#------------------------------------------------------------------------------ #$Date: 2020-10-06 12:02:34 +0300 (Tue, 06 Oct 2020) $ #$Revision: 257564 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/52/7705203.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_7705203 loop_ _publ_author_name 'Siewert, Jan-Erik' 'Schumann, Andr\'e' 'Fischer, Malte' 'Schmidt, Christoph' 'Taeufer, Tobias' 'Hering-Junghans, Christian' _publ_section_title ; Terphenyl(bisamino)phosphines: electron-rich ligands for gold-catalysis. ; _journal_issue 35 _journal_name_full 'Dalton transactions (Cambridge, England : 2003)' _journal_page_first 12354 _journal_page_last 12364 _journal_paper_doi 10.1039/d0dt02435j _journal_volume 49 _journal_year 2020 _chemical_formula_moiety 'C32 H45 Au Cl P N2' _chemical_formula_sum 'C32 H45 Au Cl N2 P' _chemical_formula_weight 721.08 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' _space_group_name_H-M_alt 'P 1 21/n 1' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2014/7 _audit_update_record ; 2020-07-07 deposited with the CCDC. 2020-08-18 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90.233(2) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 8.7135(7) _cell_length_b 25.580(2) _cell_length_c 13.8947(11) _cell_measurement_reflns_used 9374 _cell_measurement_temperature 150(2) _cell_measurement_theta_max 30.44 _cell_measurement_theta_min 2.47 _cell_volume 3097.0(4) _computing_cell_refinement 'SAINT (Bruker, 2013)' _computing_data_collection 'APEX2 (Bruker, 2014)' _computing_data_reduction SAINT _computing_molecular_graphics 'ORTEP-3v2.01 (Farrugia, 1997)' _computing_publication_material 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _diffrn_ambient_temperature 150(2) _diffrn_detector_area_resol_mean 8.333 _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0317 _diffrn_reflns_av_unetI/netI 0.0141 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 1.000 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_number 88092 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 1.000 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.499 _diffrn_reflns_theta_min 1.592 _diffrn_source 'fine-focus sealed tube' _exptl_absorpt_coefficient_mu 4.911 _exptl_absorpt_correction_T_max 0.68 _exptl_absorpt_correction_T_min 0.49 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details 'SADABS (Bruker, 2014)' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.546 _exptl_crystal_description prism _exptl_crystal_F_000 1448 _exptl_crystal_size_max 0.360 _exptl_crystal_size_mid 0.176 _exptl_crystal_size_min 0.086 _refine_diff_density_max 1.254 _refine_diff_density_min -0.609 _refine_diff_density_rms 0.071 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 344 _refine_ls_number_reflns 7114 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.049 _refine_ls_R_factor_all 0.0219 _refine_ls_R_factor_gt 0.0180 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0194P)^2^+2.6797P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0412 _refine_ls_wR_factor_ref 0.0427 _reflns_Friedel_coverage 0.000 _reflns_number_gt 6387 _reflns_number_total 7114 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d0dt02435j2.cif _cod_data_source_block ax1345_num_TerPNEt22_AuCl_cmp2b _cod_depositor_comments 'Adding full bibliography for 7705201--7705209.cif.' _cod_original_sg_symbol_H-M 