# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_all_cif _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 #TrackingRef '- 1.cif' _journal_year 2012 _journal_page_first ? _publ_contact_author_name 'Wanzhi Chen' _publ_contact_author_address ; Department of Chemistry Zhejiang University Hangzhou 310027, P. R. China ; _publ_contact_author_email chenwzz@zju.edu.cn _publ_contact_author_fax 86-571-88273314 _publ_contact_author_phone 86-571-88273314 _publ_section_title ; Reactions of [PdL(NH3)2](PF6)2 (L = 1,1'-di(alkyl)-3,3'-methylenediimidazolin-2,2'-diylidene) with N-Donors ; loop_ _publ_author_name _publ_author_address 'Chao Chen' ; Department of Chemistry Zhejiang University Hangzhou 310027, P. R. China ; 'Huayu Qiu' ; College of Materials, Chemistry and Chemical Engineering Hangzhou Normal University Hangzhou 310036, P. R. China ; 'Wanzhi Chen' ; Department of Chemistry Zhejiang University Hangzhou 310027, P. R. China ; data_1 _database_code_depnum_ccdc_archive 'CCDC 894013' #TrackingRef 'web_deposit_cif_file_0_ChaoChen_1346500744.1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C11 H21 F12 N7 P2 Pd' _chemical_formula_weight 647.69 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' F F 0.0171 0.0103 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' '-x, -y, -z' 'x, -y-1/2, z' _cell_length_a 7.9610(3) _cell_length_b 9.8975(5) _cell_length_c 13.6347(5) _cell_angle_alpha 90.00 _cell_angle_beta 92.558(4) _cell_angle_gamma 90.00 _cell_volume 1073.26(8) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2481 _cell_measurement_theta_min 2.9849 _cell_measurement_theta_max 29.2386 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.004 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 640 _exptl_absorpt_coefficient_mu 1.132 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7134 _exptl_absorpt_correction_T_max 0.7888 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'multiwire proportional' _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 4988 _diffrn_reflns_av_R_equivalents 0.0279 _diffrn_reflns_av_sigmaI/netI 0.0350 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.99 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2006 _reflns_number_gt 1811 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker FRAMBO' _computing_cell_refinement 'Bruker FRAMBO' _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^)+(0.0208P)^2^+0.3984P] 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 2006 _refine_ls_number_parameters 169 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0294 _refine_ls_R_factor_gt 0.0239 _refine_ls_wR_factor_ref 0.0534 _refine_ls_wR_factor_gt 0.0504 _refine_ls_goodness_of_fit_ref 1.076 _refine_ls_restrained_S_all 1.076 _refine_ls_shift/su_max 0.011 _refine_ls_shift/su_mean 0.001 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 0.78255(3) 0.2500 0.789699(17) 0.00946(9) Uani 1 2 d S . . C1 C 0.6064(3) 0.1172(2) 0.81921(15) 0.0111(5) Uani 1 1 d . . . C5 C 0.5218(5) 0.2500 0.9598(2) 0.0119(7) Uani 1 2 d S . . H5A H 0.4329 0.2500 1.0061 0.014 Uiso 1 2 calc SR . . H5B H 0.6292 0.2500 0.9963 0.014 Uiso 1 2 calc SR . . C3 C 0.4098(3) -0.0453(2) 0.81848(16) 0.0139(5) Uani 1 1 d . . . H3 H 0.3470 -0.1208 0.7993 0.017 Uiso 1 1 calc R . . C4 C 0.3853(3) 0.0337(2) 0.89715(16) 0.0115(5) Uani 1 1 d . . . H4 H 0.3023 0.0240 0.9425 0.014 Uiso 1 1 calc R . . C2 C 0.6120(3) -0.0477(3) 0.68160(17) 0.0188(6) Uani 1 1 d . . . H2A H 0.6636 0.0232 0.6455 0.028 Uiso 1 1 calc R . . H2B H 0.5216 -0.0867 0.6421 0.028 Uiso 1 1 calc R . . H2C H 0.6941 -0.1161 0.6980 0.028 Uiso 1 1 calc R . . C6 C 0.3069(5) 0.2500 0.6326(3) 0.0212(9) Uani 1 2 d S . . C7 C 0.3350(7) 0.2500 0.5293(3) 0.079(2) Uani 1 2 d S . . H7A H 0.2694 0.1797 0.4978 0.118 Uiso 0.50 1 calc PR . . H7B H 0.4521 0.2344 0.5194 0.118 Uiso 0.50 1 calc PR . . H7C H 0.3025 0.3358 0.5017 0.118 Uiso 0.50 1 calc PR . . N3 N 0.9632(3) 0.0992(2) 0.76613(14) 0.0166(5) Uani 1 1 d . . . H3A H 0.9398 0.0262 0.8010 0.025 Uiso 1 1 calc R . . H3B H 1.0648 0.1298 0.7848 0.025 Uiso 1 1 calc R . . H3C H 0.9613 0.0780 0.7027 0.025 Uiso 1 1 calc R . . N1 N 0.5465(3) 0.00745(19) 0.77140(13) 0.0115(4) Uani 1 1 d . . . N2 N 0.5078(2) 0.13125(19) 0.89673(13) 0.0100(4) Uani 1 1 d . . . N4 N 0.2855(4) 0.2500 0.7136(2) 0.0192(7) Uani 1 2 d S . . P1 P 0.04887(12) 0.2500 0.07154(6) 0.0160(2) Uani 1 2 d S . . P2 P 0.85356(13) 0.2500 0.44925(7) 0.0243(2) Uani 1 2 d S . . F2 F 0.1089(3) 0.2500 -0.03841(13) 0.0234(5) Uani 1 2 d S . . F3 F 0.1859(2) 0.13582(16) 0.09848(11) 0.0311(4) Uani 1 1 d . . . F1 F -0.0857(2) 0.13646(16) 0.04349(13) 0.0407(5) Uani 1 1 d . . . F4 F -0.0077(4) 0.2500 0.18095(17) 0.0584(8) Uani 1 2 d S . . F5 F 0.7469(3) 0.2500 0.34726(14) 0.0283(5) Uani 1 2 d S . . F7 F 0.9547(3) 0.2500 0.55271(15) 0.0614(9) Uani 1 2 d S . . F6 F 0.9744(2) 0.13704(19) 0.40940(12) 0.0437(5) Uani 1 1 d . . . F8 F 0.7311(2) 0.1365(2) 0.48849(12) 0.0513(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.00801(15) 0.00879(15) 0.01169(14) 0.000 0.00163(10) 0.000 C1 0.0110(13) 0.0099(12) 0.0123(11) 0.0016(9) -0.0023(10) 0.0036(10) C5 0.0151(19) 0.0097(17) 0.0109(16) 0.000 0.0008(14) 0.000 C3 0.0129(13) 0.0086(12) 0.0199(12) 0.0029(10) -0.0023(10) -0.0030(10) C4 0.0092(13) 0.0085(12) 0.0167(12) 0.0037(10) 0.0004(10) 0.0002(10) C2 0.0222(15) 0.0163(13) 0.0181(12) -0.0060(10) 0.0036(11) -0.0020(11) C6 0.0081(19) 0.032(2) 0.023(2) 0.000 -0.0011(16) 0.000 C7 0.027(3) 0.192(7) 0.018(2) 0.000 0.010(2) 0.000 N3 0.0135(12) 0.0136(11) 0.0231(11) 0.0007(9) 0.0041(9) -0.0006(9) N1 0.0134(11) 0.0086(10) 0.0126(9) 0.0004(8) 0.0004(8) 0.0007(9) N2 0.0106(11) 0.0074(10) 0.0118(9) 0.0010(8) -0.0004(8) -0.0003(8) N4 0.0111(17) 0.0245(18) 0.0216(17) 0.000 -0.0035(13) 0.000 P1 0.0130(5) 0.0145(5) 0.0209(5) 0.000 0.0062(4) 0.000 P2 0.0151(5) 0.0445(7) 0.0132(5) 0.000 -0.0005(4) 0.000 F2 0.0279(13) 0.0282(12) 0.0139(10) 0.000 -0.0002(9) 0.000 F3 0.0286(10) 0.0295(9) 0.0349(8) 0.0139(7) -0.0009(7) 0.0107(8) F1 0.0219(10) 0.0238(9) 0.0768(13) 0.0019(9) 0.0050(9) -0.0117(7) F4 0.070(2) 0.075(2) 0.0330(14) 0.000 0.0375(14) 0.000 F5 0.0273(14) 0.0375(14) 0.0191(11) 0.000 -0.0092(10) 0.000 F7 0.0254(15) 0.143(3) 0.0148(12) 0.000 -0.0054(11) 0.000 F6 0.0372(11) 0.0514(12) 0.0427(10) 0.0060(9) 0.0040(8) 0.0195(9) F8 0.0376(12) 0.0744(14) 0.0421(10) 0.0282(10) 0.0045(9) -0.0114(10) _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 C1 1.976(2) . ? Pd1 C1 1.976(2) 4_565 ? Pd1 N3 2.107(2) 4_565 ? Pd1 N3 2.107(2) . ? C1 N1 1.344(3) . ? C1 N2 1.351(3) . ? C5 N2 1.457(3) 4_565 ? C5 N2 1.457(3) . ? C3 C4 1.348(3) . ? C3 N1 1.390(3) . ? C4 N2 1.372(3) . ? C2 N1 1.458(3) . ? C6 N4 1.125(4) . ? C6 C7 1.435(5) . ? P1 F4 1.577(2) . ? P1 F1 1.5874(17) . ? P1 F1 1.5874(17) 4_565 ? P1 F2 1.594(2) . ? P1 F3 1.6018(16) 4_565 ? P1 F3 1.6018(16) . ? P2 F6 1.5864(19) 4_565 ? P2 F6 1.5864(19) . ? P2 F7 1.593(2) . ? P2 F8 1.5956(19) . ? P2 F8 1.5956(19) 4_565 ? P2 F5 1.597(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 C1 Pd1 C1 83.34(13) . 4_565 ? C1 Pd1 N3 175.81(8) . 4_565 ? C1 Pd1 N3 93.19(9) 4_565 4_565 ? C1 Pd1 N3 93.19(9) . . ? C1 Pd1 N3 175.81(8) 4_565 . ? N3 Pd1 N3 90.17(11) 4_565 . ? N1 C1 N2 104.9(2) . . ? N1 C1 Pd1 132.74(17) . . ? N2 C1 Pd1 122.22(16) . . ? N2 C5 N2 107.5(2) 4_565 . ? C4 C3 N1 107.1(2) . . ? C3 C4 N2 106.1(2) . . ? N4 C6 C7 179.7(4) . . ? C1 N1 C3 110.36(19) . . ? C1 N1 C2 125.3(2) . . ? C3 N1 C2 124.3(2) . . ? C1 N2 C4 111.62(19) . . ? C1 N2 C5 120.8(2) . . ? C4 N2 C5 126.9(2) . . ? F4 P1 F1 90.56(11) . . ? F4 P1 F1 90.56(11) . 4_565 ? F1 P1 F1 90.14(13) . 4_565 ? F4 P1 F2 179.13(15) . . ? F1 P1 F2 90.05(10) . . ? F1 P1 F2 90.05(10) 4_565 . ? F4 P1 F3 90.19(11) . 4_565 ? F1 P1 F3 179.22(11) . 4_565 ? F1 P1 F3 90.06(9) 4_565 4_565 ? F2 P1 F3 89.19(9) . 4_565 ? F4 P1 F3 90.19(11) . . ? F1 P1 F3 90.06(9) . . ? F1 P1 F3 179.22(11) 4_565 . ? F2 P1 F3 89.19(9) . . ? F3 P1 F3 89.74(13) 4_565 . ? F6 P2 F6 89.62(15) 4_565 . ? F6 P2 F7 90.76(10) 4_565 . ? F6 P2 F7 90.76(10) . . ? F6 P2 F8 179.51(11) 4_565 . ? F6 P2 F8 90.43(11) . . ? F7 P2 F8 89.73(10) . . ? F6 P2 F8 90.43(11) 4_565 4_565 ? F6 P2 F8 179.51(11) . 4_565 ? F7 P2 F8 89.73(10) . 4_565 ? F8 P2 F8 89.52(16) . 4_565 ? F6 P2 F5 90.50(9) 4_565 . ? F6 P2 F5 90.50(9) . . ? F7 P2 F5 178.23(15) . . ? F8 P2 F5 89.01(9) . . ? F8 P2 F5 89.01(9) 4_565 . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.335 _refine_diff_density_min -0.403 _refine_diff_density_rms 0.083 #===END data_5 _database_code_depnum_ccdc_archive 'CCDC 894014' #TrackingRef '- 1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C58 H57.50 F24 N18 P4 Pd2' _chemical_formula_weight 1799.40 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' 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' F F 0.0171 0.0103 '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 17.8254(3) _cell_length_b 19.0418(3) _cell_length_c 28.6028(5) _cell_angle_alpha 96.653(2) _cell_angle_beta 98.400(2) _cell_angle_gamma 109.012(2) _cell_volume 8940.8(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 24165 _cell_measurement_theta_min 2.9370 _cell_measurement_theta_max 29.5542 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.39 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.32 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.337 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3598 _exptl_absorpt_coefficient_mu 0.566 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8094 _exptl_absorpt_correction_T_max 0.8396 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'multiwire proportional' _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 111703 _diffrn_reflns_av_R_equivalents 0.0535 _diffrn_reflns_av_sigmaI/netI 0.0596 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 2.94 _diffrn_reflns_theta_max 25.01 _reflns_number_total 31476 _reflns_number_gt 20136 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker FRAMBO' _computing_cell_refinement 'Bruker FRAMBO' _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 fullcycle _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.3300P)^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 31476 _refine_ls_number_parameters 1921 _refine_ls_number_restraints 1197 _refine_ls_R_factor_all 0.1658 _refine_ls_R_factor_gt 0.1319 _refine_ls_wR_factor_ref 0.4467 _refine_ls_wR_factor_gt 0.4032 _refine_ls_goodness_of_fit_ref 1.125 _refine_ls_restrained_S_all 1.145 _refine_ls_shift/su_max 0.012 _refine_ls_shift/su_mean 0.002 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 0.4437 0.9775 0.6241 0.0554(3) Uani 1 1 d . . . Pd2 Pd -0.0213 0.3606 0.8489 0.0637(3) Uani 1 1 d . . . Pd3 Pd 0.5684 0.6438 0.9038 0.0541(3) Uani 1 1 d . . . Pd4 Pd -0.1454 0.7305 0.5907 0.0562(3) Uani 1 1 d . . . P1 P 0.2725 0.4967 0.8524 0.0662(8) Uani 1 1 d DU . . P2 P 0.1510 0.8691 0.6289 0.0694(8) Uani 1 1 d DU . . P6 P 0.2624 0.6197 0.0528 0.0779(10) Uani 1 1 d DU . . P3 P 0.1257 0.6929 0.4367 0.0950(13) Uani 1 1 d DU . . N5 N 0.4593 0.9465 0.6914 0.0491(18) Uani 1 1 d . . . P8 P 0.8459 0.7245 0.8887 0.0787(9) Uani 1 1 d DU . . C59 C 0.5690 0.6196 0.9680 0.061(3) Uani 1 1 d . . . N23 N 0.5798 0.5445 0.8734 0.057(2) Uani 1 1 d . . . N14 N -0.1540 0.8327 0.6171 0.0449(17) Uani 1 1 d . . . P5 P 0.7055 0.1126 0.6683 0.0785(10) Uani 1 1 d DU . . P4 P 0.5898 0.6379 0.6107 0.0983(12) Uani 1 1 d DU . . N32 N -0.0315 0.4008 0.7843 0.055(2) Uani 1 1 d . . . N9 N -0.1245 0.7102 0.6586 0.0518(19) Uani 1 1 d . . . N18 N 0.4339 1.0760 0.6567 0.0444(17) Uani 1 1 d . . . F1 F 0.2824 0.5102 0.9089 0.098(2) Uani 1 1 d DU . . C66 C 0.5461 0.7340 0.9334 0.054(3) Uani 1 1 d . . . F34 F 0.2730 0.6383 0.1092 0.089(2) Uani 1 1 d DU . . N8 N -0.0488 0.6999 0.7259 0.0521(19) Uani 1 1 d . . . C1 C 0.4197 0.9991 0.5593 0.059(3) Uani 1 1 d . . . N33 N 0.0103 0.4704 0.7304 0.0523(19) Uani 1 1 d . . . C38 C -0.1592 0.7538 0.5258 0.059(3) Uani 1 1 d . . . C47 C 0.0767 1.1208 0.6587 0.053(2) Uani 1 1 d . . . C86 C -0.0530 0.4127 0.7076 0.071(3) Uani 1 1 d . . . H86 H -0.0750 0.4022 0.6749 0.085 Uiso 1 1 calc R . . C27 C -0.0506 0.7066 0.6803 0.057(2) Uani 1 1 d . . . H27 H -0.0079 0.7087 0.6646 0.068 Uiso 1 1 calc R . . N27 N -0.0087 0.2623 0.8138 0.072(3) Uani 1 1 d . . . C115 C 0.6186 0.4576 0.8364 0.065(3) Uani 1 1 d . . . H115 H 0.6489 0.4340 0.8211 0.079 Uiso 1 1 calc R . . F14 F 0.1277 0.6125 0.4168 0.153(4) Uani 1 1 d DU . . C93 C 0.0618 0.3318 0.9815 0.099(5) Uani 1 1 d . . . H93 H 0.1026 0.3501 1.0087 0.119 Uiso 1 1 calc R . . C91 C -0.0160 0.4557 0.8873 0.050(2) Uani 1 1 d . . . C33 C -0.1284 0.6392 0.5617 0.067(3) Uani 1 1 d . . . C74 C 0.3406 0.6425 0.7411 0.057(2) Uani 1 1 d . . . H74 H 0.3323 0.6203 0.7681 0.068 Uiso 1 1 calc R . . F35 F 0.3448 0.6042 0.0610 0.092(2) Uani 1 1 d DU . . C75 C 0.2753 0.6393 0.7068 0.056(2) Uani 1 1 d . . . N31 N -0.0581 0.5004 0.8836 0.065(2) Uani 1 1 d . . . F31 F 0.3173 0.7039 0.0532 0.108(3) Uani 1 1 d DU . . N22 N 0.6142 0.5921 0.9983 0.070(3) Uani 1 1 d . . . C77 C 0.2091 0.6811 0.5906 0.069(3) Uani 1 1 d . . . H77A H 0.2420 0.7329 0.5906 0.083 Uiso 1 1 calc R . . H77B H 0.1530 0.6753 0.5796 0.083 Uiso 1 1 calc R . . N15 N -0.1071 0.9578 0.6370 0.0437(17) Uani 1 1 d . . . F11 F 0.1597 0.8395 0.5766 0.127(3) Uani 1 1 d DU . . C8 C 0.4446 0.8808 0.5900 0.055(2) Uani 1 1 d . . . C19 C 0.1585 0.7384 0.7863 0.063(3) Uani 1 1 d . . . N30 N 0.0396 0.4843 0.9274 0.065(2) Uani 1 1 d . . . N34 N 0.2197 0.6655 0.6387 0.058(2) Uani 1 1 d . . . C109 C 0.3614 0.2484 0.8106 0.058(3) Uani 1 1 d . . . C26 C 0.0954 0.7421 0.7537 0.052(2) Uani 1 1 d . . . H26 H 0.1038 0.7708 0.7295 0.063 Uiso 1 1 calc R . . C81 C 0.1411 0.5585 0.7266 0.053(2) Uani 1 1 d . . . H81 H 0.1639 0.5510 0.7561 0.063 Uiso 1 1 calc R . . N26 N 0.0670 0.2008 0.7930 0.060(2) Uani 1 1 d . . . C102 C 0.2792 0.2092 0.8011 0.067(3) Uani 1 1 d . . . N20 N 0.4935 0.7257 0.9618 0.068(2) Uani 1 1 d . . . N24 N 0.5406 0.4231 0.8456 0.0516(19) Uani 1 1 d . . . F44 F 0.8233 0.6536 0.9148 0.132(4) Uani 1 1 d DU . . C73 C 0.4220 0.6809 0.7343 0.071(3) Uani 1 1 d . . . C68 C 0.4865 0.6707 0.8138 0.060(3) Uani 1 1 d . . . H68 H 0.4422 0.6641 0.8287 0.072 Uiso 1 1 calc R . . N6 N 0.4233 0.8940 0.7528 0.057(2) Uani 1 1 d . . . C80 C 0.1906 0.6063 0.7019 0.054(2) Uani 1 1 d . . . F29 F 0.7936 0.1728 0.6873 0.129(3) Uani 1 1 d DU . . C85 C 0.0198 0.4631 0.7762 0.056(2) Uani 1 1 d . . . H85 H 0.0591 0.4987 0.8002 0.068 Uiso 1 1 calc R . . C95 C -0.0027 0.3297 0.9127 0.083(4) Uani 1 1 d . . . F32 F 0.2515 0.6021 -0.0036 0.112(3) Uani 1 1 d DU . . N21 N 0.5110 0.6240 0.9934 0.070(3) Uani 1 1 d . . . C60 