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_7211040
_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         'C6 H8 K2 N6 O2 S6'
_chemical_formula_sum            'C6 H8 K2 N6 O2 S6'
_chemical_formula_weight         466.74
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_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                76.285(3)
_cell_angle_beta                 80.914(4)
_cell_angle_gamma                87.551(4)
_cell_formula_units_Z            2
_cell_length_a                   7.3438(4)
_cell_length_b                   10.3247(4)
_cell_length_c                   11.6813(5)
_cell_measurement_reflns_used    5620
_cell_measurement_temperature    298.6(2)
_cell_measurement_theta_max      71.1960
_cell_measurement_theta_min      3.9250
_cell_volume                     849.64(7)
_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
;
olex2.solve (L.J. Bourhis, O.V. Dolomanov, R.J. Gildea, J.A.K. Howard,
H. Puschmann, in preparation, 2011)
;
_diffrn_ambient_temperature      298.6(2)
_diffrn_detector_area_resol_mean 16.1183
_diffrn_measured_fraction_theta_full 0.9755
_diffrn_measured_fraction_theta_max 0.9918
_diffrn_measurement_details
;
  1 omega  -22.00   33.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -99.0000 -120.0000 55

  2 omega   41.00   69.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000 -178.0000  120.0000 28

  3 omega   -2.00   25.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -37.0000  -30.0000 27

  4 omega  -50.00  -18.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -37.0000  -30.0000 32

  5 omega  -70.00   -4.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -54.7500   57.0000  -60.0000 66

  6 omega  -90.00  -29.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -54.7500  138.0000  -67.0000 61

  7 omega -126.00  -32.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -54.7500  -37.0000  120.0000 94

  8 omega   95.00  124.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       54.7500   77.0000  150.0000 29

  9 omega   87.00  125.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       54.7500  125.0000   90.0000 38

 10 omega   83.00  122.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       54.7500  125.0000 -180.0000 39

 11 omega  -72.00  -20.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -64.0000   25.0000  -60.0000 52

 12 omega  -17.00    9.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -64.0000   25.0000  -60.0000 26

 13 omega -139.00  -63.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -64.0000  178.0000    0.0000 76

 14 omega   47.00   73.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000 -111.0000 -180.0000 26

 15 omega  104.00  139.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -77.0000 -120.0000 35

 16 omega   37.00   62.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -37.0000  -90.0000 25

 17 omega   40.00   65.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -37.0000 -150.0000 25

 18 omega   95.00  137.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000   50.0000 -150.0000 42

 19 omega   43.00   71.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -25.0000  120.0000 28

 20 omega   94.00  130.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -63.0000    0.0000 36

 21 omega   93.00  178.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000   50.0000  -60.0000 85

 22 omega   37.00   62.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -37.0000 -180.0000 25

 23 omega   62.00   88.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -15.0000  114.6601 26

 24 omega   67.00  142.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -91.0000  120.0000 75

 25 omega   48.00  117.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -63.0000  120.0000 69

 26 omega   48.00   94.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -77.0000 -120.0000 46

 27 omega   67.00  147.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -91.0000  -60.0000 80

 28 omega   90.00  132.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000   50.0000  120.0000 42

 29 omega  151.00  177.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000   50.0000  120.0000 26

 30 omega   37.00   63.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -37.0000   30.0000 26

 31 omega  139.00  174.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000   50.0000  150.0000 35

 32 omega  132.00  178.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000   37.0000 -120.0000 46

 33 omega  104.00  129.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -63.0000 -180.0000 25

 34 omega   71.00  122.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -91.0000   30.0000 51

 35 omega   37.00   62.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -25.0000 -180.0000 25

 36 omega   80.00  121.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  111.0000  -30.0000 41

 37 omega   42.00   71.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -25.0000  150.0000 29

 38 omega   47.00   83.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -50.0000  -60.0000 36

 39 omega   75.00  117.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000   25.0000   90.0000 42

 40 omega   88.00  120.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000   50.0000  150.0000 32

 41 omega   42.00   71.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -63.0000    0.0000 29

 42 omega  129.00  163.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -15.0000  114.6601 34

 43 omega   99.00  133.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  178.0000  120.0000 34

 44 omega   64.00   90.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -91.0000 -150.0000 26

 45 omega   87.00  113.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -93.0000 -175.2424 26

 46 omega   32.00   77.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000 -178.0000 -120.0000 45

 47 omega  -69.00   21.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -57.0000  150.0000 90

 48 omega   32.00   77.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000 -178.0000 -150.0000 45

 49 omega -125.00  -25.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -54.7500  -77.0000 -150.0000 100

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

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

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

 53 omega -124.00  -33.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -54.7500  -57.0000  -90.0000 91

 54 omega   73.00  126.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       54.7500  125.0000  -90.0000 53

 55 omega -134.00  -75.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -64.0000  -77.0000  150.0000 59

 56 omega   84.00  178.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000   37.0000   30.0000 94

 57 omega   79.00  178.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000   77.0000  -30.0000 99

 58 omega   88.00  123.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000   50.0000   90.0000 35
;
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0059621000
_diffrn_orient_matrix_UB_12      0.1526770000
_diffrn_orient_matrix_UB_13      -0.0189048000
_diffrn_orient_matrix_UB_21      0.0267706000
_diffrn_orient_matrix_UB_22      0.0151647000
_diffrn_orient_matrix_UB_23      -0.1360086000
_diffrn_orient_matrix_UB_31      -0.2106692000
_diffrn_orient_matrix_UB_32      0.0071019000
_diffrn_orient_matrix_UB_33      0.0032729000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0385
_diffrn_reflns_av_unetI/netI     0.0281
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            10459
_diffrn_reflns_theta_full        71.9829
_diffrn_reflns_theta_max         71.22
_diffrn_reflns_theta_min         3.94
_diffrn_source                   'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    11.961
_exptl_absorpt_correction_T_max  0.498
_exptl_absorpt_correction_T_min  0.098
_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 colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.824
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rhombohedral
_exptl_crystal_F_000             472
_exptl_crystal_size_max          0.5209
_exptl_crystal_size_mid          0.1775
_exptl_crystal_size_min          0.0688
_refine_diff_density_max         0.361
_refine_diff_density_min         -0.481
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     215
_refine_ls_number_reflns         3266
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0401
_refine_ls_R_factor_gt           0.0372
_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^)+(0.0710P)^2^+0.0613P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1028
_refine_ls_wR_factor_ref         0.1066
_reflns_number_gt                2968
_reflns_number_total             3266
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3ce41150h.txt
_cod_data_source_block           KTTC
_cod_database_code               7211040
_chemical_oxdiff_formula         'S3 N3 C3 H4 O1 K1'
_reflns_odcompleteness_completeness 97.55
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     71.98
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All N(H) groups
2. Restrained distances
 H2B-O2 = O2-H2A
 0.958 with sigma of 0.02
 H1B-O1 = O1-H1A
 0.958 with sigma of 0.02
 H2B-H2A
 1.515 with sigma of 0.04
 H1B-H1A
 1.515 with sigma of 0.04
3.a Aromatic/amide H refined with riding coordinates:
 N3(H3), N4(H4), N10(H10), N14(H14)
;