# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2010 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Xu, Chen' _publ_contact_author_email xubohan@163.com _publ_section_title ; Design and synthesis of tetranuclear cluster monophosphine-cyclopalladated ferrocenylpyrimidinone complexes from the palladium-catalyzed hydroxylation of chloropyrimidine ; _publ_author_name 'Chen Xu' # Attachment 'Compound-3-.cif' data_a _database_code_depnum_ccdc_archive 'CCDC 779859' #TrackingRef 'Compound-3-.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C128 H100 Fe4 N8 O4 P4 Pd4' _chemical_formula_weight 2587.04 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M P4(2)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-y, x+1/2, z+1/2' 'y+1/2, -x, z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'y, -x-1/2, -z-1/2' '-y-1/2, x, -z-1/2' _cell_length_a 17.7245(9) _cell_length_b 17.7245(9) _cell_length_c 22.880(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7187.9(9) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 2701 _cell_measurement_theta_min 2.30 _cell_measurement_theta_max 16.30 _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.195 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2608 _exptl_absorpt_coefficient_mu 0.970 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8222 _exptl_absorpt_correction_T_max 0.9352 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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_reflns_number 54649 _diffrn_reflns_av_R_equivalents 0.1183 _diffrn_reflns_av_sigmaI/netI 0.0796 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.30 _diffrn_reflns_theta_max 25.50 _reflns_number_total 6696 _reflns_number_gt 3975 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0241P)^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 6696 _refine_ls_number_parameters 343 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0938 _refine_ls_R_factor_gt 0.0453 _refine_ls_wR_factor_ref 0.0898 _refine_ls_wR_factor_gt 0.0821 _refine_ls_goodness_of_fit_ref 1.071 _refine_ls_restrained_S_all 1.071 _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 Pd1 Pd 0.761235(18) 0.586718(18) 0.149622(14) 0.03984(11) Uani 1 1 d . . . Fe1 Fe 0.61315(4) 0.48650(4) 0.08524(3) 0.0526(2) Uani 1 1 d . . . P1 P 0.85922(7) 0.55868(7) 0.09201(5) 0.0450(3) Uani 1 1 d . . . O1 O 0.46569(17) 0.69761(19) 0.26332(13) 0.0642(10) Uani 1 1 d . . . N1 N 0.66325(19) 0.62565(18) 0.19322(15) 0.0398(9) Uani 1 1 d . . . N2 N 0.5920(2) 0.67665(18) 0.27207(14) 0.0416(9) Uani 1 1 d . . . C1 C 0.6120(2) 0.5989(2) 0.10004(18) 0.0426(11) Uani 1 1 d . . . C2 C 0.5614(3) 0.5803(2) 0.05383(19) 0.0513(12) Uani 1 1 d . . . H2 H 0.5070 0.5900 0.0528 0.062 Uiso 1 1 calc R . . C3 C 0.6046(3) 0.5470(3) 0.0098(2) 0.0582(14) Uani 1 1 d . . . H3 H 0.5850 0.5278 -0.0273 0.070 Uiso 1 1 calc R . . C4 C 0.6804(3) 0.5429(2) 0.02803(19) 0.0514(13) Uani 1 1 d . . . H4 H 0.7216 0.5203 0.0054 0.062 Uiso 1 1 calc R . . C5 C 0.6880(2) 0.5762(2) 0.08467(18) 0.0423(11) Uani 1 1 d . . . C6 C 0.5819(4) 0.4359(3) 0.1610(2) 0.0782(18) Uani 1 1 d . . . H6 H 0.5681 0.4616 0.1974 0.094 Uiso 