#------------------------------------------------------------------------------ #$Date: 2013-12-28 13:58:47 +0000 (Sat, 28 Dec 2013) $ #$Revision: 91933 $ #$URL: svn://www.crystallography.net/cod/cif/2/20/07/2200790.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_2200790 loop_ _publ_author_name 'Jonathan P. H. Charmant' 'Pablo Espinet' 'Katerina Soulantica' _publ_section_title ; Square [Pd~4~(\m-CN)~4~(C~6~F~5~)~4~(PEt~3~)~4~]·2C~6~H~5~CH~3~ ; _journal_issue 10 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first m451 _journal_page_last m453 _journal_volume 57 _journal_year 2001 _chemical_formula_iupac '[Pd4 (C N)4 (C6 F5)4 (C6 H15 P)4], 2C7 H8' _chemical_formula_moiety 'C52 H60 F20 N4 P4 Pd4, 2C7 H8' _chemical_formula_sum 'C66 H76 F20 N4 P4 Pd4' _chemical_formula_weight 1854.79 _chemical_name_systematic ; Palladium, tetrakis[\m-(cyano-C:N)]tetrakis(pentafluorophenyl) tetrakis(triethylphosphine)tetra-, cyclo (9CI), ditoluene ; _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 97.372(9) _cell_angle_gamma 90.00 _cell_formula_units_Z 2 _cell_length_a 11.8845(10) _cell_length_b 14.8554(18) _cell_length_c 21.652(3) _cell_measurement_reflns_used 441 _cell_measurement_temperature 173(2) _cell_measurement_theta_max 25 _cell_measurement_theta_min 2 _cell_volume 3791.0(8) _computing_cell_refinement SMART _computing_data_collection 'SMART (Bruker, 1998)' _computing_data_reduction 'SAINT (Bruker, 1998)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _computing_structure_refinement SHELXTL _computing_structure_solution 'SHELXTL (Bruker, 1998)' _diffrn_ambient_temperature 173(2) _diffrn_measured_fraction_theta_full .998 _diffrn_measured_fraction_theta_max .998 _diffrn_measurement_device_type 'CCD area-detector' _diffrn_measurement_method \w _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength .71073 _diffrn_reflns_av_R_equivalents .038 _diffrn_reflns_av_sigmaI/netI .034 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_number 38987 _diffrn_reflns_theta_full 27.5 _diffrn_reflns_theta_max 27.5 _diffrn_reflns_theta_min 1.67 _diffrn_standards_decay_% 0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 1.11 _exptl_absorpt_correction_T_max .801 _exptl_absorpt_correction_T_min .695 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(SADABS; Sheldrick, 2001)' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.625 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 1848 _exptl_crystal_size_max .3 _exptl_crystal_size_mid .3 _exptl_crystal_size_min .3 _refine_diff_density_max 1.01 _refine_diff_density_min -.75 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref .97 