# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_[(iPr3PCu)3(SC2H4S)2GaMe2] _database_code_depnum_ccdc_archive 'CCDC 907023' #TrackingRef '17783_web_deposit_cif_file_0_DirkFriedrich_1360942266.25_[(iPr3PCu)3(SC2H4S)2GaMe2].cif' _audit_creation_date 2012-10-10T16:00:21-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; bis(\m~3~-1,2-dithiolatoethane-S,S,S',S')-dimethanido -tris(triisopropylphosphine)-tricopper(+1)-gallium(+3) ; _chemical_formula_moiety 'C33 H77 Cu3 Ga1 P3 S4' _chemical_formula_sum 'C33 H77 Cu3 Ga P3 S4' _chemical_formula_weight 955.44 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.5596(10) _cell_length_b 13.7730(11) _cell_length_c 15.3803(12) _cell_angle_alpha 112.901(6) _cell_angle_beta 94.918(6) _cell_angle_gamma 112.310(6) _cell_volume 2354.3(3) _cell_formula_units_Z 2 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 20369 _cell_measurement_theta_min 2.12 _cell_measurement_theta_max 29.36 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.11 _exptl_crystal_density_diffrn 1.348 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1004 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 2.19 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details ; Busing, W. R. & Levy, H. A. (1957) Acta Cryst. 10, 180-182. and Coppens, P., Leiserowitz, L. & Rabinovich, D. (1965) Acta Cryst. 1965, 1035-1038. ; _exptl_absorpt_correction_T_min 0.5026 _exptl_absorpt_correction_T_max 0.8013 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 180(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 '2-circle goniometer' _diffrn_measurement_device_type 'STOE IPDS-2T' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 6.67 _diffrn_detector 'image plate (34 cm diameter / schwenk)' _diffrn_detector_type STOE _diffrn_standards_number 0 _diffrn_reflns_av_R_equivalents 0.0318 _diffrn_reflns_av_unetI/netI 0.0481 _diffrn_reflns_number 26265 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.12 _diffrn_reflns_theta_max 29.18 _diffrn_reflns_theta_full 29.18 _diffrn_measured_fraction_theta_full 0.981 _diffrn_measured_fraction_theta_max 0.981 _reflns_number_total 12505 _reflns_number_gt 8971 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_cell_refinement 'STOE X-AREA' _computing_data_reduction 'STOE X-AREA, STOE X-RED' _computing_structure_solution ; 'SIR-92' Altomare, A., Cascarano, G., Giacovazzo, C. & Guagliardi, A. (1993) J. Appl. Cryst. 26, 343-350. ; _computing_structure_refinement ; 'SHELXL-97' Sheldrick, G.M. (2008) Acta Cryst. A64, 112 ; _computing_molecular_graphics 'DIAMOND 3.2' _computing_publication_material ; 'WinGX publication routines' Farrugia, L. J. (1999) WinGX, J. Appl. Cryst. 32, 837-838 ; #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0253P)^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_number_reflns 12505 _refine_ls_number_parameters 417 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0488 _refine_ls_R_factor_gt 0.0274 _refine_ls_wR_factor_ref 0.0536 _refine_ls_wR_factor_gt 0.05 _refine_ls_goodness_of_fit_ref 0.861 _refine_ls_restrained_S_all 0.861 _refine_ls_shift/su_max 0.015 _refine_ls_shift/su_mean 0.001 _refine_diff_density_max 1.073 _refine_diff_density_min -0.521 _refine_diff_density_rms 0.063 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.61883(16) 0.28794(18) 0.07043(14) 0.0292(4) Uani 1 1 d . . . H1A H 0.5798 0.252 0.0001 0.035 Uiso 1 1 calc R . . H1B H 0.6955 0.2975 0.0748 0.035 Uiso 1 1 calc R . . C2 C 0.56048(16) 0.20427(18) 0.11226(14) 0.0274(4) Uani 1 1 d . . . H2A H 0.6023 0.2375 0.1813 0.033 Uiso 1 1 calc R . . H2B H 0.5608 0.1275 0.0748 0.033 Uiso 1 1 calc R . . C3 C 0.53366(15) 0.42660(18) 0.38362(13) 0.0255(4) Uani 1 1 d . . . H3A H 0.5197 0.4112 0.3142 0.031 Uiso 1 1 calc R . . H3B H 0.4814 0.4555 0.4118 0.031 Uiso 1 1 calc R . . C4 C 0.65172(16) 0.52244(18) 0.43897(13) 0.0272(4) Uani 1 1 d . . . H4A H 0.6636 0.5429 0.5095 0.033 Uiso 1 1 calc R . . H4B H 0.6614 0.5941 0.4325 0.033 Uiso 1 1 calc R . . C5 C 0.4797(3) 0.6418(3) 0.1414(2) 0.0661(8) Uani 1 1 d . . . H5A H 0.5197 0.7269 0.163 0.099 Uiso 1 1 calc R . . H5B H 0.4278 0.6034 0.0764 0.099 Uiso 1 1 calc R . . H5C H 0.5328 0.609 0.1381 0.099 Uiso 1 1 calc R . . C6 C 0.4148(2) 0.6201(2) 0.21538(17) 0.0392(5) Uani 1 1 d . . . H6 H 0.3592 0.6515 0.2164 0.047 Uiso 1 1 calc R . . C7 C 0.4939(2) 0.6848(2) 0.3186(2) 0.0606(7) Uani 1 1 d . . . H7A H 0.5432 0.6486 0.3206 0.091 Uiso 1 1 calc R . . H7B H 0.4508 0.6793 0.3661 0.091 Uiso 1 1 calc R . . H7C H 0.538 0.768 0.3353 0.091 Uiso 1 1 calc R . . C8 C 0.1738(3) 0.4754(3) 0.0567(2) 0.0732(9) Uani 1 1 d . . . H8A H 0.2305 0.5372 0.0469 0.11 Uiso 1 1 calc R . . H8B H 0.1535 0.5117 0.1164 0.11 Uiso 1 1 calc R . . H8C H 0.1081 0.4299 0.0002 0.11 Uiso 1 1 calc R . . C9 C 0.2198(2) 0.3926(3) 0.0669(2) 0.0584(7) Uani 1 1 d . . . H9 H 0.1582 0.3326 0.0769 0.07 Uiso 1 1 calc R . . C10 C 0.2394(3) 0.3236(3) -0.02691(19) 0.0669(8) Uani 1 1 d . . . H10A H 0.1713 0.2821 -0.0805 0.1 Uiso 1 1 calc R . . H10B H 0.2609 0.266 -0.0199 0.1 Uiso 1 1 calc R . . H10C H 0.2989 0.3775 -0.0416 0.1 Uiso 1 1 calc R . . C11 C 0.2055(2) 0.5181(3) 0.3042(2) 0.0596(8) Uani 1 1 d . . . H11A H 0.1371 0.4778 0.2512 0.089 Uiso 1 1 calc R . . H11B H 0.2476 0.5989 0.3138 0.089 Uiso 1 1 calc R . . H11C H 0.187 0.5204 0.365 0.089 Uiso 1 1 calc R . . C12 C 0.27530(19) 0.4515(2) 0.27709(18) 0.0397(5) Uani 1 1 d . . . H12 H 0.3386 0.4909 0.3369 0.048 Uiso 1 1 calc R . . C13 C 0.2131(2) 0.3246(2) 0.2598(2) 0.0548(7) Uani 1 1 d . . . H13A H 0.1858 0.3239 0.3167 0.082 Uiso 1 1 calc R . . H13B H 0.2631 0.2877 0.2507 0.082 Uiso 1 1 calc R . . H13C H 0.1502 0.2806 0.201 0.082 Uiso 1 1 calc R . . C14 C 0.19855(19) 0.1498(2) 0.40088(16) 0.0397(5) Uani 1 1 d . . . H14A H 0.1537 0.187 0.4323 0.059 Uiso 1 1 calc R . . H14B H 0.2654 0.2096 0.3987 0.059 Uiso 1 1 calc R . . H14C H 0.2197 0.1141 0.4385 0.059 Uiso 1 1 calc R . . C15 C 0.13060(15) 0.05356(18) 0.29551(14) 0.0272(4) Uani 1 1 d . . . H15 H 0.1058 0.0929 0.2619 0.033 Uiso 1 1 calc R . . C16 C 0.02492(18) -0.0406(2) 0.29742(19) 0.0431(5) Uani 1 1 d . . . H16A H 0.0452 -0.0785 0.3333 0.065 Uiso 1 1 calc R . . H16B H -0.0186 -0.1 0.2301 0.065 Uiso 1 1 calc R . . H16C H -0.0192 -0.0032 0.3302 0.065 Uiso 1 1 calc R . . C17 C 0.0822(2) -0.0418(3) 0.05769(18) 0.0511(6) Uani 1 1 d . . . H17A H 0.1438 0.029 0.0633 0.077 Uiso 1 1 calc R . . H17B H 0.0325 -0.0192 0.0945 0.077 Uiso 1 1 calc R . . H17C H 0.0412 -0.0946 -0.0115 0.077 Uiso 1 1 calc R . . C18 C 0.12821(17) -0.10608(19) 0.09988(15) 0.0341(5) Uani 1 1 d . . . H18 H 0.0648 -0.1717 0.1023 0.041 Uiso 1 1 calc R . . C19 C 0.1923(2) -0.1583(2) 0.03372(16) 0.0487(6) Uani 1 1 d . . . H19A H 0.1437 -0.2111 -0.0332 0.073 Uiso 1 1 calc R . . H19B H 0.2173 -0.2027 0.0589 0.073 Uiso 1 1 calc R . . H19C H 0.2567 -0.0943 0.0333 0.073 Uiso 1 1 calc R . . C20 C 0.35934(18) -0.0928(2) 0.27331(18) 0.0399(5) Uani 1 1 d . . . H20A H 0.3743 -0.1366 0.3056 0.06 Uiso 1 1 calc R . . H20B H 0.417 -0.0108 0.3063 0.06 Uiso 1 1 calc R . . H20C H 0.3592 -0.1292 0.2044 0.06 Uiso 1 1 calc R . . C21 C 0.24509(16) -0.09572(18) 0.27905(15) 0.0290(4) Uani 1 1 d . . . H21 H 0.2501 -0.0566 0.3505 0.035 Uiso 1 1 calc R . . C22 C 0.1550(2) -0.2231(2) 0.2379(2) 0.0455(6) Uani 1 1 d . . . H22A H 0.1513 -0.2675 0.1691 0.068 Uiso 1 1 calc R . . H22B H 0.0833 -0.2233 0.2423 0.068 Uiso 1 1 calc R . . H22C H 0.1729 -0.26 0.276 0.068 Uiso 1 1 calc R . . C23 C 0.64349(19) 0.1037(2) 0.48247(16) 0.0408(5) Uani 1 1 d . . . H23A H 0.6028 0.0412 0.4998 0.061 Uiso 1 1 calc R . . H23B H 0.5943 0.1346 0.466 0.061 Uiso 1 1 calc R . . H23C H 0.7069 0.1676 0.5383 0.061 Uiso 1 1 calc R . . C24 C 0.68513(16) 0.05318(18) 0.39351(14) 0.0295(4) Uani 1 1 d . . . H24 H 0.618 -0.0152 0.3409 0.035 Uiso 1 1 calc R . . C25 C 0.7608(2) 0.0011(2) 0.4165(2) 0.0465(6) Uani 1 1 d . . . H25A H 0.8274 0.0643 0.4693 0.07 Uiso 1 1 calc R . . H25B H 0.7821 -0.0357 0.3576 0.07 Uiso 1 1 calc R . . H25C H 0.7207 -0.0584 0.4372 0.07 Uiso 1 1 calc R . . C26 C 0.92265(18) 0.3156(2) 0.50982(17) 0.0493(6) Uani 1 1 d . . . H26A H 1.0033 0.3583 0.5375 0.074 Uiso 1 1 calc R . . H26B H 0.8904 0.2658 0.5412 0.074 Uiso 1 1 calc R . . H26C H 0.8922 0.3722 0.5215 0.074 Uiso 1 1 calc R . . C27 C 0.89450(15) 0.23782(19) 0.39887(15) 0.0317(4) Uani 1 1 d . . . H27 H 0.9222 0.1774 0.3876 0.038 Uiso 1 1 calc R . . C28 C 0.95193(19) 0.3149(2) 0.3505(2) 0.0502(6) Uani 1 1 d . . . H28A H 0.9205 0.3698 0.3562 0.075 Uiso 1 1 calc R . . H28B H 0.9403 0.2644 0.281 0.075 Uiso 1 1 calc R . . H28C H 1.0315 0.3597 0.3836 0.075 Uiso 1 1 calc R . . C29 C 0.59574(19) -0.01202(19) 0.16023(15) 0.0384(5) Uani 1 1 d . . . H29A H 0.5825 -0.045 0.0888 0.058 Uiso 1 1 calc R . . H29B H 0.5538 0.0332 0.1815 0.058 Uiso 1 1 calc R . . H29C H 0.5717 -0.0763 0.1786 0.058 Uiso 1 1 calc R . . C30 C 0.72067(17) 0.07001(19) 0.21032(14) 0.0315(4) Uani 1 1 d . . . H30 H 0.7434 0.1263 0.1815 0.038 Uiso 1 1 calc R . . C31 C 0.7875(2) 0.0000(3) 0.18276(18) 0.0561(7) Uani 1 1 d . . . H31A H 0.764 -0.0609 0.2049 0.084 Uiso 1 1 calc R . . H31B H 0.8665 0.0534 0.2143 0.084 Uiso 1 1 calc R . . H31C H 0.7747 -0.0374 0.1114 0.084 Uiso 1 1 calc R . . C32 C 0.89773(17) 0.4899(2) 0.21668(16) 0.0401(5) Uani 1 1 d . . . H32A H 0.9043 0.5001 0.1575 0.06 Uiso 1 1 calc R . . H32B H 0.8754 0.407 0.2006 0.06 Uiso 1 1 calc R . . H32C H 0.9694 0.5398 0.2667 0.06 Uiso 1 1 calc R . . C33 C 0.8122(2) 0.7046(2) 0.32382(17) 0.0429(5) Uani 1 1 d . . . H33A H 0.8821 0.7543 0.376 0.064 Uiso 1 1 calc R . . H33B H 0.7513 0.7129 0.3509 0.064 Uiso 1 1 calc R . . H33C H 0.8168 0.7293 0.2719 0.064 Uiso 1 1 calc R . . P1 P 0.34062(4) 0.45996(5) 0.17573(4) 0.02779(11) Uani 1 1 d . . . P2 P 0.22080(4) -0.00131(4) 0.22676(3) 0.02173(9) Uani 1 1 d . . . P3 P 0.74199(4) 0.16126(4) 0.34366(3) 0.02152(9) Uani 1 1 d . . . S1 S 0.62367(4) 0.43406(4) 0.13420(3) 0.02651(10) Uani 1 1 d . . . S2 S 0.41582(4) 0.17972(4) 0.10723(3) 0.02537(10) Uani 1 1 d . . . S3 S 0.50558(4) 0.28667(5) 0.38822(3) 0.02612(10) Uani 1 1 d . . . S4 S 0.75663(4) 0.47767(4) 0.39411(3) 0.02509(9) Uani 1 1 d . . . Cu1 Cu 0.445591(19) 0.36742(2) 0.150176(16) 0.02598(5) Uani 1 1 d . . . Cu2 Cu 0.377649(18) 0.14737(2) 0.238961(17) 0.02466(5) Uani 1 1 d . . . Cu3 Cu 0.666089(18) 0.28276(2) 0.364836(16) 0.02382(5) Uani 1 1 d . . . Ga1 Ga 0.784201(17) 0.536078(19) 0.267996(15) 0.02645(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0276(9) 0.0311(11) 0.0256(9) 0.0092(8) 0.0111(8) 0.0130(8) C2 0.0324(10) 0.0269(10) 0.0241(9) 0.0097(8) 0.0070(8) 0.0168(8) C3 0.0239(9) 0.0325(11) 0.0227(9) 0.0125(8) 0.0078(7) 0.0151(8) C4 0.0301(10) 0.0247(10) 0.0230(9) 0.0073(8) 0.0077(7) 0.0123(8) C5 0.084(2) 0.0601(19) 0.088(2) 0.0576(18) 0.0436(18) 0.0370(17) C6 0.0475(13) 0.0308(12) 0.0498(13) 0.0236(11) 0.0170(11) 0.0218(10) C7 0.0575(16) 0.0354(14) 0.0599(17) 0.0103(13) 0.0037(13) 0.0074(13) C8 0.073(2) 0.081(2) 0.0688(19) 0.0271(18) -0.0092(16) 0.0517(19) C9 0.0594(17) 0.0586(18) 0.0492(15) 0.0153(14) -0.0048(12) 0.0325(15) C10 0.081(2) 0.065(2) 0.0369(14) 0.0091(14) -0.0042(13) 0.0350(18) C11 0.0678(18) 0.0577(18) 0.092(2) 0.0449(17) 0.0532(17) 0.0478(16) C12 0.0419(12) 0.0412(13) 0.0518(13) 0.0262(11) 0.0244(11) 0.0264(11) C13 0.0579(16) 0.0497(16) 0.084(2) 0.0431(16) 0.0439(15) 0.0329(14) C14 0.0424(12) 0.0370(13) 0.0352(11) 0.0095(10) 0.0173(10) 0.0194(10) C15 0.0245(9) 0.0256(10) 0.0343(10) 0.0143(9) 0.0113(8) 0.0126(8) C16 0.0293(11) 0.0395(13) 0.0608(15) 0.0216(12) 0.0218(11) 0.0151(10) C17 0.0594(16) 0.0566(17) 0.0350(12) 0.0185(12) -0.0027(11) 0.0296(14) C18 0.0327(11) 0.0282(11) 0.0287(10) 0.0069(9) -0.0005(8) 0.0097(9) C19 0.0608(16) 0.0419(14) 0.0294(11) 0.0043(11) 0.0081(11) 0.0229(13) C20 0.0360(11) 0.0465(14) 0.0537(14) 0.0299(12) 0.0143(10) 0.0269(11) C21 0.0314(10) 0.0288(11) 0.0361(10) 0.0194(9) 0.0120(8) 0.0172(9) C22 0.0462(13) 0.0330(13) 0.0691(16) 0.0324(13) 0.0179(12) 0.0194(11) C23 0.0377(12) 0.0538(15) 0.0362(11) 0.0276(11) 0.0145(9) 0.0176(11) C24 0.0266(9) 0.0304(11) 0.0306(10) 0.0176(9) 0.0038(8) 0.0090(8) C25 0.0475(13) 0.0495(15) 0.0619(15) 0.0387(14) 0.0157(12) 0.0267(12) C26 0.0260(11) 0.0465(15) 0.0399(12) 0.0031(11) -0.0029(9) 0.0018(10) C27 0.0215(9) 0.0303(11) 0.0397(11) 0.0138(9) 0.0083(8) 0.0106(8) C28 0.0303(11) 0.0479(15) 0.0755(18) 0.0343(14) 0.0239(12) 0.0123(11) C29 0.0509(13) 0.0252(11) 0.0231(10) 0.0054(9) -0.0021(9) 0.0102(10) C30 0.0415(11) 0.0303(11) 0.0236(9) 0.0101(9) 0.0088(8) 0.0194(9) C31 0.0756(19) 0.0651(19) 0.0346(12) 0.0086(13) 0.0146(12) 0.0531(17) C32 0.0278(10) 0.0521(15) 0.0371(11) 0.0177(11) 0.0122(9) 0.0170(10) C33 0.0521(14) 0.0245(11) 0.0439(13) 0.0159(10) 0.0141(11) 0.0089(10) P1 0.0305(3) 0.0259(3) 0.0305(3) 0.0122(2) 0.0074(2) 0.0171(2) P2 0.0212(2) 0.0193(2) 0.0236(2) 0.00995(19) 0.00558(18) 0.00802(19) P3 0.0204(2) 0.0207(2) 0.0217(2) 0.00865(19) 0.00540(17) 0.00863(18) S1 0.0262(2) 0.0261(2) 0.0285(2) 0.0146(2) 0.00836(18) 0.01072(19) S2 0.0269(2) 0.0239(2) 0.0242(2) 0.01192(19) 0.00686(18) 0.00937(19) S3 0.0195(2) 0.0311(3) 0.0278(2) 0.0168(2) 0.00632(17) 0.00804(19) S4 0.0194(2) 0.0235(2) 0.0288(2) 0.0117(2) 0.00605(17) 0.00671(18) Cu1 0.02912(12) 0.02907(13) 0.02539(11) 0.01277(10) 0.00942(9) 0.01779(10) Cu2 0.02401(11) 0.02213(12) 0.02931(12) 0.01325(10) 0.01006(9) 0.00971(9) Cu3 0.02473(11) 0.02340(12) 0.02333(11) 0.00967(10) 0.00622(9) 0.01194(9) Ga1 0.02293(10) 0.02336(11) 0.02897(11) 0.01171(9) 0.00897(8) 0.00634(9) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.530(3) . ? C1 S1 1.835(2) . ? C2 S2 1.8489(19) . ? C3 C4 1.522(3) . ? C3 S3 1.849(2) . ? C4 S4 1.8394(19) . ? C5 C6 1.547(3) . ? C6 C7 1.532(4) . ? C6 P1 1.847(2) . ? C8 C9 1.542(4) . ? C9 C10 1.499(4) . ? C9 P1 1.874(3) . ? C11 C12 1.530(3) . ? C12 C13 1.523(3) . ? C12 P1 1.878(2) . ? C14 C15 1.542(3) . ? C15 C16 1.537(3) . ? C15 P2 1.8673(19) . ? C17 C18 1.546(3) . ? C18 C19 1.538(3) . ? C18 P2 1.865(2) . ? C20 C21 1.546(3) . ? C21 C22 1.532(3) . ? C21 P2 1.8814(19) . ? C23 C24 1.538(3) . ? C24 C25 1.544(3) . ? C24 P3 1.8752(19) . ? C26 C27 1.536(3) . ? C27 C28 1.541(3) . ? C27 P3 1.8590(19) . ? C29 C30 1.544(3) . ? C30 C31 1.530(3) . ? C30 P3 1.867(2) . ? C32 Ga1 1.990(2) . ? C33 Ga1 1.999(2) . ? P1 Cu1 2.2110(6) . ? P2 Cu2 2.2534(5) . ? P3 Cu3 2.2150(6) . ? S1 Cu1 2.3082(5) . ? S1 Ga1 2.3679(6) . ? S2 Cu1 2.2616(6) . ? S2 Cu2 2.2976(5) . ? S3 Cu3 2.2534(5) . ? S3 Cu2 2.3071(6) . ? S4 Cu3 2.3192(6) . ? S4 Ga1 2.3790(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 C2 C1 S1 113.25(13) . . ? C1 C2 S2 112.55(13) . . ? C4 C3 S3 113.26(13) . . ? C3 C4 S4 112.85(13) . . ? C7 C6 C5 110.3(2) . . ? C7 C6 P1 110.86(16) . . ? C5 C6 P1 109.58(18) . . ? C10 C9 C8 111.7(2) . . ? C10 C9 P1 112.1(2) . . ? C8 C9 P1 116.6(2) . . ? C13 C12 C11 111.7(2) . . ? C13 C12 P1 111.60(17) . . ? C11 C12 P1 116.21(17) . . ? C16 C15 C14 110.19(17) . . ? C16 C15 P2 116.29(15) . . ? C14 C15 P2 110.42(13) . . ? C19 C18 C17 110.11(19) . . ? C19 C18 P2 110.06(15) . . ? C17 C18 P2 110.00(16) . . ? C22 C21 C20 110.54(18) . . ? C22 C21 P2 117.21(14) . . ? C20 C21 P2 109.82(13) . . ? C23 C24 C25 110.61(17) . . ? C23 C24 P3 111.24(15) . . ? C25 C24 P3 116.53(14) . . ? C26 C27 C28 109.5(2) . . ? C26 C27 P3 110.27(14) . . ? C28 C27 P3 110.07(15) . . ? C31 C30 C29 110.49(19) . . ? C31 C30 P3 117.47(15) . . ? C29 C30 P3 109.49(14) . . ? C6 P1 C9 108.56(12) . . ? C6 P1 C12 103.49(11) . . ? C9 P1 C12 104.06(13) . . ? C6 P1 Cu1 114.98(8) . . ? C9 P1 Cu1 112.81(9) . . ? C12 P1 Cu1 112.00(7) . . ? C18 P2 C15 104.14(9) . . ? C18 P2 C21 105.54(10) . . ? C15 P2 C21 104.51(9) . . ? C18 P2 Cu2 115.57(7) . . ? C15 P2 Cu2 112.13(6) . . ? C21 P2 Cu2 113.87(6) . . ? C27 P3 C30 105.38(9) . . ? C27 P3 C24 105.61(9) . . ? C30 P3 C24 105.56(10) . . ? C27 P3 Cu3 113.75(7) . . ? C30 P3 Cu3 110.66(7) . . ? C24 P3 Cu3 115.09(7) . . ? C1 S1 Cu1 96.27(6) . . ? C1 S1 Ga1 102.60(7) . . ? Cu1 S1 Ga1 123.45(2) . . ? C2 S2 Cu1 97.40(7) . . ? C2 S2 Cu2 106.43(6) . . ? Cu1 S2 Cu2 105.75(2) . . ? C3 S3 Cu3 97.46(6) . . ? C3 S3 Cu2 102.40(6) . . ? Cu3 S3 Cu2 103.78(2) . . ? C4 S4 Cu3 97.21(7) . . ? C4 S4 Ga1 103.70(6) . . ? Cu3 S4 Ga1 123.74(2) . . ? P1 Cu1 S2 134.83(2) . . ? P1 Cu1 S1 128.34(2) . . ? S2 Cu1 S1 96.14(2) . . ? P2 Cu2 S2 122.92(2) . . ? P2 Cu2 S3 121.75(2) . . ? S2 Cu2 S3 115.18(2) . . ? P3 Cu3 S3 137.88(2) . . ? P3 Cu3 S4 125.95(2) . . ? S3 Cu3 S4 95.62(2) . . ? C32 Ga1 C33 120.16(10) . . ? C32 Ga1 S1 106.70(7) . . ? C33 Ga1 S1 104.41(8) . . ? C32 Ga1 S4 105.48(7) . . ? C33 Ga1 S4 107.34(7) . . ? S1 Ga1 S4 112.981(18) . . ? _chemical_name_common ; bis(mu!3$-1,2-dithiolatoethane-S,S,S',S')-dimethanido - tris(triisopropylphosphine)-tricopper(+1)-gallium(+3) ; data_[(iPr3PCu)3(SC2H4S)2GaEt2] _database_code_depnum_ccdc_archive 'CCDC 907024' #TrackingRef '17884_web_deposit_cif_file_0_DirkFriedrich_1361280301.26_[(iPr3PCu)3(SC2H4S)2GaEt2].cif' _audit_creation_date 2013-02-14T13:13:45-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; bis(\m~3~-1,2-dithiolatoethane-S,S,S',S')-diethanido -tris(triisopropylphosphine)-tricopper(+1)-gallium(+3) ; _chemical_formula_moiety 'C35 H81 Cu3 Ga1 P3 S4' _chemical_formula_sum 'C35 H81 Cu3 Ga P3 S4' _chemical_formula_weight 983.49 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.5627(11) _cell_length_b 13.9556(11) _cell_length_c 16.0504(14) _cell_angle_alpha 64.190(6) _cell_angle_beta 68.597(7) _cell_angle_gamma 66.960(6) _cell_volume 2446.4(3) _cell_formula_units_Z 2 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 16807 _cell_measurement_theta_min 1.95 _cell_measurement_theta_max 29.37 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.462 _exptl_crystal_size_mid 0.41 _exptl_crystal_size_min 0.365 _exptl_crystal_density_diffrn 1.335 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1036 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 2.12 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details ; Busing, W. R. & Levy, H. A. (1957) Acta Cryst. 10, 180-182. and Coppens, P., Leiserowitz, L. & Rabinovich, D. (1965) Acta Cryst. 1965, 1035-1038. ; _exptl_absorpt_correction_T_min 0.4452 _exptl_absorpt_correction_T_max 0.5447 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 180(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 '2-circle goniometer' _diffrn_measurement_device_type 'STOE IPDS-2T' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 6.67 _diffrn_detector 'image plate (34 cm diameter / schwenk)' _diffrn_detector_type STOE _diffrn_standards_number 0 _diffrn_reflns_av_R_equivalents 0.0346 _diffrn_reflns_av_unetI/netI 0.059 _diffrn_reflns_number 22102 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.94 _diffrn_reflns_theta_max 27 _diffrn_reflns_theta_full 27 _diffrn_measured_fraction_theta_full 0.992 _diffrn_measured_fraction_theta_max 0.992 _reflns_number_total 10610 _reflns_number_gt 7445 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_cell_refinement 'STOE X-AREA' _computing_data_reduction 'STOE X-AREA, STOE X-RED' _computing_structure_solution ; 'SIR-92' Altomare, A., Cascarano, G., Giacovazzo, C. & Guagliardi, A. (1993) J. Appl. Cryst. 26, 343-350. ; _computing_structure_refinement ; 'SHELXL-97' Sheldrick, G.M. (2008) Acta Cryst. A64, 112 ; _computing_molecular_graphics 'DIAMOND 3.2' _computing_publication_material ; 'WinGX publication routines' Farrugia, L. J. (1999) WinGX, J. Appl. Cryst. 32, 837-838 ; #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0338P)^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_number_reflns 10610 _refine_ls_number_parameters 521 _refine_ls_number_restraints 183 _refine_ls_R_factor_all 0.058 _refine_ls_R_factor_gt 0.0344 _refine_ls_wR_factor_ref 0.0745 _refine_ls_wR_factor_gt 0.0706 _refine_ls_goodness_of_fit_ref 0.94 _refine_ls_restrained_S_all 0.962 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.022 _refine_diff_density_min -0.904 _refine_diff_density_rms 0.066 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.6656(2) 0.3852(3) 0.0565(2) 0.0311(7) Uani 1 1 d . B . H1A H 0.6742 0.4371 -0.01 0.037 Uiso 1 1 calc R . . H1B H 0.679 0.3108 0.0551 0.037 Uiso 1 1 calc R . . C2 C 0.5475(2) 0.4219(2) 0.1119(2) 0.0284(6) Uani 1 1 d . B . H2A H 0.5375 0.3676 0.1774 0.034 Uiso 1 1 calc R . . H2B H 0.4959 0.4225 0.0811 0.034 Uiso 1 1 calc R . . C3A C 0.5759(3) 0.3910(3) 0.3767(3) 0.0290(9) Uiso 0.782(9) 1 d PD A 1 H3A1 H 0.6102 0.4224 0.3084 0.035 Uiso 0.782(9) 1 calc PR A 1 H3A2 H 0.5783 0.4349 0.4102 0.035 Uiso 0.782(9) 1 calc PR A 1 C4A C 0.6418(3) 0.2723(4) 0.4160(3) 0.0290(9) Uiso 0.782(9) 1 d PD A 1 H4A1 H 0.6105 0.2421 0.4852 0.035 Uiso 0.782(9) 1 calc PR A 1 H4A2 H 0.7188 0.2702 0.407 0.035 Uiso 0.782(9) 1 calc PR A 1 C3B C 0.5305(11) 0.3756(16) 0.4436(13) 0.051(5) Uiso 0.218(9) 1 d PD A 2 H3B1 H 0.5347 0.4433 0.4464 0.061 Uiso 0.218(9) 1 calc PR A 2 H3B2 H 0.5215 0.3197 0.5083 0.061 Uiso 0.218(9) 1 calc PR A 2 C4B C 0.6303(11) 0.3302(13) 0.3739(12) 0.033(4) Uiso 0.218(9) 1 d PD A 2 H4B1 H 0.6971 0.3174 0.3932 0.04 Uiso 0.218(9) 1 calc PR A 2 H4B2 H 0.6328 0.3889 0.3104 0.04 Uiso 0.218(9) 1 calc PR A 2 C5A C 0.9281(7) 0.6299(9) 0.0391(6) 0.099(3) Uani 0.682(7) 1 d PDU B 1 H5A1 H 1.0085 0.6142 0.0221 0.149 Uiso 0.682(7) 1 calc PR B 1 H5A2 H 0.8956 0.7069 0.0028 0.149 Uiso 0.682(7) 1 calc PR B 1 H5A3 H 0.9077 0.5801 0.0241 0.149 Uiso 0.682(7) 1 calc PR B 1 C6A C 0.8849(6) 0.6117(7) 0.1459(6) 0.061(2) Uani 0.682(7) 1 d PDU B 1 H6A H 0.9062 0.6621 0.1612 0.073 Uiso 0.682(7) 1 calc PR B 1 C7A C 0.9303(6) 0.4909(7) 0.2070(8) 0.088(3) Uani 0.682(7) 1 d PDU B 1 H7A1 H 0.9058 0.4417 0.1949 0.132 Uiso 0.682(7) 1 calc PR B 1 H7A2 H 0.903 0.4832 0.2745 0.132 Uiso 0.682(7) 1 calc PR B 1 H7A3 H 1.011 0.4708 0.1904 0.132 Uiso 0.682(7) 1 calc PR B 1 C5B C 0.9703(11) 0.5379(14) 0.1041(11) 0.060(4) Uani 0.318(7) 1 d PDU B 2 H5B1 H 1.046 0.5066 0.1122 0.091 Uiso 0.318(7) 1 calc PR B 2 H5B2 H 0.9668 0.6023 0.0454 0.091 Uiso 0.318(7) 1 calc PR B 2 H5B3 H 0.9473 0.4818 0.1002 0.091 Uiso 0.318(7) 1 calc PR B 2 C6B C 0.8933(9) 0.5736(10) 0.1893(7) 0.022(3) Uani 0.318(7) 1 d PDU B 2 H6B H 0.9185 0.6302 0.1922 0.027 Uiso 0.318(7) 1 calc PR B 2 C7B C 0.9058(12) 0.4709(9) 0.2809(10) 0.048(3) Uani 0.318(7) 1 d PDU B 2 H7B1 H 0.8778 0.4158 0.2812 0.072 Uiso 0.318(7) 1 calc PR B 2 H7B2 H 0.8638 0.4933 0.3368 0.072 Uiso 0.318(7) 1 calc PR B 2 H7B3 H 0.9838 0.4387 0.2826 0.072 Uiso 0.318(7) 1 calc PR B 2 C8A C 0.7534(7) 0.8689(6) 0.1040(6) 0.064(2) Uani 0.682(7) 1 d PDU B 1 H8A1 H 0.8265 0.849 0.0631 0.095 Uiso 0.682(7) 1 calc PR B 1 H8A2 H 0.7611 0.8559 0.1668 0.095 Uiso 0.682(7) 1 calc PR B 1 H8A3 H 0.7167 0.9473 0.0752 0.095 Uiso 0.682(7) 1 calc PR B 1 C9A C 0.6836(5) 0.7968(5) 0.1151(4) 0.0418(14) Uani 0.682(7) 1 d PDU B 1 H9A H 0.6094 0.8215 0.1556 0.05 Uiso 0.682(7) 1 calc PR B 1 C10A C 0.6649(7) 0.8199(6) 0.0184(5) 0.066(2) Uani 0.682(7) 1 d PDU B 1 H10A H 0.6144 0.894 -0.0022 0.099 Uiso 0.682(7) 1 calc PR B 1 H10B H 0.6328 0.7645 0.0246 0.099 Uiso 0.682(7) 1 calc PR B 1 H10C H 0.7355 0.8158 -0.0289 0.099 Uiso 0.682(7) 1 calc PR B 1 C8B C 0.8260(19) 0.8330(18) 0.0658(17) 0.093(6) Uani 0.318(7) 1 d PDU B 2 H8B1 H 0.899 0.802 0.0302 0.139 Uiso 0.318(7) 1 calc PR B 2 H8B2 H 0.8319 0.8274 0.127 0.139 Uiso 0.318(7) 1 calc PR B 2 H8B3 H 0.7976 0.911 0.029 0.139 Uiso 0.318(7) 1 calc PR B 2 C9B C 0.7463(17) 0.7675(16) 0.0838(13) 0.081(6) Uani 0.318(7) 1 d PDU B 2 H9B H 0.6717 0.819 0.0984 0.098 Uiso 0.318(7) 1 calc PR B 2 C10B C 0.752(2) 0.761(2) -0.0122(15) 0.119(8) Uani 0.318(7) 1 d PDU B 2 H10D H 0.7581 0.8319 -0.0631 0.178 Uiso 0.318(7) 1 calc PR B 2 H10E H 0.6846 0.7465 -0.0074 0.178 Uiso 0.318(7) 1 calc PR B 2 H10F H 0.8161 0.7015 -0.0264 0.178 Uiso 0.318(7) 1 calc PR B 2 C11A C 0.7435(8) 0.6738(8) 0.3432(6) 0.066(2) Uani 0.682(7) 1 d PDU B 1 H11A H 0.7187 0.7549 0.3177 0.098 Uiso 0.682(7) 1 calc PR B 1 H11B H 0.8237 0.6487 0.3209 0.098 Uiso 0.682(7) 1 calc PR B 1 H11C H 0.7236 0.6487 0.4129 0.098 Uiso 0.682(7) 1 calc PR B 1 C12A C 0.6879(6) 0.6255(7) 0.3089(6) 0.0362(17) Uani 0.682(7) 1 d PDU B 1 H12A H 0.7075 0.5439 0.3444 0.043 Uiso 0.682(7) 1 calc PR B 1 C13A C 0.5604(5) 0.6667(6) 0.3386(5) 0.0453(15) Uani 0.682(7) 1 d PDU B 1 H13A H 0.5362 0.6415 0.4082 0.068 Uiso 0.682(7) 1 calc PR B 1 H13B H 0.5277 0.6368 0.3133 0.068 Uiso 0.682(7) 1 calc PR B 1 H13C H 0.5368 0.7478 0.3131 0.068 Uiso 0.682(7) 1 calc PR B 1 C11B C 0.7168(12) 0.7306(15) 0.3149(14) 0.057(4) Uani 0.318(7) 1 d PDU B 2 H11D H 0.7054 0.8066 0.2695 0.085 Uiso 0.318(7) 1 calc PR B 2 H11E H 0.7954 0.6975 0.3145 0.085 Uiso 0.318(7) 1 calc PR B 2 H11F H 0.6747 0.7316 0.379 0.085 Uiso 0.318(7) 1 calc PR B 2 C12B C 0.6774(13) 0.6614(15) 0.2862(15) 0.047(5) Uani 0.318(7) 1 d PDU B 2 H12B H 0.684 0.5867 0.337 0.057 Uiso 0.318(7) 1 calc PR B 2 C13B C 0.5530(12) 0.7166(19) 0.2866(17) 0.083(6) Uani 0.318(7) 1 d PDU B 2 H13D H 0.5153 0.7423 0.3412 0.124 Uiso 0.318(7) 1 calc PR B 2 H13E H 0.5203 0.6625 0.2914 0.124 Uiso 0.318(7) 1 calc PR B 2 H13F H 0.5451 0.7798 0.2276 0.124 Uiso 0.318(7) 1 calc PR B 2 C14 C 0.3604(4) 0.8485(4) 0.1238(4) 0.0719(14) Uani 1 1 d . . . H14A H 0.3225 0.8628 0.0762 0.108 Uiso 1 1 calc R . . H14B H 0.4218 0.7809 0.1266 0.108 Uiso 1 1 calc R . . H14C H 0.3887 0.9112 0.106 0.108 Uiso 1 1 calc R . . C15 C 0.2789(3) 0.8337(3) 0.2219(3) 0.0425(9) Uani 1 1 d . . . H15 H 0.3207 0.8241 0.2663 0.051 Uiso 1 1 calc R . . C16 C 0.1841(3) 0.9405(3) 0.2207(4) 0.0598(12) Uani 1 1 d . . . H16A H 0.2141 1.0016 0.2042 0.09 Uiso 1 1 calc R . . H16B H 0.1334 0.9297 0.2838 0.09 Uiso 1 1 calc R . . H16C H 0.1443 0.9582 0.1734 0.09 Uiso 1 1 calc R . . C17 C 0.0247(3) 0.7938(3) 0.2215(3) 0.0529(11) Uani 1 1 d . . . H17A H -0.0118 0.8171 0.1704 0.079 Uiso 1 1 calc R . . H17B H 0.0207 0.8592 0.2325 0.079 Uiso 1 1 calc R . . H17C H -0.0121 0.7452 0.28 0.079 Uiso 1 1 calc R . . C18 C 0.1464(3) 0.7309(3) 0.1925(3) 0.0374(8) Uani 1 1 d . . . H18 H 0.1765 0.7787 0.1273 0.045 Uiso 1 1 calc R . . C19 C 0.1546(3) 0.6233(3) 0.1827(3) 0.0504(10) Uani 1 1 d . . . H19A H 0.1212 0.5754 0.2441 0.076 Uiso 1 1 calc R . . H19B H 0.2323 0.5849 0.1629 0.076 Uiso 1 1 calc R . . H19C H 0.1157 0.6407 0.1349 0.076 Uiso 1 1 calc R . . C20 C 0.2146(3) 0.6945(4) 0.4511(3) 0.0545(11) Uani 1 1 d . . . H20A H 0.1695 0.6851 0.5162 0.082 Uiso 1 1 calc R . . H20B H 0.2328 0.7652 0.424 0.082 Uiso 1 1 calc R . . H20C H 0.2827 0.6336 0.452 0.082 Uiso 1 1 calc R . . C21 C 0.1497(3) 0.6942(3) 0.3898(3) 0.0398(8) Uani 1 1 d . . . H21 H 0.0837 0.7603 0.3846 0.048 Uiso 1 1 calc R . . C22 C 0.1113(3) 0.5893(4) 0.4354(3) 0.0534(10) Uani 1 1 d . . . H22A H 0.1756 0.5244 0.4364 0.08 Uiso 1 1 calc R . . H22B H 0.0654 0.5931 0.3983 0.08 Uiso 1 1 calc R . . H22C H 0.0682 0.5831 0.5006 0.08 Uiso 1 1 calc R . . C23 C 0.2060(3) 0.2024(5) 0.5079(3) 0.0687(14) Uani 1 1 d . . . H23A H 0.1324 0.2375 0.5397 0.103 Uiso 1 1 calc R . . H23B H 0.2604 0.231 0.5098 0.103 Uiso 1 1 calc R . . H23C H 0.2237 0.122 0.5407 0.103 Uiso 1 1 calc R . . C24 C 0.2085(3) 0.2291(3) 0.4023(3) 0.0463(9) Uani 1 1 d . . . H24 H 0.187 0.3117 0.373 0.056 Uiso 1 1 calc R . . C25 C 0.1199(3) 0.1901(4) 0.3975(4) 0.0659(13) Uani 1 1 d . . . H25A H 0.1317 0.1105 0.433 0.099 Uiso 1 1 calc R . . H25B H 0.1246 0.2045 0.3309 0.099 Uiso 1 1 calc R . . H25C H 0.0468 0.2305 0.4255 0.099 Uiso 1 1 calc R . . C26 C 0.3460(4) -0.0295(3) 0.3480(4) 0.0650(13) Uani 1 1 d . . . H26A H 0.3854 -0.0193 0.2814 0.097 Uiso 1 1 calc R . . H26B H 0.2668 0.0048 0.3519 0.097 Uiso 1 1 calc R . . H26C H 0.3591 -0.1089 0.385 0.097 Uiso 1 1 calc R . . C27 C 0.3881(3) 0.0254(3) 0.3889(3) 0.0414(8) Uani 1 1 d . . . H27 H 0.351 0.0066 0.4582 0.05 Uiso 1 1 calc R . . C28 C 0.5122(3) -0.0282(3) 0.3829(3) 0.0527(10) Uani 1 1 d . . . H28A H 0.5254 -0.1078 0.419 0.079 Uiso 1 1 calc R . . H28B H 0.5384 0.0058 0.4097 0.079 Uiso 1 1 calc R . . H28C H 0.5518 -0.017 0.3162 0.079 Uiso 1 1 calc R . . C29 C 0.4631(3) 0.1817(3) 0.1514(3) 0.0472(9) Uani 1 1 d . . . H29A H 0.4607 0.2118 0.0842 0.071 Uiso 1 1 calc R . . H29B H 0.49 0.1007 0.1717 0.071 Uiso 1 1 calc R . . H29C H 0.5128 0.2108 0.1595 0.071 Uiso 1 1 calc R . . C30 C 0.3452(3) 0.2164(3) 0.2129(3) 0.0379(8) Uani 1 1 d . . . H30 H 0.2993 0.1745 0.214 0.045 Uiso 1 1 calc R . . C31 C 0.2912(3) 0.3404(3) 0.1707(3) 0.0521(10) Uani 1 1 d . . . H31A H 0.3253 0.3825 0.182 0.078 Uiso 1 1 calc R . . H31B H 0.2122 0.3571 0.201 0.078 Uiso 1 1 calc R . . H31C H 0.3013 0.3609 0.102 0.078 Uiso 1 1 calc R . . C32 C 0.8896(3) 0.0963(4) 0.0768(3) 0.0580(11) Uani 1 1 d . . . H32A H 0.876 0.1706 0.029 0.087 Uiso 1 1 calc R . . H32B H 0.8883 0.0431 0.0529 0.087 Uiso 1 1 calc R . . H32C H 0.9619 0.0754 0.0897 0.087 Uiso 1 1 calc R . . C33 C 0.7997(3) 0.0957(3) 0.1691(3) 0.0417(8) Uani 1 1 d . . . H33A H 0.8129 0.0198 0.2163 0.05 Uiso 1 1 calc R . . H33B H 0.7272 0.1153 0.1557 0.05 Uiso 1 1 calc R . . C34 C 0.9281(3) 0.0731(4) 0.3698(3) 0.0614(12) Uani 1 1 d . . . H34A H 0.8624 0.0874 0.42 0.092 Uiso 1 1 calc R . . H34B H 0.9939 0.0602 0.3896 0.092 Uiso 1 1 calc R . . H34C H 0.9331 0.0075 0.3586 0.092 Uiso 1 1 calc R . . C35 C 0.9204(3) 0.1745(3) 0.2770(3) 0.0446(9) Uani 1 1 d . . . H35A H 0.99 0.1626 0.2283 0.053 Uiso 1 1 calc R . . H35B H 0.9116 0.2412 0.2895 0.053 Uiso 1 1 calc R . . P1 P 0.73807(7) 0.64100(7) 0.17738(7) 0.03494(19) Uani 1 1 d . . . P2 P 0.23923(6) 0.70240(7) 0.26815(6) 0.02723(17) Uani 1 1 d . . . P3 P 0.35276(6) 0.17966(7) 0.33726(6) 0.02746(17) Uani 1 1 d . . . S1 S 0.76978(6) 0.37998(7) 0.10810(6) 0.03157(17) Uani 1 1 d . . . S2 S 0.51333(6) 0.56026(6) 0.11790(6) 0.03002(17) Uani 1 1 d . . . S3 S 0.42599(7) 0.40428(7) 0.39040(7) 0.0387(2) Uani 1 1 d D . . S4 S 0.64123(6) 0.18722(8) 0.35849(6) 0.03640(19) Uani 1 1 d D . . Cu1 Cu 0.67303(3) 0.53961(3) 0.14682(3) 0.03270(10) Uani 1 1 d . B . Cu2 Cu 0.38804(3) 0.55650(3) 0.26092(3) 0.02883(9) Uani 1 1 d . A . Cu3 Cu 0.45970(3) 0.25707(3) 0.34926(3) 0.02858(9) Uani 1 1 d . A . Ga1 Ga 0.79408(3) 0.20081(3) 0.22586(3) 0.02986(9) Uani 1 1 d . A . