#------------------------------------------------------------------------------ #$Date: 2016-02-19 14:29:56 +0000 (Fri, 19 Feb 2016) $ #$Revision: 176759 $ #$URL: svn://www.crystallography.net/cod/cif/2/00/65/2006515.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_2006515 loop_ _publ_author_name 'Eric S. Raper' 'Maria Kubiak' 'Tadeusz G\/lowiak' _publ_section_title ; Dimethylammonium Trichloropalladate ; _journal_issue 9 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 1201 _journal_page_last 1204 _journal_paper_doi 10.1107/S010827019700379X _journal_volume 53 _journal_year 1997 _chemical_formula_moiety '[NH2 (CH3)2] [PdCl3]' _chemical_formula_sum 'C2 H8 Cl3 N Pd' _chemical_formula_weight 258.84 _chemical_name_systematic ; dimethylammonium trichloropalladate ; _space_group_IT_number 15 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-C 2yc' _symmetry_space_group_name_H-M 'C 1 2/c 1' _audit_creation_method SHELXL _cell_angle_alpha 90.00 _cell_angle_beta 91.24(3) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 7.802(2) _cell_length_b 13.221(3) _cell_length_c 7.1420(10) _cell_measurement_reflns_used 25 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 30 _cell_measurement_theta_min 3 _cell_volume 736.5(3) _computing_cell_refinement XTL/XTLE _computing_data_collection 'XTL/XTLE (Syntex, 1976)' _computing_data_reduction XTL/XTLE _computing_molecular_graphics 'ORTEPII (Johnson, 1976)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _diffrn_ambient_temperature 293(2) _diffrn_measurement_device 'Syntex P2~1~ diffractometer' _diffrn_measurement_method \q/2\q _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71069 _diffrn_reflns_av_R_equivalents 0.0274 _diffrn_reflns_av_sigmaI/netI 0.0223 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_number 1119 _diffrn_reflns_theta_max 30.06 _diffrn_reflns_theta_min 3.03 _diffrn_standards_decay_% 2 _diffrn_standards_interval_count 100 _diffrn_standards_number 2 _exptl_absorpt_coefficient_mu 3.498 _exptl_absorpt_correction_type none _exptl_crystal_colour red-brown _exptl_crystal_density_diffrn 2.334 _exptl_crystal_density_meas 2.30 _exptl_crystal_density_method 'flotation in C~2~H~4~Br~2~/CHBr~3~' _exptl_crystal_description prism _exptl_crystal_F_000 496 _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _refine_diff_density_max 1.18 _refine_diff_density_min -1.36 _refine_ls_extinction_coef 0.0046(6) _refine_ls_extinction_method 'SHELXL93 (Sheldrick, 1993)' _refine_ls_goodness_of_fit_all 1.192 _refine_ls_goodness_of_fit_obs 1.257 _refine_ls_hydrogen_treatment refall _refine_ls_matrix_type full _refine_ls_number_parameters 52 _refine_ls_number_reflns 1066 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.192 _refine_ls_restrained_S_obs 1.257 _refine_ls_R_factor_all 0.0336 _refine_ls_R_factor_obs .0267 _refine_ls_shift/esd_max 0.202 _refine_ls_shift/esd_mean 0.020 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.0348P)^2^+0.4125P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_all 0.0673 _refine_ls_wR_factor_obs .0652 _reflns_number_observed 908 _reflns_number_total 1066 _reflns_observed_criterion >2sigma(I) _cod_data_source_file mu1264.cif _cod_data_source_block PdCl3 _cod_original_sg_symbol_H-M 'C 2/c' _cod_database_code 2006515 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' 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 Pd .0273(2) .0289(2) .0209(2) .00035(11) .00196(10) .00136(10) Cl1 .0491(6) .0324(5) .0244(4) .000 .0025(4) .000 Cl2 .0351(4) .0464(4) .0381(4) .0089(3) -.0041(3) -.0002(3) C1 .046(2) .048(2) .044(2) -.003(2) -.007(2) -.006(2) N .039(2) .034(2) .040(2) .000 -.003(2) .000 loop_ _atom_site_label _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_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_disorder_group _atom_site_type_symbol Pd 0 0 0 .02568(12) Uani d S 1 . Pd Cl1 0 .11093(8) .25 .0353(2) Uani d S 1 . Cl Cl2 .24957(10) -.07267(6) .11471(11) .0399(2) Uani d . 1 . Cl C1 .5803(5) .1884(3) .4001(6) .0463(8) Uani d . 1 . C N .5 .1264(3) .25 .0376(8) Uani d S 1 . N H1 .497(5) .229(3) .460(6) .039(11) Uiso d . 1 . H H2 .616(5) .144(3) .481(5) .034(9) Uiso d . 1 . H H3 .658(7) .231(4) .332(8) .081(17) Uiso d . 1 . H H4 .583(5) .085(3) .187(6) .049(11) Uiso d . 1 . H 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_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag Cl2 Pd Cl1 . . 90.23(3) y Pd Cl1 Pd . 2 101.20(4) y N C1 H1 . . 111.(2) no N C1 H2 . . 103.(3) no H1 C1 H2 . . 107.(3) no N C1 H3 . . 103.(3) no H1 C1 H3 . . 110.(4) no H2 C1 H3 . . 123.(4) no C1 N C1 . 2_655 112.6(4) y C1 N H4 . . 112.(3) no C1 N H4 2_655 . 105.(3) no 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 Pd Cl2 . 2.3060(10) y Pd Cl1 . 2.3110(10) y C1 N . 1.478(4) y C1 H1 . .95(4) no C1 H2 . .87(4) no C1 H3 . .97(6) no N C1 2_655 1.478(4) no N H4 . .96(4) no 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_site_symmetry_1 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag Cl2 Pd Cl1 Pd 5 2 122.41(3) y