# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Cyril Godard' _publ_contact_author_email cyril.godard@urv.cat loop_ _publ_author_name C.Godard M.A.R.Manrique C.Claver C.Blanco E.Zangrando data_4a _database_code_depnum_ccdc_archive 'CCDC 866062' #TrackingRef '- 4a-7a-new.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H48 Cl2 Fe P2 Pd C4 H8 O' _chemical_formula_sum 'C32 H56 Cl2 Fe O P2 Pd' _chemical_formula_weight 751.86 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' 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' Fe Fe 0.3463 0.8444 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.558(3) _cell_length_b 14.646(3) _cell_length_c 20.721(4) _cell_angle_alpha 90.00 _cell_angle_beta 94.29(3) _cell_angle_gamma 90.00 _cell_volume 3497.8(13) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 394 _cell_measurement_theta_min 6.78 _cell_measurement_theta_max 21.55 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.428 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1568 _exptl_absorpt_coefficient_mu 1.196 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.4219 _exptl_absorpt_correction_T_max 1.0385 _exptl_absorpt_process_details ; Parkin S,Moezzi B & Hope H, (1995) J. Appl. Cryst. 28, 53-56 Cubic fit to sin(theta)/lambda - 24 parameters ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mok\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Enraf-Nonius dip1030 image plate diffractometer' _diffrn_measurement_method '\f-scans with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 42519 _diffrn_reflns_av_R_equivalents 0.1362 _diffrn_reflns_av_sigmaI/netI 0.1183 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.70 _diffrn_reflns_theta_max 25.02 _reflns_number_total 6015 _reflns_number_gt 3489 _reflns_threshold_expression >2\s(I) _computing_data_collection 'XPRESS (MacScience, 2002)' _computing_cell_refinement 'Denzo (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELX97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELX97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep3 for Windows (Farrugia,1997)' _computing_publication_material 'Wingx 1.80.05 (Farrugia, 1999)' _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^ > 2\s(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^)+(0.0561P)^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_extinction_coef ? _refine_ls_number_reflns 6015 _refine_ls_number_parameters 352 _refine_ls_number_restraints 24 _refine_ls_R_factor_all 0.1008 _refine_ls_R_factor_gt 0.0510 _refine_ls_wR_factor_ref 0.1354 _refine_ls_wR_factor_gt 0.1159 _refine_ls_goodness_of_fit_ref 0.894 _refine_ls_restrained_S_all 0.903 _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 0.79494(4) 0.96662(3) 0.23381(2) 0.04961(17) Uani 1 1 d . . . Fe Fe 0.77381(8) 0.70281(7) 0.01894(4) 0.0585(3) Uani 1 1 d . . . Cl1 Cl 0.93254(14) 1.03430(14) 0.30808(8) 0.0716(5) Uani 1 1 d . . . Cl2 Cl 0.67248(14) 1.08363(13) 0.26629(8) 0.0688(5) Uani 1 1 d . . . P1 P 0.63062(12) 0.89222(12) 0.18747(7) 0.0485(4) Uani 1 1 d . . . P2 P 0.94833(12) 0.88923(12) 0.19255(7) 0.0491(4) Uani 1 1 d . . . C1 C 0.6498(5) 0.7908(4) 0.1354(3) 0.0523(15) Uani 1 1 d . . . H1A H 0.6906 0.7442 0.1615 0.063 Uiso 1 1 calc R . . H1B H 0.5736 0.7667 0.1219 0.063 Uiso 1 1 calc R . . C2 C 0.5224(5) 0.9657(5) 0.1365(3) 0.0617(17) Uani 1 1 d . . . C3 C 0.5587(5) 0.8360(4) 0.2568(3) 0.0537(15) Uani 1 1 d . . . C4 C 0.9167(5) 0.7926(4) 0.1369(3) 0.0523(15) Uani 1 1 d . . . H4A H 0.9901 0.7702 0.1234 0.063 Uiso 1 1 calc R . . H4B H 0.8835 0.7440 0.1615 0.063 Uiso 1 1 calc R . . C5 C 1.0224(5) 0.9752(5) 0.1418(3) 0.0586(16) Uani 1 1 d . . . C6 C 1.0531(5) 0.8290(5) 0.2553(3) 0.0585(16) Uani 1 1 d . . . C7 C 0.5968(6) 1.0315(5) 0.0993(3) 0.080(2) Uani 1 1 d . . . H7A H 0.6489 0.9970 0.0747 0.120 Uiso 1 1 calc R . . H7B H 0.6408 1.0702 0.1293 0.120 Uiso 1 1 calc R . . H7C H 0.5474 1.0683 0.0705 0.120 Uiso 1 1 calc R . . C8 C 0.4458(6) 0.9105(6) 0.0879(3) 0.076(2) Uani 1 1 d . . . H8A H 0.4937 0.8740 0.0621 0.114 Uiso 1 1 calc R . . H8B H 0.3996 0.9512 0.0604 0.114 Uiso 1 1 calc R . . H8C H 0.3959 0.8714 0.1106 0.114 Uiso 1 1 calc R . . C9 C 0.4404(5) 1.0219(5) 0.1763(3) 0.0719(19) Uani 1 1 d . . . H9A H 0.4854 1.0582 0.2075 0.108 Uiso 1 1 calc R . . H9B H 0.3913 0.9813 0.1983 0.108 Uiso 1 1 calc R . . H9C H 0.3935 1.0611 0.1479 0.108 Uiso 1 1 calc R . . C10 C 0.4500(6) 0.7829(5) 0.2332(4) 0.075(2) Uani 1 1 d . . . H10A H 0.4687 0.7408 0.2000 0.113 Uiso 1 1 calc R . . H10B H 0.3916 0.8246 0.2160 0.113 Uiso 1 1 