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#$Date: 2022-06-29 01:53:26 +0300 (Wed, 29 Jun 2022) $
#$Revision: 276372 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/06/7710630.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7710630
loop_
_publ_author_name
'Gross, Peter'
'Zhang, Yue'
'Bayarjargal, Lkhamsuren'
'Winkler, Bjoern'
'Höppe, Henning A.'
_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+0.001xFc²λ³/sin(2θ)]^-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/[σ²(Fo²)+(0.0268P)²] where P=(Fo²+2Fc²)/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 > 2σ(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
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelxl_version_number           2013-4
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'x+1/2, -y+1/2, z'
'-x+1/2, y+1/2, z+1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ba1 Ba 0.32408(2) 0.31495(2) 0.39274(5) 0.01265(6) Uani 1 1 d . . . . .
S1 S 0.04951(9) 0.31722(7) -0.04908(19) 0.01154(17) Uani 1 1 d . . . . .
S2 S 0.16942(9) 0.05042(7) 0.4727(2) 0.01175(16) Uani 1 1 d . . . . .
O11 O 0.4381(2) 0.24267(19) 0.8886(11) 0.0202(5) Uani 1 1 d . . . . .
O23 O 0.2807(3) 0.1056(2) 0.3879(12) 0.0243(6) Uani 1 1 d . . . . .
O21 O 0.3250(3) 0.4460(2) 0.8886(12) 0.0246(6) Uani 1 1 d . . . . .
O13 O 0.0646(4) 0.3362(3) 0.2469(7) 0.0229(7) Uani 1 1 d . . . . .
O22 O 0.5530(3) 0.4034(2) 0.3868(13) 0.0311(7) Uani 1 1 d . . . . .
O12 O 0.1650(3) 0.2737(2) 0.8400(8) 0.0198(8) Uani 1 1 d . . . . .
N1 N 0.0207(4) 0.4250(3) -0.1919(9) 0.0194(7) Uani 1 1 d D . . . .
H11 H 0.095(3) 0.467(3) -0.165(13) 0.023 Uiso 1 1 d D U . . .
H12 H 0.001(6) 0.417(4) -0.391(4) 0.023 Uiso 1 1 d D U . . .
N2 N 0.1742(5) 0.0466(4) 0.8128(10) 0.0301(11) Uani 1 1 d D . . . .
H21 H 0.230(5) 0.102(3) 0.869(18) 0.036 Uiso 1 1 d D U . . .
H22 H 0.102(5) 0.054(4) 0.941(12) 0.036 Uiso 1 1 d D U . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ba Ba -0.3244 2.2819 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O22 Ba1 O12 129.58(15) . . ?
O22 Ba1 O23 125.35(9) . . ?
O12 Ba1 O23 73.34(12) . . ?
O22 Ba1 O11 77.15(13) . . ?
O12 Ba1 O11 62.60(10) . . ?
O23 Ba1 O11 74.90(13) . . ?
O22 Ba1 O13 145.02(11) . . ?
O12 Ba1 O13 68.22(10) . . ?
O23 Ba1 O13 86.61(11) . . ?
O11 Ba1 O13 130.52(10) . . ?
O22 Ba1 O11 76.27(14) . 1_554 ?
O12 Ba1 O11 146.89(9) . 1_554 ?
O23 Ba1 O11 74.27(12) . 1_554 ?
O11 Ba1 O11 114.58(8) . 1_554 ?
O13 Ba1 O11 103.25(10) . 1_554 ?
O22 Ba1 O21 75.25(14) . . ?
O12 Ba1 O21 59.79(10) . . ?
O23 Ba1 O21 126.26(14) . . ?
O11 Ba1 O21 61.55(10) . . ?
O13 Ba1 O21 98.21(10) . . ?
O11 Ba1 O21 151.34(9) 1_554 . ?
O22 Ba1 O21 74.41(13) . 1_554 ?
O12 Ba1 O21 138.09(9) . 1_554 ?
O23 Ba1 O21 124.88(14) . 1_554 ?
O11 Ba1 O21 151.43(9) . 1_554 ?
O13 Ba1 O21 75.21(10) . 1_554 ?
O11 Ba1 O21 60.79(10) 1_554 1_554 ?
O21 Ba1 O21 107.85(8) . 1_554 ?
O22 Ba1 N2 63.73(13) . 4_554 ?
O12 Ba1 N2 107.19(11) . 4_554 ?
O23 Ba1 N2 168.31(14) . 4_554 ?
O11 Ba1 N2 116.01(11) . 4_554 ?
O13 Ba1 N2 82.89(13) . 4_554 ?
O11 Ba1 N2 103.14(11) 1_554 4_554 ?
O21 Ba1 N2 60.77(12) . 4_554 ?
O21 Ba1 N2 47.08(12) 1_554 4_554 ?
O22 Ba1 O12 122.67(14) . 1_554 ?
O12 Ba1 O12 106.95(10) . 1_554 ?
O23 Ba1 O12 74.78(13) . 1_554 ?
O11 Ba1 O12 149.66(8) . 1_554 ?
O13 Ba1 O12 45.95(9) . 1_554 ?
O11 Ba1 O12 57.31(8) 1_554 1_554 ?
