# 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 'Dr Alan Brisdon' _publ_contact_author_address ; School of Chemistry, University of Manchester Oxford Road Manchester, UK M13 9PL ; _publ_section_title ; The synthesis of gold(I) fluoroalkyl and fluoroalkenyl- substituted phosphine complexes and factors effecting their packing. ; _publ_requested_category FM _publ_contact_author_email alan.brisdon@manchester.ac.uk loop_ _publ_author_name A.Brisdon N.Barnes W.Brown W.Cross I.Crossley C.Fish ; C.Herbert ; R.Pritchard J.Warren data_Ph2CFCHF _database_code_depnum_ccdc_archive 'CCDC 789438' #TrackingRef '- CIFS.cif' _audit_creation_date 2004-05-18T12:01:54-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.2 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C14 H11 Au1 Cl1 F2 P1' _chemical_formula_sum 'C14 H11 Au Cl F2 P' _chemical_formula_weight 480.61 _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 11.9461(4) _cell_length_b 8.0806(3) _cell_length_c 15.4475(6) _cell_angle_alpha 90 _cell_angle_beta 92.3500(10) _cell_angle_gamma 90 _cell_volume 1489.92(9) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 7012 _cell_measurement_theta_min 1.018 _cell_measurement_theta_max 27.485 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.08 _exptl_crystal_density_diffrn 2.143 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 896 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 10.164 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; R.H. Blessing, Acta Cryst. (1995), A51, 33-38 ; _exptl_absorpt_correction_T_min 0.2357 _exptl_absorpt_correction_T_max 0.4969 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 293(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_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 0.737932E-1 _diffrn_orient_matrix_ub_12 -0.511838E-1 _diffrn_orient_matrix_ub_13 -0.125815E-1 _diffrn_orient_matrix_ub_21 -0.209575E-1 _diffrn_orient_matrix_ub_22 0.8474E-3 _diffrn_orient_matrix_ub_23 -0.633402E-1 _diffrn_orient_matrix_ub_31 0.336807E-1 _diffrn_orient_matrix_ub_32 0.112669 _diffrn_orient_matrix_ub_33 -0.52392E-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 0.0717 _diffrn_reflns_av_unetI/netI 0.0658 _diffrn_reflns_number 9993 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.04 _diffrn_reflns_theta_max 27.43 _diffrn_reflns_theta_full 27.43 _diffrn_measured_fraction_theta_full 0.979 _diffrn_measured_fraction_theta_max 0.979 _reflns_number_total 3329 _reflns_number_gt 2353 _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. ; _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^)+(0.0288P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_coef 0.0036(3) _refine_ls_number_reflns 3329 _refine_ls_number_parameters 173 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0614 _refine_ls_R_factor_gt 0.036 _refine_ls_wR_factor_ref 0.0832 _refine_ls_wR_factor_gt 0.0744 _refine_ls_goodness_of_fit_ref 1.003 _refine_ls_restrained_S_all 1.003 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.265 _refine_diff_density_min -1.155 _refine_diff_density_rms 0.139 #----------------------------------------------------------------------------# # 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' F F 0.0171 0.0103 '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' Au Au -2.0133 8.8022 '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 0.7146(5) 0.1670(7) 0.5832(4) 0.0652(16) Uani 1 1 d . . . C2 C 0.6938(6) 0.1098(9) 0.6590(5) 0.089(2) Uani 1 1 d . . . H2 H 0.629 0.0477 0.665 0.107 Uiso 1 1 calc R . . C3 C 0.7441(4) 0.4757(6) 0.5075(3) 0.0479(12) Uani 1 1 d . . . C4 C 0.7572(5) 0.5364(7) 0.4251(4) 0.0619(15) Uani 1 1 d . . . H4 H 0.8076 0.4861 0.389 0.074 Uiso 1 1 calc R . . C5 C 0.6958(6) 0.6713(8) 0.3960(5) 0.0749(18) Uani 1 1 d . . . H5 H 0.7048 0.7122 0.3405 0.09 Uiso 1 1 calc R . . C6 C 0.6213(6) 0.7452(8) 0.4493(5) 0.0813(19) Uani 1 1 d . . . H6 H 0.5802 0.8364 0.4295 0.098 Uiso 1 1 calc R . . C7 C 0.6065(6) 0.6863(9) 0.5314(5) 0.080(2) Uani 1 1 d . . . H7 H 0.5552 0.7361 0.5669 0.096 Uiso 1 1 calc R . . C8 C 0.6685(5) 0.5524(8) 0.5605(4) 0.0690(16) Uani 1 1 d . . . H8 H 0.6598 0.5128 0.6163 0.083 Uiso 1 1 calc R . . C9 C 0.8920(4) 0.2054(6) 0.4610(3) 0.0472(12) Uani 1 1 d . . . C10 C 0.8338(5) 0.1191(8) 0.3968(4) 0.0727(18) Uani 1 1 d . . . H10 H 0.7569 0.1046 0.4004 0.087 Uiso 1 1 calc R . . C11 C 0.8875(6) 0.0538(8) 0.3275(4) 0.0782(18) Uani 1 1 d . . . H11 H 0.8478 -0.0041 0.2842 0.094 Uiso 1 1 calc R . . C12 C 1.0024(8) 0.0767(9) 0.3237(4) 0.081(2) Uani 1 1 d . . . H12 H 1.0403 0.0298 0.2784 0.097 Uiso 1 1 calc R . . C13 C 1.0588(6) 0.1636(8) 0.3832(5) 0.0712(18) Uani 1 1 d . . . H13 H 1.1348 0.1837 0.377 0.085 Uiso 1 1 calc R . . C14 C 1.0062(4) 0.2254(7) 0.4549(4) 0.0597(14) Uani 1 1 d . . . H14 H 1.0476 0.2798 0.4985 0.072 Uiso 1 1 calc R . . F1 F 0.6397(3) 0.1275(4) 0.5192(3) 0.0801(11) Uani 1 1 d . . . F2 F 0.7586(4) 0.1347(7) 0.7272(3) 0.140(2) Uani 1 1 d . . . P1 P 0.82601(11) 0.30419(18) 0.55098(9) 0.0478(3) Uani 1 1 d . . . Cl1 Cl 1.06682(13) 0.4196(3) 0.77369(11) 0.0872(5) Uani 1 1 d . . . Au1 Au 0.945162(17) 0.36436(3) 0.660397(14) 0.05808(15) 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 0.057(4) 0.070(4) 0.069(4) 0.007(3) 0.013(3) 0.003(3) C2 0.060(4) 0.129(6) 0.078(5) 0.032(4) 0.014(4) -0.002(4) C3 0.044(3) 0.053(3) 0.046(3) 0.001(2) -0.005(2) -0.002(2) C4 0.061(3) 0.066(4) 0.059(4) 0.006(3) 0.001(3) 0.005(3) C5 0.092(5) 0.075(4) 0.056(4) 0.014(3) -0.012(4) -0.004(3) C6 0.091(5) 0.060(4) 0.092(5) -0.003(4) -0.017(4) 0.011(3) C7 0.076(5) 0.081(5) 0.084(5) -0.005(4) 0.008(4) 0.027(4) C8 0.073(4) 0.078(4) 0.055(4) -0.006(3) 0.005(3) 0.009(3) C9 0.046(3) 0.047(3) 0.048(3) 0.001(2) -0.002(2) 0.001(2) C10 0.054(3) 0.099(5) 0.064(4) -0.017(4) -0.004(3) -0.001(3) C11 0.087(5) 0.091(5) 0.057(4) -0.019(4) 0.000(3) -0.002(4) C12 0.118(6) 0.077(4) 0.049(4) 0.001(3) 0.032(4) 0.029(4) C13 0.057(4) 0.075(4) 0.083(5) -0.001(4) 0.018(3) 0.010(3) C14 0.048(3) 0.063(4) 0.069(4) -0.011(3) 0.006(3) 0.002(3) F1 0.064(2) 0.104(3) 0.071(3) -0.0073(19) -0.001(2) -0.0243(18) F2 0.098(3) 0.244(7) 0.080(3) 0.071(4) 0.013(3) -0.012(3) P1 0.0396(7) 0.0623(8) 0.0413(7) 0.0022(6) 0.0005(6) 0.0023(6) Cl1 0.0608(9) 0.1471(15) 0.0525(9) -0.0264(10) -0.0124(7) 0.0160(10) Au1 0.04855(18) 0.0838(2) 0.04148(18) -0.00718(10) -0.00272(11) 0.01014(10) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.292(9) . ? C1 F1 1.345(8) . ? C1 P1 1.817(6) . ? C2 F2 1.297(9) . ? C2 H2 0.93 . ? C3 C4 1.380(7) . ? C3 C8 1.388(7) . ? C3 P1 1.810(5) . ? C4 C5 1.379(8) . ? C4 H4 0.93 . ? C5 C6 1.374(10) . ? C5 H5 0.93 . ? C6 C7 1.372(10) . ? C6 H6 0.93 . ? C7 C8 1.376(9) . ? C7 H7 0.93 . ? C8 H8 0.93 . ? C9 C10 1.377(7) . ? C9 C14 1.381(7) . ? C9 P1 1.811(5) . ? C10 C11 1.375(9) . ? C10 H10 0.93 . ? C11 C12 1.389(10) . ? C11 H11 0.93 . ? C12 C13 1.319(12) . ? C12 H12 0.93 . ? C13 C14 1.388(9) . ? C13 H13 0.93 . ? C14 H14 0.93 . ? P1 Au1 2.2186(14) . ? Cl1 Au1 2.2728(15) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 F1 115.8(6) . . ? C2 C1 P1 129.5(6) . . ? F1 C1 P1 114.6(4) . . ? C1 C2 F2 123.4(7) . . ? C1 C2 H2 118.3 . . ? F2 C2 H2 118.3 . . ? C4 C3 C8 119.1(5) . . ? C4 C3 P1 122.3(4) . . ? C8 C3 P1 118.6(4) . . ? C5 C4 C3 120.1(6) . . ? C5 C4 H4 119.9 . . ? C3 C4 H4 119.9 . . ? C6 C5 C4 119.9(6) . . ? C6 C5 H5 120.1 . . ? C4 C5 H5 120.1 . . ? C7 C6 C5 120.9(6) . . ? C7 C6 H6 119.5 . . ? C5 C6 H6 119.5 . . ? C6 C7 C8 119.1(6) . . ? C6 C7 H7 120.5 . . ? C8 C7 H7 120.5 . . ? C7 C8 C3 120.9(6) . . ? C7 C8 H8 119.6 . . ? C3 C8 H8 119.6 . . ? C10 C9 C14 118.7(5) . . ? C10 C9 P1 123.6(4) . . ? C14 C9 P1 117.6(4) . . ? C11 C10 C9 121.2(6) . . ? C11 C10 H10 119.4 . . ? C9 C10 H10 119.4 . . ? C10 C11 C12 118.3(6) . . ? C10 C11 H11 120.8 . . ? C12 C11 H11 120.8 . . ? C13 C12 C11 121.3(6) . . ? C13 C12 H12 119.4 . . ? C11 C12 H12 119.4 . . ? C12 C13 C14 120.8(6) . . ? C12 C13 H13 119.6 . . ? C14 C13 H13 119.6 . . ? C9 C14 C13 119.6(5) . . ? C9 C14 H14 120.2 . . ? C13 C14 H14 120.2 . . ? C3 P1 C9 107.4(2) . . ? C3 P1 C1 100.3(3) . . ? C9 P1 C1 106.7(3) . . ? C3 P1 Au1 115.77(17) . . ? C9 P1 Au1 113.29(16) . . ? C1 P1 Au1 112.3(2) . . ? P1 Au1 Cl1 178.61(6) . . ? 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 F1 C1 C2 F2 178.9(6) . . . . ? P1 C1 C2 F2 -5.3(12) . . . . ? C8 C3 C4 C5 0.0(8) . . . . ? P1 C3 C4 C5 -177.6(4) . . . . ? C3 C4 C5 C6 -0.1(9) . . . . ? C4 C5 C6 C7 -0.3(11) . . . . ? C5 C6 C7 C8 0.8(11) . . . . ? C6 C7 C8 C3 -0.9(10) . . . . ? C4 C3 C8 C7 0.6(9) . . . . ? P1 C3 C8 C7 178.2(5) . . . . ? C14 C9 C10 C11 -0.2(9) . . . . ? P1 C9 C10 C11 176.6(5) . . . . ? C9 C10 C11 C12 0.2(10) . . . . ? C10 C11 C12 C13 -2.4(11) . . . . ? C11 C12 C13 C14 4.5(11) . . . . ? C10 C9 C14 C13 2.3(8) . . . . ? P1 C9 C14 C13 -174.7(5) . . . . ? C12 C13 C14 C9 -4.5(10) . . . . ? C4 C3 P1 C9 -14.5(5) . . . . ? C8 C3 P1 C9 167.9(4) . . . . ? C4 C3 P1 C1 -125.8(5) . . . . ? C8 C3 P1 C1 56.6(5) . . . . ? C4 C3 P1 Au1 113.2(4) . . . . ? C8 C3 P1 Au1 -64.4(5) . . . . ? C10 C9 P1 C3 -68.4(5) . . . . ? C14 C9 P1 C3 108.4(4) . . . . ? C10 C9 P1 C1 38.5(6) . . . . ? C14 C9 P1 C1 -144.8(4) . . . . ? C10 C9 P1 Au1 162.5(4) . . . . ? C14 C9 P1 Au1 -20.7(5) . . . . ? C2 C1 P1 C3 -119.6(7) . . . . ? F1 C1 P1 C3 56.1(5) . . . . ? C2 C1 P1 C9 128.6(7) . . . . ? F1 C1 P1 C9 -55.7(5) . . . . ? C2 C1 P1 Au1 3.9(7) . . . . ? F1 C1 P1 Au1 179.6(3) . . . . ? C3 P1 Au1 Cl1 152(2) . . . . ? C9 P1 Au1 Cl1 -84(2) . . . . ? C1 P1 Au1 Cl1 37(2) . . . . ? #===END data_Ph2CClCF2 _database_code_depnum_ccdc_archive 'CCDC 789439' #TrackingRef '- CIFS.cif' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C14 H10 Au Cl2 F2 P' _chemical_formula_sum 'C14 H10 Au Cl2 F2 