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 'Prof. Evamarie Hey-Hawkins' _publ_contact_author_address ;Institut fur Anorganische Chemie der Universitat Leipzig Johannisallee 29 D-04103 Leipzig Germany ; _publ_contact_author_email hey@rz.uni-leipzig.de _publ_contact_author_fax (+49)3419739319 _publ_section_title ; Oxidative cleavage of tetraaryltetraphosphane-1,4-diides by nickel(II) and palladium(II): formation of unusual Ni0 and Pd0 diaryldiphosphene complexes ; loop_ _publ_author_name _publ_author_address S.Gomez-Ruiz ;Institut fur Anorganische Chemie der Universitat Leipzig Johannisallee 29 D-04103 Leipzig Germany ; E.Hey-Hawkins ;Institut fur Anorganische Chemie der Universitat Leipzig Johannisallee 29 D-04103 Leipzig Germany ; _publ_requested_category FM data_c2270fin _database_code_depnum_ccdc_archive 'CCDC 655520' _audit_creation_date 2007-03-15T10:40:23-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_sum 'C30 H52 Ni P4' _chemical_formula_weight 595.31 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 18.6263(10) _cell_length_b 15.3768(9) _cell_length_c 22.9378(13) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 6569.7(6) _cell_formula_units_Z 8 _cell_measurement_temperature 213(2) #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description plates _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.05 _exptl_crystal_density_diffrn 1.204 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2560 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.802 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.900 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2001)' #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 213(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_reflns_av_R_equivalents 0.0466 _diffrn_reflns_av_unetI/netI 0.035 _diffrn_reflns_number 36836 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.93 _diffrn_reflns_theta_max 24.73 _diffrn_reflns_theta_full 24.73 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _reflns_number_total 5594 _reflns_number_gt 4287 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick,1997)' _computing_molecular_graphics 'ORTEP3 for Windows (L. J. Farrugia, 1997)' _computing_publication_material 'WINGX (L.J. Farrugia,1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0359P)^2^+1.3303P] 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 5594 _refine_ls_number_parameters 328 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0527 _refine_ls_R_factor_gt 0.0337 _refine_ls_wR_factor_ref 0.074 _refine_ls_wR_factor_gt 0.0693 _refine_ls_goodness_of_fit_ref 1.017 _refine_ls_restrained_S_all 1.017 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.251 _refine_diff_density_min -0.195 _refine_diff_density_rms 0.045 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 C1 C 0.21792(11) 0.81304(15) 0.31039(10) 0.0300(5) Uani 1 1 d . . . C2 C 0.17484(11) 0.88801(16) 0.30473(10) 0.0322(6) Uani 1 1 d . . . C3 C 0.17202(12) 0.94811(16) 0.35012(11) 0.0389(6) Uani 1 1 d . . . H3 H 0.1448 0.999 0.345 0.047 Uiso 1 1 calc R . . C4 C 0.20767(13) 0.93584(17) 0.40237(11) 0.0409(6) Uani 1 1 d . . . C5 C 0.24833(13) 0.86125(17) 0.40806(11) 0.0406(6) Uani 1 1 d . . . H5 H 0.2724 0.8511 0.4434 0.049 Uiso 1 1 calc R . . C6 C 0.25495(12) 0.80069(16) 0.36349(10) 0.0348(6) Uani 1 1 d . . . C7 C 0.12956(13) 0.90569(16) 0.25156(11) 0.0416(6) Uani 1 1 d . . . H7A H 0.0973 0.9538 0.2594 0.062 Uiso 1 1 calc R . . H7B H 0.1018 0.8543 0.2421 0.062 Uiso 1 1 calc R . . H7C H 0.1605 0.9204 0.219 0.062 Uiso 1 1 calc R . . C8 C 0.20203(17) 1.00087(19) 0.45153(12) 0.0613(8) Uani 1 1 d . . . H8A H 0.2396 1.0441 0.4475 0.092 Uiso 1 1 calc R . . H8B H 0.2073 0.971 0.4885 0.092 Uiso 1 1 calc R . . H8C H 0.1555 1.0292 0.4501 0.092 Uiso 1 1 calc R . . C9 C 0.30139(15) 0.72143(18) 0.37471(12) 0.0540(8) Uani 1 1 d . . . H9A H 0.3221 0.7253 0.4134 0.081 Uiso 1 1 calc R . . H9B H 0.3395 0.719 0.346 0.081 Uiso 1 1 calc R . . H9C H 0.2722 0.6693 0.3719 0.081 Uiso 1 1 calc R . . C10 C 0.27638(11) 0.69526(15) 0.12652(10) 0.0302(5) Uani 1 1 d . . . C11 C 0.31774(11) 0.73691(16) 0.08312(10) 0.0343(6) Uani 1 1 d . . . C12 C 0.35793(12) 0.68690(18) 0.04430(10) 0.0416(6) Uani 1 1 d . . . H12 H 0.3853 0.7155 0.0157 0.05 Uiso 1 1 calc R . . C13 C 0.35919(12) 0.59766(19) 0.04615(11) 0.0429(7) Uani 1 1 d . . . C14 C 0.31941(12) 0.55685(17) 0.08925(11) 0.0416(6) Uani 1 1 d . . . H14 H 0.3202 0.4958 0.0916 0.05 Uiso 1 1 calc R . . C15 C 0.27824(11) 0.60353(16) 0.12928(10) 0.0336(6) Uani 1 1 d . . . C16 C 0.32002(15) 0.83449(17) 0.07658(12) 0.0524(7) Uani 1 1 d . . . H16A H 0.3557 0.8501 0.0476 0.079 Uiso 1 1 calc R . . H16B H 0.3325 0.8607 0.1137 0.079 Uiso 1 1 calc R . . H16C H 0.2733 0.8554 0.0642 0.079 Uiso 1 1 calc R . . C17 C 0.40081(15) 0.5452(2) 0.00142(13) 0.0636(9) Uani 1 1 d . . . H17A H 0.3856 0.5617 -0.0375 0.095 Uiso 1 1 calc R . . H17B H 0.3917 0.4837 0.0074 0.095 Uiso 1 1 calc R . . H17C H 0.4517 0.5566 0.0058 0.095 Uiso 1 1 calc R . . C18 C 0.23715(12) 0.55104(16) 0.17388(12) 0.0434(7) Uani 1 1 d . . . H18A H 0.2382 0.4901 0.1631 0.065 Uiso 1 1 calc R . . H18B H 0.1878 0.571 0.1753 0.065 Uiso 1 1 calc R . . H18C H 0.2591 0.5584 0.2119 0.065 Uiso 1 1 calc R . . C19 C 0.10998(13) 0.67448(18) 0.05954(11) 0.0454(7) Uani 1 1 d . . . H19A H 0.1393 0.7269 0.0551 0.054 Uiso 1 1 calc R . . H19B H 0.1429 0.6249 0.0621 0.054 Uiso 1 1 calc R . . C20 C 0.06475(16) 0.6637(2) 0.00409(11) 0.0624(9) Uani 1 1 d . . . H20A H 0.04 0.6082 0.0053 0.094 Uiso 1 1 calc R . . H20B H 0.0958 0.6656 -0.0298 0.094 Uiso 1 1 calc R . . H20C H 0.0299 0.7104 0.0018 0.094 Uiso 1 1 calc R . . C21 C -0.00246(14) 0.59125(17) 0.12326(12) 0.0483(7) Uani 1 1 d . . . H21A H -0.0332 0.5908 0.158 0.058 Uiso 1 1 calc R . . H21B H -0.0334 0.6011 0.0893 0.058 Uiso 1 1 calc R . . C22 C 0.03302(17) 0.50257(19) 0.11722(14) 0.0659(9) Uani 1 1 d . . . H22A H 0.0581 0.4994 0.0802 0.099 Uiso 1 1 calc R . . H22B H -0.0034 0.4575 0.1188 0.099 Uiso 1 1 calc R . . H22C H 0.0669 0.4942 0.1488 0.099 Uiso 1 1 calc R . . C23 C 0.00135(14) 0.77580(17) 0.11721(11) 0.0465(7) Uani 1 1 d . . . H23A H -0.03 0.7629 0.084 0.056 Uiso 1 1 calc R . . H23B H -0.0292 0.7831 0.1516 0.056 Uiso 1 1 calc R . . C24 C 0.04074(17) 0.86126(18) 0.10548(13) 0.0613(8) Uani 1 1 d . . . H24A H 0.0744 0.8726 0.1369 0.092 Uiso 1 1 calc R . . H24B H 0.0062 0.9084 0.1032 0.092 Uiso 1 1 calc R . . H24C H 0.0666 0.857 0.0689 0.092 Uiso 1 1 calc R . . C25 C 0.05366(14) 0.52684(17) 0.28503(12) 0.0485(7) Uani 1 1 d . . . H25A H 0.0176 0.5113 0.3144 0.058 Uiso 1 1 calc R . . H25B H 0.0369 0.5046 0.2474 0.058 Uiso 1 1 calc R . . C26 C 0.12406(16) 0.48161(19) 0.30042(14) 0.0661(9) Uani 1 1 d . . . H26A H 0.1605 0.4971 0.272 0.099 Uiso 1 1 calc R . . H26B H 0.117 0.4191 0.3001 0.099 Uiso 1 1 calc R . . H26C H 0.1395 0.4998 0.3389 0.099 Uiso 1 1 calc R . . C27 C -0.03692(13) 0.67589(19) 0.28189(12) 0.0491(7) Uani 1 1 d . . . H27A H -0.059 0.6574 0.2451 0.059 Uiso 1 1 calc R . . H27B H -0.0606 0.644 0.3135 0.059 Uiso 1 1 calc R . . C28 C -0.05073(16) 0.7727(2) 0.29020(14) 0.0681(9) Uani 1 1 d . . . H28A H -0.0339 0.7904 0.3284 0.102 Uiso 1 1 calc R . . H28B H -0.1018 0.7841 0.287 0.102 Uiso 1 1 calc R . . H28C H -0.0253 0.8052 0.2604 0.102 Uiso 1 1 calc R . . C29 C 0.08838(14) 0.67528(19) 0.35467(11) 0.0476(7) Uani 1 1 d . . . H29A H 0.1382 0.656 0.3595 0.057 Uiso 1 1 calc R . . H29B H 0.0882 0.7389 0.3578 0.057 Uiso 1 1 calc R . . C30 C 0.04452(16) 0.6388(2) 0.40515(12) 0.0643(9) Uani 1 1 d . . . H30A H -0.0038 0.6621 0.4036 0.097 Uiso 1 1 calc R . . H30B H 