#------------------------------------------------------------------------------ #$Date: 2013-08-29 16:37:19 +0100 (Thu, 29 Aug 2013) $ #$Revision: 88064 $ #$URL: svn://www.crystallography.net/cod/cif/2/01/13/2011314.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_2011314 loop_ _publ_author_name 'Decken, Andreas' 'Gisia L. Pisegna' 'Christopher M. Vogels' 'Stephen A. Westcott' _publ_section_title ; trans-Bis(benzylamine)dichloropalladium(II) bis(dimethyl sulfoxide) solvate ; _journal_issue 9 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 1071 _journal_page_last 1072 _journal_volume 56 _journal_year 2000 _chemical_formula_iupac '[PdCl2 (C7 H9 N)2 ] , 2C2 H6 OS ' _chemical_formula_moiety 'C14 H18 Cl2 N2 Pd , 2C2 H6 OS' _chemical_formula_sum 'C18 H30 Cl2 N2 O2 Pd S2' _chemical_formula_weight 547.86 _chemical_name_systematic ' Trans-Dichlorodibenzylaminepalladium(II)' _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _cell_angle_alpha 90.00 _cell_angle_beta 109.700(10) _cell_angle_gamma 90.00 _cell_formula_units_Z 2 _cell_length_a 7.242(2) _cell_length_b 16.187(5) _cell_length_c 10.596(3) _cell_measurement_reflns_used 12890 _cell_measurement_temperature 173.0(10) _cell_measurement_theta_max 30.64 _cell_measurement_theta_min 3 _cell_volume 1169.4(6) _computing_cell_refinement CrystalClear _computing_data_collection 'CrystalClear (Rigaku Corporation, 1999)' _computing_data_reduction CrystalClear _computing_molecular_graphics 'SHELXTL (Sheldrick, 1990)' _computing_publication_material SHELXTL _computing_structure_refinement 'SHELXL93 (Sheldrick, 1993)' _computing_structure_solution 'SHELXS86 (Sheldrick, 1990)' _diffrn_ambient_temperature 173.0(10) _diffrn_measured_fraction_theta_full 100 _diffrn_measurement_device 'Rigaku AFC8/Mercury CCD' _diffrn_measurement_method \w _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength .71073 _diffrn_reflns_av_R_equivalents .018 _diffrn_reflns_av_sigmaI/netI .0289 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_number 12890 _diffrn_reflns_theta_full 26.4 _diffrn_reflns_theta_max 30.64 _diffrn_reflns_theta_min 3.00 _diffrn_standards_decay_% 0 _diffrn_standards_number 'all frames' _exptl_absorpt_coefficient_mu 1.216 _exptl_absorpt_correction_T_max .864 _exptl_absorpt_correction_T_min .500 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details '(CrystalClear; Rigaku Corporation, 1999)' _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.556 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method none _exptl_crystal_description plate _exptl_crystal_F_000 560 _exptl_crystal_size_max .38 _exptl_crystal_size_mid .23 _exptl_crystal_size_min .12 _refine_diff_density_max .804 _refine_diff_density_min -.728 _refine_ls_extinction_coef .0117(18) _refine_ls_extinction_method 'SHELXL93 (Sheldrick, 1993)' _refine_ls_goodness_of_fit_all 1.093 _refine_ls_goodness_of_fit_ref 1.085 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 130 _refine_ls_number_reflns 3088 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.093 _refine_ls_restrained_S_obs 1.085 _refine_ls_R_factor_all .0355 _refine_ls_R_factor_gt .0256 _refine_ls_shift/esd_mean .000 _refine_ls_shift/su_max .001 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_scheme ; calc w = 1/[\s^2^(Fo^2^)+(0.0150P)^2^+1.2000P] where P=(Fo^2^+2Fc^2^)/3 ; _refine_ls_wR_factor_all .0641 _refine_ls_wR_factor_ref .0594 _reflns_number_gt 2703 _reflns_number_total 3088 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file fr1279.cif _[local]_cod_data_source_block I _[local]_cod_cif_authors_sg_H-M 'P 21/n' _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius The following automatic conversions were performed: '_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic' according to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana ; _cod_database_code 2011314 