P' _chemical_formula_weight 515.06 #----------------------------------------------------------------------------# # 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 10.2980(4) _cell_length_b 9.3190(3) _cell_length_c 16.0560(6) _cell_angle_alpha 90 _cell_angle_beta 100.631(2) _cell_angle_gamma 90 _cell_volume 1514.40(10) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3615 _cell_measurement_theta_min 2 _cell_measurement_theta_max 25.5 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.08 _exptl_crystal_density_diffrn 2.259 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 960 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 10.179 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2541 _exptl_absorpt_correction_T_max 0.3427 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_detector_area_resol_mean 9 _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 0.092119 _diffrn_orient_matrix_ub_12 0.0127733 _diffrn_orient_matrix_ub_13 -0.0103622 _diffrn_orient_matrix_ub_21 0.0201014 _diffrn_orient_matrix_ub_22 0.0652241 _diffrn_orient_matrix_ub_23 0.0501862 _diffrn_orient_matrix_ub_31 0.0295272 _diffrn_orient_matrix_ub_32 -0.0842531 _diffrn_orient_matrix_ub_33 0.0372804 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_av_unetI/netI 0.0529 _diffrn_reflns_number 2794 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.97 _diffrn_reflns_theta_max 25.5 _diffrn_reflns_theta_full 25.5 _diffrn_measured_fraction_theta_full 0.989 _diffrn_measured_fraction_theta_max 0.989 _reflns_number_total 2794 _reflns_number_gt 1908 _reflns_threshold_expression >2\s(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_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # 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^ > 2\s(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^)+(0.0708P)^2^+69.7591P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 2794 _refine_ls_number_parameters 181 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1124 _refine_ls_R_factor_gt 0.072 _refine_ls_wR_factor_ref 0.1954 _refine_ls_wR_factor_gt 0.1671 _refine_ls_goodness_of_fit_ref 1.09 _refine_ls_restrained_S_all 1.09 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 6.491 _refine_diff_density_min -2.363 _refine_diff_density_rms 0.367 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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 0.3182(17) 0.1906(19) 0.4360(11) 0.038(4) Uani 1 1 d . . . C2 C 0.292(2) 0.080(2) 0.3870(12) 0.048(5) Uani 1 1 d . . . C3 C 0.2689(16) 0.369(2) 0.5728(11) 0.039(4) Uani 1 1 d . . . C4 C 0.305(2) 0.272(2) 0.6386(12) 0.048(5) Uani 1 1 d . . . H4 H 0.2963 0.1743 0.6272 0.058 Uiso 1 1 calc R . . C5 C 0.353(2) 0.315(2) 0.7189(14) 0.056(5) Uani 1 1 d . . . H5 H 0.3742 0.2478 0.762 0.067 Uiso 1 1 calc R . . C6 C 0.371(2) 0.460(2) 0.7366(12) 0.052(5) Uani 1 1 d . . . H6 H 0.404 0.4901 0.7917 0.062 Uiso 1 1 calc R . . C7 C 0.341(2) 0.557(2) 0.6731(11) 0.047(5) Uani 1 1 d . . . H7 H 0.3548 0.6547 0.6843 0.057 Uiso 1 1 calc R . . C8 C 0.2899(18) 0.511(2) 0.5911(11) 0.043(4) Uani 1 1 d . . . H8 H 0.2696 0.5785 0.5479 0.051 Uiso 1 1 calc R . . C9 C 0.1835(19) 0.4636(19) 0.4004(11) 0.042(4) Uani 1 1 d . . . C10 C 0.292(2) 0.528(2) 0.3798(10) 0.044(4) Uani 1 1 d . . . H10 H 0.3743 0.4866 0.3986 0.053 Uiso 1 1 calc R . . C11 C 0.284(2) 0.655(2) 0.3309(13) 0.056(5) Uani 1 1 d . . . H11 H 0.3603 0.6997 0.3202 0.067 Uiso 1 1 calc R . . C12 C 0.159(2) 0.7108(19) 0.2991(12) 0.048(5) Uani 1 1 d . . . H12 H 0.1496 0.792 0.2648 0.058 Uiso 1 1 calc R . . C13 C 0.049(2) 0.643(2) 0.3195(14) 0.059(6) Uani 1 1 d . . . H13 H -0.0341 0.6812 0.2998 0.071 Uiso 1 1 calc R . . C14 C 0.0616(18) 0.521(2) 0.3688(11) 0.043(4) Uani 1 1 d . . . H14 H -0.0138 0.4762 0.3807 0.051 Uiso 1 1 calc R . . P1 P 0.1952(4) 0.3072(5) 0.4680(3) 0.0326(9) Uani 1 1 d . . . Au1 Au 0.00009(6) 0.20329(7) 0.46560(4) 0.0379(3) Uani 1 1 d . . . F1 F 0.1677(11) 0.0417(14) 0.3513(7) 0.057(3) Uani 1 1 d . . . F2 F 0.3746(12) -0.0094(12) 0.3639(7) 0.055(3) Uani 1 1 d . . . Cl1 Cl -0.2059(4) 0.1066(5) 0.4573(3) 0.0462(11) Uani 1 1 d . . . Cl2 Cl 0.4853(4) 0.2236(5) 0.4723(3) 0.0540(13) 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 0.038(9) 0.035(9) 0.040(9) -0.001(8) 0.003(7) -0.002(8) C2 0.050(11) 0.047(12) 0.045(11) 0.014(9) 0.003(9) -0.010(10) C3 0.028(8) 0.055(12) 0.035(9) 0.004(9) 0.006(7) -0.005(8) C4 0.057(12) 0.044(11) 0.042(11) 0.004(9) 0.002(9) -0.013(9) C5 0.046(11) 0.066(14) 0.052(12) 0.016(11) -0.002(9) -0.008(10) C6 0.051(12) 0.061(13) 0.042(11) -0.015(10) 0.004(9) -0.002(10) C7 0.058(12) 0.047(11) 0.037(10) -0.009(9) 0.008(9) 0.007(9) C8 0.043(10) 0.039(10) 0.044(10) 0.013(9) 0.003(8) 0.010(8) C9 0.050(11) 0.031(9) 0.043(10) -0.010(8) 0.008(8) -0.017(8) C10 0.059(12) 0.040(10) 0.030(9) 0.008(8) -0.001(8) -0.004(9) C11 0.060(13) 0.055(13) 0.051(12) 0.007(10) 0.012(10) -0.005(11) C12 0.075(14) 0.026(9) 0.043(10) 0.001(8) 0.009(10) 0.009(9) C13 0.049(12) 0.055(13) 0.067(14) 0.016(11) -0.004(10) 0.018(10) C14 0.040(10) 0.047(11) 0.039(9) 0.015(9) 0.003(8) -0.002(8) P1 0.029(2) 0.032(2) 0.035(2) 0.0024(19) 0.0008(17) -0.0029(18) Au1 0.0350(4) 0.0365(4) 0.0411(4) 0.0011(3) 0.0039(3) -0.0027(3) F1 0.048(7) 0.067(8) 0.054(7) -0.014(6) 0.005(5) -0.007(6) F2 0.067(7) 0.041(6) 0.060(7) -0.003(6) 0.017(6) 0.017(6) Cl1 0.035(2) 0.043(2) 0.061(3) 0.006(2) 0.008(2) -0.008(2) Cl2 0.033(2) 0.048(3) 0.077(4) 0.002(2) 0.000(2) 0.000(2) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.29(3) . ? C1 Cl2 1.739(18) . ? C1 P1 1.814(18) . ? C2 F2 1.29(2) . ? C2 F1 1.35(2) . ? C3 C8 1.37(3) . ? C3 C4 1.39(3) . ? C3 P1 1.807(18) . ? C4 C5 1.35(3) . ? C4 H4 0.93 . ? C5 C6 1.38(3) . ? C5 H5 0.93 . ? C6 C7 1.36(3) . ? C6 H6 0.93 . ? C7 C8 1.39(3) . ? C7 H7 0.93 . ? C8 H8 0.93 . ? C9 C10 1.36(3) . ? C9 C14 1.37(3) . ? C9 P1 1.808(19) . ? C10 C11 1.41(3) . ? C10 H10 0.93 . ? C11 C12 1.40(3) . ? C11 H11 0.93 . ? C12 C13 1.38(3) . ? C12 H12 0.93 . ? C13 C14 1.38(3) . ? C13 H13 0.93 . ? C14 H14 0.93 . ? P1 Au1 2.224(4) . ? Au1 Cl1 2.286(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 Cl2 115.2(15) . . ? C2 C1 P1 124.8(15) . . ? Cl2 C1 P1 120.0(10) . . ? C1 C2 F2 127.9(19) . . ? C1 C2 F1 123(2) . . ? F2 C2 F1 109.2(17) . . ? C8 C3 C4 117.3(17) . . ? C8 C3 P1 122.0(14) . . ? C4 C3 P1 120.7(15) . . ? C5 C4 C3 122(2) . . ? C5 C4 H4 118.9 . . ? C3 C4 H4 118.9 . . ? C4 C5 C6 120(2) . . ? C4 C5 H5 120.1 . . ? C6 C5 H5 120.1 . . ? C7 C6 C5 119.7(18) . . ? C7 C6 H6 120.2 . . ? C5 C6 H6 120.2 . . ? C6 C7 C8 119.7(19) . . ? C6 C7 H7 120.1 . . ? C8 C7 H7 120.1 . . ? C3 C8 C7 121.3(17) . . ? C3 C8 H8 119.3 . . ? C7 C8 H8 119.3 . . ? C10 C9 C14 118.4(18) . . ? C10 C9 P1 122.3(15) . . ? C14 C9 P1 119.3(14) . . ? C9 C10 C11 123(2) . . ? C9 C10 H10 118.6 . . ? C11 C10 H10 118.6 . . ? C12 C11 C10 118(2) . . ? C12 C11 H11 121.1 . . ? C10 C11 H11 121.1 . . ? C13 C12 C11 118.8(18) . . ? C13 C12 H12 120.6 . . ? C11 C12 H12 120.6 . . ? C12 C13 C14 121.3(19) . . ? C12 C13 H13 119.4 . . ? C14 C13 H13 119.4 . . ? C9 C14 C13 120.9(18) . . ? C9 C14 H14 119.6 . . ? C13 C14 H14 119.6 . . ? C9 P1 C3 105.9(8) . . ? C9 P1 C1 106.6(9) . . ? C3 P1 C1 105.0(8) . . ? C9 P1 Au1 112.4(6) . . ? C3 P1 Au1 112.2(6) . . ? C1 P1 Au1 114.2(6) . . ? P1 Au1 Cl1 176.55(16) . . ? #===END data_Et2CFCF2 _database_code_depnum_ccdc_archive 'CCDC 789440' #TrackingRef '- CIFS.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C6 H10 Au Cl F3 P' _chemical_formula_weight 402.53 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' Au Au -2.0133 8.8022 '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' F F 0.0171 0.0103 '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 17.114(2) _cell_length_b 7.3330(10) _cell_length_c 16.937(2) _cell_angle_alpha 90.00 _cell_angle_beta 93.01(2) _cell_angle_gamma 90.00 _cell_volume 2122.7(5) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.519 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1472 _exptl_absorpt_coefficient_mu 14.253 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.0998 _exptl_absorpt_correction_T_max 0.1628 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 1921 _diffrn_reflns_av_R_equivalents 0.0642 _diffrn_reflns_av_sigmaI/netI 0.0389 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.38 _diffrn_reflns_theta_max 24.97 _reflns_number_total 1855 _reflns_number_gt 1394 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0783P)^2^+4.8325P] 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 1855 _refine_ls_number_parameters 109 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0718 _refine_ls_R_factor_gt 0.0455 _refine_ls_wR_factor_ref 0.1230 _refine_ls_wR_factor_gt 0.1090 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.025 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Au1 Au 0.00047(2) 0.09810(8) 0.65125(3) 0.0506(2) Uani 1 d . . . Cl1 Cl -0.12284(19) -0.0155(7) 0.6573(2) 0.0733(11) Uani 1 d . . . P1 P 0.12059(17) 0.2013(6) 0.63724(19) 0.0524(8) Uani 1 d . . . C1 C 0.1961(7) 0.026(2) 0.6342(9) 0.071(4) Uani 1 d . . . H1A H 0.2456 0.0846 0.6249 0.085 Uiso 1 calc R . . H1B H 0.2014 -0.0323 0.6856 0.085 Uiso 1 calc R . . C2 C 0.1817(10) -0.117(2) 0.5736(13) 0.096(6) Uani 1 d . . . H2A H 0.2231 -0.2050 0.5775 0.144 Uiso 1 calc R . . H2B H 0.1798 -0.0621 0.5220 0.144 Uiso 1 calc R . . H2C H 0.1327 -0.1757 0.5818 0.144 Uiso 1 calc R . . C3 C 0.1582(9) 0.361(3) 0.7073(9) 0.082(6) Uani 1 d . . . H3A H 0.1673 0.2980 0.7574 0.098 Uiso 1 calc R . . H3B H 0.2086 0.4020 0.6906 0.098 Uiso 1 calc R . . C4 C 0.1086(12) 0.525(3) 0.7210(11) 0.109(7) Uani 1 d . . . H4A H 0.1347 0.6025 0.7599 0.164 Uiso 1 calc R . . H4B H 0.0591 0.4876 0.7394 0.164 Uiso 1 calc R . . H4C H 0.1004 0.5918 0.6723 0.164 