Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _audit_creation_date 'Thu Apr 7 19:54:58 2005' _audit_creation_method 'by teXsan' _audit_update_record ? _publ_contact_author_name 'Shigekazu Ito' _publ_contact_author_address ; Department of Chemistry Tohoku University Aoba Sendai 980-8578 JAPAN ; _publ_contact_author_email S-ITO@JD6.SO-NET.NE.JP _publ_section_title ; Structural and coordination properties of 1,2-bis(cyclopropyl)-3,4-bis(2,4,6-tri-t-butylphenyl)-3,4-diphosphiniden ecyclobutene prepared by dehydrogenative homocoupling of 3-cyclopropyl-1-(2,4,6-tri-t-butylphenyl)-1-phosphaallene ; _publ_section_synopsis ; #------------------------------------------------------------------------------ Molecular Structure Corporation, Rigaku Corporation. (1999). teXsan. Single Crystal Structure Analysis Software. Version 1.10. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. Rigaku, 3-9-12 Akishima, Tokyo, Japan. ; loop_ _publ_author_name 'Shigekazu Ito' 'Matthias Freytag' 'Masaaki Yoshifuji' #------------------------------------------------------------------------------ data_No.4 _database_code_depnum_ccdc_archive 'CCDC 272085' #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C24 H38 Br O P ' _chemical_formula_moiety 'C24 H38 Br O P ' _chemical_formula_weight 453.44 _chemical_melting_point 76-78 #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z _cell_length_a 9.9117(5) _cell_length_b 13.2871(5) _cell_length_c 9.7067(5) _cell_angle_alpha 105.593(2) _cell_angle_beta 96.440(4) _cell_angle_gamma 90.888(3) _cell_volume 1222.1(1) _cell_formula_units_Z 2 _cell_measurement_reflns_used 3922 _cell_measurement_theta_min 3.2 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 133 #------------------------------------------------------------------------------ _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.300 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.200 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.232 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 1.763 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(Higashi, 1995)' _exptl_absorpt_correction_T_min 0.619 _exptl_absorpt_correction_T_max 0.703 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku RAXIS-IV Imaging Plate' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 0.010000 _diffrn_reflns_number 9728 _diffrn_reflns_av_R_equivalents 0.024 _diffrn_reflns_theta_max 27.48 _diffrn_measured_fraction_theta_max 0.9130 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.9130 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > 2.0 sigma(F^2^). The weighted R-factor (wR), goodness of fit (S) and R-factor (gt) are based on F, with F set to zero for negative F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 5101 _reflns_number_gt 4388 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0508 _refine_ls_wR_factor_ref 0.0775 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 4388 _refine_ls_number_parameters 244 _refine_ls_goodness_of_fit_ref 1.311 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00250|Fo|^2^]' _refine_ls_shift/su_max 0.0038 _refine_diff_density_max 0.96 _refine_diff_density_min -1.15 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? 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 for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H H 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; P P 0.102 0.094 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; O O 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Br Br -0.290 2.459 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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 Br Br 0.13834(4) 0.14027(3) 1.29983(4) 0.0355(1) Uani 1.00 d . . . P P 0.08279(8) 0.35634(6) 1.22719(8) 0.0224(2) Uani 1.00 d . . . O O -0.0873(3) 0.2734(2) 1.5018(3) 0.0438(8) Uani 1.00 d . . . C(1) C 0.0816(3) 0.2801(3) 1.3388(3) 0.0245(7) Uani 1.00 d . . . C(2) C 0.0348(4) 0.3228(3) 1.4880(3) 0.0299(8) Uani 1.00 d . . . C(3) C 0.1391(4) 0.3138(3) 1.6063(4) 0.0274(8) Uani 1.00 d . . . C(4) C 0.2582(5) 0.3907(3) 1.6502(4) 0.044(1) Uani 1.00 d . . . C(5) C 0.1511(4) 0.3947(3) 1.7479(4) 0.0374(10) Uani 1.00 d . . . C(6) C -0.2057(4) 0.3102(4) 1.4403(5) 0.053(1) Uani 1.00 d . . . C(7) C 0.1554(3) 0.2772(2) 1.0689(3) 0.0196(7) Uani 1.00 d . . . C(8) C 0.0710(3) 0.2089(2) 0.9519(3) 0.0204(7) Uani 1.00 d . . . C(9) C 0.1340(3) 0.1389(2) 0.8460(3) 0.0227(7) Uani 1.00 d . . . C(10) C 0.2745(3) 0.1354(2) 0.8479(3) 0.0209(7) Uani 1.00 d . . . C(11) C 0.3529(3) 0.2095(3) 0.9574(3) 0.0240(7) Uani 1.00 d . . . C(12) C 0.2995(3) 0.2817(2) 1.0662(3) 0.0225(7) Uani 1.00 d . . . C(13) C -0.0864(3) 0.2104(3) 0.9290(3) 0.0235(7) Uani 1.00 d . . . C(14) C -0.1503(4) 0.1516(3) 1.0235(4) 0.0326(9) Uani 1.00 d . . . C(15) C -0.1356(4) 0.3224(3) 0.9575(4) 0.0359(9) Uani 1.00 d . . . C(16) C -0.1428(3) 0.1555(3) 0.7709(4) 0.0308(9) Uani 1.00 d . . . C(17) C 0.3440(3) 0.0588(3) 0.7311(3) 0.0256(8) Uani 1.00 d . . . C(18) C 0.2397(4) -0.0136(3) 0.6174(4) 0.0372(9) Uani 1.00 d . . . C(19) C 0.4277(4) 0.1219(3) 0.6568(4) 0.0363(9) Uani 1.00 d . . . C(20) C 0.4377(4) -0.0089(3) 0.8005(4) 0.040(1) Uani 1.00 d . . . C(21) C 0.3998(3) 0.3656(3) 1.1732(4) 0.0307(8) Uani 1.00 d . . . C(22) C 0.5403(4) 0.3663(3) 1.1182(4) 0.041(1) Uani 1.00 d . . . C(23) C 0.4269(4) 0.3434(4) 1.3214(4) 0.041(1) Uani 1.00 d . . . C(24) C 0.3472(4) 0.4760(3) 1.1878(5) 0.044(1) Uani 1.00 d . . . H(1) H -0.0443 0.3851 1.4926 0.0535 Uiso 1.00 calc . . . H(2) H 0.1583 0.2427 1.6114 0.0535 Uiso 1.00 calc . . . H(3) H 0.2674 0.4515 1.5925 0.0535 Uiso 1.00 calc . . . H(4) H 0.3670 0.3663 1.7010 0.0535 Uiso 1.00 calc . . . H(5) H 0.0896 0.4596 1.7648 0.0535 Uiso 1.00 calc . . . H(6) H 0.1700 0.3699 1.8478 0.0535 Uiso 1.00 calc . . . H(7) H -0.2063 0.3083 1.3340 0.0535 Uiso 1.00 calc . . . H(8) H -0.2990 0.2744 1.4624 0.0535 Uiso 1.00 calc . . . H(9) H -0.2041 0.3802 1.4672 0.0535 Uiso 1.00 calc . . . H(10) H 0.0714 0.0758 0.7624 0.0535 Uiso 1.00 calc . . . H(11) H 0.4538 0.2159 0.9373 0.0535 Uiso 1.00 calc . . . H(12) H -0.1259 0.0781 0.9941 0.0535 Uiso 1.00 calc . . . H(13) H -0.2577 0.1527 1.0005 0.0535 Uiso 1.00 calc . . . H(14) H -0.1337 0.1817 1.1346 0.0535 Uiso 1.00 calc . . . H(15) H -0.2353 0.3256 0.9084 0.0535 Uiso 1.00 calc . . . H(16) H -0.1316 0.3622 1.0731 0.0535 Uiso 1.00 calc . . . H(17) H -0.0796 0.3715 0.8982 0.0535 Uiso 1.00 calc . . . H(18) H -0.1006 0.1923 0.6954 0.0535 Uiso 1.00 calc . . . H(19) H -0.1324 0.0757 0.7547 0.0535 Uiso 1.00 calc . . . H(20) H -0.2494 0.1543 0.7671 0.0535 Uiso 1.00 calc . . . H(21) H 0.2833 -0.0569 0.5377 0.0535 Uiso 1.00 calc . . . H(22) H 0.1695 0.0297 0.5579 0.0535 Uiso 1.00 calc . . . H(23) H 0.1828 -0.0600 0.6652 0.0535 Uiso 1.00 calc . . . H(24) H 0.4782 0.0808 0.5651 0.0535 Uiso 1.00 calc . . . H(25) H 0.3707 0.1634 0.6011 0.0535 Uiso 1.00 calc . . . H(26) H 0.5003 0.1770 0.7286 0.0535 Uiso 1.00 calc . . . H(27) H 0.4818 -0.0558 0.7285 0.0535 Uiso 1.00 calc . . . H(28) H 0.4954 0.0335 0.8750 0.0535 Uiso 1.00 calc . . . H(29) H 0.3979 -0.0478 0.8668 0.0535 Uiso 1.00 calc . . . H(30) H 0.5300 0.3786 1.0292 0.0535 Uiso 1.00 calc . . . H(31) H 0.5933 0.2958 1.1054 0.0535 Uiso 1.00 calc . . . H(32) H 0.6112 0.4268 1.1921 0.0535 Uiso 1.00 calc . . . H(33) H 0.4682 0.2671 1.3076 0.0535 Uiso 1.00 calc . . . H(34) H 0.5144 0.4000 1.3683 0.0535 Uiso 1.00 calc . . . H(35) H 0.3426 0.3483 1.3844 0.0535 Uiso 1.00 calc . . . H(36) H 0.4110 0.5264 1.2383 0.0535 Uiso 1.00 calc . . . H(37) H 0.2565 0.4828 1.2357 0.0535 Uiso 1.00 calc . . . H(38) H 0.3340 0.4817 1.0688 0.0535 Uiso 1.00 calc . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Br 0.0499(3) 0.0233(2) 0.0321(2) 0.0053(1) -0.0007(2) 0.0075(1) P 0.0246(4) 0.0209(4) 0.0202(4) 0.0043(3) 0.0034(3) 0.0024(3) O 0.036(1) 0.049(2) 0.049(2) 0.002(1) 0.005(1) 0.017(1) C(1) 0.023(2) 0.025(2) 0.023(1) 0.004(1) 0.001(1) 0.004(1) C(2) 0.030(2) 0.040(2) 0.021(1) 0.004(1) 0.003(1) 0.009(1) C(3) 0.032(2) 0.022(1) 0.024(1) 0.001(1) -0.004(1) 0.002(1) C(4) 0.054(3) 0.036(2) 0.034(2) -0.015(2) 0.002(2) -0.003(2) C(5) 0.049(2) 0.038(2) 0.024(2) 0.007(2) 0.004(2) 0.007(2) C(6) 0.031(2) 0.078(3) 0.052(2) 0.014(2) 0.007(2) 0.022(2) C(7) 0.021(1) 0.016(1) 0.020(1) 0.004(1) 0.001(1) 0.003(1) C(8) 0.019(1) 0.019(1) 0.021(1) 0.000(1) -0.001(1) 0.004(1) C(9) 0.022(1) 0.024(1) 0.020(1) 0.000(1) 0.002(1) 0.003(1) C(10) 0.021(1) 0.021(1) 0.019(1) 0.001(1) 0.000(1) 0.002(1) C(11) 0.018(1) 0.026(2) 0.023(1) 0.002(1) 0.001(1) -0.001(1) C(12) 0.019(1) 0.022(1) 0.021(1) -0.003(1) 0.000(1) -0.001(1) C(13) 0.017(1) 0.026(2) 0.024(1) -0.001(1) 0.001(1) 0.003(1) C(14) 0.025(2) 0.041(2) 0.030(2) -0.006(1) 0.005(1) 0.007(2) C(15) 0.023(2) 0.034(2) 0.047(2) 0.007(1) -0.001(1) 0.006(2) C(16) 0.021(2) 0.042(2) 0.025(2) 0.000(1) -0.002(1) 0.005(1) C(17) 0.025(2) 0.027(2) 0.019(1) 0.003(1) 0.003(1) -0.002(1) C(18) 0.035(2) 0.032(2) 0.032(2) -0.001(2) 0.003(1) -0.012(1) C(19) 0.031(2) 0.040(2) 0.032(2) 0.002(2) 0.011(1) -0.003(2) C(20) 0.046(2) 0.038(2) 0.031(2) 0.015(2) 0.000(2) 0.000(2) C(21) 0.024(2) 0.031(2) 0.028(2) -0.004(1) -0.003(1) -0.006(1) C(22) 0.030(2) 0.045(2) 0.037(2) -0.011(2) 0.004(2) -0.006(2) C(23) 0.028(2) 0.057(3) 0.030(2) -0.003(2) -0.006(1) 0.000(2) C(24) 0.034(2) 0.024(2) 0.062(3) -0.007(1) 0.005(2) -0.005(2) #------------------------------------------------------------------------------ _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction 'teXsan Ver. 1.10' _computing_structure_solution SIR92 _computing_structure_refinement 'teXsan Ver. 1.10' _computing_publication_material 'teXsan Ver. 1.10' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Br C(1) 1.901(3) . . yes P C(1) 1.671(3) . . yes P C(7) 1.841(3) . . yes O C(2) 1.404(4) . . yes O C(6) 1.411(5) . . yes C(1) C(2) 1.533(4) . . yes C(2) C(3) 1.488(5) . . yes C(3) C(4) 1.495(5) . . yes C(3) C(5) 1.492(5) . . yes C(4) C(5) 1.493(6) . . yes C(7) C(8) 1.422(4) . . yes C(7) C(12) 1.431(4) . . yes C(8) C(9) 1.401(4) . . yes C(8) C(13) 1.552(4) . . yes C(9) C(10) 1.391(4) . . yes C(10) C(11) 1.390(4) . . yes C(10) C(17) 1.541(4) . . yes C(11) C(12) 1.383(4) . . yes C(12) C(21) 1.556(4) . . yes C(13) C(14) 1.535(5) . . yes C(13) C(15) 1.536(5) . . yes C(13) C(16) 1.547(4) . . yes C(17) C(18) 1.535(5) . . yes C(17) C(19) 1.533(5) . . yes C(17) C(20) 1.528(5) . . yes C(21) C(22) 1.547(5) . . yes C(21) C(23) 1.541(5) . . yes C(21) C(24) 1.539(5) . . yes #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C(1) P C(7) 105.0(1) . 1_555 1_555 yes C(2) O C(6) 114.8(3) . 1_555 1_555 yes Br C(1) P 125.5(2) . 1_555 1_555 yes Br C(1) C(2) 114.6(2) . 1_555 1_555 yes P C(1) C(2) 120.0(2) . 1_555 1_555 yes O C(2) C(1) 112.6(3) . 1_555 1_555 yes O C(2) C(3) 108.5(3) . 1_555 1_555 yes C(1) C(2) C(3) 112.3(3) . 1_555 1_555 yes C(2) C(3) C(4) 118.8(3) . 1_555 1_555 yes C(2) C(3) C(5) 119.5(3) . 1_555 1_555 yes C(4) C(3) C(5) 60.0(3) . 1_555 1_555 yes C(3) C(4) C(5) 59.9(3) . 1_555 1_555 yes C(3) C(5) C(4) 60.1(2) . 1_555 1_555 yes P C(7) C(8) 120.9(2) . 1_555 1_555 yes P C(7) C(12) 119.4(2) . 1_555 1_555 yes C(8) C(7) C(12) 119.7(3) . 1_555 1_555 yes C(7) C(8) C(9) 117.9(3) . 1_555 1_555 yes C(7) C(8) C(13) 124.6(3) . 1_555 1_555 yes C(9) C(8) C(13) 117.4(3) . 1_555 1_555 yes C(8) C(9) C(10) 123.1(3) . 1_555 1_555 yes C(9) C(10) C(11) 116.9(3) . 1_555 1_555 yes C(9) C(10) C(17) 123.2(3) . 1_555 1_555 yes C(11) C(10) C(17) 119.7(3) . 1_555 1_555 yes C(10) C(11) C(12) 123.8(3) . 1_555 1_555 yes C(7) C(12) C(11) 117.9(3) . 1_555 1_555 yes C(7) C(12) C(21) 124.5(3) . 1_555 1_555 yes C(11) C(12) C(21) 117.5(3) . 1_555 1_555 yes C(8) C(13) C(14) 110.7(3) . 1_555 1_555 yes C(8) C(13) C(15) 111.9(3) . 1_555 1_555 yes C(8) C(13) C(16) 111.1(2) . 1_555 1_555 yes C(14) C(13) C(15) 110.6(3) . 1_555 1_555 yes C(14) C(13) C(16) 106.9(3) . 1_555 1_555 yes C(15) C(13) C(16) 105.4(3) . 1_555 1_555 yes C(10) C(17) C(18) 111.6(3) . 1_555 1_555 yes C(10) C(17) C(19) 108.8(3) . 1_555 1_555 yes C(10) C(17) C(20) 109.6(3) . 1_555 1_555 yes C(18) C(17) C(19) 108.9(3) . 1_555 1_555 yes C(18) C(17) C(20) 108.3(3) . 1_555 1_555 yes C(19) C(17) C(20) 109.5(3) . 1_555 1_555 yes C(12) C(21) C(22) 111.2(3) . 1_555 1_555 yes C(12) C(21) C(23) 111.8(3) . 1_555 1_555 yes C(12) C(21) C(24) 110.6(3) . 1_555 1_555 yes C(22) C(21) C(23) 105.7(3) . 1_555 1_555 yes C(22) C(21) C(24) 106.2(3) . 1_555 1_555 yes C(23) C(21) C(24) 111.1(3) . 1_555 1_555 yes #------------------------------------------------------------------------------ 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 Br C(1) P C(7) -2.2(2) 1_555 1_555 1_555 1_555 yes Br C(1) C(2) O -68.4(3) 1_555 1_555 1_555 1_555 yes Br C(1) C(2) C(3) 54.5(3) 1_555 1_555 1_555 1_555 yes P C(1) C(2) O 112.9(3) 1_555 1_555 1_555 1_555 yes P C(1) C(2) C(3) -124.2(3) 1_555 1_555 1_555 1_555 yes P C(7) C(8) C(9) -170.0(2) 1_555 1_555 1_555 1_555 yes P C(7) C(8) C(13) 13.3(4) 1_555 1_555 1_555 1_555 yes P C(7) C(12) C(11) 169.8(2) 1_555 1_555 1_555 1_555 yes P C(7) C(12) C(21) -13.1(4) 1_555 1_555 1_555 1_555 yes O C(2) C(3) C(4) -157.4(3) 1_555 1_555 1_555 1_555 yes O C(2) C(3) C(5) -87.6(4) 1_555 1_555 1_555 1_555 yes C(1) P C(7) C(8) 88.3(3) 1_555 1_555 1_555 1_555 yes C(1) P C(7) C(12) -89.4(3) 1_555 1_555 1_555 1_555 yes C(1) C(2) O C(6) -80.0(4) 1_555 1_555 1_555 1_555 yes C(1) C(2) C(3) C(4) 77.4(4) 1_555 1_555 1_555 1_555 yes C(1) C(2) C(3) C(5) 147.2(3) 1_555 1_555 1_555 1_555 yes C(2) C(1) P C(7) 176.5(2) 1_555 1_555 1_555 1_555 yes C(2) C(3) C(4) C(5) 109.3(4) 1_555 1_555 1_555 1_555 yes C(2) C(3) C(5) C(4) -108.2(4) 1_555 1_555 1_555 1_555 yes C(3) C(2) O C(6) 155.0(3) 1_555 1_555 1_555 1_555 yes C(7) C(8) C(9) C(10) -2.0(5) 1_555 1_555 1_555 1_555 yes C(7) C(8) C(13) C(14) -80.8(4) 1_555 1_555 1_555 1_555 yes C(7) C(8) C(13) C(15) 43.1(4) 1_555 1_555 1_555 1_555 yes C(7) C(8) C(13) C(16) 160.5(3) 1_555 1_555 1_555 1_555 yes C(7) C(12) C(11) C(10) 2.5(5) 1_555 1_555 1_555 1_555 yes C(7) C(12) C(21) C(22) -165.3(3) 1_555 1_555 1_555 1_555 yes C(7) C(12) C(21) C(23) 76.8(4) 1_555 1_555 1_555 1_555 yes C(7) C(12) C(21) C(24) -47.6(4) 1_555 1_555 1_555 1_555 yes C(8) C(7) C(12) C(11) -8.0(4) 1_555 1_555 1_555 1_555 yes C(8) C(7) C(12) C(21) 169.1(3) 1_555 1_555 1_555 1_555 yes C(8) C(9) C(10) C(11) -3.4(5) 1_555 1_555 1_555 1_555 yes C(8) C(9) C(10) C(17) -179.6(3) 1_555 1_555 1_555 1_555 yes C(9) C(8) C(7) C(12) 7.7(4) 1_555 1_555 1_555 1_555 yes C(9) C(8) C(13) C(14) 102.5(3) 1_555 1_555 1_555 1_555 yes C(9) C(8) C(13) C(15) -133.6(3) 1_555 1_555 1_555 1_555 yes C(9) C(8) C(13) C(16) -16.2(4) 1_555 1_555 1_555 1_555 yes C(9) C(10) C(11) C(12) 3.1(5) 1_555 1_555 1_555 1_555 yes C(9) C(10) C(17) C(18) -1.7(5) 1_555 1_555 1_555 1_555 yes C(9) C(10) C(17) C(19) 118.5(3) 1_555 1_555 1_555 1_555 yes C(9) C(10) C(17) C(20) -121.7(3) 1_555 1_555 1_555 1_555 yes C(10) C(9) C(8) C(13) 174.9(3) 1_555 1_555 1_555 1_555 yes C(10) C(11) C(12) C(21) -174.9(3) 1_555 1_555 1_555 1_555 yes C(11) C(10) C(17) C(18) -177.8(3) 1_555 1_555 1_555 1_555 yes C(11) C(10) C(17) C(19) -57.6(4) 1_555 1_555 1_555 1_555 yes C(11) C(10) C(17) C(20) 62.1(4) 1_555 1_555 1_555 1_555 yes C(11) C(12) C(21) C(22) 11.8(5) 1_555 1_555 1_555 1_555 yes C(11) C(12) C(21) C(23) -106.1(4) 1_555 1_555 1_555 1_555 yes C(11) C(12) C(21) C(24) 129.5(4) 1_555 1_555 1_555 1_555 yes C(12) C(7) C(8) C(13) -169.0(3) 1_555 1_555 1_555 1_555 yes C(12) C(11) C(10) C(17) 179.5(3) 1_555 1_555 1_555 1_555 yes #------------------------------------------------------------------------------ #------------------------------------------------------------------------------ data_cPr-DPCB _database_code_depnum_ccdc_archive 'CCDC 272086' _audit_creation_date 'Wed Mar 9 23:05:55 2005' _audit_creation_method 'by teXsan' _audit_update_record ? #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C46 H68 P2 ' _chemical_formula_moiety 'C46 H68 P2 ' _chemical_formula_weight 682.99 _chemical_melting_point 312-315 #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz x,y,z 1/2-x,1/2+y,1/2-z -x,-y,-z 1/2+x,1/2-y,1/2+z _cell_length_a 15.9000(4) _cell_length_b 24.1687(7) _cell_length_c 11.3333(5) _cell_angle_alpha 90 _cell_angle_beta 89.711(1) _cell_angle_gamma 90 _cell_volume 4355.1(3) _cell_formula_units_Z 4 _cell_measurement_reflns_used 15541 _cell_measurement_theta_min 1.5 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 140 #------------------------------------------------------------------------------ _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.250 _exptl_crystal_size_mid 0.250 _exptl_crystal_size_min 0.200 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.042 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 0.128 _exptl_absorpt_correction_type none #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku RAXIS-IV Imaging Plate' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 35515 _diffrn_reflns_av_R_equivalents 0.084 _diffrn_reflns_theta_max 27.48 _diffrn_measured_fraction_theta_max 0.9889 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.9889 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > 2.0 sigma(F^2^). The weighted R-factor (wR), goodness of fit (S) and R-factor (gt) are based on F, with F set to zero for negative F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 9885 _reflns_number_gt 4764 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0969 _refine_ls_wR_factor_ref 0.1075 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 4764 _refine_ls_number_parameters 433 _refine_ls_goodness_of_fit_ref 1.673 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00123|Fo|^2^]' _refine_ls_shift/su_max 0.1276 _refine_diff_density_max 0.78 _refine_diff_density_min -0.82 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? 