Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Petr Stepnicka' _publ_contact_author_address ; Department of Inorganic Chemistry Charles University in Prague, Faculty of Science Hlavova 2030 Prague 12840 CZECH REPUBLIC ; _publ_contact_author_email STEPNIC@NATUR.CUNI.CZ _publ_section_title ; Synthesis, coordination and catalytic use of 1-(diphenylphosphino)-1'-carbamoylferrocenes with pyridyl-containing N-substituents ; loop_ _publ_author_name P.Stepnicka J.Demel M.Dusek J.Kuhnert H.Lang data_jk6 _database_code_depnum_ccdc_archive 'CCDC 633466' _audit_creation_method SHELXL-97 _chemical_name_systematic ; N-{(pyrid-2yl)methyl} 1'-(diphenylphosphino)ferrocenecarboxamide ; _chemical_formula_moiety 'C29 H25 Fe N2 O P' _chemical_formula_sum 'C29 H25 Fe N2 O P' _chemical_formula_weight 504.33 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' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.217(4) _cell_length_b 11.453(2) _cell_length_c 13.079(4) _cell_angle_alpha 81.11(2) _cell_angle_beta 73.58(4) _cell_angle_gamma 80.57(3) _cell_volume 1157.1(7) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 8814 _cell_measurement_theta_min 2.57 _cell_measurement_theta_max 26.50 _exptl_crystal_description orange _exptl_crystal_colour plate _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.03 _exptl_crystal_density_diffrn 1.448 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 524 _exptl_absorpt_coefficient_mu 0.747 _exptl_absorpt_correction_type none _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford KM4 CCD diffractometer' _diffrn_measurement_method '\w and \p scans to fill the Ewald sphere' _diffrn_detector_area_resol_mean 8.3438 _diffrn_standards_number 0 _diffrn_reflns_number 15853 _diffrn_reflns_av_R_equivalents 0.0428 _diffrn_reflns_av_sigmaI/netI 0.0487 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.61 _diffrn_reflns_theta_max 26.65 _reflns_number_total 4825 _reflns_number_gt 3607 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.29.5 (release 22-02-2006 CrysAlis171 .NET) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.29.5 (release 22-02-2006 CrysAlis171 .NET) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.29.5 (release 22-02-2006 CrysAlis171 .NET) ; _computing_structure_solution 'SIR-97 (Altomare et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness 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 threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) 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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0396P)^2^+0.0000P] 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 none _refine_ls_number_reflns 4825 _refine_ls_number_parameters 311 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0424 _refine_ls_R_factor_gt 0.0291 _refine_ls_wR_factor_ref 0.0724 _refine_ls_wR_factor_gt 0.0705 _refine_ls_goodness_of_fit_ref 0.991 _refine_ls_restrained_S_all 0.991 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_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_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe Fe 0.43253(3) 0.19524(2) 0.724221(19) 0.02033(9) Uani 1 1 d . . . P P 0.39633(6) 0.22072(4) 0.46631(3) 0.01987(11) Uani 1 1 d . . . O O 0.38954(16) 0.19395(11) 1.01492(10) 0.0312(3) Uani 1 1 d . . . N1 N 0.23719(19) 0.05102(13) 1.00521(12) 0.0242(3) Uani 1 1 d . . . N2 N -0.14978(19) 0.16501(13) 1.06319(11) 0.0264(3) Uani 1 1 d . . . H1N H 0.227(2) -0.0015(16) 0.9724(15) 0.031(6) Uiso 1 1 d . . . C1 C 0.3420(2) 0.27386(14) 0.59665(13) 0.0206(4) Uani 1 1 d . . . C2 C 0.4178(2) 0.35586(14) 0.63453(14) 0.0257(4) Uani 1 1 d . . . H2 H 0.5097 0.3954 0.5944 0.031 Uiso 1 1 calc R . . C3 C 0.3308(3) 0.36735(16) 0.74312(15) 0.0323(5) Uani 1 1 d . . . H3 H 0.3554 0.4154 0.7865 0.039 Uiso 1 1 calc R . . C4 C 0.2001(2) 0.29326(16) 0.77410(15) 0.0326(5) Uani 1 1 d . . . H4 H 0.1233 0.2840 0.8415 0.039 Uiso 1 1 calc R . . C5 C 0.2063(2) 0.23493(16) 0.68394(14) 0.0265(4) Uani 1 1 d . . . H5 H 0.1343 0.1809 0.6824 0.032 Uiso 1 1 calc R . . C6 C 0.4787(2) 0.09666(14) 0.85790(13) 0.0209(4) Uani 1 1 d . . . C7 C 0.4644(2) 0.02010(14) 0.78566(13) 0.0223(4) Uani 1 1 d . . . H7 H 0.3851 -0.0336 0.7997 0.027 Uiso 1 1 calc R . . C8 C 0.5919(2) 0.04015(14) 0.68895(13) 0.0248(4) Uani 1 1 d . . . H8 H 0.6113 0.0016 0.6282 0.030 Uiso 1 1 calc R . . C9 C 0.6849(2) 0.12851(15) 0.69995(14) 0.0268(4) Uani 1 1 d . . . H9 H 0.7756 0.1585 0.6476 0.032 Uiso 1 1 calc R . . C10 C 0.6165(2) 0.16355(15) 0.80418(14) 0.0246(4) Uani 1 1 d . . . H10 H 0.6547 0.2202 0.8327 0.030 Uiso 1 1 calc R . . C11 C 0.3660(2) 0.11784(15) 0.96542(14) 0.0237(4) Uani 1 1 d . . . C12 C 0.3306(2) 0.35296(14) 0.38159(13) 0.0206(4) Uani 1 1 d . . . C13 C 0.2322(2) 0.45515(15) 0.42093(14) 0.0245(4) Uani 1 1 d . . . H13 H 0.2048 0.4620 0.4939 0.029 Uiso 1 1 calc R . . C14 C 0.1745(2) 0.54700(15) 0.35226(16) 0.0318(5) Uani 1 1 d . . . H14 H 0.1093 0.6153 0.3793 0.038 Uiso 1 1 calc R . . C15 C 0.2134(2) 0.53728(17) 0.24418(16) 0.0347(5) Uani 1 1 d . . . H15 H 0.1743 0.5988 0.1982 0.042 Uiso 1 1 calc R . . C16 C 0.3106(2) 0.43601(17) 0.20413(15) 0.0338(5) Uani 1 1 d . . . H16 H 0.3377 0.4294 0.1311 0.041 Uiso 1 1 calc R . . C17 C 0.3676(2) 0.34460(17) 0.27261(14) 0.0300(4) Uani 1 1 d . . . H17 H 0.4319 0.2762 0.2452 0.036 Uiso 1 1 calc R . . C18 C 0.6295(2) 0.21332(14) 0.42384(12) 0.0193(4) Uani 1 1 d . . . C19 C 0.7187(2) 0.31177(15) 0.40270(14) 0.0257(4) Uani 1 1 d . . . H19 H 0.6590 0.3881 0.4031 0.031 Uiso 1 1 calc R . . C20 C 0.8943(2) 0.29693(16) 0.38120(15) 0.0310(4) Uani 1 1 d . . . H20 H 0.9524 0.3631 0.3680 0.037 Uiso 1 1 calc R . . C21 C 0.9846(2) 0.18364(17) 0.37914(14) 0.0309(4) Uani 1 1 d . . . H21 H 1.1029 0.1738 0.3667 0.037 Uiso 1 1 calc R . . C22 C 0.8996(2) 0.08606(16) 0.39548(14) 0.0282(4) Uani 1 1 d . . . H22 H 0.9605 0.0102 0.3920 0.034 Uiso 1 1 calc R . . C23 C 0.7228(2) 0.10073(14) 0.41718(13) 0.0222(4) Uani 1 1 d . . . H23 H 0.6658 0.0343 0.4274 0.027 Uiso 1 1 calc R . . C24 C 0.1127(2) 0.07133(15) 1.10672(14) 0.0292(4) Uani 1 1 d . . . H24A H 0.1717 0.0813 1.1588 0.035 Uiso 1 1 calc R . . H24B H 0.0520 0.0024 1.1335 0.035 Uiso 1 1 calc R . . C25 C -0.0137(2) 0.18030(15) 1.09447(13) 0.0227(4) Uani 1 1 d . . . C26 C -0.2599(2) 0.26187(17) 1.04754(14) 0.0315(4) Uani 1 1 d . . . H26 H -0.3545 0.2526 1.0253 0.038 Uiso 1 1 calc R . . C27 C -0.2396(2) 0.37483(16) 1.06280(14) 0.0319(5) Uani 1 1 d . . . H27 H -0.3188 0.4400 1.0512 0.038 Uiso 1 1 calc R . . C28 C -0.1004(3) 0.38822(17) 1.09532(16) 0.0363(5) Uani 1 1 d . . . H28 H -0.0834 0.4630 1.1065 0.044 Uiso 1 1 calc R . . C29 C 0.0137(2) 0.29031(16) 1.11130(15) 0.0308(4) Uani 1 1 d . . . H29 H 0.1091 0.2981 1.1334 0.037 Uiso 1 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 Fe 0.01967(14) 0.01874(14) 0.02195(14) -0.00151(10) -0.00784(10) 0.00273(10) P 0.0187(2) 0.0178(2) 0.0235(2) 0.00030(17) -0.00781(19) -0.00215(18) O 0.0315(7) 0.0369(7) 0.0310(7) -0.0121(6) -0.0126(6) -0.0051(6) N1 0.0266(9) 0.0230(8) 0.0225(8) -0.0043(7) -0.0058(7) -0.0013(7) N2 0.0248(8) 0.0291(8) 0.0256(8) -0.0048(6) -0.0056(7) -0.0043(7) C1 0.0193(9) 0.0178(8) 0.0236(9) 0.0009(7) -0.0091(7) 0.0039(7) C2 0.0319(10) 0.0157(8) 0.0302(10) 0.0000(7) -0.0140(8) 0.0029(8) C3 0.0406(12) 0.0246(10) 0.0326(11) -0.0091(8) -0.0172(9) 0.0122(9) C4 0.0274(10) 0.0389(11) 0.0247(10) -0.0041(8) -0.0064(8) 0.0149(9) C5 0.0182(9) 0.0308(10) 0.0287(10) 0.0021(8) -0.0099(8) 0.0029(8) C6 0.0211(9) 0.0201(9) 0.0225(9) 0.0012(7) -0.0117(8) 0.0017(7) C7 0.0244(9) 0.0184(8) 0.0236(10) -0.0009(7) -0.0083(8) 0.0005(7) C8 0.0278(10) 0.0215(9) 0.0226(10) -0.0027(7) -0.0076(8) 0.0060(8) C9 0.0181(9) 0.0283(10) 0.0293(10) 0.0012(8) -0.0050(8) 0.0040(8) C10 0.0208(9) 0.0241(9) 0.0312(10) -0.0033(7) -0.0131(8) 0.0023(8) C11 0.0233(10) 0.0240(9) 0.0253(10) -0.0009(7) -0.0141(8) 0.0047(8) C12 0.0165(9) 0.0213(9) 0.0258(10) 0.0025(7) -0.0104(7) -0.0040(7) C13 0.0238(10) 0.0234(9) 0.0292(10) -0.0009(7) -0.0122(8) -0.0038(8) C14 0.0263(10) 0.0216(9) 0.0508(13) 0.0018(8) -0.0187(9) -0.0025(8) C15 0.0290(11) 0.0333(11) 0.0440(13) 0.0161(9) -0.0198(10) -0.0110(9) C16 0.0297(11) 0.0461(12) 0.0260(10) 0.0073(9) -0.0114(9) -0.0097(10) C17 0.0247(10) 0.0346(10) 0.0287(11) 0.0003(8) -0.0073(8) -0.0018(8) C18 0.0192(9) 0.0205(9) 0.0179(9) -0.0002(7) -0.0063(7) -0.0007(7) C19 0.0240(10) 0.0200(9) 0.0319(10) -0.0020(7) -0.0065(8) -0.0021(8) C20 0.0263(10) 0.0301(10) 0.0375(11) -0.0042(8) -0.0053(9) -0.0118(9) C21 0.0175(9) 0.0433(12) 0.0315(11) -0.0061(8) -0.0065(8) -0.0010(9) C22 0.0239(10) 0.0275(10) 0.0308(11) -0.0046(8) -0.0077(8) 0.0053(8) C23 0.0250(10) 0.0197(9) 0.0216(9) -0.0010(7) -0.0061(8) -0.0036(8) C24 0.0306(11) 0.0308(10) 0.0237(10) -0.0001(8) -0.0065(8) -0.0011(9) C25 0.0228(9) 0.0278(9) 0.0159(9) -0.0023(7) -0.0028(7) -0.0028(8) C26 0.0248(10) 0.0447(12) 0.0266(10) -0.0054(8) -0.0096(8) -0.0027(9) C27 0.0300(11) 0.0274(10) 0.0323(11) 0.0016(8) -0.0063(9) 0.0052(9) C28 0.0353(12) 0.0268(10) 0.0429(12) -0.0107(9) 0.0004(10) -0.0052(9) C29 0.0254(10) 0.0356(11) 0.0338(11) -0.0137(8) -0.0072(8) -0.0032(9) _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 Fe C6 2.0247(17) . ? Fe C10 2.0269(19) . ? Fe C2 2.0285(17) . ? Fe C3 2.0346(18) . ? Fe C5 2.035(2) . ? Fe C4 2.038(2) . ? Fe C1 2.0411(17) . ? Fe C9 2.042(2) . ? Fe C7 2.0461(17) . ? Fe C8 2.0571(18) . ? P C1 1.8102(18) . ? P C18 1.8296(19) . ? P C12 1.8344(17) . ? O C11 1.232(2) . ? N1 C11 1.344(2) . ? N1 C24 1.454(2) . ? N1 H1N 0.819(18) . ? N2 C25 1.339(2) . ? N2 C26 1.340(2) . ? C1 C2 1.423(2) . ? C1 C5 1.425(2) . ? C2 C3 1.414(3) . ? C2 H2 0.9300 . ? C3 C4 1.408(3) . ? C3 H3 0.9300 . ? C4 C5 1.427(3) . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? C6 C7 1.424(2) . ? C6 C10 1.425(2) . ? C6 C11 1.480(2) . ? C7 C8 1.411(2) . ? C7 H7 0.9300 . ? C8 C9 1.411(2) . ? C8 H8 0.9300 . ? C9 C10 1.413(2) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? C12 C17 1.386(2) . ? C12 C13 1.389(2) . ? C13 C14 1.387(2) . ? C13 H13 0.9300 . ? C14 C15 1.376(3) . ? C14 H14 0.9300 . ? C15 C16 1.380(3) . ? C15 H15 0.9300 . ? C16 C17 1.380(2) . ? C16 H16 0.9300 . ? C17 H17 0.9300 . ? C18 C23 1.389(2) . ? C18 C19 1.394(2) . ? C19 C20 1.377(3) . ? C19 H19 0.9300 . ? C20 C21 1.385(3) . ? C20 H20 0.9300 . ? C21 C22 1.371(3) . ? C21 H21 0.9300 . ? C22 C23 1.386(3) . ? C22 H22 0.9300 . ? C23 H23 0.9300 . ? C24 C25 1.506(2) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 C29 1.376(2) . ? C26 C27 1.382(3) . ? C26 H26 0.9300 . ? C27 C28 1.366(3) . ? C27 H27 0.9300 . ? C28 C29 1.369(3) . ? C28 H28 0.9300 . ? C29 H29 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C6 Fe C10 41.20(7) . . ? C6 Fe C2 149.00(7) . . ? C10 Fe C2 115.78(8) . . ? C6 Fe C3 114.84(7) . . ? C10 Fe C3 104.32(8) . . ? C2 Fe C3 40.72(7) . . ? C6 Fe C5 127.83(8) . . ? C10 Fe C5 164.49(7) . . ? C2 Fe C5 68.52(8) . . ? C3 Fe C5 68.62(8) . . ? C6 Fe C4 105.64(8) . . ? C10 Fe C4 124.88(8) . . ? C2 Fe C4 68.34(8) . . ? C3 Fe C4 40.46(8) . . ? C5 Fe C4 41.03(7) . . ? C6 Fe C1 167.47(6) . . ? C10 Fe C1 151.14(7) . . ? C2 Fe C1 40.94(7) . . ? C3 Fe C1 68.98(7) . . ? C5 Fe C1 40.93(7) . . ? C4 Fe C1 69.02(8) . . ? C6 Fe C9 68.69(8) . . ? C10 Fe C9 40.65(7) . . ? C2 Fe C9 107.89(8) . . ? C3 Fe C9 126.15(8) . . ? C5 Fe C9 154.47(7) . . ? C4 Fe C9 163.20(8) . . ? C1 Fe C9 119.63(8) . . ? C6 Fe C7 40.95(7) . . ? C10 Fe C7 68.74(7) . . ? C2 Fe C7 168.53(7) . . ? C3 Fe C7 150.37(7) . . ? C5 Fe C7 110.13(8) . . ? C4 Fe C7 118.67(8) . . ? C1 Fe C7 130.68(7) . . ? C9 Fe C7 68.11(8) . . ? C6 Fe C8 68.29(7) . . ? C10 Fe C8 68.14(7) . . ? C2 Fe C8 130.00(7) . . ? C3 Fe C8 165.49(8) . . ? C5 Fe C8 121.70(8) . . ? C4 Fe C8 153.99(8) . . ? C1 Fe C8 111.23(7) . . ? C9 Fe C8 40.26(7) . . ? C7 Fe C8 40.21(7) . . ? C1 P C18 102.87(9) . . ? C1 P C12 102.46(8) . . ? C18 P C12 101.97(8) . . ? C11 N1 C24 120.68(16) . . ? C11 N1 H1N 120.7(14) . . ? C24 N1 H1N 118.6(14) . . ? C25 N2 C26 117.49(15) . . ? C2 C1 C5 106.86(16) . . ? C2 C1 P 130.20(13) . . ? C5 C1 P 122.94(14) . . ? C2 C1 Fe 69.06(9) . . ? C5 C1 Fe 69.32(10) . . ? P C1 Fe 126.00(9) . . ? C3 C2 C1 108.88(16) . . ? C3 C2 Fe 69.87(10) . . ? C1 C2 Fe 70.00(9) . . ? C3 C2 H2 125.6 . . ? C1 C2 H2 125.6 . . ? Fe C2 H2 126.1 . . ? C4 C3 C2 108.06(17) . . ? C4 C3 Fe 69.89(11) . . ? C2 C3 Fe 69.41(10) . . ? C4 C3 H3 126.0 . . ? C2 C3 H3 126.0 . . ? Fe C3 H3 126.3 . . ? C3 C4 C5 108.00(17) . . ? C3 C4 Fe 69.65(11) . . ? C5 C4 Fe 69.39(11) . . ? C3 C4 H4 126.0 . . ? C5 C4 H4 126.0 . . ? Fe C4 H4 126.5 . . ? C1 C5 C4 108.20(17) . . ? C1 C5 Fe 69.76(10) . . ? C4 C5 Fe 69.58(11) . . ? C1 C5 H5 125.9 . . ? C4 C5 H5 125.9 . . ? Fe C5 H5 126.3 . . ? C7 C6 C10 107.60(15) . . ? C7 C6 C11 129.14(16) . . ? C10 C6 C11 122.97(15) . . ? C7 C6 Fe 70.33(9) . . ? C10 C6 Fe 69.48(10) . . ? C11 C6 Fe 120.79(12) . . ? C8 C7 C6 107.87(15) . . ? C8 C7 Fe 70.32(10) . . ? C6 C7 Fe 68.72(9) . . ? C8 C7 H7 126.1 . . ? C6 C7 H7 126.1 . . ? Fe C7 H7 126.5 . . ? C7 C8 C9 108.46(16) . . ? C7 C8 Fe 69.47(10) . . ? C9 C8 Fe 69.29(10) . . ? C7 C8 H8 125.8 . . ? C9 C8 H8 125.8 . . ? Fe C8 H8 127.1 . . ? C8 C9 C10 108.23(16) . . ? C8 C9 Fe 70.46(10) . . ? C10 C9 Fe 69.11(10) . . ? C8 C9 H9 125.9 . . ? C10 C9 H9 125.9 . . ? Fe C9 H9 126.1 . . ? C9 C10 C6 107.83(15) . . ? C9 C10 Fe 70.24(10) . . ? C6 C10 Fe 69.32(10) . . ? C9 C10 H10 126.1 . . ? C6 C10 H10 126.1 . . ? Fe C10 H10 125.9 . . ? O C11 N1 122.19(17) . . ? O C11 C6 121.03(16) . . ? N1 C11 C6 116.78(16) . . ? C17 C12 C13 118.41(16) . . ? C17 C12 P 117.13(13) . . ? C13 C12 P 124.13(13) . . ? C14 C13 C12 120.57(17) . . ? C14 C13 H13 119.7 . . ? C12 C13 H13 119.7 . . ? C15 C14 C13 120.14(18) . . ? C15 C14 H14 119.9 . . ? C13 C14 H14 119.9 . . ? C14 C15 C16 119.86(17) . . ? C14 C15 H15 120.1 . . ? C16 C15 H15 120.1 . . ? C17 C16 C15 119.92(19) . . ? C17 C16 H16 120.0 . . ? C15 C16 H16 120.0 . . ? C16 C17 C12 121.10(18) . . ? C16 C17 H17 119.5 . . ? C12 C17 H17 119.5 . . ? C23 C18 C19 118.35(16) . . ? C23 C18 P 117.02(13) . . ? C19 C18 P 124.57(13) . . ? C20 C19 C18 120.58(17) . . ? C20 C19 H19 119.7 . . ? C18 C19 H19 119.7 . . ? C19 C20 C21 120.18(17) . . ? C19 C20 H20 119.9 . . ? C21 C20 H20 119.9 . . ? C22 C21 C20 120.02(17) . . ? C22 C21 H21 120.0 . . ? C20 C21 H21 120.0 . . ? C21 C22 C23 119.89(17) . . ? C21 C22 H22 120.1 . . ? C23 C22 H22 120.1 . . ? C22 C23 C18 120.87(16) . . ? C22 C23 H23 119.6 . . ? C18 C23 H23 119.6 . . ? N1 C24 C25 111.37(14) . . ? N1 C24 H24A 109.4 . . ? C25 C24 H24A 109.4 . . ? N1 C24 H24B 109.4 . . ? C25 C24 H24B 109.4 . . ? H24A C24 H24B 108.0 . . ? N2 C25 C29 122.15(17) . . ? N2 C25 C24 116.69(15) . . ? C29 C25 C24 121.13(17) . . ? N2 C26 C27 123.22(18) . . ? N2 C26 H26 118.4 . . ? C27 C26 H26 118.4 . . ? C28 C27 C26 118.28(18) . . ? C28 C27 H27 120.9 . . ? C26 C27 H27 120.9 . . ? C27 C28 C29 119.29(18) . . ? C27 C28 H28 120.4 . . ? C29 C28 H28 120.4 . . ? C28 C29 C25 119.56(18) . . ? C28 C29 H29 120.2 . . ? C25 C29 H29 120.2 . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 26.65 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.427 _refine_diff_density_min -0.266 _refine_diff_density_rms 0.053 _chemical_name_common ;N-((pyrid-2yl)methyl) 1'- (diphenylphosphino)ferrocenecarboxamide ; #===END data_jk8c _database_code_depnum_ccdc_archive 'CCDC 633467' _audit_creation_method SHELXL-97 _chemical_name_systematic ; N-[2-(2-pyridyl)ethyl] 1'-(diphennylphosphino)ferrocenecarboxamide ; _chemical_formula_moiety 'C30 H27 Fe N2 O P' _chemical_formula_sum 'C30 H27 Fe N2 O P' _chemical_formula_weight 518.36 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' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.709(4) _cell_length_b 11.067(2) _cell_length_c 13.459(7) _cell_angle_alpha 87.88(2) _cell_angle_beta 75.51(4) _cell_angle_gamma 77.53(2) _cell_volume 1226.1(9) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 6940 _cell_measurement_theta_min 2.56 _cell_measurement_theta_max 26.50 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.404 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 540 _exptl_absorpt_coefficient_mu 0.707 _exptl_absorpt_correction_type none _diffrn_ambient_temperature 150(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_type 'Oxford KM4 CCD diffractometer' _diffrn_measurement_method '\w and \p scans to fill the Ewald sphere' _diffrn_detector_area_resol_mean 8.3438 _diffrn_standards_number 0 _diffrn_reflns_number 16668 _diffrn_reflns_av_R_equivalents 0.0418 _diffrn_reflns_av_sigmaI/netI 0.0724 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.58 _diffrn_reflns_theta_max 26.63 _reflns_number_total 5081 _reflns_number_gt 3273 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.30.2 (release 11-05-2006 CrysAlis171 .NET) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.30.2 (release 11-05-2006 CrysAlis171 .NET) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.30.2 (release 11-05-2006 CrysAlis171 .NET) ; _computing_structure_solution 'SIR-97 (Altomare et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness 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 threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) 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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0319P)^2^+0.0000P] 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 constr _refine_ls_extinction_method none _refine_ls_number_reflns 5081 _refine_ls_number_parameters 317 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0549 _refine_ls_R_factor_gt 0.0308 _refine_ls_wR_factor_ref 0.0646 _refine_ls_wR_factor_gt 0.0624 _refine_ls_goodness_of_fit_ref 0.882 _refine_ls_restrained_S_all 0.882 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_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_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe Fe -0.13458(3) 0.28629(2) 0.220285(19) 0.02615(9) Uani 1 1 d . . . P P 0.10315(6) 0.29512(4) -0.02838(4) 0.02716(13) Uani 1 1 d . . . O O -0.32684(15) 0.23249(12) 0.49279(9) 0.0363(3) Uani 1 1 d . . . N1 N -0.26561(17) 0.41889(14) 0.50871(11) 0.0290(4) Uani 1 1 d . . . H1N H -0.2521 0.4975 0.4803 0.066(7) Uiso 1 1 d R . . N2 N 0.17520(19) 0.32905(14) 0.54696(12) 0.0344(4) Uani 1 1 d . . . C1 C 0.0572(2) 0.22710(16) 0.09715(13) 0.0281(4) Uani 1 1 d . . . C2 C -0.0304(2) 0.13289(16) 0.13175(14) 0.0353(5) Uani 1 1 d . . . H2 H -0.0813 0.0944 0.0929 0.042 Uiso 1 1 calc R . . C3 C -0.0275(3) 0.10726(18) 0.23476(16) 0.0451(6) Uani 1 1 d . . . H3 H -0.0750 0.0485 0.2750 0.054 Uiso 1 1 calc R . . C4 C 0.0593(3) 0.1855(2) 0.26607(15) 0.0455(6) Uani 1 1 d . . . H4 H 0.0788 0.1880 0.3307 0.055 Uiso 1 1 calc R . . C5 C 0.1120(2) 0.26015(18) 0.18210(14) 0.0358(5) Uani 1 1 d . . . H5 H 0.1720 0.3203 0.1821 0.043 Uiso 1 1 calc R . . C6 C -0.3036(2) 0.36178(15) 0.34835(13) 0.0239(4) Uani 1 1 d . . . C7 C -0.2461(2) 0.45722(16) 0.28577(13) 0.0279(4) Uani 1 1 d . . . H7 H -0.1960 0.5153 0.3054 0.033 Uiso 1 1 calc R . . C8 C -0.2780(2) 0.44847(15) 0.18898(13) 0.0282(4) Uani 1 1 d . . . H8 H -0.2523 0.4997 0.1337 0.034 Uiso 1 1 calc R . . C9 C -0.3556(2) 0.34857(17) 0.19026(14) 0.0314(5) Uani 1 1 d . . . H9 H -0.3901 0.3226 0.1362 0.038 Uiso 1 1 calc R . . C10 C -0.3713(2) 0.29549(16) 0.28777(14) 0.0298(5) Uani 1 1 d . . . H10 H -0.4182 0.2280 0.3092 0.036 Uiso 1 1 calc R . . C11 C -0.2982(2) 0.33091(18) 0.45606(14) 0.0285(4) Uani 1 1 d . . . C12 C 0.2512(2) 0.16736(16) -0.10445(13) 0.0260(4) Uani 1 1 d . . . C13 C 0.3181(2) 0.05857(16) -0.06335(15) 0.0315(5) Uani 1 1 d . . . H13 H 0.2797 0.0433 0.0059 0.038 Uiso 1 1 calc R . . C14 C 0.4418(2) -0.02828(17) -0.12386(16) 0.0366(5) Uani 1 1 d . . . H14 H 0.4844 -0.1016 -0.0951 0.044 Uiso 1 1 calc R . . C15 C 0.5015(2) -0.00741(18) -0.22489(16) 0.0377(5) Uani 1 1 d . . . H15 H 0.5853 -0.0658 -0.2648 0.045 Uiso 1 1 calc R . . C16 C 0.4372(3) 0.10061(19) -0.26783(15) 0.0438(5) Uani 1 1 d . . . H16 H 0.4776 0.1155 -0.3369 0.053 Uiso 1 1 calc R . . C17 C 0.3125(2) 0.18690(18) -0.20796(15) 0.0383(5) Uani 1 1 d . . . H17 H 0.2689 0.2593 -0.2375 0.046 Uiso 1 1 calc R . . C18 C -0.0795(2) 0.29613(15) -0.07272(13) 0.0249(4) Uani 1 1 d . . . C19 C -0.1172(2) 0.19191(17) -0.10604(15) 0.0365(5) Uani 1 1 d . . . H19 H -0.0443 0.1161 -0.1103 0.044 Uiso 1 1 calc R . . C20 C -0.2619(3) 0.1991(2) -0.13308(16) 0.0452(6) Uani 1 1 d . . . H20 H -0.2858 0.1284 -0.1554 0.054 Uiso 1 1 calc R . . C21 C -0.3704(3) 0.3105(2) -0.12703(15) 0.0439(6) Uani 1 1 d . . . H21 H -0.4694 0.3150 -0.1430 0.053 Uiso 1 1 calc R . . C22 C -0.3321(3) 0.4149(2) -0.09739(14) 0.0417(5) Uani 1 1 d . . . H22 H -0.4038 0.4910 -0.0953 0.050 Uiso 1 1 calc R . . C23 C -0.1874(2) 0.40780(17) -0.07061(13) 0.0323(5) Uani 1 1 d . . . H23 H -0.1624 0.4794 -0.0509 0.039 Uiso 1 1 calc R . . C24 C -0.2677(2) 0.40770(19) 0.61677(13) 0.0359(5) Uani 1 1 d . . . H24A H -0.3013 0.3319 0.6422 0.043 Uiso 1 1 calc R . . H24B H -0.3466 0.4765 0.6547 0.043 Uiso 1 1 calc R . . C25 C -0.1025(2) 0.40632(17) 0.63577(14) 0.0328(5) Uani 1 1 d . . . H25A H -0.0712 0.4832 0.6115 0.039 Uiso 1 1 calc R . . H25B H -0.1126 0.4038 0.7092 0.039 Uiso 1 1 calc R . . C26 C 0.0309(2) 0.30080(16) 0.58569(13) 0.0254(4) Uani 1 1 d . . . C27 C 0.2982(3) 0.2357(2) 0.50553(16) 0.0503(6) Uani 1 1 d . . . H27 H 0.3997 0.2540 0.4787 0.060 Uiso 1 1 calc R . . C28 C 0.2851(3) 0.1155(2) 0.49989(16) 0.0512(6) Uani 1 1 d . . . H28 H 0.3749 0.0543 0.4702 0.061 Uiso 1 1 calc R . . C29 C 0.1379(3) 0.08793(19) 0.53868(16) 0.0481(6) Uani 1 1 d . . . H29 H 0.1244 0.0071 0.5359 0.058 Uiso 1 1 calc R . . C30 C 0.0095(3) 0.18079(17) 0.58203(15) 0.0374(5) Uani 1 1 d . . . H30 H -0.0924 0.1633 0.6091 0.045 Uiso 1 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 Fe 0.02895(17) 0.02522(16) 0.02320(16) 0.00133(12) -0.00760(12) -0.00230(12) P 0.0332(3) 0.0259(3) 0.0240(3) -0.0001(2) -0.0086(2) -0.0082(2) O 0.0366(8) 0.0438(8) 0.0333(8) 0.0094(7) -0.0092(6) -0.0201(7) N1 0.0297(9) 0.0364(10) 0.0209(9) -0.0008(8) -0.0067(7) -0.0065(8) N2 0.0278(10) 0.0449(10) 0.0303(9) -0.0055(8) -0.0050(8) -0.0086(8) C1 0.0289(11) 0.0265(10) 0.0248(10) -0.0002(8) -0.0059(9) 0.0021(9) C2 0.0458(13) 0.0228(10) 0.0305(12) -0.0025(9) -0.0022(10) -0.0006(9) C3 0.0568(15) 0.0289(11) 0.0335(13) 0.0093(10) 0.0013(11) 0.0088(11) C4 0.0392(13) 0.0618(15) 0.0250(12) 0.0033(11) -0.0115(10) 0.0156(12) C5 0.0263(11) 0.0490(13) 0.0293(12) -0.0010(10) -0.0089(9) 0.0008(10) C6 0.0220(10) 0.0261(10) 0.0234(10) 0.0001(8) -0.0067(8) -0.0035(8) C7 0.0315(11) 0.0238(10) 0.0293(11) -0.0018(9) -0.0103(9) -0.0047(9) C8 0.0368(12) 0.0230(10) 0.0224(11) 0.0033(8) -0.0093(9) 0.0006(9) C9 0.0298(11) 0.0366(11) 0.0302(12) -0.0020(9) -0.0158(9) -0.0023(9) C10 0.0278(11) 0.0321(11) 0.0323(12) -0.0001(9) -0.0092(9) -0.0103(9) C11 0.0175(10) 0.0380(12) 0.0278(11) -0.0014(10) -0.0035(8) -0.0031(9) C12 0.0278(11) 0.0287(10) 0.0248(11) -0.0007(8) -0.0105(9) -0.0081(9) C13 0.0303(12) 0.0338(11) 0.0317(11) 0.0034(9) -0.0088(9) -0.0090(10) C14 0.0334(12) 0.0313(11) 0.0469(14) 0.0007(10) -0.0166(10) -0.0028(10) C15 0.0294(12) 0.0411(12) 0.0421(13) -0.0135(11) -0.0101(10) -0.0024(10) C16 0.0461(14) 0.0559(14) 0.0261(12) -0.0080(11) -0.0063(10) -0.0054(12) C17 0.0465(13) 0.0374(12) 0.0300(12) -0.0017(10) -0.0155(10) 0.0005(10) C18 0.0323(11) 0.0245(10) 0.0185(10) 0.0024(8) -0.0075(8) -0.0065(9) C19 0.0441(13) 0.0268(11) 0.0442(13) 0.0057(9) -0.0207(11) -0.0094(10) C20 0.0555(15) 0.0448(13) 0.0499(14) 0.0109(11) -0.0259(12) -0.0288(12) C21 0.0330(13) 0.0682(16) 0.0360(13) 0.0172(12) -0.0147(10) -0.0182(12) C22 0.0401(13) 0.0501(14) 0.0264(12) 0.0028(10) -0.0096(10) 0.0097(11) C23 0.0480(13) 0.0275(11) 0.0215(10) -0.0016(8) -0.0119(9) -0.0040(10) C24 0.0292(12) 0.0537(13) 0.0215(11) -0.0059(10) -0.0052(9) -0.0020(10) C25 0.0316(12) 0.0419(12) 0.0245(11) -0.0055(9) -0.0072(9) -0.0057(10) C26 0.0279(12) 0.0331(11) 0.0159(10) 0.0021(8) -0.0088(9) -0.0045(9) C27 0.0243(12) 0.0815(18) 0.0424(14) -0.0153(13) -0.0056(10) -0.0055(13) C28 0.0495(16) 0.0570(16) 0.0397(14) -0.0212(12) -0.0245(12) 0.0240(13) C29 0.0731(18) 0.0330(12) 0.0403(14) 0.0016(11) -0.0286(13) 0.0011(13) C30 0.0445(14) 0.0373(12) 0.0323(12) 0.0036(10) -0.0086(10) -0.0143(11) _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 Fe C10 2.016(2) . ? Fe C2 2.0171(19) . ? Fe C3 2.0243(19) . ? Fe C4 2.033(2) . ? Fe C9 2.034(2) . ? Fe C6 2.035(2) . ? Fe C5 2.037(2) . ? Fe C1 2.047(2) . ? Fe C8 2.0489(18) . ? Fe C7 2.0494(18) . ? P C1 1.811(2) . ? P C18 1.8315(19) . ? P C12 1.836(2) . ? O C11 1.228(2) . ? N1 C11 1.342(2) . ? N1 C24 1.451(2) . ? N1 H1N 0.9565 . ? N2 C26 1.334(2) . ? N2 C27 1.338(3) . ? C1 C2 1.420(2) . ? C1 C5 1.431(3) . ? C2 C3 1.410(3) . ? C2 H2 0.9300 . ? C3 C4 1.403(3) . ? C3 H3 0.9300 . ? C4 C5 1.416(3) . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? C6 C10 1.422(2) . ? C6 C7 1.424(2) . ? C6 C11 1.487(3) . ? C7 C8 1.409(2) . ? C7 H7 0.9300 . ? C8 C9 1.412(2) . ? C8 H8 0.9300 . ? C9 C10 1.405(2) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? C12 C13 1.380(2) . ? C12 C17 1.389(3) . ? C13 C14 1.385(3) . ? C13 H13 0.9300 . ? C14 C15 1.359(3) . ? C14 H14 0.9300 . ? C15 C16 1.378(3) . ? C15 H15 0.9300 . ? C16 C17 1.383(3) . ? C16 H16 0.9300 . ? C17 H17 0.9300 . ? C18 C23 1.378(2) . ? C18 C19 1.384(2) . ? C19 C20 1.382(3) . ? C19 H19 0.9300 . ? C20 C21 1.373(3) . ? C20 H20 0.9300 . ? C21 C22 1.368(3) . ? C21 H21 0.9300 . ? C22 C23 1.381(3) . ? C22 H22 0.9300 . ? C23 H23 0.9300 . ? C24 C25 1.520(2) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 C26 1.499(2) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 C30 1.385(2) . ? C27 C28 1.366(3) . ? C27 H27 0.9300 . ? C28 C29 1.353(3) . ? C28 H28 0.9300 . ? C29 C30 1.367(3) . ? C29 H29 0.9300 . ? C30 H30 0.9300 . ? 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 C10 Fe C2 113.02(8) . . ? C10 Fe C3 104.17(9) . . ? C2 Fe C3 40.84(8) . . ? C10 Fe C4 127.08(8) . . ? C2 Fe C4 68.54(9) . . ? C3 Fe C4 40.47(8) . . ? C10 Fe C9 40.59(7) . . ? C2 Fe C9 105.80(8) . . ? C3 Fe C9 126.17(9) . . ? C4 Fe C9 164.68(8) . . ? C10 Fe C6 41.09(7) . . ? C2 Fe C6 146.40(8) . . ? C3 Fe C6 114.13(8) . . ? C4 Fe C6 107.55(8) . . ? C9 Fe C6 68.80(8) . . ? C10 Fe C5 167.26(7) . . ? C2 Fe C5 68.65(9) . . ? C3 Fe C5 68.38(9) . . ? C4 Fe C5 40.72(8) . . ? C9 Fe C5 152.13(8) . . ? C6 Fe C5 131.16(8) . . ? C10 Fe C1 147.53(7) . . ? C2 Fe C1 40.90(7) . . ? C3 Fe C1 68.81(8) . . ? C4 Fe C1 68.87(8) . . ? C9 Fe C1 116.83(8) . . ? C6 Fe C1 171.17(7) . . ? C5 Fe C1 41.03(7) . . ? C10 Fe C8 68.10(8) . . ? C2 Fe C8 129.78(8) . . ? C3 Fe C8 165.90(9) . . ? C4 Fe C8 153.50(9) . . ? C9 Fe C8 40.47(7) . . ? C6 Fe C8 68.41(7) . . ? C5 Fe C8 121.32(8) . . ? C1 Fe C8 110.92(8) . . ? C10 Fe C7 68.37(8) . . ? C2 Fe C7 169.56(7) . . ? C3 Fe C7 149.60(8) . . ? C4 Fe C7 119.53(9) . . ? C9 Fe C7 68.12(8) . . ? C6 Fe C7 40.81(7) . . ? C5 Fe C7 112.46(8) . . ? C1 Fe C7 133.15(7) . . ? C8 Fe C7 40.22(7) . . ? C1 P C18 102.51(9) . . ? C1 P C12 101.83(9) . . ? C18 P C12 102.40(8) . . ? C11 N1 C24 122.37(16) . . ? C11 N1 H1N 122.5 . . ? C24 N1 H1N 114.7 . . ? C26 N2 C27 116.79(17) . . ? C2 C1 C5 106.62(17) . . ? C2 C1 P 129.74(14) . . ? C5 C1 P 123.61(14) . . ? C2 C1 Fe 68.44(10) . . ? C5 C1 Fe 69.15(11) . . ? P C1 Fe 128.62(10) . . ? C3 C2 C1 108.73(18) . . ? C3 C2 Fe 69.85(11) . . ? C1 C2 Fe 70.66(11) . . ? C3 C2 H2 125.6 . . ? C1 C2 H2 125.6 . . ? Fe C2 H2 125.4 . . ? C4 C3 C2 108.29(18) . . ? C4 C3 Fe 70.08(11) . . ? C2 C3 Fe 69.30(11) . . ? C4 C3 H3 125.9 . . ? C2 C3 H3 125.9 . . ? Fe C3 H3 126.3 . . ? C3 C4 C5 108.13(18) . . ? C3 C4 Fe 69.45(12) . . ? C5 C4 Fe 69.83(11) . . ? C3 C4 H4 125.9 . . ? C5 C4 H4 125.9 . . ? Fe C4 H4 126.4 . . ? C4 C5 C1 108.22(18) . . ? C4 C5 Fe 69.45(12) . . ? C1 C5 Fe 69.82(11) . . ? C4 C5 H5 125.9 . . ? C1 C5 H5 125.9 . . ? Fe C5 H5 126.4 . . ? C10 C6 C7 106.78(16) . . ? C10 C6 C11 123.79(16) . . ? C7 C6 C11 129.43(16) . . ? C10 C6 Fe 68.73(10) . . ? C7 C6 Fe 70.13(10) . . ? C11 C6 Fe 125.79(12) . . ? C8 C7 C6 108.27(16) . . ? C8 C7 Fe 69.87(10) . . ? C6 C7 Fe 69.06(10) . . ? C8 C7 H7 125.9 . . ? C6 C7 H7 125.9 . . ? Fe C7 H7 126.8 . . ? C7 C8 C9 108.30(16) . . ? C7 C8 Fe 69.91(10) . . ? C9 C8 Fe 69.21(10) . . ? C7 C8 H8 125.8 . . ? C9 C8 H8 125.8 . . ? Fe C8 H8 126.6 . . ? C10 C9 C8 107.79(16) . . ? C10 C9 Fe 69.00(11) . . ? C8 C9 Fe 70.32(10) . . ? C10 C9 H9 126.1 . . ? C8 C9 H9 126.1 . . ? Fe C9 H9 126.1 . . ? C9 C10 C6 108.86(16) . . ? C9 C10 Fe 70.41(11) . . ? C6 C10 Fe 70.19(11) . . ? C9 C10 H10 125.6 . . ? C6 C10 H10 125.6 . . ? Fe C10 H10 125.4 . . ? O C11 N1 123.92(17) . . ? O C11 C6 120.79(17) . . ? N1 C11 C6 115.25(17) . . ? C13 C12 C17 117.83(17) . . ? C13 C12 P 124.10(14) . . ? C17 C12 P 117.70(14) . . ? C12 C13 C14 120.85(18) . . ? C12 C13 H13 119.6 . . ? C14 C13 H13 119.6 . . ? C15 C14 C13 120.66(19) . . ? C15 C14 H14 119.7 . . ? C13 C14 H14 119.7 . . ? C14 C15 C16 119.68(19) . . ? C14 C15 H15 120.2 . . ? C16 C15 H15 120.2 . . ? C15 C16 C17 119.83(19) . . ? C15 C16 H16 120.1 . . ? C17 C16 H16 120.1 . . ? C16 C17 C12 121.14(19) . . ? C16 C17 H17 119.4 . . ? C12 C17 H17 119.4 . . ? C23 C18 C19 118.23(18) . . ? C23 C18 P 117.54(13) . . ? C19 C18 P 124.22(14) . . ? C20 C19 C18 120.79(19) . . ? C20 C19 H19 119.6 . . ? C18 C19 H19 119.6 . . ? C21 C20 C19 120.06(19) . . ? C21 C20 H20 120.0 . . ? C19 C20 H20 120.0 . . ? C22 C21 C20 119.66(19) . . ? C22 C21 H21 120.2 . . ? C20 C21 H21 120.2 . . ? C21 C22 C23 120.24(19) . . ? C21 C22 H22 119.9 . . ? C23 C22 H22 119.9 . . ? C18 C23 C22 120.95(18) . . ? C18 C23 H23 119.5 . . ? C22 C23 H23 119.5 . . ? N1 C24 C25 112.11(15) . . ? N1 C24 H24A 109.2 . . ? C25 C24 H24A 109.2 . . ? N1 C24 H24B 109.2 . . ? C25 C24 H24B 109.2 . . ? H24A C24 H24B 107.9 . . ? C26 C25 C24 115.22(15) . . ? C26 C25 H25A 108.5 . . ? C24 C25 H25A 108.5 . . ? C26 C25 H25B 108.5 . . ? C24 C25 H25B 108.5 . . ? H25A C25 H25B 107.5 . . ? N2 C26 C30 121.42(17) . . ? N2 C26 C25 115.44(16) . . ? C30 C26 C25 123.11(18) . . ? N2 C27 C28 124.6(2) . . ? N2 C27 H27 117.7 . . ? C28 C27 H27 117.7 . . ? C29 C28 C27 118.2(2) . . ? C29 C28 H28 120.9 . . ? C27 C28 H28 120.9 . . ? C28 C29 C30 118.9(2) . . ? C28 C29 H29 120.6 . . ? C30 C29 H29 120.6 . . ? C29 C30 C26 120.1(2) . . ? C29 C30 H30 120.0 . . ? C26 C30 H30 120.0 . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 26.63 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.368 _refine_diff_density_min -0.224 _refine_diff_density_rms 0.047 _chemical_name_common ;N-(2-(2-pyridyl)ethyl) 1'- (diphennylphosphino)ferrocenecarboxamide ; #===END data_jk13sq _database_code_depnum_ccdc_archive 'CCDC 633468' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C60 H54 Cl2 Fe2 N4 O2 P2 Pd, 2 (C H Cl3)' _chemical_formula_sum 'C64 H56 Cl14 Fe2 N4 O2 P2 Pd' _chemical_formula_weight 1689.47 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' Cl Cl 0.1484 0.1585 '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' 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' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.069(2) _cell_length_b 12.650(3) _cell_length_c 13.042(4) _cell_angle_alpha 93.48(2) _cell_angle_beta 102.39(2) _cell_angle_gamma 91.18(2) _cell_volume 1779.3(8) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 13230 _cell_measurement_theta_min 2.52 _cell_measurement_theta_max 26.50 _exptl_crystal_description red _exptl_crystal_colour prism _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_diffrn 1.577 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 620 _exptl_absorpt_coefficient_mu 1.260 _exptl_absorpt_correction_T_min 0.706 _exptl_absorpt_correction_T_max 0.773 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.30.2 (release 11-05-2006 CrysAlis171 .NET) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_measurement_device_type 'Oxford KM4 CCD diffractometer' _diffrn_measurement_method '\w and \p scans to fill the Ewald sphere' _diffrn_detector_area_resol_mean 8.3438 _diffrn_standards_number 0 _diffrn_reflns_number 24109 _diffrn_reflns_av_R_equivalents 0.0262 _diffrn_reflns_av_sigmaI/netI 0.0455 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.70 _diffrn_reflns_theta_max 26.58 _reflns_number_total 7356 _reflns_number_gt 5406 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.29.5 (release 22-02-2006 CrysAlis171 .NET) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.29.5 (release 22-02-2006 CrysAlis171 .NET) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.29.5 (release 22-02-2006 CrysAlis171 .NET) ; _computing_structure_solution 'SIR-97 (Altomare et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' # SQUEEZE RESULTS (APPEND TO CIF) loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 -0.014 -0.006 0.000 609.8 54.5 _platon_squeeze_details ; ? ; _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness 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 threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) 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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0631P)^2^+0.0000P] 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 constr _refine_ls_extinction_method none _refine_ls_number_reflns 7356 _refine_ls_number_parameters 331 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0446 _refine_ls_R_factor_gt 0.0329 _refine_ls_wR_factor_ref 0.0982 _refine_ls_wR_factor_gt 0.0962 _refine_ls_goodness_of_fit_ref 0.984 _refine_ls_restrained_S_all 0.984 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_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_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd Pd 1.0000 0.0000 0.5000 0.01903(9) Uani 1 2 d S . . Fe Fe 0.79869(3) 0.22826(3) 0.66532(3) 0.02153(10) Uani 1 1 d . . . Cl Cl 0.93863(6) 0.10793(6) 0.36433(5) 0.02942(16) Uani 1 1 d . . . P P 0.79395(6) -0.00512(5) 0.51344(5) 0.01985(15) Uani 1 1 d . . . O O 0.75636(19) 0.50045(15) 0.75214(16) 0.0364(5) Uani 1 1 d . . . N1 N 0.9205(2) 0.51892(18) 0.67698(18) 0.0290(5) Uani 1 1 d . . . H1N H 0.9938 0.4932 0.6666 0.035 Uiso 1 1 d R . . N2 N 0.8305(2) 0.5172(2) 0.3769(2) 0.0450(7) Uani 1 1 d . . . C1 C 0.7292(2) 0.1190(2) 0.5432(2) 0.0225(6) Uani 1 1 d . . . C2 C 0.6440(2) 0.1335(2) 0.6111(2) 0.0294(6) Uani 1 1 d . . . H2 H 0.6141 0.0810 0.6471 0.035 Uiso 1 1 calc R . . C3 C 0.6133(3) 0.2416(2) 0.6140(3) 0.0354(7) Uani 1 1 d . . . H3 H 0.5596 0.2722 0.6523 0.042 Uiso 1 1 calc R . . C4 C 0.6782(3) 0.2954(2) 0.5487(2) 0.0337(7) Uani 1 1 d . . . H4 H 0.6740 0.3671 0.5367 0.040 Uiso 1 1 calc R . . C5 C 0.7503(3) 0.2214(2) 0.5051(2) 0.0280(6) Uani 1 1 d . . . H5 H 0.8022 0.2360 0.4600 0.034 Uiso 1 1 calc R . . C6 C 0.8887(2) 0.3559(2) 0.7522(2) 0.0250(6) Uani 1 1 d . . . C7 C 0.9742(2) 0.2914(2) 0.7110(2) 0.0257(6) Uani 1 1 d . . . H7 H 1.0242 0.3131 0.6668 0.031 Uiso 1 1 calc R . . C8 C 0.9703(2) 0.1897(2) 0.7487(2) 0.0279(6) Uani 1 1 d . . . H8 H 1.0167 0.1328 0.7332 0.034 Uiso 1 1 calc R . . C9 C 0.8839(3) 0.1891(2) 0.8138(2) 0.0315(7) Uani 1 1 d . . . H9 H 0.8638 0.1318 0.8491 0.038 Uiso 1 1 calc R . . C10 C 0.8328(3) 0.2909(2) 0.8164(2) 0.0307(6) Uani 1 1 d . . . H10 H 0.7733 0.3118 0.8535 0.037 Uiso 1 1 calc R . . C11 C 0.8499(2) 0.4641(2) 0.7280(2) 0.0251(6) Uani 1 1 d . . . C12 C 0.7039(2) -0.0554(2) 0.38577(19) 0.0218(5) Uani 1 1 d . . . C13 C 0.6138(2) 0.0017(2) 0.3255(2) 0.0278(6) Uani 1 1 d . . . H13 H 0.5942 0.0679 0.3512 0.033 Uiso 1 1 calc R . . C14 C 0.5521(3) -0.0391(3) 0.2267(2) 0.0382(7) Uani 1 1 d . . . H14 H 0.4915 0.0000 0.1863 0.046 Uiso 1 1 calc R . . C15 C 0.5802(3) -0.1371(3) 0.1880(2) 0.0436(8) Uani 1 1 d . . . H15 H 0.5384 -0.1641 0.1217 0.052 Uiso 1 1 calc R . . C16 C 0.6697(3) -0.1951(3) 0.2471(2) 0.0429(8) Uani 1 1 d . . . H16 H 0.6881 -0.2616 0.2212 0.052 Uiso 1 1 calc R . . C17 C 0.7323(3) -0.1542(2) 0.3453(2) 0.0330(7) Uani 1 1 d . . . H17 H 0.7940 -0.1930 0.3847 0.040 Uiso 1 1 calc R . . C18 C 0.7459(2) -0.0882(2) 0.6081(2) 0.0212(5) Uani 1 1 d . . . C19 C 0.6412(2) -0.1556(2) 0.5793(2) 0.0250(6) Uani 1 1 d . . . H19 H 0.5986 -0.1631 0.5094 0.030 Uiso 1 1 calc R . . C20 C 0.6001(3) -0.2118(2) 0.6545(2) 0.0301(6) Uani 1 1 d . . . H20 H 0.5299 -0.2563 0.6350 0.036 Uiso 1 1 calc R . . C21 C 0.6632(3) -0.2013(2) 0.7575(2) 0.0328(7) Uani 1 1 d . . . H21 H 0.6358 -0.2393 0.8075 0.039 Uiso 1 1 calc R . . C22 C 0.7672(3) -0.1348(2) 0.7876(2) 0.0308(6) Uani 1 1 d . . . H22 H 0.8095 -0.1279 0.8575 0.037 Uiso 1 1 calc R . . C23 C 0.8083(2) -0.0783(2) 0.7124(2) 0.0259(6) Uani 1 1 d . . . H23 H 0.8782 -0.0336 0.7325 0.031 Uiso 1 1 calc R . . C24 C 0.8936(3) 0.6265(2) 0.6461(2) 0.0372(7) Uani 1 1 d . . . H24B H 0.9551 0.6758 0.6889 0.045 Uiso 1 1 calc R . . H24A H 0.8133 0.6451 0.6588 0.045 Uiso 1 1 calc R . . C25 C 0.8940(3) 0.6365(2) 0.5305(2) 0.0335(7) Uani 1 1 d . . . H25A H 0.8872 0.7108 0.5162 0.040 Uiso 1 1 calc R . . H25B H 0.9733 0.6141 0.5184 0.040 Uiso 1 1 calc R . . C26 C 0.7941(3) 0.5747(2) 0.4534(2) 0.0294(6) Uani 1 1 d . . . C27 C 0.7437(4) 0.4628(4) 0.3051(3) 0.0655(12) Uani 1 1 d . . . H27 H 0.7694 0.4212 0.2529 0.079 Uiso 1 1 calc R . . C28 C 0.6194(3) 0.4639(3) 0.3028(3) 0.0548(10) Uani 1 1 d . . . H28 H 0.5625 0.4258 0.2500 0.066 Uiso 1 1 calc R . . C29 C 0.5825(3) 0.5221(3) 0.3798(3) 0.0481(9) Uani 1 1 d . . . H29 H 0.4990 0.5247 0.3812 0.058 Uiso 1 1 calc R . . C30 C 0.6698(3) 0.5777(2) 0.4565(3) 0.0470(9) Uani 1 1 d . . . H30 H 0.6453 0.6174 0.5104 0.056 Uiso 1 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 0.01760(16) 0.01993(16) 0.01851(15) 0.00298(11) 0.00126(11) -0.00131(11) Fe 0.0208(2) 0.0218(2) 0.0214(2) -0.00058(16) 0.00390(15) -0.00053(15) Cl 0.0260(4) 0.0348(4) 0.0282(4) 0.0140(3) 0.0039(3) 0.0026(3) P 0.0180(3) 0.0201(3) 0.0201(3) 0.0011(3) 0.0014(3) -0.0010(3) O 0.0426(13) 0.0350(12) 0.0351(12) -0.0017(9) 0.0170(10) 0.0067(10) N1 0.0313(13) 0.0238(12) 0.0328(13) 0.0002(10) 0.0096(11) 0.0008(10) N2 0.0385(16) 0.0602(19) 0.0357(15) -0.0093(14) 0.0112(12) -0.0080(13) C1 0.0187(13) 0.0221(14) 0.0236(14) -0.0024(11) -0.0012(10) -0.0007(10) C2 0.0192(14) 0.0296(15) 0.0377(16) -0.0029(13) 0.0044(12) -0.0038(11) C3 0.0220(15) 0.0326(16) 0.0479(19) -0.0084(14) 0.0022(13) 0.0036(12) C4 0.0354(17) 0.0262(15) 0.0327(16) -0.0008(13) -0.0076(13) 0.0079(13) C5 0.0333(16) 0.0248(15) 0.0222(14) 0.0023(11) -0.0026(12) 0.0012(12) C6 0.0292(15) 0.0248(14) 0.0187(13) -0.0030(11) 0.0019(11) -0.0037(11) C7 0.0218(14) 0.0273(15) 0.0266(14) -0.0005(12) 0.0029(11) -0.0019(11) C8 0.0284(15) 0.0245(15) 0.0267(15) 0.0009(12) -0.0032(12) 0.0028(11) C9 0.0430(18) 0.0296(16) 0.0203(14) 0.0027(12) 0.0031(12) -0.0032(13) C10 0.0397(17) 0.0341(16) 0.0191(14) -0.0021(12) 0.0091(12) -0.0005(13) C11 0.0299(15) 0.0263(14) 0.0184(13) -0.0048(11) 0.0054(11) -0.0007(12) C12 0.0184(13) 0.0270(14) 0.0190(13) -0.0002(11) 0.0027(10) -0.0038(10) C13 0.0232(15) 0.0318(16) 0.0276(15) -0.0004(12) 0.0041(12) 0.0024(12) C14 0.0276(16) 0.053(2) 0.0294(16) 0.0015(15) -0.0044(13) 0.0035(14) C15 0.0407(19) 0.058(2) 0.0261(16) -0.0119(15) -0.0005(14) -0.0067(16) C16 0.052(2) 0.0344(18) 0.0379(18) -0.0115(15) 0.0043(16) -0.0011(15) C17 0.0352(17) 0.0288(16) 0.0323(16) -0.0014(13) 0.0021(13) 0.0056(13) C18 0.0200(13) 0.0199(13) 0.0250(14) 0.0030(11) 0.0071(11) 0.0047(10) C19 0.0231(14) 0.0217(14) 0.0307(15) 0.0017(12) 0.0066(12) 0.0029(11) C20 0.0237(15) 0.0245(15) 0.0440(18) 0.0041(13) 0.0115(13) 0.0004(11) C21 0.0354(17) 0.0298(16) 0.0393(18) 0.0110(13) 0.0187(14) 0.0063(13) C22 0.0384(17) 0.0322(16) 0.0233(14) 0.0042(12) 0.0086(12) 0.0062(13) C23 0.0267(15) 0.0239(14) 0.0267(14) -0.0004(11) 0.0054(11) -0.0003(11) C24 0.051(2) 0.0211(15) 0.0394(18) 0.0007(13) 0.0098(15) -0.0010(13) C25 0.0438(18) 0.0218(15) 0.0340(17) 0.0057(13) 0.0059(14) -0.0024(13) C26 0.0334(16) 0.0212(14) 0.0344(16) 0.0074(12) 0.0073(13) 0.0043(12) C27 0.055(2) 0.101(3) 0.039(2) -0.027(2) 0.0181(18) -0.025(2) C28 0.043(2) 0.073(3) 0.043(2) 0.0065(19) -0.0034(16) -0.0148(18) C29 0.0243(17) 0.0341(18) 0.083(3) 0.0097(18) 0.0035(17) 0.0008(14) C30 0.045(2) 0.0284(17) 0.072(3) -0.0056(16) 0.0242(18) 0.0042(14) _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 Cl 2.2960(9) 2_756 ? Pd Cl 2.2960(9) . ? Pd P 2.3245(8) . ? Pd P 2.3246(8) 2_756 ? Fe C6 2.027(3) . ? Fe C3 2.031(3) . ? Fe C10 2.033(3) . ? Fe C4 2.036(3) . ? Fe C7 2.037(3) . ? Fe C5 2.038(3) . ? Fe C2 2.040(3) . ? Fe C1 2.050(3) . ? Fe C9 2.059(3) . ? Fe C8 2.060(3) . ? P C1 1.795(3) . ? P C12 1.818(3) . ? P C18 1.824(3) . ? O C11 1.235(3) . ? N1 C11 1.338(3) . ? N1 C24 1.461(4) . ? N1 H1N 0.9142 . ? N2 C26 1.335(4) . ? N2 C27 1.336(4) . ? C1 C2 1.434(4) . ? C1 C5 1.447(4) . ? C2 C3 1.416(4) . ? C2 H2 0.9300 . ? C3 C4 1.420(4) . ? C3 H3 0.9300 . ? C4 C5 1.413(4) . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? C6 C7 1.430(4) . ? C6 C10 1.431(4) . ? C6 C11 1.475(4) . ? C7 C8 1.408(4) . ? C7 H7 0.9300 . ? C8 C9 1.409(4) . ? C8 H8 0.9300 . ? C9 C10 1.419(4) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? C12 C13 1.378(4) . ? C12 C17 1.395(4) . ? C13 C14 1.386(4) . ? C13 H13 0.9300 . ? C14 C15 1.377(5) . ? C14 H14 0.9300 . ? C15 C16 1.373(5) . ? C15 H15 0.9300 . ? C16 C17 1.382(4) . ? C16 H16 0.9300 . ? C17 H17 0.9300 . ? C18 C23 1.385(4) . ? C18 C19 1.394(4) . ? C19 C20 1.392(4) . ? C19 H19 0.9300 . ? C20 C21 1.371(4) . ? C20 H20 0.9300 . ? C21 C22 1.383(4) . ? C21 H21 0.9300 . ? C22 C23 1.393(4) . ? C22 H22 0.9300 . ? C23 H23 0.9300 . ? C24 C25 1.521(4) . ? C24 H24B 0.9700 . ? C24 H24A 0.9700 . ? C25 C26 1.496(4) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 C30 1.386(4) . ? C27 C28 1.370(5) . ? C27 H27 0.9300 . ? C28 C29 1.347(5) . ? C28 H28 0.9300 . ? C29 C30 1.379(5) . ? C29 H29 0.9300 . ? C30 H30 0.9300 . ? 