C 0.6894 0.5748 0.9840 0.075(3) Uani 1 1 d . . . H60A H 0.6846 0.5687 0.9498 0.113 Uiso 1 1 calc R . . H60B H 0.6914 0.5292 0.9946 0.113 Uiso 1 1 calc R . . H60C H 0.7382 0.6159 0.9991 0.113 Uiso 1 1 calc R . . C82 C 0.0597 0.5215 0.7095 0.066(3) Uani 1 1 d . . . F43 F 0.8019 0.6714 0.8387 0.149(4) Uani 1 1 d DU . . F46 F 0.8801 0.7785 0.9391 0.141(4) Uani 1 1 d DU . . N29 N 0.0558 0.3751 0.9465 0.078(3) Uani 1 1 d . . . C69 C 0.6045 0.6789 0.8021 0.088(4) Uani 1 1 d . . . H69 H 0.6582 0.6818 0.8066 0.105 Uiso 1 1 calc R . . F33 F 0.2146 0.5337 0.0526 0.114(3) Uani 1 1 d DU . . F36 F 0.1794 0.6342 0.0463 0.120(3) Uani 1 1 d DU . . C25 C 0.0160 0.6989 0.7596 0.057(2) Uani 1 1 d . . . C48 C 0.1651 1.1572 0.6668 0.052(2) Uani 1 1 d . . . C55 C 0.2295 1.1290 0.6696 0.049(2) Uani 1 1 d . . . H55 H 0.2200 1.0774 0.6654 0.059 Uiso 1 1 calc R . . F48 F 0.7583 0.7280 0.8879 0.132(3) Uani 1 1 d DU . . C17 C 0.2440 0.7749 0.7912 0.058(3) Uani 1 1 d . . . F18 F 0.1435 0.7196 0.3878 0.131(3) Uani 1 1 d DU . . C71 C 0.3688 0.7126 0.6638 0.066(3) Uani 1 1 d . . . H71 H 0.3780 0.7380 0.6382 0.079 Uiso 1 1 calc R . . C88 C -0.1320 0.4824 0.8473 0.084(4) Uani 1 1 d . . . H88A H -0.1177 0.4938 0.8172 0.126 Uiso 1 1 calc R . . H88B H -0.1632 0.5119 0.8573 0.126 Uiso 1 1 calc R . . H88C H -0.1634 0.4298 0.8435 0.126 Uiso 1 1 calc R . . C56 C 0.3638 1.0845 0.6497 0.057(3) Uani 1 1 d . . . H56 H 0.3172 1.0495 0.6301 0.069 Uiso 1 1 calc R . . C76 C 0.2892 0.6751 0.6690 0.061(3) Uani 1 1 d . . . C18 C 0.2905 0.8201 0.7645 0.059(3) Uani 1 1 d . . . H18 H 0.2665 0.8309 0.7364 0.071 Uiso 1 1 calc R . . C39 C -0.0917 0.8963 0.6170 0.048(2) Uani 1 1 d . . . H39 H -0.0455 0.8980 0.6050 0.058 Uiso 1 1 calc R . . C114 C 0.5223 0.4793 0.8669 0.060(3) Uani 1 1 d . . . H114 H 0.4730 0.4726 0.8763 0.072 Uiso 1 1 calc R . . N19 N 0.5723 0.8035 0.9305 0.082(3) Uani 1 1 d . . . C101 C 0.2106 0.2324 0.7995 0.062(3) Uani 1 1 d . . . H101 H 0.2156 0.2830 0.8035 0.074 Uiso 1 1 calc R . . C79 C 0.1576 0.6236 0.6595 0.055(2) Uani 1 1 d . . . F27 F 0.6174 0.0524 0.6493 0.129(3) Uani 1 1 d DU . . C100 C 0.1381 0.1768 0.7918 0.064(3) Uani 1 1 d . . . F4 F 0.2625 0.4831 0.7958 0.139(4) Uani 1 1 d DU . . C99 C 0.0636 0.2608 0.8201 0.079(4) Uani 1 1 d . . . H99 H 0.1078 0.2970 0.8410 0.095 Uiso 1 1 calc R . . C42 C 0.0294 1.0517 0.6538 0.0412(19) Uani 1 1 d . . . H42 H 0.0514 1.0139 0.6567 0.049 Uiso 1 1 calc R . . C84 C 0.0738 0.5943 0.6415 0.065(3) Uani 1 1 d . . . H84 H 0.0512 0.6064 0.6135 0.078 Uiso 1 1 calc R . . C110 C 0.4138 0.3260 0.8200 0.061(3) Uani 1 1 d . . . H110 H 0.3911 0.3632 0.8169 0.073 Uiso 1 1 calc R . . C83 C 0.0288 0.5494 0.6657 0.066(3) Uani 1 1 d . . . H83 H -0.0270 0.5332 0.6552 0.080 Uiso 1 1 calc R . . C54 C 0.3072 1.1810 0.6787 0.063(3) Uani 1 1 d . . . C13 C 0.3748 0.8498 0.7801 0.061(3) Uani 1 1 d . . . C43 C -0.0551 1.0327 0.6441 0.051(2) Uani 1 1 d . . . C10 C 0.4005 0.8943 0.7065 0.062(3) Uani 1 1 d . . . H10 H 0.3513 0.8633 0.6873 0.074 Uiso 1 1 calc R . . F3 F 0.3291 0.5813 0.8551 0.163(4) Uani 1 1 d DU . . F30 F 0.6832 0.1292 0.7190 0.161(4) Uani 1 1 d DU . . C89 C -0.0237 0.5623 0.9227 0.075(3) Uani 1 1 d . . . H89 H -0.0429 0.6019 0.9279 0.090 Uiso 1 1 calc R . . F2 F 0.3491 0.4713 0.8569 0.155(4) Uani 1 1 d DU . . C87 C -0.0800 0.3716 0.7410 0.066(3) Uani 1 1 d . . . H87 H -0.1263 0.3286 0.7349 0.079 Uiso 1 1 calc R . . F5 F 0.1958 0.5220 0.8478 0.163(4) Uani 1 1 d DU . . C90 C 0.0356 0.5562 0.9491 0.070(3) Uani 1 1 d . . . H90 H 0.0693 0.5895 0.9762 0.084 Uiso 1 1 calc R . . C63 C 0.4488 0.6540 0.9756 0.075(3) Uani 1 1 d . . . H63A H 0.4195 0.6624 1.0005 0.090 Uiso 1 1 calc R . . H63B H 0.4107 0.6195 0.9482 0.090 Uiso 1 1 calc R . . F19 F 0.6786 0.6478 0.6033 0.158(4) Uani 1 1 d DU . . C72 C 0.4262 0.7119 0.6928 0.072(3) Uani 1 1 d . . . H72 H 0.4775 0.7344 0.6865 0.086 Uiso 1 1 calc R . . C78 C 0.2343 0.6249 0.5538 0.089(4) Uani 1 1 d . . . H78A H 0.2537 0.5921 0.5712 0.133 Uiso 1 1 calc R . . H78B H 0.2761 0.6542 0.5391 0.133 Uiso 1 1 calc R . . H78C H 0.1879 0.5954 0.5295 0.133 Uiso 1 1 calc R . . C70 C 0.5562 0.6808 0.7607 0.077(4) Uani 1 1 d . . . H70 H 0.5715 0.6826 0.7310 0.093 Uiso 1 1 calc R . . C116 C 0.6404 0.5317 0.8541 0.068(3) Uani 1 1 d . . . H116 H 0.6895 0.5684 0.8533 0.082 Uiso 1 1 calc R . . C112 C 0.5327 0.2933 0.8371 0.074(3) Uani 1 1 d . . . H112 H 0.5887 0.3082 0.8454 0.088 Uiso 1 1 calc R . . C111 C 0.4906 0.3457 0.8325 0.057(2) Uani 1 1 d . . . N28 N -0.0380 0.2602 0.9264 0.103(4) Uani 1 1 d . . . F15 F 0.1065 0.6658 0.4853 0.159(4) Uani 1 1 d DU . . C97 C -0.0132 0.1577 0.7656 0.075(3) Uani 1 1 d . . . H97 H -0.0313 0.1116 0.7449 0.091 Uiso 1 1 calc R . . C62 C 0.5224 0.6057 1.0375 0.087(4) Uani 1 1 d . . . H62 H 0.4927 0.6082 1.0613 0.104 Uiso 1 1 calc R . . C64 C 0.4840 0.7941 0.9780 0.083(4) Uani 1 1 d . . . H64 H 0.4549 0.8039 1.0009 0.100 Uiso 1 1 calc R . . C92 C 0.1001 0.4516 0.9434 0.073(3) Uani 1 1 d . . . H92A H 0.1357 0.4532 0.9207 0.087 Uiso 1 1 calc R . . H92B H 0.1324 0.4789 0.9745 0.087 Uiso 1 1 calc R . . C61 C 0.5919 0.5814 1.0391 0.087(4) Uani 1 1 d . . . H61 H 0.6151 0.5625 1.0637 0.104 Uiso 1 1 calc R . . N25 N 0.3377 0.1246 0.8044 0.129(6) Uani 1 1 d . . . C65 C 0.5228 0.8374 0.9552 0.113(6) Uani 1 1 d . . . H65 H 0.5213 0.8854 0.9535 0.136 Uiso 1 1 calc R . . F16 F 0.0312 0.6639 0.4168 0.179(5) Uani 1 1 d DU . . C98 C -0.0565 0.2049 0.7788 0.081(3) Uani 1 1 d . . . H98 H -0.1099 0.1974 0.7654 0.097 Uiso 1 1 calc R . . C113 C 0.4815 0.2178 0.8280 0.084(4) Uani 1 1 d . . . H113 H 0.5033 0.1805 0.8330 0.101 Uiso 1 1 calc R . . C108 C 0.4030 0.1984 0.8126 0.094(4) Uani 1 1 d . . . C67 C 0.6286 0.8398 0.9052 0.111(6) Uani 1 1 d . . . H67A H 0.6596 0.8088 0.8973 0.166 Uiso 1 1 calc R . . H67B H 0.6641 0.8869 0.9243 0.166 Uiso 1 1 calc R . . H67C H 0.6016 0.8490 0.8762 0.166 Uiso 1 1 calc R . . F28 F 0.6761 0.1756 0.6489 0.179(5) Uani 1 1 d DU . . F47 F 0.8684 0.7953 0.8626 0.206(6) Uani 1 1 d DU . . F20 F 0.5013 0.6293 0.6180 0.185(5) Uani 1 1 d DU . . C105 C 0.1218 0.1000 0.7825 0.092(4) Uani 1 1 d . . . H105 H 0.0697 0.0654 0.7713 0.111 Uiso 1 1 calc R . . C103 C 0.2653 0.1330 0.7947 0.092(4) Uani 1 1 d . . . F25 F 0.7316 0.0526 0.6940 0.189(5) Uani 1 1 d DU . . F6 F 0.2158 0.4121 0.8496 0.196(5) Uani 1 1 d DU . . F45 F 0.9356 0.7250 0.8933 0.173(4) Uani 1 1 d DU . . F17 F 0.1236 0.7733 0.4566 0.194(5) Uani 1 1 d DU . . F23 F 0.6248 0.7154 0.6469 0.198(5) Uani 1 1 d DU . . C94 C 0.0127 0.2706 0.9754 0.131(7) Uani 1 1 d . . . H94 H 0.0066 0.2362 0.9964 0.157 Uiso 1 1 calc R . . F12 F 0.0745 0.8879 0.6068 0.179(5) Uani 1 1 d DU . . C96 C -0.1133 0.1973 0.9014 0.121(6) Uani 1 1 d . . . H96A H -0.1551 0.2173 0.8921 0.182 Uiso 1 1 calc R . . H96B H -0.1303 0.1623 0.9226 0.182 Uiso 1 1 calc R . . H96C H -0.1030 0.1720 0.8733 0.182 Uiso 1 1 calc R . . C104 C 0.1905 0.0777 0.7912 0.099(5) Uani 1 1 d . . . H104 H 0.1856 0.0284 0.7944 0.119 Uiso 1 1 calc R . . F26 F 0.7320 0.0867 0.6207 0.172(5) Uani 1 1 d DU . . F10 F 0.0943 0.7871 0.6320 0.208(5) Uani 1 1 d DU . . C106 C 0.3621 0.0617 0.8036 0.149(8) Uani 1 1 d U . . H10A H 0.3486 0.0370 0.8306 0.179 Uiso 1 1 calc R . . H10B H 0.4201 0.0771 0.8056 0.179 Uiso 1 1 calc R . . F8 F 0.1986 0.9482 0.6164 0.231(6) Uani 1 1 d DU . . F22 F 0.5722 0.6542 0.5580 0.209(5) Uani 1 1 d DU . . F9 F 0.1427 0.8991 0.6811 0.211(5) Uani 1 1 d DU . . F21 F 0.5557 0.5610 0.5740 0.231(7) Uani 1 1 d DU . . F7 F 0.2279 0.8507 0.6509 0.203(5) Uani 1 1 d DU . . F24 F 0.6008 0.5943 0.6534 0.215(6) Uani 1 1 d DU . . N35 N 0.4836 0.6799 0.7692 0.069(3) Uani 1 1 d . . . N17 N 0.3677 1.1533 0.6755 0.054(2) Uani 1 1 d . . . C107 C 0.3202 0.0104 0.7589 0.213(16) Uani 1 1 d . . . H10C H 0.2774 0.0256 0.7441 0.320 Uiso 1 1 calc R . . H10D H 0.2978 -0.0399 0.7653 0.320 Uiso 1 1 calc R . . H10E H 0.3576 0.0115 0.7378 0.320 Uiso 1 1 calc R . . F13 F 0.2188 0.7201 0.4598 0.168(5) Uani 1 1 d DU . . N36 N 0.5557 0.6715 0.8358 0.057(2) Uani 1 1 d . . . P7 P 0.3814 0.9403 0.0895 0.170(3) Uani 1 1 d DU . . F41 F 0.4177 0.9050 0.1307 0.175(5) Uani 1 1 d DU . . F40 F 0.4648 1.0083 0.0982 0.185(5) Uani 1 1 d DU . . F39 F 0.3512 0.9863 0.1276 0.211(6) Uani 1 1 d DU . . F37 F 0.4117 0.8944 0.0514 0.195(5) Uani 1 1 d DU . . F38 F 0.2981 0.8724 0.0808 0.232(6) Uani 1 1 d DU . . F42 F 0.3452 0.9757 0.0483 0.165(4) Uani 1 1 d DU . . N16 N 0.1064 1.2438 0.6649 0.058(2) Uani 1 1 d . . . N7 N 0.2183 0.7132 0.8534 0.069(3) Uani 1 1 d . . . N13 N -0.2123 0.7729 0.4991 0.075(3) Uani 1 1 d . . . C41 C -0.1819 0.9301 0.6537 0.052(2) Uani 1 1 d . . . H41 H -0.2069 0.9587 0.6698 0.063 Uiso 1 1 calc R . . N4 N 0.4864 0.8354 0.5940 0.072(3) Uani 1 1 d . . . N2 N 0.3650 0.9446 0.5223 0.072(2) Uani 1 1 d U . . N11 N -0.0752 0.6438 0.5292 0.088(4) Uani 1 1 d . . . C45 C -0.0390 1.1625 0.6484 0.056(2) Uani 1 1 d . . . H45 H -0.0605 1.2009 0.6478 0.067 Uiso 1 1 calc R . . N3 N 0.3837 0.8399 0.5482 0.073(3) Uani 1 1 d . . . N10 N -0.1421 0.5724 0.5693 0.091(4) Uani 1 1 d . . . C51 C 0.1798 1.2362 0.6722 0.051(2) Uani 1 1 d . . . N1 N 0.4442 1.0598 0.5395 0.086(3) Uani 1 1 d . . . C28 C -0.1245 0.7039 0.7369 0.070(3) Uani 1 1 d . . . H28 H -0.1405 0.7024 0.7664 0.084 Uiso 1 1 calc R . . C46 C 0.0424 1.1788 0.6574 0.051(2) Uani 1 1 d . . . C23 C 0.0681 0.6604 0.8311 0.061(3) Uani 1 1 d . . . H23 H 0.0609 0.6321 0.8556 0.073 Uiso 1 1 calc R . . N12 N -0.1021 0.7462 0.4955 0.089(4) Uani 1 1 d . . . C20 C 0.1434 0.7014 0.8259 0.058(3) Uani 1 1 d . . . C52 C 0.2599 1.2866 0.6810 0.062(3) Uani 1 1 d . . . H52 H 0.2715 1.3384 0.6847 0.074 Uiso 1 1 calc R . . C24 C 0.0009 0.6614 0.7987 0.064(3) Uani 1 1 d . . . H24 H -0.0516 0.6381 0.8030 0.077 Uiso 1 1 calc R . . C49 C 0.0995 1.3233 0.6720 0.060(3) Uani 1 1 d . . . H49A H 0.1399 1.3569 0.6577 0.072 Uiso 1 1 calc R . . H49B H 0.0466 1.3202 0.6556 0.072 Uiso 1 1 calc R . . C16 C 0.2781 0.7554 0.8328 0.070(3) Uani 1 1 d . . . C40 C -0.2080 0.8560 0.6416 0.061(3) Uani 1 1 d . . . H40 H -0.2553 0.8234 0.6482 0.073 Uiso 1 1 calc R . . C44 C -0.0905 1.0861 0.6400 0.058(3) Uani 1 1 d . . . H44 H -0.1464 1.0727 0.6319 0.069 Uiso 1 1 calc R . . C58 C 0.4863 1.1349 0.6886 0.064(3) Uani 1 1 d . . . H58 H 0.5404 1.1422 0.6999 0.077 Uiso 1 1 calc R . . C53 C 0.3200 1.2571 0.6839 0.066(3) Uani 1 1 d . . . H53 H 0.3731 1.2904 0.6898 0.079 Uiso 1 1 calc R . . C7 C 0.4633 0.7765 0.5590 0.092(5) Uani 1 1 d . . . H7 H 0.4876 0.7404 0.5549 0.110 Uiso 1 1 calc R . . C57 C 0.4476 1.1813 0.7014 0.067(3) Uani 1 1 d . . . H57 H 0.4702 1.2254 0.7240 0.081 Uiso 1 1 calc R . . C9 C 0.5610 0.8629 0.6319 0.088(4) Uani 1 1 d . . . H9A H 0.5844 0.9168 0.6359 0.132 Uiso 1 1 calc R . . H9B H 0.5991 0.8408 0.6227 0.132 Uiso 1 1 calc R . . H9C H 0.5476 0.8489 0.6616 0.132 Uiso 1 1 calc R . . C29 C -0.1658 0.7101 0.6965 0.069(3) Uani 1 1 d . . . H29 H -0.2169 0.7140 0.6935 0.083 Uiso 1 1 calc R . . C31 C -0.1046 0.5365 0.5357 0.123(9) Uani 1 1 d . . . H31 H -0.1121 0.4853 0.5315 0.148 Uiso 1 1 calc R . . C430 C 0.4995 0.9487 0.7689 0.089(4) Uani 1 1 d . . . H430 H 0.5305 0.9602 0.7997 0.106 Uiso 1 1 calc R . . C15 C 0.3640 0.7856 0.8501 0.073(3) Uani 1 1 d . . . H15 H 0.3871 0.7745 0.8783 0.088 Uiso 1 1 calc R . . C432 C 0.5198 0.9818 0.7314 0.087(4) Uani 1 1 d . . . H432 H 0.5670 1.0220 0.7322 0.105 Uiso 1 1 calc R . . C34 C -0.0431 0.7151 0.5097 0.106(6) Uani 1 1 d . . . H34A H -0.0003 0.7519 0.5341 0.127 Uiso 1 1 calc R . . H34B H -0.0196 0.7048 0.4823 0.127 Uiso 1 1 calc R . . C35 C -0.1271 0.7654 0.4519 0.089(4) Uani 1 1 d . . . H35 H -0.0998 0.7694 0.4264 0.107 Uiso 1 1 calc R . . C6 C 0.3970 0.7793 0.5302 0.077(3) Uani 1 1 d . . . H6 H 0.3666 0.7447 0.5028 0.092 Uiso 1 1 calc R . . C3 C 0.4164 1.0493 0.4926 0.089(4) Uani 1 1 d U . . H3 H 0.4316 1.0844 0.4726 0.107 Uiso 1 1 calc R . . C36 C -0.1954 0.7768 0.4528 0.108(6) Uani 1 1 d . . . H36 H -0.2274 0.7859 0.4272 0.130 Uiso 1 1 calc R . . C5 C 0.3255 0.8705 0.5275 0.094(5) Uani 1 1 d . . . H5A H 0.2966 0.8403 0.4964 0.113 Uiso 1 1 calc R . . H5B H 0.2865 0.8693 0.5480 0.113 Uiso 1 1 calc R . . C21 C 0.2284 0.6871 0.9019 0.095(5) Uani 1 1 d . . . H21A H 0.2806 0.6812 0.9098 0.115 Uiso 1 1 calc R . . H21B H 0.1861 0.6395 0.9015 0.115 Uiso 1 1 calc R . . C37 C -0.2814 0.7901 0.5143 0.093(4) Uani 1 1 d . . . H37A H -0.2989 0.7617 0.5388 0.139 Uiso 1 1 calc R . . H37B H -0.3252 0.7767 0.4872 0.139 Uiso 1 1 calc R . . H37C H -0.2648 0.8430 0.5268 0.139 Uiso 1 1 calc R . . C14 C 0.4136 0.8337 0.8225 0.078(4) Uani 1 1 d . . . H14 H 0.4696 0.8537 0.8322 0.094 Uiso 1 1 calc R . . C50 C 0.1109 1.3539 0.7221 0.115(5) Uani 1 1 d . . . H50A H 0.0669 1.3244 0.7353 0.173 Uiso 1 1 calc R . . H50B H 0.1124 1.4051 0.7254 0.173 Uiso 1 1 calc R . . H50C H 0.1610 1.3526 0.7390 0.173 Uiso 1 1 calc R . . C30 C -0.1983 0.5362 0.6019 0.102(6) Uani 1 1 d . . . H30A H -0.1668 0.5368 0.6323 0.154 Uiso 1 1 calc R . . H30B H -0.2299 0.4850 0.5872 0.154 Uiso 1 1 calc R . . H30C H -0.2336 0.5640 0.6068 0.154 Uiso 1 1 calc R . . C2 C 0.5088 1.1330 0.5669 0.099(5) Uani 1 1 d . . . H2A H 0.4838 1.1691 0.5753 0.149 Uiso 1 1 calc R . . H2B H 0.5471 1.1526 0.5471 0.149 Uiso 1 1 calc R . . H2C H 0.5362 1.1234 0.5956 0.149 Uiso 1 1 calc R . . C32 C -0.0606 0.5823 0.5127 0.120(7) Uani 1 1 d . . . H32 H -0.0284 0.5748 0.4912 0.144 Uiso 1 1 calc R . . C22 C 0.2220 0.7514 0.9387 0.130(7) Uani 1 1 d . . . H22A H 0.2707 0.7947 0.9440 0.195 Uiso 1 1 calc R . . H22B H 0.2148 0.7341 0.9685 0.195 Uiso 1 1 calc R . . H22C H 0.1766 0.7649 0.9262 0.195 Uiso 1 1 calc R . . C4 C 0.3628 0.9795 0.4794 0.090(4) Uani 1 1 d U . . H4 H 0.3307 0.9575 0.4492 0.107 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 0.0420(4) 0.0736(6) 0.0617(5) 0.0208(4) 0.0202(3) 0.0278(4) Pd2 0.0726(6) 0.0645(6) 0.0443(5) 0.0038(4) 0.0117(4) 0.0130(4) Pd3 0.0737(6) 0.0364(4) 0.0350(4) 0.0134(3) -0.0063(3) 0.0011(4) Pd4 0.0603(5) 0.0554(5) 0.0490(5) -0.0082(3) -0.0086(3) 0.0292(4) P1 0.079(2) 0.0584(17) 0.0417(14) 0.0118(12) -0.0092(12) 0.0056(15) P2 0.082(2) 0.085(2) 0.0561(16) 0.0210(15) 0.0118(14) 0.0467(18) P6 0.105(3) 0.0614(19) 0.0435(15) 0.0006(13) -0.0008(15) 0.0069(18) P3 0.133(3) 0.114(3) 0.0479(16) -0.0109(17) -0.0233(18) 0.081(3) N5 0.040(4) 0.065(5) 0.055(4) 0.016(4) 0.012(3) 0.032(4) P8 0.0654(19) 0.080(2) 0.080(2) 0.0338(17) 0.0112(15) 0.0059(16) C59 0.097(8) 0.042(5) 0.029(4) -0.002(4) -0.009(5) 0.016(5) N23 0.096(6) 0.028(4) 0.023(3) 0.004(3) 0.013(4) -0.012(4) N14 0.037(4) 0.040(4) 0.055(4) 0.001(3) 0.011(3) 0.012(3) P5 0.0447(16) 0.097(3) 0.091(2) -0.0124(18) 0.0147(14) 0.0299(16) P4 0.071(2) 0.086(3) 0.125(3) 0.001(2) 0.008(2) 