data_3 #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C25 H37 Cl Ir O2 P3' _chemical_formula_sum 'C25 H37 Cl Ir O2 P3' _chemical_formula_weight 690.13 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 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 13.0118(8) _cell_length_b 13.8569(8) _cell_length_c 15.1758(10) _cell_angle_alpha 90 _cell_angle_beta 94.793(3) _cell_angle_gamma 90 _cell_volume 2726.7(3) _cell_formula_units_Z 4 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 9691 _cell_measurement_theta_min 2.61 _cell_measurement_theta_max 31.58 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _exptl_crystal_density_diffrn 1.681 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1368 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 5.191 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(SADABS; Bruker, 2008)' _exptl_absorpt_correction_T_min 0.542 _exptl_absorpt_correction_T_max 0.660 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 193(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'microfocus sealed tube' _diffrn_radiation_monochromator 'multilayer optics' _diffrn_measurement_device_type 'Bruker Kappa APEX II Quazar' _diffrn_measurement_method 'phi and omega scans' _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_radiation_probe x-ray _diffrn_reflns_av_R_equivalents 0.0474 _diffrn_reflns_av_unetI/netI 0.0537 _diffrn_reflns_number 40449 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.99 _diffrn_reflns_theta_max 32.82 _diffrn_reflns_theta_full 32.82 _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.996 _reflns_number_total 10068 _reflns_number_gt 7585 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'APEX2 (Bruker, 2008)' _computing_cell_refinement 'APEX2 and SAINT (Bruker, 2008)' _computing_data_reduction 'SAINT (Bruker, 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # 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^)+(0.0190P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 10068 _refine_ls_number_parameters 301 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0513 _refine_ls_R_factor_gt 0.0297 _refine_ls_wR_factor_ref 0.056 _refine_ls_wR_factor_gt 0.0505 _refine_ls_goodness_of_fit_ref 1.006 _refine_ls_restrained_S_all 1.006 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.336 _refine_diff_density_min -0.742 _refine_diff_density_rms 0.149 #----------------------------------------------------------------------------# # 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' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ir Ir -1.4442 7.9887 '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 H1 H 0.529(2) 0.5978(19) 0.1547(16) 0.025(7) Uiso 1 1 d . . . C1 C 0.28535(19) 0.63847(19) 0.13270(15) 0.0199(5) Uani 1 1 d . . . C2 C 0.1945(2) 0.6671(2) 0.08463(18) 0.0284(6) Uani 1 1 d . . . H2 H 0.1852 0.7328 0.0678 0.034 Uiso 1 1 calc R . . C3 C 0.1173(2) 0.6003(2) 0.06119(18) 0.0343(7) Uani 1 1 d . . . H3 H 0.0565 0.6201 0.027 0.041 Uiso 1 1 calc R . . C4 C 0.1287(2) 0.5056(2) 0.08739(18) 0.0335(7) Uani 1 1 d . . . H4 H 0.0762 0.4601 0.0702 0.04 Uiso 1 1 calc R . . C5 C 0.2161(2) 0.4761(2) 0.13853(17) 0.0275(6) Uani 1 1 d . . . H5 H 0.222 0.4113 0.1585 0.033 Uiso 1 1 calc R . . C6 C 0.29619(19) 0.54208(19) 0.16104(16) 0.0200(5) Uani 1 1 d . . . C7 C 0.4700(2) 0.40200(19) 0.19737(17) 0.0224(6) Uani 1 1 d . . . H7 H 0.5377 0.3964 0.2333 0.027 Uiso 1 1 calc R . . C8 C 0.4949(2) 0.4135(2) 0.10103(18) 0.0342(7) Uani 1 1 d . . . H8A H 0.5268 0.3541 0.0813 0.051 Uiso 1 1 calc R . . H8B H 0.5427 0.4676 0.0965 0.051 Uiso 1 1 calc R . . H8C H 0.4312 0.4262 0.0637 0.051 Uiso 1 1 calc R . . C9 C 0.4139(3) 0.3067(2) 0.2085(2) 0.0463(9) Uani 1 1 d . . . H9A H 0.3495 0.3062 0.1701 0.069 Uiso 1 1 calc R . . H9B H 0.3985 0.2993 0.2702 0.069 Uiso 1 1 calc R . . H9C H 0.4578 0.2532 0.1922 0.069 Uiso 1 1 calc R . . C10 C 0.3444(2) 0.47145(19) 0.33726(16) 0.0221(5) Uani 1 1 d . . . H10 H 0.3005 0.4139 0.3208 0.027 Uiso 1 1 calc R . . C11 C 0.2750(3) 0.5498(2) 0.3693(2) 0.0444(9) Uani 1 1 d . . . H11A H 0.2417 0.5264 0.4208 0.067 Uiso 1 1 calc R . . H11B H 0.2222 0.5666 0.3219 0.067 Uiso 1 1 calc R . . H11C H 0.3164 0.6071 0.3859 0.067 Uiso 1 1 calc R . . C12 C 0.4264(2) 0.4409(3) 0.40988(18) 0.0399(8) Uani 1 1 d . . . H12A H 0.4754 0.4939 0.4221 0.06 Uiso 1 1 calc R . . H12B H 0.4632 0.3841 0.3903 0.06 Uiso 1 1 calc R . . H12C H 0.3932 0.4252 0.4637 0.06 Uiso 1 1 calc R . . C13 C 0.4366(2) 0.78503(18) 0.07941(16) 0.0195(5) Uani 1 1 d . . . C14 C 0.3749(2) 0.8213(2) 0.00700(17) 0.0260(6) Uani 1 1 d . . . H14 H 0.3027 0.8095 0.0022 0.031 Uiso 1 1 calc R . . C15 C 0.4187(2) 0.8744(2) -0.05799(18) 0.0302(7) Uani 1 1 d . . . H15 H 0.3765 0.8977 -0.1075 0.036 Uiso 1 1 calc R . . C16 C 0.5228(2) 0.8932(2) -0.05090(19) 0.0324(7) Uani 1 1 d . . . H16 H 0.5522 0.9295 -0.0956 0.039 Uiso 1 1 calc R . . C17 C 0.5854(2) 0.8595(2) 0.02145(18) 0.0295(6) Uani 1 1 d . . . H17 H 0.657 0.8741 0.0267 0.035 Uiso 1 1 calc R . . C18 C 0.5427(2) 0.80405(18) 0.08655(16) 0.0209(5) Uani 1 1 d . . . C19 C 0.7431(2) 0.7087(2) 0.15331(17) 0.0259(6) Uani 1 1 d . . . H19 H 0.7755 0.6769 0.2079 0.031 Uiso 1 1 calc R . . C20 C 0.7273(3) 0.6286(2) 0.0847(2) 0.0437(9) Uani 1 1 d . . . H20A H 0.6962 0.6556 0.029 0.066 Uiso 1 1 calc R . . H20B H 0.6815 0.5792 0.1061 0.066 Uiso 1 1 calc R . . H20C H 0.794 0.5994 0.0749 0.066 