#------------------------------------------------------------------------------ #$Date: 2020-10-06 12:02:34 +0300 (Tue, 06 Oct 2020) $ #$Revision: 257564 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/52/7705208.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_7705208 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 'C56 H74 Ag2 Cl2 N4 P2' _chemical_formula_sum 'C56 H74 Ag2 Cl2 N4 P2' _chemical_formula_weight 1151.77 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 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 98.4356(16) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 9.7963(9) _cell_length_b 14.5920(14) _cell_length_c 19.4635(18) _cell_measurement_reflns_used 9917 _cell_measurement_temperature 150(2) _cell_measurement_theta_max 29.58 _cell_measurement_theta_min 2.52 _cell_volume 2752.2(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_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.998 _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 0.0441 _diffrn_reflns_av_unetI/netI 0.0305 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_number 56649 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 30.560 _diffrn_reflns_theta_min 1.751 _exptl_absorpt_coefficient_mu 0.906 _exptl_absorpt_correction_T_max 0.961 _exptl_absorpt_correction_T_min 0.807 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS 2014/5' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.390 _exptl_crystal_description plate _exptl_crystal_F_000 1192 _exptl_crystal_size_max 0.247 _exptl_crystal_size_mid 0.126 _exptl_crystal_size_min 0.044 _refine_diff_density_max 1.039 _refine_diff_density_min -0.969 _refine_diff_density_rms 0.072 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 308 _refine_ls_number_reflns 8407 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.022 _refine_ls_R_factor_all 0.0554 _refine_ls_R_factor_gt 0.0349 _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^)+(0.0424P)^2^+1.3912P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0830 _refine_ls_wR_factor_ref 0.0941 _reflns_Friedel_coverage 0.000 _reflns_number_gt 6269 _reflns_number_total 8407 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d0dt02435j2.cif _cod_data_source_block ax1925_TerP_NMe2_2_AgCl_cmp6a _cod_depositor_comments 'Adding full bibliography for 7705201--7705209.cif.' _cod_original_sg_symbol_H-M 'P 21/c' _cod_database_code 7705208 _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 0.807 _shelx_estimated_absorpt_t_max 0.961 _shelx_res_file ; shelx.res created by SHELXL-2014/7 TITL shelxt_a.res in P2(1)/c CELL 0.71073 9.7963 14.5920 19.4635 90.000 98.436 90.000 ZERR 2.00 0.0009 0.0014 0.0018 0.000 0.002 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H P CL AG N UNIT 112 148 4 4 4 8 MERG 2 FMAP 2 PLAN 20 SIZE 0.044 0.126 0.247 ACTA BOND $H