data_nb96 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ; 2(C24 H28 F2 N2 Pd), 0.5(C6 H6), 0.5(C6 H6), 0.5(C6 H6) ; _chemical_formula_sum 'C57 H65 F4 N4 Pd2' _chemical_formula_weight 1094.93 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M Ia loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y, z' 'x+1/2, y+1/2, z+1/2' 'x+1, -y+1/2, z+1/2' _cell_length_a 17.9592(12) _cell_length_b 17.5332(12) _cell_length_c 20.2950(14) _cell_angle_alpha 90.00 _cell_angle_beta 95.1350(10) _cell_angle_gamma 90.00 _cell_volume 6364.9(8) _cell_formula_units_Z 4 _cell_measurement_temperature 85(2) _cell_measurement_reflns_used 9918 _cell_measurement_theta_min 2.51 _cell_measurement_theta_max 24.92 _exptl_crystal_description blade _exptl_crystal_colour yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.143 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2252 _exptl_absorpt_coefficient_mu 0.610 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8625 _exptl_absorpt_correction_T_max 0.9472 _exptl_absorpt_process_details ; Blessing, R. Acta Cryst. (1995) A51 33-38. Sheldrick, G. SADABS (Version 2007/4) Bruker AXS area detector absorption and other corrections, University of Gottingen, Germany 2007. ; _exptl_special_details ; 3365 frames x 60 sec. @ 5.055 cm; 0.5 deg. steps in omega, 0.45 in phi ; _diffrn_ambient_temperature 85(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 70232 _diffrn_reflns_av_R_equivalents 0.0652 _diffrn_reflns_av_sigmaI/netI 0.0445 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.28 _diffrn_reflns_theta_max 25.05 _reflns_number_total 11189 _reflns_number_gt 9308 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART-APEX' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Restraints (SAME/DELU/SIMU) were placed on the three 0.5 occupancy benzene solvate molecules to maintain chemical sensibility. The partial occupancy solvates were assigned different PART numbers and there are no close contacts. There are four solvent accessible voids of approximately 40 A^3 each. They could well contain an additional solvate, say water. However, the final electron density is quite flat and no discrete atoms positions could be determined. The SQUEEZE subroutine of the PLATON program suite was NOT employed. 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^)+(0.1065P)^2^+3.1299P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.01(4) _refine_ls_number_reflns 11189 _refine_ls_number_parameters 682 _refine_ls_number_restraints 218 _refine_ls_R_factor_all 0.0700 _refine_ls_R_factor_gt 0.0552 _refine_ls_wR_factor_ref 0.1651 _refine_ls_wR_factor_gt 0.1553 _refine_ls_goodness_of_fit_ref 1.135 _refine_ls_restrained_S_all 