# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 1999 # CCDC Number: 186/1690 data_global _audit_creation_date ? _audit_creation_method 'PARSTCIF' _audit_update_record ? # PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ? _journal_techeditor_code ? _iucr_compatibility_tag ? _journal_techeditor_notes ? _journal_coden_ASTM ? _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? # SUBMISSION DETAILS _publ_contact_author_name 'Prof. Antonio Tiripicchio' _publ_contact_author_address ; Dipartimento di Chimica Generale ed Inorganica, Chimica Analitica, Chimica Fisica Universit\`a degli Studi di Parma Viale delle Scienze 78 I-43100 Parma Italy ; _publ_contact_author_email 'tiri@unipr.it' _publ_contact_author_fax '[01039]521 905 5557' _publ_contact_author_phone '[01039]521 905 418' _publ_contact_letter ; ; _publ_requested_journal 'J. Chem. Soc., Dalton Trans.' _publ_requested_category ? _publ_requested_coeditor_name ? # AUTHOR LIST loop_ _publ_author_name _publ_author_address 'Tiripicchio Antonio','Ugozzoli Franco' et al. ; Dipartimento di Chimica Generale ed Inorganica, Chimica Analitica, Chimica Fisica Universit\`a degli Studi di Parma Centro di Studio per la Strutturistica Diffrattometrica del CNR Viale delle Scienze 78 I-43100 Parma Italy ; # TITLE _publ_section_title ;'Hydrocarbyl derivatives of dppm- or dppa-bridged alkoxysilyl hetero bimetallic Fe-Pd complexes and CO insertion reactions. Crystal structures of [(OC)3[(MeO)3Si]Fe(mu-dppm)Pd(8-mq)] (dppm= Ph2PCH2PPh2), [(OC)3Fe[mu-Si(OMe)2(OMe)](mu-dppa)PdCl] [(OC)3Fe[mu-Si(OMe)2(OMe)](mu-dppa)PdPh] (dppa=Ph2PNHPPh2) ; _publ_section_title_footnote ; ...... ; # TEXT _publ_section_abstract ; ...... ; _publ_section_comment ; ...... ; _publ_section_acknowledgements ; ...... ; _publ_section_references ; Nardelli, M.(1983). Comput. Chem. 7, 95-98. Nardelli, M.(1991). PARSTCIF. Program for Creating a CIF from the Output of PARST. University of Parma, Italy. Nardelli, M.(1995). J. Appl. Cryst. 28, 659. ; _publ_section_figure_captions ; ...... ; _publ_section_exptl_prep ; ...... ; _publ_section_exptl_refinement ; ...... ; _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement ? _computing_molecular_graphics ? _computing_publication_material ; PARST (Nardelli, 1983, 1995); PARSTCIF (Nardelli, 1991) ; #-------------------------- data section of block --------------------------- data_(I) # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_type_symbol _atom_type_number_in_cell _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source # # symbol number description f' f'' source # 'Pd' 4 'Palladium ' -0.9988 1.0072 'Int. Tab. C, 4.2.6.8, 6.1.1.4' 'Fe' 4 'Iron ' 0.3463 0.8444 'Int. Tab. C, 4.2.6.8, 6.1.1.4' 'P ' 8 'Phosphorus ' 0.1023 0.0942 'Int. Tab. C, 4.2.6.8, 6.1.1.4' 'Si' 4 'Silicium ' 0.0817 0.0704 'Int. Tab. C, 4.2.6.8, 6.1.1.4' 'O ' 24 'Oxygen ' 0.0106 0.0060 'Int. Tab. C, 4.2.6.8, 6.1.1.4' 'N ' 4 'Nitrogen ' 0.0061 0.0033 'Int. Tab. C, 4.2.6.8, 6.1.1.4' 'C ' 192 'Carbon ' 0.0033 0.0016 'Int. Tab. C, 4.2.6.8, 6.1.1.4' 'H ' 156 'Hydrogen ' 0.0000 0.0000 'Int. Tab. C, 4.2.6.8, 6.1.1.4' 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_type_symbol _atom_site_calc_flag _atom_site_occupancy _atom_site_disorder_group # # Table of coordinates # -------------------- # #label x/a y/b z/c Ueq tmf typ calc sof dis Pd 0.1262(1) 0.11220(0) 0.3618(1) 0.0518(3) Uani Pd . . . Fe 0.2390(2) 0.2329(1) 0.3736(1) 0.0537(7) Uani Fe . . . P1 0.0241(3) 0.1394(2) 0.2583(2) 0.0499(12) Uani P . . . P2 0.1775(3) 0.2571(2) 0.2614(2) 0.0520(12) Uani P . . . Si 0.3061(4) 0.2365(2) 0.4924(2) 0.0690(16) Uani Si . . . O1 0.4418(9) 0.2118(6) 0.5166(6) 0.0991(52) Uani O . . . O2 0.3156(9) 0.3089(5) 0.5291(6) 0.0933(46) Uani O . . . O3 0.2302(8) 0.1941(5) 0.5438(6) 0.0831(45) Uani O . . . O4 0.3815(11) 0.3463(6) 0.3777(7) 0.1146(65) Uani O . . . O5 0.0084(9) 0.2468(5) 0.4239(6) 0.0812(49) Uani O . . . O6 0.3900(8) 0.1265(4) 0.3448(6) 0.0768(42) Uani O . . . N 0.2141(10) 0.0554(5) 0.4464(6) 0.0587(47) Uani N . . . C1 0.5341(16) 0.2205(14) 0.4813(14) 0.151(13) Uani C . . . C2 0.2241(18) 0.3551(10) 0.5196(14) 0.127(11) Uani C . . . C3 0.2609(17) 0.1898(13) 0.6177(9) 0.121(11) Uani C . . . C4 0.3241(13) 0.3011(7) 0.3782(8) 0.0756(63) Uani C . . . C5 0.1012(13) 0.2402(6) 0.4039(7) 0.0593(56) Uani C . . . C6 0.3248(12) 0.1660(7) 0.3579(8) 0.0606(54) Uani C . . . C7 -0.1352(11) 0.1299(6) 0.2528(7) 0.0517(51) Uiso C . . . C8 -0.1931(13) 0.0830(7) 0.2112(8) 0.0772(68) Uiso C . . . C9 -0.3180(16) 0.0753(9) 0.2134(10) 0.0597(49) Uiso C . . . C10 -0.3700(18) 0.1143(9) 0.2555(10) 0.0793(71) Uiso C . . . C11 -0.3175(15) 0.1591(8) 0.2961(9) 0.1015(86) Uiso C . . . C12 -0.1933(13) 0.1680(8) 0.2965(8) 0.0870(72) Uiso C . . . C13 0.0638(11) 0.0938(6) 0.1828(7) 0.0767(63) Uiso C . . . C14 0.0175(12) 0.1055(7) 0.1150(8) 0.0571(56) Uiso C . . . C15 0.0492(15) 0.0729(8) 0.0584(11) 0.0772(69) Uiso C . . . C16 0.1362(17) 0.0274(10) 0.0695(12) 0.1054(86) Uiso C . . . C17 0.1848(16) 0.0142(9) 0.1376(10) 0.1020(90) Uiso C . . . C18 0.1516(13) 0.0470(7) 0.1961(9) 0.0782(45) Uiso C . . . C19 0.0355(10) 0.2226(5) 0.2310(8) 0.0391(73) Uani C . . . C20 0.1430(10) 0.3406(6) 0.2409(7) 0.0523(32) Uiso C . . . C21 0.0664(14) 0.3707(8) 0.2798(10) 0.0889(49) Uiso C . . . C22 0.0298(16) 0.4349(9) 0.2663(10) 0.0972(55) Uiso C . . . C23 0.0751(14) 0.4665(8) 0.2132(8) 0.0795(47) Uiso C . . . C24 0.1543(15) 0.4384(9) 0.1745(10) 0.0898(52) Uiso C . . . C25 0.1879(13) 0.3733(7) 0.1876(8) 0.0695(41) Uiso C . . . C26 0.2710(12) 0.2371(6) 0.1938(7) 0.0610(37) Uiso C . . . C27 0.3901(14) 0.2421(8) 0.2109(10) 0.0872(48) Uiso C . . . C28 0.4676(19) 0.2330(9) 0.1601(10) 0.1038(60) Uiso C . . . C29 0.4247(18) 0.2160(8) 0.0934(11) 0.1016(58) Uiso C . . . C30 0.3061(19) 0.2101(10) 0.0750(13) 0.1223(71) Uiso C . . . C31 0.2308(17) 0.2221(8) 0.1269(9) 0.0939(52) Uiso C . . . C32 0.0131(12) 0.0361(7) 0.3543(10) 0.0529(96) Uani C . . . C33 0.0573(13) -0.0140(6) 0.4083(7) 0.0675(98) Uani C . . . C34 -0.0008(15) -0.0713(7) 0.4143(9) 0.091(12) Uani C . . . C35 0.0429(19) -0.1174(8) 0.4655(11) 0.132(17) Uani C . . . C36 0.1415(16) -0.1071(8) 0.5087(9) 0.099(13) Uani C . . . C37 0.2030(14) -0.0484(7) 0.5050(8) 0.069(11) Uani C . . . C38 0.1579(12) -0.0020(6) 0.4545(7) 0.0626(91) Uani C . . . C39 0.3076(14) 0.0671(7) 0.4876(9) 0.074(11) Uani C . . . C40 0.3606(16) 0.0234(10) 0.5397(10) 0.085(13) Uani C . . . C41 0.3066(17) -0.0332(10) 0.5480(10) 0.108(15) Uani C . . . C42 0.1369(32) 0.0946(17) 0.7739(21) 0.229(14) Uiso C . . . C43 0.1078(53) 0.1091(30) 0.8130(35) 0.336(29) Uiso C . . . C44 0.1587(45) 0.0683(24) 0.8845(26) 0.321(22) Uiso C . . . C45 0.2569(39) 0.0898(23) 0.9011(23) 0.2500(0) Uiso C . . . C46 0.2583(25) 0.1689(14) 0.8676(16) 0.1630(97) Uiso C . . . C47 0.1831(38) 0.1707(20) 0.8088(22) 0.261(16) Uiso C . . . C48 0.4535(38) 0.0240(22) 0.0227(24) 0.296(21) Uiso C . . . H1A 0.59550(0) 0.19980(0) 0.51560(0) 0.228(55) Uiso H calc . . H1B 0.55180(0) 0.26680(0) 0.47770(0) 0.228(55) Uiso H calc . . H1C 0.53260(0) 0.20030(0) 0.43320(0) 0.228(55) Uiso H calc . . H2A 0.26920(0) 0.39340(0) 0.53820(0) 0.123(37) Uiso H calc . . H2B 0.17530(0) 0.33960(0) 0.55640(0) 0.123(37) Uiso H calc . . H2C 0.17260(0) 0.36650(0) 0.47490(0) 0.123(37) Uiso H calc . . H3A 0.18100(0) 0.17750(0) 0.62780(0) 0.097(45) Uiso H calc . . H3B 0.28420(0) 0.23050(0) 0.64290(0) 0.097(45) Uiso H calc . . H3C 0.31740(0) 0.15560(0) 0.63500(0) 0.097(45) Uiso H calc . . H8 -0.14870(0) 0.05500(0) 0.18120(0) 0.067(39) Uiso H calc . . H9 -0.36320(0) 0.04270(0) 0.18290(0) 0.306(75) Uiso H calc . . H10 -0.45510(0) 0.10760(0) 0.25750(0) 0.249(75) Uiso H calc . . H11 -0.36290(0) 0.18670(0) 0.32590(0) 0.186(57) Uiso H calc . . H12 -0.14900(0) 0.20060(0) 0.32750(0) 0.044(25) Uiso H calc . . H14 -0.04240(0) 0.13990(0) 0.10670(0) 0.083(32) Uiso H calc . . H15 0.01100(0) 0.08170(0) 0.00880(0) 0.136(63) Uiso H calc . . H16 0.16110(0) 0.00240(0) 0.02880(0) 0.223(72) Uiso H calc . . H17 0.24730(0) -0.01880(0) 0.14570(0) 0.238(70) Uiso H calc . . H18 0.18880(0) 0.03780(0) 0.24580(0) 0.069(32) Uiso H calc . . H19A 0.02330(0) 0.22420(0) 0.17750(0) 0.072(50) Uiso H calc . . H19B -0.02650(0) 0.24800(0) 0.25050(0) 0.041(44) Uiso H calc . . H21 0.03480(0) 0.34660(0) 0.31890(0) 0.157(56) Uiso H calc . . H22 -0.02590(0) 0.45620(0) 0.29540(0) 0.127(46) Uiso H calc . . H23 0.04980(0) 0.51120(0) 0.20190(0) 0.166(57) Uiso H calc . . H24 0.18900(0) 0.46370(0) 0.13740(0) 0.193(53) Uiso H calc . . H25 0.24270(0) 0.35170(0) 0.15820(0) 0.058(31) Uiso H calc . . H27 0.42180(0) 0.25310(0) 0.26110(0) 0.055(32) Uiso H calc . . H28 0.55330(0) 0.23960(0) 0.17270(0) 0.236(67) Uiso H calc . . H29 0.48070(0) 0.20890(0) 0.05760(0) 0.219(66) Uiso H calc . . H30 0.27510(0) 0.19590(0) 0.02560(0) 0.142(57) Uiso H calc . . H31 0.14450(0) 0.21860(0) 0.11460(0) 0.106(37) Uiso H calc . . H32A 0.00720(0) 0.01750(0) 0.30510(0) 0.125(63) Uiso H calc . . H32B -0.06560(0) 0.05090(0) 0.36410(0) 0.110(50) Uiso H calc . . H34 -0.07620(0) -0.07910(0) 0.38340(0) 0.190(63) Uiso H calc . . H35 -0.00080(0) -0.15810(0) 0.46900(0) 0.151(69) Uiso H calc . . H36 0.17330(0) -0.14110(0) 0.54280(0) 0.076(50) Uiso H calc . . H39 0.34560(0) 0.10940(0) 0.48250(0) 0.079(38) Uiso H calc . . H40 0.43500(0) 0.03450(0) 0.57000(0) 0.107(49) Uiso H calc . . H41 0.34180(0) -0.06410(0) 0.58490(0) 0.070(47) Uiso H calc . . 