#------------------------------------------------------------------------------
#$Date: 2011-09-10 04:16:28 +0100 (Sat, 10 Sep 2011) $
#$Revision: 25271 $
#$URL: svn://www.crystallography.net/cod/cif/2/2007085.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# 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_2007085
loop_
_publ_author_name
'Blake, A. J.'
'Gilby, L. M.'
'Gould, R. O.'
'Lippolis, V.'
'Parsons, S.'
'Schr\"oder, M.'
_publ_section_title
;
 Macrocyclic Thioether Complexes of Palladium with Dibromoiodide Anions
;
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              295
_journal_page_last               298
_journal_volume                  54
_journal_year                    1998
_chemical_formula_iupac          '[Pd (C6 H12 S3)2] (I Br2)2'
_chemical_formula_moiety         'C12 H24 Pd S6 2+, 2I Br2 -'
_chemical_formula_sum            'C12 H24 Br4 I2 Pd S6'
_chemical_formula_weight         1040.51
_chemical_name_systematic
;
 ?
;
_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'
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 109.69(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.253(8)
_cell_length_b                   12.88(2)
_cell_length_c                   12.455(10)
_cell_measurement_reflns_used    36
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      16.0
_cell_measurement_theta_min      15.5
_cell_volume                     1398(3)
_computing_cell_refinement       DIF4
_computing_data_collection       'DIF4 (Stoe & Cie, 1992a)'
_computing_data_reduction        'REDU4 (Stoe & Cie, 1992b)'
_computing_molecular_graphics    'SHELXTL/PC (Sheldrick, 1995)'
_computing_publication_material  'SHELXL97 (Sheldrick, 1993)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Stoe Stadi-4 four-circle'
_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     0.71073
_diffrn_reflns_av_R_equivalents  0.0191
_diffrn_reflns_av_sigmaI/netI    0.0364
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2478
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.82
_diffrn_standards_decay_%        'variation +-2'
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    9.039
_exptl_absorpt_correction_T_max  0.062
_exptl_absorpt_correction_T_min  0.010
_exptl_absorpt_correction_type
;
\y scans (North, Phillips & Mathews, 1968), and then
refdelf (Walker & Stuart, 1983)
;
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    2.473
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             968
_exptl_crystal_size_max          0.58
_exptl_crystal_size_mid          0.44
_exptl_crystal_size_min          0.28
_refine_diff_density_max         '3.46 (0.30\%A from Br2)'
_refine_diff_density_min         '-3.56 (0.89\%A from I1)'
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    'riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     116
_refine_ls_number_reflns         2435
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.1236
_refine_ls_R_factor_gt           0.0935
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme
'calc w = 1/[\s^2^(Fo^2^)+(0.192P)^2^+20.95P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_wR_factor_ref         0.2882
_reflns_number_gt                1740
_reflns_number_total             2435
_reflns_threshold_expression     I>2\s(I)
_[local]_cod_data_source_file    ha1202.cif
_[local]_cod_data_source_block   1
_[local]_cod_cif_authors_sg_H-M  'P 21/n'
_cod_database_code               2007085
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x+1/2, -y+1/2, z+1/2'
'-x, -y, -z'
'-x-1/2, y-1/2, -z-1/2'
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_type_symbol
