# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_emma _database_code_depnum_ccdc_archive 'CCDC 925372' #TrackingRef '1a_Emma.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C11 H25 Au Cl P S' _chemical_formula_weight 452.76 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' 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 26.953(3) _cell_length_b 8.1226(4) _cell_length_c 18.690(2) _cell_angle_alpha 90.00 _cell_angle_beta 132.03(2) _cell_angle_gamma 90.00 _cell_volume 3039.0(5) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 12955 _cell_measurement_theta_min 2.1761 _cell_measurement_theta_max 30.8072 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.979 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1744 _exptl_absorpt_coefficient_mu 10.072 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.20370 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Xcalibur, Eos' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 16.1419 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 40680 _diffrn_reflns_av_R_equivalents 0.0400 _diffrn_reflns_av_sigmaI/netI 0.0252 _diffrn_reflns_limit_h_min -37 _diffrn_reflns_limit_h_max 37 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.18 _diffrn_reflns_theta_max 30.88 _reflns_number_total 4529 _reflns_number_gt 4056 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker XP' _computing_publication_material SHELXL-97 _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. Both tert. butyl groups are disordered over two positions. Appropriate restraints were used to improve stability of refinement, but dimensions of disordered groups should be interpreted with caution. ; _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^)+(0.0155P)^2^+6.0860P] 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 4529 _refine_ls_number_parameters 170 _refine_ls_number_restraints 78 _refine_ls_R_factor_all 0.0269 _refine_ls_R_factor_gt 0.0210 _refine_ls_wR_factor_ref 0.0428 _refine_ls_wR_factor_gt 0.0406 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.072 _refine_ls_shift/su_max 0.004 _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 Au1 Au 0.328870(5) 0.544663(12) 0.967415(7) 0.01987(4) Uani 1 1 d . . . Cl1 Cl 0.42308(4) 0.38796(9) 1.05516(5) 0.02908(15) Uani 1 1 d . . . S1 S 0.24118(4) 0.72088(8) 0.88824(5) 0.02335(14) Uani 1 1 d . . . P1 P 0.15826(3) 0.59393(8) 0.77777(5) 0.01738(13) Uani 1 1 d . A . C1 C 0.13908(14) 0.4284(3) 0.82685(19) 0.0225(6) Uani 1 1 d D . . C11 C 0.1559(3) 0.4909(5) 0.9184(3) 0.0307(11) Uani 0.843(9) 1 d PDU A 1 H11A H 0.1273 0.5850 0.9024 0.046 Uiso 0.843(9) 1 calc PR A 1 H11B H 0.2028 0.5250 0.9654 0.046 Uiso 0.843(9) 1 calc PR A 1 H11C H 0.1484 0.4026 0.9460 0.046 Uiso 0.843(9) 1 calc PR A 1 C12 C 0.06754(18) 0.3693(6) 0.7540(3) 0.0288(9) Uani 0.843(9) 1 d PDU A 1 H12A H 0.0576 0.3317 0.6958 0.043 Uiso 0.843(9) 1 calc PR A 1 H12B H 0.0374 0.4598 0.7376 0.043 Uiso 0.843(9) 1 calc PR A 1 H12C H 0.0612 0.2780 0.7815 0.043 Uiso 0.843(9) 1 calc PR A 1 C13 C 0.18626(17) 0.2800(4) 0.8578(3) 0.0246(9) Uani 0.843(9) 1 d PDU A 1 H13A H 0.1812 0.1985 0.8912 0.037 Uiso 0.843(9) 1 calc PR A 1 H13B H 0.2326 0.3185 0.9011 0.037 Uiso 0.843(9) 1 calc PR A 1 H13C H 0.1746 0.2296 0.8006 0.037 Uiso 0.843(9) 1 calc PR A 1 C11' C 0.1151(12) 0.506(2) 0.8783(16) 0.028(5) Uiso 0.157(9) 1 d PDU A 2 H11D H 0.0716 0.5594 0.8299 0.041 Uiso 0.157(9) 1 calc PR A 2 H11E H 0.1478 0.5881 0.9260 0.041 Uiso 0.157(9) 1 calc PR A 2 H11F H 0.1113 0.4189 0.9106 0.041 Uiso 0.157(9) 1 calc PR A 2 C12' C 0.0774(9) 0.318(3) 0.7493(13) 0.024(5) Uiso 0.157(9) 1 d PDU A 2 H12D H 0.0670 0.2477 0.7805 0.037 Uiso 0.157(9) 1 calc PR A 2 H12E H 0.0878 0.2483 0.7179 0.037 Uiso 0.157(9) 1 calc PR A 2 H12F H 0.0389 0.3875 0.7011 0.037 Uiso 0.157(9) 1 calc PR A 2 C13' C 0.1968(8) 0.317(2) 0.9016(15) 0.028(5) Uiso 0.157(9) 1 d PDU A 2 H13D H 0.1817 0.2334 0.9212 0.042 Uiso 0.157(9) 1 calc PR A 2 H13E H 0.2327 0.3824 0.9578 0.042 Uiso 0.157(9) 1 calc PR A 2 H13F H 0.2134 0.2632 0.8743 0.042 Uiso 0.157(9) 1 calc PR A 2 C2 C 0.09200(14) 0.7560(3) 0.70742(18) 0.0219(5) Uani 1 1 d D . . C21 C 0.0735(2) 0.8143(6) 0.7636(3) 0.0285(10) Uani 0.808(10) 1 d PDU A 1 H21A H 0.1139 0.8507 0.8277 0.043 Uiso 0.808(10) 1 calc PR A 1 H21B H 0.0527 0.7238 0.7701 0.043 Uiso 0.808(10) 1 calc PR A 1 H21C H 0.0420 0.9063 0.7296 0.043 Uiso 0.808(10) 1 calc PR A 1 C22 C 0.03082(18) 0.6918(4) 0.6069(3) 0.0284(11) Uani 0.808(10) 1 d PDU A 1 H22A H 0.0151 0.5893 0.6136 0.043 Uiso 0.808(10) 1 calc PR A 1 H22B H 0.0433 0.6710 0.5691 0.043 Uiso 0.808(10) 1 calc PR A 1 H22C H -0.0049 0.7743 0.5741 0.043 Uiso 0.808(10) 1 calc PR A 1 C23 C 0.1202(2) 0.9038(5) 0.6914(4) 0.0262(9) Uani 0.808(10) 1 d PDU A 1 H23A H 0.0849 0.9857 0.6502 0.039 Uiso 0.808(10) 1 calc PR A 1 H23B H 0.1362 0.8650 0.6603 0.039 Uiso 0.808(10) 1 calc PR A 1 H23C H 0.1572 0.9538 0.7537 0.039 Uiso 0.808(10) 1 calc PR A 1 C21' C 0.0916(11) 0.869(2) 0.7778(12) 0.028(5) Uiso 0.192(10) 1 d PDU A 2 H21D H 0.0564 0.9525 0.7397 0.042 Uiso 0.192(10) 1 calc PR A 2 H21E H 0.1350 0.9238 0.8248 0.042 Uiso 0.192(10) 1 calc PR A 2 H21F H 0.0831 0.8002 0.8118 0.042 Uiso 0.192(10) 1 calc PR A 2 C22' C 0.0171(6) 0.6929(19) 0.6376(12) 0.030(4) Uiso 0.192(10) 1 d PDU A 2 H22D H 0.0081 0.6432 0.6758 0.045 Uiso 0.192(10) 1 calc PR A 2 H22E H 0.0101 0.6106 0.5933 0.045 Uiso 0.192(10) 1 calc PR A 2 H22F H -0.0133 0.7859 0.6007 0.045 Uiso 0.192(10) 1 calc PR A 2 C23' C 0.1004(11) 0.877(2) 0.6556(15) 0.033(5) Uiso 0.192(10) 1 d PDU A 2 H23D H 0.0697 0.9701 0.6330 0.049 Uiso 0.192(10) 1 calc PR A 2 H23E H 0.0905 0.8235 0.6003 0.049 Uiso 0.192(10) 1 calc PR A 2 H23F H 0.1465 0.9181 0.6996 0.049 Uiso 0.192(10) 1 calc PR A 2 C3 C 0.17547(15) 0.4914(3) 0.70790(19) 0.0218(5) Uani 1 1 d . . . H3 H 0.2128 0.4134 0.7546 0.026 Uiso 1 1 calc R A . C31 C 0.12066(18) 0.3834(5) 0.6238(2) 0.0438(9) Uani 1 1 d . A . H31A H 0.0826 0.4523 0.5732 0.066 Uiso 1 1 calc R . . H31B H 0.1063 0.3030 0.6458 0.066 Uiso 1 1 calc R . . H31C H 0.1378 0.3254 0.5981 0.066 Uiso 1 1 calc R . . C32 C 0.20343(17) 0.6053(4) 0.6780(2) 0.0339(7) Uani 1 1 d . A . H32A H 0.2231 0.5397 0.6584 0.051 Uiso 1 1 calc R . . H32B H 0.2378 0.6759 0.7324 0.051 Uiso 1 1 calc R . . H32C H 0.1674 0.6738 0.6239 0.051 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 Au1 0.01700(6) 0.02399(6) 0.01309(5) -0.00284(4) 0.00780(4) -0.00739(4) Cl1 0.0202(3) 0.0347(4) 0.0228(3) 0.0018(3) 0.0104(3) -0.0020(3) S1 0.0222(3) 0.0192(3) 0.0166(3) -0.0064(2) 0.0080(3) -0.0073(3) P1 0.0175(3) 0.0158(3) 0.0137(3) -0.0044(2) 0.0084(3) -0.0042(2) C1 0.0246(15) 0.0203(12) 0.0219(13) -0.0048(10) 0.0153(13) -0.0064(10) C11 0.045(3) 0.0285(18) 0.0262(19) -0.0053(14) 0.027(2) -0.0083(17) C12 0.0203(18) 0.031(2) 0.033(2) -0.0026(17) 0.0172(17) -0.0072(16) C13 0.0246(18) 0.0205(16) 0.0263(19) -0.0017(14) 0.0161(16) -0.0057(13) C2 0.0194(13) 0.0182(12) 0.0189(12) -0.0027(10) 0.0090(12) 0.0004(10) C21 0.025(2) 0.033(2) 0.033(2) -0.0012(18) 0.0215(19) 0.0041(19) C22 0.0204(19) 0.0259(18) 0.0209(18) -0.0023(14) 0.0064(16) 0.0025(14) C23 0.031(2) 0.0192(17) 0.028(2) 0.0039(16) 0.020(2) 0.0061(16) C3 0.0253(15) 0.0204(12) 0.0171(12) -0.0039(10) 0.0130(12) -0.0008(11) C31 0.042(2) 0.061(2) 0.0364(18) -0.0301(17) 0.0292(18) -0.0250(18) C32 0.0386(19) 0.0337(16) 0.0463(19) -0.0082(14) 0.0354(17) -0.0041(14) _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 Au1 S1 2.2674(8) . ? Au1 Cl1 2.2762(9) . ? S1 P1 2.0351(11) . ? P1 C3 1.851(3) . ? P1 C2 1.873(3) . ? P1 C1 1.885(3) . ? C1 C13' 1.509(12) . ? C1 C12 1.512(4) . ? C1 C11 1.534(4) . ? C1 C13 1.555(4) . ? C1 C12' 1.564(13) . ? C1 C11' 1.605(12) . ? C2 C23' 1.503(12) . ? C2 C21 1.508(4) . ? C2 C22 1.540(4) . ? C2 C23 1.553(4) . ? C2 C22' 1.586(11) . ? C2 C21' 1.612(12) . ? C3 C32 1.516(4) . ? C3 C31 1.521(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 S1 Au1 Cl1 174.71(3) . . ? P1 S1 Au1 107.39(4) . . ? C3 P1 C2 113.13(12) . . ? C3 P1 C1 107.60(12) . . ? C2 P1 C1 113.56(13) . . ? C3 P1 S1 108.67(10) . . ? C2 P1 S1 103.84(9) . . ? C1 P1 S1 109.91(9) . . ? C13' C1 C12 123.1(8) . . ? C13' C1 C11 79.3(9) . . ? C12 C1 C11 110.8(3) . . ? C13' C1 C13 27.4(9) . . ? C12 C1 C13 108.7(3) . . ? C11 C1 C13 106.5(3) . . ? C13' C1 C12' 108.0(11) . . ? C12 C1 C12' 19.9(8) . . ? C11 C1 C12' 124.1(9) . . ? C13 C1 C12' 89.8(9) . . ? C13' C1 C11' 105.1(11) . . ? C12 C1 C11' 83.2(9) . . ? C11 C1 C11' 30.4(8) . . ? C13 C1 C11' 129.8(8) . . ? C12' C1 C11' 100.2(11) . . ? C13' C1 P1 115.4(8) . . ? C12 C1 P1 112.9(2) . . ? C11 C1 P1 109.5(2) . . ? C13 C1 P1 108.1(2) . . ? C12' C1 P1 115.3(9) . . ? C11' C1 P1 111.3(7) . . ? C23' C2 C21 120.4(9) . . ? C23' C2 C22 86.4(9) . . ? C21 C2 C22 111.9(3) . . ? C23' C2 C23 20.6(8) . . ? C21 C2 C23 108.9(3) . . ? C22 C2 C23 106.8(3) . . ? C23' C2 C22' 109.9(10) . . ? C21 C2 C22' 80.9(7) . . ? C22 C2 C22' 32.2(7) . . ? C23 C2 C22' 127.5(6) . . ? C23' C2 C21' 103.8(10) . . ? C21 C2 C21' 21.0(7) . . ? C22 C2 C21' 127.0(8) . . ? C23 C2 C21' 89.3(7) . . ? C22' C2 C21' 98.9(9) . . ? C23' C2 P1 115.4(9) . . ? C21 C2 P1 109.6(2) . . ? C22 C2 P1 110.9(2) . . ? C23 C2 P1 108.6(2) . . ? C22' C2 P1 116.2(6) . . ? C21' C2 P1 110.7(7) . . ? C32 C3 C31 110.4(2) . . ? C32 C3 P1 113.99(19) . . ? C31 C3 P1 117.4(2) . . ? _diffrn_measured_fraction_theta_max 0.943 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 1.354 _refine_diff_density_min -1.240 _refine_diff_density_rms 0.131 _iucr_refine_instructions_details ; TITL Emma in C2/c REM C2/c (#15 in standard setting) CELL 0.71073 26.952558 8.122620 18.689686 90.0000 132.0347 90.0000 ZERR 8.00 0.003 0.0004 0.002 0.0000 0.02 0.0000 LATT 7 SYMM -x, y,-z+1/2 SFAC C H P S Cl Au UNIT 88.00 200.00 8.00 8.00 8.00 8.00 L.S. 4 BOND FMAP 2 PLAN 10 TEMP -173 SIZE 0.3 0.2 0.02 ACTA 60 WGHT 0.015500 6.086000 FVAR 1.13910 0.84342 0.80832 AU1 6 0.328870 0.544663 0.967415 11.00000 0.01700 0.02399 = 0.01309 -0.00284 0.00780 -0.00739 CL1 5 0.423084 0.387958 1.055162 11.00000 0.02023 0.03465 = 0.02278 0.00178 0.01045 -0.00201 S1 4 0.241180 0.720885 0.888239 11.00000 0.02217 0.01920 = 0.01659 -0.00638 0.00799 -0.00735 P1 3 0.158264 0.593929 0.777765 11.00000 0.01753 0.01582 = 0.01373 -0.00435 0.00838 -0.00415 SADI C1 C11 C1 C12 C1 C13 SAME C1 C11' C12' C13' SADI C11 C12 C11 C13 C12 C13 SIMU C1 > C13' 0.02 0.04 0.9 C1 1 0.139079 0.428409 0.826846 11.00000 0.02460 0.02031 = 0.02187 -0.00478 0.01528 -0.00641 Part 1 21 C11 1 0.155910 0.490886 0.918438 21.00000 0.04479 0.02850 = 0.02619 -0.00534 0.02685 -0.00828 AFIX 137 H11A 2 0.127252 0.584954 0.902420 21.00000 -1.50000 H11B 2 0.202836 0.525047 0.965415 21.00000 -1.50000 H11C 2 0.148395 0.402567 0.945985 21.00000 -1.50000 AFIX 0 C12 1 0.067537 0.369282 0.754020 21.00000 0.02032 0.03144 = 0.03301 -0.00256 0.01715 -0.00716 AFIX 137 H12A 2 0.057646 0.331673 0.695786 21.00000 -1.50000 H12B 2 0.037411 0.459827 0.737566 21.00000 -1.50000 H12C 2 0.061190 0.278026 0.781512 21.00000 -1.50000 AFIX 0 C13 1 0.186257 0.280022 0.857794 21.00000 0.02460 0.02046 = 0.02629 -0.00174 0.01607 -0.00568 AFIX 137 H13A 2 0.181231 0.198473 0.891209 21.00000 -1.50000 H13B 2 0.232638 0.318469 0.901095 21.00000 -1.50000 H13C 2 0.174627 0.229629 0.800579 21.00000 -1.50000 AFIX 0 Part 2 -21 C11' 1 0.115101 0.506287 0.878332 -21.00000 0.02753 AFIX 33 H11D 2 0.071562 0.559434 0.829880 -21.00000 -1.50000 H11E 2 0.147824 0.588067 0.925984 -21.00000 -1.50000 H11F 2 0.111279 0.418906 0.910565 -21.00000 -1.50000 AFIX 0 C12' 1 0.077424 0.317636 0.749343 -21.00000 0.02443 AFIX 33 H12D 2 0.066974 0.247663 0.780475 -21.00000 -1.50000 H12E 2 0.087789 0.248294 0.717901 -21.00000 -1.50000 H12F 2 0.038876 0.387535 0.701086 -21.00000 -1.50000 AFIX 0 C13' 1 0.196777 0.317078 0.901569 -21.00000 0.02812 AFIX 33 H13D 2 0.181705 0.233369 0.921153 -21.00000 -1.50000 H13E 2 0.232657 0.382418 0.957805 -21.00000 -1.50000 H13F 2 0.213431 0.263162 0.874267 -21.00000 -1.50000 AFIX 0 Part 0 SADI C2 C21 C2 C22 C2 C23 SAME C2 C21' C22' C23' SADI C21 C22 C21 C23 C22 C23 SIMU C2 > C23' 0.02 0.04 0.9 C2 1 0.091997 0.756001 0.707418 11.00000 0.01943 0.01821 = 0.01886 -0.00273 0.00902 0.00043 Part 1 31 C21 1 0.073538 0.814291 0.763624 31.00000 0.02508 0.03282 = 0.03263 -0.00116 0.02146 0.00406 AFIX 137 H21A 2 0.113860 0.850692 0.827736 31.00000 -1.50000 H21B 2 0.052723 0.723790 0.770084 31.00000 -1.50000 H21C 2 0.042036 0.906264 0.729570 31.00000 -1.50000 AFIX 0 C22 1 0.030817 0.691812 0.606928 31.00000 0.02044 0.02590 = 0.02089 -0.00233 0.00644 0.00253 AFIX 137 H22A 2 0.015081 0.589291 0.613645 31.00000 -1.50000 H22B 2 0.043325 0.671033 0.569121 31.00000 -1.50000 H22C 2 -0.004892 0.774259 0.574060 31.00000 -1.50000 AFIX 0 C23 1 0.120180 0.903752 0.691420 31.00000 0.03124 0.01916 = 0.02816 0.00395 0.01993 0.00606 AFIX 137 H23A 2 0.084857 0.985654 0.650172 31.00000 -1.50000 H23B 2 0.136228 0.865045 0.660322 31.00000 -1.50000 H23C 2 0.157243 0.953813 0.753669 31.00000 -1.50000 AFIX 0 Part 2 -31 C21' 1 0.091575 0.869224 0.777840 -31.00000 0.02809 AFIX 33 H21D 2 0.056351 0.952479 0.739732 -31.00000 -1.50000 H21E 2 0.134974 0.923801 0.824847 -31.00000 -1.50000 H21F 2 0.083144 0.800229 0.811756 -31.00000 -1.50000 AFIX 0 C22' 1 0.017058 0.692892 0.637611 -31.00000 0.02981 AFIX 33 H22D 2 0.008080 0.643242 0.675754 -31.00000 -1.50000 H22E 2 0.010103 0.610565 0.593294 -31.00000 -1.50000 H22F 2 -0.013312 0.785873 0.600651 -31.00000 -1.50000 AFIX 0 C23' 1 0.100433 0.877461 0.655572 -31.00000 0.03268 AFIX 33 H23D 2 0.069741 0.970053 0.632962 -31.00000 -1.50000 H23E 2 0.090529 0.823466 0.600333 -31.00000 -1.50000 H23F 2 0.146531 0.918058 0.699617 -31.00000 -1.50000 AFIX 0 Part 0 C3 1 0.175470 0.491401 0.707903 11.00000 0.02526 0.02035 = 0.01705 -0.00395 0.01299 -0.00077 AFIX 13 H3 2 0.212812 0.413391 0.754621 11.00000 -1.20000 AFIX 0 C31 1 0.120664 0.383433 0.623786 11.00000 0.04185 0.06055 = 0.03636 -0.03014 0.02920 -0.02503 AFIX 137 H31A 2 0.082599 0.452266 0.573167 11.00000 -1.50000 H31B 2 0.106301 0.303010 0.645850 11.00000 -1.50000 H31C 2 0.137775 0.325448 0.598136 11.00000 -1.50000 AFIX 0 C32 1 0.203426 0.605259 0.678025 11.00000 0.03856 0.03366 = 0.04633 -0.00824 0.03540 -0.00406 AFIX 137 H32A 2 0.223107 0.539667 0.658396 11.00000 -1.50000 H32B 2 0.237836 0.675888 0.732436 11.00000 -1.50000 H32C 2 0.167407 0.673822 0.623929 11.00000 -1.50000 HKLF 4 ; data_jens _database_code_depnum_ccdc_archive 'CCDC 925373' #TrackingRef '1b_Jens.