0.022(2) N32 0.050(5) 0.065(6) 0.043(4) 0.002(4) 0.005(3) 0.015(4) N9 0.046(4) 0.054(5) 0.049(4) -0.005(4) -0.008(3) 0.021(4) N18 0.039(4) 0.059(5) 0.048(4) 0.017(4) 0.023(3) 0.025(4) F1 0.137(6) 0.092(5) 0.053(4) 0.002(3) 0.014(4) 0.028(5) C66 0.068(6) 0.038(5) 0.044(5) 0.022(4) -0.012(4) 0.009(5) F34 0.120(5) 0.089(5) 0.044(3) -0.006(3) 0.014(3) 0.025(4) N8 0.051(5) 0.054(5) 0.046(4) 0.011(4) 0.004(3) 0.011(4) C1 0.038(5) 0.095(8) 0.050(5) 0.016(5) 0.011(4) 0.030(5) N33 0.048(5) 0.064(5) 0.037(4) 0.001(4) -0.002(3) 0.017(4) C38 0.084(7) 0.053(6) 0.047(5) -0.004(4) -0.002(5) 0.044(6) C47 0.044(5) 0.082(8) 0.051(5) 0.030(5) 0.021(4) 0.034(5) C86 0.074(7) 0.088(9) 0.034(5) 0.009(5) -0.016(5) 0.019(6) C27 0.067(6) 0.043(5) 0.059(6) 0.005(4) 0.012(5) 0.019(5) N27 0.089(7) 0.064(6) 0.055(5) 0.002(4) 0.031(5) 0.011(5) C115 0.100(9) 0.034(5) 0.044(5) 0.009(4) 0.014(5) -0.002(5) F14 0.178(9) 0.155(9) 0.116(7) 0.006(6) 0.014(6) 0.059(8) C93 0.126(13) 0.110(12) 0.082(9) 0.035(9) 0.025(9) 0.061(11) C91 0.051(5) 0.051(6) 0.047(5) 0.006(4) 0.025(4) 0.010(5) C33 0.092(8) 0.052(6) 0.057(6) -0.015(5) -0.026(5) 0.051(6) C74 0.076(7) 0.060(6) 0.035(4) 0.025(4) 0.010(4) 0.019(5) F35 0.136(6) 0.079(5) 0.062(4) 0.020(3) 0.028(4) 0.033(4) C75 0.076(7) 0.052(6) 0.031(4) 0.008(4) -0.001(4) 0.014(5) N31 0.047(5) 0.087(7) 0.059(5) 0.012(5) 0.017(4) 0.017(5) F31 0.144(7) 0.067(5) 0.084(5) 0.010(4) -0.002(5) 0.010(5) N22 0.115(8) 0.050(5) 0.046(5) 0.024(4) -0.006(5) 0.033(5) C77 0.087(8) 0.063(7) 0.040(5) 0.018(5) -0.014(5) 0.012(6) N15 0.030(4) 0.046(4) 0.052(4) 0.001(3) 0.005(3) 0.014(3) F11 0.203(8) 0.145(7) 0.080(5) 0.025(5) 0.052(5) 0.112(6) C8 0.034(5) 0.069(7) 0.067(6) 0.015(5) 0.032(4) 0.015(5) C19 0.073(7) 0.068(7) 0.052(6) 0.021(5) 0.007(5) 0.029(6) N30 0.056(5) 0.090(7) 0.043(4) 0.005(4) 0.006(4) 0.021(5) N34 0.079(6) 0.056(5) 0.034(4) 0.005(3) -0.005(4) 0.025(5) C109 0.086(8) 0.027(5) 0.050(5) 0.009(4) 0.010(5) 0.005(5) C26 0.053(6) 0.064(6) 0.036(4) 0.017(4) 0.003(4) 0.016(5) C81 0.070(7) 0.052(6) 0.030(4) -0.006(4) -0.008(4) 0.025(5) N26 0.077(6) 0.045(5) 0.047(4) 0.002(4) 0.025(4) 0.003(4) C102 0.107(9) 0.034(5) 0.046(5) 0.008(4) 0.011(5) 0.007(6) N20 0.076(6) 0.061(6) 0.047(5) 0.008(4) -0.013(4) 0.009(5) N24 0.072(5) 0.040(4) 0.040(4) 0.011(3) 0.000(4) 0.019(4) F44 0.138(7) 0.124(7) 0.089(5) 0.042(5) -0.012(5) -0.005(6) C73 0.082(8) 0.073(8) 0.038(5) 0.024(5) 0.004(5) -0.001(6) C68 0.078(7) 0.052(6) 0.036(5) 0.027(4) -0.004(4) 0.003(5) N6 0.041(4) 0.068(6) 0.061(5) 0.020(4) 0.000(4) 0.016(4) C80 0.075(7) 0.047(5) 0.034(4) 0.001(4) 0.000(4) 0.020(5) F29 0.064(5) 0.163(8) 0.118(6) -0.007(6) -0.017(4) 0.008(5) C85 0.052(6) 0.069(7) 0.041(5) 0.009(4) -0.002(4) 0.015(5) C95 0.110(10) 0.106(10) 0.042(6) -0.010(6) -0.006(6) 0.068(9) F32 0.167(7) 0.082(5) 0.043(3) 0.004(3) 0.006(4) -0.006(5) N21 0.107(8) 0.056(5) 0.039(4) 0.017(4) 0.000(4) 0.019(5) C60 0.084(8) 0.072(8) 0.051(6) 0.012(5) -0.006(5) 0.009(6) C82 0.064(7) 0.069(7) 0.056(6) 0.017(5) -0.001(5) 0.015(6) F43 0.153(8) 0.151(8) 0.092(6) 0.028(6) 0.036(5) -0.022(7) F46 0.122(7) 0.108(7) 0.145(8) -0.027(6) -0.027(6) 0.014(6) N29 0.097(8) 0.091(8) 0.062(6) 0.014(5) 0.025(5) 0.049(7) C69 0.075(8) 0.109(11) 0.058(7) 0.036(7) 0.009(6) -0.001(7) F33 0.159(7) 0.081(5) 0.057(4) 0.006(3) 0.027(4) -0.021(5) F36 0.118(6) 0.117(7) 0.112(6) -0.003(5) -0.007(5) 0.044(5) C25 0.054(6) 0.065(7) 0.051(5) 0.012(5) 0.015(4) 0.015(5) C48 0.038(5) 0.063(6) 0.072(6) 0.024(5) 0.019(4) 0.030(5) C55 0.039(5) 0.057(6) 0.054(5) 0.011(4) 0.007(4) 0.020(4) F48 0.090(6) 0.143(8) 0.145(7) -0.009(6) -0.021(5) 0.046(5) C17 0.054(6) 0.079(7) 0.034(5) 0.024(5) 0.008(4) 0.011(5) F18 0.184(8) 0.163(8) 0.094(5) 0.031(5) 0.017(5) 0.125(7) C71 0.080(8) 0.068(7) 0.040(5) 0.020(5) 0.002(5) 0.014(6) C88 0.060(7) 0.143(13) 0.064(7) 0.036(7) 0.014(5) 0.049(8) C56 0.039(5) 0.084(8) 0.063(6) 0.038(6) 0.029(4) 0.025(5) C76 0.085(8) 0.055(6) 0.032(4) 0.011(4) -0.001(5) 0.016(6) C18 0.053(6) 0.090(8) 0.042(5) 0.027(5) 0.003(4) 0.031(6) C39 0.040(5) 0.065(6) 0.048(5) 0.006(4) 0.009(4) 0.029(5) C114 0.080(7) 0.039(5) 0.044(5) 0.022(4) 0.003(5) -0.005(5) N19 0.076(7) 0.040(5) 0.101(7) 0.029(5) -0.024(6) -0.007(5) C101 0.098(8) 0.047(6) 0.032(4) 0.006(4) 0.012(5) 0.015(6) C79 0.079(7) 0.046(5) 0.038(5) 0.004(4) -0.001(4) 0.027(5) F27 0.066(5) 0.140(8) 0.163(8) 0.025(6) 0.020(5) 0.013(5) C100 0.088(8) 0.038(5) 0.052(5) 0.016(4) 0.011(5) 0.002(5) F4 0.178(8) 0.148(8) 0.065(5) 0.000(5) 0.020(5) 0.029(7) C99 0.093(9) 0.077(9) 0.053(6) 0.022(6) 0.016(6) 0.007(7) C42 0.044(5) 0.038(5) 0.043(4) 0.001(4) 0.010(4) 0.018(4) C84 0.091(8) 0.072(7) 0.042(5) 0.021(5) 0.013(5) 0.037(6) C110 0.119(9) 0.031(5) 0.026(4) 0.002(3) 0.012(5) 0.019(5) C83 0.066(7) 0.082(8) 0.046(5) 0.011(5) -0.011(5) 0.030(6) C54 0.047(6) 0.064(7) 0.082(7) 0.029(6) 0.014(5) 0.021(5) C13 0.056(6) 0.077(7) 0.044(5) 0.013(5) -0.002(4) 0.021(5) C43 0.042(5) 0.064(6) 0.056(5) 0.012(5) 0.012(4) 0.028(5) C10 0.059(6) 0.072(7) 0.056(6) 0.020(5) 0.007(5) 0.024(6) F3 0.213(10) 0.107(7) 0.133(7) 0.049(6) 0.040(7) -0.005(7) F30 0.114(7) 0.188(10) 0.163(9) -0.040(7) 0.040(6) 0.046(7) C89 0.092(9) 0.060(7) 0.082(8) 0.004(6) 0.052(7) 0.026(7) F2 0.192(9) 0.194(10) 0.115(7) 0.025(7) 0.014(7) 0.122(8) C87 0.052(6) 0.055(6) 0.070(7) 0.004(5) -0.002(5) -0.001(5) F5 0.140(8) 0.217(11) 0.124(7) 0.018(7) 0.008(6) 0.066(8) C90 0.052(6) 0.081(8) 0.059(6) 0.012(6) 0.002(5) 0.005(6) C63 0.105(9) 0.069(8) 0.053(6) 0.019(5) 0.017(6) 0.030(7) F19 0.096(6) 0.206(10) 0.193(9) 0.040(8) -0.002(6) 0.090(7) C72 0.094(9) 0.068(7) 0.060(6) 0.042(6) 0.014(6) 0.026(6) C78 0.136(12) 0.096(10) 0.034(5) 0.012(5) -0.010(6) 0.052(9) C70 0.085(8) 0.100(10) 0.040(5) 0.041(6) 0.011(5) 0.014(7) C116 0.080(8) 0.060(7) 0.053(6) 0.008(5) 0.026(5) 0.005(6) C112 0.096(9) 0.053(7) 0.056(6) 0.008(5) -0.008(6) 0.016(6) C111 0.057(6) 0.051(6) 0.043(5) -0.002(4) 0.008(4) -0.001(5) N28 0.184(13) 0.097(9) 0.064(6) 0.042(6) 0.051(7) 0.075(10) F15 0.175(8) 0.247(11) 0.095(6) 0.035(7) 0.027(6) 0.123(8) C97 0.092(9) 0.052(7) 0.061(6) 0.012(5) 0.024(6) -0.010(6) C62 0.130(12) 0.098(10) 0.042(6) 0.026(6) 0.019(6) 0.046(9) C64 0.082(9) 0.064(8) 0.091(9) 0.019(7) -0.023(7) 0.022(7) C92 0.068(7) 0.104(10) 0.048(6) 0.011(6) 0.008(5) 0.033(7) C61 0.128(11) 0.110(11) 0.042(6) 0.035(6) 0.008(6) 0.065(9) N25 0.147(12) 0.018(5) 0.191(15) 0.005(6) -0.016(10) 0.011(6) C65 0.124(13) 0.084(11) 0.141(14) -0.002(9) -0.020(11) 0.078(11) F16 0.153(8) 0.302(12) 0.097(6) 0.033(8) -0.014(6) 0.117(9) C98 0.097(9) 0.070(8) 0.059(7) 0.003(6) 0.012(6) 0.012(7) C113 0.094(9) 0.037(6) 0.108(10) 0.000(6) -0.008(7) 0.022(6) C108 0.116(11) 0.031(6) 0.109(10) -0.005(6) 0.002(8) 0.007(7) C67 0.106(11) 0.051(8) 0.182(16) 0.055(9) 0.008(11) 0.033(8) F28 0.111(7) 0.178(10) 0.222(11) 0.071(9) -0.021(7) 0.026(7) F47 0.205(10) 0.139(9) 0.188(10) 0.082(8) -0.020(9) -0.045(8) F20 0.140(8) 0.192(11) 0.225(11) 0.008(9) 0.090(8) 0.047(8) C105 0.109(11) 0.040(7) 0.104(10) 0.010(6) 0.010(8) -0.001(7) C103 0.120(12) 0.052(7) 0.098(10) 0.003(6) -0.016(8) 0.038(8) F25 0.157(9) 0.185(11) 0.211(11) 0.009(9) -0.017(8) 0.072(8) F6 0.226(11) 0.152(10) 0.146(9) -0.024(7) 0.053(8) -0.008(9) F45 0.104(7) 0.182(10) 0.216(11) 0.001(9) 0.029(7) 0.040(7) F17 0.279(11) 0.150(8) 0.175(9) -0.024(7) 0.014(9) 0.137(8) F23 0.181(10) 0.131(9) 0.240(12) -0.043(9) 0.062(9) 0.016(8) C94 0.23(2) 0.115(14) 0.086(11) 0.055(11) 0.050(13) 0.096(16) F12 0.153(8) 0.220(10) 0.203(10) 0.015(9) 0.004(7) 0.139(8) C96 0.159(16) 0.071(10) 0.101(11) 0.009(8) -0.014(11) 0.017(10) C104 0.126(12) 0.020(5) 0.124(11) 0.018(6) 0.007(9) -0.005(7) F26 0.054(4) 0.282(12) 0.157(8) -0.060(8) 0.009(5) 0.065(6) F10 0.265(12) 0.163(10) 0.206(11) 0.053(9) 0.107(10) 0.053(10) C106 0.149(8) 0.149(8) 0.149(8) 0.0258(17) 0.0290(18) 0.052(3) F8 0.278(13) 0.158(11) 0.209(12) -0.011(10) 0.028(11) 0.036(11) F22 0.142(9) 0.250(13) 0.258(12) 0.031(11) 0.060(9) 0.096(9) F9 0.324(13) 0.214(11) 0.121(8) -0.005(8) 0.070(9) 0.127(10) F21 0.178(11) 0.192(12) 0.255(13) -0.046(11) 0.024(10) 0.010(10) F7 0.238(11) 0.195(10) 0.177(10) -0.021(8) -0.071(9) 0.141(9) F24 0.208(11) 0.208(12) 0.243(12) 0.061(10) 0.048(10) 0.083(10) N35 0.063(6) 0.076(6) 0.045(5) 0.030(4) 0.001(4) -0.009(5) N17 0.040(4) 0.062(5) 0.072(5) 0.027(4) 0.021(4) 0.022(4) C107 0.27(3) 0.32(4) 0.22(3) 0.16(3) 0.15(3) 0.25(3) F13 0.162(9) 0.200(10) 0.120(7) 0.024(7) -0.053(7) 0.068(8) N36 0.064(5) 0.050(5) 0.036(4) 0.022(3) 0.002(4) -0.009(4) P7 0.241(8) 0.089(4) 0.163(5) 0.017(4) -0.005(5) 0.056(4) F41 0.245(11) 0.130(8) 0.147(8) 0.033(7) -0.014(8) 0.082(8) F40 0.259(12) 0.107(8) 0.152(9) 0.034(7) -0.014(9) 0.033(8) F39 0.299(13) 0.163(10) 0.154(9) -0.004(8) 0.005(10) 0.087(10) F37 0.269(12) 0.159(9) 0.143(9) -0.036(7) 0.006(9) 0.091(9) F38 0.261(12) 0.147(10) 0.230(12) 0.034(9) -0.022(11) 0.026(10) F42 0.240(11) 0.127(8) 0.125(7) 0.012(6) -0.011(8) 0.084(8) N16 0.061(5) 0.052(5) 0.074(5) 0.027(4) 0.014(4) 0.032(4) N7 0.091(7) 0.091(7) 0.031(4) 0.024(4) 0.005(4) 0.040(6) N13 0.093(7) 0.096(8) 0.045(5) -0.009(5) -0.007(4) 0.060(6) C41 0.050(5) 0.043(5) 0.072(6) 0.003(4) 0.027(5) 0.021(4) N4 0.069(6) 0.078(7) 0.089(7) 0.044(6) 0.024(5) 0.040(5) N2 0.072(3) 0.073(3) 0.071(3) 0.0122(11) 0.0147(11) 0.0253(13) N11 0.134(10) 0.095(8) 0.050(5) -0.027(5) -0.018(5) 0.087(8) C45 0.053(6) 0.058(6) 0.069(6) 0.020(5) 0.008(5) 0.035(5) N3 0.068(6) 0.072(7) 0.077(6) 0.007(5) 0.038(5) 0.012(5) N10 0.102(8) 0.076(7) 0.073(6) -0.027(5) -0.057(6) 0.047(6) C51 0.047(5) 0.042(5) 0.068(6) 0.023(4) 0.014(4) 0.015(4) N1 0.093(8) 0.143(11) 0.061(6) 0.051(7) 0.041(5) 0.072(8) C28 0.065(7) 0.084(8) 0.058(6) 0.026(6) 0.016(5) 0.015(6) C46 0.054(6) 0.050(6) 0.064(6) 0.027(5) 0.019(4) 0.028(5) C23 0.070(7) 0.081(8) 0.043(5) 0.031(5) 0.019(5) 0.029(6) N12 0.145(10) 0.101(8) 0.042(5) -0.012(5) -0.007(5) 0.088(8) C20 0.069(7) 0.061(6) 0.041(5) 0.015(4) 0.009(4) 0.019(5) C52 0.045(6) 0.054(6) 0.100(8) 0.044(6) 0.024(5) 0.022(5) C24 0.072(7) 0.058(7) 0.051(6) -0.001(5) 0.001(5) 0.018(6) C49 0.069(7) 0.047(6) 0.078(7) 0.027(5) 0.011(5) 0.035(5) C16 0.060(7) 0.105(9) 0.038(5) 0.024(5) 0.008(4) 0.018(6) C40 0.050(6) 0.080(8) 0.061(6) 0.002(5) 0.016(4) 0.034(6) C44 0.047(6) 0.075(7) 0.063(6) 0.014(5) 0.018(4) 0.034(5) C58 0.026(5) 0.081(8) 0.085(7) 0.031(6) 0.012(5) 0.013(5) C53 0.059(6) 0.058(7) 0.083(7) 0.038(6) 0.016(5) 0.012(5) C7 0.127(12) 0.054(7) 0.119(11) 0.010(7) 0.081(10) 0.041(8) C57 0.036(5) 0.065(7) 0.099(8) 0.025(6) 0.013(5) 0.012(5) C9 0.091(9) 0.108(11) 0.103(10) 0.035(8) 0.056(8) 0.064(9) C29 0.057(6) 0.072(8) 0.071(7) 0.005(6) 0.012(5) 0.018(6) C31 0.118(12) 0.114(13) 0.119(12) -0.087(11) -0.082(10) 0.097(11) C430 0.079(9) 0.101(10) 0.087(9) 0.036(8) -0.015(7) 0.039(8) C15 0.061(7) 0.098(9) 0.061(6) 0.040(6) 0.001(5) 0.025(6) C432 0.039(6) 0.137(13) 0.091(9) 0.062(9) 0.013(6) 0.024(7) C34 0.138(13) 0.159(15) 0.054(7) -0.014(8) 0.012(7) 0.111(13) C35 0.099(10) 0.122(12) 0.051(6) -0.022(7) 0.009(6) 0.058(9) C6 0.065(7) 0.077(9) 0.088(8) 0.009(7) 0.027(6) 0.020(6) C3 0.089(4) 0.090(4) 0.089(4) 0.0158(12) 0.0177(13) 0.0313(16) C36 0.145(14) 0.155(15) 0.067(8) 0.009(8) 0.013(8) 0.116(13) C5 0.043(6) 0.141(13) 0.091(9) -0.017(8) 0.007(6) 0.037(8) C21 0.162(14) 0.129(12) 0.039(6) 0.030(7) 0.025(7) 0.101(12) C37 0.083(9) 0.094(10) 0.111(11) 0.013(8) 0.000(8) 0.054(8) C14 0.060(7) 0.102(10) 0.072(7) 0.023(7) -0.011(5) 0.037(7) C50 0.088(11) 0.136(16) 0.116(13) 0.022(11) 0.022(9) 0.030(10) C30 0.068(8) 0.048(7) 0.160(14) 0.012(8) -0.039(9) 0.008(6) C2 0.126(12) 0.094(11) 0.121(12) 0.060(9) 0.071(10) 0.061(10) C32 0.138(16) 0.111(14) 0.104(12) -0.026(10) -0.023(11) 0.071(13) C22 0.180(18) 0.094(11) 0.058(8) -0.005(7) 0.034(9) -0.027(11) C4 0.089(4) 0.090(4) 0.089(4) 0.0160(12) 0.0175(13) 0.0314(16) _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 C1 1.9611 . ? Pd1 C8 1.9876 . ? Pd1 N18 2.0678 . ? Pd1 N5 2.0844 . ? Pd2 C91 1.9728 . ? Pd2 C95 1.9978 . ? Pd2 N32 2.0855 . ? Pd2 N27 2.1128 . ? Pd3 C59 1.9456 . ? Pd3 C66 2.0077 . ? Pd3 N23 2.0710 . ? Pd3 N36 2.0719 . ? Pd4 C38 1.9577 . ? Pd4 C33 1.9725 . ? Pd4 N9 2.0281 . ? Pd4 N14 2.0654 . ? P1 F1 1.5828 . ? P1 F4 1.5831 . ? P1 F2 1.5832 . ? P1 F3 1.5834 . ? P1 F6 1.5835 . ? P1 F5 1.5836 . ? P2 F10 1.5800 . ? P2 F8 1.5803 . ? P2 F9 1.5829 . ? P2 F12 1.5831 . ? P2 F7 1.5832 . ? P2 F11 1.5833 . ? P6 F35 1.5799 . ? P6 F32 1.5800 . ? P6 F34 1.5801 . ? P6 F33 1.5801 . ? P6 F31 1.5802 . ? P6 F36 1.5803 . ? P3 F15 1.5819 . ? P3 F13 1.5819 . ? P3 F16 1.5819 . ? P3 F18 1.5821 . ? P3 F17 1.5836 . ? P3 F14 1.5841 . ? N5 C10 1.3511 . ? N5 C432 1.3821 . ? P8 F48 1.5815 . ? P8 F46 1.5818 . ? P8 F43 1.5821 . ? P8 F45 1.5823 . ? P8 F47 1.5837 . ? P8 F44 1.5842 . ? C59 N22 1.3597 . ? C59 N21 1.3660 . ? N23 C114 1.3009 . ? N23 C116 1.3587 . ? N14 C39 1.3515 . ? N14 C40 1.4201 . ? P5 F25 1.5818 . ? P5 F30 1.5818 . ? P5 F26 1.5821 . ? P5 F28 1.5821 . ? P5 F29 1.5837 . ? P5 F27 1.5844 . ? P4 F21 1.5799 . ? P4 F24 1.5799 . ? P4 F19 1.5800 . ? P4 F20 1.5800 . ? P4 F23 1.5801 . ? P4 F22 1.5806 . ? N32 C85 1.3102 . ? N32 C87 1.3436 . ? N9 C29 1.3956 . ? N9 C27 1.3992 . ? N18 C56 1.3004 . ? N18 C58 1.3395 . ? C66 N19 1.2694 . ? C66 N20 1.3114 . ? N8 C27 1.3216 . ? N8 C25 1.3979 . ? N8 C28 1.4535 . ? C1 N1 1.3216 . ? C1 N2 1.3901 . ? N33 C86 1.3105 . ? N33 C85 1.3255 . ? N33 C82 1.3457 . ? C38 N13 1.2995 . ? C38 N12 1.4616 . ? C47 C42 1.2904 . ? C47 C46 1.4268 . ? C47 C48 1.4697 . ? C86 C87 1.3501 . ? N27 C99 1.2859 . ? N27 C98 1.3461 . ? C115 C116 1.3489 . ? C115 N24 1.4098 . ? C93 C94 1.1830 . ? C93 N29 1.3825 . ? C91 N31 1.3073 . ? C91 N30 1.3299 . ? C33 N10 1.2653 . ? C33 N11 1.4114 . ? C74 C75 1.3897 . ? C74 C73 1.4500 . ? C75 C76 1.3561 . ? C75 C80 1.4110 . ? N31 C89 1.4280 . ? N31 C88 1.4695 . ? N22 C61 1.3045 . ? N22 C60 1.5781 . ? C77 N34 1.4390 . ? C77 C78 1.6243 . ? N15 C39 1.3701 . ? N15 C43 1.3966 . ? N15 C41 1.4390 . ? C8 N4 1.3164 . ? C8 N3 1.4379 . ? C19 C26 1.3801 . ? C19 C20 1.4150 . ? C19 C17 1.4320 . ? N30 C92 1.4561 . ? N30 C90 1.4641 . ? N34 C76 1.3494 . ? N34 C79 1.3946 . ? C109 C102 1.3791 . ? C109 C108 1.3863 . ? C109 C110 1.4365 . ? C26 C25 1.4318 . ? C81 C82 1.3730 . ? C81 C80 1.3839 . ? N26 C99 1.3288 . ? N26 C97 1.4458 . ? N26 C100 1.4849 . ? C102 C103 1.3743 . ? C102 C101 1.4255 . ? N20 C64 1.4029 . ? N20 C63 1.4719 . ? N24 C114 1.3254 . ? N24 C111 1.4237 . ? C73 N35 1.3784 . ? C73 C72 1.3855 . ? C68 N36 1.2951 . ? C68 N35 1.3050 . ? N6 C10 1.3291 . ? N6 C430 1.3884 . ? N6 C13 1.3926 . ? C80 C79 1.3920 . ? C95 N29 1.3012 . ? C95 N28 1.3958 . ? N21 C62 1.3492 . ? N21 C63 1.4589 . ? C82 C83 1.5152 . ? N29 C92 1.4320 . ? C69 C70 1.3713 . ? C69 N36 1.3783 . ? C25 C24 1.4089 . ? C48 C55 1.4151 . ? C48 C51 1.4256 . ? C55 C54 1.3818 . ? C17 C18 1.3728 . ? C17 C16 1.4005 . ? C71 C72 1.2247 . ? C71 C76 1.4027 . ? C56 N17 1.4031 . ? C18 C13 1.4040 . ? N19 C67 1.3742 . ? N19 C65 1.4625 . ? C101 C100 1.3456 . ? C79 C84 1.4046 . ? C100 C105 1.3789 . ? C42 C43 1.4052 . ? C84 C83 1.3065 . ? C110 C111 1.2769 . ? C54 N17 1.3557 . ? C54 C53 1.3773 . ? C13 C14 1.4214 . ? C43 C44 1.3673 . ? C89 C90 1.2518 . ? C70 N35 1.3462 . ? C112 C113 1.3997 . ? C112 C111 1.4370 . ? N28 C96 1.4902 . ? N28 C94 1.5050 . ? C97 C98 1.4174 . ? C62 C61 1.4526 . ? C64 C65 1.2132 . ? N25 C103 1.3455 . ? N25 C106 1.4004 . ? N25 C108 1.4711 . ? C113 C108 1.3161 . ? C105 C104 1.4203 . ? C103 C104 1.3843 . ? C106 C107 1.4497 . ? N17 C57 1.4018 . ? P7 F37 1.5829 . ? P7 F39 1.5829 . ? P7 F38 1.5833 . ? P7 F42 1.5833 . ? P7 F41 1.5835 . ? P7 F40 1.5836 . ? N16 C46 1.3515 . ? N16 C51 1.3517 . ? N16 C49 1.5509 . ? N7 C16 1.3654 . ? N7 C20 1.3815 . ? N7 C21 1.5326 . ? N13 C36 1.4053 . ? N13 C37 1.4832 . ? C41 C40 1.3188 . ? N4 C7 1.3222 . ? N4 C9 1.4870 . ? N2 C5 1.3931 . ? N2 C4 1.4631 . ? N11 C32 1.3298 . ? N11 C34 1.4981 . ? C45 C46 1.3590 . ? C45 C44 1.4147 . ? N3 C6 1.3149 . ? N3 C5 1.4355 . ? N10 C31 1.4734 . ? N10 C30 1.5232 . ? C51 C52 1.4033 . ? N1 C3 1.3282 . ? N1 C2 1.5233 . ? C28 C29 1.3156 . ? C23 C20 1.3549 . ? C23 C24 1.4102 . ? N12 C35 1.3917 . ? N12 C34 1.3994 . ? C52 C53 1.3591 . ? C49 C50 1.4417 . ? C16 C15 1.4350 . ? C58 C57 1.3366 . ? C7 C6 1.3583 . ? C31 C32 1.2832 . ? C430 C432 1.3417 . ? C15 C14 1.4449 . ? C35 C36 1.3077 . ? C3 C4 1.3315 . ? C21 C22 1.5645 . ? 