data_global _publ_contact_author_email M.SCHRODER@NOTTINGHAM.AC.UK _publ_contact_author_name 'Prof Martin Schroder' _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name M.Schroder A.J.Amoroso A.J.Blake S.S.M.Chung P.A.Cooke ; M.W.Glenny ; D.J.E.Spencer C.Wilson #===END of CIF data_ni3pzs _database_code_CSD 207885 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H65 B4 F16 N9 Ni6 S8' _chemical_formula_weight 1555.93 _chemical_absolute_configuration ad 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' B B 0.0013 0.0007 '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' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Cubic _symmetry_space_group_name_H-M 'I 4 3 2' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x, y, -z' 'x, -y, -z' 'z, x, y' 'z, -x, -y' '-z, -x, y' '-z, x, -y' 'y, z, x' '-y, z, -x' 'y, -z, -x' '-y, -z, x' 'y, x, -z' '-y, -x, -z' 'y, -x, z' '-y, x, z' 'x, z, -y' '-x, z, y' '-x, -z, -y' 'x, -z, y' 'z, y, -x' 'z, -y, x' '-z, y, x' '-z, -y, -x' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z+1/2' 'z+1/2, x+1/2, y+1/2' 'z+1/2, -x+1/2, -y+1/2' '-z+1/2, -x+1/2, y+1/2' '-z+1/2, x+1/2, -y+1/2' 'y+1/2, z+1/2, x+1/2' '-y+1/2, z+1/2, -x+1/2' 'y+1/2, -z+1/2, -x+1/2' '-y+1/2, -z+1/2, x+1/2' 'y+1/2, x+1/2, -z+1/2' '-y+1/2, -x+1/2, -z+1/2' 'y+1/2, -x+1/2, z+1/2' '-y+1/2, x+1/2, z+1/2' 'x+1/2, z+1/2, -y+1/2' '-x+1/2, z+1/2, y+1/2' '-x+1/2, -z+1/2, -y+1/2' 'x+1/2, -z+1/2, y+1/2' 'z+1/2, y+1/2, -x+1/2' 'z+1/2, -y+1/2, x+1/2' '-z+1/2, y+1/2, x+1/2' '-z+1/2, -y+1/2, -x+1/2' _cell_length_a 25.796(5) _cell_length_b 25.796(5) _cell_length_c 25.796(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 17166(6) _cell_formula_units_Z 12 _cell_measurement_temperature 220(2) _cell_measurement_reflns_used 34 _cell_measurement_theta_min 10 _cell_measurement_theta_max 13.5 _exptl_crystal_description tablet _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.806 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 9504 _exptl_absorpt_coefficient_mu 2.316 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.588 _exptl_absorpt_correction_T_max 0.697 _exptl_special_details ; ? ; _diffrn_ambient_temperature 220(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 'Stoe Stadi-4 four circle' _diffrn_measurement_method omega-theta _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time '60 min' _diffrn_standards_decay_% 'random variation +/-2.4' _diffrn_reflns_number 4060 _diffrn_reflns_av_R_equivalents 0.094 _diffrn_reflns_av_sigmaI/netI 0.108 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.74 _diffrn_reflns_theta_max 22.54 _reflns_number_total 1899 _reflns_number_gt 1422 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Stadi-4 (Stoe & Cie, 1996a)' _computing_cell_refinement 'Stadi-4 (Stoe & Cie, 1996a)' _computing_data_reduction 'X-RED (Stoe & Cie, 1996b)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL/PC (Sheldrick, 1994)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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 w=1/[\s^2^(Fo^2^)+(0.0126P)^2^+262.3P] 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 model' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.02(6) _refine_ls_number_reflns 1899 _refine_ls_number_parameters 181 _refine_ls_number_restraints 58 _refine_ls_R_factor_all 0.103 _refine_ls_R_factor_gt 0.066 _refine_ls_wR_factor_ref 0.129 _refine_ls_wR_factor_gt 0.113 _refine_ls_goodness_of_fit_ref 1.13 _refine_ls_restrained_S_all 1.15 _refine_ls_shift/su_max 0.039 _refine_ls_shift/su_mean 0.016 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni -0.42355(6) -0.15408(6) -0.60226(6) 0.0248(4) Uani 1 d . . . Ni2 Ni -0.5000 -0.20259(13) -0.5000 0.0211(8) Uani 1 d S . . Ni3 Ni -0.5000 -0.08537(12) -0.5000 0.0213(8) Uani 1 d S . . N1 N -0.3576(4) -0.1238(4) -0.6200(4) 0.027(3) Uani 1 d U . . C2 C -0.3521(6) -0.1316(5) -0.6772(5) 0.041(4) Uani 1 d U . . H2A H -0.3154 -0.1313 -0.6871 0.049 Uiso 1 calc R . . H2B H -0.3700 -0.1039 -0.6961 0.049 Uiso 1 calc R . . C3 C -0.3766(6) -0.1841(5) -0.6896(5) 0.035(3) Uani 1 d U . . H3A H -0.4074 -0.1795 -0.7112 0.042 Uiso 1 calc R . . H3B H -0.3518 -0.2060 -0.7083 0.042 Uiso 1 calc R . . N4 N -0.3906(4) -0.2081(5) -0.6405(4) 0.036(3) Uani 1 d U . . C5 C -0.3419(5) -0.2164(5) -0.6099(6) 0.035(3) Uani 1 d U . . H5A H -0.3162 -0.2352 -0.6306 0.042 Uiso 1 calc R . . H5B H -0.3493 -0.2366 -0.5785 0.042 Uiso 1 calc R . . C6 C -0.3210(5) -0.1609(5) -0.5950(6) 0.035(3) Uani 1 d U . . H6A H -0.3208 -0.1563 -0.5573 0.042 Uiso 1 calc R . . H6B H -0.2857 -0.1559 -0.6081 0.042 Uiso 1 calc R . . C11 C -0.3494(6) -0.0703(5) -0.6019(6) 0.044(4) Uani 1 d U . . H11A H -0.3614 -0.0458 -0.6283 0.053 Uiso 1 calc R . . H11B H -0.3124 -0.0643 -0.5958 0.053 Uiso 1 calc R . . C12 C -0.3792(5) -0.0619(5) -0.5522(5) 0.031(3) Uani 1 d U . . H12A H -0.3781 -0.0253 -0.5420 0.037 Uiso 1 calc R . . H12B H -0.3646 -0.0829 -0.5241 0.037 Uiso 1 calc R . . S1 S -0.44538(13) -0.08163(13) -0.56599(13) 0.0275(8) Uani 1 d . . . C41 C -0.4212(6) -0.2568(5) -0.6460(5) 0.039(3) Uani 1 d U . . H41A H -0.4428 -0.2549 -0.6771 0.046 Uiso 1 calc R . . H41B H -0.3976 -0.2864 -0.6496 0.046 Uiso 1 calc R . . C42 C -0.4542(5) -0.2642(6) -0.6001(5) 0.036(4) Uani 1 d U . . H42A H -0.4327 -0.2741 -0.5704 0.043 Uiso 1 calc R . . H42B H -0.4791 -0.2921 -0.6066 0.043 Uiso 1 calc R . . S4 S -0.48892(13) -0.20402(14) -0.58559(13) 0.0278(9) Uani 1 d . . . B1 B -0.7500 -0.2500 -0.7500 0.044(12) Uani 1 d SD . . F10 F -0.7851(5) -0.2149(5) -0.7851(5) 0.048(8) Uani 0.50 d SPD . . F11 F -0.7140(3) -0.2140(3) -0.7500 0.066(4) Uani 1 d SD . . B2 B -0.5000 -0.2202(8) -0.7798(8) 0.057(8) Uani 1 d SD . . F20 F -0.5138(5) -0.2306(7) -0.8288(5) 0.141(6) Uani 1 d D . . F21 F -0.5398(6) -0.2296(5) -0.7508(6) 0.189(9) Uani 1 d D . . B3 B -0.4090(18) -0.4090(18) -0.5910(18) 0.03(3) Uiso 0.25 d SPD A 1 F30 F -0.3733(13) -0.4422(13) -0.6041(13) 0.055(10) Uiso 0.25 d PD A 1 F31 F -0.4389(17) -0.4389(17) -0.5611(17) 0.28(15) Uiso 0.25 d SPD A 1 C1A C -0.4341(12) -0.4341(12) -0.5659(12) 0.18(9) Uiso 0.75 d SPDU B 2 C2A C -0.4020(11) -0.4020(11) -0.5980(11) 0.12(3) Uiso 0.75 d SPDU B 2 N1A N -0.3771(10) -0.3771(10) -0.6229(10) 0.096(13) Uiso 0.75 d SPDU B 2 B4 B -0.2500 0.0290(14) -0.5290(14) 0.051(16) Uiso 0.50 d SPD . . F40 F -0.2141(11) 0.0525(12) -0.5535(13) 0.151(12) Uiso 0.50 d PD . . F41 F -0.2430(19) -0.0201(11) -0.5388(12) 0.163(13) Uiso 0.50 d PD . . 