CONF LIST 6 L.S. 64 TEMP -123.14 WGHT 0.042400 1.391200 FVAR 0.08423 PART 1 C1 1 0.276084 0.240296 0.642054 11.00000 0.02382 0.03918 = 0.01964 0.00314 0.00442 0.00730 C2 1 0.376560 0.177740 0.624635 11.00000 0.03231 0.06284 = 0.01971 0.00663 0.00450 0.02161 C3 1 0.424983 0.107212 0.669626 11.00000 0.05997 0.07839 = 0.02785 0.01322 0.01284 0.04671 AFIX 43 H3 2 0.488621 0.064143 0.655997 11.00000 -1.20000 AFIX 0 C4 1 0.381894 0.098577 0.734275 11.00000 0.06102 0.07058 = 0.02757 0.01608 0.00991 0.03929 AFIX 43 H4 2 0.414089 0.049529 0.764459 11.00000 -1.20000 AFIX 0 C5 1 0.291078 0.162971 0.753726 11.00000 0.04498 0.05309 = 0.02020 0.00715 0.00704 0.01774 AFIX 43 H5 2 0.264735 0.159201 0.798710 11.00000 -1.20000 AFIX 0 C6 1 0.236884 0.233505 0.709065 11.00000 0.02589 0.03986 = 0.01923 0.00168 0.00439 0.00663 C7 1 0.449314 0.191787 0.562250 11.00000 0.02870 0.06925 = 0.02358 0.00619 0.00638 0.02537 C8 1 0.561708 0.252937 0.569847 11.00000 0.02096 0.10106 = 0.03031 -0.00051 0.00382 0.01892 C9 1 0.623830 0.273618 0.511124 11.00000 0.02100 0.11520 = 0.03888 -0.00639 0.01000 0.00554 AFIX 43 H9 2 0.697100 0.316842 0.515298 11.00000 -1.20000 AFIX 0 C10 1 0.581790 0.233209 0.447858 11.00000 0.02734 0.09357 = 0.03580 0.00161 0.01606 0.01659 C11 1 0.479528 0.166761 0.443298 11.00000 0.04264 0.07168 = 0.02513 -0.00068 0.01157 0.02320 AFIX 43 H11 2 0.454449 0.135426 0.400525 11.00000 -1.20000 AFIX 0 C12 1 0.411715 0.144271 0.500028 11.00000 0.03911 0.05561 = 0.02773 0.00642 0.00970 0.02481 C13 1 0.618080 0.292636 0.639832 11.00000 0.02484 0.13571 = 0.03346 -0.01109 -0.00088 0.00786 AFIX 137 H13A 2 0.688999 0.338307 0.634292 11.00000 -1.50000 H13B 2 0.658716 0.243548 0.670608 11.00000 -1.50000 H13C 2 0.543148 0.321846 0.660065 11.00000 -1.50000 AFIX 0 C14 1 0.643553 0.262354 0.383718 11.00000 0.04351 0.12118 = 0.03928 -0.00500 0.02319 -0.00052 AFIX 137 H14A 2 0.599768 0.319342 0.365170 11.00000 -1.50000 H14B 2 0.627567 0.214207 0.348348 11.00000 -1.50000 H14C 2 0.743001 0.272235 0.396432 11.00000 -1.50000 AFIX 0 C15 1 0.305981 0.068830 0.492778 11.00000 0.06557 0.04639 = 0.03776 0.00333 0.01774 0.01709 AFIX 137 H15A 2 0.352277 0.009560 0.490774 11.00000 -1.50000 H15B 2 0.240921 0.077960 0.450038 11.00000 -1.50000 H15C 2 0.255845 0.069809 0.532798 11.00000 -1.50000 AFIX 0 C16 1 0.147000 0.299790 0.741277 11.00000 0.03172 0.03129 = 0.01843 0.00249 0.00683 0.00346 C17 1 0.201499 0.384561 0.765765 11.00000 0.04325 0.03903 = 0.02215 -0.00039 0.00703 -0.00476 C18 1 0.124007 0.440366 0.803595 11.00000 0.07229 0.02820 = 0.02923 -0.00161 0.01428 -0.00393 AFIX 43 H18 2 0.160951 0.497890 0.819892 11.00000 -1.20000 AFIX 0 C20 1 -0.004653 0.414987 0.818236 11.00000 0.06665 0.02974 = 0.03095 0.00705 0.02297 0.01634 C21 1 -0.057588 0.331624 0.792908 11.00000 0.04226 0.03500 = 0.03340 0.01006 0.02040 