Uiso 1 calc R . . C5 C 0.1315(8) 0.321(2) 0.5455(8) 0.064(4) Uani 1 d . . . C6 C 0.0810(9) 0.350(2) 0.4879(8) 0.067(4) Uani 1 d . . . F5 F 0.2020(5) 0.3971(15) 0.5377(6) 0.101(3) Uani 1 d . . . F6A F 0.0955(7) 0.4434(14) 0.4242(5) 0.098(3) Uani 1 d . . . F6B F 0.0102(5) 0.2872(15) 0.4827(5) 0.094(3) Uani 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 Au1 0.0504(3) 0.0515(4) 0.0498(3) -0.0036(3) 0.0030(2) -0.0096(2) Cl1 0.0593(17) 0.094(3) 0.067(2) -0.013(2) 0.0107(15) -0.025(2) P1 0.0504(16) 0.060(2) 0.0462(17) -0.0033(19) -0.0021(13) -0.0111(17) C1 0.055(7) 0.094(13) 0.064(9) 0.029(10) 0.007(6) 0.003(8) C2 0.097(12) 0.066(13) 0.125(17) 0.003(12) 0.010(11) -0.003(9) C3 0.069(9) 0.116(17) 0.061(9) -0.015(10) 0.008(7) -0.036(9) C4 0.148(18) 0.111(17) 0.071(11) -0.030(12) 0.036(12) -0.045(15) C5 0.066(8) 0.067(10) 0.059(8) -0.017(8) 0.011(7) -0.013(8) C6 0.086(10) 0.069(12) 0.047(8) -0.002(7) 0.012(7) -0.007(8) F5 0.085(6) 0.132(9) 0.085(6) 0.021(6) 0.010(5) -0.051(6) F6A 0.144(8) 0.092(8) 0.058(5) 0.030(5) 0.014(5) 0.015(6) F6B 0.089(6) 0.122(9) 0.067(6) -0.005(6) -0.017(4) -0.008(6) _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 P1 2.215(3) . ? Au1 Cl1 2.276(3) . ? Au1 Au1 3.3458(10) 2_556 ? P1 C3 1.762(16) . ? P1 C5 1.802(16) . ? P1 C1 1.826(15) . ? C1 C2 1.48(2) . ? C3 C4 1.50(3) . ? C5 C6 1.29(2) . ? C5 F5 1.343(15) . ? C6 F6B 1.294(16) . ? C6 F6A 1.315(16) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P1 Au1 Cl1 176.18(12) . . ? P1 Au1 Au1 99.22(9) . 2_556 ? Cl1 Au1 Au1 84.36(9) . 2_556 ? C3 P1 C5 102.0(8) . . ? C3 P1 C1 104.6(8) . . ? C5 P1 C1 102.3(7) . . ? C3 P1 Au1 117.6(5) . . ? C5 P1 Au1 113.4(4) . . ? C1 P1 Au1 115.1(5) . . ? C2 C1 P1 115.2(11) . . ? C4 C3 P1 116.6(12) . . ? C6 C5 F5 115.4(14) . . ? C6 C5 P1 129.6(11) . . ? F5 C5 P1 114.9(10) . . ? C5 C6 F6B 125.7(14) . . ? C5 C6 F6A 124.0(15) . . ? F6B C6 F6A 110.2(13) . . ? _diffrn_measured_fraction_theta_max 0.458 _diffrn_reflns_theta_full 24.97 _diffrn_measured_fraction_theta_full 0.458 _refine_diff_density_max 0.965 _refine_diff_density_min -1.564 _refine_diff_density_rms 0.213 #===END #------------------ SECTION 2. COMPOUND(S) DETAILS -------------------------# data_Cy2CFCF2 _database_code_depnum_ccdc_archive 'CCDC 789441' #TrackingRef '- CIFS_new.cif' _audit_creation_date 2010-10-22T00:20:03-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.4 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C14 H22 Au1 Cl1 F3 P1' _chemical_formula_sum 'C14 H22 Au Cl F3 P' _chemical_formula_weight 510.7 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.532(4) _cell_length_b 9.156(2) _cell_length_c 19.213(6) _cell_angle_alpha 90 _cell_angle_beta 102.47(3) _cell_angle_gamma 90 _cell_volume 1637.2(9) _cell_formula_units_Z 4 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 10 _cell_measurement_theta_max 16 _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 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 2.072 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 976 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 9.264 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details ; North A.C.T., Phillips D.C. & Mathews F.S. (1968) Acta. Cryst. A24, 351 Number of psi-scan sets used was 4 Theta correction was applied. Averaged transmission function was used. No Fourier smoothing was applied. ; _exptl_absorpt_correction_T_min 0.3371 _exptl_absorpt_correction_T_max 0.4577 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 203(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_reflns_av_R_equivalents 0.0726 _diffrn_reflns_av_unetI/netI 0.0568 _diffrn_reflns_number 3037 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.11 _diffrn_reflns_theta_max 24.97 _diffrn_reflns_theta_full 24.97 _diffrn_measured_fraction_theta_full 0.992 _diffrn_measured_fraction_theta_max 0.992 _reflns_number_total 2855 _reflns_number_gt 2179 _reflns_threshold_expression >2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # 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^ > 2\s(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^)+(0.0445P)^2^+43.5685P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 2855 _refine_ls_number_parameters 181 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0831 _refine_ls_R_factor_gt 0.0521 _refine_ls_wR_factor_ref 0.1536 _refine_ls_wR_factor_gt 0.1356 _refine_ls_goodness_of_fit_ref 1.257 _refine_ls_restrained_S_all 1.256 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 2.161 _refine_diff_density_min -2.119 _refine_diff_density_rms 0.269 #----------------------------------------------------------------------------# # 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' F F 0.0171 0.0103 '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' Au Au -2.0133 8.8022 '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 0.45067(7) 0.03355(7) 0.35477(3) 0.0265(2) Uani 1 1 d . . . Cl1 Cl 0.3840(6) 0.2688(5) 0.3630(3) 0.0472(12) Uani 1 1 d . . . P1 P 0.5074(4) -0.2008(4) 0.3461(2) 0.0209(8) Uani 1 1 d . . . F1 F 0.7437(11) -0.3660(11) 0.3859(6) 0.045(3) Uani 1 1 d . . . F2 F 0.8689(10) -0.2152(13) 0.4986(6) 0.051(3) Uani 1 1 d . . . F3 F 0.7026(11) -0.0542(12) 0.4824(5) 0.047(3) Uani 1 1 d . . . C1 C 0.3815(18) -0.3237(17) 0.3778(9) 0.028(4) Uani 1 1 d U . . H1 H 0.4087 -0.426 0.3707 0.033 Uiso 1 1 calc R . . C2 C 0.3893(18) -0.298(2) 0.4568(9) 0.034(4) Uani 1 1 d . . . H2A H 0.4866 -0.319 0.4842 0.04 Uiso 1 1 calc R . . H2B H 0.3667 -0.1961 0.4651 0.04 Uiso 1 1 calc R . . C3 C 0.282(2) -0.398(2) 0.4807(11) 0.047(5) Uani 1 1 d . . . H3A H 0.2855 -0.3835 0.5315 0.056 Uiso 1 1 calc R . . H3B H 0.3071 -0.5005 0.4738 0.056 Uiso 1 1 calc R . . C4 C 0.1305(19) -0.367(2) 0.4378(11) 0.043(5) Uani 1 1 d . . . H4A H 0.0619 -0.4318 0.4538 0.052 Uiso 1 1 calc R . . H4B H 0.1044 -0.266 0.446 0.052 Uiso 1 1 calc R . . C5 C 0.122(2) -0.390(2) 0.3598(12) 0.049(5) Uani 1 1 d . . . H5A H 0.0258 -0.3652 0.333 0.059 Uiso 1 1 calc R . . H5B H 0.1397 -0.4934 0.351 0.059 Uiso 1 1 calc R . . C6 C 0.2328(19) -0.296(2) 0.3339(9) 0.040(4) Uani 1 1 d . . . H6A H 0.2307 -0.3187 0.2838 0.049 Uiso 1 1 calc R . . H6B H 0.2084 -0.193 0.3372 0.049 Uiso 1 1 calc R . . C7 C 0.5177(16) -0.2537(16) 0.2554(8) 0.023(3) Uani 1 1 d U . . H7 H 0.4284 -0.2177 0.2237 0.027 Uiso 1 1 calc R . . C8 C 0.641(2) -0.174(2) 0.2326(9) 0.038(4) Uani 1 1 d . . . H8A H 0.7329 -0.2068 0.2621 0.046 Uiso 1 1 calc R . . H8B H 0.6324 -0.0689 0.2395 0.046 Uiso 1 1 calc R . . C9 C 0.638(2) -0.2065(18) 0.1541(9) 0.037(4) Uani 1 1 d . . . H9A H 0.5505 -0.1641 0.1245 0.044 Uiso 1 1 calc R . . H9B H 0.7207 -0.1602 0.1406 0.044 Uiso 1 1 calc R . . C10 C 0.640(2) -0.3697(18) 0.1396(9) 0.036(4) Uani 1 1 d . . . H10A H 0.6328 -0.386 0.0885 0.043 Uiso 1 1 calc R . . H10B H 0.7322 -0.4106 0.1652 0.043 Uiso 1 1 calc R . . C11 C 0.5181(19) -0.447(2) 0.1632(9) 0.036(4) Uani 1 1 d . . . H11A H 0.5245 -0.5521 0.1551 0.043 Uiso 1 1 calc R . . H11B H 0.4263 -0.4122 0.1346 0.043 Uiso 1 1 calc R . . C12 C 0.5226(18) -0.4190(17) 0.2425(8) 0.026(4) Uani 1 1 d . . . H12A H 0.6108 -0.4602 0.2717 0.032 Uiso 1 1 calc R . . H12B H 0.4404 -0.4664 0.2562 0.032 Uiso 1 1 calc R . . C13 C 0.6805(18) -0.2423(18) 0.4009(9) 0.030(4) Uani 1 1 d . . . C14 C 0.7484(18) -0.1773(18) 0.4582(9) 0.031(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Au1 0.0385(4) 0.0167(3) 0.0247(3) -0.0008(3) 0.0076(2) 0.0032(3) Cl1 0.069(3) 0.024(2) 0.042(3) -0.0066(19) -0.001(2) 0.010(2) P1 0.029(2) 0.0129(19) 0.022(2) -0.0011(15) 0.0078(16) -0.0004(16) F1 0.046(6) 0.038(6) 0.045(6) -0.010(5) 0.000(5) 0.022(5) F2 0.029(6) 0.074(8) 0.045(7) -0.015(6) -0.002(5) 0.006(5) F3 0.055(7) 0.048(7) 0.036(6) -0.014(5) 0.004(5) -0.002(5) C1 0.039(7) 0.013(6) 0.033(7) -0.001(6) 0.014(6) 0.001(6) C2 0.034(9) 0.041(10) 0.027(9) -0.003(8) 0.010(7) 0.003(8) C3 0.064(13) 0.036(11) 0.044(11) 0.001(9) 0.021(10) 0.003(10) C4 0.039(11) 0.030(10) 0.071(14) -0.004(10) 0.033(10) -0.004(8) C5 0.038(11) 0.045(12) 0.068(14) -0.008(11) 0.019(10) -0.002(9) C6 0.043(11) 0.049(12) 0.027(9) -0.004(8) 0.002(8) 0.001(9) C7 0.026(7) 0.019(6) 0.023(6) 0.003(5) 0.007(5) 0.011(5) C8 0.047(11) 0.037(10) 0.036(10) 0.000(8) 0.019(8) -0.017(9) C9 0.059(12) 0.025(9) 0.033(10) 0.007(7) 0.023(9) -0.007(8) C10 0.051(11) 0.029(10) 0.032(10) -0.002(8) 0.017(8) 0.008(8) C11 0.047(11) 0.037(11) 0.026(9) -0.013(8) 0.012(7) 0.002(8) C12 0.031(9) 0.022(8) 0.029(9) -0.004(7) 0.011(7) 0.000(7) C13 0.036(9) 0.030(9) 0.027(9) 0.001(7) 0.016(7) 0.004(7) C14 0.038(10) 0.026(9) 0.033(9) -0.007(7) 0.018(8) 0.003(7) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 P1 2.228(4) . ? Au1 Cl1 2.261(4) . ? P1 C13 1.796(17) . ? P1 C7 1.832(15) . ? P1 C1 1.842(16) . ? F1 C13 1.343(18) . ? F2 C14 1.287(19) . ? F3 C14 1.329(18) . ? C1 C6 1.50(2) . ? C1 C2 1.52(2) . ? C1 H1 0.99 . ? C2 C3 1.52(3) . ? C2 H2A 0.98 . ? C2 H2B 0.98 . ? C3 C4 1.53(3) . ? C3 H3A 0.98 . ? C3 H3B 0.98 . ? C4 C5 1.50(3) . ? C4 H4A 0.98 . ? C4 H4B 0.98 . ? C5 C6 1.52(3) . ? C5 H5A 0.98 . ? C5 H5B 0.98 . ? C6 H6A 0.98 . ? C6 H6B 0.98 . ? C7 C8 1.52(2) . ? C7 C12 1.54(2) . ? C7 H7 0.99 . ? C8 C9 1.53(2) . ? C8 H8A 0.98 . ? C8 H8B 0.98 . ? C9 C10 1.52(2) . ? C9 H9A 0.98 . ? C9 H9B 0.98 . ? C10 C11 1.52(2) . ? C10 H10A 0.98 . ? C10 H10B 0.98 . ? C11 C12 1.54(2) . ? C11 H11A 0.98 . ? C11 H11B 0.98 . ? C12 H12A 0.98 . ? C12 H12B 0.98 . ? C13 C14 1.29(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P1 Au1 Cl1 177.76(18) . . ? C13 P1 C7 105.7(7) . . ? C13 P1 C1 105.0(8) . . ? C7 P1 C1 109.0(7) . . ? C13 P1 Au1 111.5(6) . . ? C7 P1 Au1 112.9(5) . . ? C1 P1 Au1 112.2(5) . . ? C6 C1 C2 111.8(14) . . ? C6 C1 P1 108.4(12) . . ? C2 C1 P1 109.9(11) . . ? C6 C1 H1 108.9 . . ? C2 