# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Dr XiaoMing Ren' _publ_contact_author_email xmren@njut.edu.cn _publ_section_title ; Observation of metal ion dependent packing structures and magnetic behaviors of metal-bis-1, 2-dithiolene complexes ; _publ_author_name 'XiaoMing Ren' # Attachment '- 1.cif' data_1 _database_code_depnum_ccdc_archive 'CCDC 775007' #TrackingRef '- 1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H11 Br F N6 Pt S4' _chemical_formula_weight 757.59 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 '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 5.3139(13) _cell_length_b 13.267(3) _cell_length_c 17.945(5) _cell_angle_alpha 105.715(5) _cell_angle_beta 97.314(5) _cell_angle_gamma 100.347(5) _cell_volume 1177.2(5) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 3478 _cell_measurement_theta_min 2.3021 _cell_measurement_theta_max 27.3814 _exptl_crystal_description stick-shaped _exptl_crystal_colour dark-green _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.137 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 718 _exptl_absorpt_coefficient_mu 8.042 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.220 _exptl_absorpt_correction_T_max 0.312 _exptl_absorpt_process_details 'SADABS(Bruker, 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 7149 _diffrn_reflns_av_R_equivalents 0.0245 _diffrn_reflns_av_sigmaI/netI 0.0474 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.20 _diffrn_reflns_theta_max 26.00 _reflns_number_total 4575 _reflns_number_gt 3962 _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 ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1407P)^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_number_reflns 4575 _refine_ls_number_parameters 298 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0550 _refine_ls_R_factor_gt 0.0412 _refine_ls_wR_factor_ref 0.1826 _refine_ls_wR_factor_gt 0.1219 _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_restrained_S_all 1.058 _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 Pt1 Pt 0.83890(6) 0.78324(3) 0.67571(2) 0.03120(19) Uani 1 1 d . . . S1 S 1.0980(5) 0.8123(2) 0.58928(16) 0.0376(6) Uani 1 1 d . . . S2 S 1.0682(5) 0.9368(2) 0.76651(15) 0.0363(5) Uani 1 1 d . . . S3 S 0.5950(5) 0.6303(2) 0.58675(16) 0.0373(6) Uani 1 1 d . . . S4 S 0.5960(5) 0.7575(2) 0.76525(16) 0.0388(6) Uani 1 1 d . . . Br1 Br 0.7772(3) 0.15533(13) 1.06938(9) 0.0699(4) Uani 1 1 d . . . F1 F 0.7126(14) 0.4596(6) 0.9468(4) 0.0629(19) Uani 1 1 d . . . N1 N 1.689(2) 0.9973(10) 0.5790(7) 0.061(3) Uani 1 1 d . . . N2 N 1.6361(18) 1.1564(8) 0.7942(6) 0.047(2) Uani 1 1 d . . . N3 N 0.013(2) 0.4171(9) 0.5696(6) 0.056(3) Uani 