0.0668 0.6551 0.4418 0.097 Uiso 1 1 calc R . . H30C H 0.0427 0.5759 0.4022 0.097 Uiso 1 1 calc R . . P1 P 0.22841(3) 0.72170(4) 0.25787(3) 0.03308(16) Uani 1 1 d . . . P2 P 0.21914(3) 0.76954(4) 0.17079(3) 0.03260(16) Uani 1 1 d . . . P3 P 0.06144(3) 0.68262(4) 0.12926(3) 0.03332(16) Uani 1 1 d . . . P4 P 0.05916(3) 0.64595(4) 0.28074(3) 0.03419(16) Uani 1 1 d . . . Ni1 Ni 0.125521(14) 0.694829(19) 0.208796(12) 0.02830(9) 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 C1 0.0248(11) 0.0320(15) 0.0333(13) -0.0004(11) 0.0008(9) -0.0046(10) C2 0.0295(11) 0.0340(15) 0.0330(14) 0.0012(11) 0.0014(10) -0.0004(10) C3 0.0400(13) 0.0350(16) 0.0416(16) -0.0003(12) 0.0019(11) 0.0034(11) C4 0.0489(14) 0.0379(17) 0.0358(15) -0.0049(12) 0.0018(12) -0.0048(12) C5 0.0463(14) 0.0438(18) 0.0316(14) 0.0010(13) -0.0075(12) -0.0047(12) C6 0.0305(11) 0.0348(16) 0.0392(14) 0.0023(12) -0.0032(11) -0.0022(10) C7 0.0417(14) 0.0406(16) 0.0426(16) -0.0058(13) -0.0057(12) 0.0126(12) C8 0.090(2) 0.051(2) 0.0428(18) -0.0118(15) -0.0041(16) 0.0025(16) C9 0.0559(16) 0.055(2) 0.0510(18) 0.0005(15) -0.0215(14) 0.0114(14) C10 0.0245(11) 0.0343(15) 0.0317(13) -0.0034(11) -0.0010(9) 0.0008(10) C11 0.0302(11) 0.0411(16) 0.0317(14) 0.0028(12) -0.0010(10) 0.0012(11) C12 0.0349(13) 0.058(2) 0.0320(14) 0.0036(13) 0.0035(11) 0.0047(12) C13 0.0366(13) 0.059(2) 0.0331(15) -0.0074(13) -0.0014(11) 0.0126(12) C14 0.0390(13) 0.0397(16) 0.0462(16) -0.0053(13) -0.0048(12) 0.0097(12) C15 0.0279(11) 0.0352(16) 0.0378(14) -0.0039(12) -0.0009(10) 0.0036(10) C16 0.0584(17) 0.0495(19) 0.0494(18) 0.0112(14) 0.0160(14) -0.0032(14) C17 0.0634(18) 0.078(2) 0.0498(19) -0.0103(16) 0.0114(15) 0.0244(16) C18 0.0423(14) 0.0307(16) 0.0572(18) -0.0021(13) 0.0073(13) 0.0018(12) C19 0.0444(15) 0.0559(19) 0.0358(15) -0.0030(13) 0.0002(11) 0.0032(12) C20 0.0667(19) 0.086(3) 0.0347(16) -0.0034(15) -0.0057(14) 0.0067(17) C21 0.0449(14) 0.0493(19) 0.0508(17) -0.0050(14) -0.0076(13) -0.0092(13) C22 0.079(2) 0.045(2) 0.073(2) -0.0065(17) -0.0105(18) -0.0098(16) C23 0.0448(14) 0.0511(19) 0.0437(16) -0.0008(14) -0.0049(12) 0.0120(13) C24 0.086(2) 0.043(2) 0.0547(19) 0.0027(15) -0.0199(16) 0.0161(16) C25 0.0568(16) 0.0416(17) 0.0471(17) 0.0070(14) -0.0008(14) -0.0128(13) C26 0.0695(19) 0.047(2) 0.081(2) 0.0201(17) 0.0045(17) 0.0089(16) C27 0.0337(13) 0.065(2) 0.0484(18) 0.0105(15) 0.0077(12) 0.0003(12) C28 0.0515(17) 0.071(2) 0.082(2) 0.0135(19) 0.0200(16) 0.0164(16) C29 0.0522(16) 0.056(2) 0.0350(15) 0.0043(13) 0.0054(12) -0.0126(13) C30 0.078(2) 0.074(2) 0.0415(18) 0.0089(16) 0.0091(15) -0.0122(17) P1 0.0279(3) 0.0346(4) 0.0368(4) -0.0039(3) -0.0029(3) 0.0023(3) P2 0.0314(3) 0.0292(4) 0.0373(4) -0.0015(3) 0.0070(3) -0.0011(3) P3 0.0301(3) 0.0365(4) 0.0334(4) -0.0011(3) -0.0026(3) 0.0004(3) P4 0.0306(3) 0.0382(4) 0.0339(4) 0.0050(3) 0.0013(3) -0.0050(3) Ni1 0.02512(14) 0.03007(18) 0.02972(17) 0.00082(14) 0.00058(12) -0.00215(12) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 C1 C2 1.410(3) . ? C1 C6 1.413(3) . ? C1 P1 1.861(2) . ? C2 C3 1.393(3) . ? C2 C7 1.507(3) . ? C3 C4 1.383(3) . ? C4 C5 1.381(3) . ? C4 C8 1.511(3) . ? C5 C6 1.388(3) . ? C6 C9 1.516(3) . ? C10 C11 1.412(3) . ? C10 C15 1.412(3) . ? C10 P2 1.864(2) . ? C11 C12 1.394(3) . ? C11 C16 1.509(3) . ? C12 C13 1.373(3) . ? C13 C14 1.386(3) . ? C13 C17 1.518(3) . ? C14 C15 1.395(3) . ? C15 C18 1.511(3) . ? C19 C20 1.535(3) . ? C19 P3 1.841(2) . ? C21 C22 1.522(4) . ? C21 P3 1.847(2) . ? C23 C24 1.529(4) . ? C23 P3 1.839(3) . ? C25 C26 1.526(4) . ? C25 P4 1.837(3) . ? C27 C28 1.522(4) . ? C27 P4 1.848(2) . ? C29 C30 1.524(3) . ? C29 P4 1.837(3) . ? P1 P2 2.1355(9) . ? P1 Ni1 2.2606(6) . ? P2 Ni1 2.2629(7) . ? P3 Ni1 2.1883(7) . ? P4 Ni1 2.1945(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 C6 117.8(2) . . ? C2 C1 P1 128.10(17) . . ? C6 C1 P1 113.92(17) . . ? C3 C2 C1 119.7(2) . . ? C3 C2 C7 117.6(2) . . ? C1 C2 C7 122.7(2) . . ? C4 C3 C2 122.6(2) . . ? C5 C4 C3 117.3(2) . . ? C5 C4 C8 121.2(2) . . ? C3 C4 C8 121.5(2) . . ? C4 C5 C6 122.4(2) . . ? C5 C6 C1 120.1(2) . . ? C5 C6 C9 117.7(2) . . ? C1 C6 C9 122.2(2) . . ? C11 C10 C15 118.1(2) . . ? C11 C10 P2 114.72(18) . . ? C15 C10 P2 126.99(17) . . ? C12 C11 C10 119.5(2) . . ? C12 C11 C16 118.0(2) . . ? C10 C11 C16 122.5(2) . . ? C13 C12 C11 122.7(2) . . ? C12 C13 C14 117.7(2) . . ? C12 C13 C17 121.3(2) . . ? C14 C13 C17 121.0(3) . . ? C13 C14 C15 122.0(2) . . ? C14 C15 C10 119.8(2) . . ? C14 C15 C18 116.7(2) . . ? C10 C15 C18 123.5(2) . . ? C20 C19 P3 117.23(18) . . ? C22 C21 P3 114.13(19) . . ? C24 C23 P3 113.83(19) . . ? C26 C25 P4 114.76(19) . . ? C28 C27 P4 114.14(19) . . ? C30 C29 P4 116.87(19) . . ? C1 P1 P2 109.70(8) . . ? C1 P1 Ni1 111.80(7) . . ? P2 P1 Ni1 61.88(2) . . ? C10 P2 P1 104.62(8) . . ? C10 P2 Ni1 109.86(8) . . ? P1 P2 Ni1 61.78(2) . . ? C23 P3 C19 102.79(12) . . ? C23 P3 C21 100.91(12) . . ? C19 P3 C21 101.54(12) . . ? C23 P3 Ni1 112.98(9) . . ? C19 P3 Ni1 117.52(8) . . ? C21 P3 Ni1 118.62(9) . . ? C25 P4 C29 102.23(12) . . ? C25 P4 C27 101.16(12) . . ? C29 P4 C27 102.27(13) . . ? C25 P4 Ni1 114.41(9) . . ? C29 P4 Ni1 116.31(8) . . ? C27 P4 Ni1 118.09(9) . . ? P3 Ni1 P4 106.88(3) . . ? P3 Ni1 P1 153.28(3) . . ? P4 Ni1 P1 99.54(3) . . ? P3 Ni1 P2 98.20(3) . . ? P4 Ni1 P2 153.84(3) . . ? P1 Ni1 P2 56.34(2) . . ? #============================================================================ data_x0016fin _database_code_depnum_ccdc_archive 'CCDC 655521' _audit_creation_date 2006-10-15T01:19:41-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_sum 'C41 H52 Ni P4' _chemical_formula_weight 727.42 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _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 11.209(3) _cell_length_b 12.402(3) _cell_length_c 15.808(3) _cell_angle_alpha 85.182(19) _cell_angle_beta 72.99(2) _cell_angle_gamma 66.42(3) _cell_volume 1924.7(9) _cell_formula_units_Z 2 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 12302 _cell_measurement_theta_min 2.6912 _cell_measurement_theta_max 28.5456 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description plates _exptl_crystal_colour red _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 1.255 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 772 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.698 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.93529 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.5 (release 28-08-2006 CrysAlis171 .NET) (compiled Aug 28 2006,13:05:05) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_detector_area_resol_mean 16.356 _diffrn_orient_matrix_ub_11 -0.0521155905 _diffrn_orient_matrix_ub_12 -0.0206650043 _diffrn_orient_matrix_ub_13 0.0198854768 _diffrn_orient_matrix_ub_21 0.0217693572 _diffrn_orient_matrix_ub_22 -0.0378161309 _diffrn_orient_matrix_ub_23 -0.0376340304 _diffrn_orient_matrix_ub_31 0.0449032389 _diffrn_orient_matrix_ub_32 -0.0452203618 _diffrn_orient_matrix_ub_33 0.0199311004 _diffrn_measurement_device_type 'ccd xcalibur s' _diffrn_measurement_method '\w scans and \f scans' _diffrn_reflns_av_R_equivalents 0.0546 _diffrn_reflns_av_unetI/netI 0.0699 _diffrn_reflns_number 36758 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.7 _diffrn_reflns_theta_max 26.37 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.993 _diffrn_measured_fraction_theta_max 0.993 _reflns_number_total 7811 _reflns_number_gt 5378 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.31.5 (release 28-08-2006 CrysAlis171 .NET) (compiled Aug 28 2006,13:05:05) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.5 (release 28-08-2006 