'P 21/n' _cod_database_code 7705203 _shelx_shelxl_version_number 2014/7 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_min 0.271 _shelx_estimated_absorpt_t_max 0.677 _shelx_res_file ; ax1345_num.res created by SHELXL-2014/7 TITL shelxt_a.res in P2(1)/n CELL 0.71073 8.7135 25.5805 13.8947 90.000 90.233 90.000 ZERR 4.00 0.0007 0.0021 0.0011 0.000 0.002 0.000 LATT 1 SYMM 1/2 - X, 1/2 + Y, 1/2 - Z SFAC C H N P CL AU UNIT 128 180 8 4 4 4 MERG 2 OMIT -3.00 55.00 FMAP 2 PLAN 20 SIZE 0.086 0.176 0.360 BOND $H CONF ACTA LIST 4 L.S. 8 TEMP -123.14 WGHT 0.019400 2.679700 FVAR 0.06306 C1 1 0.526577 0.667949 0.253997 11.00000 0.01515 0.01747 = 0.01643 0.00102 -0.00311 -0.00136 C2 1 0.565667 0.688387 0.162632 11.00000 0.01641 0.01910 = 0.01877 0.00101 -0.00235 -0.00174 C3 1 0.514568 0.738276 0.136281 11.00000 0.02753 0.02229 = 0.01909 0.00500 -0.00192 -0.00086 AFIX 43 H3 2 0.540657 0.751414 0.074526 11.00000 -1.20000 AFIX 0 C4 1 0.427860 0.769006 0.196610 11.00000 0.03242 0.01980 = 0.02613 0.00415 -0.00549 0.00566 AFIX 43 H4 2 0.391327 0.802206 0.176175 11.00000 -1.20000 AFIX 0 C5 1 0.395314 0.750354 0.287598 11.00000 0.02736 0.02081 = 0.02315 -0.00308 -0.00060 0.00598 AFIX 43 H5 2 0.337875 0.771595 0.330439 11.00000 -1.20000 AFIX 0 C6 1 0.444594 0.701095 0.318310 11.00000 0.01745 0.02001 = 0.01790 -0.00106 -0.00147 -0.00027 C7A 1 0.667527 0.663691 0.088230 11.00000 0.02171 0.01896 = 0.01847 0.00390 0.00175 0.00131 C8A 1 0.827460 0.665349 0.101275 11.00000 0.02401 0.02422 = 0.02384 0.00897 0.00157 -0.00033 C9A 1 0.920857 0.646478 0.027696 11.00000 0.02136 0.03364 = 0.03427 0.01200 0.00656 0.00244 AFIX 43 H9A 2 1.028999 0.646851 0.036641 11.00000 -1.20000 AFIX 0 C10A 1 0.861559 0.627200 -0.058012 11.00000 0.03786 0.03003 = 0.02661 0.00872 0.01258 0.00621 C11A 1 0.703412 0.627757 -0.070644 11.00000 0.03742 0.02813 = 0.01813 0.00199 0.00235 0.00474 AFIX 43 H11A 2 0.661008 0.615428 -0.129508 11.00000 -1.20000 AFIX 0 C12A 1 0.605292 0.645973 0.000966 11.00000 0.02640 0.02291 = 0.01807 0.00370 0.00094 0.00329 C13A 1 0.897138 0.688911 0.190292 11.00000 0.02223 0.03474 = 0.03058 0.00611 -0.00476 -0.00439 AFIX 137 H13A 2 1.009280 0.687470 0.185888 11.00000 -1.50000 H13B 2 0.863390 0.669237 0.246905 11.00000 -1.50000 H13C 2 0.864212 0.725399 0.196168 11.00000 -1.50000 AFIX 0 C14A 1 0.966570 0.606719 -0.135649 11.00000 0.04604 0.05630 = 0.03882 0.00274 0.02089 0.01265 AFIX 137 H14A 2 1.049686 0.631812 -0.146558 11.00000 -1.50000 H14B 2 0.908039 0.601926 -0.195375 11.00000 -1.50000 H14C 2 1.010089 0.573135 -0.115363 11.00000 -1.50000 AFIX 0 C15A 1 0.434474 0.646105 -0.016971 11.00000 0.02951 0.03318 = 0.02158 -0.00265 -0.00518 0.00295 AFIX 137 H15A 2 0.380922 0.636591 0.042390 11.00000 -1.50000 H15B 2 0.409467 0.620737 -0.067506 11.00000 -1.50000 H15C 2 0.402035 0.681074 -0.037452 11.00000 -1.50000 AFIX 0 C16 1 0.417562 0.690149 0.423190 11.00000 0.02013 0.01862 = 0.01687 -0.00133 -0.00025 0.00526 C17 1 0.535498 0.702985 0.488659 11.00000 0.02236 0.01937 = 0.02208 -0.00289 -0.00084 0.00313 C18 1 0.514645 0.693142 0.585835 11.00000 0.03077 0.02837 = 0.01897 -0.00429 -0.00524 0.00636 AFIX 43 H18 2 0.594751 0.701393 0.629862 11.00000 -1.20000 AFIX 0 C19 1 0.379750 0.671555 0.620303 11.00000 0.03928 0.03010 = 0.01842 0.00101 0.00250 0.00956 C20 1 0.259948 0.663323 0.556478 11.00000 0.02717 0.02674 = 0.02672 -0.00053 0.00878 