#------------------------------------------------------------------------------
#$Date: 2015-07-21 20:35:22 +0300 (Tue, 21 Jul 2015) $
#$Revision: 152364 $
#$URL: svn://www.crystallography.net/cod/cif/1/52/92/1529237.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1529237
loop_
_publ_author_name
'Golovnev, Nikolay'
'Molokeev, Maxim'
'Golovneva, Irina'
_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(mu₃-1,3-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       'φ and ω 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/[σ²(Fo²)+(0.0140P)²+7.1510P] where P=(Fo²+2Fc²)/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 > 2σ(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_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.3333 0.6667 0.1667 0.04080(11) Uani 1 6 d S T P . .
Pb2 Pb 0.6667 0.3333 0.12068(2) 0.04054(9) Uani 1 3 d S T P . .
S S 0.19923(10) 0.15828(11) 0.27671(4) 0.0672(3) Uani 1 1 d . . . . .
O1 O 0.4061(3) 0.5511(3) 0.20677(9) 0.0674(8) Uani 1 1 d . . . . .
O2 O 0.5070(2) 0.2616(3) 0.16987(9) 0.0620(8) Uani 1 1 d . . . . .
N1 N 0.3760(3) 0.2302(3) 0.22204(10) 0.0429(8) Uani 1 1 d . . . . .
N3 N 0.3116(3) 0.3653(3) 0.23564(10) 0.0483(8) Uani 1 1 d . . . . .
C2 C 0.3009(3) 0.2561(3) 0.24308(12) 0.0440(9) Uani 1 1 d . . . . .
C4 C 0.3963(3) 0.4502(4) 0.20767(13) 0.0480(10) Uani 1 1 d . . . . .
C5 C 0.4585(3) 0.4119(4) 0.18390(13) 0.0485(10) Uani 1 1 d . . . . .
H5 H 0.5072 0.4612 0.1627 0.058 Uiso 1 1 calc R U . . .
C6 C 0.4518(3) 0.3029(3) 0.19008(12) 0.0456(10) Uani 1 1 d . . . . .
C9 C 0.2387(4) 0.4032(4) 0.25993(15) 0.0697(13) Uani 1 1 d . . . . .
H91 H 0.2235 0.4566 0.2432 0.084 Uiso 1 1 calc R U . . .
H92 H 0.1625 0.3339 0.2668 0.084 Uiso 1 1 calc R U . . .
C7 C 0.3804(4) 0.1212(4) 0.23257(14) 0.0574(11) Uani 1 1 d . . . . .
H71 H 0.4071 0.0959 0.2084 0.069 Uiso 1 1 calc R U . . .
H72 H 0.3009 0.0578 0.2397 0.069 Uiso 1 1 calc R U . . .
C8 C 0.4631(5) 0.1418(5) 0.26862(15) 0.0853(16) Uani 1 1 d . . . . .
H81 H 0.4347 0.1632 0.2929 0.102 Uiso 1 1 calc R U . . .
H82 H 0.5417 0.2052 0.2618 0.102 Uiso 1 1 calc R U . . .
H83 H 0.4657 0.0703 0.2741 0.102 Uiso 1 1 calc R U . . .
C10 C 0.3010(5) 0.4646(5) 0.29888(17) 0.0969(18) Uani 1 1 d . . . . .
H101 H 0.3148 0.4112 0.3156 0.116 Uiso 1 1 calc R U . . .
H102 H 0.2526 0.4884 0.3141 0.116 Uiso 1 1 calc R U . . .
H103 H 0.3759 0.5337 0.2921 0.116 Uiso 1 1 calc R U . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
O1 Pb1 O1 95.69(10) 15 14_455
O1 Pb1 O1 84.31(10) 15 2_665
O1 Pb1 O1 180.0 14_455 2_665
O1 Pb1 O1 180.0 15 3_565
O1 Pb1 O1 84.31(10) 14_455 3_565
O1 Pb1 O1 95.69(10) 2_665 3_565
O1 Pb1 O1 95.69(10) 15 13_565
O1 Pb1 O1 95.69(10) 14_455 13_565
O1 Pb1 O1 84.31(10) 2_665 13_565
O1 Pb1 O1 84.31(10) 3_565 13_565
O1 Pb1 O1 84.31(10) 15 .
O1 Pb1 O1 84.31(10) 14_455 .
O1 Pb1 O1 95.69(10) 2_665 .
O1 Pb1 O1 95.69(10) 3_565 .
O1 Pb1 O1 180.0 13_565 .
O2 Pb2 O2 81.13(11) 2_655 3_665
O2 Pb2 O2 81.13(11) 2_655 .
O2 Pb2 O2 81.13(11) 3_665 .
O2 Pb2 S 84.78(7) 2_655 14
O2 Pb2 S 120.75(8) 3_665 14
O2 Pb2 S 151.72(7) . 14
O2 Pb2 S 120.75(8) 2_655 13
O2 Pb2 S 151.72(7) 3_665 13
O2 Pb2 S 84.78(7) . 13
S Pb2 S 81.56(3) 14 13
O2 Pb2 S 151.72(7) 2_655 15
O2 Pb2 S 84.78(7) 3_665 15
O2 Pb2 S 120.75(8) . 15
S Pb2 S 81.56(3) 14 15
S Pb2 S 81.56(3) 13 15
C2 S Pb2 98.67(13) . 13
C4 O1 Pb1 140.4(3) . .