1 1 d . . . N4 N 0.051(2) 0.5674(10) 0.7937(7) 0.067(4) Uani 1 1 d . . . N5 N 0.2850(16) 0.3348(7) 0.7746(5) 0.0369(19) Uani 1 1 d . . . N6 N 0.503(2) 0.2513(8) 0.5601(6) 0.045(2) Uani 1 1 d . . . H6A H 0.4081 0.1993 0.5214 0.054 Uiso 1 1 calc R . . H6B H 0.6425 0.2892 0.5535 0.054 Uiso 1 1 calc R . . C1 C 1.516(2) 0.9703(9) 0.6059(7) 0.041(2) Uani 1 1 d . . . C2 C 1.316(2) 0.9287(8) 0.6425(7) 0.034(2) Uani 1 1 d . . . C3 C 1.3003(19) 0.9856(9) 0.7180(6) 0.037(2) Uani 1 1 d . . . C4 C 1.486(2) 1.0792(8) 0.7606(6) 0.034(2) Uani 1 1 d . . . C5 C 0.168(2) 0.4945(9) 0.5999(6) 0.041(2) Uani 1 1 d . . . C6 C 0.364(2) 0.5907(8) 0.6383(7) 0.037(2) Uani 1 1 d . . . C7 C 0.3718(19) 0.6428(8) 0.7156(7) 0.034(2) Uani 1 1 d . . . C8 C 0.192(2) 0.6010(8) 0.7588(6) 0.036(2) Uani 1 1 d . . . C9 C 0.499(2) 0.3938(10) 0.7601(7) 0.047(3) Uani 1 1 d . . . H9A H 0.5920 0.4559 0.7990 0.056 Uiso 1 1 calc R . . C10 C 0.584(2) 0.3646(8) 0.6896(6) 0.036(2) Uani 1 1 d . . . H10A H 0.7353 0.4044 0.6817 0.043 Uiso 1 1 calc R . . C11 C 0.4344(19) 0.2727(8) 0.6292(6) 0.034(2) Uani 1 1 d . . . C12 C 0.214(2) 0.2161(8) 0.6450(6) 0.040(2) Uani 1 1 d . . . H12A H 0.1131 0.1556 0.6062 0.048 Uiso 1 1 calc R . . C13 C 0.142(2) 0.2473(9) 0.7170(7) 0.039(2) Uani 1 1 d . . . H13A H -0.0081 0.2079 0.7263 0.046 Uiso 1 1 calc R . . C14 C 0.212(2) 0.3657(10) 0.8541(6) 0.043(3) Uani 1 1 d . . . H14A H 0.0250 0.3425 0.8489 0.052 Uiso 1 1 calc R . . H14B H 0.2591 0.4432 0.8765 0.052 Uiso 1 1 calc R . . C15 C 0.350(2) 0.3144(8) 0.9089(6) 0.037(2) Uani 1 1 d . . . C16 C 0.592(2) 0.3635(8) 0.9516(6) 0.040(2) Uani 1 1 d . . . C17 C 0.722(2) 0.3176(9) 1.0008(6) 0.042(2) Uani 1 1 d . . . H17A H 0.8854 0.3531 1.0307 0.051 Uiso 1 1 calc R . . C18 C 0.605(2) 0.2194(10) 1.0046(6) 0.047(3) Uani 1 1 d . . . C19 C 0.357(2) 0.1725(10) 0.9632(7) 0.051(3) Uani 1 1 d . . . H19A H 0.2750 0.1065 0.9670 0.061 Uiso 1 1 calc R . . C20 C 0.232(2) 0.2187(9) 0.9175(7) 0.044(3) Uani 1 1 d . . . H20A H 0.0621 0.1857 0.8913 0.052 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 Pt1 0.0269(2) 0.0286(3) 0.0360(3) 0.01107(17) 0.00296(16) 0.00099(16) S1 0.0342(13) 0.0339(13) 0.0387(13) 0.0057(10) 0.0080(10) 0.0000(10) S2 0.0364(13) 0.0330(13) 0.0363(13) 0.0102(10) 0.0055(10) 0.0006(10) S3 0.0401(14) 0.0309(13) 0.0373(13) 0.0099(10) 0.0088(11) -0.0014(10) S4 0.0378(13) 0.0359(13) 0.0378(13) 0.0085(11) 0.0075(11) -0.0007(10) Br1 0.0873(11) 0.0801(10) 0.0530(8) 0.0304(7) 0.0048(7) 0.0351(8) F1 0.055(4) 0.050(4) 0.068(5) 0.008(4) 0.002(4) -0.005(3) N1 0.060(7) 0.062(7) 0.056(6) 0.017(5) 0.021(5) -0.004(5) N2 0.037(5) 0.042(5) 0.050(6) -0.001(4) 0.010(4) 0.002(4) N3 0.061(6) 0.053(6) 0.039(5) 0.010(5) 