#------------------------------------------------------------------------------
#$Date: 2016-02-20 22:30:07 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176789 $
#$URL: svn://www.crystallography.net/cod/cif/2/22/53/2225335.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2225335
loop_
_publ_author_name
'Du, Mei'
'Liu, Bing-Xin'
'Nie, Jing-Jing'
'Xu, Duan-Jun'
_publ_section_title
;
 Bis(μ-iminodiacetato)bis[(2,2'-diamino-4,4'-bi-1,3-thiazole)lead(II)]
 tetrahydrate
;
_journal_coeditor_code           NG2733
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m343
_journal_page_last               m344
_journal_paper_doi               10.1107/S1600536810006926
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          '[Pb2 (C4 H5 N O4)2 (C6 H6 N4 S2)2], 4H2 O'
_chemical_formula_moiety         'C20 H22 N10 O8 Pb2 S4, 4(H2 O)'
_chemical_formula_sum            'C20 H30 N10 O12 Pb2 S4'
_chemical_formula_weight         1145.16
_chemical_name_systematic
;
Bis(μ-iminodiacetato)bis[(2,2'-diamino-4,4'-bi-1,3-thiazole)lead(II)]
tetrahydrate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                77.0732(12)
_cell_angle_beta                 67.4141(15)
_cell_angle_gamma                69.0690(12)
_cell_formula_units_Z            1
_cell_length_a                   9.2241(8)
_cell_length_b                   9.8526(9)
_cell_length_c                   10.6380(11)
_cell_measurement_reflns_used    4336
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      24.6
_cell_measurement_theta_min      2.1
_cell_volume                     829.54(14)
_computing_cell_refinement       'PROCESS-AUTO (Rigaku, 1998)'
_computing_data_collection       'PROCESS-AUTO (Rigaku, 1998)'
_computing_data_reduction        'CrystalStructure (Rigaku/MSC, 2002)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR92 (Altomare et al.,  1993)'
_diffrn_ambient_temperature      295(2)
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       ω
_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  0.021
_diffrn_reflns_av_sigmaI/netI    0.030
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            5960
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.0
_diffrn_reflns_theta_min         2.1
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    10.459
_exptl_absorpt_correction_T_max  0.350
_exptl_absorpt_correction_T_min  0.132
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(ABSCOR; Higashi, 1995)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.292
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             544
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.540
_refine_diff_density_min         -0.703
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         2878
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0211
_refine_ls_R_factor_gt           0.0197
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0190P)²+0.7917P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0476
_refine_ls_wR_factor_ref         0.0481
_reflns_number_gt                2745
_reflns_number_total             2878
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            ng2733.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_database_code               2225335
_cod_database_fobs_code          2225335
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb Pb 0.545731(18) 0.724630(15) 0.424338(14) 0.02919(7) Uani d . 1 . .
S S1 0.85653(18) 1.10157(14) 0.16319(14) 0.0551(3) Uani d . 1 . .
S S2 0.70556(17) 0.84111(15) 0.78711(13) 0.0513(3) Uani d . 1 . .
O O1 0.6288(4) 0.4760(3) 0.5554(3) 0.0400(7) Uani d . 1 . .
O O2 0.8401(5) 0.2774(4) 0.5652(4) 0.0696(11) Uani d . 1 . .
O O3 0.5809(4) 0.7154(3) 0.1777(3) 0.0431(7) Uani d . 1 . .
O O4 0.6770(6) 0.5550(4) 0.0268(4) 0.0714(12) Uani d . 1 . .
O O1W 0.7380(5) 1.1758(4) -0.1588(4) 0.0577(9) Uani d D 1 . .
O O2W 1.0741(5) 0.6671(5) 0.1186(5) 0.0717(11) Uani d D 1 . .
N N1 0.7119(4) 0.9098(4) 0.3108(4) 0.0359(8) Uani d . 1 . .
N N2 0.7160(6) 0.9566(5) 0.0832(4) 0.0541(11) Uani d D 1 . .
N N3 0.6755(4) 0.7770(4) 0.5787(3) 0.0357(8) Uani d . 1 . .
N N4 0.5919(6) 0.6270(5) 0.7807(4) 0.0563(11) Uani d D 1 . .
N N5 0.8084(4) 0.5688(4) 0.2998(4) 0.0355(8) Uani d D 1 . .
C C1 0.7507(5) 0.9781(5) 0.1862(4) 0.0382(10) Uani d . 1 . .