1.130 _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 0.63123(3) 0.85618(4) 0.43251(2) 0.03779(16) Uani 1 1 d . . . Pd2 Pd 0.41278(3) 0.10523(3) 0.17881(2) 0.03691(16) Uani 1 1 d . . . F1 F 0.7409(2) 0.8351(3) 0.44559(19) 0.0454(11) Uani 1 1 d . . . F2 F 0.6265(4) 0.8562(6) 0.7326(3) 0.113(3) Uani 1 1 d . . . F3 F 0.4192(3) -0.0077(2) 0.1803(2) 0.0443(10) Uani 1 1 d . . . F4 F 0.4956(3) 0.0948(3) 0.4782(2) 0.0640(15) Uani 1 1 d . . . N1 N 0.6304(4) 0.8661(4) 0.3300(3) 0.0392(17) Uani 1 1 d . . . N2 N 0.5211(4) 0.8765(4) 0.4081(3) 0.0445(16) Uani 1 1 d . . . N3 N 0.3975(3) 0.2169(4) 0.1633(3) 0.0395(14) Uani 1 1 d . . . N4 N 0.3754(4) 0.1053(4) 0.0792(3) 0.0377(16) Uani 1 1 d . . . C1 C 0.6264(5) 0.8563(5) 0.5297(4) 0.044(2) Uani 1 1 d D . . C2 C 0.5997(5) 0.9189(7) 0.5634(4) 0.065(3) Uani 1 1 d D . . H2A H 0.5813 0.9628 0.5398 0.078 Uiso 1 1 calc R . . C3 C 0.6004(6) 0.9156(9) 0.6316(5) 0.091(5) Uani 1 1 d D . . H3A H 0.5807 0.9574 0.6542 0.109 Uiso 1 1 calc R . . C4 C 0.6269(6) 0.8578(8) 0.6656(4) 0.076(4) Uani 1 1 d D . . C5 C 0.6546(6) 0.7960(7) 0.6360(4) 0.074(3) Uani 1 1 d D . . H5A H 0.6725 0.7534 0.6616 0.089 Uiso 1 1 calc R . . C6 C 0.6565(5) 0.7956(6) 0.5679(4) 0.050(2) Uani 1 1 d D . . H6A H 0.6785 0.7538 0.5470 0.060 Uiso 1 1 calc R . . C7 C 0.6885(5) 0.8627(5) 0.2962(4) 0.0432(19) Uani 1 1 d . . . H7A H 0.7341 0.8439 0.3175 0.052 Uiso 1 1 calc R . . C8 C 0.6873(5) 0.8855(6) 0.2294(4) 0.049(2) Uani 1 1 d . . . H8A H 0.7311 0.8832 0.2065 0.059 Uiso 1 1 calc R . . C9 C 0.6204(5) 0.9114(5) 0.1983(4) 0.045(2) Uani 1 1 d . . . C10 C 0.5584(4) 0.9137(5) 0.2344(3) 0.0421(19) Uani 1 1 d . . . H10A H 0.5118 0.9315 0.2145 0.050 Uiso 1 1 calc R . . C11 C 0.5649(4) 0.8901(5) 0.2989(4) 0.0403(17) Uani 1 1 d . . . C12 C 0.5021(4) 0.8905(5) 0.3422(3) 0.0392(17) Uani 1 1 d . . . C13 C 0.4281(4) 0.9019(4) 0.3199(3) 0.0387(17) Uani 1 1 d . . . H13A H 0.4156 0.9131 0.2744 0.046 Uiso 1 1 calc R . . C14 C 0.3709(4) 0.8975(5) 0.3620(4) 0.0430(18) Uani 1 1 d . . . C15 C 0.3930(5) 0.8839(5) 0.4275(4) 0.047(2) Uani 1 1 d . . . H15A H 0.3564 0.8818 0.4584 0.057 Uiso 1 1 calc R . . C16 C 0.4661(5) 0.8735(6) 0.4489(4) 0.051(2) Uani 1 1 d . . . H16A H 0.4789 0.8638 0.4946 0.061 Uiso 1 1 calc R . . C17 C 0.6149(4) 0.9416(6) 0.1271(4) 0.051(2) Uani 1 1 d . . . C18 C 0.5954(5) 1.0279(6) 0.1282(4) 0.060(2) Uani 1 1 d . . . H18A H 0.6353 1.0554 0.1543 0.089 Uiso 1 1 calc R . . H18B H 0.5481 1.0349 0.1480 0.089 Uiso 1 1 calc R . . H18C H 0.5905 1.0477 0.0829 0.089 Uiso 1 1 calc R . . C19 C 0.5511(5) 0.8970(7) 0.0861(4) 0.064(3) Uani 1 1 d . . . H19A H 0.5465 0.9157 0.0404 0.096 Uiso 1 1 calc R . . H19B H 0.5038 0.9049 0.1057 0.096 Uiso 1 1 calc R . . H19C