0.011(5) -0.019(5) N4 0.062(7) 0.068(7) 0.045(6) -0.005(5) 0.018(5) -0.021(6) N5 0.032(4) 0.051(5) 0.032(4) 0.018(4) 0.005(3) 0.014(4) N6 0.057(6) 0.038(5) 0.044(5) 0.020(4) 0.013(4) 0.007(4) C1 0.043(6) 0.035(5) 0.046(6) 0.015(5) 0.004(5) 0.010(5) C2 0.030(5) 0.031(5) 0.045(6) 0.019(4) 0.005(4) 0.006(4) C3 0.023(4) 0.043(6) 0.042(6) 0.014(5) 0.003(4) -0.004(4) C4 0.037(5) 0.033(5) 0.032(5) 0.010(4) 0.004(4) 0.006(4) C5 0.037(5) 0.048(6) 0.033(5) 0.012(5) 0.008(4) -0.008(5) C6 0.033(5) 0.034(5) 0.044(6) 0.017(4) 0.006(4) 0.005(4) C7 0.030(5) 0.023(5) 0.053(6) 0.018(4) 0.011(4) 0.005(4) C8 0.044(6) 0.030(5) 0.038(5) 0.019(4) 0.006(5) 0.006(4) C9 0.038(6) 0.049(6) 0.037(6) -0.004(5) 0.003(5) -0.003(5) C10 0.035(5) 0.031(5) 0.043(6) 0.020(4) 0.002(4) 0.001(4) C11 0.034(5) 0.033(5) 0.037(5) 0.011(4) 0.006(4) 0.015(4) C12 0.043(6) 0.036(5) 0.039(5) 0.018(4) 0.002(4) -0.004(4) C13 0.029(5) 0.040(6) 0.051(6) 0.020(5) 0.007(4) 0.009(4) C14 0.036(5) 0.064(7) 0.030(5) 0.005(5) 0.009(4) 0.023(5) C15 0.039(5) 0.044(6) 0.030(5) 0.013(4) 0.014(4) 0.012(4) C16 0.042(6) 0.030(5) 0.046(6) 0.006(4) 0.014(5) 0.009(4) C17 0.043(6) 0.047(6) 0.029(5) 0.007(4) -0.001(4) 0.002(5) C18 0.057(7) 0.061(7) 0.024(5) 0.014(5) 0.010(5) 0.009(5) C19 0.057(7) 0.045(6) 0.047(6) 0.012(5) 0.012(5) 0.004(5) C20 0.040(6) 0.049(6) 0.041(6) 0.016(5) 0.008(5) 0.004(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 Pt1 S4 2.243(3) . ? Pt1 S2 2.257(3) . ? Pt1 S3 2.262(3) . ? Pt1 S1 2.264(3) . ? S1 C2 1.708(11) . ? S2 C3 1.729(10) . ? S3 C6 1.720(11) . ? S4 C7 1.694(10) . ? Br1 C18 1.859(12) . ? F1 C16 1.351(12) . ? N1 C1 1.140(16) . ? N2 C4 1.139(14) . ? N3 C5 1.144(15) . ? N4 C8 1.140(15) . ? N5 C13 1.352(14) . ? N5 C9 1.358(14) . ? N5 C14 1.495(12) . ? N6 C11 1.308(14) . ? N6 H6A 0.8600 . ? N6 H6B 0.8600 . ? C1 C2 1.423(16) . ? C2 C3 1.383(16) . ? C3 C4 1.398(14) . ? C5 C6 1.433(15) . ? C6 C7 1.364(16) . ? C7 C8 1.435(14) . ? C9 C10 1.376(15) . ? C9 H9A 0.9300 . ? C10 C11 1.417(14) . ? C10 H10A 0.9300 . ? C11 C12 1.377(15) . ? C12 C13 1.374(16) . ? C12 H12A 0.9300 . ? C13 H13A 0.9300 . ? C14 C15 1.525(15) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 C16 1.358(15) . ? C15 C20 1.369(15) . ? C16 C17 1.384(15) . ? C17 C18 1.361(15) . ? C17 H17A 0.9300 . ? C18 C19 1.370(17) . ? C19 C20 1.332(17) . ? C19 H19A 0.9300 . ? C20 H20A 0.9300 . ? 