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_7211043
_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 H2 Cs N3 S3'
_chemical_formula_sum            'C3 H2 Cs N3 S3'
_chemical_formula_weight         309.17
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-05-30
_audit_creation_method
;
  Olex2 1.2
  (compiled Apr 23 2013 17:54:37, GUI svn.r4466)
;
_cell_angle_alpha                96.431(5)
_cell_angle_beta                 103.270(5)
_cell_angle_gamma                104.265(5)
_cell_formula_units_Z            2
_cell_length_a                   5.1031(3)
_cell_length_b                   7.9838(6)
_cell_length_c                   10.9408(6)
_cell_measurement_reflns_used    2771
_cell_measurement_temperature    300.00(14)
_cell_measurement_theta_max      71.1650
_cell_measurement_theta_min      4.2150
_cell_volume                     413.70(5)
_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 0.979
_diffrn_measured_fraction_theta_max 0.9794
_diffrn_measurement_details
;
  1 omega   32.00   57.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000 -178.0000 -120.0000 25

  2 omega  -64.00  -37.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -77.0000 -150.0000 27

  3 omega    2.00   28.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -77.0000 -150.0000 26

  4 omega -123.00  -90.00   1.0000    2.1700
omega____ theta____ kappa____ phi______ frames
    -      -54.7500 -158.0000  -10.0000 33

  5 omega -123.00  -28.00   1.0000    2.1700
omega____ theta____ kappa____ phi______ frames
    -      -54.7500  -77.0000 -180.0000 95

  6 omega  -12.00   43.00   1.0000    2.1700
omega____ theta____ kappa____ phi______ frames
    -       54.7500  -57.0000    0.0000 55

  7 omega   -5.00   70.00   1.0000    2.1700
omega____ theta____ kappa____ phi______ frames
    -       54.7500  -37.0000 -180.0000 75

  8 omega   73.00  113.00   1.0000    2.1700
omega____ theta____ kappa____ phi______ frames
    -       54.7500  125.0000 -120.0000 40

  9 omega    0.00   94.00   1.0000    2.1700
omega____ theta____ kappa____ phi______ frames
    -       54.7500 -125.0000  -30.0000 94

 10 omega  -74.00  -47.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -64.0000  -50.0000   30.0000 27

 11 omega   42.00   71.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -25.0000  -90.0000 29

 12 omega   79.00  138.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -91.0000 -150.0000 59

 13 omega   85.00  122.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000   37.0000  150.0000 37

 14 omega   39.00   66.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -37.0000 -180.0000 27

 15 omega   43.00   69.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -50.0000  -90.0000 26

 16 omega   38.00   67.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -25.0000 -150.0000 29

 17 omega   37.00   71.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -25.0000 -120.0000 34

 18 omega   37.00   62.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -37.0000   90.0000 25

 19 omega   39.00  111.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -91.0000    0.0000 72

 20 omega   94.00  121.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -91.0000  120.0000 27

 21 omega   87.00  176.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000   63.0000 -180.0000 89

 22 omega   42.00   68.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -37.0000  150.0000 26

 23 omega   44.00   90.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -91.0000  120.0000 46

 24 omega   53.00  103.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -91.0000  -60.0000 50

 25 omega   91.00  122.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000   37.0000   30.0000 31

 26 omega  153.00  178.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000   37.0000   30.0000 25

 27 omega   43.00   70.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -37.0000  -30.0000 27

 28 omega  147.00  173.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000   37.0000  150.0000 26

 29 omega   76.00  126.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000   12.0000  150.0000 50

 30 omega   82.00  111.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  111.0000 -150.0000 29

 31 omega   43.00   72.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000   12.0000  150.0000 29

 32 omega   37.00   71.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -25.0000   30.0000 34

 33 omega  140.00  169.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  111.0000 -150.0000 29

 34 omega   46.00   95.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -77.0000  150.0000 49

 35 omega  110.00  140.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -77.0000  150.0000 30

 36 omega   47.00   88.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000 -111.0000   90.0000 41

 37 omega  120.00  164.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000   63.0000  -60.0000 44

 38 omega  107.00  133.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000   50.0000  150.0000 26

 39 omega   73.00  119.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  178.0000  -30.0000 46

 40 omega   78.00  123.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -85.0000   -7.4306 45

 41 omega  -70.00   30.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -77.0000  -60.0000 100

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

 43 omega -124.00  -33.00   1.0000    2.1700
omega____ theta____ kappa____ phi______ frames
    -      -54.7500  -57.0000 -120.0000 91

 44 omega -125.00  -25.00   1.0000    2.1700
omega____ theta____ kappa____ phi______ frames
    -      -54.7500  -77.0000   90.0000 100

 45 omega   25.00   50.00   1.0000    2.1700
omega____ theta____ kappa____ phi______ frames
    -       54.7500   77.0000    0.0000 25

 46 omega   33.00  124.00   1.0000    2.1700
omega____ theta____ kappa____ phi______ frames
    -       54.7500   57.0000  -30.0000 91
;
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.1139233000
_diffrn_orient_matrix_UB_12      -0.0738053000
_diffrn_orient_matrix_UB_13      -0.1441089000
_diffrn_orient_matrix_UB_21      -0.0944874000
_diffrn_orient_matrix_UB_22      0.1658948000
_diffrn_orient_matrix_UB_23      -0.0213044000
_diffrn_orient_matrix_UB_31      0.2873498000
_diffrn_orient_matrix_UB_32      0.0893325000
_diffrn_orient_matrix_UB_33      -0.0199781000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0271
_diffrn_reflns_av_unetI/netI     0.0288
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            3826
_diffrn_reflns_theta_full        71.06
_diffrn_reflns_theta_max         71.06
_diffrn_reflns_theta_min         4.22
_diffrn_source                   'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    41.431
_exptl_absorpt_correction_T_max  0.293
_exptl_absorpt_correction_T_min  0.034
_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_density_diffrn    2.482
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             288
_exptl_crystal_size_max          0.1963
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.0449
_refine_diff_density_max         0.938
_refine_diff_density_min         -0.444
_refine_diff_density_rms         0.115
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.149
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     91
_refine_ls_number_reflns         1568
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.149
_refine_ls_R_factor_all          0.0307
_refine_ls_R_factor_gt           0.0301
_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^)+(0.0482P)^2^+0.1938P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0852
_refine_ls_wR_factor_ref         0.0857
_reflns_number_gt                1527
_reflns_number_total             1568
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3ce41150h.txt
_cod_data_source_block           CsTTC1
_cod_original_cell_volume        413.70(4)
_cod_database_code               7211043
_chemical_oxdiff_formula         'Cs C3 N3 S3 H2'
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All N(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 N1(H1), N3(H3)
;