0.01158 AFIX 43 H21 2 -0.147107 0.313923 0.801125 11.00000 -1.20000 AFIX 0 C22 1 0.016801 0.272856 0.755651 11.00000 0.03374 0.02666 = 0.02560 0.00492 0.01155 0.00487 C23 1 0.343722 0.413927 0.753523 11.00000 0.04864 0.07137 = 0.03337 -0.01142 0.00752 -0.02918 AFIX 137 H23A 2 0.367850 0.471976 0.777595 11.00000 -1.50000 H23B 2 0.344618 0.422009 0.703607 11.00000 -1.50000 H23C 2 0.411025 0.366858 0.771421 11.00000 -1.50000 AFIX 0 C24 1 -0.083817 0.475355 0.862208 11.00000 0.10398 0.03759 = 0.05307 0.00586 0.04354 0.02512 AFIX 137 H24A 2 -0.130556 0.524283 0.833298 11.00000 -1.50000 H24B 2 -0.019550 0.502405 0.900121 11.00000 -1.50000 H24C 2 -0.152450 0.438347 0.881590 11.00000 -1.50000 AFIX 0 C25 1 -0.044650 0.180856 0.732584 11.00000 0.04407 0.03554 = 0.04303 0.00152 0.01718 -0.00357 AFIX 137 H25A 2 -0.137582 0.176016 0.745247 11.00000 -1.50000 H25B 2 0.013561 0.131838 0.755449 11.00000 -1.50000 H25C 2 -0.049752 0.175094 0.682106 11.00000 -1.50000 AFIX 0 C26 1 0.028038 0.197242 0.524130 11.00000 0.03597 0.03470 = 0.03889 -0.00399 0.00305 -0.00830 AFIX 137 H26A 2 -0.062809 0.226545 0.514810 11.00000 -1.50000 H26B 2 0.044462 0.175846 0.572364 11.00000 -1.50000 H26C 2 0.031008 0.144985 0.492756 11.00000 -1.50000 AFIX 0 C27 1 0.126451 0.290813 0.440228 11.00000 0.04557 0.03995 = 0.02367 0.00295 -0.00403 -0.00044 AFIX 137 H27A 2 0.137719 0.236804 0.411663 11.00000 -1.50000 H27B 2 0.199839 0.335065 0.435669 11.00000 -1.50000 H27C 2 0.036474 0.319049 0.424623 11.00000 -1.50000 AFIX 0 C28 1 -0.030123 0.385610 0.609526 11.00000 0.02476 0.04485 = 0.03457 0.00573 0.00836 0.00708 AFIX 137 H28A 2 -0.054979 0.415926 0.650882 11.00000 -1.50000 H28B 2 -0.044230 0.319384 0.613034 11.00000 -1.50000 H28C 2 -0.088297 0.409234 0.568047 11.00000 -1.50000 AFIX 0 C29 1 0.144733 0.502042 0.604878 11.00000 0.06514 0.02822 = 0.04387 -0.00254 0.02278 -0.00199 AFIX 137 H29A 2 0.082699 0.532187 0.567579 11.00000 -1.50000 H29B 2 0.240623 0.511474 0.597606 11.00000 -1.50000 H29C 2 0.131019 0.528259 0.649716 11.00000 -1.50000 AFIX 0 P1 3 0.221312 0.328676 0.574959 11.00000 0.01861 0.03100 = 0.01903 0.00120 0.00412 -0.00134 CL1 4 0.415303 0.474139 0.410839 11.00000 0.06725 0.09219 = 0.02426 -0.01342 0.01284 -0.05056 AG1 5 0.401659 0.412869 0.532087 11.00000 0.03415 0.06283 = 0.03382 -0.00428 0.01345 -0.01955 N1 6 0.134389 0.263252 0.512906 11.00000 0.02591 0.03091 = 0.02186 0.00175 -0.00042 -0.00129 N2 6 0.114698 0.403928 0.604482 11.00000 0.02749 0.02604 = 0.03083 0.00189 0.00985 -0.00004 HKLF 4 REM shelxt_a.res in P2(1)/c REM R1 = 0.0349 for 6269 Fo > 4sig(Fo) and 0.0554 for all 8407 data REM 308 parameters refined using 0 restraints END WGHT 0.0424 1.3913 REM Highest difference peak 1.039, deepest hole -0.969, 1-sigma level 0.072 Q1 1 0.4750 0.4409 0.4155 11.00000 0.05 1.04 Q2 1 0.3485 0.4199 0.5009 