#------------------------------------------------------------------------------
#$Date: 2022-05-10 11:31:38 +0300 (Tue, 10 May 2022) $
#$Revision: 275298 $
#$URL: file:///home/coder/svn-repositories/cod/cif/8/10/52/8105204.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_8105204
loop_
_publ_author_name
'Tai, Xi-Shi'
'Wang, Li-Hua'
'Xia, Yu-Pei'
_publ_section_title
;
 The crystal structure of poly[μ2-aqua-
 aqua-(μ3-(E)-2-(4-((2-carbamothioylhydrazineylidene)methyl)phenoxy)acetato-κ3
 O:S:S)sodium(I)], C10H14N3O5SNa
;
_journal_issue                   2
_journal_name_full
'Zeitschrift für Kristallographie - New Crystal Structures'
_journal_page_first              277
_journal_page_last               279
_journal_paper_doi               10.1515/ncrs-2022-0006
_journal_volume                  237
_journal_year                    2022
_chemical_formula_moiety         'C10 H14 N3 Na O5 S'
_chemical_formula_sum            'C10 H14 N3 Na O5 S'
_chemical_formula_weight         311.29
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_cell_angle_alpha                97.080(5)
_cell_angle_beta                 93.159(5)
_cell_angle_gamma                112.125(7)
_cell_formula_units_Z            2
_cell_length_a                   6.7015(5)
_cell_length_b                   7.5656(5)
_cell_length_c                   14.1332(8)
_cell_measurement_reflns_used    2133
_cell_measurement_temperature    273
_cell_measurement_theta_max      28.7140
_cell_measurement_theta_min      2.9240
_cell_volume                     654.71(8)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      273
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2684
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
--------------------------------------------------------------------------
  1  ω    -76.00  14.00   1.00    2.00    --  -11.59 -57.00  90.00   90
  2  ω    -36.00  62.00   1.00    2.00    --  -11.59  57.00-120.00   98
  3  ω    -15.00  77.00   1.00    2.00    --   11.74  77.00   0.00   92
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0263208000
_diffrn_orient_matrix_UB_12      -0.0334932000
_diffrn_orient_matrix_UB_13      -0.0448264000
_diffrn_orient_matrix_UB_21      0.0521318000
_diffrn_orient_matrix_UB_22      -0.0514571000
_diffrn_orient_matrix_UB_23      0.0232691000
_diffrn_orient_matrix_UB_31      -0.0990189000
_diffrn_orient_matrix_UB_32      -0.0820203000
_diffrn_orient_matrix_UB_33      -0.0061889000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0269
_diffrn_reflns_av_unetI/netI     0.0485
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            4268
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        24.997
_diffrn_reflns_theta_max         24.997
_diffrn_reflns_theta_min         2.923
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.303
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.76451
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43f (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.579
_exptl_crystal_description       block
_exptl_crystal_F_000             324
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.264
_refine_diff_density_min         -0.267
_refine_diff_density_rms         0.063
_refine_ls_extinction_coef       0.012(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     205
_refine_ls_number_reflns         2284
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0433
_refine_ls_R_factor_gt           0.0357
_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)+(0.0374P)²+0.1070P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0818
_refine_ls_wR_factor_ref         0.0872
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1969
_reflns_number_total             2284
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            suppl_j_ncrs-2022-0006_suppl.cif
_cod_data_source_block           w14_sx
_cod_database_code               8105204
_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_max   0.976
_shelx_estimated_absorpt_t_min   0.967
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C1) \\sim Ueq, Uanis(S1) \\sim Ueq: with sigma of 0.0005 and sigma for
terminal atoms of 0.001
3.a Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B)
3.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C5(H5), C7(H7), C8(H8)
3.c X=CH2 refined with riding coordinates:
 N1(H1A,H1B)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.676
_oxdiff_exptl_absorpt_empirical_full_min 0.707
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
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 1.2614(3) 0.8211(3) 0.20138(13) 0.0093(4) Uani 1 1 d . U . . .
C2 C 0.8917(3) 0.8458(3) 0.36091(14) 0.0105(4) Uani 1 1 d . . . . .
H2 H 0.829020 0.911663 0.325921 0.013 Uiso 1 1 calc R U . . .
C3 C 0.8089(3) 0.7887(3) 0.45049(13) 0.0096(4) Uani 1 1 d . . . . .
