Supplementary Material (ESI) for Dalton Transactions This journal is (C) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'M. Hosseini' _publ_contact_author_address ; Laboratoire de Chimie de Coordination Organique Universite Louis Pasteur 4 rue Blaise Pascal Strasbourg 67000 FRANCE ; _publ_contact_author_email HOSSEINI@CHIMIE.U-STRASBG.FR _publ_section_title ; Molecular tectonics: design and generation of charge assisted H bonded hybrid molecular networks based on amidinium cations and thio- or isothio-cyanatometallates ; loop_ _publ_author_name 'M. Hosseini' 'Sylvie Ferlay' 'Nathalie Kyritsakas' 'G. Marinescu' # Attachment '1-_HgSCN_4.cif' data_3 _database_code_depnum_ccdc_archive 'CCDC 663025' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C14 H20 N4, C4 Hg N4 S4' _chemical_formula_sum 'C18 H20 Hg N8 S4' _chemical_formula_weight 677.25 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Hg Hg -2.3894 9.2266 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/c _symmetry_space_group_name_Hall '-P 2ybc' 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 7.18500(10) _cell_length_b 12.6540(2) _cell_length_c 26.1910(6) _cell_angle_alpha 90.00 _cell_angle_beta 95.7000(8) _cell_angle_gamma 90.00 _cell_volume 2369.49(7) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 6089 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 30.034 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.898 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1312 _exptl_absorpt_coefficient_mu 6.871 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4927 _exptl_absorpt_correction_T_max 0.6094 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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_% ? _diffrn_reflns_number 12059 _diffrn_reflns_av_R_equivalents 0.0706 _diffrn_reflns_av_sigmaI/netI 0.1331 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 2.84 _diffrn_reflns_theta_max 30.04 _reflns_number_total 6889 _reflns_number_gt 3654 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _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^)+(0.0128P)^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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6889 _refine_ls_number_parameters 280 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1329 _refine_ls_R_factor_gt 0.0492 _refine_ls_wR_factor_ref 0.0869 _refine_ls_wR_factor_gt 0.0706 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.030 _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 -0.1380(8) 0.1884(4) 0.8959(2) 0.0227(13) Uani 1 1 d . . . N1 N -0.3024(7) 0.1754(3) 0.86921(18) 0.0267(12) Uani 1 1 d . . . H1 H -0.3175 0.1982 0.8373 0.032 Uiso 1 1 calc R . . C2 C -0.4597(8) 0.1248(4) 0.8906(2) 0.0322(15) Uani 1 1 d . . . H2A H -0.5402 0.0890 0.8629 0.039 Uiso 1 1 calc R . . H2B H -0.5359 0.1786 0.9063 0.039 Uiso 1 1 calc R . . C3 C -0.3875(8) 0.0460(4) 0.9300(2) 0.0337(16) Uani 1 1 d . . . H3A H -0.3281 -0.0134 0.9131 0.040 Uiso 1 1 calc R . . H3B H -0.4930 0.0173 0.9473 0.040 Uiso 1 1 calc R . . C4 C -0.2470(8) 0.0957(4) 0.9693(2) 0.0307(15) Uani 1 1 d . . . H4A H -0.3112 0.1451 0.9911 0.037 Uiso 1 1 calc R . . H4B H -0.1854 0.0403 0.9916 0.037 Uiso 1 1 calc R . . N2 N -0.1062(7) 0.1531(3) 0.94327(18) 0.0278(12) Uani 1 1 d . . . H2 H 0.0043 0.1645 0.9600 0.033 Uiso 1 1 calc R . . C5 C 0.0114(8) 0.2459(4) 0.8732(2) 0.0219(13) Uani 1 1 d . . . C6 C 0.1050(8) 0.3281(4) 0.9010(2) 0.0255(14) Uani 1 1 d . . . H6 H 0.0728 0.3452 0.9344 0.031 Uiso 1 1 calc R . . C7 C 