# 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_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email krautscheid@rz.uni-leipzig.de _publ_contact_author_name 'Krautscheid, Harald' loop_ _publ_author_name 'Kluge, Oliver' 'Wagner, Gerald' 'Friedrich, Dirk' 'Krautscheid, Harald' data_1 _database_code_depnum_ccdc_archive 'CCDC 879009' #TrackingRef '- 1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; bis(\m~2~-ethane-1,2-disulfido)-tetrakis(triisopropylphosphine)-tetra-copper ; _chemical_formula_moiety 'C40 H92 Cu4 P4 S4' _chemical_formula_sum 'C40 H92 Cu4 P4 S4' _chemical_formula_weight 1079.42 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' 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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.4153(6) _cell_length_b 21.1400(10) _cell_length_c 11.0770(6) _cell_angle_alpha 90.00 _cell_angle_beta 100.105(5) _cell_angle_gamma 90.00 _cell_volume 2631.6(2) _cell_formula_units_Z 2 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 22655 _cell_measurement_theta_min 1.81 _cell_measurement_theta_max 29.65 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.362 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1144 _exptl_absorpt_coefficient_mu 1.900 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.5857 _exptl_absorpt_correction_T_max 0.7540 _exptl_absorpt_process_details 'STOE X-RED' loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist -1 1 0 0.1178 0 1 0 0.1184 -1 0 0 0.0750 1 0 0 0.0731 0 -1 0 0.1368 1 -2 -3 0.1530 1 1 -2 0.2030 2 3 -3 0.2057 0 0 1 0.1353 -1 0 2 0.1310 _diffrn_measurement_device '2-circle goniometer' _diffrn_measurement_device_type 'STOE IPDS 2T' _diffrn_detector 'image plate (34 cm diameter / schwenk)' _diffrn_detector_type STOE _diffrn_detector_area_resol_mean 6.67 _diffrn_source 'sealed X-ray tube, 12 x 0.4 mm long-fine focus' _diffrn_source_voltage 50 _diffrn_source_current 40 _diffrn_source_power 2.00 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_monochromator 'plane graphite' _diffrn_radiation_polarisn_norm 0 _diffrn_radiation_collimation '0.5 mm diameter, multiple pinhole' _diffrn_ambient_temperature 180(2) _diffrn_measurement_method 'rotation method' _diffrn_measurement_details ; 175 frames, detector distance = 100 mm ; _diffrn_reflns_number 15748 _diffrn_reflns_av_R_equivalents 0.0235 _diffrn_reflns_av_sigmaI/netI 0.0226 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.81 _diffrn_reflns_theta_max 27.00 _reflns_number_total 5733 _reflns_number_gt 4921 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE X-AREA' _computing_cell_refinement 'STOE X-AREA' _computing_data_reduction 'STOE X-RED' _computing_structure_solution 'SIR 92' _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^)+(0.0245P)^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 5733 _refine_ls_number_parameters 247 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0268 _refine_ls_R_factor_gt 0.0197 _refine_ls_wR_factor_ref 0.0439 _refine_ls_wR_factor_gt 0.0427 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.021 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.414457(15) 0.601945(8) 0.409167(14) 0.02197(5) Uani 1 1 d . . . Cu2 Cu 0.287032(14) 0.446689(8) 0.401704(14) 0.02237(5) Uani 1 1 d . . . S1 S 0.29911(3) 0.539354(17) 0.50484(3) 0.02246(7) Uani 1 1 d . . . S2 S 0.55603(3) 0.622821(17) 0.57580(3) 0.02299(7) Uani 1 1 d . . . P1 P 0.40453(3) 0.651998(17) 0.23409(3) 0.02244(8) Uani 1 1 d . . . P2 P 0.10963(3) 0.420792(17) 0.29009(3) 0.02117(7) Uani 1 1 d . . . C1 C 0.40938(12) 0.52847(7) 0.64479(12) 0.0228(3) Uani 1 1 d . . . H1A H 0.3700 0.5122 0.7092 0.027 Uiso 1 1 calc R . . H1B H 0.4676 0.4974 0.6296 0.027 Uiso 1 1 calc R . . C2 C 0.47264(12) 0.58976(7) 0.68758(11) 0.0233(3) Uani 1 1 d . . . H2A H 0.5269 0.5821 0.7639 0.028 Uiso 1 1 calc R . . H2B H 0.4143 0.6205 0.7038 0.028 Uiso 1 1 calc R . . C3 C 0.54905(14) 0.68502(8) 0.21112(15) 0.0359(4) Uani 1 1 d . . . H3 H 0.5391 0.7050 0.1301 0.043 Uiso 1 1 calc R . . C4 C 0.64066(16) 0.63139(10) 0.21703(19) 0.0488(5) Uani 1 1 d . . . H4A H 0.7157 0.6485 0.2050 0.073 Uiso 1 1 calc R . . H4B H 0.6135 0.6010 0.1540 0.073 Uiso 1 1 calc R . . H4C H 0.6500 0.6112 0.2958 0.073 Uiso 1 1 calc R . . C5 C 0.59318(16) 0.73443(9) 0.30889(17) 0.0460(4) Uani 1 1 d . . . H5A H 0.5902 0.7173 0.3885 0.069 Uiso 1 1 calc R . . H5B H 0.5434 0.7713 0.2955 0.069 Uiso 1 1 calc R . . H5C H 0.6736 0.7458 0.3042 0.069 Uiso 1 1 calc R . . C6 C 0.34238(14) 0.60886(7) 0.09088(12) 0.0288(3) Uani 1 1 d . . . H6 H 0.2562 0.6157 0.0775 0.035 