C1 H1 108.9 . . ? P1 C1 H1 108.9 . . ? C3 C2 C1 108.5(14) . . ? C3 C2 H2A 110 . . ? C1 C2 H2A 110 . . ? C3 C2 H2B 110 . . ? C1 C2 H2B 110 . . ? H2A C2 H2B 108.4 . . ? C2 C3 C4 110.1(16) . . ? C2 C3 H3A 109.6 . . ? C4 C3 H3A 109.6 . . ? C2 C3 H3B 109.6 . . ? C4 C3 H3B 109.6 . . ? H3A C3 H3B 108.1 . . ? C5 C4 C3 110.6(15) . . ? C5 C4 H4A 109.5 . . ? C3 C4 H4A 109.5 . . ? C5 C4 H4B 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 108.1 . . ? C4 C5 C6 110.9(16) . . ? C4 C5 H5A 109.5 . . ? C6 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? C6 C5 H5B 109.5 . . ? H5A C5 H5B 108.1 . . ? C1 C6 C5 110.9(16) . . ? C1 C6 H6A 109.5 . . ? C5 C6 H6A 109.5 . . ? C1 C6 H6B 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 108 . . ? C8 C7 C12 111.8(13) . . ? C8 C7 P1 110.5(11) . . ? C12 C7 P1 115.0(11) . . ? C8 C7 H7 106.3 . . ? C12 C7 H7 106.3 . . ? P1 C7 H7 106.3 . . ? C7 C8 C9 109.7(14) . . ? C7 C8 H8A 109.7 . . ? C9 C8 H8A 109.7 . . ? C7 C8 H8B 109.7 . . ? C9 C8 H8B 109.7 . . ? H8A C8 H8B 108.2 . . ? C10 C9 C8 111.8(14) . . ? C10 C9 H9A 109.3 . . ? C8 C9 H9A 109.3 . . ? C10 C9 H9B 109.3 . . ? C8 C9 H9B 109.3 . . ? H9A C9 H9B 107.9 . . ? C11 C10 C9 111.0(14) . . ? C11 C10 H10A 109.4 . . ? C9 C10 H10A 109.4 . . ? C11 C10 H10B 109.4 . . ? C9 C10 H10B 109.4 . . ? H10A C10 H10B 108 . . ? C10 C11 C12 111.1(14) . . ? C10 C11 H11A 109.4 . . ? C12 C11 H11A 109.4 . . ? C10 C11 H11B 109.4 . . ? C12 C11 H11B 109.4 . . ? H11A C11 H11B 108 . . ? C11 C12 C7 109.2(13) . . ? C11 C12 H12A 109.8 . . ? C7 C12 H12A 109.8 . . ? C11 C12 H12B 109.8 . . ? C7 C12 H12B 109.8 . . ? H12A C12 H12B 108.3 . . ? C14 C13 F1 113.9(15) . . ? C14 C13 P1 128.9(13) . . ? F1 C13 P1 116.7(12) . . ? F2 C14 C13 127.3(15) . . ? F2 C14 F3 109.6(14) . . ? C13 C14 F3 123.1(16) . . ? 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 Cl1 Au1 P1 C13 -147(4) . . . . ? Cl1 Au1 P1 C7 95(4) . . . . ? Cl1 Au1 P1 C1 -29(4) . . . . ? C13 P1 C1 C6 -179.6(12) . . . . ? C7 P1 C1 C6 -66.7(13) . . . . ? Au1 P1 C1 C6 59.1(12) . . . . ? C13 P1 C1 C2 57.9(13) . . . . ? C7 P1 C1 C2 170.8(11) . . . . ? Au1 P1 C1 C2 -63.4(12) . . . . ? C6 C1 C2 C3 58.3(19) . . . . ? P1 C1 C2 C3 178.7(12) . . . . ? C1 C2 C3 C4 -59.2(19) . . . . ? C2 C3 C4 C5 60(2) . . . . ? C3 C4 C5 C6 -56(2) . . . . ? C2 C1 C6 C5 -56(2) . . . . ? P1 C1 C6 C5 -177.5(13) . . . . ? C4 C5 C6 C1 55(2) . . . . ? C13 P1 C7 C8 -56.8(13) . . . . ? C1 P1 C7 C8 -169.2(11) . . . . ? Au1 P1 C7 C8 65.4(12) . . . . ? C13 P1 C7 C12 71.0(13) . . . . ? C1 P1 C7 C12 -41.4(13) . . . . ? Au1 P1 C7 C12 -166.8(10) . . . . ? C12 C7 C8 C9 56.8(19) . . . . ? P1 C7 C8 C9 -173.7(12) . . . . ? C7 C8 C9 C10 -55(2) . . . . ? C8 C9 C10 C11 56(2) . . . . ? C9 C10 C11 C12 -57(2) . . . . ? C10 C11 C12 C7 57.1(18) . . . . ? C8 C7 C12 C11 -57.7(17) . . . . ? P1 C7 C12 C11 175.2(11) . . . . ? C7 P1 C13 C14 148.8(17) . . . . ? C1 P1 C13 C14 -96.0(18) . . . . ? Au1 P1 C13 C14 25.7(18) . . . . ? C7 P1 C13 F1 -39.0(14) . . . . ? C1 P1 C13 F1 76.2(13) . . . . ? Au1 P1 C13 F1 -162.0(10) . . . . ? F1 C13 C14 F2 3(3) . . . . ? P1 C13 C14 F2 175.6(14) . . . . ? F1 C13 C14 F3 -179.4(14) . . . . ? P1 C13 C14 F3 -7(3) . . . . ? #===END #------------------ SECTION 2. COMPOUND(S) DETAILS -------------------------# data_Ph2CF3 _database_code_depnum_ccdc_archive 'CCDC 789442' #TrackingRef '- CIFS_new.cif' _audit_creation_date 2010-10-23T20:44:38-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.4 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C13 H10 Au1 Cl1 F3 P1' _chemical_formula_sum 'C13 H10 Au Cl F3 P' _chemical_formula_weight 486.6 _chemical_compound_source 'synthesis as described' _chemical_absolute_configuration ad #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P n a 21' _symmetry_space_group_name_Hall 'P 2c -2n' _symmetry_Int_Tables_number 33 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x+1/2, y+1/2, z+1/2' 'x+1/2, -y+1/2, z' _cell_length_a 9.1057(3) _cell_length_b 13.7198(5) _cell_length_c 11.2174(5) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 1401.37(9) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 1922 _cell_measurement_theta_min 2 _cell_measurement_theta_max 26 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.13 _exptl_crystal_density_diffrn 2.306 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 904 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 10.817 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1923 _exptl_absorpt_correction_T_max 0.3971 _exptl_absorpt_process_details ; Blessing, R. H. (1995) Acta Cryst., A51, 33-38. ; #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 100(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 0.107827 _diffrn_orient_matrix_ub_12 -0.161876E-1 _diffrn_orient_matrix_ub_13 -0.40018E-2 _diffrn_orient_matrix_ub_21 0.134395E-1 _diffrn_orient_matrix_ub_22 0.343334E-1 _diffrn_orient_matrix_ub_23 0.666709E-1 _diffrn_orient_matrix_ub_31 -0.159187E-1 _diffrn_orient_matrix_ub_32 -0.806623E-1 _diffrn_orient_matrix_ub_33 0.291811E-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 0.094 _diffrn_reflns_av_unetI/netI 0.0514 _diffrn_reflns_number 11556 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.97 _diffrn_reflns_theta_max 25.39 _diffrn_reflns_theta_full 25.39 _diffrn_measured_fraction_theta_full 0.993 _diffrn_measured_fraction_theta_max 0.993 _reflns_number_total 2415 _reflns_number_gt 1908 _reflns_threshold_expression >2\s(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, 2008)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # 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^ > 2\s(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. Highest peak 5.19 at 0.1385 0.8419 0.4714 [ 1.70 A from AU1 ] Deepest hole -2.64 at 0.0512 0.8431 0.5074 [ 0.99 A from AU1 ] ; _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^)+(0.0362P)^2^+55.2229P] where P=(Fo^2^+2Fc^2^)/3' _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 0.0007(3) _refine_ls_number_reflns 2415 _refine_ls_number_parameters 174 _refine_ls_number_restraints 79 _refine_ls_R_factor_all 0.0869 _refine_ls_R_factor_gt 0.0631 _refine_ls_wR_factor_ref 0.1507 _refine_ls_wR_factor_gt 0.1339 _refine_ls_goodness_of_fit_ref 1.15 _refine_ls_restrained_S_all 1.135 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.50(3) _refine_diff_density_max 5.189 _refine_diff_density_min -2.643 _refine_diff_density_rms 0.323 #----------------------------------------------------------------------------# # 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' F F 0.0171 0.0103 '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' Au Au -2.0133 8.8022 '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 0.328(2) 0.5012(14) 0.6691(18) 0.030(4) Uani 1 1 d U . . C2 C 0.610(2) 0.4485(14) 0.5698(19) 0.031(5) Uani 1 1 d U . . C3 C 0.730(2) 0.4909(15) 0.5212(19) 0.031(4) Uani 1 1 d U . . H3 H 0.7201 0.5466 0.4716 0.038 Uiso 1 1 calc R . . C4 C 0.870(2) 0.4504(15) 0.5456(19) 0.035(5) Uani 1 1 d U . . H4 H 0.9547 0.4761 0.5073 0.042 Uiso 1 1 calc R . . C5 C 0.884(3) 0.3738(16) 0.625(2) 0.038(5) Uani 1 1 d U . . H5 H 0.9782 0.349 0.6441 0.046 Uiso 1 1 calc R . . C6 C 0.757(3) 0.3325(14) 0.677(2) 0.037(5) Uani 1 1 d U . . H6 H 0.7666 0.2795 0.7313 0.045 Uiso 1 1 calc R . . C7 C 0.620(2) 0.3689(15) 0.650(2) 0.032(5) Uani 1 1 d U . . H7 H 0.5346 0.3413 0.6845 0.039 Uiso 1 1 calc R . . C8 C 0.338(2) 0.4244(14) 0.4331(16) 0.032(5) Uani 1 1 d U . . C9 C 0.382(2) 0.3228(14) 0.4211(19) 0.032(4) Uani 1 1 d U . . H9 H 0.4646 0.2975 0.4631 0.038 Uiso 1 1 calc R . . C10 C 0.298(2) 0.2635(15) 0.344(2) 0.035(5) Uani 1 1 d U . . H10 H 0.3259 0.1974 0.3327 0.042 Uiso 1 1 calc R . . C11 C 0.176(3) 0.2979(17) 0.285(2) 0.038(5) Uani 1 1 d U . . H11 H 0.1181 0.2561 0.2364 0.046 Uiso 1 1 calc R . . C12 C 0.141(3) 0.3978(14) 0.2975(19) 0.033(5) Uani 1 1 d U . . H12 H 0.0603 0.4236 0.2536 0.04 Uiso 1 1 calc R . . C13 C 0.220(3) 0.4597(17) 0.373(2) 0.044(6) Uani 1 1 d U . . H13 H 0.1913 0.5259 0.3816 0.053 Uiso 1 1 calc R . . F1 F 0.2920(16) 0.4116(9) 0.7078(12) 0.047(3) Uani 1 1 d . . . F2 F 0.3917(16) 0.5482(9) 0.7582(12) 0.045(3) Uani 1 1 d . . . F3 F 0.1942(15) 0.5473(10) 0.6520(12) 0.045(3) Uani 1 1 d . . . P1 P 0.4394(6) 0.5048(4) 0.5293(5) 0.0270(11) Uani 1 1 d . . . Cl1 Cl 0.4677(7) 0.8174(4) 0.4133(6) 0.0420(13) Uani 1 1 d . . . Au1 Au 0.45228(7) 0.65875(4) 0.47035(13) 0.0294(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.030(8) 0.030(7) 0.030(8) 0.008(6) 0.004(7) 0.003(7) C2 0.036(8) 0.029(8) 0.027(8) -0.001(6) -0.007(7) 0.001(7) C3 0.040(8) 0.030(7) 0.024(7) -0.003(6) 0.000(7) -0.002(7) C4 0.036(8) 0.038(8) 0.030(8) 0.005(7) 0.018(7) -0.013(7) C5 0.037(9) 0.039(8) 0.038(9) -0.003(7) -0.004(7) 0.001(7) C6 0.044(9) 0.033(8) 0.035(8) -0.001(7) 0.000(7) -0.004(7) C7 0.033(8) 0.032(8) 0.032(8) 0.001(7) -0.006(7) -0.001(7) C8 0.034(8) 0.033(8) 0.029(9) 0.005(6) 0.005(6) 0.004(6) C9 0.021(8) 0.038(8) 0.036(8) 0.005(7) -0.009(6) -0.002(6) C10 0.034(8) 0.032(8) 0.038(8) -0.004(7) -0.003(7) -0.002(7) C11 0.041(9) 0.038(8) 0.035(8) 0.003(7) -0.011(7) 0.001(7) C12 0.039(8) 0.028(7) 0.032(8) 0.005(7) -0.010(7) 0.001(7) C13 0.042(9) 0.038(8) 0.052(9) -0.005(7) -0.008(8) -0.001(7) F1 0.052(9) 0.041(7) 0.048(8) 0.002(6) 0.010(7) -0.001(6) F2 0.056(9) 0.041(7) 0.038(8) -0.003(6) 0.010(7) -0.001(6) F3 0.043(8) 0.054(8) 0.037(7) -0.002(6) 0.000(6) 0.007(6) P1 0.032(3) 0.027(2) 0.022(2) -0.002(2) -0.002(2) -0.001(2) Cl1 0.050(3) 0.028(2) 0.048(3) 0.004(2) 0.009(3) 0.002(2) Au1 0.0313(4) 0.0241(3) 0.0329(4) 0.0007(5) 0.0003(8) 0.0002(3) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 F2 1.32(2) . ? C1 F1 1.34(2) . ? C1 F3 1.39(2) . ? C1 P1 1.87(2) . ? C2 C3 1.35(3) . ? C2 C7 1.42(3) . ? C2 