0.2438(8) 0.3843(4) 0.8802(2) 0.0256(14) Uani 1 1 d . . . H7 H 0.3047 0.4410 0.8989 0.031 Uiso 1 1 calc R . . C8 C 0.2945(8) 0.3581(4) 0.8321(2) 0.0219(13) Uani 1 1 d . . . C9 C 0.2018(8) 0.2763(4) 0.8038(2) 0.0236(13) Uani 1 1 d . . . H9 H 0.2334 0.2595 0.7704 0.028 Uiso 1 1 calc R . . C10 C 0.0641(8) 0.2205(4) 0.8252(2) 0.0238(13) Uani 1 1 d . . . H10 H 0.0041 0.1634 0.8067 0.029 Uiso 1 1 calc R . . C11 C 0.4508(8) 0.4151(4) 0.8108(2) 0.0211(13) Uani 1 1 d . . . N3 N 0.5908(7) 0.4480(3) 0.84264(18) 0.0276(12) Uani 1 1 d . . . H3 H 0.5890 0.4360 0.8757 0.033 Uiso 1 1 calc R . . C12 C 0.7502(8) 0.5041(4) 0.8249(2) 0.0303(15) Uani 1 1 d . . . H12A H 0.8630 0.4928 0.8492 0.036 Uiso 1 1 calc R . . H12B H 0.7239 0.5809 0.8228 0.036 Uiso 1 1 calc R . . C13 C 0.7827(9) 0.4619(4) 0.7723(2) 0.0328(16) Uani 1 1 d . . . H13A H 0.8222 0.3870 0.7752 0.039 Uiso 1 1 calc R . . H13B H 0.8838 0.5026 0.7583 0.039 Uiso 1 1 calc R . . C14 C 0.6045(9) 0.4706(4) 0.7362(2) 0.0302(15) Uani 1 1 d . . . H14A H 0.5831 0.5453 0.7259 0.036 Uiso 1 1 calc R . . H14B H 0.6170 0.4287 0.7048 0.036 Uiso 1 1 calc R . . N4 N 0.4464(6) 0.4320(3) 0.76145(18) 0.0235(11) Uani 1 1 d . . . H4 H 0.3411 0.4192 0.7423 0.028 Uiso 1 1 calc R . . Hg1 Hg 0.26826(4) 0.735235(16) 0.900339(9) 0.03246(9) Uani 1 1 d . . . S1 S 0.1433(3) 0.64777(12) 0.81508(6) 0.0409(5) Uani 1 1 d . . . C15 C 0.2915(8) 0.6832(4) 0.7741(2) 0.0234(14) Uani 1 1 d . . . N5 N 0.3918(7) 0.7057(3) 0.74363(19) 0.0340(13) Uani 1 1 d . . . S2 S 0.6154(3) 0.71745(16) 0.90948(8) 0.0659(6) Uani 1 1 d . . . C16 C 0.6781(9) 0.7813(4) 0.9640(3) 0.0336(16) Uani 1 1 d . . . N6 N 0.7265(7) 0.8265(4) 1.0005(2) 0.0393(14) Uani 1 1 d . . . S3 S 0.0930(2) 0.62150(12) 0.95984(6) 0.0366(4) Uani 1 1 d . . . C17 C 0.2496(9) 0.6139(4) 1.0120(3) 0.0295(16) Uani 1 1 d . . . N7 N 0.3432(8) 0.6100(4) 1.0496(2) 0.0434(15) Uani 1 1 d . . . S4 S 0.1545(3) 0.92643(11) 0.89510(7) 0.0423(5) Uani 1 1 d . . . C18 C -0.0159(10) 0.9193(4) 0.8477(3) 0.0344(16) Uani 1 1 d . . . N8 N -0.1329(9) 0.9178(4) 0.8143(2) 0.0559(18) 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 0.025(4) 0.020(3) 0.023(4) -0.002(3) 0.003(3) -0.003(3) N1 0.028(3) 0.033(3) 0.019(3) 0.007(2) 0.003(2) -0.008(2) C2 0.027(4) 0.043(4) 0.027(4) 0.006(3) 0.004(3) -0.011(3) C3 0.027(4) 0.037(3) 0.038(5) 0.006(3) 0.009(3) -0.010(3) C4 0.037(4) 0.033(3) 0.023(4) 0.005(3) 0.004(3) -0.011(3) N2 0.032(3) 0.028(3) 0.023(3) -0.002(2) 0.000(3) -0.007(2) C5 0.019(3) 0.020(3) 0.027(4) 0.005(2) 0.006(3) 0.000(2) C6 0.027(4) 0.030(3) 0.021(4) 0.000(3) 0.007(3) 0.000(3) C7 0.027(4) 0.020(3) 0.030(4) 0.000(2) 0.005(3) -0.003(3) C8 0.021(3) 0.023(3) 0.022(4) 0.003(2) 0.003(3) 0.001(2) C9 0.025(3) 0.029(3) 0.017(3) 0.000(3) 0.003(3) 0.003(3) C10 0.026(3) 0.023(3) 0.022(3) -0.003(2) 0.001(3) 0.001(3) C11 0.019(3) 0.020(3) 0.024(4) 0.003(2) 0.002(3) 0.005(2) N3 0.026(3) 0.044(3) 0.014(3) 0.005(2) 0.005(2) -0.010(2) C12 0.020(4) 0.037(3) 0.034(4) 0.007(3) 0.003(3) -0.009(3) C13 0.034(4) 0.028(3) 0.040(5) 0.001(3) 0.015(3) -0.005(3) C14 0.040(4) 0.031(3) 0.020(4) 0.007(3) 0.009(3) -0.001(3) N4 0.019(3) 0.028(2) 0.022(3) 0.001(2) -0.002(2) 0.002(2) Hg1 0.03773(16) 0.03639(14) 0.02234(15) 0.00041(11) -0.00156(11) 0.00004(12) S1 0.0488(12) 0.0485(10) 0.0267(11) -0.0087(8) 0.0095(9) -0.0247(9) C15 0.036(4) 0.017(3) 0.017(3) -0.002(2) 0.000(3) 0.006(3) N5 0.043(4) 0.031(3) 0.029(3) -0.005(2) 0.009(3) -0.004(2) S2 0.0369(12) 0.0979(15) 0.0610(15) -0.0456(12) -0.0042(10) 0.0115(11) C16 0.033(4) 0.033(3) 0.034(4) 