Uiso 1 1 calc R . . C7 C 0.36111(17) 0.53764(8) 0.10685(14) 0.0380(4) Uani 1 1 d . . . H7A H 0.3193 0.5161 0.0358 0.057 Uiso 1 1 calc R . . H7B H 0.3313 0.5238 0.1782 0.057 Uiso 1 1 calc R . . H7C H 0.4445 0.5282 0.1165 0.057 Uiso 1 1 calc R . . C8 C 0.38386(19) 0.63078(10) -0.02596(14) 0.0468(5) Uani 1 1 d . . . H8A H 0.4672 0.6219 -0.0200 0.070 Uiso 1 1 calc R . . H8B H 0.3707 0.6755 -0.0362 0.070 Uiso 1 1 calc R . . H8C H 0.3399 0.6088 -0.0952 0.070 Uiso 1 1 calc R . . C9 C 0.30721(14) 0.72277(7) 0.23234(14) 0.0319(3) Uani 1 1 d . . . H9 H 0.3480 0.7513 0.2959 0.038 Uiso 1 1 calc R . . C10 C 0.19045(15) 0.70495(8) 0.27133(15) 0.0376(4) Uani 1 1 d . . . H10A H 0.1464 0.7426 0.2818 0.056 Uiso 1 1 calc R . . H10B H 0.2064 0.6822 0.3474 0.056 Uiso 1 1 calc R . . H10C H 0.1448 0.6788 0.2095 0.056 Uiso 1 1 calc R . . C11 C 0.28585(17) 0.76100(8) 0.11287(17) 0.0447(4) Uani 1 1 d . . . H11A H 0.2385 0.7366 0.0493 0.067 Uiso 1 1 calc R . . H11B H 0.3609 0.7709 0.0895 0.067 Uiso 1 1 calc R . . H11C H 0.2448 0.7995 0.1250 0.067 Uiso 1 1 calc R . . C12 C 0.04485(13) 0.35393(7) 0.36435(13) 0.0289(3) Uani 1 1 d . . . H12 H -0.0327 0.3433 0.3152 0.035 Uiso 1 1 calc R . . C13 C 0.02648(17) 0.37306(9) 0.49329(15) 0.0422(4) Uani 1 1 d . . . H13A H 0.0047 0.3365 0.5357 0.063 Uiso 1 1 calc R . . H13B H -0.0357 0.4041 0.4871 0.063 Uiso 1 1 calc R . . H13C H 0.0990 0.3906 0.5378 0.063 Uiso 1 1 calc R . . C14 C 0.12579(16) 0.29605(8) 0.36997(17) 0.0415(4) Uani 1 1 d . . . H14A H 0.2034 0.3065 0.4143 0.062 Uiso 1 1 calc R . . H14B H 0.1321 0.2832 0.2882 0.062 Uiso 1 1 calc R . . H14C H 0.0928 0.2621 0.4109 0.062 Uiso 1 1 calc R . . C15 C 0.09553(13) 0.39892(7) 0.12441(12) 0.0280(3) Uani 1 1 d . . . H15 H 0.0756 0.4381 0.0780 0.034 Uiso 1 1 calc R . . C16 C 0.21333(15) 0.37660(9) 0.09368(15) 0.0375(4) Uani 1 1 d . . . H16A H 0.2362 0.3376 0.1358 0.056 Uiso 1 1 calc R . . H16B H 0.2733 0.4080 0.1190 0.056 Uiso 1 1 calc R . . H16C H 0.2050 0.3700 0.0068 0.056 Uiso 1 1 calc R . . C17 C -0.00344(15) 0.35166(10) 0.07582(15) 0.0433(4) Uani 1 1 d . . . H17A H -0.0104 0.3479 -0.0115 0.065 Uiso 1 1 calc R . . H17B H -0.0775 0.3664 0.0954 0.065 Uiso 1 1 calc R . . H17C H 0.0156 0.3111 0.1132 0.065 Uiso 1 1 calc R . . C18 C 0.00050(13) 0.48598(7) 0.28790(13) 0.0281(3) Uani 1 1 d . . . H18 H -0.0034 0.4953 0.3738 0.034 Uiso 1 1 calc R . . C19 C 0.04771(15) 0.54570(8) 0.23586(15) 0.0349(3) Uani 1 1 d . . . H19A H 0.0513 0.5393 0.1508 0.052 Uiso 1 1 calc R . . H19B H 0.1259 0.5549 0.2801 0.052 Uiso 1 1 calc R . . H19C H -0.0044 0.5805 0.2439 0.052 Uiso 1 1 calc R . . C20 C -0.12708(14) 0.47250(9) 0.22475(18) 0.0432(4) Uani 1 1 d . . . H20A H -0.1766 0.5082 0.2348 0.065 Uiso 1 1 calc R . . H20B H -0.1563 0.4357 0.2608 0.065 Uiso 1 1 calc R . . H20C H -0.1286 0.4651 0.1390 0.065 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 Cu1 0.02292(8) 0.02577(9) 0.01639(7) 0.00102(6) 0.00111(6) 0.00223(7) Cu2 0.01884(8) 0.02762(9) 0.01979(8) -0.00064(6) 0.00102(6) -0.00280(7) S1 0.01805(15) 0.02547(17) 0.02245(15) -0.00081(12) -0.00037(12) -0.00038(13) S2 0.01988(15) 0.02527(17) 0.02216(15) -0.00040(12) -0.00085(12) -0.00180(13) P1 0.02421(17) 0.02450(18) 0.01748(15) 0.00145(13) 0.00058(12) -0.00233(14) P2 0.01767(15) 0.02397(17) 0.02065(15) -0.00216(13) -0.00003(12) -0.00168(13) C1 0.0207(6) 0.0279(7) 0.0194(6) 0.0031(5) 0.0028(5) 0.0014(5) C2 0.0232(6) 0.0292(7) 0.0166(6) -0.0028(5) 0.0009(5) 0.0022(5) C3 0.0316(8) 0.0417(9) 0.0338(8) 0.0078(7) 0.0042(6) -0.0103(7) C4 0.0313(9) 0.0588(13) 0.0590(11) 0.0026(10) 0.0151(8) -0.0024(8) C5 0.0410(9) 0.0404(10) 0.0526(10) 0.0039(8) -0.0031(8) -0.0178(8) C6 0.0342(8) 0.0309(8) 0.0197(6) -0.0006(5) 0.0002(6) -0.0011(6) C7 0.0511(10) 0.0311(9) 0.0295(7) -0.0049(6) 0.0006(7) 0.0020(7) C8 0.0674(12) 0.0530(11) 0.0202(7) 0.0008(7) 0.0081(7) -0.0103(9) C9 0.0364(8) 0.0250(7) 0.0312(7) -0.0025(6) -0.0027(6) -0.0008(6) C10 0.0374(8) 0.0351(9) 0.0397(8) -0.0016(7) 0.0051(7) 0.0082(7) C11 0.0493(10) 0.0312(9) 0.0497(10) 0.0142(8) -0.0018(8) 0.0011(8) C12 0.0251(7) 0.0304(8) 0.0308(7) 0.0017(6) 0.0037(6) -0.0052(6) C13 0.0469(10) 0.0475(11) 0.0340(8) 0.0046(7) 0.0123(7) -0.0063(8) C14 0.0424(9) 0.0295(9) 0.0529(10) 0.0068(7) 0.0091(8) -0.0012(7) C15 0.0296(7) 0.0308(8) 0.0220(6) -0.0035(6) -0.0001(5) 0.0002(6) C16 0.0380(9) 0.0408(9) 0.0355(8) -0.0068(7) 0.0114(7) 0.0001(7) C17 0.0376(9) 0.0563(11) 0.0329(8) -0.0163(8) -0.0023(7) -0.0103(8) C18 0.0253(7) 0.0305(8) 0.0280(7) -0.0014(6) 0.0035(5) 0.0031(6) C19 0.0345(8) 0.0300(8) 0.0386(8) 0.0028(7) 0.0020(7) 0.0048(7) C20 