# Copyright The royal Society of chemistry, 1998 # CCDC Number: 186/1184 data_cad6 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C38 H30 Cl2 N4 P2 Pd' _chemical_formula_weight 781.90 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' '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 'P 2(1)/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.5452(7) _cell_length_b 12.9923(5) _cell_length_c 13.8799(7) _cell_angle_alpha 90.00 _cell_angle_beta 93.862(6) _cell_angle_gamma 90.00 _cell_volume 1717.4(2) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.512 _exptl_crystal_density_method ? _exptl_crystal_F_000 792 _exptl_absorpt_coefficient_mu 0.823 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.69596 _exptl_absorpt_correction_T_max 0.85904 _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device ? _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3226 _diffrn_reflns_av_R_equivalents 0.0399 _diffrn_reflns_av_sigmaI/netI 0.0308 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.15 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3022 _reflns_number_observed 2595 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R- factors wR and all goodnesses of fit S are based on F^2^, conventional R- factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0651P)^2^+0.4530P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3022 _refine_ls_number_parameters 214 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0432 _refine_ls_R_factor_obs 0.0349 _refine_ls_wR_factor_all 0.1006 _refine_ls_wR_factor_obs 0.0937 _refine_ls_goodness_of_fit_all 1.045 _refine_ls_goodness_of_fit_obs 1.056 _refine_ls_restrained_S_all 1.045 _refine_ls_restrained_S_obs 1.056 _refine_ls_shift/esd_max 0.002 _refine_ls_shift/esd_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Pd1 Pd 0.0000 0.0000 0.0000 0.02408(14) Uani 1 d S . P1 P 0.25747(8) -0.33841(6) 0.15828(6) 0.0228(2) Uani 1 d . . Cl1 Cl 0.18251(9) 0.10297(6) -0.04067(6) 0.0347(2) Uani 1 d . . N1 N 0.1276(3) -0.1183(2) 0.0215(2) 0.0327(6) Uani 1 d . . C1 C 0.1696(3) -0.1995(2) 0.0397(2) 0.0251(6) Uani 1 d . . N2 N 0.2182(3) -0.2917(2) 0.0525(2) 0.0266(6) Uani 1 d . . C2 C 0.3754(3) -0.2565(2) 0.2287(2) 0.0248(6) Uani 1 d . . C3 C 0.4891(3) -0.2171(2) 0.1820(2) 0.0314(7) Uani 1 d . . H3A H 0.4987(3) -0.2325(2) 0.1159(2) 0.038 Uiso 1 calc R . C4 C 0.5870(4) -0.1562(3) 0.2320(3) 0.0366(8) Uani 1 d . . H4A H 0.6636(4) -0.1286(3) 0.2001(3) 0.044 Uiso 1 calc R . C5 C 0.5738(4) -0.1354(3) 0.3282(3) 0.0377(8) Uani 1 d . . H5A H 0.6432(4) -0.0951(3) 0.3630(3) 0.045 Uiso 1 calc R . C6 C 0.4613(4) -0.1724(3) 0.3742(3) 0.0390(8) Uani 1 d . . H6A H 0.4517(4) -0.1562(3) 0.4402(3) 0.047 Uiso 1 calc R . C7 C 0.3617(4) -0.2334(3) 0.3244(2) 0.0333(7) Uani 1 d . . H7A H 0.2840(4) -0.2593(3) 0.3562(2) 0.040 Uiso 1 calc R . C8 C 0.3472(3) -0.4567(2) 