1 1 calc R . . C7 C 0.5319(3) 0.4158(3) 0.1151(3) 0.0830(18) Uani 1 1 d . . . H7 H 0.4773 0.4250 0.1142 0.100 Uiso 1 1 calc R . . C8 C 0.5742(4) 0.3791(3) 0.0721(3) 0.0777(18) Uani 1 1 d . . . H8 H 0.5545 0.3591 0.0352 0.093 Uiso 1 1 calc R . . C9 C 0.6495(3) 0.3767(3) 0.0900(3) 0.0788(17) Uani 1 1 d . . . H9 H 0.6915 0.3548 0.0679 0.095 Uiso 1 1 calc R . . C10 C 0.6546(3) 0.4113(3) 0.1456(3) 0.0709(16) Uani 1 1 d . . . H10 H 0.7006 0.4174 0.1689 0.085 Uiso 1 1 calc R . . C11 C 0.5987(3) 0.6269(2) 0.15896(19) 0.0432(11) Uani 1 1 d . . . C12 C 0.5316(3) 0.6510(2) 0.1808(2) 0.0505(12) Uani 1 1 d . . . H12 H 0.4893 0.6510 0.1567 0.061 Uiso 1 1 calc R . . C13 C 0.5243(3) 0.6765(2) 0.2399(2) 0.0458(12) Uani 1 1 d . . . C14 C 0.6546(2) 0.6514(2) 0.24722(19) 0.0429(12) Uani 1 1 d . . . H14 H 0.6977 0.6517 0.2704 0.051 Uiso 1 1 calc R . . C15 C 0.8557(3) 0.4648(3) 0.0610(2) 0.0513(13) Uani 1 1 d . . . C16 C 0.8458(3) 0.4044(3) 0.0992(2) 0.0590(14) Uani 1 1 d . . . H16 H 0.8417 0.4136 0.1391 0.071 Uiso 1 1 calc R . . C17 C 0.8419(3) 0.3307(3) 0.0788(3) 0.0786(17) Uani 1 1 d . . . H17 H 0.8358 0.2908 0.1048 0.094 Uiso 1 1 calc R . . C18 C 0.8471(3) 0.3172(3) 0.0193(3) 0.0849(19) Uani 1 1 d . . . H18 H 0.8452 0.2680 0.0052 0.102 Uiso 1 1 calc R . . C19 C 0.8549(3) 0.3753(4) -0.0185(3) 0.0846(18) Uani 1 1 d . . . H19 H 0.8570 0.3657 -0.0585 0.101 Uiso 1 1 calc R . . C20 C 0.8599(3) 0.4494(3) 0.0016(2) 0.0622(14) Uani 1 1 d . . . H20 H 0.8660 0.4888 -0.0249 0.075 Uiso 1 1 calc R . . C21 C 0.8752(3) 0.6254(3) 0.03332(19) 0.0470(12) Uani 1 1 d . . . C22 C 0.8329(3) 0.6913(3) 0.0305(2) 0.0586(14) Uani 1 1 d . . . H22 H 0.7922 0.6980 0.0555 0.070 Uiso 1 1 calc R . . C23 C 0.8509(3) 0.7466(3) -0.0092(2) 0.0745(17) Uani 1 1 d . . . H23 H 0.8226 0.7908 -0.0104 0.089 Uiso 1 1 calc R . . C24 C 0.9107(3) 0.7375(3) -0.0474(2) 0.0771(17) Uani 1 1 d . . . H24 H 0.9217 0.7749 -0.0746 0.093 Uiso 1 1 calc R . . C25 C 0.9535(3) 0.6733(4) -0.0450(2) 0.0783(18) Uani 1 1 d . . . H25 H 0.9937 0.6671 -0.0706 0.094 Uiso 1 1 calc R . . C26 C 0.9372(3) 0.6181(3) -0.0047(2) 0.0704(16) Uani 1 1 d . . . H26 H 0.9676 0.5754 -0.0026 0.084 Uiso 1 1 calc R . . C27 C 0.9503(3) 0.5636(3) 0.12868(19) 0.0501(12) Uani 1 1 d . . . C28 C 0.9753(3) 0.6339(3) 0.1464(2) 0.0682(15) Uani 1 1 d . . . H28 H 0.9453 0.6759 0.1391 0.082 Uiso 1 1 calc R . . C29 C 1.0434(3) 0.6436(4) 0.1743(2) 0.0800(18) Uani 1 1 d . . . H29 H 1.0591 0.6913 0.1860 0.096 Uiso 1 1 calc R . . C30 C 1.0871(3) 0.5822(5) 0.1844(2) 0.0853(19) Uani 1 1 d . . . H30 H 1.1332 0.5881 0.2034 0.102 Uiso 1 1 calc R . . C31 C 1.0648(3) 0.5124(4) 0.1674(3) 0.096(2) Uani 1 1 d . . . H31 H 1.0958 0.4709 0.1743 0.115 Uiso 1 1 calc R . . C32 C 0.9953(3) 0.5027(3) 0.1394(2) 0.0767(17) Uani 1 1 d . . . H32 H 0.9798 0.4547 0.1281 0.092 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 Pd1 0.0414(2) 0.0397(2) 0.03837(19) -0.00607(18) -0.00175(18) 0.00090(18) Fe1 0.0564(5) 0.0487(4) 0.0526(4) -0.0057(4) -0.0115(4) -0.0043(4) P1 0.0463(8) 0.0412(7) 0.0474(8) -0.0055(6) 0.0014(6) 0.0059(6) O1 0.038(2) 0.090(3) 0.065(2) -0.013(2) 0.0072(17) 0.0102(19) N1 0.040(2) 0.039(2) 