# Supplementary Material (ESI) for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _publ_contact_author_name 'Flower, Kevin' _publ_contact_author_email k.r.flower@manchester.ac.uk _publ_section_title ; Structural relationships between o-, m- and p-tolyl substituted R3PEI2 (E = As, P) and [(R3P)AuX)] (R = As, P; X = Cl, Br, I). ; _publ_requested_category FO loop_ _publ_author_name K.Flower R.Pritchard S.Godfrey N.Barnes # Attachment '- Combined.cif' #\#N.A. Barnes et al Structural relationships between....submitted to CEngComm # CIF produced by WinGX routine CIF_UPDATE # Created on 2009-01-26 at 23:35:11 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.3 # Request file : c:\wingx\files\archive.dat # CIF files read : robin dreduc sortav struct data_1a _database_code_depnum_ccdc_archive 'CCDC 770652' #TrackingRef '- Combined.cif' _audit_creation_date 2009-01-26T23:35:11-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C21 H21 As1 I2' _chemical_formula_sum 'C21 H21 As I2' _chemical_formula_weight 601.93 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.2609(2) _cell_length_b 11.1853(3) _cell_length_c 11.6126(3) _cell_angle_alpha 61.9350(10) _cell_angle_beta 89.5740(10) _cell_angle_gamma 88.945(2) _cell_volume 1061.28(5) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 4164 _cell_measurement_theta_min 2 _cell_measurement_theta_max 27 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_diffrn 1.884 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 572 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 4.511 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; R.H. Blessing, Acta Cryst. (1995), A51, 33-38 ; _exptl_absorpt_correction_T_min 0.4973 _exptl_absorpt_correction_T_max 0.551 #----------------------------------------------------------------------------# # 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 -0.69089E-1 _diffrn_orient_matrix_ub_12 0.701773E-1 _diffrn_orient_matrix_ub_13 -0.619403E-1 _diffrn_orient_matrix_ub_21 -0.94909E-2 _diffrn_orient_matrix_ub_22 0.400318E-1 _diffrn_orient_matrix_ub_23 0.607143E-1 _diffrn_orient_matrix_ub_31 0.82465E-1 _diffrn_orient_matrix_ub_32 0.611595E-1 _diffrn_orient_matrix_ub_33 -0.447284E-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 0.071 _diffrn_reflns_av_unetI/netI 0.0405 _diffrn_reflns_number 15020 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.99 _diffrn_reflns_theta_max 26 _diffrn_reflns_theta_full 26 _diffrn_measured_fraction_theta_full 0.98 _diffrn_measured_fraction_theta_max 0.98 _reflns_number_total 4092 _reflns_number_gt 2995 _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^)+(0.0625P)^2^+21.9376P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 4092 _refine_ls_number_parameters 220 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.097 _refine_ls_R_factor_gt 0.0673 _refine_ls_wR_factor_ref 0.1791 _refine_ls_wR_factor_gt 0.1538 _refine_ls_goodness_of_fit_ref 1.143 _refine_ls_restrained_S_all 1.143 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0 _refine_diff_density_max 5.139 _refine_diff_density_min -2.325 _refine_diff_density_rms 0.282 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' As As 0.05 2.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.474 1.812 '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 0.6967(10) 0.6886(10) 0.5109(10) 0.027(2) Uani 1 1 d . . . C2 C 0.7183(11) 0.8237(11) 0.4155(10) 0.031(2) Uani 1 1 d . . . C3 C 0.8061(11) 0.8461(11) 0.3097(10) 0.034(2) Uani 1 1 d . . . H3 H 0.8203 0.9362 0.2427 0.041 Uiso 1 1 calc R . . C4 C 0.8729(13) 0.7394(13) 0.3006(11) 0.040(3) Uani 1 1 d . . . H4 H 0.9358 0.7566 0.2298 0.048 Uiso 1 1 calc R . . C5 C 0.8481(12) 0.6063(13) 0.3954(12) 0.041(3) Uani 1 1 d . . . H5 H 0.8915 0.5325 0.3883 0.049 Uiso 1 1 calc R . . C6 C 0.7589(11) 0.5833(11) 0.5004(11) 0.033(2) Uani 1 1 d . . . H6 H 0.7413 0.4931 0.5654 0.04 Uiso 1 1 calc R . . C7 C 0.6508(12) 0.9443(11) 0.4210(12) 0.039(3) Uani 1 1 d . . . H7A H 0.6653 1.0258 0.3374 0.058 Uiso 1 1 calc R . . H7B H 0.6959 0.9559 0.4911 0.058 Uiso 1 1 calc R . . H7C H 0.5471 0.9298 0.438 0.058 Uiso 1 1 calc R . . C8 C 0.6019(11) 0.4530(10) 0.7738(9) 0.026(2) Uani 1 1 d . . . C9 C 0.7320(11) 0.3847(10) 0.8310(10) 0.028(2) Uani 1 1 d . . . C10 C 0.7280(11) 0.2444(11) 0.8986(11) 0.034(2) Uani 1 1 d . . . H10 H 0.8147 0.1953 0.9369 0.041 Uiso 1 1 calc R . . C11 C 0.6042(13) 0.1735(12) 0.9125(13) 0.044(3) Uani 1 1 d . . . H11 H 0.606 0.0773 0.9593 0.053 Uiso 1 1 calc R . . C12 C 0.4749(13) 0.2439(12) 0.8574(12) 0.044(3) Uani 1 1 d . . . H12 H 0.3881 0.1959 0.8679 0.052 Uiso 1 1 calc R . . C13 C 0.4748(11) 0.3839(12) 0.7876(11) 0.035(2) Uani 1 1 d . . . H13 H 0.388 0.4325 0.7491 0.042 Uiso 1 1 calc R . . C14 C 0.8714(10) 0.4555(11) 0.8217(11) 0.032(2) Uani 1 1 d . . . H14A H 0.9493 0.388 0.8614 0.048 Uiso 1 1 calc R . . H14B H 0.8617 0.5095 0.8677 0.048 Uiso 1 1 calc R . . H14C H 0.894 0.5151 0.7297 0.048 Uiso 1 1 calc R . . C15 C 0.3910(11) 0.6943(10) 0.6218(10) 0.032(2) Uani 1 1 d . . . C16 C 0.2909(12) 0.6901(11) 0.7145(11) 0.033(2) Uani 1 1 d . . . C17 C 0.1479(12) 0.7312(12) 0.6733(13) 0.039(3) Uani 1 1 d . . . H17 H 0.0774 0.7286 0.7342 0.047 Uiso 1 1 calc R . . C18 C 0.1085(12) 0.7759(12) 0.5432(12) 0.041(3) Uani 1 1 d . . . H18 H 0.0117 0.8036 0.516 0.049 Uiso 1 1 calc R . . C19 C 0.2102(13) 0.7798(13) 0.4546(13) 0.045(3) Uani 1 1 d . . . H19 H 0.1831 0.8092 0.3664 0.054 Uiso 1 1 calc R . . C20 C 0.3509(12) 0.7411(11) 0.4931(10) 0.032(2) Uani 1 1 d . . . H20 H 0.4211 0.7467 0.4307 0.038 Uiso 1 1 calc R . . C21 C 0.3265(13) 0.6393(14) 0.8560(12) 0.044(3) Uani 1 1 d . . . H21A H 0.3263 0.54 0.9013 0.067 Uiso 1 1 calc R . . H21B H 0.2542 0.6739 0.8954 0.067 Uiso 1 1 calc R . . H21C H 0.4223 0.6707 0.8637 0.067 Uiso 1 1 calc R . . As1 As 0.59136(11) 0.65006(10) 0.67010(9) 0.0242(3) Uani 1 1 d . . . I1 I 0.72108(7) 0.78094(7) 0.78893(6) 0.0294(2) Uani 1 1 d . . . I2 I 0.88755(8) 0.91060(7) 0.91464(7) 0.0343(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 0.018(5) 0.029(5) 0.033(5) -0.015(4) -0.004(4) -0.005(4) C2 0.029(5) 0.037(6) 0.029(5) -0.018(5) -0.006(4) 0.001(4) C3 0.028(5) 0.037(6) 0.026(5) -0.005(5) 0.005(4) -0.010(5) C4 0.033(6) 0.049(7) 0.032(6) -0.013(5) -0.001(5) -0.005(5) C5 0.028(6) 0.056(8) 0.041(6) -0.025(6) -0.002(5) 0.001(5) C6 0.019(5) 0.036(6) 0.039(6) -0.013(5) 0.003(4) -0.001(4) C7 0.031(6) 0.033(6) 0.045(7) -0.013(5) 0.003(5) -0.002(5) C8 0.024(5) 0.028(5) 0.022(5) -0.008(4) -0.008(4) 0.003(4) C9 0.028(5) 0.028(5) 0.029(5) -0.013(4) 0.002(4) -0.002(4) C10 0.019(5) 0.035(6) 0.041(6) -0.012(5) -0.012(4) 0.005(4) C11 0.034(6) 0.028(6) 0.059(8) -0.013(6) -0.003(6) 0.000(5) C12 0.029(6) 0.039(7) 0.051(7) -0.012(6) -0.002(5) -0.013(5) C13 0.022(5) 0.041(6) 0.038(6) -0.016(5) -0.002(4) -0.006(4) C14 0.015(5) 0.040(6) 0.042(6) -0.021(5) -0.015(4) 0.010(4) C15 0.028(5) 0.026(5) 0.032(5) -0.004(4) 0.000(4) 0.001(4) C16 0.030(6) 0.030(6) 0.037(6) -0.014(5) 0.004(5) -0.004(4) C17 0.020(5) 0.044(7) 0.062(8) -0.032(6) -0.001(5) -0.001(5) C18 0.018(5) 0.040(6) 0.052(7) -0.010(5) -0.010(5) 0.000(4) C19 0.034(6) 0.047(7) 0.045(7) -0.014(6) -0.010(5) -0.003(5) C20 0.031(6) 0.035(6) 0.028(5) -0.012(5) -0.007(4) 0.002(4) C21 0.030(6) 0.069(9) 0.042(7) -0.032(6) 0.003(5) -0.002(6) As1 0.0224(5) 0.0249(5) 0.0246(5) -0.0109(4) -0.0008(4) -0.0004(4) I1 0.0278(4) 0.0288(4) 0.0301(4) -0.0126(3) -0.0013(3) 0.0005(3) I2 0.0315(4) 0.0366(4) 0.0336(4) -0.0154(3) -0.0072(3) -0.0037(3) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C6 1.358(15) . ? C1 C2 1.408(15) . ? C1 As1 1.948(10) . ? C2 C3 1.391(15) . ? C2 C7 1.506(16) . ? C3 C4 1.382(17) . ? C3 H3 0.95 . ? C4 C5 1.395(17) . ? C4 H4 0.95 . ? C5 C6 1.390(15) . ? C5 H5 0.95 . ? C6 H6 0.95 . ? C7 H7A 0.98 . ? C7 H7B 0.98 . ? C7 H7C 0.98 . ? C8 C13 1.387(14) . ? C8 C9 1.406(14) . ? C8 As1 1.953(10) . ? C9 C10 1.387(15) . ? C9 C14 1.503(14) . ? C10 C11 1.371(16) . ? C10 H10 0.95 . ? C11 C12 1.403(17) . ? C11 H11 0.95 . ? C12 C13 1.383(16) . ? C12 H12 0.95 . ? C13 H13 0.95 . ? C14 H14A 0.98 . ? C14 H14B 0.98 . ? C14 H14C 0.98 . ? C15 C20 1.383(15) . ? C15 C16 1.399(15) . ? C15 As1 1.929(11) . ? C16 C17 1.406(15) . ? C16 C21 1.501(16) . ? C17 C18 1.398(17) . ? C17 H17 0.95 . ? C18 C19 1.376(18) . ? C18 H18 0.95 . ? C19 C20 1.375(16) . ? C19 H19 0.95 . ? C20 H20 0.95 . ? C21 H21A 0.98 . ? C21 H21B 0.98 . ? C21 H21C 0.98 . ? As1 I1 2.7351(12) . ? I1 I2 2.9528(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C6 C1 C2 121.3(10) . . ? C6 C1 As1 118.3(8) . . ? C2 C1 As1 120.1(8) . . ? C3 C2 C1 117.9(10) . . ? C3 C2 C7 118.4(10) . . ? C1 C2 C7 123.7(10) . . ? C4 C3 C2 120.9(10) . . ? C4 C3 H3 119.5 . . ? C2 C3 H3 119.5 . . ? C3 C4 C5 120.2(11) . . ? C3 C4 H4 119.9 . . ? C5 C4 H4 119.9 . . ? C6 C5 C4 119.1(12) . . ? C6 C5 H5 120.5 . . ? C4 C5 H5 120.5 . . ? C1 C6 C5 120.6(11) . . ? C1 C6 H6 119.7 . . ? C5 C6 H6 119.7 . . ? C2 C7 H7A 109.5 . . ? C2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C13 C8 C9 121.7(10) . . ? C13 C8 As1 116.6(8) . . ? C9 C8 As1 121.6(7) . . ? C10 C9 C8 116.7(9) . . ? C10 C9 C14 119.7(9) . . ? C8 C9 C14 123.6(9) . . ? C11 C10 C9 122.8(10) . . ? C11 C10 H10 118.6 . . ? C9 C10 H10 118.6 . . ? C10 C11 C12 119.6(11) . . ? C10 C11 H11 120.2 . . ? C12 C11 H11 120.2 . . ? C13 C12 C11 119.4(10) . . ? C13 C12 H12 120.3 . . ? C11 C12 H12 120.3 . . ? C12 C13 C8 119.8(10) . . ? C12 C13 H13 120.1 . . ? C8 C13 H13 120.1 . . ? C9 C14 H14A 109.5 . . ? C9 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C9 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C20 C15 C16 120.9(10) . . ? C20 C15 As1 119.2(8) . . ? C16 C15 As1 119.7(8) . . ? C15 C16 C17 117.9(10) . . ? C15 C16 C21 123.7(10) . . ? C17 C16 C21 118.3(10) . . ? C18 C17 C16 120.5(11) . . ? C18 C17 H17 119.8 . . ? C16 C17 H17 119.8 . . ? C19 C18 C17 120.0(10) . . ? C19 C18 H18 120 . . ? C17 C18 H18 120 . . ? C20 C19 C18 120.3(11) . . ? C20 C19 H19 119.9 . . ? C18 C19 H19 119.9 . . ? C19 C20 C15 120.5(11) . . ? C19 C20 H20 119.7 . . ? C15 C20 H20 119.7 . . ? C16 C21 H21A 109.5 . . ? C16 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C16 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C15 As1 C1 106.8(4) . . ? C15 As1 C8 105.8(4) . . ? C1 As1 C8 104.5(4) . . ? C15 As1 I1 117.1(3) . . ? C1 As1 I1 108.7(3) . . ? C8 As1 I1 112.9(3) . . ? As1 I1 I2 174.50(4) . . ? ## end #\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2010-03-18 at 18:00:39 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.4 # Request file : c:\wingx\files\archive.reqdat # CIF files read : new dreduc sortav struct #------------------ SECTION 1. GLOBAL INFORMATION ---------------------------# data_1c _database_code_depnum_ccdc_archive 'CCDC 770653' #TrackingRef '- Combined.cif' _audit_creation_date 2010-03-18T18:00:39-00:00 _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 'C21 H21 I2 P1' _chemical_formula_sum 'C21 H21 I2 P' _chemical_formula_weight 557.98 _chemical_compound_source 'synthesis as described' _chemical_absolute_configuration unk #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' _symmetry_space_group_name_Hall 'P 2ac 2ab' _symmetry_Int_Tables_number 19 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 11.0385(6) _cell_length_b 13.8805(8) _cell_length_c 13.4773(9) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 2065.0(2) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 2493 _cell_measurement_theta_min 2 _cell_measurement_theta_max 27 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour brown _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.16 _exptl_crystal_density_diffrn 1.795 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1072 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 3.123 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; R.H. Blessing, Acta Cryst. (1995), A51, 33-38 ; _exptl_absorpt_correction_T_min 0.5739 _exptl_absorpt_correction_T_max 0.6349 #----------------------------------------------------------------------------# # 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 -0.846631E-1 _diffrn_orient_matrix_ub_12 -0.245868E-1 _diffrn_orient_matrix_ub_13 0.93401E-2 _diffrn_orient_matrix_ub_21 -0.86498E-2 _diffrn_orient_matrix_ub_22 -0.87147E-2 _diffrn_orient_matrix_ub_23 -0.712134E-1 _diffrn_orient_matrix_ub_31 0.310525E-1 _diffrn_orient_matrix_ub_32 -0.694623E-1 _diffrn_orient_matrix_ub_33 0.56284E-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 0.088 _diffrn_reflns_av_unetI/netI 0.0482 _diffrn_reflns_number 10207 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.3 _diffrn_reflns_theta_max 25.49 _diffrn_reflns_theta_full 25.49 _diffrn_measured_fraction_theta_full 0.995 _diffrn_measured_fraction_theta_max 0.995 _reflns_number_total 2188 _reflns_number_gt 1760 _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 'SHELXS-86 (Sheldrick, 1986)' _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^)+(0.0885P)^2^+15.1879P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 2188 _refine_ls_number_parameters 221 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0799 _refine_ls_R_factor_gt 0.0597 _refine_ls_wR_factor_ref 0.1708 _refine_ls_wR_factor_gt 0.1512 _refine_ls_goodness_of_fit_ref 1.129 _refine_ls_restrained_S_all 1.129 _refine_ls_shift/su_max 0.006 _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 0.37(10) _refine_diff_density_max 1.983 _refine_diff_density_min -1.201 _refine_diff_density_rms 0.204 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.474 1.812 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.102 0.094 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 0.3976(16) 0.7909(10) 0.2084(11) 0.038(4) Uani 1 1 d . . . C2 C 0.2683(18) 0.7817(12) 0.1994(12) 0.044(4) Uani 1 1 d . . . H2 H 0.2171 0.819 0.2411 0.053 Uiso 1 1 calc R . . C3 C 0.2187(18) 0.7212(13) 0.1330(12) 0.045(4) Uani 1 1 d . . . C4 C 0.2946(18) 0.6685(13) 0.0728(13) 0.051(5) Uani 1 1 d . . . H4 H 0.2593 0.6251 0.0266 0.062 Uiso 1 1 calc R . . C5 C 0.421(2) 0.6754(13) 0.0762(15) 0.060(5) Uani 1 1 d . . . H5 H 0.4708 0.6401 0.0317 0.072 Uiso 1 1 calc R . . C6 C 0.4684(17) 0.7342(12) 0.1450(13) 0.046(4) Uani 1 1 d . . . H6 H 0.5541 0.7376 0.1509 0.056 Uiso 1 1 calc R . . C7 C 0.0814(18) 0.7064(16) 0.1313(18) 0.066(6) Uani 1 1 d . . . H7A H 0.0593 0.6559 0.1787 0.1 Uiso 1 1 calc R . . H7B H 0.0561 0.6872 0.0645 0.1 Uiso 1 1 calc R . . H7C H 0.0409 0.7667 0.1496 0.1 Uiso 1 1 calc R . . C8 C 0.3730(14) 0.9642(9) 0.3295(10) 0.034(3) Uani 1 1 d . . . C9 C 0.3292(14) 1.0221(11) 0.2529(12) 0.044(4) Uani 1 1 d . . . H9 H 0.3512 1.0058 0.1868 0.053 Uiso 1 1 calc R . . C10 C 0.2549(19) 1.1026(13) 0.2672(15) 0.057(5) Uani 1 1 d . . . C11 C 0.227(2) 1.1208(14) 0.3688(18) 0.063(6) Uani 1 1 d . . . H11 H 0.1792 1.1758 0.3838 0.076 Uiso 1 1 calc R . . C12 C 0.2646(18) 1.0647(13) 0.4459(17) 0.060(5) Uani 1 1 d . . . H12 H 0.2415 1.0809 0.5117 0.072 Uiso 1 1 calc R . . C13 C 0.3362(18) 0.9841(12) 0.4292(13) 0.051(4) Uani 1 1 d . . . H13 H 0.3601 0.9434 0.4823 0.061 Uiso 1 1 calc R . . C14 C 0.214(2) 1.1599(12) 0.183(2) 0.072(7) Uani 1 1 d . . . H14A H 0.2768 1.1594 0.1312 0.108 Uiso 1 1 calc R . . H14B H 0.1994 1.2263 0.2043 0.108 Uiso 1 1 calc R . . H14C H 0.1392 1.1324 0.1562 0.108 Uiso 1 1 calc R . . C15 C 0.4919(17) 0.7909(13) 0.4086(12) 0.044(4) Uani 1 1 d . . . C16 C 0.4410(18) 0.6994(12) 0.4161(12) 0.047(4) Uani 1 1 d . . . H16 H 0.3904 0.6758 0.3645 0.056 Uiso 1 1 calc R . . C17 C 0.4640(16) 0.6420(12) 0.4997(11) 0.045(4) Uani 1 1 d . . . C18 C 0.5387(19) 0.6791(11) 