0.004(3) 0.001(3) 0.005(3) N6 0.042(4) 0.034(3) 0.040(4) 0.001(3) -0.006(3) -0.003(3) S3 0.0370(11) 0.0468(9) 0.0255(10) 0.0031(7) 0.0012(8) -0.0054(8) C17 0.035(4) 0.025(3) 0.031(4) -0.002(3) 0.017(3) -0.003(3) N7 0.054(4) 0.050(3) 0.025(4) 0.010(3) -0.001(3) -0.001(3) S4 0.0509(13) 0.0315(8) 0.0405(12) -0.0031(7) -0.0153(9) 0.0026(8) C18 0.040(5) 0.030(3) 0.033(5) 0.002(3) 0.004(4) 0.008(3) N8 0.059(5) 0.068(4) 0.037(4) -0.001(3) -0.009(4) 0.009(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N2 1.316(7) . ? C1 N1 1.322(7) . ? C1 C5 1.472(7) . ? N1 C2 1.458(6) . ? N1 H1 0.8800 . ? C2 C3 1.492(7) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.505(8) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 N2 1.467(6) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? N2 H2 0.8800 . ? C5 C10 1.385(7) . ? C5 C6 1.404(7) . ? C6 C7 1.380(7) . ? C6 H6 0.9500 . ? C7 C8 1.385(7) . ? C7 H7 0.9500 . ? C8 C9 1.402(7) . ? C8 C11 1.490(7) . ? C9 C10 1.379(7) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C11 N4 1.308(7) . ? C11 N3 1.309(7) . ? N3 C12 1.462(6) . ? N3 H3 0.8800 . ? C12 C13 1.517(7) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.519(8) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 N4 1.455(6) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? N4 H4 0.8800 . ? Hg1 S2 2.492(2) . ? Hg1 S3 2.5447(16) . ? Hg1 S4 2.5531(15) . ? Hg1 S1 2.5728(17) . ? S1 C15 1.648(6) . ? C15 N5 1.162(6) . ? S2 C16 1.664(7) . ? C16 N6 1.139(7) . ? S3 C17 1.684(7) . ? C17 N7 1.138(8) . ? S4 C18 1.657(7) . ? C18 N8 1.152(8) . ? 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 C1 N1 121.3(5) . . ? N2 C1 C5 119.0(5) . . ? N1 C1 C5 119.7(5) . . ? C1 N1 C2 122.5(5) . . ? C1 N1 H1 118.8 . . ? C2 N1 H1 118.8 . . ? N1 C2 C3 109.3(5) . . ? N1 C2 H2A 109.8 . . ? C3 C2 H2A 109.8 . . ? N1 C2 H2B 109.8 . . ? C3 C2 H2B 109.8 . . ? H2A C2 H2B 108.3 . . ? C2 C3 C4 110.9(5) . . ? C2 C3 H3A 109.4 . . ? C4 C3 H3A 109.4 . . ? C2 C3 H3B 109.4 . . ? C4 C3 H3B 109.4 . . ? H3A C3 H3B 108.0 . . ? N2 C4 C3 109.7(5) . . ? N2 C4 H4A 109.7 . . ? C3 C4 H4A 109.7 . . ? N2 C4 H4B 109.7 . . ? C3 C4 H4B 109.7 . . ? H4A C4 H4B 108.2 . . ? C1 N2 C4 122.8(5) . . ? C1 N2 H2 118.6 . . ? C4 N2 H2 118.6 . . ? C10 C5 C6 118.9(5) . . ? C10 C5 C1 121.9(5) . . ? C6 C5 C1 119.2(5) . . ? C7 C6 C5 120.2(5) . . ? C7 C6 H6 119.9 . . ? C5 C6 H6 119.9 . . ? C6 C7 C8 120.1(5) . . ? C6 C7 H7 119.9 . . ? C8 C7 H7 119.9 . . ? C7 C8 C9 120.2(5) . . ? C7 C8 C11 120.0(5) . . ? C9 C8 C11 119.7(5) . . ? C10 C9 C8 119.0(5) . . ? C10 C9 H9 120.5 . . ? C8 C9 H9 120.5 . . ? C9 C10 C5 121.4(5) . . ? C9 C10 H10 119.3 . . ? C5 C10 H10 119.3 . . ? N4 C11 N3 121.3(5) . . ? N4 C11 C8 120.3(5) . . ? N3 C11 C8 118.5(5) . . ? C11 N3 C12 121.9(5) . . ? C11 N3 H3 119.1 . . ? C12 N3 H3 119.1 . . ? N3 C12 C13 108.3(5) . . ? N3 C12 H12A 110.0 . . ? C13 C12 H12A 110.0 . . ? N3 C12 H12B 110.0 . . ? C13 C12 H12B 110.0 . . ? H12A C12 H12B 108.4 . . ? C12 C13 C14 110.1(5) . . ? C12 C13 H13A 109.6 . . ? C14 C13 H13A 109.6 . . ? C12 C13 H13B 109.6 . . ? C14 C13 H13B 109.6 . . ? H13A C13 H13B 108.2 . . ? N4 C14 C13 109.9(5) . . ? N4 C14 H14A 109.7 . . ? C13 C14 H14A 109.7 . . ? N4 C14 H14B 109.7 . . ? C13 C14 H14B 109.7 . . ? H14A C14 H14B 108.2 . . ? C11 N4 C14 124.2(5) . . ? C11 N4 H4 117.9 . . ? C14 N4 H4 117.9 . . ? S2 Hg1 S3 116.20(7) . . ? S2 Hg1 S4 113.75(7) . . ? S3 Hg1 S4 113.18(6) . . ? S2 Hg1 S1 107.71(6) . . ? S3 Hg1 S1 97.87(5) . . ? S4 Hg1 S1 106.18(6) . . ? C15 S1 Hg1 104.8(2) . . ? N5 C15 