Palladium Phosphinothiolato Complexes. Syntheses and Crystal Structures of Mononuclear [PdCl(SC2H4PPh2)PPh3] and Binuclear [Pd2Cl2(μ-SC3H6PPh2)2] and Their Performance in Catalytic Carbonylation
Nuria Brugat; Alfonso Polo; Ángel Álvarez-Larena; J. Francesc Piniella; Julio Real; Inorganic Chemistry 38 (1999) 4829–4837; doi:10.1021/ic981224+

data_4327663
_publ_contact_author
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Julio Real 
Departament de Qu\'imica 
Universitat Aut\'onoma de Barcelona 
08193 Bellaterra 
Spain 
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_publ_contact_author_email       real@cc.uab.es
_publ_contact_author_fax         '34 93 5813101'
_publ_contact_author_phone       '34 93 5812894'
_publ_section_title
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 Palladium Phosphinothiolato Complexes. Syntheses and Crystal Structures
 of Mononuclear [PdCl(SC2H4PPh2)PPh3] and Binuclear
 [Pd2Cl2(\m-SC3H6PPh2)2] and Their Performance in Catalytic Carbonylation
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_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4829
_journal_page_last               4837
_journal_paper_doi               10.1021/ic981224+
_journal_volume                  38
_journal_year                    1999
_chemical_formula_moiety         '[Pd Cl ((C6 H5)2 C3 H6 P S)]2 (C H2 Cl2)'
_chemical_formula_sum            'C31 H34 Cl4 P2 Pd2 S2'
_chemical_formula_weight         887.24
_chemical_name_systematic
; 
Dichlorobis{\m-[3-(diphenylphosphino)propanethiolato]-P,\m-S}-dipalladium(II) 
;
_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                 97.36(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.701(3)
_cell_length_b                   12.040(4)
_cell_length_c                   22.495(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12.43
_cell_measurement_theta_min      11.37
_cell_volume                     3411.6(14)
_computing_cell_refinement       'CAD4 (Enraf-Nonius)'
_computing_data_collection       'CAD4 (Enraf-Nonius)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.950
_diffrn_measured_fraction_theta_max 0.950
_diffrn_measurement_device_type  'Enraf-Nonius CAD4'
_diffrn_measurement_method       'omega/2theta scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0140
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5995
_diffrn_reflns_theta_full        24.97
_diffrn_reflns_theta_max         24.97
_diffrn_reflns_theta_min         1.75
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.606
_exptl_absorpt_correction_T_max  0.999
_exptl_absorpt_correction_T_min  0.923
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.727
_exptl_crystal_description       prism
_exptl_crystal_F_000             1768
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.29
_refine_diff_density_max         0.691
_refine_diff_density_min         -0.578
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     331
_refine_ls_number_reflns         5995
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.0329
_refine_ls_R_factor_gt           0.0274
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0318P)^2^+5.0267P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0729
_refine_ls_wR_factor_ref         0.0743
_reflns_number_gt                5297
_reflns_number_total             5995
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic9812242B_2.cif
_cod_data_source_block           compound6
_cod_depositor_comments
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The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0318P)^2^+5.0267P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0318P)^2^+5.0267P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
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_cod_database_code               4327663