0.040(2) -0.0080(18) -0.0006(19) 0.0036(18) N2 0.042(2) 0.038(2) 0.044(2) -0.0026(18) 0.009(2) 0.0011(18) C1 0.043(3) 0.049(3) 0.035(3) -0.001(2) -0.010(2) 0.003(2) C2 0.052(3) 0.054(3) 0.048(3) -0.005(3) -0.006(3) 0.008(2) C3 0.061(4) 0.066(4) 0.047(3) -0.012(3) -0.012(3) -0.004(3) C4 0.059(3) 0.054(3) 0.042(3) -0.010(2) -0.003(3) 0.003(3) C5 0.048(3) 0.042(3) 0.036(3) -0.002(2) -0.002(2) 0.001(2) C6 0.105(5) 0.067(4) 0.063(4) 0.017(3) -0.011(4) -0.026(4) C7 0.068(4) 0.073(4) 0.108(5) 0.032(4) -0.011(4) -0.016(4) C8 0.099(5) 0.052(4) 0.082(5) -0.007(3) -0.026(4) -0.021(3) C9 0.078(4) 0.055(4) 0.103(5) -0.021(3) -0.024(4) 0.001(3) C10 0.062(4) 0.052(3) 0.098(5) 0.024(3) -0.027(4) -0.007(3) C11 0.046(3) 0.038(3) 0.046(3) 0.001(2) -0.002(2) 0.004(2) C12 0.045(3) 0.055(3) 0.052(3) -0.007(3) -0.013(3) 0.003(2) C13 0.045(3) 0.046(3) 0.046(3) -0.004(2) 0.000(3) 0.000(2) C14 0.045(3) 0.044(3) 0.039(3) -0.005(2) 0.001(2) -0.005(2) C15 0.054(3) 0.042(3) 0.058(3) -0.010(3) 0.001(3) 0.011(2) C16 0.066(4) 0.052(3) 0.060(3) -0.005(3) 0.006(3) 0.003(3) C17 0.089(4) 0.043(3) 0.103(5) -0.002(3) 0.011(4) 0.007(3) C18 0.094(5) 0.059(4) 0.102(5) -0.030(4) 0.010(4) -0.005(4) C19 0.110(5) 0.075(4) 0.069(4) -0.027(4) 0.008(4) 0.008(4) C20 0.076(4) 0.050(3) 0.061(4) -0.008(3) 0.010(3) 0.001(3) C21 0.048(3) 0.050(3) 0.043(3) -0.001(2) 0.009(2) 0.000(2) C22 0.056(3) 0.049(3) 0.071(4) 0.007(3) 0.013(3) 0.006(3) C23 0.079(4) 0.045(3) 0.100(5) 0.022(3) 0.019(4) 0.009(3) C24 0.074(4) 0.080(4) 0.078(4) 0.023(3) 0.018(4) -0.007(4) C25 0.066(4) 0.091(5) 0.077(4) 0.013(4) 0.032(3) 0.006(4) C26 0.065(4) 0.069(4) 0.077(4) 0.009(3) 0.019(3) 0.014(3) C27 0.050(3) 0.052(3) 0.049(3) -0.005(3) 0.005(2) 0.005(3) C28 0.054(3) 0.074(4) 0.076(4) -0.013(3) -0.011(3) 0.004(3) C29 0.069(4) 0.085(5) 0.085(4) -0.023(4) -0.004(4) -0.006(4) C30 0.058(4) 0.126(6) 0.072(4) -0.003(4) -0.014(3) -0.006(4) C31 0.063(4) 0.101(5) 0.124(6) 0.003(4) -0.023(4) 0.029(4) C32 0.060(4) 0.071(4) 0.099(5) -0.003(3) -0.016(3) 0.012(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 C5 1.982(4) . ? Pd1 N2 2.105(3) 8_756 ? Pd1 N1 2.118(3) . ? Pd1 P1 2.2362(12) . ? Fe1 C1 2.021(4) . ? Fe1 C7 2.028(5) . ? Fe1 C6 2.029(5) . ? Fe1 C2 2.030(4) . ? Fe1 C4 2.033(5) . ? Fe1 C3 2.037(5) . ? Fe1 C8 2.047(5) . ? Fe1 C9 2.053(5) . ? Fe1 C10 2.055(5) . ? Fe1 C5 2.071(4) . ? P1 C15 1.810(4) . ? P1 C21 1.812(4) . ? P1 C27 1.821(5) . ? O1 C13 1.228(5) . ? N1 C14 1.326(5) . ? N1 C11 1.387(5) . ? N2 C14 1.325(5) . ? N2 C13 1.407(5) . ? N2 Pd1 2.105(3) 7_576 ? C1 C2 1.425(5) . ? C1 C5 1.448(5) . ? C1 C11 1.456(5) . ? C2 C3 1.396(6) . ? C2 H2 0.9800 . ? C3 C4 1.409(6) . ? C3 H3 0.9800 . ? C4 C5 1.431(5) . ? C4 H4 0.9800 . ? C6 C10 1.405(7) . ? C6 C7 1.420(7) . ? C6 H6 0.9800 . ? C7 C8 1.399(7) . ? C7 H7 0.9800 . ? C8 C9 1.396(7) . ? C8 H8 0.9800 . ? C9 C10 1.414(7) . ? C9 H9 0.9800 . ? C10 H10 0.9800 . ? C11 C12 1.359(5) . ? C12 C13 1.433(6) . ? C12 H12 0.9300 . ? C14 H14 0.9300 . ? C15 C20 1.387(6) . ? C15 C16 1.393(6) . ? C16 C17 1.389(6) . ? C16 H16 0.9300 . ? C17 C18 1.386(7) . ? C17 H17 0.9300 . ? C18 C19 1.351(7) . ? C18 H18 0.9300 . ? C19 C20 