# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Kevin Flower' _publ_contact_author_email K.R.FLOWER@MANCHESTER.AC.UK _publ_section_title ; Isolation of 1,4-Li2-C6H4 and its reaction with [(Ph3P)AuCl] ; _publ_requested_category FM loop_ _publ_author_name 'Kevin Flower' 'Alan T McGown' 'Philip J Miles' 'R Pritchard' 'John E Warren' ##End # CIF produced by WinGX routine CIF_UPDATE # Created on 2007-02-26 at 13:27:00 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.3 # Request file : c:\wingx\files\archive.dat # CIF files read : k dreduc sortav struct data_compound_5 _database_code_depnum_ccdc_archive 'CCDC 688498' #TrackingRef 'Flower1.cif' _audit_creation_date 2007-02-26T13:27:00-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C34 H32 Au1 Br2 P1' _chemical_formula_sum 'C34 H32 Au Br2 P' _chemical_formula_weight 828.35 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.8504(5) _cell_length_b 11.4943(6) _cell_length_c 14.3012(8) _cell_angle_alpha 91.006(3) _cell_angle_beta 110.699(3) _cell_angle_gamma 111.903(2) _cell_volume 1524.93(14) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 4784 _cell_measurement_theta_min 1.018 _cell_measurement_theta_max 25.028 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description parallelopiped _exptl_crystal_colour colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.08 _exptl_crystal_density_diffrn 1.804 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 800 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 7.518 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; R.H. Blessing, Acta Cryst. (1995), A51, 33-38 ; _exptl_absorpt_correction_T_min 0.2614 _exptl_absorpt_correction_T_max 0.5915 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 9 _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 -0.945351E-1 _diffrn_orient_matrix_ub_12 0.3277E-2 _diffrn_orient_matrix_ub_13 -0.98943E-2 _diffrn_orient_matrix_ub_21 0.233498E-1 _diffrn_orient_matrix_ub_22 0.33136E-2 _diffrn_orient_matrix_ub_23 0.744513E-1 _diffrn_orient_matrix_ub_31 0.461977E-1 _diffrn_orient_matrix_ub_32 0.950746E-1 _diffrn_orient_matrix_ub_33 0.108236E-1 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.137 _diffrn_reflns_av_unetI/netI 0.1621 _diffrn_reflns_number 5179 _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 0 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.02 _diffrn_reflns_theta_max 24.88 _diffrn_reflns_theta_full 24.88 _diffrn_measured_fraction_theta_full 0.979 _diffrn_measured_fraction_theta_max 0.979 _reflns_number_total 5179 _reflns_number_gt 3021 _reflns_threshold_expression >2sigma(I) _diffrn_reflns_reduction_process ; Scaled and merged with SORTAV R.H. Blessing, (1987) Cryst. Rev. 1, 3-58 R.H. Blessing, (1989) J. Appl. Cryst. 22, 396-397 ; #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. High esd on bonds due to the crystal being a thin plate and hence poor diffractor. ; _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^)+(0.1283P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 5179 _refine_ls_number_parameters 343 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1429 _refine_ls_R_factor_gt 0.0789 _refine_ls_wR_factor_ref 0.2379 _refine_ls_wR_factor_gt 0.192 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.022 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 2.835 _refine_diff_density_min -1.907 _refine_diff_density_rms 0.251 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Au Au -1.9162 8.821 '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' Br Br -0.291 2.4679 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.7042(16) 0.4149(15) 0.9489(11) 0.046(4) Uani 1 1 d . . . C2 C 0.6662(18) 0.4936(16) 0.9931(12) 0.052(4) Uani 1 1 d . . . H2 H 0.6196 0.5402 0.9511 0.063 Uiso 1 1 calc R . . C3 C 0.6903(17) 0.5112(17) 1.0957(12) 0.052(4) Uani 1 1 d . . . H3 H 0.6632 0.5681 1.1244 0.062 Uiso 1 1 calc R . . C4 C 0.7570(18) 0.4392(18) 1.1527(12) 0.061(5) Uani 1 1 d . . . H4 H 0.7755 0.4461 1.2231 0.073 Uiso 1 1 calc R . . C5 C 0.7975(19) 0.3581(17) 1.1103(12) 0.058(4) Uani 1 1 d . . . H5 H 0.8454 0.3116 1.1514 0.069 Uiso 1 1 calc R . . C6 C 0.767(2) 0.3446(17) 1.0050(12) 0.063(5) Uani 1 1 d . . . H6 H 0.7907 0.2865 0.9743 0.075 Uiso 1 1 calc R . . C7 C 0.7053(14) 0.2663(13) 0.7796(9) 0.033(3) Uani 1 1 d . . . C8 C 0.8591(16) 0.3068(17) 0.8158(11) 0.050(4) Uani 1 1 d . . . H8 H 0.9237 0.3924 0.846 0.06 Uiso 1 1 calc R . . C9 C 0.9090(19) 0.2113(19) 0.8038(13) 0.063(5) Uani 1 1 d . . . H9 H 1.0088 0.2327 0.8215 0.075 Uiso 1 1 calc R . . C10 C 0.813(2) 0.091(2) 0.7672(14) 0.068(5) Uani 1 1 d . . . H10 H 0.8441 0.0244 0.7645 0.081 Uiso 1 1 calc R . . C11 C 0.673(2) 0.0643(19) 0.7349(14) 0.066(5) Uani 1 1 d . . . H11 H 0.6085 -0.0209 0.703 0.079 Uiso 1 1 calc R . . C12 C 0.6126(17) 0.1466(15) 0.7427(12) 0.052(4) Uani 1 1 d . . . H12 H 0.5117 0.1203 0.7232 0.063 Uiso 1 1 calc R . . C13 C 0.4662(16) 0.3409(15) 0.7555(10) 0.047(4) Uani 1 1 d . . . C14 C 0.3989(15) 0.3938(14) 0.6799(10) 0.043(3) Uani 1 1 d . . . H14 H 0.4556 0.4623 0.6566 0.051 Uiso 1 1 calc R . . C15 C 0.2502(15) 0.3504(15) 0.6363(13) 0.052(4) Uani 1 1 d . . . H15 H 0.2059 0.3894 0.5845 0.063 Uiso 1 1 calc R . . C16 C 0.1668(17) 0.2495(17) 0.6690(11) 0.053(4) Uani 1 1 d . . . H16 H 0.0646 0.2162 0.638 0.063 Uiso 1 1 calc R . . C17 C 0.233(2) 0.1981(17) 0.7465(12) 0.059(4) Uani 1 1 d . . . H17 H 0.1765 0.1317 0.7713 0.071 Uiso 1 1 calc R . . C18 C 0.3804(16) 0.2404(18) 0.7891(12) 0.057(4) Uani 1 1 d . . . H18 H 0.4242 0.2017 0.8414 0.068 Uiso 1 1 calc R . . C19 C 0.7596(17) 0.7088(16) 0.8504(11) 0.051(4) Uani 1 1 d . . . C20 C 0.8701(17) 0.7863(17) 0.9349(12) 0.054(4) Uani 1 1 d . . . H20 H 0.961 0.7816 0.9528 0.064 Uiso 1 1 calc R . . C21 C 0.8583(19) 0.8706(17) 0.9958(14) 0.057(4) Uani 1 1 d . . . H21 H 0.937 0.9201 1.0564 0.069 Uiso 1 1 calc R . . C22 C 0.728(2) 0.8817(16) 0.9664(14) 0.068(5) Uani 1 1 d . . . C23 C 0.6096(17) 0.8072(15) 0.8814(13) 0.059(4) Uani 1 1 d . . . H23 H 0.5203 0.815 0.8635 0.071 Uiso 1 1 calc R . . C24 C 0.626(2) 0.7192(16) 0.8222(14) 0.059(4) Uani 1 1 d . . . H24 H 0.5465 0.6664 0.763 0.071 Uiso 1 1 calc R . . C25 C 0.7639(17) 0.4729(14) 0.6276(12) 0.050(4) Uani 1 1 d . . . C26 C 0.6373(19) 0.3979(18) 0.5506(13) 0.064(5) Uani 1 1 d . . . H26 H 0.5502 0.397 0.5523 0.077 Uiso 1 1 calc R . . C27 C 0.629(2) 0.3218(19) 0.4688(13) 0.066(5) Uani 1 1 d . . . H27 H 0.5389 0.2707 0.4164 0.079 Uiso 1 1 calc R . . C28 C 0.7510(19) 0.3230(17) 0.4667(12) 0.055(4) Uani 1 1 d . . . C29 C 0.887(2) 0.398(2) 0.5432(15) 0.079(6) Uani 1 1 d . . . H29 H 0.9737 0.4007 0.5402 0.094 Uiso 1 1 calc R . . C30 C 0.8867(18) 0.468(2) 0.6216(13) 0.078(6) Uani 1 1 d . . . H30 H 