H 0.5632 0.8425 0.0865 0.096 Uiso 1 1 calc R . . C20 C 0.6875(5) 0.9311(7) 0.0952(4) 0.064(3) Uani 1 1 d . . . H20A H 0.7276 0.9593 0.1205 0.096 Uiso 1 1 calc R . . H20B H 0.6815 0.9505 0.0497 0.096 Uiso 1 1 calc R . . H20C H 0.7003 0.8768 0.0946 0.096 Uiso 1 1 calc R . . C21 C 0.2879(4) 0.9089(5) 0.3382(4) 0.047(2) Uani 1 1 d . . . C22 C 0.2792(5) 0.9346(7) 0.2653(5) 0.064(3) Uani 1 1 d . . . H22A H 0.3050 0.9834 0.2610 0.095 Uiso 1 1 calc R . . H22B H 0.2260 0.9408 0.2507 0.095 Uiso 1 1 calc R . . H22C H 0.3011 0.8961 0.2378 0.095 Uiso 1 1 calc R . . C23 C 0.2546(5) 0.9718(5) 0.3781(4) 0.0493(19) Uani 1 1 d . . . H23A H 0.2806 1.0199 0.3712 0.074 Uiso 1 1 calc R . . H23B H 0.2605 0.9584 0.4252 0.074 Uiso 1 1 calc R . . H23C H 0.2014 0.9775 0.3637 0.074 Uiso 1 1 calc R . . C24 C 0.2489(5) 0.8354(7) 0.3479(6) 0.070(3) Uani 1 1 d . . . H24A H 0.2560 0.8208 0.3947 0.105 Uiso 1 1 calc R . . H24B H 0.2697 0.7958 0.3209 0.105 Uiso 1 1 calc R . . H24C H 0.1954 0.8413 0.3346 0.105 Uiso 1 1 calc R . . C25 C 0.4448(5) 0.1101(4) 0.2748(4) 0.037(2) Uani 1 1 d . . . C26 C 0.3955(5) 0.1347(5) 0.3205(4) 0.048(2) Uani 1 1 d . . . H26A H 0.3489 0.1557 0.3036 0.057 Uiso 1 1 calc R . . C27 C 0.4102(5) 0.1302(6) 0.3882(4) 0.050(2) Uani 1 1 d . . . H27A H 0.3744 0.1454 0.4173 0.060 Uiso 1 1 calc R . . C28 C 0.4797(5) 0.1026(5) 0.4116(4) 0.048(2) Uani 1 1 d . . . C29 C 0.5317(5) 0.0813(6) 0.3700(4) 0.053(2) Uani 1 1 d . . . H29A H 0.5795 0.0640 0.3879 0.064 Uiso 1 1 calc R . . C30 C 0.5153(4) 0.0848(5) 0.3004(4) 0.046(2) Uani 1 1 d . . . H30A H 0.5517 0.0701 0.2716 0.055 Uiso 1 1 calc R . . C31 C 0.4150(4) 0.2724(5) 0.2083(3) 0.0417(18) Uani 1 1 d . . . H31A H 0.4372 0.2590 0.2510 0.050 Uiso 1 1 calc R . . C32 C 0.4010(5) 0.3488(5) 0.1932(4) 0.0447(19) Uani 1 1 d . . . H32A H 0.4143 0.3865 0.2257 0.054 Uiso 1 1 calc R . . C33 C 0.3680(4) 0.3712(5) 0.1314(4) 0.0406(17) Uani 1 1 d . . . C34 C 0.3498(4) 0.3127(5) 0.0867(3) 0.0387(17) Uani 1 1 d . . . H34A H 0.3263 0.3249 0.0441 0.046 Uiso 1 1 calc R . . C35 C 0.3648(4) 0.2377(5) 0.1023(3) 0.0363(16) Uani 1 1 d . . . C36 C 0.3507(4) 0.1720(5) 0.0559(4) 0.0411(18) Uani 1 1 d . . . C37 C 0.3133(4) 0.1810(5) -0.0070(3) 0.0387(17) Uani 1 1 d . . . H37A H 0.2952 0.2294 -0.0220 0.046 Uiso 1 1 calc R . . C38 C 0.3032(4) 0.1161(5) -0.0471(4) 0.0436(19) Uani 1 1 d . . . C39 C 0.3304(4) 0.0468(5) -0.0224(4) 0.0457(19) Uani 1 1 d . . . H39A H 0.3249 0.0021 -0.0489 0.055 Uiso 1 1 calc R . . C40 C 0.3661(5) 0.0429(5) 0.0421(4) 0.0453(19) Uani 1 1 d . . . H40A H 0.3837 -0.0049 0.0593 0.054 Uiso 1 1 calc R . . C41 C 0.3534(5) 0.4551(5) 0.1172(4) 0.0471(19) Uani 1 1 d . . . C42 C 0.4297(6) 0.4959(6) 0.1197(5) 0.063(2) Uani 1 1 