Pd -0.5000 1.0000 0.0000 0.0380(6) Uani d S 1 Pd
S1 -0.6845(6) 0.8360(4) -0.1544(4) 0.0488(13) Uani d . 1 S
C2 -0.822(2) 0.9362(16) -0.2246(18) 0.046(5) Uani d . 1 C
H2A -0.8954 0.9059 -0.2926 0.055 Uiso calc R 1 H
H2B -0.8789 0.9543 -0.1742 0.055 Uiso calc R 1 H
C3 -0.763(2) 1.0372(18) -0.2598(17) 0.052(6) Uani d . 1 C
H3A -0.8508 1.0795 -0.3021 0.063 Uiso calc R 1 H
H3B -0.7072 1.0204 -0.3107 0.063 Uiso calc R 1 H
S4 -0.6387(6) 1.1139(4) -0.1405(4) 0.0438(12) Uani d . 1 S
C5 -0.487(2) 1.1545(14) -0.1948(16) 0.040(4) Uani d . 1 C
H5A -0.5317 1.1957 -0.2632 0.048 Uiso calc R 1 H
H5B -0.4145 1.1982 -0.1384 0.048 Uiso calc R 1 H
C6 -0.400(2) 1.0621(17) -0.2225(16) 0.047(5) Uani d . 1 C
H6A -0.3131 1.0875 -0.2411 0.056 Uiso calc R 1 H
H6B -0.4678 1.0255 -0.2885 0.056 Uiso calc R 1 H
S7 -0.3342(5) 0.9729(4) -0.1019(4) 0.0413(11) Uani d . 1 S
C8 -0.395(3) 0.8444(16) -0.1726(17) 0.050(5) Uani d . 1 C
H8A -0.3363 0.8327 -0.2232 0.059 Uiso calc R 1 H
H8B -0.3634 0.7915 -0.1138 0.059 Uiso calc R 1 H
C9 -0.556(3) 0.827(2) -0.238(2) 0.059(6) Uani d . 1 C
H9A -0.5664 0.7580 -0.2722 0.071 Uiso calc R 1 H
H9B -0.5880 0.8768 -0.2997 0.071 Uiso calc R 1 H
I1 0.18218(15) 0.61898(12) 0.03933(11) 0.0504(6) Uani d . 1 I
Br1 0.3212(2) 0.42217(17) 0.05488(18) 0.0491(6) Uani d . 1 Br
Br2 0.0353(2) 0.81623(16) 0.01655(17) 0.0434(6) Uani d . 1 Br
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Pd 0.0371(11) 0.0412(12) 0.0336(10) 0.0064(9) 0.0092(8) 0.0028(9)
S1 0.052(3) 0.047(3) 0.047(3) -0.009(2) 0.016(2) 0.001(2)
C2 0.031(10) 0.045(11) 0.055(12) -0.008(9) 0.005(8) 0.006(10)
C3 0.030(9) 0.074(15) 0.037(9) -0.003(10) -0.008(7) 0.019(10)
S4 0.042(3) 0.042(3) 0.043(2) 0.008(2) 0.008(2) 0.004(2)
C5 0.032(9) 0.035(10) 0.044(10) 0.007(8) 0.000(8) 0.006(9)
C6 0.038(10) 0.060(13) 0.039(10) 0.004(10) 0.010(8) 0.013(10)
S7 0.036(2) 0.045(3) 0.043(2) 0.000(2) 0.0130(19) 0.001(2)
C8 0.072(14) 0.036(10) 0.037(10) 0.015(10) 0.014(9) 0.007(9)
C9 0.057(13) 0.058(14) 0.053(12) -0.002(11) 0.007(10) 0.003(11)
I1 0.0477(9) 0.0606(10) 0.0420(8) -0.0136(6) 0.0142(6) 0.0006(6)
Br1 0.0412(11) 0.0457(12) 0.0529(12) -0.0016(9) 0.0061(9) 0.0074(9)
Br2 0.0333(10) 0.0460(11) 0.0535(11) -0.0054(8) 0.0179(8) 0.0072(9)
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'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9988 1.0072 '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'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
S4 Pd S4 . 3_475 180.0 ?
S4 Pd S7 . 3_475 91.05(19) ?
S4 Pd S7 3_475 3_475 88.95(19) ?
S1 Pd S4 . . 84.8(2) ?
S1 Pd S7 . . 83.2(2) ?
S4 Pd S7 . . 88.95(19) ?
S4 Pd S7 3_475 . 91.05(19) ?
S7 Pd S7 3_475 . 180.0 ?
C2 S1 C9 . . 105.0(11) ?
C3 C2 S1 . . 118.7(14) ?
C2 C3 S4 . . 114.5(14) ?
C5 S4 C3 . . 102.0(10) ?
C5 S4 Pd . . 99.3(6) ?
C3 S4 Pd . . 108.0(7) ?
C6 C5 S4 . . 112.6(13) ?
C5 C6 S7 . . 111.0(13) ?
C6 S7 C8 . . 101.9(10) ?
C6 S7 Pd . . 104.7(7) ?
C8 S7 Pd . . 104.0(8) ?
C9 C8 S7 . . 119.4(16) ?
C8 C9 S1 . . 114.2(17) ?
Br1 I1 Br2 . . 178.18(7) yes
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Pd S1 . 2.997(6) yes
Pd S4 . 2.313(5) yes
Pd S7 . 2.323(5) yes
Pd S4 3_475 2.313(5) ?
Pd S7 3_475 2.323(5) ?
S1 C2 . 1.82(2) ?
S1 C9 . 1.83(3) ?
C2 C3 . 1.53(3) ?
C3 S4 . 1.83(2) ?
S4 C5 . 1.83(2) ?
C5 C6 . 1.54(3) ?
C6 S7 . 1.825(19) ?
S7 C8 . 1.87(2) ?
C8 C9 . 1.46(3) ?
I1 Br1 . 2.819(4) yes
I1 Br2 . 2.850(4) yes
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
S1 C2 C3 S4 -64(2)
C2 C3 S4 C5 137.4(16)
C3 S4 C5 C6 -60.4(15)
S4 C5 C6 S7 -51.6(16)
C5 C6 S7 C8 132.9(15)
C6 S7 C8 C9 -57(2)
S7 C8 C9 S1 -61(2)
C8 C9 S1 C2 122.4(17)
C9 S1 C2 C3 -45.5(19)