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 Ni1 0.0233(10) 0.0302(10) 0.0210(9) 0.0005(8) 0.0020(8) 0.0024(8) Ni2 0.0202(12) 0.023(2) 0.0202(12) 0.000 0.000 0.000 Ni3 0.0205(11) 0.0229(19) 0.0205(11) 0.000 0.000 0.000 N1 0.022(6) 0.034(5) 0.025(5) 0.005(4) 0.012(5) 0.009(5) C2 0.058(10) 0.044(7) 0.022(5) 0.007(5) 0.008(6) 0.001(7) C3 0.033(9) 0.048(8) 0.025(6) 0.002(4) 0.006(6) 0.005(6) N4 0.031(6) 0.047(7) 0.030(6) 0.004(5) 0.004(5) -0.004(5) C5 0.036(7) 0.038(5) 0.032(8) 0.004(7) 0.007(6) 0.013(6) C6 0.026(7) 0.052(7) 0.027(7) 0.008(6) -0.003(6) 0.002(5) C11 0.043(9) 0.039(6) 0.050(9) -0.004(7) 0.019(7) -0.021(7) C12 0.033(8) 0.021(7) 0.039(8) 0.001(6) 0.008(6) -0.015(7) S1 0.0253(19) 0.0307(18) 0.027(2) 0.0034(17) 0.0043(15) 0.0050(16) C41 0.047(8) 0.033(7) 0.036(8) -0.001(6) 0.004(6) 0.004(6) C42 0.022(8) 0.045(9) 0.042(8) -0.010(7) 0.001(6) -0.009(6) S4 0.022(2) 0.037(2) 0.0246(19) -0.0019(17) -0.0009(17) -0.0041(17) B1 0.044(12) 0.044(12) 0.044(12) -0.017(16) 0.017(16) -0.017(16) F10 0.048(8) 0.048(8) 0.048(8) 0.000(9) 0.000(9) 0.000(9) F11 0.074(7) 0.074(7) 0.050(9) 0.006(6) -0.006(6) -0.046(8) B2 0.029(15) 0.071(13) 0.071(13) -0.006(18) 0.010(12) 0.010(12) F20 0.101(12) 0.230(17) 0.092(10) 0.049(11) -0.036(9) -0.007(11) F21 0.230(17) 0.121(12) 0.217(17) -0.120(12) 0.171(14) -0.117(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 Ni1 N4 1.909(12) . y Ni1 N1 1.928(10) . y Ni1 S1 2.165(4) . y Ni1 S4 2.165(4) . y Ni2 S4 2.227(3) . y Ni3 S1 2.212(3) . y N1 C11 1.471(16) . y N1 C6 1.493(16) . y N1 C2 1.495(15) . y C2 C3 1.529(18) . y C3 N4 1.454(17) . ? N4 C41 1.490(17) . ? N4 C5 1.499(16) . ? C5 C6 1.577(18) . ? C11 C12 1.510(18) . ? C12 S1 1.816(13) . ? C41 C42 1.469(18) . ? C42 S4 1.830(14) . ? B1 F11 1.314(12) . ? B1 F10 1.57(2) . ? B2 F21 1.294(17) . ? B2 F20 1.341(17) . ? B3 F30 1.30(3) . ? B3 F31 1.33(5) . ? C1A C2A 1.44(2) . ? C2A N1A 1.11(2) . ? B4 F40 1.27(3) . ? B4 F41 1.30(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 N4 Ni1 N1 77.3(5) . . y N4 Ni1 S1 166.0(4) . . y N1 Ni1 S1 89.0(3) . . y N4 Ni1 S4 90.9(4) . . y N1 Ni1 S4 167.4(3) . . y S1 Ni1 S4 103.02(15) . . y S4 Ni2 S4 178.1(3) 21_554 23_455 ? S4 Ni2 S4 89.984(4) 21_554 . ? S4 Ni2 S4 89.984(5) 23_455 . ? S4 Ni2 S4 89.984(4) 21_554 3_454 ? S4 Ni2 S4 89.984(5) 23_455 3_454 ? S4 Ni2 S4 178.1(3) . 3_454 ? S1 Ni3 S1 175.0(2) 23_455 21_554 ? S1 Ni3 S1 89.891(10) 23_455 . ? S1 Ni3 S1 89.891(10) 21_554 . ? S1 Ni3 S1 89.891(11) 23_455 3_454 ? S1 Ni3 S1 89.891(11) 21_554 3_454 ? S1 Ni3 S1 175.0(2) . 3_454 ? C11 N1 C6 112.0(11) . . y C11 N1 C2 115.2(11) . . ? C6 N1 C2 106.3(11) . . ? C11 N1 Ni1 115.5(8) . . ? C6 N1 Ni1 101.3(8) . . ? C2 N1 Ni1 105.2(8) . . y N1 C2 C3 106.7(11) . . ? N4 C3 C2 107.3(11) . . ? C3 N4 C41 114.1(10) . . ? C3 N4 C5 108.2(11) . . ? C41 N4 C5 111.9(11) . . ? C3 N4 Ni1 104.4(9) . . y C41 N4 Ni1 115.4(9) . . ? C5 N4 Ni1 101.8(8) . . y N4 C5 C6 106.6(10) . . ? N1 C6 C5 105.1(10) . . ? N1 C11 C12 109.4(11) . . ? C11 C12 S1 105.8(9) . . ? C12 S1 Ni1 94.7(4) . . ? C12 S1 Ni3 117.4(4) . . y Ni1 S1 Ni3 117.43(18) . . y C42 C41 N4 109.9(11) . . ? C41 C42 S4 109.9(11) . . ? C42 S4 Ni1 94.7(4) . . y C42 S4 Ni2 106.3(5) . . ? Ni1 S4 Ni2 106.68(16) . . y F21 B2 F21 115(3) 19_444 . ? F21 B2 F20 107.4(10) 19_444 19_444 ? F21 B2 F20 105.7(8) . 19_444 ? F21 B2 F20 107.3(10) . . ? F30 B3 F30 117(2) 11_544 . ? F30 B3 F31 100(4) . . ? N1A C2A C1A 180(4) . . ? F40 B4 F41 105(2) . . ? F40 B4 F41 119(2) 43_444 . ? F40 B4 F41 119(2) . 43_444 ? F40 B4 F41 105(2) 43_444 43_444 ? F41 B4 F41 113(5) . 43_444 ? F40 B4 F41 118(2) . 4_554 ? F40 B4 F41 127(2) 43_444 4_554 ? F40 B4 F41 127(2) . 42_454 ? F40 B4 F41 118(2) 43_444 42_454 ? F41 F41 B4 115(5) 42_454 . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 22.54 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.95 _refine_diff_density_min -0.47 _refine_diff_density_rms 0.11 data_PDN2S2 _database_code_CSD 207886 _refine_special_details ; The data show signs of twinning and an hklf 5 format file was generated for the a 180 degree rotation about the 0 0 1 direct lattice direction and refines to give 15% of the twin component. Although this gave some improvement there is probably another, unidentified component present as well as there remain some large peaks of residual electron density. The largest peaks are now adjacent to Pd sites and there does not appear to be a sensible structural model for the remaining smaller peaks. Alternative absorption corrections have been tried, as has refinement in space group P1, neither of which makes an improvement. There is disorder in several parts of the structure, 3 of 4 of the BF4 counterions are disordered. Those of B2 and B4 have 3 of 4 F sites modeled over two half occupied sites and that of B3 has all 4. Geometric restraints were applied. C8, C10 and C11 are also modeled over 2 sites, occupancy ratio 0.35:0.65 Distance restraints were also applied to this group and to other C-C and C-N distances. There is likely the same disorder in the second half cation, indicated by the large Uiso for equivalent atoms, however no additional sites could be found. The hydrogen sites for C7 and C12 are modeled over two sites as they are necessarily disordered.One of the MeCN molecules is also modeled over 2 sites, 6:4 ratio. ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44 H92 B4 F16 N12 Pd6 S8' _chemical_formula_weight 2031.42 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' B B 0.0013 0.0007 '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' 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 11.594(5) _cell_length_b 13.393(6) _cell_length_c 25.598(11) _cell_angle_alpha 77.182(7) _cell_angle_beta 89.969(8) _cell_angle_gamma 76.473(7) _cell_volume 3763(3) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 2726 _cell_measurement_theta_min 2 _cell_measurement_theta_max 22.5 _exptl_crystal_description lath _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.793 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2016 _exptl_absorpt_coefficient_mu 1.704 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.714 _exptl_absorpt_correction_T_max 0.881 _exptl_absorpt_process_details '(SADABS; Bruker, 1999)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART CCD area detector' _diffrn_measurement_method omega _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24288 _diffrn_reflns_av_R_equivalents 0.091 _diffrn_reflns_av_sigmaI/netI 0.190 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.61 _diffrn_reflns_theta_max 25.00 _reflns_number_total 16451 _reflns_number_gt 6448 _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^)+(0.155P)^2^P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens 'geometrically placed, MeCN from delta-F' _refine_ls_hydrogen_treatment 'Riding model MeCN as rigid rotor' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13033 _refine_ls_number_parameters 542 _refine_ls_number_restraints 453 _refine_ls_R_factor_all 0.179 _refine_ls_R_factor_gt 0.095 _refine_ls_wR_factor_ref 0.288 _refine_ls_wR_factor_gt 0.245 _refine_ls_goodness_of_fit_ref 0.98 _refine_ls_restrained_S_all 0.97 _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 0.04725(13) 0.18972(10) 0.38700(5) 0.0270(4) Uani 1 1 d . B . S1 S -0.1297(4) 0.1535(3) 0.4136(2) 0.0337(12) Uani 1 1 d . . . Pd2 Pd 0.11250(12) 0.01072(10) 0.52842(5) 0.0226(3) Uani 1 1 d . . . C2 C -0.190(2) 0.1483(17) 0.3484(9) 0.053(6) Uiso 1 1 d D . . H2A H -0.1600 0.0776 0.3409 0.063 Uiso 1 1 calc R . . H2B H -0.2781 0.1641 0.3475 0.063 Uiso 1 1 calc R . . Pd3 Pd 0.17486(12) -0.20363(10) 0.44619(6) 0.0254(4) Uani 1 1 d . . . C3 C -0.148(4) 0.232(3) 0.3072(15) 0.161(17) Uiso 1 1 d D . . H3A H -0.1783 0.2334 0.2709 0.194 Uiso 1 1 calc R . . H3B H -0.1819 0.3025 0.3147 0.194 Uiso 1 1 calc R . . N4 N -0.0178(16) 0.2142(13) 0.3077(6) 0.045(4) Uani 1 1 d D . . C5 C 0.011(3) 0.1149(18) 0.2898(13) 0.107(11) Uiso 1 1 d D . . H5A H -0.0066 0.1294 0.2511 0.160 Uiso 1 1 calc R . . H5B H -0.0363 0.0677 0.3086 0.160 Uiso 1 1 calc R . . H5C H 0.0958 0.0812 0.2979 0.160 Uiso 1 1 calc R . . C6 C 0.016(2) 0.296(3) 0.2722(15) 0.124(13) Uiso 1 1 d D B . H6A H -0.0231 0.3628 0.2825 0.149 Uiso 1 1 calc R . . H6B H -0.0180 0.3003 0.2361 0.149 Uiso 1 1 calc R . . C7 C 0.148(2) 0.2952(19) 0.2667(9) 0.069(7) Uiso 1 1 d D . . H7A H 0.1932 0.2248 0.2629 0.083 Uiso 0.65 1 calc PR A 2 H7B H 0.1583 0.3480 0.2343 0.083 Uiso 0.65 1 calc PR A 2 H7C H 0.1712 0.2651 0.2351 0.083 Uiso 0.35 1 d PR A 1 H7D H 0.1575 0.3686 0.2576 0.083 Uiso 0.35 1 d PR A 1 C8 C 0.234(4) 0.220(4) 0.3112(7) 0.047(16) Uiso 0.35 1 d PD B 1 H8A H 0.2329 0.1466 0.3104 0.057 Uiso 0.35 1 calc PR B 1 H8B H 0.3153 0.2285 0.3040 0.057 Uiso 0.35 1 calc PR B 1 C8' C 0.196(4) 0.321(2) 0.3166(8) 0.071(11) Uiso 0.65 1 d PD B 2 H8'A H 0.2750 0.3353 0.3097 0.085 Uiso 0.65 1 calc PR B 2 H8'B H 0.1423 0.3858 0.3230 0.085 Uiso 0.65 1 calc PR B 2 N9 N 0.2060(14) 0.2362(11) 0.3652(6) 0.046(5) Uani 1 1 d D . . C10 C 0.185(5) 0.3475(19) 0.368(3) 0.052(17) Uiso 0.35 1 d PD B 1 H10A H 0.2563 0.3729 0.3591 0.078 Uiso 0.35 1 calc PR B 1 H10B H 0.1641 0.3538 0.4047 0.078 Uiso 0.35 1 calc PR B 1 H10C H 0.1187 0.3898 0.3428 0.078 Uiso 0.35 1 calc PR B 1 C10' C 0.296(3) 0.145(2) 0.3563(16) 0.068(11) Uiso 0.65 1 d PD B 2 H10D H 0.3698 0.1655 0.3465 0.102 Uiso 0.65 1 calc PR B 2 H10E H 0.2667 0.1186 0.3271 0.102 Uiso 0.65 1 calc PR B 2 H10F H 0.3102 0.0886 0.3892 0.102 Uiso 0.65 1 calc PR B 2 C11 C 0.295(3) 0.169(3) 0.4071(7) 0.027(12) Uiso 0.35 1 d PD B 1 H11A H 0.3731 0.1857 0.3996 0.033 Uiso 0.35 1 calc PR B 1 H11B H 0.3023 0.0944 0.4070 0.033 Uiso 0.35 1 calc PR B 1 C11' C 0.252(3) 0.270(2) 0.4099(7) 0.056(9) Uiso 0.65 1 d PD B 2 H11C H 0.2002 0.3384 0.4134 0.067 Uiso 0.65 1 calc PR B 2 H11D H 0.3327 0.2815 0.4023 0.067 Uiso 0.65 1 calc PR B 2 C12 C 0.2584(17) 0.1886(15) 0.4623(7) 0.042(5) Uiso 1 1 d D . . H12F H 0.2648 0.2599 0.4646 0.050 Uiso 0.35 1 calc PR B 1 H12G H 0.3129 0.1364 0.4906 0.050 Uiso 0.35 1 calc PR B 1 H12H H 0.2903 0.2117 0.4923 0.050 Uiso 0.65 1 d PR B 2 H12I H 0.3102 0.1200 0.4595 0.050 Uiso 0.65 1 d PR B 2 S13 S 0.1054(4) 0.1768(3) 0.47343(18) 0.0284(11) Uani 1 1 d . B . S14 S 0.2363(4) -0.0679(3) 0.4690(2) 0.0298(11) Uani 1 1 d . . . C15 C 0.3724(17) -0.1462(13) 0.5076(8) 0.040(5) Uiso 1 1 d D . . H15A H 0.4282 -0.1013 0.5098 0.048 Uiso 1 1 calc R . . H15B H 0.3542 -0.1779 0.5445 0.048 Uiso 1 1 calc R . . C16 C 0.4270(16) -0.2326(14) 0.4782(9) 0.054(6) Uiso 1 1 d D . . H16A H 0.4462 -0.2001 0.4416 0.065 Uiso 1 1 calc R . . H16B H 0.5016 -0.2773 0.4977 0.065 Uiso 1 1 calc R . . N17 N 0.3428(12) -0.2975(10) 0.4750(5) 0.031(4) Uani 1 1 d D . . C18 C 0.335(2) -0.3611(17) 0.5292(7) 0.065(7) Uiso 1 1 d D . . H18A H 0.4141 -0.4045 0.5428 0.098 Uiso 1 1 calc R . . H18B H 0.2810 -0.4069 0.5277 0.098 Uiso 1 1 calc R . . H18C H 0.3049 -0.3143 0.5531 0.098 Uiso 1 1 calc R . . C19 C 0.3916(18) -0.3637(15) 0.4375(8) 0.058(6) Uiso 1 1 d D . . H19A H 0.4727 -0.4039 0.4514 0.070 Uiso 1 1 calc R . . H19B H 0.3995 -0.3161 0.4027 0.070 Uiso 1 1 calc R . . C20 C 0.3228(16) -0.4427(13) 0.4262(9) 0.050(6) Uiso 1 1 d D . . H20A H 0.3738 -0.4940 0.4084 0.060 Uiso 1 1 calc R . . H20B H 0.2990 -0.4820 0.4603 0.060 Uiso 1 1 calc R . . C21 C 0.2129(14) -0.3817(16) 0.3901(7) 0.058(6) Uiso 1 1 d D . . H21A H 0.2372 -0.3327 0.3595 0.070 Uiso 1 1 calc R . . H21B H 0.1799 -0.4322 0.3753 0.070 Uiso 1 1 calc R . . N22 N 0.1186(12) -0.3207(9) 0.4170(5) 0.033(4) Uani 1 1 d D . . C23 C 0.0664(19) -0.3889(16) 0.4585(8) 0.059(6) Uiso 1 1 d D . . H23A H 0.0414 -0.4418 0.4431 0.089 Uiso 1 1 calc R . . H23B H -0.0027 -0.3461 0.4719 0.089 Uiso 1 1 calc R . . H23C H 0.1256 -0.4245 0.4881 0.089 Uiso 1 1 calc R . . C24 C 0.0267(15) -0.2680(15) 0.3739(7) 0.055(6) Uiso 1 1 d D . . H24A H -0.0098 -0.3211 0.3635 0.066 Uiso 1 1 calc R . . H24B H 0.0635 -0.2339 0.3421 0.066 Uiso 1 1 calc R . . C25 C -0.0695(15) -0.1852(13) 0.3917(8) 0.038(5) Uiso 1 1 d D . . H25A H -0.1087 -0.2187 0.4228 0.045 Uiso 1 1 calc R . . H25B H -0.1304 -0.1500 0.3621 0.045 Uiso 1 1 calc R . . S26 S 0.0019(4) -0.0899(3) 0.40982(18) 0.0295(11) Uani 1 1 d . . . Pd1A Pd 0.53238(15) 0.17642(12) 0.07820(6) 0.0412(4) Uani 1 1 d . . . S1A S 0.3588(5) 0.1406(4) 