#------------------------------------------------------------------------------ #$Date: 2016-03-26 16:33:12 +0200 (Sat, 26 Mar 2016) $ #$Revision: 180342 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/20/11/7201147.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_7201147 loop_ _publ_author_name 'Peuronen, Anssi' 'Lahtinen, Manu' 'Valkonen, Jussi' _publ_section_title ; The conformational polymorphism and weak interactions in solid state structures of ten new monomeric and dimeric substituted dibenzyldimethylammonium chloridopalladate salts ; _journal_issue 11 _journal_name_full CrystEngComm _journal_page_first 2344 _journal_paper_doi 10.1039/b905421a _journal_volume 11 _journal_year 2009 _chemical_formula_moiety '2(C16 H20 N), Cl4 Pd' _chemical_formula_sum 'C32 H40 Cl4 N2 Pd' _chemical_formula_weight 700.86 _chemical_name_systematic ; ? ; _space_group_IT_number 2 _symmetry_cell_setting triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 63.85(3) _cell_angle_beta 82.50(3) _cell_angle_gamma 65.19(3) _cell_formula_units_Z 1 _cell_length_a 8.6420(17) _cell_length_b 10.201(2) _cell_length_c 10.998(2) _cell_measurement_temperature 153(2) _cell_volume 788.2(4) _computing_cell_refinement DENZO-SMN _computing_data_collection Collect _computing_data_reduction DENZO-SMN _computing_molecular_graphics 'Diamond 3.0' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution SHELXS-97 _diffrn_ambient_temperature 153(2) _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.996 _diffrn_measurement_device_type 'Kappa APEX II' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0415 _diffrn_reflns_av_sigmaI/netI 0.0581 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_number 11388 _diffrn_reflns_theta_full 28.78 _diffrn_reflns_theta_max 28.78 _diffrn_reflns_theta_min 2.07 _exptl_absorpt_coefficient_mu 0.952 _exptl_absorpt_correction_T_max 0.8037 _exptl_absorpt_correction_T_min 0.7504 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Denzo (Z. Otwinowski, 2003)' _exptl_crystal_colour Yellow _exptl_crystal_density_diffrn 1.476 _exptl_crystal_density_method 'not measured' _exptl_crystal_description Block _exptl_crystal_F_000 360 _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.24 _refine_diff_density_max 0.373 _refine_diff_density_min -0.550 _refine_diff_density_rms 0.091 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 180 _refine_ls_number_reflns 4087 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.048 _refine_ls_R_factor_all 0.0481 _refine_ls_R_factor_gt 0.0380 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0218P)^2^+0.4361P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0778 _refine_ls_wR_factor_ref 0.0816 _reflns_number_gt 3483 _reflns_number_total 4087 _reflns_threshold_expression >2\s(I) _cod_data_source_file b905421a.txt _cod_data_source_block 1b _cod_original_cell_volume 788.3(3) _cod_database_code 7201147 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 1.0000 0.5000 0.5000 0.02042(8) Uani 1 2 d S . . Cl2 Cl 1.19423(8) 0.23638(7) 0.57795(7) 0.02873(15) Uani 1 1 d . . . Cl1 Cl 0.83225(8) 0.43826(8) 0.68070(7) 0.02923(15) Uani 1 1 d . . . N1 N 0.6948(3) 0.1624(2) 0.5834(2) 0.0223(4) Uani 1 1 d . . . C31 C 0.5944(3) 0.1849(3) 0.7039(3) 0.0252(5) Uani 1 1 d . . . H31A H 0.5987 0.2773 0.7100 0.030 Uiso 1 1 calc R . . H31B H 0.4732 0.2108 0.6862 0.030 Uiso 1 1 calc R . . C12 C 0.8813(3) 0.1059(3) 0.6141(3) 0.0255(5) Uani 1 1 d . . . H12A H 0.9237 -0.0015 0.6891 0.038 Uiso 1 1 calc R . . H12B H 0.8993 0.1792 0.6398 0.038 Uiso 1 1 calc R . . H12C H 0.9432 0.1028 0.5334 0.038 Uiso 1 1 calc R . . C21 C 0.6283(3) 0.3265(3) 0.4622(3) 0.0258(5) Uani 1 1 d . . . H21A H 0.5025 0.3671 0.4517 0.031 Uiso 1 1 calc R . . H21B H 0.6541 0.4008 0.4827 0.031 Uiso 1 1 calc R . . C22 C 0.7005(3) 0.3298(3) 0.3291(3) 0.0271(6) Uani 1 1 d . . . C32 C 0.6595(3) 0.0418(3) 0.8377(3) 0.0255(5) Uani 1 1 d . . . C11 C 0.6653(4) 0.0439(3) 0.5552(3) 0.0299(6) Uani 1 1 d . . . H11A H 0.7236 0.0362 0.4744 0.045 Uiso 1 1 calc R . . H11B H 0.5425 0.0788 0.5393 0.045 Uiso 1 1 calc R . . H11C H 0.7104 -0.0609 0.6332 0.045 Uiso 1 1 calc R . . C34 C 0.6704(4) -0.2145(3) 1.0044(3) 0.0332(6) Uani 1 1 d . . . H34 H 0.6385 -0.3014 1.0310 0.040 Uiso 1 1 calc R . . C37 C 0.7674(3) 0.0364(3) 0.9260(3) 0.0296(6) Uani 1 1 d . . . H37 H 0.8011 0.1221 0.8995 0.036 Uiso 1 1 calc R . . C36 C 0.8252(4) -0.0924(4) 1.0510(3) 0.0340(6) Uani 1 1 d . . . H36 H 0.8973 -0.0943 1.1106 0.041 Uiso 1 1 calc R . . C25 C 0.8274(4) 0.3415(3) 0.0795(3) 0.0407(7) Uani 1 1 d . . . H25 H 0.8717 0.3440 -0.0049 0.049 Uiso 1 1 calc R . . C35 C 0.7782(3) -0.2192(4) 1.0899(3) 0.0333(6) Uani 1 1 d . . . H35 H 0.8200 -0.3089 1.1752 0.040 Uiso 1 1 calc R . . C23 C 0.8512(4) 0.3510(3) 0.2897(3) 0.0306(6) Uani 1 1 d . . . H23 H 0.9116 0.3618 0.3485 0.037 Uiso 1 1 calc R . . C33 C 0.6083(3) -0.0839(3) 0.8799(3) 0.0294(6) Uani 1 1 d . . . H33 H 0.5308 -0.0799 0.8232 0.035 Uiso 1 1 calc R . . C24 C 0.9141(4) 0.3564(3) 0.1664(3) 0.0366(7) Uani 1 1 d . . . H24 H 1.0174 0.3705 0.1412 0.044 Uiso 1 1 calc R . . C27 C 0.6117(4) 0.3174(4) 0.2393(3) 0.0367(7) Uani 1 1 d . . . H27 H 0.5073 0.3052 0.2633 0.044 Uiso 1 1 calc R . . C26 C 0.6760(4) 0.3228(4) 0.1157(3) 0.0422(8) Uani 1 1 d . . . H26 H 0.6158 0.3137 0.0556 0.051 Uiso 1 1 calc R . . 