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_4086030
_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         'C64 H80 K2 N10 O2 Pd2, 4(C4 H8 O)'
_chemical_formula_sum            'C80 H112 K2 N10 O6 Pd2'
_chemical_formula_weight         1600.79
_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                 99.2200(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.6602(2)
_cell_length_b                   16.1278(3)
_cell_length_c                   25.0995(5)
_cell_measurement_reflns_used    9504
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      27.56
_cell_measurement_theta_min      2.31
_cell_volume                     4259.49(14)
_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-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      170(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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_unetI/netI     0.0250
_diffrn_reflns_laue_measured_fraction_full 1.000
_diffrn_reflns_laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            95135
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.282
_diffrn_reflns_theta_min         1.507
_diffrn_source                   microsource
_exptl_absorpt_coefficient_mu    0.573
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.9292
_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            brown
_exptl_crystal_density_diffrn    1.248
_exptl_crystal_description       plate
_exptl_crystal_F_000             1680
_exptl_crystal_size_max          0.347
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.194
_platon_squeeze_details
;
the eliminated contribution is consistent with a thf solvent molecule
;
_refine_diff_density_max         0.627
_refine_diff_density_min         -0.731
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     532
_refine_ls_number_reflns         10583
_refine_ls_number_restraints     665
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0447
_refine_ls_R_factor_gt           0.0359
_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^)+(0.0518P)^2^+2.6691P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0952
_refine_ls_wR_factor_ref         0.0990
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8986
_reflns_number_total             10583
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om500836m_si_001.cif
_cod_data_source_block           Compound6
_cod_original_cell_volume        4259.50(14)
_cod_database_code               4086030
_shelx_estimated_absorpt_t_min   0.826
_shelx_estimated_absorpt_t_max   0.897
_shelxl_version_number           2014-1
_shelx_res_checksum              6465
_shelx_hkl_checksum              44845