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#$Date: 2022-10-26 11:45:26 +0300 (Wed, 26 Oct 2022) $
#$Revision: 278803 $
#$URL: file:///home/coder/svn-repositories/cod/cif/8/10/59/8105978.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_8105978
loop_
_publ_author_name
'Jiang, Jin-Ke'
'Li, Gang-Mei'
'Sun, Jian-Nan'
'Ju, Ge-Shuang'
'Du, Jing-Jie'
'Jin, Xin'
_publ_section_title
;
 Crystal structure of
 poly[(μ2-4-amino-1,5-naphthalenedisulfonato-κ4O,N:O′,
 N&#x2032;)bis(\m2-hexamethylenetetramino-\k2N;N&#x2032;)silver(I)],
 {C22H30Ag2N9O6S2}n
;
_journal_issue                   6
_journal_name_full
'Zeitschrift für Kristallographie - New Crystal Structures'
_journal_page_first              1201
_journal_page_last               1202
_journal_paper_doi               10.1515/ncrs-2019-0326
_journal_volume                  234
_journal_year                    2019
_chemical_formula_moiety         'C22 H30 Ag2 N9 O6 S2'
_chemical_formula_sum            'C22 H30 Ag2 N9 O6 S2'
_chemical_formula_weight         796.41
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2017/1
_cell_angle_alpha                90
_cell_angle_beta                 109.766(12)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.4629(10)
_cell_length_b                   10.9785(8)
_cell_length_c                   12.3483(15)
_cell_measurement_reflns_used    4297
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.7200
_cell_measurement_theta_min      5.2900
_cell_volume                     1334.8(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_molecular_graphics    Diamond
_computing_publication_material  publCIF
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.883
_diffrn_measurement_device       'four-circle diffractometer'
_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  0.0238
_diffrn_reflns_av_unetI/netI     0.0221
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.883
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            12927
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.883
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         29.736
_diffrn_reflns_theta_min         4.859
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    1.682
_exptl_absorpt_correction_T_max  0.811
_exptl_absorpt_correction_T_min  0.719
_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            colourless
_exptl_crystal_density_diffrn    1.981
_exptl_crystal_description       block
_exptl_crystal_F_000             798
_exptl_crystal_size_max          0.210
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.130
_refine_diff_density_max         1.085
_refine_diff_density_min         -0.764
_refine_diff_density_rms         0.117
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.210
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     190
_refine_ls_number_reflns         3348
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.210
_refine_ls_R_factor_all          0.0759
_refine_ls_R_factor_gt           0.0662
_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)+9.9098P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1325
_refine_ls_wR_factor_ref         0.1356
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2804
_reflns_number_total             3348
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            suppl_ncrs-2019-0326_suppl.cif
_cod_data_source_block           shelx
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               8105978
_shelx_shelxl_version_number     2017/1
_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   0.719
_shelx_estimated_absorpt_t_max   0.811
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'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
C1 C 0.6023(7) 0.4133(7) 0.6338(5) 0.0497(18) Uani 1 1 d . . . . .
C2 C 0.5401(9) 0.4552(9) 0.7090(6) 0.063(2) Uani 1 1 d . . . . .
H1 H 0.570401 0.426636 0.784343 0.076 Uiso 1 1 calc R U . . .
C3 C 0.4350(8) 0.5378(8) 0.6765(6) 0.056(2) Uani 1 1 d . . . . .
H2 H 0.397174 0.564217 0.730513 0.068 Uiso 1 1 calc R U . . .
C4 C 0.3846(6) 0.5822(7) 0.5658(5) 0.0455(16) Uani 1 1 d . . . . .
C5 C 0.4445(6) 0.5428(6) 0.4833(5) 0.0365(13) Uani 1 1 d . . . . .
C6 C 0.1984(7) 0.2979(5) 0.4737(5) 0.0382(13) Uani 1 1 d . . . . .
H3 H 0.277198 0.346814 0.514293 0.046 Uiso 1 1 calc R U . . .
H4 H 0.121086 0.330482 0.490664 0.046 Uiso 1 1 calc R U . . .
C7 C 0.0505(6) 0.2307(5) 0.2876(5) 0.0354(13) Uani 1 1 d . . . . .
H5 H 0.032211 0.233654 0.205200 0.043 Uiso 1 1 calc R U . . .
