data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Dr Jason Love' _publ_contact_author_email jason.love@ed.ac.uk _publ_section_title ; Chlorometallate and palladium cluster complexes of wide-span diimine and diamine ligands ; _publ_author_name J.Love # Attachment '- combined.cif' data_j11005b _database_code_depnum_ccdc_archive 'CCDC 824566' #TrackingRef '- combined.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H48 N2' _chemical_formula_sum 'C36 H48 N2' _chemical_formula_weight 508.76 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.4355(9) _cell_length_b 23.1135(12) _cell_length_c 9.0064(9) _cell_angle_alpha 90.00 _cell_angle_beta 117.123(13) _cell_angle_gamma 90.00 _cell_volume 1562.9(2) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 1793 _cell_measurement_theta_min 3.2292 _cell_measurement_theta_max 29.8933 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.2483950 _exptl_crystal_size_mid 0.1035049 _exptl_crystal_size_min 0.0238892 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.081 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 556 _exptl_absorpt_coefficient_mu 0.062 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.89648 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.34.46 (release 25-11-2010 CrysAlis171 .NET) (compiled Nov 25 2010,17:55:46) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Eos' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.1042 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11022 _diffrn_reflns_av_R_equivalents 0.0306 _diffrn_reflns_av_sigmaI/netI 0.1036 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 3.24 _diffrn_reflns_theta_max 29.96 _reflns_number_total 3937 _reflns_number_gt 2837 _reflns_threshold_expression >2\s(I) _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.34.46 (release 25-11-2010 CrysAlis171 .NET) (compiled Nov 25 2010,17:55:46) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.34.46 (release 25-11-2010 CrysAlis171 .NET) (compiled Nov 25 2010,17:55:46) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.34.46 (release 25-11-2010 CrysAlis171 .NET) (compiled Nov 25 2010,17:55:46) ; _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Checkcif comments: 412_ALERT_2_B Short Intra XH3 .. XHn H17C .. H18C .. 1.73 Ang. This is an intramolecular contact involving methyl groups. There is not a completely unambiguous method to assign the orientations of these groups, and they were allowed to optimise using the Sheldrick rotating rigid body model (AFIX 137). 220_ALERT_2_C Large Non-Solvent C Ueq(max)/Ueq(min) ... 3.34 Ratio 242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C9 C9 is the pivot atom of a librating iPr group. 910_ALERT_3_C Missing # of FCF Reflections Below Th(Min) ..... 6 911_ALERT_3_C Missing # FCF Refl Between THmin & STh/L= 0.600 20 912_ALERT_4_C Missing # of FCF Reflections Above STh/L= 0.600 525 Coverage stats: Data are complete to 50 deg in 2theta. Section 4: #============================================================================== Resolution & Completeness Statistics (Cumulative and Friedel Pairs Averaged) #============================================================================== Theta sin(th)/Lambda Complete Expected Measured Missing #------------------------------------------------------------------------------ 20.82 0.500 0.996 1635 1629 6 23.01 0.550 0.994 2175 2161 14 25.24 0.600 0.991 2826 2800 26 #----------------------------------------------------------- ACTA Min. Res. --- 27.51 0.650 0.979 3590 3514 76 29.84 0.700 0.886 4437 3929 508 29.96 0.703 0.877 4488 3938 550 125_ALERT_4_C No '_symmetry_space_group_name_Hall' Given ..... ? No action taken 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^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0756P)^2^+0.7528P] 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_number_reflns 3937 _refine_ls_number_parameters 178 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0933 _refine_ls_R_factor_gt 0.0646 _refine_ls_wR_factor_ref 0.1759 _refine_ls_wR_factor_gt 0.1564 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.023 _refine_ls_shift/su_max 0.033 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.7437(3) 0.25072(10) 0.5127(3) 0.0533(6) Uani 1 1 d . . . H1A H 0.8571 0.2501 0.5073 0.080 Uiso 1 1 calc R . . H1B H 0.7571 0.2734 0.6097 0.080 Uiso 1 1 calc R . . H1C H 0.6517 0.2683 0.4108 0.080 Uiso 1 1 calc R . . C2 C 0.6893(3) 0.18856(8) 0.5290(2) 0.0330(4) Uani 1 1 d . . . H2 H 0.7894 0.1709 0.6294 0.040 Uiso 1 1 calc R . . C3 C 0.6656(3) 0.15308(11) 0.3781(3) 0.0539(6) Uani 1 1 d . . . H3A H 0.6416 0.1127 0.3942 0.081 Uiso 1 1 calc R . . H3B H 0.7746 0.1552 0.3649 0.081 Uiso 1 1 calc R . . H3C H 0.5654 0.1685 0.2779 0.081 Uiso 1 1 calc R . . C4 C 0.5231(2) 0.18541(7) 0.5544(2) 0.0263(4) Uani 1 1 d . . . C5 C 0.3909(3) 0.22739(8) 0.4902(2) 0.0349(4) Uani 1 1 d . . . H5 H 0.4046 0.2591 0.4299 0.042 Uiso 1 1 calc R . . C6 C 0.2394(3) 0.22375(8) 0.5128(3) 0.0395(5) Uani 1 1 d . . . H6 H 0.1509 0.2530 0.4690 0.047 Uiso 1 1 calc R . . C7 C 0.2171(2) 0.17778(8) 0.5984(2) 0.0354(4) Uani 1 1 d . . . H7 H 0.1124 0.1758 0.6128 0.042 Uiso 1 1 calc R . . C8 C 0.3444(2) 0.13396(7) 0.6647(2) 0.0277(4) Uani 1 1 d . . . C9 C 0.3129(3) 0.08301(8) 0.7554(2) 0.0362(4) Uani 1 1 d . . . H9 H 0.3995 0.0520 0.7641 0.043 Uiso 1 1 calc R . . C10 C 0.3515(4) 0.09925(13) 0.9318(3) 0.0711(8) Uani 1 1 d . . . H10A H 0.4747 0.1128 0.9928 0.107 Uiso 1 1 calc R . . H10B H 0.3346 0.0653 0.9883 0.107 Uiso 1 1 calc R . . H10C H 0.2701 0.1301 0.9282 0.107 Uiso 1 1 calc R . . C11 C 0.1270(4) 0.05739(14) 0.6611(4) 0.0785(9) Uani 1 1 d . . . H11A H 0.0395 0.0843 0.6654 0.118 Uiso 1 1 calc R . . H11B H 0.1214 0.0206 0.7125 0.118 Uiso 1 1 calc R . . H11C H 0.1004 0.0507 0.5446 0.118 Uiso 1 1 calc R . . C12 C 0.4986(2) 0.13863(7) 0.64283(19) 0.0242(3) Uani 1 1 d . . . C13 C 0.7307(2) 0.08736(7) 0.8495(2) 0.0312(4) Uani 1 1 d . . . H13 H 0.7179 0.1136 0.9246 0.037 Uiso 1 1 calc R . . C14 C 0.8687(2) 0.04184(7) 0.92310(19) 0.0236(3) Uani 1 1 d . . . C15 C 1.0163(2) 0.05430(7) 1.0764(2) 0.0250(4) Uani 1 1 d . . . C16 C 0.8507(2) -0.01264(7) 0.8462(2) 0.0281(4) Uani 1 1 d . . . C17 C 1.0362(3) 0.11345(8) 1.1565(3) 0.0456(5) Uani 1 1 d . . . H17A H 0.9689 0.1144 1.2209 0.068 Uiso 1 1 calc R . . H17B H 0.9902 0.1432 1.0694 0.068 Uiso 1 1 calc R . . H17C H 1.1624 0.1209 1.2307 0.068 Uiso 1 1 calc R . . C18 C 0.6892(3) -0.02736(9) 0.6852(3) 0.0563(7) Uani 1 1 d . . . H18A H 0.7067 -0.0135 0.5908 0.084 Uiso 1 1 calc R . . H18B H 0.5838 -0.0087 0.6831 0.084 Uiso 1 1 calc R . . H18C H 0.6720 -0.0694 0.6770 0.084 Uiso 1 1 calc R . . N1 N 0.6308(2) 0.09428(6) 0.69916(18) 0.0314(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 C1 0.0575(14) 0.0382(11) 0.0773(17) 0.0045(11) 0.0422(13) -0.0065(10) C2 0.0336(10) 0.0306(9) 0.0351(9) 0.0076(7) 0.0159(8) 0.0029(8) C3 0.0632(15) 0.0547(14) 0.0578(14) -0.0094(11) 0.0397(12) -0.0049(12) C4 0.0274(9) 0.0235(8) 0.0237(7) 0.0013(6) 0.0080(7) 0.0020(7) C5 0.0386(11) 0.0239(8) 0.0381(10) 0.0088(7) 0.0138(8) 0.0056(7) C6 0.0334(10) 0.0303(9) 0.0480(11) 0.0067(8) 0.0125(9) 0.0133(8) C7 0.0289(9) 0.0357(10) 0.0412(10) -0.0028(8) 0.0156(8) 0.0020(8) C8 0.0302(9) 0.0242(8) 0.0267(8) -0.0027(6) 0.0111(7) -0.0023(7) C9 0.0373(10) 0.0324(9) 0.0429(10) 0.0021(8) 0.0217(9) -0.0046(8) C10 0.101(2) 0.0747(18) 0.0525(14) -0.0010(13) 0.0482(16) -0.0241(16) C11 0.0628(17) 0.0702(18) 0.086(2) 0.0136(16) 0.0197(15) -0.0352(15) C12 0.0267(9) 0.0196(7) 0.0211(7) -0.0007(6) 0.0064(7) 0.0028(6) C13 0.0304(9) 0.0233(8) 0.0305(9) -0.0048(7) 0.0058(7) 0.0036(7) C14 0.0246(8) 0.0198(7) 0.0225(7) 0.0013(6) 0.0075(6) 0.0013(6) C15 0.0267(9) 0.0188(7) 0.0245(8) -0.0010(6) 0.0073(7) 0.0003(6) C16 0.0290(9) 0.0220(8) 0.0253(8) -0.0025(6) 0.0055(7) 0.0012(7) C17 0.0426(12) 0.0274(9) 0.0426(11) -0.0127(8) -0.0015(9) 0.0077(8) C18 0.0518(14) 0.0327(10) 0.0439(12) -0.0130(9) -0.0133(10) 0.0139(9) N1 0.0370(9) 0.0250(7) 0.0261(7) 0.0028(6) 0.0090(6) 0.0091(6) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.536(3) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C3 1.521(3) . ? C2 C4 1.521(2) . ? C2 H2 1.0000 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 C5 1.390(2) . ? C4 C12 1.413(2) . ? C5 C6 1.385(3) . ? C5 H5 0.9500 . ? C6 C7 1.376(3) . ? C6 H6 0.9500 . ? C7 C8 1.397(3) . ? C7 H7 0.9500 . ? C8 C12 1.406(2) . ? C8 C9 1.524(2) . ? C9 C10 1.516(3) . ? C9 C11 1.522(3) . ? C9 H9 1.0000 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 N1 1.427(2) . ? C13 N1 1.236(2) . ? C13 C14 1.483(2) . ? C13 H13 0.9500 . ? C14 C15 1.404(2) . ? C14 C16 1.411(2) . ? C15 C16 1.399(2) 3_757 ? C15 C17 1.519(2) . ? C16 C15 1.399(2) 3_757 ? C16 C18 1.508(3) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 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 C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C3 C2 C4 110.73(16) . . ? C3 C2 C1 110.01(18) . . ? C4 C2 C1 113.28(16) . . ? C3 C2 H2 107.5 . . ? C4 C2 H2 107.5 . . ? C1 C2 H2 107.5 . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C5 C4 C12 118.21(16) . . ? C5 C4 C2 121.59(15) . . ? C12 C4 C2 120.19(14) . . ? C6 C5 C4 121.04(17) . . ? C6 C5 H5 119.5 . . ? C4 C5 H5 119.5 . . ? C7 C6 C5 120.05(17) . . ? C7 C6 H6 120.0 . . ? C5 C6 H6 120.0 . . ? C6 C7 C8 121.65(17) . . ? C6 C7 H7 119.2 . . ? C8 C7 H7 119.2 . . ? C7 C8 C12 117.68(16) . . ? C7 C8 C9 120.10(16) . . ? C12 C8 C9 122.22(15) . . ? C10 C9 C11 110.8(2) . . ? C10 C9 C8 111.31(17) . . ? C11 C9 C8 112.87(18) . . ? C10 C9 H9 107.2 . . ? C11 C9 H9 107.2 . . ? C8 C9 H9 107.2 . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? 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 . . ? C8 C12 C4 121.36(15) . . ? C8 C12 N1 121.20(15) . . ? C4 C12 N1 117.31(15) . . ? N1 C13 C14 125.86(16) . . ? N1 C13 H13 117.1 . . ? C14 C13 H13 117.1 . . ? C15 C14 C16 120.93(14) . . ? C15 C14 C13 117.24(14) . . ? C16 C14 C13 121.79(15) . . ? C16 C15 C14 119.90(14) 3_757 . ? C16 C15 C17 119.54(15) 3_757 . ? C14 C15 C17 120.52(15) . . ? C15 C16 C14 119.16(15) 3_757 . ? C15 C16 C18 119.43(15) 3_757 . ? C14 C16 C18 121.39(15) . . ? 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 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C13 N1 C12 120.96(15) . . ? 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 C3 C2 C4 C5 -94.7(2) . . . . ? C1 C2 C4 C5 29.4(2) . . . . ? C3 C2 C4 C12 84.3(2) . . . . ? C1 C2 C4 C12 -151.56(18) . . . . ? C12 C4 C5 C6 0.3(3) . . . . ? C2 C4 C5 C6 179.37(18) . . . . ? C4 C5 C6 C7 -0.6(3) . . . . ? C5 C6 C7 C8 0.1(3) . . . . ? C6 C7 C8 C12 0.7(3) . . . . ? C6 C7 C8 C9 -178.59(18) . . . . ? C7 C8 C9 C10 -78.7(2) . . . . ? C12 C8 C9 C10 102.0(2) . . . . ? C7 C8 C9 C11 46.7(3) . . . . ? C12 C8 C9 C11 -132.6(2) . . . . ? C7 C8 C12 C4 -1.1(2) . . . . ? C9 C8 C12 C4 178.24(16) . . . . ? C7 C8 C12 N1 -176.74(15) . . . . ? C9 C8 C12 N1 2.6(2) . . . . ? C5 C4 C12 C8 0.6(2) . . . . ? C2 C4 C12 C8 -178.51(15) . . . . ? C5 C4 C12 N1 176.39(15) . . . . ? C2 C4 C12 N1 -2.7(2) . . . . ? N1 C13 C14 C15 152.37(19) . . . . ? N1 C13 C14 C16 -29.8(3) . . . . ? C16 C14 C15 C16 0.9(3) . . . 3_757 ? C13 C14 C15 C16 178.75(16) . . . 3_757 ? C16 C14 C15 C17 178.81(18) . . . . ? C13 C14 C15 C17 -3.4(3) . . . . ? C15 C14 C16 C15 -0.9(3) . . . 3_757 ? C13 C14 C16 C15 -178.64(16) . . . 3_757 ? C15 C14 C16 C18 177.44(19) . . . . ? C13 C14 C16 C18 -0.3(3) . . . . ? C14 C13 N1 C12 177.99(16) . . . . ? C8 C12 N1 C13 -72.7(2) . . . . ? C4 C12 N1 C13 111.4(2) . . . . ? _diffrn_measured_fraction_theta_max 0.866 _diffrn_reflns_theta_full 29.96 _diffrn_measured_fraction_theta_full 0.99 _refine_diff_density_max 0.410 _refine_diff_density_min -0.282 _refine_diff_density_rms 0.045 data_j11004c _database_code_depnum_ccdc_archive 'CCDC 824567' #TrackingRef '- combined.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H52 N2' _chemical_formula_sum 'C36 H52 N2' _chemical_formula_weight 512.80 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 1 2/c 1' 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' '-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 23.679(3) _cell_length_b 10.6920(10) _cell_length_c 26.106(4) _cell_angle_alpha 90.00 _cell_angle_beta 109.228(14) _cell_angle_gamma 90.00 _cell_volume 6240.7(12) _cell_formula_units_Z 8 _cell_measurement_temperature 171(2) _cell_measurement_reflns_used 4233 _cell_measurement_theta_min 3.2000 _cell_measurement_theta_max 30.0679 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.2240525 _exptl_crystal_size_mid 0.0931596 _exptl_crystal_size_min 0.0146693 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.092 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2256 _exptl_absorpt_coefficient_mu 0.062 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.33506 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.34.46 (release 25-11-2010 CrysAlis171 .NET) (compiled Nov 25 2010,17:55:46) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 171(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Eos' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.1042 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 40816 _diffrn_reflns_av_R_equivalents 0.0530 _diffrn_reflns_av_sigmaI/netI 0.0556 _diffrn_reflns_limit_h_min -33 _diffrn_reflns_limit_h_max 33 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 3.21 _diffrn_reflns_theta_max 30.13 _reflns_number_total 8429 _reflns_number_gt 5606 _reflns_threshold_expression >2\s(I) _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.34.46 (release 25-11-2010 CrysAlis171 .NET) (compiled Nov 25 2010,17:55:46) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.34.46 (release 25-11-2010 CrysAlis171 .NET) (compiled Nov 25 2010,17:55:46) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.34.46 (release 25-11-2010 CrysAlis171 .NET) (compiled Nov 25 2010,17:55:46) ; _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0728P)^2^+3.0089P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8429 _refine_ls_number_parameters 363 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1018 _refine_ls_R_factor_gt 0.0639 _refine_ls_wR_factor_ref 0.1708 _refine_ls_wR_factor_gt 0.1489 _refine_ls_goodness_of_fit_ref 1.011 _refine_ls_restrained_S_all 1.011 _refine_ls_shift/su_max 0.056 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.47495(9) 0.2532(2) -0.17745(9) 0.0544(5) Uani 1 1 d . . . H1A H 0.4629 0.1793 -0.1614 0.082 Uiso 1 1 calc R . . H1B H 0.5118 0.2349 -0.1854 0.082 Uiso 1 1 calc R . . H1C H 0.4431 0.2755 -0.2111 0.082 Uiso 1 1 calc R . . C2 C 0.48593(7) 0.36228(16) -0.13765(7) 0.0343(4) Uani 1 1 d . . . H2 H 0.5182 0.3369 -0.1036 0.041 Uiso 1 1 calc R . . C3 C 0.50754(10) 0.4783(2) -0.16009(10) 0.0582(6) Uani 1 1 d . . . H3A H 0.4761 0.5069 -0.1928 0.087 Uiso 1 1 calc R . . H3B H 0.5435 0.4574 -0.1691 0.087 Uiso 1 1 calc R . . H3C H 0.5169 0.5448 -0.1327 0.087 Uiso 1 1 calc R . . C4 C 0.43022(7) 0.39229(15) -0.12301(7) 0.0305(3) Uani 1 1 d . . . C5 C 0.37795(8) 0.42234(18) -0.16438(7) 0.0391(4) Uani 1 1 d . . . H5 H 0.3775 0.4198 -0.2009 0.047 Uiso 1 1 calc R . . C6 C 0.32667(8) 0.4559(2) -0.15388(8) 0.0443(5) Uani 1 1 d . . . H6 H 0.2912 