11.00000 0.05 0.44 Q3 1 0.2806 0.3556 0.5673 11.00000 0.05 0.42 Q4 1 0.2117 0.5853 0.5976 11.00000 0.05 0.41 Q5 1 0.0548 0.4006 0.6110 11.00000 0.05 0.38 Q6 1 -0.0256 0.3022 0.7717 11.00000 0.05 0.37 Q7 1 0.2000 0.2640 0.7201 11.00000 0.05 0.36 Q8 1 0.4440 0.1534 0.4761 11.00000 0.05 0.35 Q9 1 0.1821 0.3674 0.5846 11.00000 0.05 0.34 Q10 1 -0.0378 0.3840 0.8026 11.00000 0.05 0.34 Q11 1 0.2135 0.4965 0.5763 11.00000 0.05 0.34 Q12 1 0.4169 0.5003 0.5131 11.00000 0.05 0.34 Q13 1 0.1631 0.4081 0.7857 11.00000 0.05 0.33 Q14 1 0.5812 0.2578 0.4335 11.00000 0.05 0.33 Q15 1 0.5925 0.2868 0.5966 11.00000 0.05 0.33 Q16 1 0.1632 0.2870 0.5490 11.00000 0.05 0.33 Q17 1 0.1757 0.3358 0.7654 11.00000 0.05 0.33 Q18 1 0.5601 0.2827 0.5454 11.00000 0.05 0.33 Q19 1 0.0269 0.1572 0.6399 11.00000 0.05 0.33 Q20 1 0.2688 0.2390 0.6746 11.00000 0.05 0.32 ; _shelx_res_checksum 76363 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -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 0.27608(19) 0.24030(14) 0.64205(9) 0.0274(4) Uani 1 1 d . . . A 1 C2 C 0.3766(2) 0.17774(18) 0.62464(10) 0.0382(5) Uani 1 1 d . . . A 1 C3 C 0.4250(3) 0.1072(2) 0.66963(12) 0.0548(8) Uani 1 1 d . . . A 1 H3 H 0.4886 0.0641 0.6560 0.066 Uiso 1 1 calc R U . A 1 C4 C 0.3819(3) 0.0986(2) 0.73427(12) 0.0527(7) Uani 1 1 d . . . A 1 H4 H 0.4141 0.0495 0.7645 0.063 Uiso 1 1 calc R U . A 1 C5 C 0.2911(2) 0.16297(17) 0.75373(10) 0.0392(5) Uani 1 1 d . . . A 1 H5 H 0.2647 0.1592 0.7987 0.047 Uiso 1 1 calc R U . A 1 C6 C 0.2369(2) 0.23350(14) 0.70907(9) 0.0282(4) Uani 1 1 d . . . A 1 C7 C 0.4493(2) 0.19179(18) 0.56225(10) 0.0403(6) Uani 1 1 d . . . A 1 C8 C 0.5617(2) 0.2529(2) 0.56985(12) 0.0508(7) Uani 1 1 d . . . A 1 C9 C 0.6238(2) 0.2736(3) 0.51112(13) 0.0578(8) Uani 1 1 d . . . A 1 H9 H 0.6971 0.3168 0.5153 0.069 Uiso 1 1 calc R U . A 1 C10 C 0.5818(2) 0.2332(2) 0.44786(13) 0.0511(7) Uani 1 1 d . . . A 1 C11 C 0.4795(3) 0.1668(2) 0.44330(11) 0.0458(6) Uani 1 1 d . . . A 1 H11 H 0.4544 0.1354 0.4005 0.055 Uiso 1 1 calc R U . A 1 C12 C 0.4117(2) 0.14427(18) 0.50003(11) 0.0403(5) Uani 1 1 d . . . A 1 C13 C 0.6181(3) 0.2926(3) 0.63983(13) 0.0652(9) Uani 1 1 d . . . A 1 H13A H 0.6890 0.3383 0.6343 0.098 Uiso 1 1 calc R U . A 1 H13B H 0.6587 0.2435 0.6706 0.098 Uiso 1 1 calc R U . A 1 H13C H 0.5431 0.3218 0.6601 0.098 Uiso 1 1 calc R U . A 1 C14 C 0.6436(3) 0.2624(3) 0.38372(14) 0.0663(9) Uani 1 1 d . . . A 1 H14A H 0.5998 0.3193 0.3652 0.099 Uiso 1 1 calc R U . A 1 H14B H 0.6276 0.2142 0.3483 0.099 Uiso 1 1 calc R U . A 1 H14C H 0.7430 0.2722 0.3964 0.099 Uiso 1 1 calc R U . A 1 C15 C 0.3060(3) 0.06883(18) 0.49278(13) 0.0489(6) Uani 1 1 d . . . A 1 H15A H 0.3523 0.0096 0.4908 0.073 Uiso 1 1 calc R U . A 1 H15B H 0.2409 0.0780 0.4500 0.073 Uiso 1 1 calc R U . A 1 H15C H 0.2558 0.0698 0.5328 0.073 Uiso 1 1 calc R U . A 1 C16 C 