# Supplementary Material (ESI) for New Journal of Chemistry # This journal is (c) The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2009 data_global _journal_name_full 'New J.Chem.' _journal_coden_Cambridge 0440 _publ_contact_author_name 'Evamarie Hey-Hawkins' _publ_contact_author_email HEY@RZ.UNI-LEIPZIG.DE _publ_section_title ; Stabilisation of an inorganic digallane by the phosphinobisthiolato P,S,S pincer ligand PPh(2-SC6H4)2 ; _publ_requested_category FM loop_ _publ_author_name 'Evamarie Hey-Hawkins' 'Santiago Gomez-Ruiz' 'Peter Lonnecke' 'Ioan Silaghi-Dumitrescu' ; L.Silaghi-Dumitrescu ; 'Ana-Maria Valean' # Attachment 'GaGa_Hey-Hawkins_NJC.cif' data_x0136fin _database_code_depnum_ccdc_archive 'CCDC 722486' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C66 H60 Ga O3 P3 S4' _chemical_formula_weight 1192.01 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Ga Ga 0.2307 1.6083 '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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.142(5) _cell_length_b 14.078(5) _cell_length_c 18.389(5) _cell_angle_alpha 97.013(5) _cell_angle_beta 109.103(5) _cell_angle_gamma 99.798(5) _cell_volume 2873.1(17) _cell_formula_units_Z 2 _cell_measurement_temperature 130(2) _cell_measurement_reflns_used 11543 _cell_measurement_theta_min 2.5547 _cell_measurement_theta_max 32.2374 _exptl_crystal_description plates _exptl_crystal_colour colourless _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.378 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1240 _exptl_absorpt_coefficient_mu 0.755 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET) (compiled Oct 18 2006,16:28:17) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_correction_T_min 0.91663 _exptl_absorpt_correction_T_max 1 _exptl_special_details ; ? ; _diffrn_ambient_temperature 130(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'ccd xcalibur s' _diffrn_measurement_method '\w scans and \f scans' _diffrn_detector_area_resol_mean 16.356 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 46215 _diffrn_reflns_av_R_equivalents 0.0608 _diffrn_reflns_av_sigmaI/netI 0.0975 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.56 _diffrn_reflns_theta_max 26.02 _reflns_number_total 11299 _reflns_number_gt 6865 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET) (compiled Oct 18 2006,16:28:17) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET) (compiled Oct 18 2006,16:28:17) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET) (compiled Oct 18 2006,16:28:17) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP3 for Windows (L. J. Farrugia, 1997)' _computing_publication_material 'WINGX (L.J. Farrugia,1999)' _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^)+(0.0089P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11299 _refine_ls_number_parameters 696 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0698 _refine_ls_R_factor_gt 0.0325 _refine_ls_wR_factor_ref 0.0483 _refine_ls_wR_factor_gt 0.0429 _refine_ls_goodness_of_fit_ref 0.950 _refine_ls_restrained_S_all 0.950 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.2629(2) 0.33896(15) 0.77022(12) 0.0179(6) Uani 1 1 d . . . C2 C 0.2632(2) 0.41381(15) 0.82852(12) 0.0164(6) Uani 1 1 d . . . C3 C 0.3708(2) 0.47792(16) 0.87508(13) 0.0222(6) Uani 1 1 d . . . H3 H 0.3709 0.5268 0.9156 0.027 Uiso 1 1 calc R . . C4 C 0.4773(2) 0.47339(16) 0.86470(13) 0.0242(6) Uani 1 1 d . . . H4 H 0.5494 0.5188 0.8967 0.029 Uiso 1 1 calc R . . C5 C 0.4761(2) 0.40063(17) 0.80616(13) 0.0244(6) Uani 1 1 d . . . H5 H 0.5481 0.3968 0.7972 0.029 Uiso 1 1 calc R . . C6 C 0.3717(2) 0.33391(16) 0.76092(13) 0.0227(6) Uani 1 1 d . . . H6 H 0.3735 0.2832 0.7225 0.027 Uiso 1 1 calc R . . C7 C 0.1570(2) 0.42770(15) 0.94323(12) 0.0175(5) Uani 1 1 d . . . C8 C 0.1574(2) 0.33575(15) 0.96570(12) 0.0164(5) Uani 1 1 d . . . C9 C 0.1849(2) 0.33166(17) 1.04496(12) 0.0209(6) Uani 1 1 d . . . H9 H 0.1869 0.2701 1.0609 0.025 Uiso 1 1 calc R . . C10 C 0.2092(2) 0.41476(17) 1.10058(13) 0.0224(6) Uani 1 1 d . . . H10 H 0.2297 0.4102 1.1543 0.027 Uiso 1 1 calc R . . C11 C 0.2040(2) 0.50461(17) 1.07864(13) 0.0244(6) Uani 1 1 d . . . H11 H 0.2171 0.5616 1.1166 0.029 Uiso 1 1 calc R . . C12 C 0.1793(2) 0.51070(16) 1.00038(13) 0.0231(6) Uani 1 1 d . . . H12 H 0.1776 0.5728 0.9853 0.028 Uiso 1 1 calc R . . C13 C 0.1197(2) 0.55343(15) 0.82776(12) 0.0179(6) Uani 1 1 d . . . C14 C 0.0401(2) 0.59866(16) 0.85151(12) 0.0253(6) Uani 1 1 d . . . H14 H -0.0067 0.5649 0.8769 0.030 Uiso 1 1 calc R . . C15 C 0.0284(2) 0.69156(17) 0.83875(13) 0.0288(7) Uani 1 1 d . . . H15 H -0.0252 0.7214 0.8563 0.035 Uiso 1 1 calc R . . C16 C 0.0935(2) 0.74143(17) 0.80096(12) 0.0280(7) Uani 1 1 d . . . H16 H 0.0865 0.8060 0.7934 0.034 Uiso 1 1 calc R . . C17 C 0.1692(2) 0.69665(16) 0.77413(12) 0.0260(6) Uani 1 1 d . . . H17 H 0.2119 0.7295 0.7461 0.031 Uiso 1 1 calc R . . C18 C 0.1832(2) 0.60374(16) 0.78790(12) 0.0220(6) Uani 1 1 d . . . H18 H 0.2367 0.5742 0.7699 0.026 Uiso 1 1 calc R . . C19 C -0.0892(2) -0.01629(16) 0.66107(12) 0.0205(6) Uani 1 1 d . . . C20 C -0.1413(2) 0.02670(15) 0.59675(12) 0.0190(6) Uani 1 1 d . . . C21 C -0.1699(2) -0.02341(16) 0.52104(13) 0.0247(6) Uani 1 1 d . . . H21 H -0.2030 0.0071 0.4781 0.030 Uiso 1 1 calc R . . C22 C -0.1512(2) -0.11687(17) 0.50655(13) 0.0293(7) Uani 1 1 d . . . H22 H -0.1706 -0.1505 0.4544 0.035 Uiso 1 1 calc R . . C23 C -0.1034(2) -0.16059(17) 0.56977(14) 0.0285(7) Uani 1 1 d . . . H23 H -0.0923 -0.2256 0.5608 0.034 Uiso 1 1 calc R . . C24 C -0.0719(2) -0.11080(16) 0.64552(13) 0.0240(6) Uani 1 1 d . . . H24 H -0.0378 -0.1416 0.6880 0.029 Uiso 1 1 calc R . . C25 C -0.2811(2) 0.19710(15) 0.71940(12) 0.0181(6) Uani 1 1 d . . . C26 C -0.2870(2) 0.13213(16) 0.65314(12) 0.0192(6) Uani 1 1 d . . . C27 C -0.3909(2) 0.05948(17) 0.61261(13) 0.0235(6) Uani 1 1 d . . . H27 H -0.3929 0.0133 0.5697 0.028 Uiso 1 1 calc R . . C28 C -0.4905(2) 0.05339(17) 0.63354(13) 0.0273(6) Uani 1 1 d . . . H28 H -0.5609 0.0041 0.6052 0.033 Uiso 1 1 calc R . . C29 C -0.4858(2) 0.12070(17) 0.69693(13) 0.0259(6) Uani 1 1 d . . . H29 H -0.5547 0.1188 0.7110 0.031 Uiso 1 1 calc R . . C30 C -0.3836(2) 0.18951(17) 0.73918(13) 0.0222(6) Uani 1 1 d . . . H30 H -0.3820 0.2335 0.7832 0.027 Uiso 1 1 calc R . . C31 C -0.2075(2) 0.19568(15) 0.53246(11) 0.0169(6) Uani 1 1 d . . . C32 C -0.1205(2) 0.23005(16) 0.50255(12) 0.0243(6) Uani 1 1 d . . . H32 H -0.0412 0.2223 0.5264 0.029 Uiso 1 1 calc R . . C33 C -0.1481(2) 0.27549(16) 0.43835(13) 0.0273(6) Uani 1 1 d . . . H33 H -0.0884 0.2972 0.4174 0.033 Uiso 1 1 calc R . . C34 C -0.2619(2) 0.28928(16) 0.40484(13) 0.0252(6) Uani 1 1 d . . . H34 H -0.2797 0.3233 0.3623 0.030 Uiso 1 1 calc R . . C35 C -0.3499(2) 0.25405(16) 0.43264(12) 0.0279(7) Uani 1 1 d . . . H35 H -0.4292 0.2616 0.4081 0.034 Uiso 1 1 calc R . . C36 C -0.3231(2) 0.20745(16) 0.49659(12) 0.0245(6) Uani 1 1 d . . . H36 H -0.3840 0.1835 0.5159 0.029 Uiso 1 1 calc R . . C37 C 0.5811(2) 0.80614(16) 0.80226(12) 0.0179(6) Uani 1 1 d . . . C38 C 0.6627(2) 0.83624(17) 0.76663(13) 0.0289(7) Uani 1 1 d . . . H38 H 0.7054 0.9027 0.7790 0.035 Uiso 1 1 calc R . . C39 C 0.6811(2) 0.76834(19) 0.71285(14) 0.0361(7) Uani 1 1 d . . . H39 H 0.7359 0.7887 0.6879 0.043 Uiso 1 1 calc R . . C40 C 0.6202(2) 0.67153(19) 0.69556(13) 0.0314(7) Uani 1 1 d . . . H40 H 0.6334 0.6254 0.6588 0.038 Uiso 1 1 calc R . . C41 C 0.5407(2) 0.64145(17) 0.73122(12) 0.0272(6) Uani 1 1 d . . . H41 H 0.4994 0.5746 0.7194 0.033 Uiso 1 1 calc R . . C42 C 0.5208(2) 0.70894(16) 0.78455(12) 0.0233(6) Uani 1 1 d . . . H42 H 0.4654 0.6882 0.8090 0.028 Uiso 1 1 calc R . . C43 C 0.4978(2) 0.82699(15) 0.93235(11) 0.0164(6) Uani 1 1 d . . . C44 C 0.5657(2) 0.76827(15) 0.97486(12) 0.0190(6) Uani 1 1 d . . . H44 H 0.6405 0.7638 0.9703 0.023 Uiso 1 1 calc R . . C45 C 0.5247(2) 0.71646(15) 1.02359(12) 0.0227(6) Uani 1 1 d . . . H45 H 0.5722 0.6781 1.0537 0.027 Uiso 1 1 calc R . . C46 C 0.4139(2) 0.72079(16) 1.02824(12) 0.0232(6) Uani 1 1 d . . . H46 H 0.3856 0.6849 1.0615 0.028 Uiso 1 1 calc R . . C47 C 0.3445(2) 0.77671(16) 0.98500(12) 0.0236(6) Uani 1 1 d . . . H47 H 0.2679 0.7783 0.9877 0.028 Uiso 1 1 calc R . . C48 C 0.3870(2) 0.83073(15) 0.93754(12) 0.0186(6) Uani 1 1 d . . . H48 H 0.3401 0.8704 0.9085 0.022 Uiso 1 1 calc R . . C49 C 0.4398(2) 0.95246(15) 0.81809(12) 0.0164(6) Uani 1 1 d . . . C50 C 0.3639(2) 0.90922(16) 0.74250(12) 0.0198(6) Uani 1 1 d . . . H50 H 0.3789 0.8535 0.7158 0.024 Uiso 1 1 calc R . . C51 C 0.2666(2) 0.94641(16) 0.70559(12) 0.0224(6) Uani 1 1 d . . . H51 H 0.2142 0.9158 0.6540 0.027 Uiso 1 1 calc R . . C52 C 0.2454(2) 1.02855(16) 0.74406(13) 0.0229(6) Uani 1 1 d . . . H52 H 0.1781 1.0540 0.7190 0.027 Uiso 1 1 calc R . . C53 C 0.3221(2) 1.07315(16) 0.81855(13) 0.0232(6) Uani 1 1 d . . . H53 H 0.3081 1.1302 0.8442 0.028 Uiso 1 1 calc R . . C54 C 0.4191(2) 1.03605(15) 0.85647(12) 0.0205(6) Uani 1 1 d . . . H54 H 0.4712 1.0669 0.9081 0.025 Uiso 1 1 calc R . . C55 C 0.6880(2) 0.98246(15) 0.92430(12) 0.0165(6) Uani 1 1 d . . . C56 C 0.7619(2) 0.97555(16) 0.99879(12) 0.0205(6) Uani 1 1 d . . . H56 H 0.7353 0.9281 1.0255 0.025 Uiso 1 1 calc R . . C57 C 0.8732(2) 1.03727(17) 1.03362(13) 0.0278(6) Uani 1 1 d . . . H57 H 0.9234 1.0326 1.0844 0.033 Uiso 1 1 calc R . . C58 C 0.9122(2) 1.10631(16) 0.99459(14) 0.0280(6) Uani 1 1 d . . . H58 H 0.9898 1.1479 1.0184 0.034 Uiso 1 1 calc R . . C59 C 0.8398(2) 1.11522(16) 0.92184(14) 0.0248(6) Uani 1 1 d . . . H59 H 0.8667 1.1634 0.8958 0.030 Uiso 1 1 calc R . . C60 C 0.7279(2) 1.05389(16) 0.88676(13) 0.0219(6) Uani 1 1 d . . . H60 H 0.6775 1.0603 0.8366 0.026 Uiso 1 1 calc R . . P1 P 0.12265(6) 0.42686(4) 0.83906(3) 0.01895(16) Uani 1 1 d . . . P2 P -0.15827(6) 0.14920(4) 0.62315(3) 0.01893(16) Uani 1 1 d . . . P3 P 0.55286(6) 0.89394(4) 0.87009(3) 0.01783(15) Uani 1 1 d . . . S1 S 0.13254(6) 0.25685(4) 0.70403(3) 0.02230(16) Uani 1 1 d . . . S2 S 0.13265(6) 0.22466(4) 0.90006(3) 0.02012(15) Uani 1 1 d . . . S3 S -0.05130(6) 0.04346(4) 0.75955(3) 0.02169(15) Uani 1 1 d . . . S4 S -0.15163(6) 0.28733(4) 0.77647(3) 0.02237(15) Uani 1 1 d . . . Ga1 Ga 0.00408(3) 0.217196(18) 0.769281(14) 0.01941(7) Uani 1 1 d . . . O1 O 0.1508(2) 0.40704(13) 0.54824(10) 0.0482(5) Uani 1 1 d . . . O2 O 0.46728(19) 0.42761(12) 0.60244(9) 0.0418(5) Uani 1 1 d . . . O3 O 0.70915(19) 0.49735(14) 0.59919(10) 0.0466(5) Uani 1 1 d . . . C100 C 0.0818(3) 0.45264(18) 0.58464(14) 0.0452(8) Uani 1 1 d . . . H10A H 0.0965 0.4365 0.6369 0.068 Uiso 1 1 calc R . . H10B H -0.0033 0.4290 0.5528 0.068 Uiso 1 1 calc R . . H10C H 0.1044 0.5240 0.5895 0.068 Uiso 1 1 calc R . . C101 C 0.2744(3) 0.44776(19) 0.58735(15) 0.0417(8) Uani 1 1 d . . . H10D H 0.2949 0.4526 0.6446 0.050 Uiso 1 1 calc R . . H10E H 0.2945 0.5147 0.5770 0.050 Uiso 1 1 calc R . . C102 C 0.5417(3) 0.3700(2) 0.58288(16) 0.0555(10) Uani 1 1 d . . . H10F H 0.5282 0.3638 0.5263 0.067 Uiso 1 1 calc R . . H10G H 0.5214 0.3033 0.5937 0.067 Uiso 1 1 calc R . . C103 C 0.3447(3) 0.38464(19) 0.55924(15) 0.0454(8) Uani 1 1 d . . . H10H H 0.3238 0.3171 0.5682 0.054 Uiso 1 1 calc R . . H10I H 0.3275 0.3818 0.5024 0.054 Uiso 1 1 calc R . . C104 C 0.6697(3) 0.4160(2) 0.62948(16) 0.0519(9) Uani 1 1 d . . . H10J H 0.6792 0.4378 0.6849 0.062 Uiso 1 1 calc R . . H10K H 0.7190 0.3672 0.6277 0.062 Uiso 1 1 calc R . . C105 C 0.8326(3) 0.5379(3) 0.63749(18) 0.0758(11) Uani 1 1 d . . . H10L H 0.8488 0.5641 0.6927 0.114 Uiso 1 1 calc R . . H10M H 0.8576 0.5909 0.6124 0.114 Uiso 1 1 calc R . . H10N H 0.8773 0.4868 0.6339 0.114 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0182(16) 0.0175(13) 0.0200(14) 0.0082(11) 0.0073(12) 0.0044(12) C2 0.0163(16) 0.0152(12) 0.0204(14) 0.0071(11) 0.0084(12) 0.0045(12) C3 0.0226(18) 0.0216(14) 0.0252(15) 0.0069(12) 0.0100(13) 0.0073(13) C4 0.0167(17) 0.0230(14) 0.0310(15) 0.0079(12) 0.0061(13) 0.0021(12) C5 0.0202(17) 0.0297(15) 0.0323(16) 0.0139(13) 0.0160(14) 0.0106(14) C6 0.0264(18) 0.0216(14) 0.0238(15) 0.0056(12) 0.0122(13) 0.0081(13) C7 0.0090(15) 0.0177(13) 0.0247(14) 0.0021(11) 0.0065(12) 0.0007(11) C8 0.0086(15) 0.0221(13) 0.0187(14) 0.0013(11) 0.0070(11) 0.0018(11) C9 0.0132(16) 0.0268(14) 