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0396(16) 0.0313(17) 0.0270(17) -0.0127(14) -0.0098(13) -0.0095(13) C2 0.0374(16) 0.0263(16) 0.0249(16) -0.0062(14) -0.0125(13) -0.0105(13) C5A 0.066(4) 0.131(7) 0.123(7) -0.087(6) 0.041(4) -0.059(4) C6A 0.040(3) 0.061(5) 0.089(6) -0.039(5) -0.002(4) -0.019(3) C7A 0.050(4) 0.064(5) 0.161(8) -0.043(5) -0.043(5) -0.004(3) C5B 0.057(6) 0.079(8) 0.069(8) -0.053(7) 0.005(5) -0.029(6) C6B 0.018(4) 0.021(6) 0.029(6) -0.010(5) 0.002(4) -0.011(4) C7B 0.051(6) 0.026(6) 0.061(7) 0.003(5) -0.035(6) -0.005(4) C8A 0.088(5) 0.049(4) 0.071(5) -0.006(3) -0.032(4) -0.039(3) C9A 0.055(3) 0.031(3) 0.041(3) -0.003(2) -0.016(3) -0.020(2) C10A 0.101(5) 0.062(4) 0.052(4) 0.008(3) -0.036(4) -0.053(4) C8B 0.113(10) 0.084(9) 0.104(10) -0.011(7) -0.046(8) -0.056(8) C9B 0.096(9) 0.089(9) 0.090(9) -0.013(7) -0.058(7) -0.043(7) C10B 0.140(12) 0.127(12) 0.114(12) -0.026(8) -0.049(9) -0.061(9) C11A 0.097(5) 0.075(5) 0.052(4) -0.018(4) -0.027(4) -0.045(4) C12A 0.054(4) 0.030(4) 0.027(3) -0.003(3) -0.013(3) -0.019(3) C13A 0.056(3) 0.043(3) 0.035(3) -0.020(3) 0.005(3) -0.018(3) C11B 0.049(6) 0.073(8) 0.071(9) -0.054(7) -0.010(6) -0.011(6) C12B 0.049(7) 0.051(10) 0.053(9) -0.027(7) -0.016(6) -0.012(6) C13B 0.076(8) 0.092(10) 0.094(10) -0.051(8) -0.016(7) -0.019(7) C14 0.068(3) 0.044(3) 0.081(4) -0.013(2) 0.010(2) -0.028(2) C15 0.0374(17) 0.0309(19) 0.062(3) -0.0169(18) -0.0182(17) -0.0054(14) C16 0.052(2) 0.035(2) 0.093(4) -0.027(2) -0.025(2) 0.0004(17) C17 0.0366(18) 0.056(3) 0.075(3) -0.030(2) -0.0310(19) 0.0034(17) C18 0.0351(17) 0.043(2) 0.0326(19) -0.0088(16) -0.0145(14) -0.0079(14) C19 0.047(2) 0.066(3) 0.056(3) -0.036(2) -0.0137(18) -0.0132(18) C20 0.053(2) 0.080(3) 0.043(2) -0.031(2) -0.0124(18) -0.019(2) C21 0.0353(17) 0.052(2) 0.036(2) -0.0228(18) -0.0067(14) -0.0078(15) C22 0.047(2) 0.075(3) 0.036(2) -0.017(2) 0.0008(17) -0.026(2) C23 0.043(2) 0.122(4) 0.061(3) -0.055(3) 0.0079(19) -0.034(2) C24 0.0315(17) 0.059(2) 0.057(2) -0.029(2) -0.0065(16) -0.0147(16) C25 0.043(2) 0.097(4) 0.069(3) -0.033(3) -0.007(2) -0.031(2) C26 0.083(3) 0.038(2) 0.091(4) -0.013(2) -0.043(3) -0.024(2) C27 0.0468(19) 0.0342(19) 0.046(2) -0.0052(17) -0.0173(17) -0.0185(15) C28 0.050(2) 0.035(2) 0.072(3) -0.013(2) -0.029(2) -0.0035(17) C29 0.055(2) 0.060(3) 0.034(2) -0.021(2) -0.0072(17) -0.0205(18) C30 0.0397(17) 0.0383(19) 0.041(2) -0.0093(17) -0.0186(15) -0.0119(14) C31 0.051(2) 0.042(2) 0.052(2) -0.0001(19) -0.0237(19) -0.0098(17) C32 0.065(3) 0.055(3) 0.051(3) -0.032(2) -0.010(2) -0.002(2) C33 0.0443(19) 0.0317(19) 0.048(2) -0.0182(18) -0.0136(16) -0.0019(15) C34 0.048(2) 0.070(3) 0.063(3) -0.013(2) -0.026(2) -0.012(2) C35 0.0334(17) 0.048(2) 0.051(2) -0.0103(19) -0.0155(16) -0.0129(15) P1 0.0431(5) 0.0359(5) 0.0366(5) -0.0146(4) -0.0091(4) -0.0193(4) P2 0.0231(3) 0.0268(4) 0.0313(4) -0.0115(4) -0.0085(3) -0.0027(3) P3 0.0282(4) 0.0284(4) 0.0304(4) -0.0090(4) -0.0101(3) -0.0108(3) S1 0.0289(4) 0.0338(4) 0.0326(4) -0.0123(4) -0.0029(3) -0.0121(3) S2 0.0350(4) 0.0269(4) 0.0274(4) -0.0091(3) -0.0087(3) -0.0068(3) S3 0.0501(5) 0.0270(4) 0.0419(5) -0.0092(4) -0.0233(4) -0.0051(4) S4 0.0284(4) 0.0508(5) 0.0315(5) -0.0129(4) -0.0068(3) -0.0140(3) Cu1 0.0435(2) 0.0363(2) 0.0275(2) -0.01198(18) -0.00440(16) -0.02248(17) Cu2 0.02553(17) 0.0276(2) 0.0349(2) -0.01338(18) -0.00871(15) -0.00435(15) Cu3 0.03064(18) 0.0307(2) 0.0285(2) -0.00681(17) -0.00995(15) -0.01363(15) Ga1 0.02453(16) 0.03147(19) 0.0331(2) -0.01279(17) -0.00709(14) -0.00500(13) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.527(4) . ? C1 S1 1.846(3) . ? C2 S2 1.838(3) . ? C3A C4A 1.511(6) . ? C3A S3 1.905(4) . ? C4A S4 1.798(4) . ? C3B C4B 1.525(16) . ? C3B S3 1.744(13) . ? C4B S4 2.058(12) . ? C5A C6A 1.534(9) . ? C6A C7A 1.540(9) . ? C6A P1 1.788(8) . ? C5B C6B 1.534(11) . ? C6B C7B 1.549(12) . ? C6B P1 1.985(12) . ? C8A C9A 1.552(7) . ? C9A C10A 1.538(7) . ? C9A P1 1.914(6) . ? C8B C9B 1.551(13) . ? C9B C10B 1.552(14) . ? C9B P1 1.763(17) . ? C11A C12A 1.533(8) . ? C12A C13A 1.552(8) . ? C12A P1 1.906(8) . ? C11B C12B 1.550(13) . ? C12B C13B 1.556(13) . ? C12B P1 1.74(2) . ? C14 C15 1.540(6) . ? C15 C16 1.539(5) . ? C15 P2 1.869(4) . ? C17 C18 1.540(5) . ? C18 C19 1.535(5) . ? C18 P2 1.876(3) . ? C20 C21 1.544(5) . ? C21 C22 1.528(6) . ? C21 P2 1.866(3) . ? C23 C24 1.560(6) . ? C24 C25 1.537(5) . ? C24 P3 1.863(3) . ? C26 C27 1.549(5) . ? C27 C28 1.536(5) . ? C27 P3 1.865(4) . ? C29 C30 1.557(5) . ? C30 C31 1.529(5) . ? C30 P3 1.864(3) . ? C32 C33 1.536(5) . ? C33 Ga1 2.003(3) . ? C34 C35 1.548(6) . ? C35 Ga1 2.003(3) . ? P1 Cu1 2.2176(9) . ? P2 Cu2 2.2474(8) . ? P3 Cu3 2.2179(8) . ? S1 Cu1 2.3224(9) . ? S1 Ga1 2.3722(10) . ? S2 Cu1 2.2624(8) . ? S2 Cu2 2.2973(9) . ? S3 Cu3 2.2563(9) . ? S3 Cu2 2.2753(10) . ? S4 Cu3 2.3012(8) . ? S4 Ga1 2.3665(9) . ? 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 C2 C1 S1 113.0(2) . . ? C1 C2 S2 112.6(2) . . ? C4A C3A S3 112.6(3) . . ? C3A C4A S4 111.7(3) . . ? C4B C3B S3 99.9(10) . . ? C3B C4B S4 118.6(11) . . ? C5A C6A C7A 111.9(7) . . ? C5A C6A P1 109.8(6) . . ? C7A C6A P1 107.0(6) . . ? C5B C6B C7B 107.8(11) . . ? C5B C6B P1 112.3(8) . . ? C7B C6B P1 112.3(8) . . ? C10A C9A C8A 110.8(5) . . ? C10A C9A P1 110.5(4) . . ? C8A C9A P1 115.5(4) . . ? C8B C9B C10B 109.0(15) . . ? C8B C9B P1 124.0(12) . . ? C10B C9B P1 111.1(14) . . ? C11A C12A C13A 111.7(6) . . ? C11A C12A P1 115.8(5) . . ? C13A C12A P1 111.5(5) . . ? C11B C12B C13B 108.3(13) . . ? C11B C12B P1 121.0(13) . . ? C13B C12B P1 104.8(12) . . ? C16 C15 C14 110.6(4) . . ? C16 C15 P2 116.7(3) . . ? C14 C15 P2 111.3(3) . . ? C19 C18 C17 110.3(3) . . ? C19 C18 P2 110.3(2) . . ? C17 C18 P2 116.9(2) . . ? C22 C21 C20 110.6(3) . . ? C22 C21 P2 109.9(2) . . ? C20 C21 P2 109.4(2) . . ? C25 C24 C23 110.5(3) . . ? C25 C24 P3 117.4(3) . . ? C23 C24 P3 109.5(2) . . ? C28 C27 C26 109.6(3) . . ? C28 C27 P3 112.4(3) . . ? C26 C27 P3 115.0(3) . . ? C31 C30 C29 111.0(3) . . ? C31 C30 P3 110.6(3) . . ? C29 C30 P3 109.6(2) . . ? C32 C33 Ga1 113.5(3) . . ? C34 C35 Ga1 112.3(2) . . ? C12B P1 C9B 110.9(9) . . ? C12B P1 C6A 113.4(6) . . ? C9B P1 C6A 83.0(7) . . ? C12B P1 C12A 14.1(6) . . ? C9B P1 C12A 124.2(7) . . ? C6A P1 C12A 108.1(4) . . ? C12B P1 C9A 89.0(6) . . ? C9B P1 C9A 26.6(7) . . ? C6A P1 C9A 105.8(3) . . ? C12A P1 C9A 103.0(3) . . ? C12B P1 C6B 98.9(6) . . ? C9B P1 C6B 101.3(7) . . ? C6A P1 C6B 20.0(3) . . ? C12A P1 C6B 90.9(4) . . ? C9A P1 C6B 121.0(4) . . ? C12B P1 Cu1 116.7(6) . . ? C9B P1 Cu1 112.8(4) . . ? C6A P1 Cu1 115.2(3) . . ? C12A P1 Cu1 110.6(2) . . ? C9A P1 Cu1 113.17(17) . . ? C6B P1 Cu1 114.3(3) . . ? C21 P2 C15 104.96(17) . . ? C21 P2 C18 106.26(15) . . ? C15 P2 C18 104.21(16) . . ? C21 P2 Cu2 115.44(12) . . ? C15 P2 Cu2 111.58(11) . . ? C18 P2 Cu2 113.43(11) . . ? C24 P3 C30 105.52(16) . . ? C24 P3 C27 105.32(18) . . ? C30 P3 C27 105.85(16) . . ? C24 P3 Cu3 109.27(11) . . ? C30 P3 Cu3 114.12(11) . . ? C27 P3 Cu3 115.93(11) . . ? C1 S1 Cu1 96.35(10) . . ? C1 S1 Ga1 102.31(11) . . ? Cu1 S1 Ga1 122.13(4) . . ? C2 S2 Cu1 97.57(9) . . ? C2 S2 Cu2 105.27(11) . . ? Cu1 S2 Cu2 103.63(3) . . ? C3B S3 C3A 31.4(6) . . ? C3B S3 Cu3 107.0(6) . . ? C3A S3 Cu3 96.55(12) . . ? C3B S3 Cu2 123.3(7) . . ? C3A S3 Cu2 100.53(13) . . ? Cu3 S3 Cu2 105.92(4) . . ? C4A S4 C4B 22.6(4) . . ? C4A S4 Cu3 99.11(12) . . ? C4B S4 Cu3 89.3(4) . . ? C4A S4 Ga1 104.87(14) . . ? C4B S4 Ga1 94.4(4) . . ? Cu3 S4 Ga1 124.84(4) . . ? P1 Cu1 S2 135.72(4) . . ? P1 Cu1 S1 127.93(3) . . ? S2 Cu1 S1 95.66(3) . . ? P2 Cu2 S3 123.32(4) . . ? P2 Cu2 S2 119.55(3) . . ? S3 Cu2 S2 117.10(3) . . ? P3 Cu3 S3 133.69(3) . . ? P3 Cu3 S4 129.89(3) . . ? S3 Cu3 S4 95.04(3) . . ? C35 Ga1 C33 119.83(15) . . ? C35 Ga1 S4 105.45(12) . . ? C33 Ga1 S4 104.30(11) . . ? C35 Ga1 S1 107.06(11) . . ? C33 Ga1 S1 107.58(11) . . ? S4 Ga1 S1 112.76(3) . . ? _chemical_name_common ; bis(mu!3$-1,2-dithiolatoethane-S,S,S',S')-diethanido - tris(triisopropylphosphine)-tricopper(+1)-gallium(+3) ; data_[(iPr3PCu)3(SC2H4S)2GaiPr2] _database_code_depnum_ccdc_archive 'CCDC 907025' #TrackingRef '17785_web_deposit_cif_file_0_DirkFriedrich_1360942523.27_[(iPr3PCu)3(SC2H4S)2GaiPr2].cif' _audit_creation_date 2012-10-11T14:08:52-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; bis(\m~3~-1,2-dithiolatoethane-S,S,S',S')-di(propan-2-ido) -tris(triisopropylphosphine)-tricopper(+1)-gallium(+3) ; _chemical_formula_moiety 'C37 H85 Cu3 Ga1 P3 S4' _chemical_formula_sum 'C37 H85 Cu3 Ga P3 S4' _chemical_formula_weight 1011.54 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.6195(14) _cell_length_b 14.4070(15) _cell_length_c 16.1191(16) _cell_angle_alpha 63.741(7) _cell_angle_beta 68.366(8) _cell_angle_gamma 68.500(8) _cell_volume 2557.0(5) _cell_formula_units_Z 2 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 14475 _cell_measurement_theta_min 2.01 _cell_measurement_theta_max 29.29 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description platelet _exptl_crystal_colour colorless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.175 _exptl_crystal_size_min 0.054 _exptl_crystal_density_diffrn 1.314 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1068 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 2.03 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details ; Busing, W. R. & Levy, H. A. (1957) Acta Cryst. 10, 180-182. and Coppens, P., Leiserowitz, L. & Rabinovich, D. (1965) Acta Cryst. 1965, 1035-1038. ; _exptl_absorpt_correction_T_min 0.6684 _exptl_absorpt_correction_T_max 0.8911 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 180(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 '2-circle goniometer' _diffrn_measurement_device_type 'STOE IPDS-2T' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 6.67 _diffrn_detector 'image plate (34 cm diameter / schwenk)' _diffrn_detector_type STOE _diffrn_standards_number 0 _diffrn_reflns_av_R_equivalents 0.0576 _diffrn_reflns_av_unetI/netI 0.0948 _diffrn_reflns_number 24930 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.02 _diffrn_reflns_theta_max 27.5 _diffrn_reflns_theta_full 27.5 _diffrn_measured_fraction_theta_full 0.994 _diffrn_measured_fraction_theta_max 0.994 _reflns_number_total 11667 _reflns_number_gt 7231 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_cell_refinement 'STOE X-AREA' _computing_data_reduction 'STOE X-AREA, STOE X-RED' _computing_structure_solution ; 'SIR-92' Altomare, A., Cascarano, G., Giacovazzo, C. & Guagliardi, A. (1993) J. Appl. Cryst. 26, 343-350. ; _computing_structure_refinement ; 'SHELXL-97' Sheldrick, G.M. (2008) Acta Cryst. A64, 112 ; _computing_molecular_graphics 'DIAMOND 3.2' _computing_publication_material ; 'WinGX publication routines' Farrugia, L. J. (1999) WinGX, J. Appl. Cryst. 32, 837-838 ; #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0145P)^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_number_reflns 11667 _refine_ls_number_parameters 455 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0791 _refine_ls_R_factor_gt 0.0363 _refine_ls_wR_factor_ref 0.059 _refine_ls_wR_factor_gt 0.0529 _refine_ls_goodness_of_fit_ref 0.825 _refine_ls_restrained_S_all 0.825 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.715 _refine_diff_density_min -0.402 _refine_diff_density_rms 0.075 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.6648(3) 0.3932(2) 0.0571(2) 0.0272(7) Uani 1 1 d . . . H1A H 0.6753 0.4449 -0.0093 0.033 Uiso 1 1 calc R . . H1B H 0.677 0.3223 0.0546 0.033 Uiso 1 1 calc R . . C2 C 0.5478(2) 0.4261(2) 0.1122(2) 0.0252(7) Uani 1 1 d . . . H2A H 0.5362 0.3731 0.1779 0.03 Uiso 1 1 calc R . . H2B H 0.4972 0.4263 0.081 0.03 Uiso 1 1 calc R . . C3 C 0.5698(3) 0.3916(2) 0.3814(2) 0.0303(7) Uani 1 1 d . . . H3A H 0.6064 0.4247 0.3137 0.036 Uiso 1 1 calc R . . H3B H 0.5712 0.4317 0.4174 0.036 Uiso 1 1 calc R . . C4 C 0.6334(3) 0.2766(2) 0.4197(2) 0.0311(7) Uani 1 1 d . . . H4A H 0.6017 0.246 0.4892 0.037 Uiso 1 1 calc R . . H4B H 0.7096 0.2758 0.4106 0.037 Uiso 1 1 calc R . . C32 C 0.7880(4) 0.0020(3) 0.2398(3) 0.0565(11) Uani 1 1 d . . . H32A H 0.783 -0.0421 0.2101 0.085 Uiso 1 1 calc R . . H32B H 0.7267 0.0028 0.2958 0.085 Uiso 1 1 calc R . . H32C H 0.8566 -0.0277 0.2594 0.085 Uiso 1 1 calc R . . C33 C 0.7845(3) 0.1155(3) 0.1682(2) 0.0371(8) Uani 1 1 d . . . H33 H 0.7143 0.1431 0.149 0.045 Uiso 1 1 calc R . . C34 C 0.8781(4) 0.1160(3) 0.0771(3) 0.0540(11) Uani 1 1 d . . . H34A H 0.9483 0.0892 0.0936 0.081 Uiso 1 1 calc R . . H34B H 0.8725 0.1891 0.0305 0.081 Uiso 1 1 calc R . . H34C H 0.8728 0.0702 0.0494 0.081 Uiso 1 1 calc R . . C35 C 0.9291(3) 0.0807(3) 0.3599(3) 0.0482(9) Uani 1 1 d . . . H35A H 0.9403 0.0235 0.3376 0.072 Uiso 1 1 calc R . . H35B H 0.8651 0.0793 0.4142 0.072 Uiso 1 1 calc R . . H35C H 0.9934 0.0701 0.3798 0.072 Uiso 1 1 calc R . . C36 C 0.9108(3) 0.1896(3) 0.2782(2) 0.0316(7) Uani 1 1 d . . . H36 H 0.8919 0.2465 0.3049 0.038 Uiso 1 1 calc R . . C37 C 1.0157(3) 0.2011(3) 0.1978(3) 0.0473(9) Uani 1 1 d . . . H37A H 1.0765 0.1838 0.225 0.071 Uiso 1 1 calc R . . H37B H 1.0061 0.2747 0.1522 0.071 Uiso 1 1 calc R . . H37C H 1.0313 0.1522 0.1648 0.071 Uiso 1 1 calc R . . C7 C 0.9049(3) 0.4804(3) 0.2667(3) 0.0558(11) Uani 1 1 d . . . H7A H 0.8799 0.4266 0.2634 0.084 Uiso 1 1 calc R . . H7B H 0.8641 0.4937 0.3263 0.084 Uiso 1 1 calc R . . H7C H 0.9827 0.4543 0.2647 0.084 Uiso 1 1 calc R . . C6 C 0.8858(3) 0.5851(3) 0.1809(2) 0.0345(8) Uani 1 1 d . . . H6 H 0.9105 0.6398 0.1854 0.041 Uiso 1 1 calc R . . C5 C 0.9529(3) 0.5655(4) 0.0868(3) 0.0594(12) Uani 1 1 d . . . H5A H 1.0305 0.5414 0.0856 0.089 Uiso 1 1 calc R . . H5B H 0.9401 0.6319 0.0326 0.089 Uiso 1 1 calc R . . H5C H 0.9306 0.5107 0.0825 0.089 Uiso 1 1 calc R . . C8 C 0.8080(4) 0.8345(3) 0.0762(3) 0.0614(12) Uani 1 1 d . . . H8A H 0.8781 0.8016 0.0413 0.092 Uiso 1 1 calc R . . H8B H 0.8155 0.8289 0.1365 0.092 Uiso 1 1 calc R . . H8C H 0.7854 0.9099 0.0375 0.092 Uiso 1 1 calc R . . C9 C 0.7214(3) 0.7763(3) 0.0970(2) 0.0416(9) Uani 1 1 d . . . H9 H 0.6508 0.8172 0.127 0.05 Uiso 1 1 calc R . . C10 C 0.7074(4) 0.7855(4) 0.0041(3) 0.0664(13) Uani 1 1 d . . . H10A H 0.6871 0.861 -0.0353 0.1 Uiso 1 1 calc R . . H10B H 0.6501 0.7512 0.0181 0.1 Uiso 1 1 calc R . . H10C H 0.7761 0.7503 -0.0305 0.1 Uiso 1 1 calc R . . C13 C 0.5471(3) 0.6847(3) 0.3188(3) 0.0492(10) Uani 1 1 d . . . H13A H 0.513 0.6763 0.3861 0.074 Uiso 1 1 calc R . . H13B H 0.5215 0.6421 0.3014 0.074 Uiso 1 1 calc R . . H13C H 0.5273 0.7601 0.2789 0.074 Uiso 1 1 calc R . . C12 C 0.6714(3) 0.6467(3) 0.3033(2) 0.0326(8) Uani 1 1 d . . . H12 H 0.6862 0.5724 0.3506 0.039 Uiso 1 1 calc R . . C11 C 0.7147(3) 0.7126(3) 0.3291(3) 0.0548(11) Uani 1 1 d . . . H11A H 0.6993 0.7874 0.2866 0.082 Uiso 1 1 calc R . . H11B H 0.7936 0.6847 0.3217 0.082 Uiso 1 1 calc R . . H11C H 0.679 0.7079 0.3954 0.082 Uiso 1 1 calc R . . C14 C 0.3707(4) 0.8392(3) 0.1185(3) 0.0636(13) Uani 1 1 d . . . H14A H 0.3325 0.8532 0.0716 0.095 Uiso 1 1 calc R . . H14B H 0.4302 0.7748 0.1208 0.095 Uiso 1 1 calc R . . H14C H 0.4004 0.9001 0.0999 0.095 Uiso 1 1 calc R . . C15 C 0.2903(3) 0.8229(3) 0.2177(3) 0.0389(8) Uani 1 1 d . . . H15 H 0.3324 0.8138 0.2613 0.047 Uiso 1 1 calc R . . C16 C 0.1979(3) 0.9239(3) 0.2179(3) 0.0553(11) Uani 1 1 d . . . H16A H 0.2288 0.9843 0.198 0.083 Uiso 1 1 calc R . . H16B H 0.1499 0.9127 0.2823 0.083 Uiso 1 1 calc R . . H16C H 0.1559 0.9391 0.1734 0.083 Uiso 1 1 calc R . . C17 C 0.0403(3) 0.7791(3) 0.2154(3) 0.0568(11) Uani 1 1 d . . . H17A H 0.0046 0.794 0.1665 0.085 Uiso 1 1 calc R . . H17B H 0.0378 0.8464 0.2184 0.085 Uiso 1 1 calc R . . H17C H 0.0024 0.7358 0.2776 0.085 Uiso 1 1 calc R . . C18 C 0.1594(3) 0.7180(3) 0.1901(2) 0.0358(8) Uani 1 1 d . . . H18 H 0.1917 0.763 0.1241 0.043 Uiso 1 1 calc R . . C19 C 0.1652(3) 0.6143(3) 0.1827(3) 0.0462(9) Uani 1 1 d . . . H19A H 0.1287 0.569 0.2444 0.069 Uiso 1 1 calc R . . H19B H 0.2416 0.5769 0.1651 0.069 Uiso 1 1 calc R . . H19C H 0.129 0.6301 0.1338 0.069 Uiso 1 1 calc R . . C22 C 0.1176(3) 0.5840(3) 0.4344(3) 0.0511(10) Uani 1 1 d . . . H22A H 0.1801 0.5219 0.4369 0.077 Uiso 1 1 calc R . . H22B H 0.0731 0.5862 0.3974 0.077 Uiso 1 1 calc R . . H22C H 0.0736 0.5784 0.4994 0.077 Uiso 1 1 calc R . . C21 C 0.1586(3) 0.6871(3) 0.3863(2) 0.0362(8) Uani 1 1 d . . . H21 H 0.0946 0.7502 0.3801 0.043 Uiso 1 1 calc R . . C20 C 0.2213(3) 0.6884(3) 0.4474(3) 0.0525(10) Uani 1 1 d . . . H20A H 0.1756 0.6786 0.5125 0.079 Uiso 1 1 calc R . . H20B H 0.2408 0.757 0.4198 0.079 Uiso 1 1 calc R . . H20C H 0.2878 0.6305 0.449 0.079 Uiso 1 1 calc R . . C31 C 0.2830(3) 0.3449(3) 0.1742(2) 0.0408(8) Uani 1 1 d . . . H31A H 0.3219 0.3859 0.1805 0.061 Uiso 1 1 calc R . . H31B H 0.206 0.3619 0.2074 0.061 Uiso 1 1 calc R . . H31C H 0.2892 0.3636 0.1064 0.061 Uiso 1 1 calc R . . C30 C 0.3332(3) 0.2245(2) 0.2184(2) 0.0306(7) Uani 1 1 d . . . H30 H 0.2858 0.1838 0.221 0.037 Uiso 1 1 calc R . . C29 C 0.4490(3) 0.1915(3) 0.1571(2) 0.0380(8) Uani 1 1 d . . . H29A H 0.448 0.2232 0.0895 0.057 Uiso 1 1 calc R . . H29B H 0.4718 0.1136 0.1764 0.057 Uiso 1 1 calc R . . H29C H 0.5002 0.217 0.1665 0.057 Uiso 1 1 calc R . . C25 C 0.1066(3) 0.2047(3) 0.4078(3) 0.0531(10) Uani 1 1 d . . . H25A H 0.1153 0.1282 0.445 0.08 Uiso 1 1 calc R . . H25B H 0.1079 0.2182 0.3423 0.08 Uiso 1 1 calc R . . H25C H 0.037 0.2444 0.437 0.08 Uiso 1 1 calc R . . C24 C 0.2002(3) 0.2411(3) 0.4065(2) 0.0350(8) Uani 1 1 d . . . H24 H 0.1831 0.3204 0.3742 0.042 Uiso 1 1 calc R . . C23 C 0.1995(3) 0.2189(4) 0.5100(3) 0.0638(13) Uani 1 1 d . . . H23A H 0.1286 0.2552 0.541 0.096 Uiso 1 1 calc R . . H23B H 0.2569 0.2457 0.5086 0.096 Uiso 1 1 calc R . . H23C H 0.2126 0.1419 0.5459 0.096 Uiso 1 1 calc R . . C26 C 0.3162(3) -0.0109(3) 0.3607(3) 0.0512(10) Uani 1 1 d . . . H26A H 0.3528 -0.002 0.2937 0.077 Uiso 1 1 calc R . . H26B H 0.2385 0.024 0.3667 0.077 Uiso 1 1 calc R . . H26C H 0.3252 -0.0871 0.3992 0.077 Uiso 1 1 calc R . . C27 C 0.3671(3) 0.0402(2) 0.3964(2) 0.0335(8) Uani 1 1 d . . . H27 H 0.3325 0.0228 0.4663 0.04 Uiso 1 1 calc R . . C28 C 0.4895(3) -0.0126(3) 0.3867(3) 0.0440(9) Uani 1 1 d . . . H28A H 0.4999 -0.0891 0.4243 0.066 Uiso 1 1 calc R . . H28B H 0.5204 0.02 0.4101 0.066 Uiso 1 1 calc R . . H28C H 0.5263 -0.0024 0.3194 0.066 Uiso 1 1 calc R . . P1 P 0.73885(7) 0.63568(6) 0.18289(5) 0.02415(17) Uani 1 1 d . . . P2 P 0.24911(6) 0.69491(6) 0.26503(6) 0.02647(17) Uani 1 1 d . . . P3 P 0.34126(7) 0.18955(6) 0.34159(5) 0.02551(17) Uani 1 1 d . . . S1 S 0.76672(6) 0.38695(6) 0.11044(5) 0.02603(17) Uani 1 1 d . . . S2 S 0.51669(6) 0.55966(6) 0.11750(5) 0.02564(16) Uani 1 1 d . . . S3 S 0.42637(7) 0.40449(6) 0.39016(5) 0.02900(18) Uani 1 1 d . . . S4 S 0.63292(6) 0.19267(6) 0.36186(5) 0.02718(17) Uani 1 1 d . . . Cu1 Cu 0.67325(3) 0.53782(3) 0.15128(3) 0.02560(9) Uani 1 1 d . . . Cu2 Cu 0.39204(3) 0.55434(3) 0.26072(3) 0.02656(9) Uani 1 1 d . . . Cu3 Cu 0.45447(3) 0.26198(3) 0.35068(3) 0.02652(9) Uani 1 1 d . . . Ga1 Ga 0.78571(3) 0.21271(3) 0.22745(2) 0.02483(8) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0390(19) 0.0217(15) 0.0238(15) -0.0086(12) -0.0098(14) -0.0079(14) C2 0.0369(18) 0.0191(14) 0.0239(15) -0.0024(12) -0.0123(13) -0.0131(13) C3 0.0343(19) 0.0338(17) 0.0302(16) -0.0119(14) -0.0079(14) -0.0156(15) C4 0.0302(18) 0.0381(18) 0.0297(16) -0.0125(15) -0.0097(14) -0.0105(15) C32 0.076(3) 0.033(2) 0.062(2) -0.0242(19) -0.004(2) -0.018(2) C33 0.043(2) 0.0305(17) 0.045(2) -0.0186(16) -0.0135(17) -0.0075(16) C34 0.077(3) 0.046(2) 0.042(2) -0.0282(19) -0.005(2) -0.011(2) C35 0.038(2) 0.048(2) 0.049(2) -0.0010(18) -0.0235(18) -0.0075(18) C36 0.0276(18) 0.0307(17) 0.0372(18) -0.0125(15) -0.0115(15) -0.0041(14) C37 0.030(2) 0.060(2) 0.045(2) -0.0135(19) -0.0102(17) -0.0093(18) C7 0.046(2) 0.046(2) 0.076(3) -0.017(2) -0.032(2) -0.002(2) C6 0.0290(18) 0.0372(18) 0.0409(19) -0.0181(16) -0.0048(15) -0.0106(15) C5 0.036(2) 0.085(3) 0.069(3) -0.052(3) 0.010(2) -0.019(2) C8 0.103(4) 0.046(2) 0.052(2) 0.0025(19) -0.033(2) -0.047(2) C9 0.060(2) 0.0333(18) 0.0391(19) -0.0040(16) -0.0218(18) -0.0217(18) C10 0.101(4) 0.069(3) 0.044(2) 0.008(2) -0.039(2) -0.051(3) C13 0.039(2) 0.061(2) 0.058(2) -0.039(2) 0.0030(19) -0.0159(19) C12 0.0352(19) 0.0396(18) 0.0282(16) -0.0158(15) -0.0009(14) -0.0170(16) C11 0.065(3) 0.083(3) 0.045(2) -0.041(2) 0.0030(19) -0.042(2) C14 0.066(3) 0.039(2) 0.064(3) -0.013(2) 0.008(2) -0.020(2) C15 0.0348(19) 0.0283(17) 0.051(2) -0.0134(16) -0.0119(17) -0.0042(15) C16 0.052(3) 0.035(2) 0.084(3) -0.029(2) -0.024(2) 0.0007(19) C17 0.035(2) 0.065(3) 0.087(3) -0.044(3) -0.034(2) 0.010(2) C18 0.0305(18) 0.045(2) 0.0341(18) -0.0174(16) -0.0113(15) -0.0035(16) C19 0.042(2) 0.059(2) 0.052(2) -0.034(2) -0.0121(18) -0.0094(19) C22 0.046(2) 0.064(3) 0.040(2) -0.021(2) 0.0027(18) -0.022(2) C21 0.0275(18) 0.049(2) 0.0362(18) -0.0244(17) -0.0048(15) -0.0059(16) C20 0.050(2) 0.078(3) 0.039(2) -0.029(2) -0.0090(18) -0.018(2) C31 0.047(2) 0.0373(19) 0.0346(18) -0.0026(16) -0.0177(17) -0.0113(17) C30 0.0399(19) 0.0309(17) 0.0289(16) -0.0073(14) -0.0145(15) -0.0153(15) C29 0.048(2) 0.043(2) 0.0261(16) -0.0131(15) -0.0094(16) -0.0135(17) C25 0.038(2) 0.074(3) 0.054(2) -0.030(2) -0.0037(19) -0.019(2) C24 0.0313(19) 0.047(2) 0.0338(17) -0.0168(16) -0.0070(15) -0.0149(16) C23 0.045(2) 0.116(4) 0.043(2) -0.043(3) -0.0009(19) -0.026(3) C26 0.070(3) 0.0287(19) 0.064(2) -0.0020(18) -0.034(2) -0.0222(19) C27 0.039(2) 0.0293(17) 0.0317(17) -0.0008(14) -0.0145(15) -0.0146(15) C28 0.048(2) 0.0289(18) 0.051(2) -0.0029(17) -0.0251(19) -0.0067(17) P1 0.0282(4) 0.0262(4) 0.0222(4) -0.0102(3) -0.0042(3) -0.0111(3) P2 0.0226(4) 0.0277(4) 0.0282(4) -0.0126(3) -0.0056(3) -0.0025(3) P3 0.0287(4) 0.0274(4) 0.0238(4) -0.0067(3) -0.0085(3) -0.0114(4) S1 0.0266(4) 0.0215(4) 0.0281(4) -0.0079(3) -0.0052(3) -0.0065(3) S2 0.0261(4) 0.0229(4) 0.0256(4) -0.0071(3) -0.0063(3) -0.0056(3) S3 0.0313(4) 0.0250(4) 0.0279(4) -0.0073(3) -0.0080(3) -0.0058(3) S4 0.0268(4) 0.0289(4) 0.0255(4) -0.0087(3) -0.0057(3) -0.0084(3) Cu1 0.0323(2) 0.02545(19) 0.02404(19) -0.00900(16) -0.00607(16) -0.01303(17) Cu2 0.0257(2) 0.02463(19) 0.0293(2) -0.01004(17) -0.00883(17) -0.00346(16) Cu3 0.0300(2) 0.0295(2) 0.02376(19) -0.00636(16) -0.00843(16) -0.01327(17) Ga1 0.02524(18) 0.02103(17) 0.02706(17) -0.00906(14) -0.00636(14) -0.00388(14) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.526(4) . ? C1 S1 1.841(3) . ? C2 S2 1.846(3) . ? C3 C4 1.521(4) . ? C3 S3 1.850(3) . ? C4 S4 1.828(3) . ? C32 C33 1.524(5) . ? C33 C34 1.549(5) . ? C33 Ga1 2.021(3) . ? C35 C36 1.544(5) . ? C36 C37 1.538(4) . ? C36 Ga1 2.013(3) . ? C7 C6 1.546(5) . ? C6 C5 1.544(4) . ? C6 P1 1.855(3) . ? C8 C9 1.547(5) . ? C9 C10 1.521(5) . ? C9 P1 1.867(3) . ? C13 C12 1.536(5) . ? C12 C11 1.537(4) . ? C12 P1 1.868(3) . ? C14 C15 1.542(5) . ? C15 C16 1.537(5) . ? C15 P2 1.869(3) . ? C17 C18 1.535(5) . ? C18 C19 1.522(5) . ? C18 P2 1.871(3) . ? C22 C21 1.545(5) . ? C21 C20 1.534(5) . ? C21 P2 1.867(3) . ? C31 C30 1.543(4) . ? C30 C29 1.552(4) . ? C30 P3 1.855(3) . ? C25 C24 1.536(5) . ? C24 C23 1.551(5) . ? C24 P3 1.869(3) . ? C26 C27 1.548(5) . ? C27 C28 1.539(5) . ? C27 P3 1.878(3) . ? P1 Cu1 2.2226(9) . ? P2 Cu2 2.2429(9) . ? P3 Cu3 2.2292(9) . ? S1 Cu1 2.3235(8) . ? S1 Ga1 2.3707(8) . ? S2 Cu1 2.2705(9) . ? S2 Cu2 2.2949(8) . ? S3 Cu3 2.2732(9) . ? S3 Cu2 2.2862(9) . ? S4 Cu3 2.3067(9) . ? S4 Ga1 2.3812(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 C2 C1 S1 113.1(2) . . ? C1 C2 S2 111.92(19) . . ? C4 C3 S3 113.4(2) . . ? C3 C4 S4 113.2(2) . . ? C32 C33 C34 110.5(3) . . ? C32 C33 Ga1 111.4(2) . . ? C34 C33 Ga1 112.2(2) . . ? C37 C36 C35 110.9(3) . . ? C37 C36 Ga1 111.1(2) . . ? C35 C36 Ga1 111.8(2) . . ? C5 C6 C7 109.7(3) . . ? C5 C6 P1 110.3(3) . . ? C7 C6 P1 110.2(2) . . ? C10 C9 C8 110.2(3) . . ? C10 C9 P1 111.5(2) . . ? C8 C9 P1 116.8(3) . . ? C13 C12 C11 111.0(3) . . ? C13 C12 P1 111.2(2) . . ? C11 C12 P1 115.9(2) . . ? C16 C15 C14 111.0(3) . . ? C16 C15 P2 116.6(2) . . ? C14 C15 P2 111.0(2) . . ? C19 C18 C17 110.3(3) . . ? C19 C18 P2 111.2(2) . . ? C17 C18 P2 117.3(2) . . ? C20 C21 C22 110.0(3) . . ? C20 C21 P2 109.6(2) . . ? C22 C21 P2 110.0(2) . . ? C31 C30 C29 110.8(3) . . ? C31 C30 P3 110.8(2) . . ? C29 C30 P3 109.2(2) . . ? C25 C24 C23 109.8(3) . . ? C25 C24 P3 118.3(2) . . ? C23 C24 P3 109.4(3) . . ? C28 C27 C26 110.4(3) . . ? C28 C27 P3 111.2(2) . . ? C26 C27 P3 115.3(2) . . ? C6 P1 C9 106.06(16) . . ? C6 P1 C12 104.02(15) . . ? C9 P1 C12 104.98(16) . . ? C6 P1 Cu1 114.69(10) . . ? C9 P1 Cu1 112.26(11) . . ? C12 P1 Cu1 113.92(10) . . ? C21 P2 C15 104.34(15) . . ? C21 P2 C18 106.22(15) . . ? C15 P2 C18 105.15(16) . . ? C21 P2 Cu2 115.26(12) . . ? C15 P2 Cu2 112.79(11) . . ? C18 P2 Cu2 112.23(10) . . ? C30 P3 C24 105.57(15) . . ? C30 P3 C27 105.53(14) . . ? C24 P3 C27 105.41(15) . . ? C30 P3 Cu3 114.43(10) . . ? C24 P3 Cu3 108.57(10) . . ? C27 P3 Cu3 116.46(11) . . ? C1 S1 Cu1 96.50(9) . . ? C1 S1 Ga1 102.41(10) . . ? Cu1 S1 Ga1 121.85(3) . . ? C2 S2 Cu1 97.16(10) . . ? C2 S2 Cu2 105.50(9) . . ? Cu1 S2 Cu2 101.83(3) . . ? C3 S3 Cu3 97.88(10) . . ? C3 S3 Cu2 102.06(10) . . ? Cu3 S3 Cu2 107.08(4) . . ? C4 S4 Cu3 97.77(11) . . ? C4 S4 Ga1 104.17(10) . . ? Cu3 S4 Ga1 123.75(4) . . ? P1 Cu1 S2 135.29(3) . . ? P1 Cu1 S1 128.21(3) . . ? S2 Cu1 S1 95.44(3) . . ? P2 Cu2 S3 124.88(3) . . ? P2 Cu2 S2 118.68(3) . . ? S3 Cu2 S2 116.43(3) . . ? P3 Cu3 S3 132.56(3) . . ? P3 Cu3 S4 130.64(3) . . ? S3 Cu3 S4 95.14(3) . . ? C36 Ga1 C33 122.48(14) . . ? C36 Ga1 S1 105.76(9) . . ? C33 Ga1 S1 106.76(10) . . ? C36 Ga1 S4 105.66(9) . . ? C33 Ga1 S4 102.75(10) . . ? S1 Ga1 S4 113.74(3) . . ? _chemical_name_common ; bis(mu!3$-1,2-dithiolatoethane-S,S,S',S')-di(propan-2-ido) - tris(triisopropylphosphine)-tricopper(+1)-gallium(+3) ; data_[(iPr3PCu)3(SC2H4S)2GaBu2] _database_code_depnum_ccdc_archive 'CCDC 907026' #TrackingRef '17885_web_deposit_cif_file_0_DirkFriedrich_1361281188.28_[(iPr3PCu)3(SC2H4S)2GanBu2].cif' _audit_creation_date 2012-10-11T14:38:53-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; bis(\m~3~-1,2-dithiolatoethane-S,S,S',S')-di(butan-1-ido) -tris(triisopropylphosphine)-tricopper(+1)-gallium(+3) ; _chemical_formula_moiety 'C39 H89 Cu3 Ga1 P3 S4' _chemical_formula_sum 'C39 H89 Cu3 Ga P3 S4' _chemical_formula_weight 1039.59 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P b c a' _symmetry_space_group_name_Hall '-P 2ac 2ab' _symmetry_Int_Tables_number 61 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 15.7297(7) _cell_length_b 26.1766(18) _cell_length_c 25.2306(13) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 10388.7(10) _cell_formula_units_Z 8 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used 28248 _cell_measurement_theta_min 2.07 _cell_measurement_theta_max 25.94 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.33 _exptl_crystal_size_min 0.27 _exptl_crystal_density_diffrn 1.329 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4400 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 2.00 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details ; Busing, W. R. & Levy, H. A. (1957) Acta Cryst. 10, 180-182. and Coppens, P., Leiserowitz, L. & Rabinovich, D. (1965) Acta Cryst. 1965, 1035-1038. ; _exptl_absorpt_correction_T_min 0.3377 _exptl_absorpt_correction_T_max 0.6807 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 213(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 '1-circle goniometer' _diffrn_measurement_device_type 'STOE IPDS 1' _diffrn_measurement_method '\f scans' _diffrn_detector 'image plate' _diffrn_detector_type STOE _diffrn_standards_number 0 _diffrn_reflns_av_R_equivalents 0.0616 _diffrn_reflns_av_unetI/netI 0.053 _diffrn_reflns_number 42905 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.18 _diffrn_reflns_theta_max 25.48 _diffrn_reflns_theta_full 25.48 _diffrn_measured_fraction_theta_full 0.985 _diffrn_measured_fraction_theta_max 0.985 _reflns_number_total 9479 _reflns_number_gt 6547 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_cell_refinement 'STOE X-AREA' _computing_data_reduction 'STOE X-AREA, STOE X-RED' _computing_structure_solution ; 'SIR-92' Altomare, A., Cascarano, G., Giacovazzo, C. & Guagliardi, A. (1993) J. Appl. Cryst. 26, 343-350. ; _computing_structure_refinement ; 'SHELXL-97' Sheldrick, G.M. (2008) Acta Cryst. A64, 112 ; _computing_molecular_graphics 'DIAMOND 3.2' _computing_publication_material ; 'WinGX publication routines' Farrugia, L. J. (1999) WinGX, J. Appl. Cryst. 