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_7211041
_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 N6 O2 Rb2 S6'
_chemical_formula_sum            'C6 H8 N6 O2 Rb2 S6'
_chemical_formula_weight         559.48
_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             2013-06-12
_audit_creation_method
;
  Olex2 1.2
  (compiled Apr 23 2013 17:54:37, GUI svn.r4466)
;
_cell_angle_alpha                76.921(4)
_cell_angle_beta                 80.641(4)
_cell_angle_gamma                88.730(4)
_cell_formula_units_Z            2
_cell_length_a                   7.3545(3)
_cell_length_b                   10.5336(4)
_cell_length_c                   11.7338(5)
_cell_measurement_reflns_used    7334
_cell_measurement_temperature    298.6(8)
_cell_measurement_theta_max      71.0580
_cell_measurement_theta_min      4.3040
_cell_volume                     873.54(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      298.6(8)
_diffrn_detector_area_resol_mean 16.1183
_diffrn_measured_fraction_theta_full 0.9938
_diffrn_measured_fraction_theta_max 0.9900
_diffrn_measurement_details
;
  1 omega   47.00   74.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000 -178.0000   90.0000 27

  2 omega   32.00   57.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000 -178.0000 -120.0000 25

  3 omega   38.00   65.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   57.0000 -150.0000 27

  4 omega   40.00   73.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000 -178.0000 -150.0000 33

  5 omega   -4.00   24.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   57.0000 -150.0000 28

  6 omega -112.00  -21.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -54.7500  125.0000    0.0000 91

  7 omega    6.00  127.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       54.7500    0.0000 -120.0000 121

  8 omega   48.00  124.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       54.7500   57.0000 -120.0000 76

  9 omega  -12.00   34.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       54.7500  -57.0000   90.0000 46

 10 omega   -4.00   73.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       54.7500  -57.0000  -90.0000 77

 11 omega -140.00  -63.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -64.0000  178.0000   60.0000 77

 12 omega   42.00   75.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -63.0000 -120.0000 33

 13 omega   38.00   71.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -37.0000   30.0000 33

 14 omega   90.00  122.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -63.0000 -120.0000 32

 15 omega   38.00   72.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -25.0000  -60.0000 34

 16 omega   40.00   68.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -50.0000   30.0000 28

 17 omega  150.00  178.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000   37.0000 -150.0000 28

 18 omega   40.00   66.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -37.0000   60.0000 26

 19 omega   78.00  105.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -91.0000  -30.0000 27

 20 omega   38.00   66.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000 -111.0000 -150.0000 28

 21 omega   38.00   63.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  178.0000   60.0000 25

 22 omega   84.00  141.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000   37.0000 -150.0000 57

 23 omega   97.00  154.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000   37.0000  120.0000 57

 24 omega   37.00   69.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -37.0000 -180.0000 32

 25 omega  120.00  147.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000   37.0000    0.0000 27

 26 omega   39.00  144.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -91.0000    0.0000 105

 27 omega   89.00  116.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -91.0000  150.0000 27

 28 omega   51.00  114.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -63.0000    0.0000 63

 29 omega   41.00   71.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -25.0000  -30.0000 30

 30 omega   40.00   71.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -25.0000 -180.0000 31

 31 omega   42.00   67.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -37.0000  -30.0000 25

 32 omega  147.00  177.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  111.0000    0.0000 30

 33 omega   84.00  123.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  111.0000    0.0000 39

 34 omega   47.00   78.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -50.0000   90.0000 31

 35 omega   61.00  111.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -91.0000  -90.0000 50

 36 omega   51.00  141.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -91.0000 -180.0000 90

 37 omega   47.00   74.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -50.0000 -120.0000 27

 38 omega   90.00  177.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000   50.0000  -30.0000 87

 39 omega   46.00   71.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -25.0000 -120.0000 25

 40 omega   68.00  132.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -63.0000   90.0000 64

 41 omega  121.00  171.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000   63.0000   60.0000 50

 42 omega  106.00  133.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  178.0000   60.0000 27