Uiso 1 1 calc R . . C21 C 0.8238(2) 0.7795(2) 0.1245(2) 0.0440(8) Uani 1 1 d . . . H21A H 0.8906 0.7468 0.1244 0.066 Uiso 1 1 calc R . . H21B H 0.8299 0.834 0.1657 0.066 Uiso 1 1 calc R . . H21C H 0.8027 0.8032 0.0648 0.066 Uiso 1 1 calc R . . C22 C 0.6574(2) 0.86941(19) 0.24804(18) 0.0255(6) Uani 1 1 d . . . H22 H 0.7006 0.9097 0.2108 0.031 Uiso 1 1 calc R . . C23 C 0.7244(3) 0.8423(2) 0.3331(2) 0.0399(8) Uani 1 1 d . . . H23A H 0.7464 0.9011 0.3651 0.06 Uiso 1 1 calc R . . H23B H 0.7852 0.8064 0.3175 0.06 Uiso 1 1 calc R . . H23C H 0.6842 0.802 0.3707 0.06 Uiso 1 1 calc R . . C24 C 0.5640(3) 0.9287(2) 0.2672(2) 0.0381(7) Uani 1 1 d . . . H24A H 0.5196 0.8906 0.3031 0.057 Uiso 1 1 calc R . . H24B H 0.5254 0.9467 0.2114 0.057 Uiso 1 1 calc R . . H24C H 0.5866 0.9872 0.2996 0.057 Uiso 1 1 calc R . . C25 C 0.4915(2) 0.7008(2) 0.35898(17) 0.0265(6) Uani 1 1 d . . . O1 O 0.32742(14) 0.80329(13) 0.22309(12) 0.0261(4) Uani 1 1 d . . . O2 O 0.47725(19) 0.73440(17) 0.42450(13) 0.0469(6) Uani 1 1 d . . . P1 P 0.38196(5) 0.72742(5) 0.17424(4) 0.01729(13) Uani 1 1 d . . . P2 P 0.40591(5) 0.51077(5) 0.23815(4) 0.01664(13) Uani 1 1 d . . . P3 P 0.61965(5) 0.75962(5) 0.18466(4) 0.01881(14) Uani 1 1 d . . . Cl1 Cl 0.66353(5) 0.55262(5) 0.31568(5) 0.03318(16) Uani 1 1 d . . . Ir1 Ir 0.514260(7) 0.645070(7) 0.244718(6) 0.01617(3) 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 0.0154(12) 0.0235(14) 0.0208(11) 0.0001(10) 0.0007(9) -0.0014(11) C2 0.0189(14) 0.0292(16) 0.0359(15) 0.0104(12) -0.0039(11) -0.0020(12) C3 0.0198(15) 0.048(2) 0.0332(15) 0.0115(14) -0.0097(12) -0.0073(14) C4 0.0246(16) 0.0414(19) 0.0327(15) 0.0039(13) -0.0082(12) -0.0146(14) C5 0.0273(16) 0.0275(16) 0.0271(13) 0.0025(12) -0.0019(11) -0.0081(12) C6 0.0159(13) 0.0209(14) 0.0225(12) 0.0005(10) -0.0010(10) -0.0020(10) C7 0.0215(14) 0.0186(14) 0.0270(13) -0.0025(11) 0.0015(11) 0.0038(11) C8 0.0365(18) 0.0324(18) 0.0347(15) -0.0111(13) 0.0084(13) 0.0013(14) C9 0.056(2) 0.0223(17) 0.065(2) -0.0090(16) 0.0276(19) -0.0034(16) C10 0.0202(14) 0.0223(14) 0.0241(12) -0.0003(11) 0.0028(10) -0.0045(11) C11 0.043(2) 0.043(2) 0.0511(19) -0.0068(16) 0.0271(16) -0.0011(17) C12 0.0387(19) 0.054(2) 0.0264(14) 0.0109(14) -0.0035(13) -0.0108(16) C13 0.0212(14) 0.0141(13) 0.0234(12) 0.0007(10) 0.0023(10) -0.0011(10) C14 0.0205(14) 0.0270(15) 0.0296(14) 0.0027(12) -0.0024(11) -0.0005(12) C15 0.0302(17) 0.0307(17) 0.0290(14) 0.0059(12) -0.0032(12) 0.0013(13) C16 0.0345(18) 0.0326(17) 0.0306(14) 0.0073(13) 0.0059(13) 0.0000(14) C17 0.0228(15) 0.0329(17) 0.0331(14) 0.0090(13) 0.0039(12) -0.0055(13) C18 0.0233(14) 0.0149(13) 0.0243(12) -0.0006(10) 0.0005(10) 0.0002(11) C19 0.0144(13) 0.0321(17) 0.0309(14) -0.0029(12) 0.0001(11) -0.0003(12) C20 0.0320(19) 0.041(2) 0.059(2) -0.0217(16) 0.0111(16) -0.0013(15) C21 0.0248(17) 0.044(2) 0.065(2) -0.0093(17) 0.0153(16) -0.0074(15) C22 0.0238(15) 0.0185(14) 0.0342(14) -0.0016(11) 0.0024(11) -0.0088(11) C23 0.0358(19) 0.042(2) 0.0400(17) -0.0114(15) -0.0087(14) -0.0091(15) C24 0.046(2) 0.0228(16) 0.0459(17) -0.0099(14) 0.0046(15) -0.0049(15) C25 0.0289(16) 0.0231(15) 0.0266(13) 0.0004(11) -0.0029(11) -0.0057(12) O1 0.0247(11) 0.0217(10) 0.0321(10) -0.0036(8) 0.0031(8) 0.0063(8) O2 0.0639(18) 0.0464(15) 0.0312(11) -0.0114(10) 0.0088(11) -0.0141(13) P1 0.0132(3) 0.0160(3) 0.0224(3) -0.0004(3) -0.0001(2) 0.0007(3) P2 0.0155(3) 0.0151(3) 0.0191(3) -0.0009(2) 0.0005(2) -0.0011(3) P3 0.0148(3) 0.0185(3) 0.0228(3) -0.0011(3) 0.0000(3) -0.0023(3) Cl1 0.0197(3) 0.0274(4) 0.0508(4) 0.0085(3) -0.0069(3) 0.0033(3) Ir1 0.01272(5) 0.01450(5) 0.02086(5) -0.00052(4) -0.00113(3) -0.00061(4) #----------------------------------------------------------------------------# # 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 1.394(4) . ? C1 C6 1.407(4) . ? C1 P1 1.834(3) . ? C2 C3 1.390(4) . ? C2 H2 0.95 . ? C3 C4 1.376(4) . ? C3 H3 0.95 . ? C4 C5 1.383(4) . ? C4 H4 0.95 . ? C5 C6 1.407(4) . ? C5 H5 0.95 . ? C6 P2 1.821(3) . ? C7 C9 1.525(4) . ? C7 C8 1.532(4) . ? C7 P2 1.854(3) . ? C7 H7 1 . ? C8 H8A 0.98 . ? C8 H8B 0.98 . ? C8 H8C 0.98 . ? C9 H9A 0.98 . ? C9 H9B 0.98 . ? C9 H9C 0.98 . ? C10 C11 1.518(4) . ? C10 C12 1.528(4) . ? C10 P2 1.844(2) . ? C10 H10 1 . ? C11 H11A 0.98 . ? C11 H11B 0.98 . ? C11 H11C 0.98 . ? C12 H12A 0.98 . ? C12 H12B 0.98 . ? C12 H12C 0.98 . ? C13 C14 1.399(3) . ? C13 C18 1.401(4) . ? C13 P1 1.840(2) . ? C14 C15 1.390(4) . ? C14 H14 0.95 . ? C15 C16 1.375(4) . ? C15 H15 0.95 . ? C16 C17 1.392(4) . ? C16 H16 0.95 . ? C17 C18 1.403(4) . ? C17 H17 0.95 . ? C18 P3 1.830(3) . ? C19 C20 1.524(4) . ? C19 C21 1.528(4) . ? C19 P3 1.853(3) . ? C19 H19 1 . ? C20 H20A 0.98 . ? C20 H20B 0.98 . ? C20 H20C 0.98 . ? C21 H21A 0.98 . ? C21 H21B 0.98 . ? C21 H21C 0.98 . ? C22 C24 1.515(4) . ? C22 C23 1.543(4) . ? C22 P3 1.844(3) . ? C22 H22 1 . ? C23 H23A 0.98 . ? C23 H23B 0.98 . ? C23 H23C 0.98 . ? C24 H24A 0.98 . ? C24 H24B 0.98 . ? C24 H24C 0.98 . ? C25 O2 1.127(3) . ? C25 Ir1 1.943(3) . ? O1 P1 1.4988(18) . ? P1 Ir1 2.2587(7) . ? P2 Ir1 2.3318(7) . ? P3 Ir1 2.3324(7) . ? Cl1 Ir1 2.4947(7) . ? Ir1 H1 1.54(2) . ? 