P1 1.79(2) . ? C3 C4 1.42(3) . ? C4 C5 1.38(3) . ? C5 C6 1.41(3) . ? C6 C7 1.38(3) . ? C8 C13 1.36(3) . ? C8 C9 1.46(3) . ? C8 P1 1.80(2) . ? C9 C10 1.42(3) . ? C10 C11 1.37(3) . ? C11 C12 1.42(3) . ? C12 C13 1.40(3) . ? P1 Au1 2.217(5) . ? Cl1 Au1 2.274(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag F2 C1 F1 108.0(16) . . ? F2 C1 F3 105.5(16) . . ? F1 C1 F3 104.3(16) . . ? F2 C1 P1 112.6(14) . . ? F1 C1 P1 115.3(14) . . ? F3 C1 P1 110.4(13) . . ? C3 C2 C7 122(2) . . ? C3 C2 P1 114.3(16) . . ? C7 C2 P1 123.3(17) . . ? C2 C3 C4 118.7(19) . . ? C5 C4 C3 120(2) . . ? C4 C5 C6 120(2) . . ? C7 C6 C5 120(2) . . ? C6 C7 C2 119(2) . . ? C13 C8 C9 120.8(19) . . ? C13 C8 P1 119.1(16) . . ? C9 C8 P1 120.0(16) . . ? C10 C9 C8 117.1(19) . . ? C11 C10 C9 122(2) . . ? C10 C11 C12 118(2) . . ? C11 C12 C13 122(2) . . ? C8 C13 C12 120(2) . . ? C2 P1 C8 109.4(10) . . ? C2 P1 C1 104.2(10) . . ? C8 P1 C1 102.1(9) . . ? C2 P1 Au1 116.1(7) . . ? C8 P1 Au1 115.6(6) . . ? C1 P1 Au1 107.7(6) . . ? P1 Au1 Cl1 178.9(2) . . ? #===END #------------------ SECTION 2. COMPOUND(S) DETAILS -------------------------# data_Ph2C3F7 _database_code_depnum_ccdc_archive 'CCDC 789443' #TrackingRef '- CIFS_new.cif' _audit_creation_date 2010-10-23T17:56:49-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.4 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C15 H10 Au1 Cl1 F7 P1' _chemical_formula_sum 'C15 H10 Au Cl F7 P' _chemical_formula_weight 586.62 _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 16.037(2) _cell_length_b 11.7410(9) _cell_length_c 19.334(2) _cell_angle_alpha 90 _cell_angle_beta 109.717(4) _cell_angle_gamma 90 _cell_volume 3427.0(5) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 2893 _cell_measurement_theta_min 2 _cell_measurement_theta_max 26 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.04 _exptl_crystal_density_diffrn 2.274 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2192 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 8.901 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1952 _exptl_absorpt_correction_T_max 0.4405 _exptl_absorpt_process_details ; Blessing, R. H. (1995) Acta Cryst., A51, 33-38. ; #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 100(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 0.563013E-1 _diffrn_orient_matrix_ub_12 -0.386085E-1 _diffrn_orient_matrix_ub_13 0.18696E-2 _diffrn_orient_matrix_ub_21 -0.200942E-1 _diffrn_orient_matrix_ub_22 -0.713521E-1 _diffrn_orient_matrix_ub_23 0.178615E-1 _diffrn_orient_matrix_ub_31 -0.285313E-1 _diffrn_orient_matrix_ub_32 -0.259345E-1 _diffrn_orient_matrix_ub_33 -0.519245E-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 0.153 _diffrn_reflns_av_unetI/netI 0.0904 _diffrn_reflns_number 11857 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.45 _diffrn_reflns_theta_max 25.39 _diffrn_reflns_theta_full 25.39 _diffrn_measured_fraction_theta_full 0.909 _diffrn_measured_fraction_theta_max 0.909 _reflns_number_total 2861 _reflns_number_gt 1619 _reflns_threshold_expression >2\s(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 'SHELXD (Sheldrick, 2002)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # 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^ > 2\s(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. Highest peak 5.37 at 0.2351 0.7287 0.0241 [ 1.67 A from C12 ] Deepest hole -2.76 at 0.0992 0.7939 0.2211 [ 1.15 A from AU1 ] ; _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^)+(0.0100P)^2^+390.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 2861 _refine_ls_number_parameters 226 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1896 _refine_ls_R_factor_gt 0.1061 _refine_ls_wR_factor_ref 0.2484 _refine_ls_wR_factor_gt 0.2041 _refine_ls_goodness_of_fit_ref 1.267 _refine_ls_restrained_S_all 1.267 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 5.365 _refine_diff_density_min -2.764 _refine_diff_density_rms 0.369 #----------------------------------------------------------------------------# # 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' F F 0.0171 0.0103 '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 0.1668(11) 0.4700(15) 0.1684(11) 0.053(6) Uani 1 1 d . . . C2 C 0.1459(13) 0.4567(17) 0.0853(12) 0.065(6) Uani 1 1 d . . . C3 C 0.0920(10) 0.4208(14) 0.1878(10) 0.047(5) Uani 1 1 d . . . C4 C 0.2579(13) 0.6033(15) 0.2983(11) 0.057(6) Uani 1 1 d . . . C5 C 0.2188(14) 0.6467(15) 0.3436(11) 0.065(6) Uani 1 1 d . . . H5 H 0.1655 0.6851 0.3228 0.078 Uiso 1 1 calc R . . C6 C 0.2533(13) 0.6380(13) 0.4210(13) 0.070(7) Uani 1 1 d . . . H6 H 0.2249 0.6669 0.4519 0.083 Uiso 1 1 calc R . . C7 C 0.3362(13) 0.5802(16) 0.4466(12) 0.067(6) Uani 1 1 d . . . H7 H 0.3645 0.576 0.4971 0.08 Uiso 1 1 calc R . . C8 C 0.3744(11) 0.5343(13) 0.4064(10) 0.048(5) Uani 1 1 d . . . H8 H 0.4266 0.4941 0.4283 0.057 Uiso 1 1 calc R . . C9 C 0.3392(11) 0.5424(14) 0.3277(12) 0.058(5) Uani 1 1 d . . . H9 H 0.3677 0.5101 0.2978 0.069 Uiso 1 1 calc R . . C10 C 0.2806(12) 0.6671(13) 0.1540(11) 0.055(6) Uani 1 1 d . . . C11 C 0.2602(14) 0.7699(15) 0.1158(11) 0.062(6) Uani 1 1 d . . . H11 H 0.21 0.8108 0.1146 0.075 Uiso 1 1 calc R . . C12 C 0.3149(13) 0.8097(15) 0.0803(12) 0.065(6) Uani 1 1 d . . . H12 H 0.3025 0.8782 0.0548 0.078 Uiso 1 1 calc R . . C13 C 0.3886(11) 0.7474(14) 0.0827(9) 0.048(5) Uani 1 1 d . . . H13 H 0.426 0.7716 0.0579 0.057 Uiso 1 1 calc R . . C14 C 0.4059(11) 0.6440(16) 0.1248(12) 0.065(6) Uani 1 1 d . . . H14 H 0.4566 0.6023 0.1287 0.078 Uiso 1 1 calc R . . C15 C 0.3486(12) 0.6044(16) 0.1599(13) 0.067(7) Uani 1 1 d . . . H15 H 0.3589 0.5364 0.1861 0.08 Uiso 1 1 calc R . . Cl1 Cl -0.0446(3) 0.8440(4) 0.1430(3) 0.0588(14) Uani 1 1 d . . . F1 F 0.2363(7) 0.3967(8) 0.1975(7) 0.067(4) Uani 1 1 d . . . F2 F 0.0979(7) 0.3616(8) 0.0570(7) 0.070(4) Uani 1 1 d . . . F3 F 0.2163(8) 0.4540(9) 0.0640(6) 0.072(4) Uani 1 1 d . . . F4 F 0.0954(8) 0.5463(9) 0.0455(7) 0.069(4) Uani 1 1 d . . . F5 F 0.0120(8) 0.4674(9) 0.1450(7) 0.076(4) Uani 1 1 d . . . F6 F 0.1007(7) 0.4557(9) 0.2583(6) 0.064(3) Uani 1 1 d . . . F7 F 0.0865(7) 0.3108(8) 0.1844(6) 0.057(3) Uani 1 1 d . . . P1 P 0.2003(3) 0.6198(4) 0.2001(3) 0.0533(14) Uani 1 1 d . . . Au1 Au 0.07917(5) 0.72981(6) 0.17351(5) 0.0588(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 0.038(9) 0.054(10) 0.066(13) 0.002(9) 0.014(9) 0.010(8) C2 0.049(11) 0.072(12) 0.075(14) -0.021(10) 0.022(10) -0.003(9) C3 0.026(8) 0.050(9) 0.068(13) 0.002(8) 0.018(8) -0.006(7) C4 0.064(11) 0.058(10) 0.047(11) -0.012(8) 0.017(9) -0.023(9) C5 0.089(13) 0.044(9) 0.064(13) 0.020(8) 0.030(11) -0.015(9) C6 0.069(12) 0.016(7) 0.118(18) 0.002(9) 0.024(12) 0.003(8) C7 0.075(12) 0.066(11) 0.072(13) 0.029(9) 0.042(10) 0.025(10) C8 0.047(9) 0.031(8) 0.070(12) 0.006(7) 0.028(9) 0.011(7) C9 0.054(10) 0.045(10) 0.094(14) 0.000(8) 0.052(9) -0.001(8) C10 0.050(10) 0.033(8) 0.074(13) -0.002(8) 0.012(10) -0.013(7) C11 0.077(13) 0.047(10) 0.051(12) -0.003(9) 0.006(10) 0.006(10) C12 0.076(12) 0.043(10) 0.094(14) -0.001(9) 0.053(11) -0.012(9) C13 0.037(9) 0.066(11) 0.028(9) -0.005(8) -0.005(8) -0.009(8) C14 0.036(9) 0.064(11) 0.111(16) -0.008(10) 0.047(9) -0.001(8) C15 0.049(10) 0.052(10) 0.096(16) 0.019(10) 0.021(11) 0.025(9) Cl1 0.057(3) 0.046(2) 0.077(3) 0.008(2) 0.028(2) 0.0119(19) F1 0.058(6) 0.049(6) 0.089(8) -0.002(5) 0.020(6) 0.005(5) F2 0.067(7) 0.036(5) 0.102(9) -0.008(5) 0.022(6) -0.007(5) F3 0.084(7) 0.066(7) 0.079(8) -0.008(5) 0.044(6) 0.011(6) F4 0.078(7) 0.054(6) 0.079(8) 0.005(5) 0.031(6) 0.003(5) F5 0.075(7) 0.044(6) 0.105(9) -0.002(6) 0.024(7) -0.012(5) F6 0.060(6) 0.063(6) 0.079(7) 0.005(5) 0.037(5) -0.007(5) F7 0.060(6) 0.042(5) 0.068(7) 0.007(5) 0.019(5) 0.001(5) P1 0.060(3) 0.033(2) 0.073(3) -0.001(2) 0.030(2) 0.000(2) Au1 0.0617(4) 0.0452(4) 0.0752(5) 0.0025(4) 0.0305(4) 0.0027(3) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 F1 1.370(19) . ? C1 C3 1.49(3) . ? C1 C2 1.54(3) . ? C1 P1 1.879(18) . ? C2 F3 1.33(3) . ? C2 F2 1.36(2) . ? C2 F4 1.39(2) . ? C3 F7 1.295(19) . ? C3 F5 1.383(18) . ? C3 F6 1.38(2) . ? C4 C5 1.34(3) . ? C4 C9 1.43(2) . ? C4 P1 1.820(19) . ? C5 C6 1.41(3) . ? C6 C7 1.42(3) . ? C7 C8 1.26(3) . ? C8 C9 1.44(3) . ? C10 C15 1.29(3) . ? C10 C11 1.39(2) . ? C10 P1 1.88(2) . ? C11 C12 1.37(3) . ? C12 C13 1.38(3) . ? C13 C14 1.44(3) . ? C14 C15 1.39(3) . ? Cl1 Au1 2.301(5) . ? P1 Au1 2.243(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag F1 C1 C3 105.4(15) . . ? F1 C1 C2 103.0(15) . . ? C3 C1 C2 108.3(15) . . ? F1 C1 P1 110.6(11) . . ? C3 C1 P1 116.5(14) . . ? C2 C1 P1 112.0(14) . . ? F3 C2 F2 106.3(16) . . ? F3 C2 F4 104.2(17) . . ? F2 C2 F4 104.7(14) . . ? F3 C2 C1 114.8(15) . . ? F2 C2 C1 113.5(18) . . ? F4 C2 C1 112.4(16) . . ? F7 C3 F5 109.3(12) . . ? F7 C3 F6 109.1(15) . . ? F5 C3 F6 103.7(14) . . ? F7 C3 C1 114.9(15) . . ? F5 C3 C1 111.0(15) . . ? F6 C3 C1 108.1(13) . . ? C5 C4 C9 119.9(18) . . ? C5 C4 P1 117.2(15) . . ? C9 C4 P1 122.9(16) . . ? C4 C5 C6 124(2) . . ? C5 C6 C7 113(2) . . ? C8 C7 C6 125(2) . . ? C7 C8 C9 121.7(17) . . ? C4 C9 C8 115.7(18) . . ? C15 C10 C11 126(2) . . ? C15 C10 P1 118.9(15) . . ? C11 C10 P1 115.5(15) . . ? C12 C11 C10 119(2) . . ? C11 C12 C13 119.4(18) . . ? C12 C13 C14 117.9(19) . . ? C15 C14 C13 121.7(17) . . ? C10 C15 C14 116.3(19) . . ? C4 P1 C1 103.2(8) . . ? C4 P1 C10 109.7(9) . . ? C1 P1 C10 106.8(9) . . ? C4 P1 Au1 113.3(7) . . ? C1 P1 Au1 109.5(6) . . ? C10 P1 Au1 113.5(6) . . ? P1 Au1 Cl1 178.4(2) . . ? #===END #------------------ SECTION 2. COMPOUND(S) DETAILS -------------------------# data_Ph2C4F9 _database_code_depnum_ccdc_archive 'CCDC 789444' #TrackingRef '- CIFS_new.cif' _audit_creation_date 2010-10-23T17:26:20-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.4 