Supplementary Material (ESI) for Journal of Materials Chemistry This journal is © The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 1145 loop_ _publ_author_name 'Yun Chi' 'Yao-Lun Chen' 'Yi-Ching Cheng' 'Gene-Hsiang Lee' 'Yan-Hsiu Liu' 'Chao-Shiuan Liu' 'Shie-Ming Peng' 'Yung-Liang Tung' _publ_contact_author_name 'Prof Yun Chi' _publ_contact_author_address ; Department of Chemistry National Tsing Hua University No 101, Kung Fu Road Sec. 2 Hsin Chu 30013 TAJIKISTAN ; _publ_contact_author_email 'YCHI@MX.NTHU.EDU.TW' _publ_requested_journal 'Journal of Materials Chemistry' _publ_section_title ; Synthesis and Characterization of Fluorinated b-Ketoiminate and Imino-Alcoholate Pd Complexes: Precursors for Palladium Chemical Vapor Deposition ; data_ic8148 _database_code_CSD 192599 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H16 F12 N2 O4 Pd' _chemical_formula_weight 634.71 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' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pd' 'Pd' -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.7507(2) _cell_length_b 9.4424(2) _cell_length_c 13.7058(2) _cell_angle_alpha 74.0139(9) _cell_angle_beta 86.8875(10) _cell_angle_gamma 81.3120(10) _cell_volume 1076.09(4) _cell_formula_units_Z 2 _cell_measurement_temperature 150(1) _cell_measurement_reflns_used all _cell_measurement_theta_min 2.27 _cell_measurement_theta_max 27.50 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas not_measured _exptl_crystal_density_diffrn 1.959 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 624 _exptl_absorpt_coefficient_mu 0.993 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.833 _exptl_absorpt_correction_T_max 0.906 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(1) _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 'NONIUS KappaCCD' _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_% 0 _diffrn_reflns_number 26095 _diffrn_reflns_av_R_equivalents 0.0498 _diffrn_reflns_av_sigmaI/netI 0.0362 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.27 _diffrn_reflns_theta_max 27.50 _reflns_number_total 4952 _reflns_number_gt 4371 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'NONIUS COLLECT' _computing_cell_refinement DENZO-SMN _computing_data_reduction DENZO-SMN _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material 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^)+(0.0527P)^2^+0.1716P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0177(13) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 4952 _refine_ls_number_parameters 344 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0428 _refine_ls_R_factor_gt 