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_4113456
_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            'C36 H35 I N O P Pd'
_chemical_formula_weight         761.92
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 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                 112.07(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.619(8)
_cell_length_b                   36.11(2)
_cell_length_c                   10.078(18)
_cell_measurement_temperature    293(2)
_cell_volume                     3244(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.495
_diffrn_measured_fraction_theta_max 0.495
_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  0.0292
_diffrn_reflns_av_sigmaI/netI    0.3257
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       50
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -2
_diffrn_reflns_number            4933
_diffrn_reflns_theta_full        29.98
_diffrn_reflns_theta_max         29.98
_diffrn_reflns_theta_min         2.35
_exptl_absorpt_coefficient_mu    1.601
_exptl_crystal_density_diffrn    1.560
_exptl_crystal_F_000             1520
_refine_diff_density_max         0.736
_refine_diff_density_min         -0.675
_refine_diff_density_rms         0.106
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.05(3)
_refine_ls_extinction_expression Fc
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.758
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     370
_refine_ls_number_reflns         4933
_refine_ls_number_restraints     134
_refine_ls_restrained_S_all      0.749
_refine_ls_R_factor_all          0.2056
_refine_ls_R_factor_gt           0.0394
_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^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0423
_refine_ls_wR_factor_ref         0.0629
_reflns_number_gt                1947
_reflns_number_total             4933
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja029114w_s3_1.cif
_cod_data_source_block           sofc42a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0000P)^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^)+(0.0000P)^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               4113456