#------------------------------------------------------------------------------
#$Date: 2016-02-20 22:30:07 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176789 $
#$URL: svn://www.crystallography.net/cod/cif/2/22/84/2228402.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_2228402
loop_
_publ_author_name
'Li, Bao'
'Li, Wen'
'Ye, Ling'
'Hou, Guang-Feng'
'Wu, Li-Xin'
_publ_section_title
;
 Poly[di-μ₂-aqua-μ₄-chlorido-μ₄-(2-mercaptopyrimidine-4,6-diolato-κ⁴O:O:O':O')-disodium(I)]
;
_journal_coeditor_code           HY2376
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1546
_journal_paper_doi               10.1107/S1600536810045836
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          '[Na2 (C4 H3 N2 O2 S) Cl (H2 O)2]'
_chemical_formula_moiety         'C4 H7 Cl N2 Na2 O4 S'
_chemical_formula_sum            'C4 H7 Cl N2 Na2 O4 S'
_chemical_formula_weight         260.61
_chemical_name_systematic
;
Poly[di-μ₂-aqua-μ₄-chlorido-μ₄-(2-mercaptopyrimidine-4,6-diolato-
κ⁴O:O:O':O')-disodium(I)]
;
_space_group_IT_number           74
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-I 2b 2'
_symmetry_space_group_name_H-M   'I m m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.815(3)
_cell_length_b                   6.5938(13)
_cell_length_c                   8.8587(18)
_cell_measurement_reflns_used    4272
_cell_measurement_temperature    290(2)
_cell_measurement_theta_max      27.40
_cell_measurement_theta_min      3.32
_cell_volume                     982.2(3)
_computing_cell_refinement       'RAPID-AUTO (Rigaku, 1998)'
_computing_data_collection       'RAPID-AUTO (Rigaku, 1998)'
_computing_data_reduction        'CrystalStructure (Rigaku/MSC, 2002)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'PLATON (Spek, 2009)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      290(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotation anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0171
_diffrn_reflns_av_sigmaI/netI    0.0103
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            4752
_diffrn_reflns_theta_full        27.40
_diffrn_reflns_theta_max         27.40
_diffrn_reflns_theta_min         3.85
_exptl_absorpt_coefficient_mu    0.677
_exptl_absorpt_correction_T_max  0.9416
_exptl_absorpt_correction_T_min  0.9232
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(ABSCOR; Higashi, 1995)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.762
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             528
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.260
_refine_diff_density_min         -0.301
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     46
_refine_ls_number_reflns         633
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.093
_refine_ls_R_factor_all          0.0255
_refine_ls_R_factor_gt           0.0238
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0282P)²+1.0461P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0610
_refine_ls_wR_factor_ref         0.0619
_reflns_number_gt                581
_reflns_number_total             633
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            hy2376.cif
_cod_data_source_block           I
_cod_database_code               2228402
_cod_database_fobs_code          2228402
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y+1/2, z'
'-x, y+1/2, -z'
'x, -y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1, z+1/2'
'-x+1/2, y+1, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x, y-1/2, -z'
'x, -y-1/2, z'
'-x, y, z'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y, -z+1/2'
'x+1/2, -y, z+1/2'
'-x+1/2, y+1/2, z+1/2'
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
C C1 0.5000 0.2500 0.7898(3) 0.0222(5) Uani d S 1 . .
C C2 0.42785(10) 0.2500 1.02887(18) 0.0174(3) Uani d S 1 . .
C C3 0.5000 0.2500 1.1064(3) 0.0199(5) Uani d S 1 . .
H H3 0.5000 0.2500 1.2113 0.024 Uiso calc SR 1 . .
Cl Cl1 0.2500 0.2500 0.7500 0.02138(17) Uani d S 1 . .
N N1 0.43218(8) 0.2500 0.87105(16) 0.0204(3) Uani d S 1 . .
H H1 0.3881 0.2500 0.8220 0.025 Uiso calc SR 1 . .
Na Na1 0.25570(4) 0.5000 1.0000 0.0256(2) Uani d S 1 . .
O O1 0.35874(7) 0.2500 1.08459(14) 0.0242(3) Uani d S 1 . .
O O2 0.16839(8) 0.2500 1.10168(15) 0.0294(3) Uani d S 1 . .
H H2A 0.1533 0.2500 1.1978 0.044 Uiso d SR 1 . .
H H2B 0.1232 0.2500 1.0538 0.044 Uiso d SR 1 . .
