Redetermination of <i>catena</i>-poly[[chloridolead(II)]-μ~2~-chlorido-di-μ~2~-thiourea-κ^4^<i>S</i>:<i>S</i>] at 100K
Zouihri, Hafid; Yamni, Khalid; Messouss, Youssef; Tijani, Najib; Messaoudi, Lahcen; IUCrData 1 (2016) x161745–; doi:10.1107/S2414314616017454

data_1544528
_publ_section_title
;
 Redetermination of
 <i>catena</i>-poly[[chloridolead(II)]-\m~2~-chlorido-di-\m~2~-thiourea-\k^4^<i>S</i>:<i>S</i>]
 at 100K
;
_journal_coeditor_code           WM4030
_journal_issue                   11
_journal_name_full               IUCrData
_journal_page_first              x161745
_journal_paper_doi               10.1107/S2414314616017454
_journal_volume                  1
_journal_year                    2016
_chemical_formula_iupac          '[Pb Cl2 (C1 H4 N2 S1)2]'
_chemical_formula_moiety         'C2 H8 Cl2 N4 Pb S2'
_chemical_formula_sum            'C2 H8 Cl2 N4 Pb S2'
_chemical_formula_weight         430.33
_chemical_name_systematic
<i>catena</i>-Poly[[chloridolead(II)]-\m~2~-chlorido-di-\m~2~-thiourea-\k^2^<i>S</i>:<i>S</i>]
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.1951(6)
_cell_length_b                   4.02800(10)
_cell_length_c                   11.9433(3)
_cell_measurement_reflns_used    318
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.3
_cell_measurement_theta_min      1.5
_cell_volume                     1019.65(5)
_computing_cell_refinement
;
SAINT (Bruker, 2009)
;
_computing_data_collection
;
APEX2 (Bruker, 2009)
;
_computing_data_reduction
;
SAINT (Bruker, 2009)
;
_computing_molecular_graphics
;
PLATON (Spek, 2009)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEXII CCD detector'
_diffrn_measurement_method       '\w and \f'
_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  0.0319
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            23237
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         39.999
_diffrn_reflns_theta_min         2.569
_exptl_absorpt_coefficient_mu    17.428
_exptl_absorpt_correction_T_max  0.087
_exptl_absorpt_correction_T_min  0.040
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(<i>SADABS</i>; Krause <i>et al.</i>, 2015)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.803
_exptl_crystal_description       prism
_exptl_crystal_F_000             784
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.182
_refine_diff_density_min         -2.384
_refine_ls_abs_structure_details
;
Refined as an inversion twin
;
_refine_ls_abs_structure_Flack   0.315(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     101
_refine_ls_number_reflns         6206
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0204
_refine_ls_R_factor_gt           0.0181
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0121P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0406
_refine_ls_wR_factor_ref         0.0412
_reflns_number_gt                5867
_reflns_number_total             6206
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            wm4030sup1.cif
_cod_data_source_block           I
_cod_database_code               1544528
_shelx_hkl_checksum              28710
_shelx_res_checksum              28646
_cod_database_fobs_code 1544528