0.0245(15) 0.0063(12) 0.0090(12) 0.0038(12) C10 0.0144(16) 0.0364(15) 0.0161(14) 0.0005(12) 0.0072(12) 0.0052(13) C11 0.0150(16) 0.0305(15) 0.0258(15) -0.0032(12) 0.0094(12) 0.0018(13) C12 0.0200(17) 0.0204(13) 0.0299(16) 0.0036(12) 0.0104(13) 0.0049(12) C13 0.0149(16) 0.0173(13) 0.0166(13) 0.0000(10) 0.0025(11) -0.0004(12) C14 0.0227(17) 0.0287(15) 0.0282(15) 0.0098(12) 0.0109(13) 0.0088(13) C15 0.0249(18) 0.0316(15) 0.0332(16) 0.0056(13) 0.0106(14) 0.0144(14) C16 0.0327(19) 0.0200(14) 0.0268(15) 0.0077(12) 0.0026(14) 0.0080(14) C17 0.0327(19) 0.0252(14) 0.0194(14) 0.0072(12) 0.0094(13) 0.0021(13) C18 0.0205(17) 0.0253(14) 0.0194(14) 0.0021(11) 0.0073(12) 0.0040(13) C19 0.0154(16) 0.0227(13) 0.0234(14) 0.0038(11) 0.0077(12) 0.0028(12) C20 0.0155(16) 0.0218(13) 0.0199(14) 0.0038(11) 0.0061(12) 0.0053(12) C21 0.0243(17) 0.0281(14) 0.0207(15) 0.0043(12) 0.0058(13) 0.0077(13) C22 0.0322(19) 0.0282(15) 0.0247(15) -0.0035(12) 0.0095(14) 0.0066(14) C23 0.0283(18) 0.0206(14) 0.0381(17) -0.0013(13) 0.0145(14) 0.0084(13) C24 0.0206(17) 0.0230(14) 0.0289(15) 0.0078(12) 0.0072(13) 0.0072(13) C25 0.0190(16) 0.0200(13) 0.0188(14) 0.0101(11) 0.0066(12) 0.0091(12) C26 0.0216(17) 0.0205(13) 0.0162(14) 0.0048(11) 0.0054(12) 0.0087(13) C27 0.0264(18) 0.0240(14) 0.0208(14) 0.0024(12) 0.0091(13) 0.0073(13) C28 0.0200(18) 0.0267(15) 0.0287(15) 0.0015(12) 0.0047(13) -0.0013(13) C29 0.0200(18) 0.0336(15) 0.0316(16) 0.0138(13) 0.0135(14) 0.0112(14) C30 0.0256(18) 0.0216(14) 0.0230(15) 0.0061(12) 0.0109(13) 0.0094(13) C31 0.0178(16) 0.0176(13) 0.0132(13) -0.0015(10) 0.0038(12) 0.0047(12) C32 0.0218(17) 0.0263(14) 0.0253(15) 0.0070(12) 0.0072(13) 0.0077(13) C33 0.0309(19) 0.0297(15) 0.0247(15) 0.0074(12) 0.0147(14) 0.0046(14) C34 0.036(2) 0.0179(13) 0.0186(14) 0.0025(11) 0.0064(13) 0.0059(13) C35 0.0272(18) 0.0344(15) 0.0216(15) 0.0052(12) 0.0038(13) 0.0151(14) C36 0.0235(18) 0.0282(14) 0.0228(14) 0.0029(12) 0.0100(13) 0.0064(13) C37 0.0202(16) 0.0180(13) 0.0157(13) 0.0016(11) 0.0058(11) 0.0068(12) C38 0.0331(19) 0.0212(14) 0.0325(16) -0.0034(12) 0.0160(14) 0.0033(14) C39 0.035(2) 0.0415(17) 0.0407(17) 0.0012(15) 0.0275(16) 0.0093(16) C40 0.037(2) 0.0354(17) 0.0256(16) 0.0009(13) 0.0114(14) 0.0215(16) C41 0.0340(19) 0.0210(14) 0.0263(15) 0.0037(12) 0.0078(14) 0.0120(14) C42 0.0232(17) 0.0256(14) 0.0218(15) 0.0065(12) 0.0065(13) 0.0089(13) C43 0.0171(16) 0.0156(12) 0.0149(13) 0.0005(10) 0.0049(11) 0.0030(12) C44 0.0145(16) 0.0167(12) 0.0240(14) 0.0014(11) 0.0061(12) 0.0023(12) C45 0.0221(17) 0.0176(13) 0.0270(15) 0.0069(11) 0.0060(13) 0.0041(12) C46 0.0248(18) 0.0223(14) 0.0187(14) 0.0024(11) 0.0080(13) -0.0042(13) C47 0.0198(17) 0.0257(14) 0.0230(14) -0.0018(12) 0.0091(13) 0.0010(13) C48 0.0184(16) 0.0156(12) 0.0164(13) -0.0019(10) 0.0008(12) 0.0041(12) C49 0.0179(16) 0.0181(13) 0.0182(14) 0.0064(11) 0.0101(12) 0.0072(12) C50 0.0216(17) 0.0160(13) 0.0224(14) 0.0034(11) 0.0090(13) 0.0034(12) C51 0.0199(17) 0.0224(14) 0.0180(14) 0.0009(11) 0.0010(12) 0.0002(12) C52 0.0181(16) 0.0258(14) 0.0281(15) 0.0115(12) 0.0084(13) 0.0088(13) C53 0.0267(18) 0.0212(14) 0.0254(15) 0.0028(12) 0.0125(13) 0.0101(13) C54 0.0215(17) 0.0193(13) 0.0185(14) 0.0016(11) 0.0052(12) 0.0039(12) C55 0.0158(16) 0.0147(12) 0.0214(14) 0.0028(11) 0.0093(12) 0.0047(11) C56 0.0193(17) 0.0192(13) 0.0225(14) 0.0051(11) 0.0058(13) 0.0056(13) C57 0.0215(18) 0.0320(15) 0.0247(15) 0.0020(12) 0.0018(13) 0.0074(14) C58 0.0176(17) 0.0254(14) 0.0385(17) -0.0039(13) 0.0134(14) -0.0016(13) C59 0.0250(18) 0.0228(14) 0.0334(16) 0.0059(12) 0.0195(14) 0.0041(13) C60 0.0218(17) 0.0251(14) 0.0197(14) 0.0022(12) 0.0090(13) 0.0059(13) P1 0.0180(4) 0.0177(3) 0.0221(4) 0.0034(3) 0.0091(3) 0.0029(3) P2 0.0184(4) 0.0211(3) 0.0165(4) 0.0025(3) 0.0052(3) 0.0051(3) P3 0.0178(4) 0.0181(3) 0.0192(4) 0.0043(3) 0.0077(3) 0.0055(3) S1 0.0239(4) 0.0223(3) 0.0209(4) 0.0024(3) 0.0103(3) 0.0023(3) S2 0.0196(4) 0.0188(3) 0.0209(3) 0.0039(3) 0.0054(3) 0.0049(3) S3 0.0238(4) 0.0210(3) 0.0196(3) 0.0055(3) 0.0064(3) 0.0047(3) S4 0.0197(4) 0.0218(3) 0.0238(4) -0.0010(3) 0.0060(3) 0.0070(3) Ga1 0.01816(18) 0.02066(15) 0.02144(16) 0.00638(12) 0.00790(13) 0.00625(13) O1 0.0485(16) 0.0491(13) 0.0380(12) -0.0020(10) 0.0152(12) -0.0049(12) O2 0.0544(16) 0.0303(11) 0.0389(12) 0.0016(9) 0.0131(11) 0.0153(12) O3 0.0464(16) 0.0576(14) 0.0370(12) 0.0082(10) 0.0093(11) 0.0263(13) C100 0.052(2) 0.0312(16) 0.0412(18) 0.0050(14) 0.0076(17) 0.0004(16) C101 0.048(2) 0.0322(16) 0.0379(18) 0.0058(14) 0.0081(17) 0.0069(17) C102 0.078(3) 0.0401(19) 0.052(2) 0.0073(16) 0.020(2) 0.030(2) C103 0.056(3) 0.0309(17) 0.0369(18) -0.0004(14) 0.0072(17) 0.0020(18) C104 0.072(3) 0.047(2) 0.0423(19) 0.0107(16) 0.0130(19) 0.040(2) C105 0.047(3) 0.108(3) 0.071(2) 0.013(2) 0.013(2) 0.032(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.407(3) . ? C1 C6 1.398(3) . ? C1 S1 1.760(2) . ? C2 C3 1.390(3) . ? C2 P1 1.816(2) . ? C3 C4 1.378(3) . ? C4 C5 1.387(3) . ? C5 C6 1.377(3) . ? C7 C12 1.396(3) . ? C7 C8 1.406(3) . ? C7 P1 1.820(2) . ? C8 C9 1.396(3) . ? C8 S2 1.770(2) . ? C9 C10 1.376(3) . ? C10 C11 1.379(3) . ? C11 C12 1.387(3) . ? C13 C14 1.395(3) . ? C13 C18 1.395(3) . ? C13 P1 1.824(2) . ? C14 C15 1.379(3) . ? C15 C16 1.375(3) . ? C16 C17 1.379(3) . ? C17 C18 1.390(3) . ? C19 C24 1.392(3) . ? C19 C20 1.407(3) . ? C19 S3 1.775(2) . ? C20 C21 1.385(3) . ? C20 P2 1.798(2) . ? C21 C22 1.382(3) . ? C22 C23 1.386(3) . ? C23 C24 1.378(3) . ? C25 C26 1.406(3) . ? C25 C30 1.397(3) . ? C25 S4 1.761(3) . ? C26 C27 1.398(3) . ? C26 P2 1.809(2) . ? C27 C28 1.376(3) . ? C28 C29 1.389(3) . ? C29 C30 1.363(3) . ? C31 C32 1.387(3) . ? C31 C36 1.390(3) . ? C31 P2 1.820(2) . ? C32 C33 1.383(3) . ? C33 C34 1.375(3) . ? C34 C35 1.375(3) . ? C35 C36 1.389(3) . ? C37 C42 1.381(3) . ? C37 C38 1.393(3) . ? C37 P3 1.802(2) . ? C38 C39 1.389(3) . ? C39 C40 1.379(3) . ? C40 C41 1.373(3) . ? C41 C42 1.389(3) . ? C43 C44 1.394(3) . ? C43 C48 1.389(3) . ? C43 P3 1.788(2) . ? C44 C45 1.382(3) . ? C45 C46 1.386(3) . ? C46 C47 1.380(3) . ? C47 C48 1.389(3) . ? C49 C50 1.384(3) . ? C49 C54 1.400(3) . ? C49 P3 1.788(2) . ? C50 C51 1.380(3) . ? C51 C52 1.387(3) . ? C52 C53 1.376(3) . ? C53 C54 1.381(3) . ? C55 C60 1.395(3) . ? C55 C56 1.396(3) . ? C55 P3 1.780(2) . ? C56 C57 1.375(3) . ? C57 C58 1.385(3) . ? C58 C59 1.374(3) . ? C59 C60 1.378(3) . ? P2 Ga1 2.6992(9) . ? S1 Ga1 2.2970(9) . ? S2 Ga1 2.3784(8) . ? S3 Ga1 2.3918(10) . ? S4 Ga1 2.3095(10) . ? O1 C101 1.414(3) . ? O1 C100 1.416(3) . ? O2 C102 1.413(3) . ? O2 C103 1.419(3) . ? O3 C104 1.412(3) . ? O3 C105 1.410(4) . ? C101 C103 1.490(3) . ? C102 C104 1.490(4) . ? 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 C6 118.0(2) . . ? C2 C1 S1 123.83(19) . . ? C6 C1 S1 118.05(17) . . ? C3 C2 C1 119.1(2) . . ? C3 C2 P1 121.58(17) . . ? C1 C2 P1 119.32(19) . . ? C4 C3 C2 122.6(2) . . ? C5 C4 C3 118.1(2) . . ? C6 C5 C4 120.6(2) . . ? C5 C6 C1 121.6(2) . . ? C12 C7 C8 118.92(19) . . ? C12 C7 P1 125.29(16) . . ? C8 C7 P1 115.77(16) . . ? C9 C8 C7 118.54(19) . . ? C9 C8 S2 117.43(16) . . ? C7 C8 S2 123.94(15) . . ? C10 C9 C8 121.5(2) . . ? C11 C10 C9 120.3(2) . . ? C10 C11 C12 119.1(2) . . ? C11 C12 C7 121.5(2) . . ? C14 C13 C18 117.68(19) . . ? C14 C13 P1 119.07(17) . . ? C18 C13 P1 122.80(16) . . ? C15 C14 C13 121.0(2) . . ? C14 C15 C16 120.8(2) . . ? C15 C16 C17 119.2(2) . . ? C18 C17 C16 120.4(2) . . ? C17 C18 C13 120.8(2) . . ? C24 C19 C20 117.8(2) . . ? C24 C19 S3 119.72(16) . . ? C20 C19 S3 122.44(17) . . ? C21 C20 C19 120.11(19) . . ? C21 C20 P2 125.55(16) . . ? C19 C20 P2 114.28(16) . . ? C22 C21 C20 121.4(2) . . ? C23 C22 C21 118.6(2) . . ? C22 C23 C24 120.7(2) . . ? C19 C24 C23 121.4(2) . . ? C26 C25 C30 117.8(2) . . ? C26 C25 S4 122.62(19) . . ? C30 C25 S4 119.60(18) . . ? C25 C26 C27 119.5(2) . . ? C25 C26 P2 117.45(19) . . ? C27 C26 P2 123.01(18) . . ? C28 C27 C26 121.4(2) . . ? C29 C28 C27 118.7(2) . . ? C30 C29 C28 120.8(2) . . ? C29 C30 C25 121.7(2) . . ? C32 C31 C36 118.8(2) . . ? C32 C31 P2 116.99(18) . . ? C36 C31 P2 123.90(18) . . ? C31 C32 C33 120.7(2) . . ? C34 C33 C32 120.0(2) . . ? C33 C34 C35 120.2(2) . . ? C34 C35 C36 120.0(2) . . ? C31 C36 C35 120.3(2) . . ? C42 C37 C38 119.7(2) . . ? C42 C37 P3 120.20(18) . . ? C38 C37 P3 120.14(18) . . ? C39 C38 C37 119.5(2) . . ? C40 C39 C38 120.3(2) . . ? C41 C40 C39 120.3(2) . . ? C40 C41 C42 119.9(2) . . ? C41 C42 C37 120.4(2) . . ? C44 C43 C48 119.5(2) . . ? C44 C43 P3 119.52(18) . . ? C48 C43 P3 120.98(16) . . ? C45 C44 C43 120.2(2) . . ? C44 C45 C46 119.7(2) . . ? C47 C46 C45 120.6(2) . . ? C46 C47 C48 119.7(2) . . ? C47 C48 C43 120.2(2) . . ? C50 C49 C54 119.6(2) . . ? C50 C49 P3 119.97(16) . . ? C54 C49 P3 120.09(17) . . ? C51 C50 C49 120.5(2) . . ? C50 C51 C52 119.8(2) . . ? C53 C52 C51 119.9(2) . . ? C52 C53 C54 120.8(2) . . ? C53 C54 C49 119.3(2) . . ? C60 C55 C56 119.0(2) . . ? C60 C55 P3 118.16(18) . . ? C56 C55 P3 122.32(17) . . ? C57 C56 C55 120.1(2) . . ? C56 C57 C58 119.9(2) . . ? C59 C58 C57 120.7(3) . . ? C58 C59 C60 119.7(2) . . ? C55 C60 C59 120.5(2) . . ? C2 P1 C13 102.49(10) . . ? C2 P1 C7 101.38(10) . . ? C13 P1 C7 105.44(9) . . ? C20 P2 C26 104.41(11) . . ? C20 P2 C31 106.60(10) . . ? C26 P2 C31 104.63(10) . . ? C20 P2 Ga1 104.92(8) . . ? C26 P2 Ga1 95.41(8) . . ? C31 P2 Ga1 136.66(8) . . ? C55 P3 C43 111.80(10) . . ? C55 P3 C49 110.44(11) . . ? C43 P3 C49 108.23(11) . . ? C55 P3 C37 109.11(11) . . ? C43 P3 C37 107.15(10) . . ? C49 P3 C37 110.05(10) . . ? C1 S1 Ga1 108.53(8) . . ? C8 S2 Ga1 115.12(7) . . ? C19 S3 Ga1 109.52(7) . . ? C25 S4 Ga1 104.24(8) . . ? S1 Ga1 S4 128.65(3) . . ? S1 Ga1 S2 104.10(4) . . ? S4 Ga1 S2 107.25(3) . . ? S1 Ga1 S3 111.41(2) . . ? S4 Ga1 S3 109.70(3) . . ? S2 Ga1 S3 87.32(2) . . ? S1 Ga1 P2 83.55(3) . . ? S4 Ga1 P2 78.79(3) . . ? S2 Ga1 P2 162.15(2) . . ? S3 Ga1 P2 74.85(2) . . ? C101 O1 C100 111.2(2) . . ? C102 O2 C103 111.2(2) . . ? C104 O3 C105 111.9(2) . . ? O1 C101 C103 109.7(2) . . ? O2 C102 C104 110.2(2) . . ? O2 C103 C101 106.9(2) . . ? O3 C104 C102 110.2(2) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.02 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.313 _refine_diff_density_min -0.342 _refine_diff_density_rms 0.061 #============================================================================ data_x0098fin _database_code_depnum_ccdc_archive 'CCDC 722487' _audit_creation_date 2006-12-12T13:33:52-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_sum 'C19 H16 Ga P S2' _chemical_formula_weight 409.13 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 15.84180(10) _cell_length_b 14.39930(10) _cell_length_c 15.89700(10) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 3626.28(4) _cell_formula_units_Z 8 _cell_measurement_temperature 130(2) _cell_measurement_reflns_used 56554 _cell_measurement_theta_min 2.8176 _cell_measurement_theta_max 32.2736 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.2 _exptl_crystal_density_diffrn 1.499 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1664 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.832 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET) (compiled Oct 18 2006,16:28:17) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_correction_T_min 0.69135 _exptl_absorpt_correction_T_max 1 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 130(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_detector_area_resol_mean 16.356 _diffrn_orient_matrix_ub_11 0.0134093536 _diffrn_orient_matrix_ub_12 -0.024811494 _diffrn_orient_matrix_ub_13 -0.034985004 _diffrn_orient_matrix_ub_21 -0.0161382915 _diffrn_orient_matrix_ub_22 0.0319193905 _diffrn_orient_matrix_ub_23 -0.0275431449 _diffrn_orient_matrix_ub_31 0.0444912164 _diffrn_orient_matrix_ub_32 0.0190509895 _diffrn_orient_matrix_ub_33 0.0005749774 _diffrn_measurement_device_type 'ccd Xcalibur S' _diffrn_measurement_method '\w- amd \f-scans' _diffrn_reflns_av_R_equivalents 0.0213 _diffrn_reflns_av_unetI/netI 0.009 _diffrn_reflns_number 94604 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.83 _diffrn_reflns_theta_max 30.5 _diffrn_reflns_theta_full 30.5 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _reflns_number_total 