0.00269 AFIX 43 H20 2 0.164985 0.650381 0.579910 11.00000 -1.20000 AFIX 0 C21 1 0.275607 0.673612 0.458548 11.00000 0.02053 0.02244 = 0.02331 -0.00444 0.00163 0.00297 C22 1 0.680185 0.730371 0.455683 11.00000 0.02631 0.02867 = 0.02976 -0.00417 -0.00465 -0.00488 AFIX 137 H22A 2 0.655512 0.766303 0.436672 11.00000 -1.50000 H22B 2 0.723483 0.711619 0.400608 11.00000 -1.50000 H22C 2 0.755161 0.730907 0.508438 11.00000 -1.50000 AFIX 0 C23 1 0.362005 0.658773 0.726385 11.00000 0.05698 0.05995 = 0.02171 0.01122 0.00662 0.00737 AFIX 137 H23A 2 0.269435 0.675751 0.751200 11.00000 -1.50000 H23B 2 0.451938 0.671479 0.761922 11.00000 -1.50000 H23C 2 0.353187 0.620837 0.734504 11.00000 -1.50000 AFIX 0 C24 1 0.135544 0.669997 0.395097 11.00000 0.02024 0.04497 = 0.03047 -0.00843 0.00052 0.00112 AFIX 137 H24A 2 0.073066 0.640048 0.414922 11.00000 -1.50000 H24B 2 0.167230 0.665442 0.328026 11.00000 -1.50000 H24C 2 0.075161 0.702148 0.401039 11.00000 -1.50000 AFIX 0 C25 1 0.647878 0.546089 0.135309 11.00000 0.02194 0.02198 = 0.02150 -0.00186 0.00325 0.00222 AFIX 23 H25A 2 0.727452 0.553364 0.086451 11.00000 -1.20000 H25B 2 0.552678 0.563981 0.114390 11.00000 -1.20000 AFIX 0 C26 1 0.617876 0.487479 0.136886 11.00000 0.03889 0.02385 = 0.03676 -0.00559 -0.00555 0.00147 AFIX 137 H26A 2 0.715621 0.468754 0.142523 11.00000 -1.50000 H26B 2 0.565956 0.477102 0.077176 11.00000 -1.50000 H26C 2 0.552736 0.478843 0.191975 11.00000 -1.50000 AFIX 0 C27 1 0.858485 0.558942 0.254088 11.00000 0.01580 0.03275 = 0.02869 0.00581 0.00224 0.00383 AFIX 23 H27A 2 0.892954 0.587475 0.297188 11.00000 -1.20000 H27B 2 0.922098 0.560501 0.195284 11.00000 -1.20000 AFIX 0 C28 1 0.888697 0.507036 0.304095 11.00000 0.03186 0.03408 = 0.03342 0.00356 -0.00124 0.01341 AFIX 137 H28A 2 0.822962 0.504139 0.360908 11.00000 -1.50000 H28B 2 0.996629 0.505247 0.323928 11.00000 -1.50000 H28C 2 0.865965 0.478280 0.259668 11.00000 -1.50000 AFIX 0 C29 1 0.394998 0.524324 0.357636 11.00000 0.02827 0.01941 = 0.02602 0.00306 0.00302 -0.00492 AFIX 23 H29A 2 0.498183 0.510141 0.372312 11.00000 -1.20000 H29B 2 0.336415 0.496836 0.323340 11.00000 -1.20000 AFIX 0 C30 1 0.314776 0.536875 0.450875 11.00000 0.04995 0.02919 = 0.03002 0.00513 0.01304 -0.00808 AFIX 137 H30A 2 0.374824 0.562779 0.486835 11.00000 -1.50000 H30B 2 0.304847 0.504956 0.489354 11.00000 -1.50000 H30C 2 0.212562 0.551040 0.436982 11.00000 -1.50000 AFIX 0 C31 1 0.279774 0.581193 0.230795 11.00000 0.01442 0.03120 = 0.02434 -0.00248 -0.00063 -0.00150 AFIX 23 H31A 2 0.297855 0.615071 0.198312 11.00000 -1.20000 H31B 2 0.187685 0.585306 0.271599 11.00000 -1.20000 AFIX 0 C32 1 0.244743 0.540176 0.153828 11.00000 0.01994 0.04901 = 0.03557 -0.01323 -0.00280 -0.00449 AFIX 137 H32A 2 0.332892 0.536825 0.110685 11.00000 -1.50000 H32B 2 0.154270 0.550952 0.116691 11.00000 -1.50000 H32C 2 0.224601 0.506448 0.184747 11.00000 -1.50000 AFIX 0 N1 3 0.697480 0.568822 0.226725 11.00000 0.01462 0.02032 = 0.02189 0.00038 0.00132 0.00213 N2 3 0.411403 0.570205 0.293580 11.00000 0.01642 0.01982 = 0.01989 0.00201 0.00037 -0.00228 P1 4 0.578043 0.601608 0.298063 11.00000 0.01432 0.01384 = 0.01441 0.00174 -0.00040 -0.00008 CL1 5 0.824713 0.599561 0.587650 11.00000 0.04564 0.02521 = 0.02679 -0.00004 -0.01906 -0.00125 AU1 6 0.690802 0.602597 0.443576 11.00000 0.02417 0.01746 = 0.01899 0.00142 -0.00602 -0.00037 HKLF 4 REM shelxt_a.res