#------------------------------------------------------------------------------
#$Date: 2016-03-25 16:35:29 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179978 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/72/7027211.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided the Crystal Eye server at
# http://wwmm.ch.cam.ac.uk/crystaleye/, created by Nick Day at the
# Peter Murray-Rust laboratory.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_7027211
loop_
_publ_author_name
'Koch, Klaus R.'
'Wang, Yali'
'Coetzee, Anita'
_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 ′-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]
;
_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       'ω - 2θ'
_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/[σ²(Fo²)+(0.0425P)²+0.3740P] where P=(Fo²+2Fc²)/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
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
Pd Pd 0.0000 0.0000 0.0000 0.03944(16) Uani 1 d S
Br Br 0.05827(6) 0.24090(5) 0.21385(5) 0.05501(18) Uani 1 d .
S S 0.13936(14) 0.17199(14) -0.08422(12) 0.0577(3) Uani 1 d .
N1 N -0.1267(4) 0.0410(4) -0.3727(4) 0.0423(8) Uani 1 d .
H1 H -0.145(5) -0.029(5) -0.339(4) 0.035(11) Uiso 1 d .
N2 N 0.0793(4) 0.2694(4) -0.3236(4) 0.0441(8) Uani 1 d .
H2 H 0.015(5) 0.255(5) -0.419(5) 0.048(12) Uiso 1 d .
C1 C 0.0247(5) 0.1608(4) -0.2712(4) 0.0403(9) Uani 1 d .
C11 C -0.2376(5) 0.0284(4) -0.5225(4) 0.0400(9) Uani 1 d .
C12 C -0.4019(5) -0.1052(4) -0.6068(4) 0.0397(9) Uani 1 d .
C13 C -0.4533(5) -0.2132(5) -0.5422(5) 0.0486(10) Uani 1 d .
H131 H -0.3833 -0.2049 -0.4399 0.069(6) Uiso 1 calc R
C14 C -0.6083(6) -0.3331(5) -0.6298(5) 0.0583(11) Uani 1 d .
H141 H -0.6414 -0.4065 -0.5869 0.069(6) Uiso 1 calc R
C15 C -0.7134(5) -0.3441(6) -0.7797(5) 0.0599(12) Uani 1 d .
H151 H -0.8176 -0.4250 -0.8384 0.069(6) Uiso 1 calc R
C16 C -0.6648(6) -0.2359(6) -0.8429(5) 0.0585(12) Uani 1 d .
H161 H -0.7375 -0.2427 -0.9439 0.069(6) Uiso 1 calc R
C17 C -0.5089(5) -0.1167(5) -0.7582(5) 0.0519(10) Uani 1 d .
H171 H -0.4761 -0.0447 -0.8025 0.069(6) Uiso 1 calc R
O11 O -0.2026(4) 0.1237(4) -0.5831(3) 0.0582(8) Uani 1 d .
C21 C 0.2327(5) 0.4070(5) -0.2272(5) 0.0480(10) Uani 1 d .
H211 H 0.3347 0.3696 -0.1933 0.068(7) Uiso 1 calc R
H212 H 0.2246 0.4656 -0.1349 0.068(7) Uiso 1 calc R
C22 C 0.2496(5) 0.5168(5) -0.3172(5) 0.0492(10) Uani 1 d .
H221 H 0.1512 0.5598 -0.3448 0.068(7) Uiso 1 calc R
H222 H 0.2491 0.4560 -0.4133 0.068(7) Uiso 1 calc R
C23 C 0.4150(6) 0.6544(5) -0.2229(6) 0.0629(12) Uani 1 d .
H231 H 0.4231 0.7210 -0.2842 0.097(10) Uiso 1 calc R
H232 H 0.5126 0.6121 -0.1953 0.097(10) Uiso 1 calc R
H233 H 0.4139 0.7171 -0.1295 0.097(10) Uiso 1 calc R
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -1.1770 1.0070 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
S Pd S 180.0 2 .
S Pd Br 94.54(3) 2 .
S Pd Br 85.46(3) . .
S Pd Br 85.46(3) 2 2
S Pd Br 94.54(3) . 2
Br Pd Br 180.0 . 2
C1 S Pd 114.83(13) . .
C1 N1 C11 126.9(3) . .
C1 N2 C21 123.9(3) . .
N2 C1 N1 118.0(3) . .
N2 C1 S 119.8(3) . .
N1 C1 S 122.2(3) . .
O11 C11 N1 121.0(3) . .
O11 C11 C12 121.4(3) . .
N1 C11 C12 117.6(3) . .
C17 C12 C13 119.5(4) . .
C17 C12 C11 116.2(4) . .
C13 C12 C11 124.3(3) . .
C14 C13 C12 120.1(4) . .
C15 C14 C13 120.2(4) . .
C16 C15 C14 119.9(4) . .
C15 C16 C17 120.8(4) . .
C16 C17 C12 119.5(4) . .
N2 C21 C22 110.7(3) . .
C21 C22 C23 111.5(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pd S 2.3164(10) 2
Pd S 2.3164(10) .
Pd Br 2.4415(5) .
Pd Br 2.4415(5) 2
S C1 1.689(4) .
N1 C1 1.378(5) .
N1 C11 1.379(5) .
N2 C1 1.315(5) .
N2 C21 1.460(5) .
C11 O11 1.220(5) .
C11 C12 1.492(5) .
C12 C17 1.386(5) .
C12 C13 1.388(6) .
C13 C14 1.382(6) .
C14 C15 1.371(6) .
C15 C16 1.370(7) .
C16 C17 1.383(6) .
C21 C22 1.502(6) .
C22 C23 1.517(6) .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
S Pd S C1 0.00(5) 2
Br Pd S C1 -125.94(15) .
Br Pd S C1 54.06(15) 2
C21 N2 C1 N1 177.0(3) .
C21 N2 C1 S -2.7(5) .
C11 N1 C1 N2 -5.7(6) .
C11 N1 C1 S 174.0(3) .
Pd S C1 N2 169.4(3) .
Pd S C1 N1 -10.2(4) .
C1 N1 C11 O11 4.4(6) .
C1 N1 C11 C12 -175.2(3) .
O11 C11 C12 C17 1.7(5) .
N1 C11 C12 C17 -178.7(3) .
O11 C11 C12 C13 -176.9(4) .
N1 C11 C12 C13 2.7(5) .
C17 C12 C13 C14 1.4(6) .
C11 C12 C13 C14 179.9(4) .
C12 C13 C14 C15 -1.2(7) .
C13 C14 C15 C16 -0.1(7) .
C14 C15 C16 C17 1.2(7) .
C15 C16 C17 C12 -1.0(6) .
C13 C12 C17 C16 -0.3(6) .
C11 C12 C17 C16 -179.0(4) .
C1 N2 C21 C22 -174.3(4) .
N2 C21 C22 C23 -176.0(3) .