d . . . H42A H 0.4562 0.4895 0.1638 0.095 Uiso 1 1 calc R . . H42B H 0.4219 0.5504 0.1107 0.095 Uiso 1 1 calc R . . H42C H 0.4596 0.4738 0.0864 0.095 Uiso 1 1 calc R . . C43 C 0.3048(6) 0.4886(6) 0.1681(4) 0.068(3) Uani 1 1 d . . . H43A H 0.3294 0.4809 0.2127 0.101 Uiso 1 1 calc R . . H43B H 0.2561 0.4630 0.1644 0.101 Uiso 1 1 calc R . . H43C H 0.2978 0.5433 0.1599 0.101 Uiso 1 1 calc R . . C44 C 0.3151(6) 0.4682(6) 0.0459(4) 0.068(3) Uani 1 1 d . . . H44A H 0.3064 0.5229 0.0387 0.102 Uiso 1 1 calc R . . H44B H 0.2672 0.4411 0.0410 0.102 Uiso 1 1 calc R . . H44C H 0.3476 0.4489 0.0134 0.102 Uiso 1 1 calc R . . C45 C 0.2570(5) 0.1226(5) -0.1156(4) 0.0459(19) Uani 1 1 d . . . C46 C 0.1775(5) 0.1467(6) -0.1026(4) 0.055(2) Uani 1 1 d . . . H46A H 0.1554 0.1078 -0.0757 0.082 Uiso 1 1 calc R . . H46B H 0.1470 0.1522 -0.1448 0.082 Uiso 1 1 calc R . . H46C H 0.1793 0.1955 -0.0790 0.082 Uiso 1 1 calc R . . C47 C 0.2935(6) 0.1824(6) -0.1562(4) 0.060(2) Uani 1 1 d . . . H47A H 0.3442 0.1660 -0.1636 0.090 Uiso 1 1 calc R . . H47B H 0.2958 0.2311 -0.1324 0.090 Uiso 1 1 calc R . . H47C H 0.2641 0.1888 -0.1989 0.090 Uiso 1 1 calc R . . C48 C 0.2515(6) 0.0472(6) -0.1525(4) 0.065(3) Uani 1 1 d . . . H48A H 0.3017 0.0302 -0.1611 0.098 Uiso 1 1 calc R . . H48B H 0.2209 0.0538 -0.1946 0.098 Uiso 1 1 calc R . . H48C H 0.2285 0.0089 -0.1256 0.098 Uiso 1 1 calc R . . C49 C 0.4728(11) 0.8164(12) 0.9045(10) 0.084(4) Uani 0.50 1 d PDU A 1 H49A H 0.5164 0.8074 0.9336 0.101 Uiso 0.50 1 calc PR A 1 C50 C 0.4771(12) 0.8142(13) 0.8376(11) 0.088(4) Uani 0.50 1 d PDU A 1 H50A H 0.5225 0.7998 0.8203 0.105 Uiso 0.50 1 calc PR A 1 C51 C 0.4162(13) 0.8327(13) 0.7960(11) 0.093(4) Uani 0.50 1 d PDU A 1 H51A H 0.4196 0.8308 0.7495 0.112 Uiso 0.50 1 calc PR A 1 C52 C 0.3527(12) 0.8531(11) 0.8185(11) 0.085(4) Uani 0.50 1 d PDU A 1 H52A H 0.3116 0.8695 0.7892 0.102 Uiso 0.50 1 calc PR A 1 C53 C 0.3475(11) 0.8502(11) 0.8838(11) 0.081(4) Uani 0.50 1 d PDU A 1 H53A H 0.3005 0.8616 0.8994 0.097 Uiso 0.50 1 calc PR A 1 C54 C 0.4057(10) 0.8316(9) 0.9299(8) 0.081(4) Uani 0.50 1 d PDU A 1 H54A H 0.4000 0.8295 0.9760 0.098 Uiso 0.50 1 calc PR A 1 C55 C 0.1433(10) 0.6288(9) 0.1932(8) 0.108(5) Uani 0.50 1 d PRDU A 3 H55A H 0.1664 0.5848 0.2133 0.129 Uiso 0.50 1 calc PR A 3 C56 C 0.1371(15) 0.6965(12) 0.2264(12) 0.108(5) Uani 0.50 1 d PDU A 3 H56A H 0.1523 0.6997 0.2724 0.130 Uiso 0.50 1 calc PR A 3 C57 C 0.1085(13) 0.7600(12) 0.1926(12) 0.099(5) Uani 0.50 1 d PDU A 3 H57A H 0.1115 0.8069 0.2161 0.118 Uiso 0.50 1 calc PR A 3 C58 C 0.0782(10) 0.7625(11) 0.1324(11) 0.085(4) Uani 0.50 1 d PDU A 3 H58A H 0.0577 0.8077 0.1123 0.102 Uiso 0.50 1 calc PR A 3 C59 C 0.0785(11) 0.6955(11) 0.1013(10) 