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_7718375
_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         'H6 K2 N2 O10 S3'
_chemical_formula_sum            'H6 K2 N2 O10 S3'
_chemical_formula_weight         368.45
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-12-06
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2025-01-06 deposited with the CCDC.	2025-03-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.113(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   5.6647(5)
_cell_length_b                   18.6566(14)
_cell_length_c                   10.6598(7)
_cell_measurement_reflns_used    3657
_cell_measurement_temperature    273.15
_cell_measurement_theta_max      26.65
_cell_measurement_theta_min      2.20
_cell_volume                     1126.36(15)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      273.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0975
_diffrn_reflns_av_unetI/netI     0.0339
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            24003
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        24.698
_diffrn_reflns_theta_max         24.698
_diffrn_reflns_theta_min         2.183
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    1.443
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6711
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1291 before and 0.0743 after correction.
The Ratio of minimum to maximum transmission is 0.9001.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.173
_exptl_crystal_description       block
_exptl_crystal_F_000             744
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.0115
_exptl_crystal_size_min          0.011
_refine_diff_density_max         1.349
_refine_diff_density_min         -0.884
_refine_diff_density_rms         0.118
_refine_ls_extinction_coef       0.0034(13)
_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   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     157
_refine_ls_number_reflns         1921
_refine_ls_number_restraints     72
_refine_ls_restrained_S_all      1.162
_refine_ls_R_factor_all          0.0730
_refine_ls_R_factor_gt           0.0591
_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^)+(0.0726P)^2^+6.1224P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1550
_refine_ls_wR_factor_ref         0.1638
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1541
_reflns_number_total             1921
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt00401b2.cif
_cod_data_source_block           111s
_cod_depositor_comments
'Adding full bibliography for 7718374--7718375.cif.'
_cod_database_code               7718375
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.984
_shelx_estimated_absorpt_t_min   0.846
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All N(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 2A
3.a Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C), N2(H2A,H2B,H2C)
;
_shelx_res_checksum              8143
_shelx_hkl_checksum              57320
_olex2_submission_special_instructions 'No special instructions were received'