# Copyright The Royal Society of Chemistry, 1999 # CCDC Number 186/1298 data_s92 _audit_creation_method SHELXL-96 _chemical_name_systematic ; 'Dicloro-{3S-(R-methylamino)pyrrolidine}palladium(II)' ; _chemical_name_common ? _chemical_formula_moiety 'C5 H12 Cl2 N2 Pd' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C5 H12 Cl2 N2 Pd' _chemical_formula_weight 277.47 _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' '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 P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 7.2131(4) _cell_length_b 10.595(2) _cell_length_c 11.664(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 891.4(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 250 _cell_measurement_theta_min 3.32 _cell_measurement_theta_max 29.71 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.068 _exptl_crystal_density_method ? _exptl_crystal_F_000 544 _exptl_absorpt_coefficient_mu 2.612 _exptl_absorpt_correction_type 'DIFABS (Walker, 1983)' _exptl_absorpt_correction_T_min 0.893 _exptl_absorpt_correction_T_max 1.106 _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode generator' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'FAST area detector diffractometer' _diffrn_measurement_method 'Darr, Drake, Hursthouse & Malik, 1993' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 4313 _diffrn_reflns_av_R_equivalents 0.0230 _diffrn_reflns_av_sigmaI/netI 0.0519 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 7 _diffrn_reflns_theta_min 3.32 _diffrn_reflns_theta_max 29.71 _reflns_number_total 2203 _reflns_number_observed 2183 _reflns_observed_criterion >2sigma(I) _computing_data_collection MADNES _computing_cell_refinement 'REFINE in MADNES' _computing_data_reduction 'ABSMAD (Karaulov, 1991)' _computing_structure_solution 'SHELXS-96 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-96 (Sheldrick, 1996)' _computing_molecular_graphics 'SNOOPI (Davies, 1983)' _computing_publication_material SHELXL-96 _refine_special_details ; Refinement of F^2^ against ALL reflections. 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^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment 'calculated positions, riding model' _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 -0.07(4) _refine_ls_number_reflns 2203 _refine_ls_number_parameters 92 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0234 _refine_ls_R_factor_obs 0.0231 _refine_ls_wR_factor_all 0.0548 _refine_ls_wR_factor_obs 0.0544 _refine_ls_goodness_of_fit_all 0.898 _refine_ls_goodness_of_fit_obs 0.897 _refine_ls_restrained_S_all 0.898 _refine_ls_restrained_S_obs 0.897 _refine_ls_shift/esd_max 0.001 _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 0.36114(3) 0.18903(2) 0.34835(2) 0.02719(7) Uani 1 d . . Cl1 Cl 0.66993(11) 0.19052(9) 0.39768(8) 0.04187(18) Uani 1 d . . Cl2 Cl 0.31070(13) -0.01701(8) 0.40815(8) 0.0404(2) Uani 1 d . . N1 N 0.0931(4) 0.2067(2) 0.2955(2) 0.0327(6) Uani 1 d . . H1 H 0.0123 0.1584 0.3363 0.039 Uiso 1 calc R . N2 N 0.3803(4) 0.3682(2) 0.2822(2) 0.0334(6) Uani 1 d . . H2 H 0.4730 0.3687 0.2293 0.040 Uiso 1 calc R . C1 C 0.0889(5) 0.1807(4) 0.1693(3) 0.0453(8) Uani 1 d . . H1A H -0.0373 0.1738 0.1413 0.054 Uiso 1 calc R . H1B H 0.1560 0.1041 0.1507 0.054 Uiso 1 calc R . C2 C 0.1859(6) 0.2971(4) 0.1202(3) 0.0494(9) Uani 1 d . . H2A H 0.3076 0.2754 0.0909 0.059 Uiso 1 calc R . H2B H 0.1133 0.3339 0.0587 0.059 Uiso 1 calc R . C3 C 0.2017(5) 0.3886(3) 0.2208(3) 0.0393(8) Uani 1 d . . H3 H 0.1846 0.4766 0.1974 0.047 Uiso 1 calc R . C4 C 0.0513(5) 0.3439(3) 0.3011(3) 0.0375(7) Uani 1 d . . H4A H 0.0661 0.3777 0.3779 0.045 Uiso 1 calc R . H4B H -0.0718 0.3634 0.2726 0.045 Uiso 1 calc R . C5 C 0.4222(6) 0.4660(3) 0.3689(3) 0.0447(9) Uani 1 d . . H5A H 0.5443 0.4522 0.3992 0.067 Uiso 1 calc R . H5B H 0.3331 0.4613 0.4298 0.067 Uiso 1 calc R . H5C H 0.4166 0.5479 0.3338 0.067 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 0.02538(12) 0.02791(10) 0.02827(11) 0.00102(9) 0.00072(9) 0.00042(8) Cl1 0.0274(4) 0.0511(4) 0.0471(4) -0.0031(4) -0.0031(3) 0.0032(4) Cl2 0.0468(5) 0.0319(4) 0.0424(4) 0.0067(3) 0.0077(4) 0.0026(3) N1 0.0278(14) 0.0334(13) 0.0368(13) 0.0060(12) -0.0007(11) -0.0032(10) N2 0.0346(16) 0.0309(12) 0.0346(14) 0.0026(11) 0.0042(12) -0.0041(11) C1 0.046(2) 0.0485(19) 0.0415(19) -0.0004(17) -0.0122(16) -0.0081(16) C2 0.057(2) 0.057(2) 0.0340(17) 0.0039(17) -0.0050(17) -0.0144(19) C3 0.0367(19) 0.0349(16) 0.0461(19) 0.0142(15) -0.0078(16) -0.0004(13) C4 0.0314(18) 0.0322(15) 0.0488(19) 0.0049(14) 0.0005(16) 0.0049(11) C5 0.055(2) 0.0359(16) 0.044(2) 0.0013(15) 0.0024(17) -0.0043(15) _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 2.0379(28) . ? Pd1 N2 2.0537(25) . ? Pd1 Cl1 2.3005(8) . ? Pd1 Cl2 2.3204(9) . ? N1 C4 1.4865(40) . ? N1 C1 1.4977(46) . ? N2 C5 1.4785(43) . ? N2 C3 1.4893(45) . ? C1 C2 1.5289(49) . ? C2 C3 1.5254(52) . ? C3 C4 1.5096(52) . ? 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 N2 82.26(11) . . ? N1 Pd1 Cl1 173.50(8) . . ? N2 Pd1 Cl1 91.29(9) . . ? N1 Pd1 Cl2 91.64(8) . . ? N2 Pd1 Cl2 173.24(8) . . ? Cl1 Pd1 Cl2 94.76(3) . . ? C4 N1 C1 102.6(3) . . ? C4 N1 Pd1 105.6(2) . . ? C1 N1 Pd1 107.4(2) . . ? C5 N2 C3 113.9(3) . . ? C5 N2 Pd1 113.9(2) . . ? C3 N2 Pd1 104.85(19) . . ? N1 C1 C2 102.2(3) . . ? C3 C2 C1 105.0(3) . . ? N2 C3 C4 106.1(3) . . ? N2 C3 C2 110.0(3) . . ? C4 C3 C2 103.0(3) . . ? N1 C4 C3 97.7(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 N2 Pd1 N1 C4 -28.6(2) . . . . ? Cl1 Pd1 N1 C4 -35.6(9) . . . . ? Cl2 Pd1 N1 C4 154.3(2) . . . . ? N2 Pd1 N1 C1 80.4(2) . . . . ? Cl1 Pd1 N1 C1 73.4(8) . . . . ? Cl2 Pd1 N1 C1 -96.7(2) . . . . ? N1 Pd1 N2 C5 115.6(3) . . . . ? Cl1 Pd1 N2 C5 -65.2(3) . . . . ? Cl2 Pd1 N2 C5 141.2(6) . . . . ? N1 Pd1 N2 C3 -9.5(2) . . . . ? Cl1 Pd1 N2 C3 169.7(2) . . . . ? Cl2 Pd1 N2 C3 16.1(9) . . . . ? C4 N1 C1 C2 40.4(4) . . . . ? Pd1 N1 C1 C2 -70.6(3) . . . . ? N1 C1 C2 C3 -10.6(4) . . . . ? C5 N2 C3 C4 -78.8(3) . . . . ? Pd1 N2 C3 C4 46.3(3) . . . . ? C5 N2 C3 C2 170.4(3) . . . . ? Pd1 N2 C3 C2 -64.5(3) . . . . ? C1 C2 C3 N2 90.6(4) . . . . ? C1 C2 C3 C4 -22.2(4) . . . . ? C1 N1 C4 C3 -54.1(3) . . . . ? Pd1 N1 C4 C3 58.3(3) . . . . ? N2 C3 C4 N1 -69.5(3) . . . . ? C2 C3 C4 N1 46.1(3) . . . . ? _refine_diff_density_max 0.715 _refine_diff_density_min -0.325 _refine_diff_density_rms 0.081