#------------------------------------------------------------------------------
#$Date: 2017-03-02 07:38:46 +0200 (Thu, 02 Mar 2017) $
#$Revision: 192757 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/24/20/2242044.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_2242044
loop_
_publ_author_name
'Assoumatine, Tokouré'
'Stoeckli-Evans, Helen'
_publ_section_title
;
 Silver(I) nitrate complexes of three tetrakis-thioether-substituted
 pyrazine ligands: metal--organic chain, network and framework structures
;
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              434
_journal_page_last               440
_journal_paper_doi               10.1107/S2056989017002791
_journal_volume                  73
_journal_year                    2017
_chemical_formula_iupac          '[Ag3 (N O3)3 (C28 H24 N6 S4)]'
_chemical_formula_moiety         'C28 H24 Ag3 N9 O9 S4'
_chemical_formula_sum            'C28 H24 Ag3 N9 O9 S4'
_chemical_formula_weight         1082.41
_chemical_name_systematic
Poly[[trinitrato{μ₆-2,3,5,6-tetrakis[(pyridin-2-ylsulfanyl)methyl]pyrazine}trisilver(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'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                90
_cell_angle_beta                 96.607(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.6319(9)
_cell_length_b                   16.2211(10)
_cell_length_c                   15.7201(11)
_cell_measurement_reflns_used    5000
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      25.87
_cell_measurement_theta_min      1.96
_cell_volume                     3453.0(4)
_computing_cell_refinement
;
CELL in IPDS-I (Stoe & Cie, 1998)
;
_computing_data_collection
;
EXPOSE in IPDS-I (Stoe & Cie, 1998)
;
_computing_data_reduction
;
INTEGRATE in IPDS-I (Stoe & Cie, 1998)
;
_computing_molecular_graphics
;
Mercury (Macrae et al.,  2008)
;
_computing_publication_material
;
SHELXL2014/6 (Sheldrick, 2015), PLATON (Spek, 2009) and
publcif (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2014/6 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.991
_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  0.0720
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            13264
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.875
_diffrn_reflns_theta_min         1.959
_exptl_absorpt_coefficient_mu    1.994
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.9492
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(MULABS; Spek, 2009)
;
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    2.082
_exptl_crystal_description       needle
_exptl_crystal_F_000             2128
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.433
_refine_diff_density_min         -0.438
_refine_ls_extinction_coef       0.00014(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.755
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     242
_refine_ls_number_reflns         3311
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.755
_refine_ls_R_factor_all          0.0735
_refine_ls_R_factor_gt           0.0303
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0179P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0468
_refine_ls_wR_factor_ref         0.0518
_reflns_number_gt                1936
_reflns_number_total             3311
