#------------------------------------------------------------------------------
#$Date: 2020-03-14 08:02:46 +0200 (Sat, 14 Mar 2020) $
#$Revision: 249387 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/24/33/2243318.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_2243318
loop_
_publ_author_name
'Assoumatine, Tokouré'
'Stoeckli-Evans, Helen'
_publ_section_title
;
 Silver(I) nitrate two-dimensional coordination polymers of two new
 pyrazinethiophane ligands:
 5,7-dihydro-1H,3H-dithieno[3,4-b:3',4'-e]pyrazine
 and
 3,4,8,10,11,13-hexahydro-1H,6H-bis([1,4]dithiocino)[6,7-b:6',7'-e]pyrazine
;
_journal_coeditor_code           LH5951
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              539
_journal_page_last               546
_journal_paper_doi               10.1107/S205698902000362X
_journal_volume                  76
_journal_year                    2020
_chemical_formula_iupac          '[Ag (N O3) (C12 H16 N2 S4)]'
_chemical_formula_moiety         'C12 H16 N2 S4'
_chemical_formula_sum            'C12 H16 N2 S4'
_chemical_formula_weight         316.51
_chemical_name_systematic
Poly[[μ₃3,4,8,10,11,13-hexahydro-1H,6H-bis([1,4]dithiocino)[6,7-b;6',7'-e]pyrazine-κ³S:S':S''](nitrato-κO)silver(I)]
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 94.470(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.1618(18)
_cell_length_b                   7.0585(5)
_cell_length_c                   9.5057(7)
_cell_measurement_reflns_used    5000
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      25.90
_cell_measurement_theta_min      3.04
_cell_volume                     1415.55(19)
_computing_cell_refinement
;
CELL in IPDS1 (Stoe & Cie, 1998)
;
_computing_data_collection
;
EXPOSE in IPDS1 (Stoe & Cie, 1998)
;
_computing_data_reduction
;
INTEGRATE in IPDS1 (Stoe & Cie, 1998)
;
_computing_molecular_graphics
;
Mercury (Macrae et al.,  2020)
;
_computing_publication_material
;
SHELXL-2018/3 (Sheldrick, 2015), PLATON (Spek, 2020) and
publcif (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL-2018/3 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS-97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      223(2)
_diffrn_detector                 'image plate'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device       '1 circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS 1'
_diffrn_measurement_method       'φ rotation'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0292
_diffrn_reflns_av_unetI/netI     0.0221
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_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            5086
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.903
_diffrn_reflns_theta_min         3.043
_exptl_absorpt_coefficient_mu    0.654
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            plate
_exptl_crystal_density_diffrn    1.485
_exptl_crystal_description       colourless
_exptl_crystal_F_000             664
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.312
_refine_diff_density_min         -0.247
_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     82
_refine_ls_number_reflns         1367
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0318
_refine_ls_R_factor_gt           0.0264
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0427P)²+0.4610P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0689
_refine_ls_wR_factor_ref         0.0706
_reflns_number_gt                1174
_reflns_number_total             1367
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            lh5951sup1.cif
_cod_data_source_block           L2
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2243318
_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.
;
_shelx_estimated_absorpt_t_min   0.780
_shelx_estimated_absorpt_t_max   0.937
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'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_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
S S1 0.90795(2) 0.54315(6) 0.52645(5) 0.03312(15) Uani d 1 . .
S S2 0.89795(2) 0.01187(6) 0.34452(5) 0.03987(16) Uani d 1 . .
N N1 0.75497(6) 0.42931(19) 0.55990(14) 0.0268(3) Uani d 1 . .
C C1 0.78592(7) 0.1989(2) 0.39521(15) 0.0253(3) Uani d 1 . .
C C2 0.79056(6) 0.3798(2) 0.45558(15) 0.0246(3) Uani d 1 . .
C C3 0.83585(8) 0.5281(2) 0.41003(18) 0.0303(4) Uani d 1 . .
H H3A 0.814637 0.651638 0.407231 0.036 Uiso calc 1 . .
H H3B 0.847038 0.498872 0.314291 0.036 Uiso calc 1 . .
C C4 0.93325(8) 0.2996(2) 0.54130(17) 0.0323(4) Uani d 1 . .
H H4A 0.970847 0.293157 0.608187 0.039 Uiso calc 1 . .
H H4B 0.899694 0.225955 0.581154 0.039 Uiso calc 1 . .
