#------------------------------------------------------------------------------ #$Date: 2010-01-30 15:59:17 +0200 (Sat, 30 Jan 2010) $ #$Revision: 966 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/2203350.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2203350 _space_group_IT_number 5 _symmetry_space_group_name_Hall 'C 2y' _symmetry_space_group_name_H-M 'C 1 2 1' _[local]_cod_cif_authors_sg_H-M 'C 2' loop_ _publ_author_name 'Cruz-Cruz, Sandra' 'Rodr\'iguez-Pastrana, Modesto' 'Bern\`es, Sylvain' 'Guti\'errez-P\'erez, Ren\'e' _publ_section_title ; Bis[(S)-(-)-1-phenylethylammonium] tetrachloropalladate(II) ; _journal_issue 3 _journal_name_full 'Acta Crystallographica, Section E' _journal_page_first m342 _journal_page_last m344 _journal_volume 60 _journal_year 2004 _chemical_formula_iupac '(C8 H12 N)2 [Pd Cl4]' _chemical_formula_moiety '2C8 H12 N 1+, Cl4 Pd 2-' _chemical_formula_sum 'C16 H24 Cl4 N2 Pd' _chemical_formula_weight 492.57 _chemical_melting_point 463 _chemical_name_common ' (S)-(-)-\a-Methylbenzylammonium tetrachloropalladate(II)' _chemical_name_systematic ' (S)-(-)-1-Phenylethylammonium tetrachloropalladate(II)' _symmetry_cell_setting Monoclinic _atom_sites_solution_hydrogens geom _atom_sites_solution_primary heavy _atom_sites_solution_secondary difmap _audit_creation_method SHELXTL-Plus _cell_angle_alpha 90.00 _cell_angle_beta 97.800(10) _cell_angle_gamma 90.00 _cell_formula_units_Z 2 _cell_length_a 11.2280(11) _cell_length_b 7.2220(11) _cell_length_c 13.3393(16) _cell_measurement_reflns_used 79 _cell_measurement_temperature 296.0(10) _cell_measurement_theta_max 12.96 _cell_measurement_theta_min 4.62 _cell_volume 1071.7(2) _computing_cell_refinement XSCANS _computing_data_collection 'XSCANS (Siemens, 1996)' _computing_data_reduction XSCANS _computing_molecular_graphics SHELXTL-Plus _computing_publication_material SHELXTL-Plus _computing_structure_refinement SHELXTL-Plus _computing_structure_solution 'SHELXTL-Plus (Sheldrick, 1998)' _diffrn_ambient_temperature 296.0(10) _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method 2\q/\w _diffrn_radiation_monochromator graphite _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0254 _diffrn_reflns_av_sigmaI/netI 0.0299 _diffrn_reflns_limit_h_max 3 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_number 2431 _diffrn_reflns_theta_full 29.99 _diffrn_reflns_theta_max 29.99 _diffrn_reflns_theta_min 3.08 _diffrn_standards_decay_% <1 _diffrn_standards_interval_count 97 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 1.364 _exptl_absorpt_correction_T_max 0.898 _exptl_absorpt_correction_T_min 0.643 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details '(XSCANS; Siemens, 1996)' _exptl_crystal_colour orange _exptl_crystal_density_diffrn 1.526 _exptl_crystal_density_method 'not measured' _exptl_crystal_description plate _exptl_crystal_F_000 496 _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.08 _refine_diff_density_max 0.514 _refine_diff_density_min -1.167 _refine_ls_abs_structure_details 'Flack (1983), 227 Friedel pairs' _refine_ls_abs_structure_Flack -0.01(4) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.065 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 125 _refine_ls_number_reflns 1904 _refine_ls_number_restraints 7 _refine_ls_restrained_S_all 1.063 _refine_ls_R_factor_all 0.0287 _refine_ls_R_factor_gt 0.0276 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w = 1/[\s^2^(Fo^2^)+(0.0464P)^2^+0.1903P] where P = (Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0731 _refine_ls_wR_factor_ref 0.0744 _reflns_number_gt 1836 _reflns_number_total 1904 _reflns_threshold_expression I>2\s(I) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_type_symbol Pd1 0.5000 0.61456(9) 0.5000 0.03668(9) Uani d S 1 Pd Cl1 0.59668(18) 0.84213(12) 0.42090(15) 0.0469(3) Uani d . 1 Cl Cl2 0.58619(19) 0.38868(15) 0.41181(17) 0.0536(4) Uani d . 1 Cl C1 0.3641(3) 0.0700(5) 0.2733(2) 0.0463(8) Uani d . 1 C H1A 0.4512 0.0674 0.2725 0.056 Uiso calc R 1 H N1 0.3428(2) 0.1143(10) 0.37981(16) 0.0444(5) Uani d D 1 N H11 0.390(4) 0.205(5) 0.399(4) 0.057(7) Uiso d D 1 H H12 0.361(4) 0.023(6) 0.420(3) 0.057(7) Uiso d D 1 H H13 0.268(2) 0.134(10) 0.389(3) 0.057(7) Uiso d D 1 H C2 0.3161(6) -0.1224(8) 0.2451(4) 0.0672(12) Uani d D 1 C H21 0.349(5) -0.136(9) 0.181(3) 0.066(9) Uiso d D 1 H H22 0.2290(19) -0.127(9) 0.234(4) 0.066(9) Uiso d D 1 H H23 0.351(5) -0.224(6) 0.289(3) 0.066(9) Uiso d D 1 H C3 0.3133(4) 0.2192(6) 0.2021(3) 0.0533(8) Uani d . 1 C C4 0.3890(7) 0.3280(9) 0.1525(4) 0.0802(17) Uani d . 1 C H4A 0.4718 0.3112 0.1649 0.096 Uiso calc R 1 H C5 0.3397(11) 0.4637(11) 0.0833(5) 0.115(3) Uani d . 1 C H5A 0.3905 0.5372 0.0507 0.138 Uiso calc R 1 H C6 0.2194(11) 0.4886(10) 0.0638(4) 0.122(4) Uani d . 1 C H6A 0.1880 0.5768 0.0167 0.146 Uiso calc R 1 H C7 0.1437(8) 0.3843(12) 0.1131(4) 0.099(3) Uani d . 1 C H7A 0.0612 0.4046 0.1010 0.119 Uiso calc R 1 H C8 0.1900(5) 0.2477(9) 0.1815(3) 0.0704(13) Uani d . 1 C H8A 0.1380 0.1753 0.2135 0.085 Uiso calc R 1 H loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Pd1 0.03646(13) 0.03294(13) 0.03924(13) 0.000 0.00010(8) 0.000 Cl1 0.0515(7) 0.0392(6) 0.0513(6) -0.0028(5) 0.0116(5) 0.0002(5) Cl2 0.0541(8) 0.0409(7) 0.0681(9) -0.0051(6) 0.0163(6) -0.0142(6) C1 0.0498(14) 0.047(2) 0.0430(13) 0.0004(12) 0.0080(11) -0.0019(12) N1 0.0487(11) 0.0464(12) 0.0367(9) 0.001(3) 0.0004(8) 0.002(2) C2 0.091(3) 0.050(2) 0.058(2) -0.003(2) 0.000(2) -0.0122(19) C3 0.077(2) 0.048(2) 0.0351(13) 0.0007(18) 0.0091(14) -0.0041(15) C4 0.119(5) 0.067(3) 