#------------------------------------------------------------------------------ #$Date: 2025-05-14 02:59:23 +0100 (Wed, 14 May 2025) $ #$Revision: 299652 $ #$URL: svn://www.crystallography.net/cod/cif/2/02/35/2023502.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2023502 loop_ _publ_author_name 'Bosch, Eric' _publ_section_title ; Phenyl palladium(II) iodide complexes isolated after Sonogashira coupling of iodobenzenes with terminal alkynes ; _journal_coeditor_code JY2058 _journal_issue 6 _journal_name_full 'Acta Crystallographica Section E Crystallographic Communications' _journal_paper_doi 10.1107/S2056989025004025 _journal_volume 81 _journal_year 2025 _chemical_formula_iupac '[Pd (C6 H2 F3) I (C18 H15 P)2]' _chemical_formula_moiety 'C42 H32 F3 I P2 Pd' _chemical_formula_sum 'C42 H32 F3 I P2 Pd' _chemical_formula_weight 888.985 _space_group_crystal_system monoclinic _space_group_IT_number 15 _space_group_name_Hall '-I 2ya' _space_group_name_H-M_alt 'I 1 2/a 1' _atom_sites_solution_primary dual _audit_creation_method ; Olex2 1.5 (compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498) ; _cell_angle_alpha 90 _cell_angle_beta 93.218(2) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 11.6327(5) _cell_length_b 12.8059(5) _cell_length_c 23.4327(9) _cell_measurement_reflns_used 9946 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 27.17 _cell_measurement_theta_min 2.37 _cell_volume 3485.2(2) _computing_molecular_graphics ; X-SEED 4 (Barbour, 2020) ; _computing_publication_material ; Olex2 1.5 (Dolomanov et al., 2009) ; _computing_structure_refinement ; olex2.refine 1.5 (Bourhis et al., 2015) ; _computing_structure_solution ; SHELXT (Sheldrick, 2015) ; _diffrn_ambient_temperature 100.15 _diffrn_measured_fraction_theta_full 0.9994 _diffrn_measured_fraction_theta_max 0.9979 _diffrn_measurement_device_type 'Bruker APEXI CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0175 _diffrn_reflns_av_unetI/netI 0.0114 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_number 22427 _diffrn_reflns_theta_full 25.2417 _diffrn_reflns_theta_max 27.18 _diffrn_reflns_theta_min 1.74 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 1.557 _exptl_absorpt_correction_T_max 0.7455 _exptl_absorpt_correction_T_min 0.7049 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (SADABS; Krause et al., 2015) ; _exptl_crystal_colour 'clear orange' _exptl_crystal_density_diffrn 1.694 _exptl_crystal_description irregular _exptl_crystal_F_000 1756.204 _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.272 _exptl_crystal_size_min 0.232 _refine_diff_density_max 2.0511 _refine_diff_density_min -1.1175 _refine_ls_goodness_of_fit_ref 1.0523 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_constraints 39 _refine_ls_number_parameters 229 _refine_ls_number_reflns 3875 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.0523 _refine_ls_R_factor_all 0.0223 _refine_ls_R_factor_gt 0.0214 _refine_ls_shift/su_max -0.0006 _refine_ls_shift/su_mean 0.0000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0197P)^2^+13.0801P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0515 _refine_ls_wR_factor_ref 0.0522 _reflns_number_gt 3735 _reflns_number_total 3875 _reflns_threshold_expression I>=2u(I) _iucr_refine_instructions_details ; TITL eb445 in C2/c New: I2/a CELL 0.71073 11.6327 12.8059 23.4327 90 