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_4120988
_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         'C38 H46 P2 Pd2 S, 2(B F4), C H3 N O2'
_chemical_formula_sum            'C39 H49 B2 F8 N O2 P2 Pd2 S'
_chemical_formula_weight         1044.21
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2012-12-24
_audit_creation_method
;
  Olex2 1.2
  (compiled 2012.05.09 svn.r2324, GUI svn.r4230)
;
_cell_angle_alpha                90
_cell_angle_beta                 94.887(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.9974(4)
_cell_length_b                   14.9331(6)
_cell_length_c                   28.0415(11)
_cell_measurement_reflns_used    9670
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.56
_cell_measurement_theta_min      2.46
_cell_volume                     4171.2(3)
_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 0.999
_diffrn_measured_fraction_theta_max 0.997
_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  0.0401
_diffrn_reflns_av_unetI/netI     0.0157
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            124213
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.570
_diffrn_reflns_theta_min         1.996
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.061
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6260
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
sadabs was used for absorption correction.
wR2(int) was 0.0563 before and 0.0510 after correction.
The Ratio of minimum to maximum transmission is 0.8396.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.663
_exptl_crystal_description       prism
_exptl_crystal_F_000             2104
_exptl_crystal_recrystallization_method
'Grown from vapor diffusion of ether into nitromethane solution'
_exptl_crystal_size_max          0.420
_exptl_crystal_size_mid          0.111
_exptl_crystal_size_min          0.097
_refine_diff_density_max         0.924
_refine_diff_density_min         -0.604
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.111
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     626
_refine_ls_number_reflns         9622
_refine_ls_number_restraints     23
_refine_ls_restrained_S_all      1.116
_refine_ls_R_factor_all          0.0243
_refine_ls_R_factor_gt           0.0214
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0149P)^2^+4.3391P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0479
_refine_ls_wR_factor_ref         0.0489
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8911
_reflns_number_total             9622
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja406696k_15.cif
_cod_data_source_block           sbl50_sadabs
_cod_database_code               4120988
_shelxl_version_number           2012-6