0.1470(2) 0.29979(14) 0.74128(9) 0.0268(4) Uani 1 1 d . . . A 1 C17 C 0.2015(2) 0.38456(16) 0.76576(10) 0.0346(4) Uani 1 1 d . . . A 1 C18 C 0.1240(3) 0.44037(16) 0.80359(11) 0.0426(6) Uani 1 1 d . . . A 1 H18 H 0.1610 0.4979 0.8199 0.051 Uiso 1 1 calc R U . A 1 C20 C -0.0047(3) 0.41499(15) 0.81824(12) 0.0409(6) Uani 1 1 d . . . A 1 C21 C -0.0576(2) 0.33162(15) 0.79291(11) 0.0354(5) Uani 1 1 d . . . A 1 H21 H -0.1471 0.3139 0.8011 0.042 Uiso 1 1 calc R U . A 1 C22 C 0.0168(2) 0.27286(13) 0.75565(10) 0.0279(4) Uani 1 1 d . . . A 1 C23 C 0.3437(3) 0.4139(2) 0.75352(13) 0.0510(7) Uani 1 1 d . . . A 1 H23A H 0.3678 0.4720 0.7776 0.076 Uiso 1 1 calc R U . A 1 H23B H 0.3446 0.4220 0.7036 0.076 Uiso 1 1 calc R U . A 1 H23C H 0.4110 0.3669 0.7714 0.076 Uiso 1 1 calc R U . A 1 C24 C -0.0838(4) 0.47535(18) 0.86221(15) 0.0617(9) Uani 1 1 d . . . A 1 H24A H -0.1306 0.5243 0.8333 0.093 Uiso 1 1 calc R U . A 1 H24B H -0.0195 0.5024 0.9001 0.093 Uiso 1 1 calc R U . A 1 H24C H -0.1524 0.4383 0.8816 0.093 Uiso 1 1 calc R U . A 1 C25 C -0.0446(3) 0.18086(15) 0.73258(13) 0.0398(5) Uani 1 1 d . . . A 1 H25A H -0.1376 0.1760 0.7452 0.060 Uiso 1 1 calc R U . A 1 H25B H 0.0136 0.1318 0.7554 0.060 Uiso 1 1 calc R U . A 1 H25C H -0.0498 0.1751 0.6821 0.060 Uiso 1 1 calc R U . A 1 C26 C 0.0280(2) 0.19724(16) 0.52413(12) 0.0368(5) Uani 1 1 d . . . A 1 H26A H -0.0628 0.2265 0.5148 0.055 Uiso 1 1 calc R U . A 1 H26B H 0.0445 0.1758 0.5724 0.055 Uiso 1 1 calc R U . A 1 H26C H 0.0310 0.1450 0.4928 0.055 Uiso 1 1 calc R U . A 1 C27 C 0.1265(2) 0.29081(16) 0.44023(11) 0.0373(5) Uani 1 1 d . . . A 1 H27A H 0.1377 0.2368 0.4117 0.056 Uiso 1 1 calc R U . A 1 H27B H 0.1998 0.3351 0.4357 0.056 Uiso 1 1 calc R U . A 1 H27C H 0.0365 0.3190 0.4246 0.056 Uiso 1 1 calc R U . A 1 C28 C -0.0301(2) 0.38561(16) 0.60953(11) 0.0343(4) Uani 1 1 d . . . A 1 H28A H -0.0550 0.4159 0.6509 0.051 Uiso 1 1 calc R U . A 1 H28B H -0.0442 0.3194 0.6130 0.051 Uiso 1 1 calc R U . A 1 H28C H -0.0883 0.4092 0.5680 0.051 Uiso 1 1 calc R U . A 1 C29 C 0.1447(3) 0.50204(15) 0.60488(13) 0.0443(6) Uani 1 1 d . . . A 1 H29A H 0.0827 0.5322 0.5676 0.066 Uiso 1 1 calc R U . A 1 H29B H 0.2406 0.5115 0.5976 0.066 Uiso 1 1 calc R U . A 1 H29C H 0.1310 0.5283 0.6497 0.066 Uiso 1 1 calc R U . A 1 P1 P 0.22131(5) 0.32868(3) 0.57496(2) 0.02274(10) Uani 1 1 d . . . A 1 Cl1 Cl 0.41530(8) 0.47414(6) 0.41084(3) 0.0606(2) Uani 1 1 d . . . A 1 Ag1 Ag 0.40166(2) 0.41287(2) 0.53209(2) 0.04275(7) Uani 1 1 d . . . A 1 N1 N 0.13439(16) 0.26325(11) 0.51291(8) 0.0266(3) Uani 1 1 d . . . A 1 N2 N 0.11470(17) 0.40393(11) 0.60448(9) 0.0276(3) Uani 1 1 d . . . A 1 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 0.0238(9) 0.0392(11) 0.0196(8) 0.0031(7) 0.0044(7) 0.0073(8) C2 0.0323(10) 0.0628(15) 0.0197(9) 0.0066(9) 0.0045(8) 0.0216(10) C3 0.0600(16) 0.0784(19) 