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            wm5369sup1.cif
_cod_data_source_block           III
_cod_database_code               2242044
_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.
;
_shelxl_version_number           2014/6
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
Ag Ag1 0.01942(2) 0.37808(2) -0.08024(3) 0.04096(12) Uani d 1
Ag Ag2 0.5000 -0.03325(3) 0.2500 0.05015(18) Uani d 1
S S1 0.09150(7) 0.43818(6) 0.08153(8) 0.0309(3) Uani d 1
S S2 0.37324(7) 0.12904(6) 0.20654(7) 0.0293(3) Uani d 1
O O11 0.0033(3) 0.2151(3) -0.1140(3) 0.0993(17) Uani d 1
O O12 0.0505(3) 0.1241(2) -0.0186(3) 0.0881(13) Uani d 1
O O13 -0.0038(3) 0.2406(3) 0.0181(3) 0.0871(14) Uani d 1
O O21 0.5000 -0.1915(3) 0.2500 0.082(2) Uani d 1
O O22 0.5755(3) -0.3025(3) 0.2419(3) 0.0890(15) Uani d 1
N N1 0.1890(2) 0.31443(19) -0.0280(2) 0.0228(8) Uani d 1
N N2 0.1418(2) 0.59202(19) 0.0729(2) 0.0278(8) Uani d 1
N N3 0.3466(2) -0.0278(2) 0.1875(2) 0.0277(8) Uani d 1
N N11 0.0173(3) 0.1915(3) -0.0375(4) 0.0643(14) Uani d 1
N N21 0.5000 -0.2669(3) 0.2500 0.0365(13) Uani d 1
C C1 0.2093(3) 0.2984(2) 0.0553(3) 0.0232(9) Uani d 1
C C2 0.2715(3) 0.2341(2) 0.0833(3) 0.0217(9) Uani d 1
C C3 0.1631(3) 0.3497(2) 0.1204(3) 0.0306(11) Uani d 1
H H3A 0.2161 0.3689 0.1632 0.037 Uiso calc 1
H H3B 0.1204 0.3136 0.1499 0.037 Uiso calc 1
C C4 0.1816(3) 0.5165(2) 0.0793(3) 0.0295(10) Uani d 1
C C5 0.2821(3) 0.5034(3) 0.0844(3) 0.0517(14) Uani d 1
H H5 0.3082 0.4497 0.0867 0.062 Uiso calc 1
C C6 0.3433(3) 0.5714(3) 0.0861(4) 0.0617(16) Uani d 1
H H6 0.4122 0.5645 0.0912 0.074 Uiso calc 1
C C7 0.3033(3) 0.6488(3) 0.0803(3) 0.0518(14) Uani d 1
H H7 0.3442 0.6956 0.0814 0.062 Uiso calc 1
C C8 0.2039(3) 0.6569(3) 0.0731(3) 0.0407(12) Uani d 1
H H8 0.1768 0.7102 0.0679 0.049 Uiso calc 1
C C9 0.2962(3) 0.2171(2) 0.1786(3) 0.0279(10) Uani d 1
H H9A 0.2341 0.2099 0.2036 0.034 Uiso calc 1
H H9B 0.3290 0.2660 0.2053 0.034 Uiso calc 1
C C11 0.2968(3) -0.0982(3) 0.1679(3) 0.0406(12) Uani d 1
H H11 0.3317 -0.1483 0.1722 0.049 Uiso calc 1
C C12 0.1982(4) -0.0998(3) 0.1421(3) 0.0568(15) Uani d 1
H H12 0.1653 -0.1501 0.1296 0.068 Uiso calc 1
C C13 0.1476(4) -0.0263(3) 0.1347(4) 0.0654(17) Uani d 1
H H13 0.0792 -0.0260 0.1174 0.079 Uiso calc 1
C C14 0.1966(3) 0.0468(3) 0.1524(3) 0.0492(13) Uani d 1
H H14 0.1631 0.0976 0.1466 0.059 Uiso calc 1
C C15 0.2959(3) 0.0433(2) 0.1789(3) 0.0276(10) Uani 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 0.0016 '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
N1 Ag1 N2 . 5_565 155.31(11) yes
S1 Ag1 S2 . 7_555 122.71(3) yes
S1 Ag1 N1 . . 68.98(7) yes
S1 Ag1 N2 . 5_565 96.92(8) yes
S2 Ag1 N1 7_555 . 70.29(7) yes
S2 Ag1 N2 7_555 5_565 133.03(8) yes
S1 Ag1 O11 . . 122.18(10) yes
S1 Ag1 O13 . . 79.78(10) yes
S2 Ag1 O11 7_555 . 81.18(10) yes
S2 Ag1 O13 7_555 . 120.26(10) yes
O11 Ag1 N1 . . 73.76(11) yes
O11 Ag1 N2 . 5_565 99.33(12) yes
O13 Ag1 N1 . . 69.73(11) yes
O13 Ag1 N2 . 5_565 88.28(12) yes
O11 Ag1 O13 . . 45.99(14) yes
N3 Ag2 N3 . 2_655 175.41(12) yes
O21 Ag2 N3 . . 92.30(9) yes
O21 Ag2 N3 . 2_655 92.30(9) ?
C4 S1 C3 . . 103.19(19) ?
C4 S1 Ag1 . . 113.84(14) ?
C3 S1 Ag1 . . 98.68(14) ?
C15 S2 C9 . . 104.50(18) ?
C15 S2 Ag1 . 7 98.56(13) ?
C9 S2 Ag1 . 7 102.31(13) ?
N21 O21 Ag2 . . 180.0 ?
C2 N1 C1 7 . 118.2(3) ?
C2 N1 Ag1 7 . 116.4(3) ?
C1 N1 Ag1 . . 118.0(2) ?
C4 N2 C8 . . 117.6(3) ?
