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_7211039
_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_formula_moiety         'C3 H8 N3 Na O3 S3'
_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           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-06-12
_audit_creation_method
;
  Olex2 1.2
  (compiled Apr 23 2013 17:54:37, GUI svn.r4466)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 109.644(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.4530(2)
_cell_length_b                   12.7369(2)
_cell_length_c                   7.86207(17)
_cell_measurement_reflns_used    10603
_cell_measurement_temperature    298
_cell_measurement_theta_max      71.1740
_cell_measurement_theta_min      3.4450
_cell_volume                     985.83(3)
_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      298
_diffrn_detector_area_resol_mean 16.1183
_diffrn_measured_fraction_theta_full 0.9995
_diffrn_measured_fraction_theta_max 0.9754
_diffrn_measurement_details
;
  1 omega   43.00   70.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   77.0000 -120.0000 27

  2 omega   33.00   77.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000 -178.0000  120.0000 44

  3 omega   -5.00   21.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   77.0000 -120.0000 26

  4 omega   32.00   69.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000 -178.0000 -180.0000 37

  5 omega   33.00   74.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000 -178.0000  -30.0000 41

  6 omega  -65.00  -39.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -54.7500  -57.0000  -60.0000 26

  7 omega -124.00  -85.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -54.7500  -57.0000  -60.0000 39

  8 omega   76.00  123.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       54.7500  125.0000   30.0000 47

  9 omega   79.00  126.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       54.7500  125.0000 -180.0000 47

 10 omega   42.00  113.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       54.7500   57.0000  120.0000 71

 11 omega  -17.00   70.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       54.7500  -37.0000  120.0000 87

 12 omega  -85.00  -24.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -64.0000   63.0000   30.0000 61

 13 omega  -80.00  -40.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -64.0000  -75.0000  -52.8755 40

 14 omega -110.00  -43.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -64.0000  -77.0000 -120.0000 67

 15 omega  -66.00  -36.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -64.0000  -77.0000  -90.0000 30

 16 omega   41.00   67.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -25.0000 -180.0000 26

 17 omega  122.00  148.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000   50.0000  150.0000 26

 18 omega   56.00   82.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000 -111.0000  -30.0000 26

 19 omega   54.00   90.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000 -111.0000  120.0000 36

 20 omega   44.00   69.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -50.0000 -120.0000 25

 21 omega   38.00   69.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -25.0000   60.0000 31

 22 omega  134.00  171.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000   63.0000  -90.0000 37

 23 omega  145.00  171.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000   77.0000  -30.0000 26

 24 omega   79.00  112.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000   77.0000  -90.0000 33

 25 omega   88.00  134.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000   63.0000 -180.0000 46

 26 omega   91.00  117.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000   50.0000  -90.0000 26

 27 omega   84.00  142.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000   37.0000  -60.0000 58

 28 omega   49.00   75.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -50.0000 -180.0000 26

 29 omega   37.00   72.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -25.0000 -120.0000 35

 30 omega   82.00  108.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000   77.0000  -30.0000 26

 31 omega   37.00   63.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000 -111.0000  150.0000 26

 32 omega  122.00  148.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000   63.0000   30.0000 26

 33 omega   53.00   79.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000 -111.0000  -60.0000 26

 34 omega   38.00   71.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -25.0000  150.0000 33

 35 omega   39.00   75.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -50.0000  -90.0000 36

 36 omega  118.00  165.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000   25.0000  120.0000 47

 37 omega   83.00  109.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000   25.0000  120.0000 26

 38 omega   43.00   69.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -25.0000  -30.0000 26

 39 omega   79.00  106.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000   77.0000 -150.0000 27

 40 omega   92.00  118.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000   63.0000   30.0000 26

 41 omega  140.00  169.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000   63.0000  -60.0000 29

 42 omega   87.00  122.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000   63.0000  -30.0000 35

 43 omega   79.00  105.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000   77.0000 -120.0000 26

 44 omega   75.00  101.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -63.0000   60.0000 26

 45 omega  107.00  132.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -63.0000   60.0000 25

 46 omega   37.00   69.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -25.0000   30.0000 32

 47 omega  134.00  164.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000   37.0000 -120.0000 30

 48 omega   87.00  135.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000   63.0000  -60.0000 48

 49 omega   83.00  127.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -63.0000  150.0000 44

 50 omega   87.00  146.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000   63.0000 -120.0000 59