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 #label U11 U22 U33 U23 U13 U12 Pd 0.0421(5) 0.0408(5) 0.0712(7) 0.0073(6) 0.0020(4) -0.0026(5) Fe 0.0464(11) 0.0461(11) 0.0688(13) -0.0005(10) 0.0077(9) -0.0074(9) P1 0.0374(18) 0.0417(18) 0.0687(25) 0.0062(17) -0.0011(17) 0.0010(15) P2 0.0448(19) 0.0423(19) 0.0697(25) 0.0043(17) 0.0105(17) 0.0010(15) Si 0.0562(25) 0.0790(29) 0.0700(28) -0.0079(24) 0.0007(21) -0.0172(22) O1 0.0518(69) 0.1258(97) 0.1168(98) 0.0139(75) -0.0011(65) -0.0094(64) O2 0.0838(76) 0.0818(75) 0.1095(88) -0.0291(65) -0.0078(63) -0.0185(61) O3 0.0678(66) 0.1091(85) 0.0717(79) 0.0014(63) 0.0060(57) -0.0392(59) O4 0.121(11) 0.097(9) 0.124(11) 0.004(8) 0.007(8) -0.065(9) O5 0.0592(66) 0.0845(74) 0.1036(86) -0.0066(63) 0.0244(60) -0.0063(57) O6 0.0605(62) 0.0581(67) 0.1137(88) 0.0071(58) 0.0189(58) 0.0098(52) N 0.0504(74) 0.0515(68) 0.0725(83) 0.0079(59) 0.0003(63) 0.0015(55) C1 0.042(11) 0.266(28) 0.142(23) 0.003(20) 0.004(13) -0.021(14) C2 0.100(16) 0.109(17) 0.174(23) -0.083(16) 0.023(15) -0.014(14) C3 0.087(14) 0.208(25) 0.065(13) 0.006(14) -0.001(11) -0.059(15) C4 0.069(11) 0.068(10) 0.088(12) 0.004(9) 0.000(9) -0.014(8) C5 0.067(10) 0.052(9) 0.058(10) 0.000(8) 0.004(8) -0.012(8) C6 0.0516(85) 0.0587(93) 0.0710(99) 0.0038(77) 0.0052(72) -0.0132(75) C19 0.039(7) 0.039(7) 0.080(11) 0.003(6) 0.017(7) 0.002(6) C32 0.053(10) 0.061(9) 0.116(15) 0.033(10) 0.002(9) -0.015(7) C33 0.0675(98) 0.0593(88) 0.0536(91) 0.0004(72) 0.0130(79) -0.0013(74) C34 0.091(12) 0.058(10) 0.089(12) 0.004(9) 0.009(10) -0.020(9) C35 0.132(17) 0.046(10) 0.126(17) 0.022(11) 0.014(14) -0.003(11) C36 0.099(13) 0.057(10) 0.103(13) 0.042(10) 0.004(10) 0.004(10) C37 0.069(11) 0.075(11) 0.083(11) 0.020(9) -0.001(9) 0.010(9) C38 0.0626(91) 0.0485(82) 0.0615(96) 0.0063(71) 0.0134(78) 0.0038(69) C39 0.074(11) 0.071(10) 0.083(12) 0.021(9) -0.004(10) -0.007(9) C40 0.085(13) 0.118(16) 0.102(14) 0.024(13) -0.032(11) -0.023(12) C41 0.108(15) 0.098(17) 0.093(14) 0.049(13) -0.010(12) 0.007(13) # MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd FE 2.850(2) . . no Pd P1 2.227(4) . . no Pd N 2.15(1) . . no Pd C6 2.57(1) . . no Pd C32 2.06(1) . . no Fe P2 2.206(4) . . no Fe SI 2.279(4) . . no Fe C4 1.74(1) . . no Fe C5 1.76(1) . . no Fe C6 1.77(1) . . no P1 C7 1.84(1) . . no P1 C13 1.82(1) . . no P1 C19 1.83(1) . . no P2 C19 1.82(1) . . no P2 C20 1.83(1) . . no P2 C26 1.82(1) . . no Si O1 1.66(1) . . no Si O2 1.67(1) . . no Si O3 1.65(1) . . no O1 C1 1.34(2) . . no O2 C2 1.43(2) . . no O3 C3 1.40(2) . . no O4 C4 1.16(2) . . no O5 C5 1.19(1) . . no O6 C6 1.17(1) . . no N C38 1.39(1) . . no N C39 1.28(1) . . no C1 H1A 1.00(2) . . no C1 H1B 1.00(2) . . no C1 H1C 1.00(2) . . no C2 H2A 1.00(2) . . no C2 H2B 1.00(2) . . no C2 H2C 1.00(2) . . no C3 H3A 1.00(2) . . no C3 H3B 1.00(2) . . no C3 H3C 1.00(2) . . no C7 C8 1.38(1) . . no C7 C12 1.38(2) . . no C8 C9 1.46(2) . . no C8 H8 1.00(1) . . no C9 C10 1.33(2) . . no C9 H9 1.00(1) . . no C10 C11 1.31(2) . . no C10 H10 1.00(2) . . no C11 C12 1.45(2) . . no C11 H11 1.00(1) . . no C12 H12 1.00(1) . . no C13 C14 1.35(1) . . no C13 C18 1.41(1) . . no C14 C15 1.36(2) . . no C14 H14 1.00(1) . . no C15 C16 1.39(2) . . no C15 H15 1.00(1) . . no C16 C17 1.36(2) . . no C16 H16 1.00(2) . . no C17 C18 1.39(2) . . no C17 H17 1.00(1) . . no C18 H18 1.00(1) . . no C19 H19A 1.00(1) . . no C19 H19B 1.00(1) . . no C20 C21 1.37(2) . . no C20 C25 1.37(2) . . no C21 C22 1.43(2) . . no C21 H21 1.00(1) . . no C22 C23 1.36(2) . . no C22 H22 1.00(2) . . no C23 C24 1.37(2) . . no C23 H23 1.00(1) . . no C24 C25 1.44(2) . . no C24 H24 1.00(1) . . no C25 H25 1.00(1) . . no C26 C27 1.38(2) . . no C26 C31 1.33(2) . . no C27 C28 1.40(2) . . no C27 H27 1.00(1) . . no C28 C29 1.34(2) . . no C28 H28 1.00(2) . . no C29 C30 1.38(3) . . no C29 H29 1.00(2) . . no C30 C31 1.41(3) . . no C30 H30 1.00(2) . . no C31 H31 1.00(1) . . no C32 C33 1.51(2) . . no C32 H32A 1.00(1) . . no C32 H32B 1.00(1) . . no C33 C34 1.39(2) . . no C33 C38 1.39(1) . . no C34 C35 1.42(2) . . no C34 H34 1.00(1) . . no C35 C36 1.34(2) . . no C35 H35 1.00(1) . . no C36 C37 1.43(2) . . no C36 H36 1.00(1) . . no C37 C38 1.42(1) . . no C37 C41 1.40(2) . . no C39 C40 1.43(2) . . no C39 H39 1.00(1) . . no C40 C41 1.36(2) . . no C40 H40 1.00(1) . . no C41 H41 1.00(1) . . no C42 C43 0.90(7) . . no C42 C47 1.79(5) . . no C43 C44 1.64(7) . . no C43 C47 1.57(7) . . no C44 C45 1.23(6) . . no C45 C46 1.78(5) . . no C46 C47 1.32(4) . . no 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Fe Pd P1 91.6(1) . . . no Fe Pd N 105.5(3) . . . no Fe Pd C6 37.6(3) . . . no Fe Pd C32 167.9(4) . . . no P1 Pd N 161.0(3) . . . no P1 Pd C6 104.0(3) . . . no P1 Pd C32 82.8(5) . . . no N Pd C6 85.5(5) . . . no N Pd C32 81.8(5) . . . no C6 Pd C32 154.4(5) . . . no Pd Fe P2 92.3(1) . . . no Pd Fe Si 101.8(1) . . . no Pd Fe C4 172.4(5) . . . no Pd Fe C5 71.3(5) . . . no Pd Fe C6 62.5(5) . . . no P2 Fe Si 164.8(2) . . . no P2 Fe C4 88.4(5) . . . no P2 Fe C5 95.3(4) . . . no P2 Fe C6 98.4(5) . . . no Si Fe C4 78.5(5) . . . no Si Fe C5 83.8(5) . . . no Si Fe C6 93.4(5) . . . no C4 Fe C5 116.2(7) . . . no C4 Fe C6 109.9(7) . . . no C5 Fe C6 132.2(7) . . . no Pd P1 C7 116.2(4) . . . no Pd P1 C13 113.1(5) . . . no Pd P1 C19 116.2(4) . . . no C7 P1 C13 104.2(6) . . . no C7 P1 C19 101.1(6) . . . no C13 P1 C19 104.5(6) . . . no Fe P2 C19 112.5(5) . . . no Fe P2 C20 117.4(5) . . . no Fe P2 C26 117.9(5) . . . no C19 P2 C20 98.7(5) . . . no C19 P2 C26 106.1(6) . . . no C20 P2 C26 101.9(6) . . . no Fe Si O1 117.1(4) . . . no Fe Si O2 115.7(4) . . . no Fe Si O3 114.7(4) . . . no O1 Si O2 99.2(6) . . . no O1 Si O3 102.8(6) . . . no O2 Si O3 105.3(6) . . . no Si O1 C1 127(1) . . . no Si O2 C2 124(1) . . . no Si O3 C3 122(1) . . . no Pd N C38 112.3(8) . . . no Pd N C39 129(1) . . . no C38 N C39 118(1) . . . no O1 C1 H1A 100(2) . . . no O1 C1 H1B 110(2) . . . no O1 C1 H1C 118(2) . . . no H1A C1 H1B 109(3) . . . no H1A C1 H1C 109(2) . . . no H1B C1 H1C 110(3) . . . no O2 C2 H2A 99(2) . . . no O2 C2 H2B 99(2) . . . no O2 C2 H2C 129(2) . . . no H2A C2 H2B 110(2) . . . no H2A C2 H2C 110(2) . . . no H2B C2 H2C 109(2) . . . no O3 C3 H3A 94(1) . . . no O3 C3 H3B 116(2) . . . no O3 C3 H3C 117(2) . . . no H3A C3 H3B 109(2) . . . no H3A C3 H3C 110(2) . . . no H3B C3 H3C 110(2) . . . no Fe C4 O4 177(1) . . . no Fe C5 O5 178(1) . . . no Pd C6 Fe 79.8(5) . . . no Pd C6 O6 107(1) . . . no Fe C6 O6 173(1) . . . no P1 C7 C8 121(1) . . . no P1 C7 C12 117(1) . . . no C8 C7 C12 121(1) . . . no C7 C8 C9 118(1) . . . no C7 C8 H8 120(1) . . . no C9 C8 H8 122(1) . . . no C8 C9 C10 118(2) . . . no C8 C9 H9 121(2) . . . no C10 C9 H9 121(2) . . . no C9 C10 C11 125(2) . . . no C9 C10 H10 117(2) . . . no C11 C10 H10 118(2) . . . no C10 C11 C12 119(2) . . . no C10 C11 H11 120(2) . . . no C12 C11 H11 121(2) . . . no C7 C12 C11 118(1) . . . no C7 C12 H12 120(1) . . . no C11 C12 H12 122(1) . . . no P1 C13 C14 122(1) . . . no P1 C13 C18 118(1) . . . no C14 C13 C18 119(1) . . . no C13 C14 C15 123(2) . . . no C13 C14 H14 118(1) . . . no C15 C14 H14 119(1) . . . no C14 C15 C16 119(2) . . . no C14 C15 H15 121(2) . . . no C16 C15 H15 120(2) . . . no C15 C16 C17 119(2) . . . no C15 C16 H16 121(2) . . . no C17 C16 H16 119(2) . . . no C16 C17 C18 121(2) . . . no C16 C17 H17 119(2) . . . no C18 C17 H17 119(2) . . . no C13 C18 C17 118(1) . . . no C13 C18 H18 121(1) . . . no C17 C18 H18 121(2) . . . no P1 C19 P2 112.6(6) . . . no P1 C19 H19A 108.0(9) . . . no P1 C19 H19B 109.1(8) . . . no P2 C19 H19A 108(1) . . . no P2 C19 H19B 109.3(9) . . . no H19A C19 H19B 109(1) . . . no P2 C20 C21 118(1) . . . no P2 C20 C25 123(1) . . . no C21 C20 C25 119(1) . . . no C20 C21 C22 123(2) . . . no C20 C21 H21 119(2) . . . no C22 C21 H21 119(2) . . . no C21 C22 C23 117(2) . . . no C21 C22 H22 121(2) . . . no C23 C22 H22 121(2) . . . no C22 C23 C24 122(2) . . . no C22 C23 H23 119(2) . . . no C24 C23 H23 119(2) . . . no C23 C24 C25 120(2) . . . no C23 C24 H24 120(2) . . . no C25 C24 H24 120(2) . . . no C20 C25 C24 119(1) . . . no C20 C25 H25 120(1) . . . no C24 C25 H25 121(1) . . . no P2 C26 C27 119(1) . . . no P2 C26 C31 123(1) . . . no C27 C26 C31 118(1) . . . no C26 C27 C28 122(2) . . . no C26 C27 H27 119(2) . . . no C28 C27 H27 119(2) . . . no C27 C28 C29 119(2) . . . no C27 C28 H28 121(2) . . . no C29 C28 H28 120(2) . . . no C28 C29 C30 120(2) . . . no C28 C29 H29 118(2) . . . no C30 C29 H29 121(2) . . . no C29 C30 C31 119(2) . . . no C29 C30 H30 120(2) . . . no C31 C30 H30 121(2) . . . no C26 C31 C30 122(2) . . . no C26 C31 H31 118(2) . . . no C30 C31 H31 121(2) . . . no Pd C32 C33 110(1) . . . no Pd C32 H32A 110(1) . . . no Pd C32 H32B 109(1) . . . no C33 C32 H32A 109(2) . . . no C33 C32 H32B 110(1) . . . no H32A C32 H32B 109(1) . . . no C32 C33 C34 122(1) . . . no C32 C33 C38 119(1) . . . no C34 C33 C38 119(1) . . . no C33 C34 C35 121(1) . . . no C33 C34 H34 119(2) . . . no C35 C34 H34 120(2) . . . no C34 C35 C36 121(2) . . . no C34 C35 H35 119(2) . . . no C36 C35 H35 120(2) . . . no C35 C36 C37 120(2) . . . no C35 C36 H36 120(2) . . . no C37 C36 H36 120(2) . . . no C36 C37 C38 119(1) . . . no C36 C37 C41 124(2) . . . no C38 C37 C41 117(1) . . . no N C38 C33 117(1) . . . no N C38 C37 122(1) . . . no C33 C38 C37 120(1) . . . no N C39 C40 124(2) . . . no N C39 H39 118(1) . . . no C40 C39 H39 119(2) . . . no C39 C40 C41 119(2) . . . no C39 C40 H40 121(2) . . . no C41 C40 H40 121(2) . . . no C37 C41 C40 120(2) . . . no C37 C41 H41 120(2) . . . no C40 C41 H41 120(2) . . . no C43 C42 C47 61(5) . . . no C42 C43 C44 111(6) . . . no C42 C43 C47 88(5) . . . no C44 C43 C47 109(4) . . . no C43 C44 C45 104(4) . . . no C44 C45 C46 108(4) . . . no C45 C46 C47 107(3) . . . no C42 C47 C43 30(3) . . . no C42 C47 C46 115(3) . . . no C43 C47 C46 104(4) . . . 