#------------------------------------------------------------------------------ #$Date: 2018-09-01 00:18:24 +0100 (Sat, 01 Sep 2018) $ #$Revision: 210276 $ #$URL: svn://www.crystallography.net/cod/cif/4/30/83/4308394.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_4308394 loop_ _publ_author_name 'Bacchi, Alessia' 'Bosetti, Elsa' 'Carcelli, Mauro' 'Pelagatti, Paolo' 'Rogolino, Dominga' 'Pelizzi, Giancarlo' _publ_section_title ; "Venetian Blinds" Mechanism of Solvation/Desolvation in Palladium(II) Wheel-and-Axle Organic--Inorganic Diols ; _journal_coden_ASTM INOCAJ _journal_issue 2 _journal_name_full 'Inorganic Chemistry' _journal_page_first 431 _journal_page_last 442 _journal_paper_doi 10.1021/ic048896m _journal_volume 44 _journal_year 2005 _chemical_formula_sum 'C40 H42 Cl2 N2 O4 Pd S2' _chemical_formula_weight 856.18 _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' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 106.166(2) _cell_angle_gamma 90.00 _cell_formula_units_Z 2 _cell_length_a 7.6906(3) _cell_length_b 18.5017(8) _cell_length_c 14.5046(5) _cell_measurement_temperature 293(2) _cell_volume 1982.24(14) _computing_cell_refinement ; SAINT: SAX, Area Detector Integration, Siemens Analytical instruments INC., Madison, Wisconsin, USA. ; _computing_data_collection ; SAINT: SAX, Area Detector Integration, Siemens Analytical instruments INC., Madison, Wisconsin, USA. ; _computing_data_reduction ; SAINT: SAX, Area Detector Integration, Siemens Analytical instruments INC., Madison, Wisconsin, USA. SADABS: Siemens Area Detector Absorption Correction Software, Sheldrick G., 1996, University of Goettingen, Germany. ; _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'PARST - M. Nardelli, J. Appl. Crystallogr. 1995, 28, 659' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SIR97 (Altomare et al., 1997)' _diffrn_ambient_temperature 293(2) _diffrn_detector_area_resol_mean 8.2 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device_type 'Bruker AXS CCD diffractometer' _diffrn_measurement_method '\w scan' _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 0.0269 _diffrn_reflns_av_sigmaI/netI 0.0214 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 27199 _diffrn_reflns_theta_full 28.71 _diffrn_reflns_theta_max 28.71 _diffrn_reflns_theta_min 1.83 _exptl_absorpt_coefficient_mu 0.750 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_correction_T_min 0.860402 _exptl_absorpt_correction_type 'symmetry related measurements' _exptl_absorpt_process_details 'as implemented in SAINT+/SADABS package' _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.434 _exptl_crystal_density_method 'not measured' _exptl_crystal_description