32, 837-838 ; #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0384P)^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_number_reflns 9479 _refine_ls_number_parameters 559 _refine_ls_number_restraints 33 _refine_ls_R_factor_all 0.0548 _refine_ls_R_factor_gt 0.0336 _refine_ls_wR_factor_ref 0.0735 _refine_ls_wR_factor_gt 0.0692 _refine_ls_goodness_of_fit_ref 0.872 _refine_ls_restrained_S_all 0.872 _refine_ls_shift/su_max 0.015 _refine_ls_shift/su_mean 0.001 _refine_diff_density_max 0.693 _refine_diff_density_min -0.369 _refine_diff_density_rms 0.064 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.3613(2) 0.57271(13) 0.63650(12) 0.0461(8) Uani 1 1 d . . . H1A H 0.4094 0.5528 0.6501 0.055 Uiso 1 1 calc R . . H1B H 0.3718 0.6087 0.6449 0.055 Uiso 1 1 calc R . . C2 C 0.2811(2) 0.55565(12) 0.66412(12) 0.0439(8) Uani 1 1 d . A . H2A H 0.2335 0.5768 0.652 0.053 Uiso 1 1 calc R . . H2B H 0.2875 0.5609 0.7024 0.053 Uiso 1 1 calc R . . C3 C 0.0978(2) 0.53107(12) 0.53294(11) 0.0440(8) Uani 1 1 d . A . H3A H 0.1568 0.5221 0.5412 0.053 Uiso 1 1 calc R . . H3B H 0.0766 0.5062 0.507 0.053 Uiso 1 1 calc R . . C4 C 0.0959(2) 0.58338(14) 0.50855(12) 0.0504(9) Uani 1 1 d . A . H4A H 0.0376 0.5911 0.4974 0.06 Uiso 1 1 calc R . . H4B H 0.1317 0.5834 0.4768 0.06 Uiso 1 1 calc R . . C5 C 0.2433(3) 0.48392(17) 0.41664(16) 0.0743(12) Uani 1 1 d . . . H5A H 0.2424 0.5137 0.4396 0.111 Uiso 1 1 calc R . . H5B H 0.1887 0.4668 0.4182 0.111 Uiso 1 1 calc R . . H5C H 0.2546 0.4946 0.3805 0.111 Uiso 1 1 calc R . . C6 C 0.3126(3) 0.44754(15) 0.43482(14) 0.0590(10) Uani 1 1 d . . . H6 H 0.3108 0.4168 0.412 0.071 Uiso 1 1 calc R . . C7 C 0.3966(3) 0.4728(2) 0.4274(2) 0.1054(19) Uani 1 1 d . . . H7A H 0.3989 0.4884 0.3926 0.158 Uiso 1 1 calc R . . H7B H 0.4415 0.4476 0.4305 0.158 Uiso 1 1 calc R . . H7C H 0.4041 0.4989 0.4544 0.158 Uiso 1 1 calc R . . C8 C 0.4552(3) 0.4105(3) 0.5388(2) 0.110(2) Uani 1 1 d . . . H8A H 0.4421 0.4299 0.5705 0.165 Uiso 1 1 calc R . . H8B H 0.4734 0.4336 0.511 0.165 Uiso 1 1 calc R . . H8C H 0.5004 0.3864 0.5464 0.165 Uiso 1 1 calc R . . C9 C 0.3770(3) 0.38186(17) 0.52091(16) 0.0783(14) Uani 1 1 d . . . H9 H 0.3911 0.3617 0.4889 0.094 Uiso 1 1 calc R . . C10 C 0.3519(5) 0.3451(2) 0.5659(2) 0.122(2) Uani 1 1 d . . . H10A H 0.4008 0.3248 0.576 0.184 Uiso 1 1 calc R . . H10B H 0.3067 0.3228 0.5538 0.184 Uiso 1 1 calc R . . H10C H 0.3324 0.3647 0.5962 0.184 Uiso 1 1 calc R . . C11 C 0.2005(4) 0.34233(19) 0.46057(18) 0.104(2) Uani 1 1 d . . . H11A H 0.234 0.3173 0.4798 0.155 Uiso 1 1 calc R . . H11B H 0.2292 0.3512 0.4278 0.155 Uiso 1 1 calc R . . H11C H 0.145 0.328 0.4526 0.155 Uiso 1 1 calc R . . C12 C 0.1895(3) 0.39100(16) 0.49509(15) 0.0719(12) Uani 1 1 d . . . H12 H 0.153 0.414 0.4738 0.086 Uiso 1 1 calc R . . C13 C 0.1413(3) 0.38186(18) 0.54447(18) 0.0822(13) Uani 1 1 d . . . H13A H 0.0854 0.3685 0.5358 0.123 Uiso 1 1 calc R . . H13B H 0.1352 0.4137 0.5637 0.123 Uiso 1 1 calc R . . H13C H 0.1715 0.3573 0.5663 0.123 Uiso 1 1 calc R . . C14A C -0.0101(16) 0.3147(7) 0.6975(8) 0.088(6) Uani 0.492(5) 1 d PD A 1 H14A H -0.0604 0.3205 0.7189 0.132 Uiso 0.492(5) 1 calc PR A 1 H14B H 0.0368 0.3049 0.7203 0.132 Uiso 0.492(5) 1 calc PR A 1 H14C H -0.0212 0.2877 0.6722 0.132 Uiso 0.492(5) 1 calc PR A 1 C15A C 0.0132(6) 0.3645(3) 0.6674(3) 0.055(2) Uani 0.492(5) 1 d PD A 1 H15A H 0.06 0.355 0.6432 0.066 Uiso 0.492(5) 1 calc PR A 1 C16A C -0.0595(6) 0.3823(3) 0.6315(3) 0.072(3) Uani 0.492(5) 1 d PD A 1 H16A H -0.0692 0.357 0.604 0.107 Uiso 0.492(5) 1 calc PR A 1 H16B H -0.0445 0.4146 0.6153 0.107 Uiso 0.492(5) 1 calc PR A 1 H16C H -0.1108 0.3864 0.6524 0.107 Uiso 0.492(5) 1 calc PR A 1 C14B C 0.1673(7) 0.3451(4) 0.6849(5) 0.096(4) Uani 0.508(5) 1 d PD A 2 H14D H 0.1838 0.3389 0.7214 0.144 Uiso 0.508(5) 1 calc PR A 2 H14E H 0.1994 0.3738 0.671 0.144 Uiso 0.508(5) 1 calc PR A 2 H14F H 0.1788 0.3149 0.6638 0.144 Uiso 0.508(5) 1 calc PR A 2 C15B C 0.0714(6) 0.3575(3) 0.6826(3) 0.063(2) Uani 0.508(5) 1 d PD A 2 H15B H 0.0557 0.3569 0.6446 0.075 Uiso 0.508(5) 1 calc PR A 2 C16B C 0.0173(14) 0.3159(6) 0.7095(9) 0.110(8) Uani 0.508(5) 1 d PD A 2 H16D H 0.0233 0.2841 0.6902 0.166 Uiso 0.508(5) 1 calc PR A 2 H16E H -0.0419 0.3262 0.7095 0.166 Uiso 0.508(5) 1 calc PR A 2 H16F H 0.0364 0.3112 0.7457 0.166 Uiso 0.508(5) 1 calc PR A 2 C17A C 0.1754(14) 0.4284(9) 0.7862(8) 0.094(9) Uani 0.492(5) 1 d PD A 1 H17A H 0.2136 0.4126 0.8115 0.141 Uiso 0.492(5) 1 calc PR A 1 H17B H 0.13 0.4458 0.805 0.141 Uiso 0.492(5) 1 calc PR A 1 H17C H 0.2066 0.4528 0.7648 0.141 Uiso 0.492(5) 1 calc PR A 1 C18A C 0.1372(5) 0.3870(3) 0.7500(3) 0.065(3) Uani 0.492(5) 1 d PD A 1 H18A H 0.1076 0.3616 0.7725 0.078 Uiso 0.492(5) 1 calc PR A 1 C19A C 0.2046(7) 0.3592(4) 0.7175(5) 0.091(4) Uani 0.492(5) 1 d PD A 1 H19A H 0.231 0.383 0.6931 0.137 Uiso 0.492(5) 1 calc PR A 1 H19B H 0.1782 0.3317 0.6977 0.137 Uiso 0.492(5) 1 calc PR A 1 H19C H 0.2475 0.3453 0.741 0.137 Uiso 0.492(5) 1 calc PR A 1 C17B C 0.1628(11) 0.4333(10) 0.7873(9) 0.093(8) Uani 0.508(5) 1 d PD A 2 H17D H 0.1707 0.4366 0.8253 0.139 Uiso 0.508(5) 1 calc PR A 2 H17E H 0.1893 0.462 0.7695 0.139 Uiso 0.508(5) 1 calc PR A 2 H17F H 0.1885 0.4017 0.7752 0.139 Uiso 0.508(5) 1 calc PR A 2 C18B C 0.0672(6) 0.4326(3) 0.7746(3) 0.066(2) Uani 0.508(5) 1 d PD A 2 H18B H 0.0477 0.4682 0.7802 0.079 Uiso 0.508(5) 1 calc PR A 2 C19B C 0.0161(8) 0.4007(5) 0.8131(3) 0.101(4) Uani 0.508(5) 1 d PD A 2 H19D H 0.0077 0.3668 0.7985 0.151 Uiso 0.508(5) 1 calc PR A 2 H19E H -0.0387 0.4167 0.8191 0.151 Uiso 0.508(5) 1 calc PR A 2 H19F H 0.0465 0.3981 0.8464 0.151 Uiso 0.508(5) 1 calc PR A 2 C20A C -0.0602(10) 0.4039(4) 0.7926(5) 0.129(6) Uani 0.492(5) 1 d PD A 1 H20A H -0.0896 0.4226 0.8203 0.194 Uiso 0.492(5) 1 calc PR A 1 H20B H -0.0146 0.3839 0.8082 0.194 Uiso 0.492(5) 1 calc PR A 1 H20C H -0.0999 0.3812 0.775 0.194 Uiso 0.492(5) 1 calc PR A 1 C21A C -0.0236(6) 0.4410(3) 0.7529(3) 0.073(3) Uani 0.492(5) 1 d PD A 1 H21A H 0.0106 0.464 0.7755 0.087 Uiso 0.492(5) 1 calc PR A 1 C22A C -0.086(2) 0.4775(13) 0.7272(15) 0.091(10) Uani 0.492(5) 1 d PD A 1 H22A H -0.1296 0.4582 0.7087 0.136 Uiso 0.492(5) 1 calc PR A 1 H22B H -0.0563 0.4992 0.7022 0.136 Uiso 0.492(5) 1 calc PR A 1 H22C H -0.1124 0.4985 0.7543 0.136 Uiso 0.492(5) 1 calc PR A 1 C20B C -0.0990(6) 0.4160(4) 0.6412(3) 0.065(2) Uani 0.508(5) 1 d P A 2 H20D H -0.1594 0.4227 0.6378 0.097 Uiso 0.508(5) 1 calc PR A 2 H20E H -0.0878 0.3804 0.6331 0.097 Uiso 0.508(5) 1 calc PR A 2 H20F H -0.0677 0.4375 0.6168 0.097 Uiso 0.508(5) 1 calc PR A 2 C21B C -0.0706(5) 0.4275(3) 0.6983(3) 0.0508(19) Uani 0.508(5) 1 d P A 2 H21B H -0.0978 0.4024 0.7223 0.061 Uiso 0.508(5) 1 calc PR A 2 C22B C -0.099(2) 0.4809(11) 0.7146(15) 0.072(4) Uani 0.508(5) 1 d P A 2 H22D H -0.0648 0.5061 0.6961 0.108 Uiso 0.508(5) 1 calc PR A 2 H22E H -0.0912 0.485 0.7526 0.108 Uiso 0.508(5) 1 calc PR A 2 H22F H -0.1582 0.4855 0.7057 0.108 Uiso 0.508(5) 1 calc PR A 2 C23 C -0.1307(3) 0.61755(15) 0.68159(15) 0.0625(10) Uani 1 1 d . . . H23A H -0.1845 0.6069 0.6967 0.094 Uiso 1 1 calc R . . H23B H -0.1059 0.5894 0.6619 0.094 Uiso 1 1 calc R . . H23C H -0.1399 0.6463 0.658 0.094 Uiso 1 1 calc R . . C24 C -0.0698(2) 0.63351(12) 0.72636(13) 0.0457(8) Uani 1 1 d . . . H24 H -0.066 0.6039 0.7506 0.055 Uiso 1 1 calc R . . C25 C -0.1105(3) 0.67688(14) 0.75832(14) 0.0590(10) Uani 1 1 d . . . H25A H -0.1199 0.7061 0.7354 0.089 Uiso 1 1 calc R . . H25B H -0.073 0.6866 0.7871 0.089 Uiso 1 1 calc R . . H25C H -0.1645 0.6654 0.7727 0.089 Uiso 1 1 calc R . . C26 C 0.1432(3) 0.73005(16) 0.6862(2) 0.0803(13) Uani 1 1 d . . . H26A H 0.167 0.7114 0.6565 0.12 Uiso 1 1 calc R . . H26B H 0.1749 0.722 0.7181 0.12 Uiso 1 1 calc R . . H26C H 0.1466 0.7664 0.6792 0.12 Uiso 1 1 calc R . . C27 C 0.0503(2) 0.71475(12) 0.69360(15) 0.0564(10) Uani 1 1 d . . . H27 H 0.0285 0.7313 0.7261 0.068 Uiso 1 1 calc R . . C28 C -0.0027(3) 0.73290(16) 0.64663(17) 0.0779(13) Uani 1 1 d . . . H28A H 0.0006 0.7698 0.644 0.117 Uiso 1 1 calc R . . H28B H -0.0615 0.7227 0.6517 0.117 Uiso 1 1 calc R . . H28C H 0.019 0.7177 0.6143 0.117 Uiso 1 1 calc R . . C29 C 0.1114(3) 0.57169(13) 0.76754(14) 0.0554(9) Uani 1 1 d . . . H29A H 0.1549 0.5636 0.7935 0.083 Uiso 1 1 calc R . . H29B H 0.1233 0.5538 0.7347 0.083 Uiso 1 1 calc R . . H29C H 0.0563 0.5612 0.7809 0.083 Uiso 1 1 calc R . . C30 C 0.1110(2) 0.62885(12) 0.75738(13) 0.0499(8) Uani 1 1 d . . . H30 H 0.1693 0.638 0.7461 0.06 Uiso 1 1 calc R . . C31 C 0.0944(3) 0.65781(16) 0.80920(15) 0.0712(12) Uani 1 1 d . . . H31A H 0.0393 0.648 0.8233 0.107 Uiso 1 1 calc R . . H31B H 0.095 0.6943 0.8024 0.107 Uiso 1 1 calc R . . H31C H 0.1383 0.6494 0.8347 0.107 Uiso 1 1 calc R . . C32 C 0.3171(3) 0.69637(14) 0.58193(17) 0.0636(10) Uani 1 1 d . . . H32A H 0.2847 0.7266 0.571 0.076 Uiso 1 1 calc R . . H32B H 0.3012 0.6888 0.6187 0.076 Uiso 1 1 calc R . . C33 C 0.4121(4) 0.7103(2) 0.5811(2) 0.1054(18) Uani 1 1 d . . . H33A H 0.422 0.7355 0.6092 0.127 Uiso 1 1 calc R . . H33B H 0.4443 0.6796 0.5905 0.127 Uiso 1 1 calc R . . C34 C 0.4454(4) 0.7292(3) 0.5360(3) 0.126(2) Uani 1 1 d . . . H34A H 0.4085 0.7567 0.5233 0.152 Uiso 1 1 calc R . . H34B H 0.4447 0.7021 0.5091 0.152 Uiso 1 1 calc R . . C35 C 0.5375(4) 0.7502(2) 0.5402(3) 0.123(2) Uani 1 1 d . . . H35A H 0.5389 0.7781 0.5654 0.185 Uiso 1 1 calc R . . H35B H 0.5558 0.7624 0.5057 0.185 Uiso 1 1 calc R . . H35C H 0.5752 0.7232 0.552 0.185 Uiso 1 1 calc R . . C36 C 0.2960(2) 0.63894(13) 0.45939(12) 0.0482(8) Uani 1 1 d . . . H36A H 0.3569 0.637 0.4516 0.058 Uiso 1 1 calc R . . H36B H 0.2691 0.6084 0.4444 0.058 Uiso 1 1 calc R . . C37 C 0.2598(2) 0.68536(12) 0.43211(12) 0.0482(8) Uani 1 1 d . . . H37A H 0.1981 0.6856 0.4373 0.058 Uiso 1 1 calc R . . H37B H 0.2827 0.7159 0.4494 0.058 Uiso 1 1 calc R . . C38 C 0.2777(3) 0.68895(14) 0.37354(14) 0.0592(9) Uani 1 1 d . . . H38A H 0.2561 0.658 0.3563 0.071 Uiso 1 1 calc R . . H38B H 0.3394 0.6899 0.3683 0.071 Uiso 1 1 calc R . . C39 C 0.2389(3) 0.73493(18) 0.34680(17) 0.0838(14) Uani 1 1 d . . . H39A H 0.1778 0.7344 0.3516 0.126 Uiso 1 1 calc R . . H39B H 0.252 0.7341 0.3092 0.126 Uiso 1 1 calc R . . H39C H 0.2621 0.7658 0.3623 0.126 Uiso 1 1 calc R . . P1 P 0.29152(6) 0.42725(3) 0.50469(3) 0.0450(2) Uani 1 1 d . . . P2 P 0.05220(6) 0.42057(3) 0.70447(3) 0.0446(2) Uani 1 1 d . . . P3 P 0.03980(6) 0.64474(3) 0.70107(3) 0.03983(19) Uani 1 1 d . . . S1 S 0.35625(5) 0.56525(3) 0.56466(3) 0.04244(19) Uani 1 1 d . . . S2 S 0.25663(5) 0.48853(3) 0.65153(3) 0.04252(18) Uani 1 1 d . . . S3 S 0.03383(5) 0.52636(3) 0.59359(3) 0.04195(18) Uani 1 1 d . . . S4 S 0.13257(6) 0.63356(3) 0.55343(3) 0.0469(2) Uani 1 1 d . . . Cu1 Cu 0.28891(3) 0.487449(14) 0.565220(15) 0.04234(10) Uani 1 1 d . A . Cu2 Cu 0.11194(3) 0.479544(14) 0.651923(14) 0.04019(10) Uani 1 1 d . A . Cu3 Cu 0.07054(3) 0.601613(14) 0.628812(14) 0.04127(10) Uani 1 1 d . A . Ga1 Ga 0.28038(3) 0.638104(13) 0.537147(14) 0.04370(10) Uani 1 1 d . A . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.045(2) 0.0487(18) 0.0451(18) 0.0019(14) -0.0062(15) -0.0095(15) C2 0.046(2) 0.0507(18) 0.0346(15) -0.0037(13) -0.0006(14) -0.0013(15) C3 0.036(2) 0.062(2) 0.0344(16) -0.0126(14) -0.0018(13) 0.0041(15) C4 0.041(2) 0.077(2) 0.0327(16) 0.0058(15) -0.0036(14) 0.0049(17) C5 0.078(3) 0.084(3) 0.061(2) 0.016(2) 0.000(2) 0.002(2) C6 0.068(3) 0.064(2) 0.0453(19) -0.0018(17) 0.0134(18) 0.0051(19) C7 0.060(3) 0.172(6) 0.084(3) 0.043(3) 0.015(3) -0.005(3) C8 0.058(4) 0.190(6) 0.081(3) 0.023(4) 0.003(3) 0.049(4) C9 0.090(4) 0.084(3) 0.061(2) -0.002(2) 0.005(2) 0.045(3) C10 0.156(6) 0.096(4) 0.116(4) 0.038(3) -0.005(4) 0.043(4) C11 0.167(6) 0.079(3) 0.065(3) -0.024(2) 0.006(3) -0.042(3) C12 0.092(4) 0.069(3) 0.054(2) -0.0063(19) 0.001(2) -0.025(2) C13 0.065(3) 0.089(3) 0.093(3) -0.012(3) 0.009(3) -0.016(2) C14A 0.141(15) 0.059(8) 0.065(7) 0.007(6) 0.005(8) -0.050(8) C15A 0.071(7) 0.047(4) 0.047(4) 0.006(3) 0.000(4) -0.017(4) C16A 0.091(8) 0.065(6) 0.058(5) 0.007(4) -0.021(5) -0.036(5) C14B 0.086(9) 0.083(7) 0.119(10) -0.013(6) -0.015(7) 0.019(6) C15B 0.078(7) 0.049(4) 0.061(5) -0.002(4) 0.012(5) -0.003(4) C16B 0.17(2) 0.028(6) 0.129(16) -0.005(7) 0.046(14) -0.012(8) C17A 0.091(12) 0.123(18) 0.069(13) 0.045(11) -0.033(9) -0.050(12) C18A 0.065(6) 0.065(5) 0.065(5) 0.035(4) -0.022(4) -0.017(4) C19A 0.054(7) 0.087(7) 0.133(10) 0.030(7) 0.010(7) 0.023(6) C17B 0.106(15) 0.091(12) 0.081(14) -0.004(9) -0.059(10) 0.004(10) C18B 0.081(7) 0.080(5) 0.038(4) 0.005(3) -0.007(4) -0.012(5) C19B 0.103(9) 0.161(11) 0.038(4) 0.020(5) 0.012(5) -0.033(8) C20A 0.168(15) 0.106(9) 0.113(10) 0.034(7) 0.108(11) 0.027(9) C21A 0.092(8) 0.066(5) 0.061(5) 0.014(4) 0.028(5) 0.019(5) C22A 0.075(17) 0.085(11) 0.11(2) 0.025(11) 0.046(13) 0.024(10) C20B 0.060(6) 0.069(5) 0.065(5) 0.007(4) -0.025(4) -0.019(4) C21B 0.045(4) 0.055(4) 0.053(4) 0.012(3) 0.004(3) -0.010(3) C22B 0.056(9) 0.075(11) 0.086(12) 0.002(8) 0.012(7) 0.003(7) C23 0.044(3) 0.075(2) 0.068(2) -0.0088(19) -0.0023(19) 0.0024(18) C24 0.043(2) 0.0468(17) 0.0473(17) 0.0023(14) 0.0063(15) 0.0010(15) C25 0.054(3) 0.064(2) 0.059(2) -0.0004(17) 0.0191(18) 0.0098(18) C26 0.077(3) 0.060(2) 0.104(3) 0.000(2) 0.023(3) -0.017(2) C27 0.066(3) 0.0375(17) 0.066(2) -0.0036(15) 0.0246(19) -0.0016(16) C28 0.083(4) 0.061(2) 0.089(3) 0.022(2) 0.021(3) 0.018(2) C29 0.060(3) 0.056(2) 0.0500(19) -0.0024(16) -0.0002(18) 0.0080(18) C30 0.045(2) 0.0524(19) 0.0522(19) -0.0090(15) -0.0038(16) -0.0028(16) C31 0.084(3) 0.072(2) 0.057(2) -0.0204(19) -0.015(2) 0.007(2) C32 0.059(3) 0.053(2) 0.078(3) -0.0007(18) 0.011(2) -0.0105(19) C33 0.115(5) 0.086(3) 0.115(4) 0.006(3) 0.003(4) -0.035(3) C34 0.121(6) 0.118(5) 0.140(6) 0.018(4) 0.003(4) -0.041(4) C35 0.085(4) 0.134(5) 0.151(6) 0.010(4) 0.011(4) -0.057(4) C36 0.051(2) 0.0509(18) 0.0431(17) 0.0065(14) 0.0115(15) 0.0056(16) C37 0.053(2) 0.0482(19) 0.0438(17) 0.0026(14) 0.0002(15) 0.0060(16) C38 0.063(3) 0.062(2) 0.053(2) 0.0078(17) 0.0078(19) -0.0083(19) C39 0.100(4) 0.087(3) 0.064(3) 0.030(2) -0.010(2) -0.001(3) P1 0.0495(6) 0.0459(4) 0.0396(4) -0.0041(3) 0.0076(4) 0.0054(4) P2 0.0487(6) 0.0482(5) 0.0368(4) 0.0018(3) 0.0047(4) -0.0135(4) P3 0.0402(5) 0.0379(4) 0.0414(4) -0.0040(3) 0.0078(4) 0.0008(3) S1 0.0395(5) 0.0451(4) 0.0427(4) 0.0076(3) 0.0059(3) 0.0013(3) S2 0.0376(5) 0.0472(4) 0.0428(4) 0.0054(3) 0.0019(3) -0.0053(3) S3 0.0377(5) 0.0463(4) 0.0419(4) -0.0014(3) 0.0045(3) 0.0000(3) S4 0.0440(5) 0.0475(4) 0.0492(4) 0.0089(3) 0.0109(4) 0.0069(4) Cu1 0.0380(2) 0.0462(2) 0.0427(2) -0.00628(16) -0.00274(17) 0.00493(17) Cu2 0.0413(2) 0.0439(2) 0.03544(18) -0.00141(15) 0.00285(16) -0.00857(17) Cu3 0.0389(2) 0.0476(2) 0.03731(18) -0.00419(16) 0.00445(17) 0.00605(18) Ga1 0.0443(2) 0.04243(18) 0.04433(19) 0.00899(15) 0.00907(16) 0.00170(16) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.509(5) . ? C1 S1 1.825(3) . ? C2 S2 1.827(3) . ? C3 C4 1.502(5) . ? C3 S3 1.835(3) . ? C4 S4 1.828(4) . ? C5 C6 1.518(6) . ? C6 C7 1.489(6) . ? C6 P1 1.871(3) . ? C8 C9 1.509(7) . ? C9 C10 1.539(7) . ? C9 P1 1.840(4) . ? C11 C12 1.553(6) . ? C12 C13 1.478(6) . ? C12 P1 1.880(4) . ? C14A C15A 1.552(11) . ? C15A C16A 1.532(10) . ? C15A P2 1.845(7) . ? C14B C15B 1.543(12) . ? C15B C16B 1.540(13) . ? C15B P2 1.766(7) . ? C17A C18A 1.539(14) . ? C18A C19A 1.526(11) . ? C18A P2 1.969(7) . ? C17B C18B 1.537(15) . ? C18B C19B 1.513(10) . ? C18B P2 1.812(7) . ? C20A C21A 1.511(10) . ? C21A C22A 1.518(16) . ? C21A P2 1.787(8) . ? C20B C21B 1.537(10) . ? C21B C22B 1.52(3) . ? C21B P2 1.947(7) . ? C23 C24 1.538(5) . ? C24 C25 1.533(4) . ? C24 P3 1.862(4) . ? C26 C27 1.526(6) . ? C27 C28 1.525(6) . ? C27 P3 1.850(3) . ? C29 C30 1.518(5) . ? C30 C31 1.534(5) . ? C30 P3 1.856(4) . ? C32 C33 1.539(7) . ? C32 Ga1 1.984(4) . ? C33 C34 1.346(7) . ? C34 C35 1.553(7) . ? C36 C37 1.508(4) . ? C36 Ga1 1.977(3) . ? C37 C38 1.507(5) . ? C38 C39 1.509(5) . ? P1 Cu1 2.1948(9) . ? P2 Cu2 2.2414(9) . ? P3 Cu3 2.1982(8) . ? S1 Cu1 2.2955(9) . ? S1 Ga1 2.3544(9) . ? S2 Cu1 2.2362(9) . ? S2 Cu2 2.2880(9) . ? S3 Cu3 2.2370(9) . ? S3 Cu2 2.2755(9) . ? S4 Cu3 2.2954(9) . ? S4 Ga1 2.3640(10) . ? 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 C2 C1 S1 113.0(2) . . ? C1 C2 S2 112.4(2) . . ? C4 C3 S3 113.1(2) . . ? C3 C4 S4 113.3(2) . . ? C7 C6 C5 108.7(4) . . ? C7 C6 P1 113.7(3) . . ? C5 C6 P1 109.6(3) . . ? C8 C9 C10 107.4(4) . . ? C8 C9 P1 110.0(3) . . ? C10 C9 P1 112.3(4) . . ? C13 C12 C11 113.4(4) . . ? C13 C12 P1 114.3(3) . . ? C11 C12 P1 113.1(4) . . ? C16A C15A C14A 111.6(10) . . ? C16A C15A P2 107.9(5) . . ? C14A C15A P2 119.9(9) . . ? C16B C15B C14B 112.0(11) . . ? C16B C15B P2 115.4(9) . . ? C14B C15B P2 110.6(7) . . ? C19A C18A C17A 112.5(12) . . ? C19A C18A P2 111.8(6) . . ? C17A C18A P2 107.3(11) . . ? C19B C18B C17B 113.1(12) . . ? C19B C18B P2 117.5(6) . . ? C17B C18B P2 109.4(10) . . ? C20A C21A C22A 116.2(17) . . ? C20A C21A P2 121.1(6) . . ? C22A C21A P2 109.2(16) . . ? C22B C21B C20B 110.4(13) . . ? C22B C21B P2 110.6(13) . . ? C20B C21B P2 110.2(6) . . ? C25 C24 C23 109.1(3) . . ? C25 C24 P3 116.8(3) . . ? C23 C24 P3 111.6(2) . . ? C28 C27 C26 110.3(3) . . ? C28 C27 P3 109.8(3) . . ? C26 C27 P3 111.0(3) . . ? C29 C30 C31 110.1(3) . . ? C29 C30 P3 110.7(2) . . ? C31 C30 P3 116.0(3) . . ? C33 C32 Ga1 117.2(3) . . ? C34 C33 C32 118.5(5) . . ? C33 C34 C35 115.8(6) . . ? C37 C36 Ga1 114.5(2) . . ? C38 C37 C36 115.3(3) . . ? C37 C38 C39 114.4(3) . . ? C9 P1 C6 105.28(19) . . ? C9 P1 C12 109.0(2) . . ? C6 P1 C12 99.98(18) . . ? C9 P1 Cu1 108.81(15) . . ? C6 P1 Cu1 117.08(13) . . ? C12 P1 Cu1 115.85(14) . . ? C15B P2 C21A 127.3(4) . . ? C15B P2 C18B 116.4(4) . . ? C21A P2 C18B 50.8(4) . . ? C15B P2 C15A 32.4(3) . . ? C21A P2 C15A 111.2(4) . . ? C18B P2 C15A 132.5(3) . . ? C15B P2 C21B 103.4(4) . . ? C21A P2 C21B 50.6(4) . . ? C18B P2 C21B 101.0(4) . . ? C15A P2 C21B 72.7(4) . . ? C15B P2 C18A 69.4(4) . . ? C21A P2 C18A 100.8(4) . . ? C18B P2 C18A 54.5(4) . . ? C15A P2 C18A 99.6(3) . . ? C21B P2 C18A 139.6(3) . . ? C15B P2 Cu2 112.8(3) . . ? C21A P2 Cu2 118.5(3) . . ? C18B P2 Cu2 113.8(2) . . ? C15A P2 Cu2 112.8(2) . . ? C21B P2 Cu2 107.76(19) . . ? C18A P2 Cu2 111.6(2) . . ? C27 P3 C30 104.25(17) . . ? C27 P3 C24 105.91(16) . . ? C30 P3 C24 105.13(16) . . ? C27 P3 Cu3 113.87(12) . . ? C30 P3 Cu3 112.77(11) . . ? C24 P3 Cu3 114.00(11) . . ? C1 S1 Cu1 96.27(11) . . ? C1 S1 Ga1 103.20(12) . . ? Cu1 S1 Ga1 119.11(4) . . ? C2 S2 Cu1 97.68(10) . . ? C2 S2 Cu2 107.93(12) . . ? Cu1 S2 Cu2 103.22(3) . . ? C3 S3 Cu3 97.51(11) . . ? C3 S3 Cu2 106.24(11) . . ? Cu3 S3 Cu2 94.46(3) . . ? C4 S4 Cu3 96.73(11) . . ? C4 S4 Ga1 103.84(12) . . ? Cu3 S4 Ga1 125.48(4) . . ? P1 Cu1 S2 133.70(4) . . ? P1 Cu1 S1 128.61(4) . . ? S2 Cu1 S1 95.71(3) . . ? P2 Cu2 S3 121.81(4) . . ? P2 Cu2 S2 119.36(4) . . ? S3 Cu2 S2 118.62(3) . . ? P3 Cu3 S3 136.47(3) . . ? P3 Cu3 S4 126.41(4) . . ? S3 Cu3 S4 95.82(3) . . ? C36 Ga1 C32 121.37(16) . . ? C36 Ga1 S1 103.81(10) . . ? C32 Ga1 S1 107.90(13) . . ? C36 Ga1 S4 107.15(11) . . ? C32 Ga1 S4 103.05(12) . . ? S1 Ga1 S4 113.99(3) . . ? _chemical_name_common ; bis(mu!3$-1,2-dithiolatoethane-S,S,S',S')-di(butan-1-ido) - tris(triisopropylphosphine)-tricopper(+1)-gallium(+3) ; data_[(iPr3PCu)3(SC2H4S)2InMe2] _database_code_depnum_ccdc_archive 'CCDC 907027' #TrackingRef '17787_web_deposit_cif_file_0_DirkFriedrich_1360942799.29_[(iPr3PCu)3(SC2H4S)2InMe2].cif' _audit_creation_date 2013-02-14T13:32:21-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; bis(\m~3~-1,2-dithiolatoethane-S,S,S',S')-dimethanido -tris(triisopropylphosphine)-tricopper(+1)-indium(+3) ; _chemical_formula_moiety 'C33 H77 Cu3 In1 P3 S4' _chemical_formula_sum 'C33 H77 Cu3 In P3 S4' _chemical_formula_weight 1000.54 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.7124(11) _cell_length_b 13.8240(11) _cell_length_c 15.3399(13) _cell_angle_alpha 112.603(6) _cell_angle_beta 94.946(6) _cell_angle_gamma 112.568(6) _cell_volume 2383.9(3) _cell_formula_units_Z 2 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 19878 _cell_measurement_theta_min 1.92 _cell_measurement_theta_max 29.36 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.503 _exptl_crystal_size_mid 0.451 _exptl_crystal_size_min 0.115 _exptl_crystal_density_diffrn 1.394 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1040 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 2.09 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details ; Busing, W. R. & Levy, H. A. (1957) Acta Cryst. 10, 180-182. and Coppens, P., Leiserowitz, L. & Rabinovich, D. (1965) Acta Cryst. 1965, 1035-1038. ; _exptl_absorpt_correction_T_min 0.3968 _exptl_absorpt_correction_T_max 0.7809 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 180(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 '2-circle goniometer' _diffrn_measurement_device_type 'STOE IPDS-2T' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 6.67 _diffrn_detector 'image plate (34 cm diameter / schwenk)' _diffrn_detector_type STOE _diffrn_standards_number 0 _diffrn_reflns_av_R_equivalents 0.042 _diffrn_reflns_av_unetI/netI 0.0605 _diffrn_reflns_number 26872 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.91 _diffrn_reflns_theta_max 29.03 _diffrn_reflns_theta_full 29.03 _diffrn_measured_fraction_theta_full 0.99 _diffrn_measured_fraction_theta_max 0.99 _reflns_number_total 12590 _reflns_number_gt 8805 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_cell_refinement 'STOE X-AREA' _computing_data_reduction 'STOE X-AREA, STOE X-RED' _computing_structure_solution ; 'SIR-92' Altomare, A., Cascarano, G., Giacovazzo, C. & Guagliardi, A. (1993) J. Appl. Cryst. 26, 343-350. ; _computing_structure_refinement ; 'SHELXL-97' Sheldrick, G.M. (2008) Acta Cryst. A64, 112 ; _computing_molecular_graphics 'DIAMOND 3.2' _computing_publication_material ; 'WinGX publication routines' Farrugia, L. J. (1999) WinGX, J. Appl. Cryst. 32, 837-838 ; #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0190P)^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 mixed _refine_ls_extinction_method none _refine_ls_number_reflns 12590 _refine_ls_number_parameters 505 _refine_ls_number_restraints 183 _refine_ls_R_factor_all 0.0451 _refine_ls_R_factor_gt 0.0257 _refine_ls_wR_factor_ref 0.0474 _refine_ls_wR_factor_gt 0.0454 _refine_ls_goodness_of_fit_ref 0.792 _refine_ls_restrained_S_all 0.791 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.595 _refine_diff_density_min -0.748 _refine_diff_density_rms 0.068 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' In In -0.7276 1.31 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.61826(16) 0.29006(19) 0.06685(16) 0.0295(4) Uani 1 1 d . A . H1A H 0.5795 0.2518 -0.0038 0.035 Uiso 1 1 calc R . . H1B H 0.6946 0.301 0.072 0.035 Uiso 1 1 calc R . . C2 C 0.56209(16) 0.20932(19) 0.11138(15) 0.0285(4) Uani 1 1 d . A . H2A H 0.6038 0.2449 0.1808 0.034 Uiso 1 1 calc R . . H2B H 0.5632 0.1331 0.0759 0.034 Uiso 1 1 calc R . . C3 C 0.53634(15) 0.42611(19) 0.38313(15) 0.0266(4) Uani 1 1 d . A . H3A H 0.5274 0.4131 0.3142 0.032 Uiso 1 1 calc R . . H3B H 0.4824 0.4529 0.408 0.032 Uiso 1 1 calc R . . C4 C 0.65233(15) 0.52254(19) 0.44436(15) 0.0284(4) Uani 1 1 d . A . H4A H 0.6594 0.5402 0.5142 0.034 Uiso 1 1 calc R . . H4B H 0.6639 0.595 0.4389 0.034 Uiso 1 1 calc R . . C5A C 0.4791(7) 0.6431(8) 0.1409(6) 0.0524(18) Uani 0.607(10) 1 d PDU A 1 H5A1 H 0.5152 0.7275 0.1599 0.079 Uiso 0.607(10) 1 calc PR A 1 H5A2 H 0.4281 0.6008 0.0751 0.079 Uiso 0.607(10) 1 calc PR A 1 H5A3 H 0.5345 0.6148 0.1407 0.079 Uiso 0.607(10) 1 calc PR A 1 C6A C 0.4147(7) 0.6214(10) 0.2154(6) 0.0333(17) Uani 0.607(10) 1 d PDU A 1 H6A H 0.3585 0.6509 0.2157 0.04 Uiso 0.607(10) 1 calc PR A 1 C7A C 0.4936(8) 0.6866(9) 0.3194(6) 0.0461(18) Uani 0.607(10) 1 d PDU A 1 H7A1 H 0.541 0.6493 0.3222 0.069 Uiso 0.607(10) 1 calc PR A 1 H7A2 H 0.451 0.683 0.3672 0.069 Uiso 0.607(10) 1 calc PR A 1 H7A3 H 0.539 0.7689 0.3351 0.069 Uiso 0.607(10) 1 calc PR A 1 C8A C 0.1738(12) 0.4761(12) 0.0570(12) 0.069(4) Uani 0.607(10) 1 d PDU A 1 H8A1 H 0.2277 0.5359 0.0436 0.104 Uiso 0.607(10) 1 calc PR A 1 H8A2 H 0.1561 0.5146 0.1174 0.104 Uiso 0.607(10) 1 calc PR A 1 H8A3 H 0.1069 0.4282 0.0022 0.104 Uiso 0.607(10) 1 calc PR A 1 C9A C 0.2221(5) 0.3969(5) 0.0695(3) 0.0406(14) Uani 0.607(10) 1 d PDU A 1 H9A H 0.1625 0.3364 0.0803 0.049 Uiso 0.607(10) 1 calc PR A 1 C10A C 0.2422(7) 0.3283(7) -0.0274(5) 0.0534(18) Uani 0.607(10) 1 d PDU A 1 H10A H 0.1747 0.2874 -0.0809 0.08 Uiso 0.607(10) 1 calc PR A 1 H10B H 0.2636 0.2707 -0.0213 0.08 Uiso 0.607(10) 1 calc PR A 1 H10C H 0.301 0.3831 -0.0416 0.08 Uiso 0.607(10) 1 calc PR A 1 C11A C 0.2184(11) 0.5278(9) 0.3149(8) 0.042(2) Uani 0.607(10) 1 d PDU A 1 H11A H 0.1496 0.4917 0.2639 0.063 Uiso 0.607(10) 1 calc PR A 1 H11B H 0.263 0.6083 0.3254 0.063 Uiso 0.607(10) 1 calc PR A 1 H11C H 0.2019 0.5294 0.3762 0.063 Uiso 0.607(10) 1 calc PR A 1 C12A C 0.2814(7) 0.4563(7) 0.2823(6) 0.0254(13) Uani 0.607(10) 1 d PDU A 1 H12A H 0.3453 0.4927 0.3405 0.031 Uiso 0.607(10) 1 calc PR A 1 C13A C 0.2181(5) 0.3298(5) 0.2645(5) 0.0401(13) Uani 0.607(10) 1 d PDU A 1 H13A H 0.1967 0.3289 0.3235 0.06 Uiso 0.607(10) 1 calc PR A 1 H13B H 0.2647 0.2902 0.2491 0.06 Uiso 0.607(10) 1 calc PR A 1 H13C H 0.1522 0.2889 0.2093 0.06 Uiso 0.607(10) 1 calc PR A 1 C5B C 0.5127(9) 0.6696(12) 0.1715(8) 0.044(2) Uani 0.393(10) 1 d PDU A 2 H5B1 H 0.5649 0.7532 0.2075 0.066 Uiso 0.393(10) 1 calc PR A 2 H5B2 H 0.4669 0.6549 0.1107 0.066 Uiso 0.393(10) 1 calc PR A 2 H5B3 H 0.553 0.6228 0.1556 0.066 Uiso 0.393(10) 1 calc PR A 2 C6B C 0.4394(10) 0.6349(15) 0.2354(10) 0.032(3) Uani 0.393(10) 1 d PDU A 2 H6B H 0.391 0.6747 0.243 0.038 Uiso 0.393(10) 1 calc PR A 2 C7B C 0.5106(14) 0.6761(15) 0.3381(10) 0.055(3) Uani 0.393(10) 1 d PDU A 2 H7B1 H 0.5615 0.6413 0.3315 0.082 Uiso 0.393(10) 1 calc PR A 2 H7B2 H 0.4632 0.6512 0.3774 0.082 Uiso 0.393(10) 1 calc PR A 2 H7B3 H 0.5525 0.762 0.3705 0.082 Uiso 0.393(10) 1 calc PR A 2 C8B C 0.2078(11) 0.3058(10) -0.0113(10) 0.072(4) Uani 0.393(10) 1 d PDU A 2 H8B1 H 0.1566 0.2687 0.0201 0.108 Uiso 0.393(10) 1 calc PR A 2 H8B2 H 0.2606 0.2736 -0.0214 0.108 Uiso 0.393(10) 1 calc PR A 2 H8B3 H 0.1669 0.2901 -0.0748 0.108 Uiso 0.393(10) 1 calc PR A 2 C9B C 0.2692(7) 0.4385(7) 0.0546(5) 0.0378(19) Uani 0.393(10) 1 d PDU A 2 H9B H 0.3251 0.4725 0.0232 0.045 Uiso 0.393(10) 1 calc PR A 2 C10B C 0.1947(18) 0.4991(19) 0.0653(18) 0.064(5) Uani 0.393(10) 1 d PDU A 2 H10D H 0.167 0.4939 0.0017 0.095 Uiso 0.393(10) 1 calc PR A 2 H10E H 0.2368 0.5819 0.1136 0.095 Uiso 0.393(10) 1 calc PR A 2 H10F H 0.1328 0.4602 0.0872 0.095 Uiso 0.393(10) 1 calc PR A 2 C11B C 0.2018(17) 0.5133(16) 0.2889(13) 0.050(4) Uani 0.393(10) 1 d PDU A 2 H11D H 0.14 0.4853 0.2336 0.075 Uiso 0.393(10) 1 calc PR A 2 H11E H 0.2495 0.5971 0.3115 0.075 Uiso 0.393(10) 1 calc PR A 2 H11F H 0.1739 0.5018 0.3427 0.075 Uiso 0.393(10) 1 calc PR A 2 C12B C 0.2681(12) 0.4432(11) 0.2557(10) 0.044(4) Uani 0.393(10) 1 d PDU A 2 H12B H 0.3217 0.4668 0.3174 0.053 Uiso 0.393(10) 1 calc PR A 2 C13B C 0.1905(11) 0.3129(10) 0.2202(11) 0.071(4) Uani 0.393(10) 1 d PDU A 2 H13D H 0.1619 0.3023 0.274 0.107 Uiso 0.393(10) 1 calc PR A 2 H13E H 0.2306 0.2666 0.1991 0.107 Uiso 0.393(10) 1 calc PR A 2 H13F H 0.1293 0.2866 0.165 0.107 Uiso 0.393(10) 1 calc PR A 2 C14 C 0.1999(2) 0.1519(2) 0.39573(18) 0.0451(6) Uani 1 1 d . . . H14A H 0.156 0.1905 0.4254 0.068 Uiso 1 1 calc R . . H14B H 0.2679 0.2102 0.3943 0.068 Uiso 1 1 calc R . . H14C H 0.2177 0.1159 0.4346 0.068 Uiso 1 1 calc R . . C15 C 0.13381(16) 0.05617(19) 0.29026(16) 0.0304(5) Uani 1 1 d . . . H15 H 0.1104 0.0954 0.2559 0.037 Uiso 1 1 calc R . . C16 C 0.02792(18) -0.0376(2) 0.2913(2) 0.0493(7) Uani 1 1 d . . . H16A H 0.0467 -0.0763 0.327 0.074 Uiso 1 1 calc R . . H16B H -0.015 -0.0961 0.2237 0.074 Uiso 1 1 calc R . . H16C H -0.0155 -0.0001 0.3238 0.074 Uiso 1 1 calc R . . C17 C 0.0897(2) -0.0397(3) 0.0523(2) 0.0555(7) Uani 1 1 d . . . H17A H 0.1512 0.0315 0.0589 0.083 Uiso 1 1 calc R . . H17B H 0.0392 -0.0183 0.0875 0.083 Uiso 1 1 calc R . . H17C H 0.0508 -0.092 -0.0174 0.083 Uiso 1 1 calc R . . C18 C 0.13365(18) -0.1029(2) 0.09559(16) 0.0356(5) Uani 1 1 d . . . H18 H 0.0702 -0.1686 0.0974 0.043 Uiso 1 1 calc R . . C19 C 0.1988(2) -0.1543(3) 0.03095(19) 0.0531(7) Uani 1 1 d . . . H19A H 0.1509 -0.2096 -0.0357 0.08 Uiso 1 1 calc R . . H19B H 0.2256 -0.1955 0.0587 0.08 Uiso 1 1 calc R . . H19C H 0.2613 -0.0905 0.0289 0.08 Uiso 1 1 calc R . . C20 C 0.35998(19) -0.0901(2) 0.27172(19) 0.0425(6) Uani 1 1 d . . . H20A H 0.3741 -0.1332 0.3051 0.064 Uiso 1 1 calc R . . H20B H 0.4177 -0.0086 0.3039 0.064 Uiso 1 1 calc R . . H20C H 0.3596 -0.1275 0.2028 0.064 Uiso 1 1 calc R . . C21 C 0.24729(17) -0.0918(2) 0.27698(17) 0.0317(5) Uani 1 1 d . . . H21 H 0.2524 -0.0523 0.3484 0.038 Uiso 1 1 calc R . . C22 C 0.1572(2) -0.2186(2) 0.2366(2) 0.0497(7) Uani 1 1 d . . . H22A H 0.1514 -0.2626 0.1672 0.074 Uiso 1 1 calc R . . H22B H 0.0868 -0.2182 0.2431 0.074 Uiso 1 1 calc R . . H22C H 0.1757 -0.2561 0.2738 0.074 Uiso 1 1 calc R . . C23 C 0.64393(19) 0.1054(2) 0.48447(18) 0.0426(6) Uani 1 1 d . . . H23A H 0.6051 0.0437 0.5032 0.064 Uiso 1 1 calc R . . H23B H 0.5935 0.1334 0.4662 0.064 Uiso 1 1 calc R . . H23C H 0.706 0.171 0.54 0.064 Uiso 1 1 calc R . . C24 C 0.68690(16) 0.0553(2) 0.39603(16) 0.0301(4) Uani 1 1 d . . . H24 H 0.6213 -0.0143 0.3434 0.036 Uiso 1 1 calc R . . C25 C 0.7639(2) 0.0076(2) 0.4224(2) 0.0467(6) Uani 1 1 d . . . H25A H 0.8276 0.0718 0.4771 0.07 Uiso 1 1 calc R . . H25B H 0.7888 -0.0259 0.3653 0.07 Uiso 1 1 calc R . . H25C H 0.7243 -0.0535 0.4416 0.07 Uiso 1 1 calc R . . C26 C 0.92218(18) 0.3193(2) 0.51000(19) 0.0487(7) Uani 1 1 d . . . H26A H 1.0021 0.3594 0.5377 0.073 Uiso 1 1 calc R . . H26B H 0.8878 0.2715 0.5424 0.073 Uiso 1 1 calc R . . H26C H 0.895 0.3778 0.5204 0.073 Uiso 1 1 calc R . . C29 C 0.59396(18) -0.0088(2) 0.16206(17) 0.0379(5) Uani 1 1 d . . . H29A H 0.5809 -0.0434 0.0906 0.057 Uiso 1 1 calc R . . H29B H 0.5543 0.0384 0.182 0.057 Uiso 1 1 calc R . . H29C H 0.5678 -0.0716 0.182 0.057 Uiso 1 1 calc R . . C27 C 0.89339(15) 0.2397(2) 0.39947(16) 0.0319(5) Uani 1 1 d . . . H27 H 0.9208 0.1799 0.3896 0.038 Uiso 1 1 calc R . . C28 C 0.94890(18) 0.3135(2) 0.3483(2) 0.0493(7) Uani 1 1 d . . . H28A H 0.9194 0.3694 0.3543 0.074 Uiso 1 1 calc R . . H28B H 0.9345 0.2616 0.2786 0.074 Uiso 1 1 calc R . . H28C H 1.0283 0.3567 0.3791 0.074 Uiso 1 1 calc R . . C30 C 0.71799(17) 0.0704(2) 0.21181(15) 0.0315(5) Uani 1 1 d . . . H30 H 0.7423 0.1261 0.1825 0.038 Uiso 1 1 calc R . . C31 C 0.7811(2) -0.0034(3) 0.1838(2) 0.0539(7) Uani 1 1 d . . . H31A H 0.7575 -0.0622 0.2083 0.081 Uiso 1 1 calc R . . H31B H 0.8601 0.0482 0.213 0.081 Uiso 1 1 calc R . . H31C H 0.7657 -0.0432 0.1122 0.081 Uiso 1 1 calc R . . C32 C 0.91195(18) 0.4903(2) 0.21089(18) 0.0428(6) Uani 1 1 d . . . H32A H 0.9193 0.502 0.1523 0.064 Uiso 1 1 calc R . . H32B H 0.8864 0.4068 0.1933 0.064 Uiso 1 1 calc R . . H32C H 0.9833 0.5367 0.2603 0.064 Uiso 1 1 calc R . . C33 C 0.8175(2) 0.7273(2) 0.3336(2) 0.0471(6) Uani 1 1 d . . . H33A H 0.8908 0.7794 0.3799 0.071 Uiso 1 1 calc R . . H33B H 0.7618 0.7337 0.3682 0.071 Uiso 1 1 calc R . . H33C H 0.8109 0.75 0.2811 0.071 Uiso 1 1 calc R . . P1 P 0.34634(4) 0.46516(5) 0.17633(4) 0.02955(12) Uani 1 1 d . . . P2 P 0.22398(4) 0.00123(5) 0.22327(4) 0.02358(10) Uani 1 1 d . . . P3 P 0.74169(4) 0.16256(5) 0.34538(4) 0.02231(10) Uani 1 1 d . . . S1 S 0.62075(4) 0.43489(5) 0.12689(4) 0.02886(11) Uani 1 1 d . . . S2 S 0.41840(4) 0.18324(5) 0.10542(4) 0.02714(10) Uani 1 1 d . . . S3 S 0.50644(4) 0.28592(5) 0.38638(4) 0.02759(11) Uani 1 1 d . . . S4 S 0.75959(4) 0.48025(5) 0.40489(4) 0.02653(10) Uani 1 1 d . . . Cu1 Cu 0.44681(2) 0.36947(2) 0.147655(18) 0.02741(6) Uani 1 1 d . A . Cu2 Cu 0.379908(19) 0.14948(2) 0.236485(19) 0.02616(6) Uani 1 1 d . A . Cu3 Cu 0.667220(19) 0.28402(2) 0.368136(18) 0.02477(5) Uani 1 1 d . A . In1 In 0.793532(11) 0.546460(14) 0.270498(11) 0.02812(4) Uani 1 1 d . A . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0288(10) 0.0281(12) 0.0264(11) 0.0078(9) 0.0102(8) 0.0121(9) C2 0.0321(10) 0.0276(12) 0.0280(11) 0.0104(9) 0.0082(9) 0.0178(9) C3 0.0227(9) 0.0324(12) 0.0257(11) 0.0119(9) 0.0086(8) 0.0142(9) C4 0.0298(10) 0.0236(11) 0.0251(11) 0.0045(9) 0.0081(8) 0.0121(9) C5A 0.056(4) 0.047(4) 0.057(4) 0.037(4) 0.008(3) 0.015(3) C6A 0.036(3) 0.031(3) 0.033(3) 0.015(3) 0.002(3) 0.016(3) C7A 0.043(3) 0.039(3) 0.048(4) 0.020(3) 0.002(3) 0.012(3) C8A 0.068(6) 0.073(6) 0.063(6) 0.022(4) -0.004(4) 0.043(5) C9A 0.036(3) 0.044(3) 0.037(2) 0.016(2) 0.0015(18) 0.018(2) C10A 0.065(4) 0.052(4) 0.029(3) 0.012(3) 0.003(2) 0.023(3) C11A 0.051(4) 0.047(4) 0.041(5) 0.019(3) 0.023(4) 0.033(3) C12A 0.028(2) 0.031(3) 0.025(3) 0.014(2) 0.012(2) 0.019(2) C13A 0.043(3) 0.038(3) 0.048(3) 0.021(3) 0.023(3) 0.023(2) C5B 0.040(5) 0.042(5) 0.050(5) 0.030(4) 0.001(4) 0.011(4) C6B 0.034(5) 0.024(4) 0.037(6) 0.013(4) 0.000(4) 0.015(4) C7B 0.057(6) 0.035(5) 0.045(6) 0.006(4) -0.011(4) 0.013(4) C8B 0.071(7) 0.068(7) 0.050(6) 0.012(5) -0.013(4) 0.027(5) C9B 0.038(4) 0.042(4) 0.038(4) 0.021(3) 0.008(3) 0.019(3) C10B 0.057(7) 0.085(8) 0.056(7) 0.025(6) -0.010(4) 0.052(7) C11B 0.057(7) 0.053(6) 0.049(8) 0.017(5) 0.027(6) 0.038(5) C12B 0.051(6) 0.044(6) 0.044(7) 0.021(5) 0.021(5) 0.026(4) C13B 0.069(6) 0.048(5) 0.092(8) 0.026(5) 0.048(6) 0.023(4) C14 0.0451(13) 0.0419(15) 0.0383(14) 0.0062(12) 0.0173(11) 0.0210(12) C15 0.0269(10) 0.0274(12) 0.0383(13) 0.0141(10) 0.0111(9) 0.0139(9) C16 0.0320(12) 0.0421(16) 0.072(2) 0.0239(15) 0.0260(13) 0.0151(12) C17 0.0637(17) 0.060(2) 0.0338(15) 0.0154(14) -0.0052(12) 0.0293(15) C18 0.0353(11) 0.0274(12) 0.0291(12) 0.0046(10) 0.0015(9) 0.0099(10) C19 0.0627(17) 0.0452(17) 0.0337(15) 0.0019(12) 0.0089(12) 0.0246(14) C20 0.0418(12) 0.0493(16) 0.0509(16) 0.0272(14) 0.0145(11) 0.0295(12) C21 0.0352(11) 0.0298(12) 0.0375(13) 0.0185(11) 0.0135(10) 0.0177(10) C22 0.0487(14) 0.0337(15) 0.075(2) 0.0331(15) 0.0202(14) 0.0181(12) C23 0.0428(13) 0.0547(17) 0.0370(14) 0.0280(13) 0.0182(11) 0.0199(12) C24 0.0288(10) 0.0262(12) 0.0308(12) 0.0152(10) 0.0044(9) 0.0069(9) C25 0.0512(14) 0.0431(16) 0.0580(18) 0.0324(14) 0.0145(13) 0.0238(13) C26 0.0256(11) 0.0482(16) 0.0408(15) 0.0048(13) -0.0026(10) 0.0046(11) C29 0.0462(13) 0.0271(12) 0.0245(12) 0.0038(10) -0.0010(10) 0.0115(10) C27 0.0184(9) 0.0306(12) 0.0375(13) 0.0098(10) 0.0065(9) 0.0082(9) C28 0.0292(11) 0.0441(16) 0.0684(19) 0.0270(15) 0.0203(12) 0.0078(11) C30 0.0392(11) 0.0305(12) 0.0241(11) 0.0091(10) 0.0103(9) 0.0182(10) C31 0.0702(18) 0.0574(19) 0.0381(15) 0.0083(14) 0.0166(13) 0.0459(16) C32 0.0309(11) 0.0522(17) 0.0440(15) 0.0179(13) 0.0153(11) 0.0205(12) C33 0.0596(15) 0.0215(12) 0.0515(16) 0.0152(12) 0.0201(13) 0.0106(12) P1 0.0334(3) 0.0290(3) 0.0297(3) 0.0112(2) 0.0069(2) 0.0199(2) P2 0.0221(2) 0.0203(3) 0.0252(3) 0.0091(2) 0.0060(2) 0.0080(2) P3 0.0209(2) 0.0202(3) 0.0225(3) 0.0077(2) 0.00526(19) 0.0084(2) S1 0.0284(2) 0.0269(3) 0.0317(3) 0.0142(2) 0.0095(2) 0.0118(2) S2 0.0282(2) 0.0254(3) 0.0253(3) 0.0110(2) 0.0072(2) 0.0102(2) S3 0.0201(2) 0.0321(3) 0.0297(3) 0.0169(2) 0.0065(2) 0.0082(2) S4 0.0199(2) 0.0234(3) 0.0317(3) 0.0112(2) 0.0061(2) 0.0069(2) Cu1 0.03049(12) 0.03016(15) 0.02620(14) 0.01180(12) 0.00929(10) 0.01880(11) Cu2 0.02451(12) 0.02266(13) 0.03060(14) 0.01181(11) 0.00983(10) 0.00982(11) Cu3 0.02619(12) 0.02330(14) 0.02419(13) 0.00895(11) 0.00629(10) 0.01258(10) In1 0.02474(7) 0.02321(8) 0.03127(9) 0.01064(7) 0.00977(6) 0.00726(6) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.524(3) . ? C1 S1 1.839(2) . ? C2 S2 1.8490(19) . ? C3 C4 1.530(3) . ? C3 S3 1.842(2) . ? C4 S4 1.8474(18) . ? C5A C6A 1.551(8) . ? C6A C7A 1.543(8) . ? C6A P1 1.805(11) . ? C8A C9A 1.538(9) . ? C9A C10A 1.540(7) . ? C9A P1 1.891(4) . ? C11A C12A 1.524(8) . ? C12A C13A 1.520(7) . ? C12A P1 1.941(8) . ? C5B C6B 1.537(11) . ? C6B C7B 1.542(11) . ? C6B P1 1.955(16) . ? C8B C9B 1.529(11) . ? C9B C10B 1.534(11) . ? C9B P1 1.890(6) . ? C11B C12B 1.550(12) . ? C12B C13B 1.532(11) . ? C12B P1 1.728(14) . ? C14 C15 1.540(3) . ? C15 C16 1.537(3) . ? C15 P2 1.8712(19) . ? C17 C18 1.532(3) . ? C18 C19 1.545(3) . ? C18 P2 1.868(2) . ? C20 C21 1.546(3) . ? C21 C22 1.534(3) . ? C21 P2 1.877(2) . ? C23 C24 1.548(3) . ? C24 C25 1.542(3) . ? C24 P3 1.870(2) . ? C26 C27 1.536(3) . ? C29 C30 1.542(3) . ? C27 C28 1.536(3) . ? C27 P3 1.863(2) . ? C30 C31 1.542(3) . ? C30 P3 1.868(2) . ? C32 In1 2.180(2) . ? C33 In1 2.178(2) . ? P1 Cu1 2.2131(6) . ? P2 Cu2 2.2484(6) . ? P3 Cu3 2.2161(6) . ? S1 Cu1 2.3033(6) . ? S1 In1 2.5551(6) . ? S2 Cu1 2.2591(6) . ? S2 Cu2 2.2922(6) . ? S3 Cu3 2.2549(5) . ? S3 Cu2 2.3068(7) . ? S4 Cu3 2.3119(6) . ? S4 In1 2.5677(6) . ? 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 C2 C1 S1 113.03(13) . . ? C1 C2 S2 112.37(13) . . ? C4 C3 S3 112.87(14) . . ? C3 C4 S4 112.48(14) . . ? C7A C6A C5A 110.3(6) . . ? C7A C6A P1 110.5(7) . . ? C5A C6A P1 108.3(7) . . ? C8A C9A C10A 110.2(7) . . ? C8A C9A P1 118.4(6) . . ? C10A C9A P1 110.6(5) . . ? C13A C12A C11A 113.1(6) . . ? C13A C12A P1 111.5(5) . . ? C11A C12A P1 116.6(7) . . ? C5B C6B C7B 110.2(10) . . ? C5B C6B P1 112.0(10) . . ? C7B C6B P1 109.0(11) . . ? C8B C9B C10B 113.3(11) . . ? C8B C9B P1 108.2(8) . . ? C10B C9B P1 113.1(10) . . ? C13B C12B C11B 107.8(11) . . ? C13B C12B P1 112.2(9) . . ? C11B C12B P1 120.1(12) . . ? C16 C15 C14 110.20(19) . . ? C16 C15 P2 116.27(16) . . ? C14 C15 P2 110.49(13) . . ? C17 C18 C19 110.1(2) . . ? C17 C18 P2 110.22(17) . . ? C19 C18 P2 109.77(16) . . ? C22 C21 C20 110.36(19) . . ? C22 C21 P2 117.03(16) . . ? C20 C21 P2 110.21(15) . . ? C25 C24 C23 110.28(19) . . ? C25 C24 P3 116.61(15) . . ? C23 C24 P3 110.77(16) . . ? C26 C27 C28 109.9(2) . . ? C26 C27 P3 110.09(13) . . ? C28 C27 P3 109.96(16) . . ? C31 C30 C29 110.1(2) . . ? C31 C30 P3 117.33(15) . . ? C29 C30 P3 110.00(14) . . ? C12B P1 C6A 107.1(5) . . ? C12B P1 C9B 115.6(5) . . ? C6A P1 C9B 90.9(4) . . ? C12B P1 C9A 93.3(5) . . ? C6A P1 C9A 108.2(3) . . ? C9B P1 C9A 24.5(2) . . ? C12B P1 C12A 9.5(6) . . ? C6A P1 C12A 102.4(4) . . ? C9B P1 C12A 124.5(4) . . ? C9A P1 C12A 102.7(3) . . ? C12B P1 C6B 105.6(6) . . ? C6A P1 C6B 10.2(6) . . ? C9B P1 C6B 100.5(4) . . ? C9A P1 C6B 118.4(4) . . ? C12A P1 C6B 99.4(5) . . ? C12B P1 Cu1 115.0(5) . . ? C6A P1 Cu1 117.8(3) . . ? C9B P1 Cu1 108.4(2) . . ? C9A P1 Cu1 112.59(13) . . ? C12A P1 Cu1 111.7(2) . . ? C6B P1 Cu1 110.8(5) . . ? C18 P2 C15 104.17(10) . . ? C18 P2 C21 105.94(11) . . ? C15 P2 C21 104.89(9) . . ? C18 P2 Cu2 115.43(8) . . ? C15 P2 Cu2 111.85(7) . . ? C21 P2 Cu2 113.58(7) . . ? C27 P3 C30 105.80(9) . . ? C27 P3 C24 105.64(10) . . ? C30 P3 C24 105.08(10) . . ? C27 P3 Cu3 113.31(8) . . ? C30 P3 Cu3 111.10(7) . . ? C24 P3 Cu3 115.13(6) . . ? C1 S1 Cu1 96.90(6) . . ? C1 S1 In1 101.31(7) . . ? Cu1 S1 In1 122.30(2) . . ? C2 S2 Cu1 97.41(7) . . ? C2 S2 Cu2 106.42(7) . . ? Cu1 S2 Cu2 105.97(2) . . ? C3 S3 Cu3 97.49(6) . . ? C3 S3 Cu2 102.43(7) . . ? Cu3 S3 Cu2 105.44(2) . . ? C4 S4 Cu3 97.52(7) . . ? C4 S4 In1 102.43(7) . . ? Cu3 S4 In1 121.87(2) . . ? P1 Cu1 S2 136.30(2) . . ? P1 Cu1 S1 127.20(2) . . ? S2 Cu1 S1 95.81(2) . . ? P2 Cu2 S2 122.75(2) . . ? P2 Cu2 S3 121.59(2) . . ? S2 Cu2 S3 115.52(2) . . ? P3 Cu3 S3 138.30(2) . . ? P3 Cu3 S4 125.69(2) . . ? S3 Cu3 S4 95.52(2) . . ? C33 In1 C32 124.55(10) . . ? C33 In1 S1 104.03(8) . . ? C32 In1 S1 105.17(7) . . ? C33 In1 S4 106.01(7) . . ? C32 In1 S4 105.85(7) . . ? S1 In1 S4 111.038(18) . . ? _chemical_name_common ; bis(mu!3$-1,2-dithiolatoethane-S,S,S',S')-dimethanido - tris(triisopropylphosphine)-tricopper(+1)-indium(+3) ; data_[(iPr3PCu)3(SC2H4S)2InEt2] _database_code_depnum_ccdc_archive 'CCDC 907028' #TrackingRef '17886_web_deposit_cif_file_0_DirkFriedrich_1361282756.30_[(iPr3PCu)3(SC2H4S)2InEt2].cif' _audit_creation_date 2013-02-19T14:56:06-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; bis(\m~3~-1,2-dithiolatoethane-S,S,S',S')-diethanido -tris(triisopropylphosphine)-tricopper(+1)-indium(+3) ; _chemical_formula_moiety 'C35 H81 Cu3 In1 P3 S4' _chemical_formula_sum 'C35 H81 Cu3 In P3 S4' _chemical_formula_weight 1028.59 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.017(2) _cell_length_b 16.647(2) _cell_length_c 21.653(3) _cell_angle_alpha 97.771(12) _cell_angle_beta 95.500(12) _cell_angle_gamma 96.334(12) _cell_volume 4944.0(13) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 41192 _cell_measurement_theta_min 1.91 _cell_measurement_theta_max 29.25 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description needle _exptl_crystal_colour colorless _exptl_crystal_size_max 0.493 _exptl_crystal_size_mid 0.106 _exptl_crystal_size_min 0.075 _exptl_crystal_density_diffrn 1.382 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2144 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 2.01 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details ; Busing, W. R. & Levy, H. A. (1957) Acta Cryst. 10, 180-182. and Coppens, P., Leiserowitz, L. & Rabinovich, D. (1965) Acta Cryst. 1965, 1035-1038. ; _exptl_absorpt_correction_T_min 0.5522 _exptl_absorpt_correction_T_max 0.8629 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 180(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 '2-circle goniometer' _diffrn_measurement_device_type 'STOE IPDS-2T' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 6.67 _diffrn_detector 'image plate (34 cm diameter / schwenk)' _diffrn_detector_type STOE _diffrn_standards_number 0 _diffrn_reflns_av_R_equivalents 0.0742 _diffrn_reflns_av_unetI/netI 0.0766 _diffrn_reflns_number 80494 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.91 _diffrn_reflns_theta_max 26.78 _diffrn_reflns_theta_full 26.78 _diffrn_measured_fraction_theta_full 0.977 _diffrn_measured_fraction_theta_max 0.977 _reflns_number_total 20644 _reflns_number_gt 13048 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_cell_refinement 'STOE X-AREA' _computing_data_reduction 'STOE X-AREA, STOE X-RED' _computing_structure_solution ; 'SIR-92' Altomare, A., Cascarano, G., Giacovazzo, C. & Guagliardi, A. (1993) J. Appl. Cryst. 26, 343-350. ; _computing_structure_refinement ; 'SHELXL-97' Sheldrick, G.M. (2008) Acta Cryst. A64, 112 ; _computing_molecular_graphics 'DIAMOND 3.2' _computing_publication_material ; 'WinGX publication routines' Farrugia, L. J. (1999) WinGX, J. Appl. Cryst. 32, 837-838 ; #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0148P)^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 mixed _refine_ls_extinction_method none _refine_ls_number_reflns 20644 _refine_ls_number_parameters 869 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0675 _refine_ls_R_factor_gt 0.0315 _refine_ls_wR_factor_ref 0.0542 _refine_ls_wR_factor_gt 0.0489 _refine_ls_goodness_of_fit_ref 0.782 _refine_ls_restrained_S_all 0.782 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.736 _refine_diff_density_min -0.631 _refine_diff_density_rms 0.074 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' In In -0.7276 1.31 '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' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.2432(2) 0.6942(2) 0.64588(15) 0.0283(7) Uani 1 1 d . . . H1A H 0.2231 0.6586 0.6766 0.034 Uiso 1 1 calc R . . H1B H 0.3098 0.6853 0.6378 0.034 Uiso 1 1 calc R . . C2 C 0.2431(2) 0.7830(2) 0.67427(15) 0.0274(7) Uani 1 1 d . . . H2A H 0.267 0.8189 0.6447 0.033 Uiso 1 1 calc R . . H2B H 0.2881 0.7951 0.7134 0.033 Uiso 1 1 calc R . . C3 C 0.1272(2) 0.9046(2) 0.52862(15) 0.0300(8) Uani 1 1 d . . . H3A H 0.1127 0.8519 0.5441 0.036 Uiso 1 1 calc R . . H3B H 0.0651 0.9219 0.5129 0.036 Uiso 1 1 calc R . . C4 C 0.1888(2) 0.8925(2) 0.47470(15) 0.0313(8) Uani 1 1 d . . . H4A H 0.1976 0.9438 0.4564 0.038 Uiso 1 1 calc R . . H4B H 0.1541 0.8495 0.4417 0.038 Uiso 1 1 calc R . . C5 C -0.1306(3) 0.5477(2) 0.5456(2) 0.0661(13) Uani 1 1 d . . . H5A H -0.1432 0.4952 0.5179 0.099 Uiso 1 1 calc R . . H5B H -0.1762 0.549 0.5772 0.099 Uiso 1 1 calc R . . H5C H -0.0644 0.5547 0.5665 0.099 Uiso 1 1 calc R . . C6 C -0.1433(2) 0.6179(2) 0.50633(17) 0.0427(9) Uani 1 1 d . . . H6 H -0.2122 0.6128 0.4878 0.051 Uiso 1 1 calc R . . C7 C -0.0790(3) 0.6118(3) 0.45332(19) 0.0625(13) Uani 1 1 d . . . H7A H -0.0112 0.6178 0.4711 0.094 Uiso 1 1 calc R . . H7B H -0.0888 0.6552 0.4279 0.094 Uiso 1 1 calc R . . H7C H -0.0957 0.5584 0.427 0.094 Uiso 1 1 calc R . . C8 C -0.3089(3) 0.6856(3) 0.5878(2) 0.0656(13) Uani 1 1 d . . . H8A H -0.3101 0.6261 0.5795 0.098 Uiso 1 1 calc R . . H8B H -0.3296 0.7058 0.5488 0.098 Uiso 1 1 calc R . . H8C H -0.3528 0.6995 0.6191 0.098 Uiso 1 1 calc R . . C9 C -0.2052(2) 0.7255(2) 0.61284(17) 0.0390(8) Uani 1 1 d . . . H9 H -0.2097 0.7851 0.6242 0.047 Uiso 1 1 calc R . . C10 C -0.1710(3) 0.6954(3) 0.67477(18) 0.0577(12) Uani 1 1 d . . . H10A H -0.2136 0.7109 0.7065 0.087 Uiso 1 1 calc R . . H10B H -0.1047 0.7204 0.6895 0.087 Uiso 1 1 calc R . . H10C H -0.173 0.6358 0.6676 0.087 Uiso 1 1 calc R . . C11 C -0.2264(3) 0.7805(3) 0.4580(2) 0.0653(14) Uani 1 1 d . . . H11A H -0.2833 0.7794 0.481 0.098 Uiso 1 1 calc R . . H11B H -0.2275 0.7277 0.4315 0.098 Uiso 1 1 calc R . . H11C H -0.227 0.8239 0.4316 0.098 Uiso 1 1 calc R . . C12 C -0.1336(2) 0.7970(2) 0.50517(17) 0.0369(8) Uani 1 1 d . . . H12 H -0.0784 0.7993 0.4792 0.044 Uiso 1 1 calc R . . C13 C -0.1267(3) 0.8817(2) 0.5440(2) 0.0530(11) Uani 1 1 d . . . H13A H -0.1222 0.9235 0.5162 0.079 Uiso 1 1 calc R . . H13B H -0.0692 0.8904 0.5747 0.079 Uiso 1 1 calc R . . H13C H -0.1844 0.8856 0.5659 0.079 Uiso 1 1 calc R . . C14 C -0.0967(3) 0.9070(3) 0.7580(3) 0.0843(18) Uani 1 1 d . . . H14A H -0.0704 0.9031 0.8009 0.126 Uiso 1 1 calc R . . H14B H -0.0644 0.8727 0.7282 0.126 Uiso 1 1 calc R . . H14C H -0.1662 0.8882 0.7522 0.126 Uiso 1 1 calc R . . C15 C -0.0796(2) 0.9975(3) 0.74619(18) 0.0501(11) Uani 1 1 d . . . H15 H -0.1107 0.9986 0.7028 0.06 Uiso 1 1 calc R . . C16 C -0.1328(3) 1.0524(4) 0.7909(2) 0.0826(18) Uani 1 1 d . . . H16A H -0.2025 1.0352 0.7825 0.124 Uiso 1 1 calc R . . H16B H -0.1189 1.1094 0.7841 0.124 Uiso 1 1 calc R . . H16C H -0.1108 1.0476 0.8344 0.124 Uiso 1 1 calc R . . C17 C 0.0978(3) 1.1166(3) 0.87221(19) 0.0622(13) Uani 1 1 d . . . H17A H 0.1174 1.1104 0.9158 0.093 Uiso 1 1 calc R . . H17B H 0.0311 1.1292 0.8681 0.093 Uiso 1 1 calc R . . H17C H 0.1405 1.1612 0.8602 0.093 Uiso 1 1 calc R . . C18 C 0.1050(2) 1.0364(2) 0.82896(16) 0.0388(9) Uani 1 1 d . . . H18 H 0.0675 0.9921 0.8468 0.047 Uiso 1 1 calc R . . C19 C 0.2096(3) 1.0169(3) 0.83282(19) 0.0494(10) Uani 1 1 d . . . H19A H 0.2505 1.0602 0.8179 0.074 Uiso 1 1 calc R . . H19B H 0.2124 0.9646 0.8066 0.074 Uiso 1 1 calc R . . H19C H 0.2327 1.0133 0.8764 0.074 Uiso 1 1 calc R . . C20 C -0.0011(3) 1.1367(3) 0.6633(2) 0.0658(13) Uani 1 1 d . . . H20A H 0.0076 1.1921 0.6524 0.099 Uiso 1 1 calc R . . H20B H -0.0695 1.1209 0.6672 0.099 Uiso 1 1 calc R . . H20C H 0.0199 1.0985 0.6303 0.099 Uiso 1 1 calc R . . C21 C 0.0599(3) 1.1345(2) 0.72652(18) 0.0443(9) Uani 1 1 d . . . H21 H 0.0337 1.1697 0.7604 0.053 Uiso 1 1 calc R . . C22 C 0.1656(3) 1.1676(3) 0.7241(2) 0.0603(12) Uani 1 1 d . . . H22A H 0.1933 1.1317 0.6928 0.09 Uiso 1 1 calc R . . H22B H 0.202 1.1697 0.7654 0.09 Uiso 1 1 calc R . . H22C H 0.1691 1.2227 0.7125 0.09 Uiso 1 1 calc R . . C23 C 0.4472(3) 1.1535(3) 0.6346(2) 0.0551(11) Uani 1 1 d . . . H23A H 0.4346 1.2074 0.6541 0.083 Uiso 1 1 calc R . . H23B H 0.3891 1.1259 0.6081 0.083 Uiso 1 1 calc R . . H23C H 0.5006 1.1599 0.6089 0.083 Uiso 1 1 calc R . . C24 C 0.4746(2) 1.1014(2) 0.68685(15) 0.0352(8) Uani 1 1 d . . . H24 H 0.4202 1.1005 0.7136 0.042 Uiso 1 1 calc R . . C25 C 0.5649(3) 1.1449(3) 0.72992(19) 0.0572(11) Uani 1 1 d . . . H25A H 0.6188 1.1532 0.7048 0.086 Uiso 1 1 calc R . . H25B H 0.5823 1.1111 0.762 0.086 Uiso 1 1 calc R . . H25C H 0.551 1.1979 0.7502 0.086 Uiso 1 1 calc R . . C26 C 0.6840(2) 0.9962(3) 0.65065(17) 0.0472(10) Uani 1 1 d . . . H26A H 0.6842 0.9436 0.6663 0.071 Uiso 1 1 calc R . . H26B H 0.6906 1.0404 0.6862 0.071 Uiso 1 1 calc R . . H26C H 0.738 1.0043 0.6257 0.071 Uiso 1 1 calc R . . C27 C 0.5882(2) 0.9964(2) 0.60942(14) 0.0318(7) Uani 1 1 d . . . H27 H 0.5936 1.0493 0.5922 0.038 Uiso 1 1 calc R . . C28 C 0.5778(2) 0.9285(2) 0.55252(16) 0.0423(9) Uani 1 1 d . . . H28A H 0.634 0.9355 0.5292 0.063 Uiso 1 1 calc R . . H28B H 0.5189 0.9317 0.5251 0.063 Uiso 1 1 calc R . . H28C H 0.5738 0.8751 0.567 0.063 Uiso 1 1 calc R . . C29 C 0.5063(2) 0.8466(2) 0.69449(17) 0.0399(9) Uani 1 1 d . . . H29A H 0.5078 0.8153 0.7297 0.06 Uiso 1 1 calc R . . H29B H 0.5638 0.8404 0.6727 0.06 Uiso 1 1 calc R . . H29C H 0.4482 0.8264 0.6652 0.06 Uiso 1 1 calc R . . C30 C 0.5046(2) 0.9373(2) 0.71930(14) 0.0301(7) Uani 1 1 d . . . H30 H 0.57 0.9603 0.7412 0.036 Uiso 1 1 calc R . . C31 C 0.4297(2) 0.9491(3) 0.76598(16) 0.0433(9) Uani 1 1 d . . . H31A H 0.3646 0.9392 0.7432 0.065 Uiso 1 1 calc R . . H31B H 0.4412 1.0051 0.7884 0.065 Uiso 1 1 calc R . . H31C H 0.4354 0.9106 0.7962 0.065 Uiso 1 1 calc R . . C32 C 0.4141(3) 0.5816(3) 0.5207(2) 0.0690(14) Uani 1 1 d . . . H32A H 0.372 0.5648 0.5515 0.103 Uiso 1 1 calc R . . H32B H 0.4801 0.5707 0.5329 0.103 Uiso 1 1 calc R . . H32C H 0.3905 0.5508 0.4793 0.103 Uiso 1 1 calc R . . C33 C 0.4140(3) 0.6724(3) 0.5185(2) 0.0515(11) Uani 1 1 d . . . H33A H 0.4587 0.689 0.4885 0.062 Uiso 1 1 calc R . . H33B H 0.4391 0.7029 0.5604 0.062 Uiso 1 1 calc R . . C34 C 0.2330(4) 0.7169(3) 0.34785(18) 0.0799(16) Uani 1 1 d . . . H34A H 0.2261 0.7752 0.3548 0.12 Uiso 1 1 calc R . . H34B H 0.2007 0.6923 0.3064 0.12 Uiso 1 1 calc R . . H34C H 0.3017 0.7098 0.3501 0.12 Uiso 1 1 calc R . . C35 C 0.1871(4) 0.6753(3) 0.39786(18) 0.0666(14) Uani 1 1 d . . . H35A H 0.181 0.6153 0.3855 0.08 Uiso 1 1 calc R . . H35B H 0.1212 0.6909 0.4005 0.08 Uiso 1 1 calc R . . C36 C 0.7556(2) 0.2014(2) 0.14459(14) 0.0266(7) Uani 1 1 d . . . H36A H 0.734 0.1645 0.1741 0.032 Uiso 1 1 calc R . . H36B H 0.8238 0.1951 0.1392 0.032 Uiso 1 1 calc R . . C37 C 0.74923(19) 0.2894(2) 0.17280(14) 0.0246(7) Uani 1 1 d . . . H37A H 0.7739 0.3266 0.1443 0.029 Uiso 1 1 calc R . . H37B H 0.7909 0.3026 0.2133 0.029 Uiso 1 1 calc R . . C38 C 0.6403(2) 0.4117(2) 0.02679(15) 0.0318(8) Uani 1 1 d . . . H38A H 0.6254 0.3579 0.0407 0.038 Uiso 1 1 calc R . . H38B H 0.5795 0.4268 0.0069 0.038 Uiso 1 1 calc R . . C39 C 0.7123(2) 0.4043(2) -0.02173(15) 0.0346(8) Uani 1 1 d . . . H39A H 0.7234 0.457 -0.038 0.042 Uiso 1 1 calc R . . H39B H 0.684 0.3622 -0.0574 0.042 Uiso 1 1 calc R . . C40 C 0.4136(3) 0.0672(2) -0.0165(2) 0.0632(12) Uani 1 1 d . . . H40A H 0.4063 0.0281 -0.0553 0.095 Uiso 1 1 calc R . . H40B H 0.3727 0.0458 0.0133 0.095 Uiso 1 1 calc R . . H40C H 0.4813 0.0754 0.0018 0.095 Uiso 1 1 calc R . . C41 C 0.3834(2) 0.1487(2) -0.03110(16) 0.0352(8) Uani 1 1 d . . . H41 H 0.3129 0.1405 -0.0464 0.042 Uiso 1 1 calc R . . C42 C 0.4398(3) 0.1788(3) -0.08249(19) 0.0612(12) Uani 1 1 d . . . H42A H 0.5082 0.1927 -0.0664 0.092 Uiso 1 1 calc R . . H42B H 0.4143 0.2273 -0.0952 0.092 Uiso 1 1 calc R . . H42C H 0.4329 0.1357 -0.1188 0.092 Uiso 1 1 calc R . . C43 C 0.2151(3) 0.1479(3) 0.06098(19) 0.0626(13) Uani 1 1 d . . . H43A H 0.2275 0.0931 0.0435 0.094 Uiso 1 1 calc R . . H43B H 0.1879 0.1751 0.0272 0.094 Uiso 1 1 calc R . . H43C H 0.1691 0.1435 0.0921 0.094 Uiso 1 1 calc R . . C44 C 0.3107(2) 0.1981(3) 0.09270(17) 0.0436(9) Uani 1 1 d . . . H44 H 0.2927 0.2511 0.1129 0.052 Uiso 1 1 calc R . . C45 C 0.3522(3) 0.1563(3) 0.14651(19) 0.0605(13) Uani 1 1 d . . . H45A H 0.3029 0.1469 0.1748 0.091 Uiso 1 1 calc R . . H45B H 0.4085 0.1914 0.1698 0.091 Uiso 1 1 calc R . . H45C H 0.3717 0.1039 0.1293 0.091 Uiso 1 1 calc R . . C46 C 0.2682(2) 0.3124(2) -0.0240(2) 0.0493(10) Uani 1 1 d . . . H46A H 0.22 0.3011 0.0046 0.074 Uiso 1 1 calc R . . H46B H 0.261 0.2677 -0.0592 0.074 Uiso 1 1 calc R . . H46C H 0.2587 0.3637 -0.04 0.074 Uiso 1 1 calc R . . C47 C 0.3706(2) 0.3202(2) 0.01149(17) 0.0363(8) Uani 1 1 d . . . H47 H 0.4169 0.3331 -0.0192 0.044 Uiso 1 1 calc R . . C48 C 0.3860(2) 0.3932(2) 0.06450(19) 0.0442(9) Uani 1 1 d . . . H48A H 0.3809 0.4438 0.0466 0.066 Uiso 1 1 calc R . . H48B H 0.4503 0.3959 0.0875 0.066 Uiso 1 1 calc R . . H48C H 0.3367 0.3865 0.0932 0.066 Uiso 1 1 calc R . . C49 C 0.4015(3) 0.3779(3) 0.2464(2) 0.0582(12) Uani 1 1 d . . . H49A H 0.4337 0.3707 0.2872 0.087 Uiso 1 1 calc R . . H49B H 0.4343 0.3512 0.2128 0.087 Uiso 1 1 calc R . . H49C H 0.3339 0.3534 0.2422 0.087 Uiso 1 1 calc R . . C50 C 0.4058(2) 0.4699(2) 0.24193(18) 0.0389(9) Uani 1 1 d . . . H50 H 0.3738 0.4735 0.1993 0.047 Uiso 1 1 calc R . . C51 C 0.3447(3) 0.5128(3) 0.2889(2) 0.0613(12) Uani 1 1 d . . . H51A H 0.2769 0.4888 0.2794 0.092 Uiso 1 1 calc R . . H51B H 0.35 0.5712 0.2856 0.092 Uiso 1 1 calc R . . H51C H 0.3684 0.5057 0.3317 0.092 Uiso 1 1 calc R . . C52 C 0.5657(3) 0.5966(3) 0.37353(17) 0.0483(10) Uani 1 1 d . . . H52A H 0.5898 0.5905 0.4164 0.072 Uiso 1 1 calc R . . H52B H 0.4958 0.5989 0.3707 0.072 Uiso 1 1 calc R . . H52C H 0.5981 0.6472 0.3626 0.072 Uiso 1 1 calc R . . C53 C 0.5866(2) 0.5231(2) 0.32772(15) 0.0348(8) Uani 1 1 d . . . H53 H 0.5564 0.4734 0.3431 0.042 Uiso 1 1 calc R . . C54 C 0.6951(3) 0.5164(3) 0.33162(18) 0.0476(10) Uani 1 1 d . . . H54A H 0.7291 0.5658 0.32 0.071 Uiso 1 1 calc R . . H54B H 0.7063 0.4686 0.3028 0.071 Uiso 1 1 calc R . . H54C H 0.7192 0.5106 0.3746 0.071 Uiso 1 1 calc R . . C55 C 0.4617(3) 0.6218(3) 0.16614(19) 0.0500(10) Uani 1 1 d . . . H55A H 0.4603 0.6779 0.1574 0.075 Uiso 1 1 calc R . . H55B H 0.3958 0.5966 0.1683 0.075 Uiso 1 1 calc R . . H55C H 0.49 0.5902 0.1326 0.075 Uiso 1 1 calc R . . C56 C 0.5235(2) 0.6227(2) 0.22949(16) 0.0336(8) Uani 1 1 d . . . H56 H 0.4915 0.6512 0.264 0.04 Uiso 1 1 calc R . . C57 C 0.6246(3) 0.6688(2) 0.22833(19) 0.0460(9) Uani 1 1 d . . . H57A H 0.6557 0.6418 0.194 0.069 Uiso 1 1 calc R . . H57B H 0.6639 0.6686 0.2683 0.069 Uiso 1 1 calc R . . H57C H 0.6187 0.7253 0.222 0.069 Uiso 1 1 calc R . . C58 C 1.1373(3) 0.6292(3) 0.1671(2) 0.0700(15) Uani 1 1 d . . . H58A H 1.1706 0.666 0.1421 0.105 Uiso 1 1 calc R . . H58B H 1.1794 0.5888 0.1781 0.105 Uiso 1 1 calc R . . H58C H 1.1215 0.6608 0.2055 0.105 Uiso 1 1 calc R . . C59 C 1.0428(2) 0.5844(2) 0.12822(16) 0.0410(9) Uani 1 1 d . . . H59 H 1.0632 0.5577 0.0883 0.049 Uiso 1 1 calc R . . C60 C 0.9749(3) 0.6445(3) 0.1087(2) 0.0605(12) Uani 1 1 d . . . H60A H 0.9576 0.6771 0.1462 0.091 Uiso 1 1 calc R . . H60B H 0.9163 0.6143 0.0844 0.091 Uiso 1 1 calc R . . H60C H 1.0073 0.6808 0.083 0.091 Uiso 1 1 calc R . . C61 C 1.1087(5) 0.4078(4) 0.0993(3) 0.121(3) Uani 1 1 d . . . H61A H 1.1334 0.3547 0.0936 0.181 Uiso 1 1 calc R . . H61B H 1.1613 0.4514 0.0983 0.181 Uiso 1 1 calc R . . H61C H 1.0574 0.4091 0.0655 0.181 Uiso 1 1 calc R . . C62 C 1.0675(3) 0.4206(3) 0.1635(2) 0.0566(11) Uani 1 1 d . . . H62 H 1.1219 0.4396 0.1975 0.068 Uiso 1 1 calc R . . C63 C 1.0159(4) 0.3368(3) 0.1743(3) 0.0746(14) Uani 1 1 d . . . H63A H 0.9684 0.3146 0.1381 0.112 Uiso 1 1 calc R . . H63B H 0.9832 0.3443 0.2123 0.112 Uiso 1 1 calc R . . H63C H 1.0638 0.2988 0.1792 0.112 Uiso 1 1 calc R . . C64 C 0.9435(4) 0.4714(3) 0.2848(2) 0.0711(14) Uani 1 1 d . . . H64A H 0.9356 0.4953 0.3276 0.107 Uiso 1 1 calc R . . H64B H 0.988 0.4301 0.2862 0.107 Uiso 1 1 calc R . . H64C H 0.8806 0.4457 0.2633 0.107 Uiso 1 1 calc R . . C65 C 0.9844(3) 0.5387(3) 0.24919(16) 0.0458(9) Uani 1 1 d . . . H65 H 1.0531 0.5573 0.2667 0.055 Uiso 1 1 calc R . . C66 C 0.9261(4) 0.6115(3) 0.2586(2) 0.0679(13) Uani 1 1 d . . . H66A H 0.8623 0.5972 0.2343 0.102 Uiso 1 1 calc R . . H66B H 0.9604 0.6589 0.2442 0.102 Uiso 1 1 calc R . . H66C H 0.9184 0.6249 0.3031 0.102 Uiso 1 1 calc R . . C67 C 0.9289(3) 0.0887(3) 0.0235(3) 0.0814(17) Uani 1 1 d . . . H67A H 0.8816 0.0738 0.0518 0.122 Uiso 1 1 calc R . . H67B H 0.9921 0.0745 0.0387 0.122 Uiso 1 1 calc R . . H67C H 0.9081 0.059 -0.0187 0.122 Uiso 1 1 calc R . . C68 C 0.9362(2) 0.1785(3) 0.0215(2) 0.0455(10) Uani 1 1 d . . . H68A H 0.9825 0.1926 -0.0083 0.055 Uiso 1 1 calc R . . H68B H 0.9626 0.2079 0.0636 0.055 Uiso 1 1 calc R . . C69 C 0.6773(3) 0.0866(2) -0.10535(17) 0.0448(9) Uani 1 1 d . . . H69A H 0.7301 0.0536 -0.0991 0.067 Uiso 1 1 calc R . . H69B H 0.6418 0.0685 -0.1471 0.067 Uiso 1 1 calc R . . H69C H 0.6333 0.0802 -0.0733 0.067 Uiso 1 1 calc R . . C70 C 0.7191(2) 0.1776(2) -0.09994(15) 0.0342(8) Uani 1 1 d . . . H70A H 0.6659 0.2108 -0.1072 0.041 Uiso 1 1 calc R . . H70B H 0.7633 0.1842 -0.1325 0.041 Uiso 1 1 calc R . . Cu1 Cu 0.03862(3) 0.73776(2) 0.602925(18) 0.02681(9) Uani 1 1 d . . . Cu2 Cu 0.11883(3) 0.94085(3) 0.679160(18) 0.02604(9) Uani 1 1 d . . . Cu3 Cu 0.33812(2) 0.94627(2) 0.594247(18) 0.02638(9) Uani 1 1 d . . . Cu4 Cu 0.55274(2) 0.24054(2) 0.091173(18) 0.02649(9) Uani 1 1 d . . . Cu5 Cu 0.61459(3) 0.44155(2) 0.176748(18) 0.02631(9) Uani 1 1 d . . . Cu6 Cu 0.83896(3) 0.45743(3) 0.107571(19) 0.03069(10) Uani 1 1 d . . . In1 In 0.271021(17) 0.708032(16) 0.490792(11) 0.03175(6) Uani 1 1 d . . . In2 In 0.798239(15) 0.220983(15) -0.006465(10) 0.02727(6) Uani 1 1 d . . . P1 P -0.11189(5) 0.71862(5) 0.55732(4) 0.02561(18) Uani 1 1 d . . . P2 P 0.05190(6) 1.02831(6) 0.74514(4) 0.02833(19) Uani 1 1 d . . . P3 P 0.47771(5) 0.99353(5) 0.65180(4) 0.02467(18) Uani 1 1 d . . . P4 P 0.40434(5) 0.22541(5) 0.04130(4) 0.02523(18) Uani 1 1 d . . . P5 P 0.53384(5) 0.51596(5) 0.24372(4) 0.02583(18) Uani 1 1 d . . . P6 P 0.98050(6) 0.49978(6) 0.16350(4) 0.0298(2) Uani 1 1 d . . . S1 S 0.16232(5) 0.66445(5) 0.57222(4) 0.02885(18) Uani 1 1 d . . . S2 S 0.12192(5) 0.80657(5) 0.69195(4) 0.02651(18) Uani 1 1 d . . . S3 S 0.18667(5) 0.98167(5) 0.59439(4) 0.02730(18) Uani 1 1 d . . . S4 S 0.30873(5) 0.86347(5) 0.49869(4) 0.02885(18) Uani 1 1 d . . . S5 S 0.68153(5) 0.17041(5) 0.06805(4) 0.02635(17) Uani 1 1 d . . . S6 S 0.62436(5) 0.30674(5) 0.18566(4) 0.02482(17) Uani 1 1 d . . . S7 S 0.68671(5) 0.48902(5) 0.09615(4) 0.03000(19) Uani 1 1 d . . . S8 S 0.82911(6) 0.37721(5) 0.01006(4) 0.02994(18) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0326(16) 0.029(2) 0.0259(17) 0.0092(14) 0.0019(13) 0.0085(14) C2 0.0287(15) 0.0281(19) 0.0244(17) 0.0059(14) -0.0014(12) -0.0002(14) C3 0.0286(15) 0.030(2) 0.0299(18) 0.0067(15) -0.0030(13) 0.0017(14) C4 0.0412(17) 0.029(2) 0.0239(17) 0.0069(14) -0.0025(14) 0.0079(15) C5 0.080(3) 0.025(2) 0.087(3) -0.002(2) -0.009(3) 0.006(2) C6 0.0394(18) 0.037(2) 0.044(2) -0.0100(17) -0.0091(16) 0.0027(16) C7 0.055(2) 0.072(3) 0.049(3) -0.029(2) -0.0044(19) 0.014(2) C8 0.037(2) 0.096(4) 0.069(3) 0.028(3) 0.012(2) 0.002(2) C9 0.0369(17) 0.040(2) 0.042(2) 0.0091(17) 0.0151(15) 0.0008(15) C10 0.060(2) 0.071(3) 0.040(2) 0.018(2) 0.0113(19) -0.015(2) C11 0.051(2) 0.079(4) 0.073(3) 0.046(3) -0.009(2) 0.009(2) C12 0.0293(16) 0.044(2) 0.041(2) 0.0180(17) 0.0027(14) 0.0069(15) C13 0.048(2) 0.037(2) 0.084(3) 0.026(2) 0.019(2) 0.0149(18) C14 0.049(2) 0.097(5) 0.096(4) -0.008(3) 0.027(3) -0.028(3) C15 0.0320(18) 0.071(3) 0.041(2) -0.012(2) 0.0046(16) 0.0014(19) C16 0.035(2) 0.144(5) 0.058(3) -0.034(3) 0.0080(19) 0.023(3) C17 0.057(2) 0.085(4) 0.037(2) -0.024(2) -0.0098(18) 0.026(2) C18 0.0405(18) 0.046(2) 0.0277(18) -0.0011(16) -0.0031(14) 0.0075(17) C19 0.051(2) 0.045(3) 0.049(2) 0.0028(19) -0.0134(18) 0.0153(19) C20 0.085(3) 0.058(3) 0.057(3) 0.009(2) -0.013(2) 0.033(2) C21 0.054(2) 0.035(2) 0.044(2) -0.0014(17) -0.0038(17) 0.0230(18) C22 0.079(3) 0.034(2) 0.066(3) 0.013(2) 0.000(2) -0.003(2) C23 0.073(3) 0.035(2) 0.055(3) 0.0030(19) -0.013(2) 0.019(2) C24 0.0451(18) 0.0267(19) 0.0315(18) -0.0012(14) -0.0041(15) 0.0086(15) C25 0.076(3) 0.035(2) 0.051(2) -0.0044(18) -0.020(2) -0.002(2) C26 0.0246(16) 0.074(3) 0.043(2) 0.014(2) 0.0016(15) 0.0006(17) C27 0.0290(15) 0.041(2) 0.0268(17) 0.0101(14) 0.0066(13) -0.0012(14) C28 0.0374(18) 0.056(3) 0.035(2) 0.0014(17) 0.0117(15) 0.0111(17) C29 0.0421(18) 0.040(2) 0.040(2) 0.0175(17) 0.0011(16) 0.0041(16) C30 0.0310(15) 0.037(2) 0.0231(16) 0.0094(14) -0.0003(12) 0.0030(14) C31 0.049(2) 0.053(3) 0.0266(18) 0.0069(17) 0.0099(15) -0.0020(18) C32 0.077(3) 0.059(3) 0.085(4) 0.027(3) 0.029(3) 0.038(3) C33 0.048(2) 0.052(3) 0.061(3) 0.006(2) 0.0213(19) 0.0224(19) C34 0.152(5) 0.059(3) 0.024(2) -0.002(2) 0.006(3) 0.005(3) C35 0.103(3) 0.052(3) 0.033(2) 0.001(2) -0.008(2) -0.018(3) C36 0.0264(15) 0.030(2) 0.0242(16) 0.0068(14) -0.0016(12) 0.0070(13) C37 0.0234(14) 0.0280(19) 0.0221(16) 0.0076(13) -0.0003(12) 0.0002(13) C38 0.0296(16) 0.030(2) 0.0365(19) 0.0088(15) 0.0048(14) 0.0027(14) C39 0.0467(19) 0.035(2) 0.0254(17) 0.0089(15) 0.0073(14) 0.0096(16) C40 0.058(2) 0.031(2) 0.091(3) -0.011(2) -0.020(2) 0.0136(19) C41 0.0349(17) 0.031(2) 0.0364(19) -0.0022(15) -0.0050(14) 0.0059(14) C42 0.056(2) 0.086(4) 0.041(2) -0.005(2) 0.0144(19) 0.019(2) C43 0.039(2) 0.094(4) 0.052(3) 0.027(2) -0.0001(18) -0.019(2) C44 0.0346(17) 0.059(3) 0.038(2) 0.0188(18) 0.0038(15) -0.0049(17) C45 0.059(2) 0.070(3) 0.048(2) 0.033(2) -0.0112(19) -0.024(2) C46 0.046(2) 0.033(2) 0.064(3) 0.0106(19) -0.0230(18) 0.0075(17) C47 0.0343(17) 0.028(2) 0.047(2) 0.0091(16) -0.0037(15) 0.0066(14) C48 0.0367(18) 0.029(2) 0.064(3) 0.0001(18) -0.0041(17) 0.0070(16) C49 0.055(2) 0.040(3) 0.078(3) -0.001(2) 0.031(2) -0.0112(19) C50 0.0338(17) 0.035(2) 0.046(2) -0.0019(17) 0.0145(15) -0.0003(15) C51 0.040(2) 0.056(3) 0.084(3) -0.012(2) 0.026(2) 0.0003(19) C52 0.065(2) 0.050(3) 0.029(2) -0.0029(17) 0.0084(17) 0.010(2) C53 0.0482(19) 0.029(2) 0.0297(18) 0.0085(15) 0.0075(15) 0.0076(16) C54 0.054(2) 0.052(3) 0.037(2) 0.0081(19) -0.0020(17) 0.0141(19) C55 0.066(2) 0.039(2) 0.046(2) 0.0129(19) -0.0042(19) 0.0112(19) C56 0.0384(17) 0.027(2) 0.0351(19) 0.0023(15) 0.0034(14) 0.0053(15) C57 0.056(2) 0.027(2) 0.055(2) 0.0099(18) 0.0059(19) -0.0004(17) C58 0.064(3) 0.083(4) 0.052(3) 0.016(2) -0.002(2) -0.039(2) C59 0.0388(18) 0.051(2) 0.0289(18) 0.0075(16) 0.0029(14) -0.0117(17) C60 0.068(3) 0.053(3) 0.069(3) 0.030(2) 0.020(2) 0.005(2) C61 0.129(5) 0.080(4) 0.183(7) 0.027(4) 0.120(5) 0.042(4) C62 0.039(2) 0.055(3) 0.072(3) -0.007(2) 0.0029(19) 0.0109(19) C63 0.089(3) 0.055(3) 0.081(4) 0.013(3) -0.001(3) 0.024(3) C64 0.105(4) 0.065(3) 0.058(3) 0.027(3) 0.042(3) 0.025(3) C65 0.052(2) 0.054(3) 0.031(2) 0.0066(17) 0.0082(16) -0.0014(19) C66 0.115(4) 0.049(3) 0.044(2) -0.002(2) 0.040(2) 0.012(3) C67 0.057(3) 0.059(4) 0.138(5) 0.034(3) 0.005(3) 0.032(2) C68 0.0344(18) 0.049(3) 0.055(2) 0.007(2) 0.0046(16) 0.0131(17) C69 0.059(2) 0.037(2) 0.0341(19) 0.0022(16) -0.0009(17) -0.0030(18) C70 0.0449(18) 0.033(2) 0.0226(17) 0.0004(14) 0.0039(14) 0.0001(15) Cu1 0.02669(18) 0.0259(2) 0.0271(2) 0.00670(17) -0.00184(15) 0.00075(16) Cu2 0.02745(18) 0.0259(2) 0.0242(2) 0.00130(16) 0.00256(15) 0.00406(16) Cu3 0.02631(18) 0.0280(2) 0.0235(2) 0.00443(16) -0.00135(15) 0.00053(16) Cu4 0.02180(17) 0.0257(2) 0.0317(2) 0.00843(17) -0.00215(15) 0.00103(15) Cu5 0.02828(18) 0.0249(2) 0.0266(2) 0.00303(17) 0.00744(15) 0.00399(16) Cu6 0.02903(19) 0.0302(2) 0.0311(2) 0.00322(18) 0.00447(16) -0.00348(17) In1 0.04180(13) 0.02826(15) 0.02589(12) 0.00159(10) 0.00572(10) 0.00879(11) In2 0.02983(11) 0.02686(14) 0.02568(12) 