5538 _reflns_number_gt 4789 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET) (compiled Oct 18 2006,16:28:17) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET) (compiled Oct 18 2006,16:28:17) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET) (compiled Oct 18 2006,16:28:17) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP3 for Windows (L. J. Farrugia, 1997)' _computing_publication_material 'WINGX (L.J. Farrugia,1999)' #----------------------------------------------------------------------------# # 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^)+(0.0205P)^2^+3.1752P] 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 5538 _refine_ls_number_parameters 209 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0354 _refine_ls_R_factor_gt 0.0262 _refine_ls_wR_factor_ref 0.0686 _refine_ls_wR_factor_gt 0.0588 _refine_ls_goodness_of_fit_ref 1.228 _refine_ls_restrained_S_all 1.228 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.441 _refine_diff_density_min -0.372 _refine_diff_density_rms 0.072 #----------------------------------------------------------------------------# # 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 Ga Ga 0.2307 1.6083 '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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ga1 Ga 0.239039(11) 0.673697(13) 0.091419(11) 0.01983(5) Uani 1 1 d . . . S1 S 0.10845(3) 0.70781(3) 0.03864(3) 0.02640(9) Uani 1 1 d . . . S2 S 0.31593(3) 0.80446(4) 0.11708(3) 0.03084(11) Uani 1 1 d . . . P1 P 0.29182(2) 0.66703(3) -0.04654(2) 0.01459(7) Uani 1 1 d . . . C1 C 0.19814(9) 0.66807(10) -0.10994(9) 0.0166(3) Uani 1 1 d . . . C2 C 0.12140(10) 0.68924(10) -0.07025(10) 0.0183(3) Uani 1 1 d . . . C3 C 0.04872(10) 0.69548(11) -0.12025(12) 0.0234(3) Uani 1 1 d . . . H3 H -0.0039 0.7098 -0.0948 0.028 Uiso 1 1 calc R . . C4 C 0.05273(11) 0.68103(12) -0.20630(12) 0.0276(4) Uani 1 1 d . . . H4 H 0.0028 0.6855 -0.2391 0.033 Uiso 1 1 calc R . . C5 C 0.12884(12) 0.66015(13) -0.24517(11) 0.0280(4) Uani 1 1 d . . . H5 H 0.1313 0.6508 -0.3043 0.034 Uiso 1 1 calc R . . C6 C 0.20117(11) 0.65310(11) -0.19671(10) 0.0219(3) Uani 1 1 d . . . H6 H 0.2534 0.6379 -0.2227 0.026 Uiso 1 1 calc R . . C7 C 0.34051(9) 0.77902(10) -0.05668(10) 0.0174(3) Uani 1 1 d . . . C8 C 0.34785(10) 0.83621(11) 0.01467(11) 0.0211(3) Uani 1 1 d . . . C9 C 0.38568(11) 0.92372(12) 0.00459(13) 0.0272(4) Uani 1 1 d . . . H9 H 0.3907 0.9639 0.0517 0.033 Uiso 1 1 calc R . . C10 C 0.41549(11) 0.95207(12) -0.07240(14) 0.0294(4) Uani 1 1 d . . . H10 H 0.4417 1.0111 -0.0775 0.035 Uiso 1 1 calc R . . C11 C 0.40786(11) 0.89582(12) -0.14259(12) 0.0284(4) Uani 1 1 d . . . H11 H 0.4283 0.9162 -0.1956 0.034 Uiso 1 1 calc R . . C12 C 0.37016(10) 0.80974(11) -0.13471(11) 0.0224(3) Uani 1 1 d . . . H12 H 0.3643 0.7711 -0.1828 0.027 Uiso 1 1 calc R . . C13 C 0.36360(10) 0.58046(10) -0.08554(9) 0.0169(3) Uani 1 1 d . . . C14 C 0.33227(11) 0.49352(11) -0.10880(11) 0.0240(3) Uani 1 1 d . . . H14 H 0.2731 0.4825 -0.109 0.029 Uiso 1 1 calc R . . C15 C 0.38770(13) 0.42337(12) -0.13157(12) 0.0304(4) Uani 1 1 d . . . H15 H 0.3666 0.3645 -0.1483 0.037 Uiso 1 1 calc R . . C16 C 0.47407(13) 0.43927(13) -0.12985(12) 0.0307(4) Uani 1 1 d . . . H16 H 0.512 0.3911 -0.1453 0.037 Uiso 1 1 calc R . . C17 C 0.50516(11) 0.52471(13) -0.10577(13) 0.0304(4) Uani 1 1 d . . . H17 H 0.5644 0.535 -0.1042 0.037 Uiso 1 1 calc R . . C18 C 0.45013(10) 0.59589(12) -0.08374(11) 0.0232(3) Uani 1 1 d . . . H18 H 0.4716 0.6548 -0.0675 0.028 Uiso 1 1 calc R . . C19 C 0.24770(16) 0.57475(16) 0.17399(13) 0.0400(5) Uani 1 1 d . . . H19A H 0.2973 0.5852 0.2095 0.06 Uiso 1 1 calc R . . H19B H 0.2533 0.515 0.145 0.06 Uiso 1 1 calc R . . H19C H 0.1968 0.5741 0.2091 0.06 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ga1 0.01974(9) 0.02477(9) 0.01499(8) -0.00043(6) 0.00226(6) -0.00094(6) S1 0.01763(17) 0.0370(2) 0.02454(19) -0.00444(17) 0.00443(15) 0.00387(16) S2 0.0281(2) 0.0404(2) 0.0240(2) -0.01599(18) 0.00687(16) -0.01187(18) P1 0.01417(16) 0.01517(16) 0.01445(16) -0.00116(13) 0.00077(13) -0.00065(13) C1 0.0177(6) 0.0146(6) 0.0174(6) 0.0005(5) -0.0021(5) -0.0014(5) C2 0.0182(7) 0.0143(6) 0.0226(7) 0.0005(5) 0.0006(5) -0.0014(5) C3 0.0170(7) 0.0188(7) 0.0345(9) 0.0045(6) -0.0031(6) -0.0011(5) C4 0.0236(8) 0.0264(8) 0.0327(9) 0.0050(7) -0.0117(7) -0.0039(6) C5 0.0309(9) 0.0313(9) 0.0218(7) 0.0011(7) -0.0088(7) -0.0062(7) C6 0.0236(8) 0.0234(7) 0.0186(7) -0.0007(6) -0.0008(6) -0.0036(6) C7 0.0151(6) 0.0158(6) 0.0212(7) -0.0006(5) -0.0014(5) -0.0007(5) C8 0.0151(6) 0.0214(7) 0.0270(8) -0.0058(6) 0.0005(6) 0.0001(5) C9 0.0188(7) 0.0196(7) 0.0432(10) -0.0092(7) -0.0012(7) -0.0002(6) C10 0.0202(7) 0.0161(7) 0.0519(11) 0.0046(7) -0.0040(7) -0.0023(6) C11 0.0251(8) 0.0252(8) 0.0349(9) 0.0123(7) -0.0032(7) -0.0043(6) C12 0.0219(7) 0.0225(7) 0.0227(7) 0.0032(6) -0.0009(6) -0.0013(6) C13 0.0182(7) 0.0165(6) 0.0159(6) -0.0006(5) 0.0026(5) 0.0011(5) C14 0.0238(8) 0.0174(7) 0.0306(8) -0.0026(6) -0.0011(6) 0.0010(6) C15 0.0393(10) 0.0183(8) 0.0337(9) -0.0035(7) -0.0021(8) 0.0052(7) C16 0.0355(9) 0.0249(8) 0.0316(9) 0.0029(7) 0.0093(8) 0.0129(7) C17 0.0212(8) 0.0290(9) 0.0411(10) 0.0091(8) 0.0112(7) 0.0052(7) C18 0.0209(7) 0.0197(7) 0.0289(8) 0.0038(6) 0.0030(6) 0.0000(6) C19 0.0537(13) 0.0421(12) 0.0243(9) 0.0106(8) -0.0031(9) 0.0009(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 Ga1 C19 1.942(2) . ? Ga1 S2 2.2794(5) . ? Ga1 S1 2.2858(5) . ? Ga1 P1 2.3491(4) . ? S1 C2 1.7636(17) . ? S2 C8 1.7650(18) . ? P1 C1 1.7940(15) . ? P1 C7 1.7949(15) . ? P1 C13 1.7975(15) . ? C1 C6 1.397(2) . ? C1 C2 1.403(2) . ? C2 C3 1.402(2) . ? C3 C4 1.385(3) . ? C4 C5 1.388(3) . ? C5 C6 1.384(2) . ? C7 C12 1.398(2) . ? C7 C8 1.406(2) . ? C8 C9 1.405(2) . ? C9 C10 1.374(3) . ? C10 C11 1.384(3) . ? C11 C12 1.382(2) . ? C13 C18 1.389(2) . ? C13 C14 1.397(2) . ? C14 C15 1.387(2) . ? C15 C16 1.388(3) . ? C16 C17 1.379(3) . ? C17 C18 1.390(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C19 Ga1 S2 116.57(7) . . ? C19 Ga1 S1 118.02(7) . . ? S2 Ga1 S1 111.83(2) . . ? C19 Ga1 P1 125.16(7) . . ? S2 Ga1 P1 90.611(16) . . ? S1 Ga1 P1 89.327(15) . . ? C2 S1 Ga1 102.85(5) . . ? C8 S2 Ga1 101.65(5) . . ? C1 P1 C7 107.31(7) . . ? C1 P1 C13 109.59(7) . . ? C7 P1 C13 108.67(7) . . ? C1 P1 Ga1 103.28(5) . . ? C7 P1 Ga1 101.54(5) . . ? C13 P1 Ga1 125.14(5) . . ? C6 C1 C2 120.48(14) . . ? C6 C1 P1 121.67(12) . . ? C2 C1 P1 117.77(11) . . ? C3 C2 C1 118.07(15) . . ? C3 C2 S1 116.82(13) . . ? C1 C2 S1 125.11(12) . . ? C4 C3 C2 120.83(16) . . ? C3 C4 C5 120.81(16) . . ? C6 C5 C4 119.15(16) . . ? C5 C6 C1 120.64(16) . . ? C12 C7 C8 120.16(14) . . ? C12 C7 P1 120.55(12) . . ? C8 C7 P1 119.28(12) . . ? C9 C8 C7 117.94(16) . . ? C9 C8 S2 117.37(13) . . ? C7 C8 S2 124.65(12) . . ? C10 C9 C8 120.98(17) . . ? C9 C10 C11 120.95(16) . . ? C12 C11 C10 119.32(17) . . ? C11 C12 C7 120.64(16) . . ? C18 C13 C14 119.97(14) . . ? C18 C13 P1 120.42(12) . . ? C14 C13 P1 119.22(12) . . ? C15 C14 C13 119.81(16) . . ? C14 C15 C16 119.95(17) . . ? C17 C16 C15 120.31(16) . . ? C16 C17 C18 120.23(17) . . ? C13 C18 C17 119.72(16) . . ? #============================================================================ data_x0057fin _database_code_depnum_ccdc_archive 'CCDC 722488' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H22 Ga P S2' _chemical_formula_weight 451.21 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ga Ga 0.2307 1.6083 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.064(2) _cell_length_b 12.605(3) _cell_length_c 15.919(3) _cell_angle_alpha 93.733(17) _cell_angle_beta 102.653(16) _cell_angle_gamma 99.969(17) _cell_volume 2121.1(7) _cell_formula_units_Z 4 _cell_measurement_temperature 130(2) _cell_measurement_reflns_used 13965 _cell_measurement_theta_min 2.5675 _cell_measurement_theta_max 31.9798 _exptl_crystal_description plates _exptl_crystal_colour colorless _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.413 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 928 _exptl_absorpt_coefficient_mu 1.573 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET) (compiled Oct 18 2006,16:28:17) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_correction_T_min 0.88482 _exptl_absorpt_correction_T_max 1 _exptl_special_details ; ? ; _diffrn_ambient_temperature 130(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'ccd xcalibur s' _diffrn_measurement_method '\w scans and \f scans' _diffrn_detector_area_resol_mean 16.356 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 38133 _diffrn_reflns_av_R_equivalents 0.0378 _diffrn_reflns_av_sigmaI/netI 0.0582 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.57 _diffrn_reflns_theta_max 28.28 _reflns_number_total 10517 _reflns_number_gt 6962 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET) (compiled Oct 18 2006,16:28:17) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET) (compiled Oct 18 2006,16:28:17) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET) (compiled Oct 18 2006,16:28:17) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP3 for Windows (L. J. Farrugia, 1997)' _computing_publication_material 'WINGX (L.J. Farrugia,1999)' _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^)+(0.0283P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10517 _refine_ls_number_parameters 475 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0504 _refine_ls_R_factor_gt 0.0280 _refine_ls_wR_factor_ref 0.0618 _refine_ls_wR_factor_gt 0.0565 _refine_ls_goodness_of_fit_ref 0.919 _refine_ls_restrained_S_all 0.919 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C2 C 0.3525(2) 0.41897(19) 0.11594(15) 0.0444(6) Uani 1 1 d . . . H2A H 0.4334 0.4297 0.1586 0.067 Uiso 1 1 calc R . . H2B H 0.3663 0.4453 0.0616 0.067 Uiso 1 1 calc R . . H2C H 0.3145 0.3416 0.1055 0.067 Uiso 1 1 calc R . . C3 C 0.1327(2) 0.4572(2) 0.08823(18) 0.0533(7) Uani 1 1 d . . . H3A H 0.1394 0.4799 0.0314 0.080 Uiso 1 1 calc R . . H3B H 0.0766 0.4971 0.1116 0.080 Uiso 1 1 calc R . . H3C H 0.0982 0.3793 0.0821 0.080 Uiso 1 1 calc R . . C4 C 0.2538(3) 0.4494(2) 0.23991(15) 0.0476(7) Uani 1 1 d . . . H4A H 0.2169 0.3722 0.2353 0.071 Uiso 1 1 calc R . . H4B H 0.1998 0.4921 0.2628 0.071 Uiso 1 1 calc R . . H4C H 0.3380 0.4637 0.2790 0.071 Uiso 1 1 calc R . . C1 C 0.2644(2) 0.48125(17) 0.15028(13) 0.0300(5) Uani 1 1 d . . . C5 C 0.29887(18) 0.84581(16) 0.27305(12) 0.0228(4) Uani 1 1 d . . . C6 C 0.42647(18) 0.84479(15) 0.30895(12) 0.0211(4) Uani 1 1 d . . . C7 C 0.49975(19) 0.93100(16) 0.36848(13) 0.0261(5) Uani 1 1 d . . . H7 H 0.5863 0.9304 0.3920 0.031 Uiso 1 1 calc R . . C8 C 0.4488(2) 1.01669(17) 0.39365(13) 0.0298(5) Uani 1 1 d . . . H8 H 0.4997 1.0752 0.4335 0.036 Uiso 1 1 calc R . . C9 C 0.3216(2) 1.01597(18) 0.35962(14) 0.0319(5) Uani 1 1 d . . . H9 H 0.2851 1.0741 0.3772 0.038 Uiso 1 1 calc R . . C10 C 0.2482(2) 0.93273(17) 0.30112(13) 0.0277(5) Uani 1 1 d . . . H10 H 0.1614 0.9338 0.2791 0.033 Uiso 1 1 calc R . . C11 C 0.57094(17) 0.67934(15) 0.37191(11) 0.0189(4) Uani 1 1 d . . . C12 C 0.65642(19) 0.61235(17) 0.36476(13) 0.0270(5) Uani 1 1 d . . . H12 H 0.6776 0.5988 0.3109 0.032 Uiso 1 1 calc R . . C13 C 0.7107(2) 0.56533(18) 0.43642(14) 0.0344(5) Uani 1 1 d . . . H13 H 0.7693 0.5197 0.4314 0.041 Uiso 1 1 calc R . . C14 C 0.6805(2) 0.58434(19) 0.51457(14) 0.0368(6) Uani 1 1 d . . . H14 H 0.7183 0.5522 0.5635 0.044 Uiso 1 1 calc R . . C15 C 0.5947(2) 0.6505(2) 0.52190(14) 0.0388(6) Uani 1 1 d . . . H15 H 0.5734 0.6633 0.5758 0.047 Uiso 1 1 calc R . . C16 C 0.5398(2) 0.69782(18) 0.45092(13) 0.0305(5) Uani 1 1 d . . . H16 H 0.4809 0.7430 0.4562 0.037 Uiso 1 1 calc R . . C17 C 0.58938(18) 0.77827(15) 0.13140(12) 0.0198(4) Uani 1 1 d . . . C18 C 0.61809(17) 0.79019(15) 0.22263(12) 0.0177(4) Uani 1 1 d . . . C19 C 0.73577(18) 0.84717(15) 0.26934(12) 0.0210(4) Uani 1 1 d . . . H19 H 0.7551 0.8530 0.3308 0.025 Uiso 1 1 calc R . . C20 C 0.82466(18) 0.89526(16) 0.22763(13) 0.0235(4) Uani 1 1 d . . . H20 H 0.9036 0.9357 0.2600 0.028 Uiso 1 1 calc R . . C21 C 0.79731(19) 0.88384(16) 0.13795(13) 0.0246(5) Uani 1 1 d . . . H21 H 0.8583 0.9159 0.1088 0.030 Uiso 1 1 calc R . . C22 C 0.68147(19) 0.82591(16) 