The Isolation of [Pd{OC(O)H}(H)(NHC)(PR3)] (NHC = N-Heterocyclic Carbene) and Its Role in Alkene and Alkyne Reductions Using Formic Acid
Julie Broggi; Václav Jurčík; Olivier Songis; Albert Poater; Luigi Cavallo; Alexandra M. Z. Slawin; Catherine S. J. Cazin; Journal of the American Chemical Society 135 (2013) 4588–4591; doi:10.1021/ja311087c

data_4119496
_publ_section_title
;
 The Isolation of [Pd{OC(O)H}(H)(NHC)(PR3)] (NHC = N-Heterocyclic Carbene)
 and Its Role in Alkene and Alkyne Reductions Using Formic Acid
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4588
_journal_page_last               4591
_journal_paper_doi               10.1021/ja311087c
_journal_volume                  135
_journal_year                    2013
_chemical_formula_moiety         'C46 H71 N2 O2 P Pd,2(C4 H8 O)'
_chemical_formula_sum            'C54 H87 N2 O4 P Pd'
_chemical_formula_weight         965.63
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   16.206(4)
_cell_length_b                   25.131(6)
_cell_length_c                   25.621(6)
_cell_measurement_reflns_used    17919
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      28.9186
_cell_measurement_theta_min      2.1826
_cell_volume                     10435(4)
_computing_cell_refinement       'CrystalClear (Rigaku Corp., 2004)'
_computing_data_collection       'CrystalClear (Rigaku Corp., 2004)'
_computing_data_reduction        'CrystalClear (Rigaku Corp., 2004)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      93(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  CCD
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  confocal
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.2828
_diffrn_reflns_av_sigmaI/netI    0.1824
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            62653
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.33
_diffrn_reflns_theta_min         2.18
_exptl_absorpt_coefficient_mu    0.430
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.9555
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.229
_exptl_crystal_description       Prism
_exptl_crystal_F_000             4144
_exptl_crystal_size_max          0.1200
_exptl_crystal_size_mid          0.1200
_exptl_crystal_size_min          0.1000
_refine_diff_density_max         1.193
_refine_diff_density_min         -1.099
_refine_diff_density_rms         0.129
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     563
_refine_ls_number_reflns         9478
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.1742
_refine_ls_R_factor_gt           0.0911
_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^)+(0.0698P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1796
_refine_ls_wR_factor_ref         0.2133
_reflns_number_gt                5253
_reflns_number_total             9478
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja311087c_si_002.cif
_cod_data_source_block           hydride
_cod_database_code               4119496