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_4109424
_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         'C23 H42 O2 P2 Pd, 2(C F3 O3 S), 2(H2 O)'
_chemical_formula_sum            'C25 H46 F6 O10 P2 Pd S2'
_chemical_formula_weight         853.08
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 108.403(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.8608(15)
_cell_length_b                   16.6018(16)
_cell_length_c                   14.8694(15)
_cell_measurement_reflns_used    5357
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.97
_cell_measurement_theta_min      2.45
_cell_volume                     3480.9(6)
_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      100(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_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  0.0222
_diffrn_reflns_av_sigmaI/netI    0.0304
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            27146
_diffrn_reflns_theta_full        30.04
_diffrn_reflns_theta_max         30.04
_diffrn_reflns_theta_min         1.69
_exptl_absorpt_coefficient_mu    0.827
_exptl_absorpt_correction_T_max  0.850
_exptl_absorpt_correction_T_min  0.824
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v2.03; (Sheldrick)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.628
_exptl_crystal_description       block
_exptl_crystal_F_000             1752
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.607
_refine_diff_density_min         -0.419
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     453
_refine_ls_number_reflns         10013
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0351
_refine_ls_R_factor_gt           0.0260
_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^)+(0.0327P)^2^+0.8546P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0614
_refine_ls_wR_factor_ref         0.0646
_reflns_number_gt                8479
_reflns_number_total             10013
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja070331csi20070322_084400_3.cif
_cod_data_source_block           sbd0503a
_cod_database_code               4109424