Apara-Hydrogen Investigation of Palladium-Catalyzed Alkyne Hydrogenation
Joaquín López-Serrano; Simon B. Duckett; Stuart Aiken; Karina Q. Almeida Leñero; Eite Drent; John P. Dunne; Denis Konya; Adrian C. Whitwood; Journal of the American Chemical Society 129 (2007) 6513–6527; doi:10.1021/ja070331c

data_4109422
_publ_contact_author_address
;Department of Chemistry
University of York
Heslington
York
YO10 5DD
United Kingdom
;
_publ_contact_author_email       sbd3@york.ac.uk
_publ_contact_author_fax         '44 904 432516'
_publ_contact_author_name        'Prof Simon Duckett'
_publ_contact_author_phone       '44 904 432564'
_publ_section_title
;
 Apara-Hydrogen Investigation of Palladium-Catalyzed Alkyne Hydrogenation
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6513
_journal_page_last               6527
_journal_paper_doi               10.1021/ja070331c
_journal_volume                  129
_journal_year                    2007
_chemical_formula_moiety         'C20 H40 O2 P2 Pd, 2(C F3 O3 S), 2(C H4 O)'
_chemical_formula_sum            'C24 H48 F6 O10 P2 Pd S2'
_chemical_formula_weight         843.08
_space_group_IT_number           18
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2 2ab'
_symmetry_space_group_name_H-M   'P 21 21 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.1425(6)
_cell_length_b                   12.0361(8)
_cell_length_c                   14.1564(9)
_cell_measurement_reflns_used    9575
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      29.96
_cell_measurement_theta_min      2.47
_cell_volume                     1728.16(19)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'CCD area detector'
_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  0.0247
_diffrn_reflns_av_sigmaI/netI    0.0267
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            19608
_diffrn_reflns_theta_full        30.03
_diffrn_reflns_theta_max         30.03
_diffrn_reflns_theta_min         2.22
_exptl_absorpt_coefficient_mu    0.831
_exptl_absorpt_correction_T_max  0.913
_exptl_absorpt_correction_T_min  0.845
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v2.03; (Sheldrick)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.620
_exptl_crystal_description       plate
_exptl_crystal_F_000             868
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.679
_refine_diff_density_min         -0.466
_refine_diff_density_rms         0.073
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.02(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     214
_refine_ls_number_reflns         4996
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0288
_refine_ls_R_factor_gt           0.0272
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0387P)^2^+0.3968P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0651
_refine_ls_wR_factor_ref         0.0658
_reflns_number_gt                4811
_reflns_number_total             4996
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja070331csi20070322_084400_1.cif
_cod_data_source_block           sbd0601a
_cod_database_code               4109422