#------------------------------------------------------------------------------ #$Date: 2020-08-20 04:45:48 +0300 (Thu, 20 Aug 2020) $ #$Revision: 255464 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/52/7705205.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_7705205 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_name_full 'Dalton Transactions' _journal_paper_doi 10.1039/D0DT02435J _journal_year 2020 _chemical_formula_moiety 'C28 H37 Au Cl N2 P' _chemical_formula_sum 'C28 H37 Au Cl N2 P' _chemical_formula_weight 664.98 _space_group_crystal_system orthorhombic _space_group_IT_number 33 _space_group_name_Hall 'P 2c -2n' _space_group_name_H-M_alt 'P n a 21' _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 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 22.6214(7) _cell_length_b 8.4955(3) _cell_length_c 14.1420(4) _cell_measurement_reflns_used 9977 _cell_measurement_temperature 150(2) _cell_measurement_theta_max 30.53 _cell_measurement_theta_min 2.88 _cell_volume 2717.81(15) _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 'SHELXT-2014 (Sheldrick, 2014)' _diffrn_ambient_temperature 150(2) _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 0.0535 _diffrn_reflns_av_unetI/netI 0.0376 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 1.000 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_number 38610 _diffrn_reflns_point_group_measured_fraction_full 0.932 _diffrn_reflns_point_group_measured_fraction_max 0.895 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 29.995 _diffrn_reflns_theta_min 1.800 _diffrn_source 'fine-focus sealed tube' _exptl_absorpt_coefficient_mu 5.589 _exptl_absorpt_correction_T_max 0.47 _exptl_absorpt_correction_T_min 0.31 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Bruker, 2014)' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.625 _exptl_crystal_description prism _exptl_crystal_F_000 1320 _exptl_crystal_size_max 0.334 _exptl_crystal_size_mid 0.296 _exptl_crystal_size_min 0.161 _refine_diff_density_max 1.433 _refine_diff_density_min -0.898 _refine_diff_density_rms 0.084 _refine_ls_abs_structure_details ; Flack x determined using 2495 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack 0.007(6) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 308 _refine_ls_number_reflns 7081 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.025 _refine_ls_R_factor_all 0.0293 _refine_ls_R_factor_gt 0.0260 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0306P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0588 _refine_ls_wR_factor_ref 0.0601 _reflns_Friedel_coverage 0.726 _reflns_Friedel_fraction_full 0.858 _reflns_Friedel_fraction_max 0.782 _reflns_number_gt 6527 _reflns_number_total 7081 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d0dt02435j2.cif _cod_data_source_block ax1653_TerPAuCl_NMe2_2_cmp2a _cod_database_code 