# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Wanzhi Chen' _publ_contact_author_email CHENWZZ@ZJU.EDU.CN _publ_section_title ; Synthesis of Tetra- and Pentacoordinate Palladium Complexes of Functionalized N-Heterocyclic Carbenes and a Comparative Study of Their Catalytic Activities ; loop_ _publ_author_name 'Wanzhi Chen.' 'Qinqin Xia.' 'Xiaoming Zhang.' # Attachment 'xrd.cif' data_071213e _database_code_depnum_ccdc_archive 'CCDC 720713' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H40 F12 N8 P2 Pd' _chemical_formula_weight 957.08 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' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 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 17.283(2) _cell_length_b 11.3693(13) _cell_length_c 22.236(3) _cell_angle_alpha 90.00 _cell_angle_beta 109.000(2) _cell_angle_gamma 90.00 _cell_volume 4131.2(8) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.48 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.539 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1936 _exptl_absorpt_coefficient_mu 0.617 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7278 _exptl_absorpt_correction_T_max 0.7905 _exptl_absorpt_process_details Sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20274 _diffrn_reflns_av_R_equivalents 0.0532 _diffrn_reflns_av_sigmaI/netI 0.0660 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.93 _diffrn_reflns_theta_max 25.01 _reflns_number_total 7269 _reflns_number_gt 3697 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0425P)^2^+13.6151P] 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 7269 _refine_ls_number_parameters 628 _refine_ls_number_restraints 173 _refine_ls_R_factor_all 0.1276 _refine_ls_R_factor_gt 0.0572 _refine_ls_wR_factor_ref 0.1700 _refine_ls_wR_factor_gt 0.1234 _refine_ls_goodness_of_fit_ref 1.111 _refine_ls_restrained_S_all 1.163 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 1.0000 0.5000 0.5000 0.0395(2) Uani 1 2 d S . . Pd2 Pd 0.5000 0.5000 0.5000 0.0424(2) Uani 1 2 d S . . F1 F 0.6322(10) 0.8718(15) 0.3499(6) 0.076(4) Uani 0.50 1 d PU A 1 F2 F 0.5198(15) 0.9645(13) 0.4243(9) 0.107(6) Uani 0.50 1 d PU A 1 F3 F 0.4994(13) 0.889(3) 0.3252(12) 0.186(9) Uani 0.50 1 d PU A 1 F4 F 0.5891(14) 1.0378(13) 0.3717(14) 0.143(7) Uani 0.50 1 d PU A 1 F5 F 0.6325(11) 0.890(2) 0.4526(7) 0.133(6) Uani 0.50 1 d PU A 1 F6 F 0.5324(16) 0.7891(14) 0.3857(11) 0.145(6) Uani 0.50 1 d PU A 1 F7 F 0.0050(14) 0.7404(16) 0.3720(10) 0.115(7) Uani 0.50 1 d PU B 1 F8 F -0.0044(13) 0.9839(12) 0.3028(8) 0.095(5) Uani 0.50 1 d PU B 1 F9 F 0.0752(9) 0.8207(16) 0.3133(8) 0.081(4) Uani 0.50 1 d PU B 1 F10 F 0.0684(14) 0.9163(13) 0.3966(7) 0.117(6) Uani 0.50 1 d PU B 1 F11 F -0.0701(14) 0.903(2) 0.3621(10) 0.135(7) Uani 0.50 1 d PU B 1 F12 F -0.0618(10) 0.8008(17) 0.2766(8) 0.135(5) Uani 0.50 1 d PU B 1 F1' F 0.6576(13) 0.931(2) 0.3854(15) 0.188(10) Uani 0.50 1 d PU A 2 F2' F 0.4890(11) 0.918(3) 0.3983(11) 0.151(9) Uani 0.50 1 d PU A 2 F3' F 0.5215(10) 0.9806(13) 0.3212(6) 0.086(4) Uani 0.50 1 d PU A 2 F4' F 0.6040(16) 1.023(2) 0.4197(11) 0.174(10) Uani 0.50 1 d PU A 2 F5' F 0.6002(12) 0.8062(17) 0.4308(9) 0.105(5) Uani 0.50 1 d PU A 2 F6' F 0.5694(19) 0.8127(17) 0.3330(9) 0.166(7) Uani 0.50 1 d PU A 2 F7' F 0.0457(11) 0.7711(17) 0.3996(8) 0.097(6) Uani 0.50 1 d PU B 2 F8' F -0.0390(15) 0.936(2) 0.2830(12) 0.163(9) Uani 0.50 1 d PU B 2 F9' F 0.0322(19) 0.785(3) 0.2995(12) 0.190(12) Uani 0.50 1 d PU B 2 F10' F 0.0862(15) 0.930(3) 0.3605(16) 0.196(11) Uani 0.50 1 d PU B 2 F11' F -0.0203(15) 0.9366(14) 0.3920(10) 0.116(6) Uani 0.50 1 d PU B 2 F12' F -0.0788(13) 0.793(2) 0.3313(12) 0.174(7) Uani 0.50 1 d PU B 2 N1 N 1.0324(4) 0.2811(5) 0.4475(3) 0.0505(16) Uani 1 1 d . . . N2 N 0.9678(4) 0.3814(6) 0.3660(3) 0.0496(16) Uani 1 1 d . . . N3 N 0.8796(4) 0.5450(6) 0.4639(3) 0.0459(16) Uani 1 1 d . . . N4 N 0.8477(4) 0.3482(6) 0.4553(3) 0.0538(17) Uani 1 1 d . . . N5 N 0.4851(4) 0.2973(6) 0.4183(3) 0.0532(17) Uani 1 1 d . . . N6 N 0.4569(4) 0.4415(7) 0.3535(3) 0.0551(18) Uani 1 1 d . . . N7 N 0.3981(4) 0.6045(6) 0.4721(3) 0.0459(15) Uani 1 1 d . . . N8 N 0.3213(4) 0.4382(7) 0.4397(3) 0.0522(17) Uani 1 1 d . . . P1 P 0.57020(18) 0.9114(2) 0.38357(14) 0.0712(7) Uani 1 1 d . . . P2 P 0.0004(2) 0.8609(3) 0.33935(14) 0.0858(9) Uani 1 1 d . . . C1 C 0.9976(4) 0.3882(6) 0.4295(3) 0.0422(18) Uani 1 1 d . . . C2 C 0.9829(5) 0.2720(8) 0.3447(4) 0.062(2) Uani 1 1 d . . . H2 H 0.9671 0.2469 0.3026 0.075 Uiso 1 1 calc R . . C3 C 1.0243(5) 0.2096(8) 0.3958(4) 0.064(2) Uani 1 1 d . . . H3 H 1.0437 0.1331 0.3964 0.077 Uiso 1 1 calc R . . C4 C 1.0765(5) 0.2542(7) 0.5148(4) 0.058(2) Uani 1 1 d . . . H4A H 1.1000 0.1760 0.5182 0.069 Uiso 1 1 calc R . . H4B H 1.0385 0.2554 0.5386 0.069 Uiso 1 1 calc R . . C5 C 0.8567(5) 0.6575(7) 0.4576(3) 0.050(2) Uani 1 1 d . . . C6 C 0.7761(6) 0.6929(9) 0.4291(4) 0.071(3) Uani 1 1 d . . . H6 H 0.7626 0.7723 0.4242 0.085 Uiso 1 1 calc R . . C7 C 0.7173(6) 0.6084(10) 0.4085(5) 0.077(3) Uani 1 1 d . . . H7 H 0.6630 0.6309 0.3897 0.093 Uiso 1 1 calc R . . C8 C 0.7368(5) 0.4895(9) 0.4150(4) 0.062(2) Uani 1 1 d . . . C9 C 0.8208(5) 0.4590(7) 0.4443(3) 0.0455(19) Uani 1 1 d . . . C10 C 0.7932(6) 0.2626(8) 0.4360(4) 0.061(2) Uani 1 1 d . . . C11 C 0.7096(6) 0.2842(10) 0.4047(5) 0.078(3) Uani 1 1 d . . . H11 H 0.6736 0.2215 0.3908 0.094 Uiso 1 1 calc R . . C12 C 0.6816(6) 0.3948(12) 0.3947(5) 0.083(3) Uani 1 1 d . . . H12 H 0.6262 0.4091 0.3745 0.100 Uiso 1 1 calc R . . C13 C 0.8240(6) 0.1401(8) 0.4497(5) 0.086(3) Uani 1 1 d . . . H13A H 0.8590 0.1222 0.4251 0.129 Uiso 1 1 calc R . . H13B H 0.7787 0.0865 0.4386 0.129 Uiso 1 1 calc R . . H13C H 0.8544 0.1325 0.4941 0.129 Uiso 1 1 calc R . . C14 C 0.9266(5) 0.4791(8) 0.3245(4) 0.062(2) Uani 1 1 d . . . H14A H 0.9560 0.4973 0.2952 0.074 Uiso 1 1 calc R . . H14B H 0.9277 0.5483 0.3502 0.074 Uiso 1 1 calc R . . C15 C 0.8386(6) 0.4493(9) 0.2870(4) 0.077(3) Uani 1 1 d D . . H15A H 0.8381 0.3817 0.2603 0.092 Uiso 1 1 calc R . . H15B H 0.8103 0.4273 0.3165 0.092 Uiso 1 1 calc R . . C16 C 0.7934(6) 0.5469(11) 0.2464(6) 0.121(5) Uani 1 1 d D . . H16A H 0.8203 0.5670 0.2157 0.145 Uiso 1 1 calc R . . H16B H 0.7955 0.6155 0.2728 0.145 Uiso 1 1 calc R . . C17 C 0.7059(8) 0.5171(16) 0.2117(8) 0.200(9) Uani 1 1 d D . . H17A H 0.7034 0.4500 0.1849 0.300 Uiso 1 1 calc R . . H17B H 0.6796 0.5829 0.1861 0.300 Uiso 1 1 calc R . . H17C H 0.6785 0.4993 0.2418 0.300 Uiso 1 1 calc R . . C18 C 0.4765(4) 0.4143(7) 0.4155(4) 0.0466(19) Uani 1 1 d . . . C19 C 0.4520(5) 0.3412(9) 0.3183(4) 0.070(3) Uani 1 1 d . . . H19 H 0.4383 0.3371 0.2743 0.083 Uiso 1 1 calc R . . C20 C 0.4704(5) 0.2515(9) 0.3582(4) 0.067(3) Uani 1 1 d . . . H20 H 0.4729 0.1727 0.3477 0.081 Uiso 1 1 calc R . . C21 C 0.5120(5) 0.2345(7) 0.4792(4) 0.058(2) Uani 1 1 d . . . H21A H 0.5152 0.1508 0.4718 0.069 Uiso 1 1 calc R . . H21B H 0.4728 0.2465 0.5015 0.069 Uiso 1 1 calc R . . C22 C 0.4050(5) 0.7202(7) 0.4810(4) 0.050(2) Uani 1 1 d . . . C23 C 0.3371(6) 0.7950(8) 0.4580(4) 0.065(2) Uani 1 1 d . . . H23 H 0.3431 0.8759 0.4641 0.078 Uiso 1 1 calc R . . C24 C 0.2628(6) 0.7482(9) 0.4270(4) 0.071(3) Uani 1 1 d . . . H24 H 0.2183 0.7979 0.4100 0.085 Uiso 1 1 calc R . . C25 C 0.2519(6) 0.6272(9) 0.4199(4) 0.059(2) Uani 1 1 d . . . C26 C 0.3225(5) 0.5555(9) 0.4436(4) 0.053(2) Uani 1 1 d . . . C27 C 0.2501(6) 0.3858(9) 0.4112(4) 0.068(3) Uani 1 1 d . . . C28 C 0.1768(6) 0.4502(11) 0.3853(4) 0.075(3) Uani 1 1 d . . . H28 H 0.1281 0.4108 0.3651 0.090 Uiso 1 1 calc R . . C29 C 0.1770(5) 0.5684(11) 0.3898(4) 0.075(3) Uani 1 1 d . . . H29 H 0.1287 0.6107 0.3732 0.090 Uiso 1 1 calc R . . C30 C 0.2501(6) 0.2552(9) 0.4065(5) 0.089(3) Uani 1 1 d . . . H30A H 0.2648 0.2325 0.3700 0.134 Uiso 1 1 calc R . . H30B H 0.1964 0.2257 0.4021 0.134 Uiso 1 1 calc R . . H30C H 0.2889 0.2230 0.4442 0.134 Uiso 1 1 calc R . . C31 C 0.4453(7) 0.5603(9) 0.3272(4) 0.083(3) Uani 1 1 d DU . . H31A H 0.4840 0.5661 0.3040 0.099 Uiso 1 1 calc R . . H31B H 0.4666 0.6111 0.3639 0.099 Uiso 1 1 calc R . . C33 C 0.3000(11) 0.5444(16) 0.2679(9) 0.176(7) Uani 1 1 d DU . . H33A H 0.2915 0.5133 0.3059 0.212 Uiso 1 1 calc R . . H33B H 0.3099 0.4791 0.2433 0.212 Uiso 1 1 calc R . . C32 C 0.3691(12) 0.6241(18) 0.2851(10) 0.244(10) Uani 1 1 d DU . . H32A H 0.3575 0.6912 0.3077 0.293 Uiso 1 1 calc R . . H32B H 0.3785 0.6526 0.2469 0.293 Uiso 1 1 calc R . . C34 C 0.2237(9) 0.6148(15) 0.2279(7) 0.171(6) Uani 1 1 d DU . . H34A H 0.1916 0.6364 0.2543 0.256 Uiso 1 1 calc R . . H34B H 0.1913 0.5671 0.1933 0.256 Uiso 1 1 calc R . . H34C H 0.2409 0.6846 0.2115 0.256 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 0.0369(5) 0.0454(5) 0.0360(4) -0.0002(4) 0.0117(4) 0.0052(4) Pd2 0.0369(5) 0.0509(5) 0.0390(5) -0.0081(4) 0.0120(4) -0.0001(4) F1 0.078(9) 0.094(9) 0.067(7) 0.019(7) 0.039(7) 0.032(7) F2 0.158(17) 0.065(8) 0.122(12) -0.017(7) 0.078(11) 0.013(8) F3 0.115(13) 0.249(18) 0.168(15) -0.065(16) 0.014(11) 0.032(15) F4 0.165(14) 0.054(8) 0.228(17) 0.037(11) 0.090(14) -0.001(9) F5 0.140(12) 0.151(13) 0.075(9) 0.013(10) -0.010(8) 0.024(11) F6 0.211(16) 0.082(9) 0.160(14) -0.029(10) 0.084(13) -0.064(11) F7 0.155(17) 0.071(9) 0.133(15) 0.021(10) 0.069(12) 0.007(10) F8 0.152(14) 0.057(7) 0.069(8) 0.019(6) 0.028(8) -0.012(8) F9 0.070(8) 0.111(10) 0.067(8) 0.017(7) 0.027(7) 0.015(7) F10 0.165(14) 0.074(9) 0.069(8) -0.006(7) -0.022(9) 0.030(9) F11 0.139(14) 0.172(16) 0.117(13) 0.017(11) 0.072(11) 0.054(12) F12 0.114(11) 0.171(13) 0.109(11) -0.048(10) 0.023(9) -0.052(10) F1' 0.124(14) 0.178(16) 0.253(19) 0.021(15) 0.049(14) -0.026(13) F2' 0.077(10) 0.232(19) 0.158(16) 0.056(14) 0.058(10) 0.032(12) F3' 0.118(10) 0.077(8) 0.053(6) 0.021(6) 0.014(6) 0.047(8) F4' 0.175(16) 0.155(16) 0.158(14) -0.092(13) 0.005(13) -0.008(13) F5' 0.124(12) 0.105(10) 0.114(11) 0.046(9) 0.076(10) 0.059(9) F6' 0.237(17) 0.118(12) 0.132(13) -0.023(10) 0.046(13) 0.044(13) F7' 0.107(12) 0.114(13) 0.075(10) 0.032(8) 0.036(8) 0.036(10) F8' 0.161(16) 0.186(18) 0.143(16) 0.085(14) 0.052(12) 0.051(14) F9' 0.24(2) 0.207(19) 0.137(16) -0.025(13) 0.084(16) 0.057(16) F10' 0.167(16) 0.196(18) 0.25(2) 0.035(16) 0.102(15) -0.043(13) F11' 0.164(16) 0.076(8) 0.128(13) -0.002(9) 0.076(11) 0.010(10) F12' 0.143(14) 0.179(15) 0.174(15) -0.015(13) 0.017(12) -0.057(13) N1 0.058(4) 0.044(4) 0.049(4) -0.006(3) 0.018(4) 0.003(3) N2 0.048(4) 0.056(4) 0.044(4) -0.003(3) 0.014(3) 0.000(3) N3 0.043(4) 0.056(4) 0.038(4) 0.002(3) 0.012(3) 0.006(3) N4 0.056(5) 0.057(5) 0.050(4) -0.004(3) 0.019(4) -0.012(4) N5 0.054(4) 0.055(4) 0.051(4) -0.015(3) 0.019(4) -0.007(3) N6 0.041(4) 0.077(5) 0.046(4) -0.018(4) 0.013(3) 0.000(4) N7 0.042(4) 0.054(4) 0.039(4) -0.002(3) 0.010(3) 0.009(3) N8 0.035(4) 0.068(5) 0.053(4) -0.015(4) 0.013(3) -0.009(4) P1 0.078(2) 0.0570(16) 0.0819(19) 0.0009(14) 0.0311(16) 0.0075(14) P2 0.122(3) 0.0701(18) 0.077(2) 0.0125(16) 0.048(2) 0.0144(19) C1 0.043(5) 0.044(5) 0.042(4) -0.006(4) 0.018(4) 0.002(4) C2 0.053(6) 0.073(6) 0.057(6) -0.022(5) 0.013(5) -0.006(5) C3 0.056(6) 0.060(6) 0.077(7) -0.016(5) 0.023(5) -0.003(5) C4 0.063(6) 0.052(5) 0.056(5) 0.015(4) 0.015(5) 0.016(4) C5 0.052(5) 0.059(6) 0.038(4) 0.001(4) 0.013(4) 0.007(5) C6 0.065(7) 0.077(7) 0.067(6) 0.014(5) 0.015(5) 0.029(6) C7 0.044(6) 0.098(8) 0.082(7) 0.003(6) 0.009(5) 0.026(6) C8 0.051(5) 0.088(7) 0.046(5) -0.004(5) 0.014(4) 0.014(6) C9 0.036(5) 0.065(6) 0.036(4) -0.001(4) 0.012(4) 0.002(4) C10 0.066(7) 0.071(6) 0.049(5) 0.000(5) 0.021(5) -0.011(5) C11 0.067(7) 