93.218 90 ZERR 4 0.0005 0.0005 0.0009 0 0.002 0 LATT 2 SYMM 0.5-X,+Y,-Z SFAC C H F I P Pd UNIT 168 128 12 4 8 4 EQIV $1 -0.5+X,-Y,+Z EADP C1 C4 EADP C2 C2A EADP C3 C3A EXYZ C2 C2A EXYZ C3 C3A L.S. 20 PLAN 10 0 0 TEMP -173 CONF HTAB C6 I1 HTAB C16 F2_$1 BOND $H ACTA FMAP 2 1 53 GRID HTAB 2.0 LIST 4 1 MORE -1 MERG 2 OMIT -2 1 1 OMIT 0 1 3 WGHT 0.01973 13.080089 FVAR 0.047539 REM REM REM Pd1 6 0.75000 0.23697 0.00000 10.50000 0.01480 0.01060 0.00714 = 0.00000 0.00076 -0.00000 I1 4 0.75000 0.44615 0.00000 10.50000 0.02728 0.01232 0.01457 = 0.00000 0.00294 -0.00000 P1 5 0.72633 0.23781 -0.09914 11.00000 0.01256 0.01298 0.00819 = -0.00025 0.00100 0.00102 PART 1 F1 3 0.92689 0.06910 -0.04020 10.50000 0.01747 0.02581 0.02654 = 0.00150 0.00300 0.00127 PART 0 C1 1 0.75000 0.07371 0.00000 10.50000 0.04066 0.02935 0.01066 = 0.00000 -0.00449 -0.00000 PART 1 F2 3 0.92579 -0.13966 -0.03982 10.50000 0.03611 0.02416 0.04720 = -0.00154 0.00927 0.01113 C2 1 0.83766 0.02354 -0.01838 10.50000 0.03257 0.02227 0.01854 = 0.01492 -0.01788 -0.00976 PART 0 F3 3 0.75000 -0.24706 0.00000 10.50000 0.06354 0.01499 0.04862 = 0.00000 0.01285 -0.00000 PART 1 C3 1 0.84184 -0.08796 -0.02042 10.50000 0.03525 0.01992 0.02320 = -0.00182 0.00134 0.00724 PART 0 C4 1 0.75000 -0.14116 0.00000 10.50000 0.04066 0.02935 0.01066 = 0.00000 -0.00449 -0.00000 C5 1 0.58866 0.28796 -0.12888 11.00000 0.01433 0.01207 0.01504 = 0.00219 -0.00038 0.00037 C6 1 0.51028 0.33479 -0.09401 11.00000 0.01756 0.01689 0.01745 = -0.00030 0.00349 -0.00133 AFIX 43 H6 2 0.53051 0.34601 -0.05465 11.00000 -1.20000 AFIX 0 C7 1 0.40197 0.36523 -0.11691 11.00000 0.01595 0.01925 0.03159 = -0.00248 0.00509 0.00245 AFIX 43 H7 2 0.34844 0.39684 -0.09309 11.00000 -1.20000 AFIX 0 C8 1 0.37264 0.34931 -0.17438 11.00000 0.01512 0.01554 0.03442 = 0.00266 -0.00435 0.00103 AFIX 43 H8 2 0.29915 0.37059 -0.18991 11.00000 -1.20000 AFIX 0 C9 1 0.45004 0.30242 -0.20941 11.00000 0.02005 0.01758 0.01979 = 0.00199 -0.00562 -0.00053 AFIX 43 H9 2 0.42961 0.29169 -0.24880 11.00000 -1.20000 AFIX 0 C10 1 0.55753 0.27125 -0.18665 11.00000 0.01682 0.01654 0.01579 = 0.00020 0.00054 0.00186 AFIX 43 H10 2 0.61015 0.23839 -0.21050 11.00000 -1.20000 AFIX 0 C11 1 0.73091 0.11054 -0.13442 11.00000 0.01571 0.01459 0.00967 = -0.00156 -0.00307 0.00373 C12 1 0.82437 0.07795 -0.16450 11.00000 0.01714 0.02282 0.01433 = -0.00249 0.00039 0.00222 AFIX 43 H12 2 0.88437 0.12567 -0.17173 11.00000 -1.20000 AFIX 0 C13 1 0.82994 -0.02488 -0.18406 11.00000 0.02014 0.02857 0.01983 = -0.00892 -0.00096 0.00947 AFIX 43 H13 2 0.89408 -0.04698 -0.20434 11.00000 -1.20000 AFIX 0 C14 1 0.74276 -0.09460 -0.17409 11.00000 0.02631 0.01988 0.02529 = -0.00993 -0.01010 0.00816 AFIX 43 H14 2 0.74764 -0.16478 -0.18687 11.00000 -1.20000 AFIX 0 C15 1 0.64770 -0.06188 -0.14527 11.00000 0.02030 0.01739 0.02506 = -0.00273 -0.00709 0.00028 AFIX 43 H15 2 0.58697 -0.10942 -0.13905 11.00000 -1.20000 AFIX 0 C16 1 0.64151 0.04002 -0.12563 11.00000 0.01579 0.01872 0.01586 = -0.00171 -0.00106 0.00181 AFIX 43 H16 2 0.57635 0.06211 -0.10612 11.00000 -1.20000 AFIX 0 C17 1 0.84344 0.31007 -0.12955 11.00000 0.01610 0.01472 0.01167 = -0.00211 0.00339 -0.00032 C18 1 0.83228 0.36272 -0.18177 11.00000 0.02058 0.01598 0.01376 = -0.00145 0.00223 0.00005 AFIX 43 H18 2 0.76010 0.36412 -0.20284 11.00000 -1.20000 AFIX 0 C19 1 0.92721 0.41326 -0.20295 