S1 177.2(6) . . ? C16 S2 Hg1 102.8(2) . . ? N6 C16 S2 177.5(6) . . ? C17 S3 Hg1 101.4(2) . . ? N7 C17 S3 174.2(6) . . ? C18 S4 Hg1 101.4(2) . . ? N8 C18 S4 177.7(6) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 30.04 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.539 _refine_diff_density_min -1.118 _refine_diff_density_rms 0.219 data_q _database_code_depnum_ccdc_archive 'CCDC 663026' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C14 H20 N4, C4 Cu N4 S4' _chemical_formula_sum 'C18 H20 Cu N8 S4' _chemical_formula_weight 540.20 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/c _symmetry_space_group_name_Hall '-P 2ybc' 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 6.2310(2) _cell_length_b 15.8090(4) _cell_length_c 11.6190(4) _cell_angle_alpha 90.00 _cell_angle_beta 96.7880(13) _cell_angle_gamma 90.00 _cell_volume 1136.52(6) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 2985 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 30.034 _exptl_crystal_description prism _exptl_crystal_colour green _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.579 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 554 _exptl_absorpt_coefficient_mu 1.352 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.8333 _exptl_absorpt_correction_T_max 0.8766 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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_% ? _diffrn_reflns_number 6064 _diffrn_reflns_av_R_equivalents 0.0205 _diffrn_reflns_av_sigmaI/netI 0.0441 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.12 _diffrn_reflns_theta_max 30.03 _reflns_number_total 3325 _reflns_number_gt 2684 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _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^)+(0.0363P)^2^+0.4168P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3325 _refine_ls_number_parameters 142 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0458 _refine_ls_R_factor_gt 0.0322 _refine_ls_wR_factor_ref 0.0869 _refine_ls_wR_factor_gt 0.0802 _refine_ls_goodness_of_fit_ref 1.014 _refine_ls_restrained_S_all 1.014 _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 Cu1 Cu 0.0000 0.5000 0.5000 0.02954(10) Uani 1 2 d S . . S2 S -0.07019(7) 0.24509(3) 0.28265(4) 0.02643(11) Uani 1 1 d . . . S1 S 0.61451(7) 0.57256(3) 0.31308(4) 0.02857(11) Uani 1 1 d . . . N1 N 0.5609(2) 0.39812(8) 0.14079(11) 0.0206(3) Uani 1 1 d . . . H1 H 0.5879 0.4440 0.1830 0.025 Uiso 1 1 calc R . . N2 N 0.6274(2) 0.31941(8) -0.01758(11) 0.0214(3) Uani 1 1 d . . . H2 H 0.7071 0.3123 -0.0745 0.026 Uiso 1 1 calc R . . C9 C -0.0485(3) 0.33166(11) 0.36035(14) 0.0236(3) Uani 1 1 d . . . N4 N -0.0315(3) 0.39326(10) 0.41450(14) 0.0333(4) Uani 1 1 d . . . C2 C 0.3985(3) 0.33769(10) 0.17219(14) 0.0230(3) Uani 1 1 d . . . H2A H 0.2899 0.3674 0.2130 0.028 Uiso 1 1 calc R . . H2B H 0.4687 0.2939 0.2247 0.028 Uiso 1 1 calc R . . C6 C 0.8693(3) 0.46092(9) -0.09021(13) 0.0186(3) Uani 1 1 d . . . H6 H 0.7797 0.4341 -0.1514 0.022 Uiso 1 1 calc R . . C5 C 0.8367(2) 0.44551(9) 0.02540(13) 0.0177(3) Uani 1 1 d . . . C7 C 0.9680(3) 0.48479(9) 0.11524(13) 0.0188(3) Uani 1 1 d . . . H7 H 0.9459 0.4744 0.1935 0.023 Uiso 1 1 calc R . . C1 C 0.6673(2) 0.38515(9) 0.05069(13) 0.0175(3) Uani 1 1 d . . . N3 N 0.2355(3) 0.53281(10) 0.40988(14) 0.0341(4) Uani 1 1 d . . . C3 C 0.2891(3) 0.29666(11) 0.06291(15) 0.0256(3) Uani 1 1 d . . . H3A H 0.2059 0.3397 0.0143 0.031 Uiso 1 1 calc R . . H3B H 0.1871 0.2527 0.0834 0.031 Uiso 1 1 calc R . . C4 C 0.4574(3) 