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 for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H H 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; P P 0.102 0.094 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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 P(1) P -0.05336(9) 0.29120(6) 0.3159(2) 0.0341(4) Uani 1.00 d . . . P(2) P -0.23673(9) 0.35488(6) 0.1920(2) 0.0344(4) Uani 1.00 d . . . C(1) C -0.0675(3) 0.3578(2) 0.2811(6) 0.034(2) Uani 1.00 d . . . C(2) C -0.1450(3) 0.3846(2) 0.2293(6) 0.038(2) Uani 1.00 d . . . C(3) C -0.0274(4) 0.4127(3) 0.2784(6) 0.042(2) Uani 1.00 d . . . C(4) C -0.0982(3) 0.4379(2) 0.2303(6) 0.036(2) Uani 1.00 d . . . C(5) C 0.0589(4) 0.4276(3) 0.3162(7) 0.048(2) Uani 1.00 d . . . C(6) C 0.1173(4) 0.4577(4) 0.2344(9) 0.078(3) Uani 1.00 d . . . C(7) C 0.0878(4) 0.4851(3) 0.3388(9) 0.068(3) Uani 1.00 d . . . C(8) C -0.1296(4) 0.4926(3) 0.1922(7) 0.048(2) Uani 1.00 d . . . C(9) C -0.1217(5) 0.5431(3) 0.2696(9) 0.068(3) Uani 1.00 d . . . C(10) C -0.0735(5) 0.5405(3) 0.1603(9) 0.069(3) Uani 1.00 d . . . C(11) C 0.0573(3) 0.2934(2) 0.3657(5) 0.029(2) Uani 1.00 d . . . C(12) C 0.0765(4) 0.3022(2) 0.4857(6) 0.034(2) Uani 1.00 d . . . C(13) C 0.1608(4) 0.3157(2) 0.5150(6) 0.038(2) Uani 1.00 d . . . C(14) C 0.2231(3) 0.3189(2) 0.4312(6) 0.037(2) Uani 1.00 d . . . C(15) C 0.2041(3) 0.3050(2) 0.3158(6) 0.033(2) Uani 1.00 d . . . C(16) C 0.1236(3) 0.2898(2) 0.2803(5) 0.030(2) Uani 1.00 d . . . C(17) C 0.0115(4) 0.2972(3) 0.5886(6) 0.048(2) Uani 1.00 d . . . C(18) C -0.0485(5) 0.3465(3) 0.5900(7) 0.070(3) Uani 1.00 d . . . C(19) C -0.0369(5) 0.2429(4) 0.5788(7) 0.070(3) Uani 1.00 d . . . C(20) C 0.0559(6) 0.2964(3) 0.7109(7) 0.073(3) Uani 1.00 d . . . C(21) C 0.3138(4) 0.3355(3) 0.4642(7) 0.058(2) Uani 1.00 d . . . C(22) C 0.3744(4) 0.2912(5) 0.4250(9) 0.097(3) Uani 1.00 d . . . C(23) C 0.3264(5) 0.3468(5) 0.5925(9) 0.121(4) Uani 1.00 d . . . C(24) C 0.3345(6) 0.3890(5) 0.395(1) 0.159(6) Uani 1.00 d . . . C(25) C 0.1130(4) 0.2687(3) 0.1510(6) 0.041(2) Uani 1.00 d . . . C(26) C 0.1983(4) 0.2522(3) 0.0970(6) 0.055(2) Uani 1.00 d . . . C(27) C 0.0591(4) 0.2158(3) 0.1513(6) 0.055(2) Uani 1.00 d . . . C(28) C 0.0762(5) 0.3126(4) 0.0715(7) 0.073(3) Uani 1.00 d . . . C(29) C -0.2957(3) 0.4161(2) 0.1382(5) 0.029(2) Uani 1.00 d . . . C(30) C -0.2929(3) 0.4316(2) 0.0191(6) 0.032(2) Uani 1.00 d . . . C(31) C -0.3236(3) 0.4847(3) -0.0120(6) 0.037(2) Uani 1.00 d . . . C(32) C -0.3586(3) 0.5206(2) 0.0698(6) 0.039(2) Uani 1.00 d . . . C(33) C -0.3679(4) 0.5029(3) 0.1835(6) 0.046(2) Uani 1.00 d . . . C(34) C -0.3407(4) 0.4497(3) 0.2213(6) 0.038(2) Uani 1.00 d . . . C(35) C -0.2578(4) 0.3940(3) -0.0807(6) 0.044(2) Uani 1.00 d . . . C(36) C -0.1615(5) 0.3913(3) -0.0775(7) 0.069(3) Uani 1.00 d . . . C(37) C -0.2973(5) 0.3361(3) -0.0735(7) 0.063(3) Uani 1.00 d . . . C(38) C -0.2819(5) 0.4170(3) -0.2049(7) 0.062(3) Uani 1.00 d . . . C(39) C -0.3870(4) 0.5791(3) 0.0324(7) 0.052(2) Uani 1.00 d . . . C(40) C -0.431(1) 0.5768(5) -0.083(1) 0.224(8) Uani 1.00 d . . . C(41) C -0.4525(6) 0.6021(4) 0.114(1) 0.109(4) Uani 1.00 d . . . C(42) C -0.3160(5) 0.6159(4) 0.034(2) 0.191(6) Uani 1.00 d . . . C(43) C -0.3608(5) 0.4329(4) 0.3505(7) 0.065(3) Uani 1.00 d . . . C(44) C -0.4300(5) 0.4693(4) 0.4045(7) 0.076(3) Uani 1.00 d . . . C(45) C -0.3974(5) 0.3741(4) 0.3531(8) 0.086(3) Uani 1.00 d . . . C(46) C -0.2837(6) 0.4373(4) 0.4306(7) 0.089(3) Uani 1.00 d . . . H(1) H 0.1058 0.4011 0.3696 0.0512 Uiso 1.00 calc . . . H(2) H 0.1745 0.4466 0.2256 0.0879 Uiso 1.00 calc . . . H(3) H 0.0977 0.4698 0.1579 0.0879 Uiso 1.00 calc . . . H(4) H 0.0494 0.5147 0.3348 0.0796 Uiso 1.00 calc . . . H(5) H 0.1263 0.4915 0.4025 0.0796 Uiso 1.00 calc . . . H(6) H -0.1880 0.4872 0.1345 0.0512 Uiso 1.00 calc . . . H(7) H -0.1683 0.5684 0.2764 0.0804 Uiso 1.00 calc . . . H(8) H -0.0947 0.5409 0.3439 0.0804 Uiso 1.00 calc . . . H(9) H -0.0134 0.5367 0.1626 0.0814 Uiso 1.00 calc . . . H(10) H -0.0870 0.5642 0.0950 0.0814 Uiso 1.00 calc . . . H(11) H 0.1694 0.3219 0.6070 0.0512 Uiso 1.00 calc . . . H(12) H 0.2549 0.3054 0.2504 0.0512 Uiso 1.00 calc . . . H(13) H -0.0767 0.3484 0.5169 0.0827 Uiso 1.00 calc . . . H(14) H -0.0171 0.3792 0.6026 0.0827 Uiso 1.00 calc . . . H(15) H -0.0880 0.3416 0.6522 0.0827 Uiso 1.00 calc . . . H(16) H -0.0662 0.2419 0.5062 0.0830 Uiso 1.00 calc . . . H(17) H -0.0757 0.2401 0.6425 0.0830 Uiso 1.00 calc . . . H(18) H 0.0017 0.2129 0.5821 0.0830 Uiso 1.00 calc . . . H(19) H 0.0146 0.2927 0.7718 0.0869 Uiso 1.00 calc . . . H(20) H 0.0936 0.2662 0.7144 0.0869 Uiso 1.00 calc . . . H(21) H 0.0858 0.3301 0.7220 0.0869 Uiso 1.00 calc . . . H(22) H 0.3669 0.2846 0.3429 0.1144 Uiso 1.00 calc . . . H(23) H 0.3644 0.2586 0.4679 0.1144 Uiso 1.00 calc . . . H(24) H 0.4304 0.3037 0.4381 0.1144 Uiso 1.00 calc . . . H(25) H 0.3130 0.3146 0.6365 0.1464 Uiso 1.00 calc . . . H(26) H 0.3837 0.3564 0.6054 0.1464 Uiso 1.00 calc . . . H(27) H 0.2912 0.3764 0.6162 0.1464 Uiso 1.00 calc . . . H(28) H 0.3896 0.4003 0.4140 0.1905 Uiso 1.00 calc . . . H(29) H 0.3304 0.3813 0.3134 0.1905 Uiso 1.00 calc . . . H(30) H 0.2952 0.4166 0.4167 0.1905 Uiso 1.00 calc . . . H(31) H 0.2345 0.2834 0.0956 0.0655 Uiso 1.00 calc . . . H(32) H 0.2228 0.2236 0.1428 0.0655 Uiso 1.00 calc . . . H(33) H 0.1901 0.2393 0.0185 0.0655 Uiso 1.00 calc . . . H(34) H 0.0863 0.1880 0.1967 0.0663 Uiso 1.00 calc . . . H(35) H 0.0519 0.2030 0.0729 0.0663 Uiso 1.00 calc . . . H(36) H 0.0055 0.2235 0.1853 0.0663 Uiso 1.00 calc . . . H(37) H 0.0731 0.2994 -0.0074 0.0876 Uiso 1.00 calc . . . H(38) H 0.0215 0.3226 0.0980 0.0876 Uiso 1.00 calc . . . H(39) H 0.1113 0.3449 0.0727 0.0876 Uiso 1.00 calc . . . H(40) H -0.3317 0.4932 -0.0944 0.0512 Uiso 1.00 calc . . . H(41) H -0.4138 0.5109 0.2418 0.0512 Uiso 1.00 calc . . . H(42) H -0.1392 0.4273 -0.0881 0.0813 Uiso 1.00 calc . . . H(43) H -0.1440 0.3768 -0.0038 0.0813 Uiso 1.00 calc . . . H(44) H -0.1420 0.3678 -0.1394 0.0813 Uiso 1.00 calc . . . H(45) H -0.2845 0.3200 0.0003 0.0763 Uiso 1.00 calc . . . H(46) H -0.2757 0.3138 -0.1354 0.0763 Uiso 1.00 calc . . . H(47) H -0.3567 0.3394 -0.0814 0.0763 Uiso 1.00 calc . . . H(48) H -0.2596 0.3933 -0.2646 0.0718 Uiso 1.00 calc . . . H(49) H -0.3413 0.4184 -0.2116 0.0718 Uiso 1.00 calc . . . H(50) H -0.2592 0.4530 -0.2143 0.0718 Uiso 1.00 calc . . . H(51) H -0.3876 0.5652 -0.1410 0.2836 Uiso 1.00 calc . . . H(52) H -0.4742 0.5541 -0.0819 0.2836 Uiso 1.00 calc . . . H(53) H -0.4446 0.6144 -0.1043 0.2836 Uiso 1.00 calc . . . H(54) H -0.4983 0.5769 0.1187 0.1329 Uiso 1.00 calc . . . H(55) H -0.4719 0.6365 0.0833 0.1329 Uiso 1.00 calc . . . H(56) H -0.4290 0.6075 0.1893 0.1329 Uiso 1.00 calc . . . H(57) H -0.3328 0.6516 0.0099 0.2289 Uiso 1.00 calc . . . H(58) H -0.2946 0.6177 0.1129 0.2289 Uiso 1.00 calc . . . H(59) H -0.2735 0.6021 -0.0167 0.2289 Uiso 1.00 calc . . . H(60) H -0.4112 0.5067 0.4078 0.0907 Uiso 1.00 calc . . . H(61) H -0.4790 0.4673 0.3570 0.0907 Uiso 1.00 calc . . . H(62) H -0.4430 0.4569 0.4821 0.0907 Uiso 1.00 calc . . . H(63) H -0.4467 0.3732 0.3065 0.1014 Uiso 1.00 calc . . . H(64) H -0.4110 0.3644 0.4322 0.1014 Uiso 1.00 calc . . . H(65) H -0.3572 0.3489 0.3225 0.1014 Uiso 1.00 calc . . . H(66) H -0.2987 0.4256 0.5081 0.1058 Uiso 1.00 calc . . . H(67) H -0.2401 0.4146 0.4007 0.1058 Uiso 1.00 calc . . . H(68) H -0.2656 0.4747 0.4330 0.1058 Uiso 1.00 calc . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 P(1) 0.0246(7) 0.0273(8) 0.050(1) 0.0009(6) -0.0032(7) -0.0006(8) P(2) 0.0254(7) 0.0310(8) 0.047(1) 0.0033(7) -0.0013(7) 0.0050(8) C(1) 0.024(2) 0.036(3) 0.041(4) 0.005(2) -0.006(3) -0.005(3) C(2) 0.033(3) 0.035(3) 0.046(4) 0.008(3) -0.003(3) 0.004(3) C(3) 0.032(3) 0.035(3) 0.059(5) 0.001(3) 0.004(3) 0.003(3) C(4) 0.034(3) 0.027(3) 0.045(4) -0.003(3) 0.001(3) 0.005(3) C(5) 0.035(3) 0.038(4) 0.071(5) -0.009(3) -0.012(3) 0.005(4) C(6) 0.044(4) 0.074(6) 0.115(9) -0.011(4) 0.008(5) 0.019(6) C(7) 0.043(4) 0.036(4) 0.126(8) -0.006(3) -0.025(5) -0.006(5) C(8) 0.044(3) 0.029(3) 0.069(6) -0.008(3) -0.012(3) 0.001(4) C(9) 0.064(5) 0.041(4) 0.099(8) 0.002(4) -0.008(5) -0.007(5) C(10) 0.056(4) 0.041(4) 0.110(8) -0.003(3) -0.006(5) 0.027(5) C(11) 0.032(3) 0.021(3) 0.033(4) 0.006(2) -0.002(2) -0.002(3) C(12) 0.046(3) 0.023(3) 0.035(4) 0.001(3) 0.005(3) -0.005(3) C(13) 0.049(3) 0.037(3) 0.027(4) -0.003(3) -0.015(3) -0.004(3) C(14) 0.025(3) 0.038(3) 0.049(5) 0.001(3) -0.006(3) -0.009(3) C(15) 0.025(3) 0.036(3) 0.038(4) -0.002(2) -0.001(3) -0.003(3) C(16) 0.028(3) 0.036(3) 0.026(4) 0.008(2) -0.003(2) 0.002(3) C(17) 0.064(4) 0.051(4) 0.028(4) -0.024(4) 0.016(3) -0.011(3) C(18) 0.066(5) 0.081(6) 0.061(6) 0.000(4) 0.024(4) -0.036(5) C(19) 0.086(5) 0.085(6) 0.037(5) -0.036(5) 0.023(4) -0.006(4) C(20) 0.109(7) 0.078(6) 0.031(5) -0.034(5) 0.015(5) -0.006(4) C(21) 0.036(3) 0.065(5) 0.072(6) -0.005(3) -0.019(4) -0.022(5) C(22) 0.032(4) 0.167(10) 0.091(7) 0.011(5) -0.020(4) -0.058(7) C(23) 0.048(5) 0.21(1) 0.101(9) 0.018(6) -0.032(5) -0.094(9) C(24) 0.083(7) 0.13(1) 0.26(2) -0.069(7) -0.072(9) 0.05(1) C(25) 0.040(3) 0.059(4) 0.025(4) 0.006(3) -0.007(3) -0.009(3) C(26) 0.053(4) 0.081(5) 0.031(4) 0.000(4) 0.009(3) -0.010(4) C(27) 0.047(4) 0.079(5) 0.041(5) -0.006(4) -0.008(3) -0.038(4) C(28) 0.077(5) 0.103(7) 0.040(5) 0.017(5) -0.014(4) 0.005(5) C(29) 0.025(2) 0.027(3) 0.036(4) 0.000(2) 0.001(2) 0.004(3) C(30) 0.027(3) 0.035(3) 0.033(4) -0.007(2) 0.005(3) 0.005(3) C(31) 0.038(3) 0.041(4) 0.031(4) -0.004(3) -0.005(3) 0.006(3) C(32) 0.037(3) 0.035(3) 0.044(5) 0.008(3) 0.000(3) 0.007(3) C(33) 0.041(3) 0.049(4) 0.048(5) 0.022(3) 0.010(3) 0.006(4) C(34) 0.043(3) 0.045(4) 0.025(4) 0.011(3) 0.006(3) 0.007(3) C(35) 0.054(4) 0.038(4) 0.041(4) -0.008(3) 0.005(3) -0.008(3) C(36) 0.063(5) 0.087(6) 0.056(6) 0.020(4) 0.029(4) -0.005(5) C(37) 0.108(6) 0.048(4) 0.035(5) 0.002(4) -0.014(4) -0.015(4) C(38) 0.085(5) 0.055(5) 0.046(5) -0.004(4) 0.010(4) -0.010(4) C(39) 0.061(4) 0.044(4) 0.049(5) 0.021(3) -0.003(4) 0.008(4) C(40) 0.48(3) 0.090(9) 0.10(1) 0.15(1) -0.12(1) -0.012(8) C(41) 0.091(6) 0.069(6) 0.17(1) 0.056(5) 0.050(7) 0.046(7) C(42) 0.049(5) 0.049(6) 0.48(3) -0.016(4) -0.002(9) 0.11(1) C(43) 0.064(4) 0.085(6) 0.045(5) 0.038(4) 0.024(4) 0.026(4) C(44) 0.074(5) 0.110(7) 0.043(5) 0.034(5) 0.028(4) 0.015(5) C(45) 0.083(6) 0.093(7) 0.082(7) 0.031(5) 0.057(5) 0.051(6) C(46) 0.089(6) 0.146(9) 0.032(5) 0.046(6) 0.008(4) 0.012(6) #------------------------------------------------------------------------------ _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction 'teXsan Ver. 1.10' _computing_structure_solution SIR92 _computing_structure_refinement 'teXsan Ver. 1.10' _computing_publication_material 'teXsan Ver. 1.10' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag P(1) C(1) 1.674(6) . . yes P(1) C(11) 1.851(5) . . yes P(2) C(2) 1.682(6) . . yes P(2) C(29) 1.857(6) . . yes C(1) C(2) 1.513(7) . . yes C(1) C(3) 1.472(8) . . yes C(2) C(4) 1.487(8) . . yes C(3) C(4) 1.393(8) . . yes C(3) C(5) 1.484(8) . . yes C(4) C(8) 1.478(8) . . yes C(5) C(6) 1.50(1) . . yes C(5) C(7) 1.486(9) . . yes C(6) C(7) 1.43(1) . . yes C(8) C(9) 1.510(10) . . yes C(8) C(10) 1.505(9) . . yes C(9) C(10) 1.45(1) . . yes C(11) C(12) 1.412(8) . . yes C(11) C(16) 1.430(8) . . yes C(12) C(13) 1.420(8) . . yes C(12) C(17) 1.558(8) . . yes C(13) C(14) 1.371(9) . . yes C(14) C(15) 1.386(9) . . yes C(14) C(21) 1.544(8) . . yes C(15) C(16) 1.393(7) . . yes C(16) C(25) 1.562(8) . . yes C(17) C(18) 1.53(1) . . yes C(17) C(19) 1.527(9) . . yes C(17) C(20) 1.56(1) . . yes C(21) C(22) 1.51(1) . . yes C(21) C(23) 1.49(1) . . yes C(21) C(24) 1.55(1) . . yes C(25) C(26) 1.537(9) . . yes C(25) C(27) 1.538(9) . . yes C(25) C(28) 1.512(10) . . yes C(29) C(30) 1.401(8) . . yes C(29) C(34) 1.432(8) . . yes C(30) C(31) 1.418(8) . . yes C(30) C(35) 1.553(9) . . yes C(31) C(32) 1.385(8) . . yes C(32) C(33) 1.365(9) . . yes C(32) C(39) 1.544(8) . . yes C(33) C(34) 1.423(8) . . yes C(34) C(43) 1.550(9) . . yes C(35) C(36) 1.533(9) . . yes C(35) C(37) 1.536(9) . . yes C(35) C(38) 1.56(1) . . yes C(39) C(40) 1.49(1) . . yes C(39) C(41) 1.50(1) . . yes C(39) C(42) 1.44(1) . . yes C(43) C(44) 1.535(10) . . yes C(43) C(45) 1.54(1) . . yes C(43) C(46) 1.53(1) . . yes #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C(1) P(1) C(11) 100.0(2) . 1_555 1_555 yes C(2) P(2) C(29) 100.5(3) . 1_555 1_555 yes P(1) C(1) C(2) 127.8(4) . 1_555 1_555 yes P(1) C(1) C(3) 144.5(4) . 1_555 1_555 yes C(2) C(1) C(3) 87.7(4) . 1_555 1_555 yes P(2) C(2) C(1) 128.6(4) . 1_555 1_555 yes P(2) C(2) C(4) 143.7(4) . 1_555 1_555 yes C(1) C(2) C(4) 87.6(4) . 1_555 1_555 yes C(1) C(3) C(4) 92.9(5) . 1_555 1_555 yes C(1) C(3) C(5) 127.8(5) . 1_555 1_555 yes C(4) C(3) C(5) 139.2(6) . 1_555 1_555 yes C(2) C(4) C(3) 91.7(5) . 1_555 1_555 yes C(2) C(4) C(8) 127.0(5) . 1_555 1_555 yes C(3) C(4) C(8) 141.3(5) . 1_555 1_555 yes C(3) C(5) C(6) 120.7(7) . 1_555 1_555 yes C(3) C(5) C(7) 124.3(5) . 1_555 1_555 yes C(6) C(5) C(7) 57.4(5) . 1_555 1_555 yes C(5) C(6) C(7) 60.9(5) . 1_555 1_555 yes C(5) C(7) C(6) 61.7(5) . 1_555 1_555 yes C(4) C(8) C(9) 121.6(6) . 1_555 1_555 yes C(4) C(8) C(10) 123.8(5) . 1_555 1_555 yes C(9) C(8) C(10) 57.7(5) . 1_555 1_555 yes C(8) C(9) C(10) 61.0(5) . 1_555 1_555 yes C(8) C(10) C(9) 61.3(5) . 1_555 1_555 yes P(1) C(11) C(12) 120.6(4) . 1_555 1_555 yes P(1) C(11) C(16) 119.3(4) . 1_555 1_555 yes C(12) C(11) C(16) 119.9(5) . 1_555 1_555 yes C(11) C(12) C(13) 117.9(6) . 1_555 1_555 yes C(11) C(12) C(17) 124.3(5) . 1_555 1_555 yes C(13) C(12) C(17) 117.8(6) . 1_555 1_555 yes C(12) C(13) C(14) 122.1(6) . 1_555 1_555 yes C(13) C(14) C(15) 118.6(5) . 1_555 1_555 yes C(13) C(14) C(21) 121.4(6) . 1_555 1_555 yes C(15) C(14) C(21) 120.0(6) . 1_555 1_555 yes C(14) C(15) C(16) 122.9(5) . 1_555 1_555 yes C(11) C(16) C(15) 117.6(5) . 1_555 1_555 yes C(11) C(16) C(25) 124.9(5) . 1_555 1_555 yes C(15) C(16) C(25) 117.5(5) . 1_555 1_555 yes C(12) C(17) C(18) 111.1(6) . 1_555 1_555 yes C(12) C(17) C(19) 110.1(5) . 1_555 1_555 yes C(12) C(17) C(20) 111.4(6) . 1_555 1_555 yes C(18) C(17) C(19) 110.9(6) . 1_555 1_555 yes C(18) C(17) C(20) 106.7(6) . 1_555 1_555 yes C(19) C(17) C(20) 106.5(6) . 1_555 1_555 yes C(14) C(21) C(22) 109.9(6) . 1_555 1_555 yes C(14) C(21) C(23) 114.4(7) . 1_555 1_555 yes C(14) C(21) C(24) 106.9(6) . 1_555 1_555 yes C(22) C(21) C(23) 109.1(7) . 1_555 1_555 yes C(22) C(21) C(24) 108.0(9) . 1_555 1_555 yes C(23) C(21) C(24) 108.3(9) . 1_555 1_555 yes C(16) C(25) C(26) 111.1(5) . 1_555 1_555 yes C(16) C(25) C(27) 109.4(5) . 1_555 1_555 yes C(16) C(25) C(28) 112.0(6) . 1_555 1_555 yes C(26) C(25) C(27) 106.0(5) . 1_555 1_555 yes C(26) C(25) C(28) 106.7(6) . 1_555 1_555 yes C(27) C(25) C(28) 111.5(6) . 1_555 1_555 yes P(2) C(29) C(30) 121.0(4) . 1_555 1_555 yes P(2) C(29) C(34) 119.1(4) . 1_555 1_555 yes C(30) C(29) C(34) 119.8(5) . 1_555 1_555 yes C(29) C(30) C(31) 118.1(5) . 1_555 1_555 yes C(29) C(30) C(35) 123.8(5) . 1_555 1_555 yes C(31) C(30) C(35) 118.1(6) . 1_555 1_555 yes C(30) C(31) C(32) 122.6(6) . 1_555 1_555 yes C(31) C(32) C(33) 118.4(6) . 1_555 1_555 yes C(31) C(32) C(39) 120.5(6) . 1_555 1_555 yes C(33) C(32) C(39) 121.1(6) . 1_555 1_555 yes C(32) C(33) C(34) 122.5(6) . 1_555 1_555 yes C(29) C(34) C(33) 117.7(6) . 1_555 1_555 yes C(29) C(34) C(43) 125.0(6) . 1_555 1_555 yes C(33) C(34) C(43) 117.4(6) . 1_555 1_555 yes C(30) C(35) C(36) 111.3(5) . 1_555 1_555 yes C(30) C(35) C(37) 110.4(5) . 1_555 1_555 yes C(30) C(35) C(38) 111.1(5) . 1_555 1_555 yes C(36) C(35) C(37) 111.6(6) . 1_555 1_555 yes C(36) C(35) C(38) 106.6(6) . 1_555 1_555 yes C(37) C(35) C(38) 105.7(6) . 1_555 1_555 yes C(32) C(39) C(40) 110.2(7) . 1_555 1_555 yes C(32) C(39) C(41) 111.8(6) . 1_555 1_555 yes C(32) C(39) C(42) 109.4(6) . 1_555 1_555 yes C(40) C(39) C(41) 103.4(9) . 1_555 1_555 yes C(40) C(39) C(42) 114(1) . 1_555 1_555 yes C(41) C(39) C(42) 107.8(9) . 1_555 1_555 yes C(34) C(43) C(44) 111.8(6) . 1_555 1_555 yes C(34) C(43) C(45) 109.7(7) . 1_555 1_555 yes C(34) C(43) C(46) 112.3(6) . 1_555 1_555 yes C(44) C(43) C(45) 104.6(6) . 