C C2 0.8435(6) 1.0598(5) 0.3335(5) 0.0494(12) Uani d . 1 . .
H H2 0.8841 1.1027 0.3770 0.059 Uiso calc R 1 . .
C C3 0.7666(5) 0.9569(5) 0.3947(4) 0.0372(10) Uani d . 1 . .
C C4 0.6525(6) 0.7362(5) 0.7099(4) 0.0399(10) Uani d . 1 . .
C C5 0.7564(6) 0.9461(5) 0.6339(5) 0.0461(11) Uani d . 1 . .
H H5 0.7934 1.0262 0.6206 0.055 Uiso calc R 1 . .
C C6 0.7354(5) 0.8967(4) 0.5350(5) 0.0368(10) Uani d . 1 . .
C C11 0.7810(6) 0.4004(5) 0.5131(4) 0.0370(10) Uani d . 1 . .
C C12 0.8948(6) 0.4667(5) 0.3912(5) 0.0418(10) Uani d . 1 . .
H H12A 0.9443 0.5183 0.4229 0.050 Uiso calc R 1 . .
H H12B 0.9827 0.3892 0.3400 0.050 Uiso calc R 1 . .
C C13 0.7855(6) 0.4939(5) 0.2072(4) 0.0408(10) Uani d . 1 . .
H H13A 0.7393 0.4162 0.2599 0.049 Uiso calc R 1 . .
H H13B 0.8919 0.4499 0.1420 0.049 Uiso calc R 1 . .
C C14 0.6733(6) 0.5959(5) 0.1303(4) 0.0427(11) Uani d . 1 . .
H H11 0.768(8) 1.197(7) -0.2418(10) 0.080 Uiso d D 1 . .
H H12 0.6393(18) 1.220(6) -0.132(6) 0.080 Uiso d D 1 . .
H H21 1.124(7) 0.724(5) 0.113(7) 0.080 Uiso d D 1 . .
H H22 1.147(6) 0.594(4) 0.086(7) 0.080 Uiso d D 1 . .
H H2A 0.662(6) 0.895(5) 0.101(6) 0.080 Uiso d D 1 . .
H H2B 0.751(8) 0.997(6) 0.001(2) 0.080 Uiso d D 1 . .
H H4A 0.582(7) 0.570(5) 0.736(5) 0.080 Uiso d D 1 . .
H H4B 0.595(7) 0.598(6) 0.862(2) 0.080 Uiso d D 1 . .
H H5N 0.865(6) 0.626(5) 0.247(5) 0.080 Uiso d D 1 . .
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 0.0000 '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 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.0000 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N5 Pb O3 . . 66.12(11) ?
N5 Pb O1 . . 67.04(11) ?
O3 Pb O1 . . 114.56(10) ?
N5 Pb N1 . . 78.68(11) ?
O3 Pb N1 . . 81.95(10) ?
O1 Pb N1 . . 128.64(10) ?
N5 Pb N3 . . 90.68(12) ?
O3 Pb N3 . . 143.48(11) ?
O1 Pb N3 . . 77.56(10) ?
N1 Pb N3 . . 65.44(11) ?
C2 S1 C1 . . 89.0(2) ?
C5 S2 C4 . . 89.4(2) ?
C11 O1 Pb . . 116.9(3) ?
C14 O3 Pb . . 114.4(3) ?
H11 O1W H12 . . 105(6) ?
H21 O2W H22 . . 104(6) ?
C1 N1 C3 . . 110.4(4) ?
C1 N1 Pb . . 132.4(3) ?
C3 N1 Pb . . 117.1(3) ?
C1 N2 H2A . . 116(4) ?
C1 N2 H2B . . 122(4) ?
H2A N2 H2B . . 121(6) ?
C4 N3 C6 . . 111.2(4) ?
C4 N3 Pb . . 128.8(3) ?
C6 N3 Pb . . 116.8(3) ?
C4 N4 H4A . . 118(4) ?
C4 N4 H4B . . 119(4) ?
H4A N4 H4B . . 119(6) ?
C13 N5 C12 . . 112.7(3) ?
C13 N5 Pb . . 109.0(3) ?
C12 N5 Pb . . 112.3(3) ?
C13 N5 H5N . . 105(4) ?
C12 N5 H5N . . 111(4) ?
Pb N5 H5N . . 106(4) ?
N1 C1 N2 . . 124.7(4) ?
N1 C1 S1 . . 114.6(3) ?