H6 H -0.027520 0.264377 0.302640 0.043 Uiso 1 1 calc R U . . .
C8 C 0.2895(6) 0.2510(5) 0.3225(5) 0.0355(12) Uani 1 1 d . . . . .
H7 H 0.272753 0.253362 0.240287 0.043 Uiso 1 1 calc R U . . .
H8 H 0.370335 0.298735 0.360212 0.043 Uiso 1 1 calc R U . . .
C9 C 0.1003(7) 0.1010(6) 0.4530(6) 0.0447(15) Uani 1 1 d . . . . .
H9 H 0.023401 0.134200 0.470233 0.054 Uiso 1 1 calc R U . . .
H10 H 0.113202 0.017563 0.480356 0.054 Uiso 1 1 calc R U . . .
C10 C 0.1913(6) 0.0533(5) 0.3037(6) 0.0387(13) Uani 1 1 d . . . . .
H11 H 0.206462 -0.030583 0.329663 0.046 Uiso 1 1 calc R U . . .
H12 H 0.174633 0.054307 0.221518 0.046 Uiso 1 1 calc R U . . .
C11 C 0.3370(6) 0.1222(6) 0.4861(6) 0.0439(15) Uani 1 1 d . . . . .
H13 H 0.417908 0.168930 0.525892 0.053 Uiso 1 1 calc R U . . .
H14 H 0.352799 0.038693 0.513096 0.053 Uiso 1 1 calc R U . . .
Ag1 Ag 0.11633(5) 0.49666(5) 0.28144(5) 0.05294(19) Uani 1 1 d . . . . .
N1 N 0.7014(9) 0.3537(9) 0.6806(9) 0.037(2) Uani 0.5 1 d . . P . .
H15 H 0.726457 0.341227 0.753616 0.044 Uiso 0.5 1 calc R U P . .
H16 H 0.747593 0.323234 0.641303 0.044 Uiso 0.5 1 calc R U P . .
N2 N 0.1719(4) 0.3061(4) 0.3466(4) 0.0304(9) Uani 1 1 d . . . . .
N3 N 0.2219(6) 0.1719(5) 0.5142(4) 0.0438(13) Uani 1 1 d . . . . .
N4 N 0.0695(5) 0.1018(4) 0.3266(5) 0.0355(11) Uani 1 1 d . . . . .
N5 N 0.3129(5) 0.1252(5) 0.3624(5) 0.0372(11) Uani 1 1 d . . . . .
O1 O 0.2225(7) 0.7002(9) 0.6447(7) 0.112(3) Uani 1 1 d . . . . .
O2 O 0.2711(7) 0.7918(6) 0.4875(8) 0.094(2) Uani 1 1 d . . . . .
O3 O 0.1266(5) 0.6136(6) 0.4581(5) 0.0692(16) Uani 1 1 d . . . . .
S1 S 0.2401(2) 0.6807(2) 0.5364(2) 0.0655(6) Uani 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'
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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
N1 C1 C2 112.7(8) . .
N1 C1 C5 127.7(8) . 3_666
C2 C1 C5 119.0(7) . 3_666
C3 C2 C1 122.3(7) . .
C3 C2 H1 118.8 . .
C1 C2 H1 118.8 . .
C2 C3 C4 121.5(7) . .
C2 C3 H2 119.2 . .
C4 C3 H2 119.2 . .
C3 C4 C5 119.1(7) . .
C3 C4 S1 115.4(6) . .
C5 C4 S1 125.5(5) . .
C4 C5 C5 119.9(7) . 3_666
C4 C5 C1 122.0(6) . 3_666
C5 C5 C1 118.1(7) 3_666 3_666
N3 C6 N2 111.4(4) . .
N3 C6 H3 109.4 . .
N2 C6 H3 109.4 . .
N3 C6 H4 109.4 . .
N2 C6 H4 109.4 . .
H3 C6 H4 108.0 . .
N2 C7 N4 111.9(4) . .
N2 C7 H5 109.2 . .
N4 C7 H5 109.2 . .
N2 C7 H6 109.2 . .
N4 C7 H6 109.2 . .
H5 C7 H6 107.9 . .
N5 C8 N2 111.9(5) . .
N5 C8 H7 109.2 . .
N2 C8 H7 109.2 . .
N5 C8 H8 109.2 . .
