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#$Date: 2022-05-19 11:46:36 +0300 (Thu, 19 May 2022) $
#$Revision: 275541 $
#$URL: file:///home/coder/svn-repositories/cod/cif/8/10/53/8105300.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_8105300
loop_
_publ_author_name
'Jiang, Jin-Ke'
'Li, Xi-Xi'
'Wu, Hua'
'Dong, Xian-Wu'
'Jiang, Hui'
_publ_section_title
;
 Crystal structure of
 catena-poly[aqua(μ6-piperazine-1,4-bisethanesulfonato-κ6
 N:N&#x2032;:O:O&#x2032;:O&#x2032;&#x2032;:O&#x2032;&#x2032;&#x2032;)(\m2-pyrazinyl-\k2
 N:N′)disilver(I)sesquihydrate], C12H30Ag2N4O11S2
;
_journal_issue                   4
_journal_name_full
'Zeitschrift für Kristallographie - New Crystal Structures'
_journal_page_first              831
_journal_page_last               832
_journal_paper_doi               10.1515/ncrs-2020-0030
_journal_volume                  235
_journal_year                    2020
_chemical_formula_moiety         '2(C6 H12 Ag N2 O4 S), 3(H2 O)'
_chemical_formula_sum            'C12 H30 Ag2 N4 O11 S2'
_chemical_formula_weight         686.26
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_atom_sites_solution_hydrogens   difmap
_cell_angle_alpha                90
_cell_angle_beta                 93.119(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.2643(8)
_cell_length_b                   7.1481(4)
_cell_length_c                   26.2858(16)
_cell_measurement_reflns_used    13356
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      29.8930
_cell_measurement_theta_min      5.5390
_cell_volume                     2301.0(2)
_computing_cell_refinement       'CrysAlisPro 1.171.39.7e (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.7e (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.7e (Rigaku OD, 2015)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    SIR2004
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.926
_diffrn_measurement_device_type  'XtaLAB Pro: Kappa dual offset/far'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0212
_diffrn_reflns_av_unetI/netI     0.0104
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.926
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            22891
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.926
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         29.823
_diffrn_reflns_theta_min         4.879
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    1.943
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.77728
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.7e (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            coloress
_exptl_crystal_density_diffrn    1.981
_exptl_crystal_description       block
_exptl_crystal_F_000             1376
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.130
_refine_diff_density_max         0.295
_refine_diff_density_min         -0.655
_refine_diff_density_rms         0.084
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.102
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     201
_refine_ls_number_reflns         3056
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.102
_refine_ls_R_factor_all          0.0205
_refine_ls_R_factor_gt           0.0186
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0236P)²+2.0488P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0455
_refine_ls_wR_factor_ref         0.0462
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2866
_reflns_number_total             3056
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            suppl_ncrs-2020-0030_suppl.cif
_cod_data_source_block           shelx
_cod_original_sg_symbol_H-M      'I 2/a'
_cod_database_code               8105300
_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   0.759
_shelx_estimated_absorpt_t_max   0.786
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, z'
'-x+1/2, -y+1/2, -z+1/2'
'x, -y+1/2, z+1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ag1 Ag 0.74424(2) 0.14837(2) 0.13957(2) 0.03044(5) Uani 1 1 d . . . . .
S1 S 0.92925(3) 0.75737(5) 0.12405(2) 0.02419(8) Uani 1 1 d . . . . .
N1 N 0.80529(9) 0.33573(15) 0.20804(4) 0.0184(2) Uani 1 1 d . . . . .
O2 O 1.03937(9) 0.67953(17) 0.12808(5) 0.0323(2) Uani 1 1 d . . . . .
O1W O 0.61930(12) -0.1128(2) 0.15559(8) 0.0456(3) Uani 1 1 d . . . . .
O3 O 0.89452(12) 0.8042(2) 0.07213(5) 0.0467(3) Uani 1 1 d . . . . .
O1 O 0.91787(10) 0.91285(18) 0.15938(6) 0.0407(3) Uani 1 1 d . . . . .
N2 N 0.74687(11) 0.1798(2) 0.05292(5) 0.0291(3) Uani 1 1 d . . . . .
C3 C 0.86360(10) 0.2192(2) 0.24752(5) 0.0209(2) Uani 1 1 d . . . . .
C2 C 0.88267(11) 0.4795(2) 0.19126(6) 0.0252(3) Uani 1 1 d . . . . .