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C16 H10 Au1 Cl1 F9 P1' _chemical_formula_sum 'C16 H10 Au Cl F9 P' _chemical_formula_weight 636.63 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.8800(4) _cell_length_b 15.7970(4) _cell_length_c 15.9240(4) _cell_angle_alpha 90 _cell_angle_beta 95.226(1) _cell_angle_gamma 90 _cell_volume 3727.53(17) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9218 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 26.373 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 2.269 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2384 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 8.207 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3197 _exptl_absorpt_correction_T_max 0.4941 _exptl_absorpt_process_details ; Blessing, R. H. (1995) Acta Cryst., A51, 33-38. ; #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 100(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 0.662809E-1 _diffrn_orient_matrix_ub_12 0.35568E-2 _diffrn_orient_matrix_ub_13 0.169067E-1 _diffrn_orient_matrix_ub_21 -0.115318E-1 _diffrn_orient_matrix_ub_22 -0.82769E-2 _diffrn_orient_matrix_ub_23 0.603462E-1 _diffrn_orient_matrix_ub_31 0.52857E-2 _diffrn_orient_matrix_ub_32 -0.626589E-1 _diffrn_orient_matrix_ub_33 -0.70117E-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 0.079 _diffrn_reflns_av_unetI/netI 0.0439 _diffrn_reflns_number 77002 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.02 _diffrn_reflns_theta_max 25.4 _diffrn_reflns_theta_full 25.4 _diffrn_measured_fraction_theta_full 0.995 _diffrn_measured_fraction_theta_max 0.995 _reflns_number_total 6827 _reflns_number_gt 5075 _reflns_threshold_expression >2\s(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, 2008)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # 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^ > 2\s(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. Highest peak 2.15 at 0.8482 0.1367 0.1398 [ 0.06 A from AU1 ] Deepest hole -2.62 at 0.8994 0.1366 0.1748 [ 0.94 A from AU1 ] ; _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^)+(0.1096P)^2^+17.8805P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 6827 _refine_ls_number_parameters 495 _refine_ls_number_restraints 22 _refine_ls_R_factor_all 0.0839 _refine_ls_R_factor_gt 0.058 _refine_ls_wR_factor_ref 0.1688 _refine_ls_wR_factor_gt 0.1475 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.032 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0 _refine_diff_density_max 2.153 _refine_diff_density_min -2.622 _refine_diff_density_rms 0.238 #----------------------------------------------------------------------------# # 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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' 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 0.8316(6) 0.3210(6) 0.0290(5) 0.050(2) Uani 1 1 d . . . C2 C 0.9343(7) 0.3572(6) 0.0590(6) 0.044(3) Uiso 0.676(3) 1 d PD A 1 C3 C 0.7688(7) 0.3475(6) 0.0945(7) 0.049(3) Uiso 0.676(3) 1 d PD A 1 C4 C 0.7138(8) 0.4300(7) 0.0807(7) 0.072(5) Uiso 0.676(3) 1 d PD A 1 F2 F 0.9324(5) 0.4353(5) 0.0894(5) 0.0560(19) Uiso 0.676(3) 1 d PD A 1 F3 F 0.9750(5) 0.3060(5) 0.1177(5) 0.0548(19) Uiso 0.676(3) 1 d PD A 1 F4 F 0.9848(5) 0.3566(5) -0.0053(5) 0.064(2) Uiso 0.676(3) 1 d PD A 1 F5 F 0.8103(5) 0.3492(5) 0.1732(4) 0.0524(18) Uiso 0.676(3) 1 d PD A 1 F6 F 0.7014(5) 0.2849(5) 0.0921(5) 0.0554(19) Uiso 0.676(3) 1 d PD A 1 F7 F 0.6599(5) 0.4261(5) 0.0107(5) 0.067(2) Uiso 0.676(3) 1 d PD A 1 F8 F 0.6718(5) 0.4485(5) 0.1466(5) 0.062(2) Uiso 0.676(3) 1 d PD A 1 F9 F 0.7709(5) 0.4956(5) 0.0696(5) 0.069(2) Uiso 0.676(3) 1 d PD A 1 C2B C 0.7291(11) 0.3423(9) 0.0542(10) 0.055(7) Uiso 0.324(3) 1 d PD A 2 C3B C 0.9011(9) 0.3516(9) 0.0835(9) 0.040(6) Uiso 0.324(3) 1 d PD A 2 C4B C 0.9503(10) 0.4281(9) 0.0481(9) 0.060(8) Uiso 0.324(3) 1 d PD A 2 F2B F 0.7285(10) 0.4247(7) 0.0725(9) 0.045(4) Uiso 0.324(3) 1 d PD A 2 F3B F 0.7134(10) 0.2966(9) 0.1220(8) 0.047(4) Uiso 0.324(3) 1 d PD A 2 F4B F 0.6619(9) 0.3252(9) -0.0027(8) 0.056(4) Uiso 0.324(3) 1 d PD A 2 F5B F 0.8734(10) 0.3666(10) 0.1599(8) 0.063(4) Uiso 0.324(3) 1 d PD A 2 F6B F 0.9700(9) 0.2908(9) 0.0950(10) 0.055(4) Uiso 0.324(3) 1 d PD A 2 F7B F 0.9801(11) 0.4074(12) -0.0242(8) 0.076(5) Uiso 0.324(3) 1 d PD A 2 F8B F 1.0121(9) 0.4555(10) 0.1042(9) 0.064(4) Uiso 0.324(3) 1 d PD A 2 F9B F 0.8894(11) 0.4907(10) 0.0305(12) 0.087(6) Uiso 0.324(3) 1 d PD A 2 C5 C 0.9348(5) 0.1781(5) -0.0440(5) 0.0376(19) Uani 1 1 d . . . C6 C 0.9961(6) 0.1230(5) -0.0072(5) 0.048(2) Uani 1 1 d . A . H6 H 0.9909 0.1019 0.048 0.057 Uiso 1 1 calc R . . C7 C 1.0701(6) 0.0973(7) -0.0551(6) 0.058(3) Uani 1 1 d . . . H7 H 1.1134 0.0579 -0.0313 0.07 Uiso 1 1 calc R A . C8 C 1.0783(6) 0.1290(6) -0.1334(6) 0.054(2) Uani 1 1 d . A . H8 H 1.1264 0.1115 -0.1647 0.065 Uiso 1 1 calc R . . C9 C 1.0157(6) 0.1866(6) -0.1667(5) 0.051(2) Uani 1 1 d . . . H9 H 1.0217 0.2089 -0.2213 0.061 Uiso 1 1 calc R A . C10 C 0.9439(6) 0.2134(6) -0.1233(5) 0.047(2) Uani 1 1 d . A . H10 H 0.9023 0.2545 -0.1468 0.056 Uiso 1 1 calc R . . C11 C 0.7362(5) 0.1762(5) -0.0538(5) 0.040(2) Uani 1 1 d . . . C12 C 0.6765(6) 0.1196(6) -0.0235(6) 0.058(3) Uani 1 1 d . A . H12 H 0.6875 0.0992 0.0326 0.07 Uiso 1 1 calc R . . C13 C 0.6014(7) 0.0918(7) -0.0724(7) 0.074(3) Uani 1 1 d . . . H13 H 0.5613 0.0523 -0.0507 0.088 Uiso 1 1 calc R A . C14 C 0.5855(6) 0.1227(6) -0.1542(6) 0.059(3) Uani 1 1 d . A . H14 H 0.5334 0.1049 -0.1886 0.07 Uiso 1 1 calc R . . C15 C 0.6442(6) 0.1784(8) -0.1855(6) 0.068(3) Uani 1 1 d . . . H15 H 0.6339 0.1981 -0.242 0.081 Uiso 1 1 calc R A . C16 C 0.7190(6) 0.2061(8) -0.1346(6) 0.069(3) Uani 1 1 d . A . H16 H 0.7587 0.2462 -0.1559 0.083 Uiso 1 1 calc R . . C17 C 0.3074(6) 0.2833(5) 0.1228(5) 0.049(2) Uani 1 1 d . . . C18 C 0.2064(7) 0.3142(6) 0.1099(7) 0.068(3) Uani 1 1 d . . . C19 C 0.3757(8) 0.3544(7) 0.1127(6) 0.064(3) Uani 1 1 d . . . C20 C 0.4128(6) 0.3650(7) 0.0307(6) 0.063(3) Uani 1 1 d . . . C21 C 0.4354(5) 0.1688(5) 0.2237(5) 0.039(2) Uani 1 1 d . . . C22 C 0.4885(6) 0.1631(5) 0.2985(5) 0.049(2) Uani 1 1 d . . . H22 H 0.4716 0.191 0.3475 0.059 Uiso 1 1 calc R . . C23 C 0.5692(7) 0.1148(7) 0.3012(6) 0.066(3) Uani 1 1 d . . . H23 H 0.607 0.1109 0.3525 0.08 Uiso 1 1 calc R . . C24 C 0.5925(6) 0.0752(6) 0.2334(6) 0.051(2) Uani 1 1 d . . . H24 H 0.6463 0.0426 0.2365 0.061 Uiso 1 1 calc R . . C25 C 0.5396(6) 0.0810(6) 0.1588(6) 0.054(2) Uani 1 1 d . . . H25 H 0.5576 0.054 0.1097 0.065 Uiso 1 1 calc R . . C26 C 0.4596(6) 0.1263(6) 0.1550(6) 0.053(2) Uani 1 1 d . . . H26 H 0.4213 0.1278 0.1039 0.063 Uiso 1 1 calc R . . C27 C 0.2400(5) 0.1502(5) 0.2259(5) 0.041(2) Uani 1 1 d . . . C28 C 0.2348(5) 0.0790(6) 0.1725(5) 0.046(2) Uani 1 1 d . . . H28 H 0.2812 0.0695 0.1363 0.055 Uiso 1 1 calc R . . C29 C 0.1641(6) 0.0228(6) 0.1718(6) 0.057(3) Uani 1 1 d . . . H29 H 0.1612 -0.0246 0.1349 0.068 Uiso 1 1 calc R . . C30 C 0.0982(6) 0.0358(6) 0.2245(5) 0.054(2) Uani 1 1 d . . . H30 H 0.049 -0.0026 0.2234 0.065 Uiso 1 1 calc R . . C31 C 0.1014(6) 0.1034(6) 0.2792(6) 0.055(3) Uani 1 1 d . . . H31 H 0.0542 0.1123 0.3147 0.066 Uiso 1 1 calc R . . C32 C 0.1738(6) 0.1580(6) 0.2819(6) 0.054(2) Uani 1 1 d . . . H32 H 0.1788 0.2019 0.3229 0.064 Uiso 1 1 calc R . . Au1 Au 0.84478(2) 0.13506(2) 0.140238(18) 0.04027(8) Uani 1 1 d . . . Au2 Au 0.32917(2) 0.32165(2) 0.331162(18) 0.04084(9) Uani 1 1 d . . . Cl1 Cl 0.85079(12) 0.06900(13) 0.27023(10) 0.0412(5) Uani 1 1 d . A . Cl2 Cl 0.32675(15) 0.42236(13) 0.43341(11) 0.0476(5) Uani 1 1 d . . . F1 F 0.8146(4) 0.3584(3) -0.0469(3) 0.0576(15) Uani 1 1 d . A . F10 F 0.3137(3) 0.2258(3) 0.0574(3) 0.0493(13) Uani 1 1 d . . . F11 F 0.1509(4) 0.2485(4) 0.0944(4) 0.0737(18) Uani 1 1 d . . . F12 F 0.1817(3) 0.3529(4) 0.1737(4) 0.0686(17) Uani 1 1 d . . . F13 F 0.1943(4) 0.3621(4) 0.0401(4) 0.0635(16) Uani 1 1 d . . . F14 F 0.3345(4) 0.4289(3) 0.1313(3) 0.0689(17) Uani 1 1 d . . . F15 F 0.4484(4) 0.3470(4) 0.1684(3) 0.0685(17) Uani 1 1 d . . . F16 F 0.3459(5) 0.3648(5) -0.0369(4) 0.083(2) Uani 1 1 d . . . F17 F 0.4639(4) 0.2943(5) 0.0134(4) 0.085(2) Uani 1 1 d . . . F18 F 0.4619(5) 0.4299(5) 0.0249(4) 0.101(2) Uani 1 1 d . . . P1 P 0.83788(14) 0.19945(14) 0.01496(12) 0.0406(5) Uani 1 1 d . A . P2 P 0.32942(14) 0.22618(14) 0.22837(12) 0.0411(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.056(5) 0.072(6) 0.023(4) -0.003(4) 0.005(3) -0.004(4) C5 0.044(4) 0.037(4) 0.033(4) 0.001(3) 0.009(3) 0.000(3) C6 0.069(5) 0.037(4) 0.040(4) 0.002(3) 0.017(4) -0.002(4) C7 0.045(4) 0.066(6) 0.065(5) 0.008(5) 0.014(4) 0.022(4) C8 0.056(5) 0.056(5) 0.051(5) -0.005(4) 0.011(4) -0.018(4) C9 0.051(5) 0.067(6) 0.036(4) 0.001(4) 0.008(4) -0.016(4) C10 0.053(4) 0.056(5) 0.032(4) 0.014(4) 0.015(3) -0.009(4) C11 0.039(4) 0.054(5) 0.029(4) 0.006(3) 0.007(3) 0.003(4) C12 0.060(5) 0.060(6) 0.051(5) 0.024(4) -0.018(4) -0.005(5) C13 0.075(6) 0.073(7) 0.067(6) 0.023(5) -0.024(5) -0.029(5) C14 0.046(5) 0.065(6) 0.062(6) -0.001(5) -0.007(4) 0.001(4) C15 0.052(5) 0.118(9) 0.033(4) 0.009(5) 0.004(4) 0.000(6) C16 0.043(5) 0.127(9) 0.038(4) 0.018(5) 0.005(4) -0.012(5) C17 0.070(5) 0.045(5) 0.029(4) -0.016(3) -0.004(4) 0.015(4) C18 0.072(6) 0.048(5) 0.080(7) 0.010(5) -0.008(6) 0.015(5) C19 0.095(7) 0.055(6) 0.038(5) -0.004(4) -0.015(5) -0.011(5) C20 0.053(5) 0.087(7) 0.050(5) 0.027(5) 0.008(4) -0.010(5) C21 0.047(4) 0.032(4) 0.040(4) -0.006(3) 0.012(3) -0.001(3) C22 0.067(5) 0.042(4) 0.038(4) -0.002(4) 0.003(4) 0.016(4) C23 0.069(6) 0.081(7) 0.047(5) 0.007(5) -0.007(5) 0.022(5) C24 0.044(4) 0.051(5) 0.058(5) 0.002(4) 0.006(4) 0.005(4) C25 0.048(5) 0.068(6) 0.049(5) -0.011(4) 0.016(4) 0.002(4) C26 0.042(4) 0.066(6) 0.053(5) 0.006(4) 0.014(4) 