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C11 H25 Au Cl P Se' _chemical_formula_weight 499.66 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 7.64505(10) _cell_length_b 14.6437(2) _cell_length_c 13.7211(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.4954(12) _cell_angle_gamma 90.00 _cell_volume 1536.05(4) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 24794 _cell_measurement_theta_min 2.6590 _cell_measurement_theta_max 30.8179 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.161 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 944 _exptl_absorpt_coefficient_mu 12.198 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.17806 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffration Xcalibur, Eos' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 16.1419 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 63823 _diffrn_reflns_av_R_equivalents 0.0472 _diffrn_reflns_av_sigmaI/netI 0.0198 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.66 _diffrn_reflns_theta_max 30.03 _reflns_number_total 4481 _reflns_number_gt 4137 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker XP' _computing_publication_material SHELXL-97 _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^)+(0.0213P)^2^+1.8794P] 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 4481 _refine_ls_number_parameters 144 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0243 _refine_ls_R_factor_gt 0.0209 _refine_ls_wR_factor_ref 0.0466 _refine_ls_wR_factor_gt 0.0452 _refine_ls_goodness_of_fit_ref 1.080 _refine_ls_restrained_S_all 1.080 _refine_ls_shift/su_max 0.002 _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 Au1 Au 0.127027(12) 0.621412(7) 0.589735(7) 0.01643(4) Uani 1 1 d . . . Cl1 Cl 0.15334(9) 0.77263(5) 0.55002(5) 0.02254(13) Uani 1 1 d . . . Se1 Se 0.08347(3) 0.462952(18) 0.616878(19) 0.01730(6) Uani 1 1 d . . . P1 P 0.26433(8) 0.42241(4) 0.73501(5) 0.01009(11) Uani 1 1 d . . . C1 C 0.4922(3) 0.41786(18) 0.6861(2) 0.0174(5) Uani 1 1 d . . . C2 C 0.2385(3) 0.49682(17) 0.84532(19) 0.0155(5) Uani 1 1 d . . . C3 C 0.1823(4) 0.30859(17) 0.7718(2) 0.0184(5) Uani 1 1 d . . . H3 H 0.0869 0.3214 0.8193 0.022 Uiso 1 1 calc R . . C11 C 0.4952(5) 0.3404(2) 0.6098(3) 0.0322(8) Uani 1 1 d . . . H11A H 0.4022 0.3506 0.5614 0.048 Uiso 1 1 calc R . . H11B H 0.4764 0.2817 0.6423 0.048 Uiso 1 1 calc R . . H11C H 0.6088 0.3398 0.5773 0.048 Uiso 1 1 calc R . . C12 C 0.6286(4) 0.3994(3) 0.7662(3) 0.0355(8) Uani 1 1 d . . . H12A H 0.7446 0.3938 0.7369 0.053 Uiso 1 1 calc R . . H12B H 0.5994 0.3426 0.8000 0.053 Uiso 1 1 calc R . . H12C H 0.6290 0.4501 0.8128 0.053 Uiso 1 1 calc R . . C13 C 0.5390(3) 0.50710(19) 0.6343(2) 0.0197(5) Uani 1 1 d . . . H13A H 0.5412 0.5572 0.6817 0.030 Uiso 1 1 calc R . . H13B H 0.4514 0.5201 0.5836 0.030 Uiso 1 1 calc R . . H13C H 0.6545 0.5012 0.6045 0.030 Uiso 1 1 calc R . . C21 C 0.3334(4) 0.58834(19) 0.8331(2) 0.0229(6) Uani 1 1 d . . . H21A H 0.2990 0.6160 0.7708 0.034 Uiso 1 1 calc R . . H21B H 0.4601 0.5781 0.8340 0.034 Uiso 1 1 calc R . . H21C H 0.3019 0.6293 0.8865 0.034 Uiso 1 1 calc R . . C22 C 0.0418(3) 0.51501(18) 0.8594(2) 0.0186(5) Uani 1 1 d . . . H22A H 0.0252 0.5530 0.9174 0.028 Uiso 1 1 calc R . . H22B H -0.0196 0.4568 0.8677 0.028 Uiso 1 1 calc R . . H22C H -0.0052 0.5468 0.8020 0.028 Uiso 1 1 calc R . . C23 C 0.3049(4) 0.4494(2) 0.9383(2) 0.0253(6) Uani 1 1 d . . . H23A H 0.4266 0.4303 0.9294 0.038 Uiso 1 1 calc R . . H23B H 0.2324 0.3956 0.9515 0.038 Uiso 1 1 calc R . . H23C H 0.2980 0.4918 0.9933 0.038 Uiso 1 1 calc R . . C31 C 0.0945(5) 0.2534(2) 0.6900(3) 0.0342(8) Uani 1 1 d . . . H31A H 0.1831 0.2334 0.6435 0.051 Uiso 1 1 calc R . . H31B H 0.0077 0.2917 0.6565 0.051 Uiso 1 1 calc R . . H31C H 0.0364 0.1999 0.7179 0.051 Uiso 1 1 calc R . . C32 C 0.3123(5) 0.2469(2) 0.8274(3) 0.0337(8) Uani 1 1 d . . . H32A H 0.2493 0.1954 0.8562 0.051 Uiso 1 1 calc R . . H32B H 0.3698 0.2823 0.8792 0.051 Uiso 1 1 calc R . . H32C H 0.4006 0.2239 0.7823 0.051 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 Au1 0.01691(6) 0.02025(6) 0.01215(6) 0.00362(3) 0.00191(4) 0.00498(3) Cl1 0.0319(4) 0.0190(3) 0.0168(3) 0.0006(2) 0.0044(3) 0.0055(3) Se1 0.01545(12) 0.02294(13) 0.01344(13) 0.00283(10) -0.00413(9) -0.00408(9) P1 0.0106(3) 0.0092(3) 0.0105(3) 0.0001(2) 0.0014(2) -0.0002(2) C1 0.0109(11) 0.0207(13) 0.0208(14) 0.0050(10) 0.0050(9) 0.0035(9) C2 0.0186(12) 0.0166(12) 0.0113(12) -0.0033(9) 0.0017(9) -0.0044(9) C3 0.0243(13) 0.0102(11) 0.0208(14) 0.0022(10) 0.0074(10) -0.0014(9) C11 0.0384(18) 0.0190(14) 0.040(2) -0.0013(13) 0.0241(15) 0.0063(12) C12 0.0126(13) 0.058(2) 0.0360(19) 0.0213(17) 0.0029(12) 0.0079(13) C13 0.0161(12) 0.0211(13) 0.0220(14) 0.0017(11) 0.0070(10) -0.0034(10) C21 0.0310(15) 0.0192(13) 0.0187(14) -0.0059(11) 0.0047(11) -0.0113(11) C22 0.0211(13) 0.0151(12) 0.0196(13) -0.0027(10) 0.0083(10) 0.0019(9) C23 0.0248(14) 0.0365(17) 0.0146(13) 0.0033(12) -0.0019(11) -0.0061(12) C31 0.053(2) 0.0176(14) 0.0325(18) -0.0083(13) 0.0122(15) -0.0158(14) C32 0.0386(18) 0.0179(14) 0.045(2) 0.0163(14) 0.0179(15) 0.0131(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 Au1 Cl1 2.2897(7) . ? Au1 Se1 2.3741(3) . ? Se1 P1 2.2029(7) . ? P1 C3 1.852(3) . ? P1 C1 1.874(3) . ? P1 C2 1.877(3) . ? C1 C13 1.531(4) . ? C1 C12 1.532(4) . ? C1 C11 1.544(4) . ? C2 C21 1.534(4) . ? C2 C23 1.535(4) . ? C2 C22 1.541(4) . ? C3 C31 1.533(4) . ? C3 C32 1.540(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 Cl1 Au1 Se1 174.456(19) . . ? P1 Se1 Au1 106.911(19) . . ? C3 P1 C1 112.55(12) . . ? C3 P1 C2 105.34(12) . . ? C1 P1 C2 114.48(12) . . ? C3 P1 Se1 103.37(9) . . ? C1 P1 Se1 109.00(9) . . ? C2 P1 Se1 111.54(9) . . ? C13 C1 C12 108.8(2) . . ? C13 C1 C11 107.9(2) . . ? C12 C1 C11 110.1(3) . . ? C13 C1 P1 110.95(17) . . ? C12 C1 P1 112.2(2) . . ? C11 C1 P1 106.75(19) . . ? C21 C2 C23 109.5(2) . . ? C21 C2 C22 109.0(2) . . ? C23 C2 C22 106.9(2) . . ? C21 C2 P1 111.44(18) . . ? C23 C2 P1 111.77(19) . . ? C22 C2 P1 108.12(17) . . ? C31 C3 C32 109.3(3) . . ? C31 C3 P1 115.0(2) . . ? C32 C3 P1 116.4(2) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 30.03 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.740 _refine_diff_density_min -1.794 _refine_diff_density_rms 0.143 _iucr_refine_instructions_details ; TITL Jens in P2(1)/c REM P2(1)/c (#14 in standard setting) CELL 0.71073 7.645053 14.643742 13.721069 90.0000 90.4954 90.0000 ZERR 4.00 0.0001 0.0002 0.0002 0.0000 0.0012 0.0000 LATT 1 SYMM -x, y+1/2,-z+1/2 SFAC C H P Cl Se Au UNIT 44.00 100.00 4.00 4.00 4.00 4.00 L.S. 4 BOND FMAP 2 PLAN 10 TEMP -173 SIZE 0.3 0.2 0.08 SHEL 999 0.71 ACTA WGHT 0.021300 1.879400 FVAR 2.03784 AU1 6 0.127027 0.621412 0.589735 11.00000 0.01691 0.02025 = 0.01215 0.00362 0.00191 0.00498 CL1 4 0.153337 0.772632 0.550021 11.00000 0.03185 0.01900 = 0.01684 0.00064 0.00441 0.00555 SE1 5 0.083475 0.462952 0.616878 11.00000 0.01545 0.02294 = 0.01344 0.00283 -0.00413 -0.00408 P1 3 0.264328 0.422407 0.735013 11.00000 0.01060 0.00916 = 0.01053 0.00015 0.00135 -0.00018 C1 1 0.492242 0.417864 0.686076 11.00000 0.01085 0.02071 = 0.02083 0.00497 0.00501 0.00350 C2 1 0.238464 0.496819 0.845322 11.00000 0.01857 0.01662 = 0.01129 -0.00326 0.00174 -0.00443 C3 1 0.182338 0.308586 0.771777 11.00000 0.02433 0.01020 = 0.02079 0.00220 0.00740 -0.00143 AFIX 13 H3 2 0.086938 0.321442 0.819257 11.00000 -1.20000 AFIX 0 C11 1 0.495194 0.340405 0.609769 11.00000 0.03837 0.01896 = 0.03966 -0.00134 0.02411 0.00627 AFIX 137 H11A 2 0.402237 0.350573 0.561351 11.00000 -1.50000 H11B 2 0.476389 0.281664 0.642256 11.00000 -1.50000 H11C 2 0.608829 0.339813 0.577266 11.00000 -1.50000 AFIX 0 C12 1 0.628604 0.399421 0.766170 11.00000 0.01255 0.05801 = 0.03597 0.02127 0.00294 0.00787 AFIX 137 H12A 2 0.744593 0.393818 0.736908 11.00000 -1.50000 H12B 2 0.599436 0.342557 0.800002 11.00000 -1.50000 H12C 2 0.629000 0.450091 0.812828 11.00000 -1.50000 AFIX 0 C13 1 0.539029 0.507102 0.634316 11.00000 0.01614 0.02112 = 0.02199 0.00165 0.00695 -0.00341 AFIX 137 H13A 2 0.541170 0.557166 0.681708 11.00000 -1.50000 H13B 2 0.451386 0.520060 0.583640 11.00000 -1.50000 H13C 2 0.654478 0.501196 0.604473 11.00000 -1.50000 AFIX 0 C21 1 0.333434 0.588343 0.833067 11.00000 0.03100 0.01915 = 0.01874 -0.00586 0.00468 -0.01135 AFIX 137 H21A 2 0.298992 0.616043 0.770779 11.00000 -1.50000 H21B 2 0.460114 0.578098 0.834044 11.00000 -1.50000 H21C 2 0.301860 0.629349 0.886548 11.00000 -1.50000 AFIX 0 C22 1 0.041804 0.515006 0.859385 11.00000 0.02115 0.01511 = 0.01962 -0.00272 0.00826 0.00194 AFIX 137 H22A 2 0.025177 0.552967 0.917391 11.00000 -1.50000 H22B 2 -0.019619 0.456818 0.867671 11.00000 -1.50000 H22C 2 -0.005241 0.546800 0.802037 11.00000 -1.50000 AFIX 0 C23 1 0.304871 0.449354 0.938290 11.00000 0.02484 0.03651 = 0.01463 0.00335 -0.00190 -0.00613 AFIX 137 H23A 2 0.426599 0.430325 0.929440 11.00000 -1.50000 H23B 2 0.232422 0.395616 0.951454 11.00000 -1.50000 H23C 2 0.297982 0.491823 0.993323 11.00000 -1.50000 AFIX 0 C31 1 0.094470 0.253414 0.690039 11.00000 0.05284 0.01759 = 0.03249 -0.00834 0.01219 -0.01585 AFIX 137 H31A 2 0.183110 0.233397 0.643499 11.00000 -1.50000 H31B 2 0.007746 0.291662 0.656450 11.00000 -1.50000 H31C 2 0.036367 0.199904 0.717899 11.00000 -1.50000 AFIX 0 C32 1 0.312321 0.246943 0.827425 11.00000 0.03864 0.01791 = 0.04481 0.01633 0.01790 0.01310 AFIX 137 H32A 2 0.249276 0.195433 0.856194 11.00000 -1.50000 H32B 2 0.369796 0.282280 0.879215 11.00000 -1.50000 H32C 2 0.400597 0.223896 0.782274 11.00000 -1.50000 HKLF 4 ; data_rudi _database_code_depnum_ccdc_archive 'CCDC 925374' #TrackingRef '1d_Rudi.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C10 H23 Au Cl P Se' _chemical_formula_weight 485.63 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.2215(2) _cell_length_b 11.3519(3) _cell_length_c 15.2400(4) _cell_angle_alpha 90.00 _cell_angle_beta 92.389(4) _cell_angle_gamma 90.00 _cell_volume 1421.11(6) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9950 _cell_measurement_theta_min 2.2333 _cell_measurement_theta_max 30.6703 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.270 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 912 _exptl_absorpt_coefficient_mu 13.181 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.36833 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Xcalibur, Eos' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 16.1419 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 36734 _diffrn_reflns_av_R_equivalents 0.0381 _diffrn_reflns_av_sigmaI/netI 0.0213 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.24 _diffrn_reflns_theta_max 30.02 _reflns_number_total 4103 _reflns_number_gt 3360 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker XP' _computing_publication_material SHELXL-97 _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^)+(0.0129P)^2^+2.1815P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00065(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4103 _refine_ls_number_parameters 135 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0301 _refine_ls_R_factor_gt 0.0206 _refine_ls_wR_factor_ref 0.0431 _refine_ls_wR_factor_gt 0.0402 _refine_ls_goodness_of_fit_ref 1.068 _refine_ls_restrained_S_all 1.068 _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 Au Au 0.984242(12) 0.001438(10) 0.706909(7) 0.01254(4) Uani 1 1 d . . . Se Se 0.80002(4) 0.00672(2) 0.58319(2) 0.01569(6) Uani 1 1 d . . . Cl Cl 1.16671(9) -0.01630(6) 0.82363(5) 0.01805(14) Uani 1 1 d . . . P P 0.70380(8) 0.18698(6) 0.58570(5) 0.00985(14) Uani 1 1 d . . . C1 C 0.8636(3) 0.3032(2) 0.59398(19) 0.0133(5) Uani 1 1 d . . . C2 C 0.5568(3) 0.2041(3) 0.67300(19) 0.0146(6) Uani 1 1 d . . . H2 H 0.5246 0.2889 0.6751 0.018 Uiso 1 1 calc R . . C3 C 0.5831(3) 0.1950(3) 0.48104(18) 0.0148(6) Uani 1 1 d . . . H3 H 0.5146 0.1221 0.4795 0.018 Uiso 1 1 calc R . . C11 C 0.7903(4) 0.4209(3) 0.5622(2) 0.0178(6) Uani 1 1 d . . . H11A H 0.8709 0.4838 0.5716 0.027 Uiso 1 1 calc R . . H11B H 0.6936 0.4387 0.5953 0.027 Uiso 1 1 calc R . . H11C H 0.7596 0.4154 0.4995 0.027 Uiso 1 1 calc R . . C12 C 1.0073(3) 0.2699(3) 0.5373(2) 0.0204(6) Uani 1 1 d . . . H12A H 1.0894 0.3325 0.5408 0.031 Uiso 1 1 calc R . . H12B H 0.9683 0.2600 0.4761 0.031 Uiso 1 1 calc R . . H12C H 1.0558 0.1960 0.5589 0.031 Uiso 1 1 calc R . . C13 C 0.9279(4) 0.3178(3) 0.68885(19) 0.0173(6) Uani 1 1 d . . . H13A H 0.9572 0.2405 0.7133 0.026 Uiso 1 1 calc R . . H13B H 0.8435 0.3536 0.7237 0.026 Uiso 1 1 calc R . . H13C H 1.0243 0.3687 0.6903 0.026 Uiso 1 1 calc R . . C21 C 0.4034(4) 0.1316(3) 0.6518(2) 0.0277(8) Uani 1 1 d . . . H21A H 0.4316 0.0478 0.6500 0.041 Uiso 1 1 calc R . . H21B H 0.3557 0.1558 0.5946 0.041 Uiso 1 1 calc R . . H21C H 0.3244 0.1448 0.6972 0.041 Uiso 1 1 calc R . . C22 C 0.6215(4) 0.1686(3) 0.76448(19) 0.0200(6) Uani 1 1 d . . . H22A H 0.5349 0.1770 0.8063 0.030 Uiso 1 1 calc R . . H22B H 0.7132 0.2196 0.7824 0.030 Uiso 1 1 calc R . . H22C H 0.6580 0.0865 0.7635 0.030 Uiso 1 1 calc R . . C31 C 0.6862(4) 0.1870(3) 0.39964(19) 0.0204(6) Uani 1 1 d . . . H31A H 0.6152 0.1717 0.3476 0.031 Uiso 1 1 calc R . . H31B H 0.7652 0.1228 0.4073 0.031 Uiso 1 1 calc R . . H31C H 0.7442 0.2615 0.3920 0.031 Uiso 1 1 calc R . . C32 C 0.4615(3) 0.2976(3) 0.4722(2) 0.0181(6) Uani 1 1 d . . . H32A H 0.5161 0.3668 0.4486 0.027 Uiso 1 1 calc R . . H32B H 0.4207 0.3166 0.5301 0.027 Uiso 1 1 calc R . . H32C H 0.3702 0.2750 0.4324 0.027 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Au 0.01312(6) 0.01068(6) 0.01382(6) 0.00166(4) 0.00048(4) 0.00204(4) Se 0.01909(14) 0.00999(13) 0.01759(15) -0.00247(11) -0.00411(11) 0.00313(11) Cl 0.0184(3) 0.0190(3) 0.0165(3) 0.0028(3) -0.0025(3) 0.0009(3) P 0.0106(3) 0.0094(3) 0.0095(3) -0.0001(3) -0.0005(3) 0.0000(3) C1 0.0131(13) 0.0122(13) 0.0144(14) -0.0002(11) -0.0005(11) -0.0014(10) C2 0.0144(13) 0.0144(13) 0.0153(15) 0.0029(11) 0.0044(11) 0.0028(11) C3 0.0154(14) 0.0174(14) 0.0111(14) -0.0015(11) -0.0053(11) -0.0007(11) C11 0.0210(15) 0.0131(14) 0.0192(16) 0.0007(11) -0.0001(12) -0.0011(12) C12 0.0146(14) 0.0233(16) 0.0235(17) -0.0006(13) 0.0029(12) -0.0025(12) C13 0.0170(14) 0.0163(14) 0.0180(15) -0.0003(12) -0.0052(12) -0.0048(11) C21 0.0192(16) 0.039(2) 0.0254(19) 0.0057(15) 0.0054(14) -0.0067(14) C22 0.0236(16) 0.0243(16) 0.0125(15) 0.0014(12) 0.0046(12) 0.0009(13) C31 0.0266(16) 0.0222(16) 0.0120(15) -0.0025(12) -0.0033(12) 0.0032(13) C32 0.0148(14) 0.0205(15) 0.0185(15) 0.0032(12) -0.0043(11) 0.0020(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 Au Cl 2.2876(7) . ? Au Se 2.3695(3) . ? Se P 2.1948(7) . ? P C2 1.844(3) . ? P C3 1.845(3) . ? P C1 1.863(3) . ? C1 C13 1.528(4) . ? C1 C11 1.536(4) . ? C1 C12 1.540(4) . ? C2 C22 1.525(4) . ? C2 C21 1.529(4) . ? C3 C31 1.534(4) . ? C3 C32 1.538(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 Cl Au Se 176.13(2) . . ? P Se Au 103.22(2) . . ? C2 P C3 105.86(13) . . ? C2 P C1 110.98(13) . . ? C3 P C1 112.10(13) . . ? C2 P Se 110.99(10) . . ? C3 P Se 102.24(10) . . ? C1 P Se 114.08(9) . . ? C13 C1 C11 108.7(2) . . ? C13 C1 C12 108.3(2) . . ? C11 C1 C12 109.7(2) . . ? C13 C1 P 110.86(19) . . ? C11 C1 P 109.17(19) . . ? C12 C1 P 110.1(2) . . ? C22 C2 C21 107.7(2) . . ? C22 C2 P 114.7(2) . . ? C21 C2 P 110.5(2) . . ? C31 C3 C32 110.7(2) . . ? C31 C3 P 113.6(2) . . ? C32 C3 P 115.9(2) . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 30.02 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 1.736 _refine_diff_density_min -1.113 _refine_diff_density_rms 0.131 _iucr_refine_instructions_details ; TITL Rudi in P2(1)/n CELL 0.71073 8.221485 11.351928 15.240005 90.0000 92.3888 90.0000 ZERR 4.00 0.0002 0.0003 0.0004 0.0000 0.004 0.0000 LATT 1 SYMM -x+1/2, y+1/2,-z+1/2 SFAC C H P Cl Se Au UNIT 40.00 92.00 4.00 4.00 4.00 4.00 TEMP -173 SIZE 0.35 0.2 0.2 FMAP 2 SHEL 999 0.71 ACTA PLAN 10 L.S. 4 WGHT 0.012900 2.181500 EXTI 0.000645 FVAR 2.33509 AU 6 0.984242 0.001438 0.706909 11.00000 0.01312 0.01068 = 0.01382 0.00166 0.00048 0.00204 SE 5 0.800015 0.006717 0.583191 11.00000 0.01909 0.00999 = 0.01759 -0.00247 -0.00411 0.00313 CL 4 1.166706 -0.016301 0.823635 11.00000 0.01839 0.01902 = 0.01646 0.00283 -0.00250 0.00088 P 3 0.703798 0.186982 0.585701 11.00000 0.01056 0.00936 = 0.00954 -0.00011 -0.00053 0.00004 C1 1 0.863621 0.303244 0.593977 11.00000 0.01314 0.01224 = 0.01436 -0.00020 -0.00051 -0.00144 C2 1 0.556822 0.204088 0.672998 11.00000 0.01442 0.01439 = 0.01533 0.00292 0.00439 0.00283 AFIX 13 H2 2 0.524573 0.288944 0.675133 11.00000 -1.20000 AFIX 0 C3 1 0.583062 0.194955 0.481041 11.00000 0.01536 0.01744 = 0.01110 -0.00151 -0.00527 -0.00072 AFIX 13 H3 2 0.514613 0.122108 0.479492 11.00000 -1.20000 AFIX 0 C11 1 0.790286 0.420931 0.562213 11.00000 0.02105 0.01307 = 0.01922 0.00066 -0.00011 -0.00111 AFIX 137 H11A 2 0.870875 0.483778 0.571559 11.00000 -1.50000 H11B 2 0.693583 0.438715 0.595292 11.00000 -1.50000 H11C 2 0.759602 0.415402 0.499519 11.00000 -1.50000 AFIX 0 C12 1 1.007322 0.269900 0.537299 11.00000 0.01461 0.02335 = 0.02345 -0.00061 0.00292 -0.00253 AFIX 137 H12A 2 1.089383 0.332522 0.540846 11.00000 -1.50000 H12B 2 0.968254 0.259989 0.476112 11.00000 -1.50000 H12C 2 1.055802 0.195963 0.558862 11.00000 -1.50000 AFIX 0 C13 1 0.927921 0.317819 0.688847 11.00000 0.01699 0.01632 = 0.01801 -0.00025 -0.00525 -0.00479 AFIX 137 H13A 2 0.957208 0.240491 0.713340 11.00000 -1.50000 H13B 2 0.843496 0.353634 0.723727 11.00000 -1.50000 H13C 2 1.024310 0.368683 0.690336 11.00000 -1.50000 AFIX 0 C21 1 0.403352 0.131628 0.651783 11.00000 0.01923 0.03879 = 0.02535 0.00567 0.00543 -0.00665 AFIX 137 H21A 2 0.431641 0.047825 0.649989 11.00000 -1.50000 H21B 2 0.355695 0.155782 0.594572 11.00000 -1.50000 H21C 2 0.324384 0.144849 0.697192 11.00000 -1.50000 AFIX 0 C22 1 0.621519 0.168605 0.764477 11.00000 0.02355 0.02430 = 0.01248 0.00142 0.00456 0.00091 AFIX 137 H22A 2 0.534870 0.176992 0.806287 11.00000 -1.50000 H22B 2 0.713218 0.219576 0.782372 11.00000 -1.50000 H22C 2 0.658034 0.086453 0.763541 11.00000 -1.50000 AFIX 0 C31 1 0.686202 0.187008 0.399635 11.00000 0.02661 0.02216 = 0.01201 -0.00247 -0.00332 0.00323 AFIX 137 H31A 2 0.615172 0.171681 0.347650 11.00000 -1.50000 H31B 2 0.765152 0.122766 0.407275 11.00000 -1.50000 H31C 2 0.744163 0.261501 0.391984 11.00000 -1.50000 AFIX 0 C32 1 0.461499 0.297635 0.472223 11.00000 0.01476 0.02052 = 0.01849 0.00319 -0.00427 0.00203 AFIX 137 H32A 2 0.516093 0.366788 0.448634 11.00000 -1.50000 H32B 2 0.420699 0.316579 0.530062 11.00000 -1.50000 H32C 2 0.370230 0.274979 0.432352 11.00000 -1.50000 HKLF 4 ; data_eing _database_code_depnum_ccdc_archive 'CCDC 925375' #TrackingRef '2a_Eing.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C11 H25 Au Cl3 P S' _chemical_formula_weight 523.66 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Au Au -2.0133 8.8022 '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 8.6034(4) _cell_length_b 9.7779(4) _cell_length_c 11.4231(4) _cell_angle_alpha 78.876(3) _cell_angle_beta 71.456(4) _cell_angle_gamma 72.702(4) _cell_volume 864.69(6) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 31596 _cell_measurement_theta_min 2.1901 _cell_measurement_theta_max 30.7543 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.011 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 504 _exptl_absorpt_coefficient_mu 9.164 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.57723 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Xcalibur, Eos' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 16.1419 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 68815 _diffrn_reflns_av_R_equivalents 0.0375 _diffrn_reflns_av_sigmaI/netI 0.0166 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.58 _diffrn_reflns_theta_max 30.82 _reflns_number_total 5155 _reflns_number_gt 4939 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker XP' _computing_publication_material SHELXL-97 _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^)+(0.0168P)^2^+0.7671P] 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 5155 _refine_ls_number_parameters 162 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0175 _refine_ls_R_factor_gt 0.0158 _refine_ls_wR_factor_ref 0.0360 _refine_ls_wR_factor_gt 0.0355 _refine_ls_goodness_of_fit_ref 1.076 _refine_ls_restrained_S_all 1.076 _refine_ls_shift/su_max 0.005 _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 Au1 Au 0.964760(9) 0.850143(7) 0.740716(6) 0.01311(3) Uani 1 1 d . . . Cl1 Cl 1.23243(7) 0.87150(6) 0.71221(5) 0.02010(10) Uani 1 1 d . . . Cl2 Cl 1.03637(8) 0.62179(5) 0.84126(5) 0.02352(11) Uani 1 1 d . . . Cl3 Cl 0.70542(7) 0.81734(5) 0.75814(5) 0.02176(10) Uani 1 1 d . . . S1 S 0.90625(6) 1.08036(5) 0.63464(4) 0.01338(9) Uani 1 1 d . . . P1 P 0.71575(6) 1.22282(5) 0.74712(4) 0.00948(8) Uani 1 1 d . . . C1 C 0.7568(2) 1.2093(2) 0.90129(16) 0.0120(3) Uani 1 1 d . . . C2 C 0.7277(3) 1.3996(2) 0.65054(17) 0.0128(3) Uani 1 1 d . . . C3 C 0.5119(2) 1.1799(2) 0.77290(18) 0.0143(4) Uani 1 1 d . . . H3 H 0.5285 1.0777 0.8116 0.017 Uiso 1 1 calc R . . C11 C 0.7023(3) 1.0771(2) 0.98235(17) 0.0154(4) Uani 1 1 d . . . H11A H 0.7616 0.9913 0.9385 0.023 Uiso 1 1 calc R . . H11B H 0.5797 1.0924 0.9991 0.023 Uiso 1 1 calc R . . H11C H 0.7309 1.0635 1.0610 0.023 Uiso 1 1 calc R . . C12 C 0.9458(2) 1.1884(2) 0.88626(18) 0.0159(4) Uani 1 1 d . . . H12A H 0.9649 1.1743 0.9684 0.024 Uiso 1 1 calc R . . H12B H 0.9814 1.2739 0.8385 0.024 Uiso 1 1 calc R . . H12C H 1.0118 1.1036 0.8423 0.024 Uiso 1 1 calc R . . C13 C 0.6566(3) 1.3445(2) 0.96903(18) 0.0165(4) Uani 1 1 d . . . H13A H 0.6755 1.3304 1.0512 0.025 Uiso 1 1 calc R . . H13B H 0.5355 1.3606 0.9784 0.025 Uiso 1 1 calc R . . H13C H 0.6953 1.4284 0.9205 0.025 Uiso 1 1 calc R . . C21 C 0.8769(3) 1.4485(2) 0.65963(19) 0.0178(4) Uani 1 1 d . . . H21A H 0.9819 1.3731 0.6353 0.027 Uiso 1 1 calc R . . H21B H 0.8575 1.4663 0.7453 0.027 Uiso 1 1 calc R . . H21C H 0.8864 1.5373 0.6041 0.027 Uiso 1 1 calc R . . C22 C 0.5615(3) 1.5154(2) 0.69360(19) 0.0171(4) Uani 1 1 d . . . H22A H 0.5739 1.6092 0.6482 0.026 Uiso 1 1 calc R . . H22B H 0.5362 1.5203 0.7828 0.026 Uiso 1 1 calc R . . H22C H 0.4688 1.4904 0.6772 0.026 Uiso 1 1 calc R . . C23 C 0.7572(3) 1.3834(2) 0.51298(18) 0.0186(4) Uani 1 1 d . . . H23A H 0.7493 1.4783 0.4645 0.028 Uiso 1 1 calc R . . H23B H 0.6711 1.3413 0.5056 0.028 Uiso 1 1 calc R . . H23C H 0.8701 1.3203 0.4813 0.028 Uiso 1 1 calc R . . C31 C 0.4719(3) 1.1790(2) 0.6513(2) 0.0230(4) Uani 1 1 d . . . H31A H 0.3837 1.1278 0.6681 0.035 Uiso 1 1 calc R . . H31B H 0.5746 1.1302 0.5920 0.035 Uiso 1 1 calc R . . H31C H 0.4320 1.2784 0.6163 0.035 Uiso 1 1 calc R . . C32 C 0.3569(3) 1.2650(2) 0.8650(2) 0.0203(4) Uani 1 1 d . . . H32A H 0.3337 1.3673 0.8332 0.031 Uiso 1 1 calc R . . H32B H 0.3800 1.2531 0.9455 0.031 Uiso 1 1 calc R . . H32C H 0.2582 1.2288 0.8750 0.031 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 Au1 0.01587(4) 0.01023(4) 0.01322(4) -0.00402(2) -0.00557(3) 0.00006(3) Cl1 0.0156(2) 0.0205(2) 0.0244(2) -0.00703(18) -0.00742(18) 0.00003(18) Cl2 0.0333(3) 0.0124(2) 0.0271(2) -0.00032(18) -0.0165(2) -0.00150(19) Cl3 0.0194(3) 0.0143(2) 0.0337(3) -0.00532(19) -0.0088(2) -0.00422(18) S1 0.0156(2) 0.0119(2) 0.01046(18) -0.00304(15) -0.00250(16) -0.00037(17) P1 0.0099(2) 0.0090(2) 0.00963(19) -0.00142(15) -0.00347(16) -0.00154(16) C1 0.0120(9) 0.0136(8) 0.0103(7) -0.0026(6) -0.0049(6) -0.0006(7) C2 0.0157(9) 0.0111(8) 0.0113(8) 0.0006(6) -0.0039(7) -0.0040(7) C3 0.0117(9) 0.0121(8) 0.0209(9) 0.0008(7) -0.0074(7) -0.0040(7) C11 0.0185(10) 0.0144(9) 0.0114(8) -0.0003(6) -0.0049(7) -0.0015(7) C12 0.0120(9) 0.0193(9) 0.0175(9) -0.0052(7) -0.0066(7) -0.0008(7) C13 0.0173(10) 0.0166(9) 0.0145(8) -0.0067(7) -0.0040(7) 0.0001(7) C21 0.0197(10) 0.0166(9) 0.0178(9) 0.0000(7) -0.0034(7) -0.0086(8) C22 0.0184(10) 0.0112(8) 0.0204(9) 0.0004(7) -0.0073(8) -0.0011(7) C23 0.0268(11) 0.0169(9) 0.0127(8) 0.0017(7) -0.0065(8) -0.0073(8) C31 0.0242(12) 0.0245(11) 0.0281(11) 0.0023(8) -0.0168(9) -0.0105(9) C32 0.0094(9) 0.0198(10) 0.0282(10) 0.0007(8) -0.0032(8) -0.0026(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Au1 Cl1 2.2881(5) . ? Au1 Cl3 2.2889(5) . ? Au1 Cl2 2.3080(5) . ? Au1 S1 2.3346(5) . ? S1 P1 2.0666(7) . ? P1 C3 1.844(2) . ? P1 C2 1.8741(19) . ? P1 C1 1.8766(18) . ? C1 C12 1.534(3) . ? C1 C11 1.540(3) . ? C1 C13 1.543(3) . ? C2 C21 1.535(3) . ? C2 C22 1.541(3) . ? C2 C23 1.542(3) . ? C3 C31 1.535(3) . ? C3 C32 1.537(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl1 Au1 Cl3 175.765(18) . . ? Cl1 Au1 Cl2 89.44(2) . . ? Cl3 Au1 Cl2 89.35(2) . . ? Cl1 Au1 S1 87.963(19) . . ? Cl3 Au1 S1 93.176(19) . . ? Cl2 Au1 S1 177.233(19) . . ? P1 S1 Au1 111.35(2) . . ? C3 P1 C2 112.67(9) . . ? C3 P1 C1 108.88(9) . . ? C2 P1 C1 113.60(8) . . ? C3 P1 S1 109.17(7) . . ? C2 P1 S1 101.47(6) . . ? C1 P1 S1 110.81(6) . . ? C12 C1 C11 108.33(16) . . ? C12 C1 C13 108.22(16) . . ? C11 C1 C13 108.84(15) . . ? C12 C1 P1 111.17(13) . . ? C11 C1 P1 108.08(13) . . ? C13 C1 P1 112.11(13) . . ? C21 C2 C22 109.54(16) . . ? C21 C2 C23 107.67(16) . . ? C22 C2 C23 108.82(16) . . ? C21 C2 P1 110.44(13) . . ? C22 C2 P1 110.44(13) . . ? C23 C2 P1 109.86(13) . . ? C31 C3 C32 110.93(17) . . ? C31 C3 P1 112.86(14) . . ? C32 C3 P1 116.89(14) . . ? _diffrn_measured_fraction_theta_max 0.948 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 1.560 _refine_diff_density_min -1.068 _refine_diff_density_rms 0.106 _iucr_refine_instructions_details ; TITL Eing in P-1 REM P1 (#1 in standard setting) CELL 0.71073 8.603350 9.777890 11.423091 78.8756 71.4555 72.7017 ZERR 2.00 0.0004 0.0004 0.0004 0.003 0.004 0.004 LATT 1 SFAC C H P S Cl Au UNIT 22.00 50.00 2.00 2.00 6.00 2.00 L.S. 4 FMAP 2 PLAN 10 OMIT 0 1 0 OMIT 2 3 1 TEMP -173 SIZE 0.15 0.15 0.08 ACTA 60 WGHT 0.016800 0.767100 FVAR 4.20273 AU1 6 0.964760 0.850143 0.740716 11.00000 0.01587 0.01023 = 0.01322 -0.00402 -0.00557 0.00006 CL1 5 1.232427 0.871500 0.712211 11.00000 0.01558 0.02050 = 0.02440 -0.00703 -0.00742 0.00003 CL2 5 1.036375 0.621789 0.841262 11.00000 0.03325 0.01243 = 0.02710 -0.00032 -0.01648 -0.00150 CL3 5 0.705423 0.817337 0.758144 11.00000 0.01941 0.01434 = 0.03370 -0.00532 -0.00883 -0.00422 S1 4 0.906247 1.080356 0.634644 11.00000 0.01564 0.01188 = 0.01046 -0.00304 -0.00250 -0.00037 P1 3 0.715749 1.222816 0.747122 11.00000 0.00993 0.00903 = 0.00963 -0.00142 -0.00347 -0.00154 C1 1 0.756794 1.209314 0.901289 11.00000 0.01203 0.01359 = 0.01029 -0.00261 -0.00490 -0.00057 C2 1 0.727718 1.399558 0.650538 11.00000 0.01575 0.01105 = 0.01130 0.00060 -0.00392 -0.00397 C3 1 0.511872 1.179920 0.772902 11.00000 0.01167 0.01209 = 0.02089 0.00078 -0.00739 -0.00397 AFIX 13 H3 2 0.528497 1.077675 0.811600 11.00000 -1.20000 AFIX 0 C11 1 0.702280 1.077103 0.982354 11.00000 0.01848 0.01443 = 0.01142 -0.00027 -0.00495 -0.00148 AFIX 137 H11A 2 0.761564 0.991265 0.938525 11.00000 -1.50000 H11B 2 0.579671 1.092414 0.999138 11.00000 -1.50000 H11C 2 0.730912 1.063487 1.060991 11.00000 -1.50000 AFIX 0 C12 1 0.945799 1.188375 0.886257 11.00000 0.01198 0.01929 = 0.01750 -0.00525 -0.00658 -0.00076 AFIX 137 H12A 2 0.964885 1.174274 0.968370 11.00000 -1.50000 H12B 2 0.981416 1.273857 0.838459 11.00000 -1.50000 H12C 2 1.011834 1.103619 0.842338 11.00000 -1.50000 AFIX 0 C13 1 0.656620 1.344522 0.969032 11.00000 0.01726 0.01658 = 0.01446 -0.00669 -0.00404 0.00008 AFIX 137 H13A 2 0.675510 1.330364 1.051215 11.00000 -1.50000 H13B 2 0.535479 1.360630 0.978405 11.00000 -1.50000 H13C 2 0.695267 1.428420 0.920488 11.00000 -1.50000 AFIX 0 C21 1 0.876852 1.448511 0.659635 11.00000 0.01966 0.01658 = 0.01783 -0.00004 -0.00339 -0.00856 AFIX 137 H21A 2 0.981894 1.373121 0.635324 11.00000 -1.50000 H21B 2 0.857453 1.466332 0.745299 11.00000 -1.50000 H21C 2 0.886438 1.537337 0.604090 11.00000 -1.50000 AFIX 0 C22 1 0.561499 1.515429 0.693595 11.00000 0.01844 0.01119 = 0.02042 0.00037 -0.00735 -0.00112 AFIX 137 H22A 2 0.573875 1.609184 0.648158 11.00000 -1.50000 H22B 2 0.536162 1.520348 0.782838 11.00000 -1.50000 H22C 2 0.468753 1.490443 0.677172 11.00000 -1.50000 AFIX 0 C23 1 0.757250 1.383388 0.512978 11.00000 0.02680 0.01691 = 0.01268 0.00175 -0.00651 -0.00733 AFIX 137 H23A 2 0.749325 1.478306 0.464538 11.00000 -1.50000 H23B 2 0.671100 1.341278 0.505621 11.00000 -1.50000 H23C 2 0.870095 1.320301 0.481334 11.00000 -1.50000 AFIX 0 C31 1 0.471926 1.178998 0.651338 11.00000 0.02423 0.02451 = 0.02810 0.00231 -0.01685 -0.01049 AFIX 137 H31A 2 0.383655 1.127822 0.668071 11.00000 -1.50000 H31B 2 0.574581 1.130231 0.591992 11.00000 -1.50000 H31C 2 0.432041 1.278350 0.616348 11.00000 -1.50000 AFIX 0 C32 1 0.356912 1.264996 0.865012 11.00000 0.00945 0.01977 = 0.02817 0.00073 -0.00323 -0.00263 AFIX 137 H32A 2 0.333711 1.367338 0.833183 11.00000 -1.50000 H32B 2 0.379993 1.253097 0.945545 11.00000 -1.50000 H32C 2 0.258231 1.228797 0.875037 11.00000 -1.50000 HKLF 4 ; data_nils _database_code_depnum_ccdc_archive 'CCDC 925376' #TrackingRef '2b_Nils.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H26 Au Cl6 P Se' _chemical_formula_weight 689.92 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Au Au -2.0133 8.8022 '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 8.5343(2) _cell_length_b 9.7185(3) _cell_length_c 14.0759(4) _cell_angle_alpha 74.398(2) _cell_angle_beta 78.121(2) _cell_angle_gamma 73.257(2) _cell_volume 1066.31(5) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 34566 _cell_measurement_theta_min 2.2408 _cell_measurement_theta_max 30.7647 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.149 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 656 _exptl_absorpt_coefficient_mu 9.424 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.15130 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Xcalibur, Eos' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 16.1419 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 75591 _diffrn_reflns_av_R_equivalents 0.0402 _diffrn_reflns_av_sigmaI/netI 0.0171 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.25 _diffrn_reflns_theta_max 30.03 _reflns_number_total 6107 _reflns_number_gt 5903 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker XP' _computing_publication_material SHELXL-97 _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. The solvent molecule is disordered over two positions. Appropriate restraints were used to improve stability of refinement, but dimensions of disordered solvent should be interpreted with caution. ; _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^)+(0.0174P)^2^+2.3512P] 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 6107 _refine_ls_number_parameters 235 _refine_ls_number_restraints 24 _refine_ls_R_factor_all 0.0212 _refine_ls_R_factor_gt 0.0198 _refine_ls_wR_factor_ref 0.0458 _refine_ls_wR_factor_gt 0.0452 _refine_ls_goodness_of_fit_ref 1.091 _refine_ls_restrained_S_all 1.097 _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 Au1 Au 0.190088(11) 0.764547(9) 0.795877(6) 0.01280(3) Uani 1 1 d . . . Se1 Se 0.31023(3) 0.58178(3) 0.693738(17) 0.01511(5) Uani 1 1 d . . . Cl1 Cl 0.44411(8) 0.78058(7) 0.81290(5) 0.02115(13) Uani 1 1 d . . . Cl2 Cl -0.06581(8) 0.75760(7) 0.77413(5) 0.01900(12) Uani 1 1 d . . . Cl3 Cl 0.06714(8) 0.94493(7) 0.88594(5) 0.02098(12) Uani 1 1 d . . . P1 P 0.43630(7) 0.37535(6) 0.79102(4) 0.00998(11) Uani 1 1 d . . . C1 C 0.4876(3) 0.2413(3) 0.70855(18) 0.0145(4) Uani 1 1 d . . . C2 C 0.2963(3) 0.3256(3) 0.90960(17) 0.0122(4) Uani 1 1 d . . . C3 C 0.6212(3) 0.4055(3) 0.82273(19) 0.0147(5) Uani 1 1 d . . . H3 H 0.5794 0.4926 0.8541 0.018 Uiso 1 1 calc R . . C11 C 0.5491(4) 0.3147(3) 0.6007(2) 0.0232(6) Uani 1 1 d . . . H11A H 0.5867 0.2408 0.5599 0.035 Uiso 1 1 calc R . . H11B H 0.6409 0.3561 0.6010 0.035 Uiso 1 1 