1.396(6) . ? C19 H19 0.9300 . ? C20 H20 0.9300 . ? C21 C22 1.389(6) . ? C21 C26 1.408(6) . ? C22 C23 1.374(6) . ? C22 H22 0.9300 . ? C23 C24 1.383(6) . ? C23 H23 0.9300 . ? C24 C25 1.368(7) . ? C24 H24 0.9300 . ? C25 C26 1.374(6) . ? C25 H25 0.9300 . ? C26 H26 0.9300 . ? C27 C32 1.365(6) . ? C27 C28 1.384(6) . ? C28 C29 1.377(6) . ? C28 H28 0.9300 . ? C29 C30 1.356(7) . ? C29 H29 0.9300 . ? C30 C31 1.356(7) . ? C30 H30 0.9300 . ? C31 C32 1.399(7) . ? C31 H31 0.9300 . ? C32 H32 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C5 Pd1 N2 170.06(15) . 8_756 ? C5 Pd1 N1 81.18(15) . . ? N2 Pd1 N1 90.77(13) 8_756 . ? C5 Pd1 P1 92.63(13) . . ? N2 Pd1 P1 96.05(9) 8_756 . ? N1 Pd1 P1 170.64(10) . . ? C1 Fe1 C7 123.1(2) . . ? C1 Fe1 C6 106.9(2) . . ? C7 Fe1 C6 41.0(2) . . ? C1 Fe1 C2 41.20(15) . . ? C7 Fe1 C2 107.7(2) . . ? C6 Fe1 C2 122.8(2) . . ? C1 Fe1 C4 68.24(17) . . ? C7 Fe1 C4 159.6(2) . . ? C6 Fe1 C4 158.0(2) . . ? C2 Fe1 C4 68.58(18) . . ? C1 Fe1 C3 67.80(17) . . ? C7 Fe1 C3 123.9(2) . . ? C6 Fe1 C3 159.4(2) . . ? C2 Fe1 C3 40.14(16) . . ? C4 Fe1 C3 40.50(16) . . ? C1 Fe1 C8 159.7(2) . . ? C7 Fe1 C8 40.2(2) . . ? C6 Fe1 C8 67.8(2) . . ? C2 Fe1 C8 123.9(2) . . ? C4 Fe1 C8 124.0(2) . . ? C3 Fe1 C8 109.9(2) . . ? C1 Fe1 C9 158.2(2) . . ? C7 Fe1 C9 67.6(2) . . ? C6 Fe1 C9 67.7(2) . . ? C2 Fe1 C9 159.5(2) . . ? C4 Fe1 C9 108.4(2) . . ? C3 Fe1 C9 124.6(2) . . ? C8 Fe1 C9 39.82(19) . . ? C1 Fe1 C10 122.0(2) . . ? C7 Fe1 C10 68.1(2) . . ? C6 Fe1 C10 40.2(2) . . ? C2 Fe1 C10 158.5(2) . . ? C4 Fe1 C10 122.8(2) . . ? C3 Fe1 C10 159.6(2) . . ? C8 Fe1 C10 67.4(2) . . ? C9 Fe1 C10 40.27(19) . . ? C1 Fe1 C5 41.43(15) . . ? C7 Fe1 C5 158.7(2) . . ? C6 Fe1 C5 121.3(2) . . ? C2 Fe1 C5 70.02(17) . . ? C4 Fe1 C5 40.79(15) . . ? C3 Fe1 C5 68.77(17) . . ? C8 Fe1 C5 158.3(2) . . ? C9 Fe1 C5 121.8(2) . . ? C10 Fe1 C5 105.86(19) . . ? C15 P1 C21 108.3(2) . . ? C15 P1 C27 104.7(2) . . ? C21 P1 C27 99.9(2) . . ? C15 P1 Pd1 114.15(16) . . ? C21 P1 Pd1 114.43(16) . . ? C27 P1 Pd1 113.96(15) . . ? C14 N1 C11 115.2(4) . . ? C14 N1 Pd1 130.2(3) . . ? C11 N1 Pd1 114.5(3) . . ? C14 N2 C13 119.3(4) . . ? C14 N2 Pd1 125.4(3) . 7_576 ? C13 N2 Pd1 114.1(3) . 7_576 ? C2 C1 C5 110.0(4) . . ? C2 C1 C11 131.6(4) . . ? C5 C1 C11 118.0(4) . . ? C2 C1 Fe1 69.8(2) . . ? C5 C1 Fe1 71.2(2) . . ? C11 C1 Fe1 119.5(3) . . ? C3 C2 C1 106.7(4) . . ? C3 C2 Fe1 70.2(3) . . ? C1 C2 Fe1 69.0(2) . . ? C3 C2 H2 126.7 . . ? C1 C2 H2 126.7 . . ? Fe1 C2 H2 126.7 . . ? C2 C3 C4 109.4(4) . . ? C2 C3 Fe1 69.7(3) . . ? C4 C3 Fe1 69.6(3) . . ? C2 C3 H3 125.3 . . ? C4 C3 H3 125.3 . . ? Fe1 C3 H3 125.3 . . ? C3 C4 C5 109.6(4) . . ? C3 C4 Fe1 69.9(3) . . ? C5 C4 Fe1 71.0(3) . . ? C3 C4 H4 125.2 . . ? C5 C4 H4 125.2 . . ? Fe1 C4 H4 125.2 . . ? C4 C5 C1 104.3(4) . . ? C4 C5 Pd1 141.2(3) . . ? C1 C5 Pd1 113.6(3) . . ? C4 C5 Fe1 68.2(2) . . ? C1 C5 Fe1 67.4(2) . . ? Pd1 C5 Fe1 119.1(2) . . ? C10 C6 C7 108.0(5) . . ? C10 C6 Fe1 70.9(3) . . ? C7 C6 Fe1 69.5(3) . . ? C10 C6 H6 126.0 . . ? C7 C6 H6 126.0 . . ? Fe1 C6 H6 126.0 . . ? C8 C7 C6 107.5(5) . . ? C8 C7 Fe1 70.6(3) . . ? C6 C7 Fe1 69.6(3) . . ? C8 C7 H7 126.2 . . ? C6 C7 H7 126.2 . . ? Fe1 C7 H7 126.2 . . ? C9 C8 C7 108.6(5) . . ? C9 C8 Fe1 70.3(3) . . ? C7 C8 Fe1 69.2(3) . . ? C9 C8 H8 125.7 . . ? C7 C8 H8 125.7 . . ? Fe1 C8 H8 125.7 . . ? C8 C9 C10 108.2(5) . . ? C8 C9 Fe1 69.9(3) . . ? C10 C9 Fe1 70.0(3) . . ? C8 C9 H9 125.9 . . ? C10 C9 H9 125.9 . . ? Fe1 C9 H9 125.9 . . ? C6 C10 C9 107.5(5) . . ? C6 C10 Fe1 68.9(3) . . ? C9 C10 Fe1 69.8(3) . . ? C6 C10 H10 126.2 . . ? C9 C10 H10 126.2 . . ? Fe1 C10 H10 126.2 . . ? C12 C11 N1 121.3(4) . . ? C12 C11 C1 126.1(4) . . ? N1 C11 C1 112.6(4) . . ? C11 C12 C13 121.6(4) . . ? C11 C12 H12 119.2 . . ? C13 C12 H12 119.2 . . ? O1 C13 N2 119.6(4) . . ? O1 C13 C12 125.7(4) . . ? N2 C13 C12 114.7(4) . . ? N2 C14 N1 127.8(4) . . ? N2 C14 H14 116.1 . . ? N1 C14 H14 116.1 . . ? C20 C15 C16 118.0(4) . . ? C20 C15 P1 124.3(4) . . ? C16 C15 P1 117.7(4) . . ? C17 C16 C15 121.3(5) . . ? C17 C16 H16 119.3 . . ? C15 C16 H16 119.3 . . ? C18 C17 C16 119.2(5) . . ? C18 C17 H17 120.4 . . ? C16 C17 H17 120.4 . . ? C19 C18 C17 120.3(5) . . ? C19 C18 H18 119.8 . . ? C17 C18 H18 119.8 . . ? C18 C19 C20 120.8(5) . . ? C18 C19 H19 119.6 . . ? C20 C19 H19 119.6 . . ? C15 C20 C19 120.4(5) . . ? C15 C20 H20 119.8 . . ? C19 C20 H20 119.8 . . ? C22 C21 C26 117.9(4) . . ? C22 C21 P1 119.9(4) . . ? C26 C21 P1 121.4(4) . . ? C23 C22 C21 120.4(5) . . ? C23 C22 H22 119.8 . . ? C21 C22 H22 119.8 . . ? C22 C23 C24 120.8(5) . . ? C22 C23 H23 119.6 . . ? C24 C23 H23 119.6 . . ? C25 C24 C23 119.7(5) . . ? C25 C24 H24 120.1 . . ? C23 C24 H24 120.1 . . ? C24 C25 C26 120.2(5) . . ? C24 C25 H25 119.9 . . ? C26 C25 H25 119.9 . . ? C25 C26 C21 120.9(5) . . ? C25 C26 H26 119.6 . . ? C21 C26 H26 119.6 . . ? C32 C27 C28 118.2(5) . . ? C32 C27 P1 124.3(4) . . ? C28 C27 P1 117.5(4) . . ? C29 C28 C27 121.9(5) . . ? C29 C28 H28 119.0 . . ? C27 C28 H28 119.0 . . ? C30 C29 C28 118.7(6) . . ? C30 C29 H29 120.6 . . ? C28 C29 H29 120.6 . . ? C29 C30 C31 121.1(6) . . ? C29 C30 H30 119.4 . . ? C31 C30 H30 119.4 . . ? C30 C31 C32 120.0(6) . . ? C30 C31 H31 120.0 . . ? C32 C31 H31 120.0 . . ? C27 C32 C31 120.0(5) . . ? C27 C32 H32 120.0 . . ? C31 C32 H32 120.0 . . ? 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 C5 Pd1 P1 C15 -62.5(2) . . . . ? N2 Pd1 P1 C15 112.7(2) 8_756 . . . ? N1 Pd1 P1 C15 -110.8(6) . . . . ? C5 Pd1 P1 C21 63.1(2) . . . . ? N2 Pd1 P1 C21 -121.73(19) 8_756 . . . ? N1 Pd1 P1 C21 14.8(6) . . . . ? C5 Pd1 P1 C27 177.2(2) . . . . ? N2 Pd1 P1 C27 -7.6(2) 8_756 . . . ? N1 Pd1 P1 C27 128.9(6) . . . . ? C5 Pd1 N1 C14 -178.2(4) . . . . ? N2 Pd1 N1 C14 7.7(4) 8_756 . . . ? P1 Pd1 N1 C14 -129.2(5) . . . . ? C5 Pd1 N1 C11 -0.8(3) . . . . ? N2 Pd1 N1 C11 -175.0(3) 8_756 . . . ? P1 Pd1 N1 C11 48.2(7) . . . . ? C7 Fe1 C1 C2 -78.9(3) . . . . ? C6 Fe1 C1 C2 -120.8(3) . . . . ? C4 Fe1 C1 C2 81.9(3) . . . . ? C3 Fe1 C1 C2 38.1(3) . . . . ? C8 Fe1 C1 C2 -49.4(7) . . . . ? C9 Fe1 C1 C2 167.2(5) . . . . ? C10 Fe1 C1 C2 -162.1(3) . . . . ? C5 Fe1 C1 C2 120.7(4) . . . . ? C7 Fe1 C1 C5 160.4(3) . . . . ? C6 Fe1 C1 C5 118.5(3) . . . . ? C2 Fe1 C1 C5 -120.7(4) . . . . ? C4 Fe1 C1 C5 -38.8(2) . . . . ? C3 Fe1 C1 C5 -82.6(3) . . . . ? C8 Fe1 C1 C5 -170.0(5) . . . . ? C9 