#------------------------------------------------------------------------------ #$Date: 2011-09-10 06:16:28 +0300 (Sat, 10 Sep 2011) $ #$Revision: 25271 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/2009005.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_2009005 loop_ _publ_author_name 'Vila, J. M.' 'Ortigueira, J. M.' 'L\'opez, M.' 'Fern\'andez, J. J.' 'Fern\'andez, A.' _publ_section_title ; Dibromo[propane-1,3-diylbis(diphenylphosphine)-P,P']palladium(II) ; _journal_issue 10 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 1646 _journal_page_last 1647 _journal_volume 55 _journal_year 1999 _chemical_formula_iupac '[Pd Br2 (C27 H26 P2)]' _chemical_formula_moiety 'C27 H26 Br2 P2 Pd' _chemical_formula_sum 'C27 H26 Br2 P2 Pd' _chemical_formula_weight 678.64 _chemical_name_systematic ; Dibromo[1,3-propanediylbis(diphenylphosphine)-P,P']palladium(II) ; _space_group_IT_number 2 _symmetry_cell_setting triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _cell_angle_alpha 88.617(13) _cell_angle_beta 80.841(11) _cell_angle_gamma 73.689(11) _cell_formula_units_Z 2 _cell_length_a 8.6829(13) _cell_length_b 10.7510(16) _cell_length_c 14.420(2) _cell_measurement_reflns_used 25 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 18.0 _cell_measurement_theta_min 7.5 _cell_volume 1275.2(3) _computing_cell_refinement 'CAD-4 Software' _computing_data_collection 'CAD-4 Software (Enraf-Nonius, 1989)' _computing_data_reduction 'CAD-4 SDP (Frenz, 1978)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1995)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997b)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997a)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device_type 'Enraf-Nonius CAD-4' _diffrn_measurement_method \w/2\q _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 0.039 _diffrn_reflns_av_sigmaI/netI 0.1198 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_number 5526 _diffrn_reflns_theta_full 26.30 _diffrn_reflns_theta_max 26.3 _diffrn_reflns_theta_min 2.41 _diffrn_standards_decay_% <1 _diffrn_standards_interval_time 120 _diffrn_standards_number 2 _exptl_absorpt_coefficient_mu 4.001 _exptl_absorpt_correction_T_max 0.449 _exptl_absorpt_correction_T_min 0.337 _exptl_absorpt_correction_type '\y scan' _exptl_absorpt_process_details '(North et al., 1968)' _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.768 _exptl_crystal_density_method 'not measured' _exptl_crystal_description prism _exptl_crystal_F_000 668 _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _refine_diff_density_max 0.564 _refine_diff_density_min -1.100 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.985 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 289 _refine_ls_number_reflns 5173 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 0.985 _refine_ls_R_factor_all 0.137 _refine_ls_R_factor_gt 0.039 _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^)+(0.0378P)^2^] where P = (Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_ref 0.095 _reflns_number_gt 2965 _reflns_number_total 5173 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file cf1318.cif _[local]_cod_data_source_block cf1318 _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic' according to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. '_geom_bond_publ_flag' value 'Yes' changed to 'yes' according to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29 (4 times). '_geom_angle_publ_flag' value 'Yes' changed to 'yes' according to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29 (7 times). Automatic conversion script Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana ; _cod_original_cell_volume 1275.1(3) _cod_database_code 2009005 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_type_symbol Pd1 0.40052(5) 0.66115(4) 0.25632(3) 0.02336(13) Uani d . 1 Pd Br1 0.65985(8) 0.49501(7) 0.26698(5) 0.0508(2) Uani d . 1 Br Br2 0.54615(8) 0.82978(6) 0.22936(5) 0.04121(19) Uani d . 1 Br P1 0.26093(19) 0.51259(15) 0.28522(10) 0.0273(4) Uani d . 1 P P2 0.17722(19) 0.80930(14) 0.22180(10) 0.0275(4) Uani d . 1 P C1 0.0558(7) 0.5728(6) 0.3527(4) 0.0399(16) Uani d . 1 C H1A -0.0029 0.5102 0.3450 0.048 Uiso calc R 1 H H1B 0.0662 0.5743 0.4186 0.048 Uiso calc R 1 H C2 -0.0489(7) 0.7058(6) 0.3298(5) 0.0463(17) Uani d . 1 C H2A -0.0424 0.7682 0.3755 0.056 Uiso calc R 1 H H2B -0.1610 0.7031 0.3380 0.056 Uiso calc R 1 H C3 -0.0067(7) 0.7556(6) 0.2320(4) 0.0356(15) Uani d . 1 C H3A -0.0965 0.8273 0.2190 0.043 Uiso calc R 1 H H3B 0.0096 0.6871 0.1858 0.043 Uiso calc R 1 H C4 0.2398(7) 0.4443(5) 0.1755(4) 0.0294(13) Uani d . 1 C C5 0.1048(9) 0.4113(8) 0.1624(5) 0.070(3) Uani d . 1 C H5A 0.0191 0.4208 0.2119 0.084 Uiso calc R 1 H C6 0.0938(11) 0.3640(10) 0.0767(6) 0.093(3) Uani d . 1 C H6A -0.0004 0.3429 0.0693 0.111 Uiso calc R 1 H C7 0.2152(10) 0.3472(7) 0.0031(5) 0.059(2) Uani d . 1 C H7A 0.2056 0.3158 -0.0546 0.071 Uiso calc R 1 H C8 0.3510(10) 0.3775(8) 0.0159(5) 0.061(2) Uani d . 1 C H8A 0.4366 0.3658 -0.0338 0.074 Uiso calc R 1 H C9 0.3663(8) 0.4259(7) 0.1015(4) 0.052(2) Uani d . 1 C H9A 0.4614 0.4457 0.1088 0.063 Uiso calc R 1 H C10 0.3521(7) 0.3762(6) 0.3547(4) 0.0324(14) Uani d . 