0.089(4) Uani 0.50 1 d PDU A 3 H59A H 0.0534 0.6923 0.0582 0.107 Uiso 0.50 1 calc PR A 3 C60 C 0.1129(14) 0.6302(12) 0.1277(10) 0.098(5) Uani 0.50 1 d PDU A 3 H60A H 0.1158 0.5860 0.1009 0.117 Uiso 0.50 1 calc PR A 3 C61 C 0.0069(18) 0.625(2) 0.4123(18) 0.174(9) Uani 0.50 1 d PDU B 2 H61A H -0.0207 0.6361 0.4489 0.209 Uiso 0.50 1 calc PR B 2 C62 C 0.0381(17) 0.6820(17) 0.3781(19) 0.169(9) Uani 0.50 1 d PDU B 2 H62A H 0.0358 0.7338 0.3916 0.203 Uiso 0.50 1 calc PR B 2 C63 C 0.0726(18) 0.6610(19) 0.3236(18) 0.166(9) Uani 0.50 1 d PDU B 2 H63A H 0.0879 0.7005 0.2956 0.200 Uiso 0.50 1 calc PR B 2 C64 C 0.0863(16) 0.591(2) 0.3070(17) 0.167(9) Uani 0.50 1 d PDU B 2 H64A H 0.1234 0.5789 0.2780 0.200 Uiso 0.50 1 calc PR B 2 C65 C 0.0455(17) 0.5356(17) 0.3328(19) 0.168(9) Uani 0.50 1 d PDU B 2 H65A H 0.0370 0.4882 0.3106 0.202 Uiso 0.50 1 calc PR B 2 C66 C 0.0161(18) 0.5499(19) 0.3928(19) 0.173(9) Uani 0.50 1 d PDU B 2 H66A H 0.0026 0.5089 0.4200 0.208 Uiso 0.50 1 calc PR B 2 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 0.0266(3) 0.0601(4) 0.0254(3) 0.0030(3) -0.00497(19) 0.0023(3) Pd2 0.0273(3) 0.0563(4) 0.0259(3) 0.0004(3) -0.00432(19) 0.0049(3) F1 0.031(2) 0.076(3) 0.028(2) 0.007(2) -0.0056(17) 0.005(2) F2 0.084(5) 0.222(10) 0.030(3) -0.009(4) -0.014(3) 0.031(5) F3 0.042(2) 0.058(3) 0.0306(18) 0.003(2) -0.0075(16) 0.007(2) F4 0.066(3) 0.097(4) 0.026(2) -0.002(2) -0.011(2) 0.006(3) N1 0.030(4) 0.058(4) 0.028(3) -0.005(3) -0.007(3) 0.002(3) N2 0.031(3) 0.073(5) 0.029(3) 0.008(3) -0.002(3) -0.001(3) N3 0.033(3) 0.059(4) 0.025(3) 0.005(3) -0.004(2) 0.002(3) N4 0.030(4) 0.053(4) 0.029(3) 0.000(3) 0.000(3) 0.001(3) C1 0.027(4) 0.065(5) 0.041(4) -0.001(4) 0.003(4) -0.001(4) C2 0.040(5) 0.116(9) 0.036(4) -0.005(5) -0.009(4) 0.014(5) C3 0.048(6) 0.180(14) 0.041(5) -0.033(7) -0.012(4) 0.039(7) C4 0.045(5) 0.153(11) 0.030(4) -0.002(6) -0.001(4) 0.023(6) C5 0.060(6) 0.118(9) 0.040(5) 0.011(5) -0.018(4) 0.008(6) C6 0.038(4) 0.080(6) 0.032(4) 0.015(4) 0.001(3) 0.007(4) C7 0.030(4) 0.068(5) 0.031(4) 0.007(4) 0.001(3) 0.002(4) C8 0.038(5) 0.077(6) 0.032(4) -0.004(4) 0.004(3) 0.007(4) C9 0.036(4) 0.063(5) 0.033(4) -0.007(4) -0.009(3) 0.010(4) C10 0.029(4) 0.071(6) 0.025(4) -0.006(3) -0.001(3) 0.001(3) C11 0.028(4) 0.059(5) 0.032(4) -0.006(3) -0.010(3) 0.010(3) C12 0.027(4) 0.062(5) 0.027(3) -0.010(3) -0.006(3) 0.000(3) C13 0.028(4) 0.057(5) 0.030(4) -0.001(3) -0.004(3) 0.001(3) C14 0.027(4) 0.065(5) 0.035(4) -0.004(4) -0.005(3) -0.004(4) C15 0.033(4) 0.073(6) 0.036(4) 0.006(4) 0.005(3) -0.001(4) C16 0.033(4) 0.090(7) 0.029(4) 0.006(4) 0.003(3) 0.004(4) C17 0.033(4) 0.095(7) 0.024(3) 0.001(4) -0.001(3) 0.011(4) C18 0.055(5) 0.095(7) 0.028(4) 0.010(4) 0.005(4) 