data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Philip Dyer' _publ_contact_author_address ; Department of Chemistry Durham University South Road Durham DH1 3LE UNITED KINGDOM ; _publ_contact_author_email P.W.DYER@DURHAM.AC.UK _publ_section_title ; Concise syntheses of tridentate PNE ligands and their coordination chemistry with palladium(II) : a solution- and solid-state study ; loop_ _publ_author_name 'Philip Dyer' 'Carly E. Anderso' 'D. C. Apperley' 'A. Batsanov' 'J. Howard' #====================================================================== data_(1) _database_code_depnum_ccdc_archive 'CCDC 605821' _audit_creation_method SHELXL-97 _chemical_name_systematic ; 1-(2-diphenylphosphino-ethyl)-4-methyl-piperazine ; _chemical_name_common 1-(2-diphenylphosphino-ethyl)-4-methyl-piperazine _chemical_melting_point ? _chemical_formula_moiety 'C19 H25 N2 P' _chemical_formula_sum 'C19 H25 N2 P' _chemical_formula_weight 312.38 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' _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 7.1829(14) _cell_length_b 7.3477(14) _cell_length_c 33.014(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.10(1) _cell_angle_gamma 90.00 _cell_volume 1742.4(6) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 4750 _cell_measurement_theta_min 2.83 _cell_measurement_theta_max 27.22 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.191 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 672 _exptl_absorpt_coefficient_mu 0.157 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ;The data collection nominally covered full sphere of reciprocal space, by a combination of 3 sets of \w scans; each set at different \f angles and each scan (20 sec exposure) covering 0.3\% in \w. Crystal to detector distance 6.85 cm. Twinned crystal: two specimens indexed in orientation matrices (0.13204, -0.03833, 0.00438 / 0.02387, 0.00923, -0.02978 / 0.03713, 0.13026, 0.00337) [main specimen, used for data collection] and (-0.13240, -0.03687, -0.00428 / -0.02213, 0.00402, 0.02991 / -0.03686, 0.13098, -0.00218). Reflections overlap imperfectly, intensity correction was unsuccessful. ; _diffrn_ambient_temperature 120(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 'Bruker SMART 6000 CCD area detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 5.6 _diffrn_standards_number 0 _diffrn_reflns_number 16022 _diffrn_reflns_av_R_equivalents 0.0818 _diffrn_reflns_av_sigmaI/netI 0.0774 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -42 _diffrn_reflns_limit_l_max 42 _diffrn_reflns_theta_min 2.47 _diffrn_reflns_theta_max 27.50 _reflns_number_total 4000 _reflns_number_gt 3059 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'SMART version 5.625 (Bruker, 2001)' _computing_cell_refinement 'SAINT version 6.02A (Bruker, 2001)' _computing_data_reduction 'SAINT version 6.02A (Bruker, 2001)' _computing_structure_solution 'SHELXTL version 6.12 (Bruker, 2001)' _computing_structure_refinement 'SHELXTL version 6.12 (Bruker, 2001)' _computing_molecular_graphics 'SHELXTL version 6.12 (Bruker, 2001)' _computing_publication_material 'SHELXTL version 6.12 (Bruker, 2001)' _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. Methyl group - rigid rotating body, othet H atoms - riding. ; _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^)+(0.0536P)^2^+3.5991P] 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 4000 _refine_ls_number_parameters 200 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0919 _refine_ls_R_factor_gt 0.0753 _refine_ls_wR_factor_ref 0.2008 _refine_ls_wR_factor_gt 0.1933 _refine_ls_goodness_of_fit_ref 1.121 _refine_ls_restrained_S_all 1.121 _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 P P 0.43855(11) 0.72820(11) 0.16358(2) 0.0224(2) Uani 1 1 d . . . N1 N 0.7397(4) 0.7151(4) 0.10265(8) 0.0250(6) Uani 1 1 d . . . N4 N 0.8422(4) 0.4468(4) 0.04373(8) 0.0276(6) Uani 1 1 d . . . C2 C 0.7909(5) 0.7662(5) 0.06154(10) 0.0305(7) Uani 1 1 d . . . H2A H 0.7244 0.8742 0.0539 0.037 Uiso 1 1 d R . . H2B H 0.9218 0.7923 0.0605 0.037 Uiso 1 1 d R . . C3 C 0.7465(5) 0.6145(5) 0.03230(10) 0.0322(8) Uani 1 1 d . . . H3A H 0.7823 0.6492 0.0054 0.039 Uiso 1 1 d R . . H3B H 0.6146 0.5935 0.0323 0.039 Uiso 1 1 d R . . C5 C 0.7875(5) 0.3958(5) 0.08475(10) 0.0285(7) Uani 1 1 d . . . H5A H 0.6556 0.3748 0.0856 0.034 Uiso 1 1 d R . . H5B H 0.8495 0.2855 0.0926 0.034 Uiso 1 1 d R . . C6 C 0.8367(5) 0.5472(4) 0.11392(10) 0.0264(7) Uani 1 1 d . . . H6A H 0.9687 0.5677 0.1131 0.032 Uiso 1 1 d R . . H6B H 0.8040 0.5129 0.1411 0.032 Uiso 1 1 d R . . C7 C 0.7710(5) 0.8606(5) 0.13194(10) 0.0287(7) Uani 1 1 d . . . H8A H 0.9025 0.8762 0.1360 0.034 Uiso 1 1 d R . . H8B H 0.7222 0.9722 0.1212 0.034 Uiso 1 1 d R . . C8 C 0.6757(4) 0.8216(5) 0.17246(10) 0.0265(7) Uani 1 1 d . . . H7A H 0.6680 0.9310 0.1883 0.032 Uiso 1 1 d R . . H7B H 0.7485 0.7345 0.1873 0.032 Uiso 1 1 d R . . C9 C 0.7993(5) 0.2995(5) 0.01528(11) 0.0361(8) Uani 1 1 d . . . H9A H 0.8360 0.3341 -0.0116 0.046(7) Uiso 1 1 d R . . H9B H 0.6680 0.2751 0.0157 0.046(7) Uiso 1 1 d R . . H9C H 0.8661 0.1921 0.0233 0.046(7) Uiso 1 1 d R . . C11 C 0.3435(4) 0.9225(4) 0.13533(9) 0.0225(6) Uani 1 1 d . . . C12 C 0.3103(4) 1.0927(4) 0.15281(10) 0.0262(7) Uani 1 1 d . . . H12 H 0.3227 1.1069 0.1816 0.031 Uiso 1 1 d R . . C13 C 0.2576(5) 1.2401(5) 0.12902(11) 0.0301(7) Uani 1 1 d . . . H13 H 0.2380 1.3565 0.1415 0.036 Uiso 1 1 d R . . C14 C 0.2358(5) 1.2198(5) 0.08759(11) 0.0322(7) Uani 1 1 d . . . H14 H 0.1984 1.3216 0.0713 0.039 Uiso 1 1 d R . . C15 C 0.2660(5) 1.0506(5) 0.06981(10) 0.0327(8) Uani 1 1 d . . . H15 H 0.2506 1.0354 0.0411 0.039 Uiso 1 1 d R . . C16 C 0.3192(4) 0.9028(5) 0.09362(10) 0.0282(7) Uani 1 1 d . . . H16 H 0.3394 0.7862 0.0813 0.034 Uiso 1 1 d R . . C21 C 0.3306(4) 0.7553(4) 0.21376(9) 0.0239(6) Uani 1 1 d . . . C22 C 0.4161(5) 0.8279(4) 0.24805(10) 0.0279(7) Uani 1 1 d . . . H22 H 0.5389 0.8787 0.2461 0.033 Uiso 1 1 d R . . C23 C 0.3257(5) 0.8265(5) 0.28543(10) 0.0288(7) Uani 1 1 d . . . H23 H 0.3856 0.8779 0.3088 0.035 Uiso 1 1 d R . . C24 C 0.1489(5) 0.7541(5) 0.28908(10) 0.0288(7) Uani 1 1 d . . . H24 H 0.0887 0.7522 0.3150 0.035 Uiso 1 1 d R . . C25 C 0.0610(5) 0.6821(5) 0.25523(10) 0.0301(7) Uani 1 1 d . . . H25 H -0.0627 0.6338 0.2575 0.036 Uiso 1 1 d R . . C26 C 0.1518(5) 0.6818(5) 0.21821(10) 0.0281(7) Uani 1 1 d . . . H26 H 0.0913 0.6295 0.1950 0.034 Uiso 1 1 d 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 P 0.0203(4) 0.0191(4) 0.0278(4) -0.0027(3) -0.0008(3) 0.0003(3) N1 0.0213(13) 0.0235(14) 0.0301(14) 0.0045(11) 0.0004(10) 0.0042(11) N4 0.0247(14) 0.0282(15) 0.0299(14) -0.0004(11) 0.0000(11) 0.0030(11) C2 0.0272(17) 0.0309(18) 0.0336(17) 0.0069(14) -0.0001(13) 0.0046(14) C3 0.0305(18) 0.036(2) 0.0299(17) 0.0066(14) -0.0021(13) 0.0027(15) C5 0.0240(16) 0.0276(17) 0.0339(17) 0.0035(13) 0.0031(13) 0.0027(13) C6 0.0250(16) 0.0253(16) 0.0290(16) 0.0056(12) 0.0017(12) 0.0058(13) C7 0.0214(15) 0.0274(17) 0.0374(18) 0.0002(13) -0.0013(13) 0.0004(13) C8 0.0206(15) 0.0251(17) 0.0339(17) -0.0023(12) -0.0010(12) 0.0015(12) C9 0.0346(19) 0.035(2) 0.0388(19) -0.0049(15) -0.0022(15) -0.0010(16) C11 0.0157(14) 0.0214(15) 0.0304(16) -0.0001(12) 0.0001(11) 0.0003(11) C12 0.0239(16) 0.0254(17) 0.0292(16) -0.0030(12) -0.0017(12) 0.0012(13) C13 0.0262(16) 0.0220(17) 