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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag P1 Pd Fe P2 -12.9(2) . . . . no P1 Pd Fe Si 161.1(2) . . . . no P1 Pd Fe C4 -107(4) . . . . no P1 Pd Fe C5 81.9(5) . . . . no P1 Pd Fe C6 -111.1(6) . . . . no N Pd Fe P2 158.8(3) . . . . no N Pd Fe Si -27.2(3) . . . . no N Pd Fe C4 64(4) . . . . no N Pd Fe C5 -106.4(6) . . . . no N Pd Fe C6 60.5(6) . . . . no C6 Pd Fe P2 98.2(6) . . . . no C6 Pd Fe Si -87.8(6) . . . . no C6 Pd Fe C4 3(4) . . . . no C6 Pd Fe C5 -167.0(7) . . . . no C32 Pd Fe P2 -74(2) . . . . no C32 Pd Fe Si 99(2) . . . . no C32 Pd Fe C4 -169(4) . . . . no C32 Pd Fe C5 19(2) . . . . no C32 Pd Fe C6 -173(2) . . . . no Fe Pd P1 C7 -126.5(5) . . . . no Fe Pd P1 C13 113.2(5) . . . . no Fe Pd P1 C19 -7.6(5) . . . . no N Pd P1 C7 79(1) . . . . no N Pd P1 C13 -40(1) . . . . no N Pd P1 C19 -161(1) . . . . no C6 Pd P1 C7 -162.4(6) . . . . no C6 Pd P1 C13 77.3(6) . . . . no C6 Pd P1 C19 -43.6(6) . . . . no C32 Pd P1 C7 42.7(7) . . . . no C32 Pd P1 C13 -77.6(7) . . . . no C32 Pd P1 C19 161.5(7) . . . . no Fe Pd N C38 171.0(8) . . . . no Fe Pd N C39 -9(1) . . . . no P1 Pd N C38 -35(2) . . . . no P1 Pd N C39 144(1) . . . . no C6 Pd N C38 -156.8(9) . . . . no C6 Pd N C39 22(1) . . . . no C32 Pd N C38 0.9(9) . . . . no C32 Pd N C39 -179(1) . . . . no Fe Pd C6 O6 -176(1) . . . . no P1 Pd C6 Fe 74.0(5) . . . . no P1 Pd C6 O6 -102(1) . . . . no N Pd C6 Fe -122.7(5) . . . . no N Pd C6 O6 60(1) . . . . no C32 Pd C6 Fe 177(1) . . . . no C32 Pd C6 O6 0(2) . . . . no Fe Pd C32 C33 -129(2) . . . . no Fe Pd C32 H32A 110(2) . . . . no Fe Pd C32 H32B -9(3) . . . . no P1 Pd C32 C33 167(1) . . . . no P1 Pd C32 H32A 47(1) . . . . no P1 Pd C32 H32B -72(1) . . . . no N Pd C32 C33 -1(1) . . . . no N Pd C32 H32A -121(1) . . . . no N Pd C32 H32B 118(1) . . . . no C6 Pd C32 C33 59(2) . . . . no C6 Pd C32 H32A -60(2) . . . . no C6 Pd C32 H32B 179.4(8) . . . . no Pd Fe P2 C19 32.3(5) . . . . no Pd Fe P2 C20 145.7(5) . . . . no Pd Fe P2 C26 -91.7(5) . . . . no Si Fe P2 C19 -124.9(8) . . . . no Si Fe P2 C20 -11.4(9) . . . . no Si Fe P2 C26 111.1(8) . . . . no C4 Fe P2 C19 -155.3(7) . . . . no C4 Fe P2 C20 -41.8(7) . . . . no C4 Fe P2 C26 80.7(7) . . . . no C5 Fe P2 C19 -39.2(7) . . . . no C5 Fe P2 C20 74.3(7) . . . . no C5 Fe P2 C26 -163.2(7) . . . . no C6 Fe P2 C19 94.9(7) . . . . no C6 Fe P2 C20 -151.7(7) . . . . no C6 Fe P2 C26 -29.1(7) . . . . no Pd Fe Si O1 93.8(5) . . . . no Pd Fe Si O2 -149.8(5) . . . . no Pd Fe Si O3 -26.9(5) . . . . no P2 Fe Si O1 -109.5(8) . . . . no P2 Fe Si O2 6.9(9) . . . . no P2 Fe Si O3 129.8(7) . . . . no C4 Fe Si O1 -78.4(7) . . . . no C4 Fe Si O2 38.0(7) . . . . no C4 Fe Si O3 160.9(7) . . . . no C5 Fe Si O1 163.2(7) . . . . no C5 Fe Si O2 -80.3(7) . . . . no C5 Fe Si O3 42.5(6) . . . . no C6 Fe Si O1 31.1(7) . . . . no C6 Fe Si O2 147.6(7) . . . . no C6 Fe Si O3 -89.5(7) . . . . no Pd Fe C4 O4 64(*) . . . . no P2 Fe C4 O4 -30(*) . . . . no Si Fe C4 O4 157(*) . . . . no C5 Fe C4 O4 -125(*) . . . . no C6 Fe C4 O4 67(*) . . . . no Pd Fe C5 O5 -155(*) . . . . no P2 Fe C5 O5 -64(*) . . . . no Si Fe C5 O5 100(*) . . . . no C4 Fe C5 O5 26(*) . . . . no C6 Fe C5 O5 -170(*) . . . . no Pd Fe C6 O6 159(*) . . . . no P2 Fe C6 Pd -88.2(3) . . . . no P2 Fe C6 O6 71(*) . . . . no Si Fe C6 Pd 101.5(3) . . . . no Si Fe C6 O6 -98(*) . . . . no C4 Fe C6 Pd -179.5(5) . . . . no C4 Fe C6 O6 -19(*) . . . . no C5 Fe C6 Pd 16.7(9) . . . . no C5 Fe C6 O6 176(9) . . . . no Pd P1 C7 C8 -108(1) . . . . no Pd P1 C7 C12 65(1) . . . . no C13 P1 C7 C8 16(1) . . . . no C13 P1 C7 C12 -169(1) . . . . no C19 P1 C7 C8 124(1) . . . . no C19 P1 C7 C12 -60(1) . . . . no Pd P1 C13 C14 -175(1) . . . . no Pd P1 C13 C18 0(1) . . . . no C7 P1 C13 C14 57(1) . . . . no C7 P1 C13 C18 -126(1) . . . . no C19 P1 C13 C14 -48(1) . . . . no C19 P1 C13 C18 128(1) . . . . no Pd P1 C19 P2 31.7(8) . . . . no Pd P1 C19 H19A 151.3(7) . . . . no Pd P1 C19 H19B -89.9(9) . . . . no C7 P1 C19 P2 158.5(7) . . . . no C7 P1 C19 H19A -81(1) . . . . no C7 P1 C19 H19B 37(1) . . . . no C13 P1 C19 P2 -93.6(8) . . . . no C13 P1 C19 H19A 26(1) . . . . no C13 P1 C19 H19B 144.8(9) . . . . no Fe P2 C19 P1 -44.3(8) . . . . no Fe P2 C19 H19A -163.6(7) . . . . no Fe P2 C19 H19B 77(1) . . . . no C20 P2 C19 P1 -168.8(7) . . . . no C20 P2 C19 H19A 72(1) . . . . no C20 P2 C19 H19B -46(1) . . . . no C26 P2 C19 P1 86.0(8) . . . . no C26 P2 C19 H19A -32(1) . . . . no C26 P2 C19 H19B -152.5(9) . . . . no Fe P2 C20 C21 -52(1) . . . . no Fe P2 C20 C25 128(1) . . . . no C19 P2 C20 C21 67(1) . . . . no C19 P2 C20 C25 -110(1) . . . . no C26 P2 C20 C21 176(1) . . . . no C26 P2 C20 C25 -1(1) . . . . no Fe P2 C26 C27 -35(1) . . . . no Fe P2 C26 C31 149(1) . . . . no C19 P2 C26 C27 -162(1) . . . . no C19 P2 C26 C31 22(1) . . . . no C20 P2 C26 C27 94(1) . . . . no C20 P2 C26 C31 -80(1) . . . . no Fe Si O1 C1 37(2) . . . . no O2 Si O1 C1 -87(2) . . . . no O3 Si O1 C1 164(2) . . . . no Fe Si O2 C2 48(1) . . . . no O1 Si O2 C2 174(1) . . . . no O3 Si O2 C2 -79(1) . . . . no Fe Si O3 C3 178(1) . . . . no O1 Si O3 C3 50(1) . . . . no O2 Si O3 C3 -52(1) . . . . no Si O1 C1 H1A 178(1) . . . . no Si O1 C1 H1B 63(3) . . . . no Si O1 C1 H1C -63(3) . . . . no Si O2 C2 H2A -165(1) . . . . no Si O2 C2 H2B 82(2) . . . . no Si O2 C2 H2C -41(3) . . . . no Si O3 C3 H3A 158(1) . . . . no Si O3 C3 H3B 44(2) . . . . no Si O3 C3 H3C -87(2) . . . . no Pd N C38 C33 0(1) . . . . no Pd N C38 C37 177(1) . . . . no C39 N C38 C33 -178(1) . . . . no C39 N C38 C37 -1(2) . . . . no Pd N C39 C40 -176(1) . . . . no Pd N C39 H39 3(2) . . . . no C38 N C39 C40 3(2) . . . . no C38 N C39 H39 -177(1) . . . . no P1 C7 C8 C9 176(1) . . . . no P1 C7 C8 H8 -2(2) . . . . no C12 C7 C8 C9 1(2) . . . . no C12 C7 C8 H8 -177(1) . . . . no P1 C7 C12 C11 -176(1) . . . . no P1 C7 C12 H12 3(2) . . . . no C8 C7 C12 C11 -1(2) . . . . no C8 C7 C12 H12 178(1) . . . . no C7 C8 C9 C10 0(2) . . . . no C7 C8 C9 H9 178(2) . . . . no H8 C8 C9 C10 179(2) . . . . no H8 C8 C9 H9 -2(3) . . . . no C8 C9 C10 C11 0(3) . . . . no C8 C9 C10 H10 -177(2) . . . . no H9 C9 C10 C11 -178(2) . . . . no H9 C9 C10 H10 4(3) . . . . no C9 C10 C11 C12 0(3) . . . . no C9 C10 C11 H11 179(2) . . . . no H10 C10 C11 C12 177(2) . . . . no H10 C10 C11 H11 -2(3) . . . . no C10 C11 C12 C7 1(2) . . . . no C10 C11 C12 H12 -177(2) . . . . no H11 C11 C12 C7 -177(2) . . . . no H11 C11 C12 H12 2(3) . . . . no P1 C13 C14 C15 178(1) . . . . no P1 C13 C14 H14 -1(2) . . . . no C18 C13 C14 C15 2(2) . . . . no C18 C13 C14 H14 -177(1) . . . . no P1 C13 C18 C17 -176(1) . . . . no P1 C13 C18 H18 2(2) . . . . no C14 C13 C18 C17 0(2) . . . . no C14 C13 C18 H18 179(1) . . . . no C13 C14 C15 C16 -2(3) . . . . no C13 C14 C15 H15 178(2) . . . . no H14 C14 C15 C16 177(2) . . . . no H14 C14 C15 H15 -2(3) . . . . no C14 C15 C16 C17 3(3) . . . . no C14 C15 C16 H16 180(2) . . . . no H15 C15 C16 C17 -177(2) . . . . no H15 C15 C16 H16 0(3) . . . . no C15 C16 C17 C18 -1(3) . . . . no C15 C16 C17 H17 180(2) . . . . no H16 C16 C17 C18 -178(2) . . . . no H16 C16 C17 H17 3(3) . . . . no C16 C17 C18 C13 1(3) . . . . no C16 C17 C18 H18 -178(2) . . . . no H17 C17 C18 C13 179(2) . . . . no H17 C17 C18 H18 0(3) . . . . no P2 C20 C21 C22 -176(1) . . . . no P2 C20 C21 H21 2(2) . . . . no C25 C20 C21 C22 1(2) . . . . no C25 C20 C21 H21 -178(1) . . . . no P2 C20 C25 C24 179(1) . . . . no P2 C20 C25 H25 0(2) . . . . no C21 C20 C25 C24 1(2) . . . . no C21 C20 C25 H25 -178(1) . . . . no C20 C21 C22 C23 0(3) . . . . no C20 C21 C22 H22 -179(2) . . . . no H21 C21 C22 C23 179(2) . . . . no H21 C21 C22 H22 1(3) . . . . no C21 C22 C23 C24 0(3) . . . . no C21 C22 C23 H23 179(2) . . . . no H22 C22 C23 C24 178(2) . . . . no H22 C22 C23 H23 -1(3) . . . . no C22 C23 C24 C25 3(3) . . . . no C22 C23 C24 H24 -176(2) . . . . no H23 C23 C24 C25 -176(2) . . . . no H23 C23 C24 H24 3(3) . . . . no C23 C24 C25 C20 -1(2) . . . . no C23 C24 C25 H25 177(2) . . . . no H24 C24 C25 C20 177(2) . . . . no H24 C24 C25 H25 -2(3) . . . . no P2 C26 C27 C28 -173(1) . . . . no P2 C26 C27 H27 5(2) . . . . no C31 C26 C27 C28 1(2) . . . . no C31 C26 C27 H27 -179(2) . . . . no P2 C26 C31 C30 177(1) . . . . no P2 C26 C31 H31 -4(2) . . . . no C27 C26 C31 C30 1(3) . . . . no C27 C26 C31 H31 -179(2) . . . . no C26 C27 C28 C29 -2(3) . . . . no C26 C27 C28 H28 176(2) . . . . no H27 C27 C28 C29 178(2) . . . . no