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#$Date: 2024-07-24 04:56:58 +0300 (Wed, 24 Jul 2024) $
#$Revision: 293522 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/02/32/2023207.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2023207
loop_
_publ_author_name
'Rudnitskaya, Olga V.'
'Komarovskikh, Milena R.'
'Pekarskaya, Maria G.'
'Pshenichnyy, Daniil S.'
'Akkurt, Mehmet'
'Khalilov, Ali N.'
'Bhattarai, Ajaya'
'Mamedov, Ibrahim G.'
_publ_section_title
;
 Synthesis, molecular and crystal structure of
 [(NH2)2CSSC(NH2)2]2[RuBr6]Br2·3H2O
;
_journal_coeditor_code           NY2005
_journal_issue                   8
_journal_name_full
'Acta Crystallographica Section E Crystallographic Communications'
_journal_paper_doi               10.1107/S2056989024006832
_journal_volume                  80
_journal_year                    2024
_chemical_formula_iupac          '(C2 H8 N4 S2)2 [Ru Br6] Br2, 3H2 O'
_chemical_formula_moiety
'2(C2 H8 N4 S2 2+), Br6 Ru 2-, 2(Br -), 3(H2 O)'
_chemical_formula_sum            'C4 H22 Br8 N8 O3 Ru S4'
_chemical_formula_weight         1098.88
_chemical_name_systematic
;
Bis[dithiobis(formamidinium)] hexabromidoruthenium dibromide trihydrate
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           63
_space_group_name_Hall           '-C 2c 2'
_space_group_name_H-M_alt        'C m c m'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     difmap
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.6462(3)
_cell_length_b                   13.9943(4)
_cell_length_c                   16.9225(5)
_cell_measurement_reflns_used    1291
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.60
_cell_measurement_theta_min      2.28
_cell_volume                     2758.04(13)
_computing_cell_refinement
;
SAINT (Bruker, 2016)
;
_computing_data_collection
;
APEX3 (Bruker, 2016)
;
_computing_data_reduction
;
SAINT (Bruker, 2016)
;
_computing_molecular_graphics
;
ORTEP-3 for Windows (Farrugia, 2012)
;
_computing_publication_material
;
PLATON (Spek, 2020)
;
_computing_structure_refinement
;
SHELXL2019/3 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT2014/5 (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0434
_diffrn_reflns_av_unetI/netI     0.0235
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            22642
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.522
_diffrn_reflns_theta_min         2.275
_diffrn_source                   microsource
_exptl_absorpt_coefficient_mu    12.485
_exptl_absorpt_correction_T_max  0.0998
_exptl_absorpt_correction_T_min  0.0425
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Krause et al.,  2015)
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.646
_exptl_crystal_description       plate
_exptl_crystal_F_000             2056
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.020
_refine_diff_density_max         1.061
_refine_diff_density_min         -0.594
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     93
_refine_ls_number_reflns         2269
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0266
_refine_ls_R_factor_gt           0.0227
_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)+(0.0237P)²+6.8980P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0552
_refine_ls_wR_factor_ref         0.0567
_reflns_number_gt                2057
_reflns_number_total             2269
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ny2005.cif
_cod_data_source_block           I
_cod_database_code               2023207
_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.
;
_shelx_estimated_absorpt_t_min   0.117
_shelx_estimated_absorpt_t_max   0.788
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'-x, y, -z+1/2'
'x, -y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x, y, -z-1/2'
'x, -y, z-1/2'
'-x, y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, y+1/2, -z-1/2'
'x+1/2, -y+1/2, z-1/2'
'-x+1/2, y+1/2, z'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ru Ru1 0.500000 0.65423(2) 0.750000 0.01754(8) Uani d 1 . .
Br Br1 0.500000 0.77930(2) 0.85365(2) 0.02178(8) Uani d 1 . .
Br Br2 0.500000 0.52583(2) 0.64822(2) 0.02559(8) Uani d 1 . .
Br Br3 0.28649(3) 0.65551(2) 0.750000 0.02565(9) Uani d 1 . .
Br Br4 0.500000 0.17169(2) 0.58416(2) 0.02717(9) Uani d 1 . .
S S1 0.18284(5) 0.47494(4) 0.55623(4) 0.02521(13) Uani d 1 . .
N N1 0.2957(2) 0.33273(17) 0.61812(15) 0.0280(5) Uani d 1 . .
H H1A 0.264(3) 0.353(2) 0.657(2) 0.034 Uiso d 1 . .