C4 N2 Ag1 . 5_565 125.4(2) ?
C8 N2 Ag1 . 5_565 116.4(3) ?
C15 N3 C11 . . 117.8(3) ?
C15 N3 Ag2 . . 121.9(3) ?
C11 N3 Ag2 . . 119.7(3) ?
O12 N11 O13 . . 121.3(6) ?
O12 N11 O11 . . 121.5(6) ?
O13 N11 O11 . . 117.2(6) ?
O22 N21 O22 . 2_655 122.4(6) ?
O22 N21 O21 . . 118.8(3) ?
O22 N21 O21 2_655 . 118.8(3) ?
N1 C1 C2 . . 120.7(3) ?
N1 C1 C3 . . 120.1(3) ?
C2 C1 C3 . . 119.2(4) ?
N1 C2 C1 7 . 121.1(4) ?
N1 C2 C9 7 . 118.4(3) ?
C1 C2 C9 . . 120.4(4) ?
C1 C3 S1 . . 117.4(3) ?
C1 C3 H3A . . 107.9 ?
S1 C3 H3A . . 107.9 ?
C1 C3 H3B . . 107.9 ?
S1 C3 H3B . . 107.9 ?
H3A C3 H3B . . 107.2 ?
N2 C4 C5 . . 122.4(4) ?
N2 C4 S1 . . 112.5(3) ?
C5 C4 S1 . . 125.1(3) ?
C4 C5 C6 . . 118.2(4) ?
C4 C5 H5 . . 120.9 ?
C6 C5 H5 . . 120.9 ?
C7 C6 C5 . . 119.7(4) ?
C7 C6 H6 . . 120.1 ?
C5 C6 H6 . . 120.1 ?
C8 C7 C6 . . 118.8(4) ?
C8 C7 H7 . . 120.6 ?
C6 C7 H7 . . 120.6 ?
N2 C8 C7 . . 123.1(4) ?
N2 C8 H8 . . 118.4 ?
C7 C8 H8 . . 118.4 ?
C2 C9 S2 . . 116.1(3) ?
C2 C9 H9A . . 108.3 ?
S2 C9 H9A . . 108.3 ?
C2 C9 H9B . . 108.3 ?
S2 C9 H9B . . 108.3 ?
H9A C9 H9B . . 107.4 ?
N3 C11 C12 . . 122.7(4) ?
N3 C11 H11 . . 118.6 ?
C12 C11 H11 . . 118.6 ?
C11 C12 C13 . . 118.5(4) ?
C11 C12 H12 . . 120.8 ?
C13 C12 H12 . . 120.8 ?
C14 C13 C12 . . 120.3(4) ?
C14 C13 H13 . . 119.9 ?
C12 C13 H13 . . 119.9 ?
C15 C14 C13 . . 117.7(4) ?
C15 C14 H14 . . 121.1 ?
C13 C14 H14 . . 121.1 ?
N3 C15 C14 . . 123.0(4) ?
N3 C15 S2 . . 111.5(3) ?
C14 C15 S2 . . 125.5(3) ?
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 N1 . 2.578(3) yes
Ag1 N2 5_565 2.267(3) yes
Ag1 S1 . 2.7943(13) yes
Ag1 S2 7_555 2.6010(11) yes
Ag1 O11 . 2.700(5) yes
Ag1 O13 . 2.752(5) yes
Ag2 N3 . 2.208(3) yes
Ag2 N3 2_655 2.208(3) ?
Ag2 O21 . 2.567(5) yes
S1 C4 . 1.770(4) ?
S1 C3 . 1.802(4) ?
S2 C15 . 1.769(4) ?
S2 C9 . 1.798(4) ?
S2 Ag1 7 2.6011(11) ?
O11 N11 . 1.255(6) ?
O12 N11 . 1.208(5) ?
O13 N11 . 1.239(6) ?
O21 N21 . 1.223(6) ?
O22 N21 . 1.200(4) ?
N1 C2 7 1.331(5) ?
N1 C1 . 1.332(5) ?
N2 C4 . 1.339(5) ?
N2 C8 . 1.351(5) ?
N2 Ag1 5_565 2.266(3) ?
N3 C15 . 1.343(5) ?
N3 C11 . 1.345(5) ?
N21 O22 2_655 1.200(4) ?