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 449 _refine_ls_number_reflns 8699 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all .97 _refine_ls_R_factor_all .039 _refine_ls_R_factor_gt .025 _refine_ls_shift/su_max .001 _refine_ls_shift/su_mean .000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w = 1/[\s^2^(Fo^2^)+(0.0336P)^2^] where P = (Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_ref .061 _reflns_number_gt 6789 _reflns_number_total 8699 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file ya6040.cif _[local]_cod_data_source_block I _[local]_cod_cif_authors_sg_H-M 'P 21/c' _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius The following automatic conversions were performed: '_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic' according to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana ; _cod_database_code 2200790 loop_ _symmetry_equiv_pos_as_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_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_type_symbol Pd1 .549498(14) -.223794(11) .065058(8) .02383(5) Uani d . 1 . . Pd Pd2 .246938(14) .025756(11) .083650(8) .02292(5) Uani d . 1 . . Pd C1A .42579(17) -.12888(14) .06457(10) .0278(5) Uani d P .50 A 1 C C2A .30701(18) .09898(14) .01589(10) .0301(5) Uani d P .50 . 1 C N1A .35909(18) -.07465(14) .07015(10) .0285(5) Uani d P .50 A 1 N N2A .64715(16) -.14097(13) .01756(10) .0237(4) Uani d P .50 . 1 N N1B .42579(17) -.12888(14) .06457(10) .0278(5) Uani d P .50 A 2 N N2B .30701(18) .09898(14) .01589(10) .0301(5) Uani d P .50 . 2 N C1B .35909(18) -.07465(14) .07015(10) .0285(5) Uani d P .50 A 2 C C2B .64715(16) -.14097(13) .01756(10) .0237(4) Uani d P .50 . 2 C P1 .43375(6) -.31907(4) .10737(3) .03429(15) Uani d . 1 A . P P2 .11997(5) .13484(4) .10126(3) .02513(13) Uani d . 1 . . P C10 .67556(19) -.31656(15) .07088(11) .0270(5) Uani d . 1 A . C C11 .7011(2) -.36491(16) .02030(12) .0339(6) Uani d . 1 . . C F11 .63377(14) -.35788(11) -.03497(7) .0503(4) Uani d . 1 A . F C12 .7944(2) -.42179(17) .02241(15) .0437(7) Uani d . 1 A . C F12 .81750(15) -.46538(11) -.02906(9) .0643(5) Uani d . 1 . . F C13 .8634(2) -.43295(17) .07789(17) .0479(8) Uani d . 1 . . C F13 .95275(15) -.48974(12) .08120(11) .0752(6) Uani d . 1 A . F C14 .8396(2) -.38786(17) .12962(14) .0416(7) Uani d . 1 A . C F14 .90451(13) -.40133(11) .18475(9) .0600(5) Uani d . 1 . . F C15 .7478(2) -.33019(16) .12516(12) .0327(5) Uani d . 1 . . C F15 .72855(13) -.28742(10) .17839(7) .0439(4) Uani d . 1 A . F C20 .19911(19) -.04493(15) .15670(11) .0265(5) Uani d . 1 . . C C21 .2478(2) -.03018(15) .21721(12) .0325(5) Uani d . 1 . . C F21 .32964(14) .03387(10) .22920(7) .0500(4) Uani d . 