0.0323 _refine_ls_wR_factor_ref 0.0859 _refine_ls_wR_factor_gt 0.0792 _refine_ls_goodness_of_fit_ref 1.087 _refine_ls_restrained_S_all 1.087 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd Pd 0.44844(2) 0.471652(19) 0.199105(13) 0.02297(9) Uani 1 1 d . . . O1 O 0.6092(2) 0.5884(2) 0.12661(14) 0.0305(4) Uani 1 1 d . . . O2 O 0.2787(2) 0.36010(19) 0.26576(14) 0.0291(4) Uani 1 1 d . . . O3 O 0.7012(2) 0.0660(2) 0.33489(15) 0.0384(5) Uani 1 1 d . . . O4 O 0.5345(3) 0.6844(2) 0.41019(16) 0.0439(5) Uani 1 1 d . . . N1 N 0.5487(2) 0.2850(2) 0.15908(16) 0.0243(4) Uani 1 1 d . . . N2 N 0.3518(2) 0.6575(2) 0.24066(15) 0.0240(4) Uani 1 1 d . . . C1 C 0.8044(3) 0.6656(3) 0.0127(2) 0.0309(6) Uani 1 1 d . . . C2 C 0.7035(3) 0.5459(3) 0.06197(19) 0.0266(5) Uani 1 1 d . . . C3 C 0.7262(3) 0.4147(3) 0.03714(19) 0.0277(5) Uani 1 1 d . . . H3A H 0.7934 0.4069 -0.0186 0.033 Uiso 1 1 calc R . . C4 C 0.6557(3) 0.2878(3) 0.08930(19) 0.0251(5) Uani 1 1 d . . . C5 C 0.7190(3) 0.1462(3) 0.0562(2) 0.0306(5) Uani 1 1 d . . . C6 C 0.0260(3) 0.3203(3) 0.3200(2) 0.0347(6) Uani 1 1 d . . . C7 C 0.1461(3) 0.4265(3) 0.28561(19) 0.0270(5) Uani 1 1 d . A . C8 C 0.1035(3) 0.5720(3) 0.2828(2) 0.0300(5) Uani 1 1 d . . . H8A H -0.0031 0.6046 0.2923 0.036 Uiso 1 1 calc R A . C9 C 0.2073(3) 0.6790(3) 0.26673(19) 0.0267(5) Uani 1 1 d . A . C10 C 0.1331(3) 0.8295(3) 0.2839(2) 0.0346(6) Uani 1 1 d . . . C11 C 0.4941(3) 0.1441(3) 0.2180(2) 0.0289(5) Uani 1 1 d . . . H11A H 0.5394 0.0625 0.1882 0.035 Uiso 1 1 calc R . . H11B H 0.3802 0.1547 0.2134 0.035 Uiso 1 1 calc R . . C12 C 0.5389(3) 0.1047(3) 0.3282(2) 0.0322(6) Uani 1 1 d . . . H12A H 0.5055 0.1906 0.3563 0.039 Uiso 1 1 calc R . . H12B H 0.4876 0.0200 0.3681 0.039 Uiso 1 1 calc R . . C13 C 0.7497(4) 0.0372(4) 0.4358(2) 0.0497(8) Uani 1 1 d . . . H13A H 0.8629 0.0237 0.4374 0.074 Uiso 1 1 calc R . . H13B H 0.7122 -0.0533 0.4775 0.074 Uiso 1 1 calc R . . H13C H 0.7078 0.1214 0.4627 0.074 Uiso 1 1 calc R . . C14 C 0.4578(3) 0.7679(3) 0.2377(2) 0.0309(6) Uani 1 1 d . . . H14A H 0.3991 0.8551 0.2563 0.037 Uiso 1 1 calc R . . H14B H 0.4985 0.8026 0.1677 0.037 Uiso 1 1 calc R . . C15 C 0.5915(3) 0.7034(3) 0.3093(2) 0.0339(6) Uani 1 1 d . . . H15A H 0.6400 0.6064 0.2997 0.041 Uiso 1 1 calc R . . H15B H 0.6706 0.7714 0.2954 0.041 Uiso 1 1 calc R . . C16 C 0.6511(5) 0.6122(4) 0.4817(3) 0.0589(9) Uani 1 1 d . . . H16A H 0.6083 0.6016 0.5505 0.088 Uiso 1 1 calc R . . H16B H 0.7364 0.6714 0.4715 0.088 Uiso 1 1 calc R . . H16C H 0.6895 0.5136 0.4727 0.088 Uiso 1 1 calc R . . F1 F 0.7200(2) 0.79704(18) -0.02432(15) 0.0454(4) Uani 1 1 d . . . F2 F 0.9000(2) 0.6805(2) 0.07995(14) 0.0477(5) Uani 