#------------------------------------------------------------------------------
#$Date: 2016-02-20 00:18:51 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176760 $
#$URL: svn://www.crystallography.net/cod/cif/2/01/54/2015451.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_2015451
loop_
_publ_author_name
'Valkonen, Arto'
'Ahonen, Kari'
'Kolehmainen, Erkki'
_publ_section_title
;
 Bis(6-thioxo-1,6-dihydropurinium) tetrachlorozincate(II)
;
_journal_coeditor_code           OB3005
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m290
_journal_page_last               m292
_journal_paper_doi               10.1107/S0108270106019469
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          '(C5 H5 N4 S)2 [Zn Cl4]'
_chemical_formula_moiety         '2C5 H5 N4 S +, Cl4 Zn 2-'
_chemical_formula_sum            'C10 H10 Cl4 N8 S2 Zn'
_chemical_formula_weight         513.55
_chemical_name_systematic
;
Bis(6-thioxo-1,6-dihydropurinium) tetrachlorozincate(II)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 103.021(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.1397(5)
_cell_length_b                   6.8500(2)
_cell_length_c                   16.1142(5)
_cell_measurement_reflns_used    16093
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.283
_cell_measurement_theta_min      0.407
_cell_volume                     1843.27(10)
_computing_cell_refinement       'DENZO--SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'Collect (Bruker, 2004)'
_computing_data_reduction        DENZO--SMN
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR2002 (Burla, et al., 2003)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker Kappa APEX-II'
_diffrn_measurement_method       'φ and ω scans'
_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  0.0870
_diffrn_reflns_av_sigmaI/netI    0.0541
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            27322
_diffrn_reflns_theta_full        28.27
_diffrn_reflns_theta_max         28.27
_diffrn_reflns_theta_min         2.44
_exptl_absorpt_coefficient_mu    2.151
_exptl_absorpt_correction_T_max  0.7237
_exptl_absorpt_correction_T_min  0.6030
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'(MULABS in PLATON; Blessing, 1995; Spek, 2003)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.851
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1024
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.441
_refine_diff_density_min         -0.437
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     226
_refine_ls_number_reflns         4528
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0719
_refine_ls_R_factor_gt           0.0464
_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)+(0.0145P)²+3.7658P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0758
_refine_ls_wR_factor_ref         0.0836
_reflns_number_gt                3408
_reflns_number_total             4528
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            ob3005.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               2015451
_cod_database_fobs_code          2015451
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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
Zn Zn1 0.23591(2) 0.37451(6) 0.71080(3) 0.02477(11) Uani d . 1