7705205 _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 0.257 _shelx_estimated_absorpt_t_max 0.466 _shelx_res_file ; ax1657.res created by SHELXL-2014/7 TITL AX1657 in Pna2(1) CELL 0.71073 22.6214 8.4955 14.1420 90.000 90.000 90.000 ZERR 4.00 0.0007 0.0003 0.0004 0.000 0.000 0.000 LATT -1 SYMM - X, - Y, 1/2 + Z SYMM 1/2 - X, 1/2 + Y, 1/2 + Z SYMM 1/2 + X, 1/2 - Y, Z SFAC C H N P CL AU UNIT 112 148 8 4 4 4 MERG 2 OMIT -4.00 60.00 FMAP 2 PLAN 20 SIZE 0.161 0.296 0.334 ACTA BOND $H CONF LIST 4 L.S. 8 TEMP -123.15 WGHT 0.030600 FVAR 0.08248 AU1 6 0.425984 0.707292 0.255627 11.00000 0.03296 0.02755 = 0.02097 0.00274 0.00936 -0.00224 CL1 5 0.438237 0.842352 0.115905 11.00000 0.06705 0.05163 = 0.03238 0.01679 0.01995 0.00290 P1 4 0.416107 0.585218 0.394855 11.00000 0.02332 0.01740 = 0.01826 -0.00054 0.00384 -0.00064 N1 3 0.441630 0.402169 0.394640 11.00000 0.02837 0.02132 = 0.03804 -0.00432 0.00295 0.00414 N2 3 0.452773 0.687325 0.475678 11.00000 0.02805 0.02339 = 0.02383 -0.00246 0.00076 -0.00581 C1 1 0.338573 0.546029 0.427972 11.00000 0.02377 0.01529 = 0.01534 0.00350 0.00088 0.00012 C2 1 0.312464 0.587619 0.515258 11.00000 0.02341 0.01737 = 0.01382 0.00310 -0.00015 0.00082 C3 1 0.255365 0.535490 0.535969 11.00000 0.02484 0.02461 = 0.01856 0.00378 0.00383 -0.00002 AFIX 43 H3 2 0.238010 0.563571 0.594769 11.00000 -1.20000 AFIX 0 C4 1 0.223451 0.444310 0.473378 11.00000 0.02339 0.03079 = 0.02623 0.00604 -0.00199 -0.00631 AFIX 43 H4 2 0.185582 0.404996 0.490276 11.00000 -1.20000 AFIX 0 C5 1 0.247524 0.410946 0.385401 11.00000 0.02811 0.02769 = 0.02109 0.00201 -0.00353 -0.00606 AFIX 43 H5 2 0.225089 0.351819 0.341094 11.00000 -1.20000 AFIX 0 C6 1 0.303848 0.462316 0.360743 11.00000 0.02853 0.01641 = 0.01570 0.00377 -0.00053 0.00125 C7 1 0.338788 0.697000 0.587419 11.00000 0.02152 0.02082 = 0.01718 0.00089 0.00315 -0.00032 C8 1 0.355388 0.642755 0.676963 11.00000 0.02464 0.02351 = 0.01772 -0.00097 0.00239 -0.00206 C9 1 0.374999 0.750191 0.745042 11.00000 0.02315 0.03357 = 0.01929 -0.00162 0.00048 0.00145 AFIX 43 H9 2 0.386077 0.712610 0.805779 11.00000 -1.20000 AFIX 0 C10 1 0.378719 0.910912 0.726141 11.00000 0.02698 0.03316 = 0.02778 -0.01092 0.00347 -0.00178 C11 1 0.359528 0.961772 0.638196 11.00000 0.03439 0.02157 = 0.03043 -0.00574 0.00862 -0.00387 AFIX 43 H11 2 0.360611 1.071213 0.624512 11.00000 -1.20000 AFIX 0 C12 1 0.338945 0.860016 0.569821 11.00000 0.02895 0.02321 = 0.02122 0.00041 0.00497 0.00017 C13 1 0.354173 0.470156 0.702944 11.00000 0.04234 0.02594 = 0.02305 0.00596 -0.00574 -0.00438 AFIX 137 H13A 2 0.390964 0.442236 0.735463 11.00000 -1.50000 H13B 2 0.350253 0.406707 0.645411 11.00000 -1.50000 H13C 2 0.320515 0.449646 0.744797 11.00000 -1.50000 AFIX 0 C14 1 0.402689 1.023885 0.798132 11.00000 0.04601 0.03835 = 0.03989 -0.01793 -0.00165 -0.00863 AFIX 137 H14A 2 0.438995 1.072189 