H27 C27 C28 H28 -2(3) . . . . no C27 C28 C29 C30 2(3) . . . . no C27 C28 C29 H29 -178(2) . . . . no H28 C28 C29 C30 -176(2) . . . . no H28 C28 C29 H29 2(3) . . . . no C28 C29 C30 C31 0(3) . . . . no C28 C29 C30 H30 -177(2) . . . . no H29 C29 C30 C31 -177(2) . . . . no H29 C29 C30 H30 4(3) . . . . no C29 C30 C31 C26 -1(3) . . . . no C29 C30 C31 H31 179(2) . . . . no H30 C30 C31 C26 176(2) . . . . no H30 C30 C31 H31 -2(3) . . . . no Pd C32 C33 C34 -178(1) . . . . no Pd C32 C33 C38 3(2) . . . . no H32A C32 C33 C34 -57(2) . . . . no H32A C32 C33 C38 123(1) . . . . no H32B C32 C33 C34 61(2) . . . . no H32B C32 C33 C38 -116(2) . . . . no C32 C33 C34 C35 180(2) . . . . no C32 C33 C34 H34 -2(2) . . . . no C38 C33 C34 C35 0(2) . . . . no C38 C33 C34 H34 176(1) . . . . no C32 C33 C38 N -1(2) . . . . no C32 C33 C38 C37 -178(1) . . . . no C34 C33 C38 N 179(1) . . . . no C34 C33 C38 C37 2(2) . . . . no C33 C34 C35 C36 0(3) . . . . no C33 C34 C35 H35 180(2) . . . . no H34 C34 C35 C36 -177(2) . . . . no H34 C34 C35 H35 2(3) . . . . no C34 C35 C36 C37 2(3) . . . . no C34 C35 C36 H36 -176(2) . . . . no H35 C35 C36 C37 -178(2) . . . . no H35 C35 C36 H36 3(3) . . . . no C35 C36 C37 C38 0(2) . . . . no C35 C36 C37 C41 180(2) . . . . no H36 C36 C37 C38 178(1) . . . . no H36 C36 C37 C41 -1(3) . . . . no C36 C37 C38 N -177(1) . . . . no C36 C37 C38 C33 -1(2) . . . . no C41 C37 C38 N 1(2) . . . . no C41 C37 C38 C33 178(1) . . . . no C36 C37 C41 C40 179(2) . . . . no C36 C37 C41 H41 0(3) . . . . no C38 C37 C41 C40 0(3) . . . . no C38 C37 C41 H41 179(2) . . . . no N C39 C40 C41 -1(3) . . . . no N C39 C40 H40 179(2) . . . . no H39 C39 C40 C41 178(2) . . . . no H39 C39 C40 H40 0(3) . . . . no C39 C40 C41 C37 2(3) . . . . no C39 C40 C41 H41 -178(2) . . . . no H40 C40 C41 C37 -179(2) . . . . no H40 C40 C41 H41 0(3) . . . . no C47 C42 C43 C44 -109(6) . . . . no C43 C42 C47 C46 75(6) . . . . no C42 C43 C44 C45 78(7) . . . . no C47 C43 C44 C45 -17(6) . . . . no C42 C43 C47 C46 -114(5) . . . . no C44 C43 C47 C42 112(7) . . . . no C44 C43 C47 C46 -2(5) . . . . no C43 C44 C45 C46 26(5) . . . . no C44 C45 C46 C47 -30(5) . . . . no C45 C46 C47 C42 -13(4) . . . . no C45 C46 C47 C43 16(4) . . . . no # CHEMICAL DATA _chemical_name_systematic ; ..... ; _chemical_formula_analytical ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_sum 'Pd1 Fe1 P2 Si1 O6 N1 C47 H53 ' _chemical_formula_weight 980.22 _chemical_melting_point ? _chemical_compound_source ; ...... ; # CRYSTAL DATA _cell_length_a 11.562(2) _cell_length_b 21.028(3) _cell_length_c 18.837(3) _cell_angle_alpha 90.00(0) _cell_angle_beta 97.00(2) _cell_angle_gamma 90.00(0) _cell_volume 4546.(1) _cell_formula_units_Z 4.00 _cell_measurement_temperature 298K _cell_measurement_radiation 'Mokalpha' _cell_measurement_wavelength 0.71073 _cell_measurement_reflns_used 30 _cell_measurement_theta_min 13 _cell_measurement_theta_max 19 _symmetry_cell_setting 'monoclinic' _symmetry_space_group_name_H-M ' P 21/N ' _symmetry_Int_Tables_number ? _exptl_crystal_description ; ...... ; _exptl_crystal_colour ? _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 1.4323 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_F_000 2024.0 _exptl_absorpt_coefficient_mu 0.8596 _exptl_absorpt_correction_type ? _exptl_absorpt_process_details ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? # EXPERIMENTAL DATA _diffrn_special_details ; ....... ; _diffrn_ambient_temperature 298K _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type 'Mokapha' _diffrn_radiation_source ? _diffrn_radiation_monochromator 'graphite' _diffrn_radiation_detector ? _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? _reflns_number_total ? _reflns_number_gt ? _reflns_threshold_expression ? _diffrn_reflns_av_R_equivalents ? _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_number 8470 _diffrn_reflns_theta_min 3 _diffrn_reflns_theta_max 25 _diffrn_reflns_theta_full ? _diffrn_measured_fraction_theta_max ? _diffrn_measured_fraction_theta_full ? _reflns_d_resolution_high ? _reflns_d_resolution_low ? _diffrn_reflns_reduction_process ; ...... ; # REFINEMENT DATA _refine_special_details ; ...... ; _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens ? _refine_ls_hydrogen_treatment ? _refine_ls_structure_factor_coef ? _refine_ls_matrix_type ? _refine_ls_weighting_scheme ? _refine_ls_weighting_details ? _refine_ls_extinction_method ? _refine_ls_extinction_expression ? _refine_ls_extinction_coef ? _refine_ls_number_reflns 2910 _refine_ls_number_parameters 535 _refine_ls_number_restraints 0 _refine_ls_number_constraints 1 _refine_ls_R_factor_all 0.055 _refine_ls_R_factor_gt ? _refine_ls_wR_factor_all 0.075 _refine_ls_wR_factor_ref ? _refine_ls_goodness_of_fit_all 0.899 _refine_ls_goodness_of_fit_ref ? _refine_ls_restrained_S_all ? _refine_ls_restrained_S_obs ? _refine_ls_shift/su_max ? _refine_ls_shift/su_mean ? _refine_diff_density_max ? _refine_diff_density_min ? _refine_diff_density_rms ? loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' '-x,-y,-z' '-x+1/2,y+1/2,-z+1/2' 'x+1/2,-y+1/2,z+1/2' loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag #D H A D-H H..A D..A D-H..A A site sym Flg C14 H14 O2 1.00(1) 2.33(1) 3.22(2) 148.8(9) 4_454 ? # x-1/2,-y+1/2,+z-1/2 data_5bTHF _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C40 H43 Fe N O7 P2 Pd Si' _chemical_formula_weight 902.03 _chemical_melting_point ? _chemical_compound_source ? 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' 'O' 'O' 0.0106 0.0060 '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' 'Si' 'Si' 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pd' 'Pd' -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 19.6245(3) _cell_length_b 13.97780(10) _cell_length_c 29.5777(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 8113.4(2) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour brown _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.477 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3696 _exptl_absorpt_coefficient_mu 0.958 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens SMART CCD Detector' _diffrn_measurement_method omega-scans _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time 20 _diffrn_standards_decay_% ? _diffrn_reflns_number 43249 _diffrn_reflns_av_R_equivalents 0.0646 _diffrn_reflns_av_sigmaI/netI 0.0333 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -42 _diffrn_reflns_limit_l_max 40 _diffrn_reflns_theta_min 1.38 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7150 _reflns_number_observed 4860 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens SMART Software' _computing_cell_refinement 'Siemens SAINT Software' _computing_data_reduction 'Siemens SAINT Software' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL Software' _computing_publication_material 'Siemens SHELXTL Software' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 271 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0343P)^2^+12.7562P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00017(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 6879 _refine_ls_number_parameters 473 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0875 _refine_ls_R_factor_obs 0.0510 _refine_ls_wR_factor_all 0.1271 _refine_ls_wR_factor_obs 0.1013 _refine_ls_goodness_of_fit_all 1.155 _refine_ls_goodness_of_fit_obs 1.202 _refine_ls_restrained_S_all 1.224 _refine_ls_restrained_S_obs 1.202 _refine_ls_shift/esd_max 0.001 _refine_ls_shift/esd_mean 0.000 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Pd Pd 0.54022(2) 0.90936(3) 0.120268(14) 0.05519(14) Uani 1 d . . Fe Fe 0.56355(3) 0.72236(5) 0.12168(2) 0.0494(2) Uani 1 d . . Si Si 0.66778(8) 0.79333(12) 0.12234(6) 0.0720(5) Uani 1 d . . N1 N 0.4044(2) 0.7809(3) 0.12254(15) 0.0529(11) Uani 1 d . . H1 H 0.3678(25) 0.7797(36) 0.1243(16) 0.051(17) Uiso 1 d . . O1 O 0.6507(2) 0.9096(3) 0.11759(14) 0.0793(11) Uani 1 d . . C1 C 0.6989(3) 0.9861(5) 0.1236(2) 0.098(2) Uani 1 d . . H1A H 0.6765(3) 1.0464(5) 0.1191(2) 0.147 Uiso 1 calc R . H1B H 0.7353(3) 0.9794(5) 0.1021(2) 0.147 Uiso 1 calc R . H1C H 0.7172(3) 0.9836(5) 0.1537(2) 0.147 Uiso 1 calc R . P1 P 0.45514(6) 0.68333(8) 0.12083(4) 0.0453(3) Uani 1 d . . P2 P 0.43003(6) 0.89521(9) 0.12633(4) 0.0484(3) Uani 1 d . . O2 O 0.7127(2) 0.7910(4) 0.1690(2) 0.122(2) Uani 1 d . . C2 C 0.7456(5) 0.7224(6) 0.1895(3) 0.157(4) Uani 1 d . . H2A H 0.7664(5) 0.7470(6) 0.2164(3) 0.235 Uiso 1 calc R . H2B H 0.7801(5) 0.6975(6) 0.1698(3) 0.235 Uiso 1 calc R . H2C H 0.7143(5) 0.6722(6) 0.1973(3) 0.235 Uiso 1 calc R . O3 O 0.7221(2) 0.7733(5) 0.0819(2) 0.148(3) Uani 1 d . . C3 C 0.7300(5) 0.7099(6) 0.0505(3) 0.132(3) Uani 1 d . . H3A H 0.7700(5) 0.7248(6) 0.0332(3) 0.198 Uiso 1 calc R . H3B H 0.6909(5) 0.7100(6) 0.0311(3) 0.198 Uiso 1 calc R . H3C H 0.7351(5) 0.6479(6) 0.0640(3) 0.198 Uiso 1 calc R . O10 O 0.5557(2) 0.7839(3) 0.02703(14) 0.0839(12) Uani 1 d . . C10 C 0.5585(3) 0.7622(4) 0.0649(2) 0.0602(13) Uani 1 d . . O11 O 0.6245(2) 0.5321(3) 0.12076(13) 0.0790(11) Uani 1 d . . C11 C 0.5997(3) 0.6076(4) 0.1213(2) 0.0578(13) Uani 1 d . . C12 C 0.5594(3) 0.7600(4) 0.1786(2) 0.0595(13) Uiso 1 d . . O12 O 0.5556(2) 0.7800(3) 0.21676(14) 