0.1389(2) 0.0269(7) Uani 1 d . . C9 C 0.4450(4) -0.4949(2) 0.2087(3) 0.0359(8) Uani 1 d . . H9A H 0.4655(4) -0.4577(2) 0.2669(3) 0.043 Uiso 1 calc R . C10 C 0.5127(4) -0.5872(3) 0.1930(3) 0.0437(9) Uani 1 d . . H10A H 0.5793(4) -0.6135(3) 0.2407(3) 0.052 Uiso 1 calc R . C11 C 0.4836(4) -0.6406(3) 0.1090(3) 0.0464(10) Uani 1 d . . H11A H 0.5313(4) -0.7033(3) 0.0981(3) 0.056 Uiso 1 calc R . C12 C 0.3849(4) -0.6037(3) 0.0397(3) 0.0456(9) Uani 1 d . . H12A H 0.3636(4) -0.6417(3) -0.0179(3) 0.055 Uiso 1 calc R . C13 C 0.3176(4) -0.5117(3) 0.0546(3) 0.0358(8) Uani 1 d . . H13A H 0.2507(4) -0.4860(3) 0.0068(3) 0.043 Uiso 1 calc R . C14 C 0.1044(3) -0.3650(2) 0.2225(2) 0.0257(6) Uani 1 d . . C15 C -0.0264(3) -0.3315(2) 0.1854(2) 0.0311(7) Uani 1 d . . H15A H -0.0344(3) -0.2948(2) 0.1261(2) 0.037 Uiso 1 calc R . C16 C -0.1454(4) -0.3514(3) 0.2345(3) 0.0391(8) Uani 1 d . . H16A H -0.2352(4) -0.3306(3) 0.2079(3) 0.047 Uiso 1 calc R . C17 C -0.1325(4) -0.4014(3) 0.3221(3) 0.0467(10) Uani 1 d . . H17A H -0.2134(4) -0.4134(3) 0.3568(3) 0.056 Uiso 1 calc R . C18 C -0.0023(4) -0.4343(3) 0.3601(3) 0.0459(10) Uani 1 d . . H18A H 0.0055(4) -0.4685(3) 0.4207(3) 0.055 Uiso 1 calc R . C19 C 0.1157(4) -0.4177(3) 0.3106(2) 0.0370(8) Uani 1 d . . H19A H 0.2045(4) -0.4418(3) 0.3362(2) 0.044 Uiso 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 0.0327(2) 0.0182(2) 0.0213(2) 0.00342(12) 0.00068(13) 0.00978(13) P1 0.0251(4) 0.0176(4) 0.0251(4) 0.0030(3) -0.0024(3) 0.0037(3) Cl1 0.0394(5) 0.0300(4) 0.0349(4) 0.0035(3) 0.0046(3) 0.0038(3) N1 0.040(2) 0.0252(15) 0.033(2) 0.0045(12) 0.0045(12) 0.0098(12) C1 0.027(2) 0.027(2) 0.0221(14) 0.0029(12) 0.0028(12) 0.0041(13) N2 0.0331(14) 0.0202(13) 0.0260(13) 0.0032(10) -0.0007(11) 0.0091(11) C2 0.0251(15) 0.0188(14) 0.030(2) 0.0036(12) -0.0035(12) 0.0034(12) C3 0.031(2) 0.026(2) 0.037(2) -0.0034(14) 0.0057(14) -0.0012(14) C4 0.031(2) 0.030(2) 0.050(2) 0.001(2) 0.006(2) -0.0048(14) C5 0.035(2) 0.033(2) 0.043(2) -0.001(2) -0.008(2) -0.0074(15) C6 0.042(2) 0.042(2) 0.032(2) -0.002(2) -0.004(2) -0.006(2) C7 0.033(2) 0.036(2) 0.030(2) 0.0025(14) -0.0015(13) -0.0054(15) C8 0.030(2) 0.0158(15) 0.035(2) 0.0070(13) -0.0019(13) 0.0047(12) C9 0.041(2) 0.025(2) 0.040(2) 0.0047(14) -0.011(2) 0.0059(14) C10 0.038(2) 0.029(2) 0.062(2) 0.013(2) -0.011(2) 0.010(2) C11 0.048(2) 0.023(2) 0.070(3) 0.008(2) 0.012(2) 0.013(2) C12 0.064(3) 0.031(2) 0.043(2) -0.003(2) 0.006(2) 0.011(2) C13 0.049(2) 0.028(2) 0.030(2) 0.0025(13) -0.003(2) 0.0086(15) C14 0.029(2) 0.0212(15) 0.027(2) -0.0011(12) 0.0017(12) -0.0039(13) C15 0.032(2) 0.024(2) 0.038(2) -0.0048(14) 0.0017(14) 0.0036(13) C16 0.030(2) 0.030(2) 0.059(2) -0.009(2) 0.009(2) -0.0022(14) C17 0.050(2) 0.036(2) 0.056(2) -0.013(2) 0.021(2) -0.018(2) C18 0.061(3) 0.041(2) 0.037(2) 0.005(2) 0.009(2) -0.020(2) C19 0.040(2) 0.034(2) 0.036(2) 