0.0219(7) 0.0492(11) 0.0572(11) 0.0016(8) 0.0036(7) 0.0066(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 P1 2.1946(4) . ? Cu1 S1 2.2578(4) . ? Cu1 S2 2.2731(4) . ? Cu2 P2 2.2474(4) . ? Cu2 S1 2.2597(4) . ? Cu2 S2 2.2965(4) 3_666 ? S1 C1 1.8319(12) . ? S2 C2 1.8279(15) . ? S2 Cu2 2.2965(4) 3_666 ? P1 C3 1.8497(16) . ? P1 C6 1.8591(14) . ? P1 C9 1.8616(16) . ? P2 C12 1.8532(16) . ? P2 C18 1.8551(15) . ? P2 C15 1.8719(14) . ? C1 C2 1.5181(19) . ? C3 C5 1.525(2) . ? C3 C4 1.536(3) . ? C6 C8 1.526(2) . ? C6 C7 1.527(2) . ? C9 C10 1.519(2) . ? C9 C11 1.533(2) . ? C12 C14 1.528(2) . ? C12 C13 1.534(2) . ? C15 C16 1.519(2) . ? C15 C17 1.533(2) . ? C18 C19 1.525(2) . ? C18 C20 1.528(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 P1 Cu1 S1 138.885(14) . . ? P1 Cu1 S2 122.895(15) . . ? S1 Cu1 S2 97.050(13) . . ? P2 Cu2 S1 117.287(15) . . ? P2 Cu2 S2 120.950(15) . 3_666 ? S1 Cu2 S2 121.507(13) . 3_666 ? C1 S1 Cu1 95.74(5) . . ? C1 S1 Cu2 106.91(5) . . ? Cu1 S1 Cu2 105.046(16) . . ? C2 S2 Cu1 95.46(4) . . ? C2 S2 Cu2 99.84(5) . 3_666 ? Cu1 S2 Cu2 113.192(16) . 3_666 ? C3 P1 C6 106.49(7) . . ? C3 P1 C9 103.90(8) . . ? C6 P1 C9 104.34(7) . . ? C3 P1 Cu1 113.24(5) . . ? C6 P1 Cu1 118.06(5) . . ? C9 P1 Cu1 109.57(5) . . ? C12 P2 C18 104.66(7) . . ? C12 P2 C15 105.93(7) . . ? C18 P2 C15 103.22(7) . . ? C12 P2 Cu2 109.44(5) . . ? C18 P2 Cu2 111.37(5) . . ? C15 P2 Cu2 120.91(5) . . ? C2 C1 S1 112.06(9) . . ? C1 C2 S2 112.99(9) . . ? C5 C3 C4 109.74(14) . . ? C5 C3 P1 110.62(13) . . ? C4 C3 P1 109.42(12) . . ? C8 C6 C7 109.86(14) . . ? C8 C6 P1 116.49(12) . . ? C7 C6 P1 111.11(10) . . ? C10 C9 C11 111.20(13) . . ? C10 C9 P1 110.46(11) . . ? C11 C9 P1 115.90(12) . . ? C14 C12 C13 110.71(14) . . ? C14 C12 P2 110.08(11) . . ? C13 C12 P2 110.04(11) . . ? C16 C15 C17 110.22(13) . . ? C16 C15 P2 111.67(10) . . ? C17 C15 P2 115.87(11) . . ? C19 C18 C20 110.68(13) . . ? C19 C18 P2 109.81(11) . . ? C20 C18 P2 116.83(11) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.335 _refine_diff_density_min -0.225 _refine_diff_density_rms 0.042 # Attachment '- 3.cif' data_3 _database_code_depnum_ccdc_archive 'CCDC 879010' #TrackingRef '- 3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; bis(ethane-1,\m~2~2-disulfido)-dimethyl-di-gallium ; _chemical_name_common methyl-gallium-ethanedithiolate _chemical_formula_moiety 'C6 H14 Ga2 S4' _chemical_formula_sum 'C6 H14 Ga2 S4' _chemical_formula_weight 353.85 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ga Ga 0.2307 1.6083 '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_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.6025(10) _cell_length_b 6.7608(10) _cell_length_c 7.1157(10) _cell_angle_alpha 73.926(11) _cell_angle_beta 80.799(12) _cell_angle_gamma 83.692(12) _cell_volume 300.57(8) _cell_formula_units_Z 1 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 5913 _cell_measurement_theta_min 3.01 _cell_measurement_theta_max 29.61 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.955 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 176 _exptl_absorpt_coefficient_mu 5.126 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.4034 _exptl_absorpt_correction_T_max 0.5467 _exptl_absorpt_process_details 'STOE X-RED' loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0 1 0 0.0591 0 -1 0 0.0892 1 0 0 0.0821 -1 0 0 0.0620 0 0 -1 0.1235 0 0 1 0.1020 -1 0 -1 0.0998 _diffrn_measurement_device '2-circle goniometer' _diffrn_measurement_device_type 'STOE IPDS 2T' _diffrn_detector 'image plate (34 cm diameter / schwenk)' _diffrn_detector_type STOE _diffrn_detector_area_resol_mean 6.67 _diffrn_source 'sealed X-ray tube, 12 x 0.4 mm long-fine focus' _diffrn_source_voltage 50 _diffrn_source_current 40 _diffrn_source_power 2.00 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_monochromator 'plane graphite' _diffrn_radiation_polarisn_norm 0 _diffrn_radiation_collimation '0.5 mm diameter, multiple pinhole' _diffrn_ambient_temperature 180(2) _diffrn_measurement_method 'rotation method' _diffrn_measurement_details ; 275 frames, detector distance = 100 mm ; _diffrn_reflns_number 3134 _diffrn_reflns_av_R_equivalents 0.0288 _diffrn_reflns_av_sigmaI/netI 0.0236 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 27.99 _reflns_number_total 1452 _reflns_number_gt 1366 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE X-AREA' _computing_cell_refinement 'STOE X-AREA' _computing_data_reduction 'STOE X-RED' _computing_structure_solution 'SIR 92' _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^)+(0.0245P)^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 