Unexpected isolation, and structural characterization, of a β-hydrogen-containing σ-alkylpalladium halide complex in the course of an intramolecular Heck reaction. Synthesis of polycyclic isoquinoline derivatives
Clique, Blandine; Fabritius, Charles-Henry; Couturier, Cédric; Monteiro, Nuno; Balme, Geneviève; Chemical Communications (Cambridge, United Kingdom)  (2003) 272–273; doi:10.1039/b211856b

data_7103941
_publ_section_title
;
 Unexpected isolation, and structural characterization, of a
 \b-hydrogen-containing \s-alkylpalladium halide complex in the course of
 an intramolecular Heck reaction. Synthesis of polycyclic isoquinoline
 derivatives
;
_journal_coden_ASTM              CHCOFS
_journal_issue                   2
_journal_name_full
;
 Chemical Communications (Cambridge, United Kingdom)
;
_journal_page_first              272
_journal_page_last               273
_journal_paper_doi               10.1039/b211856b
_journal_year                    2003
_chemical_formula_moiety         '(C40 H37 I N O4 P Pd),1/2(C H2 Cl2)'
_chemical_formula_sum            'C40.5 H38 Cl I N O4 P Pd'
_chemical_formula_weight         902.44
_chemical_name_systematic
;
((9-methylene-5,6-dihydro-10,10-dimethoxycarbonyl-benzo(f)
pyrrolidino(2,1-a)isoquinoline-5-methyl)Pd(PPh3)I), C40H37NO4IPPd
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                86.99(3)
_cell_angle_beta                 78.04(3)
_cell_angle_gamma                68.60(3)
_cell_formula_units_Z            2
_cell_length_a                   11.291(2)
_cell_length_b                   12.161(2)
_cell_length_c                   15.324(3)
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      1
_cell_volume                     1915.8(7)
_computing_cell_refinement       'DENZO (Otwinowski & Minor, 1997)'
_computing_data_collection       'Kappa CCD Server Software (Nonius, 1997)'
_computing_data_reduction        'DENZO (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'PLATON (Spek, 1999)'
_computing_publication_material  'SHELXTL (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 1997)'
_computing_structure_solution    'SHELXTL (Sheldrick, 1997)'
_diffrn_ambient_temperature      273(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Nonius Kappa CCD diffractometer'
_diffrn_measurement_method       'area detector'
_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  0.1260
_diffrn_reflns_av_sigmaI/netI    0.1044
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            22340
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.36
_exptl_absorpt_coefficient_mu    1.442
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.564
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rhombic
_exptl_crystal_F_000             902
_exptl_crystal_size_max          0.7
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.412
_refine_diff_density_min         -1.143
_refine_diff_density_rms         0.160
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     451
_refine_ls_number_reflns         8721
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0873
_refine_ls_R_factor_gt           0.0572
_refine_ls_shift/su_max          0.026
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0884P)^2^+0.1549P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1506
_refine_ls_wR_factor_ref         0.1757
_reflns_number_gt                6175
_reflns_number_total             8721
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b211856b.txt
_cod_data_source_block           cf41f2
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C40.50 H38 Cl I N O4 P Pd'
_cod_database_code               7103941