The crystal structure of lead(II) 1,3-diethyl-2-thiobarbiturate
Golovnev, Nikolay; Molokeev, Maxim; Golovneva, Irina; Russian Journal of Coordination Chemistry 41 (2015) 300–; doi:10.1134/S1070328415050012

data_1529237
_publ_section_title
;
 The crystal structure of lead(II) 1,3-diethyl-2-thiobarbiturate
;
_journal_issue                   5
_journal_name_full               'Russian Journal of Coordination Chemistry'
_journal_page_first              300
_journal_paper_doi               10.1134/S1070328415050012
_journal_volume                  41
_journal_year                    2015
_chemical_formula_sum            'C16 H22 N4 O4 Pb S2'
_chemical_formula_weight         605.68
_chemical_name_systematic
;
Catena-tetrakis(mu~3~-1,3-diethyl-2-thiobarbiturato-O,O',S)-dilead(II)
;
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            9
_cell_length_a                   12.9503(3)
_cell_length_b                   12.9503(3)
_cell_length_c                   32.0771(10)
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.68
_cell_measurement_theta_min      1.90
_cell_volume                     4658.9(2)
_computing_cell_refinement       'APEX2 (Bruker, 2003-2008)'
_computing_data_collection       'APEX2 (Bruker, 2003-2008)'
_computing_data_reduction        'SAINT (Bruker, 2009)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2005)'
_computing_publication_material  'publCIF (Westrip, 2009)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0421
_diffrn_reflns_av_unetI/netI     0.0297
_diffrn_reflns_laue_measured_fraction_full 0.999
_diffrn_reflns_laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            13104
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.676
_diffrn_reflns_theta_min         1.905
_exptl_absorpt_coefficient_mu    8.378
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.5782
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2004/1. Bruker AXS Inc., Madison, Wisconsin, USA, 2004
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.943
_exptl_crystal_description       block
_exptl_crystal_F_000             2628
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.362
_refine_diff_density_min         -0.450
_refine_diff_density_rms         0.080
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     125
_refine_ls_number_reflns         1979
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.0369
_refine_ls_R_factor_gt           0.0226
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0140P)^2^+7.1510P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0381
_refine_ls_wR_factor_ref         0.0415
_reflns_Friedel_coverage         0.000
_reflns_friedel_fraction_full    .
_reflns_friedel_fraction_max     .
_reflns_number_gt                1610
_reflns_number_total             1979
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            PbDETBA2.cif
_cod_data_source_block           f
_cod_original_cell_volume        4658.9(3)
_cod_database_code               1529237
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              58492
_shelx_hkl_checksum              41438
_cod_database_fobs_code 1529237