1 1 d . . . F3 F 0.8920(2) 0.63466(19) -0.06388(13) 0.0428(4) Uani 1 1 d . . . F4 F 0.8198(2) 0.17279(19) -0.02038(13) 0.0426(4) Uani 1 1 d . . . F5 F 0.7899(2) 0.03867(18) 0.13076(13) 0.0413(4) Uani 1 1 d . . . F6 F 0.60530(19) 0.09106(18) 0.02328(13) 0.0399(4) Uani 1 1 d . . . F7 F 0.0411(15) 0.2170(14) 0.2733(9) 0.093(5) Uani 0.50 1 d P A 1 F8 F 0.0353(17) 0.2582(16) 0.4164(8) 0.102(5) Uani 0.50 1 d P A 1 F9 F -0.1163(10) 0.3839(10) 0.3049(10) 0.090(5) Uani 0.50 1 d P A 1 F7' F 0.0691(13) 0.1934(12) 0.3078(12) 0.109(6) Uani 0.50 1 d P A 2 F8' F -0.0037(17) 0.2970(16) 0.4147(7) 0.100(5) Uani 0.50 1 d P A 2 F9' F -0.1014(11) 0.3724(12) 0.2750(9) 0.096(4) Uani 0.50 1 d P A 2 F10 F -0.0178(2) 0.8360(2) 0.29950(17) 0.0520(5) Uani 1 1 d . A . F11 F 0.1921(2) 0.85408(19) 0.36456(13) 0.0446(4) Uani 1 1 d . A . F12 F 0.1551(2) 0.94275(17) 0.20387(13) 0.0440(4) Uani 1 1 d . A . 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 0.02307(12) 0.01983(12) 0.02697(12) -0.00782(7) 0.00231(8) -0.00423(7) O1 0.0317(10) 0.0269(9) 0.0367(10) -0.0137(8) 0.0078(8) -0.0096(7) O2 0.0260(9) 0.0229(9) 0.0380(10) -0.0086(7) 0.0071(8) -0.0041(7) O3 0.0348(11) 0.0451(12) 0.0326(10) -0.0087(9) 0.0021(8) -0.0013(9) O4 0.0467(13) 0.0532(13) 0.0345(11) -0.0166(10) -0.0037(9) -0.0057(10) N1 0.0247(10) 0.0217(10) 0.0278(10) -0.0085(8) 0.0001(8) -0.0041(8) N2 0.0284(11) 0.0184(9) 0.0257(10) -0.0068(8) -0.0010(8) -0.0032(8) C1 0.0259(13) 0.0304(13) 0.0361(14) -0.0076(11) 0.0001(11) -0.0060(10) C2 0.0220(11) 0.0291(13) 0.0277(12) -0.0054(10) -0.0035(10) -0.0036(9) C3 0.0230(12) 0.0319(13) 0.0291(12) -0.0097(10) 0.0014(10) -0.0042(10) C4 0.0232(11) 0.0261(12) 0.0268(12) -0.0094(10) -0.0024(10) -0.0008(9) C5 0.0303(13) 0.0300(13) 0.0324(13) -0.0107(11) 0.0008(11) -0.0029(10) C6 0.0275(13) 0.0344(15) 0.0403(15) -0.0077(12) 0.0036(12) -0.0048(11) C7 0.0250(12) 0.0281(13) 0.0284(12) -0.0084(10) -0.0004(10) -0.0044(10) C8 0.0231(12) 0.0302(13) 0.0359(14) -0.0090(11) 0.0000(11) -0.0009(10) C9 0.0304(13) 0.0229(12) 0.0270(12) -0.0090(10) -0.0026(10) 0.0007(10) C10 0.0334(14) 0.0321(14) 0.0400(15) -0.0153(12) 0.0000(12) 0.0002(11) C11 0.0317(13) 0.0206(12) 0.0364(14) -0.0103(10) 0.0052(11) -0.0070(10) C12 0.0341(14) 0.0273(13) 0.0343(14) -0.0081(11) 0.0091(11) -0.0053(10) C13 0.0470(18) 0.060(2) 0.0388(17) -0.0083(15) -0.0037(15) -0.0064(16) C14 0.0343(14) 0.0224(12) 0.0378(14) -0.0102(11) 0.0035(12) -0.0076(10) C15 0.0319(14) 0.0353(14) 0.0403(15) -0.0178(12) 0.0031(12) -0.0101(11) C16 0.064(2) 0.068(2) 0.048(2) -0.0180(18) -0.0181(18) -0.0080(19) F1 0.0356(9) 0.0284(8) 0.0632(12) 0.0011(8) 0.0053(8) -0.0040(7) F2 0.0431(10) 0.0583(12) 