0.4755 -0.1828 0.053 Uiso 1 1 calc R . . C7 C 0.32743(8) 0.46061(18) -0.10114(8) 0.0408(4) Uani 1 1 d . . . H7 H 0.2923 0.4857 -0.0940 0.049 Uiso 1 1 calc R . . C8 C 0.37826(7) 0.42974(16) -0.05776(7) 0.0327(4) Uani 1 1 d . . . C9 C 0.37450(8) 0.4362(2) -0.00064(8) 0.0452(5) Uani 1 1 d . . . H9 H 0.4141 0.4105 0.0255 0.054 Uiso 1 1 calc R . . C10 C 0.32676(12) 0.3466(2) 0.00612(11) 0.0689(7) Uani 1 1 d . . . H10A H 0.2871 0.3745 -0.0169 0.103 Uiso 1 1 calc R . . H10B H 0.3285 0.3461 0.0441 0.103 Uiso 1 1 calc R . . H10C H 0.3342 0.2620 -0.0046 0.103 Uiso 1 1 calc R . . C11 C 0.36128(10) 0.5686(2) 0.01355(9) 0.0575(6) Uani 1 1 d . . . H11A H 0.3920 0.6256 0.0096 0.086 Uiso 1 1 calc R . . H11B H 0.3613 0.5708 0.0511 0.086 Uiso 1 1 calc R . . H11C H 0.3220 0.5947 -0.0109 0.086 Uiso 1 1 calc R . . C12 C 0.43028(7) 0.39404(14) -0.06907(6) 0.0277(3) Uani 1 1 d . . . C13 C 0.49946(7) 0.22569(15) -0.02165(7) 0.0323(4) Uani 1 1 d . . . H13A H 0.5433 0.2163 -0.0047 0.039 Uiso 1 1 calc R . . H13B H 0.4881 0.1880 -0.0583 0.039 Uiso 1 1 calc R . . C14 C 0.46893(7) 0.15358(14) 0.01172(6) 0.0286(3) Uani 1 1 d . . . C15 C 0.49276(7) 0.15980(15) 0.06847(6) 0.0294(3) Uani 1 1 d . . . C16 C 0.46478(7) 0.09508(15) 0.10029(6) 0.0300(3) Uani 1 1 d . . . C17 C 0.41371(7) 0.02289(14) 0.07479(6) 0.0288(3) Uani 1 1 d . . . C18 C 0.38871(7) 0.02006(14) 0.01807(7) 0.0295(3) Uani 1 1 d . . . C19 C 0.41655(7) 0.08455(15) -0.01364(6) 0.0290(3) Uani 1 1 d . . . C20 C 0.54937(8) 0.23463(17) 0.09618(8) 0.0407(4) Uani 1 1 d . . . H20A H 0.5802 0.1789 0.1193 0.061 Uiso 1 1 calc R . . H20B H 0.5405 0.3006 0.1185 0.061 Uiso 1 1 calc R . . H20C H 0.5638 0.2725 0.0686 0.061 Uiso 1 1 calc R . . C21 C 0.48971(9) 0.10680(19) 0.16141(7) 0.0439(4) Uani 1 1 d . . . H21A H 0.5279 0.0622 0.1750 0.066 Uiso 1 1 calc R . . H21B H 0.4614 0.0705 0.1774 0.066 Uiso 1 1 calc R . . H21C H 0.4960 0.1953 0.1714 0.066 Uiso 1 1 calc R . . C22 C 0.33060(8) -0.04930(18) -0.00873(8) 0.0432(4) Uani 1 1 d . . . H22A H 0.3031 0.0045 -0.0362 0.065 Uiso 1 1 calc R . . H22B H 0.3124 -0.0719 0.0187 0.065 Uiso 1 1 calc R . . H22C H 0.3387 -0.1254 -0.0261 0.065 Uiso 1 1 calc R . . C23 C 0.38954(8) 0.07961(18) -0.07470(7) 0.0398(4) Uani 1 1 d . . . H23A H 0.3633 0.0064 -0.0852 0.060 Uiso 1 1 calc R . . H23B H 0.4215 0.0734 -0.0907 0.060 Uiso 1 1 calc R . . H23C H 0.3662 0.1558 -0.0878 0.060 Uiso 1 1 calc R . . C24 C 0.38491(8) -0.05422(16) 0.10800(7) 0.0348(4) Uani 1 1 d . . . H24A H 0.3705 -0.1341 0.0891 0.042 Uiso 1 1 calc R . . H24B H 0.4151 -0.0739 0.1436 0.042 Uiso 1 1 calc R . . C25 C 0.32999(7) 0.00423(15) 0.16963(6) 0.0271(3) Uani 1 1 d . . . C26 C 0.31562(7) -0.11286(15) 0.18717(6) 0.0302(3) Uani 1 1 d . . . C27 C 0.29794(8) -0.22499(16) 0.14925(7) 0.0375(4) Uani 1 1 d . . . H27 H 0.2928 -0.1954 0.1116 0.045 Uiso 1 1 calc R . . C28 C 0.34677(10) -0.32508(18) 0.16404(9) 0.0525(5) Uani 1 1 d . . . H28A H 0.3846 -0.2882 0.1639 0.079 Uiso 1 1 calc R . . H28B H 0.3354 -0.3932 0.1375 0.079 Uiso 1 1 calc R . . H28C H 0.3516 -0.3580 0.2003 0.079 Uiso 1 1 calc R . . C29 C 0.23866(9) -0.2829(2) 0.14890(9) 0.0564(6) Uani 1 1 d . . . H29A H 0.2430 -0.3154 0.1851 0.085 Uiso 1 1 calc R . . H29B H 0.2278 -0.3513 0.1225 0.085 Uiso 1 1 calc R . . H29C H 0.2073 -0.2190 0.1389 0.085 Uiso 1 1 calc R . . C30 C 0.31484(8) -0.12276(17) 0.23997(7) 0.0370(4) Uani 1 1 d . . . H30 H 0.3072 -0.2017 0.2531 0.044 Uiso 1 1 calc R . . C31 C 0.32499(8) -0.01995(18) 0.27380(7) 0.0406(4) Uani 1 1 d . . . H31 H 0.3247 -0.0286 0.3099 0.049 Uiso 1 1 calc R . . C32 C 0.33557(8) 0.09558(17) 0.25499(7) 0.0371(4) Uani 1 1 d . . . H32 H 0.3408 0.1664 0.2781 0.045 Uiso 1 1 calc R . . C33 C 0.33875(7) 0.11047(15) 0.20333(7) 0.0303(3) Uani 1 1 d . . . C34 C 0.34822(8) 0.24015(16) 0.18295(7) 0.0389(4) Uani 1 1 d . . . H34 H 0.3705 0.2282 0.1567 0.047 Uiso 1 1 calc R . . C35 C 0.38562(12) 0.3271(2) 0.22732(10) 0.0685(7) Uani 1 1 d . . . H35A H 0.3633 0.3483 0.2518 0.103 Uiso 1 1 calc R . . H35B H 0.3946 0.4037 0.2109 0.103 Uiso 1 1 calc R . . H35C H 0.4231 0.2854 0.2479 0.103 Uiso 1 1 calc R . . C36 C 0.28819(10) 0.3002(2) 0.15161(10) 0.0572(6) Uani 1 1 d . . . H36A H 0.2651 0.2431 0.1230 0.086 Uiso 1 1 calc R . . H36B H 0.2951 0.3787 0.1353 0.086 Uiso 1 1 calc R . . H36C H 0.2659 0.3173 0.1765 0.086 Uiso 1 1 calc R . . N1 N 0.48473(6) 0.36150(13) -0.02736(6) 0.0296(3) Uani 1 1 d . . . N2 N 0.33404(6) 0.01320(14) 0.11671(5) 0.0300(3) Uani 1 1 d . . . H100 H 0.3351(8) 0.0962(18) 0.1079(7) 0.033(5) Uiso 1 1 d . . . H101 H 0.4839(8) 0.3906(18) 0.0046(8) 0.040(5) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0460(11) 0.0646(14) 0.0574(13) -0.0092(10) 0.0232(10) 0.0128(10) C2 0.0323(9) 0.0387(9) 0.0356(9) 0.0070(7) 0.0161(7) 0.0079(7) C3 0.0543(13) 0.0546(13) 0.0830(16) 0.0261(11) 0.0460(12) 0.0165(10) C4 0.0272(8) 0.0304(8) 0.0361(9) 0.0036(7) 0.0132(7) 0.0046(6) C5 0.0354(9) 0.0492(11) 0.0325(9) 0.0047(8) 0.0110(8) 0.0084(8) C6 0.0276(9) 0.0611(13) 0.0395(10) 0.0049(9) 0.0049(8) 0.0119(8) C7 0.0261(9) 0.0505(11) 0.0476(11) 0.0027(8) 0.0146(8) 0.0099(7) C8 0.0290(8) 0.0343(9) 0.0386(9) 0.0024(7) 0.0161(7) 0.0035(7) C9 0.0371(10) 0.0647(13) 0.0387(10) 0.0077(9) 0.0193(8) 0.0141(9) C10 0.1005(19) 0.0492(13) 0.0870(17) 0.0143(12) 0.0715(16) 0.0156(12) C11 0.0556(13) 0.0667(14) 0.0596(13) -0.0209(11) 0.0318(11) -0.0131(11) C12 0.0252(8) 0.0252(8) 0.0344(8) 0.0027(6) 0.0120(7) 0.0016(6) C13 0.0285(8) 0.0330(9) 0.0389(9) 0.0068(7) 0.0157(7) 0.0068(6) C14 0.0279(8) 0.0266(8) 0.0334(8) 0.0047(6) 0.0128(7) 0.0063(6) C15 0.0271(8) 0.0265(8) 0.0342(8) 0.0034(6) 0.0094(7) 0.0048(6) C16 0.0327(8) 0.0286(8) 0.0293(8) 0.0041(6) 0.0109(7) 0.0077(6) C17 0.0314(8) 0.0250(8) 0.0341(8) 0.0018(6) 0.0162(7) 0.0050(6) C18 0.0303(8) 0.0261(8) 0.0344(8) -0.0025(6) 0.0136(7) 0.0009(6) C19 0.0306(8) 0.0279(8) 0.0290(8) 0.0001(6) 0.0103(7) 0.0059(6) C20 0.0329(9) 0.0404(10) 0.0433(10) 0.0033(8) 0.0052(8) -0.0022(7) C21 0.0492(11) 0.0485(11) 0.0313(9) 0.0036(8) 0.0094(8) 0.0015(9) C22 0.0430(10) 0.0449(11) 0.0439(10) -0.0090(8) 0.0174(9) -0.0115(8) C23 0.0449(10) 0.0422(10) 0.0315(9) -0.0025(7) 0.0114(8) -0.0022(8) C24 0.0409(9) 0.0286(9) 0.0424(9) 0.0041(7) 0.0239(8) 0.0045(7) C25 0.0245(7) 0.0299(8) 0.0276(8) 0.0018(6) 0.0094(6) 0.0029(6) C26 0.0305(8) 0.0299(8) 0.0314(8) 0.0006(6) 0.0115(7) 0.0021(6) C27 0.0470(10) 0.0330(9) 0.0373(9) -0.0005(7) 0.0201(8) -0.0056(7) C28 0.0650(13) 0.0343(10) 0.0632(13) -0.0013(9) 0.0277(11) 0.0047(9) C29 0.0581(13) 0.0541(13) 0.0631(14) -0.0131(10) 0.0283(11) -0.0220(10) C30 0.0434(10) 0.0364(9) 0.0334(9) 0.0077(7) 0.0156(8) 0.0044(8) C31 0.0446(10) 0.0510(11) 0.0251(8) 0.0016(7) 0.0098(8) 0.0046(8) C32 0.0385(9) 0.0408(10) 0.0312(9) -0.0084(7) 0.0101(7) -0.0010(7) C33 0.0265(8) 0.0313(9) 0.0326(8) -0.0022(6) 0.0088(7) 0.0008(6) C34 0.0448(10) 0.0304(9) 0.0442(10) -0.0029(7) 0.0185(8) -0.0024(7) C35 0.0906(18) 0.0402(12) 0.0625(15) -0.0060(10) 0.0087(13) -0.0218(12) C36 0.0598(13) 0.0396(11) 0.0699(14) 0.0134(10) 0.0183(11) 0.0082(9) N1 0.0279(7) 0.0302(7) 0.0310(7) 0.0025(6) 0.0101(6) 0.0048(5) N2 0.0348(7) 0.0286(7) 0.0299(7) 0.0039(6) 0.0153(6) 0.0045(6) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.526(3) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C4 1.524(2) . ? C2 C3 1.530(3) . ? C2 H2 1.0000 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 C5 1.386(2) . ? C4 C12 1.408(2) . ? C5 C6 1.378(2) . ? C5 H5 0.9500 . ? C6 C7 1.372(3) . ? C6 H6 0.9500 . ? C7 C8 1.394(2) . ? C7 H7 0.9500 . ? C8 C12 1.411(2) . ? C8 C9 1.524(2) . ? C9 C11 1.522(3) . ? C9 C10 1.535(3) . ? C9 H9 1.0000 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 N1 1.430(2) . ? C13 N1 1.489(2) . ? C13 C14 1.513(2) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.403(2) . ? C14 C19 1.407(2) . ? C15 C16 1.404(2) . ? C15 C20 1.524(2) . ? C16 C17 1.404(2) . ? C16 C21 1.513(2) . ? C17 C18 1.402(2) . ? C17 C24 1.512(2) . ? C18 C19 1.398(2) . ? C18 C22 1.516(2) . ? C19 C23 1.510(2) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 N2 1.484(2) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C33 1.410(2) . ? C25 C26 1.413(2) . ? C25 N2 1.4194(19) . ? C26 C30 1.388(2) . ? C26 C27 1.523(2) . ? C27 C28 1.529(3) . ? C27 C29 1.531(3) . ? C27 H27 1.0000 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 C31 1.381(3) . ? C30 H30 0.9500 . ? C31 C32 1.382(3) . ? C31 H31 0.9500 . ? C32 C33 1.385(2) . ? C32 H32 0.9500 . ? C33 C34 1.528(2) . ? C34 C35 1.522(3) . ? C34 C36 1.529(3) . ? C34 H34 1.0000 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? N1 H101 0.90(2) . ? N2 H100 0.918(19) . ? 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 C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C4 C2 C1 111.37(15) . . ? C4 C2 C3 110.60(14) . . ? C1 C2 C3 111.24(17) . . ? C4 C2 H2 107.8 . . ? C1 C2 H2 107.8 . . ? C3 C2 H2 107.8 . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C5 C4 C12 118.88(14) . . ? C5 C4 C2 118.55(15) . . ? C12 C4 C2 122.55(14) . . ? C6 C5 C4 121.64(16) . . ? C6 C5 H5 119.2 . . ? C4 C5 H5 119.2 . . ? C7 C6 C5 119.22(16) . . ? C7 C6 H6 120.4 . . ? C5 C6 H6 120.4 . . ? C6 C7 C8 121.96(16) . . ? C6 C7 H7 119.0 . . ? C8 C7 H7 119.0 . . ? C7 C8 C12 118.28(15) . . ? C7 C8 C9 118.12(15) . . ? C12 C8 C9 123.60(15) . . ? C11 C9 C8 111.28(17) . . ? C11 C9 C10 109.51(16) . . ? C8 C9 C10 111.52(17) . . ? C11 C9 H9 108.1 . . ? C8 C9 H9 108.1 . . ? C10 C9 H9 108.1 . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? 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 . . ? C4 C12 C8 119.98(14) . . ? C4 C12 N1 117.54(13) . . ? C8 C12 N1 122.47(14) . . ? N1 C13 C14 114.44(13) . . ? N1 C13 H13A 108.7 . . ? C14 C13 H13A 108.7 . . ? N1 C13 H13B 108.7 . . ? C14 C13 H13B 108.7 . . ? H13A C13 H13B 107.6 . . ? C15 C14 C19 120.48(14) . . ? C15 C14 C13 118.79(14) . . ? C19 C14 C13 120.71(14) . . ? C14 C15 C16 119.85(15) . . ? C14 C15 C20 120.75(15) . . ? C16 C15 C20 119.40(15) . . ? C15 C16 C17 119.42(14) . . ? C15 C16 C21 119.14(15) . . ? C17 C16 C21 121.43(15) . . ? C18 C17 C16 120.70(14) . . ? C18 C17 C24 118.71(15) . . ? C16 C17 C24 120.58(15) . . ? C19 C18 C17 119.82(14) . . ? C19 C18 C22 120.08(15) . . ? C17 C18 C22 120.08(15) . . ? C18 C19 C14 119.64(14) . . ? C18 C19 C23 119.30(15) . . ? C14 C19 C23 121.06(15) . . ? C15 C20 H20A 109.5 . . ? C15 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C15 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C16 C21 H21A 109.5 . . ? C16 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C16 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C18 C22 H22A 109.5 . . ? C18 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C18 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C19 C23 H23A 109.5 . . ? C19 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C19 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? N2 C24 C17 111.41(13) . . ? N2 C24 H24A 109.3 . . ? C17 C24 H24A 109.3 . . ? N2 C24 H24B 109.3 . . ? C17 C24 H24B 109.3 . . ? H24A C24 H24B 108.0 . . ? C33 C25 C26 120.90(14) . . ? C33 C25 N2 120.65(14) . . ? C26 C25 N2 118.43(14) . . ? C30 C26 C25 118.21(15) . . ? C30 C26 C27 119.65(15) . . ? C25 C26 C27 122.06(14) . . ? C26 C27 C28 111.33(15) . . ? C26 C27 C29 112.15(15) . . ? C28 C27 C29 109.52(16) . . ? C26 C27 H27 107.9 . . ? C28 C27 H27 107.9 . . ? C29 C27 H27 107.9 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C31 C30 C26 121.19(16) . . ? C31 C30 H30 119.4 . . ? C26 C30 H30 119.4 . . ? C30 C31 C32 119.86(16) . . ? C30 C31 H31 120.1 . . ? C32 C31 H31 120.1 . . ? C31 C32 C33 121.55(16) . . ? C31 C32 H32 119.2 . . ? C33 C32 H32 119.2 . . ? C32 C33 C25 118.11(15) . . ? C32 C33 C34 120.32(15) . . ? C25 C33 C34 121.49(14) . . ? C35 C34 C33 113.89(16) . . ? C35 C34 C36 110.86(18) . . ? C33 C34 C36 110.50(15) . . ? C35 C34 H34 107.1 . . ? C33 C34 H34 107.1 . . ? C36 C34 H34 107.1 . . ? C34 C35 H35A 109.5 . . ? C34 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C34 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C34 C36 H36A 109.5 . . ? C34 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C34 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C12 N1 C13 115.86(13) . . ? C12 N1 H101 109.5(12) . . ? C13 N1 H101 108.7(12) . . ? C25 N2 C24 115.77(13) . . ? C25 N2 H100 108.9(11) . . ? C24 N2 H100 109.9(11) . . ? 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 C1 C2 C4 C5 -57.8(2) . . . . ? C3 C2 C4 C5 66.4(2) . . . . ? C1 C2 C4 C12 124.00(18) . . . . ? C3 C2 C4 C12 -111.77(19) . . . . ? C12 C4 C5 C6 1.2(3) . . . . ? C2 C4 C5 C6 -177.07(18) . . . . ? C4 C5 C6 C7 0.5(3) . . . . ? C5 C6 C7 C8 -1.5(3) . . . . ? C6 C7 C8 C12 0.7(3) . . . . ? C6 C7 C8 C9 -179.18(18) . . . . ? C7 C8 C9 C11 -62.0(2) . . . . ? C12 C8 C9 C11 118.10(19) . . . . ? C7 C8 C9 C10 60.6(2) . . . . ? C12 C8 C9 C10 -119.29(19) . . . . ? C5 C4 C12 C8 -2.0(2) . . . . ? C2 C4 C12 C8 176.22(15) . . . . ? C5 C4 C12 N1 179.45(15) . . . . ? C2 C4 C12 N1 -2.4(2) . . . . ? C7 C8 C12 C4 1.0(2) . . . . ? C9 C8 C12 C4 -179.09(16) . . . . ? C7 C8 C12 N1 179.57(15) . . . . ? C9 C8 C12 N1 -0.6(3) . . . . ? N1 C13 C14 C15 -79.88(18) . . . . ? N1 C13 C14 C19 98.22(18) . . . . ? C19 C14 C15 C16 1.1(2) . . . . ? C13 C14 C15 C16 179.16(14) . . . . ? C19 C14 C15 C20 -179.85(15) . . . . ? C13 C14 C15 C20 -1.7(2) . . . . ? C14 C15 C16 C17 1.1(2) . . . . ? C20 C15 C16 C17 -177.98(14) . . . . ? C14 C15 C16 C21 -177.68(15) . . . . ? C20 C15 C16 C21 3.2(2) . . . . ? C15 C16 C17 C18 -3.3(2) . . . . ? C21 C16 C17 C18 175.47(15) . . . . ? C15 C16 C17 C24 176.16(14) . . . . ? C21 C16 C17 C24 -5.1(2) . . . . ? C16 C17 C18 C19 3.3(2) . . . . ? C24 C17 C18 C19 -176.18(14) . . . . ? C16 C17 C18 C22 -174.75(15) . . . . ? C24 C17 C18 C22 5.8(2) . . . . ? C17 C18 C19 C14 -1.1(2) . . . . ? C22 C18 C19 C14 176.97(15) . . . . ? C17 C18 C19 C23 179.34(14) . . . . ? C22 C18 C19 C23 -2.6(2) . . . . ? C15 C14 C19 C18 -1.1(2) . . . . ? C13 C14 C19 C18 -179.14(14) . . . . ? C15 C14 C19 C23 178.49(15) . . . . ? C13 C14 C19 C23 0.4(2) . . . . ? C18 C17 C24 N2 -84.04(18) . . . . ? C16 C17 C24 N2 96.48(18) . . . . ? C33 C25 C26 C30 -4.9(2) . . . . ? N2 C25 C26 C30 176.62(14) . . . . ? C33 C25 C26 C27 171.84(15) . . . . ? N2 C25 C26 C27 -6.7(2) . . . . ? C30 C26 C27 C28 -73.6(2) . . . . ? C25 C26 C27 C28 109.72(18) . . . . ? C30 C26 C27 C29 49.5(2) . . . . ? C25 C26 C27 C29 -127.18(18) . . . . ? C25 C26 C30 C31 3.1(2) . . . . ? C27 C26 C30 C31 -173.71(16) . . . . ? C26 C30 C31 C32 0.6(3) . . . . ? C30 C31 C32 C33 -2.7(3) . . . . ? C31 C32 C33 C25 0.9(2) . . . . ? C31 C32 C33 C34 177.76(16) . . . . ? C26 C25 C33 C32 2.9(2) . . . . ? N2 C25 C33 C32 -178.60(14) . . . . ? C26 C25 C33 C34 -173.90(15) . . . . ? N2 C25 C33 C34 4.6(2) . . . . ? C32 C33 C34 C35 31.8(2) . . . . ? C25 C33 C34 C35 -151.50(19) . . . . ? C32 C33 C34 C36 -93.8(2) . . . . ? C25 C33 C34 C36 82.9(2) . . . . ? C4 C12 N1 C13 -76.11(18) . . . . ? C8 C12 N1 C13 105.33(18) . . . . ? C14 C13 N1 C12 -82.99(18) . . . . ? C33 C25 N2 C24 113.22(17) . . . . ? C26 C25 N2 C24 -68.25(19) . . . . ? C17 C24 N2 C25 -138.11(15) . . . . ? _diffrn_measured_fraction_theta_max 0.914 _diffrn_reflns_theta_full 30.13 _diffrn_measured_fraction_theta_full 0.99 _refine_diff_density_max 0.308 _refine_diff_density_min -0.240 _refine_diff_density_rms 0.043 data_j1011b _database_code_depnum_ccdc_archive 'CCDC 824568' #TrackingRef '- combined.