in P2(1)/n REM R1 = 0.0180 for 6387 Fo > 4sig(Fo) and 0.0219 for all 7114 data REM 344 parameters refined using 0 restraints END WGHT 0.0192 2.7781 REM Highest difference peak 1.254, deepest hole -0.609, 1-sigma level 0.071 Q1 1 0.8067 0.6916 0.0569 11.00000 0.05 1.25 Q2 1 0.9230 0.6014 0.6710 11.00000 0.05 0.97 Q3 1 0.6616 0.6071 0.4964 11.00000 0.05 0.66 Q4 1 0.6961 0.5731 0.4365 11.00000 0.05 0.64 Q5 1 0.6921 0.6260 0.4086 11.00000 0.05 0.56 Q6 1 0.7550 0.6024 0.6136 11.00000 0.05 0.56 Q7 1 0.6869 0.6350 0.4270 11.00000 0.05 0.54 Q8 1 0.6953 0.6097 0.3822 11.00000 0.05 0.54 Q9 1 0.8414 0.6108 0.5777 11.00000 0.05 0.43 Q10 1 0.2590 0.6733 0.5030 11.00000 0.05 0.39 Q11 1 0.5873 0.6074 0.3606 11.00000 0.05 0.39 Q12 1 0.5465 0.7143 0.1600 11.00000 0.05 0.38 Q13 1 0.5481 0.6376 0.2737 11.00000 0.05 0.36 Q14 1 0.4227 0.6946 0.3703 11.00000 0.05 0.35 Q15 1 0.6235 0.6477 0.0543 11.00000 0.05 0.35 Q16 1 0.6122 0.6727 0.1221 11.00000 0.05 0.35 Q17 1 0.6000 0.7153 0.4672 11.00000 0.05 0.34 Q18 1 0.8586 0.6763 0.1428 11.00000 0.05 0.34 Q19 1 0.3423 0.6853 0.4449 11.00000 0.05 0.34 Q20 1 0.4604 0.7482 0.1737 11.00000 0.05 0.31 ; _shelx_res_checksum 51718 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' 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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.5266(2) 0.66795(8) 0.25400(14) 0.0164(4) Uani 1 1 d . . . . . C2 C 0.5657(2) 0.68839(8) 0.16263(14) 0.0181(4) Uani 1 1 d . . . . . C3 C 0.5146(3) 0.73828(8) 0.13628(15) 0.0230(4) Uani 1 1 d . . . . . H3 H 0.5407 0.7514 0.0745 0.028 Uiso 1 1 calc R U . . . C4 C 0.4279(3) 0.76901(9) 0.19661(16) 0.0261(5) Uani 1 1 d . . . . . H4 H 0.3913 0.8022 0.1762 0.031 Uiso 1 1 calc R U . . . C5 C 0.3953(3) 0.75035(8) 0.28760(15) 0.0238(4) Uani 1 1 d . . . . . H5 H 0.3379 0.7716 0.3304 0.029 Uiso 1 1 calc R U . . . C6 C 0.4446(2) 0.70110(8) 0.31831(14) 0.0185(4) Uani 1 1 d . . . . . C7A C 0.6675(2) 0.66369(8) 0.08823(14) 0.0197(4) Uani 1 1 d . . . . . C8A C 0.8275(3) 0.66535(9) 0.10128(16) 0.0240(4) Uani 1 1 d . . . . . C9A C 0.9209(3) 0.64648(9) 0.02770(17) 0.0297(5) Uani 1 1 d . . . . . H9A H 1.0290 0.6469 0.0366 0.036 Uiso 1 1 calc R U . . . C10A C 0.8616(3) 0.62720(10) -0.05801(17) 0.0315(5) Uani 1 1 d . . . . . C11A C 0.7034(3) 0.62776(9) -0.07064(15) 0.0279(5) Uani 1 1 d . . . . . H11A H 0.6610 0.6154 -0.1295 0.033 Uiso 1 1 calc R U . . . C12A C 0.6053(3) 0.64597(8) 0.00097(15) 0.0225(4) Uani 1 1 d . . . . . C13A C 0.8971(3) 0.68891(10) 0.19029(16) 0.0292(5) Uani 1 1 d . . . . . H13A H 1.0093 0.6875 0.1859 0.044 Uiso 1 1 calc R U . . . H13B H 0.8634 0.6692 0.2469 0.044 Uiso 1 1 calc R U . . . H13C H 0.8642 0.7254 0.1962 0.044 Uiso 1 1 calc R U . . . C14A C 0.9666(4) 0.60672(12) -0.1356(2) 0.0470(7) Uani 1 1 d . . . . . H14A H 1.0497 0.6318 -0.1466 0.070 Uiso 1 1 calc R U . . . H14B H 0.9080 0.6019 -0.1954 0.070 Uiso 1 1 calc R U . . . H14C H 1.0101 0.5731 -0.1154 0.070 Uiso 1 1 calc R U . . . C15A C 0.4345(3) 0.64610(9) -0.01697(16) 0.0281(5) Uani 1 1 d . . . . . H15A H 0.3809 0.6366 0.0424 0.042 Uiso 1 1 calc R U . . . H15B H 0.4095 0.6207 -0.0675 0.042 Uiso 1 1 calc R U . . . H15C H 0.4020 0.6811 -0.0375 0.042 Uiso 1 1 calc R U . . . C16 C 0.4176(2) 0.69015(8) 0.42319(14) 0.0185(4) Uani 1 1 d . . . . . C17 C 0.5355(2) 0.70299(8) 0.48866(15) 0.0213(4) Uani 1 1 d . . . . . C18 C 0.5146(3) 0.69314(9) 