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_4086029
_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 H32 Cl N5 Pd'
_chemical_formula_sum            'C28 H32 Cl N5 Pd'
_chemical_formula_weight         580.43
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 93.648(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   25.9380(12)
_cell_length_b                   14.6570(6)
_cell_length_c                   13.8367(6)
_cell_measurement_reflns_used    9234
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      30.55
_cell_measurement_theta_min      2.36
_cell_volume                     5249.7(4)
_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 1.000
_diffrn_measured_fraction_theta_max 0.997
_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  0.0515
_diffrn_reflns_av_unetI/netI     0.0299
_diffrn_reflns_laue_measured_fraction_full 1.000
_diffrn_reflns_laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            151861
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.575
_diffrn_reflns_theta_min         1.573
_diffrn_source                   microsource
_exptl_absorpt_coefficient_mu    0.835
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.9237
_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    1.469
_exptl_crystal_description       block
_exptl_crystal_F_000             2384
_exptl_crystal_size_max          0.155
_exptl_crystal_size_mid          0.132
_exptl_crystal_size_min          0.125
_refine_diff_density_max         0.464
_refine_diff_density_min         -0.539
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     680
_refine_ls_number_reflns         16048
_refine_ls_number_restraints     66
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0499
_refine_ls_R_factor_gt           0.0303
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0253P)^2^+4.0252P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0638
_refine_ls_wR_factor_ref         0.0717
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12181
_reflns_number_total             16048
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om500836m_si_001.cif
_cod_data_source_block           Compound4b
_cod_database_code               4086029
_shelx_estimated_absorpt_t_min   0.882
_shelx_estimated_absorpt_t_max   0.903
_shelxl_version_number           2014-1
_shelx_res_checksum              36358
_shelx_hkl_checksum              38062