0.010(4) C27 0.031(4) 0.044(4) 0.048(4) 0.000(4) 0.003(3) 0.008(3) C28 0.038(4) 0.051(5) 0.051(4) -0.008(4) 0.015(4) -0.002(4) C29 0.059(5) 0.040(5) 0.069(6) -0.011(4) -0.010(5) -0.001(4) C30 0.051(5) 0.067(6) 0.044(4) 0.008(4) -0.003(4) -0.007(4) C31 0.057(5) 0.050(5) 0.059(5) 0.004(4) 0.004(4) -0.003(4) C32 0.051(5) 0.049(5) 0.060(5) -0.003(4) 0.004(4) 0.003(4) Au1 0.04545(16) 0.04473(18) 0.03085(14) 0.00275(12) 0.00460(13) 0.00120(13) Au2 0.05249(18) 0.03720(17) 0.03307(15) -0.00341(12) 0.00519(13) -0.00390(13) Cl1 0.0436(9) 0.0559(12) 0.0240(8) 0.0008(8) 0.0026(7) -0.0007(9) Cl2 0.0701(12) 0.0409(10) 0.0321(9) -0.0060(8) 0.0063(9) -0.0138(9) F1 0.085(4) 0.047(3) 0.040(3) 0.010(2) 0.002(3) -0.003(3) F10 0.066(3) 0.045(3) 0.035(2) -0.009(2) -0.006(2) 0.004(2) F11 0.056(3) 0.061(4) 0.102(4) 0.007(3) -0.003(3) -0.008(3) F12 0.050(3) 0.097(4) 0.060(3) -0.009(3) 0.015(3) 0.007(3) F13 0.064(3) 0.062(3) 0.063(3) 0.013(3) -0.001(3) 0.002(3) F14 0.114(4) 0.036(3) 0.056(3) -0.007(2) 0.008(3) -0.004(3) F15 0.050(3) 0.102(4) 0.054(3) 0.004(3) 0.002(3) -0.012(3) F16 0.094(4) 0.109(5) 0.046(3) 0.006(3) 0.001(3) -0.001(4) F17 0.075(4) 0.110(5) 0.072(4) -0.010(4) 0.018(3) 0.004(4) F18 0.109(5) 0.131(6) 0.064(4) 0.015(4) 0.014(4) -0.039(5) P1 0.0469(11) 0.0466(11) 0.0288(9) 0.0031(9) 0.0053(8) 0.0060(9) P2 0.0471(11) 0.0418(11) 0.0341(9) -0.0059(9) 0.0023(9) -0.0021(9) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 F1 1.348(9) . ? C1 C3B 1.376(17) . ? C1 C3 1.521(13) . ? C1 C2B 1.647(19) . ? C1 C2 1.661(13) . ? C1 P1 1.936(10) . ? C2 F4 1.324(12) . ? C2 F2 1.326(12) . ? C2 F3 1.339(12) . ? C3 F5 1.347(12) . ? C3 F6 1.406(12) . ? C3 C4 1.544(14) . ? C4 F8 1.302(13) . ? C4 F7 1.315(13) . ? C4 F9 1.361(14) . ? C2B F4B 1.314(17) . ? C2B F2B 1.334(16) . ? C2B F3B 1.337(17) . ? C3B F5B 1.341(16) . ? C3B F6B 1.405(16) . ? C3B C4B 1.545(17) . ? C4B F8B 1.297(16) . ? C4B F7B 1.313(17) . ? C4B F9B 1.352(17) . ? C5 C6 1.356(11) . ? C5 C10 1.398(10) . ? C5 P1 1.823(8) . ? C6 C7 1.453(13) . ? C6 H6 0.95 . ? C7 C8 1.360(13) . ? C7 H7 0.95 . ? C8 C9 1.374(13) . ? C8 H8 0.95 . ? C9 C10 1.389(12) . ? C9 H9 0.95 . ? C10 H10 0.95 . ? C11 C16 1.373(12) . ? C11 C12 1.379(12) . ? C11 P1 1.822(8) . ? C12 C13 1.374(13) . ? C12 H12 0.95 . ? C13 C14 1.392(14) . ? C13 H13 0.95 . ? C14 C15 1.366(14) . ? C14 H14 0.95 . ? C15 C16 1.387(13) . ? C15 H15 0.95 . ? C16 H16 0.95 . ? C17 F10 1.392(9) . ? C17 C19 1.533(14) . ? C17 C18 1.576(14) . ? C17 P2 1.910(8) . ? C18 F12 1.269(13) . ? C18 F11 1.335(12) . ? C18 F13 1.342(12) . ? C19 F15 1.341(11) . ? C19 F14 1.372(12) . ? C19 C20 1.473(14) . ? C20 F18 1.267(12) . ? C20 F17 1.392(13) . ? C20 F16 1.397(11) . ? C21 C26 1.360(12) . ? C21 C22 1.371(11) . ? C21 P2 1.826(8) . ? C22 C23 1.421(13) . ? C22 H22 0.95 . ? C23 C24 1.321(14) . ? C23 H23 0.95 . ? C24 C25 1.367(12) . ? C24 H24 0.95 . ? C25 C26 1.386(12) . ? C25 H25 0.95 . ? C26 H26 0.95 . ? C27 C32 1.393(13) . ? C27 C28 1.408(12) . ? C27 P2 1.790(8) . ? C28 C29 1.376(12) . ? C28 H28 0.95 . ? C29 C30 1.363(13) . ? C29 H29 0.95 . ? C30 C31 1.377(13) . ? C30 H30 0.95 . ? C31 C32 1.378(13) . ? C31 H31 0.95 . ? C32 H32 0.95 . ? Au1 P1 2.233(2) . ? Au1 Cl1 2.3126(18) . ? Au2 P2 2.226(2) . ? Au2 Cl2 2.2789(19) . ? 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 F1 C1 C3B 118.7(9) . . ? F1 C1 C3 114.6(8) . . ? C3B C1 C3 86.8(9) . . ? F1 C1 C2B 91.5(8) . . ? C3B C1 C2B 115.7(10) . . ? C3 C1 C2B 30.2(6) . . ? F1 C1 C2 101.5(7) . . ? C3B C1 C2 22.8(7) . . ? C3 C1 C2 108.3(7) . . ? C2B C1 C2 135.1(9) . . ? F1 C1 P1 109.7(5) . . ? C3B C1 P1 112.3(8) . . ? C3 C1 P1 113.0(6) . . ? C2B C1 P1 106.6(7) . . ? C2 C1 P1 108.8(6) . . ? F4 C2 F2 108.8(9) . . ? F4 C2 F3 106.5(9) . . ? F2 C2 F3 109.3(8) . . ? F4 C2 C1 110.3(8) . . ? F2 C2 C1 112.0(8) . . ? F3 C2 C1 109.8(8) . . ? F5 C3 F6 107.7(8) . . ? F5 C3 C1 112.7(8) . . ? F6 C3 C1 105.6(8) . . ? F5 C3 C4 107.9(8) . . ? F6 C3 C4 102.9(8) . . ? C1 C3 C4 119.1(9) . . ? F8 C4 F7 113.1(10) . . ? F8 C4 F9 106.5(9) . . ? F7 C4 F9 105.4(9) . . ? F8 C4 C3 111.3(9) . . ? F7 C4 C3 110.8(9) . . ? F9 C4 C3 109.4(9) . . ? F4B C2B F2B 109.3(14) . . ? F4B C2B F3B 105.5(14) . . ? F2B C2B F3B 110.1(14) . . ? F4B C2B C1 117.0(13) . . ? F2B C2B C1 106.1(12) . . ? F3B C2B C1 108.7(12) . . ? F5B C3B C1 111.0(12) . . ? F5B C3B F6B 106.5(13) . . ? C1 C3B F6B 109.9(12) . . ? F5B C3B C4B 112.8(13) . . ? C1 C3B C4B 113.5(11) . . ? F6B C3B C4B 102.6(11) . . ? F8B C4B F7B 114.3(14) . . ? F8B C4B F9B 108.5(14) . . ? F7B C4B F9B 105.9(14) . . ? F8B C4B C3B 109.9(13) . . ? F7B C4B C3B 109.5(13) . . ? F9B C4B C3B 108.5(13) . . ? C6 C5 C10 122.0(8) . . ? C6 C5 P1 115.4(6) . . ? C10 C5 P1 122.6(6) . . ? C5 C6 C7 117.7(8) . . ? C5 C6 H6 121.2 . . ? C7 C6 H6 121.2 . . ? C8 C7 C6 121.0(8) . . ? C8 C7 H7 119.5 . . ? C6 C7 H7 119.5 . . ? C7 C8 C9 118.9(9) . . ? C7 C8 H8 120.6 . . ? C9 C8 H8 120.6 . . ? C8 C9 C10 122.4(8) . . ? C8 C9 H9 118.8 . . ? C10 C9 H9 118.8 . . ? C9 C10 C5 118.0(8) . . ? C9 C10 H10 121 . . ? C5 C10 H10 121 . . ? C16 C11 C12 118.7(8) . . ? C16 C11 P1 124.6(7) . . ? C12 C11 P1 116.6(6) . . ? C13 C12 C11 121.8(9) . . ? C13 C12 H12 119.1 . . ? C11 C12 H12 119.1 . . ? C12 C13 C14 118.6(10) . . ? C12 C13 H13 120.7 . . ? C14 C13 H13 120.7 . . ? C15 C14 C13 120.5(9) . . ? C15 C14 H14 119.7 . . ? C13 C14 H14 119.7 . . ? C14 C15 C16 119.7(9) . . ? C14 C15 H15 120.1 . . ? C16 C15 H15 120.1 . . ? C11 C16 C15 120.7(10) . . ? C11 C16 H16 119.6 . . ? C15 C16 H16 119.6 . . ? F10 C17 C19 108.0(7) . . ? F10 C17 C18 103.4(7) . . ? C19 C17 C18 113.1(8) . . ? F10 C17 P2 109.4(5) . . ? C19 C17 P2 112.1(6) . . ? C18 C17 P2 110.3(6) . . ? F12 C18 F11 107.6(9) . . ? F12 C18 F13 111.5(8) . . ? F11 C18 F13 104.6(8) . . ? F12 C18 C17 112.7(8) . . ? F11 C18 C17 110.4(8) . . ? F13 C18 C17 109.7(9) . . ? F15 C19 F14 106.4(7) . . ? F15 C19 C20 104.5(9) . . ? F14 C19 C20 107.8(8) . . ? F15 C19 C17 111.7(8) . . ? F14 C19 C17 107.0(9) . . ? C20 C19 C17 118.8(8) . . ? F18 C20 F17 107.8(8) . . ? F18 C20 F16 108.8(8) . . ? F17 C20 F16 102.1(8) . . ? F18 C20 C19 114.9(9) . . ? F17 C20 C19 109.9(8) . . ? F16 C20 C19 112.5(8) . . ? C26 C21 C22 119.5(8) . . ? C26 C21 P2 124.8(6) . . ? C22 C21 P2 115.4(6) . . ? C21 C22 C23 118.7(8) . . ? C21 C22 H22 120.6 . . ? C23 C22 H22 120.6 . . ? C24 C23 C22 120.9(9) . . ? C24 C23 H23 119.6 . . ? C22 C23 H23 119.6 . . ? C23 C24 C25 120.4(9) . . ? C23 C24 H24 119.8 . . ? C25 C24 H24 119.8 . . ? C24 C25 C26 119.7(8) . . ? C24 C25 H25 120.1 . . ? C26 C25 H25 120.1 . . ? C21 C26 C25 120.7(8) . . ? C21 C26 H26 119.7 . . ? C25 C26 H26 119.7 . . ? C32 C27 C28 117.0(8) . . ? C32 C27 P2 119.6(7) . . ? C28 C27 P2 123.3(6) . . ? C29 C28 C27 121.3(8) . . ? C29 C28 H28 119.3 . . ? C27 C28 H28 119.3 . . ? C30 C29 C28 119.3(9) . . ? C30 C29 H29 120.3 . . ? C28 C29 H29 120.3 . . ? C29 C30 C31 121.4(9) . . ? C29 C30 H30 119.3 . . ? C31 C30 H30 119.3 . . ? C30 C31 C32 119.1(9) . . ? C30 C31 H31 120.4 . . ? C32 C31 H31 120.4 . . ? C31 C32 C27 121.4(9) . . ? C31 C32 H32 119.3 . . ? C27 C32 H32 119.3 . . ? P1 Au1 Cl1 179.50(8) . . ? P2 Au2 Cl2 178.18(8) . . ? C11 P1 C5 107.8(3) . . ? C11 P1 C1 102.9(4) . . ? C5 P1 C1 106.9(4) . . ? C11 P1 Au1 114.4(3) . . ? C5 P1 Au1 113.7(3) . . ? C1 P1 Au1 110.3(2) . . ? C27 P2 C21 108.0(4) . . ? C27 P2 C17 103.3(4) . . ? C21 P2 C17 106.1(4) . . ? C27 P2 Au2 114.8(3) . . ? C21 P2 Au2 115.2(3) . . ? C17 P2 Au2 108.4(3) . . ? 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 F1 C1 C2 F4 -41.7(10) . . . . ? C3B C1 C2 F4 177(2) . . . . ? C3 C1 C2 F4 -162.8(8) . . . . ? C2B C1 C2 F4 -145.8(11) . . . . ? P1 C1 C2 F4 74.0(8) . . . . ? F1 C1 C2 F2 79.6(9) . . . . ? C3B C1 C2 F2 -61.6(17) . . . . ? C3 C1 C2 F2 -41.4(10) . . . . ? C2B C1 C2 F2 -24.4(16) . . . . ? P1 C1 C2 F2 -164.7(6) . . . . ? F1 C1 C2 F3 -158.8(8) . . . . ? C3B C1 C2 F3 60.0(17) . . . . ? C3 C1 C2 F3 80.2(10) . . . . ? C2B C1 C2 F3 97.2(13) . . . . ? P1 C1 C2 F3 -43.0(9) . . . . ? F1 C1 C3 F5 -146.4(8) . . . . ? C3B C1 C3 F5 -26.1(11) . . . . ? C2B C1 C3 F5 170.4(16) . . . . ? C2 C1 C3 F5 -33.8(10) . . . . ? P1 C1 C3 F5 86.9(8) . . . . ? F1 C1 C3 F6 96.3(9) . . . . ? C3B C1 C3 F6 -143.4(8) . . . . ? C2B C1 C3 F6 53.1(12) . . . . ? C2 C1 C3 F6 -151.1(7) . . . . ? P1 C1 C3 F6 -30.5(9) . . . . ? F1 C1 C3 C4 -18.5(12) . . . . ? C3B C1 C3 C4 101.8(10) . . . . ? C2B C1 C3 C4 -61.8(13) . . . . ? C2 C1 C3 C4 94.1(10) . . . . ? P1 C1 C3 C4 -145.3(7) . . . . ? F5 C3 C4 F8 -42.6(12) . . . . ? F6 C3 C4 F8 71.1(11) . . . . ? C1 C3 C4 F8 -172.6(9) . . . . ? F5 C3 C4 F7 -169.3(9) . . . . ? F6 C3 C4 F7 -55.7(11) . . . . ? C1 C3 C4 F7 60.6(12) . . . . ? F5 C3 C4 F9 74.8(11) . . . . ? F6 C3 C4 F9 -171.5(8) . . . . ? C1 C3 C4 F9 -55.2(12) . . . . ? F1 C1 C2B F4B 46.9(13) . . . . ? C3B C1 C2B F4B 170.0(13) . . . . ? C3 C1 C2B F4B -172(2) . . . . ? C2 C1 C2B F4B 154.9(11) . . . . ? P1 C1 C2B F4B -64.3(13) . . . . ? F1 C1 C2B F2B -75.4(11) . . . . ? C3B C1 C2B F2B 47.8(15) . . . . ? C3 C1 C2B F2B 66.1(13) . . . . ? C2 C1 C2B F2B 32.7(18) . . . . ? P1 C1 C2B F2B 173.5(9) . . . . ? F1 C1 C2B F3B 166.2(11) . . . . ? C3B C1 C2B F3B -70.7(14) . . . . ? C3 C1 C2B F3B -52.4(13) . . . . ? C2 C1 C2B F3B -85.8(15) . . . . ? P1 C1 C2B F3B 55.0(12) . . . . ? F1 C1 C3B F5B 129.0(12) . . . . ? C3 C1 C3B F5B 12.5(13) . . . . ? C2B C1 C3B F5B 21.7(16) . . . . ? C2 C1 C3B F5B 173(2) . . . . ? P1 C1 C3B F5B -101.1(12) . . . . ? F1 C1 C3B F6B -113.5(12) . . . . ? C3 C1 C3B F6B 130.1(11) . . . . ? C2B C1 C3B F6B 139.2(12) . . . . ? C2 C1 C3B F6B -69.1(18) . . . . ? P1 C1 C3B F6B 16.5(13) . . . . ? F1 C1 C3B C4B 0.8(15) . . . . ? C3 C1 C3B C4B -115.7(11) . . . . ? C2B C1 C3B C4B -106.6(12) . . . . ? C2 C1 C3B C4B 45.1(15) . . . . ? P1 C1 C3B C4B 130.7(10) . . . . ? F5B