0.773893 11.00000 -1.50000 H14B 2 0.411416 0.967195 0.856847 11.00000 -1.50000 H14C 2 0.373311 1.106054 0.810673 11.00000 -1.50000 AFIX 0 C15 1 0.316573 0.923163 0.476515 11.00000 0.04833 0.01922 = 0.02750 0.00355 0.00139 0.00586 AFIX 137 H15A 2 0.310298 1.036975 0.481699 11.00000 -1.50000 H15B 2 0.279151 0.871593 0.460416 11.00000 -1.50000 H15C 2 0.345766 0.901859 0.426940 11.00000 -1.50000 AFIX 0 C16 1 0.320904 0.440601 0.257281 11.00000 0.02538 0.02174 = 0.01580 0.00083 -0.00318 -0.00326 C17 1 0.343837 0.299660 0.221422 11.00000 0.03533 0.02027 = 0.01802 -0.00199 -0.00128 -0.00354 C18 1 0.356268 0.289226 0.125156 11.00000 0.03622 0.02650 = 0.02112 -0.00523 0.00087 -0.00029 AFIX 43 H18 2 0.373968 0.195899 0.101327 11.00000 -1.20000 AFIX 0 C19 1 0.343662 0.410227 0.063417 11.00000 0.03322 0.03444 = 0.01828 0.00060 -0.00187 -0.00749 C20 1 0.317747 0.544627 0.099530 11.00000 0.04197 0.02858 = 0.01819 0.00618 -0.00449 -0.00074 AFIX 43 H20 2 0.307685 0.627491 0.057392 11.00000 -1.20000 AFIX 0 C21 1 0.305872 0.562922 0.195323 11.00000 0.03034 0.02389 = 0.02144 0.00124 -0.00310 -0.00075 C22 1 0.352809 0.156763 0.282272 11.00000 0.07174 0.02257 = 0.03082 -0.00077 -0.00551 0.00082 AFIX 137 H22A 2 0.323794 0.076013 0.265098 11.00000 -1.50000 H22B 2 0.347678 0.185508 0.348880 11.00000 -1.50000 H22C 2 0.392808 0.115523 0.272546 11.00000 -1.50000 AFIX 0 C23 1 0.356218 0.394662 -0.041013 11.00000 0.05442 0.05219 = 0.01337 -0.00085 0.00493 -0.00338 AFIX 137 H23A 2 0.341391 0.487910 -0.074204 11.00000 -1.50000 H23B 2 0.336466 0.300535 -0.065640 11.00000 -1.50000 H23C 2 0.398949 0.385436 -0.050984 11.00000 -1.50000 AFIX 0 C24 1 0.275111 0.710026 0.228941 11.00000 0.04283 0.02854 = 0.02747 0.00628 -0.00346 0.01148 AFIX 137 H24A 2 0.269941 0.782482 0.175657 11.00000 -1.50000 H24B 2 0.299047 0.760840 0.277975 11.00000 -1.50000 H24C 2 0.236346 0.682397 0.255047 11.00000 -1.50000 AFIX 0 C25 1 0.497390 0.371183 0.347235 11.00000 0.03885 0.04188 = 0.06983 -0.01383 0.01517 0.00984 AFIX 137 H25A 2 0.529725 0.376536 0.393242 11.00000 -1.50000 H25B 2 0.503744 0.450064 0.297704 11.00000 -1.50000 H25C 2 0.496323 0.266043 0.318776 11.00000 -1.50000 AFIX 0 C26 1 0.429169 0.286300 0.469375 11.00000 0.04913 0.02140 = 0.03931 0.00455 -0.00733 0.00787 AFIX 137 H26A 2 0.425089 0.181500 0.441161 11.00000 -1.50000 H26B 2 0.392361 0.314666 0.501703 11.00000 -1.50000 H26C 2 0.461758 0.285570 0.515031 11.00000 -1.50000 AFIX 0 C27 1 0.472859 0.848461 0.461112 11.00000 0.04230 0.02914 = 0.03497 -0.00631 0.00371 -0.01495 AFIX 137 H27A 2 0.455470 0.916871 0.509481 11.00000 -1.50000 H27B 2 0.460559 0.884524 0.398298 11.00000 -1.50000 H27C 2 0.516058 0.852371 0.465760 11.00000 -1.50000 AFIX 0 C28 1 0.476361 0.618199 0.562388 11.00000 0.03050 0.04592 = 0.02391 -0.00357 -0.00356 -0.00414 AFIX 137 H28A 2 0.518105 0.591457 0.553152 11.00000 -1.50000 H28B 