#------------------------------------------------------------------------------ #$Date: 2008-01-26 15:05:32 +0200 (Sat, 26 Jan 2008) $ #$Revision: 19 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/1100804.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_1100804 _publ_requested_journal 'Organometallics' _publ_section_title ; The reactivity of [Pd{CH2C(O)Me}Cl]n toward Isocyanides. ; _chemical_formula_sum 'C32 H33 Cl3 F3 N3 O4 Pd S' _chemical_formula_weight 825.42 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' 'F' 'F' 0.0171 0.0103 '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' 'Pd' 'Pd' -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.6505(5) _cell_length_b 11.8001(5) _cell_length_c 18.7442(14) _cell_angle_alpha 83.546(5) _cell_angle_beta 87.742(5) _cell_angle_gamma 70.234(4) _cell_volume 1789.20(19) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 85 _cell_measurement_theta_min 5.3 _cell_measurement_theta_max 12.4 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.46 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.532 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 836 _exptl_absorpt_coefficient_mu 0.856 _exptl_absorpt_correction_type Psi-scans _exptl_absorpt_correction_T_min 0.743 _exptl_absorpt_correction_T_max 0.910 _exptl_absorpt_process_details ? _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens P4' _diffrn_measurement_method \w-scan _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 247 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.7 _diffrn_reflns_number 6735 _diffrn_reflns_av_R_equivalents 0.0181 _diffrn_reflns_av_sigmaI/netI 0.0287 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6278 _reflns_number_gt 5432 _reflns_threshold_expression >2sigma(I) _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^)+(0.0377P)^2^+0.6583P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary Patterson _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment 'ordered methyls rigid,hydrogens at C3 free, others riding' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6278 _refine_ls_number_parameters 455 _refine_ls_number_restraints 39 _refine_ls_R_factor_all 0.0361 _refine_ls_R_factor_gt 0.0290 _refine_ls_wR_factor_ref 0.0705 _refine_ls_wR_factor_gt 0.0684 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.038 _refine_ls_shift/su_max 0.002 _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 Pd Pd 0.64574(2) 0.908779(17) 0.689302(10) 0.02155(7) Uani 1 1 d . . . O1 O 0.6859(3) 0.75021(18) 0.51907(11) 0.0419(5) Uani 1 1 d . . . N1 N 0.6976(3) 0.9102(2) 0.85565(12) 0.0292(5) Uani 1 1 d . . . N2 N 0.5565(3) 1.18920(19) 0.66640(11) 0.0271(5) Uani 1 1 d . . . N3 N 0.8073(3) 0.62751(19) 