0.5752(14) 0.051(5) Uani 1 1 d . . . H18 H 0.5533 0.6421 0.6333 0.061 Uiso 1 1 calc R . . C19 C 0.5903(17) 0.7682(13) 0.5651(12) 0.049(4) Uani 1 1 d . . . H19 H 0.6408 0.7926 0.6163 0.059 Uiso 1 1 calc R . . C20 C 0.5702(19) 0.8222(13) 0.4827(12) 0.049(4) Uani 1 1 d . . . H20 H 0.6103 0.8824 0.4756 0.059 Uiso 1 1 calc R . . C21 C 0.4135(19) 0.5417(10) 0.5143(11) 0.049(5) Uani 1 1 d . . . H21A H 0.4129 0.526 0.5852 0.073 Uiso 1 1 calc R . . H21B H 0.4643 0.4951 0.4789 0.073 Uiso 1 1 calc R . . H21C H 0.3307 0.5389 0.4883 0.073 Uiso 1 1 calc R . . I1 I 0.93383(11) 0.97502(8) 0.17619(8) 0.0477(3) Uani 1 1 d . . . I2 I 0.66661(9) 0.92261(7) 0.24622(8) 0.0429(3) Uani 1 1 d . . . P1 P 0.4661(4) 0.8636(3) 0.3022(3) 0.0401(10) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.056(10) 0.023(6) 0.035(7) 0.005(6) 0.001(7) -0.005(7) C2 0.063(11) 0.039(8) 0.031(8) 0.001(7) -0.004(8) 0.007(8) C3 0.058(11) 0.046(9) 0.032(8) 0.015(7) -0.005(8) 0.003(9) C4 0.065(12) 0.047(9) 0.042(9) 0.000(8) -0.010(9) -0.012(9) C5 0.075(14) 0.049(10) 0.055(11) -0.022(9) 0.012(11) -0.003(11) C6 0.045(10) 0.044(9) 0.050(10) -0.002(8) 0.010(8) 0.000(8) C7 0.046(11) 0.069(12) 0.084(14) -0.038(11) -0.010(11) 0.011(10) C8 0.050(9) 0.023(6) 0.031(7) -0.010(6) -0.007(7) 0.003(6) C9 0.052(9) 0.044(8) 0.037(7) -0.002(8) 0.018(9) -0.012(8) C10 0.061(11) 0.047(10) 0.063(12) -0.005(9) -0.009(10) -0.029(9) C11 0.052(11) 0.044(10) 0.093(15) -0.011(11) -0.027(12) 0.006(9) C12 0.050(11) 0.055(10) 0.076(13) -0.018(10) 0.008(10) -0.001(9) C13 0.059(11) 0.047(9) 0.046(9) -0.007(8) -0.002(9) -0.002(10) C14 0.076(14) 0.039(9) 0.100(16) 0.000(11) -0.051(14) -0.016(9) C15 0.050(10) 0.048(9) 0.034(8) -0.007(7) 0.002(8) -0.012(8) C16 0.052(10) 0.053(9) 0.035(8) 0.005(7) -0.004(9) 0.002(9) C17 0.054(11) 0.054(9) 0.027(7) -0.001(7) 0.018(7) -0.016(8) C18 0.079(14) 0.028(7) 0.045(9) 0.000(7) 0.000(9) 0.000(8) C19 0.052(11) 0.059(10) 0.037(8) 0.008(8) -0.005(8) 0.002(9) C20 0.056(11) 0.056(9) 0.036(8) 0.000(8) 0.006(9) 0.002(10) C21 0.083(13) 0.038(8) 0.025(7) -0.008(6) 0.008(8) -0.024(9) I1 0.0558(7) 0.0457(6) 0.0416(6) -0.0002(5) 0.0045(5) -0.0063(6) I2 0.0493(6) 0.0412(5) 0.0383(5) 0.0040(5) -0.0004(6) -0.0033(5) P1 0.047(2) 0.039(2) 0.035(2) 0.0044(17) 0.0015(18) -0.0027(19) #----------------------------------------------------------------------------# # 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 C6 1.40(2) . ? C1 C2 1.44(3) . ? C1 P1 1.785(16) . ? C2 C3 1.34(2) . ? C2 H2 0.95 . ? C3 C4 1.38(3) . ? C3 C7 1.53(3) . ? C4 C5 1.40(3) . ? C4 H4 0.95 . ? C5 C6 1.34(3) . ? C5 H5 0.95 . ? C6 H6 0.95 . ? C7 H7A 0.98 . ? C7 H7B 0.98 . ? C7 H7C 0.98 . ? C8 C9 1.39(2) . ? C8 C13 1.43(2) . ? C8 P1 1.774(14) . ? C9 C10 1.40(3) . ? C9 H9 0.95 . ? C10 C11 1.43(3) . ? C10 C14 1.46(3) . ? C11 C12 1.36(3) . ? C11 H11 0.95 . ? C12 C13 1.39(3) . ? C12 H12 0.95 . ? C13 H13 0.95 . ? C14 H14A 0.98 . ? C14 H14B 0.98 . ? C14 H14C 0.98 . ? C15 C20 1.39(2) . ? C15 C16 1.39(2) . ? C15 P1 1.777(18) . ? C16 C17 1.40(2) . ? C16 H16 0.95 . ? C17 C18 1.41(3) . ? C17 C21 1.51(2) . ? C18 C19 1.37(2) . ? C18 H18 0.95 . ? C19 C20 1.36(2) . ? C19 H19 0.95 . ? C20 H20 0.95 . ? C21 H21A 0.98 . ? C21 H21B 0.98 . ? C21 H21C 0.98 . ? I1 I2 3.1813(16) . ? I2 P1 2.478(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C6 C1 C2 117.0(16) . . ? C6 C1 P1 120.8(14) . . ? C2 C1 P1 122.0(13) . . ? C3 C2 C1 121.0(17) . . ? C3 C2 H2 119.5 . . ? C1 C2 H2 119.5 . . ? C2 C3 C4 118.5(19) . . ? C2 C3 C7 119.9(18) . . ? C4 C3 C7 121.5(17) . . ? C3 C4 C5 123.4(18) . . ? C3 C4 H4 118.3 . . ? C5 C4 H4 118.3 . . ? C6 C5 C4 117.0(19) . . ? C6 C5 H5 121.5 . . ? C4 C5 H5 121.5 . . ? C5 C6 C1 123.0(18) . . ? C5 C6 H6 118.5 . . ? C1 C6 H6 118.5 . . ? C3 C7 H7A 109.5 . . ? C3 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C3 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C9 C8 C13 119.1(14) . . ? C9 C8 P1 120.0(11) . . ? C13 C8 P1 120.8(12) . . ? C8 C9 C10 124.1(15) . . ? C8 C9 H9 117.9 . . ? C10 C9 H9 117.9 . . ? C9 C10 C11 113.6(18) . . ? C9 C10 C14 120.5(19) . . ? C11 C10 C14 126(2) . . ? C12 C11 C10 124(2) . . ? C12 C11 H11 117.8 . . ? C10 C11 H11 117.8 . . ? C11 C12 C13 121(2) . . ? C11 C12 H12 119.7 . . ? C13 C12 H12 119.7 . . ? C12 C13 C8 118.0(17) . . ? C12 C13 H13 121 . . ? C8 C13 H13 121 . . ? C10 C14 H14A 109.5 . . ? C10 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C10 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C20 C15 C16 119.0(16) . . ? C20 C15 P1 120.1(13) . . ? C16 C15 P1 120.7(13) . . ? C15 C16 C17 120.2(16) . . ? C15 C16 H16 119.9 . . ? C17 C16 H16 119.9 . . ? C16 C17 C18 118.7(15) . . ? C16 C17 C21 124.1(16) . . ? C18 C17 C21 117.3(15) . . ? C19 C18 C17 120.1(16) . . ? C19 C18 H18 120 . . ? C17 C18 H18 120 . . ? C20 C19 C18 120.9(18) . . ? C20 C19 H19 119.6 . . ? C18 C19 H19 119.6 . . ? C19 C20 C15 121.0(17) . . ? C19 C20 H20 119.5 . . ? C15 C20 H20 119.5 . . ? C17 C21 H21A 109.5 . . ? C17 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C17 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? P1 I2 I1 173.81(11) . . ? C8 P1 C15 111.9(8) . . ? C8 P1 C1 110.3(8) . . ? C15 P1 C1 108.6(7) . . ? C8 P1 I2 108.7(5) . . ? C15 P1 I2 106.9(6) . . ? C1 P1 I2 110.5(6) . . ? ## END #\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2010-03-18 at 18:28:45 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.4 # Request file : c:\wingx\files\archive.reqdat # CIF files read : p dreduc sortav struct #------------------ SECTION 1. GLOBAL INFORMATION ---------------------------# data_1d _database_code_depnum_ccdc_archive 'CCDC 770654' #TrackingRef '- Combined.cif' _audit_creation_date 2010-03-18T18:28:45-00:00 _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 'C21 H21 As1 I2' _chemical_formula_sum 'C21 H21 As I2' _chemical_formula_weight 601.93 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.6190(3) _cell_length_b 12.2125(3) _cell_length_c 18.4827(5) _cell_angle_alpha 90 _cell_angle_beta 126.5640(10) _cell_angle_gamma 90 _cell_volume 2106.48(9) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 4731 _cell_measurement_theta_min 2 _cell_measurement_theta_max 27 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.18 _exptl_crystal_density_diffrn 1.898 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1144 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 4.545 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; R.H. Blessing, Acta Cryst. (1995), A51, 33-38 ; _exptl_absorpt_correction_T_min 0.4634 _exptl_absorpt_correction_T_max 0.4951 #----------------------------------------------------------------------------# # 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 -0.228101E-1 _diffrn_orient_matrix_ub_12 -0.548242E-1 _diffrn_orient_matrix_ub_13 -0.474452E-1 _diffrn_orient_matrix_ub_21 -0.275458E-1 _diffrn_orient_matrix_ub_22 -0.506095E-1 _diffrn_orient_matrix_ub_23 0.474589E-1 _diffrn_orient_matrix_ub_31 -0.783627E-1 _diffrn_orient_matrix_ub_32 0.337485E-1 _diffrn_orient_matrix_ub_33 -0.59047E-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 0.064 _diffrn_reflns_av_unetI/netI 0.0517 _diffrn_reflns_number 15527 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.21 _diffrn_reflns_theta_max 25.29 _diffrn_reflns_theta_full 25.29 _diffrn_measured_fraction_theta_full 0.989 _diffrn_measured_fraction_theta_max 0.989 _reflns_number_total 3795 _reflns_number_gt 2550 _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_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 4.35 at 0.1421 0.2987 0.2119 [ 0.04 A from I2 ] Deepest hole -1.81 at 0.2349 0.2893 0.2391 [ 0.90 A from I2 ] ; _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^)+(0.1138P)^2^+32.3579P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 3795 _refine_ls_number_parameters 220 _refine_ls_number_restraints 126 _refine_ls_R_factor_all 0.121 _refine_ls_R_factor_gt 0.0809 _refine_ls_wR_factor_ref 0.238 _refine_ls_wR_factor_gt 0.2018 _refine_ls_goodness_of_fit_ref 1.186 _refine_ls_restrained_S_all 1.166 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0 _refine_diff_density_max 4.348 _refine_diff_density_min -1.808 _refine_diff_density_rms 0.328 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' As As 0.05 2.