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 119.3(2) . . ? C2 C1 P1 121.0(2) . . ? C6 C1 P1 118.99(19) . . ? C3 C2 C1 120.5(3) . . ? C3 C2 H2 119.8 . . ? C1 C2 H2 119.8 . . ? C4 C3 C2 120.2(3) . . ? C4 C3 H3 119.9 . . ? C2 C3 H3 119.9 . . ? C3 C4 C5 120.5(3) . . ? C3 C4 H4 119.8 . . ? C5 C4 H4 119.8 . . ? C4 C5 C6 120.2(3) . . ? C4 C5 H5 119.9 . . ? C6 C5 H5 119.9 . . ? C1 C6 C5 119.3(2) . . ? C1 C6 P2 118.42(19) . . ? C5 C6 P2 121.8(2) . . ? C9 C7 C8 109.7(2) . . ? C9 C7 P2 115.8(2) . . ? C8 C7 P2 111.77(19) . . ? C9 C7 H7 106.3 . . ? C8 C7 H7 106.3 . . ? P2 C7 H7 106.3 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C11 C10 C12 111.4(2) . . ? C11 C10 P2 111.11(19) . . ? C12 C10 P2 110.18(19) . . ? C11 C10 H10 108 . . ? C12 C10 H10 108 . . ? P2 C10 H10 108 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C14 C13 C18 119.4(2) . . ? C14 C13 P1 122.5(2) . . ? C18 C13 P1 117.63(19) . . ? C15 C14 C13 120.4(3) . . ? C15 C14 H14 119.8 . . ? C13 C14 H14 119.8 . . ? C16 C15 C14 120.3(3) . . ? C16 C15 H15 119.9 . . ? C14 C15 H15 119.9 . . ? C15 C16 C17 120.4(3) . . ? C15 C16 H16 119.8 . . ? C17 C16 H16 119.8 . . ? C16 C17 C18 120.0(3) . . ? C16 C17 H17 120 . . ? C18 C17 H17 120 . . ? C13 C18 C17 119.6(2) . . ? C13 C18 P3 117.94(19) . . ? C17 C18 P3 122.4(2) . . ? C20 C19 C21 109.2(2) . . ? C20 C19 P3 112.5(2) . . ? C21 C19 P3 117.4(2) . . ? C20 C19 H19 105.6 . . ? C21 C19 H19 105.6 . . ? P3 C19 H19 105.6 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C24 C22 C23 112.2(2) . . ? C24 C22 P3 111.4(2) . . ? C23 C22 P3 110.0(2) . . ? C24 C22 H22 107.7 . . ? C23 C22 H22 107.7 . . ? P3 C22 H22 107.7 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? O2 C25 Ir1 178.7(3) . . ? O1 P1 C1 107.59(11) . . ? O1 P1 C13 108.21(11) . . ? C1 P1 C13 108.74(11) . . ? O1 P1 Ir1 119.59(8) . . ? C1 P1 Ir1 107.25(9) . . ? C13 P1 Ir1 105.11(9) . . ? C6 P2 C10 102.93(12) . . ? C6 P2 C7 109.23(12) . . ? C10 P2 C7 105.67(12) . . ? C6 P2 Ir1 106.02(9) . . ? C10 P2 Ir1 120.20(9) . . ? C7 P2 Ir1 112.09(9) . . ? C18 P3 C22 104.51(12) . . ? C18 P3 C19 110.28(12) . . ? C22 P3 C19 104.46(13) . . ? C18 P3 Ir1 104.31(9) . . ? C22 P3 Ir1 119.80(9) . . ? C19 P3 Ir1 113.05(10) . . ? C25 Ir1 P1 93.15(9) . . ? C25 Ir1 P2 102.64(8) . . ? P1 Ir1 P2 87.07(2) . . ? C25 Ir1 P3 102.50(8) . . ? P1 Ir1 P3 85.46(2) . . ? P2 Ir1 P3 154.10(2) . . ? C25 Ir1 Cl1 89.42(9) . . ? P1 Ir1 Cl1 177.31(2) . . ? P2 Ir1 Cl1 93.14(2) . . ? P3 Ir1 Cl1 93.22(2) . . ? C25 Ir1 H1 177.7(10) . . ? P1 Ir1 H1 86.7(10) . . ? P2 Ir1 H1 75.1(10) . . ? P3 Ir1 H1 79.7(10) . . ? Cl1 Ir1 H1 90.8(10) . . ? #===END data_4 #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C24 H37 O P3 Pd ' _chemical_formula_sum 'C24 H37 O P3 Pd' _chemical_formula_weight 540.85 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 15.3362(5) _cell_length_b 11.3804(4) _cell_length_c 15.2944(5) _cell_angle_alpha 90 _cell_angle_beta 104.799(2) _cell_angle_gamma 90 _cell_volume 2580.82(15) _cell_formula_units_Z 4 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 9337 _cell_measurement_theta_min 2.26 _cell_measurement_theta_max 31.15 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_diffrn 1.392 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1120 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.918 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(SADABS; Bruker, 2006)' _exptl_absorpt_correction_T_min 0.8020 _exptl_absorpt_correction_T_max 0.8320 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 193(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_radiation_probe x-ray _diffrn_reflns_av_R_equivalents 0.0266 _diffrn_reflns_av_unetI/netI 0.0129 _diffrn_reflns_number 49439 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.27 _diffrn_reflns_theta_max 25.35 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.993 _diffrn_measured_fraction_theta_max 0.993 _reflns_number_total 4686 _reflns_number_gt 4304 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'APEX2 (Bruker, 2006)' _computing_cell_refinement 'APEX2 and SAINT (Bruker, 2006)' _computing_data_reduction 'SAINT (Bruker, 2006)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # 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^)+(0.0220P)^2^+2.2483P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 4686 _refine_ls_number_parameters 299 _refine_ls_number_restraints 66 _refine_ls_R_factor_all 0.0249 _refine_ls_R_factor_gt 0.0213 _refine_ls_wR_factor_ref 0.0577 _refine_ls_wR_factor_gt 0.0547 _refine_ls_goodness_of_fit_ref 1.086 _refine_ls_restrained_S_all 1.098 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.351 _refine_diff_density_min -0.561 _refine_diff_density_rms 0.076 #----------------------------------------------------------------------------# # 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' O O 0.0106 0.006 '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' P P 0.1023 0.0942 '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 0.36377(15) 0.47388(19) 0.53314(13) 0.0310(4) Uani 1 1 d . A . C2 C 0.44472(15) 0.4281(2) 0.58496(15) 0.0389(5) Uani 1 1 d . . . H2 H 0.4562 0.3464 0.5823 0.047 Uiso 1 1 calc R . . C3 C 0.50859(17) 0.4992(2) 0.64007(17) 0.0433(6) Uani 1 1 d . . . H3 H 0.5641 0.4665 0.6736 0.052 Uiso 1 1 calc R . . C4 C 0.49217(16) 0.6174(2) 0.64663(16) 0.0435(6) Uani 1 1 d . . . H4 H 0.5356 0.6659 0.6857 0.052 Uiso 1 1 calc R . . C5 C 0.41247(17) 0.6649(2) 0.59630(16) 0.0433(6) Uani 1 1 d . . . H5 H 0.4012 0.7464 0.6009 0.052 Uiso 1 1 calc R . . C6 C 0.34811(15) 0.5946(2) 0.53870(14) 0.0344(5) Uani 1 1 d . A . C7 C 0.27638(19) 0.7962(2) 0.42845(17) 0.0474(6) Uani 1 1 d . A . H7 H 0.3092 