Preparation and C-X Reductive Elimination Reactivity of Monoaryl PdIV-X Complexes in Water (X = OH, OH2, Cl, Br)
Williamson Oloo; Peter Y. Zavalij; Jing Zhang; Eugene Khaskin; Andrei N. Vedernikov; Journal of the American Chemical Society 132 (2010) 14400–14402; doi:10.1021/ja107185w

data_4103323
_publ_section_title
;
 Preparation and C-X Reductive Elimination Reactivity of Monoaryl PdIV-X
 Complexes in Water (X = OH, OH2, Cl, Br)
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              14400
_journal_page_last               14402
_journal_paper_doi               10.1021/ja107185w
_journal_volume                  132
_journal_year                    2010
_chemical_formula_moiety         'C23 H20 N3 O3 Pd, C2 H3 O2, (C3 H6 O)0.925'
_chemical_formula_sum            'C27.775 H28.55 N3 O5.925 Pd'
_chemical_formula_weight         605.59
_chemical_name_common            'Pd-complex acetate'
_chemical_name_systematic
;
Pd-complex acetate, acetone
;
_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 & ZCIF'
_cell_angle_alpha                90.00
_cell_angle_beta                 107.340(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.0970(16)
_cell_length_b                   17.566(2)
_cell_length_c                   13.4039(16)
_cell_measurement_reflns_used    18284
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      27.9
_cell_measurement_theta_min      2.2
_cell_volume                     2943.6(6)
_computing_cell_refinement       Apex2
_computing_data_collection       'Apex2 (Bruker, 2005)'
_computing_data_reduction        Apex2
_computing_molecular_graphics    'XSHEL (Bruker, 2004)'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 11.198
_diffrn_detector_type            'Bruker Smart Apex II'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details      610,610,380
_diffrn_measurement_device_type  'three-circle diffractometer'
_diffrn_measurement_method       '\w scans'
_diffrn_measurement_specimen_support 'glass capillary'
_diffrn_orient_matrix_type       standard
_diffrn_orient_matrix_UB_11      -0.0769723
_diffrn_orient_matrix_UB_12      0.0040630
_diffrn_orient_matrix_UB_13      -0.0028355
_diffrn_orient_matrix_UB_21      -0.0108878
_diffrn_orient_matrix_UB_22      -0.0547603
_diffrn_orient_matrix_UB_23      -0.0208645
_diffrn_orient_matrix_UB_31      0.0188371
_diffrn_orient_matrix_UB_32      -0.0150194
_diffrn_orient_matrix_UB_33      0.0752671
_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  0.0346
_diffrn_reflns_av_sigmaI/netI    0.0235
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            26369
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.91
_diffrn_source_current           30.00
_diffrn_source_voltage           50.00
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.672
_exptl_absorpt_correction_T_max  0.905
_exptl_absorpt_correction_T_min  0.721
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.366
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1238
_exptl_crystal_id                'Vedern/Oloo 4-C-O-Pd 200K vial#2'
_exptl_crystal_size_max          0.495
_exptl_crystal_size_mid          0.245
_exptl_crystal_size_min          0.15
_platon_squeeze_details
; 215 electorns corresponds to 3.7 acetone molecules per unit cell or
0.925 molecule per asymmetric unit.
;
_refine_diff_density_max         0.668
_refine_diff_density_min         -0.976
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     330
_refine_ls_number_reflns         5185
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.0404
_refine_ls_R_factor_gt           0.0357
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.001P)^2^+8.17P], P=(max(Fo^2^,0)+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0783
_refine_ls_wR_factor_ref         0.0798
_reflns_number_gt                4587
_reflns_number_total             5185
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja107185w_si_004.cif
_cod_data_source_block           1850
_cod_database_code               4103323
_diffrn_measurement_frame_width-ccd -0.3
_diffrn_measurement_total_frames-ccd 1600
_diffrn_measurement_frame_time-ccd 20
_diffrn_measurement_total_time-ccd 12
_diffrn_detector_distance-ccd    5.000
_diffrn_measurement_frame_size-ccd 512