CrysAlis171 .NET) (compiled Aug 28 2006,13:05:05) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.5 (release 28-08-2006 CrysAlis171 .NET) (compiled Aug 28 2006,13:05:05) ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP3 for Windows (L. J. Farrugia, 1997)' _computing_publication_material 'WINGX (L.J. Farrugia,1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0388P)^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 7811 _refine_ls_number_parameters 426 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0739 _refine_ls_R_factor_gt 0.0399 _refine_ls_wR_factor_ref 0.0841 _refine_ls_wR_factor_gt 0.0724 _refine_ls_goodness_of_fit_ref 1 _refine_ls_restrained_S_all 1 _refine_ls_shift/su_max 0.034 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.588 _refine_diff_density_min -0.342 _refine_diff_density_rms 0.06 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 C1 C 0.0425(2) 0.7564(2) 0.08344(15) 0.0213(5) Uani 1 1 d . . . C2 C -0.0382(3) 0.8450(2) 0.03785(16) 0.0245(6) Uani 1 1 d . . . C3 C 0.0149(3) 0.8573(2) -0.05203(16) 0.0311(6) Uani 1 1 d . . . H3 H -0.0408 0.917 -0.0817 0.037 Uiso 1 1 calc R . . C4 C 0.1447(3) 0.7866(2) -0.10007(16) 0.0310(6) Uani 1 1 d . . . C5 C 0.2249(3) 0.7028(2) -0.05448(16) 0.0298(6) Uani 1 1 d . . . H5 H 0.3157 0.655 -0.0856 0.036 Uiso 1 1 calc R . . C6 C 0.1774(2) 0.6860(2) 0.03527(16) 0.0250(6) Uani 1 1 d . . . C7 C -0.1820(3) 0.9265(2) 0.08136(17) 0.0323(7) Uani 1 1 d . . . H7A H -0.1825 0.9811 0.123 0.049 Uiso 1 1 calc R . . H7B H -0.2335 0.8804 0.1134 0.049 Uiso 1 1 calc R . . H7C H -0.2238 0.9712 0.0361 0.049 Uiso 1 1 calc R . . C8 C 0.1949(3) 0.7993(3) -0.19849(17) 0.0484(8) Uani 1 1 d . . . H8A H 0.2937 0.7742 -0.2161 0.073 Uiso 1 1 calc R . . H8B H 0.1527 0.8818 -0.213 0.073 Uiso 1 1 calc R . . H8C H 0.1708 0.7501 -0.2303 0.073 Uiso 1 1 calc R . . C9 C 0.2731(3) 0.5905(2) 0.07826(17) 0.0341(7) Uani 1 1 d . . . H9A H 0.3633 0.557 0.0357 0.051 Uiso 1 1 calc R . . H9B H 0.2387 0.5284 0.0969 0.051 Uiso 1 1 calc R . . H9C H 0.2792 0.6241 0.13 0.051 Uiso 1 1 calc R . . C10 C -0.1275(2) 0.8257(2) 0.39504(15) 0.0219(6) Uani 1 1 d . . . C11 C -0.1299(2) 0.9158(2) 0.44618(16) 0.0260(6) Uani 1 1 d . . . C12 C -0.1313(3) 0.8979(2) 0.53481(16) 0.0316(7) Uani 1 1 d . . . H12 H -0.1326 0.9588 0.5682 0.038 Uiso 1 1 calc R . . C13 C -0.1310(3) 0.7954(3) 0.57570(16) 0.0337(7) Uani 1 1 d . . . C14 C -0.1309(3) 0.7087(2) 0.52603(16) 0.0309(6) Uani 1 1 d . . . H14 H -0.132 0.6379 0.5535 0.037 Uiso 1 1 calc R . . C15 C -0.1292(2) 0.7212(2) 0.43725(16) 0.0252(6) Uani 1 1 d . . . C16 C -0.1328(3) 1.0325(2) 0.40856(17) 0.0342(7) Uani 1 1 d . . . H16A H -0.1309 1.0809 0.4537 0.051 Uiso 1 1 calc R . . H16B H -0.2158 1.0734 0.3904 0.051 Uiso 1 1 calc R . . H16C H -0.0535 1.0191 0.3571 0.051 Uiso 1 1 calc R . . C17 C -0.1308(3) 0.7778(3) 0.67189(17) 0.0528(9) Uani 1 1 d . . . H17A H -0.0456 0.776 0.6782 0.079 Uiso 1 1 calc R . . H17B H -0.1393 0.7033 0.6907 0.079 Uiso 1 1 calc R . . H17C H -0.2073 0.8429 0.7088 0.079 Uiso 1 1 calc R . . C18 C -0.1295(3) 0.6194(2) 0.39151(17) 0.0332(7) Uani 1 1 d . . . H18A H -0.0387 0.5763 0.3521 0.05 Uiso 1 1 calc R . . H18B H -0.195 0.6492 0.3569 0.05 Uiso 1 1 calc R . . H18C H -0.1549 0.5664 0.4359 0.05 Uiso 1 1 calc R . . C19 C -0.4953(3) 0.8367(3) 0.42695(17) 0.0458(8) Uani 1 1 d . . . H19A H -0.5859 0.8937 0.4574 0.069 Uiso 1 1 calc R . . H19B H -0.4306 0.8342 0.4583 0.069 Uiso 1 1 calc R . . H19C H -0.4973 0.7586 0.4261 0.069 Uiso 1 1 calc R . . C20 C -0.4780(3) 1.0353(2) 0.3319(2) 0.0467(8) Uani 1 1 d . . . H20A H -0.5728 1.0762 0.3665 0.07 Uiso 1 1 calc R . . H20B H -0.4621 1.072 0.2746 0.07 Uiso 1 1 calc R . . H20C H -0.4179 1.0408 0.3641 0.07 Uiso 1 1 calc R . . C21 C -0.5810(2) 0.8944(2) 0.26827(16) 0.0240(6) Uani 1 1 d . . . C22 C -0.6749(3) 0.8449(2) 0.30578(18) 0.0321(6) Uani 1 1 d . . . H22 H -0.6721 0.805 0.3596 0.039 Uiso 1 1 calc R . . C23 C -0.7730(3) 0.8531(2) 0.2655(2) 0.0373(7) Uani 1 1 d . . . H23 H -0.8364 0.8186 0.2919 0.045 Uiso 1 1 calc R . . C24 C -0.7788(3) 0.9108(2) 0.1878(2) 0.0425(8) Uani 1 1 d . . . H24 H -0.8456 0.9159 0.1602 0.051 Uiso 1 1 calc R . . C25 C -0.6871(3) 0.9609(2) 0.1503(2) 0.0408(8) Uani 1 1 d . . . H25 H -0.6918 1.0021 0.0971 0.049 Uiso 1 1 calc R . . C26 C -0.5874(3) 0.9520(2) 0.18944(17) 0.0319(6) Uani 1 1 d . . . H26 H -0.5234 0.9856 0.1621 0.038 Uiso 1 1 calc R . . C27 C -0.3725(3) 0.5664(2) 0.24159(18) 0.0375(7) Uani 1 1 d . . . H27A H -0.4637 0.6282 0.2621 0.056 Uiso 1 1 calc R . . H27B H -0.3412 0.5297 0.2928 0.056 Uiso 1 1 calc R . . H27C H -0.3748 0.5067 0.2059 0.056 Uiso 1 1 calc R . . C28 C -0.1017(3) 0.4986(2) 0.13782(19) 0.0391(7) Uani 1 1 d . . . H28A H -0.1205 0.4423 0.1094 0.059 Uiso 1 1 calc R . . H28B H -0.0697 0.463 0.189 0.059 Uiso 1 1 calc R . . H28C H -0.0317 0.5197 0.0954 0.059 Uiso 1 1 calc R . . C29 C -0.3096(3) 0.6720(2) 0.07380(16) 0.0254(6) Uani 1 1 d . . . C30 C -0.2189(3) 0.6925(2) -0.00107(17) 0.0350(7) Uani 1 1 d . . . H30 H -0.13 0.6791 0.0006 0.042 Uiso 1 1 calc R . . C31 C -0.2563(4) 0.7322(3) -0.07767(19) 0.0499(9) Uani 1 1 d . . . H31 H -0.1935 0.7455 -0.1282 0.06 Uiso 1 1 calc R . . C32 C -0.3858(4) 0.7522(3) -0.0800(2) 0.0530(9) Uani 1 1 d . . . H32 H -0.4118 0.7792 -0.1325 0.064 Uiso 1 1 calc R . . C33 C -0.4769(4) 0.7335(3) -0.0073(2) 0.0505(9) Uani 1 1 d . . . H33 H -0.5659 0.7482 -0.0095 0.061 Uiso 1 1 calc R . . C34 C -0.4391(3) 0.6928(2) 0.07038(19) 0.0387(7) Uani 1 1 d . . . H34 H -0.5023 0.6794 0.1206 0.046 Uiso 1 1 calc R . . C35 C 0.7039(4) 0.4497(3) 0.5599(3) 0.0729(12) Uani 1 1 d . . . C36 C 0.7597(4) 0.4334(4) 0.6320(4) 0.0806(15) Uani 1 1 d . . . H36 H 0.8344 0.3631 0.636 0.097 Uiso 1 1 calc R . . C37 C 0.7009(6) 0.5250(6) 0.6980(4) 0.109(2) Uani 1 1 d . . . H37 H 0.7386 0.515 0.7461 0.131 Uiso 1 1 calc R . . C38 C 0.5966(5) 0.6232(4) 0.6956(3) 0.0822(13) Uani 1 1 d . . . H38 H 0.5589 0.6823 0.7414 0.099 Uiso 1 1 calc R . . C39 C 0.5425(4) 0.6385(3) 0.6243(2) 0.0592(10) Uani 1 1 d . . . H39 H 0.4679 0.7094 0.6213 0.071 Uiso 1 1 calc R . . C40 C 0.5946(3) 0.5541(3) 0.5592(2) 0.0504(9) Uani 1 1 d . . . H40 H 0.5548 0.5668 0.5118 0.06 Uiso 1 1 calc R . . C41 C 0.7592(4) 0.3600(3) 0.4907(3) 0.1105(19) Uani 1 1 d . . . H41A H 0.6914 0.3285 0.4916 0.166 Uiso 1 1 calc R . . H41B H 0.8404 0.2963 0.5003 0.166 Uiso 1 1 calc R . . H41C H 0.7834 0.394 0.4332 0.166 Uiso 1 1 calc R . . P1 P -0.01143(6) 0.70910(6) 0.19829(4) 0.02295(16) Uani 1 1 d . . . P2 P -0.13150(7) 0.86643(6) 0.27926(4) 0.02293(16) Uani 1 1 d . . . P3 P -0.44326(7) 0.88067(6) 0.31403(4) 0.02440(16) Uani 1 1 d . . . P4 P -0.25640(7) 0.63058(6) 0.17443(4) 0.02428(16) Uani 1 1 d . . . Ni1 Ni -0.23977(3) 0.76996(3) 0.238798(19) 0.02007(9) 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 C1 0.0247(14) 0.0239(13) 0.0196(12) 0.0010(11) -0.0065(11) -0.0136(11) C2 0.0309(15) 0.0230(14) 0.0226(13) 0.0007(11) -0.0086(11) -0.0129(12) C3 0.0416(17) 0.0271(15) 0.0267(14) 0.0087(12) -0.0124(13) -0.0153(13) C4 0.0426(18) 0.0310(15) 0.0220(13) 0.0000(12) -0.0036(13) -0.0209(14) C5 0.0320(16) 0.0299(15) 0.0268(14) -0.0070(12) 0.0007(12) -0.0163(13) C6 0.0253(14) 0.0270(14) 0.0250(13) -0.0030(11) -0.0051(11) -0.0132(12) C7 0.0312(16) 0.0351(16) 0.0274(14) 0.0061(12) -0.0112(12) -0.0086(13) C8 0.066(2) 0.0482(19) 0.0257(15) 0.0026(14) -0.0009(15) -0.0259(17) C9 0.0229(15) 0.0383(17) 0.0330(15) -0.0014(13) -0.0039(12) -0.0063(13) C10 0.0162(13) 0.0286(14) 0.0206(12) -0.0023(11) -0.0066(10) -0.0069(11) C11 0.0176(14) 0.0318(15) 0.0276(14) -0.0063(12) -0.0066(11) -0.0074(11) C12 0.0246(15) 0.0393(17) 