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 Pd1 0.01427(13) 0.02465(15) 0.02754(16) -0.01636(12) 0.00053(10) -0.00678(11) Cl2 0.0184(3) 0.0266(3) 0.0420(4) -0.0182(3) 0.0004(3) -0.0057(3) Cl1 0.0230(3) 0.0333(3) 0.0322(4) -0.0168(3) 0.0054(3) -0.0103(3) N1 0.0161(10) 0.0249(11) 0.0309(12) -0.0188(10) 0.0028(8) -0.0058(8) C31 0.0162(12) 0.0330(14) 0.0346(15) -0.0239(12) 0.0065(10) -0.0085(11) C12 0.0150(12) 0.0294(13) 0.0318(14) -0.0156(12) 0.0034(10) -0.0068(10) C21 0.0214(13) 0.0245(13) 0.0301(14) -0.0161(11) -0.0013(10) -0.0025(10) C22 0.0247(13) 0.0234(13) 0.0290(14) -0.0145(11) -0.0039(11) -0.0009(11) C32 0.0171(12) 0.0320(14) 0.0313(14) -0.0197(12) 0.0053(10) -0.0080(10) C11 0.0289(14) 0.0360(15) 0.0407(16) -0.0290(14) 0.0064(12) -0.0152(12) C34 0.0261(14) 0.0366(15) 0.0408(17) -0.0204(14) 0.0079(12) -0.0139(12) C37 0.0212(13) 0.0399(16) 0.0365(16) -0.0231(13) 0.0062(11) -0.0142(12) C36 0.0230(14) 0.0502(18) 0.0317(15) -0.0213(14) 0.0014(11) -0.0134(13) C25 0.0466(19) 0.0364(16) 0.0329(16) -0.0199(14) 0.0061(14) -0.0071(14) C35 0.0239(14) 0.0397(16) 0.0332(15) -0.0167(13) 0.0046(12) -0.0099(12) C23 0.0293(15) 0.0286(14) 0.0353(16) -0.0151(13) -0.0023(12) -0.0102(12) C33 0.0218(13) 0.0402(16) 0.0356(15) -0.0244(13) 0.0055(11) -0.0131(12) C24 0.0300(15) 0.0317(15) 0.0373(17) -0.0098(13) 0.0039(13) -0.0088(12) C27 0.0301(15) 0.0482(18) 0.0373(16) -0.0237(15) 0.0006(12) -0.0146(14) C26 0.0449(19) 0.0541(19) 0.0369(17) -0.0296(16) -0.0010(14) -0.0166(16) 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 _geom_angle_publ_flag Cl2 Pd1 Cl2 180.0 2_766 . ? Cl2 Pd1 Cl1 88.24(4) 2_766 . ? Cl2 Pd1 Cl1 91.76(4) . . ? Cl2 Pd1 Cl1 91.76(4) 2_766 2_766 ? Cl2 Pd1 Cl1 88.24(4) . 2_766 ? Cl1 Pd1 Cl1 180.000(1) . 2_766 ? C11 N1 C12 109.67(19) . . ? C11 N1 C21 110.54(19) . . ? C12 N1 C21 110.2(2) . . ? C11 N1 C31 110.35(19) . . ? C12 N1 C31 109.90(19) . . ? C21 N1 C31 106.15(18) . . ? C32 C31 N1 114.1(2) . . ? C32 C31 H31A 108.7 . . ? N1 C31 H31A 108.7 . . ? C32 C31 H31B 108.7 . . ? N1 C31 H31B 108.7 . . ? H31A C31 H31B 107.6 . . ? N1 C12 H12A 109.5 . . ? N1 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? N1 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C22 C21 N1 115.22(19) . . ? C22 C21 H21A 108.5 . . ? N1 C21 H21A 108.5 . . ? C22 C21 H21B 108.5 . . ? N1 C21 H21B 108.5 . . ? H21A C21 H21B 107.5 . . ? C23 C22 C27 118.5(3) . . ? C23 C22 C21 121.7(2) . . ? C27 C22 C21 119.8(3) . . ? C33 C32 C37 118.8(3) . . ? C33 C32 C31 121.4(2) . . ? C37 C32 C31 119.7(2) . . ? N1 C11 H11A 109.5 . . ? N1 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? N1 