Palladium-Catalyzed Dehydrogenative Cis Double Phosphorylation of Alkynes with H-Phosphonate Leading to (Z)-Bisphosphoryl-1-alkenes
Li-Biao Han; Yutaka Ono; Shigeru Shimada; Journal of the American Chemical Society 130 (2008) 2752–2753; doi:10.1021/ja7108272

data_4107489
_publ_contact_author_address
;
National Institute of Advanced Industrial Science and Technology,
Tukuba Central 5, Tsukuba, Ibaraki 305-8565, Japan
;
_publ_contact_author_email       libiao-han@aist.go.jp
_publ_contact_author_fax         +81-29-861-4511
_publ_contact_author_name        'Li-Biao Han'
_publ_contact_author_phone       +81-29-861-4855
_publ_section_title
;
 Palladium-Catalyzed Dehydrogenative Cis Double Phosphorylation of Alkynes
 with H-Phosphonate Leading to (Z)-Bisphosphoryl-1-alkenes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              2752
_journal_page_last               2753
_journal_paper_doi               10.1021/ja7108272
_journal_volume                  130
_journal_year                    2008
_chemical_formula_moiety         'C20 H37 F3 O9 P2 Pd '
_chemical_formula_sum            'C20 H37 F3 O9 P2 Pd'
_chemical_formula_weight         646.85
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_date             2007-12-16
_audit_creation_method           'by CrystalStructure 3.8'
_cell_angle_alpha                90.0000
_cell_angle_beta                 98.3410(10)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   12.5585(8)
_cell_length_b                   10.5717(7)
_cell_length_c                   21.1910(14)
_cell_measurement_reflns_used    5348
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      28.2
_cell_measurement_theta_min      2.5
_cell_volume                     2783.7(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        CrystalStructure
_computing_publication_material  'CrystalStructure 3.8'
_computing_structure_refinement  CRYSTALS
_computing_structure_solution    'DIRDIF99 (PATTY)'
_diffrn_ambient_temperature      153(2)
_diffrn_detector_area_resol_mean '8.366 [pixels/mm]'
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.918
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.030
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            16356
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         28.28
_exptl_absorpt_coefficient_mu    0.845
_exptl_absorpt_correction_T_max  0.9511
_exptl_absorpt_correction_T_min  0.8697
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
SADABS; Sheldrick 1996
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.543
_exptl_crystal_description       needle
_exptl_crystal_F_000             1328.00
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.10
_refine_diff_density_min         -0.58
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    mixed
_refine_ls_number_parameters     356
_refine_ls_number_reflns         6211
_refine_ls_R_factor_gt           0.0309
_refine_ls_shift/su_max          0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     'w = 1/[0.4500\s(Fo^2^) + 0.0650]/(4Fo^2^)'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0698
_reflns_number_gt                4885
_reflns_number_total             6212
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ja7108272-file003.cif
_cod_data_source_block           8
_cod_depositor_comments
;
The following automatic conversions were performed:

'_atom_sites_solution_hydrogens' value 'difmap & geom' was changed to
'mixed'.

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 
;
_cod_original_formula_sum        'C20 H37 F3 O9 P2 Pd '
_cod_database_code               4107489