0.58584(15) 0.0261(5) Uani 1 1 d . . . . . H18 H 0.5948 0.7014 0.6299 0.031 Uiso 1 1 calc R U . . . C19 C 0.3798(3) 0.67155(9) 0.62030(16) 0.0293(5) Uani 1 1 d . . . . . C20 C 0.2599(3) 0.66332(9) 0.55648(16) 0.0269(5) Uani 1 1 d . . . . . H20 H 0.1650 0.6504 0.5799 0.032 Uiso 1 1 calc R U . . . C21 C 0.2756(2) 0.67361(8) 0.45855(15) 0.0221(4) Uani 1 1 d . . . . . C22 C 0.6802(3) 0.73037(9) 0.45568(16) 0.0283(5) Uani 1 1 d . . . . . H22A H 0.6555 0.7663 0.4367 0.042 Uiso 1 1 calc R U . . . H22B H 0.7235 0.7116 0.4006 0.042 Uiso 1 1 calc R U . . . H22C H 0.7552 0.7309 0.5084 0.042 Uiso 1 1 calc R U . . . C23 C 0.3620(4) 0.65877(13) 0.72638(18) 0.0462(7) Uani 1 1 d . . . . . H23A H 0.2694 0.6758 0.7512 0.069 Uiso 1 1 calc R U . . . H23B H 0.4519 0.6715 0.7619 0.069 Uiso 1 1 calc R U . . . H23C H 0.3532 0.6208 0.7345 0.069 Uiso 1 1 calc R U . . . C24 C 0.1355(3) 0.67000(11) 0.39510(18) 0.0319(5) Uani 1 1 d . . . . . H24A H 0.0731 0.6400 0.4149 0.048 Uiso 1 1 calc R U . . . H24B H 0.1672 0.6654 0.3280 0.048 Uiso 1 1 calc R U . . . H24C H 0.0752 0.7021 0.4010 0.048 Uiso 1 1 calc R U . . . C25 C 0.6479(2) 0.54609(8) 0.13531(15) 0.0218(4) Uani 1 1 d . . . . . H25A H 0.7275 0.5534 0.0865 0.026 Uiso 1 1 calc R U . . . H25B H 0.5527 0.5640 0.1144 0.026 Uiso 1 1 calc R U . . . C26 C 0.6179(3) 0.48748(9) 0.13689(18) 0.0332(5) Uani 1 1 d . . . . . H26A H 0.7156 0.4688 0.1425 0.050 Uiso 1 1 calc R U . . . H26B H 0.5660 0.4771 0.0772 0.050 Uiso 1 1 calc R U . . . H26C H 0.5527 0.4788 0.1920 0.050 Uiso 1 1 calc R U . . . C27 C 0.8585(2) 0.55894(9) 0.25409(17) 0.0257(5) Uani 1 1 d . . . . . H27A H 0.8930 0.5875 0.2972 0.031 Uiso 1 1 calc R U . . . H27B H 0.9221 0.5605 0.1953 0.031 Uiso 1 1 calc R U . . . C28 C 0.8887(3) 0.50704(10) 0.30410(18) 0.0331(5) Uani 1 1 d . . . . . H28A H 0.8230 0.5041 0.3609 0.050 Uiso 1 1 calc R U . . . H28B H 0.9966 0.5052 0.3239 0.050 Uiso 1 1 calc R U . . . H28C H 0.8660 0.4783 0.2597 0.050 Uiso 1 1 calc R U . . . C29 C 0.3950(3) 0.52432(8) 0.35764(15) 0.0246(5) Uani 1 1 d . . . . . H29A H 0.4982 0.5101 0.3723 0.029 Uiso 1 1 calc R U . . . H29B H 0.3364 0.4968 0.3233 0.029 Uiso 1 1 calc R U . . . C30 C 0.3148(3) 0.53688(10) 0.45087(18) 0.0364(6) Uani 1 1 d . . . . . H30A H 0.3748 0.5628 0.4868 0.055 Uiso 1 1 calc R U . . . H30B H 0.3048 0.5050 0.4894 0.055 Uiso 1 1 calc R U . . . H30C H 0.2126 0.5510 0.4370 0.055 Uiso 1 1 calc R U . . . C31 C 0.2798(2) 0.58119(9) 0.23079(15) 0.0233(4) Uani 1 1 d . . . . . H31A H 0.2979 0.6151 0.1983 0.028 Uiso 1 1 calc R U . . . H31B H 0.1877 0.5853 0.2716 0.028 Uiso 1 1 calc R U . . . C32 C 0.2447(3) 0.54018(11) 0.15383(18) 0.0348(6) Uani 1 1 d . . . . . H32A H 0.3329 0.5368 0.1107 0.052 Uiso 1 1 calc R U . . . H32B H 0.1543 0.5510 0.1167 0.052 Uiso 1 1 calc R U . . . H32C H 0.2246 0.5064 0.1847 0.052 Uiso 1 1 calc R U . . . N1 N 0.69748(19) 0.56882(7) 0.22673(12) 0.0189(3) Uani 1 1 d . . . . . N2 N 0.41140(19) 0.57021(7) 0.29358(12) 0.0187(3) Uani 1 1 d . . . . . P1 P 0.57804(6) 0.60161(2) 0.29806(3) 0.01419(9) Uani 1 1 d . . . . . Cl1 Cl 0.82471(7) 0.59956(2) 0.58765(4) 0.03260(13) Uani 1 1 d . . . . . Au1 Au 0.69080(2) 0.60260(2) 0.44358(2) 0.02022(3) Uani 1 1 d . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0152(9) 0.0175(9) 0.0164(9) 0.0010(7) -0.0031(7) -0.0014(7) C2 0.0164(9) 0.0191(10) 0.0188(9) 0.0010(8) -0.0023(7) -0.0017(8) C3 0.0275(11) 0.0223(11) 0.0191(10) 0.0050(8) -0.0019(8) -0.0009(9) C4 0.0324(12) 0.0198(10) 0.0261(11) 0.0042(8) -0.0055(9) 0.0057(9) C5 0.0274(11) 0.0208(11) 0.0232(10) -0.0031(8) -0.0006(8) 0.0060(9) C6 0.0174(10) 0.0200(10) 0.0179(9) -0.0011(8) -0.0015(7) -0.0003(8) C7A 0.0217(10) 0.0190(10) 0.0185(10) 0.0039(8) 0.0018(8) 0.0013(8) C8A 0.0240(11) 0.0242(11) 0.0238(11) 0.0090(9) 0.0016(9) -0.0003(9) C9A 0.0214(11) 0.0336(13) 0.0343(13) 0.0120(10) 0.0066(9) 0.0024(9) C10A 0.0379(14) 0.0300(13) 0.0266(12) 0.0087(10) 0.0126(10) 0.0062(10) C11A 0.0374(13) 0.0281(12) 0.0181(10) 0.0020(9) 0.0024(9) 0.0047(10) C12A 0.0264(11) 0.0229(11) 0.0181(10) 0.0037(8) 0.0009(8) 0.0033(9) C13A 0.0222(11) 0.0347(13) 0.0306(12) 0.0061(10) -0.0048(9) -0.0044(10) C14A 0.0460(17) 0.0563(19) 0.0388(15) 0.0027(13) 0.0209(13) 0.0126(14) C15A 0.0295(12) 0.0332(13) 0.0216(11) -0.0027(9) -0.0052(9) 0.0029(10) C16 0.0201(10) 0.0186(10) 0.0169(9) -0.0013(8) -0.0002(7) 0.0053(8) C17 0.0224(10) 0.0194(10) 0.0221(10) -0.0029(8) -0.0008(8) 0.0031(8) C18 0.0308(12) 0.0284(11) 0.0190(10) -0.0043(9) -0.0052(9) 0.0064(10) C19 0.0393(14) 0.0301(12) 0.0184(11) 0.0010(9) 0.0025(9) 0.0096(10) C20 0.0272(11) 0.0267(12) 0.0267(11) -0.0005(9) 0.0088(9) 0.0027(9) C21 0.0205(11) 0.0224(10) 0.0233(10) -0.0044(8) 0.0016(8) 0.0030(8) C22 0.0263(12) 0.0287(12) 0.0298(12) -0.0042(9) -0.0047(9) -0.0049(9) C23 0.0570(19) 0.0599(19) 0.0217(12) 0.0112(12) 0.0066(12) 0.0074(15) C24 0.0202(11) 0.0450(15) 0.0305(12) -0.0084(11) 0.0005(9) 0.0011(10) C25 0.0219(11) 0.0220(11) 0.0215(10) -0.0019(8) 0.0032(8) 0.0022(8) C26 0.0389(14) 0.0238(12) 0.0368(13) -0.0056(10) -0.0055(11) 0.0015(10) C27 0.0158(10) 0.0328(12) 0.0287(11) 0.0058(9) 0.0022(8) 0.0038(9) C28 0.0319(13) 0.0341(13) 0.0334(13) 0.0036(10) -0.0012(10) 0.0134(11) C29 0.0283(12) 0.0194(10) 0.0260(11) 0.0031(8) 0.0030(9) -0.0049(9) C30 0.0500(16) 0.0292(13) 0.0300(13) 0.0051(10) 0.0130(11) -0.0081(11) C31 0.0144(10) 0.0312(12) 0.0243(11) -0.0025(9) -0.0006(8) -0.0015(9) C32 0.0199(11) 0.0490(16) 0.0356(13) -0.0132(11) -0.0028(10) -0.0045(10) N1 0.0146(8) 0.0203(9) 0.0219(9) 0.0004(7) 0.0013(7) 0.0021(7) N2 0.0164(8) 0.0198(9) 0.0199(8) 0.0020(7) 0.0004(7) -0.0023(7) P1 0.0143(2) 0.0138(2) 0.0144(2) 0.00174(18) -0.00040(18) -0.00008(18) Cl1 0.0456(3) 0.0252(3) 0.0268(3) 0.0000(2) -0.0191(2) -0.0012(2) Au1 0.02417(5) 0.01746(4) 0.01899(4) 0.00142(3) -0.00602(3) -0.00037(3) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 C6 117.73(18) . . ? C2 C1 P1 125.03(15) . . ? C6 C1 P1 117.22(14) . . ? C3 C2 C1 119.59(19) . . ? C3 C2 C7A 113.02(18) . . ? C1 C2 C7A 127.29(18) . . ? C4 C3 C2 122.40(19) . . ? C4 C3 H3 118.8 . . ? C2 C3 H3 118.8 . . ? C3 C4 C5 118.4(2) . . ? C3 C4 H4 120.8 . . ? C5 C4 H4 120.8 . . ? C4 C5 C6 121.8(2) . . ? C4 C5 H5 119.1 . . ? C6 C5 H5 119.1 . . ? C5 C6 C1 119.93(19) . . ? C5 C6 C16 114.51(18) . . ? C1 C6 C16 125.28(18) . . ? C12A C7A C8A 120.1(2) . . ? C12A C7A C2 120.20(18) . . ? C8A C7A C2 119.09(18) . . ? C9A C8A C7A 118.4(2) . . ? C9A C8A C13A 120.5(2) . . ? C7A C8A C13A 121.0(2) . . ? C10A C9A C8A 122.4(2) . . ? C10A C9A H9A 118.8 . . ? C8A C9A H9A 118.8 . . ? C9A C10A C11A 118.1(2) . . ? C9A C10A C14A 120.8(2) . . ? C11A C10A C14A 121.1(2) . . ? C10A C11A C12A 121.6(2) . . ? C10A C11A H11A 119.2 . . ? C12A C11A H11A 119.2 . . ? C11A C12A C7A 119.3(2) . . ? C11A C12A C15A 119.4(2) . . ? C7A