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.474 1.812 '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 I1 I -0.30342(10) -0.19657(7) -0.14884(6) 0.0382(3) Uani 1 1 d . . . I2 I -0.14149(10) -0.29838(6) -0.21396(5) 0.0328(3) Uani 1 1 d . . . As1 As -0.00046(15) -0.38046(10) -0.27228(9) 0.0321(4) Uani 1 1 d . . . C1 C -0.1246(15) -0.4644(10) -0.3811(9) 0.035(3) Uani 1 1 d U . . C2 C -0.2684(15) -0.4505(12) -0.4313(9) 0.040(3) Uani 1 1 d U . . H2 H -0.3085 -0.4022 -0.4115 0.048 Uiso 1 1 calc R . . C3 C -0.3588(16) -0.5083(12) -0.5136(9) 0.040(3) Uani 1 1 d U . . H3 H -0.4597 -0.4994 -0.5484 0.047 Uiso 1 1 calc R . . C4 C -0.2997(16) -0.5795(10) -0.5442(9) 0.040(3) Uani 1 1 d U . . C5 C -0.1559(16) -0.5868(10) -0.4918(10) 0.043(3) Uani 1 1 d U . . H5 H -0.114 -0.6321 -0.5121 0.052 Uiso 1 1 calc R . . C6 C -0.0645(16) -0.5329(11) -0.4104(9) 0.039(3) Uani 1 1 d U . . H6 H 0.0363 -0.5427 -0.3756 0.047 Uiso 1 1 calc R . . C7 C -0.3942(18) -0.6294(14) -0.6363(9) 0.054(4) Uani 1 1 d U . . H7A H -0.3513 -0.6979 -0.6375 0.081 Uiso 1 1 calc R . . H7B H -0.4043 -0.5784 -0.6807 0.081 Uiso 1 1 calc R . . H7C H -0.4888 -0.6446 -0.651 0.081 Uiso 1 1 calc R . . C8 C 0.1586(15) -0.4749(10) -0.1851(8) 0.033(3) Uani 1 1 d U . . C9 C 0.2729(15) -0.4880(10) -0.1899(9) 0.036(3) Uani 1 1 d U . . H9 H 0.2764 -0.4501 -0.2334 0.044 Uiso 1 1 calc R . . C10 C 0.3799(15) -0.5578(12) -0.1293(9) 0.040(3) Uani 1 1 d U . . H10 H 0.4584 -0.5684 -0.1319 0.048 Uiso 1 1 calc R . . C11 C 0.3794(14) -0.6123(9) -0.0660(9) 0.033(3) Uani 1 1 d U . . C12 C 0.2658(17) -0.5988(10) -0.0607(9) 0.040(3) Uani 1 1 d U . . H12 H 0.2642 -0.6368 -0.0165 0.049 Uiso 1 1 calc R . . C13 C 0.1545(16) -0.5288(11) -0.1213(9) 0.039(3) Uani 1 1 d U . . H13 H 0.076 -0.5183 -0.1187 0.046 Uiso 1 1 calc R . . C14 C 0.5012(17) -0.6895(11) 0.0002(10) 0.045(4) Uani 1 1 d U . . H14A H 0.5923 -0.6496 0.033 0.068 Uiso 1 1 calc R . . H14B H 0.5047 -0.7505 -0.0329 0.068 Uiso 1 1 calc R . . H14C H 0.4849 -0.718 0.0429 0.068 Uiso 1 1 calc R . . C15 C 0.0819(15) -0.2684(10) -0.3024(9) 0.033(3) Uani 1 1 d U . . C16 C 0.1942(16) -0.2043(10) -0.2359(10) 0.040(3) Uani 1 1 d U . . H16 H 0.2291 -0.2134 -0.1749 0.047 Uiso 1 1 calc R . . C17 C 0.2557(17) -0.1271(10) -0.2577(9) 0.041(3) Uani 1 1 d U . . H17 H 0.3355 -0.085 -0.2122 0.049 Uiso 1 1 calc R . . C18 C 0.1983(17) -0.1126(10) -0.3473(11) 0.046(4) Uani 1 1 d U . . C19 C 0.0839(16) -0.1734(10) -0.4147(10) 0.039(3) Uani 1 1 d U . . H19 H 0.0459 -0.1609 -0.4759 0.047 Uiso 1 1 calc R . . C20 C 0.0249(14) -0.2522(10) -0.3928(8) 0.032(3) Uani 1 1 d U . . H20 H -0.0536 -0.2952 -0.4386 0.038 Uiso 1 1 calc R . . C21 C 0.2734(19) -0.0298(13) -0.3728(12) 0.056(4) Uani 1 1 d U . . H21A H 0.2363 0.0442 -0.3783 0.084 Uiso 1 1 calc R . . H21B H 0.2535 -0.0516 -0.4303 0.084 Uiso 1 1 calc R . . H21C H 0.3771 -0.0306 -0.3256 0.084 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 I1 0.0482(6) 0.0362(5) 0.0376(5) -0.0018(3) 0.0297(5) 0.0045(4) I2 0.0410(6) 0.0289(5) 0.0312(5) -0.0002(3) 0.0228(4) 0.0005(3) As1 0.0384(8) 0.0291(7) 0.0303(7) 0.0004(5) 0.0213(6) 0.0006(5) C1 0.044(8) 0.026(6) 0.034(7) -0.009(5) 0.023(7) -0.004(6) C2 0.042(9) 0.050(8) 0.033(7) 0.004(6) 0.026(7) 0.008(7) C3 0.036(8) 0.054(8) 0.037(7) -0.003(6) 0.026(7) 0.002(6) C4 0.052(9) 0.026(6) 0.042(8) -0.004(6) 0.029(7) -0.004(6) C5 0.045(9) 0.028(7) 0.051(8) -0.015(6) 0.025(8) 0.003(6) C6 0.041(8) 0.041(7) 0.033(7) -0.008(6) 0.021(7) -0.003(6) C7 0.050(10) 0.067(10) 0.023(7) -0.017(7) 0.009(7) -0.023(8) C8 0.047(8) 0.031(6) 0.028(6) 0.000(5) 0.026(6) 0.004(6) C9 0.040(8) 0.037(7) 0.033(7) -0.002(6) 0.022(7) -0.006(6) C10 0.032(8) 0.054(8) 0.040(8) 0.003(6) 0.025(7) 0.008(6) C11 0.030(7) 0.021(6) 0.036(7) -0.010(5) 0.013(6) 0.004(5) C12 0.065(10) 0.026(6) 0.035(7) 0.002(5) 0.032(7) -0.012(6) C13 0.051(9) 0.042(7) 0.032(7) 0.005(6) 0.030(7) 0.007(6) C14 0.050(9) 0.030(7) 0.047(9) -0.002(6) 0.024(8) 0.006(6) C15 0.048(8) 0.022(6) 0.046(7) 0.000(5) 0.037(7) 0.006(6) C16 0.040(8) 0.032(7) 0.042(8) 0.010(6) 0.022(7) 0.006(6) C17 0.051(9) 0.021(6) 0.037(7) 0.004(5) 0.019(7) 0.000(6) C18 0.055(10) 0.014(6) 0.069(10) -0.004(6) 0.037(9) 0.000(6) C19 0.053(9) 0.028(6) 0.043(8) 0.001(6) 0.032(7) 0.011(6) C20 0.039(8) 0.028(6) 0.027(6) 0.005(5) 0.019(6) 0.001(5) C21 0.071(12) 0.045(9) 0.082(12) -0.005(8) 0.062(11) -0.010(8) #----------------------------------------------------------------------------# # 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 I1 I2 3.0385(12) . ? I2 As1 2.6375(15) . ? As1 C1 1.928(12) . ? As1 C15 1.931(13) . ? As1 C8 1.948(13) . ? C1 C2 1.35(2) . ? C1 C6 1.390(19) . ? C2 C3 1.418(19) . ? C2 H2 0.95 . ? C3 C4 1.419(19) . ? C3 H3 0.95 . ? C4 C5 1.34(2) . ? C4 C7 1.499(18) . ? C5 C6 1.386(19) . ? C5 H5 0.95 . ? C6 H6 0.95 . ? C7 H7A 0.98 . ? C7 H7B 0.98 . ? C7 H7C 0.98 . ? C8 C13 1.375(17) . ? C8 C9 1.392(19) . ? C9 C10 1.366(19) . ? C9 H9 0.95 . ? C10 C11 1.350(19) . ? C10 H10 0.95 . ? C11 C12 1.39(2) . ? C11 C14 1.525(18) . ? C12 C13 1.39(2) . ? C12 H12 0.95 . ? C13 H13 0.95 . ? C14 H14A 0.98 . ? C14 H14B 0.98 . ? C14 H14C 0.98 . ? C15 C16 1.384(19) . ? C15 C20 1.398(17) . ? C16 C17 1.381(19) . ? C16 H16 0.95 . ? C17 C18 1.38(2) . ? C17 H17 0.95 . ? C18 C19 1.38(2) . ? C18 C21 1.58(2) . ? C19 C20 1.375(19) . ? C19 H19 0.95 . ? C20 H20 0.95 . ? C21 H21A 0.98 . ? C21 H21B 0.98 . ? C21 H21C 0.98 . ? 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 As1 I2 I1 178.15(4) . . ? C1 As1 C15 105.5(6) . . ? C1 As1 C8 107.5(5) . . ? C15 As1 C8 105.6(6) . . ? C1 As1 I2 111.5(4) . . ? C15 As1 I2 112.5(3) . . ? C8 As1 I2 113.7(4) . . ? C2 C1 C6 120.6(12) . . ? C2 C1 As1 120.0(10) . . ? C6 C1 As1 119.3(11) . . ? C1 C2 C3 119.7(12) . . ? C1 C2 H2 120.1 . . ? C3 C2 H2 120.1 . . ? C4 C3 C2 120.5(13) . . ? C4 C3 H3 119.7 . . ? C2 C3 H3 119.7 . . ? C5 C4 C3 116.2(13) . . ? C5 C4 C7 123.1(14) . . ? C3 C4 C7 120.1(14) . . ? C4 C5 C6 124.8(13) . . ? C4 C5 H5 117.6 . . ? C6 C5 H5 117.6 . . ? C5 C6 C1 118.1(13) . . ? C5 C6 H6 120.9 . . ? C1 C6 H6 120.9 . . ? C4 C7 H7A 109.5 . . ? C4 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C4 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C13 C8 C9 121.4(12) . . ? C13 C8 As1 119.5(10) . . ? C9 C8 As1 119.1(9) . . ? C10 C9 C8 117.2(12) . . ? C10 C9 H9 121.4 . . ? C8 C9 H9 121.4 . . ? C11 C10 C9 123.1(13) . . ? C11 C10 H10 118.5 . . ? C9 C10 H10 118.5 . . ? C10 C11 C12 119.8(12) . . ? C10 C11 C14 121.2(13) . . ? C12 C11 C14 118.9(13) . . ? C11 C12 C13 118.9(12) . . ? C11 C12 H12 120.6 . . ? C13 C12 H12 120.6 . . ? C8 C13 C12 119.6(13) . . ? C8 C13 H13 120.2 . . ? C12 C13 H13 120.2 . . ? C11 C14 H14A 109.5 . . ? C11 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C11 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C16 C15 C20 120.4(12) . . ? C16 C15 As1 120.8(10) . . ? C20 C15 As1 118.8(10) . . ? C15 C16 C17 120.3(13) . . ? C15 C16 H16 119.8 . . ? C17 C16 H16 119.8 . . ? C18 C17 C16 118.3(14) . . ? C18 C17 H17 120.8 . . ? C16 C17 H17 120.8 . . ? C19 C18 C17 122.2(14) . . ? C19 C18 C21 118.9(14) . . ? C17 C18 C21 118.8(14) . . ? C18 C19 C20 119.6(13) . . ? C18 C19 H19 120.2 . . ? C20 C19 H19 120.2 . . ? C19 C20 C15 119.1(13) . . ? C19 C20 H20 120.4 . . ? C15 C20 H20 120.4 . . ? C18 C21 H21A 109.5 . . ? C18 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C18 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? 