C6 C 0.65587(13) 0.1817(3) 0.02273(6) 0.0314(3) Uani 1 1 d . . . . .
C1 C 0.84017(12) 0.5771(2) 0.14293(6) 0.0282(3) Uani 1 1 d . . . . .
C4 C 0.71163(11) 0.42612(19) 0.23144(5) 0.0210(2) Uani 1 1 d . . . . .
C5 C 0.84104(13) 0.1822(2) 0.02983(6) 0.0311(3) Uani 1 1 d . . . . .
O2W O 0.58423(15) -0.3538(2) 0.07500(8) 0.0539(4) Uani 1 1 d . . . . .
O3W O 0.750000 0.6456(4) 0.000000 0.0622(7) Uani 1 2 d S T P . .
H1 H 0.8368(16) 0.489(3) 0.1163(8) 0.036(5) Uiso 1 1 d . . . . .
H8 H 0.6714(15) 0.499(3) 0.2059(8) 0.029(5) Uiso 1 1 d . . . . .
H4 H 0.9498(16) 0.423(3) 0.1862(8) 0.030(5) Uiso 1 1 d . . . . .
H2 H 0.772(2) 0.642(3) 0.1450(10) 0.051(7) Uiso 1 1 d . . . . .
H5 H 0.8924(15) 0.302(3) 0.2751(7) 0.022(4) Uiso 1 1 d . . . . .
H6 H 0.9247(16) 0.160(2) 0.2318(8) 0.023(4) Uiso 1 1 d . . . . .
H7 H 0.7383(15) 0.508(3) 0.2590(7) 0.026(4) Uiso 1 1 d . . . . .
H10 H 0.5876(19) 0.186(3) 0.0384(9) 0.042(6) Uiso 1 1 d . . . . .
H9 H 0.9054(19) 0.182(3) 0.0510(9) 0.043(6) Uiso 1 1 d . . . . .
H3 H 0.8949(17) 0.569(3) 0.2178(8) 0.036(5) Uiso 1 1 d . . . . .
H2A H 0.571(3) -0.455(6) 0.0867(14) 0.092(12) Uiso 1 1 d . . . . .
H2B H 0.632(4) -0.371(6) 0.050(2) 0.134(18) Uiso 1 1 d . . . . .
H3A H 0.789(2) 0.711(4) 0.0191(11) 0.063(8) Uiso 1 1 d . . . . .
H1A H 0.551(3) -0.058(5) 0.1607(13) 0.083(9) Uiso 1 1 d . . . . .
H1B H 0.615(2) -0.160(4) 0.1305(11) 0.045(8) Uiso 1 1 d . . . . .
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'
Ag Ag -0.8971 1.1015 '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_site_symmetry_1
_geom_angle_site_symmetry_3
N2 Ag1 N1 133.57(4) . .
N2 Ag1 O1W 106.66(6) . .
N1 Ag1 O1W 118.61(5) . .
O3 S1 O2 112.38(8) . .
O3 S1 O1 112.97(9) . .
O2 S1 O1 111.36(8) . .
O3 S1 C1 106.11(8) . .
O2 S1 C1 106.48(7) . .
O1 S1 C1 107.03(8) . .
C4 N1 C2 110.17(11) . .
C4 N1 C3 108.05(10) . .
C2 N1 C3 107.78(10) . .
C4 N1 Ag1 110.32(8) . .
C2 N1 Ag1 110.61(8) . .
C3 N1 Ag1 109.84(8) . .
Ag1 O1W H1A 106(2) . .
Ag1 O1W H1B 102(2) . .
H1A O1W H1B 107(3) . .
C5 N2 C6 116.52(13) . .
C5 N2 Ag1 120.87(10) . .
C6 N2 Ag1 122.41(10) . .
N1 C3 C4 111.14(10) . 7_655
N1 C3 H5 108.3(11) . .
C4 C3 H5 110.3(11) 7_655 .
N1 C3 H6 107.6(12) . .
C4 C3 H6 110.7(11) 7_655 .
H5 C3 H6 108.8(15) . .
N1 C2 C1 111.82(11) . .
N1 C2 H4 109.2(13) . .
C1 C2 H4 110.1(12) . .
N1 C2 H3 108.9(13) . .
C1 C2 H3 109.9(13) . .