prism _exptl_crystal_F_000 880 _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.06 _refine_diff_density_max 1.013 _refine_diff_density_min -0.626 _refine_diff_density_rms 0.060 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 294 _refine_ls_number_reflns 5123 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.042 _refine_ls_R_factor_all 0.0411 _refine_ls_R_factor_gt 0.0307 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0581P)^2^+0.2277P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0881 _refine_ls_wR_factor_ref 0.0933 _reflns_number_gt 4115 _reflns_number_total 5123 _reflns_threshold_expression >2sigma(I) _cod_data_source_file ic048896msi20040811_044420_03.cif _cod_data_source_block 3 _cod_original_cell_volume 1982.24(13) _cod_database_code 4308394 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_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 Pd Pd 0.0000 0.0000 0.5000 0.03140(8) Uani 1 2 d S . . Cl Cl 0.27042(7) -0.03723(3) 0.60271(4) 0.04864(14) Uani 1 1 d . . . N1 N -0.1220(2) -0.09241(9) 0.52519(12) 0.0339(3) Uani 1 1 d . . . O1 O -0.6072(2) -0.26117(9) 0.52647(14) 0.0528(4) Uani 1 1 d . . . O2 O -0.8596(3) -0.36721(12) 0.49177(15) 0.0722(6) Uani 1 1 d . . . S S -1.00190(9) -0.38429(4) 0.40024(6) 0.05820(17) Uani 1 1 d . . . C1 C -0.4278(3) -0.28693(10) 0.54055(15) 0.0383(4) Uani 1 1 d . . . C2 C -0.3138(3) -0.21887(10) 0.53802(14) 0.0340(4) Uani 1 1 d . . . C3 C -0.3782(3) -0.15122(11) 0.55453(15) 0.0375(4) Uani 1 1 d . . . C4 C -0.2811(3) -0.09004(11) 0.54693(15) 0.0377(4) Uani 1 1 d . . . C5 C -0.0560(3) -0.15767(11) 0.51330(16) 0.0376(4) Uani 1 1 d . . . C6 C -0.1465(3) -0.22079(11) 0.51854(16) 0.0393(4) Uani 1 1 d . . . C7 C -0.4249(3) -0.33779(11) 0.45719(14) 0.0365(4) Uani 1 1 d . . . C8 C -0.4034(3) -0.41221(11) 0.46848(17) 0.0425(5) Uani 1 1 d . . . C9 C -0.4176(4) -0.45678(13) 0.38995(19) 0.0517(6) Uani 1 1 d . . . C10 C -0.4533(4) -0.42764(15) 0.29860(19) 0.0561(6) Uani 1 1 d . . . C11 C -0.4735(4) -0.35418(17) 0.28684(19) 0.0579(7) Uani 1 1 d . . . C12 C -0.4608(3) -0.30933(13) 0.36502(16) 0.0489(5) Uani 1 1 d . . . C13 C -0.3580(4) -0.32345(12) 0.63980(17) 0.0520(6) Uani 1 1 d . . . C14 C -0.1814(6) -0.34165(16) 0.6785(2) 0.0714(9) Uani 1 1 d . . . C15 C -0.1238(9) -0.37627(19) 0.7679(3) 0.1018(17) Uani 1 1 d . . . C16 C -0.2443(11) -0.3924(2) 0.8176(3) 0.116(2) Uani 1 1 d . . . C17 C -0.4235(12) -0.3764(2) 0.7788(3) 0.108(2) Uani 1 1 d . . . C18 C -0.4837(7) -0.34136(17) 0.6906(2) 0.0749(10) Uani 1 1 d . . . C19 C -0.9464(6) -0.4696(2) 0.3627(3) 0.1064(15) Uani 1 1 d . . . H19A H -0.8261 -0.4682 0.3555 0.160 Uiso 1 1 calc R . . H19B H -1.0307 -0.4819 0.3024 0.160 Uiso 1 1 calc R . . H19C H -0.9522 -0.5053 0.4098 0.160 Uiso 1 1 calc R . . C20 C -0.9605(7) -0.3302(2) 0.3091(3) 0.1042(13) Uani 1 1 d . . . H20A H -0.9659 -0.2802 0.3255 0.156 Uiso 1 1 calc R . . H20B H -1.0504 -0.3399 0.2497 0.156 Uiso 1 1 calc R . . H20C H -0.8426 -0.3410 0.3023 0.156 Uiso 1 1 calc R . . H5 H 0.031(3) -0.1582(14) 0.5012(15) 0.032(7) Uiso 1 1 d . . . H6 H -0.483(4) -0.1479(14) 0.5665(18) 0.050(7) Uiso 1 1 d . . . H4 H -0.322(3) -0.0451(14) 0.5589(16) 0.041(6) Uiso 1 1 d . . . H3 H -0.094(3) -0.2616(13) 0.5044(17) 0.039(6) Uiso 1 1 d . . . H12 H -0.477(4) -0.2552(15) 0.3536(18) 0.053(7) Uiso 1 1 d . . . H8 H -0.373(3) -0.4303(14) 0.5325(19) 0.051(7) Uiso 1 1 d . . . H10 H -0.462(4) -0.4582(17) 0.242(2) 0.073(9) Uiso 1 1 d . . . H11 H -0.480(4) -0.3373(17) 0.230(2) 0.071(9) Uiso 1 1 d . . . H9 H -0.391(4) -0.5145(17) 0.400(2) 0.068(9) Uiso 1 1 d . . . H1O H -0.685(4) -0.2951(17) 0.511(2) 0.066(9) Uiso 1 1 d . . . H14 H -0.102(4) -0.3355(15) 0.649(2) 0.047(8) Uiso 1 1 d . . . H15 H -0.023(6) -0.388(2) 0.792(3) 0.095(15) Uiso 1 1 d . . . H16 H -0.206(5) -0.418(2) 0.882(3) 0.108(13) Uiso 1 1 d . . . H18 H -0.604(6) -0.331(2) 0.662(3) 0.100(14) Uiso 1 1 d . . . H17 H -0.494(6) -0.389(2) 0.802(3) 0.098(15) 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 Pd 0.03597(12) 0.02465(11) 0.03406(12) 0.00045(7) 0.01052(8) -0.00242(8) Cl 0.0408(3) 0.0473(3) 0.0531(3) 0.0125(2) 0.0053(2) 0.0009(2) N1 0.0379(8) 0.0275(7) 0.0369(8) 0.0009(6) 0.0112(7) -0.0024(6) O1 0.0491(9) 0.0415(9) 0.0748(12) -0.0096(8) 0.0291(9) -0.0106(7) O2 0.0763(13) 0.0765(13) 0.0650(12) -0.0165(10) 0.0214(10) -0.0312(11) S 0.0470(3) 0.0530(4) 0.0763(4) -0.0086(3) 0.0201(3) -0.0059(3) C1 0.0471(11) 0.0283(9) 0.0412(11) -0.0009(8) 0.0152(9) -0.0060(8) C2 0.0414(10) 0.0279(9) 0.0322(9) 0.0005(7) 0.0096(8) -0.0044(7) C3 0.0389(10) 0.0316(9) 0.0448(11) -0.0002(8) 0.0165(9) -0.0022(8) C4 0.0442(11) 0.0260(9) 0.0453(11) -0.0015(8) 0.0163(9) 0.0004(8) C5 0.0383(10) 0.0335(10) 0.0445(11) -0.0012(8) 0.0172(9) -0.0015(8) C6 0.0461(11) 0.0263(9) 0.0467(11) -0.0034(8) 0.0151(9) 0.0005(8) C7 0.0386(10) 0.0338(9) 0.0365(10) -0.0015(8) 0.0095(8) -0.0077(8) C8 0.0529(12) 0.0324(10) 0.0460(12) -0.0008(9) 0.0202(10) -0.0083(9) C9 0.0618(14) 0.0374(11) 0.0634(15) -0.0122(10) 0.0299(12) -0.0138(10) C10 0.0581(14) 0.0620(16) 0.0515(14) -0.0215(12) 0.0206(11) -0.0174(12) C11 0.0654(16) 0.0660(17) 0.0376(13) -0.0028(12) 0.0064(11) -0.0071(13) C12 0.0599(14) 0.0419(12) 0.0398(12) 0.0022(9) 0.0056(10) -0.0018(11) C13 0.0900(19) 0.0289(10) 0.0376(11) -0.0050(8) 0.0188(12) -0.0152(11) C14 0.095(3) 0.0491(15) 0.0576(17) 0.0103(13) 0.0007(17) -0.0117(16) C15 0.156(4) 0.0501(18) 0.065(2) 0.0081(15) -0.025(3) -0.010(2) C16 