Fe1 C1 C5 46.6(6) . . . . ? C10 Fe1 C1 C5 77.2(3) . . . . ? C7 Fe1 C1 C11 48.2(4) . . . . ? C6 Fe1 C1 C11 6.3(4) . . . . ? C2 Fe1 C1 C11 127.1(5) . . . . ? C4 Fe1 C1 C11 -151.0(4) . . . . ? C3 Fe1 C1 C11 165.2(4) . . . . ? C8 Fe1 C1 C11 77.8(7) . . . . ? C9 Fe1 C1 C11 -65.6(7) . . . . ? C10 Fe1 C1 C11 -35.0(4) . . . . ? C5 Fe1 C1 C11 -112.2(4) . . . . ? C5 C1 C2 C3 -0.4(5) . . . . ? C11 C1 C2 C3 -172.4(5) . . . . ? Fe1 C1 C2 C3 -60.4(3) . . . . ? C5 C1 C2 Fe1 60.0(3) . . . . ? C11 C1 C2 Fe1 -112.0(5) . . . . ? C1 Fe1 C2 C3 117.7(4) . . . . ? C7 Fe1 C2 C3 -122.0(3) . . . . ? C6 Fe1 C2 C3 -164.5(3) . . . . ? C4 Fe1 C2 C3 36.7(3) . . . . ? C8 Fe1 C2 C3 -80.8(4) . . . . ? C9 Fe1 C2 C3 -48.7(7) . . . . ? C10 Fe1 C2 C3 163.0(5) . . . . ? C5 Fe1 C2 C3 80.4(3) . . . . ? C7 Fe1 C2 C1 120.3(3) . . . . ? C6 Fe1 C2 C1 77.8(3) . . . . ? C4 Fe1 C2 C1 -81.0(3) . . . . ? C3 Fe1 C2 C1 -117.7(4) . . . . ? C8 Fe1 C2 C1 161.5(3) . . . . ? C9 Fe1 C2 C1 -166.4(6) . . . . ? C10 Fe1 C2 C1 45.3(6) . . . . ? C5 Fe1 C2 C1 -37.3(2) . . . . ? C1 C2 C3 C4 1.3(5) . . . . ? Fe1 C2 C3 C4 -58.3(3) . . . . ? C1 C2 C3 Fe1 59.7(3) . . . . ? C1 Fe1 C3 C2 -39.1(3) . . . . ? C7 Fe1 C3 C2 76.8(4) . . . . ? C6 Fe1 C3 C2 39.7(7) . . . . ? C4 Fe1 C3 C2 -121.1(4) . . . . ? C8 Fe1 C3 C2 119.4(3) . . . . ? C9 Fe1 C3 C2 161.4(3) . . . . ? C10 Fe1 C3 C2 -162.1(5) . . . . ? C5 Fe1 C3 C2 -83.8(3) . . . . ? C1 Fe1 C3 C4 82.0(3) . . . . ? C7 Fe1 C3 C4 -162.2(3) . . . . ? C6 Fe1 C3 C4 160.7(5) . . . . ? C2 Fe1 C3 C4 121.1(4) . . . . ? C8 Fe1 C3 C4 -119.6(3) . . . . ? C9 Fe1 C3 C4 -77.5(3) . . . . ? C10 Fe1 C3 C4 -41.0(7) . . . . ? C5 Fe1 C3 C4 37.3(2) . . . . ? C2 C3 C4 C5 -1.8(5) . . . . ? Fe1 C3 C4 C5 -60.2(3) . . . . ? C2 C3 C4 Fe1 58.4(3) . . . . ? C1 Fe1 C4 C3 -80.8(3) . . . . ? C7 Fe1 C4 C3 46.9(7) . . . . ? C6 Fe1 C4 C3 -162.0(5) . . . . ? C2 Fe1 C4 C3 -36.4(3) . . . . ? C8 Fe1 C4 C3 80.8(4) . . . . ? C9 Fe1 C4 C3 122.1(3) . . . . ? C10 Fe1 C4 C3 164.2(3) . . . . ? C5 Fe1 C4 C3 -120.2(4) . . . . ? C1 Fe1 C4 C5 39.4(2) . . . . ? C7 Fe1 C4 C5 167.1(6) . . . . ? C6 Fe1 C4 C5 -41.8(7) . . . . ? C2 Fe1 C4 C5 83.8(3) . . . . ? C3 Fe1 C4 C5 120.2(4) . . . . ? C8 Fe1 C4 C5 -158.9(3) . . . . ? C9 Fe1 C4 C5 -117.7(3) . . . . ? C10 Fe1 C4 C5 -75.6(3) . . . . ? C3 C4 C5 C1 1.5(5) . . . . ? Fe1 C4 C5 C1 -58.0(3) . . . . ? C3 C4 C5 Pd1 169.3(4) . . . . ? Fe1 C4 C5 Pd1 109.8(5) . . . . ? C3 C4 C5 Fe1 59.5(3) . . . . ? C2 C1 C5 C4 -0.6(5) . . . . ? C11 C1 C5 C4 172.6(4) . . . . ? Fe1 C1 C5 C4 58.5(3) . . . . ? C2 C1 C5 Pd1 -172.3(3) . . . . ? C11 C1 C5 Pd1 0.9(5) . . . . ? Fe1 C1 C5 Pd1 -113.2(2) . . . . ? C2 C1 C5 Fe1 -59.2(3) . . . . ? C11 C1 C5 Fe1 114.1(4) . . . . ? N2 Pd1 C5 C4 -130.9(8) 8_756 . . . ? N1 Pd1 C5 C4 -167.1(5) . . . . ? P1 Pd1 C5 C4 19.9(5) . . . . ? N2 Pd1 C5 C1 36.2(11) 8_756 . . . ? N1 Pd1 C5 C1 0.0(3) . . . . ? P1 Pd1 C5 C1 -173.0(3) . . . . ? N2 Pd1 C5 Fe1 -40.1(10) 8_756 . . . ? N1 Pd1 C5 Fe1 -76.4(2) . . . . ? P1 Pd1 C5 Fe1 110.7(2) . . . . ? C1 Fe1 C5 C4 -117.1(4) . . . . ? C7 Fe1 C5 C4 -167.6(5) . . . . ? C6 Fe1 C5 C4 163.0(3) . . . . ? C2 Fe1 C5 C4 -80.0(3) . . . . ? C3 Fe1 C5 C4 -37.0(3) . . . . ? C8 