0.09027(13) 0.0240(4) Uani 1 1 d . . . H22 H 0.6645 0.8185 0.0288 0.029 Uiso 1 1 calc R . . C23 C 0.88465(19) 0.20161(16) 0.47736(12) 0.0237(4) Uani 1 1 d . . . C24 C 0.8218(2) 0.08342(18) 0.44810(15) 0.0467(7) Uani 1 1 d . . . H24A H 0.8822 0.0445 0.4291 0.070 Uiso 1 1 calc R . . H24B H 0.7483 0.0799 0.4000 0.070 Uiso 1 1 calc R . . H24C H 0.7946 0.0500 0.4964 0.070 Uiso 1 1 calc R . . C25 C 1.0009(2) 0.2069(2) 0.55131(13) 0.0389(6) Uani 1 1 d . . . H25A H 0.9747 0.1762 0.6010 0.058 Uiso 1 1 calc R . . H25B H 1.0437 0.2826 0.5683 0.058 Uiso 1 1 calc R . . H25C H 1.0588 0.1653 0.5320 0.058 Uiso 1 1 calc R . . C26 C 0.7923(2) 0.2636(2) 0.50734(15) 0.0415(6) Uani 1 1 d . . . H26A H 0.7687 0.2333 0.5579 0.062 Uiso 1 1 calc R . . H26B H 0.7166 0.2574 0.4605 0.062 Uiso 1 1 calc R . . H26C H 0.8322 0.3402 0.5229 0.062 Uiso 1 1 calc R . . C27 C 0.90024(17) 0.47127(15) 0.27802(12) 0.0189(4) Uani 1 1 d . . . C28 C 0.80474(17) 0.39356(15) 0.22182(11) 0.0175(4) Uani 1 1 d . . . C29 C 0.72338(19) 0.42524(16) 0.15178(12) 0.0239(5) Uani 1 1 d . . . H29 H 0.6571 0.3729 0.1156 0.029 Uiso 1 1 calc R . . C30 C 0.7390(2) 0.53233(17) 0.13500(13) 0.0294(5) Uani 1 1 d . . . H30 H 0.6820 0.5542 0.0885 0.035 Uiso 1 1 calc R . . C31 C 0.8382(2) 0.60754(17) 0.18640(13) 0.0291(5) Uani 1 1 d . . . H31 H 0.8517 0.6804 0.1730 0.035 Uiso 1 1 calc R . . C32 C 0.91772(19) 0.57790(16) 0.25683(13) 0.0239(4) Uani 1 1 d . . . H32 H 0.9852 0.6307 0.2913 0.029 Uiso 1 1 calc R . . C33 C 0.63865(17) 0.18152(15) 0.20173(12) 0.0192(4) Uani 1 1 d . . . C34 C 0.54466(18) 0.22236(17) 0.23090(13) 0.0261(5) Uani 1 1 d . . . H34 H 0.5654 0.2884 0.2679 0.031 Uiso 1 1 calc R . . C35 C 0.42025(19) 0.16686(17) 0.20611(14) 0.0309(5) Uani 1 1 d . . . H35 H 0.3560 0.1950 0.2260 0.037 Uiso 1 1 calc R . . C36 C 0.39013(19) 0.07072(17) 0.15249(13) 0.0271(5) Uani 1 1 d . . . H36 H 0.3051 0.0329 0.1354 0.033 Uiso 1 1 calc R . . C37 C 0.48329(19) 0.02958(16) 0.12367(13) 0.0278(5) Uani 1 1 d . . . H37 H 0.4622 -0.0367 0.0870 0.033 Uiso 1 1 calc R . . C38 C 0.60749(18) 0.08447(16) 0.14784(13) 0.0253(5) Uani 1 1 d . . . H38 H 0.6713 0.0559 0.1277 0.030 Uiso 1 1 calc R . . C40 C 1.00274(17) 0.16545(14) 0.20788(12) 0.0189(4) Uani 1 1 d . . . C41 C 0.89213(17) 0.20172(14) 0.16958(12) 0.0177(4) Uani 1 1 d . . . C42 C 0.85561(19) 0.19830(15) 0.07906(12) 0.0237(5) Uani 1 1 d . . . H42 H 0.7811 0.2231 0.0534 0.028 Uiso 1 1 calc R . . C43 C 0.9258(2) 0.15960(16) 0.02683(13) 0.0293(5) Uani 1 1 d . . . H43 H 0.9004 0.1579 -0.0343 0.035 Uiso 1 1 calc R . . C44 C 1.03514(19) 0.12276(16) 0.06487(13) 0.0281(5) Uani 1 1 d . . . H44 H 1.0842 0.0958 0.0294 0.034 Uiso 1 1 calc R . . C45 C 1.07196(18) 0.12542(16) 0.15355(13) 0.0239(5) Uani 1 1 d . . . H45 H 1.1460 0.0995 0.1784 0.029 Uiso 1 1 calc R . . P1 P 0.49647(5) 0.73455(4) 0.27609(3) 0.01812(11) Uani 1 1 d . . . P2 P 0.80036(5) 0.25332(4) 0.23799(3) 0.01714(11) Uani 1 1 d . . . S1 S 0.19579(5) 0.74389(5) 0.19594(4) 0.03221(13) Uani 1 1 d . . . S2 S 0.44349(5) 0.70917(4) 0.06441(3) 0.02879(13) Uani 1 1 d . . . S3 S 0.99833(5) 0.44517(4) 0.37524(3) 0.02481(12) Uani 1 1 d . . . S4 S 1.06362(5) 0.16612(4) 0.32046(3) 0.02547(12) Uani 1 1 d . . . Ga1 Ga 0.33202(2) 0.639092(18) 0.161913(14) 0.02383(6) Uani 1 1 d . . . Ga2 Ga 0.93721(2) 0.262868(17) 0.376478(13) 0.01920(6) 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 C2 0.0582(17) 0.0359(14) 0.0419(14) 0.0068(12) 0.0143(13) 0.0124(13) C3 0.0387(15) 0.0362(15) 0.0686(18) -0.0039(13) -0.0088(13) -0.0068(12) C4 0.0608(18) 0.0395(15) 0.0463(15) 0.0141(12) 0.0244(13) 0.0018(13) C1 0.0281(12) 0.0308(12) 0.0264(11) 0.0001(9) 0.0026(9) -0.0008(10) C5 0.0220(11) 0.0279(11) 0.0219(10) 0.0116(9) 0.0088(8) 0.0063(9) C6 0.0214(11) 0.0252(11) 0.0195(10) 0.0078(8) 0.0071(8) 0.0068(9) C7 0.0242(11) 0.0286(12) 0.0275(11) 0.0058(9) 0.0058(9) 0.0095(9) C8 0.0351(13) 0.0257(12) 0.0310(12) 0.0027(9) 0.0102(10) 0.0096(10) C9 0.0402(14) 0.0314(13) 0.0349(12) 0.0127(10) 0.0190(11) 0.0201(11) C10 0.0231(11) 0.0364(13) 0.0323(12) 0.0172(10) 0.0131(9) 0.0159(10) C11 0.0153(10) 0.0241(11) 0.0162(9) 0.0049(8) 0.0017(8) 0.0024(8) C12 0.0262(12) 0.0369(13) 0.0235(11) 0.0098(9) 0.0106(9) 0.0127(10) C13 0.0267(12) 0.0426(14) 0.0425(14) 0.0206(11) 0.0121(10) 0.0186(10) C14 0.0295(13) 0.0536(16) 0.0297(12) 0.0240(11) 0.0034(10) 0.0120(11) C15 0.0456(15) 0.0559(16) 0.0216(11) 0.0152(11) 0.0113(10) 0.0198(12) C16 0.0317(13) 0.0390(13) 0.0257(11) 0.0084(10) 0.0087(9) 0.0159(10) C17 0.0220(11) 0.0178(10) 0.0197(10) 0.0027(8) 0.0038(8) 0.0056(8) C18 0.0192(10) 0.0164(10) 0.0194(10) 0.0036(8) 0.0059(8) 0.0056(8) C19 0.0218(11) 0.0221(11) 0.0183(10) 0.0012(8) 0.0020(8) 0.0059(8) C20 0.0189(11) 0.0229(11) 0.0284(11) 0.0023(9) 0.0063(9) 0.0024(8) C21 0.0254(11) 0.0231(11) 0.0292(11) 0.0068(9) 0.0132(9) 0.0048(9) C22 0.0324(12) 0.0238(11) 0.0190(10) 0.0051(8) 0.0091(9) 0.0088(9) C23 0.0286(12) 0.0226(11) 0.0175(10) 0.0038(8) 0.0033(8) 0.0009(9) C24 0.0643(18) 0.0342(14) 0.0354(14) 0.0037(11) 0.0169(12) -0.0137(12) C25 0.0423(14) 0.0499(15) 0.0220(11) 0.0103(11) -0.0004(10) 0.0095(12) C26 0.0426(15) 0.0513(16) 0.0397(14) 0.0144(12) 0.0226(12) 0.0135(12) C27 0.0187(10) 0.0220(11) 0.0174(9) 0.0008(8) 0.0063(8) 0.0061(8) C28 0.0190(10) 0.0195(10) 0.0159(9) 0.0027(8) 0.0055(8) 0.0068(8) C29 0.0272(12) 0.0266(12) 0.0184(10) -0.0005(9) 0.0026(9) 0.0107(9) C30 0.0409(14) 0.0310(12) 0.0202(11) 0.0069(9) 0.0051(10) 0.0188(10) C31 0.0452(14) 0.0205(11) 0.0281(11) 0.0086(9) 0.0161(10) 0.0125(10) C32 0.0274(11) 0.0189(11) 0.0261(11) -0.0002(9) 0.0096(9) 0.0030(9) C33 0.0152(10) 0.0208(10) 0.0209(10) 0.0040(8) 0.0015(8) 0.0045(8) C34 0.0223(11) 0.0259(11) 0.0294(11) -0.0029(9) 0.0075(9) 0.0031(9) C35 0.0187(11) 0.0357(13) 0.0402(13) 0.0015(10) 0.0107(10) 0.0067(9) C36 0.0146(10) 0.0298(12) 0.0346(12) 0.0062(10) 0.0031(9) 0.0006(9) C37 0.0234(11) 0.0215(11) 0.0344(12) -0.0013(9) 0.0013(9) 0.0017(9) C38 0.0208(11) 0.0197(11) 0.0354(12) -0.0008(9) 0.0052(9) 0.0070(9) C40 0.0169(10) 0.0148(10) 0.0234(10) 0.0019(8) 0.0038(8) -0.0002(8) C41 0.0170(10) 0.0151(10) 0.0193(10) -0.0011(8) 0.0030(8) 0.0014(8) C42 0.0227(11) 0.0223(11) 0.0239(11) 0.0032(9) 0.0016(9) 0.0031(9) C43 0.0381(13) 0.0273(12) 0.0213(11) -0.0018(9) 0.0079(10) 0.0037(10) C44 0.0291(12) 0.0267(12) 0.0312(12) -0.0024(9) 0.0166(10) 0.0027(9) C45 0.0160(10) 0.0241(11) 0.0316(12) 0.0000(9) 0.0071(9) 0.0029(8) P1 0.0163(3) 0.0213(3) 0.0167(2) 0.0038(2) 0.0026(2) 0.0043(2) P2 0.0155(3) 0.0178(3) 0.0178(2) 0.0012(2) 0.0020(2) 0.0050(2) S1 0.0179(3) 0.0389(3) 0.0368(3) 0.0048(3) 0.0001(2) 0.0052(2) S2 0.0283(3) 0.0359(3) 0.0169(3) 0.0038(2) 0.0001(2) -0.0021(2) S3 0.0231(3) 0.0220(3) 0.0241(3) 0.0009(2) -0.0028(2) 0.0015(2) S4 0.0215(3) 0.0325(3) 0.0228(3) 0.0008(2) 0.0001(2) 0.0136(2) Ga1 0.02128(13) 0.02481(13) 0.02148(12) 0.00449(9) -0.00018(9) -0.00029(9) Ga2 0.01868(12) 0.02178(12) 0.01701(11) 0.00298(9) 0.00275(9) 0.00504(9) _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 C2 C1 1.519(3) . ? C3 C1 1.539(3) . ? C4 C1 1.530(3) . ? C1 Ga1 1.982(2) . ? C5 C6 1.405(3) . ? C5 C10 1.404(3) . ? C5 S1 1.770(2) . ? C6 C7 1.400(3) . ? C6 P1 1.805(2) . ? C7 C8 1.377(3) . ? C8 C9 1.392(3) . ? C9 C10 1.369(3) . ? C11 C16 1.391(3) . ? C11 C12 1.390(3) . ? C11 P1 1.8100(18) . ? C12 C13 1.387(3) . ? C13 C14 1.374(3) . ? C14 C15 1.385(3) . ? C15 C16 1.384(3) . ? C17 C22 1.400(3) . ? C17 C18 1.409(2) . ? C17 S2 1.7718(19) . ? C18 C19 1.395(3) . ? C18 P1 1.8110(19) . ? C19 C20 1.381(3) . ? C20 C21 1.385(3) . ? C21 C22 1.389(3) . ? C23 C26 1.525(3) . ? C23 C24 1.526(3) . ? C23 C25 1.530(3) . ? C23 Ga2 1.9821(19) . ? C27 C32 1.398(3) . ? C27 C28 1.411(3) . ? C27 S3 1.7707(19) . ? C28 C29 1.398(2) . ? C28 P2 1.7969(19) . ? C29 C30 1.382(3) . ? C30 C31 1.385(3) . ? C31 C32 1.381(3) . ? C33 C34 1.388(3) . ? C33 C38 1.393(3) . ? C33 P2 1.8088(19) . ? C34 C35 1.390(3) . ? C35 C36 1.382(3) . ? C36 C37 1.379(3) . ? C37 C38 1.385(3) . ? C40 C45 1.399(3) . ? C40 C41 1.408(3) . ? C40 S4 1.7700(19) . ? C41 C42 1.405(3) . ? C41 P2 1.806(2) . ? C42 C43 1.376(3) . ? C43 C44 1.398(3) . ? C44 C45 1.377(3) . ? P1 Ga1 2.3602(8) . ? P2 Ga2 2.3680(7) . ? S1 Ga1 2.2943(7) . ? S2 Ga1 2.3132(7) . ? S3 Ga2 2.2828(8) . ? S4 Ga2 2.2876(7) . ? 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 C4 109.79(19) . . ? C2 C1 C3 110.37(19) . . ? C4 C1 C3 109.7(2) . . ? C2 C1 Ga1 110.16(15) . . ? C4 C1 Ga1 108.01(14) . . ? C3 C1 Ga1 108.79(15) . . ? C6 C5 C10 118.04(18) . . ? C6 C5 S1 124.67(16) . . ? C10 C5 S1 117.28(15) . . ? C7 C6 C5 119.68(18) . . ? C7 C6 P1 120.25(15) . . ? C5 C6 P1 120.04(15) . . ? C8 C7 C6 121.30(19) . . ? C7 C8 C9 118.8(2) . . ? C10 C9 C8 120.9(2) . . ? C9 C10 C5 121.21(19) . . ? C16 C11 C12 119.51(18) . . ? C16 C11 P1 121.63(15) . . ? C12 C11 P1 118.77(15) . . ? C13 C12 C11 119.89(19) . . ? C14 C13 C12 120.5(2) . . ? C13 C14 C15 119.87(19) . . ? C14 C15 C16 120.2(2) . . ? C15 C16 C11 120.0(2) . . ? C22 C17 C18 117.98(17) . . ? C22 C17 S2 117.28(14) . . ? C18 C17 S2 124.72(15) . . ? C19 C18 C17 120.14(18) . . ? C19 C18 P1 121.67(14) . . ? C17 C18 P1 118.14(14) . . ? C20 C19 C18 121.05(18) . . ? C19 C20 C21 119.18(18) . . ? C20 C21 C22 120.63(19) . . ? C21 C22 C17 120.99(18) . . ? C26 C23 C24 110.32(19) . . ? C26 C23 C25 109.94(17) . . ? C24 C23 C25 109.39(19) . . ? C26 C23 Ga2 110.57(14) . . ? C24 C23 Ga2 106.93(14) . . ? C25 C23 Ga2 109.64(14) . . ? C32 C27 C28 117.92(16) . . ? C32 C27 S3 117.00(14) . . ? C28 C27 S3 125.06(14) . . ? C29 C28 C27 120.32(17) . . ? C29 C28 P2 121.62(14) . . ? C27 C28 P2 117.86(13) . . ? C30 C29 C28 120.28(18) . . ? C29 C30 C31 119.52(18) . . ? C32 C31 C30 120.80(19) . . ? C31 C32 C27 120.89(18) . . ? C34 C33 C38 119.55(18) . . ? C34 C33 P2 119.08(15) . . ? C38 C33 P2 121.33(15) . . ? C33 C34 C35 120.14(19) . . ? C36 C35 C34 119.9(2) . . ? C37 C36 C35 120.14(19) . . ? C36 C37 C38 120.35(19) . . ? C37 C38 C33 119.89(19) . . ? C45 C40 C41 118.25(17) . . ? C45 C40 S4 116.24(14) . . ? C41 C40 S4 125.51(15) . . ? C40 C41 C42 119.62(18) . . ? C40 C41 P2 119.29(14) . . ? C42 C41 P2 121.08(15) . . ? C43 C42 C41 121.16(19) . . ? C42 C43 C44 119.19(19) . . ? C45 C44 C43 120.27(19) . . ? C44 C45 C40 121.49(19) . . ? C6 P1 C18 107.59(9) . . ? C6 P1 C11 108.72(9) . . ? C18 P1 C11 108.13(9) . . ? C6 P1 Ga1 101.26(6) . . ? C18 P1 Ga1 103.96(6) . . ? C11 P1 Ga1 125.97(7) . . ? C28 P2 C41 106.88(9) . . ? C28 P2 C33 108.41(9) . . ? C41 P2 C33 108.36(9) . . ? C28 P2 Ga2 102.70(6) . . ? C41 P2 Ga2 101.05(6) . . ? C33 P2 Ga2 127.81(6) . . ? C5 S1 Ga1 101.89(7) . . ? C17 S2 Ga1 103.53(7) . . ? C27 S3 Ga2 102.90(7) . . ? C40 S4 Ga2 101.41(7) . . ? C1 Ga1 S1 113.79(7) . . ? C1 Ga1 S2 119.37(7) . . ? S1 Ga1 S2 113.79(3) . . ? C1 Ga1 P1 125.07(6) . . ? S1 Ga1 P1 90.90(3) . . ? S2 Ga1 P1 89.01(3) . . ? C23 Ga2 S3 121.42(6) . . ? C23 Ga2 S4 112.88(6) . . ? S3 Ga2 S4 112.31(3) . . ? C23 Ga2 P2 124.05(6) . . ? S3 Ga2 P2 89.90(3) . . ? S4 Ga2 P2 91.03(2) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.590 _refine_diff_density_min -0.307 _refine_diff_density_rms 0.063 #============================================================================ data_x0138fin _database_code_depnum_ccdc_archive 'CCDC 722489' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44.75 H36 Ga2 P2 S4' _chemical_formula_weight 903.36 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Ga Ga 0.2307 1.6083 '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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.4389(14) _cell_length_b 13.867(3) _cell_length_c 24.7218(11) _cell_angle_alpha 83.400(9) _cell_angle_beta 83.011(6) _cell_angle_gamma 73.175(14) _cell_volume 4037.1(9) _cell_formula_units_Z 4 _cell_measurement_temperature 130(2) _cell_measurement_reflns_used 39161 _cell_measurement_theta_min 2.7204 _cell_measurement_theta_max 32.2263 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.3 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.486 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1842 _exptl_absorpt_coefficient_mu 1.653 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET) (compiled Oct 18 2006,16:28:17) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_correction_T_min 