0.0469(10) -0.0112(9) -0.0044(8) -0.0275(9) F3 0.0398(9) 0.0429(10) 0.0456(10) -0.0116(8) 0.0182(8) -0.0135(7) F4 0.0465(10) 0.0393(9) 0.0457(10) -0.0208(8) 0.0183(8) -0.0067(8) F5 0.0447(10) 0.0338(9) 0.0416(9) -0.0118(7) -0.0058(8) 0.0110(7) F6 0.0399(9) 0.0395(9) 0.0497(10) -0.0269(8) -0.0021(8) -0.0062(7) F7 0.118(9) 0.099(9) 0.108(5) -0.080(6) 0.073(5) -0.085(7) F8 0.085(6) 0.126(8) 0.066(7) 0.056(6) -0.037(5) -0.072(5) F9 0.019(3) 0.032(3) 0.211(13) -0.026(5) 0.014(5) 0.001(2) F7' 0.052(4) 0.029(3) 0.250(16) -0.052(6) 0.073(7) -0.019(2) F8' 0.139(11) 0.143(10) 0.051(6) -0.042(7) 0.046(6) -0.110(8) F9' 0.060(6) 0.099(8) 0.104(5) 0.046(5) -0.053(5) -0.054(5) F10 0.0328(9) 0.0421(10) 0.0845(14) -0.0302(10) 0.0049(9) 0.0065(8) F11 0.0532(11) 0.0430(10) 0.0433(10) -0.0257(8) -0.0013(8) 0.0022(8) F12 0.0582(11) 0.0236(8) 0.0458(10) -0.0072(7) -0.0043(8) 0.0056(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd O1 1.9738(18) . ? Pd O2 1.9863(17) . ? Pd N2 2.041(2) . ? Pd N1 2.047(2) . ? O1 C2 1.282(3) . ? O2 C7 1.286(3) . ? O3 C13 1.411(4) . ? O3 C12 1.413(3) . ? O4 C16 1.414(4) . ? O4 C15 1.417(3) . ? N1 C4 1.300(3) . ? N1 C11 1.487(3) . ? N2 C9 1.297(3) . ? N2 C14 1.488(3) . ? C1 F1 1.327(3) . ? C1 F2 1.327(3) . ? C1 F3 1.337(3) . ? C1 C2 1.526(3) . ? C2 C3 1.357(4) . ? C3 C4 1.425(3) . ? C4 C5 1.543(3) . ? C5 F4 1.328(3) . ? C5 F5 1.329(3) . ? C5 F6 1.341(3) . ? C6 F7' 1.254(9) . ? C6 F9' 1.268(9) . ? C6 F8' 1.275(10) . ? C6 F8 1.291(11) . ? C6 F7 1.293(10) . ? C6 F9 1.299(8) . ? C6 C7 1.529(4) . ? C7 C8 1.358(4) . ? C8 C9 1.425(4) . ? C9 C10 1.544(4) . ? C10 F10 1.321(3) . ? C10 F12 1.333(3) . ? C10 F11 1.336(3) . ? C11 C12 1.512(4) . ? C14 C15 1.511(4) . ? 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 O1 Pd O2 176.81(7) . . ? O1 Pd N2 87.26(8) . . ? O2 Pd N2 92.02(8) . . ? O1 Pd N1 92.35(8) . . ? O2 Pd N1 88.43(8) . . ? N2 Pd N1 178.96(8) . . ? C2 O1 Pd 123.03(16) . . ? C7 O2 Pd 122.02(16) . . ? C13 O3 C12 110.8(2) . . ? C16 O4 C15 111.5(3) . . ? C4 N1 C11 122.0(2) . . ? C4 N1 Pd 122.80(17) . . ? C11 N1 Pd 115.20(16) . . ? C9 N2 C14 122.1(2) . . ? C9 N2 Pd 122.40(17) . . ? C14 N2 Pd 115.55(16) . . ? F1 C1 F2 107.7(2) . . ? F1 C1 F3 106.9(2) . . ? F2 C1 F3 106.8(2) . . ? F1 C1 C2 111.7(2) . . ? F2 C1 C2 110.5(2) . . ? F3 C1 C2 113.0(2) . . ? O1 C2 C3 129.7(2) . . ? O1 C2 C1 110.5(2) . . ? C3 C2 C1 119.7(2) . . ? C2 C3 C4 124.2(2) . . ? N1 C4 C3 125.5(2) . . ? N1 C4 C5 120.8(2) . . ? C3 C4 C5 113.7(2) . . ? F4 C5 F5 106.9(2) . . ? F4 C5 F6 105.9(2) . . ? F5 C5 F6 107.5(2) . . ? F4 C5 C4 112.2(2) . . ? F5 C5 C4 112.7(2) . . ? F6 C5 C4 111.2(2) . . ? F7' C6 F9' 108.3(9) . . ? F7' C6 