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_7211042
_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 H10.5 N6 O3 Rb1.5 S6'
_chemical_formula_sum            'C6 H10.5 N6 O3 Rb1.5 S6'
_chemical_formula_weight         535.27
_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                107.984(4)
_cell_angle_beta                 94.103(3)
_cell_angle_gamma                102.469(4)
_cell_formula_units_Z            2
_cell_length_a                   7.5673(3)
_cell_length_b                   11.2806(6)
_cell_length_c                   11.4428(4)
_cell_measurement_reflns_used    7535
_cell_measurement_temperature    298.9(8)
_cell_measurement_theta_max      71.1390
_cell_measurement_theta_min      4.1040
_cell_volume                     897.06(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
;
SHELXS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      298.9(8)
_diffrn_detector_area_resol_mean 16.1183
_diffrn_measured_fraction_theta_full 0.9763
_diffrn_measured_fraction_theta_max 0.9920
_diffrn_measurement_details
;
  1 omega    4.00   30.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -99.0000  -30.0000 26

  2 omega   32.00   64.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000 -178.0000  150.0000 32

  3 omega  -65.00  -31.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -77.0000  -90.0000 34

  4 omega   -2.00   24.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -77.0000  -90.0000 26

  5 omega  -66.00  -21.00   1.0000    1.1400
omega____ theta____ kappa____ phi______ frames
    -      -54.7500  125.0000  -60.0000 45

  6 omega   79.00  126.00   1.0000    1.1400
omega____ theta____ kappa____ phi______ frames
    -       54.7500  125.0000   90.0000 47

  7 omega   33.00  124.00   1.0000    1.1400
omega____ theta____ kappa____ phi______ frames
    -       54.7500   77.0000   60.0000 91

  8 omega   75.00  113.00   1.0000    1.1400
omega____ theta____ kappa____ phi______ frames
    -       54.7500  125.0000    0.0000 38

  9 omega   29.00  124.00   1.0000    1.1400
omega____ theta____ kappa____ phi______ frames
    -       54.7500   37.0000 -180.0000 95

 10 omega  -17.00    8.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -64.0000   37.0000  120.0000 25

 11 omega  -69.00  -41.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -64.0000   37.0000  120.0000 28

 12 omega -110.00  -20.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -64.0000  111.0000 -150.0000 90

 13 omega   37.00   70.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -37.0000  -60.0000 33

 14 omega   38.00   68.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -25.0000   90.0000 30

 15 omega   89.00  154.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000   50.0000   30.0000 65

 16 omega   37.00   62.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -37.0000 -180.0000 25

 17 omega   43.00   72.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -25.0000    0.0000 29

 18 omega   97.00  136.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -70.0000  127.9469 39

 19 omega   44.00   70.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -93.0000  139.8682 26

 20 omega   71.00  101.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -77.0000    0.0000 30

 21 omega  122.00  177.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000   25.0000  -30.0000 55

 22 omega   39.00   64.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -37.0000    0.0000 25

 23 omega   84.00  126.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000   37.0000  -60.0000 42

 24 omega   41.00   71.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -50.0000  150.0000 30

 25 omega   42.00   67.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -25.0000   60.0000 25

 26 omega   77.00  117.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000   25.0000    0.0000 40

 27 omega  136.00  173.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000   25.0000    0.0000 37

 28 omega  108.00  133.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  178.0000   60.0000 25

 29 omega   38.00   64.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  178.0000   60.0000 26

 30 omega   38.00   72.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000 -111.0000  -30.0000 34

 31 omega   49.00   80.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -70.0000  127.9469 31

 32 omega   47.00   73.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -50.0000   30.0000 26

 33 omega   95.00  140.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000   25.0000  -90.0000 45

 34 omega   48.00   81.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -91.0000 -120.0000 33

 35 omega   53.00   80.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -50.0000  -90.0000 27

 36 omega  119.00  145.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000   37.0000  120.0000 26

 37 omega  148.00  173.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000   25.0000  -90.0000 25

 38 omega   53.00   82.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -50.0000  -30.0000 29

 39 omega   38.00   70.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -37.0000  150.0000 32

 40 omega  135.00  175.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000   77.0000 -120.0000 40

 41 omega   79.00  120.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -63.0000    0.0000 41

 42 omega   92.00  117.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000   77.0000 -120.0000 25

 43 omega   89.00  116.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000   37.0000  120.0000 27

 44 omega   46.00   71.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -50.0000 -120.0000 25

 45 omega   74.00  145.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -93.0000  139.8682 71

 46 omega   89.00  116.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -63.0000   90.0000 27

 47 omega   68.00  134.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -92.0000    5.3638 66

