A C5 S1 O1 -66.0(9) . . . . ? F3B C5 S1 O3 60.9(6) . . . . ? F1A C5 S1 O3 -70.8(11) . . . . ? F2B C5 S1 O3 -173.3(14) . . . . ? F2A C5 S1 O3 166.3(12) . . . . ? F1B C5 S1 O3 -54.9(10) . . . . ? F3A C5 S1 O3 52.3(9) . . . . ? loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag ? ? ? ? ? ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N2 H2C O1 0.87(3) 2.35(3) 3.182(3) 160(2) . N2 H2C O3 0.87(3) 2.47(2) 3.137(2) 134.5(19) . N2 H2D O3 0.84(3) 2.04(3) 2.882(2) 172(2) 4_565 _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. ; #===END data_4c_CCDC-000000 _database_code_depnum_ccdc_archive 'CCDC 849022' #TrackingRef 'DTrans. aziridine.cif' # CCDC: 000000 # Messcode: kn532 _audit_author_name 'S. Wirth, S. Albrecht' _audit_block_code ? _audit_creation_method SHELXL-97 _audit_creation_date 27-Okt-06 _chemical_name_systematic '[Tris(N-(2-aminoethyl)aziridine-N,N)copper(II)]dichloride' _chemical_name_common ? _chemical_formula_moiety 'C16 H36 Cl Cu N4, Cl' _chemical_formula_sum 'C16 H36 Cl2 Cu N4' _chemical_compound_source ? _exptl_crystal_recrystallization_method ; slow isothermic diffusion of n-pentane into a solution in dichloromethane ; _chemical_melting_point ? _exptl_crystal_description rod _exptl_crystal_colour light_blue _diffrn_ambient_temperature 200(2) _chemical_formula_weight 418.935 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' Cu Cu 0.3201 1.2651 '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 n a 21' _symmetry_Int_Tables_number 33 _chemical_absolute_configuration unk _symmetry_space_group_name_Hall P2c-2n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z+1/2' _cell_length_a 24.9994(5) _cell_length_b 9.05370(10) _cell_length_c 18.8146(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4258.44(12) _cell_formula_units_Z 8 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 99796 _cell_measurement_theta_min 3.134 _cell_measurement_theta_max 27.485 _cell_special_details ? _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.30690 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1784 _exptl_absorpt_coefficient_mu 1.281 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ? loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 1 0 0 0.095000 -1 0 0 0.060000 0 1 0 0.025000 0 -1 0 0.015000 0 0 1 0.010000 0 0 -1 0.015000 _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source "'rotating anode X-ray tube" _diffrn_source_type ? _diffrn_source_power 3.025 _diffrn_source_voltage 55.00 _diffrn_source_current 55.00 _diffrn_radiation_monochromator graphite _diffrn_radiation_collimation 0.25 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD; rotation images; thick slices' _diffrn_detector_area_resol_mean 9 _kl_diffrn_measurement_scan_angle phi/omega-scan _kl_diffrn_measurement_scan_step_degree 0.80 _kl_diffrn_measurement_scan_time_per_degree 150 _kl_diffrn_measurement_detector_distance 30 _diffrn_special_details ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7966 _diffrn_reflns_av_R_equivalents 0.0275 _diffrn_reflns_av_sigmaI/netI 0.0345 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.23 _diffrn_reflns_theta_max 26.00 _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.208 _refine_diff_density_min -0.366 _refine_diff_density_rms 0.087 _reflns_number_total 4295 _reflns_number_gt 3240 _reflns_threshold_expression >2sigma(I) _reflns_special_details ? _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; Ortep-3 for Windows: L. J. Farrugia, J. Appl. Cryst. 1997, 30, 565 ; _computing_publication_material ? _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^)+(0.0877P)^2^+1.5391P] 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 0.29(6) _refine_ls_number_reflns 4295 _refine_ls_number_parameters 416 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0692 _refine_ls_R_factor_gt 0.0465 _refine_ls_wR_factor_ref 0.1352 _refine_ls_wR_factor_gt 0.1204 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.020 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_special_details ; Friedel pairs merged before use. 