0.239(7) 0.0504(18) 0.0413(18) 0.0043(14) 0.012(3) -0.032(3) C17 0.213(6) 0.075(2) 0.050(2) -0.0038(17) 0.060(3) -0.035(3) C18 0.127(3) 0.0567(17) 0.0545(16) -0.0059(13) 0.047(2) -0.0193(19) C19 0.119(3) 0.082(2) 0.094(3) -0.035(2) -0.010(2) 0.035(2) C20 0.127(3) 0.109(3) 0.078(2) 0.013(2) 0.030(2) -0.023(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' 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' O O 0.0106 0.0060 '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' S S 0.1246 0.1234 '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 N1 Pd N1 180.00(5) 3_556 . ? N1 Pd Cl 89.36(5) 3_556 . ? N1 Pd Cl 90.64(5) . . ? N1 Pd Cl 90.64(5) 3_556 3_556 ? N1 Pd Cl 89.36(5) . 3_556 ? Cl Pd Cl 180.00(3) . 3_556 ? C5 N1 C4 117.47(17) . . ? C5 N1 Pd 121.64(14) . . ? C4 N1 Pd 120.67(13) . . ? O2 S C20 107.81(17) . . ? O2 S C19 106.41(17) . . ? C20 S C19 99.7(2) . . ? O1 C1 C7 108.59(17) . . ? O1 C1 C2 105.01(16) . . ? C7 C1 C2 110.40(16) . . ? O1 C1 C13 110.66(19) . . ? C7 C1 C13 112.82(17) . . ? C2 C1 C13 109.09(17) . . ? C3 C2 C6 116.83(18) . . ? C3 C2 C1 119.92(18) . . ? C6 C2 C1 123.24(18) . . ? C4 C3 C2 119.9(2) . . ? N1 C4 C3 122.72(19) . . ? N1 C5 C6 122.9(2) . . ? C5 C6 C2 120.08(19) . . ? C8 C7 C12 118.2(2) . . ? C8 C7 C1 122.73(18) . . ? C12 C7 C1 118.81(19) . . ? C9 C8 C7 120.9(2) . . ? C10 C9 C8 120.3(2) . . ? C11 C10 C9 119.3(2) . . ? C10 C11 C12 120.7(3) . . ? C11 C12 C7 120.6(2) . . ? C14 C13 C18 118.6(3) . . ? C14 C13 C1 122.8(2) . . ? C18 C13 C1 118.6(3) . . ? C13 C14 C15 121.1(4) . . ? C16 C15 C14 120.3(5) . . ? C15 C16 C17 119.5(4) . . ? C16 C17 C18 121.2(5) . . ? C17 C18 C13 119.3(5) . . ? 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 Pd N1 2.0318(16) 3_556 ? Pd N1 2.0318(16) . ? Pd Cl 2.3009(5) . ? Pd Cl 2.3009(5) 3_556 ? N1 C5 1.340(3) . ? N1 C4 1.346(3) . ? O1 C1 1.420(3) . ? O2 S 1.500(2) . ? S C20 1.756(4) . ? S C19 1.761(4) . ? C1 C7 1.537(3) . ? C1 C2 1.541(3) . ? C1 C13 1.545(3) . ? C2 C3 1.391(3) . ? C2 C6 1.392(3) . ? C3 C4 1.378(3) . ? C5 C6 1.373(3) . ? C7 C8 1.391(3) . ? C7 C12 1.391(3) . ? C8 C9 1.386(3) . ? C9 C10 1.385(4) . ? C10 C11 1.373(4) . ? C11 C12 1.387(4) . ? C13 C14 1.359(5) . ? C13 C18 1.408(4) . ? C14 C15 1.403(5) . ? C15 C16 1.357(8) . ? C16 C17 1.368(8) . ? C17 C18 1.394(6) . ? 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 O1 H1O O2 0.86(3) 1.86(3) 2.707(3) 173(3) . C12 H12 C15 1.02(3) 2.82(3) 3.790(4) 159(2) 4 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 C4 N1 N1 C5 5.5(3) . . 3_556 3_556 ? O1 C1 C2 C3 20.3(2) . . . . ? O1 C1 C1 O1 180.0 . . 3_556 3_556 ? C3 C2 C1 O1 20.3(2) . . . . ? C12 C7 C1 O1 65.6(2) . . . . ? C18 C13 C1 O1 14.3(3) . . . . ?