F8' 104.7(9) . . ? F9' C6 F8' 106.4(9) . . ? F7' C6 F8 87.1(10) . . ? F9' C6 F8 123.0(8) . . ? F8' C6 F8 20.5(12) . . ? F7' C6 F7 23.5(11) . . ? F9' C6 F7 88.1(8) . . ? F8' C6 F7 123.4(9) . . ? F8 C6 F7 108.5(9) . . ? F7' C6 F9 121.3(8) . . ? F9' C6 F9 20.6(9) . . ? F8' C6 F9 87.1(9) . . ? F8 C6 F9 105.4(9) . . ? F7 C6 F9 104.9(8) . . ? F7' C6 C7 113.7(6) . . ? F9' C6 C7 111.8(5) . . ? F8' C6 C7 111.4(6) . . ? F8 C6 C7 110.5(7) . . ? F7 C6 C7 112.7(6) . . ? F9 C6 C7 114.3(5) . . ? O2 C7 C8 129.1(2) . . ? O2 C7 C6 112.6(2) . . ? C8 C7 C6 118.3(2) . . ? C7 C8 C9 124.6(2) . . ? N2 C9 C8 125.3(2) . . ? N2 C9 C10 120.9(2) . . ? C8 C9 C10 113.8(2) . . ? F10 C10 F12 106.8(2) . . ? F10 C10 F11 106.9(2) . . ? F12 C10 F11 107.6(2) . . ? F10 C10 C9 112.1(2) . . ? F12 C10 C9 111.5(2) . . ? F11 C10 C9 111.5(2) . . ? N1 C11 C12 111.3(2) . . ? O3 C12 C11 108.7(2) . . ? N2 C14 C15 112.1(2) . . ? O4 C15 C14 108.4(2) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.115 _refine_diff_density_min -1.103 _refine_diff_density_rms 0.204 #===END data_ic6753 _database_code_CSD 192600 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C18 H24 F12 N2 O4 Pd' _chemical_formula_weight 666.79 _chemical_melting_point ? _chemical_compound_source ? 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' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pd' 'Pd' -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 5.8906(1) _cell_length_b 10.2740(2) _cell_length_c 10.9422(1) _cell_angle_alpha 77.307(1) _cell_angle_beta 89.906(1) _cell_angle_gamma 75.714(1) _cell_volume 625.09(2) _cell_formula_units_Z 1 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 5903 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour 'light yellow' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas not_measured _exptl_crystal_density_diffrn 1.771 _exptl_crystal_density_method ? _exptl_crystal_F_000 332 _exptl_absorpt_coefficient_mu 0.859 _exptl_absorpt_correction_type 'empirical used sadabs' _exptl_absorpt_correction_T_min 0.8087 _exptl_absorpt_correction_T_max 0.8944 _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(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 'Siemens SMART CCD' _diffrn_measurement_method '\w scans' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 8392 _diffrn_reflns_av_R_equivalents 0.0278 _diffrn_reflns_av_sigmaI/netI 0.0322 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.91 _diffrn_reflns_theta_max 27.47 _reflns_number_total 2874 _reflns_number_observed 2811 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens SMART' _computing_cell_refinement 'Siemens SAINT' _computing_data_reduction 