0.25709(11) -0.00430(16) 0.0277(4) Uani 1 1 d . . . H4A H 0.5209 0.2068 0.0376 0.033 Uiso 1 1 calc R . . H4B H 0.3892 0.2387 -0.0815 0.033 Uiso 1 1 calc R . . C8 C 0.3945(3) 0.54812(11) 0.37131(14) 0.0260(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 Cu1 0.0394(2) 0.02655(17) 0.02574(17) -0.00329(11) 0.01666(14) -0.00574(12) S2 0.0304(2) 0.0252(2) 0.0254(2) -0.00022(15) 0.01078(17) -0.00188(16) S1 0.0286(2) 0.0323(2) 0.0262(2) -0.00544(16) 0.00898(18) -0.00296(18) N1 0.0228(7) 0.0209(6) 0.0194(6) -0.0008(5) 0.0076(5) -0.0011(5) N2 0.0243(7) 0.0201(6) 0.0221(7) -0.0021(5) 0.0122(5) -0.0030(5) C9 0.0211(8) 0.0276(8) 0.0233(8) 0.0069(6) 0.0076(6) 0.0005(6) N4 0.0400(9) 0.0300(8) 0.0321(8) -0.0018(6) 0.0131(7) -0.0028(7) C2 0.0221(8) 0.0265(8) 0.0220(8) 0.0024(6) 0.0094(6) -0.0022(6) C6 0.0214(7) 0.0193(7) 0.0154(7) 0.0005(5) 0.0034(6) -0.0004(6) C5 0.0186(7) 0.0175(7) 0.0179(7) 0.0016(5) 0.0061(6) 0.0019(5) C7 0.0209(8) 0.0201(7) 0.0164(7) 0.0017(5) 0.0060(6) 0.0012(6) C1 0.0185(7) 0.0183(7) 0.0165(7) 0.0022(5) 0.0047(6) 0.0014(6) N3 0.0390(9) 0.0368(9) 0.0291(8) -0.0019(7) 0.0143(7) -0.0057(7) C3 0.0229(8) 0.0294(8) 0.0258(8) -0.0014(6) 0.0087(7) -0.0051(6) C4 0.0293(9) 0.0237(8) 0.0329(9) -0.0058(6) 0.0144(7) -0.0088(7) C8 0.0343(10) 0.0251(8) 0.0186(8) -0.0038(6) 0.0034(7) -0.0004(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 Cu1 N4 1.9562(16) 3_566 ? Cu1 N4 1.9562(16) . ? Cu1 N3 1.9702(16) . ? Cu1 N3 1.9702(16) 3_566 ? S2 C9 1.6364(18) . ? S1 C8 1.6449(18) . ? N1 C1 1.3196(19) . ? N1 C2 1.469(2) . ? N1 H1 0.8800 . ? N2 C1 1.3132(19) . ? N2 C4 1.468(2) . ? N2 H2 0.8800 . ? C9 N4 1.157(2) . ? C2 C3 1.514(2) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C6 C7 1.385(2) 3_765 ? C6 C5 1.403(2) . ? C6 H6 0.9500 . ? C5 C7 1.394(2) . ? C5 C1 1.478(2) . ? C7 C6 1.385(2) 3_765 ? C7 H7 0.9500 . ? N3 C8 1.160(2) . ? C3 C4 1.515(2) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? 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 N4 Cu1 N4 180.0 3_566 . ? N4 Cu1 N3 90.37(7) 3_566 . ? N4 Cu1 N3 89.63(7) . . ? N4 Cu1 N3 89.63(7) 3_566 3_566 ? N4 Cu1 N3 90.37(7) . 3_566 ? N3 Cu1 N3 180.00(7) . 3_566 ? C1 N1 C2 121.43(13) . . ? C1 N1 H1 119.3 . . ? C2 N1 H1 119.3 . . ? C1 N2 C4 123.71(13) . . ? C1 N2 H2 118.1 . . ? C4 N2 H2 118.1 . . ? N4 C9 S2 179.23(16) . . ? C9 N4 Cu1 177.51(14) . . ? N1 C2 C3 108.99(13) . . ? N1 C2 H2A 109.9 . . ? C3 C2 H2A 109.9 . . ? N1 C2 H2B 109.9 . . ? C3 C2 H2B 109.9 . . ? H2A C2 H2B 108.3 . . ? C7 C6 C5 120.06(14) 3_765 . ? C7 C6 H6 120.0 3_765 . ? C5 C6 H6 120.0 . . ? C7 C5 C6 120.07(14) . . ? C7 C5 C1 120.56(13) . . ? C6 C5 C1 119.34(14) . . ? C6 C7 C5 119.87(14) 3_765 . ? C6 C7 H7 120.1 3_765 . ? C5 C7 H7 120.1 . . ? N2 C1 N1 121.69(14) . . ? N2 C1 C5 118.65(13) . . ? N1 C1 C5 119.66(13) . . ? C8 N3 Cu1 169.69(16) . . ? C2 C3 C4 109.80(14) . . ? C2 C3 H3A 109.7 . . ? C4 C3 H3A 109.7 . . ? C2 C3 H3B 109.7 . . ? C4 C3 H3B 109.7 . . ? H3A C3 H3B 108.2 . . ? N2 C4 C3 109.23(13) . . ? N2 C4 H4A 109.8 . . ? C3 C4 H4A 109.8 . . ? N2 C4 H4B 109.8 . . ? C3 C4 H4B 109.8 . . ? H4A C4 H4B 108.3 . . ? N3 C8 S1 177.69(18) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 30.03 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.319 _refine_diff_density_min -0.519 _refine_diff_density_rms 0.067 # Attachment '1-Pd_SCN_4.cif' data_e659a _database_code_depnum_ccdc_archive 'CCDC 663027' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C14 H20 N4, C4 N4 Pd S4' _chemical_formula_sum 'C18 H20 N8 Pd