0.0422(19) -0.0001(13) -0.0005(14) 0.0040(13) C14 0.0272(17) 0.0302(18) 0.0393(19) 0.0079(14) -0.0001(14) 0.0061(14) C15 0.0285(17) 0.041(2) 0.0284(17) 0.0000(14) -0.0022(13) 0.0047(15) C16 0.0227(16) 0.0295(17) 0.0322(17) -0.0044(13) -0.0014(13) 0.0024(13) C21 0.0233(15) 0.0241(16) 0.0244(15) -0.0014(12) -0.0009(11) 0.0034(12) C22 0.0250(16) 0.0245(17) 0.0341(17) -0.0040(13) -0.0034(13) 0.0004(13) C23 0.0340(18) 0.0253(17) 0.0271(16) -0.0049(12) -0.0066(13) 0.0050(14) C24 0.0312(17) 0.0272(18) 0.0280(16) -0.0003(13) 0.0030(13) 0.0048(14) C25 0.0261(16) 0.0292(18) 0.0349(18) 0.0002(13) 0.0025(13) -0.0027(13) C26 0.0258(16) 0.0289(18) 0.0295(16) -0.0015(13) -0.0045(13) -0.0014(13) _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 P C11 1.836(3) . ? P C21 1.841(3) . ? P C8 1.859(3) . ? N1 C2 1.456(4) . ? N1 C7 1.459(4) . ? N1 C6 1.465(4) . ? N4 C5 1.460(4) . ? N4 C3 1.460(4) . ? N4 C9 1.465(4) . ? C2 C3 1.508(5) . ? C5 C6 1.513(5) . ? C7 C8 1.531(5) . ? C11 C16 1.395(4) . ? C11 C12 1.398(4) . ? C12 C13 1.390(5) . ? C13 C14 1.384(5) . ? C14 C15 1.392(5) . ? C15 C16 1.394(5) . ? C21 C22 1.393(4) . ? C21 C26 1.401(5) . ? C22 C23 1.395(5) . ? C23 C24 1.382(5) . ? C24 C25 1.387(5) . ? C25 C26 1.386(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C11 P C21 102.49(14) . . ? C11 P C8 97.63(14) . . ? C21 P C8 101.86(15) . . ? C2 N1 C7 113.0(3) . . ? C2 N1 C6 109.5(2) . . ? C7 N1 C6 112.1(3) . . ? C5 N4 C3 109.2(3) . . ? C5 N4 C9 110.4(3) . . ? C3 N4 C9 111.1(3) . . ? N1 C2 C3 110.6(3) . . ? N4 C3 C2 111.1(3) . . ? N4 C5 C6 109.8(3) . . ? N1 C6 C5 110.3(3) . . ? N1 C7 C8 111.9(3) . . ? C7 C8 P 110.0(2) . . ? C16 C11 C12 118.7(3) . . ? C16 C11 P 117.8(2) . . ? C12 C11 P 123.3(2) . . ? C13 C12 C11 120.7(3) . . ? C14 C13 C12 120.3(3) . . ? C13 C14 C15 119.7(3) . . ? C14 C15 C16 120.1(3) . . ? C15 C16 C11 120.6(3) . . ? C22 C21 C26 117.7(3) . . ? C22 C21 P 125.9(3) . . ? C26 C21 P 116.1(2) . . ? C21 C22 C23 120.7(3) . . ? C24 C23 C22 120.6(3) . . ? C23 C24 C25 119.6(3) . . ? C26 C25 C24 119.7(3) . . ? C25 C26 C21 121.7(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C7 N1 C2 C3 -177.1(3) . . . . ? C6 N1 C2 C3 57.2(3) . . . . ? C5 N4 C3 C2 58.1(4) . . . . ? C9 N4 C3 C2 -179.9(3) . . . . ? N1 C2 C3 N4 -57.8(4) . . . . ? C3 N4 C5 C6 -59.0(3) . . . . ? C9 N4 C5 C6 178.6(3) . . . . ? C2 N1 C6 C5 -58.6(3) . . . . ? C7 N1 C6 C5 175.2(3) . . . . ? N4 C5 C6 N1 60.0(3) . . . . ? C2 N1 C7 C8 166.7(3) . . . . ? C6 N1 C7 C8 -69.1(3) . . . . ? N1 C7 C8 P -42.5(3) . . . . ? C11 P C8 C7 -59.8(2) . . . . ? C21 P C8 C7 -164.3(2) . . . . ? C21 P C11 C16 -149.7(2) . . . . ? C8 P C11 C16 106.2(3) . . . . ? C21 P C11 C12 36.1(3) . . . . ? C8 P C11 C12 -67.9(3) . . . . ? P C11 C12 C13 172.9(2) . . . . ? P C11 C16 C15 -173.4(3) . . . . ? C11 P C21 C22 -101.0(3) . . . . ? C8 P C21 C22 -0.3(3) . . . . ? C11 P C21 C26 84.6(3) . . . . ? C8 P C21 C26 -174.7(2) . . . . ? P C21 C22 C23 -174.2(3) . . . . ? P C21 C26 C25 175.4(3) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.917 _refine_diff_density_min -0.426 _refine_diff_density_rms 0.083 #=====================================END data_(5) _database_code_depnum_ccdc_archive 'CCDC 605822' _audit_creation_method SHELXL-97 _chemical_name_systematic ; 1-(2-diphenylphosphino-isopropyl)-4-methyl-piperazine hydrochloride ; _chemical_name_common ;1-(2-diphenylphosphino-isopropyl)-4-methyl-piperazine hydrochloride ; _chemical_melting_point ? _chemical_formula_moiety 'C20 H28 N2 P 1+,Cl 1-' _chemical_formula_sum 'C20 H28 Cl N2 P' _chemical_formula_weight 362.86 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' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Fdd2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/4, -y+1/4, z+1/4' '-x+1/4, y+1/4, z+1/4' 'x, y+1/2, z+1/2' '-x, -y+1/2, z+1/2' 'x+1/4, -y+3/4, z+3/4' '-x+1/4, y+3/4, z+3/4' 'x+1/2, y, z+1/2' '-x+1/2, -y, z+1/2' 'x+3/4, -y+1/4, z+3/4' '-x+3/4, y+1/4, z+3/4' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z' 'x+3/4, -y+3/4, z+1/4' '-x+3/4, y+3/4, z+1/4' _cell_length_a 20.016(2) _cell_length_b 68.506(9) _cell_length_c 5.9460(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 8153.3(17) _cell_formula_units_Z 16 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 5762 _cell_measurement_theta_min 2.36 _cell_measurement_theta_max 25.35 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.52 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.182 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3104 _exptl_absorpt_coefficient_mu 0.270 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8031 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'SADABS v.2.10 (Bruker,2003), R(int)=0.085 before correction' _exptl_special_details ;The data collection nominally covered full sphere of reciprocal space, by a combination of 4 runs of narrow-frame \w-scans (scan width 0.3\% \w, 31.4 s exposure), every run at a different \f angle. Crystal to detector distance 5.47 cm. 2298 unique reflections after merging Friedel equivalents. ; _diffrn_ambient_temperature 120(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 'Siemens SMART 1K CCD area detector' _diffrn_measurement_method '\W scans' _diffrn_detector_area_resol_mean 8 _diffrn_standards_number 0 _diffrn_reflns_number 16540 _diffrn_reflns_av_R_equivalents 0.0521 _diffrn_reflns_av_sigmaI/netI 0.0520 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -85 _diffrn_reflns_limit_k_max 86 _diffrn_reflns_limit_l_min -7 _diffrn_reflns_limit_l_max 7 _diffrn_reflns_theta_min 2.12 _diffrn_reflns_theta_max 27.06 _reflns_number_total 3952 _reflns_number_gt 3234 _reflns_threshold_expression I>2\s(I) _reflns_Friedel_coverage 0.72 _computing_data_collection 'SMART version 5.054 (Bruker, 1999)' _computing_cell_refinement 'SAINT version 6.45A (Bruker, 2003)' _computing_data_reduction 'SAINT version 6.45A (Bruker, 2003)' _computing_structure_solution 'SHELXTL version 6.14 (Bruker, 2003)' _computing_structure_refinement 'SHELXTL version 6.14 (Bruker, 2003)' _computing_molecular_graphics 'SHELXTL version 6.14 (Bruker, 2003)' _computing_publication_material 'SHELXTL version 6.14 (Bruker, 2003)' _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. Methyl groups were refined as rigid bodies rotating around C---C and N---C bonds, with a common refined U for three H atoms. Other H atoms - "riding" (constr). ; _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^)+(0.0600P)^2^+31.7710P] 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 mixed _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(13) _refine_ls_number_reflns 3952 _refine_ls_number_parameters 225 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0909 _refine_ls_R_factor_gt 0.0711 _refine_ls_wR_factor_ref 0.1639 _refine_ls_wR_factor_gt 0.1554 _refine_ls_goodness_of_fit_ref 1.132 _refine_ls_restrained_S_all 1.132 _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 Cl Cl 0.61434(5) 0.620541(18) -0.29445(18) 0.0429(3) Uani 1 1 d . . . P P 0.41564(7) 0.54703(2) 0.4178(2) 0.0520(4) Uani 1 1 d . . . N1 N 0.50797(16) 0.57498(5) 0.1692(7) 0.0406(9) Uani 1 1 d . . . N4 N 0.49337(16) 0.61371(6) -0.0067(6) 0.0343(9) Uani 1 1 d . . . H4N H 0.5248(19) 0.6141(5) -0.097(7) 0.017(10) Uiso 1 1 d . . . C2 C 0.55400(19) 0.59064(6) 0.2341(8) 0.0391(11) Uani 1 1 d . . . H20 H 0.5932 0.5906 0.1326 0.047 Uiso 1 1 d R . . H21 H 0.5700 0.5884 0.3894 0.047 Uiso 1 1 d R . . C3 C 0.51995(19) 0.61006(6) 0.2207(8) 0.0340(9) Uani 1 1 d . . . H31 H 0.4829 0.6104 0.3308 0.041 Uiso 1 1 d R . . H32 H 0.5520 0.6205 0.2607 0.041 Uiso 1 1 d R . . C5 C 0.44712(19) 0.59741(7) -0.0763(8) 0.0446(12) Uani 1 1 d . . . H51 H 0.4076 0.5971 0.0236 0.054 Uiso 1 1 d R . . H52 H 0.4316 0.5995 -0.2325 0.054 Uiso 1 1 d R . . C6 C 0.4842(2) 0.57834(7) -0.0581(9) 0.0489(12) Uani 1 1 d . . . H61 H 0.4543 0.5675 -0.1038 0.059 Uiso 1 1 d R . . H62 H 0.5227 0.5786 -0.1627 0.059 Uiso 1 1 d R . . C7 C 0.5376(2) 0.55566(7) 0.2129(11) 0.0564(14) Uani 1 1 d . . . H7 H 0.5562 0.5561 0.3688 0.068 Uiso 1 1 d R . . C8 C 0.4818(2) 0.54017(7) 0.2148(12) 0.0599(14) Uani 1 1 d . . . H81 H 0.5008 0.5273 0.2563 0.072 Uiso 1 1 d R . . H82 H 0.4623 0.5391 0.0623 0.072 Uiso 1 1 d R . . C9 C 0.4635(2) 0.63321(7) -0.0338(10) 0.0466(12) Uani 1 1 d . . . H91 H 0.4984 0.6432 -0.0217 0.051(8) Uiso 1 1 d R . . H92 H 0.4299 0.6353 0.0840 0.051(8) Uiso 1 1 d R . . H93 H 0.4420 0.6342 -0.1818 0.051(8) Uiso 1 1 d R . . C10 C 0.5936(3) 0.54965(10) 0.0600(15) 0.088(3) Uani 1 1 d . . . H101 H 0.6295 0.5594 0.0666 0.088(13) Uiso 1 1 d R . . H102 H 0.5771 0.5486 -0.0948 0.088(13) Uiso 1 1 d R . . H103 H 0.6108 0.5369 0.1089 0.088(13) Uiso 1 1 d R . . C11 C 0.3832(3) 0.52234(8) 0.4838(11) 0.0596(15) Uani 1 1 d . . . C12 C 0.3214(3) 0.51507(10) 0.4262(17) 0.094(2) Uani 1 1 d . . . H12 H 0.2914 0.5230 0.3428 0.113 Uiso 1 1 d R . . C13 C 0.3031(4) 0.49612(11) 0.487(2) 0.119(3) Uani 1 1 d . . . H13 H 0.2617 0.4911 0.4353 0.143 Uiso 1 1 d R . . C14 C 0.3419(3) 0.48504(11) 0.6149(16) 0.093(3) Uani 1 1 d . . . H14 H 0.3302 0.4719 0.6491 0.112 Uiso 1 1 d R . . C15 C 0.3967(5) 0.49306(11) 0.693(2) 0.129(4) Uani 1 1 d . . . H15 H 0.4240 0.4859 0.7945 0.155 Uiso 1 1 d R . . C16 C 0.4167(4) 0.51121(9) 0.6295(16) 0.112(3) Uani 1 1 d . . . H16 H 0.4562 0.5164 0.6943 0.134 Uiso 1 1 d R . . C21 C 0.3487(2) 0.55682(7) 0.2455(9) 0.0470(12) Uani 1 1 d . . . C22 C 0.3277(3) 0.54882(8) 0.0426(10) 0.0583(15) Uani 1 1 d . . . H22 H 0.3511 0.5380 -0.0177 0.070 Uiso 1 1 d R . . C23 C 0.2738(3) 0.55614(9) -0.0752(12) 0.0665(15) Uani 1 1 d . . . H23 H 0.2606 0.5502 -0.2128 0.080 Uiso 1 1 d R . . C24 C 0.2394(3) 0.57162(9) 0.0047(13) 0.0722(18) Uani 1 1 d . . . H24 H 0.2021 0.5764 -0.0769 0.087 Uiso 1 1 d R . . C25 C 0.2584(3) 0.58047(9) 0.2032(14) 0.0755(18) Uani 1 1 d . . . H25 H 0.2341 0.5914 0.2577 0.091 Uiso 1 1 d R . . C26 C 0.3138(3) 0.57338(8) 0.3228(10) 0.0598(15) Uani 1 1 d . . . H26 H 0.3276 0.5797 0.4571 0.072 Uiso 1 1 d 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 Cl 0.0243(4) 0.0744(8) 0.0298(5) -0.0054(6) 0.0052(4) -0.0098(5) P 0.0548(7) 0.0487(7) 0.0526(8) -0.0015(7) -0.0064(7) -0.0119(6) N1 0.0281(17) 0.048(2) 0.046(2) -0.008(2) -0.0048(17) -0.0079(15) N4 0.0193(16) 0.061(2) 0.0230(18) 0.0014(17) 0.0049(14) -0.0049(16) C2 0.0246(19) 0.050(3) 0.043(3) -0.006(2) -0.0042(19) -0.0007(18) C3 0.0261(19) 0.047(2) 0.029(2) -0.007(2) 0.0004(19) 0.0007(17) C5 0.029(2) 0.071(3) 0.033(3) 0.007(3) -0.002(2) -0.017(2) C6 0.043(2) 0.065(3) 0.038(3) -0.010(3) -0.002(2) -0.022(2) C7 0.038(2) 0.059(3) 0.072(4) -0.010(3) 0.003(3) -0.004(2) C8 0.046(3) 0.050(3) 0.083(4) -0.013(3) -0.004(3) -0.003(2) C9 0.032(2) 0.066(3) 0.042(3) 0.011(3) 0.007(2) 0.016(2) C10 0.067(4) 0.060(4) 0.137(8) -0.024(4) 0.014(4) -0.006(3) C11 0.052(3) 0.054(3) 0.073(4) 0.010(3) -0.001(3) -0.013(2) C12 0.072(4) 0.091(5) 0.119(6) 0.045(5) -0.018(5) -0.015(4) C13 0.088(5) 0.093(5) 0.177(9) 0.061(6) -0.029(6) -0.035(4) C14 0.064(4) 0.072(4) 0.144(8) 0.040(5) -0.017(4) -0.007(4) C15 0.138(7) 0.079(5) 0.170(10) 0.059(7) -0.057(8) -0.008(5) C16 0.137(7) 0.049(4) 0.150(9) 0.024(5) -0.060(7) -0.005(4) C21 0.046(3) 0.036(3) 0.058(3) -0.001(2) 0.005(2) -0.011(2) C22 0.046(3) 0.055(3) 0.074(4) -0.004(3) 0.003(3) -0.003(3) C23 0.060(3) 0.073(4) 0.067(4) 0.006(4) -0.002(3) -0.005(3) C24 0.065(4) 0.068(4) 0.083(5) 0.029(4) -0.011(3) -0.001(3) C25 0.069(4) 0.063(4) 0.095(5) 0.012(4) 0.009(4) 0.025(3) C26 0.073(4) 0.051(3) 0.056(4) -0.003(3) 0.008(3) -0.010(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag P C21 1.815(5) . ? P C8 1.851(6) . ? P C11 1.854(5) . ? N1 C6 1.452(7) . ? N1 C2 1.466(5) . ? N1 C7 1.473(6) . ? N4 C9 1.473(6) . ? N4 C3 1.474(6) . ? N4 C5 1.509(5) . ? N4 H4N 0.83(4) . ? C2 C3 1.497(6) . ? C2 H20 0.9901 . ? C2 H21 0.9899 . ? C3 H31 0.9900 . ? C3 H32 0.9903 . ? C5 C6 1.506(7) . ? C5 H51 0.9901 . ? C5 H52 0.9900 . ? C6 H61 0.9899 . ? C6 H62 0.9899 . ? C7 C10 1.501(8) . ? C7 C8 1.541(6) . ? C7 H7 1.0000 . ? C8 H81 0.9898 . ? C8 H82 0.9900 . ? C9 H91 0.9813 . ? C9 H92 0.9813 . ? C9 H93 0.9812 . ? C10 H101 0.9805 . ? C10 H102 0.9804 . ? C10 H103 0.9805 . ? C11 C16 1.334(9) . ? C11 C12 1.376(8) . ? C12 C13 1.396(9) . ? C12 H12 0.9502 . ? C13 C14 1.326(10) . ? C13 H13 0.9500 . ? C14 C15 1.314(11) . ? C14 H14 0.9499 . ? C15 C16 1.360(10) . ? C15 H15 0.9497 . ? C16 H16 0.9499 . ? C21 C22 1.390(8) . ? C21 C26 1.409(7) . ? C22 C23 1.381(8) . ? C22 H22 0.9496 . ? C23 C24 1.350(8) . ? C23 H23 0.9498 . ? C24 C25 1.380(10) . ? C24 H24 0.9500 . ? C25 C26 1.404(8) . ? C25 H25 0.9499 . ? C26 H26 0.9499 . ? 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 C21 P C8 104.7(3) . . ? C21 P C11 101.4(2) . . ? C8 P C11 99.0(2) . . ? C6 N1 C2 109.6(4) . . ? C6 N1 C7 116.0(4) . . ? C2 N1 C7 111.0(3) . . ? C9 N4 C3 113.6(4) . . ? C9 N4 C5 113.1(3) . . ? C3 N4 C5 110.4(3) . . ? C9 N4 H4N 102(3) . . ? C3 N4 H4N 109(3) . . ? C5 N4 H4N 108(3) . . ? N1 C2 C3 110.5(3) . . ? N1 C2 H20 109.6 . . ? C3 C2 H20 109.4 . . ? N1 C2 H21 109.5 . . ? C3 C2 H21 109.7 . . ? H20 C2 H21 108.1 . . ? N4 C3 C2 111.3(4) . . ? N4 C3 H31 109.4 . . ? C2 C3 H31 109.2 . . ? N4 C3 H32 109.4 . . ? C2 C3 H32 109.5 . . ? H31 C3 H32 108.0 . . ? C6 C5 N4 108.7(3) . . ? C6 C5 H51 109.6 . . ? N4 C5 H51 109.9 . . ? C6 C5 H52 110.4 . . ? N4 C5 H52 110.1 . . ? H51 C5 H52 108.3 . . ? N1 C6 C5 111.5(4) . . ? N1 C6 H61 109.6 . . ? C5 C6 H61 109.3 . . ? N1 C6 H62 109.4 . . ? C5 C6 H62 109.0 . . ? H61 C6 H62 108.0 . . ? N1 C7 C10 116.1(5) . . ? N1 C7 C8 109.2(4) . . ? C10 C7 C8 110.9(5) . . ? N1 C7 H7 106.7 . . ? C10 C7 H7 106.9 . . ? C8 C7 H7 106.5 . . ? C7 C8 P 110.4(4) . . ? C7 C8 H81 109.6 . . ? P C8 H81 109.8 . . ? C7 C8 H82 109.4 . . ? P C8 H82 109.5 . . ? H81 C8 H82 108.2 . . ? N4 C9 H91 109.6 . . ? N4 C9 H92 109.5 . . ? H91 C9 H92 109.4 . . ? N4 C9 H93 109.7 . . ? H91 C9 H93 109.3 . . ? H92 C9 H93 109.3 . . ? C7 C10 H101 109.7 . . ? C7 C10 H102 109.7 . . ? H101 C10 H102 109.4 . . ? C7 C10 H103 109.0 . . ? H101 C10 H103 109.5 . . ? H102 C10 H103 109.4 . . ? C16 C11 C12 114.0(6) . . ? C16 C11 P 118.9(5) . . ? C12 C11 P 126.3(5) . . ? C11 C12 C13 120.5(7) . . ? C11 C12 H12 119.4 . . ? C13 C12 H12 120.1 . . ? C14 C13 C12 121.9(7) . . ? C14 C13 H13 119.1 . . ? C12 C13 H13 119.0 . . ? C15 C14 C13 117.0(7) . . ? C15 C14 H14 121.6 . . ? C13 C14 H14 121.4 . . ? C14 C15 C16 121.9(8) . . ? C14 C15 H15 119.2 . . ? C16 C15 H15 118.9 . . ? C11 C16 C15 123.8(8) . . ? C11 C16 H16 117.9 . . ? C15 C16 H16 118.2 . . ? C22 C21 C26 116.8(5) . . ? C22 C21 P 124.6(4) . . ? C26 C21 P 118.6(4) . . ? C23 C22 C21 122.2(6) . . ? C23 C22 H22 118.6 . . ? C21 C22 H22 119.2 . . ? C24 C23 C22 120.3(6) . . ? C24 C23 H23 119.8 . . ? C22 C23 H23 119.9 . . ? C23 C24 C25 120.4(6) . . ? C23 C24 H24 119.5 . . ? C25 C24 H24 120.1 . . ? C24 C25 C26 119.9(6) . . ? C24 C25 H25 119.8 . . ? C26 C25 H25 120.3 . . ? C25 C26 C21 120.3(6) . . ? C25 C26 H26 119.7 . . ? C21 C26 H26 119.9 . . ? 