Cl Cl1 0.17815(5) 0.39452(13) 0.57077(5) 0.02776(19) Uani d . 1
Cl Cl2 0.24644(5) 0.66457(13) 0.78154(5) 0.02746(19) Uani d . 1
Cl Cl3 0.35860(5) 0.23304(13) 0.72793(6) 0.0311(2) Uani d . 1
Cl Cl4 0.15987(5) 0.17928(13) 0.77642(6) 0.0285(2) Uani d . 1
S S6 0.59798(6) 0.22584(14) 0.88019(6) 0.0321(2) Uani d . 1
S S26 -0.00637(5) 0.77810(14) 0.62897(6) 0.0281(2) Uani d . 1
N N1 0.48598(16) 0.5044(4) 0.84906(18) 0.0265(7) Uani d . 1
H H1 0.4609 0.4281 0.8076 0.032 Uiso calc R 1
N N3 0.47771(16) 0.8030(4) 0.91970(19) 0.0258(6) Uani d . 1
N N7 0.66257(16) 0.5891(4) 1.01923(17) 0.0238(6) Uani d . 1
H H7 0.7004 0.4996 1.0277 0.029 Uiso calc R 1
N N9 0.59655(16) 0.8543(4) 1.03268(18) 0.0252(6) Uani d . 1
H H9 0.5839 0.9673 1.0521 0.030 Uiso calc R 1
N N21 0.14076(17) 0.8882(4) 0.61649(18) 0.0250(6) Uani d . 1
H H21 0.1491 0.9172 0.6710 0.030 Uiso calc R 1
N N23 0.19977(16) 0.8842(4) 0.49758(18) 0.0239(6) Uani d . 1
N N27 0.00114(16) 0.7200(4) 0.42570(17) 0.0223(6) Uani d . 1
H H27 -0.0473 0.6876 0.4306 0.027 Uiso calc R 1
N N29 0.10400(16) 0.7714(4) 0.37104(17) 0.0238(6) Uani d . 1
H H29 0.1344 0.7781 0.3338 0.029 Uiso calc R 1
C C2 0.4499(2) 0.6740(5) 0.8601(2) 0.0274(8) Uani d . 1
H H2 0.4004 0.7025 0.8218 0.033 Uiso calc R 1
C C4 0.55008(19) 0.7493(5) 0.9677(2) 0.0221(7) Uani d . 1
C C5 0.59081(18) 0.5804(5) 0.9593(2) 0.0207(7) Uani d . 1
C C6 0.5592(2) 0.4381(5) 0.8969(2) 0.0244(7) Uani d . 1
C C8 0.66458(19) 0.7552(5) 1.0615(2) 0.0263(8) Uani d . 1
H H8 0.7078 0.7978 1.1057 0.032 Uiso calc R 1
C C22 0.2022(2) 0.9159(5) 0.5783(2) 0.0262(8) Uani d . 1
H H22 0.2512 0.9621 0.6126 0.031 Uiso calc R 1
C C24 0.12665(19) 0.8192(5) 0.4555(2) 0.0208(7) Uani d . 1
C C25 0.06210(19) 0.7868(5) 0.4905(2) 0.0208(7) Uani d . 1
C C26 0.06553(19) 0.8180(5) 0.5776(2) 0.0216(7) Uani d . 1
C C28 0.0278(2) 0.7130(5) 0.3550(2) 0.0263(8) Uani d . 1
H H28 -0.0026 0.6724 0.3009 0.032 Uiso calc R 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 0.0016 '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'
S S 0.1246 0.1234 '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'
Zn Zn 0.2839 1.4301 '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_publ_flag
Cl1 Zn1 Cl3 109.44(4) y
Cl1 Zn1 Cl2 114.54(4) y
Cl3 Zn1 Cl2 110.12(3) y
Cl1 Zn1 Cl4 109.33(3) y
Cl3 Zn1 Cl4 107.60(4) y
Cl2 Zn1 Cl4 105.54(4) y
C2 N1 C6 126.2(3) ?
C2 N1 H1 116.9 ?
C6 N1 H1 116.9 ?
C2 N3 C4 111.7(3) ?
C8 N7 C5 108.2(3) ?
C8 N7 H7 125.9 ?
C5 N7 H7 125.9 ?
C8 N9 C4 108.1(3) ?
C8 N9 H9 126.0 ?
C4 N9 H9 126.0 ?
C22 N21 C26 125.8(3) ?
C22 N21 H21 117.1 ?
C26 N21 H21 117.1 ?
C22 N23 C24 111.7(3) ?
C28 N27 C25 108.3(3) ?
C28 N27 H27 125.8 ?
C25 N27 H27 125.8 ?
C28 N29 C24 108.1(3) ?
C28 N29 H29 125.9 ?
C24 N29 H29 125.9 ?
N3 C2 N1 125.1(3) ?
N3 C2 H2 117.4 ?
N1 C2 H2 117.4 ?
N3 C4 N9 126.4(3) ?
N3 C4 C5 126.3(3) ?
N9 C4 C5 107.3(3) ?
C4 C5 N7 106.6(3) ?
C4 C5 C6 121.8(3) ?
N7 C5 C6 131.5(3) ?
N1 C6 C5 108.8(3) ?
N1 C6 S6 123.0(3) ?
C5 C6 S6 128.2(3) ?
N7 C8 N9 109.7(3) ?
N7 C8 H8 125.1 ?
N9 C8 H8 125.1 ?
N23 C22 N21 125.2(3) ?
N23 C22 H22 117.4 ?
N21 C22 H22 117.4 ?
N23 C24 N29 126.7(3) ?
N23 C24 C25 126.0(3) ?
N29 C24 C25 107.3(3) ?
C24 C25 N27 106.7(3) ?
C24 C25 C26 122.0(3) ?
N27 C25 C26 131.3(3) ?
N21 C26 C25 109.2(3) ?
N21 C26 S26 123.6(3) ?
C25 C26 S26 127.2(3) ?