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C35 C34 C33 120.5(3) . . ? C35 C34 H34 119.7 . . ? C33 C34 H34 119.7 . . ? C36 C37 C32 120.6(3) . . ? C36 C37 H37 119.7 . . ? C32 C37 H37 119.7 . . ? C37 C36 C35 120.1(3) . . ? C37 C36 H36 120.0 . . ? C35 C36 H36 120.0 . . ? C24 C25 C26 119.8(3) . . ? C24 C25 H25 120.1 . . ? C26 C25 H25 120.1 . . ? C34 C35 C36 119.8(3) . . ? C34 C35 H35 120.1 . . ? C36 C35 H35 120.1 . . ? C24 C23 C22 120.9(3) . . ? C24 C23 H23 119.5 . . ? C22 C23 H23 119.5 . . ? C34 C33 C32 120.1(3) . . ? C34 C33 H33 120.0 . . ? C32 C33 H33 120.0 . . ? C23 C24 C25 120.3(3) . . ? C23 C24 H24 119.9 . . ? C25 C24 H24 119.9 . . ? C26 C27 C22 120.1(3) . . ? C26 C27 H27 119.9 . . ? C22 C27 H27 119.9 . . ? C25 C26 C27 120.4(3) . . ? C25 C26 H26 119.8 . . ? C27 C26 H26 119.8 . . ? 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 Cl2 2.3108(13) 2_766 ? Pd1 Cl2 2.3108(13) . ? Pd1 Cl1 2.3150(10) . ? Pd1 Cl1 2.3150(10) 2_766 ? N1 C11 1.494(3) . ? N1 C12 1.494(3) . ? N1 C21 1.528(3) . ? N1 C31 1.537(3) . ? C31 C32 1.499(4) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C21 C22 1.507(3) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C23 1.391(4) . ? C22 C27 1.404(4) . ? C32 C33 1.398(4) . ? C32 C37 1.400(4) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C34 C35 1.381(4) . ? C34 C33 1.386(4) . ? C34 H34 0.9500 . ? C37 C36 1.379(4) . ? C37 H37 0.9500 . ? C36 C35 1.389(4) . ? C36 H36 0.9500 . ? C25 C24 1.381(4) . ? C25 C26 1.383(4) . ? C25 H25 0.9500 . ? C35 H35 0.9500 . ? C23 C24 1.380(4) . ? C23 H23 0.9500 . ? C33 H33 0.9500 . ? C24 H24 0.9500 . ? C27 C26 1.386(4) . ? C27 H27 0.9500 . ? C26 H26 0.9500 . ? 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 _geom_torsion_publ_flag C11 N1 C31 C32 68.7(3) . . . . ? C12 N1 C31 C32 -52.3(3) . . . . ? C21 N1 C31 C32 -171.5(2) . . . . ? C11 N1 C21 C22 -55.9(3) . . . . ? C12 N1 C21 C22 65.5(3) . . . . ? C31 N1 C21 C22 -175.6(2) . . . . ? N1 C21 C22 C23 -87.8(3) . . . . ? N1 C21 C22 C27 94.6(3) . . . . ? N1 C31 C32 C33 -84.5(3) . . . . ? N1 C31 C32 C37 98.7(3) . . . . ? C33 C32 C37 C36 1.5(4) . . . . ? C31 C32 C37 C36 178.3(2) . . . . ? C32 C37 C36 C35 0.7(4) . . . . ? C33 C34 C35 C36 -0.2(4) . . . . ? C37 C36 C35 C34 -1.4(4) . . . . ? C27 C22 C23 C24 -1.3(4) . . . . ? C21 C22 C23 C24 -178.9(2) . . . . ? C35 C34 C33 C32 2.4(4) . . . . ? C37 C32 C33 C34 -3.0(4) . . . . ? C31 C32 C33 C34 -179.8(2) . . . . ? C22 C23 C24 C25 0.3(4) . . . . ? C26 C25 C24 C23 0.7(5) . . . . ? C23 C22 C27 C26 1.3(4) . . . . ? C21 C22 C27 C26 179.0(3) . . . . ? C24 C25 C26 C27 -0.7(5) . . . . ? C22 C27 C26 C25 -0.4(5) . . . . ?