11.00000 0.02915 0.01632 0.01767 = 0.00026 0.00860 -0.00131 AFIX 43 H19 2 0.91967 0.44869 -0.23858 11.00000 -1.20000 AFIX 0 C20 1 1.03256 0.41195 -0.17216 11.00000 0.02225 0.02080 0.02710 = -0.00402 0.01216 -0.00469 AFIX 43 H20 2 1.09673 0.44704 -0.18663 11.00000 -1.20000 AFIX 0 C21 1 1.04467 0.35962 -0.12031 11.00000 0.01599 0.02711 0.02698 = -0.00504 0.00325 -0.00207 AFIX 43 H21 2 1.11705 0.35847 -0.09942 11.00000 -1.20000 AFIX 0 C22 1 0.95025 0.30879 -0.09903 11.00000 0.01742 0.02276 0.01577 = 0.00036 0.00115 -0.00027 AFIX 43 H22 2 0.95847 0.27299 -0.06353 11.00000 -1.20000 AFIX 0 PART 2 C2A 1 0.83766 0.02354 -0.01838 10.50000 0.03257 0.02227 0.01854 = 0.01492 -0.01788 -0.00976 AFIX 43 H2A 2 0.90118 0.06228 -0.03091 10.50000 -1.20000 AFIX 0 C3A 1 0.84184 -0.08796 -0.02042 10.50000 0.03525 0.01992 0.02320 = -0.00182 0.00134 0.00724 AFIX 43 H3A 2 0.90523 -0.12371 -0.03523 10.50000 -1.20000 AFIX 0 HKLF 4 1 0 0 1 0 1 0 -1 0 -1 END Q1 1 0.75 0.022222 0 11 0.05 2.05 Q2 1 0.85 -0.011111 -0.0125 11 0.05 0.78 Q4 1 0.775 0.277778 -0.1125 11 0.05 0.39 Q7 1 0.725 0.166667 -0.125 11 0.05 0.34 Q8 1 0.85 0.344444 -0.15 11 0.05 0.34 Q9 1 0.65 0.266667 -0.1125 11 0.05 0.34 Q6 1 0.7 0.066667 -0.125 11 0.05 0.35 Q10 1 0.975 0.411111 -0.1875 11 0.05 0.33 Q3 1 0.75 -0.133333 -0.025 11 0.05 0.46 Q5 1 0.5 0.277778 -0.1875 11 0.05 0.36 REM The information below was added by Olex2. REM REM R1 = 0.0214 for 3735 Fo > 4sig(Fo) and 0.0223 for all 3875 data REM 229 parameters refined using 0 restraints REM Highest difference peak 2.0511, deepest hole -1.1175 REM Mean Shift 0.0000, Max Shift -0.0006. REM +++ Tabular Listing of Refinement Information +++ REM R1_all = 0.0223 REM R1_gt = 0.0214 REM wR_ref = 0.0522 REM GOOF = 1.0523 REM Shift_max = -0.0006 REM Shift_mean = 0.0000 REM Reflections_all = 3875 REM Reflections_gt = 3735 REM Parameters = 229 REM Hole = -1.1175 REM Peak = 2.0511 REM Flack = n/a ; _cod_data_source_file jy2058.cif _cod_data_source_block 3 _cod_original_sg_symbol_Hall '-C 2yc' _cod_original_sg_symbol_H-M 'I 2/a' _cod_database_code 2023502 loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 x,y,z 2 -x+1/2,y,-z 3 -x,-y,-z 4 x-1/2,-y,z 5 x+1/2,y+1/2,z+1/2 6 -x+1,y+1/2,-z+1/2 7 -x+1/2,-y+1/2,-z+1/2 8 x,-y+1/2,z+1/2 loop_ _atom_site_type_symbol _atom_site_label _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_disorder_group Pd Pd1 0.75 0.236973(16) 0.0 0.01084(6) Uani 1.000000 . I I1 0.75 0.446148(14) 0.0 0.01799(6) Uani 1.000000 . P P1 0.72633(4) 0.23781(4) -0.09914(2) 0.01123(10) Uani 1.000000 . F F1 0.9269(2) 0.0691(2) -0.04020(11) 0.0232(5) Uani 0.500000 1 C C1 0.75 0.0737(3) 0.0 0.0271(5) Uani 1.000000 . F F2 0.9258(3) -0.1397(2) -0.03982(14) 0.0356(7) Uani 0.500000 1 C C2 0.8377(2) 0.02354(18) -0.01838(9) 0.0252(5) Uani 0.500000 1 F F3 0.75 -0.24706(16) 0.0 0.0420(6) Uani 1.000000 . C C3 0.8418(2) -0.08796(19) -0.02042(10) 0.0261(5) Uani 0.500000 1 C C4 0.75 -0.1412(3) 0.0 0.0271(5) Uani 1.000000 . C C5 0.58866(17) 0.28796(15) -0.12888(8) 0.0139(4) Uani 1.000000 . C C6 0.51028(18) 0.33479(16) -0.09401(9) 0.0172(4) Uani 1.000000 . H H6 0.53051(18) 0.34601(16) -0.05465(9) 0.0207(5) Uiso 1.000000 . C C7 0.40197(19) 0.36523(18) -0.11691(10) 0.0221(4) Uani 1.000000 . H H7 0.34844(19) 0.39684(18) -0.09309(10) 0.0265(5) Uiso 1.000000 . C C8 0.37264(19) 0.34931(17) -0.17438(11) 0.0219(5) Uani 