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 C1 Pd1 C8 84.4 . . ? C1 Pd1 N18 93.2 . . ? C8 Pd1 N18 175.6 . . ? C1 Pd1 N5 174.8 . . ? C8 Pd1 N5 93.3 . . ? N18 Pd1 N5 88.8 . . ? C91 Pd2 C95 84.1 . . ? C91 Pd2 N32 93.2 . . ? C95 Pd2 N32 175.1 . . ? C91 Pd2 N27 171.2 . . ? C95 Pd2 N27 91.3 . . ? N32 Pd2 N27 90.8 . . ? C59 Pd3 C66 82.9 . . ? C59 Pd3 N23 95.5 . . ? C66 Pd3 N23 174.4 . . ? C59 Pd3 N36 173.6 . . ? C66 Pd3 N36 92.8 . . ? N23 Pd3 N36 88.3 . . ? C38 Pd4 C33 86.5 . . ? C38 Pd4 N9 176.8 . . ? C33 Pd4 N9 93.8 . . ? C38 Pd4 N14 89.4 . . ? C33 Pd4 N14 173.7 . . ? N9 Pd4 N14 90.0 . . ? F1 P1 F4 180.0 . . ? F1 P1 F2 90.0 . . ? F4 P1 F2 90.0 . . ? F1 P1 F3 90.0 . . ? F4 P1 F3 90.0 . . ? F2 P1 F3 90.0 . . ? F1 P1 F6 90.0 . . ? F4 P1 F6 90.0 . . ? F2 P1 F6 90.0 . . ? F3 P1 F6 180.0 . . ? F1 P1 F5 90.0 . . ? F4 P1 F5 90.0 . . ? F2 P1 F5 180.0 . . ? F3 P1 F5 90.0 . . ? F6 P1 F5 90.0 . . ? F10 P2 F8 169.8 . . ? F10 P2 F9 90.2 . . ? F8 P2 F9 97.2 . . ? F10 P2 F12 90.2 . . ? F8 P2 F12 82.8 . . ? F9 P2 F12 90.0 . . ? F10 P2 F7 90.2 . . ? F8 P2 F7 96.9 . . ? F9 P2 F7 90.0 . . ? F12 P2 F7 179.7 . . ? F10 P2 F11 90.2 . . ? F8 P2 F11 82.5 . . ? F9 P2 F11 179.7 . . ? F12 P2 F11 90.0 . . ? F7 P2 F11 90.0 . . ? F35 P6 F32 92.8 . . ? F35 P6 F34 87.9 . . ? F32 P6 F34 179.2 . . ? F35 P6 F33 89.9 . . ? F32 P6 F33 89.5 . . ? F34 P6 F33 91.0 . . ? F35 P6 F31 85.1 . . ? F32 P6 F31 90.2 . . ? F34 P6 F31 89.3 . . ? F33 P6 F31 174.9 . . ? F35 P6 F36 177.9 . . ? F32 P6 F36 89.0 . . ? F34 P6 F36 90.4 . . ? F33 P6 F36 89.1 . . ? F31 P6 F36 96.0 . . ? F15 P3 F13 88.4 . . ? F15 P3 F16 87.9 . . ? F13 P3 F16 176.3 . . ? F15 P3 F18 179.2 . . ? F13 P3 F18 92.4 . . ? F16 P3 F18 91.3 . . ? F15 P3 F17 90.0 . . ? F13 P3 F17 90.0 . . ? F16 P3 F17 90.0 . . ? F18 P3 F17 90.0 . . ? F15 P3 F14 90.0 . . ? F13 P3 F14 90.0 . . ? F16 P3 F14 90.0 . . ? F18 P3 F14 90.0 . . ? F17 P3 F14 180.0 . . ? C10 N5 C432 106.3 . . ? C10 N5 Pd1 123.1 . . ? C432 N5 Pd1 129.4 . . ? F48 P8 F46 92.0 . . ? F48 P8 F43 81.5 . . ? F46 P8 F43 173.5 . . ? F48 P8 F45 175.7 . . ? F46 P8 F45 83.7 . . ? F43 P8 F45 102.8 . . ? F48 P8 F47 90.0 . . ? F46 P8 F47 90.0 . . ? F43 P8 F47 90.0 . . ? F45 P8 F47 90.0 . . ? F48 P8 F44 90.0 . . ? F46 P8 F44 90.0 . . ? F43 P8 F44 90.0 . . ? F45 P8 F44 90.0 . . ? F47 P8 F44 179.9 . . ? N22 C59 N21 101.4 . . ? N22 C59 Pd3 136.0 . . ? N21 C59 Pd3 122.5 . . ? C114 N23 C116 105.9 . . ? C114 N23 Pd3 122.9 . . ? C116 N23 Pd3 131.1 . . ? C39 N14 C40 105.9 . . ? C39 N14 Pd4 118.0 . . ? C40 N14 Pd4 135.6 . . ? F25 P5 F30 80.0 . . ? F25 P5 F26 91.5 . . ? F30 P5 F26 171.5 . . ? F25 P5 F28 172.6 . . ? F30 P5 F28 92.5 . . ? F26 P5 F28 96.0 . . ? F25 P5 F29 90.0 . . ? F30 P5 F29 90.0 . . ? F26 P5 F29 90.0 . . ? F28 P5 F29 90.0 . . ? F25 P5 F27 90.0 . . ? F30 P5 F27 90.0 . . ? F26 P5 F27 90.0 . . ? F28 P5 F27 90.0 . . ? F29 P5 F27 180.0 . . ? F21 P4 F24 90.3 . . ? F21 P4 F19 90.3 . . ? F24 P4 F19 90.3 . . ? F21 P4 F20 90.3 . . ? F24 P4 F20 90.3 . . ? F19 P4 F20 179.2 . . ? F21 P4 F23 179.2 . . ? F24 P4 F23 90.3 . . ? F19 P4 F23 89.1 . . ? F20 P4 F23 90.3 . . ? F21 P4 F22 70.6 . . ? F24 P4 F22 160.7 . . ? F19 P4 F22 87.2 . . ? F20 P4 F22 92.4 . . ? F23 P4 F22 108.8 . . ? C85 N32 C87 102.2 . . ? C85 N32 Pd2 124.0 . . ? C87 N32 Pd2 133.4 . . ? C29 N9 C27 103.2 . . ? C29 N9 Pd4 133.2 . . ? C27 N9 Pd4 122.7 . . ? C56 N18 C58 108.7 . . ? C56 N18 Pd1 118.9 . . ? C58 N18 Pd1 132.2 . . ? N19 C66 N20 106.6 . . ? N19 C66 Pd3 133.5 . . ? N20 C66 Pd3 119.9 . . ? C27 N8 C25 127.9 . . ? C27 N8 C28 106.7 . . ? C25 N8 C28 124.9 . . ? N1 C1 N2 104.1 . . ? N1 C1 Pd1 134.0 . . ? N2 C1 Pd1 121.8 . . ? C86 N33 C85 106.5 . . ? C86 N33 C82 125.3 . . ? C85 N33 C82 127.8 . . ? N13 C38 N12 105.3 . . ? N13 C38 Pd4 135.5 . . ? N12 C38 Pd4 119.2 . . ? C42 C47 C46 119.2 . . ? C42 C47 C48 133.3 . . ? C46 C47 C48 107.6 . . ? N33 C86 C87 106.3 . . ? N8 C27 N9 111.6 . . ? C99 N27 C98 109.1 . . ? C99 N27 Pd2 115.5 . . ? C98 N27 Pd2 134.2 . . ? C116 C115 N24 106.1 . . ? C94 C93 N29 117.2 . . ? N31 C91 N30 107.0 . . ? N31 C91 Pd2 134.5 . . ? N30 C91 Pd2 118.5 . . ? N10 C33 N11 101.3 . . ? N10 C33 Pd4 137.0 . . ? N11 C33 Pd4 120.5 . . ? C75 C74 C73 119.1 . . ? C76 C75 C74 119.1 . . ? C76 C75 C80 107.2 . . ? C74 C75 C80 133.6 . . ? C91 N31 C89 108.1 . . ? C91 N31 C88 123.1 . . ? C89 N31 C88 128.5 . . ? C61 N22 C59 116.3 . . ? C61 N22 C60 122.8 . . ? C59 N22 C60 121.0 . . ? N34 C77 C78 111.6 . . ? C39 N15 C43 125.7 . . ? C39 N15 C41 107.2 . . ? C43 N15 C41 126.8 . . ? N4 C8 N3 100.7 . . ? N4 C8 Pd1 139.0 . . ? N3 C8 Pd1 120.3 . . ? C26 C19 C20 120.5 . . ? C26 C19 C17 130.1 . . ? C20 C19 C17 109.0 . . ? C91 N30 C92 123.6 . . ? C91 N30 C90 109.7 . . ? C92 N30 C90 126.3 . . ? C76 N34 C79 105.9 . . ? C76 N34 C77 128.5 . . ? C79 N34 C77 124.7 . . ? C102 C109 C108 109.8 . . ? C102 C109 C110 137.0 . . ? C108 C109 C110 113.2 . . ? C19 C26 C25 115.6 . . ? C82 C81 C80 123.0 . . ? C99 N26 C97 108.5 . . ? C99 N26 C100 127.7 . . ? C97 N26 C100 123.7 . . ? C103 C102 C109 109.5 . . ? C103 C102 C101 117.4 . . ? C109 C102 C101 132.9 . . ? C66 N20 C64 112.0 . . ? C66 N20 C63 125.1 . . ? C64 N20 C63 122.8 . . ? C114 N24 C115 104.8 . . ? C114 N24 C111 127.5 . . ? C115 N24 C111 127.6 . . ? N35 C73 C72 129.5 . . ? N35 C73 C74 115.7 . . ? C72 C73 C74 114.8 . . ? N36 C68 N35 114.8 . . ? C10 N6 C430 108.0 . . ? C10 N6 C13 124.5 . . ? C430 N6 C13 127.3 . . ? C81 C80 C79 120.2 . . ? C81 C80 C75 133.8 . . ? C79 C80 C75 105.7 . . ? N32 C85 N33 113.5 . . ? N29 C95 N28 111.3 . . ? N29 C95 Pd2 119.0 . . ? N28 C95 Pd2 129.2 . . ? C62 N21 C59 113.6 . . ? C62 N21 C63 124.5 . . ? C59 N21 C63 121.6 . . ? N33 C82 C81 125.2 . . ? N33 C82 C83 122.3 . . ? C81 C82 C83 112.2 . . ? C95 N29 C93 104.1 . . ? C95 N29 C92 123.5 . . ? C93 N29 C92 132.3 . . ? C70 C69 N36 104.7 . . ? N8 C25 C24 119.8 . . ? N8 C25 C26 116.5 . . ? C24 C25 C26 123.5 . . ? C55 C48 C51 121.2 . . ? C55 C48 C47 133.2 . . ? C51 C48 C47 105.6 . . ? C54 C55 C48 117.4 . . ? C18 C17 C16 122.2 . . ? C18 C17 C19 133.0 . . ? C16 C17 C19 104.8 . . ? C72 C71 C76 120.4 . . ? N18 C56 N17 111.2 . . ? N34 C76 C75 111.7 . . ? N34 C76 C71 128.0 . . ? C75 C76 C71 120.2 . . ? C17 C18 C13 119.0 . . ? N14 C39 N15 109.7 . . ? N23 C114 N24 113.5 . . ? C66 N19 C67 128.4 . . ? C66 N19 C65 105.9 . . ? C67 N19 C65 125.4 . . ? C100 C101 C102 116.1 . . ? C80 C79 N34 109.5 . . ? C80 C79 C84 120.9 . . ? N34 C79 C84 129.4 . . ? C101 C100 C105 127.8 . . ? C101 C100 N26 116.2 . . ? C105 C100 N26 115.9 . . ? N27 C99 N26 111.2 . . ? C47 C42 C43 120.7 . . ? C83 C84 C79 117.3 . . ? C111 C110 C109 122.3 . . ? C84 C83 C82 125.5 . . ? N17 C54 C53 122.4 . . ? N17 C54 C55 116.6 . . ? C53 C54 C55 120.4 . . ? N6 C13 C18 119.9 . . ? N6 C13 C14 118.1 . . ? C18 C13 C14 122.0 . . ? C44 C43 N15 116.7 . . ? C44 C43 C42 122.0 . . ? N15 C43 C42 121.3 . . ? N6 C10 N5 109.9 . . ? C90 C89 N31 111.1 . . ? N32 C87 C86 111.2 . . ? C89 C90 N30 103.9 . . ? N21 C63 N20 104.8 . . ? C71 C72 C73 126.2 . . ? N35 C70 C69 110.2 . . ? C115 C116 N23 109.6 . . ? C113 C112 C111 113.6 . . ? C110 C111 N24 121.2 . . ? C110 C111 C112 123.9 . . ? N24 C111 C112 114.8 . . ? C95 N28 C96 127.9 . . ? C95 N28 C94 101.8 . . ? C96 N28 C94 129.7 . . ? C98 C97 N26 101.0 . . ? N21 C62 C61 104.3 . . ? C65 C64 N20 103.5 . . ? N29 C92 N30 105.9 . . ? N22 C61 C62 104.2 . . ? C103 N25 C106 133.6 . . ? C103 N25 C108 110.1 . . ? C106 N25 C108 115.9 . . ? C64 C65 N19 110.5 . . ? N27 C98 C97 109.7 . . ? C108 C113 C112 121.5 . . ? C113 C108 C109 124.8 . . ? C113 C108 N25 130.9 . . ? C109 C108 N25 103.0 . . ? C100 C105 C104 115.0 . . ? N25 C103 C102 107.2 . . ? N25 C103 C104 126.2 . . ? C102 C103 C104 124.8 . . ? C93 C94 N28 105.4 . . ? C103 C104 C105 116.6 . . ? N25 C106 C107 107.8 . . ? C68 N35 C70 103.9 . . ? C68 N35 C73 132.2 . . ? C70 N35 C73 123.6 . . ? C54 N17 C57 129.1 . . ? C54 N17 C56 128.7 . . ? C57 N17 C56 101.9 . . ? C68 N36 C69 106.1 . . ? C68 N36 Pd3 120.6 . . ? C69 N36 Pd3 132.1 . . ? F37 P7 F39 180.0 . . ? F37 P7 F38 90.0 . . ? F39 P7 F38 90.0 . . ? F37 P7 F42 90.0 . . ? F39 P7 F42 90.0 . . ? F38 P7 F42 90.0 . . ? F37 P7 F41 90.0 . . ? F39 P7 F41 90.0 . . ? F38 P7 F41 90.0 . . ? F42 P7 F41 180.0 . . ? F37 P7 F40 90.0 . . ? F39 P7 F40 90.0 . . ? F38 P7 F40 180.0 . . ? F42 P7 F40 90.0 . . ? F41 P7 F40 90.0 . . ? C46 N16 C51 115.4 . . ? C46 N16 C49 123.8 . . ? C51 N16 C49 120.3 . . ? C16 N7 C20 110.1 . . ? C16 N7 C21 127.1 . . ? C20 N7 C21 122.6 . . ? C38 N13 C36 111.0 . . ? C38 N13 C37 126.0 . . ? C36 N13 C37 123.0 . . ? C40 C41 N15 106.2 . . ? C8 N4 C7 115.0 . . ? C8 N4 C9 116.4 . . ? C7 N4 C9 127.7 . . ? C1 N2 C5 123.3 . . ? C1 N2 C4 107.2 . . ? C5 N2 C4 129.5 . . ? C32 N11 C33 119.2 . . ? C32 N11 C34 120.6 . . ? C33 N11 C34 119.8 . . ? C46 C45 C44 118.8 . . ? C6 N3 C5 127.5 . . ? C6 N3 C8 110.5 . . ? C5 N3 C8 121.4 . . ? C33 N10 C31 106.8 . . ? C33 N10 C30 123.9 . . ? C31 N10 C30 128.7 . . ? N16 C51 C52 134.5 . . ? N16 C51 C48 106.3 . . ? C52 C51 C48 119.1 . . ? C1 N1 C3 114.9 . . ? C1 N1 C2 122.1 . . ? C3 N1 C2 122.4 . . ? C29 C28 N8 105.8 . . ? N16 C46 C45 133.4 . . ? N16 C46 C47 105.0 . . ? C45 C46 C47 121.5 . . ? C20 C23 C24 118.7 . . ? C35 N12 C34 131.4 . . ? C35 N12 C38 106.5 . . ? C34 N12 C38 121.6 . . ? C23 C20 N7 130.7 . . ? C23 C20 C19 123.1 . . ? N7 C20 C19 106.1 . . ? C53 C52 C51 117.8 . . ? C25 C24 C23 117.8 . . ? C50 C49 N16 111.7 . . ? N7 C16 C17 109.9 . . ? N7 C16 C15 129.6 . . ? C17 C16 C15 120.1 . . ? C41 C40 N14 110.8 . . ? C43 C44 C45 117.6 . . ? C57 C58 N18 108.4 . . ? C52 C53 C54 124.2 . . ? N4 C7 C6 106.3 . . ? C58 C57 N17 109.6 . . ? C28 C29 N9 112.6 . . ? C32 C31 N10 113.8 . . ? C432 C430 N6 106.8 . . ? C16 C15 C14 118.2 . . ? C430 C432 N5 109.0 . . ? N12 C34 N11 113.4 . . ? C36 C35 N12 108.5 . . ? N3 C6 C7 107.4 . . ? N1 C3 C4 107.7 . . ? C35 C36 N13 108.4 . . ? N2 C5 N3 109.5 . . ? N7 C21 C22 104.5 . . ? C13 C14 C15 118.4 . . ? C31 C32 N11 98.2 . . ? C3 C4 N2 105.7 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 3.185 _refine_diff_density_min -1.402 _refine_diff_density_rms 0.178 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material 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 -0.003 0.003 -0.003 2631 457 ' ' 2 0.000 1.000 0.500 251 39 ' ' _platon_squeeze_details ; ; #===END data_6 _database_code_depnum_ccdc_archive 'CCDC 894015' #TrackingRef 'web_deposit_cif_file_0_ChaoChen_1346500744.1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H35 F12 N11 P2 Pd2 S2' _chemical_formula_weight 1116.61 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' F F 0.0171 0.0103 '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' 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M p_n_a_21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x+1/2, y+1/2, z+1/2' 'x+1/2, -y+1/2, z' _cell_length_a 15.7470(4) _cell_length_b 15.2248(5) _cell_length_c 17.4931(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4193.9(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 8153 _cell_measurement_theta_min 2.9083 _cell_measurement_theta_max 29.3111 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.768 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2216 _exptl_absorpt_coefficient_mu 1.126 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6743 _exptl_absorpt_correction_T_max 0.7739 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'multiwire proportional' _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 20789 _diffrn_reflns_av_R_equivalents 0.0375 _diffrn_reflns_av_sigmaI/netI 0.0503 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.19 _diffrn_reflns_theta_max 25.10 _reflns_number_total 7357 _reflns_number_gt 5359 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker FRAMBO' _computing_cell_refinement 'Bruker FRAMBO' _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^)+(0.0368P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.08(3) _refine_ls_number_reflns 7357 _refine_ls_number_parameters 537 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0565 _refine_ls_R_factor_gt 0.0338 _refine_ls_wR_factor_ref 0.0765 _refine_ls_wR_factor_gt 0.0713 _refine_ls_goodness_of_fit_ref 0.990 _refine_ls_restrained_S_all 0.994 _refine_ls_shift/su_max 0.002 _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 0.38869(2) 0.34409(3) 0.76255(2) 0.03890(13) Uani 1 1 d . . . Pd2 Pd 0.37139(3) 0.34275(3) 0.95283(2) 0.03875(13) Uani 1 1 d . . . S1 S 0.25206(9) 0.30299(11) 0.80642(10) 0.0494(4) Uani 1 1 d . . . S2 S 0.50704(9) 0.29860(11) 0.90968(10) 0.0516(4) Uani 1 1 d . . . N1 N 0.4362(3) 0.2200(3) 0.7876(3) 0.0430(12) Uani 1 1 d . . . N3 N 0.5309(3) 0.4683(4) 0.7366(3) 0.0468(13) Uani 1 1 d . . . N4 N 0.5630(3) 0.3504(4) 0.6772(3) 0.0497(13) Uani 1 1 d . . . N5 N 0.3983(3) 0.5363(3) 0.7581(5) 0.0486(13) Uani 1 1 d . . . N6 N 0.2787(3) 0.4999(4) 0.7107(3) 0.0536(14) Uani 1 1 d . . . N9 N 0.2324(3) 0.4705(3) 0.9728(3) 0.0447(13) Uani 1 1 d . . . N10 N 0.1999(3) 0.3586(4) 1.0403(3) 