Generation of Mono- and Bimetallic Palladium Complexes and Mechanistic Insight into an Operative Metal Ring-Walking Process
Orbach, Meital; Shankar, Sreejith; Zenkina, Olena V.; Milko, Petr; Diskin-Posner, Yael; van der Boom, Milko E.; Organometallics 34 (2015) 1098–; doi:10.1021/acs.organomet.5b00051

data_4087388
_publ_section_title
;
 Generation of Mono- and Bimetallic Palladium Complexes and Mechanistic
 Insight into an Operative Metal Ring-Walking Process
;
_journal_issue                   6
_journal_name_full               Organometallics
_journal_page_first              1098
_journal_paper_doi               10.1021/acs.organomet.5b00051
_journal_volume                  34
_journal_year                    2015
_chemical_formula_moiety         'C44 H72 F4 N2 P4 Pd2, C7 H8'
_chemical_formula_sum            'C51 H80 F4 N2 P4 Pd2'
_chemical_formula_weight         1133.85
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                79.223(2)
_cell_angle_beta                 77.307(2)
_cell_angle_gamma                75.198(2)
_cell_formula_units_Z            1
_cell_length_a                   9.0332(3)
_cell_length_b                   11.0003(4)
_cell_length_c                   14.6167(5)
_cell_measurement_reflns_used    28541
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.17
_cell_measurement_theta_min      1.93
_cell_volume                     1356.67(8)
_computing_cell_refinement       'Bruker Apex2'
_computing_data_collection       'Bruker Apex2'
_computing_data_reduction        'Bruker Apex2'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Bruker KappaApexII CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0351
_diffrn_reflns_av_sigmaI/netI    0.0373
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            28541
_diffrn_reflns_theta_full        30.17
_diffrn_reflns_theta_max         30.17
_diffrn_reflns_theta_min         1.93
_exptl_absorpt_coefficient_mu    0.829
_exptl_absorpt_correction_T_max  0.9520
_exptl_absorpt_correction_T_min  0.9071
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.388
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             588
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.916
_refine_diff_density_min         -0.721
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     298
_refine_ls_number_reflns         7913
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0356
_refine_ls_R_factor_gt           0.0283
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0328P)^2^+0.4884P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0646
_refine_ls_wR_factor_ref         0.0683
_reflns_number_gt                6946
_reflns_number_total             7913
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om5b00051_si_001.cif
_cod_data_source_block           complex6
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4087388