#------------------------------------------------------------------------------ #$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $ #$Revision: 176435 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/50/16/1501622.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_1501622 loop_ _publ_author_name 'Thierry Maris' 'Georges Bravic' 'Nguyen Ba Chan' 'Jean-Michel Leger' 'Jean-Claude Bissey' 'Antoine Villesuzanne' 'Ridha Zouari' 'Abdelaziz Daoud' _publ_section_title ; Structures and thermal behavior in the series of two-dimensional molecular composites NH~3~-(CH~2~)~4~-NH~3~ MCl~4~ related to the nature of the metal M. Part 1 : Crystal structure and phase transition in the case M=Cu and Pd. ; _journal_name_full 'J. Phys. Chem. Solids' _journal_page_first 1963 _journal_page_last 1975 _journal_paper_doi 10.1016/S0022-3697(96)00045-5 _journal_volume 57 _journal_year 1996 _chemical_formula_moiety 'C4 H14 N2, Cl4 Pd' _chemical_formula_sum 'C4 H14 Cl4 N2 Pd' _chemical_formula_weight 338.37 _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_Int_Tables_number 14 _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _cell_angle_alpha 90 _cell_angle_beta 103.82(2) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 9.087(2) _cell_length_b 7.699(2) _cell_length_c 7.792(2) _cell_measurement_temperature 293 _cell_volume 529.4(2) _diffrn_ambient_temperature 293 _diffrn_measurement_device_type Nonius-CAD4 _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_radiation_source 'Sealed Tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _exptl_absorpt_coefficient_mu 2.707 _exptl_crystal_F_000 332 _refine_ls_hydrogen_treatment constr _refine_ls_R_factor_gt 0.0178 _refine_ls_structure_factor_coef F _refine_ls_wR_factor_gt 0.0220 _cod_data_source_file deposit.cif _cod_data_source_block 2C4PdCl4 _cod_original_sg_symbol_H-M 'P 21/c' _cod_original_formula_sum 'C4 H14 N2, Cl4 Pd' _cod_database_code 1501622 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -x,1/2+y,1/2-z 3 -x,-y,-z 4 x,1/2-y,1/2+z 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 N1 0.0258(8) 0.0378(10) 0.0461(10) 0.0013(7) 0.0126(7) 0.0037(8) C1 0.0292(9) 0.0474(13) 0.0366(10) 0.0043(9) 0.0033(8) 0.0117(9) C2 0.0295(9) 0.0270(9) 0.0382(10) 0.0026(8) 0.0133(8) -0.0004(8) Pd1 0.0210(1) 0.0194(1) 0.0186(1) 0.0008(1) 0.0061(1) -0.0003(1) Cl1 0.0357(2) 0.0290(2) 0.0266(2) -0.0034(2) 0.0104(2) -0.0080(2) Cl2 0.0233(2) 0.0359(3) 0.0447(3) 0.0024(2) 0.0066(2) -0.0040(2) loop_ _atom_site_label _atom_site_type_symbol _atom_site_thermal_displace_type _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_U_iso_or_equiv N1 N Uani 0.2219(2) -0.0385(3) 0.5700(3) 1.000 0.0359(5) C1 C Uani 0.3614(2) 0.0627(3) 0.6455(3) 1.000 0.0385(6) C2 C Uani 0.4618(2) 0.0829(3) 0.5173(3) 1.000 0.0307(5) Pd1 Pd Uani 0.00000 0.00000 0.00000 1.000 0.0194(1) Cl1 Cl Uani 0.03750(10) 0.19660(10) 0.22970(10) 1.000 0.0299(1) Cl2 Cl Uani -0.25880(10) 0.04460(10) -0.04900(10) 1.000 0.0349(2) H1 H Uiso 0.1547(2) -0.0500(3) 0.6667(3) 1.000 0.0500 H2 H Uiso 0.1568(2) 0.0274(3) 0.4542(3) 1.000 0.0500 H3 H Uiso 0.2526(2) -0.1664(3) 0.5336(3) 1.000 0.0500 H4 H Uiso 0.4251(2) -0.0039(3) 0.7617(3) 1.000 0.0500 H5 H Uiso 0.3292(2) 0.1899(3) 0.6822(3) 1.000 0.0500 H6 H Uiso 0.538(3) 0.171(3) 0.562(3) 1.000 0.0500 H7 H Uiso 0.402(3) 0.133(3) 0.409(3) 1.000 0.0500 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' Cl Cl 0.1484 0.1585 ' 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' 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 _geom_angle_publ_flag Cl2 Pd1 Cl2 180.00 . 3_555 yes Cl1 Pd1 Cl2 89.23(4) 3_555 3_555 yes Cl1 Pd1 Cl2 90.77(4) . 3_555 yes Cl1 Pd1 Cl2 89.23(4) . . yes Cl1 Pd1 Cl1 180.00 . 3_555 yes Cl1 Pd1 Cl2 90.77(4) 3_555 . yes C1 N1 H1 109.8(2) . . no H1 N1 H3 109.4(3) . . no H2 N1 H3 109.5(3) . . no C1 N1 H3 109.5(2) . . no H1 N1 H2 109.5(2) . . no C1 N1 H2 109.3(2) . . no N1 C1 C2 112.63(19) . . yes C1 C2 C2 114.02(19) . 3_656 no C2 C1 H4 108.4(2) . . no N1 C1 H5 108.7(2) . . no N1 C1 H4 108.6(2) . . no C2 C1 H5 109.0(2) . . no H4 C1 H5 109.5(3) . . no C2 C2 H7 111.6(14) 3_656 . no C1 C2 H6 109.0(14) . . no C1 C2 H7 108.4(16) . . no H6 C2 H7 104(2) . . no C2 C2 H6 109.6(15) 3_656 . no 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 Cl1 2.3064(10) . yes Pd1 Cl2 2.3163(11) . yes Pd1 Cl1 2.3064(10) 3_555 yes Pd1 Cl2 2.3163(11) 3_555 yes N1 C1 1.485(3) . yes N1 H1 1.081(3) . no N1 H2 1.080(3) . no N1 H3 1.080(3) . no C1 C2 1.513(3) . no C2 C2 1.508(3) 3_656 no C1 H5 1.080(3) . no C1 H4 1.081(3) . no C2 H6 0.97(3) . no C2 H7 0.97(2) . no 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 H1 Cl1 1.081(3) 2.377(2) 3.351(2) 149.2(2) 3_556 yes N1 H2 Cl1 1.080(3) 2.242(2) 3.316(3) 172.3(2) . yes N1 H3 Cl2 1.080(3) 2.228(3) 3.235(3) 154.3(2) 2_545 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_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 C2 -70.2(2) . 3_656 no C1 C2 C2 C1 180.00(17) 3_656 3_656 no