Facile synthesis of a cesium trithiocyanurate with high ionic conductivity and large birefringence properties
Zhao, Jianmin; Liu, Hongkun; Zhang, Xiaodong; Zhang, Bingbing; Wang, Ying; CrystEngComm  (2020) –; doi:10.1039/D0CE01116A

data_7241114
_publ_section_title
;
 Facile synthesis of a cesium trithiocyanurate with high ionic
 conductivity and large birefringence properties
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D0CE01116A
_journal_year                    2020
_chemical_formula_moiety         '0.25(C24 H40 Cs16 N24 O16 S24)'
_chemical_formula_sum            'C6 H10 Cs4 N6 O4 S6'
_chemical_formula_weight         954.20
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2019-09-08
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-03-17 deposited with the CCDC.	2020-08-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.961(5)
_cell_length_b                   11.928(3)
_cell_length_c                   8.903(2)
_cell_measurement_reflns_used    2523
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      24.88
_cell_measurement_theta_min      2.95
_cell_volume                     2332.1(9)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0465
_diffrn_reflns_av_unetI/netI     0.0325
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            15954
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.522
_diffrn_reflns_theta_min         1.855
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.764
_exptl_absorpt_correction_T_max  0.6299
_exptl_absorpt_correction_T_min  0.5693
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0559 before and 0.0454 after correction. The Ratio of minimum to maximum transmission is 0.9038. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.718
_exptl_crystal_description       block
_exptl_crystal_F_000             1744
_exptl_crystal_size_max          0.198
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.097
_refine_diff_density_max         1.575
_refine_diff_density_min         -1.271
_refine_diff_density_rms         0.135
_refine_ls_extinction_coef       0.00065(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     154
_refine_ls_number_reflns         2819
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0617
_refine_ls_R_factor_gt           0.0356
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0233P)^2^+5.9056P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0671
_refine_ls_wR_factor_ref         0.0757
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1970
_reflns_number_total             2819
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ce01116a2.cif
_cod_data_source_block           1
_cod_original_cell_volume        2332.2(10)
_cod_database_code               7241114
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.560
_shelx_estimated_absorpt_t_min   0.348
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All N(H) groups
 At 1.4 times of:
  All O(H,H) groups
2. Restrained distances
 O2-H2A = O2-H2B = O3-H3A = O3-H3B = O1-H1B = O1-H1A
 0.88 with sigma of 0.02
3.a Aromatic/amide H refined with riding coordinates:
 N3(H3), N4(H4)
;
_shelx_res_checksum              69974
_olex2_submission_special_instructions 'No special instructions were received'