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. ; 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 Cu1 Cu 1.00149(3) 0.73948(7) 0.62319(6) 0.0226(3) Uani 1 1 d . . . Cl3 Cl 0.82751(8) 0.2683(2) 0.86451(17) 0.0463(6) Uani 1 1 d . . . Cl4 Cl 0.65768(7) 0.75740(15) 0.73804(18) 0.0351(5) Uani 1 1 d . . . N1 N 0.7760(2) 0.1636(5) 0.7193(3) 0.0292(12) Uani 1 1 d . . . N2 N 0.7083(2) 0.4071(6) 0.7378(3) 0.0330(13) Uani 1 1 d . . . H1N H 0.6727 0.3855 0.7312 0.040 Uiso 1 1 calc R . . H2N H 0.7112 0.5017 0.7552 0.040 Uiso 1 1 calc R . . N3 N 0.7030(2) 0.3317(5) 0.8973(3) 0.0300(12) Uani 1 1 d . . . N4 N 0.6806(2) 0.0966(5) 0.8085(4) 0.0314(12) Uani 1 1 d . . . H3N H 0.6563 0.1217 0.7738 0.038 Uiso 1 1 calc R . . H4N H 0.6936 0.0036 0.7988 0.038 Uiso 1 1 calc R . . C1 C 0.7973(3) 0.0077(7) 0.7129(4) 0.0299(16) Uani 1 1 d . . . C2 C 0.8334(3) 0.1347(7) 0.7056(4) 0.0336(15) Uani 1 1 d . . . H2A H 0.8473 0.1571 0.6576 0.040 Uiso 1 1 calc R . . H2B H 0.8588 0.1539 0.7448 0.040 Uiso 1 1 calc R . . C3 C 0.7829(3) -0.0815(7) 0.6484(4) 0.0434(19) Uani 1 1 d . . . H3A H 0.7583 -0.1610 0.6621 0.065 Uiso 1 1 calc R . . H3B H 0.8154 -0.1241 0.6277 0.065 Uiso 1 1 calc R . . H3C H 0.7655 -0.0175 0.6133 0.065 Uiso 1 1 calc R . . C4 C 0.7981(3) -0.0801(8) 0.7809(4) 0.0399(17) Uani 1 1 d . . . H4A H 0.7722 -0.1609 0.7778 0.060 Uiso 1 1 calc R . . H4B H 0.7888 -0.0156 0.8209 0.060 Uiso 1 1 calc R . . H4C H 0.8340 -0.1209 0.7884 0.060 Uiso 1 1 calc R . . C5 C 0.7455(3) 0.2266(10) 0.6596(7) 0.037(2) Uani 1 1 d . . . H5A H 0.7101 0.1779 0.6565 0.044 Uiso 1 1 calc R . . H5B H 0.7648 0.2083 0.6145 0.044 Uiso 1 1 calc R . . C6 C 0.7378(3) 0.3931(7) 0.6699(4) 0.0317(15) Uani 1 1 d . . . C7 C 0.7057(3) 0.4555(8) 0.6075(4) 0.0468(19) Uani 1 1 d . . . H7A H 0.7002 0.5617 0.6145 0.070 Uiso 1 1 calc R . . H7B H 0.6709 0.4057 0.6050 0.070 Uiso 1 1 calc R . . H7C H 0.7253 0.4390 0.5632 0.070 Uiso 1 1 calc R . . C8 C 0.7911(3) 0.4744(8) 0.6788(6) 0.049(2) Uani 1 1 d . . . H8A H 0.7843 0.5799 0.6861 0.074 Uiso 1 1 calc R . . H8B H 0.8129 0.4608 0.6360 0.074 Uiso 1 1 calc R . . H8C H 0.8102 0.4345 0.7201 0.074 Uiso 1 1 calc R . . C9 C 0.7075(3) 0.4847(7) 0.9310(4) 0.0327(18) Uani 1 1 d . . . C10 C 0.7271(3) 0.3512(7) 0.9687(4) 0.0373(16) Uani 1 1 d . . . H10A H 0.7663 0.3382 0.9730 0.045 Uiso 1 1 calc R . . H10B H 0.7063 0.3163 1.0103 0.045 Uiso 1 1 calc R . . C11 C 0.6579(3) 0.5591(8) 0.9561(5) 0.053(2) Uani 1 1 d . . . H11A H 0.6498 0.6431 0.9250 0.080 Uiso 1 1 calc R . . H11B H 0.6631 0.5942 1.0049 0.080 Uiso 1 1 calc R . . H11C H 0.6280 0.4889 0.9548 0.080 Uiso 1 1 calc R . . C12 C 0.7477(3) 0.5844(8) 0.8956(5) 0.047(2) Uani 1 1 d . . . H12A H 0.7291 0.6662 0.8721 0.071 Uiso 1 1 calc R . . H12B H 0.7679 0.5280 0.8601 0.071 Uiso 1 1 calc R . . H12C H 0.7724 0.6237 0.9314 0.071 Uiso 1 1 calc R . . C13 C 0.6497(3) 0.2616(6) 0.8978(5) 0.0270(17) Uani 1 1 d . . . H13A H 0.6262 0.3111 0.8628 0.032 Uiso 1 1 calc R . . H13B H 0.6333 0.2724 0.9455 0.032 Uiso 1 1 calc R . . C14 C 0.6547(3) 0.0989(7) 0.8794(4) 0.0333(15) Uani 1 1 d . . . C15 C 0.5991(3) 0.0289(8) 0.8773(5) 0.0468(19) Uani 1 1 d . . . H15A H 0.6023 -0.0761 0.8654 0.070 Uiso 1 1 calc R . . H15B H 0.5773 0.0786 0.8412 0.070 Uiso 1 1 calc R . . H15C H 0.5820 0.0393 0.9239 0.070 Uiso 1 1 calc R . . C16 C 0.6908(3) 0.0169(8) 0.9324(5) 0.046(2) Uani 1 1 d . . . H16A H 0.6926 -0.0878 0.9194 0.069 Uiso 1 1 calc R . . H16B H 0.6760 0.0265 0.9804 0.069 Uiso 1 1 calc R . . H16C H 0.7268 0.0596 0.9311 0.069 Uiso 1 1 calc R . . Cu2 Cu 0.74431(3) 0.25152(7) 0.81051(6) 0.0214(3) Uani 1 1 d . . . Cl1 Cl 1.08853(7) 0.24757(14) 0.69506(18) 0.0328(5) Uani 1 1 d . . . Cl2 Cl 0.91785(7) 0.75470(19) 0.57169(18) 0.0422(5) Uani 1 1 d . . . N5 N 1.0416(2) 0.8162(5) 0.5346(3) 0.0310(12) Uani 1 1 d . . . N6 N 1.06466(19) 0.5858(5) 0.6259(3) 0.0281(12) Uani 1 1 d . . . H5N H 1.0895 0.6133 0.6595 0.034 Uiso 1 1 calc R . . H6N H 1.0519 0.4937 0.6375 0.034 Uiso 1 1 calc R . . N7 N 0.97052(19) 0.6533(5) 0.7167(3) 0.0277(12) Uani 1 1 d . . . N8 N 1.0370(2) 0.8965(5) 0.6943(3) 0.0277(11) Uani 1 1 d . . . H7N H 1.0728 0.8760 0.7004 0.033 Uiso 1 1 calc R . . H8N H 1.0338 0.9905 0.6762 0.033 Uiso 1 1 calc R . . C17 C 1.0373(3) 0.9706(7) 0.5039(4) 0.0366(18) Uani 1 1 d . . . C18 C 1.0162(3) 0.8384(7) 0.4635(4) 0.0341(16) Uani 1 1 d . . . H18A H 0.9769 0.8263 0.4601 0.041 Uiso 1 1 calc R . . H18B H 1.0364 0.8056 0.4210 0.041 Uiso 1 1 calc R . . C19 C 0.9982(3) 1.0717(8) 0.5399(5) 0.046(2) Uani 1 1 d . . . H19A H 1.0176 1.1508 0.5643 0.069 Uiso 1 1 calc R . . H19C H 0.9771 1.0156 0.5745 0.069 Uiso 1 1 calc R . . H19E H 0.9742 1.1148 0.5042 0.069 Uiso 1 1 calc R . . C20 C 1.0868(3) 1.0461(8) 0.4770(5) 0.049(2) Uani 1 1 d . . . H20A H 1.1102 0.9733 0.4541 0.073 Uiso 1 1 calc R . . H20C H 1.1058 1.0918 0.5169 0.073 Uiso 1 1 calc R . . H20E H 1.0768 1.1223 0.4425 0.073 Uiso 1 1 calc R . . C21 C 1.0952(3) 0.7457(6) 0.5333(6) 0.0283(18) Uani 1 1 d . . . H21A H 1.1195 0.7972 0.5666 0.034 Uiso 1 1 calc R . . H21B H 1.1106 0.7523 0.4849 0.034 Uiso 1 1 calc R . . C22 C 1.0894(3) 0.5826(7) 0.5552(4) 0.0322(15) Uani 1 1 d . . . C23 C 1.0522(3) 0.5000(8) 0.5048(5) 0.041(2) Uani 1 1 d . . . H23A H 1.0168 0.5462 0.5055 0.061 Uiso 1 1 calc R . . H23B H 1.0492 0.3968 0.5200 0.061 Uiso 1 1 calc R . . H23C H 1.0668 0.5038 0.4565 0.061 Uiso 1 1 calc R . . C24 C 1.1448(3) 0.5111(7) 0.5555(4) 0.0422(19) Uani 1 1 d . . . H24A H 1.1684 0.5655 0.5879 0.063 Uiso 1 1 calc