0.00167(10) 0.00545(9) 0.00668(10) P1 0.0260(4) 0.0240(5) 0.0265(4) 0.0037(3) 0.0003(3) 0.0039(3) P2 0.0257(4) 0.0329(5) 0.0241(4) -0.0035(4) 0.0004(3) 0.0056(4) P3 0.0248(4) 0.0260(5) 0.0223(4) 0.0026(3) 0.0005(3) 0.0025(3) P4 0.0222(4) 0.0248(5) 0.0279(4) 0.0037(3) -0.0018(3) 0.0036(3) P5 0.0296(4) 0.0212(5) 0.0276(4) 0.0025(3) 0.0086(3) 0.0036(3) P6 0.0279(4) 0.0318(5) 0.0280(4) 0.0003(4) 0.0057(3) -0.0009(4) S1 0.0328(4) 0.0240(5) 0.0283(4) 0.0005(3) 0.0012(3) 0.0033(3) S2 0.0308(4) 0.0244(5) 0.0234(4) 0.0028(3) 0.0028(3) 0.0005(3) S3 0.0295(4) 0.0249(5) 0.0286(4) 0.0056(3) 0.0061(3) 0.0039(3) S4 0.0315(4) 0.0298(5) 0.0243(4) 0.0010(3) 0.0036(3) 0.0027(3) S5 0.0270(4) 0.0248(5) 0.0265(4) 0.0016(3) 0.0027(3) 0.0031(3) S6 0.0279(4) 0.0219(4) 0.0253(4) 0.0042(3) 0.0053(3) 0.0031(3) S7 0.0324(4) 0.0272(5) 0.0324(5) 0.0057(4) 0.0129(3) 0.0029(3) S8 0.0352(4) 0.0268(5) 0.0288(4) 0.0031(3) 0.0106(3) 0.0033(3) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.522(5) . ? C1 S1 1.841(3) . ? C2 S2 1.848(3) . ? C3 C4 1.522(4) . ? C3 S3 1.847(3) . ? C4 S4 1.846(3) . ? C5 C6 1.551(6) . ? C6 C7 1.526(5) . ? C6 P1 1.862(4) . ? C8 C9 1.546(5) . ? C9 C10 1.546(5) . ? C9 P1 1.862(3) . ? C11 C12 1.549(5) . ? C12 C13 1.529(6) . ? C12 P1 1.869(4) . ? C14 C15 1.559(7) . ? C15 C16 1.543(6) . ? C15 P2 1.861(3) . ? C17 C18 1.543(6) . ? C18 C19 1.532(5) . ? C18 P2 1.876(3) . ? C20 C21 1.551(5) . ? C21 C22 1.531(5) . ? C21 P2 1.860(4) . ? C23 C24 1.561(5) . ? C24 C25 1.545(5) . ? C24 P3 1.859(3) . ? C26 C27 1.540(4) . ? C27 C28 1.539(5) . ? C27 P3 1.873(3) . ? C29 C30 1.536(5) . ? C30 C31 1.536(4) . ? C30 P3 1.870(3) . ? C32 C33 1.519(6) . ? C33 In1 2.203(4) . ? C34 C35 1.518(6) . ? C35 In1 2.200(4) . ? C36 C37 1.524(5) . ? C36 S5 1.847(3) . ? C37 S6 1.846(3) . ? C38 C39 1.527(4) . ? C38 S7 1.855(3) . ? C39 S8 1.841(3) . ? C40 C41 1.529(5) . ? C41 C42 1.532(5) . ? C41 P4 1.861(3) . ? C43 C44 1.545(5) . ? C44 C45 1.536(5) . ? C44 P4 1.859(3) . ? C46 C47 1.546(4) . ? C47 C48 1.536(5) . ? C47 P4 1.874(4) . ? C49 C50 1.542(6) . ? C50 C51 1.544(5) . ? C50 P5 1.868(3) . ? C52 C53 1.541(5) . ? C53 C54 1.531(5) . ? C53 P5 1.880(3) . ? C55 C56 1.548(5) . ? C56 C57 1.541(4) . ? C56 P5 1.863(4) . ? C58 C59 1.555(5) . ? C59 C60 1.527(6) . ? C59 P6 1.865(3) . ? C61 C62 1.553(7) . ? C62 C63 1.556(6) . ? C62 P6 1.892(4) . ? C64 C65 1.535(5) . ? C65 C66 1.537(6) . ? C65 P6 1.874(4) . ? C67 C68 1.493(6) . ? C68 In2 2.191(4) . ? C69 C70 1.547(5) . ? C70 In2 2.201(3) . ? Cu1 P1 2.2123(9) . ? Cu1 S2 2.2512(9) . ? Cu1 S1 2.3250(10) . ? Cu2 P2 2.2444(10) . ? Cu2 S2 2.2939(10) . ? Cu2 S3 2.2945(9) . ? Cu3 P3 2.2199(9) . ? Cu3 S3 2.2651(9) . ? Cu3 S4 2.3003(10) . ? Cu4 P4 2.2219(9) . ? Cu4 S6 2.2716(9) . ? Cu4 S5 2.3135(10) . ? Cu5 P5 2.2487(10) . ? Cu5 S7 2.2863(9) . ? Cu5 S6 2.2962(10) . ? Cu6 P6 2.2135(10) . ? Cu6 S7 2.2524(10) . ? Cu6 S8 2.3240(10) . ? In1 S4 2.5623(10) . ? In1 S1 2.5640(9) . ? In2 S8 2.5593(10) . ? In2 S5 2.5608(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 C2 C1 S1 113.1(2) . . ? C1 C2 S2 112.7(2) . . ? C4 C3 S3 112.8(2) . . ? C3 C4 S4 113.2(2) . . ? C7 C6 C5 109.8(4) . . ? C7 C6 P1 110.1(3) . . ? C5 C6 P1 110.1(3) . . ? C8 C9 C10 110.6(3) . . ? C8 C9 P1 117.1(3) . . ? C10 C9 P1 110.8(3) . . ? C13 C12 C11 110.5(3) . . ? C13 C12 P1 110.5(3) . . ? C11 C12 P1 117.5(3) . . ? C16 C15 C14 110.6(4) . . ? C16 C15 P2 117.1(3) . . ? C14 C15 P2 109.6(3) . . ? C19 C18 C17 110.5(3) . . ? C19 C18 P2 110.8(2) . . ? C17 C18 P2 116.7(3) . . ? C22 C21 C20 110.7(3) . . ? C22 C21 P2 109.8(3) . . ? C20 C21 P2 110.2(3) . . ? C25 C24 C23 110.1(3) . . ? C25 C24 P3 117.3(3) . . ? C23 C24 P3 110.3(2) . . ? C28 C27 C26 110.2(3) . . ? C28 C27 P3 112.0(2) . . ? C26 C27 P3 115.3(2) . . ? C29 C30 C31 111.8(3) . . ? C29 C30 P3 109.3(2) . . ? C31 C30 P3 109.9(2) . . ? C32 C33 In1 114.4(3) . . ? C34 C35 In1 112.6(3) . . ? C37 C36 S5 112.9(2) . . ? C36 C37 S6 112.15(19) . . ? C39 C38 S7 112.5(2) . . ? C38 C39 S8 113.1(2) . . ? C40 C41 C42 110.1(3) . . ? C40 C41 P4 109.9(3) . . ? C42 C41 P4 110.6(3) . . ? C45 C44 C43 109.5(3) . . ? C45 C44 P4 111.3(3) . . ? C43 C44 P4 117.5(3) . . ? C48 C47 C46 110.6(3) . . ? C48 C47 P4 110.9(3) . . ? C46 C47 P4 115.4(2) . . ? C49 C50 C51 111.4(3) . . ? C49 C50 P5 110.1(3) . . ? C51 C50 P5 116.8(3) . . ? C54 C53 C52 111.1(3) . . ? C54 C53 P5 110.5(2) . . ? C52 C53 P5 116.7(3) . . ? C57 C56 C55 109.7(3) . . ? C57 C56 P5 110.0(2) . . ? C55 C56 P5 109.8(2) . . ? C60 C59 C58 111.7(4) . . ? C60 C59 P6 112.8(2) . . ? C58 C59 P6 115.1(3) . . ? C61 C62 C63 107.8(4) . . ? C61 C62 P6 110.2(4) . . ? C63 C62 P6 111.0(3) . . ? C64 C65 C66 109.4(3) . . ? C64 C65 P6 111.0(3) . . ? C66 C65 P6 110.1(3) . . ? C67 C68 In2 113.8(3) . . ? C69 C70 In2 110.6(2) . . ? P1 Cu1 S2 137.77(4) . . ? P1 Cu1 S1 125.64(4) . . ? S2 Cu1 S1 95.94(3) . . ? P2 Cu2 S2 122.18(4) . . ? P2 Cu2 S3 121.26(4) . . ? S2 Cu2 S3 116.56(3) . . ? P3 Cu3 S3 133.73(4) . . ? P3 Cu3 S4 129.48(3) . . ? S3 Cu3 S4 95.46(3) . . ? P4 Cu4 S6 134.72(4) . . ? P4 Cu4 S5 129.05(4) . . ? S6 Cu4 S5 95.43(3) . . ? P5 Cu5 S7 124.72(4) . . ? P5 Cu5 S6 119.53(3) . . ? S7 Cu5 S6 115.73(3) . . ? P6 Cu6 S7 141.08(4) . . ? P6 Cu6 S8 120.77(4) . . ? S7 Cu6 S8 95.72(4) . . ? C35 In1 C33 126.17(19) . . ? C35 In1 S4 101.98(13) . . ? C33 In1 S4 101.96(12) . . ? C35 In1 S1 107.63(12) . . ? C33 In1 S1 105.99(11) . . ? S4 In1 S1 113.01(3) . . ? C68 In2 C70 121.02(15) . . ? C68 In2 S8 106.35(11) . . ? C70 In2 S8 109.31(10) . . ? C68 In2 S5 105.71(11) . . ? C70 In2 S5 103.28(9) . . ? S8 In2 S5 110.99(3) . . ? C9 P1 C6 106.39(17) . . ? C9 P1 C12 105.30(17) . . ? C6 P1 C12 105.70(17) . . ? C9 P1 Cu1 114.41(12) . . ? C6 P1 Cu1 113.03(12) . . ? C12 P1 Cu1 111.33(10) . . ? C21 P2 C15 104.44(19) . . ? C21 P2 C18 106.22(18) . . ? C15 P2 C18 104.71(17) . . ? C21 P2 Cu2 114.70(13) . . ? C15 P2 Cu2 112.61(13) . . ? C18 P2 Cu2 113.25(12) . . ? C24 P3 C30 105.81(15) . . ? C24 P3 C27 104.69(16) . . ? C30 P3 C27 105.79(14) . . ? C24 P3 Cu3 109.36(11) . . ? C30 P3 Cu3 113.82(10) . . ? C27 P3 Cu3 116.50(10) . . ? C44 P4 C41 107.64(17) . . ? C44 P4 C47 105.30(17) . . ? C41 P4 C47 102.34(16) . . ? C44 P4 Cu4 112.20(11) . . ? C41 P4 Cu4 114.92(11) . . ? C47 P4 Cu4 113.54(10) . . ? C56 P5 C50 103.75(16) . . ? C56 P5 C53 106.33(16) . . ? C50 P5 C53 104.82(16) . . ? C56 P5 Cu5 116.23(11) . . ? C50 P5 Cu5 112.06(12) . . ? C53 P5 Cu5 112.65(12) . . ? C59 P6 C65 106.04(17) . . ? C59 P6 C62 104.79(18) . . ? C65 P6 C62 102.29(19) . . ? C59 P6 Cu6 108.50(11) . . ? C65 P6 Cu6 119.19(12) . . ? C62 P6 Cu6 114.82(13) . . ? C1 S1 Cu1 96.33(11) . . ? C1 S1 In1 101.97(10) . . ? Cu1 S1 In1 122.00(4) . . ? C2 S2 Cu1 97.20(10) . . ? C2 S2 Cu2 105.33(11) . . ? Cu1 S2 Cu2 103.35(4) . . ? C3 S3 Cu3 98.08(11) . . ? C3 S3 Cu2 102.85(10) . . ? Cu3 S3 Cu2 109.73(4) . . ? C4 S4 Cu3 97.46(11) . . ? C4 S4 In1 101.59(11) . . ? Cu3 S4 In1 121.42(4) . . ? C36 S5 Cu4 97.15(11) . . ? C36 S5 In2 101.05(10) . . ? Cu4 S5 In2 120.21(4) . . ? C37 S6 Cu4 96.75(10) . . ? C37 S6 Cu5 105.99(10) . . ? Cu4 S6 Cu5 102.88(4) . . ? C38 S7 Cu6 97.68(11) . . ? C38 S7 Cu5 104.21(10) . . ? Cu6 S7 Cu5 105.37(4) . . ? C39 S8 Cu6 96.79(12) . . ? C39 S8 In2 101.92(12) . . ? Cu6 S8 In2 123.53(4) . . ? _chemical_name_common ; bis(mu!3$-1,2-dithiolatoethane-S,S,S',S')-diethanido - tris(triisopropylphosphine)-tricopper(+1)-indium(+3) ; data_[(iPr3PCu)3(SC2H4S)2IniPr2] _database_code_depnum_ccdc_archive 'CCDC 907029' #TrackingRef '17788_web_deposit_cif_file_0_DirkFriedrich_1360943962.31_[(iPr3PCu)3(SC2H4S)2IniPr2].cif' _audit_creation_date 2012-10-11T16:17:35-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; bis(\m~3~-1,2-dithiolatoethane-S,S,S',S')-di(propan-2-ido) -tris(triisopropylphosphine)-tricopper(+1)-indium(+3) ; _chemical_formula_moiety 'C37 H85 Cu3 In1 P3 S4' _chemical_formula_sum 'C37 H85 Cu3 In P3 S4' _chemical_formula_weight 1056.64 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.6293(11) _cell_length_b 14.5947(12) _cell_length_c 16.0344(13) _cell_angle_alpha 63.753(6) _cell_angle_beta 69.277(6) _cell_angle_gamma 68.494(6) _cell_volume 2590.3(4) _cell_formula_units_Z 2 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 21648 _cell_measurement_theta_min 1.99 _cell_measurement_theta_max 29.26 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description needle _exptl_crystal_colour colorless _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.07 _exptl_crystal_density_diffrn 1.355 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1104 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.92 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details ; Busing, W. R. & Levy, H. A. (1957) Acta Cryst. 10, 180-182. and Coppens, P., Leiserowitz, L. & Rabinovich, D. (1965) Acta Cryst. 1965, 1035-1038. ; _exptl_absorpt_correction_T_min 0.5411 _exptl_absorpt_correction_T_max 0.9255 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 180(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 '2-circle goniometer' _diffrn_measurement_device_type 'STOE IPDS-2T' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 6.67 _diffrn_detector 'image plate (34 cm diameter / schwenk)' _diffrn_detector_type STOE _diffrn_standards_number 0 _diffrn_reflns_av_R_equivalents 0.0552 _diffrn_reflns_av_unetI/netI 0.0685 _diffrn_reflns_number 33761 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.99 _diffrn_reflns_theta_max 26.5 _diffrn_reflns_theta_full 26.5 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _reflns_number_total 10711 _reflns_number_gt 7274 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_cell_refinement 'STOE X-AREA' _computing_data_reduction 'STOE X-AREA, STOE X-RED' _computing_structure_solution ; 'SIR-92' Altomare, A., Cascarano, G., Giacovazzo, C. & Guagliardi, A. (1993) J. Appl. Cryst. 26, 343-350. ; _computing_structure_refinement ; 'SHELXL-97' Sheldrick, G.M. (2008) Acta Cryst. A64, 112 ; _computing_molecular_graphics 'DIAMOND 3.2' _computing_publication_material ; 'WinGX publication routines' Farrugia, L. J. (1999) WinGX, J. Appl. Cryst. 32, 837-838 ; #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0192P)^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_number_reflns 10711 _refine_ls_number_parameters 485 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0623 _refine_ls_R_factor_gt 0.0322 _refine_ls_wR_factor_ref 0.0573 _refine_ls_wR_factor_gt 0.0532 _refine_ls_goodness_of_fit_ref 0.886 _refine_ls_restrained_S_all 0.886 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.639 _refine_diff_density_min -0.601 _refine_diff_density_rms 0.068 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' In In -0.7276 1.31 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.6617(2) 0.4010(3) 0.0553(2) 0.0304(7) Uani 1 1 d . . . H1A H 0.6667 0.4511 -0.0116 0.036 Uiso 1 1 calc R . . H1B H 0.6771 0.3294 0.0549 0.036 Uiso 1 1 calc R . . C2 C 0.5470(2) 0.4290(2) 0.1131(2) 0.0277(7) Uani 1 1 d . . . H2A H 0.5405 0.3765 0.179 0.033 Uiso 1 1 calc R . . H2B H 0.4955 0.4253 0.0845 0.033 Uiso 1 1 calc R . . C3 C 0.5707(2) 0.3926(3) 0.3809(2) 0.0327(7) Uani 1 1 d . A . H3A H 0.6073 0.422 0.3129 0.039 Uiso 1 1 calc R . . H3B H 0.5721 0.4352 0.4141 0.039 Uiso 1 1 calc R . . C4 C 0.6326(2) 0.2790(3) 0.4246(2) 0.0328(7) Uani 1 1 d . A . H4A H 0.5996 0.252 0.4939 0.039 Uiso 1 1 calc R . . H4B H 0.7083 0.2777 0.4173 0.039 Uiso 1 1 calc R . . C5 C 0.9078(3) 0.4947(4) 0.2433(5) 0.0864(18) Uani 1 1 d . . . H5A H 0.8717 0.4474 0.2438 0.13 Uiso 1 1 calc R . . H5B H 0.8835 0.5021 0.3058 0.13 Uiso 1 1 calc R . . H5C H 0.9864 0.4652 0.2298 0.13 Uiso 1 1 calc R . . C6 C 0.8800(3) 0.6013(3) 0.1673(3) 0.0501(11) Uani 1 1 d . . . H6 H 0.9039 0.6529 0.1762 0.06 Uiso 1 1 calc R . . C7 C 0.9383(3) 0.5963(5) 0.0675(4) 0.106(2) Uani 1 1 d . . . H7A H 1.0168 0.5755 0.0611 0.158 Uiso 1 1 calc R . . H7B H 0.9181 0.6658 0.0188 0.158 Uiso 1 1 calc R . . H7C H 0.9171 0.5443 0.0588 0.158 Uiso 1 1 calc R . . C8 C 0.7818(5) 0.8510(4) 0.0815(4) 0.100(2) Uani 1 1 d . . . H8A H 0.8526 0.8216 0.0462 0.15 Uiso 1 1 calc R . . H8B H 0.7887 0.8451 0.1426 0.15 Uiso 1 1 calc R . . H8C H 0.7556 0.9254 0.0439 0.15 Uiso 1 1 calc R . . C9 C 0.7006(4) 0.7893(3) 0.1002(3) 0.0566(11) Uani 1 1 d . . . H9 H 0.6297 0.8238 0.1344 0.068 Uiso 1 1 calc R . . C10 C 0.6830(4) 0.8044(4) 0.0053(3) 0.0793(15) Uani 1 1 d . . . H10A H 0.6611 0.88 -0.0315 0.119 Uiso 1 1 calc R . . H10B H 0.626 0.771 0.0179 0.119 Uiso 1 1 calc R . . H10C H 0.7505 0.7719 -0.0314 0.119 Uiso 1 1 calc R . . C11 C 0.7197(3) 0.7065(4) 0.3316(3) 0.0653(13) Uani 1 1 d . . . H11A H 0.6973 0.7822 0.2956 0.098 Uiso 1 1 calc R . . H11B H 0.799 0.6831 0.3175 0.098 Uiso 1 1 calc R . . H11C H 0.6916 0.6931 0.4001 0.098 Uiso 1 1 calc R . . C12 C 0.6741(2) 0.6452(3) 0.3024(2) 0.0382(8) Uani 1 1 d . . . H12 H 0.6934 0.5697 0.3451 0.046 Uiso 1 1 calc R . . C13 C 0.5489(3) 0.6805(4) 0.3246(3) 0.0560(12) Uani 1 1 d . . . H13A H 0.5205 0.6633 0.3937 0.084 Uiso 1 1 calc R . . H13B H 0.5213 0.6437 0.3028 0.084 Uiso 1 1 calc R . . H13C H 0.5256 0.7568 0.2916 0.084 Uiso 1 1 calc R . . C14 C 0.3619(4) 0.8371(3) 0.1238(4) 0.0772(15) Uani 1 1 d . . . H14A H 0.3232 0.8502 0.0768 0.116 Uiso 1 1 calc R . . H14B H 0.4231 0.7749 0.1253 0.116 Uiso 1 1 calc R . . H14C H 0.3888 0.8986 0.1058 0.116 Uiso 1 1 calc R . . C15 C 0.2848(3) 0.8180(3) 0.2224(3) 0.0548(11) Uani 1 1 d . . . H15 H 0.3278 0.8077 0.2664 0.066 Uiso 1 1 calc R . . C16 C 0.1905(4) 0.9180(3) 0.2246(4) 0.0815(17) Uani 1 1 d . . . H16A H 0.2203 0.9771 0.2085 0.122 Uiso 1 1 calc R . . H16B H 0.1427 0.9041 0.2887 0.122 Uiso 1 1 calc R . . H16C H 0.1491 0.9359 0.1781 0.122 Uiso 1 1 calc R . . C17 C 0.0359(3) 0.7758(4) 0.2166(4) 0.0687(14) Uani 1 1 d . . . H17A H -0.0005 0.7913 0.1673 0.103 Uiso 1 1 calc R . . H17B H 0.0321 0.842 0.221 0.103 Uiso 1 1 calc R . . H17C H 0.0002 0.7313 0.2783 0.103 Uiso 1 1 calc R . . C18 C 0.1555(3) 0.7175(3) 0.1902(3) 0.0427(9) Uani 1 1 d . . . H18 H 0.1862 0.7642 0.1251 0.051 Uiso 1 1 calc R . . C19 C 0.1626(3) 0.6159(3) 0.1793(3) 0.0492(10) Uani 1 1 d . . . H19A H 0.1288 0.5689 0.2403 0.074 Uiso 1 1 calc R . . H19B H 0.2388 0.5807 0.1601 0.074 Uiso 1 1 calc R . . H19C H 0.1246 0.6333 0.1304 0.074 Uiso 1 1 calc R . . C20 C 0.2171(4) 0.6832(5) 0.4513(3) 0.0770(15) Uani 1 1 d . . . H20A H 0.1702 0.6767 0.5151 0.115 Uiso 1 1 calc R . . H20B H 0.2382 0.7501 0.4224 0.115 Uiso 1 1 calc R . . H20C H 0.2821 0.6244 0.4564 0.115 Uiso 1 1 calc R . . C21 C 0.1557(3) 0.6810(4) 0.3887(3) 0.0542(11) Uani 1 1 d . . . H21 H 0.0904 0.7421 0.3826 0.065 Uiso 1 1 calc R . . C22 C 0.1197(3) 0.5789(4) 0.4336(3) 0.0693(14) Uani 1 1 d . . . H22A H 0.1835 0.5187 0.4398 0.104 Uiso 1 1 calc R . . H22B H 0.0805 0.5786 0.3931 0.104 Uiso 1 1 calc R . . H22C H 0.0721 0.5737 0.497 0.104 Uiso 1 1 calc R . . C23A C 0.1660(7) 0.3305(8) 0.3918(7) 0.091(4) Uani 0.548(9) 1 d PD A 1 H23A H 0.0891 0.3459 0.4237 0.137 Uiso 0.548(9) 1 calc PR A 1 H23B H 0.1752 0.3728 0.3234 0.137 Uiso 0.548(9) 1 calc PR A 1 H23C H 0.2075 0.3479 0.4194 0.137 Uiso 0.548(9) 1 calc PR A 1 C24A C 0.2074(13) 0.2120(10) 0.4059(9) 0.042(4) Uani 0.548(9) 1 d PD A 1 H24A H 0.1638 0.1947 0.3786 0.05 Uiso 0.548(9) 1 calc PR A 1 C25A C 0.1881(9) 0.1501(8) 0.5142(7) 0.097(5) Uani 0.548(9) 1 d PD A 1 H25A H 0.2421 0.1537 0.5393 0.146 Uiso 0.548(9) 1 calc PR A 1 H25B H 0.1947 0.0762 0.5268 0.146 Uiso 0.548(9) 1 calc PR A 1 H25C H 0.1153 0.1809 0.5456 0.146 Uiso 0.548(9) 1 calc PR A 1 C23B C 0.2119(8) 0.2102(13) 0.5144(7) 0.071(4) Uani 0.452(9) 1 d PD A 2 H23D H 0.1387 0.2265 0.5535 0.106 Uiso 0.452(9) 1 calc PR A 2 H23E H 0.2554 0.2508 0.5144 0.106 Uiso 0.452(9) 1 calc PR A 2 H23F H 0.2457 0.1347 0.5408 0.106 Uiso 0.452(9) 1 calc PR A 2 C24B C 0.2057(15) 0.2395(13) 0.4123(10) 0.036(4) Uani 0.452(9) 1 d PD A 2 H24B H 0.1894 0.3182 0.3823 0.044 Uiso 0.452(9) 1 calc PR A 2 C25B C 0.1119(6) 0.2065(9) 0.4114(7) 0.063(3) Uani 0.452(9) 1 d PD A 2 H25D H 0.1267 0.1293 0.4375 0.094 Uiso 0.452(9) 1 calc PR A 2 H25E H 0.1043 0.233 0.3457 0.094 Uiso 0.452(9) 1 calc PR A 2 H25F H 0.0448 0.236 0.4506 0.094 Uiso 0.452(9) 1 calc PR A 2 C26 C 0.3255(3) -0.0110(3) 0.3571(3) 0.0565(11) Uani 1 1 d . . . H26A H 0.3555 0.0031 0.2886 0.085 Uiso 1 1 calc R . . H26B H 0.2474 0.0215 0.3684 0.085 Uiso 1 1 calc R . . H26C H 0.3384 -0.0873 0.392 0.085 Uiso 1 1 calc R . . C27 C 0.3813(3) 0.0363(3) 0.3925(3) 0.0427(9) Uani 1 1 d . A . H27 H 0.3515 0.0157 0.4631 0.051 Uiso 1 1 calc R . . C28 C 0.5037(3) -0.0147(3) 0.3783(3) 0.0575(11) Uani 1 1 d . . . H28A H 0.5162 -0.091 0.4139 0.086 Uiso 1 1 calc R . . H28B H 0.5369 0.0158 0.4018 0.086 Uiso 1 1 calc R . . H28C H 0.5363 -0.0016 0.3102 0.086 Uiso 1 1 calc R . . C29 C 0.4583(3) 0.1937(3) 0.1574(3) 0.0471(9) Uani 1 1 d . . . H29A H 0.4583 0.2295 0.0893 0.071 Uiso 1 1 calc R . . H29B H 0.4819 0.1172 0.1728 0.071 Uiso 1 1 calc R . . H29C H 0.508 0.2159 0.172 0.071 Uiso 1 1 calc R . . C30 C 0.3429(3) 0.2227(3) 0.2173(3) 0.0390(8) Uani 1 1 d . A . H30 H 0.2983 0.1818 0.2168 0.047 Uiso 1 1 calc R . . C31 C 0.2900(3) 0.3424(3) 0.1728(3) 0.0530(10) Uani 1 1 d . . . H31A H 0.3243 0.3834 0.1838 0.08 Uiso 1 1 calc R . . H31B H 0.2124 0.3571 0.2027 0.08 Uiso 1 1 calc R . . H31C H 0.3001 0.3623 0.104 0.08 Uiso 1 1 calc R . . C32 C 0.8009(5) 0.0062(4) 0.2297(4) 0.100(2) Uani 1 1 d . . . H32A H 0.7969 -0.0373 0.1993 0.15 Uiso 1 1 calc R . . H32B H 0.7371 0.0104 0.2824 0.15 Uiso 1 1 calc R . . H32C H 0.8666 -0.0256 0.2545 0.15 Uiso 1 1 calc R . . C33 C 0.8038(4) 0.1125(3) 0.1592(3) 0.0673(13) Uani 1 1 d . . . H33 H 0.7364 0.1413 0.1348 0.081 Uiso 1 1 calc R . . C34 C 0.8998(4) 0.1161(4) 0.0722(3) 0.0862(18) Uani 1 1 d . . . H34A H 0.967 0.0982 0.0916 0.129 Uiso 1 1 calc R . . H34B H 0.8892 0.1871 0.0234 0.129 Uiso 1 1 calc R . . H34C H 0.9045 0.0651 0.0458 0.129 Uiso 1 1 calc R . . C35 C 0.9416(3) 0.0940(4) 0.3748(4) 0.094(2) Uani 1 1 d . . . H35A H 0.9613 0.0358 0.3522 0.142 Uiso 1 1 calc R . . H35B H 0.8736 0.0922 0.4237 0.142 Uiso 1 1 calc R . . H35C H 0.9991 0.0869 0.4022 0.142 Uiso 1 1 calc R . . C36 C 0.9274(3) 0.1984(3) 0.2914(3) 0.0519(10) Uani 1 1 d . . . H36 H 0.9056 0.2566 0.3164 0.062 Uiso 1 1 calc R . . C37 C 1.0327(3) 0.2090(4) 0.2131(3) 0.0792(16) Uani 1 1 d . . . H37A H 1.0916 0.1956 0.2417 0.119 Uiso 1 1 calc R . . H37B H 1.0221 0.2805 0.165 0.119 Uiso 1 1 calc R . . H37C H 1.0513 0.1576 0.1827 0.119 Uiso 1 1 calc R . . P1 P 0.73058(6) 0.64686(7) 0.17808(6) 0.02938(19) Uani 1 1 d . . . P2 P 0.24502(6) 0.69166(7) 0.26753(7) 0.0330(2) Uani 1 1 d . . . P3 P 0.34878(6) 0.18458(7) 0.34280(6) 0.03031(18) Uani 1 1 d . . . S1 S 0.76517(6) 0.40450(6) 0.10220(6) 0.02948(18) Uani 1 1 d . . . S2 S 0.50967(6) 0.56202(6) 0.11744(6) 0.02828(17) Uani 1 1 d . . . S3 S 0.42822(6) 0.40359(6) 0.38914(6) 0.03137(18) Uani 1 1 d . . . S4 S 0.63368(6) 0.19064(6) 0.37048(6) 0.03102(18) Uani 1 1 d . . . Cu1 Cu 0.66585(3) 0.55026(3) 0.14572(3) 0.02915(9) Uani 1 1 d . . . Cu2 Cu 0.38905(3) 0.55414(3) 0.26110(3) 0.02871(9) Uani 1 1 d . A . Cu3 Cu 0.45615(3) 0.25881(3) 0.35616(3) 0.03071(9) Uani 1 1 d . A . In1 In 0.797090(18) 0.218779(19) 0.227946(18) 0.03367(7) Uani 1 1 d . A . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0353(16) 0.0313(17) 0.0279(18) -0.0150(15) -0.0063(13) -0.0074(13) C2 0.0322(15) 0.0303(17) 0.0233(17) -0.0069(14) -0.0082(12) -0.0123(13) C3 0.0360(17) 0.041(2) 0.0291(19) -0.0150(16) -0.0063(14) -0.0168(15) C4 0.0321(16) 0.0378(19) 0.0297(19) -0.0112(16) -0.0102(13) -0.0082(14) C5 0.049(2) 0.068(3) 0.154(6) -0.052(4) -0.043(3) 0.008(2) C6 0.0327(17) 0.063(3) 0.072(3) -0.046(2) 0.0010(18) -0.0165(17) C7 0.049(2) 0.189(6) 0.133(5) -0.132(5) 0.048(3) -0.060(3) C8 0.181(6) 0.072(4) 0.083(4) 0.016(3) -0.069(4) -0.088(4) C9 0.090(3) 0.043(2) 0.044(3) 0.001(2) -0.027(2) -0.033(2) C10 0.127(4) 0.077(3) 0.047(3) 0.008(3) -0.035(3) -0.062(3) C11 0.070(3) 0.108(4) 0.047(3) -0.048(3) 0.011(2) -0.050(3) C12 0.0377(17) 0.051(2) 0.031(2) -0.0212(18) 0.0024(14) -0.0192(16) C13 0.0377(19) 0.079(3) 0.061(3) -0.049(3) 0.0120(18) -0.0176(19) C14 0.070(3) 0.041(3) 0.099(4) -0.016(3) -0.004(3) -0.018(2) C15 0.0404(19) 0.039(2) 0.093(3) -0.032(2) -0.027(2) 0.0031(16) C16 0.069(3) 0.042(3) 0.154(5) -0.056(3) -0.049(3) 0.011(2) C17 0.041(2) 0.075(3) 0.117(4) -0.061(3) -0.042(2) 0.013(2) C18 0.0378(18) 0.048(2) 0.047(2) -0.0199(19) -0.0166(16) -0.0061(16) C19 0.044(2) 0.061(3) 0.055(3) -0.036(2) -0.0131(17) -0.0067(18) C20 0.068(3) 0.133(5) 0.058(3) -0.058(3) -0.010(2) -0.030(3) C21 0.0301(18) 0.093(3) 0.054(3) -0.050(3) -0.0020(17) -0.0084(19) C22 0.051(2) 0.117(4) 0.045(3) -0.038(3) 0.010(2) -0.035(3) C23A 0.056(5) 0.079(8) 0.085(7) -0.023(6) 0.009(5) 0.008(5) C24A 0.034(5) 0.046(8) 0.057(7) -0.029(5) -0.006(4) -0.011(5) C25A 0.082(7) 0.074(7) 0.066(7) -0.004(6) 0.028(6) -0.015(6) C23B 0.059(6) 0.125(13) 0.041(6) -0.037(8) 0.006(5) -0.046(7) C24B 0.031(5) 0.041(9) 0.044(6) -0.028(6) 0.002(4) -0.009(6) C25B 0.039(5) 0.099(8) 0.072(7) -0.047(7) -0.001(4) -0.031(5) C26 0.075(3) 0.031(2) 0.070(3) -0.003(2) -0.036(2) -0.0221(19) C27 0.049(2) 0.033(2) 0.044(2) 0.0000(17) -0.0202(17) -0.0166(16) C28 0.062(2) 0.034(2) 0.074(3) -0.010(2) -0.033(2) -0.0046(18) C29 0.066(2) 0.049(2) 0.028(2) -0.0106(19) -0.0107(17) -0.0207(19) C30 0.0475(19) 0.037(2) 0.037(2) -0.0036(17) -0.0176(15) -0.0205(16) C31 0.051(2) 0.043(2) 0.052(3) 0.004(2) -0.0211(18) -0.0159(18) C32 0.118(4) 0.059(3) 0.119(5) -0.053(4) 0.018(4) -0.036(3) C33 0.093(3) 0.044(3) 0.053(3) -0.023(2) -0.003(2) -0.010(2) C34 0.121(4) 0.067(3) 0.050(3) -0.037(3) 0.012(3) -0.012(3) C35 0.047(2) 0.090(4) 0.083(4) 0.031(3) -0.029(2) -0.015(2) C36 0.0281(17) 0.056(2) 0.051(3) 0.001(2) -0.0114(16) -0.0110(16) C37 0.032(2) 0.093(4) 0.071(3) 0.002(3) -0.007(2) -0.016(2) P1 0.0310(4) 0.0335(5) 0.0282(5) -0.0150(4) -0.0004(3) -0.0142(3) P2 0.0234(4) 0.0372(5) 0.0416(5) -0.0221(4) -0.0073(3) -0.0012(3) P3 0.0310(4) 0.0305(5) 0.0299(5) -0.0054(4) -0.0094(3) -0.0129(3) S1 0.0251(4) 0.0291(4) 0.0322(5) -0.0117(4) -0.0025(3) -0.0077(3) S2 0.0264(4) 0.0273(4) 0.0269(4) -0.0078(4) -0.0040(3) -0.0068(3) S3 0.0305(4) 0.0303(4) 0.0288(5) -0.0081(4) -0.0042(3) -0.0085(3) S4 0.0284(4) 0.0311(4) 0.0309(5) -0.0094(4) -0.0054(3) -0.0083(3) Cu1 0.03285(19) 0.0318(2) 0.0272(2) -0.01215(18) -0.00282(16) -0.01476(16) Cu2 0.02508(18) 0.0285(2) 0.0309(2) -0.01152(18) -0.00546(15) -0.00486(15) Cu3 0.03255(19) 0.0344(2) 0.0271(2) -0.00702(19) -0.00713(16) -0.01521(17) In1 0.03010(11) 0.02753(13) 0.03475(15) -0.01182(11) -0.00156(10) -0.00281(9) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.521(4) . ? C1 S1 1.843(3) . ? C2 S2 1.844(3) . ? C3 C4 1.523(5) . ? C3 S3 1.849(3) . ? C4 S4 1.840(3) . ? C5 C6 1.506(7) . ? C6 C7 1.536(6) . ? C6 P1 1.865(3) . ? C8 C9 1.543(6) . ? C9 C10 1.532(6) . ? C9 P1 1.868(4) . ? C11 C12 1.545(5) . ? C12 C13 1.546(5) . ? C12 P1 1.858(3) . ? C14 C15 1.527(6) . ? C15 C16 1.557(5) . ? C15 P2 1.868(4) . ? C17 C18 1.540(5) . ? C18 C19 1.534(5) . ? C18 P2 1.868(4) . ? C20 C21 1.533(6) . ? C21 C22 1.522(6) . ? C21 P2 1.865(4) . ? C23A C24A 1.546(11) . ? C24A C25A 1.538(11) . ? C24A P3 1.819(16) . ? C23B C24B 1.523(12) . ? C24B C25B 1.527(13) . ? C24B P3 1.948(18) . ? C26 C27 1.554(5) . ? C27 C28 1.537(5) . ? C27 P3 1.880(3) . ? C29 C30 1.542(5) . ? C30 C31 1.556(5) . ? C30 P3 1.859(4) . ? C32 C33 1.466(7) . ? C33 C34 1.535(6) . ? C33 In1 2.228(4) . ? C35 C36 1.520(6) . ? C36 C37 1.542(5) . ? C36 In1 2.214(4) . ? P1 Cu1 2.2176(9) . ? P2 Cu2 2.2457(9) . ? P3 Cu3 2.2250(9) . ? S1 Cu1 2.3191(8) . ? S1 In1 2.5542(9) . ? S2 Cu1 2.2611(9) . ? S2 Cu2 2.2905(8) . ? S3 Cu3 2.2684(9) . ? S3 Cu2 2.2920(10) . ? S4 Cu3 2.3071(9) . ? S4 In1 2.5672(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 C2 C1 S1 113.1(2) . . ? C1 C2 S2 112.4(2) . . ? C4 C3 S3 112.4(2) . . ? C3 C4 S4 113.4(2) . . ? C5 C6 C7 110.5(4) . . ? C5 C6 P1 109.9(3) . . ? C7 C6 P1 109.8(3) . . ? C10 C9 C8 109.9(4) . . ? C10 C9 P1 111.4(3) . . ? C8 C9 P1 116.4(3) . . ? C11 C12 C13 110.3(3) . . ? C11 C12 P1 116.2(2) . . ? C13 C12 P1 111.0(3) . . ? C14 C15 C16 111.0(4) . . ? C14 C15 P2 111.5(3) . . ? C16 C15 P2 116.3(3) . . ? C19 C18 C17 109.9(3) . . ? C19 C18 P2 111.2(3) . . ? C17 C18 P2 117.2(3) . . ? C22 C21 C20 110.3(4) . . ? C22 C21 P2 109.4(2) . . ? C20 C21 P2 109.8(3) . . ? C25A C24A C23A 107.0(9) . . ? C25A C24A P3 113.8(10) . . ? C23A C24A P3 109.3(9) . . ? C23B C24B C25B 110.8(11) . . ? C23B C24B P3 108.1(10) . . ? C25B C24B P3 116.4(9) . . ? C28 C27 C26 111.0(3) . . ? C28 C27 P3 112.7(2) . . ? C26 C27 P3 114.1(3) . . ? C29 C30 C31 110.2(3) . . ? C29 C30 P3 109.4(2) . . ? C31 C30 P3 111.7(3) . . ? C32 C33 C34 114.3(4) . . ? C32 C33 In1 110.9(3) . . ? C34 C33 In1 110.8(3) . . ? C35 C36 C37 112.5(3) . . ? C35 C36 In1 110.8(3) . . ? C37 C36 In1 109.3(3) . . ? C12 P1 C6 103.81(17) . . ? C12 P1 C9 105.20(18) . . ? C6 P1 C9 106.9(2) . . ? C12 P1 Cu1 113.36(11) . . ? C6 P1 Cu1 113.77(11) . . ? C9 P1 Cu1 112.98(13) . . ? C21 P2 C18 106.27(17) . . ? C21 P2 C15 104.77(19) . . ? C18 P2 C15 104.51(19) . . ? C21 P2 Cu2 115.71(15) . . ? C18 P2 Cu2 112.27(11) . . ? C15 P2 Cu2 112.38(11) . . ? C24A P3 C30 104.2(4) . . ? C24A P3 C27 98.9(4) . . ? C30 P3 C27 105.01(16) . . ? C24A P3 C24B 13.1(6) . . ? C30 P3 C24B 108.4(4) . . ? C27 P3 C24B 109.0(5) . . ? C24A P3 Cu3 116.7(4) . . ? C30 P3 Cu3 113.34(11) . . ? C27 P3 Cu3 116.81(12) . . ? C24B P3 Cu3 104.1(4) . . ? C1 S1 Cu1 96.87(9) . . ? C1 S1 In1 100.59(11) . . ? Cu1 S1 In1 121.12(3) . . ? C2 S2 Cu1 97.13(10) . . ? C2 S2 Cu2 105.70(10) . . ? Cu1 S2 Cu2 102.81(4) . . ? C3 S3 Cu3 98.20(10) . . ? C3 S3 Cu2 102.12(11) . . ? Cu3 S3 Cu2 110.40(4) . . ? C4 S4 Cu3 97.06(10) . . ? C4 S4 In1 100.81(10) . . ? Cu3 S4 In1 123.62(4) . . ? P1 Cu1 S2 137.41(3) . . ? P1 Cu1 S1 126.35(3) . . ? S2 Cu1 S1 95.50(3) . . ? P2 Cu2 S2 118.90(4) . . ? P2 Cu2 S3 125.06(3) . . ? S2 Cu2 S3 116.03(3) . . ? P3 Cu3 S3 134.32(3) . . ? P3 Cu3 S4 129.38(3) . . ? S3 Cu3 S4 95.32(3) . . ? C36 In1 C33 123.61(18) . . ? C36 In1 S1 108.10(10) . . ? C33 In1 S1 105.46(13) . . ? C36 In1 S4 104.08(10) . . ? C33 In1 S4 102.70(12) . . ? S1 In1 S4 112.95(3) . . ? _chemical_name_common ; bis(mu!3$-1,2-dithiolatoethane-S,S,S',S')-di(propan-2-ido) - tris(triisopropylphosphine)-tricopper(+1)-indium(+3) ; data_[(iPr3PCu)3(SC2H4S)2InBu2] _database_code_depnum_ccdc_archive 'CCDC 907030' #TrackingRef '17790_web_deposit_cif_file_0_DirkFriedrich_1360944830.32_[(iPr3PCu)3(SC2H4S)2InBu2].cif' _audit_creation_date 2012-10-11T18:05:03-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; bis(\m~3~-1,2-dithiolatoethane-S,S,S',S')-di(butan-1-ido) -tris(triisopropylphosphine)-copper(+1)-indium(+3) ; _chemical_formula_moiety 'C39 H89 Cu3 In1 P3 S4' _chemical_formula_sum 'C39 H89 Cu3 In P3 S4' _chemical_formula_weight 1084.69 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P b c a' _symmetry_space_group_name_Hall '-P 2ac 2ab' _symmetry_Int_Tables_number 61 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 15.7369(7) _cell_length_b 26.3293(13) _cell_length_c 25.2791(14) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 10474.2(9) _cell_formula_units_Z 8 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used 30804 _cell_measurement_theta_min 2.07 _cell_measurement_theta_max 26.01 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.17 _exptl_crystal_density_diffrn 1.376 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4544 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.91 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details ; Busing, W. R. & Levy, H. A. (1957) Acta Cryst. 10, 180-182. and Coppens, P., Leiserowitz, L. & Rabinovich, D. (1965) Acta Cryst. 1965, 1035-1038. ; _exptl_absorpt_correction_T_min 0.7380 _exptl_absorpt_correction_T_max 0.8005 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 213(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 '1-circle goniometer' _diffrn_measurement_device_type 'STOE IPDS 1' _diffrn_measurement_method '\f scans' _diffrn_detector 'image plate' _diffrn_detector_type STOE _diffrn_standards_number 0 _diffrn_reflns_av_R_equivalents 0.066 _diffrn_reflns_av_unetI/netI 0.0546 _diffrn_reflns_number 60483 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 2.17 _diffrn_reflns_theta_max 25.93 _diffrn_reflns_theta_full 25.93 _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.996 _reflns_number_total 10173 _reflns_number_gt 6823 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_cell_refinement 'STOE X-AREA' _computing_data_reduction 'STOE X-AREA, STOE X-RED' _computing_structure_solution ; 'SIR-92' Altomare, A., Cascarano, G., Giacovazzo, C. & Guagliardi, A. (1993) J. Appl. Cryst. 26, 343-350. ; _computing_structure_refinement ; 'SHELXL-97' Sheldrick, G.M. (2008) Acta Cryst. A64, 112 ; _computing_molecular_graphics 'DIAMOND 3.2' _computing_publication_material ; 'WinGX publication routines' Farrugia, L. J. (1999) WinGX, J. Appl. Cryst. 