0.90134 _exptl_absorpt_correction_T_max 1 _exptl_special_details ; ? ; _diffrn_ambient_temperature 130(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'ccd xcalibur s' _diffrn_measurement_method '\w scans and \f scans' _diffrn_detector_area_resol_mean 16.356 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 104559 _diffrn_reflns_av_R_equivalents 0.0437 _diffrn_reflns_av_sigmaI/netI 0.0584 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 2.73 _diffrn_reflns_theta_max 28.28 _reflns_number_total 19952 _reflns_number_gt 14120 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET) (compiled Oct 18 2006,16:28:17) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET) (compiled Oct 18 2006,16:28:17) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET) (compiled Oct 18 2006,16:28:17) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP3 for Windows (L. J. Farrugia, 1997)' _computing_publication_material 'WINGX (L.J. Farrugia,1999)' _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^)+(0.0271P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 19952 _refine_ls_number_parameters 970 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0554 _refine_ls_R_factor_gt 0.0293 _refine_ls_wR_factor_ref 0.0627 _refine_ls_wR_factor_gt 0.0549 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.027 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ga1 Ga 0.812085(17) 0.507760(17) 0.736046(9) 0.01785(5) Uani 1 1 d . . . Ga2 Ga 0.834248(17) 0.399379(18) 0.818471(9) 0.01856(5) Uani 1 1 d . . . S1 S 0.88299(4) 0.45448(5) 0.65014(2) 0.02750(13) Uani 1 1 d . . . S2 S 0.79504(5) 0.67658(4) 0.73663(3) 0.03167(14) Uani 1 1 d . . . S3 S 0.96668(4) 0.24409(4) 0.83444(2) 0.02292(12) Uani 1 1 d . . . S4 S 0.66713(4) 0.41887(5) 0.87334(2) 0.02717(13) Uani 1 1 d . . . P1 P 0.62873(4) 0.54694(4) 0.70589(2) 0.01747(11) Uani 1 1 d . . . P2 P 0.91076(4) 0.44774(4) 0.89167(2) 0.01759(11) Uani 1 1 d . . . C1 C 0.76274(17) 0.45750(15) 0.61801(8) 0.0205(5) Uani 1 1 d . . . C2 C 0.65121(16) 0.49432(15) 0.64071(8) 0.0189(4) Uani 1 1 d . . . C3 C 0.56172(19) 0.49390(17) 0.61232(9) 0.0287(5) Uani 1 1 d . . . H3 H 0.4865 0.5191 0.6281 0.034 Uiso 1 1 calc R . . C4 C 0.5808(2) 0.45720(18) 0.56127(9) 0.0320(6) Uani 1 1 d . . . H4 H 0.5194 0.4574 0.5419 0.038 Uiso 1 1 calc R . . C5 C 0.6909(2) 0.42010(17) 0.53885(9) 0.0337(6) Uani 1 1 d . . . H5 H 0.7046 0.3943 0.5039 0.040 Uiso 1 1 calc R . . C6 C 0.7805(2) 0.41993(16) 0.56626(8) 0.0275(5) Uani 1 1 d . . . H6 H 0.8553 0.3942 0.5501 0.033 Uiso 1 1 calc R . . C7 C 0.67179(17) 0.73311(16) 0.70238(8) 0.0235(5) Uani 1 1 d . . . C8 C 0.59608(16) 0.68193(16) 0.69119(8) 0.0213(5) Uani 1 1 d . . . C9 C 0.49870(18) 0.73505(18) 0.66573(9) 0.0296(5) Uani 1 1 d . . . H9 H 0.4471 0.7002 0.6588 0.036 Uiso 1 1 calc R . . C10 C 0.4771(2) 0.83674(18) 0.65077(10) 0.0369(6) Uani 1 1 d . . . H10 H 0.4110 0.8721 0.6335 0.044 Uiso 1 1 calc R . . C11 C 0.5521(2) 0.88723(18) 0.66099(10) 0.0380(6) Uani 1 1 d . . . H11 H 0.5377 0.9575 0.6503 0.046 Uiso 1 1 calc R . . C12 C 0.6479(2) 0.83704(17) 0.68663(9) 0.0325(6) Uani 1 1 d . . . H12 H 0.6981 0.8733 0.6937 0.039 Uiso 1 1 calc R . . C13 C 0.50646(15) 0.51852(16) 0.74358(8) 0.0188(4) Uani 1 1 d . . . C14 C 0.48331(17) 0.42746(17) 0.73995(9) 0.0242(5) Uani 1 1 d . . . H14 H 0.5298 0.3807 0.7157 0.029 Uiso 1 1 calc R . . C15 C 0.39258(18) 0.40458(18) 0.77155(9) 0.0292(5) Uani 1 1 d . . . H15 H 0.3765 0.3426 0.7687 0.035 Uiso 1 1 calc R . . C16 C 0.32551(18) 0.47220(19) 0.80730(9) 0.0311(6) Uani 1 1 d . . . H16 H 0.2630 0.4567 0.8288 0.037 Uiso 1 1 calc R . . C17 C 0.34907(18) 0.56143(19) 0.81185(9) 0.0317(6) Uani 1 1 d . . . H17 H 0.3030 0.6072 0.8367 0.038 Uiso 1 1 calc R . . C18 C 0.43961(17) 0.58553(17) 0.78048(8) 0.0250(5) Uani 1 1 d . . . H18 H 0.4560 0.6472 0.7841 0.030 Uiso 1 1 calc R . . C19 C 1.06863(16) 0.27133(16) 0.86959(8) 0.0193(4) Uani 1 1 d . . . C20 C 1.04890(16) 0.36104(16) 0.89514(8) 0.0187(4) Uani 1 1 d . . . C21 C 1.13424(16) 0.38010(17) 0.92003(8) 0.0225(5) Uani 1 1 d . . . H21 H 1.1201 0.4413 0.9369 0.027 Uiso 1 1 calc R . . C22 C 1.23991(17) 0.31036(18) 0.92041(9) 0.0279(5) Uani 1 1 d . . . H22 H 1.2985 0.3238 0.9369 0.034 Uiso 1 1 calc R . . C23 C 1.25854(17) 0.22107(18) 0.89639(9) 0.0291(5) Uani 1 1 d . . . H23 H 1.3304 0.1727 0.8969 0.035 Uiso 1 1 calc R . . C24 C 1.17448(17) 0.20104(17) 0.87169(8) 0.0260(5) Uani 1 1 d . . . H24 H 1.1888 0.1387 0.8559 0.031 Uiso 1 1 calc R . . C25 C 0.71385(16) 0.40691(17) 0.93897(8) 0.0226(5) Uani 1 1 d . . . C26 C 0.82024(16) 0.41456(15) 0.94900(8) 0.0193(4) Uani 1 1 d . . . C27 C 0.85286(17) 0.39653(17) 1.00204(8) 0.0255(5) Uani 1 1 d . . . H27 H 0.9263 0.3982 1.0081 0.031 Uiso 1 1 calc R . . C28 C 0.78077(19) 0.3765(2) 1.04572(9) 0.0371(6) Uani 1 1 d . . . H28 H 0.8040 0.3641 1.0817 0.045 Uiso 1 1 calc R . . C29 C 0.6733(2) 0.3745(2) 1.03661(10) 0.0425(7) Uani 1 1 d . . . H29 H 0.6219 0.3635 1.0668 0.051 Uiso 1 1 calc R . . C30 C 0.64040(18) 0.3885(2) 0.98426(9) 0.0354(6) Uani 1 1 d . . . H30 H 0.5672 0.3856 0.9788 0.042 Uiso 1 1 calc R . . C31 C 0.91989(16) 0.57344(16) 0.89773(8) 0.0192(4) Uani 1 1 d . . . C32 C 0.98993(17) 0.61311(17) 0.85872(9) 0.0254(5) Uani 1 1 d . . . H32 H 1.0355 0.5722 0.8316 0.030 Uiso 1 1 calc R . . C33 C 0.99343(19) 0.71150(18) 0.85936(9) 0.0295(5) Uani 1 1 d . . . H33 H 1.0413 0.7382 0.8327 0.035 Uiso 1 1 calc R . . C34 C 0.92722(19) 0.77143(18) 0.89884(9) 0.0298(5) Uani 1 1 d . . . H34 H 0.9302 0.8390 0.8994 0.036 Uiso 1 1 calc R . . C35 C 0.85733(19) 0.73321(17) 0.93709(9) 0.0308(5) Uani 1 1 d . . . H35 H 0.8115 0.7748 0.9639 0.037 Uiso 1 1 calc R . . C36 C 0.85293(17) 0.63439(16) 0.93695(9) 0.0247(5) Uani 1 1 d . . . H36 H 0.8043 0.6085 0.9636 0.030 Uiso 1 1 calc R . . Ga3 Ga 0.104040(17) 0.264313(17) 0.707052(9) 0.01821(5) Uani 1 1 d . . . Ga4 Ga -0.057923(17) 0.211637(17) 0.695004(9) 0.01784(5) Uani 1 1 d . . . S5 S 0.25136(4) 0.13309(4) 0.73514(2) 0.02676(13) Uani 1 1 d . . . S6 S 0.09434(4) 0.41110(4) 0.74645(2) 0.02390(12) Uani 1 1 d . . . S7 S -0.09054(5) 0.17154(4) 0.61215(2) 0.02669(13) Uani 1 1 d . . . S8 S -0.22981(4) 0.27201(4) 0.74495(2) 0.02067(11) Uani 1 1 d . . . P3 P 0.22894(4) 0.31665(4) 0.63568(2) 0.01808(11) Uani 1 1 d . . . P4 P -0.05671(4) 0.04537(4) 0.73289(2) 0.01836(11) Uani 1 1 d . . . C37 C 0.36906(16) 0.16861(16) 0.70114(8) 0.0216(5) Uani 1 1 d . . . C38 C 0.36428(16) 0.24498(16) 0.65818(8) 0.0205(5) Uani 1 1 d . . . C39 C 0.46361(17) 0.26842(18) 0.63591(9) 0.0273(5) Uani 1 1 d . . . H39 H 0.4597 0.3224 0.6081 0.033 Uiso 1 1 calc R . . C40 C 0.56711(18) 0.21474(19) 0.65347(10) 0.0329(6) Uani 1 1 d . . . H40 H 0.6339 0.2310 0.6378 0.039 Uiso 1 1 calc R . . C41 C 0.57196(18) 0.13734(19) 0.69404(10) 0.0330(6) Uani 1 1 d . . . H41 H 0.6430 0.0988 0.7056 0.040 Uiso 1 1 calc R . . C42 C 0.47518(17) 0.11483(17) 0.71817(9) 0.0277(5) Uani 1 1 d . . . H42 H 0.4805 0.0621 0.7467 0.033 Uiso 1 1 calc R . . C43 C 0.15363(15) 0.48427(15) 0.69452(8) 0.0188(4) Uani 1 1 d . . . C44 C 0.21292(16) 0.44691(16) 0.64589(8) 0.0192(4) Uani 1 1 d . . . C45 C 0.26043(18) 0.50874(17) 0.60802(9) 0.0270(5) Uani 1 1 d . . . H45 H 0.2987 0.4833 0.5747 0.032 Uiso 1 1 calc R . . C46 C 0.25272(19) 0.60639(17) 0.61812(9) 0.0300(5) Uani 1 1 d . . . H46 H 0.2876 0.6474 0.5926 0.036 Uiso 1 1 calc R . . C47 C 0.19340(19) 0.64398(18) 0.66594(9) 0.0316(5) Uani 1 1 d . . . H47 H 0.1871 0.7114 0.6730 0.038 Uiso 1 1 calc R . . C48 C 0.14351(18) 0.58473(16) 0.70338(9) 0.0270(5) Uani 1 1 d . . . H48 H 0.1018 0.6122 0.7356 0.032 Uiso 1 1 calc R . . C49 C 0.23069(17) 0.31328(16) 0.56232(8) 0.0213(5) Uani 1 1 d . . . C50 C 0.13020(19) 0.3592(2) 0.53950(9) 0.0338(6) Uani 1 1 d . . . H50 H 0.0648 0.3905 0.5621 0.041 Uiso 1 1 calc R . . C51 C 0.1245(2) 0.3598(2) 0.48408(10) 0.0400(6) Uani 1 1 d . . . H51 H 0.0554 0.3922 0.4687 0.048 Uiso 1 1 calc R . . C52 C 0.2178(2) 0.31396(19) 0.45106(9) 0.0369(6) Uani 1 1 d . . . H52 H 0.2133 0.3139 0.4130 0.044 Uiso 1 1 calc R . . C53 C 0.3173(2) 0.2684(2) 0.47318(10) 0.0426(7) Uani 1 1 d . . . H53 H 0.3820 0.2368 0.4503 0.051 Uiso 1 1 calc R . . C54 C 0.3248(2) 0.26789(19) 0.52916(9) 0.0354(6) Uani 1 1 d . . . H54 H 0.3944 0.2364 0.5443 0.042 Uiso 1 1 calc R . . C55 C -0.08173(16) 0.04099(16) 0.62368(9) 0.0225(5) Uani 1 1 d . . . C56 C -0.06715(16) -0.01699(16) 0.67466(8) 0.0210(5) Uani 1 1 d . . . C57 C -0.06270(18) -0.11929(17) 0.67805(9) 0.0269(5) Uani 1 1 d . . . H57 H -0.0534 -0.1581 0.7123 0.032 Uiso 1 1 calc R . . C58 C -0.07150(19) -0.16518(18) 0.63275(10) 0.0331(6) Uani 1 1 d . . . H58 H -0.0678 -0.2350 0.6357 0.040 Uiso 1 1 calc R . . C59 C -0.08585(19) -0.10811(18) 0.58296(10) 0.0329(6) Uani 1 1 d . . . H59 H -0.0926 -0.1390 0.5517 0.039 Uiso 1 1 calc R . . C60 C -0.09040(18) -0.00733(18) 0.57837(9) 0.0287(5) Uani 1 1 d . . . H60 H -0.0996 0.0303 0.5438 0.034 Uiso 1 1 calc R . . C61 C -0.25470(16) 0.16326(16) 0.78306(8) 0.0197(4) Uani 1 1 d . . . C62 C -0.18550(16) 0.06425(16) 0.77751(8) 0.0195(4) Uani 1 1 d . . . C63 C -0.21637(17) -0.01738(17) 0.80728(9) 0.0267(5) Uani 1 1 d . . . H63 H -0.1701 -0.0843 0.8030 0.032 Uiso 1 1 calc R . . C64 C -0.31324(18) -0.00160(19) 0.84277(9) 0.0316(6) Uani 1 1 d . . . H64 H -0.3340 -0.0572 0.8628 0.038 Uiso 1 1 calc R . . C65 C -0.37979(18) 0.09640(19) 0.84886(9) 0.0301(5) Uani 1 1 d . . . H65 H -0.4462 0.1076 0.8735 0.036 Uiso 1 1 calc R . . C66 C -0.35178(16) 0.17771(18) 0.81996(9) 0.0259(5) Uani 1 1 d . . . H66 H -0.3985 0.2442 0.8250 0.031 Uiso 1 1 calc R . . C67 C 0.05245(16) -0.03848(15) 0.77204(8) 0.0191(4) Uani 1 1 d . . . C68 C 0.14588(17) -0.10465(17) 0.74593(9) 0.0263(5) Uani 1 1 d . . . H68 H 0.1509 -0.1088 0.7076 0.032 Uiso 1 1 calc R . . C69 C 0.23128(18) -0.16424(18) 0.77619(10) 0.0314(6) Uani 1 1 d . . . H69 H 0.2947 -0.2099 0.7586 0.038 Uiso 1 1 calc R . . C70 C 0.22478(18) -0.15765(17) 0.83172(10) 0.0323(6) Uani 1 1 d . . . H70 H 0.2833 -0.1995 0.8523 0.039 Uiso 1 1 calc R . . C71 C 0.13421(18) -0.09092(17) 0.85767(9) 0.0278(5) Uani 1 1 d . . . H71 H 0.1307 -0.0860 0.8959 0.033 Uiso 1 1 calc R . . C72 C 0.04785(17) -0.03077(16) 0.82768(9) 0.0238(5) Uani 1 1 d . . . H72 H -0.0145 0.0158 0.8454 0.029 Uiso 1 1 calc R . . C101 C 0.5192(3) 0.1513(3) -0.00448(13) 0.0787(11) Uani 1 1 d . . . H10E H 0.4427 0.1658 -0.0156 0.118 Uiso 1 1 calc R . . H10F H 0.5640 0.0845 -0.0153 0.118 Uiso 1 1 calc R . . H10G H 0.5545 0.2028 -0.0224 0.118 Uiso 1 1 calc R . . C102 C 0.5136(2) 0.1524(2) 0.05658(12) 0.0471(7) Uani 1 1 d . . . C103 C 0.4449(2) 0.2335(2) 0.08342(16) 0.0623(9) Uani 1 1 d . . . H103 H 0.4017 0.2905 0.0628 0.075 Uiso 1 1 calc R . . C104 C 0.4379(2) 0.2333(3) 0.13970(17) 0.0689(10) Uani 1 1 d . . . H104 H 0.3901 0.2897 0.1574 0.083 Uiso 1 1 calc R . . C105 C 0.5003(3) 0.1509(3) 0.16999(14) 0.0616(9) Uani 1 1 d . . . H105 H 0.4952 0.1497 0.2087 0.074 Uiso 1 1 calc R . . C106 C 0.5701(2) 0.0705(2) 0.14364(12) 0.0470(7) Uani 1 1 d . . . H106 H 0.6146 0.0141 0.1642 0.056 Uiso 1 1 calc R . . C107 C 0.5758(2) 0.0714(2) 0.08770(11) 0.0402(6) Uani 1 1 d . . . H107 H 0.6237 0.0149 0.0701 0.048 Uiso 1 1 calc R . . C201 C 0.2323(2) 1.0539(2) 0.60109(11) 0.0515(8) Uani 1 1 d . . . H20E H 0.2995 1.0744 0.6058 0.077 Uiso 1 1 calc R . . H20F H 0.2051 1.0243 0.6361 0.077 Uiso 1 1 calc R . . H20G H 0.1732 1.1132 0.5885 0.077 Uiso 1 1 calc R . . C202 C 0.26147(19) 0.97768(18) 0.55982(10) 0.0336(6) Uani 1 1 d . . . C203 C 0.3428(2) 0.9797(2) 0.51576(11) 0.0407(6) Uani 1 1 d . . . H203 H 0.3800 1.0315 0.5116 0.049 Uiso 1 1 calc R . . C204 C 0.3700(2) 0.9090(2) 0.47855(11) 0.0460(7) Uani 1 1 d . . . H204 H 0.4260 0.9113 0.4491 0.055 Uiso 1 1 calc R . . C205 C 0.3156(2) 0.8342(2) 0.48392(11) 0.0454(7) Uani 1 1 d . . . H205 H 0.3343 0.7848 0.4581 0.054 Uiso 1 1 calc R . . C206 C 0.2337(2) 0.83126(19) 0.52695(10) 0.0369(6) Uani 1 1 d . . . H206 H 0.1958 0.7802 0.5304 0.044 Uiso 1 1 calc R . . C207 C 0.20721(19) 0.90205(18) 0.56477(10) 0.0331(6) Uani 1 1 d . . . H207 H 0.1516 0.8992 0.5944 0.040 Uiso 1 1 calc R . . C301 C 0.0679(3) 0.9522(2) 0.01578(14) 0.0430(16) Uani 0.50 1 d PG A -1 C302 C 0.0627(4) 1.0516(3) -0.00230(17) 0.050(3) Uani 0.50 1 d PG A -1 H302 