0.8419 0.4827 0.057 Uiso 1 1 calc R . . C8 C 0.34095(19) 0.7742(2) 0.3696(2) 0.0548(7) Uani 1 1 d . . . H8A H 0.3114 0.7249 0.318 0.082 Uiso 1 1 calc R . . H8B H 0.395 0.7341 0.4053 0.082 Uiso 1 1 calc R . . H8C H 0.3582 0.8493 0.3476 0.082 Uiso 1 1 calc R . . C9 C 0.1952(2) 0.8684(3) 0.37790(19) 0.0631(8) Uani 1 1 d . . . H9A H 0.2161 0.9412 0.3558 0.095 Uiso 1 1 calc R . . H9B H 0.1574 0.8874 0.4189 0.095 Uiso 1 1 calc R . . H9C H 0.1598 0.8229 0.3266 0.095 Uiso 1 1 calc R . . P2 P 0.24237(4) 0.65374(5) 0.46744(4) 0.03473(13) Uani 1 1 d D . . C10 C 0.1773(4) 0.6986(6) 0.5477(4) 0.0448(13) Uani 0.64 1 d PDU A 1 H10 H 0.1983 0.7785 0.5711 0.054 Uiso 0.64 1 calc PR A 1 C11 C 0.1928(3) 0.6163(5) 0.6269(3) 0.0617(11) Uani 0.64 1 d PDU A 1 H11A H 0.1574 0.6424 0.6684 0.093 Uiso 0.64 1 calc PR A 1 H11B H 0.257 0.6159 0.6585 0.093 Uiso 0.64 1 calc PR A 1 H11C H 0.174 0.5368 0.6054 0.093 Uiso 0.64 1 calc PR A 1 C12 C 0.0811(3) 0.7078(5) 0.4965(3) 0.0592(11) Uani 0.64 1 d PDU A 1 H12A H 0.0561 0.6289 0.482 0.089 Uiso 0.64 1 calc PR A 1 H12B H 0.0769 0.7515 0.4403 0.089 Uiso 0.64 1 calc PR A 1 H12C H 0.0471 0.7492 0.5333 0.089 Uiso 0.64 1 calc PR A 1 C10' C 0.1580(8) 0.6726(13) 0.5375(8) 0.0502(19) Uani 0.36 1 d PDU A 2 H10' H 0.1136 0.733 0.5061 0.06 Uiso 0.36 1 calc PR A 2 C11' C 0.2024(6) 0.7214(9) 0.6293(5) 0.0675(19) Uani 0.36 1 d PDU A 2 H11D H 0.1571 0.7317 0.6638 0.101 Uiso 0.36 1 calc PR A 2 H11E H 0.2298 0.7975 0.6226 0.101 Uiso 0.36 1 calc PR A 2 H11F H 0.2491 0.6669 0.6614 0.101 Uiso 0.36 1 calc PR A 2 C12' C 0.1047(6) 0.5639(7) 0.5449(6) 0.064(2) Uani 0.36 1 d PDU A 2 H12D H 0.1427 0.5088 0.5873 0.095 Uiso 0.36 1 calc PR A 2 H12E H 0.0846 0.5268 0.4853 0.095 Uiso 0.36 1 calc PR A 2 H12F H 0.0521 0.5851 0.5668 0.095 Uiso 0.36 1 calc PR A 2 C13 C 0.31211(14) 0.27104(18) 0.40648(13) 0.0298(4) Uani 1 1 d . A . C14 C 0.37450(17) 0.1861(2) 0.44825(15) 0.0390(5) Uani 1 1 d . . . H14 H 0.3958 0.1855 0.5123 0.047 Uiso 1 1 calc R . . C15 C 0.40576(17) 0.1031(2) 0.39828(16) 0.0438(6) Uani 1 1 d . . . H15 H 0.4494 0.0471 0.4277 0.053 Uiso 1 1 calc R . . C16 C 0.37315(16) 0.1013(2) 0.30426(15) 0.0392(5) Uani 1 1 d . . . H16 H 0.3962 0.0459 0.2694 0.047 Uiso 1 1 calc R . . C17 C 0.30747(15) 0.17991(19) 0.26211(14) 0.0328(5) Uani 1 1 d . . . H17 H 0.2837 0.1766 0.1984 0.039 Uiso 1 1 calc R . . C18 C 0.27575(13) 0.26443(18) 0.31260(13) 0.0286(4) Uani 1 1 d . A . C19 C 0.19040(16) 0.3930(2) 0.14730(14) 0.0382(5) Uani 1 1 d . A . H19 H 0.1938 0.3163 0.1164 0.046 Uiso 1 1 calc R . . C20 C 0.27690(18) 0.4614(3) 0.15100(17) 0.0496(6) Uani 1 1 d . . . H20A H 0.2812 0.4778 0.0894 0.074 Uiso 1 1 calc R . . H20B H 0.3291 0.4146 0.1828 0.074 Uiso 1 1 calc R . . H20C H 0.2759 0.5356 0.1832 0.074 Uiso 1 1 calc R . . C21 C 0.10706(19) 0.4591(3) 0.09365(17) 0.0539(7) Uani 1 1 d . . . H21A H 0.1022 0.5343 0.1233 0.081 Uiso 1 1 calc R . . H21B H 0.053 0.4119 0.0911 0.081 Uiso 1 1 calc R . . H21C H 0.1125 0.4736 0.0321 0.081 Uiso 1 1 calc R . . C22 C 0.08051(16) 0.2685(2) 0.24985(16) 0.0446(6) Uani 1 1 d . A . H22 H 0.0275 0.3147 0.215 0.053 Uiso 1 1 calc R . . C23 C 0.0643(2) 0.2407(3) 0.3417(2) 0.0722(10) Uani 1 1 d . . . H23A H 0.0086 0.195 0.3334 0.108 Uiso 1 1 calc R . . H23B H 0.0588 0.3141 0.3733 0.108 Uiso 1 1 calc R . . H23C H 0.1151 0.1949 0.3775 0.108 Uiso 1 1 calc R . . C24 C 0.0838(2) 0.1545(3) 0.1978(2) 0.0640(8) Uani 1 1 d . . . H24A H 0.1325 0.1046 0.2324 0.096 Uiso 1 1 calc R . . H24B H 0.0947 0.1729 0.1389 0.096 Uiso 1 1 calc R . . H24C H 0.0261 0.1131 0.1888 0.096 Uiso 1 1 calc R . . O1 O 0.22813(11) 0.32632(15) 0.53816(10) 0.0422(4) Uani 1 1 d . A . Pd1 Pd 0.192223(10) 0.514140(15) 0.360536(10) 0.02993(6) Uani 1 1 d . A . P1 P 0.26792(4) 0.38515(5) 0.46921(3) 0.02955(12) Uani 1 1 d . . . P3 P 0.18137(4) 0.36235(5) 0.26280(3) 0.03091(13) Uani 1 1 d . . . H101 H 0.1444(17) 0.609(2) 0.2813(17) 0.054(7) Uiso 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 0.0378(11) 0.0353(12) 0.0209(10) 0.0000(8) 0.0093(8) 0.0042(9) C2 0.0425(13) 0.0359(12) 0.0359(12) -0.0008(10) 0.0057(10) 0.0080(10) C3 0.0369(12) 0.0508(15) 0.0379(13) -0.0018(11) 0.0018(10) 0.0059(10) C4 0.0441(13) 0.0461(14) 0.0366(12) -0.0038(11) 0.0039(10) -0.0047(11) C5 0.0546(15) 0.0348(13) 0.0376(13) -0.0036(10) 0.0065(11) 0.0032(11) C6 0.0431(12) 0.0370(12) 0.0228(10) -0.0004(9) 0.0078(9) 0.0080(10) C7 0.0685(17) 0.0307(12) 0.0370(13) -0.0017(10) 0.0022(12) 0.0103(11) C8 0.0602(17) 0.0413(14) 0.0642(18) 0.0120(13) 0.0182(14) -0.0005(12) C9 0.092(2) 0.0499(17) 0.0494(16) 0.0129(13) 0.0214(15) 0.0333(15) P2 0.0451(3) 0.0358(3) 0.0235(3) 0.0002(2) 0.0090(2) 0.0129(2) C10 0.054(3) 0.053(3) 0.030(2) -0.0027(19) 0.016(2) 0.017(2) C11 0.071(3) 0.084(3) 0.037(2) 0.010(2) 0.0275(19) 0.018(2) C12 0.049(2) 0.085(3) 0.047(2) 0.000(2) 0.0196(18) 0.008(2) C10' 0.061(4) 0.061(4) 0.035(3) -0.004(3) 0.022(3) 0.020(3) C11' 0.073(4) 0.090(5) 0.043(3) -0.024(3) 0.020(3) 0.009(4) C12' 0.077(5) 0.058(4) 0.077(5) -0.007(4) 0.060(4) 0.000(4) C13 0.0367(11) 0.0288(11) 0.0241(10) 0.0016(8) 0.0085(8) -0.0023(9) C14 0.0555(14) 0.0328(12) 0.0253(11) 0.0030(9) 0.0042(10) 0.0022(10) C15 0.0581(15) 0.0299(12) 0.0392(13) 0.0035(10) 0.0047(11) 0.0102(11) C16 0.0535(14) 0.0292(11) 0.0361(12) -0.0030(9) 0.0135(10) 0.0021(10) C17 0.0404(12) 0.0325(11) 0.0254(10) -0.0005(9) 0.0079(9) -0.0032(9) C18 0.0317(10) 0.0298(11) 0.0244(10) 