0.0260(14) -0.0128(13) -0.0063(12) -0.0054(13) C13 0.0223(15) 0.0490(19) 0.0195(13) -0.0035(13) -0.0066(11) -0.0022(13) C14 0.0266(15) 0.0395(17) 0.0236(14) 0.0075(12) -0.0064(12) -0.0117(13) C15 0.0188(13) 0.0315(15) 0.0234(13) 0.0011(11) -0.0061(11) -0.0082(11) C16 0.0357(17) 0.0346(16) 0.0350(15) -0.0098(13) -0.0097(13) -0.0147(13) C17 0.051(2) 0.076(2) 0.0208(15) -0.0042(15) -0.0121(14) -0.0120(18) C18 0.0433(18) 0.0344(16) 0.0279(14) 0.0094(12) -0.0120(13) -0.0217(14) C19 0.0269(16) 0.077(2) 0.0250(15) 0.0023(15) -0.0082(13) -0.0113(16) C20 0.0293(17) 0.0386(18) 0.072(2) -0.0236(16) -0.0138(16) -0.0086(14) C21 0.0183(13) 0.0239(14) 0.0289(14) -0.0032(11) -0.0085(11) -0.0053(11) C22 0.0251(15) 0.0309(16) 0.0389(16) 0.0056(13) -0.0108(13) -0.0093(13) C23 0.0238(15) 0.0344(17) 0.059(2) 0.0026(15) -0.0156(14) -0.0145(13) C24 0.0363(18) 0.0327(17) 0.067(2) -0.0020(16) -0.0338(17) -0.0075(14) C25 0.050(2) 0.0340(17) 0.0436(18) 0.0095(14) -0.0287(16) -0.0122(15) C26 0.0321(16) 0.0328(16) 0.0361(15) 0.0037(13) -0.0135(13) -0.0158(13) C27 0.0437(18) 0.0359(17) 0.0373(16) -0.0007(13) -0.0090(14) -0.0215(14) C28 0.0355(17) 0.0288(16) 0.0512(18) -0.0106(14) -0.0177(15) -0.0046(13) C29 0.0287(15) 0.0214(14) 0.0280(14) -0.0070(11) -0.0085(12) -0.0098(12) C30 0.0414(18) 0.0349(16) 0.0285(15) -0.0046(13) -0.0076(13) -0.0153(14) C31 0.078(3) 0.0435(19) 0.0300(16) -0.0015(14) -0.0127(17) -0.0270(18) C32 0.088(3) 0.0406(19) 0.044(2) 0.0039(16) -0.038(2) -0.0260(19) C33 0.058(2) 0.0432(19) 0.063(2) -0.0069(17) -0.042(2) -0.0141(17) C34 0.0387(18) 0.0408(17) 0.0406(17) -0.0056(14) -0.0142(14) -0.0160(14) C35 0.036(2) 0.047(2) 0.120(4) 0.027(2) -0.001(2) -0.0200(18) C36 0.040(2) 0.068(3) 0.139(4) 0.069(3) -0.042(3) -0.029(2) C37 0.093(4) 0.159(6) 0.111(4) 0.090(4) -0.055(4) -0.085(4) C38 0.081(3) 0.114(4) 0.063(3) 0.021(3) -0.018(2) -0.054(3) C39 0.049(2) 0.069(3) 0.055(2) 0.0107(19) -0.0144(18) -0.0198(19) C40 0.0318(18) 0.042(2) 0.070(2) 0.0220(18) -0.0145(17) -0.0100(15) C41 0.056(3) 0.043(2) 0.199(5) -0.013(3) 0.027(3) -0.027(2) P1 0.0194(3) 0.0284(4) 0.0207(3) 0.0027(3) -0.0054(3) -0.0097(3) P2 0.0253(4) 0.0279(4) 0.0210(3) 0.0011(3) -0.0086(3) -0.0145(3) P3 0.0193(4) 0.0289(4) 0.0245(3) -0.0040(3) -0.0060(3) -0.0082(3) P4 0.0242(4) 0.0245(4) 0.0257(3) -0.0030(3) -0.0070(3) -0.0104(3) Ni1 0.01790(18) 0.02379(18) 0.01993(17) -0.00215(13) -0.00521(13) -0.00917(14) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 C1 C2 1.413(3) . ? C1 C6 1.418(3) . ? C1 P1 1.863(2) . ? C2 C3 1.392(3) . ? C2 C7 1.503(3) . ? C3 C4 1.381(4) . ? C4 C5 1.383(3) . ? C4 C8 1.510(3) . ? C5 C6 1.392(3) . ? C6 C9 1.513(3) . ? C10 C15 1.412(3) . ? C10 C11 1.421(3) . ? C10 P2 1.866(2) . ? C11 C12 1.396(3) . ? C11 C16 1.509(4) . ? C12 C13 1.376(4) . ? C13 C14 1.383(4) . ? C13 C17 1.518(3) . ? C14 C15 1.394(3) . ? C15 C18 1.508(3) . ? C19 P3 1.818(3) . ? C20 P3 1.827(3) . ? C21 C26 1.389(3) . ? C21 C22 1.388(4) . ? C21 P3 1.833(2) . ? C22 C23 1.390(4) . ? C23 C24 1.374(4) . ? C24 C25 1.373(4) . ? C25 C26 1.392(4) . ? C27 P4 1.826(3) . ? C28 P4 1.823(3) . ? C29 C34 1.385(4) . ? C29 C30 1.398(4) . ? C29 P4 1.823(3) . ? C30 C31 1.384(4) . ? C31 C32 1.382(5) . ? C32 C33 1.369(5) . ? C33 C34 1.405(4) . ? C35 C40 1.383(4) . ? C35 C36 1.417(6) . ? C35 C41 1.441(6) . ? C36 C37 1.418(7) . ? C37 C38 1.316(6) . ? C38 C39 1.394(5) . ? C39 C40 1.356(4) . ? P1 P2 2.1374(12) . ? P1 Ni1 2.2601(11) . ? P2 Ni1 2.2490(9) . ? P3 Ni1 2.1643(12) . ? P4 Ni1 2.1731(9) . ? 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 C2 C1 C6 117.7(2) . . ? C2 C1 P1 127.68(19) . . ? C6 C1 P1 114.28(18) . . ? C3 C2 C1 119.5(2) . . ? C3 C2 C7 117.4(2) . . ? C1 C2 C7 123.1(2) . . ? C4 C3 C2 123.1(2) . . ? C5 C4 C3 117.1(2) . . ? C5 C4 C8 121.8(2) . . ? C3 C4 C8 121.0(2) . . ? C4 C5 C6 122.4(2) . . ? C5 C6 C1 120.0(2) . . ? C5 C6 C9 118.0(2) . . ? C1 C6 C9 121.9(2) . . ? C15 C10 C11 117.9(2) . . ? C15 C10 P2 128.13(18) . . ? C11 C10 P2 113.88(19) . . ? C12 C11 C10 119.6(2) . . ? C12 C11 C16 118.0(2) . . ? C10 C11 C16 122.3(2) . . ? C13 C12 C11 122.5(2) . . ? C12 C13 C14 117.6(2) . . ? C12 C13 C17 121.3(3) . . ? C14 C13 C17 121.1(3) . . ? C13 C14 C15 122.6(3) . . ? C14 C15 C10 119.7(2) . . ? C14 C15 C18 116.8(2) . . ? C10 C15 C18 123.6(2) . . ? C26 C21 C22 118.3(2) . . ? C26 C21 P3 118.2(2) . . ? C22 C21 P3 123.4(2) . . ? C23 C22 C21 120.8(3) . . ? C24 C23 C22 120.4(3) . . ? C23 C24 C25 119.4(3) . . ? C24 C25 C26 120.7(3) . . ? C21 C26 C25 120.4(3) . . ? C34 C29 C30 118.7(2) . . ? C34 C29 P4 122.9(2) . . ? C30 C29 P4 118.2(2) . . ? C31 C30 C29 121.1(3) . . ? C32 C31 C30 119.4(3) . . ? C33 C32 C31 120.6(3) . . ? C32 C33 C34 120.1(3) . . ? C29 C34 C33 120.0(3) . . ? C40 C35 C36 117.5(4) . . ? C40 C35 C41 121.7(4) . . ? C36 C35 C41 120.8(4) . . ? C37 C36 C35 118.1(4) . . ? C38 C37 C36 123.0(5) . . ? C37 C38 C39 118.5(5) . . ? C40 C39 C38 121.2(4) . . ? C39 C40 C35 121.7(4) . . ? C1 P1 P2 106.48(8) . . ? C1 P1 Ni1 107.96(8) . . ? P2 P1 Ni1 61.44(4) . . ? C10 P2 P1 106.70(8) . . ? C10 P2 Ni1 106.79(8) . . ? P1 P2 Ni1 61.97(3) . . ? C19 P3 C20 101.35(15) . . ? C19 P3 C21 104.09(13) . . ? C20 P3 C21 101.08(12) . . ? C19 P3 Ni1 114.62(10) . . ? C20 P3 Ni1 116.99(11) . . ? C21 P3 Ni1 116.52(8) . . ? C28 P4 C27 100.69(14) . . ? C28 P4 C29 102.51(12) . . ? C27 P4 C29 104.37(13) . . ? C28 P4 Ni1 116.33(10) . . ? C27 P4 Ni1 116.03(9) . . ? C29 P4 Ni1 114.90(8) . . ? P3 Ni1 P4 106.81(4) . . ? P3 Ni1 P2 97.09(4) . . ? P4 Ni1 P2 156.00(3) . . ? P3 Ni1 P1 153.39(3) . . ? P4 Ni1 P1 99.41(4) . . ? P2 Ni1 P1 56.59(3) . . ? #============================================================================ data_x0012fin _database_code_depnum_ccdc_archive 'CCDC 655522' _audit_creation_date 2006-10-14T01:12:25-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_sum 'C42 H76 P4 Pd' _chemical_formula_weight 811.31 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _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 9.083(2) _cell_length_b 12.2987(8) _cell_length_c 21.174(8) _cell_angle_alpha 93.065(13) _cell_angle_beta 91.79(3) _cell_angle_gamma 103.773(11) _cell_volume 2291.7(10) _cell_formula_units_Z 2 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 16789 _cell_measurement_theta_min 2.6481 _cell_measurement_theta_max 31.9896 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description plates _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 1.176 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 868 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.57 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.5 (release 28-08-2006 CrysAlis171 .NET) (compiled Aug 28 2006,13:05:05) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_correction_T_min 0.85642 _exptl_absorpt_correction_T_max 1 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_detector_area_resol_mean 16.356 _diffrn_orient_matrix_ub_11 0.0422343322 _diffrn_orient_matrix_ub_12 0.0011206757 _diffrn_orient_matrix_ub_13 0.0288973072 _diffrn_orient_matrix_ub_21 -0.0277206715 _diffrn_orient_matrix_ub_22 -0.0589095596 _diffrn_orient_matrix_ub_23 0.0009054532 _diffrn_orient_matrix_ub_31 0.0627024608 _diffrn_orient_matrix_ub_32 -0.0084670038 _diffrn_orient_matrix_ub_33 -0.0171297708 _diffrn_measurement_device_type 'ccd xcalibur s' _diffrn_measurement_method '\w scans and \f scans' _diffrn_reflns_av_R_equivalents 0.0688 _diffrn_reflns_av_unetI/netI 0.077 _diffrn_reflns_number 57191 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.66 _diffrn_reflns_theta_max 28.28 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _reflns_number_total 11353 _reflns_number_gt 7673 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.31.5 (release 28-08-2006 CrysAlis171 .NET) (compiled Aug 28 2006,13:05:05) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.5 (release 28-08-2006 CrysAlis171 .NET) (compiled Aug 28 2006,13:05:05) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.5 (release 28-08-2006 CrysAlis171 .NET) (compiled Aug 28 2006,13:05:05) ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP3 for Windows (L. J. Farrugia, 1997)' _computing_publication_material 'WINGX (L.J. Farrugia,1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0247P)^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 11353 _refine_ls_number_parameters 436 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0719 _refine_ls_R_factor_gt 0.0366 _refine_ls_wR_factor_ref 0.0643 _refine_ls_wR_factor_gt 0.0558 _refine_ls_goodness_of_fit_ref 0.966 _refine_ls_restrained_S_all 0.966 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.369 _refine_diff_density_min -0.39 _refine_diff_density_rms 0.065 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' 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 C1 C -0.0554(2) 1.00810(17) 0.30970(10) 0.0290(5) Uani 1 1 d . . . C2 C -0.0950(2) 1.11224(18) 0.31331(10) 0.0342(5) Uani 1 1 d . . . C3 C -0.1536(3) 1.14821(19) 0.36846(11) 0.0423(6) Uani 1 1 d . . . H3 H -0.1825 1.2176 0.3698 0.051 Uiso 1 1 calc R . . C4 C -0.1711(3) 1.0857(2) 0.42144(11) 0.0418(6) Uani 1 1 d . . . C5 C -0.1311(2) 0.9846(2) 0.41784(11) 0.0384(6) Uani 1 1 d . . . H5 H -0.1418 0.941 0.4539 0.046 Uiso 1 1 calc R . . C6 C -0.0753(2) 0.94365(18) 0.36315(10) 0.0313(5) Uani 1 1 d . . . C7 C -0.0755(3) 1.18939(19) 0.25910(11) 0.0481(7) Uani 1 1 d . . . H7A H -0.1201 1.2529 0.2695 0.072 Uiso 1 1 calc R . . H7B H -0.1267 1.148 0.2206 0.072 Uiso 1 1 calc R . . H7C H 0.0328 1.2172 0.2521 0.072 Uiso 1 1 calc R . . C8 C -0.2351(3) 1.1275(2) 0.48092(12) 0.0645(8) Uani 1 1 d . . . H8A H -0.3404 1.0854 0.4843 0.097 Uiso 1 1 calc R . . H8B H -0.2318 1.2075 0.4788 0.097 Uiso 1 1 calc R . . H8C H -0.1744 1.1167 0.5181 0.097 Uiso 1 1 calc R . . C9 C -0.0441(3) 0.82884(19) 0.36399(11) 0.0406(6) Uani 1 1 d . . . H9A H -0.0537 0.8031 0.407 0.061 Uiso 1 1 calc R . . H9B H 0.059 0.8323 0.3504 0.061 Uiso 1 1 calc R . . H9C H -0.1172 0.7764 0.3351 0.061 Uiso 1 1 calc R . . C10 C -0.0907(2) 0.80366(17) 0.11230(10) 0.0324(5) Uani 1 1 d . . . C11 C -0.2097(3) 0.71929(18) 0.08284(12) 0.0398(6) Uani 1 1 d . . . C12 C -0.2215(3) 0.7028(2) 0.01694(13) 0.0492(7) Uani 1 1 d . . . H12 H -0.3025 0.6455 -0.0019 0.059 Uiso 1 1 calc R . . C13 C -0.1209(3) 0.7657(2) -0.02162(12) 0.0507(7) Uani 1 1 d . . . C14 C -0.0046(3) 0.84774(19) 0.00728(11) 0.0429(6) Uani 1 1 d . . . H14 H 0.0658 0.8928 -0.0186 0.051 Uiso 1 1 calc R . . C15 C 0.0147(3) 0.86779(18) 0.07269(10) 0.0339(5) Uani 1 1 d . . . C16 C -0.3261(3) 0.6437(2) 0.12049(14) 0.0609(8) Uani 1 1 d . . . H16A H -0.3809 0.6891 0.1456 0.091 Uiso 1 1 calc R . . H16B H -0.275 0.6024 0.1488 0.091 Uiso 1 1 calc R . . H16C H -0.398 0.5904 0.0915 0.091 Uiso 1 1 calc R . . C17 C -0.1330(4) 0.7438(2) -0.09281(12) 0.0816(10) Uani 1 1 d . . . H17A H -0.1089 0.6718 -0.1039 0.122 Uiso 1 1 calc R . . H17B H -0.0614 0.8039 -0.1123 0.122 Uiso 1 1 calc R . . H17C H -0.2365 0.7414 -0.1084 0.122 Uiso 1 1 calc R . . C18 C 0.1514(3) 0.95604(19) 0.09740(11) 0.0421(6) Uani 1 1 d . . . H18A H 0.22 0.9771 0.0629 0.063 Uiso 1 1 calc R . . H18B H 0.204 0.9265 0.1311 0.063 Uiso 1 1 calc R . . H18C H 0.1193 1.0221 0.1142 0.063 Uiso 1 1 calc R . . C19 C 0.0054(3) 0.54394(18) 0.24997(11) 0.0392(6) Uani 1 1 d . . . H19A H -0.0925 0.5607 0.2376 0.047 Uiso 1 1 calc R . . H19B H 0.0032 0.4673 0.2323 0.047 Uiso 1 1 calc R . . C20 C 0.0190(3) 0.54541(19) 0.32170(11) 0.0437(6) Uani 1 1 d . . . H20A H 0.0565 0.6239 0.339 0.052 Uiso 1 1 calc R . . H20B H 0.0947 0.5034 0.334 0.052 Uiso 1 1 calc R . . C21 C -0.1312(3) 0.4941(2) 0.35106(13) 0.0577(8) Uani 1 1 d . . . H21A H -0.2057 0.5381 0.3404 0.069 Uiso 1 1 calc R . . H21B H -0.1709 0.4167 0.3325 0.069 Uiso 1 1 calc R . . C22 C -0.1155(4) 0.4915(3) 0.42222(14) 0.0889(11) Uani 1 1 d . . . H22A H -0.0418 0.448 0.4331 0.133 Uiso 1 1 calc R . . H22B H -0.2141 0.4565 0.4386 0.133 Uiso 1 1 calc R . . H22C H -0.0804 0.5683 0.441 0.133 Uiso 1 1 calc R . . C23 C 0.1205(3) 0.59819(18) 0.13043(10) 0.0358(5) Uani 1 1 d . . . H23A H 0.1148 0.5168 0.1255 0.043 Uiso 1 1 calc R . . H23B H 0.0196 0.6092 0.1175 0.043 Uiso 1 1 calc R . . C24 C 0.2359(3) 0.65774(19) 0.08537(11) 0.0406(6) Uani 1 1 d . . . H24A H 0.3368 0.6457 0.0972 0.049 Uiso 1 1 calc R . . H24B H 0.2428 0.7394 0.09 0.049 Uiso 1 1 calc R . . C25 C 0.1952(3) 0.6167(2) 0.01658(11) 0.0510(7) Uani 1 1 d . . . H25A H 0.1916 0.5355 0.0119 0.061 Uiso 1 1 calc R . . H25B H 0.0926 0.6262 0.0054 0.061 Uiso 1 1 calc R . . C26 C 0.3055(4) 0.6773(3) -0.02939(14) 0.0794(10) Uani 1 1 d . . . H26A H 0.3092 0.7577 -0.0254 0.119 Uiso 1 1 calc R . . H26B H 0.272 0.6477 -0.0727 0.119 Uiso 1 1 calc R . . H26C H 0.4068 0.6658 -0.0198 0.119 Uiso 1 1 calc R . . C27 C 0.3287(2) 0.59601(17) 0.23579(11) 0.0354(5) Uani 1 1 d . . . H27A H 0.4172 0.6503 0.2205 0.042 Uiso 1 1 calc R . . H27B H 0.3396 0.6011 0.2826 0.042 Uiso 1 1 calc R . . C28 C 0.3410(3) 0.47912(18) 0.21292(11) 0.0395(6) Uani 1 1 d . . . H28A H 0.2486 0.4237 0.2239 0.047 Uiso 1 1 calc R . . H28B H 0.346 0.4755 0.1662 0.047 Uiso 1 1 calc R . . C29 C 0.4791(3) 0.4476(2) 0.24154(12) 0.0482(7) Uani 1 1 d . . . H29A H 0.5705 0.5077 0.2349 0.058 Uiso 1 1 calc R . . H29B H 0.4683 0.4426 0.2877 0.058 Uiso 1 1 calc R . . C30 C 0.5018(3) 0.3370(2) 0.21333(14) 0.0713(9) Uani 1 1 d . . . H30A H 0.4132 0.2767 0.2209 0.107 Uiso 1 1 calc R . . H30B H 0.5927 0.3213 0.2332 0.107 Uiso 1 1 calc R . . H30C H 0.514 0.3417 0.1677 0.107 Uiso 1 1 calc R . . C31 C 0.4954(2) 1.02198(17) 0.23719(10) 0.0359(6) Uani 1 1 d . . . H31A H 0.4361 1.0744 0.2225 0.043 Uiso 1 1 calc R . . H31B H 0.5883 1.067 0.2603 0.043 Uiso 1 1 calc R . . C32 C 0.5407(2) 0.95914(18) 0.17985(10) 0.0351(5) Uani 1 1 d . . . H32A H 0.627 0.9276 0.1925 0.042 Uiso 1 1 calc R . . H32B H 0.4546 0.8957 0.1656 0.042 Uiso 1 1 calc R . . C33 C 0.5854(3) 1.0327(2) 0.12496(11) 0.0443(6) Uani 1 1 d . . . H33A H 0.501 1.0672 0.1136 0.053 Uiso 1 1 calc R . . H33B H 0.6749 1.0939 0.1384 0.053 Uiso 1 1 calc R . . C34 C 0.6225(3) 0.9682(2) 0.06719(12) 0.0639(8) Uani 1 1 d . . . H34A H 0.7141 0.9419 0.0765 0.096 Uiso 1 1 calc R . . H34B H 0.6398 1.0172 0.0318 0.096 Uiso 1 1 calc R . . H34C H 0.5375 0.9036 0.0558 0.096 Uiso 1 1 calc R . . C35 C 0.5163(2) 0.85287(17) 0.32324(10) 0.0307(5) Uani 1 1 d . . . H35A H 0.5431 0.8044 0.2888 0.037 Uiso 1 1 calc R . . H35B H 0.6105 0.9075 0.3391 0.037 Uiso 1 1 calc R . . C36 C 0.4513(2) 0.78041(18) 0.37700(10) 0.0347(5) Uani 1 1 d . . . H36A H 0.4424 0.8303 0.4142 0.042 Uiso 1 1 calc R . . H36B H 0.3478 0.7366 0.3636 0.042 Uiso 1 1 calc R . . C37 C 0.5448(3) 0.70001(19) 0.39680(11) 0.0440(6) Uani 1 1 d . . . H37A H 0.6439 0.7437 0.4155 0.053 Uiso 1 1 calc R . . H37B H 0.5645 0.656 0.3588 0.053 Uiso 1 1 calc R . . C38 C 0.4673(3) 0.6199(2) 0.44450(13) 0.0622(8) Uani 1 1 d . . . H38A H 0.4514 0.6628 0.483 0.093 Uiso 1 1 calc R . . H38B H 0.5312 0.5689 0.455 0.093 Uiso 1 1 calc R . . H38C H 0.3691 0.5763 0.4263 0.093 Uiso 1 1 calc R . . C39 C 0.3724(3) 1.02227(18) 0.36113(11) 0.0393(6) Uani 1 1 d . . . H39A H 0.2937 0.9813 0.3883 0.047 Uiso 1 1 calc R . . H39B H 0.4705 1.0369 0.3856 0.047 Uiso 1 1 calc R . . C40 C 0.3378(3) 1.13436(18) 0.34985(11) 0.0415(6) Uani 1 1 d . . . H40A H 0.2556 1.1234 0.3166 