0.007(5) C19 0.044(5) 0.114(9) 0.032(4) -0.007(5) -0.005(4) 0.012(5) C20 0.052(5) 0.117(8) 0.023(4) 0.000(4) 0.000(3) 0.015(5) C21 0.025(4) 0.072(6) 0.044(4) -0.007(4) -0.005(3) -0.002(4) C22 0.029(5) 0.104(9) 0.054(6) -0.008(5) -0.012(4) 0.007(5) C23 0.035(4) 0.061(5) 0.052(5) -0.003(4) 0.004(3) -0.004(4) C24 0.033(5) 0.083(7) 0.091(8) 0.002(6) -0.012(5) -0.003(5) C25 0.032(5) 0.043(5) 0.035(4) 0.000(3) 0.001(4) -0.003(3) C26 0.027(4) 0.076(6) 0.040(4) 0.007(4) -0.001(3) 0.010(4) C27 0.033(4) 0.079(6) 0.037(4) -0.002(4) 0.006(4) -0.005(4) C28 0.050(5) 0.069(6) 0.025(4) -0.002(4) -0.003(3) 0.003(4) C29 0.032(4) 0.088(7) 0.038(4) -0.004(4) -0.010(3) 0.006(4) C30 0.027(4) 0.076(6) 0.033(4) -0.011(4) -0.001(3) 0.004(4) C31 0.038(4) 0.060(5) 0.026(3) -0.002(3) -0.004(3) -0.006(4) C32 0.036(4) 0.067(6) 0.031(4) -0.004(3) 0.005(3) 0.001(4) C33 0.031(4) 0.059(5) 0.031(4) 0.002(3) -0.002(3) 0.001(3) C34 0.030(4) 0.060(5) 0.024(3) 0.000(3) -0.005(3) -0.002(3) C35 0.024(3) 0.060(5) 0.025(3) 0.003(3) 0.001(3) 0.001(3) C36 0.032(4) 0.059(5) 0.032(4) -0.004(4) 0.000(3) -0.010(4) C37 0.033(4) 0.056(5) 0.027(3) 0.003(3) -0.001(3) -0.007(3) C38 0.033(4) 0.073(6) 0.025(4) -0.004(3) 0.003(3) -0.008(4) C39 0.041(4) 0.064(5) 0.031(4) -0.005(4) -0.006(3) -0.003(4) C40 0.044(5) 0.060(5) 0.031(4) -0.002(4) 0.002(3) 0.005(4) C41 0.043(4) 0.063(5) 0.033(4) 0.007(4) -0.005(3) -0.002(4) C42 0.066(6) 0.065(6) 0.058(5) -0.003(4) -0.003(4) -0.020(5) C43 0.077(7) 0.076(7) 0.049(5) 0.005(5) -0.001(5) 0.002(6) C44 0.074(7) 0.079(7) 0.047(5) 0.009(5) -0.015(5) -0.010(5) C45 0.047(5) 0.064(5) 0.027(4) 0.002(3) 0.005(3) -0.003(4) C46 0.044(5) 0.084(7) 0.033(4) 0.003(4) -0.015(4) -0.006(4) C47 0.073(7) 0.079(6) 0.028(4) 0.003(4) -0.001(4) 0.001(5) C48 0.072(6) 0.091(7) 0.029(4) -0.006(4) -0.013(4) -0.004(5) C49 0.082(8) 0.053(7) 0.113(10) 0.004(8) -0.005(8) -0.009(7) C50 0.086(8) 0.060(8) 0.116(10) 0.008(8) -0.001(8) -0.013(7) C51 0.098(9) 0.059(8) 0.119(10) 0.011(8) -0.011(8) -0.016(8) C52 0.088(9) 0.040(7) 0.122(10) 0.012(8) -0.020(9) -0.015(7) C53 0.082(8) 0.032(7) 0.125(10) 0.010(8) -0.009(8) -0.018(7) C54 0.085(9) 0.041(7) 0.116(10) 0.009(8) -0.004(8) -0.004(7) C55 0.076(9) 0.103(9) 0.145(12) -0.040(9) 0.007(9) -0.025(8) C56 0.077(9) 0.107(10) 0.139(11) -0.045(9) 0.007(9) -0.025(9) C57 0.067(9) 0.098(9) 0.133(11) -0.045(9) 0.026(8) -0.025(8) C58 0.042(7) 0.095(8) 0.125(11) -0.033(9) 0.040(7) -0.036(7) C59 0.056(8) 0.100(9) 0.117(11) -0.032(8) 0.034(8) -0.036(7) C60 0.073(9) 0.097(9) 0.128(11) -0.042(9) 0.030(8) -0.028(8) C61 0.066(11) 0.194(19) 0.26(2) 0.089(18) -0.003(12) 0.034(12) C62 0.058(11) 0.189(18) 0.25(2) 0.088(18) -0.020(12) 0.031(11) C63 0.063(12) 0.188(18) 