32, 837-838 ; #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0378P)^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_number_reflns 10173 _refine_ls_number_parameters 559 _refine_ls_number_restraints 33 _refine_ls_R_factor_all 0.0611 _refine_ls_R_factor_gt 0.0352 _refine_ls_wR_factor_ref 0.0737 _refine_ls_wR_factor_gt 0.0689 _refine_ls_goodness_of_fit_ref 0.853 _refine_ls_restrained_S_all 0.853 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.922 _refine_diff_density_min -0.384 _refine_diff_density_rms 0.075 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' In In -0.7276 1.31 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.3604(2) 0.57153(15) 0.63788(13) 0.0475(9) Uani 1 1 d . . . H1A H 0.4077 0.5522 0.6531 0.057 Uiso 1 1 calc R . . H1B H 0.3702 0.6076 0.6455 0.057 Uiso 1 1 calc R . . C2 C 0.2782(2) 0.55494(14) 0.66395(13) 0.0439(8) Uani 1 1 d . A . H2A H 0.2311 0.5752 0.6498 0.053 Uiso 1 1 calc R . . H2B H 0.2817 0.5614 0.7021 0.053 Uiso 1 1 calc R . . C3 C 0.0969(2) 0.52863(13) 0.53390(13) 0.0406(8) Uani 1 1 d . A . H3A H 0.1567 0.5226 0.5425 0.049 Uiso 1 1 calc R . . H3B H 0.0789 0.5022 0.5089 0.049 Uiso 1 1 calc R . . C4 C 0.0886(2) 0.57931(15) 0.50798(13) 0.0447(9) Uani 1 1 d . A . H4A H 0.0295 0.5841 0.4967 0.054 Uiso 1 1 calc R . . H4B H 0.1243 0.5799 0.4762 0.054 Uiso 1 1 calc R . . C5 C 0.2445(3) 0.4859(2) 0.41935(19) 0.0795(15) Uani 1 1 d . . . H5A H 0.2493 0.5171 0.4396 0.119 Uiso 1 1 calc R . . H5B H 0.189 0.4709 0.4253 0.119 Uiso 1 1 calc R . . H5C H 0.2513 0.4934 0.382 0.119 Uiso 1 1 calc R . . C6 C 0.3133(3) 0.44888(18) 0.43678(16) 0.0628(12) Uani 1 1 d . . . H6 H 0.309 0.4188 0.4135 0.075 Uiso 1 1 calc R . . C7 C 0.3972(4) 0.4716(3) 0.4275(2) 0.115(2) Uani 1 1 d . . . H7A H 0.4 0.4846 0.3916 0.173 Uiso 1 1 calc R . . H7B H 0.4409 0.4461 0.4325 0.173 Uiso 1 1 calc R . . H7C H 0.4062 0.4993 0.4522 0.173 Uiso 1 1 calc R . . C8 C 0.4577(3) 0.4096(3) 0.5378(2) 0.0959(19) Uani 1 1 d . . . H8A H 0.4461 0.4287 0.5698 0.144 Uiso 1 1 calc R . . H8B H 0.4751 0.4327 0.51 0.144 Uiso 1 1 calc R . . H8C H 0.5027 0.3853 0.5445 0.144 Uiso 1 1 calc R . . C9 C 0.3783(3) 0.38170(18) 0.52078(18) 0.0699(13) Uani 1 1 d . . . H9 H 0.391 0.3613 0.4889 0.084 Uiso 1 1 calc R . . C10 C 0.3530(4) 0.3458(2) 0.5664(2) 0.104(2) Uani 1 1 d . . . H10A H 0.4019 0.3257 0.5769 0.155 Uiso 1 1 calc R . . H10B H 0.3078 0.3234 0.5548 0.155 Uiso 1 1 calc R . . H10C H 0.3335 0.3657 0.5963 0.155 Uiso 1 1 calc R . . C11 C 0.2040(4) 0.3420(2) 0.46094(19) 0.0898(18) Uani 1 1 d . . . H11A H 0.2375 0.3173 0.4805 0.135 Uiso 1 1 calc R . . H11B H 0.233 0.3505 0.4283 0.135 Uiso 1 1 calc R . . H11C H 0.1488 0.3276 0.4529 0.135 Uiso 1 1 calc R . . C12 C 0.1926(3) 0.39048(17) 0.49482(16) 0.0620(12) Uani 1 1 d . . . H12 H 0.1559 0.4131 0.4735 0.074 Uiso 1 1 calc R . . C13 C 0.1435(3) 0.38035(19) 0.54455(19) 0.0712(13) Uani 1 1 d . . . H13A H 0.0884 0.3663 0.5356 0.107 Uiso 1 1 calc R . . H13B H 0.1359 0.4119 0.5638 0.107 Uiso 1 1 calc R . . H13C H 0.1745 0.3564 0.5664 0.107 Uiso 1 1 calc R . . C14A C -0.0062(16) 0.3162(6) 0.7004(8) 0.076(5) Uani 0.490(6) 1 d PD A 1 H14A H -0.0615 0.3211 0.7166 0.114 Uiso 0.490(6) 1 calc PR A 1 H14B H 0.0361 0.3109 0.7278 0.114 Uiso 0.490(6) 1 calc PR A 1 H14C H -0.008 0.2867 0.6775 0.114 Uiso 0.490(6) 1 calc PR A 1 C15A C 0.0172(6) 0.3631(3) 0.6679(3) 0.053(2) Uani 0.490(6) 1 d PD A 1 H15A H 0.0655 0.353 0.6452 0.063 Uiso 0.490(6) 1 calc PR A 1 C16A C -0.0547(7) 0.3796(4) 0.6299(4) 0.072(3) Uani 0.490(6) 1 d PD A 1 H16A H -0.0625 0.3539 0.6029 0.108 Uiso 0.490(6) 1 calc PR A 1 H16B H -0.0396 0.4116 0.6133 0.108 Uiso 0.490(6) 1 calc PR A 1 H16C H -0.1071 0.3837 0.6497 0.108 Uiso 0.490(6) 1 calc PR A 1 C14B C 0.1697(7) 0.3448(5) 0.6878(5) 0.090(4) Uani 0.510(6) 1 d PD A 2 H14D H 0.1861 0.3396 0.7244 0.135 Uiso 0.510(6) 1 calc PR A 2 H14E H 0.2005 0.3736 0.6735 0.135 Uiso 0.510(6) 1 calc PR A 2 H14F H 0.1832 0.3146 0.6675 0.135 Uiso 0.510(6) 1 calc PR A 2 C15B C 0.0736(6) 0.3551(3) 0.6848(4) 0.061(3) Uani 0.510(6) 1 d PD A 2 H15B H 0.0598 0.3544 0.6466 0.074 Uiso 0.510(6) 1 calc PR A 2 C16B C 0.0241(17) 0.3100(8) 0.7091(11) 0.135(12) Uani 0.510(6) 1 d PD A 2 H16D H 0.0409 0.2788 0.6916 0.203 Uiso 0.510(6) 1 calc PR A 2 H16E H -0.0364 0.3154 0.7042 0.203 Uiso 0.510(6) 1 calc PR A 2 H16F H 0.0367 0.3077 0.7465 0.203 Uiso 0.510(6) 1 calc PR A 2 C17A C 0.1709(14) 0.4283(9) 0.7877(8) 0.084(8) Uani 0.490(6) 1 d PD A 1 H17A H 0.2104 0.4134 0.8127 0.126 Uiso 0.490(6) 1 calc PR A 1 H17B H 0.1242 0.4439 0.8066 0.126 Uiso 0.490(6) 1 calc PR A 1 H17C H 0.2 0.4538 0.7667 0.126 Uiso 0.490(6) 1 calc PR A 1 C18A C 0.1364(6) 0.3866(3) 0.7511(3) 0.063(3) Uani 0.490(6) 1 d PD A 1 H18A H 0.1073 0.3607 0.7729 0.076 Uiso 0.490(6) 1 calc PR A 1 C19A C 0.2063(7) 0.3606(5) 0.7189(5) 0.083(4) Uani 0.490(6) 1 d PD A 1 H19A H 0.229 0.3843 0.6932 0.124 Uiso 0.490(6) 1 calc PR A 1 H19B H 0.1828 0.3314 0.7007 0.124 Uiso 0.490(6) 1 calc PR A 1 H19C H 0.2513 0.3496 0.7424 0.124 Uiso 0.490(6) 1 calc PR A 1 C17B C 0.1609(12) 0.4343(11) 0.7882(9) 0.112(12) Uani 0.510(6) 1 d PD A 2 H17D H 0.1678 0.4427 0.8254 0.167 Uiso 0.510(6) 1 calc PR A 2 H17E H 0.1872 0.4605 0.7667 0.167 Uiso 0.510(6) 1 calc PR A 2 H17F H 0.1879 0.4019 0.7811 0.167 Uiso 0.510(6) 1 calc PR A 2 C18B C 0.0670(6) 0.4309(4) 0.7751(3) 0.071(3) Uani 0.510(6) 1 d PD A 2 H18B H 0.0455 0.4659 0.7803 0.085 Uiso 0.510(6) 1 calc PR A 2 C19B C 0.0156(8) 0.3987(5) 0.8138(3) 0.094(4) Uani 0.510(6) 1 d PD A 2 H19D H 0.0378 0.3643 0.8141 0.141 Uiso 0.510(6) 1 calc PR A 2 H19E H -0.0434 0.3982 0.8028 0.141 Uiso 0.510(6) 1 calc PR A 2 H19F H 0.0198 0.4131 0.849 0.141 Uiso 0.510(6) 1 calc PR A 2 C20A C -0.0610(13) 0.4021(7) 0.7925(7) 0.168(10) Uani 0.490(6) 1 d PD A 1 H20A H -0.0792 0.4206 0.8237 0.252 Uiso 0.490(6) 1 calc PR A 1 H20B H -0.0167 0.3782 0.8021 0.252 Uiso 0.490(6) 1 calc PR A 1 H20C H -0.1089 0.3838 0.7776 0.252 Uiso 0.490(6) 1 calc PR A 1 C21A C -0.0271(7) 0.4389(4) 0.7521(4) 0.070(3) Uani 0.490(6) 1 d PD A 1 H21A H 0.0034 0.4643 0.7739 0.084 Uiso 0.490(6) 1 calc PR A 1 C22A C -0.0936(19) 0.4708(14) 0.7231(14) 0.112(12) Uani 0.490(6) 1 d PD A 1 H22A H -0.1183 0.451 0.6947 0.169 Uiso 0.490(6) 1 calc PR A 1 H22B H -0.0669 0.501 0.7086 0.169 Uiso 0.490(6) 1 calc PR A 1 H22C H -0.1379 0.4807 0.7477 0.169 Uiso 0.490(6) 1 calc PR A 1 C20B C -0.0974(7) 0.4134(5) 0.6422(4) 0.070(3) Uani 0.510(6) 1 d P A 2 H20D H -0.1583 0.4182 0.6388 0.105 Uiso 0.510(6) 1 calc PR A 2 H20E H -0.083 0.3786 0.6335 0.105 Uiso 0.510(6) 1 calc PR A 2 H20F H -0.0682 0.4362 0.6182 0.105 Uiso 0.510(6) 1 calc PR A 2 C21B C -0.0704(5) 0.4248(3) 0.6988(3) 0.055(2) Uani 0.510(6) 1 d P A 2 H21B H -0.0978 0.4001 0.7229 0.066 Uiso 0.510(6) 1 calc PR A 2 C22B C -0.0950(14) 0.4802(11) 0.7164(11) 0.067(4) Uani 0.510(6) 1 d P A 2 H22D H -0.0658 0.5046 0.6941 0.1 Uiso 0.510(6) 1 calc PR A 2 H22E H -0.0785 0.4854 0.7529 0.1 Uiso 0.510(6) 1 calc PR A 2 H22F H -0.1559 0.4848 0.7129 0.1 Uiso 0.510(6) 1 calc PR A 2 C23 C -0.1361(3) 0.61419(19) 0.68132(18) 0.0666(12) Uani 1 1 d . . . H23A H -0.1898 0.6038 0.6967 0.1 Uiso 1 1 calc R . . H23B H -0.1111 0.5858 0.6625 0.1 Uiso 1 1 calc R . . H23C H -0.1458 0.642 0.6569 0.1 Uiso 1 1 calc R . . C24 C -0.0762(2) 0.63139(15) 0.72491(15) 0.0494(9) Uani 1 1 d . . . H24 H -0.0715 0.6023 0.7495 0.059 Uiso 1 1 calc R . . C25 C -0.1172(3) 0.67441(17) 0.75684(17) 0.0622(11) Uani 1 1 d . . . H25A H -0.1256 0.7037 0.7341 0.093 Uiso 1 1 calc R . . H25B H -0.0802 0.6836 0.786 0.093 Uiso 1 1 calc R . . H25C H -0.1716 0.6632 0.7705 0.093 Uiso 1 1 calc R . . C26 C 0.1367(3) 0.72697(19) 0.6842(2) 0.0861(17) Uani 1 1 d . . . H26A H 0.1575 0.7127 0.6513 0.129 Uiso 1 1 calc R . . H26B H 0.1702 0.714 0.7134 0.129 Uiso 1 1 calc R . . H26C H 0.1414 0.7637 0.6829 0.129 Uiso 1 1 calc R . . C27 C 0.0437(3) 0.71206(15) 0.69191(17) 0.0590(11) Uani 1 1 d . . . H27 H 0.0224 0.7286 0.7245 0.071 Uiso 1 1 calc R . . C28 C -0.0099(3) 0.73024(18) 0.6455(2) 0.0814(16) Uani 1 1 d . . . H28A H -0.0054 0.7669 0.6424 0.122 Uiso 1 1 calc R . . H28B H -0.0688 0.7209 0.6512 0.122 Uiso 1 1 calc R . . H28C H 0.0105 0.7145 0.6131 0.122 Uiso 1 1 calc R . . C29 C 0.1061(3) 0.57059(15) 0.76583(16) 0.0581(11) Uani 1 1 d . . . H29A H 0.1519 0.5625 0.7901 0.087 Uiso 1 1 calc R . . H29B H 0.115 0.5529 0.7327 0.087 Uiso 1 1 calc R . . H29C H 0.0523 0.5601 0.7811 0.087 Uiso 1 1 calc R . . C30 C 0.1044(3) 0.62717(15) 0.75593(16) 0.0533(10) Uani 1 1 d . . . H30 H 0.1625 0.6365 0.7444 0.064 Uiso 1 1 calc R . . C31 C 0.0888(4) 0.65548(19) 0.80768(17) 0.0753(14) Uani 1 1 d . . . H31A H 0.0349 0.6448 0.8226 0.113 Uiso 1 1 calc R . . H31B H 0.0872 0.6917 0.8009 0.113 Uiso 1 1 calc R . . H31C H 0.1342 0.648 0.8324 0.113 Uiso 1 1 calc R . . C32 C 0.3159(3) 0.70236(17) 0.58498(19) 0.0657(12) Uani 1 1 d . . . H32A H 0.2824 0.7323 0.5752 0.079 Uiso 1 1 calc R . . H32B H 0.3013 0.6936 0.6216 0.079 Uiso 1 1 calc R . . C33 C 0.4099(4) 0.7166(3) 0.5830(2) 0.115(2) Uani 1 1 d . . . H33A H 0.4175 0.746 0.6063 0.138 Uiso 1 1 calc R . . H33B H 0.4416 0.6884 0.5988 0.138 Uiso 1 1 calc R . . C34 C 0.4485(4) 0.7279(3) 0.5365(3) 0.109(2) Uani 1 1 d . . . H34A H 0.4128 0.7528 0.5181 0.131 Uiso 1 1 calc R . . H34B H 0.4486 0.697 0.5149 0.131 Uiso 1 1 calc R . . C35 C 0.5376(4) 0.7484(2) 0.5371(3) 0.111(2) Uani 1 1 d . . . H35A H 0.5394 0.7792 0.558 0.167 Uiso 1 1 calc R . . H35B H 0.5554 0.7557 0.5012 0.167 Uiso 1 1 calc R . . H35C H 0.5754 0.7233 0.5525 0.167 Uiso 1 1 calc R . . C36 C 0.2931(3) 0.63984(16) 0.44898(15) 0.0537(10) Uani 1 1 d . . . H36A H 0.3534 0.6361 0.4402 0.064 Uiso 1 1 calc R . . H36B H 0.2626 0.6107 0.4342 0.064 Uiso 1 1 calc R . . C37 C 0.2593(3) 0.68854(17) 0.42379(16) 0.0628(11) Uani 1 1 d . . . H37A H 0.1985 0.6913 0.4317 0.075 Uiso 1 1 calc R . . H37B H 0.2877 0.7176 0.4404 0.075 Uiso 1 1 calc R . . C38 C 0.2708(3) 0.69223(19) 0.36530(17) 0.0708(13) Uani 1 1 d . . . H38A H 0.3317 0.6923 0.3572 0.085 Uiso 1 1 calc R . . H38B H 0.2457 0.6622 0.3486 0.085 Uiso 1 1 calc R . . C39 C 0.2313(4) 0.7385(2) 0.3423(2) 0.0992(19) Uani 1 1 d . . . H39A H 0.1707 0.7382 0.3493 0.149 Uiso 1 1 calc R . . H39B H 0.241 0.7391 0.3044 0.149 Uiso 1 1 calc R . . H39C H 0.2565 0.7685 0.3582 0.149 Uiso 1 1 calc R . . P1 P 0.29274(6) 0.42680(4) 0.50550(4) 0.0433(2) Uani 1 1 d . . . P2 P 0.05292(6) 0.41872(4) 0.70510(3) 0.0428(2) Uani 1 1 d . . . P3 P 0.03289(6) 0.64270(4) 0.69951(4) 0.0422(2) Uani 1 1 d . . . S1 S 0.35909(6) 0.56206(4) 0.56614(4) 0.0425(2) Uani 1 1 d . . . S2 S 0.25623(6) 0.48761(4) 0.65282(4) 0.0435(2) Uani 1 1 d . . . S3 S 0.03332(6) 0.52320(3) 0.59446(3) 0.0405(2) Uani 1 1 d . . . S4 S 0.11903(6) 0.63205(4) 0.55096(4) 0.0470(2) Uani 1 1 d . . . Cu1 Cu 0.28998(3) 0.485496(17) 0.567000(17) 0.04243(11) Uani 1 1 d . A . Cu2 Cu 0.11215(3) 0.477428(16) 0.652773(15) 0.03864(10) Uani 1 1 d . A . Cu3 Cu 0.06322(3) 0.599778(17) 0.627458(16) 0.04225(11) Uani 1 1 d . A . In1 In 0.278522(17) 0.639824(10) 0.534263(10) 0.04364(7) Uani 1 1 d . A . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.045(2) 0.058(2) 0.0399(19) -0.0002(17) -0.0069(17) -0.0156(18) C2 0.046(2) 0.053(2) 0.0324(17) -0.0044(16) 0.0000(17) -0.0034(18) C3 0.0335(19) 0.055(2) 0.0335(16) -0.0083(16) -0.0002(15) 0.0034(16) C4 0.036(2) 0.068(2) 0.0305(17) 0.0043(17) -0.0037(15) 0.0013(18) C5 0.085(4) 0.089(4) 0.065(3) 0.030(3) 0.009(3) 0.009(3) C6 0.071(3) 0.067(3) 0.050(2) 0.005(2) 0.019(2) 0.006(2) C7 0.065(4) 0.193(7) 0.088(4) 0.056(4) 0.013(3) -0.010(4) C8 0.054(3) 0.149(5) 0.085(4) 0.018(4) 0.002(3) 0.030(3) C9 0.073(3) 0.075(3) 0.063(3) -0.006(2) 0.005(2) 0.035(3) C10 0.116(5) 0.088(4) 0.107(4) 0.033(3) -0.009(4) 0.035(4) C11 0.138(5) 0.074(3) 0.058(3) -0.016(2) 0.005(3) -0.033(3) C12 0.074(3) 0.063(3) 0.049(2) -0.001(2) -0.005(2) -0.013(2) C13 0.055(3) 0.082(3) 0.077(3) -0.008(3) 0.008(2) -0.012(2) C14A 0.132(14) 0.022(6) 0.074(8) 0.003(5) 0.009(9) -0.018(8) C15A 0.070(7) 0.042(4) 0.047(5) 0.006(4) 0.009(4) -0.004(5) C16A 0.085(9) 0.068(7) 0.063(6) 0.009(5) -0.026(6) -0.032(6) C14B 0.096(10) 0.077(8) 0.096(9) 0.001(7) 0.004(7) 0.030(7) C15B 0.075(7) 0.055(5) 0.054(5) 0.007(4) 0.008(5) 0.000(5) C16B 0.19(3) 0.066(10) 0.149(19) 0.033(11) 0.092(18) 0.008(12) C17A 0.076(12) 0.107(16) 0.070(15) 0.047(12) -0.027(10) -0.034(11) C18A 0.068(6) 0.065(6) 0.057(5) 0.024(5) -0.019(5) -0.012(5) C19A 0.063(7) 0.082(8) 0.103(9) 0.027(7) 0.001(7) 0.025(6) C17B 0.15(2) 0.119(17) 0.064(14) -0.008(12) -0.062(13) -0.034(16) C18B 0.069(6) 0.114(8) 0.030(4) 0.002(4) -0.012(4) -0.021(6) C19B 0.109(10) 0.141(11) 0.033(4) 0.020(6) 0.020(6) -0.005(9) C20A 0.21(2) 0.137(13) 0.159(16) 0.069(12) 0.158(16) 0.070(14) C21A 0.089(8) 0.067(6) 0.054(5) 0.012(4) 0.026(5) 0.011(6) C22A 0.111(19) 0.09(2) 0.135(19) 0.031(13) 0.070(14) 0.029(14) C20B 0.056(6) 0.089(8) 0.065(6) 0.007(5) -0.030(5) -0.025(5) C21B 0.043(5) 0.070(6) 0.051(4) 0.019(4) 0.003(4) -0.023(4) C22B 0.050(9) 0.063(9) 0.087(10) 0.002(8) 0.023(8) -0.002(6) C23 0.046(3) 0.089(3) 0.065(3) -0.010(2) -0.003(2) 0.001(2) C24 0.043(2) 0.053(2) 0.053(2) -0.0008(18) 0.0073(18) 0.0002(18) C25 0.051(3) 0.073(3) 0.062(3) -0.002(2) 0.020(2) 0.010(2) C26 0.079(4) 0.068(3) 0.111(4) -0.009(3) 0.032(3) -0.024(3) C27 0.065(3) 0.044(2) 0.068(3) -0.006(2) 0.029(2) 0.002(2) C28 0.089(4) 0.064(3) 0.091(4) 0.024(3) 0.026(3) 0.023(3) C29 0.060(3) 0.060(3) 0.055(2) -0.008(2) -0.003(2) 0.009(2) C30 0.048(2) 0.057(2) 0.055(2) -0.0136(19) 0.004(2) -0.0027(19) C31 0.090(4) 0.079(3) 0.058(3) -0.027(2) -0.015(3) 0.007(3) C32 0.066(3) 0.057(3) 0.074(3) -0.014(2) 0.017(2) -0.012(2) C33 0.128(6) 0.119(5) 0.098(4) -0.045(4) 0.018(4) -0.066(4) C34 0.103(5) 0.112(5) 0.112(5) -0.019(4) 0.021(4) -0.050(4) C35 0.084(4) 0.108(5) 0.142(6) -0.013(4) 0.019(4) -0.044(4) C36 0.047(2) 0.064(2) 0.050(2) 0.0103(19) 0.0067(18) 0.000(2) C37 0.066(3) 0.068(3) 0.055(2) 0.002(2) 0.002(2) -0.004(2) C38 0.078(3) 0.074(3) 0.061(3) 0.011(2) 0.003(2) -0.014(3) C39 0.111(5) 0.095(4) 0.091(4) 0.038(3) -0.005(4) 0.005(4) P1 0.0463(6) 0.0448(5) 0.0389(5) -0.0033(4) 0.0077(4) 0.0049(4) P2 0.0470(6) 0.0492(5) 0.0321(4) 0.0026(4) 0.0034(4) -0.0141(5) P3 0.0425(5) 0.0409(5) 0.0433(5) -0.0072(4) 0.0108(4) 0.0000(4) S1 0.0387(5) 0.0480(5) 0.0410(5) 0.0054(4) 0.0057(4) -0.0022(4) S2 0.0374(5) 0.0490(5) 0.0440(5) 0.0068(4) 0.0021(4) -0.0068(4) S3 0.0370(5) 0.0444(5) 0.0401(4) 0.0006(4) 0.0056(4) 0.0011(4) S4 0.0456(6) 0.0454(5) 0.0501(5) 0.0075(4) 0.0106(4) 0.0041(4) Cu1 0.0363(2) 0.0466(3) 0.0444(2) -0.00799(19) -0.00308(19) 0.0043(2) Cu2 0.0402(2) 0.0434(2) 0.0323(2) -0.00076(18) 0.00285(19) -0.00891(19) Cu3 0.0386(2) 0.0502(3) 0.0379(2) -0.0068(2) 0.0053(2) 0.0053(2) In1 0.04455(15) 0.04259(14) 0.04376(13) 0.00675(12) 0.00562(12) -0.00439(12) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.517(5) . ? C1 S1 1.831(3) . ? C2 S2 1.828(4) . ? C3 C4 1.492(5) . ? C3 S3 1.834(3) . ? C4 S4 1.827(4) . ? C5 C6 1.523(7) . ? C6 C7 1.469(7) . ? C6 P1 1.860(4) . ? C8 C9 1.512(8) . ? C9 C10 1.544(7) . ? C9 P1 1.836(4) . ? C11 C12 1.549(6) . ? C12 C13 1.500(6) . ? C12 P1 1.863(5) . ? C14A C15A 1.530(11) . ? C15A C16A 1.546(10) . ? C15A P2 1.828(8) . ? C14B C15B 1.539(13) . ? C15B C16B 1.547(14) . ? C15B P2 1.781(9) . ? C17A C18A 1.534(15) . ? C18A C19A 1.530(12) . ? C18A P2 1.947(8) . ? C17B C18B 1.517(16) . ? C18B C19B 1.526(11) . ? C18B P2 1.812(7) . ? C20A C21A 1.505(12) . ? C21A C22A 1.529(16) . ? C21A P2 1.810(9) . ? C20B C21B 1.522(12) . ? C21B C22B 1.57(3) . ? C21B P2 1.954(8) . ? C23 C24 1.519(6) . ? C24 C25 1.533(5) . ? C24 P3 1.857(4) . ? C26 C27 1.528(6) . ? C27 C28 1.522(7) . ? C27 P3 1.844(4) . ? C29 C30 1.511(6) . ? C30 C31 1.526(5) . ? C30 P3 1.863(4) . ? C32 C33 1.526(8) . ? C32 In1 2.168(4) . ? C33 C34 1.356(8) . ? C34 C35 1.502(8) . ? C36 C37 1.528(6) . ? C36 In1 2.168(4) . ? C37 C38 1.493(6) . ? C38 C39 1.487(7) . ? P1 Cu1 2.1926(10) . ? P2 Cu2 2.2377(10) . ? P3 Cu3 2.1960(10) . ? S1 Cu1 2.2907(10) . ? S1 In1 2.5395(10) . ? S2 Cu1 2.2342(10) . ? S2 Cu2 2.2831(10) . ? S3 Cu3 2.2320(10) . ? S3 Cu2 2.2726(10) . ? S4 Cu3 2.2875(10) . ? S4 In1 2.5534(10) . ? 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 C2 C1 S1 112.4(2) . . ? C1 C2 S2 111.9(3) . . ? C4 C3 S3 112.9(2) . . ? C3 C4 S4 113.3(2) . . ? C7 C6 C5 109.4(4) . . ? C7 C6 P1 115.7(4) . . ? C5 C6 P1 110.3(3) . . ? C8 C9 C10 107.3(4) . . ? C8 C9 P1 110.6(4) . . ? C10 C9 P1 111.4(4) . . ? C13 C12 C11 112.1(4) . . ? C13 C12 P1 113.9(3) . . ? C11 C12 P1 113.9(4) . . ? C14A C15A C16A 112.6(10) . . ? C14A C15A P2 116.4(8) . . ? C16A C15A P2 108.7(6) . . ? C14B C15B C16B 109.8(12) . . ? C14B C15B P2 109.4(7) . . ? C16B C15B P2 121.0(12) . . ? C19A C18A C17A 112.7(12) . . ? C19A C18A P2 111.2(7) . . ? C17A C18A P2 106.8(11) . . ? C17B C18B C19B 114.1(13) . . ? C17B C18B P2 110.1(10) . . ? C19B C18B P2 117.5(7) . . ? C20A C21A C22A 115.8(16) . . ? C20A C21A P2 120.2(8) . . ? C22A C21A P2 108.9(15) . . ? C20B C21B C22B 112.2(11) . . ? C20B C21B P2 109.7(7) . . ? C22B C21B P2 107.3(9) . . ? C23 C24 C25 110.0(4) . . ? C23 C24 P3 111.8(3) . . ? C25 C24 P3 116.9(3) . . ? C28 C27 C26 110.5(4) . . ? C28 C27 P3 109.9(3) . . ? C26 C27 P3 110.8(3) . . ? C29 C30 C31 110.0(4) . . ? C29 C30 P3 110.7(3) . . ? C31 C30 P3 116.8(3) . . ? C33 C32 In1 115.5(3) . . ? C34 C33 C32 121.1(6) . . ? C33 C34 C35 119.3(6) . . ? C37 C36 In1 112.2(3) . . ? C38 C37 C36 115.2(4) . . ? C39 C38 C37 113.0(5) . . ? C9 P1 C6 105.7(2) . . ? C9 P1 C12 108.6(2) . . ? C6 P1 C12 99.9(2) . . ? C9 P1 Cu1 108.74(16) . . ? C6 P1 Cu1 116.44(15) . . ? C12 P1 Cu1 116.61(14) . . ? C15B P2 C21A 126.3(4) . . ? C15B P2 C18B 115.2(5) . . ? C21A P2 C18B 52.6(5) . . ? C15B P2 C15A 32.4(4) . . ? C21A P2 C15A 111.0(5) . . ? C18B P2 C15A 133.0(4) . . ? C15B P2 C18A 68.9(4) . . ? C21A P2 C18A 101.8(4) . . ? C18B P2 C18A 54.0(4) . . ? C15A P2 C18A 99.6(4) . . ? C15B P2 C21B 103.6(4) . . ? C21A P2 C21B 48.6(4) . . ? C18B P2 C21B 100.8(4) . . ? C15A P2 C21B 73.6(4) . . ? C18A P2 C21B 138.9(3) . . ? C15B P2 Cu2 113.7(3) . . ? C21A P2 Cu2 118.3(3) . . ? C18B P2 Cu2 113.8(3) . . ? C15A P2 Cu2 112.2(2) . . ? C18A P2 Cu2 111.8(3) . . ? C21B P2 Cu2 108.0(2) . . ? C27 P3 C24 106.25(18) . . ? C27 P3 C30 104.0(2) . . ? C24 P3 C30 105.02(19) . . ? C27 P3 Cu3 113.78(14) . . ? C24 P3 Cu3 113.90(13) . . ? C30 P3 Cu3 112.99(13) . . ? C1 S1 Cu1 96.65(12) . . ? C1 S1 In1 102.14(14) . . ? Cu1 S1 In1 118.39(4) . . ? C2 S2 Cu1 97.40(11) . . ? C2 S2 Cu2 107.54(13) . . ? Cu1 S2 Cu2 103.46(4) . . ? C3 S3 Cu3 97.28(12) . . ? C3 S3 Cu2 106.57(12) . . ? Cu3 S3 Cu2 96.98(4) . . ? C4 S4 Cu3 96.87(12) . . ? C4 S4 In1 102.73(12) . . ? Cu3 S4 In1 123.15(4) . . ? P1 Cu1 S2 135.30(4) . . ? P1 Cu1 S1 127.17(4) . . ? S2 Cu1 S1 95.75(4) . . ? P2 Cu2 S3 121.49(4) . . ? P2 Cu2 S2 119.64(4) . . ? S3 Cu2 S2 118.69(4) . . ? P3 Cu3 S3 136.80(4) . . ? P3 Cu3 S4 126.40(4) . . ? S3 Cu3 S4 95.77(4) . . ? C36 In1 C32 124.00(17) . . ? C36 In1 S1 105.24(11) . . ? C32 In1 S1 106.80(14) . . ? C36 In1 S4 105.57(11) . . ? C32 In1 S4 103.29(12) . . ? S1 In1 S4 111.95(3) . . ? _chemical_name_common ; bis(mu!3$-1,2-dithiolatoethane-S,S,S',S')-di(butan-1-ido) - tris(triisopropylphosphine)-copper(+1)-indium(+3) ; data_[iPr3PCuSC2H4SGaEt2]2 _database_code_depnum_ccdc_archive 'CCDC 907031' #TrackingRef '17791_web_deposit_cif_file_0_DirkFriedrich_1360944977.37_[iPr3PCuSC2H4SGaEt2]2.cif' _audit_creation_date 2012-10-12T09:29:47-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; bis(\m~3~-1,2-dithiolatoethane-S,S,S',S')-tetraethanido -bis(triisopropylphosphine)-dicopper(+1)-digallium(+3) ; _chemical_formula_moiety 'C30 H70 Cu2 Ga2 P2 S4' _chemical_formula_sum 'C30 H70 Cu2 Ga2 P2 S4' _chemical_formula_weight 887.56 _chemical_compound_source 'synthesis as described' _chemical_absolute_configuration ad #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21 1' _symmetry_space_group_name_Hall 'P 2yb' _symmetry_Int_Tables_number 4 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 10.9836(7) _cell_length_b 15.1580(7) _cell_length_c 13.1324(8) _cell_angle_alpha 90 _cell_angle_beta 107.200(5) _cell_angle_gamma 90 _cell_volume 2088.6(2) _cell_formula_units_Z 2 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 27320 _cell_measurement_theta_min 2.11 _cell_measurement_theta_max 29.39 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description cuboid _exptl_crystal_colour colorless _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.22 _exptl_crystal_density_diffrn 1.411 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 928 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 2.58 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details ; Busing, W. R. & Levy, H. A. (1957) Acta Cryst. 10, 180-182. and Coppens, P., Leiserowitz, L. & Rabinovich, D. (1965) Acta Cryst. 1965, 1035-1038. ; _exptl_absorpt_correction_T_min 0.5883 _exptl_absorpt_correction_T_max 0.6429 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 110(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 '2-circle goniometer' _diffrn_measurement_device_type 'STOE IPDS-2T' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 6.67 _diffrn_detector 'image plate (34 cm diameter / schwenk)' _diffrn_detector_type STOE _diffrn_standards_number 0 _diffrn_reflns_av_R_equivalents 0.0235 _diffrn_reflns_av_unetI/netI 0.0302 _diffrn_reflns_number 23990 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.11 _diffrn_reflns_theta_max 29.11 _diffrn_reflns_theta_full 29.11 _diffrn_measured_fraction_theta_full 0.991 _diffrn_measured_fraction_theta_max 0.991 _reflns_number_total 11017 _reflns_number_gt 10118 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_cell_refinement 'STOE X-AREA' _computing_data_reduction 'STOE X-AREA, STOE X-RED' _computing_structure_solution ; 'SIR-92' Altomare, A., Cascarano, G., Giacovazzo, C. & Guagliardi, A. (1993) J. Appl. Cryst. 26, 343-350. ; _computing_structure_refinement ; 'SHELXL-97' Sheldrick, G.M. (2008) Acta Cryst. A64, 112 ; _computing_molecular_graphics 'DIAMOND 3.2' _computing_publication_material ; 'WinGX publication routines' Farrugia, L. J. (1999) WinGX, J. Appl. Cryst. 32, 837-838 ; #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0298P)^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_number_reflns 11017 _refine_ls_number_parameters 378 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0268 _refine_ls_R_factor_gt 0.023 _refine_ls_wR_factor_ref 0.0502 _refine_ls_wR_factor_gt 0.0494 _refine_ls_goodness_of_fit_ref 0.974 _refine_ls_restrained_S_all 0.974 _refine_ls_shift/su_max 0.014 _refine_ls_shift/su_mean 0.001 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.439(5) _refine_diff_density_max 0.248 _refine_diff_density_min -0.438 _refine_diff_density_rms 0.058 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.8695(2) 0.08884(15) 0.87822(18) 0.0141(4) Uani 1 1 d . . . H1A H 0.9032 0.0742 0.9549 0.017 Uiso 1 1 calc R . . H1B H 0.7801 0.1084 0.8643 0.017 Uiso 1 1 calc R . . C2 C 0.8725(2) 0.00584(15) 0.81232(19) 0.0161(4) Uani 1 1 d . . . H2A H 0.8158 -0.0392 0.8287 0.019 Uiso 1 1 calc R . . H2B H 0.9602 -0.0183 0.8338 0.019 Uiso 1 1 calc R . . C3 C 0.6172(2) 0.24116(15) 0.65422(19) 0.0151(4) Uani 1 1 d . . . H3A H 0.7057 0.2197 0.6678 0.018 Uiso 1 1 calc R . . H3B H 0.5834 0.2549 0.5773 0.018 Uiso 1 1 calc R . . C4 C 0.6185(2) 0.32561(15) 0.71844(19) 0.0163(4) Uani 1 1 d . . . H4A H 0.5324 0.3522 0.6956 0.02 Uiso 1 1 calc R . . H4B H 0.6782 0.3682 0.7016 0.02 Uiso 1 1 calc R . . C9 C 0.9231(2) 0.26224(18) 1.08371(19) 0.0198(5) Uani 1 1 d . . . H9A H 0.8984 0.3114 1.1232 0.024 Uiso 1 1 calc R . . H9B H 0.8675 0.2113 1.086 0.024 Uiso 1 1 calc R . . C10 C 1.0632(3) 0.2366(2) 1.1407(2) 0.0303(6) Uani 1 1 d . . . H10A H 1.0874 0.1862 1.104 0.045 Uiso 1 1 calc R . . H10B H 1.0718 0.2205 1.2148 0.045 Uiso 1 1 calc R . . H10C H 1.1189 0.2867 1.1393 0.045 Uiso 1 1 calc R . . C11 C 0.9828(2) 0.40446(15) 0.9000(2) 0.0193(5) Uani 1 1 d . . . H11A H 0.9879 0.4484 0.9569 0.023 Uiso 1 1 calc R . . H11B H 1.0712 0.3865 0.9056 0.023 Uiso 1 1 calc R . . C12 C 0.9284(3) 0.4513(2) 0.7926(2) 0.0325(6) Uani 1 1 d . . . H12A H 0.9203 0.409 0.7346 0.049 Uiso 1 1 calc R . . H12B H 0.9859 0.4991 0.7864 0.049 Uiso 1 1 calc R . . H12C H 0.8444 0.4757 0.7882 0.049 Uiso 1 1 calc R . . C7 C 0.5456(2) 0.04594(18) 0.4587(2) 0.0231(5) Uani 1 1 d . . . H7A H 0.5969 0.0952 0.4436 0.028 Uiso 1 1 calc R . . H7B H 0.5675 -0.0078 0.4249 0.028 Uiso 1 1 calc R . . C8 C 0.4035(3) 0.0668(2) 0.4066(2) 0.0311(6) Uani 1 1 d . . . H8A H 0.3518 0.0168 0.4168 0.047 Uiso 1 1 calc R . . H8B H 0.3881 0.0772 0.3302 0.047 Uiso 1 1 calc R . . H8C H 0.3803 0.1196 0.4397 0.047 Uiso 1 1 calc R . . C5 C 0.5438(2) -0.07416(15) 0.6920(2) 0.0183(4) Uani 1 1 d . . . H5A H 0.5793 -0.0652 0.7698 0.022 Uiso 1 1 calc R . . H5B H 0.4497 -0.0745 0.6747 0.022 Uiso 1 1 calc R . . C6 C 0.5877(3) -0.16440(17) 0.6629(2) 0.0256(5) Uani 1 1 d . . . H6A H 0.5537 -0.1737 0.5858 0.038 Uiso 1 1 calc R . . H6B H 0.5564 -0.211 0.7005 0.038 Uiso 1 1 calc R . . H6C H 0.681 -0.1661 0.6838 0.038 Uiso 1 1 calc R . . C13 C 0.7878(2) 0.32655(18) 0.4809(2) 0.0238(5) Uani 1 1 d . . . H13A H 0.7509 0.3822 0.448 0.036 Uiso 1 1 calc R . . H13B H 0.7863 0.3249 0.5551 0.036 Uiso 1 1 calc R . . H13C H 0.7381 0.2771 0.4416 0.036 Uiso 1 1 calc R . . C14 C 0.9265(2) 0.31936(15) 0.47770(19) 0.0155(4) Uani 1 1 d . . . H14 H 0.9729 0.371 0.5188 0.019 Uiso 1 1 calc R . . C15 C 0.9317(3) 0.33088(18) 0.3622(2) 0.0221(5) Uani 1 1 d . . . H15A H 0.883 0.2835 0.3175 0.033 Uiso 1 1 calc R . . H15B H 1.0205 0.3284 0.3613 0.033 Uiso 1 1 calc R . . H15C H 0.8948 0.3881 0.3345 0.033 Uiso 1 1 calc R . . C16 C 1.1909(2) 0.31212(18) 0.7089(2) 0.0245(5) Uani 1 1 d . . . H16A H 1.2816 0.3205 0.7462 0.037 Uiso 1 1 calc R . . H16B H 1.149 0.2849 0.7574 0.037 Uiso 1 1 calc R . . H16C H 1.1513 0.3694 0.6849 0.037 Uiso 1 1 calc R . . C17 C 1.1761(2) 0.25155(16) 0.61168(19) 0.0162(4) Uani 1 1 d . . . H17 H 1.2242 0.1963 0.6393 0.019 Uiso 1 1 calc R . . C18 C 1.2398(2) 0.29223(19) 0.5331(2) 0.0226(5) Uani 1 1 d . . . H18A H 1.1982 0.3483 0.5062 0.034 Uiso 1 1 calc R . . H18B H 1.2316 0.2516 0.4733 0.034 Uiso 1 1 calc R . . H18C H 1.3303 0.3027 0.5696 0.034 Uiso 1 1 calc R . . C19 C 0.8759(3) 0.10080(17) 0.3884(2) 0.0239(5) Uani 1 1 d . . . H19A H 0.8792 0.0621 0.3296 0.036 Uiso 1 1 calc R . . H19B H 0.8182 0.1502 0.3604 0.036 Uiso 1 1 calc R . . H19C H 0.8447 0.0674 0.4396 0.036 Uiso 1 1 calc R . . C20 C 1.0114(2) 0.13676(15) 0.44494(19) 0.0173(4) Uani 1 1 d . . . H20 H 1.045 0.1667 0.3909 0.021 Uiso 1 1 calc R . . C21 C 1.1020(3) 0.06052(17) 0.4961(2) 0.0252(5) Uani 1 1 d . . . H21A H 1.0746 0.0345 0.554 0.038 Uiso 1 1 calc R . . H21B H 1.189 0.0833 0.5247 0.038 Uiso 1 1 calc R . . H21C H 1.1 0.0154 0.4421 0.038 Uiso 1 1 calc R . . C22 C 0.6964(2) 0.01691(17) 1.0625(2) 0.0221(5) Uani 1 1 d . . . H22A H 0.7439 0.0691 1.0966 0.033 Uiso 1 1 calc R . . H22B H 0.6989 0.0131 0.9886 0.033 Uiso 1 1 calc R . . H22C H 0.7351 -0.0361 1.1014 0.033 Uiso 1 1 calc R . . C23 C 0.5566(2) 0.02426(16) 1.06362(18) 0.0143(4) Uani 1 1 d . . . H23 H 0.5116 -0.0289 1.0252 0.017 Uiso 1 1 calc R . . C24 C 0.5502(2) 0.01733(17) 1.1791(2) 0.0204(5) Uani 1 1 d . . . H24A H 0.5952 -0.0359 1.2125 0.031 Uiso 1 1 calc R . . H24B H 0.4609 0.0141 1.1786 0.031 Uiso 1 1 calc R . . H24C H 0.5904 0.0694 1.2195 0.031 Uiso 1 1 calc R . . C25 C 0.2948(2) 0.02313(19) 0.8299(2) 0.0262(5) Uani 1 1 d . . . H25A H 0.3356 -0.0331 0.8571 0.039 Uiso 1 1 calc R . . H25B H 0.3367 0.0488 0.7805 0.039 Uiso 1 1 calc R . . H25C H 0.2045 0.0131 0.7924 0.039 Uiso 1 1 calc R . . C26 C 0.3068(2) 0.08691(16) 0.9235(2) 0.0158(4) Uani 1 1 d . . . H26 H 0.2573 0.141 0.8929 0.019 Uiso 1 1 calc R . . C27 C 0.2438(2) 0.04826(17) 1.0032(2) 0.0214(5) Uani 1 1 d . . . H27A H 0.1526 0.0395 0.9679 0.032 Uiso 1 1 calc R . . H27B H 0.255 0.089 1.0632 0.032 Uiso 1 1 calc R . . H27C H 0.2834 -0.0085 1.0295 0.032 Uiso 1 1 calc R . . C28 C 0.5988(2) 0.24786(16) 1.1395(2) 0.0208(5) Uani 1 1 d . . . H28A H 0.6316 0.2762 1.0859 0.031 Uiso 1 1 calc R . . H28B H 0.6571 0.2007 1.1749 0.031 Uiso 1 1 calc R . . H28C H 0.592 0.2917 1.1924 0.031 Uiso 1 1 calc R . . C29 C 0.4652(2) 0.20818(14) 1.08445(19) 0.0149(4) Uani 1 1 d . . . H29 H 0.4321 0.1799 1.1398 0.018 Uiso 1 1 calc R . . C30 C 0.3723(3) 0.28254(16) 1.0290(2) 0.0233(5) Uani 1 1 d . . . H30A H 0.3751 0.3303 1.08 0.035 Uiso 1 1 calc R . . H30B H 0.2855 0.2589 1.0036 0.035 Uiso 1 1 calc R . . H30C H 0.3976 0.3054 0.9685 0.035 Uiso 1 1 calc R . . P1 P 1.00586(5) 0.21816(4) 0.54992(4) 0.01136(10) Uani 1 1 d . . . P2 P 0.47588(5) 0.12302(4) 0.98534(4) 0.01117(10) Uani 1 1 d . . . S1 S 0.96349(5) 0.17975(4) 0.84745(4) 0.01270(10) Uani 1 1 d . . . S2 S 0.82231(5) 0.02602(4) 0.66686(4) 0.01442(10) Uani 1 1 d . . . S3 S 0.52034(5) 0.15320(4) 0.68745(4) 0.01354(10) Uani 1 1 d . . . S4 S 0.66585(5) 0.30844(4) 0.86465(4) 0.01341(10) Uani 1 1 d . . . Cu1 Cu 0.92288(2) 0.159130(17) 0.66852(2) 0.01283(6) Uani 1 1 d . . . Cu2 Cu 0.56089(2) 0.177602(17) 0.86564(2) 0.01262(5) Uani 1 1 d . . . Ga2 Ga 0.89239(2) 0.298870(15) 0.931681(19) 0.01282(5) Uani 1 1 d . . . Ga1 Ga 0.59544(2) 0.027013(15) 0.616972(19) 0.01363(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0132(9) 0.0157(10) 0.0131(10) 0.0025(8) 0.0035(8) -0.0015(8) C2 0.0162(10) 0.0150(11) 0.0163(11) 0.0023(8) 0.0037(9) -0.0002(8) C3 0.0152(10) 0.0176(11) 0.0132(11) 0.0023(8) 0.0054(9) 0.0011(8) C4 0.0162(10) 0.0146(10) 0.0167(11) 0.0043(8) 0.0028(9) 0.0019(8) C9 0.0190(11) 0.0294(12) 0.0114(10) -0.0010(9) 0.0052(8) -0.0010(9) C10 0.0256(13) 0.0469(17) 0.0170(13) 0.0040(11) 0.0044(10) 0.0095(12) C11 0.0193(11) 0.0179(11) 0.0226(12) -0.0029(9) 0.0092(9) -0.0050(8) C12 0.0334(14) 0.0322(15) 0.0305(15) 0.0110(12) 0.0073(12) -0.0111(12) C7 0.0212(11) 0.0334(14) 0.0151(11) -0.0019(10) 0.0061(9) 0.0022(10) C8 0.0246(13) 0.0490(17) 0.0178(12) -0.0057(12) 0.0032(10) 0.0048(12) C5 0.0178(10) 0.0176(10) 0.0219(12) -0.0028(9) 0.0094(9) -0.0043(8) C6 0.0332(13) 0.0192(11) 0.0287(14) -0.0018(10) 0.0160(11) -0.0023(10) C13 0.0159(11) 0.0285(13) 0.0270(13) 0.0048(10) 0.0064(10) 0.0059(9) C14 0.0150(10) 0.0144(10) 0.0173(11) 0.0025(8) 0.0049(8) 0.0013(8) C15 0.0266(12) 0.0238(12) 0.0153(12) 0.0070(9) 0.0053(10) 0.0020(10) C16 0.0224(12) 0.0277(14) 0.0211(12) -0.0045(10) 0.0028(10) -0.0091(10) C17 0.0134(10) 0.0173(11) 0.0172(11) 0.0025(9) 0.0035(9) -0.0021(8) C18 0.0158(10) 0.0275(13) 0.0260(13) 0.0062(11) 0.0087(9) -0.0037(10) C19 0.0277(12) 0.0240(12) 0.0196(13) -0.0065(9) 0.0062(10) -0.0077(10) C20 0.0221(11) 0.0163(11) 0.0156(11) -0.0017(8) 0.0087(9) -0.0004(8) C21 0.0307(13) 0.0179(11) 0.0302(14) -0.0026(10) 0.0139(11) 0.0035(10) C22 0.0166(10) 0.0226(12) 0.0284(13) 0.0074(10) 0.0089(10) 0.0053(9) C23 0.0140(9) 0.0143(9) 0.0149(10) 0.0025(9) 0.0048(8) 0.0023(8) C24 0.0195(11) 0.0234(12) 0.0189(11) 0.0073(10) 0.0062(9) 0.0023(9) C25 0.0230(12) 0.0269(13) 0.0263(13) -0.0076(12) 0.0034(10) -0.0075(11) C26 0.0125(10) 0.0157(10) 0.0182(11) 0.0015(9) 0.0032(9) -0.0006(8) C27 0.0130(10) 0.0231(12) 0.0281(13) 0.0067(10) 0.0059(9) -0.0003(9) C28 0.0220(12) 0.0218(12) 0.0185(12) -0.0062(9) 0.0060(9) -0.0078(9) C29 0.0176(10) 0.0143(10) 0.0140(10) -0.0019(8) 0.0066(9) -0.0009(8) C30 0.0272(12) 0.0163(11) 0.0270(13) -0.0017(9) 0.0089(10) 0.0050(9) P1 0.0121(2) 0.0121(2) 0.0103(2) 0.0006(2) 0.0041(2) -0.00076(19) P2 0.0115(2) 0.0114(2) 0.0113(3) -0.00010(19) 0.0045(2) -0.00034(19) S1 0.0126(2) 0.0142(2) 0.0119(2) 0.0000(2) 0.00469(18) -0.00047(19) S2 0.0149(2) 0.0142(2) 0.0152(2) -0.0015(2) 0.00582(19) -0.0016(2) S3 0.0137(2) 0.0154(2) 0.0119(2) -0.00160(19) 0.00450(19) -0.00069(19) S4 0.0132(2) 0.0133(2) 0.0141(2) -0.00136(19) 0.00459(19) -0.00144(19) Cu1 0.01308(12) 0.01468(13) 0.01193(13) 0.00165(10) 0.00556(10) -0.00022(10) Cu2 0.01303(11) 0.01408(13) 0.01187(12) 0.00099(10) 0.00540(10) -0.00011(9) Ga2 0.01266(10) 0.01468(11) 0.01139(11) -0.00137(9) 0.00397(9) -0.00172(9) Ga1 0.01407(11) 0.01506(11) 0.01175(11) -0.00187(9) 0.00381(9) -0.00171(9) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.533(3) . ? C1 S1 1.837(2) . ? C2 S2 1.850(2) . ? C3 C4 1.531(3) . ? C3 S3 1.837(2) . ? C4 S4 1.853(2) . ? C9 C10 1.548(3) . ? C9 Ga2 2.002(2) . ? C11 C12 1.533(4) . ? C11 Ga2 1.992(2) . ? C7 C8 1.540(4) . ? C7 Ga1 2.007(2) . ? C5 C6 1.536(3) . ? C5 Ga1 1.994(2) . ? C13 C14 1.540(3) . ? C14 C15 1.545(3) . ? C14 P1 1.877(2) . ? C16 C17 1.542(3) . ? C17 C18 1.537(3) . ? C17 P1 1.875(2) . ? C19 C20 1.552(3) . ? C20 C21 1.543(3) . ? C20 P1 1.864(2) . ? C22 C23 1.544(3) . ? C23 C24 1.542(3) . ? C23 P2 1.883(2) . ? C25 C26 1.539(3) . ? C26 C27 1.532(3) . ? C26 P2 1.875(2) . ? C28 C29 1.553(3) . ? C29 C30 1.549(3) . ? C29 P2 1.861(2) . ? P1 Cu1 2.2129(6) . ? P2 Cu2 2.2125(6) . ? S1 Cu1 2.2800(6) . ? S1 Ga2 2.3675(6) . ? S2 Cu1 2.2973(6) . ? S2 Ga1 2.3819(6) . ? S3 Cu2 2.2792(6) . ? S3 Ga1 2.3764(6) . ? S4 Cu2 2.2959(6) . ? S4 Ga2 2.3857(6) . ? 