N2 C1 S1 . . 120.7(3) ?
C3 C2 S1 . . 110.9(4) ?
C3 C2 H2 . . 124.5 ?
S1 C2 H2 . . 124.5 ?
C2 C3 N1 . . 115.0(4) ?
C2 C3 C6 . . 125.7(4) ?
N1 C3 C6 . . 119.3(4) ?
N3 C4 N4 . . 124.6(4) ?
N3 C4 S2 . . 113.7(3) ?
N4 C4 S2 . . 121.7(3) ?
C6 C5 S2 . . 111.0(4) ?
C6 C5 H5 . . 124.5 ?
S2 C5 H5 . . 124.5 ?
C5 C6 N3 . . 114.7(4) ?
C5 C6 C3 . . 126.4(4) ?
N3 C6 C3 . . 119.0(4) ?
O2 C11 O1 . . 124.6(4) ?
O2 C11 C12 . . 118.1(4) ?
O1 C11 C12 . . 117.3(4) ?
N5 C12 C11 . . 112.3(4) ?
N5 C12 H12A . . 109.1 ?
C11 C12 H12A . . 109.1 ?
N5 C12 H12B . . 109.1 ?
C11 C12 H12B . . 109.1 ?
H12A C12 H12B . . 107.9 ?
N5 C13 C14 . . 112.6(4) ?
N5 C13 H13A . . 109.1 ?
C14 C13 H13A . . 109.1 ?
N5 C13 H13B . . 109.1 ?
C14 C13 H13B . . 109.1 ?
H13A C13 H13B . . 107.8 ?
O4 C14 O3 . . 124.8(5) ?
O4 C14 C13 . . 117.8(4) ?
O3 C14 C13 . . 117.4(4) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Pb O1 . 2.546(3) y
Pb O1 2_666 2.892(3) y
Pb O3 . 2.536(3) y
Pb N1 . 2.593(3) y
Pb N3 . 2.594(3) y
Pb N5 . 2.402(4) y
S1 C2 . 1.732(5) ?
S1 C1 . 1.739(4) ?
S2 C5 . 1.718(5) ?
S2 C4 . 1.741(4) ?
O1 C11 . 1.283(5) ?
O2 C11 . 1.237(5) ?
O3 C14 . 1.259(5) ?
O4 C14 . 1.239(5) ?
O1W H11 . 0.819(16) ?
O1W H12 . 0.82(5) ?
O2W H21 . 0.82(7) ?
O2W H22 . 0.82(5) ?
N1 C1 . 1.321(5) ?
N1 C3 . 1.403(5) ?
N2 C1 . 1.331(6) ?
N2 H2A . 0.86(6) ?
N2 H2B . 0.86(3) ?
N3 C4 . 1.318(5) ?
N3 C6 . 1.391(5) ?
N4 C4 . 1.335(6) ?
N4 H4A . 0.86(5) ?
N4 H4B . 0.86(3) ?
N5 C13 . 1.468(5) ?
N5 C12 . 1.475(5) ?
N5 H5N . 0.86(5) ?
C2 C3 . 1.348(6) ?
C2 H2 . 0.9300 ?
C3 C6 . 1.435(6) ?
C5 C6 . 1.354(6) ?
C5 H5 . 0.9300 ?
C11 C12 . 1.509(6) ?
C12 H12A . 0.9700 ?
C12 H12B . 0.9700 ?
C13 C14 . 1.513(6) ?
C13 H13A . 0.9700 ?
C13 H13B . 0.9700 ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
N2 H2A O3 . 0.86(6) 2.05(5) 2.880(6) 162(5) y
N2 H2B O1W . 0.86(3) 2.16(4) 2.959(6) 153(6) y
N4 H4A O1 . 0.86(5) 2.15(5) 2.946(5) 155(5) y
N4 H4B O4 1_556 0.86(3) 2.07(5) 2.885(7) 159(6) y
N5 H5N O2W . 0.87(5) 2.01(6) 2.809(7) 153(4) y
O1W H11 O2 1_564 0.819(16) 1.97(2) 2.783(6) 171(5) y
O1W H12 O3 2_675 0.82(5) 2.11(4) 2.819(6) 144(5) y
O2W H21 O1W 2_775 0.82(7) 2.10(7) 2.892(7) 161(6) y
O2W H22 O4 2_765 0.82(5) 1.95(5) 2.766(6) 168(7) y
C5 H5 O2 1_565 0.93 2.56 3.476(6) 167 y