0.05 Uiso 1 1 calc R . . H40B H 0.4291 1.1851 0.3342 0.05 Uiso 1 1 calc R . . C41 C 0.2901(3) 1.1893(2) 0.40922(13) 0.0554(7) Uani 1 1 d . . . H41A H 0.1947 1.1408 0.423 0.067 Uiso 1 1 calc R . . H41B H 0.3689 1.1946 0.4434 0.067 Uiso 1 1 calc R . . C42 C 0.2660(4) 1.3049(2) 0.40060(15) 0.0744(9) Uani 1 1 d . . . H42A H 0.3623 1.3555 0.3909 0.112 Uiso 1 1 calc R . . H42B H 0.2287 1.3331 0.4396 0.112 Uiso 1 1 calc R . . H42C H 0.1913 1.3012 0.3656 0.112 Uiso 1 1 calc R . . P1 P 0.03410(7) 0.97936(5) 0.23448(3) 0.03049(14) Uani 1 1 d . . . P2 P -0.09485(6) 0.81651(5) 0.20013(3) 0.03231(14) Uani 1 1 d . . . P3 P 0.15900(6) 0.64377(5) 0.21409(3) 0.03137(14) Uani 1 1 d . . . P4 P 0.38286(6) 0.92862(4) 0.29157(3) 0.02875(13) Uani 1 1 d . . . Pd1 Pd 0.154770(19) 0.828189(14) 0.241893(8) 0.02669(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 C1 0.0266(12) 0.0336(12) 0.0272(12) 0.0018(10) 0.0040(10) 0.0078(9) C2 0.0388(14) 0.0344(13) 0.0308(13) -0.0001(10) 0.0058(11) 0.0114(10) C3 0.0484(16) 0.0389(14) 0.0420(15) -0.0055(12) 0.0097(13) 0.0163(12) C4 0.0405(15) 0.0536(16) 0.0287(13) -0.0072(12) 0.0075(11) 0.0080(12) C5 0.0351(14) 0.0502(15) 0.0279(13) 0.0063(11) 0.0058(11) 0.0049(11) C6 0.0250(12) 0.0399(13) 0.0281(12) 0.0031(10) 0.0034(10) 0.0052(10) C7 0.0707(18) 0.0388(14) 0.0440(15) 0.0084(12) 0.0167(14) 0.0281(13) C8 0.082(2) 0.078(2) 0.0355(16) -0.0090(14) 0.0178(15) 0.0236(17) C9 0.0412(15) 0.0490(15) 0.0370(14) 0.0177(12) 0.0118(12) 0.0171(12) C10 0.0339(13) 0.0330(12) 0.0348(13) -0.0013(10) -0.0045(11) 0.0180(10) C11 0.0349(14) 0.0335(13) 0.0532(16) -0.0043(12) -0.0077(12) 0.0151(11) C12 0.0544(17) 0.0375(14) 0.0564(18) -0.0154(13) -0.0238(14) 0.0198(12) C13 0.081(2) 0.0378(15) 0.0393(15) -0.0086(12) -0.0151(15) 0.0309(14) C14 0.0671(18) 0.0369(14) 0.0286(13) 0.0004(11) -0.0014(13) 0.0211(13) C15 0.0427(14) 0.0336(12) 0.0296(13) -0.0018(10) -0.0018(11) 0.0189(11) C16 0.0402(16) 0.0581(18) 0.076(2) -0.0079(16) -0.0058(15) -0.0001(13) C17 0.152(3) 0.0516(18) 0.0407(17) -0.0165(14) -0.0266(19) 0.0324(19) C18 0.0455(15) 0.0489(15) 0.0296(13) 0.0044(11) 0.0102(12) 0.0056(12) C19 0.0380(14) 0.0317(12) 0.0475(15) 0.0011(11) 0.0028(12) 0.0078(10) C20 0.0467(16) 0.0374(14) 0.0500(16) 0.0105(12) 0.0048(13) 0.0139(11) C21 0.0650(19) 0.0474(16) 0.0600(19) 0.0102(14) 0.0163(16) 0.0088(14) C22 0.113(3) 0.088(2) 0.066(2) 0.0211(19) 0.033(2) 0.018(2) C23 0.0371(14) 0.0318(12) 0.0404(14) -0.0005(11) -0.0019(11) 0.0132(10) C24 0.0419(15) 0.0435(14) 0.0401(15) 0.0011(12) 0.0012(12) 0.0177(11) C25 0.0686(19) 0.0478(16) 0.0419(16) -0.0013(13) 0.0016(14) 0.0253(14) C26 0.093(3) 0.106(3) 0.0436(18) 0.0078(18) 0.0186(18) 0.029(2) C27 0.0348(13) 0.0339(13) 0.0399(14) 0.0013(11) -0.0001(11) 0.0136(10) C28 0.0484(15) 0.0314(13) 0.0424(15) -0.0025(11) -0.0013(12) 0.0184(11) C29 0.0544(17) 0.0473(15) 0.0526(17) 0.0065(13) 0.0021(14) 0.0305(13) C30 0.093(2) 0.0630(19) 0.077(2) 0.0065(17) 0.0053(19) 0.0548(18) C31 0.0355(14) 0.0346(13) 0.0361(14) 0.0070(11) 0.0052(11) 0.0037(10) C32 0.0321(13) 0.0397(13) 0.0367(14) 0.0106(11) 0.0093(11) 0.0122(10) C33 0.0431(15) 0.0494(15) 0.0394(15) 0.0155(12) 0.0081(12) 0.0055(12) C34 0.073(2) 0.085(2) 0.0489(18) 0.0234(16) 0.0271(16) 0.0411(17) C35 0.0271(12) 0.0337(12) 0.0311(12) -0.0001(10) -0.0006(10) 0.0074(10) C36 0.0382(14) 0.0356(13) 0.0305(13) 0.0008(10) 0.0033(11) 0.0093(10) C37 0.0506(16) 0.0420(14) 0.0411(15) 0.0061(12) -0.0077(12) 0.0149(12) C38 0.076(2) 0.0456(16) 0.0641(19) 0.0175(14) -0.0072(16) 0.0106(14) C39 0.0472(15) 0.0382(13) 0.0326(13) -0.0001(11) 0.0056(12) 0.0104(11) C40 0.0464(15) 0.0321(13) 0.0434(15) -0.0041(11) 0.0045(12) 0.0054(11) C41 0.0670(19) 0.0440(16) 0.0544(18) -0.0108(13) 0.0080(15) 0.0138(14) C42 0.091(2) 0.0489(18) 0.084(2) -0.0205(16) 0.0046(19) 0.0235(16) P1 0.0368(4) 0.0319(3) 0.0271(3) 0.0045(3) 0.0081(3) 0.0152(3) P2 0.0261(3) 0.0376(3) 0.0352(3) 0.0044(3) 0.0026(3) 0.0107(3) P3 0.0307(3) 0.0274(3) 0.0371(4) 0.0023(3) 0.0011(3) 0.0090(3) P4 0.0300(3) 0.0277(3) 0.0287(3) 0.0030(2) 0.0043(3) 0.0066(2) Pd1 0.02622(10) 0.02660(9) 0.02912(10) 0.00340(7) 0.00352(7) 0.00939(7) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 C1 C6 1.408(3) . ? C1 C2 1.409(3) . ? C1 P1 1.866(2) . ? C2 C3 1.392(3) . ? C2 C7 1.516(3) . ? C3 C4 1.385(3) . ? C4 C5 1.376(3) . ? C4 C8 1.519(3) . ? C5 C6 1.395(3) . ? C6 C9 1.506(3) . ? C10 C11 1.411(3) . ? C10 C15 1.415(3) . ? C10 P2 1.860(2) . ? C11 C12 1.396(3) . ? C11 C16 1.511(3) . ? C12 C13 1.371(4) . ? C13 C14 1.376(3) . ? C13 C17 1.513(3) . ? C14 C15 1.392(3) . ? C15 C18 1.500(3) . ? C19 C20 1.519(3) . ? C19 P3 1.839(2) . ? C20 C21 1.526(3) . ? C21 C22 1.512(4) . ? C23 C24 1.522(3) . ? C23 P3 1.827(2) . ? C24 C25 1.521(3) . ? C25 C26 1.513(3) . ? C27 C28 1.523(3) . ? C27 P3 1.830(2) . ? C28 C29 1.517(3) . ? C29 C30 1.518(3) . ? C31 C32 1.524(3) . ? C31 P4 1.829(2) . ? C32 C33 1.517(3) . ? C33 C34 1.513(3) . ? C35 C36 1.529(3) . ? C35 P4 1.828(2) . ? C36 C37 1.515(3) . ? C37 C38 1.519(3) . ? C39 C40 1.514(3) . ? C39 P4 1.840(2) . ? C40 C41 1.519(3) . ? C41 C42 1.509(3) . ? P1 P2 2.1416(9) . ? P1 Pd1 2.3818(6) . ? P2 Pd1 2.3770(9) . ? P3 Pd1 2.3222(6) . ? P4 Pd1 2.3304(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C6 C1 C2 118.20(19) . . ? C6 C1 P1 127.93(16) . . ? C2 C1 P1 113.65(15) . . ? C3 C2 C1 120.0(2) . . ? C3 C2 C7 117.4(2) . . ? C1 C2 C7 122.65(19) . . ? C4 C3 C2 121.9(2) . . ? C5 C4 C3 117.9(2) . . ? C5 C4 C8 121.6(2) . . ? C3 C4 C8 120.6(2) . . ? C4 C5 C6 122.4(2) . . ? C5 C6 C1 119.6(2) . . ? C5 C6 C9 117.23(19) . . ? C1 C6 C9 123.09(19) . . ? C11 C10 C15 117.5(2) . . ? C11 C10 P2 114.33(17) . . ? C15 C10 P2 128.21(17) . . ? C12 C11 C10 120.0(2) . . ? C12 C11 C16 118.0(2) . . ? C10 C11 C16 122.0(2) . . ? C13 C12 C11 122.7(2) . . ? C12 C13 C14 117.1(2) . . ? C12 C13 C17 121.7(3) . . ? C14 C13 C17 121.1(3) . . ? C13 C14 C15 123.1(2) . . ? C14 C15 C10 119.6(2) . . ? C14 C15 C18 117.0(2) . . ? C10 C15 C18 123.39(19) . . ? C20 C19 P3 114.64(16) . . ? C19 C20 C21 112.9(2) . . ? C22 C21 C20 112.6(2) . . ? C24 C23 P3 115.61(16) . . ? C23 C24 C25 112.6(2) . . ? C26 C25 C24 113.7(2) . . ? C28 C27 P3 119.66(16) . . ? C29 C28 C27 112.85(19) . . ? C30 C29 C28 113.0(2) . . ? C32 C31 P4 112.95(15) . . ? C33 C32 C31 113.08(18) . . ? C34 C33 C32 112.6(2) . . ? C36 C35 P4 112.33(14) . . ? C37 C36 C35 114.37(18) . . ? C36 C37 C38 112.8(2) . . ? C40 C39 P4 117.89(16) . . ? C39 C40 C41 112.6(2) . . ? C42 C41 C40 113.8(2) . . ? C1 P1 P2 104.18(7) . . ? C1 P1 Pd1 111.74(7) . . ? P2 P1 Pd1 63.14(3) . . ? C10 P2 P1 109.44(7) . . ? C10 P2 Pd1 107.70(7) . . ? P1 P2 Pd1 63.37(3) . . ? C23 P3 C27 104.18(10) . . ? C23 P3 C19 100.64(11) . . ? C27 P3 C19 103.53(10) . . ? C23 P3 Pd1 116.32(7) . . ? C27 P3 Pd1 118.44(7) . . ? C19 P3 Pd1 111.55(8) . . ? C35 P4 C31 103.56(10) . . ? C35 P4 C39 99.86(11) . . ? C31 P4 C39 103.66(10) . . ? C35 P4 Pd1 119.45(7) . . ? C31 P4 Pd1 110.76(8) . . ? C39 P4 Pd1 117.50(8) . . ? P3 Pd1 P4 112.04(2) . . ? P3 Pd1 P2 96.41(3) . . ? P4 Pd1 P2 151.53(2) . . ? P3 Pd1 P1 149.30(2) . . ? P4 Pd1 P1 98.10(3) . . ? P2 Pd1 P1 53.49(2) . . ? #============================================================================ data_x0017fin _database_code_depnum_ccdc_archive 'CCDC 655523' _audit_creation_date 2006-10-15T01:27:51-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_sum 'C41 H52 P4 Pd' _chemical_formula_weight 775.11 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _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 11.3887(16) _cell_length_b 12.423(2) _cell_length_c 15.829(3) _cell_angle_alpha 84.327(17) _cell_angle_beta 