1.000000 . H H8 0.29915(19) 0.37059(17) -0.18991(11) 0.0263(5) Uiso 1.000000 . C C9 0.45004(18) 0.30242(17) -0.20941(9) 0.0194(4) Uani 1.000000 . H H9 0.42961(18) 0.29169(17) -0.24880(9) 0.0233(5) Uiso 1.000000 . C C10 0.55753(18) 0.27125(16) -0.18665(9) 0.0164(4) Uani 1.000000 . H H10 0.61015(18) 0.23839(16) -0.21050(9) 0.0197(5) Uiso 1.000000 . C C11 0.73091(17) 0.11054(16) -0.13442(8) 0.0135(4) Uani 1.000000 . C C12 0.82437(18) 0.07795(17) -0.16450(9) 0.0181(4) Uani 1.000000 . H H12 0.88437(18) 0.12567(17) -0.17173(9) 0.0217(5) Uiso 1.000000 . C C13 0.82994(19) -0.02488(19) -0.18406(9) 0.0229(5) Uani 1.000000 . H H13 0.89408(19) -0.04698(19) -0.20434(9) 0.0275(5) Uiso 1.000000 . C C14 0.7428(2) -0.09460(18) -0.17409(10) 0.0243(5) Uani 1.000000 . H H14 0.7476(2) -0.16478(18) -0.18687(10) 0.0291(6) Uiso 1.000000 . C C15 0.64770(19) -0.06188(17) -0.14527(10) 0.0212(4) Uani 1.000000 . H H15 0.58697(19) -0.10942(17) -0.13905(10) 0.0255(5) Uiso 1.000000 . C C16 0.64151(18) 0.04002(16) -0.12563(9) 0.0169(4) Uani 1.000000 . H H16 0.57635(18) 0.06211(16) -0.10612(9) 0.0202(5) Uiso 1.000000 . C C17 0.84344(17) 0.31007(16) -0.12955(8) 0.0141(4) Uani 1.000000 . C C18 0.83228(18) 0.36272(16) -0.18177(9) 0.0167(4) Uani 1.000000 . H H18 0.76010(18) 0.36412(16) -0.20284(9) 0.0201(5) Uiso 1.000000 . C C19 0.9272(2) 0.41326(17) -0.20295(9) 0.0208(4) Uani 1.000000 . H H19 0.9197(2) 0.44869(17) -0.23858(9) 0.0249(5) Uiso 1.000000 . C C20 1.0326(2) 0.41195(18) -0.17216(10) 0.0230(5) Uani 1.000000 . H H20 1.0967(2) 0.44704(18) -0.18663(10) 0.0276(5) Uiso 1.000000 . C C21 1.04467(19) 0.35962(19) -0.12031(10) 0.0233(5) Uani 1.000000 . H H21 1.11705(19) 0.35847(19) -0.09942(10) 0.0279(5) Uiso 1.000000 . C C22 0.95025(18) 0.30879(18) -0.09903(9) 0.0186(4) Uani 1.000000 . H H22 0.95847(18) 0.27299(18) -0.06353(9) 0.0224(5) Uiso 1.000000 . C C2A 0.8377(2) 0.02354(18) -0.01838(9) 0.0252(5) Uani 0.500000 2 H H2A 0.9012(2) 0.06228(18) -0.03091(9) 0.0302(6) Uiso 0.500000 2 C C3A 0.8418(2) -0.08796(19) -0.02042(10) 0.0261(5) Uani 0.500000 2 H H3A 0.9052(2) -0.12371(19) -0.03523(10) 0.0314(6) Uiso 0.500000 2 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 Pd1 0.01480(10) 0.01060(10) 0.00714(10) -0.000000 0.00076(7) 0.000000 I1 0.02728(11) 0.01232(9) 0.01457(9) -0.000000 0.00294(7) 0.000000 P1 0.0126(2) 0.0130(2) 0.0082(2) 0.00102(18) 0.00100(17) -0.00025(17) F1 0.0175(12) 0.0258(14) 0.0265(14) 0.0013(10) 0.0030(10) 0.0015(11) C1 0.0407(14) 0.0293(12) 0.0107(10) -0.000000 -0.0045(9) 0.000000 F2 0.0361(16) 0.0242(15) 0.0472(19) 0.0111(13) 0.0093(14) -0.0015(13) C2 0.0326(12) 0.0223(11) 0.0185(10) -0.0098(9) -0.0179(9) 0.0149(9) F3 0.0635(16) 0.0150(10) 0.0486(14) -0.000000 0.0128(12) 0.000000 C3 0.0353(13) 0.0199(11) 0.0232(11) 0.0072(10) 0.0013(10) -0.0018(9) C4 0.0407(14) 0.0293(12) 0.0107(10) -0.000000 -0.0045(9) 0.000000 C5 0.0143(9) 0.0121(9) 0.0150(9) 0.0004(7) -0.0004(7) 0.0022(7) C6 0.0176(10) 0.0169(10) 0.0175(10) -0.0013(8) 0.0035(8) -0.0003(8) C7 0.0159(10) 0.0193(10) 0.0316(12) 0.0024(8) 0.0051(9) -0.0025(9) C8 0.0151(10) 0.0155(10) 0.0344(12) 0.0010(8) -0.0043(9) 0.0027(9) C9 0.0201(10) 0.0176(10) 0.0198(10) -0.0005(8) -0.0056(8) 0.0020(8) C10 0.0168(10) 0.0165(10) 0.0158(10) 0.0019(8) 0.0005(8) 0.0002(8) C11 0.0157(9) 0.0146(9) 0.0097(8) 0.0037(7) -0.0031(7) -0.0016(7) C12 0.0171(10) 0.0228(11) 