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 Cl Pd Cl 180.0 2_756 . ? Cl Pd P 93.78(3) 2_756 . ? Cl Pd P 86.22(3) . . ? Cl Pd P 86.22(3) 2_756 2_756 ? Cl Pd P 93.78(3) . 2_756 ? P Pd P 180.0 . 2_756 ? C6 Fe C3 115.45(11) . . ? C6 Fe C10 41.27(11) . . ? C3 Fe C10 103.91(13) . . ? C6 Fe C4 102.78(12) . . ? C3 Fe C4 40.88(12) . . ? C10 Fe C4 121.34(12) . . ? C6 Fe C7 41.20(11) . . ? C3 Fe C7 152.08(12) . . ? C10 Fe C7 68.63(11) . . ? C4 Fe C7 118.57(12) . . ? C6 Fe C5 122.70(11) . . ? C3 Fe C5 68.73(12) . . ? C10 Fe C5 159.12(11) . . ? C4 Fe C5 40.58(11) . . ? C7 Fe C5 108.23(11) . . ? C6 Fe C2 151.70(11) . . ? C3 Fe C2 40.71(11) . . ? C10 Fe C2 118.71(12) . . ? C4 Fe C2 68.80(12) . . ? C7 Fe C2 166.36(11) . . ? C5 Fe C2 69.21(12) . . ? C6 Fe C1 162.76(10) . . ? C3 Fe C1 68.84(11) . . ? C10 Fe C1 155.95(11) . . ? C4 Fe C1 68.97(11) . . ? C7 Fe C1 128.33(11) . . ? C5 Fe C1 41.45(10) . . ? C2 Fe C1 41.05(11) . . ? C6 Fe C9 68.73(11) . . ? C3 Fe C9 124.87(13) . . ? C10 Fe C9 40.56(11) . . ? C4 Fe C9 159.94(12) . . ? C7 Fe C9 67.70(11) . . ? C5 Fe C9 159.10(12) . . ? C2 Fe C9 109.62(12) . . ? C1 Fe C9 123.86(11) . . ? C6 Fe C8 68.70(11) . . ? C3 Fe C8 163.60(12) . . ? C10 Fe C8 68.12(12) . . ? C4 Fe C8 155.52(12) . . ? C7 Fe C8 40.18(11) . . ? C5 Fe C8 123.68(12) . . ? C2 Fe C8 129.29(11) . . ? C1 Fe C8 112.27(11) . . ? C9 Fe C8 40.02(11) . . ? C1 P C12 106.16(12) . . ? C1 P C18 101.43(12) . . ? C12 P C18 105.20(12) . . ? C1 P Pd 116.69(9) . . ? C12 P Pd 106.69(9) . . ? C18 P Pd 119.50(9) . . ? C11 N1 C24 122.8(2) . . ? C11 N1 H1N 120.6 . . ? C24 N1 H1N 116.2 . . ? C26 N2 C27 117.8(3) . . ? C2 C1 C5 107.0(2) . . ? C2 C1 P 124.7(2) . . ? C5 C1 P 128.3(2) . . ? C2 C1 Fe 69.11(15) . . ? C5 C1 Fe 68.84(15) . . ? P C1 Fe 127.29(14) . . ? C3 C2 C1 108.1(2) . . ? C3 C2 Fe 69.31(16) . . ? C1 C2 Fe 69.84(15) . . ? C3 C2 H2 126.0 . . ? C1 C2 H2 126.0 . . ? Fe C2 H2 126.5 . . ? C2 C3 C4 108.6(3) . . ? C2 C3 Fe 69.98(16) . . ? C4 C3 Fe 69.74(16) . . ? C2 C3 H3 125.7 . . ? C4 C3 H3 125.7 . . ? Fe C3 H3 126.1 . . ? C5 C4 C3 108.4(3) . . ? C5 C4 Fe 69.80(16) . . ? C3 C4 Fe 69.39(17) . . ? C5 C4 H4 125.8 . . ? C3 C4 H4 125.8 . . ? Fe C4 H4 126.6 . . ? C4 C5 C1 108.0(2) . . ? C4 C5 Fe 69.62(16) . . ? C1 C5 Fe 69.71(15) . . ? C4 C5 H5 126.0 . . ? C1 C5 H5 126.0 . . ? Fe C5 H5 126.2 . . ? C7 C6 C10 106.7(2) . . ? C7 C6 C11 129.6(2) . . ? C10 C6 C11 123.5(2) . . ? C7 C6 Fe 69.78(15) . . ? C10 C6 Fe 69.61(15) . . ? C11 C6 Fe 120.54(19) . . ? C8 C7 C6 108.7(2) . . ? C8 C7 Fe 70.78(15) . . ? C6 C7 Fe 69.01(15) . . ? C8 C7 H7 125.6 . . ? C6 C7 H7 125.6 . . ? Fe C7 H7 126.1 . . ? C7 C8 C9 108.2(2) . . ? C7 C8 Fe 69.04(15) . . ? C9 C8 Fe 69.94(16) . . ? C7 C8 H8 125.9 . . ? C9 C8 H8 125.9 . . ? Fe C8 H8 126.7 . . ? C8 C9 C10 108.3(2) . . ? C8 C9 Fe 70.05(15) . . ? C10 C9 Fe 68.76(16) . . ? C8 C9 H9 125.8 . . ? C10 C9 H9 125.8 . . ? Fe C9 H9 126.9 . . ? C9 C10 C6 108.1(2) . . ? C9 C10 Fe 70.67(16) . . ? C6 C10 Fe 69.13(15) . . ? C9 C10 H10 126.0 . . ? C6 C10 H10 126.0 . . ? Fe C10 H10 125.8 . . ? O C11 N1 122.5(3) . . ? O C11 C6 121.4(2) . . ? N1 C11 C6 116.1(2) . . ? C13 C12 C17 118.9(2) . . ? C13 C12 P 123.0(2) . . ? C17 C12 P 118.1(2) . . ? C12 C13 C14 120.2(3) . . ? C12 C13 H13 119.9 . . ? C14 C13 H13 119.9 . . ? C15 C14 C13 120.3(3) . . ? C15 C14 H14 119.8 . . ? C13 C14 H14 119.8 . . ? C16 C15 C14 120.2(3) . . ? C16 C15 H15 119.9 . . ? C14 C15 H15 119.9 . . ? C15 C16 C17 119.7(3) . . ? C15 C16 H16 120.2 . . ? C17 C16 H16 120.2 . . ? C16 C17 C12 120.7(3) . . ? C16 C17 H17 119.7 . . ? C12 C17 H17 119.7 . . ? C23 C18 C19 119.0(2) . . ? C23 C18 P 119.6(2) . . ? C19 C18 P 121.2(2) . . ? C20 C19 C18 120.4(3) . . ? C20 C19 H19 119.8 . . ? C18 C19 H19 119.8 . . ? C21 C20 C19 119.9(3) . . ? C21 C20 H20 120.1 . . ? C19 C20 H20 120.1 . . ? C20 C21 C22 120.5(3) . . ? C20 C21 H21 119.7 . . ? C22 C21 H21 119.7 . . ? C21 C22 C23 119.6(3) . . ? C21 C22 H22 120.2 . . ? C23 C22 H22 120.2 . . ? C18 C23 C22 120.6(3) . . ? C18 C23 H23 119.7 . . ? C22 C23 H23 119.7 . . ? N1 C24 C25 111.4(2) . . ? N1 C24 H24B 109.4 . . ? C25 C24 H24B 109.4 . . ? N1 C24 H24A 109.4 . . ? C25 C24 H24A 109.4 . . ? H24B C24 H24A 108.0 . . ? C26 C25 C24 115.9(3) . . ? C26 C25 H25A 108.3 . . ? C24 C25 H25A 108.3 . . ? C26 C25 H25B 108.3 . . ? C24 C25 H25B 108.3 . . ? H25A C25 H25B 107.4 . . ? N2 C26 C30 120.4(3) . . ? N2 C26 C25 116.0(3) . . ? C30 C26 C25 123.5(3) . . ? N2 C27 C28 124.5(3) . . ? N2 C27 H27 117.7 . . ? C28 C27 H27 117.7 . . ? C29 C28 C27 117.7(3) . . ? C29 C28 H28 121.1 . . ? C27 C28 H28 121.1 . . ? C28 C29 C30 119.4(3) . . ? C28 C29 H29 120.3 . . ? C30 C29 H29 120.3 . . ? C29 C30 C26 120.1(3) . . ? C29 C30 H30 119.9 . . ? C26 C30 H30 119.9 . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 26.58 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.630 _refine_diff_density_min -0.302 _refine_diff_density_rms 0.082 #===END data_jk11abs _database_code_depnum_ccdc_archive 'CCDC 633469' _audit_creation_method SHELXL-97 _chemical_name_systematic ; trans-dichloro[N-{2-(pyrid-2-yl-kappa.N)methyl} 1'-(diphenylphosphino-kappa.P)ferrocenecarboxamide] - acetic acid (1/1) ; _chemical_formula_moiety 'C29 H25 Cl2 Fe N2 O P Pd, C2 H4 O2' _chemical_formula_sum 'C31 H29 Cl2 Fe N2 O3 P Pd' _chemical_formula_weight 741.68 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' Cl Cl 0.1484 0.1585 '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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.343(2) _cell_length_b 10.403(3) _cell_length_c 15.822(5) _cell_angle_alpha 100.40(2) _cell_angle_beta 99.44(2) _cell_angle_gamma 93.87(2) _cell_volume 1484.6(7) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9334 _cell_measurement_theta_min 2.60 _cell_measurement_theta_max 26.50 _exptl_crystal_description red _exptl_crystal_colour plate _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.02 _exptl_crystal_density_diffrn 1.659 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 748 _exptl_absorpt_coefficient_mu 1.364 _exptl_absorpt_correction_T_min 0.759 _exptl_absorpt_correction_T_max 0.959 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.30.2 (release 11-05-2006 CrysAlis171 .NET) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford KM4 CCD diffractometer' _diffrn_measurement_method '\w and \p scans to fill the Ewald sphere' _diffrn_detector_area_resol_mean 8.3438 _diffrn_standards_number 0 _diffrn_reflns_number 20227 _diffrn_reflns_av_R_equivalents 0.0355 _diffrn_reflns_av_sigmaI/netI 0.0672 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.61 _diffrn_reflns_theta_max 26.62 _reflns_number_total 6157 _reflns_number_gt 4185 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.29.5 (release 22-02-2006 CrysAlis171 .NET) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.29.5 (release 22-02-2006 CrysAlis171 .NET) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.29.5 (release 22-02-2006 CrysAlis171 .NET) ; _computing_structure_solution 'SIR-97 (Altomare et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness 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 threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) 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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0218P)^2^+0.0000P] 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 constr _refine_ls_extinction_method none _refine_ls_number_reflns 6157 _refine_ls_number_parameters 372 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0462 _refine_ls_R_factor_gt 0.0253 _refine_ls_wR_factor_ref 0.0490 _refine_ls_wR_factor_gt 0.0475 _refine_ls_goodness_of_fit_ref 0.887 _refine_ls_restrained_S_all 0.887 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_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_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd Pd -0.027180(19) 0.288761(18) 0.320872(12) 0.01567(6) Uani 1 1 d . . . Fe Fe 0.36223(3) 0.46076(3) 0.26640(2) 0.01886(9) Uani 1 1 d . . . P P -0.00253(6) 0.34972(6) 0.19464(4) 0.01548(15) Uani 1 1 d . . . Cl1 Cl -0.09546(6) 0.48915(6) 0.37857(4) 0.02037(14) Uani 1 1 d . . . Cl2 Cl 0.04445(7) 0.08598(6) 0.27015(4) 0.02496(15) Uani 1 1 d . . . O O 0.41486(17) 0.22459(16) 0.41290(11) 0.0267(4) Uani 1 1 d . . . N1 N 0.2302(2) 0.32479(19) 0.46307(12) 0.0179(5) Uani 1 1 d . . . H1N H 0.1962 0.4110 0.4868 0.031(7) Uiso 1 1 d R . . N2 N -0.0723(2) 0.21881(17) 0.43278(12) 0.0159(5) Uani 1 1 d . . . C1 C 0.1830(2) 0.3712(2) 0.17826(15) 0.0170(6) Uani 1 1 d . . . C2 C 0.2883(2) 0.2810(2) 0.19276(15) 0.0215(6) Uani 1 1 d . . . H2 H 0.2735 0.2044 0.2141 0.026 Uiso 1 1 calc R . . C3 C 0.4182(3) 0.3270(3) 0.16944(16) 0.0277(7) Uani 1 1 d . . . H3 H 0.5038 0.2860 0.1723 0.033 Uiso 1 1 calc R . . C4 C 0.3960(3) 0.4471(3) 0.14078(15) 0.0281(7) Uani 1 1 d . . . H4 H 0.4649 0.4987 0.1220 0.034 Uiso 1 1 calc R . . C5 C 0.2512(2) 0.4747(2) 0.14578(15) 0.0220(6) Uani 1 1 d . . . H5 H 0.2079 0.5472 0.1306 0.026 Uiso 1 1 calc R . . C6 C 0.3906(2) 0.4428(2) 0.39428(15) 0.0191(6) Uani 1 1 d . . . C7 C 0.5278(2) 0.4676(3) 0.36852(15) 0.0237(6) Uani 1 1 d . . . H7 H 0.6027 0.4131 0.3696 0.028 Uiso 1 1 calc R . . C8 C 0.5295(3) 0.5898(2) 0.34098(16) 0.0250(6) Uani 1 1 d . . . H8 H 0.6058 0.6297 0.3207 0.030 Uiso 1 1 calc R . . C9 C 0.3951(3) 0.6406(2) 0.34967(16) 0.0248(6) Uani 1 1 d . . . H9 H 0.3675 0.7198 0.3363 0.030 Uiso 1 1 calc R . . C10 C 0.3095(3) 0.5498(2) 0.38234(15) 0.0209(6) Uani 1 1 d . . . H10 H 0.2159 0.5592 0.3939 0.025 Uiso 1 1 calc R . . C11 C 0.3470(2) 0.3221(2) 0.42365(15) 0.0189(6) Uani 1 1 d . . . C12 C -0.0744(2) 0.5009(2) 0.17300(15) 0.0167(5) Uani 1 1 d . . . C13 C -0.0069(3) 0.6214(2) 0.21995(16) 0.0227(6) Uani 1 1 d . . . H13 H 0.0722 0.6239 0.2645 0.027 Uiso 1 1 calc R . . C14 C -0.0549(3) 0.7371(2) 0.20179(17) 0.0287(7) Uani 1 1 d . . . H14 H -0.0074 0.8171 0.2333 0.034 Uiso 1 1 calc R . . C15 C -0.1739(3) 0.7344(3) 0.13649(17) 0.0316(7) Uani 1 1 d . . . H15 H -0.2063 0.8125 0.1237 0.038 Uiso 1 1 calc R . . C16 C -0.2441(3) 0.6158(3) 0.09047(17) 0.0308(7) Uani 1 1 d . . . H16 H -0.3252 0.6141 0.0473 0.037 Uiso 1 1 calc R . . C17 C -0.1951(3) 0.4990(3) 0.10785(16) 0.0239(6) Uani 1 1 d . . . H17 H -0.2428 0.4193 0.0761 0.029 Uiso 1 1 calc R . . C18 C -0.0960(2) 0.2249(2) 0.10357(15) 0.0166(6) Uani 1 1 d . . . C19 C -0.0483(3) 0.2010(3) 0.02490(16) 0.0277(6) Uani 1 1 d . . . H19 H 0.0341 0.2498 0.0174 0.033 Uiso 1 1 calc R . . C20 C -0.1230(3) 0.1040(3) -0.04341(17) 0.0359(7) Uani 1 1 d . . . H20 H -0.0897 0.0874 -0.0962 0.043 Uiso 1 1 calc R . . C21 C -0.2460(3) 0.0329(3) -0.03278(18) 0.0354(7) Uani 1 1 d . . . H21 H -0.2955 -0.0323 -0.0783 0.042 Uiso 1 1 calc R . . C22 C -0.2963(3) 0.0581(2) 0.04538(17) 0.0285(7) Uani 1 1 d . . . H22 H -0.3809 0.0115 0.0521 0.034 Uiso 1 1 calc R . . C23 C -0.2206(2) 0.1525(2) 0.11333(16) 0.0208(6) Uani 1 1 d . . . H23 H -0.2533 0.1679 0.1664 0.025 Uiso 1 1 calc R . . C24 C 0.1841(2) 0.2118(2) 0.49668(16) 0.0232(6) Uani 1 1 d . . . H24A H 0.2383 0.2187 0.5554 0.028 Uiso 1 1 calc R . . H24B H 0.2093 0.1336 0.4609 0.028 Uiso 1 1 calc R . . C25 C 0.0245(3) 0.1950(2) 0.49931(15) 0.0184(6) Uani 1 1 d . . . C26 C -0.2156(3) 0.1945(2) 0.43354(16) 0.0229(6) Uani 1 1 d . . . H26 H -0.2826 0.2110 0.3874 0.027 Uiso 1 1 calc R . . C27 C -0.2672(3) 0.1466(2) 0.49938(16) 0.0240(6) Uani 1 1 d . . . H27 H -0.3669 0.1305 0.4978 0.029 Uiso 1 1 calc R . . C28 C -0.1673(3) 0.1229(2) 0.56802(16) 0.0240(6) Uani 1 1 d . . . H28 H -0.1984 0.0912 0.6140 0.029 Uiso 1 1 calc R . . C29 C -0.0212(3) 0.1470(2) 0.56727(16) 0.0219(6) Uani 1 1 d . . . H29 H 0.0473 0.1308 0.6128 0.026 Uiso 1 1 calc R . . C30 C 0.4843(3) -0.0220(3) 0.2497(2) 0.0413(8) Uani 1 1 d . . . C31 C 0.4791(4) -0.1563(3) 0.1965(2) 0.0707(12) Uani 1 1 d . . . H31A H 0.4971 -0.1500 0.1393 0.106 Uiso 1 1 calc R . . H31B H 0.3846 -0.2023 0.1916 0.106 Uiso 1 1 calc R . . H31C H 0.5522 -0.2032 0.2242 0.106 Uiso 1 1 calc R . . O31 O 0.5396(2) 0.0742(2) 0.23129(15) 0.0571(6) Uani 1 1 d . . . O32 O 0.4184(2) -0.01740(19) 0.31719(14) 0.0496(6) Uani 1 1 d . . . H1O H 0.4374 0.0837 0.3482 0.074 Uiso 1 1 d 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 0.01799(11) 0.01472(11) 0.01381(11) 0.00208(8) 0.00262(8) 0.00058(8) Fe 0.01521(19) 0.0220(2) 0.0170(2) -0.00016(16) 0.00235(15) -0.00255(16) P 0.0162(3) 0.0157(4) 0.0131(4) 0.0009(3) 0.0016(3) -0.0011(3) Cl1 0.0244(3) 0.0168(3) 0.0211(4) 0.0019(3) 0.0090(3) 0.0032(3) Cl2 0.0381(4) 0.0162(3) 0.0207(4) 0.0023(3) 0.0053(3) 0.0065(3) O 0.0248(10) 0.0269(11) 0.0302(11) 0.0057(9) 0.0072(8) 0.0090(9) N1 0.0180(11) 0.0187(12) 0.0160(12) 0.0012(9) 0.0035(9) -0.0008(9) N2 0.0209(11) 0.0115(11) 0.0153(12) 0.0014(9) 0.0044(9) 0.0012(9) C1 0.0167(13) 0.0183(14) 0.0130(14) -0.0014(11) 0.0008(10) -0.0033(11) C2 0.0203(14) 0.0207(14) 0.0193(15) -0.0046(11) 0.0019(11) -0.0021(12) C3 0.0204(14) 0.0347(17) 0.0247(16) -0.0059(13) 0.0069(12) 0.0031(13) C4 0.0219(14) 0.0440(19) 0.0162(15) 0.0016(13) 0.0058(11) -0.0060(13) C5 0.0216(14) 0.0271(15) 0.0168(15) 0.0045(12) 0.0027(11) -0.0012(12) C6 0.0179(13) 0.0224(15) 0.0138(14) -0.0020(11) -0.0007(10) 0.0035(12) C7 0.0157(13) 0.0322(17) 0.0193(15) 0.0013(12) -0.0016(11) -0.0029(12) C8 0.0188(14) 0.0272(16) 0.0237(15) -0.0003(12) 0.0002(11) -0.0114(12) C9 0.0270(15) 0.0213(15) 0.0223(15) -0.0017(12) 0.0018(12) -0.0020(12) C10 0.0192(13) 0.0220(14) 0.0173(14) -0.0039(11) 0.0014(11) -0.0031(12) C11 0.0169(13) 0.0245(15) 0.0104(13) -0.0022(11) -0.0044(10) -0.0002(12) C12 0.0168(13) 0.0194(14) 0.0154(14) 0.0047(11) 0.0062(10) 0.0019(11) C13 0.0250(14) 0.0230(15) 0.0202(15) 0.0058(12) 0.0029(11) 0.0011(12) C14 0.0429(17) 0.0183(15) 0.0254(16) 0.0048(12) 0.0083(13) 0.0005(13) C15 0.0421(17) 0.0262(17) 0.0335(18) 0.0142(14) 0.0141(14) 0.0136(14) C16 0.0310(16) 0.0358(18) 0.0297(17) 0.0159(14) 0.0035(13) 0.0111(14) C17 0.0236(14) 0.0255(16) 0.0227(16) 0.0045(12) 0.0047(12) 0.0021(12) C18 0.0177(13) 0.0155(13) 0.0146(14) 0.0014(11) -0.0011(10) 0.0013(11) C19 0.0279(15) 0.0323(16) 0.0204(16) -0.0012(12) 0.0082(12) -0.0066(13) C20 0.0407(18) 0.0414(19) 0.0193(16) -0.0090(14) 0.0058(13) -0.0030(15) C21 0.0387(17) 0.0282(17) 0.0284(18) -0.0060(13) -0.0081(14) -0.0074(14) C22 0.0244(15) 0.0260(16) 0.0305(18) 0.0062(13) -0.0044(13) -0.0090(13) C23 0.0198(13) 0.0232(15) 0.0181(15) 0.0029(12) 0.0016(11) 0.0006(12) C24 0.0234(14) 0.0261(15) 0.0203(15) 0.0093(12) 0.0001(11) 0.0012(12) C25 0.0255(14) 0.0117(13) 0.0160(14) -0.0006(11) 0.0011(11) 0.0025(11) C26 0.0229(14) 0.0224(15) 0.0243(16) 0.0076(12) 0.0040(11) 0.0017(12) C27 0.0234(14) 0.0227(15) 0.0288(16) 0.0069(12) 0.0107(12) 0.0035(12) C28 0.0369(16) 0.0155(14) 0.0242(16) 0.0060(12) 0.0160(12) 0.0039(12) C29 0.0291(15) 0.0209(14) 0.0156(14) 0.0049(11) 0.0018(11) 0.0043(12) C30 0.0373(18) 0.041(2) 0.055(2) 0.0180(17) 0.0220(16) 0.0128(16) C31 0.122(3) 0.055(2) 0.055(3) 0.021(2) 0.049(2) 0.037(2) O31 0.0570(15) 0.0502(15) 0.0714(17) 0.0235(13) 0.0228(12) -0.0027(12) O32 0.0651(14) 0.0346(13) 0.0578(15) 0.0070(11) 0.0387(12) 0.0028(11) _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 N2 2.124(2) . ? Pd P 2.2433(9) . ? Pd Cl1 2.2956(9) . ? Pd Cl2 2.3017(9) . ? Fe C2 2.027(2) . ? Fe C7 2.033(2) . ? Fe C3 2.038(3) . ? Fe C6 2.041(2) . ? Fe C1 2.042(2) . ? Fe C8 2.044(2) . ? Fe C4 2.045(3) . ? Fe C5 2.052(2) . ? Fe C10 2.052(2) . ? Fe C9 2.056(3) . ? P C1 1.800(2) . ? P C18 1.812(2) . ? P C12 1.817(2) . ? O C11 1.233(3) . ? N1 C11 1.342(3) . ? N1 C24 1.443(3) . ? N1 H1N 1.0012 . ? N2 C25 1.341(3) . ? N2 C26 1.348(3) . ? C1 C2 1.424(3) . ? C1 C5 1.429(3) . ? C2 C3 1.404(3) . ? C2 H2 0.9300 . ? C3 C4 1.421(3) . ? C3 H3 0.9300 . ? C4 C5 1.414(3) . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? C6 C10 1.412(3) . ? C6 C7 1.428(3) . ? C6 C11 1.470(3) . ? C7 C8 1.416(3) . ? C7 H7 0.9300 . ? C8 C9 1.413(3) . ? C8 H8 0.9300 . ? C9 C10 1.417(3) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? C12 C13 1.387(3) . ? C12 C17 1.394(3) . ? C13 C14 1.374(3) . ? C13 H13 0.9300 . ? C14 C15 1.383(3) . ? C14 H14 0.9300 . ? C15 C16 1.375(3) . ? C15 H15 0.9300 . ? C16 C17 1.384(3) . ? C16 H16 0.9300 . ? C17 H17 0.9300 . ? C18 C19 1.376(3) . ? C18 C23 1.389(3) . ? C19 C20 1.391(3) . ? C19 H19 0.9300 . ? C20 C21 1.375(4) . ? C20 H20 0.9300 . ? C21 C22 1.382(4) . ? C21 H21 0.9300 . ? C22 C23 1.377(3) . ? C22 H22 0.9300 . ? C23 H23 0.9300 . ? C24 C25 1.498(3) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 C29 1.380(3) . ? C26 C27 1.374(3) . ? C26 H26 0.9300 . ? C27 C28 1.381(3) . ? C27 H27 0.9300 . ? C28 C29 1.374(3) . ? C28 H28 0.9300 . ? C29 H29 0.9300 . ? C30 O31 1.199(3) . ? C30 O32 1.312(3) . ? C30 C31 1.489(4) . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? O32 H1O 1.0667 . ? 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 N2 Pd P 173.67(5) . . ? N2 Pd Cl1 88.84(6) . . ? P Pd Cl1 92.78(3) . . ? N2 Pd Cl2 88.54(6) . . ? P Pd Cl2 89.96(3) . . ? Cl1 Pd Cl2 177.08(2) . . ? C2 Fe C7 116.63(10) . . ? C2 Fe C3 40.40(9) . . ? C7 Fe C3 103.25(10) . . ? C2 Fe C6 107.48(10) . . ? C7 Fe C6 41.05(9) . . ? C3 Fe C6 123.96(10) . . ? C2 Fe C1 40.98(9) . . ? C7 Fe C1 153.55(10) . . ? C3 Fe C1 68.49(10) . . ? C6 Fe C1 121.63(10) . . ? C2 Fe C8 150.14(10) . . ? C7 Fe C8 40.66(9) . . ? C3 Fe C8 115.62(10) . . ? C6 Fe C8 68.55(10) . . ? C1 Fe C8 165.74(10) . . ? C2 Fe C4 68.32(11) . . ? C7 Fe C4 122.49(10) . . ? C3 Fe C4 40.74(10) . . ? C6 Fe C4 160.68(10) . . ? C1 Fe C4 68.42(10) . . ? C8 Fe C4 105.19(11) . . ? C2 Fe C5 68.59(10) . . ? C7 Fe C5 161.14(10) . . ? C3 Fe C5 68.33(10) . . ? C6 Fe C5 157.49(9) . . ? C1 Fe C5 40.86(9) . . ? C8 Fe C5 126.24(10) . . ? C4 Fe C5 40.39(9) . . ? C2 Fe C10 129.06(10) . . ? C7 Fe C10 68.27(10) . . ? C3 Fe C10 163.20(11) . . ? C6 Fe C10 40.35(9) . . ? C1 Fe C10 112.29(9) . . ? C8 Fe C10 68.06(10) . . ? C4 Fe C10 156.03(11) . . ? C5 Fe C10 124.03(10) . . ? C2 Fe C9 167.78(10) . . ? C7 Fe C9 68.06(10) . . ? C3 Fe C9 151.63(10) . . ? C6 Fe C9 68.04(10) . . ? C1 Fe C9 130.70(10) . . ? C8 Fe C9 40.31(9) . . ? C4 Fe C9 119.77(11) . . ? C5 Fe C9 110.88(10) . . ? C10 Fe C9 40.35(9) . . ? C1 P C18 105.93(11) . . ? C1 P C12 103.10(11) . . ? C18 P C12 104.20(11) . . ? C1 P Pd 114.42(8) . . ? C18 P Pd 109.79(8) . . ? C12 P Pd 118.26(8) . . ? C11 N1 C24 119.4(2) . . ? C11 N1 H1N 119.8 . . ? C24 N1 H1N 117.6 . . ? C25 N2 C26 118.6(2) . . ? C25 N2 Pd 127.33(16) . . ? C26 N2 Pd 114.08(15) . . ? C2 C1 C5 107.3(2) . . ? C2 C1 P 124.58(18) . . ? C5 C1 P 128.07(18) . . ? C2 C1 Fe 68.92(13) . . ? C5 C1 Fe 69.93(13) . . ? P C1 Fe 128.28(13) . . ? C3 C2 C1 108.6(2) . . ? C3 C2 Fe 70.25(14) . . ? C1 C2 Fe 70.10(14) . . ? C3 C2 H2 125.7 . . ? C1 C2 H2 125.7 . . ? Fe C2 H2 125.5 . . ? C2 C3 C4 108.1(2) . . ? C2 C3 Fe 69.35(14) . . ? C4 C3 Fe 69.87(15) . . ? C2 C3 H3 126.0 . . ? C4 C3 H3 126.0 . . ? Fe C3 H3 126.4 . . ? C5 C4 C3 108.2(2) . . ? C5 C4 Fe 70.08(14) . . ? C3 C4 Fe 69.39(15) . . ? C5 C4 H4 125.9 . . ? C3 C4 H4 125.9 . . ? Fe C4 H4 126.2 . . ? C4 C5 C1 107.8(2) . . ? C4 C5 Fe 69.53(14) . . ? C1 C5 Fe 69.21(13) . . ? C4 C5 H5 126.1 . . ? C1 C5 H5 126.1 . . ? Fe C5 H5 126.7 . . ? C10 C6 C7 107.6(2) . . ? C10 C6 C11 128.8(2) . . ? C7 C6 C11 123.5(2) . . ? C10 C6 Fe 70.25(14) . . ? C7 C6 Fe 69.16(14) . . ? C11 C6 Fe 123.90(16) . . ? C8 C7 C6 107.9(2) . . ? C8 C7 Fe 70.10(14) . . ? C6 C7 Fe 69.79(13) . . ? C8 C7 H7 126.0 . . ? C6 C7 H7 126.0 . . ? Fe C7 H7 125.7 . . ? C9 C8 C7 108.0(2) . . ? C9 C8 Fe 70.31(14) . . ? C7 C8 Fe 69.24(13) . . ? C9 C8 H8 126.0 . . ? C7 C8 H8 126.0 . . ? Fe C8 H8 126.0 . . ? C8 C9 C10 108.2(2) . . ? C8 C9 Fe 69.38(14) . . ? C10 C9 Fe 69.66(14) . . ? C8 C9 H9 125.9 . . ? C10 C9 H9 125.9 . . ? Fe C9 H9 126.6 . . ? C6 C10 C9 108.3(2) . . ? C6 C10 Fe 69.41(14) . . ? C9 C10 Fe 69.99(14) . . ? C6 C10 H10 125.9 . . ? C9 C10 H10 125.9 . . ? Fe C10 H10 126.3 . . ? O C11 N1 122.2(2) . . ? O C11 C6 121.6(2) . . ? N1 C11 C6 116.2(2) . . ? C13 C12 C17 118.6(2) . . ? C13 C12 P 120.19(17) . . ? C17 C12 P 121.20(18) . . ? C14 C13 C12 121.2(2) . . ? C14 C13 H13 119.4 . . ? C12 C13 H13 119.4 . . ? C13 C14 C15 119.8(2) . . ? C13 C14 H14 120.1 . . ? C15 C14 H14 120.1 . . ? C16 C15 C14 119.8(2) . . ? C16 C15 H15 120.1 . . ? C14 C15 H15 120.1 . . ? C15 C16 C17 120.6(2) . . ? C15 C16 H16 119.7 . . ? C17 C16 H16 119.7 . . ? C16 C17 C12 120.0(2) . . ? C16 C17 H17 120.0 . . ? C12 C17 H17 120.0 . . ? C19 C18 C23 119.2(2) . . ? C19 C18 P 122.03(19) . . ? C23 C18 P 118.81(18) . . ? C18 C19 C20 120.3(2) . . ? C18 C19 H19 119.9 . . ? C20 C19 H19 119.9 . . ? C21 C20 C19 119.9(3) . . ? C21 C20 H20 120.0 . . ? C19 C20 H20 120.0 . . ? C20 C21 C22 120.2(2) . . ? C20 C21 H21 119.9 . . ? C22 C21 H21 119.9 . . ? C23 C22 C21 119.7(2) . . ? C23 C22 H22 120.2 . . ? C21 C22 H22 120.2 . . ? C22 C23 C18 120.7(2) . . ? C22 C23 H23 119.6 . . ? C18 C23 H23 119.6 . . ? N1 C24 C25 114.73(19) . . ? N1 C24 H24A 108.6 . . ? C25 C24 H24A 108.6 . . ? N1 C24 H24B 108.6 . . ? C25 C24 H24B 108.6 . . ? H24A C24 H24B 107.6 . . ? N2 C25 C29 120.9(2) . . ? N2 C25 C24 119.5(2) . . ? C29 C25 C24 119.5(2) . . ? N2 C26 C27 123.0(2) . . ? N2 C26 H26 118.5 . . ? C27 C26 H26 118.5 . . ? C26 C27 C28 118.3(2) . . ? C26 C27 H27 120.9 . . ? C28 C27 H27 120.9 . . ? C29 C28 C27 118.9(2) . . ? C29 C28 H28 120.6 . . ? C27 C28 H28 120.6 . . ? C28 C29 C25 120.4(2) . . ? C28 C29 H29 119.8 . . ? C25 C29 H29 119.8 . . ? O31 C30 O32 122.8(3) . . ? O31 C30 C31 123.2(3) . . ? O32 C30 C31 114.0(3) . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C30 O32 H1O 103.2 . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 26.62 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.780 _refine_diff_density_min -0.362 _refine_diff_density_rms 0.071 _chemical_name_common ; trans-dichloro(N-(2-(pyrid-2-yl-kappa.N)methyl) 1'- (diphenylphosphino-kappa.P)ferrocenecarboxamide) -acetic acid (1/1) ; #===END data_jk12c _database_code_depnum_ccdc_archive 'CCDC 633470' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C60 H54 Cl4 Fe2 N4 O2 P2 Pd2, 8(C H Cl3)' _chemical_formula_sum 'C68 H62 Cl28 Fe2 N4 O2 P2 Pd2' _chemical_formula_weight 2346.26 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' Cl Cl 0.1484 0.1585 '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 monoclinic _symmetry_space_group_name_H-M P21/c 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' _cell_length_a 12.541(1) _cell_length_b 17.300(3) _cell_length_c 21.570(4) _cell_angle_alpha 90.00 _cell_angle_beta 101.99(1) _cell_angle_gamma 90.00 _cell_volume 4578(1) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 19728 _cell_measurement_theta_min 2.54 _cell_measurement_theta_max 26.50 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.702 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2328 _exptl_absorpt_coefficient_mu 1.593 _exptl_absorpt_correction_T_min 0.636 _exptl_absorpt_correction_T_max 0.725 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.30.2 (release 11-05-2006 CrysAlis171 .NET) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford KM4 CCD diffractometer' _diffrn_measurement_method '\w and \p scans to fill the Ewald sphere' _diffrn_detector_area_resol_mean 8.3438 _diffrn_standards_number 0 _diffrn_reflns_number 60436 _diffrn_reflns_av_R_equivalents 0.0489 _diffrn_reflns_av_sigmaI/netI 0.0782 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.54 _diffrn_reflns_theta_max 26.59 _reflns_number_total 9544 _reflns_number_gt 5832 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.29.5 (release 22-02-2006 CrysAlis171 .NET) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.29.5 (release 22-02-2006 CrysAlis171 .NET) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.29.5 (release 22-02-2006 CrysAlis171 .NET) ; _computing_structure_solution 'SIR-97 (Altomare et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness 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 threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) 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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0675P)^2^+0.0000P] 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 constr _refine_ls_extinction_method none _refine_ls_number_reflns 9544 _refine_ls_number_parameters 488 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0795 _refine_ls_R_factor_gt 0.0435 _refine_ls_wR_factor_ref 0.1308 _refine_ls_wR_factor_gt 0.1252 _refine_ls_goodness_of_fit_ref 1.064 _refine_ls_restrained_S_all 1.064 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_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_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd Pd 0.76089(3) 0.05241(2) 0.008169(17) 0.02180(11) Uani 1 1 d . . . Cl1 Cl 0.92442(10) 0.08208(7) 0.07429(6) 0.0302(3) Uani 1 1 d . . . Cl2 Cl 0.61039(10) 0.00549(7) -0.06104(6) 0.0349(3) Uani 1 1 d . . . Fe Fe 0.43228(5) -0.25177(4) -0.00415(3) 0.02205(17) Uani 1 1 d . . . P P 0.24002(10) -0.15446(7) 0.05611(6) 0.0214(3) Uani 1 1 d . . . N1 N 0.7074(3) -0.1868(2) -0.04948(19) 0.0277(10) Uani 1 1 d . . . H1N H 0.6723 -0.1356 -0.0665 0.039(14) Uiso 1 1 d R . . N2 N 0.7564(3) -0.0429(2) 0.06838(18) 0.0245(9) Uani 1 1 d . . . O O 0.6975(3) -0.31528(18) -0.03186(17) 0.0321(8) Uani 1 1 d . . . C1 C 0.3593(4) -0.2143(3) 0.0667(2) 0.0226(11) Uani 1 1 d . . . C2 C 0.4714(4) -0.1902(3) 0.0777(2) 0.0255(11) Uani 1 1 d . . . H2 H 0.4964 -0.1394 0.0814 0.031 Uiso 1 1 calc R . . C3 C 0.5368(4) -0.2572(3) 0.0820(2) 0.0276(12) Uani 1 1 d . . . H3 H 0.6125 -0.2580 0.0893 0.033 Uiso 1 1 calc R . . C4 C 0.4680(4) -0.3230(3) 0.0733(2) 0.0325(13) Uani 1 1 d . . . H4 H 0.4907 -0.3742 0.0735 0.039 Uiso 1 1 calc R . . C5 C 0.3578(4) -0.2971(3) 0.0641(2) 0.0283(12) Uani 1 1 d . . . H5 H 0.2961 -0.3283 0.0576 0.034 Uiso 1 1 calc R . . C6 C 0.5306(4) -0.2474(3) -0.0674(2) 0.0249(11) Uani 1 1 d . . . C7 C 0.4630(4) -0.3141(3) -0.0786(2) 0.0278(12) Uani 1 1 d . . . H7 H 0.4863 -0.3653 -0.0771 0.033 Uiso 1 1 calc R . . C8 C 0.3533(4) -0.2880(3) -0.0924(2) 0.0282(12) Uani 1 1 d . . . H8 H 0.2917 -0.3193 -0.1018 0.034 Uiso 1 1 calc R . . C9 C 0.3534(4) -0.2064(3) -0.0894(2) 0.0279(12) Uani 1 1 d . . . H9 H 0.2922 -0.1747 -0.0963 0.034 Uiso 1 1 calc R . . C10 C 0.4632(4) -0.1817(3) -0.0740(2) 0.0257(11) Uani 1 1 d . . . H10 H 0.4867 -0.1307 -0.0690 0.031 Uiso 1 1 calc R . . C11 C 0.6524(4) -0.2535(3) -0.0481(2) 0.0246(11) Uani 1 1 d . . . C12 C 0.2286(4) -0.1205(3) 0.1334(2) 0.0254(11) Uani 1 1 d . . . C13 C 0.1418(4) -0.0709(3) 0.1378(3) 0.0389(14) Uani 1 1 d . . . H13 H 0.0931 -0.0556 0.1012 0.047 Uiso 1 1 calc R . . C14 C 0.1287(5) -0.0448(3) 0.1962(3) 0.0478(16) Uani 1 1 d . . . H14 H 0.0705 -0.0126 0.1990 0.057 Uiso 1 1 calc R . . C15 C 0.2007(6) -0.0661(4) 0.2497(3) 0.0580(19) Uani 1 1 d . . . H15 H 0.1914 -0.0484 0.2889 0.070 Uiso 1 1 calc R . . C16 C 0.2890(6) -0.1145(4) 0.2462(3) 0.0542(17) Uani 1 1 d . . . H16 H 0.3390 -0.1281 0.2828 0.065 Uiso 1 1 calc R . . C17 C 0.3009(4) -0.1419(3) 0.1878(2) 0.0361(13) Uani 1 1 d . . . H17 H 0.3581 -0.1751 0.1852 0.043 Uiso 1 1 calc R . . C18 C 0.1346(3) -0.2282(3) 0.0353(2) 0.0212(10) Uani 1 1 d . . . C19 C 0.1116(4) -0.2580(3) -0.0261(2) 0.0272(11) Uani 1 1 d . . . H19 H 0.1426 -0.2353 -0.0572 0.033 Uiso 1 1 calc R . . C20 C 0.0431(4) -0.3209(3) -0.0413(2) 0.0297(12) Uani 1 1 d . . . H20 H 0.0275 -0.3399 -0.0825 0.036 Uiso 1 1 calc R . . C21 C -0.0018(4) -0.3551(3) 0.0049(3) 0.0377(14) Uani 1 1 d . . . H21 H -0.0475 -0.3977 -0.0050 0.045 Uiso 1 1 calc R . . C22 C 0.0211(4) -0.3260(3) 0.0661(3) 0.0326(13) Uani 1 1 d . . . H22 H -0.0089 -0.3493 0.0973 0.039 Uiso 1 1 calc R . . C23 C 0.0876(4) -0.2632(3) 0.0808(2) 0.0273(11) Uani 1 1 d . . . H23 H 0.1015 -0.2437 0.1218 0.033 Uiso 1 1 calc R . . C24 C 0.8265(4) -0.1858(3) -0.0314(3) 0.0320(12) Uani 1 1 d . . . H24A H 0.8570 -0.1849 -0.0692 0.038 Uiso 1 1 calc R . . H24B H 0.8518 -0.2323 -0.0078 0.038 Uiso 1 1 calc R . . C25 C 0.8652(4) -0.1153(3) 0.0091(2) 0.0274(12) Uani 1 1 d . . . H25A H 0.9435 -0.1187 0.0239 0.033 Uiso 1 1 calc R . . H25B H 0.8501 -0.0694 -0.0171 0.033 Uiso 1 1 calc R . . C26 C 0.8138(4) -0.1062(3) 0.0648(2) 0.0264(11) Uani 1 1 d . . . C27 C 0.7038(4) -0.0336(3) 0.1168(2) 0.0334(13) Uani 1 1 d . . . H27 H 0.6636 0.0112 0.1184 0.040 Uiso 1 1 calc R . . C28 C 0.7077(4) -0.0876(3) 0.1629(2) 0.0372(13) Uani 1 1 d . . . H28 H 0.6686 -0.0809 0.1947 0.045 Uiso 1 1 calc R . . C29 C 0.7712(5) -0.1526(3) 0.1616(3) 0.0423(14) Uani 1 1 d . . . H29 H 0.7797 -0.1888 0.1942 0.051 Uiso 1 1 calc R . . C30 C 0.8212(4) -0.1628(3) 0.1118(3) 0.0383(14) Uani 1 1 d . . . H30 H 0.8605 -0.2078 0.1090 0.046 Uiso 1 1 calc R . . C60 C -0.2702(5) -0.4361(3) -0.1284(3) 0.0464(15) Uani 1 1 d . . . H60 H -0.2827 -0.4079 -0.0912 0.056 Uiso 1 1 calc R . . Cl61 Cl -0.19411(16) -0.51840(10) -0.10198(10) 0.0771(6) Uani 1 1 d . . . Cl62 Cl -0.19658(18) -0.37607(14) -0.16953(9) 0.0991(8) Uani 1 1 d . . . Cl63 Cl -0.39585(14) -0.45794(11) -0.17559(9) 0.0674(5) Uani 1 1 d . . . C70 C -0.2503(5) -0.4451(3) 0.0686(3) 0.0479(15) Uani 1 1 d . . . H70 H -0.2418 -0.4060 0.0371 0.058 Uiso 1 1 calc R . . Cl71 Cl -0.13548(14) -0.50330(9) 0.08180(9) 0.0623(5) Uani 1 1 d . . . Cl72 Cl -0.36630(16) -0.49905(11) 0.03781(13) 0.0973(8) Uani 1 1 d . . . Cl73 Cl -0.25680(19) -0.39716(13) 0.13890(9) 0.0935(8) Uani 1 1 d . . . C80 C 0.0228(5) -0.3216(4) 0.2880(3) 0.0587(18) Uani 1 1 d . . . H80 H 0.0594 -0.3357 0.3311 0.070 Uiso 1 1 calc R . . Cl81 Cl 0.05707(18) -0.39038(12) 0.23623(10) 0.0834(6) Uani 1 1 d . . . Cl82 Cl 0.0684(2) -0.22999(13) 0.27170(11) 0.1015(8) Uani 1 1 d . . . Cl83 Cl -0.11876(16) -0.31963(11) 0.28502(9) 0.0734(5) Uani 1 1 d . . . C90 C 0.5075(6) -0.3449(4) 0.2417(3) 0.065(2) Uani 1 1 d . . . H90 H 0.5109 -0.3553 0.1975 0.078 Uiso 1 1 calc R . . Cl91 Cl 0.57556(18) -0.41916(12) 0.28910(10) 0.0912(7) Uani 1 1 d . . . Cl92 Cl 0.57127(17) -0.25640(12) 0.26385(9) 0.0811(6) Uani 1 1 d . . . Cl93 Cl 0.37059(16) -0.34172(11) 0.24762(9) 0.0729(5) Uani 1 1 d . . . 