72.773(18) _cell_angle_gamma 66.212(16) _cell_volume 1956.7(6) _cell_formula_units_Z 2 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 19761 _cell_measurement_theta_min 2.6873 _cell_measurement_theta_max 28.4559 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description plates _exptl_crystal_colour yellow _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 1.316 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 808 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.665 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.5 (release 28-08-2006 CrysAlis171 .NET) (compiled Aug 28 2006,13:05:05) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_correction_T_min 0.90726 _exptl_absorpt_correction_T_max 1 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_detector_area_resol_mean 16.356 _diffrn_orient_matrix_ub_11 0.0551485537 _diffrn_orient_matrix_ub_12 0.0169010986 _diffrn_orient_matrix_ub_13 -0.0113606651 _diffrn_orient_matrix_ub_21 -0.0400067849 _diffrn_orient_matrix_ub_22 0.0523340992 _diffrn_orient_matrix_ub_23 0.0259615502 _diffrn_orient_matrix_ub_31 0.0194934242 _diffrn_orient_matrix_ub_32 -0.0294037425 _diffrn_orient_matrix_ub_33 0.0373701038 _diffrn_measurement_device_type 'ccd xcalibur s' _diffrn_measurement_method '\w scans and \f scans' _diffrn_reflns_av_R_equivalents 0.0324 _diffrn_reflns_av_unetI/netI 0.047 _diffrn_reflns_number 39060 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.7 _diffrn_reflns_theta_max 28.54 _diffrn_reflns_theta_full 28.54 _diffrn_measured_fraction_theta_full 0.887 _diffrn_measured_fraction_theta_max 0.887 _reflns_number_total 8848 _reflns_number_gt 6989 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.31.5 (release 28-08-2006 CrysAlis171 .NET) (compiled Aug 28 2006,13:05:05) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.5 (release 28-08-2006 CrysAlis171 .NET) (compiled Aug 28 2006,13:05:05) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.5 (release 28-08-2006 CrysAlis171 .NET) (compiled Aug 28 2006,13:05:05) ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP3 for Windows (L. J. Farrugia, 1997)' _computing_publication_material 'WINGX (L.J. Farrugia,1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0364P)^2^+0.4071P] 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 8848 _refine_ls_number_parameters 426 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0469 _refine_ls_R_factor_gt 0.0301 _refine_ls_wR_factor_ref 0.0712 _refine_ls_wR_factor_gt 0.0656 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.023 _refine_ls_shift/su_max 0.008 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.056 _refine_diff_density_min -0.467 _refine_diff_density_rms 0.065 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' 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 C1 C 0.0492(2) 0.75423(19) 0.08280(14) 0.0225(5) Uani 1 1 d . . . C2 C -0.0272(2) 0.8417(2) 0.03451(15) 0.0270(5) Uani 1 1 d . . . C3 C 0.0303(3) 0.8528(2) -0.05542(15) 0.0338(6) Uani 1 1 d . . . H3 H -0.0226 0.9111 -0.0876 0.041 Uiso 1 1 calc R . . C4 C 0.1598(3) 0.7832(2) -0.09940(15) 0.0347(6) Uani 1 1 d . . . C5 C 0.2354(2) 0.7004(2) -0.05117(15) 0.0324(6) Uani 1 1 d . . . H5 H 0.3258 0.6527 -0.0799 0.039 Uiso 1 1 calc R . . C6 C 0.1832(2) 0.6846(2) 0.03855(14) 0.0269(5) Uani 1 1 d . . . C7 C -0.1696(2) 0.9248(2) 0.07371(16) 0.0336(6) Uani 1 1 d . . . H7A H -0.2028 0.9764 0.0276 0.05 Uiso 1 1 calc R . . H7B H -0.1738 0.9726 0.121 0.05 Uiso 1 1 calc R . . H7C H -0.225 0.8796 0.098 0.05 Uiso 1 1 calc R . . C8 C 0.2161(3) 0.7951(3) -0.19764(17) 0.0549(8) Uani 1 1 d . . . H8A H 0.1925 0.7479 -0.2307 0.082 Uiso 1 1 calc R . . H8B H 0.3136 0.7672 -0.2124 0.082 Uiso 1 1 calc R . . H8C H 0.1785 0.8779 -0.2134 0.082 Uiso 1 1 calc R . . C9 C 0.2753(2) 0.5909(2) 0.08433(16) 0.0351(6) Uani 1 1 d . . . H9A H 0.3656 0.5585 0.0436 0.053 Uiso 1 1 calc R . . H9B H 0.2426 0.5278 0.1024 0.053 Uiso 1 1 calc R . . H9C H 0.2773 0.6254 0.1367 0.053 Uiso 1 1 calc R . . C10 C -0.1226(2) 0.8270(2) 0.39387(14) 0.0226(5) Uani 1 1 d . . . C11 C -0.1228(2) 0.7229(2) 0.43842(14) 0.0277(5) Uani 1 1 d . . . C12 C -0.1247(2) 0.7134(2) 0.52740(15) 0.0342(6) Uani 1 1 d . . . H12 H -0.1261 0.6434 0.557 0.041 Uiso 1 1 calc R . . C13 C -0.1248(2) 0.8014(2) 0.57427(15) 0.0361(6) Uani 1 1 d . . . C14 C -0.1258(2) 0.9031(2) 0.53081(15) 0.0333(6) Uani 1 1 d . . . H14 H -0.1266 0.965 0.5621 0.04 Uiso 1 1 calc R . . C15 C -0.1258(2) 0.9187(2) 0.44200(14) 0.0266(5) Uani 1 1 d . . . C16 C -0.1211(3) 0.6189(2) 0.39563(16) 0.0343(6) Uani 1 1 d . . . H16A H -0.0344 0.5813 0.3518 0.052 Uiso 1 1 calc R . . H16B H -0.1924 0.6456 0.3664 0.052 Uiso 1 1 calc R . . H16C H -0.1352 0.5621 0.4409 0.052 Uiso 1 1 calc R . . C17 C -0.1232(3) 0.7861(3) 0.67040(16) 0.0535(8) Uani 1 1 d . . . H17A H -0.0326 0.7673 0.6739 0.08 Uiso 1 1 calc R . . H17B H -0.1512 0.722 0.6953 0.08 Uiso 1 1 calc R . . H17C H -0.1849 0.8592 0.704 0.08 Uiso 1 1 calc R . . C18 C -0.1305(2) 1.0355(2) 0.40219(16) 0.0339(6) Uani 1 1 d . . . H18A H -0.1284 1.0846 0.446 0.051 Uiso 1 1 calc R . . H18B H -0.213 1.0753 0.3845 0.051 Uiso 1 1 calc R . . H18C H -0.0532 1.0223 0.3502 0.051 Uiso 1 1 calc R . . C19 C -0.4893(3) 1.0397(2) 0.3321(2) 0.0475(7) Uani 1 1 d . . . H19A H -0.5829 1.0823 0.3652 0.071 Uiso 1 1 calc R . . H19B H -0.4709 1.0749 0.274 0.071 Uiso 1 1 calc R . . H19C H -0.4309 1.0446 0.3649 0.071 Uiso 1 1 calc R . . C20 C -0.5114(3) 0.8424(3) 0.43071(16) 0.0508(8) Uani 1 1 d . . . H20A H -0.6025 0.8976 0.4592 0.076 Uiso 1 1 calc R . . H20B H -0.4507 0.8434 0.4632 0.076 Uiso 1 1 calc R . . H20C H -0.5097 0.7629 0.4308 0.076 Uiso 1 1 calc R . . C21 C -0.5893(2) 0.89783(19) 0.26882(15) 0.0251(5) Uani 1 1 d . . . C22 C -0.6838(2) 0.8494(2) 0.30604(17) 0.0340(6) Uani 1 1 d . . . H22 H -0.6854 0.8127 0.3617 0.041 Uiso 1 1 calc R . . C23 C -0.7750(2) 0.8541(2) 0.2633(2) 0.0427(7) Uani 1 1 d . . . H23 H -0.8379 0.8197 0.2892 0.051 Uiso 1 1 calc R . . C24 C -0.7752(3) 0.9081(2) 0.1834(2) 0.0464(7) Uani 1 1 d . . . H24 H -0.8385 0.9117 0.1542 0.056 Uiso 1 1 calc R . . C25 C -0.6831(3) 0.9573(2) 0.14575(19) 0.0452(7) Uani 1 1 d . . . H25 H -0.6836 0.9956 0.0908 0.054 Uiso 1 1 calc R . . C26 C -0.5897(2) 0.9509(2) 0.18787(16) 0.0350(6) Uani 1 1 d . . . H26 H -0.5252 0.9833 0.1608 0.042 Uiso 1 1 calc R . . C27 C -0.1138(3) 0.4913(2) 0.13874(18) 0.0410(6) Uani 1 1 d . . . H27A H -0.1307 0.4354 0.1095 0.062 Uiso 1 1 calc R . . H27B H -0.0868 0.4559 0.1917 0.062 Uiso 1 1 calc R . . H27C H -0.0421 0.5112 0.098 0.062 Uiso 1 1 calc R . . C28 C -0.3863(3) 0.5644(2) 0.23414(17) 0.0428(7) Uani 1 1 d . . . H28A H -0.4755 0.6279 0.251 0.064 Uiso 1 1 calc R . . H28B H -0.3615 0.5282 0.2875 0.064 Uiso 1 1 calc R . . H28C H -0.3869 0.5049 0.1981 0.064 Uiso 1 1 calc R . . C29 C -0.3082(2) 0.6681(2) 0.06741(15) 0.0284(5) Uani 1 1 d . . . C30 C -0.4343(3) 0.6923(2) 0.05876(19) 0.0419(6) Uani 1 1 d . . . H30 H -0.5005 0.6799 0.1069 0.05 Uiso 1 1 calc R . . C31 C -0.4634(3) 0.7349(3) -0.0206(2) 0.0568(9) Uani 1 1 d . . . H31 H -0.5498 0.7518 -0.0264 0.068 Uiso 1 1 calc R . . C32 C -0.3685(4) 0.7522(3) -0.0902(2) 0.0588(9) Uani 1 1 d . . . H32 H -0.3892 0.7809 -0.1442 0.071 Uiso 1 1 calc R . . C33 C -0.2438(3) 0.7287(3) -0.08286(18) 0.0530(8) Uani 1 1 d . . . H33 H -0.178 0.7403 -0.1317 0.064 Uiso 1 1 calc R . . C34 C -0.2140(3) 0.6884(2) -0.00488(16) 0.0387(6) Uani 1 1 d . . . H34 H -0.1279 0.6741 0.0002 0.046 Uiso 1 1 calc R . . C35 C 0.7061(4) 0.4485(4) 0.5491(4) 0.1010(18) Uani 1 1 d . . . C36 C 0.7666(4) 0.4236(5) 0.6196(4) 0.105(2) Uani 1 1 d . . . H36 H 