H 0.1258 1.0764 -0.0008 0.060 Uiso 0.50 1 calc PR A -1 C303 C -0.0345(5) 1.1148(2) -0.02260(18) 0.069(3) Uani 0.50 1 d PG A -1 H303 H -0.0381 1.1830 -0.0350 0.083 Uiso 0.50 1 calc PR A -1 C304 C -0.1265(4) 1.0787(4) -0.0248(2) 0.075(3) Uani 0.50 1 d PG A -1 H304 H -0.1932 1.1221 -0.0387 0.090 Uiso 0.50 1 calc PR A -1 C305 C -0.1212(3) 0.9794(5) -0.0067(2) 0.073(3) Uani 0.50 1 d PG A -1 H305 H -0.1844 0.9546 -0.0082 0.087 Uiso 0.50 1 calc PR A -1 C306 C -0.0240(3) 0.9161(3) 0.01357(19) 0.051(3) Uani 0.50 1 d PG A -1 H306 H -0.0204 0.8479 0.0260 0.061 Uiso 0.50 1 calc PR A -1 C307 C 0.1742(3) 0.8831(4) 0.03796(19) 0.090(3) Uani 0.50 1 d PG A -1 H30A H 0.1541 0.8363 0.0676 0.135 Uiso 0.50 1 calc PR A -1 H30B H 0.2157 0.9236 0.0520 0.135 Uiso 0.50 1 calc PR A -1 H30C H 0.2216 0.8446 0.0086 0.135 Uiso 0.50 1 calc PR A -1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ga1 0.01775(10) 0.01825(12) 0.01656(12) -0.00024(9) -0.00134(8) -0.00405(9) Ga2 0.01813(10) 0.02156(12) 0.01528(12) -0.00104(10) -0.00127(9) -0.00474(9) S1 0.0191(2) 0.0379(3) 0.0179(3) -0.0012(2) 0.0014(2) 0.0023(2) S2 0.0306(3) 0.0211(3) 0.0466(4) 0.0003(3) -0.0115(3) -0.0102(2) S3 0.0275(3) 0.0188(3) 0.0229(3) -0.0023(2) -0.0074(2) -0.0050(2) S4 0.0183(2) 0.0453(4) 0.0195(3) -0.0057(3) -0.0007(2) -0.0105(2) P1 0.0165(2) 0.0183(3) 0.0165(3) -0.0015(2) -0.0007(2) -0.0034(2) P2 0.0167(2) 0.0198(3) 0.0161(3) -0.0024(2) -0.0006(2) -0.0049(2) C1 0.0285(11) 0.0152(11) 0.0158(11) 0.0009(8) -0.0012(8) -0.0039(9) C2 0.0250(10) 0.0163(11) 0.0155(11) -0.0010(8) -0.0018(8) -0.0060(8) C3 0.0319(12) 0.0298(13) 0.0264(13) 0.0042(10) -0.0041(10) -0.0135(10) C4 0.0517(15) 0.0354(14) 0.0169(12) 0.0041(10) -0.0127(11) -0.0233(12) C5 0.0634(17) 0.0248(13) 0.0155(12) -0.0005(10) -0.0049(11) -0.0163(12) C6 0.0428(13) 0.0198(12) 0.0150(12) -0.0014(9) 0.0020(10) -0.0032(10) C7 0.0277(11) 0.0202(11) 0.0191(12) -0.0001(9) 0.0013(9) -0.0030(9) C8 0.0207(10) 0.0194(11) 0.0189(11) -0.0005(9) 0.0026(8) -0.0002(8) C9 0.0298(11) 0.0284(13) 0.0259(13) 0.0001(10) -0.0034(9) -0.0011(10) C10 0.0386(13) 0.0264(14) 0.0364(15) 0.0013(11) -0.0082(11) 0.0061(11) C11 0.0532(16) 0.0184(12) 0.0333(15) -0.0002(11) -0.0036(12) 0.0033(11) C12 0.0427(13) 0.0186(12) 0.0354(14) -0.0029(10) -0.0009(11) -0.0083(10) C13 0.0157(9) 0.0241(11) 0.0149(11) 0.0015(9) -0.0040(8) -0.0030(8) C14 0.0214(10) 0.0259(12) 0.0249(12) -0.0026(10) -0.0042(9) -0.0052(9) C15 0.0282(11) 0.0296(13) 0.0316(14) 0.0022(10) -0.0031(10) -0.0128(10) C16 0.0239(11) 0.0406(15) 0.0257(13) 0.0062(11) 0.0023(9) -0.0094(10) C17 0.0271(11) 0.0380(15) 0.0250(13) -0.0057(11) 0.0096(9) -0.0053(10) C18 0.0246(10) 0.0275(12) 0.0231(12) -0.0062(10) 0.0013(9) -0.0074(9) C19 0.0222(10) 0.0239(11) 0.0119(11) 0.0032(9) -0.0031(8) -0.0077(9) C20 0.0188(9) 0.0225(11) 0.0139(11) 0.0007(9) -0.0002(8) -0.0058(8) C21 0.0232(10) 0.0273(12) 0.0175(11) -0.0045(9) 0.0005(8) -0.0078(9) C22 0.0217(10) 0.0389(14) 0.0233(12) -0.0011(11) -0.0056(9) -0.0078(10) C23 0.0200(10) 0.0334(14) 0.0276(13) 0.0040(11) -0.0047(9) 0.0010(10) C24 0.0283(11) 0.0229(12) 0.0225(12) -0.0006(10) -0.0029(9) -0.0005(9) C25 0.0221(10) 0.0280(12) 0.0165(11) -0.0032(9) 0.0002(8) -0.0052(9) C26 0.0221(10) 0.0199(11) 0.0162(11) -0.0027(9) 0.0007(8) -0.0067(8) C27 0.0230(10) 0.0329(13) 0.0215(12) -0.0025(10) -0.0019(9) -0.0091(10) C28 0.0360(13) 0.0615(18) 0.0162(12) 0.0010(12) -0.0032(10) -0.0186(13) C29 0.0376(13) 0.077(2) 0.0174(13) 0.0012(13) 0.0046(10) -0.0283(14) C30 0.0244(11) 0.0575(18) 0.0280(14) -0.0024(12) 0.0021(9) -0.0197(11) C31 0.0201(9) 0.0224(11) 0.0161(11) -0.0039(9) -0.0037(8) -0.0058(8) C32 0.0294(11) 0.0280(13) 0.0205(12) -0.0043(10) 0.0013(9) -0.0113(10) C33 0.0351(12) 0.0299(13) 0.0267(13) 0.0021(10) 0.0003(10) -0.0174(10) C34 0.0386(13) 0.0223(12) 0.0307(14) -0.0014(10) -0.0075(10) -0.0104(10) C35 0.0379(13) 0.0235(12) 0.0288(13) -0.0066(10) 0.0001(10) -0.0044(10) C36 0.0245(10) 0.0230(12) 0.0258(12) -0.0016(10) 0.0017(9) -0.0073(9) Ga3 0.01631(10) 0.01950(12) 0.01863(12) -0.00118(9) -0.00078(8) -0.00517(9) Ga4 0.01701(10) 0.01758(12) 0.01885(13) -0.00162(9) -0.00177(9) -0.00462(9) S5 0.0219(3) 0.0262(3) 0.0271(3) 0.0068(2) -0.0015(2) -0.0026(2) S6 0.0271(3) 0.0266(3) 0.0207(3) -0.0072(2) 0.0058(2) -0.0129(2) S7 0.0376(3) 0.0207(3) 0.0213(3) -0.0004(2) -0.0078(2) -0.0057(2) S8 0.0177(2) 0.0182(3) 0.0252(3) -0.0038(2) -0.0001(2) -0.0036(2) P3 0.0192(2) 0.0176(3) 0.0166(3) -0.0020(2) 0.0011(2) -0.0046(2) P4 0.0180(2) 0.0168(3) 0.0199(3) -0.0006(2) -0.0023(2) -0.0042(2) C37 0.0203(10) 0.0217(11) 0.0232(12) -0.0068(9) -0.0029(8) -0.0044(9) C38 0.0178(9) 0.0213(11) 0.0234(12) -0.0079(9) -0.0014(8) -0.0049(8) C39 0.0284(11) 0.0282(13) 0.0285(13) -0.0096(10) 0.0020(9) -0.0120(10) C40 0.0198(10) 0.0431(15) 0.0402(15) -0.0153(12) 0.0004(10) -0.0124(10) C41 0.0215(11) 0.0384(15) 0.0407(15) -0.0188(12) -0.0068(10) -0.0032(10) C42 0.0270(11) 0.0281(13) 0.0278(13) -0.0070(10) -0.0089(9) -0.0030(10) C43 0.0167(9) 0.0199(11) 0.0196(11) 0.0007(9) -0.0039(8) -0.0047(8) C44 0.0193(9) 0.0194(11) 0.0174(11) 0.0014(9) -0.0027(8) -0.0037(8) C45 0.0332(12) 0.0269(13) 0.0198(12) 0.0006(10) -0.0005(9) -0.0083(10) C46 0.0421(13) 0.0241(13) 0.0255(13) 0.0056(10) -0.0027(10) -0.0149(11) C47 0.0423(13) 0.0204(12) 0.0329(14) -0.0008(10) -0.0057(11) -0.0095(10) C48 0.0302(11) 0.0230(12) 0.0266(13) -0.0079(10) 0.0012(9) -0.0048(10) C49 0.0274(10) 0.0201(11) 0.0178(11) -0.0025(9) 0.0027(8) -0.0103(9) C50 0.0305(12) 0.0513(17) 0.0184(13) -0.0050(11) 0.0005(9) -0.0097(11) C51 0.0440(14) 0.0522(18) 0.0260(14) -0.0006(12) -0.0081(11) -0.0156(13) C52 0.0632(17) 0.0378(15) 0.0151(13) -0.0014(11) -0.0023(11) -0.0234(13) C53 0.0584(17) 0.0410(16) 0.0231(14) -0.0137(12) 0.0122(12) -0.0080(13) C54 0.0364(13) 0.0360(15) 0.0283(14) -0.0053(11) 0.0036(10) -0.0032(11) C55 0.0200(10) 0.0232(12) 0.0236(12) -0.0051(9) -0.0037(8) -0.0029(9) C56 0.0193(9) 0.0209(11) 0.0232(12) -0.0042(9) -0.0039(8) -0.0046(8) C57 0.0311(11) 0.0235(12) 0.0284(13) 0.0005(10) -0.0049(10) -0.0112(10) C58 0.0365(13) 0.0241(13) 0.0419(16) -0.0088(11) -0.0080(11) -0.0094(10) C59 0.0346(12) 0.0325(14) 0.0353(15) -0.0124(12) -0.0114(11) -0.0082(11) C60 0.0311(12) 0.0292(13) 0.0259(13) -0.0025(10) -0.0090(10) -0.0058(10) C61 0.0177(9) 0.0232(11) 0.0209(11) -0.0043(9) -0.0035(8) -0.0086(8) C62 0.0196(9) 0.0244(12) 0.0160(11) 0.0001(9) -0.0051(8) -0.0076(9) C63 0.0243(10) 0.0247(12) 0.0303(13) 0.0055(10) -0.0056(9) -0.0074(9) C64 0.0296(12) 0.0357(14) 0.0319(14) 0.0075(11) -0.0015(10) -0.0173(11) C65 0.0241(11) 0.0446(15) 0.0216(12) -0.0029(11) 0.0030(9) -0.0118(11) C66 0.0192(10) 0.0307(13) 0.0266(13) -0.0044(10) 0.0017(9) -0.0060(9) C67 0.0214(10) 0.0145(10) 0.0221(12) 0.0009(9) -0.0053(8) -0.0057(8) C68 0.0230(10) 0.0254(12) 0.0284(13) -0.0006(10) -0.0029(9) -0.0039(9) C69 0.0241(11) 0.0282(13) 0.0359(15) -0.0003(11) -0.0013(10) 0.0004(10) C70 0.0256(11) 0.0239(13) 0.0476(16) 0.0089(11) -0.0152(11) -0.0072(10) C71 0.0343(12) 0.0272(13) 0.0266(13) 0.0022(10) -0.0114(10) -0.0140(10) C72 0.0245(10) 0.0191(11) 0.0285(13) -0.0027(9) -0.0046(9) -0.0062(9) C101 0.084(3) 0.092(3) 0.062(2) 0.014(2) -0.0233(19) -0.028(2) C102 0.0384(14) 0.0501(18) 0.0561(19) -0.0045(15) -0.0075(13) -0.0165(13) C103 0.0324(15) 0.0448(19) 0.109(3) -0.0064(19) -0.0119(17) -0.0074(14) C104 0.0382(16) 0.071(3) 0.103(3) -0.049(2) 0.0230(18) -0.0210(17) C105 0.0505(18) 0.088(3) 0.061(2) -0.028(2) 0.0124(15) -0.0406(19) C106 0.0431(15) 0.058(2) 0.0471(18) -0.0009(15) -0.0036(13) -0.0270(14) C107 0.0326(13) 0.0403(16) 0.0496(18) -0.0074(13) 0.0001(12) -0.0132(12) C201 0.0552(17) 0.0402(17) 0.0584(19) -0.0151(14) 0.0024(14) -0.0110(14) C202 0.0341(12) 0.0267(13) 0.0376(15) -0.0052(11) -0.0120(11) -0.0002(10) C203 0.0367(13) 0.0324(15) 0.0519(17) 0.0007(13) -0.0011(12) -0.0106(12) C204 0.0421(15) 0.0470(18) 0.0426(17) -0.0030(14) 0.0039(12) -0.0062(13) C205 0.0542(17) 0.0381(16) 0.0408(17) -0.0037(13) -0.0063(13) -0.0074(14) C206 0.0433(14) 0.0302(14) 0.0367(15) 0.0031(12) -0.0123(12) -0.0084(12) C207 0.0304(12) 0.0317(14) 0.0353(14) 0.0027(11) -0.0081(10) -0.0059(11) C301 0.055(4) 0.047(4) 0.021(3) -0.005(3) 0.003(3) -0.008(3) C302 0.079(7) 0.029(4) 0.040(4) -0.010(4) 0.024(5) -0.024(5) C303 0.117(8) 0.035(4) 0.033(4) 0.000(3) 0.025(5) 0.000(5) C304 0.073(7) 0.099(9) 0.033(4) 0.000(5) -0.012(4) 0.006(6) C305 0.075(6) 0.069(7) 0.073(6) -0.038(5) 0.012(5) -0.015(5) C306 0.056(5) 0.025(4) 0.061(5) 0.000(4) 0.013(4) -0.004(4) C307 0.068(5) 0.132(9) 0.049(5) 0.016(5) -0.007(4) -0.004(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ga1 S2 2.2902(8) . ? Ga1 S1 2.3155(6) . ? Ga1 P1 2.3783(6) . ? Ga1 Ga2 2.3832(4) . ? Ga2 S4 2.3037(6) . ? Ga2 S3 2.3272(7) . ? Ga2 P2 2.3870(6) . ? S1 C1 1.765(2) . ? S2 C7 1.775(2) . ? S3 C19 1.768(2) . ? S4 C25 1.763(2) . ? P1 C8 1.800(2) . ? P1 C2 1.803(2) . ? P1 C13 1.804(2) . ? P2 C20 1.795(2) . ? P2 C31 1.803(2) . ? P2 C26 1.803(2) . ? C1 C2 1.402(3) . ? C1 C6 1.405(3) . ? C2 C3 1.388(3) . ? C3 C4 1.383(3) . ? C4 C5 1.385(3) . ? C5 C6 1.373(3) . ? C7 C8 1.401(3) . ? C7 C12 1.403(3) . ? C8 C9 1.403(3) . ? C9 C10 1.372(3) . ? C10 C11 1.379(4) . ? C11 C12 1.382(3) . ? C13 C14 1.389(3) . ? C13 C18 1.396(3) . ? C14 C15 1.386(3) . ? C15 C16 1.384(3) . ? C16 C17 1.371(3) . ? C17 C18 1.388(3) . ? C19 C24 1.396(3) . ? C19 C20 1.405(3) . ? C20 C21 1.391(3) . ? C21 C22 1.389(3) . ? C22 C23 1.381(3) . ? C23 C24 1.381(3) . ? C25 C30 1.405(3) . ? C25 C26 1.411(3) . ? C26 C27 1.393(3) . ? C27 C28 1.374(3) . ? C28 C29 1.391(3) . ? C29 C30 1.380(3) . ? C31 C36 1.390(3) . ? C31 C32 1.394(3) . ? C32 C33 1.380(3) . ? C33 C34 1.384(3) . ? C34 C35 1.372(3) . ? C35 C36 1.388(3) . ? Ga3 S5 2.2891(7) . ? Ga3 S6 2.3219(7) . ? Ga3 Ga4 2.3935(4) . ? Ga3 P3 2.3969(6) . ? Ga4 S7 2.2945(6) . ? Ga4 S8 2.3142(6) . ? Ga4 P4 2.3832(7) . ? S5 C37 1.765(2) . ? S6 C43 1.768(2) . ? S7 C55 1.773(2) . ? S8 C61 1.769(2) . ? P3 C44 1.803(2) . ? P3 C38 1.807(2) . ? P3 C49 1.817(2) . ? P4 C56 1.798(2) . ? P4 C62 1.801(2) . ? P4 C67 1.811(2) . ? C37 C38 1.405(3) . ? C37 C42 1.403(3) . ? C38 C39 1.400(3) . ? C39 C40 1.381(3) . ? C40 C41 1.375(3) . ? C41 C42 1.379(3) . ? C43 C44 1.401(3) . ? C43 C48 1.402(3) . ? C44 C45 1.391(3) . ? C45 C46 1.379(3) . ? C46 C47 1.386(3) . ? C47 C48 1.377(3) . ? C49 C54 1.377(3) . ? C49 C50 1.384(3) . ? C50 C51 1.380(3) . ? C51 C52 1.371(3) . ? C52 C53 1.364(4) . ? C53 C54 1.397(3) . ? C55 C60 1.400(3) . ? C55 C56 1.416(3) . ? C56 C57 1.397(3) . ? C57 C58 1.380(3) . ? C58 C59 1.386(3) . ? C59 C60 1.374(3) . ? C61 C66 1.402(3) . ? C61 C62 1.405(3) . ? C62 C63 1.401(3) . ? C63 C64 1.380(3) . ? C64 C65 1.386(3) . ? C65 C66 1.373(3) . ? C67 C72 1.385(3) . ? C67 C68 1.395(3) . ? C68 C69 1.383(3) . ? C69 C70 1.377(3) . ? C70 C71 1.376(3) . ? C71 C72 1.390(3) . ? C101 C102 1.504(4) . ? C102 C107 1.377(4) . ? C102 C103 1.382(4) . ? C103 C104 1.383(4) . ? C104 C105 1.379(5) . ? C105 C106 1.375(4) . ? C106 C107 1.375(4) . ? C201 C202 1.492(3) . ? C202 C207 1.389(3) . ? C202 C203 1.397(3) . ? C203 C204 1.365(4) . ? C204 C205 1.379(4) . ? C205 C206 1.386(4) . ? C206 C207 1.376(3) . ? C301 C306 1.3840 . ? C301 C302 1.3840 . ? C301 C307 1.5130 . ? C302 C303 1.3840 . ? C303 C304 1.3840 . ? C304 C305 1.3840 . ? C305 C306 1.3840 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S2 Ga1 S1 110.08(3) . . ? S2 Ga1 P1 90.20(2) . . ? S1 Ga1 P1 87.53(2) . . ? S2 Ga1 Ga2 120.56(2) . . ? S1 Ga1 Ga2 123.87(2) . . ? P1 Ga1 Ga2 113.538(19) . . ? S4 Ga2 S3 114.20(3) . . ? S4 Ga2 Ga1 112.15(2) . . ? S3 Ga2 Ga1 128.542(19) . . ? S4 Ga2 P2 88.03(2) . . ? S3 Ga2 P2 84.26(2) . . ? Ga1 Ga2 P2 118.59(2) . . ? C1 S1 Ga1 104.54(7) . . ? C7 S2 Ga1 102.13(8) . . ? C19 S3 Ga2 104.72(7) . . ? C25 S4 Ga2 101.41(7) . . ? C8 P1 C2 106.21(9) . . ? C8 P1 C13 107.90(9) . . ? C2 P1 C13 108.38(10) . . ? C8 P1 Ga1 101.71(7) . . ? C2 P1 Ga1 104.54(7) . . ? C13 P1 Ga1 126.50(7) . . ? C20 P2 C31 108.58(10) . . ? C20 P2 C26 108.24(9) . . ? C31 P2 C26 108.39(9) . . ? C20 P2 Ga2 105.31(7) . . ? C31 P2 Ga2 124.96(7) . . ? C26 P2 Ga2 100.30(7) . . ? C2 C1 C6 118.06(19) . . ? C2 C1 S1 124.46(15) . . ? C6 C1 S1 117.48(16) . . ? C3 C2 C1 120.43(19) . . ? C3 C2 P1 