0.0023(8) 0.0074(8) -0.0023(8) C19 0.0488(13) 0.0414(13) 0.0220(10) 0.0011(9) 0.0045(9) 0.0044(10) C20 0.0562(16) 0.0614(17) 0.0333(13) 0.0107(12) 0.0156(11) 0.0030(13) C21 0.0580(16) 0.0627(17) 0.0326(13) 0.0079(12) -0.0037(11) 0.0056(13) C22 0.0322(12) 0.0559(15) 0.0437(13) -0.0063(11) 0.0061(10) -0.0066(11) C23 0.0578(18) 0.101(3) 0.0668(19) -0.0183(18) 0.0332(15) -0.0361(18) C24 0.0582(17) 0.0670(19) 0.0695(19) -0.0219(16) 0.0213(15) -0.0259(15) O1 0.0505(10) 0.0519(10) 0.0275(8) 0.0053(7) 0.0159(7) -0.0036(8) Pd1 0.03070(10) 0.03681(11) 0.02189(9) 0.00146(6) 0.00603(6) 0.00586(6) P1 0.0360(3) 0.0341(3) 0.0193(2) 0.0019(2) 0.0083(2) 0.0025(2) P3 0.0302(3) 0.0383(3) 0.0226(3) -0.0001(2) 0.0038(2) 0.0009(2) #----------------------------------------------------------------------------# # 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 1.392(3) . ? C1 C6 1.401(3) . ? C1 P1 1.845(2) . ? C2 C3 1.379(3) . ? C2 H2 0.95 . ? C3 C4 1.377(3) . ? C3 H3 0.95 . ? C4 C5 1.378(3) . ? C4 H4 0.95 . ? C5 C6 1.395(3) . ? C5 H5 0.95 . ? C6 P2 1.835(2) . ? C7 C8 1.519(4) . ? C7 C9 1.527(3) . ? C7 P2 1.848(3) . ? C7 H7 1 . ? C8 H8A 0.98 . ? C8 H8B 0.98 . ? C8 H8C 0.98 . ? C9 H9A 0.98 . ? C9 H9B 0.98 . ? C9 H9C 0.98 . ? P2 C10 1.842(6) . ? P2 C10' 1.891(11) . ? P2 Pd1 2.2685(6) . ? C10 C12 1.486(7) . ? C10 C11 1.501(8) . ? C10 H10 1 . ? C11 H11A 0.98 . ? C11 H11B 0.98 . ? C11 H11C 0.98 . ? C12 H12A 0.98 . ? C12 H12B 0.98 . ? C12 H12C 0.98 . ? C10' C11' 1.501(11) . ? C10' C12' 1.503(13) . ? C10' H10' 1 . ? C11' H11D 0.98 . ? C11' H11E 0.98 . ? C11' H11F 0.98 . ? C12' H12D 0.98 . ? C12' H12E 0.98 . ? C12' H12F 0.98 . ? C13 C14 1.395(3) . ? C13 C18 1.403(3) . ? C13 P1 1.843(2) . ? C14 C15 1.376(3) . ? C14 H14 0.95 . ? C15 C16 1.397(3) . ? C15 H15 0.95 . ? C16 C17 1.378(3) . ? C16 H16 0.95 . ? C17 C18 1.397(3) . ? C17 H17 0.95 . ? C18 P3 1.831(2) . ? C19 C20 1.527(4) . ? C19 C21 1.529(3) . ? C19 P3 1.840(2) . ? C19 H19 1 . ? C20 H20A 0.98 . ? C20 H20B 0.98 . ? C20 H20C 0.98 . ? C21 H21A 0.98 . ? C21 H21B 0.98 . ? C21 H21C 0.98 . ? C22 C23 1.521(4) . ? C22 C24 1.530(4) . ? C22 P3 1.848(2) . ? C22 H22 1 . ? C23 H23A 0.98 . ? C23 H23B 0.98 . ? C23 H23C 0.98 . ? C24 H24A 0.98 . ? C24 H24B 0.98 . ? C24 H24C 0.98 . ? O1 P1 1.5038(15) . ? Pd1 P3 2.2626(6) . ? Pd1 P1 2.2976(5) . ? Pd1 H101 1.65(3) . ? 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 118.3(2) . . ? C2 C1 P1 124.84(17) . . ? C6 C1 P1 116.31(16) . . ? C3 C2 C1 121.3(2) . . ? C3 C2 H2 119.3 . . ? C1 C2 H2 119.3 . . ? C4 C3 C2 120.2(2) . . ? C4 C3 H3 119.9 . . ? C2 C3 H3 119.9 . . ? C3 C4 C5 119.7(2) . . ? C3 C4 H4 120.2 . . ? C5 C4 H4 120.2 . . ? C4 C5 C6 120.8(2) . . ? C4 C5 H5 119.6 . . ? C6 C5 H5 119.6 . . ? C5 C6 C1 119.7(2) . . ? C5 C6 P2 122.69(17) . . ? C1 C6 P2 117.57(17) . . ? C8 C7 C9 111.1(2) . . ? C8 C7 P2 109.08(16) . . ? C9 C7 P2 112.0(2) . . ? C8 C7 H7 108.2 . . ? C9 C7 H7 108.2 . . ? P2 C7 H7 108.2 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C6 P2 C10 104.6(2) . . ? C6 P2 C7 103.53(11) . . ? C10 P2 C7 102.6(2) . . ? C6 P2 C10' 109.5(5) . . ? C7 P2 C10' 111.9(5) . . ? C6 P2 Pd1 104.87(7) . . ? C10 P2 Pd1 122.21(18) . . ? C7 P2 Pd1 116.97(8) . . ? C10' P2 Pd1 109.4(3) . . ? C12 C10 C11 113.6(5) . . ? C12 C10 P2 107.5(4) . . ? C11 C10 P2 111.3(5) . . ? C12 C10 H10 108 . . ? C11 C10 H10 108 . . ? P2 C10 H10 108 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11' C10' C12' 111.1(10) . . ? C11' C10' P2 111.1(7) . . ? C12' C10' P2 114.4(8) . . ? C11' C10' H10' 106.6 . . ? C12' C10' H10' 106.6 . . ? P2 C10' H10' 106.6 . . ? C10' C11' H11D 109.5 . . ? C10' C11' H11E 109.5 . . ? H11D C11' H11E 109.5 . . ? C10' C11' H11F 109.5 . . ? H11D C11' H11F 109.5 . . ? H11E C11' H11F 109.5 . . ? C10' C12' H12D 109.5 . . ? C10' C12' H12E 109.5 . . ? H12D C12' H12E 109.5 . . ? C10' C12' H12F 109.5 . . ? H12D C12' H12F 109.5 . . ? H12E C12' H12F 109.5 . . ? C14 C13 C18 118.57(19) . . ? C14 C13 P1 123.38(16) . . ? C18 C13 P1 117.87(15) . . ? C15 C14 C13 121.1(2) . . ? C15 C14 H14 119.4 . . ? C13 C14 H14 119.4 . . ? C14 C15 C16 119.9(2) . . ? C14 C15 H15 120.1 . . ? C16 C15 H15 120.1 . . ? C17 C16 C15 119.9(2) . . ? C17 C16 H16 120 . . ? C15 C16 H16 120 . . ? C16 C17 C18 120.32(19) . . ? C16 C17 H17 119.8 . . ? C18 C17 H17 119.8 . . ? C17 C18 C13 119.95(19) . . ? C17 C18 P3 122.62(15) . . ? C13 C18 P3 117.27(15) . . ? C20 C19 C21 111.6(2) . . ? C20 C19 P3 109.80(15) . . ? C21 C19 P3 110.54(17) . . ? C20 C19 H19 108.3 . . ? C21 C19 H19 108.3 . . ? P3 C19 H19 108.3 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C23 C22 C24 109.8(2) . . ? C23 C22 P3 110.57(17) . . ? C24 C22 P3 114.09(17) . . ? C23 C22 H22 107.4 . . ? C24 C22 H22 107.4 . . ? P3 C22 H22 107.4 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? P3 Pd1 P2 164.81(2) . . ? P3 Pd1 P1 85.90(2) . . ? P2 Pd1 P1 84.86(2) . . ? P3 Pd1 H101 94.1(9) . . ? P2 Pd1 H101 94.3(9) . . ? P1 Pd1 H101 176.2(9) . . ? O1 P1 C13 108.68(9) . . ? O1 P1 C1 106.45(9) . . ? C13 P1 C1 108.21(10) . . ? O1 P1 Pd1 124.84(7) . . ? C13 P1 Pd1 104.99(7) . . ? C1 P1 Pd1 102.75(7) . . ? C18 P3 C19 105.62(10) . . ? C18 P3 C22 104.12(11) . . ? C19 P3 C22 105.82(11) . . ? C18 P3 Pd1 105.83(7) . . ? C19 P3 Pd1 118.61(8) . . ? C22 P3 Pd1 115.48(8) . . ? #===END data_7 #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C28 H43 O3 P3 Pd, C7 H8' _chemical_formula_sum 'C35 H51 O3 P3 