Bond Activation, Substrate Addition and Catalysis by an Isolable Two-Coordinate Pd(0) Bis-Isocyanide Monomer
Liezel A. Labios; Matthew D. Millard; Arnold L. Rheingold; Joshua S. Figueroa; Journal of the American Chemical Society 131 (2009) 11318–11319; doi:10.1021/ja905338x

data_4104886
_publ_section_title
;
 Bond Activation, Substrate Addition and Catalysis by an Isolable
 Two-Coordinate Pd(0) Bis-Isocyanide Monomer
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11318
_journal_page_last               11319
_journal_paper_doi               10.1021/ja905338x
_journal_volume                  131
_journal_year                    2009
_chemical_formula_sum            'C75 H95 Br N2 O Pd'
_chemical_formula_weight         1226.84
_chemical_name_common            Pd(Br)(Mes)(CNArDipp2)2
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 90.998(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.2424(10)
_cell_length_b                   14.6791(11)
_cell_length_c                   18.6713(15)
_cell_measurement_reflns_used    9920
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      68.43
_cell_measurement_theta_min      3.83
_cell_volume                     3354.9(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_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      100(2)
_diffrn_measured_fraction_theta_full 0.921
_diffrn_measured_fraction_theta_max 0.921
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0294
_diffrn_reflns_av_sigmaI/netI    0.0616
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            18340
_diffrn_reflns_theta_full        68.43
_diffrn_reflns_theta_max         68.43
_diffrn_reflns_theta_min         2.37
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.246
_exptl_absorpt_correction_T_max  0.7372
_exptl_absorpt_correction_T_min  0.5629
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            Pale-yellow
_exptl_crystal_density_diffrn    1.214
_exptl_crystal_density_meas      0
_exptl_crystal_description       Block
_exptl_crystal_F_000             1296
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.619
_refine_diff_density_min         -0.794
_refine_diff_density_rms         0.062
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.014(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.995
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     742
_refine_ls_number_reflns         9192
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.995
_refine_ls_R_factor_all          0.0305
_refine_ls_R_factor_gt           0.0273
_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^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0590
_refine_ls_wR_factor_ref         0.0603
_reflns_number_gt                8666
_reflns_number_total             9192
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja905338x_si_002_4.cif
_cod_data_source_block           jfig157
_cod_database_code               4104886