0.093(8) 0.076(7) -0.019(6) 0.025(6) -0.027(6) C12 0.040(6) 0.138(10) 0.069(7) -0.024(7) 0.014(5) -0.012(7) C13 0.106(9) 0.064(7) 0.087(7) -0.006(5) 0.028(7) -0.021(6) C14 0.059(5) 0.079(7) 0.043(5) 0.007(4) 0.012(4) 0.003(5) C15 0.073(7) 0.099(7) 0.050(5) 0.006(5) 0.009(5) 0.001(6) C16 0.076(8) 0.136(11) 0.114(10) 0.046(8) -0.017(7) 0.020(8) C17 0.087(10) 0.28(2) 0.186(16) 0.093(15) -0.022(10) 0.026(13) C18 0.036(4) 0.062(5) 0.044(5) -0.015(4) 0.015(4) -0.006(4) C19 0.065(6) 0.089(7) 0.046(5) -0.024(5) 0.007(5) 0.010(5) C20 0.063(6) 0.072(6) 0.059(6) -0.027(5) 0.010(5) -0.005(5) C21 0.069(6) 0.050(5) 0.058(5) -0.006(4) 0.026(5) -0.013(4) C22 0.058(6) 0.048(5) 0.048(5) 0.000(4) 0.022(4) 0.008(4) C23 0.089(8) 0.052(5) 0.055(6) 0.003(4) 0.025(5) 0.015(5) C24 0.059(7) 0.085(8) 0.061(6) 0.010(5) 0.009(5) 0.015(6) C25 0.055(6) 0.074(7) 0.050(5) 0.002(5) 0.018(5) 0.012(5) C26 0.047(6) 0.074(6) 0.039(5) -0.011(4) 0.016(4) -0.006(5) C27 0.056(7) 0.091(8) 0.062(6) -0.009(5) 0.029(5) -0.003(6) C28 0.044(6) 0.104(8) 0.071(7) -0.019(6) 0.012(5) -0.011(6) C29 0.035(6) 0.110(9) 0.075(7) -0.005(6) 0.010(5) 0.010(6) C30 0.065(7) 0.082(8) 0.118(9) -0.032(7) 0.027(6) -0.028(6) C31 0.099(8) 0.086(7) 0.053(6) 0.009(5) 0.011(5) 0.032(6) C33 0.186(15) 0.181(14) 0.177(14) 0.022(12) 0.080(13) 0.014(13) C32 0.245(18) 0.246(19) 0.238(18) -0.011(15) 0.073(15) -0.040(16) C34 0.152(12) 0.212(15) 0.135(12) 0.017(11) 0.029(10) 0.060(12) _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 2.008(7) . ? Pd1 C1 2.008(7) 3_766 ? Pd1 N3 2.037(6) 3_766 ? Pd1 N3 2.037(6) . ? Pd2 C18 2.038(7) 3_666 ? Pd2 C18 2.038(7) . ? Pd2 N7 2.046(6) 3_666 ? Pd2 N7 2.046(6) . ? F1 P1 1.560(11) . ? F2 P1 1.567(18) . ? F3 P1 1.49(2) . ? F4 P1 1.515(14) . ? F5 P1 1.580(14) . ? F6 P1 1.544(14) . ? F7 P2 1.540(19) . ? F8 P2 1.605(15) . ? F9 P2 1.645(16) . ? F10 P2 1.557(15) . ? F11 P2 1.538(18) . ? F12 P2 1.610(14) . ? F1' P1 1.51(2) . ? F2' P1 1.544(19) . ? F3' P1 1.579(11) . ? F4' P1 1.509(19) . ? F5' P1 1.564(13) . ? F6' P1 1.586(16) . ? F7' P2 1.664(17) . ? F8' P2 1.48(2) . ? F9' P2 1.47(2) . ? F10' P2 1.61(2) . ? F11' P2 1.584(17) . ? F12' P2 1.532(18) . ? N1 C1 1.359(9) . ? N1 C3 1.377(10) . ? N1 C4 1.474(9) . ? N2 C1 1.338(9) . ? N2 C2 1.386(10) . ? N2 C14 1.471(9) . ? N3 C5 1.332(9) . ? N3 C9 1.375(9) . ? N4 C10 1.326(10) . ? N4 C9 1.338(9) . ? N5 C18 1.337(9) . ? N5 C20 1.379(10) . ? N5 C21 1.466(10) . ? N6 C18 1.343(9) . ? N6 C19 1.370(10) . ? N6 C31 1.459(11) . ? N7 C22 1.329(9) . ? N7 C26 1.372(10) . ? N8 C27 1.327(10) . ? N8 C26 1.336(10) . ? C2 C3 1.334(11) . ? C4 C5 1.502(11) 3_766 ? C5 C6 1.389(11) . ? C5 C4 1.502(11) 3_766 ? C6 C7 1.364(13) . ? C7 C8 1.389(12) . ? C8 C12 1.413(13) . ? C8 C9 1.426(11) . ? C10 C11 1.406(13) . ? C10 C13 1.488(12) . ? C11 C12 1.339(14) . ? C14 C15 1.514(11) . ? C15 C16 1.482(11) . ? C16 C17 1.497(13) . ? C19 C20 1.320(12) . ? C21 C22 1.510(11) 3_666 ? C22 C23 1.404(11) . ? C22 C21 1.510(11) 3_666 ? C23 C24 1.353(12) . ? C24 C25 1.391(12) . ? C25 C29 1.416(12) . ? C25 C26 1.419(11) . ? C27 C28 1.413(12) . ? C27 C30 1.489(13) . ? C28 C29 1.346(13) . ? C31 C32 1.528(16) . ? C33 C32 1.447(16) . ? C33 C34 1.552(14) . ? 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(2) . 3_766 ? C1 Pd1 N3 84.7(3) . 3_766 ? C1 Pd1 N3 95.3(3) 3_766 3_766 ? C1 Pd1 N3 95.3(3) . . ? C1 Pd1 N3 84.7(3) 3_766 . ? N3 Pd1 N3 180.000(1) 3_766 . ? C18 Pd2 C18 180.000(1) 3_666 . ? C18 Pd2 N7 96.0(3) 3_666 3_666 ? C18 Pd2 N7 84.0(3) . 3_666 ? C18 Pd2 N7 84.0(3) 3_666 . ? C18 Pd2 N7 96.0(3) . . ? N7 Pd2 N7 180.000(2) 3_666 . ? C1 N1 C3 111.6(7) . . ? C1 N1 C4 121.2(6) . . ? C3 N1 C4 127.1(7) . . ? C1 N2 C2 111.2(7) . . ? C1 N2 C14 124.1(7) . . ? C2 N2 C14 124.7(7) . . ? C5 N3 C9 119.0(7) . . ? C5 N3 Pd1 120.9(6) . . ? C9 N3 Pd1 120.1(5) . . ? C10 N4 C9 117.6(8) . . ? C18 N5 C20 110.3(7) . . ? C18 N5 C21 121.7(6) . . ? C20 N5 C21 127.9(7) . . ? C18 N6 C19 110.0(8) . . ? C18 N6 C31 125.5(7) . . ? C19 N6 C31 124.5(7) . . ? C22 N7 C26 119.8(7) . . ? C22 N7 Pd2 120.2(5) . . ? C26 N7 Pd2 120.0(6) . . ? C27 N8 C26 118.1(8) . . ? F3 P1 F4' 132.2(15) . . ? F3 P1 F1' 125.4(16) . . ? F4' P1 F1' 69.5(15) . . ? F3 P1 F4 99.9(14) . . ? F4' P1 F4 39.7(10) . . ? F1' P1 F4 65.9(12) . . ? F3 P1 F2' 69.3(12) . . ? F4' P1 F2' 93.9(14) . . ? F1' P1 F2' 162.7(16) . . ? F4 P1 F2' 104.7(13) . . ? F3 P1 F6 68.7(14) . . ? F4' P1 F6 146.4(14) . . ? F1' P1 F6 124.2(14) . . ? F4 P1 F6 167.6(14) . . ? F2' P1 F6 67.3(12) . . ? F3 P1 F1 91.8(11) . . ? F4' P1 F1 106.9(13) . . ? F1' P1 F1 38.9(9) . . ? F4 P1 F1 88.2(10) . . ? F2' P1 F1 158.4(13) . . ? F6 P1 F1 96.8(10) . . ? F3 P1 F5' 117.0(16) . . ? F4' P1 F5' 107.3(14) . . ? F1' P1 F5' 89.3(11) . . ? F4 P1 F5' 143.0(14) . . ? F2' P1 F5' 91.2(10) . . ? F6 P1 F5' 48.9(8) . . ? F1 P1 F5' 88.4(6) . . ? F3 P1 F2 96.6(12) . . ? F4' P1 F2 64.0(11) . . ? F1' P1 F2 131.6(15) . . ? F4 P1 F2 85.9(10) . . ? F2' P1 F2 31.1(10) . . ? F6 P1 F2 90.5(10) . . ? F1 P1 F2 170.5(11) . . ? F5' P1 F2 91.8(8) . . ? F3 P1 F3' 42.8(11) . . ? F4' P1 F3' 93.1(11) . . ? F1' P1 F3' 101.0(12) . . ? F4 P1 F3' 57.2(10) . . ? F2' P1 F3' 84.3(10) . . ? F6 P1 F3' 111.4(12) . . ? F1 P1 F3' 88.6(7) . . ? F5' P1 F3' 159.4(12) . . ? F2 P1 F3' 94.5(9) . . ? F3 P1 F5 158.3(15) . . ? F4' P1 F5 65.6(12) . . ? F1' P1 F5 68.8(12) . . ? F4 P1 F5 101.2(13) . . ? F2' P1 F5 100.4(11) . . ? F6 P1 F5 89.8(10) . . ? F1 P1 F5 93.8(9) . . ? F5' P1 F5 42.3(8) . . ? F2 P1 F5 80.1(11) . . ? F3' P1 F5 158.2(10) . . ? F3 P1 F6' 56.4(11) . . ? F4' P1 F6' 152.0(16) . . ? F1' P1 F6' 84.5(12) . . ? F4 P1 F6' 120.0(14) . . ? F2' P1 F6' 112.7(16) . . ? F6 P1 F6' 58.5(10) . . ? F1 P1 F6' 45.9(9) . . ? F5' P1 F6' 81.9(10) . . ? F2 P1 F6' 143.5(14) . . ? F3' P1 F6' 81.4(9) . . ? F5 P1 F6' 115.3(11) . . ? F9' P2 F8' 89.3(15) . . ? F9' P2 F12' 97.2(16) . . ? F8' P2 F12' 92.6(14) . . ? F9' P2 F11 150.8(16) . . ? F8' P2 F11 84.6(12) . . ? F12' P2 F11 54.8(10) . . ? F9' P2 F7 77.7(13) . . ? F8' P2 F7 147.9(14) . . ? F12' P2 F7 60.8(10) . . ? F11 P2 F7 92.7(12) . . ? F9' P2 F10 113.6(14) . . ? F8' P2 F10 118.3(13) . . ? F12' P2 F10 135.2(12) . . ? F11 P2 F10 94.2(11) . . ? F7 P2 F10 93.7(10) . . ? F9' P2 F11' 170.1(14) . . ? F8' P2 F11' 99.2(13) . . ? F12' P2 F11' 87.4(11) . . ? F11 P2 F11' 36.5(9) . . ? F7 P2 F11' 97.2(10) . . ? F10 P2 F11' 57.9(9) . . ? F9' P2 F8 100.1(13) . . ? F8' P2 F8 30.6(11) . . ? F12' P2 F8 119.1(12) . . ? F11 P2 F8 88.9(12) . . ? F7 P2 F8 177.7(10) . . ? F10 P2 F8 87.8(8) . . ? F11' P2 F8 85.1(9) . . ? F9' P2 F10' 88.4(14) . . ? F8' P2 F10' 95.4(13) . . ? F12' P2 F10' 170.3(14) . . ? F11 P2 F10' 120.5(15) . . ? F7 P2 F10' 113.2(13) . . ? F10 P2 F10' 35.3(9) . . ? F11' P2 F10' 85.9(13) . . ? F8 P2 F10' 67.3(11) . . ? F9' P2 F12 60.1(11) . . ? F8' P2 F12 61.2(11) . . ? F12' P2 F12 50.5(9) . . ? F11 P2 F12 92.3(12) . . ? F7 P2 F12 87.0(11) . . ? F10 P2 F12 173.3(11) . . ? F11' P2 F12 128.6(11) . . ? F8 P2 F12 91.2(9) . . ? F10' P2 F12 138.8(12) . . ? F9' P2 F9 29.7(13) . . ? F8' P2 F9 93.3(11) . . ? F12' P2 F9 126.3(13) . . ? F11 P2 F9 177.8(10) . . ? F7 P2 F9 89.6(10) . . ? F10 P2 F9 85.9(10) . . ? F11' P2 F9 143.5(11) . . ? F8 P2 F9 88.9(9) . . ? F10' P2 F9 58.8(11) . . ? F12 P2 F9 87.5(9) . . ? F9' P2 F7' 87.3(13) . . ? F8' P2 F7' 176.5(13) . . ? F12' P2 F7' 87.2(10) . . ? F11 P2 F7' 98.1(10) . . ? F7 P2 F7' 30.2(8) . . ? F10 P2 F7' 63.7(8) . . ? F11' P2 F7' 84.2(10) . . ? F8 P2 F7' 151.1(10) . . ? F10' P2 F7' 85.1(12) . . ? F12 P2 F7' 116.3(10) . . ? F9 P2 F7' 84.0(8) . . ? N2 C1 N1 103.9(6) . . ? N2 C1 Pd1 139.7(6) . . ? N1 C1 Pd1 116.3(5) . . ? C3 C2 N2 107.2(8) . . ? C2 C3 N1 106.1(8) . . ? N1 C4 C5 110.5(6) . 3_766 ? N3 C5 C6 123.1(8) . . ? N3 C5 C4 115.9(7) . 3_766 ? C6 C5 C4 121.0(8) . 3_766 ? C7 C6 C5 118.4(9) . . ? C6 C7 C8 121.4(9) . . ? C7 C8 C12 126.4(9) . . ? C7 C8 C9 117.4(9) . . ? C12 C8 C9 116.2(9) . . ? N4 C9 N3 115.7(7) . . ? N4 C9 C8 123.7(8) . . ? N3 C9 C8 120.6(8) . . ? N4 C10 C11 122.7(9) . . ? N4 C10 C13 116.8(9) . . ? C11 C10 C13 120.5(9) . . ? C12 C11 C10 120.2(10) . . ? C11 C12 C8 119.5(9) . . ? N2 C14 C15 111.8(7) . . ? C16 C15 C14 113.8(8) . . ? C15 C16 C17 112.9(11) . . ? N5 C18 N6 105.4(6) . . ? N5 C18 Pd2 116.5(6) . . ? N6 C18 Pd2 138.0(6) . . ? C20 C19 N6 107.7(8) . . ? C19 C20 N5 106.7(8) . . ? N5 C21 C22 109.3(6) . 3_666 ? N7 C22 C23 121.4(8) . . ? N7 C22 C21 116.6(7) . 3_666 ? C23 C22 C21 121.9(8) . 3_666 ? C24 C23 C22 119.3(9) . . ? C23 C24 C25 121.2(9) . . ? C24 C25 C29 126.2(9) . . ? C24 C25 C26 117.2(9) . . ? C29 C25 C26 116.5(9) . . ? N8 C26 N7 115.3(8) . . ? N8 C26 C25 123.8(8) . . ? N7 C26 C25 120.8(8) . . ? N8 C27 C28 122.0(9) . . ? N8 C27 C30 117.4(9) . . ? C28 C27 C30 120.6(9) . . ? C29 C28 C27 120.4(10) . . ? C28 C29 C25 119.1(9) . . ? N6 C31 C32 131.5(12) . . ? C32 C33 C34 107.6(15) . . ? C33 C32 C31 109.7(16) . . ? 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 N3 C5 -129.9(6) . . . . ? C1 Pd1 N3 C5 50.1(6) 3_766 . . . ? N3 Pd1 N3 C5 157(100) 3_766 . . . ? C1 Pd1 N3 C9 48.7(5) . . . . ? C1 Pd1 N3 C9 -131.3(5) 3_766 . . . ? N3 Pd1 N3 C9 -24(100) 3_766 . . . ? C18 Pd2 N7 C22 51.1(6) 3_666 . . . ? C18 Pd2 N7 C22 -128.9(6) . . . . ? N7 Pd2 N7 C22 176(100) 3_666 . . . ? C18 Pd2 N7 C26 -129.4(6) 3_666 . . . ? C18 Pd2 N7 C26 50.6(6) . . . . ? N7 Pd2 N7 C26 -5(100) 3_666 . . . ? C2 N2 C1 N1 0.6(8) . . . . ? C14 N2 C1 N1 -177.8(7) . . . . ? C2 N2 C1 Pd1 -175.4(7) . . . . ? C14 N2 C1 Pd1 6.2(12) . . . . ? C3 N1 C1 N2 0.1(8) . . . . ? C4 N1 C1 N2 176.9(6) . . . . ? C3 N1 C1 Pd1 177.2(5) . . . . ? C4 N1 C1 Pd1 -6.0(9) . . . . ? C1 Pd1 C1 N2 81(100) 3_766 . . . ? N3 Pd1 C1 N2 -136.3(9) 3_766 . . . ? N3 Pd1 C1 N2 43.7(9) . . . . ? C1 Pd1 C1 N1 -94(100) 3_766 . . . ? N3 Pd1 C1 N1 48.0(5) 3_766 . . . ? N3 Pd1 C1 N1 -132.0(5) . . . . ? C1 N2 C2 C3 -1.1(9) . . . . ? C14 N2 C2 C3 177.3(7) . . . . ? N2 C2 C3 N1 1.1(9) . . . . ? C1 N1 C3 C2 -0.8(9) . . . . ? C4 N1 C3 C2 -177.3(7) . . . . ? C1 N1 C4 C5 -55.6(9) . . . 3_766 ? C3 N1 C4 C5 120.6(8) . . . 3_766 ? C9 N3 C5 C6 -3.4(11) . . . . ? Pd1 N3 C5 C6 175.2(6) . . . . ? C9 N3 C5 C4 174.9(6) . . . 3_766 ? Pd1 N3 C5 C4 -6.5(9) . . . 3_766 ? N3 C5 C6 C7 2.3(13) . . . . ? C4 C5 C6 C7 -175.8(8) 3_766 . . . ? C5 C6 C7 C8 -0.7(14) . . . . ? C6 C7 C8 C12 -178.9(9) . . . . ? C6 C7 C8 C9 0.2(13) . . . . ? C10 N4 C9 N3 -178.7(6) . . . . ? C10 N4 C9 C8 2.1(11) . . . . ? C5 N3 C9 N4 -176.4(6) . . . . ? Pd1 N3 C9 N4 5.0(8) . . . . ? C5 N3 C9 C8 2.8(10) . . . . ? Pd1 N3 C9 C8 -175.8(5) . . . . ? C7 C8 C9 N4 177.8(7) . . . . ? C12 C8 C9 N4 -2.9(12) . . . . ? C7 C8 C9 N3 -1.3(11) . . . . ? C12 C8 C9 N3 178.0(7) . . . . ? C9 N4 C10 C11 0.3(12) . . . . ? C9 N4 C10 C13 -179.0(7) . . . . ? N4 C10 C11 C12 -1.9(14) . . . . ? C13 C10 C11 C12 177.4(9) . . . . ? C10 C11 C12 C8 1.0(14) . . . . ? C7 C8 C12 C11 -179.6(9) . . . . ? C9 C8 C12 C11 1.2(13) . . . . ? C1 N2 C14 C15 -117.8(8) . . . . ? C2 N2 C14 C15 64.1(10) . . . . ? N2 C14 C15 C16 177.6(9) . . . . ? C14 C15 C16 C17 -177.9(11) . . . . ? C20 N5 C18 N6 -0.4(9) . . . . ? C21 N5 C18 N6 175.9(6) . . . . ? C20 N5 C18 Pd2 -177.7(5) . . . . ? C21 N5 C18 Pd2 -1.5(9) . . . . ? C19 N6 C18 N5 1.1(9) . . . . ? C31 N6 C18 N5 -176.8(8) . . . . ? C19 N6 C18 Pd2 177.5(6) . . . . ? C31 N6 C18 Pd2 -0.4(13) . . . . ? C18 Pd2 C18 N5 13(100) 3_666 . . . ? N7 Pd2 C18 N5 46.1(6) 3_666 . . . ? N7 Pd2 C18 N5 -133.9(6) . . . . ? C18 Pd2 C18 N6 -163(100) 3_666 . . . ? N7 Pd2 C18 N6 -130.0(8) 3_666 . . . ? N7 Pd2 C18 N6 50.0(8) . . . . ? C18 N6 C19 C20 -1.4(10) . . . . ? C31 N6 C19 C20 176.5(8) . . . . ? N6 C19 C20 N5 1.1(10) . . . . ? C18 N5 C20 C19 -0.5(10) . . . . ? C21 N5 C20 C19 -176.4(8) . . . . ? C18 N5 C21 C22 -58.8(9) . . . 