SHELXL _refine_ls_extinction_coef 0.054(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 1452 _refine_ls_number_parameters 57 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0177 _refine_ls_R_factor_gt 0.0161 _refine_ls_wR_factor_ref 0.0397 _refine_ls_wR_factor_gt 0.0393 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.024 _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 Ga1 Ga 0.64235(2) 0.28575(2) 0.51256(2) 0.01754(7) Uani 1 1 d . . . S1 S 0.75770(6) 0.28934(5) 0.19966(5) 0.02227(9) Uani 1 1 d . . . S2 S 0.72049(5) 0.62895(5) 0.47924(5) 0.01866(9) Uani 1 1 d . . . C1 C 0.7105(3) 0.0671(2) 0.7409(2) 0.0255(3) Uani 1 1 d . . . H1A H 0.6109 -0.0347 0.7745 0.038 Uiso 1 1 calc R . . H1B H 0.7095 0.1242 0.8505 0.038 Uiso 1 1 calc R . . H1C H 0.8447 0.0040 0.7103 0.038 Uiso 1 1 calc R . . C2 C 0.7251(2) 0.5694(2) 0.1015(2) 0.0228(3) Uani 1 1 d . . . H2A H 0.7875 0.6067 -0.0354 0.027 Uiso 1 1 calc R . . H2B H 0.5794 0.6107 0.1052 0.027 Uiso 1 1 calc R . . C3 C 0.8198(2) 0.6867(2) 0.2149(2) 0.0228(3) Uani 1 1 d . . . H3A H 0.7952 0.8334 0.1565 0.027 Uiso 1 1 calc R . . H3B H 0.9674 0.6548 0.2006 0.027 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 Ga1 0.01863(10) 0.01630(9) 0.01705(10) -0.00425(6) -0.00176(6) 0.00019(6) S1 0.02409(19) 0.02302(17) 0.02052(17) -0.00980(13) 0.00152(14) -0.00122(14) S2 0.01767(17) 0.01955(16) 0.02027(16) -0.00707(13) -0.00285(12) -0.00264(12) C1 0.0289(8) 0.0198(6) 0.0258(7) -0.0016(5) -0.0074(6) 0.0010(6) C2 0.0243(7) 0.0247(7) 0.0177(6) -0.0042(5) -0.0011(5) -0.0003(6) C3 0.0227(7) 0.0218(6) 0.0222(7) -0.0042(5) 0.0019(5) -0.0053(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 Ga1 C1 1.9454(15) . ? Ga1 S1 2.2293(5) . ? Ga1 S2 2.3718(5) . ? Ga1 S2 2.3969(5) 2_666 ? S1 C2 1.8290(15) . ? S2 C3 1.8370(15) . ? S2 Ga1 2.3969(5) 2_666 ? C2 C3 1.515(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 C1 Ga1 S1 124.77(5) . . ? C1 Ga1 S2 119.82(5) . . ? S1 Ga1 S2 95.119(18) . . ? C1 Ga1 S2 112.71(5) . 2_666 ? S1 Ga1 S2 105.119(18) . 2_666 ? S2 Ga1 S2 93.978(17) . 2_666 ? C2 S1 Ga1 95.83(5) . . ? C3 S2 Ga1 96.13(5) . . ? C3 S2 Ga1 104.26(5) . 2_666 ? Ga1 S2 Ga1 86.022(17) . 2_666 ? C3 C2 S1 113.09(10) . . ? C2 C3 S2 114.25(10) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.99 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.458 _refine_diff_density_min -0.451 _refine_diff_density_rms 0.069 # Attachment '- 4.cif' data_4 _database_code_depnum_ccdc_archive 'CCDC 879011' #TrackingRef '- 4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; bis(\m~2~-ethane-1,2-disulfido)-bis(triisopropylphosphine)-tetramethyl-di-copper-di-gallium ; _chemical_formula_moiety 'C26 H62 Cu2 Ga2 P2 S4' _chemical_formula_sum 'C26 H62 Cu2 Ga2 P2 S4' _chemical_formula_weight 831.46 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' 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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ga Ga 0.2307 1.6083 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 17.4373(11) _cell_length_b 15.7295(7) _cell_length_c 15.3649(10) _cell_angle_alpha 90.00 _cell_angle_beta 116.444(5) _cell_angle_gamma 90.00 _cell_volume 3773.3(4) _cell_formula_units_Z 4 _cell_measurement_temperature 105(2) _cell_measurement_reflns_used 23168 _cell_measurement_theta_min 1.84 _cell_measurement_theta_max 29.62 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.464 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1728 _exptl_absorpt_coefficient_mu 2.846 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.4406 _exptl_absorpt_correction_T_max 0.5564 _exptl_absorpt_process_details 'STOE X-RED' loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist -4 -2 -1 0.1900 1 -1 -1 0.1230 -1 1 1 0.1170 1 1 -1 0.1460 -1 -1 1 0.1280 -1 0 -1 0.2010 1 0 1 0.1530 -3 1 0 0.1790 _diffrn_measurement_device '2-circle goniometer' _diffrn_measurement_device_type 'STOE IPDS 2T' _diffrn_detector 'image plate (34 cm diameter / schwenk)' _diffrn_detector_type STOE _diffrn_detector_area_resol_mean 6.67 _diffrn_source 'sealed X-ray tube, 12 x 0.4 mm long-fine focus' _diffrn_source_voltage 50 _diffrn_source_current 40 _diffrn_source_power 2.00 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_monochromator 'plane graphite' _diffrn_radiation_polarisn_norm 0 _diffrn_radiation_collimation '0.5 mm diameter, multiple pinhole' _diffrn_ambient_temperature 105(2) _diffrn_measurement_method 'rotation method' _diffrn_measurement_details ; 195 frames, detector distance = 100 mm ; _diffrn_reflns_number 