1 C C11 0.4071(8) 0.2514(6) 0.3189(4) 0.0418(16) Uani d . 1 C H11A 0.3954 0.2342 0.2579 0.050 Uiso calc R 1 H C12 0.4798(9) 0.1513(6) 0.3736(5) 0.0527(19) Uani d . 1 C H12A 0.5189 0.0673 0.3487 0.063 Uiso calc R 1 H C13 0.4945(9) 0.1751(7) 0.4643(5) 0.056(2) Uani d . 1 C H13A 0.5411 0.1072 0.5013 0.068 Uiso calc R 1 H C14 0.4405(9) 0.2984(7) 0.5000(5) 0.054(2) Uani d . 1 C H14A 0.4515 0.3142 0.5614 0.064 Uiso calc R 1 H C15 0.3696(8) 0.4006(6) 0.4466(4) 0.0435(17) Uani d . 1 C H15A 0.3340 0.4847 0.4716 0.052 Uiso calc R 1 H C16 0.2150(7) 0.8552(6) 0.0999(4) 0.0295(13) Uani d . 1 C C17 0.2079(9) 0.7714(7) 0.0297(4) 0.0491(18) Uani d . 1 C H17A 0.1765 0.6966 0.0449 0.059 Uiso calc R 1 H C18 0.2486(10) 0.8017(8) -0.0640(5) 0.062(2) Uani d . 1 C H18A 0.2426 0.7467 -0.1113 0.075 Uiso calc R 1 H C19 0.2964(9) 0.9090(8) -0.0876(5) 0.056(2) Uani d . 1 C H19A 0.3237 0.9272 -0.1505 0.068 Uiso calc R 1 H C20 0.3046(8) 0.9912(7) -0.0181(5) 0.054(2) Uani d . 1 C H20A 0.3372 1.0653 -0.0338 0.065 Uiso calc R 1 H C21 0.2646(8) 0.9637(6) 0.0745(5) 0.0444(17) Uani d . 1 C H21A 0.2711 1.0195 0.1210 0.053 Uiso calc R 1 H C22 0.1097(7) 0.9567(5) 0.2926(4) 0.0320(14) Uani d . 1 C C23 0.1709(8) 0.9689(7) 0.3737(4) 0.0467(18) Uani d . 1 C H23A 0.2538 0.9017 0.3916 0.056 Uiso calc R 1 H C24 0.1086(9) 1.0815(8) 0.4283(5) 0.066(2) Uani d . 1 C H24A 0.1509 1.0896 0.4825 0.080 Uiso calc R 1 H C25 -0.0135(10) 1.1800(8) 0.4038(6) 0.070(2) Uani d . 1 C H25A -0.0535 1.2555 0.4407 0.084 Uiso calc R 1 H C26 -0.0776(10) 1.1685(7) 0.3251(6) 0.072(3) Uani d . 1 C H26A -0.1623 1.2357 0.3091 0.086 Uiso calc R 1 H C27 -0.0176(9) 1.0574(7) 0.2688(5) 0.058(2) Uani d . 1 C H27A -0.0622 1.0500 0.2154 0.069 Uiso calc R 1 H 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 Pd1 0.0210(3) 0.0231(2) 0.0264(2) -0.00581(19) -0.00607(18) 0.00046(18) Br1 0.0316(4) 0.0374(4) 0.0798(6) -0.0021(3) -0.0123(4) 0.0041(4) Br2 0.0353(4) 0.0387(4) 0.0536(5) -0.0167(3) -0.0080(3) 0.0051(3) P1 0.0292(9) 0.0282(9) 0.0256(8) -0.0102(7) -0.0032(7) 0.0001(7) P2 0.0249(8) 0.0279(9) 0.0309(8) -0.0071(7) -0.0091(7) 0.0028(7) C1 0.038(4) 0.046(4) 0.034(4) -0.013(3) 0.002(3) -0.007(3) C2 0.030(4) 0.052(4) 0.056(5) -0.015(3) 0.002(3) 0.005(3) C3 0.024(4) 0.037(4) 0.047(4) -0.008(3) -0.011(3) 0.003(3) C4 0.034(4) 0.029(3) 0.028(3) -0.012(3) -0.006(3) 0.004(3) C5 0.056(5) 0.109(7) 0.056(5) -0.054(5) 0.013(4) -0.024(5) C6 0.070(6) 0.145(9) 0.087(7) -0.064(7) -0.017(5) -0.047(6) C7 0.061(5) 0.069(5) 0.043(4) -0.006(4) -0.019(4) -0.021(4) C8 0.067(6) 0.087(6) 