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -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 .01657(11) .01723(11) .01963(11) .00221(7) .00519(7) .00030(7) Cl .0254(2) .0296(2) .0239(2) .0025(2) .0051(2) -.0044(2) N .0185(7) .0198(7) .0231(7) .0025(6) .0072(6) .0003(6) C2 .0206(9) .0201(8) .0308(9) .0010(7) .0095(7) .0028(7) C3 .0192(8) .0181(8) .0244(8) .0006(7) .0056(7) -.0017(7) C4 .0209(9) .0223(8) .0275(9) .0002(7) .0066(7) .0033(7) C5 .0220(9) .0280(10) .0368(11) .0004(8) .0123(8) -.0020(8) C6 .0237(9) .0263(9) .0355(11) .0059(8) .0045(8) -.0024(8) C7 .0322(10) .0199(8) .0257(9) .0047(8) .0028(8) .0010(7) C8 .0271(9) .0201(8) .0243(9) .0000(7) .0078(7) -.0002(7) S .0404(3) .0217(2) .0235(2) -.0029(2) -.0013(2) .0002(2) O .0256(7) .0302(7) .0261(7) -.0009(6) .0026(6) .0074(6) C9 .058(2) .0408(13) .0317(11) .0018(12) .0195(11) .0056(10) C10 .0324(12) .0331(11) .0434(13) .0027(9) .0027(10) .0103(10) 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 .0000 .0000 .5000 .01804(8) Uani d S 1 . Pd Cl .14461(7) .05561(3) .71091(5) .02712(12) Uani d . 1 . Cl N -.2573(2) .05810(9) .4856(2) .0204(3) Uani d . 1 . N H1A -.2860 .04779 .5603 .033(3) Uiso d R 1 . H H1B -.3543 .03678 .4157 .033(3) Uiso d R 1 . H C2 -.2506(3) .14866(12) .4676(2) .0236(4) Uani d . 1 . C H2A -.2090 .15930 .3922 .033(3) Uiso d R 1 . H H2B -.1533 .17154 .5454 .033(3) Uiso d R 1 . H C3 -.4421(3) .19311(11) .4458(2) .0210(3) Uani d . 1 . C C4 -.5670(3) .17323(12) .5166(2) .0239(4) Uani d . 1 . C H4A -.5337 .12874 .5802 .032(3) Uiso d R 1 . H C5 -.7397(3) .21723(13) .4957(2) .0283(4) Uani d . 1 . C H5A -.8246 .20288 .5451 .032(3) Uiso d R 1 . H C6 -.7902(3) .28194(13) .4040(2) .0299(4) Uani d . 1 . C H6A -.9102 .31183 .3891 .032(3) Uiso d R 1 . H C7 -.6658(3) .30282(12) .3344(2) .0277(4) Uani d . 1 . C H7A -.6990 .34773 .2716 .032(3) Uiso d R 1 . H C8 -.4932(3) .25890(12) .3552(2) .0241(4) Uani d . 1 . C H8A -.4077 .27401 .3067 .032(3) Uiso d R 1 . H S -.25387(9) -.02443(3) .85229(5) .03160(13) Uani d . 1 . S O -.3700(2) .00169(9) .71130(15) .0289(3) Uani d . 1 . O C9 -.4180(4) -.0858(2) .9076(2) .0425(6) Uani d . 1 . C H9A -.5335 -.0543 .9001 .062(4) Uiso calc R 1 . H H9B -.3543 -.1016 .9994 .062(4) Uiso calc R 1 . H H9C -.4541 -.1345 .8529 .062(4) Uiso calc R 1 . H C10 -.0956(4) -.10537(15) .8374(3) .0388(5) Uani d . 1 . C H10A .0000 -.0835 .8020 .062(4) Uiso calc R 1 . H H10B -.1714 -.1472 .7782 .062(4) Uiso calc R 1 . H H10C -.0301 -.1290 .9241 .062(4) Uiso calc R 1 . H 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 N . 2.046(2) yes Pd N 3_556 2.046(2) yes Pd Cl . 2.3072(7) yes Pd Cl 3_556 2.3072(7) yes N C2 . 1.481(2) yes C2 C3 . 1.510(3) yes C3 C4 . 1.393(3) no C3 C8 . 1.397(3) no C4 C5 . 1.390(3) no C5 C6 . 1.392(3) no C6 C7 . 1.384(3) no C7 C8 . 1.390(3) no S O . 1.507(2) no S C10 . 1.782(3) no S C9 . 1.793(3) no loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N .0061 .0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl .1484 .1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S .1246 .1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O .0106 .0060 '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 N Pd N . 3_556 180.0 yes N Pd Cl . . 89.86(5) yes N Pd Cl 3_556 . 90.14(5) yes N Pd Cl . 3_556 90.14(5) no N Pd Cl 3_556 3_556 89.86(5) no Cl Pd Cl . 3_556 180.0 yes C2 N Pd . . 113.33(12) no N C2 C3 . . 115.0(2) yes C4 C3 C8 . . 118.4(2) no C4 C3 C2 . . 122.5(2) no C8 C3 C2 . . 119.0(2) no C5 C4 C3 . . 120.6(2) no C4 C5 C6 . . 120.5(2) no C7 C6 C5 . . 119.4(2) no C6 C7 C8 . . 120.2(2) no C7 C8 C3 . . 121.0(2) no O S C10 . . 106.21(11) no O S C9 . . 105.65(12) no C10 S C9 . . 97.96(13) no 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 N H1A O ? .900 2.035 2.922(2) 168.24 no N H1B O 2_555 .900 2.092 2.963(2) 162.69 no C10 H10A Cl ? .900 2.789 3.631(3) 146.96 no _cod_database_fobs_code 2011314