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 C2 C1 S1 112.61(16) . . ? C1 C2 S2 113.42(15) . . ? C4 C3 S3 112.82(16) . . ? C3 C4 S4 114.05(15) . . ? C10 C9 Ga2 113.70(17) . . ? C12 C11 Ga2 118.80(17) . . ? C8 C7 Ga1 114.79(18) . . ? C6 C5 Ga1 113.95(16) . . ? C13 C14 C15 110.0(2) . . ? C13 C14 P1 111.06(16) . . ? C15 C14 P1 116.25(16) . . ? C18 C17 C16 111.1(2) . . ? C18 C17 P1 114.31(17) . . ? C16 C17 P1 111.48(16) . . ? C21 C20 C19 110.4(2) . . ? C21 C20 P1 109.35(17) . . ? C19 C20 P1 110.47(16) . . ? C24 C23 C22 109.84(19) . . ? C24 C23 P2 116.10(16) . . ? C22 C23 P2 111.17(16) . . ? C27 C26 C25 110.9(2) . . ? C27 C26 P2 113.93(17) . . ? C25 C26 P2 111.69(16) . . ? C30 C29 C28 109.69(19) . . ? C30 C29 P2 110.18(16) . . ? C28 C29 P2 110.34(16) . . ? C20 P1 C17 104.61(11) . . ? C20 P1 C14 106.20(11) . . ? C17 P1 C14 104.64(10) . . ? C20 P1 Cu1 111.29(8) . . ? C17 P1 Cu1 111.74(8) . . ? C14 P1 Cu1 117.37(8) . . ? C29 P2 C26 104.24(11) . . ? C29 P2 C23 106.65(10) . . ? C26 P2 C23 104.50(10) . . ? C29 P2 Cu2 111.39(8) . . ? C26 P2 Cu2 111.93(8) . . ? C23 P2 Cu2 117.11(7) . . ? C1 S1 Cu1 99.93(8) . . ? C1 S1 Ga2 100.66(8) . . ? Cu1 S1 Ga2 126.52(2) . . ? C2 S2 Cu1 98.04(7) . . ? C2 S2 Ga1 104.66(8) . . ? Cu1 S2 Ga1 117.26(3) . . ? C3 S3 Cu2 100.08(8) . . ? C3 S3 Ga1 101.51(8) . . ? Cu2 S3 Ga1 123.06(3) . . ? C4 S4 Cu2 98.03(8) . . ? C4 S4 Ga2 109.46(8) . . ? Cu2 S4 Ga2 114.59(2) . . ? P1 Cu1 S1 132.39(2) . . ? P1 Cu1 S2 130.20(2) . . ? S1 Cu1 S2 94.42(2) . . ? P2 Cu2 S3 132.33(2) . . ? P2 Cu2 S4 130.18(2) . . ? S3 Cu2 S4 94.61(2) . . ? C11 Ga2 C9 118.95(10) . . ? C11 Ga2 S1 105.15(7) . . ? C9 Ga2 S1 105.83(8) . . ? C11 Ga2 S4 113.84(7) . . ? C9 Ga2 S4 103.57(7) . . ? S1 Ga2 S4 109.03(2) . . ? C5 Ga1 C7 126.24(11) . . ? C5 Ga1 S3 104.15(7) . . ? C7 Ga1 S3 105.58(8) . . ? C5 Ga1 S2 106.67(7) . . ? C7 Ga1 S2 103.20(7) . . ? S3 Ga1 S2 110.69(2) . . ? _chemical_name_common ; bis(mu!3$-1,2-dithiolatoethane-S,S,S',S')-tetraethanido - bis(triisopropylphosphine)-dicopper(+1)-digallium(+3) ; data_[iPr3PCuSC2H4SGaiPr2]2 _database_code_depnum_ccdc_archive 'CCDC 907032' #TrackingRef '17792_web_deposit_cif_file_0_DirkFriedrich_1360945041.38_[iPr3PCuSC2H4SGaiPr2]2.cif' _audit_creation_date 2012-10-12T10:26:29-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; bis(\m~3~-1,2-dithiolatoethane-S,S,S',S')-tetra(propan-2-ido) -bis(triisopropylphosphine)-dicopper(+1)-digallium(+3) ; _chemical_formula_moiety 'C34 H78 Cu2 Ga2 P2 S4' _chemical_formula_sum 'C34 H78 Cu2 Ga2 P2 S4' _chemical_formula_weight 943.66 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.4082(9) _cell_length_b 11.7713(12) _cell_length_c 13.4698(15) _cell_angle_alpha 65.472(8) _cell_angle_beta 72.916(9) _cell_angle_gamma 86.325(9) _cell_volume 1156.8(2) _cell_formula_units_Z 1 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 9727 _cell_measurement_theta_min 1.9 _cell_measurement_theta_max 29.3 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description platelet _exptl_crystal_colour colorless _exptl_crystal_size_max 0.273 _exptl_crystal_size_mid 0.128 _exptl_crystal_size_min 0.065 _exptl_crystal_density_diffrn 1.355 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 496 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 2.33 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details ; Busing, W. R. & Levy, H. A. (1957) Acta Cryst. 10, 180-182. and Coppens, P., Leiserowitz, L. & Rabinovich, D. (1965) Acta Cryst. 1965, 1035-1038. ; _exptl_absorpt_correction_T_min 0.5932 _exptl_absorpt_correction_T_max 0.8678 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 180(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 '2-circle goniometer' _diffrn_measurement_device_type 'STOE IPDS-2T' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 6.67 _diffrn_detector 'image plate (34 cm diameter / schwenk)' _diffrn_detector_type STOE _diffrn_standards_number 0 _diffrn_reflns_av_R_equivalents 0.0485 _diffrn_reflns_av_unetI/netI 0.065 _diffrn_reflns_number 12635 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.91 _diffrn_reflns_theta_max 29 _diffrn_reflns_theta_full 29 _diffrn_measured_fraction_theta_full 0.981 _diffrn_measured_fraction_theta_max 0.981 _reflns_number_total 6045 _reflns_number_gt 4247 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_cell_refinement 'STOE X-AREA' _computing_data_reduction 'STOE X-AREA, STOE X-RED' _computing_structure_solution ; 'SIR-92' Altomare, A., Cascarano, G., Giacovazzo, C. & Guagliardi, A. (1993) J. Appl. Cryst. 26, 343-350. ; _computing_structure_refinement ; 'SHELXL-97' Sheldrick, G.M. (2008) Acta Cryst. A64, 112 ; _computing_molecular_graphics 'DIAMOND 3.2' _computing_publication_material ; 'WinGX publication routines' Farrugia, L. J. (1999) WinGX, J. Appl. Cryst. 32, 837-838 ; #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0334P)^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_number_reflns 6045 _refine_ls_number_parameters 209 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0536 _refine_ls_R_factor_gt 0.0313 _refine_ls_wR_factor_ref 0.068 _refine_ls_wR_factor_gt 0.064 _refine_ls_goodness_of_fit_ref 0.839 _refine_ls_restrained_S_all 0.839 _refine_ls_shift/su_max 0.011 _refine_ls_shift/su_mean 0.001 _refine_diff_density_max 0.737 _refine_diff_density_min -0.788 _refine_diff_density_rms 0.083 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.7380(3) 0.5133(2) 0.5086(2) 0.0255(5) Uani 1 1 d . . . H1A H 0.8405 0.4702 0.5198 0.031 Uiso 1 1 calc R . . H1B H 0.6839 0.4726 0.4745 0.031 Uiso 1 1 calc R . . C2 C 0.7859(3) 0.6507(2) 0.4255(2) 0.0260(5) Uani 1 1 d . . . H2A H 0.8507 0.6546 0.3497 0.031 Uiso 1 1 calc R . . H2B H 0.8593 0.6865 0.4524 0.031 Uiso 1 1 calc R . . C3 C 0.3416(4) 0.2934(3) 0.9488(3) 0.0434(7) Uani 1 1 d . . . H3A H 0.2414 0.2907 1.0097 0.065 Uiso 1 1 calc R . . H3B H 0.3975 0.3775 0.9105 0.065 Uiso 1 1 calc R . . H3C H 0.4175 0.2325 0.9817 0.065 Uiso 1 1 calc R . . C4 C 0.2922(3) 0.2612(2) 0.8618(2) 0.0274(5) Uani 1 1 d . . . H4 H 0.2095 0.3215 0.8335 0.033 Uiso 1 1 calc R . . C5 C 0.2065(4) 0.1281(3) 0.9187(3) 0.0415(7) Uani 1 1 d . . . H5A H 0.2844 0.0669 0.9482 0.062 Uiso 1 1 calc R . . H5B H 0.1731 0.1107 0.8623 0.062 Uiso 1 1 calc R . . H5C H 0.1077 0.1221 0.9818 0.062 Uiso 1 1 calc R . . C6 C 0.7875(4) 0.2014(3) 0.8045(3) 0.0447(8) Uani 1 1 d . . . H6A H 0.7185 0.1766 0.8837 0.067 Uiso 1 1 calc R . . H6B H 0.8225 0.2906 0.7704 0.067 Uiso 1 1 calc R . . H6C H 0.8861 0.1524 0.8028 0.067 Uiso 1 1 calc R . . C7 C 0.6864(3) 0.1774(2) 0.7365(2) 0.0273(5) Uani 1 1 d . . . H7 H 0.7609 0.2001 0.657 0.033 Uiso 1 1 calc R . . C8 C 0.6295(4) 0.0376(2) 0.7883(3) 0.0390(7) Uani 1 1 d . . . H8A H 0.7275 -0.0121 0.7856 0.059 Uiso 1 1 calc R . . H8B H 0.5639 0.0242 0.7443 0.059 Uiso 1 1 calc R . . H8C H 0.561 0.0118 0.8677 0.059 Uiso 1 1 calc R . . C9 C 0.2944(4) 0.9706(2) 0.5059(2) 0.0330(6) Uani 1 1 d . . . H9A H 0.2059 0.95 0.4811 0.05 Uiso 1 1 calc R . . H9B H 0.3982 0.9366 0.4766 0.05 Uiso 1 1 calc R . . H9C H 0.3112 1.0617 0.4763 0.05 Uiso 1 1 calc R . . C10 C 0.2444(3) 0.9132(2) 0.6369(2) 0.0261(5) Uani 1 1 d . . . H10 H 0.3349 0.9418 0.6573 0.031 Uiso 1 1 calc R . . C11 C 0.0835(4) 0.9684(2) 0.6849(3) 0.0351(6) Uani 1 1 d . . . H11A H 0.1029 1.0592 0.6563 0.053 Uiso 1 1 calc R . . H11B H 0.0526 0.9306 0.7685 0.053 Uiso 1 1 calc R . . H11C H -0.007 0.9504 0.6604 0.053 Uiso 1 1 calc R . . C12 C -0.0298(4) 0.7155(3) 0.6273(3) 0.0390(7) Uani 1 1 d . . . H12A H 0.0451 0.6775 0.5805 0.059 Uiso 1 1 calc R . . H12B H -0.0213 0.8066 0.5841 0.059 Uiso 1 1 calc R . . H12C H -0.1448 0.6832 0.6476 0.059 Uiso 1 1 calc R . . C13 C 0.0197(3) 0.6829(2) 0.7371(2) 0.0275(5) Uani 1 1 d . . . H13 H -0.0517 0.728 0.7809 0.033 Uiso 1 1 calc R . . C14 C -0.0112(4) 0.5419(3) 0.8115(3) 0.0507(9) Uani 1 1 d . . . H14A H -0.1274 0.516 0.8262 0.076 Uiso 1 1 calc R . . H14B H 0.0108 0.5228 0.8842 0.076 Uiso 1 1 calc R . . H14C H 0.0632 0.4966 0.7718 0.076 Uiso 1 1 calc R . . C15 C 0.1870(5) 0.7475(3) 0.9179(3) 0.0440(8) Uani 1 1 d . . . H15A H 0.2105 0.7072 0.9915 0.066 Uiso 1 1 calc R . . H15B H 0.0679 0.7342 0.9293 0.066 Uiso 1 1 calc R . . H15C H 0.2175 0.8374 0.8844 0.066 Uiso 1 1 calc R . . C16 C 0.2892(4) 0.6903(2) 0.8370(2) 0.0297(6) Uani 1 1 d . . . H16 H 0.2632 0.5978 0.8788 0.036 Uiso 1 1 calc R . . C17 C 0.4780(4) 0.7119(3) 0.8143(3) 0.0411(7) Uani 1 1 d . . . H17A H 0.5103 0.8017 0.7729 0.062 Uiso 1 1 calc R . . H17B H 0.5398 0.668 0.7684 0.062 Uiso 1 1 calc R . . H17C H 0.5039 0.6796 0.8871 0.062 Uiso 1 1 calc R . . P1 P 0.24178(8) 0.73738(5) 0.69852(5) 0.02083(13) Uani 1 1 d . . . S1 S 0.59533(8) 0.49472(5) 0.64876(5) 0.02267(12) Uani 1 1 d . . . S2 S 0.60649(8) 0.74802(5) 0.40961(5) 0.02294(13) Uani 1 1 d . . . Cu1 Cu 0.43402(4) 0.66063(3) 0.59295(3) 0.02224(8) Uani 1 1 d . . . Ga1 Ga 0.48981(4) 0.28298(2) 0.72694(2) 0.02088(7) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0222(13) 0.0282(11) 0.0314(14) -0.0178(10) -0.0079(11) 0.0038(10) C2 0.0227(13) 0.0310(12) 0.0253(13) -0.0123(10) -0.0067(10) -0.0020(10) C3 0.0477(19) 0.0571(18) 0.0302(15) -0.0271(14) -0.0044(14) -0.0001(15) C4 0.0282(14) 0.0315(12) 0.0218(12) -0.0119(10) -0.0065(11) 0.0068(10) C5 0.0358(17) 0.0421(15) 0.0378(17) -0.0154(13) 0.0013(14) -0.0044(13) C6 0.0377(18) 0.0472(17) 0.061(2) -0.0239(16) -0.0306(17) 0.0140(14) C7 0.0261(14) 0.0267(11) 0.0264(13) -0.0093(10) -0.0075(11) 0.0066(10) C8 0.0416(18) 0.0246(12) 0.0468(18) -0.0120(12) -0.0135(15) 0.0123(12) C9 0.0359(16) 0.0259(12) 0.0324(15) -0.0076(11) -0.0104(13) 0.0029(11) C10 0.0256(13) 0.0221(11) 0.0312(14) -0.0116(10) -0.0085(11) 0.0015(10) C11 0.0333(16) 0.0274(12) 0.0445(17) -0.0182(12) -0.0076(13) 0.0064(11) C12 0.0286(16) 0.0485(16) 0.0500(19) -0.0270(15) -0.0158(14) 0.0016(13) C13 0.0213(13) 0.0288(12) 0.0335(14) -0.0167(11) -0.0033(11) -0.0008(10) C14 0.0423(19) 0.0325(15) 0.067(2) -0.0088(15) -0.0168(17) -0.0100(14) C15 0.054(2) 0.0556(18) 0.0294(15) -0.0271(14) -0.0088(14) 0.0078(15) C16 0.0364(16) 0.0309(12) 0.0261(13) -0.0148(10) -0.0109(12) 0.0026(11) C17 0.0430(18) 0.0538(17) 0.0463(18) -0.0306(15) -0.0282(15) 0.0108(14) P1 0.0215(3) 0.0216(3) 0.0220(3) -0.0121(2) -0.0056(3) 0.0014(2) S1 0.0276(3) 0.0204(2) 0.0227(3) -0.0106(2) -0.0089(3) 0.0020(2) S2 0.0283(3) 0.0211(3) 0.0209(3) -0.0100(2) -0.0074(2) 0.0004(2) Cu1 0.02274(16) 0.02449(14) 0.02433(16) -0.01501(12) -0.00683(13) 0.00298(12) Ga1 0.02478(15) 0.01935(12) 0.01920(14) -0.00793(10) -0.00783(11) 0.00284(10) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.532(3) . ? C1 S1 1.847(3) . ? C2 S2 1.843(3) . ? C3 C4 1.537(4) . ? C4 C5 1.545(4) . ? C4 Ga1 2.005(3) . ? C6 C7 1.531(4) . ? C7 C8 1.541(3) . ? C7 Ga1 2.006(3) . ? C9 C10 1.535(4) . ? C10 C11 1.547(4) . ? C10 P1 1.882(2) . ? C12 C13 1.542(4) . ? C13 C14 1.533(4) . ? C13 P1 1.864(3) . ? C15 C16 1.536(4) . ? C16 C17 1.543(4) . ? C16 P1 1.870(3) . ? P1 Cu1 2.2316(7) . ? S1 Cu1 2.2933(7) . ? S1 Ga1 2.3799(7) . ? S2 Cu1 2.2886(8) . ? S2 Ga1 2.3754(7) 2_666 ? Ga1 S2 2.3754(7) 2_666 ? 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 C2 C1 S1 112.71(17) . . ? C1 C2 S2 114.09(18) . . ? C3 C4 C5 111.0(2) . . ? C3 C4 Ga1 111.02(19) . . ? C5 C4 Ga1 111.73(18) . . ? C6 C7 C8 110.6(2) . . ? C6 C7 Ga1 112.06(19) . . ? C8 C7 Ga1 110.47(18) . . ? C9 C10 C11 110.4(2) . . ? C9 C10 P1 111.63(17) . . ? C11 C10 P1 115.75(17) . . ? C14 C13 C12 109.9(2) . . ? C14 C13 P1 111.9(2) . . ? C12 C13 P1 109.46(19) . . ? C15 C16 C17 111.2(2) . . ? C15 C16 P1 116.7(2) . . ? C17 C16 P1 109.7(2) . . ? C13 P1 C16 105.77(12) . . ? C13 P1 C10 105.24(12) . . ? C16 P1 C10 105.25(11) . . ? C13 P1 Cu1 117.60(8) . . ? C16 P1 Cu1 107.31(9) . . ? C10 P1 Cu1 114.68(9) . . ? C1 S1 Cu1 100.34(9) . . ? C1 S1 Ga1 101.68(7) . . ? Cu1 S1 Ga1 122.62(3) . . ? C2 S2 Cu1 100.04(9) . . ? C2 S2 Ga1 105.87(8) . 2_666 ? Cu1 S2 Ga1 115.00(3) . 2_666 ? P1 Cu1 S2 133.10(3) . . ? P1 Cu1 S1 129.69(3) . . ? S2 Cu1 S1 93.62(3) . . ? C4 Ga1 C7 123.50(11) . . ? C4 Ga1 S2 107.92(8) . 2_666 ? C7 Ga1 S2 103.23(8) . 2_666 ? C4 Ga1 S1 106.13(7) . . ? C7 Ga1 S1 106.74(7) . . ? S2 Ga1 S1 108.72(2) 2_666 . ? _chemical_name_common ; bis(mu!3$-1,2-dithiolatoethane-S,S,S',S')-tetra(propan-2-ido) -bis(triisopropylphosphine)-dicopper(+1)-digallium(+3) ; data_[iPr3PCuSC2H4SInMe2]2 _database_code_depnum_ccdc_archive 'CCDC 907033' #TrackingRef '17793_web_deposit_cif_file_0_DirkFriedrich_1360945157.40_[iPr3PCuSC2H4SInMe2]2.cif' _audit_creation_date 2012-10-12T11:22:29-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; bis(\m~3~-1,2-dithiolatoethane-S,S,S',S')-tetramethanido -bis(triisopropylphosphine)-dicopper(+1)-diindium(+3) ; _chemical_formula_moiety 'C26 H62 Cu2 In2 P2 S4' _chemical_formula_sum 'C26 H62 Cu2 In2 P2 S4' _chemical_formula_weight 921.66 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_space_group_name_Hall '-P 2ybc' _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 11.8930(7) _cell_length_b 23.8556(10) _cell_length_c 15.1497(9) _cell_angle_alpha 90 _cell_angle_beta 113.804(4) _cell_angle_gamma 90 _cell_volume 3932.5(4) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 29570 _cell_measurement_theta_min 1.69 _cell_measurement_theta_max 28.36 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description cuboid _exptl_crystal_colour colorless _exptl_crystal_size_max 0.79 _exptl_crystal_size_mid 0.49 _exptl_crystal_size_min 0.38 _exptl_crystal_density_diffrn 1.557 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1872 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 2.53 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details ; Busing, W. R. & Levy, H. A. (1957) Acta Cryst. 10, 180-182. and Coppens, P., Leiserowitz, L. & Rabinovich, D. (1965) Acta Cryst. 1965, 1035-1038. ; _exptl_absorpt_correction_T_min 0.2820 _exptl_absorpt_correction_T_max 0.4733 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 180(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 '2-circle goniometer' _diffrn_measurement_device_type 'STOE IPDS-2T' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 6.67 _diffrn_detector 'image plate (34 cm diameter / schwenk)' _diffrn_detector_type STOE _diffrn_standards_number 0 _diffrn_reflns_av_R_equivalents 0.0588 _diffrn_reflns_av_unetI/netI 0.046 _diffrn_reflns_number 25509 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.7 _diffrn_reflns_theta_max 27.5 _diffrn_reflns_theta_full 27.5 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _reflns_number_total 9039 _reflns_number_gt 7606 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_cell_refinement 'STOE X-AREA' _computing_data_reduction 'STOE X-AREA, STOE X-RED' _computing_structure_solution ; 'SIR-92' Altomare, A., Cascarano, G., Giacovazzo, C. & Guagliardi, A. (1993) J. Appl. Cryst. 26, 343-350. ; _computing_structure_refinement ; 'SHELXL-97' Sheldrick, G.M. (2008) Acta Cryst. A64, 112 ; _computing_molecular_graphics 'DIAMOND 3.2' _computing_publication_material ; 'WinGX publication routines' Farrugia, L. J. (1999) WinGX, J. Appl. Cryst. 32, 837-838 ; #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0431P)^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_number_reflns 9039 _refine_ls_number_parameters 371 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0402 _refine_ls_R_factor_gt 0.0317 _refine_ls_wR_factor_ref 0.0799 _refine_ls_wR_factor_gt 0.0774 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.033 _refine_ls_shift/su_max 0.01 _refine_ls_shift/su_mean 0.001 _refine_diff_density_max 0.82 _refine_diff_density_min -1.273 _refine_diff_density_rms 0.122 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' In In -0.7276 1.31 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.5036(3) 0.58832(14) 0.0357(2) 0.0410(7) Uani 1 1 d . A . H1A H 0.5193 0.5475 0.0424 0.049 Uiso 1 1 calc R . . H1B H 0.4381 0.5952 -0.0291 0.049 Uiso 1 1 calc R . . C2 C 0.6187(3) 0.61772(13) 0.0428(2) 0.0381(6) Uani 1 1 d . A . H2A H 0.6412 0.6045 -0.0098 0.046 Uiso 1 1 calc R . . H2B H 0.6867 0.6078 0.1049 0.046 Uiso 1 1 calc R . . C3 C 0.8667(3) 0.70927(13) 0.3275(2) 0.0370(6) Uani 1 1 d . A . H3A H 0.9262 0.7097 0.3958 0.044 Uiso 1 1 calc R . . H3B H 0.8414 0.7485 0.3082 0.044 Uiso 1 1 calc R . . C4 C 0.7553(3) 0.67595(13) 0.31968(19) 0.0338(6) Uani 1 1 d . A . H4A H 0.69 0.6804 0.254 0.041 Uiso 1 1 calc R . . H4B H 0.7236 0.6908 0.3663 0.041 Uiso 1 1 calc R . . C5 C 0.8349(4) 0.81276(15) 0.1038(3) 0.0575(9) Uani 1 1 d . . . H5A H 0.9058 0.8272 0.0934 0.086 Uiso 1 1 calc R . . H5B H 0.844 0.8221 0.1694 0.086 Uiso 1 1 calc R . . H5C H 0.7595 0.8298 0.057 0.086 Uiso 1 1 calc R . . C6 C 0.8853(3) 0.66828(16) -0.0017(2) 0.0442(7) Uani 1 1 d . . . H6A H 0.8565 0.6834 -0.0673 0.066 Uiso 1 1 calc R . . H6B H 0.8514 0.6306 -0.0038 0.066 Uiso 1 1 calc R . . H6C H 0.9753 0.6664 0.0266 0.066 Uiso 1 1 calc R . . C7 C 0.6037(4) 0.47546(14) 0.2230(3) 0.0551(9) Uani 1 1 d . . . H7A H 0.6642 0.4536 0.2755 0.083 Uiso 1 1 calc R . . H7B H 0.6328 0.4808 0.1716 0.083 Uiso 1 1 calc R . . H7C H 0.5251 0.4554 0.1973 0.083 Uiso 1 1 calc R . . C8 C 0.5130(4) 0.5713(2) 0.3879(3) 0.0639(12) Uani 1 1 d . . . H8A H 0.4229 0.5716 0.3591 0.096 Uiso 1 1 calc R . . H8B H 0.5435 0.6076 0.4184 0.096 Uiso 1 1 calc R . . H8C H 0.5423 0.5416 0.4365 0.096 Uiso 1 1 calc R . . C9A C 0.3780(9) 0.7160(3) 0.3058(4) 0.053(2) Uani 0.614(18) 1 d PD A 1 H9A1 H 0.4563 0.7318 0.3507 0.079 Uiso 0.614(18) 1 calc PR A 1 H9A2 H 0.3939 0.6832 0.2736 0.079 Uiso 0.614(18) 1 calc PR A 1 H9A3 H 0.3289 0.7048 0.3414 0.079 Uiso 0.614(18) 1 calc PR A 1 C10A C 0.3081(9) 0.7599(4) 0.2305(6) 0.0415(18) Uani 0.614(18) 1 d PD A 1 H10A H 0.2266 0.7433 0.189 0.05 Uiso 0.614(18) 1 calc PR A 1 C11A C 0.283(2) 0.8124(6) 0.2766(17) 0.066(5) Uani 0.614(18) 1 d PD A 1 H11A H 0.2487 0.8018 0.3232 0.099 Uiso 0.614(18) 1 calc PR A 1 H11B H 0.2243 0.8363 0.2265 0.099 Uiso 0.614(18) 1 calc PR A 1 H11C H 0.36 0.833 0.3099 0.099 Uiso 0.614(18) 1 calc PR A 1 C9B C 0.295(3) 0.7129(6) 0.260(2) 0.119(12) Uani 0.386(18) 1 d PD A 2 H9B1 H 0.2847 0.7078 0.3208 0.179 Uiso 0.386(18) 1 calc PR A 2 H9B2 H 0.3454 0.6822 0.2527 0.179 Uiso 0.386(18) 1 calc PR A 2 H9B3 H 0.2147 0.7128 0.2061 0.179 Uiso 0.386(18) 1 calc PR A 2 C10B C 0.3595(18) 0.7686(5) 0.2632(15) 0.050(4) Uani 0.386(18) 1 d PD A 2 H10B H 0.4419 0.7662 0.3183 0.06 Uiso 0.386(18) 1 calc PR A 2 C11B C 0.289(3) 0.8151(10) 0.289(3) 0.065(9) Uani 0.386(18) 1 d PD A 2 H11D H 0.2743 0.8463 0.2436 0.097 Uiso 0.386(18) 1 calc PR A 2 H11E H 0.3377 0.8283 0.3547 0.097 Uiso 0.386(18) 1 calc PR A 2 H11F H 0.2103 0.8004 0.2851 0.097 Uiso 0.386(18) 1 calc PR A 2 C12 C 0.1878(4) 0.73887(17) -0.0107(3) 0.0617(11) Uani 1 1 d . . . H12A H 0.1452 0.7255 0.0287 0.093 Uiso 1 1 calc R . . H12B H 0.2441 0.7097 -0.0141 0.093 Uiso 1 1 calc R . . H12C H 0.1275 0.7475 -0.0759 0.093 Uiso 1 1 calc R . . C13 C 0.2598(3) 0.79096(15) 0.0341(2) 0.0464(8) Uani 1 1 d . A . H13 H 0.2987 0.803 -0.0103 0.056 Uiso 1 1 calc R . . C14 C 0.1756(4) 0.83951(17) 0.0347(3) 0.0645(11) Uani 1 1 d . . . H14A H 0.1154 0.8465 -0.0312 0.097 Uiso 1 1 calc R . . H14B H 0.225 0.8733 0.0599 0.097 Uiso 1 1 calc R . . H14C H 0.1326 0.8297 0.0758 0.097 Uiso 1 1 calc R . . C15 C 0.5925(4) 0.83261(19) 0.2748(3) 0.0614(10) Uani 1 1 d . . . H15A H 0.6443 0.8049 0.2615 0.092 Uiso 1 1 calc R . . H15B H 0.5717 0.8192 0.3276 0.092 Uiso 1 1 calc R . . H15C H 0.6369 0.8682 0.2934 0.092 Uiso 1 1 calc R . . C16 C 0.4743(3) 0.84134(13) 0.1842(2) 0.0412(7) Uani 1 1 d . A . H16 H 0.422 0.8698 0.1984 0.049 Uiso 1 1 calc R . . C17 C 0.5070(4) 0.86326(19) 0.1026(3) 0.0665(11) Uani 1 1 d . . . H17A H 0.5519 0.8987 0.1224 0.1 Uiso 1 1 calc R . . H17B H 0.4315 0.8694 0.0448 0.1 Uiso 1 1 calc R . . H17C H 0.5586 0.8357 0.0885 0.1 Uiso 1 1 calc R . . C18 C 1.1666(3) 0.58397(17) 0.2036(3) 0.0580(10) Uani 1 1 d . . . H18A H 1.2067 0.5896 0.2736 0.087 Uiso 1 1 calc R . . H18B H 1.0996 0.6111 0.1756 0.087 Uiso 1 1 calc R . . H18C H 1.2267 0.5893 0.1752 0.087 Uiso 1 1 calc R . . C19 C 1.1152(3) 0.52498(16) 0.1828(2) 0.0415(7) Uani 1 1 d . . . H19 H 1.07 0.5224 0.1111 0.05 Uiso 1 1 calc R . . C20 C 1.2198(3) 0.48163(18) 0.2110(3) 0.0543(9) Uani 1 1 d . . . H20A H 1.2743 0.4909 0.1789 0.081 Uiso 1 1 calc R . . H20B H 1.185 0.4442 0.191 0.081 Uiso 1 1 calc R . . H20C H 1.2667 0.4822 0.2811 0.081 Uiso 1 1 calc R . . C21 C 1.1660(3) 0.51033(17) 0.4251(2) 0.0517(9) Uani 1 1 d . . . H21A H 1.1217 0.5414 0.439 0.078 Uiso 1 1 calc R . . H21B H 1.2264 0.5253 0.4024 0.078 Uiso 1 1 calc R . . H21C H 1.2083 0.4883 0.4839 0.078 Uiso 1 1 calc R . . C22 C 1.0747(3) 0.47286(13) 0.3469(2) 0.0361(6) Uani 1 1 d . . . H22 H 1.1205 0.4408 0.3345 0.043 Uiso 1 1 calc R . . C23 C 0.9804(4) 0.44971(15) 0.3816(2) 0.0482(8) Uani 1 1 d . . . H23A H 1.0229 0.4323 0.4451 0.072 Uiso 1 1 calc R . . H23B H 0.9294 0.4217 0.3356 0.072 Uiso 1 1 calc R . . H23C H 0.9282 0.4803 0.3865 0.072 Uiso 1 1 calc R . . C24 C 0.9416(4) 0.40760(16) 0.1321(3) 0.0605(10) Uani 1 1 d . . . H24A H 0.8741 0.3822 0.0954 0.091 Uiso 1 1 calc R . . H24B H 0.9921 0.3906 0.1945 0.091 Uiso 1 1 calc R . . H24C H 0.9923 0.4145 0.0958 0.091 Uiso 1 1 calc R . . C25 C 0.8887(3) 0.46330(13) 0.1487(2) 0.0383(6) Uani 1 1 d . . . H25 H 0.8291 0.4533 0.1775 0.046 Uiso 1 1 calc R . . C26 C 0.8138(3) 0.49230(16) 0.0536(2) 0.0501(8) Uani 1 1 d . . . H26A H 0.8669 0.5008 0.0199 0.075 Uiso 1 1 calc R . . H26B H 0.7795 0.5272 0.0662 0.075 Uiso 1 1 calc R . . H26C H 0.7468 0.4676 0.0135 0.075 Uiso 1 1 calc R . . P1 P 0.38943(7) 0.77494(3) 0.15074(5) 0.02989(15) Uani 1 1 d . . . P2 P 0.99861(6) 0.51298(3) 0.23406(5) 0.02805(14) Uani 1 1 d . . . S1 S 0.44903(7) 0.61089(3) 0.12653(5) 0.03299(15) Uani 1 1 d . . . S2 S 0.60045(7) 0.69483(3) 0.03498(5) 0.03178(14) Uani 1 1 d . . . S3 S 0.94304(7) 0.68203(3) 0.25346(5) 0.03192(14) Uani 1 1 d . . . S4 S 0.79158(6) 0.60111(3) 0.34396(5) 0.03156(14) Uani 1 1 d . . . Cu1 Cu 0.48773(3) 0.704002(15) 0.12297(2) 0.02952(8) Uani 1 1 d . A . Cu2 Cu 0.91165(3) 0.588823(14) 0.26209(2) 0.02740(8) Uani 1 1 d . A . In1 In 0.825145(19) 0.722286(9) 0.085381(14) 0.03284(6) Uani 1 1 d . A . In2 In 0.579276(19) 0.556191(9) 0.277492(14) 0.03438(6) Uani 1 1 d . A . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0522(19) 0.0330(15) 0.0388(14) -0.0056(12) 0.0196(13) -0.0003(14) C2 0.0460(17) 0.0321(15) 0.0416(14) -0.0043(12) 0.0233(13) 0.0045(13) C3 0.0394(16) 0.0332(15) 0.0348(13) -0.0075(11) 0.0113(12) -0.0004(13) C4 0.0335(14) 0.0332(15) 0.0328(12) -0.0057(11) 0.0115(11) 0.0049(12) C5 0.072(3) 0.0257(16) 0.076(2) 0.0023(16) 0.031(2) -0.0071(17) C6 0.0445(18) 0.051(2) 0.0451(15) -0.0001(14) 0.0267(14) 0.0014(16) C7 0.064(2) 0.0234(16) 0.076(2) -0.0002(15) 0.0266(19) -0.0001(16) C8 0.049(2) 0.107(4) 0.0477(18) 0.004(2) 0.0319(16) -0.002(2) C9A 0.085(6) 0.039(4) 0.045(3) 0.001(2) 0.037(3) -0.008(4) C10A 0.054(5) 0.036(4) 0.046(4) -0.005(3) 0.032(3) -0.008(3) C11A 0.107(13) 0.056(9) 0.064(6) 0.004(6) 0.066(7) 0.016(8) C9B 0.18(2) 0.057(8) 0.21(3) -0.054(12) 0.18(2) -0.054(13) C10B 0.064(9) 0.030(5) 0.074(10) -0.003(6) 0.047(8) -0.008(6) C11B 0.073(15) 0.065(15) 0.083(15) -0.028(12) 0.059(12) 0.001(11) C12 0.051(2) 0.053(2) 0.060(2) -0.0144(18) -0.0007(17) 0.0098(19) C13 0.0399(17) 0.0424(18) 0.0470(16) -0.0048(14) 0.0072(13) 0.0087(15) C14 0.059(2) 0.047(2) 0.066(2) -0.0081(18) 0.0022(18) 0.0229(19) C15 0.054(2) 0.058(2) 0.055(2) -0.0123(18) 0.0044(17) -0.006(2) C16 0.0508(19) 0.0295(15) 0.0411(14) -0.0028(12) 0.0163(13) -0.0002(14) C17 0.073(3) 0.057(3) 0.069(2) 0.010(2) 0.028(2) -0.019(2) C18 0.0416(19) 0.056(2) 0.089(3) 0.016(2) 0.0395(19) 0.0009(17) C19 0.0293(15) 0.056(2) 0.0445(15) 0.0031(14) 0.0200(12) 0.0040(14) C20 0.0411(18) 0.063(2) 0.068(2) 0.0023(19) 0.0319(16) 0.0151(18) C21 0.052(2) 0.057(2) 0.0385(15) 0.0040(15) 0.0098(14) 0.0013(18) C22 0.0408(16) 0.0303(15) 0.0384(13) 0.0053(12) 0.0172(12) 0.0094(13) C23 0.061(2) 0.0433(18) 0.0467(16) 0.0114(14) 0.0279(16) 0.0063(17) C24 0.072(3) 0.0338(18) 0.073(2) -0.0188(17) 0.026(2) -0.0002(18) C25 0.0434(17) 0.0331(15) 0.0413(14) -0.0067(12) 0.0200(13) -0.0024(13) C26 0.0445(19) 0.054(2) 0.0441(16) -0.0108(15) 0.0098(14) 0.0014(17) P1 0.0322(4) 0.0251(3) 0.0339(3) -0.0021(3) 0.0150(3) 0.0041(3) P2 0.0293(3) 0.0262(3) 0.0315(3) 0.0000(3) 0.0153(3) 0.0043(3) S1 0.0357(4) 0.0283(3) 0.0354(3) -0.0024(3) 0.0148(3) -0.0023(3) S2 0.0320(3) 0.0309(3) 0.0339(3) -0.0013(3) 0.0148(3) 0.0011(3) S3 0.0321(3) 0.0272(3) 0.0356(3) -0.0007(3) 0.0128(3) -0.0016(3) S4 0.0309(3) 0.0326(4) 0.0333(3) 0.0020(3) 0.0152(3) 0.0028(3) Cu1 0.02874(17) 0.02682(17) 0.03131(15) -0.00408(12) 0.01037(13) 0.00508(14) Cu2 0.02724(17) 0.02509(16) 0.02891(15) -0.00137(12) 0.01034(12) 0.00333(13) In1 0.03502(11) 0.02815(11) 0.03761(10) 0.00336(8) 0.01700(8) -0.00220(8) In2 0.03567(11) 0.03391(11) 0.03841(10) 0.00427(8) 0.01997(8) -0.00201(9) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.503(5) . ? C1 S1 1.824(3) . ? C2 S2 1.851(3) . ? C3 C4 1.508(4) . ? C3 S3 1.824(3) . ? C4 S4 1.839(3) . ? C5 In1 2.173(4) . ? C6 In1 2.162(3) . ? C7 In2 2.161(3) . ? C8 In2 2.148(3) . ? C9A C10A 1.524(9) . ? C10A C11A 1.522(11) . ? C10A P1 1.861(8) . ? C9B C10B 1.526(15) . ? C10B C11B 1.532(14) . ? C10B P1 1.881(15) . ? C12 C13 1.506(5) . ? C13 C14 1.533(5) . ? C13 P1 1.856(3) . ? C15 C16 1.532(5) . ? C16 C17 1.530(5) . ? C16 P1 1.836(3) . ? C18 C19 1.516(5) . ? C19 C20 1.540(5) . ? C19 P2 1.865(3) . ? C21 C22 1.530(5) . ? C22 C23 1.521(4) . ? C22 P2 1.847(3) . ? C24 C25 1.534(5) . ? C25 C26 1.521(5) . ? C25 P2 1.849(3) . ? P1 Cu1 2.1920(8) . ? P2 Cu2 2.2085(8) . ? S1 Cu1 2.2735(8) . ? S1 In2 2.5442(7) . ? S2 Cu1 2.2504(7) . ? S2 In1 2.5507(8) . ? S3 Cu2 2.2671(8) . ? S3 In1 2.5476(7) . ? S4 Cu2 2.2569(7) . ? S4 In2 2.5466(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 C2 C1 S1 113.5(2) . . ? C1 C2 S2 112.3(2) . . ? C4 C3 S3 113.8(2) . . ? C3 C4 S4 111.6(2) . . ? C11A C10A C9A 111.8(10) . . ? C11A C10A P1 112.9(10) . . ? C9A C10A P1 110.4(7) . . ? C9B C10B C11B 108.6(16) . . ? C9B C10B P1 108.7(15) . . ? C11B C10B P1 119.7(17) . . ? C12 C13 C14 111.9(3) . . ? C12 C13 P1 111.2(3) . . ? C14 C13 P1 116.3(2) . . ? C17 C16 C15 109.2(3) . . ? C17 C16 P1 111.2(2) . . ? C15 C16 P1 109.5(2) . . ? C18 C19 C20 110.6(3) . . ? C18 C19 P2 111.1(2) . . ? C20 C19 P2 115.8(2) . . ? C23 C22 C21 109.7(3) . . ? C23 C22 P2 110.7(2) . . ? C21 C22 P2 110.1(2) . . ? C26 C25 C24 111.1(3) . . ? C26 C25 P2 110.4(2) . . ? C24 C25 P2 116.7(2) . . ? C16 P1 C13 103.78(16) . . ? C16 P1 C10A 111.0(3) . . ? C13 P1 C10A 102.0(3) . . ? C16 P1 C10B 95.9(5) . . ? C13 P1 C10B 119.4(7) . . ? C10A P1 C10B 19.9(4) . . ? C16 P1 Cu1 116.28(12) . . ? C13 P1 Cu1 106.18(11) . . ? C10A P1 Cu1 115.6(3) . . ? C10B P1 Cu1 115.0(4) . . ? C22 P2 C25 105.00(14) . . ? C22 P2 C19 107.27(14) . . ? C25 P2 C19 103.98(15) . . ? C22 P2 Cu2 109.82(10) . . ? C25 P2 Cu2 113.94(11) . . ? C19 P2 Cu2 116.03(12) . . ? C1 S1 Cu1 97.67(11) . . ? C1 S1 In2 104.71(11) . . ? Cu1 S1 In2 117.82(3) . . ? C2 S2 Cu1 98.12(10) . . ? C2 S2 In1 98.87(11) . . ? Cu1 S2 In1 126.89(3) . . ? C3 S3 Cu2 100.35(11) . . ? C3 S3 In1 105.70(10) . . ? Cu2 S3 In1 112.97(3) . . ? C4 S4 Cu2 99.54(9) . . ? C4 S4 In2 102.37(10) . . ? Cu2 S4 In2 118.31(3) . . ? P1 Cu1 S2 132.85(3) . . ? P1 Cu1 S1 128.39(3) . . ? S2 Cu1 S1 95.38(3) . . ? P2 Cu2 S4 131.40(3) . . ? P2 Cu2 S3 133.76(3) . . ? S4 Cu2 S3 93.42(3) . . ? C6 In1 C5 131.04(15) . . ? C6 In1 S3 101.60(9) . . ? C5 In1 S3 105.46(11) . . ? C6 In1 S2 103.24(10) . . ? C5 In1 S2 106.78(12) . . ? S3 In1 S2 106.85(2) . . ? C8 In2 C7 126.53(18) . . ? C8 In2 S1 109.41(12) . . ? C7 In2 S1 103.93(11) . . ? C8 In2 S4 103.79(12) . . ? C7 In2 S4 105.16(11) . . ? S1 In2 S4 106.64(2) . . ? _chemical_name_common ; bis(mu!3$-1,2-dithiolatoethane-S,S,S',S')-tetramethanido - bis(triisopropylphosphine)-dicopper(+1)-diindium(+3) ; data_[iPr3PCuSC2H4SInEt2]2 _database_code_depnum_ccdc_archive 'CCDC 907034' #TrackingRef '17794_web_deposit_cif_file_0_DirkFriedrich_1360945227.41_[iPr3PCuSC2H4SInEt2]2.cif' _audit_creation_date 2012-10-12T12:46:18-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; bis(\m~3~-1,2-dithiolatoethane-S,S,S',S')-tetraethanido -bis(triisopropylphosphine)-dicopper(+1)-diindium(+3) ; _chemical_formula_moiety 'C30 H70 Cu2 In2 P2 S4' _chemical_formula_sum 'C30 H70 Cu2 In2 P2 S4' _chemical_formula_weight 977.76 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.0923(8) _cell_length_b 15.2034(7) _cell_length_c 13.3064(9) _cell_angle_alpha 90 _cell_angle_beta 107.628(5) _cell_angle_gamma 90 _cell_volume 2138.6(2) _cell_formula_units_Z 2 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 28245 _cell_measurement_theta_min 2.09 _cell_measurement_theta_max 29.46 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.16 _exptl_crystal_density_diffrn 1.518 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1000 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 2.33 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details ; Busing, W. R. & Levy, H. A. (1957) Acta Cryst. 10, 180-182. and Coppens, P., Leiserowitz, L. & Rabinovich, D. (1965) Acta Cryst. 