0.030(4) -0.027(5) 0.003(4) -0.012(4) C9 0.049(5) 0.078(5) 0.042(4) -0.039(4) -0.002(3) -0.015(4) C10 0.036(4) 0.034(4) 0.028(3) -0.013(3) -0.003(3) 0.005(3) C11 0.056(5) 0.033(4) 0.039(4) -0.014(3) -0.013(3) -0.001(3) C12 0.060(5) 0.034(4) 0.067(5) -0.012(4) -0.023(4) 0.007(4) C13 0.069(5) 0.052(5) 0.060(5) -0.027(4) -0.033(4) 0.029(4) C14 0.075(6) 0.061(5) 0.033(4) -0.024(4) -0.024(4) 0.009(4) C15 0.064(5) 0.035(4) 0.036(4) -0.020(4) -0.013(3) 0.005(3) C16 0.027(3) 0.031(3) 0.031(3) -0.006(3) -0.009(3) 0.002(3) C17 0.068(5) 0.050(4) 0.037(4) -0.024(4) -0.019(4) 0.008(3) C18 0.085(6) 0.077(6) 0.029(4) -0.028(5) -0.011(4) 0.001(4) C19 0.060(5) 0.080(6) 0.030(4) -0.023(5) -0.006(4) 0.016(4) C20 0.054(5) 0.057(5) 0.053(5) -0.018(4) -0.012(4) 0.023(4) C21 0.057(5) 0.042(4) 0.040(4) -0.018(4) -0.016(3) 0.007(3) C22 0.032(4) 0.027(3) 0.035(3) -0.008(3) -0.001(3) 0.002(3) C23 0.040(4) 0.053(5) 0.043(4) -0.009(3) -0.002(3) -0.010(3) C24 0.055(5) 0.078(6) 0.064(5) -0.017(5) 0.003(4) -0.039(5) C25 0.068(6) 0.046(5) 0.086(7) -0.012(5) 0.012(5) -0.025(5) C26 0.066(6) 0.039(5) 0.089(7) 0.014(4) -0.003(5) 0.009(4) C27 0.057(5) 0.041(4) 0.067(5) 0.004(4) -0.021(4) -0.004(4) 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 '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_publ_flag P2 Pd1 P1 90.80(6) yes P2 Pd1 Br1 170.92(5) no P1 Pd1 Br1 91.22(5) yes P2 Pd1 Br2 88.04(5) yes P1 Pd1 Br2 177.78(5) ? Br1 Pd1 Br2 90.22(3) yes C4 P1 C10 106.4(3) ? C4 P1 C1 107.0(3) ? C10 P1 C1 101.9(3) ? C4 P1 Pd1 110.20(19) ? C10 P1 Pd1 115.2(2) ? C1 P1 Pd1 115.3(2) ? C22 P2 C16 107.3(3) ? C22 P2 C3 102.7(3) ? C16 P2 C3 105.0(3) ? C22 P2 Pd1 115.9(2) ? C16 P2 Pd1 109.17(19) ? C3 P2 Pd1 115.8(2) ? C2 C1 P1 118.3(4) yes C1 C2 C3 116.6(5) yes C2 C3 P2 111.3(4) yes C5 C4 C9 118.2(6) ? C5 C4 P1 123.2(5) ? C9 C4 P1 118.6(5) ? C4 C5 C6 120.6(7) ? C7 C6 C5 122.1(7) ? C6 C7 C8 117.8(7) ? C7 C8 C9 121.7(7) ? C4 C9 C8 119.6(6) ? C11 C10 C15 119.4(6) ? C11 C10 P1 122.2(5) ? C15 C10 P1 118.4(5) ? C10 C11 C12 120.1(6) ? C13 C12 C11 120.5(7) ? C14 C13 C12 119.7(6) ? C13 C14 C15 121.1(6) ? C14 C15 C10 119.2(6) ? C21 C16 C17 118.8(6) ? C21 C16 P2 122.2(4) ? C17 C16 P2 118.7(5) ? C16 C17 C18 118.8(7) ? C19 C18 C17 121.5(7) ? C18 C19 C20 119.6(6) ? C21 C20 C19 119.9(7) ? C20 C21 C16 121.3(6) ? C23 C22 C27 118.9(6) ? C23 C22 P2 122.2(5) ? C27 C22 P2 118.7(5) ? C22 C23 C24 119.9(7) ? C25 C24 C23 120.9(7) ? C24 C25 C26 120.0(7) ? C25 C26 C27 120.6(7) ? C26 C27 C22 119.8(7) ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag Pd1 P2 2.2535(16) yes Pd1 P1 2.2557(16) yes Pd1 Br1 