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_4103322
_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_absolute_configuration ad
_chemical_formula_moiety
'(C23 H18 N3 O4 Pd 1+), (C2 H3 O2 1-), (C H4 O)'
_chemical_formula_sum            'C26 H25 N3 O7 Pd'
_chemical_formula_weight         597.89
_chemical_name_common            Pd-complex
_chemical_name_systematic
;
Pd-complex
;
_space_group_IT_number           29
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.4911(7)
_cell_length_b                   8.1017(4)
_cell_length_c                   23.2701(11)
_cell_measurement_reflns_used    9818
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      28.4
_cell_measurement_theta_min      2.6
_cell_volume                     2920.5(2)
_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 11.2
_diffrn_detector_type            'Bruker Smart Apex II'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details      610,610,610,120
_diffrn_measurement_device_type  'three-circle diffractometer'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_measurement_specimen_support 'nylon loop'
_diffrn_orient_matrix_type       standard
_diffrn_orient_matrix_UB_11      -0.0134244
_diffrn_orient_matrix_UB_12      -0.0051914
_diffrn_orient_matrix_UB_13      -0.0425783
_diffrn_orient_matrix_UB_21      0.0818529
_diffrn_orient_matrix_UB_22      -0.0482997
_diffrn_orient_matrix_UB_23      -0.0004984
_diffrn_orient_matrix_UB_31      -0.0914057
_diffrn_orient_matrix_UB_32      -0.0425126
_diffrn_orient_matrix_UB_33      0.0057938
_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  0.0389
_diffrn_reflns_av_sigmaI/netI    0.0209
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            28176
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         1.75
_diffrn_source_current           30.00
_diffrn_source_voltage           50.00
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.679
_exptl_absorpt_correction_T_max  0.960
_exptl_absorpt_correction_T_min  0.794
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.360
_exptl_crystal_description       prism
_exptl_crystal_F_000             1216
_exptl_crystal_id
'Vedernikov/Oloo Pd Acetophenone oxime-Pd-DPMS'
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.06
_platon_squeeze_details
;
 Due to strong disorder that cannot be reasonable modelled, methanol solvent
 and acetate ions were removed using SQUEEZE procedure. Total amount of the
 electron density removed was 380 e which corresponds to approximately one
 acetate ion CH3COO- and one methanol molecule CH3OH (four of each per unit
 cell).
;
_refine_diff_density_max         0.760
_refine_diff_density_min         -0.924
_refine_diff_density_rms         0.064
_refine_ls_abs_structure_details '(Flack, 1983)'
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     270
_refine_ls_number_reflns         3445
_refine_ls_number_restraints     49
_refine_ls_restrained_S_all      0.995
_refine_ls_R_factor_all          0.0444
_refine_ls_R_factor_gt           0.0343
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.01P)^2^+5.65P], P=(max(Fo^2^,0)+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0666
_refine_ls_wR_factor_ref         0.0695
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2577
_reflns_number_total             3445
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja107185w_si_003.cif
_cod_data_source_block           1765
_cod_original_sg_symbol_H-M      'P b c n'
_cod_database_code               4103322
_diffrn_measurement_frame_width-ccd -0.30
_diffrn_measurement_total_frames-ccd 1950
_diffrn_measurement_frame_time-ccd 30
_diffrn_measurement_total_time-ccd 19.5
_diffrn_detector_distance-ccd    5.000
_diffrn_measurement_frame_size-ccd 512