Intramolecular Pd-Mediated Processes of Amino-Tethered Aryl Halides and Ketones: Insight into the Ketone α-Arylation and Carbonyl-Addition Dichotomy. A New Class of Four-Membered Azapalladacycles
Daniel Solé; Lluís Vallverdú; Xavier Solans; Mercè Font-Bardía; Josep Bonjoch; Journal of the American Chemical Society 125 (2003) 1587–1594; doi:10.1021/ja029114w

data_4113457
_publ_section_title
;
 Intramolecular Pd-Mediated Processes of Amino-Tethered Aryl Halides and
 Ketones: Insight into the Ketone \a-Arylation and Carbonyl-Addition
 Dichotomy. A New Class of Four-Membered Azapalladacycles
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1587
_journal_page_last               1594
_journal_paper_doi               10.1021/ja029114w
_journal_volume                  125
_journal_year                    2003
_chemical_formula_sum            'C38 H37 Cl2 I N O P Pd'
_chemical_formula_weight         858.86
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.54
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.7190(10)
_cell_length_b                   20.6330(10)
_cell_length_c                   17.7930(10)
_cell_measurement_temperature    293(2)
_cell_volume                     3567.9(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.695
_diffrn_measured_fraction_theta_max 0.695
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0319
_diffrn_reflns_av_sigmaI/netI    0.0460
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            17632
_diffrn_reflns_theta_full        28.86
_diffrn_reflns_theta_max         28.86
_diffrn_reflns_theta_min         1.97
_exptl_absorpt_coefficient_mu    1.611
_exptl_crystal_density_diffrn    1.599
_exptl_crystal_F_000             1712
_refine_diff_density_max         0.590
_refine_diff_density_min         -0.741
_refine_diff_density_rms         0.122
_refine_ls_extinction_expression Fc
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.906
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     401
_refine_ls_number_reflns         6928
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      0.907
_refine_ls_R_factor_all          0.0766
_refine_ls_R_factor_gt           0.0319
_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^)+(0.0761P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0880
_refine_ls_wR_factor_ref         0.1156
_reflns_number_gt                4320
_reflns_number_total             6928
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja029114w_s3_2.cif
_cod_data_source_block           sofm66b
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0761P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0761P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4113457