H4 C2 H3 106.8(17) . .
N2 C6 C5 121.76(14) . 2_655
N2 C6 H10 118.0(14) . .
C5 C6 H10 120.2(14) 2_655 .
C2 C1 S1 112.27(10) . .
C2 C1 H1 108.4(13) . .
S1 C1 H1 106.2(13) . .
C2 C1 H2 115.8(15) . .
S1 C1 H2 102.6(14) . .
H1 C1 H2 111(2) . .
N1 C4 C3 110.76(11) . 7_655
N1 C4 H8 109.0(11) . .
C3 C4 H8 109.0(11) 7_655 .
N1 C4 H7 109.5(11) . .
C3 C4 H7 109.0(11) 7_655 .
H8 C4 H7 109.6(16) . .
N2 C5 C6 121.70(14) . 2_655
N2 C5 H9 116.8(15) . .
C6 C5 H9 121.5(15) 2_655 .
H2A O2W H2B 108(4) . .
H3A O3W H3A 110(4) . 2_655
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ag1 N2 2.2907(13) .
Ag1 N1 2.3339(11) .
Ag1 O1W 2.4659(15) .
S1 O3 1.4467(13) .
S1 O2 1.4593(12) .
S1 O1 1.4599(13) .
S1 C1 1.7777(15) .
N1 C4 1.4806(16) .
N1 C2 1.4820(17) .
N1 C3 1.4839(17) .
O1W H1A 0.94(3) .
O1W H1B 0.74(3) .
N2 C5 1.334(2) .
N2 C6 1.334(2) .
C3 C4 1.5136(19) 7_655
C3 H5 0.988(19) .
C3 H6 0.973(19) .
C2 C1 1.517(2) .
C2 H4 0.93(2) .
C2 H3 0.95(2) .
C6 C5 1.384(2) 2_655
C6 H10 0.95(2) .
C1 H1 0.94(2) .
C1 H2 0.96(3) .
C4 H8 0.96(2) .
C4 H7 0.973(19) .
C5 H9 0.94(2) .
O2W H2A 0.81(4) .
O2W H2B 0.91(5) .
O3W H3A 0.82(3) .
O3W H3A 0.82(3) 2_655
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
C1 H2 O1W 0.96(3) 2.59(3) 3.530(2) 166(2) 1_565 yes
C3 H6 O1 0.973(19) 2.594(19) 3.2822(19) 127.9(14) 1_545 yes
C6 H10 O2 0.95(2) 2.64(2) 3.335(2) 129.9(18) 6_565 yes
C6 H10 O3 0.95(2) 2.57(2) 3.525(2) 175(2) 6_565 yes
C5 H9 O2W 0.94(2) 2.56(2) 3.380(2) 145.6(19) 6_655 yes
O2W H2A O2 0.81(4) 1.99(4) 2.785(2) 169(4) 6 yes
O2W H2B O3W 0.91(5) 2.02(5) 2.908(2) 168(4) 1_545 yes
O3W H3A O3 0.82(3) 1.97(3) 2.7671(18) 165(3) . yes
O1W H1A O1 0.94(3) 1.94(4) 2.8604(19) 168(3) 6_565 yes
O1W H1B O2W 0.74(3) 2.03(3) 2.746(3) 163(3) . yes
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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
C4 N1 C3 C4 58.29(15) . . . 7_655
C2 N1 C3 C4 177.33(12) . . . 7_655
Ag1 N1 C3 C4 -62.09(12) . . . 7_655
C4 N1 C2 C1 -75.38(15) . . . .
C3 N1 C2 C1 166.95(13) . . . .
Ag1 N1 C2 C1 46.86(15) . . . .
C5 N2 C6 C5 1.3(2) . . . 2_655
Ag1 N2 C6 C5 -173.53(13) . . . 2_655
N1 C2 C1 S1 177.23(11) . . . .
O3 S1 C1 C2 165.75(13) . . . .
O2 S1 C1 C2 45.83(14) . . . .
O1 S1 C1 C2 -73.36(14) . . . .
C2 N1 C4 C3 -175.57(11) . . . 7_655
C3 N1 C4 C3 -58.05(15) . . . 7_655
Ag1 N1 C4 C3 62.02(11) . . . 7_655
C6 N2 C5 C6 -1.7(2) . . . 2_655
Ag1 N2 C5 C6 173.22(13) . . . 2_655