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 S4 Pt1 S2 87.97(9) . . ? S4 Pt1 S3 90.13(9) . . ? S2 Pt1 S3 177.76(9) . . ? S4 Pt1 S1 177.72(9) . . ? S2 Pt1 S1 90.14(9) . . ? S3 Pt1 S1 91.78(9) . . ? C2 S1 Pt1 102.8(4) . . ? C3 S2 Pt1 103.1(4) . . ? C6 S3 Pt1 101.8(4) . . ? C7 S4 Pt1 103.3(4) . . ? C13 N5 C9 119.4(9) . . ? C13 N5 C14 120.6(9) . . ? C9 N5 C14 120.0(9) . . ? C11 N6 H6A 120.0 . . ? C11 N6 H6B 120.0 . . ? H6A N6 H6B 120.0 . . ? N1 C1 C2 173.4(13) . . ? C3 C2 C1 119.1(9) . . ? C3 C2 S1 122.7(8) . . ? C1 C2 S1 118.2(9) . . ? C2 C3 C4 121.1(9) . . ? C2 C3 S2 121.1(8) . . ? C4 C3 S2 117.5(8) . . ? N2 C4 C3 178.6(12) . . ? N3 C5 C6 179.3(14) . . ? C7 C6 C5 119.0(9) . . ? C7 C6 S3 122.6(8) . . ? C5 C6 S3 118.3(8) . . ? C6 C7 C8 120.9(9) . . ? C6 C7 S4 122.0(8) . . ? C8 C7 S4 117.1(8) . . ? N4 C8 C7 179.2(13) . . ? N5 C9 C10 122.1(10) . . ? N5 C9 H9A 119.0 . . ? C10 C9 H9A 119.0 . . ? C9 C10 C11 118.6(9) . . ? C9 C10 H10A 120.7 . . ? C11 C10 H10A 120.7 . . ? N6 C11 C12 123.8(10) . . ? N6 C11 C10 118.1(10) . . ? C12 C11 C10 118.0(9) . . ? C13 C12 C11 121.2(10) . . ? C13 C12 H12A 119.4 . . ? C11 C12 H12A 119.4 . . ? N5 C13 C12 120.7(10) . . ? N5 C13 H13A 119.6 . . ? C12 C13 H13A 119.6 . . ? N5 C14 C15 110.8(8) . . ? N5 C14 H14A 109.5 . . ? C15 C14 H14A 109.5 . . ? N5 C14 H14B 109.5 . . ? C15 C14 H14B 109.5 . . ? H14A C14 H14B 108.1 . . ? C16 C15 C20 118.2(10) . . ? C16 C15 C14 120.7(10) . . ? C20 C15 C14 121.1(10) . . ? F1 C16 C15 120.2(10) . . ? F1 C16 C17 118.2(10) . . ? C15 C16 C17 121.6(10) . . ? C18 C17 C16 118.8(10) . . ? C18 C17 H17A 120.6 . . ? C16 C17 H17A 120.6 . . ? C17 C18 C19 118.8(11) . . ? C17 C18 Br1 119.6(9) . . ? C19 C18 Br1 121.5(9) . . ? C20 C19 C18 121.8(12) . . ? C20 C19 H19A 119.1 . . ? C18 C19 H19A 119.1 . . ? C19 C20 C15 120.7(11) . . ? C19 C20 H20A 119.7 . . ? C15 C20 H20A 119.7 . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 2.289 _refine_diff_density_min -2.202 _refine_diff_density_rms 0.404 # Attachment '- 2.cif' data_x _database_code_depnum_ccdc_archive 'CCDC 775221' #TrackingRef '- 2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H11 Br F N6 Pd S4' _chemical_formula_weight 668.90 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.5200(15) _cell_length_b 11.804(2) _cell_length_c 14.435(3) _cell_angle_alpha 68.52(3) _cell_angle_beta 85.10(3) _cell_angle_gamma 87.31(3) _cell_volume 1187.8(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4295 _cell_measurement_theta_min 10 _cell_measurement_theta_max 13 _exptl_crystal_description Purple _exptl_crystal_colour Rod _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.870 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 654 _exptl_absorpt_coefficient_mu 2.845 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.6000 _exptl_absorpt_correction_T_max 0.7640 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius cad4' _diffrn_measurement_method \w/2\q _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 200 _diffrn_standards_interval_time 