3_666 ? C20 N5 C21 C22 116.7(8) . . . 3_666 ? C26 N7 C22 C23 -4.4(11) . . . . ? Pd2 N7 C22 C23 175.1(5) . . . . ? C26 N7 C22 C21 171.5(6) . . . 3_666 ? Pd2 N7 C22 C21 -9.0(9) . . . 3_666 ? N7 C22 C23 C24 1.0(12) . . . . ? C21 C22 C23 C24 -174.7(8) 3_666 . . . ? C22 C23 C24 C25 3.0(13) . . . . ? C23 C24 C25 C29 178.5(8) . . . . ? C23 C24 C25 C26 -3.3(13) . . . . ? C27 N8 C26 N7 -178.4(6) . . . . ? C27 N8 C26 C25 1.0(12) . . . . ? C22 N7 C26 N8 -176.7(7) . . . . ? Pd2 N7 C26 N8 3.8(9) . . . . ? C22 N7 C26 C25 3.9(11) . . . . ? Pd2 N7 C26 C25 -175.6(5) . . . . ? C24 C25 C26 N8 -179.4(8) . . . . ? C29 C25 C26 N8 -1.1(12) . . . . ? C24 C25 C26 N7 -0.1(11) . . . . ? C29 C25 C26 N7 178.3(7) . . . . ? C26 N8 C27 C28 0.0(12) . . . . ? C26 N8 C27 C30 179.2(8) . . . . ? N8 C27 C28 C29 -1.0(14) . . . . ? C30 C27 C28 C29 179.9(9) . . . . ? C27 C28 C29 C25 0.8(14) . . . . ? C24 C25 C29 C28 178.3(9) . . . . ? C26 C25 C29 C28 0.1(13) . . . . ? C18 N6 C31 C32 -112.4(15) . . . . ? C19 N6 C31 C32 70.0(18) . . . . ? C34 C33 C32 C31 177.4(13) . . . . ? N6 C31 C32 C33 -4(3) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.751 _refine_diff_density_min -0.517 _refine_diff_density_rms 0.088 #===END data_080606e _database_code_depnum_ccdc_archive 'CCDC 720714' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H22 F12 N10 P2 Pd' _chemical_formula_weight 798.82 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' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.0400(10) _cell_length_b 12.9230(13) _cell_length_c 13.5160(16) _cell_angle_alpha 111.148(2) _cell_angle_beta 101.0820(10) _cell_angle_gamma 107.4680(10) _cell_volume 1614.7(3) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Prism _exptl_crystal_colour pale-yellow _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.643 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 792 _exptl_absorpt_coefficient_mu 0.773 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8244 _exptl_absorpt_correction_T_max 0.8608 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8405 _diffrn_reflns_av_R_equivalents 0.0175 _diffrn_reflns_av_sigmaI/netI 0.0493 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.72 _diffrn_reflns_theta_max 25.01 _reflns_number_total 5582 _reflns_number_gt 4224 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0595P)^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 5582 _refine_ls_number_parameters 454 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0596 _refine_ls_R_factor_gt 0.0436 _refine_ls_wR_factor_ref 0.1024 _refine_ls_wR_factor_gt 0.0981 _refine_ls_goodness_of_fit_ref 0.951 _refine_ls_restrained_S_all 0.951 _refine_ls_shift/su_max 0.142 _refine_ls_shift/su_mean 0.012 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 0.36389(3) 0.76095(3) 0.65358(2) 0.04947(13) Uani 1 1 d . . . F1 F -0.0729(4) 0.1134(3) 0.7893(4) 0.1371(13) Uani 1 1 d . A . F2 F 0.0786(3) -0.0608(3) 0.7463(3) 0.1054(10) Uani 1 1 d . A . F3 F -0.1201(13) -0.0763(10) 0.7593(11) 0.115(4) Uani 0.59(3) 1 d P A 1 F4 F -0.0585(17) -0.0299(16) 0.6368(10) 0.162(6) Uani 0.59(3) 1 d P A 1 F5 F 0.1155(19) 0.1278(9) 0.760(2) 0.139(6) Uani 0.59(3) 1 d P A 1 F6 F 0.0571(14) 0.0852(17) 0.8927(8) 0.131(5) Uani 0.59(3) 1 d P A 1 F7 F 0.6207(6) 0.3821(5) 0.7958(4) 0.1812(19) Uani 1 1 d . B . F8 F 0.4910(5) 0.3204(5) 0.5457(4) 0.1778(19) Uani 1 1 d . B . F9 F 0.4833(19) 0.4248(15) 0.7164(13) 0.187(7) Uani 0.58(2) 1 d P B 1 F10 F 0.4593(15) 0.2416(10) 0.6777(12) 0.141(4) Uani 0.58(2) 1 d P B 1 F11 F 0.6424(18) 0.2748(19) 0.633(2) 0.151(6) Uani 0.58(2) 1 d P B 1 F12 F 0.660(2) 0.4571(10) 0.6716(13) 0.224(9) Uani 0.58(2) 1 d P B 1 F3' F -0.1355(15) -0.073(2) 0.726(3) 0.177(12) Uani 0.41(3) 1 d P A 2 F4' F -0.013(3) 0.019(3) 0.652(2) 0.161(11) Uani 0.41(3) 1 d P A 2 F5' F 0.1545(14) 0.1202(19) 0.8266(18) 0.138(7) Uani 0.41(3) 1 d P A 2 F6' F 0.023(2) 0.029(2) 0.8946(17) 0.131(7) Uani 0.41(3) 1 d P A 2 F9' F 0.5097(17) 0.4645(12) 0.7115(13) 0.112(6) Uani 0.42(2) 1 d P B 2 F10' F 0.6935(13) 0.429(2) 0.6899(18) 0.192(11) Uani 0.42(2) 1 d P B 2 F11' F 0.576(4) 0.234(3) 0.618(3) 0.182(13) Uani 0.42(2) 1 d P B 2 F12' F 0.3982(19) 0.273(2) 0.6385(18) 0.194(10) Uani 0.42(2) 1 d P B 2 N1 N 0.1313(3) 0.6519(3) 0.4652(3) 0.0651(9) Uani 1 1 d . . . N2 N 0.1776(3) 0.8412(3) 0.5187(3) 0.0600(9) Uani 1 1 d . . . N3 N 0.2631(3) 0.5770(3) 0.5438(2) 0.0518(8) Uani 1 1 d . . . N4 N 0.0659(4) 0.4435(4) 0.3843(3) 0.0855(12) Uani 1 1 d . . . N5 N 0.4152(3) 0.9912(3) 0.8486(2) 0.0490(8) Uani 1 1 d . . . N6 N 0.5369(3) 1.0258(3) 0.7492(3) 0.0568(8) Uani 1 1 d . . . N7 N 0.2608(3) 0.8126(3) 0.8319(3) 0.0571(9) Uani 1 1 d . . . N8 N 0.3090(4) 1.0030(3) 0.9820(3) 0.0586(9) Uani 1 1 d . . . N9 N 0.5190(4) 0.7430(3) 0.7487(3) 0.0643(10) Uani 1 1 d . . . P1 P 0.00357(12) 0.02642(11) 0.76750(11) 0.0669(3) Uani 1 1 d . . . P2 P 0.5520(2) 0.34822(14) 0.67064(13) 0.0910(5) Uani 1 1 d . . . C1 C 0.2193(4) 0.7651(4) 0.5454(3) 0.0503(9) Uani 1 1 d . . . C2 C 0.0647(5) 0.7755(5) 0.4213(4) 0.0870(16) Uani 1 1 d . . . H2 H 0.0175 0.8084 0.3859 0.104 Uiso 1 1 calc R . . C3 C 0.0357(5) 0.6587(5) 0.3875(4) 0.0886(16) Uani 1 1 d . . . H3 H -0.0344 0.5943 0.3245 0.106 Uiso 1 1 calc R . . C4 C 0.1519(4) 0.5505(4) 0.4631(3) 0.0617(11) Uani 1 1 d . . . C5 C 0.0960(6) 0.3518(5) 0.3872(5) 0.0991(18) Uani 1 1 d . . . H5 H 0.0368 0.2732 0.3348 0.119 Uiso 1 1 calc R . . C6 C 0.2089(5) 0.3675(4) 0.4630(4) 0.0851(15) Uani 1 1 d . . . H6 H 0.2296 0.3022 0.4606 0.102 Uiso 1 1 calc R . . C7 C 0.2907(5) 0.4834(4) 0.5429(4) 0.0693(12) Uani 1 1 d . . . H7 H 0.3670 0.4970 0.5976 0.083 Uiso 1 1 calc R . . C8 C 0.2422(4) 0.9746(4) 0.5755(4) 0.0653(11) Uani 1 1 d . . . H8A H 0.2804 1.0023 0.6551 0.098 Uiso 1 1 calc R . . H8B H 0.1762 1.0064 0.5614 0.098 Uiso 1 1 calc R . . H8C H 0.3123 1.0019 0.5469 0.098 Uiso 1 1 calc R . . C9 C 0.4446(4) 0.9378(3) 0.7549(3) 0.0467(9) Uani 1 1 d . . . C10 C 0.5654(5) 1.1350(4) 0.8382(4) 0.0712(13) Uani 1 1 d . . . H10 H 0.6275 1.2101 0.8523 0.085 Uiso 1 1 calc R . . C11 C 0.4919(5) 1.1163(4) 0.8989(4) 0.0644(11) Uani 1 1 d . . . H11 H 0.4904 1.1745 0.9633 0.077 Uiso 1 1 calc R . . C12 C 0.3213(4) 0.9316(3) 0.8895(3) 0.0486(9) Uani 1 1 d . . . C13 C 0.2202(5) 0.9481(5) 1.0172(4) 0.0736(13) Uani 1 1 d . . . H13 H 0.2058 0.9943 1.0811 0.088 Uiso 1 1 calc R . . C14 C 0.1468(5) 0.8246(5) 0.9637(4) 0.0756(13) Uani 1 1 d . . . H14 H 0.0828 0.7868 0.9892 0.091 Uiso 1 1 calc R . . C15 C 0.1730(5) 0.7600(4) 0.8708(4) 0.0665(12) Uani 1 1 d . . . H15 H 0.1270 0.6761 0.8339 0.080 Uiso 1 1 calc R . . C16 C 0.5978(5) 1.0079(5) 0.6608(5) 0.0832(15) Uani 1 1 d . . . H16A H 0.6938 1.0375 0.6943 0.125 Uiso 1 1 calc R . . H16B H 0.5777 1.0514 0.6200 0.125 Uiso 1 1 calc R . . H16C H 0.5619 0.9230 0.6101 0.125 Uiso 1 1 calc R . . C17 C 0.6067(5) 0.7369(4) 0.7984(4) 0.0715(13) Uani 1 1 d . . . C18 C 0.7252(6) 0.7320(5) 0.8652(5) 0.117(2) Uani 1 1 d . . . H18A H 0.7903 0.7331 0.8272 0.176 Uiso 1 1 calc R . . H18B H 0.6979 0.6589 0.8740 0.176 Uiso 1 1 calc R . . H18C H 0.7647 0.8009 0.9381 0.176 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 0.0558(2) 0.04077(19) 0.04232(18) 0.01217(13) 0.00680(13) 0.02123(15) F1 0.153(3) 0.112(3) 0.190(4) 0.071(3) 0.083(3) 0.090(3) F2 0.115(2) 0.094(2) 0.132(3) 0.055(2) 0.043(2) 0.068(2) F3 0.143(11) 0.074(6) 0.140(8) 0.047(5) 0.096(9) 0.029(6) F4 0.177(9) 0.189(10) 0.065(5) 0.047(6) 0.022(6) 0.028(9) F5 0.137(11) 0.064(5) 0.228(17) 0.061(8) 0.106(11) 0.035(6) F6 0.128(8) 0.159(10) 0.047(4) 0.003(5) 0.008(4) 0.049(8) F7 0.243(5) 0.195(5) 0.108(3) 0.079(3) 0.042(3) 0.088(4) F8 0.214(5) 0.232(6) 0.113(3) 0.079(4) 0.055(3) 0.122(4) F9 0.363(18) 0.168(12) 0.243(13) 0.168(11) 0.223(14) 0.213(14) F10 0.129(9) 0.104(6) 0.195(10) 0.091(6) 0.048(8) 0.026(6) F11 0.147(11) 0.137(16) 0.194(15) 0.066(13) 0.092(11) 0.079(10) F12 0.42(2) 0.078(6) 0.177(11) 0.061(7) 0.193(15) 0.047(10) F3' 0.051(8) 0.118(13) 0.23(2) 0.000(12) -0.044(11) 0.014(8) F4' 0.24(2) 0.30(3) 0.162(18) 0.20(2) 0.142(17) 0.23(2) F5' 0.078(7) 0.118(11) 0.147(12) 0.034(8) 0.008(8) -0.004(6) F6' 0.111(11) 0.23(2) 0.137(13) 0.141(15) 0.063(9) 0.097(12) F9' 0.159(10) 0.052(6) 0.126(9) 0.044(6) 0.016(9) 0.057(7) F10' 0.079(9) 0.25(3) 0.195(15) 0.057(16) 0.026(9) 0.070(12) F11' 0.26(3) 0.101(15) 0.196(15) 0.047(14) 0.07(3) 0.12(2) F12' 0.107(11) 0.171(19) 0.199(16) 0.049(12) 0.032(11) -0.027(10) N1 0.062(2) 0.052(2) 0.059(2) 0.0164(17) -0.0048(17) 0.0200(18) N2 0.061(2) 0.060(2) 0.059(2) 0.0252(18) 0.0119(17) 0.0292(19) N3 0.056(2) 0.0423(18) 0.0449(18) 0.0120(15) 0.0068(15) 0.0199(16) N4 0.079(3) 0.051(2) 0.077(3) 0.006(2) -0.012(2) 0.015(2) N5 0.058(2) 0.0353(17) 0.0417(18) 0.0101(14) 0.0047(15) 0.0196(16) N6 0.056(2) 0.051(2) 0.065(2) 0.0281(18) 0.0192(18) 0.0218(18) N7 0.070(2) 0.0394(19) 0.0454(19) 0.0103(16) 0.0134(17) 0.0149(18) N8 0.072(2) 0.049(2) 0.0441(19) 0.0113(17) 0.0156(17) 0.0257(19) N9 0.072(2) 0.052(2) 0.051(2) 0.0134(17) -0.0040(17) 0.0297(19) P1 0.0688(8) 0.0577(7) 0.0714(8) 0.0259(6) 0.0199(6) 0.0279(7) P2 0.1366(16) 0.0652(9) 0.0887(11) 0.0396(8) 0.0447(10) 0.0526(10) C1 0.049(2) 0.048(2) 0.046(2) 0.0157(19) 0.0073(18) 0.021(2) C2 0.080(3) 0.086(4) 0.082(3) 0.038(3) -0.006(3) 0.038(3) C3 0.076(3) 0.070(3) 0.083(3) 0.025(3) -0.018(3) 0.023(3) C4 0.059(3) 0.048(3) 0.057(3) 0.014(2) 0.004(2) 0.015(2) C5 0.108(4) 0.046(3) 0.090(4) 0.006(3) -0.006(3) 0.019(3) C6 0.102(4) 0.043(3) 0.085(3) 0.015(2) 0.005(3) 0.030(3) C7 0.077(3) 0.053(3) 0.066(3) 0.021(2) 0.010(2) 0.027(2) C8 0.077(3) 0.053(3) 0.072(3) 0.031(2) 0.020(2) 0.034(2) C9 0.044(2) 0.041(2) 0.047(2) 0.0172(18) 0.0065(17) 0.0144(19) C10 0.068(3) 0.038(2) 0.082(3) 0.021(2) 0.002(3) 0.010(2) C11 0.076(3) 0.037(2) 0.064(3) 0.015(2) 0.011(2) 0.020(2) C12 0.056(2) 0.042(2) 0.040(2) 0.0134(18) 0.0054(18) 0.024(2) C13 0.092(4) 0.070(3) 0.054(3) 0.017(3) 0.027(3) 0.038(3) C14 0.077(3) 0.086(4) 0.062(3) 0.036(3) 0.026(3) 0.027(3) C15 0.075(3) 0.053(3) 0.060(3) 0.022(2) 0.016(2) 0.020(2) C16 0.068(3) 0.083(4) 0.113(4) 0.056(3) 0.038(3) 0.030(3) C17 0.091(3) 0.045(3) 0.056(3) 0.008(2) 0.001(2) 0.031(3) C18 0.124(5) 0.088(4) 0.099(4) 0.014(3) -0.028(3) 0.065(4) _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 1.975(4) . ? Pd1 C9 1.986(4) . ? Pd1 N9 2.061(3) . ? Pd1 N3 2.079(3) . ? Pd1 N7 2.810(3) . ? F1 P1 1.578(3) . ? F2 P1 1.568(3) . ? F3 P1 1.545(10) . ? F4 P1 1.558(11) . ? F5 P1 1.560(9) . ? F6 P1 1.486(9) . ? F7 P2 1.550(4) . ? F8 P2 1.553(4) . ? F9 P2 1.458(13) . ? F10 P2 1.497(10) . ? F11 P2 1.60(2) . ? F12 P2 1.539(11) . ? F3' P1 1.514(18) . ? F4' P1 1.498(16) . ? F5' P1 1.569(14) . ? F6' P1 1.679(15) . ? F9' P2 1.644(14) . ? F10' P2 1.505(18) . ? F11' P2 1.52(3) . ? F12' P2 1.562(15) . ? N1 C1 1.362(5) . ? N1 C3 1.386(5) . ? N1 C4 1.388(5) . ? N2 C1 1.331(5) . ? N2 C2 1.391(5) . ? N2 C8 1.472(5) . ? N3 C7 1.329(5) . ? N3 C4 1.333(5) . ? N4 C4 1.307(5) . ? N4 C5 1.334(6) . ? N5 C9 1.359(5) . ? N5 C11 1.398(5) . ? N5 C12 1.423(5) . ? N6 C9 1.317(5) . ? N6 C10 1.378(5) . ? N6 C16 1.462(6) . ? N7 C15 1.318(5) . ? N7 C12 1.318(5) . ? N8 C13 1.303(6) . ? N8 C12 1.319(5) . ? N9 C17 1.108(5) . ? C2 C3 1.322(7) . ? C2 H2 0.9300 . ? C3 H3 0.9300 . ? C5 C6 1.361(7) . ? C5 H5 0.9300 . ? C6 C7 1.368(6) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C10 C11 1.292(6) . ? C10 H10 0.9300 . ? C11 H11 0.9300 . ? C13 C14 1.376(7) . ? C13 H13 0.9300 . ? C14 C15 1.374(6) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 C18 1.472(7) . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 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 C9 95.44(15) . . ? C1 Pd1 N9 172.64(14) . . ? C9 Pd1 N9 89.64(14) . . ? C1 Pd1 N3 80.11(14) . . ? C9 Pd1 N3 174.92(13) . . ? N9 Pd1 N3 95.02(12) . . ? C1 Pd1 N7 96.31(13) . . ? C9 Pd1 N7 69.17(13) . . ? N9 Pd1 N7 90.47(12) . . ? N3 Pd1 N7 108.69(11) . . ? C1 N1 C3 110.5(4) . . ? C1 N1 C4 120.5(3) . . ? C3 N1 C4 128.7(4) . . ? C1 N2 C2 109.5(4) . . ? C1 N2 C8 127.3(3) . . ? C2 N2 C8 123.1(4) . . ? C7 N3 C4 116.0(4) . . ? C7 N3 Pd1 130.5(3) . . ? C4 N3 Pd1 113.5(3) . . ? C4 N4 C5 114.4(4) . . ? C9 N5 C11 108.8(4) . . ? C9 N5 C12 126.3(3) . . ? C11 N5 C12 124.9(4) . . ? C9 N6 C10 109.6(4) . . ? C9 N6 C16 124.2(4) . . ? C10 N6 C16 126.2(4) . . ? C15 N7 C12 114.5(4) . . ? C15 N7 Pd1 141.7(3) . . ? C12 N7 Pd1 103.7(3) . . ? C13 N8 C12 114.9(4) . . ? C17 N9 Pd1 176.6(4) . . ? F3' P1 F4' 91.4(13) . . ? F3' P1 F6 109.6(11) . . ? F4' P1 F6 156.2(12) . . ? F3' P1 F3 17.6(13) . . ? F4' P1 F3 108.2(14) . . ? F6 P1 F3 94.0(7) . . ? F3' P1 F5 154.2(11) . . ? F4' P1 F5 64.2(10) . . ? F6 P1 F5 93.1(7) . . ? F3 P1 F5 171.8(9) . . ? F3' P1 F4 69.7(12) . . ? F4' P1 F4 22.8(15) . . ? F6 P1 F4 176.0(8) . . ? F3 P1 F4 85.9(7) . . ? F5 P1 F4 86.7(9) . . ? F3' P1 F5' 169.2(11) . . ? F4' P1 F5' 97.8(11) . . ? F6 P1 F5' 62.7(8) . . ? F3 P1 F5' 151.8(10) . . ? F5 P1 F5' 36.3(5) . . ? F4 P1 F5' 118.5(9) . . ? F3' P1 F2 95.2(9) . . ? F4' P1 F2 91.2(5) . . ? F6 P1 F2 97.7(6) . . ? F3 P1 F2 89.4(5) . . ? F5 P1 F2 93.6(5) . . ? F4 P1 F2 86.3(6) . . ? F5' P1 F2 79.1(8) . . ? F3' P1 F1 84.4(9) . . ? F4' P1 F1 89.2(5) . . ? F6 P1 F1 82.1(6) . . ? F3 P1 F1 90.1(5) . . ? F5 P1 F1 87.0(5) . . ? F4 P1 F1 93.9(6) . . ? F5' P1 F1 101.2(8) . . ? F2 P1 F1 179.4(2) . . ? F3' P1 F6' 87.7(11) . . ? F4' P1 F6' 177.6(10) . . ? F6 P1 F6' 25.7(8) . . ? F3 P1 F6' 70.7(8) . . ? F5 P1 F6' 117.0(8) . . ? F4 P1 F6' 155.6(9) . . ? F5' P1 F6' 82.9(8) . . ? F2 P1 F6' 86.6(7) . . ? F1 P1 F6' 93.0(7) . . ? F9 P2 F10 93.4(7) . . ? F9 P2 F10' 108.4(10) . . ? F10 P2 F10' 148.8(9) . . ? F9 P2 F11' 159.1(13) . . ? F10 P2 F11' 66.6(13) . . ? F10' P2 F11' 92.4(13) . . ? F9 P2 F12 89.8(8) . . ? F10 P2 F12 173.9(8) . . ? F10' P2 F12 25.3(10) . . ? F11' P2 F12 110.7(13) . . ? F9 P2 F7 84.0(6) . . ? F10 P2 F7 80.7(6) . . ? F10' P2 F7 79.8(9) . . ? F11' P2 F7 97.9(15) . . ? F12 P2 F7 94.5(7) . . ? F9 P2 F8 96.4(6) . . ? F10 P2 F8 102.7(6) . . ? F10' P2 F8 96.8(9) . . ? F11' P2 F8 82.9(15) . . ? F12 P2 F8 82.1(7) . . ? F7 P2 F8 176.5(3) . . ? F9 P2 F12' 68.2(11) . . ? F10 P2 F12' 39.6(10) . . ? F10' P2 F12' 171.3(13) . . ? F11' P2 F12' 91.5(12) . . ? F12 P2 F12' 146.5(12) . . ? F7 P2 F12' 107.4(10) . . ? F8 P2 F12' 76.0(10) . . ? F9 P2 F11 173.3(11) . . ? F10 P2 F11 89.4(8) . . ? F10' P2 F11 66.7(10) . . ? F11' P2 F11 25.8(14) . . ? F12 P2 F11 86.8(9) . . ? F7 P2 F11 90.5(11) . . ? F8 P2 F11 88.8(11) . . ? F12' P2 F11 117.3(11) . . ? F9 P2 F9' 19.0(9) . . ? F10 P2 F9' 112.3(8) . . ? F10' P2 F9' 91.6(10) . . ? F11' P2 F9' 172.2(15) . . ? F12 P2 F9' 71.2(8) . . ? F7 P2 F9' 89.4(6) . . ? F8 P2 F9' 90.0(6) . . ? F12' P2 F9' 83.6(12) . . ? F11 P2 F9' 158.0(9) . . ? N2 C1 N1 105.5(3) . . ? N2 C1 Pd1 142.2(3) . . ? N1 C1 Pd1 112.2(3) . . ? C3 C2 N2 108.7(4) . . ? C3 C2 H2 125.7 . . ? N2 C2 H2 125.7 . . ? C2 C3 N1 105.8(4) . . ? C2 C3 H3 127.1 . . ? N1 C3 H3 127.1 . . ? N4 C4 N3 127.8(4) . . ? N4 C4 N1 118.7(4) . . ? N3 C4 N1 113.5(3) . . ? N4 C5 C6 123.3(5) . . ? N4 C5 H5 118.3 . . ? C6 C5 H5 118.3 . . ? C5 C6 C7 117.2(5) . . ? C5 C6 H6 121.4 . . ? C7 C6 H6 121.4 . . ? N3 C7 C6 121.2(4) . . ? N3 C7 H7 119.4 . . ? C6 C7 H7 119.4 . . ? N2 C8 H8A 109.5 . . ? N2 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? N2 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N6 C9 N5 106.1(3) . . ? N6 C9 Pd1 129.0(3) . . ? N5 C9 Pd1 124.9(3) . . ? C11 C10 N6 109.1(4) . . ? C11 C10 H10 125.5 . . ? N6 C10 H10 125.5 . . ? C10 C11 N5 106.5(4) . . ? C10 C11 H11 126.8 . . ? N5 C11 H11 126.8 . . ? N7 C12 N8 128.8(4) . . ? N7 C12 N5 115.9(3) . . ? N8 C12 N5 115.3(3) . . ? N8 C13 C14 122.7(4) . . ? N8 C13 H13 118.7 . . ? C14 C13 H13 118.7 . . ? C15 C14 C13 116.6(5) . . ? C15 C14 H14 121.7 . . ? C13 C14 H14 121.7 . . ? N7 C15 C14 122.4(4) . . ? N7 C15 H15 118.8 . . ? C14 C15 H15 118.8 . . ? N6 C16 H16A 109.5 . . ? N6 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? N6 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N9 C17 C18 178.6(5) . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 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 N3 C7 177.3(4) . . . . ? C9 Pd1 N3 C7 -153.6(15) . . . . ? N9 Pd1 N3 C7 2.9(4) . . . . ? N7 Pd1 N3 C7 -89.3(4) . . . . ? C1 Pd1 N3 C4 -4.1(3) . . . . ? C9 Pd1 N3 C4 25.0(17) . . . . ? N9 Pd1 N3 C4 -178.5(3) . . . . ? N7 Pd1 N3 C4 89.3(3) . . . . ? C1 Pd1 N7 C15 83.6(5) . . . . ? C9 Pd1 N7 C15 177.1(5) . . . . ? N9 Pd1 N7 C15 -93.5(4) . . . . ? N3 Pd1 N7 C15 2.0(5) . . . . ? C1 Pd1 N7 C12 -92.4(3) . . . . ? C9 Pd1 N7 C12 1.0(2) . . . . ? N9 Pd1 N7 C12 90.5(3) . . . . ? N3 Pd1 N7 C12 -174.1(2) . . . . ? C1 Pd1 N9 C17 71(6) . . . . ? C9 Pd1 N9 C17 -62(6) . . . . ? N3 Pd1 N9 C17 120(6) . . . . ? N7 Pd1 N9 C17 -132(6) . . . . ? C2 N2 C1 N1 -0.7(5) . . . . ? C8 N2 C1 N1 -176.6(4) . . . . ? C2 N2 C1 Pd1 175.9(4) . . . . ? C8 N2 C1 Pd1 -0.1(7) . . . . ? C3 N1 C1 N2 0.9(5) . . . . ? C4 N1 C1 N2 175.1(4) . . . . ? C3 N1 C1 Pd1 -176.8(3) . . . . ? C4 N1 C1 Pd1 -2.6(5) . . . . ? C9 Pd1 C1 N2 9.5(5) . . . . ? N9 Pd1 C1 N2 -123.9(11) . . . . ? N3 Pd1 C1 N2 -173.0(5) . . . . ? N7 Pd1 C1 N2 79.1(5) . . . . ? C9 Pd1 C1 N1 -174.1(3) . . . . ? N9 Pd1 C1 N1 52.5(13) . . . . ? N3 Pd1 C1 N1 3.4(3) . . . . ? N7 Pd1 C1 N1 -104.5(3) . . . . ? C1 N2 C2 C3 0.2(6) . . . . ? C8 N2 C2 C3 176.4(4) . . . . ? N2 C2 C3 N1 0.3(6) . . . . ? C1 N1 C3 C2 -0.8(6) . . . . ? C4 N1 C3 C2 -174.3(5) . . . . ? C5 N4 C4 N3 0.0(8) . . . . ? C5 N4 C4 N1 178.3(5) . . . . ? C7 N3 C4 N4 0.9(7) . . . . ? Pd1 N3 C4 N4 -177.9(4) . . . . ? C7 N3 C4 N1 -177.4(4) . . . . ? Pd1 N3 C4 N1 3.8(5) . . . . ? C1 N1 C4 N4 -179.4(4) . . . . ? C3 N1 C4 N4 -6.4(8) . . . . ? C1 N1 C4 N3 -0.9(6) . . . . ? C3 N1 C4 N3 172.1(4) . . . . ? C4 N4 C5 C6 -2.2(9) . . . . ? N4 C5 C6 C7 3.3(9) . . . . ? C4 N3 C7 C6 0.3(7) . . . . ? Pd1 N3 C7 C6 178.9(4) . . . . ? C5 C6 C7 N3 -2.3(8) . . . . ? C10 N6 C9 N5 -0.6(4) . . . . ? C16 N6 C9 N5 179.6(3) . . . . ? C10 N6 C9 Pd1 -178.9(3) . . . . ? C16 N6 C9 Pd1 1.3(6) . . . . ? C11 N5 C9 N6 1.1(4) . . . . ? C12 N5 C9 N6 -179.5(3) . . . . ? C11 N5 C9 Pd1 179.5(3) . . . . ? C12 N5 C9 Pd1 -1.1(5) . . . . ? C1 Pd1 C9 N6 -87.3(3) . . . . ? N9 Pd1 C9 N6 87.4(3) . . . . ? N3 Pd1 C9 N6 -116.1(15) . . . . ? N7 Pd1 C9 N6 178.0(4) . . . . ? C1 Pd1 C9 N5 94.7(3) . . . . ? N9 Pd1 C9 N5 -90.6(3) . . . . ? N3 Pd1 C9 N5 65.9(17) . . . . ? N7 Pd1 C9 N5 0.0(3) . . . . ? C9 N6 C10 C11 -0.2(5) . . . . ? C16 N6 C10 C11 179.6(4) . . . . ? N6 C10 C11 N5 0.9(5) . . . . ? C9 N5 C11 C10 -1.2(5) . . . . ? C12 N5 C11 C10 179.4(4) . . . . ? C15 N7 C12 N8 2.8(6) . . . . ? Pd1 N7 C12 N8 -179.9(3) . . . . ? C15 N7 C12 N5 -179.1(3) . . . . ? Pd1 N7 C12 N5 -1.8(3) . . . . ? C13 N8 C12 N7 -3.6(6) . . . . ? C13 N8 C12 N5 178.3(3) . . . . ? C9 N5 C12 N7 2.2(5) . . . . ? C11 N5 C12 N7 -178.5(3) . . . . ? C9 N5 C12 N8 -179.4(3) . . . . ? C11 N5 C12 N8 -0.1(5) . . . . ? C12 N8 C13 C14 1.4(7) . . . . ? N8 C13 C14 C15 1.0(7) . . . . ? C12 N7 C15 C14 0.1(6) . . . . ? Pd1 N7 C15 C14 -175.6(3) . . . . ? C13 C14 C15 N7 -1.8(7) . . . . ? Pd1 N9 C17 C18 36(27) . . . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.683 _refine_diff_density_min -0.254 _refine_diff_density_rms 0.072 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 1 0.077 0.500 1.000 307.8 53.4 #===END data_080709c _database_code_depnum_ccdc_archive 'CCDC 720715' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H30 F12 N10 P2 Pd' _chemical_formula_weight 951.00 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' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P-1 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.2820(13) _cell_length_b 13.3260(13) _cell_length_c 13.4030(15) _cell_angle_alpha 67.8290(10) _cell_angle_beta 65.292(2) _cell_angle_gamma 72.3640(10) _cell_volume 1965.8(3) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_min 0.45 _exptl_crystal_size_mid 0.46 _exptl_crystal_size_max 0.50 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.607 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 952 _exptl_absorpt_coefficient_mu 0.649 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8291 _exptl_absorpt_correction_T_max 0.8704 _exptl_absorpt_process_details sadbas _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10131 _diffrn_reflns_av_R_equivalents 0.0202 _diffrn_reflns_av_sigmaI/netI 0.0384 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.71 _diffrn_reflns_theta_max 25.01 _reflns_number_total 6820 _reflns_number_gt 5513 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0754P)^2^+3.1114P] 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 SHELXL _refine_ls_extinction_coef 0.0049(7) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 6820 _refine_ls_number_parameters 517 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0658 _refine_ls_R_factor_gt 0.0500 _refine_ls_wR_factor_ref 0.1486 _refine_ls_wR_factor_gt 0.1297 _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_restrained_S_all 1.059 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.29655(3) 0.36651(3) 0.74688(3) 0.04552(16) Uani 1 1 d . . . F1 F 0.2772(7) 0.8170(4) 0.9209(6) 0.173(3) Uani 1 1 d . . . F2 F 0.2610(4) 1.0721(3) 0.8564(5) 0.1205(16) Uani 1 1 d . . . F3 F 0.3931(5) 0.9341(6) 0.8452(12) 0.295(7) Uani 1 1 d . . . F4 F 0.2680(9) 0.9252(6) 1.0105(6) 0.202(4) Uani 1 1 d . . . F5 F 0.1408(5) 0.9587(6) 0.9413(8) 0.200(3) Uani 1 1 d . . . F6 F 0.2592(10) 0.9625(5) 0.7757(6) 0.223(5) Uani 1 1 d . . . F7 F 0.1633(6) 0.5383(11) 0.3931(6) 0.250(6) Uani 1 1 d . . . F8 F 0.3536(8) 0.5826(12) 0.1738(9) 0.320(7) Uani 1 1 d . . . F9 F 0.2296(10) 0.6800(6) 0.2804(11) 0.242(5) Uani 1 1 d . . . F10 F 0.3354(5) 0.5300(5) 0.3549(7) 0.163(2) Uani 1 1 d . . . F11 F 0.2777(10) 0.4407(5) 0.2861(9) 0.238(5) Uani 1 1 d . . . F12 F 0.1789(7) 0.5860(5) 0.2122(6) 0.173(3) Uani 1 1 d . . . N1 N 0.4684(3) 0.1824(3) 0.7298(3) 0.0437(8) Uani 1 1 d . . . N2 N 0.4720(3) 0.2229(3) 0.8679(3) 0.0473(9) Uani 1 1 d . . . N3 N 0.3467(3) 0.2759(3) 0.6326(3) 0.0514(9) Uani 1 1 d . . . N4 N 0.4832(4) 0.1228(4) 0.5804(4) 0.0652(12) Uani 1 1 d . . . N5 N 0.1831(3) 0.4377(3) 0.9616(3) 0.0441(8) Uani 1 1 d . . . N6 N 0.3150(3) 0.5305(3) 0.8397(4) 0.0510(9) Uani 1 1 d . . . N7 N 0.1122(4) 0.3042(3) 0.9495(4) 0.0542(10) Uani 1 1 d . . . N8 N 0.0366(4) 0.3617(4) 1.1186(4) 0.0563(10) Uani 1 1 d . . . N9 N 0.1706(3) 0.4738(3) 0.6885(3) 0.0534(10) Uani 1 1 d . . . N10 N 0.0427(14) 0.1211(13) 0.5743(10) 0.263(9) Uani 1 1 d . . . P1 P 0.27045(15) 0.94255(13) 0.88970(16) 0.0712(4) Uani 1 1 d . . . P2 P 0.25838(16) 0.56016(16) 0.27903(17) 0.0831(5) Uani 1 1 d . . . C1 C 0.4198(4) 0.2568(3) 0.7921(4) 0.0406(9) Uani 1 1 d . . . C2 C 0.5522(4) 0.1283(4) 0.8544(5) 0.0558(12) Uani 1 1 d . . . H2 H 0.5991 0.0904 0.8974 0.067 Uiso 1 1 calc R . . C3 C 0.5497(4) 0.1024(4) 0.7697(4) 0.0553(12) Uani 1 1 d . . . H3 H 0.5933 0.0428 0.7423 0.066 Uiso 1 1 calc R . . C4 C 0.4324(4) 0.1916(4) 