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H38 N2, Cl4 Co, C H Cl3, H2 O' _chemical_formula_sum 'C21 H41 Cl7 Co N2 O' _chemical_formula_weight 644.64 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' Co Co 0.3494 0.9721 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.0602(13) _cell_length_b 12.1270(9) _cell_length_c 18.9923(17) _cell_angle_alpha 90.00 _cell_angle_beta 107.588(9) _cell_angle_gamma 90.00 _cell_volume 3087.0(5) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 5407 _cell_measurement_theta_min 2.8452 _cell_measurement_theta_max 26.6744 _exptl_crystal_description needle _exptl_crystal_colour blue _exptl_crystal_size_max 0.0317724 _exptl_crystal_size_mid 0.0161955 _exptl_crystal_size_min 0.0074209 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.387 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1340 _exptl_absorpt_coefficient_mu 1.178 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.81370 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Eos' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.1042 _diffrn_standards_number 24382 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23685 _diffrn_reflns_av_R_equivalents 0.0395 _diffrn_reflns_av_sigmaI/netI 0.1044 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.85 _diffrn_reflns_theta_max 26.73 _reflns_number_total 6533 _reflns_number_gt 4804 _reflns_threshold_expression >2\s(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40) ; _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Checkcif output: 412_ALERT_2_B Short Intra XH3 .. XHn H12A .. H13C .. 1.70 Ang. 412_ALERT_2_C Short Intra XH3 .. XHn H5A .. H15A .. 1.86 Ang. 412_ALERT_2_C Short Intra XH3 .. XHn H14A .. H16A .. 1.83 Ang. These are intramolecular contacts involving methyl groups. There is not a completely unambiguous method to assign the orientations of these groups, and they were allowed to optimise using the Sheldrick rotating rigid body model (AFIX 137). 353_ALERT_3_C Long N-H Bond (0.87A) N1 - H2N ... 1.06 Ang. The H-atom in question was located in a difference map and refined. It was treated in this manner because its distance to N is potentially influenced by H-bonding. 125_ALERT_4_C No '_symmetry_space_group_name_Hall' Given ..... ? 244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors of C100 794_ALERT_5_G Note: Tentative Bond Valency for Co1 ....... 2.05 No action taken. 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^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0439P)^2^+4.1538P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6533 _refine_ls_number_parameters 317 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0777 _refine_ls_R_factor_gt 0.0500 _refine_ls_wR_factor_ref 0.1169 _refine_ls_wR_factor_gt 0.1052 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.022 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C -0.1965(3) 0.2863(4) 0.7784(2) 0.0627(13) Uani 1 1 d . . . H1A H -0.1560 0.3527 0.7806 0.094 Uiso 1 1 calc R . . H1B H -0.1537 0.2255 0.8036 0.094 Uiso 1 1 calc R . . H1C H -0.2476 0.3006 0.8027 0.094 Uiso 1 1 calc R . . C2 C -0.3091(3) 0.3491(3) 0.6547(3) 0.0579(12) Uani 1 1 d . . . H2A H -0.2673 0.4149 0.6589 0.087 Uiso 1 1 calc R . . H2B H -0.3642 0.3650 0.6747 0.087 Uiso 1 1 calc R . . H2C H -0.3359 0.3279 0.6027 0.087 Uiso 1 1 calc R . . C3 C -0.3095(3) 0.1529(3) 0.6930(2) 0.0445(9) Uani 1 1 d . . . H3A H -0.3412 0.1342 0.6409 0.067 Uiso 1 1 calc R . . H3B H -0.3611 0.1666 0.7169 0.067 Uiso 1 1 calc R . . H3C H -0.2672 0.0916 0.7177 0.067 Uiso 1 1 calc R . . C4 C -0.2467(2) 0.2551(3) 0.69803(19) 0.0342(8) Uani 1 1 d . . . C5 C -0.1844(2) 0.1720(3) 0.59344(17) 0.0300(7) Uani 1 1 d . . . H5A H -0.2022 0.0947 0.6006 0.036 Uiso 1 1 calc R . . H5B H -0.2417 0.2066 0.5563 0.036 Uiso 1 1 calc R . . C6 C -0.0935(2) 0.1745(3) 0.56645(17) 0.0258(7) Uani 1 1 d . . . C7 C -0.0826(2) 0.2605(3) 0.51961(16) 0.0266(7) Uani 1 1 d . . . C8 C 0.0056(2) 0.2689(3) 0.50107(16) 0.0256(7) Uani 1 1 d . . . C9 C 0.0812(2) 0.1897(3) 0.52741(16) 0.0253(7) Uani 1 1 d . . . C10 C 0.0680(2) 0.0998(3) 0.56988(16) 0.0257(7) Uani 1 1 d . . . C11 C -0.0199(2) 0.0933(3) 0.59063(16) 0.0259(7) Uani 1 1 d . . . C12 C 0.0211(3) 0.3642(3) 0.45435(18) 0.0371(8) Uani 1 1 d . . . H12A H -0.0416 0.4048 0.4348 0.056 Uiso 1 1 calc R . . H12B H 0.0426 0.3359 0.4133 0.056 Uiso 1 1 calc R . . H12C H 0.0724 0.4136 0.4847 0.056 Uiso 1 1 calc R . . C13 C -0.1657(3) 0.3431(3) 0.4890(2) 0.0380(8) Uani 1 1 d . . . H13A H -0.1660 0.3972 0.5273 0.057 Uiso 1 1 calc R . . H13B H -0.2299 0.3045 0.4735 0.057 Uiso 1 1 calc R . . H13C H -0.1549 0.3811 0.4465 0.057 Uiso 1 1 calc R . . C14 C 0.1451(2) 0.0101(3) 0.5950(2) 0.0364(8) Uani 1 1 d . . . H14A H 0.1941 0.0159 0.5679 0.055 Uiso 1 1 calc R . . H14B H 0.1123 -0.0621 0.5855 0.055 Uiso 1 1 calc R . . H14C H 0.1789 0.0180 0.6481 0.055 Uiso 1 1 calc R . . C15 C -0.0317(3) -0.0013(3) 0.63909(19) 0.0349(8) Uani 1 1 d . . . H15A H -0.0947 0.0068 0.6507 0.052 Uiso 1 1 calc R . . H15B H 0.0240 -0.0009 0.6850 0.052 Uiso 1 1 calc R . . H15C H -0.0320 -0.0712 0.6131 0.052 Uiso 1 1 calc R . . C16 C 0.1796(2) 0.2062(3) 0.51203(18) 0.0298(7) Uani 1 1 d . . . H16A H 0.2139 0.1345 0.5141 0.036 Uiso 1 1 calc R . . H16B H 0.1679 0.2376 0.4620 0.036 Uiso 1 1 calc R . . C17 C 0.3392(2) 0.3291(3) 0.5570(2) 0.0360(8) Uani 1 1 d . . . C18 C 0.3802(3) 0.4119(4) 0.6187(2) 0.0575(12) Uani 1 1 d . . . H18A H 0.3329 0.4729 0.6135 0.086 Uiso 1 1 calc R . . H18B H 0.4442 0.4404 0.6160 0.086 Uiso 1 1 calc R . . H18C H 0.3899 0.3757 0.6665 0.086 Uiso 1 1 calc R . . C19 C 0.3131(3) 0.3846(3) 0.4816(2) 0.0447(9) Uani 1 1 d . . . H19A H 0.2674 0.4462 0.4801 0.067 Uiso 1 1 calc R . . H19B H 0.2810 0.3310 0.4431 0.067 Uiso 1 1 calc R . . H19C H 0.3742 0.4123 0.4731 0.067 Uiso 1 1 calc R . . C20 C 0.4097(3) 0.2334(3) 0.5625(2) 0.0450(9) Uani 1 1 d . . . H20A H 0.4248 0.1999 0.6116 0.068 Uiso 1 1 calc R . . H20B H 0.4716 0.2598 0.5547 0.068 Uiso 1 1 calc R . . H20C H 0.3785 0.1783 0.5248 0.068 Uiso 1 1 calc R . . C100 C 0.5292(3) 0.1407(4) 0.3733(2) 0.0600(12) Uani 1 1 d . . . H100 H 0.4549 0.1436 0.3611 0.072 Uiso 1 1 calc R . . Cl1 Cl 0.31073(7) 0.18772(8) 0.73464(5) 0.0449(2) Uani 1 1 d . . . Cl2 Cl 0.07074(6) 0.20379(7) 0.78138(5) 0.0383(2) Uani 1 1 d . . . Cl3 Cl 0.28386(6) 0.38713(7) 0.87344(4) 0.03062(19) Uani 1 1 d . . . Cl4 Cl 0.14619(6) 0.43010(7) 0.67340(4) 0.0344(2) Uani 1 1 d . . . Cl5 Cl 0.57879(10) 0.08740(12) 0.46281(6) 0.0739(4) Uani 1 1 d . . . Cl6 Cl 0.56021(10) 0.05089(14) 0.31061(7) 0.0825(4) Uani 1 1 d . . . Cl7 Cl 0.57301(11) 0.27293(14) 0.36640(12) 0.1130(6) Uani 1 1 d . . . N1 N -0.1613(2) 0.2343(3) 0.66591(16) 0.0303(6) Uani 1 1 d . . . N2 N 0.2436(2) 0.2836(3) 0.56909(16) 0.0303(6) Uani 1 1 d . . . O1 O -0.0836(2) 0.4467(3) 0.65886(16) 0.0446(7) Uani 1 1 d . . . Co1 Co 0.20153(3) 0.30104(4) 0.76602(2) 0.02676(12) Uani 1 1 d . . . H1N H -0.116(3) 0.196(3) 0.695(2) 0.042(11) Uiso 1 1 d . . . H4N H 0.208(3) 0.340(3) 0.5767(19) 0.035(10) Uiso 1 1 d . . . H3N H 0.258(3) 0.245(3) 0.614(2) 0.048(11) Uiso 1 1 d . . . H2N H -0.133(4) 0.314(4) 0.661(3) 0.080(15) Uiso 1 1 d . . . H1O H -0.090(3) 0.509(4) 0.676(3) 0.069(16) Uiso 1 1 d . . . H2O H -0.019(4) 0.445(4) 0.663(3) 0.093(19) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.042(2) 0.104(4) 0.048(2) -0.034(3) 0.0222(19) -0.016(2) C2 0.044(2) 0.052(3) 0.088(3) 0.008(2) 0.036(2) 0.011(2) C3 0.046(2) 0.046(2) 0.052(2) -0.0090(19) 0.0304(19) -0.0065(18) C4 0.0320(18) 0.0364(19) 0.0392(19) -0.0069(16) 0.0184(15) 0.0009(15) C5 0.0236(15) 0.0378(19) 0.0274(17) -0.0066(15) 0.0059(13) -0.0035(14) C6 0.0225(15) 0.0294(18) 0.0244(16) -0.0080(13) 0.0055(12) -0.0042(13) C7 0.0287(16) 0.0311(17) 0.0182(15) -0.0060(13) 0.0042(12) -0.0013(13) C8 0.0317(16) 0.0295(17) 0.0156(14) -0.0043(13) 0.0071(12) -0.0030(14) C9 0.0280(16) 0.0332(18) 0.0167(14) -0.0076(13) 0.0096(12) -0.0034(14) C10 0.0257(16) 0.0292(17) 0.0206(15) -0.0056(13) 0.0043(12) 0.0003(13) C11 0.0279(16) 0.0270(17) 0.0221(15) -0.0051(13) 0.0065(12) -0.0061(13) C12 0.0403(19) 0.044(2) 0.0285(18) 0.0086(16) 0.0127(15) 0.0004(16) C13 0.0355(19) 0.042(2) 0.0353(19) 0.0034(17) 0.0095(15) 0.0059(16) C14 0.0326(18) 0.038(2) 0.041(2) 0.0018(17) 0.0139(15) 0.0036(15) C15 0.0362(18) 0.0315(19) 0.0386(19) 0.0013(16) 0.0136(15) -0.0025(15) C16 0.0316(17) 0.0340(18) 0.0278(17) -0.0088(15) 0.0147(14) -0.0066(14) C17 0.0257(17) 0.045(2) 0.040(2) -0.0095(17) 0.0141(15) -0.0055(15) C18 0.043(2) 0.068(3) 0.065(3) -0.028(2) 0.021(2) -0.019(2) C19 0.040(2) 0.044(2) 0.056(2) 0.0036(19) 0.0232(18) -0.0035(17) C20 0.0300(18) 0.060(3) 0.045(2) -0.005(2) 0.0114(16) 0.0009(17) C100 0.0271(19) 0.086(3) 0.065(3) 0.000(3) 0.0112(19) -0.009(2) Cl1 0.0452(5) 0.0558(6) 0.0332(5) -0.0053(4) 0.0110(4) 0.0191(4) Cl2 0.0334(4) 0.0431(5) 0.0369(5) 0.0046(4) 0.0086(4) -0.0076(4) Cl3 0.0278(4) 0.0401(5) 0.0245(4) -0.0029(3) 0.0087(3) 0.0003(3) Cl4 0.0360(4) 0.0405(5) 0.0276(4) 0.0072(4) 0.0109(3) 0.0080(4) Cl5 0.0710(8) 0.1057(10) 0.0454(6) -0.0098(7) 0.0184(6) -0.0116(7) Cl6 0.0696(8) 0.1337(13) 0.0490(7) 0.0001(7) 0.0249(6) 0.0096(8) Cl7 0.0615(9) 0.0862(11) 0.1750(18) 0.0251(11) 0.0110(10) -0.0147(8) N1 0.0233(14) 0.0389(18) 0.0287(15) -0.0039(13) 0.0078(12) 0.0037(13) N2 0.0267(14) 0.0399(18) 0.0270(15) -0.0076(14) 0.0120(12) 0.0004(13) O1 0.0387(16) 0.0428(17) 0.0533(17) -0.0079(14) 0.0151(13) -0.0067(13) Co1 0.0259(2) 0.0327(3) 0.0219(2) 0.00056(19) 0.00759(17) 0.00179(19) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C4 1.522(5) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C4 1.519(5) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 C4 1.508(5) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 N1 1.522(4) . ? C5 C6 1.514(4) . ? C5 N1 1.517(4) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C11 1.401(4) . ? C6 C7 1.409(4) . ? C7 C8 1.392(4) . ? C7 C13 1.515(5) . ? C8 C9 1.408(4) . ? C8 C12 1.513(4) . ? C9 C10 1.401(4) . ? C9 C16 1.511(4) . ? C10 C11 1.409(4) . ? C10 C14 1.508(4) . ? C11 C15 1.510(4) . ? 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 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 N2 1.509(4) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C20 1.510(5) . ? C17 C18 1.518(5) . ? C17 C19 1.524(5) . ? C17 N2 1.533(4) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C100 Cl7 1.737(5) . ? C100 Cl5 1.754(5) . ? C100 Cl6 1.763(5) . ? C100 H100 1.0000 . ? Cl1 Co1 2.2703(9) . ? Cl2 Co1 2.2763(9) . ? Cl3 Co1 2.2726(9) . ? Cl4 Co1 2.3070(9) . ? N1 H1N 0.85(4) . ? N1 H2N 1.06(5) . ? N2 H4N 0.88(4) . ? N2 H3N 0.94(4) . ? O1 H1O 0.84(5) . ? O1 H2O 0.89(6) . ? 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 C4 C1 H1A 109.5 . . ? C4 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C4 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C4 C2 H2A 109.5 . . ? C4 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C4 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C4 C3 H3A 109.5 . . ? C4 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C4 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C3 C4 C2 110.5(3) . . ? C3 C4 N1 110.9(3) . . ? C2 C4 N1 107.7(3) . . ? C3 C4 C1 110.7(3) . . ? C2 C4 C1 111.9(3) . . ? N1 C4 C1 105.1(3) . . ? C6 C5 N1 109.1(2) . . ? C6 C5 H5A 109.9 . . ? N1 C5 H5A 109.9 . . ? C6 C5 H5B 109.9 . . ? N1 C5 H5B 109.9 . . ? H5A C5 H5B 108.3 . . ? C11 C6 C7 121.2(3) . . ? C11 C6 C5 119.3(3) . . ? C7 C6 C5 119.4(3) . . ? C8 C7 C6 119.2(3) . . ? C8 C7 C13 119.9(3) . . ? C6 C7 C13 120.9(3) . . ? C7 C8 C9 119.7(3) . . ? C7 C8 C12 120.1(3) . . ? C9 C8 C12 120.2(3) . . ? C10 C9 C8 121.2(3) . . ? C10 C9 C16 120.2(3) . . ? C8 C9 C16 118.6(3) . . ? C9 C10 C11 119.0(3) . . ? C9 C10 C14 122.5(3) . . ? C11 C10 C14 118.5(3) . . ? C6 C11 C10 119.4(3) . . ? C6 C11 C15 121.9(3) . . ? C10 C11 C15 118.7(3) . . ? C8 C12 H12A 109.5 . . ? C8 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C8 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C7 C13 H13A 109.5 . . ? C7 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C7 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C10 C14 H14A 109.5 . . ? C10 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C10 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C11 C15 H15A 109.5 . . ? C11 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C11 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N2 C16 C9 109.0(2) . . ? N2 C16 H16A 109.9 . . ? C9 C16 H16A 109.9 . . ? N2 C16 H16B 109.9 . . ? C9 C16 H16B 109.9 . . ? H16A C16 H16B 108.3 . . ? C20 C17 C18 111.5(3) . . ? C20 C17 C19 111.8(3) . . ? C18 C17 C19 111.2(3) . . ? C20 C17 N2 107.5(3) . . ? C18 C17 N2 105.5(3) . . ? C19 C17 N2 109.1(3) . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C17 C20 H20A 109.5 . . ? C17 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C17 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? Cl7 C100 Cl5 111.5(2) . . ? Cl7 C100 Cl6 110.7(2) . . ? Cl5 C100 Cl6 108.7(3) . . ? Cl7 C100 H100 108.6 . . ? Cl5 C100 H100 108.6 . . ? Cl6 C100 H100 108.6 . . ? C5 N1 C4 117.9(3) . . ? C5 N1 H1N 103(3) . . ? C4 N1 H1N 111(3) . . ? C5 N1 H2N 112(3) . . ? C4 N1 H2N 104(3) . . ? H1N N1 H2N 109(4) . . ? C16 N2 C17 118.4(2) . . ? C16 N2 H4N 111(2) . . ? C17 N2 H4N 108(2) . . ? C16 N2 H3N 105(2) . . ? C17 N2 H3N 111(2) . . ? H4N N2 H3N 102(3) . . ? H1O O1 H2O 103(4) . . ? Cl1 Co1 Cl3 108.20(3) . . ? Cl1 Co1 Cl2 110.89(4) . . ? Cl3 Co1 Cl2 109.58(3) . . ? Cl1 Co1 Cl4 108.03(4) . . ? Cl3 Co1 Cl4 109.62(4) . . ? Cl2 Co1 Cl4 110.47(4) . . ? 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 C5 C6 C11 87.1(3) . . . . ? N1 C5 C6 C7 -90.6(3) . . . . ? C11 C6 C7 C8 -4.3(4) . . . . ? C5 C6 C7 C8 173.5(3) . . . . ? C11 C6 C7 C13 175.4(3) . . . . ? C5 C6 C7 C13 -6.9(4) . . . . ? C6 C7 C8 C9 1.9(4) . . . . ? C13 C7 C8 C9 -177.7(3) . . . . ? C6 C7 C8 C12 -176.6(3) . . . . ? C13 C7 C8 C12 3.8(4) . . . . ? C7 C8 C9 C10 2.4(4) . . . . ? C12 C8 C9 C10 -179.1(3) . . . . ? C7 C8 C9 C16 -174.7(3) . . . . ? C12 C8 C9 C16 3.8(4) . . . . ? C8 C9 C10 C11 -4.4(4) . . . . ? C16 C9 C10 C11 172.7(3) . . . . ? C8 C9 C10 C14 176.2(3) . . . . ? C16 C9 C10 C14 -6.7(4) . . . . ? C7 C6 C11 C10 2.3(4) . . . . ? C5 C6 C11 C10 -175.5(3) . . . . ? C7 C6 C11 C15 -178.2(3) . . . . ? C5 C6 C11 C15 4.0(4) . . . . ? C9 C10 C11 C6 2.0(4) . . . . ? C14 C10 C11 C6 -178.6(3) . . . . ? C9 C10 C11 C15 -177.5(3) . . . . ? C14 C10 C11 C15 1.9(4) . . . . ? C10 C9 C16 N2 -94.2(3) . . . . ? C8 C9 C16 N2 82.9(3) . . . . ? C6 C5 N1 C4 172.2(3) . . . . ? C3 C4 N1 C5 44.0(4) . . . . ? C2 C4 N1 C5 -77.0(4) . . . . ? C1 C4 N1 C5 163.6(3) . . . . ? C9 C16 N2 C17 -169.3(3) . . . . ? C20 C17 N2 C16 -66.5(4) . . . . ? C18 C17 N2 C16 174.4(3) . . . . ? C19 C17 N2 C16 54.9(4) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 26.73 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.291 _refine_diff_density_min -0.717 _refine_diff_density_rms 0.072 data_monoc _database_code_depnum_ccdc_archive 'CCDC 824569' #TrackingRef '- combined.