0.9766 0.5151 0.6757 0.093 Uiso 1 1 calc R . . C31 C 0.8789(18) 0.7461(14) 0.6943(11) 0.046(4) Uani 1 1 d . . . H31A H 0.9419 0.817 0.7523 0.056 Uiso 1 1 calc R . . H31B H 0.9411 0.7267 0.6655 0.056 Uiso 1 1 calc R . . C32 C 0.7784(16) 0.7869(17) 0.6160(13) 0.061(5) Uani 1 1 d . . . H32A H 0.7197 0.8111 0.6456 0.073 Uiso 1 1 calc R . . H32B H 0.7123 0.7151 0.5591 0.073 Uiso 1 1 calc R . . C33 C 0.8618(19) 0.9011(15) 0.5756(12) 0.057(4) Uani 1 1 d . . . H33A H 0.9322 0.9709 0.6332 0.068 Uiso 1 1 calc R . . H33B H 0.9161 0.8751 0.5426 0.068 Uiso 1 1 calc R . . C34 C 0.760(2) 0.9495(19) 0.4990(13) 0.067(5) Uani 1 1 d . . . H34A H 0.816 1.0209 0.4742 0.101 Uiso 1 1 calc R . . H34B H 0.7083 0.9778 0.532 0.101 Uiso 1 1 calc R . . H34C H 0.6903 0.8806 0.4418 0.101 Uiso 1 1 calc R . . Au1 Au 0.76971(7) 0.58418(6) 0.74682(5) 0.0537(3) Uani 1 1 d . . . P1 P 0.6619(4) 0.3998(4) 0.8107(3) 0.0456(10) Uani 1 1 d . . . Br1 Br 0.7443(2) 0.2214(2) 0.35363(14) 0.0738(6) Uani 1 1 d . . . Br2 Br 0.7118(2) 1.0078(2) 1.04654(15) 0.0743(6) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.035(8) 0.046(9) 0.061(8) 0.015(7) 0.021(7) 0.017(7) C2 0.051(10) 0.050(10) 0.063(9) 0.022(8) 0.021(8) 0.029(9) C3 0.048(10) 0.062(11) 0.067(9) 0.015(8) 0.028(8) 0.038(9) C4 0.044(10) 0.069(13) 0.053(8) -0.003(8) 0.021(8) 0.003(9) C5 0.064(11) 0.065(12) 0.064(9) 0.039(9) 0.031(8) 0.040(10) C6 0.080(13) 0.057(11) 0.056(9) 0.026(8) 0.022(9) 0.036(10) C7 0.035(8) 0.032(8) 0.045(7) 0.031(6) 0.022(6) 0.020(7) C8 0.040(9) 0.057(11) 0.060(8) 0.025(8) 0.021(7) 0.025(8) C9 0.038(10) 0.069(13) 0.083(11) 0.013(10) 0.024(8) 0.023(10) C10 0.055(12) 0.071(14) 0.075(11) 0.009(10) 0.017(9) 0.031(11) C11 0.062(12) 0.051(11) 0.084(11) 0.004(9) 0.019(10) 0.031(10) C12 0.040(9) 0.037(10) 0.091(11) 0.022(8) 0.035(8) 0.018(8) C13 0.041(9) 0.043(9) 0.051(8) 0.013(7) 0.006(7) 0.021(8) C14 0.036(8) 0.035(8) 0.057(8) 0.006(7) 0.017(7) 0.016(7) C15 0.024(8) 0.043(10) 0.092(11) 0.010(8) 0.013(8) 0.023(7) C16 0.045(9) 0.065(12) 0.065(9) 0.026(8) 0.024(8) 0.036(9) C17 0.073(13) 0.047(10) 0.073(10) 0.020(8) 0.039(10) 0.032(10) C18 0.033(9) 0.068(12) 0.065(9) 0.012(9) 0.007(7) 0.025(9) C19 0.046(10) 0.057(11) 0.057(9) 0.039(8) 0.024(8) 0.022(8) C20 0.031(8) 0.062(11) 0.065(9) 0.028(9) 0.012(8) 0.020(8) C21 0.050(10) 0.049(11) 0.083(11) 0.016(9) 0.025(9) 0.032(9) C22 0.096(16) 0.029(9) 0.078(11) 0.016(8) 0.042(11) 0.018(10) C23 0.035(9) 0.032(9) 0.087(11) 0.007(9) 0.008(8) 0.003(8) C24 0.059(11) 0.040(10) 0.079(11) 0.021(9) 0.026(9) 0.020(9) C25 0.042(9) 0.022(8) 0.075(10) 0.015(7) 0.017(8) 0.007(7) C26 0.045(10) 0.066(13) 0.080(11) 0.006(10) 0.037(9) 0.010(9) C27 0.050(11) 0.075(14) 0.069(10) 0.010(9) 0.024(9) 0.021(10) C28 0.054(11) 0.062(12) 0.060(9) 0.016(8) 0.027(8) 0.031(9) C29 0.054(12) 0.103(18) 0.091(13) 0.029(12) 0.028(10) 0.045(12) C30 0.034(10) 0.130(19) 0.059(10) -0.007(11) -0.001(8) 0.043(12) C31 0.059(10) 0.030(8) 0.059(8) 0.012(7) 0.033(8) 0.018(8) C32 0.028(8) 0.061(12) 0.074(10) 0.019(9) 0.008(8) 0.008(8) C33 0.062(11) 0.038(10) 0.069(10) 0.019(8) 0.027(8) 0.017(9) C34 0.062(12) 0.073(13) 0.065(10) 0.022(9) 0.020(9) 0.028(11) Au1 0.0428(4) 0.0544(5) 0.0671(4) 0.0180(3) 0.0216(3) 0.0225(3) P1 0.038(2) 0.047(3) 0.059(2) 0.0137(19) 0.0198(18) 0.023(2) Br1 0.0835(14) 0.0808(14) 0.0783(11) 0.0241(10) 0.0418(10) 0.0451(12) Br2 0.0872(15) 0.0604(13) 0.0882(12) 0.0198(10) 0.0437(11) 0.0343(11) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C6 1.34(2) . ? C1 C2 1.35(2) . ? C1 P1 1.853(15) . ? C2 C3 1.39(2) . ? C2 H2 0.95 . ? C3 C4 1.39(2) . ? C3 H3 0.95 . ? C4 C5 1.38(2) . ? C4 H4 0.95 . ? C5 C6 1.41(2) . ? C5 H5 0.95 . ? C6 H6 0.95 . ? C7 C12 1.32(2) . ? C7 C8 1.439(19) . ? C7 P1 1.854(14) . ? C8 C9 1.42(2) . ? C8 H8 0.95 . ? C9 C10 1.34(3) . ? C9 H9 0.95 . ? C10 C11 1.33(3) . ? C10 H10 0.95 . ? C11 C12 1.36(2) . ? C11 H11 0.95 . ? C12 H12 0.95 . ? C13 C14 1.367(19) . ? C13 C18 1.40(2) . ? C13 P1 1.821(15) . ? C14 C15 1.38(2) . ? C14 H14 0.95 . ? C15 C16 1.38(2) . ? C15 H15 0.95 . ? C16 C17 1.37(2) . ? C16 H16 0.95 . ? C17 C18 1.37(2) . ? C17 H17 0.95 . ? C18 H18 0.95 . ? C19 C20 1.35(2) . ? C19 C24 1.41(2) . ? C19 Au1 2.101(18) . ? C20 C21 1.36(2) . ? C20 H20 0.95 . ? C21 C22 1.38(3) . ? C21 H21 0.95 . ? C22 C23 1.38(2) . ? C22 Br2 1.929(18) . ? C23 C24 1.41(2) . ? C23 H23 0.95 . ? C24 H24 0.95 . ? C25 C26 1.36(2) . ? C25 C30 1.39(2) . ? C25 Au1 2.082(17) . ? C26 C27 1.41(2) . ? C26 H26 0.95 . ? C27 C28 1.33(2) . ? C27 H27 0.95 . ? C28 C29 1.41(3) . ? C28 Br1 1.942(16) . ? C29 C30 1.36(3) . ? C29 H29 0.95 . ? C30 H30 0.95 . ? C31 C32 1.48(2) . ? C31 Au1 2.114(14) . ? C31 H31A 0.99 . ? C31 H31B 0.99 . ? C32 C33 1.54(2) . ? C32 H32A 0.99 . ? C32 H32B 0.99 . ? C33 C34 1.54(2) . ? C33 H33A 0.99 . ? C33 H33B 0.99 . ? C34 H34A 0.98 . ? C34 H34B 0.98 . ? C34 H34C 0.98 . ? Au1 P1 2.381(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C6 C1 C2 119.5(15) . . ? C6 C1 P1 120.8(13) . . ? C2 C1 P1 119.7(12) . . ? C1 C2 C3 124.8(15) . . ? C1 C2 H2 117.6 . . ? C3 C2 H2 117.6 . . ? C4 C3 C2 114.8(14) . . ? C4 C3 H3 122.6 . . ? C2 C3 H3 122.6 . . ? C5 C4 C3 122.0(15) . . ? C5 C4 H4 119 . . ? C3 C4 H4 119 . . ? C4 C5 C6 119.4(15) . . ? C4 C5 H5 120.3 . . ? C6 C5 H5 120.3 . . ? C1 C6 C5 119.4(17) . . ? C1 C6 H6 120.3 . . ? C5 C6 H6 120.3 . . ? C12 C7 C8 123.4(14) . . ? C12 C7 P1 126.0(11) . . ? C8 C7 P1 109.9(11) . . ? C9 C8 C7 116.3(15) . . ? C9 C8 H8 121.9 . . ? C7 C8 H8 121.9 . . ? C10 C9 C8 118.7(16) . . ? C10 C9 H9 120.6 . . ? C8 C9 H9 120.6 . . ? C11 C10 C9 120(2) . . ? C11 C10 H10 120.1 . . ? C9 C10 H10 120.1 . . ? C10 C11 C12 127(2) . . ? C10 C11 H11 116.7 . . ? C12 C11 H11 116.7 . . ? C7 C12 C11 114.8(15) . . ? C7 C12 H12 122.6 . . ? C11 C12 H12 122.6 . . ? C14 C13 C18 118.2(14) . . ? C14 C13 P1 120.7(12) . . ? C18 C13 P1 121.1(11) . . ? C13 C14 C15 121.8(15) . . ? C13 C14 H14 119.1 . . ? C15 C14 H14 119.1 . . ? C14 C15 C16 119.4(15) . . ? C14 C15 H15 120.3 . . ? C16 C15 H15 120.3 . . ? C17 C16 C15 119.2(15) . . ? C17 C16 H16 120.4 . . ? C15 C16 H16 120.4 . . ? C18 C17 C16 121.4(17) . . ? C18 C17 H17 119.3 . . ? C16 C17 H17 119.3 . . ? C17 C18 C13 120.0(15) . . ? C17 C18 H18 120 . . ? C13 C18 H18 120 . . ? C20 C19 C24 117.9(17) . . ? C20 C19 Au1 126.6(13) . . ? C24 C19 Au1 115.2(12) . . ? C19 C20 C21 123.7(16) . . ? C19 C20 H20 118.2 . . ? C21 C20 H20 118.2 . . ? C20 C21 C22 117.8(17) . . ? C20 C21 H21 121.1 . . ? C22 C21 H21 121.1 . . ? C23 C22 C21 122.6(18) . . ? C23 C22 Br2 118.7(16) . . ? C21 C22 Br2 118.7(14) . . ? C22 C23 C24 117.5(17) . . ? C22 C23 H23 121.2 . . ? C24 C23 H23 121.2 . . ? C23 C24 C19 120.4(17) . . ? C23 C24 H24 119.8 . . ? C19 C24 H24 119.8 . . ? C26 C25 C30 115.4(16) . . ? C26 C25 Au1 121.6(13) . . ? C30 C25 Au1 123.0(12) . . ? C25 C26 C27 123.2(17) . . ? C25 C26 H26 118.4 . . ? C27 C26 H26 118.4 . . ? C28 C27 C26 118.3(17) . . ? C28 C27 H27 120.9 . . ? C26 C27 H27 120.9 . . ? C27 C28 C29 122.1(17) . . ? C27 C28 Br1 119.4(14) . . ? C29 C28 Br1 118.4(13) . . ? C30 C29 C28 116.6(17) . . ? C30 C29 H29 121.7 . . ? C28 C29 H29 121.7 . . ? C29 C30 C25 124.3(17) . . ? C29 C30 H30 117.9 . . ? C25 C30 H30 117.9 . . ? C32 C31 Au1 112.4(11) . . ? C32 C31 H31A 109.1 . . ? Au1 C31 H31A 109.1 . . ? C32 C31 H31B 109.1 . . ? Au1 C31 H31B 109.1 . . ? H31A C31 H31B 107.9 . . ? C31 C32 C33 110.9(13) . . ? C31 C32 H32A 109.5 . . ? C33 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? C33 C32 H32B 109.5 . . ? H32A C32 H32B 108 . . ? C34 C33 C32 111.6(14) . . ? C34 C33 H33A 109.3 . . ? C32 C33 H33A 109.3 . . ? C34 C33 H33B 109.3 . . ? C32 C33 H33B 109.3 . . ? H33A C33 H33B 108 . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C25 Au1 C19 171.5(5) . . ? C25 Au1 C31 87.7(6) . . ? C19 Au1 C31 87.6(6) . . ? C25 Au1 P1 91.3(4) . . ? C19 Au1 P1 93.9(4) . . ? C31 Au1 P1 176.0(4) . . ? C13 P1 C1 103.1(7) . . ? C13 P1 C7 106.1(7) . . ? C1 P1 C7 105.1(6) . . ? C13 P1 Au1 111.1(5) . . ? C1 P1 Au1 118.1(5) . . ? C7 P1 Au1 112.2(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 C3 2(3) . . . . ? P1 C1 C2 C3 179.0(13) . . . . ? C1 C2 C3 C4 -1(3) . . . . ? C2 C3 C4 C5 1(2) . . . . ? C3 C4 C5 C6 -2(3) . . . . ? C2 C1 C6 C5 -3(3) . . . . ? P1 C1 C6 C5 -179.8(13) . . . . ? C4 C5 C6 C1 3(3) . . . . ? C12 C7 C8 C9 4(2) . . . . ? P1 C7 C8 C9 175.6(11) . . . . ? C7 C8 C9 C10 -5(2) . . . . ? C8 C9 C10 C11 6(3) . . . . ? C9 C10 C11 C12 -6(3) . . . . ? C8 C7 C12 C11 -4(2) . . . . ? P1 C7 C12 C11 -174.3(12) . . . . ? C10 C11 C12 C7 5(3) . . . . ? C18 C13 C14 C15 0(2) . . . . ? P1 C13 C14 C15 179.7(12) . . . . ? C13 C14 C15 C16 -1(2) . . . . ? C14 C15 C16 C17 3(2) . . . . ? C15 C16 C17 C18 -3(2) . . . . ? C16 C17 C18 C13 2(2) . . . . ? C14 C13 C18 C17 0(2) . . . . ? P1 C13 C18 C17 179.8(12) . . . . ? C24 C19 C20 C21 2(2) . . . . ? Au1 C19 C20 C21 175.9(12) . . . . ? C19 C20 C21 C22 -3(3) . . . . ? C20 C21 C22 C23 3(3) . . . . ? C20 C21 C22 Br2 -176.2(12) . . . . ? C21 C22 C23 C24 -2(3) . . . . ? Br2 C22 C23 C24 177.7(12) . . . . ? C22 C23 C24 C19 0(2) . . . . ? C20 C19 C24 C23 0(2) . . . . ? Au1 C19 C24 C23 -174.9(12) . . . . ? C30 C25 C26 C27 -1(3) . . . . ? Au1 C25 C26 C27 179.9(14) . . . . ? C25 C26 C27 C28 0(3) . . . . ? C26 C27 C28 C29 0(3) . . . . ? C26 C27 C28 Br1 -178.9(13) . . . . ? C27 C28 C29 C30 2(3) . . . . ? Br1 C28 C29 C30 -179.5(16) . . . . ? C28 C29 C30 C25 -3(3) . . . . ? C26 C25 C30 C29 3(3) . . . . ? Au1 C25 C30 C29 -178.1(17) . . . . ? Au1 C31 C32 C33 -177.2(11) . . . . ? C31 C32 C33 C34 -176.7(15) . . . . ? C26 C25 Au1 C19 -57(4) . . . . ? C30 C25 Au1 C19 124(4) . . . . ? C26 C25 Au1 C31 -114.4(14) . . . . ? C30 C25 Au1 C31 67.1(16) . . . . ? C26 C25 Au1 P1 69.5(13) . . . . ? C30 C25 Au1 P1 -109.0(16) . . . . ? C20 C19 Au1 C25 -130(4) . . . . ? C24 C19 Au1 C25 44(4) . . . . ? C20 C19 Au1 C31 -73.4(14) . . . . ? C24 C19 Au1 C31 100.6(12) . . . . ? C20 C19 Au1 P1 102.9(13) . . . . ? C24 C19 Au1 P1 -83.1(11) . . . . ? C32 C31 Au1 C25 87.4(12) . . . . ? C32 C31 Au1 C19 -85.4(12) . . . . ? C32 C31 Au1 P1 163(5) . . . . ? C14 C13 P1 C1 133.6(13) . . . . ? C18 C13 P1 C1 -46.4(15) . . . . ? C14 C13 P1 C7 -116.1(12) . . . . ? C18 C13 P1 C7 63.9(14) . . . . ? C14 C13 P1 Au1 6.2(14) . . . . ? C18 C13 P1 Au1 -173.8(12) . . . . ? C6 C1 P1 C13 116.9(15) . . . . ? C2 C1 P1 C13 -60.3(15) . . . . ? C6 C1 P1 C7 6.0(16) . . . . ? C2 C1 P1 C7 -171.3(13) . . . . ? C6 C1 P1 Au1 -120.1(14) . . . . ? C2 C1 P1 Au1 62.6(14) . . . . ? C12 C7 P1 C13 -11.9(14) . . . . ? C8 C7 P1 C13 176.9(9) . . . . ? C12 C7 P1 C1 96.9(13) . . . . ? C8 C7 P1 C1 -74.4(10) . . . . ? C12 C7 P1 Au1 -133.5(11) . . . . ? C8 C7 P1 Au1 55.3(9) . . . . ? C25 Au1 P1 C13 -89.8(7) . . . . ? C19 Au1 P1 C13 83.3(7) . . . . ? C31 Au1 P1 C13 -165(6) . . . . ? C25 Au1 P1 C1 151.4(7) . . . . ? C19 Au1 P1 C1 -35.4(7) . . . . ? C31 Au1 P1 C1 76(6) . . . . ? C25 Au1 P1 C7 28.8(6) . . . . ? C19 Au1 P1 C7 -158.0(6) . . . . ? C31 Au1 P1 C7 -47(6) . . . . ? ##End # Attachment 'Flower1.cif' #\#isolation of 1,4-Li2-C6H6 and its reaction.....k.r.flower et al sub to Dalton trans # CIF produced by WinGX routine CIF_UPDATE # Created on 2008-02-29 at 11:21:33 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.3 # Request file : c:\chem\wingx\files\archive.dat # CIF files read : h1abs14 struct final data_h1abs14 _database_code_depnum_ccdc_archive 'CCDC 756405' #TrackingRef 'Flower1.cif' _audit_creation_date 2008-02-29T11:21:33-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ? _chemical_formula_moiety 'C21 H17 Au P, C0.9 H1.8 Cl1.80' _chemical_formula_sum 'C21.90 H18.80 Au Cl1.80 P' _chemical_formula_weight 573.93 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_Int_Tables_number 14 _symmetry_space_group_name_Hall '-P 2yn' 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 8.2662(5) _cell_length_b 17.3899(11) _cell_length_c 14.2615(9) _cell_angle_alpha 90 _cell_angle_beta 91.4370(10) _cell_angle_gamma 90 _cell_volume 2049.4(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 7028 _cell_measurement_theta_min 4.423 _cell_measurement_theta_max 58.92 _cell_measurement_wavelength 0.671 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.07 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.03 _exptl_crystal_density_diffrn 1.86 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1100 _exptl_special_details ; Distance AUCL 3.6331 (0.0020) Au1 - Cl1S Beam decay, scaling and absorption correction undertaken using SADABS-2004/1 (Bruker-Nonius, 2004) >From 3 independent data collections this sample contained the smallest residual Q-peaks all located around Au(1). The use of other absorption correction programs and settings for SADABS failed to reduce these peaks. SADABS was run with the "strong" correction setting. Data collection utilised 0.1 degree slicing. ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 6.436 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS-2004/1 (Bruker-Nonius, 2004)' _exptl_absorpt_correction_T_min 0.6615 _exptl_absorpt_correction_T_max 0.8557 _diffrn_radiation_probe x-ray _diffrn_radiation_type synchrotron _diffrn_radiation_wavelength 0.671 _diffrn_source synchrotron _diffrn_radiation_collimation '0.2 mm double-pinhole' #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source_type 'Station 9.8, SRS, Daresbury' _diffrn_radiation_monochromator 'Silicon 111' _diffrn_ambient_temperature 150(2) _diffrn_measurement_device 'APEXII CCD camera on D8 diffractometer' _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'omega rotation' _diffrn_reflns_av_R_equivalents 0.0301 _diffrn_reflns_av_unetI/netI 0.0295 _diffrn_reflns_number 21858 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.74 _diffrn_reflns_theta_max 27.77 _diffrn_reflns_theta_full 27.77 _diffrn_measured_fraction_theta_full 0.991 _diffrn_measured_fraction_theta_max 0.991 _reflns_number_total 5700 _reflns_number_gt 4438 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'APEXII (Bruker, 2004)' _computing_cell_refinement 'APEXII (Bruker, 2004)' _computing_data_reduction 'SAINT v7.34a (Bruker, 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 2001)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0464P)^2^+1.8155P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 5700 _refine_ls_number_parameters 233 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0495 _refine_ls_R_factor_gt 0.0327 _refine_ls_wR_factor_ref 0.084 _refine_ls_wR_factor_gt 0.0761 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.039 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0 _refine_diff_density_max 2.158 _refine_diff_density_min -0.771 _refine_diff_density_rms 0.151 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C -0.002 0.0014 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Au Au -1.7731 8.0564 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1134 0.1425 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Au1 Au 0.11509(2) 0.870876(9) 0.175697(11) 0.02979(6) Uani 1 1 d . . . P1 P 0.19339(14) 0.77589(7) 0.27871(7) 0.0275(2) Uani 1 1 d . . . C1 C 0.0470(6) 0.9493(3) 0.0757(3) 0.0319(9) Uani 1 1 d . . . C2 C -0.1021(6) 0.9423(3) 0.0274(3) 0.0345(10) Uani 1 1 d . . . H2 H -0.1747 0.9027 0.0447 0.041 Uiso 1 1 calc R . . C3 C -0.1465(6) 0.9921(3) -0.0453(3) 0.0336(10) Uani 1 1 d . . . H3 H -0.2494 0.9856 -0.0754 0.04 Uiso 1 1 calc R . . C4 C 0.3133(5) 0.8077(3) 0.3801(3) 0.0287(9) Uani 1 1 d . . . C5 C 0.4256(6) 0.7612(3) 0.4255(3) 0.0371(10) Uani 1 1 d . . . H5 H 0.444 0.7105 0.4034 0.045 Uiso 1 1 calc R . . C6 C 0.5119(7) 0.7885(3) 0.5035(4) 0.0456(13) Uani 1 1 d . . . H6 H 0.5892 0.7564 0.5346 0.055 Uiso 1 1 calc R . . C7 C 0.4858(7) 0.8618(3) 0.5359(4) 0.0453(13) Uani 1 1 d . . . H7 H 0.5454 0.8801 0.5892 0.054 Uiso 1 1 calc R . . C8 C 0.3736(7) 0.9089(3) 0.4914(4) 0.0415(12) Uani 1 1 d . . . H8 H 0.3557 0.9595 0.5139 0.05 Uiso 1 1 calc R . . C9 C 0.2873(6) 0.8820(3) 0.4137(3) 0.0372(10) Uani 1 1 d . . . H9 H 0.2099 0.9143 0.383 0.045 Uiso 1 1 calc R . . C10 C 0.0263(5) 0.7218(3) 0.3259(3) 0.0294(9) Uani 1 1 d . . . C11 C 0.0381(6) 0.6822(3) 0.4100(3) 0.0339(10) Uani 1 1 d . . . H11 H 0.134 0.6857 0.4478 0.041 Uiso 1 1 calc R . . C12 C -0.0915(7) 0.6369(3) 0.4393(4) 0.0380(11) Uani 1 1 d . . . H12 H -0.082 0.6083 0.4959 0.046 Uiso 1 1 calc R . . C13 C -0.2327(6) 0.6340(3) 0.3858(4) 0.0406(11) Uani 1 1 d . . . H13 H -0.3213 0.6041 0.4062 0.049 Uiso 1 1 calc R . . C14 C -0.2456(6) 0.6744(3) 0.3026(4) 0.0431(12) Uani 1 1 d . . . H14 H -0.343 0.6723 0.266 0.052 Uiso 1 1 calc R . . C15 C -0.1168(6) 0.7180(3) 0.2726(4) 0.0384(11) Uani 1 1 d . . . H15 H -0.1261 0.7455 0.2151 0.046 Uiso 1 1 calc R . . C16 C 0.3104(5) 0.7031(3) 0.2185(3) 0.0297(9) Uani 1 1 d . . . C17 C 0.3971(6) 0.7240(3) 0.1403(3) 0.0399(11) Uani 1 1 d . . . H17 H 0.3987 0.7763 0.1212 0.048 Uiso 1 1 calc R . . C18 C 0.4812(8) 0.6700(3) 0.0897(4) 0.0480(14) Uani 1 1 d . . . H18 H 0.5414 0.6854 0.037 0.058 Uiso 1 1 calc R . . C19 C 0.4777(7) 0.5932(3) 0.1157(4) 0.0444(12) Uani 1 1 d . . . H19 H 0.5323 0.5557 0.0798 0.053 Uiso 1 1 calc R . . C20 C 0.3945(6) 0.5715(3) 0.1942(4) 0.0400(11) Uani 1 1 d . . . H20 H 0.3947 0.5193 0.2136 0.048 Uiso 1 1 calc R . . C21 C 0.3109(5) 0.6257(2) 0.2446(3) 0.0352(10) Uani 1 1 d . . . H21 H 0.2528 0.6101 0.298 0.042 Uiso 1 1 calc R . . C1S C 0.7103(5) 0.9735(2) 0.2598(3) 0.0550(17) Uani 0.907(5) 1 d PR . . H1S1 H 0.7045 1.0269 0.2835 0.066 Uiso 0.907(5) 1 calc PR . . H1S2 H 0.7917 0.9722 0.21 0.066 Uiso 0.907(5) 1 calc PR . . Cl1S Cl 0.5208(3) 0.94767(16) 0.21098(16) 0.0797(8) Uani 0.907(5) 1 d P . . Cl2S Cl 0.7742(2) 0.91215(10) 0.35236(13) 0.0569(6) Uani 0.907(5) 1 d P . . 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 0.03585(10) 0.03107(10) 0.02223(8) 0.00370(7) -0.00376(6) 0.00462(7) P1 0.0284(5) 0.0322(6) 0.0216(5) 0.0038(4) -0.0028(4) 0.0020(4) C1 0.047(3) 0.027(2) 0.0212(19) -0.0008(16) -0.0057(18) 0.0039(19) C2 0.043(3) 0.036(2) 0.024(2) -0.0022(18) -0.0047(18) 0.004(2) C3 0.036(2) 0.039(2) 0.025(2) -0.0038(18) -0.0073(17) 0.0072(19) C4 0.033(2) 0.031(2) 0.0225(19) 0.0083(16) -0.0016(16) -0.0061(17) C5 0.037(2) 0.043(3) 0.031(2) 0.006(2) -0.0100(19) 0.001(2) C6 0.043(3) 0.053(3) 0.040(3) 0.007(2) -0.015(2) -0.005(2) C7 0.041(3) 0.065(4) 0.029(2) -0.002(2) -0.007(2) -0.014(3) C8 0.047(3) 0.044(3) 0.034(2) -0.004(2) 0.001(2) -0.012(2) C9 0.037(2) 0.040(3) 0.034(2) 0.002(2) 0.0010(19) -0.002(2) C10 0.032(2) 0.033(2) 0.0238(19) 0.0020(17) -0.0004(16) -0.0006(17) C11 0.031(2) 0.042(3) 0.029(2) 0.0040(19) -0.0040(18) -0.0026(19) C12 0.042(3) 0.040(3) 0.032(2) -0.0010(19) 0.005(2) -0.006(2) C13 0.035(3) 0.043(3) 0.044(3) 0.000(2) 0.008(2) -0.004(2) C14 0.029(2) 0.052(3) 0.048(3) 0.001(2) -0.005(2) -0.005(2) C15 0.034(2) 0.043(3) 0.037(3) 0.005(2) -0.003(2) 0.002(2) C16 0.028(2) 0.036(2) 0.0245(19) 0.0015(17) -0.0035(16) 0.0012(17) C17 0.042(3) 0.045(3) 0.033(2) 0.009(2) 0.005(2) 0.008(2) C18 0.057(3) 0.054(3) 0.035(3) 0.009(2) 0.018(2) 0.009(3) C19 0.050(3) 0.048(3) 0.035(3) -0.006(2) -0.001(2) 0.013(2) C20 0.041(3) 0.035(3) 0.044(3) -0.003(2) -0.002(2) -0.001(2) C21 0.036(2) 0.035(2) 0.034(2) -0.0001(19) 0.0006(18) -0.0041(19) C1S 0.052(4) 0.065(4) 0.048(4) 0.005(3) 0.002(3) -0.014(3) Cl1S 0.0606(12) 0.1118(19) 0.0662(13) 0.0178(12) -0.0073(9) -0.0285(12) Cl2S 0.0660(12) 0.0482(10) 0.0569(10) 0.0049(7) 0.0094(8) 0.0028(7) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Au1 C1 2.041(4) . ? Au1 P1 2.2930(11) . ? P1 C10 1.814(5) . ? P1 C4 1.818(4) . ? P1 C16 1.821(5) . ? C1 C3 1.386(7) 3_575 ? C1 C2 1.403(7) . ? C2 C3 1.393(6) . ? C2 H2 0.95 . ? C3 C1 1.386(7) 3_575 ? C3 H3 0.95 . ? C4 C5 1.381(6) . ? C4 C9 1.397(7) . ? C5 C6 1.391(7) . ? C5 H5 0.95 . ? C6 C7 1.374(8) . ? C6 H6 0.95 . ? C7 C8 1.381(8) . ? C7 H7 0.95 . ? C8 C9 1.384(7) . ? C8 H8 0.95 . ? C9 H9 0.95 . ? C10 C11 1.384(6) . ? C10 C15 1.392(6) . ? C11 C12 1.402(7) . ? C11 H11 0.95 . ? C12 C13 1.380(8) . ? C12 H12 0.95 . ? C13 C14 1.381(8) . ? C13 H13 0.95 . ? C14 C15 1.384(7) . ? C14 H14 0.95 . ? C15 H15 0.95 . ? C16 C17 1.389(7) . ? C16 C21 1.397(6) . ? C17 C18 1.383(8) . ? C17 H17 0.95 . ? C18 C19 1.387(8) . ? C18 H18 0.95 . ? C19 C20 1.380(8) . ? C19 H19 