calc R . . H10C H 0.4215 0.7497 0.2687 0.113 Uiso 1 1 calc R . . C11 C 0.5269(6) 0.9035(5) 0.3091(3) 0.078(2) Uani 1 1 d . . . H11A H 0.5948 0.9371 0.3245 0.116 Uiso 1 1 calc R . . H11B H 0.4973 0.8706 0.3444 0.116 Uiso 1 1 calc R . . H11C H 0.4688 0.9450 0.2912 0.116 Uiso 1 1 calc R . . C12 C 0.6482(6) 0.7686(5) 0.2891(3) 0.0705(19) Uani 1 1 d . . . H12A H 0.7168 0.8013 0.3043 0.106 Uiso 1 1 calc R . . H12B H 0.6678 0.7234 0.2582 0.106 Uiso 1 1 calc R . . H12C H 0.6156 0.7391 0.3250 0.106 Uiso 1 1 calc R . . C13 C 0.9281(6) 1.0177(5) 0.0962(3) 0.076(2) Uani 1 1 d . . . H13A H 0.8878 0.9704 0.0715 0.114 Uiso 1 1 calc R . . H13B H 0.9626 1.0593 0.0674 0.114 Uiso 1 1 calc R . . H13C H 0.8743 1.0501 0.1209 0.114 Uiso 1 1 calc R . . C14 C 1.1137(5) 0.9290(5) 0.1030(3) 0.0682(18) Uani 1 1 d . . . H14A H 1.1735 0.9035 0.1322 0.102 Uiso 1 1 calc R . . H14B H 1.1471 0.9733 0.0757 0.102 Uiso 1 1 calc R . . H14C H 1.0779 0.8814 0.0767 0.102 Uiso 1 1 calc R . . C15 C 1.0826(6) 1.0550(5) 0.1802(4) 0.076(2) Uani 1 1 d . . . H15A H 1.1437 1.0314 0.2094 0.114 Uiso 1 1 calc R . . H15B H 1.0268 1.0863 0.2043 0.114 Uiso 1 1 calc R . . H15C H 1.1145 1.0969 0.1506 0.114 Uiso 1 1 calc R . . C16 C 1.1104(5) 0.7441(5) 0.2267(3) 0.071(2) Uani 1 1 d . . . H16A H 1.1569 0.7627 0.1925 0.107 Uiso 1 1 calc R . . H16B H 1.0513 0.7026 0.2098 0.107 Uiso 1 1 calc R . . H16C H 1.1587 0.7142 0.2600 0.107 Uiso 1 1 calc R . . C17 C 1.1519(5) 0.8907(6) 0.2836(3) 0.077(2) Uani 1 1 d . . . H17A H 1.1976 0.9108 0.2495 0.115 Uiso 1 1 calc R . . H17B H 1.2000 0.8570 0.3150 0.115 Uiso 1 1 calc R . . H17C H 1.1197 0.9427 0.3040 0.115 Uiso 1 1 calc R . . C18 C 0.9810(6) 0.7974(5) 0.3092(3) 0.0689(19) Uani 1 1 d . . . H18A H 0.9191 0.7590 0.2916 0.103 Uiso 1 1 calc R . . H18B H 0.9490 0.8495 0.3296 0.103 Uiso 1 1 calc R . . H18C H 1.0291 0.7637 0.3406 0.103 Uiso 1 1 calc R . . C19 C 0.8376(5) 0.8078(4) 0.0769(3) 0.0504(15) Uani 1 1 d . . . C20 C 0.7142(5) 0.8059(4) 0.0758(3) 0.0521(15) Uani 1 1 d . . . C21 C 0.6717(6) 0.8139(5) 0.0096(3) 0.0641(18) Uani 1 1 d . . . H21 H 0.5940 0.8128 -0.0058 0.077 Uiso 1 1 calc R . . C22 C 0.7667(6) 0.8238(5) -0.0286(3) 0.0686(19) Uani 1 1 d . . . H22 H 0.7626 0.8327 -0.0732 0.082 Uiso 1 1 calc R . . C23 C 0.8687(6) 0.8180(5) 0.0124(3) 0.0644(18) Uani 1 1 d . . . H23 H 0.9440 0.8204 -0.0005 0.077 Uiso 1 1 calc R . . C24 C 0.8233(14) 0.5838(7) 0.0588(5) 0.123(4) Uani 1 1 d U . . H24 H 0.8601 0.5786 0.1001 0.148 Uiso 1 1 calc R . . C25 C 0.7079(12) 0.5818(7) 0.0453(6) 0.122(4) Uani 1 1 d U . . H25 H 0.6516 0.5738 0.0746 0.146 Uiso 1 1 calc R . . C26 C 0.6891(7) 0.5942(6) -0.0218(5) 0.100(3) Uani 1 1 d . . . H26 H 0.6177 0.5966 -0.0456 0.120 Uiso 1 1 calc R . . C27 C 0.7954(8) 0.6019(6) -0.0453(3) 0.085(2) Uani 1 1 d . . . H27 H 0.8088 0.6110 -0.0886 0.102 Uiso 1 1 calc R . . C28 C 0.8789(8) 0.5943(7) 0.0041(6) 0.110(3) Uani 1 1 d . . . H28 H 0.9587 0.5960 0.0009 0.132 Uiso 1 1 calc R . . O1 O 0.1835(10) 0.7106(12) 0.0453(9) 0.240(6) Uani 1 1 d . . . C31 C 0.2118(16) 0.7284(16) -0.0164(8) 0.238(11) Uani 1 1 d . . . H31A H 0.1556 0.6991 -0.0467 0.286 Uiso 1 1 calc R . . H31B H 0.2070 0.7937 -0.0239 0.286 Uiso 1 1 calc R . . C30 C 0.3630(11) 0.6544(12) 0.0333(10) 0.185(7) Uani 1 1 d . . . H30A H 0.3862 0.5919 0.0257 0.223 Uiso 1 1 calc R . . H30B H 0.4285 0.6875 0.0539 0.223 Uiso 1 1 calc R . . C32 C 0.3187(17) 0.6995(13) -0.0279(8) 0.189(6) Uani 1 1 d U . . H32A H 0.3678 0.7505 -0.0380 0.227 Uiso 1 1 calc R . . H32B H 0.3154 0.6566 -0.0637 0.227 Uiso 1 1 calc R . . C29 C 0.267(2) 0.6575(13) 0.0711(8) 0.199(7) Uani 1 1 d U . . H29A H 0.2369 0.5962 0.0758 0.239 Uiso 1 1 calc R . . H29B H 0.2918 0.6800 0.1140 0.239 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 0.0533(3) 0.0457(3) 0.0508(3) -0.0048(2) 0.00995(19) -0.0023(2) Fe 0.0749(6) 0.0565(7) 0.0444(5) -0.0043(4) 0.0059(4) 0.0020(5) Cl1 0.0645(9) 0.0777(13) 0.0728(10) -0.0258(10) 0.0047(8) -0.0083(9) Cl2 0.0711(10) 0.0527(11) 0.0836(11) -0.0160(9) 0.0136(9) 0.0056(8) P1 0.0511(8) 0.0447(10) 0.0501(8) -0.0017(8) 0.0073(7) -0.0001(7) P2 0.0505(8) 0.0473(10) 0.0504(8) -0.0013(8) 0.0093(7) -0.0003(7) C1 0.054(3) 0.052(4) 0.052(3) -0.005(3) 0.005(3) 0.001(3) C2 0.060(4) 0.063(5) 0.061(4) 0.003(4) 0.000(3) 0.013(3) C3 0.050(3) 0.047(4) 0.063(4) 0.005(3) 0.005(3) -0.007(3) C4 0.053(3) 0.052(4) 0.052(3) -0.001(3) 0.010(3) 0.005(3) C5 0.058(3) 0.056(5) 0.064(4) 0.001(4) 0.020(3) -0.004(3) C6 0.054(3) 0.063(5) 0.058(4) 0.001(3) -0.001(3) 0.004(3) C7 0.086(5) 0.072(6) 0.082(5) 0.027(5) 0.007(4) 