'Siemens SAINT' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0363P)^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 ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0111(17) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 2874 _refine_ls_number_parameters 170 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0273 _refine_ls_R_factor_obs 0.0262 _refine_ls_wR_factor_all 0.0636 _refine_ls_wR_factor_obs 0.0630 _refine_ls_goodness_of_fit_all 1.061 _refine_ls_goodness_of_fit_obs 1.064 _refine_ls_restrained_S_all 1.061 _refine_ls_restrained_S_obs 1.064 _refine_ls_shift/esd_max -0.001 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Pd Pd 0.0000 0.0000 0.0000 0.03058(9) Uani 1 d S . O1 O 0.0190(4) -0.3342(2) 0.3406(2) 0.0719(6) Uani 1 d . . O2 O 0.0043(3) 0.12081(15) 0.12095(13) 0.0399(3) Uani 1 d . . N1 N -0.1956(3) -0.1073(2) 0.1184(2) 0.0371(4) Uani 1 d . . C1 C 0.2117(7) -0.4113(4) 0.4263(3) 0.0882(11) Uani 1 d . . H1A H 0.1692(7) -0.4072(4) 0.5104(3) 0.132 Uiso 1 calc R . H1B H 0.3442(7) -0.3731(4) 0.4073(3) 0.132 Uiso 1 calc R . H1C H 0.2515(7) -0.5056(4) 0.4189(3) 0.132 Uiso 1 calc R . C2 C 0.0709(4) -0.3363(2) 0.2153(2) 0.0515(6) Uani 1 d . . H2A H 0.1180(4) -0.4309(2) 0.2061(2) 0.062 Uiso 1 calc R . H2B H 0.1998(4) -0.2942(2) 0.1925(2) 0.062 Uiso 1 calc R . C3 C -0.1436(4) -0.2582(2) 0.1299(2) 0.0461(5) Uani 1 d . . H3A H -0.1194(4) -0.2774(2) 0.0473(2) 0.055 Uiso 1 calc R . H3B H -0.2779(4) -0.2908(2) 0.1623(2) 0.055 Uiso 1 calc R . C4 C -0.3496(4) -0.0459(2) 0.1841(2) 0.0424(5) Uani 1 d . . C5 C -0.4042(4) 0.1088(2) 0.1596(2) 0.0480(5) Uani 1 d . . H5A H -0.5291(4) 0.1407(2) 0.2120(2) 0.058 Uiso 1 calc R . H5B H -0.4612(4) 0.1470(2) 0.0728(2) 0.058 Uiso 1 calc R . C6 C -0.1900(4) 0.1647(2) 0.1852(2) 0.0426(5) Uani 1 d . . C7 C -0.4878(5) -0.1142(3) 0.2819(3) 0.0638(7) Uani 1 d . . H7A H -0.4401(5) -0.2122(3) 0.2904(3) 0.096 Uiso 1 calc R . H7B H -0.6520(5) -0.0813(3) 0.2572(3) 0.096 Uiso 1 calc R . H7C H -0.4599(5) -0.0927(3) 0.3607(3) 0.096 Uiso 1 calc R . C8 C -0.2701(6) 0.3243(3) 0.1442(3) 0.0707(8) Uani 1 d . . C9 C -0.1186(5) 0.1213(3) 0.3275(2) 0.0549(6) Uani 1 d . . F1 F -0.3462(4) 0.3633(2) 0.0234(2) 0.0881(6) Uani 1 d . . F2 F -0.0982(5) 0.3836(2) 0.1549(2) 0.1104(8) Uani 1 d . . F3 F -0.4460(4) 0.3805(2) 0.2092(2) 0.1117(8) Uani 1 d . . F4 F -0.2970(3) 0.1605(2) 0.3991(2) 0.0864(6) Uani 1 d . . F5 F 0.0553(3) 0.1726(2) 0.3569(2) 0.0814(5) Uani 1 d . . F6 F -0.0441(3) -0.0157(2) 0.36359(13) 0.0652(4) Uani 1 d . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd 0.03185(13) 0.02851(12) 0.02876(12) -0.00562(8) -0.00098(8) -0.00353(8) O1 0.0785(13) 0.0687(13) 0.0519(11) -0.0002(9) -0.0095(10) 0.0005(10) O2 0.0424(8) 0.0411(8) 0.0391(8) -0.0160(6) 0.0036(6) -0.0099(6) N1 0.0350(9) 0.0382(9) 0.0352(9) -0.0041(7) -0.0038(7) -0.0075(7) C1 0.094(2) 0.088(2) 0.067(2) 0.014(2) -0.027(2) -0.022(2) C2 0.0554(14) 0.0362(11) 0.0586(14) -0.0042(10) -0.0017(11) -0.0094(10) C3 0.0534(13) 0.0380(11) 0.0490(12) -0.0066(9) -0.0005(10) -0.0183(10) C4 0.0306(10) 0.0545(13) 0.0388(11) -0.0070(9) -0.0030(8) -0.0073(9) C5 0.0361(11) 0.0550(13) 0.0460(12) -0.0140(10) -0.0026(9) 0.0035(10) C6 0.0464(12) 0.0397(11) 0.0381(11) -0.0129(9) 0.0008(9) -0.0004(9) C7 0.0481(14) 0.078(2) 0.065(2) -0.0107(14) 0.0170(12) -0.0207(13) C8 0.089(2) 0.0435(14) 0.076(2) -0.0226(14) 0.012(2) -0.0008(14) C9 0.0527(14) 0.072(2) 0.0414(12) -0.0240(12) 0.0030(10) -0.0075(12) F1 0.114(2) 0.0477(9) 0.0764(12) 0.0044(8) -0.0013(11) 0.0128(9) F2 0.145(2) 0.0534(10) 0.144(2) -0.0331(12) 0.004(2) -0.0365(12) F3 0.137(2) 0.0650(12) 0.113(2) -0.0358(11) 0.0387(14) 0.0259(12) F4 0.0736(11) 0.130(2) 0.0508(9) -0.0375(10) 0.0161(8) -0.0010(11) F5 0.0852(12) 0.1101(15) 0.0646(10) -0.0395(10) -0.0068(9) -0.0364(11) F6 0.0690(10) 0.0732(11) 0.0421(7) -0.0022(7) -0.0098(7) -0.0063(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd O2 2.0076(13) 2 ? Pd O2 2.0076(13) . ? Pd N1 2.053(2) 2 ? Pd N1 2.053(2) . ? O1 C2 1.408(3) . ? O1 C1 1.424(3) . ? O2 C6 1.375(3) . ? N1 C4 1.285(3) . ? N1 C3 1.481(3) . ? C2 C3 1.513(3) . ? C4 C7 1.500(3) . ? C4 C5 1.504(3) . ? C5 C6 1.559(3) . ? C6 C9 1.550(3) . ? C6 C8 1.551(4) . ? C8 F2 1.322(4) . ? C8 F1 1.338(4) . ? C8 F3 1.340(3) . ? C9 F5 1.331(3) . ? C9 F6 1.335(3) . ? C9 F4 1.344(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 O2 Pd O2 180.0 2 . ? O2 Pd N1 90.16(6) 2 2 ? O2 Pd N1 89.84(6) . 2 ? O2 Pd N1 89.83(6) 2 . ? O2 Pd N1 90.16(6) . . ? N1 Pd N1 180.0 2 . ? C2 O1 C1 112.1(2) . . ? C6 O2 Pd 121.32(13) . . ? C4 N1 C3 121.6(2) . . ? C4 N1 Pd 120.78(15) . . ? C3 N1 Pd 117.52(14) . . ? O1 C2 C3 109.5(2) . . ? N1 C3 C2 112.7(2) . . ? N1 C4 C7 125.9(2) . . ? N1 C4 C5 118.1(2) . . ? C7 C4 C5 116.0(2) . . ? C4 C5 C6 113.8(2) . . ? O2 C6 C9 108.3(2) . . ? O2 C6 C8 108.0(2) . . ? C9 C6 C8 109.5(2) . . ? O2 C6 C5 114.6(2) . . ? C9 C6 C5 109.4(2) . . ? C8 C6 C5 107.0(2) . . ? F2 C8 F1 106.5(3) . . ? F2 C8 F3 106.9(3) . . ? F1 C8 F3 106.7(3) . . ? F2 C8 C6 112.6(3) . . ? F1 C8 C6 110.3(2) . . ? F3 C8 C6 113.5(3) . . ? F5 C9 F6 106.9(2) . . ? F5 C9 F4 107.1(2) . . ? F6 C9 F4 106.8(2) . . ? F5 C9 C6 112.5(2) . . ? F6 C9 C6 110.2(2) . . ? F4 C9 C6 113.0(2) . . ? _refine_diff_density_max 0.412 _refine_diff_density_min -0.315 _refine_diff_density_rms 0.059 #===END