0.95 . ? C20 C21 1.381(7) . ? C20 H20 0.95 . ? C21 H21 0.95 . ? C1S Cl1S 1.756(4) . ? C1S Cl2S 1.768(4) . ? C1S H1S1 0.99 . ? C1S H1S2 0.99 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Au1 P1 175.49(12) . . ? C10 P1 C4 105.5(2) . . ? C10 P1 C16 103.5(2) . . ? C4 P1 C16 107.5(2) . . ? C10 P1 Au1 113.92(15) . . ? C4 P1 Au1 115.44(15) . . ? C16 P1 Au1 110.05(14) . . ? C3 C1 C2 115.5(4) 3_575 . ? C3 C1 Au1 123.7(3) 3_575 . ? C2 C1 Au1 120.6(4) . . ? C3 C2 C1 121.6(5) . . ? C3 C2 H2 119.2 . . ? C1 C2 H2 119.2 . . ? C1 C3 C2 122.9(4) 3_575 . ? C1 C3 H3 118.6 3_575 . ? C2 C3 H3 118.6 . . ? C5 C4 C9 119.2(4) . . ? C5 C4 P1 122.8(4) . . ? C9 C4 P1 118.0(4) . . ? C4 C5 C6 120.1(5) . . ? C4 C5 H5 120 . . ? C6 C5 H5 120 . . ? C7 C6 C5 120.3(5) . . ? C7 C6 H6 119.9 . . ? C5 C6 H6 119.9 . . ? C6 C7 C8 120.3(5) . . ? C6 C7 H7 119.8 . . ? C8 C7 H7 119.8 . . ? C7 C8 C9 119.7(5) . . ? C7 C8 H8 120.2 . . ? C9 C8 H8 120.2 . . ? C8 C9 C4 120.4(5) . . ? C8 C9 H9 119.8 . . ? C4 C9 H9 119.8 . . ? C11 C10 C15 119.4(4) . . ? C11 C10 P1 122.8(4) . . ? C15 C10 P1 117.8(3) . . ? C10 C11 C12 120.1(4) . . ? C10 C11 H11 120 . . ? C12 C11 H11 120 . . ? C13 C12 C11 119.8(5) . . ? C13 C12 H12 120.1 . . ? C11 C12 H12 120.1 . . ? C12 C13 C14 120.2(5) . . ? C12 C13 H13 119.9 . . ? C14 C13 H13 119.9 . . ? C13 C14 C15 120.1(5) . . ? C13 C14 H14 119.9 . . ? C15 C14 H14 119.9 . . ? C14 C15 C10 120.4(5) . . ? C14 C15 H15 119.8 . . ? C10 C15 H15 119.8 . . ? C17 C16 C21 117.9(4) . . ? C17 C16 P1 119.2(4) . . ? C21 C16 P1 122.8(3) . . ? C18 C17 C16 121.2(5) . . ? C18 C17 H17 119.4 . . ? C16 C17 H17 119.4 . . ? C17 C18 C19 120.0(5) . . ? C17 C18 H18 120 . . ? C19 C18 H18 120 . . ? C20 C19 C18 119.6(5) . . ? C20 C19 H19 120.2 . . ? C18 C19 H19 120.2 . . ? C19 C20 C21 120.1(5) . . ? C19 C20 H20 119.9 . . ? C21 C20 H20 119.9 . . ? C20 C21 C16 121.2(4) . . ? C20 C21 H21 119.4 . . ? C16 C21 H21 119.4 . . ? Cl1S C1S Cl2S 112.9(2) . . ? Cl1S C1S H1S1 109 . . ? Cl2S C1S H1S1 109 . . ? Cl1S C1S H1S2 109 . . ? Cl2S C1S H1S2 109 . . ? H1S1 C1S H1S2 107.8 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 Au1 P1 C10 -91.4(18) . . . . ? C1 Au1 P1 C4 146.3(18) . . . . ? C1 Au1 P1 C16 24.3(19) . . . . ? P1 Au1 C1 C3 -105.5(18) . . . 3_575 ? P1 Au1 C1 C2 69(2) . . . . ? C3 C1 C2 C3 -0.8(8) 3_575 . . . ? Au1 C1 C2 C3 -175.7(4) . . . . ? C1 C2 C3 C1 0.8(8) . . . 3_575 ? C10 P1 C4 C5 82.0(4) . . . . ? C16 P1 C4 C5 -28.0(5) . . . . ? Au1 P1 C4 C5 -151.3(4) . . . . ? C10 P1 C4 C9 -96.8(4) . . . . ? C16 P1 C4 C9 153.2(4) . . . . ? Au1 P1 C4 C9 29.9(4) . . . . ? C9 C4 C5 C6 -0.2(7) . . . . ? P1 C4 C5 C6 -179.1(4) . . . . ? C4 C5 C6 C7 0.0(8) . . . . ? C5 C6 C7 C8 0.1(9) . . . . ? C6 C7 C8 C9 -0.1(8) . . . . ? C7 C8 C9 C4 -0.1(8) . . . . ? C5 C4 C9 C8 0.3(7) . . . . ? P1 C4 C9 C8 179.1(4) . . . . ? C4 P1 C10 C11 -29.2(5) . . . . ? C16 P1 C10 C11 83.7(4) . . . . ? Au1 P1 C10 C11 -156.9(4) . . . . ? C4 P1 C10 C15 153.6(4) . . . . ? C16 P1 C10 C15 -93.6(4) . . . . ? Au1 P1 C10 C15 25.9(4) . . . . ? C15 C10 C11 C12 1.9(7) . . . . ? P1 C10 C11 C12 -175.3(4) . . . . ? C10 C11 C12 C13 -2.2(8) . . . . ? C11 C12 C13 C14 1.2(8) . . . . ? C12 C13 C14 C15 0.0(8) . . . . ? C13 C14 C15 C10 -0.3(8) . . . . ? C11 C10 C15 C14 -0.7(8) . . . . ? P1 C10 C15 C14 176.7(4) . . . . ? C10 P1 C16 C17 149.7(4) . . . . ? C4 P1 C16 C17 -99.0(4) . . . . ? Au1 P1 C16 C17 27.6(4) . . . . ? C10 P1 C16 C21 -27.1(4) . . . . ? C4 P1 C16 C21 84.3(4) . . . . ? Au1 P1 C16 C21 -149.2(3) . . . . ? C21 C16 C17 C18 0.1(8) . . . . ? P1 C16 C17 C18 -176.8(4) . . . . ? C16 C17 C18 C19 1.1(9) . . . . ? C17 C18 C19 C20 -2.2(9) . . . . ? C18 C19 C20 C21 2.1(8) . . . . ? C19 C20 C21 C16 -0.9(7) . . . . ? C17 C16 C21 C20 -0.2(7) . . . . ? P1 C16 C21 C20 176.6(4) . . . . ? ##End #\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2006-11-29 at 00:28:23 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.3 # Request file : c:\wingx\files\archive.dat # CIF files read : k dreduc struct data_compound_2b _database_code_depnum_ccdc_archive 'CCDC 756406' #TrackingRef 'Flower1.cif' _audit_creation_date 2006-11-29T00:28:23-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C32 H30 Au2 P2' _chemical_formula_sum 'C32 H30 Au2 P2' _chemical_formula_weight 870.2 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.4871(3) _cell_length_b 10.8176(4) _cell_length_c 15.1648(7) _cell_angle_alpha 90 _cell_angle_beta 90.8900(10) _cell_angle_gamma 90 _cell_volume 1392.11(10) _cell_formula_units_Z 2 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 2820 _cell_measurement_theta_min 2 _cell_measurement_theta_max 27 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.08 _exptl_crystal_density_diffrn 2.076 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 820 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 10.326 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; R.H. Blessing, Acta Cryst. (1995), A51, 33-38 ; _exptl_absorpt_correction_T_min 0.3065 _exptl_absorpt_correction_T_max 0.4922 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 9 _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 -0.88923E-2 _diffrn_orient_matrix_ub_12 0.858766E-1 _diffrn_orient_matrix_ub_13 -0.239721E-1 _diffrn_orient_matrix_ub_21 -0.623666E-1 _diffrn_orient_matrix_ub_22 0.250214E-1 _diffrn_orient_matrix_ub_23 0.52484E-1 _diffrn_orient_matrix_ub_31 0.995873E-1 _diffrn_orient_matrix_ub_32 0.233378E-1 _diffrn_orient_matrix_ub_33 0.319404E-1 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.0726 _diffrn_reflns_av_unetI/netI 0.0547 _diffrn_reflns_number 2849 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.05 _diffrn_reflns_theta_max 26.5 _diffrn_reflns_theta_full 26.5 _diffrn_measured_fraction_theta_full 0.987 _diffrn_measured_fraction_theta_max 0.987 _reflns_number_total 2849 _reflns_number_gt 1915 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SIR92 (Giacovazzo et al, 1993)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0963P)^2^+13.7554P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 2849 _refine_ls_number_parameters 164 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.097 _refine_ls_R_factor_gt 0.0584 _refine_ls_wR_factor_ref 0.1782 _refine_ls_wR_factor_gt 0.1492 _refine_ls_goodness_of_fit_ref 1.084 _refine_ls_restrained_S_all 1.084 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0 _refine_diff_density_max 4.726 _refine_diff_density_min -2.641 _refine_diff_density_rms 0.302 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.102 0.094 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Au Au -1.9162 8.821 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.5522(15) 0.8861(11) 0.5374(8) 0.037(3) Uani 1 1 d . . . C2 C 0.6506(14) 