#------------------------------------------------------------------------------ #$Date: 2012-02-28 12:14:52 +0000 (Tue, 28 Feb 2012) $ #$Revision: 35911 $ #$URL: svn://www.crystallography.net/cod/cif/1/10/08/1100893.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_1100893 _publ_section_title ; Synthesis and Structures of Electron-poor Pentafluorophenyl -substituted PCP-Pd Pincer Complexes ; _space_group_IT_number 14 _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _[local]_cod_cif_authors_sg_H-M 'P 21/c' loop_ _publ_author_name 'Chase, Preston A.' 'Gagliardo, Marcella' 'van Klink, Gerard P. M.' 'Lutz, Martin' 'Spek, Anthony L.' 'van Koten, Gerard' _chemical_formula_moiety 'C34 H10 F20 N P2 Pd, B F4' _chemical_formula_sum 'C34 H10 B F24 N P2 Pd' _chemical_formula_weight 1067.58 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' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 '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' 'P' 'P' 0.1023 0.0942 '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' _symmetry_cell_setting monoclinic loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.1565(2) _cell_length_b 25.6619(5) _cell_length_c 16.1795(3) _cell_angle_alpha 90.00 _cell_angle_beta 110.5437(8) _cell_angle_gamma 90.00 _cell_volume 3948.77(13) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 72429 _cell_measurement_theta_min 1.02 _cell_measurement_theta_max 27.48 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.39 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.796 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2072 _exptl_absorpt_coefficient_mu 0.693 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.70 _exptl_absorpt_correction_T_max 0.96 _exptl_absorpt_process_details ? _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 40386 _diffrn_reflns_av_R_equivalents 0.0659 _diffrn_reflns_av_sigmaI/netI 0.0473 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.56 _diffrn_reflns_theta_max 26.14 _reflns_number_total 7802 _reflns_number_gt 5863 _reflns_threshold_expression 'I>2\s(I)' loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.316 0.631 0.288 128.4 42.3 2 0.316 0.869 0.788 128.4 42.4 3 0.684 0.131 0.212 128.5 42.0 4 0.684 0.369 0.712 128.5 42.2 _platon_squeeze_details ; ? ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0335P)^2^+3.7955P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7802 _refine_ls_number_parameters 623 _refine_ls_number_restraints 258 _refine_ls_R_factor_all 0.0577 _refine_ls_R_factor_gt 0.0407 _refine_ls_wR_factor_ref 0.1001 _refine_ls_wR_factor_gt 0.0931 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.152 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.000 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 0.99146(3) 0.079376(12) 0.777666(18) 0.03873(10) Uani 1 1 d . . . P1 P 0.85438(10) 0.00640(4) 0.74168(6) 0.0390(2) Uani 1 1 d . . . P2 P 1.16523(10) 0.13583(4) 0.85151(7) 0.0405(2) Uani 1 1 d . . . F1 F 0.7587(3) -0.10546(10) 0.69740(16) 0.0634(7) Uani 1 1 d . . . F2 F 0.8422(4) -0.17527(11) 0.60229(19) 0.0893(10) Uani 1 1 d . . . F3 F 1.0252(4) -0.14618(13) 0.52210(19) 0.0907(10) Uani 1 1 d . . . F4 F 1.1306(3) -0.04839(13) 0.54302(17) 0.0780(9) Uani 1 1 d . . . F5 F 1.0467(2) 0.02133(10) 0.63569(15) 0.0546(6) Uani 1 1 d . . . F6 F 0.7092(2) 0.04411(9) 0.56105(13) 0.0467(5) Uani 1 1 d . . . F7 F 0.4419(2) 0.07551(10) 0.48272(15) 0.0559(6) Uani 1 1 d . . . F8 F 0.2546(2) 0.06177(12) 0.56484(17) 0.0697(8) Uani 1 1 d . . . F9 F 0.3354(2) 0.01527(14) 0.72576(17) 0.0785(9) Uani 1 1 d . . . F10 F 0.5978(2) -0.01669(12) 0.80310(15) 0.0681(8) Uani 1 1 d . . . F11 F 1.1539(3) 0.14042(13) 0.66451(17) 0.0790(8) Uani 1 1 d . . . F12 F 1.2845(3) 0.20632(15) 0.58995(18) 0.0966(11) Uani 1 1 d . . . F13 F 1.4429(4) 0.28432(14) 0.6842(2) 0.1042(11) Uani 1 1 d . . . F14 F 1.4762(4) 0.29627(13) 0.8579(2) 0.0994(11) Uani 1 1 d . . . F15 F 1.3511(3) 0.22982(11) 0.93449(17) 0.0667(7) Uani 1 1 d . . . F16 F 0.9616(3) 0.22089(11) 0.8062(2) 0.0744(8) Uani 1 1 d . . . F17 F 0.8332(3) 0.26924(13) 0.9040(3) 0.1146(13) Uani 1 1 d . . . F18 F 0.9136(4) 0.24872(15) 1.0799(3) 0.1304(15) Uani 1 1 d . . . F19 F 1.1130(5) 0.17599(13) 1.1538(2) 0.1097(13) Uani 1 1 d . . . F20 F 1.2389(3) 0.12658(10) 1.05758(17) 0.0697(7) Uani 1 1 d . . . N1 N 0.8617(3) 0.12913(14) 0.6820(2) 0.0508(9) Uani 1 1 d . . . C1 C 1.1078(4) 0.03157(14) 0.8755(2) 0.0359(8) Uani 1 1 d . . . C2 C 1.0494(4) -0.01456(15) 0.8951(2) 0.0395(9) Uani 1 1 d . . . C3 C 1.1301(4) -0.04845(17) 0.9604(2) 0.0458(9) Uani 1 1 d . . . H3 H 1.0906 -0.0800 0.9719 0.055 Uiso 1 1 calc R . . C4 C 1.2687(4) -0.03587(17) 1.0086(3) 0.0462(10) Uani 1 1 d . . . H4 H 1.3250 -0.0593 1.0523 0.055 Uiso 1 1 calc R . . C5 C 1.3250(4) 0.01017(16) 0.9935(2) 0.0403(9) Uani 1 1 d . . . H5 H 1.4185 0.0192 1.0290 0.048 Uiso 1 1 calc R . . C6 C 1.2474(3) 0.04371(15) 0.9271(2) 0.0359(8) Uani 1 1 d . . . C7 C 0.8946(4) -0.02542(18) 0.8477(2) 