0.0800(11) Uiso 1 d . . C100 C 0.4254(2) 0.6212(4) 0.0700(2) 0.0521(12) Uani 1 d . . C101 C 0.4392(3) 0.5240(4) 0.0658(2) 0.0677(15) Uani 1 d . . H101 H 0.4595(3) 0.4910(4) 0.0895(2) 0.081 Uiso 1 calc R . C102 C 0.4225(4) 0.4765(6) 0.0263(3) 0.097(2) Uani 1 d . . H102 H 0.4318(4) 0.4116(6) 0.0234(3) 0.116 Uiso 1 calc R . C103 C 0.3923(4) 0.5255(7) -0.0087(2) 0.103(3) Uani 1 d . . H103 H 0.3807(4) 0.4930(7) -0.0351(2) 0.124 Uiso 1 calc R . C104 C 0.3791(4) 0.6208(6) -0.0053(2) 0.095(2) Uani 1 d . . H104 H 0.3591(4) 0.6535(6) -0.0292(2) 0.114 Uiso 1 calc R . C105 C 0.3959(3) 0.6687(4) 0.0342(2) 0.068(2) Uani 1 d . . H105 H 0.3871(3) 0.7339(4) 0.0366(2) 0.082 Uiso 1 calc R . C110 C 0.4217(2) 0.6052(3) 0.16521(15) 0.0464(11) Uani 1 d . . C111 C 0.4649(3) 0.5517(4) 0.1918(2) 0.0648(14) Uani 1 d . . H111 H 0.5117(3) 0.5581(4) 0.1881(2) 0.078 Uiso 1 calc R . C112 C 0.4401(3) 0.4887(5) 0.2238(2) 0.084(2) Uani 1 d . . H112 H 0.4702(3) 0.4522(5) 0.2409(2) 0.101 Uiso 1 calc R . C113 C 0.3710(4) 0.4800(5) 0.2304(2) 0.086(2) Uani 1 d . . H113 H 0.3543(4) 0.4376(5) 0.2520(2) 0.103 Uiso 1 calc R . C114 C 0.3267(3) 0.5344(4) 0.2049(2) 0.081(2) Uani 1 d . . H114 H 0.2800(3) 0.5302(4) 0.2098(2) 0.097 Uiso 1 calc R . C115 C 0.3518(3) 0.5952(4) 0.1718(2) 0.0679(15) Uani 1 d . . H115 H 0.3217(3) 0.6297(4) 0.1539(2) 0.081 Uiso 1 calc R . C200 C 0.3973(2) 0.9373(4) 0.1798(2) 0.0555(13) Uani 1 d . . C201 C 0.3796(3) 0.8747(5) 0.2141(2) 0.079(2) Uani 1 d . . H201 H 0.3818(3) 0.8091(5) 0.2090(2) 0.095 Uiso 1 calc R . C202 C 0.3586(4) 0.9082(6) 0.2558(2) 0.106(2) Uani 1 d . . H202 H 0.3472(4) 0.8653(6) 0.2786(2) 0.127 Uiso 1 calc R . C203 C 0.3546(4) 1.0035(7) 0.2632(2) 0.097(2) Uani 1 d . . H203 H 0.3395(4) 1.0254(7) 0.2912(2) 0.116 Uiso 1 calc R . C204 C 0.3721(3) 1.0681(5) 0.2308(2) 0.087(2) Uani 1 d . . H204 H 0.3699(3) 1.1333(5) 0.2367(2) 0.104 Uiso 1 calc R . C205 C 0.3933(3) 1.0352(4) 0.1889(2) 0.071(2) Uani 1 d . . H205 H 0.4049(3) 1.0789(4) 0.1665(2) 0.085 Uiso 1 calc R . C210 C 0.3778(2) 0.9527(3) 0.0833(2) 0.0470(11) Uani 1 d . . C211 C 0.4030(3) 0.9563(4) 0.0394(2) 0.0646(14) Uani 1 d . . H211 H 0.4465(3) 0.9338(4) 0.0330(2) 0.077 Uiso 1 calc R . C212 C 0.3627(3) 0.9938(4) 0.0051(2) 0.077(2) Uani 1 d . . H212 H 0.3796(3) 0.9969(4) -0.0242(2) 0.093 Uiso 1 calc R . C213 C 0.2982(3) 1.0262(4) 0.0142(2) 0.074(2) Uani 1 d . . H213 H 0.2717(3) 1.0516(4) -0.0090(2) 0.089 Uiso 1 calc R . C214 C 0.2726(3) 1.0212(4) 0.0568(2) 0.0667(15) Uani 1 d . . H214 H 0.2284(3) 1.0418(4) 0.0627(2) 0.080 Uiso 1 calc R . C215 C 0.3127(2) 0.9854(3) 0.0917(2) 0.0567(13) Uani 1 d . . H215 H 0.2954(2) 0.9834(3) 0.1210(2) 0.068 Uiso 1 calc R . C300 C 0.5332(2) 1.0559(3) 0.1219(2) 0.0552(12) Uani 1 d . . C301 C 0.5485(3) 1.1013(5) 0.1620(2) 0.093(2) Uani 1 d . . H301 H 0.5539(3) 1.0649(5) 0.1881(2) 0.111 Uiso 1 calc R . C302 C 0.5560(4) 1.1999(6) 0.1645(3) 0.112(3) Uani 1 d . . H302 H 0.5664(4) 1.2286(6) 0.1921(3) 0.135 Uiso 1 calc R . C303 C 0.5484(4) 1.2543(6) 0.1271(4) 0.125(4) Uani 1 d . . H303 H 0.5537(4) 1.3203(6) 0.1287(4) 0.150 Uiso 1 calc R . C304 C 0.5328(4) 1.2112(5) 0.0869(3) 0.104(3) Uani 1 d . . H304 H 0.5279(4) 1.2484(5) 0.0611(3) 0.125 Uiso 1 calc R . C305 C 0.5241(3) 1.1116(4) 0.0842(2) 0.072(2) Uani 1 d . . H305 H 0.5122(3) 1.0835(4) 0.0568(2) 0.086 Uiso 1 calc R . O400 O 0.2557(2) 0.7679(4) 0.1198(2) 0.103(2) Uani 1 d . . C401 C 0.2105(4) 0.7801(7) 0.1564(3) 0.130(3) Uani 1 d . . H40A H 0.2255(4) 0.8324(7) 0.1756(3) 0.156 Uiso 1 calc R . H40B H 0.2085(4) 0.7222(7) 0.1745(3) 0.156 Uiso 1 calc R . C402 C 0.1419(4) 0.8018(7) 0.1366(4) 0.166(5) Uani 1 d . . H40C H 0.1056(4) 0.7736(7) 0.1544(4) 0.199 Uiso 1 calc R . H40D H 0.1344(4) 0.8702(7) 0.1341(4) 0.199 Uiso 1 calc R . C403 C 0.1472(5) 0.7566(7) 0.0918(4) 0.165(5) Uani 1 d . . H40E H 0.1168(5) 0.7871(7) 0.0703(4) 0.198 Uiso 1 calc R . H40F H 0.1363(5) 0.6890(7) 0.0935(4) 0.198 Uiso 1 calc R . C404 C 0.2193(4) 0.7709(5) 0.0786(3) 0.123(3) Uani 1 d . . H40G H 0.2343(4) 0.7205(5) 0.0584(3) 0.148 Uiso 1 calc R . H40H H 0.2253(4) 0.8322(5) 0.0637(3) 0.148 Uiso 1 calc R . 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 Pd 0.0458(2) 0.0490(2) 0.0707(3) 0.0052(2) -0.0114(2) -0.0068(2) Fe 0.0444(4) 0.0503(4) 0.0536(4) -0.0007(3) -0.0079(3) 0.0011(3) Si 0.0441(8) 0.0789(11) 0.0932(12) -0.0069(10) -0.0112(8) -0.0013(7) N1 0.039(3) 0.045(2) 0.074(3) 0.008(2) -0.010(2) -0.002(2) O1 0.049(2) 0.072(2) 0.117(3) -0.002(2) -0.011(2) -0.017(2) C1 0.071(4) 0.088(5) 0.135(6) 0.001(4) -0.015(4) -0.038(4) P1 0.0455(7) 0.0427(6) 0.0477(6) 0.0038(6) -0.0068(6) -0.0011(5) P2 0.0447(7) 0.0449(7) 0.0554(8) 0.0047(6) -0.0105(6) -0.0017(5) O2 0.087(3) 0.126(4) 0.154(5) 0.014(4) -0.058(3) -0.004(3) C2 0.184(10) 0.116(7) 0.170(9) 0.021(7) -0.082(8) 0.006(7) O3 0.078(3) 0.160(5) 0.205(6) -0.089(5) 0.060(4) -0.040(3) C3 0.149(8) 0.118(7) 0.129(7) -0.001(6) 0.060(6) -0.003(6) O10 0.089(3) 0.102(3) 0.060(2) 0.017(2) -0.002(2) -0.007(3) C10 0.048(3) 0.063(3) 0.070(4) 0.004(3) -0.005(3) -0.003(2) O11 0.097(3) 0.072(3) 0.068(2) -0.008(2) -0.005(2) 0.032(2) C11 0.060(3) 0.065(3) 0.049(3) -0.006(3) -0.001(2) 0.009(3) C100 0.048(3) 0.060(3) 0.048(3) 0.002(2) 0.004(2) -0.017(2) C101 0.070(4) 0.066(4) 0.068(4) -0.020(3) 0.009(3) -0.013(3) C102 0.090(5) 0.096(5) 0.103(6) -0.043(5) 0.027(4) -0.026(4) C103 0.092(5) 0.156(8) 0.062(5) -0.040(5) 0.025(4) -0.056(6) C104 0.094(5) 0.143(7) 0.049(4) 0.007(4) -0.012(3) -0.052(5) C105 0.071(4) 0.082(4) 0.052(3) 0.012(3) -0.010(3) -0.026(3) C110 0.052(3) 0.039(3) 0.047(3) 0.003(2) 0.000(2) -0.003(2) C111 0.063(3) 0.069(3) 0.062(3) 0.015(3) -0.011(3) -0.001(3) C112 0.085(5) 0.088(5) 0.078(4) 0.033(4) -0.009(3) -0.002(4) C113 0.107(6) 0.084(5) 0.066(4) 0.029(3) 0.005(4) -0.015(4) C114 0.072(4) 0.082(4) 0.090(5) 0.020(4) 0.021(3) -0.001(3) C115 0.063(4) 0.062(3) 0.079(4) 0.015(3) 0.005(3) 0.008(3) C200 0.051(3) 0.060(3) 0.055(3) 0.001(3) -0.014(2) -0.003(2) C201 0.095(5) 0.074(4) 0.068(4) 0.012(3) -0.006(3) 0.011(3) C202 0.135(7) 0.123(7) 0.060(4) 0.018(5) 0.001(4) 0.015(6) C203 0.092(5) 0.149(8) 0.049(4) -0.020(5) -0.013(3) 0.016(5) C204 0.079(4) 0.097(5) 0.085(5) -0.032(4) -0.010(4) -0.001(4) C205 0.070(4) 0.070(4) 0.073(4) -0.011(3) -0.004(3) -0.012(3) C210 0.050(3) 0.036(2) 0.055(3) 0.005(2) -0.010(2) -0.002(2) C211 0.056(3) 0.070(4) 0.069(4) 0.010(3) -0.004(3) 0.011(3) C212 0.085(4) 0.091(5) 0.055(4) 0.016(3) -0.009(3) 0.010(4) C213 0.078(4) 0.070(4) 0.073(4) 0.012(3) -0.021(3) 0.018(3) C214 0.061(3) 0.062(3) 0.077(4) 0.003(3) -0.011(3) 0.018(3) C215 0.056(3) 0.048(3) 0.066(3) 0.002(3) -0.004(2) 0.009(2) C300 0.050(3) 0.045(3) 0.070(3) 0.004(3) 0.001(3) -0.011(2) C301 0.099(5) 0.082(5) 0.097(5) -0.001(4) -0.020(4) -0.029(4) C302 0.111(6) 0.075(5) 0.151(8) -0.032(5) -0.021(5) -0.024(5) C303 0.085(5) 0.058(5) 0.231(12) -0.017(7) -0.005(7) -0.014(4) C304 0.085(5) 0.069(5) 0.159(8) 0.048(5) 0.016(5) -0.003(4) C305 0.062(4) 0.071(4) 0.082(4) 0.016(3) 0.013(3) -0.007(3) O400 0.062(3) 0.110(4) 0.136(4) 0.036(3) -0.023(3) -0.004(3) C401 0.083(6) 0.126(7) 0.181(9) 0.016(7) 0.001(6) 0.005(5) C402 0.069(5) 0.127(8) 0.302(15) -0.080(9) -0.047(7) 0.022(5) C403 0.090(7) 0.110(8) 0.297(16) 0.000(9) -0.071(8) 0.006(5) C404 0.114(7) 0.076(5) 0.181(9) 0.017(5) -0.060(6) -0.020(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 Pd C300 2.054(5) . ? Pd O1 2.170(4) . ? Pd P2 2.1788(13) . ? Pd Fe 2.6539(8) . ? Pd Si 2.983(2) . ? Fe C11 1.754(5) . ? Fe C12 1.767(5) . ? Fe C10 1.772(6) . ? Fe P1 2.1965(14) . ? Fe Si 2.273(2) . ? Si O3 1.626(5) . ? Si O2 1.638(5) . ? Si O1 1.665(4) . ? N1 P2 1.678(4) . ? N1 P1 1.689(4) . ? N1 H1 0.72(5) . ? O1 C1 1.439(6) . ? C1 H1A 0.96 . ? C1 H1B 0.96 . ? C1 H1C 0.96 . ? P1 C110 1.829(4) . ? P1 C100 1.833(5) . ? P2 C200 1.806(5) . ? P2 C210 1.820(5) . ? O2 C2 1.304(8) . ? C2 H2A 0.96 . ? C2 H2B 0.96 . ? C2 H2C 0.96 . ? O3 C3 1.293(8) . ? C3 H3A 0.96 . ? C3 H3B 0.96 . ? C3 H3C 0.96 . ? O10 C10 1.162(6) . ? O11 C11 1.163(6) . ? C12 O12 1.164(6) . ? C100 C105 1.376(7) . ? C100 C101 1.390(7) . ? C101 C102 1.382(8) . ? C101 H101 0.93 . ? C102 C103 1.376(10) . ? C102 H102 0.93 . ? C103 C104 1.361(10) . ? C103 H103 0.93 . ? C104 C105 1.387(8) . ? C104 H104 0.93 . ? C105 H105 0.93 . ? C110 C111 1.376(6) . ? C110 C115 1.393(7) . ? C111 C112 1.380(7) . ? C111 H111 0.93 . ? C112 C113 1.375(9) . ? C112 H112 0.93 . ? C113 C114 1.380(8) . ? C113 H113 0.93 . ? C114 C115 1.386(7) . ? C114 H114 0.93 . ? C115 H115 0.93 . ? C200 C201 1.385(7) . ? C200 C205 1.397(7) . ? C201 C202 1.381(9) . ? C201 H201 0.93 . ? C202 C203 1.353(10) . ? C202 H202 0.93 . ? C203 C204 1.360(9) . ? C203 H203 0.93 . ? C204 C205 1.385(8) . ? C204 H204 0.93 . ? C205 H205 0.93 . ? C210 C215 1.380(6) . ? C210 C211 1.391(7) . ? C211 C212 1.389(7) . ? C211 H211 0.93 . ? C212 C213 1.371(8) . ? C212 H212 0.93 . ? C213 C214 1.359(8) . ? C213 H213 0.93 . ? C214 C215 1.390(7) . ? C214 H214 0.93 . ? C215 H215 0.93 . ? C300 C305 1.371(7) . ? C300 C301 1.380(8) . ? C301 C302 1.388(9) . ? C301 H301 0.93 . ? C302 C303 1.351(11) . ? C302 H302 0.93 . ? C303 C304 1.366(11) . ? C303 H303 0.93 . ? C304 C305 1.405(9) . ? C304 H304 0.93 . ? C305 H305 0.93 . ? O400 C401 1.410(9) . ? O400 C404 1.415(8) . ? C401 C402 1.500(10) . ? C401 H40A 0.97 . ? C401 H40B 0.97 . ? C402 C403 1.472(14) . ? C402 H40C 0.97 . ? C402 H40D 0.97 . ? C403 C404 1.481(12) . ? C403 H40E 0.97 . ? C403 H40F 0.97 . ? C404 H40G 0.97 . ? C404 H40H 0.97 . ? 