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H50 N2, Cl10 Zn4' _chemical_formula_sum 'C36 H50 Cl10 N2 Zn4' _chemical_formula_weight 1126.76 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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.5094(8) _cell_length_b 10.1009(8) _cell_length_c 13.8791(10) _cell_angle_alpha 88.205(6) _cell_angle_beta 85.706(6) _cell_angle_gamma 61.321(8) _cell_volume 1166.29(16) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 4989 _cell_measurement_theta_min 2.9377 _cell_measurement_theta_max 26.3134 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.0453997 _exptl_crystal_size_mid 0.02231426 _exptl_crystal_size_min 0.0078385 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.604 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 570 _exptl_absorpt_coefficient_mu 2.633 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.80738 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Eos' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.1042 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12460 _diffrn_reflns_av_R_equivalents 0.0277 _diffrn_reflns_av_sigmaI/netI 0.0843 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.94 _diffrn_reflns_theta_max 26.37 _reflns_number_total 4663 _reflns_number_gt 3703 _reflns_threshold_expression >2\s(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40) ; _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0391P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4663 _refine_ls_number_parameters 244 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0450 _refine_ls_R_factor_gt 0.0307 _refine_ls_wR_factor_ref 0.0792 _refine_ls_wR_factor_gt 0.0712 _refine_ls_goodness_of_fit_ref 0.956 _refine_ls_restrained_S_all 0.956 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.2042(3) 0.8815(3) 0.52409(18) 0.0348(7) Uani 1 1 d . . . H1 H 0.1627 0.8656 0.5852 0.042 Uiso 1 1 calc R . . C2 C 0.2773(3) 0.7650(3) 0.45821(18) 0.0345(7) Uani 1 1 d . . . H2 H 0.2811 0.6710 0.4735 0.041 Uiso 1 1 calc R . . C3 C 0.3459(3) 0.7816(3) 0.36940(17) 0.0285(6) Uani 1 1 d . . . C4 C 0.3327(3) 0.9231(3) 0.35095(16) 0.0236(5) Uani 1 1 d . . . C5 C 0.2541(3) 1.0462(3) 0.41393(16) 0.0256(6) Uani 1 1 d . . . C6 C 0.1905(3) 1.0207(3) 0.50227(18) 0.0337(7) Uani 1 1 d . . . H6 H 0.1371 1.1007 0.5479 0.040 Uiso 1 1 calc R . . C7 C 0.4231(4) 0.6522(3) 0.29798(19) 0.0374(7) Uani 1 1 d . . . H7 H 0.4725 0.6841 0.2421 0.045 Uiso 1 1 calc R . . C8 C 0.5579(4) 0.5111(3) 0.3416(2) 0.0523(9) Uani 1 1 d . . . H8A H 0.6088 0.4313 0.2924 0.078 Uiso 1 1 calc R . . H8B H 0.5128 0.4763 0.3962 0.078 Uiso 1 1 calc R . . H8C H 0.6381 0.5354 0.3641 0.078 Uiso 1 1 calc R . . C9 C 0.2977(4) 0.6193(4) 0.2594(2) 0.0568(9) Uani 1 1 d . . . H9A H 0.3481 0.5433 0.2079 0.085 Uiso 1 1 calc R . . H9B H 0.2122 0.7122 0.2336 0.085 Uiso 1 1 calc R . . H9C H 0.2521 0.5813 0.3118 0.085 Uiso 1 1 calc R . . C10 C 0.2404(3) 1.1996(3) 0.39091(18) 0.0329(6) Uani 1 1 d . . . H10 H 0.2541 1.2059 0.3191 0.039 Uiso 1 1 calc R . . C11 C 0.3765(5) 1.2124(4) 0.4328(2) 0.0662(11) Uani 1 1 d . . . H11A H 0.3672 1.3115 0.4171 0.099 Uiso 1 1 calc R . . H11B H 0.4797 1.1331 0.4051 0.099 Uiso 1 1 calc R . . H11C H 0.3705 1.2009 0.5031 0.099 Uiso 1 1 calc R . . C12 C 0.0761(4) 1.3280(3) 0.4230(2) 0.0601(10) Uani 1 1 d . . . H12A H 0.0692 1.4243 0.4020 0.090 Uiso 1 1 calc R . . H12B H 0.0604 1.3278 0.4936 0.090 Uiso 1 1 calc R . . H12C H -0.0073 1.3146 0.3942 0.090 Uiso 1 1 calc R . . C13 C 0.3456(3) 0.9874(3) 0.18154(16) 0.0254(6) Uani 1 1 d . . . H13 H 0.2337 1.0202 0.1823 0.030 Uiso 1 1 calc R . . C14 C 0.4284(3) 0.9954(3) 0.08891(17) 0.0225(5) Uani 1 1 d . . . C15 C 0.4052(3) 0.9267(3) 0.00963(17) 0.0234(5) Uani 1 1 d . . . C16 C 0.5213(3) 1.0700(3) 0.08121(16) 0.0230(5) Uani 1 1 d . . . C17 C 0.3083(3) 0.8448(3) 0.02133(18) 0.0319(6) Uani 1 1 d . . . H17A H 0.2392 0.8780 0.0812 0.048 Uiso 1 1 calc R . . H17B H 0.3810 0.7359 0.0241 0.048 Uiso 1 1 calc R . . H17C H 0.2417 0.8671 -0.0337 0.048 Uiso 1 1 calc R . . C18 C 0.5395(3) 1.1505(3) 0.16485(17) 0.0313(6) Uani 1 1 d . . . H18A H 0.4607 1.1608 0.2178 0.047 Uiso 1 1 calc R . . H18B H 0.5215 1.2509 0.1443 0.047 Uiso 1 1 calc R . . H18C H 0.6482 1.0924 0.1869 0.047 Uiso 1 1 calc R . . Cl1 Cl 1.11087(8) 0.40556(7) 0.15790(5) 0.03278(16) Uani 1 1 d . . . Cl2 Cl 0.72758(8) 0.56050(8) 0.08712(5) 0.03301(16) Uani 1 1 d . . . Cl3 Cl 0.78555(8) 0.76788(8) 0.28748(5) 0.03954(18) Uani 1 1 d . . . Cl4 Cl 0.92250(8) 0.15683(8) 0.20186(5) 0.03738(18) Uani 1 1 d . . . Cl5 Cl 0.96289(8) 0.78379(7) 0.04728(5) 0.03477(17) Uani 1 1 d . . . N1 N 0.4135(3) 0.9397(2) 0.26046(14) 0.0231(5) Uani 1 1 d . . . Zn1 Zn 0.89242(4) 0.64348(3) 0.15093(2) 0.03009(10) Uani 1 1 d . . . Zn2 Zn 0.94160(4) 0.32144(3) 0.10342(2) 0.03119(10) Uani 1 1 d . . . H1N H 0.525(3) 0.895(3) 0.2621(18) 0.037 Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0360(16) 0.0487(18) 0.0187(13) 0.0085(12) 0.0028(12) -0.0205(14) C2 0.0362(16) 0.0383(16) 0.0308(15) 0.0106(12) -0.0018(13) -0.0200(14) C3 0.0278(15) 0.0335(15) 0.0241(13) 0.0032(11) -0.0016(11) -0.0150(13) C4 0.0221(13) 0.0336(14) 0.0147(12) 0.0033(10) -0.0005(10) -0.0133(12) C5 0.0229(14) 0.0329(15) 0.0191(12) 0.0017(11) -0.0036(11) -0.0117(12) C6 0.0300(15) 0.0435(17) 0.0216(13) -0.0031(12) 0.0025(12) -0.0132(14) C7 0.0477(18) 0.0310(15) 0.0321(15) 0.0008(12) 0.0091(13) -0.0195(14) C8 0.053(2) 0.0364(18) 0.0544(19) 0.0030(15) 0.0093(16) -0.0126(16) C9 0.076(3) 0.057(2) 0.0484(19) -0.0065(16) -0.0064(18) -0.040(2) C10 0.0418(17) 0.0324(15) 0.0219(13) -0.0017(11) 0.0040(12) -0.0164(14) C11 0.099(3) 0.079(3) 0.057(2) 0.0243(19) -0.032(2) -0.070(3) C12 0.074(3) 0.0315(18) 0.055(2) -0.0079(15) 0.0272(19) -0.0136(18) C13 0.0235(13) 0.0311(14) 0.0223(13) 0.0006(11) 0.0011(11) -0.0141(12) C14 0.0198(13) 0.0280(13) 0.0166(11) 0.0055(10) -0.0013(10) -0.0091(11) C15 0.0175(13) 0.0273(14) 0.0230(13) 0.0077(10) -0.0045(10) -0.0088(11) C16 0.0201(13) 0.0252(13) 0.0195(12) 0.0042(10) -0.0031(10) -0.0074(11) C17 0.0335(16) 0.0418(16) 0.0267(14) 0.0057(12) 0.0000(12) -0.0238(14) C18 0.0341(16) 0.0401(16) 0.0256(14) -0.0020(12) 0.0004(12) -0.0226(14) Cl1 0.0252(3) 0.0330(4) 0.0365(4) 0.0040(3) -0.0072(3) -0.0105(3) Cl2 0.0233(3) 0.0374(4) 0.0331(4) -0.0005(3) -0.0034(3) -0.0101(3) Cl3 0.0304(4) 0.0512(5) 0.0280(4) -0.0099(3) 0.0008(3) -0.0121(3) Cl4 0.0354(4) 0.0447(4) 0.0344(4) 0.0077(3) -0.0003(3) -0.0218(3) Cl5 0.0387(4) 0.0325(4) 0.0321(4) -0.0016(3) 0.0043(3) -0.0171(3) N1 0.0226(11) 0.0274(12) 0.0186(11) 0.0012(9) 0.0002(9) -0.0117(10) Zn1 0.02687(18) 0.03240(19) 0.02615(17) -0.00211(13) 0.00198(13) -0.01071(15) Zn2 0.02889(19) 0.03354(19) 0.02958(18) 0.00269(14) -0.00115(14) -0.01398(15) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.375(4) . ? C1 C6 1.375(4) . ? C1 H1 0.9500 . ? C2 C3 1.395(3) . ? C2 H2 0.9500 . ? C3 C4 1.391(3) . ? C3 C7 1.510(4) . ? C4 C5 1.395(3) . ? C4 N1 1.470(3) . ? C5 C6 1.398(3) . ? C5 C10 1.518(3) . ? C6 H6 0.9500 . ? C7 C9 1.519(4) . ? C7 C8 1.533(4) . ? C7 H7 1.0000 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C11 1.519(4) . ? C10 C12 1.520(4) . ? C10 H10 1.0000 . ? 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 N1 1.274(3) . ? C13 C14 1.477(3) . ? C13 H13 0.9500 . ? C14 C15 1.404(3) . ? C14 C16 1.407(3) . ? C15 C16 1.403(3) 2_675 ? C15 C17 1.503(3) . ? C16 C15 1.403(3) 2_675 ? C16 C18 1.504(3) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? Cl1 Zn1 2.3074(8) . ? Cl1 Zn2 2.3282(7) . ? Cl2 Zn2 2.3113(8) . ? Cl2 Zn1 2.3365(7) . ? Cl3 Zn1 2.1996(7) . ? Cl4 Zn2 2.1850(7) . ? Cl5 Zn1 2.2730(7) . ? Cl5 Zn2 2.2930(7) 2_765 ? N1 H1N 0.94(3) . ? Zn1 Zn2 3.1406(5) . ? Zn2 Cl5 2.2930(7) 2_765 ? 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 C2 C1 C6 120.6(2) . . ? C2 C1 H1 119.7 . . ? C6 C1 H1 119.7 . . ? C1 C2 C3 121.5(3) . . ? C1 C2 H2 119.2 . . ? C3 C2 H2 119.2 . . ? C4 C3 C2 116.1(2) . . ? C4 C3 C7 123.6(2) . . ? C2 C3 C7 120.2(2) . . ? C3 C4 C5 124.3(2) . . ? C3 C4 N1 116.7(2) . . ? C5 C4 N1 118.9(2) . . ? C4 C5 C6 116.4(2) . . ? C4 C5 C10 122.9(2) . . ? C6 C5 C10 120.6(2) . . ? C1 C6 C5 121.0(2) . . ? C1 C6 H6 119.5 . . ? C5 C6 H6 119.5 . . ? C3 C7 C9 110.7(2) . . ? C3 C7 C8 111.7(2) . . ? C9 C7 C8 111.6(3) . . ? C3 C7 H7 107.5 . . ? C9 C7 H7 107.5 . . ? C8 C7 H7 107.5 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C5 C10 C11 110.1(2) . . ? C5 C10 C12 112.1(2) . . ? C11 C10 C12 112.6(3) . . ? C5 C10 H10 107.2 . . ? C11 C10 H10 107.2 . . ? C12 C10 H10 107.2 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N1 C13 C14 124.8(2) . . ? N1 C13 H13 117.6 . . ? C14 C13 H13 117.6 . . ? C15 C14 C16 122.8(2) . . ? C15 C14 C13 115.6(2) . . ? C16 C14 C13 121.6(2) . . ? C14 C15 C16 119.3(2) . 2_675 ? C14 C15 C17 121.1(2) . . ? C16 C15 C17 119.6(2) 2_675 . ? C15 C16 C14 118.0(2) 2_675 . ? C15 C16 C18 119.1(2) 2_675 . ? C14 C16 C18 122.9(2) . . ? 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 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? Zn1 Cl1 Zn2 85.30(2) . . ? Zn2 Cl2 Zn1 85.02(2) . . ? Zn1 Cl5 Zn2 114.24(3) . 2_765 ? C13 N1 C4 124.5(2) . . ? C13 N1 H1N 121.0(15) . . ? C4 N1 H1N 113.7(15) . . ? Cl3 Zn1 Cl5 109.65(3) . . ? Cl3 Zn1 Cl1 117.89(3) . . ? Cl5 Zn1 Cl1 107.98(3) . . ? Cl3 Zn1 Cl2 111.87(3) . . ? Cl5 Zn1 Cl2 114.20(3) . . ? Cl1 Zn1 Cl2 94.69(3) . . ? Cl3 Zn1 Zn2 125.85(2) . . ? Cl5 Zn1 Zn2 124.49(2) . . ? Cl1 Zn1 Zn2 47.631(19) . . ? Cl2 Zn1 Zn2 47.152(19) . . ? Cl4 Zn2 Cl5 109.87(3) . 2_765 ? Cl4 Zn2 Cl2 121.40(3) . . ? Cl5 Zn2 Cl2 108.69(3) 2_765 . ? Cl4 Zn2 Cl1 111.68(3) . . ? Cl5 Zn2 Cl1 109.19(3) 2_765 . ? Cl2 Zn2 Cl1 94.81(3) . . ? Cl4 Zn2 Zn1 128.64(2) . . ? Cl5 Zn2 Zn1 121.12(2) 2_765 . ? Cl2 Zn2 Zn1 47.831(19) . . ? Cl1 Zn2 Zn1 47.074(18) . . ? 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 C6 C1 C2 C3 2.9(4) . . . . ? C1 C2 C3 C4 -1.4(4) . . . . ? C1 C2 C3 C7 -179.1(3) . . . . ? C2 C3 C4 C5 -1.2(4) . . . . ? C7 C3 C4 C5 176.3(2) . . . . ? C2 C3 C4 N1 176.2(2) . . . . ? C7 C3 C4 N1 -6.3(4) . . . . ? C3 C4 C5 C6 2.3(4) . . . . ? N1 C4 C5 C6 -175.0(2) . . . . ? C3 C4 C5 C10 -179.3(2) . . . . ? N1 C4 C5 C10 3.3(4) . . . . ? C2 C1 C6 C5 -1.7(4) . . . . ? C4 C5 C6 C1 -0.8(4) . . . . ? C10 C5 C6 C1 -179.2(2) . . . . ? C4 C3 C7 C9 -110.1(3) . . . . ? C2 C3 C7 C9 67.4(3) . . . . ? C4 C3 C7 C8 124.9(3) . . . . ? C2 C3 C7 C8 -57.6(3) . . . . ? C4 C5 C10 C11 -93.8(3) . . . . ? C6 C5 C10 C11 84.5(3) . . . . ? C4 C5 C10 C12 140.1(3) . . . . ? C6 C5 C10 C12 -41.7(3) . . . . ? N1 C13 C14 C15 127.9(3) . . . . ? N1 C13 C14 C16 -53.3(4) . . . . ? C16 C14 C15 C16 0.9(4) . . . 2_675 ? C13 C14 C15 C16 179.6(2) . . . 2_675 ? C16 C14 C15 C17 178.5(2) . . . . ? C13 C14 C15 C17 -2.7(3) . . . . ? C15 C14 C16 C15 -0.8(4) . . . 2_675 ? C13 C14 C16 C15 -179.5(2) . . . 2_675 ? C15 C14 C16 C18 176.8(2) . . . . ? C13 C14 C16 C18 -1.9(4) . . . . ? C14 C13 N1 C4 -176.0(2) . . . . ? C3 C4 N1 C13 94.3(3) . . . . ? C5 C4 N1 C13 -88.1(3) . . . . ? Zn2 Cl5 Zn1 Cl3 -175.43(3) 2_765 . . . ? Zn2 Cl5 Zn1 Cl1 54.91(4) 2_765 . . . ? Zn2 Cl5 Zn1 Cl2 -48.98(4) 2_765 . . . ? Zn2 Cl5 Zn1 Zn2 4.45(4) 2_765 . . . ? Zn2 Cl1 Zn1 Cl3 114.47(3) . . . . ? Zn2 Cl1 Zn1 Cl5 -120.65(3) . . . . ? Zn2 Cl1 Zn1 Cl2 -3.32(2) . . . . ? Zn2 Cl2 Zn1 Cl3 -119.24(3) . . . . ? Zn2 Cl2 Zn1 Cl5 115.46(3) . . . . ? Zn2 Cl2 Zn1 Cl1 3.35(2) . . . . ? Zn1 Cl2 Zn2 Cl4 115.74(3) . . . . ? Zn1 Cl2 Zn2 Cl5 -115.45(3) . . . 2_765 ? Zn1 Cl2 Zn2 Cl1 -3.32(2) . . . . ? Zn1 Cl1 Zn2 Cl4 -123.23(3) . . . . ? Zn1 Cl1 Zn2 Cl5 115.06(3) . . . 2_765 ? Zn1 Cl1 Zn2 Cl2 3.36(2) . . . . ? Cl3 Zn1 Zn2 Cl4 -12.61(4) . . . . ? Cl5 Zn1 Zn2 Cl4 167.52(3) . . . . ? Cl1 Zn1 Zn2 Cl4 84.39(4) . . . . ? Cl2 Zn1 Zn2 Cl4 -100.12(4) . . . . ? Cl3 Zn1 Zn2 Cl5 175.12(3) . . . 2_765 ? Cl5 Zn1 Zn2 Cl5 -4.74(5) . . . 2_765 ? Cl1 Zn1 Zn2 Cl5 -87.87(3) . . . 2_765 ? Cl2 Zn1 Zn2 Cl5 87.61(3) . . . 2_765 ? Cl3 Zn1 Zn2 Cl2 87.51(3) . . . . ? Cl5 Zn1 Zn2 Cl2 -92.35(3) . . . . ? Cl1 Zn1 Zn2 Cl2 -175.48(3) . . . . ? Cl3 Zn1 Zn2 Cl1 -97.01(4) . . . . ? Cl5 Zn1 Zn2 Cl1 83.13(3) . . . . ? Cl2 Zn1 Zn2 Cl1 175.48(3) . . . . ? _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.978 _refine_diff_density_max 0.556 _refine_diff_density_min -0.287 _refine_diff_density_rms 0.072 data_simon_a _database_code_depnum_ccdc_archive 'CCDC 824570' #TrackingRef '- combined.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H50 Cl6 N2 Pd3' _chemical_formula_sum 'C36 H50 Cl6 N2 Pd3' _chemical_formula_weight 1042.68 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 'C 1 c 1' 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 15.708(3) _cell_length_b 18.709(3) _cell_length_c 14.422(2) _cell_angle_alpha 90.00 _cell_angle_beta 101.312(18) _cell_angle_gamma 90.00 _cell_volume 4155.9(12) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 2506 _cell_measurement_theta_min 3.1146 _cell_measurement_theta_max 26.6738 _exptl_crystal_description needle _exptl_crystal_colour brown _exptl_crystal_size_max 0.0064373 _exptl_crystal_size_mid 0.0030471 _exptl_crystal_size_min 0.0003215 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.666 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2080 _exptl_absorpt_coefficient_mu 1.697 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.971 _exptl_absorpt_correction_T_max 0.992 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET) (compiled Jan 20 2011,15:58:25) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Eos' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.1042 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16382 _diffrn_reflns_av_R_equivalents 0.0699 _diffrn_reflns_av_sigmaI/netI 0.1323 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max -4 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 5.30 _diffrn_reflns_theta_max 26.73 _reflns_number_total 2932 _reflns_number_gt 2169 _reflns_threshold_expression >2\s(I) _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET) (compiled Jan 20 2011,15:58:25) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET) (compiled Jan 20 2011,15:58:25) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET) (compiled Jan 20 2011,15:58:25) ; _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0548P)^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 0.08(11) _refine_ls_number_reflns 2932 _refine_ls_number_parameters 287 _refine_ls_number_restraints 143 _refine_ls_R_factor_all 0.1045 _refine_ls_R_factor_gt 0.0687 _refine_ls_wR_factor_ref 0.1537 _refine_ls_wR_factor_gt 0.1328 _refine_ls_goodness_of_fit_ref 1.076 _refine_ls_restrained_S_all 1.060 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd -0.06969(8) 0.43249(10) 0.53362(11) 0.0238(4) Uani 0.886(3) 1 d PD A 1 Pd2 Pd 0.11312(9) 0.36379(10) 0.61892(12) 0.0226(4) Uani 0.886(3) 1 d PD A 1 Pd3 Pd 0.29895(8) 0.42892(10) 0.62102(11) 0.0225(4) Uani 0.886(3) 1 d PD A 1 Cl1 Cl -0.1433(3) 0.5234(4) 0.5876(4) 0.0345(15) Uani 0.886(3) 1 d PD A 1 Cl2 Cl 0.0056(3) 0.3326(3) 0.4922(4) 0.0281(12) Uani 0.886(3) 1 d PD A 1 Cl3 Cl -0.0009(3) 0.4003(4) 0.6870(4) 0.0333(15) Uani 0.886(3) 1 d PD A 1 Cl4 Cl 0.2237(3) 0.3285(3) 0.5452(4) 0.0263(12) Uani 0.886(3) 1 d PD A 1 Cl5 Cl 0.2220(3) 0.4011(4) 0.7406(3) 0.0299(14) Uani 