data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Juan Tejeda' _publ_contact_author_address ; Ciudad Real 13071 ; _publ_contact_author_email juan.tejeda@uclm.es loop_ _publ_author_name V.Hornillos J.Guerra 'A.de Cozar' P.Prieto S.Merino M.Maestro ; E.Diez-Barra ; J.Tejeda # Attachment '- compound 4.CIF' data_mm _database_code_depnum_ccdc_archive 'CCDC 699228' #TrackingRef '- compound 4.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C15 H26 Br2 N6 O Pd' _chemical_formula_sum 'C15 H26 Br2 N6 O Pd' _chemical_formula_weight 572.65 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 '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 Rhombohedral _symmetry_space_group_name_H-M R-3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'z, x, y' 'y, z, x' '-x, -y, -z' '-z, -x, -y' '-y, -z, -x' _cell_length_a 20.1373(7) _cell_length_b 20.1373(7) _cell_length_c 20.1373(7) _cell_angle_alpha 117.27 _cell_angle_beta 117.27 _cell_angle_gamma 117.27 _cell_volume 3442.3(2) _cell_formula_units_Z 6 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Needle _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.622 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1692 _exptl_absorpt_coefficient_mu 4.304 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.2005 _exptl_absorpt_correction_T_max 0.5281 _exptl_absorpt_process_details ; Siemens SADABS program multi-scan Blessing, Acta Cryst. (1995) A51 33-38 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.2 _diffrn_reflns_number 22268 _diffrn_reflns_av_R_equivalents 0.0358 _diffrn_reflns_av_sigmaI/netI 0.0380 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.05 _diffrn_reflns_theta_max 28.28 _reflns_number_total 5576 _reflns_number_gt 3872 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0520P)^2^+5.1010P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5576 _refine_ls_number_parameters 264 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0710 _refine_ls_R_factor_gt 0.0365 _refine_ls_wR_factor_ref 0.1147 _refine_ls_wR_factor_gt 0.0973 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.043 _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 0.31118(3) 0.54970(3) 0.13698(3) 0.03778(11) Uani 1 1 d . . . Br1 Br 0.47650(6) 0.66540(6) 0.17475(6) 0.05880(16) Uani 1 1 d . . . Br2 Br 0.21196(7) 0.33851(6) -0.01701(6) 0.0723(2) Uani 1 1 d . . . O1A O 0.505(2) 0.722(2) 0.561(2) 0.136(8) Uani 0.349(9) 1 d P A 1 O1B O 0.412(2) 0.567(2) 0.403(2) 0.110(6) Uani 0.349(9) 1 d P A 2 O1C O 0.620(2) 0.741(2) 0.5838(19) 0.124(7) Uani 0.349(9) 1 d P A 3 N1 N 0.4234(4) 0.8031(4) 0.2790(4) 0.0407(8) Uani 1 1 d . . . N2 N 0.4894(4) 0.8948(4) 0.4519(4) 0.0464(9) Uani 1 1 d . . . N3 N 0.4326(4) 0.7755(4) 0.3707(4) 0.0383(8) Uani 1 1 d . . . N4 N 0.2716(4) 0.5688(4) 0.2628(4) 0.0458(9) Uani 1 1 d . . . N5 N 0.1879(6) 0.5069(5) 0.2514(6) 0.0685(13) Uani 1 1 d . . . N6 N 0.0760(5) 0.3602(5) 0.0480(5) 0.0595(11) Uani 1 1 d . B . C1 C 0.3936(5) 0.7191(5) 0.2667(5) 0.0385(9) Uani 1 1 d . . . C2 C 0.4818(5) 0.9074(5) 0.3919(5) 0.0486(12) Uani 1 1 d . . . H2A H 