0.69476(11) 0.0253(5) Uani 1 1 d . . . C1 C 0.5728(3) 0.9214(2) 0.58288(13) 0.0318(6) Uani 1 1 d . . . H1A H 0.4715 0.9001 0.5826 0.038 Uiso 1 1 calc R . . H1B H 0.5453 1.0066 0.5617 0.038 Uiso 1 1 calc R . . C2 C 0.6966(3) 0.8433(2) 0.53701(13) 0.0301(6) Uani 1 1 d . . . C3 C 0.8376(5) 0.8852(4) 0.51182(19) 0.0442(8) Uani 1 1 d D . . H3A H 0.911(10) 0.809(4) 0.516(6) 0.09(4) Uiso 0.54(8) 1 d PD A 1 H3B H 0.811(7) 0.920(5) 0.4663(17) 0.03(2) Uiso 0.54(8) 1 d PD A 1 H3C H 0.881(12) 0.925(9) 0.540(4) 0.08(3) Uiso 0.54(8) 1 d PD A 1 H3A' H 0.924(7) 0.857(9) 0.543(3) 0.04(3) Uiso 0.46(8) 1 d PD A 2 H3B' H 0.899(8) 0.843(7) 0.477(3) 0.04(2) Uiso 0.46(8) 1 d PD A 2 H3C' H 0.822(8) 0.966(2) 0.510(4) 0.02(2) Uiso 0.46(8) 1 d PD A 2 C4 C 0.6882(3) 0.9059(2) 0.79515(14) 0.0272(6) Uani 1 1 d . . . C5 C 0.5826(3) 1.0868(2) 0.67577(13) 0.0268(6) Uani 1 1 d . . . C6 C 0.7393(3) 0.7304(2) 0.69186(13) 0.0251(6) Uani 1 1 d . . . C11 C 0.7092(4) 0.9137(3) 0.93002(14) 0.0328(6) Uani 1 1 d D . . C12 C 0.6611(4) 0.8303(3) 0.97616(15) 0.0405(7) Uani 1 1 d D . . C13 C 0.6762(4) 0.8354(3) 1.04894(16) 0.0531(9) Uani 1 1 d D . . H13 H 0.6454 0.7804 1.0826 0.064 Uiso 1 1 calc R . . C14 C 0.7356(4) 0.9194(4) 1.07366(17) 0.0544(9) Uani 1 1 d D . . H14 H 0.7459 0.9208 1.1238 0.065 Uiso 1 1 calc R . . C15 C 0.7796(4) 1.0009(3) 1.02588(16) 0.0465(8) Uani 1 1 d D . . H15 H 0.8194 1.0581 1.0436 0.056 Uiso 1 1 calc R . . C16 C 0.7670(4) 1.0009(3) 0.95240(15) 0.0366(7) Uani 1 1 d D . . C17 C 0.8085(4) 1.0910(3) 0.89907(17) 0.0440(8) Uani 1 1 d . . . H17A H 0.8514 1.1423 0.9244 0.053 Uiso 1 1 calc R . . H17B H 0.7095 1.1415 0.8724 0.053 Uiso 1 1 calc R . . H17C H 0.8919 1.0480 0.8655 0.053 Uiso 1 1 calc R . . C18 C 0.5957(5) 0.7411(3) 0.94832(18) 0.0536(9) Uani 1 1 d . . . H18A H 0.6873 0.6733 0.9326 0.064 Uiso 1 1 calc R . . H18B H 0.5223 0.7809 0.9077 0.064 Uiso 1 1 calc R . . H18C H 0.5347 0.7107 0.9865 0.064 Uiso 1 1 calc R . . C21 C 0.5283(3) 1.3146(2) 0.65580(13) 0.0260(6) Uani 1 1 d D . . C22 C 0.4339(3) 1.3860(2) 0.70653(14) 0.0310(6) Uani 1 1 d D . . C23 C 0.4091(4) 1.5096(2) 0.69499(15) 0.0359(7) Uani 1 1 d D . . H23 H 0.3433 1.5624 0.7275 0.043 Uiso 1 1 calc R . . C24 C 0.4795(4) 1.5560(2) 0.63645(16) 0.0375(7) Uani 1 1 d D . . H24 H 0.4629 1.6403 0.6297 0.045 Uiso 1 1 calc R . . C25 C 0.5735(4) 1.4819(2) 0.58761(15) 0.0344(7) Uani 1 1 d D . . H25 H 0.6212 1.5159 0.5480 0.041 Uiso 1 1 calc R . . C26 C 0.5997(3) 1.3583(2) 0.59541(14) 0.0287(6) Uani 1 1 d D . . C27 C 0.3670(4) 1.3317(3) 0.77148(16) 0.0442(8) Uani 1 1 d . . . H27A H 0.3217 1.2718 0.7573 0.053 Uiso 1 1 calc R . . H27B H 0.2801 1.3957 0.7932 0.053 Uiso 1 1 calc R . . H27C H 0.4554 1.2922 0.8064 0.053 Uiso 1 1 calc R . . C28 