0.0279(11) 0.0132(11) 0.0128(11) 0.0467(15) C4 0.0610(16) 0.0706(18) 0.0276(11) 0.0161(11) 0.0099(11) 0.0393(14) C5 0.0450(12) 0.0531(14) 0.0202(9) 0.0072(9) 0.0070(8) 0.0177(11) C6 0.0259(9) 0.0399(11) 0.0192(8) 0.0017(7) 0.0044(7) 0.0066(8) C7 0.0287(10) 0.0693(16) 0.0236(9) 0.0062(10) 0.0064(8) 0.0254(10) C8 0.0210(10) 0.101(2) 0.0303(11) -0.0005(12) 0.0038(8) 0.0189(12) C9 0.0210(10) 0.115(3) 0.0389(13) -0.0064(14) 0.0100(9) 0.0055(13) C10 0.0273(11) 0.094(2) 0.0358(11) 0.0016(13) 0.0161(9) 0.0166(12) C11 0.0426(13) 0.0717(17) 0.0251(10) -0.0007(10) 0.0116(9) 0.0232(12) C12 0.0391(12) 0.0556(14) 0.0277(10) 0.0064(9) 0.0097(9) 0.0248(11) C13 0.0248(11) 0.136(3) 0.0335(12) -0.0111(15) -0.0009(9) 0.0079(15) C14 0.0435(14) 0.121(3) 0.0393(13) -0.0050(16) 0.0232(11) -0.0005(16) C15 0.0656(17) 0.0464(14) 0.0378(12) 0.0033(10) 0.0177(12) 0.0171(12) C16 0.0317(10) 0.0313(10) 0.0184(8) 0.0025(7) 0.0068(7) 0.0035(8) C17 0.0433(12) 0.0390(11) 0.0222(9) -0.0004(8) 0.0070(8) -0.0048(9) C18 0.0723(17) 0.0282(10) 0.0292(10) -0.0016(8) 0.0143(11) -0.0039(11) C20 0.0666(16) 0.0297(11) 0.0310(10) 0.0071(9) 0.0230(10) 0.0163(10) C21 0.0423(12) 0.0350(11) 0.0334(10) 0.0101(9) 0.0204(9) 0.0116(9) C22 0.0337(10) 0.0267(9) 0.0256(9) 0.0049(7) 0.0116(7) 0.0049(8) C23 0.0486(14) 0.0714(18) 0.0334(12) -0.0114(12) 0.0075(10) -0.0292(13) C24 0.104(2) 0.0376(13) 0.0531(16) 0.0059(12) 0.0435(16) 0.0251(15) C25 0.0441(12) 0.0355(12) 0.0430(12) 0.0015(10) 0.0172(10) -0.0036(10) C26 0.0360(11) 0.0347(11) 0.0389(11) -0.0040(9) 0.0031(9) -0.0083(9) C27 0.0456(12) 0.0399(12) 0.0237(9) 0.0029(8) -0.0040(9) -0.0004(10) C28 0.0248(9) 0.0448(12) 0.0346(10) 0.0057(9) 0.0084(8) 0.0071(8) C29 0.0651(16) 0.0282(11) 0.0439(13) -0.0025(9) 0.0228(12) -0.0020(11) P1 0.0186(2) 0.0310(2) 0.0190(2) 0.00120(18) 0.00412(16) -0.00134(18) Cl1 0.0673(4) 0.0922(5) 0.0243(2) -0.0134(3) 0.0128(3) -0.0506(4) Ag1 0.03415(10) 0.06283(13) 0.03382(9) -0.00428(8) 0.01345(7) -0.01955(8) N1 0.0259(8) 0.0309(8) 0.0219(7) 0.0017(6) -0.0004(6) -0.0013(6) N2 0.0275(8) 0.0260(8) 0.0308(8) 0.0019(6) 0.0098(6) 0.0000(6) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 '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' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C6 C1 C2 117.79(17) . . ? C6 C1 P1 127.35(15) . . ? C2 C1 P1 114.67(14) . . ? C3 C2 C1 120.70(19) . . ? C3 C2 C7 116.74(19) . . ? C1 C2 C7 122.05(19) . . ? C2 C3 C4 121.1(2) . . ? C2 C3 H3 119.4 . . ? C4 C3 H3 119.4 . . ? C5 C4 C3 118.6(2) . . ? C5 C4 H4 120.7 . . ? C3 C4 H4 120.7 . . ? C4 C5 C6 121.96(19) . . ? C4 C5 H5 119.0 . . ? C6 C5 H5 119.0 . . ? C5 C6 C1 119.59(18) . . ? C5 C6 C16 113.91(16) . . ? C1 C6 C16 126.36(17) . . ? C12 C7 C8 120.5(2) . . ? C12 C7 C2 122.3(2) . . ? C8 C7 C2 117.1(2) . . ? C9 C8 C7 118.4(2) . . ? C9 C8 C13 120.5(3) . . ? C7 C8 C13 121.0(2) . . ? C10 C9 C8 121.9(3) . . ? C10 C9 H9 119.0 . . ? C8 C9 H9 119.0 . . ? C9 C10 C11 118.4(2) . . ? C9 C10 C14 120.8(3) . . ? C11 C10 C14 120.8(2) . . ? C10 C11 C12 122.1(2) . . ? C10 C11 H11 118.9 . . ? C12 C11 H11 118.9 . . ? C7 C12 C11 118.0(2) . . ? C7 C12 C15 122.3(2) . . ? C11 C12 C15 119.6(2) . . ? 