Pd' _chemical_formula_weight 719.07 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 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 8.7055(3) _cell_length_b 14.7418(5) _cell_length_c 27.8417(10) _cell_angle_alpha 90 _cell_angle_beta 90.0300(10) _cell_angle_gamma 90 _cell_volume 3573.1(2) _cell_formula_units_Z 4 _cell_measurement_temperature 253(2) _cell_measurement_reflns_used 9893 _cell_measurement_theta_min 2.45 _cell_measurement_theta_max 27.69 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 1.337 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1504 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.685 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(SADABS; Bruker, 2008)' _exptl_absorpt_correction_T_min 0.906 _exptl_absorpt_correction_T_max 0.934 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 253(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'microfocus sealed tube' _diffrn_radiation_monochromator 'multilayer optics' _diffrn_measurement_device_type 'Bruker Kappa APEX II Quazar' _diffrn_measurement_method 'phi and omega scans' _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_radiation_probe x-ray _diffrn_reflns_av_R_equivalents 0.0352 _diffrn_reflns_av_unetI/netI 0.0326 _diffrn_reflns_number 35456 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 5.1 _diffrn_reflns_theta_max 26.37 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.987 _diffrn_measured_fraction_theta_max 0.987 _reflns_number_total 7221 _reflns_number_gt 5837 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'APEX2 (Bruker, 2008)' _computing_cell_refinement 'APEX2 and SAINT (Bruker, 2008)' _computing_data_reduction 'SAINT (Bruker, 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # 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^)+(0.0318P)^2^+2.1330P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 7221 _refine_ls_number_parameters 390 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.046 _refine_ls_R_factor_gt 0.031 _refine_ls_wR_factor_ref 0.0772 _refine_ls_wR_factor_gt 0.0694 _refine_ls_goodness_of_fit_ref 1.061 _refine_ls_restrained_S_all 1.061 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.499 _refine_diff_density_min -0.267 _refine_diff_density_rms 0.059 #----------------------------------------------------------------------------# # 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' O O 0.0106 0.006 '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 0.1585(3) 0.51613(16) 0.40924(8) 0.0312(5) Uani 1 1 d . . . C2 C 0.1243(3) 0.59517(17) 0.43423(9) 0.0415(6) Uani 1 1 d . . . H2 H 0.0968 0.5919 0.4665 0.05 Uiso 1 1 calc R . . C3 C 0.1308(4) 0.67839(18) 0.41168(11) 0.0481(7) Uani 1 1 d . . . H3 H 0.1116 0.7311 0.429 0.058 Uiso 1 1 calc R . . C4 C 0.1659(4) 0.68341(18) 0.36327(11) 0.0473(7) Uani 1 1 d . . . H4 H 0.1725 0.7397 0.3483 0.057 Uiso 1 1 calc R . . C5 C 0.1909(3) 0.60598(18) 0.33718(10) 0.0424(6) Uani 1 1 d . . . H5 H 0.2104 0.6098 0.3044 0.051 Uiso 1 1 calc R . . C6 C 0.1872(3) 0.52093(16) 0.35975(8) 0.0321(5) Uani 1 1 d . . . C7 C 0.3486(3) 0.4435(2) 0.27988(9) 0.0416(6) Uani 1 1 d . . . H7 H 0.3213 0.5041 0.2683 0.05 Uiso 1 1 calc R . . C8 C 0.3460(4) 0.3813(2) 0.23678(11) 0.0628(9) Uani 1 1 d . . . H8A H 0.4319 0.3947 0.2164 0.094 Uiso 1 1 calc R . . H8B H 0.2522 0.3903 0.2192 0.094 Uiso 1 1 calc R . . H8C H 0.352 0.3194 0.2473 0.094 Uiso 1 1 calc R . . C9 C 0.5066(3) 0.4514(2) 0.30293(11) 0.0543(8) Uani 1 1 d . . . H9A H 0.535 0.3941 0.3167 0.081 Uiso 1 1 calc R . . H9B H 0.5039 0.4967 0.3277 0.081 Uiso 1 1 calc R . . H9C H 0.5805 0.4683 0.279 0.081 Uiso 1 1 calc R . . C10 C 0.0227(3) 0.39682(19) 0.29565(9) 0.0411(6) Uani 1 1 d . . . H10 H 0.0366 0.3448 0.2742 0.049 Uiso 1 1 calc R . . C11 C -0.0291(4) 0.4757(2) 0.26433(11) 0.0591(9) Uani 1 1 d . . . H11A H -0.1178 0.458 0.2461 0.089 Uiso 1 1 calc R . . H11B H 0.0523 0.4924 0.2428 0.089 Uiso 1 1 calc R . . H11C H -0.0547 0.5266 0.2843 0.089 Uiso 1 1 calc R . . C12 C -0.1011(3) 0.3701(3) 0.33169(12) 0.0624(9) Uani 1 1 d . . . H12A H -0.1272 0.4217 0.3511 0.094 Uiso 1 1 calc R . . H12B H -0.0633 0.3223 0.3519 0.094 Uiso 1 1 calc R . . H12C H -0.1906 0.3495 0.3148 0.094 Uiso 1 1 calc R . . C13 C 0.2815(3) 0.40484(16) 0.48958(8) 0.0311(5) Uani 1 1 d . . . C14 C 0.2824(4) 0.47255(19) 0.52387(10) 0.0467(7) Uani 1 1 d . . . H14 H 0.2251 0.525 0.5189 0.056 Uiso 1 1 calc R . . C15 C 0.3678(4) 0.4630(2) 0.56551(10) 0.0550(8) Uani 1 1 d . . . H15 H 0.3712 0.5102 0.5877 0.066 Uiso 1 1 calc R . . C16 C 0.4473(4) 0.3844(2) 0.57430(10) 0.0566(8) Uani 1 1 d . . . H16 H 0.504 0.3782 0.6024 0.068 Uiso 1 1 calc R . . C17 C 0.4432(4) 0.3152(2) 0.54162(10) 0.0527(8) Uani 1 1 d . . . H17 H 0.4942 0.2612 0.5482 0.063 Uiso 1 1 calc R . . C18 C 0.3629(3) 0.32509(16) 0.49837(9) 0.0355(6) Uani 1 1 d . . . C19 C 0.5502(3) 0.19393(17) 0.44354(10) 0.0405(6) Uani 1 1 d . . . H19 H 0.5458 0.1557 0.4148 0.049 Uiso 1 1 calc R . . C20 C 0.6557(4) 0.2732(2) 0.43089(13) 0.0599(8) Uani 1 1 d . . . H20A H 0.6762 0.3082 0.4592 0.09 Uiso 1 1 calc R . . H20B H 0.6068 0.3109 0.4073 0.09 Uiso 1 1 calc R . . H20C H 0.7506 0.2502 0.4182 0.09 Uiso 1 1 calc R . . C21 C 0.6220(4) 0.1353(2) 0.48266(12) 0.0591(8) Uani 1 1 d . . . H21A H 0.7172 0.1105 0.4713 0.089 Uiso 1 1 calc R . . H21B H 0.5531 0.0868 0.4907 0.089 Uiso 1 1 calc R . . H21C H 0.6409 0.1717 0.5106 0.089 Uiso 1 1 calc