0.886(3) 1 d PD A 1 Cl6 Cl 0.3713(3) 0.5193(4) 0.7073(4) 0.0342(14) Uani 0.886(3) 1 d PD A 1 N1 N 0.3517(5) 0.4581(10) 0.5082(10) 0.030(5) Uiso 0.886(3) 1 d PD A 1 N2 N -0.1174(6) 0.4647(11) 0.3996(10) 0.051(6) Uiso 0.886(3) 1 d PD A 1 C1 C -0.2543(6) 0.3968(6) 0.3423(12) 0.021(4) Uiso 0.886(3) 1 d PD A 1 C2 C -0.3457(7) 0.4003(8) 0.3132(15) 0.028(5) Uiso 0.886(3) 1 d PD A 1 H2 H -0.3765 0.3565 0.3007 0.034 Uiso 0.886(3) 1 calc PR A 1 C3 C -0.3919(8) 0.4613(7) 0.3022(15) 0.029(4) Uiso 0.886(3) 1 d PD A 1 H3 H -0.4535 0.4605 0.2845 0.035 Uiso 0.886(3) 1 calc PR A 1 C4 C -0.3476(7) 0.5251(8) 0.3172(15) 0.029(5) Uiso 0.886(3) 1 d PD A 1 H4 H -0.3795 0.5685 0.3069 0.035 Uiso 0.886(3) 1 calc PR A 1 C5 C -0.2569(6) 0.5285(6) 0.3472(11) 0.016(4) Uiso 0.886(3) 1 d PD A 1 C6 C -0.2117(5) 0.4638(6) 0.3629(10) 0.013(3) Uiso 0.886(3) 1 d PD A 1 C7 C -0.2168(9) 0.5993(7) 0.3592(11) 0.028(5) Uiso 0.886(3) 1 d PD A 1 H7 H -0.1542 0.5920 0.3887 0.034 Uiso 0.886(3) 1 calc PR A 1 C8 C -0.2192(15) 0.6383(13) 0.2610(13) 0.052(6) Uiso 0.886(3) 1 d PD A 1 H8A H -0.1916 0.6853 0.2722 0.078 Uiso 0.886(3) 1 calc PR A 1 H8B H -0.2796 0.6443 0.2283 0.078 Uiso 0.886(3) 1 calc PR A 1 H8C H -0.1879 0.6095 0.2219 0.078 Uiso 0.886(3) 1 calc PR A 1 C9 C -0.2552(13) 0.6543(11) 0.4248(15) 0.042(6) Uiso 0.886(3) 1 d PD A 1 H9A H -0.2232 0.6995 0.4278 0.063 Uiso 0.886(3) 1 calc PR A 1 H9B H -0.2494 0.6344 0.4885 0.063 Uiso 0.886(3) 1 calc PR A 1 H9C H -0.3167 0.6630 0.3982 0.063 Uiso 0.886(3) 1 calc PR A 1 C10 C -0.2096(9) 0.3273(7) 0.3526(11) 0.028(4) Uiso 0.886(3) 1 d PD A 1 H10 H -0.1462 0.3373 0.3738 0.034 Uiso 0.886(3) 1 calc PR A 1 C11 C -0.2382(17) 0.2762(14) 0.4314(18) 0.070(8) Uiso 0.886(3) 1 d PD A 1 H11A H -0.2061 0.2311 0.4348 0.104 Uiso 0.886(3) 1 calc PR A 1 H11B H -0.3006 0.2665 0.4141 0.104 Uiso 0.886(3) 1 calc PR A 1 H11C H -0.2253 0.3000 0.4931 0.104 Uiso 0.886(3) 1 calc PR A 1 C12 C -0.2219(16) 0.2967(14) 0.2529(13) 0.062(8) Uiso 0.886(3) 1 d PD A 1 H12A H -0.1935 0.2499 0.2550 0.094 Uiso 0.886(3) 1 calc PR A 1 H12B H -0.1961 0.3291 0.2127 0.094 Uiso 0.886(3) 1 calc PR A 1 H12C H -0.2840 0.2913 0.2268 0.094 Uiso 0.886(3) 1 calc PR A 1 C13 C -0.0682(5) 0.4778(10) 0.3422(9) 0.016(4) Uiso 0.886(3) 1 d PD A 1 H13A H -0.0840 0.5261 0.3165 0.020 Uiso 0.886(3) 1 calc PR A 1 H13B H -0.0849 0.4440 0.2889 0.020 Uiso 0.886(3) 1 calc PR A 1 C14 C 0.0305(5) 0.4761(8) 0.3683(11) 0.016(3) Uiso 0.886(3) 1 d PD A 1 C15 C 0.0726(5) 0.5317(7) 0.4277(11) 0.011(3) Uiso 0.886(3) 1 d PD A 1 C16 C 0.1632(5) 0.5288(7) 0.4504(10) 0.010(3) Uiso 0.886(3) 1 d PD A 1 C17 C 0.2058(5) 0.4781(8) 0.4138(12) 0.022(4) Uiso 0.886(3) 1 d PD A 1 C18 C 0.1621(5) 0.4246(9) 0.3488(12) 0.020(4) Uiso 0.886(3) 1 d PD A 1 C19 C 0.0741(6) 0.4257(9) 0.3277(13) 0.023(4) Uiso 0.886(3) 1 d PD A 1 C20 C 0.0227(10) 0.5952(10) 0.4701(17) 0.034(5) Uiso 0.886(3) 1 d PD A 1 H20A H -0.0401 0.5898 0.4479 0.052 Uiso 0.886(3) 1 calc PR A 1 H20B H 0.0414 0.6414 0.4489 0.052 Uiso 0.886(3) 1 calc PR A 1 H20C H 0.0363 0.5931 0.5393 0.052 Uiso 0.886(3) 1 calc PR A 1 C21 C 0.2125(10) 0.5908(10) 0.5160(15) 0.033(5) Uiso 0.886(3) 1 d PD A 1 H21A H 0.1698 0.6232 0.5348 0.050 Uiso 0.886(3) 1 calc PR A 1 H21B H 0.2494 0.6177 0.4808 0.050 Uiso 0.886(3) 1 calc PR A 1 H21C H 0.2486 0.5698 0.5726 0.050 Uiso 0.886(3) 1 calc PR A 1 C22 C 0.2140(8) 0.3729(10) 0.3046(13) 0.019(4) Uiso 0.886(3) 1 d PD A 1 H22A H 0.2759 0.3810 0.3293 0.028 Uiso 0.886(3) 1 calc PR A 1 H22B H 0.2016 0.3797 0.2359 0.028 Uiso 0.886(3) 1 calc PR A 1 H22C H 0.1986 0.3241 0.3195 0.028 Uiso 0.886(3) 1 calc PR A 1 C23 C 0.0222(11) 0.3685(13) 0.2591(18) 0.041(6) Uiso 0.886(3) 1 d PD A 1 H23A H -0.0402 0.3776 0.2517 0.061 Uiso 0.886(3) 1 calc PR A 1 H23B H 0.0355 0.3206 0.2855 0.061 Uiso 0.886(3) 1 calc PR A 1 H23C H 0.0390 0.3716 0.1972 0.061 Uiso 0.886(3) 1 calc PR A 1 C24 C 0.3051(6) 0.4756(11) 0.4338(10) 0.023(4) Uiso 0.886(3) 1 d PD A 1 H24A H 0.3208 0.4437 0.3851 0.028 Uiso 0.886(3) 1 calc PR A 1 H24B H 0.3242 0.5242 0.4197 0.028 Uiso 0.886(3) 1 calc PR A 1 C25 C 0.4454(5) 0.4572(6) 0.5190(13) 0.018(4) Uiso 0.886(3) 1 d PD A 1 C26 C 0.4924(6) 0.5227(6) 0.5238(12) 0.014(3) Uiso 0.886(3) 1 d PD A 1 C27 C 0.5805(6) 0.5191(8) 0.5448(15) 0.029(5) Uiso 0.886(3) 1 d PD A 1 H27 H 0.6128 0.5624 0.5508 0.035 Uiso 0.886(3) 1 calc PR A 1 C28 C 0.6251(7) 0.4550(7) 0.5576(15) 0.028(5) Uiso 0.886(3) 1 d PD A 1 H28 H 0.6867 0.4548 0.5740 0.034 Uiso 0.886(3) 1 calc PR A 1 C29 C 0.5783(7) 0.3894(8) 0.5463(16) 0.028(5) Uiso 0.886(3) 1 d PD A 1 H29 H 0.6070 0.3445 0.5536 0.034 Uiso 0.886(3) 1 calc PR A 1 C30 C 0.4890(6) 0.3945(6) 0.5240(13) 0.019(4) Uiso 0.886(3) 1 d PD A 1 C31 C 0.4403(8) 0.3184(7) 0.5063(11) 0.023(4) Uiso 0.886(3) 1 d PD A 1 H31 H 0.3766 0.3281 0.4967 0.027 Uiso 0.886(3) 1 calc PR A 1 C32 C 0.4580(15) 0.2856(14) 0.4117(14) 0.061(8) Uiso 0.886(3) 1 d PD A 1 H32A H 0.4430 0.3206 0.3607 0.091 Uiso 0.886(3) 1 calc PR A 1 H32B H 0.4225 0.2425 0.3960 0.091 Uiso 0.886(3) 1 calc PR A 1 H32C H 0.5196 0.2730 0.4196 0.091 Uiso 0.886(3) 1 calc PR A 1 C33 C 0.4611(15) 0.2693(12) 0.5834(16) 0.057(7) Uiso 0.886(3) 1 d PD A 1 H33A H 0.4487 0.2914 0.6409 0.086 Uiso 0.886(3) 1 calc PR A 1 H33B H 0.5229 0.2569 0.5933 0.086 Uiso 0.886(3) 1 calc PR A 1 H33C H 0.4261 0.2259 0.5690 0.086 Uiso 0.886(3) 1 calc PR A 1 C34 C 0.4488(9) 0.5940(7) 0.5102(11) 0.030(5) Uiso 0.886(3) 1 d PD A 1 H34 H 0.3853 0.5867 0.5078 0.036 Uiso 0.886(3) 1 calc PR A 1 C35 C 0.4850(17) 0.6511(14) 0.5964(18) 0.079(10) Uiso 0.886(3) 1 d PD A 1 H35A H 0.4542 0.6966 0.5834 0.119 Uiso 0.886(3) 1 calc PR A 1 H35B H 0.5473 0.6588 0.6006 0.119 Uiso 0.886(3) 1 calc PR A 1 H35C H 0.4749 0.6316 0.6564 0.119 Uiso 0.886(3) 1 calc PR A 1 C36 C 0.4600(13) 0.6277(13) 0.4147(14) 0.045(6) Uiso 0.886(3) 1 d PD A 1 H36A H 0.4308 0.6742 0.4066 0.067 Uiso 0.886(3) 1 calc PR A 1 H36B H 0.4343 0.5960 0.3626 0.067 Uiso 0.886(3) 1 calc PR A 1 H36C H 0.5219 0.6340 0.4148 0.067 Uiso 0.886(3) 1 calc PR A 1 Pd1B Pd -0.0697(4) 0.4343(6) 0.2503(7) 0.013(3) Uani 0.114(3) 1 d PD A -2 Pd2B Pd 0.1140(4) 0.3653(6) 0.2460(7) 0.028(4) Uani 0.114(3) 1 d PD A -2 Pd3B Pd 0.2991(4) 0.4302(7) 0.3299(7) 0.020(3) Uani 0.114(3) 1 d PD A -2 Cl1B Cl -0.123(2) 0.4602(19) 0.3833(16) 0.031(4) Uiso 0.114(3) 1 d PD A -2 Cl2B Cl 0.0059(9) 0.4092(15) 0.1286(9) 0.031(4) Uiso 0.114(3) 1 d PD A -2 Cl3B Cl 0.0015(9) 0.3317(10) 0.3186(16) 0.031(4) Uiso 0.114(3) 1 d PD A -2 Cl4B Cl 0.2245(8) 0.4038(15) 0.1742(9) 0.031(4) Uiso 0.114(3) 1 d PD A -2 Cl5B Cl 0.2232(8) 0.3303(11) 0.3694(15) 0.031(4) Uiso 0.114(3) 1 d PD A -2 Cl6B Cl 0.360(2) 0.453(2) 0.4833(12) 0.031(4) Uiso 0.114(3) 1 d PD A -2 N1B N 0.3537(13) 0.5221(13) 0.291(2) 0.060 Uiso 0.114(3) 1 d PGD A -2 N2B N -0.1162(13) 0.5304(12) 0.197(2) 0.060 Uiso 0.114(3) 1 d PGD A -2 C1B C -0.2539(13) 0.509(2) 0.083(3) 0.060 Uiso 0.114(3) 1 d PGD A -2 C2B C -0.3449(13) 0.517(3) 0.064(3) 0.060 Uiso 0.114(3) 1 d PGD A -2 H2' H -0.3760 0.4972 0.0058 0.072 Uiso 0.114(3) 1 calc PR A -2 C3' C -0.3913(14) 0.549(2) 0.120(4) 0.060 Uiso 0.114(3) 1 d PGD A -2 H3' H -0.4530 0.5483 0.1069 0.072 Uiso 0.114(3) 1 calc PR A -2 C4' C -0.3460(16) 0.584(2) 0.199(4) 0.060 Uiso 0.114(3) 1 d PGD A -2 H4' H -0.3773 0.6127 0.2345 0.072 Uiso 0.114(3) 1 calc PR A -2 C5' C -0.2551(16) 0.579(2) 0.228(3) 0.060 Uiso 0.114(3) 1 d PGD A -2 C6' C -0.2105(13) 0.5402(16) 0.170(3) 0.060 Uiso 0.114(3) 1 d PGD A -2 C7' C -0.215(2) 0.618(3) 0.312(4) 0.060 Uiso 0.114(3) 1 d PGD A -2 H7' H -0.1524 0.6036 0.3254 0.072 Uiso 0.114(3) 1 calc PR A -2 C8' C -0.214(2) 0.702(3) 0.298(6) 0.060 Uiso 0.114(3) 1 d PGD A -2 H8'1 H -0.1860 0.7250 0.3574 0.090 Uiso 0.114(3) 1 calc PR A -2 H8'2 H -0.2737 0.7196 0.2797 0.090 Uiso 0.114(3) 1 calc PR A -2 H8'3 H -0.1817 0.7138 0.2484 0.090 Uiso 0.114(3) 1 calc PR A -2 C9' C -0.249(2) 0.603(4) 0.407(4) 0.060 Uiso 0.114(3) 1 d PGD A -2 H9'1 H -0.2164 0.6327 0.4585 0.090 Uiso 0.114(3) 1 calc PR A -2 H9'2 H -0.2396 0.5524 0.4243 0.090 Uiso 0.114(3) 1 calc PR A -2 H9'3 H -0.3106 0.6142 0.3981 0.090 Uiso 0.114(3) 1 calc PR A -2 C10B C -0.2100(13) 0.465(3) 0.022(3) 0.060 Uiso 0.114(3) 1 d PGD A -2 H10' H -0.1468 0.4672 0.0512 0.072 Uiso 0.114(3) 1 calc PR A -2 C11B C -0.2343(14) 0.381(3) 0.019(5) 0.060 Uiso 0.114(3) 1 d PGD A -2 H11D H -0.2021 0.3557 -0.0225 0.090 Uiso 0.114(3) 1 calc PR A -2 H11E H -0.2967 0.3749 -0.0043 0.090 Uiso 0.114(3) 1 calc PR A -2 H11F H -0.2187 0.3607 0.0833 0.090 Uiso 0.114(3) 1 calc PR A -2 C12B C -0.2204(17) 0.505(5) -0.071(3) 0.060 Uiso 0.114(3) 1 d PGD A -2 H12D H -0.1923 0.4783 -0.1147 0.090 Uiso 0.114(3) 1 calc PR A -2 H12E H -0.1933 0.5523 -0.0592 0.090 Uiso 0.114(3) 1 calc PR A -2 H12F H -0.2823 0.5108 -0.0978 0.090 Uiso 0.114(3) 1 calc PR A -2 C13B C -0.0663(15) 0.5809(12) 0.186(3) 0.060 Uiso 0.114(3) 1 d PGD A -2 H13C H -0.0809 0.6213 0.2242 0.072 Uiso 0.114(3) 1 calc PR A -2 H13D H -0.0835 0.5957 0.1189 0.072 Uiso 0.114(3) 1 calc PR A -2 C14B C 0.0328(15) 0.5754(10) 0.206(2) 0.060 Uiso 0.114(3) 1 d PGD A -2 C15B C 0.0749(16) 0.5730(15) 0.304(2) 0.060 Uiso 0.114(3) 1 d PGD A -2 C16B C 0.1654(15) 0.5704(15) 0.321(2) 0.060 Uiso 0.114(3) 1 d PGD A -2 C17B C 0.2064(14) 0.5706(9) 0.248(2) 0.060 Uiso 0.114(3) 1 d PGD A -2 C18B C 0.1618(15) 0.577(2) 0.150(2) 0.060 Uiso 0.114(3) 1 d PGD A -2 C19B C 0.0744(15) 0.576(2) 0.132(2) 0.060 Uiso 0.114(3) 1 d PGD A -2 C20B C 0.0235(18) 0.576(3) 0.390(2) 0.060 Uiso 0.114(3) 1 d PGD A -2 H20D H -0.0391 0.5778 0.3653 0.090 Uiso 0.114(3) 1 calc PR A -2 H20E H 0.0410 0.6192 0.4283 0.090 Uiso 0.114(3) 1 calc PR A -2 H20F H 0.0375 0.5337 0.4302 0.090 Uiso 0.114(3) 1 calc PR A -2 C21B C 0.2181(18) 0.573(3) 0.428(2) 0.060 Uiso 0.114(3) 1 d PGD A -2 H21D H 0.1771 0.5723 0.4713 0.090 Uiso 0.114(3) 1 calc PR A -2 H21E H 0.2530 0.6166 0.4380 0.090 Uiso 0.114(3) 1 calc PR A -2 H21F H 0.2564 0.5311 0.4403 0.090 Uiso 0.114(3) 1 calc PR A -2 C22B C 0.2115(17) 0.582(3) 0.073(2) 0.060 Uiso 0.114(3) 1 d PGD A -2 H22D H 0.2739 0.5815 0.0998 0.090 Uiso 0.114(3) 1 calc PR A -2 H22E H 0.1962 0.6261 0.0375 0.090 Uiso 0.114(3) 1 calc PR A -2 H22F H 0.1973 0.5407 0.0302 0.090 Uiso 0.114(3) 1 calc PR A -2 C23B C 0.0184(16) 0.565(3) 0.029(2) 0.060 Uiso 0.114(3) 1 d PGD A -2 H23D H -0.0435 0.5666 0.0320 0.090 Uiso 0.114(3) 1 calc PR A -2 H23E H 0.0325 0.5194 0.0038 0.090 Uiso 0.114(3) 1 calc PR A -2 H23F H 0.0313 0.6041 -0.0118 0.090 Uiso 0.114(3) 1 calc PR A -2 C24B C 0.3062(14) 0.5722(12) 0.263(2) 0.060 Uiso 0.114(3) 1 d PGD A -2 H24C H 0.3202 0.5872 0.2024 0.072 Uiso 0.114(3) 1 calc PR A -2 H24D H 0.3253 0.6117 0.3085 0.072 Uiso 0.114(3) 1 calc PR A -2 C25B C 0.4473(13) 0.5250(16) 0.308(3) 0.060 Uiso 0.114(3) 1 d PGD A -2 C26B C 0.4949(15) 0.568(2) 0.383(3) 0.060 Uiso 0.114(3) 1 d PGD A -2 C27B C 0.5826(15) 0.567(2) 0.396(3) 0.060 Uiso 0.114(3) 1 d PGD A -2 H27' H 0.6151 0.5946 0.4454 0.072 Uiso 0.114(3) 1 calc PR A -2 C28B C 0.6270(13) 0.526(2) 0.340(3) 0.060 Uiso 0.114(3) 1 d PGD A -2 H28' H 0.6883 0.5215 0.3569 0.072 Uiso 0.114(3) 1 calc PR A -2 C29B C 0.5795(12) 0.492(2) 0.258(3) 0.060 Uiso 0.114(3) 1 d PGD A -2 H29' H 0.6077 0.4684 0.2137 0.072 Uiso 0.114(3) 1 calc PR A -2 C30B C 0.4905(12) 0.494(2) 0.246(3) 0.060 Uiso 0.114(3) 1 d PGD A -2 C31B C 0.4409(14) 0.453(3) 0.153(3) 0.060 Uiso 0.114(3) 1 d PGD A -2 H31' H 0.3771 0.4560 0.1514 0.072 Uiso 0.114(3) 1 calc PR A -2 C32B C 0.4595(17) 0.495(5) 0.064(3) 0.060 Uiso 0.114(3) 1 d PGD A -2 H32D H 0.4437 0.5450 0.0685 0.090 Uiso 0.114(3) 1 calc PR A -2 H32E H 0.4250 0.4739 0.0062 0.090 Uiso 0.114(3) 1 calc PR A -2 H32F H 0.5213 0.4910 0.0619 0.090 Uiso 0.114(3) 1 calc PR A -2 C33B C 0.4628(14) 0.379(3) 0.149(5) 0.060 Uiso 0.114(3) 1 d PGD A -2 H33D H 0.4504 0.3545 0.2055 0.090 Uiso 0.114(3) 1 calc PR A -2 H33E H 0.5247 0.3741 0.1481 0.090 Uiso 0.114(3) 1 calc PR A -2 H33F H 0.4284 0.3569 0.0924 0.090 Uiso 0.114(3) 1 calc PR A -2 C34B C 0.4521(19) 0.612(3) 0.447(3) 0.060 Uiso 0.114(3) 1 d PGD A -2 H34' H 0.3889 0.5997 0.4321 0.072 Uiso 0.114(3) 1 calc PR A -2 C35B C 0.487(2) 0.596(5) 0.560(3) 0.060 Uiso 0.114(3) 1 d PGD A -2 H35D H 0.4565 0.6266 0.5977 0.090 Uiso 0.114(3) 1 calc PR A -2 H35E H 0.5498 0.6058 0.5769 0.090 Uiso 0.114(3) 1 calc PR A -2 H35F H 0.4768 0.5456 0.5737 0.090 Uiso 0.114(3) 1 calc PR A -2 C36B C 0.459(2) 0.693(3) 0.427(5) 0.060 Uiso 0.114(3) 1 d PGD A -2 H36D H 0.4305 0.7201 0.4705 0.090 Uiso 0.114(3) 1 calc PR A -2 H36E H 0.4313 0.7035 0.3618 0.090 Uiso 0.114(3) 1 calc PR A -2 H36F H 0.5206 0.7067 0.4374 0.090 Uiso 0.114(3) 1 calc PR A -2 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 0.0189(7) 0.0325(13) 0.0191(8) -0.0022(8) 0.0018(5) -0.0013(6) Pd2 0.0219(6) 0.0258(10) 0.0205(7) 0.0012(8) 0.0047(5) -0.0002(6) Pd3 0.0169(6) 0.0306(12) 0.0197(8) 0.0004(9) 0.0026(5) 0.0020(6) Cl1 0.025(2) 0.050(5) 0.028(3) -0.006(3) 0.0032(16) 0.007(2) Cl2 0.027(2) 0.026(4) 0.029(3) 0.000(3) -0.0021(16) 0.0000(19) Cl3 0.025(2) 0.053(5) 0.021(3) -0.002(3) 0.0029(16) 0.005(2) Cl4 0.028(2) 0.027(4) 0.026(3) 0.002(3) 0.0088(16) 0.0043(19) Cl5 0.026(2) 0.044(4) 0.019(3) 0.001(3) 0.0021(16) -0.003(2) Cl6 0.028(2) 0.047(5) 0.027(3) -0.009(3) 0.0043(17) -0.010(2) Pd1B 0.014(5) 0.009(7) 0.013(6) -0.005(5) -0.006(3) -0.001(4) Pd2B 0.016(5) 0.034(10) 0.031(8) -0.008(7) 0.000(4) -0.006(5) Pd3B 0.008(5) 0.027(9) 0.024(6) -0.010(6) -0.001(3) 0.005(4) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 N2 2.023(14) . ? Pd1 Cl1 2.279(6) . ? Pd1 Cl3 2.343(6) . ? Pd1 Cl2 2.351(6) . ? Pd1 Pd2 3.166(2) . ? Pd2 Cl4 2.304(4) . ? Pd2 Cl5 2.305(5) . ? Pd2 Cl2 2.307(5) . ? Pd2 Cl3 2.309(5) . ? Pd2 Pd3 3.1577(19) . ? Pd3 N1 2.040(14) . ? Pd3 Cl6 2.268(6) . ? Pd3 Cl5 2.351(5) . ? Pd3 Cl4 2.370(6) . ? N1 C24 1.219(9) . ? N1 C25 1.450(8) . ? N2 C13 1.263(9) . ? N2 C6 1.472(8) . ? C1 C2 1.415(9) . ? C1 C6 1.424(8) . ? C1 C10 1.471(9) . ? C2 C3 1.347(9) . ? C2 H2 0.9500 . ? C3 C4 1.376(9) . ? C3 H3 0.9500 . ? C4 C5 1.407(9) . ? C4 H4 0.9500 . ? C5 C6 1.400(8) . ? C5 C7 1.461(9) . ? C7 C8 1.588(10) . ? C7 C9 1.595(9) . ? C7 H7 1.0000 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C12 1.525(10) . ? C10 C11 1.615(9) . ? C10 H10 1.0000 . ? 