C C5 0.94907(7) 0.2061(2) 0.40278(18) 0.0319(4) Uani d 1 . .
H H5A 0.992794 0.159497 0.414165 0.038 Uiso calc 1 . .
H H5B 0.947061 0.302840 0.328648 0.038 Uiso calc 1 . .
C C6 0.82558(7) 0.1326(3) 0.27995(17) 0.0332(4) Uani d 1 . .
H H6A 0.836729 0.242364 0.223784 0.040 Uiso calc 1 . .
H H6B 0.800162 0.046620 0.217500 0.040 Uiso calc 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'
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
C4 S1 C3 . . 102.85(8) ?
C5 S2 C6 . . 102.50(8) ?
C2 N1 C1 . 7_656 118.24(14) ?
N1 C1 C2 7_656 . 120.67(14) ?
N1 C1 C6 7_656 . 115.54(14) ?
C2 C1 C6 . . 123.79(13) ?
N1 C2 C1 . . 121.09(13) ?
N1 C2 C3 . . 116.07(14) ?
C1 C2 C3 . . 122.83(14) ?
C2 C3 S1 . . 112.86(11) ?
C2 C3 H3A . . 109.0 ?
S1 C3 H3A . . 109.0 ?
C2 C3 H3B . . 109.0 ?
S1 C3 H3B . . 109.0 ?
H3A C3 H3B . . 107.8 ?
C5 C4 S1 . . 115.28(11) ?
C5 C4 H4A . . 108.5 ?
S1 C4 H4A . . 108.5 ?
C5 C4 H4B . . 108.5 ?
S1 C4 H4B . . 108.5 ?
H4A C4 H4B . . 107.5 ?
C4 C5 S2 . . 115.13(11) ?
C4 C5 H5A . . 108.5 ?
S2 C5 H5A . . 108.5 ?
C4 C5 H5B . . 108.5 ?
S2 C5 H5B . . 108.5 ?
H5A C5 H5B . . 107.5 ?
C1 C6 S2 . . 113.75(11) ?
C1 C6 H6A . . 108.8 ?
S2 C6 H6A . . 108.8 ?
C1 C6 H6B . . 108.8 ?
S2 C6 H6B . . 108.8 ?
H6A C6 H6B . . 107.7 ?
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
S1 C4 . 1.8025(17) ?
S1 C3 . 1.8168(17) ?
S2 C5 . 1.8062(16) ?
S2 C6 . 1.8171(18) ?
N1 C2 . 1.338(2) ?
N1 C1 7_656 1.3443(19) ?
C1 C2 . 1.401(2) ?
C1 C6 . 1.506(2) ?
C2 C3 . 1.506(2) ?
C3 H3A . 0.9800 ?
C3 H3B . 0.9800 ?
C4 C5 . 1.533(2) ?
C4 H4A . 0.9800 ?
C4 H4B . 0.9800 ?
C5 H5A . 0.9800 ?
C5 H5B . 0.9800 ?
C6 H6A . 0.9800 ?
C6 H6B . 0.9800 ?
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
C4 H4B S2 6_556 0.98 3.02 3.7465(17) 132 no
C5 H5A S1 5_766 0.98 2.99 3.5248(16) 115 no
C6 H6A S1 6_565 0.98 2.92 3.8389(18) 157 no
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_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
C1 N1 C2 C1 7_656 . . . -0.5(2) ?
C1 N1 C2 C3 7_656 . . . -179.60(14) ?
N1 C1 C2 N1 7_656 . . . 0.6(2) ?
C6 C1 C2 N1 . . . . -178.56(14) ?
N1 C1 C2 C3 7_656 . . . 179.55(14) ?
C6 C1 C2 C3 . . . . 0.4(2) ?
N1 C2 C3 S1 . . . . 80.06(15) ?
C1 C2 C3 S1 . . . . -98.99(15) ?
C4 S1 C3 C2 . . . . 49.78(13) ?
C3 S1 C4 C5 . . . . 61.99(13) ?
S1 C4 C5 S2 . . . . -115.40(11) ?
C6 S2 C5 C4 . . . . 74.34(13) ?
N1 C1 C6 S2 7_656 . . . -86.52(14) ?
C2 C1 C6 S2 . . . . 92.63(17) ?
C5 S2 C6 C1 . . . . -77.62(13) ?

_cod_database_fobs_code 2243318