N2 C8 H8 109.2 . .
H7 C8 H8 107.9 . .
N3 C9 N4 112.4(5) . .
N3 C9 H9 109.1 . .
N4 C9 H9 109.1 . .
N3 C9 H10 109.1 . .
N4 C9 H10 109.1 . .
H9 C9 H10 107.9 . .
N5 C10 N4 111.6(5) . .
N5 C10 H11 109.3 . .
N4 C10 H11 109.3 . .
N5 C10 H12 109.3 . .
N4 C10 H12 109.3 . .
H11 C10 H12 108.0 . .
N5 C11 N3 111.9(5) . .
N5 C11 H13 109.2 . .
N3 C11 H13 109.2 . .
N5 C11 H14 109.2 . .
N3 C11 H14 109.2 . .
H13 C11 H14 107.9 . .
N2 Ag1 N4 138.75(17) . 2
N2 Ag1 N1 117.9(2) . 3_666
N4 Ag1 N1 103.2(2) 2 3_666
N2 Ag1 O3 103.6(2) . .
N4 Ag1 O3 91.56(19) 2 .
N1 Ag1 O3 71.7(3) 3_666 .
C1 N1 Ag1 102.6(6) . 3_666
C1 N1 H15 120.0 . .
Ag1 N1 H15 88.0 3_666 .
C1 N1 H16 120.0 . .
Ag1 N1 H16 79.5 3_666 .
H15 N1 H16 120.0 . .
C7 N2 C8 107.6(4) . .
C7 N2 C6 107.7(4) . .
C8 N2 C6 108.2(4) . .
C7 N2 Ag1 105.6(3) . .
C8 N2 Ag1 116.0(3) . .
C6 N2 Ag1 111.4(3) . .
C6 N3 C9 108.0(5) . .
C6 N3 C11 109.2(5) . .
C9 N3 C11 108.7(5) . .
C9 N4 C7 107.7(5) . .
C9 N4 C10 107.5(5) . .
C7 N4 C10 107.9(5) . .
C9 N4 Ag1 117.0(4) . 2_545
C7 N4 Ag1 107.5(3) . 2_545
C10 N4 Ag1 108.9(3) . 2_545
C8 N5 C11 108.9(5) . .
C8 N5 C10 108.9(5) . .
C11 N5 C10 108.6(5) . .
S1 O3 Ag1 128.7(3) . .
O1 S1 O2 112.5(5) . .
O1 S1 O3 111.4(4) . .
O2 S1 O3 113.5(5) . .
O1 S1 C4 105.5(4) . .
O2 S1 C4 107.5(4) . .
O3 S1 C4 105.8(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 N1 1.198(11) .
C1 C2 1.380(11) .
C1 C5 1.444(8) 3_666
C2 C3 1.376(12) .
C2 H1 0.9300 .
C3 C4 1.377(10) .
C3 H2 0.9300 .
C4 C5 1.432(9) .
C4 S1 1.793(8) .
C5 C5 1.441(13) 3_666
C6 N3 1.463(8) .
C6 N2 1.501(8) .
C6 H3 0.9700 .
C6 H4 0.9700 .
C7 N2 1.484(6) .
C7 N4 1.486(7) .
C7 H5 0.9700 .
C7 H6 0.9700 .
C8 N5 1.459(7) .
C8 N2 1.489(7) .
C8 H7 0.9700 .
C8 H8 0.9700 .
C9 N3 1.465(8) .
C9 N4 1.483(8) .
C9 H9 0.9700 .
C9 H10 0.9700 .
C10 N5 1.464(8) .
C10 N4 1.494(8) .
C10 H11 0.9700 .
C10 H12 0.9700 .
C11 N5 1.462(8) .
C11 N3 1.466(9) .
C11 H13 0.9700 .
C11 H14 0.9700 .
Ag1 N2 2.247(4) .
Ag1 N4 2.267(5) 2
Ag1 N1 2.440(9) 3_666
Ag1 O3 2.502(6) .
N1 H15 0.8600 .
N1 H16 0.8600 .
O1 S1 1.427(7) .
O2 S1 1.446(8) .
O3 S1 1.453(6) .
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
N1 H15 O1 0.86 1.95 2.638(11) 136.1 2_646 yes
N1 H16 O2 0.86 1.99 2.711(14) 140.9 3_666 yes