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 1.523(8) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C19 1.362(8) . ? C14 C15 1.426(8) . ? C15 C16 1.399(8) . ? C15 C20 1.608(9) . ? C16 C17 1.327(8) . ? C16 C21 1.599(9) . ? C17 C18 1.448(8) . ? C17 C24 1.530(8) . ? C18 C19 1.357(8) . ? C18 C22 1.486(9) . ? C19 C23 1.572(9) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C30 1.353(8) . ? C25 C26 1.426(8) . ? C26 C27 1.359(8) . ? C26 C34 1.496(9) . ? C27 C28 1.383(9) . ? C27 H27 0.9500 . ? C28 C29 1.424(9) . ? C28 H28 0.9500 . ? C29 C30 1.379(9) . ? C29 H29 0.9500 . ? C30 C31 1.612(9) . ? C31 C33 1.431(10) . ? C31 C32 1.570(9) . ? C31 H31 1.0000 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 C36 1.555(10) . ? C34 C35 1.652(10) . ? C34 H34 1.0000 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? Pd1B N2B 2.031(14) . ? Pd1B Cl1B 2.294(11) . ? Pd1B Cl3B 2.339(10) . ? Pd1B Cl2B 2.351(10) . ? Pd1B Pd2B 3.173(7) . ? Pd2B Cl2B 2.302(10) . ? Pd2B Cl4B 2.303(9) . ? Pd2B Cl5B 2.310(10) . ? Pd2B Cl3B 2.312(9) . ? Pd2B Pd3B 3.164(7) . ? Pd3B N1B 2.049(15) . ? Pd3B Cl6B 2.271(11) . ? Pd3B Cl5B 2.347(10) . ? Pd3B Cl4B 2.373(11) . ? N1B C24B 1.2148 . ? N1B C25B 1.4431 . ? N2B C13B 1.2589 . ? N2B C6' 1.4689 . ? C1B C2B 1.4099 . ? C1B C6' 1.4290 . ? C1B C10B 1.4683 . ? C2B C3' 1.3459 . ? C2B H2' 0.9500 . ? C3' C4' 1.3727 . ? C3' H3' 0.9500 . ? C4' C5' 1.4101 . ? C4' H4' 0.9500 . ? C5' C6' 1.3985 . ? C5' C7' 1.4572 . ? C7' C8' 1.5795 . ? C7' C9' 1.5928 . ? C7' H7' 1.0000 . ? C8' H8'1 0.9800 . ? C8' H8'2 0.9800 . ? C8' H8'3 0.9800 . ? C9' H9'1 0.9800 . ? C9' H9'2 0.9800 . ? C9' H9'3 0.9800 . ? C10B C12B 1.5210 . ? C10B C11B 1.6121 . ? C10B H10' 1.0000 . ? C11B H11D 0.9800 . ? C11B H11E 0.9800 . ? C11B H11F 0.9800 . ? C12B H12D 0.9800 . ? C12B H12E 0.9800 . ? C12B H12F 0.9800 . ? C13B C14B 1.5300 . ? C13B H13C 0.9900 . ? C13B H13D 0.9900 . ? C14B C19B 1.3625 . ? C14B C15B 1.4322 . ? C15B C16B 1.3947 . ? C15B C20B 1.6146 . ? C16B C17B 1.3314 . ? C16B C21B 1.6060 . ? C17B C18B 1.4525 . ? C17B C24B 1.5398 . ? C18B C19B 1.3470 . ? C18B C22B 1.4863 . ? C19B C23B 1.5795 . ? C20B H20D 0.9800 . ? C20B H20E 0.9800 . ? C20B H20F 0.9800 . ? C21B H21D 0.9800 . ? C21B H21E 0.9800 . ? C21B H21F 0.9800 . ? C22B H22D 0.9800 . ? C22B H22E 0.9800 . ? C22B H22F 0.9800 . ? C23B H23D 0.9800 . ? C23B H23E 0.9800 . ? C23B H23F 0.9800 . ? C24B H24C 0.9900 . ? C24B H24D 0.9900 . ? C25B C30B 1.3549 . ? C25B C26B 1.4262 . ? C26B C27B 1.3532 . ? C26B C34B 1.4919 . ? C27B C28B 1.3863 . ? C27B H27' 0.9500 . ? C28B C29B 1.4272 . ? C28B H28' 0.9500 . ? C29B C30B 1.3770 . ? C29B H29' 0.9500 . ? C30B C31B 1.6177 . ? C31B C33B 1.4316 . ? C31B C32B 1.5738 . ? C31B H31' 1.0000 . ? C32B H32D 0.9800 . ? C32B H32E 0.9800 . ? C32B H32F 0.9800 . ? C33B H33D 0.9800 . ? C33B H33E 0.9800 . ? C33B H33F 0.9800 . ? C34B C36B 1.5501 . ? C34B C35B 1.6523 . ? C34B H34' 1.0000 . ? C35B H35D 0.9800 . ? C35B H35E 0.9800 . ? C35B H35F 0.9800 . ? C36B H36D 0.9800 . ? C36B H36E 0.9800 . ? C36B H36F 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 N2 Pd1 Cl1 89.2(5) . . ? N2 Pd1 Cl3 174.2(4) . . ? Cl1 Pd1 Cl3 92.3(2) . . ? N2 Pd1 Cl2 96.0(6) . . ? Cl1 Pd1 Cl2 174.2(2) . . ? Cl3 Pd1 Cl2 82.7(2) . . ? N2 Pd1 Pd2 129.0(3) . . ? Cl1 Pd1 Pd2 130.74(14) . . ? Cl3 Pd1 Pd2 46.65(12) . . ? Cl2 Pd1 Pd2 46.59(12) . . ? Cl4 Pd2 Cl5 85.68(18) . . ? Cl4 Pd2 Cl2 93.59(18) . . ? Cl5 Pd2 Cl2 176.5(2) . . ? Cl4 Pd2 Cl3 177.7(2) . . ? Cl5 Pd2 Cl3 96.20(19) . . ? Cl2 Pd2 Cl3 84.46(18) . . ? Cl4 Pd2 Pd3 48.39(15) . . ? Cl5 Pd2 Pd3 47.91(12) . . ? Cl2 Pd2 Pd3 129.55(14) . . ? Cl3 Pd2 Pd3 132.44(18) . . ? Cl4 Pd2 Pd1 130.20(14) . . ? Cl5 Pd2 Pd1 130.81(17) . . ? Cl2 Pd2 Pd1 47.77(14) . . ? Cl3 Pd2 Pd1 47.55(14) . . ? Pd3 Pd2 Pd1 127.83(7) . . ? N1 Pd3 Cl6 90.0(5) . . ? N1 Pd3 Cl5 172.9(3) . . ? Cl6 Pd3 Cl5 92.1(2) . . ? N1 Pd3 Cl4 95.1(5) . . ? Cl6 Pd3 Cl4 174.3(2) . . ? Cl5 Pd3 Cl4 83.18(18) . . ? N1 Pd3 Pd2 127.9(3) . . ? Cl6 Pd3 Pd2 130.97(13) . . ? Cl5 Pd3 Pd2 46.69(12) . . ? Cl4 Pd3 Pd2 46.62(10) . . ? Pd2 Cl2 Pd1 85.6(2) . . ? Pd2 Cl3 Pd1 85.79(18) . . ? Pd2 Cl4 Pd3 84.99(19) . . ? Pd2 Cl5 Pd3 85.40(17) . . ? C24 N1 C25 121.3(9) . . ? C24 N1 Pd3 120.4(8) . . ? C25 N1 Pd3 118.3(8) . . ? C13 N2 C6 118.0(10) . . ? C13 N2 Pd1 121.6(8) . . ? C6 N2 Pd1 119.9(8) . . ? C2 C1 C6 115.4(8) . . ? C2 C1 C10 120.4(9) . . ? C6 C1 C10 124.1(9) . . ? C3 C2 C1 124.5(10) . . ? C3 C2 H2 117.8 . . ? C1 C2 H2 117.8 . . ? C2 C3 C4 118.2(10) . . ? C2 C3 H3 120.9 . . ? C4 C3 H3 120.9 . . ? C3 C4 C5 122.6(10) . . ? C3 C4 H4 118.7 . . ? C5 C4 H4 118.7 . . ? C6 C5 C4 117.4(8) . . ? C6 C5 C7 124.8(9) . . ? C4 C5 C7 117.7(9) . . ? C5 C6 C1 121.7(8) . . ? C5 C6 N2 119.4(10) . . ? C1 C6 N2 118.9(10) . . ? C5 C7 C8 112.1(12) . . ? C5 C7 C9 116.8(11) . . ? C8 C7 C9 106.6(11) . . ? C5 C7 H7 106.9 . . ? C8 C7 H7 106.9 . . ? C9 C7 H7 106.9 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C1 C10 C12 105.5(11) . . ? C1 C10 C11 113.6(11) . . ? C12 C10 C11 116.1(13) . . ? C1 C10 H10 107.0 . . ? C12 C10 H10 107.0 . . ? C11 C10 H10 107.0 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N2 C13 C14 124.0(11) . . ? N2 C13 H13A 106.3 . . ? C14 C13 H13A 106.3 . . ? N2 C13 H13B 106.3 . . ? C14 C13 H13B 106.3 . . ? H13A C13 H13B 106.4 . . ? C19 C14 C15 123.5(7) . . ? C19 C14 C13 118.8(9) . . ? C15 C14 C13 117.5(9) . . ? C16 C15 C14 116.2(8) . . ? C16 C15 C20 119.3(9) . . ? C14 C15 C20 124.4(9) . . ? C17 C16 C15 120.3(8) . . ? C17 C16 C21 122.1(9) . . ? C15 C16 C21 117.6(8) . . ? C16 C17 C18 122.7(8) . . ? C16 C17 C24 121.4(9) . . ? C18 C17 C24 115.9(9) . . ? C19 C18 C17 117.9(8) . . ? C19 C18 C22 122.2(9) . . ? C17 C18 C22 119.8(8) . . ? C18 C19 C14 119.3(8) . . ? C18 C19 C23 120.7(9) . . ? C14 C19 C23 120.0(9) . . ? C15 C20 H20A 109.5 . . ? C15 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C15 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C16 C21 H21A 109.5 . . ? C16 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C16 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C18 C22 H22A 109.5 . . ? C18 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C18 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C19 C23 H23A 109.5 . . ? C19 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C19 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? N1 C24 C17 126.0(11) . . ? N1 C24 H24A 105.8 . . ? C17 C24 H24A 105.8 . . ? N1 C24 H24B 105.8 . . ? C17 C24 H24B 105.8 . . ? H24A C24 H24B 106.2 . . ? C30 C25 C26 119.3(8) . . ? C30 C25 N1 120.7(9) . . ? C26 C25 N1 120.0(9) . . ? C27 C26 C25 117.6(8) . . ? C27 C26 C34 119.6(9) . . ? C25 C26 C34 122.8(8) . . ? C26 C27 C28 122.7(10) . . ? C26 C27 H27 118.7 . . ? C28 C27 H27 118.7 . . ? C27 C28 C29 119.7(10) . . ? C27 C28 H28 120.1 . . ? C29 C28 H28 120.1 . . ? C30 C29 C28 116.4(10) . . ? C30 C29 H29 121.8 . . ? C28 C29 H29 121.8 . . ? C25 C30 C29 123.7(9) . . ? C25 C30 C31 122.4(8) . . ? C29 C30 C31 113.9(8) . . ? C33 C31 C32 111.8(12) . . ? C33 C31 C30 114.5(12) . . ? C32 C31 C30 108.9(11) . . ? C33 C31 H31 107.1 . . ? C32 C31 H31 107.1 . . ? C30 C31 H31 107.1 . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C31 C33 H33A 109.5 . . ? C31 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C31 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C26 C34 C36 110.4(11) . . ? C26 C34 C35 113.3(12) . . ? C36 C34 C35 108.9(12) . . ? C26 C34 H34 108.0 . . ? C36 C34 H34 108.0 . . ? C35 C34 H34 108.0 . . ? C34 C35 H35A 109.5 . . ? C34 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C34 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C34 C36 H36A 109.5 . . ? C34 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C34 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? N2B Pd1B Cl1B 87.9(8) . . ? N2B Pd1B Cl3B 172.2(9) . . ? Cl1B Pd1B Cl3B 92.5(6) . . ? N2B Pd1B Cl2B 95.4(8) . . ? Cl1B Pd1B Cl2B 171.4(10) . . ? Cl3B Pd1B Cl2B 83.2(5) . . ? N2B Pd1B Pd2B 127.9(6) . . ? Cl1B Pd1B Pd2B 125.9(7) . . ? Cl3B Pd1B Pd2B 46.6(3) . . ? Cl2B Pd1B Pd2B 46.4(3) . . ? Cl2B Pd2B Cl4B 94.0(6) . . ? Cl2B Pd2B Cl5B 175.4(9) . . ? Cl4B Pd2B Cl5B 85.7(5) . . ? Cl2B Pd2B Cl3B 84.9(5) . . ? Cl4B Pd2B Cl3B 177.6(9) . . ? Cl5B Pd2B Cl3B 95.3(5) . . ? Cl2B Pd2B Pd3B 129.4(7) . . ? Cl4B Pd2B Pd3B 48.4(3) . . ? Cl5B Pd2B Pd3B 47.7(3) . . ? Cl3B Pd2B Pd3B 131.2(6) . . ? Cl2B Pd2B Pd1B 47.7(3) . . ? Cl4B Pd2B Pd1B 130.5(7) . . ? Cl5B Pd2B Pd1B 129.9(6) . . ? Cl3B Pd2B Pd1B 47.3(3) . . ? Pd3B Pd2B Pd1B 127.4(4) . . ? N1B Pd3B Cl6B 89.7(8) . . ? N1B Pd3B Cl5B 174.3(8) . . ? Cl6B Pd3B Cl5B 92.8(6) . . ? N1B Pd3B Cl4B 94.0(8) . . ? Cl6B Pd3B Cl4B 175.1(8) . . ? Cl5B Pd3B Cl4B 83.3(5) . . ? N1B Pd3B Pd2B 128.3(6) . . ? Cl6B Pd3B Pd2B 128.6(7) . . ? Cl5B Pd3B Pd2B 46.7(3) . . ? Cl4B Pd3B Pd2B 46.5(2) . . ? Pd2B Cl2B Pd1B 86.0(4) . . ? Pd2B Cl3B Pd1B 86.0(4) . . ? Pd2B Cl4B Pd3B 85.1(4) . . ? Pd2B Cl5B Pd3B 85.6(4) . . ? C24B N1B C25B 124.6 . . ? C24B N1B Pd3B 118.2(6) . . ? C25B N1B Pd3B 116.7(5) . . ? C13B N2B C6' 119.4 . . ? C13B N2B Pd1B 121.8(5) . . ? C6' N2B Pd1B 118.8(5) . . ? C2B C1B C6' 114.9 . . ? C2B C1B C10B 121.1 . . ? C6' C1B C10B 123.6 . . ? C3' C2B C1B 125.2 . . ? C3' C2B H2' 117.4 . . ? C1B C2B H2' 117.4 . . ? C2B C3' C4' 117.3 . . ? C2B C3' H3' 121.3 . . ? C4' C3' H3' 121.3 . . ? C3' C4' C5' 123.2 . . ? C3' C4' H4' 118.4 . . ? C5' C4' H4' 118.4 . . ? C6' C5' C4' 116.7 . . ? C6' C5' C7' 125.3 . . ? C4' C5' C7' 117.9 . . ? C5' C6' C1B 122.1 . . ? C5' C6' N2B 119.9 . . ? C1B C6' N2B 118.0 . . ? C5' C7' C8' 114.0 . . ? C5' C7' C9' 117.5 . . ? C8' C7' C9' 107.7 . . ? C5' C7' H7' 105.5 . . ? C8' C7' H7' 105.5 . . ? C9' C7' H7' 105.5 . . ? C7' C8' H8'1 109.5 . . ? C7' C8' H8'2 109.5 . . ? H8'1 C8' H8'2 109.5 . . ? C7' C8' H8'3 109.5 . . ? H8'1 C8' H8'3 109.5 . . ? H8'2 C8' H8'3 109.5 . . ? C7' C9' H9'1 109.5 . . ? C7' C9' H9'2 109.5 . . ? H9'1 C9' H9'2 109.5 . . ? C7' C9' H9'3 109.5 . . ? H9'1 C9' H9'3 109.5 . . ? H9'2 C9' H9'3 109.5 . . ? C1B C10B C12B 105.2 . . ? C1B C10B C11B 115.3 . . ? C12B C10B C11B 118.5 . . ? C1B C10B H10' 105.6 . . ? C12B C10B H10' 105.6 . . ? C11B C10B H10' 105.6 . . ? C10B C11B H11D 109.5 . . ? C10B C11B H11E 109.5 . . ? H11D C11B H11E 109.5 . . ? C10B C11B H11F 109.5 . . ? H11D C11B H11F 109.5 . . ? H11E C11B H11F 109.5 . . ? C10B C12B H12D 109.5 . . ? C10B C12B H12E 109.5 . . ? H12D C12B H12E 109.5 . . ? C10B C12B H12F 109.5 . . ? H12D C12B H12F 109.5 . . ? H12E C12B H12F 109.5 . . ? N2B C13B C14B 124.0 . . ? N2B C13B H13C 106.3 . . ? C14B C13B H13C 106.3 . . ? N2B C13B H13D 106.3 . . ? C14B C13B H13D 106.3 . . ? H13C C13B H13D 106.4 . . ? C19B C14B C15B 125.0 . . ? C19B C14B C13B 118.2 . . ? C15B C14B C13B 116.7 . . ? C16B C15B C14B 115.5 . . ? C16B C15B C20B 120.9 . . ? C14B C15B C20B 123.5 . . ? C17B C16B C15B 119.8 . . ? C17B C16B C21B 121.2 . . ? C15B C16B C21B 118.8 . . ? C16B C17B C18B 123.3 . . ? C16B C17B C24B 121.6 . . ? C18B C17B C24B 114.9 . . ? C19B C18B C17B 117.9 . . ? C19B C18B C22B 121.2 . . ? C17B C18B C22B 120.8 . . ? C18B C19B C14B 118.2 . . ? C18B C19B C23B 123.0 . . ? C14B C19B C23B 118.3 . . ? C15B C20B H20D 109.5 . . ? C15B C20B H20E 109.5 . . ? H20D C20B H20E 109.5 . . ? C15B C20B H20F 109.5 . . ? H20D C20B H20F 109.5 . . ? H20E C20B H20F 109.5 . . ? C16B C21B H21D 109.5 . . ? C16B C21B H21E 109.5 . . ? H21D C21B H21E 109.5 . . ? C16B C21B H21F 109.5 . . ? H21D C21B H21F 109.5 . . ? H21E C21B H21F 109.5 . . ? C18B C22B H22D 109.5 . . ? C18B C22B H22E 109.5 . . ? H22D C22B H22E 109.5 . . ? C18B C22B H22F 109.5 . . ? H22D C22B H22F 109.5 . . ? H22E C22B H22F 109.5 . . ? C19B C23B H23D 109.5 . . ? C19B C23B H23E 109.5 . . ? H23D C23B H23E 109.5 . . ? C19B C23B H23F 109.5 . . ? H23D C23B H23F 109.5 . . ? H23E C23B H23F 109.5 . . ? N1B C24B C17B 125.1 . . ? N1B C24B H24C 106.0 . . ? C17B C24B H24C 106.0 . . ? N1B C24B H24D 106.0 . . ? C17B C24B H24D 106.0 . . ? H24C C24B H24D 106.3 . . ? C30B C25B C26B 118.7 . . ? C30B C25B N1B 119.4 . . ? C26B C25B N1B 121.4 . . ? C27B C26B C25B 117.7 . . ? C27B C26B C34B 119.5 . . ? C25B C26B C34B 122.8 . . ? C26B C27B C28B 122.8 . . ? C26B C27B H27' 118.6 . . ? C28B C27B H27' 118.6 . . ? C27B C28B C29B 119.3 . . ? C27B C28B H28' 120.4 . . ? C29B C28B H28' 120.4 . . ? C30B C29B C28B 116.0 . . ? C30B C29B H29' 122.0 . . ? C28B C29B H29' 122.0 . . ? C25B C30B C29B 124.2 . . ? C25B C30B C31B 122.4 . . ? C29B C30B C31B 113.4 . . ? C33B C31B C32B 111.8 . . ? C33B C31B C30B 114.1 . . ? C32B C31B C30B 107.9 . . ? C33B C31B H31' 107.6 . . ? C32B C31B H31' 107.6 . . ? C30B C31B H31' 107.6 . . ? C31B C32B H32D 109.5 . . ? C31B C32B H32E 109.5 . . ? H32D C32B H32E 109.5 . . ? C31B C32B H32F 109.5 . . ? H32D C32B H32F 109.5 . . ? H32E C32B H32F 109.5 . . ? C31B C33B H33D 109.5 . . ? C31B C33B H33E 109.5 . . ? H33D C33B H33E 109.5 . . ? C31B C33B H33F 109.5 . . ? H33D C33B H33F 109.5 . . ? H33E C33B H33F 109.5 . . ? C26B C34B C36B 111.9 . . ? C26B C34B C35B 114.0 . . ? C36B C34B C35B 109.5 . . ? C26B C34B H34' 107.0 . . ? C36B C34B H34' 107.0 . . ? C35B C34B H34' 107.0 . . ? C34B C35B H35D 109.5 . . ? C34B C35B H35E 109.5 . . ? H35D C35B H35E 109.5 . . ? C34B C35B H35F 109.5 . . ? H35D C35B H35F 109.5 . . ? H35E C35B H35F 109.5 . . ? C34B C36B H36D 109.5 . . ? C34B C36B H36E 109.5 . . ? H36D C36B H36E 109.5 . . ? C34B C36B H36F 109.5 . . ? H36D C36B H36F 109.5 . . ? H36E C36B H36F 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 N2 Pd1 Pd2 Cl4 -5.4(8) . . . . ? Cl1 Pd1 Pd2 Cl4 -138.0(3) . . . . ? Cl3 Pd1 Pd2 Cl4 179.8(3) . . . . ? Cl2 Pd1 Pd2 Cl4 49.0(3) . . . . ? N2 Pd1 Pd2 Cl5 121.4(8) . . . . ? Cl1 Pd1 Pd2 Cl5 -11.1(3) . . . . ? Cl3 Pd1 Pd2 Cl5 -53.4(3) . . . . ? Cl2 Pd1 Pd2 Cl5 175.8(3) . . . . ? N2 Pd1 Pd2 Cl2 -54.4(8) . . . . ? Cl1 Pd1 Pd2 Cl2 173.1(3) . . . . ? Cl3 Pd1 Pd2 Cl2 130.8(3) . . . . ? N2 Pd1 Pd2 Cl3 174.8(8) . . . . ? Cl1 Pd1 Pd2 Cl3 42.2(3) . . . . ? Cl2 Pd1 Pd2 Cl3 -130.8(3) . . . . ? N2 Pd1 Pd2 Pd3 58.2(8) . . . . ? Cl1 Pd1 Pd2 Pd3 -74.4(2) . . . . ? Cl3 Pd1 Pd2 Pd3 -116.6(2) . . . . ? Cl2 Pd1 Pd2 Pd3 112.58(19) . . . . ? Cl4 Pd2 Pd3 N1 54.3(7) . . . . ? Cl5 Pd2 Pd3 N1 -173.9(7) . . . . ? Cl2 Pd2 Pd3 N1 3.0(7) . . . . ? Cl3 Pd2 Pd3 N1 -122.8(7) . . . . ? Pd1 Pd2 Pd3 N1 -59.4(6) . . . . ? Cl4 Pd2 Pd3 Cl6 -173.0(3) . . . . ? Cl5 Pd2 Pd3 Cl6 -41.3(3) . . . . ? Cl2 Pd2 Pd3 Cl6 135.6(3) . . . . ? Cl3 Pd2 Pd3 Cl6 9.8(3) . . . . ? Pd1 Pd2 Pd3 Cl6 73.2(2) . . . . ? Cl4 Pd2 Pd3 Cl5 -131.8(3) . . . . ? Cl2 Pd2 Pd3 Cl5 176.9(3) . . . . ? Cl3 Pd2 Pd3 Cl5 51.0(3) . . . . ? Pd1 Pd2 Pd3 Cl5 114.4(2) . . . . ? Cl5 Pd2 Pd3 Cl4 131.8(3) . . . . ? Cl2 Pd2 Pd3 Cl4 -51.3(3) . . . . ? Cl3 Pd2 Pd3 Cl4 -177.2(3) . . . . ? Pd1 Pd2 Pd3 Cl4 -113.8(2) . . . . ? Cl4 Pd2 Cl2 Pd1 -144.7(2) . . . . ? Cl5 Pd2 Cl2 Pd1 -67(3) . . . . ? Cl3 Pd2 Cl2 Pd1 34.1(2) . . . . ? Pd3 Pd2 Cl2 Pd1 -108.93(15) . . . . ? N2 Pd1 Cl2 Pd2 140.6(4) . . . . ? Cl1 Pd1 Cl2 Pd2 -65.0(18) . . . . ? Cl3 Pd1 Cl2 Pd2 -33.69(18) . . . . ? Cl4 Pd2 Cl3 Pd1 -4(6) . . . . ? Cl5 Pd2 Cl3 Pd1 142.3(2) . . . . ? Cl2 Pd2 Cl3 Pd1 -34.3(2) . . . . ? Pd3 Pd2 Cl3 Pd1 106.85(17) . . . . ? N2 Pd1 Cl3 Pd2 -44(6) . . . . ? Cl1 Pd1 Cl3 Pd2 -149.4(2) . . . . ? Cl2 Pd1 Cl3 Pd2 33.65(19) . . . . ? Cl5 Pd2 Cl4 Pd3 -33.7(2) . . . . ? Cl2 Pd2 Cl4 Pd3 142.9(2) . . . . ? Cl3 Pd2 Cl4 Pd3 113(6) . . . . ? Pd1 Pd2 Cl4 Pd3 108.87(16) . . . . ? N1 Pd3 Cl4 Pd2 -140.0(4) . . . . ? Cl6 Pd3 Cl4 Pd2 67.3(19) . . . . ? Cl5 Pd3 Cl4 Pd2 33.12(17) . . . . ? Cl4 Pd2 Cl5 Pd3 34.0(2) . . . . ? Cl2 Pd2 Cl5 Pd3 -44(3) . . . . ? Cl3 Pd2 Cl5 Pd3 -144.7(2) . . . . ? Pd1 Pd2 Cl5 Pd3 -108.17(15) . . . . ? N1 Pd3 Cl5 Pd2 43(5) . . . . ? Cl6 Pd3 Cl5 Pd2 150.1(2) . . . . ? Cl4 Pd3 Cl5 Pd2 -33.08(19) . . . . ? Cl6 Pd3 N1 C24 -120.1(18) . . . . ? Cl5 Pd3 N1 C24 -13(6) . . . . ? Cl4 Pd3 N1 C24 62.5(18) . . . . ? Pd2 Pd3 N1 C24 26(2) . . . . ? Cl6 Pd3 N1 C25 60.1(11) . . . . ? Cl5 Pd3 N1 C25 167(4) . . . . ? Cl4 Pd3 N1 C25 -117.3(11) . . . . ? Pd2 Pd3 N1 C25 -153.6(8) . . . . ? Cl1 Pd1 N2 C13 126.2(18) . . . . ? Cl3 Pd1 N2 C13 21(8) . . . . ? Cl2 Pd1 N2 C13 -56.3(19) . . . . ? Pd2 Pd1 N2 C13 -20(2) . . . . ? Cl1 Pd1 N2 C6 -62.2(13) . . . . ? Cl3 Pd1 N2 C6 -168(5) . . . . ? Cl2 Pd1 N2 C6 115.3(13) . . . . ? Pd2 Pd1 N2 C6 151.8(9) . . . . ? C6 C1 C2 C3 2(3) . . . . ? C10 C1 C2 C3 180(2) . . . . ? C1 C2 C3 C4 2(4) . . . . ? C2 C3 C4 C5 -3(4) . . . . ? C3 C4 