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 0.0231(2) 0.01832(19) 0.0241(2) 0.00126(17) 0.00512(15) 0.00116(16) Cl1 0.0279(6) 0.0280(7) 0.0317(7) 0.0007(5) -0.0008(6) -0.0001(5) Cl2 0.0324(7) 0.0246(7) 0.0422(8) 0.0030(6) -0.0053(6) -0.0052(5) Fe 0.0231(4) 0.0195(4) 0.0243(4) -0.0003(3) 0.0067(3) 0.0011(3) P 0.0223(6) 0.0186(6) 0.0240(7) 0.0001(5) 0.0062(6) 0.0014(5) N1 0.019(2) 0.024(2) 0.041(3) 0.007(2) 0.0080(19) 0.0050(18) N2 0.021(2) 0.024(2) 0.030(2) 0.0031(18) 0.0079(18) -0.0025(17) O 0.0343(19) 0.0173(18) 0.045(2) 0.0028(16) 0.0091(17) 0.0062(16) C1 0.026(3) 0.022(3) 0.021(3) 0.001(2) 0.007(2) 0.001(2) C2 0.026(3) 0.027(3) 0.023(3) -0.006(2) 0.005(2) -0.001(2) C3 0.022(3) 0.034(3) 0.026(3) 0.003(2) 0.004(2) 0.005(2) C4 0.036(3) 0.034(3) 0.028(3) 0.007(2) 0.009(2) 0.011(2) C5 0.032(3) 0.027(3) 0.027(3) 0.006(2) 0.009(2) 0.006(2) C6 0.031(3) 0.021(3) 0.025(3) -0.001(2) 0.013(2) 0.001(2) C7 0.030(3) 0.027(3) 0.029(3) -0.010(2) 0.013(2) -0.001(2) C8 0.027(3) 0.031(3) 0.028(3) -0.007(2) 0.008(2) -0.006(2) C9 0.033(3) 0.029(3) 0.021(3) 0.002(2) 0.003(2) 0.002(2) C10 0.027(3) 0.026(3) 0.024(3) 0.002(2) 0.007(2) -0.002(2) C11 0.029(3) 0.026(3) 0.019(3) -0.004(2) 0.006(2) 0.003(2) C12 0.034(3) 0.019(3) 0.026(3) -0.006(2) 0.011(2) -0.006(2) C13 0.046(3) 0.027(3) 0.045(4) 0.000(3) 0.013(3) 0.003(3) C14 0.061(4) 0.037(4) 0.055(4) -0.012(3) 0.035(4) 0.002(3) C15 0.096(6) 0.046(4) 0.044(4) -0.018(3) 0.044(4) -0.020(4) C16 0.078(5) 0.058(4) 0.027(3) 0.001(3) 0.011(3) -0.015(4) C17 0.044(3) 0.038(3) 0.028(3) 0.001(3) 0.011(3) -0.006(3) C18 0.019(2) 0.018(2) 0.027(3) 0.005(2) 0.006(2) 0.0020(19) C19 0.025(3) 0.025(3) 0.032(3) -0.001(2) 0.007(2) -0.001(2) C20 0.029(3) 0.023(3) 0.035(3) -0.004(2) 0.003(2) 0.002(2) C21 0.035(3) 0.021(3) 0.057(4) -0.007(3) 0.009(3) -0.002(2) C22 0.026(3) 0.027(3) 0.047(4) 0.006(3) 0.012(3) -0.001(2) C23 0.027(3) 0.024(3) 0.029(3) 0.002(2) 0.003(2) 0.007(2) C24 0.028(3) 0.030(3) 0.043(3) 0.003(3) 0.016(3) 0.007(2) C25 0.015(2) 0.022(3) 0.045(3) 0.006(2) 0.006(2) 0.003(2) C26 0.024(3) 0.021(3) 0.030(3) 0.004(2) -0.003(2) -0.003(2) C27 0.038(3) 0.036(3) 0.028(3) 0.000(2) 0.012(3) 0.006(2) C28 0.045(3) 0.039(3) 0.032(3) 0.002(3) 0.018(3) -0.001(3) C29 0.054(4) 0.038(3) 0.033(3) 0.016(3) 0.006(3) -0.002(3) C30 0.041(3) 0.029(3) 0.044(4) 0.010(3) 0.006(3) 0.008(2) C60 0.069(4) 0.032(3) 0.037(3) -0.003(3) 0.007(3) -0.001(3) Cl61 0.0842(13) 0.0461(10) 0.0947(15) 0.0022(10) 0.0042(11) 0.0125(9) Cl62 0.1038(16) 0.1202(19) 0.0586(12) 0.0310(12) -0.0169(11) -0.0590(14) Cl63 0.0583(10) 0.0698(12) 0.0722(12) -0.0148(10) 0.0093(9) 0.0005(9) C70 0.066(4) 0.026(3) 0.049(4) 0.003(3) 0.005(3) -0.001(3) Cl71 0.0642(11) 0.0484(10) 0.0833(13) 0.0147(9) 0.0360(10) 0.0117(8) Cl72 0.0611(12) 0.0476(11) 0.178(3) -0.0102(13) 0.0135(14) -0.0136(9) Cl73 0.1224(18) 0.0966(16) 0.0549(11) -0.0070(11) 0.0032(11) 0.0708(14) C80 0.076(5) 0.051(4) 0.044(4) 0.016(3) 0.002(4) -0.016(3) Cl81 0.1063(16) 0.0819(14) 0.0719(13) 0.0064(11) 0.0409(12) 0.0055(12) Cl82 0.141(2) 0.0796(15) 0.0838(15) 0.0091(12) 0.0229(15) -0.0557(14) Cl83 0.0747(12) 0.0667(12) 0.0759(13) 0.0125(10) 0.0087(10) 0.0037(10) C90 0.095(6) 0.069(5) 0.030(4) 0.000(3) 0.011(4) 0.014(4) Cl91 0.1113(16) 0.0619(12) 0.0817(14) -0.0008(11) -0.0232(12) 0.0292(12) Cl92 0.0982(15) 0.0707(13) 0.0688(13) 0.0116(10) 0.0045(11) -0.0136(11) Cl93 0.0816(13) 0.0678(12) 0.0704(13) -0.0013(10) 0.0184(11) 0.0082(10) _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 N2 2.107(4) . ? Pd P 2.2434(13) 3_655 ? Pd Cl2 2.2978(13) . ? Pd Cl1 2.2996(13) . ? Fe C6 2.022(4) . ? Fe C10 2.032(5) . ? Fe C2 2.034(5) . ? Fe C7 2.036(5) . ? Fe C3 2.041(5) . ? Fe C1 2.043(4) . ? Fe C4 2.050(5) . ? Fe C8 2.052(5) . ? Fe C9 2.053(5) . ? Fe C5 2.056(5) . ? P C1 1.794(5) . ? P C12 1.801(5) . ? P C18 1.824(5) . ? P Pd 2.2434(13) 3_655 ? N1 C11 1.347(6) . ? N1 C24 1.463(6) . ? N1 H1N 1.0225 . ? N2 C26 1.322(6) . ? N2 C27 1.355(6) . ? O C11 1.227(5) . ? C1 C5 1.434(7) . ? C1 C2 1.438(6) . ? C2 C3 1.411(6) . ? C2 H2 0.9300 . ? C3 C4 1.418(7) . ? C3 H3 0.9300 . ? C4 C5 1.427(7) . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? C6 C10 1.405(6) . ? C6 C7 1.424(7) . ? C6 C11 1.501(7) . ? C7 C8 1.420(7) . ? C7 H7 0.9300 . ? C8 C9 1.413(7) . ? C8 H8 0.9300 . ? C9 C10 1.413(6) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? C12 C17 1.375(7) . ? C12 C13 1.405(7) . ? C13 C14 1.380(7) . ? C13 H13 0.9300 . ? C14 C15 1.361(9) . ? C14 H14 0.9300 . ? C15 C16 1.403(9) . ? C15 H15 0.9300 . ? C16 C17 1.384(7) . ? C16 H16 0.9300 . ? C17 H17 0.9300 . ? C18 C23 1.384(6) . ? C18 C19 1.394(7) . ? C19 C20 1.382(7) . ? C19 H19 0.9300 . ? C20 C21 1.376(7) . ? C20 H20 0.9300 . ? C21 C22 1.386(7) . ? C21 H21 0.9300 . ? C22 C23 1.366(7) . ? C22 H22 0.9300 . ? C23 H23 0.9300 . ? C24 C25 1.520(7) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 C26 1.484(7) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 C30 1.399(7) . ? C27 C28 1.358(7) . ? C27 H27 0.9300 . ? C28 C29 1.382(7) . ? C28 H28 0.9300 . ? C29 C30 1.363(7) . ? C29 H29 0.9300 . ? C30 H30 0.9300 . ? C60 Cl63 1.731(6) . ? C60 Cl61 1.742(6) . ? C60 Cl62 1.749(6) . ? C60 H60 0.9800 . ? C70 Cl71 1.732(6) . ? C70 Cl72 1.740(6) . ? C70 Cl73 1.744(6) . ? C70 H70 0.9800 . ? C80 Cl82 1.745(6) . ? C80 Cl81 1.745(7) . ? C80 Cl83 1.764(7) . ? C80 H80 0.9800 . ? C90 Cl92 1.747(7) . ? C90 Cl93 1.749(7) . ? C90 Cl91 1.750(7) . ? C90 H90 0.9800 . ? 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 N2 Pd P 178.19(10) . 3_655 ? N2 Pd Cl2 90.04(11) . . ? P Pd Cl2 88.76(5) 3_655 . ? N2 Pd Cl1 85.80(11) . . ? P Pd Cl1 95.57(5) 3_655 . ? Cl2 Pd Cl1 171.19(5) . . ? C6 Fe C10 40.57(18) . . ? C6 Fe C2 119.69(19) . . ? C10 Fe C2 106.4(2) . . ? C6 Fe C7 41.08(18) . . ? C10 Fe C7 68.61(19) . . ? C2 Fe C7 155.68(18) . . ? C6 Fe C3 104.47(19) . . ? C10 Fe C3 121.12(19) . . ? C2 Fe C3 40.52(18) . . ? C7 Fe C3 120.17(19) . . ? C6 Fe C1 157.45(19) . . ? C10 Fe C1 123.30(19) . . ? C2 Fe C1 41.31(18) . . ? C7 Fe C1 160.97(19) . . ? C3 Fe C1 68.67(18) . . ? C6 Fe C4 120.81(19) . . ? C10 Fe C4 156.91(19) . . ? C2 Fe C4 68.6(2) . . ? C7 Fe C4 106.2(2) . . ? C3 Fe C4 40.57(19) . . ? C1 Fe C4 68.74(19) . . ? C6 Fe C8 68.32(19) . . ? C10 Fe C8 67.95(19) . . ? C2 Fe C8 161.47(19) . . ? C7 Fe C8 40.65(18) . . ? C3 Fe C8 157.7(2) . . ? C1 Fe C8 125.83(19) . . ? C4 Fe C8 123.6(2) . . ? C6 Fe C9 68.26(19) . . ? C10 Fe C9 40.48(18) . . ? C2 Fe C9 124.2(2) . . ? C7 Fe C9 68.4(2) . . ? C3 Fe C9 158.6(2) . . ? C1 Fe C9 109.92(19) . . ? C4 Fe C9 160.5(2) . . ? C8 Fe C9 40.25(19) . . ? C6 Fe C5 158.33(19) . . ? C10 Fe C5 160.60(19) . . ? C2 Fe C5 68.98(19) . . ? C7 Fe C5 123.4(2) . . ? C3 Fe C5 68.39(19) . . ? C1 Fe C5 40.95(18) . . ? C4 Fe C5 40.67(18) . . ? C8 Fe C5 110.1(2) . . ? C9 Fe C5 125.50(19) . . ? C1 P C12 107.2(2) . . ? C1 P C18 99.8(2) . . ? C12 P C18 105.2(2) . . ? C1 P Pd 115.43(15) . 3_655 ? C12 P Pd 108.91(16) . 3_655 ? C18 P Pd 119.18(15) . 3_655 ? C11 N1 C24 120.2(4) . . ? C11 N1 H1N 124.4 . . ? C24 N1 H1N 115.1 . . ? C26 N2 C27 120.1(4) . . ? C26 N2 Pd 121.8(3) . . ? C27 N2 Pd 117.5(3) . . ? C5 C1 C2 107.5(4) . . ? C5 C1 P 124.6(4) . . ? C2 C1 P 127.9(4) . . ? C5 C1 Fe 70.0(3) . . ? C2 C1 Fe 69.0(3) . . ? P C1 Fe 125.4(2) . . ? C3 C2 C1 107.9(4) . . ? C3 C2 Fe 70.0(3) . . ? C1 C2 Fe 69.7(3) . . ? C3 C2 H2 126.1 . . ? C1 C2 H2 126.1 . . ? Fe C2 H2 125.8 . . ? C2 C3 C4 108.8(4) . . ? C2 C3 Fe 69.4(3) . . ? C4 C3 Fe 70.0(3) . . ? C2 C3 H3 125.6 . . ? C4 C3 H3 125.6 . . ? Fe C3 H3 126.5 . . ? C3 C4 C5 108.1(4) . . ? C3 C4 Fe 69.4(3) . . ? C5 C4 Fe 69.9(3) . . ? C3 C4 H4 126.0 . . ? C5 C4 H4 126.0 . . ? Fe C4 H4 126.3 . . ? C4 C5 C1 107.7(4) . . ? C4 C5 Fe 69.4(3) . . ? C1 C5 Fe 69.0(3) . . ? C4 C5 H5 126.1 . . ? C1 C5 H5 126.1 . . ? Fe C5 H5 127.0 . . ? C10 C6 C7 108.3(4) . . ? C10 C6 C11 129.9(4) . . ? C7 C6 C11 121.7(4) . . ? C10 C6 Fe 70.1(3) . . ? C7 C6 Fe 70.0(3) . . ? C11 C6 Fe 122.6(3) . . ? C8 C7 C6 107.1(4) . . ? C8 C7 Fe 70.3(3) . . ? C6 C7 Fe 68.9(3) . . ? C8 C7 H7 126.4 . . ? C6 C7 H7 126.4 . . ? Fe C7 H7 125.9 . . ? C9 C8 C7 108.5(4) . . ? C9 C8 Fe 69.9(3) . . ? C7 C8 Fe 69.1(3) . . ? C9 C8 H8 125.8 . . ? C7 C8 H8 125.8 . . ? Fe C8 H8 126.8 . . ? C8 C9 C10 107.7(4) . . ? C8 C9 Fe 69.8(3) . . ? C10 C9 Fe 68.9(3) . . ? C8 C9 H9 126.1 . . ? C10 C9 H9 126.1 . . ? Fe C9 H9 126.7 . . ? C6 C10 C9 108.4(4) . . ? C6 C10 Fe 69.3(3) . . ? C9 C10 Fe 70.6(3) . . ? C6 C10 H10 125.8 . . ? C9 C10 H10 125.8 . . ? Fe C10 H10 125.9 . . ? O C11 N1 123.0(4) . . ? O C11 C6 121.5(4) . . ? N1 C11 C6 115.5(4) . . ? C17 C12 C13 119.3(5) . . ? C17 C12 P 122.4(4) . . ? C13 C12 P 118.2(4) . . ? C14 C13 C12 120.2(5) . . ? C14 C13 H13 119.9 . . ? C12 C13 H13 119.9 . . ? C15 C14 C13 120.1(6) . . ? C15 C14 H14 120.0 . . ? C13 C14 H14 120.0 . . ? C14 C15 C16 120.6(5) . . ? C14 C15 H15 119.7 . . ? C16 C15 H15 119.7 . . ? C17 C16 C15 119.2(6) . . ? C17 C16 H16 120.4 . . ? C15 C16 H16 120.4 . . ? C12 C17 C16 120.6(5) . . ? C12 C17 H17 119.7 . . ? C16 C17 H17 119.7 . . ? C23 C18 C19 118.4(4) . . ? C23 C18 P 121.7(4) . . ? C19 C18 P 119.3(3) . . ? C20 C19 C18 120.8(5) . . ? C20 C19 H19 119.6 . . ? C18 C19 H19 119.6 . . ? C21 C20 C19 119.7(5) . . ? C21 C20 H20 120.2 . . ? C19 C20 H20 120.2 . . ? C20 C21 C22 119.8(5) . . ? C20 C21 H21 120.1 . . ? C22 C21 H21 120.1 . . ? C23 C22 C21 120.4(5) . . ? C23 C22 H22 119.8 . . ? C21 C22 H22 119.8 . . ? C22 C23 C18 120.8(5) . . ? C22 C23 H23 119.6 . . ? C18 C23 H23 119.6 . . ? N1 C24 C25 110.4(4) . . ? N1 C24 H24A 109.6 . . ? C25 C24 H24A 109.6 . . ? N1 C24 H24B 109.6 . . ? C25 C24 H24B 109.6 . . ? H24A C24 H24B 108.1 . . ? C26 C25 C24 114.2(4) . . ? C26 C25 H25A 108.7 . . ? C24 C25 H25A 108.7 . . ? C26 C25 H25B 108.7 . . ? C24 C25 H25B 108.7 . . ? H25A C25 H25B 107.6 . . ? N2 C26 C30 119.5(5) . . ? N2 C26 C25 117.9(4) . . ? C30 C26 C25 122.6(5) . . ? N2 C27 C28 122.3(5) . . ? N2 C27 H27 118.9 . . ? C28 C27 H27 118.9 . . ? C27 C28 C29 118.5(5) . . ? C27 C28 H28 120.7 . . ? C29 C28 H28 120.7 . . ? C30 C29 C28 118.9(5) . . ? C30 C29 H29 120.6 . . ? C28 C29 H29 120.6 . . ? C29 C30 C26 120.6(5) . . ? C29 C30 H30 119.7 . . ? C26 C30 H30 119.7 . . ? Cl63 C60 Cl61 112.6(3) . . ? Cl63 C60 Cl62 110.1(3) . . ? Cl61 C60 Cl62 109.9(3) . . ? Cl63 C60 H60 108.0 . . ? Cl61 C60 H60 108.0 . . ? Cl62 C60 H60 108.0 . . ? Cl71 C70 Cl72 110.5(3) . . ? Cl71 C70 Cl73 108.7(3) . . ? Cl72 C70 Cl73 113.7(4) . . ? Cl71 C70 H70 107.9 . . ? Cl72 C70 H70 107.9 . . ? Cl73 C70 H70 107.9 . . ? Cl82 C80 Cl81 110.9(4) . . ? Cl82 C80 Cl83 110.2(4) . . ? Cl81 C80 Cl83 111.7(4) . . ? Cl82 C80 H80 108.0 . . ? Cl81 C80 H80 108.0 . . ? Cl83 C80 H80 108.0 . . ? Cl92 C90 Cl93 110.7(4) . . ? Cl92 C90 Cl91 110.1(4) . . ? Cl93 C90 Cl91 110.3(4) . . ? Cl92 C90 H90 108.5 . . ? Cl93 C90 H90 108.5 . . ? Cl91 C90 H90 108.5 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 26.59 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.745 _refine_diff_density_min -1.283 _refine_diff_density_rms 0.098 #===END