0.014(4) C8 0.073(4) 0.076(6) 0.077(4) -0.012(4) -0.008(3) 0.018(4) C9 0.060(4) 0.062(5) 0.093(5) -0.002(4) 0.000(3) 0.014(4) C10 0.067(4) 0.069(5) 0.092(5) 0.005(4) 0.017(4) -0.006(4) C11 0.096(5) 0.066(5) 0.074(4) -0.002(4) 0.034(4) 0.000(4) C12 0.076(4) 0.073(5) 0.065(4) 0.017(4) 0.019(3) 0.009(4) C13 0.085(5) 0.064(6) 0.080(4) 0.011(4) 0.019(4) -0.003(4) C14 0.065(4) 0.066(5) 0.076(4) -0.001(4) 0.022(3) -0.012(4) C15 0.084(5) 0.056(5) 0.091(5) -0.003(4) 0.026(4) -0.013(4) C16 0.058(4) 0.076(6) 0.079(4) -0.001(4) -0.004(3) 0.016(4) C17 0.057(4) 0.094(6) 0.077(4) -0.007(4) -0.011(3) 0.000(4) C18 0.080(4) 0.069(5) 0.057(4) 0.014(4) 0.000(3) 0.008(4) C19 0.061(3) 0.043(4) 0.048(3) -0.003(3) 0.011(3) -0.002(3) C20 0.062(4) 0.047(4) 0.047(3) 0.000(3) 0.004(3) 0.003(3) C21 0.069(4) 0.061(5) 0.061(4) -0.004(4) -0.003(3) 0.011(4) C22 0.088(5) 0.069(5) 0.049(4) 0.002(3) 0.005(4) 0.000(4) C23 0.078(4) 0.062(5) 0.055(4) 0.003(3) 0.018(3) -0.008(4) C24 0.249(12) 0.051(6) 0.063(5) -0.006(4) -0.025(7) 0.022(8) C25 0.201(10) 0.054(6) 0.124(8) -0.016(6) 0.096(8) -0.024(7) C26 0.086(6) 0.079(7) 0.135(8) -0.024(6) 0.001(6) -0.018(5) C27 0.121(7) 0.076(6) 0.058(4) -0.013(4) 0.013(5) 0.013(5) C28 0.101(6) 0.082(7) 0.142(9) -0.027(7) -0.019(7) 0.038(5) O1 0.173(9) 0.280(18) 0.272(16) -0.033(14) 0.050(10) 0.052(10) C31 0.177(15) 0.42(4) 0.113(10) 0.045(14) 0.004(10) 0.101(17) C30 0.126(10) 0.166(15) 0.258(18) -0.068(15) -0.026(12) 0.041(10) C32 0.187(12) 0.224(15) 0.164(11) -0.005(11) 0.068(11) 0.009(11) C29 0.255(15) 0.167(13) 0.181(12) 0.007(11) 0.058(13) 0.031(12) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 P2 2.3206(16) . ? Pd P1 2.3331(17) . ? Pd Cl1 2.3481(17) . ? Pd Cl2 2.3529(17) . ? Fe C24 1.995(9) . ? Fe C21 2.011(7) . ? Fe C27 2.017(7) . ? Fe C26 2.020(8) . ? Fe C25 2.021(10) . ? Fe C23 2.022(7) . ? Fe C22 2.026(7) . ? Fe C28 2.037(9) . ? Fe C19 2.053(6) . ? Fe C20 2.064(6) . ? P1 C1 1.860(6) . ? P1 C3 1.901(6) . ? P1 C2 1.908(6) . ? P2 C4 1.845(6) . ? P2 C5 1.887(6) . ? P2 C6 1.923(6) . ? C1 C20 1.506(8) . ? C2 C8 1.522(9) . ? C2 C7 1.538(9) . ? C2 C9 1.540(8) . ? C3 C10 1.526(9) . ? C3 C11 1.532(9) . ? C3 C12 1.546(9) . ? C4 C19 1.504(8) . ? C5 C13 1.521(9) . ? C5 C14 1.531(8) . ? C5 C15 1.550(9) . ? C6 C18 1.515(9) . ? C6 C17 1.538(9) . ? C6 C16 1.548(9) . ? C19 C23 1.417(8) . ? C19 C20 1.425(8) . ? C20 C21 1.426(8) . ? C21 C22 1.409(9) . ? C22 C23 1.403(9) . ? C24 C25 1.343(14) . ? C24 C28 1.353(14) . ? C25 C26 1.402(13) . ? C26 C27 1.360(11) . ? C27 C28 1.358(11) . ? O1 C29 1.321(18) . ? O1 C31 1.368(16) . ? C31 C32 1.344(18) . ? C30 C29 1.407(19) . ? C30 C32 1.487(18) . ? 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 P2 Pd P1 103.95(6) . . ? P2 Pd Cl1 87.08(6) . . ? P1 Pd Cl1 163.23(6) . . ? P2 Pd Cl2 162.48(6) . . ? P1 Pd Cl2 88.24(6) . . ? Cl1 Pd Cl2 84.12(6) . . ? C24 Fe C21 153.5(5) . . ? C24 Fe C27 65.6(4) . . ? C21 Fe C27 129.0(3) . . ? C24 Fe C26 66.4(4) . . ? C21 Fe C26 109.5(3) . . ? C27 Fe C26 39.4(3) . . ? C24 Fe C25 39.1(4) . . ? C21 Fe C25 120.3(4) . . ? C27 Fe C25 66.6(4) . . ? C26 Fe C25 40.6(4) . . ? C24 Fe C23 128.1(5) . . ? C21 Fe C23 68.7(3) . . ? C27 Fe C23 118.2(3) . . ? C26 Fe C23 151.4(4) . . ? C25 Fe C23 165.3(5) . . ? C24 Fe C22 164.9(5) . . ? C21 Fe C22 40.8(3) . . ? C27 Fe C22 108.8(3) . . ? C26 Fe C22 119.0(4) . . ? C25 Fe C22 153.7(5) . . ? C23 Fe C22 40.6(2) . . ? C24 Fe C28 39.2(4) . . ? C21 Fe C28 165.7(4) . . ? C27 Fe C28 39.1(3) . . ? C26 Fe C28 66.3(4) . . ? C25 Fe C28 66.3(4) . . ? C23 Fe C28 107.9(4) . . ? C22 Fe C28 127.7(4) . . ? C24 Fe C19 109.4(3) . . ? C21 Fe C19 68.5(2) . . ? C27 Fe C19 151.4(3) . . ? C26 Fe C19 167.4(3) . . ? C25 Fe C19 128.7(4) . . ? C23 Fe C19 40.7(2) . . ? C22 Fe C19 68.2(2) . . ? C28 Fe C19 118.7(3) . . ? C24 Fe C20 120.1(4) . . ? C21 Fe C20 40.9(2) . . ? C27 Fe C20 167.2(3) . . ? C26 Fe C20 130.0(3) . . ? C25 Fe C20 109.8(3) . . ? C23 Fe C20 68.5(3) . . ? C22 Fe C20 68.6(3) . . ? C28 Fe C20 152.2(3) . . ? C19 Fe C20 40.5(2) . . ? C1 P1 C3 99.8(3) . . ? C1 P1 C2 103.4(3) . . ? C3 P1 C2 110.9(3) . . ? C1 P1 Pd 118.89(19) . . ? C3 P1 Pd 106.27(18) . . ? C2 P1 Pd 116.4(2) . . ? C4 P2 C5 103.9(3) . . ? C4 P2 C6 98.9(3) . . ? C5 P2 C6 113.2(3) . . ? C4 P2 Pd 118.94(18) . . ? C5 P2 Pd 105.7(2) . . ? C6 P2 Pd 115.76(19) . . ? C20 C1 P1 116.5(5) . . ? C8 C2 C7 108.7(5) . . ? C8 C2 C9 106.7(5) . . ? C7 C2 C9 108.9(6) . . ? C8 C2 P1 113.0(5) . . ? C7 C2 P1 105.2(4) . . ? C9 C2 P1 114.1(4) . . ? C10 C3 C11 108.7(5) . . ? C10 C3 C12 108.8(6) . . ? C11 C3 C12 