0.0462(10) Uani 1 1 d . . . H7A H 0.8375 -0.0107 0.8806 0.055 Uiso 1 1 calc R . . H7B H 0.8766 -0.0634 0.8402 0.055 Uiso 1 1 calc R . . C8 C 0.9033(4) -0.04013(16) 0.6730(2) 0.0407(9) Uani 1 1 d . . . C9 C 0.8527(4) -0.09083(17) 0.6608(3) 0.0501(10) Uani 1 1 d . . . C10 C 0.8946(5) -0.12662(18) 0.6121(3) 0.0596(12) Uani 1 1 d . . . C11 C 0.9864(5) -0.1123(2) 0.5721(3) 0.0635(13) Uani 1 1 d . . . C12 C 1.0393(4) -0.0625(2) 0.5819(3) 0.0556(11) Uani 1 1 d . . . C13 C 0.9967(4) -0.02700(18) 0.6312(3) 0.0474(10) Uani 1 1 d . . . C14 C 0.6652(4) 0.01407(16) 0.6864(2) 0.0404(9) Uani 1 1 d . . . C15 C 0.6184(4) 0.03696(16) 0.6038(2) 0.0420(9) Uani 1 1 d . . . C16 C 0.4818(4) 0.05286(17) 0.5619(2) 0.0460(10) Uani 1 1 d . . . C17 C 0.3871(4) 0.04552(19) 0.6039(3) 0.0526(11) Uani 1 1 d . . . C18 C 0.4269(4) 0.0218(2) 0.6844(3) 0.0557(12) Uani 1 1 d . . . C19 C 0.5651(4) 0.00603(18) 0.7247(2) 0.0484(10) Uani 1 1 d . . . C20 C 1.3117(4) 0.09339(16) 0.9104(3) 0.0439(9) Uani 1 1 d . . . H20A H 1.3710 0.0866 0.8743 0.053 Uiso 1 1 calc R . . H20B H 1.3706 0.1096 0.9668 0.053 Uiso 1 1 calc R . . C21 C 1.2421(4) 0.18422(16) 0.8009(3) 0.0474(10) Uani 1 1 d . . . C22 C 1.2312(4) 0.17948(19) 0.7136(3) 0.0563(11) Uani 1 1 d . . . C23 C 1.2974(5) 0.2128(2) 0.6750(3) 0.0674(13) Uani 1 1 d . . . C24 C 1.3781(5) 0.2524(2) 0.7232(4) 0.0727(15) Uani 1 1 d . . . C25 C 1.3947(5) 0.2581(2) 0.8098(4) 0.0678(13) Uani 1 1 d . . . C26 C 1.3273(4) 0.22436(18) 0.8480(3) 0.0530(11) Uani 1 1 d . . . C27 C 1.1040(4) 0.17231(16) 0.9273(3) 0.0481(10) Uani 1 1 d . . . C28 C 1.0002(5) 0.20903(19) 0.8929(3) 0.0591(12) Uani 1 1 d . . . C29 C 0.9333(5) 0.2341(2) 0.9415(5) 0.0812(18) Uani 1 1 d . . . C30 C 0.9744(7) 0.2232(2) 1.0305(5) 0.0856(18) Uani 1 1 d . . . C31 C 1.0752(7) 0.1870(2) 1.0674(4) 0.0774(16) Uani 1 1 d . . . C32 C 1.1408(5) 0.16180(18) 1.0174(3) 0.0576(12) Uani 1 1 d . . . C33 C 0.7752(5) 0.1546(2) 0.6382(3) 0.0645(13) Uani 1 1 d . . . C34 C 0.6595(6) 0.1876(2) 0.5822(4) 0.102(2) Uani 1 1 d . . . H34A H 0.5695 0.1734 0.5815 0.153 Uiso 1 1 calc R . . H34B H 0.6610 0.1881 0.5219 0.153 Uiso 1 1 calc R . . H34C H 0.6711 0.2231 0.6058 0.153 Uiso 1 1 calc R . . F22A F 0.6440(6) 0.3106(2) 0.2777(4) 0.0725(17) Uani 0.60 1 d PDU A 1 F23A F 0.5173(5) 0.3830(3) 0.2843(5) 0.079(2) Uani 0.60 1 d PDU A 1 F24A F 0.6247(7) 0.3360(3) 0.4050(3) 0.0907(19) Uani 0.60 1 d PDU A 1 F22B F 0.6022(12) 0.3346(6) 0.2365(7) 0.114(5) Uani 0.28 1 d PDU A 2 F23B F 0.5229(8) 0.3881(4) 0.3175(8) 