0.5125 0.9791 0.4222 0.058 Uiso 1 1 calc R . . C3 C 0.4152(5) 0.7189(5) 0.3984(5) 0.0446(10) Uani 1 1 d . . . H3A H 0.4237 0.7612 0.4589 0.054 Uiso 1 1 calc R . . C4 C 0.0685(7) 0.3792(7) 0.1171(8) 0.0758(18) Uani 1 1 d . . . H4A H -0.0125 0.3092 0.0735 0.091 Uiso 1 1 calc R . . C5 C 0.2083(5) 0.4840(5) 0.1436(5) 0.0434(10) Uani 1 1 d . . . C6 C 0.3948(5) 0.7864(5) 0.1861(5) 0.0499(12) Uani 1 1 d . . . H6A H 0.4449 0.8721 0.2317 0.060 Uiso 1 1 calc R . . H6B H 0.4312 0.7736 0.1743 0.060 Uiso 1 1 calc R . . C7 C 0.2452(6) 0.6681(6) 0.0468(6) 0.0633(14) Uani 1 1 d . . . H7A H 0.2075 0.6793 0.0578 0.076 Uiso 1 1 calc R . . H7B H 0.1948 0.5816 -0.0008 0.076 Uiso 1 1 calc R . . C8 C 0.2227(7) 0.6586(7) -0.0411(7) 0.0735(17) Uani 1 1 d . . . H8A H 0.2592 0.6457 -0.0530 0.088 Uiso 1 1 calc R . . H8B H 0.2764 0.7468 0.0089 0.088 Uiso 1 1 calc R . . C9 C 0.0728(9) 0.5425(10) -0.1831(8) 0.114(3) Uani 1 1 d . . . H9A H 0.0674 0.5438 -0.2324 0.171 Uiso 1 1 calc R . . H9B H 0.0361 0.5554 -0.1728 0.171 Uiso 1 1 calc R . . H9C H 0.0190 0.4543 -0.2349 0.171 Uiso 1 1 calc R . . C10 C 0.5269(6) 0.7537(6) 0.4732(6) 0.0619(14) Uani 1 1 d . A . H10A H 0.5219 0.7160 0.4158 0.074 Uiso 1 1 calc R . . H10B H 0.6182 0.8546 0.5605 0.074 Uiso 1 1 calc R . . C11 C 0.5149(13) 0.6983(13) 0.5045(12) 0.111(3) Uani 1 1 d . . . C12 C -0.0467(6) 0.2300(6) -0.1077(7) 0.079(2) Uani 1 1 d . . . C13A C -0.1340(19) 0.231(2) -0.1735(19) 0.073(6) Uani 0.48(2) 1 d P B 1 C14A C -0.0584(14) 0.3426(14) -0.1357(14) 0.067(5) Uani 0.48(2) 1 d P B 1 C13B C -0.0841(17) 0.2422(15) -0.1698(13) 0.086(7) Uani 0.52(2) 1 d P B 2 C14B C -0.129(2) 0.282(2) -0.150(2) 0.096(8) Uani 0.52(2) 1 d P B 2 C15 C -0.1457(8) 0.3293(9) -0.2009(8) 0.105(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.03805(19) 0.03484(18) 0.03452(18) 0.02724(16) 0.03112(17) 0.03104(17) Br1 0.0576(3) 0.0632(3) 0.0593(3) 0.0490(3) 0.0532(3) 0.0510(3) Br2 0.0652(4) 0.0485(3) 0.0621(4) 0.0383(3) 0.0509(3) 0.0495(3) O1A 0.163(19) 0.157(18) 0.156(18) 0.143(17) 0.138(17) 0.138(17) O1B 0.178(17) 0.122(13) 0.172(16) 0.136(14) 0.160(16) 0.138(14) O1C 0.171(17) 0.203(19) 0.133(14) 0.153(16) 0.133(14) 0.176(17) N1 0.046(2) 0.0365(19) 0.044(2) 0.0342(19) 0.040(2) 0.0341(19) N2 0.052(2) 0.036(2) 0.047(2) 0.033(2) 0.043(2) 0.036(2) N3 0.044(2) 0.0353(19) 0.0392(19) 0.0310(18) 0.0363(19) 0.0333(18) N4 0.053(2) 0.045(2) 0.053(2) 0.042(2) 0.048(2) 0.042(2) N5 0.080(3) 0.065(3) 0.084(4) 0.065(3) 0.076(3) 0.059(3) N6 0.054(3) 0.045(2) 0.065(3) 0.044(2) 0.052(3) 0.040(2) C1 0.037(2) 0.037(2) 0.036(2) 0.029(2) 0.031(2) 0.030(2) C2 0.059(3) 0.038(2) 0.054(3) 0.038(2) 0.050(3) 0.040(3) C3 0.056(3) 0.046(3) 0.048(3) 0.041(2) 0.047(3) 0.044(3) C4 0.074(4) 0.059(4) 0.090(5) 0.062(4) 0.074(4) 0.053(4) C5 0.042(2) 0.036(2) 0.046(3) 0.033(2) 0.037(2) 0.032(2) C6 0.059(3) 0.052(3) 0.057(3) 0.048(3) 0.052(3) 0.046(3) C7 0.062(3) 0.071(4) 0.064(3) 0.059(3) 0.055(3) 0.055(3) C8 0.083(4) 0.079(4) 0.069(4) 0.066(4) 0.065(4) 0.067(4) C9 0.106(6) 0.120(7) 0.084(5) 0.089(6) 0.078(5) 0.089(6) C10 0.070(4) 0.070(4) 0.056(3) 