0.0020(15) -0.0021(15) -0.011(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 N1 1.971(3) 3 ? Pd1 N1 1.971(3) . y Pd1 Cl1 2.2969(9) . y Pd1 Cl1 2.2969(9) 3 ? P1 N2 1.609(3) . y P1 C8 1.789(3) . y P1 C2 1.791(3) . y P1 C14 1.796(3) . y N1 C1 1.151(4) . y C1 N2 1.292(4) . y C2 C7 1.375(5) . ? C2 C3 1.398(4) . ? C3 C4 1.377(5) . ? C3 H3A 0.95 . ? C4 C5 1.376(5) . ? C4 H4A 0.95 . ? C5 C6 1.373(5) . ? C5 H5A 0.95 . ? C6 C7 1.387(5) . ? C6 H6A 0.95 . ? C7 H7A 0.95 . ? C8 C13 1.384(5) . ? C8 C9 1.391(4) . ? C9 C10 1.386(5) . ? C9 H9A 0.95 . ? C10 C11 1.370(6) . ? C10 H10A 0.95 . ? C11 C12 1.385(5) . ? C11 H11A 0.95 . ? C12 C13 1.380(5) . ? C12 H12A 0.95 . ? C13 H13A 0.95 . ? C14 C15 1.388(4) . ? C14 C19 1.399(5) . ? C15 C16 1.388(5) . ? C15 H15A 0.95 . ? C16 C17 1.377(6) . ? C16 H16A 0.95 . ? C17 C18 1.384(6) . ? C17 H17A 0.95 . ? C18 C19 1.375(5) . ? C18 H18A 0.95 . ? C19 H19A 0.95 . ? 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 N1 Pd1 N1 180.0 3 . y N1 Pd1 Cl1 88.84(9) 3 . y N1 Pd1 Cl1 91.16(9) . . y N1 Pd1 Cl1 91.16(9) 3 3 ? N1 Pd1 Cl1 88.84(9) . 3 ? Cl1 Pd1 Cl1 180.0 . 3 ? N2 P1 C8 105.74(14) . . y N2 P1 C2 111.91(14) . . y C8 P1 C2 107.65(14) . . y N2 P1 C14 112.23(14) . . y C8 P1 C14 108.84(14) . . y C2 P1 C14 110.22(14) . . y C1 N1 Pd1 161.9(3) . . y N1 C1 N2 175.2(3) . . y C1 N2 P1 122.3(2) . . y C7 C2 C3 119.7(3) . . ? C7 C2 P1 124.0(2) . . ? C3 C2 P1 116.3(2) . . ? C4 C3 C2 119.9(3) . . ? C4 C3 H3A 120.1(2) . . ? C2 C3 H3A 120.1(2) . . ? C3 C4 C5 119.9(3) . . ? C3 C4 H4A 120.0(2) . . ? C5 C4 H4A 120.0(2) . . ? C6 C5 C4 120.6(3) . . ? C6 C5 H5A 119.7(2) . . ? C4 C5 H5A 119.7(2) . . ? C5 C6 C7 119.9(3) . . ? C5 C6 H6A 120.0(2) . . ? C7 C6 H6A 120.0(2) . . ? C2 C7 C6 120.0(3) . . ? C2 C7 H7A 120.0(2) . . ? C6 C7 H7A 120.0(2) . . ? C13 C8 C9 119.6(3) . . ? C13 C8 P1 119.9(2) . . ? C9 C8 P1 120.5(3) . . ? C10 C9 C8 119.8(4) . . ? C10 C9 H9A 120.1(2) . . ? C8 C9 H9A 120.1(2) . . ? C11 C10 C9 120.1(3) . . ? C11 C10 H10A 119.9(2) . . ? C9 C10 H10A 119.9(2) . . ? C10 C11 C12 120.3(3) . . ? C10 C11 H11A 119.8(2) . . ? C12 C11 H11A 119.8(2) . . ? C13 C12 C11 119.9(4) . . ? C13 C12 H12A 120.1(2) . . ? C11 C12 H12A 120.1(2) . . ? C12 C13 C8 120.2(3) . . ? C12 C13 H13A 119.9(2) . . ? C8 C13 H13A 119.9(2) . . ? C15 C14 C19 119.5(3) . . ? C15 C14 P1 119.8(2) . . ? C19 C14 P1 120.7(2) . . ? C14 C15 C16 120.3(3) . . ? C14 C15 H15A 119.8(2) . . ? C16 C15 H15A 119.8(2) . . ? C17 C16 C15 119.6(4) . . ? C17 C16 H16A 120.2(2) . . ? C15 C16 H16A 120.2(2) . . ? C16 C17 C18 120.4(4) . . ? C16 C17 H17A 119.8(2) . . ? C18 C17 H17A 119.8(2) . . ? C19 C18 C17 120.4(4) . . ? C19 C18 H18A 119.8(2) . . ? C17 C18 H18A 119.8(2) . . ? C18 C19 C14 119.7(3) . . ? C18 C19 H19A 120.2(2) . . ? C14 C19 H19A 120.2(2) . . ? _refine_diff_density_max 0.875 _refine_diff_density_min -0.924 _refine_diff_density_rms 0.085