107.1(5) . . ? C10 C3 P1 112.0(4) . . ? C11 C3 P1 113.4(5) . . ? C12 C3 P1 106.7(4) . . ? C19 C4 P2 118.9(4) . . ? C13 C5 C14 110.2(5) . . ? C13 C5 C15 106.5(6) . . ? C14 C5 C15 107.6(5) . . ? C13 C5 P2 106.6(4) . . ? C14 C5 P2 110.9(5) . . ? C15 C5 P2 115.0(4) . . ? C18 C6 C17 109.4(5) . . ? C18 C6 C16 108.2(6) . . ? C17 C6 C16 106.9(5) . . ? C18 C6 P2 106.6(4) . . ? C17 C6 P2 113.6(5) . . ? C16 C6 P2 112.1(4) . . ? C23 C19 C20 108.1(5) . . ? C23 C19 C4 127.9(5) . . ? C20 C19 C4 123.8(5) . . ? C23 C19 Fe 68.5(4) . . ? C20 C19 Fe 70.2(3) . . ? C4 C19 Fe 122.9(4) . . ? C19 C20 C21 106.7(5) . . ? C19 C20 C1 123.0(5) . . ? C21 C20 C1 130.1(5) . . ? C19 C20 Fe 69.3(3) . . ? C21 C20 Fe 67.5(4) . . ? C1 C20 Fe 124.5(4) . . ? C22 C21 C20 108.7(6) . . ? C22 C21 Fe 70.2(4) . . ? C20 C21 Fe 71.5(4) . . ? C23 C22 C21 108.0(5) . . ? C23 C22 Fe 69.5(4) . . ? C21 C22 Fe 69.0(4) . . ? C22 C23 C19 108.5(5) . . ? C22 C23 Fe 69.9(4) . . ? C19 C23 Fe 70.9(4) . . ? C25 C24 C28 110.7(9) . . ? C25 C24 Fe 71.5(6) . . ? C28 C24 Fe 72.1(6) . . ? C24 C25 C26 106.4(9) . . ? C24 C25 Fe 69.4(6) . . ? C26 C25 Fe 69.7(5) . . ? C27 C26 C25 106.8(8) . . ? C27 C26 Fe 70.2(5) . . ? C25 C26 Fe 69.7(6) . . ? C28 C27 C26 109.4(8) . . ? C28 C27 Fe 71.2(5) . . ? C26 C27 Fe 70.4(5) . . ? C24 C28 C27 106.6(9) . . ? C24 C28 Fe 68.7(6) . . ? C27 C28 Fe 69.6(5) . . ? C29 O1 C31 105.8(13) . . ? C32 C31 O1 113.2(14) . . ? C29 C30 C32 103.0(12) . . ? C31 C32 C30 104.5(13) . . ? O1 C29 C30 112.1(15) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag P2 Pd P1 C1 3.3(2) . . . . ? Cl1 Pd P1 C1 -126.6(3) . . . . ? Cl2 Pd P1 C1 170.6(2) . . . . ? P2 Pd P1 C3 114.7(2) . . . . ? Cl1 Pd P1 C3 -15.3(3) . . . . ? Cl2 Pd P1 C3 -78.1(2) . . . . ? P2 Pd P1 C2 -121.3(2) . . . . ? Cl1 Pd P1 C2 108.8(3) . . . . ? Cl2 Pd P1 C2 46.0(2) . . . . ? P1 Pd P2 C4 -0.4(2) . . . . ? Cl1 Pd P2 C4 166.8(2) . . . . ? Cl2 Pd P2 C4 -133.4(3) . . . . ? P1 Pd P2 C5 115.8(2) . . . . ? Cl1 Pd P2 C5 -77.0(2) . . . . ? Cl2 Pd P2 C5 -17.2(3) . . . . ? P1 Pd P2 C6 -118.0(2) . . . . ? Cl1 Pd P2 C6 49.2(2) . . . . ? Cl2 Pd P2 C6 109.0(3) . . . . ? C3 P1 C1 C20 -175.5(4) . . . . ? C2 P1 C1 C20 70.1(5) . . . . ? Pd P1 C1 C20 -60.7(5) . . . . ? C1 P1 C2 C8 25.2(5) . . . . ? C3 P1 C2 C8 -80.9(5) . . . . ? Pd P1 C2 C8 157.4(4) . . . . ? C1 P1 C2 C7 -93.2(5) . . . . ? C3 P1 C2 C7 160.6(4) . . . . ? Pd P1 C2 C7 39.0(5) . . . . ? C1 P1 C2 C9 147.4(5) . . . . ? C3 P1 C2 C9 41.3(6) . . . . ? Pd P1 C2 C9 -80.3(5) . . . . ? C1 P1 C3 C10 -54.9(5) . . . . ? C2 P1 C3 C10 53.6(5) . . . . ? Pd P1 C3 C10 -179.0(4) . . . . ? C1 P1 C3 C11 -178.3(5) . . . . ? C2 P1 C3 C11 -69.8(5) . . . . ? Pd P1 C3 C11 57.5(5) . . . . ? C1 P1 C3 C12 64.1(5) . . . . ? C2 P1 C3 C12 172.6(4) . . . . ? Pd P1 C3 C12 -60.1(5) . . . . ? C5 P2 C4 C19 -61.7(5) . . . . ? C6 P2 C4 C19 -178.5(4) . . . . ? Pd P2 C4 C19 55.4(5) . . . . ? C4 P2 C5 C13 74.9(5) . . . . ? C6 P2 C5 C13 -178.8(4) . . . . ? Pd P2 C5 C13 -51.1(5) . . . . ? C4 P2 C5 C14 -45.0(5) . . . . ? C6 P2 C5 C14 61.3(5) . . . . ? Pd P2 C5 C14 -171.0(4) . . . . ? C4 P2 C5 C15 -167.4(5) . . . . ? C6 P2 C5 C15 -61.1(5) . . . . ? Pd P2 C5 C15 66.7(5) . . . . ? C4 P2 C6 C18 -95.3(5) . . . . ? C5 P2 C6 C18 155.3(5) . . . . ? Pd P2 C6 C18 33.0(5) . . . . ? C4 P2 C6 C17 144.2(5) . . . . ? C5 P2 C6 C17 34.7(5) . . . . ? Pd P2 C6 C17 -87.5(4) . . . . ? C4 P2 C6 C16 22.9(5) . . . . ? C5 P2 C6 C16 -86.6(5) . . . . ? Pd P2 C6 C16 151.2(4) . . . . ? P2 C4 C19 C23 103.3(7) . . . . ? P2 C4 C19 C20 -82.7(7) . . . . ? P2 C4 C19 Fe -169.6(3) . . . . ? C24 Fe C19 C23 126.3(6) . . . . ? C21 Fe C19 C23 -81.9(4) . . . . ? C27 Fe C19 C23 51.8(7) . . . . ? C26 Fe C19 C23 -165.2(14) . . . . ? C25 Fe C19 C23 165.8(6) . . . . ? C22 Fe C19 C23 -37.8(4) . . . . ? C28 Fe C19 C23 84.4(6) . . . . ? C20 Fe C19 C23 -119.8(5) . . . . ? C24 Fe C19 C20 -113.9(6) . . . . ? C21 Fe C19 C20 37.9(4) . . . . ? C27 Fe C19 C20 171.6(6) . . . . ? C26 Fe C19 C20 -45.4(16) . . . . ? C25 Fe C19 C20 -74.4(6) . . . . ? C23 Fe C19 C20 119.8(5) . . . . ? C22 Fe C19 C20 82.0(4) . . . . ? C28 Fe C19 C20 -155.8(5) . . . . ? C24 Fe C19 C4 4.3(7) . . . . ? C21 Fe C19 C4 156.1(5) . . . . ? C27 Fe C19 C4 -70.2(7) . . . . ? C26 Fe C19 C4 72.7(16) . . . . ? C25 Fe C19 C4 43.7(7) . . . . ? C23 Fe C19 C4 -122.1(6) . . . . ? C22 Fe C19 C4 -159.8(5) . . . . ? C28 Fe C19 C4 -37.7(6) . . . . ? C20 Fe C19 C4 118.1(6) . . . . ? C23 C19 C20 C21 0.8(7) . . . . ? C4 C19 C20 C21 -174.3(6) . . . . ? Fe C19 C20 C21 -57.3(5) . . . . ? C23 C19 C20 C1 176.6(6) . . . . ? C4 C19 C20 C1 