C4 C 0.6266(3) 0.8194(3) 0.47820(14) 0.0105(4) Uani 1 1 d . . . . .
H4 H 0.560939 0.877113 0.439220 0.013 Uiso 1 1 calc R U . . .
C5 C 0.5405(3) 0.7665(3) 0.56205(14) 0.0105(4) Uani 1 1 d . . . . .
H5 H 0.417806 0.787286 0.578535 0.013 Uiso 1 1 calc R U . . .
C6 C 0.6382(3) 0.6822(3) 0.62135(13) 0.0098(4) Uani 1 1 d . . . . .
C7 C 0.8259(3) 0.6554(3) 0.59643(14) 0.0114(5) Uani 1 1 d . . . . .
H7 H 0.894868 0.602880 0.636993 0.014 Uiso 1 1 calc R U . . .
C8 C 0.9085(3) 0.7064(3) 0.51219(14) 0.0113(5) Uani 1 1 d . . . . .
H8 H 1.031726 0.686224 0.495946 0.014 Uiso 1 1 calc R U . . .
C9 C 0.3739(3) 0.6464(3) 0.73119(14) 0.0103(4) Uani 1 1 d . . . . .
H9A H 0.259916 0.588714 0.678176 0.012 Uiso 1 1 calc R U . . .
H9B H 0.403109 0.783253 0.744570 0.012 Uiso 1 1 calc R U . . .
C10 C 0.2982(3) 0.5538(3) 0.81928(13) 0.0099(5) Uani 1 1 d . . . . .
H2A H 1.047(4) 0.929(3) 0.2175(15) 0.010(6) Uiso 1 1 d . . . . .
H4A H -0.330(4) 0.620(3) 0.9382(18) 0.029(7) Uiso 1 1 d . . . . .
H4B H -0.289(4) 0.641(4) 1.036(2) 0.039(8) Uiso 1 1 d . . . . .
H5A H 0.124(4) 0.828(4) 0.8493(18) 0.039(8) Uiso 1 1 d . . . . .
H5B H 0.259(4) 1.004(3) 0.8610(17) 0.023(8) Uiso 1 1 d . . . . .
N1 N 1.3532(3) 0.7232(2) 0.24710(11) 0.0134(4) Uani 1 1 d . . . . .
H1A H 1.316859 0.694239 0.302336 0.016 Uiso 1 1 calc R U . . .
H1B H 1.448956 0.688713 0.221483 0.016 Uiso 1 1 calc R U . . .
N2 N 1.1127(3) 0.8718(2) 0.24420(12) 0.0107(4) Uani 1 1 d . . . . .
N3 N 1.0488(3) 0.8073(2) 0.32929(11) 0.0105(4) Uani 1 1 d . . . . .
Na1 Na 0.000000 0.500000 1.000000 0.0124(3) Uani 1 2 d S . P . .
Na2 Na 0.000000 1.000000 1.000000 0.0127(3) Uani 1 2 d S . P . .
O1 O 0.5654(2) 0.62119(18) 0.70468(9) 0.0119(3) Uani 1 1 d . . . . .
O2 O 0.3924(2) 0.45320(18) 0.85119(9) 0.0121(3) Uani 1 1 d . . . . .
O3 O 0.1427(2) 0.58362(18) 0.85230(9) 0.0118(3) Uani 1 1 d . . . . .
O4 O -0.2275(2) 0.6722(2) 0.98521(12) 0.0132(3) Uani 1 1 d . . . . .
O5 O 0.1361(3) 0.9456(2) 0.85079(11) 0.0141(4) Uani 1 1 d . . . . .
S1 S 1.33292(8) 0.88919(7) 0.09353(3) 0.01171(17) Uani 1 1 d . U . . .
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'
Na Na 0.0362 0.0249 '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 N2 117.86(18) . .
N1 C1 S1 122.11(15) . .
N2 C1 S1 120.00(15) . .
C3 C2 H2 119.2 . .
N3 C2 H2 119.2 . .
N3 C2 C3 121.56(19) . .
C4 C3 C2 119.59(19) . .
C4 C3 C8 117.80(18) . .
C8 C3 C2 122.59(19) . .
C3 C4 H4 119.1 . .
C5 C4 C3 121.89(19) . .
C5 C4 H4 119.1 . .
C4 C5 H5 120.2 . .
C4 C5 C6 119.64(19) . .
C6 C5 H5 120.2 . .