C 0.6993(4) 1.2743(3) 0.54332(16) 0.0410(7) Uani 1 1 d . . . H28A H 0.7484 1.3190 0.5074 0.049 Uiso 1 1 calc R . . H28B H 0.6281 1.2411 0.5193 0.049 Uiso 1 1 calc R . . H28C H 0.7865 1.2080 0.5692 0.049 Uiso 1 1 calc R . . C31 C 0.8889(3) 0.5022(2) 0.69463(14) 0.0292(6) Uani 1 1 d D . . C32 C 0.8489(4) 0.4252(3) 0.74904(16) 0.0376(7) Uani 1 1 d D . . C33 C 0.9278(5) 0.3009(3) 0.7448(2) 0.0560(10) Uani 1 1 d D . . H33 H 0.9052 0.2440 0.7800 0.067 Uiso 1 1 calc R . . C34 C 1.0379(5) 0.2599(3) 0.6902(2) 0.0571(10) Uani 1 1 d D . . H34 H 1.0881 0.1753 0.6880 0.068 Uiso 1 1 calc R . . C35 C 1.0760(4) 0.3390(3) 0.6393(2) 0.0488(8) Uani 1 1 d D . . H35 H 1.1537 0.3085 0.6029 0.059 Uiso 1 1 calc R . . C36 C 1.0024(4) 0.4631(2) 0.64015(16) 0.0343(6) Uani 1 1 d D . . C37 C 0.7310(4) 0.4727(3) 0.80761(17) 0.0475(8) Uani 1 1 d . . . H37A H 0.7867 0.4987 0.8439 0.057 Uiso 1 1 calc R . . H37B H 0.6905 0.4089 0.8298 0.057 Uiso 1 1 calc R . . H37C H 0.6385 0.5419 0.7876 0.057 Uiso 1 1 calc R . . C38 C 1.0455(4) 0.5507(3) 0.58539(16) 0.0404(7) Uani 1 1 d . . . H38A H 1.1363 0.5062 0.5554 0.049 Uiso 1 1 calc R . . H38B H 1.0787 0.6079 0.6099 0.049 Uiso 1 1 calc R . . H38C H 0.9497 0.5951 0.5551 0.049 Uiso 1 1 calc R . . S S 0.25070(9) 0.87868(6) 0.76549(4) 0.02947(15) Uani 1 1 d . . . C99 C 0.1227(4) 0.8781(3) 0.69072(16) 0.0375(7) Uani 1 1 d . . . F1 F 0.2053(3) 0.8675(2) 0.62904(10) 0.0644(6) Uani 1 1 d . . . F2 F -0.0072(2) 0.97890(17) 0.68221(13) 0.0624(6) Uani 1 1 d . . . F3 F 0.0661(2) 0.78549(16) 0.70069(10) 0.0493(5) Uani 1 1 d . . . O2 O 0.2974(3) 0.98350(17) 0.74548(12) 0.0421(5) Uani 1 1 d . . . O3 O 0.3809(3) 0.76457(17) 0.76560(12) 0.0458(5) Uani 1 1 d . . . O4 O 0.1408(3) 0.8881(2) 0.82572(11) 0.0503(6) Uani 1 1 d . . . C90 C 0.1714(4) 0.6404(3) 0.91241(17) 0.0457(8) Uani 1 1 d . . . H90 H 0.1771 0.7190 0.8885 0.055 Uiso 1 1 calc R . . Cl1 Cl 0.37043(13) 0.53571(9) 0.91684(6) 0.0686(3) Uani 1 1 d . . . Cl2 Cl 0.04443(12) 0.59402(10) 0.86074(6) 0.0701(3) Uani 1 1 d . . . Cl3 Cl 0.09008(19) 0.66470(13) 0.99809(6) 0.0979(4) Uani 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 0.02698(11) 0.01841(10) 0.01852(10) 0.00002(7) -0.00042(7) -0.00722(8) O1 0.0536(14) 0.0372(12) 0.0359(11) -0.0113(9) -0.0044(10) -0.0138(10) N1 0.0373(14) 0.0296(12) 0.0227(12) -0.0040(9) -0.0009(10) -0.0133(10) N2 0.0318(13) 0.0213(12) 0.0262(11) 0.0000(9) -0.0008(9) -0.0070(10) N3 0.0324(13) 0.0222(12) 0.0229(11) -0.0004(8) -0.0053(9) -0.0115(10) C1 0.0339(16) 0.0349(15) 0.0218(13) -0.0019(11) -0.0081(11) -0.0050(12) C2 0.0341(16) 0.0344(15) 0.0180(13) 0.0039(11) -0.0078(11) -0.0077(12) C3 0.044(2) 0.054(2) 0.0359(19) -0.0034(16) 0.0055(16) -0.0192(18) C4 0.0325(15) 0.0207(13) 