0.0514(14) Uani 1 1 d . . . N11 N 0.4840(3) 0.4992(4) 1.0017(3) 0.0524(14) Uani 1 1 d . . . N12 N 0.3652(3) 0.5345(3) 0.9493(5) 0.0479(13) Uani 1 1 d . . . N13 N 0.3194(3) 0.2203(3) 0.9270(3) 0.0407(12) Uani 1 1 d . . . C1 C 0.3500(3) 0.4656(4) 0.7402(3) 0.0395(15) Uani 1 1 d . . . C2 C 0.5029(4) 0.3858(4) 0.7222(3) 0.0440(14) Uani 1 1 d . . . C3 C 0.2605(4) 0.3885(4) 0.9931(4) 0.0444(15) Uani 1 1 d . . . C4 C 0.4845(4) 0.5279(4) 0.7863(4) 0.0548(17) Uani 1 1 d . . . H4A H 0.4840 0.5052 0.8381 0.066 Uiso 1 1 calc R . . H4B H 0.5119 0.5850 0.7868 0.066 Uiso 1 1 calc R . . C5 C 0.3581(4) 0.6131(5) 0.7413(5) 0.063(2) Uani 1 1 d . . . H5 H 0.3785 0.6699 0.7483 0.076 Uiso 1 1 calc R . . C6 C 0.5609(5) 0.2624(5) 0.6459(5) 0.068(2) Uani 1 1 d . . . H6A H 0.5885 0.2227 0.6806 0.101 Uiso 1 1 calc R . . H6B H 0.5899 0.2616 0.5977 0.101 Uiso 1 1 calc R . . H6C H 0.5030 0.2444 0.6388 0.101 Uiso 1 1 calc R . . C7 C 0.4883(3) 0.2107(4) 0.8483(4) 0.0456(15) Uani 1 1 d . . . C8 C 0.4188(5) 0.1514(4) 0.7436(4) 0.0602(19) Uani 1 1 d . . . H8 H 0.3796 0.1585 0.7043 0.072 Uiso 1 1 calc R . . C9 C 0.4556(5) 0.0706(5) 0.7533(6) 0.080(2) Uani 1 1 d . . . H9 H 0.4426 0.0243 0.7207 0.096 Uiso 1 1 calc R . . C10 C 0.1556(4) 0.4902(5) 1.0088(4) 0.0598(18) Uani 1 1 d . . . H10 H 0.1245 0.5419 1.0047 0.072 Uiso 1 1 calc R . . C11 C 0.2258(4) 0.1335(4) 0.8537(5) 0.0599(17) Uani 1 1 d . . . H11 H 0.1864 0.1291 0.8143 0.072 Uiso 1 1 calc R . . C12 C 0.2415(4) 0.0634(5) 0.8981(5) 0.071(2) Uani 1 1 d . . . H12 H 0.2138 0.0106 0.8886 0.085 Uiso 1 1 calc R . . C13 C 0.2973(4) 0.0694(4) 0.9564(5) 0.0621(17) Uani 1 1 d . . . H13 H 0.3087 0.0213 0.9876 0.074 Uiso 1 1 calc R . . C14 C 0.2681(3) 0.2131(4) 0.8660(4) 0.0429(14) Uani 1 1 d . . . C16 C 0.3369(4) 0.1488(4) 0.9684(4) 0.0519(18) Uani 1 1 d . . . H16 H 0.3774 0.1528 1.0069 0.062 Uiso 1 1 calc R . . C17 C 0.2803(3) 0.5234(4) 0.9201(4) 0.0495(16) Uani 1 1 d . . . H17A H 0.2534 0.5803 0.9140 0.059 Uiso 1 1 calc R . . H17B H 0.2823 0.4950 0.8705 0.059 Uiso 1 1 calc R . . C18 C 0.4115(4) 0.4643(4) 0.9724(3) 0.0467(16) Uani 1 1 d . . . C19 C 0.5518(4) 0.4506(6) 1.0385(4) 0.070(2) Uani 1 1 d . . . H19A H 0.5323 0.3926 1.0508 0.104 Uiso 1 1 calc R . . H19B H 0.5685 0.4803 1.0845 0.104 Uiso 1 1 calc R . . H19C H 0.5996 0.4467 1.0045 0.104 Uiso 1 1 calc R . . C20 C 0.2064(4) 0.4502(5) 0.6788(4) 0.069(2) Uani 1 1 d . . . H20A H 0.2236 0.3907 0.6691 0.103 Uiso 1 1 calc R . . H20B H 0.1883 0.4770 0.6319 0.103 Uiso 1 1 calc R . . H20C H 0.1603 0.4505 0.7147 0.103 Uiso 1 1 calc R . . C21 C 0.2821(5) 0.5892(5) 0.7123(5) 0.074(2) Uani 1 1 d . . . H21 H 0.2394 0.6271 0.6962 0.089 Uiso 1 1 calc R . . C22 C 0.6076(4) 0.4855(5) 0.7020(4) 0.0620(19) Uani 1 1 d . . . H22 H 0.6387 0.5374 0.7036 0.074 Uiso 1 1 calc R . . C23 C 0.6276(4) 0.4100(5) 0.6653(4) 0.063(2) Uani 1 1 d . . . H23 H 0.6766 0.4001 0.6369 0.075 Uiso 1 1 calc R . . C24 C 0.4802(4) 0.5895(5) 0.9935(5) 0.073(2) Uani 1 1 d . . . H24 H 0.5223 0.6286 1.0088 0.088 Uiso 1 1 calc R . . C25 C 0.5119(6) 0.0598(5) 0.8119(6) 0.086(3) Uani 1 1 d . . . H25 H 0.5386 0.0060 0.8192 0.103 Uiso 1 1 calc R . . C26 C 0.5289(4) 0.1295(4) 0.8603(5) 0.0652(18) Uani 1 1 d . . . H26 H 0.5670 0.1228 0.9005 0.078 Uiso 1 1 calc R . . C27 C 0.1367(4) 0.4221(5) 1.0491(4) 0.0617(19) Uani 1 1 d . . . H27 H 0.0884 0.4161 1.0793 0.074 Uiso 1 1 calc R . . C33 C 0.4093(4) 0.6114(5) 0.9613(5) 0.067(2) Uani 1 1 d . . . H33 H 0.3916 0.6678 0.9488 0.080 Uiso 1 1 calc R . . C34 C 0.1986(5) 0.2720(5) 1.0766(5) 0.075(2) Uani 1 1 d . . . H34A H 0.1930 0.2274 1.0381 0.112 Uiso 1 1 calc R . . H34B H 0.1513 0.2686 1.1112 0.112 Uiso 1 1 calc R . . H34C H 0.2505 0.2631 1.1043 0.112 Uiso 1 1 calc R . . P1 P 0.20120(12) 0.77666(15) -0.00089(16) 0.0769(6) Uani 1 1 d . . . F1 F 0.2456(5) 0.7391(4) -0.0743(4) 0.143(3) Uani 1 1 d . . . F2 F 0.1735(3) 0.8585(3) -0.0475(4) 0.144(2) Uani 1 1 d . . . F3 F 0.1170(4) 0.7311(5) -0.0203(5) 0.168(3) Uani 1 1 d . . . F4 F 0.1566(4) 0.8141(5) 0.0695(4) 0.152(2) Uani 1 1 d . . . F5 F 0.2347(4) 0.6921(5) 0.0416(4) 0.144(2) Uani 1 1 d . . . F6 F 0.2871(4) 0.8204(5) 0.0228(5) 0.165(3) Uani 1 1 d . . . P2 P 0.04939(11) 0.70973(14) 0.71077(12) 0.0709(6) Uani 1 1 d D . . F7 F 0.1367(3) 0.7527(5) 0.7024(8) 0.230(7) Uani 1 1 d D . . F8 F 0.0103(4) 0.7789(5) 0.6558(4) 0.183(4) Uani 1 1 d . . . F9 F 0.0228(5) 0.7642(4) 0.7832(3) 0.157(3) Uani 1 1 d D . . F10 F -0.0384(4) 0.6665(5) 0.7166(4) 0.151(2) Uani 1 1 d . . . F11 F 0.0902(3) 0.6398(3) 0.7648(3) 0.1023(14) Uani 1 1 d D . . F12 F 0.0800(7) 0.6549(6) 0.6427(3) 0.235(5) Uani 1 1 d D . . N37 N 0.4718(15) 0.9353(19) 1.0540(13) 0.372(15) Uani 1 1 d D . . C35 C 0.4575(6) 0.9042(9) 0.9989(11) 0.176(9) Uani 1 1 d D . . C36 C 0.4411(15) 0.8596(14) 0.9127(11) 0.327(15) Uani 1 1 d . . . H36A H 0.3815 0.8611 0.9010 0.490 Uiso 1 1 calc R . . H36B H 0.4605 0.7998 0.9128 0.490 Uiso 1 1 calc R . . H36C H 0.4718 0.8924 0.8748 0.490 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 0.0397(2) 0.0377(3) 0.0394(3) 0.0047(3) 0.0016(2) 0.0059(2) Pd2 0.03528(19) 0.0398(3) 0.0411(3) -0.0040(3) 0.0022(2) -0.0023(2) S1 0.0406(8) 0.0568(10) 0.0506(9) 0.0119(9) -0.0031(7) -0.0016(7) S2 0.0360(8) 0.0592(11) 0.0596(10) -0.0068(9) -0.0022(7) 0.0057(7) N1 0.042(3) 0.045(3) 0.042(3) 0.001(3) 0.004(2) 0.002(2) N3 0.034(3) 0.051(3) 0.056(3) 0.009(3) 0.006(2) 0.007(2) N4 0.045(3) 0.064(4) 0.039(3) 0.013(3) 0.013(2) 0.019(3) N5 0.037(2) 0.043(3) 0.065(4) 0.014(4) 0.007(3) 0.002(2) N6 0.039(3) 0.058(4) 0.063(4) 0.021(3) 0.010(2) 0.012(3) N9 0.034(2) 0.048(3) 0.053(3) -0.004(3) 0.011(2) -0.007(2) N10 0.039(3) 0.057(4) 0.058(3) 0.009(3) 0.008(2) -0.003(3) N11 0.038(3) 0.062(4) 0.057(3) -0.025(3) 0.004(3) -0.014(3) N12 0.046(2) 0.039(3) 0.059(3) -0.012(3) 0.012(3) -0.014(2) N13 0.047(3) 0.034(3) 0.041(3) 0.004(3) -0.001(2) -0.003(2) C1 0.034(3) 0.044(4) 0.040(4) 0.011(3) 0.005(3) 0.008(3) C2 0.047(3) 0.047(4) 0.038(3) 0.010(3) 0.001(3) 0.015(3) C3 0.040(3) 0.040(4) 0.053(4) -0.011(3) 0.004(3) -0.007(3) C4 0.051(4) 0.043(4) 0.071(5) 0.007(3) 0.010(3) 0.002(3) C5 0.054(4) 0.041(4) 0.094(6) 0.019(4) 0.008(4) 0.004(3) C6 0.072(5) 0.067(5) 0.064(5) 0.002(4) 0.020(4) 0.030(4) C7 0.045(3) 0.043(4) 0.049(4) 0.000(4) 0.015(3) 0.007(3) C8 0.085(5) 0.036(4) 0.059(5) -0.012(4) 0.007(4) -0.002(4) C9 0.109(6) 0.047(5) 0.082(6) -0.012(5) 0.019(5) 0.009(4) C10 0.045(4) 0.058(5) 0.076(5) -0.018(4) 0.016(3) 0.005(3) C11 0.058(4) 0.048(4) 0.074(4) -0.005(5) 0.001(4) -0.017(3) C12 0.083(5) 0.040(4) 0.089(6) 0.000(4) 0.009(4) -0.024(4) C13 0.078(4) 0.038(4) 0.070(5) 0.022(4) 0.011(5) -0.001(3) C14 0.033(3) 0.044(4) 0.052(4) -0.008(4) 0.007(3) -0.009(2) C16 0.059(4) 0.047(5) 0.050(4) -0.010(4) -0.010(3) 0.021(3) C17 0.047(3) 0.044(4) 0.058(4) -0.003(3) 0.009(3) 0.007(3) C18 0.038(3) 0.056(5) 0.047(4) -0.008(3) 0.011(3) -0.007(3) C19 0.048(4) 0.092(7) 0.069(5) -0.016(4) -0.007(3) -0.014(4) C20 0.050(4) 0.069(5) 0.089(5) 0.027(4) -0.023(4) 0.002(3) C21 0.061(5) 0.063(6) 0.098(6) 0.026(5) 0.009(4) 0.028(4) C22 0.037(3) 0.080(5) 0.068(4) 0.023(4) 0.000(3) 0.004(3) C23 0.052(4) 0.081(6) 0.054(4) 0.019(4) 0.014(3) 0.017(4) C24 0.047(4) 0.065(6) 0.107(6) -0.037(5) 0.016(4) -0.021(4) C25 0.112(7) 0.044(5) 0.103(7) 0.014(5) 0.030(5) 0.031(5) C26 0.068(4) 0.067(5) 0.061(4) 0.008(6) -0.005(4) 0.029(3) C27 0.042(4) 0.076(5) 0.067(5) -0.013(4) 0.018(3) -0.010(4) C33 0.053(4) 0.050(5) 0.098(6) -0.012(5) 0.026(4) -0.016(4) C34 0.071(5) 0.073(5) 0.082(6) 0.012(5) 0.026(4) -0.005(4) P1 0.0528(11) 0.0598(13) 0.1180(19) -0.0064(14) -0.0049(12) 0.0128(10) F1 0.182(6) 0.144(6) 0.103(5) -0.017(4) 0.019(4) 0.074(4) F2 0.125(4) 0.097(4) 0.209(6) 0.057(4) 0.048(5) 0.047(3) F3 0.131(5) 0.137(6) 0.235(8) 0.039(6) -0.083(5) -0.060(4) F4 0.132(5) 0.188(7) 0.136(5) -0.023(5) 0.038(4) 0.048(5) F5 0.160(5) 0.131(5) 0.140(5) 0.017(4) -0.024(4) 0.070(4) F6 0.084(4) 0.199(7) 0.213(7) -0.054(6) -0.031(4) -0.037(4) P2 0.0537(11) 0.0780(15) 0.0809(15) 0.0144(13) 0.0135(10) 0.0168(11) F7 0.079(4) 0.196(9) 0.416(17) 0.176(10) 0.031(6) -0.013(4) F8 0.123(4) 0.227(7) 0.199(7) 0.133(7) 0.031(5) 0.091(5) F9 0.220(7) 0.104(5) 0.147(7) -0.043(4) -0.039(6) 0.077(4) F10 0.096(4) 0.173(6) 0.185(6) 0.018(5) -0.018(4) -0.035(4) F11 0.097(3) 0.095(3) 0.114(3) 0.038(3) 0.008(3) 0.027(3) F12 0.303(11) 0.298(12) 0.104(5) -0.026(6) 0.040(6) 0.184(10) N37 0.35(3) 0.45(4) 0.31(3) -0.12(2) 0.02(2) -0.02(2) C35 0.050(5) 0.123(11) 0.35(2) 0.130(14) 0.047(9) 0.007(6) C36 0.44(4) 0.36(3) 0.182(16) -0.026(18) 0.16(2) -0.11(2) _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 C1 1.987(6) . ? Pd1 C2 2.033(6) . ? Pd1 N1 2.078(5) . ? Pd1 S1 2.3683(15) . ? Pd1 Pd2 3.3397(5) . ? Pd2 C18 1.986(6) . ? Pd2 C3 2.008(6) . ? Pd2 N13 2.085(5) . ? Pd2 S2 2.3632(15) . ? S1 C14 1.738(7) . ? S2 C7 1.742(6) . ? N1 C8 1.326(8) . ? N1 C7 1.350(8) . ? N3 C2 1.356(8) . ? N3 C22 1.374(7) . ? N3 C4 1.454(7) . ? N4 C2 1.343(7) . ? N4 C23 1.380(8) . ? N4 C6 1.448(8) . ? N5 C1 1.355(8) . ? N5 C5 1.363(8) . ? N5 C4 1.449(8) . ? N6 C1 1.342(7) . ? N6 C21 1.360(9) . ? N6 C20 1.476(8) . ? N9 C3 1.372(8) . ? N9 C10 1.395(7) . ? N9 C17 1.438(7) . ? N10 C3 1.340(8) . ? N10 C27 1.396(9) . ? N10 C34 1.464(9) . ? N11 C18 1.359(7) . ? N11 C24 1.384(9) . ? N11 C19 1.450(9) . ? N12 C18 1.355(8) . ? N12 C33 1.377(8) . ? N12 C17 1.440(7) . ? N13 C16 1.337(8) . ? N13 C14 1.343(8) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C21 1.350(10) . ? C5 H5 0.9300 . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 C26 1.406(8) . ? C8 C9 1.371(9) . ? C8 H8 0.9300 . ? C9 C25 1.365(11) . ? C9 H9 0.9300 . ? C10 C27 1.289(9) . ? C10 H10 0.9300 . ? C11 C12 1.342(9) . ? C11 C14 1.399(7) . ? C11 H11 0.9300 . ? C12 C13 1.350(9) . ? C12 H12 0.9300 . ? C13 C16 1.375(9) . ? C13 H13 0.9300 . ? C16 H16 0.9300 . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 H21 0.9300 . ? C22 C23 1.354(10) . ? C22 H22 0.9300 . ? C23 H23 0.9300 . ? C24 C33 1.294(10) . ? C24 H24 0.9300 . ? C25 C26 1.384(11) . ? C25 H25 0.9300 . ? C26 H26 0.9300 . ? C27 H27 0.9300 . ? C33 H33 0.9300 . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? P1 F4 1.528(6) . ? P1 F3 1.534(6) . ? P1 F2 1.551(5) . ? P1 F6 1.564(6) . ? P1 F1 1.569(6) . ? P1 F5 1.578(6) . ? P2 F7 1.529(4) . ? P2 F12 1.532(4) . ? P2 F10 1.534(6) . ? P2 F8 1.554(6) . ? P2 F11 1.562(3) . ? P2 F9 1.571(4) . ? N37 C35 1.096(5) . ? C35 C36 1.67(2) . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? 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 C1 Pd1 C2 84.9(2) . . ? C1 Pd1 N1 176.6(2) . . ? C2 Pd1 N1 92.2(2) . . ? C1 Pd1 S1 91.80(16) . . ? C2 Pd1 S1 176.63(17) . . ? N1 Pd1 S1 91.07(13) . . ? C1 Pd1 Pd2 100.21(16) . . ? C2 Pd1 Pd2 114.86(17) . . ? N1 Pd1 Pd2 79.28(13) . . ? S1 Pd1 Pd2 66.51(4) . . ? C18 Pd2 C3 83.9(2) . . ? C18 Pd2 N13 174.6(2) . . ? C3 Pd2 N13 92.6(2) . . ? C18 Pd2 S2 91.86(18) . . ? C3 Pd2 S2 175.53(17) . . ? N13 Pd2 S2 91.81(13) . . ? C18 Pd2 Pd1 98.08(17) . . ? C3 Pd2 Pd1 114.76(18) . . ? N13 Pd2 Pd1 79.71(13) . . ? S2 Pd2 Pd1 67.02(5) . . ? C14 S1 Pd1 105.69(17) . . ? C7 S2 Pd2 105.24(18) . . ? C8 N1 C7 119.9(5) . . ? C8 N1 Pd1 121.3(4) . . ? C7 N1 Pd1 118.7(4) . . ? C2 N3 C22 112.4(5) . . ? C2 N3 C4 121.7(5) . . ? C22 N3 C4 125.8(6) . . ? C2 N4 C23 110.2(6) . . ? C2 N4 C6 125.2(6) . . ? C23 N4 C6 124.6(6) . . ? C1 N5 C5 111.7(5) . . ? C1 N5 C4 122.3(5) . . ? C5 N5 C4 125.8(6) . . ? C1 N6 C21 110.4(6) . . ? C1 N6 C20 126.2(6) . . ? C21 N6 C20 123.4(6) . . ? C3 N9 C10 111.0(5) . . ? C3 N9 C17 120.4(5) . . ? C10 N9 C17 128.6(6) . . ? C3 N10 C27 109.9(6) . . ? C3 N10 C34 125.7(5) . . ? C27 N10 C34 124.4(6) . . ? C18 N11 C24 108.3(6) . . ? C18 N11 C19 125.9(6) . . ? C24 N11 C19 125.8(5) . . ? C18 N12 C33 110.7(6) . . ? C18 N12 C17 120.9(5) . . ? C33 N12 C17 128.4(6) . . ? C16 N13 C14 119.2(5) . . ? C16 N13 Pd2 122.0(4) . . ? C14 N13 Pd2 118.8(4) . . ? N6 C1 N5 104.5(5) . . ? N6 C1 Pd1 134.0(5) . . ? N5 C1 Pd1 121.5(4) . . ? N4 C2 N3 104.5(5) . . ? N4 C2 Pd1 134.5(5) . . ? N3 C2 Pd1 120.9(4) . . ? N10 C3 N9 103.8(5) . . ? N10 C3 Pd2 135.8(5) . . ? N9 C3 Pd2 120.4(4) . . ? N5 C4 N3 108.8(5) . . ? N5 C4 H4A 109.9 . . ? N3 C4 H4A 109.9 . . ? N5 C4 H4B 109.9 . . ? N3 C4 H4B 109.9 . . ? H4A C4 H4B 108.3 . . ? C21 C5 N5 105.2(6) . . ? C21 C5 H5 127.4 . . ? N5 C5 H5 127.4 . . ? N4 C6 H6A 109.5 . . ? N4 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? N4 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? N1 C7 C26 119.1(6) . . ? N1 C7 S2 120.5(4) . . ? C26 C7 S2 120.4(6) . . ? N1 C8 C9 123.2(7) . . ? N1 C8 H8 118.4 . . ? C9 C8 H8 118.4 . . ? C25 C9 C8 118.4(8) . . ? C25 C9 H9 120.8 . . ? C8 C9 H9 120.8 . . ? C27 C10 N9 105.9(6) . . ? C27 C10 H10 127.0 . . ? N9 C10 H10 127.0 . . ? C12 C11 C14 120.9(7) . . ? C12 C11 H11 119.6 . . ? C14 C11 H11 119.6 . . ? C11 C12 C13 120.2(7) . . ? C11 C12 H12 119.9 . . ? C13 C12 H12 119.9 . . ? C12 C13 C16 118.0(6) . . ? C12 C13 H13 121.0 . . ? C16 C13 H13 121.0 . . ? N13 C14 C11 118.6(6) . . ? N13 C14 S1 120.0(4) . . ? C11 C14 S1 121.4(5) . . ? N13 C16 C13 122.7(6) . . ? N13 C16 H16 118.7 . . ? C13 C16 H16 118.7 . . ? N9 C17 N12 109.0(5) . . ? N9 C17 H17A 109.9 . . ? N12 C17 H17A 109.9 . . ? N9 C17 H17B 109.9 . . ? N12 C17 H17B 109.9 . . ? H17A C17 H17B 108.3 . . ? N12 C18 N11 104.9(6) . . ? N12 C18 Pd2 120.8(4) . . ? N11 C18 Pd2 134.2(5) . . ? N11 C19 H19A 109.5 . . ? N11 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? N11 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? N6 C20 H20A 109.5 . . ? N6 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? N6 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C5 C21 N6 108.2(6) . . ? C5 C21 H21 125.9 . . ? N6 C21 H21 125.9 . . ? C23 C22 N3 104.6(6) . . ? C23 C22 H22 127.7 . . ? N3 C22 H22 127.7 . . ? C22 C23 N4 108.3(6) . . ? C22 C23 H23 125.8 . . ? N4 C23 H23 125.8 . . ? C33 C24 N11 109.7(6) . . ? C33 C24 H24 125.1 . . ? N11 C24 H24 125.1 . . ? C9 C25 C26 119.5(7) . . ? C9 C25 H25 120.2 . . ? C26 C25 H25 120.2 . . ? C25 C26 C7 119.6(7) . . ? C25 C26 H26 120.2 . . ? C7 C26 H26 120.2 . . ? C10 C27 N10 109.3(6) . . ? C10 C27 H27 125.3 . . ? N10 C27 H27 125.3 . . ? C24 C33 N12 106.5(7) . . ? C24 C33 H33 126.8 . . ? N12 C33 H33 126.8 . . ? N10 C34 H34A 109.5 . . ? N10 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? N10 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? F4 P1 F3 87.1(4) . . ? F4 P1 F2 89.7(4) . . ? F3 P1 F2 90.2(4) . . ? F4 P1 F6 91.4(4) . . ? F3 P1 F6 177.0(5) . . ? F2 P1 F6 92.4(4) . . ? F4 P1 F1 178.8(4) . . ? F3 P1 F1 92.2(5) . . ? F2 P1 F1 89.3(4) . . ? F6 P1 F1 89.3(4) . . ? F4 P1 F5 94.5(4) . . ? F3 P1 F5 91.4(4) . . ? F2 P1 F5 175.6(4) . . ? F6 P1 F5 86.2(4) . . ? F1 P1 F5 86.5(3) . . ? F7 P2 F12 82.9(6) . . ? F7 P2 F10 178.3(6) . . ? F12 P2 F10 95.8(6) . . ? F7 P2 F8 90.4(4) . . ? F12 P2 F8 90.7(4) . . ? F10 P2 F8 88.5(4) . . ? F7 P2 F11 88.8(3) . . ? F12 P2 F11 88.2(4) . . ? F10 P2 F11 92.2(3) . . ? F8 P2 F11 178.8(3) . . ? F7 P2 F9 95.2(6) . . ? F12 P2 F9 176.6(4) . . ? F10 P2 F9 86.2(4) . . ? F8 P2 F9 92.1(4) . . ? F11 P2 F9 88.9(3) . . ? N37 C35 C36 176.5(19) . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? 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 C1 Pd1 Pd2 C18 -38.63(19) . . . . ? C2 Pd1 Pd2 C18 50.5(3) . . . . ? N1 Pd1 Pd2 C18 137.9(2) . . . . ? S1 Pd1 Pd2 C18 -126.14(19) . . . . ? C1 Pd1 Pd2 C3 48.3(3) . . . . ? C2 Pd1 Pd2 C3 137.4(2) . . . . ? N1 Pd1 Pd2 C3 -135.1(2) . . . . ? S1 Pd1 Pd2 C3 -39.2(2) . . . . ? C1 Pd1 Pd2 N13 136.4(2) . . . . ? C2 Pd1 Pd2 N13 -134.5(2) . . . . ? N1 Pd1 Pd2 N13 -47.07(14) . . . . ? S1 Pd1 Pd2 N13 48.85(14) . . . . ? C1 Pd1 Pd2 S2 -127.22(17) . . . . ? C2 Pd1 Pd2 S2 -38.11(19) . . . . ? N1 Pd1 Pd2 S2 49.35(13) . . . . ? S1 Pd1 Pd2 S2 145.27(5) . . . . ? C1 Pd1 S1 C14 -157.2(3) . . . . ? C2 Pd1 S1 C14 -171(3) . . . . ? N1 Pd1 S1 C14 21.0(3) . . . . ? Pd2 Pd1 S1 C14 -56.9(2) . . . . ? C18 Pd2 S2 C7 -154.2(3) . . . . ? C3 Pd2 S2 C7 -171(3) . . . . ? N13 Pd2 S2 C7 21.8(3) . . . . ? Pd1 Pd2 S2 C7 -56.2(2) . . . . ? C1 Pd1 N1 C8 -137(3) . . . . ? C2 Pd1 N1 C8 -104.0(5) . . . . ? S1 Pd1 N1 C8 75.2(4) . . . . ? Pd2 Pd1 N1 C8 141.1(5) . . . . ? C1 Pd1 N1 C7 40(4) . . . . ? C2 Pd1 N1 C7 73.4(4) . . . . ? S1 Pd1 N1 C7 -107.3(4) . . . . ? Pd2 Pd1 N1 C7 -41.5(4) . . . . ? C18 Pd2 N13 C16 -155(2) . . . . ? C3 Pd2 N13 C16 -107.0(5) . . . . ? S2 Pd2 N13 C16 72.0(4) . . . . ? Pd1 Pd2 N13 C16 138.3(4) . . . . ? C18 Pd2 N13 C14 26(2) . . . . ? C3 Pd2 N13 C14 74.3(4) . . . . ? S2 Pd2 N13 C14 -106.7(4) . . . . ? Pd1 Pd2 N13 C14 -40.5(4) . . . . ? C21 N6 C1 N5 -1.6(7) . . . . ? C20 N6 C1 N5 177.1(6) . . . . ? C21 N6 C1 Pd1 175.8(5) . . . . ? C20 N6 C1 Pd1 -5.6(9) . . . . ? C5 N5 C1 N6 0.8(8) . . . . ? C4 N5 C1 N6 -175.0(6) . . . . ? C5 N5 C1 Pd1 -177.0(5) . . . . ? C4 N5 C1 Pd1 7.3(9) . . . . ? C2 Pd1 C1 N6 139.7(6) . . . . ? N1 Pd1 C1 N6 173(3) . . . . ? S1 Pd1 C1 N6 -39.5(6) . . . . ? Pd2 Pd1 C1 N6 -105.9(5) . . . . ? C2 Pd1 C1 N5 -43.3(5) . . . . ? N1 Pd1 C1 N5 -10(4) . . . . ? S1 Pd1 C1 N5 137.5(5) . . . . ? Pd2 Pd1 C1 N5 71.0(5) . . . . ? C23 N4 C2 N3 0.9(6) . . . . ? C6 N4 C2 N3 -179.4(6) . . . . ? C23 N4 C2 Pd1 177.5(4) . . . . ? C6 N4 C2 Pd1 -2.7(9) . . . . ? C22 N3 C2 N4 -0.3(6) . . . . ? C4 N3 C2 N4 -177.7(5) . . . . ? C22 N3 C2 Pd1 -177.5(4) . . . . ? C4 N3 C2 Pd1 5.1(7) . . . . ? C1 Pd1 C2 N4 -139.0(6) . . . . ? N1 Pd1 C2 N4 42.9(6) . . . . ? S1 Pd1 C2 N4 -125(3) . . . . ? Pd2 Pd1 C2 N4 122.1(5) . . . . ? C1 Pd1 C2 N3 37.2(5) . . . . ? N1 Pd1 C2 N3 -140.9(5) . . . . ? S1 Pd1 C2 N3 52(3) . . . . ? Pd2 Pd1 C2 N3 -61.7(5) . . . . ? C27 N10 C3 N9 -0.8(7) . . . . ? C34 N10 C3 N9 178.3(6) . . . . ? C27 N10 C3 Pd2 178.2(5) . . . . ? C34 N10 C3 Pd2 -2.7(10) . . . . ? C10 N9 C3 N10 1.0(6) . . . . ? C17 N9 C3 N10 -178.4(5) . . . . ? C10 N9 C3 Pd2 -178.2(4) . . . . ? C17 N9 C3 Pd2 2.4(7) . . . . ? C18 Pd2 C3 N10 -137.8(7) . . . . ? N13 Pd2 C3 N10 46.2(7) . . . . ? S2 Pd2 C3 N10 -121(2) . . . . ? Pd1 Pd2 C3 N10 126.1(6) . . . . ? C18 Pd2 C3 N9 41.0(5) . . . . ? N13 Pd2 C3 N9 -134.9(5) . . . . ? S2 Pd2 C3 N9 58(3) . . . . ? Pd1 Pd2 C3 N9 -55.0(5) . . . . ? C1 N5 C4 N3 49.0(9) . . . . ? C5 N5 C4 N3 -126.1(8) . . . . ? C2 N3 C4 N5 -55.4(7) . . . . ? C22 N3 C4 N5 127.5(6) . . . . ? C1 N5 C5 C21 0.3(9) . . . . ? C4 N5 C5 C21 175.9(8) . . . . ? C8 N1 C7 C26 5.1(8) . . . . ? Pd1 N1 C7 C26 -172.4(5) . . . . ? C8 N1 C7 S2 -176.3(5) . . . . ? Pd1 N1 C7 S2 6.2(6) . . . . ? Pd2 S2 C7 N1 56.3(5) . . . . ? Pd2 S2 C7 C26 -125.2(5) . . . . ? C7 N1 C8 C9 -4.4(9) . . . . ? Pd1 N1 C8 C9 173.0(5) . . . . ? N1 C8 C9 C25 1.2(11) . . . . ? C3 N9 C10 C27 -0.8(7) . . . . ? C17 N9 C10 C27 178.5(6) . . . . ? C14 C11 C12 C13 1.3(11) . . . . ? C11 C12 C13 C16 0.0(11) . . . . ? C16 N13 C14 C11 8.3(8) . . . . ? Pd2 N13 C14 C11 -173.0(4) . . . . ? C16 N13 C14 S1 -174.2(4) . . . . ? Pd2 N13 C14 S1 4.5(6) . . . . ? C12 C11 C14 N13 -5.5(10) . . . . ? C12 C11 C14 S1 177.1(6) . . . . ? Pd1 S1 C14 N13 57.7(5) . . . . ? Pd1 S1 C14 C11 -124.9(5) . . . . ? C14 N13 C16 C13 -7.3(9) . . . . ? Pd2 N13 C16 C13 174.0(5) . . . . ? C12 C13 C16 N13 3.0(10) . . . . ? C3 N9 C17 N12 -56.6(7) . . . . ? C10 N9 C17 N12 124.2(6) . . . . ? C18 N12 C17 N9 50.5(9) . . . . ? C33 N12 C17 N9 -126.4(8) . . . . ? C33 N12 C18 N11 2.2(8) . . . . ? C17 N12 C18 N11 -175.2(6) . . . . ? C33 N12 C18 Pd2 -173.4(5) . . . . ? C17 N12 C18 Pd2 9.2(10) . . . . ? C24 N11 C18 N12 -1.5(7) . . . . ? C19 N11 C18 N12 175.7(6) . . . . ? C24 N11 C18 Pd2 173.2(5) . . . . ? C19 N11 C18 Pd2 -9.5(10) . . . . ? C3 Pd2 C18 N12 -47.1(6) . . . . ? N13 Pd2 C18 N12 2(3) . . . . ? S2 Pd2 C18 N12 134.2(5) . . . . ? Pd1 Pd2 C18 N12 67.1(5) . . . . ? C3 Pd2 C18 N11 138.9(6) . . . . ? N13 Pd2 C18 N11 -172.4(18) . . . . ? S2 Pd2 C18 N11 -39.9(6) . . . . ? Pd1 Pd2 C18 N11 -106.9(6) . . . . ? N5 C5 C21 N6 -1.2(9) . . . . ? C1 N6 C21 C5 1.8(8) . . . . ? C20 N6 C21 C5 -176.8(6) . . . . ? C2 N3 C22 C23 -0.4(7) . . . . ? C4 N3 C22 C23 176.9(5) . . . . ? N3 C22 C23 N4 1.0(7) . . . . ? C2 N4 C23 C22 -1.2(7) . . . . ? C6 N4 C23 C22 179.0(6) . . . . ? C18 N11 C24 C33 0.4(8) . . . . ? C19 N11 C24 C33 -176.9(6) . . . . ? C8 C9 C25 C26 1.2(12) . . . . ? C9 C25 C26 C7 -0.3(11) . . . . ? N1 C7 C26 C25 -2.8(10) . . . . ? S2 C7 C26 C25 178.6(6) . . . . ? N9 C10 C27 N10 0.3(7) . . . . ? C3 N10 C27 C10 0.3(8) . . . . ? C34 N10 C27 C10 -178.8(7) . . . . ? N11 C24 C33 N12 0.9(9) . . . . ? C18 N12 C33 C24 -2.0(9) . . . . ? C17 N12 C33 C24 175.2(8) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.10 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.511 _refine_diff_density_min -0.337 _refine_diff_density_rms 0.068 #===END data_7 _database_code_depnum_ccdc_archive 'CCDC 894016' #TrackingRef 'web_deposit_cif_file_0_ChaoChen_1346500744.1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H46 F12 N12 P2 Pd2' _chemical_formula_weight 1101.55 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' P P 0.1023 0.0942 '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 Monoclinic _symmetry_space_group_name_H-M P2(1)/c 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 14.8227(4) _cell_length_b 20.3413(5) _cell_length_c 15.2998(5) _cell_angle_alpha 90.00 _cell_angle_beta 112.113(4) _cell_angle_gamma 90.00 _cell_volume 4273.8(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 8360 _cell_measurement_theta_min 2.8672 _cell_measurement_theta_max 29.3952 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.29 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.712 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2208 _exptl_absorpt_coefficient_mu 1.010 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6764 _exptl_absorpt_correction_T_max 0.7583 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'multiwire proportional' _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 30090 _diffrn_reflns_av_R_equivalents 0.0365 _diffrn_reflns_av_sigmaI/netI 0.0343 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.87 _diffrn_reflns_theta_max 25.01 _reflns_number_total 7523 _reflns_number_gt 6036 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker FRAMBO' _computing_cell_refinement 'Bruker FRAMBO' _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^)+(0.0644P)^2^+10.8594P] 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 7523 _refine_ls_number_parameters 549 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.0602 _refine_ls_R_factor_gt 0.0448 _refine_ls_wR_factor_ref 0.1286 _refine_ls_wR_factor_gt 0.1154 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.050 _refine_ls_shift/su_max 0.062 _refine_ls_shift/su_mean 0.001 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 0.37731(3) 0.682521(17) 0.19212(2) 0.03131(12) Uani 1 1 d . . . Pd2 Pd 0.14869(3) 0.740942(18) 0.01459(3) 0.03383(13) Uani 1 1 d . . . C1 C 0.2423(6) 0.4678(3) 0.1661(6) 0.082(2) Uani 1 1 d . . . H1A H 0.2831 0.4668 0.1301 0.122 Uiso 1 1 calc R . . H1B H 0.1753 0.4639 0.1243 0.122 Uiso 1 1 calc R . . H1C H 0.2590 0.4318 0.2100 0.122 Uiso 1 1 calc R . . C2 C 0.2571(5) 0.5325(3) 0.2199(5) 0.0586(16) Uani 1 1 d . . . H2A H 0.2300 0.5680 0.1755 0.070 Uiso 1 1 calc R . . H2B H 0.2220 0.5310 0.2621 0.070 Uiso 1 1 calc R . . C3 C 0.4093(4) 0.6004(2) 0.2701(4) 0.0396(12) Uani 1 1 d . . . C4 C 0.4200(6) 0.5034(3) 0.3417(5) 0.0685(19) Uani 1 1 d . . . H4 H 0.4024 0.4625 0.3574 0.082 Uiso 1 1 calc R . . C5 C 0.5076(6) 0.5313(3) 0.3794(5) 0.0670(19) Uani 1 1 d . . . H5 H 0.5624 0.5140 0.4266 0.080 Uiso 1 1 calc R . . C6 C 0.5774(4) 0.6388(3) 0.3538(4) 0.0532(15) Uani 1 1 d . . . H6A H 0.5970 0.6421 0.3002 0.064 Uiso 1 1 calc R . . H6B H 0.6336 0.6255 0.4084 0.064 Uiso 1 1 calc R . . C7 C 0.4566(4) 0.7269(3) 0.3119(4) 0.0410(12) Uani 1 1 d . . . C8 C 0.5851(5) 0.7410(4) 0.4497(5) 0.0661(19) Uani 1 1 d . . . H8 H 0.6438 0.7336 0.4998 0.079 Uiso 1 1 calc R . . C9 C 0.5256(6) 0.7912(4) 0.4386(5) 0.075(2) Uani 1 1 d . . . H9 H 0.5350 0.8264 0.4800 0.090 Uiso 1 1 calc R . . C12 C 0.0095(6) 0.5708(4) 0.1194(6) 0.090(3) Uani 1 1 d . . . H12A H -0.0587 0.5606 0.0914 0.135 Uiso 1 1 calc R . . H12B H 0.0368 0.5513 0.1810 0.135 Uiso 1 1 calc R . . H12C H 0.0419 0.5536 0.0805 0.135 Uiso 1 1 calc R . . C13 C 0.0227(6) 0.6442(4) 0.1276(5) 0.0683(19) Uani 1 1 d . . . H13A H -0.0009 0.6606 0.1747 0.082 Uiso 1 1 calc R . . H13B H 0.0915 0.6545 0.1487 0.082 Uiso 1 1 calc R . . C14 C -0.1297(5) 0.6766(4) -0.0116(6) 0.071(2) Uani 1 1 d . . . H14 H -0.1749 0.6541 0.0059 0.085 Uiso 1 1 calc R . . C15 C -0.1502(4) 0.7135(3) -0.0877(6) 0.0658(19) Uani 1 1 d . . . H15 H -0.2114 0.7222 -0.1332 0.079 Uiso 1 1 calc R . . C16 C 0.0123(4) 0.7146(3) -0.0085(4) 0.0416(12) Uani 1 1 d . . . C17 C -0.0467(5) 0.7822(3) -0.1507(4) 0.0554(15) Uani 1 1 d . . . H17A H -0.1089 0.7972 -0.1958 0.066 Uiso 1 1 calc R . . H17B H -0.0114 0.7612 -0.1851 0.066 Uiso 1 1 calc R . . C18 C -0.0130(5) 0.9025(3) -0.1169(5) 0.0602(17) Uani 1 1 d . . . H18 H -0.0650 0.9199 -0.1672 0.072 Uiso 1 1 calc R . . C19 C 0.0549(5) 0.9356(3) -0.0499(5) 0.0618(17) Uani 1 1 d . . . H19 H 0.0599 0.9811 -0.0446 0.074 Uiso 1 1 calc R . . C20 C 0.0896(4) 0.8299(3) -0.0188(4) 0.0405(12) Uani 1 1 d . . . C23 C 0.0677(4) 0.6029(3) -0.1236(4) 0.0590(16) Uani 1 1 d . . . H23A H 0.0214 0.5977 -0.0939 0.088 Uiso 1 1 calc R . . H23B H 0.0605 0.5674 -0.1671 0.088 Uiso 1 1 calc R . . H23C H 0.0563 0.6439 -0.1570 0.088 Uiso 1 1 calc R . . C24 C 0.1684(4) 0.6023(3) -0.0502(4) 0.0406(12) Uani 1 1 d . . . C25 C 0.2416(4) 0.5587(3) -0.0429(4) 0.0459(13) Uani 1 1 d . . . H25 H 0.2377 0.5228 -0.0817 0.055 Uiso 1 1 calc R . . C26 C 0.3224(4) 0.5787(2) 0.0333(4) 0.0394(12) Uani 1 1 d . . . C27 C 0.4219(4) 0.5497(3) 0.0711(5) 0.0575(16) Uani 1 1 d . . . H27A H 0.4690 0.5839 0.0974 0.086 Uiso 1 1 calc R . . H27B H 0.4346 0.5283 0.0210 0.086 Uiso 1 1 calc R . . H27C H 0.4263 0.5182 0.1192 0.086 Uiso 1 1 calc R . . C28 C 0.2359(5) 0.8371(5) -0.1217(6) 0.098(3) Uani 1 1 d . . . H28A H 0.1848 0.8049 -0.1425 0.148 Uiso 1 1 calc R . . H28B H 0.2688 0.8385 -0.1651 0.148 Uiso 1 1 calc R . . H28C H 0.2086 0.8795 -0.1192 0.148 Uiso 1 1 calc R . . C29 C 0.3077(4) 0.8188(3) -0.0246(5) 0.0587(17) Uani 1 1 d . . . C30 C 0.4032(5) 0.8361(3) 0.0184(5) 0.0593(17) Uani 1 1 d . . . H30 H 0.4380 0.8649 -0.0044 0.071 Uiso 1 1 calc R . . C31 C 0.4379(4) 0.8020(3) 0.1032(4) 0.0453(13) Uani 1 1 d . . . C32 C 0.5393(4) 0.8025(3) 0.1758(5) 0.0561(15) Uani 1 1 d . . . H32A H 0.5399 0.8244 0.2315 0.084 Uiso 1 1 calc R . . H32B H 0.5814 0.8253 0.1513 0.084 Uiso 1 1 calc R . . H32C H 0.5617 0.7581 0.1911 0.084 Uiso 1 1 calc R . . N1 N 0.3605(4) 0.5463(2) 0.2752(3) 0.0495(12) Uani 1 1 d . . . N2 N 0.5008(3) 0.5910(2) 0.3348(3) 0.0469(11) Uani 1 1 d . . . N3 N 0.5420(3) 0.7018(2) 0.3713(3) 0.0476(11) Uani 1 1 d . . . N4 N 0.4462(4) 0.7826(2) 0.3542(3) 0.0543(13) Uani 1 1 d . . . N5 N 0.1176(3) 0.8907(2) 0.0112(3) 0.0482(12) Uani 1 1 d . . . N6 N 0.0084(3) 0.8373(2) -0.0975(3) 0.0471(11) Uani 1 1 d . . . N7 N -0.0617(3) 0.7364(2) -0.0857(4) 0.0502(12) Uani 1 1 d . . . N8 N -0.0292(3) 0.6771(2) 0.0380(4) 0.0495(12) Uani 1 1 d . . . N9 N 0.2026(3) 0.64683(19) 0.0199(3) 0.0361(9) Uani 1 1 d . . . N10 N 0.2983(3) 0.63262(19) 0.0711(3) 0.0349(9) Uani 1 1 d . . . N11 N 0.3654(3) 0.76553(19) 0.1100(3) 0.0360(9) Uani 1 1 d . . . N12 N 0.2840(3) 0.7760(2) 0.0302(3) 0.0409(10) Uani 1 1 d . . . F2 F 0.9228(5) 0.5996(4) 0.5890(7) 0.190(4) Uani 1 1 d D . . F3 F 0.8650(6) 0.5562(4) 0.6769(6) 0.181(3) Uani 1 1 d . . . F4 F 0.7835(8) 0.5651(4) 0.5252(7) 0.265(7) Uani 1 1 d D . . F5 F 0.7930(5) 0.6693(3) 0.5336(5) 0.159(3) Uani 1 1 d . . . F6 F 0.7258(4) 0.6134(5) 0.6097(8) 0.219(5) Uani 1 1 d D . . F7 F 0.7591(5) 0.8177(3) 0.6458(4) 0.123(2) Uani 1 1 d . . . F8 F 0.7521(3) 0.8653(2) 0.7746(2) 0.0769(12) Uani 1 1 d . . . F9 F 0.8141(3) 0.9203(3) 0.6830(3) 0.116(2) Uani 1 1 d . . . F10 F 0.6798(3) 0.9012(2) 0.5565(3) 0.0925(15) Uani 1 1 d . . . F11 F 0.6151(3) 0.8472(2) 0.6474(3) 0.0800(12) Uani 1 1 d . . . F12 F 0.6701(4) 0.9484(2) 0.6845(4) 0.1153(19) Uani 1 1 d . . . P1 P 0.82923(14) 0.61398(11) 0.60702(14) 0.0744(6) Uani 1 1 d D . . P2 P 0.71485(11) 0.88374(8) 0.66555(11) 0.0508(4) Uani 1 1 d . . . F1 F 0.8791(9) 0.6627(4) 0.6854(7) 0.314(9) Uani 1 1 d D . . C10 C 0.3640(5) 0.8282(3) 0.3203(5) 0.0691(19) Uani 1 1 d D . . H10A H 0.3304 0.8291 0.3638 0.083 Uiso 1 1 calc R . . H10B H 0.3183 0.8141 0.2590 0.083 Uiso 1 1 calc R . . C21 C 0.1983(5) 0.9083(3) 0.0976(5) 0.073(2) Uani 1 1 d D . . H21A H 0.2398 0.9399 0.0835 0.088 Uiso 1 1 calc R . . H21B H 0.2368 0.8695 0.1241 0.088 Uiso 1 1 calc R . . C11 C 0.4027(9) 0.8953(4) 0.3129(9) 0.147(4) Uani 1 1 d DU . . H11A H 0.4594 0.9041 0.3683 0.220 Uiso 1 1 calc R . . H11B H 0.3537 0.9277 0.3073 0.220 Uiso 1 1 calc R . . H11C H 0.4196 0.8972 0.2582 0.220 Uiso 1 1 calc R . . C22 C 0.1615(14) 0.9372(9) 0.1685(11) 0.237(8) Uani 1 1 d DU . . H22A H 0.1092 0.9672 0.1372 0.356 Uiso 1 1 calc R . . H22B H 0.2134 0.9603 0.2161 0.356 Uiso 1 1 calc R . . H22C H 0.1383 0.9026 0.1973 0.356 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 0.0317(2) 0.0292(2) 0.0302(2) -0.00245(15) 0.00859(16) -0.00005(15) Pd2 0.0297(2) 0.0319(2) 0.0387(2) 0.00306(16) 0.01157(17) 0.00340(15) C1 0.104(6) 0.052(4) 0.083(5) -0.015(4) 0.029(5) -0.025(4) C2 0.067(4) 0.045(3) 0.062(4) -0.001(3) 