New Alkaline-Earth Amidosulfates and their Unexpected Decomposition to S4N4
Gross, Peter; Zhang, Yue; Bayarjargal, Lkhamsuren; Winkler, Bjoern; Höppe, Henning A.; Dalton Transactions  (2022) –; doi:10.1039/D2DT01380K

data_7710630
_publ_section_title
;
 New Alkaline-Earth Amidosulfates and their Unexpected Decomposition to
 S4N4
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT01380K
_journal_year                    2022
_chemical_formula_sum            'Ba H4 N2 O6 S2'
_chemical_formula_weight         329.51
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_atom_sites_solution_hydrogens   difmap
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2021-10-27 deposited with the CCDC.	2022-06-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.5749(8)
_cell_length_b                   13.3927(10)
_cell_length_c                   4.8168(4)
_cell_measurement_reflns_used    18652
_cell_measurement_temperature    283(2)
_cell_measurement_theta_max      42.975
_cell_measurement_theta_min      2.454
_cell_volume                     682.19(9)
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      283(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0670
_diffrn_reflns_av_unetI/netI     0.0665
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            18652
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         42.975
_diffrn_reflns_theta_min         2.454
_exptl_absorpt_coefficient_mu    6.421
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., J. Appl. Cryst. 48 (2015) 3-10.'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    3.208
_exptl_crystal_description       needle
_exptl_crystal_F_000             616
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.02
_exptl_transmission_factor_max   0.7484
_exptl_transmission_factor_min   0.4832
_refine_diff_density_max         1.582
_refine_diff_density_min         -1.816
_refine_diff_density_rms         0.296
_refine_ls_abs_structure_details
;
 Flack x determined using 1403 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.062(11)
_refine_ls_extinction_coef       0.0147(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.953
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     113
_refine_ls_number_reflns         4979
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      0.953
_refine_ls_R_factor_all          0.0637
_refine_ls_R_factor_gt           0.0364
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0268P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0631
_refine_ls_wR_factor_ref         0.0700
_reflns_Friedel_coverage         0.831
_reflns_Friedel_fraction_full    0.985
_reflns_Friedel_fraction_max     0.974
_reflns_number_gt                3672
_reflns_number_total             4979
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01380k2.cif
_cod_data_source_block           mo_PG_19_1145_0m-300K
_cod_original_formula_sum        'H4 Ba N2 O6 S2'
_cod_database_code               7710630
_shelxl_version_number           2013-4
_shelx_res_checksum              35254
_shelx_hkl_checksum              12111