S4' _chemical_formula_weight 583.06 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.1632(4) _cell_length_b 12.3179(7) _cell_length_c 13.0249(6) _cell_angle_alpha 94.640(2) _cell_angle_beta 96.935(2) _cell_angle_gamma 91.823(2) _cell_volume 1136.11(10) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.704 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 588 _exptl_absorpt_coefficient_mu 1.208 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9095 _exptl_absorpt_correction_T_max 0.9420 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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_% ? _diffrn_reflns_number 29893 _diffrn_reflns_av_R_equivalents 0.0287 _diffrn_reflns_av_sigmaI/netI 0.0303 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.66 _diffrn_reflns_theta_max 30.22 _reflns_number_total 6697 _reflns_number_gt 5343 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _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^)+(0.0420P)^2^+0.2619P] 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 6697 _refine_ls_number_parameters 283 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0377 _refine_ls_R_factor_gt 0.0282 _refine_ls_wR_factor_ref 0.0777 _refine_ls_wR_factor_gt 0.0754 _refine_ls_goodness_of_fit_ref 1.082 _refine_ls_restrained_S_all 1.082 _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 0.2249(3) 0.11171(15) 0.10735(15) 0.0182(4) Uani 1 1 d . . . N1 N 0.2513(2) 0.21680(13) 0.13718(13) 0.0212(3) Uani 1 1 d . . . H1 H 0.3578 0.2500 0.1279 0.025 Uiso 1 1 calc R . . C2 C 0.1100(3) 0.27997(16) 0.18500(17) 0.0249(4) Uani 1 1 d . . . H2A H 0.0277 0.3136 0.1308 0.030 Uiso 1 1 calc R . . H2B H 0.1731 0.3391 0.2343 0.030 Uiso 1 1 calc R . . C3 C -0.0068(3) 0.20661(17) 0.24156(17) 0.0267(4) Uani 1 1 d . . . H3A H -0.1138 0.2469 0.2645 0.032 Uiso 1 1 calc R . . H3B H 0.0709 0.1847 0.3040 0.032 Uiso 1 1 calc R . . C4 C -0.0809(3) 0.10565(17) 0.17248(18) 0.0264(5) Uani 1 1 d . . . H4A H -0.1338 0.0519 0.2148 0.032 Uiso 1 1 calc R . . H4B H -0.1828 0.1253 0.1198 0.032 Uiso 1 1 calc R . . N2 N 0.0710(2) 0.05736(13) 0.12070(13) 0.0193(3) Uani 1 1 d . . . H2 H 0.0581 -0.0119 0.0973 0.023 Uiso 1 1 calc R . . C5 C 0.3700(3) 0.05473(16) 0.05385(15) 0.0188(4) Uani 1 1 d . . . C6 C 0.4548(3) 0.10558(16) -0.02141(16) 0.0212(4) Uani 1 1 d . . . H6 H 0.4238 0.1777 -0.0359 0.025 Uiso 1 1 calc R . . C7 C 0.5847(3) 0.05115(16) -0.07540(16) 0.0210(4) Uani 1 1 d . . . H7 H 0.6424 0.0858 -0.1268 0.025 Uiso 1 1 calc R . . C8 C 0.6736(3) 0.58763(15) 0.38925(15) 0.0181(4) Uani 1 1 d . . . N3 N 0.5184(2) 0.52548(13) 0.36752(13) 0.0207(3) Uani 1 1 d . . . H3 H 0.5179 0.4594 0.3887 0.025 Uiso 1 1 calc R . . C9 C 0.3468(3) 0.56166(17) 0.30958(17) 0.0242(4) Uani 1 1 d . . . H9A H 0.2350 0.5279 0.3342 0.029 Uiso 1 1 calc R . . H9B H 0.3444 0.5384 0.2348 0.029 Uiso 1 1 calc R . . C10 C 0.3407(3) 0.68495(16) 0.32483(17) 0.0252(4) Uani 1 1 d . . . H10A H 0.2354 0.7103 0.2775 0.030 Uiso 1 1 calc R . . H10B H 0.3194 0.7073 0.3971 0.030 Uiso 1 1 calc R . . C11 C 0.5248(3) 0.73616(17) 0.30256(18) 0.0257(4) Uani 1 1 d . . . H11A H 0.5350 0.7251 0.2273 0.031 Uiso 1 1 calc R . . H11B H 0.5284 0.8156 0.3224 0.031 Uiso 1 1 calc R . . N4 N 0.6825(2) 0.68709(13) 0.36093(13) 0.0212(3) Uani 1 1 d . . . H4 H 0.7885 0.7261 0.3779 0.025 Uiso 1 1 calc R . . C12 C 0.8421(3) 0.54305(15) 0.44669(15) 0.0182(4) Uani 1 1 d . . . C13 C 0.8805(3) 0.43324(16) 0.42838(16) 0.0210(4) Uani 1 1 d . . . H13 H 0.7987 0.3876 0.3790 0.025 Uiso 1 1 calc R . . C14 C 1.0364(3) 