0.022(3) -0.013(3) C3 0.045(3) 0.036(3) 0.036(3) -0.004(2) 0.013(2) 0.003(2) C4 0.096(6) 0.039(3) 0.066(4) 0.020(3) 0.025(4) 0.008(4) C5 0.082(5) 0.056(4) 0.054(4) 0.015(3) 0.016(4) 0.025(4) C6 0.040(3) 0.072(4) 0.042(3) 0.001(3) 0.008(3) 0.002(3) C7 0.041(3) 0.048(3) 0.032(3) -0.005(2) 0.011(2) -0.007(2) C8 0.061(4) 0.079(5) 0.042(3) -0.011(3) 0.001(3) -0.016(4) C9 0.088(5) 0.070(5) 0.049(4) -0.023(4) 0.007(4) -0.019(4) C12 0.082(5) 0.082(6) 0.099(6) 0.021(5) 0.027(5) -0.015(4) C13 0.079(5) 0.077(5) 0.062(4) 0.002(4) 0.040(4) -0.008(4) C14 0.043(4) 0.080(5) 0.102(6) -0.021(4) 0.042(4) -0.016(3) C15 0.033(3) 0.064(4) 0.093(5) -0.010(4) 0.016(3) -0.002(3) C16 0.035(3) 0.037(3) 0.053(3) -0.004(2) 0.018(3) 0.003(2) C17 0.052(4) 0.053(4) 0.047(3) 0.004(3) 0.002(3) 0.005(3) C18 0.047(3) 0.053(4) 0.073(4) 0.018(3) 0.013(3) 0.015(3) C19 0.054(4) 0.042(3) 0.082(5) 0.012(3) 0.018(4) 0.013(3) C20 0.033(3) 0.039(3) 0.050(3) 0.008(2) 0.015(2) 0.005(2) C23 0.048(3) 0.061(4) 0.052(3) -0.017(3) 0.001(3) -0.002(3) C24 0.041(3) 0.039(3) 0.036(3) -0.007(2) 0.008(2) -0.002(2) C25 0.050(3) 0.040(3) 0.043(3) -0.016(2) 0.012(3) 0.005(2) C26 0.039(3) 0.038(3) 0.038(3) -0.006(2) 0.010(2) 0.003(2) C27 0.044(3) 0.057(4) 0.065(4) -0.014(3) 0.014(3) 0.015(3) C28 0.062(5) 0.157(8) 0.082(5) 0.070(6) 0.033(4) 0.026(5) C29 0.046(3) 0.068(4) 0.067(4) 0.032(3) 0.028(3) 0.018(3) C30 0.051(4) 0.061(4) 0.076(4) 0.027(3) 0.036(3) 0.006(3) C31 0.042(3) 0.039(3) 0.061(4) -0.003(3) 0.025(3) -0.004(2) C32 0.043(3) 0.053(3) 0.071(4) -0.008(3) 0.021(3) -0.015(3) N1 0.063(3) 0.033(2) 0.051(3) 0.006(2) 0.020(2) 0.003(2) N2 0.053(3) 0.045(3) 0.039(2) 0.005(2) 0.012(2) 0.013(2) N3 0.043(3) 0.057(3) 0.036(2) -0.004(2) 0.006(2) -0.005(2) N4 0.065(3) 0.042(3) 0.049(3) -0.018(2) 0.014(3) -0.008(2) N5 0.041(3) 0.032(2) 0.064(3) 0.003(2) 0.011(2) 0.002(2) N6 0.038(2) 0.040(2) 0.056(3) 0.011(2) 0.010(2) 0.010(2) N7 0.032(2) 0.048(3) 0.063(3) -0.002(2) 0.010(2) 0.003(2) N8 0.048(3) 0.049(3) 0.059(3) -0.006(2) 0.029(2) -0.010(2) N9 0.036(2) 0.032(2) 0.034(2) -0.0021(18) 0.0061(19) 0.0056(18) N10 0.034(2) 0.030(2) 0.036(2) -0.0035(18) 0.0075(18) 0.0019(17) N11 0.035(2) 0.031(2) 0.042(2) -0.0001(18) 0.014(2) -0.0011(17) N12 0.034(2) 0.042(2) 0.048(3) 0.013(2) 0.016(2) 0.0040(19) F2 0.158(7) 0.183(7) 0.286(11) 0.039(7) 0.150(8) 0.043(6) F3 0.182(7) 0.183(7) 0.180(7) 0.118(6) 0.068(6) 0.070(6) F4 0.214(10) 0.205(10) 0.249(11) -0.064(9) -0.059(9) 0.063(8) F5 0.121(5) 0.140(5) 0.181(7) 0.093(5) 0.017(5) 0.008(4) F6 0.131(6) 0.267(11) 0.307(12) 0.135(9) 0.137(7) 0.069(6) F7 0.169(6) 0.105(4) 0.124(4) 0.019(3) 0.090(4) 0.063(4) F8 0.055(2) 0.124(4) 0.049(2) 0.021(2) 0.0167(18) 0.007(2) F9 0.056(2) 0.188(6) 0.082(3) 0.044(3) 0.001(2) -0.044(3) F10 0.094(3) 0.104(3) 0.057(2) 0.024(2) 0.003(2) -0.026(3) F11 0.072(3) 0.090(3) 0.072(3) -0.003(2) 0.020(2) -0.033(2) F12 0.105(4) 0.068(3) 0.142(5) -0.029(3) 0.010(3) 0.015(3) P1 0.0624(11) 0.0857(14) 0.0689(12) 0.0232(11) 0.0176(10) 0.0195(10) P2 0.0428(8) 0.0542(9) 0.0497(9) 0.0088(7) 0.0107(7) -0.0003(7) F1 0.381(16) 0.173(8) 0.178(8) -0.101(7) -0.133(10) 0.103(9) C10 0.079(5) 0.048(4) 0.077(5) -0.021(3) 0.025(4) 0.004(3) C21 0.055(4) 0.047(4) 0.087(5) -0.001(4) -0.007(4) 0.000(3) C11 0.147(5) 0.146(5) 0.147(5) -0.0003(10) 0.0548(19) 0.0006(10) C22 0.237(8) 0.237(8) 0.237(8) -0.0009(10) 0.089(3) 0.0008(10) _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 C7 1.983(5) . ? Pd1 C3 2.003(5) . ? Pd1 N10 2.049(4) . ? Pd1 N11 2.072(4) . ? Pd2 C16 1.991(5) . ? Pd2 C20 1.992(5) . ? Pd2 N12 2.057(4) . ? Pd2 N9 2.064(4) . ? C1 C2 1.525(9) . ? C2 N1 1.472(8) . ? C3 N1 1.336(7) . ? C3 N2 1.359(7) . ? C4 C5 1.333(10) . ? C4 N1 1.379(8) . ? C5 N2 1.377(8) . ? C6 N2 1.440(8) . ? C6 N3 1.447(8) . ? C7 N4 1.343(7) . ? C7 N3 1.350(7) . ? C8 C9 1.318(10) . ? C8 N3 1.379(8) . ? C9 N4 1.392(8) . ? C12 C13 1.506(10) . ? C13 N8 1.457(8) . ? C14 C15 1.320(10) . ? C14 N8 1.395(8) . ? C15 N7 1.381(8) . ? C16 N8 1.340(7) . ? C16 N7 1.349(7) . ? C17 N7 1.440(8) . ? C17 N6 1.443(8) . ? C18 C19 1.320(9) . ? C18 N6 1.371(7) . ? C19 N5 1.384(7) . ? C20 N5 1.330(7) . ? C20 N6 1.352(7) . ? C23 C24 1.493(7) . ? C24 N9 1.348(6) . ? C24 C25 1.373(7) . ? C25 C26 1.381(7) . ? C26 N10 1.349(6) . ? C26 C27 1.489(7) . ? C28 C29 1.513(9) . ? C29 N12 1.344(7) . ? C29 C30 1.363(9) . ? C30 C31 1.388(8) . ? C31 N11 1.342(7) . ? C31 C32 1.496(8) . ? N4 C10 1.461(8) . ? N5 C21 1.455(8) . ? N9 N10 1.369(5) . ? N11 N12 1.372(6) . ? F2 P1 1.540(4) . ? F3 P1 1.543(6) . ? F4 P1 1.542(5) . ? F5 P1 1.536(6) . ? F6 P1 1.550(4) . ? F7 P2 1.572(5) . ? F8 P2 1.593(4) . ? F9 P2 1.579(4) . ? F10 P2 1.590(4) . ? F11 P2 1.582(4) . ? F12 P2 1.549(5) . ? P1 F1 1.517(4) . ? C10 C11 1.502(5) . ? C21 C22 1.505(5) . ? 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 C7 Pd1 C3 84.5(2) . . ? C7 Pd1 N10 177.3(2) . . ? C3 Pd1 N10 92.97(18) . . ? C7 Pd1 N11 94.30(19) . . ? C3 Pd1 N11 170.97(19) . . ? N10 Pd1 N11 88.09(16) . . ? C16 Pd2 C20 83.1(2) . . ? C16 Pd2 N12 174.42(19) . . ? C20 Pd2 N12 91.74(19) . . ? C16 Pd2 N9 96.28(19) . . ? C20 Pd2 N9 168.3(2) . . ? N12 Pd2 N9 88.33(17) . . ? N1 C2 C1 112.5(6) . . ? N1 C3 N2 104.8(5) . . ? N1 C3 Pd1 135.2(4) . . ? N2 C3 Pd1 120.0(4) . . ? C5 C4 N1 107.3(6) . . ? C4 C5 N2 106.5(6) . . ? N2 C6 N3 108.9(5) . . ? N4 C7 N3 104.0(4) . . ? N4 C7 Pd1 133.9(4) . . ? N3 C7 Pd1 122.0(4) . . ? C9 C8 N3 105.5(6) . . ? C8 C9 N4 108.2(6) . . ? N8 C13 C12 111.7(6) . . ? C15 C14 N8 108.7(6) . . ? C14 C15 N7 105.7(6) . . ? N8 C16 N7 105.6(5) . . ? N8 C16 Pd2 134.3(4) . . ? N7 C16 Pd2 120.2(4) . . ? N7 C17 N6 108.3(5) . . ? C19 C18 N6 106.2(5) . . ? C18 C19 N5 108.0(6) . . ? N5 C20 N6 105.2(4) . . ? N5 C20 Pd2 135.0(4) . . ? N6 C20 Pd2 119.1(4) . . ? N9 C24 C25 108.7(4) . . ? N9 C24 C23 124.3(5) . . ? C25 C24 C23 127.1(5) . . ? C24 C25 C26 106.6(4) . . ? N10 C26 C25 108.4(4) . . ? N10 C26 C27 122.6(5) . . ? C25 C26 C27 128.9(5) . . ? N12 C29 C30 109.5(5) . . ? N12 C29 C28 121.3(6) . . ? C30 C29 C28 129.0(6) . . ? C29 C30 C31 105.9(5) . . ? N11 C31 C30 108.9(5) . . ? N11 C31 C32 123.8(5) . . ? C30 C31 C32 127.3(5) . . ? C3 N1 C4 110.7(5) . . ? C3 N1 C2 126.4(5) . . ? C4 N1 C2 122.8(5) . . ? C3 N2 C5 110.6(5) . . ? C3 N2 C6 123.1(5) . . ? C5 N2 C6 126.3(5) . . ? C7 N3 C8 112.2(5) . . ? C7 N3 C6 121.5(5) . . ? C8 N3 C6 126.3(5) . . ? C7 N4 C9 110.0(6) . . ? C7 N4 C10 126.6(5) . . ? C9 N4 C10 123.4(5) . . ? C20 N5 C19 109.8(5) . . ? C20 N5 C21 125.8(5) . . ? C19 N5 C21 124.4(5) . . ? C20 N6 C18 110.9(5) . . ? C20 N6 C17 122.8(4) . . ? C18 N6 C17 126.4(5) . . ? C16 N7 C15 111.1(5) . . ? C16 N7 C17 122.2(5) . . ? C15 N7 C17 126.5(5) . . ? C16 N8 C14 108.9(6) . . ? C16 N8 C13 125.1(5) . . ? C14 N8 C13 126.0(6) . . ? C24 N9 N10 108.2(4) . . ? C24 N9 Pd2 124.6(3) . . ? N10 N9 Pd2 121.4(3) . . ? C26 N10 N9 108.1(4) . . ? C26 N10 Pd1 129.5(3) . . ? N9 N10 Pd1 122.0(3) . . ? C31 N11 N12 107.8(4) . . ? C31 N11 Pd1 127.6(4) . . ? N12 N11 Pd1 120.8(3) . . ? C29 N12 N11 107.9(4) . . ? C29 N12 Pd2 128.7(4) . . ? N11 N12 Pd2 122.8(3) . . ? F1 P1 F5 91.8(5) . . ? F1 P1 F2 93.6(7) . . ? F5 P1 F2 95.7(5) . . ? F1 P1 F4 176.6(9) . . ? F5 P1 F4 87.3(5) . . ? F2 P1 F4 83.2(6) . . ? F1 P1 F3 90.7(5) . . ? F5 P1 F3 177.3(5) . . ? F2 P1 F3 83.2(4) . . ? F4 P1 F3 90.1(6) . . ? F1 P1 F6 100.1(8) . . ? F5 P1 F6 87.0(4) . . ? F2 P1 F6 165.9(6) . . ? F4 P1 F6 83.1(6) . . ? F3 P1 F6 93.5(4) . . ? F12 P2 F7 179.3(4) . . ? F12 P2 F9 90.3(3) . . ? F7 P2 F9 90.4(4) . . ? F12 P2 F11 89.6(3) . . ? F7 P2 F11 89.7(3) . . ? F9 P2 F11 179.7(3) . . ? F12 P2 F10 90.8(3) . . ? F7 P2 F10 89.1(3) . . ? F9 P2 F10 89.3(2) . . ? F11 P2 F10 90.3(2) . . ? F12 P2 F8 90.4(3) . . ? F7 P2 F8 89.7(3) . . ? F9 P2 F8 90.0(2) . . ? F11 P2 F8 90.3(2) . . ? F10 P2 F8 178.6(3) . . ? N4 C10 C11 108.3(7) . . ? N5 C21 C22 110.7(9) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.501 _refine_diff_density_min -0.892 _refine_diff_density_rms 0.108 #===END data_9 _database_code_depnum_ccdc_archive 'CCDC 894018' #TrackingRef 'web_deposit_cif_file_0_ChaoChen_1346500744.1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H32 F12 N8 P2 Pd' _chemical_formula_weight 804.90 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' F F 0.0171 0.0103 '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' 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' _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 7.9986(5) _cell_length_b 10.1660(7) _cell_length_c 11.0073(7) _cell_angle_alpha 62.877(7) _cell_angle_beta 76.974(6) _cell_angle_gamma 89.553(5) _cell_volume 771.45(9) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2776 _cell_measurement_theta_min 2.9454 _cell_measurement_theta_max 29.5117 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.733 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 404 _exptl_absorpt_coefficient_mu 0.807 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.816 _exptl_absorpt_correction_T_max 0.865 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'multiwire proportional' _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 5408 _diffrn_reflns_av_R_equivalents 0.0257 _diffrn_reflns_av_sigmaI/netI 0.0468 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.95 _diffrn_reflns_theta_max 25.01 _reflns_number_total 2722 _reflns_number_gt 2582 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker FRAMBO' _computing_cell_refinement 'Bruker FRAMBO' _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^)+(0.0478P)^2^+0.1948P] 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 2722 _refine_ls_number_parameters 207 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0411 _refine_ls_R_factor_gt 0.0378 _refine_ls_wR_factor_ref 0.0940 _refine_ls_wR_factor_gt 0.0911 _refine_ls_goodness_of_fit_ref 1.089 _refine_ls_restrained_S_all 1.089 _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 Pd1 Pd 0.5000 0.0000 0.5000 0.02716(14) Uani 1 2 d S . . N1 N 0.3397(4) 0.2190(3) 0.6078(3) 0.0341(7) Uani 1 1 d . . . N2 N 0.4114(4) 0.3119(3) 0.3844(3) 0.0343(7) Uani 1 1 d . . . N3 N 0.3654(4) 0.1911(3) 0.2522(3) 0.0341(7) Uani 1 1 d . . . N4 N 0.2509(4) -0.0305(3) 0.3316(3) 0.0355(7) Uani 1 1 d . . . C1 C 0.4138(4) 0.1862(4) 0.5046(3) 0.0302(7) Uani 1 1 d . . . C2 C 0.3643(4) 0.0499(4) 0.3523(3) 0.0298(7) Uani 1 1 d . . . C5 C 0.4038(6) 0.1635(6) 0.8362(4) 0.0584(12) Uani 1 1 d . . . H5A H 0.3817 0.2625 0.8196 0.088 Uiso 1 1 calc R . . H5B H 0.5249 0.1620 0.8020 0.088 Uiso 1 1 calc R . . H5C H 0.3686 0.0969 0.9355 0.088 Uiso 1 1 calc R . . C6 C 0.3035(5) 0.1152(4) 0.7600(4) 0.0434(9) Uani 1 1 d . . . H6A H 0.3317 0.0176 0.7726 0.052 Uiso 1 1 calc R . . H6B H 0.1810 0.1069 0.8018 0.052 Uiso 1 1 calc R . . C7 C 0.2914(5) 0.3614(4) 0.5536(4) 0.0467(10) Uani 1 1 d . . . H7 H 0.2380 0.4082 0.6052 0.056 Uiso 1 1 calc R . . C8 C 0.3352(5) 0.4191(4) 0.4141(4) 0.0455(10) Uani 1 1 d . . . H8 H 0.3178 0.5133 0.3493 0.055 Uiso 1 1 calc R . . C9 C 0.4633(5) 0.3148(4) 0.2467(3) 0.0399(9) Uani 1 1 d . . . H9A H 0.4407 0.4081 0.1743 0.048 Uiso 1 1 calc R . . H9B H 0.5859 0.3061 0.2238 0.048 Uiso 1 1 calc R . . C10 C 0.2543(5) 0.1979(5) 0.1705(4) 0.0451(10) Uani 1 1 d . . . H10 H 0.2328 0.2826 0.0957 0.054 Uiso 1 1 calc R . . C11 C 0.1840(5) 0.0592(5) 0.2200(4) 0.0458(10) Uani 1 1 d . . . H11 H 0.1045 0.0286 0.1855 0.055 Uiso 1 1 calc R . . C12 C 0.1916(5) -0.1890(4) 0.4250(4) 0.0459(10) Uani 1 1 d . . . H12A H 0.2904 -0.2425 0.4479 0.055 Uiso 1 1 calc R . . H12B H 0.1379 -0.2285 0.3761 0.055 Uiso 1 1 calc R . . C13 C 0.0646(7) -0.2138(6) 0.5591(5) 0.0757(15) Uani 1 1 d . . . H13A H -0.0347 -0.1631 0.5370 0.114 Uiso 1 1 calc R . . H13B H 0.1178 -0.1758 0.6084 0.114 Uiso 1 1 calc R . . H13C H 0.0296 -0.3184 0.6176 0.114 Uiso 1 1 calc R . . P1 P 0.12267(14) 0.68667(12) 0.07143(11) 0.0445(3) Uani 1 1 d . . . F1 F 0.3162(5) 0.7444(6) 0.0311(5) 0.1464(18) Uani 1 1 d . . . F2 F -0.0726(4) 0.6293(5) 0.1109(4) 0.1142(12) Uani 1 1 d . . . F3 F 0.1761(6) 0.5294(4) 0.1040(4) 0.1276(14) Uani 1 1 d . . . F4 F 0.0661(6) 0.8447(4) 0.0406(4) 0.1326(17) Uani 1 1 d . . . F5 F 0.1401(5) 0.7274(5) -0.0865(3) 0.1099(13) Uani 1 1 d . . . F6 F 0.1025(5) 0.6491(5) 0.2294(3) 0.1130(13) 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 Pd1 0.0292(2) 0.0307(2) 0.0258(2) -0.01447(16) -0.01191(15) 0.00976(15) N1 0.0375(17) 0.0335(16) 0.0354(15) -0.0192(13) -0.0099(13) 0.0087(13) N2 0.0395(17) 0.0327(16) 0.0317(15) -0.0133(12) -0.0143(13) 0.0097(13) N3 0.0362(17) 0.0404(17) 0.0274(14) -0.0157(13) -0.0115(13) 0.0102(13) N4 0.0342(17) 0.0475(19) 0.0345(15) -0.0254(14) -0.0131(13) 0.0082(14) C1 0.0300(19) 0.0332(19) 0.0314(17) -0.0164(15) -0.0120(15) 0.0063(15) C2 0.0307(19) 0.0357(19) 0.0280(16) -0.0183(15) -0.0093(14) 0.0109(15) C5 0.059(3) 0.084(3) 0.044(2) -0.039(2) -0.015(2) 0.015(2) C6 0.046(2) 0.050(2) 0.0328(19) -0.0205(17) -0.0046(17) 0.0069(19) C7 0.057(3) 0.048(2) 0.052(2) -0.035(2) -0.019(2) 0.022(2) C8 0.059(3) 0.030(2) 0.053(2) -0.0201(17) -0.023(2) 0.0185(18) C9 0.048(2) 0.040(2) 0.0283(18) -0.0125(15) -0.0103(16) 0.0108(17) C10 0.052(2) 0.063(3) 0.0308(18) -0.0245(19) -0.0236(18) 0.027(2) C11 0.045(2) 0.067(3) 0.045(2) -0.036(2) -0.0274(19) 0.019(2) C12 0.044(2) 0.050(2) 0.055(2) -0.032(2) -0.0171(19) 0.0038(19) C13 0.067(3) 0.064(3) 0.074(3) -0.029(3) 0.016(3) -0.016(3) P1 0.0486(7) 0.0464(6) 0.0434(6) -0.0225(5) -0.0177(5) 0.0181(5) F1 0.058(2) 0.236(5) 0.186(4) -0.138(4) -0.016(2) -0.017(3) F2 0.059(2) 0.160(4) 0.123(3) -0.068(3) -0.0167(19) -0.003(2) F3 0.181(4) 0.073(2) 0.147(3) -0.059(2) -0.059(3) 0.070(2) F4 0.187(4) 0.058(2) 0.109(3) -0.0265(19) 0.014(3) 0.045(2) F5 0.117(3) 0.165(4) 0.0594(18) -0.058(2) -0.0325(19) 0.057(3) F6 0.153(3) 0.150(3) 0.0633(19) -0.062(2) -0.053(2) 0.058(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 C1 2.028(3) 2_656 ? Pd1 C1 2.028(3) . ? Pd1 C2 2.028(3) . ? Pd1 C2 2.028(3) 2_656 ? N1 C1 1.339(4) . ? N1 C7 1.382(5) . ? N1 C6 1.476(4) . ? N2 C1 1.361(4) . ? N2 C8 1.375(5) . ? N2 C9 1.466(4) . ? N3 C2 1.352(4) . ? N3 C10 1.380(4) . ? N3 C9 1.457(5) . ? N4 C2 1.347(4) . ? N4 C11 1.376(4) . ? N4 C12 1.470(5) . ? C5 C6 1.508(5) . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C8 1.328(5) . ? C7 H7 0.9300 . ? C8 H8 0.9300 . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C11 1.333(6) . ? C10 H10 0.9300 . ? C11 H11 0.9300 . ? C12 C13 1.504(6) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? P1 F3 1.550(3) . ? P1 F1 1.551(3) . ? P1 F2 1.564(3) . ? P1 F5 1.564(3) . ? P1 F4 1.569(3) . ? P1 F6 1.569(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 C1 Pd1 C1 180.000(1) 2_656 . ? C1 Pd1 C2 96.37(12) 2_656 . ? C1 Pd1 C2 83.63(12) . . ? C1 Pd1 C2 83.63(12) 2_656 2_656 ? C1 Pd1 C2 96.37(12) . 