calc R . . H11C H 0.4586 0.3936 0.5728 0.035 Uiso 1 1 calc R . . C12 C 0.6250(3) 0.1067(3) 0.7467(2) 0.0197(5) Uani 1 1 d . . . H12A H 0.5908 0.0634 0.8166 0.030 Uiso 1 1 calc R . . H12B H 0.7267 0.1379 0.7411 0.030 Uiso 1 1 calc R . . H12C H 0.6451 0.0334 0.7067 0.030 Uiso 1 1 calc R . . C13 C 0.3344(4) 0.1911(3) 0.7054(2) 0.0201(5) Uani 1 1 d . . . H13A H 0.3615 0.1280 0.6575 0.030 Uiso 1 1 calc R . . H13B H 0.2452 0.2776 0.6849 0.030 Uiso 1 1 calc R . . H13C H 0.2987 0.1357 0.7716 0.030 Uiso 1 1 calc R . . C21 C 0.2967(3) 0.4236(3) 0.97906(18) 0.0154(5) Uani 1 1 d . . . H21A H 0.2227 0.4006 1.0411 0.023 Uiso 1 1 calc R . . H21B H 0.2586 0.5275 0.9463 0.023 Uiso 1 1 calc R . . H21C H 0.4091 0.4052 0.9941 0.023 Uiso 1 1 calc R . . C22 C 0.3539(3) 0.1624(3) 0.96192(19) 0.0164(5) Uani 1 1 d . . . H22A H 0.4674 0.1422 0.9755 0.025 Uiso 1 1 calc R . . H22B H 0.3498 0.0998 0.9188 0.025 Uiso 1 1 calc R . . H22C H 0.2810 0.1414 1.0247 0.025 Uiso 1 1 calc R . . C23 C 0.1177(3) 0.3544(3) 0.8902(2) 0.0173(5) Uani 1 1 d . . . H23A H 0.0470 0.3306 0.9536 0.026 Uiso 1 1 calc R . . H23B H 0.1140 0.2926 0.8464 0.026 Uiso 1 1 calc R . . H23C H 0.0780 0.4585 0.8583 0.026 Uiso 1 1 calc R . . C31 C 0.7423(4) 0.4522(3) 0.7309(2) 0.0240(6) Uani 1 1 d . . . H31A H 0.8169 0.4975 0.7494 0.036 Uiso 1 1 calc R . . H31B H 0.6805 0.5234 0.6794 0.036 Uiso 1 1 calc R . . H31C H 0.8068 0.3654 0.7052 0.036 Uiso 1 1 calc R . . C32 C 0.7134(3) 0.2816(3) 0.9007(2) 0.0192(5) Uani 1 1 d . . . H32A H 0.7567 0.1917 0.8749 0.029 Uiso 1 1 calc R . . H32B H 0.6371 0.2625 0.9622 0.029 Uiso 1 1 calc R . . H32C H 0.8052 0.3116 0.9144 0.029 Uiso 1 1 calc R . . C99 C 0.8899(9) 0.8176(8) 0.5186(5) 0.0273(16) Uani 0.524(4) 1 d PDU A 1 H99 H 0.9442 0.8317 0.5706 0.033 Uiso 0.524(4) 1 calc PR A 1 Cl4 Cl 0.6681(6) 0.8457(4) 0.5622(2) 0.0386(9) Uani 0.524(4) 1 d PDU A 1 Cl5 Cl 0.9374(3) 0.9395(2) 0.40555(12) 0.0433(7) Uani 0.524(4) 1 d PD A 1 Cl6 Cl 0.9692(2) 0.6339(3) 0.50482(14) 0.0419(6) Uani 0.524(4) 1 d PDU A 1 C99' C 0.8331(12) 0.8626(10) 0.5320(7) 0.030(2) Uani 0.476(4) 1 d PU A 2 H99' H 0.8683 0.8817 0.5898 0.036 Uiso 0.476(4) 1 calc PR A 2 Cl4' Cl 0.6570(10) 0.8366(9) 0.5641(6) 0.088(2) Uani 0.476(4) 1 d PU A 2 Cl5' Cl 0.8096(5) 1.0248(3) 0.43816(19) 0.0703(12) Uani 0.476(4) 1 d P A 2 Cl6' Cl 0.9810(3) 0.7175(4) 0.4928(3) 0.0581(8) Uani 0.476(4) 1 d PU A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Au1 0.01411(5) 0.00835(5) 0.01369(5) -0.00097(3) -0.00226(3) -0.00048(3) Se1 0.01998(12) 0.01042(11) 0.01206(11) -0.00108(8) -0.00389(9) 0.00047(9) Cl1 0.0173(3) 0.0139(3) 0.0333(3) -0.0075(2) -0.0038(2) -0.0033(2) Cl2 0.0154(3) 0.0173(3) 0.0222(3) -0.0024(2) -0.0059(2) -0.0003(2) Cl3 0.0215(3) 0.0152(3) 0.0252(3) -0.0090(2) 0.0004(2) -0.0012(2) P1 0.0093(3) 0.0085(3) 0.0116(3) -0.0022(2) -0.0014(2) -0.0015(2) C1 0.0172(11) 0.0120(11) 0.0151(11) -0.0054(9) -0.0015(9) -0.0031(9) C2 0.0099(10) 0.0103(10) 0.0135(10) -0.0002(8) -0.0008(8) -0.0010(8) C3 0.0113(10) 0.0151(11) 0.0203(12) -0.0070(9) -0.0018(9) -0.0047(9) C11 0.0326(15) 0.0221(13) 0.0134(11) -0.0074(10) 0.0026(10) -0.0052(11) C12 0.0188(12) 0.0149(12) 0.0252(13) -0.0096(10) -0.0038(10) 0.0015(10) C13 0.0241(13) 0.0176(12) 0.0227(13) -0.0069(10) -0.0081(10) -0.0059(10) C21 0.0158(11) 0.0150(11) 0.0132(10) -0.0037(9) -0.0006(9) -0.0010(9) C22 0.0162(11) 0.0116(11) 0.0181(11) 0.0016(9) -0.0028(9) -0.0023(9) C23 0.0093(10) 0.0184(12) 0.0220(12) -0.0008(10) -0.0019(9) -0.0036(9) C31 0.0189(13) 0.0280(15) 0.0277(14) -0.0078(12) 0.0044(11) -0.0140(11) C32 0.0110(11) 0.0204(13) 0.0271(13) -0.0085(10) -0.0079(10) 0.0013(9) C99 0.027(4) 0.040(5) 0.017(3) 0.001(3) -0.004(3) -0.018(3) Cl4 0.051(2) 0.0365(13) 0.0264(13) -0.0231(11) -0.0151(13) 0.0132(12) Cl5 0.0655(14) 0.0525(13) 0.0209(7) 0.0107(7) -0.0126(7) -0.0412(11) Cl6 0.0358(9) 0.0414(13) 0.0336(8) -0.0028(8) 0.0074(7) -0.0002(8) C99' 0.038(5) 0.028(4) 0.019(3) -0.005(3) -0.003(3) 0.002(3) Cl4' 0.055(3) 0.122(5) 0.078(4) -0.031(3) -0.011(3) 0.002(3) Cl5' 0.142(3) 0.0371(13) 0.0465(13) 0.0140(10) -0.0562(18) -0.0360(17) Cl6' 0.0432(12) 0.0572(19) 0.0750(18) -0.0432(16) -0.0055(11) 0.0103(13) _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 Au1 Cl1 2.2826(7) . ? Au1 Cl2 2.2889(6) . ? Au1 Cl3 2.3172(6) . ? Au1 Se1 2.4476(3) . ? Se1 P1 2.2232(6) . ? P1 C3 1.844(3) . ? P1 C1 1.874(2) . ? P1 C2 1.877(2) . ? C1 C13 1.533(4) . ? C1 C12 1.540(4) . ? C1 C11 1.548(4) . ? C2 C23 1.537(3) . ? C2 C21 1.538(3) . ? C2 C22 1.540(3) . ? C3 C31 1.532(4) . ? C3 C32 1.540(4) . ? C99 Cl5 1.759(7) . ? C99 Cl6 1.765(8) . ? C99 Cl4 1.830(8) . ? C99' Cl4' 1.551(13) . ? C99' Cl6' 1.730(8) . ? C99' Cl5' 1.754(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl1 Au1 Cl2 177.64(2) . . ? Cl1 Au1 Cl3 89.67(2) . . ? Cl2 Au1 Cl3 89.66(2) . . ? Cl1 Au1 Se1 92.333(18) . . ? Cl2 Au1 Se1 88.235(17) . . ? Cl3 Au1 Se1 176.854(18) . . ? P1 Se1 Au1 107.618(18) . . ? C3 P1 C1 112.97(11) . . ? C3 P1 C2 108.46(11) . . ? C1 P1 C2 114.19(11) . . ? C3 P1 Se1 108.64(9) . . ? C1 P1 Se1 101.79(8) . . ? C2 P1 Se1 110.55(7) . . ? C13 C1 C12 109.9(2) . . ? C13 C1 C11 107.5(2) . . ? C12 C1 C11 108.6(2) . . ? C13 C1 P1 110.79(17) . . ? C12 C1 P1 109.77(17) . . ? C11 C1 P1 110.23(18) . . ? C23 C2 C21 107.9(2) . . ? C23 C2 C22 108.3(2) . . ? C21 C2 C22 109.4(2) . . ? C23 C2 P1 111.36(17) . . ? C21 C2 P1 108.17(17) . . ? C22 C2 P1 111.66(16) . . ? C31 C3 C32 110.6(2) . . ? C31 C3 P1 113.08(18) . . ? C32 C3 P1 116.51(18) . . ? Cl5 C99 Cl6 109.7(4) . . ? Cl5 C99 Cl4 113.5(4) . . ? Cl6 C99 Cl4 108.2(4) . . ? Cl4' C99' Cl6' 114.6(7) . . ? Cl4' C99' Cl5' 104.7(6) . . ? Cl6' C99' Cl5' 112.2(5) . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 30.03 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 1.849 _refine_diff_density_min -1.253 _refine_diff_density_rms 0.118 _iucr_refine_istructions_details ; TITL Nils in P-1 CELL 0.71073 8.534328 9.718549 14.075921 74.3980 78.1212 73.2565 ZERR 2.00 0.0002 0.0003 0.0004 0.002 0.002 0.002 LATT 1 SFAC C H P Cl Se Au UNIT 24.00 52.00 2.00 12.00 2.00 2.00 L.S. 8 BOND FMAP 2 PLAN 10 OMIT 0 8 2 OMIT -3 -4 3 OMIT -1 8 1 OMIT -2 0 18 OMIT 0 10 2 TEMP -173 SIZE 0.4 0.25 0.08 SHEL 999 0.71 ACTA SADI C99 CL4 C99 CL5 C99 CL6 SADI CL4 CL5 CL4 CL6 CL5 CL6 SIMU C99 > CL6' 0.02 0.04 0.9 WGHT 0.017400 2.351200 FVAR 3.65339 0.52396 AU1 6 0.190088 0.764547 0.795877 11.00000 0.01411 0.00835 = 0.01369 -0.00097 -0.00226 -0.00048 SE1 5 0.310232 0.581778 0.693738 11.00000 0.01998 0.01042 = 0.01206 -0.00108 -0.00389 0.00047 CL1 4 0.444111 0.780580 0.812900 11.00000 0.01734 0.01393 = 0.03330 -0.00750 -0.00379 -0.00335 CL2 4 -0.065806 0.757596 0.774126 11.00000 0.01538 0.01727 = 0.02223 -0.00244 -0.00592 -0.00030 CL3 4 0.067139 0.944928 0.885945 11.00000 0.02151 0.01515 = 0.02516 -0.00898 0.00038 -0.00120 P1 3 0.436304 0.375351 0.791021 11.00000 0.00929 0.00854 = 0.01158 -0.00215 -0.00140 -0.00152 C1 1 0.487607 0.241281 0.708552 11.00000 0.01719 0.01198 = 0.01515 -0.00540 -0.00151 -0.00307 C2 1 0.296344 0.325622 0.909601 11.00000 0.00990 0.01028 = 0.01351 -0.00022 -0.00080 -0.00101 C3 1 0.621206 0.405498 0.822727 11.00000 0.01129 0.01511 = 0.02031 -0.00696 -0.00180 -0.00466 AFIX 13 H3 2 0.579380 0.492582 0.854053 11.00000 -1.20000 AFIX 0 C11 1 0.549093 0.314710 0.600654 11.00000 0.03264 0.02212 = 0.01335 -0.00743 0.00262 -0.00524 AFIX 137 H11A 2 0.586711 0.240840 0.559903 11.00000 -1.50000 H11B 2 0.640907 0.356148 0.600970 11.00000 -1.50000 H11C 2 0.458589 0.393632 0.572776 11.00000 -1.50000 AFIX 0 C12 1 0.625017 0.106738 0.746734 11.00000 0.01883 0.01489 = 0.02521 -0.00960 -0.00377 0.00154 AFIX 137 H12A 2 0.590771 0.063361 0.816620 11.00000 -1.50000 H12B 2 0.726658 0.137870 0.741127 11.00000 -1.50000 H12C 2 0.645062 0.033369 0.706750 11.00000 -1.50000 AFIX 0 C13 1 0.334420 0.191146 0.705366 11.00000 0.02411 0.01763 = 0.02270 -0.00695 -0.00810 -0.00594 AFIX 137 H13A 2 0.361472 0.128006 0.657505 11.00000 -1.50000 H13B 2 0.245214 0.277643 0.684919 11.00000 -1.50000 H13C 2 0.298675 0.135749 0.771636 11.00000 -1.50000 AFIX 0 C21 1 0.296708 0.423627 0.979055 11.00000 0.01583 0.01503 = 0.01315 -0.00374 -0.00056 -0.00104 AFIX 137 H21A 2 0.222712 0.400559 1.041070 11.00000 -1.50000 H21B 2 0.258586 0.527528 0.946259 11.00000 -1.50000 H21C 2 0.409058 0.405223 0.994080 11.00000 -1.50000 AFIX 0 C22 1 0.353853 0.162402 0.961916 11.00000 0.01616 0.01158 = 0.01807 0.00162 -0.00284 -0.00234 AFIX 137 H22A 2 0.467358 0.142212 0.975544 11.00000 -1.50000 H22B 2 0.349830 0.099767 0.918754 11.00000 -1.50000 H22C 2 0.280969 0.141352 1.024745 11.00000 -1.50000 AFIX 0 C23 1 0.117653 0.354420 0.890202 11.00000 0.00932 0.01836 = 0.02202 -0.00079 -0.00193 -0.00364 AFIX 137 H23A 2 0.047028 0.330555 0.953559 11.00000 -1.50000 H23B 2 0.114007 0.292569 0.846403 11.00000 -1.50000 H23C 2 0.078003 0.458495 0.858278 11.00000 -1.50000 AFIX 0 C31 1 0.742262 0.452154 0.730931 11.00000 0.01891 0.02799 = 0.02775 -0.00781 0.00441 -0.01397 AFIX 137 H31A 2 0.816930 0.497520 0.749443 11.00000 -1.50000 H31B 2 0.680486 0.523432 0.679415 11.00000 -1.50000 H31C 2 0.806797 0.365351 0.705223 11.00000 -1.50000 AFIX 0 C32 1 0.713441 0.281555 0.900661 11.00000 0.01099 0.02042 = 0.02714 -0.00851 -0.00786 0.00127 AFIX 137 H32A 2 0.756708 0.191672 0.874893 11.00000 -1.50000 H32B 2 0.637137 0.262518 0.962241 11.00000 -1.50000 H32C 2 0.805163 0.311614 0.914436 11.00000 -1.50000 AFIX 0 PART 1 C99 1 0.889894 0.817589 0.518572 21.00000 0.02697 0.03956 = 0.01702 0.00130 -0.00358 -0.01758 AFIX 13 H99 2 0.944224 0.831672 0.570586 21.00000 -1.20000 AFIX 0 CL4 4 0.668139 0.845690 0.562193 21.00000 0.05124 0.03655 = 0.02638 -0.02311 -0.01511 0.01325 CL5 4 0.937363 0.939457 0.405553 21.00000 0.06554 0.05245 = 0.02087 0.01066 -0.01256 -0.04120 CL6 4 0.969238 0.633949 0.504823 21.00000 0.03578 0.04140 = 0.03363 -0.00279 0.00736 -0.00021 PART 2 C99' 1 0.833109 0.862609 0.531986 -21.00000 0.03802 0.02761 = 0.01861 -0.00518 -0.00279 0.00177 AFIX 13 H99' 2 0.868261 0.881671 0.589793 -21.00000 -1.20000 AFIX 0 CL4' 4 0.656989 0.836579 0.564070 -21.00000 0.05501 0.12200 = 0.07756 -0.03056 -0.01055 0.00180 CL5' 4 0.809583 1.024841 0.438157 -21.00000 0.14198 0.03709 = 0.04650 0.01395 -0.05617 -0.03595 CL6' 4 0.980962 0.717482 0.492751 -21.00000 0.04322 0.05719 = 0.07498 -0.04315 -0.00548 0.01033 PART 0 HKLF4 ; data_philip _database_code_depnum_ccdc_archive 'CCDC 925377' #TrackingRef '2c_Philip.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C10 H23 Au Cl3 P S' _chemical_formula_weight 509.63 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.4533(2) _cell_length_b 17.0563(4) _cell_length_c 11.4826(3) _cell_angle_alpha 90.00 _cell_angle_beta 94.525(2) _cell_angle_gamma 90.00 _cell_volume 1650.43(7) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 16512 _cell_measurement_theta_min 2.1384 _cell_measurement_theta_max 30.7885 _exptl_crystal_description plate _exptl_crystal_colour 'dichroic red-range' _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.051 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 976 _exptl_absorpt_coefficient_mu 9.599 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.19206 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Xcalibur, Eos' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 16.1419 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 40023 _diffrn_reflns_av_R_equivalents 0.0400 _diffrn_reflns_av_sigmaI/netI 0.0242 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.39 _diffrn_reflns_theta_max 30.86 _reflns_number_total 4862 _reflns_number_gt 4482 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker XP' _computing_publication_material SHELXL-97 _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0190P)^2^+1.7388P] 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 4862 _refine_ls_number_parameters 152 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0247 _refine_ls_R_factor_gt 0.0210 _refine_ls_wR_factor_ref 0.0457 _refine_ls_wR_factor_gt 0.0443 _refine_ls_goodness_of_fit_ref 1.072 _refine_ls_restrained_S_all 1.072 _refine_ls_shift/su_max 0.004 _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 Au1 Au 0.537319(11) 0.458112(6) 0.698923(8) 0.01252(3) Uani 1 1 d . . . Cl1 Cl 0.78118(7) 0.49570(4) 0.77945(6) 0.01953(13) Uani 1 1 d . . . Cl2 Cl 0.60148(8) 0.33007(4) 0.74375(6) 0.02142(13) Uani 1 1 d . . . Cl3 Cl 0.29411(8) 0.41591(4) 0.62396(6) 0.01961(13) Uani 1 1 d . . . S1 S 0.49553(7) 0.58842(4) 0.64406(6) 0.01545(12) Uani 1 1 d . . . P1 P 0.29578(8) 0.63290(4) 0.71080(5) 0.01204(12) Uani 1 1 d . . . C1 C 0.2845(3) 0.61053(17) 0.8698(2) 0.0175(5) Uani 1 1 d . . . C2 C 0.3186(3) 0.73938(16) 0.6906(2) 0.0181(5) Uani 1 1 d . . . H2 H 0.2257 0.7652 0.7236 0.022 Uiso 1 1 calc R . . C3 C 0.1136(3) 0.59895(16) 0.6267(2) 0.0135(5) Uani 1 1 d . . . H3 H 0.0868 0.5468 0.6599 0.016 Uiso 1 1 calc R . . C11 C 0.1916(4) 0.6760(2) 0.9271(3) 0.0302(7) Uani 1 1 d . . . H11A H 0.0873 0.6822 0.8844 0.045 Uiso 1 1 calc R . . H11B H 0.2506 0.7253 0.9249 0.045 Uiso 1 1 calc R . . H11C H 0.1778 0.6620 1.0085 0.045 Uiso 1 1 calc R . . C12 C 0.4523(3) 0.60527(18) 0.9315(2) 0.0210(6) Uani 1 1 d . . . H12A H 0.4449 0.5990 1.0158 0.032 Uiso 1 1 calc R . . H12B H 0.5110 0.6533 0.9169 0.032 Uiso 1 1 calc R . . H12C H 0.5079 0.5601 0.9013 0.032 Uiso 1 1 calc R . . C13 C 0.2002(4) 0.53229(19) 0.8846(3) 0.0255(7) Uani 1 1 d . . . H13A H 0.2511 0.4916 0.8404 0.038 Uiso 1 1 calc R . . H13B H 0.0885 0.5371 0.8555 0.038 Uiso 1 1 calc R . . H13C H 0.2069 0.5180 0.9675 0.038 Uiso 1 1 calc R . . C21 C 0.4685(4) 0.77241(18) 0.7570(3) 0.0269(7) Uani 1 1 d . . . H21A H 0.5624 0.7474 0.7286 0.040 Uiso 1 1 calc R . . H21B H 0.4652 0.7618 0.8407 0.040 Uiso 1 1 calc R . . H21C H 0.4737 0.8291 0.7443 0.040 Uiso 1 1 calc R . . C22 C 0.3144(4) 0.76265(18) 0.5614(3) 0.0255(6) Uani 1 1 d . . . H22A H 0.3270 0.8196 0.5551 0.038 Uiso 1 1 calc R . . H22B H 0.2126 0.7469 0.5215 0.038 Uiso 1 1 calc R . . H22C H 0.4010 0.7363 0.5250 0.038 Uiso 1 1 calc R . . C31 C -0.0295(3) 0.65284(17) 0.6416(2) 0.0181(5) Uani 1 1 d . . . H31A H -0.0087 0.7048 0.6097 0.027 Uiso 1 1 calc R . . H31B H -0.0463 0.6576 0.7248 0.027 Uiso 1 1 calc R . . H31C H -0.1244 0.6304 0.5998 0.027 Uiso 1 1 calc R . . C32 C 0.1375(3) 0.58528(16) 0.4971(2) 0.0165(5) Uani 1 1 d . . . H32A H 0.0383 0.5662 0.4570 0.025 Uiso 1 1 calc R . . H32B H 0.2213 0.5463 0.4902 0.025 Uiso 1 1 calc R . . H32C H 0.1681 0.6347 0.4615 0.025 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 Au1 0.01036(5) 0.01403(6) 0.01302(5) -0.00017(3) -0.00001(3) -0.00005(4) Cl1 0.0117(3) 0.0263(4) 0.0201(3) 0.0003(3) -0.0024(2) -0.0019(3) Cl2 0.0212(3) 0.0170(3) 0.0257(3) 0.0029(3) -0.0009(2) 0.0027(3) Cl3 0.0141(3) 0.0168(3) 0.0270(3) -0.0010(3) -0.0045(2) -0.0017(2) S1 0.0124(3) 0.0152(3) 0.0192(3) 0.0019(2) 0.0032(2) -0.0009(2) P1 0.0111(3) 0.0123(3) 0.0124(3) -0.0005(2) -0.0011(2) -0.0007(2) C1 0.0145(12) 0.0266(15) 0.0110(11) -0.0001(10) -0.0020(9) 0.0019(11) C2 0.0157(12) 0.0137(13) 0.0244(13) -0.0023(10) -0.0016(10) -0.0018(10) C3 0.0120(11) 0.0154(12) 0.0128(11) -0.0007(9) -0.0022(8) -0.0020(10) C11 0.0291(16) 0.045(2) 0.0170(13) -0.0052(13) 0.0014(11) 0.0156(15) C12 0.0196(13) 0.0260(15) 0.0165(12) -0.0012(11) -0.0040(10) 0.0014(12) C13 0.0257(15) 0.0346(18) 0.0157(13) 0.0074(12) -0.0006(11) -0.0060(13) C21 0.0222(15) 0.0181(14) 0.0392(17) -0.0049(13) -0.0060(12) -0.0056(12) C22 