1 . . F C22 .2184(2) -.07704(18) .26800(12) .0410(6) Uani d . 1 . . C F22 .27015(18) -.05946(12) .32598(7) .0659(5) Uani d . 1 . . F C23 .1357(2) -.14152(18) .25910(14) .0438(7) Uani d . 1 . . C F23 .10380(17) -.18584(12) .30849(9) .0682(6) Uani d . 1 . . F C24 .0861(2) -.16043(17) .19995(14) .0413(7) Uani d . 1 . . C F24 .00538(15) -.22464(11) .19080(10) .0670(5) Uani d . 1 . . F C25 .1193(2) -.11361(16) .15038(12) .0335(5) Uani d . 1 . . C F25 .06995(14) -.13713(11) .09261(8) .0559(5) Uani d . 1 . . F C30 .3051(2) -.33575(19) .04913(15) .0483(7) Uani d . 1 . . C H30A .2551 -.3809 .0654 .058 Uiso calc R 1 A . H H30B .2626 -.2784 .0437 .058 Uiso calc R 1 . . H C31 .3336(3) -.3668(3) -.01369(16) .0711(10) Uani d . 1 A . C H31A .3788 -.3205 -.0313 .107 Uiso calc R 1 . . H H31B .2633 -.3770 -.0418 .107 Uiso calc R 1 . . H H31C .3771 -.4230 -.0086 .107 Uiso calc R 1 . . H C40 .4880(2) -.43085(17) .12880(13) .0400(6) Uani d . 1 . . C H40A .5069 -.4610 .0906 .048 Uiso calc R 1 A . H H40B .5597 -.4238 .1572 .048 Uiso calc R 1 . . H C41 .4104(3) -.49317(19) .16005(14) .0493(7) Uani d . 1 A . C H41A .3971 -.4676 .2002 .074 Uiso calc R 1 . . H H41B .4464 -.5523 .1668 .074 Uiso calc R 1 . . H H41C .3379 -.4996 .1333 .074 Uiso calc R 1 . . H C50 .3752(2) -.27189(19) .17340(13) .0439(7) Uani d . 1 . . C H50A .3308 -.2174 .1598 .053 Uiso calc R 1 A . H H50B .3228 -.3161 .1885 .053 Uiso calc R 1 . . H C51 .4655(3) -.2471(3) .22655(15) .0681(10) Uani d . 1 A . C H51A .5133 -.2996 .2383 .102 Uiso calc R 1 . . H H51B .4291 -.2273 .2624 .102 Uiso calc R 1 . . H H51C .5124 -.1982 .2134 .102 Uiso calc R 1 . . H C60 .1715(2) .20602(17) .16768(12) .0367(6) Uani d . 1 . . C H60A .1131 .2519 .1732 .044 Uiso calc R 1 . . H H60B .1821 .1685 .2057 .044 Uiso calc R 1 . . H C61 .2820(2) .2532(2) .16072(14) .0523(8) Uani d . 1 . . C H61A .3391 .2086 .1528 .078 Uiso calc R 1 . . H H61B .3082 .2862 .1991 .078 Uiso calc R 1 . . H H61C .2701 .2955 .1257 .078 Uiso calc R 1 . . H C70 -.01827(19) .09583(17) .11888(12) .0334(6) Uani d . 1 . . C H70A -.0064 .0541 .1548 .040 Uiso calc R 1 . . H H70B -.0616 .1482 .1314 .040 Uiso calc R 1 . . H C71 -.0887(2) .0482(2) .06484(14) .0458(7) Uani d . 1 . . C H71A -.1108 .0914 .0313 .069 Uiso calc R 1 . . H H71B -.1569 .0226 .0791 .069 Uiso calc R 1 . . H H71C -.0437 -.0002 .0494 .069 Uiso calc R 1 . . H C80 .0884(2) .21135(16) .03553(11) .0304(5) Uani d . 1 . . C H80A .1598 .2414 .0280 .036 Uiso calc R 1 . . H H80B .0617 .1753 -.0020 .036 Uiso calc R 1 . . H C81 .0001(2) .28380(19) .04288(15) .0484(7) Uani d . 