2h _diffrn_standards_decay_% 1 _diffrn_reflns_number 4654 _diffrn_reflns_av_R_equivalents 0.0299 _diffrn_reflns_av_sigmaI/netI 0.0528 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.52 _diffrn_reflns_theta_max 25.26 _reflns_number_total 4295 _reflns_number_gt 3112 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CAD4 EXPRESS(Enraf-Nonius,1994)' _computing_cell_refinement 'CAD4 EXPRESS' _computing_data_reduction 'XCAD4(Harms & Wocadlo,1995)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0660P)^2^+1.4324P] 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 4295 _refine_ls_number_parameters 298 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0733 _refine_ls_R_factor_gt 0.0447 _refine_ls_wR_factor_ref 0.1178 _refine_ls_wR_factor_gt 0.1024 _refine_ls_goodness_of_fit_ref 0.923 _refine_ls_restrained_S_all 0.923 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd Pd 0.21881(6) 0.95510(4) 0.50526(3) 0.03511(15) Uani 1 1 d . . . S1 S 0.2779(2) 1.05194(15) 0.33886(11) 0.0452(4) Uani 1 1 d . . . S2 S 0.2893(2) 1.12580(14) 0.53081(11) 0.0415(4) Uani 1 1 d . . . S3 S 0.1510(2) 0.78452(14) 0.47813(11) 0.0425(4) Uani 1 1 d . . . S4 S 0.1668(2) 0.85588(14) 0.67254(11) 0.0424(4) Uani 1 1 d . . . Br1 Br -0.08443(11) -0.17228(7) 0.94855(7) 0.0797(3) Uani 1 1 d . . . F1 F 0.5314(5) 0.0350(4) 0.8560(3) 0.0736(12) Uani 1 1 d . . . N1 N 0.4655(8) 1.3367(5) 0.1568(4) 0.0653(17) Uani 1 1 d . . . N2 N 0.4600(9) 1.4344(6) 0.3953(5) 0.0740(19) Uani 1 1 d . . . N3 N 0.0524(9) 0.4587(6) 0.6214(5) 0.0681(17) Uani 1 1 d . . . N4 N 0.0758(8) 0.5474(5) 0.8562(4) 0.0610(16) Uani 1 1 d . . . N5 N 0.5028(6) 0.2996(4) 0.7745(3) 0.0392(11) Uani 1 1 d . . . N6 N 0.7317(7) 0.4079(5) 0.9747(4) 0.0515(14) Uani 1 1 d . . . H6A H 0.8448 0.4192 0.9697 0.062 Uiso 1 1 calc R . . H6B H 0.6661 0.4168 1.0235 0.062 Uiso 1 1 calc R . . C1 C 0.4123(8) 1.2725(6) 0.2340(5) 0.0487(16) Uani 1 1 d . . . C2 C 0.3489(7) 1.1909(5) 0.3306(4) 0.0405(14) Uani 1 1 d . . . C4 C 0.4126(9) 1.3412(6) 0.4025(5) 0.0512(16) Uani 1 1 d . . . C3 C 0.3516(7) 1.2238(5) 0.4134(4) 0.0386(13) Uani 1 1 d . . . C5 C 0.0812(9) 0.5570(6) 0.6088(4) 0.0485(16) Uani 1 1 d . . . C6 C 0.1165(7) 0.6800(5) 0.5974(4) 0.0391(14) Uani 1 1 d . . . C8 C 0.0961(8) 0.6199(6) 0.7783(5) 0.0442(15) Uani 1 1 d . . . C7 C 0.1223(7) 0.7113(5) 0.6794(4) 0.0386(13) Uani 1 1 d . . . C9 C 0.6770(8) 0.3242(6) 0.7628(4) 0.0451(15) Uani 1 1 d . . . H9A H 0.7450 0.3154 0.7089 0.054 Uiso 1 1 calc R . . C10 C 0.7562(8) 0.3608(6) 0.8259(4) 0.0465(15) Uani 1 1 d . . . H10A H 0.8780 0.3759 0.8157 0.056 Uiso 1 1 calc R . . C11 C 0.6585(8) 0.3769(5) 0.9073(4) 0.0385(13) Uani 1 1 d . . . C12 C 0.4722(8) 