#------------------------------------------------------------------------------ #$Date: 2021-01-01 22:45:45 +0000 (Fri, 01 Jan 2021) $ #$Revision: 260345 $ #$URL: svn://www.crystallography.net/cod/cif/3/50/01/3500115.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_3500115 loop_ _publ_author_name 'Maris, Thierry' 'Zouari, Ridha' 'Chanh, N'Guyen Ba' _publ_section_references ; CAD-4 Software. (1989) Enraf--Nonius, Delft, The Netherlands. Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H. (2009), J. Appl. Cryst. 42, 339-341. North, A. C. T., Phillips, D. C. & Mathews, F. S. (1968). Acta Cryst. A24, 351--359 Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122. Sheldrick, G.M. (2015). Acta Cryst. A71, 3-8. XCAD4. (1995) University of Marburg, Germany. ; _publ_section_title ; 1,3 propanediammonium chloride ; _journal_name_full 'Personal communication to COD' _journal_year 2021 _chemical_formula_moiety 'Cl4 Pd, C3 H12 N2' _chemical_formula_sum 'C3 H12 Cl4 N2 Pd' _chemical_formula_weight 324.35 _chemical_name_common '1,3 propanediammonium chloride' _chemical_name_systematic ; propane-1,3-diaminium tetrachloro-palladium(ii) ; _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' _space_group_name_H-M_alt 'P 1 21/n 1' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary dual _audit_creation_date 2019-05-03 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _cell_angle_alpha 90 _cell_angle_beta 97.378(1) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 8.004(2) _cell_length_b 7.291(3) _cell_length_c 16.881(4) _cell_measurement_reflns_used 25 _cell_measurement_temperature 297(2) _cell_measurement_theta_max 24.4 _cell_measurement_theta_min 5.1 _cell_volume 977.0(5) _computing_cell_refinement ; CAD-4 Software. (1989) Enraf--Nonius, Delft, The Netherlands. ; _computing_data_collection ; CAD-4 Software. (1989) Enraf--Nonius, Delft, The Netherlands. ; _computing_data_reduction ; XCAD4. (1995) University of Marburg, Germany. ; _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'XL (Sheldrick, 2015)' _computing_structure_solution 'XS (Sheldrick, 2008)' _diffrn_ambient_temperature 297 _diffrn_measured_fraction_theta_full 0.983 _diffrn_measured_fraction_theta_max 0.983 _diffrn_measurement_device_type 'Nonius CAD4' _diffrn_measurement_method \w/2\q _diffrn_radiation_monochromator graphite _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.7107 _diffrn_reflns_av_R_equivalents 0.0211 _diffrn_reflns_av_unetI/netI 0.0310 _diffrn_reflns_Laue_measured_fraction_full 0.983 _diffrn_reflns_Laue_measured_fraction_max 0.983 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_number 1765 _diffrn_reflns_point_group_measured_fraction_full 0.983 _diffrn_reflns_point_group_measured_fraction_max 0.983 _diffrn_reflns_theta_full 24.952 _diffrn_reflns_theta_max 24.952 _diffrn_reflns_theta_min 2.695 _diffrn_source 'fine-focus sealed tube' _exptl_absorpt_coefficient_mu 2.929 _exptl_absorpt_correction_T_max 0.7785 _exptl_absorpt_correction_T_min 0.5651 