R . . H24B H 1.1598 0.5138 0.5073 0.063 Uiso 1 1 calc R . . H24C H 1.1418 0.4083 0.5713 0.063 Uiso 1 1 calc R . . C25 C 0.9495(3) 0.4981(7) 0.7260(5) 0.0347(18) Uani 1 1 d . . . C26 C 0.9127(3) 0.6261(7) 0.7319(4) 0.0347(15) Uani 1 1 d . . . H26A H 0.8993 0.6520 0.7798 0.042 Uiso 1 1 calc R . . H26B H 0.8869 0.6422 0.6928 0.042 Uiso 1 1 calc R . . C27 C 0.9640(3) 0.4081(7) 0.7893(4) 0.0389(17) Uani 1 1 d . . . H27A H 0.9883 0.3285 0.7749 0.058 Uiso 1 1 calc R . . H27B H 0.9316 0.3655 0.8100 0.058 Uiso 1 1 calc R . . H27C H 0.9818 0.4710 0.8245 0.058 Uiso 1 1 calc R . . C28 C 0.9484(3) 0.4090(7) 0.6572(5) 0.0394(17) Uani 1 1 d . . . H28A H 0.9744 0.3281 0.6602 0.059 Uiso 1 1 calc R . . H28B H 0.9576 0.4734 0.6171 0.059 Uiso 1 1 calc R . . H28C H 0.9125 0.3682 0.6500 0.059 Uiso 1 1 calc R . . C29 C 1.0013(2) 0.7229(9) 0.7760(6) 0.0260(18) Uani 1 1 d . . . H29A H 1.0368 0.6751 0.7800 0.031 Uiso 1 1 calc R . . H29B H 0.9820 0.7076 0.8214 0.031 Uiso 1 1 calc R . . C30 C 1.0085(2) 0.8854(7) 0.7632(4) 0.0286(14) Uani 1 1 d . . . C31 C 0.9559(3) 0.9666(8) 0.7556(5) 0.0411(19) Uani 1 1 d . . . H31A H 0.9628 1.0717 0.7472 0.062 Uiso 1 1 calc R . . H31B H 0.9349 0.9550 0.7993 0.062 Uiso 1 1 calc R . . H31C H 0.9358 0.9257 0.7154 0.062 Uiso 1 1 calc R . . C32 C 1.0415(3) 0.9479(8) 0.8236(4) 0.0411(18) Uani 1 1 d . . . H32A H 1.0460 1.0545 0.8169 0.062 Uiso 1 1 calc R . . H32B H 1.0767 0.9000 0.8243 0.062 Uiso 1 1 calc R . . H32C H 1.0232 0.9295 0.8688 0.062 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 Cu1 0.0219(4) 0.0247(5) 0.0212(6) 0.0014(4) -0.0028(3) 0.0008(3) Cl3 0.0265(9) 0.0712(13) 0.0414(14) -0.0149(10) -0.0117(9) 0.0012(8) Cl4 0.0301(9) 0.0274(9) 0.0476(14) -0.0042(7) -0.0052(9) -0.0005(6) N1 0.027(3) 0.029(3) 0.032(3) 0.000(2) -0.002(2) 0.000(2) N2 0.030(3) 0.030(3) 0.039(3) -0.001(2) -0.003(3) 0.004(2) N3 0.029(3) 0.030(3) 0.031(3) -0.002(2) -0.002(2) -0.002(2) N4 0.033(3) 0.029(3) 0.032(3) -0.005(2) -0.002(3) 0.003(2) C1 0.028(3) 0.026(3) 0.036(4) -0.007(3) 0.001(3) 0.007(3) C2 0.029(3) 0.036(3) 0.036(4) -0.002(3) 0.007(3) 0.005(3) C3 0.048(5) 0.030(4) 0.052(5) -0.014(3) 0.004(4) -0.001(3) C4 0.033(4) 0.037(4) 0.050(5) 0.003(3) -0.005(3) 0.009(3) C5 0.030(4) 0.054(5) 0.026(5) -0.003(4) -0.005(3) 0.002(3) C6 0.035(4) 0.029(3) 0.031(4) 0.001(3) -0.001(3) 0.000(3) C7 0.057(5) 0.045(4) 0.039(4) 0.010(3) -0.005(4) 0.009(4) C8 0.031(4) 0.037(4) 0.080(7) 0.013(4) 0.013(4) -0.005(3) C9 0.041(4) 0.028(4) 0.029(4) -0.010(3) -0.001(3) -0.008(3) C10 0.043(4) 0.044(4) 0.025(4) -0.005(3) -0.007(3) 0.001(3) C11 0.059(5) 0.037(4) 0.062(6) -0.016(4) -0.004(4) 0.005(4) C12 0.055(5) 0.035(4) 0.051(5) -0.004(4) -0.003(4) -0.010(3) C13 0.027(3) 0.031(4) 0.023(5) -0.004(2) 0.001(3) -0.004(2) C14 0.038(4) 0.031(3) 0.031(4) -0.002(3) 0.004(3) -0.008(3) C15 0.034(4) 0.049(4) 0.058(5) 0.001(4) 0.012(4) -0.011(3) C16 0.065(6) 0.035(4) 0.038(5) 0.005(4) -0.005(4) 0.001(4) Cu2 0.0218(4) 0.0223(5) 0.0200(6) -0.0024(3) -0.0016(4) 0.0000(3) Cl1 0.0314(9) 0.0270(9) 0.0399(13) 0.0048(6) -0.0026(8) -0.0012(6) Cl2 0.0285(9) 0.0630(13) 0.0351(13) 0.0080(8) -0.0102(9) -0.0002(7) N5 0.038(3) 0.022(3) 0.033(3) 0.004(2) -0.008(3) 0.004(2) N6 0.026(3) 0.029(3) 0.029(3) 0.007(2) 0.003(2) 0.002(2) N7 0.024(3) 0.025(2) 0.033(3) 0.002(2) -0.001(2) -0.002(2) N8 0.032(3) 0.024(3) 0.027(3) 0.004(2) 0.002(2) 0.003(2) C17 0.059(5) 0.026(3) 0.024(4) 0.008(3) -0.006(4) 0.001(3) C18 0.047(4) 0.025(3) 0.030(4) 0.004(3) -0.014(3) 0.001(3) C19 0.068(6) 0.032(4) 0.038(4) 0.003(3) -0.017(4) 0.010(3) C20 0.061(5) 0.041(4) 0.045(5) 0.014(3) -0.002(4) -0.008(4) C21 0.023(3) 0.031(4) 0.031(5) 0.004(3) 0.007(3) -0.001(2) C22 0.035(4) 0.032(3) 0.030(4) 0.004(3) 0.003(3) 0.001(3) C23 0.059(5) 0.038(4) 0.024(5) -0.003(3) -0.005(4) -0.002(4) C24 0.034(4) 0.046(4) 0.047(5) 0.011(4) 0.014(3) 0.006(3) C25 0.022(3) 0.027(3) 0.055(5) 0.008(3) 0.006(3) -0.004(3) C26 0.027(3) 0.038(3) 0.038(4) -0.001(3) 0.004(3) 0.003(3) C27 0.036(4) 0.034(4) 0.047(5) 0.005(3) -0.002(3) -0.003(3) C28 0.035(4) 0.029(3) 0.055(5) -0.003(3) 0.005(3) -0.005(3) C29 0.025(4) 0.034(4) 0.019(4) 0.004(4) -0.001(3) 0.000(2) C30 0.029(3) 0.025(3) 0.032(4) -0.001(3) 0.002(3) -0.002(3) C31 0.041(4) 0.033(4) 0.050(5) -0.008(4) -0.001(4) 0.002(3) C32 0.049(5) 0.043(4) 0.031(4) -0.009(3) 0.001(3) -0.003(3) 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 Cu1 N5 2.066(7) . ? Cu1 N7 2.074(6) . ? Cu1 N6 2.105(5) . ? Cu1 N8 2.145(6) . ? Cu1 Cl2 2.309(2) . ? Cl3 Cu2 2.320(3) . ? N1 C5 1.472(12) . ? N1 C2 1.481(8) . ? N1 C1 1.514(7) . ? N1 Cu2 2.051(6) . ? N2 C6 1.479(9) . ? N2 Cu2 2.160(6) . ? N2 H1N 0.9200 . ? N2 H2N 0.9200 . ? N3 C13 1.476(8) . ? N3 C10 1.483(8) . ? N3 C9 1.528(8) . ? N3 Cu2 2.064(6) . ? N4 C14 1.484(9) . ? N4 Cu2 2.122(5) . ? N4 