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 I1 I2 As1 C1 -106.3(16) . . . . ? I1 I2 As1 C15 12.0(16) . . . . ? I1 I2 As1 C8 132.0(15) . . . . ? C15 As1 C1 C2 -103.9(12) . . . . ? C8 As1 C1 C2 143.7(11) . . . . ? I2 As1 C1 C2 18.6(12) . . . . ? C15 As1 C1 C6 71.6(12) . . . . ? C8 As1 C1 C6 -40.8(12) . . . . ? I2 As1 C1 C6 -166.0(10) . . . . ? C6 C1 C2 C3 1(2) . . . . ? As1 C1 C2 C3 176.9(10) . . . . ? C1 C2 C3 C4 -1(2) . . . . ? C2 C3 C4 C5 -1(2) . . . . ? C2 C3 C4 C7 -172.4(13) . . . . ? C3 C4 C5 C6 2(2) . . . . ? C7 C4 C5 C6 173.4(14) . . . . ? C4 C5 C6 C1 -2(2) . . . . ? C2 C1 C6 C5 0(2) . . . . ? As1 C1 C6 C5 -175.8(10) . . . . ? C1 As1 C8 C13 -97.3(11) . . . . ? C15 As1 C8 C13 150.5(10) . . . . ? I2 As1 C8 C13 26.6(12) . . . . ? C1 As1 C8 C9 81.5(11) . . . . ? C15 As1 C8 C9 -30.8(11) . . . . ? I2 As1 C8 C9 -154.6(9) . . . . ? C13 C8 C9 C10 0.8(19) . . . . ? As1 C8 C9 C10 -177.9(10) . . . . ? C8 C9 C10 C11 -1(2) . . . . ? C9 C10 C11 C12 0(2) . . . . ? C9 C10 C11 C14 179.9(12) . . . . ? C10 C11 C12 C13 -0.1(19) . . . . ? C14 C11 C12 C13 -179.7(12) . . . . ? C9 C8 C13 C12 -1(2) . . . . ? As1 C8 C13 C12 178.1(10) . . . . ? C11 C12 C13 C8 0.2(19) . . . . ? C1 As1 C15 C16 -169.4(10) . . . . ? C8 As1 C15 C16 -55.8(11) . . . . ? I2 As1 C15 C16 68.7(11) . . . . ? C1 As1 C15 C20 11.3(11) . . . . ? C8 As1 C15 C20 125.0(10) . . . . ? I2 As1 C15 C20 -110.5(9) . . . . ? C20 C15 C16 C17 -3(2) . . . . ? As1 C15 C16 C17 177.6(10) . . . . ? C15 C16 C17 C18 3(2) . . . . ? C16 C17 C18 C19 -1(2) . . . . ? C16 C17 C18 C21 -176.3(13) . . . . ? C17 C18 C19 C20 -1(2) . . . . ? C21 C18 C19 C20 174.6(12) . . . . ? C18 C19 C20 C15 0.5(19) . . . . ? C16 C15 C20 C19 1.4(19) . . . . ? As1 C15 C20 C19 -179.3(9) . . . . ? # END of CIF #\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2010-03-18 at 17:11:19 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.4 # Request file : c:\wingx\files\archive.reqdat # CIF files read : p dreduc sortav struct #------------------ SECTION 1. GLOBAL INFORMATION ---------------------------# data_1e _database_code_depnum_ccdc_archive 'CCDC 770655' #TrackingRef '- Combined.cif' _audit_creation_date 2010-03-18T17:11:19-00:00 _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 'C21 H21 I2 P1' _chemical_formula_sum 'C21 H21 I2 P' _chemical_formula_weight 558.15 _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 11.4271(4) _cell_length_b 12.1665(5) _cell_length_c 18.3475(7) _cell_angle_alpha 90 _cell_angle_beta 126.422(2) _cell_angle_gamma 90 _cell_volume 2052.55(14) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4913 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 27.485 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.07 _exptl_crystal_density_diffrn 1.806 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1072 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 3.142 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; R.H. Blessing, Acta Cryst. (1995), A51, 33-38 ; _exptl_absorpt_correction_T_min 0.839 _exptl_absorpt_correction_T_max 1.000 #----------------------------------------------------------------------------# # 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_detector_area_resol_mean 9 _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 0.408298E-1 _diffrn_orient_matrix_ub_12 0.580207E-1 _diffrn_orient_matrix_ub_13 -0.349512E-1 _diffrn_orient_matrix_ub_21 0.294048E-1 _diffrn_orient_matrix_ub_22 0.342238E-1 _diffrn_orient_matrix_ub_23 0.580132E-1 _diffrn_orient_matrix_ub_31 0.716694E-1 _diffrn_orient_matrix_ub_32 -0.470957E-1 _diffrn_orient_matrix_ub_33 -0.9016E-3 _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 0.087 _diffrn_reflns_av_unetI/netI 0.0598 _diffrn_reflns_number 18225 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.23 _diffrn_reflns_theta_max 25.3 _diffrn_reflns_theta_full 25.3 _diffrn_measured_fraction_theta_full 0.985 _diffrn_measured_fraction_theta_max 0.985 _reflns_number_total 3683 _reflns_number_gt 2260 _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. ; _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^+67.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 3683 _refine_ls_number_parameters 220 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1287 _refine_ls_R_factor_gt 0.074 _refine_ls_wR_factor_ref 0.1832 _refine_ls_wR_factor_gt 0.146 _refine_ls_goodness_of_fit_ref 1.193 _refine_ls_restrained_S_all 1.193 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 3.972 _refine_diff_density_min -1.741 _refine_diff_density_rms 0.299 #----------------------------------------------------------------------------# # 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' I I -0.4742 1.8119 '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 I1 I 0.19828(10) 0.80110(8) 0.85102(6) 0.0334(3) Uani 1 1 d . . . I2 I 0.37040(9) 0.69470(7) 0.78186(6) 0.0302(3) Uani 1 1 d . . . P1 P 0.5023(4) 0.6153(3) 0.7257(2) 0.0300(8) Uani 1 1 d . . . C1 C 0.3835(14) 0.5342(13) 0.6253(9) 0.034(3) Uani 1 1 d . . . C2 C 0.4451(17) 0.4628(12) 0.5978(10) 0.039(3) Uani 1 1 d . . . H2 H 0.5451 0.4514 0.6337 0.046 Uiso 1 1 calc R . . C3 C 0.3524(16) 0.4076(12) 0.5139(10) 0.039(3) Uani 1 1 d . . . H3 H 0.393 0.3598 0.495 0.047 Uiso 1 1 calc R . . C4 C 0.2046(16) 0.4227(12) 0.4597(9) 0.037(3) Uani 1 1 d . . . C5 C 0.1453(15) 0.4978(13) 0.4893(9) 0.036(3) Uani 1 1 d . . . H5 H 0.0456 0.5104 0.4529 0.044 Uiso 1 1 calc R . . C6 C 0.2331(17) 0.5523(14) 0.5710(10) 0.045(4) Uani 1 1 d . . . H6 H 0.1927 0.6005 0.5898 0.053 Uiso 1 1 calc R . . C7 C 0.1067(17) 0.3706(14) 0.3678(10) 0.048(4) Uani 1 1 d . . . H7A H 0.152 0.3055 0.3657 0.073 Uiso 1 1 calc R . . H7B H 0.0898 0.4215 0.3225 0.073 Uiso 1 1 calc R . . H7C H 0.0157 0.3516 0.3565 0.073 Uiso 1 1 calc R . . C8 C 0.5757(16) 0.7232(10) 0.6977(10) 0.029(3) Uani 1 1 d . . . C9 C 0.6908(16) 0.7892(12) 0.7662(10) 0.038(3) Uani 1 1 d . . . H9 H 0.7239 0.7806 0.826 0.045 Uiso 1 1 calc R . . C10 C 0.7548(16) 0.8668(12) 0.7448(10) 0.039(3) Uani 1 1 d . . . H10 H 0.8346 0.9071 0.7903 0.046 Uiso 1 1 calc R . . C11 C 0.6988(16) 0.8835(11) 0.6554(10) 0.032(3) Uani 1 1 d . . . C12 C 0.5845(14) 0.8234(12) 0.5884(10) 0.036(3) Uani 1 1 d . . . H12 H 0.5477 0.8363 0.5283 0.043 Uiso 1 1 calc R . . C13 C 0.5227(16) 0.7432(12) 0.6088(10) 0.034(3) Uani 1 1 d . . . H13 H 0.4447 0.7022 0.5624 0.041 Uiso 1 1 calc R . . C14 C 0.7776(19) 0.9663(14) 0.6347(12) 0.051(4) Uani 1 1 d . . . H14A H 0.7642 0.9455 0.5797 0.076 Uiso 1 1 calc R . . H14B H 0.8796 0.9665 0.6837 0.076 Uiso 1 1 calc R . . H14C H 0.7383 1.0384 0.6279 0.076 Uiso 1 1 calc R . . C15 C 0.6531(16) 0.5288(11) 0.8117(9) 0.034(3) Uani 1 1 d . . . C16 C 0.6467(15) 0.4764(11) 0.8753(10) 0.036(3) Uani 1 1 d . . . H16 H 0.569 0.4884 0.8779 0.043 Uiso 1 1 calc R . . C17 C 0.7569(14) 0.4059(12) 0.9350(8) 0.032(3) Uani 1 1 d . . . H17 H 0.7509 0.3691 0.9771 0.038 Uiso 1 1 calc R . . C18 C 0.8783(15) 0.3868(11) 0.9352(9) 0.033(3) Uani 1 1 d . . . C19 C 0.8809(17) 0.4423(13) 0.8696(10) 0.042(4) Uani 1 1 d . . . H19 H 0.9601 0.4326 0.868 0.051 Uiso 1 1 calc R . . C20 C 0.7697(14) 0.5108(12) 0.8072(9) 0.031(3) Uani 1 1 d . . . H20 H 0.7719 0.5447 0.7627 0.037 Uiso 1 1 calc R . . C21 C 0.9979(15) 0.3101(12) 0.9999(9) 0.036(3) Uani 1 1 d . . . H21A H 0.9965 0.2982 1.0511 0.055 Uiso 1 1 calc R . . H21B H 1.0897 0.3414 1.02 0.055 Uiso 1 1 calc R . . H21C H 0.9846 0.2413 0.9703 0.055 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 I1 0.0372(5) 0.0343(5) 0.0332(5) -0.0008(4) 0.0234(4) 0.0020(4) I2 0.0328(5) 0.0305(5) 0.0306(5) -0.0001(4) 0.0207(4) 0.0013(4) P1 0.0310(18) 0.0286(19) 0.0332(19) 0.0006(15) 0.0206(16) 0.0006(15) C1 0.024(7) 