0.056(4) Uani 0.28 1 d PDU A 2 F24B F 0.6417(14) 0.3160(5) 0.3805(10) 0.153(9) Uani 0.28 1 d PDU A 2 F22C F 0.5436(16) 0.3689(7) 0.2375(9) 0.070(7) Uani 0.12 1 d PDU A 3 F23C F 0.5668(19) 0.3614(9) 0.3812(13) 0.112(12) Uani 0.12 1 d PDU A 3 F24C F 0.6658(15) 0.3022(3) 0.3181(14) 0.058(8) Uani 0.12 1 d PDU A 3 F21 F 0.7533(3) 0.38395(13) 0.3426(2) 0.0999(11) Uani 1 1 d DU A . B1 B 0.6333(5) 0.35424(18) 0.3225(3) 0.0769(19) Uani 1 1 d 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 Pd1 0.02894(15) 0.04466(19) 0.04048(17) -0.00277(13) 0.00955(12) -0.00210(12) P1 0.0313(5) 0.0500(6) 0.0373(5) -0.0059(4) 0.0140(4) -0.0075(4) P2 0.0327(5) 0.0422(6) 0.0462(6) -0.0038(5) 0.0132(4) -0.0044(4) F1 0.0761(17) 0.0612(16) 0.0551(14) -0.0058(12) 0.0259(14) -0.0251(13) F2 0.137(3) 0.0503(18) 0.0780(19) -0.0105(15) 0.0349(19) -0.0072(18) F3 0.112(2) 0.093(2) 0.0692(18) -0.0183(17) 0.0349(18) 0.0362(19) F4 0.0615(16) 0.119(3) 0.0673(17) -0.0106(17) 0.0400(15) 0.0121(16) F5 0.0451(13) 0.0681(17) 0.0599(14) -0.0102(12) 0.0303(12) -0.0149(12) F6 0.0359(11) 0.0690(16) 0.0389(11) -0.0035(11) 0.0177(10) -0.0058(11) F7 0.0423(12) 0.0737(17) 0.0486(13) 0.0046(12) 0.0122(11) -0.0012(12) F8 0.0320(12) 0.110(2) 0.0646(16) 0.0006(15) 0.0133(11) 0.0018(13) F9 0.0344(12) 0.150(3) 0.0567(15) -0.0008(17) 0.0229(12) -0.0120(15) F10 0.0366(12) 0.125(2) 0.0424(13) 0.0090(14) 0.0137(11) -0.0168(14) F11 0.0846(19) 0.102(2) 0.0510(15) -0.0134(15) 0.0251(14) -0.0294(17) F12 0.101(2) 0.137(3) 0.0525(17) 0.0167(18) 0.0281(17) -0.021(2) F13 0.103(2) 0.112(3) 0.104(2) 0.039(2) 0.044(2) -0.028(2) F14 0.103(2) 0.086(2) 0.112(3) -0.0060(19) 0.042(2) -0.053(2) F15 0.0615(15) 0.0760(19) 0.0621(16) -0.0141(14) 0.0210(13) -0.0279(14) F16 0.0494(15) 0.0652(18) 0.092(2) -0.0141(16) 0.0049(14) 0.0134(13) F17 0.0642(19) 0.086(2) 0.185(4) -0.053(2) 0.033(2) 0.0154(18) F18 0.152(3) 0.103(3) 0.184(4) -0.055(3) 0.120(3) 0.000(2) F19 0.190(4) 0.082(2) 0.096(2) -0.0212(19) 0.098(3) -0.016(2) F20 0.102(2) 0.0558(16) 0.0583(15) -0.0013(13) 0.0373(16) 0.0037(16) N1 0.0411(18) 0.052(2) 0.049(2) 0.0017(17) 0.0028(16) -0.0075(17) C1 0.0342(18) 0.042(2) 0.0346(18) -0.0051(16) 0.0158(16) 0.0029(16) C2 0.0361(19) 0.048(2) 0.0365(19) -0.0086(17) 0.0152(16) -0.0051(17) C3 0.048(2) 0.050(3) 0.044(2) -0.0034(19) 0.0225(19) -0.0031(19) C4 0.044(2) 0.055(3) 0.041(2) 0.0019(19) 0.0170(18) 0.0115(19) C5 0.0294(18) 0.055(3) 0.038(2) -0.0034(18) 0.0138(16) 0.0052(17) C6 0.0290(17) 0.046(2) 0.0342(18) -0.0026(16) 