Tetrakis(dimethyl sulfide)palladium(II) bis(tetrafluoroborate) and tetrakis(1,4-oxathiane-κ<i>S</i>)palladium(II) bis(tetrafluoroborate)
Johansson, Maria H.; Oskarsson, Åke; Acta Crystallographica Section C 58 (2002) m102–m104; doi:10.1107/S0108270101019357

data_2012538
_publ_section_title
;
 Tetrakis(dimethyl sulfide)palladium(II) bis(tetrafluoroborate) and
 tetrakis(1,4-oxathiane-\k<i>S</i>)palladium(II) bis(tetrafluoroborate)
;
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m102
_journal_page_last               m104
_journal_paper_doi               10.1107/S0108270101019357
_journal_volume                  58
_journal_year                    2002
_chemical_formula_iupac          '[Pd (C4 H8 O S)4] (B F4)2'
_chemical_formula_moiety         'C16 H32 O4 Pd S4 2+ , 2B F4 -'
_chemical_formula_sum            'C16 H32 B2 F8 O4 Pd S4'
_chemical_formula_weight         696.68
_chemical_name_systematic
;
tetrakis(1,4-oxathiane-S)palladium(II) bis(tetrafluoroborate)
;
_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           SHELXL97
_cell_angle_alpha                94.11(3)
_cell_angle_beta                 114.12(3)
_cell_angle_gamma                111.79(3)
_cell_formula_units_Z            1
_cell_length_a                   8.8804(18)
_cell_length_b                   9.5397(19)
_cell_length_c                   9.6999(19)
_cell_measurement_reflns_used    2469
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26
_cell_measurement_theta_min      4
_cell_volume                     671.8(4)
_computing_cell_refinement       'SAINT (Siemens, 1995)'
_computing_data_collection       'SMART (Siemens, 1995)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2000)'
_computing_publication_material  'SHELXTL (Sheldrick, 1997b)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997a)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997a)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 512
_diffrn_measured_fraction_theta_full .989
_diffrn_measured_fraction_theta_max .989
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     .71073
_diffrn_reflns_av_R_equivalents  .050
_diffrn_reflns_av_sigmaI/netI    .109
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            4856
_diffrn_reflns_theta_full        27.87
_diffrn_reflns_theta_max         27.87
_diffrn_reflns_theta_min         2.38
_diffrn_standards_decay_%        .00
_exptl_absorpt_coefficient_mu    1.079
_exptl_absorpt_correction_T_max  .882
_exptl_absorpt_correction_T_min  .813
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.722
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             352
_exptl_crystal_size_max          .20
_exptl_crystal_size_mid          .14
_exptl_crystal_size_min          .12
_refine_diff_density_max         2.56
_refine_diff_density_min         -2.61
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   .960
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     188
_refine_ls_number_reflns         3185
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      .960
_refine_ls_R_factor_all          .109
_refine_ls_R_factor_gt           .080
_refine_ls_shift/su_max          <0.001
_refine_ls_shift/su_mean         .000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.1175P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          .188
_refine_ls_wR_factor_ref         .203
_reflns_number_gt                2080
_reflns_number_total             3185
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            tr1008.cif
_cod_data_source_block           II
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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 
;
_cod_original_cell_volume        671.8(2)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               2012538
_cod_database_fobs_code          2012538