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_4327662
_publ_contact_author
; 
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
;
 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_structural
;
[Pd Cl ((C6 H5)2 (C2 H4 P S)) ((C6 H5)3 P)] (C H2 Cl2)
;
_chemical_formula_sum            'C33 H31 Cl3 P2 Pd S'
_chemical_formula_weight         734.33
_chemical_name_systematic
; 
Chloro[2-(diphenylphosphino)ethanethiolato-P,S]-triphenylphospinepalladium(II) 
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.247(3)
_cell_length_b                   17.956(9)
_cell_length_c                   19.869(9)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      13.99
_cell_measurement_theta_min      11.62
_cell_volume                     3299(2)
_computing_cell_refinement       'CAD4 (Enraf-Nonius)'
_computing_data_collection       'CAD4 (Enraf-Nonius)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       '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  0.0149
_diffrn_reflns_av_sigmaI/netI    0.0841
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -4
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3263
_diffrn_reflns_theta_max         24.95
_diffrn_reflns_theta_min         1.53
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.988
_exptl_absorpt_correction_T_max  0.994
_exptl_absorpt_correction_T_min  0.865
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.478
_exptl_crystal_description       needle
_exptl_crystal_F_000             1488
_exptl_crystal_size_max          0.58
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.563
_refine_diff_density_min         -0.478
_refine_diff_density_rms         0.076
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.04(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.934
_refine_ls_goodness_of_fit_obs   1.082
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     310
_refine_ls_number_reflns         3261
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      0.935
_refine_ls_restrained_S_obs      1.083
_refine_ls_R_factor_all          0.0701
_refine_ls_R_factor_obs          0.0435
_refine_ls_shift/esd_max         -0.004
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0616P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1023
_refine_ls_wR_factor_obs         0.0985
_reflns_number_observed          2342
_reflns_number_total             3261
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic9812242B_1.cif
_cod_data_source_block           compound3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0616P)^2^+0.0000P] 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^)+(0.0616P)^2^+0.0000P] 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_original_cell_volume        3299.0(25)
_cod_database_code               4327662