0.0559(2) 0.0461(14) Uani 1 1 d . . . Pd2A Pd 0.61159(13) 0.01950(10) -0.03008(6) 0.0297(4) Uani 1 1 d . . . C2A C 0.296(3) 0.111(2) 0.1243(11) 0.084(9) Uiso 1 1 d D . . H2AA H 0.2083 0.1239 0.1220 0.101 Uiso 1 1 calc R . . H2AB H 0.3311 0.0381 0.1447 0.101 Uiso 1 1 calc R . . Pd3A Pd 0.31682(15) 0.20477(11) -0.09914(6) 0.0396(4) Uani 1 1 d . . . C3A C 0.338(3) 0.192(2) 0.1474(13) 0.106(11) Uiso 1 1 d D . . H3AA H 0.3039 0.2625 0.1235 0.127 Uiso 1 1 calc R . . H3AB H 0.3020 0.1930 0.1825 0.127 Uiso 1 1 calc R . . N4A N 0.4620(15) 0.1826(14) 0.1553(7) 0.051(5) Uani 1 1 d D . . C5A C 0.502(4) 0.082(2) 0.1947(15) 0.19(2) Uiso 1 1 d D . . H5AA H 0.4679 0.0878 0.2292 0.292 Uiso 1 1 calc R . . H5AB H 0.5891 0.0635 0.1993 0.292 Uiso 1 1 calc R . . H5AC H 0.4763 0.0261 0.1820 0.292 Uiso 1 1 calc R . . C6A C 0.490(2) 0.267(3) 0.1744(17) 0.142(15) Uiso 1 1 d D . . H6AA H 0.4561 0.2667 0.2100 0.171 Uiso 1 1 calc R . . H6AB H 0.4480 0.3343 0.1498 0.171 Uiso 1 1 calc R . . C7A C 0.622(2) 0.268(2) 0.1798(10) 0.090(9) Uiso 1 1 d D . . H7AA H 0.6311 0.3173 0.2025 0.108 Uiso 1 1 calc R . . H7AB H 0.6688 0.1969 0.1975 0.108 Uiso 1 1 calc R . . C8A C 0.670(3) 0.3034(19) 0.1246(10) 0.112(11) Uiso 1 1 d D . . H8AA H 0.6147 0.3684 0.1042 0.135 Uiso 1 1 calc R . . H8AB H 0.7479 0.3196 0.1293 0.135 Uiso 1 1 calc R . . N9A N 0.6836(15) 0.2207(12) 0.0942(7) 0.049(5) Uani 1 1 d D . . C10A C 0.786(2) 0.133(2) 0.1166(14) 0.116(12) Uiso 1 1 d D . . H10G H 0.8540 0.1615 0.1229 0.175 Uiso 1 1 calc R . . H10H H 0.8062 0.0874 0.0913 0.175 Uiso 1 1 calc R . . H10I H 0.7656 0.0923 0.1506 0.175 Uiso 1 1 calc R . . C11A C 0.738(3) 0.261(3) 0.0447(12) 0.129(13) Uiso 1 1 d D . . H11E H 0.8215 0.2605 0.0538 0.155 Uiso 1 1 calc R . . H11F H 0.6957 0.3353 0.0299 0.155 Uiso 1 1 calc R . . C12A C 0.738(2) 0.1992(17) 0.0016(9) 0.055(6) Uiso 1 1 d D . . H12B H 0.7951 0.1295 0.0124 0.066 Uiso 1 1 calc R . . H12C H 0.7625 0.2379 -0.0326 0.066 Uiso 1 1 calc R . . S13A S 0.5895(6) 0.1818(4) -0.0074(2) 0.0498(15) Uani 1 1 d . . . S14A S 0.4981(5) 0.1027(4) -0.1092(2) 0.0473(14) Uani 1 1 d . . . C15A C 0.567(2) 0.2055(16) -0.1452(9) 0.061(7) Uiso 1 1 d D . . H15C H 0.5946 0.2433 -0.1204 0.074 Uiso 1 1 calc R . . H15D H 0.6349 0.1758 -0.1651 0.074 Uiso 1 1 calc R . . C16A C 0.4653(18) 0.278(2) -0.1836(9) 0.091(9) Uiso 1 1 d D . . H16C H 0.4957 0.3330 -0.2082 0.109 Uiso 1 1 calc R . . H16D H 0.4350 0.2364 -0.2055 0.109 Uiso 1 1 calc R . . N17A N 0.3672(15) 0.3288(11) -0.1546(6) 0.047(5) Uani 1 1 d D . . C18A C 0.392(3) 0.4066(19) -0.1265(11) 0.093(9) Uiso 1 1 d D . . H18D H 0.4143 0.4638 -0.1524 0.139 Uiso 1 1 calc R . . H18E H 0.4571 0.3724 -0.0994 0.139 Uiso 1 1 calc R . . H18F H 0.3206 0.4355 -0.1090 0.139 Uiso 1 1 calc R . . C19A C 0.2703(17) 0.386(2) -0.1948(9) 0.082(8) Uiso 1 1 d D . . H19C H 0.2508 0.3359 -0.2147 0.098 Uiso 1 1 calc R . . H19D H 0.2986 0.4404 -0.2209 0.098 Uiso 1 1 calc R . . C20A C 0.1572(19) 0.4393(17) -0.1715(10) 0.073(8) Uiso 1 1 d D . . H20C H 0.1779 0.4754 -0.1444 0.088 Uiso 1 1 calc R . . H20D H 0.1058 0.4927 -0.2004 0.088 Uiso 1 1 calc R . . C21A C 0.091(2) 0.3564(19) -0.1457(8) 0.090(9) Uiso 1 1 d D . . H21C H 0.0084 0.3929 -0.1409 0.108 Uiso 1 1 calc R . . H21D H 0.0876 0.3105 -0.1708 0.108 Uiso 1 1 calc R . . N22A N 0.1428(14) 0.2894(10) -0.0937(6) 0.041(4) Uani 1 1 d D . . C23A C 0.134(3) 0.355(2) -0.0540(10) 0.101(10) Uiso 1 1 d D . . H23D H 0.0507 0.3927 -0.0531 0.151 Uiso 1 1 calc R . . H23E H 0.1829 0.4057 -0.0640 0.151 Uiso 1 1 calc R . . H23F H 0.1613 0.3096 -0.0185 0.151 Uiso 1 1 calc R . . C24A C 0.0672(18) 0.2163(16) -0.0745(8) 0.070(7) Uiso 1 1 d D . . H24C H 0.0525 0.1818 -0.1035 0.084 Uiso 1 1 calc R . . H24D H -0.0104 0.2563 -0.0654 0.084 Uiso 1 1 calc R . . C25A C 0.1253(18) 0.1319(15) -0.0251(8) 0.049(6) Uiso 1 1 d D . . H25C H 0.0738 0.0828 -0.0127 0.059 Uiso 1 1 calc R . . H25D H 0.1393 0.1649 0.0046 0.059 Uiso 1 1 calc R . . S26A S 0.2665(5) 0.0617(4) -0.0462(2) 0.0458(14) Uani 1 1 d . . . B1 B 0.3212(16) -0.1255(14) 0.2957(7) 0.083(10) Uiso 1 1 d D . . F1 F 0.388(2) -0.1919(19) 0.2686(10) 0.224(13) Uiso 1 1 d D . . F2 F 0.3112(18) -0.0257(14) 0.2685(8) 0.153(8) Uiso 1 1 d D . . F3 F 0.3765(18) -0.1427(16) 0.3449(8) 0.160(9) Uiso 1 1 d D . . F4 F 0.2136(15) -0.1493(13) 0.3005(7) 0.117(6) Uiso 1 1 d D . . B2 B 0.8174(14) -0.1278(12) 0.2397(6) 0.092(11) Uiso 1 1 d D . . F5 F 0.9243(19) -0.2028(18) 0.2525(11) 0.087(9) Uiso 0.50 1 d PD C 1 F6 F 0.726(2) -0.167(2) 0.2631(12) 0.118(13) Uiso 0.50 1 d PD C 1 F7 F 0.799(3) -0.0973(19) 0.1850(7) 0.081(9) Uiso 0.50 1 d PD C 1 F5A F 0.847(3) -0.2235(15) 0.2769(10) 0.093(10) Uiso 0.50 1 d PD C 2 F6A F 0.6992(19) -0.116(2) 0.2214(13) 0.121(13) Uiso 0.50 1 d PD C 2 F7A F 0.884(3) -0.142(2) 0.1953(10) 0.105(11) Uiso 0.50 1 d PD C 2 F8 F 0.8264(12) -0.0418(10) 0.2596(5) 0.081(4) Uiso 1 1 d D C . B3 B 0.5222(16) 0.3914(12) 0.3115(8) 0.081(10) Uiso 1 1 d D . . F9 F 0.582(3) 0.436(2) 0.2667(13) 0.120(13) Uiso 0.50 1 d PD D 1 F10 F 0.409(2) 0.4594(19) 0.3099(13) 0.085(9) Uiso 0.50 1 d PD D 1 F11 F 0.587(3) 0.384(3) 0.3586(14) 0.18(2) Uiso 0.50 1 d PD D 1 F12 F 0.515(2) 0.2911(18) 0.3052(12) 0.074(9) Uiso 0.50 1 d PD D 1 F9' F 0.470(4) 0.420(3) 0.2609(14) 0.18(2) Uiso 0.50 1 d PD D 2 F10' F 0.450(3) 0.448(3) 0.3435(16) 0.137(15) Uiso 0.50 1 d PD D 2 F11' F 0.633(3) 0.412(3) 0.3130(18) 0.134(14) Uiso 0.50 1 d PD D 2 F12' F 0.534(4) 0.285(3) 0.3338(18) 0.24(3) Uiso 0.50 1 d PD D 2 B4 B -0.0077(13) 0.6694(11) -0.1074(6) 0.061(8) Uiso 1 1 d D . . F13 F -0.048(2) 0.701(2) -0.0615(9) 0.115(13) Uiso 0.50 1 d PD E 1 F14 F -0.006(2) 0.7579(16) -0.1480(8) 0.065(7) Uiso 0.50 1 d PD E 1 F15 F 0.1050(15) 0.6048(16) -0.0987(10) 0.063(7) Uiso 0.50 1 d PD E 1 F13A F -0.060(2) 0.758(2) -0.0876(13) 0.123(14) Uiso 0.50 1 d PD E 2 F14A F 0.063(2) 0.698(2) -0.1496(9) 0.088(9) Uiso 0.50 1 d PD E 2 F15A F 0.066(2) 0.5988(17) -0.0650(9) 0.081(9) Uiso 0.50 1 d PD E 2 F16 F -0.0883(13) 0.6208(12) -0.1247(6) 0.104(5) Uiso 1 1 d D E . N1S N 0.261(2) 0.3678(18) 0.5596(9) 0.085(7) Uiso 1 1 d D . . C2S C 0.293(3) 0.362(2) 0.6030(10) 0.083(9) Uiso 1 1 d D . . C3S C 0.327(3) 0.368(2) 0.6567(11) 0.108(11) Uiso 1 1 d D . . H3S1 H 0.3422 0.4372 0.6556 0.163 Uiso 1 1 calc R . . H3S2 H 