1965, 1035-1038. ; _exptl_absorpt_correction_T_min 0.5007 _exptl_absorpt_correction_T_max 0.7341 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 110(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 '2-circle goniometer' _diffrn_measurement_device_type 'STOE IPDS-2T' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 6.67 _diffrn_detector 'image plate (34 cm diameter / schwenk)' _diffrn_detector_type STOE _diffrn_standards_number 0 _diffrn_reflns_av_R_equivalents 0.0531 _diffrn_reflns_av_unetI/netI 0.0315 _diffrn_reflns_number 27352 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.09 _diffrn_reflns_theta_max 29.07 _diffrn_reflns_theta_full 29.07 _diffrn_measured_fraction_theta_full 0.994 _diffrn_measured_fraction_theta_max 0.994 _reflns_number_total 5688 _reflns_number_gt 4947 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_cell_refinement 'STOE X-AREA' _computing_data_reduction 'STOE X-AREA, STOE X-RED' _computing_structure_solution ; 'SIR-92' Altomare, A., Cascarano, G., Giacovazzo, C. & Guagliardi, A. (1993) J. Appl. Cryst. 26, 343-350. ; _computing_structure_refinement ; 'SHELXL-97' Sheldrick, G.M. (2008) Acta Cryst. A64, 112 ; _computing_molecular_graphics 'DIAMOND 3.2' _computing_publication_material ; 'WinGX publication routines' Farrugia, L. J. (1999) WinGX, J. Appl. Cryst. 32, 837-838 ; #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0160P)^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_number_reflns 5688 _refine_ls_number_parameters 189 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0251 _refine_ls_R_factor_gt 0.0188 _refine_ls_wR_factor_ref 0.0393 _refine_ls_wR_factor_gt 0.0382 _refine_ls_goodness_of_fit_ref 0.98 _refine_ls_restrained_S_all 0.98 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.36 _refine_diff_density_min -0.924 _refine_diff_density_rms 0.068 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' In In -0.7276 1.31 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.36697(14) 0.66138(9) 0.44968(12) 0.0221(3) Uani 1 1 d . . . H1A H 0.2807 0.6864 0.4239 0.026 Uiso 1 1 calc R . . H1B H 0.4258 0.704 0.4333 0.026 Uiso 1 1 calc R . . C2 C 0.37066(14) 0.57560(10) 0.39095(11) 0.0194(3) Uani 1 1 d . . . H2A H 0.459 0.5542 0.4098 0.023 Uiso 1 1 calc R . . H2B H 0.3415 0.5869 0.3141 0.023 Uiso 1 1 calc R . . C3 C 0.33053(17) 0.15526(10) 0.42670(13) 0.0273(3) Uani 1 1 d . . . H3A H 0.2887 0.1375 0.3536 0.041 Uiso 1 1 calc R . . H3B H 0.3049 0.1157 0.4747 0.041 Uiso 1 1 calc R . . H3C H 0.4225 0.1522 0.4411 0.041 Uiso 1 1 calc R . . C4 C 0.29222(14) 0.24983(10) 0.44343(12) 0.0217(3) Uani 1 1 d . . . H4A H 0.3303 0.265 0.5188 0.026 Uiso 1 1 calc R . . H4B H 0.1992 0.2516 0.4282 0.026 Uiso 1 1 calc R . . C5 C 0.16366(16) 0.41003(12) 0.12796(13) 0.0292(3) Uani 1 1 d . . . H5A H 0.1071 0.3606 0.1284 0.044 Uiso 1 1 calc R . . H5B H 0.153 0.4279 0.055 0.044 Uiso 1 1 calc R . . H5C H 0.143 0.4596 0.1669 0.044 Uiso 1 1 calc R . . C6 C 0.30108(15) 0.38190(11) 0.18043(12) 0.0244(3) Uani 1 1 d . . . H6A H 0.3577 0.4297 0.1716 0.029 Uiso 1 1 calc R . . H6B H 0.319 0.3294 0.1433 0.029 Uiso 1 1 calc R . . C7 C 0.00727(14) 0.38134(11) 0.74035(12) 0.0229(3) Uani 1 1 d . . . H7A H -0.0833 0.3718 0.7063 0.034 Uiso 1 1 calc R . . H7B H 0.0191 0.4213 0.8004 0.034 Uiso 1 1 calc R . . H7C H 0.0483 0.325 0.7652 0.034 Uiso 1 1 calc R . . C8 C 0.06656(13) 0.42213(9) 0.66053(11) 0.0168(3) Uani 1 1 d . . . H8 H 0.017 0.4766 0.6329 0.02 Uiso 1 1 calc R . . C9 C 0.05040(15) 0.36093(11) 0.56538(13) 0.0256(3) Uani 1 1 d . . . H9A H 0.094 0.3052 0.5893 0.038 Uiso 1 1 calc R . . H9B H 0.0866 0.3889 0.5148 0.038 Uiso 1 1 calc R . . H9C H -0.0398 0.3497 0.5315 0.038 Uiso 1 1 calc R . . C10 C 0.31584(15) 0.34636(11) 0.90441(12) 0.0249(3) Uani 1 1 d . . . H10A H 0.3555 0.2902 0.9323 0.037 Uiso 1 1 calc R . . H10B H 0.2283 0.347 0.9065 0.037 Uiso 1 1 calc R . . H10C H 0.363 0.3947 0.9474 0.037 Uiso 1 1 calc R . . C11 C 0.31709(13) 0.35748(9) 0.78946(11) 0.0184(3) Uani 1 1 d . . . H11 H 0.2706 0.3056 0.7499 0.022 Uiso 1 1 calc R . . C12 C 0.45349(15) 0.35103(11) 0.78284(14) 0.0273(3) Uani 1 1 d . . . H12A H 0.5037 0.4004 0.8212 0.041 Uiso 1 1 calc R . . H12B H 0.4517 0.3532 0.7088 0.041 Uiso 1 1 calc R . . H12C H 0.4916 0.2955 0.8143 0.041 Uiso 1 1 calc R . . C13 C 0.36327(16) 0.57705(11) 0.87315(13) 0.0274(3) Uani 1 1 d . . . H13A H 0.3918 0.6093 0.8208 0.041 Uiso 1 1 calc R . . H13B H 0.4219 0.5286 0.9018 0.041 Uiso 1 1 calc R . . H13C H 0.3609 0.617 0.9304 0.041 Uiso 1 1 calc R . . C14 C 0.22998(14) 0.53974(9) 0.82052(11) 0.0192(3) Uani 1 1 d . . . H14 H 0.1993 0.5103 0.8754 0.023 Uiso 1 1 calc R . . C15 C 0.13821(17) 0.61485(10) 0.76997(14) 0.0269(3) Uani 1 1 d . . . H15A H 0.1412 0.6602 0.823 0.04 Uiso 1 1 calc R . . H15B H 0.052 0.5915 0.7432 0.04 Uiso 1 1 calc R . . H15C H 0.1631 0.6405 0.7116 0.04 Uiso 1 1 calc R . . P1 P 0.23495(3) 0.45725(2) 0.71793(3) 0.01344(6) Uani 1 1 d . . . S1 S 0.41024(3) 0.64726(2) 0.59386(3) 0.01814(7) Uani 1 1 d . . . S2 S 0.27057(3) 0.49003(2) 0.42276(3) 0.01631(6) Uani 1 1 d . . . Cu1 Cu 0.312300(16) 0.515265(11) 0.597631(13) 0.01493(4) Uani 1 1 d . . . In1 In 0.346296(9) 0.351244(6) 0.348321(8) 0.01727(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0197(7) 0.0185(6) 0.0259(7) 0.0070(6) 0.0036(5) 0.0001(5) C2 0.0179(6) 0.0237(7) 0.0160(6) 0.0050(5) 0.0041(5) -0.0010(5) C3 0.0378(9) 0.0228(7) 0.0245(8) 0.0008(6) 0.0142(7) 0.0013(6) C4 0.0233(7) 0.0211(6) 0.0230(7) -0.0019(6) 0.0102(6) -0.0035(6) C5 0.0296(8) 0.0324(8) 0.0227(8) -0.0012(6) 0.0035(6) 0.0019(7) C6 0.0274(7) 0.0302(7) 0.0157(7) -0.0030(6) 0.0069(6) -0.0028(6) C7 0.0159(6) 0.0281(7) 0.0250(7) 0.0059(6) 0.0069(5) -0.0029(6) C8 0.0140(6) 0.0176(6) 0.0183(6) 0.0013(5) 0.0040(5) -0.0003(5) C9 0.0229(7) 0.0285(8) 0.0238(7) -0.0076(6) 0.0046(6) -0.0068(6) C10 0.0257(7) 0.0280(7) 0.0197(7) 0.0095(6) 0.0052(6) 0.0015(6) C11 0.0168(6) 0.0172(6) 0.0204(7) 0.0023(5) 0.0045(5) 0.0009(5) C12 0.0186(7) 0.0295(8) 0.0340(8) 0.0055(7) 0.0082(6) 0.0056(6) C13 0.0325(8) 0.0280(8) 0.0220(8) -0.0089(6) 0.0086(6) -0.0105(7) C14 0.0254(7) 0.0170(6) 0.0172(7) -0.0025(5) 0.0096(5) -0.0036(5) C15 0.0351(8) 0.0181(7) 0.0316(8) -0.0026(6) 0.0161(7) 0.0024(6) P1 0.01418(15) 0.01341(14) 0.01303(15) -0.00019(12) 0.00456(12) -0.00095(12) S1 0.01774(15) 0.01550(14) 0.02202(17) -0.00179(13) 0.00727(12) -0.00177(12) S2 0.01552(15) 0.01870(15) 0.01458(15) -0.00044(12) 0.00438(12) -0.00075(12) Cu1 0.01500(8) 0.01630(8) 0.01447(8) 0.00143(6) 0.00591(6) -0.00002(6) In1 0.01759(5) 0.01783(5) 0.01590(5) -0.00172(4) 0.00436(3) -0.00238(4) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.527(2) . ? C1 S1 1.8437(16) . ? C2 S2 1.8409(15) . ? C3 C4 1.534(2) . ? C4 In1 2.1906(15) . ? C5 C6 1.533(2) . ? C6 In1 2.1865(15) . ? C7 C8 1.5389(19) . ? C8 C9 1.537(2) . ? C8 P1 1.8690(14) . ? C10 C11 1.543(2) . ? C11 C12 1.545(2) . ? C11 P1 1.8740(14) . ? C13 C14 1.540(2) . ? C14 C15 1.542(2) . ? C14 P1 1.8668(14) . ? P1 Cu1 2.2155(4) . ? S1 Cu1 2.2897(4) . ? S1 In1 2.5743(4) 3_666 ? S2 Cu1 2.2635(4) . ? S2 In1 2.5773(4) . ? In1 S1 2.5743(4) 3_666 ? 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 C2 C1 S1 113.21(10) . . ? C1 C2 S2 111.98(10) . . ? C3 C4 In1 116.06(10) . . ? C5 C6 In1 114.43(10) . . ? C9 C8 C7 110.91(12) . . ? C9 C8 P1 111.24(10) . . ? C7 C8 P1 114.59(10) . . ? C10 C11 C12 110.64(12) . . ? C10 C11 P1 116.31(10) . . ? C12 C11 P1 110.87(10) . . ? C13 C14 C15 109.98(13) . . ? C13 C14 P1 110.07(10) . . ? C15 C14 P1 109.89(10) . . ? C14 P1 C8 104.10(6) . . ? C14 P1 C11 106.85(7) . . ? C8 P1 C11 104.38(6) . . ? C14 P1 Cu1 111.38(5) . . ? C8 P1 Cu1 112.10(5) . . ? C11 P1 Cu1 117.01(5) . . ? C1 S1 Cu1 98.58(5) . . ? C1 S1 In1 103.23(5) . 3_666 ? Cu1 S1 In1 117.577(15) . 3_666 ? C2 S2 Cu1 99.60(5) . . ? C2 S2 In1 101.58(5) . . ? Cu1 S2 In1 123.018(15) . . ? P1 Cu1 S2 132.213(15) . . ? P1 Cu1 S1 130.911(15) . . ? S2 Cu1 S1 94.400(14) . . ? C6 In1 C4 136.23(6) . . ? C6 In1 S1 101.46(4) . 3_666 ? C4 In1 S1 106.23(4) . 3_666 ? C6 In1 S2 102.57(4) . . ? C4 In1 S2 100.14(4) . . ? S1 In1 S2 108.203(11) 3_666 . ? _chemical_name_common ; bis(mu!3$-1,2-dithiolatoethane-S,S,S',S')-tetraethanido - bis(triisopropylphosphine)-dicopper(+1)-diindium(+3) ; data_[iPr3PCuSC2H4SIniPr2]2 _database_code_depnum_ccdc_archive 'CCDC 907035' #TrackingRef '17795_web_deposit_cif_file_0_DirkFriedrich_1360945304.42_[iPr3PCuSC2H4SIniPr2]2.cif' _audit_creation_date 2012-10-12T10:25:58-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; bis(\m~3~-1,2-dithiolatoethane-S,S,S',S')-tetra(propan-2-ido) -bis(triisopropylphosphine)-dicopper(+1)-diindium(+3) ; _chemical_formula_moiety 'C34 H78 Cu2 In2 P2 S4' _chemical_formula_sum 'C34 H78 Cu2 In2 P2 S4' _chemical_formula_weight 1033.86 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.2512(7) _cell_length_b 11.8219(11) _cell_length_c 13.1077(13) _cell_angle_alpha 71.231(7) _cell_angle_beta 79.528(7) _cell_angle_gamma 83.635(7) _cell_volume 1188.55(19) _cell_formula_units_Z 1 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 24820 _cell_measurement_theta_min 1.82 _cell_measurement_theta_max 29.37 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.29 _exptl_crystal_size_min 0.24 _exptl_crystal_density_diffrn 1.444 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 532 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 2.10 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details ; Busing, W. R. & Levy, H. A. (1957) Acta Cryst. 10, 180-182. and Coppens, P., Leiserowitz, L. & Rabinovich, D. (1965) Acta Cryst. 1965, 1035-1038. ; _exptl_absorpt_correction_T_min 0.5711 _exptl_absorpt_correction_T_max 0.6876 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 180(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 '2-circle goniometer' _diffrn_measurement_device_type 'STOE IPDS-2T' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 6.67 _diffrn_detector 'image plate (34 cm diameter / schwenk)' _diffrn_detector_type STOE _diffrn_standards_number 0 _diffrn_reflns_av_R_equivalents 0.0192 _diffrn_reflns_av_unetI/netI 0.0198 _diffrn_reflns_number 13437 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.82 _diffrn_reflns_theta_max 29 _diffrn_reflns_theta_full 29 _diffrn_measured_fraction_theta_full 0.992 _diffrn_measured_fraction_theta_max 0.992 _reflns_number_total 6264 _reflns_number_gt 5514 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_cell_refinement 'STOE X-AREA' _computing_data_reduction 'STOE X-AREA, STOE X-RED' _computing_structure_solution ; 'SIR-92' Altomare, A., Cascarano, G., Giacovazzo, C. & Guagliardi, A. (1993) J. Appl. Cryst. 26, 343-350. ; _computing_structure_refinement ; 'SHELXL-97' Sheldrick, G.M. (2008) Acta Cryst. A64, 112 ; _computing_molecular_graphics 'DIAMOND 3.2' _computing_publication_material ; 'WinGX publication routines' Farrugia, L. J. (1999) WinGX, J. Appl. Cryst. 32, 837-838 ; #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0314P)^2^+0.1556P] 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_number_reflns 6264 _refine_ls_number_parameters 209 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0278 _refine_ls_R_factor_gt 0.0223 _refine_ls_wR_factor_ref 0.0555 _refine_ls_wR_factor_gt 0.0531 _refine_ls_goodness_of_fit_ref 1.075 _refine_ls_restrained_S_all 1.075 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.563 _refine_diff_density_min -0.874 _refine_diff_density_rms 0.063 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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' 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' In In -0.7276 1.31 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.7342(2) 0.49350(15) 0.53055(16) 0.0297(4) Uani 1 1 d . . . H1A H 0.8373 0.4417 0.5344 0.036 Uiso 1 1 calc R . . H1B H 0.6709 0.4738 0.4818 0.036 Uiso 1 1 calc R . . C2 C 0.7776(2) 0.62440(16) 0.48260(16) 0.0301(4) Uani 1 1 d . . . H2A H 0.8377 0.6376 0.4075 0.036 Uiso 1 1 calc R . . H2B H 0.8529 0.6407 0.5264 0.036 Uiso 1 1 calc R . . C3 C 0.3298(4) 0.2787(3) 0.9195(3) 0.0777(11) Uani 1 1 d . . . H3A H 0.2312 0.2785 0.974 0.116 Uiso 1 1 calc R . . H3B H 0.3709 0.3593 0.8899 0.116 Uiso 1 1 calc R . . H3C H 0.4154 0.2225 0.9538 0.116 Uiso 1 1 calc R . . C4 C 0.2862(3) 0.24074(17) 0.82745(17) 0.0348(4) Uani 1 1 d . . . H4 H 0.197 0.298 0.7949 0.042 Uiso 1 1 calc R . . C5 C 0.2216(3) 0.11512(19) 0.86941(19) 0.0435(5) Uani 1 1 d . . . H5A H 0.3075 0.0573 0.9013 0.065 Uiso 1 1 calc R . . H5B H 0.1917 0.0946 0.8088 0.065 Uiso 1 1 calc R . . H5C H 0.124 0.1129 0.9251 0.065 Uiso 1 1 calc R . . C6 C 0.8833(3) 0.18285(19) 0.6617(2) 0.0427(5) Uani 1 1 d . . . H6A H 0.8999 0.2446 0.6933 0.064 Uiso 1 1 calc R . . H6B H 0.8795 0.2194 0.5836 0.064 Uiso 1 1 calc R . . H6C H 0.9746 0.1219 0.6721 0.064 Uiso 1 1 calc R . . C7 C 0.7215(2) 0.12502(15) 0.71778(16) 0.0318(4) Uani 1 1 d . . . H7 H 0.7069 0.0641 0.6826 0.038 Uiso 1 1 calc R . . C8 C 0.7283(3) 0.0590(2) 0.8387(2) 0.0529(6) Uani 1 1 d . . . H8A H 0.8243 0.0019 0.8455 0.079 Uiso 1 1 calc R . . H8B H 0.6273 0.016 0.8717 0.079 Uiso 1 1 calc R . . H8C H 0.7375 0.117 0.8763 0.079 Uiso 1 1 calc R . . C9 C 0.2112(3) 0.93213(19) 0.56282(19) 0.0441(5) Uani 1 1 d . . . H9A H 0.2208 1.019 0.5377 0.066 Uiso 1 1 calc R . . H9B H 0.1004 0.9142 0.5575 0.066 Uiso 1 1 calc R . . H9C H 0.2937 0.8956 0.5172 0.066 Uiso 1 1 calc R . . C10 C 0.2405(2) 0.88125(16) 0.68202(17) 0.0325(4) Uani 1 1 d . . . H10 H 0.1518 0.9152 0.7287 0.039 Uiso 1 1 calc R . . C11 C 0.4096(3) 0.91741(18) 0.6924(2) 0.0418(5) Uani 1 1 d . . . H11A H 0.4974 0.8836 0.6476 0.063 Uiso 1 1 calc R . . H11B H 0.4265 0.8867 0.7688 0.063 Uiso 1 1 calc R . . H11C H 0.4122 1.0048 0.6672 0.063 Uiso 1 1 calc R . . C12 C 0.0127(3) 0.5462(2) 0.7464(2) 0.0509(6) Uani 1 1 d . . . H12A H -0.0007 0.5172 0.8262 0.076 Uiso 1 1 calc R . . H12B H 0.1117 0.5066 0.7162 0.076 Uiso 1 1 calc R . . H12C H -0.0842 0.5281 0.7222 0.076 Uiso 1 1 calc R . . C13 C 0.0305(2) 0.68233(18) 0.70652(17) 0.0345(4) Uani 1 1 d . . . H13 H 0.0352 0.7077 0.6256 0.041 Uiso 1 1 calc R . . C14 C -0.1227(3) 0.7493(3) 0.7501(3) 0.0589(7) Uani 1 1 d . . . H14A H -0.22 0.7324 0.7255 0.088 Uiso 1 1 calc R . . H14B H -0.1074 0.8356 0.7225 0.088 Uiso 1 1 calc R . . H14C H -0.1384 0.7228 0.83 0.088 Uiso 1 1 calc R . . C15 C 0.1420(3) 0.7604(2) 0.9382(2) 0.0518(6) Uani 1 1 d . . . H15A H 0.124 0.7219 1.0173 0.078 Uiso 1 1 calc R . . H15B H 0.0358 0.7905 0.9134 0.078 Uiso 1 1 calc R . . H15C H 0.2136 0.8272 0.9201 0.078 Uiso 1 1 calc R . . C16 C 0.2247(3) 0.66892(18) 0.88128(17) 0.0381(4) Uani 1 1 d . . . H16 H 0.1571 0.597 0.9119 0.046 Uiso 1 1 calc R . . C17 C 0.3973(4) 0.6279(3) 0.9138(2) 0.0624(8) Uani 1 1 d . . . H17A H 0.4656 0.6971 0.891 0.094 Uiso 1 1 calc R . . H17B H 0.4493 0.5691 0.8778 0.094 Uiso 1 1 calc R . . H17C H 0.3867 0.5915 0.993 0.094 Uiso 1 1 calc R . . P1 P 0.23472(5) 0.71495(4) 0.73005(4) 0.02557(9) Uani 1 1 d . . . S1 S 0.61122(5) 0.46220(4) 0.66837(4) 0.02727(9) Uani 1 1 d . . . S2 S 0.59686(6) 0.73145(4) 0.47865(4) 0.02845(9) Uani 1 1 d . . . Cu1 Cu 0.44250(3) 0.630959(18) 0.640831(19) 0.02768(5) Uani 1 1 d . . . In1 In 0.504333(15) 0.253903(10) 0.699762(10) 0.02635(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0254(8) 0.0261(8) 0.0366(10) -0.0098(7) -0.0036(7) 0.0008(6) C2 0.0231(8) 0.0290(8) 0.0364(10) -0.0069(7) -0.0050(7) -0.0028(6) C3 0.091(2) 0.102(2) 0.0571(17) -0.0541(18) 0.0294(16) -0.055(2) C4 0.0366(10) 0.0326(9) 0.0335(10) -0.0121(8) 0.0066(8) -0.0081(7) C5 0.0457(12) 0.0398(11) 0.0432(12) -0.0127(9) 0.0042(10) -0.0142(9) C6 0.0351(10) 0.0372(10) 0.0517(13) -0.0108(9) -0.0067(9) 0.0062(8) C7 0.0367(9) 0.0228(8) 0.0350(10) -0.0065(7) -0.0108(8) 0.0039(7) C8 0.0588(14) 0.0493(13) 0.0407(12) 0.0000(10) -0.0150(11) 0.0076(11) C9 0.0559(13) 0.0307(9) 0.0406(11) -0.0044(9) -0.0104(10) 0.0039(9) C10 0.0356(9) 0.0238(8) 0.0383(10) -0.0119(7) -0.0040(8) 0.0025(7) C11 0.0457(11) 0.0306(9) 0.0525(13) -0.0165(9) -0.0049(10) -0.0094(8) C12 0.0472(12) 0.0466(12) 0.0633(16) -0.0144(11) -0.0155(11) -0.0171(10) C13 0.0268(8) 0.0418(10) 0.0388(10) -0.0162(9) -0.0080(8) -0.0020(7) C14 0.0273(10) 0.0808(18) 0.0792(19) -0.0425(16) -0.0072(11) 0.0050(11) C15 0.0621(15) 0.0593(14) 0.0373(12) -0.0231(11) -0.0042(11) 0.0015(12) C16 0.0508(12) 0.0337(9) 0.0311(10) -0.0085(8) -0.0115(9) -0.0034(8) C17 0.0787(19) 0.0633(16) 0.0576(16) -0.0291(13) -0.0401(15) 0.0248(14) P1 0.0250(2) 0.02369(19) 0.0298(2) -0.01080(17) -0.00514(17) 0.00080(15) S1 0.02686(19) 0.02172(18) 0.0322(2) -0.00712(16) -0.00422(17) -0.00119(14) S2 0.0324(2) 0.02125(18) 0.0310(2) -0.00718(16) -0.00525(17) -0.00099(15) Cu1 0.02471(10) 0.02564(10) 0.03503(12) -0.01355(9) -0.00394(9) 0.00043(8) In1 0.02741(6) 0.02151(6) 0.02724(7) -0.00413(5) -0.00291(5) -0.00176(4) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.528(2) . ? C1 S1 1.849(2) . ? C2 S2 1.8430(18) . ? C3 C4 1.526(3) . ? C4 C5 1.528(3) . ? C4 In1 2.205(2) . ? C6 C7 1.521(3) . ? C7 C8 1.534(3) . ? C7 In1 2.2147(18) . ? C9 C10 1.537(3) . ? C10 C11 1.545(3) . ? C10 P1 1.8647(18) . ? C12 C13 1.539(3) . ? C13 C14 1.536(3) . ? C13 P1 1.8686(18) . ? C15 C16 1.537(3) . ? C16 C17 1.542(3) . ? C16 P1 1.868(2) . ? P1 Cu1 2.2212(5) . ? S1 Cu1 2.2698(5) . ? S1 In1 2.5901(5) . ? S2 Cu1 2.2976(6) . ? S2 In1 2.5716(5) 2_666 ? In1 S2 2.5716(5) 2_666 ? 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 C2 C1 S1 111.89(13) . . ? C1 C2 S2 113.81(12) . . ? C3 C4 C5 111.6(2) . . ? C3 C4 In1 109.13(16) . . ? C5 C4 In1 111.73(14) . . ? C6 C7 C8 110.71(18) . . ? C6 C7 In1 113.03(12) . . ? C8 C7 In1 110.36(15) . . ? C9 C10 C11 109.72(18) . . ? C9 C10 P1 110.62(13) . . ? C11 C10 P1 109.65(13) . . ? C14 C13 C12 111.7(2) . . ? C14 C13 P1 116.96(15) . . ? C12 C13 P1 109.44(14) . . ? C15 C16 C17 109.69(19) . . ? C15 C16 P1 116.47(15) . . ? C17 C16 P1 110.97(18) . . ? C10 P1 C16 105.86(9) . . ? C10 P1 C13 105.66(9) . . ? C16 P1 C13 105.82(10) . . ? C10 P1 Cu1 111.39(7) . . ? C16 P1 Cu1 115.82(7) . . ? C13 P1 Cu1 111.58(7) . . ? C1 S1 Cu1 99.16(6) . . ? C1 S1 In1 102.27(6) . . ? Cu1 S1 In1 122.335(19) . . ? C2 S2 Cu1 98.49(6) . . ? C2 S2 In1 103.75(6) . 2_666 ? Cu1 S2 In1 118.25(2) . 2_666 ? P1 Cu1 S1 140.05(2) . . ? P1 Cu1 S2 124.28(2) . . ? S1 Cu1 S2 94.557(19) . . ? C4 In1 C7 123.33(8) . . ? C4 In1 S2 107.84(6) . 2_666 ? C7 In1 S2 108.15(5) . 2_666 ? C4 In1 S1 104.35(5) . . ? C7 In1 S1 106.57(5) . . ? S2 In1 S1 105.206(16) 2_666 . ? _chemical_name_common ; bis(mu!3$-1,2-dithiolatoethane-S,S,S',S')-tetra(propan-2-ido) -bis(triisopropylphosphine)-dicopper(+1)-diindium(+3) ; data_ip1_1157b _database_code_depnum_ccdc_archive 'CCDC 907036' #TrackingRef '17796_web_deposit_cif_file_0_DirkFriedrich_1360945448.43_[iPr3PCuSC2H4SInBu2]2.cif' _audit_creation_date 2012-10-12T13:08:47-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; bis(\m~3~-1,2-dithiolatoethane-S,S,S',S')-tetra(butan-1-ido) -bis(triisopropylphosphine)-dicopper(+1)-diindium(+3) ; _chemical_formula_moiety 'C38 H86 Cu2 In2 P2 S4' _chemical_formula_sum 'C38 H86 Cu2 In2 P2 S4' _chemical_formula_weight 1089.97 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.988(5) _cell_length_b 11.495(5) _cell_length_c 11.649(5) _cell_angle_alpha 118.253(5) _cell_angle_beta 98.990(5) _cell_angle_gamma 90.370(5) _cell_volume 1274.7(10) _cell_formula_units_Z 1 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used 16732 _cell_measurement_theta_min 2.5 _cell_measurement_theta_max 25.82 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.88 _exptl_crystal_size_mid 0.68 _exptl_crystal_size_min 0.28 _exptl_crystal_density_diffrn 1.42 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 564 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.97 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details ; Busing, W. R. & Levy, H. A. (1957) Acta Cryst. 10, 180-182. and Coppens, P., Leiserowitz, L. & Rabinovich, D. (1965) Acta Cryst. 1965, 1035-1038. ; _exptl_absorpt_correction_T_min 0.2653 _exptl_absorpt_correction_T_max 0.4985 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 213(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 '2-circle goniometer' _diffrn_measurement_device_type 'STOE IPDS-2T' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 6.67 _diffrn_detector 'image plate (34 cm diameter / schwenk)' _diffrn_detector_type STOE _diffrn_standards_number 0 _diffrn_reflns_av_R_equivalents 0.0569 _diffrn_reflns_av_unetI/netI 0.0423 _diffrn_reflns_number 14887 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.5 _diffrn_reflns_theta_max 25.77 _diffrn_reflns_theta_full 25.77 _diffrn_measured_fraction_theta_full 0.928 _diffrn_measured_fraction_theta_max 0.928 _reflns_number_total 4542 _reflns_number_gt 3815 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_cell_refinement 'STOE X-AREA' _computing_data_reduction 'STOE X-AREA, STOE X-RED' _computing_structure_solution ; 'SIR-92' Altomare, A., Cascarano, G., Giacovazzo, C. & Guagliardi, A. (1993) J. Appl. Cryst. 26, 343-350. ; _computing_structure_refinement ; 'SHELXL-97' Sheldrick, G.M. (2008) Acta Cryst. A64, 112 ; _computing_molecular_graphics 'DIAMOND 3.2' _computing_publication_material ; 'WinGX publication routines' Farrugia, L. J. (1999) WinGX, J. Appl. Cryst. 32, 837-838 ; #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0895P)^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_number_reflns 4542 _refine_ls_number_parameters 263 _refine_ls_number_restraints 15 _refine_ls_R_factor_all 0.0539 _refine_ls_R_factor_gt 0.0478 _refine_ls_wR_factor_ref 0.1227 _refine_ls_wR_factor_gt 0.1195 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.036 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.607 _refine_diff_density_min -1.193 _refine_diff_density_rms 0.134 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' In In -0.7276 1.31 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.3344(5) 0.3309(5) 0.2788(5) 0.0615(12) Uani 1 1 d . . . H1A H 0.3846 0.275 0.2142 0.074 Uiso 1 1 calc R . . H1B H 0.2498 0.3197 0.231 0.074 Uiso 1 1 calc R . . C2 C 0.6169(4) 0.5303(5) 0.6636(4) 0.0555(11) Uani 1 1 d . . . H2A H 0.5286 0.5213 0.6272 0.067 Uiso 1 1 calc R . . H2B H 0.625 0.5052 0.7338 0.067 Uiso 1 1 calc R . . C3A C 0.5459(14) 0.1967(18) 0.6274(14) 0.041(3) Uani 0.499(16) 1 d PD A 1 H3A1 H 0.5208 0.2815 0.691 0.049 Uiso 0.499(16) 1 calc PR A 1 H3A2 H 0.4806 0.1281 0.6079 0.049 Uiso 0.499(16) 1 calc PR A 1 C4A C 0.6595(13) 0.170(3) 0.6944(14) 0.144(11) Uani 0.499(16) 1 d PD A 1 H4A1 H 0.6906 0.256 0.7717 0.173 Uiso 0.499(16) 1 calc PR A 1 H4A2 H 0.6301 0.115 0.7297 0.173 Uiso 0.499(16) 1 calc PR A 1 C5A C 0.7629(14) 0.116(3) 0.6467(18) 0.143(10) Uani 0.499(16) 1 d PD A 1 H5A1 H 0.7971 0.1727 0.6162 0.171 Uiso 0.499(16) 1 calc PR A 1 H5A2 H 0.7336 0.0306 0.5673 0.171 Uiso 0.499(16) 1 calc PR A 1 C6A C 0.8698(14) 0.089(3) 0.724(2) 0.076(5) Uani 0.499(16) 1 d PD A 1 H6A1 H 0.9367 0.1578 0.7549 0.114 Uiso 0.499(16) 1 calc PR A 1 H6A2 H 0.8977 0.0035 0.6681 0.114 Uiso 0.499(16) 1 calc PR A 1 H6A3 H 0.8444 0.0873 0.7996 0.114 Uiso 0.499(16) 1 calc PR A 1 C3B C 0.5715(14) 0.1702(19) 0.6039(18) 0.057(5) Uani 0.501(16) 1 d PD A 2 H3B1 H 0.5492 0.2469 0.6805 0.069 Uiso 0.501(16) 1 calc PR A 2 H3B2 H 0.5165 0.0927 0.583 0.069 Uiso 0.501(16) 1 calc PR A 2 C4B C 0.7039(11) 0.1462(15) 0.6370(14) 0.075(4) Uani 0.501(16) 1 d PD A 2 H4B1 H 0.7264 0.0753 0.5563 0.09 Uiso 0.501(16) 1 calc PR A 2 H4B2 H 0.7563 0.2267 0.6616 0.09 Uiso 0.501(16) 1 calc PR A 2 C5B C 0.7340(12) 0.1111(14) 0.7410(15) 0.094(5) Uani 0.501(16) 1 d PD A 2 H5B1 H 0.6828 0.0297 0.7159 0.112 Uiso 0.501(16) 1 calc PR A 2 H5B2 H 0.7108 0.1814 0.8217 0.112 Uiso 0.501(16) 1 calc PR A 2 C6B C 0.8662(17) 0.090(4) 0.773(3) 0.119(10) Uani 0.501(16) 1 d PD A 2 H6B1 H 0.8702 0.0093 0.7806 0.179 Uiso 0.501(16) 1 calc PR A 2 H6B2 H 0.9053 0.1646 0.8564 0.179 Uiso 0.501(16) 1 calc PR A 2 H6B3 H 0.909 0.0815 0.7031 0.179 Uiso 0.501(16) 1 calc PR A 2 C7 C 0.5835(5) 0.0637(6) 0.2477(6) 0.0798(18) Uani 1 1 d D A . H7A H 0.5695 -0.0254 0.2373 0.096 Uiso 1 1 calc R . . H7B H 0.521 0.0703 0.1816 0.096 Uiso 1 1 calc R . . C8 C 0.7069(5) 0.0747(6) 0.2147(6) 0.0743(15) Uani 1 1 d D . . H8A H 0.7701 0.0643 0.2778 0.089 Uiso 1 1 calc R . . H8B H 0.7228 0.164 0.2264 0.089 Uiso 1 1 calc R . . C9 C 0.7210(6) -0.0251(7) 0.0762(6) 0.092(2) Uani 1 1 d D . . H9A H 0.7024 -0.1141 0.0641 0.111 Uiso 1 1 calc R . . H9B H 0.6588 -0.013 0.0136 0.111 Uiso 1 1 calc R . . C10 C 0.8412(9) -0.0195(10) 0.0416(10) 0.141(4) Uani 1 1 d D . . H10A H 0.8334 0.006 -0.0274 0.211 Uiso 1 1 calc R . . H10B H 0.8726 -0.106 0.0099 0.211 Uiso 1 1 calc R . . H10C H 0.898 0.0453 0.1192 0.211 Uiso 1 1 calc R . . C11 C 0.9665(4) 0.3640(5) 0.3020(5) 0.0571(11) Uani 1 1 d . . . H11A H 1.0157 0.2901 0.2619 0.086 Uiso 1 1 calc R . . H11B H 0.9037 0.3396 0.3388 0.086 Uiso 1 1 calc R . . H11C H 1.0196 0.4401 0.372 0.086 Uiso 1 1 calc R . . C12 C 0.9047(4) 0.3986(5) 0.1978(5) 0.0522(10) Uani 1 1 d . . . H12 H 0.8539 0.3172 0.1277 0.063 Uiso 1 1 calc R . . C13 C 1.0029(5) 0.4288(7) 0.1316(6) 0.0773(16) Uani 1 1 d . . . H13A H 1.0604 0.5029 0.1983 0.116 Uiso 1 1 calc R . . H13B H 0.9624 0.4512 0.0654 0.116 Uiso 1 1 calc R . . H13C H 1.0476 0.3514 0.0896 0.116 Uiso 1 1 calc R . . C14 C 0.9746(5) 0.7308(5) 0.4291(6) 0.0699(14) Uani 1 1 d . . . H14A H 1.0111 0.8193 0.4571 0.105 Uiso 1 1 calc R . . H14B H 1.0384 0.6697 0.4096 0.105 Uiso 1 1 calc R . . H14C H 0.9371 0.7314 0.4994 0.105 Uiso 1 1 calc R . . C15 C 0.8764(4) 0.6869(5) 0.3058(5) 0.0592(11) Uani 1 1 d . . . H15 H 0.9172 0.6745 0.2313 0.071 Uiso 1 1 calc R . . C16 C 0.7853(6) 0.7926(6) 0.3281(7) 0.0828(17) Uani 1 1 d . . . H16A H 0.7404 0.8008 0.3966 0.124 Uiso 1 1 calc R . . H16B H 0.7273 0.767 0.2464 0.124 Uiso 1 1 calc R . . H16C H 0.8304 0.8771 0.3555 0.124 Uiso 1 1 calc R . . C17 C 0.7148(6) 0.4987(9) 0.0049(6) 0.094(2) Uani 1 1 d . . . H17A H 0.7722 0.4324 -0.0311 0.142 Uiso 1 1 calc R . . H17B H 0.756 0.5862 0.0372 0.142 Uiso 1 1 calc R . . H17C H 0.6443 0.4828 -0.0638 0.142 Uiso 1 1 calc R . . C18 C 0.6705(4) 0.4904(6) 0.1195(5) 0.0653(13) Uani 1 1 d . . . H18 H 0.6117 0.5587 0.1522 0.078 Uiso 1 1 calc R . . C19 C 0.5985(5) 0.3565(7) 0.0738(6) 0.0802(17) Uani 1 1 d . . . H19A H 0.5292 0.3412 0.004 0.12 Uiso 1 1 calc R . . H19B H 0.568 0.3574 0.1481 0.12 Uiso 1 1 calc R . . H19C H 0.6528 0.2861 0.0406 0.12 Uiso 1 1 calc R . . P1 P 0.79472(9) 0.52705(12) 0.26416(11) 0.0455(2) Uani 1 1 d . . . S1 S 0.33285(10) 0.27338(10) 0.39941(11) 0.0505(3) Uani 1 1 d . . . S2 S 0.69787(9) 0.41422(10) 0.53002(10) 0.0444(2) Uani 1 1 d . A . Cu1 Cu 0.71810(4) 0.54004(5) 0.43280(5) 0.04254(15) Uani 1 1 d . . . In1 In 0.54972(3) 0.20513(3) 0.44188(3) 0.04953(14) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.058(3) 0.067(3) 0.050(2) 0.018(2) 0.018(2) 0.011(2) C2 0.055(2) 0.072(3) 0.045(2) 0.029(2) 0.0190(18) 0.007(2) C3A 0.046(6) 0.039(7) 0.045(5) 0.020(5) 0.029(5) 0.025(4) C4A 0.067(8) 0.33(3) 0.082(9) 0.130(15) 0.052(7) 0.094(13) C5A 0.087(10) 0.31(3) 0.157(16) 0.20(2) 0.069(11) 0.111(15) C6A 0.054(7) 0.105(10) 0.101(13) 0.074(11) 0.017(7) 0.017(6) C3B 0.048(7) 0.034(7) 0.083(11) 0.018(7) 0.028(7) 0.021(5) C4B 0.050(7) 0.107(10) 0.084(9) 0.061(8) 0.006(7) 0.004(6) C5B 0.098(10) 0.085(9) 0.124(13) 0.069(9) 0.027(9) 0.008(7) C6B 0.078(11) 0.18(2) 0.14(2) 0.12(2) -0.004(12) -0.006(12) C7 0.064(3) 0.072(3) 0.061(3) -0.004(3) 0.021(2) 0.002(3) C8 0.072(3) 0.073(3) 0.071(3) 0.025(3) 0.027(3) 0.013(3) C9 0.084(4) 0.097(4) 0.075(4) 0.018(3) 0.034(3) 0.021(3) C10 0.149(8) 0.116(7) 0.123(7) 0.014(5) 0.081(6) 0.002(6) C11 0.047(2) 0.069(3) 0.064(3) 0.036(2) 0.020(2) 0.014(2) C12 0.042(2) 0.064(3) 0.056(2) 0.029(2) 0.0194(18) 0.0129(18) C13 0.064(3) 0.112(5) 0.085(4) 0.060(4) 0.048(3) 0.038(3) C14 0.054(3) 0.068(3) 0.091(4) 0.041(3) 0.013(3) -0.003(2) C15 0.057(3) 0.064(3) 0.076(3) 0.046(3) 0.026(2) 0.012(2) C16 0.098(4) 0.075(4) 0.100(4) 0.057(4) 0.034(4) 0.029(3) C17 0.085(4) 0.160(7) 0.067(3) 0.076(4) 0.016(3) 0.025(4) C18 0.053(3) 0.102(4) 0.053(2) 0.045(3) 0.015(2) 0.023(3) C19 0.049(3) 0.118(5) 0.066(3) 0.039(3) 0.006(2) 0.000(3) P1 0.0381(5) 0.0628(6) 0.0472(5) 0.0329(5) 0.0170(4) 0.0129(4) S1 0.0472(5) 0.0488(5) 0.0560(6) 0.0230(5) 0.0175(4) 0.0089(4) S2 0.0393(5) 0.0493(5) 0.0484(5) 0.0243(4) 0.0152(4) 0.0055(4) Cu1 0.0314(2) 0.0586(3) 0.0423(3) 0.0260(2) 0.01340(18) 0.00584(19) In1 0.04480(19) 0.04528(19) 0.0553(2) 0.01831(15) 0.02001(13) 0.00764(12) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.465(7) 2_666 ? C1 S1 1.816(6) . ? C2 C1 1.465(7) 2_666 ? C2 S2 1.864(5) . ? C3A C4A 1.479(13) . ? C3A In1 2.215(16) . ? C4A C5A 1.367(13) . ? C5A C6A 1.492(14) . ? C3B C4B 1.506(14) . ? C3B In1 2.09(2) . ? C4B C5B 1.442(13) . ? C5B C6B 1.494(16) . ? C7 C8 1.486(7) . ? C7 In1 2.165(5) . ? C8 C9 1.507(7) . ? C9 C10 1.449(10) . ? C11 C12 1.515(7) . ? C12 C13 1.546(6) . ? C12 P1 1.863(5) . ? C14 C15 1.518(7) . ? C15 C16 1.531(8) . ? C15 P1 1.848(5) . ? C17 C18 1.533(8) . ? C18 C19 1.535(9) . ? C18 P1 1.866(5) . ? P1 Cu1 2.1979(14) . ? S1 Cu1 2.2633(13) 2_666 ? S1 In1 2.5616(15) . ? S2 Cu1 2.2470(14) . ? S2 In1 2.5635(13) . ? Cu1 S1 2.2633(13) 2_666 ? 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 C2 C1 S1 114.1(3) 2_666 . ? C1 C2 S2 113.0(3) 2_666 . ? C4A C3A In1 119.2(10) . . ? C5A C4A C3A 130.2(12) . . ? C4A C5A C6A 124.7(13) . . ? C4B C3B In1 109.8(11) . . ? C5B C4B C3B 117.4(13) . . ? C4B C5B C6B 116.3(14) . . ? C8 C7 In1 118.2(4) . . ? C7 C8 C9 114.7(5) . . ? C10 C9 C8 116.2(6) . . ? C11 C12 C13 110.2(4) . . ? C11 C12 P1 111.5(3) . . ? C13 C12 P1 115.9(4) . . ? C14 C15 C16 110.3(5) . . ? C14 C15 P1 109.3(4) . . ? C16 C15 P1 110.7(4) . . ? C17 C18 C19 112.2(5) . . ? C17 C18 P1 114.8(4) . . ? C19 C18 P1 109.4(4) . . ? C15 P1 C12 106.6(2) . . ? C15 P1 C18 105.0(3) . . ? C12 P1 C18 105.2(2) . . ? C15 P1 Cu1 111.28(18) . . ? C12 P1 Cu1 116.24(16) . . ? C18 P1 Cu1 111.71(17) . . ? C1 S1 Cu1 99.08(17) . 2_666 ? C1 S1 In1 106.71(17) . . ? Cu1 S1 In1 116.06(5) 2_666 . ? C2 S2 Cu1 98.03(17) . . ? C2 S2 In1 98.24(15) . . ? Cu1 S2 In1 127.35(5) . . ? P1 Cu1 S2 138.00(5) . . ? P1 Cu1 S1 126.23(5) . 2_666 ? S2 Cu1 S1 94.63(6) . 2_666 ? C3B In1 C7 124.0(5) . . ? C3B In1 C3A 11.2(4) . . ? C7 In1 C3A 133.9(5) . . ? C3B In1 S1 110.8(4) . . ? C7 In1 S1 104.87(18) . . ? C3A In1 S1 100.9(3) . . ? C3B In1 S2 101.9(5) . . ? C7 In1 S2 108.22(16) . . ? C3A In1 S2 100.5(5) . . ? S1 In1 S2 105.76(5) . . ? _chemical_name_common ; bis(mu!3$-1,2-dithiolatoethane-S,S,S',S')-tetra(butan-1-ido) - bis(triisopropylphosphine)-dicopper(+1)-diindium(+3) ;