S S1 0.5000 0.2500 0.60136(8) 0.0531(3) Uani d S 1 . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
C1 0.0155(11) 0.0313(13) 0.0197(11) 0.000 0.000 0.000
C2 0.0158(7) 0.0182(7) 0.0182(8) 0.000 0.0019(6) 0.000
C3 0.0178(11) 0.0262(12) 0.0158(10) 0.000 0.000 0.000
Cl1 0.0201(3) 0.0286(3) 0.0154(3) 0.000 -0.0028(2) 0.000
N1 0.0127(7) 0.0314(8) 0.0172(7) 0.000 -0.0013(5) 0.000
Na1 0.0288(4) 0.0236(4) 0.0245(4) 0.000 0.000 -0.0031(3)
O1 0.0141(6) 0.0382(7) 0.0204(6) 0.000 0.0030(5) 0.000
O2 0.0206(6) 0.0449(8) 0.0225(6) 0.000 0.0013(5) 0.000
S1 0.0199(3) 0.1243(10) 0.0150(3) 0.000 0.000 0.000
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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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
N1 C1 N1 2_655 . 115.5(2) ?
N1 C1 S1 2_655 . 122.25(11) ?
N1 C1 S1 . . 122.25(11) ?
O1 C2 C3 . . 127.48(16) ?
O1 C2 N1 . . 115.99(15) ?
C3 C2 N1 . . 116.53(15) ?
C2 C3 C2 2_655 . 121.0(2) ?
C2 C3 H3 2_655 . 119.5 ?
C2 C3 H3 . . 119.5 ?
Na1 Cl1 Na1 . 13_556 180.0 ?
Na1 Cl1 Na1 . 10_557 73.272(15) ?
Na1 Cl1 Na1 13_556 10_557 106.728(15) ?
Na1 Cl1 Na1 . 6_554 106.728(15) ?
Na1 Cl1 Na1 13_556 6_554 73.272(16) ?
Na1 Cl1 Na1 10_557 6_554 180.0 ?
C1 N1 C2 . . 125.23(16) ?
C1 N1 H1 . . 117.4 ?
C2 N1 H1 . . 117.4 ?
O2 Na1 O2 . 10_567 103.98(6) ?
O2 Na1 O1 . 10_567 173.45(5) ?
O2 Na1 O1 10_567 10_567 81.84(4) ?
O2 Na1 O1 . . 81.84(4) ?
O2 Na1 O1 10_567 . 173.45(5) ?
O1 Na1 O1 10_567 . 92.53(5) ?
O2 Na1 Cl1 . . 82.47(3) ?
O2 Na1 Cl1 10_567 . 95.07(3) ?
O1 Na1 Cl1 10_567 . 100.18(3) ?
O1 Na1 Cl1 . . 82.60(3) ?
O2 Na1 Cl1 . 6 95.07(3) ?
O2 Na1 Cl1 10_567 6 82.47(3) ?
O1 Na1 Cl1 10_567 6 82.60(3) ?
O1 Na1 Cl1 . 6 100.18(3) ?
Cl1 Na1 Cl1 . 6 176.03(3) ?
O2 Na1 Na1 . 10_567 133.74(3) ?
O2 Na1 Na1 10_567 10_567 46.26(3) ?
O1 Na1 Na1 10_567 10_567 48.87(2) ?
O1 Na1 Na1 . 10_567 131.13(2) ?
Cl1 Na1 Na1 . 10_567 126.636(8) ?
Cl1 Na1 Na1 6 10_567 53.364(8) ?
O2 Na1 Na1 . 10_557 46.26(3) ?
O2 Na1 Na1 10_567 10_557 133.74(3) ?
O1 Na1 Na1 10_567 10_557 131.13(2) ?
O1 Na1 Na1 . 10_557 48.87(2) ?
Cl1 Na1 Na1 . 10_557 53.364(8) ?
Cl1 Na1 Na1 6 10_557 126.636(8) ?
Na1 Na1 Na1 10_567 10_557 180.00(5) ?
C2 O1 Na1 . 10_557 121.29(7) ?
C2 O1 Na1 . . 121.29(7) ?
Na1 O1 Na1 10_557 . 82.26(4) ?
Na1 O2 Na1 . 10_557 87.48(5) ?
Na1 O2 H2A . . 122.5 ?
Na1 O2 H2A 10_557 . 122.5 ?
Na1 O2 H2B . . 110.7 ?
Na1 O2 H2B 10_557 . 110.7 ?
H2A O2 H2B . . 102.6 ?
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
C1 N1 . 1.3484(19) ?
C1 S1 . 1.670(3) ?
C2 O1 . 1.263(2) ?
C2 C3 . 1.394(2) ?
C2 N1 . 1.400(2) ?
C3 H3 . 0.9300 ?
Cl1 Na1 . 2.7625(4) ?
N1 H1 . 0.8600 ?
Na1 O2 . 2.3842(11) ?
Na1 O1 . 2.5062(11) ?
Na1 Cl1 6 2.7625(4) ?
Na1 Na1 10_567 3.2969(6) ?
O2 H2A . 0.8885 ?
O2 H2B . 0.8701 ?
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
N1 H1 Cl1 . 0.86 2.41 3.2457(15) 165 y
O2 H2A O1 13_557 0.89 1.94 2.8164(19) 169 y
O2 H2B S1 8_456 0.87 2.49 3.3545(15) 176 y