H3N 0.9200 . ? N4 H4N 0.9200 . ? C1 C2 1.467(9) . ? C1 C3 1.502(9) . ? C1 C4 1.506(10) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 C6 1.531(9) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C8 1.530(9) . ? C6 C7 1.531(10) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 C10 1.486(10) . ? C9 C11 1.487(10) . ? C9 C12 1.508(10) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.518(8) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.529(9) . ? C14 C16 1.536(11) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? N5 C21 1.484(8) . ? N5 C18 1.495(8) . ? N5 C17 1.517(8) . ? N6 C22 1.467(9) . ? N6 H5N 0.9200 . ? N6 H6N 0.9200 . ? N7 C26 1.494(8) . ? N7 C29 1.496(11) . ? N7 C25 1.510(7) . ? N8 C30 1.482(9) . ? N8 H7N 0.9200 . ? N8 H8N 0.9200 . ? C17 C19 1.500(10) . ? C17 C20 1.502(10) . ? C17 C18 1.513(10) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 H19A 0.9800 . ? C19 H19C 0.9800 . ? C19 H19E 0.9800 . ? C20 H20A 0.9800 . ? C20 H20C 0.9800 . ? C20 H20E 0.9800 . ? C21 C22 1.540(8) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C23 1.524(10) . ? C22 C24 1.530(9) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C26 1.484(9) . ? C25 C27 1.488(10) . ? C25 C28 1.526(10) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 C30 1.502(9) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 C31 1.513(9) . ? C30 C32 1.516(9) . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 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 N5 Cu1 N7 172.8(2) . . ? N5 Cu1 N6 83.0(2) . . ? N7 Cu1 N6 90.6(2) . . ? N5 Cu1 N8 94.5(2) . . ? N7 Cu1 N8 82.8(2) . . ? N6 Cu1 N8 96.5(2) . . ? N5 Cu1 Cl2 94.7(2) . . ? N7 Cu1 Cl2 92.30(15) . . ? N6 Cu1 Cl2 136.80(19) . . ? N8 Cu1 Cl2 126.67(15) . . ? C5 N1 C2 116.0(6) . . ? C5 N1 C1 118.9(6) . . ? C2 N1 C1 58.7(4) . . ? C5 N1 Cu2 106.8(5) . . ? C2 N1 Cu2 126.0(4) . . ? C1 N1 Cu2 124.3(4) . . ? C6 N2 Cu2 106.5(4) . . ? C6 N2 H1N 110.4 . . ? Cu2 N2 H1N 110.4 . . ? C6 N2 H2N 110.4 . . ? Cu2 N2 H2N 110.4 . . ? H1N N2 H2N 108.6 . . ? C13 N3 C10 114.4(6) . . ? C13 N3 C9 117.0(5) . . ? C10 N3 C9 59.1(4) . . ? C13 N3 Cu2 107.8(4) . . ? C10 N3 Cu2 123.7(4) . . ? C9 N3 Cu2 127.6(4) . . ? C14 N4 Cu2 107.6(4) . . ? C14 N4 H3N 110.2 . . ? Cu2 N4 H3N 110.2 . . ? C14 N4 H4N 110.2 . . ? Cu2 N4 H4N 110.2 . . ? H3N N4 H4N 108.5 . . ? C2 C1 C3 119.5(6) . . ? C2 C1 C4 119.0(6) . . ? C3 C1 C4 114.0(5) . . ? C2 C1 N1 59.6(4) . . ? C3 C1 N1 118.7(6) . . ? C4 C1 N1 115.5(6) . . ? C1 C2 N1 61.8(4) . . ? C1 C2 H2A 117.6 . . ? N1 C2 H2A 117.6 . . ? C1 C2 H2B 117.6 . . ? N1 C2 H2B 117.6 . . ? H2A C2 H2B 114.7 . . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C1 C4 H4A 109.5 . . ? C1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N1 C5 C6 110.4(8) . . ? N1 C5 H5A 109.6 . . ? C6 C5 H5A 109.6 . . ? N1 C5 H5B 109.6 . . ? C6 C5 H5B 109.6 . . ? H5A C5 H5B 108.1 . . ? N2 C6 C8 107.3(6) . . ? N2 C6 C5 104.8(6) . . ? C8 C6 C5 112.3(6) . . ? N2 C6 C7 111.6(6) . . ? C8 C6 C7 111.3(6) . . ? C5 C6 C7 109.3(7) . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C6 C8 H8A 109.5 . . ? C6 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C6 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C10 C9 C11 119.5(7) . . ? C10 C9 C12 118.5(6) . . ? C11 C9 C12 115.2(6) . . ? C10 C9 N3 59.0(4) . . ? C11 C9 N3 118.8(6) . . ? C12 C9 N3 114.1(6) . . ? N3 C10 C9 61.9(4) . . ? N3 C10 H10A 117.6 . . ? C9 C10 H10A 117.6 . . ? N3 C10 H10B 117.6 . . ? C9 C10 H10B 117.6 . . ? H10A C10 H10B 114.7 . . ? C9 C11 H11A 109.5 . . ? C9 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C9 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C9 C12 H12A 109.5 . . ? C9 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C9 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N3 C13 C14 110.0(5) . . ? N3 C13 H13A 109.7 . . ? C14 C13 H13A 109.7 . . ? N3 C13 H13B 109.7 . . ? C14 C13 H13B 109.7 . . ? H13A C13 H13B 108.2 . . ? N4 C14 C13 104.8(5) . . ? N4 C14 C15 111.6(6) . . ? C13 C14 C15 109.5(6) . . ? N4 C14 C16 108.6(6) . . ? C13 C14 C16 111.7(6) . . ? C15 C14 C16 110.6(6) . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C14 C16 H16A 109.5 . . ? C14 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C14 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N1 Cu2 N3 172.6(2) . . ? N1 Cu2 N4 91.0(2) . . ? N3 Cu2 N4 82.6(2) . . ? N1 Cu2 N2 83.3(2) . . ? N3 Cu2 N2 93.7(2) . . ? N4 Cu2 N2 96.2(2) . . ? N1 Cu2 Cl3 92.65(16) . . ? N3 Cu2 Cl3 94.54(19) . . ? N4 Cu2 Cl3 136.37(19) . . ? N2 Cu2 Cl3 127.45(16) . . ? C21 N5 C18 115.2(6) . . ? C21 N5 C17 117.1(5) . . ? C18 N5 C17 60.3(4) . . ? C21 N5 Cu1 107.9(4) . . ? C18 N5 Cu1 124.1(4) . . ? C17 N5 Cu1 125.6(4) . . ? C22 N6 Cu1 107.9(4) . . ? C22 N6 H5N 110.1 . . ? Cu1 N6 H5N 110.1 . . ? C22 N6 H6N 110.1 . . ? Cu1 N6 H6N 110.1 . . ? H5N N6 H6N 108.4 . . ? C26 N7 C29 115.1(5) . . ? C26 N7 C25 59.2(4) . . ? C29 N7 C25 118.9(6) . . ? C26 N7 Cu1 125.9(4) . . ? C29 N7 Cu1 106.4(4) . . ? C25 N7 Cu1 125.3(4) . . ? C30 N8 Cu1 107.5(4) . . ? C30 N8 H7N 110.2 . . ? Cu1 N8 H7N 110.2 . . ? C30 N8 H8N 110.2 . . ? Cu1 N8 H8N 110.2 . . ? H7N N8 H8N 108.5 . . ? C19 C17 C20 114.3(6) . . ? C19 C17 C18 118.8(7) . . ? C20 C17 C18 118.5(7) . . ? C19 C17 N5 116.0(6) . . ? C20 C17 N5 119.2(6) . . ? C18 C17 N5 59.1(4) . . ? N5 C18 C17 60.5(4) . . ? N5 C18 H18A 117.7 . . ? C17 C18 H18A 117.7 . . ? N5 C18 H18B 117.7 . . ? C17 C18 H18B 117.7 . . ? H18A C18 H18B 114.8 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? C17 C19 H19E 109.5 . . ? H19A C19 H19E 109.5 . . ? H19C C19 H19E 109.5 . . ? C17 C20 H20A 109.5 . . ? C17 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? C17 C20 H20E 109.5 . . ? H20A C20 H20E 109.5 . . ? H20C C20 H20E 109.5 . . ? N5 C21 C22 108.8(5) . . ? N5 C21 H21A 109.9 . . ? C22 C21 H21A 109.9 . . ? N5 C21 H21B 109.9 . . ? C22 C21 H21B 109.9 . . ? H21A C21 H21B 108.3 . . ? N6 C22 C23 108.5(6) . . ? N6 C22 C24 112.8(5) . . ? C23 C22 C24 110.3(6) . . ? N6 C22 C21 105.3(6) . . ? C23 C22 C21 111.2(6) . . ? C24 C22 C21 108.7(5) . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C26 C25 C27 121.3(7) . . ? C26 C25 N7 59.8(4) . . ? C27 C25 N7 121.2(6) . . ? C26 C25 C28 117.7(6) . . ? C27 C25 C28 113.2(5) . . ? N7 C25 C28 113.6(6) . . ? C25 C26 N7 60.9(4) . . ? C25 C26 H26A 117.7 . . ? N7 C26 H26A 117.7 . . ? C25 C26 H26B 117.7 . . ? N7 C26 H26B 117.7 . . ? H26A C26 H26B 114.8 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C25 C28 H28A 109.5 . . ? C25 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C25 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? N7 C29 C30 110.7(7) . . ? N7 C29 H29A 109.5 . . ? C30 C29 H29A 109.5 . . ? N7 C29 H29B 109.5 . . ? C30 C29 H29B 109.5 . . ? H29A C29 H29B 108.1 . . ? N8 C30 C29 105.4(6) . . ? N8 C30 C31 107.6(6) . . ? C29 C30 C31 112.8(5) . . ? N8 C30 C32 111.6(5) . . ? C29 C30 C32 108.0(6) . . ? C31 C30 C32 111.3(6) . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C30 C32 H32A 109.5 . . ? C30 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C30 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 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 C5 N1 C1 C2 104.4(7) . . . . ? Cu2 N1 C1 C2 -114.6(5) . . . . ? C5 N1 C1 C3 -4.9(9) . . . . ? C2 N1 C1 C3 -109.3(7) . . . . ? Cu2 N1 C1 C3 136.1(5) . . . . ? C5 N1 C1 C4 -145.5(6) . . . . ? C2 N1 C1 C4 110.0(7) . . . . ? Cu2 N1 C1 C4 -4.6(8) . . . . ? C3 C1 C2 N1 107.9(6) . . . . ? C4 C1 C2 N1 -104.2(6) . . . . ? C5 N1 C2 C1 -109.5(6) . . . . ? Cu2 N1 C2 C1 111.9(5) . . . . ? C2 N1 C5 C6 -101.2(7) . . . . ? C1 N1 C5 C6 -168.2(6) . . . . ? Cu2 N1 C5 C6 44.8(7) . . . . ? Cu2 N2 C6 C8 -77.2(5) . . . . ? Cu2 N2 C6 C5 42.3(6) . . . . ? Cu2 N2 C6 C7 160.6(5) . . . . ? N1 C5 C6 N2 -59.8(7) . . . . ? N1 C5 C6 C8 56.4(9) . . . . ? N1 C5 C6 C7 -179.5(6) . . . . ? C13 N3 C9 C10 103.6(7) . . . . ? Cu2 N3 C9 C10 -110.8(6) . . . . ? C13 N3 C9 C11 -5.4(10) . . . . ? C10 N3 C9 C11 -109.0(8) . . . . ? Cu2 N3 C9 C11 140.2(6) . . . . ? C13 N3 C9 C12 -146.4(7) . . . . ? C10 N3 C9 C12 110.0(7) . . . . ? Cu2 N3 C9 C12 -0.8(9) . . . . ? C13 N3 C10 C9 -108.0(6) . . . . ? Cu2 N3 C10 C9 117.1(5) . . . . ? C11 C9 C10 N3 107.7(7) . . . . ? C12 C9 C10 N3 -102.4(7) . . . . ? C10 N3 C13 C14 -99.9(7) . . . . ? C9 N3 C13 C14 -166.2(6) . . . . ? Cu2 N3 C13 C14 41.8(7) . . . . ? Cu2 N4 C14 C13 44.2(6) . . . . ? Cu2 N4 C14 C15 162.6(4) . . . . ? Cu2 N4 C14 C16 -75.3(5) . . . . ? N3 C13 C14 N4 -58.0(8) . . . . ? N3 C13 C14 C15 -177.8(6) . . . . ? N3 C13 C14 C16 59.4(9) . . . . ? C5 N1 Cu2 N3 50.8(19) . . . . ? C2 N1 Cu2 N3 -167.6(16) . . . . ? C1 N1 Cu2 N3 -94.0(18) . . . . ? C5 N1 Cu2 N4 80.9(5) . . . . ? C2 N1 Cu2 N4 -137.5(5) . . . . ? C1 N1 Cu2 N4 -63.9(5) . . . . ? C5 N1 Cu2 N2 -15.2(5) . . . . ? C2 N1 Cu2 N2 126.5(5) . . . . ? C1 N1 Cu2 N2 -160.0(5) . . . . ? C5 N1 Cu2 Cl3 -142.6(4) . . . . ? C2 N1 Cu2 Cl3 -0.9(5) . . . . ? C1 N1 Cu2 Cl3 72.6(5) . . . . ? C13 N3 Cu2 N1 17.9(19) . . . . ? C10 N3 Cu2 N1 155.2(16) . . . . ? C9 N3 Cu2 N1 -130.2(16) . . . . ? C13 N3 Cu2 N4 -12.5(4) . . . . ? C10 N3 Cu2 N4 124.9(5) . . . . ? C9 N3 Cu2 N4 -160.5(5) . . . . ? C13 N3 Cu2 N2 83.3(4) . . . . ? C10 N3 Cu2 N2 -139.4(5) . . . . ? C9 N3 Cu2 N2 -64.8(6) . . . . ? C13 N3 Cu2 Cl3 -148.7(4) . . . . ? C10 N3 Cu2 Cl3 -11.3(5) . . . . ? C9 N3 Cu2 Cl3 63.3(5) . . . . ? C14 N4 Cu2 N1 165.2(4) . . . . ? C14 N4 Cu2 N3 -18.5(4) . . . . ? C14 N4 Cu2 N2 -111.4(4) . . . . ? C14 N4 Cu2 Cl3 70.3(5) . . . . ? C6 N2 Cu2 N1 -16.2(4) . . . . ? C6 N2 Cu2 N3 170.5(4) . . . . ? C6 N2 Cu2 N4 -106.5(4) . . . . ? C6 N2 