0.0143(9) 0.0022(8) 0.0004(8) -0.0025(8) C13 0.0201(10) 0.0286(12) 0.0198(10) 0.0095(9) -0.0010(8) -0.0089(9) C14 0.0263(11) 0.0199(11) 0.0253(11) 0.0082(9) -0.0101(9) -0.0099(9) C15 0.0203(10) 0.0174(10) 0.0251(11) 0.0003(8) -0.0071(8) -0.0027(8) C16 0.0158(9) 0.0187(10) 0.0159(9) 0.0018(8) -0.0011(7) -0.0017(8) C17 0.0161(9) 0.0147(9) 0.0117(9) -0.0003(7) 0.0034(7) -0.0021(7) C18 0.0206(10) 0.0160(9) 0.0138(9) 0.0001(8) 0.0022(8) -0.0014(8) C19 0.0291(11) 0.0163(10) 0.0177(10) -0.0013(9) 0.0086(8) 0.0003(8) C20 0.0222(11) 0.0208(11) 0.0271(11) -0.0047(9) 0.0122(9) -0.0040(9) C21 0.0160(10) 0.0271(12) 0.0270(11) -0.0021(9) 0.0033(9) -0.0050(9) C22 0.0174(10) 0.0228(11) 0.0158(10) -0.0003(8) 0.0012(8) 0.0004(8) C2A 0.0326(12) 0.0223(11) 0.0185(10) -0.0098(9) -0.0179(9) 0.0149(9) C3A 0.0353(13) 0.0199(11) 0.0232(11) 0.0072(10) 0.0013(10) -0.0018(9) loop_ _atom_type_symbol _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_dispersion_source _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 2.31000 1.02000 1.58860 0.86500 20.84390 10.20750 0.56870 51.65120 0.21560 'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2' 0.00347 0.00161 'International Tables Volume C Table 6.1.1.4 (pp. 500-502)' F 3.53920 2.64120 1.51700 1.02430 10.28250 4.29440 0.26150 26.14760 0.27760 'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2' 0.01794 0.01033 'International Tables Volume C Table 6.1.1.4 (pp. 500-502)' H 0.49300 0.32291 0.14019 0.04081 10.51090 26.12570 3.14236 57.79970 0.00304 'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2' 0.00000 0.00000 'International Tables Volume C Table 6.1.1.4 (pp. 500-502)' I 20.14720 18.99490 7.51380 2.27350 4.34700 0.38140 27.76600 66.87760 4.07120 'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2' -0.41187 1.83264 'International Tables Volume C Table 6.1.1.4 (pp. 500-502)' P 6.43450 4.17910 1.78000 1.49080 1.90670 27.15700 0.52600 68.16450 1.11490 'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2' 0.10434 0.09671 'International Tables Volume C Table 6.1.1.4 (pp. 500-502)' Pd 19.33190 15.50170 5.29537 0.60584 0.69866 7.98929 25.20520 76.89860 5.26593 'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2' -0.98845 1.01473 'International Tables Volume C Table 6.1.1.4 (pp. 500-502)' loop_ _diffrn_refln_index_h _diffrn_refln_index_k _diffrn_refln_index_l 2 0 0 2 0 0 2 0 0 2 0 0 4 0 0 4 0 0 4 0 0 4 0 0 6 0 0 6 0 0 6 0 0 6 0 0 8 0 0 8 0 0 8 0 0 8 0 0 10 0 0 10 0 0 10 0 0 10 0 0 12 0 0 12 0 0 12 0 0 12 0 0 14 0 0 14 0 0 -14 0 0 14 0 0 16 0 0 -16 0 0 16 0 0 16 0 0 -18 0 0 18 0 0 18 0 0 18 0 0 20 0 0 20 0 0 -20 0 0 -20 0 0 22 0 0 22 0 0 -22 0 0 -22 0 0 24 0 0 24 0 0 -24 0 0 26 0 0 -26 0 0 28 0 0 -28 0 0 -30 0 0 30 0 0 -1 -1 0 1 -1 0 -1 -1 0 1 -1 0 1 1 0 -1 1 0 1 1 0 -1 1 0 3 -1 0 3 -1 0 3 -1 0 -3 -1 0 -3 -1 0 3 -1 0 3 1 0 3 1 0 5 -1 0 5 -1 0 5 -1 0 5 -1 0 -5 -1 0 5 1 0 5 1 0 -7 -1 0 7 -1 0 7 -1 0 7 -1 0 7 -1 0 7 1 0 7 1 0 7 1 0 9 -1 0 9 -1 0 9 -1 0 9 -1 0 -9 -1 0 9 1 0 9 1 0 9 1 0 11 -1 0 11 -1 0 -11 -1 0 11 -1 0 11 -1 0 11 1 0 11 1 0 11 1 0 13 -1 0 13 -1 0 13 -1 0 -13 -1 0 13 -1 0 13 1 0 13 1 0 13 1 0 15 -1 0 15 -1 0 -15 -1 0 15 -1 0 -15 -1 0 15 -1 0 15 1 0 15 1 0 -17 -1 0 -17 -1 0 17 -1 0 17 -1 0 17 -1 0 17 -1 0 17 1 0 17 1 0 -19 -1 0 -19 -1 0 19 -1 0 19 -1 0 19 -1 0 -19 1 0 19 1 0 19 1 0 21 -1 0 -21 -1 0 21 -1 0 21 -1 0 -21 -1 0 -21 1 0 21 