Molecular Adducts of Inorganic Salts. III. Non-Centrosymmetric 3Pb(ReO~4~)~2~.2tu.2H~2~O (tu = Thiourea)
Macícek, J.; Angelova, O.; Acta Crystallographica Section C 51 (1995) 2539–2542; doi:10.1107/S0108270195004653

data_2004305
_publ_contact_author
;
     Dr Josef Macicek
     Bulgarian Academy of Sciences
     Institute of Applied Mineralogy
     Rakovski str. 92
     1000 Sofia
     BULGARIA
;
_publ_section_title
;
 Molecular Adducts of Inorganic Salts. III. Non-Centrosymmetric
 3Pb(ReO~4~)~2~.2tu.2H~2~O (tu = Thiourea)
;
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              2539
_journal_page_last               2542
_journal_paper_doi               10.1107/S0108270195004653
_journal_volume                  51
_journal_year                    1995
_chemical_formula_structural     '(Pb (Re O4)2)3 (S C N2 H4)2 (H2 O)2'
_chemical_formula_sum            'C2 H12 N4 O26 Pb3 Re6 S2'
_chemical_formula_weight         2311.02
_chemical_name_systematic        'PB(REO4)2.THIOUREA                  '
_space_group_IT_number           113
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P -4 2ab'
_symmetry_space_group_name_H-M   'P -4 21 m'
_atom_type_scat_source           'as coded in SDP/PDP V3.0 (Enraf-Nonius, 1985)'
_audit_creation_method
'from SDP files using KAPPA (Macicek, 1992. Unpublished)'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   16.208(2)
_cell_length_b                   16.208(2)
_cell_length_c                   5.800(2)
_cell_measurement_reflns_used    22
_cell_measurement_temperature    292
_cell_measurement_theta_max      21.16
_cell_measurement_theta_min      20.25
_cell_volume                     1523.7(6)
_computing_data_collection       'CAD4 V5.0 (Enraf-Nonius, 1988)'
_computing_data_reduction        'SDP/PDP V3.0 (Enraf-Nonius, 1985)'
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_publication_material  'KAPPA (Mac\'i\<cek, 1992; Unpublished)'
_computing_structure_refinement  'SDP/PDP V3.0 (Enraf-Nonius, 1985)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1985)'
_diffrn_ambient_temperature      292
_diffrn_measurement_device       'Enraf-Nonius CAD-4 diffractometer'
_diffrn_measurement_method       'continuous scan profiles'
_diffrn_radiation_monochromator  'graphite (perpendicular mode)'
_diffrn_radiation_source         '2kW fine focus Philips tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.062
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            4712
_diffrn_reflns_reduction_process
'F~obs~ = ( I~raw~/LP )^1/2^, where LP = Lorentz-polarization correction'
_diffrn_reflns_theta_max         30.0
_diffrn_reflns_theta_min         0.0
_diffrn_standards_decay_%        '3.9   '
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    40.93
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    5.037
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1976
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.07
_refine_diff_density_max         4.604
_refine_diff_density_min         -2.878
_refine_ls_extinction_coef       2.751*10^7^
_refine_ls_extinction_method     'Stout & Jensen, 1968; formula 17.16'
_refine_ls_goodness_of_fit_all   1.946
_refine_ls_goodness_of_fit_obs   0.736
_refine_ls_hydrogen_treatment    'refined as riding'
_refine_ls_matrix_type           full
_refine_ls_number_constraints    12
_refine_ls_number_parameters     108
_refine_ls_number_reflns         1317
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.073
_refine_ls_R_factor_obs          0.041
_refine_ls_shift/esd_max         0.279
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s^2^(F)+(0.040*F)^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.132
_refine_ls_wR_factor_obs         0.049
_reflns_number_observed          1317
_reflns_number_total             2324
_reflns_observed_criterion       'I > 3.0\s(I)'
_cod_data_source_file            ns1002.cif
_cod_data_source_block           LRSA0167
_cod_depositor_comments
;
 Adding the _atom_site_type_symbol data item.

 Antanas Vaitkus,
 2017-01-30

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value '1/[\s^2^(F)+(0.040*F)^2^]' 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^(F)+(0.040*F)^2^]'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1523.5(8)
_cod_database_code               2004305