0.054(3) 0.054(3) 0.061(3) C11 0.169(9) 0.174(10) 0.148(9) 0.151(9) 0.144(9) 0.158(9) C12 0.045(3) 0.035(3) 0.051(4) 0.024(3) 0.036(3) 0.025(3) C13A 0.046(8) 0.071(11) 0.062(9) 0.051(10) 0.048(8) 0.044(9) C14A 0.048(7) 0.058(8) 0.065(8) 0.049(7) 0.048(7) 0.040(7) C13B 0.056(9) 0.064(9) 0.043(7) 0.035(7) 0.041(7) 0.039(8) C14B 0.072(11) 0.103(16) 0.072(11) 0.067(12) 0.059(10) 0.073(13) C15 0.064(4) 0.109(6) 0.080(5) 0.079(5) 0.055(4) 0.064(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 C1 1.971(4) . ? Pd1 C5 1.989(5) . ? Pd1 Br1 2.4571(6) . ? Pd1 Br2 2.4788(6) . ? O1A C11 1.17(2) . ? O1B C11 1.267(18) . ? O1C C11 1.320(17) . ? N1 C1 1.353(6) . ? N1 C2 1.369(6) . ? N1 C6 1.484(6) . ? N2 C2 1.302(6) . ? N2 N3 1.386(5) . ? N3 C1 1.338(5) . ? N3 C3 1.459(6) . ? N4 C5 1.322(6) . ? N4 N5 1.381(6) . ? N4 C3 1.464(6) . ? N5 C4 1.308(8) . ? N6 C5 1.355(6) . ? N6 C4 1.365(7) . ? N6 C12 1.496(8) . ? C2 H2A 0.9300 . ? C3 C10 1.519(7) . ? C3 H3A 0.9800 . ? C4 H4A 0.9300 . ? C6 C7 1.474(8) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C8 1.500(8) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C9 1.500(10) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 C11 1.496(10) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C12 C13B 1.334(19) . ? C12 C13A 1.66(2) . ? C13A C14A 1.48(3) . ? C14A C15 1.420(17) . ? C13B C14B 1.51(3) . ? C14B C15 1.72(3) . ? 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 C1 Pd1 C5 84.25(18) . . ? C1 Pd1 Br1 90.64(12) . . ? C5 Pd1 Br1 169.60(14) . . ? C1 Pd1 Br2 176.83(13) . . ? C5 Pd1 Br2 93.93(13) . . ? Br1 Pd1 Br2 90.74(2) . . ? C1 N1 C2 108.1(4) . . ? C1 N1 C6 127.7(4) . . ? C2 N1 C6 124.1(4) . . ? C2 N2 N3 102.3(4) . . ? C1 N3 N2 113.8(4) . . ? C1 N3 C3 125.4(4) . . ? N2 N3 C3 120.7(3) . . ? C5 N4 N5 114.6(4) . . ? C5 N4 C3 126.0(4) . . ? N5 N4 C3 119.3(4) . . ? C4 N5 N4 101.6(4) . . ? C5 N6 C4 107.5(5) . . ? C5 N6 C12 127.4(5) . . ? C4 N6 C12 124.7(5) . . ? N3 C1 N1 103.6(4) . . ? N3 C1 Pd1 121.9(3) . . ? N1 C1 Pd1 134.5(3) . . ? N2 C2 N1 112.1(4) . . ? N2 C2 H2A 123.9 . . ? N1 C2 H2A 123.9 . . ? N3 C3 N4 105.9(4) . . ? N3 C3 C10 111.5(4) . . ? N4 C3 C10 114.3(4) . . ? N3 C3 H3A 108.3 . . ? N4 C3 H3A 108.3 . . ? C10 C3 H3A 108.3 . . ? N5 C4 N6 112.5(5) . . ? N5 C4 H4A 123.8 . . ? N6 C4 H4A 123.8 . . ? N4 C5 N6 103.9(4) . . ? N4 C5 Pd1 121.3(3) . . ? N6 C5 Pd1 134.8(4) . . ? C7 C6 N1 114.2(4) . . ? C7 C6 H6A 108.7 . . ? N1 C6 H6A 108.7 . . ? C7 C6 H6B 108.7 . . ? N1 C6 H6B 108.7 . . ? H6A C6 H6B 107.6 . . ? C6 C7 C8 111.9(5) . . ? C6 C7 H7A 109.2 . . ? C8 C7 H7A 109.2 . . ? C6 C7 H7B 109.2 . . ? C8 C7 H7B 109.2 . . ? H7A C7 H7B 107.9 . . ? C7 C8 C9 114.6(6) . . ? C7 C8 H8A 108.6 . . ? C9 C8 H8A 108.6 . . ? C7 C8 H8B 108.6 . . ? C9 C8 H8B 108.6 . . ? H8A C8 H8B 107.6 . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C11 C10 C3 114.3(6) . . ? C11 C10 H10A 108.7 . . ? C3 C10 H10A 108.7 . . ? C11 C10 H10B 108.7 . . ? C3 C10 H10B 108.7 . . ? H10A C10 H10B 107.6 . . ? O1A C11 O1B 99.8(17) . . ? O1A C11 O1C 102.3(15) . . ? O1B C11 O1C 100.3(14) . . ? O1A C11 C10 117.8(13) . . ? O1B C11 C10 118.3(11) . . ? O1C C11 C10 115.4(12) . . ? C13B C12 N6 115.6(8) . . ? C13B C12 C13A 31.9(8) . . ? N6 C12 C13A 108.0(8) . . ? C14A C13A C12 115.3(14) . . ? C15 C14A C13A 109.5(13) . . ? C12 C13B C14B 113.1(15) . . ? C13B C14B C15 113.3(16) . . ? C14A C15 C14B 41.1(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 C2 N2 N3 C1 0.7(5) . . . . ? C2 N2 N3 C3 -177.3(4) . . . . ? C5 N4 N5 C4 -0.9(6) . . . . ? C3 N4 N5 C4 175.5(5) . . . . ? N2 N3 C1 N1 -1.3(5) . . . . ? C3 N3 C1 N1 176.5(4) . . . . ? N2 N3 C1 Pd1 179.6(3) . . . . ? C3 N3 C1 Pd1 -2.6(6) . . . . ? C2 N1 C1 N3 1.4(5) . . . . ? C6 N1 C1 N3 -176.3(4) . . . . ? C2 N1 C1 Pd1 -179.6(4) . . . . ? C6 N1 C1 Pd1 2.6(7) . . . . ? C5 Pd1 C1 N3 40.8(4) . . . . ? Br1 Pd1 C1 N3 -130.1(3) . . . . ? Br2 Pd1 C1 N3 -14(3) . . . . ? C5 Pd1 C1 N1 -138.0(5) . . . . ? Br1 Pd1 C1 N1 51.1(4) . . . . ? Br2 Pd1 C1 N1 166.8(19) . . . . ? N3 N2 C2 N1 0.3(5) . . . . ? C1 N1 C2 N2 -1.1(6) . . . . ? C6 N1 C2 N2 176.7(4) . . . . ? C1 N3 C3 N4 -46.1(6) . . . . ? N2 N3 C3 N4 131.6(4) . . . . ? C1 N3 C3 C10 78.9(6) . . . . ? N2 N3 C3 C10 -103.4(5) . . . . ? C5 N4 C3 N3 44.2(6) . . . . ? N5 N4 C3 N3 -131.8(4) . . . . ? C5 N4 C3 C10 -79.1(6) . . . . ? N5 N4 C3 C10 105.0(5) . . . . ? N4 N5 C4 N6 1.0(7) . . . . ? C5 N6 C4 N5 -0.8(8) . . . . ? C12 N6 C4 N5 -173.5(6) . . . . ? N5 N4 C5 N6 0.5(6) . . . . ? C3 N4 C5 N6 -175.7(4) . . . . ? N5 N4 C5 Pd1 -177.9(3) . . . . ? C3 N4 C5 Pd1 6.0(7) . . . . ? C4 N6 C5 N4 0.1(6) . . . . ? C12 N6 C5 N4 172.6(6) . . . . ? C4 N6 C5 Pd1 178.2(4) . . . . ? C12 N6 C5 Pd1 -9.4(9) . . . . ? C1 Pd1 C5 N4 -42.4(4) . . . . ? Br1 Pd1 C5 N4 18.5(10) . . . . ? Br2 Pd1 C5 N4 135.0(4) . . . . ? C1 Pd1 C5 N6 139.8(5) . . . . ? Br1 Pd1 C5 N6 -159.3(5) . . . . ? Br2 Pd1 C5 N6 -42.8(5) . . . . ? C1 N1 C6 C7 70.4(6) . . . . ? C2 N1 C6 C7 -107.1(6) . . . . ? N1 C6 C7 C8 178.5(5) . . . . ? C6 C7 C8 C9 -178.4(6) . . . . ? N3 C3 C10 C11 -179.8(6) . . . . ? N4 C3 C10 C11 -59.7(7) . . . . ? C3 C10 C11 O1A -51.1(19) . . . . ? C3 C10 C11 O1B 69.0(13) . . . . ? C3 C10 C11 O1C -172.3(11) . . . . ? C5 N6 C12 C13B -60.5(13) . . . . ? C4 N6 C12 C13B 110.7(12) . . . . ? C5 N6 C12 C13A -94.0(9) . . . . ? C4 N6 C12 C13A 77.3(11) . . . . ? C13B C12 C13A C14A -43.5(16) . . . . ? N6 C12 C13A C14A 66.3(16) . . . . ? C12 C13A C14A C15 178.8(11) . . . . ? N6 C12 C13B C14B -61.6(17) . . . . ? C13A C12 C13B C14B 21.3(18) . . . . ? C12 C13B C14B C15 168.7(11) . . . . ? C13A C14A C15 C14B 22.7(14) . . . . ? C13B C14B C15 C14A -36.5(13) . . . . ? _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.128 _refine_diff_density_min -1.083 _refine_diff_density_rms 0.111 # Attachment '- Compound 7.cif' data_VHG-42 _database_code_depnum_ccdc_archive 'CCDC 699229' #TrackingRef '- Compound 7.