C6 O2 Pb2 137.4(3) . .
C2 N1 C6 122.9(3) . .
C2 N1 C7 119.8(3) . .
C6 N1 C7 117.3(3) . .
C2 N3 C4 123.3(3) . .
C2 N3 C9 119.8(3) . .
C4 N3 C9 116.7(3) . .
N1 C2 N3 117.0(3) . .
N1 C2 S 121.3(3) . .
N3 C2 S 121.7(3) . .
O1 C4 C5 126.6(4) . .
O1 C4 N3 117.4(4) . .
C5 C4 N3 116.1(4) . .
C4 C5 C6 122.8(4) . .
C4 C5 H5 118.6 . .
C6 C5 H5 118.6 . .
O2 C6 C5 126.7(4) . .
O2 C6 N1 116.3(4) . .
C5 C6 N1 117.0(4) . .
C10 C9 N3 110.7(4) . .
C10 C9 H91 109.5 . .
N3 C9 H91 109.5 . .
C10 C9 H92 109.5 . .
N3 C9 H92 109.5 . .
H91 C9 H92 108.1 . .
N1 C7 C8 111.7(3) . .
N1 C7 H71 109.3 . .
C8 C7 H71 109.3 . .
N1 C7 H72 109.3 . .
C8 C7 H72 109.3 . .
H71 C7 H72 108.0 . .
C7 C8 H81 109.5 . .
C7 C8 H82 109.5 . .
H81 C8 H82 109.5 . .
C7 C8 H83 109.5 . .
H81 C8 H83 109.5 . .
H82 C8 H83 109.5 . .
C9 C10 H101 109.5 . .
C9 C10 H102 109.5 . .
H101 C10 H102 109.5 . .
C9 C10 H103 109.5 . .
H101 C10 H103 109.5 . .
H102 C10 H103 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pb1 O1 2.488(3) 15
Pb1 O1 2.488(3) 14_455
Pb1 O1 2.488(3) 2_665
Pb1 O1 2.488(3) 3_565
Pb1 O1 2.488(3) 13_565
Pb1 O1 2.489(3) .
Pb2 O2 2.389(3) 2_655
Pb2 O2 2.389(3) 3_665
Pb2 O2 2.389(3) .
Pb2 S 3.1292(12) 14
Pb2 S 3.1292(12) 13
Pb2 S 3.1293(12) 15
S C2 1.683(4) .
S Pb2 3.1292(12) 13
O1 C4 1.249(5) .
O2 C6 1.265(4) .
N1 C2 1.357(4) .
N1 C6 1.406(5) .
N1 C7 1.480(5) .
N3 C2 1.371(5) .
N3 C4 1.418(5) .
N3 C9 1.484(5) .
C4 C5 1.369(5) .
C5 C6 1.384(5) .
C5 H5 0.9300 .
C9 C10 1.484(6) .
C9 H91 0.9700 .
C9 H92 0.9700 .
C7 C8 1.507(6) .
C7 H71 0.9700 .
C7 H72 0.9700 .
C8 H81 0.9600 .
C8 H82 0.9600 .
C8 H83 0.9600 .
C10 H101 0.9600 .
C10 H102 0.9600 .
C10 H103 0.9600 .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
C6 N1 C2 N3 -7.9(5) . . . .
C7 N1 C2 N3 172.0(3) . . . .
C6 N1 C2 S 172.0(3) . . . .
C7 N1 C2 S -8.1(5) . . . .
C4 N3 C2 N1 -0.3(5) . . . .
C9 N3 C2 N1 -175.4(3) . . . .
C4 N3 C2 S 179.8(3) . . . .
C9 N3 C2 S 4.7(5) . . . .
Pb2 S C2 N1 -82.6(3) 13 . . .
Pb2 S C2 N3 97.3(3) 13 . . .
Pb1 O1 C4 C5 83.1(6) . . . .
Pb1 O1 C4 N3 -96.1(5) . . . .
C2 N3 C4 O1 -172.6(3) . . . .
C9 N3 C4 O1 2.6(5) . . . .
C2 N3 C4 C5 8.1(5) . . . .
C9 N3 C4 C5 -176.7(3) . . . .
O1 C4 C5 C6 172.6(4) . . . .
N3 C4 C5 C6 -8.2(6) . . . .
Pb2 O2 C6 C5 11.6(6) . . . .
Pb2 O2 C6 N1 -168.5(2) . . . .
C4 C5 C6 O2 -179.2(4) . . . .
C4 C5 C6 N1 0.8(5) . . . .
C2 N1 C6 O2 -172.2(3) . . . .
C7 N1 C6 O2 8.0(5) . . . .
C2 N1 C6 C5 7.8(5) . . . .
C7 N1 C6 C5 -172.1(3) . . . .
C2 N3 C9 C10 88.4(5) . . . .
C4 N3 C9 C10 -87.0(5) . . . .
C2 N1 C7 C8 -84.7(4) . . . .
C6 N1 C7 C8 95.2(4) . . . .

_cod_database_fobs_code 1529237