2 0.454090 0.522697 0.577928 11.00000 -1.50000 H28C 2 0.472715 0.694063 0.614264 11.00000 -1.50000 AFIX 0 HKLF 4 1.0 1.00 0.00 0.00 0.00 1.00 0.00 0.00 0.00 1.00 REM AX1657 in Pna2(1) REM R1 = 0.0260 for 6527 Fo > 4sig(Fo) and 0.0293 for all 7081 data REM 308 parameters refined using 1 restraints END WGHT 0.0306 0.0000 REM Highest difference peak 1.433, deepest hole -0.898, 1-sigma level 0.084 Q1 1 0.4582 0.7163 0.2302 11.00000 0.05 1.29 Q2 1 0.4557 0.7145 0.2824 11.00000 0.05 1.19 Q3 1 0.3933 0.7146 0.2843 11.00000 0.05 1.13 Q4 1 0.3929 0.7141 0.2222 11.00000 0.05 1.07 Q5 1 0.2221 0.7958 0.2580 11.00000 0.05 0.84 Q6 1 0.4267 0.8881 0.2556 11.00000 0.05 0.60 Q7 1 0.4386 0.7036 0.1704 11.00000 0.05 0.36 Q8 1 0.4141 0.7084 0.3399 11.00000 0.05 0.35 Q9 1 0.4873 0.7335 0.2142 11.00000 0.05 0.34 Q10 1 0.4655 0.8638 0.1431 11.00000 0.05 0.34 Q11 1 0.3910 0.9634 0.7568 11.00000 0.05 0.33 Q12 1 0.4128 0.5777 0.1119 11.00000 0.05 0.33 Q13 1 0.4358 0.6327 0.4327 11.00000 0.05 0.32 Q14 1 0.4447 0.5957 0.3508 11.00000 0.05 0.31 Q15 1 0.4369 0.8366 0.4037 11.00000 0.05 0.30 Q16 1 0.3813 0.5709 0.4301 11.00000 0.05 0.30 Q17 1 0.3476 0.3957 0.2531 11.00000 0.05 0.29 Q18 1 0.4106 0.8498 0.1367 11.00000 0.05 0.28 Q19 1 0.3363 0.6728 0.6363 11.00000 0.05 0.28 Q20 1 0.2904 0.5393 0.5109 11.00000 0.05 0.28 ; _shelx_res_checksum 16294 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, z+1/2' '-x+1/2, y+1/2, z+1/2' 'x+1/2, -y+1/2, z' 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 Au1 Au 0.42598(2) 0.70729(2) 0.25563(2) 0.02716(5) Uani 1 1 d . . . . . Cl1 Cl 0.43824(7) 0.8424(2) 0.11590(11) 0.0504(3) Uani 1 1 d . . . . . P1 P 0.41611(4) 0.58522(12) 0.39486(8) 0.0197(2) Uani 1 1 d . . . . . N1 N 0.44163(17) 0.4022(4) 0.3946(3) 0.0292(8) Uani 1 1 d . . . . . N2 N 0.45277(17) 0.6873(4) 0.4757(3) 0.0251(8) Uani 1 1 d . . . . . C1 C 0.33857(18) 0.5460(5) 0.4280(3) 0.0181(8) Uani 1 1 d . . . . . C2 C 0.31246(17) 0.5876(4) 0.5153(3) 0.0182(7) Uani 1 1 d . . . . . C3 C 0.25537(18) 0.5355(5) 0.5360(3) 0.0227(8) Uani 1 1 d . . . . . H3 H 0.2380 0.5636 0.5948 0.027 Uiso 1 1 calc R U . . . C4 C 0.22345(18) 0.4443(5) 0.4734(3) 0.0268(9) Uani 1 1 d . . . . . H4 H 0.1856 0.4050 0.4903 0.032 Uiso 1 1 calc R U . . . C5 C 0.24752(18) 0.4109(5) 0.3854(3) 0.0256(8) Uani 1 1 d . . . . . H5 H 0.2251 0.3518 0.3411 0.031 Uiso 1 1 calc R U . . . C6 C 0.30385(17) 0.4623(4) 0.3607(3) 0.0202(7) Uani 1 1 d . . . . . C7 C 0.33879(19) 0.6970(4) 0.5874(3) 0.0198(8) Uani 1 1 d . . . . . C8 C 0.35539(18) 0.6428(5) 0.6770(3) 0.0220(8) Uani 1 1 d . . . . . C9 C 0.37500(17) 0.7502(5) 0.7450(4) 0.0253(9) Uani 1 1 d . . . . . H9 H 0.3861 0.7126 0.8058 0.030 Uiso 1 1 calc R U . . . C10 C 0.37872(19) 0.9109(5) 0.7261(3) 0.0293(9) Uani 1 1 d . . . . . C11 C 0.3595(2) 0.9618(5) 0.6382(3) 0.0288(9) Uani 1 1 d . . . . . H11 H 0.3606 1.0712 0.6245 0.035 Uiso 