12527 _diffrn_reflns_av_R_equivalents 0.0339 _diffrn_reflns_av_sigmaI/netI 0.0237 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.84 _diffrn_reflns_theta_max 27.00 _reflns_number_total 4106 _reflns_number_gt 3742 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE X-AREA' _computing_cell_refinement 'STOE X-AREA' _computing_data_reduction 'STOE X-RED' _computing_structure_solution 'SIR 92' _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^)+(0.0210P)^2^+2.2702P] 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 4106 _refine_ls_number_parameters 168 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0225 _refine_ls_R_factor_gt 0.0188 _refine_ls_wR_factor_ref 0.0464 _refine_ls_wR_factor_gt 0.0455 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.037 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.704266(12) 0.405713(11) 0.471403(13) 0.01929(5) Uani 1 1 d . B . Ga1 Ga 0.910126(10) 0.289180(10) 0.479980(12) 0.01956(5) Uani 1 1 d . . . S1 S 0.77001(2) 0.34173(2) 0.39028(3) 0.02055(8) Uani 1 1 d . . . S2 S 0.59047(2) 0.31688(2) 0.41307(3) 0.01907(8) Uani 1 1 d . . . P1 P 0.72773(3) 0.53516(2) 0.53241(3) 0.02132(9) Uani 1 1 d . . . C1 C 0.97946(12) 0.38477(12) 0.55889(16) 0.0392(4) Uani 1 1 d . . . H1A H 0.9783 0.4304 0.5169 0.059 Uiso 1 1 calc R . . H1B H 1.0375 0.3663 0.5966 0.059 Uiso 1 1 calc R . . H1C H 0.9563 0.4041 0.6016 0.059 Uiso 1 1 calc R . . C2 C 0.93645(12) 0.22589(12) 0.38564(13) 0.0337(4) Uani 1 1 d . . . H2A H 0.9740 0.1794 0.4179 0.051 Uiso 1 1 calc R . . H2B H 0.9638 0.2632 0.3586 0.051 Uiso 1 1 calc R . . H2C H 0.8843 0.2044 0.3345 0.051 Uiso 1 1 calc R . . C3 C 0.70607(9) 0.24456(10) 0.35153(10) 0.0201(3) Uani 1 1 d . . . H3A H 0.7126 0.2196 0.2975 0.024 Uiso 1 1 calc R . . H3B H 0.7271 0.2039 0.4045 0.024 Uiso 1 1 calc R . . C4 C 0.61160(10) 0.26165(11) 0.32085(11) 0.0236(3) Uani 1 1 d . . . H4A H 0.5812 0.2079 0.3057 0.028 Uiso 1 1 calc R . . H4B H 0.5889 0.2956 0.2620 0.028 Uiso 1 1 calc R . . C5 C 0.70691(12) 0.60721(10) 0.42920(14) 0.0306(4) Uani 1 1 d . B . H5 H 0.7107 0.6661 0.4517 0.037 Uiso 1 1 calc R . . C6 C 0.61637(13) 0.59156(13) 0.34869(15) 0.0417(5) Uani 1 1 d . . . H6A H 0.6119 0.5341 0.3259 0.063 Uiso 1 1 calc R B . H6B H 0.6049 0.6301 0.2958 0.063 Uiso 1 1 calc R . . H6C H 0.5755 0.6007 0.3738 0.063 Uiso 1 1 calc R . . C7 C 0.77354(14) 0.59405(13) 0.39097(16) 0.0420(5) Uani 1 1 d . . . H7A H 0.7593 0.6289 0.3346 0.063 Uiso 1 1 calc R B . H7B H 0.7740 0.5354 0.3740 0.063 Uiso 1 1 calc R . . H7C H 0.8292 0.6096 0.4404 0.063 Uiso 1 1 calc R . . C8 C 0.83986(11) 0.55735(10) 0.62097(13) 0.0275(3) Uani 1 1 d . B . H8 H 0.8755 0.5363 0.5911 0.033 Uiso 1 1 calc R . . C9 C 0.86426(13) 0.65081(12) 0.64551(19) 0.0499(6) Uani 1 1 d . . . H9A H 0.9254 0.6556 0.6815 0.075 Uiso 1 1 calc R B . H9B H 0.8377 0.6723 0.6840 0.075 Uiso 1 1 calc R . . H9C H 0.8450 0.6831 0.5865 0.075 Uiso 1 1 calc R . . C10 C 0.86527(14) 0.50550(14) 0.71353(14) 0.0425(5) Uani 1 1 d . . . H10A H 0.8379 0.5286 0.7504 0.064 Uiso 1 1 calc R B . H10B H 0.9263 0.5077 0.7517 0.064 Uiso 1 1 calc R . . H10C H 0.8476 0.4475 0.6968 0.064 Uiso 1 1 calc R . . C11 C 0.65231(11) 0.66870(11) 0.59666(13) 0.0283(3) Uani 1 1 d . . . H11A H 0.6565 0.7029 0.5472 0.042 Uiso 0.50 1 calc PR A 1 H11B H 0.7025 0.6768 0.6572 0.042 Uiso 0.50 1 calc PR A 1 H11C H 0.6025 0.6852 0.6039 0.042 Uiso 0.50 1 calc PR A 1 H11D H 0.6511 0.6737 0.6583 0.042 Uiso 0.50 1 calc PR A 1 H11E H 0.6052 0.6998 0.5484 0.042 Uiso 0.50 1 calc PR A 1 H11F H 0.7052 0.6914 0.6016 0.042 Uiso 0.50 1 calc PR A 1 C12A C 0.6449(2) 0.57302(19) 0.5668(3) 0.0198(7) Uiso 0.536(5) 1 d P B 1 H12A H 0.5904 0.5678 0.5081 0.024 Uiso 0.536(5) 1 calc PR B 1 C13A C 0.6374(2) 0.5146(2) 0.6416(2) 0.0316(9) Uiso 0.536(5) 1 d P B 1 H13A H 0.6328 0.4567 0.6199 0.047 Uiso 0.536(5) 1 calc PR B 1 H13B H 0.5874 0.5295 0.6492 0.047 Uiso 0.536(5) 1 calc PR B 1 H13C H 0.6873 0.5207 0.7027 0.047 Uiso 0.536(5) 1 calc PR B 1 C12B C 0.6706(3) 0.5764(2) 0.6048(3) 0.0210(8) Uiso 0.464(5) 1 d P B 2 H12B H 0.7085 0.5650 0.6734 0.025 Uiso 0.464(5) 1 calc PR B 2 C13B C 0.5898(2) 0.5237(2) 0.5785(3) 0.0297(10) Uiso 0.464(5) 1 d P B 2 H13D H 0.6042 0.4643 0.5848 0.045 Uiso 0.464(5) 1 calc PR B 2 H13E H 0.5492 0.5356 0.5127 0.045 Uiso 0.464(5) 1 calc PR B 2 H13F H 0.5653 0.5379 0.6215 0.045 Uiso 0.464(5) 1 calc PR B 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 Cu1 0.02099(10) 0.01610(9) 0.02247(9) 0.00329(7) 0.01120(8) 0.00303(7) Ga1 0.01608(9) 0.02017(8) 0.02555(9) 0.00000(6) 0.01208(7) 0.00051(6) S1 0.01929(17) 0.02089(17) 