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C16 H28 Br2 N6 O3 Pd S' _chemical_formula_sum 'C16 H28 Br2 N6 O3 Pd S' _chemical_formula_weight 650.72 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n 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 10.4862(6) _cell_length_b 15.5606(9) _cell_length_c 14.7375(8) _cell_angle_alpha 90.00 _cell_angle_beta 100.5700(10) _cell_angle_gamma 90.00 _cell_volume 2363.9(2) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.48 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.828 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1288 _exptl_absorpt_coefficient_mu 4.282 _exptl_absorpt_correction_type Multiscan _exptl_absorpt_correction_T_min 0.2233 _exptl_absorpt_correction_T_max 0.3598 _exptl_absorpt_process_details ; Siemens SADABS program multi-scan Blessing, Acta Cryst. (1995) A51 33-38 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.3 _diffrn_reflns_number 14026 _diffrn_reflns_av_R_equivalents 0.0233 _diffrn_reflns_av_sigmaI/netI 0.0268 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.92 _diffrn_reflns_theta_max 26.37 _reflns_number_total 4836 _reflns_number_gt 3930 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0523P)^2^+2.1157P] 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 4836 _refine_ls_number_parameters 272 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0466 _refine_ls_R_factor_gt 0.0337 _refine_ls_wR_factor_ref 0.0945 _refine_ls_wR_factor_gt 0.0885 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.054 _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 0.12724(3) 0.232735(19) 0.797242(18) 0.03085(10) Uani 1 1 d . . . Br1 Br 0.20630(5) 0.22388(4) 0.64989(3) 0.06120(16) Uani 1 1 d . . . Br2 Br -0.01687(4) 0.35279(3) 0.73564(3) 0.04946(13) Uani 1 1 d . . . S1 S 0.23817(11) 0.51173(7) 1.03397(9) 0.0526(3) Uani 1 1 d . . . O1 O 0.2682(3) 0.42499(19) 0.9904(2) 0.0495(7) Uani 1 1 d . . . O2 O 0.3549(3) 0.5573(2) 1.0646(3) 0.0705(10) Uani 1 1 d . . . O3 O 0.1390(3) 0.5505(2) 0.9671(3) 0.0745(10) Uani 1 1 d . . . N1 N 0.3212(3) 0.1511(2) 0.9378(2) 0.0376(7) Uani 1 1 d . . . N2 N 0.3955(4) 0.0811(2) 0.9679(2) 0.0519(9) Uani 1 1 d . . . H2B H 0.4486 0.0743 1.0192 0.062 Uiso 1 1 calc R . . N3 N 0.2771(3) 0.0622(2) 0.8300(2) 0.0484(9) Uani 1 1 d . . . N4 N 0.1825(3) 0.2459(2) 0.9969(2) 0.0338(7) Uani 1 1 d . . . N5 N 0.1416(4) 0.2641(2) 1.0778(2) 0.0430(8) Uani 1 1 d . . . H5A H 0.1869 0.2680 1.1325 0.052 Uiso 1 1 calc R . . N6 N -0.0193(3) 0.2637(2) 0.9594(2) 0.0367(7) Uani 1 1 d . . . C1 C 0.3666(4) 0.0278(3) 0.9005(3) 0.0581(13) Uani 1 1 d . . . H1A H 0.4018 -0.0270 0.8995 0.070 Uiso 1 1 calc R . . C2 C 0.2473(4) 0.1419(3) 0.8543(3) 0.0371(8) Uani 1 1 d . . . C3 C 0.3192(4) 0.2259(3) 0.9987(3) 0.0367(8) Uani 1 1 d . . . H3B H 0.3584 0.2089 1.0617 0.044 Uiso 1 1 calc R . . C4 C 0.0185(4) 0.2741(3) 1.0516(3) 0.0439(10) Uani 1 1 d . . . H4A H -0.0381 0.2870 1.0915 0.053 Uiso 1 1 calc R . . C5 C 0.0877(4) 0.2463(2) 0.9230(3) 0.0316(8) Uani 1 1 d . . . C6 C 0.2106(5) 0.0119(3) 0.7487(4) 0.0721(16) Uani 1 1 d . A . H6A H 0.1930 0.0496 0.6954 0.087 Uiso 1 1 calc R . . H6B H 0.2684 -0.0331 0.7353 0.087 Uiso 1 1 calc R . . C7 C 0.0891(11) -0.0269(9) 0.7629(7) 0.165(5) Uani 1 1 d . . . C8A C 0.0085(18) -0.0030(13) 0.8099(16) 0.062(8) Uani 0.34(3) 1 d P A 1 C8B C 0.0475(15) -0.0483(13) 