1 1 calc R U . . . C12 C 0.33894(19) 0.8600(5) 0.5698(3) 0.0245(8) Uani 1 1 d . . . . . C13 C 0.3542(2) 0.4702(5) 0.7029(3) 0.0304(9) Uani 1 1 d . . . . . H13A H 0.3910 0.4422 0.7355 0.046 Uiso 1 1 calc R U . . . H13B H 0.3503 0.4067 0.6454 0.046 Uiso 1 1 calc R U . . . H13C H 0.3205 0.4496 0.7448 0.046 Uiso 1 1 calc R U . . . C14 C 0.4027(2) 1.0239(6) 0.7981(4) 0.0414(12) Uani 1 1 d . . . . . H14A H 0.4390 1.0722 0.7739 0.062 Uiso 1 1 calc R U . . . H14B H 0.4114 0.9672 0.8568 0.062 Uiso 1 1 calc R U . . . H14C H 0.3733 1.1061 0.8107 0.062 Uiso 1 1 calc R U . . . C15 C 0.3166(2) 0.9232(5) 0.4765(3) 0.0317(10) Uani 1 1 d . . . . . H15A H 0.3103 1.0370 0.4817 0.048 Uiso 1 1 calc R U . . . H15B H 0.2792 0.8716 0.4604 0.048 Uiso 1 1 calc R U . . . H15C H 0.3458 0.9019 0.4269 0.048 Uiso 1 1 calc R U . . . C16 C 0.32090(14) 0.4406(4) 0.2573(4) 0.0210(6) Uani 1 1 d . . . . . C17 C 0.3438(2) 0.2997(4) 0.2214(3) 0.0245(9) Uani 1 1 d . . . . . C18 C 0.3563(2) 0.2892(5) 0.1252(3) 0.0279(9) Uani 1 1 d . . . . . H18 H 0.3740 0.1959 0.1013 0.034 Uiso 1 1 calc R U . . . C19 C 0.3437(2) 0.4102(6) 0.0634(3) 0.0286(9) Uani 1 1 d . . . . . C20 C 0.3177(2) 0.5446(5) 0.0995(3) 0.0296(10) Uani 1 1 d . . . . . H20 H 0.3077 0.6275 0.0574 0.035 Uiso 1 1 calc R U . . . C21 C 0.30587(19) 0.5629(5) 0.1953(3) 0.0252(8) Uani 1 1 d . . . . . C22 C 0.3528(3) 0.1568(6) 0.2823(3) 0.0417(13) Uani 1 1 d . . . . . H22A H 0.3238 0.0760 0.2651 0.063 Uiso 1 1 calc R U . . . H22B H 0.3477 0.1855 0.3489 0.063 Uiso 1 1 calc R U . . . H22C H 0.3928 0.1155 0.2725 0.063 Uiso 1 1 calc R U . . . C23 C 0.3562(3) 0.3947(7) -0.0410(3) 0.0400(12) Uani 1 1 d . . . . . H23A H 0.3414 0.4879 -0.0742 0.060 Uiso 1 1 calc R U . . . H23B H 0.3365 0.3005 -0.0656 0.060 Uiso 1 1 calc R U . . . H23C H 0.3989 0.3854 -0.0510 0.060 Uiso 1 1 calc R U . . . C24 C 0.2751(2) 0.7100(5) 0.2289(4) 0.0329(11) Uani 1 1 d . . . . . H24A H 0.2699 0.7825 0.1757 0.049 Uiso 1 1 calc R U . . . H24B H 0.2990 0.7608 0.2780 0.049 Uiso 1 1 calc R U . . . H24C H 0.2363 0.6824 0.2550 0.049 Uiso 1 1 calc R U . . . C25 C 0.4974(2) 0.3712(7) 0.3472(5) 0.0502(15) Uani 1 1 d . . . . . H25A H 0.5297 0.3765 0.3932 0.075 Uiso 1 1 calc R U . . . H25B H 0.5037 0.4501 0.2977 0.075 Uiso 1 1 calc R U . . . H25C H 0.4963 0.2660 0.3188 0.075 Uiso 1 1 calc R U . . . C26 C 0.4292(2) 0.2863(5) 0.4694(5) 0.0366(13) Uani 1 1 d . . . . . H26A H 0.4251 0.1815 0.4412 0.055 Uiso 1 1 calc R U . . . H26B H 0.3924 0.3147 0.5017 0.055 Uiso 1 1 calc R U . . . H26C H 0.4618 0.2856 0.5150 0.055 Uiso 1 1 calc R U . . . C27 C 0.4729(2) 0.8485(6) 0.4611(4) 0.0355(11) Uani 1 1 d . . . . . H27A H 0.4555 0.9169 0.5095 0.053 Uiso 1 1 calc R U . . . H27B H 0.4606 0.8845 0.3983 0.053 Uiso 1 1 calc R U . . . H27C H 0.5161 0.8524 0.4658 0.053 Uiso 1 1 calc R U . . . C28 C 0.4764(2) 0.6182(6) 0.5624(3) 0.0334(10) Uani 1 1 d . . . . . H28A H 0.5181 0.5915 0.5532 0.050 Uiso 1 1 calc R U . . . H28B H 0.4541 0.5227 0.5779 0.050 Uiso 1 1 calc R U . . . H28C H 0.4727 0.6941 0.6143 0.050 Uiso 1 1 calc R U . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Au1 0.03296(8) 0.02755(8) 0.02097(8) 0.00274(9) 0.00936(8) -0.00224(5) Cl1 0.0670(9) 0.0516(7) 0.0324(7) 0.0168(7) 0.0199(7) 0.0029(7) P1 0.0233(5) 0.0174(4) 0.0183(5) -0.0005(4) 0.0038(4) -0.0006(4) N1 0.0284(17) 0.0213(17) 0.038(2) -0.0043(16) 0.0029(17) 0.0041(14) N2 0.0281(19) 0.0234(17) 0.0238(19) -0.0025(14) 0.0008(15) -0.0058(14) C1 0.024(2) 0.0153(18) 0.0153(18) 0.0035(14) 0.0009(15) 0.0001(14) C2 0.0234(18) 0.0174(17) 0.0138(17) 0.0031(13) -0.0001(14) 0.0008(13) C3 0.0248(19) 0.0246(19) 0.0186(18) 0.0038(16) 0.0038(15) 0.0000(15) C4 0.023(2) 0.031(2) 0.026(2) 0.0060(17) -0.0020(17) -0.0063(17) C5 0.028(2) 0.028(2) 0.0211(19) 0.0020(16) -0.0035(17) -0.0061(16) C6 0.0285(19) 0.0164(18) 0.0157(17) 0.0038(14) -0.0005(14) 0.0012(14) C7 0.0215(18) 0.0208(19) 0.0172(19) 0.0009(14) 0.0031(15) -0.0003(14) C8 0.0246(19) 0.024(2) 0.0177(18) -0.0010(16) 0.0024(15) -0.0021(15) C9 0.0231(17) 0.0336(18) 0.019(3) -0.0016(18) 0.0005(17) 0.0015(14) C10 0.027(2) 0.033(2) 0.028(2) -0.0109(17) 0.0035(16) -0.0018(17) C11 0.034(2) 0.022(2) 0.030(2) -0.0057(17) 0.0086(18) -0.0039(17) C12 0.029(2) 0.023(2) 0.0212(19) 0.0004(16) 0.0050(16) 0.0002(16) C13 0.042(3) 0.026(2) 0.023(2) 0.0060(17) -0.0057(18) -0.0044(19) C14 0.046(3) 0.038(3) 0.040(3) -0.018(2) -0.002(2) -0.009(2) C15 0.048(3) 0.019(2) 0.027(2) 0.0036(16) 0.001(2) 0.0059(18) C16 0.0254(15) 0.0217(14) 0.0158(14) 0.001(2) -0.003(2) -0.0033(12) C17 0.035(2) 0.020(2) 0.0180(18) -0.0020(14) -0.0013(17) -0.0035(15) C18 0.036(2) 0.027(2) 0.021(2) -0.0052(16) 0.0009(18) -0.0003(16) C19 0.033(2) 0.034(2) 0.0183(19) 0.0006(17) -0.0019(17) -0.0075(18) C20 0.042(3) 0.029(2) 0.018(2) 0.0062(17) -0.0045(19) -0.001(2) C21 0.030(2) 0.024(2) 0.0214(19) 0.0012(16) -0.0031(16) -0.0008(16) C22 0.072(4) 0.023(2) 0.031(3) -0.0008(17) -0.006(2) 0.001(2) C23 0.054(3) 0.052(3) 0.0134(19) -0.001(2) 0.005(2) -0.003(2) C24 0.043(3) 0.029(2) 0.027(2) 0.0063(16) -0.0035(19) 0.0115(18) C25 0.039(3) 0.042(3) 0.070(4) -0.014(3) 0.015(3) 0.010(2) C26 0.049(3) 0.021(3) 0.039(3) 0.0046(19) -0.007(2) 0.0079(18) C27 0.042(3) 0.029(2) 0.035(3) -0.006(2) 0.004(2) -0.015(2) C28 0.031(2) 0.046(3) 0.024(2) -0.004(2) -0.0036(18) -0.004(2) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 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 P1 Au1 Cl1 177.37(5) . . ? N2 P1 N1 108.5(2) . . ? N2 P1 C1 113.3(2) . . ? N1 P1 C1 99.33(19) . . ? N2 P1 Au1 108.33(13) . . ? N1 P1 Au1 113.47(16) . . ? C1 P1 Au1 113.70(13) . . ? C25 N1 C26 112.1(4) . . ? C25 N1 P1 118.2(3) . . ? C26 N1 P1 124.0(3) . . ? C27 N2 C28 112.5(4) . . ? C27 N2 P1 123.4(3) . . ? C28 N2 P1 123.5(3) . . ? C2 C1 C6 