1_555 1_555 yes C(44) C(43) C(46) 107.3(7) . 1_555 1_555 yes C(45) C(43) C(46) 110.9(7) . 1_555 1_555 yes #------------------------------------------------------------------------------ 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 P(1) C(1) C(2) P(2) -0.5(10) 1_555 1_555 1_555 1_555 yes P(1) C(1) C(2) C(4) -179.3(5) 1_555 1_555 1_555 1_555 yes P(1) C(1) C(3) C(4) 179.1(8) 1_555 1_555 1_555 1_555 yes P(1) C(1) C(3) C(5) 0(1) 1_555 1_555 1_555 1_555 yes P(1) C(11) C(12) C(13) -166.2(4) 1_555 1_555 1_555 1_555 yes P(1) C(11) C(12) C(17) 14.6(8) 1_555 1_555 1_555 1_555 yes P(1) C(11) C(16) C(15) 164.5(4) 1_555 1_555 1_555 1_555 yes P(1) C(11) C(16) C(25) -17.0(8) 1_555 1_555 1_555 1_555 yes P(2) C(2) C(1) C(3) 178.9(6) 1_555 1_555 1_555 1_555 yes P(2) C(2) C(4) C(3) -178.6(8) 1_555 1_555 1_555 1_555 yes P(2) C(2) C(4) C(8) 2(1) 1_555 1_555 1_555 1_555 yes P(2) C(29) C(30) C(31) -166.5(4) 1_555 1_555 1_555 1_555 yes P(2) C(29) C(30) C(35) 13.1(7) 1_555 1_555 1_555 1_555 yes P(2) C(29) C(34) C(33) 165.1(5) 1_555 1_555 1_555 1_555 yes P(2) C(29) C(34) C(43) -13.7(8) 1_555 1_555 1_555 1_555 yes C(1) P(1) C(11) C(12) 91.6(5) 1_555 1_555 1_555 1_555 yes C(1) P(1) C(11) C(16) -84.2(5) 1_555 1_555 1_555 1_555 yes C(1) C(2) P(2) C(29) 179.4(6) 1_555 1_555 1_555 1_555 yes C(1) C(2) C(4) C(3) -0.2(5) 1_555 1_555 1_555 1_555 yes C(1) C(2) C(4) C(8) -179.0(7) 1_555 1_555 1_555 1_555 yes C(1) C(3) C(4) C(2) 0.2(6) 1_555 1_555 1_555 1_555 yes C(1) C(3) C(4) C(8) 178.7(9) 1_555 1_555 1_555 1_555 yes C(1) C(3) C(5) C(6) 126.6(8) 1_555 1_555 1_555 1_555 yes C(1) C(3) C(5) C(7) -164.1(8) 1_555 1_555 1_555 1_555 yes C(2) P(2) C(29) C(30) 90.8(5) 1_555 1_555 1_555 1_555 yes C(2) P(2) C(29) C(34) -85.7(5) 1_555 1_555 1_555 1_555 yes C(2) C(1) P(1) C(11) 177.5(6) 1_555 1_555 1_555 1_555 yes C(2) C(1) C(3) C(4) -0.2(5) 1_555 1_555 1_555 1_555 yes C(2) C(1) C(3) C(5) -179.7(7) 1_555 1_555 1_555 1_555 yes C(2) C(4) C(3) C(5) 179.5(9) 1_555 1_555 1_555 1_555 yes C(2) C(4) C(8) C(9) 129.6(7) 1_555 1_555 1_555 1_555 yes C(2) C(4) C(8) C(10) -160.5(7) 1_555 1_555 1_555 1_555 yes C(3) C(1) P(1) C(11) -1.5(9) 1_555 1_555 1_555 1_555 yes C(3) C(1) C(2) C(4) 0.2(5) 1_555 1_555 1_555 1_555 yes C(3) C(4) C(8) C(9) -48(1) 1_555 1_555 1_555 1_555 yes C(3) C(4) C(8) C(10) 21(1) 1_555 1_555 1_555 1_555 yes C(3) C(5) C(6) C(7) 113.5(7) 1_555 1_555 1_555 1_555 yes C(3) C(5) C(7) C(6) -107.2(9) 1_555 1_555 1_555 1_555 yes C(4) C(2) P(2) C(29) -2.6(9) 1_555 1_555 1_555 1_555 yes C(4) C(3) C(5) C(6) -52(1) 1_555 1_555 1_555 1_555 yes C(4) C(3) C(5) C(7) 16(1) 1_555 1_555 1_555 1_555 yes C(4) C(8) C(9) C(10) 112.6(7) 1_555 1_555 1_555 1_555 yes C(4) C(8) C(10) C(9) -108.9(8) 1_555 1_555 1_555 1_555 yes C(5) C(3) C(4) C(8) -1(1) 1_555 1_555 1_555 1_555 yes C(11) C(12) C(13) C(14) -1.7(9) 1_555 1_555 1_555 1_555 yes C(11) C(12) C(17) C(18) -73.9(7) 1_555 1_555 1_555 1_555 yes C(11) C(12) C(17) C(19) 49.4(8) 1_555 1_555 1_555 1_555 yes C(11) C(12) C(17) C(20) 167.3(6) 1_555 1_555 1_555 1_555 yes C(11) C(16) C(15) C(14) 5.4(9) 1_555 1_555 1_555 1_555 yes C(11) C(16) C(25) C(26) -161.4(6) 1_555 1_555 1_555 1_555 yes C(11) C(16) C(25) C(27) -44.7(8) 1_555 1_555 1_555 1_555 yes C(11) C(16) C(25) C(28) 79.5(8) 1_555 1_555 1_555 1_555 yes C(12) C(11) C(16) C(15) -11.3(8) 1_555 1_555 1_555 1_555 yes C(12) C(11) C(16) C(25) 167.1(5) 1_555 1_555 1_555 1_555 yes C(12) C(13) C(14) C(15) -4.3(9) 1_555 1_555 1_555 1_555 yes C(12) C(13) C(14) C(21) 178.1(6) 1_555 1_555 1_555 1_555 yes C(13) C(12) C(11) C(16) 9.6(8) 1_555 1_555 1_555 1_555 yes C(13) C(12) C(17) C(18) 107.0(7) 1_555 1_555 1_555 1_555 yes C(13) C(12) C(17) C(19) -129.8(6) 1_555 1_555 1_555 1_555 yes C(13) C(12) C(17) C(20) -11.8(8) 1_555 1_555 1_555 1_555 yes C(13) C(14) C(15) C(16) 2.4(9) 1_555 1_555 1_555 1_555 yes C(13) C(14) C(21) C(22) 123.7(8) 1_555 1_555 1_555 1_555 yes C(13) C(14) C(21) C(23) 0(1) 1_555 1_555 1_555 1_555 yes C(13) C(14) C(21) C(24) -119.3(9) 1_555 1_555 1_555 1_555 yes C(14) C(13) C(12) C(17) 177.5(6) 1_555 1_555 1_555 1_555 yes C(14) C(15) C(16) C(25) -173.2(6) 1_555 1_555 1_555 1_555 yes C(15) C(14) C(21) C(22) -54.0(9) 1_555 1_555 1_555 1_555 yes C(15) C(14) C(21) C(23) -177.1(8) 1_555 1_555 1_555 1_555 yes C(15) C(14) C(21) C(24) 63.0(10) 1_555 1_555 1_555 1_555 yes C(15) C(16) C(25) C(26) 17.0(8) 1_555 1_555 1_555 1_555 yes C(15) C(16) C(25) C(27) 133.7(6) 1_555 1_555 1_555 1_555 yes C(15) C(16) C(25) C(28) -102.1(6) 1_555 1_555 1_555 1_555 yes C(16) C(11) C(12) C(17) -169.6(5) 1_555 1_555 1_555 1_555 yes C(16) C(15) C(14) C(21) -179.9(6) 1_555 1_555 1_555 1_555 yes C(29) C(30) C(31) C(32) -2.5(8) 1_555 1_555 1_555 1_555 yes C(29) C(30) C(35) C(36) -74.3(7) 1_555 1_555 1_555 1_555 yes C(29) C(30) C(35) C(37) 50.2(8) 1_555 1_555 1_555 1_555 yes C(29) C(30) C(35) C(38) 167.1(5) 1_555 1_555 1_555 1_555 yes C(29) C(34) C(33) C(32) 5.6(9) 1_555 1_555 1_555 1_555 yes C(29) C(34) C(43) C(44) -163.6(7) 1_555 1_555 1_555 1_555 yes C(29) C(34) C(43) C(45) -48.1(8) 1_555 1_555 1_555 1_555 yes C(29) C(34) C(43) C(46) 75.7(9) 1_555 1_555 1_555 1_555 yes C(30) C(29) C(34) C(33) -11.5(8) 1_555 1_555 1_555 1_555 yes C(30) C(29) C(34) C(43) 169.8(6) 1_555 1_555 1_555 1_555 yes C(30) C(31) C(32) C(33) -3.4(9) 1_555 1_555 1_555 1_555 yes C(30) C(31) C(32) C(39) 176.9(5) 1_555 1_555 1_555 1_555 yes C(31) C(30) C(29) C(34) 10.0(8) 1_555 1_555 1_555 1_555 yes C(31) C(30) C(35) C(36) 105.3(6) 1_555 1_555 1_555 1_555 yes C(31) C(30) C(35) C(37) -130.2(6) 1_555 1_555 1_555 1_555 yes C(31) C(30) C(35) C(38) -13.3(7) 1_555 1_555 1_555 1_555 yes C(31) C(32) C(33) C(34) 1.8(10) 1_555 1_555 1_555 1_555 yes C(31) C(32) C(39) C(40) 42(1) 1_555 1_555 1_555 1_555 yes C(31) C(32) C(39) C(41) 156.7(7) 1_555 1_555 1_555 1_555 yes C(31) C(32) C(39) C(42) -84(1) 1_555 1_555 1_555 1_555 yes C(32) C(31) C(30) C(35) 177.8(5) 1_555 1_555 1_555 1_555 yes C(32) C(33) C(34) C(43) -175.6(6) 1_555 1_555 1_555 1_555 yes C(33) C(32) C(39) C(40) -137(1) 1_555 1_555 1_555 1_555 yes C(33) C(32) C(39) C(41) -23.0(10) 1_555 1_555 1_555 1_555 yes C(33) C(32) C(39) C(42) 96(1) 1_555 1_555 1_555 1_555 yes C(33) C(34) C(43) C(44) 17.6(10) 1_555 1_555 1_555 1_555 yes C(33) C(34) C(43) C(45) 133.1(6) 1_555 1_555 1_555 1_555 yes C(33) C(34) C(43) C(46) -103.1(7) 1_555 1_555 1_555 1_555 yes C(34) C(29) C(30) C(35) -170.4(5) 1_555 1_555 1_555 1_555 yes C(34) C(33) C(32) C(39) -178.6(6) 1_555 1_555 1_555 1_555 yes data_cPr-DPCB-Au2 _database_code_depnum_ccdc_archive 'CCDC 272087' _audit_creation_date 'Fri Apr 8 20:10:13 2005' _audit_creation_method 'by teXsan' _audit_update_record ? #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C46 H68 Au2 Cl2 P2 ' _chemical_formula_moiety 'C46 H68 Au2 Cl2 P2 ' _chemical_formula_weight 1147.83 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P n a 21 ' _symmetry_Int_Tables_number 33 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,1/2+z 1/2-x,1/2+y,1/2+z 1/2+x,1/2-y,z _cell_length_a 19.4009(5) _cell_length_b 15.0454(4) _cell_length_c 15.8448(7) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 4625.0(3) _cell_formula_units_Z 4 _cell_measurement_reflns_used 31947 _cell_measurement_theta_min 1.7 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 133 #------------------------------------------------------------------------------ _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.200 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_min 0.100 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.648 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 6.573 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(Higashi, 1995)' _exptl_absorpt_correction_T_min 0.361 _exptl_absorpt_correction_T_max 0.518 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\/Ya' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku RAXIS-IV Imaging Plate' _diffrn_measurement_method \/Yw _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 36160 _diffrn_reflns_av_R_equivalents 0.065 _diffrn_reflns_theta_max 27.48 _diffrn_measured_fraction_theta_max 0.9692 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.9692 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 20 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > 0.0 sigma(F^2^). The weighted R-factor (wR), goodness of fit (S) and R-factor (gt) are based on F, with F set to zero for negative F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 5323 _reflns_number_gt 