data_1100803 _publ_requested_journal 'Organometallics' _publ_section_title ; The reactivity of [Pd{CH2C(O)Me}Cl]n toward Isocyanides. ; _chemical_formula_sum 'C13 H23 Cl N2 O Pd' _chemical_formula_weight 365.18 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' 'O' 'O' 0.0106 0.0060 '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' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'Pca21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y, z' '-x+1/2, y, z+1/2' _cell_length_a 18.2636(11) _cell_length_b 9.3501(4) _cell_length_c 9.2895(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1586.34(14) _cell_formula_units_Z 4 _cell_measurement_temperature 133(2) _cell_measurement_reflns_used 7094 _cell_measurement_theta_min 2.45 _cell_measurement_theta_max 30.47 _exptl_crystal_description tablet _exptl_crystal_colour colourless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.529 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 744 _exptl_absorpt_coefficient_mu 1.330 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.6419 _exptl_absorpt_correction_T_max 0.8799 _exptl_absorpt_process_details XPREP loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0.00 0.00 -1.00 0.1900 0.00 -1.00 0.00 0.0420 0.00 1.00 0.00 0.0560 1.00 0.00 0.00 0.1880 -1.00 0.00 0.00 0.1550 -2.00 0.00 -1.00 0.1720 3.00 0.00 -2.00 0.1950 2.00 -1.00 3.00 0.1530 -1.00 0.00 1.00 0.2340 _diffrn_ambient_temperature 133(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 'Bruker smart 1000 CCD' _diffrn_measurement_method '\w- & \f-scan' _diffrn_detector_area_resol_mean 8.192 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 31977 _diffrn_reflns_av_R_equivalents 0.0289 _diffrn_reflns_av_sigmaI/netI 0.0163 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.18 _diffrn_reflns_theta_max 30.03 _reflns_number_total 4637 _reflns_number_gt 4447 _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^)+(0.0242P)^2^+0.0210P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment 'NH free with DFIX, methyls rigid, others riding' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.020(16) _refine_ls_number_reflns 4637 _refine_ls_number_parameters 174 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0166 _refine_ls_R_factor_gt 0.0152 _refine_ls_wR_factor_ref 0.0386 _refine_ls_wR_factor_gt 0.0381 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.044 _refine_ls_shift/su_max 0.077 _refine_ls_shift/su_mean 0.002 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 0.894076(4) 0.618848(8) 0.74628(2) 0.01817(3) Uani 1 1 d . . . Cl Cl 0.94570(2) 0.71392(4) 0.96038(4) 0.02777(7) Uani 1 1 d . . . O O 0.83158(6) 0.79624(10) 0.71227(11) 0.0248(2) Uani 1 1 d . . . C1 C 0.84585(8) 0.55467(15) 0.56498(15) 0.0207(3) Uani 1 1 d . . . C2 C 0.79308(8) 0.65563(16) 0.51966(18) 0.0242(3) Uani 1 1 d . . . H2 H 0.7625 0.6402 0.4385 0.029 Uiso 1 1 calc R . . C3 C 0.78927(8) 0.77854(15) 0.60211(17) 0.0239(3) Uani 1 1 d . . . N1 N 0.86133(7) 0.43315(14) 0.49802(13) 0.0221(2) Uani 1 1 d D . . H01 H 0.9010(10) 0.395(3) 0.521(4) 0.061(10) Uiso 1 1 d D . . N2 