0.9876(12) 0.5246(10) 0.046(3) Uani 1 1 d . . . H2 H 0.7583 0.9804 0.5419 0.056 Uiso 1 1 calc R . . C3 C 0.6009(15) 1.0960(12) 0.4890(8) 0.040(3) Uani 1 1 d . . . H3 H 0.6745 1.1613 0.4822 0.048 Uiso 1 1 calc R . . C4 C 0.5322(17) 0.4522(12) 0.6950(9) 0.046(3) Uani 1 1 d . . . C5 C 0.445(2) 0.4987(14) 0.7611(11) 0.061(4) Uani 1 1 d . . . H5 H 0.478 0.5738 0.7883 0.074 Uiso 1 1 calc R . . C6 C 0.311(2) 0.4418(16) 0.7908(11) 0.066(5) Uani 1 1 d . . . H6 H 0.2518 0.4781 0.8368 0.079 Uiso 1 1 calc R . . C7 C 0.2636(19) 0.3348(18) 0.7542(12) 0.063(4) Uani 1 1 d . . . H7 H 0.172 0.2945 0.775 0.075 Uiso 1 1 calc R . . C8 C 0.347(2) 0.2835(15) 0.6868(14) 0.065(5) Uani 1 1 d . . . H8 H 0.3124 0.208 0.6612 0.079 Uiso 1 1 calc R . . C9 C 0.4827(15) 0.3402(13) 0.6553(9) 0.043(3) Uani 1 1 d . . . H9 H 0.5401 0.3046 0.6085 0.052 Uiso 1 1 calc R . . C10 C 0.8005(15) 0.4323(13) 0.5772(9) 0.045(3) Uani 1 1 d . . . C11 C 0.9017(15) 0.3403(12) 0.6067(10) 0.044(3) Uani 1 1 d . . . H11 H 0.9195 0.3272 0.668 0.053 Uiso 1 1 calc R . . C12 C 0.9784(19) 0.2658(15) 0.5432(13) 0.058(4) Uani 1 1 d . . . H12 H 1.0474 0.2019 0.5629 0.07 Uiso 1 1 calc R . . C13 C 0.9557(18) 0.2835(13) 0.4547(12) 0.053(4) Uani 1 1 d . . . H13 H 1.0091 0.2337 0.4131 0.064 Uiso 1 1 calc R . . C14 C 0.8551(17) 0.3737(15) 0.4278(10) 0.051(4) Uani 1 1 d . . . H14 H 0.8356 0.3853 0.3665 0.061 Uiso 1 1 calc R . . C15 C 0.7797(15) 0.4498(13) 0.4882(9) 0.045(3) Uani 1 1 d . . . H15 H 0.7131 0.5145 0.4675 0.054 Uiso 1 1 calc R . . C16 C 0.8285(17) 0.5485(14) 0.7494(9) 0.050(3) Uani 1 1 d . . . H16A H 0.8437 0.4664 0.7756 0.075 Uiso 1 1 calc R . . H16B H 0.7795 0.6034 0.7925 0.075 Uiso 1 1 calc R . . H16C H 0.9308 0.5824 0.7326 0.075 Uiso 1 1 calc R . . P1 P 0.7030(4) 0.5360(3) 0.6532(2) 0.0405(8) Uani 1 1 d . . . Au1 Au 0.62677(6) 0.72131(4) 0.59249(3) 0.0399(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.049(7) 0.035(7) 0.027(6) 0.006(5) 0.003(5) 0.011(5) C2 0.031(6) 0.040(7) 0.067(10) 0.019(7) -0.004(6) 0.002(5) C3 0.043(7) 0.038(7) 0.039(7) -0.002(6) -0.004(6) -0.009(6) C4 0.058(8) 0.032(7) 0.047(8) 0.016(6) -0.005(7) -0.004(6) C5 0.076(11) 0.042(8) 0.066(11) -0.003(7) 0.023(9) 0.006(7) C6 0.081(11) 0.056(10) 0.062(11) 0.017(8) 0.032(9) 0.019(9) C7 0.053(9) 0.071(12) 0.065(11) 0.027(9) 0.005(8) 0.003(8) C8 0.055(10) 0.061(11) 0.079(13) 0.007(9) -0.024(9) -0.014(8) C9 0.044(7) 0.045(8) 0.041(7) 0.007(6) -0.008(6) 0.012(6) C10 0.045(7) 0.042(8) 0.048(8) -0.002(6) -0.003(6) -0.007(6) C11 0.047(7) 0.032(7) 0.053(8) 0.004(6) -0.010(6) -0.005(6) C12 0.050(9) 0.052(9) 0.073(12) -0.016(8) -0.002(8) 0.005(7) C13 0.044(8) 0.044(9) 0.072(12) -0.011(7) 0.011(7) -0.005(6) C14 0.062(9) 0.052(9) 0.038(8) 0.004(6) -0.002(7) -0.010(7) C15 0.042(7) 0.043(8) 0.051(9) 0.004(6) 0.002(6) -0.004(6) C16 0.058(8) 0.053(9) 0.038(8) -0.001(6) -0.003(6) -0.010(7) P1 0.0494(19) 0.0335(17) 0.0384(19) 0.0012(14) -0.0046(15) -0.0001(14) Au1 0.0504(4) 0.0276(3) 0.0416(4) 0.0032(2) 0.0005(2) 0.0006(2) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C3 1.367(17) 3_676 ? C1 C2 1.395(18) . ? C1 Au1 2.064(12) . ? C2 C3 1.356(18) . ? C2 H2 0.95 . ? C3 C1 1.367(17) 3_676 ? C3 H3 0.95 . ? C4 C5 1.35(2) . ? C4 C9 1.41(2) . ? C4 P1 1.831(14) . ? C5 C6 1.38(2) . ? C5 H5 0.95 . ? C6 C7 1.34(3) . ? C6 H6 0.95 . ? C7 C8 1.37(3) . ? C7 H7 0.95 . ? C8 C9 1.39(2) . ? C8 H8 0.95 . ? C9 H9 0.95 . ? C10 C15 1.372(19) . ? C10 C11 1.384(19) . ? C10 P1 1.817(14) . ? C11 C12 1.42(2) . ? C11 H11 0.95 . ? C12 C13 1.37(3) . ? C12 H12 0.95 . ? C13 C14 1.36(2) . ? C13 H13 0.95 . ? C14 C15 1.39(2) . ? C14 H14 0.95 . ? C15 H15 0.95 . ? C16 P1 1.798(14) . ? C16 H16A 0.98 . ? C16 H16B 0.98 . ? C16 H16C 0.98 . ? P1 Au1 2.295(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 C3 C1 C2 114.6(11) 3_676 . ? C3 C1 Au1 121.7(10) 3_676 . ? C2 C1 Au1 123.7(9) . . ? C3 C2 C1 123.6(12) . . ? C3 C2 H2 118.2 . . ? C1 C2 H2 118.2 . . ? C2 C3 C1 121.8(12) . 3_676 ? C2 C3 H3 119.1 . . ? C1 C3 H3 119.1 3_676 . ? C5 C4 C9 118.2(14) . . ? C5 C4 P1 121.1(12) . . ? C9 C4 P1 120.6(11) . . ? C4 C5 C6 122.7(16) . . ? C4 C5 H5 118.7 . . ? C6 C5 H5 118.7 . . ? C7 C6 C5 119.6(16) . . ? C7 C6 H6 120.2 . . ? C5 C6 H6 120.2 . . ? C6 C7 C8 120.2(16) . . ? C6 C7 H7 119.9 . . ? C8 C7 H7 119.9 . . ? C7 C8 C9 121.1(16) . . ? C7 C8 H8 119.4 . . ? C9 C8 H8 119.4 . . ? C8 C9 C4 118.2(15) . . ? C8 C9 H9 120.9 . . ? C4 C9 H9 120.9 . . ? C15 C10 C11 119.1(13) . . ? C15 C10 P1 119.1(11) . . ? C11 C10 P1 121.7(11) . . ? C10 C11 C12 118.5(14) . . ? C10 C11 H11 120.7 . . ? C12 C11 H11 120.7 . . ? C13 C12 C11 121.8(15) . . ? C13 C12 H12 119.1 . . ? C11 C12 H12 119.1 . . ? C14 C13 C12 118.4(15) . . ? C14 C13 H13 120.8 . . ? C12 C13 H13 120.8 . . ? C13 C14 C15 121.4(14) . . ? C13 C14 H14 119.3 . . ? C15 C14 H14 119.3 . . ? C10 C15 C14 120.8(13) . . ? C10 C15 H15 119.6 . . ? C14 C15 H15 119.6 . . ? P1 C16 H16A 109.5 . . ? P1 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? P1 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C16 P1 C10 106.9(7) . . ? C16 P1 C4 102.7(7) . . ? C10 P1 C4 106.5(6) . . ? C16 P1 Au1 114.8(5) . . ? C10 P1 Au1 114.4(5) . . ? C4 P1 Au1 110.6(4) . . ? C1 Au1 P1 178.5(4) . . ? ##End #\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2006-11-29 at 15:44:27 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.3 # Request file : c:\wingx\files\archive.dat # CIF files read : new dreduc struct data_Compound_2c _database_code_depnum_ccdc_archive 'CCDC 756407' #TrackingRef 'Flower1.cif' _audit_creation_date 2006-11-29T15:44:27-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C22 H26 Au2 P2' _chemical_formula_sum 'C22 H26 Au2 P2' _chemical_formula_weight 746.3 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 1 2/c 1' _symmetry_space_group_name_Hall '-C 2yc' _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 11.5373(3) _cell_length_b 13.6031(3) _cell_length_c 14.1294(3) _cell_angle_alpha 90 _cell_angle_beta 95.9330(10) _cell_angle_gamma 90 _cell_volume 2205.63(9) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 10079 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 27.485 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.07 _exptl_crystal_density_diffrn 2.247 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1384 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 13.002 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; R.H. Blessing, Acta Cryst. (1995), A51, 33-38 ; _exptl_absorpt_correction_T_min 0.2031 _exptl_absorpt_correction_T_max 0.463 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 9 _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 -0.10537E-2 _diffrn_orient_matrix_ub_12 -0.416739E-1 _diffrn_orient_matrix_ub_13 