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_4103324
_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 H17 N3 O4 Pd, 7(H2 O)'
_chemical_formula_sum            'C23 H31 N3 O11 Pd'
_chemical_formula_weight         631.91
_chemical_name_common            Pd-complex
_chemical_name_systematic
;
Pd-complex
;
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   difmap
_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                   17.0379(14)
_cell_length_b                   8.0260(7)
_cell_length_c                   18.8860(16)
_cell_measurement_reflns_used    14779
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      31.0
_cell_measurement_theta_min      2.4
_cell_volume                     2582.6(4)
_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      150(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_device_type  'three-circle diffractometer'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_measurement_specimen_support 'MiTeGen loop'
_diffrn_orient_matrix_type       standard
_diffrn_orient_matrix_UB_11      -0.0585073
_diffrn_orient_matrix_UB_12      0.0009131
_diffrn_orient_matrix_UB_13      -0.0041806
_diffrn_orient_matrix_UB_21      0.0043800
_diffrn_orient_matrix_UB_22      -0.0336123
_diffrn_orient_matrix_UB_23      -0.0508336
_diffrn_orient_matrix_UB_31      -0.0016611
_diffrn_orient_matrix_UB_32      -0.1199782
_diffrn_orient_matrix_UB_33      0.0142248
_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  0.0173
_diffrn_reflns_av_sigmaI/netI    0.0147
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            30887
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         2.16
_diffrn_source_current           30.00
_diffrn_source_voltage           50.00
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.784
_exptl_absorpt_correction_T_max  0.917
_exptl_absorpt_correction_T_min  0.828
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.625
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1296
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.376
_refine_diff_density_min         -0.354
_refine_diff_density_rms         0.056
_refine_ls_abs_structure_details '(Flack, 1983)'
_refine_ls_abs_structure_Flack   0.36(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     388
_refine_ls_number_reflns         7481
_refine_ls_number_restraints     113
_refine_ls_restrained_S_all      0.995
_refine_ls_R_factor_all          0.0269
_refine_ls_R_factor_gt           0.0229
_refine_ls_shift/su_max          0.002
_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^+2.627P], P=(max(Fo^2^,0)+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0454
_refine_ls_wR_factor_ref         0.0469
_reflns_Friedel_coverage         0.929
_reflns_number_gt                6648
_reflns_number_total             7481
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja107185w_si_005.cif
_cod_data_source_block           1894
_cod_database_code               4103324