N 0.95833(7) 0.32290(13) 0.80924(14) 0.0222(2) Uani 1 1 d . . . C4 C 0.73723(10) 0.89860(17) 0.5688(2) 0.0342(4) Uani 1 1 d . . . H4A H 0.7082 0.9209 0.6547 0.041 Uiso 1 1 calc R . . H4B H 0.7045 0.8698 0.4904 0.041 Uiso 1 1 calc R . . H4C H 0.7650 0.9834 0.5397 0.041 Uiso 1 1 calc R . . C5 C 0.83110(8) 0.37294(15) 0.36133(16) 0.0220(3) Uani 1 1 d . . . C6 C 0.86537(9) 0.22455(17) 0.34627(18) 0.0275(3) Uani 1 1 d . . . H6A H 0.9187 0.2338 0.3392 0.033 Uiso 1 1 calc R . . H6B H 0.8465 0.1782 0.2593 0.033 Uiso 1 1 calc R . . H6C H 0.8529 0.1666 0.4307 0.033 Uiso 1 1 calc R . . C7 C 0.74815(9) 0.35358(18) 0.3726(2) 0.0310(3) Uani 1 1 d . . . H7A H 0.7366 0.2964 0.4580 0.037 Uiso 1 1 calc R . . H7B H 0.7301 0.3045 0.2864 0.037 Uiso 1 1 calc R . . H7C H 0.7246 0.4475 0.3806 0.037 Uiso 1 1 calc R . . C8 C 0.85330(8) 0.46777(17) 0.2358(2) 0.0328(3) Uani 1 1 d . . . H8A H 0.8336 0.5642 0.2503 0.039 Uiso 1 1 calc R . . H8B H 0.8338 0.4279 0.1461 0.039 Uiso 1 1 calc R . . H8C H 0.9068 0.4723 0.2301 0.039 Uiso 1 1 calc R . . C9 C 0.93967(7) 0.43716(16) 0.78196(14) 0.0213(3) Uani 1 1 d . . . C10 C 0.97263(8) 0.17277(15) 0.84504(16) 0.0225(3) Uani 1 1 d . . . C11 C 1.05497(9) 0.14802(19) 0.8375(2) 0.0322(3) Uani 1 1 d . . . H11A H 1.0724 0.1687 0.7399 0.039 Uiso 1 1 calc R . . H11B H 1.0658 0.0482 0.8615 0.039 Uiso 1 1 calc R . . H11C H 1.0797 0.2112 0.9061 0.039 Uiso 1 1 calc R . . C12 C 0.94246(12) 0.1488(2) 0.9961(2) 0.0396(4) Uani 1 1 d . . . H12A H 0.9680 0.2114 1.0641 0.048 Uiso 1 1 calc R . . H12B H 0.9499 0.0487 1.0239 0.048 Uiso 1 1 calc R . . H12C H 0.8900 0.1707 0.9973 0.048 Uiso 1 1 calc R . . C13 C 0.93160(9) 0.08318(16) 0.7352(3) 0.0328(3) Uani 1 1 d . . . H13A H 0.8792 0.1052 0.7403 0.039 Uiso 1 1 calc R . . H13B H 0.9392 -0.0185 0.7559 0.039 Uiso 1 1 calc R . . H13C H 0.9499 0.1050 0.6385 0.039 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 Pd 0.01994(4) 0.01501(4) 0.01957(5) -0.00072(6) -0.00061(6) -0.00074(3) Cl 0.03078(16) 0.02726(17) 0.02527(16) -0.00669(14) -0.00447(15) -0.00052(14) O 0.0253(5) 0.0168(4) 0.0323(6) -0.0022(4) -0.0029(4) 0.0019(4) C1 0.0210(6) 0.0192(6) 0.0218(6) 0.0014(5) 0.0015(5) -0.0024(5) C2 0.0221(6) 0.0231(7) 0.0275(7) -0.0004(6) -0.0036(6) 0.0000(5) C3 0.0202(6) 0.0207(6) 0.0308(8) 0.0032(6) 0.0013(6) -0.0009(5) N1 0.0245(6) 0.0213(6) 0.0204(6) -0.0022(5) -0.0056(5) 0.0023(5) N2 0.0242(6) 0.0213(6) 0.0211(5) -0.0002(5) -0.0018(5) 0.0005(5) C4 0.0287(8) 0.0253(8) 0.0487(11) -0.0021(7) -0.0053(8) 0.0068(6) C5 0.0218(6) 0.0250(7) 0.0192(7) -0.0039(5) -0.0035(5) -0.0002(5) C6 0.0285(8) 0.0273(8) 0.0266(7) -0.0073(6) -0.0009(6) 0.0016(6) C7 0.0236(7) 0.0333(8) 0.0359(9) -0.0088(7) -0.0016(6) -0.0025(6) C8 0.0387(8) 0.0356(7) 0.0240(8) 0.0037(9) -0.0033(8) -0.0054(6) C9 0.0215(6) 0.0235(7) 0.0188(7) -0.0026(5) -0.0012(5) -0.0015(5) C10 0.0265(7) 0.0174(6) 0.0236(7) 0.0020(5) -0.0005(6) 0.0033(5) C11 0.0257(7) 0.0320(8) 0.0388(9) 0.0038(7) -0.0040(7) 0.0067(6) C12 0.0497(11) 0.0404(10) 0.0287(9) 0.0113(7) 0.0094(8) 0.0142(8) C13 0.0346(7) 0.0219(6) 0.0418(10) -0.0044(9) -0.0071(9) -0.0041(5)