Thermal and Electrochemical C-X Activation (X = Cl, Br, I) by the Strong Lewis Acid Pd3(dppm)3(CO)2+ Cluster and Its Catalytic Applications
Frédéric Lemaître; Dominique Lucas; Katherine Groison; Philippe Richard; Yves Mugnier; Pierre D. Harvey; Journal of the American Chemical Society 125 (2003) 5511–5522; doi:10.1021/ja0297786

data_4113714
_publ_contact_author_address
;
L.S.E.O. facult\'e des sciences, 
6 Bd Gabriel 21000 Dijon, FRANCE
;
_publ_contact_author_email       prichard@u-bourgogne.fr
_publ_contact_author_fax         +33-0380396098
_publ_contact_author_name        'RICHARD, Philippe'
_publ_contact_author_phone       +33-0380396079
_publ_section_title
;
 Thermal and Electrochemical C-X Activation (X = Cl, Br, I) by the Strong
 Lewis Acid Pd3(dppm)3(CO)2+ Cluster and Its Catalytic Applications
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5511
_journal_page_last               5522
_journal_paper_doi               10.1021/ja0297786
_journal_volume                  125
_journal_year                    2003
_chemical_formula_sum            'C97 H90 F8 O3 P8 Pd3'
_chemical_formula_weight         2022.65
_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
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.2
_audit_creation_date             date
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90.00
_cell_angle_beta                 91.24
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.8603(1)
_cell_length_b                   37.0351(2)
_cell_length_c                   21.3783(2)
_cell_measurement_reflns_used    4245
_cell_measurement_temperature    110(2)
_cell_volume                     8596.60(12)
_computing_cell_refinement       'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'KappaCCD Server Software (Nonius,1997)'
_computing_data_reduction        'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'ORTEPIII (Burnett, 1996)'
_computing_publication_material  'SHELXL97 and WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 0.929
_diffrn_measured_fraction_theta_max 0.929
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       '\f scans (\k = 0) + additional \w scans'
_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  0.0282
_diffrn_reflns_av_sigmaI/netI    0.0549
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       46
_diffrn_reflns_limit_k_min       -48
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            34960
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         2.20
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.839
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.563
_exptl_crystal_description       prism
_exptl_crystal_F_000             4104
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.569
_refine_diff_density_min         -0.647
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.102
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     667
_refine_ls_number_reflns         18307
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.102
_refine_ls_R_factor_all          0.0606
_refine_ls_R_factor_gt           0.0405
_refine_ls_shift/su_max          0.272
_refine_ls_shift/su_mean         0.009
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0520P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1007
_refine_ls_wR_factor_ref         0.1059
_reflns_number_gt                13772
_reflns_number_total             18307
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0297786si20030106_123723.cif
_cod_data_source_block           mug3s
_cod_original_cell_volume        8596.61(12)
_cod_database_code               4113714