0.8471(15) 0.134(7) Uani 0.66(3) 1 d P A 2 C9 C -0.0939(10) -0.0639(5) 0.8459(8) 0.143(4) Uani 1 1 d . . . C10 C 0.3958(4) 0.3004(3) 0.9708(3) 0.0428(9) Uani 1 1 d . . . H10A H 0.3630 0.3140 0.9065 0.051 Uiso 1 1 calc R . . H10B H 0.4857 0.2830 0.9760 0.051 Uiso 1 1 calc R . . C11 C 0.3901(4) 0.3804(3) 1.0283(3) 0.0485(10) Uani 1 1 d . . . H11A H 0.3920 0.3651 1.0923 0.058 Uiso 1 1 calc R . . H11B H 0.4637 0.4173 1.0251 0.058 Uiso 1 1 calc R . . C12 C 0.1724(5) 0.4817(4) 1.1294(4) 0.0693(14) Uani 1 1 d . . . H12A H 0.1508 0.5322 1.1607 0.104 Uiso 1 1 calc R . . H12B H 0.2347 0.4482 1.1706 0.104 Uiso 1 1 calc R . . H12C H 0.0956 0.4481 1.1094 0.104 Uiso 1 1 calc R . . C13 C -0.1560(4) 0.2596(3) 0.9126(3) 0.0489(10) Uani 1 1 d . . . H13A H -0.1671 0.2922 0.8556 0.059 Uiso 1 1 calc R . . H13B H -0.2107 0.2851 0.9517 0.059 Uiso 1 1 calc R . . C14 C -0.1969(5) 0.1680(4) 0.8916(5) 0.0821(18) Uani 1 1 d . . . H14A H -0.1601 0.1487 0.8393 0.099 Uiso 1 1 calc R . . H14B H -0.1599 0.1326 0.9441 0.099 Uiso 1 1 calc R . . C15 C -0.3374(7) 0.1531(6) 0.8708(7) 0.116(3) Uani 1 1 d . . . H15A H -0.3525 0.0936 0.8522 0.139 Uiso 1 1 calc R . . H15B H -0.3716 0.1612 0.9270 0.139 Uiso 1 1 calc R . . C16 C -0.4061(8) 0.2048(8) 0.8031(5) 0.142(4) Uani 1 1 d . . . H16A H -0.4966 0.1908 0.7948 0.213 Uiso 1 1 calc R . . H16B H -0.3758 0.1956 0.7462 0.213 Uiso 1 1 calc R . . H16C H -0.3936 0.2639 0.8211 0.213 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 0.02843(15) 0.03772(17) 0.02602(15) -0.00283(11) 0.00400(10) 0.00449(11) Br1 0.0544(3) 0.0971(4) 0.0356(2) -0.0074(2) 0.0174(2) 0.0088(2) Br2 0.0560(3) 0.0517(3) 0.0393(2) 0.00816(18) 0.00522(18) 0.0175(2) S1 0.0487(6) 0.0400(6) 0.0704(8) -0.0048(5) 0.0141(5) 0.0009(5) O1 0.0374(15) 0.0516(18) 0.0576(18) -0.0042(14) 0.0040(13) 0.0059(13) O2 0.057(2) 0.051(2) 0.104(3) -0.019(2) 0.0183(19) -0.0105(16) O3 0.067(2) 0.057(2) 0.097(3) 0.016(2) 0.009(2) 0.0165(18) N1 0.0376(17) 0.0374(17) 0.0353(17) -0.0072(13) 0.0000(13) 0.0141(14) N2 0.052(2) 0.050(2) 0.046(2) -0.0079(17) -0.0097(16) 0.0236(17) N3 0.048(2) 0.048(2) 0.045(2) -0.0165(16) -0.0021(15) 0.0173(16) N4 0.0391(17) 0.0362(18) 0.0275(15) -0.0016(12) 0.0101(13) 0.0041(13) N5 0.059(2) 0.047(2) 0.0262(16) -0.0014(14) 0.0153(15) 0.0054(16) N6 0.0333(16) 0.0353(17) 0.0454(19) -0.0001(14) 0.0176(14) 0.0006(13) C1 0.056(3) 0.052(3) 0.059(3) -0.013(2) -0.010(2) 0.027(2) C2 0.0349(19) 0.042(2) 0.034(2) -0.0075(16) 0.0057(15) 0.0084(16) C3 0.037(2) 0.042(2) 0.0277(18) -0.0074(16) -0.0014(15) 0.0119(16) C4 0.053(3) 0.046(2) 0.039(2) -0.0003(18) 0.0243(19) 0.0025(19) C5 0.0330(18) 0.0274(18) 0.0360(19) 0.0011(14) 0.0110(15) 0.0024(14) C6 0.079(4) 0.066(3) 0.061(3) -0.036(3) -0.015(3) 0.027(3) C7 0.148(9) 0.220(13) 0.118(8) -0.069(9) 0.005(7) -0.104(9) C8A 0.060(10) 0.035(11) 0.085(15) 0.008(8) -0.005(9) -0.003(7) C8B 0.085(9) 0.101(12) 0.209(17) 0.055(12) 0.007(10) -0.020(9) C9 0.138(7) 0.068(5) 0.217(11) 0.027(6) 0.017(7) -0.021(5) C10 0.0300(19) 0.051(2) 0.047(2) -0.0122(19) 0.0048(16) 0.0041(17) C11 0.036(2) 0.048(2) 0.059(3) -0.012(2) 