C5 C6 C7 119.47(18) . .
O1 C6 C5 124.70(18) . .
O1 C6 C7 115.83(18) . .
C6 C7 H7 119.8 . .
C8 C7 C6 120.34(19) . .
C8 C7 H7 119.8 . .
C3 C8 H8 119.6 . .
C7 C8 C3 120.82(19) . .
C7 C8 H8 119.6 . .
H9A C9 H9B 108.0 . .
C10 C9 H9A 109.4 . .
C10 C9 H9B 109.4 . .
O1 C9 H9A 109.4 . .
O1 C9 H9B 109.4 . .
O1 C9 C10 111.10(16) . .
O2 C10 C9 118.63(18) . .
O3 C10 C9 115.21(18) . .
O3 C10 O2 126.14(18) . .
C1 N1 H1A 120.0 . .
C1 N1 H1B 120.0 . .
H1A N1 H1B 120.0 . .
C1 N2 H2A 121.3(15) . .
C1 N2 N3 119.21(18) . .
N3 N2 H2A 119.0(16) . .
C2 N3 N2 115.52(17) . .
H4B Na1 H4B 180.000(15) . 2_567
Na1 Na1 H4B 0(10) 2_567 .
Na1 Na1 H4B 0(10) 2_567 2_567
Na1 Na1 Na2 0.0 2_567 1_545
Na1 Na1 O3 0(10) 2_567 2_567
Na1 Na1 O3 0(10) 2_567 .
Na1 Na1 O4 0(10) 2_567 2_567
Na1 Na1 O4 0(10) 2_567 .
Na1 Na1 S1 0(10) 2_567 2_666
Na1 Na1 S1 0(8) 2_567 1_456
Na2 Na1 H4B 132.2(6) 1_545 .
Na2 Na1 H4B 47.8(6) 1_545 2_567
O3 Na1 H4B 110.4(6) 2_567 2_567
O3 Na1 H4B 69.6(6) . 2_567
O3 Na1 H4B 110.4(6) . .
O3 Na1 H4B 69.6(7) 2_567 .
O3 Na1 Na2 102.75(3) . 1_545
O3 Na1 Na2 77.25(3) 2_567 1_545
O3 Na1 O3 180.00(11) 2_567 .
O3 Na1 S1 93.84(3) 2_567 1_456
O3 Na1 S1 93.84(3) . 2_666
O3 Na1 S1 86.16(3) . 1_456
O3 Na1 S1 86.16(3) 2_567 2_666
O4 Na1 H4B 19.3(6) . .
O4 Na1 H4B 160.7(6) . 2_567
O4 Na1 H4B 160.7(6) 2_567 .
O4 Na1 H4B 19.3(6) 2_567 2_567
O4 Na1 Na2 36.43(4) 2_567 1_545
O4 Na1 Na2 143.57(4) . 1_545
O4 Na1 O3 88.82(5) . 2_567
O4 Na1 O3 91.18(5) 2_567 2_567
O4 Na1 O3 88.82(5) 2_567 .
O4 Na1 O3 91.18(5) . .
O4 Na1 O4 180.0 . 2_567
O4 Na1 S1 96.05(4) 2_567 1_456
O4 Na1 S1 83.95(4) 2_567 2_666
O4 Na1 S1 83.95(4) . 1_456
O4 Na1 S1 96.05(4) . 2_666
S1 Na1 H4B 93.4(6) 2_666 .
S1 Na1 H4B 86.6(6) 2_666 2_567
S1 Na1 H4B 86.6(6) 1_456 .
S1 Na1 H4B 93.4(6) 1_456 2_567
S1 Na1 Na2 50.107(11) 2_666 1_545
S1 Na1 Na2 129.893(11) 1_456 1_545
S1 Na1 S1 180.0 1_456 2_666
O4 Na2 O4 180.0 2_577 .
O4 Na2 O5 91.39(6) 2_577 2_577
O4 Na2 O5 88.61(6) 2_577 .
O4 Na2 O5 91.39(6) . .
O4 Na2 O5 88.61(6) . 2_577
O4 Na2 S1 85.69(4) 2_577 2_676
O4 Na2 S1 94.31(4) 2_577 1_456
O4 Na2 S1 94.31(4) . 2_676
O4 Na2 S1 85.69(4) . 1_456
O5 Na2 O5 180.0 . 2_577
O5 Na2 S1 92.16(4) . 2_676
O5 Na2 S1 87.84(4) 2_577 2_676
O5 Na2 S1 87.84(4) . 1_456
O5 Na2 S1 92.16(4) 2_577 1_456
S1 Na2 S1 180.0 2_676 1_456
C6 O1 C9 116.74(15) . .
