# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_safin96 _database_code_depnum_ccdc_archive 'CCDC 864257' #TrackingRef 'web_deposit_cif_file_0_DamirSafin_1327416754.[PdL2].cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H38 N6 O4 P2 Pd S4' _chemical_formula_sum 'C24 H38 N6 O4 P2 Pd S4' _chemical_formula_weight 771.18 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' P P 0.1023 0.0942 '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' S S 0.1246 0.1234 '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 7.9596(12) _cell_length_b 10.4276(15) _cell_length_c 11.7207(18) _cell_angle_alpha 112.870(9) _cell_angle_beta 94.830(9) _cell_angle_gamma 107.321(6) _cell_volume 833.3(2) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 5000 _cell_measurement_theta_min 2.5 _cell_measurement_theta_max 25.0 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.49 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.537 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 396 _exptl_absorpt_coefficient_mu 0.943 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6552 _exptl_absorpt_correction_T_max 0.9284 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _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 'Siemens CCD three-circle diffractometer' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% ? _diffrn_reflns_number 20545 _diffrn_reflns_av_R_equivalents 0.0493 _diffrn_reflns_av_sigmaI/netI 0.0575 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.75 _diffrn_reflns_theta_max 30.51 _reflns_number_total 5080 _reflns_number_gt 3920 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'SMART (Siemens, 1995)' _computing_cell_refinement 'SMART (Siemens, 1995)' _computing_data_reduction 'SAINT (Siemens, 1995)' _computing_structure_solution 'SHELXS97 (Sheldrick, 2008) ' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008) ' _computing_molecular_graphics 'XP (Sheldrick, 2008)' _computing_publication_material SHELXL97 _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^)+(0.0242P)^2^+0.2479P] 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 5080 _refine_ls_number_parameters 191 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0581 _refine_ls_R_factor_gt 0.0363 _refine_ls_wR_factor_ref 0.0709 _refine_ls_wR_factor_gt 0.0641 _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_restrained_S_all 1.018 _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 1.0000 0.5000 1.0000 0.02063(7) Uani 1 2 d S . . P1 P 0.76361(7) 0.50181(6) 0.76407(5) 0.02111(12) Uani 1 1 d . . . S1 S 0.72202(7) 0.50951(6) 0.93179(5) 0.02470(13) Uani 1 1 d . . . S2 S 0.99180(8) 0.29789(7) 0.82082(5) 0.03054(14) Uani 1 1 d . . . O1 O 0.9378(2) 0.63016(16) 0.77568(14) 0.0257(3) Uani 1 1 d . . . O2 O 0.60875(19) 0.53227(16) 0.70021(14) 0.0247(3) Uani 1 1 d . . . N1 N 0.7765(2) 0.35196(19) 0.66255(16) 0.0242(4) Uani 1 1 d . . . N2 N 0.8554(3) 0.1440(2) 0.58066(17) 0.0243(4) Uani 1 1 d . . . H2 H 0.933(3) 0.107(3) 0.593(2) 0.034(7) Uiso 1 1 d . . . C1 C 0.8611(3) 0.2699(2) 0.68078(19) 0.0222(4) Uani 1 1 d . . . C2 C 0.9648(3) 0.7879(2) 0.8515(2) 0.0291(5) Uani 1 1 d . . . H2A H 0.8811 0.7954 0.9109 0.035 Uiso 1 1 calc R . . C3 C 0.9221(4) 0.8507(3) 0.7616(3) 0.0480(7) Uani 1 1 d . . . H3A H 0.7952 0.7974 0.7157 0.072 Uiso 1 1 calc R . . H3B H 0.9999 0.8386 0.7007 0.072 Uiso 1 1 calc R . . H3C H 0.9433 0.9569 0.8098 0.072 Uiso 1 1 calc R . . C4 C 1.1567(3) 0.8628(3) 0.9270(3) 0.0434(7) Uani 1 1 d . . . H4A H 1.1751 0.8178 0.9842 0.065 Uiso 1 1 calc R . . H4B H 1.1818 0.9694 0.9771 0.065 Uiso 1 1 calc R . . H4C H 1.2385 0.8503 0.8689 0.065 Uiso 1 1 calc R . . C5 C 0.4193(3) 0.4829(3) 0.7079(2) 0.0328(6) Uani 1 1 d . . . H5 H 0.4022 0.4190 0.7543 0.039 Uiso 1 1 calc R . . C6 C 0.3079(4) 0.3913(4) 0.5741(3) 0.0618(9) Uani 1 1 d . . . H6A H 0.3417 0.3040 0.5329 0.093 Uiso 1 1 calc R . . H6B H 0.3298 0.4517 0.5267 0.093 Uiso 1 1 calc R . . H6C H 0.1796 0.3584 0.5755 0.093 Uiso 1 1 calc R . . C7 C 0.3796(4) 0.6183(4) 0.7814(4) 0.0657(10) Uani 1 1 d . . . H7A H 0.4571 0.6708 0.8673 0.099 Uiso 1 1 calc R . . H7B H 0.2526 0.5893 0.7865 0.099 Uiso 1 1 calc R . . H7C H 0.4030 0.6841 0.7389 0.099 Uiso 1 1 calc R . . C11 C 0.7457(3) 0.0699(2) 0.4571(2) 0.0227(4) Uani 1 1 d . . . N12 N 0.7916(2) -0.0401(2) 0.38011(17) 0.0245(4) Uani 1 1 d . . . C13 C 0.6878(3) -0.1220(3) 0.2621(2) 0.0290(5) Uani 1 1 d . . . H13 H 0.7189 -0.2010 0.2058 0.035 Uiso 1 1 calc R . . C14 C 0.5397(3) -0.0996(3) 0.2173(2) 0.0296(5) Uani 1 1 d . . . H14 H 0.4699 -0.1614 0.1329 0.036 Uiso 1 1 calc R . . C15 C 0.4957(3) 0.0151(3) 0.2984(2) 0.0353(6) Uani 1 1 d . . . H15 H 0.3937 0.0338 0.2706 0.042 Uiso 1 1 calc R . . C16 C 0.5998(3) 0.1031(3) 0.4203(2) 0.0337(6) Uani 1 1 d . . . H16 H 0.5725 0.1841 0.4774 0.040 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 0.02330(13) 0.02119(13) 0.01750(12) 0.00471(10) 0.00494(9) 0.01308(10) P1 0.0225(3) 0.0203(3) 0.0219(3) 0.0071(2) 0.0064(2) 0.0119(2) S1 0.0251(3) 0.0303(3) 0.0215(3) 0.0092(2) 0.0072(2) 0.0161(3) S2 0.0374(3) 0.0314(3) 0.0211(3) 0.0020(2) 0.0019(2) 0.0240(3) O1 0.0251(8) 0.0195(8) 0.0319(8) 0.0070(7) 0.0115(7) 0.0117(7) O2 0.0227(8) 0.0293(9) 0.0291(8) 0.0155(7) 0.0087(6) 0.0143(7) N1 0.0312(10) 0.0206(10) 0.0204(9) 0.0060(8) 0.0062(7) 0.0125(8) N2 0.0289(11) 0.0233(10) 0.0195(9) 0.0030(8) 0.0035(7) 0.0166(9) C1 0.0225(11) 0.0233(11) 0.0207(10) 0.0074(9) 0.0077(8) 0.0104(9) C2 0.0299(13) 0.0201(12) 0.0366(13) 0.0074(10) 0.0137(10) 0.0128(10) C3 0.0588(19) 0.0303(15) 0.0578(18) 0.0210(14) 0.0093(15) 0.0186(14) C4 0.0370(15) 0.0272(14) 0.0527(17) 0.0064(13) 0.0046(13) 0.0100(12) C5 0.0235(12) 0.0440(15) 0.0406(14) 0.0256(13) 0.0099(10) 0.0146(11) C6 0.0311(16) 0.090(3) 0.0494(18) 0.0317(18) -0.0025(13) 0.0039(16) C7 0.052(2) 0.072(2) 0.094(3) 0.036(2) 0.0394(19) 0.0449(19) C11 0.0257(12) 0.0195(11) 0.0219(11) 0.0070(9) 0.0058(9) 0.0095(9) N12 0.0281(10) 0.0210(10) 0.0225(9) 0.0051(8) 0.0047(7) 0.0125(8) C13 0.0331(13) 0.0239(12) 0.0255(12) 0.0041(10) 0.0050(10) 0.0135(11) C14 0.0295(13) 0.0245(12) 0.0267(12) 0.0055(10) -0.0012(9) 0.0085(10) C15 0.0338(14) 0.0347(14) 0.0353(13) 0.0096(11) -0.0010(10) 0.0198(12) C16 0.0346(14) 0.0324(14) 0.0298(13) 0.0027(11) 0.0033(10) 0.0221(11) _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 S2 2.3046(7) 2_767 ? Pd1 S2 2.3046(7) . ? Pd1 S1 2.3321(6) 2_767 ? Pd1 S1 2.3322(6) . ? P1 O2 1.5630(14) . ? P1 O1 1.5664(16) . ? P1 N1 1.5933(19) . ? P1 S1 1.9958(8) . ? S2 C1 1.738(2) . ? O1 C2 1.471(3) . ? O2 C5 1.464(3) . ? N1 C1 1.301(3) . ? N2 C1 1.364(3) . ? N2 C11 1.405(3) . ? N2 H2 0.85(3) . ? C2 C4 1.500(3) . ? C2 C3 1.505(3) . ? C2 H2A 1.0000 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 C7 1.483(4) . ? C5 C6 1.502(4) . ? C5 H5 1.0000 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C11 N12 1.328(3) . ? C11 C16 1.388(3) . ? N12 C13 1.339(3) . ? C13 C14 1.369(3) . ? C13 H13 0.9500 . ? C14 C15 1.370(3) . ? C14 H14 0.9500 . ? C15 C16 1.378(3) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S2 Pd1 S2 180.0 2_767 . ? S2 Pd1 S1 97.93(2) 2_767 2_767 ? S2 Pd1 S1 82.07(2) . 