Macrocyclic Thioether Complexes of Palladium with Dibromoiodide Anions
Blake, Alexander J.; Gilby, Liam M.; Gould, Robert O.; Lippolis, Vito; Parsons, Simon; Schröder, Martin; Acta Crystallographica Section C 54 (1998) 295–298; doi:10.1107/S0108270197014212

data_2007086
_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_paper_doi               10.1107/S0108270197014212
_journal_volume                  54
_journal_year                    1998
_chemical_formula_iupac          '[Pd (C10 H20 S4)] [I Br2]2'
_chemical_formula_moiety         'C10 H20 Pd S4 2+, 2I Br2 -'
_chemical_formula_sum            'C10 H20 Br4 I2 Pd S4'
_chemical_formula_weight         948.34
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-I 2ya'
_symmetry_space_group_name_H-M   'I 1 2/a 1'
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 93.468(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.651(2)
_cell_length_b                   9.3117(7)
_cell_length_c                   16.7648(11)
_cell_measurement_reflns_used    48
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      14
_cell_measurement_theta_min      13
_cell_volume                     2283.0(4)
_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  'SHELXL93 (Sheldrick, 1993)'
_computing_structure_refinement  'SHELXL93 (Sheldrick, 1993)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Stoe Stadi-4 four-circle'
_diffrn_measurement_method       \w/\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  0.0190
_diffrn_reflns_av_sigmaI/netI    0.0338
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            2523
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.50
_diffrn_standards_decay_%        none
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    10.877
_exptl_absorpt_correction_T_max  0.694
_exptl_absorpt_correction_T_min  0.176
_exptl_absorpt_correction_type   '\y scans (North, Phillips & Matthews, 1968)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.759
_exptl_crystal_density_meas      ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1744
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.04
_refine_diff_density_max         '1.12 (0.89\%A from Br2)'
_refine_diff_density_min         '-1.07 (0.84\%A from Br2)'
_refine_ls_extinction_coef       0.00123(10)
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.055
_refine_ls_goodness_of_fit_obs   1.053
_refine_ls_hydrogen_treatment    'constr with U~iso~(H) = 1.2U~eq~(C)'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     98
_refine_ls_number_reflns         1878
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.164
_refine_ls_restrained_S_obs      1.053
_refine_ls_R_factor_all          0.0523
_refine_ls_R_factor_obs          .0392
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.041P)^2^+29.01P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1102
_refine_ls_wR_factor_obs         .0903
_reflns_number_observed          1564
_reflns_number_total             1894
_reflns_observed_criterion       I>2\s(I)
_cod_data_source_file            ha1202.cif
_cod_data_source_block           2
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_geom_bond_publ_flag' value 'Yes' changed to 'yes' according
to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (6 times).

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w =
1/[\s^2^(Fo^2^)+(0.041P)^2^+29.01P] 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^)+(0.041P)^2^+29.01P] 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        2282.9(4)
_cod_original_sg_symbol_H-M      'I 2/a'
_cod_database_code               2007086