C12A C15A 121.36(19) . . ? C8A C13A H13A 109.5 . . ? C8A C13A H13B 109.5 . . ? H13A C13A H13B 109.5 . . ? C8A C13A H13C 109.5 . . ? H13A C13A H13C 109.5 . . ? H13B C13A H13C 109.5 . . ? C10A C14A H14A 109.5 . . ? C10A C14A H14B 109.5 . . ? H14A C14A H14B 109.5 . . ? C10A C14A H14C 109.5 . . ? H14A C14A H14C 109.5 . . ? H14B C14A H14C 109.5 . . ? C12A C15A H15A 109.5 . . ? C12A C15A H15B 109.5 . . ? H15A C15A H15B 109.5 . . ? C12A C15A H15C 109.5 . . ? H15A C15A H15C 109.5 . . ? H15B C15A H15C 109.5 . . ? C21 C16 C17 119.19(19) . . ? C21 C16 C6 122.63(18) . . ? C17 C16 C6 117.76(18) . . ? C18 C17 C16 119.2(2) . . ? C18 C17 C22 119.42(19) . . ? C16 C17 C22 121.22(19) . . ? C19 C18 C17 121.6(2) . . ? C19 C18 H18 119.2 . . ? C17 C18 H18 119.2 . . ? C20 C19 C18 118.6(2) . . ? C20 C19 C23 120.7(2) . . ? C18 C19 C23 120.7(2) . . ? C19 C20 C21 121.4(2) . . ? C19 C20 H20 119.3 . . ? C21 C20 H20 119.3 . . ? C20 C21 C16 119.4(2) . . ? C20 C21 C24 118.6(2) . . ? C16 C21 C24 121.9(2) . . ? C17 C22 H22A 109.5 . . ? C17 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C17 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C19 C23 H23A 109.5 . . ? C19 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C19 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C21 C24 H24A 109.5 . . ? C21 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C21 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N1 C25 C26 115.46(18) . . ? N1 C25 H25A 108.4 . . ? C26 C25 H25A 108.4 . . ? N1 C25 H25B 108.4 . . ? C26 C25 H25B 108.4 . . ? H25A C25 H25B 107.5 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? N1 C27 C28 115.49(19) . . ? N1 C27 H27A 108.4 . . ? C28 C27 H27A 108.4 . . ? N1 C27 H27B 108.4 . . ? C28 C27 H27B 108.4 . . ? H27A C27 H27B 107.5 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? N2 C29 C30 113.18(19) . . ? N2 C29 H29A 108.9 . . ? C30 C29 H29A 108.9 . . ? N2 C29 H29B 108.9 . . ? C30 C29 H29B 108.9 . . ? H29A C29 H29B 107.8 . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? N2 C31 C32 116.01(19) . . ? N2 C31 H31A 108.3 . . ? C32 C31 H31A 108.3 . . ? N2 C31 H31B 108.3 . . ? C32 C31 H31B 108.3 . . ? H31A C31 H31B 107.4 . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C25 N1 C27 115.72(17) . . ? C25 N1 P1 122.29(14) . . ? C27 N1 P1 121.93(14) . . ? C31 N2 C29 115.64(17) . . ? C31 N2 P1 127.72(14) . . ? C29 N2 P1 116.59(14) . . ? N2 P1 N1 106.40(9) . . ? N2 P1 C1 102.69(9) . . ? N1 P1 C1 114.46(9) . . ? N2 P1 Au1 114.76(6) . . ? N1 P1 Au1 105.62(6) . . ? C1 P1 Au1 113.00(6) . . ? P1 Au1 Cl1 174.96(2) . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.416(3) . ? C1 C6 1.426(3) . ? C1 P1 1.858(2) . ? C2 C3 1.400(3) . ? C2 C7A 1.504(3) . ? C3 C4 1.377(3) . ? C3 H3 0.9500 . ? C4 C5 1.382(3) . ? C4 H4 0.9500 . ? C5 C6 1.397(3) . ? C5 H5 0.9500 . ? C6 C16 1.503(3) . ? C7A C12A 1.402(3) . ? C7A C8A 1.405(3) . ? C8A C9A 1.395(3) . ? C8A C13A 1.502(3) . ? C9A C10A 1.387(4) . ? C9A H9A 0.9500 . ? C10A C11A 1.389(3) . ? C10A C14A 1.511(3) . ? C11A C12A 1.395(3) . ? C11A H11A 0.9500 . ? C12A C15A 1.508(3) . ? C13A H13A 0.9800 . ? C13A H13B 0.9800 . ? C13A H13C 0.9800 . ? C14A H14A 0.9800 . ? C14A H14B 0.9800 . ? C14A H14C 0.9800 . ? C15A H15A 0.9800 . ? C15A H15B 0.9800 . ? C15A H15C 0.9800 . ? C16 C21 1.398(3) . ? C16 C17 1.408(3) . ? C17 C18 1.386(3) . ? C17 C22 1.515(3) . ? C18 C19 1.386(3) . ? C18 