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 C300 Pd O1 93.8(2) . . ? C300 Pd P2 91.25(14) . . ? O1 Pd P2 174.23(11) . . ? C300 Pd Fe 173.54(14) . . ? O1 Pd Fe 80.19(10) . . ? P2 Pd Fe 94.62(4) . . ? C300 Pd Si 126.75(14) . . ? O1 Pd Si 33.18(11) . . ? P2 Pd Si 141.42(5) . . ? Fe Pd Si 47.12(4) . . ? C11 Fe C12 107.3(2) . . ? C11 Fe C10 107.7(2) . . ? C12 Fe C10 143.9(2) . . ? C11 Fe P1 99.5(2) . . ? C12 Fe P1 92.3(2) . . ? C10 Fe P1 90.8(2) . . ? C11 Fe Si 92.0(2) . . ? C12 Fe Si 84.4(2) . . ? C10 Fe Si 85.5(2) . . ? P1 Fe Si 168.51(6) . . ? C11 Fe Pd 166.0(2) . . ? C12 Fe Pd 73.4(2) . . ? C10 Fe Pd 70.5(2) . . ? P1 Fe Pd 94.44(4) . . ? Si Fe Pd 74.08(5) . . ? O3 Si O2 105.3(3) . . ? O3 Si O1 103.7(3) . . ? O2 Si O1 101.5(3) . . ? O3 Si Fe 120.5(2) . . ? O2 Si Fe 118.9(2) . . ? O1 Si Fe 104.15(14) . . ? O3 Si Pd 128.9(3) . . ? O2 Si Pd 118.7(2) . . ? O1 Si Pd 45.51(12) . . ? Fe Si Pd 58.81(4) . . ? P2 N1 P1 126.5(3) . . ? P2 N1 H1 108.4(41) . . ? P1 N1 H1 124.8(42) . . ? C1 O1 Si 125.7(4) . . ? C1 O1 Pd 130.8(4) . . ? Si O1 Pd 101.3(2) . . ? O1 C1 H1A 109.5(3) . . ? O1 C1 H1B 109.5(3) . . ? H1A C1 H1B 109.5 . . ? O1 C1 H1C 109.5(3) . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N1 P1 C110 104.5(2) . . ? N1 P1 C100 102.7(2) . . ? C110 P1 C100 101.1(2) . . ? N1 P1 Fe 111.7(2) . . ? C110 P1 Fe 119.2(2) . . ? C100 P1 Fe 115.8(2) . . ? N1 P2 C200 105.2(2) . . ? N1 P2 C210 101.8(2) . . ? C200 P2 C210 105.6(2) . . ? N1 P2 Pd 112.2(2) . . ? C200 P2 Pd 113.3(2) . . ? C210 P2 Pd 117.5(2) . . ? C2 O2 Si 132.2(6) . . ? O2 C2 H2A 109.5(5) . . ? O2 C2 H2B 109.5(6) . . ? H2A C2 H2B 109.5 . . ? O2 C2 H2C 109.5(5) . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C3 O3 Si 136.5(5) . . ? O3 C3 H3A 109.5(4) . . ? O3 C3 H3B 109.5(5) . . ? H3A C3 H3B 109.5 . . ? O3 C3 H3C 109.5(5) . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? O10 C10 Fe 176.8(5) . . ? O11 C11 Fe 179.0(5) . . ? O12 C12 Fe 176.5(5) . . ? C105 C100 C101 119.0(5) . . ? C105 C100 P1 122.4(4) . . ? C101 C100 P1 118.3(4) . . ? C102 C101 C100 119.9(6) . . ? C102 C101 H101 120.1(5) . . ? C100 C101 H101 120.1(3) . . ? C103 C102 C101 120.0(7) . . ? C103 C102 H102 120.0(5) . . ? C101 C102 H102 120.0(5) . . ? C104 C103 C102 120.8(7) . . ? C104 C103 H103 119.6(5) . . ? C102 C103 H103 119.6(5) . . ? C103 C104 C105 119.3(7) . . ? C103 C104 H104 120.3(5) . . ? C105 C104 H104 120.3(4) . . ? C100 C105 C104 121.0(6) . . ? C100 C105 H105 119.5(3) . . ? C104 C105 H105 119.5(4) . . ? C111 C110 C115 118.1(5) . . ? C111 C110 P1 120.9(4) . . ? C115 C110 P1 120.9(4) . . ? C110 C111 C112 121.5(5) . . ? C110 C111 H111 119.3(3) . . ? C112 C111 H111 119.3(4) . . ? C113 C112 C111 120.0(6) . . ? C113 C112 H112 120.0(4) . . ? C111 C112 H112 120.0(4) . . ? C112 C113 C114 119.6(6) . . ? C112 C113 H113 120.2(4) . . ? C114 C113 H113 120.2(4) . . ? C113 C114 C115 120.0(6) . . ? C113 C114 H114 120.0(4) . . ? C115 C114 H114 120.0(4) . . ? C114 C115 C110 120.7(5) . . ? C114 C115 H115 119.6(4) . . ? C110 C115 H115 119.6(3) . . ? C201 C200 C205 117.6(5) . . ? C201 C200 P2 121.7(4) . . ? C205 C200 P2 120.5(4) . . ? C202 C201 C200 121.0(6) . . ? C202 C201 H201 119.5(5) . . ? C200 C201 H201 119.5(4) . . ? C203 C202 C201 119.7(7) . . ? C203 C202 H202 120.1(5) . . ? C201 C202 H202 120.1(4) . . ? C202 C203 C204 121.6(7) . . ? C202 C203 H203 119.2(5) . . ? C204 C203 H203 119.2(4) . . ? C203 C204 C205 119.1(7) . . ? C203 C204 H204 120.5(4) . . ? C205 C204 H204 120.5(4) . . ? C204 C205 C200 120.9(6) . . ? C204 C205 H205 119.5(4) . . ? C200 C205 H205 119.5(3) . . ? C215 C210 C211 118.9(4) . . ? C215 C210 P2 122.9(4) . . ? C211 C210 P2 118.0(4) . . ? C212 C211 C210 119.6(5) . . ? C212 C211 H211 120.2(4) . . ? C210 C211 H211 120.2(3) . . ? C213 C212 C211 120.5(6) . . ? C213 C212 H212 119.8(3) . . ? C211 C212 H212 119.8(4) . . ? C214 C213 C212 120.3(5) . . ? C214 C213 H213 119.8(3) . . ? C212 C213 H213 119.8(3) . . ? C213 C214 C215 119.9(5) . . ? C213 C214 H214 120.0(3) . . ? C215 C214 H214 120.0(3) . . ? C210 C215 C214 120.7(5) . . ? C210 C215 H215 119.7(3) . . ? C214 C215 H215 119.7(3) . . ? C305 C300 C301 117.8(5) . . ? C305 C300 Pd 123.8(4) . . ? C301 C300 Pd 117.6(4) . . ? C300 C301 C302 121.7(7) . . ? C300 C301 H301 119.1(4) . . ? C302 C301 H301 119.1(5) . . ? C303 C302 C301 120.2(8) . . ? C303 C302 H302 119.9(5) . . ? C301 C302 H302 119.9(5) . . ? C302 C303 C304 119.3(7) . . ? C302 C303 H303 120.3(5) . . ? C304 C303 H303 120.3(5) . . ? C303 C304 C305 120.9(7) . . ? C303 C304 H304 119.5(5) . . ? C305 C304 H304 119.5(5) . . ? C300 C305 C304 120.0(6) . . ? C300 C305 H305 120.0(3) . . ? C304 C305 H305 120.0(5) . . ? C401 O400 C404 109.9(6) . . ? O400 C401 C402 106.8(8) . . ? O400 C401 H40A 110.4(4) . . ? C402 C401 H40A 110.4(5) . . ? O400 C401 H40B 110.4(4) . . ? C402 C401 H40B 110.4(6) . . ? H40A C401 H40B 108.6 . . ? C403 C402 C401 101.6(8) . . ? C403 C402 H40C 111.4(6) . . ? C401 C402 H40C 111.4(6) . . ? C403 C402 H40D 111.4(6) . . ? C401 C402 H40D 111.4(5) . . ? H40C C402 H40D 109.3 . . ? C402 C403 C404 104.3(8) . . ? C402 C403 H40E 110.9(5) . . ? C404 C403 H40E 110.9(5) . . ? C402 C403 H40F 110.9(7) . . ? C404 C403 H40F 110.9(5) . . ? H40E C403 H40F 108.9 . . ? O400 C404 C403 104.5(8) . . ? O400 C404 H40G 110.8(4) . . ? C403 C404 H40G 110.8(6) . . ? O400 C404 H40H 110.8(4) . . ? C403 C404 H40H 110.8(5) . . ? H40G C404 H40H 108.9 . . ? 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 C300 Pd Fe C11 -25.2(15) . . . . ? O1 Pd Fe C11 -2.9(7) . . . . ? P2 Pd Fe C11 179.6(7) . . . . ? Si Pd Fe C11 -5.9(7) . . . . ? C300 Pd Fe C12 69.6(13) . . . . ? O1 Pd Fe C12 91.9(2) . . . . ? P2 Pd Fe C12 -85.6(2) . . . . ? Si Pd Fe C12 88.9(2) . . . . ? C300 Pd Fe C10 -110.1(13) . . . . ? O1 Pd Fe C10 -87.7(2) . . . . ? P2 Pd Fe C10 94.8(2) . . . . ? Si Pd Fe C10 -90.8(2) . . . . ? C300 Pd Fe P1 160.7(13) . . . . ? O1 Pd Fe P1 -176.99(12) . . . . ? P2 Pd Fe P1 5.54(5) . . . . ? Si Pd Fe P1 179.95(7) . . . . ? C300 Pd Fe Si -19.3(13) . . . . ? O1 Pd Fe Si 3.05(12) . . . . ? P2 Pd Fe Si -174.42(6) . . . . ? Si Pd Fe Si 0.0 . . . . ? C11 Fe Si O3 58.9(4) . . . . ? C12 Fe Si O3 166.0(4) . . . . ? C10 Fe Si O3 -48.7(4) . . . . ? P1 Fe Si O3 -119.9(4) . . . . ? Pd Fe Si O3 -119.7(3) . . . . ? C11 Fe Si O2 -73.6(3) . . . . ? C12 Fe Si O2 33.6(3) . . . . ? C10 Fe Si O2 178.9(3) . . . . ? P1 Fe Si O2 107.6(4) . . . . ? Pd Fe Si O2 107.9(3) . . . . ? C11 Fe Si O1 174.5(2) . . . . ? C12 Fe Si O1 -78.3(2) . . . . ? C10 Fe Si O1 67.0(2) . . . . ? P1 Fe Si O1 -4.3(4) . . . . ? Pd Fe Si O1 -4.0(2) . . . . ? C11 Fe Si Pd 178.6(2) . . . . ? C12 Fe Si Pd -74.3(2) . . . . ? C10 Fe Si Pd 71.0(2) . . . . ? P1 Fe Si Pd -0.2(3) . . . . ? Pd Fe Si Pd 0.0 . . . . ? C300 Pd Si O3 -76.7(3) . . . . ? O1 Pd Si O3 -68.6(3) . . . . ? P2 Pd Si O3 114.9(3) . . . . ? Fe Pd Si O3 105.9(3) . . . . ? C300 Pd Si O2 69.2(3) . . . . ? O1 Pd Si O2 77.3(3) . . . . ? P2 Pd Si O2 -99.2(2) . . . . ? Fe Pd Si O2 -108.2(2) . . . . ? C300 Pd Si O1 -8.2(3) . . . . ? O1 Pd Si O1 0.0 . . . . ? P2 Pd Si O1 -176.6(2) . . . . ? Fe Pd Si O1 174.5(2) . . . . ? C300 Pd Si Fe 177.3(2) . . . . ? O1 Pd Si Fe -174.5(2) . . . . ? P2 Pd Si Fe 8.95(10) . . . . ? Fe Pd Si Fe 0.0 . . . . ? O3 Si O1 C1 -63.7(5) . . . . ? O2 Si O1 C1 45.4(5) . . . . ? Fe Si O1 C1 169.4(5) . . . . ? Pd Si O1 C1 164.5(6) . . . . ? O3 Si O1 Pd 131.8(3) . . . . ? O2 Si O1 Pd -119.1(3) . . . . ? Fe Si O1 Pd 4.9(2) . . . . ? Pd Si O1 Pd 0.0 . . . . ? C300 Pd O1 C1 10.1(5) . . . . ? P2 Pd O1 C1 -141.5(10) . . . . ? Fe Pd O1 C1 -167.4(5) . . . . ? Si Pd O1 C1 -163.3(6) . . . . ? C300 Pd O1 Si 173.5(2) . . . . ? P2 Pd O1 Si 21.9(13) . . . . ? Fe Pd O1 Si -4.1(2) . . . . ? Si Pd O1 Si 0.0 . . . . ? P2 N1 P1 C110 128.0(3) . . . . ? P2 N1 P1 C100 -126.9(3) . . . . ? P2 N1 P1 Fe -2.1(4) . . . . ? C11 Fe P1 N1 178.4(2) . . . . ? C12 Fe P1 N1 70.4(2) . . . . ? C10 Fe P1 N1 -73.6(2) . . . . ? Si Fe P1 N1 -2.8(4) . . . . ? Pd Fe P1 N1 -3.1(2) . . . . ? C11 Fe P1 C110 56.4(2) . . . . ? C12 Fe P1 C110 -51.6(2) . . . . ? C10 Fe P1 C110 164.4(2) . . . . ? Si Fe P1 C110 -124.8(3) . . . . ? Pd Fe P1 C110 -125.1(2) . . . . ? C11 Fe P1 C100 -64.5(2) . . . . ? C12 Fe P1 C100 -172.5(3) . . . . ? C10 Fe P1 C100 43.5(3) . . . . ? Si Fe P1 C100 114.2(4) . . . . ? Pd Fe P1 C100 114.0(2) . . . . ? P1 N1 P2 C200 -116.2(3) . . . . ? P1 N1 P2 C210 133.9(3) . . . . ? P1 N1 P2 Pd 7.4(4) . . . . ? C300 Pd P2 N1 175.3(2) . . . . ? O1 Pd P2 N1 -33.0(12) . . . . ? Fe Pd P2 N1 -7.4(2) . . . . ? Si Pd P2 N1 -14.0(2) . . . . ? C300 Pd P2 C200 -65.7(2) . . . . ? O1 Pd P2 C200 85.9(11) . . . . ? Fe Pd P2 C200 111.6(2) . . . . ? Si Pd P2 C200 105.0(2) . . . . ? C300 Pd P2 C210 57.8(2) . . . . ? O1 Pd P2 C210 -150.5(11) . . . . ? Fe Pd P2 C210 -124.9(2) . . . . ? Si Pd P2 C210 -131.4(2) . . . . ? O3 Si O2 C2 -66.4(9) . . . . ? O1 Si O2 C2 -174.2(9) . . . . ? Fe Si O2 C2 72.4(9) . . . . ? Pd Si O2 C2 140.5(8) . . . . ? O2 Si O3 C3 120.3(10) . . . . ? O1 Si O3 C3 -133.5(10) . . . . ? Fe Si O3 C3 -17.6(12) . . . . ? Pd Si O3 C3 -90.4(10) . . . . ? C11 Fe C10 O10 15.8(83) . . . . ? C12 Fe C10 O10 -179.4(1000) . . . . ? P1 Fe C10 O10 -84.4(83) . . . . ? Si Fe C10 O10 106.5(83) . . . . ? Pd Fe C10 O10 -178.8(1000) . . . . ? C12 Fe C11 O11 -108.8(238) . . . . ? C10 Fe C11 O11 61.9(239) . . . . ? P1 Fe C11 O11 155.7(238) . . . . ? Si Fe C11 O11 -24.0(238) . . . . ? Pd Fe C11 O11 -18.3(243) . . . . ? C11 Fe C12 O12 -41.1(75) . . . . ? C10 Fe C12 O12 154.0(73) . . . . ? P1 Fe C12 O12 59.5(75) . . . . ? Si Fe C12 O12 -131.5(75) . . . . ? Pd Fe C12 O12 153.5(75) . . . . ? N1 P1 C100 C105 27.3(5) . . . . ? C110 P1 C100 C105 135.0(4) . . . . ? Fe P1 C100 C105 -94.7(4) . . . . ? N1 P1 C100 C101 -159.0(4) . . . . ? C110 P1 C100 C101 -51.2(4) . . . . ? Fe P1 C100 C101 79.0(4) . . . . ? C105 C100 C101 C102 -0.7(8) . . . . ? P1 C100 C101 C102 -174.7(4) . . . . ? C100 C101 C102 C103 -0.1(9) . . . . ? C101 C102 C103 C104 0.8(10) . . . . ? C102 C103 C104 C105 -0.6(10) . . . . ? C101 C100 C105 C104 0.8(8) . . . . ? P1 C100 C105 C104 174.6(4) . . . . ? C103 C104 C105 C100 -0.2(9) . . . . ? N1 P1 C110 C111 -142.1(4) . . . . ? C100 P1 C110 C111 111.5(4) . . . . ? Fe P1 C110 C111 -16.6(5) . . . . ? N1 P1 C110 C115 40.5(5) . . . . ? C100 P1 C110 C115 -65.9(5) . . . . ? Fe P1 C110 C115 166.0(4) . . . . ? C115 C110 C111 C112 0.9(8) . . . . ? P1 C110 C111 C112 -176.6(5) . . . . ? C110 C111 C112 C113 -1.5(10) . . . . ? C111 C112 C113 C114 0.0(10) . . . . ? C112 C113 C114 C115 2.0(10) . . . . ? C113 C114 C115 C110 -2.7(9) . . . . ? C111 C110 C115 C114 1.2(8) . . . . ? P1 C110 C115 C114 178.7(4) . . . . ? N1 P2 C200 C201 21.1(5) . . . . ? C210 P2 C200 C201 128.4(4) . . . . ? Pd P2 C200 C201 -101.8(4) . . . . ? N1 P2 C200 C205 -163.0(4) . . . . ? C210 P2 C200 C205 -55.8(5) . . . . ? Pd P2 C200 C205 74.0(4) . . . . ? C205 C200 C201 C202 0.1(9) . . . . ? P2 C200 C201 C202 176.0(5) . . . . ? C200 C201 C202 C203 0.6(11) . . . . ? C201 C202 C203 C204 -1.3(12) . . . . ? C202 C203 C204 C205 1.3(11) . . . . ? C203 C204 C205 C200 -0.6(9) . . . . ? C201 C200 C205 C204 -0.1(8) . . . . ? P2 C200 C205 C204 -176.1(4) . . . . ? N1 P2 C210 C215 85.7(4) . . . . ? C200 P2 C210 C215 -23.9(5) . . . . ? Pd P2 C210 C215 -151.3(4) . . . . ? N1 P2 C210 C211 -88.8(4) . . . . ? C200 P2 C210 C211 161.5(4) . . . . ? Pd P2 C210 C211 34.1(4) . . . . ? C215 C210 C211 C212 0.9(8) . . . . ? P2 C210 C211 C212 175.7(4) . . . . ? C210 C211 C212 C213 -0.7(9) . . . . ? C211 C212 C213 C214 -0.5(10) . . . . ? C212 C213 C214 C215 1.6(9) . . . . ? C211 C210 C215 C214 0.1(7) . . . . ? P2 C210 C215 C214 -174.4(4) . . . . ? C213 C214 C215 C210 -1.4(8) . . . . ? O1 Pd C300 C305 94.3(4) . . . . ? P2 Pd C300 C305 -88.5(4) . . . . ? Fe Pd C300 C305 116.3(12) . . . . ? Si Pd C300 C305 98.7(4) . . . . ? O1 Pd C300 C301 -75.7(5) . . . . ? P2 Pd C300 C301 101.5(4) . . . . ? Fe Pd C300 C301 -53.7(15) . . . . ? Si Pd C300 C301 -71.3(5) . . . . ? C305 C300 C301 C302 -1.3(10) . . . . ? Pd C300 C301 C302 169.3(6) . . . . ? C300 C301 C302 C303 0.0(12) . . . . ? C301 C302 C303 C304 0.4(13) . . . . ? C302 C303 C304 C305 0.5(12) . . . . ? C301 C300 C305 C304 2.2(8) . . . . ? Pd C300 C305 C304 -167.8(5) . . . . ? C303 C304 C305 C300 -1.9(10) . . . . ? C404 O400 C401 C402 -5.8(9) . . . . ? O400 C401 C402 C403 25.6(10) . . . . ? C401 C402 C403 C404 -35.1(10) . . . . ? C401 O400 C404 C403 -16.5(9) . . . . ? C402 C403 C404 O400 32.6(9) . . . . ? _refine_diff_density_max 0.462 _refine_diff_density_min -0.342 _refine_diff_density_rms 0.066 data_br88 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C90 H90 Cl3 Fe3 N3 O18 P6 Pd3 Si3' _chemical_formula_weightical 2364.84 _chemical_melting_point ? _chemical_compound_source ? 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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Si' 'Si' 0.0817 0.0704 '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' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pd' 'Pd' -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'z, x, y' 'y, z, x' '-x, -y, -z' '-z, -x, -y' '-y, -z, -x' _cell_length_a 25.113(2) _cell_length_b 25.113(2) _cell_length_c 25.113(3) _cell_angle_alpha 118.39(2) _cell_angle_beta 118.39(2) _cell_angle_gamma 118.39(2) _cell_volume 5175.8(8) _cell_formula_units_Z 2 _cell_measurement_temperature 298 _cell_measurement_reflns_used 24 _cell_measurement_theta_min 13 _cell_measurement_theta_max 18 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.517 _exptl_crystal_density_method ? _exptl_crystal_F_000 2388 _exptl_absorpt_coefficient_mu 1.187 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device ? _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14457 _diffrn_reflns_av_R_equivalents 0.0409 _diffrn_reflns_av_sigmaI/netI 0.0368 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 3.04 _diffrn_reflns_theta_max 22.50 _reflns_number_total 4503 _reflns_number_observed 2796 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-96 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-96 (Sheldrick, 1996)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0001P)^2^+27.7168P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00000(15) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 4503 _refine_ls_number_parameters 395 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1309 _refine_ls_R_factor_obs 0.0316 _refine_ls_wR_factor_all 0.1271 _refine_ls_wR_factor_obs 0.0629 _refine_ls_goodness_of_fit_all 1.389 _refine_ls_goodness_of_fit_obs 0.899 _refine_ls_restrained_S_all 1.389 _refine_ls_restrained_S_obs 0.899 _refine_ls_shift/esd_max 1.684 _refine_ls_shift/esd_mean 0.012 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Pd1 Pd 0.13672(7) 0.96811(7) 0.33765(7) 0.0386(2) Uani 1 d . . Fe1 Fe 0.18618(12) 0.90359(12) 0.35789(12) 0.0389(3) Uani 1 d . . P1 P 0.1259(2) 0.8045(2) 0.2066(2) 0.0347(5) Uani 1 d . . P2 P 0.0486(2) 0.8596(2) 0.1675(2) 0.0350(5) Uani 1 d . . Cl1 Cl 0.1063(3) 1.0458(3) 0.3427(3) 0.0547(6) Uani 1 d . . Si1 Si 0.2390(3) 1.0068(3) 0.5067(3) 0.0558(7) Uani 1 d . . O1 O -0.1108(7) 0.6371(7) 0.1265(8) 0.069(2) Uani 1 d . . O2 O 0.2922(9) 0.8936(10) 0.4592(10) 0.097(3) Uani 1 d . . O3 O 0.4396(7) 1.1862(7) 0.5615(8) 0.078(2) Uani 1 d . . O4 O 0.2267(8) 1.0656(7) 0.5055(7) 0.0673(19) Uani 1 d . . O5 O 0.3887(10) 1.1350(10) 0.6689(8) 0.106(3) Uani 1 d . . O6 O 0.1227(9) 0.9001(10) 0.4490(9) 0.105(3) Uani 1 d . . N1 N 0.0819(7) 0.8176(7) 0.1461(7) 0.0376(16) Uani 1 d . . H1 H 0.0764 0.8023 0.1032 0.08(3) Uiso 1 calc R . C1 C 0.0063(11) 0.7426(11) 0.2179(10) 0.047(2) Uani 1 d . . C2 C 0.2503(10) 0.8970(10) 0.4190(10) 0.057(3) Uani 1 d . . C3 C 0.3382(11) 1.0750(11) 0.4811(10) 0.051(2) Uani 1 d . . C4 C 0.2550(9) 0.8731(9) 0.2655(9) 0.040(2) Uani 1 d . . C5 C 0.2122(10) 0.8055(10) 0.1663(10) 0.048(2) Uani 1 d . . H5 H 0.1199 0.7273 0.0722 0.078(7) Uiso 1 calc R . C6 C 0.3083(11) 0.8555(11) 0.2088(11) 0.056(2) Uani 1 d . . H6 H 0.2800 0.8104 0.1428 0.078(7) Uiso 1 calc R . C7 C 0.4452(11) 0.9715(11) 0.3484(12) 0.061(3) Uani 1 d . . H7 H 0.5099 1.0060 0.3771 0.078(7) Uiso 1 calc R . C8 C 0.4863(11) 1.0367(11) 0.4459(12) 0.064(3) Uani 1 d . . H8 H 0.5781 1.1138 0.5396 0.078(7) Uiso 1 calc R . C9 C 0.3910(9) 0.9872(9) 0.4040(10) 0.050(2) Uani 1 d . . H9 H 0.4190 1.0313 0.4698 0.078(7) Uiso 1 calc R . C10 C -0.0263(9) 0.6153(8) 0.0488(8) 0.039(2) Uani 1 d . . C11 C -0.0117(13) 0.5770(11) 0.0660(11) 0.121(6) Uani 1 d . . H11 H 0.0761 0.6473 0.1567 0.078(7) Uiso 1 calc R . C12 C -0.1260(15) 0.4347(13) -0.0497(13) 0.136(7) Uani 1 d . . H12 H -0.1140 0.4110 -0.0345 0.078(7) Uiso 1 calc R . C13 C -0.2548(12) 0.3281(11) -0.1844(12) 0.081(4) Uani 1 d . . H13 H -0.3315 0.2322 -0.2621 0.078(7) Uiso 1 calc R . C14 C -0.2660(10) 0.3692(10) -0.1999(11) 0.076(3) Uani 1 d . . H14 H -0.3525 0.2990 -0.2913 0.078(7) Uiso 1 calc R . C15 C -0.1543(9) 0.5103(9) -0.0858(10) 0.064(3) Uani 1 d . . H15 H -0.1665 0.5340 -0.1007 0.078(7) Uiso 1 calc R . C16 C 0.1251(9) 0.9718(9) 0.2031(9) 0.045(2) Uani 1 d . . C17 C 0.0639(10) 0.9708(10) 0.1564(11) 0.056(2) Uani 1 d . . H17 H -0.0239 0.9037 0.0962 0.078(7) Uiso 1 calc R . C18 C 0.1355(13) 1.0710(12) 0.2005(12) 0.075(3) Uani 1 d . . H18 H 0.0960 1.0717 0.1709 0.078(7) Uiso 1 calc R . C19 C 0.2625(13) 1.1674(12) 0.2867(13) 0.080(3) Uani 1 d . . H19 H 0.3087 1.2330 0.3145 0.078(7) Uiso 1 calc R . C20 C 0.3249(12) 1.1708(12) 0.3339(12) 0.072(3) Uani 1 d . . H20 H 0.4126 1.2383 0.3935 0.078(7) Uiso 1 calc R . C21 C 0.2564(10) 1.0732(10) 0.2921(10) 0.054(2) Uani 1 d . . H21 H 0.2982 1.0749 0.3237 0.078(7) Uiso 1 calc R . C22 C -0.1430(9) 0.6962(9) -0.0057(9) 0.040(2) Uani 1 d . . C23 C -0.2207(10) 0.6459(10) -0.0239(11) 0.063(3) Uani 1 d . . H23 H -0.1728 0.7000 0.0557 0.078(7) Uiso 1 calc R . C24 C -0.3668(11) 0.5183(12) -0.1557(13) 0.080(3) Uani 1 d . . H24 H -0.4164 0.4890 -0.1643 0.078(7) Uiso 1 calc R . C25 C -0.4393(12) 0.4344(12) -0.2742(13) 0.085(4) Uani 1 d . . H25 H -0.5389 0.3453 -0.3644 0.078(7) Uiso 1 calc R . C26 C -0.3662(12) 0.4807(12) -0.2612(11) 0.079(4) Uani 1 d . . H26 H -0.4158 0.4239 -0.3422 0.078(7) Uiso 1 calc R . C27 C -0.2175(10) 0.6130(10) -0.1265(10) 0.064(3) Uani 1 d . . H27 H -0.1674 0.6462 -0.1170 0.078(7) Uiso 1 calc R . C28 C 0.2571(13) 1.1484(12) 0.5874(12) 0.084(4) Uani 1 d . . H28A H 0.3337 1.2111 0.6784 0.20(3) Uiso 1 calc R . H28B H 0.1731 1.0852 0.5362 0.20(3) Uiso 1 calc R . H28C H 0.2850 1.2043 0.6022 0.20(3) Uiso 1 calc R . C29 C 0.5245(16) 1.2511(18) 0.7732(16) 0.169(8) Uani 1 d . . H29A H 0.5444 1.2962 0.7751 0.20(3) Uiso 1 calc R . H29B H 0.5395 1.2238 0.7559 0.20(3) Uiso 1 calc R . H29C H 0.5873 1.3170 0.8636 0.20(3) Uiso 1 calc R . C30 C 0.121(2) 0.869(2) 0.479(2) 0.195(9) Uani 1 d . . H30A H 0.0687 0.7849 0.4107 0.20(3) Uiso 1 calc R . H30B H 0.0749 0.8525 0.4761 0.20(3) Uiso 1 calc R . H30C H 0.2172 0.9481 0.5737 0.20(3) Uiso 1 calc R . 