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_7211044
_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         'C6 H4 Cs2 N6 S6'
_chemical_formula_sum            'C6 H4 Cs2 N6 S6'
_chemical_formula_weight         618.33
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 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                 92.3402(13)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   5.41409(8)
_cell_length_b                   21.2829(3)
_cell_length_c                   14.9761(2)
_cell_measurement_reflns_used    10388
_cell_measurement_temperature    300.00(14)
_cell_measurement_theta_max      71.1550
_cell_measurement_theta_min      4.1590
_cell_volume                     1724.22(4)
_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      300.00(14)
_diffrn_detector_area_resol_mean 16.1183
_diffrn_measured_fraction_theta_full 0.9994
_diffrn_measured_fraction_theta_max 0.8386
_diffrn_measurement_details
;
  1 omega   13.00   41.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -99.0000    0.0000 28

  2 omega  -25.00    6.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -99.0000    0.0000 31

  3 omega    8.00   62.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   57.0000   60.0000 54

  4 omega   36.00   62.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000 -178.0000  -60.0000 26

  5 omega   27.00  123.00   1.0000    1.4800
omega____ theta____ kappa____ phi______ frames
    -       54.7500   77.0000  -30.0000 96

  6 omega   33.00  112.00   1.0000    1.4800
omega____ theta____ kappa____ phi______ frames
    -       54.7500   57.0000  150.0000 79

  7 omega   75.00  121.00   1.0000    1.4800
omega____ theta____ kappa____ phi______ frames
    -       54.7500  125.0000   60.0000 46

  8 omega   57.00   96.00   1.0000    1.4800
omega____ theta____ kappa____ phi______ frames
    -       54.7500   57.0000   90.0000 39

  9 omega  -46.00    3.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -64.0000   37.0000   60.0000 49

 10 omega  -85.00   -3.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -64.0000   63.0000 -120.0000 82

 11 omega -141.00  -72.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -64.0000  178.0000 -150.0000 69

 12 omega   39.00   68.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -25.0000 -150.0000 29

 13 omega   39.00   72.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -25.0000  120.0000 33

 14 omega   39.00   72.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -25.0000  -60.0000 33

 15 omega   80.00  124.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000   25.0000   90.0000 44

 16 omega   40.00   67.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -25.0000   30.0000 27

 17 omega   40.00   71.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -25.0000  -90.0000 31

 18 omega   41.00   81.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -50.0000  -30.0000 40

 19 omega   84.00  110.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -91.0000  -90.0000 26

 20 omega   41.00  107.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -91.0000  150.0000 66

 21 omega   42.00   78.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -91.0000 -120.0000 36

 22 omega   79.00  107.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -91.0000    0.0000 28

 23 omega   43.00   69.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000 -111.0000  -90.0000 26

 24 omega   39.00   64.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -50.0000  -90.0000 25

 25 omega   45.00  143.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -91.0000 -150.0000 98

 26 omega   39.00   72.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -25.0000   90.0000 33

 27 omega  150.00  176.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000   25.0000   90.0000 26

 28 omega   38.00   71.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -25.0000   60.0000 33

 29 omega   63.00   99.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -12.0000  -60.0000 36

 30 omega  134.00  177.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -12.0000  -60.0000 43

 31 omega   42.00   68.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -25.0000  -30.0000 26

 32 omega   88.00  114.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000   25.0000    0.0000 26

 33 omega  109.00  178.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000   50.0000    0.0000 69

 34 omega   50.00   75.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -50.0000   60.0000 25

 35 omega   52.00   77.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -50.0000  120.0000 25

 36 omega  102.00  129.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -91.0000   30.0000 27

 37 omega   88.00  115.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000   63.0000  120.0000 27

 38 omega  146.00  172.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000   63.0000  120.0000 26

 39 omega   50.00   95.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -77.0000  -30.0000 45

 40 omega  100.00  138.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -77.0000  -30.0000 38

 41 omega   42.00   71.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -25.0000 -120.0000 29

 42 omega  101.00  146.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -91.0000 -120.0000 45

 43 omega   42.00   71.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -25.0000 -180.0000 29

 44 omega   39.00   70.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -25.0000    0.0000 31

 45 omega   39.00   64.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -50.0000 -120.0000 25