Cu2 Cl3 72.0(5) . . . . ? N7 Cu1 N5 C21 16(2) . . . . ? N6 Cu1 N5 C21 -12.1(4) . . . . ? N8 Cu1 N5 C21 83.8(4) . . . . ? Cl2 Cu1 N5 C21 -148.8(4) . . . . ? N7 Cu1 N5 C18 155.0(16) . . . . ? N6 Cu1 N5 C18 127.3(5) . . . . ? N8 Cu1 N5 C18 -136.7(5) . . . . ? Cl2 Cu1 N5 C18 -9.3(5) . . . . ? N7 Cu1 N5 C17 -129.5(17) . . . . ? N6 Cu1 N5 C17 -157.2(5) . . . . ? N8 Cu1 N5 C17 -61.2(5) . . . . ? Cl2 Cu1 N5 C17 66.2(5) . . . . ? N5 Cu1 N6 C22 -19.2(4) . . . . ? N7 Cu1 N6 C22 164.1(4) . . . . ? N8 Cu1 N6 C22 -113.0(4) . . . . ? Cl2 Cu1 N6 C22 70.1(5) . . . . ? N5 Cu1 N7 C26 -165.8(16) . . . . ? N6 Cu1 N7 C26 -138.4(5) . . . . ? N8 Cu1 N7 C26 125.2(5) . . . . ? Cl2 Cu1 N7 C26 -1.5(5) . . . . ? N5 Cu1 N7 C29 54.8(19) . . . . ? N6 Cu1 N7 C29 82.3(4) . . . . ? N8 Cu1 N7 C29 -14.1(4) . . . . ? Cl2 Cu1 N7 C29 -140.8(4) . . . . ? N5 Cu1 N7 C25 -91.0(18) . . . . ? N6 Cu1 N7 C25 -63.5(5) . . . . ? N8 Cu1 N7 C25 -160.0(5) . . . . ? Cl2 Cu1 N7 C25 73.4(5) . . . . ? N5 Cu1 N8 C30 170.6(4) . . . . ? N7 Cu1 N8 C30 -16.2(4) . . . . ? N6 Cu1 N8 C30 -106.0(4) . . . . ? Cl2 Cu1 N8 C30 71.3(4) . . . . ? C21 N5 C17 C19 -145.4(7) . . . . ? C18 N5 C17 C19 109.5(8) . . . . ? Cu1 N5 C17 C19 -3.1(9) . . . . ? C21 N5 C17 C20 -2.6(10) . . . . ? C18 N5 C17 C20 -107.6(8) . . . . ? Cu1 N5 C17 C20 139.7(6) . . . . ? C21 N5 C17 C18 105.1(7) . . . . ? Cu1 N5 C17 C18 -112.7(6) . . . . ? C21 N5 C18 C17 -108.1(6) . . . . ? Cu1 N5 C18 C17 115.1(5) . . . . ? C19 C17 C18 N5 -104.7(7) . . . . ? C20 C17 C18 N5 108.8(7) . . . . ? C18 N5 C21 C22 -102.9(7) . . . . ? C17 N5 C21 C22 -170.9(6) . . . . ? Cu1 N5 C21 C22 40.6(7) . . . . ? Cu1 N6 C22 C23 -74.2(5) . . . . ? Cu1 N6 C22 C24 163.3(4) . . . . ? Cu1 N6 C22 C21 44.9(6) . . . . ? N5 C21 C22 N6 -57.6(8) . . . . ? N5 C21 C22 C23 59.7(9) . . . . ? N5 C21 C22 C24 -178.7(6) . . . . ? C29 N7 C25 C26 103.6(6) . . . . ? Cu1 N7 C25 C26 -114.5(5) . . . . ? C26 N7 C25 C27 -110.5(8) . . . . ? C29 N7 C25 C27 -6.9(9) . . . . ? Cu1 N7 C25 C27 135.1(6) . . . . ? C26 N7 C25 C28 109.4(7) . . . . ? C29 N7 C25 C28 -147.0(6) . . . . ? Cu1 N7 C25 C28 -5.0(7) . . . . ? C27 C25 C26 N7 110.4(7) . . . . ? C28 C25 C26 N7 -102.6(6) . . . . ? C29 N7 C26 C25 -110.1(6) . . . . ? Cu1 N7 C26 C25 113.6(6) . . . . ? C26 N7 C29 C30 -100.7(6) . . . . ? C25 N7 C29 C30 -168.0(5) . . . . ? Cu1 N7 C29 C30 43.6(6) . . . . ? Cu1 N8 C30 C29 42.5(5) . . . . ? Cu1 N8 C30 C31 -78.1(5) . . . . ? Cu1 N8 C30 C32 159.5(4) . . . . ? N7 C29 C30 N8 -58.6(6) . . . . ? N7 C29 C30 C31 58.6(9) . . . . ? N7 C29 C30 C32 -178.0(5) . . . . ? loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag ? ? ? ? ? ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N2 H1N Cl1 0.92 2.52 3.403(6) 161.2 3_455 N2 H2N Cl4 0.92 2.69 3.416(5) 136.0 . N4 H3N Cl1 0.92 2.54 3.442(6) 165.5 3_455 N4 H4N Cl4 0.92 2.66 3.394(5) 137.2 1_545 N6 H5N Cl4 0.92 2.54 3.446(6) 167.5 3_565 N6 H6N Cl1 0.92 2.64 3.380(5) 137.9 . N8 H7N Cl4 0.92 2.54 3.423(5) 160.3 3_565 N8 H8N Cl1 0.92 2.72 3.429(5) 134.3 1_565 _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. ; #===END data_5d_CCDC-000000 _database_code_depnum_ccdc_archive 'CCDC 849023' #TrackingRef 'DTrans. aziridine.cif' # CCDC: 000000 # Messcode: ln268 _audit_author_name 's. Wirth, P. Mayer' _audit_block_code ? _audit_creation_method SHELXL-97 _audit_creation_date 31-May-07 _chemical_name_systematic Trans-bis[(2H-phenylazirine)dichlorido]palladium(II) _chemical_name_common ? _chemical_formula_moiety 'C16 H14 Cl2 N2 Pd' _chemical_formula_sum 'C16 H14 Cl2 N2 Pd' _chemical_compound_source ? _exptl_crystal_recrystallization_method 'slow isothermic diffusion of n-pentane into a solution in dichloromethane' _chemical_melting_point ? _exptl_crystal_description rod _exptl_crystal_colour yellow _diffrn_ambient_temperature 200(2) _chemical_formula_weight 411.62 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 orthorhombic _symmetry_space_group_name_H-M 'P c a 21' _symmetry_Int_Tables_number 29 _chemical_absolute_configuration unk _symmetry_space_group_name_Hall P2c-2ac loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y, z' '-x+1/2, y, z+1/2' _cell_length_a 21.4333(5) _cell_length_b 5.64490(10) _cell_length_c 12.6506(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1530.58(6) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 12836 _cell_measurement_theta_min 3.134 _cell_measurement_theta_max 27.485 _cell_special_details ? _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.78631 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 816 _exptl_absorpt_coefficient_mu 1.554 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ? loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0 0 1 0.010000 0 0 -1 0.010000 0 -1 0 0.037000 0 1 0 0.013000 1 0 0 0.088000 -15 -1 0 0.091000 _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'rotating anode X-ray tube' _diffrn_source_type ? _diffrn_source_power 3.025 _diffrn_source_voltage 55.00 _diffrn_source_current 55.00 _diffrn_radiation_monochromator graphite _diffrn_radiation_collimation 0.25 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD; rotation images; thick slices' _diffrn_detector_area_resol_mean 9 _kl_diffrn_measurement_scan_angle omega-scan _kl_diffrn_measurement_scan_step_degree 1.50 _kl_diffrn_measurement_scan_time_per_degree 20 _kl_diffrn_measurement_detector_distance 30 _diffrn_special_details ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3291 _diffrn_reflns_av_R_equivalents 0.0410 _diffrn_reflns_av_sigmaI/netI 0.0331 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.61 _diffrn_reflns_theta_max 27.48 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 2.186 _refine_diff_density_min -0.618 _refine_diff_density_rms 0.095 _reflns_number_total 3291 _reflns_number_gt 2689 _reflns_threshold_expression >2sigma(I) _reflns_special_details ? _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; Ortep-3 for Windows: L. J. Farrugia, J. Appl. Cryst. 1997, 30, 565 ; _computing_publication_material ? _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^)+(0.0408P)^2^+1.2123P] 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 0.47(7) _refine_ls_number_reflns 3291 _refine_ls_number_parameters 191 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0473 _refine_ls_R_factor_gt 0.0322 _refine_ls_wR_factor_ref 0.0808 _refine_ls_wR_factor_gt 0.0730 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.049 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_special_details ; Rint determined directly on diffractometer. 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. ; 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 0.372883(11) 0.25123(6) 0.57356(11) 0.02077(9) Uani 1 1 d . . . Cl1 Cl 0.40395(5) 0.4197(2) 0.41652(8) 0.0331(2) Uani 1 1 d . . . Cl2 Cl 0.34284(5) 0.0807(2) 0.73024(8) 0.0332(2) Uani 1 1 d . . . N1 N 0.42105(19) 0.4870(6) 0.6579(4) 0.0270(10) Uani 1 1 d . . . N2 N 0.32473(18) 0.0163(6) 0.4918(4) 0.0255(9) Uani 1 1 d . . . C1 C 0.4307(2) 0.5467(9) 0.7726(4) 0.0331(11) Uani 1 1 d . . . H1A H 0.3968 0.6291 0.8112 0.040 Uiso 1 1 calc R . . H1B H 0.4581 0.4437 0.8157 0.040 Uiso 1 1 calc R . . C2 C 0.4563(2) 0.6571(8) 0.6774(4) 0.0260(9) Uani 1 1 d . . . C3 C 0.4961(2) 0.8393(9) 0.6338(4) 0.0242(9) Uani 1 1 d . . . C4 C 0.5233(2) 1.0008(8) 0.7022(5) 0.0297(14) Uani 1 1 d . . . H4 H 0.5169 0.9871 0.7762 0.036 Uiso 1 1 calc R . . C5 C 0.5597(2) 1.1815(9) 0.6624(4) 0.0309(10) Uani 1 1 d . . . H5 H 0.5778 1.2939 0.7091 0.037 Uiso 1 1 calc R . . C6 C 0.5699(2) 1.1993(9) 0.5559(5) 0.0374(14) Uani 1 1 d . . . H6 H 0.5943 1.3259 0.5287 0.045 Uiso 1 1 calc R . . C7 C 0.5446(2) 1.0328(10) 0.4875(5) 0.0347(13) Uani 1 1 d . . . H7 H 0.5534 1.0421 0.4140 0.042 Uiso 1 1 calc R . . C8 C 0.5067(2) 0.8539(10) 0.5252(4) 0.0329(12) Uani 1 1 d . . . H8 H 0.4883 0.7429 0.4782 0.040 Uiso 1 1 calc R . . C9 C 0.3115(2) -0.0463(9) 0.3770(4) 0.0317(11) Uani 1 1 d . . . H9A H 0.2832 0.0570 0.3358 0.038 Uiso 1 1 calc R . . H9B H 0.3441 -0.1301 0.3360 0.038 Uiso 1 1 calc R . . C10 C 0.28811(19) -0.1557(8) 0.4744(3) 0.0255(9) Uani 1 1 d . . . C11 C 0.2496(2) -0.3366(9) 0.5214(4) 0.0252(10) Uani 1 1 d . . . C12 C 0.2395(2) -0.3505(10) 0.6302(4) 0.0267(10) Uani 1 1 d . . . H12 H 0.2582 -0.2387 0.6765 0.032 Uiso 1 1 calc R . . C13 C 0.2020(2) -0.5276(9) 0.6700(5) 0.0310(12) Uani 1 1 d . . . H13 H 0.1943 -0.5367 0.7438 0.037 Uiso 1 1 calc R . . C14 C 0.1756(2) -0.6920(9) 0.6027(4) 0.0298(12) Uani 1 1 d . . . H14 H 0.1506 -0.8157 0.6311 0.036 Uiso 1 1 calc R . . C15 C 0.1848(2) -0.6794(9) 0.4947(4) 0.0320(11) Uani 1 1 d . . . H15 H 0.1662 -0.7933 0.4492 0.038 Uiso 1 1 calc R . . C16 C 0.2212(2) -0.4994(8) 0.4533(5) 0.0281(14) Uani 1 1 d . . . H16 H 0.2269 -0.4865 0.3790 0.034 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 0.02246(14) 0.02036(14) 0.01947(14) 0.00002(10) 0.00015(16) -0.00124(10) Cl1 0.0410(6) 0.0353(6) 0.0229(5) 0.0051(5) -0.0011(5) -0.0095(5) Cl2 0.0412(6) 0.0352(6) 0.0231(5) 0.0007(5) 0.0008(5) -0.0108(5) N1 0.034(2) 0.027(2) 0.020(2) 0.0021(15) 0.0021(18) -0.0040(16) N2 0.0310(19) 0.027(2) 0.018(2) 0.0015(15) 0.0021(17) -0.0007(15) C1 0.044(3) 0.033(3) 0.023(3) -0.003(2) -0.005(2) -0.011(2) C2 0.027(2) 0.026(2) 0.025(2) 0.0022(19) 0.0030(18) 0.0018(19) C3 0.024(2) 0.024(2) 0.025(2) 0.000(2) -0.0002(17) 0.0016(19) C4 0.026(2) 0.037(4) 0.026(3) -0.0021(18) 0.0036(19) -0.0010(19) C5 0.026(2) 0.028(2) 0.039(3) -0.003(2) -0.001(2) -0.0052(19) C6 0.034(2) 0.032(2) 0.046(4) 0.008(2) -0.001(2) -0.0054(18) C7 0.035(3) 0.046(3) 0.023(3) 0.010(2) -0.004(2) -0.006(2) C8 