0.24(2) 0.093(18) -0.023(11) 0.027(12) C64 0.066(11) 0.189(19) 0.24(2) 0.098(18) -0.019(11) 0.030(11) C65 0.071(12) 0.186(18) 0.24(2) 0.104(18) -0.009(12) 0.037(11) C66 0.073(12) 0.189(18) 0.26(2) 0.094(19) 0.003(12) 0.035(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 1.981(8) . ? Pd1 F1 1.999(4) . ? Pd1 N2 2.026(6) . ? Pd1 N1 2.086(7) . ? Pd2 C25 1.983(9) . ? Pd2 F3 1.983(4) . ? Pd2 N3 1.998(7) . ? Pd2 N4 2.073(7) . ? F2 C4 1.360(11) . ? F4 C28 1.363(9) . ? N1 C7 1.300(11) . ? N1 C11 1.351(10) . ? N2 C16 1.347(10) . ? N2 C12 1.372(9) . ? N3 C31 1.353(10) . ? N3 C35 1.370(9) . ? N4 C36 1.323(11) . ? N4 C40 1.331(11) . ? C1 C6 1.397(11) . ? C1 C2 1.400(13) . ? C2 C3 1.384(12) . ? C3 C4 1.294(15) . ? C4 C5 1.354(14) . ? C5 C6 1.386(11) . ? C7 C8 1.412(11) . ? C8 C9 1.382(12) . ? C9 C10 1.388(11) . ? C9 C17 1.534(11) . ? C10 C11 1.367(11) . ? C11 C12 1.492(11) . ? C12 C13 1.380(10) . ? C13 C14 1.396(11) . ? C14 C15 1.372(11) . ? C14 C21 1.540(10) . ? C15 C16 1.358(12) . ? C17 C20 1.519(12) . ? C17 C18 1.553(14) . ? C17 C19 1.563(13) . ? C21 C24 1.487(14) . ? C21 C23 1.521(12) . ? C21 C22 1.541(12) . ? C25 C30 1.397(12) . ? C25 C26 1.407(12) . ? C26 C27 1.377(12) . ? C27 C28 1.381(12) . ? C28 C29 1.367(12) . ? C29 C30 1.418(11) . ? C31 C32 1.392(12) . ? C32 C33 1.395(11) . ? C33 C34 1.389(11) . ? C33 C41 1.518(12) . ? C34 C35 1.374(11) . ? C35 C36 1.497(11) . ? C36 C37 1.397(10) . ? C37 C38 1.401(12) . ? C38 C39 1.388(12) . ? C38 C45 1.558(11) . ? C39 C40 1.407(11) . ? C41 C43 1.528(13) . ? C41 C42 1.542(12) . ? C41 C44 1.562(11) . ? C45 C47 1.518(13) . ? C45 C48 1.519(13) . ? C45 C46 1.534(13) . ? C49 C50 1.366(18) . ? C49 C54 1.379(18) . ? C50 C51 1.360(19) . ? C51 C52 1.32(2) . ? C52 C53 1.338(19) . ? C53 C54 1.378(18) . ? C55 C56 1.375(18) . ? C55 C60 1.392(18) . ? C56 C57 1.382(19) . ? C57 C58 1.293(19) . ? C58 C59 1.334(18) . ? C59 C60 1.387(18) . ? C61 C62 1.37(2) . ? C61 C66 1.384(19) . ? C62 C63 1.37(2) . ? C63 C64 1.31(2) . ? C64 C65 1.35(2) . ? C65 C66 1.393(19) . ? 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 F1 89.9(3) . . ? C1 Pd1 N2 96.6(3) . . ? F1 Pd1 N2 173.5(2) . . ? C1 Pd1 N1 174.3(3) . . ? F1 Pd1 N1 93.8(2) . . ? N2 Pd1 N1 79.7(3) . . ? C25 Pd2 F3 90.9(3) . . ? C25 Pd2 N3 97.9(3) . . ? F3 Pd2 N3 171.0(2) . . ? C25 Pd2 N4 176.8(3) . . ? F3 Pd2 N4 91.6(2) . . ? N3 Pd2 N4 79.5(2) . . ? C7 N1 C11 118.2(7) . . ? C7 N1 Pd1 126.0(6) . . ? C11 N1 Pd1 114.8(5) . . ? C16 N2 C12 118.3(6) . . ? C16 N2 Pd1 126.6(5) . . ? C12 N2 Pd1 115.0(5) . . ? C31 N3 C35 118.2(7) . . ? C31 N3 Pd2 125.3(5) . . ? C35 N3 Pd2 116.4(5) . . ? C36 N4 C40 120.2(7) . . ? C36 N4 Pd2 114.7(5) . . ? C40 N4 Pd2 124.4(6) . . ? C6 C1 C2 117.3(8) . . ? C6 