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 . . ? C22 C16 C17 119.45(18) . . ? C22 C16 C6 120.53(18) . . ? C17 C16 C6 119.43(18) . . ? C18 C17 C16 119.0(2) . . ? C18 C17 C23 120.3(2) . . ? C16 C17 C23 120.7(2) . . ? C20 C18 C17 122.4(2) . . ? C20 C18 H18 118.8 . . ? C17 C18 H18 118.8 . . ? C18 C20 C21 117.8(2) . . ? C18 C20 C24 121.1(2) . . ? C21 C20 C24 121.0(2) . . ? C20 C21 C22 121.9(2) . . ? C20 C21 H21 119.1 . . ? C22 C21 H21 119.1 . . ? C21 C22 C16 119.43(19) . . ? C21 C22 C25 118.97(19) . . ? C16 C22 C25 121.60(17) . . ? C17 C23 H23A 109.5 . . ? C17 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C17 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C20 C24 H24A 109.5 . . ? C20 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C20 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C22 C25 H25A 109.5 . . ? C22 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C22 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 . . ? N1 C27 H27A 109.5 . . ? N1 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? N1 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 . . ? N2 C29 H29A 109.5 . . ? N2 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? N2 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? N1 P1 N2 110.20(9) . . ? N1 P1 C1 100.10(9) . . ? N2 P1 C1 110.15(8) . . ? N1 P1 Ag1 111.36(6) . . ? N2 P1 Ag1 108.16(6) . . ? C1 P1 Ag1 116.64(6) . . ? Ag1 Cl1 Ag1 87.291(19) . 3_666 ? P1 Ag1 Cl1 130.064(19) . . ? P1 Ag1 Cl1 132.984(18) . 3_666 ? Cl1 Ag1 Cl1 92.708(19) . 3_666 ? C26 N1 C27 112.88(16) . . ? C26 N1 P1 124.63(14) . . ? C27 N1 P1 119.43(14) . . ? C28 N2 C29 112.06(18) . . ? C28 N2 P1 124.32(14) . . ? C29 N2 P1 120.60(15) . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C6 1.416(2) . ? C1 C2 1.419(3) . ? C1 P1 1.858(2) . ? C2 C3 1.389(3) . ? C2 C7 1.509(3) . ? C3 C4 1.390(3) . ? C3 H3 0.9500 . ? C4 C5 1.384(3) . ? C4 H4 0.9500 . ? C5 C6 1.400(3) . ? C5 H5 0.9500 . ? C6 C16 1.505(3) . ? C7 C12 1.397(3) . ? C7 C8 1.408(4) . ? C8 C9 1.404(3) . ? C8 C13 1.508(4) . ? C9 C10 1.373(4) . ? C9 H9 0.9500 . ? C10 C11 1.388(4) . ? C10 C14 1.525(3) . ? C11 C12 1.408(3) . ? C11 H11 0.9500 . ? C12 C15 1.504(4) . ? 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 C22 1.402(3) . ? C16 C17 1.403(3) . ? C17 C18 1.395(3) . ? C17 C23 1.510(3) . ? C18 C20 1.383(4) . ? C18 H18 0.9500 . ? C20 C21 1.384(3) . ? C20 C24 1.518(3) . ? C21 C22 1.395(3) . ? C21 H21 0.9500 . ? C22 C25 1.512(3) . ? 