H18 0.9500 . ? C19 C20 1.383(3) . ? C19 C23 1.518(3) . ? C20 C21 1.393(3) . ? C20 H20 0.9500 . ? C21 C24 1.506(3) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 N1 1.461(3) . ? C25 C26 1.522(3) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 N1 1.474(3) . ? C27 C28 1.521(3) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 N2 1.480(3) . ? C29 C30 1.509(3) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 N2 1.465(3) . ? C31 C32 1.528(3) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? N1 P1 1.6665(17) . ? N2 P1 1.6604(17) . ? P1 Au1 2.2445(5) . ? Cl1 Au1 2.3143(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 C6 C1 C2 C3 -4.2(3) . . . . ? P1 C1 C2 C3 177.34(15) . . . . ? C6 C1 C2 C7A 171.81(19) . . . . ? P1 C1 C2 C7A -6.6(3) . . . . ? C1 C2 C3 C4 0.6(3) . . . . ? C7A C2 C3 C4 -175.9(2) . . . . ? C2 C3 C4 C5 2.4(3) . . . . ? C3 C4 C5 C6 -1.6(3) . . . . ? C4 C5 C6 C1 -2.1(3) . . . . ? C4 C5 C6 C16 172.2(2) . . . . ? C2 C1 C6 C5 4.9(3) . . . . ? P1 C1 C6 C5 -176.52(16) . . . . ? C2 C1 C6 C16 -168.62(18) . . . . ? P1 C1 C6 C16 9.9(3) . . . . ? C3 C2 C7A C12A -71.7(3) . . . . ? C1 C2 C7A C12A 112.0(2) . . . . ? C3 C2 C7A C8A 99.3(2) . . . . ? C1 C2 C7A C8A -76.9(3) . . . . ? C12A C7A C8A C9A -3.3(3) . . . . ? C2 C7A C8A C9A -174.36(19) . . . . ? C12A C7A C8A C13A 174.1(2) . . . . ? C2 C7A C8A C13A 3.1(3) . . . . ? C7A C8A C9A C10A 1.3(3) . . . . ? C13A C8A C9A C10A -176.2(2) . . . . ? C8A C9A C10A C11A 1.1(4) . . . . ? C8A C9A C10A C14A -179.5(2) . . . . ? C9A C10A C11A C12A -1.4(4) . . . . ? C14A C10A C11A C12A 179.2(2) . . . . ? C10A C11A C12A C7A -0.6(3) . . . . ? C10A C11A C12A C15A 179.5(2) . . . . ? C8A C7A C12A C11A 3.0(3) . . . . ? C2 C7A C12A C11A 173.97(19) . . . . ? C8A C7A C12A C15A -177.1(2) . . . . ? C2 C7A C12A C15A -6.2(3) . . . . ? C5 C6 C16 C21 81.4(3) . . . . ? C1 C6 C16 C21 -104.7(2) . . . . ? C5 C6 C16 C17 -91.2(2) . . . . ? C1 C6 C16 C17 82.7(3) . . . . ? C21 C16 C17 C18 7.5(3) . . . . ? C6 C16 C17 C18 -179.65(19) . . . . ? C21 C16 C17 C22 -168.6(2) . . . . ? C6 C16 C17 C22 4.2(3) . . . . ? C16 C17 C18 C19 -0.8(3) . . . . ? C22 C17 C18 C19 175.4(2) . . . . ? C17 C18 C19 C20 -4.7(3) . . . . ? C17 C18 C19 C23 177.2(2) . . . . ? C18 C19 C20 C21 3.5(3) . . . . ? C23 C19 C20 C21 -178.4(2) . . . . ? C19 C20 C21 C16 3.2(3) . . . . ? C19 C20 C21 C24 -172.7(2) . . . . ? C17 C16 C21 C20 -8.7(3) . . . . ? C6 C16 C21 C20 178.86(19) . . . . ? C17 C16 C21 C24 167.1(2) . . . . ? C6 C16 C21 C24 -5.4(3) . . . . ? C26 C25 N1 C27 76.1(2) . . . . ? C26 C25 N1 P1 -101.3(2) . . . . ? C28 C27 N1 C25 -83.9(2) . . . . ? C28 C27 N1 P1 93.5(2) . . . . ? C32 C31 N2 C29 -65.7(2) . . . . ? C32 C31 N2 P1 111.7(2) . . . . ? C30 C29 N2 C31 -85.6(2) . . . . ? C30 C29 N2 P1 96.8(2) . . . . ? C31 N2 P1 N1 -94.45(18) . . . . ? C29 N2 P1 N1 82.92(16) . . . . ? C31 N2 P1 C1 26.13(19) . . . . ? C29 N2 P1 C1 -156.51(15) . . . . ? C31 N2 P1 Au1 149.14(16) . . . . ? C29 N2 P1 Au1 -33.50(16) . . . . ? C25 N1 P1 N2 38.84(18) . . . . ? C27 N1 P1 N2 -138.39(16) . . . . ? C25 N1 P1 C1 -73.83(18) . . . . ? C27 N1 P1 C1 108.94(17) . . . . ? C25 N1 P1 Au1 161.22(14) . . . . ? C27 N1 P1 Au1 -16.01(17) . . . . ? C2 C1 P1 N2 -106.92(17) . . . . ? C6 C1 P1 N2 74.66(16) . . . . ? C2 C1 P1 N1 7.9(2) . . . . ? C6 C1 P1 N1 -170.49(14) . . . . ? C2 C1 P1 Au1 128.90(15) . . . . ? C6 C1 P1 Au1 -49.53(16) . . . . ?