1 0 21 1 0 23 -1 0 -23 -1 0 23 -1 0 -23 1 0 -23 1 0 23 1 0 23 1 0 25 -1 0 25 -1 0 -25 -1 0 -25 1 0 25 1 0 -27 -1 0 27 -1 0 -27 1 0 27 1 0 29 -1 0 -29 -1 0 -29 1 0 29 1 0 0 -2 0 0 -2 0 0 2 0 0 2 0 2 -2 0 2 -2 0 -2 -2 0 -2 -2 0 2 2 0 -2 2 0 -2 2 0 2 2 0 4 -2 0 4 -2 0 -4 -2 0 -4 -2 0 4 -2 0 4 -2 0 4 2 0 4 2 0 6 -2 0 -6 -2 0 6 -2 0 6 -2 0 6 -2 0 -6 -2 0 6 2 0 6 2 0 -8 -2 0 8 -2 0 -8 -2 0 8 -2 0 8 -2 0 8 -2 0 8 2 0 8 2 0 10 -2 0 -10 -2 0 10 -2 0 10 -2 0 10 -2 0 -10 -2 0 10 2 0 10 2 0 12 -2 0 12 -2 0 12 -2 0 -12 -2 0 12 -2 0 -12 -2 0 12 2 0 12 2 0 14 -2 0 14 -2 0 14 -2 0 -14 -2 0 -14 -2 0 14 -2 0 14 2 0 14 2 0 16 -2 0 -16 -2 0 -16 -2 0 16 -2 0 16 -2 0 16 -2 0 16 2 0 16 2 0 18 -2 0 18 -2 0 18 -2 0 18 -2 0 -18 -2 0 -18 -2 0 18 2 0 18 2 0 -20 -2 0 20 -2 0 20 -2 0 20 -2 0 -20 -2 0 20 -2 0 20 2 0 20 2 0 22 -2 0 22 -2 0 -22 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0 9 5 0 -9 5 0 9 5 0 -11 -5 0 11 -5 0 -11 -5 0 11 -5 0 -11 5 0 -11 5 0 11 5 0 11 5 0 13 -5 0 13 -5 0 -13 -5 0 -13 -5 0 -13 5 0 13 5 0 13 5 0 -13 5 0 15 -5 0 15 -5 0 -15 -5 0 -15 -5 0 15 5 0 15 5 0 -15 5 0 -15 5 0 17 -5 0 17 -5 0 -17 -5 0 17 5 0 -17 5 0 17 5 0 19 -5 0 -19 -5 0 19 -5 0 19 -5 0 19 5 0 19 5 0 -19 5 0 21 -5 0 -21 -5 0 21 -5 0 21 -5 0 -21 5 0 21 5 0 -23 -5 0 23 -5 0 23 -5 0 23 -5 0 23 5 0 -23 5 0 25 -5 0 25 -5 0 -25 -5 0 25 -5 0 25 5 0 -25 5 0 -27 -5 0 27 -5 0 27 -5 0 27 5 0 0 -6 0 0 -6 0 0 6 0 0 6 0 -2 -6 0 2 -6 0 -2 -6 0 2 -6 0 -2 6 0 2 6 0 -2 6 0 2 6 0 -4 -6 0 4 -6 0 -4 -6 0 4 -6 0 4 6 0 4 6 0 -4 6 0 -4 6 0 6 -6 0 6 -6 0 -6 -6 0 -6 -6 0 6 6 0 -6 6 0 6 6 0 -6 6 0 8 -6 0 -8 -6 0 8 -6 0 -8 -6 0 -8 6 0 8 6 0 8 6 0 -8 6 0 10 -6 0 -10 -6 0 -10 -6 0 10 -6 0 -10 6 0 -10 6 0 10 6 0 10 6 0 12 -6 0 -12 -6 0 12 -6 0 -12 -6 0 -12 6 0 12 6 0 -12 6 0 12 6 0 14 -6 0 -14 -6 0 14 -6 0 -14 -6 0 14 6 0 -14 6 0 14 6 0 -14 6 0 -16 -6 0 16 -6 0 16 -6 0 -16 6 0 16 6 0 16 6 0 -16 6 0 18 -6 0 18 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0 4 -8 0 4 -8 0 -4 -8 0 -4 -8 0 -4 8 0 4 8 0 4 8 0 -4 8 0 -6 -8 0 6 -8 0 -6 -8 0 6 -8 0 -6 8 0 -6 8 0 6 8 0 6 8 0 8 -8 0 -8 -8 0 -8 -8 0 8 -8 0 8 8 0 -8 8 0 -8 8 0 8 8 0 10 -8 0 -10 -8 0 -10 -8 0 10 -8 0 10 8 0 10 8 0 -10 8 0 12 -8 0 12 -8 0 -12 -8 0 -12 -8 0 12 8 0 12 8 0 -12 8 0 14 -8 0 -14 -8 0 14 -8 0 -14 8 0 14 8 0 14 8 0 -16 -8 0 16 -8 0 16 -8 0 -16 8 0 16 8 0 16 8 0 18 -8 0 18 -8 0 -18 -8 0 -18 8 0 18 8 0 18 8 0 -20 -8 0 20 -8 0 20 -8 0 20 8 0 -20 8 0 -22 -8 0 22 -8 0 -22 8 0 22 8 0 24 -8 0 -24 -8 0 -24 8 0 24 8 0 26 -8 0 -26 -8 0 26 8 0 -26 8 0 -1 -9 0 1 -9 0 1 -9 0 -1 -9 0 -1 9 0 -1 9 0 1 9 0 1 9 0 -3 -9 0 -3 -9 0 3 -9 0 3 -9 0 -3 9 0 3 9 0 -3 9 0 3 9 0 -5 -9 0 5 -9 0 5 -9 0 -5 -9 0 -5 9 0 5 9 0 -5 9 0 5 9 0 -7 -9 0 7 -9 0 7 -9 0 -7 -9 0 -7 9 0 7 9 0 7 9 0 9 -9 0 -9 -9 0 9 -9 0 -9 -9 0 9 9 0 9 9 0 -9 9 0 -11 -9 0 -11 -9 0 11 -9 0 11 -9 0 11 9 0 -11 9 0 11 9 0 -13 -9 0 13 -9 0 13 -9 0 13 9 0 -13 9 0 13 9 0 15 -9 0 15 -9 0 -15 -9 0 -15 9 0 15 9 0 15 9 0 17 -9 0 17 -9 0 -17 -9 0 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14 -7 -1 14 -7 1 14 7 1 -14 5 -1 -14 -5 -1 14 -5 1 14 5 1 -14 -3 -1 14 3 -1 -14 -3 1 14 3 1 -14 22 -2 -14 22 2 -14 -22 2 14 20 -2 -14 -20 -2 14 -20 2 14 20 2 -14 -18 -2 14 18 -2 -14 -18 2 14 18 2 -14 16 -2 -14 16 -2 -14 -16 -2 14 16 2 -14 -16 2 14 -14 -2 14 14 -2 -14 -14 2 14 14 2 -14 -12 -2 14 12 -2 -14 -12 2 14 12 2 -14 10 -2 -14 -10 -2 14 10 2 -14 -10 2 14 8 -2 -14 -8 -2 14 -8 -2 14 -8 2 14 8 2 -14 6 -2 -14 -6 -2 14 -6 -2 14 -6 2 14 6 2 -14 -4 -2 14 4 -2 -14 4 2 -14 -4 2 14 21 -3 -14 -21 3 14 21 3 -14 19 -3 -14 -19 3 14 19 3 -14 -17 -3 14 17 -3 -14 17 3 -14 -17 3 14 15 -3 -14 -15 -3 14 -15 3 14 15 3 -14 13 -3 -14 13 -3 -14 -13 -3 14 13 3 -14 -13 3 14 -11 -3 14 11 -3 -14 -11 3 14 11 3 -14 9 -3 -14 -9 -3 14 9 3 -14 -9 3 14 -7 -3 14 -7 -3 14 7 -3 -14 7 3 -14 -7 3 14 -5 -3 14 5 -3 -14 -5 -3 14 -5 3 14 -20 4 14 20 4 -14 18 -4 -14 -18 -4 14 -18 4 14 16 -4 -14 -16 -4 14 -16 4 14 16 4 -14 14 -4 -14 -14 -4 14 -14 4 14 14 4 -14 -12 -4 14 12 -4 -14 12 4 -14 -12 4 14 -10 -4 14 10 -4 -14 -10 4 14 10 4 -14 8 -4 -14 -8 -4 14 -8 4 14 8 4 -14 -6 -4 14 6 -4 -14 -6 -4 14 6 4 -14 -6 4 14 17 -5 -14 17 5 -14 -17 5 14 15 -5 -14 -15 -5 14 -15 5 14 15 5 -14 13 -5 -14 -13 -5 14 13 5 -14 -13 5 14 11 -5 -14 -11 -5 14 -11 5 14 9 -5 -14 -9 -5 14 -9 5 14 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist -1.00 1.00 1.00 0.1250 1.00 -1.00 -1.00 0.0520 -1.00 -1.00 1.00 0.0970 -1.00 0.00 0.00 0.1390 1.00 0.00 0.00 0.0710 -1.00 1.00 0.00 0.1360 1.00 0.00 -1.00 0.0430 0.00 1.00 -1.00 0.0950 1.00 1.00 0.00 0.1420 loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag P1 Pd1 I1 . . 89.737(13) ? P1 Pd1 I1 2_655 . 89.737(13) ? P1 Pd1 P1 2_655 . 179.47(3) ? C1 Pd1 I1 . . 180.0 ? C1 Pd1 P1 . . 90.263(13) ? C1 Pd1 P1 . 2_655 90.263(13) ? C5 P1 Pd1 . . 115.79(7) ? C11 P1 Pd1 . . 116.28(6) ? C11 P1 C5 . . 100.83(9) ? C17 P1 Pd1 . . 110.10(7) ? C17 P1 C5 . . 109.29(9) ? C17 P1 C11 . . 103.53(9) ? C2 C1 Pd1 . . 119.64(17) ? C2 C1 Pd1 2_655 . 119.64(17) ? C2 C1 C2 2_655 . 120.7(3) ? C2A C1 Pd1 2_655 . 119.64(17) ? C2A C1 Pd1 . . 119.64(17) ? C2A C1 C2 . 2_655 120.7(3) ? C2A C1 C2 2_655 2_655 0.0 ? C2A C1 C2 2_655 . 120.7(3) ? C2A C1 C2 . . 0.0 ? C2A C1 C2A 2_655 . 120.7(3) ? C1 C2 F1 . . 124.0(3) ? C3 C2 F1 . . 113.6(3) ? C3 C2 C1 . . 122.3(2) ? C2 C3 F2 . . 123.7(3) ? C4 C3 F2 2_655 . 119.3(3) ? C4 C3 C2 2_655 . 117.0(2) ? C3 C4 F3 2_655 . 119.69(16) ? C3 C4 F3 . . 119.69(16) ? C3 C4 C3 . 2_655 120.6(3) ? C3A C4 F3 . . 119.69(16) ? C3A C4 F3 2_655 . 119.69(16) ? C3A C4 C3 2_655 . 120.6(3) ? C3A C4 C3 2_655 2_655 0.0 ? C3A C4 C3 . 2_655 120.6(3) ? C3A C4 C3 . . 0.0 ? C3A C4 C3A . 2_655 120.6(3) ? C6 C5 P1 . . 121.06(15) ? C10 C5 P1 . . 119.31(15) ? C10 C5 C6 . . 119.41(19) ? H6 C6 C5 . . 119.98(12) ? C7 C6 C5 . . 120.0(2) ? C7 C6 H6 . . 119.98(13) ? H7 C7 C6 . . 120.01(13) ? C8 C7 C6 . . 120.0(2) ? C8 C7 H7 . . 120.01(13) ? H8 C8 C7 . . 119.81(13) ? C9 C8 C7 . . 120.4(2) ? C9 C8 H8 . . 119.81(13) ? H9 C9 C8 . . 120.12(13) ? C10 C9 C8 . . 119.8(2) ? C10 C9 H9 . . 120.12(13) ? C9 C10 C5 . . 120.41(19) ? H10 C10 C5 . . 119.80(12) ? H10 C10 C9 . . 119.80(13) ? C12 C11 P1 . . 122.62(16) ? C16 C11 P1 . . 117.84(15) ? C16 C11 C12 . . 119.23(19) ? H12 C12 C11 . . 119.99(12) ? C13 C12 C11 . . 120.0(2) ? C13 C12 H12 . . 119.99(13) ? H13 C13 C12 . . 119.80(13) ? C14 C13 C12 . . 120.4(2) ? C14 C13 H13 . . 119.80(13) ? H14 C14 C13 . . 120.05(13) ? C15 C14 C13 . . 119.9(2) ? C15 C14 H14 . . 120.05(13) ? H15 C15 C14 . . 119.95(13) ? C16 C15 C14 . . 120.1(2) ? C16 C15 H15 . . 119.95(13) ? C15 C16 C11 . . 120.3(2) ? H16 C16 C11 . . 119.84(12) ? H16 C16 C15 . . 119.84(13) ? C18 C17 P1 . . 123.52(16) ? C22 C17 P1 . . 117.11(15) ? C22 C17 C18 . . 119.33(19) ? H18 C18 C17 . . 120.03(12) ? C19 C18 C17 . . 