1 . . C H81A -.0718 .2552 .0494 .073 Uiso calc R 1 . . H H81B -.0114 .3209 .0052 .073 Uiso calc R 1 . . H H81C .0266 .3218 .0788 .073 Uiso calc R 1 . . H C90 .4079(3) -.4081(3) .38117(18) .0876(13) Uani d . 1 . . C H90A .4827 -.4230 .3695 .131 Uiso calc R 1 . . H H90B .3997 -.4356 .4215 .131 Uiso calc R 1 . . H H90C .4005 -.3426 .3842 .131 Uiso calc R 1 . . H C91 .3177(3) -.4434(2) .33287(14) .0549(8) Uani d . 1 . . C C92 .2981(3) -.5363(2) .32470(16) .0613(9) Uani d . 1 . . C H92 .3435 -.5781 .3501 .074 Uiso calc R 1 . . H C93 .2134(3) -.5675(2) .27999(17) .0627(9) Uani d . 1 . . C H93 .2006 -.6304 .2754 .075 Uiso calc R 1 . . H C94 .1490(3) -.5096(3) .24281(17) .0616(9) Uani d . 1 . . C H94 .0912 -.5316 .2121 .074 Uiso calc R 1 . . H C95 .1669(2) -.4188(2) .24934(16) .0564(9) Uani d . 1 . . C H95 .1221 -.3782 .2227 .068 Uiso calc R 1 . . H C96 .2488(2) -.3858(2) .29394(14) .0458(7) Uani d . 1 . . C H96 .2587 -.3226 .2983 .055 Uiso calc R 1 . . H 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 .02402(9) .02250(9) .02620(10) .00150(7) .00799(7) .00186(7) Pd2 .02295(9) .02252(9) .02429(9) .00100(7) .00689(7) .00197(7) C1A .0278(11) .0279(11) .0294(12) .0017(9) .0100(9) .0047(9) C2A .0283(11) .0280(11) .0346(13) .0062(9) .0066(10) -.0009(9) N1A .0290(11) .0279(11) .0300(12) .0000(9) .0087(9) .0046(9) N2A .0238(10) .0212(10) .0278(11) .0031(8) .0095(9) .0033(8) N1B .0278(11) .0279(11) .0294(12) .0017(9) .0100(9) .0047(9) N2B .0283(11) .0280(11) .0346(13) .0062(9) .0066(10) -.0009(9) C1B .0290(11) .0279(11) .0300(12) .0000(9) .0087(9) .0046(9) C2B .0238(10) .0212(10) .0278(11) .0031(8) .0095(9) .0033(8) P1 .0366(4) .0275(3) .0418(4) -.0042(3) .0166(3) .0006(3) P2 .0246(3) .0265(3) .0250(3) .0023(2) .0061(2) -.0008(2) C10 .0253(11) .0222(11) .0351(14) .0018(9) .0103(10) .0034(10) C11 .0341(13) .0290(12) .0404(15) -.0015(11) .0120(11) .0008(11) F11 .0627(11) .0529(10) .0370(9) .0052(8) .0127(8) -.0090(8) C12 .0445(16) .0264(13) .066(2) -.0002(12) .0304(15) -.0070(13) F12 .0674(12) .0477(10) .0863(14) .0028(9) .0421(11) -.0236(9) C13 .0290(14) .0266(13) .090(3) .0077(11) .0159(15) .0056(15) F13 .0442(10) .0461(10) .137(2) .0238(8) .0192(11) .0014(11) C14 .0303(13) .0305(13) .062(2) .0022(11) -.0009(13) .0094(13) F14 .0413(9) .0504(10) .0821(14) .0071(8) -.0166(9) .0142(9) C15 .0308(13) .0259(12) .0423(15) .0007(10) .0084(11) .0021(11) F15 .0476(9) .0447(9) .0375(9) .0047(7) -.0012(7) .0000(7) C20 .0255(11) .0261(11) .0289(13) .0026(9) .0081(10) .0032(9) C21 .0397(14) .0268(12) .0309(13) .0006(11) .0046(11) .0019(10) F21 .0630(10) .0422(9) .0400(9) -.0174(8) -.0122(8) .0039(7) C22 .0627(18) .0351(14) .0265(14) .0111(14) .0103(12) .0041(11) F22 .1157(16) .0535(11) .0264(9) .0065(11) .0016(9) .0049(8) C23 .0562(17) .0358(14) .0450(17) .0119(13) .0282(14) .0183(12) F23 .0927(14) .0564(11) .0648(12) .0111(10) .0455(11) .0326(9) C24 .0339(14) .0294(13) .063(2) -.0027(11) .0155(13) .0124(13) F24 .0523(10) .0486(10) .1005(16) -.0206(9) .0109(10) .0240(10) C25 .0316(13) .0307(13) .0378(15) -.0011(11) .0032(11) .0020(11) F25 .0646(11) .0455(9) .0519(11) -.0229(8) -.0149(8) .0033(8) C30 .0361(15) .0385(15) .070(2) -.0060(12) .0064(14) .0045(14) C31 .074(2) .083(3) .052(2) -.025(2) -.0048(18) -.0018(19) C40 .0383(14) .0344(14) .0486(17) -.0001(12) .0102(12) .0152(12) C41 .0579(19) .0395(15) .0518(19) -.0122(14) .0124(15) .0121(13) C50 .0460(16) .0426(15) .0463(17) .0001(13) .0183(13) .0061(13) C51 .054(2) .115(3) .0368(18) -.021(2) .0110(15) -.0038(18) C60 .0423(15) .0371(14) .0304(14) .0065(12) .0037(11) -.0075(11) C61 .0505(18) .0564(18) .0478(18) -.0141(15) -.0014(14) -.0162(14) C70 .0282(12) .0355(13) .0397(15) .0041(10) .0167(11) .0028(11) C71 .0324(14) .0542(17) .0530(18) -.0110(13) .0141(13) -.0049(14) C80 .0288(12) .0313(13) .0317(13) .0041(10) .0060(10) .0069(10) C81 .0459(16) .0442(16) .0571(19) .0184(13) .0137(14) .0152(14) C90 .070(2) .134(4) .057(2) .002(3) .002(2) .004(2) C91 .0488(18) .082(2) .0376(17) .0106(17) .0179(14) .0087(16) C92 .072(2) .065(2) .050(2) .0305(18) .0223(18) .0268(17) C93 .077(2) .0516(19) .065(2) .0111(18) .030(2) .0057(17) C94 .0497(19) .077(2) .062(2) .0007(18) .0185(17) .0057(18) C95 .0393(16) .066(2) .068(2) .0114(15) .0213(16) .0264(17) C96 .0369(15) .0482(16) .0570(19) .0057(13) .0234(14) .0107(14) 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 C1A . 2.036(2) yes Pd1 N2A . 2.0554(19) yes Pd1 P1 . 2.2490(7) yes Pd1 C10 . 2.028(2) yes Pd2 C2A . 2.028(2) yes Pd2 N1A . 2.046(2) yes Pd2 P2 . 2.2795(6) yes Pd2 C20 . 2.039(2) yes C1A N1A . 1.147(3) yes C2A N2A 3_655 1.145(3) yes N2A C2A 3_655 1.145(3) no P1 C50 . 1.809(3) no P1 C40 . 1.820(3) no P1 C30 . 1.870(3) no P2 C80 . 1.822(2) no P2 C60 . 1.826(3) no P2 C70 . 1.828(2) no C10 C11 . 1.376(3) no C10 C15 . 1.379(3) no C11 F11 . 1.356(3) no C11 C12 . 1.390(3) no C12 F12 . 1.347(3) no C12 C13 . 1.375(4) no C13 F13 . 1.351(3) no C13 C14 . 1.366(4) no C14 F14 . 1.350(3) no C14 C15 . 1.381(3) no C15 F15 . 1.361(3) no C20 C21 . 1.380(3) no C20 C25 . 1.388(3) no C21 F21 . 1.361(3) no C21 C22 . 1.384(3) no C22 F22 . 1.351(3) no C22 C23 . 1.368(4) no C23 F23 . 1.351(3) no C23 C24 . 1.368(4) no C24 F24 . 1.350(3) no C24 C25 . 1.378(4) no C25 F25 . 1.357(3) no C30 C31 . 1.515(4) no C40 C41 . 1.525(3) no C50 C51 . 1.514(4) no C60 C61 . 1.513(4) no C70 C71 . 1.523(4) no C80 C81 . 1.526(3) no C90 C91 . 