118.5(4) . . ? C2 C1 P1 125.0(3) . . ? C6 C1 P1 116.4(3) . . ? C3 C2 C1 119.4(4) . . ? C3 C2 C7 114.8(3) . . ? C1 C2 C7 125.6(4) . . ? C4 C3 C2 121.8(4) . . ? C4 C3 H3 119.1 . . ? C2 C3 H3 119.1 . . ? C3 C4 C5 119.0(4) . . ? C3 C4 H4 120.5 . . ? C5 C4 H4 120.5 . . ? C4 C5 C6 121.3(4) . . ? C4 C5 H5 119.3 . . ? C6 C5 H5 119.3 . . ? C5 C6 C1 119.6(3) . . ? C5 C6 C16 115.7(3) . . ? C1 C6 C16 124.2(3) . . ? C8 C7 C12 118.9(4) . . ? C8 C7 C2 121.1(3) . . ? C12 C7 C2 119.3(3) . . ? C9 C8 C7 119.6(4) . . ? C9 C8 C13 118.1(4) . . ? C7 C8 C13 122.3(4) . . ? C10 C9 C8 121.8(4) . . ? C10 C9 H9 119.1 . . ? C8 C9 H9 119.1 . . ? C11 C10 C9 117.3(4) . . ? C11 C10 C14 121.5(4) . . ? C9 C10 C14 121.2(4) . . ? C12 C11 C10 122.7(4) . . ? C12 C11 H11 118.7 . . ? C10 C11 H11 118.7 . . ? C11 C12 C7 119.6(4) . . ? C11 C12 C15 120.2(4) . . ? C7 C12 C15 120.2(4) . . ? C8 C13 H13A 109.5 . . ? C8 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C8 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C10 C14 H14A 109.5 . . ? C10 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C10 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C12 C15 H15A 109.5 . . ? C12 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C12 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C17 C16 C21 119.8(5) . . ? C17 C16 C6 123.0(4) . . ? C21 C16 C6 116.7(3) . . ? C18 C17 C16 118.9(4) . . ? C18 C17 C22 118.8(4) . . ? C16 C17 C22 122.3(4) . . ? C19 C18 C17 122.0(4) . . ? C19 C18 H18 119.0 . . ? C17 C18 H18 119.0 . . ? C18 C19 C20 118.0(4) . . ? C18 C19 C23 121.0(4) . . ? C20 C19 C23 120.9(4) . . ? C19 C20 C21 122.3(4) . . ? C19 C20 H20 118.8 . . ? C21 C20 H20 118.8 . . ? C20 C21 C16 118.7(4) . . ? C20 C21 C24 119.3(4) . . ? C16 C21 C24 122.0(4) . . ? 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 H25A 109.5 . . ? N1 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? N1 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? N1 C26 H26A 109.5 . . ? N1 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? N1 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? N2 C27 H27A 109.5 . . ? N2 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? N2 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? N2 C28 H28A 109.5 . . ? N2 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? N2 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Au1 P1 2.2366(11) . ? Au1 Cl1 2.3017(14) . ? P1 N2 1.657(4) . ? P1 N1 1.659(4) . ? P1 C1 1.846(4) . ? N1 C25 1.453(6) . ? N1 C26 1.472(7) . ? N2 C27 1.457(6) . ? N2 C28 1.461(6) . ? C1 C2 1.413(5) . ? C1 C6 1.424(5) . ? C2 C3 1.397(5) . ? C2 C7 1.503(6) . ? C3 C4 1.380(6) . ? C3 H3 0.9500 . ? C4 C5 1.387(6) . ? C4 H4 0.9500 . ? C5 C6 1.391(6) . ? C5 H5 0.9500 . ? C6 C16 1.524(6) . ? C7 C8 1.399(6) . ? C7 C12 1.407(6) . ? C8 C9 1.399(6) . ? C8 C13 1.512(6) . ? C9 C10 1.394(6) . ? C9 H9 0.9500 . ? C10 C11 1.386(7) . ? C10 C14 1.501(6) . ? C11 C12 1.378(6) . ? C11 H11 0.9500 . ? C12 C15 1.512(6) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.400(5) . ? C16 C21 1.401(6) . ? C17 C18 1.393(6) . ? C17 C22 1.502(6) . ? C18 C19 1.379(6) . ? C18 H18 0.9500 . ? C19 C20 1.381(7) . ? C19 C23 1.510(6) . ? C20 C21 1.390(6) . ? C20 H20 0.9500 . ? C21 C24 1.507(6) . ? 