N27 C28 N29 109.6(3) ?
N27 C28 H28 125.2 ?
N29 C28 H28 125.2 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
Zn1 Cl1 2.2547(9) y
Zn1 Cl2 2.2776(10) y
Zn1 Cl3 2.2750(9) y
Zn1 Cl4 2.2861(9) y
S6 C6 1.647(4) y
S26 C26 1.655(3) y
N1 C2 1.347(4) ?
N1 C6 1.392(4) ?
N1 H1 0.8800 ?
N3 C2 1.313(4) ?
N3 C4 1.357(4) ?
C4 C5 1.374(4) y
C5 C6 1.418(5) ?
N7 C5 1.383(4) y
N7 C8 1.323(4) y
N7 H7 0.8800 ?
N9 C8 1.339(4) y
N9 C4 1.368(4) y
N9 H9 0.8800 ?
N21 C22 1.348(4) ?
N21 C26 1.386(4) ?
N21 H21 0.8800 ?
N23 C22 1.310(4) ?
N23 C24 1.359(4) ?
C24 C25 1.368(4) y
N27 C25 1.378(4) y
N27 C28 1.321(4) y
N27 H27 0.8800 ?
N29 C28 1.334(4) y
N29 C24 1.368(4) y
N29 H29 0.8800 ?
C2 H2 0.9500 ?
C8 H8 0.9500 ?
C22 H22 0.9500 ?
C25 C26 1.408(5) ?
C28 H28 0.9500 ?
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
N1 H1 Cl3 . 0.88 2.34 3.180(3) 158.7
N21 H21 Cl2 . 0.88 2.76 3.245(3) 116.2
N7 H7 N23 2_646 0.88 2.01 2.811(4) 150.9
N9 H9 N3 3_677 0.88 2.00 2.857(4) 162.9
N21 H21 Cl4 1_565 0.88 2.45 3.216(3) 145.8
N27 H27 Cl1 3_566 0.88 2.31 3.184(3) 174.4
N29 H29 Cl2 4_575 0.88 2.30 3.134(3) 158.6
C2 H2 Cl2 . 0.95 2.58 3.432(3) 148.6
C8 H8 Cl4 3_667 0.95 2.61 3.540(3) 164.8
C28 H28 S26 4_575 0.95 2.78 3.556(4) 139.8
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
C4 N3 C2 N1 2.6(5)
C6 N1 C2 N3 -1.5(6)
C2 N3 C4 N9 177.3(3)
C2 N3 C4 C5 -1.6(5)
C8 N9 C4 N3 -177.5(3)
C8 N9 C4 C5 1.6(4)
N3 C4 C5 N7 178.1(3)
N9 C4 C5 N7 -1.1(4)
N3 C4 C5 C6 -0.5(5)
N9 C4 C5 C6 -179.7(3)
C8 N7 C5 C4 0.1(4)
C8 N7 C5 C6 178.5(3)
C2 N1 C6 C5 -0.8(5)
C2 N1 C6 S6 178.6(3)
C4 C5 C6 N1 1.7(4)
N7 C5 C6 N1 -176.6(3)
C4 C5 C6 S6 -177.7(3)
N7 C5 C6 S6 4.1(6)
C5 N7 C8 N9 1.0(4)
C4 N9 C8 N7 -1.6(4)
C24 N23 C22 N21 0.2(5)
C26 N21 C22 N23 1.4(6)
C22 N23 C24 N29 -179.7(3)
C22 N23 C24 C25 -0.6(5)
C28 N29 C24 N23 179.6(3)
C28 N29 C24 C25 0.4(4)
N23 C24 C25 N27 -179.4(3)
N29 C24 C25 N27 -0.2(4)
N23 C24 C25 C26 -0.4(5)
N29 C24 C25 C26 178.7(3)
C28 N27 C25 C24 -0.1(4)
C28 N27 C25 C26 -178.9(4)
C22 N21 C26 C25 -2.2(5)
C22 N21 C26 S26 177.3(3)
C24 C25 C26 N21 1.7(4)
N27 C25 C26 N21 -179.7(3)
C24 C25 C26 S26 -177.8(3)
N27 C25 C26 S26 0.8(6)
C25 N27 C28 N29 0.3(4)
C24 N29 C28 N27 -0.5(4)