O21 Ba1 O12 140.82(9) . 1_554 ?
O21 Ba1 O12 55.12(9) 1_554 1_554 ?
N2 Ba1 O12 94.14(11) 4_554 1_554 ?
O22 Ba1 O13 65.06(10) . 3 ?
O12 Ba1 O13 120.25(9) . 3 ?
O23 Ba1 O13 61.38(9) . 3 ?
O11 Ba1 O13 69.27(9) . 3 ?
O13 Ba1 O13 138.23(9) . 3 ?
O11 Ba1 O13 45.31(9) 1_554 3 ?
O21 Ba1 O13 121.88(9) . 3 ?
O21 Ba1 O13 100.53(9) 1_554 3 ?
N2 Ba1 O13 125.00(12) 4_554 3 ?
O12 Ba1 O13 96.96(8) 1_554 3 ?
O22 Ba1 S1 135.60(12) . . ?
O12 Ba1 S1 88.38(7) . . ?
O23 Ba1 S1 82.72(9) . . ?
O11 Ba1 S1 147.24(6) . . ?
O13 Ba1 S1 22.46(7) . . ?
O11 Ba1 S1 80.92(7) 1_554 . ?
O21 Ba1 S1 118.29(7) . . ?
O21 Ba1 S1 61.22(7) 1_554 . ?
N2 Ba1 S1 85.62(10) 4_554 . ?
O12 Ba1 S1 23.79(5) 1_554 . ?
O13 Ba1 S1 119.81(7) 3 . ?
O12 S1 O11 112.5(2) 1_554 3_454 ?
O12 S1 O13 109.7(2) 1_554 . ?
O11 S1 O13 112.7(3) 3_454 . ?
O12 S1 N1 111.0(2) 1_554 . ?
O11 S1 N1 104.5(2) 3_454 . ?
O13 S1 N1 106.2(2) . . ?
O12 S1 Ba1 62.41(15) 1_554 . ?
O11 S1 Ba1 140.32(17) 3_454 . ?
O13 S1 Ba1 48.31(16) . . ?
N1 S1 Ba1 114.10(15) . . ?
O12 S1 Ba1 124.56(14) 1_554 3_455 ?
O11 S1 Ba1 47.6(2) 3_454 3_455 ?
O13 S1 Ba1 65.51(16) . 3_455 ?
N1 S1 Ba1 123.61(16) . 3_455 ?
Ba1 S1 Ba1 100.25(2) . 3_455 ?
O22 S2 O23 113.3(2) 3_455 . ?
O22 S2 O21 111.6(2) 3_455 4_544 ?
O23 S2 O21 112.2(2) . 4_544 ?
O22 S2 N2 109.1(3) 3_455 . ?
O23 S2 N2 105.8(3) . . ?
O21 S2 N2 104.3(3) 4_544 . ?
S1 O11 Ba1 134.7(3) 3_556 . ?
S1 O11 Ba1 110.5(3) 3_556 1_556 ?
Ba1 O11 Ba1 114.58(8) . 1_556 ?
S2 O23 Ba1 129.21(19) . . ?
S2 O21 Ba1 142.4(3) 4 . ?
S2 O21 Ba1 109.7(3) 4 1_556 ?
Ba1 O21 Ba1 107.85(8) . 1_556 ?
S1 O13 Ba1 109.2(2) . . ?
S1 O13 Ba1 90.99(17) . 3_455 ?
Ba1 O13 Ba1 128.64(13) . 3_455 ?
S2 O22 Ba1 162.7(4) 3 . ?
S1 O12 Ba1 135.27(19) 1_556 . ?
S1 O12 Ba1 93.81(17) 1_556 1_556 ?
Ba1 O12 Ba1 106.95(10) . 1_556 ?
S2 N2 Ba1 98.8(2) . 4_545 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ba1 O22 2.695(3) . ?
Ba1 O12 2.789(3) . ?
Ba1 O23 2.841(3) . ?
Ba1 O11 2.845(5) . ?
Ba1 O13 2.847(4) . ?
Ba1 O11 2.879(5) 1_554 ?
Ba1 O21 2.964(5) . ?
Ba1 O21 2.996(5) 1_554 ?
Ba1 N2 3.127(5) 4_554 ?
Ba1 O12 3.198(4) 1_554 ?
Ba1 O13 3.325(4) 3 ?
Ba1 S1 3.6001(10) . ?
S1 O12 1.455(3) 1_554 ?
S1 O11 1.456(3) 3_454 ?
S1 O13 1.457(4) . ?
S1 N1 1.628(4) . ?
S1 Ba1 3.6532(10) 3_455 ?
S2 O22 1.439(3) 3_455 ?
S2 O23 1.448(3) . ?
S2 O21 1.458(3) 4_544 ?
S2 N2 1.640(5) . ?
O11 S1 1.456(3) 3_556 ?
O11 Ba1 2.879(5) 1_556 ?
O21 S2 1.458(3) 4 ?
O21 Ba1 2.996(5) 1_556 ?
O13 Ba1 3.325(4) 3_455 ?
O22 S2 1.439(3) 3 ?
O12 S1 1.455(3) 1_556 ?
O12 Ba1 3.198(4) 1_556 ?
N2 Ba1 3.127(5) 4_545 ?