121.65(16) . . ? C1 C2 P1 117.85(15) . . ? C4 C3 C2 120.7(2) . . ? C3 C4 C5 119.1(2) . . ? C6 C5 C4 121.1(2) . . ? C5 C6 C1 120.6(2) . . ? C8 C7 C12 118.1(2) . . ? C8 C7 S2 124.71(16) . . ? C12 C7 S2 117.15(18) . . ? C7 C8 C9 119.9(2) . . ? C7 C8 P1 119.63(15) . . ? C9 C8 P1 120.32(18) . . ? C10 C9 C8 120.9(2) . . ? C9 C10 C11 119.5(2) . . ? C10 C11 C12 120.9(2) . . ? C11 C12 C7 120.7(2) . . ? C14 C13 C18 119.47(19) . . ? C14 C13 P1 121.09(15) . . ? C18 C13 P1 119.22(17) . . ? C15 C14 C13 120.2(2) . . ? C16 C15 C14 119.9(2) . . ? C17 C16 C15 120.2(2) . . ? C16 C17 C18 120.6(2) . . ? C17 C18 C13 119.5(2) . . ? C24 C19 C20 118.09(19) . . ? C24 C19 S3 118.69(17) . . ? C20 C19 S3 123.21(15) . . ? C21 C20 C19 120.48(18) . . ? C21 C20 P2 123.52(16) . . ? C19 C20 P2 115.98(15) . . ? C22 C21 C20 120.5(2) . . ? C23 C22 C21 119.0(2) . . ? C24 C23 C22 121.07(19) . . ? C23 C24 C19 120.8(2) . . ? C30 C25 C26 117.82(19) . . ? C30 C25 S4 117.89(16) . . ? C26 C25 S4 124.29(16) . . ? C27 C26 C25 120.05(19) . . ? C27 C26 P2 121.81(16) . . ? C25 C26 P2 118.14(15) . . ? C28 C27 C26 121.2(2) . . ? C27 C28 C29 119.1(2) . . ? C30 C29 C28 120.8(2) . . ? C29 C30 C25 120.9(2) . . ? C36 C31 C32 119.3(2) . . ? C36 C31 P2 122.27(17) . . ? C32 C31 P2 118.25(15) . . ? C33 C32 C31 120.3(2) . . ? C32 C33 C34 120.1(2) . . ? C35 C34 C33 120.0(2) . . ? C34 C35 C36 120.6(2) . . ? C35 C36 C31 119.8(2) . . ? S5 Ga3 S6 111.41(3) . . ? S5 Ga3 Ga4 112.86(2) . . ? S6 Ga3 Ga4 123.67(2) . . ? S5 Ga3 P3 89.66(2) . . ? S6 Ga3 P3 86.50(2) . . ? Ga4 Ga3 P3 126.180(18) . . ? S7 Ga4 S8 108.51(2) . . ? S7 Ga4 P4 89.38(2) . . ? S8 Ga4 P4 88.48(2) . . ? S7 Ga4 Ga3 122.51(2) . . ? S8 Ga4 Ga3 121.990(19) . . ? P4 Ga4 Ga3 115.84(2) . . ? C37 S5 Ga3 102.06(7) . . ? C43 S6 Ga3 104.74(7) . . ? C55 S7 Ga4 103.35(7) . . ? C61 S8 Ga4 104.23(7) . . ? C44 P3 C38 106.55(9) . . ? C44 P3 C49 105.32(10) . . ? C38 P3 C49 109.97(9) . . ? C44 P3 Ga3 104.36(7) . . ? C38 P3 Ga3 100.79(7) . . ? C49 P3 Ga3 128.22(7) . . ? C56 P4 C62 109.94(9) . . ? C56 P4 C67 108.20(9) . . ? C62 P4 C67 105.91(9) . . ? C56 P4 Ga4 103.46(7) . . ? C62 P4 Ga4 103.90(7) . . ? C67 P4 Ga4 124.93(7) . . ? C38 C37 C42 118.1(2) . . ? C38 C37 S5 125.00(15) . . ? C42 C37 S5 116.88(17) . . ? C39 C38 C37 119.43(19) . . ? C39 C38 P3 121.13(17) . . ? C37 C38 P3 119.32(15) . . ? C40 C39 C38 121.4(2) . . ? C41 C40 C39 119.0(2) . . ? C40 C41 C42 121.0(2) . . ? C41 C42 C37 121.0(2) . . ? C44 C43 C48 118.2(2) . . ? C44 C43 S6 123.88(16) . . ? C48 C43 S6 117.88(16) . . ? C45 C44 C43 120.1(2) . . ? C45 C44 P3 121.90(16) . . ? C43 C44 P3 117.94(16) . . ? C46 C45 C44 120.9(2) . . ? C45 C46 C47 119.1(2) . . ? C48 C47 C46 120.8(2) . . ? C47 C48 C43 120.7(2) . . ? C54 C49 C50 119.3(2) . . ? C54 C49 P3 123.93(17) . . ? C50 C49 P3 116.75(15) . . ? C51 C50 C49 120.3(2) . . ? C52 C51 C50 120.5(2) . . ? C53 C52 C51 119.6(2) . . ? C52 C53 C54 120.6(2) . . ? C49 C54 C53 119.6(2) . . ? C60 C55 C56 118.2(2) . . ? C60 C55 S7 116.55(17) . . ? C56 C55 S7 125.23(16) . . ? C57 C56 C55 119.24(19) . . ? C57 C56 P4 122.61(17) . . ? C55 C56 P4 118.15(16) . . ? C58 C57 C56 121.4(2) . . ? C57 C58 C59 119.1(2) . . ? C60 C59 C58 120.7(2) . . ? C59 C60 C55 121.2(2) . . ? C66 C61 C62 118.6(2) . . ? C66 C61 S8 117.14(16) . . ? C62 C61 S8 124.29(15) . . ? C63 C62 C61 119.80(18) . . ? C63 C62 P4 121.28(16) . . ? C61 C62 P4 118.91(16) . . ? C64 C63 C62 120.7(2) . . ? C63 C64 C65 119.1(2) . . ? C66 C65 C64 121.3(2) . . ? C65 C66 C61 120.4(2) . . ? C72 C67 C68 119.65(18) . . ? C72 C67 P4 119.61(15) . . ? C68 C67 P4 120.52(16) . . ? C69 C68 C67 119.6(2) . . ? C70 C69 C68 120.3(2) . . ? C71 C70 C69 120.5(2) . . ? C70 C71 C72 119.7(2) . . ? C67 C72 C71 120.2(2) . . ? C107 C102 C103 117.8(3) . . ? C107 C102 C101 120.7(3) . . ? C103 C102 C101 121.5(3) . . ? C104 C103 C102 121.4(3) . . ? C105 C104 C103 119.7(3) . . ? C106 C105 C104 119.4(3) . . ? C105 C106 C107 120.3(3) . . ? C106 C107 C102 121.4(3) . . ? C207 C202 C203 118.4(2) . . ? C207 C202 C201 119.9(2) . . ? C203 C202 C201 121.7(2) . . ? C204 C203 C202 121.4(3) . . ? C203 C204 C205 119.7(3) . . ? C204 C205 C206 120.0(3) . . ? C207 C206 C205 120.3(3) . . ? C206 C207 C202 120.3(2) . . ? C306 C301 C302 120.0 . . ? C306 C301 C307 120.0 . . ? C302 C301 C307 120.0 . . ? C303 C302 C301 120.0 . . ? C302 C303 C304 120.0 . . ? C303 C304 C305 120.0 . . ? C306 C305 C304 120.0 . . ? C305 C306 C301 120.0 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag S2 Ga1 Ga2 S4 76.18(3) . . . . ? S1 Ga1 Ga2 S4 -132.62(3) . . . . ? P1 Ga1 Ga2 S4 -28.98(3) . . . . ? S2 Ga1 Ga2 S3 -130.95(3) . . . . ? S1 Ga1 Ga2 S3 20.25(3) . . . . ? P1 Ga1 Ga2 S3 123.89(3) . . . . ? S2 Ga1 Ga2 P2 -24.18(3) . . . . ? S1 Ga1 Ga2 P2 127.02(3) . . . . ? P1 Ga1 Ga2 P2 -129.33(2) . . . . ? S2 Ga1 S1 C1 -97.19(8) . . . . ? P1 Ga1 S1 C1 -7.88(8) . . . . ? Ga2 Ga1 S1 C1 109.03(7) . . . . ? S1 Ga1 S2 C7 76.56(7) . . . . ? P1 Ga1 S2 C7 -10.88(7) . . . . ? Ga2 Ga1 S2 C7 -128.64(7) . . . . ? S4 Ga2 S3 C19 -105.89(7) . . . . ? Ga1 Ga2 S3 C19 101.68(7) . . . . ? P2 Ga2 S3 C19 -20.65(7) . . . . ? S3 Ga2 S4 C25 60.79(8) . . . . ? Ga1 Ga2 S4 C25 -142.22(8) . . . . ? P2 Ga2 S4 C25 -22.02(8) . . . . ? S2 Ga1 P1 C8 8.75(7) . . . . ? S1 Ga1 P1 C8 -101.33(7) . . . . ? Ga2 Ga1 P1 C8 132.53(7) . . . . ? S2 Ga1 P1 C2 119.14(7) . . . . ? S1 Ga1 P1 C2 9.05(7) . . . . ? Ga2 Ga1 P1 C2 -117.08(7) . . . . ? S2 Ga1 P1 C13 -114.20(9) . . . . ? S1 Ga1 P1 C13 135.71(9) . . . . ? Ga2 Ga1 P1 C13 9.58(9) . . . . ? S4 Ga2 P2 C20 136.33(7) . . . . ? S3 Ga2 P2 C20 21.77(7) . . . . ? Ga1 Ga2 P2 C20 -109.41(7) . . . . ? S4 Ga2 P2 C31 -97.19(8) . . . . ? S3 Ga2 P2 C31 148.25(8) . . . . ? Ga1 Ga2 P2 C31 17.07(8) . . . . ? S4 Ga2 P2 C26 24.02(7) . . . . ? S3 Ga2 P2 C26 -90.54(7) . . . . ? Ga1 Ga2 P2 C26 138.28(7) . . . . ? Ga1 S1 C1 C2 5.2(2) . . . . ? Ga1 S1 C1 C6 -174.45(15) . . . . ? C6 C1 C2 C3 -0.4(3) . . . . ? S1 C1 C2 C3 179.86(17) . . . . ? C6 C1 C2 P1 -177.63(16) . . . . ? S1 C1 C2 P1 2.7(3) . . . . ? C8 P1 C2 C3 -78.9(2) . . . . ? C13 P1 C2 C3 36.8(2) . . . . ? Ga1 P1 C2 C3 174.01(17) . . . . ? C8 P1 C2 C1 98.24(18) . . . . ? C13 P1 C2 C1 -146.05(16) . . . . ? Ga1 P1 C2 C1 -8.85(18) . . . . ? C1 C2 C3 C4 0.1(3) . . . . ? P1 C2 C3 C4 177.13(18) . . . . ? C2 C3 C4 C5 0.4(4) . . . . ? C3 C4 C5 C6 -0.4(4) . . . . ? C4 C5 C6 C1 0.1(4) . . . . ? C2 C1 C6 C5 0.4(3) . . . . ? S1 C1 C6 C5 -179.89(18) . . . . ? Ga1 S2 C7 C8 12.83(19) . . . . ? Ga1 S2 C7 C12 -168.66(15) . . . . ? C12 C7 C8 C9 -1.0(3) . . . . ? S2 C7 C8 C9 177.47(16) . . . . ? C12 C7 C8 P1 175.27(16) . . . . ? S2 C7 C8 P1 -6.2(3) . . . . ? C2 P1 C8 C7 -112.99(17) . . . . ? C13 P1 C8 C7 130.98(16) . . . . ? Ga1 P1 C8 C7 -3.88(17) . . . . ? C2 P1 C8 C9 63.29(18) . . . . ? C13 P1 C8 C9 -52.74(19) . . . . ? Ga1 P1 C8 C9 172.40(15) . . . . ? C7 C8 C9 C10 1.0(3) . . . . ? P1 C8 C9 C10 -175.29(17) . . . . ? C8 C9 C10 C11 -0.1(4) . . . . ? C9 C10 C11 C12 -0.8(4) . . . . ? C10 C11 C12 C7 0.7(4) . . . . ? C8 C7 C12 C11 0.2(3) . . . . ? S2 C7 C12 C11 -178.40(18) . . . . ? C8 P1 C13 C14 150.58(16) . . . . ? C2 P1 C13 C14 35.98(19) . . . . ? Ga1 P1 C13 C14 -89.12(17) . . . . ? C8 P1 C13 C18 -34.91(19) . . . . ? C2 P1 C13 C18 -149.52(16) . . . . ? Ga1 P1 C13 C18 85.38(17) . . . . ? C18 C13 C14 C15 1.9(3) . . . . ? P1 C13 C14 C15 176.36(16) . . . . ? C13 C14 C15 C16 -0.7(3) . . . . ? C14 C15 C16 C17 -0.5(3) . . . . ? C15 C16 C17 C18 0.5(3) . . . . ? C16 C17 C18 C13 0.6(3) . . . . ? C14 C13 C18 C17 -1.8(3) . . . . ? P1 C13 C18 C17 -176.43(16) . . . . ? Ga2 S3 C19 C24 -162.14(15) . . . . ? Ga2 S3 C19 C20 17.15(19) . . . . ? C24 C19 C20 C21 2.2(3) . . . . ? S3 C19 C20 C21 -177.07(16) . . . . ? C24 C19 C20 P2 -179.34(15) . . . . ? S3 C19 C20 P2 1.4(2) . . . . ? C31 P2 C20 C21 23.7(2) . . . . ? C26 P2 C20 C21 -93.75(19) . . . . ? Ga2 P2 C20 C21 159.67(16) . . . . ? C31 P2 C20 C19 -154.66(15) . . . . ? C26 P2 C20 C19 87.88(17) . . . . ? Ga2 P2 C20 C19 -18.70(17) . . . . ? C19 C20 C21 C22 -0.6(3) . . . . ? P2 C20 C21 C22 -178.88(16) . . . . ? C20 C21 C22 C23 -0.9(3) . . . . ? C21 C22 C23 C24 0.7(3) . . . . ? C22 C23 C24 C19 1.0(3) . . . . ? C20 C19 C24 C23 -2.4(3) . . . . ? S3 C19 C24 C23 176.90(17) . . . . ? Ga2 S4 C25 C30 -163.78(17) . . . . ? Ga2 S4 C25 C26 16.2(2) . . . . ? C30 C25 C26 C27 4.7(3) . . . . ? S4 C25 C26 C27 -175.21(17) . . . . ? C30 C25 C26 P2 -175.35(17) . . . . ? S4 C25 C26 P2 4.7(3) . . . . ? C20 P2 C26 C27 47.9(2) . . . . ? C31 P2 C26 C27 -69.65(19) . . . . ? Ga2 P2 C26 C27 157.97(17) . . . . ? C20 P2 C26 C25 -131.96(17) . . . . ? C31 P2 C26 C25 110.45(17) . . . . ? Ga2 P2 C26 C25 -21.93(17) . . . . ? C25 C26 C27 C28 -3.5(3) . . . . ? P2 C26 C27 C28 176.59(19) . . . . ? C26 C27 C28 C29 -0.2(4) . . . . ? C27 C28 C29 C30 2.6(4) . . . . ? C28 C29 C30 C25 -1.2(4) . . . . ? C26 C25 C30 C29 -2.4(4) . . . . ? S4 C25 C30 C29 177.5(2) . . . . ? C20 P2 C31 C36 -125.49(17) . . . . ? C26 P2 C31 C36 -8.1(2) . . . . ? Ga2 P2 C31 C36 109.41(17) . . . . ? C20 P2 C31 C32 59.93(18) . . . . ? C26 P2 C31 C32 177.30(16) . . . . ? Ga2 P2 C31 C32 -65.17(18) . . . . ? C36 C31 C32 C33 0.6(3) . . . . ? P2 C31 C32 C33 175.31(17) . . . . ? C31 C32 C33 C34 0.0(3) . . . . ? C32 C33 C34 C35 -0.6(3) . . . . ? C33 C34 C35 C36 0.6(3) . . . . ? C34 C35 C36 C31 0.0(3) . . . . ? C32 C31 C36 C35 -0.6(3) . . . . ? P2 C31 C36 C35 -175.09(16) . . . . ? S5 Ga3 Ga4 S7 -93.45(3) . . . . ? S6 Ga3 Ga4 S7 127.37(3) . . . . ? P3 Ga3 Ga4 S7 14.02(3) . . . . ? S5 Ga3 Ga4 S8 119.21(3) . . . . ? S6 Ga3 Ga4 S8 -19.97(3) . . . . ? P3 Ga3 Ga4 S8 -133.32(3) . . . . ? S5 Ga3 Ga4 P4 13.67(3) . . . . ? S6 Ga3 Ga4 P4 -125.50(3) . . . . ? P3 Ga3 Ga4 P4 121.15(3) . . . . ? S6 Ga3 S5 C37 -71.08(7) . . . . ? Ga4 Ga3 S5 C37 144.68(7) . . . . ? P3 Ga3 S5 C37 15.03(7) . . . . ? S5 Ga3 S6 C43 101.64(7) . . . . ? Ga4 Ga3 S6 C43 -118.68(7) . . . . ? P3 Ga3 S6 C43 13.38(7) . . . . ? S8 Ga4 S7 C55 -93.60(7) . . . . ? P4 Ga4 S7 C55 -5.40(7) . . . . ? Ga3 Ga4 S7 C55 115.26(7) . . . . ? S7 Ga4 S8 C61 91.48(7) . . . . ? P4 Ga4 S8 C61 2.64(7) . . . . ? Ga3 Ga4 S8 C61 -117.19(7) . . . . ? S5 Ga3 P3 C44 -124.93(7) . . . . ? S6 Ga3 P3 C44 -13.46(7) . . . . ? Ga4 Ga3 P3 C44 116.59(7) . . . . ? S5 Ga3 P3 C38 -14.56(7) . . . . ? S6 Ga3 P3 C38 96.91(7) . . . . ? Ga4 Ga3 P3 C38 -133.04(7) . . . . ? S5 Ga3 P3 C49 111.79(9) . . . . ? S6 Ga3 P3 C49 -136.74(9) . . . . ? Ga4 Ga3 P3 C49 -6.69(9) . . . . ? S7 Ga4 P4 C56 5.57(7) . . . . ? S8 Ga4 P4 C56 114.10(7) . . . . ? Ga3 Ga4 P4 C56 -120.73(7) . . . . ? S7 Ga4 P4 C62 -109.30(7) . . . . ? S8 Ga4 P4 C62 -0.77(7) . . . . ? Ga3 Ga4 P4 C62 124.41(7) . . . . ? S7 Ga4 P4 C67 129.55(8) . . . . ? S8 Ga4 P4 C67 -121.92(8) . . . . ? Ga3 Ga4 P4 C67 3.25(9) . . . . ? Ga3 S5 C37 C38 -13.86(19) . . . . ? Ga3 S5 C37 C42 167.15(15) . . . . ? C42 C37 C38 C39 -3.3(3) . . . . ? S5 C37 C38 C39 177.70(16) . . . . ? C42 C37 C38 P3 -179.36(16) . . . . ? S5 C37 C38 P3 1.7(3) . . . . ? C44 P3 C38 C39 -56.37(19) . . . . ? C49 P3 C38 C39 57.3(2) . . . . ? Ga3 P3 C38 C39 -165.03(16) . . . . ? C44 P3 C38 C37 119.60(17) . . . . ? C49 P3 C38 C37 -126.74(17) . . . . ? Ga3 P3 C38 C37 10.94(17) . . . . ? C37 C38 C39 C40 3.2(3) . . . . ? P3 C38 C39 C40 179.13(17) . . . . ? C38 C39 C40 C41 -0.6(3) . . . . ? C39 C40 C41 C42 -1.8(3) . . . . ? C40 C41 C42 C37 1.6(3) . . . . ? C38 C37 C42 C41 1.0(3) . . . . ? S5 C37 C42 C41 -179.91(17) . . . . ? Ga3 S6 C43 C44 -11.78(18) . . . . ? Ga3 S6 C43 C48 170.22(14) . . . . ? C48 C43 C44 C45 0.3(3) . . . . ? S6 C43 C44 C45 -177.65(15) . . . . ? C48 C43 C44 P3 178.29(15) . . . . ? S6 C43 C44 P3 0.3(2) . . . . ? C38 P3 C44 C45 82.75(19) . . . . ? C49 P3 C44 C45 -34.05(19) . . . . ? Ga3 P3 C44 C45 -171.12(16) . . . . ? C38 P3 C44 C43 -95.16(17) . . . . ? C49 P3 C44 C43 148.04(15) . . . . ? Ga3 P3 C44 C43 10.96(16) . . . . ? C43 C44 C45 C46 1.7(3) . . . . ? P3 C44 C45 C46 -176.19(17) . . . . ? C44 C45 C46 C47 -2.2(3) . . . . ? C45 C46 C47 C48 0.7(3) . . . . ? C46 C47 C48 C43 1.4(3) . . . . ? C44 C43 C48 C47 -1.9(3) . . . . ? S6 C43 C48 C47 176.26(17) . . . . ? C44 P3 C49 C54 110.5(2) . . . . ? C38 P3 C49 C54 -4.0(2) . . . . ? Ga3 P3 C49 C54 -126.64(19) . . . . ? C44 P3 C49 C50 -69.8(2) . . . . ? C38 P3 C49 C50 175.73(18) . . . . ? Ga3 