0.6425(4) 0.0480(11) Uani 1 1 d . . . C5 C 0.4467(7) 0.1425(6) 0.4945(6) 0.086(2) Uani 1 1 d . . . H5 H 0.4807 0.0974 0.4464 0.103 Uiso 1 1 calc R . . C6 C 0.3608(7) 0.2267(6) 0.4751(6) 0.097(2) Uani 1 1 d . . . H6 H 0.3368 0.2389 0.4149 0.116 Uiso 1 1 calc R . . C7 C 0.3112(6) 0.2928(5) 0.5467(5) 0.0761(17) Uani 1 1 d . . . H7 H 0.2523 0.3499 0.5354 0.091 Uiso 1 1 calc R . . C8 C 0.4438(4) 0.2651(4) 0.9648(4) 0.0536(12) Uani 1 1 d . . . H8A H 0.4182 0.3439 0.9422 0.064 Uiso 1 1 calc R . . H8B H 0.5112 0.2523 0.9824 0.064 Uiso 1 1 calc R . . C9 C 0.3546(4) 0.2132(4) 1.0710(4) 0.0531(12) Uani 1 1 d . . . C10 C 0.3239(5) 0.2398(6) 1.1732(6) 0.0772(18) Uani 1 1 d . . . H10 H 0.3598 0.2895 1.1740 0.093 Uiso 1 1 calc R . . C11 C 0.2433(6) 0.1948(7) 1.2707(6) 0.093(2) Uani 1 1 d . . . H11 H 0.2248 0.2147 1.3365 0.111 Uiso 1 1 calc R . . C12 C 0.1884(5) 0.1204(6) 1.2740(6) 0.084(2) Uani 1 1 d . . . H12 H 0.1334 0.0898 1.3412 0.101 Uiso 1 1 calc R . . C13 C 0.2170(5) 0.0927(5) 1.1756(5) 0.0694(15) Uani 1 1 d . . . H13 H 0.1811 0.0422 1.1763 0.083 Uiso 1 1 calc R . . C14 C 0.2982(5) 0.1387(4) 1.0754(4) 0.0558(12) Uani 1 1 d . . . H14 H 0.3154 0.1192 1.0096 0.067 Uiso 1 1 calc R . . C15 C 0.2634(4) 0.4511(3) 0.8555(4) 0.0436(10) Uani 1 1 d . . . C16 C 0.2681(5) 0.5668(4) 0.9367(5) 0.0600(13) Uani 1 1 d . . . H16 H 0.2893 0.6217 0.9468 0.072 Uiso 1 1 calc R . . C17 C 0.1869(5) 0.5090(4) 1.0131(5) 0.0583(13) Uani 1 1 d . . . H17 H 0.1419 0.5152 1.0862 0.070 Uiso 1 1 calc R . . C18 C 0.1059(4) 0.3627(4) 1.0132(4) 0.0438(10) Uani 1 1 d . . . C19 C -0.0336(5) 0.2893(5) 1.1674(5) 0.0666(14) Uani 1 1 d . . . H19 H -0.0839 0.2846 1.2418 0.080 Uiso 1 1 calc R . . C20 C -0.0344(5) 0.2216(5) 1.1118(5) 0.0675(15) Uani 1 1 d . . . H20 H -0.0831 0.1710 1.1470 0.081 Uiso 1 1 calc R . . C21 C 0.0406(5) 0.2323(5) 1.0012(5) 0.0647(14) Uani 1 1 d . . . H21 H 0.0417 0.1882 0.9610 0.078 Uiso 1 1 calc R . . C22 C 0.4035(4) 0.5781(4) 0.7336(5) 0.0654(14) Uani 1 1 d . . . H22A H 0.4534 0.5202 0.6999 0.078 Uiso 1 1 calc R . . H22B H 0.4478 0.6099 0.7522 0.078 Uiso 1 1 calc R . . C23 C 0.3542(4) 0.6649(4) 0.6483(4) 0.0565(12) Uani 1 1 d . . . C24 C 0.3069(5) 0.7692(5) 0.6628(5) 0.0749(17) Uani 1 1 d . . . H24 H 0.3116 0.7845 0.7228 0.090 Uiso 1 1 calc R . . C25 C 0.2541(7) 0.8498(7) 0.5933(7) 0.110(3) Uani 1 1 d . . . H25 H 0.2237 0.9185 0.6057 0.132 Uiso 1 1 calc R . . C26 C 0.2463(8) 0.8291(10) 0.5066(9) 0.125(4) Uani 1 1 d . . . H26 H 0.2081 0.8838 0.4608 0.150 Uiso 1 1 calc R . . C27 C 0.2926(9) 0.7302(10) 0.4830(7) 0.118(4) Uani 1 1 d . . . H27 H 0.2869 0.7176 0.4220 0.142 Uiso 1 1 calc R . . C28 C 0.3498(7) 0.6469(7) 0.5554(6) 0.093(2) Uani 1 1 d . . . H28 H 0.3845 0.5799 0.5397 0.111 Uiso 1 1 calc R . . C29 C 0.1029(4) 0.5332(4) 0.6551(4) 0.0537(12) Uani 1 1 d . . . C30 C 0.0154(5) 0.6119(6) 0.6148(5) 0.0766(17) Uani 1 1 d . . . H30A H -0.0409 0.6398 0.6761 0.115 Uiso 1 1 calc R . . H30B H -0.0184 0.5764 0.5892 0.115 Uiso 1 1 calc R . . H30C H 0.0475 0.6716 0.5522 0.115 Uiso 1 1 calc R . . C31 C 0.0235(10) 0.1354(10) 0.6574(9) 0.151(5) Uani 1 1 d . . . C32 C -0.0025(9) 0.1522(9) 0.7628(9) 0.147(4) Uani 1 1 d . . . H32A H -0.0818 0.1556 0.8041 0.221 Uiso 1 1 calc R . . H32B H 0.0185 0.2201 0.7500 0.221 Uiso 1 1 calc R . . H32C H 0.0381 0.0926 0.8068 0.221 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 0.0493(2) 0.0431(2) 0.0491(2) -0.01232(15) -0.02920(17) 0.00183(15) F1 0.325(9) 0.055(3) 0.183(6) -0.007(3) -0.144(6) -0.045(4) F2 0.134(4) 0.069(3) 0.168(5) -0.026(3) -0.065(3) -0.021(2) F3 0.083(4) 0.132(5) 0.493(17) 0.025(8) -0.042(7) -0.010(4) F4 0.365(12) 0.168(6) 0.165(6) -0.026(5) -0.168(7) -0.086(7) F5 0.117(4) 0.176(6) 0.258(9) 0.015(6) -0.069(5) -0.054(4) F6 0.467(15) 0.112(4) 0.145(5) -0.035(4) -0.177(8) -0.022(6) F7 0.115(5) 0.522(18) 0.134(5) -0.169(8) -0.014(4) -0.030(7) F8 0.196(9) 0.409(17) 0.215(9) -0.004(10) 0.049(8) -0.148(10) F9 0.366(13) 0.123(5) 0.392(14) -0.116(7) -0.306(12) 0.060(6) F10 0.134(4) 0.162(5) 0.238(7) -0.080(5) -0.119(5) 0.019(4) F11 0.403(13) 0.090(4) 0.293(10) -0.083(5) -0.201(10) 0.014(6) F12 0.254(8) 0.163(5) 0.190(6) -0.077(5) -0.165(6) 0.005(5) N1 0.044(2) 0.043(2) 0.0420(19) -0.0108(16) -0.0183(16) -0.0007(16) N2 0.052(2) 0.042(2) 0.053(2) -0.0079(17) -0.0326(19) -0.0021(17) N3 0.061(2) 0.051(2) 0.052(2) -0.0161(18) -0.033(2) -0.0017(19) N4 0.085(3) 0.056(3) 0.053(2) -0.021(2) -0.025(2) -0.002(2) N5 0.053(2) 0.0362(19) 0.048(2) -0.0122(16) -0.0273(18) 0.0006(16) N6 0.056(2) 0.041(2) 0.063(2) -0.0114(18) -0.033(2) -0.0040(18) N7 0.061(2) 0.052(2) 0.060(2) -0.021(2) -0.029(2) -0.007(2) N8 0.055(2) 0.062(3) 0.057(3) -0.020(2) -0.021(2) -0.009(2) N9 0.054(2) 0.055(2) 0.053(2) -0.0135(19) -0.029(2) 0.000(2) N10 0.306(18) 0.280(16) 0.114(8) -0.072(10) -0.086(10) 0.108(13) P1 0.0883(11) 0.0570(9) 0.0899(11) -0.0143(8) -0.0513(9) -0.0207(8) P2 0.0856(12) 0.0815(12) 0.0926(13) -0.0419(10) -0.0320(10) -0.0049(9) C1 0.043(2) 0.035(2) 0.044(2) -0.0067(18) -0.0189(19) -0.0075(18) C2 0.055(3) 0.047(3) 0.067(3) -0.014(2) -0.037(3) 0.008(2) C3 0.052(3) 0.045(3) 0.060(3) -0.013(2) -0.025(2) 0.007(2) C4 0.053(3) 0.049(3) 0.042(2) -0.011(2) -0.019(2) -0.007(2) C5 0.128(6) 0.071(4) 0.076(4) -0.035(3) -0.046(4) -0.005(4) C6 0.139(7) 0.098(5) 0.088(5) -0.043(4) -0.073(5) 0.001(5) C7 0.089(4) 0.083(4) 0.078(4) -0.034(3) -0.057(4) 0.009(3) C8 0.069(3) 0.045(3) 0.065(3) -0.018(2) -0.047(3) 0.001(2) C9 0.063(3) 0.048(3) 0.061(3) -0.022(2) -0.044(3) 0.015(2) C10 0.067(4) 0.113(5) 0.081(4) -0.057(4) -0.042(3) 0.005(3) C11 0.074(4) 0.143(7) 0.072(4) -0.063(5) -0.036(4) 0.024(4) C12 0.068(4) 0.098(5) 0.068(4) -0.021(4) -0.032(3) 0.020(4) C13 0.072(4) 0.058(3) 0.074(4) -0.014(3) -0.037(3) 0.006(3) C14 0.070(3) 0.046(3) 0.054(3) -0.018(2) -0.032(3) 0.007(2) C15 0.051(2) 0.035(2) 0.052(3) -0.0098(19) -0.033(2) 0.0030(19) C16 0.077(4) 0.043(3) 0.075(4) -0.018(3) -0.040(3) -0.008(3) C17 0.084(4) 0.043(3) 0.060(3) -0.019(2) -0.039(3) -0.003(3) C18 0.046(2) 0.038(2) 0.051(3) -0.012(2) -0.029(2) 0.0035(19) C19 0.059(3) 0.079(4) 0.063(3) -0.024(3) -0.016(3) -0.017(3) C20 0.056(3) 0.070(4) 0.080(4) -0.020(3) -0.024(3) -0.016(3) C21 0.071(3) 0.062(3) 0.080(4) -0.027(3) -0.038(3) -0.011(3) C22 0.053(3) 0.053(3) 0.086(4) -0.017(3) -0.022(3) -0.011(2) C23 0.057(3) 0.061(3) 0.052(3) -0.014(2) -0.012(2) -0.022(2) C24 0.072(4) 0.060(4) 0.062(3) -0.010(3) -0.011(3) 0.002(3) C25 0.091(5) 0.086(5) 0.088(5) 0.010(4) -0.009(4) -0.002(4) C26 0.108(7) 0.150(9) 0.099(7) 0.026(7) -0.051(6) -0.053(7) C27 0.162(9) 0.154(9) 0.064(4) 0.015(5) -0.048(5) -0.109(8) C28 0.125(6) 0.098(5) 0.065(4) -0.017(4) -0.015(4) -0.066(5) C29 0.050(3) 0.059(3) 0.054(3) -0.011(2) -0.029(2) -0.002(2) C30 0.060(3) 0.093(4) 0.072(4) -0.023(3) -0.039(3) 0.015(3) C31 0.144(9) 0.155(9) 0.084(6) -0.012(6) -0.041(6) 0.043(7) C32 0.150(9) 0.161(10) 0.108(7) -0.048(7) -0.061(7) 0.040(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 C1 1.974(4) . ? Pd1 C15 1.996(4) . ? Pd1 N9 2.062(4) . ? Pd1 N3 2.075(4) . ? Pd1 N7 2.834(4) . ? F1 P1 1.547(4) . ? F2 P1 1.590(4) . ? F3 P1 1.466(6) . ? F4 P1 1.534(6) . ? F5 P1 1.544(7) . ? F6 P1 1.513(6) . ? F7 P2 1.513(7) . ? F8 P2 1.449(8) . ? F9 P2 1.531(6) . ? F10 P2 1.598(6) . ? F11 P2 1.506(6) . ? F12 P2 1.540(5) . ? N1 C1 1.373(6) . ? N1 C4 1.393(6) . ? N1 C3 1.394(6) . ? N2 C1 1.331(5) . ? N2 C2 1.397(6) . ? N2 C8 1.469(6) . ? N3 C7 1.338(6) . ? N3 C4 1.346(6) . ? N4 C4 1.311(6) . ? N4 C5 1.338(8) . ? N5 C15 1.359(6) . ? N5 C17 1.391(6) . ? N5 C18 1.427(6) . ? N6 C15 1.337(6) . ? N6 C16 1.387(7) . ? N6 C22 1.476(7) . ? N7 C18 1.322(6) . ? N7 C21 1.342(7) . ? N8 C18 1.323(6) . ? N8 C19 1.337(7) . ? N9 C29 1.129(6) . ? N10 C31 1.111(15) . ? C2 C3 1.320(7) . ? C2 H2 0.9300 . ? C3 H3 0.9300 . ? C5 C6 1.372(10) . ? C5 H5 0.9300 . ? C6 C7 1.375(9) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 C9 1.500(8) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C14 1.385(7) . ? C9 C10 1.408(7) . ? C10 C11 1.357(10) . ? C10 H10 0.9300 . ? C11 C12 1.376(10) . ? C11 H11 0.9300 . ? C12 C13 1.374(9) . ? C12 H12 0.9300 . ? C13 C14 1.383(8) . ? C13 H13 0.9300 . ? C14 H14 0.9300 . ? C16 C17 1.338(8) . ? C16 H16 0.9300 . ? C17 H17 0.9300 . ? C19 C20 1.375(8) . ? C19 H19 0.9300 . ? C20 C21 1.379(8) . ? C20 H20 0.9300 . ? C21 H21 0.9300 . ? C22 C23 1.498(8) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 C28 1.380(8) . ? C23 C24 1.392(8) . ? C24 C25 1.360(10) . ? C24 H24 0.9300 . ? C25 C26 1.341(14) . ? C25 H25 0.9300 . ? C26 C27 1.369(14) . ? C26 H26 0.9300 . ? C27 C28 1.430(12) . ? C27 H27 0.9300 . ? C28 H28 0.9300 . ? C29 C30 1.450(7) . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C31 C32 1.397(15) . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 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 C15 95.73(17) . . ? C1 Pd1 N9 174.64(16) . . ? C15 Pd1 N9 89.63(16) . . ? C1 Pd1 N3 79.85(16) . . ? C15 Pd1 N3 174.66(16) . . ? N9 Pd1 N3 94.79(15) . . ? C1 Pd1 N7 99.51(15) . . ? C15 Pd1 N7 68.42(16) . . ? N9 Pd1 N7 82.56(14) . . ? N3 Pd1 N7 115.08(14) . . ? C1 N1 C4 120.3(4) . . ? C1 N1 C3 110.8(4) . . ? C4 N1 C3 128.9(4) . . ? C1 N2 C2 110.8(4) . . ? C1 N2 C8 127.3(4) . . ? C2 N2 C8 121.4(4) . . ? C7 N3 C4 115.7(4) . . ? C7 N3 Pd1 129.6(4) . . ? C4 N3 Pd1 114.6(3) . . ? C4 N4 C5 114.9(5) . . ? C15 N5 C17 109.6(4) . . ? C15 N5 C18 125.8(4) . . ? C17 N5 C18 124.6(4) . . ? C15 N6 C16 109.4(4) . . ? C15 N6 C22 125.9(4) . . ? C16 N6 C22 124.6(4) . . ? C18 N7 C21 114.8(4) . . ? C18 N7 Pd1 103.6(3) . . ? C21 N7 Pd1 141.3(3) . . ? C18 N8 C19 115.0(4) . . ? C29 N9 Pd1 178.9(5) . . ? F3 P1 F6 95.8(7) . . ? F3 P1 F4 90.3(7) . . ? F6 P1 F4 173.8(6) . . ? F3 P1 F5 175.1(6) . . ? F6 P1 F5 87.2(6) . . ? F4 P1 F5 86.6(5) . . ? F3 P1 F1 93.1(4) . . ? F6 P1 F1 92.2(3) . . ? F4 P1 F1 88.3(4) . . ? F5 P1 F1 90.6(4) . . ? F3 P1 F2 88.0(4) . . ? F6 P1 F2 86.7(3) . . ? F4 P1 F2 92.6(3) . . ? F5 P1 F2 88.4(3) . . ? F1 P1 F2 178.5(3) . . ? F8 P2 F11 93.0(7) . . ? F8 P2 F7 176.0(7) . . ? F11 P2 F7 88.6(7) . . ? F8 P2 F9 91.7(7) . . ? F11 P2 F9 175.2(7) . . ? F7 P2 F9 86.7(6) . . ? F8 P2 F12 91.7(6) . . ? F11 P2 F12 88.9(4) . . ? F7 P2 F12 92.0(4) . . ? F9 P2 F12 90.4(4) . . ? F8 P2 F10 91.5(6) . . ? F11 P2 F10 90.0(4) . . ? F7 P2 F10 84.8(4) . . ? F9 P2 F10 90.4(3) . . ? F12 P2 F10 176.7(4) . . ? N2 C1 N1 104.4(4) . . ? N2 C1 Pd1 142.7(3) . . ? N1 C1 Pd1 112.8(3) . . ? C3 C2 N2 108.0(4) . . ? C3 C2 H2 126.0 . . ? N2 C2 H2 126.0 . . ? C2 C3 N1 106.1(4) . . ? C2 C3 H3 127.0 . . ? N1 C3 H3 127.0 . . ? N4 C4 N3 128.1(4) . . ? N4 C4 N1 119.5(4) . . ? N3 C4 N1 112.4(4) . . ? N4 C5 C6 122.3(6) . . ? N4 C5 H5 118.9 . . ? C6 C5 H5 118.9 . . ? C5 C6 C7 118.4(6) . . ? C5 C6 H6 120.8 . . ? C7 C6 H6 120.8 . . ? N3 C7 C6 120.7(6) . . ? N3 C7 H7 119.7 . . ? C6 C7 H7 119.7 . . ? N2 C8 C9 113.5(4) . . ? N2 C8 H8A 108.9 . . ? C9 C8 H8A 108.9 . . ? N2 C8 H8B 108.9 . . ? C9 C8 H8B 108.9 . . ? H8A C8 H8B 107.7 . . ? C14 C9 C10 116.4(5) . . ? C14 C9 C8 123.5(4) . . ? C10 C9 C8 120.1(5) . . ? C11 C10 C9 121.6(6) . . ? C11 C10 H10 119.2 . . ? C9 C10 H10 119.2 . . ? C10 C11 C12 121.3(6) . . ? C10 C11 H11 119.3 . . ? C12 C11 H11 119.3 . . ? C13 C12 C11 118.3(7) . . ? C13 C12 H12 120.9 . . ? C11 C12 H12 120.9 . . ? C12 C13 C14 121.0(6) . . ? C12 C13 H13 119.5 . . ? C14 C13 H13 119.5 . . ? C13 C14 C9 121.3(5) . . ? C13 C14 H14 119.3 . . ? C9 C14 H14 119.3 . . ? N6 C15 N5 106.5(4) . . ? N6 C15 Pd1 127.5(4) . . ? N5 C15 Pd1 126.0(3) . . ? C17 C16 N6 108.1(4) . . ? C17 C16 H16 126.0 . . ? N6 C16 H16 126.0 . . ? C16 C17 N5 106.3(5) . . ? C16 C17 H17 126.8 . . ? N5 C17 H17 126.8 . . ? N7 C18 N8 128.6(5) . . ? N7 C18 N5 116.0(4) . . ? N8 C18 N5 115.4(4) . . ? N8 C19 C20 122.5(5) . . ? N8 C19 H19 118.8 . . ? C20 C19 H19 118.8 . . ? C19 C20 C21 116.7(5) . . ? C19 C20 H20 121.6 . . ? C21 C20 H20 121.6 . . ? N7 C21 C20 122.4(5) . . ? N7 C21 H21 118.8 . . ? C20 C21 H21 118.8 . . ? N6 C22 C23 111.5(4) . . ? N6 C22 H22A 109.3 . . ? C23 C22 H22A 109.3 . . ? N6 C22 H22B 109.3 . . ? C23 C22 H22B 109.3 . . ? H22A C22 H22B 108.0 . . ? C28 C23 C24 116.8(6) . . ? C28 C23 C22 123.5(6) . . ? C24 C23 C22 119.7(5) . . ? C25 C24 C23 123.0(7) . . ? C25 C24 H24 118.5 . . ? C23 C24 H24 118.5 . . ? C26 C25 C24 119.3(9) . . ? C26 C25 H25 120.4 . . ? C24 C25 H25 120.4 . . ? C25 C26 C27 122.4(9) . . ? C25 C26 H26 118.8 . . ? C27 C26 H26 118.8 . . ? C26 C27 C28 117.8(8) . . ? C26 C27 H27 121.1 . . ? C28 C27 H27 121.1 . . ? C23 C28 C27 120.7(8) . . ? C23 C28 H28 119.6 . . ? C27 C28 H28 119.6 . . ? N9 C29 C30 178.0(6) . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? N10 C31 C32 179(2) . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 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 N3 C7 -175.3(5) . . . . ? C15 Pd1 N3 C7 -140.9(17) . . . . ? N9 Pd1 N3 C7 4.9(5) . . . . ? N7 Pd1 N3 C7 88.9(5) . . . . ? C1 Pd1 N3 C4 0.2(3) . . . . ? C15 Pd1 N3 C4 34.5(19) . . . . ? N9 Pd1 N3 C4 -179.7(3) . . . . ? N7 Pd1 N3 C4 -95.7(4) . . . . ? C1 Pd1 N7 C18 89.2(3) . . . . ? C15 Pd1 N7 C18 -3.3(3) . . . . ? N9 Pd1 N7 C18 -95.8(3) . . . . ? N3 Pd1 N7 C18 172.3(3) . . . . ? C1 Pd1 N7 C21 -83.5(6) . . . . ? C15 Pd1 N7 C21 -176.0(6) . . . . ? N9 Pd1 N7 C21 91.5(5) . . . . ? N3 Pd1 N7 C21 -0.4(6) . . . . ? C1 Pd1 N9 C29 -75(25) . . . . ? C15 Pd1 N9 C29 104(24) . . . . ? N3 Pd1 N9 C29 -73(24) . . . . ? N7 Pd1 N9 C29 172(100) . . . . ? C2 N2 C1 N1 -0.3(5) . . . . ? C8 N2 C1 N1 -172.2(4) . . . . ? C2 N2 C1 Pd1 174.9(4) . . . . ? C8 N2 C1 Pd1 2.9(8) . . . . ? C4 N1 C1 N2 178.9(4) . . . . ? C3 N1 C1 N2 0.8(5) . . . . ? C4 N1 C1 Pd1 2.1(5) . . . . ? C3 N1 C1 Pd1 -176.0(3) . . . . ? C15 Pd1 C1 N2 7.0(6) . . . . ? N9 Pd1 C1 N2 -174.4(15) . . . . ? N3 Pd1 C1 N2 -176.0(6) . . . . ? N7 Pd1 C1 N2 -62.0(5) . . . . ? C15 Pd1 C1 N1 -178.1(3) . . . . ? N9 Pd1 C1 N1 0(2) . . . . ? N3 Pd1 C1 N1 -1.2(3) . . . . ? N7 Pd1 C1 N1 112.8(3) . . . . ? C1 N2 C2 C3 -0.4(6) . . . . ? C8 N2 C2 C3 172.1(4) . . . . ? N2 C2 C3 N1 0.8(6) . . . . ? C1 N1 C3 C2 -1.0(6) . . . . ? C4 N1 C3 C2 -179.0(5) . . . . ? C5 N4 C4 N3 2.5(8) . . . . ? C5 N4 C4 N1 -176.3(5) . . . . ? C7 N3 C4 N4 -1.9(8) . . . . ? Pd1 N3 C4 N4 -178.0(4) . . . . ? C7 N3 C4 N1 177.0(5) . . . . ? Pd1 N3 C4 N1 0.9(5) . . . . ? C1 N1 C4 N4 177.0(4) . . . . ? C3 N1 C4 N4 -5.3(7) . . . . ? C1 N1 C4 N3 -2.0(6) . . . . ? C3 N1 C4 N3 175.8(4) . . . . ? C4 N4 C5 C6 -1.4(10) . . . . ? N4 C5 C6 C7 0.0(12) . . . . ? C4 N3 C7 C6 0.1(9) . . . . ? Pd1 N3 C7 C6 175.5(5) . . . . ? C5 C6 C7 N3 0.7(11) . . . . ? C1 N2 C8 C9 85.0(5) . . . . ? C2 N2 C8 C9 -86.2(5) . . . . ? N2 C8 C9 C14 -4.5(6) . . . . ? N2 C8 C9 C10 175.8(4) . . . . ? C14 C9 C10 C11 0.0(8) . . . . ? C8 C9 C10 C11 179.7(5) . . . . ? C9 C10 C11 C12 0.4(10) . . . . ? C10 C11 C12 C13 -0.2(10) . . . . ? C11 C12 C13 C14 -0.4(8) . . . . ? C12 C13 C14 C9 0.8(8) . . . . ? C10 C9 C14 C13 -0.6(7) . . . . ? C8 C9 C14 C13 179.7(5) . . . . ? C16 N6 C15 N5 0.6(5) . . . . ? C22 N6 C15 N5 -175.9(4) . . . . ? C16 N6 C15 Pd1 -178.9(3) . . . . ? C22 N6 C15 Pd1 4.6(6) . . . . ? C17 N5 C15 N6 -1.1(5) . . . . ? C18 N5 C15 N6 178.6(4) . . . . ? C17 N5 C15 Pd1 178.4(3) . . . . ? C18 N5 C15 Pd1 -1.9(6) . . . . ? C1 Pd1 C15 N6 84.0(4) . . . . ? N9 Pd1 C15 N6 -95.9(4) . . . . ? N3 Pd1 C15 N6 50.1(19) . . . . ? N7 Pd1 C15 N6 -178.0(4) . . . . ? C1 Pd1 C15 N5 -95.4(4) . . . . ? N9 Pd1 C15 N5 84.8(4) . . . . ? N3 Pd1 C15 N5 -129.3(17) . . . . ? N7 Pd1 C15 N5 2.6(3) . . . . ? C15 N6 C16 C17 0.2(6) . . . . ? C22 N6 C16 C17 176.7(4) . . . . ? N6 C16 C17 N5 -0.9(6) . . . . ? C15 N5 C17 C16 1.3(5) . . . . ? C18 N5 C17 C16 -178.5(4) . . . . ? C21 N7 C18 N8 -2.3(7) . . . . ? Pd1 N7 C18 N8 -177.2(4) . . . . ? C21 N7 C18 N5 178.3(4) . . . . ? Pd1 N7 C18 N5 3.4(4) . . . . ? C19 N8 C18 N7 2.2(7) . . . . ? C19 N8 C18 N5 -178.4(4) . . . . ? C15 N5 C18 N7 -2.0(6) . . . . ? C17 N5 C18 N7 177.6(4) . . . . ? C15 N5 C18 N8 178.5(4) . . . . ? C17 N5 C18 N8 -1.9(6) . . . . ? C18 N8 C19 C20 -0.5(8) . . . . ? N8 C19 C20 C21 -0.7(9) . . . . ? C18 N7 C21 C20 0.7(7) . . . . ? Pd1 N7 C21 C20 172.9(4) . . . . ? C19 C20 C21 N7 0.6(9) . . . . ? C15 N6 C22 C23 82.3(6) . . . . ? C16 N6 C22 C23 -93.6(6) . . . . ? N6 C22 C23 C28 -100.8(6) . . . . ? N6 C22 C23 C24 77.4(6) . . . . ? C28 C23 C24 C25 2.7(9) . . . . ? C22 C23 C24 C25 -175.5(6) . . . . ? C23 C24 C25 C26 0.2(11) . . . . ? C24 C25 C26 C27 -1.9(14) . . . . ? C25 C26 C27 C28 0.7(14) . . . . ? C24 C23 C28 C27 -3.9(9) . . . . ? C22 C23 C28 C27 174.2(6) . . . . ? C26 C27 C28 C23 2.4(11) . . . . ? Pd1 N9 C29 C30 -100(28) . . . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.869 _refine_diff_density_min -0.576 _refine_diff_density_rms 0.087 #===END data_080711c _database_code_depnum_ccdc_archive 'CCDC 720716' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H24 Cl F6 N8 O2 P Pd' _chemical_formula_weight 671.27 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' 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 12.0874(14) _cell_length_b 7.4205(11) _cell_length_c 29.316(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.932(2) _cell_angle_gamma 90.00 _cell_volume 2629.2(6) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_min 0.30 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_max 0.50 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.696 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1344 _exptl_absorpt_coefficient_mu 0.943 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8193 _exptl_absorpt_correction_T_max 0.8952 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12718 _diffrn_reflns_av_R_equivalents 0.0335 _diffrn_reflns_av_sigmaI/netI 0.0423 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 1.39 _diffrn_reflns_theta_max 25.01 _reflns_number_total 4614 _reflns_number_gt 3589 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0317P)^2^+6.1668P] 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 4614 _refine_ls_number_parameters 373 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0692 _refine_ls_R_factor_gt 0.0504 _refine_ls_wR_factor_ref 0.1120 _refine_ls_wR_factor_gt 0.1037 _refine_ls_goodness_of_fit_ref 1.102 _refine_ls_restrained_S_all 1.102 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.19884(3) -0.03074(6) 0.123102(14) 0.04513(15) Uani 1 1 d . . . Cl1 Cl 0.08729(15) -0.2681(2) 0.09837(6) 0.0804(5) Uani 1 1 d . . . F1 F 0.5699(6) 1.0447(7) 0.1299(3) 0.167(3) Uani 1 1 d . A . F2 F 0.6249(4) 0.6379(7) 0.1364(2) 0.140(2) Uani 1 1 d . A . F3 F 0.594(3) 0.894(3) 0.1814(5) 0.146(10) Uani 0.48(3) 1 d P A 1 F4 F 0.719(2) 0.907(6) 0.1268(13) 0.192(14) Uani 0.48(3) 1 d P A 1 F5 F 0.602(3) 0.801(5) 0.0805(7) 0.187(13) Uani 0.48(3) 1 d P A 1 F6 F 0.4761(14) 0.790(3) 0.1294(10) 0.118(7) Uani 0.48(3) 1 d P A 1 F3' F 0.670(2) 0.842(3) 0.1786(6) 0.123(6) Uani 0.52(3) 1 d P A 2 F4' F 0.707(2) 0.864(5) 0.1086(8) 0.158(11) Uani 0.52(3) 1 d P A 2 F5' F 0.538(2) 0.826(3) 0.0869(9) 0.162(11) Uani 0.52(3) 1 d P A 2 F6' F 0.490(2) 0.796(3) 0.1607(13) 0.157(11) Uani 0.52(3) 1 d P A 2 N1 N 0.3350(3) 0.1090(7) 0.19301(14) 0.0498(11) Uani 1 1 d . . . N2 N 0.3475(4) 0.3114(7) 0.14160(17) 0.0569(12) Uani 1 1 d . . . N3 N 0.2370(3) -0.1511(6) 0.18559(14) 0.0463(11) Uani 1 1 d . . . N4 N 0.3430(4) -0.0945(9) 0.25329(16) 0.0689(15) Uani 1 1 d . . . N5 N 0.0839(3) 0.1964(6) 0.05220(14) 0.0491(11) Uani 1 1 d . . . N6 N 0.2232(4) 0.0578(7) 0.02523(15) 0.0660(14) Uani 1 1 d . . . N7 N 0.0203(5) 0.2396(8) 0.12569(18) 0.0810(18) Uani 1 1 d . . . N8 N -0.0747(4) 0.3613(7) 0.06225(18) 0.0685(15) Uani 1 1 d . . . O1 O 0.9266(6) 0.8466(11) 0.1854(3) 0.169(3) Uani 1 1 d . . . H1C H 0.8575 0.8432 0.1796 0.203 Uiso 1 1 d R . . H1D H 0.9611 0.8161 0.1616 0.203 Uiso 1 1 d R . . O2 O 0.0812(8) 0.0893(19) 0.2483(3) 0.280(7) Uani 1 1 d . . . H2C H 0.0250 0.0397 0.2358 0.337 Uiso 1 1 d R . . H2D H 0.0594 0.1639 0.2682 0.337 Uiso 1 1 d R . . P1 P 0.59881(14) 0.8427(2) 0.13182(6) 0.0625(4) Uani 1 1 d . . . C1 C 0.2997(4) 0.1549(8) 0.14994(16) 0.0434(13) Uani 1 1 d . . . C2 C 0.4122(5) 0.3653(9) 0.1785(2) 0.0692(18) Uani 1 1 d . . . H2 H 0.4537 0.4705 0.1805 0.083 Uiso 1 1 calc R . . C3 C 0.4044(5) 0.2408(10) 0.2105(2) 0.0681(18) Uani 1 1 d . . . H3 H 0.4388 0.2416 0.2391 0.082 Uiso 1 1 calc R . . C4 C 0.3038(4) -0.0534(8) 0.21260(17) 0.0495(14) Uani 1 1 d . . . C5 C 0.3093(6) -0.2522(12) 0.2687(2) 0.081(2) Uani 1 1 d . . . H5 H 0.3350 -0.2893 0.2973 0.097 Uiso 1 1 calc R . . C6 C 0.2391(6) -0.3640(11) 0.2453(2) 0.081(2) Uani 1 1 d . . . H6 H 0.2158 -0.4729 0.2576 0.098 Uiso 1 1 calc R . . C7 C 0.2041(5) -0.3083(9) 0.2025(2) 0.0645(17) Uani 1 1 d . . . H7 H 0.1569 -0.3815 0.1853 0.077 Uiso 1 1 calc R . . C8 C 0.3385(6) 0.4144(9) 0.0987(2) 0.0722(19) Uani 1 1 d . . . H8A H 0.3359 0.5422 0.1056 0.087 Uiso 1 1 calc R . . H8B H 0.2701 0.3825 0.0829 0.087 Uiso 1 1 calc R . . C9 C 0.4335(6) 0.3779(11) 0.0684(2) 0.093(2) Uani 1 1 d . . . H9A H 0.5014 0.4056 0.0843 0.139 Uiso 1 1 calc R . . H9B H 0.4271 0.4514 0.0416 0.139 Uiso 1 1 calc R . . H9C H 0.4333 0.2530 0.0598 0.139 Uiso 1 1 calc R . . C10 C 0.1693(4) 0.0875(7) 0.06366(17) 0.0484(13) Uani 1 1 d . . . C11 C 0.1699(6) 0.1428(10) -0.0108(2) 0.083(2) Uani 1 1 d . . . H11 H 0.1904 0.1388 -0.0412 0.099 Uiso 1 1 calc R . . C12 C 0.0851(6) 0.2303(9) 0.0057(2) 0.0717(19) Uani 1 1 d . . . H12 H 0.0352 0.3017 -0.0107 0.086 Uiso 1 1 calc R . . C13 C 0.0042(5) 0.2692(7) 0.0821(2) 0.0525(14) Uani 1 1 d . . . C14 C -0.1479(6) 0.4321(9) 0.0906(3) 0.081(2) Uani 1 1 d . . . H14 H -0.2055 0.5007 0.0784 0.097 Uiso 1 1 calc R . . C15 C -0.1423(6) 0.4085(10) 0.1370(3) 0.087(2) Uani 1 1 d . . . H15 H -0.1952 0.4566 0.1562 0.104 Uiso 1 1 calc R . . C16 C -0.0550(7) 0.3109(11) 0.1533(3) 0.101(3) Uani 1 1 d . . . H16 H -0.0475 0.2933 0.1846 0.121 Uiso 1 1 calc R . . C17 C 0.3240(6) -0.0541(11) 0.0209(2) 0.086(2) Uani 1 1 d . . . H17A H 0.3805 0.0160 0.0058 0.103 Uiso 1 1 calc R . . H17B H 0.3519 -0.0843 0.0511 0.103 Uiso 1 1 calc R . . C18 C 0.3057(8) -0.2136(13) -0.0038(3) 0.131(4) Uani 1 1 d . . . H18A H 0.2509 -0.2848 0.0113 0.196 Uiso 1 1 calc R . . H18B H 0.3735 -0.2805 -0.0053 0.196 Uiso 1 1 calc R . . H18C H 0.2801 -0.1847 -0.0341 0.196 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(2) 0.0498(3) 0.0434(2) 0.0054(2) -0.00746(16) 0.0071(2) Cl1 0.0873(13) 0.0725(11) 0.0805(11) 0.0048(9) -0.0292(10) -0.0177(9) F1 0.187(6) 0.075(3) 0.240(7) 0.014(4) 0.005(5) 0.025(4) F2 0.128(4) 0.100(4) 0.193(6) 0.001(4) -0.012(4) 0.038(3) F3 0.24(3) 0.135(15) 0.065(7) -0.027(8) 0.009(13) -0.039(17) F4 0.063(12) 0.25(2) 0.26(4) 0.01(3) -0.033(16) -0.072(14) F5 0.18(2) 0.30(3) 0.081(11) -0.063(14) 0.063(14) -0.07(2) F6 0.058(7) 0.118(10) 0.18(2) -0.020(14) 0.010(11) -0.020(6) F3' 0.152(15) 0.145(12) 0.070(8) -0.002(7) -0.040(9) 0.012(10) F4' 0.12(2) 0.25(3) 0.108(12) 0.031(14) 0.072(13) -0.008(16) F5' 0.142(18) 0.218(16) 0.123(18) -0.003(15) -0.094(15) 0.031(16) F6' 0.114(16) 0.117(11) 0.24(3) -0.009(17) 0.106(18) 0.022(11) N1 0.040(3) 0.067(3) 0.042(3) -0.005(2) -0.003(2) 0.006(2) N2 0.052(3) 0.054(3) 