0.0287(16) 0.0194(15) 0.0284(15) 0.0057(12) 0.0026(12) -0.0053(13) C31 0.0119(12) 0.0204(14) 0.0214(13) -0.0028(10) -0.0020(9) 0.0010(11) C32 0.0185(13) 0.0181(13) 0.0124(11) -0.0005(10) -0.0026(9) -0.0002(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Au1 Cl3 2.2818(6) . ? Au1 Cl1 2.2836(6) . ? Au1 Cl2 2.2989(7) . ? Au1 S1 2.3294(7) . ? S1 P1 2.0538(9) . ? P1 C2 1.843(3) . ? P1 C3 1.845(2) . ? P1 C1 1.875(3) . ? C1 C13 1.529(4) . ? C1 C12 1.537(4) . ? C1 C11 1.542(4) . ? C2 C21 1.534(4) . ? C2 C22 1.534(4) . ? C3 C32 1.535(3) . ? C3 C31 1.539(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 Cl3 Au1 Cl1 177.46(2) . . ? Cl3 Au1 Cl2 88.54(2) . . ? Cl1 Au1 Cl2 89.23(2) . . ? Cl3 Au1 S1 94.93(2) . . ? Cl1 Au1 S1 87.39(2) . . ? Cl2 Au1 S1 174.30(2) . . ? P1 S1 Au1 111.29(3) . . ? C2 P1 C3 109.57(12) . . ? C2 P1 C1 109.68(13) . . ? C3 P1 C1 109.95(12) . . ? C2 P1 S1 102.69(10) . . ? C3 P1 S1 111.45(9) . . ? C1 P1 S1 113.24(9) . . ? C13 C1 C12 108.6(2) . . ? C13 C1 C11 109.1(3) . . ? C12 C1 C11 109.1(2) . . ? C13 C1 P1 110.25(18) . . ? C12 C1 P1 110.19(19) . . ? C11 C1 P1 109.58(19) . . ? C21 C2 C22 109.9(2) . . ? C21 C2 P1 113.0(2) . . ? C22 C2 P1 112.45(19) . . ? C32 C3 C31 111.3(2) . . ? C32 C3 P1 112.75(18) . . ? C31 C3 P1 112.67(18) . . ? _diffrn_measured_fraction_theta_max 0.934 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 2.150 _refine_diff_density_min -1.415 _refine_diff_density_rms 0.135 _iucr_refine_instructions_details ; TITL Philip in P2(1)/n REM P2(1)/n (#14 in standard setting) CELL 0.71073 8.453325 17.056295 11.482596 90.0000 94.5250 90.0000 ZERR 4.00 0.0002 0.0004 0.0003 0.0000 0.002 0.0000 LATT 1 SYMM -x+1/2, y+1/2,-z+1/2 SFAC C H P S Cl Au UNIT 40.00 92.00 4.00 4.00 12.00 4.00 L.S. 4 BOND FMAP 2 PLAN 10 OMIT 2 1 1 OMIT -2 6 3 TEMP -173 SIZE 0.3 0.2 0.02 ACTA 60 OMIT 0 1 1 WGHT 0.019000 1.738800 FVAR 2.12700 AU1 6 0.537319 0.458112 0.698923 11.00000 0.01036 0.01403 = 0.01302 -0.00017 -0.00001 -0.00005 CL1 5 0.781179 0.495704 0.779455 11.00000 0.01171 0.02626 = 0.02006 0.00025 -0.00237 -0.00191 CL2 5 0.601483 0.330069 0.743755 11.00000 0.02115 0.01696 = 0.02570 0.00292 -0.00093 0.00269 CL3 5 0.294110 0.415914 0.623957 11.00000 0.01409 0.01678 = 0.02697 -0.00095 -0.00454 -0.00167 S1 4 0.495529 0.588417 0.644059 11.00000 0.01236 0.01515 = 0.01916 0.00192 0.00322 -0.00094 P1 3 0.295776 0.632896 0.710797 11.00000 0.01107 0.01232 = 0.01240 -0.00049 -0.00106 -0.00069 C1 1 0.284509 0.610528 0.869779 11.00000 0.01447 0.02662 = 0.01101 -0.00005 -0.00195 0.00188 C2 1 0.318631 0.739385 0.690639 11.00000 0.01572 0.01367 = 0.02440 -0.00225 -0.00158 -0.00182 AFIX 13 H2 2 0.225746 0.765189 0.723563 11.00000 -1.20000 AFIX 0 C3 1 0.113613 0.598948 0.626743 11.00000 0.01200 0.01535 = 0.01277 -0.00072 -0.00224 -0.00199 AFIX 13 H3 2 0.086785 0.546830 0.659875 11.00000 -1.20000 AFIX 0 C11 1 0.191595 0.675973 0.927112 11.00000 0.02908 0.04452 = 0.01699 -0.00516 0.00144 0.01564 AFIX 137 H11A 2 0.087313 0.682202 0.884430 11.00000 -1.50000 H11B 2 0.250596 0.725339 0.924876 11.00000 -1.50000 H11C 2 0.177826 0.661970 1.008467 11.00000 -1.50000 AFIX 0 C12 1 0.452263 0.605267 0.931536 11.00000 0.01963 0.02604 = 0.01648 -0.00123 -0.00404 0.00137 AFIX 137 H12A 2 0.444872 0.599012 1.015773 11.00000 -1.50000 H12B 2 0.511000 0.653340 0.916868 11.00000 -1.50000 H12C 2 0.507857 0.560097 0.901338 11.00000 -1.50000 AFIX 0 C13 1 0.200189 0.532292 0.884619 11.00000 0.02571 0.03462 = 0.01570 0.00743 -0.00056 -0.00597 AFIX 137 H13A 2 0.251096 0.491561 0.840377 11.00000 -1.50000 H13B 2 0.088504 0.537142 0.855461 11.00000 -1.50000 H13C 2 0.206910 0.518019 0.967533 11.00000 -1.50000 AFIX 0 C21 1 0.468533 0.772410 0.757031 11.00000 0.02218 0.01806 = 0.03921 -0.00492 -0.00597 -0.00556 AFIX 137 H21A 2 0.562434 0.747356 0.728574 11.00000 -1.50000 H21B 2 0.465208 0.761849 0.840695 11.00000 -1.50000 H21C 2 0.473749 0.829129 0.744252 11.00000 -1.50000 AFIX 0 C22 1 0.314448 0.762652 0.561385 11.00000 0.02875 0.01935 = 0.02838 0.00575 0.00264 -0.00526 AFIX 137 H22A 2 0.327004 0.819577 0.555088 11.00000 -1.50000 H22B 2 0.212623 0.746904 0.521522 11.00000 -1.50000 H22C 2 0.401046 0.736340 0.524972 11.00000 -1.50000 AFIX 0 C31 1 -0.029461 0.652836 0.641582 11.00000 0.01191 0.02043 = 0.02142 -0.00285 -0.00199 0.00102 AFIX 137 H31A 2 -0.008720 0.704795 0.609687 11.00000 -1.50000 H31B 2 -0.046326 0.657596 0.724750 11.00000 -1.50000 H31C 2 -0.124431 0.630428 0.599756 11.00000 -1.50000 AFIX 0 C32 1 0.137482 0.585285 0.497130 11.00000 0.01854 0.01812 = 0.01235 -0.00048 -0.00260 -0.00025 AFIX 137 H32A 2 0.038287 0.566217 0.456984 11.00000 -1.50000 H32B 2 0.221281 0.546251 0.490165 11.00000 -1.50000 H32C 2 0.168112 0.634665 0.461512 11.00000 -1.50000 HKLF 4 ; data_sandra2_hklf5 _database_code_depnum_ccdc_archive 'CCDC 925378' #TrackingRef '2d_Sandra.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C10 H23 Au Cl3 P Se' _chemical_formula_weight 556.53 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Au Au -2.0133 8.8022 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 7.9388(2) _cell_length_b 14.5821(3) _cell_length_c 14.3875(4) _cell_angle_alpha 90.00 _cell_angle_beta 91.285(3) _cell_angle_gamma 90.00 _cell_volume 1665.16(7) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 29528 _cell_measurement_theta_min 2.5654 _cell_measurement_theta_max 30.8049 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.220 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1048 _exptl_absorpt_coefficient_mu 11.575 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.24584 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _exptl_special_details ; The crystal was a non-merohedral twin. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Xcalibur, Eos' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 16.1419 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5908 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0794 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.79 _diffrn_reflns_theta_max 28.28 _reflns_number_total 5925 _reflns_number_gt 4433 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker XP' _computing_publication_material SHELXL-97 _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. The structure was refined using the "HKLF 5" method, as appropriate for a non-merohedral twin. The scale factor for the minor component was 0.064(3). Because the untwinning routines merge all equivalent reflections before refinement, R(int) is meaningless. The number of reflections is not well-defined for a dataset with two twinning components (reflection types "twin component 1 alone" and "twin components 1 & 2 overlapped"). ; _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^)+(0.0351P)^2^+10.4358P] 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 5925 _refine_ls_number_parameters 153 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0707 _refine_ls_R_factor_gt 0.0439 _refine_ls_wR_factor_ref 0.0955 _refine_ls_wR_factor_gt 0.0922 _refine_ls_goodness_of_fit_ref 1.106 _refine_ls_restrained_S_all 1.106 _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 Au1 Au 0.04080(3) 0.066206(16) 0.184109(18) 0.01808(8) Uani 1 1 d . . . Cl1 Cl 0.3261(2) 0.08727(12) 0.18017(13) 0.0299(4) Uani 1 1 d . . . Cl2 Cl 0.0688(2) 0.01284(12) 0.33642(12) 0.0286(4) Uani 1 1 d . . . Cl3 Cl -0.24127(19) 0.03578(11) 0.18382(12) 0.0246(3) Uani 1 1 d . . . Se1 Se 0.02969(8) 0.12096(4) 0.02360(5) 0.02006(14) Uani 1 1 d . . . P1 P -0.14953(19) 0.23730(10) 0.01490(11) 0.0150(3) Uani 1 1 d . . . C1 C -0.1074(9) 0.3271(4) 0.1053(5) 0.0243(15) Uani 1 1 d . . . C2 C -0.1089(8) 0.2816(4) -0.1032(4) 0.0206(13) Uani 1 1 d . . . H2 H -0.1936 0.3306 -0.1178 0.025 Uiso 1 1 calc R . . C3 C -0.3685(8) 0.1986(4) 0.0235(5) 0.0243(15) Uani 1 1 d . . . H3 H -0.3833 0.1808 0.0899 0.029 Uiso 1 1 calc R . . C11 C -0.1695(10) 0.4212(4) 0.0691(5) 0.0282(16) Uani 1 1 d . . . H11A H -0.1511 0.4676 0.1175 0.042 Uiso 1 1 calc R . . H11B H -0.2900 0.4175 0.0532 0.042 Uiso 1 1 calc R . . H11C H -0.1069 0.4381 0.0138 0.042 Uiso 1 1 calc R . . C12 C -0.2032(12) 0.3016(5) 0.1944(5) 0.041(2) Uani 1 1 d . . . H12A H -0.1636 0.2419 0.2174 0.061 Uiso 1 1 calc R . . H12B H -0.3243 0.2982 0.1799 0.061 Uiso 1 1 calc R . . H12C H -0.1823 0.3484 0.2421 0.061 Uiso 1 1 calc R . . C13 C 0.0802(11) 0.3335(5) 0.1298(6) 0.039(2) Uani 1 1 d . . . H13A H 0.1426 0.3491 0.0740 0.058 Uiso 1 1 calc R . . H13B H 0.1199 0.2744 0.1542 0.058 Uiso 1 1 calc R . . H13C H 0.0987 0.3811 0.1770 0.058 Uiso 1 1 calc R . . C21 C -0.1273(12) 0.2060(5) -0.1777(5) 0.041(2) Uani 1 1 d . . . H21A H -0.0917 0.2300 -0.2378 0.061 Uiso 1 1 calc R . . H21B H -0.2453 0.1866 -0.1827 0.061 Uiso 1 1 calc R . . H21C H -0.0566 0.1535 -0.1601 0.061 Uiso 1 1 calc R . . C22 C 0.0671(9) 0.3227(5) -0.1133(5) 0.0285(16) Uani 1 1 d . . . H22A H 0.1520 0.2744 -0.1049 0.043 Uiso 1 1 calc R . . H22B H 0.0854 0.3704 -0.0662 0.043 Uiso 1 1 calc R . . H22C H 0.0768 0.3496 -0.1754 0.043 Uiso 1 1 calc R . . C31 C -0.4126(10) 0.1136(6) -0.0339(5) 0.040(2) Uani 1 1 d . . . H31A H -0.5139 0.0848 -0.0094 0.061 Uiso 1 1 calc R . . H31B H -0.3186 0.0701 -0.0303 0.061 Uiso 1 1 calc R . . H31C H -0.4335 0.1314 -0.0988 0.061 Uiso 1 1 calc R . . C32 C -0.4990(10) 0.2758(6) 0.0032(8) 0.054(3) Uani 1 1 d . . . H32A H -0.4885 0.2968 -0.0611 0.081 Uiso 1 1 calc R . . H32B H -0.4780 0.3272 0.0457 0.081 Uiso 1 1 calc R . . H32C H -0.6130 0.2520 0.0121 0.081 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 Au1 0.01695(11) 0.01520(12) 0.02229(13) 0.00240(11) 0.00484(8) 0.00072(10) Cl1 0.0173(7) 0.0392(10) 0.0334(10) 0.0010(8) 0.0031(7) -0.0024(7) Cl2 0.0278(8) 0.0334(9) 0.0245(9) 0.0067(7) -0.0006(7) -0.0003(7) Cl3 0.0183(7) 0.0276(8) 0.0282(9) 0.0109(7) 0.0049(6) -0.0013(6) Se1 0.0229(3) 0.0161(3) 0.0216(3) 0.0023(3) 0.0097(3) 0.0047(2) P1 0.0156(7) 0.0127(7) 0.0170(8) 0.0005(6) 0.0045(6) -0.0006(6) C1 0.039(4) 0.011(3) 0.023(4) -0.002(3) 0.012(3) -0.002(3) C2 0.025(3) 0.019(3) 0.018(3) 0.004(3) 0.005(3) -0.002(3) C3 0.015(3) 0.025(3) 0.033(4) 0.010(3) 0.002(3) -0.004(3) C11 0.038(4) 0.017(3) 0.031(4) -0.002(3) 0.010(3) 0.001(3) C12 0.077(6) 0.020(4) 0.026(4) -0.004(3) 0.019(4) -0.007(4) C13 0.053(5) 0.020(4) 0.043(5) -0.005(3) -0.014(4) -0.011(3) C21 0.080(6) 0.032(4) 0.010(3) 0.003(3) 0.001(4) -0.016(4) C22 0.033(4) 0.029(4) 0.024(4) 0.001(3) 0.013(3) -0.006(3) C31 0.042(5) 0.050(5) 0.030(4) -0.002(4) 0.004(3) -0.034(4) C32 0.023(4) 0.048(5) 0.092(8) 0.037(5) 0.000(4) -0.001(4) _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 Au1 Cl3 2.2827(15) . ? Au1 Cl1 2.2875(16) . ? Au1 Cl2 2.3314(17) . ? Au1 Se1 2.4432(7) . ? Se1 P1 2.2159(16) . ? P1 C3 1.835(6) . ? P1 C2 1.853(6) . ? P1 C1 1.870(7) . ? C1 C13 1.526(11) . ? C1 C11 1.545(9) . ? C1 C12 1.550(9) . ? C2 C22 1.531(9) . ? C2 C21 1.542(9) . ? C3 C31 1.526(10) . ? C3 C32 1.553(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl3 Au1 Cl1 176.19(6) . . ? Cl3 Au1 Cl2 90.55(6) . . ? Cl1 Au1 Cl2 89.69(6) . . ? Cl3 Au1 Se1 92.70(5) . . ? Cl1 Au1 Se1 86.99(5) . . ? Cl2 Au1 Se1 176.57(5) . . ? P1 Se1 Au1 108.25(5) . . ? C3 P1 C2 110.7(3) . . ? C3 P1 C1 108.9(3) . . ? C2 P1 C1 111.2(3) . . ? C3 P1 Se1 111.7(2) . . ? C2 P1 Se1 101.2(2) . . ? C1 P1 Se1 113.1(2) . . ? C13 C1 C11 109.0(6) . . ? C13 C1 C12 108.5(7) . . ? C11 C1 C12 109.5(6) . . ? C13 C1 P1 111.2(5) . . ? C11 C1 P1 109.7(5) . . ? C12 C1 P1 108.9(5) . . ? C22 C2 C21 106.6(6) . . ? C22 C2 P1 113.7(5) . . ? C21 C2 P1 111.9(4) . . ? C31 C3 C32 110.1(7) . . ? C31 C3 P1 114.8(5) . . ? C32 C3 P1 113.2(5) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 3.233 _refine_diff_density_min -2.063 _refine_diff_density_rms 0.220 _iucr_refine_instructions_details ; TITL Sandra2 in P2(1)/n CELL 0.71073 7.938834 14.582133 14.387529 90.0000 91.2846 90.0000 ZERR 4.00 0.0002 0.0003 0.0004 0.0000 0.003 0.0000 LATT 1 SYMM -x+1/2, y+1/2,-z+1/2 SFAC C H Cl Se Au P UNIT 40.00 92.00 12.00 4.00 4.00 4.0 L.S. 4 BOND FMAP 2 PLAN 10 TEMP -173 OMIT 5 -8 3 OMIT 7 0 5 OMIT -3 -1 -6 SIZE 0.15 0.15 0.1 SHEL 999 0.75 ACTA WGHT 0.035100 10.435800 BASF 0.06410 FVAR 1.33925 AU1 5 0.040800 0.066206 0.184109 11.00000 0.01695 0.01520 = 0.02229 0.00240 0.00484 0.00072 CL1 3 0.326079 0.087267 0.180172 11.00000 0.01727 0.03918 = 0.03345 0.00097 0.00311 -0.00237 CL2 3 0.068771 0.012842 0.336423 11.00000 0.02783 0.03338 = 0.02454 0.00674 -0.00064 -0.00033 CL3 3 -0.241266 0.035777 0.183819 11.00000 0.01832 0.02758 = 0.02822 0.01086 0.00490 -0.00132 SE1 4 0.029689 0.120964 0.023599 11.00000 0.02294 0.01605 = 0.02160 0.00232 0.00967 0.00472 P1 6 -0.149531 0.237304 0.014905 11.00000 0.01565 0.01266 = 0.01702 0.00050 0.00454 -0.00061 C1 1 -0.107442 0.327086 0.105305 11.00000 0.03930 0.01055 = 0.02344 -0.00215 0.01155 -0.00192 C2 1 -0.108905 0.281598 -0.103232 11.00000 0.02492 0.01884 = 0.01823 0.00401 0.00480 -0.00211 AFIX 13 H2 2 -0.193599 0.330578 -0.117832 11.00000 -1.20000 AFIX 0 C3 1 -0.368541 0.198622 0.023507 11.00000 0.01476 0.02496 = 0.03315 0.00994 0.00207 -0.00424 AFIX 13 H3 2 -0.383320 0.180813 0.089947 11.00000 -1.20000 AFIX 0 C11 1 -0.169550 0.421187 0.069126 11.00000 0.03774 0.01667 = 0.03054 -0.00175 0.00953 0.00052 AFIX 137 H11A 2 -0.151128 0.467646 0.117512 11.00000 -1.50000 H11B 2 -0.290016 0.417543 0.053156 11.00000 -1.50000 H11C 2 -0.106912 0.438081 0.013754 11.00000 -1.50000 AFIX 0 C12 1 -0.203192 0.301560 0.194393 11.00000 0.07659 0.02008 = 0.02591 -0.00393 0.01854 -0.00660 AFIX 137 H12A 2 -0.163583 0.241926 0.217445 11.00000 -1.50000 H12B 2 -0.324258 0.298214 0.179944 11.00000 -1.50000 H12C 2 -0.182268 0.348403 0.242110 11.00000 -1.50000 AFIX 0 C13 1 0.080234 0.333471 0.129821 11.00000 0.05333 0.01979 = 0.04304 -0.00482 -0.01404 -0.01051 AFIX 137 H13A 2 0.142617 0.349063 0.073975 11.00000 -1.50000 H13B 2 0.119909 0.274358 0.154208 11.00000 -1.50000 H13C 2 0.098683 0.381093 0.177022 11.00000 -1.50000 AFIX 0 C21 1 -0.127304 0.206040 -0.177745 11.00000 0.07970 0.03249 = 0.00953 0.00325 0.00138 -0.01552 AFIX 137 H21A 2 -0.091666 0.230034 -0.237816 11.00000 -1.50000 H21B 2 -0.245312 0.186572 -0.182727 11.00000 -1.50000 H21C 2 -0.056626 0.153492 -0.160051 11.00000 -1.50000 AFIX 0 C22 1 0.067147 0.322693 -0.113322 11.00000 0.03319 0.02885 = 0.02389 0.00062 0.01303 -0.00593 AFIX 137 H22A 2 0.151972 0.274402 -0.104893 11.00000 -1.50000 H22B 2 0.085421 0.370362 -0.066152 11.00000 -1.50000 H22C 2 0.076771 0.349627 -0.175382 11.00000 -1.50000 AFIX 0 C31 1 -0.412554 0.113622 -0.033879 11.00000 0.04157 0.05011 = 0.02994 -0.00247 0.00373 -0.03364 AFIX 137 H31A 2 -0.513874 0.084823 -0.009373 11.00000 -1.50000 H31B 2 -0.318607 0.070075 -0.030314 11.00000 -1.50000 H31C 2 -0.433454 0.131362 -0.098817 11.00000 -1.50000 AFIX 0 C32 1 -0.499047 0.275754 0.003191 11.00000 0.02327 0.04752 = 0.09195 0.03707 0.00019 -0.00078 AFIX 137 H32A 2 -0.488456 0.296777 -0.061109 11.00000 -1.50000 H32B 2 -0.478050 0.327183 0.045741 11.00000 -1.50000 H32C 2 -0.613015 0.251990 0.012118 11.00000 -1.50000 HKLF 5 ; data_florian _database_code_depnum_ccdc_archive 'CCDC 925379' #TrackingRef '3a_Florian.