Cine-Substitution in the Stille Coupling: Evidence for the Carbenoid Reactivity of sp3-gem-Organodimetallic Iodopalladio-trialkylstannylalkane Intermediates
Eric Fillion; Nicholas J. Taylor; Journal of the American Chemical Society 125 (2003) 12700–12701; doi:10.1021/ja037409j

data_4114291
_publ_section_title
;
 Cine-Substitution in the Stille Coupling: Evidence for the Carbenoid
 Reactivity of sp3-gem-Organodimetallic Iodopalladio-trialkylstannylalkane
 Intermediates
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12700
_journal_page_last               12701
_journal_paper_doi               10.1021/ja037409j
_journal_volume                  125
_journal_year                    2003
_chemical_formula_sum            'C28 H46 Cl6 Fe I2 P2 Pd'
_chemical_formula_weight         1073.34
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     'Patterson and Fourier'
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 109.591(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.8823(11)
_cell_length_b                   12.4917(9)
_cell_length_c                   21.3487(15)
_cell_measurement_reflns_used    6724
_cell_measurement_temperature    150(1)
_cell_measurement_theta_max      30.03
_cell_measurement_theta_min      2.54
_cell_volume                     3990.3(5)
_computing_cell_refinement       SAINT
_computing_data_collection       SMART
_computing_data_reduction        SAINT
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  SHELXTL
_computing_structure_solution    SHELXTL
_diffrn_ambient_temperature      150(1)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX'
_diffrn_measurement_method       Omega
_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  0.0443
_diffrn_reflns_av_sigmaI/netI    0.0435
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            37284
_diffrn_reflns_theta_full        30.04
_diffrn_reflns_theta_max         30.04
_diffrn_reflns_theta_min         1.40
_exptl_absorpt_coefficient_mu    2.862
_exptl_absorpt_correction_T_max  0.8687
_exptl_absorpt_correction_T_min  0.6092
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'Face-indexed analytical'
_exptl_crystal_colour            red-black
_exptl_crystal_density_diffrn    1.787
_exptl_crystal_description       Plate
_exptl_crystal_F_000             2096
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.048
_refine_diff_density_max         1.190
_refine_diff_density_min         -1.219
_refine_diff_density_rms         0.125
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.371
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     373
_refine_ls_number_reflns         11631
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.371
_refine_ls_R_factor_all          0.0592
_refine_ls_R_factor_gt           0.0494
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0200P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0841
_refine_ls_wR_factor_ref         0.0866
_reflns_number_gt                10218
_reflns_number_total             11631
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja037409jsi20030719_052047.cif
_cod_data_source_block           ef1141m
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Integration' changed to
'integration' according to the built-in table from CIF Core
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_formula_sum        'C28 H46 Cl6 Fe1 I2 P2 Pd1'
_cod_database_code               4114291