0.033(3) 0.036(3) 0.030(3) -0.001(2) -0.006(2) -0.009(2) C9 0.041(3) 0.035(2) 0.019(2) -0.001(2) 0.000(2) -0.011(2) C10 0.027(2) 0.028(2) 0.022(2) -0.0026(19) 0.0008(18) 0.0046(19) C11 0.026(2) 0.018(2) 0.032(2) 0.001(2) 0.0056(19) 0.0000(19) C12 0.030(2) 0.029(3) 0.021(2) 0.001(2) -0.0031(18) 0.002(2) C13 0.030(2) 0.035(3) 0.028(3) 0.004(2) -0.001(2) 0.000(2) C14 0.027(2) 0.026(2) 0.036(3) 0.0066(19) 0.0027(18) -0.0011(17) C15 0.032(2) 0.028(2) 0.036(3) -0.009(2) 0.000(2) -0.007(2) C16 0.036(3) 0.025(3) 0.023(3) -0.0037(17) 0.000(2) 0.0016(19) 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 1.973(4) . ? Pd1 N1 1.994(4) . ? Pd1 Cl2 2.2957(15) . ? Pd1 Cl1 2.3009(15) . ? N1 C2 1.245(6) . ? N1 C1 1.504(7) . ? N2 C10 1.268(6) . ? N2 C9 1.521(7) . ? C1 C2 1.463(7) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C3 1.447(7) . ? C3 C4 1.385(7) . ? C3 C8 1.394(7) . ? C4 C5 1.379(7) . ? C4 H4 0.9500 . ? C5 C6 1.369(8) . ? C5 H5 0.9500 . ? C6 C7 1.388(8) . ? C6 H6 0.9500 . ? C7 C8 1.381(7) . ? C7 H7 0.9500 . ? C8 H8 0.9500 . ? C9 C10 1.467(7) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C11 1.441(7) . ? C11 C12 1.395(6) . ? C11 C16 1.400(7) . ? C12 C13 1.377(7) . ? C12 H12 0.9500 . ? C13 C14 1.380(8) . ? C13 H13 0.9500 . ? C14 C15 1.382(8) . ? C14 H14 0.9500 . ? C15 C16 1.384(7) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? 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 179.3(3) . . ? N2 Pd1 Cl2 91.39(14) . . ? N1 Pd1 Cl2 87.89(15) . . ? N2 Pd1 Cl1 88.63(14) . . ? N1 Pd1 Cl1 92.09(14) . . ? Cl2 Pd1 Cl1 179.38(5) . . ? C2 N1 C1 63.5(3) . . ? C2 N1 Pd1 159.0(4) . . ? C1 N1 Pd1 137.5(3) . . ? C10 N2 C9 62.7(3) . . ? C10 N2 Pd1 158.3(4) . . ? C9 N2 Pd1 138.9(3) . . ? C2 C1 N1 49.6(3) . . ? C2 C1 H1A 118.7 . . ? N1 C1 H1A 118.7 . . ? C2 C1 H1B 118.7 . . ? N1 C1 H1B 118.7 . . ? H1A C1 H1B 116.1 . . ? N1 C2 C3 146.1(5) . . ? N1 C2 C1 66.9(3) . . ? C3 C2 C1 147.0(4) . . ? C4 C3 C8 120.5(5) . . ? C4 C3 C2 118.5(5) . . ? C8 C3 C2 120.9(5) . . ? C5 C4 C3 119.8(5) . . ? C5 C4 H4 120.1 . . ? C3 C4 H4 120.1 . . ? C6 C5 C4 120.2(5) . . ? C6 C5 H5 119.9 . . ? C4 C5 H5 119.9 . . ? C5 C6 C7 120.1(5) . . ? C5 C6 H6 119.9 . . ? C7 C6 H6 119.9 . . ? C8 C7 C6 120.6(6) . . ? C8 C7 H7 119.7 . . ? C6 C7 H7 119.7 . . ? C7 C8 C3 118.7(5) . . ? C7 C8 H8 120.7 . . ? C3 C8 H8 120.7 . . ? C10 C9 N2 50.2(3) . . ? C10 C9 H9A 118.7 . . ? N2 C9 H9A 118.7 . . ? C10 C9 H9B 118.7 . . ? N2 C9 H9B 118.7 . . ? H9A C9 H9B 116.0 . . ? N2 C10 C11 145.6(5) . . ? N2 C10 C9 67.1(3) . . ? C11 C10 C9 147.2(4) . . ? C12 C11 C16 120.2(5) . . ? C12 C11 C10 122.4(5) . . ? C16 C11 C10 117.4(4) . . ? C13 C12 C11 119.5(5) . . ? C13 C12 H12 120.3 . . ? C11 C12 H12 120.3 . . ? C12 C13 C14 120.1(6) . . ? C12 C13 H13 119.9 . . ? C14 C13 H13 119.9 . . ? C13 C14 C15 121.1(5) . . ? C13 C14 H14 119.5 . . ? C15 C14 H14 119.5 . . ? C14 C15 C16 119.5(5) . . ? C14 C15 H15 120.3 . . ? C16 C15 H15 120.3 . . ? C15 C16 C11 119.6(5) . . ? C15 C16 H16 120.2 . . ? C11 C16 H16 120.2 . . ? 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 C2 -175(100) . . . . ? Cl2 Pd1 N1 C2 177.0(10) . . . . ? Cl1 Pd1 N1 C2 -2.4(10) . . . . ? N2 Pd1 N1 C1 4(16) . . . . ? Cl2 Pd1 N1 C1 -4.5(5) . . . . ? Cl1 Pd1 N1 C1 176.1(5) . . . . ? N1 Pd1 N2 C10 -4(16) . . . . ? Cl2 Pd1 N2 C10 4.9(9) . . . . ? Cl1 Pd1 N2 C10 -175.7(9) . . . . ? N1 Pd1 N2 C9 173(100) . . . . ? Cl2 Pd1 N2 C9 -178.3(5) . . . . ? Cl1 Pd1 N2 C9 1.1(5) . . . . ? Pd1 N1 C1 C2 -179.4(6) . . . . ? C1 N1 C2 C3 179.4(9) . . . . ? Pd1 N1 C2 C3 -1.7(16) . . . . ? Pd1 N1 C2 C1 178.9(10) . . . . ? N1 C1 C2 C3 -179.4(9) . . . . ? N1 C2 C3 C4 176.4(7) . . . . ? C1 C2 C3 C4 -4.6(11) . . . . ? N1 C2 C3 C8 -3.2(11) . . . . ? C1 C2 C3 C8 175.8(7) . . . . ? C8 C3 C4 C5 1.9(8) . . . . ? C2 C3 C4 C5 -177.7(4) . . . . ? C3 C4 C5 C6 -1.1(7) . . . . ? C4 C5 C6 C7 -1.3(8) . . . . ? C5 C6 C7 C8 2.9(8) . . . . ? C6 C7 C8 C3 -2.1(8) . . . . ? C4 C3 C8 C7 -0.3(9) . . . . ? C2 C3 C8 C7 179.3(4) . . . . ? Pd1 N2 C9 C10 -178.7(5) . . . . ? C9 N2 C10 C11 179.9(8) . . . . ? Pd1 N2 C10 C11 -2.4(15) . . . . ? Pd1 N2 C10 C9 177.7(10) . . . . ? N2 C9 C10 C11 -179.9(9) . . . . ? N2 C10 C11 C12 5.9(11) . . . . ? C9 C10 C11 C12 -174.3(7) . . . . ? N2 C10 C11 C16 -175.2(6) . . . . ? C9 C10 C11 C16 4.6(11) . . . . ? C16 C11 C12 C13 0.9(8) . . . . ? C10 C11 C12 C13 179.8(4) . . . . ? C11 C12 C13 C14 1.0(8) . . . . ? C12 C13 C14 C15 -1.6(8) . . . . ? C13 C14 C15 C16 0.2(8) . . . . ? C14 C15 C16 C11 1.7(8) . . . . ? C12 C11 C16 C15 -2.3(8) . . . . ? C10 C11 C16 C15 178.7(4) . . . . ? loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag ? ? ? ? ? ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A ? ? ? ? ? ? ? ? _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. ; #===END