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details ; North, A. C. T., Phillips, D. C. & Mathews, F. S. (1968). Acta Cryst. A24, 351--359. ; _exptl_crystal_colour black _exptl_crystal_colour_primary black _exptl_crystal_density_diffrn 2.205 _exptl_crystal_description plate _exptl_crystal_F_000 632 _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.07 _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. ; _refine_diff_density_max 0.603 _refine_diff_density_min -0.481 _refine_diff_density_rms 0.091 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.082 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 118 _refine_ls_number_reflns 1681 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.082 _refine_ls_R_factor_all 0.0491 _refine_ls_R_factor_gt 0.0244 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0090P)^2^+2.4063P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0506 _refine_ls_wR_factor_ref 0.0558 _refine_special_details ; 1. Fixed Uiso At 1.2 times of: All C(H,H) groups 2.a Secondary CH2 refined with riding coordinates: C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B) ; _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 1213 _reflns_number_total 1682 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file 2c3pd.cif _cod_data_source_block 2c3pd _cod_database_code 3500115 loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x+1/2, y+1/2, -z+1/2' 3 '-x, -y, -z' 4 'x-1/2, -y-1/2, z-1/2' 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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Cl3 Cl 0.09188(15) 0.46981(19) 0.63543(7) 0.0356(3) Uani 1 1 d . . . . . Cl4 Cl 0.19677(15) 0.28557(17) 0.47302(8) 0.0336(3) Uani 1 1 d . . . . . Pd2 Pd 0.000000 0.500000 0.500000 0.02172(13) Uani 1 2 d S T P . . Pd1 Pd 0.500000 1.000000 0.500000 0.02243(13) Uani 1 2 d S T P . . Cl1 Cl 0.51584(15) 1.0194(2) 0.36379(7) 0.0362(3) Uani 1 1 d . . . . . Cl2 Cl 0.29119(15) 0.78133(17) 0.47858(7) 0.0322(3) Uani 1 1 d . . . . . N1 N 0.5776(7) 0.4916(9) 0.1161(3) 0.0366(11) Uani 1 1 d . . . . . H1A H 0.496(7) 0.537(8) 0.089(3) 0.038(18) Uiso 1 1 d . . . . . H1B H 0.655(9) 0.544(10) 0.102(4) 0.07(2) Uiso 1 1 d . . . . . H1C H 0.565(10) 0.358(13) 0.106(5) 0.12(3) Uiso 1 1 d . . . . . C2 C 0.5690(7) 0.5387(9) 0.2000(3) 0.0455(15) Uani 1 1 d . . . . . H2A H 0.671179 0.497439 0.232240 0.055 Uiso 1 1 calc R . . . . H2B H 0.562924 0.670967 0.205143 0.055 Uiso 1 1 calc R . . . . C3 C 0.4232(7) 0.4558(10) 0.2305(3) 0.0524(17) Uani 1 1 d . . . . . H3A H 0.444691 0.325746 0.238408 0.063 Uiso 1 1 calc R . . . . H3B H 0.326151 0.468309 0.190088 0.063 Uiso 1 1 calc R . . . . C4 C 0.3796(6) 0.5355(9) 0.3072(3) 0.0411(14) Uani 1 1 d . . . . . H4A H 0.372493 0.667761 0.301529 0.049 Uiso 1 1 calc R . . . . H4B H 0.268982 0.491398 0.315695 0.049 Uiso 1 1 calc R . . . . N5 N 0.4986(7) 0.4924(11) 0.3783(3) 0.0409(12) Uani 1 1 d . . . . . H5A H 0.591(8) 0.518(9) 0.372(3) 0.05(2) Uiso 1 1 d . . . . . H5B H 0.468(10) 0.566(12) 0.414(5) 0.10(3) Uiso 1 1 d . . . . . H5C H 0.502(10) 0.384(12) 0.387(5) 0.09(3) 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 Cl3 0.0327(6) 0.0447(8) 0.0281(6) 0.0015(6) -0.0009(4) 0.0007(6) Cl4 0.0279(6) 0.0287(6) 0.0456(7) 0.0000(6) 0.0100(5) 0.0071(5) Pd2 0.0174(2) 0.0219(3) 0.0258(2) 0.0012(3) 0.00240(17) 0.0006(2) Pd1 0.0180(2) 0.0220(3) 0.0276(3) 0.0007(3) 0.00417(17) -0.0009(2) Cl1 0.0305(6) 0.0495(8) 0.0288(6) 0.0017(7) 0.0048(4) -0.0039(7) Cl2 0.0273(6) 0.0285(6) 0.0413(7) -0.0023(6) 0.0059(5) -0.0081(5) N1 0.032(3) 0.050(3) 0.028(2) 0.002(3) 0.005(2) -0.001(3) C2 0.049(3) 0.056(4) 0.032(3) -0.007(3) 0.008(2) -0.008(3) C3 0.040(3) 0.080(5) 0.037(3) 0.001(3) 0.003(2) -0.009(3) C4 0.034(3) 0.058(4) 0.032(3) 0.000(3) 0.005(2) 0.009(3) N5 0.037(3) 0.055(4) 0.031(2) -0.004(3) 0.009(2) 0.000(3) 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_ _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 Cl3 Pd2 Cl3 180.0 3_566 . Cl4 Pd2 Cl3 89.55(5) . . Cl4 Pd2 Cl3 90.45(5) . 3_566 Cl4 Pd2 Cl3 89.55(5) 3_566 3_566 Cl4 Pd2 Cl3 90.45(5) 3_566 . Cl4 Pd2 Cl4 180.0 . 3_566 Cl1 Pd1 Cl1 180.0 3_676 . Cl2 Pd1 Cl1 89.00(4) 3_676 . Cl2 Pd1 Cl1 89.00(4) . 3_676 Cl2 Pd1 Cl1 91.00(4) . . Cl2 Pd1 Cl1 91.00(4) 3_676 3_676 Cl2 Pd1 Cl2 180.0 . 3_676 H1A N1 H1B 104(6) . . H1A N1 H1C 104(6) . . H1B N1 H1C 119(7) . . C2 N1 H1A 108(4) . . C2 N1 H1B 108(5) . . C2 N1 H1C 112(5) . . N1 C2 H2A 109.1 . . N1 C2 H2B 109.1 . . H2A C2 H2B 107.9 . . C3 C2 N1 112.4(5) . . C3 C2 H2A 109.1 . . C3 C2 H2B 109.1 . . C2 C3 H3A 108.5 . . C2 C3 H3B 108.5 . . C2 C3 C4 115.3(5) . . H3A C3 H3B 107.5 . . C4 C3 H3A 108.5 . . C4 C3 H3B 108.5 . . C3 C4 H4A 108.5 . . C3 C4 H4B 108.5 . . H4A C4 H4B 107.5 . . N5 C4 C3 115.1(5) . . N5 C4 H4A 108.5 . . N5 C4 H4B 108.5 . . C4 N5 H5A 111(4) . . C4 N5 H5B 103(5) . . C4 N5 H5C 112(6) . . H5A N5 H5B 108(7) . . H5A N5 H5C 105(8) . . H5B N5 H5C 119(8) . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Cl3 Pd2 2.3204(13) . Cl4 Pd2 2.3057(13) . Pd1 Cl1 2.3234(12) 3_676 Pd1 Cl1 2.3234(12) . Pd1 Cl2 2.3045(13) . Pd1 Cl2 2.3045(13) 3_676 N1 H1A 0.82(6) . N1 H1B 0.79(7) . N1 H1C 0.99(10) . N1 C2 1.468(6) . C2 H2A 0.9700 . C2 H2B 0.9700 . C2 C3 1.465(7) . C3 H3A 0.9700 . C3 H3B 0.9700 . C3 C4 1.500(7) . C4 H4A 0.9700 . C4 H4B 0.9700 . C4 N5 1.467(7) . N5 H5A 0.78(6) . N5 H5B 0.86(9) . N5 H5C 0.81(9) . 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 _geom_hbond_publ_flag N1 H1A Cl4 0.82(6) 2.52(6) 3.291(6) 158(5) 2 yes N1 H1B Cl1 0.79(7) 2.63(7) 3.235(5) 135(6) 2_645 yes N1 H1B Cl2 0.79(7) 2.78(7) 3.475(5) 147(6) 4_675 yes N1 H1C Cl3 0.99(10) 2.45(10) 3.380(7) 157(7) 4_665 yes N1 H1C Cl4 0.99(10) 2.80(8) 3.379(5) 118(6) 4_665 yes N5 H5A Cl3 0.78(6) 2.56(6) 3.327(6) 167(6) 3_666 yes N5 H5B Cl2 0.86(9) 2.46(9) 3.284(7) 160(7) . yes N5 H5C Cl1 0.81(9) 2.69(9) 3.461(8) 160(7) 1_545 yes N5 H5C Cl2 0.81(9) 2.89(8) 3.407(6) 124(7) 3_666 yes 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 N1 C2 C3 C4 -164.5(5) . . . . C2 C3 C4 N5 -70.8(7) . . . . _cod_database_fobs_code 3500115