4554 _reflns_threshold_expression F^2^>2.0\/Ys(F^2^) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0314 _refine_ls_wR_factor_ref 0.0380 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 5323 _refine_ls_number_parameters 470 _refine_ls_goodness_of_fit_ref 0.789 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\/Ys^2^(Fo) + 0.00063|Fo|^2^]' _refine_ls_shift/su_max 0.0234 _refine_diff_density_max 1.37 _refine_diff_density_min -1.93 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack 0.32(2) 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 for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H H 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; P P 0.102 0.094 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Au Au -2.013 8.802 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Cl Cl 0.148 0.159 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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 Au(1) Au 0.29073(2) -0.51680(3) 0.876(1) 0.01570(8) Uani 1.00 d . . . Au(2) Au 0.30376(2) -0.32090(3) 0.841(1) 0.02272(9) Uani 1.00 d . . . Cl(1) Cl 0.3636(2) -0.5015(2) 0.989(1) 0.0291(7) Uani 1.00 d . . . Cl(2) Cl 0.2462(2) -0.2787(3) 0.960(1) 0.061(1) Uani 1.00 d . . . P(1) P 0.2284(1) -0.5363(2) 0.760(1) 0.0133(6) Uani 1.00 d . . . P(2) P 0.3531(1) -0.3522(2) 0.718(1) 0.0132(6) Uani 1.00 d . . . C(1) C 0.2611(5) -0.4946(6) 0.671(1) 0.013(2) Uani 1.00 d . . . C(2) C 0.3192(5) -0.4314(7) 0.657(1) 0.014(2) Uani 1.00 d . . . C(3) C 0.3184(5) -0.4580(6) 0.567(1) 0.014(2) Uani 1.00 d . . . C(4) C 0.2580(6) -0.5068(7) 0.578(1) 0.017(2) Uani 1.00 d . . . C(5) C 0.3672(6) -0.4392(7) 0.499(1) 0.020(3) Uani 1.00 d . . . C(6) C 0.4226(6) -0.5077(8) 0.482(1) 0.024(3) Uani 1.00 d . . . C(7) C 0.3672(6) -0.4932(8) 0.418(1) 0.027(3) Uani 1.00 d . . . C(8) C 0.2109(6) -0.5562(8) 0.523(1) 0.025(3) Uani 1.00 d . . . C(9) C 0.1953(7) -0.5253(9) 0.435(1) 0.033(3) Uani 1.00 d . . . C(10) C 0.1413(6) -0.518(1) 0.501(2) 0.037(3) Uani 1.00 d . . . C(11) C 0.1491(5) -0.5952(6) 0.731(1) 0.011(2) Uani 1.00 d . . . C(12) C 0.1498(5) -0.6870(7) 0.707(1) 0.014(2) Uani 1.00 d . . . C(13) C 0.0955(6) -0.7179(7) 0.660(1) 0.016(3) Uani 1.00 d . . . C(14) C 0.0402(5) -0.6639(7) 0.636(1) 0.012(2) Uani 1.00 d . . . C(15) C 0.0372(5) -0.5784(7) 0.668(1) 0.013(2) Uani 1.00 d . . . C(16) C 0.0900(5) -0.5416(6) 0.717(1) 0.013(2) Uani 1.00 d . . . C(17) C 0.2051(5) -0.7542(7) 0.738(1) 0.016(2) Uani 1.00 d . . . C(18) C 0.2771(5) -0.7366(7) 0.702(1) 0.020(3) Uani 1.00 d . . . C(19) C 0.2076(5) -0.7508(6) 0.835(1) 0.017(2) Uani 1.00 d . . . C(20) C 0.1870(6) -0.8497(7) 0.712(1) 0.026(3) Uani 1.00 d . . . C(21) C -0.0174(5) -0.7022(7) 0.581(1) 0.017(2) Uani 1.00 d . . . C(22) C -0.0511(5) -0.7818(8) 0.626(1) 0.023(3) Uani 1.00 d . . . C(23) C -0.0742(6) -0.6354(8) 0.562(1) 0.025(3) Uani 1.00 d . . . C(24) C 0.0123(6) -0.7356(9) 0.496(1) 0.030(3) Uani 1.00 d . . . C(25) C 0.0776(5) -0.4466(7) 0.754(1) 0.018(2) Uani 1.00 d . . . C(26) C -0.0009(6) -0.4247(8) 0.755(2) 0.029(3) Uani 1.00 d . . . C(27) C 0.1008(6) -0.4416(9) 0.848(2) 0.033(3) Uani 1.00 d . . . C(28) C 0.1122(8) -0.3750(8) 0.700(2) 0.044(4) Uani 1.00 d . . . C(29) C 0.4148(5) -0.2944(6) 0.651(1) 0.011(2) Uani 1.00 d . . . C(30) C 0.3927(6) -0.2253(7) 0.597(1) 0.014(2) Uani 1.00 d . . . C(31) C 0.4358(5) -0.2055(7) 0.528(1) 0.016(2) Uani 1.00 d . . . C(32) C 0.4970(5) -0.2501(7) 0.511(1) 0.013(2) Uani 1.00 d . . . C(33) C 0.5201(5) -0.3103(7) 0.572(1) 0.015(2) Uani 1.00 d . . . C(34) C 0.4829(5) -0.3325(6) 0.644(1) 0.013(2) Uani 1.00 d . . . C(35) C 0.3262(5) -0.1683(7) 0.607(1) 0.018(2) Uani 1.00 d . . . C(36) C 0.2610(6) -0.2238(8) 0.584(1) 0.025(3) Uani 1.00 d . . . C(37) C 0.3193(6) -0.1330(7) 0.699(1) 0.023(3) Uani 1.00 d . . . C(38) C 0.3262(6) -0.0876(7) 0.550(1) 0.021(3) Uani 1.00 d . . . C(39) C 0.5357(5) -0.2391(7) 0.427(1) 0.018(2) Uani 1.00 d . . . C(40) C 0.5162(5) -0.1537(7) 0.383(1) 0.027(3) Uani 1.00 d . . . C(41) C 0.6142(5) -0.2405(8) 0.442(1) 0.024(3) Uani 1.00 d . . . C(42) C 0.5175(6) -0.3200(8) 0.371(1) 0.031(3) Uani 1.00 d . . . C(43) C 0.5168(6) -0.3938(7) 0.711(1) 0.018(2) Uani 1.00 d . . . C(44) C 0.5955(6) -0.3915(7) 0.701(1) 0.021(3) Uani 1.00 d . . . C(45) C 0.5004(6) -0.3622(8) 0.800(1) 0.027(3) Uani 1.00 d . . . C(46) C 0.4959(7) -0.4907(8) 0.697(2) 0.033(3) Uani 1.00 d . . . H(1) H 0.3817 -0.3784 0.4940 0.0244 Uiso 1.00 calc . . . H(2) H 0.4688 -0.4893 0.4704 0.0304 Uiso 1.00 calc . . . H(3) H 0.4239 -0.5609 0.5145 0.0304 Uiso 1.00 calc . . . H(4) H 0.3772 -0.4659 0.3652 0.0333 Uiso 1.00 calc . . . H(5) H 0.3324 -0.5375 0.4094 0.0333 Uiso 1.00 calc . . . H(6) H 0.2123 -0.6200 0.5303 0.0287 Uiso 1.00 calc . . . H(7) H 0.2167 -0.4742 0.4131 0.0395 Uiso 1.00 calc . . . H(8) H 0.1904 -0.5686 0.3905 0.0395 Uiso 1.00 calc . . . H(9) H 0.1017 -0.5568 0.5007 0.0480 Uiso 1.00 calc . . . H(10) H 0.1280 -0.4624 0.5233 0.0480 Uiso 1.00 calc . . . H(11) H 0.0948 -0.7795 0.6421 0.0202 Uiso 1.00 calc . . . H(12) H -0.0027 -0.5432 0.6564 0.0150 Uiso 1.00 calc . . . H(13) H 0.2760 -0.7428 0.6419 0.0252 Uiso 1.00 calc . . . H(14) H 0.2914 -0.6774 0.7153 0.0252 Uiso 1.00 calc . . . H(15) H 0.3091 -0.7775 0.7247 0.0252 Uiso 1.00 calc . . . H(16) H 0.2187 -0.6924 0.8540 0.0212 Uiso 1.00 calc . . . H(17) H 0.2422 -0.7910 0.8554 0.0212 Uiso 1.00 calc . . . H(18) H 0.1643 -0.7678 0.8580 0.0212 Uiso 1.00 calc . . . H(19) H 0.2200 -0.8893 0.7356 0.0331 Uiso 1.00 calc . . . H(20) H 0.1425 -0.8641 0.7339 0.0331 Uiso 1.00 calc . . . H(21) H 0.1868 -0.8543 0.6529 0.0331 Uiso 1.00 calc . . . H(22) H -0.0168 -0.8264 0.6382 0.0281 Uiso 1.00 calc . . . H(23) H -0.0713 -0.7634 0.6776 0.0281 Uiso 1.00 calc . . . H(24) H -0.0853 -0.8077 0.5909 0.0281 Uiso 1.00 calc . . . H(25) H -0.0961 -0.6170 0.6153 0.0292 Uiso 1.00 calc . . . H(26) H -0.1098 -0.6620 0.5288 0.0292 Uiso 1.00 calc . . . H(27) H -0.0571 -0.5847 0.5355 0.0292 Uiso 1.00 calc . . . H(28) H -0.0247 -0.7604 0.4624 0.0374 Uiso 1.00 calc . . . H(29) H 0.0334 -0.6896 0.4665 0.0374 Uiso 1.00 calc . . . H(30) H 0.0448 -0.7829 0.5058 0.0374 Uiso 1.00 calc . . . H(31) H -0.0188 -0.4261 0.7001 0.0369 Uiso 1.00 calc . . . H(32) H -0.0243 -0.4675 0.7896 0.0369 Uiso 1.00 calc . . . H(33) H -0.0082 -0.3670 0.7793 0.0369 Uiso 1.00 calc . . . H(34) H 0.0768 -0.4831 0.8812 0.0407 Uiso 1.00 calc . . . H(35) H 0.0927 -0.3827 0.8702 0.0407 Uiso 1.00 calc . . . H(36) H 0.1494 -0.4528 0.8522 0.0407 Uiso 1.00 calc . . . H(37) H 0.1041 -0.3169 0.7235 0.0570 Uiso 1.00 calc . . . H(38) H 0.1606 -0.3844 0.6971 0.0570 Uiso 1.00 calc . . . H(39) H 0.0937 -0.3757 0.6441 0.0570 Uiso 1.00 calc . . . H(40) H 0.4220 -0.1595 0.4901 0.0202 Uiso 1.00 calc . . . H(41) H 0.5637 -0.3383 0.5647 0.0162 Uiso 1.00 calc . . . H(42) H 0.2630 -0.2423 0.5277 0.0309 Uiso 1.00 calc . . . H(43) H 0.2576 -0.2747 0.6204 0.0309 Uiso 1.00 calc . . . H(44) H 0.2199 -0.1887 0.5926 0.0309 Uiso 1.00 calc . . . H(45) H 0.3184 -0.1811 0.7380 0.0285 Uiso 1.00 calc . . . H(46) H 0.2778 -0.0993 0.7053 0.0285 Uiso 1.00 calc . . . H(47) H 0.3575 -0.0955 0.7119 0.0285 Uiso 1.00 calc . . . H(48) H 0.2847 -0.0548 0.5578 0.0282 Uiso 1.00 calc . . . H(49) H 0.3645 -0.0521 0.5619 0.0282 Uiso 1.00 calc . . . H(50) H 0.3279 -0.1080 0.4928 0.0282 Uiso 1.00 calc . . . H(51) H 0.4674 -0.1528 0.3749 0.0320 Uiso 1.00 calc . . . H(52) H 0.5285 -0.1046 0.4184 0.0320 Uiso 1.00 calc . . . H(53) H 0.5390 -0.1501 0.3314 0.0320 Uiso 1.00 calc . . . H(54) H 0.6272 -0.1904 0.4778 0.0298 Uiso 1.00 calc . . . H(55) H 0.6383 -0.2357 0.3908 0.0298 Uiso 1.00 calc . . . H(56) H 0.6279 -0.2933 0.4710 0.0298 Uiso 1.00 calc . . . H(57) H 0.5408 -0.3144 0.3182 0.0362 Uiso 1.00 calc . . . H(58) H 0.5319 -0.3737 0.3976 0.0362 Uiso 1.00 calc . . . H(59) H 0.4693 -0.3220 0.3615 0.0362 Uiso 1.00 calc . . . H(60) H 0.6073 -0.4117 0.6466 0.0269 Uiso 1.00 calc . . . H(61) H 0.6119 -0.3326 0.7092 0.0269 Uiso 1.00 calc . . . H(62) H 0.6162 -0.4295 0.7424 0.0269 Uiso 1.00 calc . . . H(63) H 0.5181 -0.3021 0.8079 0.0316 Uiso 1.00 calc . . . H(64) H 0.5229 -0.3990 0.8410 0.0316 Uiso 1.00 calc . . . H(65) H 0.4528 -0.3614 0.8105 0.0316 Uiso 1.00 calc . . . H(66) H 0.5175 -0.5275 0.7389 0.0377 Uiso 1.00 calc . . . H(67) H 0.4467 -0.4964 0.7042 0.0377 Uiso 1.00 calc . . . H(68) H 0.5085 -0.5092 0.6432 0.0377 Uiso 1.00 calc . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Au(1) 0.0162(1) 0.0199(2) 0.0110(2) -0.0051(2) -0.0016(2) 0.0004(2) Au(2) 0.0320(2) 0.0211(2) 0.0151(2) -0.0122(2) 0.0125(2) -0.0083(2) Cl(1) 0.031(1) 0.035(2) 0.021(1) -0.002(1) -0.015(1) -0.001(1) Cl(2) 0.089(3) 0.048(2) 0.046(2) -0.033(2) 0.057(2) -0.036(2) P(1) 0.015(1) 0.017(1) 0.008(1) -0.007(1) -0.0011(9) 0.000(1) P(2) 0.017(1) 0.016(1) 0.007(1) -0.005(1) 0.0049(9) -0.003(1) C(1) 0.018(4) 0.012(4) 0.008(3) -0.006(3) 0.002(3) -0.001(3) C(2) 0.013(4) 0.019(4) 0.012(4) -0.007(3) -0.001(4) 0.000(3) C(3) 0.021(4) 0.005(4) 0.014(4) 0.002(3) 0.001(4) -0.005(4) C(4) 0.024(5) 0.018(5) 0.008(4) -0.001(4) 0.005(4) -0.001(4) C(5) 0.029(5) 0.020(5) 0.010(5) 0.005(4) 0.004(4) 0.001(4) C(6) 0.031(5) 0.023(6) 0.019(6) 0.007(4) 0.004(4) -0.006(5) C(7) 0.030(5) 0.036(7) 0.015(5) -0.002(5) 0.005(4) -0.012(5) C(8) 0.035(5) 0.022(5) 0.017(5) -0.009(4) -0.008(5) -0.006(4) C(9) 0.042(7) 0.038(7) 0.019(5) -0.016(6) -0.002(4) 0.007(5) C(10) 0.028(5) 0.061(9) 0.024(6) -0.011(6) -0.010(4) -0.005(7) C(11) 0.018(3) 0.011(4) 0.002(4) -0.005(3) -0.006(4) 0.002(4) C(12) 0.006(4) 0.013(4) 0.023(6) -0.004(3) 0.010(3) 0.000(4) C(13) 0.015(5) 0.013(5) 0.022(6) 0.004(4) -0.001(4) -0.006(4) C(14) 0.011(4) 0.017(4) 0.006(4) -0.001(3) 0.002(3) 0.000(4) C(15) 0.013(4) 0.014(4) 0.011(5) 0.000(4) -0.004(4) 0.003(4) C(16) 0.016(4) 0.010(4) 0.012(5) -0.003(3) -0.001(4) 0.000(4) C(17) 0.014(4) 0.016(4) 0.018(4) -0.005(4) -0.004(4) 0.006(4) C(18) 0.018(4) 0.023(6) 0.020(6) 0.001(4) 0.005(4) -0.009(5) C(19) 0.020(5) 0.011(4) 0.019(4) -0.010(4) -0.005(5) 0.003(5) C(20) 0.025(5) 0.019(4) 0.036(7) 0.009(5) -0.006(5) -0.014(5) C(21) 0.015(4) 0.023(5) 0.011(4) -0.002(3) -0.004(3) -0.002(4) C(22) 0.015(5) 0.018(5) 0.036(7) -0.012(4) -0.008(5) 0.000(5) C(23) 0.021(5) 0.029(6) 0.025(6) 0.008(4) -0.010(5) 0.002(5) C(24) 0.029(6) 0.044(8) 0.016(6) 0.001(6) 0.011(5) -0.011(5) C(25) 0.018(4) 0.012(4) 0.025(5) -0.006(4) -0.006(4) -0.011(4) C(26) 0.020(4) 0.032(7) 0.037(8) 0.004(5) -0.003(5) -0.014(6) C(27) 0.023(5) 0.049(7) 0.025(5) 0.011(5) -0.002(5) -0.021(7) C(28) 0.066(10) 0.013(5) 0.053(10) 0.004(6) 0.039(8) 0.011(6) C(29) 0.014(4) 0.014(4) 0.004(4) -0.007(3) 0.000(3) -0.004(3) C(30) 0.015(4) 0.014(5) 0.012(5) -0.001(4) 0.000(3) 0.002(4) C(31) 0.014(4) 0.019(5) 0.014(5) -0.001(4) 0.002(4) 0.004(4) C(32) 0.016(4) 0.016(4) 0.007(4) 0.003(4) -0.001(3) 0.001(4) C(33) 0.015(5) 0.021(5) 0.009(4) -0.002(4) -0.001(4) 0.006(4) C(34) 0.018(4) 0.011(5) 0.010(4) -0.001(4) 0.003(3) 0.001(4) C(35) 0.013(4) 0.020(5) 0.022(5) -0.001(3) -0.002(4) 0.002(4) C(36) 0.013(5) 0.029(6) 0.032(7) -0.001(4) -0.005(5) 0.002(6) C(37) 0.020(5) 0.022(5) 0.027(5) 0.010(5) 0.004(5) -0.008(5) C(38) 0.019(5) 0.020(5) 0.024(6) 0.007(5) 0.003(5) 0.005(4) C(39) 0.015(4) 0.030(5) 0.010(5) 0.008(4) 0.003(4) 0.009(4) C(40) 0.024(5) 0.032(6) 0.024(6) 0.005(4) 0.003(6) 0.021(5) C(41) 0.011(3) 0.034(6) 0.027(7) 0.009(5) 0.016(4) 0.012(5) C(42) 0.038(6) 0.040(6) 0.014(6) -0.003(5) 0.002(5) -0.005(5) C(43) 0.026(4) 0.015(4) 0.012(4) 0.000(4) 0.000(4) 0.007(4) C(44) 0.026(4) 0.018(5) 0.020(6) -0.005(5) -0.009(5) 0.005(5) C(45) 0.029(6) 0.037(7) 0.013(5) 0.015(5) -0.001(5) -0.002(5) C(46) 0.038(6) 0.013(4) 0.049(9) -0.002(5) -0.016(7) 0.005(6) #------------------------------------------------------------------------------ _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction 'teXsan Ver. 1.10' _computing_structure_solution 'DIRDIF94 (PATTY)' _computing_structure_refinement 'teXsan Ver. 1.10' _computing_publication_material 'teXsan Ver. 1.10' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Au(1) Au(2) 3.0096(5) . . yes Au(1) Cl(1) 2.293(3) . . yes Au(1) P(1) 2.223(3) . . yes Au(2) Cl(2) 2.280(3) . . yes Au(2) P(2) 2.220(3) . . yes P(1) C(1) 1.662(9) . . yes P(1) C(11) 1.834(9) . . yes P(2) C(2) 1.670(9) . . yes P(2) C(29) 1.816(9) . . yes C(1) C(2) 1.49(1) . . yes C(1) C(4) 1.48(1) . . yes C(2) C(3) 1.48(1) . . yes C(3) C(4) 1.40(1) . . yes C(3) C(5) 1.46(1) . . yes C(4) C(8) 1.47(1) . . yes C(5) C(6) 1.51(1) . . yes C(5) C(7) 1.52(1) . . yes C(6) C(7) 1.49(2) . . yes C(8) C(9) 1.51(2) . . yes C(8) C(10) 1.51(2) . . yes C(9) C(10) 1.49(2) . . yes C(11) C(12) 1.43(1) . . yes C(11) C(16) 1.42(1) . . yes C(12) C(13) 1.38(1) . . yes C(12) C(17) 1.55(1) . . yes C(13) C(14) 1.40(1) . . yes C(14) C(15) 1.38(1) . . yes C(14) C(21) 1.53(1) . . yes C(15) C(16) 1.40(1) . . yes C(16) C(25) 1.56(1) . . yes C(17) C(18) 1.53(1) . . yes C(17) C(19) 1.54(1) . . yes C(17) C(20) 1.53(1) . . yes C(21) C(22) 1.54(1) . . yes C(21) C(23) 1.52(1) . . yes C(21) C(24) 1.54(1) . . yes C(25) C(26) 1.56(1) . . yes C(25) C(27) 1.55(2) . . yes C(25) C(28) 1.54(1) . . yes C(29) C(30) 1.41(1) . . yes C(29) C(34) 1.45(1) . . yes C(30) C(31) 1.42(1) . . yes C(30) C(35) 1.56(1) . . yes C(31) C(32) 1.39(1) . . yes C(32) C(33) 1.40(1) . . yes C(32) C(39) 1.53(1) . . yes C(33) C(34) 1.39(1) . . yes C(34) C(43) 1.55(1) . . yes C(35) C(36) 1.56(1) . . yes C(35) C(37) 1.55(1) . . yes C(35) C(38) 1.52(1) . . yes C(39) C(40) 1.51(1) . . yes C(39) C(41) 1.54(1) . . yes C(39) C(42) 1.55(1) . . yes C(43) C(44) 1.53(1) . . yes C(43) C(45) 1.53(1) . . yes C(43) C(46) 1.53(1) . . yes #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Au(2) Au(1) Cl(1) 89.64(7) . 1_555 1_555 yes Au(2) Au(1) P(1) 91.27(6) . 1_555 1_555 yes Cl(1) Au(1) P(1) 174.7(1) . 1_555 1_555 yes Au(1) Au(2) Cl(2) 94.58(9) . 1_555 1_555 yes Au(1) Au(2) P(2) 89.43(6) . 1_555 1_555 yes Cl(2) Au(2) P(2) 174.1(1) . 1_555 1_555 yes Au(1) P(1) C(1) 116.1(3) . 1_555 1_555 yes Au(1) P(1) C(11) 136.7(3) . 1_555 1_555 yes C(1) P(1) C(11) 107.0(4) . 1_555 1_555 yes Au(2) P(2) C(2) 119.3(3) . 1_555 1_555 yes Au(2) P(2) C(29) 133.7(3) . 1_555 1_555 yes C(2) P(2) C(29) 105.5(4) . 1_555 1_555 yes P(1) C(1) C(2) 131.1(7) . 1_555 1_555 yes P(1) C(1) C(4) 140.6(7) . 1_555 1_555 yes C(2) C(1) C(4) 87.7(7) . 1_555 1_555 yes P(2) C(2) C(1) 131.7(7) . 1_555 1_555 yes P(2) C(2) C(3) 138.9(7) . 1_555 1_555 yes C(1) C(2) C(3) 88.1(7) . 1_555 1_555 yes C(2) C(3) C(4) 91.4(7) . 1_555 1_555 yes C(2) C(3) C(5) 130.6(8) . 1_555 1_555 yes C(4) C(3) C(5) 138.0(9) . 1_555 1_555 yes C(1) C(4) C(3) 91.7(8) . 1_555 1_555 yes C(1) C(4) C(8) 132.8(9) . 1_555 1_555 yes C(3) C(4) C(8) 135.4(9) . 1_555 1_555 yes C(3) C(5) C(6) 117.5(8) . 1_555 1_555 yes C(3) C(5) C(7) 121.2(9) . 1_555 1_555 yes C(6) C(5) C(7) 59.0(7) . 1_555 1_555 yes C(5) C(6) C(7) 60.8(7) . 1_555 1_555 yes C(5) C(7) C(6) 60.2(7) . 1_555 1_555 yes C(4) C(8) C(9) 121.5(9) . 1_555 1_555 yes C(4) C(8) C(10) 120.2(9) . 1_555 1_555 yes C(9) C(8) C(10) 59.2(8) . 1_555 1_555 yes C(8) C(9) C(10) 60.4(8) . 1_555 1_555 yes C(8) C(10) C(9) 60.4(8) . 1_555 1_555 yes P(1) C(11) C(12) 121.6(7) . 1_555 1_555 yes P(1) C(11) C(16) 116.1(6) . 1_555 1_555 yes C(12) C(11) C(16) 121.4(8) . 1_555 1_555 yes C(11) C(12) C(13) 117.4(8) . 1_555 1_555 yes C(11) C(12) C(17) 123.9(8) . 1_555 1_555 yes C(13) C(12) C(17) 118.6(8) . 1_555 1_555 yes C(12) C(13) C(14) 122.4(9) . 1_555 1_555 yes C(13) C(14) C(15) 118.5(8) . 1_555 1_555 yes C(13) C(14) C(21) 119.6(8) . 1_555 1_555 yes C(15) C(14) C(21) 121.8(8) . 1_555 1_555 yes C(14) C(15) C(16) 122.6(8) . 1_555 1_555 yes C(11) C(16) C(15) 116.5(8) . 1_555 1_555 yes C(11) C(16) C(25) 126.3(8) . 1_555 1_555 yes C(15) C(16) C(25) 117.2(8) . 1_555 1_555 yes C(12) C(17) C(18) 113.7(8) . 1_555 1_555 yes C(12) C(17) C(19) 108.1(8) . 1_555 1_555 yes C(12) C(17) C(20) 111.8(7) . 1_555 1_555 yes C(18) C(17) C(19) 109.8(8) . 1_555 1_555 yes C(18) C(17) C(20) 105.7(8) . 1_555 1_555 yes C(19) C(17) C(20) 107.7(8) . 1_555 1_555 yes C(14) C(21) C(22) 109.5(8) . 1_555 1_555 yes C(14) C(21) C(23) 112.9(8) . 1_555 1_555 yes C(14) C(21) C(24) 110.4(8) . 1_555 1_555 yes C(22) C(21) C(23) 107.2(8) . 1_555 1_555 yes C(22) C(21) C(24) 108.0(8) . 1_555 1_555 yes C(23) C(21) C(24) 108.7(9) . 1_555 1_555 yes C(16) C(25) C(26) 110.4(7) . 1_555 1_555 yes C(16) C(25) C(27) 110.8(8) . 1_555 1_555 yes C(16) C(25) C(28) 111.4(8) . 1_555 1_555 yes C(26) C(25) C(27) 105.3(8) . 1_555 1_555 yes C(26) C(25) C(28) 106.5(9) . 1_555 1_555 yes C(27) C(25) C(28) 112.1(9) . 1_555 1_555 yes P(2) C(29) C(30) 120.2(7) . 1_555 1_555 yes P(2) C(29) C(34) 117.4(6) . 1_555 1_555 yes C(30) C(29) C(34) 121.3(8) . 1_555 1_555 yes C(29) C(30) C(31) 116.6(9) . 1_555 1_555 yes C(29) C(30) C(35) 126.6(9) . 1_555 1_555 yes C(31) C(30) C(35) 116.8(8) . 1_555 1_555 yes C(30) C(31) C(32) 123.4(9) . 1_555 1_555 yes C(31) C(32) C(33) 117.1(9) . 1_555 1_555 yes C(31) C(32) C(39) 122.0(8) . 1_555 1_555 yes C(33) C(32) C(39) 120.7(8) . 