#------------------------------------------------------------------------------
#$Date: 2020-03-14 08:02:46 +0200 (Sat, 14 Mar 2020) $
#$Revision: 249387 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/24/33/2243319.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_2243319
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_moiety         '[C8 H8 N2 S2]AgNO3'
_chemical_formula_sum            'C8 H8 Ag N3 O3 S2'
_chemical_formula_weight         366.16
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yac'
_space_group_name_H-M_alt        'P 1 2/n 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                 93.121(9)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   3.8995(3)
_cell_length_b                   6.3902(6)
_cell_length_c                   20.5741(18)
_cell_measurement_reflns_used    5000
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      25.81
_cell_measurement_theta_min      3.19
_cell_volume                     511.92(8)
_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 0.966
_diffrn_measured_fraction_theta_max 0.965
_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  0.0206
_diffrn_reflns_av_unetI/netI     0.0129
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            3795
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.810
_diffrn_reflns_theta_min         3.188
_exptl_absorpt_coefficient_mu    2.374
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.9318
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(MULABS; Spek, 2020)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.375
_exptl_crystal_description       needle
_exptl_crystal_F_000             360
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.314
_refine_diff_density_min         -0.267
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.145
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     79
_refine_ls_number_reflns         958
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.145
_refine_ls_R_factor_all          0.0170
_refine_ls_R_factor_gt           0.0156
_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)+(0.0200P)²+0.3928P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0406
_refine_ls_wR_factor_ref         0.0412
_reflns_number_gt                905
_reflns_number_total             958
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            lh5951sup1.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 2/n'
_cod_database_code               2243319
_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   0.415
_shelx_estimated_absorpt_t_max   0.797
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, 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
Ag Ag1 0.250000 0.73580(3) 0.750000 0.02211(9) Uani d 1 . .
S S1 -0.02263(12) 0.64417(7) 0.85176(2) 0.01302(12) Uani d 1 . .
O O1 0.6178(4) 1.0451(2) 0.79516(7) 0.0274(3) Uani d 1 . .
O O2 0.750000 1.3371(3) 0.750000 0.0262(5) Uani d 1 . .
N N1 0.4947(4) 0.2874(2) 0.97975(7) 0.0136(3) Uani d 1 . .
N N2 0.750000 1.1423(3) 0.750000 0.0157(5) Uani d 1 . .
C C1 0.3461(5) 0.4408(3) 0.94406(8) 0.0126(4) Uani d 1 . .
C C2 0.3516(5) 0.6499(3) 0.96379(8) 0.0124(4) Uani d 1 . .
C C3 0.1666(5) 0.3949(3) 0.87926(9) 0.0143(4) Uani d 1 . .
H H3A -0.012208 0.288847 0.883653 0.017 Uiso calc 1 . .
H H3B 0.330073 0.344062 0.848344 0.017 Uiso calc 1 . .
C C4 0.1801(5) 0.8040(3) 0.91737(9) 0.0148(4) Uani d 1 . .
H H4A 0.349176 0.899858 0.900192 0.018 Uiso calc 1 . .
H H4B 0.007436 0.886025 0.939085 0.018 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'
Ag Ag -0.8971 1.1015 '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'
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
S1 Ag1 S1 . 2_556 152.57(2) y
S1 Ag1 O1 . . 97.62(3) y
S1 Ag1 O1 2_556 . 103.30(4) ?
S1 Ag1 O1 . 2_556 103.30(3) y
S1 Ag1 O1 2_556 2_556 97.62(3) ?
O1 Ag1 O1 . 2_556 80.24(7) y
C3 S1 C4 . . 96.12(9) ?
C3 S1 Ag1 . . 106.45(6) ?
C4 S1 Ag1 . . 107.66(6) ?
N2 O1 Ag1 . . 110.82(11) ?
C1 N1 C2 . 3_667 114.66(16) ?
O2 N2 O1 . . 119.74(11) ?
O2 N2 O1 . 2_656 119.74(11) ?
O1 N2 O1 . 2_656 120.5(2) ?
N1 C1 C2 . . 122.85(17) ?
N1 C1 C3 . . 120.77(16) ?
C2 C1 C3 . . 116.38(16) ?
N1 C2 C1 3_667 . 122.49(17) ?
N1 C2 C4 3_667 . 121.21(16) ?
C1 C2 C4 . . 116.29(16) ?
C1 C3 S1 . . 105.36(12) ?
C1 C3 H3A . . 110.7 ?
S1 C3 H3A . . 110.7 ?
C1 C3 H3B . . 110.7 ?
S1 C3 H3B . . 110.7 ?
H3A C3 H3B . . 108.8 ?
C2 C4 S1 . . 105.17(12) ?
C2 C4 H4A . . 110.7 ?
S1 C4 H4A . . 110.7 ?
C2 C4 H4B . . 110.7 ?
S1 C4 H4B . . 110.7 ?
H4A C4 H4B . . 108.8 ?
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
Ag1 S1 . 2.4696(5) y
Ag1 S1 2_556 2.4696(5) ?
Ag1 O1 . 2.5849(15) y
Ag1 O1 2_556 2.5849(15) ?
S1 C3 . 1.8322(19) ?
S1 C4 . 1.8368(19) ?
O1 N2 . 1.2517(18) ?
O2 N2 . 1.245(3) ?
N1 C1 . 1.337(2) ?
N1 C2 3_667 1.339(2) ?
C1 C2 . 1.397(3) ?
C1 C3 . 1.501(2) ?
C2 C4 . 1.503(3) ?
C3 H3A . 0.9800 ?
C3 H3B . 0.9800 ?
C4 H4A . 0.9800 ?
C4 H4B . 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
C3 H3B O1 1_545 0.98 2.50 3.379(2) 150 yes
C4 H4A O1 . 0.98 2.62 3.475(2) 146 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
Ag1 O1 N2 O2 . . . . 136.46(5) ?
Ag1 O1 N2 O1 . . . 2_656 -43.54(5) ?
C2 N1 C1 C2 3_667 . . . 0.3(3) ?
C2 N1 C1 C3 3_667 . . . 179.41(16) ?
N1 C1 C2 N1 . . . 3_667 -0.3(3) ?
C3 C1 C2 N1 . . . 3_667 -179.47(16) ?
N1 C1 C2 C4 . . . . 178.56(17) ?
C3 C1 C2 C4 . . . . -0.6(2) ?
N1 C1 C3 S1 . . . . 175.73(14) ?
C2 C1 C3 S1 . . . . -5.08(19) ?
C4 S1 C3 C1 . . . . 7.26(14) ?
Ag1 S1 C3 C1 . . . . 117.73(11) ?
N1 C2 C4 S1 3_667 . . . -175.17(14) ?
C1 C2 C4 S1 . . . . 5.9(2) ?
C3 S1 C4 C2 . . . . -7.54(14) ?
Ag1 S1 C4 C2 . . . . -116.99(11) ?

_cod_database_fobs_code 2243319