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 C6 N1 C2 C3 58.8(5) . . . . ? C7 N1 C2 C3 -171.8(4) . . . . ? C9 N4 C3 C2 -175.9(3) . . . . ? C5 N4 C3 C2 55.8(4) . . . . ? N1 C2 C3 N4 -57.3(5) . . . . ? C9 N4 C5 C6 175.9(4) . . . . ? C3 N4 C5 C6 -55.6(5) . . . . ? C2 N1 C6 C5 -60.7(4) . . . . ? C7 N1 C6 C5 172.6(3) . . . . ? N4 C5 C6 N1 58.8(5) . . . . ? C6 N1 C7 C10 54.5(6) . . . . ? C2 N1 C7 C10 -71.4(6) . . . . ? C6 N1 C7 C8 -71.8(6) . . . . ? C2 N1 C7 C8 162.3(5) . . . . ? N1 C7 C8 P -54.4(6) . . . . ? C10 C7 C8 P 176.4(5) . . . . ? C21 P C8 C7 102.0(5) . . . . ? C11 P C8 C7 -153.6(4) . . . . ? C21 P C11 C16 -173.3(7) . . . . ? C8 P C11 C16 79.6(7) . . . . ? C21 P C11 C12 -4.7(8) . . . . ? C8 P C11 C12 -111.8(7) . . . . ? C16 C11 C12 C13 -10.8(13) . . . . ? P C11 C12 C13 -180.0(7) . . . . ? C11 C12 C13 C14 5.2(16) . . . . ? C12 C13 C14 C15 3.8(17) . . . . ? C13 C14 C15 C16 -6.3(18) . . . . ? C12 C11 C16 C15 8.6(14) . . . . ? P C11 C16 C15 178.6(9) . . . . ? C14 C15 C16 C11 -0.1(19) . . . . ? C8 P C21 C22 41.8(5) . . . . ? C11 P C21 C22 -60.8(5) . . . . ? C8 P C21 C26 -139.9(4) . . . . ? C11 P C21 C26 117.5(4) . . . . ? C26 C21 C22 C23 -2.3(7) . . . . ? P C21 C22 C23 175.9(4) . . . . ? C21 C22 C23 C24 0.2(9) . . . . ? C22 C23 C24 C25 1.0(9) . . . . ? C23 C24 C25 C26 0.1(10) . . . . ? C24 C25 C26 C21 -2.3(9) . . . . ? C22 C21 C26 C25 3.4(8) . . . . ? P C21 C26 C25 -175.0(4) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N4 H4N Cl 0.83(4) 2.19(4) 3.002(4) 168(4) . _diffrn_measured_fraction_theta_max 0.933 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.416 _refine_diff_density_min -0.300 _refine_diff_density_rms 0.057 #===================================END data_(6b) _database_code_depnum_ccdc_archive 'CCDC 605823' _audit_creation_method SHELXL-97 _chemical_name_systematic ; 1-(2-diphenylphosphino-ethyl)-4-methyl-piperazine palladium dichloride ; _chemical_name_common ;1-(2-diphenylphosphino-ethyl)-4-methyl-piperazine palladium dichloride ; _chemical_melting_point ? _chemical_formula_moiety 'C19 H25 Cl2 N2 P Pd' _chemical_formula_sum 'C19 H25 Cl2 N2 P Pd' _chemical_formula_weight 489.68 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.938(1) _cell_length_b 9.597(1) _cell_length_c 13.675(1) _cell_angle_alpha 75.08(1) _cell_angle_beta 80.52(1) _cell_angle_gamma 88.71(1) _cell_volume 992.7(2) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 5771 _cell_measurement_theta_min 2.2 _cell_measurement_theta_max 30.0 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.638 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 496 _exptl_absorpt_coefficient_mu 1.289 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ;The data collection nominally covered full sphere of reciprocal space, by a combination of 3 sets of \w scans; each set at different \f angles and each scan (20 sec exposure) covering 0.3\% in \w. Crystal to detector distance 4.83 cm. ; _diffrn_ambient_temperature 120(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 'Bruker SMART 6K CCD area detector' _diffrn_measurement_method '\W scans' _diffrn_detector_area_resol_mean 5.6 _diffrn_standards_number 0 _diffrn_reflns_number 16957 _diffrn_reflns_av_R_equivalents 0.0469 _diffrn_reflns_av_sigmaI/netI 0.0459 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.56 _diffrn_reflns_theta_max 29.99 _reflns_number_total 5768 _reflns_number_gt 4813 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'SMART version 5.625 (Bruker, 2001)' _computing_cell_refinement 'SMART version 5.625 (Bruker, 2001)' _computing_data_reduction 'SAINT version 6.02A (Bruker, 2001)' _computing_structure_solution 'SHELXTL version 6.12 (Bruker, 2001)' _computing_structure_refinement 'SHELXTL version 6.12 (Bruker, 2001)' _computing_molecular_graphics 'SHELXTL version 6.12 (Bruker, 2001)' _computing_publication_material 'SHELXTL version 6.12 (Bruker, 2001)' _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. ; _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^)+(0.0255P)^2^] 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 5768 _refine_ls_number_parameters 228 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0367 _refine_ls_R_factor_gt 0.0272 _refine_ls_wR_factor_ref 0.0614 _refine_ls_wR_factor_gt 0.0586 _refine_ls_goodness_of_fit_ref 0.992 _refine_ls_restrained_S_all 0.992 _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 Pd Pd 0.525484(18) 0.703226(16) 0.307575(11) 0.01427(5) Uani 1 1 d . . . Cl1 Cl 0.31374(6) 0.78289(6) 0.42595(4) 0.02189(11) Uani 1 1 d . . . Cl2 Cl 0.32886(6) 0.68479(6) 0.20458(4) 0.02063(10) Uani 1 1 d . . . P P 0.71461(6) 0.61020(5) 0.20656(4) 0.01467(10) Uani 1 1 d . . . N1 N 0.72746(19) 0.72180(17) 0.38747(12) 0.0134(3) Uani 1 1 d . . . N4 N 0.7920(2) 0.77449(19) 0.57888(13) 0.0207(4) Uani 1 1 d . . . C2 C 0.6968(2) 0.6111(2) 0.48817(15) 0.0163(4) Uani 1 1 d . . . H2A H 0.7148 0.5142 0.4758 0.021 Uiso 1 1 d R . . H2B H 0.5762 0.6153 0.5204 0.021 Uiso 1 1 d R . . C3 C 0.8120(3) 0.6306(2) 0.56217(16) 0.0203(4) Uani 1 1 d . . . H3A H 0.7820 0.5571 0.6283 0.026 Uiso 1 1 d R . . H3B H 0.9326 0.6172 0.5337 0.026 Uiso 1 1 d R . . C5 C 0.8418(3) 0.8822(2) 0.48212(16) 0.0200(4) Uani 1 1 d . . . H5A H 0.9616 0.8676 0.4529 0.026 Uiso 1 1 d R . . H5B H 0.8338 0.9800 0.4937 0.026 Uiso 1 1 d R . . C6 C 0.7243(2) 0.8683(2) 0.40756(15) 0.0169(4) Uani 1 1 d . . . H6A H 0.6059 0.8885 0.4359 0.022 Uiso 1 1 d R . . H6B H 0.7586 0.9417 0.3418 0.022 Uiso 1 1 d R . . C7 C 0.8982(2) 0.7017(2) 0.32594(15) 0.0173(4) Uani 1 1 d . . . H7A H 0.9860 0.6842 0.3712 0.023 Uiso 1 1 d R . . H7B H 0.9315 0.7908 0.2710 0.023 Uiso 1 1 d R . . C8 C 0.8917(2) 0.5755(2) 0.27854(15) 0.0179(4) Uani 1 1 d . . . H8A H 0.8722 0.4835 0.3325 0.023 Uiso 1 1 d R . . H8B H 1.0002 0.5699 0.2323 0.023 Uiso 1 1 d R . . C9 C 0.8864(3) 0.7934(3) 0.65751(18) 0.0294(5) Uani 1 1 d . . . H9A H 0.8491 0.7194 0.7215 0.031(4) Uiso 1 1 d R . . H9B H 0.8647 0.8893 0.6692 0.031(4) Uiso 1 1 d R . . H9C H 1.0089 0.7843 0.6348 0.031(4) Uiso 1 1 d R . . C11 C 0.6535(2) 0.4409(2) 0.18600(15) 0.0172(4) Uani 1 1 d . . . C12 C 0.6340(3) 0.4264(2) 0.08970(16) 0.0227(4) Uani 1 1 d . . . H12 H 0.6623 0.5049 0.0307 0.027 Uiso 1 1 d R . . C13 C 0.5726(3) 0.2970(3) 0.08023(19) 0.0286(5) Uani 1 1 d . . . H13 H 0.5603 0.2866 0.0145 0.034 Uiso 1 1 d R . . C14 C 0.5294(3) 0.1830(2) 0.16618(19) 0.0281(5) Uani 1 1 d . . . H14 H 0.4867 0.0950 0.1592 0.034 Uiso 1 1 d R . . C15 C 0.5481(3) 0.1964(2) 0.26215(18) 0.0250(5) Uani 1 1 d . . . H15 H 0.5176 0.1181 0.3210 0.030 Uiso 1 1 d R . . C16 C 0.6114(3) 0.3254(2) 0.27225(16) 0.0206(4) Uani 1 1 d . . . H16 H 0.6259 0.3346 0.3379 0.025 Uiso 1 1 d R . . C21 C 0.7938(3) 0.7332(2) 0.08412(15) 0.0175(4) Uani 1 1 d . . . C22 C 0.9322(3) 0.6985(2) 0.01805(17) 0.0249(5) Uani 1 1 d . . . H22 H 0.9883 0.6096 0.0379 0.030 Uiso 1 1 d R . . C23 C 0.9882(3) 0.7935(3) -0.07702(18) 0.0305(5) Uani 1 1 d . . . H23 H 1.0813 0.7691 -0.1225 0.037 Uiso 1 1 d R . . C24 C 0.9080(3) 0.9238(3) -0.10505(17) 0.0292(5) Uani 1 1 d . . . H24 H 0.9456 0.9883 -0.1702 0.035 Uiso 1 1 d R . . C25 C 0.7739(3) 0.9608(2) -0.03895(17) 0.0262(5) Uani 1 1 d . . . H25 