0.02512(18) 0.00553(14) 0.01318(15) 0.00441(14) S2 0.01510(17) 0.02415(17) 0.01792(16) 0.00076(13) 0.00730(14) 0.00265(14) P1 0.0241(2) 0.01430(17) 0.0334(2) 0.00437(15) 0.01989(17) 0.00367(15) C1 0.0271(9) 0.0283(9) 0.0591(12) -0.0078(8) 0.0164(9) -0.0085(7) C2 0.0360(10) 0.0416(10) 0.0325(9) 0.0057(7) 0.0234(8) 0.0130(8) C3 0.0191(7) 0.0244(7) 0.0178(7) 0.0003(6) 0.0091(6) 0.0032(6) C4 0.0166(7) 0.0354(8) 0.0165(7) -0.0031(6) 0.0054(6) 0.0025(6) C5 0.0369(9) 0.0208(7) 0.0444(10) 0.0138(7) 0.0272(8) 0.0099(7) C6 0.0396(11) 0.0463(11) 0.0424(11) 0.0170(9) 0.0211(9) 0.0168(9) C7 0.0525(12) 0.0368(10) 0.0567(12) 0.0209(9) 0.0422(11) 0.0102(9) C8 0.0280(8) 0.0206(7) 0.0388(9) 0.0003(7) 0.0191(7) 0.0013(7) C9 0.0296(10) 0.0268(9) 0.0888(17) -0.0083(10) 0.0222(11) -0.0081(8) C10 0.0439(11) 0.0450(11) 0.0308(9) 0.0006(8) 0.0096(8) -0.0098(9) C11 0.0308(9) 0.0274(8) 0.0316(8) -0.0079(7) 0.0183(7) 0.0018(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 P1 2.2024(4) . ? Cu1 S2 2.2604(4) . ? Cu1 S1 2.2701(4) . ? Ga1 C1 1.9715(18) . ? Ga1 C2 1.9737(17) . ? Ga1 S2 2.3449(4) 7_656 ? Ga1 S1 2.3565(4) . ? S1 C3 1.8282(16) . ? S2 C4 1.8339(15) . ? P1 C12A 1.844(3) . ? P1 C5 1.8488(17) . ? P1 C8 1.8512(18) . ? P1 C12B 1.907(4) . ? C3 C4 1.522(2) . ? C5 C6 1.531(3) . ? C5 C7 1.532(2) . ? C8 C10 1.524(2) . ? C8 C9 1.530(2) . ? C11 C12B 1.480(4) . ? C11 C12A 1.562(3) . ? C12A C13A 1.521(5) . ? C12B C13B 1.525(5) . ? 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 P1 Cu1 S2 134.761(16) . . ? P1 Cu1 S1 126.876(16) . . ? S2 Cu1 S1 94.417(15) . . ? C1 Ga1 C2 123.84(9) . . ? C1 Ga1 S2 107.73(7) . 7_656 ? C2 Ga1 S2 103.35(6) . 7_656 ? C1 Ga1 S1 106.52(6) . . ? C2 Ga1 S1 105.49(6) . . ? S2 Ga1 S1 109.415(14) 7_656 . ? C3 S1 Cu1 99.53(5) . . ? C3 S1 Ga1 102.73(5) . . ? Cu1 S1 Ga1 118.680(18) . . ? C4 S2 Cu1 98.99(5) . . ? C4 S2 Ga1 105.64(6) . 7_656 ? Cu1 S2 Ga1 116.040(17) . 7_656 ? C12A P1 C5 99.70(12) . . ? C12A P1 C8 115.72(14) . . ? C5 P1 C8 104.75(8) . . ? C5 P1 C12B 109.74(13) . . ? C8 P1 C12B 99.35(15) . . ? C12A P1 Cu1 113.57(10) . . ? C5 P1 Cu1 105.86(6) . . ? C8 P1 Cu1 114.98(5) . . ? C12B P1 Cu1 121.08(11) . . ? C4 C3 S1 111.85(11) . . ? C3 C4 S2 113.99(10) . . ? C6 C5 C7 110.72(17) . . ? C6 C5 P1 109.42(12) . . ? C7 C5 P1 110.70(12) . . ? C10 C8 C9 110.53(17) . . ? C10 C8 P1 110.98(12) . . ? C9 C8 P1 116.68(13) . . ? C13A C12A C11 112.6(3) . . ? C13A C12A P1 111.3(2) . . ? C11 C12A P1 114.99(19) . . ? C11 C12B C13B 111.9(3) . . ? C11 C12B P1 115.6(2) . . ? C13B C12B P1 108.7(3) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.328 _refine_diff_density_min -0.315 _refine_diff_density_rms 0.051 # Attachment '- 5.cif' data_5 _database_code_depnum_ccdc_archive 'CCDC 879012' #TrackingRef '- 5.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; bis(\m~2~-ethane-1,2-disulfido)-bis(triisopropylphosphine)-bis(phenylsulfido)-dimethyl-di-copper-di-gallium tetrahydrofuran solvate ; _chemical_formula_moiety 'C36 H66 Cu2 Ga2 P2 S6, 2(C4 H8 O)' _chemical_formula_sum 'C44 H82 Cu2 Ga2 O2 P2 S6' _chemical_formula_weight 1163.92 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' 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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ga Ga 0.2307 1.6083 '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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.5998(10) _cell_length_b 11.5070(11) _cell_length_c 13.6932(15) _cell_angle_alpha 67.290(7) _cell_angle_beta 72.432(8) _cell_angle_gamma 65.161(7) _cell_volume 1378.6(2) _cell_formula_units_Z 1 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 15556 _cell_measurement_theta_min 1.64 _cell_measurement_theta_max 28.32 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.402 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 608 _exptl_absorpt_coefficient_mu 2.045 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.5638 _exptl_absorpt_correction_T_max 0.8966 _exptl_absorpt_process_details 'STOE X-RED' loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0 0 -1 0.0420 0 0 1 0.0150 0 1 0 0.1000 -1 -1 0 0.1320 1 1 0 0.1160 1 -2 1 0.1380 -1 3 -1 0.1210 _diffrn_measurement_device '2-circle goniometer' _diffrn_measurement_device_type 'STOE IPDS 2T' _diffrn_detector 'image plate (34 cm diameter / schwenk)' _diffrn_detector_type STOE _diffrn_detector_area_resol_mean 6.67 _diffrn_source 'sealed X-ray tube, 12 x 0.4 mm long-fine focus' _diffrn_source_voltage 50 _diffrn_source_current 40 _diffrn_source_power 2.00 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_monochromator 