C5 C6 -1(3) . . . . ? C3 C4 C5 C7 179.0(19) . . . . ? C4 C5 C6 C1 5(3) . . . . ? C7 C5 C6 C1 -174.7(15) . . . . ? C4 C5 C6 N2 -176.5(15) . . . . ? C7 C5 C6 N2 4(2) . . . . ? C2 C1 C6 C5 -5(3) . . . . ? C10 C1 C6 C5 176.6(15) . . . . ? C2 C1 C6 N2 176.1(15) . . . . ? C10 C1 C6 N2 -2(2) . . . . ? C13 N2 C6 C5 -79(2) . . . . ? Pd1 N2 C6 C5 109.2(16) . . . . ? C13 N2 C6 C1 100(2) . . . . ? Pd1 N2 C6 C1 -72.2(19) . . . . ? C6 C5 C7 C8 109.2(18) . . . . ? C4 C5 C7 C8 -70.4(19) . . . . ? C6 C5 C7 C9 -127.4(18) . . . . ? C4 C5 C7 C9 53(2) . . . . ? C2 C1 C10 C12 66.5(19) . . . . ? C6 C1 C10 C12 -115.6(19) . . . . ? C2 C1 C10 C11 -62(2) . . . . ? C6 C1 C10 C11 116(2) . . . . ? C6 N2 C13 C14 -176.1(14) . . . . ? Pd1 N2 C13 C14 -4(3) . . . . ? N2 C13 C14 C19 115(2) . . . . ? N2 C13 C14 C15 -71(3) . . . . ? C19 C14 C15 C16 -6(3) . . . . ? C13 C14 C15 C16 180.0(15) . . . . ? C19 C14 C15 C20 175(2) . . . . ? C13 C14 C15 C20 1(3) . . . . ? C14 C15 C16 C17 3(2) . . . . ? C20 C15 C16 C17 -177.9(18) . . . . ? C14 C15 C16 C21 179.3(17) . . . . ? C20 C15 C16 C21 -2(2) . . . . ? C15 C16 C17 C18 1(3) . . . . ? C21 C16 C17 C18 -175.4(19) . . . . ? C15 C16 C17 C24 177.1(15) . . . . ? C21 C16 C17 C24 1(3) . . . . ? C16 C17 C18 C19 -2(3) . . . . ? C24 C17 C18 C19 -178.8(17) . . . . ? C16 C17 C18 C22 175.3(19) . . . . ? C24 C17 C18 C22 -1(3) . . . . ? C17 C18 C19 C14 0(3) . . . . ? C22 C18 C19 C14 -178(2) . . . . ? C17 C18 C19 C23 -179(2) . . . . ? C22 C18 C19 C23 4(3) . . . . ? C15 C14 C19 C18 5(3) . . . . ? C13 C14 C19 C18 178.6(17) . . . . ? C15 C14 C19 C23 -177(2) . . . . ? C13 C14 C19 C23 -3(3) . . . . ? C25 N1 C24 C17 179.5(13) . . . . ? Pd3 N1 C24 C17 0(3) . . . . ? C16 C17 C24 N1 73(3) . . . . ? C18 C17 C24 N1 -110(2) . . . . ? C24 N1 C25 C30 -108(2) . . . . ? Pd3 N1 C25 C30 71.8(19) . . . . ? C24 N1 C25 C26 72(2) . . . . ? Pd3 N1 C25 C26 -108.5(16) . . . . ? C30 C25 C26 C27 -8(3) . . . . ? N1 C25 C26 C27 172.6(15) . . . . ? C30 C25 C26 C34 174.4(15) . . . . ? N1 C25 C26 C34 -5(2) . . . . ? C25 C26 C27 C28 3(3) . . . . ? C34 C26 C27 C28 -179.5(19) . . . . ? C26 C27 C28 C29 2(3) . . . . ? C27 C28 C29 C30 -1(3) . . . . ? C26 C25 C30 C29 9(3) . . . . ? N1 C25 C30 C29 -171.4(16) . . . . ? C26 C25 C30 C31 -172.3(14) . . . . ? N1 C25 C30 C31 7(2) . . . . ? C28 C29 C30 C25 -4(3) . . . . ? C28 C29 C30 C31 176.7(17) . . . . ? C25 C30 C31 C33 -122.5(19) . . . . ? C29 C30 C31 C33 56(2) . . . . ? C25 C30 C31 C32 112(2) . . . . ? C29 C30 C31 C32 -69.5(18) . . . . ? C27 C26 C34 C36 72.7(18) . . . . ? C25 C26 C34 C36 -109.5(18) . . . . ? C27 C26 C34 C35 -50(2) . . . . ? C25 C26 C34 C35 128.1(19) . . . . ? N2B Pd1B Pd2B Cl2B -54.8(14) . . . . ? Cl1B Pd1B Pd2B Cl2B -175.1(14) . . . . ? Cl3B Pd1B Pd2B Cl2B 132.4(11) . . . . ? N2B Pd1B Pd2B Cl4B -5.6(14) . . . . ? Cl1B Pd1B Pd2B Cl4B -126.0(13) . . . . ? Cl3B Pd1B Pd2B Cl4B -178.4(11) . . . . ? Cl2B Pd1B Pd2B Cl4B 49.1(11) . . . . ? N2B Pd1B Pd2B Cl5B 120.1(13) . . . . ? Cl1B Pd1B Pd2B Cl5B -0.3(14) . . . . ? Cl3B Pd1B Pd2B Cl5B -52.7(10) . . . . ? Cl2B Pd1B Pd2B Cl5B 174.9(11) . . . . ? N2B Pd1B Pd2B Cl3B 172.8(14) . . . . ? Cl1B Pd1B Pd2B Cl3B 52.4(13) . . . . ? Cl2B Pd1B Pd2B Cl3B -132.4(11) . . . . ? N2B Pd1B Pd2B Pd3B 57.9(13) . . . . ? Cl1B Pd1B Pd2B Pd3B -62.5(13) . . . . ? Cl3B Pd1B Pd2B Pd3B -115.0(9) . . . . ? Cl2B Pd1B Pd2B Pd3B 112.6(9) . . . . ? Cl2B Pd2B Pd3B N1B -1.3(14) . . . . ? Cl4B Pd2B Pd3B N1B 51.2(13) . . . . ? Cl5B Pd2B Pd3B N1B -176.5(14) . . . . ? Cl3B Pd2B Pd3B N1B -125.6(13) . . . . ? Pd1B Pd2B Pd3B N1B -63.3(12) . . . . ? Cl2B Pd2B Pd3B Cl6B 127.1(14) . . . . ? Cl4B Pd2B Pd3B Cl6B 179.6(15) . . . . ? Cl5B Pd2B Pd3B Cl6B -48.1(14) . . . . ? Cl3B Pd2B Pd3B Cl6B 2.8(15) . . . . ? Pd1B Pd2B Pd3B Cl6B 65.1(14) . . . . ? Cl2B Pd2B Pd3B Cl5B 175.3(11) . . . . ? Cl4B Pd2B Pd3B Cl5B -132.2(11) . . . . ? Cl3B Pd2B Pd3B Cl5B 50.9(10) . . . . ? Pd1B Pd2B Pd3B Cl5B 113.2(9) . . . . ? Cl2B Pd2B Pd3B Cl4B -52.5(10) . . . . ? Cl5B Pd2B Pd3B Cl4B 132.2(11) . . . . ? Cl3B Pd2B Pd3B Cl4B -176.8(11) . . . . ? Pd1B Pd2B Pd3B Cl4B -114.5(9) . . . . ? Cl4B Pd2B Cl2B Pd1B -144.8(9) . . . . ? Cl5B Pd2B Cl2B Pd1B -59(8) . . . . ? Cl3B Pd2B Cl2B Pd1B 33.0(7) . . . . ? Pd3B Pd2B Cl2B Pd1B -108.4(6) . . . . ? N2B Pd1B Cl2B Pd2B 139.6(10) . . . . ? Cl1B Pd1B Cl2B Pd2B 27(7) . . . . ? Cl3B Pd1B Cl2B Pd2B -32.7(7) . . . . ? Cl2B Pd2B Cl3B Pd1B -33.2(7) . . . . ? Cl4B Pd2B Cl3B Pd1B 30(16) . . . . ? Cl5B Pd2B Cl3B Pd1B 142.2(9) . . . . ? Pd3B Pd2B Cl3B Pd1B 107.0(7) . . . . ? N2B Pd1B Cl3B Pd2B -47(7) . . . . ? Cl1B Pd1B Cl3B Pd2B -140.0(11) . . . . ? Cl2B Pd1B Cl3B Pd2B 32.5(7) . . . . ? Cl2B Pd2B Cl4B Pd3B 142.1(9) . . . . ? Cl5B Pd2B Cl4B Pd3B -33.3(7) . . . . ? Cl3B Pd2B Cl4B Pd3B 80(16) . . . . ? Pd1B Pd2B Cl4B Pd3B 108.0(7) . . . . ? N1B Pd3B Cl4B Pd2B -142.1(9) . . . . ? Cl6B Pd3B Cl4B Pd2B -3(14) . . . . ? Cl5B Pd3B Cl4B Pd2B 32.9(7) . . . . ? Cl2B Pd2B Cl5B Pd3B -53(8) . . . . ? Cl4B Pd2B Cl5B Pd3B 33.7(7) . . . . ? Cl3B Pd2B Cl5B Pd3B -144.1(8) . . . . ? Pd1B Pd2B Cl5B Pd3B -108.1(6) . . . . ? N1B Pd3B Cl5B Pd2B 29(10) . . . . ? Cl6B Pd3B Cl5B Pd2B 144.4(11) . . . . ? Cl4B Pd3B Cl5B Pd2B -32.7(7) . . . . ? Cl6B Pd3B N1B C24B -109.2(17) . . . . ? Cl5B Pd3B N1B C24B 7(11) . . . . ? Cl4B Pd3B N1B C24B 67.6(16) . . . . ? Pd2B Pd3B N1B C24B 33.0(19) . . . . ? Cl6B Pd3B N1B C25B 63.5(11) . . . . ? Cl5B Pd3B N1B C25B 179(100) . . . . ? Cl4B Pd3B N1B C25B -119.7(6) . . . . ? Pd2B Pd3B N1B C25B -154.3(7) . . . . ? Cl1B Pd1B N2B C13B 111.6(18) . . . . ? Cl3B Pd1B N2B C13B 18(8) . . . . ? Cl2B Pd1B N2B C13B -60.5(17) . . . . ? Pd2B Pd1B N2B C13B -24(2) . . . . ? Cl1B Pd1B N2B C6' -70.2(11) . . . . ? Cl3B Pd1B N2B C6' -163(7) . . . . ? Cl2B Pd1B N2B C6' 117.7(6) . . . . ? Pd2B Pd1B N2B C6' 154.2(7) . . . . ? C6' C1B C2B C3' -1.3 . . . . ? C10B C1B C2B C3' 172.3 . . . . ? C1B C2B C3' C4' 7.0 . . . . ? C2B C3' C4' C5' -8.5 . . . . ? C3' C4' C5' C6' 4.2 . . . . ? C3' C4' C5' C7' -180.0 . . . . ? C4' C5' C6' C1B 1.9 . . . . ? C7' C5' C6' C1B -173.5 . . . . ? C4' C5' C6' N2B -177.7 . . . . ? C7' C5' C6' N2B 6.8 . . . . ? C2B C1B C6' C5' -3.3 . . . . ? C10B C1B C6' C5' -176.7 . . . . ? C2B C1B C6' N2B 176.3 . . . . ? C10B C1B C6' N2B 3.0 . . . . ? C13B N2B C6' C5' -78.1 . . . . ? Pd1B N2B C6' C5' 103.7(17) . . . . ? C13B N2B C6' C1B 102.3 . . . . ? Pd1B N2B C6' C1B -76.0(17) . . . . ? C6' C5' C7' C8' 104.3 . . . . ? C4' C5' C7' C8' -71.1 . . . . ? C6' C5' C7' C9' -128.2 . . . . ? C4' C5' C7' C9' 56.4 . . . . ? C2B C1B C10B C12B 69.4 . . . . ? C6' C1B C10B C12B -117.6 . . . . ? C2B C1B C10B C11B -63.1 . . . . ? C6' C1B C10B C11B 109.9 . . . . ? C6' N2B C13B C14B -176.1 . . . . ? Pd1B N2B C13B C14B 2.1(18) . . . . ? N2B C13B C14B C19B 110.1 . . . . ? N2B C13B C14B C15B -72.3 . . . . ? C19B C14B C15B C16B -0.5 . . . . ? C13B C14B C15B C16B -177.9 . . . . ? C19B C14B C15B C20B 177.1 . . . . ? C13B C14B C15B C20B -0.3 . . . . ? C14B C15B C16B C17B 0.4 . . . . ? C20B C15B C16B C17B -177.3 . . . . ? C14B C15B C16B C21B 176.0 . . . . ? C20B C15B C16B C21B -1.6 . . . . ? C15B C16B C17B C18B 2.7 . . . . ? C21B C16B C17B C18B -172.8 . . . . ? C15B C16B C17B C24B 176.4 . . . . ? C21B C16B C17B C24B 0.9 . . . . ? C16B C17B C18B C19B -5.7 . . . . ? C24B C17B C18B C19B -179.8 . . . . ? C16B C17B C18B C22B 175.7 . . . . ? C24B C17B C18B C22B 1.6 . . . . ? C17B C18B C19B C14B 5.3 . . . . ? C22B C18B C19B C14B -176.1 . . . . ? C17B C18B C19B C23B -166.7 . . . . ? C22B C18B C19B C23B 11.8 . . . . ? C15B C14B C19B C18B -2.5 . . . . ? C13B C14B C19B C18B 174.9 . . . . ? C15B C14B C19B C23B 169.9 . . . . ? C13B C14B C19B C23B -12.7 . . . . ? C25B N1B C24B C17B -177.3 . . . . ? Pd3B N1B C24B C17B -5.2(17) . . . . ? C16B C17B C24B N1B 73.6 . . . . ? C18B C17B C24B N1B -112.2 . . . . ? C24B N1B C25B C30B -105.7 . . . . ? Pd3B N1B C25B C30B 82.1(17) . . . . ? C24B N1B C25B C26B 65.8 . . . . ? Pd3B N1B C25B C26B -106.4(17) . . . . ? C30B C25B C26B C27B -9.7 . . . . ? N1B C25B C26B C27B 178.8 . . . . ? C30B C25B C26B C34B 171.5 . . . . ? N1B C25B C26B C34B 0.0 . . . . ? C25B C26B C27B C28B 0.3 . . . . ? C34B C26B C27B C28B 179.1 . . . . ? C26B C27B C28B C29B 8.6 . . . . ? C27B C28B C29B C30B -7.9 . . . . ? C26B C25B C30B C29B 10.5 . . . . ? N1B C25B C30B C29B -177.8 . . . . ? C26B C25B C30B C31B -172.2 . . . . ? N1B C25B C30B C31B -0.5 . . . . ? C28B C29B C30B C25B -1.6 . . . . ? C28B C29B C30B C31B -179.1 . . . . ? C25B C30B C31B C33B -118.8 . . . . ? C29B C30B C31B C33B 58.7 . . . . ? C25B C30B C31B C32B 116.3 . . . . ? C29B C30B C31B C32B -66.1 . . . . ? C27B C26B C34B C36B 71.9 . . . . ? C25B C26B C34B C36B -109.3 . . . . ? C27B C26B C34B C35B -53.1 . . . . ? C25B C26B C34B C35B 125.6 . . . . ? _diffrn_measured_fraction_theta_max 0.662 _diffrn_reflns_theta_full 26.73 _diffrn_measured_fraction_theta_full 0.662 _refine_diff_density_max 0.955 _refine_diff_density_min -0.606 _refine_diff_density_rms 0.134 data_jl1003 _database_code_depnum_ccdc_archive 'CCDC 824571' #TrackingRef 'jl1003.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H32 Cl6 N2 Pd3, 2(C H Cl3)' _chemical_formula_sum 'C22 H34 Cl12 N2 Pd3' _chemical_formula_weight 1071.11 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd 0.1215 3.9337 '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 1 21/n 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 14.0862(4) _cell_length_b 12.8822(3) _cell_length_c 20.1228(4) _cell_angle_alpha 90.00 _cell_angle_beta 96.349(2) _cell_angle_gamma 90.00 _cell_volume 3629.11(15) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 12916 _cell_measurement_theta_min 2.2073 _cell_measurement_theta_max 70.6373 _exptl_crystal_description needle _exptl_crystal_colour brown _exptl_crystal_size_max 0.0173208 _exptl_crystal_size_mid 0.0141317 _exptl_crystal_size_min 0.0084144 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.960 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2088 _exptl_absorpt_coefficient_mu 20.151 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.47788 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.34.46 (release 25-11-2010 CrysAlis171 .NET) (compiled Nov 25 2010,17:55:46) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 1.54180 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'SuperNova (Cu) X-ray Source' _diffrn_radiation_monochromator mirror _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Atlas' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 5.1574 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 33867 _diffrn_reflns_av_R_equivalents 0.0648 _diffrn_reflns_av_sigmaI/netI 0.0401 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.65 _diffrn_reflns_theta_max 70.77 _reflns_number_total 6914 _reflns_number_gt 5952 _reflns_threshold_expression >2\s(I) _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.34.46 (release 25-11-2010 CrysAlis171 .NET) (compiled Nov 25 2010,17:55:46) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.34.46 (release 25-11-2010 CrysAlis171 .NET) (compiled Nov 25 2010,17:55:46) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.34.46 (release 25-11-2010 CrysAlis171 .NET) (compiled Nov 25 2010,17:55:46) ; _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; C1, C2 and C3 of a tertiarybutyl group were disordered and were modelled over two sites with 64:36 occupancy. 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^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0700P)^2^+5.3825P] 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_number_reflns 6914 _refine_ls_number_parameters 387 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0518 _refine_ls_R_factor_gt 0.0433 _refine_ls_wR_factor_ref 0.1203 _refine_ls_wR_factor_gt 0.1134 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.052 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.71199(3) -0.09766(3) 0.163568(17) 0.02682(11) Uani 1 1 d . . . Pd2 Pd 0.53383(3) -0.23661(3) 0.116524(17) 0.02818(12) Uani 1 1 d . . . Pd3 Pd 0.35897(3) -0.24839(3) 0.192340(18) 0.02724(11) Uani 1 1 d . . . Cl1 Cl 0.82063(12) -0.11760(11) 0.25579(7) 0.0433(3) Uani 1 1 d . . . Cl2 Cl 0.59726(11) -0.09266(9) 0.07011(6) 0.0330(3) Uani 1 1 d . . . Cl3 Cl 0.68786(11) -0.27701(9) 0.15673(7) 0.0349(3) Uani 1 1 d . . . Cl4 Cl 0.37654(10) -0.19256(10) 0.08319(6) 0.0338(3) Uani 1 1 d . . . Cl5 Cl 0.47136(11) -0.37400(9) 0.17005(6) 0.0347(3) Uani 1 1 d . . . Cl6 Cl 0.35365(11) -0.30887(9) 0.29835(6) 0.0344(3) Uani 1 1 d . . . N1 N 0.7272(3) 0.0586(3) 0.16552(19) 0.0258(9) Uani 1 1 d . A . N2 N 0.2640(3) -0.1367(3) 0.2071(2) 0.0280(9) Uani 1 1 d . . . C1A C 0.8877(15) 0.125(2) 0.1839(10) 0.056(7) Uani 0.341(13) 1 d P A 1 H1A1 H 0.8669 0.1713 0.2179 0.083 Uiso 0.341(13) 1 calc PR A 1 H1A2 H 0.9401 0.1570 0.1632 0.083 Uiso 0.341(13) 1 calc PR A 1 H1A3 H 0.9098 0.0590 0.2049 0.083 Uiso 0.341(13) 1 calc PR A 1 C2A C 0.7766(17) 0.2086(16) 0.0956(13) 0.057(7) Uani 0.341(13) 1 d P A 1 H2A1 H 0.7235 0.1924 0.0615 0.086 Uiso 0.341(13) 1 calc PR A 1 H2A2 H 0.8297 0.2377 0.0741 0.086 Uiso 0.341(13) 1 calc PR A 1 H2A3 H 0.7556 0.2593 0.1272 0.086 Uiso 0.341(13) 1 calc PR A 1 C3A C 0.833(3) 0.033(2) 0.0784(14) 0.082(12) Uani 0.341(13) 1 d P A 1 H3A1 H 0.7765 0.0252 0.0462 0.123 Uiso 0.341(13) 1 calc PR A 1 H3A2 H 0.8532 -0.0345 0.0970 0.123 Uiso 0.341(13) 1 calc PR A 1 H3A3 H 0.8853 0.0633 0.0559 0.123 Uiso 0.341(13) 1 calc PR A 1 C1B C 0.9010(7) 0.0379(8) 0.1534(5) 0.045(3) Uani 0.659(13) 1 d P A 2 H1B1 H 0.9183 0.0401 0.2019 0.068 Uiso 0.659(13) 1 calc PR A 2 H1B2 H 0.9540 0.0651 0.1308 0.068 Uiso 0.659(13) 1 calc PR A 2 H1B3 H 0.8878 -0.0339 0.1393 0.068 Uiso 0.659(13) 1 calc PR A 2 C2B C 0.8357(9) 0.2155(7) 0.1598(6) 0.052(3) Uani 0.659(13) 1 d P A 2 H2B1 H 0.8535 0.2139 0.2083 0.078 Uiso 0.659(13) 1 calc PR A 2 H2B2 H 0.7801 0.2608 0.1495 0.078 Uiso 0.659(13) 1 calc PR A 2 H2B3 H 0.8893 0.2421 0.1377 0.078 Uiso 0.659(13) 1 calc PR A 2 C3B C 0.7834(8) 0.1037(12) 0.0616(4) 0.052(3) Uani 0.659(13) 1 d P A 2 H3B1 H 0.7681 0.0324 0.0471 0.078 Uiso 0.659(13) 1 calc PR A 2 H3B2 H 0.8365 0.1296 0.0387 0.078 Uiso 0.659(13) 1 calc PR A 2 H3B3 H 0.7273 0.1480 0.0505 0.078 Uiso 0.659(13) 1 calc PR A 2 C4 C 0.8108(4) 0.1053(4) 0.1346(3) 0.0289(11) Uani 1 1 d . . . C5 C 0.6633(4) 0.1158(4) 0.1874(2) 0.0289(11) Uani 1 1 d . . . H5 H 0.6774 0.1873 0.1949 0.035 Uiso 1 1 calc R A . C6 C 0.5680(4) 0.0769(4) 0.2017(2) 0.0244(10) Uani 1 1 d . A . C7 C 0.5521(4) 0.0240(4) 0.2596(2) 0.0262(10) Uani 1 1 d . . . C8 C 0.4606(4) -0.0145(3) 0.2659(2) 0.0237(10) Uani 1 1 d . A . C9 C 0.3886(4) -0.0017(4) 0.2128(2) 0.0254(10) Uani 1 1 d . . . C10 C 0.4023(4) 0.0583(4) 0.1565(2) 0.0247(10) Uani 1 1 d . A . C11 C 0.4930(4) 0.0998(4) 0.1514(2) 0.0276(11) Uani 1 1 d . . . C12 C 0.6297(4) 0.0127(4) 0.3171(3) 0.0326(12) Uani 1 1 d . A . H12A H 0.6889 0.0436 0.3048 0.049 Uiso 1 1 calc R . . H12B H 0.6402 -0.0611 0.3272 0.049 Uiso 1 1 calc R . . H12C H 0.6104 0.0482 0.3565 0.049 Uiso 1 1 calc R . . C13 C 0.4397(4) -0.0619(4) 0.3310(2) 0.0307(11) Uani 1 1 d . . . H13A H 0.3724 -0.0825 0.3278 0.046 Uiso 1 1 calc R A . H13B H 0.4530 -0.0111 0.3671 0.046 Uiso 1 1 calc R . . H13C H 0.4802 -0.1232 0.3406 0.046 Uiso 1 1 calc R . . C14 C 0.3212(4) 0.0779(5) 