H 0.7215 1.0517 -0.0580 0.031 Uiso 1 1 d R . . C26 C 0.7156(3) 0.8657(2) 0.05476(16) 0.0209(4) Uani 1 1 d . . . H26 H 0.6218 0.8905 0.0995 0.025 Uiso 1 1 d 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 Pd 0.01146(7) 0.01600(8) 0.01556(7) -0.00416(5) -0.00294(5) 0.00181(5) Cl1 0.0146(2) 0.0257(3) 0.0276(3) -0.0125(2) -0.00148(19) 0.00352(19) Cl2 0.0145(2) 0.0272(3) 0.0200(2) -0.0035(2) -0.00628(18) 0.00036(18) P 0.0132(2) 0.0165(2) 0.0151(2) -0.00500(19) -0.00334(18) 0.00232(18) N1 0.0113(7) 0.0118(8) 0.0173(8) -0.0042(6) -0.0025(6) 0.0002(6) N4 0.0208(9) 0.0246(9) 0.0196(8) -0.0089(7) -0.0069(7) 0.0009(7) C2 0.0152(9) 0.0157(9) 0.0169(9) -0.0022(7) -0.0018(7) -0.0018(7) C3 0.0211(10) 0.0210(10) 0.0188(10) -0.0036(8) -0.0058(8) -0.0009(8) C5 0.0172(10) 0.0188(10) 0.0266(11) -0.0101(8) -0.0042(8) 0.0004(8) C6 0.0165(9) 0.0131(9) 0.0217(10) -0.0050(8) -0.0044(8) 0.0004(7) C7 0.0128(9) 0.0207(10) 0.0187(9) -0.0055(8) -0.0024(7) -0.0008(7) C8 0.0137(9) 0.0233(10) 0.0183(9) -0.0071(8) -0.0047(7) 0.0040(8) C9 0.0308(13) 0.0375(14) 0.0257(12) -0.0144(10) -0.0112(10) -0.0001(10) C11 0.0148(9) 0.0173(10) 0.0211(10) -0.0068(8) -0.0052(8) 0.0037(7) C12 0.0248(11) 0.0240(11) 0.0206(10) -0.0053(8) -0.0086(9) 0.0047(9) C13 0.0325(12) 0.0309(13) 0.0301(12) -0.0164(10) -0.0146(10) 0.0063(10) C14 0.0226(11) 0.0224(11) 0.0439(14) -0.0151(10) -0.0083(10) 0.0010(9) C15 0.0209(11) 0.0185(11) 0.0330(12) -0.0050(9) 0.0001(9) 0.0036(8) C16 0.0197(10) 0.0217(11) 0.0204(10) -0.0071(8) -0.0009(8) 0.0033(8) C21 0.0171(9) 0.0193(10) 0.0159(9) -0.0040(8) -0.0028(7) -0.0022(7) C22 0.0238(11) 0.0258(12) 0.0234(11) -0.0057(9) -0.0002(9) 0.0038(9) C23 0.0267(12) 0.0372(14) 0.0243(11) -0.0064(10) 0.0037(9) -0.0038(10) C24 0.0329(13) 0.0301(13) 0.0206(11) 0.0005(9) -0.0030(9) -0.0117(10) C25 0.0304(12) 0.0194(11) 0.0276(11) -0.0004(9) -0.0099(10) -0.0041(9) C26 0.0218(10) 0.0184(10) 0.0226(10) -0.0054(8) -0.0033(8) -0.0011(8) _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 Pd N1 2.1181(16) . ? Pd P 2.2024(6) . ? Pd Cl2 2.3056(5) . ? Pd Cl1 2.3903(6) . ? P C21 1.806(2) . ? P C11 1.808(2) . ? P C8 1.8226(19) . ? N1 C2 1.494(2) . ? N1 C6 1.499(2) . ? N1 C7 1.509(2) . ? N4 C5 1.455(3) . ? N4 C9 1.457(3) . ? N4 C3 1.458(3) . ? C2 C3 1.518(3) . ? C5 C6 1.522(3) . ? C7 C8 1.519(3) . ? C11 C12 1.393(3) . ? C11 C16 1.395(3) . ? C12 C13 1.389(3) . ? C13 C14 1.385(3) . ? C14 C15 1.383(3) . ? C15 C16 1.394(3) . ? C21 C22 1.395(3) . ? C21 C26 1.396(3) . ? C22 C23 1.391(3) . ? C23 C24 1.384(3) . ? C24 C25 1.382(3) . ? C25 C26 1.383(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Pd P 86.27(4) . . ? N1 Pd Cl2 173.55(5) . . ? P Pd Cl2 87.98(2) . . ? N1 Pd Cl1 94.02(4) . . ? P Pd Cl1 174.94(2) . . ? Cl2 Pd Cl1 91.97(2) . . ? C21 P C11 109.08(9) . . ? C21 P C8 107.10(9) . . ? C11 P C8 107.59(9) . . ? C21 P Pd 114.33(7) . . ? C11 P Pd 116.06(7) . . ? C8 P Pd 101.86(6) . . ? C2 N1 C6 108.48(14) . . ? C2 N1 C7 111.09(14) . . ? C6 N1 C7 109.29(15) . . ? C2 N1 Pd 107.85(11) . . ? C6 N1 Pd 109.05(11) . . ? C7 N1 Pd 111.01(11) . . ? C5 N4 C9 111.84(17) . . ? C5 N4 C3 109.58(16) . . ? C9 N4 C3 111.91(17) . . ? N1 C2 C3 113.54(16) . . ? N4 C3 C2 109.81(16) . . ? N4 C5 C6 109.25(16) . . ? N1 C6 C5 112.96(15) . . ? N1 C7 C8 111.23(15) . . ? C7 C8 P 105.81(13) . . ? C12 C11 C16 119.79(19) . . ? C12 C11 P 122.48(16) . . ? C16 C11 P 117.50(15) . . ? C13 C12 C11 119.8(2) . . ? C14 C13 C12 120.3(2) . . ? C15 C14 C13 120.4(2) . . ? C14 C15 C16 119.7(2) . . ? C15 C16 C11 120.04(19) . . ? C22 C21 C26 119.15(19) . . ? C22 C21 P 121.29(16) . . ? C26 C21 P 119.56(15) . . ? C23 C22 C21 120.2(2) . . ? C24 C23 C22 119.7(2) . . ? C25 C24 C23 120.5(2) . . ? C24 C25 C26 120.0(2) . . ? C25 C26 C21 120.4(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Pd P C21 -102.32(8) . . . . ? Cl2 Pd P C21 74.76(7) . . . . ? N1 Pd P C11 129.32(8) . . . . ? Cl2 Pd P C11 -53.59(7) . . . . ? N1 Pd P C8 12.81(8) . . . . ? Cl2 Pd P C8 -170.11(7) . . . . ? P Pd N1 C2 -107.85(11) . . . . ? Cl1 Pd N1 C2 67.08(11) . . . . ? P Pd N1 C6 134.53(12) . . . . ? Cl1 Pd N1 C6 -50.53(12) . . . . ? P Pd N1 C7 14.06(11) . . . . ? Cl1 Pd N1 C7 -171.00(11) . . . . ? C6 N1 C2 C3 -50.8(2) . . . . ? C7 N1 C2 C3 69.35(19) . . . . ? Pd N1 C2 C3 -168.78(13) . . . . ? C5 N4 C3 C2 -61.3(2) . . . . ? C9 N4 C3 C2 174.03(17) . . . . ? N1 C2 C3 N4 56.7(2) . . . . ? C9 N4 C5 C6 -173.13(16) . . . . ? C3 N4 C5 C6 62.2(2) . . . . ? C2 N1 C6 C5 51.6(2) . . . . ? C7 N1 C6 C5 -69.6(2) . . . . ? Pd N1 C6 C5 168.86(13) . . . . ? N4 C5 C6 N1 -58.5(2) . . . . ? C2 N1 C7 C8 76.16(19) . . . . ? C6 N1 C7 C8 -164.18(15) . . . . ? Pd N1 C7 C8 -43.85(18) . . . . ? N1 C7 C8 P 54.16(18) . . . . ? C21 P C8 C7 82.21(15) . . . . ? C11 P C8 C7 -160.64(13) . . . . ? Pd P C8 C7 -38.13(14) . . . . ? C21 P C11 C12 -14.1(2) . . . . ? C8 P C11 C12 -129.97(17) . . . . ? Pd P C11 C12 116.77(16) . . . . ? C21 P C11 C16 171.32(15) . . . . ? C8 P C11 C16 55.47(18) . . . . ? Pd P C11 C16 -57.80(16) . . . . ? C16 C11 C12 C13 0.0(3) . . . . ? P C11 C12 C13 -174.44(16) . . . . ? P C11 C16 C15 174.00(16) . . . . ? C11 P C21 C22 -58.09(19) . . . . ? C8 P C21 C22 58.08(19) . . . . ? Pd P C21 C22 170.11(15) . . . . ? C11 P C21 C26 121.99(16) . . . . ? C8 P C21 C26 -121.84(16) . . . . ? Pd P C21 C26 -9.81(18) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 29.99 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.843 _refine_diff_density_min -0.668 _refine_diff_density_rms 0.090 #===================================END data_(10) _database_code_depnum_ccdc_archive 'CCDC 605824' _audit_creation_method SHELXL-97 _chemical_name_systematic ; P,N,N-{1-(2-diphenylphosphino-ethyl)-4-methyl-piperazine}- chloro-palladium tetraaqua-bis(sulfato)magnesium hexahydrate ; _chemical_name_common ; P,N,N-(1-(2-diphenylphosphino-ethyl)-4-methyl-piperazine)- chloro-palladium tetraaqua-bis(sulfato)magnesium hexahydrate ; _chemical_melting_point ? _chemical_formula_moiety '2(C19 H25 Cl N2 P Pd 1+),H8 Mg O12 S2 2-,6(H2 O)' _chemical_formula_sum 'C38 H70 Cl2 Mg N4 O18 P2 Pd2 S2' _chemical_formula_weight 1305.05 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mg Mg 0.0486 0.0363 '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' S S 0.1246 0.1234 '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 16.9252(17) _cell_length_b 8.6573(9) _cell_length_c 18.0774(18) _cell_angle_alpha 90.00 _cell_angle_beta 92.94(1) _cell_angle_gamma 90.00 _cell_volume 2645.3(5) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 8980 _cell_measurement_theta_min 2.50 _cell_measurement_theta_max 30.01 _exptl_crystal_description fragment _exptl_crystal_colour yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.638 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1340 _exptl_absorpt_coefficient_mu 1.003 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8883 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'SADABS v. 2.10 (Bruker-Nonius, 2003), R(int)=0.060 before correction' _exptl_special_details ;The data collection nominally covered full sphere of reciprocal space, by a combination of 4 sets of \w scans; each set at different \f angles and each scan (10 sec exposure) covering 0.3\% in \w. Crystal to detector distance 4.4 cm. ; _diffrn_ambient_temperature 120(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 'Siemens SMART 1K