0.3567(6) 0.9154(5) 0.0507(16) Uani 1 1 d . . . H12A H 0.3997 0.3683 0.9669 0.061 Uiso 1 1 calc R . . C13 C 0.4012(8) 0.3210(6) 0.8488(5) 0.0496(16) Uani 1 1 d . . . H13A H 0.2785 0.3105 0.8537 0.060 Uiso 1 1 calc R . . C14 C 0.4197(8) 0.2505(6) 0.7084(4) 0.0443(15) Uani 1 1 d . . . H14A H 0.5123 0.2217 0.6710 0.053 Uiso 1 1 calc R . . H14B H 0.3526 0.3149 0.6612 0.053 Uiso 1 1 calc R . . C15 C 0.2968(7) 0.1472(5) 0.7672(4) 0.0363(13) Uani 1 1 d . . . C16 C 0.3551(8) 0.0442(6) 0.8381(5) 0.0474(15) Uani 1 1 d . . . C17 C 0.2493(9) -0.0524(6) 0.8932(5) 0.0553(17) Uani 1 1 d . . . H17A H 0.2966 -0.1223 0.9396 0.066 Uiso 1 1 calc R . . C18 C 0.0708(8) -0.0422(6) 0.8772(5) 0.0473(15) Uani 1 1 d . . . C19 C 0.0037(8) 0.0589(6) 0.8075(5) 0.0472(15) Uani 1 1 d . . . H19A H -0.1171 0.0644 0.7968 0.057 Uiso 1 1 calc R . . C20 C 0.1151(7) 0.1537(5) 0.7524(4) 0.0410(14) Uani 1 1 d . . . H20A H 0.0684 0.2227 0.7048 0.049 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 Pd 0.0291(2) 0.0389(3) 0.0348(3) -0.01070(19) 0.00063(17) -0.00413(18) S1 0.0495(9) 0.0489(9) 0.0365(8) -0.0149(7) 0.0026(7) -0.0100(7) S2 0.0400(8) 0.0464(9) 0.0378(8) -0.0148(7) 0.0007(6) -0.0091(7) S3 0.0490(9) 0.0425(9) 0.0357(8) -0.0138(7) -0.0002(7) -0.0064(7) S4 0.0451(9) 0.0442(9) 0.0369(8) -0.0130(7) -0.0009(7) -0.0082(7) Br1 0.0692(5) 0.0614(5) 0.0920(6) -0.0082(4) 0.0089(4) -0.0295(4) F1 0.034(2) 0.076(3) 0.098(3) -0.015(2) -0.014(2) -0.0010(19) N1 0.074(4) 0.067(4) 0.042(3) -0.005(3) 0.009(3) -0.020(3) N2 0.073(4) 0.057(4) 0.086(5) -0.015(4) -0.014(4) -0.016(3) N3 0.081(4) 0.049(4) 0.073(4) -0.021(3) 0.001(3) -0.019(3) N4 0.066(4) 0.066(4) 0.041(3) -0.005(3) -0.007(3) -0.026(3) N5 0.028(2) 0.046(3) 0.046(3) -0.020(2) 0.002(2) -0.011(2) N6 0.044(3) 0.069(4) 0.045(3) -0.024(3) 0.001(2) -0.018(3) C1 0.047(4) 0.053(4) 0.046(4) -0.017(3) -0.004(3) -0.005(3) C2 0.030(3) 0.044(3) 0.040(3) -0.007(3) 0.000(3) -0.002(3) C4 0.044(4) 0.052(4) 0.050(4) -0.009(3) -0.005(3) -0.007(3) C3 0.031(3) 0.035(3) 0.046(3) -0.010(3) 0.000(3) -0.005(2) C5 0.055(4) 0.045(4) 0.041(4) -0.012(3) 0.005(3) -0.010(3) C6 0.032(3) 0.039(3) 0.043(3) -0.010(3) -0.003(3) -0.001(3) C8 0.037(3) 0.050(4) 0.048(4) -0.019(3) -0.006(3) -0.010(3) C7 0.036(3) 0.041(3) 0.035(3) -0.007(3) -0.005(2) -0.004(3) C9 0.036(3) 0.055(4) 0.042(3) -0.017(3) 0.009(3) -0.009(3) C10 0.030(3) 0.062(4) 0.046(4) -0.016(3) 0.001(3) -0.012(3) C11 0.039(3) 0.035(3) 0.036(3) -0.006(3) -0.001(3) -0.008(3) C12 0.037(3) 0.062(4) 0.060(4) -0.033(3) 0.015(3) -0.012(3) C13 0.036(3) 0.065(4) 0.056(4) -0.032(3) 0.011(3) -0.017(3) C14 0.039(3) 0.055(4) 0.040(3) -0.019(3) 0.002(3) -0.010(3) C15 0.028(3) 0.052(4) 0.036(3) -0.025(3) 