Synthesis of a Sulfur-bridged Diphosphine Ligand and Its Unique Complexation Properties toward Palladium(II) Ion
Morohashi, Naoya; Akahira, Yuki; Tanaka, Shinya; Nishiyama, Kensuke; Kajiwara, Takashi; Hattori, Tetsutaro; Chemistry Letters 37 (2008) 418–; doi:10.1246/cl.2008.418

data_8000186
_publ_section_title
;
 Synthesis of a Sulfur-bridged Diphosphine Ligand and Its Unique
 Complexation Properties toward Palladium(II) Ion
;
_journal_issue                   4
_journal_name_full               'Chemistry Letters'
_journal_page_first              418
_journal_paper_doi               10.1246/cl.2008.418
_journal_volume                  37
_journal_year                    2008
_chemical_formula_sum            'C45 H44 Cl F3 O3 P2 Pd S2'
_chemical_formula_weight         957.71
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                74.498(3)
_cell_angle_beta                 83.536(3)
_cell_angle_gamma                71.315(3)
_cell_formula_units_Z            2
_cell_length_a                   9.716(2)
_cell_length_b                   14.243(3)
_cell_length_c                   17.332(4)
_cell_measurement_temperature    296(2)
_cell_volume                     2188.5(8)
_computing_cell_refinement       'Bruker APEXII'
_computing_data_collection       'Bruker APEXII'
_computing_data_reduction        'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.909
_diffrn_measured_fraction_theta_max 0.909
_diffrn_measurement_device_type  'CCD are 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  0.0631
_diffrn_reflns_av_sigmaI/netI    0.0935
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            21411
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.56
_exptl_absorpt_coefficient_mu    0.705
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.453
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             980
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.749
_refine_diff_density_min         -1.254
_refine_diff_density_rms         0.136
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.336
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     551
_refine_ls_number_reflns         9133
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.336
_refine_ls_R_factor_all          0.1409
_refine_ls_R_factor_gt           0.0928
_refine_ls_shift/su_max          0.489
_refine_ls_shift/su_mean         0.010
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+33.6686P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2639
_refine_ls_wR_factor_ref         0.2799
_reflns_number_gt                6325
_reflns_number_total             9133
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            37-418sup1.cif
_cod_data_source_block           complex9
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_cell_volume        2188.5(9)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               8000186