C10 O3 Na1 126.51(13) . 2_567
C10 O3 Na1 126.51(13) . .
Na1 O3 Na1 0.0 2_567 .
H4A O4 H4B 105(2) . .
Na1 O4 H4A 113.3(16) 2_567 .
Na1 O4 H4A 113.3(16) . .
Na1 O4 H4B 94.9(19) . .
Na1 O4 H4B 94.9(19) 2_567 .
Na1 O4 Na1 0.0 2_567 .
Na2 O4 H4A 120.3(16) . .
Na2 O4 H4B 113.8(17) . .
Na2 O4 Na1 106.79(6) . .
Na2 O4 Na1 106.79(6) . 2_567
H5A O5 H5B 103(3) . .
Na2 O5 H5A 100.9(18) . .
Na2 O5 H5B 104.2(19) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 N1 1.327(3) .
C1 N2 1.343(3) .
C1 S1 1.7049(19) .
C2 H2 0.9300 .
C2 C3 1.459(3) .
C2 N3 1.282(3) .
C3 C4 1.395(3) .
C3 C8 1.406(3) .
C4 H4 0.9300 .
C4 C5 1.384(3) .
C5 H5 0.9300 .
C5 C6 1.387(3) .
C6 C7 1.404(3) .
C6 O1 1.366(2) .
C7 H7 0.9300 .
C7 C8 1.378(3) .
C8 H8 0.9300 .
C9 H9A 0.9700 .
C9 H9B 0.9700 .
C9 C10 1.522(3) .
C9 O1 1.429(2) .
C10 O2 1.263(2) .
C10 O3 1.249(2) .
N1 H1A 0.8600 .
N1 H1B 0.8600 .
N2 H2A 0.83(2) .
N2 N3 1.383(2) .
Na1 H4B 2.58(3) .
Na1 Na1 0.0000 2_567
Na1 Na2 3.7828(3) 1_545
Na1 O3 2.4005(13) .
Na1 O3 2.4005(13) 2_567
Na1 O4 2.3654(15) .
Na1 O4 2.3654(15) 2_567
Na1 S1 3.0269(6) 1_456
Na1 S1 3.0269(6) 2_666
Na2 O4 2.3467(14) 2_577
Na2 O4 2.3467(14) .
Na2 O5 2.3936(15) 2_577
Na2 O5 2.3936(15) .
Na2 S1 2.9639(6) 1_456
Na2 S1 2.9639(6) 2_676
O4 H4A 0.87(3) .
O4 H4B 0.86(3) .
O5 H5A 0.86(3) .
O5 H5B 0.77(3) .
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
C1 N2 N3 C2 -173.49(17) . . . .
C2 C3 C4 C5 179.46(16) . . . .
C2 C3 C8 C7 179.65(17) . . . .
C3 C2 N3 N2 -179.25(15) . . . .
C3 C4 C5 C6 0.7(3) . . . .
C4 C3 C8 C7 1.0(3) . . . .
C4 C5 C6 C7 1.3(3) . . . .
C4 C5 C6 O1 -178.77(16) . . . .
C5 C6 C7 C8 -2.1(3) . . . .
C5 C6 O1 C9 0.3(3) . . . .
C6 C7 C8 C3 1.0(3) . . . .
C7 C6 O1 C9 -179.75(15) . . . .
C8 C3 C4 C5 -1.8(3) . . . .
C9 C10 O3 Na1 -171.91(11) . . . 2_567
C9 C10 O3 Na1 -171.91(11) . . . .
C10 C9 O1 C6 174.07(14) . . . .
N1 C1 N2 N3 -5.2(3) . . . .
N3 C2 C3 C4 -174.78(17) . . . .
N3 C2 C3 C8 6.6(3) . . . .
O1 C6 C7 C8 177.94(15) . . . .
O1 C9 C10 O2 -7.1(2) . . . .
O1 C9 C10 O3 174.02(15) . . . .
O2 C10 O3 Na1 9.4(3) . . . .
O2 C10 O3 Na1 9.4(3) . . . 2_567
S1 C1 N2 N3 176.83(13) . . . .