 48 omega  106.00  133.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  178.0000   90.0000 27

 49 omega   88.00  114.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -91.0000 -180.0000 26

 50 omega  101.00  128.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -91.0000   60.0000 27

 51 omega   41.00  106.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -92.0000  -81.3666 65

 52 omega  -30.00   70.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   77.0000 -150.0000 100

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

 54 omega -125.00  -25.00   1.0000    1.1400
omega____ theta____ kappa____ phi______ frames
    -      -54.7500  -77.0000  120.0000 100

 55 omega -124.00  -33.00   1.0000    1.1400
omega____ theta____ kappa____ phi______ frames
    -      -54.7500  -57.0000 -150.0000 91

 56 omega  -15.00   85.00   1.0000    1.1400
omega____ theta____ kappa____ phi______ frames
    -       54.7500  -77.0000   90.0000 100

 57 omega   25.00  125.00   1.0000    1.1400
omega____ theta____ kappa____ phi______ frames
    -       54.7500   77.0000    0.0000 100

 58 omega   25.00  125.00   1.0000    1.1400
omega____ theta____ kappa____ phi______ frames
    -       54.7500   77.0000 -150.0000 100

 59 omega   25.00  125.00   1.0000    1.1400
omega____ theta____ kappa____ phi______ frames
    -       54.7500   77.0000  -60.0000 100

 60 omega   88.00  178.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000   50.0000    0.0000 90

 61 omega   84.00  178.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000   37.0000 -120.0000 94

 62 omega   37.00   72.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -25.0000  -90.0000 35

 63 omega   84.00  178.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000   37.0000   90.0000 94

 64 omega   37.00   72.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -25.0000 -150.0000 35

 65 omega   79.00  118.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000   77.0000  120.0000 39

 66 omega   88.00  119.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000   50.0000 -180.0000 31
;
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.1919855000
_diffrn_orient_matrix_UB_12      -0.0672477000
_diffrn_orient_matrix_UB_13      0.0164816000
_diffrn_orient_matrix_UB_21      -0.0533812000
_diffrn_orient_matrix_UB_22      -0.0582943000
_diffrn_orient_matrix_UB_23      -0.1421856000
_diffrn_orient_matrix_UB_31      0.0689107000
_diffrn_orient_matrix_UB_32      -0.1186580000
_diffrn_orient_matrix_UB_33      0.0009512000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0261
_diffrn_reflns_av_unetI/netI     0.0192
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            12265
_diffrn_reflns_theta_full        71.9829
_diffrn_reflns_theta_max         71.15
_diffrn_reflns_theta_min         4.11
_diffrn_source                   'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    12.154
_exptl_absorpt_correction_T_max  0.647
_exptl_absorpt_correction_T_min  0.123
_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    1.982
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'rect. Prism'
_exptl_crystal_F_000             528
_exptl_crystal_size_max          0.5026
_exptl_crystal_size_mid          0.0751
_exptl_crystal_size_min          0.0386
_refine_diff_density_max         0.354
_refine_diff_density_min         -0.654
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.222
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     229
_refine_ls_number_reflns         3453
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      1.220
_refine_ls_R_factor_all          0.0303
_refine_ls_R_factor_gt           0.0295
_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^)+(0.0259P)^2^+0.8496P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0745
_refine_ls_wR_factor_ref         0.0750
_reflns_number_gt                3368
_reflns_number_total             3453
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3ce41150h.txt
_cod_data_source_block           RbTTC2
_cod_original_formula_sum        'C6 H10.50 N6 O3 Rb1.50 S6'
_cod_database_code               7211042
_chemical_oxdiff_formula         'S6 N6 C6 H9 O2.5 Rb1.5'
_reflns_odcompleteness_completeness 97.63
_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
 H1B-O1 = O1-H1A
 0.957 with sigma of 0.02
 H2B-O2 = O2-H2A
 0.957 with sigma of 0.02
 H3A-O3
 0.957 with sigma of 0.02
 H3B-O3
 0.957 with sigma of 0.02
 H2A-O2 = O2-H2B
 0.958 with sigma of 0.02
 H1A-O1 = O1-H1B
 0.958 with sigma of 0.02
 H3A-O3
 0.958 with sigma of 0.02
 H3B-O3
 0.958 with sigma of 0.02
 H1B-H1A
 1.513 with sigma of 0.04
 H2B-H2A
 1.513 with sigma of 0.04
 H2A-H2B
 1.515 with sigma of 0.04
 H1A-H1B
 1.515 with sigma of 0.04
3. Others
 Fixed Sof: H3B(0.5)
4.a Aromatic/amide H refined with riding coordinates:
 N1(H1), N2(H2), N4(H4), N5(H5), N6(H6)
;