0.064(3) 0.000(3) 0.004(2) 0.006(2) N3 0.039(2) 0.052(3) 0.049(3) 0.007(2) 0.001(2) 0.011(2) N4 0.060(3) 0.105(5) 0.042(3) 0.010(3) -0.006(2) 0.020(3) N5 0.046(3) 0.053(3) 0.048(3) 0.012(2) -0.005(2) 0.014(2) N6 0.071(3) 0.085(4) 0.042(3) 0.003(3) -0.003(2) 0.030(3) N7 0.078(4) 0.101(5) 0.064(4) 0.025(3) 0.021(3) 0.040(3) N8 0.056(3) 0.070(4) 0.079(4) 0.007(3) -0.008(3) 0.026(3) O1 0.120(6) 0.186(8) 0.203(8) -0.051(6) 0.033(5) 0.014(5) O2 0.194(10) 0.46(2) 0.191(9) 0.019(11) 0.008(7) 0.163(12) P1 0.0581(10) 0.0637(11) 0.0659(11) -0.0084(8) 0.0013(8) 0.0094(8) C1 0.036(3) 0.061(4) 0.033(3) -0.002(2) -0.001(2) 0.015(3) C2 0.063(4) 0.065(4) 0.079(5) -0.016(4) -0.007(4) -0.008(3) C3 0.060(4) 0.082(5) 0.062(4) -0.020(4) -0.010(3) 0.000(3) C4 0.038(3) 0.069(4) 0.041(3) 0.003(3) 0.004(2) 0.016(3) C5 0.064(5) 0.121(7) 0.059(4) 0.029(5) 0.003(4) 0.029(4) C6 0.073(5) 0.091(6) 0.080(5) 0.042(4) 0.011(4) 0.021(4) C7 0.057(4) 0.064(4) 0.072(4) 0.017(3) -0.001(3) 0.011(3) C8 0.078(5) 0.053(4) 0.085(5) 0.016(3) 0.002(4) -0.005(3) C9 0.105(6) 0.097(6) 0.077(5) 0.005(4) 0.019(4) -0.005(5) C10 0.052(3) 0.054(3) 0.039(3) 0.004(2) -0.009(2) 0.007(3) C11 0.100(6) 0.103(6) 0.045(4) 0.015(4) 0.002(4) 0.035(5) C12 0.078(5) 0.083(5) 0.054(4) 0.020(3) -0.008(3) 0.030(4) C13 0.052(3) 0.045(3) 0.061(4) 0.013(3) -0.001(3) 0.006(3) C14 0.060(4) 0.069(5) 0.113(6) 0.011(4) -0.007(4) 0.024(4) C15 0.077(5) 0.076(5) 0.108(6) 0.018(4) 0.033(4) 0.024(4) C16 0.116(7) 0.110(6) 0.078(5) 0.039(5) 0.031(5) 0.047(5) C17 0.078(5) 0.110(6) 0.070(4) -0.007(4) -0.003(4) 0.036(4) C18 0.138(9) 0.117(8) 0.135(8) -0.034(7) -0.026(7) 0.044(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 C10 1.978(5) . ? Pd1 C1 1.993(6) . ? Pd1 N3 2.083(4) . ? Pd1 Cl1 2.3269(17) . ? Pd1 N7 2.948(5) . ? F1 P1 1.540(5) . ? F2 P1 1.557(5) . ? F3 P1 1.505(14) . ? F4 P1 1.53(2) . ? F5 P1 1.537(19) . ? F6 P1 1.535(17) . ? F3' P1 1.605(13) . ? F4' P1 1.497(19) . ? F5' P1 1.502(15) . ? F6' P1 1.611(18) . ? N1 C1 1.369(6) . ? N1 C3 1.382(7) . ? N1 C4 1.390(7) . ? N2 C1 1.322(7) . ? N2 C2 1.384(7) . ? N2 C8 1.474(7) . ? N3 C7 1.331(7) . ? N3 C4 1.336(7) . ? N4 C4 1.312(7) . ? N4 C5 1.321(9) . ? N5 C10 1.349(6) . ? N5 C12 1.386(7) . ? N5 C13 1.420(7) . ? N6 C10 1.329(7) . ? N6 C11 1.380(7) . ? N6 C17 1.482(8) . ? N7 C13 1.308(7) . ? N7 C16 1.337(8) . ? N8 C13 1.302(7) . ? N8 C14 1.333(8) . ? C2 C3 1.320(9) . ? C5 C6 1.365(10) . ? C6 C7 1.379(8) . ? C8 C9 1.488(9) . ? C11 C12 1.313(8) . ? C14 C15 1.370(10) . ? C15 C16 1.361(9) . ? C17 C18 1.402(10) . ? 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 C10 Pd1 C1 98.2(2) . . ? C10 Pd1 N3 177.5(2) . . ? C1 Pd1 N3 79.86(19) . . ? C10 Pd1 Cl1 88.04(17) . . ? C1 Pd1 Cl1 173.66(15) . . ? N3 Pd1 Cl1 93.91(14) . . ? C10 Pd1 N7 66.36(19) . . ? C1 Pd1 N7 87.86(19) . . ? N3 Pd1 N7 114.89(15) . . ? Cl1 Pd1 N7 95.89(14) . . ? C1 N1 C3 110.2(5) . . ? C1 N1 C4 120.9(5) . . ? C3 N1 C4 128.9(5) . . ? C1 N2 C2 110.6(5) . . ? C1 N2 C8 125.9(5) . . ? C2 N2 C8 123.4(5) . . ? C7 N3 C4 115.8(5) . . ? C7 N3 Pd1 129.9(4) . . ? C4 N3 Pd1 114.3(4) . . ? C4 N4 C5 114.1(6) . . ? C10 N5 C12 109.5(5) . . ? C10 N5 C13 126.8(4) . . ? C12 N5 C13 123.8(5) . . ? C10 N6 C11 110.1(5) . . ? C10 N6 C17 125.6(5) . . ? C11 N6 C17 124.3(5) . . ? C13 N7 C16 115.6(6) . . ? C13 N7 Pd1 100.8(4) . . ? C16 N7 Pd1 142.3(4) . . ? C13 N8 C14 114.6(6) . . ? F4' P1 F5' 91.7(12) . . ? F4' P1 F3 117.5(13) . . ? F5' P1 F3 147.2(13) . . ? F4' P1 F4 24.0(16) . . ? F5' P1 F4 112.9(13) . . ? F3 P1 F4 93.9(13) . . ? F4' P1 F6 149.3(12) . . ? F5' P1 F6 58.7(9) . . ? F3 P1 F6 93.2(11) . . ? F4 P1 F6 171.2(14) . . ? F4' P1 F5 62.7(11) . . ? F5' P1 F5 31.2(9) . . ? F3 P1 F5 176.8(14) . . ? F4 P1 F5 86.0(12) . . ? F6 P1 F5 86.7(10) . . ? F4' P1 F1 94.6(14) . . ? F5' P1 F1 86.6(9) . . ? F3 P1 F1 77.0(12) . . ? F4 P1 F1 84.7(17) . . ? F6 P1 F1 91.7(9) . . ? F5 P1 F1 99.8(15) . . ? F4' P1 F2 88.0(14) . . ? F5' P1 F2 95.2(9) . . ? F3 P1 F2 100.2(12) . . ? F4 P1 F2 97.0(17) . . ? F6 P1 F2 87.0(8) . . ? F5 P1 F2 83.1(15) . . ? F1 P1 F2 176.8(4) . . ? F4' P1 F3' 85.9(11) . . ? F5' P1 F3' 174.3(10) . . ? F3 P1 F3' 37.4(10) . . ? F4 P1 F3' 66.0(12) . . ? F6 P1 F3' 122.7(10) . . ? F5 P1 F3' 144.5(11) . . ? F1 P1 F3' 98.8(8) . . ? F2 P1 F3' 79.5(8) . . ? F4' P1 F6' 171.8(16) . . ? F5' P1 F6' 93.0(11) . . ? F3 P1 F6' 60.0(10) . . ? F4 P1 F6' 153.6(13) . . ? F6 P1 F6' 34.4(9) . . ? F5 P1 F6' 120.4(12) . . ? F1 P1 F6' 92.3(8) . . ? F2 P1 F6' 85.0(8) . . ? F3' P1 F6' 88.7(11) . . ? N2 C1 N1 105.0(5) . . ? N2 C1 Pd1 143.2(4) . . ? N1 C1 Pd1 111.8(4) . . ? C3 C2 N2 107.9(6) . . ? C2 C3 N1 106.3(6) . . ? N4 C4 N3 128.2(6) . . ? N4 C4 N1 118.7(6) . . ? N3 C4 N1 113.0(4) . . ? N4 C5 C6 124.0(6) . . ? C5 C6 C7 117.0(7) . . ? N3 C7 C6 120.8(7) . . ? N2 C8 C9 111.5(5) . . ? N6 C10 N5 105.8(4) . . ? N6 C10 Pd1 126.1(4) . . ? N5 C10 Pd1 127.7(4) . . ? C12 C11 N6 107.6(6) . . ? C11 C12 N5 107.1(5) . . ? N8 C13 N7 128.4(6) . . ? N8 C13 N5 115.0(5) . . ? N7 C13 N5 116.5(5) . . ? N8 C14 C15 123.1(6) . . ? C16 C15 C14 116.3(7) . . ? N7 C16 C15 122.0(7) . . ? C18 C17 N6 113.2(7) . . ? 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 C10 Pd1 N3 C7 -142(5) . . . . ? C1 Pd1 N3 C7 -179.4(5) . . . . ? Cl1 Pd1 N3 C7 -0.6(5) . . . . ? N7 Pd1 N3 C7 97.7(5) . . . . ? C10 Pd1 N3 C4 38(5) . . . . ? C1 Pd1 N3 C4 1.3(3) . . . . ? Cl1 Pd1 N3 C4 -179.8(3) . . . . ? N7 Pd1 N3 C4 -81.5(4) . . . . ? C10 Pd1 N7 C13 11.5(4) . . . . ? C1 Pd1 N7 C13 111.3(4) . . . . ? N3 Pd1 N7 C13 -170.9(4) . . . . ? Cl1 Pd1 N7 C13 -73.8(4) . . . . ? C10 Pd1 N7 C16 176.2(10) . . . . ? C1 Pd1 N7 C16 -83.9(9) . . . . ? N3 Pd1 N7 C16 -6.1(10) . . . . ? Cl1 Pd1 N7 C16 90.9(9) . . . . ? C2 N2 C1 N1 -0.1(6) . . . . ? C8 N2 C1 N1 177.7(5) . . . . ? C2 N2 C1 Pd1 -179.8(5) . . . . ? C8 N2 C1 Pd1 -2.0(10) . . . . ? C3 N1 C1 N2 0.3(6) . . . . ? C4 N1 C1 N2 -177.6(4) . . . . ? C3 N1 C1 Pd1 -179.9(4) . . . . ? C4 N1 C1 Pd1 2.2(6) . . . . ? C10 Pd1 C1 N2 -0.5(7) . . . . ? N3 Pd1 C1 N2 178.0(7) . . . . ? Cl1 Pd1 C1 N2 167.3(9) . . . . ? N7 Pd1 C1 N2 -66.3(6) . . . . ? C10 Pd1 C1 N1 179.7(3) . . . . ? N3 Pd1 C1 N1 -1.8(3) . . . . ? Cl1 Pd1 C1 N1 -12.4(16) . . . . ? N7 Pd1 C1 N1 114.0(3) . . . . ? C1 N2 C2 C3 -0.2(7) . . . . ? C8 N2 C2 C3 -178.1(5) . . . . ? N2 C2 C3 N1 0.4(7) . . . . ? C1 N1 C3 C2 -0.4(7) . . . . ? C4 N1 C3 C2 177.3(5) . . . . ? C5 N4 C4 N3 -1.0(8) . . . . ? C5 N4 C4 N1 -179.4(5) . . . . ? C7 N3 C4 N4 1.6(8) . . . . ? Pd1 N3 C4 N4 -179.0(4) . . . . ? C7 N3 C4 N1 -179.9(4) . . . . ? Pd1 N3 C4 N1 -0.5(5) . . . . ? C1 N1 C4 N4 177.5(5) . . . . ? C3 N1 C4 N4 0.0(8) . . . . ? C1 N1 C4 N3 -1.1(7) . . . . ? C3 N1 C4 N3 -178.6(5) . . . . ? C4 N4 C5 C6 -0.7(10) . . . . ? N4 C5 C6 C7 1.5(11) . . . . ? C4 N3 C7 C6 -0.6(8) . . . . ? Pd1 N3 C7 C6 -179.8(4) . . . . ? C5 C6 C7 N3 -0.8(10) . . . . ? C1 N2 C8 C9 -96.0(7) . . . . ? C2 N2 C8 C9 81.5(7) . . . . ? C11 N6 C10 N5 -2.0(7) . . . . ? C17 N6 C10 N5 179.6(6) . . . . ? C11 N6 C10 Pd1 170.9(5) . . . . ? C17 N6 C10 Pd1 -7.4(9) . . . . ? C12 N5 C10 N6 1.2(7) . . . . ? C13 N5 C10 N6 -178.2(5) . . . . ? C12 N5 C10 Pd1 -171.7(5) . . . . ? C13 N5 C10 Pd1 9.0(8) . . . . ? C1 Pd1 C10 N6 94.3(5) . . . . ? N3 Pd1 C10 N6 57(5) . . . . ? Cl1 Pd1 C10 N6 -84.4(5) . . . . ? N7 Pd1 C10 N6 178.4(6) . . . . ? C1 Pd1 C10 N5 -94.3(5) . . . . ? N3 Pd1 C10 N5 -131(4) . . . . ? Cl1 Pd1 C10 N5 87.1(5) . . . . ? N7 Pd1 C10 N5 -10.2(5) . . . . ? C10 N6 C11 C12 2.2(9) . . . . ? C17 N6 C11 C12 -179.4(7) . . . . ? N6 C11 C12 N5 -1.4(9) . . . . ? C10 N5 C12 C11 0.2(8) . . . . ? C13 N5 C12 C11 179.6(6) . . . . ? C14 N8 C13 N7 -0.6(10) . . . . ? C14 N8 C13 N5 -178.8(5) . . . . ? C16 N7 C13 N8 1.2(11) . . . . ? Pd1 N7 C13 N8 170.9(6) . . . . ? C16 N7 C13 N5 179.3(6) . . . . ? Pd1 N7 C13 N5 -11.0(6) . . . . ? C10 N5 C13 N8 -175.7(5) . . . . ? C12 N5 C13 N8 5.1(8) . . . . ? C10 N5 C13 N7 5.9(9) . . . . ? C12 N5 C13 N7 -173.3(6) . . . . ? C13 N8 C14 C15 -0.9(10) . . . . ? N8 C14 C15 C16 1.6(12) . . . . ? C13 N7 C16 C15 -0.3(12) . . . . ? Pd1 N7 C16 C15 -163.6(6) . . . . ? C14 C15 C16 N7 -0.9(13) . . . . ? C10 N6 C17 C18 111.3(8) . . . . ? C11 N6 C17 C18 -66.9(10) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.583 _refine_diff_density_min -0.749 _refine_diff_density_rms 0.077 #===END data_080709d _database_code_depnum_ccdc_archive 'CCDC 720717' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H12 Cl2 N4 Pd' _chemical_formula_weight 413.58 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' Cl Cl 0.1484 0.1585 '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 5.1207(14) _cell_length_b 24.454(3) _cell_length_c 23.766(3) _cell_angle_alpha 90.00 _cell_angle_beta 93.217(2) _cell_angle_gamma 90.00 _cell_volume 2971.3(9) _cell_formula_units_Z 8 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour colorless _exptl_crystal_size_min 0.15 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_max 0.48 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.849 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1632 _exptl_absorpt_coefficient_mu 1.605 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8193 _exptl_absorpt_correction_T_max 0.8952 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15239 _diffrn_reflns_av_R_equivalents 0.0458 _diffrn_reflns_av_sigmaI/netI 0.0484 _diffrn_reflns_limit_h_min -5 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.67 _diffrn_reflns_theta_max 25.01 _reflns_number_total 5218 _reflns_number_gt 4144 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0145P)^2^+10.9020P] 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 5218 _refine_ls_number_parameters 379 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0677 _refine_ls_R_factor_gt 0.0509 _refine_ls_wR_factor_ref 0.0971 _refine_ls_wR_factor_gt 0.0916 _refine_ls_goodness_of_fit_ref 1.138 _refine_ls_restrained_S_all 1.138 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.11634(9) 0.37645(2) 0.10434(2) 0.03548(14) Uani 1 1 d . . . Pd2 Pd 0.19007(9) 0.66261(2) 0.20471(2) 0.03901(14) Uani 1 1 d . . . Cl1 Cl -0.1856(3) 0.35107(8) 0.16668(8) 0.0578(5) Uani 1 1 d . . . Cl2 Cl -0.0343(4) 0.30518(7) 0.04439(7) 0.0533(5) Uani 1 1 d . . . Cl3 Cl -0.0806(3) 0.62563(7) 0.13175(7) 0.0530(4) Uani 1 1 d . . . Cl4 Cl 0.0046(4) 0.60620(9) 0.26823(9) 0.0750(6) Uani 1 1 d . . . N1 N 0.4748(9) 0.4624(2) 0.1206(2) 0.0361(12) Uani 1 1 d . . . N2 N 0.2812(10) 0.4637(2) 0.1972(2) 0.0435(13) Uani 1 1 d . . . N3 N 0.3787(9) 0.4034(2) 0.0481(2) 0.0332(11) Uani 1 1 d . . . N4 N 0.7225(10) 0.4675(2) 0.0407(2) 0.0408(13) Uani 1 1 d . . . N5 N 0.6067(9) 0.7334(2) 0.2308(2) 0.0400(13) Uani 1 1 d . . . N6 N 0.4995(10) 0.7085(2) 0.3129(2) 0.0455(14) Uani 1 1 d . . . N7 N 0.3790(9) 0.7116(2) 0.1494(2) 0.0366(12) Uani 1 1 d . . . N8 N 0.7534(10) 0.7692(2) 0.1473(3) 0.0497(14) Uani 1 1 d . . . C1 C 0.2838(11) 0.4366(2) 0.1482(3) 0.0364(14) Uani 1 1 d . . . C2 C 0.4686(13) 0.5048(3) 0.2003(3) 0.0495(17) Uani 1 1 d . . . H2 H 0.5030 0.5284 0.2305 0.059 Uiso 1 1 calc R . . C3 C 0.5892(13) 0.5043(3) 0.1526(3) 0.0462(17) Uani 1 1 d . . . H3 H 0.7235 0.5273 0.1426 0.055 Uiso 1 1 calc R . . C4 C 0.5347(11) 0.4442(2) 0.0674(2) 0.0340(14) Uani 1 1 d . . . C5 C 0.7537(12) 0.4478(3) -0.0111(3) 0.0449(17) Uani 1 1 d . . . H5 H 0.8894 0.4617 -0.0313 0.054 Uiso 1 1 calc R . . C6 C 0.5970(13) 0.4085(3) -0.0359(3) 0.0463(17) Uani 1 1 d . . . H6 H 0.6163 0.3976 -0.0730 0.056 Uiso 1 1 calc R . . C7 C 0.4091(12) 0.3857(3) -0.0040(3) 0.0439(16) Uani 1 1 d . . . H7 H 0.3031 0.3578 -0.0189 0.053 Uiso 1 1 calc R . . C8 C 0.1224(13) 0.4511(3) 0.2454(3) 0.0545(19) Uani 1 1 d . . . H8A H -0.0028 0.4227 0.2345 0.065 Uiso 1 1 calc R . . H8B H 0.0252 0.4834 0.2552 0.065 Uiso 1 1 calc R . . C9 C 0.2875(14) 0.4324(3) 0.2961(3) 0.0547(19) Uani 1 1 d . . . C10 C 0.4858(15) 0.3946(3) 0.2915(3) 0.065(2) Uani 1 1 d . . . H10 H 0.5207 0.3803 0.2564 0.078 Uiso 1 1 calc R . . C11 C 0.6310(19) 0.3783(4) 0.3387(5) 0.095(3) Uani 1 1 d . . . H11 H 0.7683 0.3538 0.3355 0.114 Uiso 1 1 calc R . . C12 C 0.575(3) 0.3979(6) 0.3898(5) 0.125(6) Uani 1 1 d . . . H12 H 0.6751 0.3865 0.4215 0.150 Uiso 1 1 calc R . . C13 C 0.376(3) 0.4338(6) 0.3960(5) 0.120(5) Uani 1 1 d . . . H13 H 0.3364 0.4458 0.4317 0.144 Uiso 1 1 calc R . . C14 C 0.2329(19) 0.4522(4) 0.3488(4) 0.083(3) Uani 1 1 d . . . H14 H 0.1004 0.4778 0.3523 0.099 Uiso 1 1 calc R . . C15 C 0.4363(12) 0.7005(3) 0.2588(3) 0.0399(15) Uani 1 1 d . . . C16 C 0.7089(13) 0.7453(3) 0.3189(3) 0.0523(18) Uani 1 1 d . . . H16 H 0.7886 0.7568 0.3529 0.063 Uiso 1 1 calc R . . C17 C 0.7749(13) 0.7609(3) 0.2687(3) 0.0472(17) Uani 1 1 d . . . H17 H 0.9067 0.7853 0.2603 0.057 Uiso 1 1 calc R . . C18 C 0.5844(12) 0.7388(3) 0.1729(3) 0.0382(15) Uani 1 1 d . . . C19 C 0.7050(15) 0.7734(3) 0.0917(3) 0.058(2) Uani 1 1 d . . . H19 H 0.8186 0.7942 0.0713 0.069 Uiso 1 1 calc R . . C20 C 0.4974(14) 0.7486(3) 0.0629(3) 0.0556(19) Uani 1 1 d . . . H20 H 0.4672 0.7530 0.0242 0.067 Uiso 1 1 calc R . . C21 C 0.3357(13) 0.7171(3) 0.0941(3) 0.0475(17) Uani 1 1 d . . . H21 H 0.1939 0.6993 0.0761 0.057 Uiso 1 1 calc R . . C22 C 0.3743(14) 0.6849(3) 0.3610(3) 0.0532(18) Uani 1 1 d . . . H22A H 0.2212 0.6643 0.3476 0.064 Uiso 1 1 calc R . . H22B H 0.3166 0.7142 0.3849 0.064 Uiso 1 1 calc R . . C23 C 0.5580(14) 0.6476(3) 0.3953(3) 0.0515(18) Uani 1 1 d . . . C24 C 0.7315(17) 0.6681(4) 0.4360(3) 0.069(2) Uani 1 1 d . . . H24 H 0.7257 0.7052 0.4446 0.083 Uiso 1 1 calc R . . C25 C 0.9130(19) 0.6358(5) 0.4645(4) 0.092(3) Uani 1 1 d . . . H25 H 1.0333 0.6509 0.4909 0.111 Uiso 1 1 calc R . . C26 C 0.914(2) 0.5810(5) 0.4536(5) 0.098(3) Uani 1 1 d . . . H26 H 1.0341 0.5584 0.4730 0.117 Uiso 1 1 calc R . . C27 C 0.741(2) 0.5596(4) 0.4145(5) 0.093(3) Uani 1 1 d . . . H27 H 0.7405 0.5221 0.4077 0.112 Uiso 1 1 calc R . . C28 C 0.5666(18) 0.5930(4) 0.3847(4) 0.073(2) Uani 1 1 d . . . H28 H 0.4530 0.5780 0.3569 0.087 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 0.0323(3) 0.0362(3) 0.0377(3) 0.0062(2) -0.00083(19) 0.0021(2) Pd2 0.0337(3) 0.0403(3) 0.0436(3) -0.0086(2) 0.0070(2) -0.0052(2) Cl1 0.0509(10) 0.0578(12) 0.0652(12) 0.0127(9) 0.0067(9) 0.0048(9) Cl2 0.0638(11) 0.0456(10) 0.0495(10) 0.0025(8) -0.0073(8) -0.0102(9) Cl3 0.0484(10) 0.0563(11) 0.0539(11) -0.0107(9) -0.0004(8) -0.0154(9) Cl4 0.0751(14) 0.0799(15) 0.0712(14) -0.0076(11) 0.0145(11) -0.0192(11) N1 0.037(3) 0.033(3) 0.039(3) 0.004(2) 0.000(2) 0.002(2) N2 0.038(3) 0.051(4) 0.041(3) 0.002(3) 0.003(2) 0.003(3) N3 0.032(3) 0.034(3) 0.033(3) 0.002(2) 0.001(2) 0.003(2) N4 0.035(3) 0.041(3) 0.045(3) 0.012(3) -0.001(2) 0.003(2) N5 0.035(3) 0.038(3) 0.047(3) -0.010(3) 0.003(2) -0.006(2) N6 0.047(3) 0.047(3) 0.042(3) -0.009(3) 0.003(3) -0.001(3) N7 0.035(3) 0.037(3) 0.039(3) -0.009(2) 0.003(2) -0.001(2) N8 0.042(3) 0.044(3) 0.064(4) 0.002(3) 0.007(3) -0.008(3) C1 0.031(3) 0.038(4) 0.040(4) 0.005(3) -0.003(3) 0.004(3) C2 0.058(4) 0.043(4) 0.047(4) -0.009(3) -0.001(3) -0.006(3) C3 0.053(4) 0.047(4) 0.038(4) 0.002(3) -0.006(3) -0.005(3) C4 0.033(3) 0.034(3) 0.035(3) 0.012(3) 0.001(3) 0.006(3) C5 0.036(4) 0.048(4) 0.051(4) 0.016(3) 0.008(3) 0.013(3) C6 0.051(4) 0.054(4) 0.034(4) 0.001(3) 0.003(3) 0.011(4) C7 0.044(4) 0.045(4) 0.043(4) -0.002(3) 0.000(3) 0.002(3) C8 0.042(4) 0.077(5) 0.046(4) -0.010(4) 0.017(3) -0.006(4) C9 0.051(4) 0.071(5) 0.044(4) -0.004(4) 0.015(3) -0.025(4) C10 0.064(5) 0.072(6) 0.058(5) 0.012(4) 0.012(4) -0.011(4) C11 0.083(7) 0.096(8) 0.104(8) 0.051(7) -0.019(6) -0.025(6) C12 0.155(13) 0.142(13) 0.071(8) 0.047(9) -0.041(9) -0.081(10) C13 0.152(12) 0.156(13) 0.053(7) -0.019(8) 0.021(8) -0.072(10) C14 0.097(7) 0.106(8) 0.045(5) -0.022(5) 0.013(5) -0.027(6) C15 0.036(4) 0.036(4) 0.047(4) -0.006(3) 0.001(3) 0.001(3) C16 0.050(4) 0.049(4) 0.056(5) -0.011(4) -0.014(3) -0.009(3) C17 0.051(4) 0.040(4) 0.049(4) -0.004(3) 0.000(3) -0.008(3) C18 0.036(4) 0.037(4) 0.041(4) -0.006(3) 0.001(3) 0.008(3) C19 0.060(5) 0.049(5) 0.066(5) 0.010(4) 0.022(4) -0.002(4) C20 0.061(5) 0.061(5) 0.046(4) 0.004(4) 0.008(4) -0.002(4) C21 0.046(4) 0.049(4) 0.047(4) -0.007(3) -0.002(3) 0.004(3) C22 0.059(5) 0.064(5) 0.038(4) -0.006(4) 0.014(3) -0.006(4) C23 0.051(4) 0.064(5) 0.042(4) -0.004(4) 0.014(3) -0.002(4) C24 0.081(6) 0.075(6) 0.052(5) -0.007(4) 0.008(4) 0.000(5) C25 0.085(7) 0.129(10) 0.062(6) 0.012(7) -0.005(5) -0.011(7) C26 0.085(8) 0.114(10) 0.096(9) 0.036(7) 0.018(6) 0.012(7) C27 0.109(9) 0.066(7) 0.108(9) 0.000(6) 0.035(7) 0.004(6) C28 0.089(7) 0.062(6) 0.068(6) -0.004(5) 0.017(5) -0.002(5) _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 1.971(6) . ? Pd1 N3 2.056(5) . ? Pd1 Cl1 2.2867(19) . ? Pd1 Cl2 2.3533(18) . ? Pd2 C15 1.980(6) . ? Pd2 N7 2.059(5) . ? Pd2 Cl4 2.290(2) . ? Pd2 Cl3 2.3402(17) . ? N1 C1 1.364(7) . ? N1 C3 1.386(8) . ? N1 C4 1.391(7) . ? N2 C1 1.339(8) . ? N2 C2 1.388(8) . ? N2 C8 1.474(8) . ? N3 C7 1.330(8) . ? N3 C4 1.342(7) . ? N4 C4 1.312(7) . ? N4 C5 1.340(8) . ? N5 C18 1.382(8) . ? N5 C17 1.384(8) . ? N5 C15 1.384(8) . ? N6 C15 1.322(8) . ? N6 C16 1.401(8) . ? N6 C22 1.461(8) . ? N7 C21 1.328(8) . ? N7 C18 1.338(7) . ? N8 C18 1.315(8) . ? N8 C19 1.335(9) . ? C2 C3 1.320(9) . ? C5 C6 1.365(9) . ? C6 C7 1.377(9) . ? C8 C9 1.504(10) . ? C9 C10 1.381(10) . ? C9 C14 1.386(10) . ? C10 C11 1.369(11) . ? C11 C12 1.351(16) . ? C12 C13 1.360(17) . ? C13 C14 1.382(15) . ? C16 C17 1.315(9) . ? C19 C20 1.372(10) . ? C20 C21 1.379(9) . ? C22 C23 1.516(10) . ? C23 C28 1.359(10) . ? C23 C24 1.372(10) . ? C24 C25 1.371(12) . ? C25 C26 1.365(14) . ? C26 C27 1.352(14) . ? C27 C28 1.379(13) . ? 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 N3 79.8(2) . . ? C1 Pd1 Cl1 98.60(19) . . ? N3 Pd1 Cl1 176.88(14) . . ? C1 Pd1 Cl2 172.25(19) . . ? N3 Pd1 Cl2 92.77(14) . . ? Cl1 Pd1 Cl2 88.90(7) . . ? C15 Pd2 N7 80.6(2) . . ? C15 Pd2 Cl4 97.3(2) . . ? N7 Pd2 Cl4 176.48(15) . . ? C15 Pd2 Cl3 172.4(2) . . ? N7 Pd2 Cl3 91.85(14) . . ? Cl4 Pd2 Cl3 90.31(7) . . ? C1 N1 C3 111.7(5) . . ? C1 N1 C4 119.4(5) . . ? C3 N1 C4 128.9(5) . . ? C1 N2 C2 111.3(5) . . ? C1 N2 C8 127.2(6) . . ? C2 N2 C8 121.3(6) . . ? C7 N3 C4 117.5(5) . . ? C7 N3 Pd1 128.0(4) . . ? C4 N3 Pd1 114.5(4) . . ? C4 N4 C5 114.6(6) . . ? C18 N5 C17 128.0(6) . . ? C18 N5 C15 121.0(5) . . ? C17 N5 C15 110.9(5) . . ? C15 N6 C16 109.8(6) . . ? C15 N6 C22 127.5(6) . . ? C16 N6 C22 122.7(6) . . ? C21 N7 C18 116.5(6) . . ? C21 N7 Pd2 129.2(4) . . ? C18 N7 Pd2 114.2(4) . . ? C18 N8 C19 114.2(6) . . ? N2 C1 N1 103.4(5) . . ? N2 C1 Pd1 143.5(5) . . ? N1 C1 Pd1 113.1(4) . . ? C3 C2 N2 107.7(6) . . ? C2 C3 N1 105.9(6) . . ? N4 C4 N3 126.6(6) . . ? N4 C4 N1 120.4(6) . . ? N3 C4 N1 113.0(5) . . ? N4 C5 C6 123.6(6) . . ? C5 C6 C7 117.3(6) . . ? N3 C7 C6 120.2(6) . . ? N2 C8 C9 112.1(5) . . ? C10 C9 C14 119.5(8) . . ? C10 C9 C8 121.5(7) . . ? C14 C9 C8 119.0(8) . . ? C11 C10 C9 119.8(9) . . ? C12 C11 C10 120.0(11) . . ? C11 C12 C13 121.7(12) . . ? C12 C13 C14 119.2(11) . . ? C13 C14 C9 119.7(10) . . ? N6 C15 N5 104.8(5) . . ? N6 C15 Pd2 144.3(5) . . ? N5 C15 Pd2 110.9(4) . . ? C17 C16 N6 109.2(6) . . ? C16 C17 N5 105.4(6) . . ? N8 C18 N7 127.6(6) . . ? N8 C18 N5 119.6(6) . . ? N7 C18 N5 112.7(6) . . ? N8 C19 C20 123.8(7) . . ? C19 C20 C21 116.7(7) . . ? N7 C21 C20 121.1(6) . . ? N6 C22 C23 111.9(6) . . ? C28 C23 C24 117.7(8) . . ? C28 C23 C22 121.1(7) . . ? C24 C23 C22 121.1(7) . . ? C25 C24 C23 122.1(9) . . ? C26 C25 C24 118.9(10) . . ? C27 C26 C25 120.1(11) . . ? C26 C27 C28 120.3(10) . . ? C23 C28 C27 120.9(9) . . ? 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 N3 C7 -176.9(5) . . . . ? Cl1 Pd1 N3 C7 -117(3) . . . . ? Cl2 Pd1 N3 C7 5.5(5) . . . . ? C1 Pd1 N3 C4 2.6(4) . . . . ? Cl1 Pd1 N3 C4 63(3) . . . . ? Cl2 Pd1 N3 C4 -175.0(4) . . . . ? C15 Pd2 N7 C21 -177.4(6) . . . . ? Cl4 Pd2 N7 C21 130(2) . . . . ? Cl3 Pd2 N7 C21 1.8(5) . . . . ? C15 Pd2 N7 C18 7.4(4) . . . . ? Cl4 Pd2 N7 C18 -46(3) . . . . ? Cl3 Pd2 N7 C18 -173.4(4) . . . . ? C2 N2 C1 N1 -1.0(7) . . . . ? C8 N2 C1 N1 -176.0(6) . . . . ? C2 N2 C1 Pd1 179.9(6) . . . . ? C8 N2 C1 Pd1 4.9(11) . . . . ? C3 N1 C1 N2 0.8(6) . . . . ? C4 N1 C1 N2 179.1(5) . . . . ? C3 N1 C1 Pd1 -179.7(4) . . . . ? C4 N1 C1 Pd1 -1.4(7) . . . . ? N3 Pd1 C1 N2 178.5(8) . . . . ? Cl1 Pd1 C1 N2 1.2(8) . . . . ? Cl2 Pd1 C1 N2 -163.8(8) . . . . ? N3 Pd1 C1 N1 -0.6(4) . . . . ? Cl1 Pd1 C1 N1 -177.9(4) . . . . ? Cl2 Pd1 C1 N1 17.0(16) . . . . ? C1 N2 C2 C3 0.8(8) . . . . ? C8 N2 C2 C3 176.1(6) . . . . ? N2 C2 C3 N1 -0.3(7) . . . . ? C1 N1 C3 C2 -0.3(7) . . . . ? C4 N1 C3 C2 -178.5(6) . . . . ? C5 N4 C4 N3 0.7(9) . . . . ? C5 N4 C4 N1 -177.3(5) . . . . ? C7 N3 C4 N4 -2.5(9) . . . . ? Pd1 N3 C4 N4 177.9(5) . . . . ? C7 N3 C4 N1 175.6(5) . . . . ? Pd1 N3 C4 N1 -4.0(6) . . . . ? C1 N1 C4 N4 -178.1(5) . . . . ? C3 N1 C4 N4 -0.1(9) . . . . ? C1 N1 C4 N3 3.6(7) . . . . ? C3 N1 C4 N3 -178.4(5) . . . . ? C4 N4 C5 C6 3.0(9) . . . . ? N4 C5 C6 C7 -4.6(9) . . . . ? C4 N3 C7 C6 0.7(9) . . . . ? Pd1 N3 C7 C6 -179.8(4) . . . . ? C5 C6 C7 N3 2.5(9) . . . . ? C1 N2 C8 C9 112.7(7) . . . . ? C2 N2 C8 C9 -61.8(9) . . . . ? N2 C8 C9 C10 -45.0(9) . . . . ? N2 C8 C9 C14 137.2(7) . . . . ? C14 C9 C10 C11 -1.8(11) . . . . ? C8 C9 C10 C11 -179.6(7) . . . . ? C9 C10 C11 C12 2.0(13) . . . . ? C10 C11 C12 C13 0.0(17) . . . . ? C11 C12 C13 C14 -2.3(19) . . . . ? C12 C13 C14 C9 2.4(17) . . . . ? C10 C9 C14 C13 -0.4(13) . . . . ? C8 C9 C14 C13 177.4(8) . . . . ? C16 N6 C15 N5 -0.8(7) . . . . ? C22 N6 C15 N5 177.8(6) . . . . ? C16 N6 C15 Pd2 -177.7(7) . . . . ? C22 N6 C15 Pd2 1.0(12) . . . . ? C18 N5 C15 N6 -175.0(5) . . . . ? C17 N5 C15 N6 0.6(7) . . . . ? C18 N5 C15 Pd2 3.0(7) . . . . ? C17 N5 C15 Pd2 178.6(4) . . . . ? N7 Pd2 C15 N6 171.4(9) . . . . ? Cl4 Pd2 C15 N6 -11.4(8) . . . . ? Cl3 Pd2 C15 N6 165.2(9) . . . . ? N7 Pd2 C15 N5 -5.3(4) . . . . ? Cl4 Pd2 C15 N5 171.9(4) . . . . ? Cl3 Pd2 C15 N5 -11.6(17) . . . . ? C15 N6 C16 C17 0.8(8) . . . . ? C22 N6 C16 C17 -177.9(6) . . . . ? N6 C16 C17 N5 -0.4(8) . . . . ? C18 N5 C17 C16 175.1(6) . . . . ? C15 N5 C17 C16 -0.1(8) . . . . ? C19 N8 C18 N7 1.4(9) . . . . ? C19 N8 C18 N5 -177.0(6) . . . . ? C21 N7 C18 N8 -1.9(9) . . . . ? Pd2 N7 C18 N8 173.9(5) . . . . ? C21 N7 C18 N5 176.5(5) . . . . ? Pd2 N7 C18 N5 -7.7(6) . . . . ? C17 N5 C18 N8 7.0(10) . . . . ? C15 N5 C18 N8 -178.2(6) . . . . ? C17 N5 C18 N7 -171.6(6) . . . . ? C15 N5 C18 N7 3.2(8) . . . . ? C18 N8 C19 C20 0.3(10) . . . . ? N8 C19 C20 C21 -1.3(11) . . . . ? C18 N7 C21 C20 0.7(9) . . . . ? Pd2 N7 C21 C20 -174.4(5) . . . . ? C19 C20 C21 N7 0.7(10) . . . . ? C15 N6 C22 C23 115.6(7) . . . . ? C16 N6 C22 C23 -66.0(8) . . . . ? N6 C22 C23 C28 -92.1(8) . . . . ? N6 C22 C23 C24 84.3(8) . . . . ? C28 C23 C24 C25 1.6(12) . . . . ? C22 C23 C24 C25 -174.9(7) . . . . ? C23 C24 C25 C26 -2.6(14) . . . . ? C24 C25 C26 C27 1.1(16) . . . . ? C25 C26 C27 C28 1.3(16) . . . . ? C24 C23 C28 C27 0.9(12) . . . . ? C22 C23 C28 C27 177.4(7) . . . . ? C26 C27 C28 C23 -2.4(15) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.702 _refine_diff_density_min -0.995 _refine_diff_density_rms 0.105 #===END