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_4103326
_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         'C24 H19 N3 O4 Pd, 10(H2 O)'
_chemical_formula_sum            'C24 H39 N3 O14 Pd'
_chemical_formula_weight         699.98
_chemical_name_common            Pd-complex
_chemical_name_systematic
;
Pd-complex
;
_space_group_IT_number           1
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  'P 1'
_symmetry_space_group_name_H-M   'P 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'SHELXL-97 & ZCIF'
_cell_angle_alpha                79.5984(9)
_cell_angle_beta                 88.5172(10)
_cell_angle_gamma                86.6206(9)
_cell_formula_units_Z            1
_cell_length_a                   8.4848(5)
_cell_length_b                   8.6172(5)
_cell_length_c                   10.4326(7)
_cell_measurement_reflns_used    16138
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      32.3
_cell_measurement_theta_min      2.4
_cell_volume                     748.85(8)
_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 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_details      366,366,366,720,720
_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      -0.0288049
_diffrn_orient_matrix_UB_12      0.0635175
_diffrn_orient_matrix_UB_13      -0.0870322
_diffrn_orient_matrix_UB_21      -0.0943727
_diffrn_orient_matrix_UB_22      -0.0638167
_diffrn_orient_matrix_UB_23      -0.0016745
_diffrn_orient_matrix_UB_31      -0.0648567
_diffrn_orient_matrix_UB_32      0.0765247
_diffrn_orient_matrix_UB_33      0.0438435
_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  0.0137
_diffrn_reflns_av_sigmaI/netI    0.0182
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            15942
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         1.98
_diffrn_source_current           30.00
_diffrn_source_voltage           50.00
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.691
_exptl_absorpt_correction_T_max  0.871
_exptl_absorpt_correction_T_min  0.783
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.552
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             362
_exptl_crystal_id
'Vedern/Oloo 3-C-Pd-IV m-benzyl, HOOH, H2O, NaOH 150K'
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.522
_refine_diff_density_min         -0.429
_refine_diff_density_rms         0.053
_refine_ls_abs_structure_details '(Flack, 1983)'
_refine_ls_abs_structure_Flack   0.455(16)
_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     444
_refine_ls_number_reflns         8188
_refine_ls_number_restraints     103
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.0208
_refine_ls_R_factor_gt           0.0208
_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^)+(0.01P)^2^+0.626P], P=(max(Fo^2^,0)+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0492
_refine_ls_wR_factor_ref         0.0492
_reflns_Friedel_coverage         0.888
_reflns_number_gt                8177
_reflns_number_total             8188
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja107185w_si_007.cif
_cod_data_source_block           1925
_cod_depositor_comments
;
The following automatic conversions were performed:

'_atom_sites_solution_hydrogens' value 'geom,difmap' was changed to
'mixed'.

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 
;
_cod_database_code               4103326
_diffrn_measurement_frame_width-ccd -0.5
_diffrn_measurement_total_frames-ccd 2538
_diffrn_measurement_frame_time-ccd 10
_diffrn_measurement_total_time-ccd 11.3
_diffrn_detector_distance-ccd    5.000
_diffrn_measurement_frame_size-ccd 512