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 Pd1 0.0454(4) 0.0429(4) 0.0413(4) 0.0382(4) 0.0399(4) 0.0413(4) Fe1 0.0394(7) 0.0405(7) 0.0381(7) 0.0356(7) 0.0349(7) 0.0367(7) P1 0.0343(12) 0.0334(12) 0.0333(12) 0.0297(11) 0.0302(11) 0.0312(11) P2 0.0397(12) 0.0407(12) 0.0391(12) 0.0365(12) 0.0362(12) 0.0377(12) Cl1 0.0711(15) 0.0673(15) 0.0763(16) 0.0666(15) 0.0691(15) 0.0662(14) Si1 0.0611(17) 0.0656(17) 0.0515(16) 0.0533(16) 0.0517(16) 0.0580(16) O1 0.051(4) 0.056(4) 0.072(5) 0.056(4) 0.055(4) 0.048(4) O2 0.118(6) 0.147(7) 0.133(7) 0.134(7) 0.115(6) 0.127(7) O3 0.049(4) 0.051(4) 0.074(5) 0.053(4) 0.052(4) 0.044(4) O4 0.096(5) 0.089(5) 0.067(4) 0.073(4) 0.077(4) 0.087(5) O5 0.089(6) 0.117(7) 0.057(5) 0.073(6) 0.064(5) 0.093(6) O6 0.113(7) 0.116(7) 0.111(7) 0.106(6) 0.106(6) 0.101(6) N1 0.043(4) 0.043(4) 0.039(4) 0.037(4) 0.037(4) 0.040(4) C1 0.060(6) 0.060(6) 0.061(6) 0.056(6) 0.057(6) 0.057(6) C2 0.050(6) 0.056(6) 0.056(6) 0.050(6) 0.047(6) 0.048(6) C3 0.057(6) 0.059(6) 0.057(6) 0.053(6) 0.053(6) 0.054(6) C4 0.039(5) 0.038(5) 0.043(5) 0.037(5) 0.036(5) 0.036(5) C5 0.055(5) 0.061(6) 0.051(5) 0.052(5) 0.049(5) 0.056(5) C6 0.078(7) 0.083(7) 0.080(7) 0.077(7) 0.076(7) 0.077(7) C7 0.059(6) 0.066(7) 0.081(7) 0.067(7) 0.065(7) 0.058(6) C8 0.055(6) 0.070(7) 0.068(7) 0.063(7) 0.056(6) 0.057(6) C9 0.047(6) 0.049(6) 0.051(6) 0.043(5) 0.045(5) 0.044(5) C10 0.040(5) 0.036(5) 0.035(5) 0.032(5) 0.034(5) 0.035(5) C11 0.086(9) 0.042(7) 0.036(6) 0.032(6) 0.035(7) 0.053(7) C12 0.108(11) 0.059(8) 0.061(9) 0.052(8) 0.057(9) 0.071(9) C13 0.072(8) 0.036(6) 0.048(7) 0.034(6) 0.049(7) 0.044(7) C14 0.034(6) 0.036(6) 0.042(6) 0.030(6) 0.028(6) 0.027(6) C15 0.039(6) 0.038(6) 0.046(6) 0.035(6) 0.032(6) 0.033(5) C16 0.056(6) 0.050(5) 0.047(5) 0.044(5) 0.048(5) 0.049(5) C17 0.067(6) 0.073(6) 0.080(7) 0.072(6) 0.068(6) 0.066(6) C18 0.095(9) 0.083(8) 0.092(8) 0.083(8) 0.084(8) 0.084(8) C19 0.083(8) 0.068(7) 0.095(9) 0.076(8) 0.081(8) 0.067(8) C20 0.063(7) 0.066(7) 0.068(7) 0.060(7) 0.060(7) 0.057(7) C21 0.054(6) 0.054(6) 0.058(6) 0.051(6) 0.051(6) 0.049(6) C22 0.041(5) 0.043(5) 0.039(5) 0.037(5) 0.035(5) 0.040(5) C23 0.048(6) 0.060(6) 0.061(7) 0.054(6) 0.050(6) 0.046(6) C24 0.040(6) 0.054(7) 0.065(8) 0.051(7) 0.044(7) 0.037(6) C25 0.044(7) 0.041(7) 0.056(8) 0.038(7) 0.036(7) 0.037(6) C26 0.065(8) 0.066(7) 0.041(6) 0.043(7) 0.044(7) 0.060(7) C27 0.048(6) 0.058(6) 0.044(6) 0.042(6) 0.040(6) 0.048(6) C28 0.109(9) 0.096(8) 0.082(8) 0.079(8) 0.090(8) 0.096(8) C29 0.084(12) 0.152(16) 0.081(11) 0.094(13) 0.069(11) 0.098(13) C30 0.23(2) 0.23(2) 0.26(2) 0.23(2) 0.23(2) 0.21(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 Pd1 O4 2.178(7) . ? Pd1 P2 2.188(4) . ? Pd1 Cl1 2.385(2) . ? Pd1 C3 2.518(11) . ? Pd1 Fe1 2.5540(13) . ? Pd1 Si1 2.985(3) . ? Fe1 C1 1.768(13) . ? Fe1 C2 1.767(10) . ? Fe1 C3 1.775(13) . ? Fe1 P1 2.209(4) . ? Fe1 Si1 2.291(4) . ? P1 N1 1.691(7) . ? P1 C10 1.820(12) . ? P1 C4 1.836(9) . ? P2 N1 1.680(6) . ? P2 C22 1.806(13) . ? P2 C16 1.805(9) . ? Si1 O5 1.595(11) . ? Si1 O6 1.627(9) . ? Si1 O4 1.658(7) . ? O1 C1 1.151(12) . ? O2 C2 1.134(10) . ? O3 C3 1.160(12) . ? O4 C28 1.436(11) . ? O5 C29 1.333(19) . ? O6 C30 1.322(16) . ? N1 H1 0.8600 . ? C4 C9 1.376(14) . ? C4 C5 1.393(11) . ? C5 C6 1.389(12) . ? C5 H5 0.9300 . ? C6 C7 1.378(15) . ? C6 H6 0.9300 . ? C7 C8 1.387(13) . ? C7 H7 0.9300 . ? C8 C9 1.382(12) . ? C8 H8 0.930(5) . ? C9 H9 0.9300 . ? C10 C11 1.350(12) . ? C10 C15 1.357(13) . ? C11 C12 1.377(16) . ? C11 H11 0.9300 . ? C12 C13 1.351(17) . ? C12 H12 0.9300 . ? C13 C14 1.357(14) . ? C13 H13 0.9300 . ? C14 C15 1.373(14) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C16 C17 1.400(11) . ? C16 C21 1.394(13) . ? C17 C18 1.393(13) . ? C17 H17 0.9300 . ? C18 C19 1.353(15) . ? C18 H18 0.9300 . ? C19 C20 1.370(15) . ? C19 H19 0.9300 . ? C20 C21 1.376(13) . ? C20 H20 0.930(3) . ? C21 H21 0.9300 . ? C22 C23 1.365(12) . ? C22 C27 1.388(12) . ? C23 C24 1.368(15) . ? C23 H23 0.9300 . ? C24 C25 1.359(16) . ? C24 H24 0.9300 . ? C25 C26 1.366(16) . ? C25 H25 0.930(5) . ? C26 C27 1.388(15) . ? C26 H26 0.9300 . ? C27 H27 0.9300 . ? C28 H28A 0.960(8) . ? C28 H28B 0.960(4) . ? C28 H28C 0.960(9) . ? C29 H29A 0.960(5) . ? C29 H29B 0.9600(11) . ? C29 H29C 0.960(5) . ? C30 H30A 0.960(5) . ? C30 H30B 0.960(5) . ? C30 H30C 0.960(7) . ? 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 O4 Pd1 P2 172.47(18) . . ? O4 Pd1 Cl1 93.13(18) . . ? P2 Pd1 Cl1 94.39(8) . . ? O4 Pd1 C3 81.3(3) . . ? P2 Pd1 C3 93.5(3) . . ? Cl1 Pd1 C3 137.0(3) . . ? O4 Pd1 Fe1 80.71(17) . . ? P2 Pd1 Fe1 91.78(6) . . ? Cl1 Pd1 Fe1 173.70(8) . . ? C3 Pd1 Fe1 41.0(3) . . ? O4 Pd1 Si1 33.01(18) . . ? P2 Pd1 Si1 139.47(8) . . ? Cl1 Pd1 Si1 125.89(10) . . ? C3 Pd1 Si1 61.5(2) . . ? Fe1 Pd1 Si1 48.09(7) . . ? C1 Fe1 C2 101.1(4) . . ? C1 Fe1 C3 152.0(4) . . ? C2 Fe1 C3 106.0(5) . . ? C1 Fe1 P1 92.3(4) . . ? C2 Fe1 P1 97.9(3) . . ? C3 Fe1 P1 91.0(4) . . ? C1 Fe1 Si1 86.2(4) . . ? C2 Fe1 Si1 88.0(3) . . ? C3 Fe1 Si1 87.6(4) . . ? P1 Fe1 Si1 174.00(10) . . ? C1 Fe1 Pd1 83.6(3) . . ? C2 Fe1 Pd1 163.0(3) . . ? C3 Fe1 Pd1 68.4(3) . . ? P1 Fe1 Pd1 98.22(7) . . ? Si1 Fe1 Pd1 75.84(8) . . ? N1 P1 C10 106.5(4) . . ? N1 P1 C4 103.7(3) . . ? C10 P1 C4 100.3(4) . . ? N1 P1 Fe1 109.7(2) . . ? C10 P1 Fe1 114.9(3) . . ? C4 P1 Fe1 120.3(4) . . ? N1 P2 C22 106.7(4) . . ? N1 P2 C16 103.3(4) . . ? C22 P2 C16 106.2(4) . . ? N1 P2 Pd1 115.6(3) . . ? C22 P2 Pd1 112.9(4) . . ? C16 P2 Pd1 111.3(4) . . ? O5 Si1 O6 103.3(6) . . ? O5 Si1 O4 108.9(5) . . ? O6 Si1 O4 103.4(5) . . ? O5 Si1 Fe1 121.3(4) . . ? O6 Si1 Fe1 117.2(5) . . ? O4 Si1 Fe1 101.2(2) . . ? O5 Si1 Pd1 136.6(4) . . ? O6 Si1 Pd1 115.6(4) . . ? O4 Si1 Pd1 45.7(2) . . ? Fe1 Si1 Pd1 56.06(8) . . ? C28 O4 Si1 127.3(6) . . ? C28 O4 Pd1 131.1(6) . . ? Si1 O4 Pd1 101.3(3) . . ? C29 O5 Si1 134.9(11) . . ? C30 O6 Si1 131.9(12) . . ? P2 N1 P1 121.8(4) . . ? P2 N1 H1 119.1(2) . . ? P1 N1 H1 119.1(2) . . ? O1 C1 Fe1 179.2(13) . . ? O2 C2 Fe1 179.5(10) . . ? O3 C3 Fe1 176.8(8) . . ? O3 C3 Pd1 112.3(7) . . ? Fe1 C3 Pd1 70.6(4) . . ? C9 C4 C5 119.9(8) . . ? C9 C4 P1 121.3(7) . . ? C5 C4 P1 118.8(7) . . ? C4 C5 C6 119.6(9) . . ? C4 C5 H5 120.2(5) . . ? C6 C5 H5 120.2(6) . . ? C7 C6 C5 120.3(9) . . ? C7 C6 H6 119.9(6) . . ? C5 C6 H6 119.9(6) . . ? C6 C7 C8 119.8(9) . . ? C6 C7 H7 120.1(6) . . ? C8 C7 H7 120.1(6) . . ? C9 C8 C7 120.1(10) . . ? C9 C8 H8 119.9(6) . . ? C7 C8 H8 119.9(6) . . ? C4 C9 C8 120.3(9) . . ? C4 C9 H9 119.8(5) . . ? C8 C9 H9 119.8(6) . . ? C11 C10 C15 118.2(9) . . ? C11 C10 P1 118.6(7) . . ? C15 C10 P1 123.2(7) . . ? C10 C11 C12 120.5(11) . . ? C10 C11 H11 119.8(6) . . ? C12 C11 H11 119.8(8) . . ? C13 C12 C11 122.4(12) . . ? C13 C12 H12 118.8(7) . . ? C11 C12 H12 118.8(7) . . ? C14 C13 C12 116.1(10) . . ? C14 C13 H13 121.9(7) . . ? C12 C13 H13 121.9(7) . . ? C15 C14 C13 122.5(10) . . ? C15 C14 H14 118.8(7) . . ? C13 C14 H14 118.8(7) . . ? C10 C15 C14 120.2(10) . . ? C10 C15 H15 119.9(5) . . ? C14 C15 H15 119.9(7) . . ? C17 C16 C21 118.6(8) . . ? C17 C16 P2 121.5(7) . . ? C21 C16 P2 119.5(7) . . ? C16 C17 C18 119.6(9) . . ? C16 C17 H17 120.2(5) . . ? C18 C17 H17 120.2(6) . . ? C19 C18 C17 120.0(10) . . ? C19 C18 H18 120.0(7) . . ? C17 C18 H18 120.0(6) . . ? C18 C19 C20 121.7(10) . . ? C18 C19 H19 119.1(7) . . ? C20 C19 H19 119.1(7) . . ? C19 C20 C21 119.3(11) . . ? C19 C20 H20 120.4(7) . . ? C21 C20 H20 120.4(6) . . ? C20 C21 C16 120.8(9) . . ? C20 C21 H21 119.6(6) . . ? C16 C21 H21 119.6(5) . . ? C23 C22 C27 117.7(9) . . ? C23 C22 P2 121.3(7) . . ? C27 C22 P2 120.9(7) . . ? C22 C23 C24 122.0(10) . . ? C22 C23 H23 119.0(6) . . ? C24 C23 H23 119.0(7) . . ? C25 C24 C23 119.9(11) . . ? C25 C24 H24 120.1(8) . . ? C23 C24 H24 120.1(7) . . ? C24 C25 C26 120.2(11) . . ? C24 C25 H25 119.9(8) . . ? C26 C25 H25 119.9(7) . . ? C25 C26 C27 119.6(10) . . ? C25 C26 H26 120.2(8) . . ? C27 C26 H26 120.2(7) . . ? C22 C27 C26 120.5(10) . . ? C22 C27 H27 119.8(6) . . ? C26 C27 H27 119.8(7) . . ? O4 C28 H28A 109.5(6) . . ? O4 C28 H28B 109.5(7) . . ? H28A C28 H28B 109.5(6) . . ? O4 C28 H28C 109.5(6) . . ? H28A C28 H28C 109.5(9) . . ? H28B C28 H28C 109.5(5) . . ? O5 C29 H29A 109.4(11) . . ? O5 C29 H29B 109.5(10) . . ? H29A C29 H29B 109.47(18) . . ? O5 C29 H29C 109.5(9) . . ? H29A C29 H29C 109.5(4) . . ? H29B C29 H29C 109.5(5) . . ? O6 C30 H30A 109.5(10) . . ? O6 C30 H30B 109.5(10) . . ? H30A C30 H30B 109.4(8) . . ? O6 C30 H30C 109.5(9) . . ? H30A C30 H30C 109.4(5) . . ? H30B C30 H30C 109.4(5) . . ? _refine_diff_density_max 1.020 _refine_diff_density_min -0.864 _refine_diff_density_rms 0.169