'plane graphite' _diffrn_radiation_polarisn_norm 0 _diffrn_radiation_collimation '0.5 mm diameter, multiple pinhole' _diffrn_ambient_temperature 180(2) _diffrn_measurement_method 'rotation method' _diffrn_measurement_details ; 273 frames, detector distance = 110 mm ; _diffrn_reflns_number 11622 _diffrn_reflns_av_R_equivalents 0.0796 _diffrn_reflns_av_sigmaI/netI 0.0677 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.64 _diffrn_reflns_theta_max 26.00 _reflns_number_total 5374 _reflns_number_gt 3829 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE X-AREA' _computing_cell_refinement 'STOE X-AREA' _computing_data_reduction 'STOE X-RED' _computing_structure_solution 'SIR 92' _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^)+(0.0844P)^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 5374 _refine_ls_number_parameters 269 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0764 _refine_ls_R_factor_gt 0.0535 _refine_ls_wR_factor_ref 0.1409 _refine_ls_wR_factor_gt 0.1306 _refine_ls_goodness_of_fit_ref 0.972 _refine_ls_restrained_S_all 0.972 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.73932(5) 0.50492(6) 0.58938(5) 0.04412(18) Uani 1 1 d . . . Ga1 Ga 0.90980(5) 0.66404(5) 0.29114(4) 0.04376(17) Uani 1 1 d . . . S1 S 0.84017(11) 0.49105(12) 0.42027(9) 0.0431(3) Uani 1 1 d . . . S2 S 0.90754(11) 0.31105(12) 0.66642(10) 0.0444(3) Uani 1 1 d . . . S3 S 0.71078(12) 0.83916(14) 0.31494(11) 0.0539(3) Uani 1 1 d . . . P1 P 0.52998(11) 0.63012(13) 0.65430(11) 0.0466(3) Uani 1 1 d . . . C1 C 0.9711(6) 0.6360(7) 0.1488(4) 0.0608(14) Uani 1 1 d . . . H1A H 0.9543 0.5585 0.1526 0.091 Uiso 1 1 calc R . . H1B H 1.0700 0.6224 0.1261 0.091 Uiso 1 1 calc R . . H1C H 0.9190 0.7135 0.0981 0.091 Uiso 1 1 calc R . . C2 C 1.0074(4) 0.3541(5) 0.4447(4) 0.0443(10) Uani 1 1 d . . . H2A H 1.0439 0.3139 0.3867 0.053 Uiso 1 1 calc R . . H2B H 1.0753 0.3897 0.4455 0.053 Uiso 1 1 calc R . . C3 C 0.9897(5) 0.2480(5) 0.5501(4) 0.0481(11) Uani 1 1 d . . . H3A H 1.0817 0.1809 0.5623 0.058 Uiso 1 1 calc R . . H3B H 0.9329 0.2038 0.5445 0.058 Uiso 1 1 calc R . . C4 C 0.7275(4) 0.9614(5) 0.1881(4) 0.0475(11) Uani 1 1 d . . . C5 C 0.8383(6) 1.0101(6) 0.1523(5) 0.0617(14) Uani 1 1 d . . . H5 H 0.9078 0.9760 0.1942 0.074 Uiso 1 1 calc R . . C6 C 0.8465(6) 1.1086(7) 0.0552(5) 0.0723(17) Uani 1 1 d . . . H6 H 0.9230 1.1381 0.0309 0.087 Uiso 1 1 calc R . . C7 C 0.7412(6) 1.1632(6) -0.0057(5) 0.0684(16) Uani 1 1 d . . . H7 H 0.7447 1.2315 -0.0700 0.082 Uiso 1 1 calc R . . C8 C 0.6318(6) 1.1157(6) 0.0294(5) 0.0661(15) Uani 1 1 d . . . H8 H 0.5617 1.1511 -0.0123 0.079 Uiso 1 1 calc R . . C9 C 0.6234(5) 1.0166(6) 0.1252(4) 0.0583(13) Uani 1 1 d . . . H9 H 0.5476 0.9863 0.1479 0.070 Uiso 1 1 calc R . . C10 C 0.5388(5) 0.7224(6) 0.7343(5) 0.0587(14) Uani 1 1 d . . . H10 H 0.4428 0.7657 0.7676 0.070 Uiso 1 1 calc R . . C11 C 0.6257(8) 0.6226(8) 0.8245(6) 0.091(2) Uani 1 1 d . . . H11A H 0.7216 0.5834 0.7932 0.137 Uiso 1 1 calc R . . H11B H 0.5864 0.5531 0.8659 0.137 Uiso 1 1 calc R . . H11C H 0.6231 0.6693 0.8704 0.137 Uiso 1 1 calc R . . C12 C 0.6017(6) 0.8303(7) 0.6638(6) 0.0775(19) Uani 1 1 d . . . H12A H 0.6162 0.8697 0.7080 0.116 Uiso 1 1 calc R . . H12B H 0.5385 0.8983 0.6159 0.116 Uiso 1 1 calc R . . H12C H 0.6904 0.7911 0.6229 0.116 Uiso 1 1 calc R . . C13 C 0.4113(5) 0.5341(6) 0.7348(5) 0.0594(14) Uani 1 1 d . . . H13 H 0.3589 0.5386 0.6848 0.071 Uiso 1 1 calc R . . C14 C 0.2991(7) 0.5903(8) 0.8242(6) 0.090(2) Uani 1 1 d . . . H14A H 0.2309 0.5460 0.8515 0.135 Uiso 1 1 calc R . . H14B H 0.2526 0.6850 0.7949 0.135 Uiso 1 1 calc R . . H14C H 0.3443 0.5747 0.8814 0.135 Uiso 1 1 calc R . . C15 C 0.4892(6) 0.3875(6) 0.7835(5) 0.0683(16) Uani 1 1 d . . . H15A H 0.5323 0.3769 0.8402 0.102 Uiso 1 1 calc R . . H15B H 0.5607 0.3525 0.7293 0.102 Uiso 1 1 calc R . . H15C H 0.4243 0.3395 0.8119 0.102 Uiso 1 1 calc R . . C16 C 0.4346(5) 0.7644(5) 0.5461(4) 0.0533(12) Uani 1 1 d . . . H16 H 0.4920 0.8215 0.5059 0.064 Uiso 1 1 calc R . . C17 C 0.2867(5) 0.8573(6) 0.5840(5) 0.0701(17) Uani 1 1 d . . . H17A H 0.2502 0.9292 0.5232 0.105 Uiso 1 1 calc R . . H17B H 0.2938 0.8937 0.6338 0.105 Uiso 1 1 calc R . . H17C H 0.2244 0.8066 0.6187 0.105 Uiso 1 1 calc R . . C18 C 0.4240(5) 0.7062(6) 0.4679(4) 0.0578(13) Uani 1 1 d . . . H18A H 0.3634 0.6539 0.5030 0.087 Uiso 1 1 calc R . . H18B H 0.5161 0.6501 0.4435 0.087 Uiso 1 1 calc R . . H18C H 0.3858 0.7779 0.4075 0.087 Uiso 1 1 calc R . . C1L C 0.9004(8) 0.9278(8) 0.7072(6) 0.0829(19) Uani 1 1 d . . . H1L1 H 0.8686 0.9593 0.6390 0.099 Uiso 1 1 calc R . . H1L2 