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 N1 1.459(3) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 N1 1.462(3) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 N2 1.461(3) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 N2 1.461(3) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? P1 N1 1.6714(17) . ? P1 N2 1.6742(17) . ? P1 Ag1 2.3999(5) . ? Cl1 Ag1 2.5454(6) . ? Cl1 Ag1 2.5657(6) 3_666 ? Ag1 Cl1 2.5658(6) 3_666 ? 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 5.7(4) . . . . ? P1 C1 C2 C3 -178.9(2) . . . . ? C6 C1 C2 C7 -165.8(2) . . . . ? P1 C1 C2 C7 9.6(3) . . . . ? C1 C2 C3 C4 -3.3(5) . . . . ? C7 C2 C3 C4 168.7(3) . . . . ? C2 C3 C4 C5 -1.2(5) . . . . ? C3 C4 C5 C6 3.0(4) . . . . ? C4 C5 C6 C1 -0.5(4) . . . . ? C4 C5 C6 C16 -176.5(2) . . . . ? C2 C1 C6 C5 -3.9(3) . . . . ? P1 C1 C6 C5 -178.56(17) . . . . ? C2 C1 C6 C16 171.6(2) . . . . ? P1 C1 C6 C16 -3.1(3) . . . . ? C3 C2 C7 C12 87.0(3) . . . . ? C1 C2 C7 C12 -101.2(3) . . . . ? C3 C2 C7 C8 -90.6(3) . . . . ? C1 C2 C7 C8 81.2(3) . . . . ? C12 C7 C8 C9 7.8(4) . . . . ? C2 C7 C8 C9 -174.5(2) . . . . ? C12 C7 C8 C13 -169.8(2) . . . . ? C2 C7 C8 C13 7.9(4) . . . . ? C7 C8 C9 C10 -2.7(4) . . . . ? C13 C8 C9 C10 174.9(3) . . . . ? C8 C9 C10 C11 -3.3(4) . . . . ? C8 C9 C10 C14 175.3(3) . . . . ? C9 C10 C11 C12 4.4(4) . . . . ? C14 C10 C11 C12 -174.1(2) . . . . ? C8 C7 C12 C11 -6.7(3) . . . . ? C2 C7 C12 C11 175.7(2) . . . . ? C8 C7 C12 C15 171.2(2) . . . . ? C2 C7 C12 C15 -6.4(3) . . . . ? C10 C11 C12 C7 0.6(3) . . . . ? C10 C11 C12 C15 -177.4(2) . . . . ? C5 C6 C16 C22 -70.5(3) . . . . ? C1 C6 C16 C22 113.8(2) . . . . ? C5 C6 C16 C17 100.7(2) . . . . ? C1 C6 C16 C17 -75.0(3) . . . . ? C22 C16 C17 C18 -0.4(3) . . . . ? C6 C16 C17 C18 -171.66(19) . . . . ? C22 C16 C17 C23 177.6(2) . . . . ? C6 C16 C17 C23 6.4(3) . . . . ? C16 C17 C18 C20 0.3(3) . . . . ? C23 C17 C18 C20 -177.7(2) . . . . ? C17 C18 C20 C21 -1.2(4) . . . . ? C17 C18 C20 C24 177.3(2) . . . . ? C18 C20 C21 C22 2.1(3) . . . . ? C24 C20 C21 C22 -176.4(2) . . . . ? C20 C21 C22 C16 -2.1(3) . . . . ? C20 C21 C22 C25 177.0(2) . . . . ? C17 C16 C22 C21 1.3(3) . . . . ? C6 C16 C22 C21 172.43(17) . . . . ? C17 C16 C22 C25 -177.91(19) . . . . ? C6 C16 C22 C25 -6.7(3) . . . . ? C6 C1 P1 N1 -115.82(19) . . . . ? C2 C1 P1 N1 69.35(18) . . . . ? C6 C1 P1 N2 0.2(2) . . . . ? C2 C1 P1 N2 -174.61(16) . . . . ? C6 C1 P1 Ag1 123.96(17) . . . . ? C2 C1 P1 Ag1 -50.86(19) . . . . ? N2 P1 N1 C26 -66.35(18) . . . . ? C1 P1 N1 C26 49.65(18) . . . . ? Ag1 P1 N1 C26 173.62(15) . . . . ? N2 P1 N1 C27 92.44(17) . . . . ? C1 P1 N1 C27 -151.56(16) . . . . ? Ag1 P1 N1 C27 -27.60(17) . . . . ? N1 P1 N2 C28 33.35(18) . . . . ? C1 P1 N2 C28 -76.17(18) . . . . ? Ag1 P1 N2 C28 155.29(14) . . . . ? N1 P1 N2 C29 -125.44(18) . . . . ? C1 P1 N2 C29 125.04(18) . . . . ? Ag1 P1 N2 C29 -3.50(19) . . . . ?