2.4744(9) yes Pd1 Br2 2.4767(9) yes P1 C4 1.816(6) ? P1 C10 1.819(6) ? P1 C1 1.835(6) ? P2 C22 1.806(6) ? P2 C16 1.819(6) ? P2 C3 1.829(6) ? C1 C2 1.524(8) ? C2 C3 1.523(8) ? C4 C5 1.357(8) ? C4 C9 1.378(8) ? C5 C6 1.376(10) ? C6 C7 1.348(10) ? C7 C8 1.349(9) ? C8 C9 1.391(9) ? C10 C11 1.375(8) ? C10 C15 1.398(8) ? C11 C12 1.384(8) ? C12 C13 1.371(9) ? C13 C14 1.360(9) ? C14 C15 1.381(8) ? C16 C21 1.375(8) ? C16 C17 1.391(8) ? C17 C18 1.395(9) ? C18 C19 1.351(10) ? C19 C20 1.375(10) ? C20 C21 1.371(9) ? C22 C23 1.384(8) ? C22 C27 1.393(8) ? C23 C24 1.385(9) ? C24 C25 1.357(10) ? C25 C26 1.364(11) ? C26 C27 1.385(10) ? 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 P2 Pd1 P1 C4 78.6(2) Br1 Pd1 P1 C4 -92.6(2) Br2 Pd1 P1 C4 137.1(13) P2 Pd1 P1 C10 -161.1(2) Br1 Pd1 P1 C10 27.8(2) Br2 Pd1 P1 C10 -102.6(13) P2 Pd1 P1 C1 -42.7(2) Br1 Pd1 P1 C1 146.1(2) Br2 Pd1 P1 C1 15.8(14) P1 Pd1 P2 C22 121.3(2) Br1 Pd1 P2 C22 -135.9(3) Br2 Pd1 P2 C22 -56.8(2) P1 Pd1 P2 C16 -117.4(2) Br1 Pd1 P2 C16 -14.5(4) Br2 Pd1 P2 C16 64.5(2) P1 Pd1 P2 C3 0.9(2) Br1 Pd1 P2 C3 103.7(4) Br2 Pd1 P2 C3 -177.2(2) C4 P1 C1 C2 -81.9(5) C10 P1 C1 C2 166.6(5) Pd1 P1 C1 C2 41.1(5) P1 C1 C2 C3 23.0(8) C1 C2 C3 P2 -74.7(6) C22 P2 C3 C2 -71.3(5) C16 P2 C3 C2 176.6(4) Pd1 P2 C3 C2 56.1(5) C10 P1 C4 C5 90.7(7) C1 P1 C4 C5 -17.6(7) Pd1 P1 C4 C5 -143.7(6) C10 P1 C4 C9 -89.8(6) C1 P1 C4 C9 161.8(5) Pd1 P1 C4 C9 35.7(6) C9 C4 C5 C6 -1.6(12) P1 C4 C5 C6 177.8(7) C4 C5 C6 C7 0.6(15) C5 C6 C7 C8 0.5(14) C6 C7 C8 C9 -0.7(13) C5 C4 C9 C8 1.5(11) P1 C4 C9 C8 -178.0(6) C7 C8 C9 C4 -0.4(12) C4 P1 C10 C11 6.8(6) C1 P1 C10 C11 118.8(5) Pd1 P1 C10 C11 -115.6(5) C4 P1 C10 C15 -174.7(5) C1 P1 C10 C15 -62.7(6) Pd1 P1 C10 C15 62.9(5) C15 C10 C11 C12 -0.3(10) P1 C10 C11 C12 178.2(5) C10 C11 C12 C13 1.4(11) C11 C12 C13 C14 -1.5(11) C12 C13 C14 C15 0.5(11) C13 C14 C15 C10 0.5(11) C11 C10 C15 C14 -0.6(10) P1 C10 C15 C14 -179.2(5) C22 P2 C16 C21 30.1(6) C3 P2 C16 C21 138.9(5) Pd1 P2 C16 C21 -96.3(5) C22 P2 C16 C17 -155.9(5) C3 P2 C16 C17 -47.1(6) Pd1 P2 C16 C17 77.7(5) C21 C16 C17 C18 -1.1(10) P2 C16 C17 C18 -175.3(5) C16 C17 C18 C19 0.9(12) C17 C18 C19 C20 -0.4(12) C18 C19 C20 C21 0.1(11) C19 C20 C21 C16 -0.4(11) C17 C16 C21 C20 0.9(10) P2 C16 C21 C20 174.9(5) C16 P2 C22 C23 -134.0(5) C3 P2 C22 C23 115.6(6) Pd1 P2 C22 C23 -11.7(6) C16 P2 C22 C27 51.4(6) C3 P2 C22 C27 -59.0(6) Pd1 P2 C22 C27 173.6(5) C27 C22 C23 C24 -1.8(10) P2 C22 C23 C24 -176.4(5) C22 C23 C24 C25 0.7(12) C23 C24 C25 C26 0.7(13) C24 C25 C26 C27 -0.9(13) C25 C26 C27 C22 -0.2(13) C23 C22 C27 C26 1.6(11) P2 C22 C27 C26 176.4(6)