0.3990 0.3128 0.6702 0.163 Uiso 1 1 calc R . . H3S3 H 0.2625 0.3575 0.6806 0.163 Uiso 1 1 calc R . . N4S N 0.583(2) -0.040(2) 0.4302(10) 0.105(8) Uiso 1 1 d D . . C5S C 0.592(2) -0.031(2) 0.3852(10) 0.075(8) Uiso 1 1 d D . . C6S C 0.587(3) -0.006(3) 0.3269(10) 0.116(12) Uiso 1 1 d D . . H6S1 H 0.5423 -0.0505 0.3139 0.174 Uiso 1 1 calc R . . H6S2 H 0.6680 -0.0205 0.3144 0.174 Uiso 1 1 calc R . . H6S3 H 0.5478 0.0681 0.3132 0.174 Uiso 1 1 calc R . . N7S N 0.121(2) -0.0617(19) 0.0883(9) 0.095(8) Uiso 1 1 d D . . C8S C 0.103(2) -0.0505(17) 0.1299(9) 0.052(6) Uiso 1 1 d D . . C9S C 0.081(2) -0.022(2) 0.1808(9) 0.084(9) Uiso 1 1 d D . . H9S1 H 0.0789 0.0530 0.1766 0.126 Uiso 1 1 calc R . . H9S2 H 0.1454 -0.0642 0.2072 0.126 Uiso 1 1 calc R . . H9S3 H 0.0053 -0.0354 0.1932 0.126 Uiso 1 1 calc R . . N10S N 0.040(3) 0.569(2) 0.2746(12) 0.055(8) Uiso 0.60 1 d PD F 1 C11S C 0.114(3) 0.604(3) 0.2537(17) 0.070(12) Uiso 0.60 1 d PD F 1 C12S C 0.214(3) 0.642(3) 0.2307(14) 0.048(9) Uiso 0.60 1 d PD F 1 H12A H 0.1905 0.7188 0.2181 0.073 Uiso 0.60 1 calc PR F 1 H12D H 0.2399 0.6100 0.2004 0.073 Uiso 0.60 1 calc PR F 1 H12E H 0.2797 0.6227 0.2579 0.073 Uiso 0.60 1 calc PR F 1 N13S N 0.246(3) 0.482(3) 0.0361(14) 0.031(9) Uiso 0.40 1 d PD G 2 C14S C 0.272(5) 0.523(4) 0.0676(19) 0.051(14) Uiso 0.40 1 d PD G 2 C15S C 0.271(6) 0.580(5) 0.110(2) 0.08(2) Uiso 0.40 1 d PD G 2 H15E H 0.2083 0.6455 0.1009 0.118 Uiso 0.40 1 calc PR G 2 H15F H 0.3484 0.5979 0.1123 0.118 Uiso 0.40 1 calc PR G 2 H15G H 0.2570 0.5366 0.1439 0.118 Uiso 0.40 1 calc PR G 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.0337(9) 0.0230(7) 0.0219(8) -0.0028(6) 0.0022(6) -0.0044(6) S1 0.028(3) 0.025(2) 0.043(3) -0.001(2) -0.007(2) -0.002(2) Pd2 0.0222(8) 0.0202(7) 0.0240(8) -0.0046(6) -0.0026(6) -0.0028(6) Pd3 0.0280(8) 0.0187(7) 0.0278(8) -0.0063(6) 0.0015(6) -0.0009(6) N4 0.057(12) 0.055(11) 0.016(9) 0.007(8) -0.003(8) -0.014(9) N9 0.049(11) 0.027(9) 0.052(11) 0.005(8) 0.020(9) -0.004(8) S13 0.038(3) 0.026(2) 0.023(2) -0.006(2) -0.002(2) -0.010(2) S14 0.027(3) 0.023(2) 0.042(3) -0.013(2) 0.008(2) -0.006(2) N17 0.025(9) 0.025(8) 0.040(10) -0.005(7) -0.001(7) 0.000(7) N22 0.053(11) 0.008(7) 0.035(9) -0.003(7) 0.004(8) -0.005(7) S26 0.034(3) 0.028(2) 0.021(2) -0.002(2) 0.000(2) -0.002(2) Pd1A 0.0476(11) 0.0408(9) 0.0380(10) -0.0161(8) -0.0011(8) -0.0097(8) S1A 0.042(3) 0.044(3) 0.050(3) -0.012(3) -0.002(3) -0.005(3) Pd2A 0.0338(9) 0.0263(7) 0.0265(8) -0.0030(6) 0.0016(7) -0.0052(6) Pd3A 0.0485(11) 0.0295(8) 0.0345(9) -0.0018(7) -0.0041(8) -0.0025(7) N4A 0.037(11) 0.061(12) 0.060(13) -0.038(10) -0.007(9) 0.000(9) N9A 0.050(12) 0.036(9) 0.064(13) -0.016(9) -0.005(10) -0.015(9) S13A 0.070(4) 0.034(3) 0.042(3) -0.006(3) 0.004(3) -0.009(3) S14A 0.058(4) 0.044(3) 0.028(3) -0.002(2) 0.002(3) 0.006(3) N17A 0.080(14) 0.022(8) 0.038(10) -0.007(8) -0.009(10) -0.006(9) N22A 0.050(11) 0.024(8) 0.045(11) -0.012(8) -0.019(9) 0.004(8) S26A 0.053(4) 0.040(3) 0.045(3) -0.006(3) -0.008(3) -0.016(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 Pd2 Pd2 3.089(3) 2_556 ? Pd1 S1 2.285(5) . ? Pd1 N4 2.094(15) . ? Pd1 N9 2.114(16) . ? Pd1 S13 2.271(5) . ? Pd2 S1 2.330(5) 2_556 ? Pd2 S13 2.337(5) . ? Pd2 S14 2.341(5) . ? Pd2 S26 2.338(5) 2_556 ? Pd3 S14 2.287(4) . ? Pd3 N17 2.088(13) . ? Pd3 N22 2.108(13) . ? Pd3 S26 2.269(5) . ? S1 C2 1.83(2) . ? C2 C3 1.534(10) . ? C3 N4 1.47(4) . ? N4 C6 1.40(3) . ? N4 C5 1.468(9) . ? C6 C7 1.537(10) . ? C7 C8 1.525(10) . ? C7 C8' 1.529(10) . ? C8 N9 1.469(9) . ? C8' N9 1.469(9) . ? N9 C11 1.468(9) . ? N9 C11' 1.468(9) . ? N9 C10 1.471(9) . ? N9 C10' 1.472(9) . ? C11 C12 1.534(10) . ? C11' C12 1.523(10) . ? C12 S13 1.83(2) . ? S14 C15 1.825(19) . ? C15 C16 1.534(9) . ? C16 N17 1.465(9) . ? N17 C18 1.472(9) . ? N17 C19 1.473(9) . ? C19 C20 1.539(10) . ? C20 C21 1.525(10) . ? C21 N22 1.472(9) . ? N22 C23 1.468(9) . ? N22 C24 1.468(9) . ? C24 C25 1.525(9) . ? C25 S26 1.813(18) . ? Pd2A Pd2A 3.100(3) 2_655 ? Pd1A S1A 2.276(6) . ? Pd1A N4A 2.148(19) . ? Pd1A N9A 2.046(16) . ? Pd1A S13A 2.280(6) . ? Pd2A S1A 2.331(5) 2_655 ? Pd2A S13A 2.329(5) . ? Pd2A S14A 2.322(5) . ? Pd2A S26A 2.309(5) 2_655 ? Pd3A S14A 2.273(6) . ? Pd3A N17A 2.126(16) . ? Pd3A N22A 2.091(15) . ? Pd3A S26A 2.284(6) . ? S1A C2A 1.89(3) . ? C2A C3A 1.519(10) . ? C3A N4A 1.43(3) . ? N4A C6A 1.43(4) . ? N4A C5A 1.471(9) . ? C6A C7A 1.545(10) . ? C7A C8A 1.534(10) . ? C8A N9A 1.469(9) . ? N9A C11A 1.47(4) . ? N9A C10A 1.470(9) . ? C11A C12A 1.522(10) . ? C12A S13A 1.81(2) . ? S14A C15A 1.83(2) . ? C15A C16A 1.530(10) . ? C16A N17A 1.473(9) . ? N17A C19A 1.469(9) . ? N17A C18A 1.469(9) . ? C19A C20A 1.528(10) . ? C20A C21A 1.526(10) . ? C21A N22A 1.468(9) . ? N22A C24A 1.469(9) . ? N22A C23A 1.470(9) . ? C24A C25A 1.531(10) . ? C25A S26A 1.83(2) . ? B1 F1 1.351(16) . ? B1 F2 1.342(16) . ? B1 F3 1.362(16) . ? B1 F4 1.356(16) . ? B2 F5 1.388(15) . ? B2 F6 1.372(15) . ? B2 F7 1.371(15) . ? B2 F8 1.384(14) . ? B2 F5A 1.384(15) . ? B2 F6A 1.409(15) . ? B2 F7A 1.399(15) . ? B3 F9 1.43(2) . ? B3 F10 1.41(2) . ? B3 F11 1.39(2) . ? B3 F12 1.41(2) . ? B3 F9' 1.37(3) . ? B3 F10' 1.39(3) . ? B3 F11' 1.38(3) . ? B3 F12' 1.39(3) . ? B4 F13 1.382(15) . ? B4 F14 1.396(15) . ? B4 F15 1.375(15) . ? B4 F16 1.381(14) . ? B4 F13A 1.399(15) . ? B4 F14A 1.392(15) . ? B4 F15A 1.406(15) . ? N1S C2S 1.154(19) . ? C2S C3S 1.45(2) . ? N4S C5S 1.138(19) . ? C5S C6S 1.45(2) . ? N7S C8S 1.122(19) . ? C8S C9S 1.44(2) . ? N10S C11S 1.15(2) . ? C11S C12S 1.45(2) . ? N13S C14S 1.15(2) . ? C14S C15S 1.46(2) . ? 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 Pd1 N9 94.4(7) . . ? N4 Pd1 S13 174.8(5) . . ? N9 Pd1 S13 87.0(4) . . ? N4 Pd1 S1 87.5(5) . . ? N9 Pd1 S1 174.6(4) . . ? S13 Pd1 S1 90.60(18) . . ? C2 S1 Pd1 98.6(8) . . ? C2 S1 Pd2 107.9(7) . 2_556 ? Pd1 S1 Pd2 114.49(19) . 2_556 ? S1 Pd2 S13 176.32(17) 2_556 . ? S1 Pd2 S26 89.38(17) 2_556 2_556 ? S13 Pd2 S26 90.19(17) . 2_556 ? S1 Pd2 S14 90.49(18) 2_556 . ? S13 Pd2 S14 89.74(17) . . ? S26 Pd2 S14 176.88(17) 2_556 . ? S1 Pd2 Pd2 90.84(13) 2_556 2_556 ? S13 Pd2 Pd2 92.82(12) . 2_556 ? S26 Pd2 Pd2 91.16(13) 2_556 2_556 ? S14 Pd2 Pd2 91.96(13) . 