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 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? 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 N2 P1 N1 C25 -78.1(4) . . . . ? C1 P1 N1 C25 163.4(4) . . . . ? Au1 P1 N1 C25 42.3(4) . . . . ? N2 P1 N1 C26 73.2(4) . . . . ? C1 P1 N1 C26 -45.3(4) . . . . ? Au1 P1 N1 C26 -166.3(3) . . . . ? N1 P1 N2 C27 139.0(4) . . . . ? C1 P1 N2 C27 -111.8(4) . . . . ? Au1 P1 N2 C27 15.4(4) . . . . ? N1 P1 N2 C28 -31.0(4) . . . . ? C1 P1 N2 C28 78.2(4) . . . . ? Au1 P1 N2 C28 -154.6(3) . . . . ? N2 P1 C1 C2 -4.0(4) . . . . ? N1 P1 C1 C2 110.9(4) . . . . ? Au1 P1 C1 C2 -128.2(3) . . . . ? N2 P1 C1 C6 178.4(3) . . . . ? N1 P1 C1 C6 -66.7(3) . . . . ? Au1 P1 C1 C6 54.2(3) . . . . ? C6 C1 C2 C3 4.9(5) . . . . ? P1 C1 C2 C3 -172.7(3) . . . . ? C6 C1 C2 C7 -169.6(3) . . . . ? P1 C1 C2 C7 12.8(6) . . . . ? C1 C2 C3 C4 -0.1(6) . . . . ? C7 C2 C3 C4 175.0(4) . . . . ? C2 C3 C4 C5 -3.6(6) . . . . ? C3 C4 C5 C6 2.5(6) . . . . ? C4 C5 C6 C1 2.3(6) . . . . ? C4 C5 C6 C16 -170.6(4) . . . . ? C2 C1 C6 C5 -5.9(5) . . . . ? P1 C1 C6 C5 171.8(3) . . . . ? C2 C1 C6 C16 166.3(3) . . . . ? P1 C1 C6 C16 -16.0(5) . . . . ? C3 C2 C7 C8 70.2(5) . . . . ? C1 C2 C7 C8 -115.1(5) . . . . ? C3 C2 C7 C12 -100.6(4) . . . . ? C1 C2 C7 C12 74.1(5) . . . . ? C12 C7 C8 C9 -3.7(6) . . . . ? C2 C7 C8 C9 -174.5(4) . . . . ? C12 C7 C8 C13 177.6(4) . . . . ? C2 C7 C8 C13 6.7(6) . . . . ? C7 C8 C9 C10 -0.2(6) . . . . ? C13 C8 C9 C10 178.6(4) . . . . ? C8 C9 C10 C11 2.9(6) . . . . ? C8 C9 C10 C14 -176.9(4) . . . . ? C9 C10 C11 C12 -1.8(6) . . . . ? C14 C10 C11 C12 178.1(4) . . . . ? C10 C11 C12 C7 -2.1(6) . . . . ? C10 C11 C12 C15 177.8(4) . . . . ? C8 C7 C12 C11 4.8(6) . . . . ? C2 C7 C12 C11 175.9(4) . . . . ? C8 C7 C12 C15 -175.1(4) . . . . ? C2 C7 C12 C15 -4.0(6) . . . . ? C5 C6 C16 C17 -84.3(5) . . . . ? C1 C6 C16 C17 103.2(5) . . . . ? C5 C6 C16 C21 88.0(4) . . . . ? C1 C6 C16 C21 -84.5(5) . . . . ? C21 C16 C17 C18 5.8(6) . . . . ? C6 C16 C17 C18 177.8(4) . . . . ? C21 C16 C17 C22 -171.3(4) . . . . ? C6 C16 C17 C22 0.8(6) . . . . ? C16 C17 C18 C19 -3.6(7) . . . . ? C22 C17 C18 C19 173.5(4) . . . . ? C17 C18 C19 C20 -0.2(7) . . . . ? C17 C18 C19 C23 -178.5(5) . . . . ? C18 C19 C20 C21 2.0(7) . . . . ? C23 C19 C20 C21 -179.7(5) . . . . ? C19 C20 C21 C16 0.1(7) . . . . ? C19 C20 C21 C24 -177.4(4) . . . . ? C17 C16 C21 C20 -4.1(6) . . . . ? C6 C16 C21 C20 -176.6(4) . . . . ? C17 C16 C21 C24 173.4(4) . . . . ? C6 C16 C21 C24 0.8(6) . . . . ?