0.38994(16) 0.48133(16) 0.0214(4) Uani 1 1 d . . . H14 H 1.0606 0.3150 0.4687 0.026 Uiso 1 1 calc R . . Pd1 Pd 0.5000 1.0000 0.5000 0.01732(6) Uani 1 2 d S . . S1 S 0.33940(8) 0.89076(5) 0.60136(5) 0.02993(13) Uani 1 1 d . . . C15 C 0.4740(3) 0.78224(17) 0.60338(16) 0.0233(4) Uani 1 1 d . . . N5 N 0.5585(3) 0.70414(15) 0.60473(16) 0.0322(4) Uani 1 1 d . . . S2 S 0.26554(8) 0.98802(5) 0.35951(4) 0.02878(12) Uani 1 1 d . . . C16 C 0.0816(3) 0.91444(18) 0.38800(19) 0.0316(5) Uani 1 1 d . . . N6 N -0.0489(3) 0.86370(18) 0.4014(2) 0.0459(6) Uani 1 1 d . . . Pd2 Pd 0.0000 0.5000 0.0000 0.01749(6) Uani 1 2 d S . . S3 S 0.27563(9) 0.60954(5) 0.03387(5) 0.03664(15) Uani 1 1 d . . . C17 C 0.3543(3) 0.61987(18) -0.0803(2) 0.0312(5) Uani 1 1 d . . . N7 N 0.4124(3) 0.6328(2) -0.15786(18) 0.0459(6) Uani 1 1 d . . . S4 S -0.13665(10) 0.60755(5) 0.12415(6) 0.04275(17) Uani 1 1 d . . . C18 C -0.0580(3) 0.73595(18) 0.11454(18) 0.0300(5) Uani 1 1 d . . . N8 N -0.0125(3) 0.82521(15) 0.11000(17) 0.0348(5) 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 0.0176(9) 0.0201(9) 0.0167(9) -0.0002(7) 0.0019(7) 0.0011(7) N1 0.0194(8) 0.0187(8) 0.0257(9) -0.0015(7) 0.0066(7) -0.0021(6) C2 0.0268(10) 0.0190(9) 0.0293(11) -0.0018(8) 0.0072(9) 0.0035(8) C3 0.0301(11) 0.0238(10) 0.0267(11) -0.0034(8) 0.0085(9) 0.0036(8) C4 0.0202(10) 0.0272(11) 0.0318(12) -0.0070(9) 0.0098(8) -0.0007(8) N2 0.0182(8) 0.0172(8) 0.0225(8) -0.0047(6) 0.0070(6) -0.0010(6) C5 0.0168(9) 0.0201(9) 0.0194(9) -0.0010(7) 0.0033(7) 0.0007(7) C6 0.0207(9) 0.0193(9) 0.0240(10) 0.0026(8) 0.0040(8) 0.0015(7) C7 0.0199(9) 0.0233(10) 0.0207(10) 0.0049(8) 0.0048(7) 0.0005(8) C8 0.0180(9) 0.0179(9) 0.0178(9) -0.0015(7) 0.0026(7) 0.0008(7) N3 0.0199(8) 0.0160(8) 0.0252(9) 0.0042(7) -0.0027(7) -0.0004(6) C9 0.0203(9) 0.0236(10) 0.0271(11) 0.0039(8) -0.0035(8) -0.0025(8) C10 0.0216(10) 0.0222(10) 0.0304(12) 0.0011(8) -0.0025(8) 0.0037(8) C11 0.0261(10) 0.0202(10) 0.0304(11) 0.0062(8) -0.0019(9) 0.0029(8) N4 0.0196(8) 0.0176(8) 0.0259(9) 0.0031(7) 0.0004(7) -0.0011(6) C12 0.0182(9) 0.0178(9) 0.0190(9) 0.0010(7) 0.0033(7) 0.0014(7) C13 0.0198(9) 0.0180(9) 0.0236(10) -0.0028(8) -0.0004(8) -0.0001(7) C14 0.0211(9) 0.0160(9) 0.0262(11) -0.0015(8) 0.0009(8) 0.0016(7) Pd1 0.01781(10) 0.01452(10) 0.02083(11) 0.00455(8) 0.00542(8) 0.00012(7) S1 0.0272(3) 0.0290(3) 0.0383(3) 0.0150(2) 0.0150(2) 0.0021(2) C15 0.0258(10) 0.0219(10) 0.0220(10) 0.0041(8) 0.0030(8) -0.0093(8) N5 0.0378(11) 0.0231(9) 0.0360(11) 0.0068(8) 0.0045(9) -0.0030(8) S2 0.0269(3) 0.0284(3) 0.0303(3) 0.0090(2) -0.0026(2) -0.0032(2) C16 0.0296(12) 0.0214(10) 0.0418(14) 0.0012(9) -0.0023(10) 0.0001(9) N6 0.0308(11) 0.0390(12) 0.0649(16) 0.0048(11) -0.0021(10) -0.0117(9) Pd2 0.01882(10) 0.01533(10) 0.01879(11) 0.00194(8) 0.00471(8) -0.00218(7) S3 0.0327(3) 0.0459(4) 0.0295(3) -0.0041(3) 0.0066(2) -0.0181(3) C17 0.0268(11) 0.0264(11) 0.0401(14) 0.0009(10) 0.0062(10) -0.0072(9) N7 0.0436(13) 0.0530(14) 0.0424(13) 0.0013(11) 0.0183(10) -0.0180(11) S4 0.0492(4) 0.0290(3) 0.0534(4) -0.0100(3) 0.0317(3) -0.0084(3) C18 0.0307(11) 0.0265(11) 0.0313(12) -0.0038(9) 0.0010(9) 0.0030(9) N8 0.0379(11) 0.0233(10) 0.0420(12) 0.0001(9) 0.0012(9) 0.0015(8) _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 C1 N2 1.308(2) . ? C1 N1 1.322(2) . ? C1 C5 1.484(3) . ? N1 C2 1.463(2) . ? N1 H1 0.8800 . ? C2 C3 1.506(3) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.516(3) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 N2 1.465(2) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? N2 