Chemoselective homogeneous hydrogenation of phenylacetylene using thiosemicarbazone and thiobenzoylhydrazone palladium(II) complexes as catalysts
Pelagatti, Paolo; Venturini, Andrea; Leporati, Andrea; Carcelli, Mauro; Costa, Mirco; Bacchi, Alessia; Pelizzi, Giancarlo; Pelizzi, Corrado; Journal of the Chemical Society, Dalton Transactions  (1998) 2715–; doi:10.1039/a804052d

data_7028011
_publ_section_title
;
 Chemoselective homogeneous hydrogenation of phenylacetylene using
 thiosemicarbazone and thiobenzoylhydrazone palladium(II) complexes as
 catalysts
;
_journal_issue                   16
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              2715
_journal_paper_doi               10.1039/a804052d
_journal_year                    1998
_chemical_formula_sum            'C13 H11 Cl N4 Pd S'
_chemical_formula_weight         397.17
_chemical_name_systematic
; 

 ? 

;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 108.35(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   12.089(4)
_cell_length_b                   21.801(7)
_cell_length_c                   11.480(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_volume                     2871.7(17)
_computing_molecular_graphics    'ZORTEP (Zsolnai & Pritzkow, H., 1994)'
_computing_publication_material  'PARST95 (Nardelli, 1995)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SIR92 (Altomare et al, 1992)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Siemens AED diffractometer'
_diffrn_measurement_method       '\q/2\q 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  0.0255
_diffrn_reflns_av_sigmaI/netI    0.0201
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4368
_diffrn_reflns_theta_max         29.98
_diffrn_reflns_theta_min         3.10
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 100
_diffrn_standards_number         1
_exptl_absorpt_coefficient_mu    1.617
_exptl_absorpt_correction_T_max  1.01
_exptl_absorpt_correction_T_min  0.94
_exptl_absorpt_correction_type   'Walker&Stuart (1983)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.837
_exptl_crystal_description       prisms
_exptl_crystal_F_000             1568
_refine_diff_density_max         1.129
_refine_diff_density_min         -1.151
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.117
_refine_ls_goodness_of_fit_obs   1.022
_refine_ls_hydrogen_treatment    iso
_refine_ls_matrix_type           full
_refine_ls_number_parameters     224
_refine_ls_number_reflns         4179
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.125
_refine_ls_restrained_S_obs      1.022
_refine_ls_R_factor_all          0.0568
_refine_ls_R_factor_obs          0.0365
_refine_ls_shift/esd_max         0.025
_refine_ls_shift/esd_mean        0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[s^2^(Fo^2^)+( 0.0322P)^2^+13.5503P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1055
_refine_ls_wR_factor_obs         0.0830
_reflns_number_observed          3188
_reflns_number_total             4184
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            d804052sup1.cif
_cod_data_source_block           1a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w=1/[s^2^(Fo^2^)+(
0.0322P)^2^+13.5503P] 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^)+( 0.0322P)^2^+13.5503P]
where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        2872(2)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7028011