C‒CN Bond Cleavage Using Palladium Supported by a Dippe Ligand
Munjanja, Lloyd; Torres-López, Coralys; Brennessel, William W.; Jones, William D.; Organometallics 35 (2016) 2010–; doi:10.1021/acs.organomet.6b00304

data_4088687
_publ_section_title
;
 C--CN Bond Cleavage Using Palladium Supported by a Dippe Ligand
;
_journal_issue                   11
_journal_name_full               Organometallics
_journal_page_first              2010
_journal_paper_doi               10.1021/acs.organomet.6b00304
_journal_volume                  35
_journal_year                    2016
_chemical_formula_moiety         'C22 H50 B N P2 Pd'
_chemical_formula_sum            'C22 H50 B N P2 Pd'
_chemical_formula_weight         507.78
_chemical_name_common            jonlm07
_chemical_name_systematic
; 
 (dippe)Pd(Me)(CNBEt3)
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   28.6819(19)
_cell_length_b                   9.0185(6)
_cell_length_c                   21.1144(14)
_cell_measurement_reflns_used    3957
_cell_measurement_temperature    100.0(5)
_cell_measurement_theta_max      34.14
_cell_measurement_theta_min      2.46
_cell_volume                     5461.6(6)
_computing_cell_refinement       'SAINT (Bruker, 2013)'
_computing_data_collection       'APEX2 (Bruker, 2013)'
_computing_data_reduction        'SAINT (Bruker, 2013)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SIR2011 (Burla et al., 2012)'
_diffrn_ambient_temperature      100.0(5)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker SMART APEX II CCD platform'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0936
_diffrn_reflns_av_unetI/netI     0.0794
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       46
_diffrn_reflns_limit_h_min       -46
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            112832
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        34.970
_diffrn_reflns_theta_max         34.984
_diffrn_reflns_theta_min         1.420
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.804
_exptl_absorpt_correction_T_max  0.7476
_exptl_absorpt_correction_T_min  0.6490
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2012)'
_exptl_crystal_colour            yellow-orange
_exptl_crystal_density_diffrn    1.235
_exptl_crystal_description       plate
_exptl_crystal_F_000             2160
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         7.141
_refine_diff_density_min         -3.725
_refine_diff_density_rms         0.257
_refine_ls_abs_structure_details
; 
 Refined as an inversion twin. 
;
_refine_ls_abs_structure_Flack   0.48(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     342
_refine_ls_number_reflns         24006
_refine_ls_number_restraints     192
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.1627
_refine_ls_R_factor_gt           0.1195
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0359P)^2^+111.3578P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2370
_refine_ls_wR_factor_ref         0.2601
_reflns_Friedel_coverage         0.957
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                16071
_reflns_number_total             24006
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00304_si_002.cif
_cod_data_source_block           2a
_cod_database_code               4088687
_shelx_estimated_absorpt_t_min   0.830
_shelx_estimated_absorpt_t_max   0.924
_shelxl_version_number           2013-4
_shelx_res_checksum              55571