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C11 H25 Au Cl5 P S' _chemical_formula_weight 594.56 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' 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 33.653(3) _cell_length_b 7.7933(3) _cell_length_c 16.212(2) _cell_angle_alpha 90.00 _cell_angle_beta 113.861(8) _cell_angle_gamma 90.00 _cell_volume 3888.5(6) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9326 _cell_measurement_theta_min 2.2558 _cell_measurement_theta_max 29.2941 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.031 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2288 _exptl_absorpt_coefficient_mu 8.430 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.69784 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Xcalibur, Eos' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 16.1419 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 85024 _diffrn_reflns_av_R_equivalents 0.0962 _diffrn_reflns_av_sigmaI/netI 0.0451 _diffrn_reflns_limit_h_min -45 _diffrn_reflns_limit_h_max 45 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.52 _diffrn_reflns_theta_max 28.70 _reflns_number_total 4978 _reflns_number_gt 3931 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker XP' _computing_publication_material SHELXL-97 _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. Two chlorine atoms are disordered over two positions. Appropriate restraints were used to improve stability of refinement, but dimensions of disordered atoms should be interpreted with caution. ; _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^)+(0.0244P)^2^+19.7674P] 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 4978 _refine_ls_number_parameters 191 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0559 _refine_ls_R_factor_gt 0.0344 _refine_ls_wR_factor_ref 0.0660 _refine_ls_wR_factor_gt 0.0598 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.035 _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 Au1 Au 0.5000 0.50309(3) 0.2500 0.01617(7) Uani 1 2 d SD . . Cl2 Cl 0.49043(18) 0.2144(3) 0.2333(3) 0.0361(14) Uani 0.50 1 d PD . . Cl3 Cl 0.51000(4) 0.50234(15) 0.11881(8) 0.0206(2) Uani 1 1 d D . . Cl4 Cl 0.5067(3) 0.7931(3) 0.2564(13) 0.0271(18) Uani 0.50 1 d PD . . Au2 Au 0.2500 0.2500 0.5000 0.01475(7) Uani 1 2 d S . . Cl5 Cl 0.27160(4) 0.52503(15) 0.49346(8) 0.0249(3) Uani 1 1 d . . . Cl6 Cl 0.22544(4) 0.22529(16) 0.34764(7) 0.0241(3) Uani 1 1 d . . . Cl1 Cl 0.61364(5) 0.60537(18) 0.44219(9) 0.0319(3) Uani 1 1 d . . . S1 S 0.57767(4) 0.73616(17) 0.49613(8) 0.0230(3) Uani 1 1 d . . . P1 P 0.62427(4) 0.88678(15) 0.59660(8) 0.0140(2) Uani 1 1 d . . . C1 C 0.65319(15) 0.7464(6) 0.6966(3) 0.0169(9) Uani 1 1 d . . . C2 C 0.58743(15) 1.0530(6) 0.6108(3) 0.0178(10) Uani 1 1 d . . . C3 C 0.66337(15) 0.9713(6) 0.5543(3) 0.0181(10) Uani 1 1 d . . . H3 H 0.6841 0.8755 0.5603 0.022 Uiso 1 1 calc R . . C11 C 0.66841(18) 0.5840(7) 0.6633(3) 0.0260(12) Uani 1 1 d . . . H11A H 0.6869 0.6172 0.6322 0.039 Uiso 1 1 calc R . . H11B H 0.6431 0.5210 0.6215 0.039 Uiso 1 1 calc R . . H11C H 0.6850 0.5107 0.7149 0.039 Uiso 1 1 calc R . . C12 C 0.69267(16) 0.8349(6) 0.7676(3) 0.0222(11) Uani 1 1 d . . . H12A H 0.6840 0.9468 0.7825 0.033 Uiso 1 1 calc R . . H12B H 0.7150 0.8511 0.7438 0.033 Uiso 1 1 calc R . . H12C H 0.7044 0.7637 0.8220 0.033 Uiso 1 1 calc R . . C13 C 0.62215(17) 0.6886(7) 0.7391(3) 0.0226(11) Uani 1 1 d . . . H13A H 0.6366 0.6029 0.7859 0.034 Uiso 1 1 calc R . . H13B H 0.5960 0.6384 0.6925 0.034 Uiso 1 1 calc R . . H13C H 0.6140 0.7878 0.7661 0.034 Uiso 1 1 calc R . . C21 C 0.57442(17) 1.1792(6) 0.5317(3) 0.0230(11) Uani 1 1 d . . . H21A H 0.5611 1.1162 0.4748 0.034 Uiso 1 1 calc R . . H21B H 0.6003 1.2398 0.5336 0.034 Uiso 1 1 calc R . . H21C H 0.5536 1.2625 0.5362 0.034 Uiso 1 1 calc R . . C22 C 0.61038(16) 1.1504(6) 0.6998(3) 0.0209(11) Uani 1 1 d . . . H22A H 0.6369 1.2036 0.7007 0.031 Uiso 1 1 calc R . . H22B H 0.6179 1.0702 0.7504 0.031 Uiso 1 1 calc R . . H22C H 0.5910 1.2396 0.7051 0.031 Uiso 1 1 calc R . . C23 C 0.54643(16) 0.9661(7) 0.6101(3) 0.0249(11) Uani 1 1 d . . . H23A H 0.5266 1.0535 0.6152 0.037 Uiso 1 1 calc R . . H23B H 0.5545 0.8865 0.6610 0.037 Uiso 1 1 calc R . . H23C H 0.5320 0.9028 0.5535 0.037 Uiso 1 1 calc R . . C31 C 0.69104(17) 1.1203(6) 0.6104(3) 0.0211(11) Uani 1 1 d . . . H31A H 0.7154 1.1412 0.5931 0.032 Uiso 1 1 calc R . . H31B H 0.7023 1.0909 0.6746 0.032 Uiso 1 1 calc R . . H31C H 0.6731 1.2239 0.5992 0.032 Uiso 1 1 calc R . . C32 C 0.64404(17) 1.0228(7) 0.4537(3) 0.0246(11) Uani 1 1 d . . . H32A H 0.6308 1.1368 0.4468 0.037 Uiso 1 1 calc R . . H32B H 0.6219 0.9390 0.4188 0.037 Uiso 1 1 calc R . . H32C H 0.6672 1.0252 0.4316 0.037 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 Au1 0.01941(13) 0.01143(13) 0.02055(13) 0.000 0.01107(10) 0.000 Cl2 0.079(5) 0.0095(10) 0.039(4) -0.0040(11) 0.044(3) -0.0074(14) Cl3 0.0247(6) 0.0207(6) 0.0193(5) 0.0009(5) 0.0120(5) 0.0025(5) Cl4 0.047(6) 0.0118(9) 0.028(5) 0.0000(17) 0.021(5) -0.0043(14) Au2 0.01793(13) 0.01262(13) 0.01362(12) -0.00001(10) 0.00631(10) 0.00187(10) Cl5 0.0352(7) 0.0142(6) 0.0275(6) -0.0008(5) 0.0149(6) -0.0032(5) Cl6 0.0343(7) 0.0222(6) 0.0128(5) 0.0000(5) 0.0063(5) 0.0050(5) Cl1 0.0390(8) 0.0307(8) 0.0255(7) -0.0112(6) 0.0126(6) 0.0011(6) S1 0.0230(6) 0.0239(7) 0.0187(6) -0.0082(5) 0.0050(5) -0.0052(5) P1 0.0162(6) 0.0138(6) 0.0118(5) -0.0004(4) 0.0056(5) -0.0002(5) C1 0.024(2) 0.012(2) 0.015(2) 0.0028(19) 0.0072(19) -0.002(2) C2 0.020(2) 0.022(3) 0.014(2) 0.0006(19) 0.0082(19) 0.003(2) C3 0.021(2) 0.017(3) 0.017(2) 0.0036(19) 0.0088(19) 0.0038(19) C11 0.033(3) 0.020(3) 0.022(3) 0.001(2) 0.008(2) 0.003(2) C12 0.026(3) 0.021(3) 0.017(2) 0.000(2) 0.006(2) -0.001(2) C13 0.026(3) 0.020(3) 0.023(3) 0.005(2) 0.011(2) -0.003(2) C21 0.024(3) 0.021(3) 0.023(3) 0.008(2) 0.008(2) 0.008(2) C22 0.024(3) 0.015(3) 0.025(3) -0.002(2) 0.012(2) 0.002(2) C23 0.024(3) 0.028(3) 0.025(3) 0.003(2) 0.012(2) 0.003(2) C31 0.030(3) 0.016(3) 0.022(3) -0.001(2) 0.015(2) -0.007(2) C32 0.030(3) 0.029(3) 0.018(2) 0.004(2) 0.013(2) -0.002(2) _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 Au1 Cl4 2.269(2) . ? Au1 Cl4 2.269(2) 2_655 ? Au1 Cl2 2.274(2) . ? Au1 Cl2 2.274(2) 2_655 ? Au1 Cl3 2.2838(11) . ? Au1 Cl3 2.2839(11) 2_655 ? Cl2 Cl2 0.653(8) 2_655 ? Cl4 Cl4 0.410(18) 2_655 ? Au2 Cl6 2.2737(12) . ? Au2 Cl6 2.2737(12) 7_556 ? Au2 Cl5 2.2794(12) 7_556 ? Au2 Cl5 2.2795(12) . ? Cl1 S1 2.0312(19) . ? S1 P1 2.1032(17) . ? P1 C3 1.834(5) . ? P1 C1 1.870(5) . ? P1 C2 1.871(5) . ? C1 C12 1.526(6) . ? C1 C13 1.533(6) . ? C1 C11 1.543(7) . ? C2 C23 1.532(7) . ? C2 C21 1.533(6) . ? C2 C22 1.533(6) . ? C3 C31 1.535(7) . ? C3 C32 1.545(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl4 Au1 Cl4 10.4(5) . 2_655 ? Cl4 Au1 Cl2 176.1(5) . . ? Cl4 Au1 Cl2 166.8(3) 2_655 . ? Cl4 Au1 Cl2 166.8(3) . 2_655 ? Cl4 Au1 Cl2 176.1(5) 2_655 2_655 ? Cl2 Au1 Cl2 16.50(19) . 2_655 ? Cl4 Au1 Cl3 89.8(6) . . ? Cl4 Au1 Cl3 90.5(6) 2_655 . ? Cl2 Au1 Cl3 87.35(17) . . ? Cl2 Au1 Cl3 92.35(17) 2_655 . ? Cl4 Au1 Cl3 90.5(6) . 2_655 ? Cl4 Au1 Cl3 89.8(6) 2_655 2_655 ? Cl2 Au1 Cl3 92.35(17) . 2_655 ? Cl2 Au1 Cl3 87.35(17) 2_655 2_655 ? Cl3 Au1 Cl3 179.70(6) . 2_655 ? Cl2 Cl2 Au1 81.75(10) 2_655 . ? Cl4 Cl4 Au1 84.8(2) 2_655 . ? Cl6 Au2 Cl6 180.00(7) . 7_556 ? Cl6 Au2 Cl5 89.33(4) . 7_556 ? Cl6 Au2 Cl5 90.67(4) 7_556 7_556 ? Cl6 Au2 Cl5 90.67(4) . . ? Cl6 Au2 Cl5 89.33(4) 7_556 . ? Cl5 Au2 Cl5 180.0 7_556 . ? Cl1 S1 P1 103.06(8) . . ? C3 P1 C1 109.5(2) . . ? C3 P1 C2 114.1(2) . . ? C1 P1 C2 115.9(2) . . ? C3 P1 S1 109.51(16) . . ? C1 P1 S1 107.97(16) . . ? C2 P1 S1 99.10(16) . . ? C12 C1 C13 109.8(4) . . ? C12 C1 C11 108.9(4) . . ? C13 C1 C11 107.4(4) . . ? C12 C1 P1 112.2(3) . . ? C13 C1 P1 110.6(3) . . ? C11 C1 P1 107.8(3) . . ? C23 C2 C21 109.0(4) . . ? C23 C2 C22 109.6(4) . . ? C21 C2 C22 109.5(4) . . ? C23 C2 P1 109.4(3) . . ? C21 C2 P1 108.7(3) . . ? C22 C2 P1 110.6(3) . . ? C31 C3 C32 108.9(4) . . ? C31 C3 P1 113.9(3) . . ? C32 C3 P1 115.4(3) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 28.70 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 2.401 _refine_diff_density_min -2.010 _refine_diff_density_rms 0.209 _iucr_refine_instructions_details ; TITL Florian in C2/c REM C2/c (#15 in standard setting) CELL 0.71073 33.652841 7.793309 16.211953 90.0000 113.8609 90.0000 ZERR 8.00 0.003 0.0003 0.002 0.0000 0.008 0.0000 LATT 7 SYMM -x, y,-z+1/2 SFAC C H P S Cl Au UNIT 88.00 200.00 8.00 8.00 40.00 8.00 L.S. 5 BOND FMAP 2 PLAN 20 SIZE 0.2 0.02 0.01 TEMP -173 SHEL 999 0.74 ACTA SADI Au1 Cl2 Au1 Cl3 Au1 Cl4 FLAT Au1 > Cl4 WGHT 0.024400 19.767401 FVAR 0.28237 AU1 6 0.500000 0.503094 0.250000 10.50000 0.01941 0.01143 = 0.02055 0.00000 0.01107 0.00000 CL2 5 0.490425 0.214357 0.233312 10.50000 0.07895 0.00950 = 0.03890 -0.00396 0.04362 -0.00743 CL3 5 0.510002 0.502335 0.118815 11.00000 0.02469 0.02073 = 0.01933 0.00087 0.01196 0.00251 CL4 5 0.506650 0.793065 0.256392 10.50000 0.04655 0.01180 = 0.02829 0.00003 0.02067 -0.00430 AU2 6 0.250000 0.250000 0.500000 10.50000 0.01793 0.01262 = 0.01362 -0.00001 0.00631 0.00187 CL5 5 0.271600 0.525026 0.493462 11.00000 0.03521 0.01418 = 0.02754 -0.00083 0.01488 -0.00320 CL6 5 0.225441 0.225291 0.347641 11.00000 0.03429 0.02220 = 0.01280 0.00004 0.00630 0.00499 CL1 5 0.613641 0.605373 0.442188 11.00000 0.03900 0.03072 = 0.02554 -0.01124 0.01259 0.00107 S1 4 0.577669 0.736159 0.496135 11.00000 0.02298 0.02386 = 0.01871 -0.00816 0.00496 -0.00518 P1 3 0.624269 0.886784 0.596601 11.00000 0.01615 0.01383 = 0.01183 -0.00041 0.00558 -0.00016 C1 1 0.653190 0.746411 0.696649 11.00000 0.02366 0.01177 = 0.01474 0.00283 0.00721 -0.00154 C2 1 0.587426 1.053001 0.610812 11.00000 0.01951 0.02181 = 0.01350 0.00056 0.00821 0.00309 C3 1 0.663370 0.971316 0.554318 11.00000 0.02115 0.01737 = 0.01686 0.00364 0.00875 0.00379 AFIX 13 H3 2 0.684128 0.875538 0.560257 11.00000 -1.20000 AFIX 0 C11 1 0.668415 0.583980 0.663267 11.00000 0.03299 0.02000 = 0.02177 0.00084 0.00772 0.00279 AFIX 137 H11A 2 0.686882 0.617169 0.632186 11.00000 -1.50000 H11B 2 0.643053 0.520967 0.621511 11.00000 -1.50000 H11C 2 0.684974 0.510669 0.714906 11.00000 -1.50000 AFIX 0 C12 1 0.692672 0.834926 0.767587 11.00000 0.02623 0.02064 = 0.01710 -0.00001 0.00613 -0.00111 AFIX 137 H12A 2 0.684024 0.946804 0.782510 11.00000 -1.50000 H12B 2 0.714951 0.851122 0.743814 11.00000 -1.50000 H12C 2 0.704401 0.763709 0.822004 11.00000 -1.50000 AFIX 0 C13 1 0.622152 0.688647 0.739095 11.00000 0.02569 0.02032 = 0.02325 0.00525 0.01138 -0.00289 AFIX 137 H13A 2 0.636593 0.602856 0.785887 11.00000 -1.50000 H13B 2 0.596019 0.638353 0.692486 11.00000 -1.50000 H13C 2 0.613997 0.787793 0.766053 11.00000 -1.50000 AFIX 0 C21 1 0.574419 1.179236 0.531729 11.00000 0.02381 0.02131 = 0.02263 0.00773 0.00825 0.00770 AFIX 137 H21A 2 0.561077 1.116182 0.474767 11.00000 -1.50000 H21B 2 0.600300 1.239754 0.533614 11.00000 -1.50000 H21C 2 0.553564 1.262487 0.536240 11.00000 -1.50000 AFIX 0 C22 1 0.610380 1.150388 0.699776 11.00000 0.02423 0.01511 = 0.02510 -0.00242 0.01190 0.00187 AFIX 137 H22A 2 0.636946 1.203595 0.700716 11.00000 -1.50000 H22B 2 0.617852 1.070232 0.750414 11.00000 -1.50000 H22C 2 0.591011 1.239575 0.705051 11.00000 -1.50000 AFIX 0 C23 1 0.546435 0.966111 0.610079 11.00000 0.02357 0.02835 = 0.02499 0.00287 0.01216 0.00333 AFIX 137 H23A 2 0.526628 1.053524 0.615229 11.00000 -1.50000 H23B 2 0.554454 0.886458 0.661042 11.00000 -1.50000 H23C 2 0.532009 0.902783 0.553498 11.00000 -1.50000 AFIX 0 C31 1 0.691036 1.120264 0.610369 11.00000 0.03001 0.01607 = 0.02207 -0.00103 0.01538 -0.00660 AFIX 137 H31A 2 0.715360 1.141169 0.593099 11.00000 -1.50000 H31B 2 0.702302 1.090851 0.674572 11.00000 -1.50000 H31C 2 0.673112 1.223879 0.599227 11.00000 -1.50000 AFIX 0 C32 1 0.644043 1.022812 0.453661 11.00000 0.03017 0.02851 = 0.01850 0.00360 0.01323 -0.00167 AFIX 137 H32A 2 0.630790 1.136808 0.446783 11.00000 -1.50000 H32B 2 0.621898 0.939048 0.418778 11.00000 -1.50000 H32C 2 0.667187 1.025234 0.431592 11.00000 -1.50000 HKLF 4 ; data_otto _database_code_depnum_ccdc_archive 'CCDC 925380' #TrackingRef '3b_Otto.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C11 H25 Au Cl5 P Se' _chemical_formula_weight 641.46 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' 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 33.7472(6) _cell_length_b 7.79306(8) _cell_length_c 16.2575(3) _cell_angle_alpha 90.00 _cell_angle_beta 113.582(3) _cell_angle_gamma 90.00 _cell_volume 3918.54(11) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 55878 _cell_measurement_theta_min 2.2412 _cell_measurement_theta_max 30.8672 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.175 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2432 _exptl_absorpt_coefficient_mu 10.116 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.30819 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET) (compiled Aug 3 2011,13:03:54) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Xcalibur, Eos' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 16.1419 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 257420 _diffrn_reflns_av_R_equivalents 0.0577 _diffrn_reflns_av_sigmaI/netI 0.0191 _diffrn_reflns_limit_h_min -48 _diffrn_reflns_limit_h_max 47 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.52 _diffrn_reflns_theta_max 30.94 _reflns_number_total 6027 _reflns_number_gt 5452 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET) (compiled Aug 3 2011,13:03:54) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET) (compiled Aug 3 2011,13:03:54) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET) (compiled Aug 3 2011,13:03:54) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker XP' _computing_publication_material SHELXL-97 _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. Two chlorine atoms are disordered over two positions. Appropriate restraints were used to improve stability of refinement, but dimensions of disordered atoms should be interpreted with caution. ; _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^)+(0.0166P)^2^+12.1957P] 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 6027 _refine_ls_number_parameters 191 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0276 _refine_ls_R_factor_gt 0.0209 _refine_ls_wR_factor_ref 0.0427 _refine_ls_wR_factor_gt 0.0407 _refine_ls_goodness_of_fit_ref 1.104 _refine_ls_restrained_S_all 1.104 _refine_ls_shift/su_max 0.002 _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 Au1 Au 0.0000 -0.010518(15) 0.2500 0.01363(3) Uani 1 2 d S . . Au2 Au 0.2500 0.2500 0.5000 0.01126(3) Uani 1 2 d S . . Cl1 Cl 0.11449(2) 0.09614(9) 0.43861(4) 0.02734(14) Uani 1 1 d . . . Cl2 Cl -0.00990(7) -0.29947(15) 0.23350(16) 0.0338(6) Uani 0.50 1 d P . . Cl3 Cl -0.01056(2) -0.01088(7) 0.38023(4) 0.01812(11) Uani 1 1 d . . . Cl4 Cl 0.0054(3) 0.27974(14) 0.2548(10) 0.0235(13) Uani 0.50 1 d P . . Cl5 Cl 0.22965(2) -0.02584(7) 0.50874(4) 0.02105(12) Uani 1 1 d . . . Cl6 Cl 0.22611(2) 0.22037(8) 0.34868(4) 0.02033(12) Uani 1 1 d . . . Se1 Se 0.074448(8) 0.23010(3) 0.493668(16) 0.01833(5) Uani 1 1 d . . . P1 P 0.124710(19) 0.39252(7) 0.59903(4) 0.01109(11) Uani 1 1 d . . . C1 C 0.15374(8) 0.2516(3) 0.69849(15) 0.0141(4) Uani 1 1 d . . . C2 C 0.08879(8) 0.5609(3) 0.61412(15) 0.0138(4) Uani 1 1 d . . . C3 C 0.16381(8) 0.4750(3) 0.55587(15) 0.0137(4) Uani 1 1 d . . . H3 H 0.1845 0.3790 0.5625 0.016 Uiso 1 1 calc R . . C11 C 0.16883(9) 0.0908(3) 0.66442(17) 0.0197(5) Uani 1 1 d . . . H11A H 0.1869 0.1251 0.6327 0.030 Uiso 1 1 calc R . . H11B H 0.1436 0.0275 0.6234 0.030 Uiso 1 1 calc R . . H11C H 0.1856 0.0175 0.7155 0.030 Uiso 1 1 calc R . . C12 C 0.19345(8) 