 43 omega   92.00  129.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -93.0000   49.7917 37

 44 omega   90.00  117.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -91.0000   30.0000 27

 45 omega   57.00   94.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -92.0000 -139.6621 37

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

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

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

 49 omega -125.00  -25.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -54.7500  -77.0000  150.0000 100

 50 omega -125.00  -25.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -54.7500  -77.0000 -150.0000 100

 51 omega -125.00  -25.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -54.7500  -77.0000    0.0000 100

 52 omega -124.00  -33.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -54.7500  -57.0000   60.0000 91

 53 omega   73.00  126.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       54.7500  125.0000    0.0000 53

 54 omega   73.00  126.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       54.7500  125.0000   60.0000 53

 55 omega   33.00  124.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       54.7500   57.0000  -30.0000 91

 56 omega   73.00  126.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       54.7500  125.0000  -60.0000 53

 57 omega   25.00  125.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       54.7500   77.0000 -120.0000 100

 58 omega -134.00  -44.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -64.0000  -77.0000   60.0000 90

 59 omega -134.00  -34.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -64.0000  -77.0000  -90.0000 100

 60 omega   84.00  178.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000   37.0000   90.0000 94

 61 omega   37.00   72.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -25.0000  -90.0000 35

 62 omega   83.00  178.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000   35.0000  -73.0000 95

 63 omega   79.00  178.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000   77.0000  120.0000 99

 64 omega   79.00  178.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000   77.0000   30.0000 99

 65 omega   37.00   90.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000 -111.0000   90.0000 53

 66 omega   79.00  178.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000   77.0000  -60.0000 99

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

 68 omega   79.00  129.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000   77.0000    0.0000 50
;
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0856111000
_diffrn_orient_matrix_UB_12      -0.1299126000
_diffrn_orient_matrix_UB_13      0.0543643000
_diffrn_orient_matrix_UB_21      0.1576957000
_diffrn_orient_matrix_UB_22      0.0752793000
_diffrn_orient_matrix_UB_23      0.0285417000
_diffrn_orient_matrix_UB_31      -0.1135056000
_diffrn_orient_matrix_UB_32      0.0023239000
_diffrn_orient_matrix_UB_33      0.1220109000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0404
_diffrn_reflns_av_unetI/netI     0.0263
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            15054
_diffrn_reflns_theta_full        70.9317
_diffrn_reflns_theta_max         71.21
_diffrn_reflns_theta_min         3.92
_diffrn_source                   'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    14.106
_exptl_absorpt_correction_T_max  0.553
_exptl_absorpt_correction_T_min  0.360
_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    2.127
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rhombohedral
_exptl_crystal_F_000             544
_exptl_crystal_size_max          0.1217
_exptl_crystal_size_mid          0.1042
_exptl_crystal_size_min          0.0739
_refine_diff_density_max         0.794
_refine_diff_density_min         -0.647
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     215
_refine_ls_number_reflns         3358
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0366
_refine_ls_R_factor_gt           0.0325
_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^)+(0.0555P)^2^+0.2841P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0885
_refine_ls_wR_factor_ref         0.0928
_reflns_number_gt                2997
_reflns_number_total             3358
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3ce41150h.txt
_cod_data_source_block           RbTTC1
_cod_original_cell_volume        873.54(7)
_cod_database_code               7211041
_chemical_oxdiff_formula         'S3 N3 C3 H4 O1 Rb1'
_reflns_odcompleteness_completeness 99.38
_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
 H2B-O2 = O2-H2A
 0.957 with sigma of 0.02
 H3A-O3
 0.958 with sigma of 0.02
 O3-H3B
 0.958 with sigma of 0.02
 H3A-O3 = O3-H3B
 0.958 with sigma of 0.02
 H2B-H2A
 1.513 with sigma of 0.04
 H3A-H3B
 1.515 with sigma of 0.04
3.a Aromatic/amide H refined with riding coordinates:
 N3(H3), N4(H4), N5(H5), N10(H10)
;