0.356287E-1 _diffrn_orient_matrix_ub_21 0.56436E-2 _diffrn_orient_matrix_ub_22 0.603161E-1 _diffrn_orient_matrix_ub_23 0.248923E-1 _diffrn_orient_matrix_ub_31 -0.709236E-1 _diffrn_orient_matrix_ub_32 0.54187E-2 _diffrn_orient_matrix_ub_33 -0.30673E-2 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.0499 _diffrn_reflns_av_unetI/netI 0.0332 _diffrn_reflns_number 2291 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.33 _diffrn_reflns_theta_max 26.5 _diffrn_reflns_theta_full 26.5 _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.997 _reflns_number_total 2291 _reflns_number_gt 1675 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0512P)^2^+59.7299P] 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_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_coef 0.00030(9) _refine_ls_number_reflns 2291 _refine_ls_number_parameters 119 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0685 _refine_ls_R_factor_gt 0.0453 _refine_ls_wR_factor_ref 0.1265 _refine_ls_wR_factor_gt 0.1107 _refine_ls_goodness_of_fit_ref 1.064 _refine_ls_restrained_S_all 1.064 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 2.766 _refine_diff_density_min -2.585 _refine_diff_density_rms 0.227 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Au Au -1.9162 8.821 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1026 0.0946 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.5545(9) -0.0615(7) 0.5746(7) 0.041(2) Uani 1 1 d . . . C2 C 0.4409(10) -0.0294(9) 0.5744(8) 0.051(3) Uani 1 1 d . . . H2 H 0.3971 -0.0481 0.6248 0.061 Uiso 1 1 calc R . . C3 C 0.6110(10) -0.0303(9) 0.4987(9) 0.054(3) Uani 1 1 d . . . H3 H 0.6895 -0.0503 0.496 0.064 Uiso 1 1 calc R . . C4 C 0.8646(9) -0.2029(8) 0.8402(8) 0.045(2) Uani 1 1 d . . . C5 C 0.9521(12) -0.2547(10) 0.8912(8) 0.063(3) Uani 1 1 d . . . H5 H 0.9454 -0.3241 0.8967 0.076 Uiso 1 1 calc R . . C6 C 1.0492(11) -0.2081(13) 0.9344(9) 0.067(4) Uani 1 1 d . . . H6 H 1.1072 -0.2475 0.9688 0.081 Uiso 1 1 calc R . . C7 C 1.0662(18) -0.120(2) 0.932(2) 0.168(13) Uani 1 1 d . . . H7 H 1.1364 -0.0901 0.9592 0.201 Uiso 1 1 calc R . . C8 C 0.969(2) -0.0609(16) 0.882(3) 0.26(3) Uani 1 1 d . . . H8 H 0.9726 0.0089 0.8836 0.308 Uiso 1 1 calc R . . C9 C 0.8761(15) -0.1069(12) 0.835(2) 0.154(13) Uani 1 1 d . . . H9 H 0.819 -0.0695 0.797 0.185 Uiso 1 1 calc R . . C10 C 0.7821(15) -0.3681(10) 0.7311(10) 0.077(4) Uani 1 1 d . . . H10A H 0.8256 -0.3506 0.6775 0.115 Uiso 1 1 calc R . . H10B H 0.7149 -0.4089 0.7082 0.115 Uiso 1 1 calc R . . H10C H 0.8329 -0.4048 0.7785 0.115 Uiso 1 1 calc R . . C11 C 0.6549(12) -0.3009(11) 0.8797(11) 0.073(4) Uani 1 1 d . . . H11A H 0.5818 -0.3319 0.8536 0.109 Uiso 1 1 calc R . . H11B H 0.6378 -0.2453 0.9201 0.109 Uiso 1 1 calc R . . H11C H 0.7029 -0.3491 0.9177 0.109 Uiso 1 1 calc R . . Au1 Au 0.63252(4) -0.15357(3) 0.67739(3) 0.0512(2) Uani 1 1 d . . . P1 P 0.7322(3) -0.2581(2) 0.78431(19) 0.0454(7) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.044(6) 0.038(5) 0.038(5) -0.001(4) -0.014(4) 0.001(4) C2 0.044(6) 0.052(7) 0.055(6) 0.004(5) 0.003(5) 0.003(5) C3 0.040(6) 0.051(7) 0.068(7) 0.008(6) -0.001(5) 0.008(5) C4 0.041(6) 0.043(6) 0.050(6) -0.002(5) 0.005(5) 0.003(5) C5 0.077(8) 0.056(7) 0.051(7) 0.011(6) -0.020(6) 0.009(6) C6 0.043(7) 0.106(12) 0.051(7) 0.003(7) 0.001(5) 0.004(7) C7 0.063(12) 0.16(2) 0.28(4) -0.08(2) 0.014(16) -0.081(15) C8 0.15(2) 0.068(14) 0.51(6) 0.07(2) -0.19(3) -0.051(14) C9 0.085(12) 0.038(8) 0.31(4) 0.028(12) -0.103(17) -0.013(8) C10 0.107(12) 0.053(7) 0.066(8) -0.003(6) -0.011(8) 0.008(8) C11 0.062(8) 0.062(8) 0.094(10) 0.036(8) 0.008(7) 0.013(7) Au1 0.0670(4) 0.0372(3) 0.0442(3) 0.00322(17) -0.0198(2) 0.0029(2) P1 0.0534(16) 0.0402(14) 0.0404(14) 0.0067(11) -0.0055(12) 0.0025(12) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C3 1.378(16) . ? C1 C2 1.382(15) . ? C1 Au1 2.053(9) . ? C2 C3 1.398(15) 5_656 ? C2 H2 0.95 . ? C3 C2 1.398(15) 5_656 ? C3 H3 0.95 . ? C4 C9 1.32(2) . ? C4 C5 1.373(15) . ? C4 P1 1.809(11) . ? C5 C6 1.375(19) . ? C5 H5 0.95 . ? C6 C7 1.22(3) . ? C6 H6 0.95 . ? C7 C8 1.49(4) . ? C7 H7 0.95 . ? C8 C9 1.36(2) . ? C8 H8 0.95 . ? C9 H9 0.95 . ? C10 P1 1.795(14) . ? C10 H10A 0.98 . ? C10 H10B 0.98 . ? C10 H10C 0.98 . ? C11 P1 1.788(14) . ? C11 H11A 0.98 . ? C11 H11B 0.98 . ? C11 H11C 0.98 . ? Au1 P1 2.295(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 C3 C1 C2 115.1(9) . . ? C3 C1 Au1 122.0(8) . . ? C2 C1 Au1 122.8(8) . . ? C1 C2 C3 121.3(11) . 5_656 ? C1 C2 H2 119.4 . . ? C3 C2 H2 119.4 5_656 . ? C1 C3 C2 123.6(10) . 5_656 ? C1 C3 H3 118.2 . . ? C2 C3 H3 118.2 5_656 . ? C9 C4 C5 117.9(12) . . ? C9 C4 P1 118.1(9) . . ? C5 C4 P1 123.9(9) . . ? C4 C5 C6 121.2(13) . . ? C4 C5 H5 119.4 . . ? C6 C5 H5 119.4 . . ? C7 C6 C5 124.6(18) . . ? C7 C6 H6 117.7 . . ? C5 C6 H6 117.7 . . ? C6 C7 C8 115.4(16) . . ? C6 C7 H7 122.3 . . ? C8 C7 H7 122.3 . . ? C9 C8 C7 120.2(18) . . ? C9 C8 H8 119.9 . . ? C7 C8 H8 119.9 . . ? C4 C9 C8 120.4(16) . . ? C4 C9 H9 119.8 . . ? C8 C9 H9 119.8 . . ? P1 C10 H10A 109.5 . . ? P1 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? P1 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? P1 C11 H11A 109.5 . . ? P1 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? P1 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C1 Au1 P1 175.2(3) . . ? C11 P1 C10 104.5(7) . . ? C11 P1 C4 105.7(6) . . ? C10 P1 C4 103.7(6) . . ? C11 P1 Au1 116.3(4) . . ? C10 P1 Au1 113.6(5) . . ? C4 P1 Au1 111.9(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C3 C1 C2 C3 0.2(18) . . . 5_656 ? Au1 C1 C2 C3 -177.5(9) . . . 5_656 ? C2 C1 C3 C2 -0.2(19) . . . 5_656 ? Au1 C1 C3 C2 177.5(9) . . . 5_656 ? C9 C4 C5 C6 0(2) . . . . ? P1 C4 C5 C6 -178.1(10) . . . . ? C4 C5 C6 C7 0(3) . . . . ? C5 C6 C7 C8 4(4) . . . . ? C6 C7 C8 C9 -7(6) . . . . ? C5 C4 C9 C8 -3(4) . . . . ? P1 C4 C9 C8 174(3) . . . . ? C7 C8 C9 C4 7(6) . . . . ? C3 C1 Au1 P1 -9(4) . . . . ? C2 C1 Au1 P1 169(3) . . . . ? C9 C4 P1 C11 -111.0(17) . . . . ? C5 C4 P1 C11 66.7(12) . . . . ? C9 C4 P1 C10 139.4(17) . . . . ? C5 C4 P1 C10 -43.0(12) . . . . ? C9 C4 P1 Au1 16.5(17) . . . . ? C5 C4 P1 Au1 -165.8(9) . . . . ? C1 Au1 P1 C11 -169(3) . . . . ? C1 Au1 P1 C10 -48(3) . . . . ? C1 Au1 P1 C4 69(3) . . . . ? ##End #\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2006-10-10 at 10:05:25 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.3 # Request file : c:\wingx\files\archive.dat # CIF files read : k dreduc sortav struct data_compound_2d _database_code_depnum_ccdc_archive 'CCDC 756408' #TrackingRef 'Flower1.cif' _audit_creation_date 2006-10-10T10:05:25-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C14 H24 Au2 Cl6 P2' _chemical_formula_sum 'C14 H24 Au2 Cl6 