0.3401(3) 0.76840(16) 0.0168(5) Uani 1 1 d . . . H12A H 0.2054 0.2687 0.8224 0.025 Uiso 1 1 calc R . . H12B H 0.1850 0.4519 0.7839 0.025 Uiso 1 1 calc R . . H12C H 0.2153 0.3565 0.7437 0.025 Uiso 1 1 calc R . . C13 C 0.12291(9) 0.1945(3) 0.74173(17) 0.0202(5) Uani 1 1 d . . . H13A H 0.0969 0.1438 0.6958 0.030 Uiso 1 1 calc R . . H13B H 0.1148 0.2940 0.7685 0.030 Uiso 1 1 calc R . . H13C H 0.1374 0.1091 0.7885 0.030 Uiso 1 1 calc R . . C21 C 0.07592(8) 0.6886(3) 0.53513(17) 0.0186(5) Uani 1 1 d . . . H21A H 0.0550 0.7711 0.5396 0.028 Uiso 1 1 calc R . . H21B H 0.0629 0.6258 0.4783 0.028 Uiso 1 1 calc R . . H21C H 0.1017 0.7498 0.5373 0.028 Uiso 1 1 calc R . . C22 C 0.11151(8) 0.6574(3) 0.70311(16) 0.0188(5) Uani 1 1 d . . . H22A H 0.1383 0.7086 0.7048 0.028 Uiso 1 1 calc R . . H22B H 0.1182 0.5771 0.7533 0.028 Uiso 1 1 calc R . . H22C H 0.0925 0.7481 0.7080 0.028 Uiso 1 1 calc R . . C23 C 0.04740(8) 0.4754(3) 0.61302(18) 0.0204(5) Uani 1 1 d . . . H23A H 0.0551 0.3905 0.6614 0.031 Uiso 1 1 calc R . . H23B H 0.0321 0.4184 0.5551 0.031 Uiso 1 1 calc R . . H23C H 0.0286 0.5630 0.6218 0.031 Uiso 1 1 calc R . . C31 C 0.19124(8) 0.6252(3) 0.61069(18) 0.0191(5) Uani 1 1 d . . . H31A H 0.2157 0.6446 0.5937 0.029 Uiso 1 1 calc R . . H31B H 0.2021 0.5978 0.6748 0.029 Uiso 1 1 calc R . . H31C H 0.1734 0.7290 0.5985 0.029 Uiso 1 1 calc R . . C32 C 0.14455(9) 0.5222(4) 0.45555(17) 0.0227(5) Uani 1 1 d . . . H32A H 0.1282 0.6296 0.4467 0.034 Uiso 1 1 calc R . . H32B H 0.1252 0.4303 0.4211 0.034 Uiso 1 1 calc R . . H32C H 0.1680 0.5369 0.4350 0.034 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 Au1 0.01365(6) 0.00993(5) 0.02032(6) 0.000 0.00996(5) 0.000 Au2 0.01106(6) 0.01076(5) 0.01175(5) 0.00043(4) 0.00433(4) 0.00169(4) Cl1 0.0316(4) 0.0280(3) 0.0228(3) -0.0093(2) 0.0112(3) 0.0020(3) Cl2 0.065(2) 0.0113(4) 0.0477(18) -0.0033(5) 0.0463(14) -0.0045(6) Cl3 0.0196(3) 0.0176(2) 0.0199(3) -0.0004(2) 0.0108(2) -0.0035(2) Cl4 0.040(4) 0.0110(4) 0.021(3) -0.0006(9) 0.014(3) -0.0037(7) Cl5 0.0266(3) 0.0134(2) 0.0244(3) 0.0005(2) 0.0115(2) -0.0031(2) Cl6 0.0252(3) 0.0205(3) 0.0124(2) -0.0003(2) 0.0046(2) 0.0039(2) Se1 0.01531(12) 0.02074(11) 0.01544(11) -0.00587(9) 0.00247(9) -0.00326(9) P1 0.0116(3) 0.0111(2) 0.0103(2) -0.00012(19) 0.0041(2) -0.00052(19) C1 0.0157(11) 0.0129(10) 0.0120(10) 0.0022(8) 0.0039(9) -0.0007(8) C2 0.0122(11) 0.0152(10) 0.0149(10) 0.0000(8) 0.0063(9) 0.0020(8) C3 0.0143(11) 0.0151(10) 0.0134(10) 0.0024(8) 0.0074(8) 0.0001(8) C11 0.0239(13) 0.0129(10) 0.0203(12) 0.0029(9) 0.0067(10) 0.0030(9) C12 0.0161(12) 0.0168(10) 0.0134(10) 0.0005(8) 0.0017(9) -0.0012(9) C13 0.0229(13) 0.0204(11) 0.0188(11) 0.0046(9) 0.0098(10) -0.0034(10) C21 0.0187(12) 0.0187(11) 0.0184(11) 0.0046(9) 0.0075(10) 0.0067(9) C22 0.0213(13) 0.0173(11) 0.0186(11) -0.0042(9) 0.0087(10) 0.0016(9) C23 0.0130(11) 0.0263(12) 0.0241(12) -0.0011(10) 0.0096(10) -0.0007(9) C31 0.0183(12) 0.0164(11) 0.0244(12) -0.0002(9) 0.0103(10) -0.0036(9) C32 0.0266(14) 0.0289(13) 0.0156(11) 0.0047(10) 0.0116(10) -0.0006(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Au1 Cl4 2.2681(13) 2 ? Au1 Cl4 2.2681(13) . ? Au1 Cl2 2.2765(12) 2 ? Au1 Cl2 2.2765(12) . ? Au1 Cl3 2.2833(6) . ? Au1 Cl3 2.2833(6) 2 ? Au2 Cl6 2.2734(6) 7_556 ? Au2 Cl6 2.2735(6) . ? Au2 Cl5 2.2784(6) . ? Au2 Cl5 2.2784(6) 7_556 ? Cl1 Se1 2.1645(7) . ? Cl2 Cl2 0.669(4) 2 ? Cl4 Cl4 0.332(18) 2 ? Se1 P1 2.2557(6) . ? P1 C3 1.840(2) . ? P1 C2 1.868(2) . ? P1 C1 1.875(2) . ? C1 C12 1.532(3) . ? C1 C13 1.536(4) . ? C1 C11 1.536(3) . ? C2 C22 1.536(3) . ? C2 C23 1.541(3) . ? C2 C21 1.543(3) . ? C3 C31 1.536(3) . ? C3 C32 1.539(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl4 Au1 Cl4 8.4(4) 2 . ? Cl4 Au1 Cl2 175.2(3) 2 2 ? Cl4 Au1 Cl2 167.6(2) . 2 ? Cl4 Au1 Cl2 167.6(2) 2 . ? Cl4 Au1 Cl2 175.2(3) . . ? Cl2 Au1 Cl2 16.89(9) 2 . ? Cl4 Au1 Cl3 89.6(5) 2 . ? Cl4 Au1 Cl3 90.5(5) . . ? Cl2 Au1 Cl3 87.68(8) 2 . ? Cl2 Au1 Cl3 92.18(8) . . ? Cl4 Au1 Cl3 90.5(5) 2 2 ? Cl4 Au1 Cl3 89.6(5) . 2 ? Cl2 Au1 Cl3 92.18(8) 2 2 ? Cl2 Au1 Cl3 87.68(8) . 2 ? Cl3 Au1 Cl3 179.86(3) . 2 ? Cl6 Au2 Cl6 180.0 7_556 . ? Cl6 Au2 Cl5 90.78(2) 7_556 . ? Cl6 Au2 Cl5 89.22(2) . . ? Cl6 Au2 Cl5 89.22(2) 7_556 7_556 ? Cl6 Au2 Cl5 90.78(2) . 7_556 ? Cl5 Au2 Cl5 179.998(1) . 7_556 ? Cl2 Cl2 Au1 81.55(4) 2 . ? Cl4 Cl4 Au1 85.8(2) 2 . ? Cl1 Se1 P1 100.40(3) . . ? C3 P1 C2 113.99(11) . . ? C3 P1 C1 109.06(11) . . ? C2 P1 C1 116.17(11) . . ? C3 P1 Se1 110.03(8) . . ? C2 P1 Se1 99.42(8) . . ? C1 P1 Se1 107.51(7) . . ? C12 C1 C13 110.0(2) . . ? C12 C1 C11 108.5(2) . . ? C13 C1 C11 108.16(19) . . ? C12 C1 P1 112.10(15) . . ? C13 C1 P1 110.40(17) . . ? C11 C1 P1 107.51(16) . . ? C22 C2 C23 109.3(2) . . ? C22 C2 C21 109.7(2) . . ? C23 C2 C21 108.5(2) . . ? C22 C2 P1 111.22(16) . . ? C23 C2 P1 109.11(16) . . ? C21 C2 P1 108.96(16) . . ? C31 C3 C32 109.5(2) . . ? C31 C3 P1 113.73(17) . . ? C32 C3 P1 115.10(17) . . ? _diffrn_measured_fraction_theta_max 0.970 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.125 _refine_diff_density_min -1.203 _refine_diff_density_rms 0.147 _iucr_refine_instructions_details ; TITL Otto in C2/c REM C2/c (#15 in standard setting) CELL 0.71073 33.747170 7.793064 16.257490 90.0000 113.5824 90.0000 ZERR 8.00 0.0006 0.00008 0.0003 0.0000 0.003 0.0000 LATT 7 SYMM -x, y,-z+1/2 SFAC C H P CL SE AU UNIT 88 200 8 40 8 8 FMAP 2 PLAN 10 L.S. 10 SIZE 0.35 0.2 0.04 TEMP -173 ACTA 60 OMIT -6 0 4 WGHT 0.016600 12.195704 FVAR 0.85727 AU1 6 0.000000 -0.010518 0.250000 10.50000 0.01365 0.00993 = 0.02032 0.00000 0.00996 0.00000 AU2 6 0.250000 0.250000 0.500000 10.50000 0.01106 0.01076 = 0.01175 0.00043 0.00433 0.00169 CL1 4 0.114491 0.096138 0.438606 11.00000 0.03161 0.02795 = 0.02276 -0.00932 0.01120 0.00202 CL2 4 -0.009897 -0.299467 0.233497 10.50000 0.06501 0.01130 = 0.04773 -0.00326 0.04626 -0.00451 CL3 4 -0.010559 -0.010879 0.380232 11.00000 0.01957 0.01764 = 0.01994 -0.00044 0.01084 -0.00351 CL4 4 0.005369 0.279742 0.254764 10.50000 0.03960 0.01104 = 0.02130 -0.00061 0.01360 -0.00373 CL5 4 0.229647 -0.025844 0.508738 11.00000 0.02656 0.01341 = 0.02441 0.00049 0.01150 -0.00308 CL6 4 0.226113 0.220365 0.348676 11.00000 0.02521 0.02053 = 0.01244 -0.00034 0.00459 0.00389 SE1 5 0.074448 0.230104 0.493668 11.00000 0.01531 0.02074 = 0.01544 -0.00587 0.00247 -0.00326 P1 3 0.124710 0.392519 0.599026 11.00000 0.01161 0.01109 = 0.01028 -0.00012 0.00407 -0.00052 C1 1 0.153741 0.251552 0.698494 11.00000 0.01575 0.01293 = 0.01198 0.00223 0.00386 -0.00066 C2 1 0.088787 0.560942 0.614125 11.00000 0.01219 0.01519 = 0.01485 0.00002 0.00633 0.00198 C3 1 0.163811 0.475014 0.555874 11.00000 0.01426 0.01515 = 0.01343 0.00243 0.00740 0.00008 AFIX 13 H3 2 0.184531 0.378996 0.562539 11.00000 -1.20000 AFIX 0 C11 1 0.168830 0.090847 0.664420 11.00000 0.02386 0.01285 = 0.02031 0.00292 0.00669 0.00297 AFIX 137 H11A 2 0.186904 0.125106 0.632720 11.00000 -1.50000 H11B 2 0.143586 0.027466 0.623352 11.00000 -1.50000 H11C 2 0.185625 0.017460 0.715452 11.00000 -1.50000 AFIX 0 C12 1 0.193454 0.340145 0.768402 11.00000 0.01612 0.01678 = 0.01342 0.00049 0.00170 -0.00125 AFIX 137 H12A 2 0.205427 0.268677 0.822404 11.00000 -1.50000 H12B 2 0.185020 0.451930 0.783867 11.00000 -1.50000 H12C 2 0.215328 0.356514 0.743667 11.00000 -1.50000 AFIX 0 C13 1 0.122914 0.194459 0.741731 11.00000 0.02287 0.02039 = 0.01885 0.00461 0.00978 -0.00335 AFIX 137 H13A 2 0.096873 0.143803 0.695823 11.00000 -1.50000 H13B 2 0.114846 0.294017 0.768506 11.00000 -1.50000 H13C 2 0.137356 0.109134 0.788451 11.00000 -1.50000 AFIX 0 C21 1 0.075915 0.688559 0.535128 11.00000 0.01868 0.01868 = 0.01843 0.00465 0.00745 0.00667 AFIX 137 H21A 2 0.054955 0.771141 0.539550 11.00000 -1.50000 H21B 2 0.062933 0.625769 0.478328 11.00000 -1.50000 H21C 2 0.101682 0.749820 0.537333 11.00000 -1.50000 AFIX 0 C22 1 0.111510 0.657390 0.703111 11.00000 0.02132 0.01733 = 0.01856 -0.00415 0.00871 0.00161 AFIX 137 H22A 2 0.138346 0.708610 0.704801 11.00000 -1.50000 H22B 2 0.118227 0.577057 0.753271 11.00000 -1.50000 H22C 2 0.092456 0.748052 0.708048 11.00000 -1.50000 AFIX 0 C23 1 0.047399 0.475420 0.613015 11.00000 0.01303 0.02630 = 0.02409 -0.00107 0.00964 -0.00068 AFIX 137 H23A 2 0.055138 0.390505 0.661395 11.00000 -1.50000 H23B 2 0.032128 0.418399 0.555139 11.00000 -1.50000 H23C 2 0.028613 0.562975 0.621806 11.00000 -1.50000 AFIX 0 C31 1 0.191241 0.625198 0.610689 11.00000 0.01833 0.01637 = 0.02439 -0.00022 0.01026 -0.00360 AFIX 137 H31A 2 0.215662 0.644567 0.593701 11.00000 -1.50000 H31B 2 0.202134 0.597780 0.674794 11.00000 -1.50000 H31C 2 0.173422 0.729036 0.598533 11.00000 -1.50000 AFIX 0 C32 1 0.144553 0.522250 0.455548 11.00000 0.02664 0.02894 = 0.01556 0.00465 0.01164 -0.00064 AFIX 137 H32A 2 0.128230 0.629578 0.446734 11.00000 -1.50000 H32B 2 0.125211 0.430342 0.421080 11.00000 -1.50000 H32C 2 0.167959 0.536899 0.434965 11.00000 -1.50000 HKLF 4 ; data_arco _database_code_depnum_ccdc_archive 'CCDC 925381' #TrackingRef '3c_Arco.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C10 H23 Au Cl5 P S' _chemical_formula_weight 580.53 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Au Au -2.0133 8.8022 '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 7.5619(4) _cell_length_b 8.7408(4) _cell_length_c 15.4558(6) _cell_angle_alpha 84.346(4) _cell_angle_beta 78.306(4) _cell_angle_gamma 66.915(5) _cell_volume 920.07(7) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 21451 _cell_measurement_theta_min 2.5285 _cell_measurement_theta_max 30.7406 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.095 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 556 _exptl_absorpt_coefficient_mu 8.904 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.31555 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET) (compiled Aug 3 2011,13:03:54) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Xcalibur, Eos' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 16.1419 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 50339 _diffrn_reflns_av_R_equivalents 0.0323 _diffrn_reflns_av_sigmaI/netI 0.0186 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.53 _diffrn_reflns_theta_max 30.81 _reflns_number_total 5453 _reflns_number_gt 4838 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET) (compiled Aug 3 2011,13:03:54) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET) (compiled Aug 3 2011,13:03:54) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET) (compiled Aug 3 2011,13:03:54) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker XP' _computing_publication_material SHELXL-97 _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^)+(0.0146P)^2^+0.7156P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00167(11) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 5453 _refine_ls_number_parameters 174 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0212 _refine_ls_R_factor_gt 0.0166 _refine_ls_wR_factor_ref 0.0360 _refine_ls_wR_factor_gt 0.0343 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.050 _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 Au1 Au 0.5000 1.0000 0.5000 0.01239(3) Uani 1 2 d S . . Au2 Au 1.0000 0.0000 0.0000 0.01355(3) Uani 1 2 d S . . Cl1 Cl 0.83963(8) 0.40481(7) 0.08881(4) 0.02207(11) Uani 1 1 d . . . Cl2 Cl 0.79512(7) 0.97158(6) 0.52926(4) 0.02032(10) Uani 1 1 d . . . Cl3 Cl 0.65506(8) 0.79771(6) 0.39766(4) 0.02293(11) Uani 1 1 d . . . Cl4 Cl 1.16568(8) 0.15648(7) -0.07470(4) 0.02303(11) Uani 1 1 d . . . Cl5 Cl 0.78628(8) 0.08779(7) -0.09592(4) 0.02613(12) Uani 1 1 d . . . S1 S 0.61541(8) 0.55864(6) 0.17559(4) 0.01794(10) Uani 1 1 d . . . P1 P 0.49846(7) 0.39246(6) 0.24666(3) 0.01224(10) Uani 1 1 d . . . C1 C 0.2556(3) 0.5351(2) 0.30323(13) 0.0153(4) Uani 1 1 d . . . C2 C 0.4948(3) 0.2469(3) 0.17039(14) 0.0177(4) Uani 1 1 d . . . H2 H 0.6350 0.1771 0.1483 0.021 Uiso 1 1 calc R . . C3 C 0.6515(3) 0.2687(2) 0.32657(14) 0.0150(4) Uani 1 1 d . . . H3 H 0.5750 0.2104 0.3665 0.018 Uiso 1 1 calc R . . C11 C 0.1898(3) 0.4497(3) 0.38824(14) 0.0202(4) Uani 1 1 d . . . H11A H 0.2802 0.4301 0.4292 0.030 Uiso 1 1 calc R . . H11B H 0.1894 0.3432 0.3737 0.030 Uiso 1 1 calc R . . H11C H 0.0579 0.5213 0.4159 0.030 Uiso 1 1 calc R . . C12 C 0.1073(3) 0.5766(3) 0.24088(14) 0.0207(4) Uani 1 1 d . . . H12A H 0.0889 0.4755 0.2304 0.031 Uiso 1 1 calc R . . H12B H 0.1564 0.6209 0.1846 0.031 Uiso 1 1 calc R . . H12C H -0.0179 0.6599 0.2680 0.031 Uiso 1 1 calc R . . C13 C 0.2660(3) 0.6982(3) 0.32643(15) 0.0206(4) Uani 1 1 d . . . H13A H 0.1412 0.7664 0.3619 0.031 Uiso 1 1 calc R . . H13B H 0.2922 0.7592 0.2719 0.031 Uiso 1 1 calc R . . H13C H 0.3711 0.6728 0.3602 0.031 Uiso 1 1 calc R . . C21 C 0.4055(4) 0.1256(3) 0.22073(16) 0.0242(5) Uani 1 1 d . . . H21A H 0.2656 0.1860 0.2419 0.036 Uiso 1 1 calc R . . H21B H 0.4704 0.0758 0.2712 0.036 Uiso 1 1 calc R . . H21C H 0.4236 0.0376 0.1811 0.036 Uiso 1 1 calc R . . C22 C 0.4073(4) 0.3229(3) 0.08773(15) 0.0272(5) Uani 1 1 d . . . H22A H 0.4485 0.2366 0.0437 0.041 Uiso 1 1 calc R . . H22B H 0.4531 0.4114 0.0631 0.041 Uiso 1 1 calc R . . H22C H 0.2644 0.3695 0.1034 0.041 Uiso 1 1 calc R . . C31 C 0.6958(3) 0.3759(3) 0.38546(15) 0.0229(5) Uani 1 1 d . . . H31A H 0.7744 0.3041 0.4279 0.034 Uiso 1 1 calc R . . H31B H 0.5729 0.4545 0.4175 0.034 Uiso 1 1 calc R . . H31C H 0.7684 0.4376 0.3486 0.034 Uiso 1 1 calc R . . C32 C 0.8420(3) 0.1330(3) 0.28274(15) 0.0216(4) Uani 1 1 d . . . H32A H 0.9202 0.1849 0.2416 0.032 Uiso 1 1 calc R . . H32B H 0.8109 0.0586 0.2504 0.032 Uiso 1 1 calc R . . H32C H 0.9163 0.0689 0.3283 0.032 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 Au1 0.00974(5) 0.01046(5) 0.01638(6) 0.00042(4) -0.00134(4) -0.00389(4) Au2 0.01509(6) 0.01277(5) 0.01290(6) -0.00121(4) -0.00292(4) -0.00503(4) Cl1 0.0175(2) 0.0233(2) 0.0232(3) -0.0011(2) 0.00370(19) -0.0088(2) Cl2 0.0134(2) 0.0207(2) 0.0283(3) 0.0000(2) -0.00544(19) -0.00718(18) Cl3 0.0181(2) 0.0202(2) 0.0277(3) -0.0092(2) -0.0005(2) -0.00397(19) Cl4 0.0239(3) 0.0218(2) 0.0256(3) 0.0033(2) -0.0035(2) -0.0125(2) Cl5 0.0254(3) 0.0343(3) 0.0223(3) 0.0057(2) -0.0121(2) -0.0129(2) S1 0.0162(2) 0.0147(2) 0.0212(3) 0.00216(19) -0.00016(19) -0.00623(18) P1 0.0107(2) 0.0125(2) 0.0131(2) -0.00008(18) -0.00189(18) -0.00431(18) C1 0.0118(9) 0.0165(9) 0.0148(9) 0.0004(7) -0.0010(7) -0.0033(7) C2 0.0173(10) 0.0222(10) 0.0158(10) -0.0055(8) -0.0012(8) -0.0095(8) C3 0.0138(9) 0.0129(9) 0.0179(10) 0.0023(7) -0.0055(8) -0.0038(7) C11 0.0157(10) 0.0233(10) 0.0175(10) 0.0016(8) 0.0013(8) -0.0055(8) C12 0.0126(10) 0.0265(11) 0.0200(11) 0.0008(8) -0.0034(8) -0.0042(8) C13 0.0197(10) 0.0143(9) 0.0250(11) -0.0033(8) -0.0040(9) -0.0027(8) C21 0.0265(12) 0.0249(11) 0.0266(12) -0.0042(9) -0.0027(9) -0.0155(9) C22 0.0271(12) 0.0406(14) 0.0167(11) -0.0049(10) -0.0036(9) -0.0152(11) C31 0.0251(11) 0.0194(10) 0.0254(12) -0.0008(9) -0.0138(9) -0.0052(9) C32 0.0177(10) 0.0165(10) 0.0264(12) -0.0001(8) -0.0065(9) -0.0010(8) _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 Au1 Cl3 2.2752(5) 2_676 ? Au1 Cl3 2.2753(5) . ? Au1 Cl2 2.2801(5) . ? Au1 Cl2 2.2801(5) 2_676 ? Au2 Cl5 2.2744(5) 2_755 ? Au2 Cl5 2.2744(5) . ? Au2 Cl4 2.2846(5) 2_755 ? Au2 Cl4 2.2847(5) . ? Cl1 S1 2.0316(7) . ? S1 P1 2.0970(7) . ? P1 C2 1.829(2) . ? P1 C3 1.836(2) . ? P1 C1 1.860(2) . ? C1 C11 1.538(3) . ? C1 C13 1.538(3) . ? C1 C12 1.539(3) . ? C2 C22 1.530(3) . ? C2 C21 1.540(3) . ? C3 C31 1.535(3) . ? C3 C32 1.538(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl3 Au1 Cl3 179.999(1) 2_676 . ? Cl3 Au1 Cl2 90.35(2) 2_676 . ? Cl3 Au1 Cl2 89.65(2) . . ? Cl3 Au1 Cl2 89.66(2) 2_676 2_676 ? Cl3 Au1 Cl2 90.34(2) . 