0.048(9) 0.024(7) 0.007(6) 0.012(6) -0.003(6) C2 0.042(8) 0.038(8) 0.044(9) -0.004(7) 0.030(8) 0.003(7) C3 0.036(8) 0.029(8) 0.042(8) -0.006(6) 0.018(7) 0.003(7) C4 0.039(8) 0.038(9) 0.026(7) 0.005(6) 0.015(6) -0.001(7) C5 0.030(7) 0.059(10) 0.018(6) -0.003(6) 0.013(6) 0.008(7) C6 0.046(9) 0.050(10) 0.043(9) -0.001(7) 0.030(8) 0.005(8) C7 0.045(9) 0.047(10) 0.033(8) -0.026(7) 0.012(7) -0.018(8) C8 0.049(8) 0.009(6) 0.045(8) -0.002(5) 0.036(7) 0.008(6) C9 0.047(9) 0.035(8) 0.041(8) -0.001(7) 0.031(7) 0.000(7) C10 0.034(8) 0.031(8) 0.046(9) -0.008(7) 0.021(7) -0.015(6) C11 0.043(8) 0.024(7) 0.041(8) 0.003(6) 0.032(7) -0.009(6) C12 0.026(7) 0.037(8) 0.035(8) -0.012(6) 0.013(6) -0.006(6) C13 0.039(8) 0.028(7) 0.038(8) 0.006(6) 0.024(7) 0.006(6) C14 0.066(11) 0.044(10) 0.068(11) -0.012(8) 0.053(10) -0.017(9) C15 0.040(8) 0.026(7) 0.034(7) -0.004(6) 0.022(7) 0.001(6) C16 0.035(8) 0.025(7) 0.050(9) 0.001(7) 0.027(7) -0.003(6) C17 0.028(7) 0.037(8) 0.015(6) 0.005(6) 0.004(5) 0.006(6) C18 0.030(7) 0.026(7) 0.038(8) -0.008(6) 0.019(7) -0.005(6) C19 0.046(9) 0.050(10) 0.035(8) -0.004(7) 0.027(7) 0.001(8) C20 0.026(7) 0.037(8) 0.030(7) -0.013(6) 0.016(6) -0.015(6) C21 0.030(7) 0.031(8) 0.027(7) 0.005(6) 0.005(6) 0.007(6) #----------------------------------------------------------------------------# # 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 I1 I2 3.1808(12) . ? I2 P1 2.472(4) . ? P1 C8 1.790(13) . ? P1 C1 1.800(15) . ? P1 C15 1.827(15) . ? C1 C2 1.39(2) . ? C1 C6 1.40(2) . ? C2 C3 1.42(2) . ? C2 H2 0.93 . ? C3 C4 1.37(2) . ? C3 H3 0.93 . ? C4 C5 1.42(2) . ? C4 C7 1.503(18) . ? C5 C6 1.38(2) . ? C5 H5 0.93 . ? C6 H6 0.93 . ? C7 H7A 0.96 . ? C7 H7B 0.96 . ? C7 H7C 0.96 . ? C8 C13 1.384(19) . ? C8 C9 1.41(2) . ? C9 C10 1.39(2) . ? C9 H9 0.93 . ? C10 C11 1.38(2) . ? C10 H10 0.93 . ? C11 C12 1.358(19) . ? C11 C14 1.541(18) . ? C12 C13 1.38(2) . ? C12 H12 0.93 . ? C13 H13 0.93 . ? C14 H14A 0.96 . ? C14 H14B 0.96 . ? C14 H14C 0.96 . ? C15 C16 1.37(2) . ? C15 C20 1.400(19) . ? C16 C17 1.373(19) . ? C16 H16 0.93 . ? C17 C18 1.404(19) . ? C17 H17 0.93 . ? C18 C19 1.40(2) . ? C18 C21 1.490(18) . ? C19 C20 1.38(2) . ? C19 H19 0.93 . ? C20 H20 0.93 . ? C21 H21A 0.96 . ? C21 H21B 0.96 . ? C21 H21C 0.96 . ? 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 I2 I1 178.77(9) . . ? C8 P1 C1 107.8(6) . . ? C8 P1 C15 107.9(7) . . ? C1 P1 C15 108.7(7) . . ? C8 P1 I2 109.8(4) . . ? C1 P1 I2 111.4(5) . . ? C15 P1 I2 111.2(5) . . ? C2 C1 C6 120.9(14) . . ? C2 C1 P1 118.6(11) . . ? C6 C1 P1 120.2(12) . . ? C1 C2 C3 118.6(14) . . ? C1 C2 H2 120.7 . . ? C3 C2 H2 120.7 . . ? C4 C3 C2 121.9(14) . . ? C4 C3 H3 119 . . ? C2 C3 H3 119 . . ? C3 C4 C5 118.0(13) . . ? C3 C4 C7 122.2(14) . . ? C5 C4 C7 119.6(13) . . ? C6 C5 C4 121.3(13) . . ? C6 C5 H5 119.4 . . ? C4 C5 H5 119.4 . . ? C5 C6 C1 119.3(14) . . ? C5 C6 H6 120.3 . . ? C1 C6 H6 120.3 . . ? C4 C7 H7A 109.5 . . ? C4 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C4 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C13 C8 C9 118.3(13) . . ? C13 C8 P1 121.0(11) . . ? C9 C8 P1 120.6(11) . . ? C10 C9 C8 120.3(13) . . ? C10 C9 H9 119.8 . . ? C8 C9 H9 119.8 . . ? C11 C10 C9 119.2(13) . . ? C11 C10 H10 120.4 . . ? C9 C10 H10 120.4 . . ? C12 C11 C10 121.0(12) . . ? C12 C11 C14 121.2(13) . . ? C10 C11 C14 117.6(13) . . ? C11 C12 C13 120.5(14) . . ? C11 C12 H12 119.8 . . ? C13 C12 H12 119.8 . . ? C12 C13 C8 120.5(14) . . ? C12 C13 H13 119.8 . . ? C8 C13 H13 119.8 . . ? C11 C14 H14A 109.5 . . ? C11 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C11 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C16 C15 C20 120.7(13) . . ? C16 C15 P1 120.3(11) . . ? C20 C15 P1 118.8(11) . . ? C15 C16 C17 119.0(13) . . ? C15 C16 H16 120.5 . . ? C17 C16 H16 120.5 . . ? C16 C17 C18 122.8(13) . . ? C16 C17 H17 118.6 . . ? C18 C17 H17 118.6 . . ? C19 C18 C17 116.4(13) . . ? C19 C18 C21 120.7(13) . . ? C17 C18 C21 122.9(13) . . ? C20 C19 C18 121.9(14) . . ? C20 C19 H19 119.1 . . ? C18 C19 H19 119.1 . . ? C19 C20 C15 119.2(13) . . ? C19 C20 H20 120.4 . . ? C15 C20 H20 120.4 . . ? C18 C21 H21A 109.5 . . ? C18 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C18 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? 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 I1 I2 P1 C8 37(5) . . . . ? I1 I2 P1 C1 -82(4) . . . . ? I1 I2 P1 C15 156(4) . . . . ? C8 P1 C1 C2 75.0(13) . . . . ? C15 P1 C1 C2 -41.7(13) . . . . ? I2 P1 C1 C2 -164.5(10) . . . . ? C8 P1 C1 C6 -97.9(12) . . . . ? C15 P1 C1 C6 145.3(12) . . . . ? I2 P1 C1 C6 22.5(13) . . . . ? C6 C1 C2 C3 -1(2) . . . . ? P1 C1 C2 C3 -173.5(11) . . . . ? C1 C2 C3 C4 0(2) . . . . ? C2 C3 C4 C5 1(2) . . . . ? C2 C3 C4 C7 175.6(15) . . . . ? C3 C4 C5 C6 -1(2) . . . . ? C7 C4 C5 C6 -176.1(15) . . . . ? C4 C5 C6 C1 1(2) . . . . ? C2 C1 C6 C5 0(2) . . . . ? P1 C1 C6 C5 173.0(12) . . . . ? C1 P1 C8 C13 9.7(13) . . . . ? C15 P1 C8 C13 126.9(11) . . . . ? I2 P1 C8 C13 -111.8(10) . . . . ? C1 P1 C8 C9 -169.5(11) . . . . ? C15 P1 C8 C9 -52.3(12) . . . . ? I2 P1 C8 C9 69.0(11) . . . . ? C13 C8 C9 C10 -4(2) . . . . ? P1 C8 C9 C10 174.9(11) . . . . ? C8 C9 C10 C11 4(2) . . . . ? C9 C10 C11 C12 -2(2) . . . . ? C9 C10 C11 C14 -177.0(14) . . . . ? C10 C11 C12 C13 -1(2) . . . . ? C14 C11 C12 C13 174.7(14) . . . . ? C11 C12 C13 C8 0(2) . . . . ? C9 C8 C13 C12 2(2) . . . . ? P1 C8 C13 C12 -177.1(11) . . . . ? C8 P1 C15 C16 148.8(12) . . . . ? C1 P1 C15 C16 -94.6(12) . . . . ? I2 P1 C15 C16 28.3(13) . . . . ? C8 P1 C15 C20 -35.9(12) . . . . ? C1 P1 C15 C20 80.7(12) . . . . ? I2 P1 C15 C20 -156.4(9) . . . . ? C20 C15 C16 C17 0(2) . . . . ? P1 C15 C16 C17 175.4(11) . . . . ? C15 C16 C17 C18 1(2) . . . . ? C16 C17 C18 C19 -1(2) . . . . ? C16 C17 C18 C21 -179.9(13) . . . . ? C17 C18 C19 C20 -1(2) . . . . ? C21 C18 C19 C20 177.9(13) . . . . ? C18 C19 C20 C15 2(2) . . . . ? C16 C15 C20 C19 -2(2) . . . . ? P1 C15 C20 C19 -177.4(11) . . . . ? ## END #\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2009-09-06 at 16:30:48 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.3 # Request file : c:\wingx\files\archive.dat # CIF files read : robin dreduc sortav struct data_2 _database_code_depnum_ccdc_archive 'CCDC 770656' #TrackingRef '- Combined.cif' _audit_creation_date 2009-09-06T16:30:48-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C21 H21 As1 Au1 Cl1' _chemical_formula_sum 'C21 H21 As Au Cl' _chemical_formula_weight 580.71 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P b c a' _symmetry_space_group_name_Hall '-P 2ac 2ab' _symmetry_Int_Tables_number 61 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 13.8475(2) _cell_length_b 19.8474(2) _cell_length_c 27.5000(4) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 7558.01(17) _cell_formula_units_Z 16 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9186 _cell_measurement_theta_min 2 _cell_measurement_theta_max 26 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 2.041 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4416 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 9.664 # 9.362 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; R.H. Blessing, Acta Cryst. (1995), A51, 33-38 ; _exptl_absorpt_correction_T_min 0.3341 _exptl_absorpt_correction_T_max 0.4545 #----------------------------------------------------------------------------# # 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 -0.675527E-1 _diffrn_orient_matrix_ub_12 0.125308E-1 _diffrn_orient_matrix_ub_13 0.91349E-2 _diffrn_orient_matrix_ub_21 -0.55445E-2 _diffrn_orient_matrix_ub_22 0.277486E-1 _diffrn_orient_matrix_ub_23 -0.302233E-1 _diffrn_orient_matrix_ub_31 -0.249184E-1 _diffrn_orient_matrix_ub_32 -0.401446E-1 _diffrn_orient_matrix_ub_33 -0.180394E-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 0.084 _diffrn_reflns_av_unetI/netI 0.0481 _diffrn_reflns_number 70987 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 3.03 _diffrn_reflns_theta_max 25.5 _diffrn_reflns_theta_full 25.5 _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.996 _reflns_number_total 7010 _reflns_number_gt 4991 _reflns_threshold_expression >2sigma(I) _diffrn_reflns_reduction_process ; Scaled and merged with SORTAV R.H. Blessing, (1987) Cryst. Rev. 1, 3-58 R.H. Blessing, (1989) J. Appl. Cryst. 