0.8393 0.3514 0.6217 0.126 Uiso 1 1 calc R . . C37 C 0.7120(8) 0.5130(9) 0.6869(5) 0.176(4) Uani 1 1 d . . . H37 H 0.7527 0.4987 0.7335 0.212 Uiso 1 1 calc R . . C38 C 0.6139(6) 0.6096(6) 0.6891(4) 0.117(2) Uani 1 1 d . . . H38 H 0.5818 0.6651 0.7362 0.14 Uiso 1 1 calc R . . C39 C 0.5526(4) 0.6332(4) 0.6195(3) 0.0791(11) Uani 1 1 d . . . H39 H 0.4781 0.7051 0.62 0.095 Uiso 1 1 calc R . . C40 C 0.5994(3) 0.5545(3) 0.5530(3) 0.0653(10) Uani 1 1 d . . . H40 H 0.5574 0.5725 0.5068 0.078 Uiso 1 1 calc R . . C41 C 0.7554(5) 0.3663(4) 0.4809(4) 0.141(3) Uani 1 1 d . . . H41A H 0.6829 0.3468 0.4751 0.212 Uiso 1 1 calc R . . H41B H 0.826 0.295 0.4938 0.212 Uiso 1 1 calc R . . H41C H 0.7922 0.3991 0.4254 0.212 Uiso 1 1 calc R . . P1 P -0.00832(5) 0.70777(5) 0.19797(4) 0.02363(13) Uani 1 1 d . . . P2 P -0.12558(6) 0.86558(5) 0.27734(4) 0.02313(13) Uani 1 1 d . . . P3 P -0.45810(5) 0.88553(5) 0.31745(4) 0.02485(13) Uani 1 1 d . . . P4 P -0.26519(6) 0.62423(5) 0.17037(4) 0.02618(13) Uani 1 1 d . . . Pd1 Pd -0.244875(16) 0.768560(15) 0.239213(11) 0.02069(6) 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 C1 0.0247(11) 0.0246(12) 0.0227(11) -0.0005(9) -0.0068(9) -0.0139(9) C2 0.0319(12) 0.0266(12) 0.0262(12) 0.0031(10) -0.0097(10) -0.0148(10) C3 0.0482(15) 0.0288(13) 0.0267(12) 0.0068(10) -0.0124(11) -0.0177(12) C4 0.0506(16) 0.0303(14) 0.0235(12) -0.0006(11) -0.0019(11) -0.0220(12) C5 0.0345(13) 0.0329(14) 0.0289(13) -0.0085(11) 0.0002(10) -0.0169(11) C6 0.0292(12) 0.0293(13) 0.0264(12) -0.0033(10) -0.0051(9) -0.0166(10) C7 0.0342(13) 0.0330(14) 0.0309(13) 0.0091(11) -0.0128(10) -0.0097(11) C8 0.079(2) 0.0456(18) 0.0277(14) 0.0026(13) 0.0021(14) -0.0251(16) C9 0.0235(12) 0.0405(15) 0.0323(13) -0.0019(11) -0.0037(10) -0.0059(11) C10 0.0158(10) 0.0301(12) 0.0215(11) 0.0020(9) -0.0061(8) -0.0083(9) C11 0.0231(11) 0.0358(14) 0.0245(12) 0.0044(10) -0.0084(9) -0.0117(10) C12 0.0278(12) 0.0435(15) 0.0245(12) 0.0081(11) -0.0053(10) -0.0103(11) C13 0.0259(12) 0.0504(17) 0.0207(12) -0.0023(12) -0.0051(10) -0.0041(11) C14 0.0269(12) 0.0410(15) 0.0265(12) -0.0090(11) -0.0077(10) -0.0054(11) C15 0.0188(10) 0.0342(13) 0.0248(12) -0.0045(10) -0.0064(9) -0.0071(10) C16 0.0434(14) 0.0345(14) 0.0330(13) 0.0108(11) -0.0150(11) -0.0225(12) C17 0.0545(18) 0.070(2) 0.0216(13) -0.0006(14) -0.0113(12) -0.0092(16) C18 0.0377(14) 0.0334(14) 0.0340(13) -0.0063(11) -0.0120(11) -0.0143(11) C19 0.0327(14) 0.0368(15) 0.074(2) -0.0209(14) -0.0192(14) -0.0064(12) C20 0.0354(15) 0.083(2) 0.0255(13) 0.0039(14) -0.0093(11) -0.0154(15) C21 0.0211(11) 0.0240(12) 0.0289(12) -0.0032(10) -0.0082(9) -0.0059(9) C22 0.0254(12) 0.0326(14) 0.0430(14) 0.0039(11) -0.0112(11) -0.0101(10) C23 0.0264(13) 0.0355(15) 0.070(2) -0.0007(14) -0.0191(13) -0.0121(11) C24 0.0399(15) 0.0344(15) 0.074(2) -0.0044(15) -0.0380(15) -0.0071(12) C25 0.0541(17) 0.0398(16) 0.0456(16) 0.0056(13) -0.0317(14) -0.0109(14) C26 0.0368(14) 0.0338(14) 0.0377(14) 0.0035(11) -0.0158(11) -0.0143(11) C27 0.0398(15) 0.0288(14) 0.0529(17) -0.0092(12) -0.0174(13) -0.0066(11) C28 0.0513(16) 0.0421(16) 0.0412(15) -0.0002(13) -0.0050(13) -0.0300(14) C29 0.0308(12) 0.0238(12) 0.0321(12) -0.0079(10) -0.0097(10) -0.0098(10) C30 0.0386(15) 0.0441(16) 0.0508(17) -0.0046(13) -0.0202(13) -0.0174(13) C31 0.063(2) 0.0460(18) 0.075(2) -0.0051(17) -0.0471(19) -0.0147(16) C32 0.099(3) 0.0405(18) 0.0459(18) 0.0028(14) -0.0429(19) -0.0211(18) C33 0.080(2) 0.0492(19) 0.0321(15) 0.0025(13) -0.0158(15) -0.0282(17) C34 0.0441(15) 0.0406(15) 0.0321(14) -0.0050(12) -0.0081(11) -0.0177(13) C35 0.040(2) 0.054(2) 0.178(5) 0.036(3) 0.007(3) -0.0216(18) C36 0.036(2) 0.103(4) 0.175(6) 0.102(4) -0.050(3) -0.034(2) C37 0.125(6) 0.299(12) 0.170(7) 0.173(8) -0.086(6) -0.154(8) C38 0.096(4) 0.180(6) 0.103(4) 0.069(4) -0.039(3) -0.090(4) C39 0.066(2) 0.090(3) 0.083(3) 0.029(3) -0.024(2) -0.036(2) C40 0.0335(16) 0.051(2) 0.095(3) 0.038(2) -0.0156(17) -0.0104(14) C41 0.070(3) 0.050(3) 0.267(7) -0.027(4) 0.027(4) -0.032(2) P1 0.0193(3) 0.0277(3) 0.0225(3) 0.0025(2) -0.0054(2) -0.0086(2) P2 0.0257(3) 0.0269(3) 0.0218(3) 0.0013(2) -0.0090(2) -0.0139(2) P3 0.0189(3) 0.0294(3) 0.0254(3) -0.0035(3) -0.0071(2) -0.0071(2) P4 0.0261(3) 0.0259(3) 0.0284(3) -0.0044(3) -0.0063(2) -0.0120(3) Pd1 0.01800(8) 0.02395(9) 0.02172(9) -0.00252(6) -0.00582(6) -0.00901(7) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 C1 C2 1.410(3) . ? C1 C6 1.410(3) . ? C1 P1 1.864(2) . ? C2 C3 1.399(3) . ? C2 C7 1.504(3) . ? C3 C4 1.375(4) . ? C4 C5 1.379(4) . ? C4 C8 1.514(3) . ? C5 C6 1.396(3) . ? C6 C9 1.509(3) . ? C10 C11 1.410(3) . ? C10 C15 1.415(3) . ? C10 P2 1.866(2) . ? C11 C12 1.396(3) . ? C11 C16 1.508(3) . ? C12 C13 1.380(4) . ? C13 C14 1.375(4) . ? C13 C17 1.519(3) . ? C14 C15 1.400(3) . ? C15 C18 1.511(3) . ? C19 P3 1.827(3) . ? C20 P3 1.816(3) . ? C21 C26 1.382(3) . ? C21 C22 1.394(3) . ? C21 P3 1.823(2) . ? C22 C23 1.379(3) . ? C23 C24 1.372(4) . ? C24 C25 1.380(4) . ? C25 C26 1.387(3) . ? C27 P4 1.818(3) . ? C28 P4 1.824(2) . ? C29 C30 1.389(3) . ? C29 C34 1.400(3) . ? C29 P4 1.810(2) . ? C30 C31 1.394(4) . ? C31 C32 1.365(5) . ? C32 C33 1.368(5) . ? C33 C34 1.371(4) . ? C35 C40 1.377(5) . ? C35 C41 1.385(7) . ? C35 C36 1.424(7) . ? C36 C37 1.429(10) . ? C37 C38 1.262(9) . ? C38 C39 1.419(6) . ? C39 C40 1.342(5) . ? P1 P2 2.1414(10) . ? P1 Pd1 2.3809(7) . ? P2 Pd1 2.3691(6) . ? P3 Pd1 2.2957(9) . ? P4 Pd1 2.3078(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 C6 118.0(2) . . ? C2 C1 P1 127.94(16) . . ? C6 C1 P1 113.79(16) . . ? C3 C2 C1 119.2(2) . . ? C3 C2 C7 116.9(2) . . ? C1 C2 C7 123.9(2) . . ? C4 C3 C2 123.0(2) . . ? C5 C4 C3 117.6(2) . . ? C5 C4 C8 121.3(2) . . ? C3 C4 C8 121.1(2) . . ? C4 C5 C6 122.1(2) . . ? C5 C6 C1 120.1(2) . . ? C5 C6 C9 117.3(2) . . ? C1 C6 C9 122.5(2) . . ? C11 C10 C15 118.21(19) . . ? C11 C10 P2 128.54(17) . . ? C15 C10 P2 113.20(16) . . ? C12 C11 C10 119.3(2) . . ? C12 C11 C16 116.8(2) . . ? C10 C11 C16 123.86(19) . . ? C13 C12 C11 122.8(2) . . ? C14 C13 C12 117.7(2) . . ? C14 C13 C17 121.2(3) . . ? C12 C13 C17 121.1(3) . . ? C13 C14 C15 122.2(2) . . ? C14 C15 C10 119.8(2) . . ? C14 C15 C18 117.3(2) . . ? C10 C15 C18 122.93(19) . . ? C26 C21 C22 118.2(2) . . ? C26 C21 P3 118.29(17) . . ? C22 C21 P3 123.39(18) . . ? C23 C22 C21 121.0(2) . . ? C24 C23 C22 120.3(2) . . ? C23 C24 C25 119.6(2) . . ? C24 C25 C26 120.2(3) . . ? C21 C26 C25 120.7(2) . . ? C30 C29 C34 118.2(2) . . ? C30 C29 P4 123.07(19) . . ? C34 C29 P4 118.49(18) . . ? C29 C30 C31 119.9(3) . . ? C32 C31 C30 120.4(3) . . ? C31 C32 C33 120.5(3) . . ? C34 C33 C32 119.9(3) . . ? C33 C34 C29 121.1(3) . . ? C40 C35 C41 123.1(6) . . ? C40 C35 C36 117.4(5) . . ? C41 C35 C36 119.5(5) . . ? C37 C36 C35 116.4(5) . . ? C38 C37 C36 125.0(7) . . ? C37 C38 C39 118.4(7) . . ? C40 C39 C38 120.2(5) . . ? C39 C40 C35 122.5(5) . . ? C1 P1 P2 106.64(8) . . ? C1 P1 Pd1 109.28(7) . . ? P2 P1 Pd1 62.92(3) . . ? C10 P2 P1 107.45(8) . . ? C10 P2 Pd1 106.74(7) . . ? P1 P2 Pd1 63.49(3) . . ? C20 P3 C21 105.00(12) . . ? C20 P3 C19 102.03(15) . . ? C21 P3 C19 102.03(11) . . ? C20 P3 Pd1 115.04(10) . . ? C21 P3 Pd1 115.26(7) . . ? C19 P3 Pd1 115.71(9) . . ? C29 P4 C27 103.08(12) . . ? C29 P4 C28 104.70(12) . . ? C27 P4 C28 101.54(13) . . ? C29 P4 Pd1 114.24(8) . . ? C27 P4 Pd1 114.77(9) . . ? C28 P4 Pd1 116.76(9) . . ? P3 Pd1 P4 105.88(3) . . ? P3 Pd1 P2 99.38(3) . . ? P4 Pd1 P2 154.73(2) . . ? P3 Pd1 P1 152.72(2) . . ? P4 Pd1 P1 101.16(3) . . ? P2 Pd1 P1 53.59(2) . . ? #=======================================================================_eof # End of Crystallographic Information File