P3 C49 C50 53.1(2) . . . . ? C54 C49 C50 C51 -0.2(4) . . . . ? P3 C49 C50 C51 -179.9(2) . . . . ? C49 C50 C51 C52 0.7(4) . . . . ? C50 C51 C52 C53 -0.7(4) . . . . ? C51 C52 C53 C54 0.2(4) . . . . ? C50 C49 C54 C53 -0.3(4) . . . . ? P3 C49 C54 C53 179.34(19) . . . . ? C52 C53 C54 C49 0.4(4) . . . . ? Ga4 S7 C55 C60 -175.61(14) . . . . ? Ga4 S7 C55 C56 4.61(18) . . . . ? C60 C55 C56 C57 -0.4(3) . . . . ? S7 C55 C56 C57 179.36(16) . . . . ? C60 C55 C56 P4 -179.71(15) . . . . ? S7 C55 C56 P4 0.1(2) . . . . ? C62 P4 C56 C57 -73.35(19) . . . . ? C67 P4 C56 C57 41.9(2) . . . . ? Ga4 P4 C56 C57 176.19(16) . . . . ? C62 P4 C56 C55 105.91(17) . . . . ? C67 P4 C56 C55 -138.85(16) . . . . ? Ga4 P4 C56 C55 -4.54(16) . . . . ? C55 C56 C57 C58 0.4(3) . . . . ? P4 C56 C57 C58 179.67(16) . . . . ? C56 C57 C58 C59 -0.5(3) . . . . ? C57 C58 C59 C60 0.5(3) . . . . ? C58 C59 C60 C55 -0.6(3) . . . . ? C56 C55 C60 C59 0.5(3) . . . . ? S7 C55 C60 C59 -179.30(18) . . . . ? Ga4 S8 C61 C66 176.66(14) . . . . ? Ga4 S8 C61 C62 -5.15(19) . . . . ? C66 C61 C62 C63 2.0(3) . . . . ? S8 C61 C62 C63 -176.14(16) . . . . ? C66 C61 C62 P4 -176.78(15) . . . . ? S8 C61 C62 P4 5.1(2) . . . . ? C56 P4 C62 C63 69.05(19) . . . . ? C67 P4 C62 C63 -47.63(19) . . . . ? Ga4 P4 C62 C63 179.22(16) . . . . ? C56 P4 C62 C61 -112.17(17) . . . . ? C67 P4 C62 C61 131.15(16) . . . . ? Ga4 P4 C62 C61 -2.00(17) . . . . ? C61 C62 C63 C64 -1.1(3) . . . . ? P4 C62 C63 C64 177.71(16) . . . . ? C62 C63 C64 C65 -0.3(3) . . . . ? C63 C64 C65 C66 0.6(3) . . . . ? C64 C65 C66 C61 0.4(3) . . . . ? C62 C61 C66 C65 -1.7(3) . . . . ? S8 C61 C66 C65 176.59(17) . . . . ? C56 P4 C67 C72 -153.25(17) . . . . ? C62 P4 C67 C72 -35.4(2) . . . . ? Ga4 P4 C67 C72 84.84(18) . . . . ? C56 P4 C67 C68 32.3(2) . . . . ? C62 P4 C67 C68 150.10(18) . . . . ? Ga4 P4 C67 C68 -89.65(19) . . . . ? C72 C67 C68 C69 2.1(3) . . . . ? P4 C67 C68 C69 176.56(18) . . . . ? C67 C68 C69 C70 -0.7(4) . . . . ? C68 C69 C70 C71 -0.9(4) . . . . ? C69 C70 C71 C72 0.9(4) . . . . ? C68 C67 C72 C71 -2.0(3) . . . . ? P4 C67 C72 C71 -176.54(17) . . . . ? C70 C71 C72 C67 0.5(3) . . . . ? C107 C102 C103 C104 -0.5(4) . . . . ? C101 C102 C103 C104 178.4(3) . . . . ? C102 C103 C104 C105 0.0(5) . . . . ? C103 C104 C105 C106 0.9(5) . . . . ? C104 C105 C106 C107 -1.3(4) . . . . ? C105 C106 C107 C102 0.9(4) . . . . ? C103 C102 C107 C106 0.1(4) . . . . ? C101 C102 C107 C106 -178.8(3) . . . . ? C207 C202 C203 C204 -0.7(4) . . . . ? C201 C202 C203 C204 179.2(2) . . . . ? C202 C203 C204 C205 0.6(4) . . . . ? C203 C204 C205 C206 0.1(4) . . . . ? C204 C205 C206 C207 -0.7(4) . . . . ? C205 C206 C207 C202 0.6(3) . . . . ? C203 C202 C207 C206 0.1(3) . . . . ? C201 C202 C207 C206 -179.9(2) . . . . ? C306 C301 C302 C303 0.0 . . . . ? C307 C301 C302 C303 180.0 . . . . ? C301 C302 C303 C304 0.0 . . . . ? C302 C303 C304 C305 0.0 . . . . ? C303 C304 C305 C306 0.0 . . . . ? C304 C305 C306 C301 0.0 . . . . ? C302 C301 C306 C305 0.0 . . . . ? C307 C301 C306 C305 180.0 . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.459 _refine_diff_density_min -0.365 _refine_diff_density_rms 0.071 #============================================================================ data_c2c _database_code_depnum_ccdc_archive 'CCDC 722490' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H32 Ga2 P2 S5' _chemical_formula_weight 898.36 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Ga Ga 0.2307 1.6083 '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' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 21.4599(8) _cell_length_b 10.1678(4) _cell_length_c 18.2790(7) _cell_angle_alpha 90.00 _cell_angle_beta 95.722(3) _cell_angle_gamma 90.00 _cell_volume 3968.6(3) _cell_formula_units_Z 4 _cell_measurement_temperature 130(2) _cell_measurement_reflns_used 11357 _cell_measurement_theta_min 2.7545 _cell_measurement_theta_max 32.4683 _exptl_crystal_description needles _exptl_crystal_colour colourless _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.504 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1824 _exptl_absorpt_coefficient_mu 1.732 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET) (compiled Oct 18 2006,16:28:17) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_correction_T_min 0.80778 _exptl_absorpt_correction_T_max 1 _exptl_special_details ; ? ; _diffrn_ambient_temperature 130(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'ccd xcalibur s' _diffrn_measurement_method '\w scans and \f scans' _diffrn_detector_area_resol_mean 16.356 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 50091 _diffrn_reflns_av_R_equivalents 0.0634 _diffrn_reflns_av_sigmaI/netI 0.0511 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.79 _diffrn_reflns_theta_max 28.27 _reflns_number_total 4922 _reflns_number_gt 3578 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET) (compiled Oct 18 2006,16:28:17) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET) (compiled Oct 18 2006,16:28:17) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET) (compiled Oct 18 2006,16:28:17) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP3 for Windows (L. J. Farrugia, 1997)' _computing_publication_material 'WINGX (L.J. Farrugia,1999)' _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^)+(0.0454P)^2^+0.9381P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4922 _refine_ls_number_parameters 231 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0662 _refine_ls_R_factor_gt 0.0377 _refine_ls_wR_factor_ref 0.0914 _refine_ls_wR_factor_gt 0.0808 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.031 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group S1 S 0.5000 0.12680(10) 0.2500 0.0334(3) Uani 1 2 d S . . C20 C 0.4384(2) -0.0136(7) 0.0127(2) 0.0872(19) Uani 1 1 d . . . H20 H 0.3961 -0.0189 0.0234 0.105 Uiso 1 1 calc R . . C21 C 0.4695(2) 0.1042(7) 0.0265(2) 0.0815(18) Uani 1 1 d . . . H21 H 0.4461 0.1750 0.0439 0.098 Uiso 1 1 calc R . . C22 C 0.5340(2) 0.1292(7) 0.0168(2) 0.105(2) Uani 1 1 d . . . H22 H 0.5554 0.2096 0.0280 0.127 Uiso 1 1 calc R . . Ga1 Ga 0.428146(13) 0.26761(3) 0.207792(17) 0.02195(10) Uani 1 1 d . . . P1 P 0.36174(3) 0.42362(7) 0.25698(4) 0.02004(16) Uani 1 1 d . . . S2 S 0.46834(3) 0.43256(7) 0.14267(4) 0.02462(16) Uani 1 1 d . . . S3 S 0.34586(3) 0.15760(8) 0.15141(5) 0.03207(19) Uani 1 1 d . . . C1 C 0.43800(12) 0.5763(3) 0.18008(15) 0.0214(6) Uani 1 1 d . . . C2 C 0.39382(12) 0.5782(3) 0.23177(15) 0.0209(6) Uani 1 1 d . . . C3 C 0.37335(13) 0.6978(3) 0.25747(16) 0.0279(7) Uani 1 1 d . . . H3 H 0.3434 0.6987 0.2924 0.033 Uiso 1 1 calc R . . C4 C 0.39591(14) 0.8151(3) 0.23306(17) 0.0328(7) Uani 1 1 d . . . H4 H 0.3820 0.8963 0.2513 0.039 Uiso 1 1 calc R . . C5 C 0.43908(14) 0.8130(3) 0.18161(17) 0.0313(7) Uani 1 1 d . . . H5 H 0.4544 0.8934 0.1639 0.038 Uiso 1 1 calc R . . C6 C 0.45997(13) 0.6956(3) 0.15593(15) 0.0264(6) Uani 1 1 d . . . H6 H 0.4900 0.6959 0.1210 0.032 Uiso 1 1 calc R . . C7 C 0.28954(12) 0.2845(3) 0.14763(15) 0.0230(6) Uani 1 1 d . . . C8 C 0.29335(11) 0.3970(3) 0.19264(15) 0.0213(6) Uani 1 1 d . . . C9 C 0.24545(13) 0.4897(3) 0.18588(15) 0.0283(7) Uani 1 1 d . . . H9 H 0.2484 0.5657 0.2162 0.034 Uiso 1 1 calc R . . C10 C 0.19376(14) 0.4725(3) 0.13566(18) 0.0369(8) Uani 1 1 d . . . H10 H 0.1610 0.5358 0.1315 0.044 Uiso 1 1 calc R . . C11 C 0.19028(14) 0.3618(3) 0.09138(17) 0.0370(8) Uani 1 1 d . . . H11 H 0.1549 0.3494 0.0565 0.044 Uiso 1 1 calc R . . C12 C 0.23731(13) 0.2696(3) 0.09713(16) 0.0314(7) Uani 1 1 d . . . H12 H 0.2340 0.1945 0.0661 0.038 Uiso 1 1 calc R . . C13 C 0.33519(13) 0.4340(3) 0.34723(15) 0.0240(6) Uani 1 1 d . . . C14 C 0.37388(14) 0.4886(3) 0.40519(16) 0.0336(7) Uani 1 1 d . . . H14 H 0.4128 0.5267 0.3962 0.040 Uiso 1 1 calc R . . C15 C 0.35571(17) 0.4875(4) 0.47550(18) 0.0422(8) Uani 1 1 d . . . H15 H 0.3825 0.5241 0.5148 0.051 Uiso 1 1 calc R . . C16 C 0.29929(17) 0.4339(3) 0.48909(18) 0.0443(9) Uani 1 1 d . . . H16 H 0.2870 0.4338 0.5376 0.053 Uiso 1 1 calc R . . C17 C 0.26063(16) 0.3803(3) 0.43224(18) 0.0387(8) Uani 1 1 d . . . H17 H 0.2215 0.3433 0.4415 0.046 Uiso 1 1 calc R . . C18 C 0.27848(14) 0.3800(3) 0.36172(16) 0.0295(7) Uani 1 1 d . . . H18 H 0.2516 0.3425 0.3228 0.035 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 S1 0.0294(5) 0.0179(5) 0.0508(7) 0.000 -0.0071(5) 0.000 C20 0.055(3) 0.165(6) 0.043(3) 0.036(3) 0.014(2) 0.042(3) C21 0.071(3) 0.139(5) 0.036(2) 0.017(3) 0.012(2) 0.057(3) C22 0.090(4) 0.198(6) 0.032(2) 0.052(3) 0.024(2) 0.092(4) Ga1 0.01858(15) 0.01881(16) 0.02817(19) -0.00251(13) 0.00089(12) -0.00056(12) P1 0.0188(3) 0.0210(4) 0.0204(4) -0.0011(3) 0.0026(3) -0.0003(3) S2 0.0266(3) 0.0225(4) 0.0258(4) -0.0015(3) 0.0076(3) 0.0006(3) S3 0.0226(3) 0.0282(4) 0.0452(5) -0.0135(4) 0.0018(3) -0.0048(3) C1 0.0200(12) 0.0221(14) 0.0208(14) -0.0020(11) -0.0034(11) 0.0010(11) C2 0.0196(12) 0.0200(14) 0.0222(15) -0.0021(11) -0.0020(11) -0.0007(10) C3 0.0268(14) 0.0260(16) 0.0315(17) -0.0040(13) 0.0054(12) 0.0033(11) C4 0.0393(17) 0.0207(16) 0.0383(19) -0.0039(14) 0.0040(14) 0.0039(13) C5 0.0370(16) 0.0190(15) 0.0373(18) 0.0043(13) 0.0002(14) -0.0027(12) C6 0.0298(15) 0.0246(16) 0.0250(16) 0.0036(12) 0.0038(12) -0.0016(12) C7 0.0176(12) 0.0278(15) 0.0244(15) 0.0036(12) 0.0063(11) -0.0049(11) C8 0.0171(12) 0.0284(15) 0.0190(14) 0.0050(12) 0.0041(10) -0.0034(11) C9 0.0261(14) 0.0322(17) 0.0270(16) 0.0061(13) 0.0043(12) 0.0005(12) C10 0.0238(15) 0.043(2) 0.044(2) 0.0145(16) 0.0017(14) 0.0033(13) C11 0.0259(15) 0.049(2) 0.0339(19) 0.0065(16) -0.0083(13) -0.0098(14) C12 0.0292(15) 0.0381(18) 0.0267(16) 0.0028(14) 0.0014(12) -0.0114(13) C13 0.0285(14) 0.0251(15) 0.0187(14) 0.0014(12) 0.0041(11) 0.0080(12) C14 0.0313(16) 0.0431(19) 0.0259(17) -0.0063(14) 0.0006(13) 0.0061(14) C15 0.048(2) 0.052(2) 0.0249(17) -0.0037(16) -0.0026(15) 0.0132(17) C16 0.064(2) 0.045(2) 0.0266(18) 0.0099(16) 0.0181(17) 0.0230(18) C17 0.0450(19) 0.0356(19) 0.038(2) 0.0120(15) 0.0179(16) 0.0066(15) C18 0.0339(16) 0.0258(16) 0.0292(17) 0.0072(13) 0.0054(13) -0.0014(12) _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 S1 Ga1 2.1876(7) 2_655 ? S1 Ga1 2.1876(7) . ? C20 C21 1.382(8) . ? C20 C22 1.444(8) 5_655 ? C21 C22 1.436(7) . ? C22 C20 1.444(8) 5_655 ? Ga1 S3 2.2513(8) . ? Ga1 S2 2.2757(8) . ? Ga1 P1 2.3688(7) . ? P1 C2 1.795(3) . ? P1 C13 1.801(3) . ? P1 C8 1.807(3) . ? S2 C1 1.766(3) . ? S3 C7 1.765(3) . ? C1 C6 1.388(4) . ? C1 C2 1.404(4) . ? C2 C3 1.391(4) . ? C3 C4 1.377(4) . ? C4 C5 1.385(4) . ? C5 C6 1.375(4) . ? C7 C12 1.387(4) . ? C7 C8 1.407(4) . ? C8 C9 1.391(4) . ? C9 C10 1.379(4) . ? C10 C11 1.385(5) . ? C11 C12 1.374(4) . ? C13 C18 1.384(4) . ? C13 C14 1.395(4) . ? C14 C15 1.380(4) . ? C15 C16 1.373(5) . ? C16 C17 1.376(5) . ? C17 C18 1.381(4) . ? 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 Ga1 S1 Ga1 98.24(4) 2_655 . ? C21 C20 C22 124.4(5) . 5_655 ? C20 C21 C22 125.8(5) . . ? C21 C22 C20 109.8(6) . 5_655 ? S1 Ga1 S3 109.23(3) . . ? S1 Ga1 S2 112.10(3) . . ? S3 Ga1 S2 116.59(3) . . ? S1 Ga1 P1 137.22(2) . . ? S3 Ga1 P1 91.86(3) . . ? S2 Ga1 P1 88.78(3) . . ? C2 P1 C13 110.39(13) . . ? C2 P1 C8 105.74(12) . . ? C13 P1 C8 107.11(12) . . ? C2 P1 Ga1 103.20(9) . . ? C13 P1 Ga1 130.09(9) . . ? C8 P1 Ga1 97.65(9) . . ? C1 S2 Ga1 103.53(9) . . ? C7 S3 Ga1 99.06(9) . . ? C6 C1 C2 118.4(2) . . ? C6 C1 S2 116.7(2) . . ? C2 C1 S2 124.9(2) . . ? C3 C2 C1 119.8(3) . . ? C3 C2 P1 122.5(2) . . ? C1 C2 P1 117.6(2) . . ? C4 C3 C2 121.0(3) . . ? C3 C4 C5 119.2(3) . . ? C6 C5 C4 120.5(3) . . ? C5 C6 C1 121.2(3) . . ? C12 C7 C8 118.3(3) . . ? C12 C7 S3 116.8(2) . . ? C8 C7 S3 124.9(2) . . ? C9 C8 C7 120.0(3) . . ? C9 C8 P1 120.1(2) . . ? C7 C8 P1 119.9(2) . . ? C10 C9 C8 120.8(3) . . ? C9 C10 C11 119.0(3) . . ? C12 C11 C10 120.9(3) . . ? C11 C12 C7 121.0(3) . . ? C18 C13 C14 118.7(3) . . ? C18 C13 P1 121.1(2) . . ? C14 C13 P1 120.0(2) . . ? C15 C14 C13 120.1(3) . . ? C16 C15 C14 120.5(3) . . ? C15 C16 C17 119.8(3) . . ? C16 C17 C18 120.2(3) . . ? C17 C18 C13 120.6(3) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 28.27 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.339 _refine_diff_density_min -0.783 _refine_diff_density_rms 0.081