H H1B 0.330(3) 0.285(2) 0.616(2) 0.034 Uiso d 1 . .
N N2 0.3321(2) 0.35163(17) 0.48633(16) 0.0329(5) Uani d 1 . .
H H2A 0.331(3) 0.386(3) 0.443(2) 0.039 Uiso d 1 . .
H H2B 0.380(3) 0.310(2) 0.489(2) 0.039 Uiso d 1 . .
C C1 0.2816(2) 0.37771(17) 0.55165(16) 0.0241(5) Uani d 1 . .
O O1 0.2061(2) 0.4299(2) 0.750000 0.0305(6) Uani d 1 . .
H H1C 0.249(4) 0.478(3) 0.750000 0.046 Uiso d 1 . .
H H1D 0.136(3) 0.445(4) 0.750000 0.046 Uiso d 1 . .
O O2 0.000000 0.5321(3) 0.750000 0.0360(9) Uani d 1 . .
H H2 0.000000 0.579(4) 0.709(3) 0.054 Uiso d 1 . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 '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'
Ru Ru -1.2594 0.8363 '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'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
Br1 Ru1 Br1 . 10_557 90.122(19) ?
Br1 Ru1 Br3 . 3_656 89.708(8) ?
Br1 Ru1 Br3 10_557 3_656 89.708(8) ?
Br1 Ru1 Br3 . . 89.708(8) ?
Br1 Ru1 Br3 10_557 . 89.708(8) ?
Br3 Ru1 Br3 3_656 . 179.17(2) ?
Br1 Ru1 Br2 . 10_557 91.151(12) ?
Br1 Ru1 Br2 10_557 10_557 178.727(16) ?
Br3 Ru1 Br2 3_656 10_557 90.298(8) ?
Br3 Ru1 Br2 . 10_557 90.298(8) ?
Br1 Ru1 Br2 . . 178.729(16) ?
Br1 Ru1 Br2 10_557 . 91.150(12) ?
Br3 Ru1 Br2 3_656 . 90.298(8) ?
Br3 Ru1 Br2 . . 90.298(8) ?
Br2 Ru1 Br2 10_557 . 87.58(2) ?
C1 S1 S1 . 4_566 102.90(9) ?
C1 N1 H1A . . 119(2) ?
C1 N1 H1B . . 117(3) ?
H1A N1 H1B . . 124(4) ?
C1 N2 H2A . . 123(2) ?
C1 N2 H2B . . 117(3) ?
H2A N2 H2B . . 117(3) ?
N1 C1 N2 . . 122.7(2) ?
N1 C1 S1 . . 114.4(2) ?
N2 C1 S1 . . 122.8(2) ?
H1C O1 H1D . . 112(5) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Ru1 Br1 . 2.4779(4) y
Ru1 Br1 10_557 2.4779(4) y
Ru1 Br3 3_656 2.4866(3) y
Ru1 Br3 . 2.4866(3) y
Ru1 Br2 10_557 2.4890(4) y
Ru1 Br2 . 2.4890(4) y
S1 C1 . 1.783(2) ?
S1 S1 4_566 2.0282(12) ?
N1 C1 . 1.299(3) ?
N1 H1A . 0.80(4) ?
N1 H1B . 0.77(3) ?
N2 C1 . 1.305(3) ?
N2 H2A . 0.88(4) ?
N2 H2B . 0.81(3) ?
O1 H1C . 0.84(3) ?
O1 H1D . 0.84(3) ?
O2 H2 . 0.95(5) ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
N1 H1A O1 . 0.80(4) 2.02(4) 2.814(3) 167(3) yes
O1 H1C Br3 . 0.84(3) 2.52(3) 3.293(3) 154(4) yes
O1 H1D O2 . 0.84(3) 2.00(4) 2.794(4) 157(5) yes
N1 H1B Br4 . 0.77(3) 2.60(4) 3.327(2) 157(3) yes
N2 H2B Br1 2_664 0.81(3) 2.96(4) 3.496(2) 125(3) yes
N2 H2A Br2 4_566 0.88(4) 2.79(4) 3.456(2) 134(3) yes
N2 H2B Br4 . 0.81(3) 2.87(4) 3.592(3) 149(3) yes
O2 H2 Br4 5_455 0.95(5) 2.48(5) 3.419(2) 167(4) yes
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
S1 S1 C1 N1 4_566 . . . -179.53(18) ?
S1 S1 C1 N2 4_566 . . . -2.0(2) ?