22, 396-397 ; #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SIR92 (Giacovazzo et al, 1993)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0809P)^2^+168.5377P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 7010 _refine_ls_number_parameters 439 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1032 _refine_ls_R_factor_gt 0.0674 _refine_ls_wR_factor_ref 0.1894 _refine_ls_wR_factor_gt 0.1647 _refine_ls_goodness_of_fit_ref 1.206 _refine_ls_restrained_S_all 1.206 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 4.05 _refine_diff_density_min -2.581 _refine_diff_density_rms 0.371 #----------------------------------------------------------------------------# # 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 0.0031 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' As As 0.0512 2.0129 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Au Au -1.9162 8.821 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.1315(9) 0.2757(7) 0.1879(5) 0.024(3) Uani 1 1 d . . . C2 C 0.0693(10) 0.3299(7) 0.1760(5) 0.025(3) Uani 1 1 d . . . C3 C -0.0213(10) 0.3156(8) 0.1590(6) 0.032(4) Uani 1 1 d . . . H3 H -0.0629 0.352 0.1509 0.038 Uiso 1 1 calc R . . C4 C -0.0552(11) 0.2502(8) 0.1529(5) 0.032(3) Uani 1 1 d . . . H4 H -0.1182 0.242 0.1406 0.039 Uiso 1 1 calc R . . C5 C 0.0069(11) 0.1959(8) 0.1657(5) 0.033(4) Uani 1 1 d . . . H5 H -0.0144 0.1506 0.1628 0.039 Uiso 1 1 calc R . . C6 C 0.0983(9) 0.2101(7) 0.1823(5) 0.024(3) Uani 1 1 d . . . H6 H 0.1402 0.1738 0.1902 0.029 Uiso 1 1 calc R . . C7 C 0.1004(10) 0.4026(7) 0.1812(6) 0.033(4) Uani 1 1 d . . . H7A H 0.0497 0.4321 0.1684 0.049 Uiso 1 1 calc R . . H7B H 0.1603 0.4099 0.1629 0.049 Uiso 1 1 calc R . . H7C H 0.1114 0.4129 0.2156 0.049 Uiso 1 1 calc R . . C8 C 0.3383(10) 0.3085(7) 0.1542(5) 0.025(3) Uani 1 1 d . . . C9 C 0.4371(10) 0.3240(7) 0.1588(5) 0.024(3) Uani 1 1 d . . . C10 C 0.4897(10) 0.3330(6) 0.1167(5) 0.025(3) Uani 1 1 d . . . H10 H 0.5567 0.3429 0.1185 0.03 Uiso 1 1 calc R . . C11 C 0.4451(11) 0.3274(8) 0.0716(6) 0.037(4) Uani 1 1 d . . . H11 H 0.4822 0.334 0.043 0.044 Uiso 1 1 calc R . . C12 C 0.3491(12) 0.3128(8) 0.0676(5) 0.035(4) Uani 1 1 d . . . H12 H 0.3197 0.3089 0.0365 0.041 Uiso 1 1 calc R . . C13 C 0.2953(9) 0.3039(7) 0.1094(5) 0.025(3) Uani 1 1 d . . . H13 H 0.2282 0.2944 0.107 0.03 Uiso 1 1 calc R . . C14 C 0.4857(10) 0.3309(8) 0.2076(6) 0.034(4) Uani 1 1 d . . . H14A H 0.4792 0.2886 0.2257 0.051 Uiso 1 1 calc R . . H14B H 0.4551 0.3674 0.226 0.051 Uiso 1 1 calc R . . H14C H 0.5543 0.3411 0.2029 0.051 Uiso 1 1 calc R . . C15 C 0.3055(9) 0.2029(7) 0.2348(5) 0.022(3) Uani 1 1 d . . . C16 C 0.2681(10) 0.1733(6) 0.2769(5) 0.023(3) Uani 1 1 d . . . C17 C 0.3039(9) 0.1120(7) 0.2907(6) 0.028(3) Uani 1 1 d . . . H17 H 0.2802 0.0917 0.3196 0.033 Uiso 1 1 calc R . . C18 C 0.3724(11) 0.0795(9) 0.2644(5) 0.035(4) Uani 1 1 d . . . H18 H 0.3961 0.0371 0.2752 0.042 Uiso 1 1 calc R . . C19 C 0.4081(10) 0.1076(8) 0.2220(5) 0.029(3) Uani 1 1 d . . . H19 H 0.4552 0.0845 0.2032 0.035 Uiso 1 1 calc R . . C20 C 0.3739(10) 0.1700(7) 0.2072(5) 0.027(3) Uani 1 1 d . . . H20 H 0.3976 0.1901 0.1782 0.032 Uiso 1 1 calc R . . C21 C 0.1883(12) 0.2057(8) 0.3065(6) 0.038(4) Uani 1 1 d . . . H21A H 0.129 0.2076 0.287 0.058 Uiso 1 1 calc R . . H21B H 0.2075 0.2514 0.3157 0.058 Uiso 1 1 calc R . . H21C H 0.1766 0.1789 0.3359 0.058 Uiso 1 1 calc R . . C22 C 0.1764(11) 0.0247(7) 0.1042(5) 0.026(3) Uani 1 1 d . . . C23 C 0.0789(10) 0.0056(7) 0.1064(5) 0.025(3) Uani 1 1 d . . . C24 C 0.0366(11) -0.0048(8) 0.1518(6) 0.034(4) Uani 1 1 d . . . H24 H -0.0298 -0.0166 0.1541 0.041 Uiso 1 1 calc R . . C25 C 0.0919(11) 0.0023(7) 0.1935(5) 0.029(3) Uani 1 1 d . . . H25 H 0.0628 -0.0057 0.2242 0.035 Uiso 1 1 calc R . . C26 C 0.1876(11) 0.0205(8) 0.1917(6) 0.032(3) Uani 1 1 d . . . H26 H 0.2242 0.0262 0.2206 0.038 Uiso 1 1 calc R . . C27 C 0.2292(11) 0.0301(7) 0.1464(5) 0.028(3) Uani 1 1 d . . . H27 H 0.2959 0.0408 0.1445 0.033 Uiso 1 1 calc R . . C28 C 0.0180(10) -0.0018(8) 0.0617(5) 0.029(3) Uani 1 1 d . . . H28A H -0.0454 -0.02 0.0706 0.043 Uiso 1 1 calc R . . H28B H 0.0497 -0.0327 0.0389 0.043 Uiso 1 1 calc R . . H28C H 0.0097 0.0423 0.0462 0.043 Uiso 1 1 calc R . . C29 C 0.3720(9) 0.0582(7) 0.0620(5) 0.022(3) Uani 1 1 d . . . C30 C 0.4367(8) 0.0035(7) 0.0661(5) 0.019(3) Uani 1 1 d . . . C31 C 0.5295(11) 0.0182(8) 0.0845(5) 0.030(3) Uani 1 1 d . . . H31 H 0.5732 -0.0177 0.0903 0.036 Uiso 1 1 calc R . . C32 C 0.5587(11) 0.0839(8) 0.0945(5) 0.031(3) Uani 1 1 d . . . H32 H 0.6228 0.0924 0.1051 0.037 Uiso 1 1 calc R . . C33 C 0.4946(10) 0.1368(8) 0.0888(5) 0.030(3) Uani 1 1 d . . . H33 H 0.5145 0.1816 0.0957 0.036 Uiso 1 1 calc R . . C34 C 0.3993(11) 0.1239(8) 0.0728(5) 0.032(4) Uani 1 1 d . . . H34 H 0.3544 0.1598 0.0694 0.038 Uiso 1 1 calc R . . C35 C 0.4109(11) -0.0677(8) 0.0544(6) 0.032(4) Uani 1 1 d . . . H35A H 0.415 -0.0747 0.0192 0.049 Uiso 1 1 calc R . . H35B H 0.3449 -0.077 0.0654 0.049 Uiso 1 1 calc R . . H35C H 0.4559 -0.0983 0.0709 0.049 Uiso 1 1 calc R . . C36 C 0.1936(11) 0.1309(7) 0.0237(5) 0.027(3) Uani 1 1 d . . . C37 C 0.2287(11) 0.1628(8) -0.0169(5) 0.029(3) Uani 1 1 d . . . C38 C 0.1939(11) 0.2271(7) -0.0290(5) 0.029(3) Uani 1 1 d . . . H38 H 0.2168 0.2496 -0.0572 0.034 Uiso 1 1 calc R . . C39 C 0.1243(11) 0.2577(8) 0.0013(6) 0.031(3) Uani 1 1 d . . . H39 H 0.1008 0.3012 -0.0067 0.038 Uiso 1 1 calc R . . C40 C 0.0905(10) 0.2266(8) 0.0414(5) 0.033(4) Uani 1 1 d . . . H40 H 0.0441 0.2481 0.0615 0.039 Uiso 1 1 calc R . . C41 C 0.1238(10) 0.1634(8) 0.0528(5) 0.031(3) Uani 1 1 d . . . H41 H 0.0994 0.1411 0.0808 0.037 Uiso 1 1 calc R . . C42 C 0.3029(12) 0.1319(8) -0.0495(6) 0.037(4) Uani 1 1 d . . . H42A H 0.3624 0.124 -0.031 0.056 Uiso 1 1 calc R . . H42B H 0.3164 0.1625 -0.0766 0.056 Uiso 1 1 calc R . . H42C H 0.2786 0.089 -0.0622 0.056 Uiso 1 1 calc R . . As1 As 0.26066(9) 0.29117(7) 0.21229(5) 0.0204(3) Uani 1 1 d . . . As2 As 0.23918(10) 0.04231(7) 0.04246(5) 0.0214(3) Uani 1 1 d . . . Au1 Au 0.26762(4) 0.37342(3) 0.273374(19) 0.02530(19) Uani 1 1 d . . . Au2 Au 0.21410(4) -0.04060(3) -0.017096(19) 0.02472(19) Uani 1 1 d . . . Cl1 Cl 0.2675(3) 0.4512(2) 0.33460(14) 0.0427(10) Uani 1 1 d . . . Cl2 Cl 0.1817(3) -0.12240(18) -0.07373(12) 0.0298(8) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.012(7) 0.030(8) 0.031(8) -0.006(6) 0.005(6) 0.005(5) C2 0.029(8) 0.033(8) 0.014(7) 0.015(6) 0.003(6) -0.006(6) C3 0.010(7) 0.050(10) 0.036(9) 0.012(7) -0.002(6) 0.010(6) C4 0.029(8) 0.048(10) 0.019(7) 0.004(7) -0.002(6) -0.011(7) C5 0.033(9) 0.034(9) 0.030(9) 0.000(7) 0.005(7) -0.005(7) C6 0.017(7) 0.032(8) 0.023(7) -0.009(6) -0.005(6) -0.005(6) C7 0.019(8) 0.038(9) 0.042(10) 0.005(7) 0.003(7) -0.002(6) C8 0.026(8) 0.021(7) 0.028(8) 0.007(6) 0.011(6) -0.004(6) C9 0.020(7) 0.019(7) 0.032(8) 0.005(6) 0.003(6) -0.005(5) C10 0.022(7) 0.021(7) 0.031(8) 0.001(6) -0.001(6) -0.003(5) C11 0.030(9) 0.040(9) 0.040(10) 0.005(7) 0.011(7) 0.005(7) C12 0.043(10) 0.050(10) 0.010(7) -0.005(6) -0.005(7) 0.009(7) C13 0.009(6) 0.047(9) 0.018(7) -0.008(6) 0.002(5) -0.004(6) C14 0.015(7) 0.047(10) 0.041(9) 0.007(7) -0.004(7) 0.003(6) C15 0.015(7) 0.031(7) 0.021(7) -0.008(6) -0.008(6) 0.001(6) C16 0.027(8) 0.010(6) 0.034(8) -0.002(6) 0.001(6) 0.005(5) C17 