Coordination polymers of alkali metal trithiocyanurates: structure determinations and ionic conductivity measurements using single crystals
Tominaka, Satoshi; Henke, Sebastian; Cheetham, Anthony K.; CrystEngComm 15 (2013) 9400–; doi:10.1039/c3ce41150h

data_7211038
_publ_section_title
;
 Coordination polymers of alkali metal trithiocyanurates: structure
 determinations and ionic conductivity measurements using single crystals
;
_journal_issue                   45
_journal_name_full               CrystEngComm
_journal_page_first              9400
_journal_paper_doi               10.1039/c3ce41150h
_journal_volume                  15
_journal_year                    2013
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C3 H2 N3 S3 -, Na +, 3(H2 O)'
_chemical_formula_sum            'C3 H8 N3 Na O3 S3'
_chemical_formula_weight         253.29
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-06-13
_audit_creation_method
;
  Olex2 1.2
  (compiled Apr 23 2013 17:54:37, GUI svn.r4466)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 109.059(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.3697(4)
_cell_length_b                   12.6801(3)
_cell_length_c                   7.7756(2)
_cell_measurement_reflns_used    6298
_cell_measurement_temperature    120
_cell_measurement_theta_max      71.2560
_cell_measurement_theta_min      4.4830
_cell_volume                     966.36(6)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
SHELXS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      120
_diffrn_detector_area_resol_mean 16.1183
_diffrn_measured_fraction_theta_full 0.9995
_diffrn_measured_fraction_theta_max 0.9897
_diffrn_measurement_details
;
  1 omega   35.00   62.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000 -178.0000  -90.0000 27

  2 omega   35.00   70.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000 -178.0000  120.0000 35

  3 omega    0.00   39.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -99.0000    0.0000 39

  4 omega  -15.00   12.00   1.0000    1.3700
omega____ theta____ kappa____ phi______ frames
    -      -54.7500   77.0000  -60.0000 27

  5 omega -117.00  -25.00   1.0000    1.3700
omega____ theta____ kappa____ phi______ frames
    -      -54.7500  -77.0000 -180.0000 92

  6 omega  -78.00  -19.00   1.0000    1.3700
omega____ theta____ kappa____ phi______ frames
    -      -54.7500   77.0000  -60.0000 59

  7 omega   76.00  103.00   1.0000    1.3700
omega____ theta____ kappa____ phi______ frames
    -       54.7500  125.0000   30.0000 27

  8 omega   93.00  121.00   1.0000    1.3700
omega____ theta____ kappa____ phi______ frames
    -       54.7500  125.0000  150.0000 28

  9 omega   82.00  125.00   1.0000    1.3700
omega____ theta____ kappa____ phi______ frames
    -       54.7500   37.0000 -150.0000 43

 10 omega   37.00   63.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -25.0000  150.0000 26

 11 omega   38.00  112.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000    0.0000   90.0000 74

 12 omega   59.00   86.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -77.0000  120.0000 27

 13 omega   45.00   80.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -50.0000  150.0000 35

 14 omega   38.00   66.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -25.0000 -180.0000 28

 15 omega   38.00   72.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -25.0000 -150.0000 34

 16 omega   82.00  153.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  111.0000  -90.0000 71

 17 omega   53.00   83.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -50.0000  -30.0000 30

 18 omega   69.00  134.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  178.0000   30.0000 65

 19 omega   65.00  104.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -91.0000 -150.0000 39

 20 omega   39.00   69.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -37.0000    0.0000 30

 21 omega  112.00  140.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -77.0000  150.0000 28

 22 omega  150.00  178.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000   50.0000  150.0000 28

 23 omega   40.00   91.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -77.0000  150.0000 51

 24 omega  114.00  139.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -77.0000  120.0000 25

 25 omega   41.00   68.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000 -111.0000  150.0000 27

 26 omega  124.00  162.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000    0.0000   90.0000 38

 27 omega   37.00   64.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -37.0000 -180.0000 27

 28 omega  -30.00   70.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   77.0000   90.0000 100

 29 omega  -21.00   69.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   57.0000   30.0000 90

 30 omega -127.00  -29.00   1.0000    1.3700
omega____ theta____ kappa____ phi______ frames
    -      -54.7500  -37.0000  -90.0000 98

 31 omega -125.00  -34.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -54.7500  -77.0000   30.0000 91

 32 omega   90.00  123.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       54.7500  125.0000  -30.0000 33

 33 omega   93.00  119.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       54.7500  105.0000  -80.0000 26

 34 omega -137.00  -99.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -64.0000  178.0000 -150.0000 38

 35 omega -100.00  -74.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -64.0000  178.0000   90.0000 26

 36 omega  -83.00  -57.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -64.0000  178.0000 -150.0000 26

 37 omega   41.00   67.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -37.0000  -90.0000 26

 38 omega   96.00  131.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  111.0000    0.0000 35

 39 omega   97.00  127.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -92.0000 -132.4267 30