0.0135(15) 0.0014(16) C7 0.038(2) 0.065(3) 0.036(2) -0.0015(19) 0.0123(17) -0.0097(19) C8 0.0320(19) 0.052(2) 0.0365(19) -0.0037(17) 0.0104(16) -0.0050(17) C9 0.054(2) 0.057(3) 0.035(2) 0.0001(19) 0.0114(19) -0.006(2) C10 0.079(3) 0.045(3) 0.047(2) -0.004(2) 0.011(2) 0.007(2) C11 0.073(3) 0.066(3) 0.052(3) -0.007(2) 0.024(2) 0.021(3) C12 0.047(2) 0.079(3) 0.043(2) -0.005(2) 0.018(2) 0.008(2) C13 0.034(2) 0.063(3) 0.044(2) -0.007(2) 0.0127(18) -0.0006(19) C14 0.0306(18) 0.054(2) 0.0357(19) -0.0121(18) 0.0099(16) -0.0079(17) C15 0.0324(19) 0.057(3) 0.040(2) -0.0126(18) 0.0159(17) -0.0106(17) C16 0.039(2) 0.060(3) 0.039(2) -0.0091(19) 0.0129(17) -0.0096(19) C17 0.031(2) 0.075(3) 0.049(2) -0.014(2) 0.0102(18) -0.009(2) C18 0.032(2) 0.094(4) 0.045(2) -0.010(2) 0.0179(19) -0.015(2) C19 0.038(2) 0.074(3) 0.033(2) -0.006(2) 0.0119(17) -0.015(2) C20 0.0305(18) 0.054(3) 0.046(2) -0.0020(19) 0.0123(17) -0.0016(17) C21 0.034(2) 0.048(2) 0.058(2) 0.004(2) 0.0145(19) -0.0004(18) C22 0.046(2) 0.068(3) 0.050(2) -0.001(2) 0.010(2) -0.008(2) C23 0.060(3) 0.092(4) 0.051(3) 0.018(3) 0.019(2) 0.003(3) C24 0.060(3) 0.075(4) 0.082(4) 0.028(3) 0.024(3) -0.012(3) C25 0.056(3) 0.064(3) 0.078(3) 0.007(3) 0.017(3) -0.017(2) C26 0.044(2) 0.059(3) 0.050(2) 0.003(2) 0.009(2) -0.007(2) C27 0.041(2) 0.043(2) 0.063(3) -0.013(2) 0.021(2) -0.0095(18) C28 0.044(2) 0.058(3) 0.071(3) -0.015(2) 0.013(2) -0.008(2) C29 0.051(3) 0.055(3) 0.142(6) -0.038(4) 0.038(3) -0.005(2) C30 0.093(4) 0.071(4) 0.119(5) -0.037(4) 0.070(4) -0.013(3) C31 0.109(5) 0.055(3) 0.092(4) -0.026(3) 0.066(4) -0.019(3) C32 0.069(3) 0.047(3) 0.070(3) -0.018(2) 0.039(3) -0.012(2) C33 0.054(3) 0.062(3) 0.065(3) 0.010(2) 0.006(2) -0.015(2) C34 0.065(3) 0.085(4) 0.116(5) 0.047(4) -0.019(3) -0.006(3) F22A 0.067(3) 0.065(3) 0.079(4) -0.015(3) 0.018(3) 0.005(3) F23A 0.074(4) 0.087(4) 0.085(5) 0.012(4) 0.041(3) 0.020(3) F24A 0.119(5) 0.068(4) 0.090(4) -0.002(3) 0.043(4) -0.002(4) F22B 0.094(8) 0.134(10) 0.137(9) -0.069(8) 0.070(7) -0.028(7) F23B 0.043(5) 0.092(7) 0.034(6) -0.015(5) 0.015(4) 0.004(5) F24B 0.147(12) 0.115(12) 0.185(13) 0.019(9) 0.043(9) 0.000(9) F22C 0.053(10) 0.044(10) 0.094(11) 0.021(9) 0.001(8) 0.010(8) F23C 0.092(14) 0.120(16) 0.134(16) -0.008(10) 0.053(11) 0.004(10) F24C 0.064(11) 0.057(11) 0.037(10) 0.022(8) -0.002(8) 0.012(8) F21 0.0701(19) 0.125(3) 0.121(3) -0.059(2) 0.0543(19) -0.0356(19) B1 0.047(3) 0.085(5) 0.103(5) -0.029(4) 0.031(3) -0.006(3) _cod_database_code 1100893