0.1017(2) 0.0324(12) Uani 1 1 d . . . H14A H 0.2657 0.0360 0.1101 0.049 Uiso 1 1 calc R A . H14B H 0.3416 0.0587 0.0584 0.049 Uiso 1 1 calc R . . H14C H 0.3040 0.1516 0.1013 0.049 Uiso 1 1 calc R . . C15 C 0.5122(4) 0.1678(4) 0.0927(3) 0.0334(12) Uani 1 1 d . A . H15A H 0.5469 0.1276 0.0618 0.050 Uiso 1 1 calc R . . H15B H 0.5507 0.2278 0.1091 0.050 Uiso 1 1 calc R . . H15C H 0.4515 0.1918 0.0694 0.050 Uiso 1 1 calc R . . C16 C 0.2894(4) -0.0425(4) 0.2159(2) 0.0269(10) Uani 1 1 d . A . H16 H 0.2418 0.0059 0.2252 0.032 Uiso 1 1 calc R . . C17 C 0.1578(4) -0.1629(4) 0.2047(3) 0.0341(12) Uani 1 1 d . . . C18 C 0.1438(5) -0.2780(5) 0.1876(4) 0.0447(15) Uani 1 1 d . . . H18A H 0.1705 -0.2931 0.1457 0.067 Uiso 1 1 calc R . . H18B H 0.0755 -0.2945 0.1826 0.067 Uiso 1 1 calc R . . H18C H 0.1766 -0.3203 0.2237 0.067 Uiso 1 1 calc R . . C19 C 0.1254(6) -0.1416(7) 0.2731(4) 0.064(2) Uani 1 1 d . . . H19A H 0.1596 -0.1878 0.3063 0.096 Uiso 1 1 calc R . . H19B H 0.0566 -0.1542 0.2715 0.096 Uiso 1 1 calc R . . H19C H 0.1392 -0.0692 0.2857 0.096 Uiso 1 1 calc R . . C20 C 0.1041(6) -0.0994(5) 0.1490(5) 0.064(2) Uani 1 1 d . . . H20A H 0.1081 -0.0256 0.1608 0.096 Uiso 1 1 calc R . . H20B H 0.0370 -0.1209 0.1430 0.096 Uiso 1 1 calc R . . H20C H 0.1326 -0.1108 0.1073 0.096 Uiso 1 1 calc R . . Cl1A Cl 0.40282(16) 0.40746(15) 0.03274(10) 0.0638(5) Uani 1 1 d . . . Cl2A Cl 0.23896(19) 0.5344(2) 0.04943(16) 0.0906(8) Uani 1 1 d . . . Cl3A Cl 0.33320(17) 0.54712(16) -0.07188(10) 0.0710(6) Uani 1 1 d . . . C100 C 0.3482(5) 0.5279(5) 0.0150(3) 0.0488(16) Uani 1 1 d . . . H100 H 0.3912 0.5835 0.0358 0.059 Uiso 1 1 calc R . . Cl1B Cl 0.44102(16) 0.62081(18) 0.47692(10) 0.0688(5) Uani 1 1 d . . . Cl2B Cl 0.32815(18) 0.77053(17) 0.53709(12) 0.0737(6) Uani 1 1 d . . . Cl3B Cl 0.51376(18) 0.8290(2) 0.49941(10) 0.0787(7) Uani 1 1 d . . . C200 C 0.4110(6) 0.7524(6) 0.4788(3) 0.0496(17) Uani 1 1 d . . . H200 H 0.3805 0.7733 0.4336 0.059 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 0.0340(2) 0.02016(19) 0.02647(18) -0.00077(12) 0.00404(15) 0.00029(15) Pd2 0.0382(2) 0.02256(19) 0.02404(18) -0.00396(13) 0.00483(16) -0.00100(15) Pd3 0.0341(2) 0.02051(19) 0.02719(19) -0.00149(12) 0.00385(16) -0.00162(15) Cl1 0.0475(9) 0.0331(7) 0.0459(7) 0.0063(6) -0.0103(6) 0.0035(6) Cl2 0.0470(8) 0.0297(6) 0.0219(5) -0.0011(4) 0.0025(5) -0.0059(5) Cl3 0.0399(8) 0.0209(5) 0.0443(7) -0.0031(5) 0.0066(6) 0.0020(5) Cl4 0.0412(8) 0.0338(6) 0.0257(5) -0.0007(4) 0.0001(5) -0.0016(6) Cl5 0.0445(8) 0.0215(6) 0.0392(6) -0.0010(5) 0.0102(6) 0.0010(5) Cl6 0.0468(8) 0.0261(6) 0.0310(6) 0.0027(4) 0.0074(5) -0.0044(5) N1 0.031(2) 0.022(2) 0.0244(19) -0.0039(15) 0.0028(17) -0.0043(18) N2 0.033(3) 0.026(2) 0.0246(19) 0.0006(16) 0.0035(17) 0.0003(19) C1A 0.036(11) 0.085(17) 0.045(10) 0.016(10) -0.001(8) -0.026(11) C2A 0.055(14) 0.040(11) 0.082(16) 0.032(10) 0.027(12) 0.006(10) C3A 0.12(3) 0.069(17) 0.071(16) -0.024(14) 0.062(19) -0.050(19) C1B 0.035(5) 0.044(6) 0.058(6) 0.010(5) 0.007(4) 0.000(4) C2B 0.060(7) 0.028(5) 0.074(7) -0.008(4) 0.041(6) -0.011(5) C3B 0.041(6) 0.089(10) 0.024(4) 0.007(5) 0.003(4) -0.023(6) C4 0.030(3) 0.027(3) 0.029(2) -0.001(2) 0.003(2) -0.005(2) C5 0.037(3) 0.021(2) 0.029(2) -0.0004(19) 0.002(2) -0.002(2) C6 0.025(3) 0.022(2) 0.026(2) -0.0032(18) 0.0017(19) -0.001(2) C7 0.035(3) 0.018(2) 0.025(2) -0.0010(17) 0.000(2) 0.003(2) C8 0.035(3) 0.016(2) 0.019(2) 0.0003(16) -0.0001(19) 0.001(2) C9 0.033(3) 0.016(2) 0.027(2) -0.0034(18) 0.003(2) 0.002(2) C10 0.029(3) 0.022(2) 0.023(2) -0.0007(17) -0.0011(19) 0.004(2) C11 0.038(3) 0.022(2) 0.023(2) 0.0028(18) 0.005(2) -0.001(2) C12 0.036(3) 0.031(3) 0.029(2) 0.000(2) -0.003(2) 0.000(2) C13 0.035(3) 0.031(3) 0.027(2) 0.004(2) 0.004(2) 0.002(2) C14 0.033(3) 0.038(3) 0.025(2) 0.004(2) -0.003(2) -0.001(2) C15 0.033(3) 0.037(3) 0.029(2) 0.008(2) 0.000(2) 0.000(2) C16 0.033(3) 0.022(2) 0.026(2) 0.0023(18) 0.001(2) 0.004(2) C17 0.028(3) 0.029(3) 0.045(3) 0.000(2) 0.003(2) -0.003(2) C18 0.038(4) 0.030(3) 0.065(4) -0.002(3) 0.003(3) -0.014(3) C19 0.054(5) 0.064(5) 0.079(5) -0.022(4) 0.031(4) -0.014(4) C20 0.047(4) 0.038(4) 0.101(6) 0.020(4) -0.027(4) -0.015(3) Cl1A 0.0673(13) 0.0500(9) 0.0722(11) 0.0103(8) -0.0010(9) 0.0152(9) Cl2A 0.0632(14) 0.0856(16) 0.127(2) -0.0359(15) 0.0262(14) 0.0054(12) Cl3A 0.0823(15) 0.0675(12) 0.0550(10) 0.0041(9) -0.0292(10) -0.0006(11) C100 0.046(4) 0.042(3) 0.055(4) -0.007(3) -0.006(3) 0.005(3) Cl1B 0.0645(13) 0.0779(13) 0.0644(11) -0.0184(10) 0.0086(9) 0.0158(11) Cl2B 0.0763(15) 0.0642(12) 0.0875(14) -0.0101(10) 0.0400(12) 0.0083(11) Cl3B 0.0799(16) 0.1037(17) 0.0501(9) 0.0105(10) -0.0029(9) -0.0364(14) C200 0.048(4) 0.065(4) 0.035(3) 0.007(3) 0.006(3) 0.001(3) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 N1 2.025(4) . ? Pd1 Cl1 2.2856(14) . ? Pd1 Cl3 2.3371(13) . ? Pd1 Cl2 2.3411(13) . ? Pd1 Pd2 3.1421(6) . ? Pd2 Cl3 2.2901(15) . ? Pd2 Cl5 2.2970(13) . ? Pd2 Cl2 2.3010(13) . ? Pd2 Cl4 2.3134(15) . ? Pd2 Pd3 3.0412(6) . ? Pd3 N2 2.009(5) . ? Pd3 Cl6 2.2801(12) . ? Pd3 Cl5 2.3417(14) . ? Pd3 Cl4 2.3502(12) . ? N1 C5 1.277(7) . ? N1 C4 1.516(7) . ? N2 C16 1.272(7) . ? N2 C17 1.529(7) . ? C1A C4 1.41(2) . ? C1A H1A1 0.9800 . ? C1A H1A2 0.9800 . ? C1A H1A3 0.9800 . ? C2A C4 1.593(19) . ? C2A H2A1 0.9800 . ? C2A H2A2 0.9800 . ? C2A H2A3 0.9800 . ? C3A C4 1.52(2) . ? C3A H3A1 0.9800 . ? C3A H3A2 0.9800 . ? C3A H3A3 0.9800 . ? C1B C4 1.550(11) . ? C1B H1B1 0.9800 . ? C1B H1B2 0.9800 . ? C1B H1B3 0.9800 . ? C2B C4 1.535(10) . ? C2B H2B1 0.9800 . ? C2B H2B2 0.9800 . ? C2B H2B3 0.9800 . ? C3B C4 1.479(10) . ? C3B H3B1 0.9800 . ? C3B H3B2 0.9800 . ? C3B H3B3 0.9800 . ? C5 C6 1.491(8) . ? C5 H5 0.9500 . ? C6 C7 1.390(7) . ? C6 C11 1.413(7) . ? C7 C8 1.400(8) . ? C7 C12 1.507(7) . ? C8 C9 1.398(7) . ? C8 C13 1.505(6) . ? C9 C10 1.402(7) . ? C9 C16 1.500(8) . ? C10 C11 1.400(8) . ? C10 C14 1.518(7) . ? C11 C15 1.518(7) . ? 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 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16 0.9500 . ? C17 C20 1.520(9) . ? C17 C19 1.523(9) . ? C17 C18 1.530(8) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? Cl1A C100 1.751(7) . ? Cl2A C100 1.757(8) . ? Cl3A C100 1.755(7) . ? C100 H100 1.0000 . ? Cl1B C200 1.748(8) . ? Cl2B C200 1.758(7) . ? Cl3B C200 1.764(8) . ? C200 H200 1.0000 . ? 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 Cl1 92.08(12) . . ? N1 Pd1 Cl3 176.95(13) . . ? Cl1 Pd1 Cl3 90.96(5) . . ? N1 Pd1 Cl2 92.88(12) . . ? Cl1 Pd1 Cl2 174.96(5) . . ? Cl3 Pd1 Cl2 84.08(5) . . ? N1 Pd1 Pd2 130.65(13) . . ? Cl1 Pd1 Pd2 128.42(4) . . ? Cl3 Pd1 Pd2 46.60(4) . . ? Cl2 Pd1 Pd2 46.86(3) . . ? Cl3 Pd2 Cl5 93.23(5) . . ? Cl3 Pd2 Cl2 86.06(5) . . ? Cl5 Pd2 Cl2 175.88(5) . . ? Cl3 Pd2 Cl4 176.12(5) . . ? Cl5 Pd2 Cl4 85.45(5) . . ? Cl2 Pd2 Cl4 94.99(5) . . ? Cl3 Pd2 Pd3 126.85(4) . . ? Cl5 Pd2 Pd3 49.67(4) . . ? Cl2 Pd2 Pd3 128.04(4) . . ? Cl4 Pd2 Pd3 49.83(3) . . ? Cl3 Pd2 Pd1 47.86(3) . . ? Cl5 Pd2 Pd1 129.22(4) . . ? Cl2 Pd2 Pd1 47.94(3) . . ? Cl4 Pd2 Pd1 130.92(4) . . ? Pd3 Pd2 Pd1 122.785(14) . . ? N2 Pd3 Cl6 90.88(12) . . ? N2 Pd3 Cl5 176.98(12) . . ? Cl6 Pd3 Cl5 92.06(5) . . ? N2 Pd3 Cl4 93.40(12) . . ? Cl6 Pd3 Cl4 175.37(5) . . ? Cl5 Pd3 Cl4 83.63(5) . . ? N2 Pd3 Pd2 128.89(12) . . ? Cl6 Pd3 Pd2 126.77(4) . . ? Cl5 Pd3 Pd2 48.40(3) . . ? Cl4 Pd3 Pd2 48.78(4) . . ? Pd2 Cl2 Pd1 85.20(4) . . ? Pd2 Cl3 Pd1 85.53(5) . . ? Pd2 Cl4 Pd3 81.40(4) . . ? Pd2 Cl5 Pd3 81.93(4) . . ? C5 N1 C4 121.4(4) . . ? C5 N1 Pd1 120.2(4) . . ? C4 N1 Pd1 118.1(3) . . ? C16 N2 C17 118.3(5) . . ? C16 N2 Pd3 121.5(4) . . ? C17 N2 Pd3 120.2(3) . . ? C4 C1A H1A1 109.5 . . ? C4 C1A H1A2 109.5 . . ? H1A1 C1A H1A2 109.5 . . ? C4 C1A H1A3 109.5 . . ? H1A1 C1A H1A3 109.5 . . ? H1A2 C1A H1A3 109.5 . . ? C4 C2A H2A1 109.5 . . ? C4 C2A H2A2 109.5 . . ? H2A1 C2A H2A2 109.5 . . ? C4 C2A H2A3 109.5 . . ? H2A1 C2A H2A3 109.5 . . ? H2A2 C2A H2A3 109.5 . . ? C4 C3A H3A1 109.5 . . ? C4 C3A H3A2 109.5 . . ? H3A1 C3A H3A2 109.5 . . ? C4 C3A H3A3 109.5 . . ? H3A1 C3A H3A3 109.5 . . ? H3A2 C3A H3A3 109.5 . . ? C4 C1B H1B1 109.5 . . ? C4 C1B H1B2 109.5 . . ? H1B1 C1B H1B2 109.5 . . ? C4 C1B H1B3 109.5 . . ? H1B1 C1B H1B3 109.5 . . ? H1B2 C1B H1B3 109.5 . . ? C4 C2B H2B1 109.5 . . ? C4 C2B H2B2 109.5 . . ? H2B1 C2B H2B2 109.5 . . ? C4 C2B H2B3 109.5 . . ? H2B1 C2B H2B3 109.5 . . ? H2B2 C2B H2B3 109.5 . . ? C4 C3B H3B1 109.5 . . ? C4 C3B H3B2 109.5 . . ? H3B1 C3B H3B2 109.5 . . ? C4 C3B H3B3 109.5 . . ? H3B1 C3B H3B3 109.5 . . ? H3B2 C3B H3B3 109.5 . . ? C1A C4 C3B 143.0(10) . . ? C1A C4 N1 110.8(9) . . ? C3B C4 N1 105.8(6) . . ? C1A C4 C3A 115.0(19) . . ? C3B C4 C3A 46.1(14) . . ? N1 C4 C3A 107.5(10) . . ? C1A C4 C2B 58.3(12) . . ? C3B C4 C2B 111.4(8) . . ? N1 C4 C2B 113.0(5) . . ? C3A C4 C2B 138.5(10) . . ? C1A C4 C1B 51.8(12) . . ? C3B C4 C1B 110.6(8) . . ? N1 C4 C1B 109.4(5) . . ? C3A C4 C1B 66.9(16) . . ? C2B C4 C1B 106.6(7) . . ? C1A C4 C2A 111.5(15) . . ? C3B C4 C2A 59.3(11) . . ? N1 C4 C2A 109.1(9) . . ? C3A C4 C2A 102.6(17) . . ? C2B C4 C2A 55.6(11) . . ? C1B C4 C2A 141.5(10) . . ? N1 C5 C6 123.8(5) . . ? N1 C5 H5 118.1 . . ? C6 C5 H5 118.1 . . ? C7 C6 C11 121.8(5) . . ? C7 C6 C5 124.0(5) . . ? C11 C6 C5 114.2(4) . . ? C6 C7 C8 119.0(5) . . ? C6 C7 C12 121.3(5) . . ? C8 C7 C12 119.6(4) . . ? C9 C8 C7 119.2(4) . . ? C9 C8 C13 121.1(5) . . ? C7 C8 C13 119.5(4) . . ? C8 C9 C10 121.9(5) . . ? C8 C9 C16 121.9(4) . . ? C10 C9 C16 116.0(4) . . ? C11 C10 C9 118.6(5) . . ? C11 C10 C14 120.1(4) . . ? C9 C10 C14 121.3(5) . . ? C10 C11 C6 119.0(4) . . ? C10 C11 C15 121.4(5) . . ? C6 C11 C15 119.6(5) . . ? C7 C12 H12A 109.5 . . ? C7 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C7 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C8 C13 H13A 109.5 . . ? C8 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C8 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C10 C14 H14A 109.5 . . ? C10 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C10 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C11 C15 H15A 109.5 . . ? C11 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C11 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N2 C16 C9 125.3(5) . . ? N2 C16 H16 117.4 . . ? C9 C16 H16 117.4 . . ? C20 C17 C19 113.3(7) . . ? C20 C17 N2 108.0(5) . . ? C19 C17 N2 108.8(5) . . ? C20 C17 C18 108.4(5) . . ? C19 C17 C18 109.5(5) . . ? N2 C17 C18 108.8(5) . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C17 C20 H20A 109.5 . . ? C17 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C17 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? Cl1A C100 Cl3A 109.2(4) . . ? Cl1A C100 Cl2A 110.3(4) . . ? Cl3A C100 Cl2A 111.8(4) . . ? Cl1A C100 H100 108.5 . . ? Cl3A C100 H100 108.5 . . ? Cl2A C100 H100 108.5 . . ? Cl1B C200 Cl2B 108.9(4) . . ? Cl1B C200 Cl3B 110.7(4) . . ? Cl2B C200 Cl3B 110.9(4) . . ? Cl1B C200 H200 108.8 . . ? Cl2B C200 H200 108.8 . . ? Cl3B C200 H200 108.8 . . ? 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 Pd2 Cl3 178.20(15) . . . . ? Cl1 Pd1 Pd2 Cl3 -43.90(7) . . . . ? Cl2 Pd1 Pd2 Cl3 133.75(7) . . . . ? N1 Pd1 Pd2 Cl5 -131.61(15) . . . . ? Cl1 Pd1 Pd2 Cl5 6.28(7) . . . . ? Cl3 Pd1 Pd2 Cl5 50.18(7) . . . . ? Cl2 Pd1 Pd2 Cl5 -176.06(7) . . . . ? N1 Pd1 Pd2 Cl2 44.45(15) . . . . ? Cl1 Pd1 Pd2 Cl2 -177.65(7) . . . . ? Cl3 Pd1 Pd2 Cl2 -133.75(7) . . . . ? N1 Pd1 Pd2 Cl4 -6.72(15) . . . . ? Cl1 Pd1 Pd2 Cl4 131.18(7) . . . . ? Cl3 Pd1 Pd2 Cl4 175.08(6) . . . . ? Cl2 Pd1 Pd2 Cl4 -51.17(6) . . . . ? N1 Pd1 Pd2 Pd3 -69.51(15) . . . . ? Cl1 Pd1 Pd2 Pd3 68.38(6) . . . . ? Cl3 Pd1 Pd2 Pd3 112.28(5) . . . . ? Cl2 Pd1 Pd2 Pd3 -113.96(5) . . . . ? Cl3 Pd2 Pd3 N2 124.70(16) . . . . ? Cl5 Pd2 Pd3 N2 -178.24(16) . . . . ? Cl2 Pd2 Pd3 N2 6.19(16) . . . . ? Cl4 Pd2 Pd3 N2 -52.75(16) . . . . ? Pd1 Pd2 Pd3 N2 65.67(16) . . . . ? Cl3 Pd2 Pd3 Cl6 -4.17(6) . . . . ? Cl5 Pd2 Pd3 Cl6 52.88(6) . . . . ? Cl2 Pd2 Pd3 Cl6 -122.69(6) . . . . ? Cl4 Pd2 Pd3 Cl6 178.38(6) . . . . ? Pd1 Pd2 Pd3 Cl6 -63.20(5) . . . . ? Cl3 Pd2 Pd3 Cl5 -57.06(6) . . . . ? Cl2 Pd2 Pd3 Cl5 -175.57(6) . . . . ? Cl4 Pd2 Pd3 Cl5 125.49(6) . . . . ? Pd1 Pd2 Pd3 Cl5 -116.09(5) . . . . ? Cl3 Pd2 Pd3 Cl4 177.45(6) . . . . ? Cl5 Pd2 Pd3 Cl4 -125.49(6) . . . . ? Cl2 Pd2 Pd3 Cl4 58.93(6) . . . . ? Pd1 Pd2 Pd3 Cl4 118.42(5) . . . . ? Cl3 Pd2 Cl2 Pd1 -32.47(4) . . . . ? Cl4 Pd2 Cl2 Pd1 143.78(4) . . . . ? Pd3 Pd2 Cl2 Pd1 102.71(4) . . . . ? N1 Pd1 Cl2 Pd2 -147.86(13) . . . . ? Cl3 Pd1 Cl2 Pd2 31.85(5) . . . . ? Cl5 Pd2 Cl3 Pd1 -143.41(4) . . . . ? Cl2 Pd2 Cl3 Pd1 32.52(4) . . . . ? Pd3 Pd2 Cl3 Pd1 -103.56(4) . . . . ? Cl1 Pd1 Cl3 Pd2 147.09(6) . . . . ? Cl2 Pd1 Cl3 Pd2 -32.00(5) . . . . ? Cl5 Pd2 Cl4 Pd3 38.51(4) . . . . ? Cl2 Pd2 Cl4 Pd3 -137.38(4) . . . . ? Pd1 Pd2 Cl4 Pd3 -101.89(4) . . . . ? N2 Pd3 Cl4 Pd2 141.64(13) . . . . ? Cl5 Pd3 Cl4 Pd2 -37.78(4) . . . . ? Cl3 Pd2 Cl5 Pd3 137.73(5) . . . . ? Cl4 Pd2 Cl5 Pd3 -38.61(4) . . . . ? Pd1 Pd2 Cl5 Pd3 102.94(4) . . . . ? Cl6 Pd3 Cl5 Pd2 -140.27(5) . . . . ? Cl4 Pd3 Cl5 Pd2 38.04(4) . . . . ? Cl1 Pd1 N1 C5 -103.4(4) . . . . ? Cl2 Pd1 N1 C5 75.6(4) . . . . ? Pd2 Pd1 N1 C5 44.8(4) . . . . ? Cl1 Pd1 N1 C4 82.1(3) . . . . ? Cl2 Pd1 N1 C4 -98.8(3) . . . . ? Pd2 Pd1 N1 C4 -129.6(3) . . . . ? Cl6 Pd3 N2 C16 105.3(4) . . . . ? Cl4 Pd3 N2 C16 -73.0(4) . . . . ? Pd2 Pd3 N2 C16 -36.1(4) . . . . ? Cl6 Pd3 N2 C17 -77.5(4) . . . . ? Cl4 Pd3 N2 C17 104.2(4) . . . . ? Pd2 Pd3 N2 C17 141.1(3) . . . . ? C5 N1 C4 C1A 89.1(13) . . . . ? Pd1 N1 C4 C1A -96.6(13) . . . . ? C5 N1 C4 C3B -96.4(8) . . . . ? Pd1 N1 C4 C3B 78.0(7) . . . . ? C5 N1 C4 C3A -144.5(17) . . . . ? Pd1 N1 C4 C3A 29.8(17) . . . . ? C5 N1 C4 C2B 25.8(8) . . . . ? Pd1 N1 C4 C2B -159.8(6) . . . . ? C5 N1 C4 C1B 144.5(6) . . . . ? Pd1 N1 C4 C1B -41.2(6) . . . . ? C5 N1 C4 C2A -34.0(12) . . . . ? Pd1 N1 C4 C2A 140.4(11) . . . . ? C4 N1 C5 C6 163.6(4) . . . . ? Pd1 N1 C5 C6 -10.6(7) . . . . ? N1 C5 C6 C7 79.9(7) . . . . ? N1 C5 C6 C11 -101.1(6) . . . . ? C11 C6 C7 C8 5.0(7) . . . . ? C5 C6 C7 C8 -176.1(4) . . . . ? C11 C6 C7 C12 -171.6(5) . . . . ? C5 C6 C7 C12 7.4(7) . . . . ? C6 C7 C8 C9 2.1(7) . . . . ? C12 C7 C8 C9 178.7(4) . . . . ? C6 C7 C8 C13 -173.6(5) . . . . ? C12 C7 C8 C13 3.0(7) . . . . ? C7 C8 C9 C10 -7.1(7) . . . . ? C13 C8 C9 C10 168.5(5) . . . . ? C7 C8 C9 C16 179.1(4) . . . . ? C13 C8 C9 C16 -5.3(7) . . . . ? C8 C9 C10 C11 4.9(7) . . . . ? C16 C9 C10 C11 179.0(4) . . . . ? C8 C9 C10 C14 -175.5(5) . . . . ? C16 C9 C10 C14 -1.3(7) . . . . ? C9 C10 C11 C6 2.2(7) . . . . ? C14 C10 C11 C6 -177.5(5) . . . . ? C9 C10 C11 C15 -178.4(5) . . . . ? C14 C10 C11 C15 1.9(7) . . . . ? C7 C6 C11 C10 -7.2(7) . . . . ? C5 C6 C11 C10 173.8(4) . . . . ? C7 C6 C11 C15 173.4(5) . . . . ? C5 C6 C11 C15 -5.6(7) . . . . ? C17 N2 C16 C9 -173.7(4) . . . . ? Pd3 N2 C16 C9 3.6(7) . . . . ? C8 C9 C16 N2 -78.3(7) . . . . ? C10 C9 C16 N2 107.6(6) . . . . ? C16 N2 C17 C20 57.7(7) . . . . ? Pd3 N2 C17 C20 -119.6(5) . . . . ? C16 N2 C17 C19 -65.7(7) . . . . ? Pd3 N2 C17 C19 117.0(5) . . . . ? C16 N2 C17 C18 175.1(5) . . . . ? Pd3 N2 C17 C18 -2.2(6) . . . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 70.77 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 1.699 _refine_diff_density_min -1.374 _refine_diff_density_rms 0.143