1.6(10) . . . . ? Fe C19 C20 C1 118.5(6) . . . . ? C23 C19 C20 Fe 58.1(5) . . . . ? C4 C19 C20 Fe -116.9(6) . . . . ? P1 C1 C20 C19 82.0(7) . . . . ? P1 C1 C20 C21 -103.3(7) . . . . ? P1 C1 C20 Fe 168.3(3) . . . . ? C24 Fe C20 C19 85.1(6) . . . . ? C21 Fe C20 C19 -119.2(5) . . . . ? C27 Fe C20 C19 -161.5(13) . . . . ? C26 Fe C20 C19 168.3(5) . . . . ? C25 Fe C20 C19 126.9(6) . . . . ? C23 Fe C20 C19 -37.5(4) . . . . ? C22 Fe C20 C19 -81.2(4) . . . . ? C28 Fe C20 C19 50.4(9) . . . . ? C24 Fe C20 C21 -155.7(6) . . . . ? C27 Fe C20 C21 -42.3(15) . . . . ? C26 Fe C20 C21 -72.5(6) . . . . ? C25 Fe C20 C21 -113.8(6) . . . . ? C23 Fe C20 C21 81.8(4) . . . . ? C22 Fe C20 C21 38.0(4) . . . . ? C28 Fe C20 C21 169.6(8) . . . . ? C19 Fe C20 C21 119.2(5) . . . . ? C24 Fe C20 C1 -31.5(7) . . . . ? C21 Fe C20 C1 124.2(6) . . . . ? C27 Fe C20 C1 81.9(14) . . . . ? C26 Fe C20 C1 51.7(6) . . . . ? C25 Fe C20 C1 10.4(7) . . . . ? C23 Fe C20 C1 -154.0(5) . . . . ? C22 Fe C20 C1 162.2(5) . . . . ? C28 Fe C20 C1 -66.2(9) . . . . ? C19 Fe C20 C1 -116.6(6) . . . . ? C19 C20 C21 C22 -2.1(8) . . . . ? C1 C20 C21 C22 -177.5(7) . . . . ? Fe C20 C21 C22 -60.6(5) . . . . ? C19 C20 C21 Fe 58.5(4) . . . . ? C1 C20 C21 Fe -116.9(7) . . . . ? C24 Fe C21 C22 171.8(8) . . . . ? C27 Fe C21 C22 -72.3(5) . . . . ? C26 Fe C21 C22 -112.1(5) . . . . ? C25 Fe C21 C22 -155.6(5) . . . . ? C23 Fe C21 C22 37.3(4) . . . . ? C28 Fe C21 C22 -41.5(16) . . . . ? C19 Fe C21 C22 81.2(4) . . . . ? C20 Fe C21 C22 118.7(6) . . . . ? C24 Fe C21 C20 53.1(9) . . . . ? C27 Fe C21 C20 169.0(4) . . . . ? C26 Fe C21 C20 129.1(5) . . . . ? C25 Fe C21 C20 85.7(6) . . . . ? C23 Fe C21 C20 -81.4(4) . . . . ? C22 Fe C21 C20 -118.7(6) . . . . ? C28 Fe C21 C20 -160.2(13) . . . . ? C19 Fe C21 C20 -37.5(4) . . . . ? C20 C21 C22 C23 2.6(9) . . . . ? Fe C21 C22 C23 -58.8(5) . . . . ? C20 C21 C22 Fe 61.5(5) . . . . ? C24 Fe C22 C23 -46.1(14) . . . . ? C21 Fe C22 C23 119.7(5) . . . . ? C27 Fe C22 C23 -111.7(4) . . . . ? C26 Fe C22 C23 -153.6(4) . . . . ? C25 Fe C22 C23 173.2(7) . . . . ? C28 Fe C22 C23 -72.3(5) . . . . ? C19 Fe C22 C23 37.9(3) . . . . ? C20 Fe C22 C23 81.6(4) . . . . ? C24 Fe C22 C21 -165.8(12) . . . . ? C27 Fe C22 C21 128.6(4) . . . . ? C26 Fe C22 C21 86.7(5) . . . . ? C25 Fe C22 C21 53.5(9) . . . . ? C23 Fe C22 C21 -119.7(5) . . . . ? C28 Fe C22 C21 168.0(5) . . . . ? C19 Fe C22 C21 -81.8(4) . . . . ? C20 Fe C22 C21 -38.1(4) . . . . ? C21 C22 C23 C19 -2.1(9) . . . . ? Fe C22 C23 C19 -60.6(5) . . . . ? C21 C22 C23 Fe 58.5(5) . . . . ? C20 C19 C23 C22 0.8(8) . . . . ? C4 C19 C23 C22 175.6(6) . . . . ? Fe C19 C23 C22 60.0(5) . . . . ? C20 C19 C23 Fe -59.2(4) . . . . ? C4 C19 C23 Fe 115.6(7) . . . . ? C24 Fe C23 C22 166.2(5) . . . . ? C21 Fe C23 C22 -37.6(4) . . . . ? C27 Fe C23 C22 86.3(5) . . . . ? C26 Fe C23 C22 54.3(8) . . . . ? C25 Fe C23 C22 -168.0(12) . . . . ? C28 Fe C23 C22 127.6(5) . . . . ? C19 Fe C23 C22 -119.0(5) . . . . ? C20 Fe C23 C22 -81.7(4) . . . . ? C24 Fe C23 C19 -74.8(6) . . . . ? C21 Fe C23 C19 81.4(4) . . . . ? C27 Fe C23 C19 -154.7(4) . . . . ? C26 Fe C23 C19 173.3(6) . . . . ? C25 Fe C23 C19 -49.0(14) . . . . ? C22 Fe C23 C19 119.0(5) . . . . ? C28 Fe C23 C19 -113.4(5) . . . . ? C20 Fe C23 C19 37.3(3) . . . . ? C21 Fe C24 C25 47.5(10) . . . . ? C27 Fe C24 C25 -82.4(7) . . . . ? C26 Fe C24 C25 -39.1(6) . . . . ? C23 Fe C24 C25 169.9(6) . . . . ? C22 Fe C24 C25 -153.5(12) . . . . ? C28 Fe C24 C25 -120.0(9) . . . . ? C19 Fe C24 C25 128.1(6) . . . . ? C20 Fe C24 C25 84.8(7) . . . . ? C21 Fe C24 C28 167.6(6) . . . . ? C27 Fe C24 C28 37.7(6) . . . . ? C26 Fe C24 C28 80.9(6) . . . . ? C25 Fe C24 C28 120.0(9) . . . . ? C23 Fe C24 C28 -70.0(7) . . . . ? C22 Fe C24 C28 -33.5(16) . . . . ? C19 Fe C24 C28 -111.9(6) . . . . ? C20 Fe C24 C28 -155.2(5) . . . . ? C28 C24 C25 C26 -1.6(13) . . . . ? Fe C24 C25 C26 60.2(7) . . . . ? C28 C24 C25 Fe -61.8(8) . . . . ? C21 Fe C25 C24 -157.6(6) . . . . ? C27 Fe C25 C24 79.6(7) . . . . ? C26 Fe C25 C24 117.4(9) . . . . ? C23 Fe C25 C24 -32.9(16) . . . . ? C22 Fe C25 C24 164.9(7) . . . . ? C28 Fe C25 C24 36.7(6) . . . . ? C19 Fe C25 C24 -72.0(7) . . . . ? C20 Fe C25 C24 -113.6(6) . . . . ? C24 Fe C25 C26 -117.4(9) . . . . ? C21 Fe C25 C26 85.0(6) . . . . ? C27 Fe C25 C26 -37.8(5) . . . . ? C23 Fe C25 C26 -150.3(11) . . . . ? C22 Fe C25 C26 47.5(10) . . . . ? C28 Fe C25 C26 -80.7(6) . . . . ? C19 Fe C25 C26 170.6(5) . . . . ? C20 Fe C25 C26 129.0(6) . . . . ? C24 C25 C26 C27 0.7(12) . . . . ? Fe C25 C26 C27 60.7(7) . . . . ? C24 C25 C26 Fe -60.0(8) . . . . ? C24 Fe C26 C27 -79.8(7) . . . . ? C21 Fe C26 C27 128.4(5) . . . . ? C25 Fe C26 C27 -117.4(9) . . . . ? C23 Fe C26 C27 47.3(10) . . . . ? C22 Fe C26 C27 84.5(6) . . . . ? C28 Fe C26 C27 -36.8(6) . . . . ? C19 Fe C26 C27 -152.9(12) . . . . ? C20 Fe C26 C27 169.9(4) . . . . ? C24 Fe C26 C25 37.7(6) . . . . ? C21 Fe C26 C25 -114.2(7) . . . . ? C27 Fe C26 C25 117.4(9) . . . . ? C23 Fe C26 C25 164.8(7) . . . . ? C22 Fe C26 C25 -158.0(6) . . . . ? C28 Fe C26 C25 80.6(7) . . . . ? C19 Fe C26 C25 -35.5(18) . . . . ? C20 Fe C26 C25 -72.6(8) . . . . ? C25 C26 C27 C28 0.4(11) . . . . ? Fe C26 C27 C28 60.8(7) . . . . ? C25 C26 C27 Fe -60.4(7) . . . . ? C24 Fe C27 C28 -37.7(7) . . . . ? C21 Fe C27 C28 168.4(6) . . . . ? C26 Fe C27 C28 -119.6(9) . . . . ? C25 Fe C27 C28 -80.6(7) . . . . ? C23 Fe C27 C28 84.0(7) . . . . ? C22 Fe C27 C28 127.2(6) . . . . ? C19 Fe C27 C28 48.4(9) . . . . ? C20 Fe C27 C28 -157.0(12) . . . . ? C24 Fe C27 C26 81.9(7) . . . . ? C21 Fe C27 C26 -72.0(7) . . . . ? C25 Fe C27 C26 39.0(6) . . . . ? C23 Fe C27 C26 -156.4(6) . . . . ? C22 Fe C27 C26 -113.2(6) . . . . ? C28 Fe C27 C26 119.6(9) . . . . ? C19 Fe C27 C26 168.0(6) . . . . ? C20 Fe C27 C26 -37.4(16) . . . . ? C25 C24 C28 C27 1.8(13) . . . . ? Fe C24 C28 C27 -59.6(7) . . . . ? C25 C24 C28 Fe 61.4(8) . . . . ? C26 C27 C28 C24 -1.3(11) . . . . ? Fe C27 C28 C24 59.0(7) . . . . ? C26 C27 C28 Fe -60.3(7) . . . . ? C21 Fe C28 C24 -157.2(13) . . . . ? C27 Fe C28 C24 -118.2(9) . . . . ? C26 Fe C28 C24 -81.1(7) . . . . ? C25 Fe C28 C24 -36.6(6) . . . . ? C23 Fe C28 C24 128.9(7) . . . . ? C22 Fe C28 C24 169.6(6) . . . . ? C19 Fe C28 C24 85.9(7) . . . . ? C20 Fe C28 C24 51.2(11) . . . . ? C24 Fe C28 C27 118.2(9) . . . . ? C21 Fe C28 C27 -39.0(17) . . . . ? C26 Fe C28 C27 37.1(6) . . . . ? C25 Fe C28 C27 81.6(7) . . . . ? C23 Fe C28 C27 -112.9(6) . . . . ? C22 Fe C28 C27 -72.3(7) . . . . ? C19 Fe C28 C27 -155.9(5) . . . . ? C20 Fe C28 C27 169.3(6) . . . . ? C29 O1 C31 C32 -9(3) . . . . ? O1 C31 C32 C30 2(3) . . . . ? C29 C30 C32 C31 5(2) . . . . ? C31 O1 C29 C30 12(2) . . . . ? C32 C30 C29 O1 -11(2) . . . . ? _diffrn_measured_fraction_theta_max 0.972 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.972 _refine_diff_density_max 0.668 _refine_diff_density_min -0.406 _refine_diff_density_rms 0.093 #===END data_7a _database_code_depnum_ccdc_archive 'CCDC 866063' #TrackingRef '- 4a-7a-new.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H43 Br P2 Pd' _chemical_formula_sum 'C28 H43 Br P2 Pd' _chemical_formula_weight 627.87 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P bca' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 15.151(3) _cell_length_b 17.180(4) _cell_length_c 21.361(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5560(2) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 424 _cell_measurement_theta_min 4.42 _cell_measurement_theta_max 25.42 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.500 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2576 _exptl_absorpt_coefficient_mu 2.234 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.4271 _exptl_absorpt_correction_T_max 0.6400 _exptl_absorpt_process_details ; Parkin S,Moezzi B & Hope H, (1995) J. Appl. Cryst. 28, 53-56 Quadratic fit to sin(theta)/lambda - 18 parameters ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'image plate dip1030' _diffrn_measurement_method 'laser scanner' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 64489 _diffrn_reflns_av_R_equivalents 0.0630 _diffrn_reflns_av_sigmaI/netI 0.0675 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.62 _diffrn_reflns_theta_max 27.10 _reflns_number_total 5864 _reflns_number_gt 3190 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Nonius Xpress' _computing_cell_refinement 'Denzo (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELX97 (Sheldrick, 1998)' _computing_structure_refinement 'SHELX97 (Sheldrick, 1998)' _computing_molecular_graphics 'Ortep3/windows (Farrugia,1997)' _computing_publication_material 'Wingx 1.80.05 (Farrugia, 1999)' _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^ > 2\s(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^)+(0.0564P)^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_extinction_coef ? _refine_ls_number_reflns 5864 _refine_ls_number_parameters 289 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0852 _refine_ls_R_factor_gt 0.0395 _refine_ls_wR_factor_ref 0.1079 _refine_ls_wR_factor_gt 0.0959 _refine_ls_goodness_of_fit_ref 0.860 _refine_ls_restrained_S_all 0.860 _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 0.66891(2) 0.05612(2) 0.662434(15) 0.05527(12) Uani 1 1 d . . . Br Br 0.54400(3) -0.03793(3) 0.64529(3) 0.0865(2) Uani 1 1 d . . . P1 P 0.65306(7) 0.11946(7) 0.56916(5) 0.0587(3) Uani 1 1 d . . . P2 P 0.71495(7) 0.00753(7) 0.75636(5) 0.0591(3) Uani 1 1 d . . . C1 C 0.5435(3) 0.1483(3) 0.5432(2) 0.0653(12) Uani 1 1 d . . . H1 H 0.5136 0.1014 0.5280 0.078 Uiso 1 1 calc R . . C2 C 0.4878(3) 0.1816(3) 0.5969(3) 0.0888(16) Uani 1 1 d . . . H2A H 0.4488 0.1421 0.6138 0.107 Uiso 1 1 calc R . . H2B H 0.5254 0.2010 0.6302 0.107 Uiso 1 1 calc R . . C3 C 0.4361(5) 0.2462(5) 0.5683(4) 0.154(3) Uani 1 1 d . . . H3A H 0.3760 0.2292 0.5605 0.184 Uiso 1 1 calc R . . H3B H 0.4340 0.2901 0.5968 0.184 Uiso 1 1 calc R . . C4 C 0.4751(6) 0.2683(5) 0.5131(4) 0.185(4) Uani 1 1 d . . . H4A H 0.5054 0.3174 0.5192 0.222 Uiso 1 1 calc R . . H4B H 0.4298 0.2762 0.4816 0.222 Uiso 1 1 calc R . . C5 C 0.5385(3) 0.2100(4) 0.4902(2) 0.0944(17) Uani 1 1 d . . . H5A H 0.5959 0.2334 0.4830 0.113 Uiso 1 1 calc R . . H5B H 0.5180 0.1866 0.4515 0.113 Uiso 1 1 calc R . . C6 C 0.7024(3) 0.0730(3) 0.5011(2) 0.0707(13) Uani 1 1 d . . . H6 H 0.6989 0.1085 0.4653 0.085 Uiso 1 1 calc R . . C7 C 0.6561(3) -0.0043(3) 0.4843(2) 0.0856(15) Uani 1 1 d . . . H7A H 0.6056 -0.0126 0.5113 0.103 Uiso 1 1 calc R . . H7B H 0.6358 -0.0031 0.4412 0.103 Uiso 1 1 calc R . . C8 C 0.7216(5) -0.0675(4) 0.4929(4) 0.120(2) Uani 1 1 d . . . H8A H 0.7424 -0.0858 0.4526 0.144 Uiso 1 1 calc R . . H8B H 0.6950 -0.1108 0.5150 0.144 Uiso 1 1 calc R . . C9 C 0.7964(4) -0.0347(5) 0.5299(3) 0.115(2) Uani 1 1 d . . . H9A H 0.8513 -0.0606 0.5194 0.137 Uiso 1 1 calc R . . H9B H 0.7858 -0.0405 0.5745 0.137 Uiso 1 1 calc R . . C10 C 0.7993(3) 0.0495(4) 0.5118(3) 0.0981(19) Uani 1 1 d . . . H10A H 0.8336 0.0567 0.4739 0.118 Uiso 1 1 calc R . . H10B H 0.8254 0.0805 0.5450 0.118 Uiso 1 1 calc R . . C11 C 0.7161(3) 0.2096(3) 0.5811(2) 0.0670(12) Uani 1 1 d . . . H11A H 0.7494 0.2219 0.5436 0.080 Uiso 1 1 calc R . . H11B H 0.6762 0.2524 0.5896 0.080 Uiso 1 1 calc R . . C12 C 0.7669(2) 0.1353(3) 0.67616(19) 0.0565(11) Uani 1 1 d . . . C13 C 0.7777(3) 0.1987(3) 0.6351(2) 0.0584(11) Uani 1 1 d . . . C14 C 0.8456(3) 0.2520(3) 0.6458(2) 0.0697(13) Uani 1 1 d . . . H14 H 0.8538 0.2930 0.6181 0.084 Uiso 1 1 calc R . . C15 C 0.8997(3) 0.2449(3) 0.6959(2) 0.0723(13) Uani 1 1 d . . . H15 H 0.9443 0.2812 0.7023 0.087 Uiso 1 1 calc R . . C16 C 0.8892(3) 0.1849(3) 0.7370(2) 0.0690(13) Uani 1 1 d . . . H16 H 0.9266 0.1810 0.7714 0.083 Uiso 1 1 calc R . . C17 C 0.8231(3) 0.1292(3) 0.72823(19) 0.0600(11) Uani 1 1 d . . . C18 C 0.8148(3) 0.0633(3) 0.7739(2) 0.0759(14) Uani 1 1 d . . . H18A H 0.8117 0.0836 0.8163 0.091 Uiso 1 1 calc R . . H18B H 0.8662 0.0298 0.7710 0.091 Uiso 1 1 calc R . . C19 C 0.7464(3) -0.0946(3) 0.7586(2) 0.0661(12) Uani 1 1 d . . . H19 H 0.6935 -0.1256 0.7500 0.079 Uiso 1 1 calc R . . C20 C 0.8165(3) -0.1165(3) 0.7096(3) 0.0866(15) Uani 1 1 d . . . H20A H 0.7886 -0.1355 0.6717 0.104 Uiso 1 1 calc R . . H20B H 0.8525 -0.0716 0.6992 0.104 Uiso 1 1 calc R . . C21 C 0.8718(4) -0.1789(4) 0.7388(3) 0.119(2) Uani 1 1 d . . . H21A H 0.8672 -0.2264 0.7145 0.143 Uiso 1 1 calc R . . H21B H 0.9332 -0.1629 0.7394 0.143 Uiso 1 1 calc R . . C22 C 0.8404(4) -0.1925(4) 0.8029(4) 0.124(2) Uani 1 1 d . . . H22A H 0.8901 -0.1983 0.8312 0.148 Uiso 1 1 calc R . . H22B H 0.8051 -0.2396 0.8047 0.148 Uiso 1 1 calc R . . C23 C 0.7862(3) -0.1236(3) 0.8211(2) 0.0841(15) Uani 1 1 d . . . H23A H 0.8226 -0.0837 0.8402 0.101 Uiso 1 1 calc R . . H23B H 0.7400 -0.1384 0.8502 0.101 Uiso 1 1 calc R . . C24 C 0.6450(3) 0.0190(3) 0.8250(2) 0.0705(13) Uani 1 1 d . . . H24 H 0.6801 0.0047 0.8618 0.085 Uiso 1 1 calc R . . C25 C 0.6109(5) 0.1020(3) 0.8353(3) 0.109(2) Uani 1 1 d . . . H25A H 0.6570 0.1355 0.8517 0.130 Uiso 1 1 calc R . . H25B H 0.5884 0.1241 0.7967 0.130 Uiso 1 1 calc R . . C26 C 0.5385(6) 0.0912(6) 0.8823(4) 0.155(4) Uani 1 1 d . . . H26A H 0.5610 0.0988 0.9244 0.187 Uiso 1 1 calc R . . H26B H 0.4915 0.1285 0.8750 0.187 Uiso 1 1 calc R . . C27 C 0.5048(4) 0.0109(6) 0.8750(4) 0.156(4) Uani 1 1 d . . . H27A H 0.4437 0.0118 0.8614 0.187 Uiso 1 1 calc R . . H27B H 0.5081 -0.0167 0.9145 0.187 Uiso 1 1 calc R . . C28 C 0.5618(4) -0.0291(4) 0.8263(3) 0.0988(19) Uani 1 1 d . . . H28A H 0.5744 -0.0824 0.8383 0.119 Uiso 1 1 calc R . . H28B H 0.5331 -0.0290 0.7857 0.119 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 0.05574(19) 0.0597(2) 0.0504(2) 