2_556 ? C3 C2 S1 105(2) . . ? N17 Pd3 N22 95.5(5) . . ? N17 Pd3 S26 174.2(4) . . ? N22 Pd3 S26 87.7(4) . . ? N17 Pd3 S14 86.6(4) . . ? N22 Pd3 S14 174.2(4) . . ? S26 Pd3 S14 89.80(17) . . ? N4 C3 C2 113(3) . . ? C6 N4 C5 113(2) . . ? C6 N4 C3 110.8(18) . . ? C5 N4 C3 100(2) . . ? C6 N4 Pd1 113.9(18) . . ? C5 N4 Pd1 110.3(15) . . ? C3 N4 Pd1 108.5(18) . . ? N4 C6 C7 120(3) . . ? C8 C7 C6 116(3) . . ? C8' C7 C6 109(3) . . ? N9 C8 C7 113.9(19) . . ? N9 C8' C7 113.7(19) . . ? C11' N9 C8' 108.4(14) . . ? C11 N9 C8 113.3(16) . . ? C11 N9 C10 110(3) . . ? C8 N9 C10 113(3) . . ? C11' N9 C10' 107(2) . . ? C8' N9 C10' 107(2) . . ? C11 N9 Pd1 104.2(19) . . ? C11' N9 Pd1 109.0(15) . . ? C8' N9 Pd1 115.5(18) . . ? C8 N9 Pd1 109(3) . . ? C10 N9 Pd1 106(3) . . ? C10' N9 Pd1 109.1(17) . . ? N9 C11 C12 110.4(16) . . ? N9 C11' C12 111.0(16) . . ? C11' C12 C11 52.2(19) . . ? C11' C12 S13 105.9(17) . . ? C11 C12 S13 110.5(19) . . ? C12 S13 Pd1 98.1(6) . . ? C12 S13 Pd2 108.1(6) . . ? Pd1 S13 Pd2 112.79(18) . . ? C15 S14 Pd3 97.6(6) . . ? C15 S14 Pd2 107.0(6) . . ? Pd3 S14 Pd2 113.0(2) . . ? C16 C15 S14 106.8(13) . . ? N17 C16 C15 109.5(14) . . ? C16 N17 C18 108.2(16) . . ? C16 N17 C19 105.7(12) . . ? C18 N17 C19 112.0(15) . . ? C16 N17 Pd3 111.0(11) . . ? C18 N17 Pd3 109.6(12) . . ? C19 N17 Pd3 110.1(12) . . ? N17 C19 C20 118.2(16) . . ? C21 C20 C19 108.5(17) . . ? N22 C21 C20 114.4(16) . . ? C23 N22 C24 107.6(15) . . ? C23 N22 C21 112.2(15) . . ? C24 N22 C21 103.5(12) . . ? C23 N22 Pd3 112.4(11) . . ? C24 N22 Pd3 108.1(10) . . ? C21 N22 Pd3 112.4(12) . . ? N22 C24 C25 111.2(14) . . ? C24 C25 S26 107.5(13) . . ? C25 S26 Pd3 97.8(6) . . ? C25 S26 Pd2 108.7(6) . 2_556 ? Pd3 S26 Pd2 113.87(19) . 2_556 ? N9A Pd1A N4A 95.0(7) . . ? N9A Pd1A S1A 175.3(5) . . ? N4A Pd1A S1A 86.4(5) . . ? N9A Pd1A S13A 88.2(6) . . ? N4A Pd1A S13A 174.1(5) . . ? S1A Pd1A S13A 89.9(2) . . ? C2A S1A Pd1A 100.5(8) . . ? C2A S1A Pd2A 103.1(8) . 2_655 ? Pd1A S1A Pd2A 112.5(2) . 2_655 ? S26A Pd2A S14A 176.9(2) 2_655 . ? S26A Pd2A S13A 90.10(19) 2_655 . ? S14A Pd2A S13A 89.8(2) . . ? S26A Pd2A S1A 90.39(19) 2_655 2_655 ? S14A Pd2A S1A 89.51(19) . 2_655 ? S13A Pd2A S1A 177.0(2) . 2_655 ? S26A Pd2A Pd2A 91.56(17) 2_655 2_655 ? S14A Pd2A Pd2A 91.55(16) . 2_655 ? S13A Pd2A Pd2A 91.49(17) . 2_655 ? S1A Pd2A Pd2A 91.45(16) 2_655 2_655 ? C3A C2A S1A 98(2) . . ? N22A Pd3A N17A 95.5(6) . . ? N22A Pd3A S14A 174.4(4) . . ? N17A Pd3A S14A 86.6(5) . . ? N22A Pd3A S26A 87.3(4) . . ? N17A Pd3A S26A 174.1(4) . . ? S14A Pd3A S26A 90.1(2) . . ? N4A C3A C2A 119(3) . . ? C3A N4A C6A 113.8(19) . . ? C3A N4A C5A 104(3) . . ? C6A N4A C5A 111(3) . . ? C3A N4A Pd1A 104.8(16) . . ? C6A N4A Pd1A 111(2) . . ? C5A N4A Pd1A 112(2) . . ? N4A C6A C7A 118(3) . . ? C8A C7A C6A 111(3) . . ? N9A C8A C7A 111(2) . . ? C11A N9A C8A 105.0(17) . . ? C11A N9A C10A 96(2) . . ? C8A N9A C10A 110(2) . . ? C11A N9A Pd1A 111.7(16) . . ? C8A N9A Pd1A 116.3(17) . . ? C10A N9A Pd1A 115.0(16) . . ? N9A C11A C12A 114(2) . . ? C11A C12A S13A 109(2) . . ? C12A S13A Pd1A 98.4(7) . . ? C12A S13A Pd2A 106.5(7) . . ? Pd1A S13A Pd2A 112.1(2) . . ? C15A S14A Pd3A 99.1(7) . . ? C15A S14A Pd2A 107.7(7) . . ? Pd3A S14A Pd2A 115.2(2) . . ? C16A C15A S14A 102.5(17) . . ? N17A C16A C15A 111.9(18) . . ? C19A N17A C18A 106.2(18) . . ? C19A N17A C16A 106.7(14) . . ? C18A N17A C16A 116(2) . . ? C19A N17A Pd3A 111.2(14) . . ? C18A N17A Pd3A 110.0(15) . . ? C16A N17A Pd3A 106.3(13) . . ? N17A C19A C20A 114.2(19) . . ? C21A C20A C19A 109(2) . . ? N22A C21A C20A 115.4(19) . . ? C21A N22A C24A 108.0(14) . . ? C21A N22A C23A 109.0(18) . . ? C24A N22A C23A 104.7(19) . . ? C21A N22A Pd3A 112.1(15) . . ? C24A N22A Pd3A 110.0(12) . . ? C23A N22A Pd3A 112.7(15) . . ? N22A C24A C25A 111.3(16) . . ? C24A C25A S26A 106.0(15) . . ? C25A S26A Pd3A 97.5(6) . . ? C25A S26A Pd2A 107.6(6) . 2_655 ? Pd3A S26A Pd2A 115.4(2) . 2_655 ? F2 B1 F1 109.2(15) . . ? F2 B1 F4 111.3(14) . . ? F1 B1 F4 107.4(14) . . ? F2 B1 F3 110.6(14) . . ? F1 B1 F3 107.5(14) . . ? F4 B1 F3 110.6(14) . . ? F7 B2 F6 111.4(14) . . ? F7 B2 F8 109.2(13) . . ? F6 B2 F8 109.1(13) . . ? F7 B2 F5A 135.2(17) . . ? F8 B2 F5A 114.6(14) . . ? F7 B2 F5 109.1(13) . . ? F6 B2 F5 110.3(14) . . ? F8 B2 F5 107.6(13) . . ? F8 B2 F7A 115.0(15) . . ? F5A B2 F7A 106.1(15) . . ? F8 B2 F6A 109.7(14) . . ? F5A B2 F6A 106.0(15) . . ? F7A B2 F6A 104.6(15) . . ? F9' B3 F11' 112.9(15) . . ? F9' B3 F10' 108.2(14) . . ? F11' B3 F10' 108.5(14) . . ? F9' B3 F12' 111.3(15) . . ? F11' B3 F12' 108.1(15) . . ? F10' B3 F12' 107.6(15) . . ? F11' B3 F12 118(2) . . ? F10' B3 F12 124(2) . . ? F11 B3 F12 111.1(14) . . ? F12' B3 F10 118(2) . . ? F11 B3 F10 110.8(14) . . ? F12 B3 F10 111.8(14) . . ? F10' B3 F9 125(2) . . ? F12' B3 F9 127(2) . . ? F11 B3 F9 109.1(14) . . ? F12 B3 F9 107.0(14) . . ? F10 B3 F9 107.0(14) . . ? F15 B4 F16 112.0(12) . . ? F15 B4 F13 111.5(14) . . ? F16 B4 F13 108.3(13) . . ? F15 B4 F14 108.6(13) . . ? F16 B4 F14 107.0(12) . . ? F13 B4 F14 109.3(14) . . ? F16 B4 F13A 114.1(13) . . ? F14A B4 F13A 109.7(14) . . ? F16 B4 F15A 109.7(12) . . ? F14A B4 F15A 108.5(13) . . ? F13A B4 F15A 105.8(13) . . ? N1S C2S C3S 173(3) . . ? N4S C5S C6S 171(3) . . ? N7S C8S C9S 172(3) . . ? N10S C11S C12S 175(5) . . ? N13S C14S C15S 164(6) . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 5.39 _refine_diff_density_min -1.46 _refine_diff_density_rms 0.27 data_nicus8 _database_code_CSD 207887 _audit_creation_method SHELXL-97 _chemical_name_systematic ; Tris-Nickel 3,7-dithianonane-1,9-dithiolate bis-copper hexaflurophosphate ; _chemical_name_common ;Tris-Nickel 3,7-dithianonane-1,9-dithiolate bis-copper hexaflurophosphate ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C17 H34 Cu2 F12 Ni3 P2 S12' _chemical_formula_weight 1216.32 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' F F 0.0171 0.0103 '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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 '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 orthorhombic _symmetry_space_group_name_H-M Pnma loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z' '-x-1/2, y-1/2, z-1/2' _cell_length_a 17.466(3) _cell_length_b 22.546(7) _cell_length_c 12.156(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4787(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 38 _cell_measurement_theta_min 10.5 _cell_measurement_theta_max 16.5 _exptl_crystal_description tablet _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.688 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2432 _exptl_absorpt_coefficient_mu 2.683 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.499 _exptl_absorpt_correction_T_max 0.565 _exptl_absorpt_process_details 'X-RED (Stoe & Cie, 1997b)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Stoe Stadi-4 four-circle' _diffrn_measurement_method omega-theta _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time '60 min' _diffrn_standards_decay_% '+/- 6.5% linear increase' _diffrn_reflns_number 4591 _diffrn_reflns_av_R_equivalents 0.0238 _diffrn_reflns_av_sigmaI/netI 0.0828 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -1 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.73 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4324 _reflns_number_gt 2788 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STADI-4 (Stoe & Cie, 1996a)' _computing_cell_refinement 'STADI-4 (Stoe & Cie, 1996a)' _computing_data_reduction 'X-RED (Stoe & Cie, 1996b)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL/PC (Sheldrick, 1994)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.1025P)^2^+179.22P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary 'difference Fourier syntheses' _atom_sites_solution_hydrogens 'geometrically located' _refine_ls_hydrogen_treatment 'riding model' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4324 _refine_ls_number_parameters 262 _refine_ls_number_restraints 144 _refine_ls_R_factor_all 0.187 _refine_ls_R_factor_gt 0.127 _refine_ls_wR_factor_ref 0.354 _refine_ls_wR_factor_gt 0.296 _refine_ls_goodness_of_fit_ref 1.20 _refine_ls_restrained_S_all 1.18 _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 Ni1 Ni -0.23279(19) 0.2500 0.5497(3) 0.0224(9) Uani 0.725(3) 2 d SPU . 1 Ni2 Ni -0.28619(19) 0.2500 0.1469(3) 0.0189(8) Uani 0.725(3) 2 d SPU . 1 Ni3 Ni -0.5039(2) 0.2500 0.3836(3) 0.0222(9) Uani 0.725(3) 2 d SPU . 1 Cu Cu -0.33491(14) 0.31614(12) 0.3532(2) 0.0264(7) Uani 0.725(3) 1 d PU . 1 S11 S -0.3225(3) 0.3175(3) 0.5413(5) 0.0297(12) Uani 0.725(3) 1 d PDU . 1 S41 S -0.1463(3) 0.3183(3) 0.5702(4) 0.0268(12) Uani 0.725(3) 1 d PDU . 1 S12 S -0.2288(3) 0.3180(2) 0.2431(4) 0.0246(12) Uani 0.725(3) 1 d PDU . 1 S42 S -0.3413(3) 0.3165(3) 0.0409(4) 0.0238(11) Uani 0.725(3) 1 d PDU . 1 S13 S -0.4548(3) 0.3175(3) 0.2771(4) 0.0266(12) Uani 0.725(3) 1 d PDU . 1 S43 S -0.5587(3) 0.3173(3) 0.4840(5) 0.0276(13) Uani 0.725(3) 1 d PDU . 1 C21 C -0.2700(9) 0.3853(7) 0.5732(18) 0.035(5) Uiso 0.725(3) 1 d PDU . 1 H21A H -0.2993 0.4196 0.5447 0.042 Uiso 0.725(3) 1 calc PR . 1 H21B H -0.2667 0.3895 0.6542 0.042 Uiso 0.725(3) 1 calc PR . 1 C31 C -0.1892(8) 0.3873(6) 0.5254(15) 0.019(4) Uiso 0.725(3) 1 d PDU . 1 H31A H -0.1604 0.4217 0.5544 0.022 Uiso 0.725(3) 1 calc PR . 1 H31B H -0.1906 0.3896 0.4441 0.022 Uiso 0.725(3) 1 calc PR . 1 C51 C -0.0712(9) 0.3083(7) 0.4678(14) 0.028(5) Uiso 0.725(3) 1 d PDU . 1 H51A H -0.0941 0.3086 0.3933 0.034 Uiso 0.725(3) 1 calc PR . 1 H51B H -0.0345 0.3417 0.4726 0.034 Uiso 0.725(3) 1 calc PR . 1 C61 C -0.0287(14) 0.2500 0.486(2) 0.020(6) Uiso 0.725(3) 2 d SPDU . 1 H61A H 0.0164 0.2500 0.4363 0.024 Uiso 0.725(3) 2 calc SPR . 1 H61B H -0.0091 0.2500 0.5620 0.024 Uiso 0.725(3) 2 calc SPR . 1 C22 C -0.2340(10) 0.3827(7) 0.1534(16) 0.035(5) Uiso 0.725(3) 1 d PDU . 1 H22A H -0.2252 0.4190 0.1975 0.042 Uiso 0.725(3) 1 calc PR . 1 H22B H -0.1931 0.3802 0.0973 0.042 Uiso 0.725(3) 1 calc PR . 1 C32 C -0.3111(10) 0.3871(10) 0.0965(18) 0.028(5) Uiso 0.725(3) 1 d PDU . 1 H32A H -0.3077 0.4165 0.0362 0.034 Uiso 0.725(3) 1 calc PR . 1 H32B H -0.3498 0.4014 0.1497 0.034 Uiso 0.725(3) 1 calc PR . 1 C52 C -0.2822(10) 0.3060(7) -0.0817(12) 0.024(4) Uiso 0.725(3) 1 d PDU . 1 H52A H -0.2889 0.3408 -0.1305 0.029 Uiso 0.725(3) 1 calc PR . 1 H52B H -0.2278 0.3048 -0.0590 0.029 Uiso 0.725(3) 1 calc PR . 1 C62 C -0.3002(17) 0.2500 -0.147(2) 0.029(7) Uiso 0.725(3) 2 d SPDU . 1 H62A H -0.2698 0.2500 -0.2158 0.035 Uiso 0.725(3) 2 calc SPR . 1 H62B H -0.3551 0.2500 -0.1674 0.035 Uiso 0.725(3) 2 calc SPR . 1 C23 C -0.5003(12) 0.3853(7) 0.3254(14) 0.030(5) Uiso 0.725(3) 1 d PDU . 1 H23A H -0.4690 0.4198 0.3027 0.036 Uiso 0.725(3) 1 calc PR . 1 H23B H -0.5512 0.3892 0.2902 0.036 Uiso 0.725(3) 1 calc PR . 1 C33 C -0.5100(13) 0.3863(7) 0.4496(14) 0.041(6) Uiso 0.725(3) 1 d PDU . 1 H33A H -0.5411 0.4209 0.4725 0.049 Uiso 0.725(3) 1 calc PR . 1 H33B H -0.4596 0.3884 0.4866 0.049 Uiso 0.725(3) 1 calc PR . 1 C53 C -0.5316(11) 0.3084(7) 0.6273(9) 0.027(5) Uiso 0.725(3) 1 d PDU . 1 H53A H -0.4751 0.3078 0.6346 0.033 Uiso 0.725(3) 1 calc PR . 1 H53B H -0.5520 0.3416 0.6718 0.033 Uiso 0.725(3) 1 calc PR . 1 C63 C -0.5653(14) 0.2500 0.666(2) 0.021(6) Uiso 0.725(3) 2 d SPDU . 1 H63A H -0.6201 0.2500 0.6452 0.025 Uiso 0.725(3) 2 calc SPR . 1 H63B H -0.5632 0.2500 0.7474 0.025 Uiso 0.725(3) 2 calc SPR . 1 Ni1' Ni -0.0759(5) 0.2500 0.1487(8) 0.017(2) Uani 0.275(3) 2 d SPU . 2 Ni2' Ni 0.1398(5) 0.2500 0.3921(7) 0.017(2) Uani 0.275(3) 2 d SPU . 2 Ni3' Ni -0.1349(5) 0.2500 0.5513(8) 0.018(2) Uani 0.275(3) 2 d SPU . 2 Cu' Cu -0.0315(4) 0.3267(5) 0.3586(6) 0.045(3) Uani 0.275(3) 1 d PU . 2 S11' S 0.0904(7) 0.3184(6) 0.2853(11) 0.022(3) Uiso 0.275(3) 1 d PDU . 2 S41' S 0.1946(9) 0.3169(6) 0.4917(13) 0.021(3) Uiso 0.275(3) 1 d PDU . 2 S12' S -0.0446(7) 0.3194(6) 0.5428(11) 0.021(3) Uiso 0.275(3) 1 d PU . 2 S42' S -0.2225(7) 0.3184(6) 0.5676(11) 0.021(3) Uiso 0.275(3) 1 d PU . 2 S13' S -0.1334(7) 0.3185(6) 0.2429(11) 0.023(3) Uiso 0.275(3) 1 d PDU . 2 S43' S -0.0218(9) 0.3171(6) 0.0405(12) 0.018(3) Uiso 0.275(3) 1 d PDU . 2 C21' C 0.142(3) 0.3837(16) 0.332(4) 0.033(14) Uiso 0.275(3) 1 d PDU . 2 C31' C 0.154(3) 0.3887(14) 0.456(4) 0.037(15) Uiso 0.275(3) 1 d PDU . 2 C23' C -0.127(2) 0.3818(14) 0.150(3) 0.015(10) Uiso 0.275(3) 1 d PDU . 2 C33' C -0.052(2) 0.3897(11) 0.090(5) 0.036(14) Uiso 0.275(3) 1 d PDU . 2 C53' C -0.085(2) 0.306(2) -0.077(3) 0.022(12) Uiso 0.275(3) 1 d PDU . 