 46 omega   50.00  108.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -91.0000   60.0000 58

 47 omega   69.00   95.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -93.0000  108.2968 26

 48 omega  -26.00   72.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   37.0000  -60.0000 98

 49 omega  -25.00   42.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -99.0000  120.0000 67

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

 51 omega -112.00  -18.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -54.7500  125.0000    0.0000 94

 52 omega   25.00  125.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       54.7500   77.0000 -180.0000 100

 53 omega   75.00  126.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       54.7500  121.0000 -122.0000 51

 54 omega   25.00  125.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       54.7500   77.0000   30.0000 100

 55 omega   25.00  125.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       54.7500   77.0000   90.0000 100

 56 omega   25.00  125.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       54.7500   77.0000 -120.0000 100

 57 omega   84.00  109.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000   37.0000  -60.0000 25

 58 omega   88.00  178.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000   50.0000   90.0000 90

 59 omega   84.00  178.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000   37.0000   30.0000 94

 60 omega   38.00  178.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000   12.0000 -120.0000 140

 61 omega   32.00   57.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000 -178.0000  150.0000 25

 62 omega  100.00  125.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       54.7500  155.0000   37.0000 25

 63 omega   91.00  117.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000   77.0000  150.0000 26

 64 omega   37.00   62.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -25.0000  150.0000 25

 65 omega   39.00   64.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -50.0000 -150.0000 25

 66 omega   43.00   68.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -37.0000  -90.0000 25

 67 omega   45.00   71.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -63.0000 -150.0000 26

 68 omega   47.00   73.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000 -111.0000 -150.0000 26

 69 omega   39.00   65.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000    0.0000 -180.0000 26

 70 omega  113.00  149.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000    0.0000 -180.0000 36

 71 omega  153.00  178.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000   77.0000  150.0000 25

 72 omega   66.00  116.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -63.0000    0.0000 50

 73 omega   56.00   95.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -91.0000  -30.0000 39

 74 omega  106.00  141.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -93.0000 -134.8294 35

 75 omega  109.00  142.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000   50.0000  -60.0000 33

 76 omega  152.00  177.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000   63.0000  -30.0000 25

 77 omega   91.00  126.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000   50.0000  -30.0000 35

 78 omega   54.00   80.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  155.0000   37.0000 26

 79 omega   78.00  104.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -91.0000 -180.0000 26

 80 omega   96.00  141.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -93.0000   13.8441 45
;
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0432566000
_diffrn_orient_matrix_UB_12      -0.0678753000
_diffrn_orient_matrix_UB_13      0.0328178000
_diffrn_orient_matrix_UB_21      -0.2005517000
_diffrn_orient_matrix_UB_22      -0.0235008000
_diffrn_orient_matrix_UB_23      -0.0679250000
_diffrn_orient_matrix_UB_31      0.1975404000
_diffrn_orient_matrix_UB_32      -0.0089928000
_diffrn_orient_matrix_UB_33      -0.0700435000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0683
_diffrn_reflns_av_unetI/netI     0.0472
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            13137
_diffrn_reflns_theta_full        69.9455
_diffrn_reflns_theta_max         71.15
_diffrn_reflns_theta_min         4.15
_diffrn_source                   'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    39.763
_exptl_absorpt_correction_T_max  0.470
_exptl_absorpt_correction_T_min  0.018
_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 orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.382
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1152
_exptl_crystal_size_max          0.3237
_exptl_crystal_size_mid          0.1699
_exptl_crystal_size_min          0.0214
_refine_diff_density_max         0.633
_refine_diff_density_min         -0.857
_refine_diff_density_rms         0.205
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.004(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.223
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     181
_refine_ls_number_reflns         2824
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.223
_refine_ls_R_factor_all          0.0478
_refine_ls_R_factor_gt           0.0460
_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^)+(0.0903P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1207
_refine_ls_wR_factor_ref         0.1236
_reflns_number_gt                2796
_reflns_number_total             2824
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3ce41150h.txt
_cod_data_source_block           CsTTC2
_cod_database_code               7211044
_chemical_oxdiff_formula         'Cs2 S6 C6 N6 H4'
_reflns_odcompleteness_completeness 99.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     69.95
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All N(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 N6(H6), N7(H7), N8(H8), N9(H9)
;