0.0293(15) -0.0009(10) -0.0003(11) -0.0107(11) C5 0.0281(14) 0.0281(15) 0.0222(13) -0.0011(10) 0.0017(11) -0.0075(11) C6 0.0313(15) 0.0299(15) 0.0166(12) -0.0003(10) -0.0038(10) -0.0138(12) C11 0.0385(17) 0.0426(16) 0.0198(13) -0.0090(11) 0.0011(12) -0.0154(14) C12 0.0476(19) 0.0515(19) 0.0283(15) -0.0032(13) 0.0010(13) -0.0246(16) C13 0.059(2) 0.080(3) 0.0245(16) 0.0004(16) 0.0054(15) -0.031(2) C14 0.056(2) 0.090(3) 0.0230(15) -0.0185(16) 0.0015(15) -0.028(2) C15 0.0452(19) 0.065(2) 0.0369(17) -0.0258(16) 0.0029(14) -0.0224(17) C16 0.0342(16) 0.0464(17) 0.0332(15) -0.0147(13) 0.0028(12) -0.0159(14) C17 0.0469(19) 0.0428(18) 0.0502(19) -0.0132(14) 0.0034(15) -0.0230(15) C18 0.077(3) 0.058(2) 0.0393(18) 0.0014(15) -0.0004(17) -0.041(2) C21 0.0291(14) 0.0181(12) 0.0293(14) -0.0016(10) -0.0069(11) -0.0056(11) C22 0.0330(15) 0.0300(14) 0.0276(14) -0.0036(11) -0.0048(12) -0.0070(12) C23 0.0403(17) 0.0272(14) 0.0361(16) -0.0081(12) -0.0111(13) -0.0033(13) C24 0.0476(18) 0.0209(13) 0.0447(17) 0.0002(12) -0.0199(14) -0.0113(13) C25 0.0383(17) 0.0323(15) 0.0353(16) 0.0067(12) -0.0109(13) -0.0173(13) C26 0.0300(15) 0.0282(14) 0.0277(14) 0.0011(11) -0.0059(11) -0.0098(12) C27 0.052(2) 0.0425(18) 0.0345(16) -0.0078(13) 0.0078(14) -0.0104(15) C28 0.0447(19) 0.0402(17) 0.0351(16) -0.0005(13) 0.0074(14) -0.0121(14) C31 0.0333(15) 0.0164(12) 0.0387(15) -0.0012(11) -0.0137(12) -0.0084(11) C32 0.0403(17) 0.0317(15) 0.0451(18) 0.0048(13) -0.0146(14) -0.0186(13) C33 0.061(2) 0.0305(17) 0.079(3) 0.0176(17) -0.024(2) -0.0244(17) C34 0.054(2) 0.0216(15) 0.092(3) -0.0083(17) -0.013(2) -0.0059(15) C35 0.045(2) 0.0298(16) 0.070(2) -0.0162(16) -0.0085(17) -0.0064(14) C36 0.0345(16) 0.0272(14) 0.0411(16) -0.0082(12) -0.0107(13) -0.0076(12) C37 0.054(2) 0.054(2) 0.0413(18) 0.0140(15) -0.0148(16) -0.0318(17) C38 0.0409(18) 0.0411(17) 0.0361(16) -0.0078(13) 0.0003(13) -0.0085(14) S 0.0326(4) 0.0237(3) 0.0318(4) -0.0037(3) -0.0025(3) -0.0087(3) C99 0.0330(17) 0.0396(17) 0.0410(17) 0.0005(13) -0.0034(13) -0.0147(14) F1 0.0678(14) 0.1025(17) 0.0322(10) -0.0035(10) -0.0025(9) -0.0417(13) F2 0.0414(11) 0.0409(11) 0.0996(17) 0.0086(10) -0.0304(11) -0.0086(9) F3 0.0483(11) 0.0439(10) 0.0659(12) -0.0110(9) -0.0061(9) -0.0265(9) O2 0.0385(12) 0.0315(11) 0.0598(14) -0.0009(9) -0.0058(10) -0.0168(9) O3 0.0434(13) 0.0298(11) 0.0572(14) -0.0076(10) -0.0143(11) -0.0006(10) O4 0.0669(16) 0.0517(14) 0.0397(12) -0.0159(10) 0.0153(11) -0.0279(12) C90 0.060(2) 0.0372(17) 0.0417(18) -0.0015(14) -0.0098(16) -0.0184(16) Cl1 0.0562(6) 0.0643(6) 0.0832(7) -0.0006(5) -0.0217(5) -0.0174(5) Cl2 0.0547(6) 0.0912(8) 0.0734(7) -0.0280(6) -0.0099(5) -0.0289(5) Cl3 0.1280(11) 0.1098(10) 0.0542(6) -0.0354(6) 0.0115(7) -0.0307(9)