0.055(2) -0.028(3) 0.016(3) 0.000(2) C5 0.222(11) 0.066(4) 0.057(3) -0.026(5) 0.017(4) 0.014(3) C6 0.235(12) 0.074(4) 0.047(2) 0.041(6) -0.020(4) 0.008(3) C7 0.134(6) 0.107(5) 0.051(2) 0.057(5) -0.012(3) -0.003(3) C8 0.083(3) 0.083(4) 0.0433(16) 0.023(3) 0.0023(18) 0.002(2) 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' loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 0 0 -3 -3 -1 0 3 -1 2 loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag Cl2 Pd1 Cl2 2_656 . 89.66(9) y Cl2 Pd1 Cl1 2_656 2_656 90.84(3) n Cl2 Pd1 Cl1 . 2_656 176.08(10) n Cl2 Pd1 Cl1 2_656 . 176.08(10) y Cl2 Pd1 Cl1 . . 90.84(3) y Cl1 Pd1 Cl1 2_656 . 88.94(8) y C3 C1 N1 . . 110.5(3) y C3 C1 C2 . . 114.2(3) y N1 C1 C2 . . 109.4(4) y C3 C1 H1A . . 107.5 n N1 C1 H1A . . 107.5 n C2 C1 H1A . . 107.5 n C1 N1 H11 . . 106(3) n C1 N1 H12 . . 112(4) n C1 N1 H13 . . 116(3) n H11 N1 H12 . . 109(4) n H11 N1 H13 . . 113(6) n H12 N1 H13 . . 101(5) n C1 C2 H21 . . 98(4) n C1 C2 H22 . . 113(4) n C1 C2 H23 . . 116(3) n H21 C2 H22 . . 111(5) n H21 C2 H23 . . 106(5) n H22 C2 H23 . . 112(5) n C8 C3 C4 . . 118.6(5) n C8 C3 C1 . . 121.0(4) n C4 C3 C1 . . 120.3(5) n C3 C4 C5 . . 119.6(8) n C3 C4 H4A . . 120.2 n C5 C4 H4A . . 120.2 n C6 C5 C4 . . 120.9(8) n C6 C5 H5A . . 119.6 n C4 C5 H5A . . 119.6 n C5 C6 C7 . . 120.2(6) n C5 C6 H6A . . 119.9 n C7 C6 H6A . . 119.9 n C6 C7 C8 . . 120.2(7) n C6 C7 H7A . . 119.9 n C8 C7 H7A . . 119.9 n C3 C8 C7 . . 120.5(6) n C3 C8 H8A . . 119.8 n C7 C8 H8A . . 119.8 n loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Pd1 Cl1 . 2.3030(17) y Pd1 Cl2 . 2.3001(18) y Pd1 Cl1 2_656 2.3030(16) n Pd1 Cl2 2_656 2.3001(18) n C1 N1 . 1.506(4) y C1 C2 . 1.519(6) y C1 C3 . 1.497(5) y C1 H1A . 0.9800 n N1 H11 . 0.856(19) ? N1 H12 . 0.860(19) ? N1 H13 . 0.872(19) ? C2 H21 . 0.98(2) ? C2 H22 . 0.970(19) ? C2 H23 . 0.99(2) ? C3 C8 . 1.390(7) n C3 C4 . 1.390(7) n C4 C5 . 1.406(10) n C4 H4A . 0.9300 n C5 C6 . 1.353(13) n C5 H5A . 0.9300 n C6 C7 . 1.369(12) n C6 H6A . 0.9300 n C7 C8 . 1.395(8) n C7 H7A . 0.9300 n C8 H8A . 0.9300 n loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag N1 H11 Cl2 1_555 0.856(19) 2.56(3) 3.356(5) 155(4) y N1 H11 Cl2 2_656 0.856(19) 2.83(4) 3.419(5) 127(4) y N1 H12 Cl1 2_646 0.860(19) 2.48(3) 3.302(5) 160(5) y N1 H12 Cl1 1_545 0.860(19) 2.95(4) 3.444(5) 119(4) y N1 H13 Cl1 3_445 0.872(19) 2.53(4) 3.325(5) 153(7) y N1 H13 Cl2 3_445 0.872(19) 2.76(6) 3.387(5) 130(6) y 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_publ_flag N1 C1 C3 C8 -67.6(5) n C2 C1 C3 C8 56.2(5) n N1 C1 C3 C4 114.7(4) n C2 C1 C3 C4 -121.5(5) n C8 C3 C4 C5 0.2(8) n C1 C3 C4 C5 178.0(5) n C3 C4 C5 C6 -0.6(10) n C4 C5 C6 C7 1.5(11) n C5 C6 C7 C8 -2.0(10) n C4 C3 C8 C7 -0.7(7) n C1 C3 C8 C7 -178.4(5) n C6 C7 C8 C3 1.6(9) n _cod_database_code 2203350