R . . C22 C 0.2443(3) 0.14415(17) 0.48230(11) 0.0443(7) Uani 1 1 d . . . H22 H 0.3013 0.1255 0.511 0.053 Uiso 1 1 calc R . . C23 C 0.0881(4) 0.1785(2) 0.49828(18) 0.0842(13) Uani 1 1 d . . . H23A H 0.03 0.1974 0.4707 0.126 Uiso 1 1 calc R . . H23B H 0.1013 0.2291 0.5196 0.126 Uiso 1 1 calc R . . H23C H 0.0341 0.1309 0.5146 0.126 Uiso 1 1 calc R . . C24 C 0.2272(4) 0.0619(2) 0.45003(13) 0.0645(9) Uani 1 1 d . . . H24A H 0.1732 0.015 0.467 0.097 Uiso 1 1 calc R . . H24B H 0.327 0.0402 0.4409 0.097 Uiso 1 1 calc R . . H24C H 0.1704 0.0784 0.4218 0.097 Uiso 1 1 calc R . . C25 C 0.3346(3) 0.18539(16) 0.33757(10) 0.0391(6) Uani 1 1 d . . . H25 H 0.3431 0.1334 0.3593 0.047 Uiso 1 1 calc R . . C26 C 0.4840(4) 0.1907(2) 0.31224(12) 0.0611(9) Uani 1 1 d . . . H26A H 0.5138 0.1312 0.3017 0.092 Uiso 1 1 calc R . . H26B H 0.5607 0.2143 0.3337 0.092 Uiso 1 1 calc R . . H26C H 0.4745 0.23 0.2849 0.092 Uiso 1 1 calc R . . C27 C 0.2006(4) 0.16964(19) 0.30982(11) 0.0509(8) Uani 1 1 d . . . C28 C -0.0633(5) 0.1213(3) 0.31058(16) 0.0885(13) Uani 1 1 d . . . H28A H -0.0857 0.1739 0.2915 0.133 Uiso 1 1 calc R . . H28B H -0.1443 0.112 0.3335 0.133 Uiso 1 1 calc R . . H28C H -0.0553 0.0691 0.2901 0.133 Uiso 1 1 calc R . . C29 C 0.3047(5) 0.2117(3) 0.66337(14) 0.0746(11) Uani 1 1 d . . . C30 C 0.1996(5) 0.1564(3) 0.64145(17) 0.0870(12) Uani 1 1 d . . . H30 H 0.0958 0.1711 0.6428 0.104 Uiso 1 1 calc R . . C31 C 0.2451(7) 0.0793(4) 0.61740(18) 0.1041(16) Uani 1 1 d . . . H31 H 0.1735 0.0422 0.6023 0.125 Uiso 1 1 calc R . . C32 C 0.3978(8) 0.0588(3) 0.61627(18) 0.1056(17) Uani 1 1 d . . . H32 H 0.4304 0.0062 0.6009 0.127 Uiso 1 1 calc R . . C33 C 0.5031(6) 0.1142(4) 0.63730(18) 0.0994(15) Uani 1 1 d . . . H33 H 0.6071 0.1003 0.6353 0.119 Uiso 1 1 calc R . . C34 C 0.4574(5) 0.1895(3) 0.66103(16) 0.0832(12) Uani 1 1 d . . . H34 H 0.53 0.2264 0.6759 0.1 Uiso 1 1 calc R . . C35 C 0.2546(8) 0.2954(4) 0.6886(2) 0.138(2) Uani 1 1 d . . . H35A H 0.1795 0.2802 0.7125 0.206 Uiso 1 1 calc R . . H35B H 0.2102 0.3367 0.6658 0.206 Uiso 1 1 calc R . . H35C H 0.3416 0.3235 0.7037 0.206 Uiso 1 1 calc R . . O1 O -0.00466(19) 0.38186(11) 0.45272(6) 0.0359(4) Uani 1 1 d . . . O2 O 0.0796(3) 0.13462(17) 0.33561(8) 0.0703(7) Uani 1 1 d . . . O3 O 0.1832(3) 0.18504(16) 0.26693(8) 0.0680(7) Uani 1 1 d . . . P1 P 0.15561(7) 0.40332(4) 0.43651(2) 0.02772(14) Uani 1 1 d . . . P2 P 0.20724(7) 0.41368(4) 0.32705(2) 0.03099(15) Uani 1 1 d . . . P3 P 0.35281(8) 0.23651(4) 0.45291(2) 0.03187(15) Uani 1 1 d . . . Pd1 Pd 0.26127(2) 0.303031(12) 0.383880(6) 0.02880(7) 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 0.0309(13) 0.0345(12) 0.0283(12) 0.0038(10) 0.0039(11) 0.0063(11) C2 0.0529(17) 0.0400(14) 0.0318(13) 0.0024(11) 0.0103(13) 0.0117(13) C3 0.0602(19) 0.0338(14) 0.0504(17) 0.0011(12) 0.0092(15) 0.0135(13) C4 0.0564(19) 0.0346(14) 0.0509(17) 0.0125(12) 0.0105(15) 0.0094(13) C5 0.0498(17) 0.0457(15) 0.0317(13) 0.0110(11) 0.0077(13) 0.0095(13) C6 0.0308(13) 0.0372(13) 0.0284(12) 0.0042(10) 0.0027(11) 0.0060(11) C7 0.0391(15) 0.0551(16) 0.0308(13) 0.0032(12) 0.0088(12) 0.0041(13) C8 0.064(2) 0.084(2) 0.0403(17) -0.0112(16) 0.0172(16) 0.0020(19) C9 0.0363(16) 0.076(2) 0.0511(18) 0.0030(16) 0.0075(14) -0.0018(15) C10 0.0360(15) 0.0521(16) 0.0351(14) 0.0004(12) -0.0026(12) 0.0059(13) C11 0.0526(19) 0.069(2) 0.0551(19) 0.0084(16) -0.0164(16) 0.0126(17) C12 0.0321(16) 0.095(3) 0.060(2) 0.0067(18) 0.0025(15) -0.0013(17) C13 0.0350(14) 0.0329(12) 0.0253(12) 0.0025(10) 0.0049(11) 0.0043(11) C14 0.0590(19) 0.0407(14) 0.0405(15) -0.0052(12) -0.0091(14) 0.0134(14) C15 0.073(2) 0.0519(17) 0.0405(16) -0.0132(13) -0.0126(16) 0.0122(16) C16 0.076(2) 0.0623(19) 0.0318(15) -0.0035(13) -0.0172(15) 0.0165(17) C17 0.071(2) 0.0491(16) 0.0380(15) -0.0007(12) -0.0147(15) 0.0206(16) C18 0.0420(15) 0.0359(13) 0.0285(12) 0.0023(10) 0.0013(12) 0.0037(11) C19 0.0364(14) 0.0385(14) 0.0466(15) 0.0015(12) 0.0001(12) 0.0053(12) C20 0.0422(18) 0.0597(19) 0.078(2) 0.0076(17) 0.0067(17) -0.0028(15) C21 0.0473(18) 0.0610(19) 0.069(2) 0.0100(16) -0.0084(17) 0.0169(16) C22 0.0444(16) 0.0369(14) 0.0515(17) 0.0125(12) 0.0041(14) 0.0039(13) C23 0.060(2) 0.063(2) 0.130(4) 0.028(2) 0.045(2) 0.0046(18) C24 0.074(2) 0.0419(16) 0.078(2) 0.0071(16) 0.002(2) -0.0128(16) C25 0.0427(15) 0.0283(12) 0.0463(15) -0.0088(11) -0.0014(13) 0.0116(12) C26 0.059(2) 0.062(2) 0.062(2) -0.0149(16) 0.0097(17) 0.0126(17) C27 0.070(2) 0.0396(15) 0.0429(17) -0.0110(12) 0.0113(16) 0.0060(15) C28 0.065(3) 0.100(3) 0.101(3) -0.016(3) -0.014(2) -0.018(2) C29 0.083(3) 0.078(3) 0.063(2) 0.0045(19) 0.011(2) 0.012(2) C30 0.065(3) 0.102(3) 0.094(3) 0.013(3) 0.005(2) 0.003(3) C31 0.126(5) 0.090(3) 0.096(4) 0.007(3) -0.009(3) -0.002(3) C32 0.151(5) 0.078(3) 0.088(3) -0.005(2) -0.008(4) 0.039(4) C33 0.094(4) 0.117(4) 0.087(3) 0.010(3) -0.001(3) 0.032(3) C34 0.075(3) 0.097(3) 0.077(3) 0.017(2) 0.001(2) 0.004(2) C35 0.159(6) 0.119(4) 0.134(5) -0.044(4) 0.029(4) 0.010(4) O1 0.0313(9) 0.0411(9) 0.0352(9) 0.0016(7) 0.0076(8) 0.0035(8) O2 0.0623(15) 0.0867(17) 0.0618(15) -0.0003(13) -0.0043(13) -0.0155(13) O3 0.0830(18) 0.0791(16) 0.0419(12) -0.0124(11) -0.0032(12) -0.0031(13) P1 0.0298(3) 0.0296(3) 0.0237(3) 0.0012(2) 0.0036(3) 0.0068(3) P2 0.0304(3) 0.0393(3) 0.0233(3) 0.0011(3) 0.0032(3) 0.0069(3) P3 0.0349(4) 0.0283(3) 0.0324(3) 0.0027(3) 0.0007(3) 0.0058(3) Pd1 0.03008(11) 0.03061(10) 