 51 omega   79.00  118.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000   77.0000  -60.0000 39

 52 omega   91.00  116.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000   50.0000 -120.0000 25

 53 omega   40.00   69.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -25.0000 -150.0000 29

 54 omega   89.00  117.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000   50.0000  150.0000 28

 55 omega   45.00   72.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -25.0000  -90.0000 27

 56 omega   85.00  112.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000   37.0000 -120.0000 27

 57 omega   85.00  110.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000   37.0000    0.0000 25

 58 omega   88.00  115.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000   63.0000  -90.0000 27

 59 omega   89.00  153.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000   50.0000   60.0000 64

 60 omega  -25.00   42.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -99.0000  150.0000 67

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

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

 63 omega  -69.00   21.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -57.0000 -120.0000 90

 64 omega -125.00  -25.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -54.7500  -77.0000 -180.0000 100

 65 omega -112.00  -18.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -54.7500  125.0000   60.0000 94

 66 omega  -75.00   14.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -54.7500   57.0000   90.0000 89

 67 omega -125.00  -25.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -54.7500  -77.0000 -120.0000 100

 68 omega -125.00  -25.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -54.7500  -77.0000    0.0000 100

 69 omega -124.00  -33.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -54.7500  -57.0000   30.0000 91

 70 omega -125.00  -25.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -54.7500  -77.0000  120.0000 100

 71 omega   -3.00   96.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       54.7500 -125.0000  -90.0000 99

 72 omega   37.00   90.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000 -111.0000   30.0000 53

 73 omega   79.00  178.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  111.0000  -30.0000 99

 74 omega   39.00   83.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -50.0000  -30.0000 44

 75 omega   38.00  147.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -91.0000  -60.0000 109

 76 omega   87.00  177.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000   63.0000   60.0000 90

 77 omega   37.00   71.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -37.0000   30.0000 34

 78 omega   79.00  178.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000   77.0000  150.0000 99

 79 omega   38.00  147.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -91.0000  150.0000 109

 80 omega   87.00  177.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000   63.0000   90.0000 90

 81 omega   79.00  158.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000   77.0000    0.0000 79

 82 omega   37.00   71.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -37.0000    0.0000 34
;
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.1550068000
_diffrn_orient_matrix_UB_12      0.0163065000
_diffrn_orient_matrix_UB_13      0.0684848000
_diffrn_orient_matrix_UB_21      0.0099508000
_diffrn_orient_matrix_UB_22      -0.0596473000
_diffrn_orient_matrix_UB_23      -0.1656073000
_diffrn_orient_matrix_UB_31      -0.0186288000
_diffrn_orient_matrix_UB_32      0.1039601000
_diffrn_orient_matrix_UB_33      -0.1057714000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0221
_diffrn_reflns_av_unetI/netI     0.0096
_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       -9
_diffrn_reflns_number            17362
_diffrn_reflns_theta_full        70.9317
_diffrn_reflns_theta_max         71.35
_diffrn_reflns_theta_min         4.49
_diffrn_source                   'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.204
_exptl_absorpt_correction_T_max  0.711
_exptl_absorpt_correction_T_min  0.312
_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    1.707
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'rect. Prism'
_exptl_crystal_F_000             520
_exptl_crystal_size_max          0.2605
_exptl_crystal_size_mid          0.0934
_exptl_crystal_size_min          0.0504
_refine_diff_density_max         0.419
_refine_diff_density_min         -0.401
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     142
_refine_ls_number_reflns         1918
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.0263
_refine_ls_R_factor_gt           0.0254
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0390P)^2^+0.4136P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0708
_refine_ls_wR_factor_ref         0.0716
_reflns_number_gt                1827
_reflns_number_total             1918
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3ce41150h.txt
_cod_data_source_block           NaTTC_RT
_cod_database_code               7211039
_chemical_oxdiff_formula         'Na 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
 H3A-O3 = O3-H3B
 0.958 with sigma of 0.02
 H1A-O1 = O1-H1B
 0.958 with sigma of 0.02
 H2A-O2
 0.958 with sigma of 0.02
 H2A-O2 = O2-H2B
 0.958 with sigma of 0.02
 H3A-H3B
 1.515 with sigma of 0.04
 H1A-H1B
 1.515 with sigma of 0.04
 H2A-H2B
 1.515 with sigma of 0.04
3.a Aromatic/amide H refined with riding coordinates:
 N5(H5), N6(H6)
;