0.002(2) -0.011(3) C16 0.036(3) 0.055(4) 0.055(4) -0.022(3) -0.009(3) -0.001(3) C17 0.053(4) 0.043(4) 0.060(4) -0.006(3) -0.002(3) -0.004(3) C18 0.042(4) 0.043(4) 0.058(4) -0.020(3) 0.006(3) -0.015(3) C19 0.032(3) 0.053(4) 0.060(4) -0.022(3) -0.011(3) -0.004(3) C20 0.035(3) 0.047(4) 0.041(3) -0.014(3) -0.006(3) -0.003(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 Pd S1 2.2645(17) . ? Pd S2 2.2704(17) . ? Pd S4 2.2729(17) . ? Pd S3 2.2750(17) . ? S1 C2 1.709(6) . ? S2 C3 1.706(6) . ? S3 C6 1.718(6) . ? S4 C7 1.720(6) . ? Br1 C18 1.894(6) . ? F1 C16 1.364(7) . ? N1 C1 1.145(8) . ? N2 C4 1.138(8) . ? N3 C5 1.136(8) . ? N4 C8 1.139(8) . ? N5 C9 1.338(7) . ? N5 C13 1.356(7) . ? N5 C14 1.475(7) . ? N6 C11 1.325(7) . ? N6 H6A 0.8600 . ? N6 H6B 0.8600 . ? C1 C2 1.429(8) . ? C2 C3 1.387(8) . ? C4 C3 1.430(9) . ? C5 C6 1.435(9) . ? C6 C7 1.367(8) . ? C8 C7 1.443(8) . ? C9 C10 1.333(8) . ? C9 H9A 0.9300 . ? C10 C11 1.400(8) . ? C10 H10A 0.9300 . ? C11 C12 1.420(8) . ? C12 C13 1.339(8) . ? C12 H12A 0.9300 . ? C13 H13A 0.9300 . ? C14 C15 1.508(8) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 C16 1.354(8) . ? C15 C20 1.394(8) . ? C16 C17 1.371(8) . ? C17 C18 1.374(9) . ? C17 H17A 0.9300 . ? C18 C19 1.357(9) . ? C19 C20 1.381(8) . ? C19 H19A 0.9300 . ? C20 H20A 0.9300 . ? 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 S1 Pd S2 89.89(6) . . ? S1 Pd S4 178.52(6) . . ? S2 Pd S4 90.25(6) . . ? S1 Pd S3 89.55(6) . . ? S2 Pd S3 179.29(6) . . ? S4 Pd S3 90.30(6) . . ? C2 S1 Pd 102.8(2) . . ? C3 S2 Pd 103.0(2) . . ? C6 S3 Pd 102.4(2) . . ? C7 S4 Pd 101.7(2) . . ? C9 N5 C13 118.8(5) . . ? C9 N5 C14 121.6(5) . . ? C13 N5 C14 119.6(5) . . ? C11 N6 H6A 120.0 . . ? C11 N6 H6B 120.0 . . ? H6A N6 H6B 120.0 . . ? N1 C1 C2 178.9(8) . . ? C3 C2 C1 120.4(6) . . ? C3 C2 S1 122.4(4) . . ? C1 C2 S1 117.1(5) . . ? N2 C4 C3 178.9(8) . . ? C2 C3 C4 120.2(5) . . ? C2 C3 S2 121.9(4) . . ? C4 C3 S2 117.9(5) . . ? N3 C5 C6 177.6(7) . . ? C7 C6 C5 120.4(5) . . ? C7 C6 S3 121.9(5) . . ? C5 C6 S3 117.6(5) . . ? N4 C8 C7 179.7(8) . . ? C6 C7 C8 120.0(5) . . ? C6 C7 S4 123.4(4) . . ? C8 C7 S4 116.5(4) . . ? C10 C9 N5 122.2(6) . . ? C10 C9 H9A 118.9 . . ? N5 C9 H9A 118.9 . . ? C9 C10 C11 120.8(5) . . ? C9 C10 H10A 119.6 . . ? C11 C10 H10A 119.6 . . ? N6 C11 C10 123.4(5) . . ? N6 C11 C12 120.5(6) . . ? C10 C11 C12 116.1(5) . . ? C13 C12 C11 119.8(6) . . ? C13 C12 H12A 120.1 . . ? C11 C12 H12A 120.1 . . ? C12 C13 N5 122.0(6) . . ? C12 C13 H13A 119.0 . . ? N5 C13 H13A 119.0 . . ? N5 C14 C15 111.4(5) . . ? N5 C14 H14A 109.3 . . ? C15 C14 H14A 109.3 . . ? N5 C14 H14B 109.3 . . ? C15 C14 H14B 109.3 . . ? H14A C14 H14B 108.0 . . ? C16 C15 C20 116.2(5) . . ? C16 