1.493(5) no C91 C96 . 1.391(4) no C91 C92 . 1.407(5) no C92 C93 . 1.384(5) no C93 C94 . 1.348(5) no C94 C95 . 1.369(5) no C95 C96 . 1.371(4) no loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N .0061 .0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F .0171 .0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P .1023 .0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -.9988 1.0072 '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_site_symmetry_1 _geom_angle _geom_angle_publ_flag C1A Pd1 N2A . 92.09(8) yes C1A Pd1 P1 . 87.65(6) yes N2A Pd1 P1 . 174.08(6) yes C10 Pd1 C1A . 176.64(9) yes C10 Pd1 N2A . 88.73(8) yes C10 Pd1 P1 . 91.87(6) yes C2A Pd2 N1A . 89.51(8) yes C2A Pd2 P2 . 92.39(6) yes C2A Pd2 C20 . 175.01(9) yes N1A Pd2 P2 . 178.10(6) yes C20 Pd2 N1A . 89.25(8) yes C20 Pd2 P2 . 88.85(6) yes N1A C1A Pd1 . 173.6(2) yes N2A C2A Pd2 3_655 171.7(2) yes C1A N1A Pd2 . 176.7(2) yes C2A N2A Pd1 3_655 170.9(2) yes C50 P1 C40 . 108.15(13) no C50 P1 C30 . 102.73(13) no C40 P1 C30 . 106.47(13) no C50 P1 Pd1 . 113.28(9) no C40 P1 Pd1 . 117.56(8) no C30 P1 Pd1 . 107.38(10) no C80 P2 C60 . 105.57(12) no C80 P2 C70 . 105.09(11) no C60 P2 C70 . 103.80(12) no C80 P2 Pd2 . 112.77(8) no C60 P2 Pd2 . 112.41(9) no C70 P2 Pd2 . 116.20(8) no C11 C10 C15 . 115.1(2) no C11 C10 Pd1 . 122.84(18) no C15 C10 Pd1 . 121.82(17) no F11 C11 C10 . 119.8(2) no F11 C11 C12 . 117.0(2) no C10 C11 C12 . 123.2(3) no F12 C12 C13 . 120.2(2) no F12 C12 C11 . 120.8(3) no C13 C12 C11 . 119.1(3) no F13 C13 C14 . 120.5(3) no F13 C13 C12 . 119.9(3) no C14 C13 C12 . 119.6(2) no F14 C14 C13 . 119.8(2) no F14 C14 C15 . 120.7(3) no C13 C14 C15 . 119.5(3) no F15 C15 C10 . 120.0(2) no F15 C15 C14 . 116.6(2) no C10 C15 C14 . 123.4(2) no C21 C20 C25 . 114.1(2) no C21 C20 Pd2 . 121.99(17) no C25 C20 Pd2 . 123.86(18) no F21 C21 C20 . 119.6(2) no F21 C21 C22 . 116.6(2) no C20 C21 C22 . 123.8(2) no F22 C22 C23 . 120.0(2) no F22 C22 C21 . 120.6(3) no C23 C22 C21 . 119.4(3) no F23 C23 C22 . 119.9(3) no F23 C23 C24 . 120.7(3) no C22 C23 C24 . 119.4(2) no F24 C24 C23 . 119.7(2) no F24 C24 C25 . 120.8(3) no C23 C24 C25 . 119.6(2) no F25 C25 C24 . 117.1(2) no F25 C25 C20 . 119.3(2) no C24 C25 C20 . 123.7(2) no C31 C30 P1 . 112.8(2) no C41 C40 P1 . 116.88(19) no C51 C50 P1 . 112.8(2) no C61 C60 P2 . 113.42(19) no C71 C70 P2 . 114.02(17) no C81 C80 P2 . 115.71(18) no C96 C91 C92 . 116.9(3) no C96 C91 C90 . 121.5(3) no C92 C91 C90 . 121.7(3) no C93 C92 C91 . 120.7(3) no C94 C93 C92 . 120.7(3) no C93 C94 C95 . 119.9(4) no C94 C95 C96 . 120.8(3) no C95 C96 C91 . 