H2 0.8800 . ? C5 C6 1.393(3) . ? C5 C7 1.396(3) 2_655 ? C6 C7 1.389(3) . ? C6 H6 0.9500 . ? C7 C5 1.396(3) 2_655 ? C7 H7 0.9500 . ? C8 N4 1.309(3) . ? C8 N3 1.318(2) . ? C8 C12 1.486(3) . ? N3 C9 1.464(2) . ? N3 H3 0.8800 . ? C9 C10 1.518(3) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C11 1.513(3) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 N4 1.460(3) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? N4 H4 0.8800 . ? C12 C14 1.396(3) 2_766 ? C12 C13 1.396(3) . ? C13 C14 1.385(3) . ? C13 H13 0.9500 . ? C14 C12 1.396(3) 2_766 ? C14 H14 0.9500 . ? Pd1 S2 2.3215(6) 2_676 ? Pd1 S2 2.3215(6) . ? Pd1 S1 2.3308(5) . ? Pd1 S1 2.3308(5) 2_676 ? S1 C15 1.673(2) . ? C15 N5 1.153(3) . ? S2 C16 1.671(3) . ? C16 N6 1.147(3) . ? Pd2 S3 2.3318(6) . ? Pd2 S3 2.3318(6) 2_565 ? Pd2 S4 2.3337(6) . ? Pd2 S4 2.3337(6) 2_565 ? S3 C17 1.665(3) . ? C17 N7 1.159(3) . ? S4 C18 1.682(2) . ? C18 N8 1.145(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 N2 C1 N1 121.66(17) . . ? N2 C1 C5 119.04(16) . . ? N1 C1 C5 119.27(17) . . ? C1 N1 C2 122.46(17) . . ? C1 N1 H1 118.8 . . ? C2 N1 H1 118.8 . . ? N1 C2 C3 109.78(17) . . ? N1 C2 H2A 109.7 . . ? C3 C2 H2A 109.7 . . ? N1 C2 H2B 109.7 . . ? C3 C2 H2B 109.7 . . ? H2A C2 H2B 108.2 . . ? C2 C3 C4 111.09(18) . . ? C2 C3 H3A 109.4 . . ? C4 C3 H3A 109.4 . . ? C2 C3 H3B 109.4 . . ? C4 C3 H3B 109.4 . . ? H3A C3 H3B 108.0 . . ? N2 C4 C3 110.16(17) . . ? N2 C4 H4A 109.6 . . ? C3 C4 H4A 109.6 . . ? N2 C4 H4B 109.6 . . ? C3 C4 H4B 109.6 . . ? H4A C4 H4B 108.1 . . ? C1 N2 C4 123.46(16) . . ? C1 N2 H2 118.3 . . ? C4 N2 H2 118.3 . . ? C6 C5 C7 120.11(17) . 2_655 ? C6 C5 C1 119.62(17) . . ? C7 C5 C1 120.20(18) 2_655 . ? C7 C6 C5 120.17(18) . . ? C7 C6 H6 119.9 . . ? C5 C6 H6 119.9 . . ? C6 C7 C5 119.72(18) . 2_655 ? C6 C7 H7 120.1 . . ? C5 C7 H7 120.1 2_655 . ? N4 C8 N3 121.52(18) . . ? N4 C8 C12 119.54(17) . . ? N3 C8 C12 118.94(17) . . ? C8 N3 C9 122.78(17) . . ? C8 N3 H3 118.6 . . ? C9 N3 H3 118.6 . . ? N3 C9 C10 109.77(16) . . ? N3 C9 H9A 109.7 . . ? C10 C9 H9A 109.7 . . ? N3 C9 H9B 109.7 . . ? C10 C9 H9B 109.7 . . ? H9A C9 H9B 108.2 . . ? C11 C10 C9 109.63(17) . . ? C11 C10 H10A 109.7 . . ? C9 C10 H10A 109.7 . . ? C11 C10 H10B 109.7 . . ? C9 C10 H10B 109.7 . . ? H10A C10 H10B 108.2 . . ? N4 C11 C10 110.03(17) . . ? N4 C11 H11A 109.7 . . ? C10 C11 H11A 109.7 . . ? N4 C11 H11B 109.7 . . ? C10 C11 H11B 109.7 . . ? H11A C11 H11B 108.2 . . ? C8 N4 C11 122.97(17) . . ? C8 N4 H4 118.5 . . ? C11 N4 H4 118.5 . . ? C14 C12 C13 119.43(18) 2_766 . ? C14 C12 C8 120.66(17) 2_766 . ? C13 C12 C8 119.90(17) . . ? C14 C13 C12 120.84(18) . . ? C14 C13 H13 119.6 . . ? C12 C13 H13 119.6 . . ? C13 C14 C12 119.73(17) . 2_766 ? C13 C14 H14 120.1 . . ? C12 C14 H14 120.1 2_766 . ? S2 Pd1 S2 179.999(1) 2_676 . ? S2 Pd1 S1 84.36(2) 2_676 . ? S2 Pd1 S1 95.65(2) . . ? S2 Pd1 S1 95.64(2) 2_676 2_676 ? S2 Pd1 S1 84.36(2) . 2_676 ? S1 Pd1 S1 180.0 . 2_676 ? C15 S1 Pd1 100.52(7) . . ? N5 C15 S1 176.47(19) . . ? C16 S2 Pd1 109.07(9) . . ? N6 C16 S2 175.9(2) . . ? S3 Pd2 S3 180.0 . 2_565 ? S3 Pd2 S4 90.32(2) . . ? S3 Pd2 S4 89.68(2) 2_565 . ? S3 Pd2 S4 89.68(2) . 2_565 ? S3 Pd2 S4 90.32(2) 2_565 2_565 ? S4 Pd2 S4 180.00(3) . 2_565 ? C17 S3 Pd2 106.13(8) . . ? N7 C17 S3 176.3(2) . . ? C18 S4 Pd2 105.49(8) . . ? N8 C18 S4 176.5(2) . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 30.22 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 1.329 _refine_diff_density_min -0.906 _refine_diff_density_rms 0.086