2 P P 0.1752(3) 0.51936(19) 0.1497(4) 0.0439(13) Uani 1 1 d DU . . F1 F 0.2646(5) 0.5171(6) 0.1410(13) 0.142(7) Uani 1 1 d DU . . F2 F 0.1817(8) 0.5159(5) 0.2782(7) 0.097(5) Uani 1 1 d DU . . F3 F 0.1714(7) 0.4498(4) 0.1437(8) 0.085(4) Uani 1 1 d DU . . F4 F 0.1778(7) 0.5889(4) 0.1558(11) 0.101(5) Uani 1 1 d DU . . F5 F 0.1702(8) 0.5233(5) 0.0213(7) 0.110(5) Uani 1 1 d DU . . F6 F 0.0855(5) 0.5221(6) 0.1584(11) 0.109(5) Uani 1 1 d DU . . 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 Ni1 0.0127(16) 0.037(2) 0.0180(18) 0.000 0.0010(14) 0.000 Ni2 0.0160(16) 0.0219(19) 0.0189(18) 0.000 -0.0039(14) 0.000 Ni3 0.0140(17) 0.033(2) 0.0191(19) 0.000 -0.0031(14) 0.000 Cu 0.0189(12) 0.0329(15) 0.0274(14) -0.0003(12) 0.0004(10) -0.0006(11) S11 0.020(2) 0.042(3) 0.027(3) 0.003(3) 0.000(2) 0.007(2) S41 0.014(2) 0.043(3) 0.023(3) -0.008(2) 0.000(2) -0.002(2) S12 0.018(2) 0.031(3) 0.025(3) -0.006(2) -0.003(2) -0.003(2) S42 0.021(3) 0.032(3) 0.019(3) 0.000(2) 0.002(2) 0.004(2) S13 0.019(2) 0.038(3) 0.022(3) 0.000(2) -0.001(2) -0.003(2) S43 0.015(3) 0.042(4) 0.026(3) -0.003(2) 0.001(2) 0.003(2) Ni1' 0.016(4) 0.016(5) 0.019(5) 0.000 0.012(4) 0.000 Ni2' 0.011(4) 0.026(5) 0.013(5) 0.000 -0.004(3) 0.000 Ni3' 0.010(4) 0.025(5) 0.018(5) 0.000 0.002(4) 0.000 Cu' 0.016(3) 0.099(7) 0.020(4) 0.008(4) 0.001(3) 0.004(4) P 0.052(3) 0.034(2) 0.046(3) 0.011(2) 0.000(2) 0.007(2) F1 0.051(6) 0.154(14) 0.220(17) 0.022(17) 0.008(8) 0.031(7) F2 0.192(14) 0.046(7) 0.054(6) -0.013(5) -0.029(8) 0.000(10) F3 0.177(13) 0.034(5) 0.044(7) -0.005(5) -0.022(9) 0.006(7) F4 0.132(12) 0.030(5) 0.142(12) 0.019(6) 0.032(12) 0.006(6) F5 0.186(15) 0.096(10) 0.049(6) 0.032(6) 0.013(7) 0.048(12) F6 0.055(6) 0.129(12) 0.142(13) 0.024(13) 0.009(7) -0.003(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 Ni1 S41 2.171(6) . y Ni1 S41 2.171(6) 7_565 ? Ni1 S11 2.186(6) 7_565 ? Ni1 S11 2.186(6) . y Ni2 S12 2.174(6) . y Ni2 S12 2.174(6) 7_565 ? Ni2 S42 2.200(6) 7_565 ? Ni2 S42 2.200(6) . y Ni3 S43 2.170(7) 7_565 ? Ni3 S43 2.170(7) . y Ni3 S13 2.174(6) 7_565 ? Ni3 S13 2.174(6) . y Cu S12 2.287(6) . y Cu S13 2.289(6) . y Cu S11 2.297(6) . y Cu Cu 2.983(6) 7_565 ? S11 C21 1.825(9) . ? S41 C31 1.810(9) . ? S41 C51 1.823(9) . ? S12 C22 1.823(9) . ? S42 C32 1.81(2) . ? S42 C52 1.828(9) . ? S13 C23 1.820(9) . ? S43 C53 1.816(9) . ? S43 C33 1.820(9) . ? C21 C31 1.527(10) . ? C51 C61 1.525(9) . ? C61 C51 1.525(9) 7_565 ? C22 C32 1.517(10) . ? C52 C62 1.525(9) . ? C62 C52 1.525(9) 7_565 ? C23 C33 1.520(10) . ? C53 C63 1.517(9) . ? C63 C53 1.517(9) 7_565 ? Ni1' S13' 2.169(15) 7_565 ? Ni1' S13' 2.169(15) . ? Ni1' S43' 2.215(15) . ? Ni1' S43' 2.215(15) 7_565 ? Ni2' S41' 2.157(17) . ? Ni2' S41' 2.157(17) 7_565 ? Ni2' S11' 2.192(15) 7_565 ? Ni2' S11' 2.192(15) . ? Ni3' S42' 2.181(15) 7_565 ? Ni3' S42' 2.181(15) . ? Ni3' S12' 2.224(14) . ? Ni3' S12' 2.224(14) 7_565 ? Cu' S12' 2.257(15) . ? Cu' S13' 2.276(15) . ? Cu' S11' 2.315(15) . ? S11' C21' 1.820(10) . ? S41' C31' 1.820(10) . ? S13' C23' 1.821(10) . ? S43' C33' 1.820(10) . ? S43' C53' 1.821(10) . ? C21' C31' 1.521(10) . ? C23' C33' 1.520(10) . ? P F5 1.565(8) . ? P F1 1.566(8) . ? P F2 1.568(8) . ? P F6 1.571(8) . ? P F4 1.571(8) . ? P F3 1.572(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 S41 Ni1 S41 90.3(3) . 7_565 ? S41 Ni1 S11 175.8(3) . 7_565 ? S41 Ni1 S11 90.6(2) 7_565 7_565 ? S41 Ni1 S11 90.6(2) . . y S41 Ni1 S11 175.8(3) 7_565 . ? S11 Ni1 S11 88.2(3) 7_565 . ? S12 Ni2 S12 89.7(3) . 7_565 ? S12 Ni2 S42 176.7(3) . 7_565 ? S12 Ni2 S42 92.1(2) 7_565 7_565 ? S12 Ni2 S42 92.1(2) . . y S12 Ni2 S42 176.7(3) 7_565 . ? S42 Ni2 S42 86.0(3) 7_565 . ? S43 Ni3 S43 88.8(4) 7_565 . ? S43 Ni3 S13 91.1(2) 7_565 7_565 ? S43 Ni3 S13 176.7(3) . 7_565 ? S43 Ni3 S13 176.7(3) 7_565 . ? S43 Ni3 S13 91.1(2) . . y S13 Ni3 S13 88.9(3) 7_565 . ? S12 Cu S13 120.3(2) . . y S12 Cu S11 120.4(2) . . y S13 Cu S11 119.2(2) . . y S12 Cu Cu 91.05(15) . 7_565 ? S13 Cu Cu 90.77(16) . 7_565 ? S11 Cu Cu 90.73(17) . 7_565 ? C21 S11 Ni1 102.3(7) . . y C21 S11 Cu 105.7(8) . . y Ni1 S11 Cu 96.0(2) . . y C31 S41 C51 101.4(7) . . ? C31 S41 Ni1 106.7(6) . . y C51 S41 Ni1 109.6(7) . . y C22 S12 Ni2 102.7(7) . . y C22 S12 Cu 108.9(7) . . y Ni2 S12 Cu 85.9(2) . . y C32 S42 C52 104.7(9) . . ? C32 S42 Ni2 104.7(6) . . y C52 S42 Ni2 98.1(7) . . y C23 S13 Ni3 102.9(7) . . y C23 S13 Cu 106.3(7) . . y Ni3 S13 Cu 96.4(2) . . y C53 S43 C33 101.2(8) . . ? C53 S43 Ni3 110.3(7) . . y C33 S43 Ni3 105.2(8) . . y C31 C21 S11 114.1(11) . . ? C21 C31 S41 104.0(11) . . ? C61 C51 S41 111.1(14) . . ? C51 C61 C51 119(2) 7_565 . ? C32 C22 S12 111.7(13) . . ? C22 C32 S42 111.8(15) . . ? C62 C52 S42 114.6(15) . . ? C52 C62 C52 112(2) . 7_565 ? C33 C23 S13 112.4(13) . . ? C23 C33 S43 105.5(12) . . ? C63 C53 S43 107.0(14) . . ? C53 C63 C53 120(2) . 7_565 ? S13' Ni1' S13' 90.9(8) 7_565 . ? S13' Ni1' S43' 175.3(7) 7_565 . ? S13' Ni1' S43' 91.4(5) . . ? S13' Ni1' S43' 91.4(5) 7_565 7_565 ? S13' Ni1' S43' 175.3(7) . 7_565 ? S43' Ni1' S43' 86.1(8) . 7_565 ? S41' Ni2' S41' 88.7(9) . 7_565 ? S41' Ni2' S11' 176.7(7) . 7_565 ? S41' Ni2' S11' 90.9(5) 7_565 7_565 ? S41' Ni2' S11' 90.9(5) . . ? S41' Ni2' S11' 176.7(7) 7_565 . ? S11' Ni2' S11' 89.4(8) 7_565 . ? S42' Ni3' S42' 90.0(8) 7_565 . ? S42' Ni3' S12' 177.4(7) 7_565 . ? S42' Ni3' S12' 90.3(5) . . ? S42' Ni3' S12' 90.3(5) 7_565 7_565 ? S42' Ni3' S12' 177.4(7) . 7_565 ? S12' Ni3' S12' 89.4(7) . 7_565 ? S12' Cu' S13' 121.9(6) . . ? S12' Cu' S11' 118.0(5) . . ? S13' Cu' S11' 118.4(6) . . ? C21' S11' Ni2' 100.8(18) . . ? C21' S11' Cu' 105.7(19) . . ? Ni2' S11' Cu' 101.0(6) . . ? C31' S41' Ni2' 108.4(19) . . ? Ni3' S12' Cu' 99.7(6) . . ? C23' S13' Ni1' 101.7(15) . . ? C23' S13' Cu' 105.8(15) . . ? Ni1' S13' Cu' 91.2(6) . . ? C33' S43' C53' 102(3) . . ? C33' S43' Ni1' 107.2(16) . . ? C53' S43' Ni1' 96.9(18) . . ? C31' C21' S11' 116(3) . . ? C21' C31' S41' 103(3) . . ? C33' C23' S13' 116(3) . . ? C23' C33' S43' 108(3) . . ? F5 P F1 89.4(6) . . ? F5 P F2 179.0(7) . . ? F1 P F2 89.7(6) . . ? F5 P F6 90.5(6) . . ? F1 P F6 179.6(7) . . ? F2 P F6 90.4(6) . . ? F5 P F4 89.5(5) . . ? F1 P F4 90.4(6) . . ? F2 P F4 90.0(5) . . ? F6 P F4 89.2(6) . . ? F5 P F3 90.5(5) . . ? F1 P F3 90.4(6) . . ? F2 P F3 90.0(5) . . ? F6 P F3 90.0(6) . . ? F4 P F3 179.2(6) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.54 _refine_diff_density_min -0.94 _refine_diff_density_rms 0.23