0.00521(16) -0.00722(15) -0.00730(16) Br 0.0802(3) 0.0872(4) 0.0922(4) 0.0128(3) -0.0163(3) -0.0230(3) P1 0.0636(7) 0.0658(7) 0.0467(6) 0.0057(5) -0.0066(5) -0.0080(6) P2 0.0619(7) 0.0644(7) 0.0510(7) 0.0066(6) -0.0077(5) -0.0005(6) C1 0.064(3) 0.072(3) 0.060(3) 0.005(2) -0.010(2) -0.003(2) C2 0.079(3) 0.101(4) 0.087(4) 0.005(3) 0.005(3) 0.013(3) C3 0.165(7) 0.142(7) 0.154(8) 0.008(6) 0.012(6) 0.073(6) C4 0.184(8) 0.185(9) 0.184(9) 0.106(7) 0.062(7) 0.089(7) C5 0.084(3) 0.125(5) 0.074(4) 0.028(3) -0.012(3) -0.001(3) C6 0.065(3) 0.086(4) 0.062(3) -0.005(3) -0.002(2) -0.011(2) C7 0.095(4) 0.097(4) 0.065(3) -0.017(3) -0.008(3) -0.008(3) C8 0.133(5) 0.086(5) 0.141(6) 0.002(4) 0.020(5) -0.001(4) C9 0.106(5) 0.143(7) 0.095(5) -0.008(4) -0.008(4) 0.031(5) C10 0.074(3) 0.126(5) 0.094(4) -0.041(4) 0.008(3) -0.004(3) C11 0.070(3) 0.064(3) 0.067(3) 0.011(2) -0.004(2) -0.010(2) C12 0.052(2) 0.062(3) 0.055(3) -0.006(2) -0.0038(19) -0.003(2) C13 0.057(2) 0.064(3) 0.054(3) -0.001(2) 0.002(2) -0.006(2) C14 0.068(3) 0.065(3) 0.076(3) 0.002(2) 0.005(3) -0.011(2) C15 0.058(3) 0.076(3) 0.083(4) -0.007(3) -0.008(3) -0.018(2) C16 0.061(3) 0.079(3) 0.067(3) -0.001(3) -0.016(2) -0.009(2) C17 0.058(2) 0.068(3) 0.054(3) 0.000(2) -0.005(2) -0.002(2) C18 0.073(3) 0.087(4) 0.068(3) 0.002(3) -0.023(2) -0.006(3) C19 0.067(3) 0.073(3) 0.058(3) 0.008(2) -0.004(2) 0.005(2) C20 0.085(3) 0.096(4) 0.079(4) -0.007(3) 0.003(3) 0.018(3) C21 0.102(4) 0.145(6) 0.111(5) -0.021(5) -0.015(4) 0.056(4) C22 0.129(5) 0.107(5) 0.136(6) 0.012(5) -0.013(5) 0.052(4) C23 0.093(4) 0.080(4) 0.080(4) 0.018(3) -0.002(3) 0.013(3) C24 0.083(3) 0.074(3) 0.055(3) 0.002(2) -0.011(2) 0.014(3) C25 0.148(6) 0.093(5) 0.086(4) 0.000(3) -0.004(4) 0.043(4) C26 0.164(8) 0.214(10) 0.088(5) -0.005(6) 0.001(5) 0.107(7) C27 0.071(4) 0.281(12) 0.116(6) -0.027(8) 0.013(4) 0.016(6) C28 0.081(3) 0.140(5) 0.075(4) 0.001(3) 0.014(3) -0.012(4) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 C12 2.034(4) . ? Pd P2 2.2823(12) . ? Pd P1 2.2828(12) . ? Pd Br 2.5152(7) . ? P1 C1 1.819(4) . ? P1 C6 1.819(5) . ? P1 C11 1.837(4) . ? P2 C19 1.818(5) . ? P2 C24 1.821(5) . ? P2 C18 1.830(5) . ? C1 C2 1.535(6) . ? C1 C5 1.551(6) . ? C2 C3 1.490(8) . ? C3 C4 1.373(9) . ? C4 C5 1.471(9) . ? C6 C10 1.541(7) . ? C6 C7 1.544(6) . ? C7 C8 1.482(7) . ? C8 C9 1.492(9) . ? C9 C10 1.499(8) . ? C11 C13 1.494(6) . ? C12 C17 1.405(5) . ? C12 C13 1.408(6) . ? C13 C14 1.396(6) . ? C14 C15 1.353(6) . ? C15 C16 1.362(6) . ? C16 C17 1.398(6) . ? C17 C18 1.501(6) . ? C19 C20 1.537(6) . ? C19 C23 1.548(6) . ? C20 C21 1.497(7) . ? C21 C22 1.470(8) . ? C22 C23 1.493(7) . ? C24 C28 1.508(7) . ? C24 C25 1.532(7) . ? C25 C26 1.499(9) . ? C26 C27 1.479(11) . ? C27 C28 1.516(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 C12 Pd P2 83.97(13) . . ? C12 Pd P1 83.33(12) . . ? P2 Pd P1 166.84(4) . . ? C12 Pd Br 178.00(12) . . ? P2 Pd Br 97.06(3) . . ? P1 Pd Br 95.74(3) . . ? C1 P1 C6 104.5(2) . . ? C1 P1 C11 106.7(2) . . ? C6 P1 C11 105.5(2) . . ? C1 P1 Pd 119.50(15) . . ? C6 P1 Pd 116.45(17) . . ? C11 P1 Pd 103.05(15) . . ? C19 P2 C24 103.7(2) . . ? C19 P2 C18 106.4(2) . . ? C24 P2 C18 105.0(2) . . ? C19 P2 Pd 117.13(15) . . ? C24 P2 Pd 119.38(16) . . ? C18 P2 Pd 103.99(16) . . ? C2 C1 C5 105.3(4) . . ? C2 C1 P1 112.0(3) . . ? C5 C1 P1 117.0(3) . . ? C3 C2 C1 105.1(5) . . ? C4 C3 C2 109.3(6) . . ? C3 C4 C5 112.2(6) . . ? C4 C5 C1 104.8(5) . . ? C10 C6 C7 104.0(4) . . ? C10 C6 P1 112.8(3) . . ? C7 C6 P1 112.2(3) . . ? C8 C7 C6 107.3(5) . . ? C7 C8 C9 107.4(5) . . ? C8 C9 C10 104.5(5) . . ? C9 C10 C6 105.2(5) . . ? C13 C11 P1 109.1(3) . . ? C17 C12 C13 118.7(4) . . ? C17 C12 Pd 120.5(3) . . ? C13 C12 Pd 120.8(3) . . ? C14 C13 C12 119.3(4) . . ? C14 C13 C11 120.3(4) . . ? C12 C13 C11 120.3(4) . . ? C15 C14 C13 121.2(5) . . ? C14 C15 C16 120.5(4) . . ? C15 C16 C17 120.9(4) . . ? C16 C17 C12 119.3(4) . . ? C16 C17 C18 119.3(4) . . ? C12 C17 C18 121.4(4) . . ? C17 C18 P2 109.3(3) . . ? C20 C19 C23 103.9(4) . . ? C20 C19 P2 113.5(3) . . ? C23 C19 P2 115.8(3) . . ? C21 C20 C19 106.2(5) . . ? C22 C21 C20 108.8(5) . . ? C21 C22 C23 107.1(5) . . ? C22 C23 C19 104.3(5) . . ? C28 C24 C25 103.1(5) . . ? C28 C24 P2 116.2(3) . . ? C25 C24 P2 114.4(4) . . ? C26 C25 C24 103.1(5) . . ? C27 C26 C25 107.3(6) . . ? C26 C27 C28 107.4(7) . . ? C24 C28 C27 103.9(5) . . ? _diffrn_measured_fraction_theta_max 0.956 _diffrn_reflns_theta_full 27.10 _diffrn_measured_fraction_theta_full 0.956 _refine_diff_density_max 0.382 _refine_diff_density_min -0.697 _refine_diff_density_rms 0.072