data_nb153 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C18 H24 F2 N2 Pd, C H2 Cl2' _chemical_formula_sum 'C19 H26 Cl2 F2 N2 Pd' _chemical_formula_weight 497.72 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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pccn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-x, y+1/2, -z+1/2' 'x+1/2, -y, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'x, -y-1/2, z-1/2' '-x-1/2, y, z-1/2' _cell_length_a 11.1616(9) _cell_length_b 11.9919(9) _cell_length_c 15.6096(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2089.3(3) _cell_formula_units_Z 4 _cell_measurement_temperature 85(2) _cell_measurement_reflns_used 9448 _cell_measurement_theta_min 2.49 _cell_measurement_theta_max 23.31 _exptl_crystal_description cube _exptl_crystal_colour yellow _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.582 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1008 _exptl_absorpt_coefficient_mu 1.166 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8923 _exptl_absorpt_correction_T_max 0.8923 _exptl_absorpt_process_details ; Blessing, R. Acta Cryst. (1995) A51 33-38. Sheldrick, G. TWINABS (Version 2008/1), Bruker AXS scaling and corrections for twinned crystals University of Gottingen, Germany 2007. ; _exptl_special_details ; 3100 frames x 25 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 92957 _diffrn_reflns_av_R_equivalents 0.0631 _diffrn_reflns_av_sigmaI/netI 0.0303 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.49 _diffrn_reflns_theta_max 28.33 _reflns_number_total 6735 _reflns_number_gt 3768 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART-APEX' _computing_cell_refinement 'Bruker CELL_NOW' _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 ; The crystal was found to be a two-component, non-merohedral twin. The two domains are related by a 180 degree rotation about the reciprocal (1 1 0) axis. The twin scale factor refined to a value of 0.4886(7). Reflections from both domains as well as overlaps were used for refinement as part of a HKLF 5 format file. The complaex lies on a two-fold axis (Wyckoff site c) in the crystal lattice. There is a dichloromethane lattice solvent molecule disordered about an alternative two-fold axis (Wyckoff site d). 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^)+(0.0424P)^2^+4.6230P] 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 6735 _refine_ls_number_parameters 128 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0507 _refine_ls_R_factor_gt 0.0386 _refine_ls_wR_factor_ref 0.1102 _refine_ls_wR_factor_gt 0.1032 _refine_ls_goodness_of_fit_ref 1.095 _refine_ls_restrained_S_all 1.095 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.7500 0.2500 0.516601(11) 0.01293(5) Uani 1 2 d S . . N1 N 0.66966(15) 0.17367(14) 0.42055(9) 0.0141(3) Uani 1 1 d . . . C2 C 0.64846(18) 0.16389(19) 0.26874(12) 0.0175(4) Uani 1 1 d . . . H2A H 0.6730 0.1883 0.2136 0.021 Uiso 1 1 calc R . . C3 C 0.55786(19) 0.08491(19) 0.27670(12) 0.0186(4) Uani 1 1 d . . . C4 C 0.52718(19) 0.05044(18) 0.35938(13) 0.0201(4) Uani 1 1 d . . . H4A H 0.4671 -0.0047 0.3673 0.024 Uiso 1 1 calc R . . C5 C 0.58386(18) 0.09628(18) 0.42928(12) 0.0173(4) Uani 1 1 d . . . H5A H 0.5616 0.0725 0.4851 0.021 Uiso 1 1 calc R . . C1 C 0.70280(17) 0.20679(17) 0.34131(11) 0.0135(3) Uani 1 1 d . . . C6 C 0.4902(2) 