CCD area detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 8 _diffrn_standards_number 0 _diffrn_reflns_number 30538 _diffrn_reflns_av_R_equivalents 0.0337 _diffrn_reflns_av_sigmaI/netI 0.0273 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.26 _diffrn_reflns_theta_max 29.00 _reflns_number_total 7011 _reflns_number_gt 6194 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'SMART version 5.054 (Bruker, 1999)' _computing_cell_refinement 'SMART version 5.054 (Bruker, 1999)' _computing_data_reduction 'SAINT version 6.45A (Bruker, 2003)' _computing_structure_solution 'SHELXTL version 6.12 (Bruker, 2001)' _computing_structure_refinement 'SHELXTL version 6.12 (Bruker, 2001)' _computing_molecular_graphics 'SHELXTL version 6.12 (Bruker, 2001)' _computing_publication_material 'SHELXTL version 6.12 (Bruker, 2001)' _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. Water H atoms - refall, methyl group - rigid rotating body, other H atoms - riding. ; _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^)+(0.0215P)^2^+1.6515P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7011 _refine_ls_number_parameters 355 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0313 _refine_ls_R_factor_gt 0.0246 _refine_ls_wR_factor_ref 0.0565 _refine_ls_wR_factor_gt 0.0542 _refine_ls_goodness_of_fit_ref 1.070 _refine_ls_restrained_S_all 1.070 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd Pd 0.834214(7) 0.394210(14) 0.280672(7) 0.01183(4) Uani 1 1 d . . . Cl Cl 0.96804(3) 0.35601(5) 0.29418(3) 0.02202(9) Uani 1 1 d . . . P P 0.79580(3) 0.25345(5) 0.37529(2) 0.01282(9) Uani 1 1 d . . . N1 N 0.71926(8) 0.45849(17) 0.26329(8) 0.0139(3) Uani 1 1 d . . . C2 C 0.69648(10) 0.3936(2) 0.18857(9) 0.0159(3) Uani 1 1 d . . . H20 H 0.6454 0.4378 0.1697 0.021 Uiso 1 1 d R . . H21 H 0.6908 0.2800 0.1915 0.021 Uiso 1 1 d R . . C3 C 0.76250(11) 0.4358(2) 0.13699(10) 0.0182(4) Uani 1 1 d . . . H31 H 0.7854 0.3407 0.1165 0.024 Uiso 1 1 d R . . H32 H 0.7405 0.4990 0.0952 0.024 Uiso 1 1 d R . . N4 N 0.82483(8) 0.52443(16) 0.17981(8) 0.0145(3) Uani 1 1 d . . . C5 C 0.78833(11) 0.6708(2) 0.20366(10) 0.0194(4) Uani 1 1 d . . . H51 H 0.7658 0.7276 0.1600 0.025 Uiso 1 1 d R . . H52 H 0.8286 0.7371 0.2295 0.025 Uiso 1 1 d R . . C6 C 0.72285(11) 0.6309(2) 0.25581(10) 0.0182(4) Uani 1 1 d . . . H61 H 0.7343 0.6790 0.3048 0.024 Uiso 1 1 d R . . H62 H 0.6714 0.6708 0.2355 0.024 Uiso 1 1 d R . . C7 C 0.66480(10) 0.4109(2) 0.32180(10) 0.0173(3) Uani 1 1 d . . . H71 H 0.6099 0.4061 0.3003 0.023 Uiso 1 1 d R . . H72 H 0.6667 0.4888 0.3619 0.023 Uiso 1 1 d R . . C8 C 0.68887(10) 0.2541(2) 0.35357(10) 0.0162(3) Uani 1 1 d . . . H81 H 0.6748 0.1720 0.3171 0.021 Uiso 1 1 d R . . H82 H 0.6604 0.2338 0.3990 0.021 Uiso 1 1 d R . . C9 C 0.89346(11) 0.5532(2) 0.13490(11) 0.0216(4) Uani 1 1 d . . . H91 H 0.8764 0.6109 0.0903 0.029(4) Uiso 1 1 d R . . H92 H 0.9165 0.4545 0.1207 0.029(4) Uiso 1 1 d R . . H93 H 0.9331 0.6134 0.1638 0.029(4) Uiso 1 1 d R . . C11 C 0.82332(10) 0.0524(2) 0.38583(9) 0.0147(3) Uani 1 1 d . . . C12 C 0.77900(11) -0.0395(2) 0.43160(10) 0.0185(3) Uani 1 1 d . . . H12 H 0.7348 0.0027 0.4548 0.022 Uiso 1 1 d R . . C13 C 0.79936(12) -0.1935(2) 0.44266(10) 0.0214(4) Uani 1 1 d . . . H13 H 0.7695 -0.2566 0.4738 0.026 Uiso 1 1 d R . . C14 C 0.86368(12) -0.2554(2) 0.40852(11) 0.0223(4) Uani 1 1 d . . . H14 H 0.8779 -0.3602 0.4170 0.027 Uiso 1 1 d R . . C15 C 0.90724(11) -0.1650(2) 0.36235(11) 0.0219(4) Uani 1 1 d . . . H15 H 0.9507 -0.2085 0.3386 0.026 Uiso 1 1 d R . . C16 C 0.88697(11) -0.0106(2) 0.35032(10) 0.0185(3) Uani 1 1 d . . . H16 H 0.9161 0.0510 0.3179 0.022 Uiso 1 1 d R . . C21 C 0.81593(10) 0.33725(19) 0.46606(10) 0.0150(3) Uani 1 1 d . . . C22 C 0.75652(11) 0.3999(2) 0.50730(10) 0.0168(3) Uani 1 1 d . . . H22 H 0.7032 0.3969 0.4883 0.020 Uiso 1 1 d R . . C23 C 0.77539(12) 0.4658(2) 0.57629(11) 0.0215(4) Uani 1 1 d . . . H23 H 0.7348 0.5076 0.6047 0.026 Uiso 1 1 d R . . C24 C 0.85333(12) 0.4696(2) 0.60382(11) 0.0241(4) Uani 1 1 d . . . H24 H 0.8662 0.5153 0.6506 0.029 Uiso 1 1 d R . . C25 C 0.91280(12) 0.4083(2) 0.56279(11) 0.0238(4) Uani 1 1 d . . . H25 H 0.9661 0.4115 0.5818 0.029 Uiso 1 1 d R . . C26 C 0.89471(11) 0.3420(2) 0.49406(11) 0.0197(4) Uani 1 1 d . . . H26 H 0.9354 0.2994 0.4661 0.024 Uiso 1 1 d R . . Mg Mg 0.5000 0.5000 0.5000 0.01136(15) Uani 1 2 d S . . S S 0.46546(3) 0.23330(5) 0.37279(2) 0.01365(8) Uani 1 1 d . . . O1 O 0.51324(7) 0.35065(14) 0.41367(7) 0.0141(2) Uani 1 1 d . . . O2 O 0.46807(8) 0.26465(14) 0.29252(7) 0.0178(3) Uani 1 1 d . . . O3 O 0.49934(10) 0.07958(15) 0.38882(8) 0.0276(3) Uani 1 1 d . . . O4 O 0.38322(8) 0.23773(19) 0.39494(8) 0.0303(3) Uani 1 1 d . . . O5 O 0.40018(8) 0.37640(15) 0.53106(8) 0.0154(2) Uani 1 1 d . . . H051 H 0.4056(14) 0.318(3) 0.5628(14) 0.027(7) Uiso 1 1 d . . . H052 H 0.3860(17) 0.340(3) 0.4963(17) 0.044(9) Uiso 1 1 d . . . O6 O 0.57448(8) 0.36658(15) 0.56645(8) 0.0163(3) Uani 1 1 d . . . H061 H 0.5838(15) 0.284(3) 0.5548(14) 0.033(7) Uiso 1 1 d . . . H062 H 0.5733(16) 0.368(3) 0.6101(17) 0.040(8) Uiso 1 1 d . . . O7 O 0.57632(9) 0.41047(17) 0.71515(8) 0.0209(3) Uani 1 1 d . . . H071 H 0.5668(15) 0.495(3) 0.7159(14) 0.035(7) Uiso 1 1 d . . . H072 H 0.5436(17) 0.367(3) 0.7378(16) 0.042(8) Uiso 1 1 d . . . O8 O 0.60672(8) 0.07821(16) 0.51312(8) 0.0192(3) Uani 1 1 d . . . H081 H 0.5932(17) 0.025(4) 0.5398(17) 0.047(9) Uiso 1 1 d . . . H082 H 0.5763(17) 0.075(3) 0.4750(17) 0.042(8) Uiso 1 1 d . . . O9 O 0.40859(9) 0.17400(18) 0.64557(8) 0.0245(3) Uani 1 1 d . . . H091 H 0.4205(16) 0.199(3) 0.6842(16) 0.036(8) Uiso 1 1 d . . . H092 H 0.4373(18) 0.102(4) 0.6399(17) 0.049(9) Uiso 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 Pd 0.01044(6) 0.01265(6) 0.01235(6) 0.00231(5) 0.00025(4) 0.00059(4) Cl 0.01163(19) 0.0266(2) 0.0278(2) 0.00801(18) 0.00121(16) 0.00148(16) P 0.0113(2) 0.01404(19) 0.0131(2) 0.00254(16) 0.00051(15) 0.00090(15) N1 0.0127(7) 0.0158(7) 0.0128(7) 0.0008(5) -0.0010(5) 0.0014(5) C2 0.0149(8) 0.0192(8) 0.0133(8) 0.0001(6) -0.0012(6) -0.0031(6) C3 0.0198(9) 0.0210(9) 0.0138(8) -0.0015(7) 0.0006(7) -0.0060(7) N4 0.0146(7) 0.0144(7) 0.0144(7) 0.0015(5) -0.0007(5) -0.0023(5) C5 0.0234(9) 0.0128(8) 0.0218(9) 0.0022(7) -0.0023(7) -0.0005(7) C6 0.0214(9) 0.0139(8) 0.0189(9) -0.0002(6) -0.0025(7) 0.0047(6) C7 0.0127(8) 0.0241(9) 0.0154(8) 0.0031(7) 0.0019(6) 0.0043(7) C8 0.0119(8) 0.0213(8) 0.0153(8) 0.0030(7) 0.0002(6) 0.0000(6) C9 0.0184(9) 0.0261(9) 0.0203(9) 0.0057(7) 0.0018(7) -0.0052(7) C11 0.0148(8) 0.0152(8) 0.0139(8) 0.0007(6) -0.0012(6) 0.0005(6) C12 0.0197(9) 0.0201(9) 0.0158(8) 0.0018(7) 0.0030(7) -0.0004(7) C13 0.0258(10) 0.0183(9) 0.0200(9) 0.0055(7) 0.0005(7) -0.0035(7) C14 0.0263(10) 0.0136(8) 0.0264(10) 0.0020(7) -0.0054(8) 0.0005(7) C15 0.0192(9) 0.0188(9) 0.0279(10) -0.0019(7) 0.0023(7) 0.0029(7) C16 0.0167(8) 0.0177(8) 0.0213(9) 0.0018(7) 0.0024(7) -0.0007(7) C21 0.0178(8) 0.0120(7) 0.0149(8) 0.0032(6) -0.0008(6) 0.0004(6) C22 0.0167(8) 0.0147(8) 0.0189(8) 0.0021(7) 0.0006(6) 0.0024(6) C23 0.0258(10) 0.0168(8) 0.0222(9) -0.0034(7) 0.0033(7) 0.0032(7) C24 0.0315(11) 0.0184(9) 0.0218(9) -0.0039(7) -0.0047(8) 0.0014(8) C25 0.0201(9) 0.0227(9) 0.0278(10) -0.0029(8) -0.0071(8) 0.0005(7) C26 0.0158(9) 0.0201(8) 0.0229(9) -0.0004(7) -0.0006(7) 0.0025(7) Mg 0.0119(4) 0.0118(4) 0.0104(4) -0.0009(3) 0.0005(3) 