H 0.9809 0.9540 0.6955 0.099 Uiso 1 1 calc R . . C2L C 0.7844(7) 0.9877(7) 0.7868(6) 0.0807(19) Uani 1 1 d . . . H2L1 H 0.6944 1.0263 0.7625 0.097 Uiso 1 1 calc R . . H2L2 H 0.8023 1.0570 0.7986 0.097 Uiso 1 1 calc R . . C3L C 0.7863(7) 0.8702(8) 0.8883(6) 0.086(2) Uani 1 1 d . . . H3L1 H 0.8021 0.8870 0.9471 0.103 Uiso 1 1 calc R . . H3L2 H 0.6981 0.8534 0.9092 0.103 Uiso 1 1 calc R . . C4L C 0.9059(7) 0.7546(7) 0.8587(6) 0.0791(19) Uani 1 1 d . . . H4L1 H 0.9873 0.7356 0.8884 0.095 Uiso 1 1 calc R . . H4L2 H 0.8794 0.6751 0.8873 0.095 Uiso 1 1 calc R . . O1L O 0.9381(6) 0.7884(6) 0.7482(4) 0.0984(17) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0276(3) 0.0411(3) 0.0607(4) -0.0226(3) -0.0037(2) -0.0050(2) Ga1 0.0348(3) 0.0416(3) 0.0485(3) -0.0126(2) -0.00580(19) -0.0089(2) S1 0.0323(5) 0.0410(6) 0.0523(7) -0.0141(5) -0.0060(4) -0.0099(4) S2 0.0316(5) 0.0406(6) 0.0537(7) -0.0126(5) -0.0050(4) -0.0086(4) S3 0.0359(6) 0.0489(7) 0.0586(7) -0.0127(6) 0.0001(5) -0.0062(5) P1 0.0287(5) 0.0470(7) 0.0622(8) -0.0264(6) -0.0044(5) -0.0046(5) C1 0.058(3) 0.070(4) 0.049(3) -0.020(3) -0.001(2) -0.020(3) C2 0.031(2) 0.039(3) 0.063(3) -0.027(2) -0.0030(18) -0.0049(17) C3 0.036(2) 0.040(3) 0.063(3) -0.021(2) -0.0040(19) -0.0061(19) C4 0.034(2) 0.038(3) 0.056(3) -0.017(2) -0.0027(19) -0.0004(19) C5 0.048(3) 0.056(3) 0.074(4) -0.012(3) -0.012(2) -0.017(2) C6 0.057(3) 0.069(4) 0.078(4) -0.007(3) -0.007(3) -0.026(3) C7 0.069(4) 0.058(4) 0.058(3) -0.012(3) 0.002(3) -0.017(3) C8 0.055(3) 0.069(4) 0.060(3) -0.018(3) -0.012(2) -0.008(3) C9 0.040(2) 0.064(4) 0.064(3) -0.017(3) -0.009(2) -0.012(2) C10 0.040(2) 0.059(3) 0.081(4) -0.041(3) -0.009(2) -0.002(2) C11 0.081(4) 0.102(6) 0.103(5) -0.060(5) -0.043(4) 0.004(4) C12 0.051(3) 0.068(4) 0.126(6) -0.058(4) -0.006(3) -0.012(3) C13 0.039(2) 0.066(4) 0.065(3) -0.018(3) -0.005(2) -0.015(2) C14 0.055(3) 0.077(5) 0.105(5) -0.029(4) 0.026(3) -0.017(3) C15 0.053(3) 0.057(4) 0.073(4) -0.011(3) -0.008(3) -0.008(3) C16 0.036(2) 0.046(3) 0.070(3) -0.021(2) -0.006(2) -0.005(2) C17 0.041(3) 0.062(4) 0.086(4) -0.029(3) -0.012(3) 0.008(3) C18 0.047(3) 0.059(3) 0.061(3) -0.015(3) -0.008(2) -0.016(2) C1L 0.078(4) 0.081(5) 0.085(5) -0.031(4) -0.009(3) -0.021(4) C2L 0.067(4) 0.066(4) 0.103(5) -0.033(4) -0.002(3) -0.019(3) C3L 0.071(4) 0.089(5) 0.087(5) -0.037(4) -0.013(3) -0.009(4) C4L 0.073(4) 0.069(4) 0.088(5) -0.034(4) -0.020(3) -0.003(3) O1L 0.112(4) 0.081(4) 0.087(4) -0.044(3) -0.019(3) 0.000(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 Cu1 P1 2.2140(12) . ? Cu1 S1 2.2756(13) . ? Cu1 S2 2.2903(13) . ? Ga1 C1 1.968(5) . ? Ga1 S3 2.2667(13) . ? Ga1 S1 2.3157(13) . ? Ga1 S2 2.3329(13) 2_766 ? S1 C2 1.828(4) . ? S2 C3 1.829(5) . ? S2 Ga1 2.3329(13) 2_766 ? S3 C4 1.778(5) . ? P1 C10 1.839(6) . ? P1 C13 1.846(6) . ? P1 C16 1.852(5) . ? C2 C3 1.510(7) . ? C4 C5 1.387(7) . ? C4 C9 1.388(7) . ? C5 C6 1.382(9) . ? C6 C7 1.380(9) . ? C7 C8 1.367(9) . ? C8 C9 1.374(8) . ? C10 C12 1.516(9) . ? C10 C11 1.548(9) . ? C13 C15 1.505(8) . ? C13 C14 1.555(8) . ? C16 C18 1.516(8) . ? C16 C17 1.549(7) . ? C1L O1L 1.397(9) . ? C1L C2L 1.494(9) . ? C2L C3L 1.519(11) . ? C3L C4L 1.494(9) . ? C4L O1L 1.379(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 P1 Cu1 S1 131.97(5) . . ? P1 Cu1 S2 133.36(5) . . ? S1 Cu1 S2 93.06(4) . . ? C1 Ga1 S3 117.68(18) . . ? C1 Ga1 S1 111.5(2) . . ? S3 Ga1 S1 98.90(5) . . ? C1 Ga1 S2 108.60(17) . 2_766 ? S3 Ga1 S2 107.89(5) . 2_766 ? S1 Ga1 S2 112.04(5) . 2_766 ? C2 S1 Cu1 101.13(16) . . ? C2 S1 Ga1 103.17(16) . . ? Cu1 S1 Ga1 120.23(6) . . ? C3 S2 Cu1 98.63(16) . . ? C3 S2 Ga1 104.25(16) . 2_766 ? Cu1 S2 Ga1 116.35(6) . 2_766 ? C4 S3 Ga1 100.67(15) . . ? C10 P1 C13 108.7(3) . . ? C10 P1 C16 103.6(3) . . ? C13 P1 C16 105.3(2) . . ? C10 P1 Cu1 113.57(16) . . ? C13 P1 Cu1 113.14(18) . . ? C16 P1 Cu1 111.88(17) . . ? C3 C2 S1 111.4(3) . . ? C2 C3 S2 114.6(3) . . ? C5 C4 C9 118.2(5) . . ? C5 C4 S3 121.8(4) . . ? C9 C4 S3 119.8(4) . . ? C6 C5 C4 120.8(5) . . ? C7 C6 C5 120.0(6) . . ? C8 C7 C6 119.3(6) . . ? C7 C8 C9 121.2(6) . . ? C8 C9 C4 120.4(5) . . ? C12 C10 C11 111.1(6) . . ? C12 C10 P1 110.8(4) . . ? C11 C10 P1 109.4(4) . . ? C15 C13 C14 108.9(5) . . ? C15 C13 P1 113.1(4) . . ? C14 C13 P1 115.5(5) . . ? C18 C16 C17 109.7(4) . . ? C18 C16 P1 110.9(4) . . ? C17 C16 P1 115.6(4) . . ? O1L C1L C2L 108.0(6) . . ? C1L C2L C3L 104.2(6) . . ? C4L C3L C2L 104.2(6) . . ? O1L C4L C3L 108.1(6) . . ? C4L O1L C1L 108.3(5) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.024 _refine_diff_density_min -0.832 _refine_diff_density_rms 0.105