0.0032(19) 0.0031(18) C12 0.079(4) 0.059(3) 0.076(4) -0.010(3) 0.029(3) 0.002(3) C13 0.035(2) 0.050(3) 0.065(3) -0.003(2) 0.017(2) 0.0031(18) C14 0.061(3) 0.070(4) 0.114(5) -0.027(4) 0.010(3) -0.010(3) C15 0.067(4) 0.125(7) 0.155(8) -0.046(6) 0.023(5) -0.032(4) C16 0.082(5) 0.276(14) 0.064(5) 0.004(6) 0.001(4) 0.012(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 C2 1.975(4) . ? Pd1 C5 1.983(4) . ? Pd1 Br1 2.4663(5) . ? Pd1 Br2 2.4686(5) . ? S1 O2 1.415(3) . ? S1 O3 1.429(4) . ? S1 O1 1.552(3) . ? S1 C12 1.740(5) . ? O1 C11 1.471(5) . ? N1 C2 1.336(5) . ? N1 N2 1.365(4) . ? N1 C3 1.472(5) . ? N2 C1 1.287(6) . ? N2 H2B 0.8600 . ? N3 C2 1.344(5) . ? N3 C1 1.375(5) . ? N3 C6 1.492(5) . ? N4 C5 1.333(5) . ? N4 N5 1.369(4) . ? N4 C3 1.462(5) . ? N5 C4 1.288(6) . ? N5 H5A 0.8600 . ? N6 C4 1.354(5) . ? N6 C5 1.357(5) . ? N6 C13 1.474(5) . ? C1 H1A 0.9300 . ? C3 C10 1.510(6) . ? C3 H3B 0.9800 . ? C4 H4A 0.9300 . ? C6 C7 1.459(12) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C8A 1.24(2) . ? C7 C8B 1.43(2) . ? C8A C9 1.59(2) . ? C8B C9 1.499(16) . ? C10 C11 1.513(6) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 C14 1.504(7) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 C15 1.467(8) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 C16 1.377(11) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? 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 Pd1 C5 84.52(15) . . ? C2 Pd1 Br1 92.53(11) . . ? C5 Pd1 Br1 172.06(11) . . ? C2 Pd1 Br2 175.87(11) . . ? C5 Pd1 Br2 92.53(10) . . ? Br1 Pd1 Br2 90.025(18) . . ? O2 S1 O3 119.1(2) . . ? O2 S1 O1 109.79(19) . . ? O3 S1 O1 105.0(2) . . ? O2 S1 C12 108.9(3) . . ? O3 S1 C12 109.0(3) . . ? O1 S1 C12 104.0(2) . . ? C11 O1 S1 118.8(3) . . ? C2 N1 N2 114.4(3) . . ? C2 N1 C3 125.1(3) . . ? N2 N1 C3 120.3(3) . . ? C1 N2 N1 103.0(3) . . ? C1 N2 H2B 128.5 . . ? N1 N2 H2B 128.5 . . ? C2 N3 C1 108.5(3) . . ? C2 N3 C6 127.0(3) . . ? C1 N3 C6 123.8(4) . . ? C5 N4 N5 113.9(3) . . ? C5 N4 C3 126.7(3) . . ? N5 N4 C3 119.4(3) . . ? C4 N5 N4 102.8(3) . . ? C4 N5 H5A 128.6 . . ? N4 N5 H5A 128.6 . . ? C4 N6 C5 108.1(3) . . ? C4 N6 C13 123.7(3) . . ? C5 N6 C13 127.6(3) . . ? N2 C1 N3 111.3(4) . . ? N2 C1 H1A 124.3 . . ? N3 C1 H1A 124.3 . . ? N1 C2 N3 102.8(3) . . ? N1 C2 Pd1 122.2(3) . . ? N3 C2 Pd1 135.0(3) . . ? N4 C3 N1 106.3(3) . . ? N4 C3 C10 113.6(3) . . ? N1 C3 C10 112.0(3) . . ? N4 C3 H3B 108.3 . . ? N1 C3 H3B 108.3 . . ? C10 C3 H3B 108.3 . . ? N5 C4 N6 112.3(3) . . ? N5 C4 H4A 123.9 . . ? N6 C4 H4A 123.9 . . ? N4 C5 N6 103.0(3) . . ? N4 C5 Pd1 120.7(3) . . ? N6 C5 Pd1 136.1(3) . . ? C7 C6 N3 113.2(5) . . ? C7 C6 H6A 108.9 . . ? N3 C6 H6A 108.9 . . ? C7 C6 H6B 108.9 . . ? N3 C6 H6B 108.9 . . ? H6A C6 H6B 107.7 . . ? C8A C7 C8B 40.4(9) . . ? C8A C7 C6 131.0(12) . . ? C8B C7 C6 129.4(9) . . ? C7 C8A C9 125.2(15) . . ? C7 C8B C9 119.1(15) . . ? C8B C9 C8A 35.2(7) . . ? C3 C10 C11 113.7(3) . . ? C3 C10 H10A 108.8 . . ? C11 C10 H10A 108.8 . . ? C3 C10 H10B 108.8 . . ? C11 C10 H10B 108.8 . . ? H10A C10 H10B 107.7 . . ? O1 C11 C10 107.2(3) . . ? O1 C11 