Dipalladium(I) Terphenyl Diphosphine Complexes as Models for Two-Site Adsorption and Activation of Organic Molecules
Sibo Lin; David E. Herbert; Alexandra Velian; Michael W. Day; Theodor Agapie; Journal of the American Chemical Society 135 (2013) 15830–15840; doi:10.1021/ja406696k

data_4120984
_publ_contact_author_name
;
;
_publ_section_title
;
 Dipalladium(I) Terphenyl Diphosphine Complexes as Models for Two-Site
 Adsorption and Activation of Organic Molecules
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              15830
_journal_page_last               15840
_journal_paper_doi               10.1021/ja406696k
_journal_volume                  135
_journal_year                    2013
_chemical_formula_moiety         'C34 H44 P2 Pd2 S, 2(B F4)'
_chemical_formula_sum            'C34 H44 B2 F8 P2 Pd2 S'
_chemical_formula_weight         933.11
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2012-12-17
_audit_creation_method
;
  Olex2 1.2
  (compiled 2012.05.09 svn.r2324, GUI svn.r4230)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   19.2900(11)
_cell_length_b                   16.1824(9)
_cell_length_c                   23.3891(13)
_cell_measurement_reflns_used    9525
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      48.90
_cell_measurement_theta_min      2.40
_cell_volume                     7301.1(7)
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
XS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0639
_diffrn_reflns_av_unetI/netI     0.0214
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       50
_diffrn_reflns_limit_l_min       -49
_diffrn_reflns_number            810600
_diffrn_reflns_theta_full        49.64
_diffrn_reflns_theta_max         49.64
_diffrn_reflns_theta_min         1.74
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.196
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8722
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
sadabs was used for absorption correction.
R(int) was 0.0637 before and 0.0588 after correction.
The Ratio of minimum to maximum transmission is 0.8722.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.698
_exptl_crystal_description       prism
_exptl_crystal_F_000             3744
_exptl_crystal_recrystallization_method
'Layering of Et2O on a MeNO2 solution of the compound'
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.507
_refine_diff_density_min         -1.140
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     618
_refine_ls_number_reflns         37544
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0418
_refine_ls_R_factor_gt           0.0269
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0300P)^2^+3.9926P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0624
_refine_ls_wR_factor_ref         0.0719
_reflns_number_gt                30541
_reflns_number_total             37544
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja406696k_07.cif
_cod_data_source_block           sbl49_sadabs
_cod_database_code               4120984