Evidence for the Formation of Anionic Zerovalent Group 10 Complexes as Highly Reactive Intermediates
Seyboldt, Alexander; Wucher, Barbara; Hohnstein, Silvia; Eichele, Klaus; Rominger, Frank; Törnroos, Karl W.; Kunz, Doris; Organometallics 34 (2015) 2717–; doi:10.1021/om500836m

data_4086027
_publ_section_title
;
 Evidence for the Formation of Anionic Zerovalent Group 10 Complexes as
 Highly Reactive Intermediates
;
_journal_issue                   12
_journal_name_full               Organometallics
_journal_page_first              2717
_journal_paper_doi               10.1021/om500836m
_journal_volume                  34
_journal_year                    2015
_chemical_formula_moiety         'C28 H33 N5 Pd'
_chemical_formula_sum            'C28 H33 N5 Pd'
_chemical_formula_weight         545.99
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           18
_space_group_name_Hall           'P 2 2ab'
_space_group_name_H-M_alt        'P 21 21 2'
_symmetry_space_group_name_Hall  'P 2 2ab'
_symmetry_space_group_name_H-M   'P 21 21 2'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.0589(2)
_cell_length_b                   11.5993(3)
_cell_length_c                   13.1546(3)
_cell_measurement_reflns_used    9946
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      27.65
_cell_measurement_theta_min      2.34
_cell_volume                     1534.83(6)
_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-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0267
_diffrn_reflns_av_unetI/netI     0.0277
_diffrn_reflns_laue_measured_fraction_full 0.999
_diffrn_reflns_laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            19681
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.835
_diffrn_reflns_theta_min         2.341
_diffrn_source                   microsource
_exptl_absorpt_coefficient_mu    0.626
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.9041
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1, G.M Sheldrick, University of 
G\"ttingen, Germany, 2008 
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.181
_exptl_crystal_description       prism
_exptl_crystal_F_000             564
_exptl_crystal_size_max          0.286
_exptl_crystal_size_mid          0.144
_exptl_crystal_size_min          0.081
_platon_squeeze_details
'the eliminated contribution is consistent with a pentane solvent molecule'
_refine_diff_density_max         0.270
_refine_diff_density_min         -0.253
_refine_diff_density_rms         0.050
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.25(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     162
_refine_ls_number_reflns         4022
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0274
_refine_ls_R_factor_gt           0.0248
_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^)+(0.0378P)^2^+0.0055P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0605
_refine_ls_wR_factor_ref         0.0617
_reflns_Friedel_coverage         0.755
_reflns_friedel_fraction_full    1.000
_reflns_friedel_fraction_max     0.998
_reflns_number_gt                3761
_reflns_number_total             4022
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om500836m_si_001.cif
_cod_data_source_block           Compound3b
_cod_database_code               4086027
_shelx_estimated_absorpt_t_min   0.841
_shelx_estimated_absorpt_t_max   0.951
_shelxl_version_number           2014-1
_shelx_res_checksum              82702
_shelx_hkl_checksum              76835