1_555 1_555 yes C(32) C(33) C(34) 123.7(8) . 1_555 1_555 yes C(29) C(34) C(33) 116.6(8) . 1_555 1_555 yes C(29) C(34) C(43) 124.7(8) . 1_555 1_555 yes C(33) C(34) C(43) 118.7(8) . 1_555 1_555 yes C(30) C(35) C(36) 110.8(8) . 1_555 1_555 yes C(30) C(35) C(37) 110.6(8) . 1_555 1_555 yes C(30) C(35) C(38) 112.4(8) . 1_555 1_555 yes C(36) C(35) C(37) 109.3(8) . 1_555 1_555 yes C(36) C(35) C(38) 106.8(8) . 1_555 1_555 yes C(37) C(35) C(38) 106.7(8) . 1_555 1_555 yes C(32) C(39) C(40) 111.8(8) . 1_555 1_555 yes C(32) C(39) C(41) 110.5(8) . 1_555 1_555 yes C(32) C(39) C(42) 107.7(8) . 1_555 1_555 yes C(40) C(39) C(41) 109.3(8) . 1_555 1_555 yes C(40) C(39) C(42) 109.8(9) . 1_555 1_555 yes C(41) C(39) C(42) 107.6(8) . 1_555 1_555 yes C(34) C(43) C(44) 109.9(8) . 1_555 1_555 yes C(34) C(43) C(45) 111.0(8) . 1_555 1_555 yes C(34) C(43) C(46) 111.3(8) . 1_555 1_555 yes C(44) C(43) C(45) 107.0(8) . 1_555 1_555 yes C(44) C(43) C(46) 105.8(9) . 1_555 1_555 yes C(45) C(43) C(46) 111.6(9) . 1_555 1_555 yes #------------------------------------------------------------------------------ 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 Au(1) Au(2) P(2) C(2) 44.6(4) 1_555 1_555 1_555 1_555 yes Au(1) Au(2) P(2) C(29) -151.9(4) 1_555 1_555 1_555 1_555 yes Au(1) P(1) C(1) C(2) -12(1) 1_555 1_555 1_555 1_555 yes Au(1) P(1) C(1) C(4) 155(1) 1_555 1_555 1_555 1_555 yes Au(1) P(1) C(11) C(12) -85.4(8) 1_555 1_555 1_555 1_555 yes Au(1) P(1) C(11) C(16) 105.6(7) 1_555 1_555 1_555 1_555 yes Au(2) Au(1) P(1) C(1) 50.8(4) 1_555 1_555 1_555 1_555 yes Au(2) Au(1) P(1) C(11) -134.6(4) 1_555 1_555 1_555 1_555 yes Au(2) P(2) C(2) C(1) -5(1) 1_555 1_555 1_555 1_555 yes Au(2) P(2) C(2) C(3) 157.3(9) 1_555 1_555 1_555 1_555 yes Au(2) P(2) C(29) C(30) -80.6(8) 1_555 1_555 1_555 1_555 yes Au(2) P(2) C(29) C(34) 111.2(6) 1_555 1_555 1_555 1_555 yes Cl(1) Au(1) Au(2) Cl(2) -68.2(2) 1_555 1_555 1_555 1_555 yes Cl(1) Au(1) Au(2) P(2) 116.10(10) 1_555 1_555 1_555 1_555 yes Cl(1) Au(1) P(1) C(1) -49(1) 1_555 1_555 1_555 1_555 yes Cl(1) Au(1) P(1) C(11) 125(1) 1_555 1_555 1_555 1_555 yes Cl(2) Au(2) Au(1) P(1) 117.0(1) 1_555 1_555 1_555 1_555 yes Cl(2) Au(2) P(2) C(2) -88(1) 1_555 1_555 1_555 1_555 yes Cl(2) Au(2) P(2) C(29) 75(1) 1_555 1_555 1_555 1_555 yes P(1) Au(1) Au(2) P(2) -58.67(10) 1_555 1_555 1_555 1_555 yes P(1) C(1) C(2) P(2) -26(1) 1_555 1_555 1_555 1_555 yes P(1) C(1) C(2) C(3) 165.3(8) 1_555 1_555 1_555 1_555 yes P(1) C(1) C(4) C(3) -163.5(10) 1_555 1_555 1_555 1_555 yes P(1) C(1) C(4) C(8) 13(1) 1_555 1_555 1_555 1_555 yes P(1) C(11) C(12) C(13) -158.0(7) 1_555 1_555 1_555 1_555 yes P(1) C(11) C(12) C(17) 26(1) 1_555 1_555 1_555 1_555 yes P(1) C(11) C(16) C(15) 158.3(7) 1_555 1_555 1_555 1_555 yes P(1) C(11) C(16) C(25) -22(1) 1_555 1_555 1_555 1_555 yes P(2) C(2) C(1) C(4) 160.9(9) 1_555 1_555 1_555 1_555 yes P(2) C(2) C(3) C(4) -158.9(10) 1_555 1_555 1_555 1_555 yes P(2) C(2) C(3) C(5) 23(1) 1_555 1_555 1_555 1_555 yes P(2) C(29) C(30) C(31) -157.9(7) 1_555 1_555 1_555 1_555 yes P(2) C(29) C(30) C(35) 22(1) 1_555 1_555 1_555 1_555 yes P(2) C(29) C(34) C(33) 156.3(7) 1_555 1_555 1_555 1_555 yes P(2) C(29) C(34) C(43) -24(1) 1_555 1_555 1_555 1_555 yes C(1) P(1) C(11) C(12) 89.5(8) 1_555 1_555 1_555 1_555 yes C(1) P(1) C(11) C(16) -79.5(8) 1_555 1_555 1_555 1_555 yes C(1) C(2) P(2) C(29) -172.8(9) 1_555 1_555 1_555 1_555 yes C(1) C(2) C(3) C(4) 8.1(8) 1_555 1_555 1_555 1_555 yes C(1) C(2) C(3) C(5) -169.5(10) 1_555 1_555 1_555 1_555 yes C(1) C(4) C(3) C(2) -8.1(7) 1_555 1_555 1_555 1_555 yes C(1) C(4) C(3) C(5) 169(1) 1_555 1_555 1_555 1_555 yes C(1) C(4) C(8) C(9) 149(1) 1_555 1_555 1_555 1_555 yes C(1) C(4) C(8) C(10) 78(1) 1_555 1_555 1_555 1_555 yes C(2) P(2) C(29) C(30) 84.5(8) 1_555 1_555 1_555 1_555 yes C(2) P(2) C(29) C(34) -83.7(7) 1_555 1_555 1_555 1_555 yes C(2) C(1) P(1) C(11) 171.0(8) 1_555 1_555 1_555 1_555 yes C(2) C(1) C(4) C(3) 8.1(7) 1_555 1_555 1_555 1_555 yes C(2) C(1) C(4) C(8) -175(1) 1_555 1_555 1_555 1_555 yes C(2) C(3) C(4) C(8) 175(1) 1_555 1_555 1_555 1_555 yes C(2) C(3) C(5) C(6) 94(1) 1_555 1_555 1_555 1_555 yes C(2) C(3) C(5) C(7) 162.9(9) 1_555 1_555 1_555 1_555 yes C(3) C(2) P(2) C(29) -10(1) 1_555 1_555 1_555 1_555 yes C(3) C(2) C(1) C(4) -7.6(7) 1_555 1_555 1_555 1_555 yes C(3) C(4) C(8) C(9) -35(1) 1_555 1_555 1_555 1_555 yes C(3) C(4) C(8) C(10) -105(1) 1_555 1_555 1_555 1_555 yes C(3) C(5) C(6) C(7) 111(1) 1_555 1_555 1_555 1_555 yes C(3) C(5) C(7) C(6) -105(1) 1_555 1_555 1_555 1_555 yes C(4) C(1) P(1) C(11) -20(1) 1_555 1_555 1_555 1_555 yes C(4) C(3) C(5) C(6) -82(1) 1_555 1_555 1_555 1_555 yes C(4) C(3) C(5) C(7) -13(1) 1_555 1_555 1_555 1_555 yes C(4) C(8) C(9) C(10) -108(1) 1_555 1_555 1_555 1_555 yes C(4) C(8) C(10) C(9) 110(1) 1_555 1_555 1_555 1_555 yes C(5) C(3) C(4) C(8) -7(2) 1_555 1_555 1_555 1_555 yes C(11) C(12) C(13) C(14) -2(1) 1_555 1_555 1_555 1_555 yes C(11) C(12) C(17) C(18) -67(1) 1_555 1_555 1_555 1_555 yes C(11) C(12) C(17) C(19) 54(1) 1_555 1_555 1_555 1_555 yes C(11) C(12) C(17) C(20) 172.5(9) 1_555 1_555 1_555 1_555 yes C(11) C(16) C(15) C(14) 2(1) 1_555 1_555 1_555 1_555 yes C(11) C(16) C(25) C(26) -158.6(10) 1_555 1_555 1_555 1_555 yes C(11) C(16) C(25) C(27) -42(1) 1_555 1_555 1_555 1_555 yes C(11) C(16) C(25) C(28) 83(1) 1_555 1_555 1_555 1_555 yes C(12) C(11) C(16) C(15) -10(1) 1_555 1_555 1_555 1_555 yes C(12) C(11) C(16) C(25) 168.0(9) 1_555 1_555 1_555 1_555 yes C(12) C(13) C(14) C(15) -5(1) 1_555 1_555 1_555 1_555 yes C(12) C(13) C(14) C(21) 178.2(9) 1_555 1_555 1_555 1_555 yes C(13) C(12) C(11) C(16) 10(1) 1_555 1_555 1_555 1_555 yes C(13) C(12) C(17) C(18) 116.3(10) 1_555 1_555 1_555 1_555 yes C(13) C(12) C(17) C(19) -121.6(9) 1_555 1_555 1_555 1_555 yes C(13) C(12) C(17) C(20) -3(1) 1_555 1_555 1_555 1_555 yes C(13) C(14) C(15) C(16) 5(1) 1_555 1_555 1_555 1_555 yes C(13) C(14) C(21) C(22) 59(1) 1_555 1_555 1_555 1_555 yes C(13) C(14) C(21) C(23) 178.9(9) 1_555 1_555 1_555 1_555 yes C(13) C(14) C(21) C(24) -59(1) 1_555 1_555 1_555 1_555 yes C(14) C(13) C(12) C(17) 174.0(9) 1_555 1_555 1_555 1_555 yes C(14) C(15) C(16) C(25) -176.0(8) 1_555 1_555 1_555 1_555 yes C(15) C(14) C(21) C(22) -116.6(10) 1_555 1_555 1_555 1_555 yes C(15) C(14) C(21) C(23) 2(1) 1_555 1_555 1_555 1_555 yes C(15) C(14) C(21) C(24) 124.6(9) 1_555 1_555 1_555 1_555 yes C(15) C(16) C(25) C(26) 20(1) 1_555 1_555 1_555 1_555 yes C(15) C(16) C(25) C(27) 136.4(9) 1_555 1_555 1_555 1_555 yes C(15) C(16) C(25) C(28) -97(1) 1_555 1_555 1_555 1_555 yes C(16) C(11) C(12) C(17) -165.4(9) 1_555 1_555 1_555 1_555 yes C(16) C(15) C(14) C(21) -178.7(9) 1_555 1_555 1_555 1_555 yes C(29) C(30) C(31) C(32) 0(1) 1_555 1_555 1_555 1_555 yes C(29) C(30) C(35) C(36) -73(1) 1_555 1_555 1_555 1_555 yes C(29) C(30) C(35) C(37) 48(1) 1_555 1_555 1_555 1_555 yes C(29) C(30) C(35) C(38) 167.5(9) 1_555 1_555 1_555 1_555 yes C(29) C(34) C(33) C(32) 3(1) 1_555 1_555 1_555 1_555 yes C(29) C(34) C(43) C(44) -157.6(8) 1_555 1_555 1_555 1_555 yes C(29) C(34) C(43) C(45) -39(1) 1_555 1_555 1_555 1_555 yes C(29) C(34) C(43) C(46) 85(1) 1_555 1_555 1_555 1_555 yes C(30) C(29) C(34) C(33) -11(1) 1_555 1_555 1_555 1_555 yes C(30) C(29) C(34) C(43) 167.0(9) 1_555 1_555 1_555 1_555 yes C(30) C(31) C(32) C(33) -7(1) 1_555 1_555 1_555 1_555 yes C(30) C(31) C(32) C(39) 168.8(9) 1_555 1_555 1_555 1_555 yes C(31) C(30) C(29) C(34) 9(1) 1_555 1_555 1_555 1_555 yes C(31) C(30) C(35) C(36) 107(1) 1_555 1_555 1_555 1_555 yes C(31) C(30) C(35) C(37) -131.2(9) 1_555 1_555 1_555 1_555 yes C(31) C(30) C(35) C(38) -11(1) 1_555 1_555 1_555 1_555 yes C(31) C(32) C(33) C(34) 5(1) 1_555 1_555 1_555 1_555 yes C(31) C(32) C(39) C(40) 21(1) 1_555 1_555 1_555 1_555 yes C(31) C(32) C(39) C(41) 143.3(9) 1_555 1_555 1_555 1_555 yes C(31) C(32) C(39) C(42) -99(1) 1_555 1_555 1_555 1_555 yes C(32) C(31) C(30) C(35) 179.5(9) 1_555 1_555 1_555 1_555 yes C(32) C(33) C(34) C(43) -174.9(9) 1_555 1_555 1_555 1_555 yes C(33) C(32) C(39) C(40) -162.6(9) 1_555 1_555 1_555 1_555 yes C(33) C(32) C(39) C(41) -40(1) 1_555 1_555 1_555 1_555 yes C(33) C(32) C(39) C(42) 76(1) 1_555 1_555 1_555 1_555 yes C(33) C(34) C(43) C(44) 21(1) 1_555 1_555 1_555 1_555 yes C(33) C(34) C(43) C(45) 139.3(9) 1_555 1_555 1_555 1_555 yes C(33) C(34) C(43) C(46) -95(1) 1_555 1_555 1_555 1_555 yes C(34) C(29) C(30) C(35) -169.6(9) 1_555 1_555 1_555 1_555 yes C(34) C(33) C(32) C(39) -170.9(9) 1_555 1_555 1_555 1_555 yes