2_676 ? Cl2 Au1 Cl2 179.998(1) . 2_676 ? Cl5 Au2 Cl5 179.999(2) 2_755 . ? Cl5 Au2 Cl4 90.43(2) 2_755 2_755 ? Cl5 Au2 Cl4 89.57(2) . 2_755 ? Cl5 Au2 Cl4 89.57(2) 2_755 . ? Cl5 Au2 Cl4 90.43(2) . . ? Cl4 Au2 Cl4 180.00(3) 2_755 . ? Cl1 S1 P1 101.57(3) . . ? C2 P1 C3 107.15(9) . . ? C2 P1 C1 115.86(10) . . ? C3 P1 C1 111.39(9) . . ? C2 P1 S1 109.35(7) . . ? C3 P1 S1 110.73(7) . . ? C1 P1 S1 102.30(7) . . ? C11 C1 C13 109.53(17) . . ? C11 C1 C12 109.89(17) . . ? C13 C1 C12 108.50(17) . . ? C11 C1 P1 109.31(14) . . ? C13 C1 P1 110.59(14) . . ? C12 C1 P1 109.01(14) . . ? C22 C2 C21 112.40(19) . . ? C22 C2 P1 116.51(16) . . ? C21 C2 P1 110.40(14) . . ? C31 C3 C32 110.39(17) . . ? C31 C3 P1 112.89(14) . . ? C32 C3 P1 112.80(14) . . ? _diffrn_measured_fraction_theta_max 0.947 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 1.299 _refine_diff_density_min -1.081 _refine_diff_density_rms 0.108 _iucr_refine_instructions_details ; TITL Arco in P-1 REM P-1 (#1 in standard setting) CELL 0.71073 7.561891 8.740809 15.455830 84.3457 78.3063 66.9145 ZERR 2.00 0.0004 0.0004 0.0006 0.004 0.004 0.005 LATT 1 SFAC C H P S CL AU UNIT 20 46 2 2 10 2 FMAP 2 PLAN 10 L.S. 4 SIZE 0.2 0.18 0.05 TEMP -173 ACTA 60 WGHT 0.014600 0.715600 EXTI 0.001668 FVAR 3.85524 AU1 6 0.500000 1.000000 0.500000 10.50000 0.00974 0.01046 = 0.01638 0.00042 -0.00134 -0.00389 AU2 6 1.000000 0.000000 0.000000 10.50000 0.01509 0.01277 = 0.01290 -0.00121 -0.00292 -0.00503 CL1 5 0.839626 0.404811 0.088811 11.00000 0.01746 0.02326 = 0.02322 -0.00110 0.00370 -0.00878 CL2 5 0.795122 0.971577 0.529256 11.00000 0.01338 0.02066 = 0.02825 -0.00004 -0.00544 -0.00718 CL3 5 0.655062 0.797707 0.397657 11.00000 0.01809 0.02017 = 0.02766 -0.00923 -0.00054 -0.00397 CL4 5 1.165679 0.156481 -0.074697 11.00000 0.02389 0.02183 = 0.02559 0.00334 -0.00345 -0.01247 CL5 5 0.786277 0.087795 -0.095919 11.00000 0.02544 0.03433 = 0.02226 0.00570 -0.01210 -0.01292 S1 4 0.615412 0.558635 0.175593 11.00000 0.01622 0.01472 = 0.02117 0.00216 -0.00016 -0.00623 P1 3 0.498461 0.392461 0.246660 11.00000 0.01075 0.01254 = 0.01314 -0.00008 -0.00189 -0.00431 C1 1 0.255605 0.535116 0.303235 11.00000 0.01177 0.01647 = 0.01477 0.00039 -0.00098 -0.00327 C2 1 0.494780 0.246876 0.170390 11.00000 0.01733 0.02216 = 0.01580 -0.00552 -0.00118 -0.00947 AFIX 13 H2 2 0.634992 0.177124 0.148265 11.00000 -1.20000 AFIX 0 C3 1 0.651505 0.268726 0.326575 11.00000 0.01380 0.01289 = 0.01787 0.00233 -0.00549 -0.00384 AFIX 13 H3 2 0.574974 0.210410 0.366492 11.00000 -1.20000 AFIX 0 C11 1 0.189813 0.449678 0.388236 11.00000 0.01575 0.02326 = 0.01745 0.00157 0.00125 -0.00550 AFIX 137 H11A 2 0.280227 0.430115 0.429217 11.00000 -1.50000 H11B 2 0.189403 0.343189 0.373724 11.00000 -1.50000 H11C 2 0.057876 0.521278 0.415942 11.00000 -1.50000 AFIX 0 C12 1 0.107307 0.576640 0.240884 11.00000 0.01258 0.02646 = 0.01997 0.00077 -0.00343 -0.00416 AFIX 137 H12A 2 0.088893 0.475549 0.230387 11.00000 -1.50000 H12B 2 0.156444 0.620880 0.184571 11.00000 -1.50000 H12C 2 -0.017861 0.659937 0.267987 11.00000 -1.50000 AFIX 0 C13 1 0.265974 0.698177 0.326426 11.00000 0.01968 0.01432 = 0.02501 -0.00328 -0.00404 -0.00273 AFIX 137 H13A 2 0.141223 0.766419 0.361943 11.00000 -1.50000 H13B 2 0.292244 0.759176 0.271910 11.00000 -1.50000 H13C 2 0.371064 0.672828 0.360202 11.00000 -1.50000 AFIX 0 C21 1 0.405472 0.125558 0.220728 11.00000 0.02645 0.02489 = 0.02655 -0.00419 -0.00266 -0.01548 AFIX 137 H21A 2 0.265593 0.185998 0.241870 11.00000 -1.50000 H21B 2 0.470406 0.075845 0.271231 11.00000 -1.50000 H21C 2 0.423589 0.037634 0.181115 11.00000 -1.50000 AFIX 0 C22 1 0.407341 0.322908 0.087727 11.00000 0.02709 0.04059 = 0.01675 -0.00491 -0.00360 -0.01515 AFIX 137 H22A 2 0.448522 0.236589 0.043695 11.00000 -1.50000 H22B 2 0.453056 0.411373 0.063127 11.00000 -1.50000 H22C 2 0.264446 0.369454 0.103420 11.00000 -1.50000 AFIX 0 C31 1 0.695782 0.375918 0.385465 11.00000 0.02513 0.01942 = 0.02537 -0.00080 -0.01378 -0.00520 AFIX 137 H31A 2 0.774359 0.304122 0.427850 11.00000 -1.50000 H31B 2 0.572900 0.454498 0.417503 11.00000 -1.50000 H31C 2 0.768355 0.437572 0.348641 11.00000 -1.50000 AFIX 0 C32 1 0.841971 0.132965 0.282741 11.00000 0.01770 0.01650 = 0.02638 -0.00006 -0.00653 -0.00097 AFIX 137 H32A 2 0.920173 0.184856 0.241631 11.00000 -1.50000 H32B 2 0.810867 0.058559 0.250370 11.00000 -1.50000 H32C 2 0.916269 0.068949 0.328284 11.00000 -1.50000 HKLF 4 ; data_helge _database_code_depnum_ccdc_archive 'CCDC 925382' #TrackingRef '3d_Helge.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C10 H23 Au Cl5 P Se' _chemical_formula_weight 627.43 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Au Au -2.0133 8.8022 '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 7.5836(2) _cell_length_b 8.7603(2) _cell_length_c 15.4719(6) _cell_angle_alpha 84.445(3) _cell_angle_beta 78.641(3) _cell_angle_gamma 67.128(3) _cell_volume 928.28(5) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 37919 _cell_measurement_theta_min 2.5189 _cell_measurement_theta_max 30.8074 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.245 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 592 _exptl_absorpt_coefficient_mu 10.673 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.23235 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Xcalibur, Eos' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 16.1419 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 102876 _diffrn_reflns_av_R_equivalents 0.0422 _diffrn_reflns_av_sigmaI/netI 0.0190 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.52 _diffrn_reflns_theta_max 30.88 _reflns_number_total 5489 _reflns_number_gt 4977 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker XP' _computing_publication_material SHELXL-97 _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^)+(0.0300P)^2^+1.3767P] 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 5489 _refine_ls_number_parameters 173 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0254 _refine_ls_R_factor_gt 0.0210 _refine_ls_wR_factor_ref 0.0542 _refine_ls_wR_factor_gt 0.0519 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.052 _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 Au1 Au 0.0000 1.0000 0.5000 0.01278(4) Uani 1 2 d S . . Au2 Au 0.5000 1.0000 0.0000 0.01247(4) Uani 1 2 d S . . Cl1 Cl 0.14673(10) 0.59827(9) 0.41498(5) 0.02206(14) Uani 1 1 d . . . Cl2 Cl 0.21089(11) 0.91781(10) 0.59699(5) 0.02617(15) Uani 1 1 d . . . Cl3 Cl -0.17349(10) 0.85514(9) 0.57968(5) 0.02235(14) Uani 1 1 d . . . Cl4 Cl 0.34763(10) 1.19883(9) 0.10371(5) 0.02282(14) Uani 1 1 d . . . Cl5 Cl 0.20491(9) 1.03003(9) -0.02957(5) 0.02027(13) Uani 1 1 d . . . Se1 Se 0.37816(4) 0.42524(3) 0.325139(18) 0.01722(6) Uani 1 1 d . . . P1 P 0.50452(9) 0.60337(9) 0.25119(4) 0.01182(12) Uani 1 1 d . . . C1 C 0.7478(4) 0.4630(3) 0.19534(17) 0.0144(5) Uani 1 1 d . . . C2 C 0.5057(4) 0.7483(4) 0.32873(18) 0.0170(5) Uani 1 1 d . . . H2 H 0.3660 0.8179 0.3498 0.020 Uiso 1 1 calc R . . C3 C 0.3525(4) 0.7280(3) 0.17102(17) 0.0146(5) Uani 1 1 d . . . H3 H 0.4280 0.7880 0.1324 0.018 Uiso 1 1 calc R . . C11 C 0.8138(4) 0.5486(4) 0.11102(18) 0.0197(5) Uani 1 1 d . . . H11A H 0.8104 0.6563 0.1256 0.029 Uiso 1 1 calc R . . H11B H 0.7266 0.5651 0.0689 0.029 Uiso 1 1 calc R . . H11C H 0.9467 0.4792 0.0848 0.029 Uiso 1 1 calc R . . C12 C 0.8938(4) 0.4218(4) 0.2588(2) 0.0203(6) Uani 1 1 d . . . H12A H 1.0179 0.3375 0.2329 0.030 Uiso 1 1 calc R . . H12B H 0.8427 0.3793 0.3150 0.030 Uiso 1 1 calc R . . H12C H 0.9137 0.5222 0.2690 0.030 Uiso 1 1 calc R . . C13 C 0.7371(4) 0.3001(4) 0.1719(2) 0.0201(5) Uani 1 1 d . . . H13A H 0.6349 0.3251 0.1365 0.030 Uiso 1 1 calc R . . H13B H 0.7074 0.2406 0.2263 0.030 Uiso 1 1 calc R . . H13C H 0.8623 0.2309 0.1381 0.030 Uiso 1 1 calc R . . C21 C 0.5903(4) 0.6724(4) 0.41187(19) 0.0255(6) Uani 1 1 d . . . H21A H 0.7325 0.6248 0.3971 0.038 Uiso 1 1 calc R . . H21B H 0.5428 0.5852 0.4362 0.038 Uiso 1 1 calc R . . H21C H 0.5500 0.7586 0.4557 0.038 Uiso 1 1 calc R . . C22 C 0.5972(4) 0.8689(4) 0.2794(2) 0.0233(6) Uani 1 1 d . . . H22A H 0.5842 0.9535 0.3199 0.035 Uiso 1 1 calc R . . H22B H 0.5303 0.9225 0.2300 0.035 Uiso 1 1 calc R . . H22C H 0.7352 0.8073 0.2570 0.035 Uiso 1 1 calc R . . C31 C 0.3106(4) 0.6224(4) 0.1106(2) 0.0230(6) Uani 1 1 d . . . H31A H 0.2331 0.5637 0.1458 0.034 Uiso 1 1 calc R . . H31B H 0.4335 0.5418 0.0810 0.034 Uiso 1 1 calc R . . H31C H 0.2383 0.6942 0.0664 0.034 Uiso 1 1 calc R . . C32 C 0.1628(4) 0.8603(4) 0.2149(2) 0.0215(6) Uani 1 1 d . . . H32A H 0.0875 0.9235 0.1697 0.032 Uiso 1 1 calc R . . H32B H 0.1927 0.9353 0.2475 0.032 Uiso 1 1 calc R . . H32C H 0.0870 0.8067 0.2558 0.032 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 Au1 0.01380(7) 0.01191(8) 0.01303(7) -0.00061(5) -0.00257(5) -0.00510(5) Au2 0.01021(6) 0.01034(7) 0.01658(7) 0.00044(5) -0.00126(5) -0.00427(5) Cl1 0.0170(3) 0.0235(4) 0.0232(3) -0.0014(3) 0.0041(2) -0.0085(3) Cl2 0.0246(3) 0.0350(4) 0.0228(3) 0.0061(3) -0.0119(3) -0.0134(3) Cl3 0.0227(3) 0.0208(4) 0.0251(3) 0.0030(3) -0.0013(2) -0.0121(3) Cl4 0.0186(3) 0.0206(4) 0.0271(3) -0.0090(3) -0.0004(2) -0.0049(3) Cl5 0.0131(3) 0.0205(3) 0.0288(3) -0.0001(3) -0.0051(2) -0.0074(2) Se1 0.01458(12) 0.01411(14) 0.02157(13) 0.00256(10) 0.00016(9) -0.00618(10) P1 0.0106(3) 0.0124(3) 0.0125(3) -0.0001(2) -0.0017(2) -0.0047(2) C1 0.0131(11) 0.0147(13) 0.0135(11) 0.0005(9) -0.0012(9) -0.0038(10) C2 0.0175(12) 0.0186(14) 0.0169(12) -0.0043(10) -0.0020(9) -0.0084(10) C3 0.0131(11) 0.0134(13) 0.0169(12) 0.0010(9) -0.0044(9) -0.0039(9) C11 0.0166(12) 0.0225(15) 0.0159(12) 0.0018(10) 0.0024(9) -0.0062(11) C12 0.0118(11) 0.0224(15) 0.0248(14) -0.0014(11) -0.0056(10) -0.0030(10) C13 0.0176(12) 0.0151(14) 0.0253(14) -0.0030(11) -0.0025(10) -0.0037(10) C21 0.0251(14) 0.0384(19) 0.0161(13) -0.0023(12) -0.0041(11) -0.0148(13) C22 0.0242(14) 0.0251(16) 0.0257(14) -0.0042(12) -0.0017(11) -0.0152(12) C31 0.0253(14) 0.0206(15) 0.0250(14) -0.0012(11) -0.0108(11) -0.0075(12) C32 0.0162(12) 0.0192(15) 0.0253(14) 0.0008(11) -0.0061(10) -0.0017(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Au1 Cl2 2.2736(7) 2_576 ? Au1 Cl2 2.2736(7) . ? Au1 Cl3 2.2841(7) 2_576 ? Au1 Cl3 2.2842(7) . ? Au2 Cl4 2.2782(7) . ? Au2 Cl4 2.2782(7) 2_675 ? Au2 Cl5 2.2823(6) 2_675 ? Au2 Cl5 2.2823(6) . ? Cl1 Se1 2.1654(7) . ? Se1 P1 2.2467(7) . ? P1 C2 1.833(3) . ? P1 C3 1.839(3) . ? P1 C1 1.865(3) . ? C1 C11 1.536(4) . ? C1 C12 1.539(4) . ? C1 C13 1.542(4) . ? C2 C21 1.529(4) . ? C2 C22 1.545(4) . ? C3 C31 1.530(4) . ? C3 C32 1.531(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 Cl2 Au1 Cl2 179.999(1) 2_576 . ? Cl2 Au1 Cl3 90.35(3) 2_576 2_576 ? Cl2 Au1 Cl3 89.65(3) . 2_576 ? Cl2 Au1 Cl3 89.65(3) 2_576 . ? Cl2 Au1 Cl3 90.35(3) . . ? Cl3 Au1 Cl3 179.998(1) 2_576 . ? Cl4 Au2 Cl4 180.0 . 2_675 ? Cl4 Au2 Cl5 90.41(3) . 2_675 ? Cl4 Au2 Cl5 89.59(3) 2_675 2_675 ? Cl4 Au2 Cl5 89.59(3) . . ? Cl4 Au2 Cl5 90.41(3) 2_675 . ? Cl5 Au2 Cl5 180.0 2_675 . ? Cl1 Se1 P1 98.35(3) . . ? C2 P1 C3 106.87(13) . . ? C2 P1 C1 115.83(12) . . ? C3 P1 C1 111.60(12) . . ? C2 P1 Se1 109.29(9) . . ? C3 P1 Se1 110.43(9) . . ? C1 P1 Se1 102.78(9) . . ? C11 C1 C12 110.2(2) . . ? C11 C1 C13 109.8(2) . . ? C12 C1 C13 108.4(2) . . ? C11 C1 P1 109.60(18) . . ? C12 C1 P1 108.95(18) . . ? C13 C1 P1 109.88(17) . . ? C21 C2 C22 112.3(2) . . ? C21 C2 P1 116.6(2) . . ? C22 C2 P1 110.03(19) . . ? C31 C3 C32 110.5(2) . . ? C31 C3 P1 112.96(19) . . ? C32 C3 P1 112.56(19) . . ? _diffrn_measured_fraction_theta_max 0.938 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 1.747 _refine_diff_density_min -1.749 _refine_diff_density_rms 0.158 _iucr_refine_instructions_details ; TITL Helge in P-1 REM P1 (#1 in standard setting) CELL 0.71073 7.583641 8.760320 15.471904 84.4454 78.6407 67.1281 ZERR 2.00 0.0002 0.0002 0.0006 0.003 0.003 0.003 LATT 1 SFAC C H P Cl Se Au UNIT 20.00 46.00 2.00 10.00 2.00 2.00 L.S. 4 FMAP 2 PLAN 10 TEMP -173 SIZE 0.2 0.2 0.03 ACTA 60 OMIT 0 -1 2 RTAB cont Cl1 Cl3 WGHT 0.030000 1.376700 FVAR 3.51402 AU1 6 0.000000 1.000000 0.500000 10.50000 0.01380 0.01191 = 0.01303 -0.00061 -0.00257 -0.00510 AU2 6 0.500000 1.000000 0.000000 10.50000 0.01021 0.01034 = 0.01658 0.00044 -0.00126 -0.00427 CL1 4 0.146732 0.598269 0.414982 11.00000 0.01702 0.02352 = 0.02318 -0.00141 0.00414 -0.00845 CL2 4 0.210886 0.917812 0.596994 11.00000 0.02461 0.03500 = 0.02281 0.00613 -0.01188 -0.01336 CL3 4 -0.173493 0.855136 0.579677 11.00000 0.02270 0.02081 = 0.02514 0.00304 -0.00135 -0.01213 CL4 4 0.347633 1.198831 0.103711 11.00000 0.01856 0.02063 = 0.02714 -0.00901 -0.00042 -0.00486 CL5 4 0.204910 1.030027 -0.029570 11.00000 0.01307 0.02048 = 0.02878 -0.00012 -0.00509 -0.00738 SE1 5 0.378157 0.425237 0.325139 11.00000 0.01458 0.01411 = 0.02157 0.00256 0.00016 -0.00618 P1 3 0.504521 0.603370 0.251186 11.00000 0.01064 0.01242 = 0.01246 -0.00006 -0.00165 -0.00467 C1 1 0.747828 0.463047 0.195342 11.00000 0.01306 0.01471 = 0.01352 0.00049 -0.00122 -0.00378 C2 1 0.505704 0.748281 0.328731 11.00000 0.01747 0.01863 = 0.01686 -0.00431 -0.00200 -0.00835 AFIX 13 H2 2 0.366046 0.817884 0.349753 11.00000 -1.20000 AFIX 0 C3 1 0.352456 0.727979 0.171022 11.00000 0.01308 0.01339 = 0.01685 0.00097 -0.00442 -0.00393 AFIX 13 H3 2 0.427969 0.788000 0.132395 11.00000 -1.20000 AFIX 0 C11 1 0.813846 0.548630 0.111024 11.00000 0.01660 0.02251 = 0.01594 0.00184 0.00236 -0.00621 AFIX 137 H11A 2 0.810385 0.656276 0.125598 11.00000 -1.50000 H11B 2 0.726589 0.565057 0.068927 11.00000 -1.50000 H11C 2 0.946680 0.479156 0.084754 11.00000 -1.50000 AFIX 0 C12 1 0.893784 0.421773 0.258818 11.00000 0.01177 0.02236 = 0.02480 -0.00141 -0.00558 -0.00300 AFIX 137 H12A 2 1.017898 0.337533 0.232853 11.00000 -1.50000 H12B 2 0.842721 0.379343 0.314998 11.00000 -1.50000 H12C 2 0.913669 0.522161 0.269020 11.00000 -1.50000 AFIX 0 C13 1 0.737127 0.300054 0.171928 11.00000 0.01756 0.01511 = 0.02528 -0.00299 -0.00250 -0.00368 AFIX 137 H13A 2 0.634924 0.325054 0.136544 11.00000 -1.50000 H13B 2 0.707364 0.240615 0.226251 11.00000 -1.50000 H13C 2 0.862293 0.230919 0.138110 11.00000 -1.50000 AFIX 0 C21 1 0.590340 0.672404 0.411873 11.00000 0.02507 0.03845 = 0.01610 -0.00232 -0.00413 -0.01477 AFIX 137 H21A 2 0.732505 0.624837 0.397090 11.00000 -1.50000 H21B 2 0.542815 0.585160 0.436159 11.00000 -1.50000 H21C 2 0.549961 0.758570 0.455673 11.00000 -1.50000 AFIX 0 C22 1 0.597216 0.868922 0.279386 11.00000 0.02421 0.02507 = 0.02573 -0.00422 -0.00171 -0.01520 AFIX 137 H22A 2 0.584220 0.953458 0.319926 11.00000 -1.50000 H22B 2 0.530316 0.922495 0.229972 11.00000 -1.50000 H22C 2 0.735165 0.807342 0.256957 11.00000 -1.50000 AFIX 0 C31 1 0.310568 0.622441 0.110625 11.00000 0.02529 0.02058 = 0.02499 -0.00118 -0.01081 -0.00751 AFIX 137 H31A 2 0.233116 0.563738 0.145803 11.00000 -1.50000 H31B 2 0.433462 0.541804 0.080993 11.00000 -1.50000 H31C 2 0.238300 0.694190 0.066396 11.00000 -1.50000 AFIX 0 C32 1 0.162836 0.860275 0.214942 11.00000 0.01619 0.01924 = 0.02532 0.00083 -0.00607 -0.00168 AFIX 137 H32A 2 0.087522 0.923508 0.169663 11.00000 -1.50000 H32B 2 0.192662 0.935289 0.247454 11.00000 -1.50000 H32C 2 0.086971 0.806695 0.255816 11.00000 -1.50000 HKLF 4 ; # end of cif file