C1 C2 . 1.384(5) ?
C1 C3 . 1.512(5) ?
C2 N1 7 1.331(5) ?
C2 C9 . 1.523(5) ?
C3 H3A . 0.9800 ?
C3 H3B . 0.9800 ?
C4 C5 . 1.379(6) ?
C5 C6 . 1.382(6) ?
C5 H5 . 0.9400 ?
C6 C7 . 1.368(6) ?
C6 H6 . 0.9400 ?
C7 C8 . 1.353(6) ?
C7 H7 . 0.9400 ?
C8 H8 . 0.9400 ?
C9 H9A . 0.9800 ?
C9 H9B . 0.9800 ?
C11 C12 . 1.360(6) ?
C11 H11 . 0.9400 ?
C12 C13 . 1.377(6) ?
C12 H12 . 0.9400 ?
C13 C14 . 1.374(6) ?
C13 H13 . 0.9400 ?
C14 C15 . 1.372(6) ?
C14 H14 . 0.9400 ?
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
C11 H11 O21 . 0.94 2.57 3.287(5) 133
C3 H3B O21 3_455 0.98 2.40 3.253(4) 145
C3 H3B O22 3_455 0.98 2.49 3.420(6) 158
C7 H7 O13 3_555 0.94 2.51 3.268(6) 138
C9 H9A O22 3_455 0.98 2.32 3.291(6) 171
C12 H12 O11 5_555 0.94 2.51 3.310(7) 142
C14 H14 O22 3_455 0.94 2.59 3.349(7) 138
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_4
_geom_torsion
C2 N1 C1 C2 7 . 1.2(6)
Ag1 N1 C1 C2 . . 150.0(3)
C2 N1 C1 C3 7 . -177.7(3)
Ag1 N1 C1 C3 . . -28.9(4)
N1 C1 C2 N1 . 7 -1.3(6)
C3 C1 C2 N1 . 7 177.7(3)
N1 C1 C2 C9 . . 178.7(3)
C3 C1 C2 C9 . . -2.3(5)
N1 C1 C3 S1 . . -6.3(5)
C2 C1 C3 S1 . . 174.7(3)
C4 S1 C3 C1 . . -85.5(3)
Ag1 S1 C3 C1 . . 31.6(3)
C8 N2 C4 C5 . . -1.0(6)
Ag1 N2 C4 C5 5_565 . -172.2(3)
C8 N2 C4 S1 . . 178.2(3)
Ag1 N2 C4 S1 5_565 . 7.1(4)
C3 S1 C4 N2 . . -164.1(3)
Ag1 S1 C4 N2 . . 90.0(3)
C3 S1 C4 C5 . . 15.1(5)
Ag1 S1 C4 C5 . . -90.8(4)
N2 C4 C5 C6 . . 2.3(7)
S1 C4 C5 C6 . . -176.8(4)
C4 C5 C6 C7 . . -1.7(8)
C5 C6 C7 C8 . . 0.0(8)
C4 N2 C8 C7 . . -0.8(6)
Ag1 N2 C8 C7 5_565 . 171.1(4)
C6 C7 C8 N2 . . 1.4(8)
N1 C2 C9 S2 7 . -2.7(5)
C1 C2 C9 S2 . . 177.3(3)
C15 S2 C9 C2 . . -72.0(3)
Ag1 S2 C9 C2 7 . 30.3(3)
C15 N3 C11 C12 . . -1.6(6)
Ag2 N3 C11 C12 . . 169.3(4)
N3 C11 C12 C13 . . 0.9(7)
C11 C12 C13 C14 . . 0.6(8)
C12 C13 C14 C15 . . -1.2(8)
C11 N3 C15 C14 . . 0.9(6)
Ag2 N3 C15 C14 . . -169.7(3)
C11 N3 C15 S2 . . -179.5(3)
Ag2 N3 C15 S2 . . 9.8(4)
C13 C14 C15 N3 . . 0.4(7)
C13 C14 C15 S2 . . -179.1(4)
C9 S2 C15 N3 . . 173.2(3)
Ag1 S2 C15 N3 7 . 68.1(3)
C9 S2 C15 C14 . . -7.2(4)
Ag1 S2 C15 C14 7 . -112.4(4)

_cod_database_fobs_code 2242044