0.02572(10) -0.00167(7) 0.00286(7) 0.00645(8) #----------------------------------------------------------------------------# # 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 1.389(3) . ? C1 C6 1.403(3) . ? C1 P1 1.828(2) . ? C2 C3 1.379(4) . ? C2 H2 0.93 . ? C3 C4 1.384(4) . ? C3 H3 0.93 . ? C4 C5 1.370(4) . ? C4 H4 0.93 . ? C5 C6 1.403(3) . ? C5 H5 0.93 . ? C6 P2 1.833(3) . ? C7 C8 1.510(4) . ? C7 C9 1.522(4) . ? C7 P2 1.853(3) . ? C7 H7 0.98 . ? C8 H8A 0.96 . ? C8 H8B 0.96 . ? C8 H8C 0.96 . ? C9 H9A 0.96 . ? C9 H9B 0.96 . ? C9 H9C 0.96 . ? C10 C11 1.522(4) . ? C10 C12 1.525(4) . ? C10 P2 1.845(3) . ? C10 H10 0.98 . ? C11 H11A 0.96 . ? C11 H11B 0.96 . ? C11 H11C 0.96 . ? C12 H12A 0.96 . ? C12 H12B 0.96 . ? C12 H12C 0.96 . ? C13 C14 1.381(3) . ? C13 C18 1.394(3) . ? C13 P1 1.839(2) . ? C14 C15 1.384(4) . ? C14 H14 0.93 . ? C15 C16 1.372(4) . ? C15 H15 0.93 . ? C16 C17 1.367(4) . ? C16 H16 0.93 . ? C17 C18 1.400(4) . ? C17 H17 0.93 . ? C18 P3 1.821(3) . ? C19 C21 1.524(4) . ? C19 C20 1.527(4) . ? C19 P3 1.848(3) . ? C19 H19 0.98 . ? C20 H20A 0.96 . ? C20 H20B 0.96 . ? C20 H20C 0.96 . ? C21 H21A 0.96 . ? C21 H21B 0.96 . ? C21 H21C 0.96 . ? C22 C24 1.516(4) . ? C22 C23 1.518(4) . ? C22 P3 1.848(3) . ? C22 H22 0.98 . ? C23 H23A 0.96 . ? C23 H23B 0.96 . ? C23 H23C 0.96 . ? C24 H24A 0.96 . ? C24 H24B 0.96 . ? C24 H24C 0.96 . ? C25 C27 1.418(4) . ? C25 C26 1.482(4) . ? C25 Pd1 2.254(2) . ? C25 H25 0.98 . ? C26 H26A 0.96 . ? C26 H26B 0.96 . ? C26 H26C 0.96 . ? C27 O3 1.225(4) . ? C27 O2 1.376(4) . ? C28 O2 1.439(4) . ? C28 H28A 0.96 . ? C28 H28B 0.96 . ? C28 H28C 0.96 . ? C29 C30 1.369(6) . ? C29 C34 1.371(6) . ? C29 C35 1.485(6) . ? C30 C31 1.377(7) . ? C30 H30 0.93 . ? C31 C32 1.363(7) . ? C31 H31 0.93 . ? C32 C33 1.360(7) . ? C32 H32 0.93 . ? C33 C34 1.352(6) . ? C33 H33 0.93 . ? C34 H34 0.93 . ? C35 H35A 0.96 . ? C35 H35B 0.96 . ? C35 H35C 0.96 . ? O1 P1 1.5004(18) . ? P1 Pd1 2.2760(6) . ? P2 Pd1 2.3204(6) . ? P3 Pd1 2.2998(6) . ? 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 119.2(2) . . ? C2 C1 P1 123.50(18) . . ? C6 C1 P1 117.15(18) . . ? C3 C2 C1 120.6(2) . . ? C3 C2 H2 119.7 . . ? C1 C2 H2 119.7 . . ? C2 C3 C4 120.0(3) . . ? C2 C3 H3 120 . . ? C4 C3 H3 120 . . ? C5 C4 C3 120.5(2) . . ? C5 C4 H4 119.8 . . ? C3 C4 H4 119.8 . . ? C4 C5 C6 120.2(2) . . ? C4 C5 H5 119.9 . . ? C6 C5 H5 119.9 . . ? C1 C6 C5 119.3(2) . . ? C1 C6 P2 117.49(18) . . ? C5 C6 P2 123.12(19) . . ? C8 C7 C9 113.3(3) . . ? C8 C7 P2 114.2(2) . . ? C9 C7 P2 108.65(18) . . ? C8 C7 H7 106.8 . . ? C9 C7 H7 106.8 . . ? P2 C7 H7 106.8 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C11 C10 C12 111.4(3) . . ? C11 C10 P2 115.2(2) . . ? C12 C10 P2 109.77(19) . . ? C11 C10 H10 106.6 . . ? C12 C10 H10 106.6 . . ? P2 C10 H10 106.6 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C14 C13 C18 119.0(2) . . ? C14 C13 P1 124.56(19) . . ? C18 C13 P1 115.67(18) . . ? C13 C14 C15 120.6(3) . . ? C13 C14 H14 119.7 . . ? C15 C14 H14 119.7 . . ? C16 C15 C14 120.4(3) . . ? C16 C15 H15 119.8 . . ? C14 C15 H15 119.8 . . ? C17 C16 C15 119.9(3) . . ? C17 C16 H16 120.1 . . ? C15 C16 H16 120.1 . . ? C16 C17 C18 120.5(3) . . ? C16 C17 H17 119.7 . . ? C18 C17 H17 119.7 . . ? C13 C18 C17 119.5(2) . . ? C13 C18 P3 117.29(18) . . ? C17 C18 P3 123.2(2) . . ? C21 C19 C20 110.6(3) . . ? C21 C19 P3 118.2(2) . . ? C20 C19 P3 109.41(19) . . ? C21 C19 H19 105.9 . . ? C20 C19 H19 105.9 . . ? P3 C19 H19 105.9 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C24 C22 C23 110.7(3) . . ? C24 C22 P3 112.1(2) . . ? C23 C22 P3 110.0(2) . . ? C24 C22 H22 108 . . ? C23 C22 H22 108 . . ? P3 C22 H22 108 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C27 C25 C26 118.1(3) . . ? C27 C25 Pd1 101.80(17) . . ? C26 C25 Pd1 118.73(19) . . ? C27 C25 H25 105.7 . . ? C26 C25 H25 105.7 . . ? Pd1 C25 H25 105.7 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? O3 C27 O2 118.9(3) . . ? O3 C27 C25 127.0(3) . . ? O2 C27 C25 114.0(3) . . ? O2 C28 H28A 109.5 . . ? O2 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? O2 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C30 C29 C34 119.0(4) . . ? C30 C29 C35 120.6(5) . . ? C34 C29 C35 120.4(5) . . ? C29 C30 C31 121.1(5) . . ? C29 C30 H30 119.5 . . ? C31 C30 H30 119.5 . . ? C32 C31 C30 118.3(5) . . ? C32 C31 H31 120.8 . . ? C30 C31 H31 120.8 . . ? C33 C32 C31 120.9(5) . . ? C33 C32 H32 119.5 . . ? C31 C32 H32 119.5 . . ? C34 C33 C32 120.3(5) . . ? C34 C33 H33 119.8 . . ? C32 C33 H33 119.8 . . ? C33 C34 C29 120.3(5) . . ? C33 C34 H34 119.8 . . ? C29 C34 H34 119.8 . . ? C29 C35 H35A 109.5 . . ? C29 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C29 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C27 O2 C28 117.4(3) . . ? O1 P1 C1 109.25(11) . . ? O1 P1 C13 108.34(11) . . ? C1 P1 C13 108.30(11) . . ? O1 P1 Pd1 115.65(7) . . ? C1 P1 Pd1 108.53(8) . . ? C13 P1 Pd1 106.52(8) . . ? C6 P2 C10 105.58(12) . . ? C6 P2 C7 102.18(12) . . ? C10 P2 C7 105.92(12) . . ? C6 P2 Pd1 106.68(8) . . ? C10 P2 Pd1 113.86(9) . . ? C7 P2 Pd1 121.02(9) . . ? C18 P3 C19 107.30(13) . . ? C18 P3 C22 104.19(13) . . ? C19 P3 C22 106.73(12) . . ? C18 P3 Pd1 106.96(8) . . ? C19 P3 Pd1 110.41(9) . . ? C22 P3 Pd1 120.46(10) . . ? C25 Pd1 P1 169.40(8) . . ? C25 Pd1 P3 92.97(7) . . ? P1 Pd1 P3 83.05(2) . . ? C25 Pd1 P2 102.02(7) . . ? P1 Pd1 P2 84.29(2) . . ? P3 Pd1 P2 159.98(2) . . ? #===END