121.1(3) no 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_publ_flag C10 Pd1 P1 C50 127.35(13) no C1A Pd1 P1 C50 -49.32(12) no C10 Pd1 P1 C40 -.03(13) no C1A Pd1 P1 C40 -176.70(13) no C10 Pd1 P1 C30 -119.93(12) no C1A Pd1 P1 C30 63.40(12) no C2A Pd2 P2 C80 21.14(11) no C20 Pd2 P2 C80 -163.69(11) no C2A Pd2 P2 C60 -98.07(11) no C20 Pd2 P2 C60 77.10(12) no C2A Pd2 P2 C70 142.56(11) no C20 Pd2 P2 C70 -42.27(12) no N2A Pd1 C10 C11 -71.23(19) no P1 Pd1 C10 C11 102.87(19) no N2A Pd1 C10 C15 103.36(19) no P1 Pd1 C10 C15 -82.53(18) no C15 C10 C11 F11 178.5(2) no Pd1 C10 C11 F11 -6.6(3) no C15 C10 C11 C12 -1.7(3) no Pd1 C10 C11 C12 173.22(18) no F11 C11 C12 F12 1.9(3) no C10 C11 C12 F12 -177.9(2) no F11 C11 C12 C13 -178.3(2) no C10 C11 C12 C13 1.9(4) no F12 C12 C13 F13 -1.9(4) no C11 C12 C13 F13 178.3(2) no F12 C12 C13 C14 179.5(2) no C11 C12 C13 C14 -.3(4) no F13 C13 C14 F14 -1.2(4) no C12 C13 C14 F14 177.4(2) no F13 C13 C14 C15 -179.9(2) no C12 C13 C14 C15 -1.4(4) no C11 C10 C15 F15 -178.3(2) no Pd1 C10 C15 F15 6.7(3) no C11 C10 C15 C14 -.1(3) no Pd1 C10 C15 C14 -175.05(18) no F14 C14 C15 F15 1.2(3) no C13 C14 C15 F15 179.9(2) no F14 C14 C15 C10 -177.2(2) no C13 C14 C15 C10 1.6(4) no N1A Pd2 C20 C21 93.8(2) no P2 Pd2 C20 C21 -86.29(19) no N1A Pd2 C20 C25 -83.6(2) no P2 Pd2 C20 C25 96.32(19) no C25 C20 C21 F21 178.2(2) no Pd2 C20 C21 F21 .6(3) no C25 C20 C21 C22 -1.9(3) no Pd2 C20 C21 C22 -179.56(19) no F21 C21 C22 F22 -.6(4) no C20 C21 C22 F22 179.6(2) no F21 C21 C22 C23 179.2(2) no C20 C21 C22 C23 -.6(4) no F22 C22 C23 F23 1.8(4) no C21 C22 C23 F23 -178.0(2) no F22 C22 C23 C24 -178.2(2) no C21 C22 C23 C24 2.0(4) no F23 C23 C24 F24 -.7(4) no C22 C23 C24 F24 179.3(2) no F23 C23 C24 C25 179.3(2) no C22 C23 C24 C25 -.7(4) no F24 C24 C25 F25 -2.1(4) no C23 C24 C25 F25 177.9(2) no F24 C24 C25 C20 177.9(2) no C23 C24 C25 C20 -2.1(4) no C21 C20 C25 F25 -176.7(2) no Pd2 C20 C25 F25 .9(3) no C21 C20 C25 C24 3.3(4) no Pd2 C20 C25 C24 -179.14(19) no C50 P1 C30 C31 174.4(2) no C40 P1 C30 C31 -72.1(3) no Pd1 P1 C30 C31 54.7(2) no C50 P1 C40 C41 47.6(3) no C30 P1 C40 C41 -62.2(3) no Pd1 P1 C40 C41 177.38(18) no C40 P1 C50 C51 71.0(3) no C30 P1 C50 C51 -176.7(2) no Pd1 P1 C50 C51 -61.2(2) no C80 P2 C60 C61 -64.6(2) no C70 P2 C60 C61 -174.9(2) no Pd2 P2 C60 C61 58.7(2) no C80 P2 C70 C71 59.0(2) no C60 P2 C70 C71 169.67(19) no Pd2 P2 C70 C71 -66.4(2) no C60 P2 C80 C81 -59.4(2) no C70 P2 C80 C81 49.9(2) no Pd2 P2 C80 C81 177.46(17) no C96 C91 C92 C93 -.3(4) no C90 C91 C92 C93 179.4(3) no C91 C92 C93 C94 .9(5) no C92 C93 C94 C95 -.2(5) no C93 C94 C95 C96 -.9(5) no C94 C95 C96 C91 1.5(4) no C92 C91 C96 C95 -.8(4) no C90 C91 C96 C95 179.4(3) no _cod_database_fobs_code 2200790 _journal_paper_doi 10.1107/S1600536801014994