0.0004(3) S 0.0171(2) 0.01411(19) 0.00971(18) -0.00173(14) 0.00042(15) -0.00257(15) O1 0.0142(6) 0.0152(6) 0.0130(6) -0.0034(4) 0.0010(4) -0.0017(4) O2 0.0246(7) 0.0192(6) 0.0096(6) -0.0009(5) -0.0010(5) 0.0002(5) O3 0.0510(10) 0.0127(6) 0.0183(7) 0.0001(5) -0.0051(6) 0.0033(6) O4 0.0176(7) 0.0518(10) 0.0218(7) -0.0157(7) 0.0055(5) -0.0145(6) O5 0.0179(6) 0.0158(6) 0.0124(6) 0.0005(5) 0.0014(5) -0.0015(5) O6 0.0210(7) 0.0151(6) 0.0125(6) 0.0001(5) -0.0002(5) 0.0039(5) O7 0.0304(8) 0.0160(7) 0.0164(6) 0.0012(5) 0.0035(5) 0.0034(6) O8 0.0226(7) 0.0175(7) 0.0174(7) 0.0030(5) 0.0002(6) -0.0016(5) O9 0.0363(9) 0.0220(7) 0.0150(7) 0.0004(6) -0.0023(6) 0.0040(6) _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 Pd N1 2.0325(14) . ? Pd N4 2.1426(14) . ? Pd P 2.2243(5) . ? Pd Cl 2.2897(5) . ? P C11 1.8089(18) . ? P C21 1.8103(18) . ? P C8 1.8322(17) . ? N1 C2 1.495(2) . ? N1 C7 1.496(2) . ? N1 C6 1.500(2) . ? C2 C3 1.536(2) . ? C2 H20 0.9893 . ? C2 H21 0.9895 . ? C3 N4 1.489(2) . ? C3 H31 0.9895 . ? C3 H32 0.9895 . ? N4 C9 1.472(2) . ? N4 C5 1.483(2) . ? C5 C6 1.531(3) . ? C5 H51 0.9894 . ? C5 H52 0.9893 . ? C6 H61 0.9894 . ? C6 H62 0.9892 . ? C7 C8 1.522(2) . ? C7 H71 0.9894 . ? C7 H72 0.9893 . ? C8 H81 0.9894 . ? C8 H82 0.9892 . ? C9 H91 0.9795 . ? C9 H92 0.9795 . ? C9 H93 0.9794 . ? C11 C16 1.393(2) . ? C11 C12 1.394(2) . ? C12 C13 1.389(3) . ? C12 H12 0.9492 . ? C13 C14 1.386(3) . ? C13 H13 0.9494 . ? C14 C15 1.384(3) . ? C14 H14 0.9495 . ? C15 C16 1.394(3) . ? C15 H15 0.9493 . ? C16 H16 0.9493 . ? C21 C22 1.392(2) . ? C21 C26 1.402(2) . ? C22 C23 1.394(3) . ? C22 H22 0.9493 . ? C23 C24 1.386(3) . ? C23 H23 0.9493 . ? C24 C25 1.386(3) . ? C24 H24 0.9494 . ? C25 C26 1.389(3) . ? C25 H25 0.9493 . ? C26 H26 0.9493 . ? Mg O1 2.0478(12) 3_666 ? Mg O1 2.0478(12) . ? Mg O6 2.0520(13) 3_666 ? Mg O6 2.0520(13) . ? Mg O5 2.1004(13) . ? Mg O5 2.1005(13) 3_666 ? S O4 1.4685(14) . ? S O3 1.4720(14) . ? S O1 1.4733(12) . ? S O2 1.4792(13) . ? O5 H051 0.77(3) . ? O5 H052 0.73(3) . ? O6 H061 0.77(3) . ? O6 H062 0.79(3) . ? O7 H071 0.75(3) . ? O7 H072 0.80(3) . ? O8 H081 0.71(3) . ? O8 H082 0.84(3) . ? O9 H091 0.75(3) . ? O9 H092 0.80(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Pd N4 72.29(6) . . ? N1 Pd P 87.35(4) . . ? N4 Pd P 158.57(4) . . ? N1 Pd Cl 171.85(4) . . ? N4 Pd Cl 101.33(4) . . ? P Pd Cl 99.520(18) . . ? C11 P C21 104.75(8) . . ? C11 P C8 105.76(8) . . ? C21 P C8 109.33(8) . . ? C11 P Pd 121.61(6) . . ? C21 P Pd 115.38(6) . . ? C8 P Pd 99.09(6) . . ? C2 N1 C7 113.29(13) . . ? C2 N1 C6 107.60(13) . . ? C7 N1 C6 111.53(14) . . ? C2 N1 Pd 103.73(10) . . ? C7 N1 Pd 115.78(10) . . ? C6 N1 Pd 104.09(10) . . ? N1 C2 C3 107.28(13) . . ? N1 C2 H20 110.2 . . ? C3 C2 H20 110.4 . . ? N1 C2 H21 110.2 . . ? C3 C2 H21 110.2 . . ? H20 C2 H21 108.5 . . ? N4 C3 C2 108.97(14) . . ? N4 C3 H31 110.1 . . ? C2 C3 H31 109.9 . . ? N4 C3 H32 109.9 . . ? C2 C3 H32 109.7 . . ? H31 C3 H32 108.3 . . ? C9 N4 C5 111.58(14) . . ? C9 N4 C3 111.01(14) . . ? C5 N4 C3 107.27(14) . . ? C9 N4 Pd 122.16(11) . . ? C5 N4 Pd 102.46(10) . . ? C3 N4 Pd 101.00(10) . . ? N4 C5 C6 108.18(14) . . ? N4 C5 H51 110.0 . . ? C6 C5 H51 109.9 . . ? N4 C5 H52 110.3 . . ? C6 C5 H52 110.0 . . ? H51 C5 H52 108.4 . . ? N1 C6 C5 108.29(14) . . ? N1 C6 H61 110.2 . . ? C5 C6 H61 110.0 . . ? N1 C6 H62 110.0 . . ? C5 C6 H62 110.1 . . ? H61 C6 H62 108.4 . . ? N1 C7 C8 110.47(14) . . ? N1 C7 H71 109.6 . . ? C8 C7 H71 109.8 . . ? N1 C7 H72 109.4 . . ? C8 C7 H72 109.5 . . ? H71 C7 H72 108.1 . . ? C7 C8 P 109.03(12) . . ? C7 C8 H81 109.8 . . ? P C8 H81 110.0 . . ? C7 C8 H82 109.9 . . ? P C8 H82 109.8 . . ? H81 C8 H82 108.3 . . ? N4 C9 H91 109.5 . . ? N4 C9 H92 109.4 . . ? H91 C9 H92 109.5 . . ? N4 C9 H93 109.5 . . ? H91 C9 H93 109.5 . . ? H92 C9 H93 109.5 . . ? C16 C11 C12 120.12(16) . . ? C16 C11 P 121.96(13) . . ? C12 C11 P 117.91(13) . . ? C13 C12 C11 119.75(17) . . ? C13 C12 H12 120.1 . . ? C11 C12 H12 120.2 . . ? C14 C13 C12 120.12(18) . . ? C14 C13 H13 119.7 . . ? C12 C13 H13 120.1 . . ? C15 C14 C13 120.30(17) . . ? C15 C14 H14 119.9 . . ? C13 C14 H14 119.8 . . ? C14 C15 C16 120.11(18) . . ? C14 C15 H15 119.9 . . ? C16 C15 H15 120.0 . . ? C11 C16 C15 119.58(17) . . ? C11 C16 H16 120.2 . . ? C15 C16 H16 120.2 . . ? C22 C21 C26 119.66(16) . . ? C22 C21 P 122.28(13) . . ? C26 C21 P 118.04(14) . . ? C21 C22 C23 120.01(17) . . ? C21 C22 H22 119.7 . . ? C23 C22 H22 120.3 . . ? C24 C23 C22 120.07(18) . . ? C24 C23 H23 119.9 . . ? C22 C23 H23 120.0 . . ? C25 C24 C23 120.18(18) . . ? C25 C24 H24 119.7 . . ? C23 C24 H24 120.1 . . ? C24 C25 C26 120.28(18) . . ? C24 C25 H25 119.9 . . ? C26 C25 H25 119.8 . . ? C25 C26 C21 119.81(17) . . ? C25 C26 H26 120.3 . . ? C21 C26 H26 119.9 . . ? O1 Mg O1 180.0 3_666 . ? O1 Mg O6 90.16(5) 3_666 3_666 ? O1 Mg O6 89.84(5) . 3_666 ? O1 Mg O6 89.84(5) 3_666 . ? O1 Mg O6 90.16(5) . . ? O6 Mg O6 180.0 3_666 . ? O1 Mg O5 89.83(5) 3_666 . ? O1 Mg O5 90.17(5) . . ? O6 Mg O5 87.99(5) 3_666 . ? O6 Mg O5 92.02(5) . . ? O1 Mg O5 90.17(5) 3_666 3_666 ? O1 Mg O5 89.83(5) . 3_666 ? O6 Mg O5 92.01(5) 3_666 3_666 ? O6 Mg O5 87.99(5) . 3_666 ? O5 Mg O5 180.0 . 3_666 ? O4 S O3 109.57(10) . . ? O4 S O1 110.41(8) . . ? O3 S O1 109.05(8) . . ? O4 S O2 109.82(8) . . ? O3 S O2 109.16(8) . . ? O1 S O2 108.80(7) . . ? S O1 Mg 137.64(8) . . ? Mg O5 H051 118.0(18) . . ? Mg O5 H052 103(2) . . ? H051 O5 H052 112(3) . . ? Mg O6 H061 119.6(19) . . ? Mg O6 H062 122(2) . . ? H061 O6 H062 108(3) . . ? H071 O7 H072 107(3) . . ? H081 O8 H082 109(3) . . ? H091 O9 H092 102(3) . . ? 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 N1 Pd P C11 129.68(8) . . . . ? N4 Pd P C11 111.73(13) . . . . ? Cl Pd P C11 -54.75(7) . . . . ? N1 Pd P C21 -101.79(8) . . . . ? N4 Pd P C21 -119.73(13) . . . . ? Cl Pd P C21 73.79(7) . . . . ? N1 Pd P C8 14.76(7) . . . . ? N4 Pd P C8 -3.19(13) . . . . ? Cl Pd P C8 -169.67(6) . . . . ? N4 Pd N1 C2 57.06(10) . . . . ? P Pd N1 C2 -116.15(10) . . . . ? N4 Pd N1 C7 -178.19(13) . . . . ? P Pd N1 C7 8.60(11) . . . . ? N4 Pd N1 C6 -55.41(10) . . . . ? P Pd N1 C6 131.38(10) . . . . ? C7 N1 C2 C3 -173.38(14) . . . . ? C6 N1 C2 C3 62.86(17) . . . . ? Pd N1 C2 C3 -47.04(15) . . . . ? N1 C2 C3 N4 0.29(19) . . . . ? C2 C3 N4 C9 173.93(15) . . . . ? C2 C3 N4 C5 -63.93(17) . . . . ? C2 C3 N4 Pd 42.97(15) . . . . ? N1 Pd N4 C9 -179.23(15) . . . . ? P Pd N4 C9 -160.38(11) . . . . ? Cl Pd N4 C9 6.02(14) . . . . ? N1 Pd N4 C5 55.04(10) . . . . ? P Pd N4 C5 73.89(15) . . . . ? Cl Pd N4 C5 -119.71(10) . . . . ? N1 Pd N4 C3 -55.61(11) . . . . ? P Pd N4 C3 -36.76(18) . . . . ? Cl Pd N4 C3 129.64(10) . . . . ? C9 N4 C5 C6 -174.70(14) . . . . ? C3 N4 C5 C6 63.51(17) . . . . ? Pd N4 C5 C6 -42.35(15) . . . . ? C2 N1 C6 C5 -63.41(17) . . . . ? C7 N1 C6 C5 171.76(14) . . . . ? Pd N1 C6 C5 46.24(15) . . . . ? N4 C5 C6 N1 -0.35(19) . . . . ? C2 N1 C7 C8 84.60(17) . . . . ? C6 N1 C7 C8 -153.83(14) . . . . ? Pd N1 C7 C8 -35.06(17) . . . . ? N1 C7 C8 P 47.41(17) . . . . ? C11 P C8 C7 -163.44(12) . . . . ? C21 P C8 C7 84.27(13) . . . . ? Pd P C8 C7 -36.80(12) . . . . ? C21 P C11 C16 -113.39(15) . . . . ? C8 P C11 C16 131.15(15) . . . . ? Pd P C11 C16 19.65(17) . . . . ? C21 P C11 C12 66.09(15) . . . . ? C8 P C11 C12 -49.38(16) . . . . ? Pd P C11 C12 -160.87(11) . . . . ? C11 P C21 C22 -117.02(15) . . . . ? C8 P C21 C22 -4.07(17) . . . . ? Pd P C21 C22 106.53(14) . . . . ? C11 P C21 C26 64.72(15) . . . . ? C8 P C21 C26 177.67(14) . . . . ? Pd P C21 C26 -71.74(15) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O5 H051 O9 0.77(3) 1.94(3) 2.710(2) 174(3) . O5 H052 O4 0.73(3) 2.03(3) 2.7396(19) 162(3) . O6 H062 O7 0.79(3) 1.93(3) 2.713(2) 170(3) . O6 H061 O8 0.77(3) 1.98(3) 2.741(2) 174(3) . O7 H071 O2 0.75(3) 2.16(3) 2.9126(19) 174(3) 3_666 O7 H072 O2 0.80(3) 2.01(3) 2.806(2) 173(3) 4_566 O8 H081 O3 0.71(3) 2.27(3) 2.925(2) 154(3) 3_656 O8 H081 O4 0.71(3) 2.59(3) 3.201(2) 146(3) 3_656 O8 H082 O3 0.84(3) 1.98(3) 2.817(2) 176(3) . O9 H091 O2 0.75(3) 2.10(3) 2.8422(19) 170(3) 4_566 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 29.