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_4104887
_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            'C63 H74 F3 N2 O3 Pd S Tl'
_chemical_formula_weight         1307.07
_chemical_name_common            '[TlPd(CNArDipp2)2]OTf'
_chemical_name_systematic
; 
 ? 
;
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                67.20(3)
_cell_angle_beta                 70.62(3)
_cell_angle_gamma                71.18(3)
_cell_formula_units_Z            2
_cell_length_a                   13.964(3)
_cell_length_b                   16.224(3)
_cell_length_c                   17.605(4)
_cell_measurement_reflns_used    26826
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23.26
_cell_measurement_theta_min      1.40
_cell_volume                     3381.1(15)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_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 0.962
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\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  0.0556
_diffrn_reflns_av_sigmaI/netI    0.0710
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            26826
_diffrn_reflns_theta_full        23.26
_diffrn_reflns_theta_max         23.26
_diffrn_reflns_theta_min         1.40
_exptl_absorpt_coefficient_mu    2.724
_exptl_absorpt_correction_T_max  0.8115
_exptl_absorpt_correction_T_min  0.7723
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            Yellow-Orange
_exptl_crystal_density_diffrn    1.284
_exptl_crystal_description       Block
_exptl_crystal_F_000             1320
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_platon_squeeze_details
;
SQUEEZE was employed to account for severely disordered molecules of ET2O
(C4H10O).  A total of 117 electrons in a solvent accessible void of 
612.9 Ang^3 were accounted for.  This corresponds to roughly 3
disordered molecules of Et2O per unit cell.  
;
_refine_diff_density_max         1.097
_refine_diff_density_min         -1.217
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     667
_refine_ls_number_reflns         9345
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0628
_refine_ls_R_factor_gt           0.0450
_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^)+(0.0459P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0956
_refine_ls_wR_factor_ref         0.1053
_reflns_number_gt                7324
_reflns_number_total             9345
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja905338x_si_002_5.cif
_cod_data_source_block           jfig176
_cod_original_cell_volume        3380.9(12)
_cod_database_code               4104887