C1 Pd1 120.2(6) . . ? C2 C1 Pd1 122.3(7) . . ? C3 C2 C1 118.9(10) . . ? C4 C3 C2 122.4(10) . . ? C3 C4 C5 121.4(9) . . ? C3 C4 F2 121.0(10) . . ? C5 C4 F2 117.6(10) . . ? C4 C5 C6 119.3(9) . . ? C5 C6 C1 120.5(9) . . ? N1 C7 C8 123.4(8) . . ? C9 C8 C7 118.0(8) . . ? C8 C9 C10 118.3(7) . . ? C8 C9 C17 121.6(8) . . ? C10 C9 C17 120.0(7) . . ? C11 C10 C9 119.5(7) . . ? N1 C11 C10 122.5(7) . . ? N1 C11 C12 113.5(7) . . ? C10 C11 C12 123.9(7) . . ? N2 C12 C13 119.7(6) . . ? N2 C12 C11 115.9(6) . . ? C13 C12 C11 124.4(6) . . ? C12 C13 C14 122.0(7) . . ? C15 C14 C13 116.0(7) . . ? C15 C14 C21 121.0(7) . . ? C13 C14 C21 123.0(7) . . ? C16 C15 C14 121.4(7) . . ? N2 C16 C15 122.6(7) . . ? C20 C17 C9 112.0(7) . . ? C20 C17 C18 109.1(8) . . ? C9 C17 C18 108.6(6) . . ? C20 C17 C19 109.2(7) . . ? C9 C17 C19 108.1(8) . . ? C18 C17 C19 109.9(7) . . ? C24 C21 C23 110.2(8) . . ? C24 C21 C14 107.4(7) . . ? C23 C21 C14 110.0(6) . . ? C24 C21 C22 111.8(8) . . ? C23 C21 C22 106.8(8) . . ? C14 C21 C22 110.6(7) . . ? C30 C25 C26 117.1(8) . . ? C30 C25 Pd2 121.7(6) . . ? C26 C25 Pd2 121.1(6) . . ? C27 C26 C25 124.4(8) . . ? C26 C27 C28 116.7(8) . . ? F4 C28 C29 119.4(8) . . ? F4 C28 C27 118.6(7) . . ? C29 C28 C27 122.0(7) . . ? C28 C29 C30 120.7(7) . . ? C25 C30 C29 119.0(7) . . ? N3 C31 C32 121.1(7) . . ? C31 C32 C33 121.5(8) . . ? C34 C33 C32 115.9(7) . . ? C34 C33 C41 124.4(7) . . ? C32 C33 C41 119.7(7) . . ? C35 C34 C33 121.7(7) . . ? N3 C35 C34 121.6(7) . . ? N3 C35 C36 113.5(7) . . ? C34 C35 C36 124.9(6) . . ? N4 C36 C37 123.0(8) . . ? N4 C36 C35 115.0(6) . . ? C37 C36 C35 122.0(8) . . ? C36 C37 C38 117.8(8) . . ? C39 C38 C37 118.6(7) . . ? C39 C38 C45 121.9(7) . . ? C37 C38 C45 119.3(8) . . ? C38 C39 C40 119.7(8) . . ? N4 C40 C39 120.7(8) . . ? C33 C41 C43 110.1(7) . . ? C33 C41 C42 107.8(7) . . ? C43 C41 C42 111.1(8) . . ? C33 C41 C44 111.8(7) . . ? C43 C41 C44 109.8(8) . . ? C42 C41 C44 106.2(7) . . ? C47 C45 C48 110.2(7) . . ? C47 C45 C46 111.0(8) . . ? C48 C45 C46 107.8(8) . . ? C47 C45 C38 108.2(7) . . ? C48 C45 C38 112.4(7) . . ? C46 C45 C38 107.3(6) . . ? C50 C49 C54 120.4(17) . . ? C51 C50 C49 119.8(19) . . ? C52 C51 C50 121.5(19) . . ? C51 C52 C53 118.2(19) . . ? C52 C53 C54 124.5(18) . . ? C53 C54 C49 115.2(16) . . ? C56 C55 C60 114.2(15) . . ? C55 C56 C57 119.7(18) . . ? C58 C57 C56 127.1(19) . . ? C57 C58 C59 113.4(18) . . ? C58 C59 C60 124.5(19) . . ? C59 C60 C55 120.5(17) . . ? C62 C61 C66 119(2) . . ? C63 C62 C61 117(2) . . ? C64 C63 C62 125(2) . . ? C63 C64 C65 117(2) . . ? C64 C65 C66 118(2) . . ? C61 C66 C65 119(2) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.805 _refine_diff_density_min -0.469 _refine_diff_density_rms 0.139