C15 C14 122.2(5) . . ? C20 C15 C14 121.5(5) . . ? C15 C16 F1 118.1(5) . . ? C15 C16 C17 124.5(6) . . ? F1 C16 C17 117.3(6) . . ? C16 C17 C18 117.5(6) . . ? C16 C17 H17A 121.2 . . ? C18 C17 H17A 121.2 . . ? C19 C18 C17 120.8(6) . . ? C19 C18 Br1 118.8(5) . . ? C17 C18 Br1 120.3(5) . . ? C18 C19 C20 119.9(6) . . ? C18 C19 H19A 120.0 . . ? C20 C19 H19A 120.0 . . ? C19 C20 C15 121.0(6) . . ? C19 C20 H20A 119.5 . . ? C15 C20 H20A 119.5 . . ? 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 S2 Pd S1 C2 2.6(2) . . . . ? S4 Pd S1 C2 -92(2) . . . . ? S3 Pd S1 C2 -177.0(2) . . . . ? S1 Pd S2 C3 -2.0(2) . . . . ? S4 Pd S2 C3 176.6(2) . . . . ? S3 Pd S2 C3 36(5) . . . . ? S1 Pd S3 C6 174.5(2) . . . . ? S2 Pd S3 C6 136(5) . . . . ? S4 Pd S3 C6 -4.0(2) . . . . ? S1 Pd S4 C7 -81(2) . . . . ? S2 Pd S4 C7 -175.9(2) . . . . ? S3 Pd S4 C7 3.7(2) . . . . ? N1 C1 C2 C3 103(41) . . . . ? N1 C1 C2 S1 -75(41) . . . . ? Pd S1 C2 C3 -3.1(5) . . . . ? Pd S1 C2 C1 174.9(4) . . . . ? C1 C2 C3 C4 2.0(9) . . . . ? S1 C2 C3 C4 179.9(4) . . . . ? C1 C2 C3 S2 -176.2(5) . . . . ? S1 C2 C3 S2 1.7(7) . . . . ? N2 C4 C3 C2 165(40) . . . . ? N2 C4 C3 S2 -16(40) . . . . ? Pd S2 C3 C2 0.7(5) . . . . ? Pd S2 C3 C4 -177.5(4) . . . . ? N3 C5 C6 C7 4(18) . . . . ? N3 C5 C6 S3 -176(100) . . . . ? Pd S3 C6 C7 3.8(5) . . . . ? Pd S3 C6 C5 -176.1(4) . . . . ? C5 C6 C7 C8 1.2(9) . . . . ? S3 C6 C7 C8 -178.7(4) . . . . ? C5 C6 C7 S4 179.0(5) . . . . ? S3 C6 C7 S4 -0.8(8) . . . . ? N4 C8 C7 C6 31(100) . . . . ? N4 C8 C7 S4 -147(100) . . . . ? Pd S4 C7 C6 -2.6(5) . . . . ? Pd S4 C7 C8 175.3(4) . . . . ? C13 N5 C9 C10 4.8(9) . . . . ? C14 N5 C9 C10 -175.4(6) . . . . ? N5 C9 C10 C11 -0.9(10) . . . . ? C9 C10 C11 N6 176.9(6) . . . . ? C9 C10 C11 C12 -2.4(9) . . . . ? N6 C11 C12 C13 -177.5(6) . . . . ? C10 C11 C12 C13 1.8(9) . . . . ? C11 C12 C13 N5 2.0(10) . . . . ? C9 N5 C13 C12 -5.4(10) . . . . ? C14 N5 C13 C12 174.9(6) . . . . ? C9 N5 C14 C15 135.2(6) . . . . ? C13 N5 C14 C15 -45.0(7) . . . . ? N5 C14 C15 C16 -59.7(7) . . . . ? N5 C14 C15 C20 119.2(6) . . . . ? C20 C15 C16 F1 -178.9(5) . . . . ? C14 C15 C16 F1 0.0(9) . . . . ? C20 C15 C16 C17 1.4(10) . . . . ? C14 C15 C16 C17 -179.6(6) . . . . ? C15 C16 C17 C18 -2.1(11) . . . . ? F1 C16 C17 C18 178.3(6) . . . . ? C16 C17 C18 C19 1.7(10) . . . . ? C16 C17 C18 Br1 179.0(5) . . . . ? C17 C18 C19 C20 -0.8(10) . . . . ? Br1 C18 C19 C20 -178.2(5) . . . . ? C18 C19 C20 C15 0.1(9) . . . . ? C16 C15 C20 C19 -0.4(9) . . . . ? C14 C15 C20 C19 -179.3(5) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.26 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.447 _refine_diff_density_min -1.013 _refine_diff_density_rms 0.102