P2' _chemical_formula_weight 860.91 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 24.5474(3) _cell_length_b 9.1914(2) _cell_length_c 12.2193(2) _cell_angle_alpha 90 _cell_angle_beta 113.8070(10) _cell_angle_gamma 90 _cell_volume 2522.39(8) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 3194 _cell_measurement_theta_min 2 _cell_measurement_theta_max 27 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 2.267 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1592 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 12.379 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; R.H. Blessing, Acta Cryst. (1995), A51, 33-38 ; _exptl_absorpt_correction_T_min 0.2111 _exptl_absorpt_correction_T_max 0.3590 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 9 _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 0.427079E-1 _diffrn_orient_matrix_ub_12 -0.193282E-1 _diffrn_orient_matrix_ub_13 0.526449E-1 _diffrn_orient_matrix_ub_21 -0.125749E-1 _diffrn_orient_matrix_ub_22 -0.607221E-1 _diffrn_orient_matrix_ub_23 0.536544E-1 _diffrn_orient_matrix_ub_31 -0.7019E-3 _diffrn_orient_matrix_ub_32 -0.881823E-1 _diffrn_orient_matrix_ub_33 -0.484852E-1 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.077 _diffrn_reflns_av_unetI/netI 0.03 _diffrn_reflns_number 25385 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.35 _diffrn_reflns_theta_max 27.5 _diffrn_reflns_theta_full 27.5 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _reflns_number_total 2881 _reflns_number_gt 2320 _reflns_threshold_expression >2sigma(I) _diffrn_reflns_reduction_process ; Scaled and merged with SORTAV R.H. Blessing, (1987) Cryst. Rev. 1, 3-58 R.H. Blessing, (1989) J. Appl. Cryst. 22, 396-397 ; #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SIR92 (Giacovazzo et al, 1993)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0426P)^2^+44.6484P] 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_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_coef 0.00029(6) _refine_ls_number_reflns 2881 _refine_ls_number_parameters 113 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0558 _refine_ls_R_factor_gt 0.0403 _refine_ls_wR_factor_ref 0.1034 _refine_ls_wR_factor_gt 0.0934 _refine_ls_goodness_of_fit_ref 1.071 _refine_ls_restrained_S_all 1.071 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 2.945 _refine_diff_density_min -1.882 _refine_diff_density_rms 0.205 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.0206(3) 0.8877(9) 0.0886(7) 0.0374(17) Uani 1 1 d . . . C2 C 0.0209(3) 1.0359(9) 0.1182(7) 0.0386(17) Uani 1 1 d . . . H2 H 0.0358 1.0629 0.2002 0.046 Uiso 1 1 calc R . . C3 C -0.0001(3) 0.8564(8) -0.0316(7) 0.0372(17) Uani 1 1 d . . . H3 H 0 0.7582 -0.0559 0.045 Uiso 1 1 calc R . . C4 C 0.0840(5) 0.5493(12) 0.4864(9) 0.066(3) Uani 1 1 d . . . H4A H 0.1074 0.4734 0.5416 0.1 Uiso 1 1 calc R . . H4B H 0.0416 0.526 0.4578 0.1 Uiso 1 1 calc R . . H4C H 0.0918 0.6432 0.5279 0.1 Uiso 1 1 calc R . . C5 C 0.0956(7) 0.3737(12) 0.3080(10) 0.087(4) Uani 1 1 d . . . H5A H 0.1215 0.3095 0.3719 0.131 Uiso 1 1 calc R . . H5B H 0.1064 0.3671 0.2392 0.131 Uiso 1 1 calc R . . H5C H 0.054 0.3439 0.2837 0.131 Uiso 1 1 calc R . . C6 C 0.1843(5) 0.5843(16) 0.4315(13) 0.088(4) Uani 1 1 d . . . H6A H 0.1935 0.6769 0.4749 0.131 Uiso 1 1 calc R . . H6B H 0.2004 0.5852 0.3699 0.131 Uiso 1 1 calc R . . H6C H 0.2024 0.5043 0.4874 0.131 Uiso 1 1 calc R . . C7 C 0.1564(4) 1.0441(13) 0.5897(10) 0.064(3) Uani 1 1 d . . . H7 H 0.1168 1.0717 0.5889 0.077 Uiso 1 1 calc R . . Au1 Au 0.056481(14) 0.73166(3) 0.22013(3) 0.03818(15) Uani 1 1 d . . . P1 P 0.10468(10) 0.5593(2) 0.36171(19) 0.0407(5) Uani 1 1 d . . . Cl1 Cl 0.20248(19) 1.1958(4) 0.6300(5) 0.1236(17) Uani 1 1 d . . . Cl2 Cl 0.18656(18) 0.9045(5) 0.6940(4) 0.1087(13) Uani 1 1 d . . . Cl3 Cl 0.14599(16) 0.9852(4) 0.4494(3) 0.0882(10) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.035(4) 0.040(4) 0.039(4) 0.012(3) 0.017(3) 0.001(3) C2 0.038(4) 0.041(4) 0.039(4) -0.002(3) 0.018(3) -0.004(3) C3 0.046(4) 0.030(4) 0.037(4) 0.006(3) 0.018(3) 0.001(3) C4 0.087(8) 0.066(7) 0.050(6) 0.023(5) 0.031(5) 0.024(6) C5 0.147(12) 0.049(6) 0.052(6) -0.005(5) 0.025(7) 0.014(7) C6 0.055(7) 0.094(10) 0.105(10) 0.033(8) 0.024(7) 0.013(6) C7 0.044(5) 0.079(7) 0.074(7) 0.006(6) 0.027(5) 0.017(5) Au1 0.0426(2) 0.0360(2) 0.03570(19) 0.00542(12) 0.01560(14) 0.00120(13) P1 0.0484(12) 0.0344(11) 0.0384(11) 0.0060(8) 0.0167(9) 0.0078(9) Cl1 0.096(3) 0.072(2) 0.156(4) -0.030(2) 0.003(3) -0.002(2) Cl2 0.100(3) 0.132(3) 0.098(3) 0.054(2) 0.045(2) 0.030(2) Cl3 0.097(2) 0.079(2) 0.0677(18) -0.0049(15) 0.0113(16) 0.0227(17) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C3 1.377(11) . ? C1 C2 1.408(11) . ? C1 Au1 2.067(7) . ? C2 C3 1.388(11) 5_575 ? C2 H2 0.95 . ? C3 C2 1.388(11) 5_575 ? C3 H3 0.95 . ? C4 P1 1.792(10) . ? C4 H4A 0.98 . ? C4 H4B 0.98 . ? C4 H4C 0.98 . ? C5 P1 1.809(11) . ? C5 H5A 0.98 . ? C5 H5B 0.98 . ? C5 H5C 0.98 . ? C6 P1 1.805(11) . ? C6 H6A 0.98 . ? C6 H6B 0.98 . ? C6 H6C 0.98 . ? C7 Cl3 1.716(11) . ? C7 Cl1 1.737(12) . ? C7 Cl2 1.748(11) . ? C7 H7 1 . ? Au1 P1 2.291(2) . ? Au1 Au1 3.1395(6) 2 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C3 C1 C2 116.0(7) . . ? C3 C1 Au1 122.8(6) . . ? C2 C1 Au1 121.0(6) . . ? C3 C2 C1 122.1(7) 5_575 . ? C3 C2 H2 118.9 5_575 . ? C1 C2 H2 118.9 . . ? C1 C3 C2 121.9(7) . 5_575 ? C1 C3 H3 119.1 . . ? C2 C3 H3 119.1 5_575 . ? P1 C4 H4A 109.5 . . ? P1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? P1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? P1 C5 H5A 109.5 . . ? P1 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? P1 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? P1 C6 H6A 109.5 . . ? P1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? P1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? Cl3 C7 Cl1 110.7(6) . . ? Cl3 C7 Cl2 110.2(6) . . ? Cl1 C7 Cl2 110.3(6) . . ? Cl3 C7 H7 108.5 . . ? Cl1 C7 H7 108.5 . . ? Cl2 C7 H7 108.5 . . ? C1 Au1 P1 174.2(2) . . ? C1 Au1 Au1 92.4(2) . 2 ? P1 Au1 Au1 93.43(6) . 2 ? C4 P1 C6 103.3(6) . . ? C4 P1 C5 103.0(6) . . ? C6 P1 C5 104.0(7) . . ? C4 P1 Au1 116.1(3) . . ? C6 P1 Au1 113.5(4) . . ? C5 P1 Au1 115.3(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C3 C1 C2 C3 1.8(13) . . . 5_575 ? Au1 C1 C2 C3 176.4(6) . . . 5_575 ? C2 C1 C3 C2 -1.8(13) . . . 5_575 ? Au1 C1 C3 C2 -176.3(6) . . . 5_575 ? C3 C1 Au1 P1 75(3) . . . . ? C2 C1 Au1 P1 -100(2) . . . . ? C3 C1 Au1 Au1 -107.0(6) . . . 2 ? C2 C1 Au1 Au1 78.7(6) . . . 2 ? C1 Au1 P1 C4 152(2) . . . . ? Au1 Au1 P1 C4 -26.3(5) 2 . . . ? C1 Au1 P1 C6 33(2) . . . . ? Au1 Au1 P1 C6 -145.8(6) 2 . . . ? C1 Au1 P1 C5 -87(2) . . . . ? Au1 Au1 P1 C5 94.3(6) 2 . . . ?