Platinum(II) and palladium(II) complexes of N-benzoyl-N ′-propylthiourea (H2L): synthesis and geometric isomer distribution of [M(H2L-S )2X2] (M = PtII or PdII; X = Cl−, Br− or I−); crystal structure of trans-[Pd(H2L-S )2Br2]
Koch, Klaus R.; Wang, Yali; Coetzee, Anita; Journal of the Chemical Society, Dalton Transactions  (1999) 1013–; doi:10.1039/a809543d

data_7027211
_publ_contact_author
;  Prof K R Koch
   Department of Chemistry
   University of Cape Town
   Rondebosch 7701
   South Africa
;
_publ_section_title
;
 Platinum(II) and palladium(II) complexes of
 N-benzoyl-N&#x200A;&#x2032;-propylthiourea (H2L): synthesis and geometric
 isomer distribution of [M(H2L-S&#x200A;)2X2] (M&#x2005;=&#x2005;PtII or
 PdII; X&#x2005;=&#x2005;Cl&#x2212;, Br&#x2212; or I&#x2212;); crystal
 structure of trans-[Pd(H2L-S&#x200A;)2Br2]
;
_journal_issue                   6
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              1013
_journal_paper_doi               10.1039/a809543d
_journal_year                    1999
_chemical_formula_sum            'C22 H28 Br2 N4 O2 Pd S2'
_chemical_formula_weight         710.84
_chemical_name_systematic
trans-bis(N-benzoyl-N'-propylthioureato)dibromopalladium(II)
_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                104.034(8)
_cell_angle_beta                 113.016(8)
_cell_angle_gamma                99.226(9)
_cell_formula_units_Z            1
_cell_length_a                   8.7678(10)
_cell_length_b                   8.9525(9)
_cell_length_c                   9.8668(8)
_cell_measurement_reflns_used    'psi scan'
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      22.54
_cell_measurement_theta_min      2.38
_cell_volume                     662.72(13)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Enraf-Nonius CAD4'
_diffrn_measurement_method       '\w - 2\q'
_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  0.0137
_diffrn_reflns_av_sigmaI/netI    0.0223
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            1867
_diffrn_reflns_theta_full        22.54
_diffrn_reflns_theta_max         22.54
_diffrn_reflns_theta_min         2.38
_diffrn_standards_interval_time  3600
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    3.849
_exptl_absorpt_correction_T_max  0.9976
_exptl_absorpt_correction_T_min  0.7837
_exptl_absorpt_correction_type
'Lorenz-polarisation as well as empirical absorption corrections '
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.781
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             348
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.492
_refine_diff_density_min         -0.607
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     163
_refine_ls_number_reflns         1744
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.093
_refine_ls_R_factor_all          0.0306
_refine_ls_R_factor_gt           0.0254
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0425P)^2^+0.3740P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0724
_refine_ls_wR_factor_ref         0.0740
_reflns_number_gt                1542
_reflns_number_total             1744
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            809543dsup1.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0425P)^2^+0.3740P] 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^)+(0.0425P)^2^+0.3740P] 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        662.72(11)
_cod_database_code               7027211