2_656 ? C2 Pd1 C2 180.0 . 2_656 ? C1 N1 C7 111.1(3) . . ? C1 N1 C6 125.2(3) . . ? C7 N1 C6 123.7(3) . . ? C1 N2 C8 111.3(3) . . ? C1 N2 C9 120.8(3) . . ? C8 N2 C9 127.4(3) . . ? C2 N3 C10 111.0(3) . . ? C2 N3 C9 121.2(3) . . ? C10 N3 C9 127.6(3) . . ? C2 N4 C11 110.8(3) . . ? C2 N4 C12 124.6(3) . . ? C11 N4 C12 124.2(3) . . ? N1 C1 N2 104.0(3) . . ? N1 C1 Pd1 134.2(3) . . ? N2 C1 Pd1 121.7(2) . . ? N4 C2 N3 104.4(3) . . ? N4 C2 Pd1 133.6(2) . . ? N3 C2 Pd1 121.8(2) . . ? C6 C5 H5A 109.5 . . ? C6 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C6 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N1 C6 C5 112.9(3) . . ? N1 C6 H6A 109.0 . . ? C5 C6 H6A 109.0 . . ? N1 C6 H6B 109.0 . . ? C5 C6 H6B 109.0 . . ? H6A C6 H6B 107.8 . . ? C8 C7 N1 107.3(3) . . ? C8 C7 H7 126.4 . . ? N1 C7 H7 126.4 . . ? C7 C8 N2 106.4(3) . . ? C7 C8 H8 126.8 . . ? N2 C8 H8 126.8 . . ? N3 C9 N2 108.7(3) . . ? N3 C9 H9A 109.9 . . ? N2 C9 H9A 109.9 . . ? N3 C9 H9B 109.9 . . ? N2 C9 H9B 109.9 . . ? H9A C9 H9B 108.3 . . ? C11 C10 N3 106.5(3) . . ? C11 C10 H10 126.8 . . ? N3 C10 H10 126.8 . . ? C10 C11 N4 107.3(3) . . ? C10 C11 H11 126.3 . . ? N4 C11 H11 126.3 . . ? N4 C12 C13 111.9(3) . . ? N4 C12 H12A 109.2 . . ? C13 C12 H12A 109.2 . . ? N4 C12 H12B 109.2 . . ? C13 C12 H12B 109.2 . . ? H12A C12 H12B 107.9 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? F3 P1 F1 88.8(3) . . ? F3 P1 F2 91.4(3) . . ? F1 P1 F2 179.6(3) . . ? F3 P1 F5 91.1(2) . . ? F1 P1 F5 88.4(2) . . ? F2 P1 F5 91.2(2) . . ? F3 P1 F4 179.1(2) . . ? F1 P1 F4 91.9(3) . . ? F2 P1 F4 87.9(3) . . ? F5 P1 F4 89.5(2) . . ? F3 P1 F6 90.2(2) . . ? F1 P1 F6 92.0(2) . . ? F2 P1 F6 88.4(2) . . ? F5 P1 F6 178.6(2) . . ? F4 P1 F6 89.1(2) . . ? 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 C7 N1 C1 N2 0.3(4) . . . . ? C6 N1 C1 N2 176.7(3) . . . . ? C7 N1 C1 Pd1 -174.7(3) . . . . ? C6 N1 C1 Pd1 1.7(5) . . . . ? C8 N2 C1 N1 -0.6(4) . . . . ? C9 N2 C1 N1 -172.7(3) . . . . ? C8 N2 C1 Pd1 175.2(2) . . . . ? C9 N2 C1 Pd1 3.1(4) . . . . ? C1 Pd1 C1 N1 -150(100) 2_656 . . . ? C2 Pd1 C1 N1 132.0(3) . . . . ? C2 Pd1 C1 N1 -48.0(3) 2_656 . . . ? C1 Pd1 C1 N2 36(100) 2_656 . . . ? C2 Pd1 C1 N2 -42.3(3) . . . . ? C2 Pd1 C1 N2 137.7(3) 2_656 . . . ? C11 N4 C2 N3 0.5(4) . . . . ? C12 N4 C2 N3 -173.1(3) . . . . ? C11 N4 C2 Pd1 175.4(3) . . . . ? C12 N4 C2 Pd1 1.9(5) . . . . ? C10 N3 C2 N4 -0.1(4) . . . . ? C9 N3 C2 N4 175.0(3) . . . . ? C10 N3 C2 Pd1 -175.8(2) . . . . ? C9 N3 C2 Pd1 -0.6(4) . . . . ? C1 Pd1 C2 N4 47.0(3) 2_656 . . . ? C1 Pd1 C2 N4 -133.0(3) . . . . ? C2 Pd1 C2 N4 134(100) 2_656 . . . ? C1 Pd1 C2 N3 -138.7(3) 2_656 . . . ? C1 Pd1 C2 N3 41.3(3) . . . . ? C2 Pd1 C2 N3 -52(100) 2_656 . . . ? C1 N1 C6 C5 115.9(4) . . . . ? C7 N1 C6 C5 -68.1(5) . . . . ? C1 N1 C7 C8 0.2(4) . . . . ? C6 N1 C7 C8 -176.3(3) . . . . ? N1 C7 C8 N2 -0.6(4) . . . . ? C1 N2 C8 C7 0.8(4) . . . . ? C9 N2 C8 C7 172.2(3) . . . . ? C2 N3 C9 N2 -54.2(4) . . . . ? C10 N3 C9 N2 120.0(4) . . . . ? C1 N2 C9 N3 52.7(4) . . . . ? C8 N2 C9 N3 -118.0(4) . . . . ? C2 N3 C10 C11 -0.3(4) . . . . ? C9 N3 C10 C11 -175.1(3) . . . . ? N3 C10 C11 N4 0.6(4) . . . . ? C2 N4 C11 C10 -0.7(4) . . . . ? C12 N4 C11 C10 172.9(3) . . . . ? C2 N4 C12 C13 75.0(5) . . . . ? C11 N4 C12 C13 -97.8(4) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.631 _refine_diff_density_min -0.529 _refine_diff_density_rms 0.087 #===END data_10 _database_code_depnum_ccdc_archive 'CCDC 894019' #TrackingRef 'web_deposit_cif_file_0_ChaoChen_1346500744.1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C15 H27 F12 N9 P2 Pd' _chemical_formula_weight 729.80 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' F F 0.0171 0.0103 '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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.4130(5) _cell_length_b 11.0655(5) _cell_length_c 13.8876(6) _cell_angle_alpha 87.178(4) _cell_angle_beta 83.506(4) _cell_angle_gamma 72.214(4) _cell_volume 1368.39(11) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5289 _cell_measurement_theta_min 2.8395 _cell_measurement_theta_max 29.6464 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.771 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 728 _exptl_absorpt_coefficient_mu 0.901 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7259 _exptl_absorpt_correction_T_max 0.8196 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'multiwire proportional' _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 10615 _diffrn_reflns_av_R_equivalents 0.0289 _diffrn_reflns_av_sigmaI/netI 0.0374 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.85 _diffrn_reflns_theta_max 25.01 _reflns_number_total 4825 _reflns_number_gt 4172 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker FRAMBO' _computing_cell_refinement 'Bruker FRAMBO' _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^)+(0.0366P)^2^+1.0866P] 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 4825 _refine_ls_number_parameters 356 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0434 _refine_ls_R_factor_gt 0.0344 _refine_ls_wR_factor_ref 0.0842 _refine_ls_wR_factor_gt 0.0783 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.045 _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 F10 F 0.9484(4) 0.2531(3) 0.7543(2) 0.1022(10) Uani 1 1 d . . . Pd1 Pd 0.60357(3) 0.81046(2) 0.693446(17) 0.03243(10) Uani 1 1 d . . . P2 P 0.93290(11) 0.34170(10) 0.84331(7) 0.0449(2) Uani 1 1 d . . . P1 P 0.23413(11) 0.75091(9) 0.54852(7) 0.0464(2) Uani 1 1 d . . . N1 N 0.7266(3) 0.7848(3) 0.56090(19) 0.0387(7) Uani 1 1 d . . . C4 C 0.4629(4) 0.8375(3) 0.8143(2) 0.0363(8) Uani 1 1 d . . . N4 N 0.6303(3) 0.6185(3) 0.6710(2) 0.0404(7) Uani 1 1 d . . . H4A H 0.6751 0.5707 0.7198 0.048 Uiso 1 1 calc R . . H4B H 0.5401 0.6067 0.6693 0.048 Uiso 1 1 calc R . . N6 N 0.4420(3) 1.0774(3) 0.7279(2) 0.0386(7) Uani 1 1 d . . . C3 C 0.5784(4) 0.9925(3) 0.7083(2) 0.0351(7) Uani 1 1 d . . . N8 N 0.4592(3) 0.7777(3) 0.9000(2) 0.0442(7) Uani 1 1 d . . . N7 N 0.3364(3) 0.9392(3) 0.8205(2) 0.0398(7) Uani 1 1 d . . . N5 N 0.6764(3) 1.0569(3) 0.7115(2) 0.0381(7) Uani 1 1 d . . . C7 C 0.6024(4) 1.1825(3) 0.7331(3) 0.0467(9) Uani 1 1 d . . . H7 H 0.6463 1.2462 0.7388 0.056 Uiso 1 1 calc R . . F9 F 0.0980(3) 0.7007(3) 0.5881(2) 0.0891(9) Uani 1 1 d . . . C1 C 0.7571(4) 0.6723(3) 0.5266(2) 0.0417(8) Uani 1 1 d . . . F3 F 1.1021(3) 0.3350(3) 0.8157(2) 0.0786(8) Uani 1 1 d . . . N3 N 0.7191(4) 0.5824(3) 0.5822(2) 0.0501(8) Uani 1 1 d . . . H3 H 0.7481 0.5046 0.5642 0.060 Uiso 1 1 calc R . . F7 F 0.3676(3) 0.8039(3) 0.5099(2) 0.0919(9) Uani 1 1 d . . . F1 F 0.8841(3) 0.4633(3) 0.7767(2) 0.0937(9) Uani 1 1 d . . . F5 F 0.7641(3) 0.3475(3) 0.8690(3) 0.1050(11) Uani 1 1 d . . . F2 F 0.9241(4) 0.4293(3) 0.9295(2) 0.0939(10) Uani 1 1 d . . . F4 F 0.9828(4) 0.2197(3) 0.9104(2) 0.0953(10) Uani 1 1 d . . . N2 N 0.7662(4) 0.8760(3) 0.4962(2) 0.0586(9) Uani 1 1 d . . . H2A H 0.8076 0.8544 0.4386 0.070 Uiso 1 1 calc R . . H2B H 0.7488 0.9526 0.5147 0.070 Uiso 1 1 calc R . . C9 C 0.3096(4) 1.0362(3) 0.7451(3) 0.0438(9) Uani 1 1 d . . . H9A H 0.2912 1.0022 0.6863 0.053 Uiso 1 1 calc R . . H9B H 0.2228 1.1071 0.7655 0.053 Uiso 1 1 calc R . . C6 C 0.8403(4) 0.9995(4) 0.7055(3) 0.0497(10) Uani 1 1 d . . . H6A H 0.8885 1.0585 0.6730 0.060 Uiso 1 1 calc R . . H6B H 0.8688 0.9234 0.6670 0.060 Uiso 1 1 calc R . . F6 F 0.3450(4) 0.6188(3) 0.5762(3) 0.1090(11) Uani 1 1 d . . . C10 C 0.2572(4) 0.9412(4) 0.9105(3) 0.0520(10) Uani 1 1 d . . . H10 H 0.1677 1.0011 0.9327 0.062 Uiso 1 1 calc R . . C8 C 0.4561(4) 1.1949(3) 0.7441(3) 0.0459(9) Uani 1 1 d . . . H8 H 0.3785 1.2687 0.7597 0.055 Uiso 1 1 calc R . . F8 F 0.2332(4) 0.6974(3) 0.4460(2) 0.1012(10) Uani 1 1 d . . . F12 F 0.2378(4) 0.7993(3) 0.6524(2) 0.1108(12) Uani 1 1 d . . . F13 F 0.1219(4) 0.8808(3) 0.5218(3) 0.1105(12) Uani 1 1 d . . . C12 C 0.5813(5) 0.6717(4) 0.9331(3) 0.0557(10) Uani 1 1 d . . . H12A H 0.6363 0.6219 0.8778 0.067 Uiso 1 1 calc R . . H12B H 0.5391 0.6172 0.9765 0.067 Uiso 1 1 calc R . . C11 C 0.3340(5) 0.8407(4) 0.9595(3) 0.0565(11) Uani 1 1 d . . . H11 H 0.3077 0.8171 1.0226 0.068 Uiso 1 1 calc R . . C2 C 0.8394(5) 0.6320(4) 0.4299(3) 0.0634(12) Uani 1 1 d . . . H2D H 0.7928 0.6904 0.3810 0.095 Uiso 1 1 calc R . . H2E H 0.8369 0.5484 0.4167 0.095 Uiso 1 1 calc R . . H2F H 0.9417 0.6313 0.4296 0.095 Uiso 1 1 calc R . . C15 C 0.2925(6) 0.5552(4) 0.8188(3) 0.0652(12) Uani 1 1 d . . . C16 C 0.1363(6) 0.6268(5) 0.8358(4) 0.0782(14) Uani 1 1 d . . . H16A H 0.0909 0.6363 0.7762 0.117 Uiso 1 1 calc R . . H16B H 0.1273 0.7091 0.8596 0.117 Uiso 1 1 calc R . . H16C H 0.0865 0.5829 0.8829 0.117 Uiso 1 1 calc R . . N9 N 0.4154(6) 0.4998(5) 0.8043(4) 0.0974(15) Uani 1 1 d . . . C13 C 0.6856(6) 0.7158(5) 0.9839(4) 0.0935(18) Uani 1 1 d . . . H13A H 0.7304 0.7673 0.9404 0.140 Uiso 1 1 calc R . . H13B H 0.7627 0.6439 1.0053 0.140 Uiso 1 1 calc R . . H13C H 0.6316 0.7650 1.0388 0.140 Uiso 1 1 calc R . . C5 C 0.8938(5) 0.9665(5) 0.8026(3) 0.0706(13) Uani 1 1 d . . . H5A H 0.8657 1.0416 0.8410 0.106 Uiso 1 1 calc R . . H5B H 1.0011 0.9310 0.7957 0.106 Uiso 1 1 calc R . . H5C H 0.8495 0.9055 0.8340 0.106 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 F10 0.123(3) 0.111(3) 0.089(2) -0.0382(19) -0.0087(19) -0.056(2) Pd1 0.03132(15) 0.02714(15) 0.03727(15) -0.00381(10) -0.00254(10) -0.00638(10) P2 0.0373(5) 0.0430(6) 0.0517(5) -0.0029(4) -0.0046(4) -0.0080(4) P1 0.0503(6) 0.0400(6) 0.0523(6) -0.0016(4) -0.0088(5) -0.0170(4) N1 0.0444(16) 0.0323(16) 0.0391(15) -0.0031(12) 0.0009(13) -0.0125(13) C4 0.0366(18) 0.0307(18) 0.0413(18) -0.0012(15) -0.0054(15) -0.0091(14) N4 0.0406(16) 0.0304(16) 0.0484(16) -0.0016(13) -0.0003(14) -0.0093(13) N6 0.0376(15) 0.0302(16) 0.0462(16) -0.0031(12) -0.0046(13) -0.0073(12) C3 0.0363(18) 0.0342(19) 0.0343(16) -0.0035(14) -0.0021(14) -0.0100(15) N8 0.0472(18) 0.0381(17) 0.0442(16) 0.0035(13) -0.0023(14) -0.0097(14) N7 0.0328(15) 0.0378(17) 0.0459(16) -0.0033(13) -0.0003(13) -0.0072(13) N5 0.0378(15) 0.0351(16) 0.0421(15) -0.0071(12) 0.0003(13) -0.0128(13) C7 0.058(2) 0.032(2) 0.054(2) -0.0065(16) -0.0022(19) -0.0207(17) F9 0.0777(18) 0.097(2) 0.109(2) 0.0137(18) -0.0080(16) -0.0538(17) C1 0.043(2) 0.040(2) 0.0400(18) -0.0048(16) -0.0047(16) -0.0088(16) F3 0.0423(13) 0.083(2) 0.106(2) -0.0151(16) 0.0043(13) -0.0144(13) N3 0.064(2) 0.0323(17) 0.0477(17) -0.0114(14) 0.0045(16) -0.0070(15) F7 0.0803(19) 0.110(2) 0.100(2) -0.0073(18) 0.0110(16) -0.0572(18) F1 0.0814(19) 0.083(2) 0.106(2) 0.0399(17) -0.0252(17) -0.0095(16) F5 0.0458(15) 0.110(3) 0.156(3) 0.015(2) 0.0050(17) -0.0278(15) F2 0.122(2) 0.086(2) 0.0674(16) -0.0337(15) 0.0029(16) -0.0219(18) F4 0.101(2) 0.0648(19) 0.104(2) 0.0277(16) -0.0070(18) -0.0074(16) N2 0.091(3) 0.050(2) 0.0402(17) -0.0027(15) 0.0068(17) -0.0322(19) C9 0.0320(18) 0.037(2) 0.058(2) 0.0007(17) -0.0077(16) -0.0032(15) C6 0.0370(19) 0.058(3) 0.056(2) -0.0135(19) 0.0040(18) -0.0189(18) F6 0.094(2) 0.065(2) 0.157(3) 0.0202(19) -0.043(2) -0.0011(17) C10 0.037(2) 0.058(3) 0.055(2) -0.007(2) 0.0126(18) -0.0119(18) C8 0.053(2) 0.0288(19) 0.052(2) -0.0046(16) -0.0007(18) -0.0069(16) F8 0.155(3) 0.107(2) 0.0625(16) -0.0148(16) -0.0133(18) -0.068(2) F12 0.179(3) 0.127(3) 0.0613(16) -0.0238(17) 0.0009(19) -0.100(3) F13 0.088(2) 0.0609(19) 0.168(3) 0.032(2) -0.016(2) -0.0046(16) C12 0.069(3) 0.041(2) 0.050(2) 0.0083(18) -0.011(2) -0.006(2) C11 0.059(3) 0.059(3) 0.047(2) 0.000(2) 0.013(2) -0.018(2) C2 0.082(3) 0.055(3) 0.049(2) -0.013(2) 0.010(2) -0.017(2) C15 0.082(3) 0.047(3) 0.073(3) 0.005(2) -0.007(3) -0.031(3) C16 0.084(4) 0.065(3) 0.081(3) 0.009(3) -0.004(3) -0.020(3) N9 0.086(3) 0.078(3) 0.129(4) 0.007(3) -0.005(3) -0.030(3) C13 0.090(4) 0.075(4) 0.110(4) -0.001(3) -0.050(3) -0.003(3) C5 0.056(3) 0.071(3) 0.078(3) 0.001(2) -0.015(2) -0.007(2) _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 F10 P2 1.581(3) . ? Pd1 C3 1.973(3) . ? Pd1 C4 1.992(3) . ? Pd1 N1 2.044(3) . ? Pd1 N4 2.097(3) . ? P2 F2 1.557(3) . ? P2 F5 1.571(3) . ? P2 F1 1.572(3) . ? P2 F3 1.575(3) . ? P2 F4 1.581(3) . ? P1 F13 1.558(3) . ? P1 F12 1.571(3) . ? P1 F8 1.571(3) . ? P1 F6 1.574(3) . ? P1 F7 1.574(3) . ? P1 F9 1.580(3) . ? N1 C1 1.291(4) . ? N1 N2 1.425(4) . ? C4 N8 1.335(4) . ? C4 N7 1.363(4) . ? N4 N3 1.411(4) . ? N6 C3 1.347(4) . ? N6 C8 1.378(4) . ? N6 C9 1.445(4) . ? C3 N5 1.333(4) . ? N8 C11 1.375(5) . ? N8 C12 1.467(5) . ? N7 C10 1.379(4) . ? N7 C9 1.448(4) . ? N5 C7 1.381(4) . ? N5 C6 1.472(4) . ? C7 C8 1.333(5) . ? C1 N3 1.339(5) . ? C1 C2 1.488(5) . ? C6 C5 1.483(6) . ? C10 C11 1.329(6) . ? C12 C13 1.478(7) . ? C15 N9 1.132(6) . ? C15 C16 1.440(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C3 Pd1 C4 82.40(13) . . ? C3 Pd1 N1 98.60(12) . . ? C4 Pd1 N1 173.29(13) . . ? C3 Pd1 N4 177.47(12) . . ? C4 Pd1 N4 99.58(12) . . ? N1 Pd1 N4 79.25(11) . . ? F2 P2 F5 91.16(19) . . ? F2 P2 F1 88.93(18) . . ? F5 P2 F1 90.16(17) . . ? F2 P2 F3 89.81(17) . . ? F5 P2 F3 178.97(19) . . ? F1 P2 F3 89.53(16) . . ? F2 P2 F4 90.92(18) . . ? F5 P2 F4 90.15(18) . . ? F1 P2 F4 179.7(2) . . ? F3 P2 F4 90.17(17) . . ? F2 P2 F10 177.65(19) . . ? F5 P2 F10 91.17(19) . . ? F1 P2 F10 90.75(19) . . ? F3 P2 F10 87.86(16) . . ? F4 P2 F10 89.40(19) . . ? F13 P1 F12 91.0(2) . . ? F13 P1 F8 91.1(2) . . ? F12 P1 F8 177.9(2) . . ? F13 P1 F6 178.9(2) . . ? F12 P1 F6 89.0(2) . . ? F8 P1 F6 88.9(2) . . ? F13 P1 F7 89.07(18) . . ? F12 P1 F7 89.39(17) . . ? F8 P1 F7 91.20(18) . . ? F6 P1 F7 91.99(19) . . ? F13 P1 F9 89.86(18) . . ? F12 P1 F9 89.93(18) . . ? F8 P1 F9 89.52(18) . . ? F6 P1 F9 89.08(19) . . ? F7 P1 F9 178.72(18) . . ? C1 N1 N2 115.5(3) . . ? C1 N1 Pd1 114.5(2) . . ? N2 N1 Pd1 129.4(2) . . ? N8 C4 N7 105.0(3) . . ? N8 C4 Pd1 135.3(2) . . ? N7 C4 Pd1 119.8(2) . . ? N3 N4 Pd1 108.5(2) . . ? C3 N6 C8 110.2(3) . . ? C3 N6 C9 120.5(3) . . ? C8 N6 C9 128.4(3) . . ? N5 C3 N6 105.6(3) . . ? N5 C3 Pd1 132.5(2) . . ? N6 C3 Pd1 121.6(2) . . ? C4 N8 C11 110.6(3) . . ? C4 N8 C12 125.4(3) . . ? C11 N8 C12 123.4(3) . . ? C4 N7 C10 110.2(3) . . ? C4 N7 C9 121.3(3) . . ? C10 N7 C9 127.9(3) . . ? C3 N5 C7 110.4(3) . . ? C3 N5 C6 124.7(3) . . ? C7 N5 C6 124.4(3) . . ? C8 C7 N5 106.9(3) . . ? N1 C1 N3 118.9(3) . . ? N1 C1 C2 124.6(4) . . ? N3 C1 C2 116.4(3) . . ? C1 N3 N4 118.4(3) . . ? N6 C9 N7 107.3(3) . . ? N5 C6 C5 112.0(3) . . ? C11 C10 N7 106.5(3) . . ? C7 C8 N6 106.8(3) . . ? N8 C12 C13 112.0(4) . . ? C10 C11 N8 107.7(3) . . ? N9 C15 C16 179.1(6) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.456 _refine_diff_density_min -0.502 _refine_diff_density_rms 0.077