K2SO4(NH3SO3)2 and Cs2SO4(NH3SO3)3: two deep-UV transparent sulfamate-sulfates with moderate birefringence
Ji, Yun; Zhang, Huili; Wen, Xin; Chen, Jindong; Yang, Guangsai; Yan, Yuchen; Peng, Guang; Ye, Ning; Dalton Transactions 54 (2025) 6596–6602; doi:10.1039/D5DT00401B

data_7718374
_publ_section_title
;
 K2SO4(NH3SO3)2 and Cs2SO4(NH3SO3)3: two deep-UV transparent
 sulfamate-sulfates with moderate birefringence
;
_journal_issue                   16
_journal_name_full               'Dalton Transactions'
_journal_page_first              6596
_journal_page_last               6602
_journal_paper_doi               10.1039/D5DT00401B
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'Cs2 H9 N3 O13 S4'
_chemical_formula_sum            'Cs2 H9 N3 O13 S4'
_chemical_formula_weight         653.16
_space_group_crystal_system      hexagonal
_space_group_IT_number           190
_space_group_name_Hall           'P -6c -2c'
_space_group_name_H-M_alt        'P -6 2 c'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2024-11-16
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2025-01-06 deposited with the CCDC.	2025-03-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   8.7339(3)
_cell_length_b                   8.7339(3)
_cell_length_c                   12.1915(9)
_cell_measurement_reflns_used    1340
_cell_measurement_temperature    273.15
_cell_measurement_theta_max      25.58
_cell_measurement_theta_min      2.69
_cell_volume                     805.39(7)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve 1.5-alpha (Bourhis et al., 2015)'
_diffrn_ambient_temperature      273.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0759
_diffrn_reflns_av_unetI/netI     0.0563
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            5203
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.480
_diffrn_reflns_theta_min         2.693
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    5.109
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5662
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1066 before and 0.0643 after correction.
The Ratio of minimum to maximum transmission is 0.7594.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.693
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             616
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.895
_refine_diff_density_min         -0.519
_refine_diff_density_rms         0.125
_refine_ls_abs_structure_details
;
 Flack x determined using 185 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.02(3)
_refine_ls_extinction_coef       0.015(2)
_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   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     47
_refine_ls_number_reflns         653
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0520
_refine_ls_R_factor_gt           0.0363
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0399P)^2^+2.2641P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0829
_refine_ls_wR_factor_ref         0.0888
_reflns_Friedel_coverage         0.679
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                536
_reflns_number_total             653
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt00401b2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7718374--7718375.cif.'
_cod_original_cell_volume        805.39(8)
_cod_database_code               7718374
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.629
_shelx_estimated_absorpt_t_min   0.556
_olex2_refinement_description
;
1. Uiso/Uaniso restraints and constraints
Uanis(O4) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
2. Others
 Fixed Sof: H1A(0.5) H1B(0.5) H1C(0.5) O3(0.166667) O4(0.5)
3.a Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C)
;
_shelx_res_checksum              62067
_shelx_hkl_checksum              81758
_olex2_submission_special_instructions 'No special instructions were received'