119.9(2) ? C19 C18 H18 . . 120.03(13) ? H19 C19 C18 . . 119.89(13) ? C20 C19 C18 . . 120.2(2) ? C20 C19 H19 . . 119.89(13) ? H20 C20 C19 . . 119.85(13) ? C21 C20 C19 . . 120.3(2) ? C21 C20 H20 . . 119.85(13) ? H21 C21 C20 . . 120.14(13) ? C22 C21 C20 . . 119.7(2) ? C22 C21 H21 . . 120.14(13) ? C21 C22 C17 . . 120.5(2) ? H22 C22 C17 . . 119.76(12) ? H22 C22 C21 . . 119.76(13) ? H2A C2A C1 . . 118.87(17) ? C3A C2A C1 . . 122.3(2) ? C3A C2A H2A . . 118.87(15) ? C2A C3A C4 . 2_655 117.0(2) ? H3A C3A C4 . 2_655 121.48(16) ? H3A C3A C2A . . 121.48(15) ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Pd1 I1 . 2.6787(3) ? Pd1 P1 2_655 2.3239(5) ? Pd1 P1 . 2.3239(5) ? Pd1 C1 . 2.091(4) ? P1 C5 . 1.827(2) ? P1 C11 . 1.830(2) ? P1 C17 . 1.825(2) ? F1 C2 . 1.319(3) ? C1 C2 2_655 1.299(3) ? C1 C2 . 1.299(3) ? C1 C2A . 1.299(3) ? C1 C2A 2_655 1.299(3) ? F2 C3 . 1.284(4) ? C2 C3 . 1.430(3) ? F3 C4 . 1.356(4) ? C3 C4 2_655 1.375(3) ? C4 C3A 2_655 1.375(3) ? C4 C3A . 1.375(3) ? C5 C6 . 1.394(3) ? C5 C10 . 1.398(3) ? C6 H6 . 0.9500 ? C6 C7 . 1.397(3) ? C7 H7 . 0.9500 ? C7 C8 . 1.386(3) ? C8 H8 . 0.9500 ? C8 C9 . 1.389(3) ? C9 H9 . 0.9500 ? C9 C10 . 1.390(3) ? C10 H10 . 0.9500 ? C11 C12 . 1.392(3) ? C11 C16 . 1.401(3) ? C12 H12 . 0.9500 ? C12 C13 . 1.397(3) ? C13 H13 . 0.9500 ? C13 C14 . 1.381(4) ? C14 H14 . 0.9500 ? C14 C15 . 1.392(3) ? C15 H15 . 0.9500 ? C15 C16 . 1.387(3) ? C16 H16 . 0.9500 ? C17 C18 . 1.397(3) ? C17 C22 . 1.399(3) ? C18 H18 . 0.9500 ? C18 C19 . 1.395(3) ? C19 H19 . 0.9500 ? C19 C20 . 1.387(3) ? C20 H20 . 0.9500 ? C20 C21 . 1.388(3) ? C21 H21 . 0.9500 ? C21 C22 . 1.393(3) ? C22 H22 . 0.9500 ? C2A H2A . 0.9500 ? C2A C3A . 1.430(3) ? C3A H3A . 0.9500 ? 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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag Pd1 C1 C2 F1 . . . . -3.43(14) ? Pd1 C1 C2 F1 . . 2_655 2_655 -3.43(14) ? Pd1 C1 C2 C3 . . . . -178.84(15) ? Pd1 C1 C2 C3 . . 2_655 2_655 -178.84(15) ? Pd1 C1 C2A C3A . . 2_655 2_655 -178.84(15) ? Pd1 C1 C2A C3A . . . . -178.84(15) ? P1 C5 C6 C7 . . . . -175.03(17) ? P1 C5 C10 C9 . . . . 175.67(16) ? P1 C11 C12 C13 . . . . 171.50(17) ? P1 C11 C16 C15 . . . . -171.90(15) ? P1 C17 C18 C19 . . . . -177.85(17) ? P1 C17 C22 C21 . . . . 178.16(16) ? F1 C2 C1 C2 . . . 2_655 176.57(13) ? F1 C2 C1 C2A . . . 2_655 176.57(14) ? F1 C2 C3 F2 . . . . 2.2(3) ? F1 C2 C3 C4 . . . 2_655 -178.11(19) ? C1 C2 C3 F2 . . . . 178.0(3) ? C1 C2 C3 F2 2_655 . . . 178.0(3) ? C1 C2 C3 C4 . . . 2_655 -2.3(2) ? C1 C2 C3 C4 . 2_655 2_655 . -2.3(2) ? C1 C2A C3A C4 . . . 2_655 -2.3(2) ? C1 C2A C3A C4 . 2_655 2_655 . -2.3(2) ? F2 C3 C4 F3 . . 2_655 2_655 0.8(3) ? F2 C3 C4 C3 . . 2_655 2_655 -179.22(18) ? F2 C3 C4 C3A . . 2_655 2_655 -179.22(18) ? C2 C3 C4 F3 . . 2_655 2_655 -178.96(14) ? C2 C3 C4 C3 . . 2_655 2_655 1.0(3) ? C2 C3 C4 C3A . . 2_655 2_655 1.0(3) ? F3 C4 C3A C2A . . 2_655 2_655 -178.96(15) ? F3 C4 C3A C2A . . . . -178.96(15) ? C3 C4 C3A C2A 2_655 . . . 1.04(15) ? C5 C6 C7 C8 . . . . -0.3(2) ? C5 C10 C9 C8 . . . . -0.8(2) ? C6 C7 C8 C9 . . . . 0.5(3) ? C7 C8 C9 C10 . . . . 0.0(3) ? C11 C12 C13 C14 . . . . 0.4(2) ? C11 C16 C15 C14 . . . . -0.3(2) ? C12 C13 C14 C15 . . . . 1.1(3) ? C13 C14 C15 C16 . . . . -1.2(3) ? C17 C18 C19 C20 . . . . -0.4(2) ? C17 C22 C21 C20 . . . . 0.0(3) ? C18 C19 C20 C21 . . . . 0.6(3) ? C19 C20 C21 C22 . . . . -0.4(3) ?