Fe1 C5 C4 53.6(6) . . . . ? C9 Fe1 C5 C4 81.4(3) . . . . ? C10 Fe1 C5 C4 122.2(3) . . . . ? C7 Fe1 C5 C1 -50.6(6) . . . . ? C6 Fe1 C5 C1 -79.9(3) . . . . ? C2 Fe1 C5 C1 37.1(2) . . . . ? C4 Fe1 C5 C1 117.1(4) . . . . ? C3 Fe1 C5 C1 80.1(3) . . . . ? C8 Fe1 C5 C1 170.7(5) . . . . ? C9 Fe1 C5 C1 -161.5(3) . . . . ? C10 Fe1 C5 C1 -120.7(3) . . . . ? C1 Fe1 C5 Pd1 105.4(3) . . . . ? C7 Fe1 C5 Pd1 54.8(6) . . . . ? C6 Fe1 C5 Pd1 25.5(4) . . . . ? C2 Fe1 C5 Pd1 142.4(3) . . . . ? C4 Fe1 C5 Pd1 -137.5(4) . . . . ? C3 Fe1 C5 Pd1 -174.6(3) . . . . ? C8 Fe1 C5 Pd1 -84.0(6) . . . . ? C9 Fe1 C5 Pd1 -56.2(3) . . . . ? C10 Fe1 C5 Pd1 -15.4(3) . . . . ? C1 Fe1 C6 C10 -120.0(3) . . . . ? C7 Fe1 C6 C10 118.7(5) . . . . ? C2 Fe1 C6 C10 -162.3(3) . . . . ? C4 Fe1 C6 C10 -46.5(7) . . . . ? C3 Fe1 C6 C10 168.4(5) . . . . ? C8 Fe1 C6 C10 80.8(4) . . . . ? C9 Fe1 C6 C10 37.6(3) . . . . ? C5 Fe1 C6 C10 -77.1(4) . . . . ? C1 Fe1 C6 C7 121.3(4) . . . . ? C2 Fe1 C6 C7 79.1(4) . . . . ? C4 Fe1 C6 C7 -165.1(5) . . . . ? C3 Fe1 C6 C7 49.8(7) . . . . ? C8 Fe1 C6 C7 -37.9(3) . . . . ? C9 Fe1 C6 C7 -81.1(4) . . . . ? C10 Fe1 C6 C7 -118.7(5) . . . . ? C5 Fe1 C6 C7 164.2(3) . . . . ? C10 C6 C7 C8 0.1(6) . . . . ? Fe1 C6 C7 C8 60.7(4) . . . . ? C10 C6 C7 Fe1 -60.7(4) . . . . ? C1 Fe1 C7 C8 164.6(3) . . . . ? C6 Fe1 C7 C8 -118.2(5) . . . . ? C2 Fe1 C7 C8 121.9(3) . . . . ? C4 Fe1 C7 C8 45.9(8) . . . . ? C3 Fe1 C7 C8 80.7(4) . . . . ? C9 Fe1 C7 C8 -36.9(3) . . . . ? C10 Fe1 C7 C8 -80.5(4) . . . . ? C5 Fe1 C7 C8 -157.8(5) . . . . ? C1 Fe1 C7 C6 -77.2(4) . . . . ? C2 Fe1 C7 C6 -119.9(4) . . . . ? C4 Fe1 C7 C6 164.0(5) . . . . ? C3 Fe1 C7 C6 -161.2(3) . . . . ? C8 Fe1 C7 C6 118.2(5) . . . . ? C9 Fe1 C7 C6 81.3(4) . . . . ? C10 Fe1 C7 C6 37.6(3) . . . . ? C5 Fe1 C7 C6 -39.6(7) . . . . ? C6 C7 C8 C9 -0.6(6) . . . . ? Fe1 C7 C8 C9 59.4(4) . . . . ? C6 C7 C8 Fe1 -60.1(4) . . . . ? C1 Fe1 C8 C9 -159.8(5) . . . . ? C7 Fe1 C8 C9 -119.9(5) . . . . ? C6 Fe1 C8 C9 -81.3(4) . . . . ? C2 Fe1 C8 C9 163.2(3) . . . . ? C4 Fe1 C8 C9 77.6(4) . . . . ? C3 Fe1 C8 C9 120.6(4) . . . . ? C10 Fe1 C8 C9 -37.6(3) . . . . ? C5 Fe1 C8 C9 38.2(7) . . . . ? C1 Fe1 C8 C7 -39.9(7) . . . . ? C6 Fe1 C8 C7 38.6(3) . . . . ? C2 Fe1 C8 C7 -76.9(4) . . . . ? C4 Fe1 C8 C7 -162.4(3) . . . . ? C3 Fe1 C8 C7 -119.5(4) . . . . ? C9 Fe1 C8 C7 119.9(5) . . . . ? C10 Fe1 C8 C7 82.3(4) . . . . ? C5 Fe1 C8 C7 158.2(5) . . . . ? C7 C8 C9 C10 0.9(6) . . . . ? Fe1 C8 C9 C10 59.7(4) . . . . ? C7 C8 C9 Fe1 -58.7(4) . . . . ? C1 Fe1 C9 C8 161.2(5) . . . . ? C7 Fe1 C9 C8 37.2(3) . . . . ? C6 Fe1 C9 C8 81.7(4) . . . . ? C2 Fe1 C9 C8 -43.4(8) . . . . ? C4 Fe1 C9 C8 -121.4(4) . . . . ? C3 Fe1 C9 C8 -79.5(4) . . . . ? C10 Fe1 C9 C8 119.2(5) . . . . ? C5 Fe1 C9 C8 -164.4(3) . . . . ? C1 Fe1 C9 C10 41.9(7) . . . . ? C7 Fe1 C9 C10 -82.1(4) . . . . ? C6 Fe1 C9 C10 -37.6(3) . . . . ? C2 Fe1 C9 C10 -162.7(5) . . . . ? C4 Fe1 C9 C10 119.3(3) . . . . ? C3 Fe1 C9 C10 161.3(3) . . . . ? C8 Fe1 C9 C10 -119.2(5) . . . . ? C5 Fe1 C9 C10 76.4(4) . . . . ? C7 C6 C10 C9 0.5(6) . . . . ? Fe1 C6 C10 C9 -59.3(4) . . . . ? C7 C6 C10 Fe1 59.8(4) . . . . ? C8 C9 C10 C6 -0.8(6) . . . . ? Fe1 C9 C10 C6 58.8(3) . . . . ? C8 C9 C10 Fe1 -59.6(4) . . . . ? C1 Fe1 C10 C6 77.9(4) . . . . ? C7 Fe1 C10 C6 -38.3(3) . . . . ? C2 Fe1 C10 C6 44.4(7) . . . . ? C4 Fe1 C10 C6 161.2(3) . . . . ? C3 Fe1 C10 C6 -168.4(5) . . . . ? C8 Fe1 C10 C6 -81.9(4) . . . . ? C9 Fe1 C10 C6 -119.1(5) . . . . ? C5 Fe1 C10 C6 120.0(3) . . . . ? C1 Fe1 C10 C9 -163.0(3) . . . . ? C7 Fe1 C10 C9 80.8(4) . . . . ? C6 Fe1 C10 C9 119.1(5) . . . . ? C2 Fe1 C10 C9 163.5(5) . . . . ? C4 Fe1 C10 C9 -79.7(4) . . . . ? C3 Fe1 C10 C9 -49.3(7) . . . . ? C8 Fe1 C10 C9 37.2(3) . . . . ? C5 Fe1 C10 C9 -120.9(3) . . . . ? C14 N1 C11 C12 -1.7(6) . . . . ? Pd1 N1 C11 C12 -179.5(3) . . . . ? C14 N1 C11 C1 179.3(4) . . . . ? Pd1 N1 C11 C1 1.5(4) . . . . ? C2 C1 C11 C12 -9.0(8) . . . . ? C5 C1 C11 C12 179.5(4) . . . . ? Fe1 C1 C11 C12 -97.4(5) . . . . ? C2 C1 C11 N1 169.9(4) . . . . ? C5 C1 C11 N1 -1.6(6) . . . . ? Fe1 C1 C11 N1 81.6(4) . . . . ? N1 C11 C12 C13 0.2(7) . . . . ? C1 C11 C12 C13 179.0(4) . . . . ? C14 N2 C13 O1 177.7(4) . . . . ? Pd1 N2 C13 O1 -14.3(5) 7_576 . . . ? C14 N2 C13 C12 -2.7(6) . . . . ? Pd1 N2 C13 C12 165.3(3) 7_576 . . . ? C11 C12 C13 O1 -178.4(4) . . . . ? C11 C12 C13 N2 2.0(6) . . . . ? C13 N2 C14 N1 1.2(6) . . . . ? Pd1 N2 C14 N1 -165.3(3) 7_576 . . . ? C11 N1 C14 N2 1.1(6) . . . . ? Pd1 N1 C14 N2 178.4(3) . . . . ? C21 P1 C15 C20 -3.9(5) . . . . ? C27 P1 C15 C20 -109.8(4) . . . . ? Pd1 P1 C15 C20 124.9(4) . . . . ? C21 P1 C15 C16 178.3(4) . . . . ? C27 P1 C15 C16 72.4(4) . . . . ? Pd1 P1 C15 C16 -52.9(4) . . . . ? C20 C15 C16 C17 1.5(7) . . . . ? P1 C15 C16 C17 179.4(4) . . . . ? C15 C16 C17 C18 -0.8(8) . . . . ? C16 C17 C18 C19 -0.9(9) . . . . ? C17 C18 C19 C20 1.7(9) . . . . ? C16 C15 C20 C19 -0.7(7) . . . . ? P1 C15 C20 C19 -178.4(4) . . . . ? C18 C19 C20 C15 -0.9(8) . . . . ? C15 P1 C21 C22 134.7(4) . . . . ? C27 P1 C21 C22 -116.0(4) . . . . ? Pd1 P1 C21 C22 6.1(4) . . . . ? C15 P1 C21 C26 -55.1(4) . . . . ? C27 P1 C21 C26 54.2(4) . . . . ? Pd1 P1 C21 C26 176.3(3) . . . . ? C26 C21 C22 C23 1.1(7) . . . . ? P1 C21 C22 C23 171.6(4) . . . . ? C21 C22 C23 C24 0.8(8) . . . . ? C22 C23 C24 C25 -1.4(9) . . . . ? C23 C24 C25 C26 0.0(9) . . . . ? C24 C25 C26 C21 2.0(8) . . . . ? C22 C21 C26 C25 -2.5(7) . . . . ? P1 C21 C26 C25 -172.9(4) . . . . ? C15 P1 C27 C32 -12.4(5) . . . . ? C21 P1 C27 C32 -124.5(4) . . . . ? Pd1 P1 C27 C32 113.0(4) . . . . ? C15 P1 C27 C28 167.1(4) . . . . ? C21 P1 C27 C28 55.0(4) . . . . ? Pd1 P1 C27 C28 -67.5(4) . . . . ? C32 C27 C28 C29 -0.4(8) . . . . ? P1 C27 C28 C29 -179.9(4) . . . . ? C27 C28 C29 C30 0.4(8) . . . . ? C28 C29 C30 C31 0.2(9) . . . . ? C29 C30 C31 C32 -0.7(10) . . . . ? C28 C27 C32 C31 -0.2(8) . . . . ? P1 C27 C32 C31 179.3(4) . . . . ? C30 C31 C32 C27 0.7(9) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.369 _refine_diff_density_min -0.355 _refine_diff_density_rms 0.074 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.105 0.203 0.250 1270 205 ' ' 2 -0.229 0.019 0.750 1270 205 ' ' 3 0.250 0.250 0.844 10 2 ' ' 4 0.250 0.250 0.655 10 1 ' ' 5 0.750 0.750 0.156 10 1 ' ' 6 0.750 0.750 0.344 10 2 ' ' _platon_squeeze_details ; ;