 40 omega   65.00   91.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -63.0000    0.0000 26

 41 omega   38.00   64.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -25.0000  -30.0000 26

 42 omega   41.00   66.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -91.0000 -180.0000 25

 43 omega   53.00   79.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000 -111.0000   90.0000 26

 44 omega   88.00  114.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000   63.0000  -60.0000 26

 45 omega  131.00  166.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000   63.0000  -60.0000 35

 46 omega  142.00  167.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000   37.0000  150.0000 25

 47 omega   36.00   91.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  178.0000  -90.0000 55

 48 omega  120.00  147.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000   63.0000   60.0000 27

 49 omega  101.00  126.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000   37.0000   90.0000 25

 50 omega   84.00  113.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -93.0000   96.1262 29

 51 omega  103.00  129.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -93.0000  -61.4574 26

 52 omega  109.00  134.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  178.0000  -60.0000 25

 53 omega   42.00  139.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -91.0000    0.0000 97

 54 omega   44.00   70.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -25.0000 -120.0000 26

 55 omega   40.00   68.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -37.0000   30.0000 28

 56 omega   37.00   62.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -25.0000  -60.0000 25

 57 omega  109.00  134.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000   50.0000   30.0000 25

 58 omega   93.00  119.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -91.0000 -180.0000 26

 59 omega  127.00  162.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000   77.0000 -120.0000 35

 60 omega   85.00  111.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -91.0000   60.0000 26

 61 omega   55.00   81.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -50.0000   30.0000 26

 62 omega   32.00   77.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000 -178.0000   90.0000 45

 63 omega  -30.00   70.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   77.0000  150.0000 100

 64 omega  -69.00   21.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -57.0000  -60.0000 90

 65 omega  -73.00   15.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -19.0000  -90.0000 88

 66 omega   32.00   77.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000 -178.0000   30.0000 45
;
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.1064159000
_diffrn_orient_matrix_UB_12      -0.0770176000
_diffrn_orient_matrix_UB_13      -0.1202899000
_diffrn_orient_matrix_UB_21      0.1075368000
_diffrn_orient_matrix_UB_22      -0.0885970000
_diffrn_orient_matrix_UB_23      0.0462866000
_diffrn_orient_matrix_UB_31      -0.0425377000
_diffrn_orient_matrix_UB_32      -0.0313049000
_diffrn_orient_matrix_UB_33      0.1653141000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0312
_diffrn_reflns_av_unetI/netI     0.0322
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            10524
_diffrn_reflns_theta_full        70.9317
_diffrn_reflns_theta_max         71.22
_diffrn_reflns_theta_min         4.51
_diffrn_source                   'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.350
_exptl_absorpt_correction_T_max  0.703
_exptl_absorpt_correction_T_min  0.273
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.741
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'rect. Prism'
_exptl_crystal_F_000             520
_exptl_crystal_size_max          0.3399
_exptl_crystal_size_mid          0.0971
_exptl_crystal_size_min          0.0512
_refine_diff_density_max         0.374
_refine_diff_density_min         -0.258
_refine_diff_density_rms         0.059
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.50(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.160
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     283
_refine_ls_number_reflns         3723
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      1.160
_refine_ls_R_factor_all          0.0315
_refine_ls_R_factor_gt           0.0290
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0509P)^2^+0.3656P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0797
_refine_ls_wR_factor_ref         0.0931
_reflns_number_gt                3531
_reflns_number_total             3723
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3ce41150h.txt
_cod_data_source_block           NaTTC_120K
_cod_depositor_comments
;

2023-11-23
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C6 H16 N6 Na2 O6 S6'
_cod_original_formula_weight         506.59
_cod_original_formula_moiety         'C6 H16 N6 Na2 O6 S6'
_cod_original_formula_units_Z            2
_cod_original_cell_volume        966.37(5)
_cod_database_code               7211038
_chemical_oxdiff_formula         'Na1 C3 H8 O3 N3 S3'
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     70.93
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All N(H) groups
2. Restrained distances
 O6-H6A
 0.958 with sigma of 0.02
 H6B-O6 = O6-H6A
 0.958 with sigma of 0.02
 H1A-O1 = O1-H1B
 0.958 with sigma of 0.02
 H5B-O5 = O5-H5A
 0.958 with sigma of 0.02
 H2B-O2 = O2-H2A
 0.958 with sigma of 0.02
 H3B-O3 = O3-H3A
 0.958 with sigma of 0.02
 H4B-O4 = O4-H4A
 0.958 with sigma of 0.02
 H6B-H6A
 1.515 with sigma of 0.04
 H1A-H1B
 1.515 with sigma of 0.04
 H5B-H5A
 1.515 with sigma of 0.04
 H2B-H2A
 1.515 with sigma of 0.04
 H3B-H3A
 1.515 with sigma of 0.04
 H4B-H4A
 1.515 with sigma of 0.04
3.a Aromatic/amide H refined with riding coordinates:
 N11(H11), N12(H12), N9(H9), N10(H10)
;