0.0369(2) 0.20030(14) 0.0268(5) Uani 1 1 d . . . C9 C 0.3565(2) 0.0639(3) 0.21120(16) 0.0391(7) Uani 1 1 d . . . H9A H 0.3454 0.1450 0.2115 0.059 Uiso 1 1 calc R . . H9B H 0.3277 0.0327 0.2654 0.059 Uiso 1 1 calc R . . H9C H 0.3112 0.0314 0.1636 0.059 Uiso 1 1 calc R . . C7 C 0.5342(2) 0.0865(2) 0.11584(14) 0.0342(6) Uani 1 1 d . . . H7A H 0.5223 0.1675 0.1165 0.051 Uiso 1 1 calc R . . H7B H 0.4889 0.0539 0.0682 0.051 Uiso 1 1 calc R . . H7C H 0.6196 0.0700 0.1086 0.051 Uiso 1 1 calc R . . C8 C 0.5086(3) -0.0898(2) 0.19925(16) 0.0373(6) Uani 1 1 d . . . H8A H 0.5940 -0.1064 0.1923 0.056 Uiso 1 1 calc R . . H8B H 0.4636 -0.1223 0.1515 0.056 Uiso 1 1 calc R . . H8C H 0.4800 -0.1216 0.2533 0.056 Uiso 1 1 calc R . . Cl1 Cl 0.25681(8) 0.12699(9) 0.47118(6) 0.0572(2) Uani 1 1 d . . . C10 C 0.3114(6) 0.2514(3) 0.5133(4) 0.062(2) Uani 0.50 1 d . . -1 H10A H 0.3986 0.2553 0.5024 0.074 Uiso 0.50 1 calc PR . -1 H10B H 0.2996 0.2505 0.5762 0.074 Uiso 0.50 1 calc PR . -1 F1 F 0.66433(12) 0.16312(11) 0.60454(7) 0.0233(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.01564(10) 0.01656(10) 0.00658(9) 0.000 0.000 -0.00126(8) N1 0.0167(8) 0.0192(8) 0.0064(6) -0.0001(6) 0.0001(6) 0.0014(6) C2 0.0164(9) 0.0260(11) 0.0103(9) -0.0001(8) -0.0007(7) -0.0026(8) C3 0.0170(10) 0.0262(11) 0.0127(8) -0.0032(8) -0.0012(7) -0.0036(8) C4 0.0195(10) 0.0256(11) 0.0151(9) 0.0001(8) 0.0001(8) -0.0064(8) C5 0.0170(9) 0.0250(10) 0.0099(8) 0.0019(8) 0.0011(7) -0.0031(7) C1 0.0110(8) 0.0182(9) 0.0114(8) 0.0010(7) 0.0018(7) 0.0017(7) C6 0.0246(11) 0.0444(13) 0.0115(9) -0.0055(9) -0.0002(8) -0.0158(10) C9 0.0230(12) 0.074(2) 0.0206(12) -0.0026(12) -0.0050(10) -0.0146(12) C7 0.0354(13) 0.0560(16) 0.0111(9) -0.0057(10) -0.0032(9) -0.0209(12) C8 0.0431(15) 0.0461(15) 0.0228(12) -0.0109(11) 0.0045(11) -0.0213(12) Cl1 0.0449(4) 0.0672(6) 0.0595(5) 0.0002(4) 0.0023(4) 0.0099(4) C10 0.062(4) 0.049(4) 0.076(5) -0.010(4) -0.033(4) 0.004(3) F1 0.0302(6) 0.0292(7) 0.0106(5) 0.0025(5) 0.0012(5) -0.0118(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 F1 1.9708(11) . ? Pd1 F1 1.9708(11) 2_655 ? Pd1 N1 1.9722(15) 2_655 ? Pd1 N1 1.9722(15) . ? N1 C5 1.341(3) . ? N1 C1 1.351(2) . ? C2 C1 1.384(3) . ? C2 C3 1.391(3) . ? C3 C4 1.398(3) . ? C3 C6 1.525(3) . ? C4 C5 1.376(3) . ? C1 C1 1.478(4) 2_655 ? C6 C7 1.528(3) . ? C6 C8 1.533(4) . ? C6 C9 1.536(4) . ? Cl1 C10 1.740(4) . ? Cl1 C10 1.772(4) 2 ? C10 Cl1 1.772(4) 2 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag F1 Pd1 F1 91.70(7) . 2_655 ? F1 Pd1 N1 174.52(6) . 2_655 ? F1 Pd1 N1 93.64(6) 2_655 2_655 ? F1 Pd1 N1 93.64(6) . . ? F1 Pd1 N1 174.52(6) 2_655 . ? N1 Pd1 N1 81.04(9) 2_655 . ? C5 N1 C1 119.49(16) . . ? C5 N1 Pd1 124.67(12) . . ? C1 N1 Pd1 115.80(13) . . ? C1 C2 C3 119.91(18) . . ? C2 C3 C4 117.50(18) . . ? C2 C3 C6 123.20(18) . . ? C4 C3 C6 119.29(19) . . ? C5 C4 C3 120.10(19) . . ? N1 C5 C4 121.63(17) . . ? N1 C1 C2 121.34(17) . . ? N1 C1 C1 113.66(11) . 2_655 ? C2 C1 C1 124.97(11) . 2_655 ? C3 C6 C7 111.63(18) . . ? C3 C6 C8 108.4(2) . . ? C7 C6 C8 109.5(2) . . ? C3 C6 C9 108.32(19) . . ? C7 C6 C9 109.0(2) . . ? C8 C6 C9 109.9(2) . . ? C10 Cl1 C10 45.9(4) . 2 ? Cl1 C10 Cl1 114.5(3) . 2 ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 28.33 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.143 _refine_diff_density_min -1.091 _refine_diff_density_rms 0.122