0.012(7) 0.022(7) 0.048(10) 0.010(6) -0.002(7) -0.007(5) C18 0.021(8) 0.063(11) 0.020(8) 0.009(7) -0.006(6) -0.001(7) C19 0.011(7) 0.048(9) 0.028(8) -0.008(7) -0.003(6) 0.002(6) C20 0.022(8) 0.047(9) 0.011(7) 0.003(6) -0.009(6) -0.005(6) C21 0.039(9) 0.041(9) 0.034(9) 0.000(7) 0.003(7) -0.013(8) C22 0.032(8) 0.030(8) 0.016(7) 0.005(6) 0.001(6) 0.005(6) C23 0.021(7) 0.027(8) 0.026(8) -0.002(6) -0.002(6) 0.003(6) C24 0.031(8) 0.034(9) 0.036(9) -0.007(7) 0.009(7) -0.003(7) C25 0.030(8) 0.034(8) 0.022(8) -0.018(6) -0.001(6) 0.008(6) C26 0.021(8) 0.046(9) 0.028(9) -0.007(7) 0.000(7) 0.002(6) C27 0.030(8) 0.028(8) 0.025(8) 0.000(6) -0.018(7) 0.008(6) C28 0.029(8) 0.041(9) 0.017(7) 0.005(6) -0.006(6) -0.015(7) C29 0.008(6) 0.034(8) 0.024(7) -0.010(6) 0.003(6) 0.000(5) C30 0.002(6) 0.035(8) 0.019(7) -0.007(6) 0.003(5) -0.002(5) C31 0.036(9) 0.040(9) 0.014(7) 0.005(6) 0.007(6) 0.005(7) C32 0.026(8) 0.044(9) 0.022(8) -0.009(7) -0.005(6) -0.005(7) C33 0.030(8) 0.039(9) 0.020(8) -0.002(6) 0.014(7) -0.003(6) C34 0.027(8) 0.047(9) 0.021(8) -0.011(7) -0.001(6) 0.007(7) C35 0.023(8) 0.042(9) 0.033(9) -0.001(7) -0.008(7) 0.002(6) C36 0.026(8) 0.029(8) 0.027(8) -0.003(6) -0.003(6) -0.002(6) C37 0.027(8) 0.042(9) 0.019(7) -0.001(6) -0.003(6) 0.009(7) C38 0.031(8) 0.034(8) 0.020(7) 0.015(6) -0.006(6) -0.019(6) C39 0.035(9) 0.031(8) 0.028(8) 0.001(6) -0.008(7) 0.004(7) C40 0.015(7) 0.059(11) 0.024(8) -0.004(7) -0.001(6) 0.005(7) C41 0.022(8) 0.045(9) 0.026(8) 0.000(7) -0.001(6) 0.001(7) C42 0.045(10) 0.045(10) 0.023(8) 0.006(7) 0.000(7) -0.005(8) As1 0.0173(7) 0.0291(7) 0.0149(7) 0.0013(6) 0.0014(5) -0.0001(6) As2 0.0197(7) 0.0282(7) 0.0165(7) -0.0020(6) -0.0004(6) 0.0019(5) Au1 0.0276(3) 0.0310(3) 0.0174(3) -0.0008(2) -0.0036(2) 0.0017(2) Au2 0.0219(3) 0.0336(3) 0.0186(3) -0.0035(2) -0.0019(2) 0.0025(2) Cl1 0.068(3) 0.035(2) 0.0254(19) -0.0092(16) -0.0175(19) 0.0110(19) Cl2 0.0291(19) 0.038(2) 0.0220(18) -0.0080(15) -0.0053(15) 0.0026(15) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C6 1.389(19) . ? C1 C2 1.416(19) . ? C1 As1 1.935(13) . ? C2 C3 1.37(2) . ? C2 C7 1.51(2) . ? C3 C4 1.39(2) . ? C3 H3 0.95 . ? C4 C5 1.42(2) . ? C4 H4 0.95 . ? C5 C6 1.37(2) . ? C5 H5 0.95 . ? C6 H6 0.95 . ? C7 H7A 0.98 . ? C7 H7B 0.98 . ? C7 H7C 0.98 . ? C8 C13 1.37(2) . ? C8 C9 1.408(19) . ? C8 As1 1.955(13) . ? C9 C10 1.378(19) . ? C9 C14 1.51(2) . ? C10 C11 1.39(2) . ? C10 H10 0.95 . ? C11 C12 1.37(2) . ? C11 H11 0.95 . ? C12 C13 1.38(2) . ? C12 H12 0.95 . ? C13 H13 0.95 . ? C14 H14A 0.98 . ? C14 H14B 0.98 . ? C14 H14C 0.98 . ? C15 C20 1.38(2) . ? C15 C16 1.40(2) . ? C15 As1 1.959(14) . ? C16 C17 1.368(19) . ? C16 C21 1.52(2) . ? C17 C18 1.36(2) . ? C17 H17 0.95 . ? C18 C19 1.38(2) . ? C18 H18 0.95 . ? C19 C20 1.39(2) . ? C19 H19 0.95 . ? C20 H20 0.95 . ? C21 H21A 0.98 . ? C21 H21B 0.98 . ? C21 H21C 0.98 . ? C22 C27 1.37(2) . ? C22 C23 1.40(2) . ? C22 As2 1.940(14) . ? C23 C24 1.39(2) . ? C23 C28 1.498(19) . ? C24 C25 1.39(2) . ? C24 H24 0.95 . ? C25 C26 1.37(2) . ? C25 H25 0.95 . ? C26 C27 1.38(2) . ? C26 H26 0.95 . ? C27 H27 0.95 . ? C28 H28A 0.98 . ? C28 H28B 0.98 . ? C28 H28C 0.98 . ? C29 C34 1.39(2) . ? C29 C30 1.412(18) . ? C29 As2 1.942(13) . ? C30 C31 1.41(2) . ? C30 C35 1.49(2) . ? C31 C32 1.39(2) . ? C31 H31 0.95 . ? C32 C33 1.38(2) . ? C32 H32 0.95 . ? C33 C34 1.42(2) . ? C33 H33 0.95 . ? C34 H34 0.95 . ? C35 H35A 0.98 . ? C35 H35B 0.98 . ? C35 H35C 0.98 . ? C36 C37 1.37(2) . ? C36 C41 1.41(2) . ? C36 As2 1.938(15) . ? C37 C38 1.40(2) . ? C37 C42 1.50(2) . ? C38 C39 1.41(2) . ? C38 H38 0.95 . ? C39 C40 1.35(2) . ? C39 H39 0.95 . ? C40 C41 1.37(2) . ? C40 H40 0.95 . ? C41 H41 0.95 . ? C42 H42A 0.98 . ? C42 H42B 0.98 . ? C42 H42C 0.98 . ? As1 Au1 2.3444(15) . ? As2 Au2 2.3476(15) . ? Au1 Cl1 2.284(4) . ? Au2 Cl2 2.294(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C6 C1 C2 119.1(12) . . ? C6 C1 As1 119.6(10) . . ? C2 C1 As1 121.4(10) . . ? C3 C2 C1 118.6(13) . . ? C3 C2 C7 119.4(13) . . ? C1 C2 C7 122.1(13) . . ? C2 C3 C4 122.9(14) . . ? C2 C3 H3 118.6 . . ? C4 C3 H3 118.6 . . ? C3 C4 C5 118.3(13) . . ? C3 C4 H4 120.8 . . ? C5 C4 H4 120.8 . . ? C6 C5 C4 118.9(14) . . ? C6 C5 H5 120.5 . . ? C4 C5 H5 120.5 . . ? C5 C6 C1 122.2(14) . . ? C5 C6 H6 118.9 . . ? C1 C6 H6 118.9 . . ? C2 C7 H7A 109.5 . . ? C2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C13 C8 C9 121.0(12) . . ? C13 C8 As1 118.9(10) . . ? C9 C8 As1 120.0(11) . . ? C10 C9 C8 117.9(13) . . ? C10 C9 C14 120.0(12) . . ? C8 C9 C14 122.1(13) . . ? C9 C10 C11 120.2(13) . . ? C9 C10 H10 119.9 . . ? C11 C10 H10 119.9 . . ? C12 C11 C10 121.5(14) . . ? C12 C11 H11 119.3 . . ? C10 C11 H11 119.3 . . ? C11 C12 C13 119.0(14) . . ? C11 C12 H12 120.5 . . ? C13 C12 H12 120.5 . . ? C8 C13 C12 120.4(13) . . ? C8 C13 H13 119.8 . . ? C12 C13 H13 119.8 . . ? C9 C14 H14A 109.5 . . ? C9 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C9 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C20 C15 C16 120.8(13) . . ? C20 C15 As1 117.8(10) . . ? C16 C15 As1 121.4(10) . . ? C17 C16 C15 118.1(13) . . ? C17 C16 C21 119.4(13) . . ? C15 C16 C21 122.5(12) . . ? C18 C17 C16 121.9(15) . . ? C18 C17 H17 119.1 . . ? C16 C17 H17 119.1 . . ? C17 C18 C19 120.5(15) . . ? C17 C18 H18 119.8 . . ? C19 C18 H18 119.8 . . ? C18 C19 C20 119.0(14) . . ? C18 C19 H19 120.5 . . ? C20 C19 H19 120.5 . . ? C15 C20 C19 119.7(13) . . ? C15 C20 H20 120.1 . . ? C19 C20 H20 120.1 . . ? C16 C21 H21A 109.5 . . ? C16 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C16 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C27 C22 C23 119.8(13) . . ? C27 C22 As2 119.1(11) . . ? C23 C22 As2 121.0(10) . . ? C24 C23 C22 118.7(13) . . ? C24 C23 C28 119.0(13) . . ? C22 C23 C28 122.3(13) . . ? C25 C24 C23 119.6(14) . . ? C25 C24 H24 120.2 . . ? C23 C24 H24 120.2 . . ? C26 C25 C24 122.0(14) . . ? C26 C25 H25 119 . . ? C24 C25 H25 119 . . ? C25 C26 C27 118.0(14) . . ? C25 C26 H26 121 . . ? C27 C26 H26 121 . . ? C22 C27 C26 121.8(14) . . ? C22 C27 H27 119.1 . . ? C26 C27 H27 119.1 . . ? C23 C28 H28A 109.5 . . ? C23 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C23 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C34 C29 C30 122.1(12) . . ? C34 C29 As2 118.0(10) . . ? C30 C29 As2 119.9(9) . . ? C31 C30 C29 116.6(12) . . ? C31 C30 C35 119.4(12) . . ? C29 C30 C35 123.9(11) . . ? C32 C31 C30 122.0(14) . . ? C32 C31 H31 119 . . ? C30 C31 H31 119 . . ? C33 C32 C31 120.1(14) . . ? C33 C32 H32 119.9 . . ? C31 C32 H32 119.9 . . ? C32 C33 C34 119.7(14) . . ? C32 C33 H33 120.1 . . ? C34 C33 H33 120.1 . . ? C29 C34 C33 119.4(14) . . ? C29 C34 H34 120.3 . . ? C33 C34 H34 120.3 . . ? C30 C35 H35A 109.5 . . ? C30 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C30 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C37 C36 C41 119.5(14) . . ? C37 C36 As2 121.4(11) . . ? C41 C36 As2 119.1(11) . . ? C36 C37 C38 119.5(14) . . ? C36 C37 C42 122.8(14) . . ? C38 C37 C42 117.7(13) . . ? C37 C38 C39 118.9(13) . . ? C37 C38 H38 120.5 . . ? C39 C38 H38 120.5 . . ? C40 C39 C38 121.5(14) . . ? C40 C39 H39 119.2 . . ? C38 C39 H39 119.2 . . ? C39 C40 C41 119.3(14) . . ? C39 C40 H40 120.4 . . ? C41 C40 H40 120.4 . . ? C40 C41 C36 121.2(14) . . ? C40 C41 H41 119.4 . . ? C36 C41 H41 119.4 . . ? C37 C42 H42A 109.5 . . ? C37 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C37 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C1 As1 C8 104.7(6) . . ? C1 As1 C15 105.1(6) . . ? C8 As1 C15 104.0(6) . . ? C1 As1 Au1 113.4(4) . . ? C8 As1 Au1 116.1(4) . . ? C15 As1 Au1 112.5(4) . . ? C36 As2 C22 104.5(6) . . ? C36 As2 C29 103.6(6) . . ? C22 As2 C29 102.1(6) . . ? C36 As2 Au2 113.7(4) . . ? C22 As2 Au2 114.7(4) . . ? C29 As2 Au2 116.6(4) . . ? Cl1 Au1 As1 177.08(13) . . ? Cl2 Au2 As2 177.04(10) . . ? ## End