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_4088689
_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_absolute_configuration ad
_chemical_formula_moiety         'C34 H50 B N P2 Pd'
_chemical_formula_sum            'C34 H50 B N P2 Pd'
_chemical_formula_weight         651.90
_chemical_name_common            jonlm38
_chemical_name_systematic        (dippe)Pd(Me)(CNBPh3)
_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-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   16.9464(15)
_cell_length_b                   13.0266(11)
_cell_length_c                   30.638(3)
_cell_measurement_reflns_used    3944
_cell_measurement_temperature    100.0(5)
_cell_measurement_theta_max      30.28
_cell_measurement_theta_min      2.38
_cell_volume                     6763.5(11)
_computing_cell_refinement       'SAINT (Bruker, 2013)'
_computing_data_collection       'APEX3 (Bruker, 2015)'
_computing_data_reduction        'SAINT (Bruker, 2013)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2015b)'
_computing_structure_solution    'SHELXT-2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.0(5)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.996
_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  0.0895
_diffrn_reflns_av_unetI/netI     0.0676
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            112743
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        31.506
_diffrn_reflns_theta_max         31.517
_diffrn_reflns_theta_min         1.699
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.666
_exptl_absorpt_correction_T_max  0.7462
_exptl_absorpt_correction_T_min  0.6670
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2015a)'
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.280
_exptl_crystal_description       needle
_exptl_crystal_F_000             2736
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.930
_refine_diff_density_min         -0.976
_refine_diff_density_rms         0.099
_refine_ls_abs_structure_details
; 
 Refined as an inversion twin. 
;
_refine_ls_abs_structure_Flack   0.31(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     722
_refine_ls_number_reflns         22422
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0848
_refine_ls_R_factor_gt           0.0523
_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^)+(0.0333P)^2^+5.9144P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0940
_refine_ls_wR_factor_ref         0.1055
_reflns_Friedel_coverage         0.968
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                16524
_reflns_number_total             22422
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00304_si_002.cif
_cod_data_source_block           3a'
_cod_original_cell_volume        6763.5(10)
_cod_database_code               4088689
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.767
_shelx_estimated_absorpt_t_max   0.901
_shelx_res_checksum              66644