Approaching the crystal structure of N-PdSO4 in the monoclinic subcell a/2, b/2, c/2 (see J. Alloys and Compounds 216, 1994, 11-19)
Yvon Laligant; Armel Le Bail; Personal communication to COD  (2016) –; doi:

data_3500059
_publ_section_title
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 Approaching the crystal structure of N-PdSO4 in the monoclinic subcell
 a/2, b/2, c/2 (see J. Alloys and Compounds 216, 1994, 11-19)
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_journal_name_full               'Personal communication to COD'
_journal_year                    2016
_chemical_compound_source
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Synthesis as in J. Alloys and Compounds 216 (1994) 11-19
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_chemical_formula_sum            'O4 Pd S'
_chemical_formula_weight         202.483
_chemical_name_common            N-PdSO4
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      12
_symmetry_space_group_name_Hall  '-I 2y'
_symmetry_space_group_name_H-M   'I 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 92.8096(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   4.9466(10)
_cell_length_b                   4.9481(10)
_cell_length_c                   6.1943(10)
_cell_measurement_temperature    293(2)
_cell_volume                     151.43(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.975
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0379
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            238
_diffrn_reflns_theta_full        29.92
_diffrn_reflns_theta_max         29.92
_diffrn_reflns_theta_min         5.15
_exptl_special_details
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High disorder.
Two SO4 tetrahedra constrained by SADI using SHELX,
leading to S exploding in 4 neoghbouring positions.
But what are these Q1, Q2 and Q3 thet make R decreasing
by 3 % ???! 
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_geom_special_details
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 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
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_refine_diff_density_max         4.954
_refine_diff_density_min         -8.047
_refine_diff_density_rms         1.564
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.273
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     40
_refine_ls_number_reflns         238
_refine_ls_number_restraints     94
_refine_ls_restrained_S_all      1.120
_refine_ls_R_factor_all          0.0739
_refine_ls_R_factor_gt           0.0665
_refine_ls_shift/su_mean         0.009
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1475P)^2^+5.8642P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1696
_refine_ls_wR_factor_ref         0.1891
_refine_special_details
; 
 Refinement of F^2^ against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F^2^, conventional R-factors R are based 
 on F, with F set to zero for negative F^2^. The threshold expression of 
 F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F^2^ are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
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_reflns_number_gt                233
_reflns_number_total             238
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            PdSO4.cif
_cod_data_source_block           PdSO4
_cod_depositor_comments
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The following automatic conversions were performed:

data name '_atom_site_symetry_multiplicity' was replaced with
'_atom_site_symmetry_multiplicity' as specified in the replacement
file 'data/replacement-values/replacement_tags.lst'.

Automatic conversion script
Id: cif_correct_tags 9268 2022-04-12 08:56:07Z antanas 
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_cod_original_sg_symbol_H-M      'I 2/m'
_cod_database_code               3500059
_cod_database_fobs_code          3500059