#------------------------------------------------------------------------------
#$Date: 2022-06-29 01:53:26 +0300 (Wed, 29 Jun 2022) $
#$Revision: 276372 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/06/7710628.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_7710628
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            'Ca2 H24 N4 O20 S4'
_chemical_formula_weight         608.63
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2021-10-27 deposited with the CCDC.	2022-06-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.957(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.6250(4)
_cell_length_b                   7.7639(3)
_cell_length_c                   11.6238(4)
_cell_measurement_reflns_used    28865
_cell_measurement_temperature    266(2)
_cell_measurement_theta_max      25.242
_cell_measurement_theta_min      3.167
_cell_volume                     1036.32(6)
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_diffrn_ambient_temperature      266(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'D8 Venture Bruker'
_diffrn_measurement_method       'generic phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1012
_diffrn_reflns_av_unetI/netI     0.0279
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            28865
_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         29.012
_diffrn_reflns_theta_min         3.167
_exptl_absorpt_coefficient_mu    1.052
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.5641
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2014/4'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.950
_exptl_crystal_description       block
_exptl_crystal_F_000             632
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_exptl_transmission_factor_max   0.7458
_exptl_transmission_factor_min   0.5641
_refine_diff_density_max         0.287
_refine_diff_density_min         -0.447
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.114
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     91
_refine_ls_number_reflns         1386
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.125
_refine_ls_R_factor_all          0.0515
_refine_ls_R_factor_gt           0.0305
_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/[σ²(Fo²)+(0.0276P)²+1.3023P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0625
_refine_ls_wR_factor_ref         0.0702
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1089
_reflns_number_total             1386
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d2dt01380k2.cif
_cod_data_source_block           mo_101b_0m
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7710628
_shelx_shelxl_version_number     2018/3
_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.
;
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'
'-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
Ca1 Ca 0.000000 0.07522(7) 0.250000 0.01836(14) Uani 1 2 d S T P . .
S1 S 0.31698(4) 0.20263(6) 0.31410(5) 0.02081(13) Uani 1 1 d . . . . .
O1 O 0.19211(12) 0.2267(2) 0.28500(15) 0.0290(4) Uani 1 1 d . . . . .
O2 O 0.34584(13) 0.0895(2) 0.41482(14) 0.0314(4) Uani 1 1 d . . . . .
O3 O -0.12153(14) -0.1348(2) 0.32898(14) 0.0301(4) Uani 1 1 d . . . . .
N1 N 0.3639(2) 0.1092(3) 0.2050(2) 0.0372(5) Uani 1 1 d D . . . .
H11 H 0.359(4) 0.188(5) 0.138(3) 0.037 Uiso 0.59(4) 1 d D U P . .
H12 H 0.331(2) -0.0062(18) 0.192(2) 0.037 Uiso 1 1 d D U . . .
H13 H 0.4489(12) 0.098(8) 0.209(5) 0.037 Uiso 0.41(4) 1 d D U P . .
OW1 O 0.02006(14) 0.2759(2) 0.09357(15) 0.0313(4) Uani 1 1 d D . . . .
HW11 H -0.0397(19) 0.311(3) 0.041(2) 0.038 Uiso 1 1 d D U . . .
HW12 H 0.070(2) 0.367(3) 0.096(2) 0.038 Uiso 1 1 d D U . . .
OW2 O -0.11578(15) -0.0500(3) 0.07407(15) 0.0371(4) Uani 1 1 d D . . . .
HW21 H -0.093(2) -0.106(3) 0.016(2) 0.045 Uiso 1 1 d D U . . .
HW22 H -0.1867(17) -0.011(4) 0.048(2) 0.045 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'
Ca Ca 0.2262 0.3064 '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
O3 Ca1 O3 95.68(8) 2 . ?
O3 Ca1 OW1 147.27(5) 2 2 ?
O3 Ca1 OW1 91.05(6) . 2 ?
O3 Ca1 OW1 91.05(6) 2 . ?
O3 Ca1 OW1 147.28(5) . . ?
OW1 Ca1 OW1 100.36(9) 2 . ?
O3 Ca1 OW2 76.95(6) 2 2 ?
O3 Ca1 OW2 72.33(6) . 2 ?
OW1 Ca1 OW2 74.71(6) 2 2 ?
OW1 Ca1 OW2 140.24(6) . 2 ?
O3 Ca1 OW2 72.33(6) 2 . ?
O3 Ca1 OW2 76.95(6) . . ?
OW1 Ca1 OW2 140.24(6) 2 . ?
OW1 Ca1 OW2 74.71(6) . . ?
OW2 Ca1 OW2 133.55(9) 2 . ?
O3 Ca1 O1 144.23(5) 2 2 ?
O3 Ca1 O1 79.63(5) . 2 ?
OW1 Ca1 O1 68.49(5) 2 2 ?
OW1 Ca1 O1 76.37(6) . 2 ?
OW2 Ca1 O1 132.74(6) 2 2 ?
OW2 Ca1 O1 72.08(5) . 2 ?
O3 Ca1 O1 79.63(5) 2 . ?
O3 Ca1 O1 144.23(5) . . ?
OW1 Ca1 O1 76.37(6) 2 . ?
OW1 Ca1 O1 68.49(5) . . ?
OW2 Ca1 O1 72.08(5) 2 . ?
OW2 Ca1 O1 132.74(6) . . ?
O1 Ca1 O1 123.89(8) 2 . ?
O3 S1 O1 111.91(9) 3 . ?
O3 S1 O2 112.40(10) 3 . ?
O1 S1 O2 111.17(9) . . ?
O3 S1 N1 105.23(10) 3 . ?
O1 S1 N1 108.68(12) . . ?
O2 S1 N1 107.09(11) . . ?
S1 O1 Ca1 144.43(10) . . ?
S1 O3 Ca1 147.72(10) 3_445 . ?
S1 N1 H11 111(3) . . ?
S1 N1 H12 111.4(15) . . ?
H11 N1 H12 118(3) . . ?
S1 N1 H13 117(4) . . ?
H11 N1 H13 92(4) . . ?
H12 N1 H13 106(4) . . ?
Ca1 OW1 HW11 123.6(18) . . ?
Ca1 OW1 HW12 127.4(17) . . ?
HW11 OW1 HW12 102(2) . . ?
Ca1 OW2 HW21 129.6(19) . . ?
Ca1 OW2 HW22 120.7(19) . . ?
HW21 OW2 HW22 106(3) . . ?
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
Ca1 O3 2.4293(15) 2 ?
Ca1 O3 2.4293(15) . ?
Ca1 OW1 2.4331(17) 2 ?
Ca1 OW1 2.4331(17) . ?
Ca1 OW2 2.4662(17) 2 ?
Ca1 OW2 2.4662(17) . ?
Ca1 O1 2.5006(15) 2 ?
Ca1 O1 2.5007(15) . ?
S1 O3 1.4476(16) 3 ?
S1 O1 1.4504(15) . ?
S1 O2 1.4602(16) . ?
S1 N1 1.627(2) . ?
N1 H11 0.982(10) . ?
N1 H12 0.975(10) . ?
N1 H13 0.985(10) . ?
OW1 HW11 0.896(17) . ?
OW1 HW12 0.914(17) . ?
OW2 HW21 0.878(17) . ?
OW2 HW22 0.887(17) . ?