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.500 _refine_diff_density_min -0.409 _refine_diff_density_rms 0.071 #=======================================END data_(14) _database_code_depnum_ccdc_archive 'CCDC 605825' _audit_creation_method SHELXL-97 _chemical_name_systematic ; N-methyl-piperazine palladium dichloride ; _chemical_name_common 'N-methyl-piperazine palladium dichloride' _chemical_melting_point ? _chemical_formula_moiety 'C5 H12 Cl2 N2 Pd' _chemical_formula_sum 'C5 H12 Cl2 N2 Pd' _chemical_formula_weight 277.47 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 Orthorhombic _symmetry_space_group_name_H-M Pnma loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z' '-x-1/2, y-1/2, z-1/2' _cell_length_a 11.0551(13) _cell_length_b 8.1413(3) _cell_length_c 9.3990(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 845.94(14) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 8903 _cell_measurement_theta_min 2.84 _cell_measurement_theta_max 30.00 _exptl_crystal_description 'tetragonal prism' _exptl_crystal_colour orange _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.179 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 544 _exptl_absorpt_coefficient_mu 2.752 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.5629 _exptl_absorpt_correction_T_max 0.8120 _exptl_absorpt_process_details 'XPREP 6.12 (Bruker, 2001), R(int)=0.075 before correction' loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist -1.00 0.00 1.00 0.0450 1.00 0.00 -1.00 0.0450 -1.00 0.00 -1.00 0.0450 1.00 0.00 1.00 0.0450 0.00 1.00 0.00 0.1400 0.00 -1.00 0.00 0.1400 0.00 1.00 1.00 0.1150 0.00 1.00 -1.00 0.1150 1.00 -2.00 -1.00 0.1200 _exptl_special_details ;The data collection nominally covered full sphere of reciprocal space, by a combination of 3 runs of narrow-frame \w-scans (scan width 0.3\% \w, 10s exposure), every run at a different \f angle. Crystal to detector distance 4.84 cm. ; _diffrn_ambient_temperature 120(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 'Bruker SMART 6K CCD area detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 5.6 _diffrn_standards_number 0 _diffrn_reflns_number 11409 _diffrn_reflns_av_R_equivalents 0.0216 _diffrn_reflns_av_sigmaI/netI 0.0117 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.84 _diffrn_reflns_theta_max 30.00 _reflns_number_total 1316 _reflns_number_gt 1233 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'SMART version 5.625 (Bruker, 2001)' _computing_cell_refinement 'SAINT version 6.02A (Bruker, 2001)' _computing_data_reduction 'SAINT version 6.02A (Bruker, 2001)' _computing_structure_solution 'SHELXTL version 6.14 (Bruker, 2003)' _computing_structure_refinement 'SHELXTL version 6.14 (Bruker, 2003)' _computing_molecular_graphics 'SHELXTL version 6.14 (Bruker, 2003)' _computing_publication_material 'SHELXTL version 6.14 (Bruker, 2003)' _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. ; _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^)+(0.0271P)^2^+0.8908P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1316 _refine_ls_number_parameters 81 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0200 _refine_ls_R_factor_gt 0.0187 _refine_ls_wR_factor_ref 0.0479 _refine_ls_wR_factor_gt 0.0471 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.054 _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 Pd Pd 0.403556(14) 0.2500 0.441116(18) 0.01511(7) Uani 1 2 d S . . Cl1 Cl 0.43974(6) 0.2500 0.19898(6) 0.02424(13) Uani 1 2 d S . . Cl2 Cl 0.60648(5) 0.2500 0.49769(7) 0.02180(12) Uani 1 2 d S . . N1 N 0.21928(19) 0.2500 0.4274(2) 0.0158(4) Uani 1 2 d S . . H1N H 0.188(3) 0.2500 0.347(4) 0.028(9) Uiso 1 2 d S . . C2 C 0.18303(14) 0.1011(2) 0.50873(17) 0.0175(3) Uani 1 1 d . . . H21 H 0.204(2) 0.008(3) 0.454(2) 0.018(6) Uiso 1 1 d . . . H22 H 0.0979(17) 0.104(3) 0.523(3) 0.017(5) Uiso 1 1 d . . . C3 C 0.25581(14) 0.1018(2) 0.64790(17) 0.0168(3) Uani 1 1 d . . . H31 H 0.3058(19) 0.008(3) 0.652(2) 0.017(5) Uiso 1 1 d . . . H32 H 0.204(2) 0.108(3) 0.729(2) 0.018(5) Uiso 1 1 d . . . N4 N 0.33520(17) 0.2500 0.6457(2) 0.0152(3) Uani 1 2 d S . . C9 C 0.4194(2) 0.2500 0.7679(3) 0.0198(4) Uani 1 2 d S . . H91 H 0.383(3) 0.2500 0.848(4) 0.017(7) Uiso 1 2 d S . . H92 H 0.470(2) 0.155(3) 0.761(2) 0.019(5) Uiso 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 Pd 0.01159(9) 0.01730(10) 0.01644(10) 0.000 0.00224(5) 0.000 Cl1 0.0223(3) 0.0313(3) 0.0192(3) 0.000 0.0075(2) 0.000 Cl2 0.0129(2) 0.0213(3) 0.0312(3) 0.000 0.0008(2) 0.000 N1 0.0152(9) 0.0183(9) 0.0139(8) 0.000 0.0000(6) 0.000 C2 0.0162(7) 0.0189(7) 0.0173(7) -0.0004(6) 0.0004(5) -0.0029(6) C3 0.0166(7) 0.0156(6) 0.0181(7) 0.0008(6) 0.0000(5) -0.0012(6) N4 0.0123(8) 0.0167(8) 0.0165(8) 0.000 -0.0012(7) 0.000 C9 0.0181(10) 0.0265(12) 0.0147(10) 0.000 -0.0040(8) 0.000 _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 Pd N1 2.041(2) . ? Pd N4 2.066(2) . ? Pd Cl2 2.3055(6) . ? Pd Cl1 2.3107(7) . ? N1 C2 1.488(2) 7_565 ? N1 C2 1.488(2) . ? N1 H1N 0.83(4) . ? C2 C3 1.536(2) . ? C2 H21 0.94(2) . ? C2 H22 0.951(19) . ? C3 N4 1.4923(19) . ? C3 H31 0.94(2) . ? C3 H32 0.95(2) . ? N4 C9 1.478(3) . ? N4 C3 1.4923(19) 7_565 ? C9 H91 0.85(3) . ? C9 H92 0.96(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 N1 Pd N4 72.16(8) . . ? N1 Pd Cl2 170.28(6) . . ? N4 Pd Cl2 98.12(5) . . ? N1 Pd Cl1 96.36(6) . . ? N4 Pd Cl1 168.52(6) . . ? Cl2 Pd Cl1 93.37(2) . . ? C2 N1 C2 109.12(18) 7_565 . ? C2 N1 Pd 103.68(11) 7_565 . ? C2 N1 Pd 103.68(11) . . ? C2 N1 H1N 110.7(12) 7_565 . ? C2 N1 H1N 110.7(12) . . ? Pd N1 H1N 118(2) . . ? N1 C2 C3 107.05(14) . . ? N1 C2 H21 108.2(13) . . ? C3 C2 H21 109.8(14) . . ? N1 C2 H22 108.6(15) . . ? C3 C2 H22 113.5(15) . . ? H21 C2 H22 110(2) . . ? N4 C3 C2 107.43(14) . . ? N4 C3 H31 108.1(13) . . ? C2 C3 H31 110.0(13) . . ? N4 C3 H32 108.6(13) . . ? C2 C3 H32 111.4(13) . . ? H31 C3 H32 111.2(19) . . ? C9 N4 C3 111.10(12) . 7_565 ? C9 N4 C3 111.10(12) . . ? C3 N4 C3 107.92(17) 7_565 . ? C9 N4 Pd 119.50(15) . . ? C3 N4 Pd 103.17(10) 7_565 . ? C3 N4 Pd 103.16(10) . . ? N4 C9 H91 113(2) . . ? N4 C9 H92 108.7(13) . . ? H91 C9 H92 109.3(17) . . ? 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 C2 N1 C2 C3 -64.0(2) 7_565 . . . ? N1 C2 C3 N4 -0.76(18) . . . . ? C2 C3 N4 C9 -173.12(15) . . . . ? C2 C3 N4 C3 64.85(19) . . . 7_565 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1N Cl1 0.83(4) 2.78(4) 3.311(2) 124(3) 6_556 N1 H1N Cl2 0.83(4) 3.36(4) 4.186(2) 171(3) 6_556 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.263 _refine_diff_density_min -0.798 _refine_diff_density_rms 0.110 #=====================================END