H11A 110.3 . . ? C10 C11 H11A 110.3 . . ? O1 C11 H11B 110.3 . . ? C10 C11 H11B 110.3 . . ? H11A C11 H11B 108.5 . . ? S1 C12 H12A 109.5 . . ? S1 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? S1 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N6 C13 C14 110.7(4) . . ? N6 C13 H13A 109.5 . . ? C14 C13 H13A 109.5 . . ? N6 C13 H13B 109.5 . . ? C14 C13 H13B 109.5 . . ? H13A C13 H13B 108.1 . . ? C15 C14 C13 115.5(5) . . ? C15 C14 H14A 108.4 . . ? C13 C14 H14A 108.4 . . ? C15 C14 H14B 108.4 . . ? C13 C14 H14B 108.4 . . ? H14A C14 H14B 107.5 . . ? C16 C15 C14 115.5(8) . . ? C16 C15 H15A 108.4 . . ? C14 C15 H15A 108.4 . . ? C16 C15 H15B 108.4 . . ? C14 C15 H15B 108.4 . . ? H15A C15 H15B 107.5 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? 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 O2 S1 O1 C11 33.4(4) . . . . ? O3 S1 O1 C11 162.6(3) . . . . ? C12 S1 O1 C11 -83.0(4) . . . . ? C2 N1 N2 C1 0.3(5) . . . . ? C3 N1 N2 C1 175.9(4) . . . . ? C5 N4 N5 C4 1.2(4) . . . . ? C3 N4 N5 C4 -177.0(3) . . . . ? N1 N2 C1 N3 -0.1(6) . . . . ? C2 N3 C1 N2 -0.2(6) . . . . ? C6 N3 C1 N2 -170.9(5) . . . . ? N2 N1 C2 N3 -0.4(5) . . . . ? C3 N1 C2 N3 -175.7(4) . . . . ? N2 N1 C2 Pd1 178.1(3) . . . . ? C3 N1 C2 Pd1 2.8(5) . . . . ? C1 N3 C2 N1 0.4(5) . . . . ? C6 N3 C2 N1 170.7(5) . . . . ? C1 N3 C2 Pd1 -177.9(4) . . . . ? C6 N3 C2 Pd1 -7.6(7) . . . . ? C5 Pd1 C2 N1 -41.0(3) . . . . ? Br1 Pd1 C2 N1 131.6(3) . . . . ? Br2 Pd1 C2 N1 3.5(19) . . . . ? C5 Pd1 C2 N3 137.0(4) . . . . ? Br1 Pd1 C2 N3 -50.4(4) . . . . ? Br2 Pd1 C2 N3 -178.5(13) . . . . ? C5 N4 C3 N1 -42.2(5) . . . . ? N5 N4 C3 N1 135.7(3) . . . . ? C5 N4 C3 C10 81.4(5) . . . . ? N5 N4 C3 C10 -100.8(4) . . . . ? C2 N1 C3 N4 44.9(5) . . . . ? N2 N1 C3 N4 -130.1(4) . . . . ? C2 N1 C3 C10 -79.7(5) . . . . ? N2 N1 C3 C10 105.3(4) . . . . ? N4 N5 C4 N6 -0.3(4) . . . . ? C5 N6 C4 N5 -0.6(5) . . . . ? C13 N6 C4 N5 171.2(4) . . . . ? N5 N4 C5 N6 -1.5(4) . . . . ? C3 N4 C5 N6 176.5(3) . . . . ? N5 N4 C5 Pd1 174.1(2) . . . . ? C3 N4 C5 Pd1 -7.9(5) . . . . ? C4 N6 C5 N4 1.2(4) . . . . ? C13 N6 C5 N4 -170.2(4) . . . . ? C4 N6 C5 Pd1 -173.3(3) . . . . ? C13 N6 C5 Pd1 15.3(6) . . . . ? C2 Pd1 C5 N4 43.2(3) . . . . ? Br1 Pd1 C5 N4 -25.3(10) . . . . ? Br2 Pd1 C5 N4 -133.9(3) . . . . ? C2 Pd1 C5 N6 -143.0(4) . . . . ? Br1 Pd1 C5 N6 148.5(5) . . . . ? Br2 Pd1 C5 N6 39.9(4) . . . . ? C2 N3 C6 C7 -78.6(9) . . . . ? C1 N3 C6 C7 90.3(8) . . . . ? N3 C6 C7 C8A 31(2) . . . . ? N3 C6 C7 C8B -23(2) . . . . ? C8B C7 C8A C9 -52.7(19) . . . . ? C6 C7 C8A C9 -158.7(13) . . . . ? C8A C7 C8B C9 52.3(17) . . . . ? C6 C7 C8B C9 162.5(13) . . . . ? C7 C8B C9 C8A -44.0(16) . . . . ? C7 C8A C9 C8B 59(2) . . . . ? N4 C3 C10 C11 56.3(4) . . . . ? N1 C3 C10 C11 176.7(3) . . . . ? S1 O1 C11 C10 -177.9(3) . . . . ? C3 C10 C11 O1 -82.0(4) . . . . ? C4 N6 C13 C14 -100.7(5) . . . . ? C5 N6 C13 C14 69.5(6) . . . . ? N6 C13 C14 C15 162.6(6) . . . . ? C13 C14 C15 C16 52.3(10) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.625 _refine_diff_density_min -0.943 _refine_diff_density_rms 0.110