2_767 ? S2 Pd1 S1 82.07(2) 2_767 . ? S2 Pd1 S1 97.93(2) . . ? S1 Pd1 S1 180.0 2_767 . ? O2 P1 O1 103.02(8) . . ? O2 P1 N1 107.28(9) . . ? O1 P1 N1 105.52(9) . . ? O2 P1 S1 108.96(6) . . ? O1 P1 S1 113.32(6) . . ? N1 P1 S1 117.62(7) . . ? P1 S1 Pd1 95.86(3) . . ? C1 S2 Pd1 115.05(8) . . ? C2 O1 P1 121.40(14) . . ? C5 O2 P1 125.69(13) . . ? C1 N1 P1 128.52(16) . . ? C1 N2 C11 129.53(18) . . ? C1 N2 H2 115.6(17) . . ? C11 N2 H2 114.8(17) . . ? N1 C1 N2 119.71(19) . . ? N1 C1 S2 128.84(17) . . ? N2 C1 S2 111.43(15) . . ? O1 C2 C4 106.77(18) . . ? O1 C2 C3 107.97(19) . . ? C4 C2 C3 113.6(2) . . ? O1 C2 H2A 109.5 . . ? C4 C2 H2A 109.5 . . ? C3 C2 H2A 109.5 . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C2 C4 H4A 109.5 . . ? C2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? O2 C5 C7 107.4(2) . . ? O2 C5 C6 107.2(2) . . ? C7 C5 C6 114.8(2) . . ? O2 C5 H5 109.1 . . ? C7 C5 H5 109.1 . . ? C6 C5 H5 109.1 . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C5 C7 H7A 109.5 . . ? C5 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C5 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N12 C11 C16 123.3(2) . . ? N12 C11 N2 112.78(18) . . ? C16 C11 N2 123.8(2) . . ? C11 N12 C13 116.74(18) . . ? N12 C13 C14 124.4(2) . . ? N12 C13 H13 117.8 . . ? C14 C13 H13 117.8 . . ? C13 C14 C15 117.8(2) . . ? C13 C14 H14 121.1 . . ? C15 C14 H14 121.1 . . ? C14 C15 C16 119.8(2) . . ? C14 C15 H15 120.1 . . ? C16 C15 H15 120.1 . . ? C15 C16 C11 118.0(2) . . ? C15 C16 H16 121.0 . . ? C11 C16 H16 121.0 . . ? 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 P1 S1 Pd1 -170.97(6) . . . . ? O1 P1 S1 Pd1 -56.92(7) . . . . ? N1 P1 S1 Pd1 66.74(8) . . . . ? S2 Pd1 S1 P1 130.10(3) 2_767 . . . ? S2 Pd1 S1 P1 -49.90(3) . . . . ? S1 Pd1 S2 C1 -153.57(9) 2_767 . . . ? S1 Pd1 S2 C1 26.43(9) . . . . ? O2 P1 O1 C2 61.26(16) . . . . ? N1 P1 O1 C2 173.63(15) . . . . ? S1 P1 O1 C2 -56.31(16) . . . . ? O1 P1 O2 C5 -156.56(17) . . . . ? N1 P1 O2 C5 92.37(18) . . . . ? S1 P1 O2 C5 -35.96(18) . . . . ? O2 P1 N1 C1 -166.02(19) . . . . ? O1 P1 N1 C1 84.6(2) . . . . ? S1 P1 N1 C1 -42.9(2) . . . . ? P1 N1 C1 N2 179.75(16) . . . . ? P1 N1 C1 S2 -1.4(3) . . . . ? C11 N2 C1 N1 -11.5(4) . . . . ? C11 N2 C1 S2 169.46(19) . . . . ? Pd1 S2 C1 N1 4.3(2) . . . . ? Pd1 S2 C1 N2 -176.75(13) . . . . ? P1 O1 C2 C4 135.83(18) . . . . ? P1 O1 C2 C3 -101.7(2) . . . . ? P1 O2 C5 C7 113.3(2) . . . . ? P1 O2 C5 C6 -122.9(2) . . . . ? C1 N2 C11 N12 172.8(2) . . . . ? C1 N2 C11 C16 -9.9(4) . . . . ? C16 C11 N12 C13 -0.8(3) . . . . ? N2 C11 N12 C13 176.51(19) . . . . ? C11 N12 C13 C14 -0.2(3) . . . . ? N12 C13 C14 C15 0.5(4) . . . . ? C13 C14 C15 C16 0.1(4) . . . . ? C14 C15 C16 C11 -1.0(4) . . . . ? N12 C11 C16 C15 1.4(4) . . . . ? N2 C11 C16 C15 -175.6(2) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N2 H2 N12 0.85(3) 2.52(3) 3.356(3) 167(2) 2_756 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.442 _refine_diff_density_min -0.694 _refine_diff_density_rms 0.096