C3B C4B F8B 50.0(17) . . . . ? C1 C3B C4B F8B 177.3(13) . . . . ? F6B C3B C4B F8B -64.2(16) . . . . ? F5B C3B C4B F7B 176.3(14) . . . . ? C1 C3B C4B F7B -56.3(16) . . . . ? F6B C3B C4B F7B 62.1(16) . . . . ? F5B C3B C4B F9B -68.5(17) . . . . ? C1 C3B C4B F9B 58.8(16) . . . . ? F6B C3B C4B F9B 177.3(14) . . . . ? C10 C5 C6 C7 -3.6(12) . . . . ? P1 C5 C6 C7 174.1(7) . . . . ? C5 C6 C7 C8 1.3(14) . . . . ? C6 C7 C8 C9 0.6(14) . . . . ? C7 C8 C9 C10 -0.4(14) . . . . ? C8 C9 C10 C5 -1.7(13) . . . . ? C6 C5 C10 C9 3.8(12) . . . . ? P1 C5 C10 C9 -173.7(6) . . . . ? C16 C11 C12 C13 0.9(15) . . . . ? P1 C11 C12 C13 -174.4(9) . . . . ? C11 C12 C13 C14 -0.6(17) . . . . ? C12 C13 C14 C15 1.1(17) . . . . ? C13 C14 C15 C16 -1.7(17) . . . . ? C12 C11 C16 C15 -1.5(16) . . . . ? P1 C11 C16 C15 173.4(8) . . . . ? C14 C15 C16 C11 2.0(17) . . . . ? F10 C17 C18 F12 165.4(8) . . . . ? C19 C17 C18 F12 -78.0(10) . . . . ? P2 C17 C18 F12 48.5(10) . . . . ? F10 C17 C18 F11 45.0(10) . . . . ? C19 C17 C18 F11 161.6(8) . . . . ? P2 C17 C18 F11 -71.9(9) . . . . ? F10 C17 C18 F13 -69.8(9) . . . . ? C19 C17 C18 F13 46.9(10) . . . . ? P2 C17 C18 F13 173.3(6) . . . . ? F10 C17 C19 F15 -104.3(8) . . . . ? C18 C17 C19 F15 141.8(8) . . . . ? P2 C17 C19 F15 16.3(10) . . . . ? F10 C17 C19 F14 139.7(7) . . . . ? C18 C17 C19 F14 25.8(10) . . . . ? P2 C17 C19 F14 -99.7(7) . . . . ? F10 C17 C19 C20 17.5(12) . . . . ? C18 C17 C19 C20 -96.4(11) . . . . ? P2 C17 C19 C20 138.1(8) . . . . ? F15 C19 C20 F18 -61.2(11) . . . . ? F14 C19 C20 F18 51.7(12) . . . . ? C17 C19 C20 F18 173.5(9) . . . . ? F15 C19 C20 F17 60.5(10) . . . . ? F14 C19 C20 F17 173.4(7) . . . . ? C17 C19 C20 F17 -64.7(11) . . . . ? F15 C19 C20 F16 173.6(8) . . . . ? F14 C19 C20 F16 -73.5(11) . . . . ? C17 C19 C20 F16 48.3(13) . . . . ? C26 C21 C22 C23 2.0(13) . . . . ? P2 C21 C22 C23 176.0(7) . . . . ? C21 C22 C23 C24 -0.8(15) . . . . ? C22 C23 C24 C25 0.8(16) . . . . ? C23 C24 C25 C26 -2.1(15) . . . . ? C22 C21 C26 C25 -3.3(14) . . . . ? P2 C21 C26 C25 -176.7(7) . . . . ? C24 C25 C26 C21 3.4(14) . . . . ? C32 C27 C28 C29 4.4(12) . . . . ? P2 C27 C28 C29 -179.0(7) . . . . ? C27 C28 C29 C30 -0.8(13) . . . . ? C28 C29 C30 C31 -0.8(14) . . . . ? C29 C30 C31 C32 -1.4(14) . . . . ? C30 C31 C32 C27 5.3(14) . . . . ? C28 C27 C32 C31 -6.7(13) . . . . ? P2 C27 C32 C31 176.7(7) . . . . ? C16 C11 P1 C5 -50.0(10) . . . . ? C12 C11 P1 C5 125.0(7) . . . . ? C16 C11 P1 C1 62.8(9) . . . . ? C12 C11 P1 C1 -122.2(7) . . . . ? C16 C11 P1 Au1 -177.5(8) . . . . ? C12 C11 P1 Au1 -2.5(8) . . . . ? C6 C5 P1 C11 -124.7(6) . . . . ? C10 C5 P1 C11 53.0(8) . . . . ? C6 C5 P1 C1 125.3(6) . . . . ? C10 C5 P1 C1 -57.0(8) . . . . ? C6 C5 P1 Au1 3.3(7) . . . . ? C10 C5 P1 Au1 -179.1(6) . . . . ? F1 C1 P1 C11 -48.9(7) . . . . ? C3B C1 P1 C11 176.7(8) . . . . ? C3 C1 P1 C11 80.5(6) . . . . ? C2B C1 P1 C11 49.0(7) . . . . ? C2 C1 P1 C11 -159.1(5) . . . . ? F1 C1 P1 C5 64.6(7) . . . . ? C3B C1 P1 C5 -69.8(8) . . . . ? C3 C1 P1 C5 -166.1(6) . . . . ? C2B C1 P1 C5 162.4(7) . . . . ? C2 C1 P1 C5 -45.7(6) . . . . ? F1 C1 P1 Au1 -171.3(5) . . . . ? C3B C1 P1 Au1 54.3(8) . . . . ? C3 C1 P1 Au1 -42.0(7) . . . . ? C2B C1 P1 Au1 -73.5(7) . . . . ? C2 C1 P1 Au1 78.4(5) . . . . ? Cl1 Au1 P1 C11 -61(10) . . . . ? Cl1 Au1 P1 C5 18E1(10) . . . . ? Cl1 Au1 P1 C1 55(10) . . . . ? C32 C27 P2 C21 134.6(7) . . . . ? C28 C27 P2 C21 -41.9(8) . . . . ? C32 C27 P2 C17 -113.3(7) . . . . ? C28 C27 P2 C17 70.3(8) . . . . ? C32 C27 P2 Au2 4.5(8) . . . . ? C28 C27 P2 Au2 -172.0(6) . . . . ? C26 C21 P2 C27 69.4(8) . . . . ? C22 C21 P2 C27 -104.2(7) . . . . ? C26 C21 P2 C17 -40.8(8) . . . . ? C22 C21 P2 C17 145.6(7) . . . . ? C26 C21 P2 Au2 -160.8(7) . . . . ? C22 C21 P2 Au2 25.6(7) . . . . ? F10 C17 P2 C27 -62.0(6) . . . . ? C19 C17 P2 C27 178.1(6) . . . . ? C18 C17 P2 C27 51.1(7) . . . . ? F10 C17 P2 C21 51.5(7) . . . . ? C19 C17 P2 C21 -68.3(7) . . . . ? C18 C17 P2 C21 164.6(6) . . . . ? F10 C17 P2 Au2 175.8(5) . . . . ? C19 C17 P2 Au2 55.9(7) . . . . ? C18 C17 P2 Au2 -71.1(6) . . . . ? Cl2 Au2 P2 C27 -99(3) . . . . ? Cl2 Au2 P2 C21 135(3) . . . . ? Cl2 Au2 P2 C17 16(3) . . . . ? #===END # CIF produced by WinGX routine CIF_UPDATE # Created on 2001-10-24 at 17:30:39 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.2 # Request file : c:\chem\wingx\files\archive.dat # CIF files read : a dreduc struct sortav data_SO _database_code_depnum_ccdc_archive 'CCDC 789445' #TrackingRef '- CIFS.cif' _audit_creation_date 2001-10-24T17:30:39-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.2 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; thiodiethanol-S-oxide ; _chemical_formula_moiety 'C4 H10 O3 S1' _chemical_formula_structural 'C4 H10 S1 O3' _chemical_formula_sum 'C4 H10 O3 S' _chemical_formula_weight 138.18 _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 11.0805(4) _cell_length_b 4.7871(2) _cell_length_c 12.3153(5) _cell_angle_alpha 90 _cell_angle_beta 103.964(2) _cell_angle_gamma 90 _cell_volume 633.94(4) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 5380 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 28.283 _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 0.15 _exptl_crystal_density_diffrn 1.448 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 296 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.43 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; R.H. Blessing, Acta Cryst. (1995), A51, 33-38 ; _exptl_absorpt_correction_T_min 0.9383 _exptl_absorpt_correction_T_max 0.9383 #----------------------------------------------------------------------------# # 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_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 -0.657538E-1 _diffrn_orient_matrix_ub_12 0.142509 _diffrn_orient_matrix_ub_13 -0.293909E-1 _diffrn_orient_matrix_ub_21 0.297866E-1 _diffrn_orient_matrix_ub_22 0.113561 _diffrn_orient_matrix_ub_23 0.69463E-1 _diffrn_orient_matrix_ub_31 0.586315E-1 _diffrn_orient_matrix_ub_32 0.102137 _diffrn_orient_matrix_ub_33 -0.362239E-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 0.0371 _diffrn_reflns_av_unetI/netI 0.0412 _diffrn_reflns_number 7272 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.41 _diffrn_reflns_theta_max 28.28 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.99 _diffrn_measured_fraction_theta_max 0.99 _reflns_number_total 1563 _reflns_number_gt 1279 _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, 1990)' _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^)+(0.0360P)^2^+0.1181P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 1563 _refine_ls_number_parameters 113 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0441 _refine_ls_R_factor_gt 0.03 _refine_ls_wR_factor_ref 0.0745 _refine_ls_wR_factor_gt 0.0686 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.049 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.344 _refine_diff_density_min -0.287 _refine_diff_density_rms 0.058 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 '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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O1 O 0.62181(4) 0.25431(11) 0.38030(4) 0.02378(12) Uani 1 d . . . O4 O 0.61729(4) -0.07300(10) 0.64281(4) 0.02469(13) Uani 1 d . . . O7 O 0.92654(5) -0.04991(10) 0.33342(4) 0.02419(13) Uani 1 d . . . S1 S 0.734188(14) 0.13746(3) 0.464332(12) 0.01615(4) Uani 1 d . . . C2 C 0.73409(6) 0.30537(14) 0.59529(5) 0.02035(17) Uani 1 d . . . C3 C 0.61910(6) 0.22259(15) 0.63332(5) 0.02256(17) Uani 1 d . . . C5 C 0.86641(6) 0.32065(14) 0.43894(5) 0.01794(16) Uani 1 d . . . C6 C 0.89297(6) 0.23713(14) 0.32849(5) 0.02014(16) Uani 1 d . . . H2A H 0.8091(6) 0.2372(15) 0.6443(6) 0.0206(18) Uiso 1 d . . . H2B H 0.7345(7) 0.4973(17) 0.5824(6) 0.034(2) Uiso 1 d . . . H3A H 0.6243(7) 0.3121(16) 0.7073(6) 0.026(2) Uiso 1 d . . . H3B H 0.5454(6) 0.2924(15) 0.5821(6) 0.0191(18) Uiso 1 d . . . H4 H 0.5446(8) -0.1139(17) 0.6288(7) 0.043(3) Uiso 1 d . . . H5B H 0.8486(7) 0.5178(16) 0.4401(6) 0.030(2) Uiso 1 d . . . H5A H 0.9328(7) 0.2671(17) 0.4992(6) 0.028(2) Uiso 1 d . . . H6B H 0.8225(6) 0.2652(15) 0.2682(5) 0.0172(17) Uiso 1 d . . . H6A H 0.9641(7) 0.3526(15) 0.3173(6) 0.024(2) Uiso 1 d . . . H7 H 0.9117(8) -0.1087(16) 0.2692(7) 0.039(2) Uiso 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 O1 0.0168(2) 0.0342(3) 0.0187(2) 0.0041(2) 0.00089(17) -0.0042(2) O4 0.0189(2) 0.0246(2) 0.0307(2) 0.0053(2) 0.00625(19) -0.00204(19) O7 0.0337(2) 0.0210(2) 0.0172(2) -0.00175(19) 0.00475(19) 0.0049(2) S1 0.01805(7) 0.01497(7) 0.01572(7) -0.00070(6) 0.00466(5) -0.00263(6) C2 0.0237(3) 0.0205(3) 0.0173(3) -0.0033(3) 0.0057(2) -0.0029(3) C3 0.0248(3) 0.0236(3) 0.0210(3) -0.0013(3) 0.0090(2) -0.0006(3) C5 0.0167(3) 0.0161(3) 0.0215(3) -0.0009(3) 0.0056(2) -0.0027(2) C6 0.0217(3) 0.0201(3) 0.0194(3) 0.0038(3) 0.0065(2) 0.0018(3) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1 S1 1.5207(4) . ? O4 C3 1.4204(9) . ? O7 C6 1.4210(8) . ? S1 C5 1.7985(7) . ? S1 C2 1.8023(7) . ? C2 C3 1.5125(10) . ? C5 C6 1.5131(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 O1 S1 C5 105.66(3) . . ? O1 S1 C2 105.53(3) . . ? C5 S1 C2 96.58(3) . . ? C3 C2 S1 110.04(4) . . ? O4 C3 C2 108.43(6) . . ? C6 C5 S1 111.76(4) . . ? O7 C6 C5 108.83(5) . . ? 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 O1 S1 C2 C3 63.96(5) . . . . ? C5 S1 C2 C3 172.27(5) . . . . ? S1 C2 C3 O4 57.72(6) . . . . ? O1 S1 C5 C6 -69.74(5) . . . . ? C2 S1 C5 C6 -177.93(5) . . . . ? S1 C5 C6 O7 -64.19(6) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O4 H4 O1 0.806(9) 1.940(9) 2.7367(7) 169.4(9) 3_656 O4 H4 S1 0.806(9) 3.026(9) 3.8109(5) 165.0(8) 3_656 O7 H7 O1 0.818(8) 1.905(8) 2.7226(6) 179.7(9) 2_645 # END of CIF